####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # If this CIF has been generated from an entry in the Cambridge # Structural Database, then it will include bibliographic, chemical, # crystal, experimental, refinement or atomic coordinate data resulting # from the CCDC's data processing and validation procedures. # ####################################################################### data_CSD_CIF_BUTXUJ _audit_creation_date 1984-02-21 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD BUTXUJ _database_code_depnum_ccdc_archive 'CCDC 1117410' _chemical_formula_sum 'C36 H86 Li2 O4 Si6' _chemical_formula_moiety ; C16 H32 Li1 O4 1+,C20 H54 Li1 Si6 1- ; _journal_coden_Cambridge 182 _journal_year 1983 _journal_page_first 827 _journal_name_full 'Chem.Commun. ' loop_ _publ_author_name "C.Eaborn" "P.B.Hitchcock" "J.D.Smith" "A.C.Sullivan" _chemical_name_systematic ; tetrakis(Tetrahydrofuran)-lithium bis(tris(trimethylsilyl)-methyl)-lithium ; _cell_volume 2633.203 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 0.97 _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; _refine_special_details ; C(27) is two-fold disordered. One position is retained. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.18 _refine_ls_wR_factor_gt 0.18 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 9.411(3) _cell_length_b 12.045(3) _cell_length_c 23.354(7) _cell_angle_alpha 94.47(2) _cell_angle_beta 90.09(3) _cell_angle_gamma 93.86(2) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 Li 1.13 O 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Si1 Si 0.22620 -0.17270 0.51750 Si2 Si 0.02360 -0.11720 0.61750 Si3 Si -0.08380 -0.25290 0.50980 C1 C 0.03810 -0.15200 0.53870 C2 C 0.35540 -0.08070 0.56670 C3 C 0.29690 -0.31470 0.52250 C4 C 0.27410 -0.13270 0.44120 C5 C 0.13380 -0.21340 0.66810 C6 C 0.07850 0.02620 0.64850 C7 C -0.17970 -0.14540 0.63850 C8 C -0.09580 -0.38860 0.55310 C9 C -0.27420 -0.20790 0.49450 C10 C -0.03900 -0.30890 0.43380 Li1 Li 0.00000 0.00000 0.50000 Si4 Si 0.07560 0.10430 0.12590 Si5 Si 0.01890 0.25980 0.03160 Si6 Si -0.22840 0.12200 0.08070 C11 C -0.04200 0.13120 0.06780 C12 C 0.24710 0.04390 0.10100 C13 C 0.11500 0.23550 0.18310 C14 C -0.01720 -0.00570 0.17120 C15 C -0.02860 0.25320 -0.04990 C16 C -0.06620 0.39040 0.06470 C17 C 0.22560 0.29340 0.03760 C18 C -0.34430 0.17470 0.01850 C19 C -0.31890 -0.02850 0.08460 C20 C -0.28120 0.20010 0.15570 Li2 Li 0.00000 0.00000 0.00000 Li3 Li 0.63760 0.37050 0.75810 O1 O 0.56560 0.40490 0.82930 O2 O 0.84740 0.38110 0.75210 O3 O 0.55930 0.45780 0.69950 O4 O 0.57560 0.20560 0.73740 C21 C 0.56640 0.34360 0.87090 C22 C 0.52460 0.40070 0.92980 C23 C 0.40050 0.42470 0.90450 C24 C 0.49670 0.49180 0.86450 C25 C 0.93190 0.47050 0.72320 C26 C 1.06410 0.46390 0.74790 C27 C 1.04100 0.35940 0.76950 C28 C 0.94410 0.34950 0.79900 C29 C 0.51850 0.58090 0.71440 C30 C 0.50570 0.59780 0.65450 C31 C 0.49170 0.49470 0.60980 C32 C 0.52140 0.40130 0.64700 C33 C 0.66440 0.11700 0.73760 C34 C 0.55580 0.00450 0.73110 C35 C 0.44420 0.04240 0.74430 C36 C 0.43020 0.16250 0.72150 C1A C -0.03810 0.15200 0.46130 Si1A Si -0.22620 0.17270 0.48250 Si2A Si -0.02360 0.11720 0.38250 Si3A Si 0.08380 0.25290 0.49020 C2A C -0.35540 0.08070 0.43330 C3A C -0.29690 0.31470 0.47750 C4A C -0.27410 0.13270 0.55880 C5A C -0.13380 0.21340 0.33190 C6A C -0.07850 -0.02620 0.35150 C7A C 0.17970 0.14540 0.36150 C8A C 0.09580 0.38860 0.44690 C9A C 0.27420 0.20790 0.50550 C10A C 0.03900 0.30890 0.56620 C11A C 0.04200 -0.13120 -0.06780 Si4A Si -0.07560 -0.10430 -0.12590 Si5A Si -0.01890 -0.25980 -0.03160 Si6A Si 0.22840 -0.12200 -0.08070 C12A C -0.24710 -0.04390 -0.10100 C13A C -0.11500 -0.23550 -0.18310 C14A C 0.01720 0.00570 -0.17120 C15A C 0.02860 -0.25320 0.04990 C16A C 0.06620 -0.39040 -0.06470 C17A C -0.22560 -0.29340 -0.03760 C18A C 0.34430 -0.17470 -0.01850 C19A C 0.31890 0.02850 -0.08460 C20A C 0.28120 -0.20010 -0.15570 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Si1 C1 1.867 1_555 1_555 Si2 C1 1.863 1_555 1_555 Si3 C1 1.712 1_555 1_555 C1 Li1 2.155 1_555 1_555 C2 Si1 1.908 1_555 1_555 C3 Si1 1.888 1_555 1_555 C4 Si1 1.928 1_555 1_555 C5 Si2 2.046 1_555 1_555 C6 Si2 1.860 1_555 1_555 C7 Si2 1.989 1_555 1_555 C8 Si3 1.985 1_555 1_555 C9 Si3 1.947 1_555 1_555 C10 Si3 1.907 1_555 1_555 Li1 C1A 2.155 1_555 1_555 Si4 C11 1.812 1_555 1_555 Si5 C11 1.878 1_555 1_555 Si6 C11 1.778 1_555 1_555 C11 Li2 2.204 1_555 1_555 C12 Si4 1.889 1_555 1_555 C13 Si4 2.002 1_555 1_555 C14 Si4 1.924 1_555 1_555 C15 Si5 1.949 1_555 1_555 C16 Si5 1.922 1_555 1_555 C17 Si5 1.963 1_555 1_555 C18 Si6 1.984 1_555 1_555 C19 Si6 1.959 1_555 1_555 C20 Si6 2.002 1_555 1_555 Li2 C11A 2.204 1_555 1_555 Li3 O1 1.825 1_555 1_555 O1 C21 1.266 1_555 1_555 O2 Li3 1.976 1_555 1_555 O3 Li3 1.961 1_555 1_555 O4 Li3 2.052 1_555 1_555 C21 C22 1.553 1_555 1_555 C22 C23 1.366 1_555 1_555 C23 C24 1.539 1_555 1_555 C24 O1 1.467 1_555 1_555 C25 O2 1.499 1_555 1_555 C26 C25 1.380 1_555 1_555 C27 C26 1.396 1_555 1_555 C28 O2 1.510 1_555 1_555 C29 O3 1.570 1_555 1_555 C30 C29 1.435 1_555 1_555 C31 C30 1.557 1_555 1_555 C32 O3 1.389 1_555 1_555 C33 O4 1.399 1_555 1_555 C34 C33 1.639 1_555 1_555 C35 C34 1.204 1_555 1_555 C36 O4 1.467 1_555 1_555 C1A Si1A 1.867 1_555 1_555 Si1A C2A 1.908 1_555 1_555 Si2A C1A 1.863 1_555 1_555 Si3A C1A 1.712 1_555 1_555 C3A Si1A 1.888 1_555 1_555 C4A Si1A 1.928 1_555 1_555 C5A Si2A 2.046 1_555 1_555 C6A Si2A 1.860 1_555 1_555 C7A Si2A 1.989 1_555 1_555 C8A Si3A 1.985 1_555 1_555 C9A Si3A 1.947 1_555 1_555 C10A Si3A 1.907 1_555 1_555 C11A Si4A 1.812 1_555 1_555 Si4A C12A 1.889 1_555 1_555 Si5A C11A 1.878 1_555 1_555 Si6A C11A 1.778 1_555 1_555 C13A Si4A 2.002 1_555 1_555 C14A Si4A 1.924 1_555 1_555 C15A Si5A 1.949 1_555 1_555 C16A Si5A 1.922 1_555 1_555 C17A Si5A 1.963 1_555 1_555 C18A Si6A 1.984 1_555 1_555 C19A Si6A 1.959 1_555 1_555 C20A Si6A 2.002 1_555 1_555 C27 C28 1.149 1_555 1_555 C31 C32 1.514 1_555 1_555 C35 C36 1.593 1_555 1_555 #END data_CSD_CIF_CEDNII _audit_creation_date 1984-10-09 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD CEDNII _database_code_depnum_ccdc_archive 'CCDC 1122168' _chemical_formula_sum 'C108 H150 Li6 N21 O5 P5' _chemical_formula_moiety ; C24 H72 Li1 N12 O4 P4 1+,C84 H78 Li5 N9 O1 P1 1- ; _journal_coden_Cambridge 182 _journal_year 1984 _journal_page_first 226 _journal_name_full 'Chem.Commun. ' loop_ _publ_author_name "D.Barr" "W.Clegg" "R.E.Mulvey" "R.Snaith" _chemical_name_systematic ; tetrakis(Hexamethylphosphoramide)-lithium tris(\m~3~-diphenylmethyleneimido)-tris(\m~2~-diphenylmethyleneimido)-hexameth ylphosphoramide-penta-lithium ; _chemical_melting_point 422.15 _cell_volume 6012.620 _exptl_crystal_colour 'orange-red' _exptl_special_details ; Melting point range 422.15-464.15K ; _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.15 _refine_ls_wR_factor_gt 0.15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,-z _cell_length_a 15.965(2) _cell_length_b 25.883(3) _cell_length_c 16.532(2) _cell_angle_alpha 90 _cell_angle_beta 118.34(1) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 Li 1.06 N 0.68 O 0.68 P 1.05 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.33210 0.50000 0.16630 Li2 Li 0.19130 0.56370 0.12550 Li3 Li 0.36630 0.57970 0.09850 Li4 Li 0.39120 0.57570 0.29180 Li5 Li 0.29750 0.66480 0.17670 O1 O 0.35040 0.43000 0.16900 P1 P 0.36070 0.37170 0.16510 N1 N 0.43890 0.35920 0.13180 C1 C 0.52210 0.39150 0.15410 C2 C 0.42990 0.31740 0.06870 N2 N 0.25950 0.34640 0.09290 C3 C 0.22650 0.29650 0.10790 C4 C 0.19720 0.36690 0.00140 N3 N 0.39530 0.34640 0.26580 C5 C 0.36270 0.36450 0.32980 C6 C 0.46280 0.30380 0.30380 N4 N 0.27810 0.52940 0.25140 C7 C 0.23800 0.50200 0.28720 C8 C 0.28580 0.48950 0.38880 C9 C 0.35770 0.52220 0.44940 C10 C 0.40850 0.50970 0.54250 C11 C 0.38740 0.46440 0.57500 C12 C 0.31550 0.43170 0.51440 C13 C 0.26470 0.44430 0.42130 C14 C 0.13810 0.47990 0.23150 C15 C 0.07290 0.48090 0.26520 C16 C -0.01980 0.46330 0.21070 C17 C -0.04740 0.44470 0.12230 C18 C 0.01780 0.44380 0.08860 C19 C 0.11050 0.46140 0.14310 N5 N 0.23940 0.53770 0.04270 C20 C 0.19520 0.51820 -0.03460 C21 C 0.08790 0.50930 -0.08620 C22 C 0.03400 0.54770 -0.07330 C23 C -0.06450 0.54220 -0.11190 C24 C -0.10900 0.49830 -0.16350 C25 C -0.05510 0.45990 -0.17640 C26 C 0.04340 0.46550 -0.13780 C27 C 0.24810 0.49790 -0.08980 C28 C 0.34080 0.47910 -0.03980 C29 C 0.38870 0.46040 -0.08570 C30 C 0.34390 0.46040 -0.18150 C31 C 0.25130 0.47920 -0.23150 C32 C 0.20340 0.49790 -0.18560 N6 N 0.45230 0.54600 0.21250 C33 C 0.53600 0.53350 0.24780 C34 C 0.59230 0.51570 0.34780 C35 C 0.54610 0.48520 0.38390 C36 C 0.59270 0.47140 0.47660 C37 C 0.68560 0.48810 0.53310 C38 C 0.73190 0.51870 0.49700 C39 C 0.68530 0.53240 0.40430 C40 C 0.59030 0.52510 0.19170 C41 C 0.56170 0.55340 0.11100 C42 C 0.60520 0.54490 0.05630 C43 C 0.67740 0.50820 0.08230 C44 C 0.70600 0.47990 0.16300 C45 C 0.66240 0.48840 0.21770 N7 N 0.15970 0.63860 0.12200 C46 C 0.08500 0.66660 0.09180 C47 C 0.09050 0.72560 0.08810 C48 C 0.15030 0.74720 0.05730 C49 C 0.15740 0.80080 0.05330 C50 C 0.10460 0.83270 0.08020 C51 C 0.04470 0.81110 0.11090 C52 C 0.03770 0.75750 0.11490 C53 C -0.01700 0.64810 0.05690 C54 C -0.09440 0.67190 -0.01620 C55 C -0.18560 0.65160 -0.04860 C56 C -0.19960 0.60740 -0.00810 C57 C -0.12220 0.58370 0.06500 C58 C -0.03100 0.60400 0.09740 N8 N 0.35290 0.65880 0.08830 C59 C 0.37080 0.68950 0.03790 C60 C 0.40570 0.66940 -0.02820 C61 C 0.36000 0.62620 -0.08160 C62 C 0.39280 0.60430 -0.13840 C63 C 0.47130 0.62540 -0.14190 C64 C 0.51710 0.66860 -0.08850 C65 C 0.48430 0.69050 -0.03170 C66 C 0.37490 0.74750 0.04510 C67 C 0.39930 0.77100 0.12940 C68 C 0.39710 0.82470 0.13540 C69 C 0.37040 0.85490 0.05710 C70 C 0.34600 0.83150 -0.02720 C71 C 0.34820 0.77780 -0.03320 N9 N 0.38740 0.64890 0.31100 C72 C 0.42100 0.68040 0.38050 C73 C 0.40800 0.73730 0.37360 C74 C 0.48340 0.77100 0.42280 C75 C 0.46910 0.82430 0.41180 C76 C 0.37930 0.84380 0.35160 C77 C 0.30380 0.81000 0.30230 C78 C 0.31820 0.75680 0.31330 C79 C 0.48040 0.65970 0.47780 C80 C 0.46640 0.68170 0.54740 C81 C 0.51810 0.66390 0.63750 C82 C 0.58380 0.62400 0.65800 C83 C 0.59780 0.60190 0.58840 C84 C 0.54610 0.61980 0.49830 Li6 Li 0.97320 0.73740 0.49540 O2 O 0.85880 0.73080 0.38250 P2 P 0.76360 0.73110 0.30360 N10 N 0.76260 0.70710 0.21240 C85 C 0.77300 0.73860 0.14450 C86 C 0.73930 0.65350 0.18270 N11 N 0.71800 0.78910 0.27930 C87 C 0.64120 0.80130 0.18780 C88 C 0.71930 0.82400 0.34920 N12 N 0.69610 0.69540 0.32990 C89 C 0.59690 0.68400 0.26510 C90 C 0.71860 0.68370 0.42450 O3 O 1.05910 0.68850 0.49640 P3 P 1.09050 0.63930 0.46580 N13 N 1.11500 0.65370 0.38410 C91 C 1.17880 0.62390 0.36150 C92 C 1.08030 0.70030 0.32810 N14 N 0.99600 0.60330 0.42570 C93 C 0.94810 0.58170 0.33310 C94 C 0.95700 0.58320 0.48340 N15 N 1.17890 0.60770 0.54570 C95 C 1.18520 0.55140 0.54680 C96 C 1.26980 0.63160 0.60800 O4 O 0.95220 0.72190 0.59290 P4 P 0.95910 0.72040 0.68520 N16 N 0.87730 0.68270 0.68440 C97 C 0.87240 0.62740 0.66570 C98 C 0.79990 0.70000 0.70120 N17 N 1.06320 0.69810 0.75780 C99 C 1.07800 0.67560 0.84460 C100 C 1.14340 0.68830 0.74060 N18 N 0.94790 0.77910 0.71560 C101 C 0.99520 0.79090 0.81370 C102 C 0.94200 0.82430 0.66030 O5 O 1.02780 0.79700 0.49570 P5 P 1.08200 0.84460 0.50240 N19 N 1.19850 0.83080 0.57600 C103 C 1.26530 0.86960 0.57670 C104 C 1.23180 0.80690 0.66610 N20 N 1.03400 0.87750 0.55710 C105 C 1.10110 0.88070 0.65510 C106 C 0.94310 0.90200 0.53480 N21 N 1.03720 0.86860 0.39140 C107 C 1.00440 0.82760 0.32240 C108 C 0.95830 0.89390 0.39690 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 O1 1.832 1_555 1_555 Li2 N4 2.074 1_555 1_555 Li3 N5 2.089 1_555 1_555 Li4 N4 1.999 1_555 1_555 Li5 N7 2.056 1_555 1_555 O1 P1 1.523 1_555 1_555 P1 N1 1.618 1_555 1_555 N1 C1 1.461 1_555 1_555 C2 N1 1.462 1_555 1_555 N2 P1 1.623 1_555 1_555 C3 N2 1.460 1_555 1_555 C4 N2 1.460 1_555 1_555 N3 P1 1.622 1_555 1_555 C5 N3 1.460 1_555 1_555 C6 N3 1.459 1_555 1_555 N4 Li1 2.110 1_555 1_555 C7 N4 1.274 1_555 1_555 C8 C7 1.514 1_555 1_555 C9 C8 1.395 1_555 1_555 C10 C9 1.395 1_555 1_555 C11 C10 1.396 1_555 1_555 C12 C11 1.395 1_555 1_555 C13 C8 1.394 1_555 1_555 C14 C7 1.525 1_555 1_555 C15 C14 1.395 1_555 1_555 C16 C15 1.394 1_555 1_555 C17 C16 1.397 1_555 1_555 C18 C17 1.395 1_555 1_555 C19 C14 1.396 1_555 1_555 N5 Li1 2.109 1_555 1_555 C20 N5 1.237 1_555 1_555 C21 C20 1.526 1_555 1_555 C22 C21 1.396 1_555 1_555 C23 C22 1.396 1_555 1_555 C24 C23 1.396 1_555 1_555 C25 C24 1.396 1_555 1_555 C26 C21 1.394 1_555 1_555 C27 C20 1.598 1_555 1_555 C28 C27 1.396 1_555 1_555 C29 C28 1.395 1_555 1_555 C30 C29 1.394 1_555 1_555 C31 C30 1.395 1_555 1_555 C32 C27 1.394 1_555 1_555 N6 Li1 2.072 1_555 1_555 C33 N6 1.221 1_555 1_555 C34 C33 1.531 1_555 1_555 C35 C34 1.393 1_555 1_555 C36 C35 1.395 1_555 1_555 C37 C36 1.394 1_555 1_555 C38 C37 1.396 1_555 1_555 C39 C34 1.395 1_555 1_555 C40 C33 1.556 1_555 1_555 C41 C40 1.395 1_555 1_555 C42 C41 1.395 1_555 1_555 C43 C42 1.395 1_555 1_555 C44 C43 1.395 1_555 1_555 C45 C40 1.394 1_555 1_555 N7 Li2 1.997 1_555 1_555 C46 N7 1.277 1_555 1_555 C47 C46 1.533 1_555 1_555 C48 C47 1.395 1_555 1_555 C49 C48 1.396 1_555 1_555 C50 C49 1.395 1_555 1_555 C51 C50 1.395 1_555 1_555 C52 C47 1.394 1_555 1_555 C53 C46 1.524 1_555 1_555 C54 C53 1.396 1_555 1_555 C55 C54 1.394 1_555 1_555 C56 C55 1.396 1_555 1_555 C57 C56 1.395 1_555 1_555 C58 C53 1.394 1_555 1_555 N8 Li3 2.057 1_555 1_555 C59 N8 1.278 1_555 1_555 C60 C59 1.534 1_555 1_555 C61 C60 1.397 1_555 1_555 C62 C61 1.394 1_555 1_555 C63 C62 1.393 1_555 1_555 C64 C63 1.397 1_555 1_555 C65 C60 1.395 1_555 1_555 C66 C59 1.505 1_555 1_555 C67 C66 1.396 1_555 1_555 C68 C67 1.395 1_555 1_555 C69 C68 1.394 1_555 1_555 C70 C69 1.395 1_555 1_555 C71 C66 1.396 1_555 1_555 N9 Li4 1.927 1_555 1_555 C72 N9 1.299 1_555 1_555 C73 C72 1.484 1_555 1_555 C74 C73 1.394 1_555 1_555 C75 C74 1.396 1_555 1_555 C76 C75 1.395 1_555 1_555 C77 C76 1.396 1_555 1_555 C78 C73 1.395 1_555 1_555 C79 C72 1.525 1_555 1_555 C80 C79 1.394 1_555 1_555 C81 C80 1.395 1_555 1_555 C82 C81 1.394 1_555 1_555 C83 C82 1.395 1_555 1_555 C84 C79 1.394 1_555 1_555 Li6 O2 1.901 1_555 1_555 O2 P2 1.459 1_555 1_555 P2 N10 1.624 1_555 1_555 N10 C85 1.459 1_555 1_555 C86 N10 1.460 1_555 1_555 N11 P2 1.633 1_555 1_555 C87 N11 1.460 1_555 1_555 C88 N11 1.459 1_555 1_555 N12 P2 1.628 1_555 1_555 C89 N12 1.460 1_555 1_555 C90 N12 1.461 1_555 1_555 O3 Li6 1.860 1_555 1_555 P3 O3 1.539 1_555 1_555 N13 P3 1.618 1_555 1_555 C91 N13 1.461 1_555 1_555 C92 N13 1.460 1_555 1_555 N14 P3 1.623 1_555 1_555 C93 N14 1.459 1_555 1_555 C94 N14 1.460 1_555 1_555 N15 P3 1.623 1_555 1_555 C95 N15 1.460 1_555 1_555 C96 N15 1.460 1_555 1_555 O4 Li6 1.840 1_555 1_555 P4 O4 1.477 1_555 1_555 N16 P4 1.625 1_555 1_555 C97 N16 1.459 1_555 1_555 C98 N16 1.460 1_555 1_555 N17 P4 1.625 1_555 1_555 C99 N17 1.460 1_555 1_555 C100 N17 1.460 1_555 1_555 N18 P4 1.637 1_555 1_555 C101 N18 1.460 1_555 1_555 C102 N18 1.460 1_555 1_555 O5 Li6 1.771 1_555 1_555 P5 O5 1.479 1_555 1_555 N19 P5 1.708 1_555 1_555 C103 N19 1.461 1_555 1_555 C104 N19 1.460 1_555 1_555 N20 P5 1.670 1_555 1_555 C105 N20 1.460 1_555 1_555 C106 N20 1.462 1_555 1_555 N21 P5 1.737 1_555 1_555 C107 N21 1.461 1_555 1_555 C108 N21 1.460 1_555 1_555 Li2 N5 1.978 1_555 1_555 Li3 N6 1.934 1_555 1_555 Li4 N6 2.115 1_555 1_555 Li5 N8 2.042 1_555 1_555 Li5 N9 2.033 1_555 1_555 C12 C13 1.396 1_555 1_555 C18 C19 1.394 1_555 1_555 C25 C26 1.396 1_555 1_555 C31 C32 1.395 1_555 1_555 C38 C39 1.395 1_555 1_555 C44 C45 1.396 1_555 1_555 C51 C52 1.396 1_555 1_555 C57 C58 1.394 1_555 1_555 C64 C65 1.394 1_555 1_555 C70 C71 1.395 1_555 1_555 C77 C78 1.394 1_555 1_555 C83 C84 1.395 1_555 1_555 #END data_CSD_CIF_COHZAA _audit_creation_date 2000-05-02 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD COHZAA _database_code_depnum_ccdc_archive 'CCDC 1128897' _chemical_formula_sum 'C19 H46 Li2 N7 Na1' _chemical_formula_moiety ; C19 H46 Li2 N7 1+,Na1 1- ; _journal_coden_Cambridge 511 _journal_volume 65 _journal_year 1993 _journal_page_first 435 _journal_name_full 'Pure Appl.Chem. ' loop_ _publ_author_name "J.L.Dye" "R.H.Huang" _chemical_name_systematic ; (\m~2~-Methylamido)-bis((1,4,7-trimethyl-1,4,7-triazacyclononane)-lithium) sodide ; _cell_volume 6033.466 _exptl_special_details ; Pbca polymorph Also crystallizes in P212121 with the same molecular structure ; _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.047 _refine_ls_wR_factor_gt 0.047 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,1/2+y,1/2-z 5 -x,-y,-z 6 -1/2+x,y,-1/2-z 7 -1/2-x,-1/2+y,z 8 x,-1/2-y,-1/2+z _cell_length_a 14.9975(53) _cell_length_b 17.7177(42) _cell_length_c 22.7060(72) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 Li 1.13 N 0.68 Na 0.97 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 0.1963(2) 0.8924(1) 0.0924(1) N1 N 0.5274(2) 1.3583(2) -0.1636(1) N2 N 0.5419(3) 1.2288(2) -0.2390(2) N3 N 0.4363(2) 1.3560(2) -0.2745(2) N4 N 0.2168(3) 1.1501(2) -0.0402(2) N5 N 0.2890(2) 1.0580(2) -0.1330(2) N6 N 0.4029(3) 1.1179(2) -0.0448(2) N7 N 0.3212(2) 1.2501(2) -0.1630(2) C1 C 0.6063(3) 1.3085(3) -0.1594(2) C2 C 0.6235(3) 1.2656(3) -0.2162(2) C3 C 0.5257(3) 1.2430(3) -0.3017(2) C4 C 0.5062(4) 1.3254(3) -0.3142(2) C5 C 0.4614(3) 1.4279(3) -0.2470(2) C6 C 0.5397(4) 1.4205(3) -0.2065(2) C7 C 0.5039(4) 1.3862(3) -0.1049(2) C8 C 0.5441(4) 1.1471(3) -0.2283(2) C9 C 0.3505(3) 1.3625(3) -0.3047(2) C10 C 0.1748(4) 1.0781(3) -0.0550(3) C11 C 0.1958(4) 1.0502(3) -0.1129(2) C12 C 0.3515(4) 1.0097(3) -0.1026(2) C13 C 0.4248(4) 1.0458(3) -0.0744(3) C14 C 0.3540(4) 1.1060(4) 0.0095(2) C15 C 0.2708(4) 1.1463(3) 0.0138(2) C16 C 0.1498(4) 1.2099(3) -0.0346(2) C17 C 0.2921(4) 1.0484(3) -0.1970(2) C18 C 0.4854(4) 1.1600(3) -0.0358(2) C19 C 0.2760(3) 1.3187(3) -0.1439(2) Li1 Li 0.3144(6) 1.1686(4) -0.1051(3) Li2 Li 0.4317(6) 1.2856(4) -0.1995(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 N1 C1 1.479 1_555 1_555 N2 C2 1.480 1_555 1_555 N3 C4 1.485 1_555 1_555 N4 C10 1.462 1_555 1_555 N5 C11 1.477 1_555 1_555 N6 C13 1.480 1_555 1_555 N7 C19 1.458 1_555 1_555 C1 C2 1.519 1_555 1_555 C3 N2 1.466 1_555 1_555 C4 C3 1.516 1_555 1_555 C5 N3 1.468 1_555 1_555 C6 N1 1.482 1_555 1_555 C7 N1 1.465 1_555 1_555 C8 N2 1.468 1_555 1_555 C9 N3 1.463 1_555 1_555 C10 C11 1.439 1_555 1_555 C12 N5 1.445 1_555 1_555 C13 C12 1.424 1_555 1_555 C14 N6 1.450 1_555 1_555 C15 N4 1.471 1_555 1_555 C16 N4 1.466 1_555 1_555 C17 N5 1.464 1_555 1_555 C18 N6 1.459 1_555 1_555 Li1 N4 2.103 1_555 1_555 Li2 N1 2.094 1_555 1_555 N2 Li2 2.133 1_555 1_555 N3 Li2 2.112 1_555 1_555 N5 Li1 2.094 1_555 1_555 N6 Li1 2.108 1_555 1_555 N7 Li1 1.955 1_555 1_555 N7 Li2 1.957 1_555 1_555 C5 C6 1.497 1_555 1_555 C14 C15 1.441 1_555 1_555 #END data_CSD_CIF_COJDIO _audit_creation_date 2000-05-02 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD COJDIO _database_code_depnum_ccdc_archive 'CCDC 1128930' _chemical_formula_sum 'C14 H34 Li1 N2 Na1 O6' _chemical_formula_moiety ; C14 H34 Li1 N2 O6 1+,Na1 1- ; _journal_coden_Cambridge 511 _journal_volume 65 _journal_year 1993 _journal_page_first 435 _journal_name_full 'Pure Appl.Chem. ' loop_ _publ_author_name "J.L.Dye" "R.H.Huang" _chemical_name_systematic ; (18-Crown-6)-bis(methylamine)-lithium sodide ; _cell_volume 2484.913 _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.04 _refine_ls_wR_factor_gt 0.04 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,-1/2-y,-1/2+z _cell_length_a 13.8772(53) _cell_length_b 12.4072(40) _cell_length_c 15.7071(67) _cell_angle_alpha 90 _cell_angle_beta 113.243(27) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.13 N 0.68 Na 0.97 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 0.29682(9) 0.19044(8) 0.35369(7) O1 O 0.7614(1) 0.0495(1) 0.9746(1) O2 O 0.9542(1) 0.1611(1) 1.0173(1) O3 O 0.9460(1) 0.3643(1) 0.9291(1) O4 O 0.7931(1) 0.3956(1) 0.7477(1) O5 O 0.6125(1) 0.2768(1) 0.6913(1) O6 O 0.6154(1) 0.0886(1) 0.7904(1) N1 N 0.8380(2) 0.1341(2) 0.8017(2) N2 N 0.7215(2) 0.2944(2) 0.9188(2) C1 C 0.8616(2) 0.0072(2) 1.0315(2) C2 C 0.9311(2) 0.0972(2) 1.0821(2) C3 C 1.0210(2) 0.2490(2) 1.0596(2) C4 C 1.0402(2) 0.3122(2) 0.9871(2) C5 C 0.9618(2) 0.4336(2) 0.8634(2) C6 C 0.8585(2) 0.4799(2) 0.8019(2) C7 C 0.6973(2) 0.4362(2) 0.6793(2) C8 C 0.6352(2) 0.3435(2) 0.6276(2) C9 C 0.5519(2) 0.1836(3) 0.6485(2) C10 C 0.5221(2) 0.1259(3) 0.7176(2) C11 C 0.5945(2) 0.0193(3) 0.8536(2) C12 C 0.6938(2) -0.0305(2) 0.9172(2) C13 C 0.8999(2) 0.1395(2) 0.7460(2) C14 C 0.6908(5) 0.3838(4) 0.9496(4) Li1 Li 0.7461(4) 0.2575(5) 0.8082(3) H1 H 0.853(2) -0.044(2) 1.076(2) H2 H 0.887(2) -0.031(2) 0.990(2) H3 H 0.994(2) 0.072(2) 1.127(2) H4 H 0.894(2) 0.141(2) 1.113(1) H5 H 0.986(2) 0.294(2) 1.092(2) H6 H 1.090(2) 0.225(2) 1.109(2) H7 H 1.066(2) 0.265(2) 0.947(1) H8 H 1.094(2) 0.365(2) 1.016(1) H9 H 1.013(2) 0.492(2) 0.898(1) H10 H 0.995(1) 0.392(1) 0.826(1) H11 H 0.870(2) 0.539(2) 0.761(2) H12 H 0.822(2) 0.515(2) 0.839(1) H13 H 0.661(2) 0.476(2) 0.712(1) H14 H 0.713(2) 0.487(2) 0.638(2) H15 H 0.672(2) 0.298(2) 0.597(1) H16 H 0.568(2) 0.363(2) 0.578(2) H17 H 0.487(2) 0.208(2) 0.593(2) H18 H 0.595(2) 0.134(2) 0.624(2) H19 H 0.483(2) 0.067(2) 0.690(2) H20 H 0.484(2) 0.178(2) 0.748(2) H21 H 0.563(2) 0.063(2) 0.888(2) H22 H 0.546(2) -0.039(2) 0.817(2) H23 H 0.730(2) -0.067(2) 0.882(2) H24 H 0.678(2) -0.084(2) 0.958(2) H25 H 0.932(2) 0.073(2) 0.744(2) H26 H 0.854(2) 0.156(2) 0.686(2) H27 H 0.952(2) 0.201(3) 0.771(2) H28 H 0.872(2) 0.123(2) 0.856(2) H29 H 0.799(2) 0.079(2) 0.784(2) H30 H 0.780(4) 0.337(4) 0.955(4) H31 H 0.730(2) 0.238(2) 0.949(2) H32 H 0.681(2) 0.440(3) 0.913(2) H33 H 0.618(2) 0.317(3) 0.906(2) H34 H 0.675(3) 0.390(3) 0.998(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 O1 C1 1.424 1_555 1_555 O2 C2 1.423 1_555 1_555 O3 C4 1.420 1_555 1_555 O4 C6 1.426 1_555 1_555 O5 C8 1.426 1_555 1_555 O6 C10 1.425 1_555 1_555 N1 C13 1.449 1_555 1_555 N2 C14 1.345 1_555 1_555 C1 C2 1.485 1_555 1_555 C2 H3 0.933 1_555 1_555 C3 O2 1.416 1_555 1_555 C4 C3 1.491 1_555 1_555 C5 O3 1.425 1_555 1_555 C6 C5 1.492 1_555 1_555 C7 O4 1.431 1_555 1_555 C8 C7 1.474 1_555 1_555 C9 O5 1.432 1_555 1_555 C10 C9 1.489 1_555 1_555 C11 O6 1.427 1_555 1_555 C12 O1 1.418 1_555 1_555 C13 H25 0.944 1_555 1_555 C14 H32 0.879 1_555 1_555 Li1 O4 2.180 1_555 1_555 H1 C1 0.986 1_555 1_555 H2 C1 0.977 1_555 1_555 H4 C2 0.997 1_555 1_555 H5 C3 1.001 1_555 1_555 H6 C3 1.011 1_555 1_555 H7 C4 1.023 1_555 1_555 H8 C4 0.962 1_555 1_555 H9 C5 1.010 1_555 1_555 H10 C5 1.019 1_555 1_555 H11 C6 1.028 1_555 1_555 H12 C6 1.009 1_555 1_555 H13 C7 0.983 1_555 1_555 H14 C7 0.988 1_555 1_555 H15 C8 1.002 1_555 1_555 H16 C8 0.981 1_555 1_555 H17 C9 1.021 1_555 1_555 H18 C9 1.033 1_555 1_555 H19 C10 0.911 1_555 1_555 H20 C10 1.060 1_555 1_555 H21 C11 0.982 1_555 1_555 H22 C11 1.001 1_555 1_555 H23 C12 0.991 1_555 1_555 H24 C12 1.005 1_555 1_555 H26 C13 0.928 1_555 1_555 H27 C13 1.017 1_555 1_555 H28 N1 0.807 1_555 1_555 H29 N1 0.848 1_555 1_555 H30 N2 0.947 1_555 1_555 H31 N2 0.827 1_555 1_555 H33 C14 1.277 1_555 1_555 H34 C14 0.874 1_555 1_555 O5 Li1 2.044 1_555 1_555 N1 Li1 2.021 1_555 1_555 N2 Li1 1.952 1_555 1_555 C11 C12 1.481 1_555 1_555 #END data_CSD_CIF_COJFAI _audit_creation_date 2000-05-02 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD COJFAI _database_code_depnum_ccdc_archive 'CCDC 1128933' _chemical_formula_sum 'C50 H106 Li1 N2 Na1 O24' _chemical_formula_moiety ; 4(C12 H24 O6),C2 H10 Li1 N2 1+,Na1 1- ; _journal_coden_Cambridge 511 _journal_volume 65 _journal_year 1993 _journal_page_first 435 _journal_name_full 'Pure Appl.Chem. ' loop_ _publ_author_name "J.L.Dye" "R.H.Huang" _chemical_name_systematic ; tetrakis(18-Crown-6) bis(methylamine)-lithium sodide ; _cell_volume 1641.783 _exptl_special_details ; Values for cell parameters b, c, beta and gamma are published ; _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; _refine_special_details ; Structure may be disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.048 _refine_ls_wR_factor_gt 0.048 _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R -3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 z,x,y 3 y,z,x 4 -x,-y,-z 5 -z,-x,-y 6 -y,-z,-x _cell_length_a 11.9817(66) _cell_length_b 11.9817(66) _cell_length_c 11.9817(66) _cell_angle_alpha 99.413(33) _cell_angle_beta 99.413(33) _cell_angle_gamma 99.413(33) _cell_formula_units_Z 1 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 0.68 N 0.68 Na 0.97 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 0.50000 0.50000 0.50000 O1 O 0.1706(1) -0.1290(1) -0.0081(1) C1 C 0.1401(2) -0.2398(2) 0.0189(2) C2 C 0.2240(2) -0.1342(2) -0.1059(2) H1 H 0.074(2) -0.288(2) -0.043(2) H2 H 0.209(2) -0.277(2) 0.021(2) H3 H 0.297(2) -0.156(2) -0.088(2) H4 H 0.171(2) -0.194(2) -0.168(2) O2 O 0.4586(1) 0.1544(1) 0.1149(1) O3 O 0.4922(1) -0.0712(1) 0.2721(1) O4 O 0.4693(1) -0.2538(1) 0.0613(1) C3 C 0.4868(2) 0.1082(2) 0.2152(2) C4 C 0.4522(2) -0.0203(2) 0.1777(2) C5 C 0.4503(2) -0.1914(2) 0.2552(2) C6 C 0.5069(2) -0.2643(2) 0.1764(2) C7 C 0.5290(2) -0.3101(2) -0.0169(2) C8 C 0.5011(2) 0.2748(2) 0.1306(2) H5 H 0.572(2) 0.131(2) 0.251(2) H6 H 0.448(2) 0.139(2) 0.274(2) H7 H 0.480(2) -0.045(2) 0.110(2) H8 H 0.367(2) -0.046(2) 0.152(2) H9 H 0.466(2) -0.212(2) 0.329(2) H10 H 0.368(2) -0.209(2) 0.227(2) H11 H 0.486(2) -0.344(2) 0.182(2) H12 H 0.593(2) -0.238(2) 0.200(2) H13 H 0.615(2) -0.287(2) 0.014(2) H14 H 0.504(2) -0.391(2) -0.028(2) H15 H 0.587(2) 0.295(2) 0.162(2) H16 H 0.468(2) 0.318(2) 0.187(2) N1 N 0.1020(3) 0.10200 0.10200 C9 C 0.1801(4) 0.18000 0.18000 Li1 Li 0.00000 0.00000 0.00000 H17 H 0.25800 0.17500 0.17500 H18? H 0.16600 0.10900 0.16600 H19? H 0.17000 0.17000 0.10000 C2D C 0.1059(2) -0.2240(2) 0.1342(2) O1D O 0.0081(1) -0.1706(1) 0.1290(1) C1D C -0.0189(2) -0.1401(2) 0.2398(2) C2B C -0.1342(2) -0.1059(2) 0.2240(2) O1B O -0.1290(1) -0.0081(1) 0.1706(1) C1B C -0.2398(2) 0.0189(2) 0.1401(2) C2C C -0.2240(2) 0.1342(2) 0.1059(2) O1C O -0.1706(1) 0.1290(1) 0.0081(1) C1C C -0.1401(2) 0.2398(2) -0.0189(2) C2A C -0.1059(2) 0.2240(2) -0.1342(2) O1A O -0.0081(1) 0.1706(1) -0.1290(1) C1A C 0.0189(2) 0.1401(2) -0.2398(2) C2E C 0.1342(2) 0.1059(2) -0.2240(2) O1E O 0.1290(1) 0.0081(1) -0.1706(1) C1E C 0.2398(2) -0.0189(2) -0.1401(2) H1E H 0.288(2) 0.043(2) -0.074(2) H2E H 0.277(2) -0.021(2) -0.209(2) H3E H 0.156(2) 0.088(2) -0.297(2) H4E H 0.194(2) 0.168(2) -0.171(2) H1A H -0.043(2) 0.074(2) -0.288(2) H2A H 0.021(2) 0.209(2) -0.277(2) H3A H -0.088(2) 0.297(2) -0.156(2) H4A H -0.168(2) 0.171(2) -0.194(2) H1C H -0.074(2) 0.288(2) 0.043(2) H2C H -0.209(2) 0.277(2) -0.021(2) H3C H -0.297(2) 0.156(2) 0.088(2) H4C H -0.171(2) 0.194(2) 0.168(2) H1B H -0.288(2) -0.043(2) 0.074(2) H2B H -0.277(2) 0.021(2) 0.209(2) H3B H -0.156(2) -0.088(2) 0.297(2) H4B H -0.194(2) -0.168(2) 0.171(2) H1D H 0.043(2) -0.074(2) 0.288(2) H2D H -0.021(2) -0.209(2) 0.277(2) H3D H 0.088(2) -0.297(2) 0.156(2) H4D H 0.168(2) -0.171(2) 0.194(2) C8C C 0.4989(2) -0.2748(2) -0.1306(2) O2C O 0.5414(1) -0.1544(1) -0.1149(1) C3C C 0.5132(2) -0.1082(2) -0.2152(2) C4C C 0.5478(2) 0.0203(2) -0.1777(2) O3C O 0.5078(1) 0.0712(1) -0.2721(1) C5C C 0.5497(2) 0.1914(2) -0.2552(2) C6C C 0.4931(2) 0.2643(2) -0.1764(2) O4C O 0.5307(1) 0.2538(1) -0.0613(1) C7C C 0.4710(2) 0.3101(2) 0.0169(2) H13C H 0.385(2) 0.287(2) -0.014(2) H14C H 0.496(2) 0.391(2) 0.028(2) H11C H 0.514(2) 0.344(2) -0.182(2) H12C H 0.407(2) 0.238(2) -0.200(2) H9C H 0.534(2) 0.212(2) -0.329(2) H10C H 0.632(2) 0.209(2) -0.227(2) H7C H 0.520(2) 0.045(2) -0.110(2) H8C H 0.633(2) 0.046(2) -0.152(2) H5C H 0.428(2) -0.131(2) -0.251(2) H6C H 0.552(2) -0.139(2) -0.274(2) H15C H 0.413(2) -0.295(2) -0.162(2) H16C H 0.532(2) -0.318(2) -0.187(2) H17A H 0.17500 0.25800 0.17500 H17B H 0.17500 0.17500 0.25800 N1C N -0.1020(3) -0.10200 -0.10200 C9C C -0.1801(4) -0.18000 -0.18000 H17C H -0.25800 -0.17500 -0.17500 H17D H -0.17500 -0.25800 -0.17500 H17E H -0.17500 -0.17500 -0.25800 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 O1 C1 1.422 1_555 1_555 C1 H1 1.014 1_555 1_555 C2 O1 1.422 1_555 1_555 H2 C1 0.999 1_555 1_555 H3 C2 0.954 1_555 1_555 H4 C2 0.996 1_555 1_555 O2 C3 1.418 1_555 1_555 O3 C4 1.423 1_555 1_555 O4 C6 1.412 1_555 1_555 C3 C4 1.499 1_555 1_555 C4 H7 0.948 1_555 1_555 C5 O3 1.415 1_555 1_555 C6 C5 1.499 1_555 1_555 C7 O4 1.419 1_555 1_555 C8 O2 1.420 1_555 1_555 H5 C3 1.014 1_555 1_555 H6 C3 0.963 1_555 1_555 H8 C4 0.998 1_555 1_555 H9 C5 0.954 1_555 1_555 H10 C5 0.965 1_555 1_555 H11 C6 0.963 1_555 1_555 H12 C6 1.006 1_555 1_555 H13 C7 1.012 1_555 1_555 H14 C7 0.947 1_555 1_555 H15 C8 1.011 1_555 1_555 H16 C8 0.960 1_555 1_555 N1 C9 1.328 1_555 1_555 C9 H17 0.956 1_555 1_555 Li1 N1 1.736 1_555 1_555 C2D C1 1.496 1_555 1_555 O1D C2D 1.422 1_555 1_555 C1D O1D 1.422 1_555 1_555 C2B C1D 1.496 1_555 1_555 O1B C2B 1.422 1_555 1_555 C1B O1B 1.422 1_555 1_555 C2C C1B 1.496 1_555 1_555 O1C C2C 1.422 1_555 1_555 C1C O1C 1.422 1_555 1_555 C2A C1C 1.496 1_555 1_555 O1A C2A 1.422 1_555 1_555 C1A O1A 1.422 1_555 1_555 C2E C1A 1.496 1_555 1_555 O1E C2E 1.422 1_555 1_555 C1E C2 1.496 1_555 1_555 H1E C1E 1.014 1_555 1_555 H2E C1E 0.999 1_555 1_555 H3E C2E 0.954 1_555 1_555 H4E C2E 0.996 1_555 1_555 H1A C1A 1.014 1_555 1_555 H2A C1A 0.999 1_555 1_555 H3A C2A 0.954 1_555 1_555 H4A C2A 0.996 1_555 1_555 H1C C1C 1.014 1_555 1_555 H2C C1C 0.999 1_555 1_555 H3C C2C 0.954 1_555 1_555 H4C C2C 0.996 1_555 1_555 H1B C1B 1.014 1_555 1_555 H2B C1B 0.999 1_555 1_555 H3B C2B 0.954 1_555 1_555 H4B C2B 0.996 1_555 1_555 H1D C1D 1.014 1_555 1_555 H2D C1D 0.999 1_555 1_555 H3D C2D 0.954 1_555 1_555 H4D C2D 0.996 1_555 1_555 C8C C7 1.498 1_555 1_555 O2C C8C 1.420 1_555 1_555 C3C O2C 1.418 1_555 1_555 C4C C3C 1.499 1_555 1_555 O3C C4C 1.423 1_555 1_555 C5C O3C 1.415 1_555 1_555 C6C C5C 1.499 1_555 1_555 O4C C6C 1.412 1_555 1_555 C7C C8 1.498 1_555 1_555 H13C C7C 1.012 1_555 1_555 H14C C7C 0.947 1_555 1_555 H11C C6C 0.963 1_555 1_555 H12C C6C 1.006 1_555 1_555 H9C C5C 0.954 1_555 1_555 H10C C5C 0.965 1_555 1_555 H7C C4C 0.948 1_555 1_555 H8C C4C 0.998 1_555 1_555 H5C C3C 1.014 1_555 1_555 H6C C3C 0.963 1_555 1_555 H15C C8C 1.011 1_555 1_555 H16C C8C 0.960 1_555 1_555 H17A C9 0.957 1_555 1_555 H17B C9 0.957 1_555 1_555 N1C Li1 1.736 1_555 1_555 C9C N1C 1.328 1_555 1_555 H17C C9C 0.956 1_555 1_555 H17D C9C 0.957 1_555 1_555 H17E C9C 0.957 1_555 1_555 O1E C1E 1.422 1_555 1_555 O4C C7C 1.419 1_555 1_555 #END data_CSD_CIF_CRYPNA10 _audit_creation_date 1975-04-17 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD CRYPNA10 _chemical_formula_sum 'C18 H36 N2 Na2 O6' _chemical_formula_moiety ; C18 H36 N2 Na1 O6 1+,Na1 1- ; _journal_coden_Cambridge 4 _journal_volume 96 _journal_year 1974 _journal_page_first 7203 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "F.J.Tehan" "B.L.Barnett" "J.L.Dye" _chemical_name_systematic ; Sodium (2,2,2)-crypt-sodium ; _cell_volume 1975.724 _exptl_crystal_density_diffrn 1.064 _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.094 _refine_ls_wR_factor_gt 0.094 _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R 3 2' _symmetry_Int_Tables_number 155 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/3+x,2/3+y,2/3+z 3 2/3+x,1/3+y,1/3+z 4 -y,x-y,z 5 -x+y,-x,z 6 1/3-y,2/3+x-y,2/3+z 7 1/3-x+y,2/3-x,2/3+z 8 2/3-y,1/3+x-y,1/3+z 9 2/3-x+y,1/3-x,1/3+z 10 y,x,-z 11 2/3+y,1/3+x,1/3-z 12 1/3+y,2/3+x,2/3-z 13 x-y,-y,-z 14 -x,-x+y,-z 15 2/3+x-y,1/3-y,1/3-z 16 2/3-x,1/3-x+y,1/3-z 17 1/3+x-y,2/3-y,2/3-z 18 1/3-x,2/3-x+y,2/3-z _cell_length_a 8.83(1) _cell_length_b 8.83(1) _cell_length_c 29.26(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 N 0.68 Na 1.68 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z C1 C 0.18400 0.09000 0.10760 C2 C 0.32100 0.18200 0.08290 C3 C 0.39100 0.35000 0.01970 Na1 Na 0.00000 0.00000 0.00000 Na2 Na 0.33333 -0.33333 0.16667 N1 N 0.00000 0.00000 0.09280 O1 O 0.30800 0.17600 0.03470 C1C C -0.09000 0.09400 0.10760 C1D C -0.09400 -0.18400 0.10760 N1I N 0.00000 0.00000 -0.09280 O1C O -0.17600 0.13200 0.03470 O1D O -0.13200 -0.30800 0.03470 O1I O 0.17600 0.30800 -0.03470 O1L O 0.13200 -0.17600 -0.03470 O1M O -0.30800 -0.13200 -0.03470 C3I C 0.35000 0.39100 -0.01970 C2C C -0.18200 0.13900 0.08290 C2D C -0.13900 -0.32100 0.08290 C1I C 0.09000 0.18400 -0.10760 C1L C 0.09400 -0.09000 -0.10760 C1M C -0.18400 -0.09400 -0.10760 C3C C -0.35000 0.04100 0.01970 C3D C -0.04100 -0.39100 0.01970 C2I C 0.18200 0.32100 -0.08290 C2L C 0.13900 -0.18200 -0.08290 C3L C 0.04100 -0.35000 -0.01970 C2M C -0.32100 -0.13900 -0.08290 C3M C -0.39100 -0.04100 -0.01970 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 C1 C2 1.290 1_555 1_555 C2 O1 1.414 1_555 1_555 C3 O1 1.402 1_555 1_555 Na1 N1 2.715 1_555 1_555 N1 C1 1.472 1_555 1_555 O1 Na1 2.572 1_555 1_555 C1C N1 1.472 1_555 1_555 C1D N1 1.472 1_555 1_555 N1I Na1 2.715 1_555 1_555 O1C Na1 2.572 1_555 1_555 O1D Na1 2.572 1_555 1_555 O1I Na1 2.572 1_555 1_555 O1L Na1 2.572 1_555 1_555 O1M Na1 2.572 1_555 1_555 C3I C3 1.312 1_555 1_555 C2C C1C 1.290 1_555 1_555 C2D C1D 1.290 1_555 1_555 C1I N1I 1.472 1_555 1_555 C1L N1I 1.472 1_555 1_555 C1M N1I 1.472 1_555 1_555 C3C O1C 1.402 1_555 1_555 C3D O1D 1.402 1_555 1_555 C2I O1I 1.414 1_555 1_555 C2L O1L 1.414 1_555 1_555 C3L O1L 1.402 1_555 1_555 C2M O1M 1.414 1_555 1_555 C3M O1M 1.402 1_555 1_555 O1C C2C 1.414 1_555 1_555 O1D C2D 1.414 1_555 1_555 O1I C3I 1.402 1_555 1_555 C1I C2I 1.290 1_555 1_555 C1L C2L 1.290 1_555 1_555 C1M C2M 1.290 1_555 1_555 C3C C3M 1.312 1_555 1_555 C3D C3L 1.312 1_555 1_555 #END data_CSD_CIF_CURWUH _audit_creation_date 1986-02-24 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD CURWUH _chemical_formula_sum 'C112 H160 Ag6 Br4 Li10 O10' _chemical_formula_moiety ; 2(C36 H30 Ag3 Li2 1-),C40 H100 Br4 Li6 O10 2+ ; _journal_coden_Cambridge 4 _journal_volume 107 _journal_year 1985 _journal_page_first 1679 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "M.Y.Chiang" "E.Bohlen" "R.Bau" _chemical_name_systematic ; bis(hexakis(\m~2~-Phenyl)-di-lithium-tri-silver) bis(\m~4~-bromo)-bis(\m~3~-bromo)-decakis(diethyl ether)-hexa-lithium ; _cell_volume 6171.278 _exptl_crystal_colour 'colorless' _exptl_special_details ; Average bond lengths only are reported ; _diffrn_ambient_temperature 171.15 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.07 _refine_ls_wR_factor_gt 0.07 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 -1/2+x,-1/2-y,-1/2+z _cell_length_a 16.466(9) _cell_length_b 29.700(15) _cell_length_c 12.821(5) _cell_angle_alpha 90 _cell_angle_beta 100.18(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.72 Ag 1.48 Br 1.21 Li 1.22 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Ag1 Ag 0.05713(9) 0.36901(5) 0.91497(10) Ag2 Ag -0.05188(10) 0.26968(5) 0.88447(10) Ag3 Ag -0.14581(9) 0.37169(5) 0.80879(10) Br1 Br 0.41197(14) 0.45948(7) 0.52436(17) Br2 Br 0.47578(18) 0.46669(9) 0.24695(19) Li1 Li -0.0759(20) 0.3406(11) 1.0086(23) Li2 Li -0.0166(20) 0.3289(11) 0.7340(23) C1 C 0.1146(11) 0.3362(6) 0.8004(13) C2 C 0.1545(12) 0.2948(6) 0.8313(13) C3 C 0.1232(12) 0.3534(6) 0.7006(14) C4 C 0.2077(13) 0.2742(7) 0.7674(15) C5 C 0.1732(13) 0.3302(7) 0.6358(15) C6 C 0.2162(13) 0.2925(7) 0.6732(15) C7 C 0.0103(12) 0.4033(7) 1.0385(14) C8 C 0.0219(11) 0.3854(6) 1.1439(13) C9 C -0.0290(12) 0.4446(6) 1.0204(14) C10 C -0.0606(13) 0.4686(7) 1.1029(15) C11 C -0.0118(13) 0.4081(7) 1.2219(15) C12 C -0.0501(13) 0.4480(7) 1.2049(15) C13 C -0.0266(12) 0.2732(6) 1.0534(13) C14 C -0.0891(12) 0.2757(6) 1.1180(14) C15 C 0.0555(13) 0.2656(6) 1.1032(14) C16 C -0.0643(13) 0.2775(7) 1.2306(14) C17 C 0.0778(13) 0.2646(7) 1.2182(14) C18 C 0.0154(14) 0.2717(7) 1.2743(16) C19 C -0.0787(11) 0.2602(6) 0.7172(12) C20 C -0.0200(12) 0.2440(6) 0.6576(14) C21 C -0.1612(12) 0.2643(6) 0.6630(13) C22 C -0.0423(13) 0.2314(7) 0.5550(14) C23 C -0.1840(12) 0.2497(7) 0.5574(14) C24 C -0.1233(13) 0.2333(7) 0.5019(14) C25 C -0.0915(11) 0.3920(6) 0.6799(12) C26 C -0.0404(11) 0.4312(6) 0.6885(13) C27 C -0.1085(11) 0.3726(6) 0.5777(13) C28 C -0.0104(12) 0.4516(6) 0.6010(13) C29 C -0.0747(12) 0.3898(7) 0.4936(14) C30 C -0.0290(12) 0.4300(7) 0.5038(14) C31 C -0.2123(12) 0.3519(7) 0.9295(14) C32 C -0.2138(12) 0.3765(7) 1.0217(14) C33 C -0.2611(11) 0.3129(6) 0.9083(12) C34 C -0.2645(13) 0.3614(7) 1.0989(14) C35 C -0.3129(13) 0.3007(7) 0.9819(15) C36 C -0.3146(13) 0.3238(7) 1.0749(15) Li3 Li 0.3496(21) 0.4415(11) 0.3278(24) Li4 Li 0.4504(29) 0.4543(15) 0.7327(33) Li5 Li 0.5385(27) 0.4591(15) 0.4339(31) C37 C 0.2831(19) 0.3158(10) 0.3884(22) C38 C 0.3561(16) 0.3440(8) 0.3864(18) O1 O 0.3394(8) 0.3779(4) 0.3025(10) C39 C 0.3355(15) 0.3620(8) 0.1908(17) C40 C 0.2444(15) 0.3602(8) 0.1347(17) C41 C 0.1853(21) 0.4333(12) 0.4126(26) C42 C 0.1768(23) 0.4683(12) 0.3389(27) O2 O 0.2418(15) 0.4740(8) 0.2819(18) C43 C 0.2345(37) 0.5058(23) 0.2004(50) C44 C 0.2460(27) 0.4972(14) 0.1011(32) C45 C 0.5265(26) 0.4177(14) 0.9946(32) C46 C 0.5628(18) 0.4107(10) 0.9017(22) O3 O 0.5089(10) 0.4080(6) 0.8006(13) C47 C 0.5095(36) 0.3572(20) 0.7673(44) C48 C 0.4545(25) 0.3478(13) 0.684(3) C49 C 0.2397(25) 0.5237(14) 0.6605(30) C50 C 0.2908(28) 0.5138(15) 0.7931(33) O4 O 0.3422(12) 0.4664(7) 0.7811(14) C51 C 0.2858(26) 0.4284(15) 0.7686(31) C52 C 0.3068(25) 0.3995(14) 0.8679(31) C53 C 0.6291(34) 0.3511(17) 0.3602(39) C54 C 0.5713(31) 0.3581(17) 0.4041(38) O5 O 0.6075(13) 0.4056(7) 0.4629(15) C55 C 0.6839(44) 0.4122(25) 0.5446(55) C56 C 0.6603(43) 0.4023(24) 0.6256(53) Li5B Li 0.4615(27) 0.5409(15) 0.5661(31) Li4B Li 0.5496(29) 0.5457(15) 0.2673(33) Br2B Br 0.52422(18) 0.53331(9) 0.75305(19) Br1B Br 0.58803(14) 0.54052(7) 0.47564(17) O5B O 0.3925(13) 0.5944(7) 0.5371(15) O3B O 0.4911(10) 0.5920(6) 0.1994(13) O4B O 0.6578(12) 0.5336(7) 0.2189(14) Li3B Li 0.6504(21) 0.5585(11) 0.6722(24) C54B C 0.4287(31) 0.6419(17) 0.5959(38) C55B C 0.3161(44) 0.5878(25) 0.4554(55) C46B C 0.4372(18) 0.5893(10) 0.0983(22) C47B C 0.4905(36) 0.6428(20) 0.2327(44) C50B C 0.7092(28) 0.4862(15) 0.2069(33) C51B C 0.7142(26) 0.5716(15) 0.2314(31) O1B O 0.6606(8) 0.6221(4) 0.6975(10) O2B O 0.7582(15) 0.5260(8) 0.7181(18) C53B C 0.3709(34) 0.6489(17) 0.6398(39) C56B C 0.3397(43) 0.5977(24) 0.3744(53) C45B C 0.4735(26) 0.5823(14) 0.0054(32) C48B C 0.5455(25) 0.6522(13) 0.316(3) C49B C 0.7603(25) 0.4763(14) 0.3395(30) C52B C 0.6932(25) 0.6005(14) 0.1321(31) C38B C 0.6439(16) 0.6560(8) 0.6136(18) C39B C 0.6645(15) 0.6380(8) 0.8092(17) C42B C 0.8232(23) 0.5317(12) 0.6611(27) C43B C 0.7655(37) 0.4942(23) 0.7996(50) C37B C 0.7169(19) 0.6842(10) 0.6116(22) C40B C 0.7556(15) 0.6398(8) 0.8653(17) C41B C 0.8147(21) 0.5667(12) 0.5874(26) C44B C 0.7540(27) 0.5028(14) 0.8989(32) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ag1 Li1 2.807 1_555 1_555 Ag2 Li1 2.711 1_555 1_555 Ag3 Li1 2.775 1_555 1_555 Br1 Li3 2.603 1_555 1_555 Br2 Li3 2.591 1_555 1_555 Li1 C7 2.332 1_555 1_555 Li2 Ag1 2.698 1_555 1_555 C1 Ag1 2.120 1_555 1_555 C2 C1 1.417 1_555 1_555 C3 C1 1.408 1_555 1_555 C4 C2 1.438 1_555 1_555 C5 C3 1.444 1_555 1_555 C6 C4 1.354 1_555 1_555 C7 Ag1 2.138 1_555 1_555 C8 C7 1.433 1_555 1_555 C9 C7 1.387 1_555 1_555 C10 C9 1.446 1_555 1_555 C11 C8 1.400 1_555 1_555 C12 C10 1.426 1_555 1_555 C13 Ag2 2.135 1_555 1_555 C14 C13 1.432 1_555 1_555 C15 C13 1.407 1_555 1_555 C16 C14 1.430 1_555 1_555 C17 C15 1.455 1_555 1_555 C18 C16 1.344 1_555 1_555 C19 Ag2 2.130 1_555 1_555 C20 C19 1.418 1_555 1_555 C21 C19 1.418 1_555 1_555 C22 C20 1.354 1_555 1_555 C23 C21 1.408 1_555 1_555 C24 C22 1.387 1_555 1_555 C25 Ag3 2.102 1_555 1_555 C26 C25 1.429 1_555 1_555 C27 C25 1.413 1_555 1_555 C28 C26 1.437 1_555 1_555 C29 C27 1.395 1_555 1_555 C30 C28 1.387 1_555 1_555 C31 Ag3 2.130 1_555 1_555 C32 C31 1.394 1_555 1_555 C33 C31 1.409 1_555 1_555 C34 C32 1.473 1_555 1_555 C35 C33 1.426 1_555 1_555 C36 C34 1.390 1_555 1_555 Li3 O1 1.919 1_555 1_555 Li4 Br1 2.638 1_555 1_555 Li5 Br1 2.557 1_555 1_555 C37 C38 1.469 1_555 1_555 C38 O1 1.464 1_555 1_555 O1 C39 1.499 1_555 1_555 C39 C40 1.546 1_555 1_555 C41 C42 1.395 1_555 1_555 C42 O2 1.409 1_555 1_555 O2 Li3 2.015 1_555 1_555 C43 O2 1.398 1_555 1_555 C44 C43 1.344 1_555 1_555 C45 C46 1.439 1_555 1_555 C46 O3 1.438 1_555 1_555 O3 Li4 1.811 1_555 1_555 C47 O3 1.569 1_555 1_555 C48 C47 1.303 1_555 1_555 C49 C50 1.783 1_555 1_555 C50 O4 1.664 1_555 1_555 O4 Li4 2.020 1_555 1_555 C51 O4 1.452 1_555 1_555 C52 C51 1.524 1_555 1_555 C53 C54 1.206 1_555 1_555 C54 O5 1.660 1_555 1_555 O5 Li5 1.951 1_555 1_555 C55 O5 1.501 1_555 1_555 C56 C55 1.208 1_555 1_555 Li5B Br1 2.578 1_555 1_555 Li4B Br2 2.634 1_555 1_555 Br2B Li4 2.634 1_555 1_555 Br1B Li5 2.578 1_555 1_555 O5B Li5B 1.951 1_555 1_555 O3B Li4B 1.811 1_555 1_555 O4B Li4B 2.020 1_555 1_555 Li3B Br2B 2.591 1_555 1_555 C54B O5B 1.660 1_555 1_555 C55B O5B 1.501 1_555 1_555 C46B O3B 1.438 1_555 1_555 C47B O3B 1.569 1_555 1_555 C50B O4B 1.664 1_555 1_555 C51B O4B 1.452 1_555 1_555 O1B Li3B 1.919 1_555 1_555 O2B Li3B 2.015 1_555 1_555 C53B C54B 1.206 1_555 1_555 C56B C55B 1.208 1_555 1_555 C45B C46B 1.439 1_555 1_555 C48B C47B 1.303 1_555 1_555 C49B C50B 1.783 1_555 1_555 C52B C51B 1.524 1_555 1_555 C38B O1B 1.464 1_555 1_555 C39B O1B 1.499 1_555 1_555 C42B O2B 1.409 1_555 1_555 C43B O2B 1.398 1_555 1_555 C37B C38B 1.469 1_555 1_555 C40B C39B 1.546 1_555 1_555 C41B C42B 1.395 1_555 1_555 C44B C43B 1.344 1_555 1_555 Ag2 Li2 2.748 1_555 1_555 Ag3 Li2 2.790 1_555 1_555 Br2 Li5 2.447 1_555 1_555 Li1 C13 2.198 1_555 1_555 Li1 C31 2.320 1_555 1_555 Li2 C1 2.188 1_555 1_555 Li2 C19 2.275 1_555 1_555 Li2 C25 2.283 1_555 1_555 C5 C6 1.366 1_555 1_555 C11 C12 1.342 1_555 1_555 C17 C18 1.371 1_555 1_555 C23 C24 1.412 1_555 1_555 C29 C30 1.405 1_555 1_555 C35 C36 1.380 1_555 1_555 Li5B Br1B 2.557 1_555 1_555 Li5B Br2B 2.447 1_555 1_555 Li4B Br1B 2.638 1_555 1_555 Br1B Li3B 2.603 1_555 1_555 #END data_CSD_CIF_CUTCEZ _audit_creation_date 1986-02-24 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD CUTCEZ _chemical_formula_sum 'C60 H90 Cu4 Li2 O6' _chemical_formula_moiety ; C36 H30 Cu4 Li1 1-,C16 H40 Li1 O4 1+,2(C4 H10 O1) ; _journal_coden_Cambridge 4 _journal_volume 107 _journal_year 1985 _journal_page_first 1682 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "S.I.Khan" "P.G.Edwards" "H.S.H.Yuan" "R.Bau" _chemical_name_systematic ; hexakis(\m~2~-Phenyl)-lithium-tetra-copper tetrakis(diethyl ether)-lithium diethyl ether solvate ; _cell_volume 2937.390 _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.16 _exptl_special_details ; dx reported as 1.16. We calculate 1.33. Average bond lengths are reported. Ether carbon x(C18) may read -0.1929 rather than -0.2199 in Suppl. Table B ; _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; _refine_special_details ; One coordinated ether molecule and two solvent ether molecules are located (and hence disordered) about a three-fold axis. Its C-atoms are not reported. Occupancy refinement revealed that the Li3 site is composed of Li:Cu 0.89:0.11. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.103 _refine_ls_wR_factor_gt 0.103 _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 31 c' _symmetry_Int_Tables_number 159 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 y,x,1/2+z 5 x-y,-y,1/2+z 6 -x,-x+y,1/2+z _cell_length_a 13.242(3) _cell_length_b 13.242(3) _cell_length_c 19.343(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 Cu 1.45 Li 0.68 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Cu1 Cu 0.33330 0.66670 0.0894(21) Cu2 Cu 0.2498(10) 0.5000(4) 0.0017(14) Li1 Li 0.33330 0.66670 -0.0835(19) C1 C 0.1832(23) 0.4738(29) 0.0967(18) C2 C 0.2287(21) 0.4551(32) 0.1572(20) C3 C 0.1298(27) 0.4149(25) 0.2164(18) C4 C 0.0454(25) 0.3933(26) 0.2151(18) C5 C 0.000(2) 0.4120(25) 0.1546(21) C6 C 0.0689(24) 0.4522(19) 0.0954(18) C7 C 0.3063(34) 0.4921(30) -0.0897(20) C8 C 0.4031(29) 0.4791(24) -0.1013(23) C9 C 0.422(3) 0.4470(34) -0.1666(26) C10 C 0.3441(39) 0.4278(37) -0.2202(20) C11 C 0.2473(33) 0.4407(32) -0.2086(21) C12 C 0.2284(28) 0.4728(33) -0.1433(24) Li2 Li 0.00000 0.00000 0.5206(45) O1 O 0.8401(39) 0.9041(80) 0.5073(48) C13 C 0.8071(82) 0.7748(78) 0.4559(44) C14 C 0.6992(83) 0.7772(74) 0.4251(42) C15 C 0.7728(78) 0.9745(82) 0.4933(44) C16 C 0.70000 0.94000 0.56000 O2 O 0.00000 0.00000 0.6162(50) O3 O 0.33330 0.66670 0.3935(39) O4 O 0.33330 0.66670 0.5347(35) Cu2A Cu 0.500(1) 0.7498(4) 0.0017(14) Cu2B Cu 0.2502(10) 0.7502(4) 0.0017(14) C1A C 0.5262(23) 0.7094(29) 0.0967(18) C1B C 0.2906(23) 0.8168(29) 0.0967(18) C7A C 0.5079(34) 0.8142(30) -0.0897(20) C7B C 0.1858(34) 0.6937(30) -0.0897(20) C2A C 0.5449(21) 0.7736(32) 0.1572(20) C6A C 0.5478(24) 0.6167(19) 0.0954(18) C2B C 0.2264(21) 0.7713(32) 0.1572(20) C6B C 0.3833(24) 0.9311(19) 0.0954(18) C8A C 0.5209(29) 0.9240(24) -0.1013(23) C12A C 0.5272(28) 0.7556(33) -0.1433(24) C8B C 0.0760(29) 0.5969(24) -0.1013(23) C12B C 0.2444(28) 0.7716(33) -0.1433(24) C3A C 0.5851(27) 0.7149(25) 0.2164(18) C5A C 0.588(2) 0.5880(25) 0.1546(21) C3B C 0.2851(27) 0.8702(25) 0.2164(18) C5B C 0.412(2) 1.0000(25) 0.1546(21) C9A C 0.553(3) 0.9750(34) -0.1666(26) C11A C 0.5593(33) 0.8066(32) -0.2086(21) C9B C 0.025(3) 0.5780(34) -0.1666(26) C11B C 0.1934(33) 0.7527(32) -0.2086(21) C4A C 0.6067(25) 0.6521(26) 0.2151(18) C4B C 0.3479(25) 0.9546(26) 0.2151(18) C10A C 0.5722(39) 0.9163(37) -0.2202(20) C10B C 0.0837(39) 0.6559(37) -0.2202(20) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cu1 Cu2 2.556 1_555 1_555 Cu2 Li1 2.524 1_555 1_555 Li1 Cu2A 2.524 1_555 1_555 C1 Cu1 2.328 1_555 1_555 C2 C1 1.394 1_555 1_555 C3 C2 1.616 1_555 1_555 C4 C3 1.006 1_555 1_555 C5 C4 1.393 1_555 1_555 C6 C1 1.393 1_555 1_555 C7 Cu2 1.943 1_555 1_555 C8 C7 1.394 1_555 1_555 C9 C8 1.395 1_555 1_555 C10 C9 1.393 1_555 1_555 C11 C10 1.393 1_555 1_555 C12 C7 1.393 1_555 1_555 Li2 O2 1.849 1_555 1_555 O1 C13 1.834 1_555 1_555 C13 C14 1.563 1_555 1_555 C15 O1 1.602 1_555 1_555 C16 C15 1.537 1_555 1_555 Cu2A Cu1 2.556 1_555 1_555 Cu2B Cu1 2.555 1_555 1_555 C1A Cu1 2.328 1_555 1_555 C1B Cu1 2.327 1_555 1_555 C7A Cu2A 1.943 1_555 1_555 C7B Cu2B 1.943 1_555 1_555 C2A C1A 1.394 1_555 1_555 C6A C1A 1.393 1_555 1_555 C2B C1B 1.394 1_555 1_555 C6B C1B 1.393 1_555 1_555 C8A C7A 1.394 1_555 1_555 C12A C7A 1.393 1_555 1_555 C8B C7B 1.394 1_555 1_555 C12B C7B 1.393 1_555 1_555 C3A C2A 1.616 1_555 1_555 C5A C6A 1.393 1_555 1_555 C3B C2B 1.616 1_555 1_555 C5B C6B 1.393 1_555 1_555 C9A C8A 1.395 1_555 1_555 C11A C12A 1.395 1_555 1_555 C9B C8B 1.395 1_555 1_555 C11B C12B 1.395 1_555 1_555 C4A C3A 1.006 1_555 1_555 C4B C3B 1.006 1_555 1_555 C10A C9A 1.393 1_555 1_555 C10B C9B 1.393 1_555 1_555 Cu2 Cu2A 3.311 1_555 1_555 Cu2 Cu2B 3.311 1_555 1_555 Cu2 C1 1.992 1_555 1_555 Li1 Cu2B 2.523 1_555 1_555 C5 C6 1.393 1_555 1_555 C11 C12 1.395 1_555 1_555 Cu2A Cu2B 3.311 1_555 1_555 Cu2A C1A 1.992 1_555 1_555 Cu2B C1B 1.992 1_555 1_555 C5A C4A 1.393 1_555 1_555 C5B C4B 1.393 1_555 1_555 C11A C10A 1.393 1_555 1_555 C11B C10B 1.393 1_555 1_555 #END data_CSD_CIF_DAQFOT _audit_creation_date 2017-05-17 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD DAQFOT _database_code_depnum_ccdc_archive 'CCDC 1550705' _chemical_formula_sum 'H12 B12 Cs1 Na1' _chemical_formula_moiety ; H12 B12 2-,Cs1 1-,Na1 1+ ; _journal_coden_Cambridge 9 _journal_volume 56 _journal_year 2017 _journal_page_first 5006 _journal_name_full 'Inorg.Chem. ' loop_ _publ_author_name "Y.Sadikin" "P.Schouwink" "M.Brighi" "Z.Lodziana" "R.Cerny" _chemical_name_systematic ; cesium sodium closo-dodecaborate ; _cell_volume 617.965 _exptl_special_details ; powder data ; _diffrn_ambient_temperature 805 _diffrn_radiation_probe x-ray _diffrn_source synchrotron _refine_special_details ; The structure is disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.35 _refine_ls_wR_factor_gt 0.35 _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63 m c' _symmetry_Int_Tables_number 186 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,1/2+z 3 -x+y,-x,z 4 -x+y,y,z 5 -y,-x,z 6 -y,x-y,z 7 y,-x+y,1/2+z 8 y,x,1/2+z 9 x-y,-y,1/2+z 10 x-y,x,1/2+z 11 -x,-x+y,1/2+z 12 x,x-y,z _cell_length_a 7.6227(5) _cell_length_b 7.6227(5) _cell_length_c 12.280488 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond H 0.23 B 0.83 Cs 2.44 Na 1.66 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Cs1 Cs 0.090(3) 0.084(3) 0.067(5) B1 B 0.21864 0.51382 0.42487 H1 H 0.13784 0.40399 0.50255 B2 B 0.47374 0.71667 0.43043 H2 H 0.57610 0.75216 0.51201 B3 B 0.16778 0.41988 0.28896 H3 H 0.05025 0.24280 0.26913 B4 B 0.58068 0.74839 0.29774 H4 H 0.75938 0.80674 0.28428 B5 B 0.27124 0.76908 0.42245 H5 H 0.22814 0.84232 0.49848 H6 H 0.04742 0.24402 0.26282 B6 B 0.40990 0.50090 0.34791 H7 H 0.46623 0.38180 0.37041 B7 B 0.49482 0.91407 0.34412 H8 H 0.61201 1.09125 0.36391 B8 B 0.18893 0.61730 0.20263 H9 H 0.08699 0.58168 0.12087 B9 B 0.39140 0.56483 0.21051 H10 H 0.43468 0.49180 0.13446 B10 B 0.08217 0.58578 0.33503 H11 H -0.09649 0.52779 0.34833 B11 B 0.44403 0.82038 0.20817 H12 H 0.52488 0.93034 0.13054 Na1 Na 0.66667 0.33333 0.247(6) B1B B 0.29518 0.78136 0.42487 H1B H 0.26616 0.86216 0.50255 B2B B 0.24293 0.52626 0.43043 H2B H 0.17606 0.42390 0.51201 B3B B 0.25211 0.83222 0.28896 H3B H 0.19255 0.94975 0.26913 B4B B 0.16771 0.41932 0.29774 H4B H 0.04736 0.24062 0.28428 B5B B 0.49784 0.72876 0.42245 H5B H 0.61418 0.77186 0.49848 H6B H 0.19661 0.95258 0.26282 B1C B 0.29518 0.51382 0.42487 H1C H 0.26616 0.40399 0.50255 B2C B 0.24293 0.71667 0.43043 H2C H 0.17606 0.75216 0.51201 B3C B 0.25211 0.41988 0.28896 H3C H 0.19255 0.24280 0.26913 B4C B 0.16771 0.74839 0.29774 H4C H 0.04736 0.80674 0.28428 B5C B 0.49784 0.76908 0.42245 H5C H 0.61418 0.84232 0.49848 H6C H 0.19661 0.24402 0.26282 B1D B 0.48618 0.78136 0.42487 H1D H 0.59601 0.86216 0.50255 B2D B 0.28333 0.52626 0.43043 H2D H 0.24784 0.42390 0.51201 B3D B 0.58012 0.83222 0.28896 H3D H 0.75720 0.94975 0.26913 B4D B 0.25161 0.41932 0.29774 H4D H 0.19326 0.24062 0.28428 B5D B 0.23092 0.72876 0.42245 H5D H 0.15768 0.77186 0.49848 H6D H 0.75598 0.95258 0.26282 B1E B 0.48618 0.70482 0.42487 H1E H 0.59601 0.73384 0.50255 B2E B 0.28333 0.75707 0.43043 H2E H 0.24784 0.82394 0.51201 B3E B 0.58012 0.74789 0.28896 H3E H 0.75720 0.80745 0.26913 B4E B 0.25161 0.83229 0.29774 H4E H 0.19326 0.95264 0.28428 B5E B 0.23092 0.50216 0.42245 H5E H 0.15768 0.38582 0.49848 H6E H 0.75598 0.80339 0.26282 B1K B 0.21864 0.70482 0.42487 H1K H 0.13784 0.73384 0.50255 B2K B 0.47374 0.75707 0.43043 H2K H 0.57610 0.82394 0.51201 B3K B 0.16778 0.74789 0.28896 H3K H 0.05025 0.80745 0.26913 B4K B 0.58068 0.83229 0.29774 H4K H 0.75938 0.95264 0.28428 B5K B 0.27124 0.50216 0.42245 H5K H 0.22814 0.38582 0.49848 H6K H 0.04742 0.80339 0.26282 B6B B 0.09100 0.59010 0.34791 H7B H -0.08443 0.53377 0.37041 B7B B 0.41926 0.50518 0.34412 H8B H 0.47924 0.38799 0.36391 B8B B 0.42837 0.81107 0.20263 H9B H 0.49469 0.91301 0.12087 B9B B 0.17343 0.60860 0.21051 H10B H 0.05712 0.56532 0.13446 B10B B 0.50362 0.91783 0.33503 H11B H 0.62429 1.09649 0.34833 B11B B 0.37635 0.55597 0.20817 H12B H 0.40546 0.47512 0.13054 B6C B 0.09100 0.50090 0.34791 H7C H -0.08443 0.38180 0.37041 B7C B 0.41926 0.91407 0.34412 H8C H 0.47924 1.09125 0.36391 B8C B 0.42837 0.61730 0.20263 H9C H 0.49469 0.58168 0.12087 B9C B 0.17343 0.56483 0.21051 H10C H 0.05712 0.49180 0.13446 B10C B 0.50362 0.58578 0.33503 H11C H 0.62429 0.52779 0.34833 B11C B 0.37635 0.82038 0.20817 H12C H 0.40546 0.93034 0.13054 B6D B 0.49910 0.59010 0.34791 H7D H 0.61820 0.53377 0.37041 B7D B 0.08593 0.50518 0.34412 H8D H -0.09125 0.38799 0.36391 B8D B 0.38270 0.81107 0.20263 H9D H 0.41832 0.91301 0.12087 B9D B 0.43517 0.60860 0.21051 H10D H 0.50820 0.56532 0.13446 B10D B 0.41422 0.91783 0.33503 H11D H 0.47221 1.09649 0.34833 B11D B 0.17962 0.55597 0.20817 H12D H 0.06966 0.47512 0.13054 B6E B 0.49910 0.90900 0.34791 H7E H 0.61820 1.08443 0.37041 B7E B 0.08593 0.58074 0.34412 H8E H -0.09125 0.52076 0.36391 B8E B 0.38270 0.57163 0.20263 H9E H 0.41832 0.50531 0.12087 B9E B 0.43517 0.82657 0.21051 H10E H 0.50820 0.94288 0.13446 B10E B 0.41422 0.49638 0.33503 H11E H 0.47221 0.37571 0.34833 B11E B 0.17962 0.62365 0.20817 H12E H 0.06966 0.59454 0.13054 B6K B 0.40990 0.90900 0.34791 H7K H 0.46623 1.08443 0.37041 B7K B 0.49482 0.58074 0.34412 H8K H 0.61201 0.52076 0.36391 B8K B 0.18893 0.57163 0.20263 H9K H 0.08699 0.50531 0.12087 B9K B 0.39140 0.82657 0.21051 H10K H 0.43468 0.94288 0.13446 B10K B 0.08217 0.49638 0.33503 H11K H -0.09649 0.37571 0.34833 B11K B 0.44403 0.62365 0.20817 H12K H 0.52488 0.59454 0.13054 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 B1 H1 1.214 1_555 1_555 H1 B2B 1.244 1_555 1_555 B2 H2 1.214 1_555 1_555 H2 B5B 1.221 1_555 1_555 B3 H3 1.214 1_555 1_555 H3 B4B 1.237 1_555 1_555 B4 H4 1.214 1_555 1_555 H4 B3D 1.474 1_555 1_555 B5 B2 1.780 1_555 1_555 H5 B5 1.214 1_555 1_555 H6 B3 1.230 1_555 1_555 B6 H7 1.214 1_555 1_555 H7 B7B 1.206 1_555 1_555 B7 H8 1.214 1_555 1_555 H8 B10B 1.210 1_555 1_555 B8 H9 1.214 1_555 1_555 H9 B9B 1.246 1_555 1_555 B9 B8 1.780 1_555 1_555 H10 B9 1.214 1_555 1_555 B10 H11 1.214 1_555 1_555 H11 B6B 1.261 1_555 1_555 B11 B8 1.781 1_555 1_555 H12 B11 1.214 1_555 1_555 B1B H5 1.238 1_555 1_555 H1B B5 1.225 1_555 1_555 B2B B2 1.627 1_555 1_555 H2B B1 1.224 1_555 1_555 B3B H3B 1.214 1_555 1_555 H3B B4C 1.492 1_555 1_555 B4B H6 1.259 1_555 1_555 H4B B3 1.208 1_555 1_555 B5B B4 1.635 1_555 1_555 H5B B2 1.253 1_555 1_555 H6B B3B 1.230 1_555 1_555 B1C H1 1.430 1_555 1_555 H1C B1 1.430 1_555 1_555 B2C B2 1.759 1_555 1_555 H2C B5 1.288 1_555 1_555 B3C B3 0.643 1_555 1_555 H3C B3 1.474 1_555 1_555 B4C B5 1.694 1_555 1_555 H4C B3B 1.474 1_555 1_555 B5C H2 1.288 1_555 1_555 H5C B2 1.318 1_555 1_555 H6C B3 1.498 1_555 1_555 B1D H2 1.348 1_555 1_555 H1D B2 1.360 1_555 1_555 B2D H1 1.360 1_555 1_555 H2D B1 1.348 1_555 1_555 B3D B4 0.650 1_555 1_555 H3D B4 1.492 1_555 1_555 B4D B3 0.650 1_555 1_555 H4D B3 1.474 1_555 1_555 B5D B2 1.901 1_555 1_555 H5D B5 1.281 1_555 1_555 H6D B3D 1.230 1_555 1_555 B1E H2 1.224 1_555 1_555 H1E B2 1.244 1_555 1_555 B2E B2 1.627 1_555 1_555 H2E B5 1.221 1_555 1_555 B3E H4 1.208 1_555 1_555 H3E B4 1.237 1_555 1_555 B4E B5 1.635 1_555 1_555 H4E B3B 1.208 1_555 1_555 B5E H1 1.225 1_555 1_555 H5E B1 1.238 1_555 1_555 H6E B4 1.259 1_555 1_555 B1K H5 1.358 1_555 1_555 H1K B5 1.342 1_555 1_555 B2K H2 1.282 1_555 1_555 H2K B2 1.282 1_555 1_555 B3K B3B 0.643 1_555 1_555 H3K B3B 1.474 1_555 1_555 B4K B4 0.640 1_555 1_555 H4K B4 1.479 1_555 1_555 B5K H1 1.342 1_555 1_555 H5K B1 1.358 1_555 1_555 H6K B3B 1.498 1_555 1_555 B6B H7B 1.214 1_555 1_555 H7B B10 1.206 1_555 1_555 B7B H8B 1.214 1_555 1_555 H8B B6 1.230 1_555 1_555 B8B B8 1.678 1_555 1_555 H9B B11 1.235 1_555 1_555 B9B B9 1.851 1_555 1_555 H10B B8 1.212 1_555 1_555 B10B H11B 1.214 1_555 1_555 H11B B7 1.240 1_555 1_555 B11B B8 1.712 1_555 1_555 H12B B9 1.232 1_555 1_555 B6C B10 0.701 1_555 1_555 H7C B10 1.498 1_555 1_555 B7C B7 0.576 1_555 1_555 H8C B7 1.434 1_555 1_555 B8C B8 1.825 1_555 1_555 H9C B9 1.322 1_555 1_555 B9C H9 1.322 1_555 1_555 H10C B8 1.290 1_555 1_555 B10C B6 0.701 1_555 1_555 H11C B7B 1.485 1_555 1_555 B11C B8 1.493 1_555 1_555 H12C B11 1.394 1_555 1_555 B6D B6 0.680 1_555 1_555 H7D B6 1.504 1_555 1_555 B7D B10 0.639 1_555 1_555 H8D B10 1.467 1_555 1_555 B8D B8 1.477 1_555 1_555 H9D B11 1.351 1_555 1_555 B9D B8 1.913 1_555 1_555 H10D B9 1.289 1_555 1_555 B10D B7 0.639 1_555 1_555 H11D B7 1.485 1_555 1_555 B11D H9 1.351 1_555 1_555 H12D B8 1.342 1_555 1_555 B6E H8 1.230 1_555 1_555 H7E B7 1.206 1_555 1_555 B7E H11 1.240 1_555 1_555 H8E B10 1.210 1_555 1_555 B8E B8 1.678 1_555 1_555 H9E B9 1.246 1_555 1_555 B9E B8 1.756 1_555 1_555 H10E B11 1.214 1_555 1_555 B10E H7 1.206 1_555 1_555 H11E B6 1.261 1_555 1_555 B11E H9 1.235 1_555 1_555 H12E B8 1.218 1_555 1_555 B6K B7 0.631 1_555 1_555 H7K B7 1.456 1_555 1_555 B7K B6 0.631 1_555 1_555 H8K B6 1.484 1_555 1_555 B8K H9 1.295 1_555 1_555 H9K B8 1.295 1_555 1_555 B9K B8 1.573 1_555 1_555 H10K B11 1.328 1_555 1_555 B10K B10 0.681 1_555 1_555 H11K B10 1.505 1_555 1_555 B11K B8 1.922 1_555 1_555 H12K B9 1.349 1_555 1_555 B2 B2D 1.451 1_555 1_555 B2 B5E 1.756 1_555 1_555 B2 B5K 1.594 1_555 1_555 H3 B3C 1.474 1_555 1_555 H3 B4D 1.492 1_555 1_555 B4 B5C 1.694 1_555 1_555 H4 B4K 1.479 1_555 1_555 B5 B2B 1.756 1_555 1_555 B5 B5B 1.900 1_555 1_555 B5 B5C 1.727 1_555 1_555 B5 B2D 1.901 1_555 1_555 B5 B5E 1.900 1_555 1_555 B5 B2K 1.594 1_555 1_555 B5 B5K 2.035 1_555 1_555 H5 B2C 1.318 1_555 1_555 H5 B5D 1.281 1_555 1_555 H5 B2E 1.253 1_555 1_555 H6 B3C 1.498 1_555 1_555 H7 B10C 1.498 1_555 1_555 H7 B6D 1.504 1_555 1_555 H7 B7K 1.456 1_555 1_555 H8 B7C 1.434 1_555 1_555 H8 B10D 1.467 1_555 1_555 H8 B6K 1.484 1_555 1_555 B9 B11 1.782 1_555 1_555 B9 B8B 1.756 1_555 1_555 B9 B9C 1.661 1_555 1_555 B9 B10C 1.720 1_555 1_555 B9 B11C 2.008 1_555 1_555 B9 B8D 1.913 1_555 1_555 B9 B11D 1.582 1_555 1_555 B9 B9E 1.851 1_555 1_555 B9 B10E 1.653 1_555 1_555 B9 B11E 1.879 1_555 1_555 B9 B8K 1.573 1_555 1_555 B9 B9K 1.995 1_555 1_555 H10 B11B 1.214 1_555 1_555 H10 B8C 1.290 1_555 1_555 H10 B9D 1.289 1_555 1_555 H10 B8E 1.212 1_555 1_555 H10 B11K 1.328 1_555 1_555 B10 B9B 1.653 1_555 1_555 B10 B9C 1.720 1_555 1_555 H11 B7D 1.485 1_555 1_555 H11 B10K 1.505 1_555 1_555 B11 B9B 1.879 1_555 1_555 B11 B11B 1.813 1_555 1_555 B11 B8C 1.493 1_555 1_555 B11 B9C 2.008 1_555 1_555 B11 B9D 1.582 1_555 1_555 B11 B11D 2.016 1_555 1_555 B11 B8E 1.712 1_555 1_555 B11 B11E 1.813 1_555 1_555 B11 B8K 1.922 1_555 1_555 B11 B11K 1.500 1_555 1_555 H12 B8B 1.218 1_555 1_555 H12 B11C 1.394 1_555 1_555 H12 B8D 1.342 1_555 1_555 H12 B9E 1.232 1_555 1_555 H12 B9K 1.349 1_555 1_555 B1B H1B 1.214 1_555 1_555 B1B H2C 1.348 1_555 1_555 B1B H5D 1.358 1_555 1_555 B1B H2E 1.224 1_555 1_555 B1B H1K 1.430 1_555 1_555 H1B B2C 1.360 1_555 1_555 H1B B5D 1.342 1_555 1_555 H1B B2E 1.244 1_555 1_555 H1B B1K 1.430 1_555 1_555 B2B H2B 1.214 1_555 1_555 B2B B5B 1.780 1_555 1_555 B2B H1C 1.360 1_555 1_555 B2B B2C 1.451 1_555 1_555 B2B B5C 1.901 1_555 1_555 B2B H2D 1.282 1_555 1_555 B2B B5D 1.594 1_555 1_555 B2B B2E 1.627 1_555 1_555 B2B H5E 1.253 1_555 1_555 B2B B2K 1.759 1_555 1_555 B2B H5K 1.318 1_555 1_555 H2B B1C 1.348 1_555 1_555 H2B B2D 1.282 1_555 1_555 H2B B5E 1.221 1_555 1_555 H2B B5K 1.288 1_555 1_555 B3B B4C 0.650 1_555 1_555 H3B B4E 1.237 1_555 1_555 H3B B3K 1.474 1_555 1_555 B4B H4B 1.214 1_555 1_555 B4B B3C 0.650 1_555 1_555 B4B H3C 1.492 1_555 1_555 B4B B4D 0.640 1_555 1_555 B4B H4D 1.479 1_555 1_555 B4B B5E 1.635 1_555 1_555 B4B B5K 1.694 1_555 1_555 H4B B3C 1.474 1_555 1_555 H4B B4D 1.479 1_555 1_555 B5B H5B 1.214 1_555 1_555 B5B B2C 1.901 1_555 1_555 B5B H5C 1.281 1_555 1_555 B5B H1D 1.342 1_555 1_555 B5B B2D 1.594 1_555 1_555 B5B B5D 2.035 1_555 1_555 B5B H1E 1.225 1_555 1_555 B5B B2E 1.756 1_555 1_555 B5B B5E 1.900 1_555 1_555 B5B H2K 1.288 1_555 1_555 B5B B4K 1.694 1_555 1_555 B5B B5K 1.727 1_555 1_555 H5B B5C 1.281 1_555 1_555 H5B B1D 1.358 1_555 1_555 H5B B1E 1.238 1_555 1_555 H5B B2K 1.318 1_555 1_555 H6B B4E 1.259 1_555 1_555 H6B B3K 1.498 1_555 1_555 B1C H1C 1.214 1_555 1_555 B1C H2D 1.224 1_555 1_555 B1C H5E 1.358 1_555 1_555 B1C H5K 1.238 1_555 1_555 H1C B2D 1.244 1_555 1_555 H1C B5E 1.342 1_555 1_555 H1C B5K 1.225 1_555 1_555 B2C H2C 1.214 1_555 1_555 B2C B5C 1.780 1_555 1_555 B2C B2D 1.627 1_555 1_555 B2C H5D 1.253 1_555 1_555 B2C H2E 1.282 1_555 1_555 B2C B5E 1.594 1_555 1_555 B2C H1K 1.244 1_555 1_555 B2C B2K 1.627 1_555 1_555 B2C B5K 1.756 1_555 1_555 H2C B5D 1.221 1_555 1_555 H2C B2E 1.282 1_555 1_555 H2C B1K 1.224 1_555 1_555 B3C H3C 1.214 1_555 1_555 B3C H6C 1.230 1_555 1_555 B3C H4D 1.208 1_555 1_555 H3C B4D 1.237 1_555 1_555 B4C H4C 1.214 1_555 1_555 B4C B5D 1.635 1_555 1_555 B4C B4E 0.640 1_555 1_555 B4C H4E 1.479 1_555 1_555 B4C H3K 1.237 1_555 1_555 B4C H6K 1.259 1_555 1_555 H4C B4E 1.479 1_555 1_555 H4C B3K 1.208 1_555 1_555 B5C H5C 1.214 1_555 1_555 B5C H1D 1.225 1_555 1_555 B5C B2D 1.756 1_555 1_555 B5C B5D 1.900 1_555 1_555 B5C H1E 1.342 1_555 1_555 B5C B2E 1.594 1_555 1_555 B5C B5E 2.035 1_555 1_555 B5C H2K 1.221 1_555 1_555 B5C B4K 1.635 1_555 1_555 B5C B5K 1.900 1_555 1_555 H5C B1D 1.238 1_555 1_555 H5C B1E 1.358 1_555 1_555 H5C B2K 1.253 1_555 1_555 H6C B4D 1.259 1_555 1_555 B1D H1D 1.214 1_555 1_555 B1D H1E 1.430 1_555 1_555 B1D H2K 1.224 1_555 1_555 H1D B1E 1.430 1_555 1_555 H1D B2K 1.244 1_555 1_555 B2D H2D 1.214 1_555 1_555 B2D B5D 1.780 1_555 1_555 B2D B2E 1.759 1_555 1_555 B2D H5E 1.318 1_555 1_555 B2D B2K 1.627 1_555 1_555 B2D H5K 1.253 1_555 1_555 H2D B5E 1.288 1_555 1_555 H2D B5K 1.221 1_555 1_555 B3D H3D 1.214 1_555 1_555 B3D B3E 0.643 1_555 1_555 B3D H3E 1.474 1_555 1_555 B3D H6E 1.498 1_555 1_555 B3D H4K 1.208 1_555 1_555 H3D B3E 1.474 1_555 1_555 H3D B4K 1.237 1_555 1_555 B4D H4D 1.214 1_555 1_555 B4D B5E 1.694 1_555 1_555 B4D B5K 1.635 1_555 1_555 B5D H5D 1.214 1_555 1_555 B5D H2E 1.288 1_555 1_555 B5D B4E 1.694 1_555 1_555 B5D B5E 1.727 1_555 1_555 B5D H1K 1.225 1_555 1_555 B5D B2K 1.756 1_555 1_555 B5D B5K 1.900 1_555 1_555 H5D B2E 1.318 1_555 1_555 H5D B1K 1.238 1_555 1_555 H6D B3E 1.498 1_555 1_555 H6D B4K 1.259 1_555 1_555 B1E H1E 1.214 1_555 1_555 B1E H2K 1.348 1_555 1_555 H1E B2K 1.360 1_555 1_555 B2E H2E 1.214 1_555 1_555 B2E B5E 1.780 1_555 1_555 B2E H1K 1.360 1_555 1_555 B2E B2K 1.451 1_555 1_555 B2E B5K 1.901 1_555 1_555 H2E B1K 1.348 1_555 1_555 B3E H3E 1.214 1_555 1_555 B3E H6E 1.230 1_555 1_555 B3E B4K 0.650 1_555 1_555 B3E H4K 1.474 1_555 1_555 H3E B4K 1.492 1_555 1_555 B4E H4E 1.214 1_555 1_555 B4E B3K 0.650 1_555 1_555 B4E H3K 1.492 1_555 1_555 H4E B3K 1.474 1_555 1_555 B5E H5E 1.214 1_555 1_555 B5E B2K 1.901 1_555 1_555 B5E H5K 1.281 1_555 1_555 H5E B5K 1.281 1_555 1_555 B1K H1K 1.214 1_555 1_555 B2K H2K 1.214 1_555 1_555 B2K B5K 1.780 1_555 1_555 B3K H3K 1.214 1_555 1_555 B3K H6K 1.230 1_555 1_555 B4K H4K 1.214 1_555 1_555 B5K H5K 1.214 1_555 1_555 B6B B6C 0.680 1_555 1_555 B6B H7C 1.504 1_555 1_555 B6B B7D 0.631 1_555 1_555 B6B H8D 1.484 1_555 1_555 B6B H8E 1.230 1_555 1_555 B6B B10K 0.701 1_555 1_555 H7B B6C 1.504 1_555 1_555 H7B B7D 1.456 1_555 1_555 H7B B7E 1.206 1_555 1_555 H7B B10K 1.498 1_555 1_555 B7B B10C 0.639 1_555 1_555 B7B B6D 0.631 1_555 1_555 B7B H7D 1.456 1_555 1_555 B7B H11E 1.240 1_555 1_555 B7B B7K 0.576 1_555 1_555 B7B H8K 1.434 1_555 1_555 H8B B10C 1.467 1_555 1_555 H8B B6D 1.484 1_555 1_555 H8B B10E 1.210 1_555 1_555 H8B B7K 1.434 1_555 1_555 B8B H9B 1.214 1_555 1_555 B8B B9B 1.780 1_555 1_555 B8B B11B 1.781 1_555 1_555 B8B B8C 1.477 1_555 1_555 B8B B9C 1.913 1_555 1_555 B8B H12C 1.342 1_555 1_555 B8B H9D 1.295 1_555 1_555 B8B B9D 1.573 1_555 1_555 B8B B11D 1.922 1_555 1_555 B8B B8E 1.678 1_555 1_555 B8B H10E 1.212 1_555 1_555 B8B B11E 1.712 1_555 1_555 B8B B8K 1.825 1_555 1_555 B8B H10K 1.290 1_555 1_555 B8B B11K 1.493 1_555 1_555 H9B B11C 1.351 1_555 1_555 H9B B8D 1.295 1_555 1_555 H9B B9E 1.246 1_555 1_555 H9B B9K 1.322 1_555 1_555 B9B H10B 1.214 1_555 1_555 B9B B11B 1.782 1_555 1_555 B9B B8C 1.913 1_555 1_555 B9B H10C 1.289 1_555 1_555 B9B B11C 1.582 1_555 1_555 B9B B8D 1.573 1_555 1_555 B9B B9D 1.995 1_555 1_555 B9B H12D 1.349 1_555 1_555 B9B B8E 1.756 1_555 1_555 B9B B9E 1.851 1_555 1_555 B9B H12E 1.232 1_555 1_555 B9B H9K 1.322 1_555 1_555 B9B B9K 1.661 1_555 1_555 B9B B10K 1.720 1_555 1_555 B9B B11K 2.008 1_555 1_555 H10B B9C 1.289 1_555 1_555 H10B B11D 1.328 1_555 1_555 H10B B11E 1.214 1_555 1_555 H10B B8K 1.290 1_555 1_555 B10B B7C 0.639 1_555 1_555 B10B H8C 1.467 1_555 1_555 B10B B10D 0.681 1_555 1_555 B10B H11D 1.505 1_555 1_555 B10B H7E 1.206 1_555 1_555 B10B B9E 1.653 1_555 1_555 B10B B6K 0.701 1_555 1_555 B10B H7K 1.498 1_555 1_555 B10B B9K 1.720 1_555 1_555 H11B B7C 1.485 1_555 1_555 H11B B10D 1.505 1_555 1_555 H11B B6E 1.261 1_555 1_555 B11B H12B 1.214 1_555 1_555 B11B H9C 1.351 1_555 1_555 B11B B9C 1.582 1_555 1_555 B11B B11C 2.016 1_555 1_555 B11B B8D 1.922 1_555 1_555 B11B H10D 1.328 1_555 1_555 B11B B11D 1.500 1_555 1_555 B11B H9E 1.235 1_555 1_555 B11B B9E 1.879 1_555 1_555 B11B B11E 1.813 1_555 1_555 B11B B8K 1.493 1_555 1_555 B11B B9K 2.008 1_555 1_555 B11B H12K 1.394 1_555 1_555 H12B B8C 1.342 1_555 1_555 H12B B9D 1.349 1_555 1_555 H12B B8E 1.218 1_555 1_555 H12B B11K 1.394 1_555 1_555 B6C H7C 1.214 1_555 1_555 B6C H8D 1.230 1_555 1_555 B6C B7E 0.631 1_555 1_555 B6C H8E 1.484 1_555 1_555 B6C H11K 1.261 1_555 1_555 H7C B7D 1.206 1_555 1_555 H7C B7E 1.456 1_555 1_555 H7C B10K 1.206 1_555 1_555 B7C H8C 1.214 1_555 1_555 B7C H11D 1.240 1_555 1_555 B7C B6E 0.631 1_555 1_555 B7C H7E 1.456 1_555 1_555 B7C H7K 1.206 1_555 1_555 H8C B10D 1.210 1_555 1_555 H8C B6E 1.484 1_555 1_555 H8C B6K 1.230 1_555 1_555 B8C H9C 1.214 1_555 1_555 B8C B9C 1.780 1_555 1_555 B8C B11C 1.781 1_555 1_555 B8C B8D 1.678 1_555 1_555 B8C H10D 1.212 1_555 1_555 B8C B11D 1.712 1_555 1_555 B8C H9E 1.295 1_555 1_555 B8C B9E 1.573 1_555 1_555 B8C B11E 1.922 1_555 1_555 B8C B8K 1.678 1_555 1_555 B8C B9K 1.756 1_555 1_555 B8C H12K 1.218 1_555 1_555 H9C B9D 1.246 1_555 1_555 H9C B8E 1.295 1_555 1_555 H9C B11K 1.235 1_555 1_555 B9C H10C 1.214 1_555 1_555 B9C B11C 1.782 1_555 1_555 B9C B8D 1.756 1_555 1_555 B9C B9D 1.851 1_555 1_555 B9C H12D 1.232 1_555 1_555 B9C B8E 1.573 1_555 1_555 B9C B9E 1.995 1_555 1_555 B9C H12E 1.349 1_555 1_555 B9C H9K 1.246 1_555 1_555 B9C B9K 1.851 1_555 1_555 B9C B10K 1.653 1_555 1_555 B9C B11K 1.879 1_555 1_555 H10C B11D 1.214 1_555 1_555 H10C B11E 1.328 1_555 1_555 H10C B8K 1.212 1_555 1_555 B10C H11C 1.214 1_555 1_555 B10C H7D 1.206 1_555 1_555 B10C B9D 1.653 1_555 1_555 B10C B10E 0.681 1_555 1_555 B10C H11E 1.505 1_555 1_555 B10C H8K 1.210 1_555 1_555 H11C B6D 1.261 1_555 1_555 H11C B10E 1.505 1_555 1_555 H11C B7K 1.240 1_555 1_555 B11C H12C 1.214 1_555 1_555 B11C H9D 1.235 1_555 1_555 B11C B9D 1.879 1_555 1_555 B11C B11D 1.813 1_555 1_555 B11C B8E 1.922 1_555 1_555 B11C H10E 1.328 1_555 1_555 B11C B11E 1.500 1_555 1_555 B11C B8K 1.712 1_555 1_555 B11C H10K 1.214 1_555 1_555 B11C B11K 1.813 1_555 1_555 H12C B8D 1.218 1_555 1_555 H12C B9E 1.349 1_555 1_555 H12C B9K 1.232 1_555 1_555 B6D H7D 1.214 1_555 1_555 B6D B10E 0.701 1_555 1_555 B6D H8K 1.230 1_555 1_555 H7D B10E 1.498 1_555 1_555 H7D B7K 1.206 1_555 1_555 B7D H8D 1.214 1_555 1_555 B7D B7E 0.576 1_555 1_555 B7D H8E 1.434 1_555 1_555 B7D H11K 1.240 1_555 1_555 H8D B7E 1.434 1_555 1_555 H8D B10K 1.210 1_555 1_555 B8D H9D 1.214 1_555 1_555 B8D B9D 1.780 1_555 1_555 B8D B11D 1.781 1_555 1_555 B8D B8E 1.825 1_555 1_555 B8D H10E 1.290 1_555 1_555 B8D B11E 1.493 1_555 1_555 B8D B8K 1.678 1_555 1_555 B8D H10K 1.212 1_555 1_555 B8D B11K 1.712 1_555 1_555 H9D B9E 1.322 1_555 1_555 H9D B9K 1.246 1_555 1_555 B9D H10D 1.214 1_555 1_555 B9D B11D 1.782 1_555 1_555 B9D H9E 1.322 1_555 1_555 B9D B9E 1.661 1_555 1_555 B9D B10E 1.720 1_555 1_555 B9D B11E 2.008 1_555 1_555 B9D B8K 1.756 1_555 1_555 B9D B9K 1.851 1_555 1_555 B9D H12K 1.232 1_555 1_555 H10D B8E 1.290 1_555 1_555 H10D B11K 1.214 1_555 1_555 B10D H11D 1.214 1_555 1_555 B10D B6E 0.701 1_555 1_555 B10D H7E 1.498 1_555 1_555 B10D B9E 1.720 1_555 1_555 B10D H7K 1.206 1_555 1_555 B10D B9K 1.653 1_555 1_555 H11D B6K 1.261 1_555 1_555 B11D H12D 1.214 1_555 1_555 B11D B8E 1.493 1_555 1_555 B11D B9E 2.008 1_555 1_555 B11D H12E 1.394 1_555 1_555 B11D H9K 1.235 1_555 1_555 B11D B9K 1.879 1_555 1_555 B11D B11K 1.813 1_555 1_555 H12D B11E 1.394 1_555 1_555 H12D B8K 1.218 1_555 1_555 B6E H7E 1.214 1_555 1_555 B6E B6K 0.680 1_555 1_555 B6E H7K 1.504 1_555 1_555 H7E B6K 1.504 1_555 1_555 B7E H8E 1.214 1_555 1_555 B7E B10K 0.639 1_555 1_555 B7E H11K 1.485 1_555 1_555 H8E B10K 1.467 1_555 1_555 B8E H9E 1.214 1_555 1_555 B8E B9E 1.780 1_555 1_555 B8E B11E 1.781 1_555 1_555 B8E B8K 1.477 1_555 1_555 B8E B9K 1.913 1_555 1_555 B8E H12K 1.342 1_555 1_555 H9E B11K 1.351 1_555 1_555 B9E H10E 1.214 1_555 1_555 B9E B11E 1.782 1_555 1_555 B9E B8K 1.913 1_555 1_555 B9E H10K 1.289 1_555 1_555 B9E B11K 1.582 1_555 1_555 H10E B9K 1.289 1_555 1_555 B10E H11E 1.214 1_555 1_555 B10E B7K 0.639 1_555 1_555 B10E H8K 1.467 1_555 1_555 H11E B7K 1.485 1_555 1_555 B11E H12E 1.214 1_555 1_555 B11E H9K 1.351 1_555 1_555 B11E B9K 1.582 1_555 1_555 B11E B11K 2.016 1_555 1_555 H12E B8K 1.342 1_555 1_555 B6K H7K 1.214 1_555 1_555 B7K H8K 1.214 1_555 1_555 B8K H9K 1.214 1_555 1_555 B8K B9K 1.780 1_555 1_555 B8K B11K 1.781 1_555 1_555 B9K H10K 1.214 1_555 1_555 B9K B11K 1.782 1_555 1_555 B10K H11K 1.214 1_555 1_555 B11K H12K 1.214 1_555 1_555 #END data_CSD_CIF_DAWCEK _audit_creation_date 2006-02-13 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD DAWCEK _database_code_depnum_ccdc_archive 'CCDC 288452' _chemical_formula_sum 'C24 H48 N8 Na2' _chemical_formula_moiety ; C24 H48 N8 Na1 1+,Na1 1- ; _journal_coden_Cambridge 4 _journal_volume 127 _journal_year 2005 _journal_page_first 12416 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "M.Y.Redko" "J.E.Jackson" "R.H.Huang" "J.L.Dye" _chemical_name_systematic ; (1,4,7,10,13,16,21,24-Octaazapentacyclo(8.8.8.2^4,7^.2^13,16^.2^21,24^)dotriac ontane)-sodium sodide ; _cell_volume 3087.829 _exptl_crystal_density_diffrn 1.064 _diffrn_ambient_temperature 173 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.1463 _refine_ls_wR_factor_gt 0.1463 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_Int_Tables_number 56 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2-y,z 3 -x,1/2+y,1/2-z 4 1/2+x,-y,1/2-z 5 -x,-y,-z 6 -1/2+x,-1/2+y,-z 7 x,-1/2-y,-1/2+z 8 -1/2-x,y,-1/2+z _cell_length_a 11.074(2) _cell_length_b 14.812(3) _cell_length_c 18.825(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 N 0.68 Na 1.97 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 0.75000 0.25000 0.36621(15) Na2 Na 0.25000 0.25000 0.1644(2) N1 N 0.9210(7) 0.4106(6) 0.3664(5) C1 C 0.8594(15) 0.4853(9) 0.4011(11) H1 H 0.920(9) 0.537(8) 0.406(6) H2 H 0.803(6) 0.520(5) 0.370(4) C2 C 0.7804(15) 0.4581(11) 0.4625(9) H3 H 0.736(6) 0.514(5) 0.472(4) H4 H 0.841(13) 0.426(8) 0.507(7) N2 N 0.6905(7) 0.3931(5) 0.4426(4) C3 C 0.6012(14) 0.4267(10) 0.3913(7) H5 H 0.580(7) 0.481(5) 0.404(4) H6 H 0.639(7) 0.426(5) 0.346(4) C4 C 0.4917(13) 0.3688(10) 0.3920(5) H7 H 0.467(6) 0.365(4) 0.342(4) H8 H 0.427(6) 0.387(4) 0.422(4) C5 C 0.6285(15) 0.3601(13) 0.5056(7) H9 H 0.679(6) 0.330(5) 0.544(4) H10 H 0.575(8) 0.398(6) 0.519(4) C6 C 0.5598(12) 0.2754(14) 0.4879(5) H11 H 0.492(8) 0.260(7) 0.508(4) H12 H 0.619(7) 0.221(5) 0.496(3) N3 N 0.5256(6) 0.2754(6) 0.4109(3) C7 C 0.4302(9) 0.2099(11) 0.3950(6) H13 H 0.406(6) 0.224(5) 0.344(4) H14 H 0.372(6) 0.228(4) 0.427(3) C8 C 1.0302(12) 0.3846(11) 0.4074(8) H15 H 1.007(10) 0.414(8) 0.454(6) H16 H 1.094(8) 0.441(6) 0.393(4) C9 C 0.8787(7) 0.2636(6) 0.2200(4) H17 H 0.949(5) 0.249(3) 0.261(3) H18 H 0.922(5) 0.282(4) 0.179(3) C10 C 0.6844(7) 0.3241(6) 0.2016(4) H19 H 0.699(6) 0.323(4) 0.154(4) H20 H 0.640(5) 0.377(3) 0.209(2) N4 N 0.7942(5) 0.3319(4) 0.2446(3) C11 C 0.8472(11) 0.4223(7) 0.2421(6) H21 H 0.766(9) 0.462(6) 0.256(5) H22 H 0.869(6) 0.434(4) 0.195(3) C12 C 0.9546(12) 0.4289(8) 0.2911(8) H23 H 1.020(7) 0.384(5) 0.274(4) H24 H 0.974(9) 0.484(6) 0.290(5) N1A N 0.5790(7) 0.0894(6) 0.3664(5) C1A C 0.6406(15) 0.0147(9) 0.4011(11) H1A H 0.580(9) -0.037(8) 0.406(6) H2A H 0.697(6) -0.020(5) 0.370(4) C2A C 0.7196(15) 0.0419(11) 0.4625(9) H3A H 0.764(6) -0.014(5) 0.472(4) H4A H 0.659(13) 0.074(8) 0.507(7) N2A N 0.8095(7) 0.1069(5) 0.4426(4) C3A C 0.8988(14) 0.0733(10) 0.3913(7) H5A H 0.920(7) 0.019(5) 0.404(4) H6A H 0.861(7) 0.074(5) 0.346(4) C4A C 1.0083(13) 0.1312(10) 0.3920(5) H7A H 1.033(6) 0.135(4) 0.342(4) H8A H 1.073(6) 0.113(4) 0.422(4) C5A C 0.8715(15) 0.1399(13) 0.5056(7) H9A H 0.821(6) 0.170(5) 0.544(4) H10A H 0.925(8) 0.102(6) 0.519(4) C6A C 0.9402(12) 0.2246(14) 0.4879(5) H11A H 1.008(8) 0.240(7) 0.508(4) H12A H 0.881(7) 0.279(5) 0.496(3) N3A N 0.9744(6) 0.2246(6) 0.4109(3) C7A C 1.0698(9) 0.2901(11) 0.3950(6) H13A H 1.094(6) 0.276(5) 0.344(4) H14A H 1.128(6) 0.272(4) 0.427(3) C8A C 0.4698(12) 0.1154(11) 0.4074(8) H15A H 0.493(10) 0.086(8) 0.454(6) H16A H 0.406(8) 0.059(6) 0.393(4) C9A C 0.6213(7) 0.2364(6) 0.2200(4) H17A H 0.551(5) 0.251(3) 0.261(3) H18A H 0.578(5) 0.218(4) 0.179(3) C10A C 0.8156(7) 0.1759(6) 0.2016(4) H19A H 0.801(6) 0.177(4) 0.154(4) H20A H 0.860(5) 0.123(3) 0.209(2) N4A N 0.7058(5) 0.1681(4) 0.2446(3) C11A C 0.6528(11) 0.0777(7) 0.2421(6) H21A H 0.734(9) 0.038(6) 0.256(5) H22A H 0.631(6) 0.066(4) 0.195(3) C12A C 0.5454(12) 0.0711(8) 0.2911(8) H23A H 0.480(7) 0.116(5) 0.274(4) H24A H 0.526(9) 0.016(6) 0.290(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Na1 N1 3.041 1_555 1_555 N1 C1 1.455 1_555 1_555 C1 H1 1.022 1_555 1_555 H2 C1 0.999 1_555 1_555 C2 C1 1.505 1_555 1_555 H3 C2 0.979 1_555 1_555 H4 C2 1.174 1_555 1_555 N2 Na1 2.645 1_555 1_555 C3 N2 1.469 1_555 1_555 H5 C3 0.871 1_555 1_555 H6 C3 0.950 1_555 1_555 C4 C3 1.485 1_555 1_555 H7 C4 0.982 1_555 1_555 H8 C4 0.951 1_555 1_555 C5 N2 1.455 1_555 1_555 H9 C5 1.017 1_555 1_555 H10 C5 0.854 1_555 1_555 C6 C5 1.505 1_555 1_555 H11 C6 0.871 1_555 1_555 H12 C6 1.050 1_555 1_555 N3 Na1 2.650 1_555 1_555 C7 N3 1.465 1_555 1_555 H13 C7 1.018 1_555 1_555 H14 C7 0.922 1_555 1_555 C8 N1 1.485 1_555 1_555 H15 C8 1.013 1_555 1_555 H16 C8 1.127 1_555 1_555 C9 H17 1.117 1_555 1_555 H18 C9 0.949 1_555 1_555 C10 H19 0.911 1_555 1_555 H20 C10 0.935 1_555 1_555 N4 Na1 2.637 1_555 1_555 C11 N4 1.463 1_555 1_555 H21 C11 1.106 1_555 1_555 H22 C11 0.935 1_555 1_555 C12 N1 1.490 1_555 1_555 H23 C12 1.035 1_555 1_555 H24 C12 0.844 1_555 1_555 N1A Na1 3.041 1_555 1_555 C1A N1A 1.455 1_555 1_555 H1A C1A 1.022 1_555 1_555 H2A C1A 0.999 1_555 1_555 C2A C1A 1.505 1_555 1_555 H3A C2A 0.979 1_555 1_555 H4A C2A 1.174 1_555 1_555 N2A Na1 2.645 1_555 1_555 C3A N2A 1.469 1_555 1_555 H5A C3A 0.871 1_555 1_555 H6A C3A 0.950 1_555 1_555 C4A C3A 1.485 1_555 1_555 H7A C4A 0.982 1_555 1_555 H8A C4A 0.951 1_555 1_555 C5A N2A 1.455 1_555 1_555 H9A C5A 1.017 1_555 1_555 H10A C5A 0.854 1_555 1_555 C6A C5A 1.505 1_555 1_555 H11A C6A 0.871 1_555 1_555 H12A C6A 1.050 1_555 1_555 N3A Na1 2.650 1_555 1_555 C7A C8 1.485 1_555 1_555 H13A C7A 1.018 1_555 1_555 H14A C7A 0.922 1_555 1_555 C8A C7 1.485 1_555 1_555 H15A C8A 1.013 1_555 1_555 H16A C8A 1.127 1_555 1_555 C9A C10 1.515 1_555 1_555 H17A C9A 1.117 1_555 1_555 H18A C9A 0.949 1_555 1_555 C10A C9 1.515 1_555 1_555 H19A C10A 0.911 1_555 1_555 H20A C10A 0.935 1_555 1_555 N4A Na1 2.637 1_555 1_555 C11A N4A 1.463 1_555 1_555 H21A C11A 1.106 1_555 1_555 H22A C11A 0.935 1_555 1_555 C12A N1A 1.490 1_555 1_555 H23A C12A 1.035 1_555 1_555 H24A C12A 0.844 1_555 1_555 C2 N2 1.435 1_555 1_555 C4 N3 1.477 1_555 1_555 C6 N3 1.498 1_555 1_555 C9 N4 1.454 1_555 1_555 C10 N4 1.465 1_555 1_555 C11 C12 1.508 1_555 1_555 N1A C8A 1.485 1_555 1_555 C2A N2A 1.435 1_555 1_555 C4A N3A 1.477 1_555 1_555 C6A N3A 1.498 1_555 1_555 N3A C7A 1.465 1_555 1_555 C9A N4A 1.454 1_555 1_555 C10A N4A 1.465 1_555 1_555 C11A C12A 1.508 1_555 1_555 #END data_CSD_CIF_DEKJUY _audit_creation_date 1986-07-24 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD DEKJUY _chemical_formula_sum 'C38 H42 Li1 N1 O8' _chemical_formula_moiety ; C30 H22 Li1 O8 1-,C8 H20 N1 1+ ; _journal_coden_Cambridge 9 _journal_volume 24 _journal_year 1985 _journal_page_first 2315 _journal_name_full 'Inorg.Chem. ' loop_ _publ_author_name "F.Teixidor" "A.Llobet" "J.Casabo" "X.Solans" "M.Font-Altaba" "M.Aguilo" _chemical_name_systematic ; Tetraethylammonium bis(1,2-bis(2-hydroxyphenyl)-1,3-propanedionato)-lithium ; _cell_volume 3532.967 _exptl_crystal_colour 'yellow' _exptl_crystal_density_diffrn 1.22 _exptl_special_details ; H81 makes a close contact with C107 and has been deleted. H4 and H26 have been deleted because of suspected error ; _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.073 _refine_ls_wR_factor_gt 0.073 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 -1/2+x,-1/2-y,-1/2+z _cell_length_a 17.278(4) _cell_length_b 18.571(4) _cell_length_c 11.015(3) _cell_angle_alpha 90 _cell_angle_beta 91.62(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 0.84 N 0.68 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.2046(14) -0.1185(12) 0.9773(20) O1 O 0.1940(6) -0.1130(5) 1.1436(8) C1 C 0.1562(8) -0.1558(7) 1.2129(13) C2 C 0.1106(8) -0.2121(7) 1.1706(11) C3 C 0.1001(7) -0.2302(7) 1.0477(14) O2 O 0.1336(5) -0.1960(5) 0.9597(8) C4 C 0.1663(6) -0.1424(5) 1.3475(6) C5 C 0.2231(6) -0.0941(5) 1.3884(6) C6 C 0.2347(6) -0.0820(5) 1.5126(6) C7 C 0.1894(6) -0.1182(5) 1.5959(6) C8 C 0.1326(6) -0.1665(6) 1.5550(6) C9 C 0.1211(6) -0.1786(5) 1.4309(6) O3 O 0.2688(6) -0.0566(5) 1.3125(8) O4 O 0.3106(5) -0.1211(5) 0.9395(9) C10 C 0.3491(8) -0.0706(8) 0.8921(11) C11 C 0.3178(8) -0.0070(7) 0.8440(12) C12 C 0.2375(9) 0.0085(8) 0.8413(11) O5 O 0.1856(5) -0.0355(5) 0.8787(8) C13 C 0.0488(4) -0.2915(4) 1.0055(9) C14 C 0.0375(4) -0.3061(4) 0.8820(9) C15 C -0.0124(4) -0.3613(4) 0.8444(9) C16 C -0.0510(4) -0.4019(4) 0.9303(9) C17 C -0.0397(4) -0.3874(4) 1.0538(9) C18 C 0.0102(4) -0.3322(4) 1.0914(9) O6 O 0.0716(5) -0.2678(5) 0.7954(7) C19 C 0.4366(5) -0.0793(6) 0.8987(9) C20 C 0.4676(5) -0.1336(6) 0.9729(9) C21 C 0.5476(5) -0.1414(6) 0.9864(9) C22 C 0.5968(5) -0.0948(6) 0.9258(9) C23 C 0.5659(5) -0.0405(6) 0.8517(9) C24 C 0.4858(5) -0.0327(6) 0.8381(9) O7 O 0.4227(6) -0.1811(5) 1.0340(9) C25 C 0.2071(7) 0.0806(4) 0.7964(8) C26 C 0.1275(7) 0.0885(4) 0.7757(8) C27 C 0.0972(7) 0.1548(4) 0.7385(8) C28 C 0.1465(7) 0.2132(4) 0.7220(8) C29 C 0.2261(7) 0.2054(4) 0.7427(8) C30 C 0.2563(7) 0.1391(4) 0.7799(8) O8 O 0.0758(5) 0.0343(6) 0.7879(11) N1 N 0.1341(4) 0.1330(4) 0.2525(7) C31 C 0.0757(6) 0.1334(6) 0.3493(10) C32 C 0.0640(6) 0.0624(6) 0.4153(10) C33 C 0.2138(7) 0.1124(6) 0.3129(11) C34 C 0.2430(7) 0.1540(9) 0.4227(14) C35 C 0.1364(6) 0.2081(5) 0.2034(9) C36 C 0.1905(6) 0.2186(5) 0.0992(10) C37 C 0.1137(7) 0.0782(5) 0.1541(11) C38 C 0.0371(7) 0.0972(7) 0.0885(12) H1 H 0.0872(38) -0.2409(35) 1.2153(59) H2 H 0.2524(35) -0.0784(34) 1.2402(56) H3 H 0.2323(36) -0.0541(33) 1.5495(57) H4 H 0.2016(38) -0.1228(33) 1.6774(59) H5 H 0.1045(35) -0.1964(32) 1.6126(55) H6 H 0.0839(35) -0.2131(33) 1.4291(55) H7 H 0.1077(34) -0.2345(34) 0.8449(55) H8 H -0.0166(36) -0.3723(33) 0.7836(55) H9 H -0.0649(35) -0.4442(32) 0.9035(58) H10 H -0.0777(34) -0.4237(34) 1.1072(56) H11 H 0.3448(35) 0.0401(33) 0.8044(59) H12 H 0.5721(35) -0.1743(34) 1.0529(58) H13 H 0.6420(36) -0.1023(33) 0.9375(58) H14 H 0.5933(35) -0.0111(33) 0.8026(55) H15 H 0.4614(35) 0.0097(34) 0.7880(59) H16 H 0.1025(35) -0.0027(33) 0.8490(56) H17 H 0.0399(34) 0.1529(33) 0.7073(58) H18 H 0.1239(35) 0.2502(34) 0.7135(57) H19 H 0.2707(35) 0.2475(34) 0.7443(58) H20 H 0.3123(36) 0.1358(35) 0.8003(58) H21 H 0.0812(36) 0.1792(35) 0.3915(56) H22 H 0.0316(37) 0.1897(35) 0.3436(60) H23 H 0.0538(36) 0.0202(34) 0.3628(60) H24 H 0.1049(37) 0.0509(33) 0.4815(58) H25 H 0.0154(38) 0.0681(34) 0.4646(59) H26 H 0.1992(37) 0.0571(35) 0.2741(59) H27 H 0.2424(38) 0.1092(36) 0.2496(58) H28 H 0.2431(35) 0.2026(35) 0.4021(57) H29 H 0.2115(37) 0.1548(36) 0.4608(60) H30 H 0.1489(35) 0.2422(33) 0.2757(56) H31 H 0.2506(34) 0.2052(33) 0.1272(56) H32 H 0.1684(35) 0.1834(34) 0.0048(58) H33 H 0.1799(36) 0.2584(35) 0.0648(59) H34 H 0.1715(35) 0.0815(34) 0.1182(58) H35 H 0.1024(39) 0.0258(36) 0.1826(62) H36 H 0.0400(37) 0.1431(35) 0.0264(58) H37 H -0.0058(38) 0.0844(36) 0.0445(59) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 O1 1.849 1_555 1_555 O1 C1 1.292 1_555 1_555 C1 C2 1.382 1_555 1_555 C2 C3 1.402 1_555 1_555 C3 O2 1.308 1_555 1_555 O2 Li1 1.897 1_555 1_555 C4 C1 1.509 1_555 1_555 C5 C4 1.395 1_555 1_555 C6 C5 1.395 1_555 1_555 C7 C6 1.395 1_555 1_555 C8 C7 1.395 1_555 1_555 C9 C4 1.395 1_555 1_555 O3 C5 1.358 1_555 1_555 O4 Li1 1.890 1_555 1_555 C10 O4 1.271 1_555 1_555 C11 C10 1.397 1_555 1_555 C12 C11 1.416 1_555 1_555 O5 Li1 1.909 1_555 1_555 C13 C3 1.508 1_555 1_555 C14 C13 1.395 1_555 1_555 C15 C14 1.395 1_555 1_555 C16 C15 1.394 1_555 1_555 C17 C16 1.395 1_555 1_555 C18 C13 1.395 1_555 1_555 O6 C14 1.340 1_555 1_555 C19 C10 1.520 1_555 1_555 C20 C19 1.395 1_555 1_555 C21 C20 1.394 1_555 1_555 C22 C21 1.396 1_555 1_555 C23 C22 1.394 1_555 1_555 C24 C19 1.396 1_555 1_555 O7 C20 1.365 1_555 1_555 C25 C12 1.516 1_555 1_555 C26 C25 1.395 1_555 1_555 C27 C26 1.395 1_555 1_555 C28 C27 1.394 1_555 1_555 C29 C28 1.395 1_555 1_555 C30 C25 1.395 1_555 1_555 O8 C26 1.355 1_555 1_555 N1 C31 1.489 1_555 1_555 C31 C32 1.522 1_555 1_555 C32 H23 0.987 1_555 1_555 C33 N1 1.560 1_555 1_555 C34 C33 1.510 1_555 1_555 C35 N1 1.497 1_555 1_555 C36 C35 1.513 1_555 1_555 C37 N1 1.521 1_555 1_555 C38 C37 1.531 1_555 1_555 H1 C2 0.839 1_555 1_555 H2 O3 0.930 1_555 1_555 H3 C6 0.661 1_555 1_555 H4 C7 0.920 1_555 1_555 H5 C8 0.982 1_555 1_555 H6 C9 0.907 1_555 1_555 H7 O6 1.024 1_555 1_555 H8 C15 0.702 1_555 1_555 H9 C16 0.871 1_555 1_555 H10 C17 1.120 1_555 1_555 H11 C11 1.088 1_555 1_555 H12 C21 1.035 1_555 1_555 H13 C22 0.800 1_555 1_555 H14 C23 0.911 1_555 1_555 H15 C24 1.044 1_555 1_555 H16 O8 1.058 1_555 1_555 H17 C27 1.039 1_555 1_555 H18 C28 0.795 1_555 1_555 H19 C29 1.098 1_555 1_555 H20 C30 0.989 1_555 1_555 H21 C31 0.973 1_555 1_555 H22 C31 1.294 1_555 1_555 H24 C32 1.024 1_555 1_555 H25 C32 1.018 1_555 1_555 H26 C33 1.138 1_555 1_555 H27 C33 0.868 1_555 1_555 H28 C34 0.931 1_555 1_555 H29 C34 0.697 1_555 1_555 H30 C35 1.035 1_555 1_555 H31 C36 1.103 1_555 1_555 H32 C36 1.277 1_555 1_555 H33 C36 0.848 1_555 1_555 H34 C37 1.086 1_555 1_555 H35 C37 1.043 1_555 1_555 H36 C38 1.095 1_555 1_555 H37 C38 0.906 1_555 1_555 C8 C9 1.394 1_555 1_555 C12 O5 1.289 1_555 1_555 C17 C18 1.395 1_555 1_555 C23 C24 1.395 1_555 1_555 C29 C30 1.394 1_555 1_555 #END data_CSD_CIF_DONYAG _audit_creation_date 1987-03-27 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD DONYAG _database_code_depnum_ccdc_archive 'CCDC 1144195' _chemical_formula_sum 'C38 H100 Cl1 Li3 N6 Si6' _chemical_formula_moiety ; C18 H46 Cl1 Li2 N6 1+,C20 H54 Li1 Si6 1- ; _journal_coden_Cambridge 182 _journal_year 1986 _journal_page_first 969 _journal_name_full 'Chem.Commun. ' loop_ _publ_author_name "N.H.Buttrus" "C.Eaborn" "P.B.Hitchcock" "J.D.Smith" "J.G.Stamper" "A.C.Sullivan" _chemical_name_systematic ; (\m~2~-Chloro)-bis((1,1,4,7,7-pentamethyl-diethylenetriamine-N,N',N'')-lithium ) bis(tris(trimethylsilyl)-methyl)-lithium ; _cell_volume 3035.112 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 0.95 _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.12 _refine_ls_wR_factor_gt 0.12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,y,1/2-z 3 -x,-y,-z 4 -1/2+x,-y,-1/2+z _cell_length_a 16.987(5) _cell_length_b 9.527(5) _cell_length_c 18.788(1) _cell_angle_alpha 90 _cell_angle_beta 93.43(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.31 Cl 0.99 Li 1.10 N 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Cl1 Cl 1.00000 0.50000 0.50000 N1 N 1.0099(8) 0.2184(12) 0.6291(6) N2 N 1.0636(10) 0.5679(14) 0.6869(7) N3 N 0.9104(8) 0.4478(14) 0.6730(7) C1 C 1.0153(13) 0.1487(19) 0.5643(9) C2 C 1.0716(13) 0.1794(25) 0.6761(11) C3 C 0.9500(17) 0.199(2) 0.6630(14) C4 C 0.905(1) 0.2904(19) 0.6934(10) C5 C 0.9292(15) 0.5462(20) 0.7239(12) C6 C 1.0149(20) 0.5730(18) 0.7466(9) C7 C 1.1383(17) 0.5226(43) 0.7060(24) C8 C 1.0777(23) 0.6770(28) 0.6671(16) C9 C 0.8397(12) 0.4866(21) 0.6386(15) Li1 Li 1.0063(18) 0.4440(26) 0.6121(14) H1 H 1.01700 0.03400 0.56900 H2 H 0.95400 0.16600 0.53200 H3 H 1.05700 0.18300 0.52900 H4 H 1.08400 0.07300 0.68900 H5 H 1.13200 0.23000 0.66700 H6 H 1.06300 0.23100 0.73300 H7 H 0.94700 0.09400 0.68400 H8 H 0.90000 0.17600 0.60900 H9 H 0.94200 0.29200 0.75000 H10 H 0.84800 0.26400 0.70700 H11 H 0.88500 0.52400 0.76800 H12 H 0.89700 0.65100 0.70100 H13 H 1.02800 0.47900 0.78300 H14 H 1.02000 0.66400 0.77900 H15 H 1.17400 0.60600 0.74700 H16 H 1.14800 0.42800 0.73700 H17 H 1.18400 0.52200 0.66500 H18 H 1.09500 0.76600 0.68400 H19 H 1.08400 0.67600 0.60200 H20 H 1.00000 0.71500 0.65000 H21 H 0.78600 0.48600 0.67100 H22 H 0.83700 0.59500 0.61300 H23 H 0.81900 0.41800 0.59100 Si1 Si -0.1594(3) -0.0172(5) -0.0987(2) Si2 Si -0.1694(3) 0.0592(4) 0.0585(2) Si3 Si -0.1266(3) -0.2425(4) 0.0157(2) C10 C -0.1252(8) -0.0477(10) -0.0082(6) C11 C -0.2521(9) -0.0972(18) -0.1332(8) C12 C -0.1804(11) 0.1793(15) -0.1203(8) C13 C -0.0887(10) -0.0595(15) -0.1665(7) C14 C -0.2781(9) 0.0772(15) 0.0442(9) C15 C -0.1271(11) 0.2486(13) 0.0634(9) C16 C -0.1544(10) 0.0019(16) 0.1539(7) C17 C -0.223(1) -0.3068(15) 0.0461(9) C18 C -0.051(1) -0.2886(13) 0.0863(8) C19 C -0.1046(10) -0.3622(14) -0.0616(8) Li2 Li 0.00000 0.00000 0.00000 H24 H -0.28200 -0.04900 -0.19200 H25 H -0.25200 -0.20800 -0.12500 H26 H -0.30100 -0.05600 -0.09800 H27 H -0.20200 0.19800 -0.17300 H28 H -0.22600 0.22000 -0.08300 H29 H -0.12800 0.24400 -0.10700 H30 H -0.11000 -0.03400 -0.22000 H31 H -0.03300 0.00900 -0.15700 H32 H -0.06800 -0.16500 -0.16300 H33 H -0.30300 0.14500 0.08900 H34 H -0.29600 0.13100 -0.00400 H35 H -0.31000 -0.02100 0.04700 H36 H -0.15200 0.31400 0.10100 H37 H -0.06200 0.24700 0.07100 H38 H -0.13800 0.30000 0.00900 H39 H -0.18400 0.06600 0.18900 H40 H -0.18100 -0.10900 0.15900 H41 H -0.09300 -0.01000 0.17000 H42 H -0.22200 -0.41900 0.05800 H43 H -0.24400 -0.25100 0.09000 H44 H -0.27100 -0.29500 0.00100 H45 H -0.05400 -0.39600 0.10000 H46 H 0.00700 -0.26100 0.07000 H47 H -0.06200 -0.22500 0.13500 H48 H -0.10700 -0.47000 -0.04800 H49 H -0.15000 -0.34400 -0.10700 H50 H -0.04800 -0.33700 -0.08300 Li1B Li 0.9937(18) 0.5560(26) 0.3879(14) N1B N 0.9901(8) 0.7816(12) 0.3709(6) N2B N 0.9364(10) 0.4321(14) 0.3131(7) N3B N 1.0896(8) 0.5522(14) 0.3270(7) C1B C 0.9847(13) 0.8513(19) 0.4357(9) C2B C 0.9284(13) 0.8206(25) 0.3239(11) C3B C 1.0500(17) 0.801(2) 0.3370(14) C6B C 0.9851(20) 0.4270(18) 0.2534(9) C7B C 0.8617(17) 0.4774(43) 0.2940(24) C8B C 0.9223(23) 0.3230(28) 0.3329(16) C4B C 1.095(1) 0.7096(19) 0.3066(10) C5B C 1.0708(15) 0.4538(20) 0.2761(12) C9B C 1.1603(12) 0.5134(21) 0.3614(15) H1B H 0.98300 0.96600 0.43100 H2B H 1.04600 0.83400 0.46800 H3B H 0.94300 0.81700 0.47100 H4B H 0.91600 0.92700 0.31100 H5B H 0.86800 0.77000 0.33300 H6B H 0.93700 0.76900 0.26700 H7B H 1.05300 0.90600 0.31600 H8B H 1.10000 0.82400 0.39100 H13B H 0.97200 0.52100 0.21700 H14B H 0.98000 0.33600 0.22100 H15B H 0.82600 0.39400 0.25300 H16B H 0.85200 0.57200 0.26300 H17B H 0.81600 0.47800 0.33500 H18B H 0.90500 0.23400 0.31600 H19B H 0.91600 0.32400 0.39800 H20B H 1.00000 0.28500 0.35000 H9B H 1.05800 0.70800 0.25000 H10B H 1.15200 0.73600 0.29300 H11B H 1.11500 0.47600 0.23200 H12B H 1.10300 0.34900 0.29900 H21B H 1.21400 0.51400 0.32900 H22B H 1.16300 0.40500 0.38700 H23B H 1.18100 0.58200 0.40900 C10B C 0.1252(8) 0.0477(10) 0.0082(6) Si1B Si 0.1594(3) 0.0172(5) 0.0987(2) Si2B Si 0.1694(3) -0.0592(4) -0.0585(2) Si3B Si 0.1266(3) 0.2425(4) -0.0157(2) C11B C 0.2521(9) 0.0972(18) 0.1332(8) C12B C 0.1804(11) -0.1793(15) 0.1203(8) C13B C 0.0887(10) 0.0595(15) 0.1665(7) C14B C 0.2781(9) -0.0772(15) -0.0442(9) C15B C 0.1271(11) -0.2486(13) -0.0634(9) C16B C 0.1544(10) -0.0019(16) -0.1539(7) C17B C 0.223(1) 0.3068(15) -0.0461(9) C18B C 0.051(1) 0.2886(13) -0.0863(8) C19B C 0.1046(10) 0.3622(14) 0.0616(8) H24B H 0.28200 0.04900 0.19200 H25B H 0.25200 0.20800 0.12500 H26B H 0.30100 0.05600 0.09800 H27B H 0.20200 -0.19800 0.17300 H28B H 0.22600 -0.22000 0.08300 H29B H 0.12800 -0.24400 0.10700 H30B H 0.11000 0.03400 0.22000 H31B H 0.03300 -0.00900 0.15700 H32B H 0.06800 0.16500 0.16300 H33B H 0.30300 -0.14500 -0.08900 H34B H 0.29600 -0.13100 0.00400 H35B H 0.31000 0.02100 -0.04700 H36B H 0.15200 -0.31400 -0.10100 H37B H 0.06200 -0.24700 -0.07100 H38B H 0.13800 -0.30000 -0.00900 H39B H 0.18400 -0.06600 -0.18900 H40B H 0.18100 0.10900 -0.15900 H41B H 0.09300 0.01000 -0.17000 H42B H 0.22200 0.41900 -0.05800 H43B H 0.24400 0.25100 -0.09000 H44B H 0.27100 0.29500 -0.00100 H45B H 0.05400 0.39600 -0.10000 H46B H -0.00700 0.26100 -0.07000 H47B H 0.06200 0.22500 -0.13500 H48B H 0.10700 0.47000 0.04800 H49B H 0.15000 0.34400 0.10700 H50B H 0.04800 0.33700 0.08300 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cl1 Li1 2.169 1_555 1_555 N1 C1 1.395 1_555 1_555 N2 C6 1.434 1_555 1_555 N3 C4 1.552 1_555 1_555 C1 H1 1.097 1_555 1_555 C2 N1 1.380 1_555 1_555 C3 N1 1.246 1_555 1_555 C4 C3 1.312 1_555 1_555 C5 N3 1.363 1_555 1_555 C6 C5 1.514 1_555 1_555 C7 N2 1.368 1_555 1_555 C8 N2 1.134 1_555 1_555 C9 N3 1.380 1_555 1_555 Li1 N1 2.173 1_555 1_555 H2 C1 1.185 1_555 1_555 H3 C1 1.051 1_555 1_555 H4 C2 1.060 1_555 1_555 H5 C2 1.156 1_555 1_555 H6 C2 1.194 1_555 1_555 H7 C3 1.078 1_555 1_555 H8 C3 1.302 1_555 1_555 H9 C4 1.203 1_555 1_555 H10 C4 1.047 1_555 1_555 H11 C5 1.170 1_555 1_555 H12 C5 1.205 1_555 1_555 H13 C6 1.141 1_555 1_555 H14 C6 1.060 1_555 1_555 H15 C7 1.240 1_555 1_555 H16 C7 1.080 1_555 1_555 H17 C7 1.126 1_555 1_555 H18 C8 0.946 1_555 1_555 H19 C8 1.234 1_555 1_555 H20 C8 1.388 1_555 1_555 H21 C9 1.127 1_555 1_555 H22 C9 1.139 1_555 1_555 H23 C9 1.146 1_555 1_555 Si1 C10 1.787 1_555 1_555 Si2 C10 1.812 1_555 1_555 Si3 C10 1.910 1_555 1_555 C10 Li2 2.171 1_555 1_555 C11 Si1 1.833 1_555 1_555 C12 Si1 1.944 1_555 1_555 C13 Si1 1.847 1_555 1_555 C14 Si2 1.858 1_555 1_555 C15 Si2 1.942 1_555 1_555 C16 Si2 1.876 1_555 1_555 C17 Si3 1.869 1_555 1_555 C18 Si3 1.843 1_555 1_555 C19 Si3 1.901 1_555 1_555 Li2 C10B 2.171 1_555 1_555 H24 C11 1.274 1_555 1_555 H25 C11 1.067 1_555 1_555 H26 C11 1.161 1_555 1_555 H27 C12 1.050 1_555 1_555 H28 C12 1.143 1_555 1_555 H29 C12 1.099 1_555 1_555 H30 C13 1.076 1_555 1_555 H31 C13 1.154 1_555 1_555 H32 C13 1.066 1_555 1_555 H33 C14 1.161 1_555 1_555 H34 C14 1.069 1_555 1_555 H35 C14 1.084 1_555 1_555 H36 C15 1.050 1_555 1_555 H37 C15 1.107 1_555 1_555 H38 C15 1.138 1_555 1_555 H39 C16 1.049 1_555 1_555 H40 C16 1.155 1_555 1_555 H41 C16 1.074 1_555 1_555 H42 C17 1.092 1_555 1_555 H43 C17 1.061 1_555 1_555 H44 C17 1.146 1_555 1_555 H45 C18 1.057 1_555 1_555 H46 C18 1.082 1_555 1_555 H47 C18 1.122 1_555 1_555 H48 C19 1.060 1_555 1_555 H49 C19 1.129 1_555 1_555 H50 C19 1.091 1_555 1_555 Li1B Cl1 2.169 1_555 1_555 N1B Li1B 2.173 1_555 1_555 N2B Li1B 2.038 1_555 1_555 N3B Li1B 2.046 1_555 1_555 C1B N1B 1.395 1_555 1_555 C2B N1B 1.380 1_555 1_555 C3B N1B 1.246 1_555 1_555 C6B N2B 1.434 1_555 1_555 C7B N2B 1.368 1_555 1_555 C8B N2B 1.134 1_555 1_555 C4B N3B 1.552 1_555 1_555 C5B N3B 1.363 1_555 1_555 C9B N3B 1.380 1_555 1_555 H1B C1B 1.097 1_555 1_555 H2B C1B 1.185 1_555 1_555 H3B C1B 1.051 1_555 1_555 H4B C2B 1.060 1_555 1_555 H5B C2B 1.156 1_555 1_555 H6B C2B 1.194 1_555 1_555 H7B C3B 1.078 1_555 1_555 H8B C3B 1.302 1_555 1_555 H13B C6B 1.141 1_555 1_555 H14B C6B 1.060 1_555 1_555 H15B C7B 1.240 1_555 1_555 H16B C7B 1.080 1_555 1_555 H17B C7B 1.126 1_555 1_555 H18B C8B 0.946 1_555 1_555 H19B C8B 1.234 1_555 1_555 H20B C8B 1.388 1_555 1_555 H9B C4B 1.203 1_555 1_555 H10B C4B 1.047 1_555 1_555 H11B C5B 1.170 1_555 1_555 H12B C5B 1.205 1_555 1_555 H21B C9B 1.127 1_555 1_555 H22B C9B 1.139 1_555 1_555 H23B C9B 1.146 1_555 1_555 C10B Si1B 1.787 1_555 1_555 Si1B C11B 1.833 1_555 1_555 Si2B C10B 1.812 1_555 1_555 Si3B C10B 1.910 1_555 1_555 C11B H24B 1.274 1_555 1_555 C12B Si1B 1.944 1_555 1_555 C13B Si1B 1.847 1_555 1_555 C14B Si2B 1.858 1_555 1_555 C15B Si2B 1.942 1_555 1_555 C16B Si2B 1.876 1_555 1_555 C17B Si3B 1.869 1_555 1_555 C18B Si3B 1.843 1_555 1_555 C19B Si3B 1.901 1_555 1_555 H25B C11B 1.067 1_555 1_555 H26B C11B 1.161 1_555 1_555 H27B C12B 1.050 1_555 1_555 H28B C12B 1.143 1_555 1_555 H29B C12B 1.099 1_555 1_555 H30B C13B 1.076 1_555 1_555 H31B C13B 1.154 1_555 1_555 H32B C13B 1.066 1_555 1_555 H33B C14B 1.161 1_555 1_555 H34B C14B 1.069 1_555 1_555 H35B C14B 1.084 1_555 1_555 H36B C15B 1.050 1_555 1_555 H37B C15B 1.107 1_555 1_555 H38B C15B 1.138 1_555 1_555 H39B C16B 1.049 1_555 1_555 H40B C16B 1.155 1_555 1_555 H41B C16B 1.074 1_555 1_555 H42B C17B 1.092 1_555 1_555 H43B C17B 1.061 1_555 1_555 H44B C17B 1.146 1_555 1_555 H45B C18B 1.057 1_555 1_555 H46B C18B 1.082 1_555 1_555 H47B C18B 1.122 1_555 1_555 H48B C19B 1.060 1_555 1_555 H49B C19B 1.129 1_555 1_555 H50B C19B 1.091 1_555 1_555 N2 Li1 2.038 1_555 1_555 N3 Li1 2.046 1_555 1_555 C3B C4B 1.312 1_555 1_555 C6B C5B 1.514 1_555 1_555 #END data_CSD_CIF_EHEHEE _audit_creation_date 2002-12-11 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD EHEHEE _database_code_depnum_ccdc_archive 'CCDC 196539' _chemical_formula_sum 'C38 H74 Li2 O4 Si4' _chemical_formula_moiety ; C16 H32 Li1 O4 1+,C22 H42 Li1 Si4 1- ; _journal_coden_Cambridge 579 _journal_volume 21 _journal_year 2002 _journal_page_first 4335 _journal_name_full 'Organometallics ' loop_ _publ_author_name "M.Westerhausen" "S.Schneiderbauer" "N.Makropoulos" "M.Warchhold" "H.Noth" "H.Piotrowski" "K.Karaghiosoff" _chemical_name_systematic ; tetrakis(Tetrahydrofuran)-lithium bis(\h^5^-1,3-bis(trimethylsilyl)cyclopentadienyl)-lithium ; _cell_volume 4755.004 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.008 _exptl_crystal_description 'prism' _diffrn_ambient_temperature 183 _refine_special_details ; One of the trimethylsilyl groups is disordered over two positions with occupancy 0.56:0.44. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_gt 0.0578 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,1/2+z 3 1/2+x,-y,z 4 1/2-x,y,1/2+z _cell_length_a 20.956(3) _cell_length_b 11.525(2) _cell_length_c 19.688(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.38 O 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Si1 Si -0.61070(4) -0.72538(7) 0.46020(4) Si2 Si -0.48153(4) -0.54142(7) 0.69840(5) Si3 Si -0.73646(4) -0.69158(8) 0.71288(6) Si4 Si -0.52326(4) -1.00548(8) 0.75405(6) O1 O -0.18590(13) -0.9495(2) 0.95472(15) O2 O -0.17140(12) -0.6750(2) 0.94758(13) O3 O -0.23103(13) -0.8225(2) 0.81935(12) O4 O -0.30703(12) -0.7781(2) 0.95144(13) Li1 Li -0.2213(3) -0.8072(5) 0.9165(3) Li2 Li -0.5808(2) -0.7873(4) 0.6382(2) C1 C -0.55632(13) -0.7130(2) 0.53294(15) C2 C -0.55336(14) -0.6206(2) 0.58040(14) H1 H -0.58020 -0.55640 0.58010 C3 C -0.50439(14) -0.6393(2) 0.62788(14) C4 C -0.47542(14) -0.7457(3) 0.60906(15) H2 H -0.44110 -0.78030 0.63120 C5 C -0.50635(15) -0.7902(2) 0.55226(16) H3 H -0.49610 -0.85920 0.53040 C6 C -0.69080(18) -0.6660(4) 0.48332(19) H4 H -0.70970 -0.71380 0.51780 H5 H -0.71770 -0.66540 0.44390 H6 H -0.68610 -0.58830 0.50020 C7 C -0.6185(2) -0.8811(3) 0.4345(2) H7 H -0.63800 -0.92430 0.47070 H8 H -0.57700 -0.91250 0.42520 H9 H -0.64450 -0.88650 0.39450 C8 C -0.58042(19) -0.6409(3) 0.38549(18) H10 H -0.60600 -0.65820 0.34630 H11 H -0.53690 -0.66190 0.37660 H12 H -0.58290 -0.55940 0.39520 C9 C -0.39878(16) -0.5751(3) 0.7258(2) H13 H -0.39640 -0.65460 0.74020 H14 H -0.38710 -0.52540 0.76290 H15 H -0.37000 -0.56280 0.68860 C10 C -0.5343(2) -0.5559(4) 0.7751(2) H16 H -0.53010 -0.63250 0.79370 H17 H -0.57790 -0.54280 0.76220 H18 H -0.52200 -0.49970 0.80860 C11 C -0.4876(2) -0.3876(3) 0.6688(3) H19 H -0.47660 -0.33640 0.70550 H20 H -0.53050 -0.37210 0.65430 H21 H -0.45880 -0.37550 0.63160 C12 C -0.59278(13) -0.9351(2) 0.71575(16) C13 C -0.62550(16) -0.9673(2) 0.65551(16) H22 H -0.61470 -1.02910 0.62740 C14 C -0.67661(15) -0.8909(3) 0.64527(17) H23 H -0.70500 -0.89350 0.60900 C15 C -0.67814(13) -0.8093(2) 0.69863(17) C16 C -0.62676(14) -0.8375(2) 0.74115(15) H24 H -0.61630 -0.79770 0.78070 C17 C -0.5475(2) -1.1327(4) 0.8070(3) H25 H -0.57250 -1.10640 0.84490 H26 H -0.51010 -1.17190 0.82340 H27 H -0.57240 -1.18530 0.78000 C18 C -0.4793(2) -0.9001(4) 0.8090(3) H28 H -0.50570 -0.87860 0.84680 H29 H -0.46900 -0.83220 0.78300 H30 H -0.44080 -0.93540 0.82530 C19 C -0.4682(2) -1.0583(4) 0.6860(3) H31 H -0.49010 -1.11340 0.65790 H32 H -0.43180 -1.09480 0.70650 H33 H -0.45450 -0.99390 0.65880 C20 C -0.8168(7) -0.747(2) 0.706(2) H34 H -0.82280 -0.80810 0.73880 H35 H -0.82390 -0.77630 0.66140 H36 H -0.84660 -0.68540 0.71550 C21? C -0.8137(9) -0.7381(19) 0.662(2) H37? H -0.83020 -0.80910 0.68040 H38? H -0.80280 -0.74970 0.61490 H39? H -0.84530 -0.67830 0.66540 C22 C -0.7271(11) -0.637(2) 0.8088(12) H40 H -0.73210 -0.70220 0.83910 H41 H -0.75910 -0.58020 0.81850 H42 H -0.68550 -0.60410 0.81490 C23? C -0.749(2) -0.672(4) 0.7984(14) H43? H -0.76450 -0.74330 0.81780 H44? H -0.77960 -0.61180 0.80520 H45? H -0.70940 -0.65140 0.81980 C24 C -0.7192(2) -0.5539(3) 0.6671(2) H46 H -0.72600 -0.56490 0.61930 H47 H -0.67570 -0.53180 0.67500 H48 H -0.74710 -0.49400 0.68340 C25 C -0.1850(3) -0.6083(5) 1.0076(4) H49 H -0.22930 -0.58350 1.00720 H50 H -0.17820 -0.65560 1.04780 C26 C -0.1439(2) -0.5092(4) 1.0094(3) H51 H -0.13040 -0.49280 1.05550 H52 H -0.16540 -0.44140 0.99120 C27 C -0.0888(2) -0.5410(4) 0.9666(3) H53 H -0.07660 -0.47650 0.93760 H54 H -0.05250 -0.56200 0.99460 C28 C -0.1095(2) -0.6404(5) 0.9254(3) H55 H -0.11080 -0.61880 0.87780 H56 H -0.07970 -0.70420 0.93060 C29 C -0.2237(2) -0.7300(4) 0.7709(2) H57 H -0.18020 -0.70120 0.77100 H58 H -0.25240 -0.66640 0.78140 C30 C -0.2401(3) -0.7826(4) 0.7032(2) H59 H -0.26110 -0.72640 0.67410 H60 H -0.20210 -0.81100 0.68040 C31 C -0.2843(2) -0.8806(4) 0.7203(2) H61 H -0.28390 -0.93990 0.68540 H62 H -0.32770 -0.85340 0.72690 C32 C -0.2559(2) -0.9246(3) 0.7856(2) H63 H -0.28820 -0.96190 0.81330 H64 H -0.22200 -0.97980 0.77650 C33 C -0.1503(3) -0.9597(5) 1.0152(3) H65 H -0.17830 -0.97230 1.05370 H66 H -0.12550 -0.88990 1.02320 C34 C -0.1071(4) -1.0620(5) 1.0052(5) H67 H -0.06710 -1.03850 0.98460 H68 H -0.09820 -1.09990 1.04820 C35 C -0.1420(3) -1.1372(4) 0.9610(3) H69 H -0.16650 -1.19310 0.98700 H70 H -0.11320 -1.17890 0.93110 C36 C -0.1839(3) -1.0635(4) 0.9222(3) H71 H -0.22640 -1.09680 0.92060 H72 H -0.16820 -1.05620 0.87600 C37 C -0.3524(2) -0.7097(5) 0.9168(3) H73 H -0.36540 -0.74780 0.87510 H74 H -0.33430 -0.63480 0.90540 C38 C -0.4095(3) -0.6945(6) 0.9638(3) H75 H -0.41330 -0.61470 0.97890 H76 H -0.44880 -0.71710 0.94130 C39 C -0.3960(5) -0.7677(9) 1.0177(5) H77 H -0.42490 -0.83340 1.01630 H78 H -0.40340 -0.72650 1.05990 C40 C -0.3315(3) -0.8090(4) 1.0163(2) H79 H -0.30660 -0.77290 1.05210 H80 H -0.33030 -0.89250 1.02240 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Si1 C1 1.836 1_555 1_555 Si2 C3 1.852 1_555 1_555 Si3 C15 1.847 1_555 1_555 Si4 C12 1.830 1_555 1_555 O1 Li1 1.951 1_555 1_555 O2 Li1 1.947 1_555 1_555 O3 Li1 1.932 1_555 1_555 O4 Li1 1.953 1_555 1_555 Li2 C1 2.300 1_555 1_555 C1 C2 1.418 1_555 1_555 C2 Li2 2.306 1_555 1_555 H1 C2 0.929 1_555 1_555 C3 Li2 2.348 1_555 1_555 C4 Li2 2.331 1_555 1_555 H2 C4 0.931 1_555 1_555 C5 Li2 2.302 1_555 1_555 H3 C5 0.929 1_555 1_555 C6 Si1 1.869 1_555 1_555 H4 C6 0.960 1_555 1_555 H5 C6 0.959 1_555 1_555 H6 C6 0.960 1_555 1_555 C7 Si1 1.872 1_555 1_555 H7 C7 0.961 1_555 1_555 H8 C7 0.960 1_555 1_555 H9 C7 0.960 1_555 1_555 C8 Si1 1.875 1_555 1_555 H10 C8 0.960 1_555 1_555 H11 C8 0.960 1_555 1_555 H12 C8 0.960 1_555 1_555 C9 Si2 1.857 1_555 1_555 H13 C9 0.960 1_555 1_555 H14 C9 0.960 1_555 1_555 H15 C9 0.959 1_555 1_555 C10 Si2 1.879 1_555 1_555 H16 C10 0.960 1_555 1_555 H17 C10 0.960 1_555 1_555 H18 C10 0.960 1_555 1_555 C11 Si2 1.870 1_555 1_555 H19 C11 0.961 1_555 1_555 H20 C11 0.960 1_555 1_555 H21 C11 0.959 1_555 1_555 C12 Li2 2.301 1_555 1_555 C13 Li2 2.302 1_555 1_555 H22 C13 0.930 1_555 1_555 C14 Li2 2.340 1_555 1_555 H23 C14 0.930 1_555 1_555 C15 Li2 2.375 1_555 1_555 C16 Li2 2.317 1_555 1_555 H24 C16 0.930 1_555 1_555 C17 Si4 1.869 1_555 1_555 H25 C17 0.961 1_555 1_555 H26 C17 0.961 1_555 1_555 H27 C17 0.960 1_555 1_555 C18 Si4 1.869 1_555 1_555 H28 C18 0.960 1_555 1_555 H29 C18 0.960 1_555 1_555 H30 C18 0.959 1_555 1_555 C19 Si4 1.870 1_555 1_555 H31 C19 0.959 1_555 1_555 H32 C19 0.960 1_555 1_555 H33 C19 0.959 1_555 1_555 C20 Si3 1.806 1_555 1_555 H34 C20 0.964 1_555 1_555 H35 C20 0.952 1_555 1_555 H36 C20 0.964 1_555 1_555 C22 Si3 2.000 1_555 1_555 H40 C22 0.965 1_555 1_555 H41 C22 0.956 1_555 1_555 H42 C22 0.958 1_555 1_555 C24 Si3 1.860 1_555 1_555 H46 C24 0.960 1_555 1_555 H47 C24 0.959 1_555 1_555 H48 C24 0.960 1_555 1_555 C25 O2 1.438 1_555 1_555 H49 C25 0.971 1_555 1_555 H50 C25 0.972 1_555 1_555 C26 C25 1.431 1_555 1_555 H51 C26 0.969 1_555 1_555 H52 C26 0.971 1_555 1_555 C27 C26 1.476 1_555 1_555 H53 C27 0.972 1_555 1_555 H54 C27 0.970 1_555 1_555 C28 O2 1.426 1_555 1_555 H55 C28 0.970 1_555 1_555 H56 C28 0.970 1_555 1_555 C29 O3 1.439 1_555 1_555 H57 C29 0.970 1_555 1_555 H58 C29 0.970 1_555 1_555 C30 C29 1.504 1_555 1_555 H59 C30 0.970 1_555 1_555 H60 C30 0.971 1_555 1_555 C31 C30 1.499 1_555 1_555 H61 C31 0.969 1_555 1_555 H62 C31 0.971 1_555 1_555 C32 O3 1.448 1_555 1_555 H63 C32 0.970 1_555 1_555 H64 C32 0.970 1_555 1_555 C33 O1 1.410 1_555 1_555 H65 C33 0.969 1_555 1_555 H66 C33 0.971 1_555 1_555 C34 C33 1.499 1_555 1_555 H67 C34 0.970 1_555 1_555 H68 C34 0.971 1_555 1_555 C35 C34 1.429 1_555 1_555 H69 C35 0.970 1_555 1_555 H70 C35 0.970 1_555 1_555 C36 O1 1.462 1_555 1_555 H71 C36 0.970 1_555 1_555 H72 C36 0.971 1_555 1_555 C37 O4 1.411 1_555 1_555 H73 C37 0.970 1_555 1_555 H74 C37 0.969 1_555 1_555 C38 C37 1.523 1_555 1_555 H75 C38 0.970 1_555 1_555 H76 C38 0.971 1_555 1_555 C39 C38 1.385 1_555 1_555 H77 C39 0.970 1_555 1_555 H78 C39 0.969 1_555 1_555 C40 O4 1.421 1_555 1_555 H79 C40 0.971 1_555 1_555 H80 C40 0.970 1_555 1_555 C1 C5 1.426 1_555 1_555 C2 C3 1.405 1_555 1_555 C3 C4 1.418 1_555 1_555 C4 C5 1.391 1_555 1_555 C12 C13 1.419 1_555 1_555 C12 C16 1.422 1_555 1_555 C13 C14 1.401 1_555 1_555 C14 C15 1.410 1_555 1_555 C15 C16 1.402 1_555 1_555 C27 C28 1.469 1_555 1_555 C31 C32 1.505 1_555 1_555 C35 C36 1.441 1_555 1_555 C39 C40 1.433 1_555 1_555 #END data_CSD_CIF_EWICET _audit_creation_date 2012-02-03 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD EWICET _database_code_depnum_ccdc_archive 'CCDC 813710' _chemical_formula_sum 'C78 H96 Li8 O9.5' _chemical_formula_moiety ; C60 H60 Li7 O5 1-,C16 H32 Li1 O4 1+,0.5(C4 H8 O1) ; _journal_coden_Cambridge 38 _journal_volume 333 _journal_year 2011 _journal_page_first 1008 _journal_name_full 'Science ' loop_ _publ_author_name "A.V.Zabula" "A.S.Filatov" "S.N.Spisak" "A.Yu.Rogachev" "M.A.Petrukhina" _chemical_name_systematic ; tetrakis(Tetrahydrofuran)-lithium (\m~6~-\h^6^,\h^6^,\h^6^,\h^6^,\h^6^,\h^6^-corannulene)-(\m~6~-\h^6^,\h^6^,\h^ 6^,\h^6^,\h^6^,\h^3^-corannulene)-pentakis(tetrahydrofuran)-hepta-lithium tetrahydrofuran solvate ; _cell_volume 6655.623 _exptl_crystal_colour 'purple' _exptl_crystal_density_diffrn 1.239 _exptl_crystal_description 'block' _diffrn_ambient_temperature 100 _refine_special_details ; C102 and C1X disordered over two sites with occupancies 0.76:0.24; C118 and C2X disordered over two sites with occupancies 0.62:0.38; C131 and C3X disordered over two sites with occupancies 0.75:0.25. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_gt 0.0468 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 17.050(2) _cell_length_b 17.646(2) _cell_length_c 22.486(3) _cell_angle_alpha 88.720(2) _cell_angle_beta 79.877(2) _cell_angle_gamma 88.189(2) _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.71 H 0.23 Li 1.68 O 0.62 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.60058(19) 0.59136(17) 0.26103(14) Li2 Li 0.7157(2) 0.55440(18) 0.35018(14) Li3 Li 0.8608(2) 0.46364(18) 0.28576(15) Li4 Li 0.83864(19) 0.44290(17) 0.15409(14) Li5 Li 0.67714(18) 0.52019(17) 0.13945(14) Li6 Li 0.5049(2) 0.4013(2) 0.32256(16) Li7 Li 0.95716(18) 0.64667(17) 0.08763(13) Li8 Li 0.34238(18) 0.85651(17) 0.22485(13) Li9 Li 0.36826(18) 1.01965(17) 0.18002(13) Li10 Li 0.22995(18) 1.12124(17) 0.24044(13) Li11 Li 0.11627(18) 1.01702(17) 0.32454(13) Li12 Li 0.18534(18) 0.85478(17) 0.31497(13) Li13 Li 0.00925(19) 0.99249(18) 0.18798(14) Li14 Li 0.47400(18) 0.86835(17) 0.36827(13) Li15 Li 0.04945(19) 0.74788(18) 0.53591(14) Li16 Li 0.55413(18) 0.74997(17) 0.99834(13) O1 O 0.41476(9) 0.37894(8) 0.38544(6) O2 O 0.54359(9) 0.30032(8) 0.30370(6) O3 O 0.92174(7) 0.72794(7) 0.14193(5) O4 O 0.94112(8) 0.69120(7) 0.00742(5) O5 O 1.07482(7) 0.65344(8) 0.07607(6) O6 O -0.08892(8) 1.03862(8) 0.17089(6) O7 O 0.04418(7) 0.94560(7) 0.11136(5) O8 O 0.44582(7) 0.96156(7) 0.41413(6) O9 O 0.58999(7) 0.88241(7) 0.34815(5) O10 O 0.47242(7) 0.78430(7) 0.43120(6) O11 O -0.03549(7) 0.78665(7) 0.49534(5) O12 O 0.10804(9) 0.67789(8) 0.47791(6) O13 O -0.00307(8) 0.69820(7) 0.60820(6) O14 O 0.11048(7) 0.82337(7) 0.56481(6) O15 O 0.46835(7) 0.80414(7) 0.96948(6) O16 O 0.50609(7) 0.66756(7) 1.04873(5) O17 O 0.62104(8) 0.70639(8) 0.92808(5) O18 O 0.61395(7) 0.81568(7) 1.03858(5) O19 O 0.2881(1) 0.57654(9) 0.34269(7) C1 C 0.62719(10) 0.70106(9) 0.20952(8) H1 H 0.58230 0.72940 0.19490 C2 C 0.63781(10) 0.71164(10) 0.27157(8) H2 H 0.59950 0.74660 0.29740 C3 C 0.70067(10) 0.67567(9) 0.29754(8) C4 C 0.73480(11) 0.68094(10) 0.35150(8) H3 H 0.70430 0.71050 0.38590 C5 C 0.80900(11) 0.64348(10) 0.35972(8) H4 H 0.82600 0.64770 0.39980 C6 C 0.85816(11) 0.59813(10) 0.31445(8) C7 C 0.93622(11) 0.5636(1) 0.30403(8) H5 H 0.96560 0.55890 0.33870 C8 C 0.97295(11) 0.5300(1) 0.24672(8) H6 H 1.02610 0.50350 0.24440 C9 C 0.93506(10) 0.52950(9) 0.19446(8) C10 C 0.95542(10) 0.51166(10) 0.13171(8) H7 H 1.00590 0.48800 0.11780 C11 C 0.90211(10) 0.52798(10) 0.08726(8) H8 H 0.92020 0.51420 0.04640 C12 C 0.82424(10) 0.56373(9) 0.10286(7) C13 C 0.76214(10) 0.59414(10) 0.07319(8) H9 H 0.76650 0.58530 0.02890 C14 C 0.6932(1) 0.63843(9) 0.10381(8) H10 H 0.65430 0.66010 0.07910 C15 C 0.67991(10) 0.65398(9) 0.16711(8) C16 C 0.73837(10) 0.61596(9) 0.19605(7) C17 C 0.74759(10) 0.62510(9) 0.25587(8) C18 C 0.81967(10) 0.59035(9) 0.26347(8) C19 C 0.85521(10) 0.55933(9) 0.20827(8) C20 C 0.80499(10) 0.57522(9) 0.16654(7) C21 C 0.49505(11) 0.51387(10) 0.26129(8) H11 H 0.44580 0.53130 0.25100 C22 C 0.50850(11) 0.52629(10) 0.32355(8) H12 H 0.46880 0.55390 0.35020 C23 C 0.57827(11) 0.49887(10) 0.34598(8) C24 C 0.60776(12) 0.49116(10) 0.40201(8) H13 H 0.57600 0.51570 0.43850 C25 C 0.68251(12) 0.45179(11) 0.40853(8) H14 H 0.69780 0.44920 0.44950 C26 C 0.73508(11) 0.41653(10) 0.35932(8) C27 C 0.80686(12) 0.36963(11) 0.34924(9) H15 H 0.83260 0.35600 0.38480 C28 C 0.84006(11) 0.33582(11) 0.29168(10) H16 H 0.88750 0.30060 0.28990 C29 C 0.80637(11) 0.34711(10) 0.23807(9) C30 C 0.81817(12) 0.31925(10) 0.17765(9) H17 H 0.86330 0.28210 0.16510 C31 C 0.76546(12) 0.33773(10) 0.13511(9) H18 H 0.77810 0.31480 0.09410 C32 C 0.69420(11) 0.38496(10) 0.14908(8) C33 C 0.62687(11) 0.40808(10) 0.12247(8) H19 H 0.62660 0.39390 0.07970 C34 C 0.55917(11) 0.45292(10) 0.15400(8) H20 H 0.51660 0.47000 0.13080 C35 C 0.55205(10) 0.47701(10) 0.21538(8) C36 C 0.62249(10) 0.45634(9) 0.23863(8) C37 C 0.63405(10) 0.46492(9) 0.29815(8) C38 C 0.70590(11) 0.42841(10) 0.30425(8) C39 C 0.73887(10) 0.39762(10) 0.24873(8) C40 C 0.68754(10) 0.41450(9) 0.20820(8) C41 C 0.38667(14) 0.42100(12) 0.43989(9) H21 H 0.36330 0.47080 0.43000 H22 H 0.43110 0.42960 0.46180 C42 C 0.32447(15) 0.37315(13) 0.47764(10) H23 H 0.27020 0.39100 0.47310 H24 H 0.32910 0.37440 0.52090 C43 C 0.34233(15) 0.29362(13) 0.45284(10) H25 H 0.38460 0.26710 0.47110 H26 H 0.29400 0.26270 0.45940 C44 C 0.37016(14) 0.31101(12) 0.38666(10) H27 H 0.40420 0.26890 0.36710 H28 H 0.32420 0.31940 0.36560 C45 C 0.59832(19) 0.25828(14) 0.33446(11) H29 H 0.57210 0.24240 0.37550 H30 H 0.64490 0.28890 0.33790 C46 C 0.62358(19) 0.18902(15) 0.29464(14) H31 H 0.67810 0.17060 0.29810 H32 H 0.58610 0.14720 0.30540 C47 C 0.62039(13) 0.21997(13) 0.23350(11) H33 H 0.61400 0.17920 0.20530 H34 H 0.66900 0.24810 0.21710 C48 C 0.54906(12) 0.27141(11) 0.24396(9) H35 H 0.55470 0.31350 0.21380 H36 H 0.50060 0.24340 0.24070 C49 C 0.94286(11) 0.73729(10) 0.20113(8) H37 H 1.00030 0.74750 0.19740 H38 H 0.93100 0.69110 0.22650 C50 C 0.89246(11) 0.80423(12) 0.22840(9) H39 H 0.87890 0.79870 0.27290 H40 H 0.92040 0.85240 0.21810 C51 C 0.81869(11) 0.80147(11) 0.19968(8) H41 H 0.77950 0.76630 0.22220 H42 H 0.79310 0.85240 0.19790 C52 C 0.85094(10) 0.77294(10) 0.13719(8) H43 H 0.81110 0.74170 0.12270 H44 H 0.86400 0.81600 0.10850 C53 C 1.12017(11) 0.63108(12) 0.12234(9) H45 H 1.08600 0.60620 0.15690 H46 H 1.14480 0.67550 0.13700 C54 C 1.18322(12) 0.57607(13) 0.09101(10) H47 H 1.16160 0.52500 0.08860 H48 H 1.22990 0.57220 0.11170 C55 C 1.20453(13) 0.61334(15) 0.02838(10) H49 H 1.24480 0.65260 0.02800 H50 H 1.22510 0.57530 -0.00260 C56 C 1.12607(12) 0.64806(12) 0.01793(9) H51 H 1.13410 0.69900 -0.00110 H52 H 1.10190 0.61590 -0.00910 C57 C 0.93682(13) 0.64583(11) -0.04424(8) H53 H 0.88390 0.62280 -0.03990 H54 H 0.97810 0.60460 -0.04810 C58 C 0.95043(13) 0.69787(11) -0.09921(8) H55 H 0.89990 0.70950 -0.11390 H56 H 0.98920 0.67470 -0.13230 C59 C 0.98334(12) 0.76917(11) -0.07665(8) H57 H 1.04210 0.76550 -0.08070 H58 H 0.96820 0.81510 -0.09860 C60 C 0.94349(12) 0.76936(11) -0.01134(8) H59 H 0.97450 0.79860 0.01310 H60 H 0.88900 0.79200 -0.00710 C61 C 0.40153(10) 0.8158(1) 0.30232(8) H61 H 0.41630 0.76380 0.30590 C62 C 0.45645(10) 0.86557(10) 0.26157(8) H62 H 0.50480 0.84360 0.24060 C63 C 0.44077(10) 0.94517(10) 0.25203(7) C64 C 0.48024(10) 1.00978(10) 0.22182(7) H63 H 0.53250 1.00100 0.19440 C65 C 0.44756(10) 1.08759(10) 0.22813(7) H64 H 0.47890 1.12900 0.20500 C66 C 0.37157(10) 1.10707(9) 0.26349(7) C67 C 0.32548(10) 1.17455(10) 0.28420(7) H65 H 0.34600 1.22480 0.26830 C68 C 0.25129(10) 1.17329(10) 0.32723(7) H66 H 0.22380 1.22290 0.33940 C69 C 0.21473(10) 1.10520(9) 0.35304(7) C70 C 0.15027(10) 1.08333(10) 0.40001(7) H67 H 0.11230 1.12390 0.41890 C71 C 0.13659(10) 1.00569(10) 0.42108(7) H68 H 0.08950 0.99600 0.45340 C72 C 0.18725(10) 0.94167(10) 0.39849(7) C73 C 0.19793(10) 0.86295(10) 0.41277(7) H69 H 0.15670 0.83880 0.44400 C74 C 0.26424(10) 0.81516(10) 0.38269(8) H70 H 0.26530 0.76010 0.39400 C75 C 0.32694(10) 0.84262(10) 0.33664(7) C76 C 0.3119(1) 0.92043(9) 0.32215(7) C77 C 0.36354(10) 0.96689(9) 0.28380(7) C78 C 0.33124(10) 1.04084(9) 0.28768(7) C79 C 0.25887(10) 1.03959(9) 0.32792(7) C80 C 0.2471(1) 0.96530(9) 0.34950(7) C81 C 0.27384(10) 0.78767(10) 0.16700(8) H71 H 0.28420 0.73160 0.16530 C82 C 0.32809(10) 0.83575(10) 0.12705(8) H72 H 0.37360 0.81100 0.09940 C83 C 0.31891(10) 0.91702(10) 0.12423(7) C84 C 0.35373(10) 0.97964(10) 0.08787(7) H73 H 0.40300 0.96930 0.05750 C85 C 0.32215(10) 1.05709(10) 0.09327(8) H74 H 0.35160 1.09720 0.06700 C86 C 0.2504(1) 1.07946(10) 0.13416(7) C87 C 0.19921(10) 1.14515(10) 0.14737(8) H75 H 0.21630 1.19410 0.12660 C88 C 0.12488(11) 1.14523(10) 0.19148(8) H76 H 0.09430 1.19440 0.19930 C89 C 0.09462(10) 1.07935(9) 0.22541(7) C90 C 0.02532(10) 1.05661(10) 0.26772(7) H77 H -0.01270 1.09470 0.28360 C91 C 0.01019(10) 0.9766(1) 0.28794(7) H78 H -0.03890 0.96590 0.31350 C92 C 0.06602(10) 0.9144(1) 0.27081(7) C93 C 0.07102(10) 0.83332(10) 0.27785(7) H79 H 0.02650 0.80780 0.30510 C94 C 0.13663(10) 0.7859(1) 0.24693(7) H80 H 0.13400 0.72970 0.25340 C95 C 0.20496(10) 0.81558(10) 0.20809(7) C96 C 0.20125(10) 0.89643(9) 0.20632(7) C97 C 0.25292(10) 0.94284(10) 0.16776(7) C98 C 0.22063(10) 1.01664(10) 0.17100(7) C99 C 0.14888(10) 1.01585(9) 0.21210(7) C100 C 0.13691(10) 0.94158(9) 0.23396(7) C101 C -0.12841(14) 1.10648(13) 0.19479(12) H81 H -0.09010 1.14760 0.19430 H82 H -0.15640 1.09810 0.23670 C102 C -0.18830(16) 1.12606(15) 0.15213(12) H83 H -0.23330 1.15860 0.17180 H84 H -0.16230 1.15070 0.11410 C103 C -0.21447(12) 1.04567(12) 0.14191(10) H85 H -0.24990 1.02520 0.17790 H86 H -0.24110 1.04360 0.10630 C104 C -0.13554(15) 1.00591(15) 0.13141(12) H87 H -0.14150 0.95100 0.14040 H88 H -0.10940 1.01250 0.08880 C105 C 0.08982(13) 0.99492(12) 0.06657(9) H89 H 0.10680 1.03990 0.08600 H90 H 0.05740 1.01230 0.03610 C106 C 0.16078(12) 0.94880(13) 0.03753(9) H91 H 0.20600 0.95350 0.05930 H92 H 0.17780 0.96430 -0.00530 C107 C 0.13024(13) 0.86856(13) 0.04272(10) H93 H 0.10160 0.85780 0.00930 H94 H 0.17450 0.83080 0.04250 C108 C 0.07431(11) 0.86796(11) 0.10287(8) H95 H 0.03010 0.83310 0.10220 H96 H 0.10310 0.85170 0.13580 C109 C 0.37231(11) 0.97941(12) 0.45552(9) H97 H 0.37820 0.96660 0.49760 H98 H 0.32780 0.95050 0.44540 C110 C 0.35673(12) 1.06362(12) 0.44825(9) H99 H 0.32930 1.08590 0.48660 H100 H 0.32430 1.07430 0.41650 C111 C 0.44050(13) 1.09366(12) 0.42996(9) H101 H 0.43990 1.14290 0.40810 H102 H 0.46670 1.09930 0.46550 C112 C 0.48095(12) 1.03163(10) 0.38892(9) H103 H 0.47120 1.04020 0.34710 H104 H 0.53920 1.03010 0.38840 C113 C 0.63550(11) 0.88092(11) 0.39637(8) H105 H 0.63300 0.83060 0.41680 H106 H 0.61480 0.91990 0.42650 C114 C 0.72008(11) 0.89731(12) 0.36674(9) H107 H 0.74970 0.85030 0.35200 H108 H 0.74910 0.92250 0.39490 C115 C 0.70754(11) 0.95018(11) 0.31455(9) H109 H 0.69490 1.00280 0.32830 H110 H 0.75490 0.94990 0.28200 C116 C 0.63672(10) 0.91509(11) 0.29413(8) H111 H 0.60490 0.95420 0.27590 H112 H 0.65480 0.87540 0.26390 C117 C 0.49544(12) 0.70591(12) 0.4173(1) H113 H 0.54610 0.69220 0.43110 H114 H 0.50260 0.69790 0.37320 C118 C 0.4278(2) 0.65745(18) 0.45072(15) H115 H 0.38670 0.64960 0.42550 H116 H 0.44820 0.60760 0.46330 C119 C 0.3968(2) 0.70441(14) 0.50288(13) H117 H 0.42530 0.69160 0.53670 H118 H 0.33930 0.69570 0.51660 C120 C 0.40938(12) 0.78550(11) 0.48344(8) H119 H 0.36000 0.80880 0.47290 H120 H 0.42510 0.81490 0.51620 C121 C -0.02572(13) 0.62013(11) 0.61387(10) H121 H 0.01870 0.58720 0.62350 H122 H -0.04070 0.60280 0.57590 C122 C -0.09577(13) 0.61807(12) 0.66458(10) H123 H -0.10060 0.56740 0.68440 H124 H -0.14600 0.63190 0.65020 C123 C -0.07494(13) 0.67757(12) 0.70697(10) H125 H -0.12330 0.69780 0.73350 H126 H -0.03720 0.65650 0.73230 C124 C -0.03667(11) 0.73796(11) 0.66340(9) H127 H -0.07690 0.77680 0.65540 H128 H 0.00570 0.76310 0.68000 C125 C -0.11447(11) 0.75516(11) 0.50360(8) H129 H -0.14100 0.75840 0.54640 H130 H -0.11130 0.70140 0.49150 C126 C -0.15958(10) 0.80300(11) 0.46329(8) H131 H -0.18440 0.84890 0.48420 H132 H -0.20130 0.77370 0.44930 C127 C -0.09354(11) 0.82331(11) 0.41122(8) H133 H -0.07960 0.78050 0.38330 H134 H -0.10860 0.86850 0.38830 C128 C -0.02616(11) 0.83962(12) 0.44400(9) H135 H 0.02600 0.83110 0.41740 H136 H -0.03000 0.89270 0.45790 C129 C 0.08288(11) 0.90167(11) 0.57207(9) H137 H 0.04210 0.90720 0.60900 H138 H 0.05930 0.91950 0.53680 C130 C 0.15537(14) 0.94667(13) 0.57694(13) H139 H 0.18060 0.96680 0.53690 H140 H 0.14110 0.98950 0.60490 C131 C 0.20938(17) 0.89033(16) 0.60108(14) H141 H 0.19620 0.88620 0.64570 H142 H 0.26590 0.90420 0.58920 C132 C 0.19313(11) 0.81713(11) 0.57190(9) H143 H 0.22830 0.81130 0.53220 H144 H 0.20210 0.77290 0.59800 C133 C 0.17557(16) 0.62979(15) 0.48259(11) H145 H 0.19100 0.63390 0.52280 H146 H 0.22160 0.64300 0.45110 C134 C 0.14830(19) 0.55108(15) 0.47348(12) H147 H 0.12310 0.52760 0.51230 H148 H 0.19330 0.51800 0.45440 C135 C 0.08716(16) 0.56564(15) 0.43098(14) H149 H 0.10620 0.54300 0.39090 H150 H 0.03490 0.54440 0.44850 C136 C 0.08138(15) 0.65150(14) 0.42604(11) H151 H 0.11560 0.67000 0.38870 H152 H 0.02570 0.66890 0.42560 C137 C 0.47576(11) 0.66013(11) 1.11258(8) H153 H 0.46050 0.71040 1.13050 H154 H 0.51600 0.63530 1.13390 C138 C 0.40342(13) 0.61127(13) 1.1163(1) H155 H 0.35420 0.64320 1.11850 H156 H 0.39800 0.57730 1.15230 C139 C 0.41865(11) 0.56562(11) 1.05865(9) H157 H 0.42240 0.51060 1.06790 H158 H 0.37570 0.57510 1.03480 C140 C 0.49768(11) 0.59394(10) 1.02482(9) H159 H 0.54210 0.55930 1.03170 H160 H 0.49720 0.59760 0.98090 C141 C 0.39524(11) 0.77137(11) 0.95992(10) H161 H 0.37510 0.73540 0.99310 H162 H 0.40330 0.74430 0.92110 C142 C 0.33879(12) 0.83788(12) 0.95894(10) H163 H 0.31450 0.85290 1.00040 H164 H 0.29590 0.82640 0.93630 C143 C 0.39106(11) 0.89906(11) 0.92734(9) H165 H 0.37180 0.94980 0.94240 H166 H 0.39270 0.89830 0.88310 C144 C 0.47275(11) 0.87935(10) 0.94296(8) H167 H 0.51410 0.88060 0.90610 H168 H 0.48630 0.91610 0.97190 C145 C 0.68873(11) 0.65552(11) 0.92879(9) H169 H 0.67300 0.61030 0.95450 H170 H 0.73130 0.68120 0.94480 C146 C 0.71728(16) 0.63298(16) 0.86463(11) H171 H 0.76600 0.66040 0.84710 H172 H 0.72950 0.57780 0.86240 C147 C 0.65245(17) 0.65323(15) 0.83216(10) H173 H 0.61740 0.60970 0.83140 H174 H 0.67360 0.66930 0.79010 C148 C 0.60813(14) 0.71718(13) 0.86661(9) H175 H 0.62880 0.76650 0.84990 H176 H 0.55060 0.71590 0.86480 C149 C 0.58023(11) 0.86427(11) 1.08855(8) H177 H 0.54190 0.83630 1.11870 H178 H 0.55230 0.90910 1.07390 C150 C 0.65033(11) 0.88808(11) 1.11590(8) H179 H 0.66260 0.85080 1.14680 H180 H 0.64050 0.93870 1.13430 C151 C 0.71694(11) 0.88959(10) 1.06082(8) H181 H 0.71310 0.93590 1.03570 H182 H 0.77020 0.88610 1.07270 C152 C 0.70029(10) 0.81952(10) 1.02851(8) H183 H 0.72220 0.82370 0.98480 H184 H 0.72420 0.77380 1.04540 C153 C 0.28157(13) 0.50117(12) 0.32147(10) H185 H 0.24000 0.47360 0.34920 H186 H 0.33290 0.47260 0.31940 C154 C 0.25950(13) 0.50907(12) 0.25921(9) H187 H 0.21890 0.47220 0.25390 H188 H 0.30690 0.50170 0.22720 C155 C 0.22635(13) 0.58974(12) 0.25829(10) H189 H 0.23280 0.61090 0.21660 H190 H 0.16940 0.59290 0.27720 C156 C 0.27755(14) 0.62911(12) 0.29515(10) H191 H 0.32960 0.64140 0.27020 H192 H 0.25100 0.67660 0.31190 C157? C -0.2146(5) 1.1030(5) 0.1837(4) C158? C 0.4582(3) 0.6644(3) 0.4744(3) C159? C 0.2188(5) 0.8981(5) 0.5641(4) H193? H -0.25120 1.09110 0.22180 H194? H -0.23190 1.15220 0.16740 H195? H 0.44040 0.61430 0.46410 H196? H 0.49820 0.65610 0.50110 H197? H 0.25720 0.90760 0.59130 H198? H 0.24600 0.90700 0.52200 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 C1 2.251 1_555 1_555 Li2 C3 2.450 1_555 1_555 Li3 C6 2.470 1_555 1_555 Li4 C9 2.570 1_555 1_555 Li5 C12 2.632 1_555 1_555 Li6 O1 1.941 1_555 1_555 Li7 O3 1.917 1_555 1_555 Li8 C61 2.255 1_555 1_555 Li9 C63 2.527 1_555 1_555 Li10 C66 2.561 1_555 1_555 Li11 C69 2.498 1_555 1_555 Li12 C72 2.456 1_555 1_555 Li13 O6 1.933 1_555 1_555 Li14 O8 1.962 1_555 1_555 Li15 O11 1.942 1_555 1_555 Li16 O15 1.921 1_555 1_555 O1 C41 1.446 1_555 1_555 O2 Li6 1.911 1_555 1_555 O3 C49 1.453 1_555 1_555 O4 Li7 2.010 1_555 1_555 O5 Li7 1.984 1_555 1_555 O6 C101 1.424 1_555 1_555 O7 Li13 1.918 1_555 1_555 O8 C109 1.454 1_555 1_555 O9 Li14 1.972 1_555 1_555 O10 Li14 2.024 1_555 1_555 O11 C125 1.453 1_555 1_555 O12 Li15 1.939 1_555 1_555 O13 Li15 1.920 1_555 1_555 O14 Li15 1.909 1_555 1_555 O15 C141 1.442 1_555 1_555 O16 Li16 1.935 1_555 1_555 O17 Li16 1.938 1_555 1_555 O18 Li16 1.910 1_555 1_555 O19 C153 1.437 1_555 1_555 C1 H1 1.000 1_555 1_555 C2 Li1 2.264 1_555 1_555 H2 C2 1.001 1_555 1_555 C3 Li1 2.551 1_555 1_555 C4 Li2 2.268 1_555 1_555 H3 C4 1.000 1_555 1_555 C5 Li2 2.311 1_555 1_555 H4 C5 0.999 1_555 1_555 C6 Li2 2.558 1_555 1_555 C7 Li3 2.301 1_555 1_555 H5 C7 0.999 1_555 1_555 C8 Li3 2.303 1_555 1_555 H6 C8 1.000 1_555 1_555 C9 Li3 2.498 1_555 1_555 C10 Li4 2.337 1_555 1_555 H7 C10 0.949 1_555 1_555 C11 Li4 2.261 1_555 1_555 H8 C11 0.951 1_555 1_555 C12 Li4 2.427 1_555 1_555 C13 Li5 2.301 1_555 1_555 H9 C13 1.001 1_555 1_555 C14 Li5 2.226 1_555 1_555 H10 C14 0.999 1_555 1_555 C15 Li1 2.549 1_555 1_555 C16 Li1 2.583 1_555 1_555 C17 Li1 2.577 1_555 1_555 C18 Li2 2.479 1_555 1_555 C19 Li3 2.411 1_555 1_555 C20 Li4 2.397 1_555 1_555 C21 Li1 2.293 1_555 1_555 H11 C21 0.950 1_555 1_555 C22 Li1 2.242 1_555 1_555 H12 C22 0.951 1_555 1_555 C23 Li1 2.470 1_555 1_555 C24 Li2 2.304 1_555 1_555 H13 C24 0.999 1_555 1_555 C25 Li2 2.240 1_555 1_555 H14 C25 1.000 1_555 1_555 C26 Li2 2.454 1_555 1_555 C27 Li3 2.273 1_555 1_555 H15 C27 0.999 1_555 1_555 C28 Li3 2.291 1_555 1_555 H16 C28 1.000 1_555 1_555 C29 Li3 2.609 1_555 1_555 C30 Li4 2.257 1_555 1_555 H17 C30 1.001 1_555 1_555 C31 Li4 2.356 1_555 1_555 H18 C31 1.001 1_555 1_555 C32 Li4 2.717 1_555 1_555 C33 Li5 2.247 1_555 1_555 H19 C33 1.000 1_555 1_555 C34 Li5 2.338 1_555 1_555 H20 C34 1.001 1_555 1_555 C35 Li1 2.511 1_555 1_555 C36 Li1 2.450 1_555 1_555 C37 Li1 2.450 1_555 1_555 C38 Li2 2.495 1_555 1_555 C39 Li3 2.679 1_555 1_555 C40 Li4 2.706 1_555 1_555 C41 H21 0.990 1_555 1_555 H22 C41 0.991 1_555 1_555 C42 C41 1.505 1_555 1_555 H23 C42 0.990 1_555 1_555 H24 C42 0.990 1_555 1_555 C43 C42 1.524 1_555 1_555 H25 C43 0.991 1_555 1_555 H26 C43 0.990 1_555 1_555 C44 O1 1.437 1_555 1_555 H27 C44 0.990 1_555 1_555 H28 C44 0.990 1_555 1_555 C45 O2 1.435 1_555 1_555 H29 C45 0.991 1_555 1_555 H30 C45 0.990 1_555 1_555 C46 C45 1.537 1_555 1_555 H31 C46 0.990 1_555 1_555 H32 C46 0.989 1_555 1_555 C47 C46 1.477 1_555 1_555 H33 C47 0.991 1_555 1_555 H34 C47 0.990 1_555 1_555 C48 O2 1.434 1_555 1_555 H35 C48 0.990 1_555 1_555 H36 C48 0.990 1_555 1_555 C49 H37 0.990 1_555 1_555 H38 C49 0.990 1_555 1_555 C50 C49 1.514 1_555 1_555 H39 C50 0.990 1_555 1_555 H40 C50 0.991 1_555 1_555 C51 C50 1.514 1_555 1_555 H41 C51 0.991 1_555 1_555 H42 C51 0.990 1_555 1_555 C52 O3 1.442 1_555 1_555 H43 C52 0.990 1_555 1_555 H44 C52 0.991 1_555 1_555 C53 O5 1.443 1_555 1_555 H45 C53 0.989 1_555 1_555 H46 C53 0.990 1_555 1_555 C54 C53 1.514 1_555 1_555 H47 C54 0.991 1_555 1_555 H48 C54 0.990 1_555 1_555 C55 C54 1.530 1_555 1_555 H49 C55 0.990 1_555 1_555 H50 C55 0.989 1_555 1_555 C56 O5 1.442 1_555 1_555 H51 C56 0.990 1_555 1_555 H52 C56 0.990 1_555 1_555 C57 O4 1.439 1_555 1_555 H53 C57 0.990 1_555 1_555 H54 C57 0.991 1_555 1_555 C58 C57 1.512 1_555 1_555 H55 C58 0.990 1_555 1_555 H56 C58 0.991 1_555 1_555 C59 C58 1.526 1_555 1_555 H57 C59 0.990 1_555 1_555 H58 C59 0.990 1_555 1_555 C60 O4 1.433 1_555 1_555 H59 C60 0.990 1_555 1_555 H60 C60 0.989 1_555 1_555 C61 Li14 2.316 1_555 1_555 H61 C61 0.949 1_555 1_555 C62 Li8 2.254 1_555 1_555 H62 C62 0.951 1_555 1_555 C63 Li8 2.491 1_555 1_555 C64 Li9 2.272 1_555 1_555 H63 C64 1.000 1_555 1_555 C65 Li9 2.261 1_555 1_555 H64 C65 1.000 1_555 1_555 C66 Li9 2.465 1_555 1_555 C67 Li10 2.282 1_555 1_555 H65 C67 0.999 1_555 1_555 C68 Li10 2.266 1_555 1_555 H66 C68 1.000 1_555 1_555 C69 Li10 2.510 1_555 1_555 C70 Li11 2.250 1_555 1_555 H67 C70 1.000 1_555 1_555 C71 Li11 2.261 1_555 1_555 H68 C71 1.000 1_555 1_555 C72 Li11 2.550 1_555 1_555 C73 Li12 2.255 1_555 1_555 H69 C73 1.000 1_555 1_555 C74 Li12 2.287 1_555 1_555 H70 C74 0.999 1_555 1_555 C75 Li8 2.488 1_555 1_555 C76 Li8 2.450 1_555 1_555 C77 Li8 2.451 1_555 1_555 C78 Li9 2.426 1_555 1_555 C79 Li10 2.521 1_555 1_555 C80 Li11 2.532 1_555 1_555 C81 Li8 2.286 1_555 1_555 H71 C81 1.000 1_555 1_555 C82 Li8 2.293 1_555 1_555 H72 C82 1.000 1_555 1_555 C83 Li8 2.570 1_555 1_555 C84 Li9 2.261 1_555 1_555 H73 C84 1.000 1_555 1_555 C85 Li9 2.304 1_555 1_555 H74 C85 1.001 1_555 1_555 C86 Li9 2.600 1_555 1_555 C87 Li10 2.273 1_555 1_555 H75 C87 1.000 1_555 1_555 C88 Li10 2.286 1_555 1_555 H76 C88 1.001 1_555 1_555 C89 Li10 2.525 1_555 1_555 C90 Li11 2.261 1_555 1_555 H77 C90 0.949 1_555 1_555 C91 Li11 2.256 1_555 1_555 H78 C91 0.950 1_555 1_555 C92 Li11 2.456 1_555 1_555 C93 Li12 2.296 1_555 1_555 H79 C93 1.000 1_555 1_555 C94 Li12 2.259 1_555 1_555 H80 C94 1.000 1_555 1_555 C95 Li8 2.566 1_555 1_555 C96 Li8 2.587 1_555 1_555 C97 Li8 2.598 1_555 1_555 C98 Li9 2.563 1_555 1_555 C99 Li10 2.510 1_555 1_555 C100 Li11 2.426 1_555 1_555 C101 H81 0.990 1_555 1_555 H82 C101 0.989 1_555 1_555 C102 C101 1.546 1_555 1_555 H83 C102 0.989 1_555 1_555 H84 C102 0.990 1_555 1_555 C103 C102 1.535 1_555 1_555 H85 C103 0.990 1_555 1_555 H86 C103 0.989 1_555 1_555 C104 O6 1.433 1_555 1_555 H87 C104 0.990 1_555 1_555 H88 C104 0.989 1_555 1_555 C105 O7 1.451 1_555 1_555 H89 C105 0.990 1_555 1_555 H90 C105 0.991 1_555 1_555 C106 C105 1.495 1_555 1_555 H91 C106 0.990 1_555 1_555 H92 C106 0.991 1_555 1_555 C107 C106 1.519 1_555 1_555 H93 C107 0.990 1_555 1_555 H94 C107 0.990 1_555 1_555 C108 O7 1.453 1_555 1_555 H95 C108 0.990 1_555 1_555 H96 C108 0.990 1_555 1_555 C109 H97 0.989 1_555 1_555 H98 C109 0.989 1_555 1_555 C110 C109 1.512 1_555 1_555 H99 C110 0.989 1_555 1_555 H100 C110 0.988 1_555 1_555 C111 C110 1.524 1_555 1_555 H101 C111 0.989 1_555 1_555 H102 C111 0.990 1_555 1_555 C112 O8 1.451 1_555 1_555 H103 C112 0.991 1_555 1_555 H104 C112 0.991 1_555 1_555 C113 O9 1.439 1_555 1_555 H105 C113 0.989 1_555 1_555 H106 C113 0.989 1_555 1_555 C114 C113 1.512 1_555 1_555 H107 C114 0.990 1_555 1_555 H108 C114 0.990 1_555 1_555 C115 C114 1.523 1_555 1_555 H109 C115 0.990 1_555 1_555 H110 C115 0.990 1_555 1_555 C116 O9 1.449 1_555 1_555 H111 C116 0.990 1_555 1_555 H112 C116 0.991 1_555 1_555 C117 O10 1.452 1_555 1_555 H113 C117 0.989 1_555 1_555 H114 C117 0.990 1_555 1_555 C118 C117 1.535 1_555 1_555 H115 C118 0.991 1_555 1_555 H116 C118 0.989 1_555 1_555 C119 C118 1.463 1_555 1_555 H117 C119 0.990 1_555 1_555 H118 C119 0.990 1_555 1_555 C120 O10 1.446 1_555 1_555 H119 C120 0.989 1_555 1_555 H120 C120 0.989 1_555 1_555 C121 O13 1.439 1_555 1_555 H121 C121 0.991 1_555 1_555 H122 C121 0.990 1_555 1_555 C122 C121 1.500 1_555 1_555 H123 C122 0.989 1_555 1_555 H124 C122 0.989 1_555 1_555 C123 C122 1.525 1_555 1_555 H125 C123 0.991 1_555 1_555 H126 C123 0.990 1_555 1_555 C124 O13 1.458 1_555 1_555 H127 C124 0.990 1_555 1_555 H128 C124 0.990 1_555 1_555 C125 H129 0.991 1_555 1_555 H130 C125 0.990 1_555 1_555 C126 C125 1.515 1_555 1_555 H131 C126 0.991 1_555 1_555 H132 C126 0.991 1_555 1_555 C127 C126 1.520 1_555 1_555 H133 C127 0.989 1_555 1_555 H134 C127 0.991 1_555 1_555 C128 O11 1.459 1_555 1_555 H135 C128 0.990 1_555 1_555 H136 C128 0.991 1_555 1_555 C129 O14 1.449 1_555 1_555 H137 C129 0.989 1_555 1_555 H138 C129 0.991 1_555 1_555 C130 C129 1.511 1_555 1_555 H139 C130 0.990 1_555 1_555 H140 C130 0.991 1_555 1_555 C131 C130 1.492 1_555 1_555 H141 C131 0.990 1_555 1_555 H142 C131 0.991 1_555 1_555 C132 O14 1.446 1_555 1_555 H143 C132 0.989 1_555 1_555 H144 C132 0.990 1_555 1_555 C133 O12 1.426 1_555 1_555 H145 C133 0.990 1_555 1_555 H146 C133 0.990 1_555 1_555 C134 C133 1.508 1_555 1_555 H147 C134 0.991 1_555 1_555 H148 C134 0.990 1_555 1_555 C135 C134 1.545 1_555 1_555 H149 C135 0.991 1_555 1_555 H150 C135 0.990 1_555 1_555 C136 O12 1.417 1_555 1_555 H151 C136 0.990 1_555 1_555 H152 C136 0.990 1_555 1_555 C137 O16 1.443 1_555 1_555 H153 C137 0.991 1_555 1_555 H154 C137 0.990 1_555 1_555 C138 C137 1.516 1_555 1_555 H155 C138 0.990 1_555 1_555 H156 C138 0.989 1_555 1_555 C139 C138 1.520 1_555 1_555 H157 C139 0.991 1_555 1_555 H158 C139 0.989 1_555 1_555 C140 O16 1.438 1_555 1_555 H159 C140 0.989 1_555 1_555 H160 C140 0.990 1_555 1_555 C141 H161 0.990 1_555 1_555 H162 C141 0.991 1_555 1_555 C142 C141 1.496 1_555 1_555 H163 C142 0.990 1_555 1_555 H164 C142 0.990 1_555 1_555 C143 C142 1.506 1_555 1_555 H165 C143 0.990 1_555 1_555 H166 C143 0.991 1_555 1_555 C144 O15 1.441 1_555 1_555 H167 C144 0.990 1_555 1_555 H168 C144 0.989 1_555 1_555 C145 O17 1.442 1_555 1_555 H169 C145 0.991 1_555 1_555 H170 C145 0.991 1_555 1_555 C146 C145 1.498 1_555 1_555 H171 C146 0.991 1_555 1_555 H172 C146 0.990 1_555 1_555 C147 C146 1.459 1_555 1_555 H173 C147 0.990 1_555 1_555 H174 C147 0.990 1_555 1_555 C148 O17 1.445 1_555 1_555 H175 C148 0.990 1_555 1_555 H176 C148 0.990 1_555 1_555 C149 O18 1.454 1_555 1_555 H177 C149 0.990 1_555 1_555 H178 C149 0.990 1_555 1_555 C150 C149 1.512 1_555 1_555 H179 C150 0.991 1_555 1_555 H180 C150 0.990 1_555 1_555 C151 C150 1.527 1_555 1_555 H181 C151 0.990 1_555 1_555 H182 C151 0.990 1_555 1_555 C152 O18 1.453 1_555 1_555 H183 C152 0.990 1_555 1_555 H184 C152 0.991 1_555 1_555 C153 H185 0.990 1_555 1_555 H186 C153 0.991 1_555 1_555 C154 C153 1.515 1_555 1_555 H187 C154 0.989 1_555 1_555 H188 C154 0.991 1_555 1_555 C155 C154 1.516 1_555 1_555 H189 C155 0.990 1_555 1_555 H190 C155 0.990 1_555 1_555 C156 O19 1.431 1_555 1_555 H191 C156 0.990 1_555 1_555 H192 C156 0.990 1_555 1_555 Li2 C17 2.423 1_555 1_555 Li2 C23 2.586 1_555 1_555 Li2 C37 2.568 1_555 1_555 Li3 C18 2.391 1_555 1_555 Li3 C26 2.613 1_555 1_555 Li3 C38 2.691 1_555 1_555 Li4 C19 2.461 1_555 1_555 Li4 C29 2.505 1_555 1_555 Li4 C39 2.607 1_555 1_555 Li5 C15 2.459 1_555 1_555 Li5 C16 2.498 1_555 1_555 Li5 C20 2.587 1_555 1_555 Li5 C32 2.404 1_555 1_555 Li5 C35 2.609 1_555 1_555 Li5 C36 2.517 1_555 1_555 Li5 C40 2.418 1_555 1_555 Li6 C21 2.410 1_555 1_555 Li6 C22 2.209 1_555 1_555 Li6 C23 2.284 1_555 1_555 Li6 C35 2.735 1_555 1_555 Li6 C36 2.690 1_555 1_555 Li6 C37 2.473 1_555 1_555 Li7 C10 2.559 1_555 1_555 Li7 C11 2.323 1_555 1_555 Li7 C12 2.704 1_555 1_555 Li9 C77 2.482 1_555 1_555 Li9 C83 2.476 1_555 1_555 Li9 C97 2.481 1_555 1_555 Li10 C78 2.559 1_555 1_555 Li10 C86 2.479 1_555 1_555 Li10 C98 2.471 1_555 1_555 Li11 C79 2.491 1_555 1_555 Li11 C89 2.543 1_555 1_555 Li11 C99 2.492 1_555 1_555 Li12 C75 2.547 1_555 1_555 Li12 C76 2.513 1_555 1_555 Li12 C80 2.449 1_555 1_555 Li12 C92 2.600 1_555 1_555 Li12 C95 2.479 1_555 1_555 Li12 C96 2.506 1_555 1_555 Li12 C100 2.583 1_555 1_555 Li13 C89 2.409 1_555 1_555 Li13 C90 2.203 1_555 1_555 Li13 C91 2.262 1_555 1_555 Li13 C92 2.596 1_555 1_555 Li13 C99 2.580 1_555 1_555 Li13 C100 2.691 1_555 1_555 Li14 C62 2.471 1_555 1_555 Li14 C75 2.777 1_555 1_555 C1 C2 1.455 1_555 1_555 C1 C15 1.447 1_555 1_555 C2 C3 1.433 1_555 1_555 C3 C4 1.441 1_555 1_555 C3 C17 1.429 1_555 1_555 C4 C5 1.448 1_555 1_555 C5 C6 1.440 1_555 1_555 C6 C7 1.429 1_555 1_555 C6 C18 1.429 1_555 1_555 C7 C8 1.460 1_555 1_555 C8 C9 1.437 1_555 1_555 C9 C10 1.432 1_555 1_555 C9 C19 1.428 1_555 1_555 C10 C11 1.483 1_555 1_555 C11 C12 1.441 1_555 1_555 C12 C13 1.432 1_555 1_555 C12 C20 1.429 1_555 1_555 C13 C14 1.466 1_555 1_555 C14 C15 1.433 1_555 1_555 C15 C16 1.426 1_555 1_555 C16 C17 1.395 1_555 1_555 C16 C20 1.397 1_555 1_555 C17 C18 1.392 1_555 1_555 C18 C19 1.397 1_555 1_555 C19 C20 1.396 1_555 1_555 C21 C22 1.480 1_555 1_555 C21 C35 1.439 1_555 1_555 C22 C23 1.438 1_555 1_555 C23 C24 1.439 1_555 1_555 C23 C37 1.433 1_555 1_555 C24 C25 1.461 1_555 1_555 C25 C26 1.436 1_555 1_555 C26 C27 1.443 1_555 1_555 C26 C38 1.422 1_555 1_555 C27 C28 1.452 1_555 1_555 C28 C29 1.431 1_555 1_555 C29 C30 1.434 1_555 1_555 C29 C39 1.423 1_555 1_555 C30 C31 1.449 1_555 1_555 C31 C32 1.443 1_555 1_555 C32 C33 1.429 1_555 1_555 C32 C40 1.423 1_555 1_555 C33 C34 1.463 1_555 1_555 C34 C35 1.437 1_555 1_555 C35 C36 1.426 1_555 1_555 C36 C37 1.399 1_555 1_555 C36 C40 1.396 1_555 1_555 C37 C38 1.393 1_555 1_555 C38 C39 1.391 1_555 1_555 C39 C40 1.392 1_555 1_555 C43 C44 1.508 1_555 1_555 C47 C48 1.482 1_555 1_555 C51 C52 1.508 1_555 1_555 C55 C56 1.507 1_555 1_555 C59 C60 1.506 1_555 1_555 C61 C62 1.484 1_555 1_555 C61 C75 1.439 1_555 1_555 C62 C63 1.440 1_555 1_555 C63 C64 1.438 1_555 1_555 C63 C77 1.429 1_555 1_555 C64 C65 1.466 1_555 1_555 C65 C66 1.432 1_555 1_555 C66 C67 1.445 1_555 1_555 C66 C78 1.423 1_555 1_555 C67 C68 1.452 1_555 1_555 C68 C69 1.435 1_555 1_555 C69 C70 1.440 1_555 1_555 C69 C79 1.432 1_555 1_555 C70 C71 1.452 1_555 1_555 C71 C72 1.446 1_555 1_555 C72 C73 1.432 1_555 1_555 C72 C80 1.428 1_555 1_555 C73 C74 1.464 1_555 1_555 C74 C75 1.439 1_555 1_555 C75 C76 1.430 1_555 1_555 C76 C77 1.392 1_555 1_555 C76 C80 1.398 1_555 1_555 C77 C78 1.399 1_555 1_555 C78 C79 1.396 1_555 1_555 C79 C80 1.396 1_555 1_555 C81 C82 1.451 1_555 1_555 C81 C95 1.441 1_555 1_555 C82 C83 1.439 1_555 1_555 C83 C84 1.440 1_555 1_555 C83 C97 1.425 1_555 1_555 C84 C85 1.453 1_555 1_555 C85 C86 1.445 1_555 1_555 C86 C87 1.433 1_555 1_555 C86 C98 1.421 1_555 1_555 C87 C88 1.466 1_555 1_555 C88 C89 1.435 1_555 1_555 C89 C90 1.442 1_555 1_555 C89 C99 1.433 1_555 1_555 C90 C91 1.490 1_555 1_555 C91 C92 1.443 1_555 1_555 C92 C93 1.437 1_555 1_555 C92 C100 1.430 1_555 1_555 C93 C94 1.459 1_555 1_555 C94 C95 1.433 1_555 1_555 C95 C96 1.426 1_555 1_555 C96 C97 1.394 1_555 1_555 C96 C100 1.397 1_555 1_555 C97 C98 1.396 1_555 1_555 C98 C99 1.398 1_555 1_555 C99 C100 1.398 1_555 1_555 C103 C104 1.482 1_555 1_555 C107 C108 1.512 1_555 1_555 C111 C112 1.516 1_555 1_555 C115 C116 1.519 1_555 1_555 C119 C120 1.498 1_555 1_555 C123 C124 1.515 1_555 1_555 C127 C128 1.508 1_555 1_555 C131 C132 1.517 1_555 1_555 C135 C136 1.518 1_555 1_555 C139 C140 1.520 1_555 1_555 C143 C144 1.523 1_555 1_555 C147 C148 1.491 1_555 1_555 C151 C152 1.507 1_555 1_555 C155 C156 1.500 1_555 1_555 #END data_CSD_CIF_EWICIX _audit_creation_date 2012-02-03 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD EWICIX _database_code_depnum_ccdc_archive 'CCDC 833488' _chemical_formula_sum 'C84 H108 Li8 O15' _chemical_formula_moiety ; C40 H20 Li5 3-,2(C12 H24 Li1 O5 1+),C16 H32 Li1 O4 1+,C4 H8 O1 ; _journal_coden_Cambridge 38 _journal_volume 333 _journal_year 2011 _journal_page_first 1008 _journal_name_full 'Science ' loop_ _publ_author_name "A.V.Zabula" "A.S.Filatov" "S.N.Spisak" "A.Yu.Rogachev" "M.A.Petrukhina" _chemical_name_systematic ; bis((12-Crown-4)-tetrahydrofuran-lithium) tetrakis(tetrahydrofuran)-lithium bis(\m~5~-\h^6^,\h^6^,\h^6^,\h^6^,\h^6^-corannulene)-penta-lithium tetrahydrofuran solvate ; _cell_volume 7280.240 _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.289 _exptl_crystal_description 'block' _diffrn_ambient_temperature 100 _refine_special_details ; C78,C79,C80,C81,C82,C83,C84,C85,O11,O12,O13,O14 and C78X,C79X,C80X,C81X,C82X,C83X,C84X,C85X,O11X,O12X,O13X,O14X disordered over two sites with occupancies 0.50:0.50; C73,C74,C75,C76,O15 and C73X, C74X,C75X,C76X,O15X disordered over two sites with occupancies 0.50:0.50. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.106 _refine_ls_wR_factor_gt 0.106 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,-1/2-y,-1/2+z _cell_length_a 16.8456(16) _cell_length_b 22.163(2) _cell_length_c 20.8849(19) _cell_angle_alpha 90 _cell_angle_beta 110.984(1) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.62 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.2978(4) 0.1750(3) 0.2465(3) Li2 Li 0.4189(4) 0.0707(3) 0.3165(3) Li3 Li 0.3159(4) -0.0468(3) 0.2892(3) Li4 Li 0.1318(4) -0.0161(3) 0.2051(3) Li5 Li 0.1201(4) 0.1202(3) 0.1771(3) Li6 Li 0.2015(4) 0.7237(3) 0.0951(3) Li7 Li 0.2286(4) 0.4114(3) 0.0776(3) Li8 Li 0.2783(4) 0.4765(3) 0.4146(3) O1 O 0.19572(18) 0.64077(12) 0.12609(13) O2 O 0.12560(16) 0.77117(12) 0.12485(13) O3 O 0.31876(17) 0.74558(13) 0.11871(15) O4 O 0.15277(17) 0.73095(12) -0.00402(13) O5 O 0.16854(16) 0.39657(11) 0.14017(12) O6 O 0.18000(18) 0.48575(12) 0.01821(13) O7 O 0.33820(17) 0.46373(13) 0.11147(13) O8 O 0.31670(17) 0.34615(12) 0.08009(13) O9 O 0.15834(17) 0.36552(12) -0.01320(12) O10 O 0.32716(17) 0.49688(13) 0.34732(12) C1 C 0.3816(2) 0.18314(15) 0.17864(17) H1 H 0.42430 0.21320 0.18760 C2 C 0.2946(2) 0.19999(15) 0.13844(17) H2 H 0.28380 0.24060 0.12310 C3 C 0.2241(2) 0.15925(15) 0.12051(16) C4 C 0.1361(2) 0.15748(16) 0.07702(17) H3 H 0.11000 0.19400 0.05610 C5 C 0.0845(2) 0.10283(17) 0.06309(16) H4 H 0.02660 0.10590 0.03360 C6 C 0.1157(2) 0.04474(16) 0.09120(16) C7 C 0.0878(2) -0.01688(16) 0.08414(16) H5 H 0.03030 -0.02520 0.05690 C8 C 0.1430(2) -0.06747(16) 0.11644(16) H6 H 0.11930 -0.10690 0.10890 C9 C 0.2314(2) -0.06121(15) 0.15914(16) C10 C 0.3040(2) -0.09875(15) 0.19176(16) H7 H 0.29550 -0.14110 0.19210 C11 C 0.3907(2) -0.07552(15) 0.22459(16) H8 H 0.43560 -0.10360 0.24330 C12 C 0.4110(2) -0.01226(15) 0.22986(15) C13 C 0.4852(2) 0.02493(15) 0.25035(16) H9 H 0.53880 0.00630 0.27280 C14 C 0.4834(2) 0.09004(16) 0.23867(16) H10 H 0.53580 0.11130 0.25370 C15 C 0.4068(2) 0.12344(15) 0.20579(16) C16 C 0.3339(2) 0.08576(14) 0.19206(15) C17 C 0.2510(2) 0.10156(15) 0.15158(15) C18 C 0.2015(2) 0.04922(15) 0.13718(16) C19 C 0.2541(2) 0.00100(15) 0.16904(15) C20 C 0.3355(2) 0.02319(15) 0.20273(15) C21 C 0.3256(2) 0.20670(16) 0.35692(17) H11 H 0.36360 0.23980 0.37210 C22 C 0.2368(2) 0.21948(15) 0.31685(17) H12 H 0.22000 0.26050 0.30820 C23 C 0.1730(2) 0.17375(15) 0.28955(16) C24 C 0.0828(2) 0.16944(16) 0.25641(16) H13 H 0.05170 0.20570 0.24090 C25 C 0.0356(2) 0.11273(16) 0.24499(15) H14 H -0.02450 0.11420 0.22290 C26 C 0.0748(2) 0.05480(16) 0.26524(15) C27 C 0.0498(2) -0.00643(16) 0.27007(16) H15 H -0.00900 -0.01600 0.25170 C28 C 0.1099(2) -0.05495(15) 0.30161(16) H16 H 0.08810 -0.09460 0.30080 C29 C 0.2004(2) -0.04596(15) 0.33385(16) C30 C 0.2747(2) -0.07923(15) 0.37402(16) H17 H 0.26880 -0.12120 0.38010 C31 C 0.3587(2) -0.05229(15) 0.40603(16) H18 H 0.40460 -0.07790 0.43100 C32 C 0.3759(2) 0.01087(15) 0.40196(15) C33 C 0.4445(2) 0.05296(16) 0.42959(15) H19 H 0.49850 0.03770 0.45740 C34 C 0.4359(2) 0.11796(16) 0.41743(16) H20 H 0.48430 0.14260 0.43900 C35 C 0.3589(2) 0.14670(15) 0.37483(16) C36 C 0.2942(2) 0.10306(15) 0.34441(15) C37 C 0.2102(2) 0.11505(15) 0.30367(15) C38 C 0.1652(2) 0.06068(15) 0.29234(15) C39 C 0.2217(2) 0.01515(15) 0.32640(15) C40 C 0.3014(2) 0.04128(15) 0.35840(16) C41 C 0.1184(3) 0.60570(19) 0.1019(2) H21 H 0.11680 0.58020 0.06250 H22 H 0.06800 0.63250 0.08730 C42 C 0.1195(3) 0.5666(2) 0.1623(2) H23 H 0.06140 0.56040 0.16240 H24 H 0.14590 0.52690 0.16130 C43 C 0.1726(3) 0.6032(2) 0.2234(2) H25 H 0.13850 0.63520 0.23450 H26 H 0.19880 0.57740 0.26420 C44 C 0.2383(2) 0.62937(18) 0.19853(19) H27 H 0.26130 0.66730 0.22310 H28 H 0.28580 0.60060 0.20610 C45 C 0.0354(2) 0.76846(19) 0.0873(2) H29 H 0.02200 0.73880 0.04950 H30 H 0.01320 0.80840 0.06790 C46 C -0.0016(3) 0.7493(2) 0.1393(2) H31 H 0.00500 0.70540 0.14830 H32 H -0.06250 0.76020 0.12510 C47 C 0.0525(3) 0.7856(3) 0.2008(3) H33 H 0.02970 0.82690 0.19920 H34 H 0.05460 0.76600 0.24400 C48 C 0.1391(2) 0.78705(18) 0.19584(18) H35 H 0.16440 0.82780 0.20690 H36 H 0.17730 0.75760 0.22780 C49 C 0.3904(3) 0.7132(2) 0.1630(2) H37 H 0.39250 0.67230 0.14450 H38 H 0.38710 0.70910 0.20920 C50 C 0.4680(3) 0.7487(3) 0.1668(3) H39 H 0.48280 0.77900 0.20410 H40 H 0.51750 0.72200 0.17360 C51 C 0.4398(3) 0.7777(3) 0.0989(3) H41 H 0.44580 0.74980 0.06380 H42 H 0.47300 0.81470 0.09990 C52 C 0.3482(3) 0.79240(17) 0.0844(2) H43 H 0.34250 0.83260 0.10290 H44 H 0.31550 0.79200 0.03450 C53 C 0.1104(3) 0.78419(18) -0.0405(2) H45 H 0.12190 0.81940 -0.00930 H46 H 0.04810 0.77770 -0.06060 C54 C 0.1468(3) 0.7943(2) -0.0966(2) H47 H 0.20010 0.81790 -0.07960 H48 H 0.10550 0.81500 -0.13670 C55 C 0.1630(3) 0.72968(19) -0.1142(2) H49 H 0.11040 0.71110 -0.14650 H50 H 0.20770 0.72840 -0.13460 C56 C 0.1919(3) 0.69808(18) -0.0453(2) H51 H 0.17300 0.65550 -0.05080 H52 H 0.25460 0.69920 -0.02360 C57 C 0.0796(2) 0.41012(18) 0.1159(2) H53 H 0.06330 0.43520 0.07390 H54 H 0.06450 0.43190 0.15130 C58 C 0.0366(3) 0.3499(2) 0.1010(3) H55 H 0.03440 0.33400 0.05600 H56 H -0.02180 0.35200 0.10170 C59 C 0.0937(3) 0.3122(2) 0.1592(3) H57 H 0.07640 0.31490 0.19970 H58 H 0.09240 0.26930 0.14550 C60 C 0.1802(3) 0.3389(2) 0.1742(2) H59 H 0.20950 0.34410 0.22430 H60 H 0.21500 0.31210 0.15690 C61 C 0.1461(2) 0.40632(19) -0.06851(17) H61 H 0.10160 0.39100 -0.11080 H62 H 0.19950 0.41160 -0.07750 C62 C 0.1182(2) 0.46678(18) -0.04627(17) H63 H 0.11270 0.49790 -0.08160 H64 H 0.06210 0.46180 -0.04160 C63 C 0.2489(3) 0.51755(18) 0.0102(2) H65 H 0.23050 0.55820 -0.00920 H66 H 0.27120 0.49540 -0.02090 C64 C 0.3167(2) 0.52247(16) 0.08171(19) H67 H 0.36810 0.54210 0.07880 H68 H 0.29520 0.54770 0.11110 C65 C 0.4036(2) 0.43551(19) 0.09462(19) H69 H 0.45970 0.45310 0.12160 H70 H 0.39360 0.44050 0.04520 C66 C 0.4004(2) 0.36927(17) 0.11221(18) H71 H 0.44040 0.34610 0.09670 H72 H 0.41810 0.36460 0.16250 C67 C 0.3007(3) 0.32554(17) 0.01212(19) H73 H 0.33280 0.28800 0.01270 H74 H 0.31810 0.35650 -0.01450 C68 C 0.2051(2) 0.31397(16) -0.01962(18) H75 H 0.18970 0.30370 -0.06870 H76 H 0.19010 0.27920 0.00350 C69 C 0.4190(2) 0.49850(19) 0.3735(2) H77 H 0.44110 0.50920 0.42280 H78 H 0.43990 0.52850 0.34820 C70 C 0.4469(3) 0.4358(2) 0.3629(2) H79 H 0.45950 0.41120 0.40490 H80 H 0.49810 0.43720 0.35020 C71 C 0.3707(3) 0.4104(2) 0.3043(2) H81 H 0.38670 0.40000 0.26440 H82 H 0.34820 0.37380 0.31910 C72 C 0.3055(3) 0.4609(2) 0.28648(19) H83 H 0.30870 0.48510 0.24760 H84 H 0.24730 0.44430 0.27400 O11 O 0.3447(4) 0.7245(3) 0.3144(3) C73 C 0.4174(9) 0.7018(6) 0.4293(7) H85 H 0.47520 0.68630 0.45500 H86 H 0.37970 0.69130 0.45460 C74 C 0.4191(5) 0.7715(4) 0.4188(4) H87 H 0.38110 0.79260 0.43830 H88 H 0.47740 0.78780 0.44010 C75 C 0.3871(6) 0.7779(4) 0.3411(4) H89 H 0.34800 0.81280 0.32620 H90 H 0.43530 0.78420 0.32530 C76 C 0.3846(7) 0.6767(5) 0.3596(5) H91 H 0.43170 0.65970 0.34750 H92 H 0.34320 0.64410 0.35660 O12 O 0.3626(3) 0.5039(2) 0.5145(2) C77 C 0.3254(4) 0.5589(3) 0.5309(4) H93 H 0.34580 0.59430 0.51220 H94 H 0.34490 0.56360 0.58130 C78 C 0.2321(4) 0.5576(3) 0.5026(4) H95 H 0.21030 0.52500 0.52420 H96 H 0.20870 0.59650 0.51100 O13 O 0.2082(3) 0.5470(2) 0.4300(2) C79 C 0.1180(6) 0.5266(4) 0.3961(5) H97 H 0.08170 0.54730 0.41740 H98 H 0.09770 0.53770 0.34690 C80 C 0.1105(5) 0.4617(3) 0.4023(4) H99 H 0.12370 0.45010 0.45080 H100 H 0.05230 0.44800 0.37500 O14 O 0.1718(3) 0.4359(2) 0.3762(3) C81 C 0.1845(7) 0.3714(4) 0.3875(5) H101 H 0.20310 0.35400 0.35150 H102 H 0.12990 0.35220 0.38370 C82 C 0.2478(6) 0.3583(5) 0.4546(5) H103 H 0.22670 0.37040 0.49120 H104 H 0.26090 0.31460 0.45910 O15 O 0.3229(4) 0.3926(3) 0.4597(3) C83 C 0.3846(5) 0.4001(3) 0.5275(4) H105 H 0.44210 0.40430 0.52530 H106 H 0.38460 0.36420 0.55570 C84 C 0.3634(6) 0.4543(4) 0.5588(4) H107 H 0.30700 0.44970 0.56300 H108 H 0.40640 0.46110 0.60510 C85? C 0.3507(10) 0.6680(7) 0.3680(8) C86? C 0.4352(13) 0.6717(9) 0.4148(12) C87? C 0.4633(6) 0.7297(4) 0.4191(5) C88? C 0.3985(12) 0.7642(9) 0.3607(10) C89? C 0.1919(5) 0.5455(4) 0.4779(4) C90? C 0.1323(7) 0.5408(5) 0.4058(5) C91? C 0.1064(5) 0.4311(4) 0.3887(4) C92? C 0.1460(6) 0.3809(4) 0.3669(5) C93? C 0.2680(7) 0.3576(6) 0.4710(6) C94? C 0.3552(5) 0.3753(4) 0.5008(5) C95? C 0.3555(6) 0.4713(4) 0.5564(5) C96? C 0.3457(6) 0.5352(4) 0.5375(5) H109? H 0.34540 0.63360 0.33650 H110? H 0.31190 0.66080 0.39330 H111? H 0.43790 0.65770 0.46050 H112? H 0.47220 0.64520 0.39940 H113? H 0.51980 0.73120 0.41470 H114? H 0.46800 0.74750 0.46380 H115? H 0.37870 0.80060 0.37820 H116? H 0.42340 0.77690 0.32650 H117? H 0.18320 0.58350 0.49930 H118? H 0.18500 0.51100 0.50560 H119? H 0.07300 0.54270 0.40450 H120? H 0.14130 0.57530 0.37900 H121? H 0.04440 0.43170 0.36270 H122? H 0.11600 0.42790 0.43820 H123? H 0.12350 0.34240 0.37770 H124? H 0.13160 0.38280 0.31670 H125? H 0.23500 0.37390 0.49790 H126? H 0.26310 0.31300 0.46990 H127? H 0.38810 0.35540 0.47590 H128? H 0.37850 0.36170 0.54920 H129? H 0.40630 0.46510 0.59820 H130? H 0.30490 0.45650 0.56520 H131? H 0.39920 0.55030 0.53380 H132? H 0.33460 0.55850 0.57380 O16? O 0.2749(3) 0.5444(2) 0.4714(3) O17? O 0.1455(3) 0.4845(2) 0.3753(3) O18? O 0.2362(4) 0.3824(3) 0.4007(3) O19? O 0.3647(3) 0.4394(2) 0.4983(3) O20? O 0.3274(6) 0.7215(4) 0.3299(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 C1 2.338 1_555 1_555 Li2 C12 2.550 1_555 1_555 Li3 C9 2.596 1_555 1_555 Li4 C6 2.662 1_555 1_555 Li5 C3 2.588 1_555 1_555 Li6 O1 1.963 1_555 1_555 Li7 O5 1.946 1_555 1_555 Li8 O10 1.919 1_555 1_555 O1 C41 1.444 1_555 1_555 O2 Li6 1.923 1_555 1_555 O3 Li6 1.919 1_555 1_555 O4 Li6 1.941 1_555 1_555 O5 C57 1.431 1_555 1_555 O6 Li7 2.049 1_555 1_555 O7 Li7 2.078 1_555 1_555 O8 Li7 2.059 1_555 1_555 O9 Li7 2.103 1_555 1_555 O10 C69 1.445 1_555 1_555 C1 H1 0.949 1_555 1_555 C2 Li1 2.306 1_555 1_555 H2 C2 0.951 1_555 1_555 C3 Li1 2.499 1_555 1_555 C4 Li5 2.351 1_555 1_555 H3 C4 0.950 1_555 1_555 C5 Li5 2.270 1_555 1_555 H4 C5 0.951 1_555 1_555 C6 Li5 2.434 1_555 1_555 C7 Li4 2.364 1_555 1_555 H5 C7 0.949 1_555 1_555 C8 Li4 2.238 1_555 1_555 H6 C8 0.950 1_555 1_555 C9 Li4 2.427 1_555 1_555 C10 Li3 2.284 1_555 1_555 H7 C10 0.950 1_555 1_555 C11 Li3 2.243 1_555 1_555 H8 C11 0.949 1_555 1_555 C12 Li3 2.472 1_555 1_555 C13 Li2 2.300 1_555 1_555 H9 C13 0.950 1_555 1_555 C14 Li2 2.296 1_555 1_555 H10 C14 0.949 1_555 1_555 C15 Li1 2.553 1_555 1_555 C16 Li1 2.464 1_555 1_555 C17 Li1 2.466 1_555 1_555 C18 Li4 2.584 1_555 1_555 C19 Li3 2.575 1_555 1_555 C20 Li2 2.517 1_555 1_555 C21 Li1 2.293 1_555 1_555 H11 C21 0.950 1_555 1_555 C22 Li1 2.295 1_555 1_555 H12 C22 0.950 1_555 1_555 C23 Li1 2.566 1_555 1_555 C24 Li5 2.253 1_555 1_555 H13 C24 0.951 1_555 1_555 C25 Li5 2.347 1_555 1_555 H14 C25 0.951 1_555 1_555 C26 Li4 2.415 1_555 1_555 C27 Li4 2.267 1_555 1_555 H15 C27 0.949 1_555 1_555 C28 Li4 2.339 1_555 1_555 H16 C28 0.950 1_555 1_555 C29 Li3 2.440 1_555 1_555 C30 Li3 2.240 1_555 1_555 H17 C30 0.949 1_555 1_555 C31 Li3 2.287 1_555 1_555 H18 C31 0.950 1_555 1_555 C32 Li2 2.529 1_555 1_555 C33 Li2 2.278 1_555 1_555 H19 C33 0.949 1_555 1_555 C34 Li2 2.278 1_555 1_555 H20 C34 0.950 1_555 1_555 C35 Li1 2.581 1_555 1_555 C36 Li1 2.611 1_555 1_555 C37 Li1 2.575 1_555 1_555 C38 Li4 2.408 1_555 1_555 C39 Li3 2.427 1_555 1_555 C40 Li2 2.520 1_555 1_555 C41 H21 0.991 1_555 1_555 H22 C41 0.991 1_555 1_555 C42 C41 1.525 1_555 1_555 H23 C42 0.989 1_555 1_555 H24 C42 0.989 1_555 1_555 C43 C42 1.506 1_555 1_555 H25 C43 0.991 1_555 1_555 H26 C43 0.989 1_555 1_555 C44 O1 1.446 1_555 1_555 H27 C44 0.989 1_555 1_555 H28 C44 0.991 1_555 1_555 C45 O2 1.440 1_555 1_555 H29 C45 0.989 1_555 1_555 H30 C45 0.989 1_555 1_555 C46 C45 1.494 1_555 1_555 H31 C46 0.990 1_555 1_555 H32 C46 0.990 1_555 1_555 C47 C46 1.513 1_555 1_555 H33 C47 0.989 1_555 1_555 H34 C47 0.991 1_555 1_555 C48 O2 1.460 1_555 1_555 H35 C48 0.990 1_555 1_555 H36 C48 0.989 1_555 1_555 C49 O3 1.424 1_555 1_555 H37 C49 0.991 1_555 1_555 H38 C49 0.990 1_555 1_555 C50 C49 1.503 1_555 1_555 H39 C50 0.990 1_555 1_555 H40 C50 0.990 1_555 1_555 C51 C50 1.472 1_555 1_555 H41 C51 0.991 1_555 1_555 H42 C51 0.989 1_555 1_555 C52 O3 1.446 1_555 1_555 H43 C52 0.989 1_555 1_555 H44 C52 0.989 1_555 1_555 C53 O4 1.447 1_555 1_555 H45 C53 0.990 1_555 1_555 H46 C53 0.991 1_555 1_555 C54 C53 1.521 1_555 1_555 H47 C54 0.989 1_555 1_555 H48 C54 0.989 1_555 1_555 C55 C54 1.527 1_555 1_555 H49 C55 0.991 1_555 1_555 H50 C55 0.989 1_555 1_555 C56 O4 1.454 1_555 1_555 H51 C56 0.989 1_555 1_555 H52 C56 0.989 1_555 1_555 C57 H53 0.991 1_555 1_555 H54 C57 0.989 1_555 1_555 C58 C57 1.497 1_555 1_555 H55 C58 0.992 1_555 1_555 H56 C58 0.990 1_555 1_555 C59 C58 1.504 1_555 1_555 H57 C59 0.990 1_555 1_555 H58 C59 0.991 1_555 1_555 C60 O5 1.441 1_555 1_555 H59 C60 0.991 1_555 1_555 H60 C60 0.989 1_555 1_555 C61 O9 1.423 1_555 1_555 H61 C61 0.992 1_555 1_555 H62 C61 0.990 1_555 1_555 C62 O6 1.439 1_555 1_555 H63 C62 0.990 1_555 1_555 H64 C62 0.990 1_555 1_555 C63 O6 1.418 1_555 1_555 H65 C63 0.991 1_555 1_555 H66 C63 0.989 1_555 1_555 C64 O7 1.432 1_555 1_555 H67 C64 0.990 1_555 1_555 H68 C64 0.990 1_555 1_555 C65 O7 1.416 1_555 1_555 H69 C65 0.991 1_555 1_555 H70 C65 0.991 1_555 1_555 C66 O8 1.422 1_555 1_555 H71 C66 0.989 1_555 1_555 H72 C66 0.989 1_555 1_555 C67 O8 1.422 1_555 1_555 H73 C67 0.990 1_555 1_555 H74 C67 0.991 1_555 1_555 C68 O9 1.421 1_555 1_555 H75 C68 0.990 1_555 1_555 H76 C68 0.989 1_555 1_555 C69 H77 0.990 1_555 1_555 H78 C69 0.989 1_555 1_555 C70 C69 1.508 1_555 1_555 H79 C70 0.989 1_555 1_555 H80 C70 0.989 1_555 1_555 C71 C70 1.529 1_555 1_555 H81 C71 0.990 1_555 1_555 H82 C71 0.991 1_555 1_555 C72 O10 1.432 1_555 1_555 H83 C72 0.991 1_555 1_555 H84 C72 0.991 1_555 1_555 O11 C75 1.392 1_555 1_555 C73 H85 0.990 1_555 1_555 H86 C73 0.988 1_555 1_555 C74 C73 1.562 1_555 1_555 H87 C74 0.990 1_555 1_555 H88 C74 0.990 1_555 1_555 C75 C74 1.522 1_555 1_555 H89 C75 0.991 1_555 1_555 H90 C75 0.990 1_555 1_555 C76 O11 1.418 1_555 1_555 H91 C76 0.989 1_555 1_555 H92 C76 0.990 1_555 1_555 O12 Li8 2.149 1_555 1_555 C77 O12 1.466 1_555 1_555 H93 C77 0.991 1_555 1_555 H94 C77 0.989 1_555 1_555 C78 C77 1.468 1_555 1_555 H95 C78 0.989 1_555 1_555 H96 C78 0.989 1_555 1_555 O13 Li8 2.052 1_555 1_555 C79 O13 1.498 1_555 1_555 H97 C79 0.988 1_555 1_555 H98 C79 0.991 1_555 1_555 C80 C79 1.454 1_555 1_555 H99 C80 0.990 1_555 1_555 H100 C80 0.989 1_555 1_555 O14 Li8 1.908 1_555 1_555 C81 O14 1.452 1_555 1_555 H101 C81 0.990 1_555 1_555 H102 C81 0.990 1_555 1_555 C82 C81 1.454 1_555 1_555 H103 C82 0.989 1_555 1_555 H104 C82 0.990 1_555 1_555 O15 Li8 2.098 1_555 1_555 C83 O15 1.435 1_555 1_555 H105 C83 0.990 1_555 1_555 H106 C83 0.990 1_555 1_555 C84 O12 1.434 1_555 1_555 H107 C84 0.990 1_555 1_555 H108 C84 0.990 1_555 1_555 Li2 C15 2.533 1_555 1_555 Li2 C16 2.500 1_555 1_555 Li2 C35 2.495 1_555 1_555 Li2 C36 2.479 1_555 1_555 Li3 C20 2.491 1_555 1_555 Li3 C32 2.549 1_555 1_555 Li3 C40 2.492 1_555 1_555 Li4 C19 2.463 1_555 1_555 Li4 C29 2.604 1_555 1_555 Li4 C39 2.538 1_555 1_555 Li5 C17 2.482 1_555 1_555 Li5 C18 2.423 1_555 1_555 Li5 C23 2.494 1_555 1_555 Li5 C26 2.660 1_555 1_555 Li5 C37 2.536 1_555 1_555 Li5 C38 2.608 1_555 1_555 C1 C2 1.453 1_555 1_555 C1 C15 1.442 1_555 1_555 C2 C3 1.431 1_555 1_555 C3 C4 1.435 1_555 1_555 C3 C17 1.432 1_555 1_555 C4 C5 1.458 1_555 1_555 C5 C6 1.434 1_555 1_555 C6 C7 1.435 1_555 1_555 C6 C18 1.424 1_555 1_555 C7 C8 1.459 1_555 1_555 C8 C9 1.443 1_555 1_555 C9 C10 1.434 1_555 1_555 C9 C19 1.426 1_555 1_555 C10 C11 1.467 1_555 1_555 C11 C12 1.438 1_555 1_555 C12 C13 1.429 1_555 1_555 C12 C20 1.428 1_555 1_555 C13 C14 1.462 1_555 1_555 C14 C15 1.432 1_555 1_555 C15 C16 1.427 1_555 1_555 C16 C17 1.394 1_555 1_555 C16 C20 1.403 1_555 1_555 C17 C18 1.397 1_555 1_555 C18 C19 1.396 1_555 1_555 C19 C20 1.388 1_555 1_555 C21 C22 1.457 1_555 1_555 C21 C35 1.440 1_555 1_555 C22 C23 1.438 1_555 1_555 C23 C24 1.430 1_555 1_555 C23 C37 1.428 1_555 1_555 C24 C25 1.460 1_555 1_555 C25 C26 1.436 1_555 1_555 C26 C27 1.435 1_555 1_555 C26 C38 1.428 1_555 1_555 C27 C28 1.462 1_555 1_555 C28 C29 1.443 1_555 1_555 C29 C30 1.436 1_555 1_555 C29 C39 1.424 1_555 1_555 C30 C31 1.459 1_555 1_555 C31 C32 1.438 1_555 1_555 C32 C33 1.436 1_555 1_555 C32 C40 1.428 1_555 1_555 C33 C34 1.461 1_555 1_555 C34 C35 1.433 1_555 1_555 C35 C36 1.425 1_555 1_555 C36 C37 1.391 1_555 1_555 C36 C40 1.396 1_555 1_555 C37 C38 1.398 1_555 1_555 C38 C39 1.395 1_555 1_555 C39 C40 1.394 1_555 1_555 C43 C44 1.498 1_555 1_555 C47 C48 1.499 1_555 1_555 C51 C52 1.498 1_555 1_555 C55 C56 1.515 1_555 1_555 C59 C60 1.498 1_555 1_555 C61 C62 1.545 1_555 1_555 C63 C64 1.525 1_555 1_555 C65 C66 1.519 1_555 1_555 C67 C68 1.528 1_555 1_555 C71 C72 1.518 1_555 1_555 C73 C76 1.469 1_555 1_555 C78 O13 1.442 1_555 1_555 C80 O14 1.447 1_555 1_555 C82 O15 1.447 1_555 1_555 C83 C84 1.471 1_555 1_555 #END data_CSD_CIF_FABMAW10 _audit_creation_date 1990-01-22 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD FABMAW10 _chemical_formula_sum 'C24 H48 Cs1 Na1 O12' _chemical_formula_moiety ; C24 H48 Cs1 O12 1+,Na1 1- ; _journal_coden_Cambridge 9 _journal_volume 28 _journal_year 1989 _journal_page_first 2132 _journal_name_full 'Inorg.Chem. ' loop_ _publ_author_name "S.B.Dawes" "D.L.Ward" "O.Fussa-Rydel" "Rui-H.Huang" "J.L.Dye" _chemical_name_systematic ; bis(18-Crown-6)-cesium sodide ; _cell_volume 3706.809 _exptl_crystal_density_diffrn 1.23 _exptl_special_details ; Isostructural with the electride ; _diffrn_ambient_temperature 213 _refine_special_details ; C15 is disordered over two positions with equal occupancies. One site has been suppressed. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.028 _refine_ls_wR_factor_gt 0.028 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,z 3 -x,y,1/2-z 4 1/2-x,1/2+y,1/2-z 5 -x,-y,-z 6 -1/2-x,-1/2-y,-z 7 x,-y,-1/2+z 8 -1/2+x,-1/2-y,-1/2+z _cell_length_a 13.581(3) _cell_length_b 15.684(2) _cell_length_c 17.429(4) _cell_angle_alpha 90 _cell_angle_beta 93.16(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Cs 2.40 Na 0.97 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Cs1 Cs 0.00000 0.02094(3) 0.25000 Na1 Na 0.00000 0.50000 0.00000 O1 O -0.0980(2) 0.1741(2) 0.3653(2) O2 O 0.1135(2) 0.1611(2) 0.3643(2) O3 O 0.1361(2) -0.0171(2) 0.4081(2) O4 O -0.0224(2) -0.1364(2) 0.3877(2) O5 O -0.1820(3) -0.1166(2) 0.2736(2) O6 O -0.2335(2) 0.0605(2) 0.2861(2) C1 C -0.0319(4) 0.2435(3) 0.3715(3) C2 C 0.0614(4) 0.2169(4) 0.4119(3) C3 C 0.1980(4) 0.1252(4) 0.4032(3) C4 C 0.1767(4) 0.0506(4) 0.4540(3) C5 C 0.1279(4) -0.0932(4) 0.4518(3) C6 C 0.0766(4) -0.1601(4) 0.4053(3) C7 C -0.0822(5) -0.2029(3) 0.3564(3) C8 C -0.1830(4) -0.1706(4) 0.3369(3) C9 C -0.2755(4) -0.0767(5) 0.2480(4) C10 C -0.307(1) 0.003(1) 0.274(1) C11? C -0.3013(7) -0.0095(6) 0.2990(5) C12 C -0.2617(4) 0.1299(4) 0.3319(3) C13 C -0.1878(4) 0.1982(4) 0.3284(3) H1 H -0.060(4) 0.297(3) 0.397(3) H2 H -0.024(4) 0.264(3) 0.327(3) H3 H 0.054(3) 0.187(3) 0.449(3) H4 H 0.107(4) 0.268(4) 0.426(3) H5 H 0.230(4) 0.176(3) 0.435(3) H6 H 0.238(3) 0.102(3) 0.367(3) H7 H 0.130(4) 0.068(4) 0.487(3) H8 H 0.241(4) 0.028(3) 0.478(3) H9 H 0.093(3) -0.080(3) 0.493(3) H10 H 0.198(4) -0.111(3) 0.468(3) H11 H 0.079(3) -0.215(3) 0.426(3) H12 H 0.105(3) -0.166(3) 0.364(2) H13 H -0.083(3) -0.250(3) 0.386(3) H14 H -0.061(4) -0.223(3) 0.319(3) H15 H -0.212(4) -0.134(4) 0.368(3) H16 H -0.226(4) -0.217(4) 0.327(3) H17 H -0.32600 -0.11700 0.25200 H18 H -0.28100 -0.06100 0.19600 H19 H -0.35500 0.02700 0.23800 H20 H -0.33500 -0.00500 0.32200 H21? H -0.36800 0.00700 0.28900 H22? H -0.29200 -0.02900 0.35000 H23 H -0.267(4) 0.111(3) 0.383(3) H24 H -0.330(4) 0.148(3) 0.309(3) H25 H -0.216(4) 0.249(3) 0.351(3) H26 H -0.180(4) 0.215(3) 0.277(3) O1B O 0.0980(2) 0.1741(2) 0.1347(2) O2B O -0.1135(2) 0.1611(2) 0.1357(2) O3B O -0.1361(2) -0.0171(2) 0.0919(2) O4B O 0.0224(2) -0.1364(2) 0.1123(2) O5B O 0.1820(3) -0.1166(2) 0.2264(2) O6B O 0.2335(2) 0.0605(2) 0.2139(2) C1B C 0.0319(4) 0.2435(3) 0.1285(3) C13B C 0.1878(4) 0.1982(4) 0.1716(3) C2B C -0.0614(4) 0.2169(4) 0.0881(3) C3B C -0.1980(4) 0.1252(4) 0.0968(3) C4B C -0.1767(4) 0.0506(4) 0.0460(3) C5B C -0.1279(4) -0.0932(4) 0.0482(3) C6B C -0.0766(4) -0.1601(4) 0.0947(3) C7B C 0.0822(5) -0.2029(3) 0.1436(3) C8B C 0.1830(4) -0.1706(4) 0.1631(3) C9B C 0.2755(4) -0.0767(5) 0.2520(4) C10B C 0.307(1) 0.003(1) 0.226(1) C12B C 0.2617(4) 0.1299(4) 0.1681(3) H1B H 0.060(4) 0.297(3) 0.103(3) H2B H 0.024(4) 0.264(3) 0.173(3) H25B H 0.216(4) 0.249(3) 0.149(3) H26B H 0.180(4) 0.215(3) 0.223(3) H3B H -0.054(3) 0.187(3) 0.051(3) H4B H -0.107(4) 0.268(4) 0.074(3) H5B H -0.230(4) 0.176(3) 0.065(3) H6B H -0.238(3) 0.102(3) 0.133(3) H7B H -0.130(4) 0.068(4) 0.013(3) H8B H -0.241(4) 0.028(3) 0.022(3) H9B H -0.093(3) -0.080(3) 0.007(3) H10B H -0.198(4) -0.111(3) 0.032(3) H11B H -0.079(3) -0.215(3) 0.074(3) H12B H -0.105(3) -0.166(3) 0.136(2) H13B H 0.083(3) -0.250(3) 0.114(3) H14B H 0.061(4) -0.223(3) 0.181(3) H15B H 0.212(4) -0.134(4) 0.132(3) H16B H 0.226(4) -0.217(4) 0.173(3) H17B H 0.32600 -0.11700 0.24800 H18B H 0.28100 -0.06100 0.30400 H19B H 0.35500 0.02700 0.26200 H20B H 0.33500 -0.00500 0.17800 H23B H 0.267(4) 0.111(3) 0.117(3) H24B H 0.330(4) 0.148(3) 0.191(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cs1 O1 3.446 1_555 1_555 O1 C1 1.411 1_555 1_555 O2 Cs1 3.292 1_555 1_555 O3 Cs1 3.287 1_555 1_555 O4 Cs1 3.467 1_555 1_555 O5 Cs1 3.323 1_555 1_555 O6 Cs1 3.325 1_555 1_555 C1 C2 1.475 1_555 1_555 C2 O2 1.421 1_555 1_555 C3 O2 1.417 1_555 1_555 C4 O3 1.422 1_555 1_555 C5 O3 1.424 1_555 1_555 C6 O4 1.412 1_555 1_555 C7 O4 1.413 1_555 1_555 C8 O5 1.392 1_555 1_555 C9 O5 1.463 1_555 1_555 C10 O6 1.353 1_555 1_555 C12 O6 1.415 1_555 1_555 C13 O1 1.399 1_555 1_555 H1 C1 1.032 1_555 1_555 H2 C1 0.852 1_555 1_555 H3 C2 0.810 1_555 1_555 H4 C2 1.034 1_555 1_555 H5 C3 1.051 1_555 1_555 H6 C3 0.929 1_555 1_555 H7 C4 0.921 1_555 1_555 H8 C4 1.011 1_555 1_555 H9 C5 0.906 1_555 1_555 H10 C5 1.017 1_555 1_555 H11 C6 0.933 1_555 1_555 H12 C6 0.840 1_555 1_555 H13 C7 0.901 1_555 1_555 H14 C7 0.792 1_555 1_555 H15 C8 0.896 1_555 1_555 H16 C8 0.943 1_555 1_555 H17 C9 0.938 1_555 1_555 H18 C9 0.938 1_555 1_555 H19 C10 0.957 1_555 1_555 H20 C10 0.946 1_555 1_555 H23 C12 0.945 1_555 1_555 H24 C12 1.029 1_555 1_555 H25 C13 0.976 1_555 1_555 H26 C13 0.945 1_555 1_555 O1B Cs1 3.446 1_555 1_555 O2B Cs1 3.292 1_555 1_555 O3B Cs1 3.287 1_555 1_555 O4B Cs1 3.467 1_555 1_555 O5B Cs1 3.323 1_555 1_555 O6B Cs1 3.325 1_555 1_555 C1B O1B 1.411 1_555 1_555 C13B O1B 1.399 1_555 1_555 C2B O2B 1.421 1_555 1_555 C3B O2B 1.417 1_555 1_555 C4B O3B 1.422 1_555 1_555 C5B O3B 1.424 1_555 1_555 C6B O4B 1.412 1_555 1_555 C7B O4B 1.413 1_555 1_555 C8B O5B 1.392 1_555 1_555 C9B O5B 1.463 1_555 1_555 C10B O6B 1.353 1_555 1_555 C12B O6B 1.415 1_555 1_555 H1B C1B 1.032 1_555 1_555 H2B C1B 0.852 1_555 1_555 H25B C13B 0.976 1_555 1_555 H26B C13B 0.945 1_555 1_555 H3B C2B 0.810 1_555 1_555 H4B C2B 1.034 1_555 1_555 H5B C3B 1.051 1_555 1_555 H6B C3B 0.929 1_555 1_555 H7B C4B 0.921 1_555 1_555 H8B C4B 1.011 1_555 1_555 H9B C5B 0.906 1_555 1_555 H10B C5B 1.017 1_555 1_555 H11B C6B 0.933 1_555 1_555 H12B C6B 0.840 1_555 1_555 H13B C7B 0.901 1_555 1_555 H14B C7B 0.792 1_555 1_555 H15B C8B 0.896 1_555 1_555 H16B C8B 0.943 1_555 1_555 H17B C9B 0.938 1_555 1_555 H18B C9B 0.938 1_555 1_555 H19B C10B 0.957 1_555 1_555 H20B C10B 0.946 1_555 1_555 H23B C12B 0.945 1_555 1_555 H24B C12B 1.029 1_555 1_555 C3 C4 1.505 1_555 1_555 C5 C6 1.477 1_555 1_555 C7 C8 1.482 1_555 1_555 C9 C10 1.404 1_555 1_555 C12 C13 1.471 1_555 1_555 C1B C2B 1.475 1_555 1_555 C13B C12B 1.471 1_555 1_555 C3B C4B 1.505 1_555 1_555 C5B C6B 1.477 1_555 1_555 C7B C8B 1.482 1_555 1_555 C9B C10B 1.404 1_555 1_555 #END data_CSD_CIF_FABMEA01 _audit_creation_date 1994-05-24 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD FABMEA01 _chemical_formula_sum 'C20 H40 Na1 O10 Rb1' _chemical_formula_moiety ; C20 H40 O10 Rb1 1+,Na1 1- ; _journal_coden_Cambridge 4 _journal_volume 115 _journal_year 1993 _journal_page_first 9542 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "R.H.Huang" "J.L.Eglin" "S.Z.Huang" "L.E.H.McMills" "J.L.Dye" _chemical_name_systematic ; (1,4,7,10,13,16-Hexaoxacyclo-octadecane)-(1,4,7,10-tetraoxacyclododecane)-rubi dium sodide ; _cell_volume 3191.918 _exptl_crystal_colour 'bright green' _exptl_special_details ; orthorhombic polymorph ; _diffrn_ambient_temperature 180 _refine_special_details ; The 12-crown-4 ligand is disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.05 _refine_ls_wR_factor_gt 0.05 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2+z 3 x,1/2-y,z 4 1/2-x,-y,1/2+z 5 -x,-y,-z 6 -1/2+x,-1/2-y,-1/2-z 7 -x,-1/2+y,-z 8 -1/2+x,y,-1/2-z _cell_length_a 13.989(5) _cell_length_b 13.677(14) _cell_length_c 16.683(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.73 H 0.23 Na 0.97 O 0.68 Rb 2.06 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Rb1 Rb 0.3930(1) 0.25000 0.35033(8) Na1 Na 0.1019(6) 0.75000 0.3595(4) O1 O 0.5803(6) 0.25000 0.4434(5) O2 O 0.5076(4) 0.0667(5) 0.3872(5) O3 O 0.4262(5) 0.0756(6) 0.2349(5) O4 O 0.3476(6) 0.25000 0.1765(6) O5 O 0.2055(4) 0.3545(5) 0.3433(4) O6 O 0.2951(5) 0.3518(6) 0.4968(5) C1 C 0.5781(7) 0.1645(9) 0.4916(6) C2 C 0.5873(7) 0.0769(9) 0.4386(7) C3 C 0.518(1) -0.0084(9) 0.3293(9) C4 C 0.431(1) -0.015(1) 0.279(1) C5 C 0.350(1) 0.075(1) 0.1795(9) C6 C 0.358(1) 0.162(1) 0.1266(7) C7? C 0.151(1) 0.396(1) 0.400(1) C8 C 0.215(2) 0.437(2) 0.414(1) C9 C 0.222(2) 0.383(2) 0.499(2) C10? C 0.228(2) 0.440(2) 0.457(1) C11 C 0.302(1) 0.260(6) 0.574(1) C12? C 0.246(1) 0.326(1) 0.561(1) C13? C 0.136(1) 0.278(1) 0.2907(7) C14 C 0.125(1) 0.312(1) 0.344(1) H1 H 0.63000 0.16410 0.52860 H2 H 0.51980 0.15950 0.51950 H3 H 0.59410 0.01790 0.46890 H4 H 0.64430 0.08250 0.40510 H5 H 0.57260 0.00560 0.29570 H6 H 0.52960 -0.06930 0.35550 H7 H 0.37680 -0.02390 0.31140 H8 H 0.43660 -0.06960 0.24270 H9 H 0.35450 0.01820 0.14590 H10 H 0.29120 0.07610 0.20570 H11 H 0.30850 0.16320 0.08640 H12 H 0.41820 0.16550 0.09960 H13 H 0.27050 0.47910 0.40520 H14 H 0.16010 0.48400 0.41240 H15 H 0.17370 0.32920 0.50640 H16 H 0.21290 0.42240 0.54790 H17 H 0.33440 0.20370 0.56810 H18? H 0.32390 0.28810 0.62970 H19 H 0.10930 0.29390 0.40390 H20 H 0.07210 0.35460 0.33180 O2B O 0.5076(4) 0.4333(5) 0.3872(5) C2B C 0.5873(7) 0.4231(9) 0.4386(7) C1B C 0.5781(7) 0.3355(9) 0.4916(6) H1B H 0.63000 0.33590 0.52860 H2B H 0.51980 0.34050 0.51950 H3B H 0.59410 0.48210 0.46890 H4B H 0.64430 0.41750 0.40510 C3B C 0.518(1) 0.5084(9) 0.3293(9) C4B C 0.431(1) 0.515(1) 0.279(1) O3B O 0.4262(5) 0.4244(6) 0.2349(5) O5B O 0.2055(4) 0.1455(5) 0.3433(4) C8B C 0.215(2) 0.063(2) 0.414(1) C9B C 0.222(2) 0.117(2) 0.499(2) O6B O 0.2951(5) 0.1482(6) 0.4968(5) C11B C 0.302(1) 0.240(6) 0.574(1) H17B H 0.33440 0.29630 0.56810 H15B H 0.17370 0.17080 0.50640 H16B H 0.21290 0.07760 0.54790 H13B H 0.27050 0.02090 0.40520 H14B H 0.16010 0.01600 0.41240 C14B C 0.125(1) 0.188(1) 0.344(1) H19B H 0.10930 0.20610 0.40390 H20B H 0.07210 0.14540 0.33180 C6B C 0.358(1) 0.338(1) 0.1266(7) C5B C 0.350(1) 0.425(1) 0.1795(9) H9B H 0.35450 0.48180 0.14590 H10B H 0.29120 0.42390 0.20570 H11B H 0.30850 0.33680 0.08640 H12B H 0.41820 0.33450 0.09960 H7B H 0.37680 0.52390 0.31140 H8B H 0.43660 0.56960 0.24270 H5B H 0.57260 0.49440 0.29570 H6B H 0.52960 0.56930 0.35550 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rb1 O1 3.046 1_555 1_555 O1 C1 1.420 1_555 1_555 O2 Rb1 3.039 1_555 1_555 O3 Rb1 3.101 1_555 1_555 O4 Rb1 2.969 1_555 1_555 O5 Rb1 2.989 1_555 1_555 O6 Rb1 3.128 1_555 1_555 C1 C2 1.495 1_555 1_555 C2 O2 1.413 1_555 1_555 C3 O2 1.417 1_555 1_555 C4 O3 1.443 1_555 1_555 C5 O3 1.411 1_555 1_555 C6 O4 1.471 1_555 1_555 C8 O5 1.638 1_555 1_555 C9 O6 1.109 1_555 1_555 C11 O6 1.801 1_555 1_555 C14 O5 1.267 1_555 1_555 H1 C1 0.953 1_555 1_555 H2 C1 0.942 1_555 1_555 H3 C2 0.957 1_555 1_555 H4 C2 0.977 1_555 1_555 H5 C3 0.967 1_555 1_555 H6 C3 0.955 1_555 1_555 H7 C4 0.939 1_555 1_555 H8 C4 0.965 1_555 1_555 H9 C5 0.960 1_555 1_555 H10 C5 0.932 1_555 1_555 H11 C6 0.964 1_555 1_555 H12 C6 0.956 1_555 1_555 H13 C8 0.978 1_555 1_555 H14 C8 1.002 1_555 1_555 H15 C9 1.007 1_555 1_555 H16 C9 0.986 1_555 1_555 H17 C11 0.899 1_555 1_555 H19 C14 1.053 1_555 1_555 H20 C14 0.964 1_555 1_555 O2B Rb1 3.039 1_555 1_555 C2B O2B 1.413 1_555 1_555 C1B O1 1.420 1_555 1_555 H1B C1B 0.953 1_555 1_555 H2B C1B 0.942 1_555 1_555 H3B C2B 0.957 1_555 1_555 H4B C2B 0.977 1_555 1_555 C3B O2B 1.417 1_555 1_555 C4B C3B 1.481 1_555 1_555 O3B Rb1 3.101 1_555 1_555 O5B Rb1 2.989 1_555 1_555 C8B O5B 1.638 1_555 1_555 C9B C8B 1.602 1_555 1_555 O6B Rb1 3.128 1_555 1_555 C11B C11 0.274 1_555 1_555 H17B C11 0.679 1_555 1_555 H15B C9B 1.007 1_555 1_555 H16B C9B 0.986 1_555 1_555 H13B C8B 0.978 1_555 1_555 H14B C8B 1.002 1_555 1_555 C14B C14 1.696 1_555 1_555 H19B C14B 1.053 1_555 1_555 H20B C14B 0.964 1_555 1_555 C6B O4 1.471 1_555 1_555 C5B O3B 1.411 1_555 1_555 H9B C5B 0.960 1_555 1_555 H10B C5B 0.932 1_555 1_555 H11B C6B 0.964 1_555 1_555 H12B C6B 0.956 1_555 1_555 H7B C4B 0.939 1_555 1_555 H8B C4B 0.965 1_555 1_555 H5B C3B 0.967 1_555 1_555 H6B C3B 0.955 1_555 1_555 C3 C4 1.481 1_555 1_555 C5 C6 1.486 1_555 1_555 C8 C9 1.602 1_555 1_555 H17 C11B 0.679 1_555 1_555 C2B C1B 1.495 1_555 1_555 C4B O3B 1.443 1_555 1_555 O5B C14B 1.267 1_555 1_555 C9B O6B 1.109 1_555 1_555 O6B C11B 1.801 1_555 1_555 C11B H17B 0.899 1_555 1_555 C6B C5B 1.486 1_555 1_555 #END data_CSD_CIF_FABMEA10 _audit_creation_date 1990-01-22 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD FABMEA10 _chemical_formula_sum 'C20 H40 Na1 O10 Rb1' _chemical_formula_moiety ; C20 H40 O10 Rb1 1+,Na1 1- ; _journal_coden_Cambridge 9 _journal_volume 28 _journal_year 1989 _journal_page_first 2132 _journal_name_full 'Inorg.Chem. ' loop_ _publ_author_name "S.B.Dawes" "D.L.Ward" "O.Fussa-Rydel" "Rui-H.Huang" "J.L.Dye" _chemical_name_systematic ; bis(15-Crown-5)-rubidium sodide ; _cell_volume 1562.403 _exptl_crystal_density_diffrn 1.17 _exptl_special_details ; monoclinic polymorph ; _diffrn_ambient_temperature 213 _refine_special_details ; C8 is disordered over two positions, one site has been suppressed. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_gt 0.044 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,z 3 -x,y,-z 4 1/2-x,1/2+y,-z 5 -x,-y,-z 6 -1/2-x,-1/2-y,-z 7 x,-y,z 8 -1/2+x,-1/2-y,z _cell_length_a 11.555(3) _cell_length_b 13.587(3) _cell_length_c 9.958(2) _cell_angle_alpha 90 _cell_angle_beta 92.03(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Na 0.97 O 0.68 Rb 2.00 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Rb1 Rb 0.50000 0.00000 0.50000 Na1 Na 0.50000 0.50000 0.00000 O1 O 0.4537(6) 0.00000 0.1948(7) O2 O 0.5015(4) -0.1794(4) 0.3268(5) O3 O 0.7204(4) -0.1047(4) 0.4366(6) C1 C 0.3880(7) -0.0891(6) 0.1675(8) C2 C 0.4714(8) -0.1713(6) 0.1891(8) C3 C 0.6058(8) -0.2347(6) 0.3525(9) C4 C 0.7115(7) -0.1780(8) 0.335(1) C5? C 0.823(1) -0.0331(9) 0.465(1) C6 C 0.811(1) -0.053(1) 0.370(2) H1 H 0.365(6) -0.078(5) 0.066(7) H2 H 0.333(5) -0.081(4) 0.245(6) H3 H 0.544(7) -0.148(7) 0.134(9) H4 H 0.437(5) -0.223(4) 0.154(6) H5 H 0.606(5) -0.281(5) 0.284(6) H6 H 0.585(5) -0.259(5) 0.439(6) H7 H 0.708(7) -0.153(7) 0.230(9) H8 H 0.774(5) -0.209(5) 0.334(6) H9? H 0.82300 -0.01200 0.55600 H10? H 0.89400 -0.06700 0.44900 H11 H 0.79000 -0.03500 0.28100 H12 H 0.88000 -0.09100 0.37000 O1D O 0.5463(6) 0.00000 0.8052(7) O2D O 0.4985(4) 0.1794(4) 0.6732(5) O2B O 0.4985(4) -0.1794(4) 0.6732(5) O2F O 0.5015(4) 0.1794(4) 0.3268(5) O3D O 0.2796(4) 0.1047(4) 0.5634(6) O3B O 0.2796(4) -0.1047(4) 0.5634(6) O3F O 0.7204(4) 0.1047(4) 0.4366(6) C1F C 0.3880(7) 0.0891(6) 0.1675(8) C6F C 0.811(1) 0.053(1) 0.370(2) C1D C 0.6120(7) 0.0891(6) 0.8325(8) C1B C 0.6120(7) -0.0891(6) 0.8325(8) C2D C 0.5286(8) 0.1713(6) 0.8109(8) C3D C 0.3942(8) 0.2347(6) 0.6475(9) C2B C 0.5286(8) -0.1713(6) 0.8109(8) C3B C 0.3942(8) -0.2347(6) 0.6475(9) C2F C 0.4714(8) 0.1713(6) 0.1891(8) C3F C 0.6058(8) 0.2347(6) 0.3525(9) C4D C 0.2885(7) 0.1780(8) 0.665(1) C6D C 0.189(1) 0.053(1) 0.630(2) C4B C 0.2885(7) -0.1780(8) 0.665(1) C6B C 0.189(1) -0.053(1) 0.630(2) C4F C 0.7115(7) 0.1780(8) 0.335(1) H1F H 0.365(6) 0.078(5) 0.066(7) H2F H 0.333(5) 0.081(4) 0.245(6) H11F H 0.79000 0.03500 0.28100 H12F H 0.88000 0.09100 0.37000 H1D H 0.635(6) 0.078(5) 0.934(7) H2D H 0.667(5) 0.081(4) 0.755(6) H1B H 0.635(6) -0.078(5) 0.934(7) H2B H 0.667(5) -0.081(4) 0.755(6) H3D H 0.456(7) 0.148(7) 0.866(9) H4D H 0.563(5) 0.223(4) 0.846(6) H5D H 0.394(5) 0.281(5) 0.716(6) H6D H 0.415(5) 0.259(5) 0.561(6) H3B H 0.456(7) -0.148(7) 0.866(9) H4B H 0.563(5) -0.223(4) 0.846(6) H5B H 0.394(5) -0.281(5) 0.716(6) H6B H 0.415(5) -0.259(5) 0.561(6) H3F H 0.544(7) 0.148(7) 0.134(9) H4F H 0.437(5) 0.223(4) 0.154(6) H5F H 0.606(5) 0.281(5) 0.284(6) H6F H 0.585(5) 0.259(5) 0.439(6) H7D H 0.292(7) 0.153(7) 0.770(9) H8D H 0.226(5) 0.209(5) 0.666(6) H11D H 0.21000 0.03500 0.71900 H12D H 0.12000 0.09100 0.63000 H7B H 0.292(7) -0.153(7) 0.770(9) H8B H 0.226(5) -0.209(5) 0.666(6) H11B H 0.21000 -0.03500 0.71900 H12B H 0.12000 -0.09100 0.63000 H7F H 0.708(7) 0.153(7) 0.230(9) H8F H 0.774(5) 0.209(5) 0.334(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rb1 O1 3.067 1_555 1_555 O1 C1 1.450 1_555 1_555 O2 Rb1 2.986 1_555 1_555 O3 Rb1 3.004 1_555 1_555 C1 C2 1.486 1_555 1_555 C2 O2 1.407 1_555 1_555 C3 O2 1.436 1_555 1_555 C4 O3 1.421 1_555 1_555 C6 O3 1.442 1_555 1_555 H1 C1 1.047 1_555 1_555 H2 C1 1.023 1_555 1_555 H3 C2 1.067 1_555 1_555 H4 C2 0.874 1_555 1_555 H5 C3 0.928 1_555 1_555 H6 C3 0.961 1_555 1_555 H7 C4 1.099 1_555 1_555 H8 C4 0.836 1_555 1_555 H11 C6 0.943 1_555 1_555 H12 C6 0.950 1_555 1_555 O1D Rb1 3.067 1_555 1_555 O2D Rb1 2.986 1_555 1_555 O2B Rb1 2.986 1_555 1_555 O2F Rb1 2.986 1_555 1_555 O3D Rb1 3.004 1_555 1_555 O3B Rb1 3.004 1_555 1_555 O3F Rb1 3.004 1_555 1_555 C1F O1 1.450 1_555 1_555 C6F C6 1.440 1_555 1_555 C1D O1D 1.450 1_555 1_555 C1B O1D 1.450 1_555 1_555 C2D O2D 1.407 1_555 1_555 C3D O2D 1.436 1_555 1_555 C2B O2B 1.407 1_555 1_555 C3B O2B 1.436 1_555 1_555 C2F O2F 1.407 1_555 1_555 C3F O2F 1.436 1_555 1_555 C4D O3D 1.421 1_555 1_555 C6D O3D 1.442 1_555 1_555 C4B O3B 1.421 1_555 1_555 C6B O3B 1.442 1_555 1_555 C4F O3F 1.421 1_555 1_555 H1F C1F 1.047 1_555 1_555 H2F C1F 1.023 1_555 1_555 H11F C6F 0.943 1_555 1_555 H12F C6F 0.950 1_555 1_555 H1D C1D 1.047 1_555 1_555 H2D C1D 1.023 1_555 1_555 H1B C1B 1.047 1_555 1_555 H2B C1B 1.023 1_555 1_555 H3D C2D 1.067 1_555 1_555 H4D C2D 0.874 1_555 1_555 H5D C3D 0.928 1_555 1_555 H6D C3D 0.961 1_555 1_555 H3B C2B 1.067 1_555 1_555 H4B C2B 0.874 1_555 1_555 H5B C3B 0.928 1_555 1_555 H6B C3B 0.961 1_555 1_555 H3F C2F 1.067 1_555 1_555 H4F C2F 0.874 1_555 1_555 H5F C3F 0.928 1_555 1_555 H6F C3F 0.961 1_555 1_555 H7D C4D 1.099 1_555 1_555 H8D C4D 0.836 1_555 1_555 H11D C6D 0.943 1_555 1_555 H12D C6D 0.950 1_555 1_555 H7B C4B 1.099 1_555 1_555 H8B C4B 0.836 1_555 1_555 H11B C6B 0.943 1_555 1_555 H12B C6B 0.950 1_555 1_555 H7F C4F 1.099 1_555 1_555 H8F C4F 0.836 1_555 1_555 C3 C4 1.460 1_555 1_555 O3F C6F 1.442 1_555 1_555 C1F C2F 1.486 1_555 1_555 C1D C2D 1.486 1_555 1_555 C1B C2B 1.486 1_555 1_555 C3D C4D 1.460 1_555 1_555 C3B C4B 1.460 1_555 1_555 C3F C4F 1.460 1_555 1_555 C6D C6B 1.440 1_555 1_555 #END data_CSD_CIF_FUJCUI _audit_creation_date 1988-07-18 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD FUJCUI _database_code_depnum_ccdc_archive 'CCDC 1160900' _chemical_formula_sum 'C24 H48 Cs2 O12' _chemical_formula_moiety ; C24 H48 Cs1 O12 1+,Cs1 1- ; _journal_coden_Cambridge 4 _journal_volume 109 _journal_year 1987 _journal_page_first 5561 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "R.H.Huang" "D.L.Ward" "M.E.Kuchenmeister" "J.L.Dye" _chemical_name_systematic ; Cesium-bis(1,4,7,10,13,16-hexaoxacyclo-octadecane-O,O',O'',O''',O'''',O''''') ceside ; _chemical_name_common ; Cesium-bis(18-crown-6) ceside; Teaching Subset: Fundamental Chemistry ; _chemical_melting_point 253.15 _cell_volume 8312.732 _exptl_crystal_colour 'bronze' _exptl_crystal_density_diffrn 1.27 _exptl_special_details ; Melts with decomposition. air- and moisture-sensitive ; _diffrn_ambient_temperature 204 _refine_special_details ; Large void space, possible disorder. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.041 _refine_ls_wR_factor_gt 0.041 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,1/2+y,1/2-z 5 -x,-y,-z 6 -1/2+x,y,-1/2-z 7 -1/2-x,-1/2+y,z 8 x,-1/2-y,-1/2+z _cell_length_a 16.212(8) _cell_length_b 16.374(6) _cell_length_c 31.315(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Cs 2.44 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Cs1 Cs 0.34763(4) 0.42001(3) 0.36264(2) O1 O 0.4636(5) 0.5064(4) 0.4312(2) O2 O 0.5077(5) 0.5372(4) 0.3433(3) O3 O 0.3824(5) 0.5604(4) 0.2809(2) O4 O 0.2260(5) 0.4780(4) 0.2890(2) O5 O 0.1829(4) 0.5353(3) 0.3710(2) O6 O 0.3044(5) 0.5816(4) 0.4324(2) O7 O 0.2389(5) 0.3601(4) 0.4383(2) O8 O 0.1887(5) 0.2994(4) 0.3561(3) O9 O 0.3060(5) 0.2581(4) 0.2921(2) O10 O 0.4609(6) 0.3390(4) 0.2906(3) O11 O 0.5152(5) 0.3048(4) 0.3755(3) O12 O 0.3970(5) 0.2826(4) 0.4419(2) C1 C 0.5458(9) 0.5090(8) 0.4142(5) C2 C 0.5552(8) 0.5658(7) 0.3771(4) C3 C 0.5151(7) 0.5891(6) 0.3072(4) C4 C 0.4660(8) 0.5557(6) 0.2720(4) C5 C 0.3314(8) 0.5337(6) 0.2461(3) C6 C 0.2441(9) 0.5365(7) 0.2582(3) C7 C 0.1442(7) 0.4824(6) 0.3051(4) C8 C 0.1317(7) 0.5500(6) 0.3357(4) C9 C 0.1711(7) 0.5952(5) 0.4043(4) C10 C 0.2213(8) 0.5729(7) 0.4434(3) C11 C 0.3562(8) 0.5664(6) 0.4688(3) C12 C 0.4430(9) 0.5756(7) 0.4555(4) C13 C 0.1575(7) 0.3491(6) 0.4252(4) C14 C 0.1424(8) 0.2817(6) 0.3936(4) C15 C 0.1755(7) 0.2393(6) 0.3240(4) C16 C 0.2221(8) 0.2639(6) 0.2852(3) C17 C 0.353(1) 0.2775(7) 0.2546(4) C18 C 0.439(1) 0.2727(7) 0.2649(4) C19 C 0.5440(9) 0.3389(7) 0.3043(5) C20 C 0.5597(9) 0.2791(8) 0.3383(5) C21 C 0.5255(8) 0.2539(7) 0.4097(4) C22 C 0.4847(8) 0.2837(7) 0.4484(4) C23 C 0.3549(9) 0.3105(7) 0.4777(3) C24 C 0.265(1) 0.3028(7) 0.4706(3) H1 H 0.56300 0.45500 0.40700 H2 H 0.58000 0.53000 0.43600 H3 H 0.54100 0.62100 0.38400 H4 H 0.61100 0.56300 0.36800 H5 H 0.57100 0.59200 0.29900 H6 H 0.49600 0.64200 0.31400 H7 H 0.47700 0.58600 0.24700 H8 H 0.48000 0.50000 0.26700 H9 H 0.34600 0.47900 0.23900 H10 H 0.34000 0.56800 0.22200 H11 H 0.23100 0.58900 0.26900 H12 H 0.21200 0.52500 0.23300 H13 H 0.13100 0.43200 0.31900 H14 H 0.10800 0.49000 0.28200 H15 H 0.14600 0.60100 0.32300 H16 H 0.07600 0.55200 0.34400 H17 H 0.11400 0.59800 0.41100 H18 H 0.18900 0.64700 0.39400 H19 H 0.20800 0.60900 0.46600 H20 H 0.21000 0.51800 0.45200 H21 H 0.34600 0.51300 0.48000 H22 H 0.34500 0.60500 0.49000 H23 H 0.45200 0.62500 0.44000 H24 H 0.47700 0.57600 0.48000 H25 H 0.13800 0.39900 0.41300 H26 H 0.12600 0.33700 0.45000 H27 H 0.15900 0.23100 0.40500 H28 H 0.08500 0.28000 0.38700 H29 H 0.11900 0.23700 0.31700 H30 H 0.19300 0.18700 0.33400 H31 H 0.20700 0.22800 0.26300 H32 H 0.20900 0.31900 0.27800 H33 H 0.33800 0.33000 0.24500 H34 H 0.34100 0.23800 0.23300 H35 H 0.45000 0.22300 0.28000 H36 H 0.47100 0.27400 0.23900 H37 H 0.55800 0.39100 0.31500 H38 H 0.57800 0.32600 0.28100 H39 H 0.53800 0.22800 0.33000 H40 H 0.61700 0.27400 0.34400 H41 H 0.58300 0.24800 0.41500 H42 H 0.50300 0.20200 0.40300 H43 H 0.49900 0.25100 0.47200 H44 H 0.50200 0.33800 0.45400 H45 H 0.37000 0.36500 0.48400 H46 H 0.36900 0.27700 0.50100 H47 H 0.25100 0.24900 0.46200 H48 H 0.23700 0.31500 0.49600 Cs2 Cs 0.35442(8) 0.42456(9) 0.09779(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cs1 O1 3.185 1_555 1_555 O1 C1 1.436 1_555 1_555 O2 Cs1 3.284 1_555 1_555 O3 Cs1 3.486 1_555 1_555 O4 Cs1 3.179 1_555 1_555 O5 Cs1 3.281 1_555 1_555 O6 Cs1 3.502 1_555 1_555 O7 Cs1 3.112 1_555 1_555 O8 Cs1 3.253 1_555 1_555 O9 Cs1 3.516 1_555 1_555 O10 Cs1 3.197 1_555 1_555 O11 Cs1 3.332 1_555 1_555 O12 Cs1 3.444 1_555 1_555 C1 C2 1.496 1_555 1_555 C2 O2 1.390 1_555 1_555 C3 O2 1.419 1_555 1_555 C4 O3 1.386 1_555 1_555 C5 O3 1.436 1_555 1_555 C6 O4 1.391 1_555 1_555 C7 O4 1.421 1_555 1_555 C8 O5 1.403 1_555 1_555 C9 O5 1.444 1_555 1_555 C10 O6 1.398 1_555 1_555 C11 O6 1.438 1_555 1_555 C12 O1 1.405 1_555 1_555 C13 O7 1.394 1_555 1_555 C14 O8 1.424 1_555 1_555 C15 O8 1.423 1_555 1_555 C16 O9 1.381 1_555 1_555 C17 O9 1.435 1_555 1_555 C18 O10 1.397 1_555 1_555 C19 O10 1.414 1_555 1_555 C20 O11 1.433 1_555 1_555 C21 O11 1.367 1_555 1_555 C22 O12 1.436 1_555 1_555 C23 O12 1.390 1_555 1_555 C24 O7 1.443 1_555 1_555 H1 C1 0.954 1_555 1_555 H2 C1 0.944 1_555 1_555 H3 C2 0.957 1_555 1_555 H4 C2 0.950 1_555 1_555 H5 C3 0.943 1_555 1_555 H6 C3 0.944 1_555 1_555 H7 C4 0.944 1_555 1_555 H8 C4 0.953 1_555 1_555 H9 C5 0.953 1_555 1_555 H10 C5 0.951 1_555 1_555 H11 C6 0.948 1_555 1_555 H12 C6 0.964 1_555 1_555 H13 C7 0.957 1_555 1_555 H14 C7 0.940 1_555 1_555 H15 C8 0.954 1_555 1_555 H16 C8 0.940 1_555 1_555 H17 C9 0.950 1_555 1_555 H18 C9 0.953 1_555 1_555 H19 C10 0.947 1_555 1_555 H20 C10 0.956 1_555 1_555 H21 C11 0.956 1_555 1_555 H22 C11 0.934 1_555 1_555 H23 C12 0.955 1_555 1_555 H24 C12 0.945 1_555 1_555 H25 C13 0.956 1_555 1_555 H26 C13 0.950 1_555 1_555 H27 C14 0.943 1_555 1_555 H28 C14 0.954 1_555 1_555 H29 C15 0.943 1_555 1_555 H30 C15 0.955 1_555 1_555 H31 C16 0.943 1_555 1_555 H32 C16 0.954 1_555 1_555 H33 C17 0.943 1_555 1_555 H34 C17 0.956 1_555 1_555 H35 C18 0.958 1_555 1_555 H36 C18 0.963 1_555 1_555 H37 C19 0.944 1_555 1_555 H38 C19 0.939 1_555 1_555 H39 C20 0.944 1_555 1_555 H40 C20 0.950 1_555 1_555 H41 C21 0.952 1_555 1_555 H42 C21 0.948 1_555 1_555 H43 C22 0.942 1_555 1_555 H44 C22 0.949 1_555 1_555 H45 C23 0.946 1_555 1_555 H46 C23 0.941 1_555 1_555 H47 C24 0.949 1_555 1_555 H48 C24 0.937 1_555 1_555 C3 C4 1.466 1_555 1_555 C5 C6 1.466 1_555 1_555 C7 C8 1.478 1_555 1_555 C9 C10 1.515 1_555 1_555 C11 C12 1.475 1_555 1_555 C13 C14 1.502 1_555 1_555 C15 C16 1.486 1_555 1_555 C17 C18 1.433 1_555 1_555 C19 C20 1.469 1_555 1_555 C21 C22 1.464 1_555 1_555 C23 C24 1.480 1_555 1_555 #END data_CSD_CIF_FUJDAP _audit_creation_date 1988-07-17 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD FUJDAP _database_code_depnum_ccdc_archive 'CCDC 1160901' _chemical_formula_sum 'C18 H36 Cs2 N2 O6' _chemical_formula_moiety ; C18 H36 Cs1 N2 O6 1+,Cs1 1- ; _journal_coden_Cambridge 4 _journal_volume 109 _journal_year 1987 _journal_page_first 5561 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "R.H.Huang" "D.L.Ward" "M.E.Kuchenmeister" "J.L.Dye" _chemical_name_systematic ; Cesium-(4,7,13,16,21,24-Hexaoxa-1,10-diazabicyclo(8.8.8)hexacosane-O,O',O'',O' '',O'''',O''''',N,N') ceside ; _chemical_name_common ; Cesium-(cryptand(2.2.2)) ceside ; _chemical_melting_point 253.15 _cell_volume 3227.689 _exptl_crystal_colour 'bronze' _exptl_crystal_density_diffrn 1.32 _exptl_special_details ; Melts with decomposition. air- and moisture-sensitive ; _diffrn_ambient_temperature 206 _refine_special_details ; Large void space, possible disorder. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.057 _refine_ls_wR_factor_gt 0.057 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 -1/2+x,-1/2-y,-1/2+z _cell_length_a 13.371(2) _cell_length_b 11.252(2) _cell_length_c 21.529(3) _cell_angle_alpha 90 _cell_angle_beta 94.80(1) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Cs 2.01 N 0.68 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Cs1 Cs 0.2363(1) 0.0587(2) 0.58667(7) O1 O 0.345(1) 0.276(1) 0.6304(7) O2 O 0.459(1) 0.063(2) 0.5946(7) O3 O 0.220(1) -0.136(1) 0.6801(7) O4 O 0.082(1) 0.066(2) 0.6780(6) O5 O 0.114(1) 0.155(2) 0.4818(7) O6 O 0.194(1) -0.081(1) 0.4703(6) N1 N 0.117(1) 0.290(2) 0.6012(8) N2 N 0.345(2) -0.178(2) 0.5732(9) C1 C 0.187(1) 0.379(2) 0.629(1) C2 C 0.293(2) 0.376(2) 0.608(1) C3 C 0.444(2) 0.270(2) 0.615(1) C4 C 0.490(2) 0.158(2) 0.635(1) C5 C 0.496(2) -0.048(2) 0.612(1) C6 C 0.453(2) -0.146(2) 0.571(1) C7 C 0.332(2) -0.254(2) 0.625(1) C8 C 0.232(2) -0.248(2) 0.649(1) C9 C 0.130(2) -0.132(2) 0.708(1) C10 C 0.107(2) -0.006(2) 0.7288(9) C11 C 0.068(2) 0.190(3) 0.696(1) C12 C 0.040(2) 0.263(2) 0.641(1) C13 C 0.082(2) 0.336(2) 0.538(1) C14 C 0.038(2) 0.239(2) 0.495(1) C15 C 0.082(2) 0.077(3) 0.432(1) C16 C 0.172(2) -0.002(2) 0.4214(9) C17 C 0.279(2) -0.149(2) 0.461(1) C18 C 0.304(2) -0.231(2) 0.513(1) H1 H 0.19200 0.36500 0.67200 H2 H 0.15900 0.45600 0.62000 H3 H 0.28800 0.37200 0.56300 H4 H 0.32900 0.44600 0.62100 H5 H 0.48200 0.33400 0.63300 H6 H 0.44400 0.27400 0.57100 H7 H 0.56100 0.16400 0.63700 H8 H 0.46900 0.14200 0.67500 H9 H 0.47500 -0.06500 0.65200 H10 H 0.56700 -0.05200 0.61400 H11 H 0.45800 -0.11500 0.53100 H12 H 0.49200 -0.21700 0.57600 H13 H 0.38000 -0.23000 0.65700 H14 H 0.34400 -0.33400 0.61300 H15 H 0.18400 -0.25200 0.61400 H16 H 0.22200 -0.31200 0.67700 H17 H 0.13300 -0.18400 0.74300 H18 H 0.07600 -0.15400 0.67900 H19 H 0.05300 -0.00800 0.75500 H20 H 0.16600 0.02300 0.75200 H21 H 0.12900 0.22100 0.71500 H22 H 0.01800 0.19400 0.72400 H23 H -0.01100 0.22000 0.61700 H24 H 0.01300 0.33600 0.65400 H25 H 0.13500 0.37400 0.51900 H26 H 0.03100 0.39100 0.54400 H27 H -0.01400 0.19900 0.51500 H28 H 0.01200 0.27300 0.45700 H29 H 0.05900 0.12100 0.39600 H30 H 0.02900 0.02700 0.44400 H31 H 0.15600 -0.04400 0.38400 H32 H 0.22800 0.04800 0.41700 H33 H 0.33300 -0.09600 0.45800 H34 H 0.26700 -0.19300 0.42400 H35 H 0.24700 -0.27800 0.51900 H36 H 0.35700 -0.28100 0.50100 Cs2 Cs 0.7442(2) 0.0689(3) 0.8196(1) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cs1 O1 2.958 1_555 1_555 O1 C2 1.388 1_555 1_555 O2 Cs1 2.969 1_555 1_555 O3 Cs1 2.994 1_555 1_555 O4 Cs1 2.968 1_555 1_555 O5 Cs1 2.886 1_555 1_555 O6 Cs1 2.972 1_555 1_555 N1 Cs1 3.082 1_555 1_555 N2 Cs1 3.059 1_555 1_555 C1 N1 1.464 1_555 1_555 C2 C1 1.524 1_555 1_555 C3 O1 1.393 1_555 1_555 C4 O2 1.418 1_555 1_555 C5 O2 1.383 1_555 1_555 C6 N2 1.493 1_555 1_555 C7 N2 1.427 1_555 1_555 C8 O3 1.442 1_555 1_555 C9 O3 1.390 1_555 1_555 C10 O4 1.379 1_555 1_555 C11 O4 1.464 1_555 1_555 C12 N1 1.426 1_555 1_555 C13 N1 1.494 1_555 1_555 C14 O5 1.434 1_555 1_555 C15 O5 1.423 1_555 1_555 C16 O6 1.390 1_555 1_555 C17 O6 1.398 1_555 1_555 C18 N2 1.489 1_555 1_555 H1 C1 0.936 1_555 1_555 H2 C1 0.957 1_555 1_555 H3 C2 0.967 1_555 1_555 H4 C2 0.953 1_555 1_555 H5 C3 0.945 1_555 1_555 H6 C3 0.948 1_555 1_555 H7 C4 0.949 1_555 1_555 H8 C4 0.945 1_555 1_555 H9 C5 0.947 1_555 1_555 H10 C5 0.948 1_555 1_555 H11 C6 0.937 1_555 1_555 H12 C6 0.955 1_555 1_555 H13 C7 0.941 1_555 1_555 H14 C7 0.954 1_555 1_555 H15 C8 0.949 1_555 1_555 H16 C8 0.956 1_555 1_555 H17 C9 0.952 1_555 1_555 H18 C9 0.947 1_555 1_555 H19 C10 0.953 1_555 1_555 H20 C10 0.955 1_555 1_555 H21 C11 0.948 1_555 1_555 H22 C11 0.938 1_555 1_555 H23 C12 0.952 1_555 1_555 H24 C12 0.949 1_555 1_555 H25 C13 0.949 1_555 1_555 H26 C13 0.938 1_555 1_555 H27 C14 0.960 1_555 1_555 H28 C14 0.943 1_555 1_555 H29 C15 0.949 1_555 1_555 H30 C15 0.957 1_555 1_555 H31 C16 0.943 1_555 1_555 H32 C16 0.948 1_555 1_555 H33 C17 0.943 1_555 1_555 H34 C17 0.940 1_555 1_555 H35 C18 0.945 1_555 1_555 H36 C18 0.957 1_555 1_555 C3 C4 1.452 1_555 1_555 C5 C6 1.497 1_555 1_555 C7 C8 1.475 1_555 1_555 C9 C10 1.526 1_555 1_555 C11 C12 1.464 1_555 1_555 C13 C14 1.518 1_555 1_555 C15 C16 1.529 1_555 1_555 C17 C18 1.468 1_555 1_555 #END data_CSD_CIF_HAGNOT _audit_creation_date 2003-08-21 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD HAGNOT _database_code_depnum_ccdc_archive 'CCDC 210705' _chemical_formula_sum 'C40 H102 Ba2 N20 Na2' _chemical_formula_moiety ; 2(C18 H41 Ba1 N8 1+),Na2 2-,4(C1 H5 N1) ; _journal_coden_Cambridge 4 _journal_volume 125 _journal_year 2003 _journal_page_first 2259 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "M.Y.Redko" "R.H.Huang" "J.E.Jackson" "J.F.Harrison" "J.L.Dye" _chemical_name_systematic ; bis((1,4,7,10,13,16,21,24-Octa-azabicyclo(8.8.8)hexacosanide)-barium) disodide aminomethane solvate ; _chemical_name_common ; bis((Pentahydrogenocta-aza(2.2.2)cryptide)-barium) disodide aminomethane solvate ; _chemical_melting_point 249.15 _cell_volume 6279.667 _exptl_crystal_colour 'bronze' _exptl_special_details ; heat-sensitive Given dx 1.220 and fw 1153.84 are based on a hydrogen count of 72 and do not take into account the 10 azaprotons and H atoms on the solvent molecules which have not been refined ; _exptl_crystal_preparation 'aminomethane/diethyl ether' _diffrn_ambient_temperature 173 _refine_special_details ; One solvent molecule has an unrealistic C-N bond length (2.183) and has been suppressed. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_gt 0.0723 loop_ _citation_database_id_CSD _citation_special_details HAGNOT01 "is a reinterpretation of this cif" _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x,-y,1/2+z 3 1/2+x,1/2+y,z 4 1/2+x,1/2-y,1/2+z _cell_length_a 17.746(4) _cell_length_b 10.375(2) _cell_length_c 34.116(7) _cell_angle_alpha 90 _cell_angle_beta 91.29(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Ba 2.08 N 0.68 Na 1.89 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Ba1 Ba 0.3934(1) 0.0199(1) 0.3354(1) Ba2 Ba 0.1564(1) 0.4758(1) 0.0947(1) Na1 Na 0.0778(8) 0.1904(17) 0.4105(5) Na2 Na -0.0280(7) 0.1962(14) 0.5184(4) N1 N 0.3832(9) -0.1752(15) 0.2722(4) C1 C 0.3311(18) -0.275(2) 0.2750(7) C2 C 0.3373(18) -0.328(2) 0.3174(9) N2 N 0.3266(7) -0.2304(13) 0.3447(4) C3 C 0.3163(11) -0.283(2) 0.3847(6) C4 C 0.3021(14) -0.181(2) 0.4174(5) N3 N 0.3714(15) -0.084(2) 0.4172(7) C5 C 0.3446(15) 0.0265(19) 0.4468(7) C6 C 0.4078(16) 0.124(2) 0.4431(6) N4 N 0.3980(13) 0.203(2) 0.4092(5) C7 C 0.3349(19) 0.288(2) 0.4045(7) C8 C 0.3098(10) 0.3386(19) 0.3625(6) N5 N 0.2919(10) 0.2374(19) 0.3428(6) C9 C 0.277(3) 0.289(3) 0.2996(9) C10 C 0.2604(14) 0.1868(18) 0.2707(7) N6 N 0.3047(11) 0.074(2) 0.2737(6) C11 C 0.3058(17) -0.010(3) 0.2380(8) C12 C 0.3669(14) -0.098(3) 0.2348(8) C13 C 0.5338(16) -0.132(3) 0.2632(9) C14 C 0.4646(18) -0.230(3) 0.2627(8) N7 N 0.5348(13) -0.072(2) 0.3051(8) C15 C 0.5956(16) 0.034(3) 0.2985(9) C16 C 0.6054(13) 0.091(3) 0.3407(11) N8 N 0.5301(11) 0.163(2) 0.3541(6) C17 C 0.5419(14) 0.223(3) 0.3877(6) C18 C 0.4751(13) 0.285(2) 0.4035(6) N9 N 0.1473(9) 0.2869(19) 0.0273(5) C19 C 0.1438(13) 0.349(3) -0.0114(8) C20 C 0.1962(17) 0.474(3) -0.0125(8) N10 N 0.1892(7) 0.5701(15) 0.0142(4) C21 C 0.2459(13) 0.672(3) 0.0141(9) C22 C 0.2263(16) 0.779(3) 0.0393(6) N11 N 0.2408(7) 0.7240(13) 0.0820(4) C23 C 0.2135(11) 0.824(2) 0.1121(6) C24 C 0.2158(9) 0.764(2) 0.1529(6) N12 N 0.1519(9) 0.6638(16) 0.1630(5) C25 C 0.1800(16) 0.587(2) 0.1953(6) C26 C 0.2534(18) 0.504(3) 0.1888(10) N13 N 0.2390(14) 0.4205(18) 0.1579(5) C27 C 0.310(2) 0.340(3) 0.1545(8) C28 C 0.287(3) 0.224(3) 0.1276(8) N14 N 0.2699(12) 0.2682(19) 0.0897(5) C29 C 0.2371(14) 0.159(3) 0.0577(7) C30 C 0.2158(11) 0.202(2) 0.0224(7) C31 C 0.0882(17) 0.200(3) 0.0279(10) C32 C 0.0112(12) 0.286(2) 0.0337(7) N15 N 0.0161(11) 0.336(2) 0.0789(6) C33 C -0.0518(13) 0.392(2) 0.0884(6) C34 C -0.0460(13) 0.466(3) 0.1258(8) N16 N 0.0101(10) 0.5631(18) 0.1283(4) C35 C 0.0215(15) 0.638(2) 0.1639(6) C36 C 0.0833(9) 0.728(2) 0.1643(6) N17 N 0.4467(16) 0.247(3) 0.2655(6) C37 C 0.4403(16) 0.374(3) 0.2496(11) N18 N 0.1168(9) 0.923(2) 0.2922(6) C38 C 0.1881(16) 0.944(3) 0.3180(9) N19 N 0.1011(18) 0.262(3) 0.1669(9) C39 C 0.116(3) 0.110(3) 0.1765(10) N20? N 0.3691(15) 0.561(3) 0.1091(10) C40? C 0.488(6) 0.587(6) 0.125(2) H1 H 0.34240 -0.34290 0.25630 H2 H 0.28050 -0.24390 0.26940 H3 H 0.29970 -0.39450 0.32090 H4 H 0.38660 -0.36630 0.32170 H5 H 0.36090 -0.33220 0.39200 H6 H 0.27400 -0.34220 0.38380 H7 H 0.29890 -0.22270 0.44270 H8 H 0.25540 -0.13520 0.41200 H9 H 0.29630 0.06260 0.43860 H10 H 0.34130 -0.00570 0.47340 H11 H 0.40950 0.17860 0.46620 H12 H 0.45550 0.07920 0.44170 H13 H 0.34500 0.36290 0.42080 H14 H 0.29170 0.24450 0.41550 H15 H 0.26710 0.39640 0.36430 H16 H 0.35090 0.38410 0.35030 H17 H 0.23410 0.34810 0.29990 H18 H 0.32020 0.33730 0.29130 H19 H 0.20790 0.16220 0.27290 H20 H 0.26650 0.22270 0.24480 H21 H 0.25930 -0.05950 0.23700 H22 H 0.30550 0.04530 0.21510 H23 H 0.41180 -0.05040 0.22810 H24 H 0.35580 -0.15770 0.21350 H25 H 0.52660 -0.06600 0.24330 H26 H 0.58060 -0.17710 0.25840 H27 H 0.47610 -0.29810 0.28140 H28 H 0.46160 -0.26970 0.23690 H29 H 0.64230 -0.00270 0.28940 H30 H 0.57790 0.09890 0.28000 H31 H 0.64690 0.15240 0.34110 H32 H 0.61780 0.02260 0.35900 H33 H 0.58050 0.28780 0.38410 H34 H 0.56120 0.16140 0.40680 H35 H 0.46280 0.35760 0.38650 H36 H 0.48950 0.32060 0.42890 H37 H 0.09220 0.37300 -0.01770 H38 H 0.16000 0.28780 -0.03110 H39 H 0.24800 0.44400 -0.01070 H40 H 0.18930 0.51210 -0.03820 H41 H 0.29410 0.63720 0.02270 H42 H 0.25120 0.70400 -0.01250 H43 H 0.17390 0.80290 0.03540 H44 H 0.25790 0.85300 0.03450 H45 H 0.24570 0.89940 0.11160 H46 H 0.16250 0.85050 0.10530 H47 H 0.21400 0.83360 0.17190 H48 H 0.26410 0.72160 0.15660 H49 H 0.14020 0.52870 0.20290 H50 H 0.18980 0.64430 0.21730 H51 H 0.29530 0.56050 0.18270 H52 H 0.26650 0.45630 0.21240 H53 H 0.35010 0.38990 0.14280 H54 H 0.32760 0.31010 0.18010 H55 H 0.32750 0.16150 0.12680 H56 H 0.24290 0.18110 0.13810 H57 H 0.27590 0.09420 0.05430 H58 H 0.19430 0.11610 0.06920 H59 H 0.20360 0.13060 0.00520 H60 H 0.25630 0.25140 0.01100 H61 H 0.09510 0.13970 0.04940 H62 H 0.08510 0.15200 0.00350 H63 H 0.00990 0.35870 0.01570 H64 H -0.03340 0.23410 0.02910 H65 H -0.08980 0.32580 0.09090 H66 H -0.06790 0.44980 0.06740 H67 H -0.09440 0.50650 0.13020 H68 H -0.03690 0.40550 0.14700 H69 H 0.02880 0.57920 0.18560 H70 H -0.02440 0.68630 0.16860 H71 H 0.07840 0.78510 0.14200 H72 H 0.08190 0.77960 0.18790 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ba1 N1 2.960 1_555 1_555 Ba2 N9 3.023 1_555 1_555 Na1 Na2 4.170 1_555 1_555 N1 C1 1.393 1_555 1_555 C1 C2 1.549 1_555 1_555 C2 N2 1.392 1_555 1_555 N2 Ba1 2.875 1_555 1_555 C3 N2 1.485 1_555 1_555 C4 C3 1.562 1_555 1_555 N3 Ba1 3.025 1_555 1_555 C5 N3 1.607 1_555 1_555 C6 C5 1.518 1_555 1_555 N4 Ba1 3.154 1_555 1_555 C7 N4 1.432 1_555 1_555 C8 C7 1.581 1_555 1_555 N5 Ba1 2.902 1_555 1_555 C9 N5 1.585 1_555 1_555 C10 C9 1.473 1_555 1_555 N6 Ba1 2.660 1_555 1_555 C11 N6 1.498 1_555 1_555 C12 N1 1.529 1_555 1_555 C13 C14 1.594 1_555 1_555 C14 N1 1.592 1_555 1_555 N7 Ba1 2.897 1_555 1_555 C15 N7 1.561 1_555 1_555 C16 C15 1.563 1_555 1_555 N8 Ba1 2.903 1_555 1_555 C17 N8 1.317 1_555 1_555 C18 N4 1.627 1_555 1_555 N9 C19 1.469 1_555 1_555 C19 C20 1.597 1_555 1_555 C20 N10 1.358 1_555 1_555 N10 Ba2 2.985 1_555 1_555 C21 N10 1.460 1_555 1_555 C22 C21 1.451 1_555 1_555 N11 Ba2 3.015 1_555 1_555 C23 N11 1.545 1_555 1_555 C24 C23 1.524 1_555 1_555 N12 Ba2 3.041 1_555 1_555 C25 N12 1.440 1_555 1_555 C26 C25 1.581 1_555 1_555 N13 Ba2 2.643 1_555 1_555 C27 N13 1.518 1_555 1_555 C28 C27 1.562 1_555 1_555 N14 Ba2 2.956 1_555 1_555 C29 N14 1.669 1_555 1_555 C30 N9 1.513 1_555 1_555 C31 N9 1.384 1_555 1_555 C32 C31 1.648 1_555 1_555 N15 Ba2 2.921 1_555 1_555 C33 N15 1.383 1_555 1_555 C34 C33 1.491 1_555 1_555 N16 Ba2 3.001 1_555 1_555 C35 N16 1.452 1_555 1_555 C36 N12 1.389 1_555 1_555 N17 C37 1.428 1_555 1_555 N18 C38 1.540 1_555 1_555 N19 C39 1.631 1_555 1_555 H1 C1 0.974 1_555 1_555 H2 C1 0.969 1_555 1_555 H3 C2 0.969 1_555 1_555 H4 C2 0.969 1_555 1_555 H5 C3 0.970 1_555 1_555 H6 C3 0.970 1_555 1_555 H7 C4 0.968 1_555 1_555 H8 C4 0.969 1_555 1_555 H9 C5 0.971 1_555 1_555 H10 C5 0.970 1_555 1_555 H11 C6 0.970 1_555 1_555 H12 C6 0.968 1_555 1_555 H13 C7 0.970 1_555 1_555 H14 C7 0.972 1_555 1_555 H15 C8 0.969 1_555 1_555 H16 C8 0.970 1_555 1_555 H17 C9 0.978 1_555 1_555 H18 C9 0.964 1_555 1_555 H19 C10 0.971 1_555 1_555 H20 C10 0.967 1_555 1_555 H21 C11 0.972 1_555 1_555 H22 C11 0.969 1_555 1_555 H23 C12 0.969 1_555 1_555 H24 C12 0.972 1_555 1_555 H25 C13 0.971 1_555 1_555 H26 C13 0.970 1_555 1_555 H27 C14 0.971 1_555 1_555 H28 C14 0.972 1_555 1_555 H29 C15 0.969 1_555 1_555 H30 C15 0.970 1_555 1_555 H31 C16 0.974 1_555 1_555 H32 C16 0.967 1_555 1_555 H33 C17 0.970 1_555 1_555 H34 C17 0.970 1_555 1_555 H35 C18 0.972 1_555 1_555 H36 C18 0.971 1_555 1_555 H37 C19 0.968 1_555 1_555 H38 C19 0.973 1_555 1_555 H39 C20 0.971 1_555 1_555 H40 C20 0.967 1_555 1_555 H41 C21 0.968 1_555 1_555 H42 C21 0.973 1_555 1_555 H43 C22 0.969 1_555 1_555 H44 C22 0.967 1_555 1_555 H45 C23 0.969 1_555 1_555 H46 C23 0.969 1_555 1_555 H47 C24 0.971 1_555 1_555 H48 C24 0.969 1_555 1_555 H49 C25 0.970 1_555 1_555 H50 C25 0.970 1_555 1_555 H51 C26 0.973 1_555 1_555 H52 C26 0.969 1_555 1_555 H53 C27 0.973 1_555 1_555 H54 C27 0.972 1_555 1_555 H55 C28 0.969 1_555 1_555 H56 C28 0.975 1_555 1_555 H57 C29 0.971 1_555 1_555 H58 C29 0.971 1_555 1_555 H59 C30 0.967 1_555 1_555 H60 C30 0.971 1_555 1_555 H61 C31 0.970 1_555 1_555 H62 C31 0.971 1_555 1_555 H63 C32 0.973 1_555 1_555 H64 C32 0.967 1_555 1_555 H65 C33 0.968 1_555 1_555 H66 C33 0.972 1_555 1_555 H67 C34 0.971 1_555 1_555 H68 C34 0.968 1_555 1_555 H69 C35 0.966 1_555 1_555 H70 C35 0.973 1_555 1_555 H71 C36 0.967 1_555 1_555 H72 C36 0.968 1_555 1_555 C4 N3 1.589 1_555 1_555 C6 N4 1.425 1_555 1_555 C8 N5 1.283 1_555 1_555 C10 N6 1.412 1_555 1_555 C11 C12 1.424 1_555 1_555 C13 N7 1.559 1_555 1_555 C16 N8 1.606 1_555 1_555 C17 C18 1.462 1_555 1_555 C22 N11 1.580 1_555 1_555 C24 N12 1.582 1_555 1_555 C26 N13 1.384 1_555 1_555 C28 N14 1.399 1_555 1_555 C29 C30 1.331 1_555 1_555 C32 N15 1.627 1_555 1_555 C34 N16 1.418 1_555 1_555 C35 C36 1.440 1_555 1_555 #END data_CSD_CIF_HAGNOT01 _audit_creation_date 2008-06-05 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD HAGNOT01 _database_code_depnum_ccdc_archive 'CCDC 625620' _chemical_formula_sum 'C40 H102 Ba2 N20 Na2' _chemical_formula_moiety ; 2(C18 H41 Ba1 N8 1+),Na2 2-,4(C1 H5 N1) ; _journal_coden_Cambridge 155 _journal_volume 360 _journal_year 2007 _journal_page_first 4017 _journal_name_full 'Inorg.Chim.Acta ' loop_ _publ_author_name "R.E.Marsh" "D.A.Clemente" _chemical_name_systematic ; bis((1,4,7,10,13,16,21,24-Octa-azabicyclo(8.8.8)hexacosanide)-barium) disodide aminomethane solvate ; _chemical_name_common ; bis((Pentahydrogenocta-aza(2.2.2)cryptide)-barium) disodide aminomethane solvate ; _cell_volume 6279.667 _exptl_crystal_density_diffrn 1.252 _exptl_special_details ; authors have reassigned the C and N atoms in one solvent molecule as N and C (as compared with the original publication) as this is consistent with the intermolecular contacts ; _diffrn_ambient_temperature 173 loop_ _citation_database_id_CSD _citation_special_details HAGNOT "is reinterpreted by this entry" _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,z 3 -x,y,1/2-z 4 1/2-x,1/2+y,1/2-z 5 -x,-y,-z 6 -1/2-x,-1/2-y,-z 7 x,-y,-1/2+z 8 -1/2+x,-1/2-y,-1/2+z _cell_length_a 17.746(4) _cell_length_b 10.375(2) _cell_length_c 34.116(7) _cell_angle_alpha 90 _cell_angle_beta 91.29(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Ba 2.04 N 0.68 Na 1.89 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Ba1 Ba 0.36850 0.02205 0.12035 N1 N 0.36565 -0.16950 0.05460 N2 N 0.29290 -0.22720 0.13135 H1 H 0.24180 -0.20390 0.12640 N3 N 0.34110 -0.07705 0.20150 H2 H 0.38710 -0.11670 0.20970 N4 N 0.37535 0.20805 0.19095 N5 N 0.26100 0.23460 0.12655 H3 H 0.21690 0.20280 0.13850 N6 N 0.28285 0.07675 0.05790 N7 N 0.51235 -0.06755 0.08840 H4 H 0.52790 -0.12980 0.10740 N8 N 0.50700 0.16350 0.13760 H5 H 0.49910 0.23390 0.12020 C1 C 0.30765 -0.26950 0.06105 C2 C 0.31190 -0.32600 0.10265 C3 C 0.29500 -0.28100 0.17270 C4 C 0.27810 -0.17650 0.20165 C5 C 0.32420 0.02625 0.22965 C6 C 0.38200 0.13750 0.22725 C7 C 0.30955 0.29300 0.19105 C8 C 0.28635 0.33980 0.15240 C9 C 0.24500 0.28250 0.08600 C10 C 0.22520 0.17340 0.05810 C11 C 0.27620 -0.00700 0.02460 C12 C 0.34345 -0.09250 0.01975 C13 C 0.50615 -0.13500 0.04965 C14 C 0.44065 -0.22900 0.04920 C15 C 0.57080 0.03400 0.08635 C16 C 0.57860 0.09950 0.12615 C17 C 0.51535 0.21850 0.17700 C18 C 0.44345 0.29250 0.18780 N9 N 0.42280 0.24250 0.04930 C19 C 0.41215 0.38200 0.03655 N10 N 0.08940 0.91800 0.08360 C20 C 0.15950 0.94150 0.10445 Na1 Na 0.05290 0.19330 0.19605 H6 H 0.31420 -0.33825 0.04220 H7 H 0.25820 -0.23275 0.05640 H8 H 0.27700 -0.39695 0.10465 H9 H 0.36205 -0.35840 0.10820 H10 H 0.34350 -0.31755 0.17830 H11 H 0.25805 -0.34760 0.17465 H12 H 0.27385 -0.21335 0.22760 H13 H 0.23065 -0.13620 0.19465 H14 H 0.27415 0.05930 0.22465 H15 H 0.32600 -0.00890 0.25580 H16 H 0.37475 0.19540 0.24865 H17 H 0.43165 0.10310 0.22970 H18 H 0.32070 0.36615 0.20780 H19 H 0.26770 0.24655 0.20225 H20 H 0.24560 0.40110 0.15500 H21 H 0.32830 0.38400 0.14055 H22 H 0.20330 0.34330 0.08655 H23 H 0.28865 0.32810 0.07660 H24 H 0.17808 0.13449 0.06579 H25 H 0.21811 0.20769 0.03182 H26 H 0.23200 -0.06000 0.02715 H27 H 0.26950 0.04450 0.00135 H28 H 0.38580 -0.03955 0.01260 H29 H 0.33300 -0.15100 -0.00190 H30 H 0.49890 -0.07260 0.02885 H31 H 0.55250 -0.18170 0.04490 H32 H 0.44885 -0.29160 0.06970 H33 H 0.43985 -0.27465 0.02450 H34 H 0.61835 -0.00460 0.07960 H35 H 0.55740 0.09670 0.06650 H36 H 0.61835 0.16330 0.12510 H37 H 0.59285 0.03640 0.14580 H38 H 0.55820 0.27654 0.17795 H39 H 0.52463 0.15003 0.19586 H40 H 0.43385 0.35895 0.16855 H41 H 0.45220 0.33430 0.21270 Na1B Na -0.05290 0.19330 0.30395 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ba1 N1 2.996 1_555 1_555 N1 C1 1.481 1_555 1_555 N2 Ba1 2.941 1_555 1_555 H1 N2 0.950 1_555 1_555 N3 Ba1 3.003 1_555 1_555 H2 N3 0.951 1_555 1_555 N4 Ba1 3.087 1_555 1_555 N5 Ba1 2.927 1_555 1_555 H3 N5 0.950 1_555 1_555 N6 Ba1 2.651 1_555 1_555 N7 Ba1 2.949 1_555 1_555 H4 N7 0.952 1_555 1_555 N8 Ba1 2.911 1_555 1_555 H5 N8 0.950 1_555 1_555 C1 C2 1.536 1_555 1_555 C2 N2 1.462 1_555 1_555 C3 N2 1.517 1_555 1_555 C4 N3 1.521 1_555 1_555 C5 N3 1.474 1_555 1_555 C6 N4 1.441 1_555 1_555 C7 N4 1.463 1_555 1_555 C8 N5 1.467 1_555 1_555 C9 N5 1.491 1_555 1_555 C10 N6 1.433 1_555 1_555 C11 N6 1.433 1_555 1_555 C12 N1 1.478 1_555 1_555 C13 N7 1.498 1_555 1_555 C14 N1 1.482 1_555 1_555 C15 N7 1.481 1_555 1_555 C16 N8 1.493 1_555 1_555 C17 N8 1.465 1_555 1_555 C18 N4 1.499 1_555 1_555 N9 C19 1.522 1_555 1_555 N10 C20 1.440 1_555 1_555 Na1 Na1B 4.170 1_555 1_555 H6 C1 0.969 1_555 1_555 H7 C1 0.967 1_555 1_555 H8 C2 0.965 1_555 1_555 H9 C2 0.966 1_555 1_555 H10 C3 0.956 1_555 1_555 H11 C3 0.956 1_555 1_555 H12 C4 0.969 1_555 1_555 H13 C4 0.965 1_555 1_555 H14 C5 0.964 1_555 1_555 H15 C5 0.964 1_555 1_555 H16 C6 0.956 1_555 1_555 H17 C6 0.953 1_555 1_555 H18 C7 0.968 1_555 1_555 H19 C7 0.971 1_555 1_555 H20 C8 0.969 1_555 1_555 H21 C8 0.970 1_555 1_555 H22 C9 0.973 1_555 1_555 H23 C9 0.968 1_555 1_555 H24 C10 0.970 1_555 1_555 H25 C10 0.970 1_555 1_555 H26 C11 0.963 1_555 1_555 H27 C11 0.962 1_555 1_555 H28 C12 0.967 1_555 1_555 H29 C12 0.971 1_555 1_555 H30 C13 0.967 1_555 1_555 H31 C13 0.971 1_555 1_555 H32 C14 0.963 1_555 1_555 H33 C14 0.966 1_555 1_555 H34 C15 0.967 1_555 1_555 H35 C15 0.965 1_555 1_555 H36 C16 0.969 1_555 1_555 H37 C16 0.967 1_555 1_555 H38 C17 0.970 1_555 1_555 H39 C17 0.970 1_555 1_555 H40 C18 0.965 1_555 1_555 H41 C18 0.963 1_555 1_555 C3 C4 1.501 1_555 1_555 C5 C6 1.548 1_555 1_555 C7 C8 1.456 1_555 1_555 C9 C10 1.515 1_555 1_555 C11 C12 1.499 1_555 1_555 C13 C14 1.517 1_555 1_555 C15 C16 1.522 1_555 1_555 C17 C18 1.541 1_555 1_555 #END data_CSD_CIF_HESJIY _audit_creation_date 1995-05-01 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD HESJIY _database_code_depnum_ccdc_fiz 'CSD 58375' _chemical_formula_sum 'C34 H30 Li1 P1' _chemical_formula_moiety ; C24 H20 P1 1+,C10 H10 Li1 1- ; _journal_coden_Cambridge 179 _journal_volume 33 _journal_year 1994 _journal_page_first 1744 _journal_name_full 'Angew.Chem.,Int.Ed. ' loop_ _publ_author_name "S.Harder" "M.H.Prosenc" _chemical_name_systematic ; Tetraphenylphosphonium bis(\h^5^-cyclopentadienyl)-lithium ; _cell_volume 1307.060 _exptl_crystal_colour 'yellow-brown' _exptl_crystal_density_diffrn 1.211 _diffrn_ambient_temperature 233 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.046 _refine_ls_wR_factor_gt 0.046 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,-1/2+z _cell_length_a 10.770(3) _cell_length_b 6.965(2) _cell_length_c 17.654(5) _cell_angle_alpha 90 _cell_angle_beta 99.25(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.30 P 1.05 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.00000 0.00000 0.00000 P1 P 0.50000 1.0611(1) 0.75000 C1 C -0.0532(3) 0.0939(6) 0.1193(2) C2 C -0.0412(3) 0.2608(5) 0.0782(2) C3 C -0.1327(3) 0.2525(5) 0.0137(2) C4 C -0.1965(3) 0.0868(5) 0.0161(2) C5 C -0.1486(3) -0.0094(5) 0.0799(2) C6 C 0.6309(2) 1.2130(3) 0.7396(1) C7 C 0.6154(2) 1.3504(3) 0.6812(1) C8 C 0.7128(2) 1.4721(3) 0.6723(1) C9 C 0.8258(2) 1.4597(3) 0.7218(1) C10 C 0.8414(2) 1.3259(3) 0.7803(1) C11 C 0.7450(2) 1.2017(3) 0.7896(1) C12 C 0.5399(2) 0.9057(3) 0.8312(1) C13 C 0.6412(2) 0.7808(3) 0.8309(1) C14 C 0.6757(2) 0.6579(3) 0.8917(1) C15 C 0.6083(2) 0.6570(3) 0.9524(1) C16 C 0.5062(2) 0.7758(3) 0.9517(1) C17 C 0.4715(2) 0.9024(3) 0.8913(1) H1 H -0.00330 0.05680 0.16710 H2 H 0.01890 0.36150 0.09240 H3 H -0.14800 0.34830 -0.02580 H4 H -0.26490 0.04480 -0.02200 H5 H -0.17810 -0.13180 0.09470 H6 H 0.53650 1.35970 0.64730 H7 H 0.70230 1.56450 0.63140 H8 H 0.89340 1.54500 0.71560 H9 H 0.91970 1.31950 0.81500 H10 H 0.75580 1.10810 0.83010 H11 H 0.68670 0.78250 0.78850 H12 H 0.74540 0.57200 0.89170 H13 H 0.63350 0.57360 0.99540 H14 H 0.45840 0.77070 0.99310 H15 H 0.40120 0.98740 0.89060 C1B C 0.0532(3) -0.0939(6) -0.1193(2) C2B C 0.0412(3) -0.2608(5) -0.0782(2) C3B C 0.1327(3) -0.2525(5) -0.0137(2) C4B C 0.1965(3) -0.0868(5) -0.0161(2) C5B C 0.1486(3) 0.0094(5) -0.0799(2) H1B H 0.00330 -0.05680 -0.16710 H2B H -0.01890 -0.36150 -0.09240 H3B H 0.14800 -0.34830 0.02580 H4B H 0.26490 -0.04480 0.02200 H5B H 0.17810 0.13180 -0.09470 C6A C 0.3691(2) 1.2130(3) 0.7604(1) C12A C 0.4601(2) 0.9057(3) 0.6688(1) C7A C 0.3846(2) 1.3504(3) 0.8188(1) C11A C 0.2550(2) 1.2017(3) 0.7104(1) C13A C 0.3588(2) 0.7808(3) 0.6691(1) C17A C 0.5285(2) 0.9024(3) 0.6087(1) C8A C 0.2872(2) 1.4721(3) 0.8277(1) H6A H 0.46350 1.35970 0.85270 C10A C 0.1586(2) 1.3259(3) 0.7197(1) H10A H 0.24420 1.10810 0.66990 C14A C 0.3243(2) 0.6579(3) 0.6083(1) H11A H 0.31330 0.78250 0.71150 C16A C 0.4938(2) 0.7758(3) 0.5483(1) H15A H 0.59880 0.98740 0.60940 C9A C 0.1742(2) 1.4597(3) 0.7782(1) H7A H 0.29770 1.56450 0.86860 H9A H 0.08030 1.31950 0.68500 C15A C 0.3917(2) 0.6570(3) 0.5476(1) H12A H 0.25460 0.57200 0.60830 H14A H 0.54160 0.77070 0.50690 H8A H 0.10660 1.54500 0.78440 H13A H 0.36650 0.57360 0.50460 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 C1 2.362 1_555 1_555 P1 C6 1.795 1_555 1_555 C1 C2 1.387 1_555 1_555 C2 Li1 2.366 1_555 1_555 C3 Li1 2.303 1_555 1_555 C4 Li1 2.262 1_555 1_555 C5 Li1 2.298 1_555 1_555 C6 C7 1.397 1_555 1_555 C7 C8 1.377 1_555 1_555 C8 C9 1.382 1_555 1_555 C9 C10 1.381 1_555 1_555 C10 C11 1.381 1_555 1_555 C11 C6 1.395 1_555 1_555 C12 P1 1.793 1_555 1_555 C13 C12 1.396 1_555 1_555 C14 C13 1.376 1_555 1_555 C15 C14 1.388 1_555 1_555 C16 C15 1.375 1_555 1_555 C17 C12 1.386 1_555 1_555 H1 C1 0.960 1_555 1_555 H2 C2 0.960 1_555 1_555 H3 C3 0.960 1_555 1_555 H4 C4 0.960 1_555 1_555 H5 C5 0.961 1_555 1_555 H6 C7 0.960 1_555 1_555 H7 C8 0.960 1_555 1_555 H8 C9 0.959 1_555 1_555 H9 C10 0.960 1_555 1_555 H10 C11 0.961 1_555 1_555 H11 C13 0.958 1_555 1_555 H12 C14 0.960 1_555 1_555 H13 C15 0.960 1_555 1_555 H14 C16 0.960 1_555 1_555 H15 C17 0.960 1_555 1_555 C1B Li1 2.362 1_555 1_555 C2B Li1 2.366 1_555 1_555 C3B Li1 2.303 1_555 1_555 C4B Li1 2.262 1_555 1_555 C5B Li1 2.298 1_555 1_555 H1B C1B 0.960 1_555 1_555 H2B C2B 0.960 1_555 1_555 H3B C3B 0.960 1_555 1_555 H4B C4B 0.960 1_555 1_555 H5B C5B 0.961 1_555 1_555 C6A P1 1.795 1_555 1_555 C12A P1 1.793 1_555 1_555 C7A C6A 1.397 1_555 1_555 C11A C6A 1.395 1_555 1_555 C13A C12A 1.396 1_555 1_555 C17A C12A 1.386 1_555 1_555 C8A C7A 1.377 1_555 1_555 H6A C7A 0.960 1_555 1_555 C10A C11A 1.381 1_555 1_555 H10A C11A 0.961 1_555 1_555 C14A C13A 1.376 1_555 1_555 H11A C13A 0.958 1_555 1_555 C16A C17A 1.388 1_555 1_555 H15A C17A 0.960 1_555 1_555 C9A C8A 1.382 1_555 1_555 H7A C8A 0.960 1_555 1_555 H9A C10A 0.960 1_555 1_555 C15A C14A 1.388 1_555 1_555 H12A C14A 0.960 1_555 1_555 H14A C16A 0.960 1_555 1_555 H8A C9A 0.959 1_555 1_555 H13A C15A 0.960 1_555 1_555 C1 C5 1.352 1_555 1_555 C2 C3 1.382 1_555 1_555 C3 C4 1.347 1_555 1_555 C4 C5 1.340 1_555 1_555 C16 C17 1.388 1_555 1_555 C1B C2B 1.387 1_555 1_555 C1B C5B 1.352 1_555 1_555 C2B C3B 1.382 1_555 1_555 C3B C4B 1.347 1_555 1_555 C4B C5B 1.340 1_555 1_555 C10A C9A 1.381 1_555 1_555 C16A C15A 1.375 1_555 1_555 #END data_CSD_CIF_IBUTOO _audit_creation_date 2001-10-05 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD IBUTOO _database_code_depnum_ccdc_archive 'CCDC 169012' _chemical_formula_sum 'C92 H142 Mo2 N12 Na2 O11' _chemical_formula_moiety ; C24 H48 Na1 O6 1+,C60 H78 Mo2 N12 Na1 O3 1-,2(C4 H8 O1) ; _journal_coden_Cambridge 9 _journal_volume 40 _journal_year 2001 _journal_page_first 3861 _journal_name_full 'Inorg.Chem. ' loop_ _publ_author_name "G.E.Greco" "R.R.Schrock" _chemical_name_systematic ; hexakis(Tetrahydrofuran)-sodium bis(\m~2~-diazenido)-bis(tris(2-(phenylamino)ethyl)amine)-tris(tetrahydrofuran ; _cell_volume 14390.173 _exptl_crystal_density_diffrn 1.268 _diffrn_ambient_temperature 183 _refine_special_details ; The three tetrahydrofuran molecules ligated to Na2 are disordered over two sites. The tetrahydrofuran solvent molecule is also disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_gt 0.0544 _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R -3 c' _symmetry_Int_Tables_number 167 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 y,x,1/2-z 5 -1/3+x,1/3+y,1/3+z 6 -1/3-y,1/3+x-y,1/3+z 7 -1/3-x+y,1/3-x,1/3+z 8 -1/3+y,1/3+x,-1/6-z 9 1/3+x,-1/3+y,-1/3+z 10 1/3+y,-1/3+x,1/6-z 11 -x+y,y,1/2+z 12 x,x-y,1/2+z 13 -1/3+y,1/3-x+y,1/3-z 14 -1/3+x-y,1/3+x,1/3-z 15 -1/3-x+y,1/3+y,-1/6+z 16 -1/3+x,1/3+x-y,-1/6+z 17 1/3-x+y,-1/3+y,1/6+z 18 1/3+x,-1/3+x-y,1/6+z 19 -x,-y,-z 20 y,-x+y,-z 21 x-y,x,-z 22 -y,-x,-1/2+z 23 1/3-x,-1/3-y,-1/3-z 24 1/3+y,-1/3-x+y,-1/3-z 25 1/3+x-y,-1/3+x,-1/3-z 26 1/3-y,-1/3-x,1/6+z 27 -1/3-x,1/3-y,1/3-z 28 -1/3-y,1/3-x,-1/6+z 29 x-y,-y,-1/2-z 30 -x,-x+y,-1/2-z 31 1/3-y,-1/3+x-y,-1/3+z 32 1/3-x+y,-1/3-x,-1/3+z 33 1/3+x-y,-1/3-y,1/6-z 34 1/3-x,-1/3-x+y,1/6-z 35 -1/3+x-y,1/3-y,-1/6-z 36 -1/3-x,1/3-x+y,-1/6-z _cell_length_a 13.3659(15) _cell_length_b 13.3659(15) _cell_length_c 93.012(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 loop_ _atom_type_symbol _atom_type_radius_bond C 0.62 H 0.23 Mo 1.47 N 0.68 Na 1.47 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Mo1 Mo 0.66670 0.33330 0.027246(10) Na1 Na 0.66670 0.33330 0.08330 Na2 Na 0.00000 0.00000 0.00000 N1 N 0.66670 0.33330 0.04726(14) N2 N 0.66670 0.33330 0.06011(15) N3 N 0.5268(4) 0.3523(4) 0.02374(6) N4 N 0.66670 0.33330 0.00349(10) O1 O 0.1392(4) -0.0112(4) 0.01494(5) O2 O 0.4772(10) 0.1439(10) 0.08330 O3? O 0.33330 0.66670 0.0785(6) C1 C 0.4591(5) 0.3740(6) 0.03345(8) C2 C 0.4297(6) 0.3162(7) 0.04649(9) H1 H 0.45430 0.26390 0.04860 C3 C 0.3634(7) 0.3353(8) 0.05657(10) H2 H 0.34420 0.29620 0.06530 C4 C 0.3265(7) 0.4127(10) 0.05344(13) H3 H 0.28320 0.42650 0.06010 C5 C 0.3538(7) 0.4694(8) 0.04048(14) H4 H 0.32840 0.52110 0.03840 C6 C 0.4194(6) 0.4497(6) 0.03049(9) H5 H 0.43680 0.48780 0.02170 C7 C 0.5122(6) 0.3760(6) 0.00883(8) H6 H 0.55700 0.45850 0.00700 H7 H 0.43160 0.35080 0.00700 C8 C 0.6876(6) 0.2402(6) -0.00116(8) H8 H 0.76980 0.26720 -0.00090 H9 H 0.66060 0.21780 -0.01090 C9 C 0.4280(13) 0.0730(14) 0.07092(14) C10? C 0.306(3) 0.009(8) 0.0755(5) C11 C 0.359(6) -0.032(3) 0.0746(3) C12 C 0.2606(6) 0.0694(6) 0.01408(8) H10 H 0.27540 0.14760 0.01550 H11 H 0.29020 0.06480 0.00470 C13 C 0.3162(7) 0.0390(8) 0.02534(11) H12 H 0.34880 -0.00570 0.02140 H13 H 0.37760 0.10800 0.02980 C14 C 0.2296(8) -0.0268(9) 0.03541(10) H14 H 0.22860 0.02210 0.04310 H15 H 0.24240 -0.08590 0.03960 C15 C 0.1191(6) -0.0801(7) 0.02727(9) H16 H 0.09640 -0.15870 0.02460 H17 H 0.05810 -0.08160 0.03310 C16? C 0.303(3) 0.556(3) 0.0874(4) C17? C 0.332(4) 0.603(3) 0.1024(4) N2I N 0.66663 0.33337 0.106557(150) N1I N 0.66663 0.33337 0.119407(140) Mo1I Mo 0.66663 0.33337 0.139421(10) N3I N 0.685633(400) 0.193467(400) 0.142927(60) C1I C 0.707333(500) 0.125767(600) 0.133217(80) C2I C 0.649533(600) 0.096367(700) 0.120177(90) H1I H 0.59723 0.12097 0.11807 C3I C 0.668633(700) 0.030067(800) 0.110097(100) H2I H 0.62953 0.01087 0.10137 C4I C 0.746033(700) -0.006833(1000) 0.113227(130) H3I H 0.75983 -0.05013 0.10657 C5I C 0.802733(700) 0.020467(800) 0.126187(140) H4I H 0.85443 -0.00493 0.12827 C6I C 0.783033(600) 0.086067(600) 0.136177(90) H5I H 0.82113 0.10347 0.14497 C7I C 0.709333(600) 0.178867(600) 0.157837(80) H6I H 0.79183 0.22367 0.15967 H7I H 0.68413 0.09827 0.15967 C8GA C 0.645733(600) 0.219267(600) 0.167827(80) N4GA N 0.66663 0.33327 0.163177(100) N3FA N 0.507833(400) 0.314367(400) 0.142927(60) C1FA C 0.418433(500) 0.292667(600) 0.133217(80) C2FA C 0.446833(600) 0.350467(700) 0.120177(90) H1FA H 0.52373 0.40277 0.11807 C3FA C 0.361433(700) 0.331367(800) 0.110097(100) H2FA H 0.38133 0.37047 0.10137 C4FA C 0.247133(700) 0.253967(1000) 0.113227(130) H3FA H 0.19003 0.24017 0.10657 C5FA C 0.217733(700) 0.197267(800) 0.126187(140) H4FA H 0.14063 0.14557 0.12827 C6FA C 0.303033(600) 0.216967(600) 0.136177(90) H5FA H 0.28233 0.17887 0.14497 C7FA C 0.469533(600) 0.290667(600) 0.157837(80) H6FA H 0.43183 0.20817 0.15967 H7FA H 0.41413 0.31587 0.15967 C8I C 0.573533(600) 0.354267(600) 0.167827(80) C8FA C 0.780733(600) 0.426467(600) 0.167827(80) C7GA C 0.821133(600) 0.530467(600) 0.157837(80) N3GA N 0.806533(400) 0.492167(400) 0.142927(60) C1GA C 0.874233(500) 0.581567(600) 0.133217(80) C2GA C 0.903633(600) 0.553167(700) 0.120177(90) H1GA H 0.87903 0.47627 0.11807 C3GA C 0.969933(700) 0.638567(800) 0.110097(100) H2GA H 0.98913 0.61867 0.10137 C4GA C 1.006833(700) 0.752867(1000) 0.113227(130) H3GA H 1.05013 0.80997 0.10657 C5GA C 0.979533(700) 0.782267(800) 0.126187(140) H4GA H 1.00493 0.85937 0.12827 C6GA C 0.913933(600) 0.696967(600) 0.136177(90) H5GA H 0.89653 0.71767 0.14497 H6GA H 0.77633 0.56817 0.15967 H7GA H 0.90173 0.58587 0.15967 H8FA H 0.83593 0.39947 0.16757 H9FA H 0.77613 0.44887 0.17757 H8I H 0.60053 0.43647 0.16757 H9I H 0.55113 0.32727 0.17757 H8GA H 0.56353 0.16407 0.16757 H9GA H 0.67273 0.22387 0.17757 C9I C 0.406333(1300) 0.094667(1400) 0.095747(140) C11I C 0.301333(6000) 0.025667(3000) 0.092067(300) O2A O 0.8561(10) 0.3333(10) 0.08330 C9A C 0.9270(13) 0.3550(14) 0.07092(14) C11A C 1.032(6) 0.391(3) 0.0746(3) C9GA C 0.905333(1300) 0.311667(1400) 0.095747(140) C11GA C 0.974333(6000) 0.275667(3000) 0.092067(300) O2B O 0.6667(10) 0.5228(10) 0.08330 C9B C 0.6450(13) 0.5720(14) 0.07092(14) C11B C 0.609(6) 0.641(3) 0.0746(3) C9FA C 0.688333(1300) 0.593667(1400) 0.095747(140) C11FA C 0.724333(6000) 0.698667(3000) 0.092067(300) C8B C 0.5526(6) 0.3124(6) -0.00116(8) N3A N 0.6477(4) 0.1745(4) 0.02374(6) C1A C 0.6260(5) 0.0851(6) 0.03345(8) C2A C 0.6838(6) 0.1135(7) 0.04649(9) H1A H 0.73610 0.19040 0.04860 C3A C 0.6647(7) 0.0281(8) 0.05657(10) H2A H 0.70380 0.04800 0.06530 C4A C 0.5873(7) -0.0862(10) 0.05344(13) H3A H 0.57350 -0.14330 0.06010 C5A C 0.5306(7) -0.1156(8) 0.04048(14) H4A H 0.47890 -0.19270 0.03840 C6A C 0.5503(6) -0.0303(6) 0.03049(9) H5A H 0.51220 -0.05100 0.02170 C7A C 0.6240(6) 0.1362(6) 0.00883(8) H6A H 0.54150 0.09850 0.00700 H7A H 0.64920 0.08080 0.00700 C8A C 0.7598(6) 0.4474(6) -0.00116(8) C7B C 0.8638(6) 0.4878(6) 0.00883(8) N3B N 0.8255(4) 0.4732(4) 0.02374(6) C1B C 0.9149(5) 0.5409(6) 0.03345(8) C2B C 0.8865(6) 0.5703(7) 0.04649(9) H1B H 0.80960 0.54570 0.04860 C3B C 0.9719(7) 0.6366(8) 0.05657(10) H2B H 0.95200 0.65580 0.06530 C4B C 1.0862(7) 0.6735(10) 0.05344(13) H3B H 1.14330 0.71680 0.06010 C5B C 1.1156(7) 0.6462(8) 0.04048(14) H4B H 1.19270 0.67160 0.03840 C6B C 1.0303(6) 0.5806(6) 0.03049(9) H5B H 1.05100 0.56320 0.02170 H6B H 0.90150 0.44300 0.00700 H7B H 0.91920 0.56840 0.00700 H8A H 0.73280 0.50260 -0.00090 H9A H 0.78220 0.44280 -0.01090 H8B H 0.49740 0.23020 -0.00090 H9B H 0.55720 0.33940 -0.01090 O1A O 0.0112(4) 0.1504(4) 0.01494(5) C12A C -0.0694(6) 0.1912(6) 0.01408(8) H10A H -0.14760 0.12780 0.01550 H11A H -0.06480 0.22540 0.00470 C13A C -0.0390(7) 0.2772(8) 0.02534(11) H12A H 0.00570 0.35450 0.02140 H13A H -0.10800 0.26960 0.02980 C14A C 0.0268(8) 0.2564(9) 0.03541(10) H14A H -0.02210 0.20650 0.04310 H15A H 0.08590 0.32830 0.03960 C15A C 0.0801(6) 0.1992(7) 0.02727(9) H16A H 0.15870 0.25510 0.02460 H17A H 0.08160 0.13970 0.03310 O1B O -0.1504(4) -0.1392(4) 0.01494(5) C12B C -0.1912(6) -0.2606(6) 0.01408(8) H10B H -0.12780 -0.27540 0.01550 H11B H -0.22540 -0.29020 0.00470 C13B C -0.2772(7) -0.3162(8) 0.02534(11) H12B H -0.35450 -0.34880 0.02140 H13B H -0.26960 -0.37760 0.02980 C14B C -0.2564(8) -0.2296(9) 0.03541(10) H14B H -0.20650 -0.22860 0.04310 H15B H -0.32830 -0.24240 0.03960 C15B C -0.1992(6) -0.1191(7) 0.02727(9) H16B H -0.25510 -0.09640 0.02460 H17B H -0.13970 -0.05810 0.03310 O1R O -0.1392(4) 0.0112(4) -0.01494(5) C12R C -0.2606(6) -0.0694(6) -0.01408(8) H10R H -0.27540 -0.14760 -0.01550 H11R H -0.29020 -0.06480 -0.00470 C13R C -0.3162(7) -0.0390(8) -0.02534(11) H12R H -0.34880 0.00570 -0.02140 H13R H -0.37760 -0.10800 -0.02980 C14R C -0.2296(8) 0.0268(9) -0.03541(10) H14R H -0.22860 -0.02210 -0.04310 H15R H -0.24240 0.08590 -0.03960 C15R C -0.1191(6) 0.0801(7) -0.02727(9) H16R H -0.09640 0.15870 -0.02460 H17R H -0.05810 0.08160 -0.03310 O1S O -0.0112(4) -0.1504(4) -0.01494(5) C12S C 0.0694(6) -0.1912(6) -0.01408(8) H10S H 0.14760 -0.12780 -0.01550 H11S H 0.06480 -0.22540 -0.00470 C13S C 0.0390(7) -0.2772(8) -0.02534(11) H12S H -0.00570 -0.35450 -0.02140 H13S H 0.10800 -0.26960 -0.02980 C14S C -0.0268(8) -0.2564(9) -0.03541(10) H14S H 0.02210 -0.20650 -0.04310 H15S H -0.08590 -0.32830 -0.03960 C15S C -0.0801(6) -0.1992(7) -0.02727(9) H16S H -0.15870 -0.25510 -0.02460 H17S H -0.08160 -0.13970 -0.03310 O1T O 0.1504(4) 0.1392(4) -0.01494(5) C12T C 0.1912(6) 0.2606(6) -0.01408(8) H10T H 0.12780 0.27540 -0.01550 H11T H 0.22540 0.29020 -0.00470 C13T C 0.2772(7) 0.3162(8) -0.02534(11) H12T H 0.35450 0.34880 -0.02140 H13T H 0.26960 0.37760 -0.02980 C14T C 0.2564(8) 0.2296(9) -0.03541(10) H14T H 0.20650 0.22860 -0.04310 H15T H 0.32830 0.24240 -0.03960 C15T C 0.1992(6) 0.1191(7) -0.02727(9) H16T H 0.25510 0.09640 -0.02460 H17T H 0.13970 0.05810 -0.03310 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mo1 N1 1.862 1_555 1_555 Na1 N2 2.157 1_555 1_555 Na2 O1 2.386 1_555 1_555 N1 N2 1.195 1_555 1_555 N3 Mo1 2.035 1_555 1_555 N4 Mo1 2.210 1_555 1_555 O1 C12 1.432 1_555 1_555 O2 Na1 2.532 1_555 1_555 C1 N3 1.407 1_555 1_555 C2 C1 1.385 1_555 1_555 H1 C2 0.930 1_555 1_555 C3 C2 1.398 1_555 1_555 H2 C3 0.930 1_555 1_555 C4 C3 1.381 1_555 1_555 H3 C4 0.927 1_555 1_555 C5 C4 1.373 1_555 1_555 H4 C5 0.930 1_555 1_555 C6 C1 1.385 1_555 1_555 H5 C6 0.929 1_555 1_555 C7 N3 1.457 1_555 1_555 H6 C7 0.971 1_555 1_555 H7 C7 0.970 1_555 1_555 C8 N4 1.470 1_555 1_555 H8 C8 0.970 1_555 1_555 H9 C8 0.966 1_555 1_555 C9 O2 1.426 1_555 1_555 C11 C9 1.282 1_555 1_555 C12 H10 0.971 1_555 1_555 H11 C12 0.973 1_555 1_555 C13 C12 1.455 1_555 1_555 H12 C13 0.970 1_555 1_555 H13 C13 0.969 1_555 1_555 C14 C13 1.404 1_555 1_555 H14 C14 0.973 1_555 1_555 H15 C14 0.970 1_555 1_555 C15 O1 1.410 1_555 1_555 H16 C15 0.969 1_555 1_555 H17 C15 0.971 1_555 1_555 N2I Na1 2.163 1_555 1_555 N1I N2I 1.195 1_555 1_555 Mo1I N1I 1.862 1_555 1_555 N3I Mo1I 2.035 1_555 1_555 C1I N3I 1.407 1_555 1_555 C2I C1I 1.385 1_555 1_555 H1I C2I 0.930 1_555 1_555 C3I C2I 1.398 1_555 1_555 H2I C3I 0.930 1_555 1_555 C4I C3I 1.381 1_555 1_555 H3I C4I 0.927 1_555 1_555 C5I C4I 1.373 1_555 1_555 H4I C5I 0.930 1_555 1_555 C6I C1I 1.385 1_555 1_555 H5I C6I 0.929 1_555 1_555 C7I N3I 1.457 1_555 1_555 H6I C7I 0.971 1_555 1_555 H7I C7I 0.970 1_555 1_555 C8GA C7I 1.529 1_555 1_555 N4GA Mo1I 2.210 1_555 1_555 N3FA Mo1I 2.034 1_555 1_555 C1FA N3FA 1.407 1_555 1_555 C2FA C1FA 1.385 1_555 1_555 H1FA C2FA 0.930 1_555 1_555 C3FA C2FA 1.398 1_555 1_555 H2FA C3FA 0.930 1_555 1_555 C4FA C3FA 1.381 1_555 1_555 H3FA C4FA 0.927 1_555 1_555 C5FA C4FA 1.373 1_555 1_555 H4FA C5FA 0.930 1_555 1_555 C6FA C1FA 1.385 1_555 1_555 H5FA C6FA 0.929 1_555 1_555 C7FA N3FA 1.457 1_555 1_555 H6FA C7FA 0.971 1_555 1_555 H7FA C7FA 0.970 1_555 1_555 C8I N4GA 1.471 1_555 1_555 C8FA N4GA 1.471 1_555 1_555 C7GA C8FA 1.529 1_555 1_555 N3GA Mo1I 2.034 1_555 1_555 C1GA N3GA 1.407 1_555 1_555 C2GA C1GA 1.385 1_555 1_555 H1GA C2GA 0.930 1_555 1_555 C3GA C2GA 1.398 1_555 1_555 H2GA C3GA 0.930 1_555 1_555 C4GA C3GA 1.381 1_555 1_555 H3GA C4GA 0.927 1_555 1_555 C5GA C4GA 1.373 1_555 1_555 H4GA C5GA 0.930 1_555 1_555 C6GA C1GA 1.385 1_555 1_555 H5GA C6GA 0.929 1_555 1_555 H6GA C7GA 0.971 1_555 1_555 H7GA C7GA 0.970 1_555 1_555 H8FA C8FA 0.970 1_555 1_555 H9FA C8FA 0.966 1_555 1_555 H8I C8I 0.970 1_555 1_555 H9I C8I 0.966 1_555 1_555 H8GA C8GA 0.970 1_555 1_555 H9GA C8GA 0.966 1_555 1_555 C9I O2 1.431 1_555 1_555 C11I C11 2.103 1_555 1_555 O2A Na1 2.532 1_555 1_555 C9A O2A 1.426 1_555 1_555 C11A C9A 1.282 1_555 1_555 C9GA O2A 1.431 1_555 1_555 C11GA C11A 2.103 1_555 1_555 O2B Na1 2.533 1_555 1_555 C9B O2B 1.426 1_555 1_555 C11B C9B 1.282 1_555 1_555 C9FA O2B 1.431 1_555 1_555 C11FA C11B 2.103 1_555 1_555 C8B N4 1.471 1_555 1_555 N3A Mo1 2.034 1_555 1_555 C1A N3A 1.407 1_555 1_555 C2A C1A 1.385 1_555 1_555 H1A C2A 0.930 1_555 1_555 C3A C2A 1.398 1_555 1_555 H2A C3A 0.930 1_555 1_555 C4A C3A 1.381 1_555 1_555 H3A C4A 0.927 1_555 1_555 C5A C4A 1.373 1_555 1_555 H4A C5A 0.930 1_555 1_555 C6A C1A 1.385 1_555 1_555 H5A C6A 0.929 1_555 1_555 C7A C8 1.529 1_555 1_555 H6A C7A 0.971 1_555 1_555 H7A C7A 0.970 1_555 1_555 C8A N4 1.471 1_555 1_555 C7B C8A 1.529 1_555 1_555 N3B Mo1 2.034 1_555 1_555 C1B N3B 1.407 1_555 1_555 C2B C1B 1.385 1_555 1_555 H1B C2B 0.930 1_555 1_555 C3B C2B 1.398 1_555 1_555 H2B C3B 0.930 1_555 1_555 C4B C3B 1.381 1_555 1_555 H3B C4B 0.927 1_555 1_555 C5B C4B 1.373 1_555 1_555 H4B C5B 0.930 1_555 1_555 C6B C1B 1.385 1_555 1_555 H5B C6B 0.929 1_555 1_555 H6B C7B 0.971 1_555 1_555 H7B C7B 0.970 1_555 1_555 H8A C8A 0.970 1_555 1_555 H9A C8A 0.966 1_555 1_555 H8B C8B 0.970 1_555 1_555 H9B C8B 0.966 1_555 1_555 O1A Na2 2.386 1_555 1_555 C12A O1A 1.432 1_555 1_555 H10A C12A 0.971 1_555 1_555 H11A C12A 0.973 1_555 1_555 C13A C12A 1.455 1_555 1_555 H12A C13A 0.970 1_555 1_555 H13A C13A 0.969 1_555 1_555 C14A C13A 1.404 1_555 1_555 H14A C14A 0.973 1_555 1_555 H15A C14A 0.970 1_555 1_555 C15A O1A 1.410 1_555 1_555 H16A C15A 0.969 1_555 1_555 H17A C15A 0.971 1_555 1_555 O1B Na2 2.386 1_555 1_555 C12B O1B 1.432 1_555 1_555 H10B C12B 0.971 1_555 1_555 H11B C12B 0.973 1_555 1_555 C13B C12B 1.455 1_555 1_555 H12B C13B 0.970 1_555 1_555 H13B C13B 0.969 1_555 1_555 C14B C13B 1.404 1_555 1_555 H14B C14B 0.973 1_555 1_555 H15B C14B 0.970 1_555 1_555 C15B O1B 1.410 1_555 1_555 H16B C15B 0.969 1_555 1_555 H17B C15B 0.971 1_555 1_555 O1R Na2 2.386 1_555 1_555 C12R O1R 1.432 1_555 1_555 H10R C12R 0.971 1_555 1_555 H11R C12R 0.973 1_555 1_555 C13R C12R 1.455 1_555 1_555 H12R C13R 0.970 1_555 1_555 H13R C13R 0.969 1_555 1_555 C14R C13R 1.404 1_555 1_555 H14R C14R 0.973 1_555 1_555 H15R C14R 0.970 1_555 1_555 C15R O1R 1.410 1_555 1_555 H16R C15R 0.969 1_555 1_555 H17R C15R 0.971 1_555 1_555 O1S Na2 2.386 1_555 1_555 C12S O1S 1.432 1_555 1_555 H10S C12S 0.971 1_555 1_555 H11S C12S 0.973 1_555 1_555 C13S C12S 1.455 1_555 1_555 H12S C13S 0.970 1_555 1_555 H13S C13S 0.969 1_555 1_555 C14S C13S 1.404 1_555 1_555 H14S C14S 0.973 1_555 1_555 H15S C14S 0.970 1_555 1_555 C15S O1S 1.410 1_555 1_555 H16S C15S 0.969 1_555 1_555 H17S C15S 0.971 1_555 1_555 O1T Na2 2.386 1_555 1_555 C12T O1T 1.432 1_555 1_555 H10T C12T 0.971 1_555 1_555 H11T C12T 0.973 1_555 1_555 C13T C12T 1.455 1_555 1_555 H12T C13T 0.970 1_555 1_555 H13T C13T 0.969 1_555 1_555 C14T C13T 1.404 1_555 1_555 H14T C14T 0.973 1_555 1_555 H15T C14T 0.970 1_555 1_555 C15T O1T 1.410 1_555 1_555 H16T C15T 0.969 1_555 1_555 H17T C15T 0.971 1_555 1_555 C5 C6 1.390 1_555 1_555 C7 C8B 1.529 1_555 1_555 C14 C15 1.487 1_555 1_555 C5I C6I 1.390 1_555 1_555 C8GA N4GA 1.470 1_555 1_555 C5FA C6FA 1.390 1_555 1_555 C7FA C8I 1.529 1_555 1_555 C7GA N3GA 1.457 1_555 1_555 C5GA C6GA 1.390 1_555 1_555 C9I C11I 1.282 1_555 1_555 C9GA C11GA 1.282 1_555 1_555 C9FA C11FA 1.282 1_555 1_555 N3A C7A 1.457 1_555 1_555 C5A C6A 1.390 1_555 1_555 C7B N3B 1.457 1_555 1_555 C5B C6B 1.390 1_555 1_555 C14A C15A 1.487 1_555 1_555 C14B C15B 1.487 1_555 1_555 C14R C15R 1.487 1_555 1_555 C14S C15S 1.487 1_555 1_555 C14T C15T 1.487 1_555 1_555 #END data_CSD_CIF_ICUNID _audit_creation_date 2002-02-07 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD ICUNID _database_code_depnum_ccdc_archive 'CCDC 162001' _chemical_formula_sum 'C54 H102 Li2 N4 Si6' _chemical_formula_moiety ; C12 H32 Li1 N4 1+,C30 H58 Li1 Si6 1-,2(C6 H6) ; _journal_coden_Cambridge 36 _journal_volume 631 _journal_year 2001 _journal_page_first 76 _journal_name_full 'J.Organomet.Chem. ' loop_ _publ_author_name "S.S.Al-Juaid" "A.G.Avent" "C.Eaborn" "S.M.El-Hamruni" "S.A.Hawkes" "M.S.Hill" "M.Hopman" "P.B.Hitchcock" "J.D.Smith" _chemical_name_systematic ; bis(1,2-bis(Dimethylamino)ethane-N,N')-lithium bis(bis(trimethylsilyl)(dimethyl(phenyl)silyl)methyl)-lithium benzene solvate ; _cell_volume 6445.809 _exptl_crystal_density_diffrn 1.02 _diffrn_ambient_temperature 173 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.095 _refine_ls_wR_factor_gt 0.095 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x,-y,1/2+z 3 1/2+x,1/2+y,z 4 1/2+x,1/2-y,1/2+z 5 -x,-y,-z 6 -x,y,-1/2-z 7 -1/2-x,-1/2-y,-z 8 -1/2-x,-1/2+y,-1/2-z _cell_length_a 15.188(7) _cell_length_b 19.117(9) _cell_length_c 22.205(9) _cell_angle_alpha 90 _cell_angle_beta 91.19(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.18 N 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.50000 0.00000 0.50000 Li2 Li 0.50000 0.3543(8) 0.25000 Si1 Si 0.49846(12) 0.16084(9) 0.48086(8) Si2 Si 0.34459(13) 0.09657(10) 0.55267(9) Si3 Si 0.53042(14) 0.10565(10) 0.60915(8) N1 N 0.5210(4) 0.4115(3) 0.3311(2) N2 N 0.6174(4) 0.2977(3) 0.2703(3) C1 C 0.4633(4) 0.1005(3) 0.5397(3) C2 C 0.5960(4) 0.1265(4) 0.4395(3) H1 H 0.6128(4) 0.1602(4) 0.4085(3) H2 H 0.5807(4) 0.0817(4) 0.4205(3) H3 H 0.6455(4) 0.1197(4) 0.4679(3) C3 C 0.4138(4) 0.1778(3) 0.4198(3) H4 H 0.4379(4) 0.2104(3) 0.3903(3) H5 H 0.3611(4) 0.1982(3) 0.4375(3) H6 H 0.3984(4) 0.1337(3) 0.3998(3) C4 C 0.5308(4) 0.2528(3) 0.5058(3) C5 C 0.6159(5) 0.2789(4) 0.5014(3) H7 H 0.6607(5) 0.2494(4) 0.4863(3) C6 C 0.6380(5) 0.3485(4) 0.5189(4) H8 H 0.6966(5) 0.3649(4) 0.5150(4) C7 C 0.5750(5) 0.3916(4) 0.5412(3) H9 H 0.5894(5) 0.4377(4) 0.5538(3) C8 C 0.4913(6) 0.3673(4) 0.5450(3) H10 H 0.4467(6) 0.3973(4) 0.5598(3) C9 C 0.4694(5) 0.2989(4) 0.5277(3) H11 H 0.4101(5) 0.2837(4) 0.5311(3) C10 C 0.2861(5) 0.1827(4) 0.5644(4) H12 H 0.2234(5) 0.1740(4) 0.5709(4) H13 H 0.2928(5) 0.2122(4) 0.5288(4) H14 H 0.3118(5) 0.2064(4) 0.5997(4) C11 C 0.3140(5) 0.0470(4) 0.6216(4) H15 H 0.2498(5) 0.0472(4) 0.6254(4) H16 H 0.3413(5) 0.0691(4) 0.6572(4) H17 H 0.3348(5) -0.0014(4) 0.6184(4) C12 C 0.2797(5) 0.0523(4) 0.4897(4) H18 H 0.2170(5) 0.0519(4) 0.4994(4) H19 H 0.3005(5) 0.0041(4) 0.4851(4) H20 H 0.2879(5) 0.0779(4) 0.4520(4) C13 C 0.4951(6) 0.1766(4) 0.6627(3) H21 H 0.5337(6) 0.1762(4) 0.6986(3) H22 H 0.4342(6) 0.1683(4) 0.6745(3) H23 H 0.4990(6) 0.2222(4) 0.6427(3) C14 C 0.5347(5) 0.0226(4) 0.6545(3) H24 H 0.5716(5) 0.0298(4) 0.6907(3) H25 H 0.5595(5) -0.0150(4) 0.6301(3) H26 H 0.4750(5) 0.0098(4) 0.6663(3) C15 C 0.6503(5) 0.1251(4) 0.5972(4) H27 H 0.6814(5) 0.1269(4) 0.6363(4) H28 H 0.6559(5) 0.1702(4) 0.5768(4) H29 H 0.6759(5) 0.0882(4) 0.5724(4) C16 C 0.6109(5) 0.3895(4) 0.3487(3) H30 H 0.6203(5) 0.3979(4) 0.3924(3) H31 H 0.6539(5) 0.4183(4) 0.3269(3) C17 C 0.6267(5) 0.3142(4) 0.3354(3) H32 H 0.6867(5) 0.3014(4) 0.3497(3) H33 H 0.5843(5) 0.2855(4) 0.3580(3) C18 C 0.5173(6) 0.4874(4) 0.3285(4) H34 H 0.5589(6) 0.5045(4) 0.2987(4) H35 H 0.5330(6) 0.5068(4) 0.3682(4) H36 H 0.4575(6) 0.5023(4) 0.3169(4) C19 C 0.4586(5) 0.3873(5) 0.3756(3) H37 H 0.4603(5) 0.3362(5) 0.3779(3) H38 H 0.3991(5) 0.4025(5) 0.3638(3) H39 H 0.4745(5) 0.4071(5) 0.4151(3) C20 C 0.6913(5) 0.3257(5) 0.2369(4) H40 H 0.6929(5) 0.3768(5) 0.2412(4) H41 H 0.6842(5) 0.3135(5) 0.1942(4) H42 H 0.7465(5) 0.3058(5) 0.2529(4) C21 C 0.6167(6) 0.2215(4) 0.2631(4) H43 H 0.5674(6) 0.2017(4) 0.2852(4) H44 H 0.6722(6) 0.2021(4) 0.2789(4) H45 H 0.6099(6) 0.2099(4) 0.2202(4) C22 C 0.6944(5) 0.4069(4) 0.7015(4) H46 H 0.7009(5) 0.4227(4) 0.6613(4) C23 C 0.7437(5) 0.4372(4) 0.7472(4) H47 H 0.7834(5) 0.4741(4) 0.7388(4) C24 C 0.7351(6) 0.4141(4) 0.8040(4) H48 H 0.7698(6) 0.4349(4) 0.8353(4) C25 C 0.6779(7) 0.3614(6) 0.8184(5) H49 H 0.6722(7) 0.3455(6) 0.8587(5) C26 C 0.6280(6) 0.3319(5) 0.7705(6) H50 H 0.5876(6) 0.2954(5) 0.7787(6) C27 C 0.6361(6) 0.3542(4) 0.7134(5) H51 H 0.6019(6) 0.3337(4) 0.6818(5) C1D C 0.5367(4) -0.1005(3) 0.4603(3) Si1D Si 0.50154(12) -0.16084(9) 0.51914(8) C2D C 0.4040(4) -0.1265(4) 0.5605(3) H1D H 0.3872(4) -0.1602(4) 0.5915(3) H2D H 0.4193(4) -0.0817(4) 0.5795(3) H3D H 0.3545(4) -0.1197(4) 0.5321(3) C3D C 0.5862(4) -0.1778(3) 0.5802(3) H4D H 0.5621(4) -0.2104(3) 0.6097(3) H5D H 0.6389(4) -0.1982(3) 0.5625(3) H6D H 0.6016(4) -0.1337(3) 0.6002(3) C4D C 0.4692(4) -0.2528(3) 0.4942(3) C5D C 0.3841(5) -0.2789(4) 0.4986(3) H7D H 0.3393(5) -0.2494(4) 0.5137(3) C6D C 0.3620(5) -0.3485(4) 0.4811(4) H8D H 0.3034(5) -0.3649(4) 0.4850(4) C7D C 0.4250(5) -0.3916(4) 0.4588(3) H9D H 0.4106(5) -0.4377(4) 0.4462(3) C8D C 0.5087(6) -0.3673(4) 0.4550(3) H10D H 0.5533(6) -0.3973(4) 0.4402(3) C9D C 0.5306(5) -0.2989(4) 0.4723(3) H11D H 0.5899(5) -0.2837(4) 0.4689(3) Si2D Si 0.65541(13) -0.09657(10) 0.44733(9) C10D C 0.7139(5) -0.1827(4) 0.4356(4) H12D H 0.7766(5) -0.1740(4) 0.4291(4) H13D H 0.7072(5) -0.2122(4) 0.4712(4) H14D H 0.6882(5) -0.2064(4) 0.4003(4) C11D C 0.6860(5) -0.0470(4) 0.3784(4) H15D H 0.7502(5) -0.0472(4) 0.3746(4) H16D H 0.6587(5) -0.0691(4) 0.3428(4) H17D H 0.6652(5) 0.0014(4) 0.3816(4) C12D C 0.7203(5) -0.0523(4) 0.5103(4) H18D H 0.7830(5) -0.0519(4) 0.5006(4) H19D H 0.6995(5) -0.0041(4) 0.5149(4) H20D H 0.7121(5) -0.0779(4) 0.5480(4) Si3D Si 0.46958(14) -0.10565(10) 0.39085(8) C13D C 0.5049(6) -0.1766(4) 0.3373(3) H21D H 0.4663(6) -0.1762(4) 0.3014(3) H22D H 0.5658(6) -0.1683(4) 0.3255(3) H23D H 0.5010(6) -0.2222(4) 0.3573(3) C14D C 0.4653(5) -0.0226(4) 0.3455(3) H24D H 0.4284(5) -0.0298(4) 0.3093(3) H25D H 0.4405(5) 0.0150(4) 0.3699(3) H26D H 0.5250(5) -0.0098(4) 0.3337(3) C15D C 0.3497(5) -0.1251(4) 0.4028(4) H27D H 0.3186(5) -0.1269(4) 0.3637(4) H28D H 0.3441(5) -0.1702(4) 0.4232(4) H29D H 0.3241(5) -0.0882(4) 0.4276(4) N1E N 0.4790(4) 0.4115(3) 0.1689(2) C16E C 0.3891(5) 0.3895(4) 0.1513(3) H30E H 0.3797(5) 0.3979(4) 0.1076(3) H31E H 0.3461(5) 0.4183(4) 0.1731(3) C17E C 0.3733(5) 0.3142(4) 0.1646(3) N2E N 0.3826(4) 0.2977(3) 0.2297(3) C20E C 0.3087(5) 0.3257(5) 0.2631(4) H40E H 0.3071(5) 0.3768(5) 0.2588(4) H41E H 0.3158(5) 0.3135(5) 0.3058(4) H42E H 0.2535(5) 0.3058(5) 0.2471(4) C21E C 0.3833(6) 0.2215(4) 0.2369(4) H43E H 0.4326(6) 0.2017(4) 0.2148(4) H44E H 0.3278(6) 0.2021(4) 0.2211(4) H45E H 0.3901(6) 0.2099(4) 0.2798(4) H32E H 0.3133(5) 0.3014(4) 0.1503(3) H33E H 0.4157(5) 0.2855(4) 0.1420(3) C18E C 0.4827(6) 0.4874(4) 0.1715(4) H34E H 0.4411(6) 0.5045(4) 0.2013(4) H35E H 0.4670(6) 0.5068(4) 0.1318(4) H36E H 0.5425(6) 0.5023(4) 0.1831(4) C19E C 0.5414(5) 0.3873(5) 0.1244(3) H37E H 0.5397(5) 0.3362(5) 0.1221(3) H38E H 0.6009(5) 0.4025(5) 0.1362(3) H39E H 0.5255(5) 0.4071(5) 0.0849(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 C1 2.191 1_555 1_555 Li2 N1 2.125 1_555 1_555 Si1 C1 1.831 1_555 1_555 Si2 C1 1.833 1_555 1_555 Si3 C1 1.834 1_555 1_555 N1 C16 1.474 1_555 1_555 N2 Li2 2.126 1_555 1_555 C2 Si1 1.878 1_555 1_555 H1 C2 0.980 1_555 1_555 H2 C2 0.981 1_555 1_555 H3 C2 0.980 1_555 1_555 C3 Si1 1.877 1_555 1_555 H4 C3 0.981 1_555 1_555 H5 C3 0.980 1_555 1_555 H6 C3 0.979 1_555 1_555 C4 Si1 1.905 1_555 1_555 C5 C4 1.391 1_555 1_555 H7 C5 0.950 1_555 1_555 C6 C5 1.424 1_555 1_555 H8 C6 0.949 1_555 1_555 C7 C6 1.364 1_555 1_555 H9 C7 0.949 1_555 1_555 C8 C7 1.358 1_555 1_555 H10 C8 0.951 1_555 1_555 C9 C4 1.379 1_555 1_555 H11 C9 0.951 1_555 1_555 C10 Si2 1.891 1_555 1_555 H12 C10 0.980 1_555 1_555 H13 C10 0.978 1_555 1_555 H14 C10 0.979 1_555 1_555 C11 Si2 1.867 1_555 1_555 H15 C11 0.980 1_555 1_555 H16 C11 0.981 1_555 1_555 H17 C11 0.981 1_555 1_555 C12 Si2 1.894 1_555 1_555 H18 C12 0.981 1_555 1_555 H19 C12 0.980 1_555 1_555 H20 C12 0.980 1_555 1_555 C13 Si3 1.889 1_555 1_555 H21 C13 0.980 1_555 1_555 H22 C13 0.980 1_555 1_555 H23 C13 0.981 1_555 1_555 C14 Si3 1.880 1_555 1_555 H24 C14 0.980 1_555 1_555 H25 C14 0.980 1_555 1_555 H26 C14 0.980 1_555 1_555 C15 Si3 1.883 1_555 1_555 H27 C15 0.980 1_555 1_555 H28 C15 0.978 1_555 1_555 H29 C15 0.980 1_555 1_555 C16 H30 0.991 1_555 1_555 H31 C16 0.988 1_555 1_555 C17 N2 1.483 1_555 1_555 H32 C17 0.990 1_555 1_555 H33 C17 0.990 1_555 1_555 C18 N1 1.453 1_555 1_555 H34 C18 0.980 1_555 1_555 H35 C18 0.981 1_555 1_555 H36 C18 0.981 1_555 1_555 C19 N1 1.459 1_555 1_555 H37 C19 0.979 1_555 1_555 H38 C19 0.980 1_555 1_555 H39 C19 0.981 1_555 1_555 C20 N2 1.460 1_555 1_555 H40 C20 0.982 1_555 1_555 H41 C20 0.980 1_555 1_555 H42 C20 0.981 1_555 1_555 C21 N2 1.465 1_555 1_555 H43 C21 0.980 1_555 1_555 H44 C21 0.979 1_555 1_555 H45 C21 0.981 1_555 1_555 C22 H46 0.949 1_555 1_555 C23 C22 1.376 1_555 1_555 H47 C23 0.949 1_555 1_555 C24 C23 1.345 1_555 1_555 H48 C24 0.951 1_555 1_555 C25 C24 1.372 1_555 1_555 H49 C25 0.951 1_555 1_555 C26 C25 1.411 1_555 1_555 H50 C26 0.949 1_555 1_555 C27 C22 1.371 1_555 1_555 H51 C27 0.949 1_555 1_555 C1D Li1 2.191 1_555 1_555 Si1D C1D 1.831 1_555 1_555 C2D Si1D 1.878 1_555 1_555 H1D C2D 0.980 1_555 1_555 H2D C2D 0.981 1_555 1_555 H3D C2D 0.980 1_555 1_555 C3D Si1D 1.877 1_555 1_555 H4D C3D 0.981 1_555 1_555 H5D C3D 0.980 1_555 1_555 H6D C3D 0.979 1_555 1_555 C4D Si1D 1.905 1_555 1_555 C5D C4D 1.391 1_555 1_555 H7D C5D 0.950 1_555 1_555 C6D C5D 1.424 1_555 1_555 H8D C6D 0.949 1_555 1_555 C7D C6D 1.364 1_555 1_555 H9D C7D 0.949 1_555 1_555 C8D C7D 1.358 1_555 1_555 H10D C8D 0.951 1_555 1_555 C9D C4D 1.379 1_555 1_555 H11D C9D 0.951 1_555 1_555 Si2D C1D 1.833 1_555 1_555 C10D Si2D 1.891 1_555 1_555 H12D C10D 0.980 1_555 1_555 H13D C10D 0.978 1_555 1_555 H14D C10D 0.979 1_555 1_555 C11D Si2D 1.867 1_555 1_555 H15D C11D 0.980 1_555 1_555 H16D C11D 0.981 1_555 1_555 H17D C11D 0.981 1_555 1_555 C12D Si2D 1.894 1_555 1_555 H18D C12D 0.981 1_555 1_555 H19D C12D 0.980 1_555 1_555 H20D C12D 0.980 1_555 1_555 Si3D C1D 1.834 1_555 1_555 C13D Si3D 1.889 1_555 1_555 H21D C13D 0.980 1_555 1_555 H22D C13D 0.980 1_555 1_555 H23D C13D 0.981 1_555 1_555 C14D Si3D 1.880 1_555 1_555 H24D C14D 0.980 1_555 1_555 H25D C14D 0.980 1_555 1_555 H26D C14D 0.980 1_555 1_555 C15D Si3D 1.883 1_555 1_555 H27D C15D 0.980 1_555 1_555 H28D C15D 0.978 1_555 1_555 H29D C15D 0.980 1_555 1_555 N1E Li2 2.125 1_555 1_555 C16E N1E 1.474 1_555 1_555 H30E C16E 0.991 1_555 1_555 H31E C16E 0.988 1_555 1_555 C17E C16E 1.490 1_555 1_555 N2E Li2 2.126 1_555 1_555 C20E N2E 1.460 1_555 1_555 H40E C20E 0.982 1_555 1_555 H41E C20E 0.980 1_555 1_555 H42E C20E 0.981 1_555 1_555 C21E N2E 1.465 1_555 1_555 H43E C21E 0.980 1_555 1_555 H44E C21E 0.979 1_555 1_555 H45E C21E 0.981 1_555 1_555 H32E C17E 0.990 1_555 1_555 H33E C17E 0.990 1_555 1_555 C18E N1E 1.453 1_555 1_555 H34E C18E 0.980 1_555 1_555 H35E C18E 0.981 1_555 1_555 H36E C18E 0.981 1_555 1_555 C19E N1E 1.459 1_555 1_555 H37E C19E 0.979 1_555 1_555 H38E C19E 0.980 1_555 1_555 H39E C19E 0.981 1_555 1_555 C8 C9 1.401 1_555 1_555 C16 C17 1.490 1_555 1_555 C26 C27 1.346 1_555 1_555 C8D C9D 1.401 1_555 1_555 C17E N2E 1.483 1_555 1_555 #END data_CSD_CIF_IVAKEX _audit_creation_date 2016-09-13 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD IVAKEX _database_code_depnum_ccdc_archive 'CCDC 1451853' _chemical_formula_sum 'C84 H128 N4 Na2 O16 Re2' _chemical_formula_moiety ; C60 H80 N4 Na1 O10 Re2 1-,C24 H48 Na1 O6 1+ ; _journal_coden_Cambridge 1220 _journal_volume 22 _journal_year 2016 _journal_page_first 10638 _journal_name_full 'Chem.-Eur.J. ' loop_ _publ_author_name "D.Sieh" "C.P.Kubiak" _chemical_name_systematic ; hexakis(tetrahydrofuran)-sodium bis(\m-carbonyl)-bis(N-(2,6-diisopropylphenyl)-1-(pyridin-2-yl)ethanimine)-tet racarbonyl-tetrakis(tetrahydrofuran)-di-rhenium-sodium ; _cell_volume 2157.675 _exptl_crystal_colour 'red' _exptl_crystal_density_diffrn 1.438 _exptl_crystal_description 'plate' _diffrn_ambient_temperature 100 _refine_special_details ; C35B,C38B,O7B and C35A,C38A,O7A disordered over two sites with occupancies 0.504:0.496; C40B,C41B,C42B and C40A,C41A,C42A disordered over two sites with occupancies 0.643:0.357. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_gt 0.0414 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 9.6231(6) _cell_length_b 10.7182(6) _cell_length_c 21.4843(14) _cell_angle_alpha 95.258(2) _cell_angle_beta 102.018(2) _cell_angle_gamma 90.197(2) _cell_formula_units_Z 1 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 N 0.68 Na 1.66 O 0.68 Re 1.51 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Re1 Re 0.371162(8) 0.732499(7) 0.212440(4) N1 N 0.23903(16) 0.86968(14) 0.23490(7) N2 N 0.17976(18) 0.63918(15) 0.21278(8) Na1 Na 0.50000 0.50000 0.00000 O1 O 0.62300(17) 0.91676(16) 0.2197(1) O2 O 0.57310(18) 0.54075(16) 0.27854(9) O3 O 0.41435(19) 0.60583(17) 0.08480(8) C1 C -0.0015(2) 0.9392(2) 0.25161(11) H1 H -0.01100 0.99910 0.21920 H2 H 0.03450 0.98310 0.29400 H3 H -0.09460 0.90050 0.25040 C2 C 0.10002(19) 0.83983(17) 0.23815(9) C3 C 0.0666(2) 0.71334(18) 0.22563(9) C4 C -0.0688(2) 0.6551(2) 0.22318(10) H4 H -0.14520 0.70510 0.23180 C5 C -0.0896(3) 0.5294(2) 0.20874(13) H5 H -0.17990 0.49150 0.20690 C6 C 0.0261(3) 0.4553(2) 0.19644(13) H6 H 0.01420 0.36720 0.18660 C7 C 0.1535(2) 0.51234(19) 0.19893(11) H7 H 0.22930 0.46140 0.19060 C8 C 0.28026(19) 1.00037(16) 0.24574(9) C9 C 0.2593(2) 1.07350(17) 0.19340(9) C10 C 0.3079(2) 1.19761(19) 0.20419(11) H8 H 0.29560 1.24790 0.16930 C11 C 0.3740(3) 1.2496(2) 0.26463(12) H9 H 0.40830 1.33400 0.27090 C12 C 0.3896(3) 1.1774(2) 0.31574(11) H10 H 0.43290 1.21370 0.35730 C13 C 0.3429(2) 1.05235(18) 0.30753(10) C14 C 0.1863(2) 1.02093(18) 0.12672(9) H11 H 0.14680 0.93580 0.12970 C15 C 0.2910(3) 1.0064(2) 0.08205(10) H12 H 0.32770 1.08920 0.07660 H13 H 0.24230 0.96600 0.04040 H14 H 0.37000 0.95460 0.10050 C16 C 0.0621(2) 1.1025(2) 0.09868(11) H15 H -0.00300 1.11310 0.12820 H16 H 0.01110 1.06180 0.05750 H17 H 0.09890 1.18480 0.09240 C17 C 0.3615(3) 0.9758(2) 0.36466(10) H18 H 0.31790 0.89080 0.34910 C18 C 0.5156(3) 0.9586(4) 0.39381(15) H19 H 0.56310 0.91840 0.36130 H20 H 0.52310 0.90570 0.42920 H21 H 0.56110 1.04050 0.40990 C19 C 0.2840(3) 1.0336(3) 0.41565(13) H22 H 0.29090 0.97800 0.44990 H23 H 0.18380 1.04450 0.39620 H24 H 0.32790 1.11530 0.43350 C20 C 0.5293(2) 0.84670(19) 0.21691(11) C21 C 0.4975(2) 0.61399(19) 0.2529(1) C22 C 0.4000(2) 0.65434(19) 0.13419(10) O4 O 0.69891(17) 0.63880(15) 0.01410(8) C23 C 0.7136(2) 0.7373(2) 0.06505(12) H25 H 0.70840 0.70300 0.10580 H26 H 0.63780 0.79920 0.05560 C24 C 0.8583(3) 0.7971(2) 0.06906(12) H27 H 0.89850 0.83530 0.11290 H28 H 0.85320 0.86200 0.03880 C25 C 0.9459(2) 0.6865(3) 0.05070(12) H29 H 1.01120 0.71180 0.02380 H30 H 1.00220 0.65270 0.08920 C26 C 0.8371(3) 0.5915(3) 0.0139(2) H31 H 0.85030 0.57560 -0.03060 H32 H 0.84830 0.51160 0.03390 O5 O 0.62869(17) 0.36382(15) 0.07044(8) C27 C 0.7129(3) 0.2628(2) 0.05076(13) H33 H 0.81520 0.28040 0.06860 H34 H 0.69770 0.25080 0.00360 C28 C 0.6632(3) 0.1473(2) 0.07675(12) H35 H 0.73870 0.08460 0.08370 H36 H 0.57730 0.10810 0.04790 C29 C 0.6309(3) 0.2038(2) 0.13952(12) H37 H 0.56410 0.14960 0.15490 H38 H 0.71880 0.21830 0.17290 C30 C 0.5635(3) 0.3265(2) 0.12084(11) H39 H 0.45960 0.31480 0.10550 H40 H 0.58180 0.39090 0.15780 Na2 Na 0.00000 0.50000 0.50000 O6 O 0.1935(2) 0.54802(19) 0.45162(10) C31 C 0.2078(4) 0.6438(3) 0.41102(19) H41 H 0.19210 0.72740 0.43180 H42 H 0.13820 0.62960 0.36990 C32 C 0.3570(5) 0.6352(3) 0.4004(2) H43 H 0.36660 0.67170 0.36080 H44 H 0.42630 0.67690 0.43710 C33 C 0.3735(6) 0.5002(4) 0.3950(3) H45 H 0.47510 0.47810 0.40290 H46 H 0.32530 0.46170 0.35230 C34 C 0.3027(4) 0.4595(4) 0.4467(3) H47 H 0.26140 0.37380 0.43490 H48 H 0.37220 0.46060 0.48780 O7 O 0.1188(6) 0.3099(5) 0.5316(3) C35 C 0.0455(6) 0.1920(5) 0.5173(2) H49 H 0.06180 0.15010 0.47650 H50 H -0.05790 0.20280 0.51370 C36 C 0.2212(8) 0.3095(6) 0.5905(4) H51 H 0.23140 0.39330 0.61480 H52 H 0.31520 0.28310 0.58290 C37 C 0.1019(3) 0.1197(3) 0.56910(19) H53 H 0.18100 0.06840 0.55900 H54 H 0.02720 0.06290 0.57690 C38 C 0.1540(4) 0.2096(4) 0.62700(14) H55 H 0.22600 0.17280 0.65970 H56 H 0.07570 0.24420 0.64630 O8 O -0.1040(2) 0.37216(19) 0.40519(9) C39 C -0.2311(4) 0.2979(4) 0.38984(19) H57 H -0.31430 0.35180 0.37890 H58 H -0.24170 0.25290 0.42690 C40 C -0.2227(11) 0.205(1) 0.3334(5) H59 H -0.30940 0.20640 0.29930 H60 H -0.20960 0.11890 0.34640 C41 C -0.0912(9) 0.2521(6) 0.3110(4) H61 H -0.02950 0.18100 0.30340 H62 H -0.12110 0.29150 0.27060 C42 C -0.0213(5) 0.3343(6) 0.3558(2) H63 H 0.00190 0.40950 0.33610 H64 H 0.06920 0.29790 0.37640 O9? O 0.1099(6) 0.3334(5) 0.5454(3) C43? C 0.1178(14) 0.2073(7) 0.5167(2) H65? H 0.21020 0.19470 0.50390 H66? H 0.04050 0.19010 0.47840 C44? C 0.1871(12) 0.3311(6) 0.6096(4) H67? H 0.15620 0.39850 0.63810 H68? H 0.29050 0.34140 0.61220 H69? H 0.00190 0.09250 0.56560 H70? H 0.16250 0.04540 0.56820 H71? H 0.08010 0.21790 0.65300 H72? H 0.24000 0.17620 0.65350 H73? H -0.31280 0.34650 0.36960 H74? H -0.25260 0.26440 0.42830 C45? C -0.1954(10) 0.1904(7) 0.3418(4) H75? H -0.12290 0.13370 0.36280 H76? H -0.28100 0.14120 0.31890 C46? C -0.1402(10) 0.2691(8) 0.3007(4) H77? H -0.21610 0.28710 0.26410 H78? H -0.06220 0.22690 0.28410 C47? C -0.0837(11) 0.3936(8) 0.3428(4) H79? H 0.01800 0.40900 0.34330 H80? H -0.13870 0.46620 0.32670 Re1A Re 0.628838(8) 0.267501(7) -0.212440(4) N1A N 0.76097(16) 0.13032(14) -0.23490(7) N2A N 0.82024(18) 0.36082(15) -0.21278(8) O1A O 0.37700(17) 0.08324(16) -0.2197(1) O2A O 0.42690(18) 0.45925(16) -0.27854(9) O3A O 0.58565(19) 0.39417(17) -0.08480(8) C1A C 1.0015(2) 0.0608(2) -0.25161(11) H1A H 1.01100 0.00090 -0.21920 H2A H 0.96550 0.01690 -0.29400 H3A H 1.09460 0.09950 -0.25040 C2A C 0.89998(19) 0.16017(17) -0.23815(9) C3A C 0.9334(2) 0.28666(18) -0.22563(9) C4A C 1.0688(2) 0.3449(2) -0.22318(10) H4A H 1.14520 0.29490 -0.23180 C5A C 1.0896(3) 0.4706(2) -0.20874(13) H5A H 1.17990 0.50850 -0.20690 C6A C 0.9739(3) 0.5447(2) -0.19644(13) H6A H 0.98580 0.63280 -0.18660 C7A C 0.8465(2) 0.48766(19) -0.19893(11) H7A H 0.77070 0.53860 -0.19060 C8A C 0.71974(19) -0.00037(16) -0.24574(9) C9A C 0.7407(2) -0.07350(17) -0.19340(9) C10A C 0.6921(2) -0.19761(19) -0.20419(11) H8A H 0.70440 -0.24790 -0.16930 C11A C 0.6260(3) -0.2496(2) -0.26463(12) H9A H 0.59170 -0.33400 -0.27090 C12A C 0.6104(3) -0.1774(2) -0.31574(11) H10A H 0.56710 -0.21370 -0.35730 C13A C 0.6571(2) -0.05235(18) -0.30753(10) C14A C 0.8137(2) -0.02093(18) -0.12672(9) H11A H 0.85320 0.06420 -0.12970 C15A C 0.7090(3) -0.0064(2) -0.08205(10) H12A H 0.67230 -0.08920 -0.07660 H13A H 0.75770 0.03400 -0.04040 H14A H 0.63000 0.04540 -0.10050 C16A C 0.9379(2) -0.1025(2) -0.09868(11) H15A H 1.00300 -0.11310 -0.12820 H16A H 0.98890 -0.06180 -0.05750 H17A H 0.90110 -0.18480 -0.09240 C17A C 0.6385(3) 0.0242(2) -0.36466(10) H18A H 0.68210 0.10920 -0.34910 C18A C 0.4844(3) 0.0414(4) -0.39381(15) H19A H 0.43690 0.08160 -0.36130 H20A H 0.47690 0.09430 -0.42920 H21A H 0.43890 -0.04050 -0.40990 C19A C 0.7160(3) -0.0336(3) -0.41565(13) H22A H 0.70910 0.02200 -0.44990 H23A H 0.81620 -0.04450 -0.39620 H24A H 0.67210 -0.11530 -0.43350 C20A C 0.4707(2) 0.15330(19) -0.21691(11) C21A C 0.5025(2) 0.38601(19) -0.2529(1) C22A C 0.6000(2) 0.34566(19) -0.13419(10) O4A O 0.30109(17) 0.36120(15) -0.01410(8) C23A C 0.2864(2) 0.2627(2) -0.06505(12) H25A H 0.29160 0.29700 -0.10580 H26A H 0.36220 0.20080 -0.05560 C24A C 0.1417(3) 0.2029(2) -0.06906(12) H27A H 0.10150 0.16470 -0.11290 H28A H 0.14680 0.13800 -0.03880 C25A C 0.0541(2) 0.3135(3) -0.05070(12) H29A H -0.01120 0.28820 -0.02380 H30A H -0.00220 0.34730 -0.08920 C26A C 0.1629(3) 0.4085(3) -0.0139(2) H31A H 0.14970 0.42440 0.03060 H32A H 0.15170 0.48840 -0.03390 O5A O 0.37131(17) 0.63618(15) -0.07044(8) C27A C 0.2871(3) 0.7372(2) -0.05076(13) H33A H 0.18480 0.71960 -0.06860 H34A H 0.30230 0.74920 -0.00360 C28A C 0.3368(3) 0.8527(2) -0.07675(12) H35A H 0.26130 0.91540 -0.08370 H36A H 0.42270 0.89190 -0.04790 C29A C 0.3691(3) 0.7962(2) -0.13952(12) H37A H 0.43590 0.85040 -0.15490 H38A H 0.28120 0.78170 -0.17290 C30A C 0.4365(3) 0.6735(2) -0.12084(11) H39A H 0.54040 0.68520 -0.10550 H40A H 0.41820 0.60910 -0.15780 O6A O -0.1935(2) 0.45198(19) 0.54838(10) C31A C -0.2078(4) 0.3562(3) 0.58898(19) H41A H -0.19210 0.27260 0.56820 H42A H -0.13820 0.37040 0.63010 C32A C -0.3570(5) 0.3648(3) 0.5996(2) H43A H -0.36660 0.32830 0.63920 H44A H -0.42630 0.32310 0.56290 C33A C -0.3735(6) 0.4998(4) 0.6050(3) H45A H -0.47510 0.52190 0.59710 H46A H -0.32530 0.53830 0.64770 C34A C -0.3027(4) 0.5405(4) 0.5533(3) H47A H -0.26140 0.62620 0.56510 H48A H -0.37220 0.53940 0.51220 O7A O -0.1188(6) 0.6901(5) 0.4684(3) C35A C -0.0455(6) 0.8080(5) 0.4827(2) H49A H -0.06180 0.84990 0.52350 H50A H 0.05790 0.79720 0.48630 C36A C -0.2212(8) 0.6905(6) 0.4095(4) H51A H -0.23140 0.60670 0.38520 H52A H -0.31520 0.71690 0.41710 C37A C -0.1019(3) 0.8803(3) 0.43090(19) H53A H -0.18100 0.93160 0.44100 H54A H -0.02720 0.93710 0.42310 C38A C -0.1540(4) 0.7904(4) 0.37300(14) H55A H -0.22600 0.82720 0.34030 H56A H -0.07570 0.75580 0.35370 O8A O 0.1040(2) 0.62784(19) 0.59481(9) C39A C 0.2311(4) 0.7021(4) 0.61016(19) H57A H 0.31430 0.64820 0.62110 H58A H 0.24170 0.74710 0.57310 C40A C 0.2227(11) 0.795(1) 0.6666(5) H59A H 0.30940 0.79360 0.70070 H60A H 0.20960 0.88110 0.65360 C41A C 0.0912(9) 0.7479(6) 0.6890(4) H61A H 0.02950 0.81900 0.69660 H62A H 0.12110 0.70850 0.72940 C42A C 0.0213(5) 0.6657(6) 0.6442(2) H63A H -0.00190 0.59050 0.66390 H64A H -0.06920 0.70210 0.62360 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Re1 N1 2.037 1_555 1_555 N1 C2 1.392 1_555 1_555 N2 Re1 2.095 1_555 1_555 Na1 O3 2.353 1_555 1_555 O1 C20 1.160 1_555 1_555 O2 C21 1.168 1_555 1_555 O3 C22 1.173 1_555 1_555 C1 H1 0.980 1_555 1_555 H2 C1 0.980 1_555 1_555 H3 C1 0.980 1_555 1_555 C2 C1 1.497 1_555 1_555 C3 N2 1.409 1_555 1_555 C4 C3 1.432 1_555 1_555 H4 C4 0.950 1_555 1_555 C5 C4 1.359 1_555 1_555 H5 C5 0.950 1_555 1_555 C6 C5 1.425 1_555 1_555 H6 C6 0.950 1_555 1_555 C7 N2 1.376 1_555 1_555 H7 C7 0.949 1_555 1_555 C8 N1 1.439 1_555 1_555 C9 C8 1.410 1_555 1_555 C10 C9 1.391 1_555 1_555 H8 C10 0.951 1_555 1_555 C11 C10 1.386 1_555 1_555 H9 C11 0.950 1_555 1_555 C12 C11 1.384 1_555 1_555 H10 C12 0.950 1_555 1_555 C13 C8 1.402 1_555 1_555 C14 C9 1.514 1_555 1_555 H11 C14 1.000 1_555 1_555 C15 C14 1.529 1_555 1_555 H12 C15 0.980 1_555 1_555 H13 C15 0.980 1_555 1_555 H14 C15 0.980 1_555 1_555 C16 C14 1.536 1_555 1_555 H15 C16 0.980 1_555 1_555 H16 C16 0.980 1_555 1_555 H17 C16 0.980 1_555 1_555 C17 C13 1.518 1_555 1_555 H18 C17 1.000 1_555 1_555 C18 C17 1.504 1_555 1_555 H19 C18 0.981 1_555 1_555 H20 C18 0.980 1_555 1_555 H21 C18 0.980 1_555 1_555 C19 C17 1.536 1_555 1_555 H22 C19 0.980 1_555 1_555 H23 C19 0.980 1_555 1_555 H24 C19 0.980 1_555 1_555 C20 Re1 1.931 1_555 1_555 C21 Re1 1.903 1_555 1_555 C22 Re1 1.882 1_555 1_555 O4 Na1 2.372 1_555 1_555 C23 O4 1.434 1_555 1_555 H25 C23 0.991 1_555 1_555 H26 C23 0.990 1_555 1_555 C24 C23 1.514 1_555 1_555 H27 C24 0.990 1_555 1_555 H28 C24 0.989 1_555 1_555 C25 C24 1.527 1_555 1_555 H29 C25 0.991 1_555 1_555 H30 C25 0.989 1_555 1_555 C26 O4 1.426 1_555 1_555 H31 C26 0.990 1_555 1_555 H32 C26 0.989 1_555 1_555 O5 Na1 2.365 1_555 1_555 C27 O5 1.440 1_555 1_555 H33 C27 0.990 1_555 1_555 H34 C27 0.989 1_555 1_555 C28 C27 1.519 1_555 1_555 H35 C28 0.989 1_555 1_555 H36 C28 0.990 1_555 1_555 C29 C28 1.519 1_555 1_555 H37 C29 0.990 1_555 1_555 H38 C29 0.990 1_555 1_555 C30 O5 1.444 1_555 1_555 H39 C30 0.989 1_555 1_555 H40 C30 0.989 1_555 1_555 Na2 O6 2.390 1_555 1_555 O6 C31 1.431 1_555 1_555 C31 H41 0.990 1_555 1_555 H42 C31 0.990 1_555 1_555 C32 C31 1.502 1_555 1_555 H43 C32 0.989 1_555 1_555 H44 C32 0.990 1_555 1_555 C33 C32 1.453 1_555 1_555 H45 C33 0.990 1_555 1_555 H46 C33 0.989 1_555 1_555 C34 O6 1.432 1_555 1_555 H47 C34 0.989 1_555 1_555 H48 C34 0.990 1_555 1_555 O7 Na2 2.422 1_555 1_555 C35 O7 1.422 1_555 1_555 H49 C35 0.990 1_555 1_555 H50 C35 0.990 1_555 1_555 C36 O7 1.433 1_555 1_555 H51 C36 0.990 1_555 1_555 H52 C36 0.990 1_555 1_555 C37 C35 1.429 1_555 1_555 H53 C37 0.989 1_555 1_555 H54 C37 0.991 1_555 1_555 C38 C36 1.594 1_555 1_555 H55 C38 0.990 1_555 1_555 H56 C38 0.990 1_555 1_555 O8 Na2 2.379 1_555 1_555 C39 O8 1.420 1_555 1_555 H57 C39 0.990 1_555 1_555 H58 C39 0.990 1_555 1_555 C40 C39 1.513 1_555 1_555 H59 C40 0.990 1_555 1_555 H60 C40 0.989 1_555 1_555 C41 C40 1.543 1_555 1_555 H61 C41 0.990 1_555 1_555 H62 C41 0.989 1_555 1_555 C42 O8 1.483 1_555 1_555 H63 C42 0.990 1_555 1_555 H64 C42 0.990 1_555 1_555 Re1A N1A 2.037 1_555 1_555 N1A C2A 1.392 1_555 1_555 N2A Re1A 2.095 1_555 1_555 O1A C20A 1.160 1_555 1_555 O2A C21A 1.168 1_555 1_555 O3A Na1 2.353 1_555 1_555 C1A H1A 0.980 1_555 1_555 H2A C1A 0.980 1_555 1_555 H3A C1A 0.980 1_555 1_555 C2A C1A 1.497 1_555 1_555 C3A N2A 1.409 1_555 1_555 C4A C3A 1.432 1_555 1_555 H4A C4A 0.950 1_555 1_555 C5A C4A 1.359 1_555 1_555 H5A C5A 0.950 1_555 1_555 C6A C5A 1.425 1_555 1_555 H6A C6A 0.950 1_555 1_555 C7A N2A 1.376 1_555 1_555 H7A C7A 0.949 1_555 1_555 C8A N1A 1.439 1_555 1_555 C9A C8A 1.410 1_555 1_555 C10A C9A 1.391 1_555 1_555 H8A C10A 0.951 1_555 1_555 C11A C10A 1.386 1_555 1_555 H9A C11A 0.950 1_555 1_555 C12A C11A 1.384 1_555 1_555 H10A C12A 0.950 1_555 1_555 C13A C8A 1.402 1_555 1_555 C14A C9A 1.514 1_555 1_555 H11A C14A 1.000 1_555 1_555 C15A C14A 1.529 1_555 1_555 H12A C15A 0.980 1_555 1_555 H13A C15A 0.980 1_555 1_555 H14A C15A 0.980 1_555 1_555 C16A C14A 1.536 1_555 1_555 H15A C16A 0.980 1_555 1_555 H16A C16A 0.980 1_555 1_555 H17A C16A 0.980 1_555 1_555 C17A C13A 1.518 1_555 1_555 H18A C17A 1.000 1_555 1_555 C18A C17A 1.504 1_555 1_555 H19A C18A 0.981 1_555 1_555 H20A C18A 0.980 1_555 1_555 H21A C18A 0.980 1_555 1_555 C19A C17A 1.536 1_555 1_555 H22A C19A 0.980 1_555 1_555 H23A C19A 0.980 1_555 1_555 H24A C19A 0.980 1_555 1_555 C20A Re1A 1.931 1_555 1_555 C21A Re1A 1.903 1_555 1_555 C22A Re1A 1.882 1_555 1_555 O4A Na1 2.372 1_555 1_555 C23A O4A 1.434 1_555 1_555 H25A C23A 0.991 1_555 1_555 H26A C23A 0.990 1_555 1_555 C24A C23A 1.514 1_555 1_555 H27A C24A 0.990 1_555 1_555 H28A C24A 0.989 1_555 1_555 C25A C24A 1.527 1_555 1_555 H29A C25A 0.991 1_555 1_555 H30A C25A 0.989 1_555 1_555 C26A O4A 1.426 1_555 1_555 H31A C26A 0.990 1_555 1_555 H32A C26A 0.989 1_555 1_555 O5A Na1 2.365 1_555 1_555 C27A O5A 1.440 1_555 1_555 H33A C27A 0.990 1_555 1_555 H34A C27A 0.989 1_555 1_555 C28A C27A 1.519 1_555 1_555 H35A C28A 0.989 1_555 1_555 H36A C28A 0.990 1_555 1_555 C29A C28A 1.519 1_555 1_555 H37A C29A 0.990 1_555 1_555 H38A C29A 0.990 1_555 1_555 C30A O5A 1.444 1_555 1_555 H39A C30A 0.989 1_555 1_555 H40A C30A 0.989 1_555 1_555 O6A Na2 2.390 1_555 1_555 C31A O6A 1.431 1_555 1_555 H41A C31A 0.990 1_555 1_555 H42A C31A 0.990 1_555 1_555 C32A C31A 1.502 1_555 1_555 H43A C32A 0.989 1_555 1_555 H44A C32A 0.990 1_555 1_555 C33A C32A 1.453 1_555 1_555 H45A C33A 0.990 1_555 1_555 H46A C33A 0.989 1_555 1_555 C34A O6A 1.432 1_555 1_555 H47A C34A 0.989 1_555 1_555 H48A C34A 0.990 1_555 1_555 O7A Na2 2.422 1_555 1_555 C35A O7A 1.422 1_555 1_555 H49A C35A 0.990 1_555 1_555 H50A C35A 0.990 1_555 1_555 C36A O7A 1.433 1_555 1_555 H51A C36A 0.990 1_555 1_555 H52A C36A 0.990 1_555 1_555 C37A C35A 1.429 1_555 1_555 H53A C37A 0.989 1_555 1_555 H54A C37A 0.991 1_555 1_555 C38A C36A 1.594 1_555 1_555 H55A C38A 0.990 1_555 1_555 H56A C38A 0.990 1_555 1_555 O8A Na2 2.379 1_555 1_555 C39A O8A 1.420 1_555 1_555 H57A C39A 0.990 1_555 1_555 H58A C39A 0.990 1_555 1_555 C40A C39A 1.513 1_555 1_555 H59A C40A 0.990 1_555 1_555 H60A C40A 0.989 1_555 1_555 C41A C40A 1.543 1_555 1_555 H61A C41A 0.990 1_555 1_555 H62A C41A 0.989 1_555 1_555 C42A O8A 1.483 1_555 1_555 H63A C42A 0.990 1_555 1_555 H64A C42A 0.990 1_555 1_555 C2 C3 1.381 1_555 1_555 C6 C7 1.357 1_555 1_555 C12 C13 1.396 1_555 1_555 C25 C26 1.503 1_555 1_555 C29 C30 1.518 1_555 1_555 C33 C34 1.513 1_555 1_555 C37 C38 1.498 1_555 1_555 C41 C42 1.314 1_555 1_555 O3A C22A 1.173 1_555 1_555 C2A C3A 1.381 1_555 1_555 C6A C7A 1.357 1_555 1_555 C12A C13A 1.396 1_555 1_555 C25A C26A 1.503 1_555 1_555 C29A C30A 1.518 1_555 1_555 C33A C34A 1.513 1_555 1_555 C37A C38A 1.498 1_555 1_555 C41A C42A 1.314 1_555 1_555 #END data_CSD_CIF_JAPVEB _audit_creation_date 1990-02-14 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD JAPVEB _chemical_formula_sum 'C18 H36 K2 N2 O6' _chemical_formula_moiety ; C18 H36 K1 N2 O6 1+,K1 1- ; _journal_coden_Cambridge 4 _journal_volume 111 _journal_year 1989 _journal_page_first 5707 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "R.H.Huang" "D.L.Ward" "J.L.Dye" _chemical_name_systematic ; Cryptand(2.2.2)-potassium potasside ; _cell_volume 1476.104 _exptl_crystal_density_diffrn 1.02 _exptl_special_details ; Isostructural with rubidium analogue ; _diffrn_ambient_temperature 211 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_gt 0.032 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 12.300(5) _cell_length_b 12.421(6) _cell_length_c 11.474(6) _cell_angle_alpha 106.55(4) _cell_angle_beta 92.68(4) _cell_angle_gamma 62.02(3) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 K 1.89 N 0.68 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z K1 K 0.53429(8) 0.37032(8) 0.63754(9) K2 K -0.15813(5) -0.18659(5) -0.04676(6) O1 O -0.3603(2) -0.0242(2) -0.1501(2) O2 O -0.3212(2) 0.0648(2) 0.0936(2) O3 O 0.0616(2) -0.2034(2) 0.0465(2) O4 O 0.0392(2) -0.2215(2) -0.2022(2) O5 O -0.1618(2) -0.4210(2) -0.1642(2) O6 O -0.2029(2) -0.3187(2) 0.0905(2) N1 N -0.1635(2) -0.2631(2) -0.3153(2) N2 N -0.1492(2) -0.1141(2) 0.2213(2) C1 C -0.2887(3) -0.1840(3) -0.3450(3) C2 C -0.3439(3) -0.0443(3) -0.2774(3) C3 C -0.4144(3) 0.1088(3) -0.0847(3) C4 C -0.4352(3) 0.1283(3) 0.0463(4) C5 C -0.3376(3) 0.0882(3) 0.2224(3) C6 C -0.2158(3) 0.0264(3) 0.2693(3) C7 C -0.0188(3) -0.1620(3) 0.2485(3) C8 C 0.0583(3) -0.1396(3) 0.1704(3) C9 C 0.1442(2) -0.1938(3) -0.0286(3) C10 C 0.1557(2) -0.2712(3) -0.1551(3) C11 C 0.0506(3) -0.2915(3) -0.3266(3) C12 C -0.0738(3) -0.2432(3) -0.3745(3) C13 C -0.1325(3) -0.3995(3) -0.3584(4) C14 C -0.1993(3) -0.4354(3) -0.2831(4) C15 C -0.2272(3) -0.4506(3) -0.0892(4) C16 C -0.1813(3) -0.4450(3) 0.0311(4) C17 C -0.1699(3) -0.3065(3) 0.2122(3) C18 C -0.2093(3) -0.1685(3) 0.2771(3) H1 H -0.336(2) -0.213(2) -0.325(3) H2 H -0.290(3) -0.190(3) -0.438(3) H3 H -0.297(2) -0.004(2) -0.289(2) H4 H -0.418(3) 0.003(3) -0.306(3) H5 H -0.486(2) 0.151(2) -0.120(3) H6 H -0.361(2) 0.141(2) -0.100(2) H7 H -0.465(2) 0.215(2) 0.091(2) H8 H -0.483(2) 0.097(2) 0.060(3) H9 H -0.391(2) 0.058(2) 0.238(2) H10 H -0.377(2) 0.177(2) 0.259(3) H11 H -0.160(3) 0.059(3) 0.244(3) H12 H -0.230(3) 0.054(3) 0.355(3) H13 H 0.011(3) -0.251(3) 0.236(3) H14 H -0.012(3) -0.129(3) 0.339(3) H15 H 0.020(2) -0.047(2) 0.181(2) H16 H 0.144(2) -0.179(2) 0.194(3) H17 H 0.217(2) -0.222(2) 0.003(2) H18 H 0.110(2) -0.101(2) -0.020(2) H19 H 0.214(2) -0.266(2) -0.207(2) H20 H 0.182(2) -0.363(2) -0.160(2) H21 H 0.086(3) -0.382(2) -0.331(3) H22 H 0.105(3) -0.280(3) -0.371(3) H23 H -0.108(2) -0.151(2) -0.362(2) H24 H -0.065(3) -0.282(3) -0.464(3) H25 H -0.050(2) -0.446(2) -0.354(2) H26 H -0.153(3) -0.421(3) -0.443(3) H27 H -0.286(3) -0.384(3) -0.276(3) H28 H -0.176(3) -0.521(3) -0.319(3) H29 H -0.216(2) -0.533(2) -0.130(3) H30 H -0.307(2) -0.391(2) -0.085(3) H31 H -0.225(2) -0.467(2) 0.082(3) H32 H -0.093(2) -0.504(3) 0.026(3) H33 H -0.086(3) -0.357(3) 0.214(3) H34 H -0.213(2) -0.336(2) 0.250(3) H35 H -0.298(2) -0.115(2) 0.276(2) H36 H -0.191(3) -0.163(3) 0.368(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 K2 O1 2.835 1_555 1_555 O1 C2 1.417 1_555 1_555 O2 K2 2.816 1_555 1_555 O3 K2 2.797 1_555 1_555 O4 K2 2.870 1_555 1_555 O5 K2 2.860 1_555 1_555 O6 K2 2.807 1_555 1_555 N1 K2 2.962 1_555 1_555 N2 K2 2.961 1_555 1_555 C1 N1 1.475 1_555 1_555 C2 C1 1.500 1_555 1_555 C3 O1 1.430 1_555 1_555 C4 O2 1.420 1_555 1_555 C5 O2 1.427 1_555 1_555 C6 N2 1.474 1_555 1_555 C7 N2 1.479 1_555 1_555 C8 O3 1.409 1_555 1_555 C9 O3 1.429 1_555 1_555 C10 O4 1.419 1_555 1_555 C11 O4 1.418 1_555 1_555 C12 N1 1.470 1_555 1_555 C13 N1 1.481 1_555 1_555 C14 O5 1.409 1_555 1_555 C15 O5 1.430 1_555 1_555 C16 O6 1.419 1_555 1_555 C17 O6 1.422 1_555 1_555 C18 N2 1.474 1_555 1_555 H1 C1 0.882 1_555 1_555 H2 C1 1.048 1_555 1_555 H3 C2 0.958 1_555 1_555 H4 C2 0.929 1_555 1_555 H5 C3 0.932 1_555 1_555 H6 C3 0.959 1_555 1_555 H7 C4 0.943 1_555 1_555 H8 C4 0.883 1_555 1_555 H9 C5 0.941 1_555 1_555 H10 C5 0.939 1_555 1_555 H11 C6 1.032 1_555 1_555 H12 C6 0.940 1_555 1_555 H13 C7 0.955 1_555 1_555 H14 C7 1.017 1_555 1_555 H15 C8 0.988 1_555 1_555 H16 C8 0.994 1_555 1_555 H17 C9 0.896 1_555 1_555 H18 C9 1.000 1_555 1_555 H19 C10 0.989 1_555 1_555 H20 C10 1.013 1_555 1_555 H21 C11 0.983 1_555 1_555 H22 C11 0.944 1_555 1_555 H23 C12 0.984 1_555 1_555 H24 C12 0.989 1_555 1_555 H25 C13 0.910 1_555 1_555 H26 C13 0.985 1_555 1_555 H27 C14 0.944 1_555 1_555 H28 C14 0.926 1_555 1_555 H29 C15 0.942 1_555 1_555 H30 C15 0.903 1_555 1_555 H31 C16 0.981 1_555 1_555 H32 C16 0.977 1_555 1_555 H33 C17 0.926 1_555 1_555 H34 C17 0.947 1_555 1_555 H35 C18 0.977 1_555 1_555 H36 C18 1.046 1_555 1_555 C3 C4 1.468 1_555 1_555 C5 C6 1.485 1_555 1_555 C7 C8 1.500 1_555 1_555 C9 C10 1.465 1_555 1_555 C11 C12 1.500 1_555 1_555 C13 C14 1.500 1_555 1_555 C15 C16 1.462 1_555 1_555 C17 C18 1.502 1_555 1_555 #END data_CSD_CIF_JAPVIF _audit_creation_date 1990-02-14 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD JAPVIF _chemical_formula_sum 'C18 H36 N2 O6 Rb2' _chemical_formula_moiety ; C18 H36 N2 O6 Rb1 1+,Rb1 1- ; _journal_coden_Cambridge 4 _journal_volume 111 _journal_year 1989 _journal_page_first 5707 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "R.H.Huang" "D.L.Ward" "J.L.Dye" _chemical_name_systematic ; Cryptand(2.2.2)-rubidium rubidide ; _cell_volume 1506.889 _exptl_crystal_density_diffrn 1.11 _exptl_special_details ; Isostructural with potassium analogue Fw reported as 502.05; we calculate 547.43. Dx reported as 1.11; we calculate 1.21 ; _diffrn_ambient_temperature 218 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.061 _refine_ls_wR_factor_gt 0.061 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 12.418(4) _cell_length_b 12.419(3) _cell_length_c 11.582(3) _cell_angle_alpha 106.36(2) _cell_angle_beta 91.46(3) _cell_angle_gamma 62.38(2) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 N 0.68 O 0.68 Rb 1.93 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Rb1 Rb -0.1561(1) -0.1890(1) -0.0467(1) Rb2 Rb 0.5357(1) 0.3664(2) 0.6427(2) O1 O -0.3598(8) -0.0203(8) -0.1442(9) O2 O -0.3200(8) 0.0660(8) 0.0994(9) O3 O 0.0653(8) -0.2053(8) 0.0430(9) O4 O 0.0427(8) -0.2229(8) -0.2076(9) O5 O -0.1622(8) -0.4271(8) -0.165(1) O6 O -0.2030(9) -0.3240(8) 0.093(1) N1 N -0.165(1) -0.264(1) -0.315(1) N2 N -0.148(1) -0.116(1) 0.220(1) C1 C -0.287(1) -0.180(2) -0.341(2) C2 C -0.339(1) -0.040(1) -0.271(1) C3 C -0.415(1) 0.111(1) -0.076(2) C4 C -0.430(1) 0.126(1) 0.054(1) C5 C -0.337(1) 0.081(1) 0.224(1) C6 C -0.219(2) 0.023(1) 0.270(2) C7 C -0.023(2) -0.162(1) 0.246(1) C8 C 0.058(1) -0.140(1) 0.166(1) C9 C 0.145(1) -0.195(1) -0.032(1) C10 C 0.153(1) -0.269(1) -0.158(1) C11 C 0.049(1) -0.295(1) -0.327(1) C12 C -0.073(1) -0.245(2) -0.375(1) C13 C -0.136(2) -0.399(1) -0.358(2) C14 C -0.205(1) -0.431(1) -0.279(2) C15 C -0.228(1) -0.452(1) -0.088(2) C16 C -0.178(1) -0.451(1) 0.031(2) C17 C -0.162(1) -0.314(1) 0.210(1) C18 C -0.203(2) -0.178(1) 0.277(1) H1 H -0.34200 -0.20700 -0.32000 H2 H -0.28300 -0.19000 -0.42600 H3 H -0.28200 -0.01300 -0.28500 H4 H -0.41400 0.00700 -0.29900 H5 H -0.49100 0.15600 -0.10300 H6 H -0.36100 0.14400 -0.08700 H7 H -0.47100 0.21400 0.09900 H8 H -0.48000 0.08800 0.06400 H9 H -0.38200 0.04000 0.23500 H10 H -0.38200 0.16900 0.26700 H11 H -0.17200 0.06100 0.25300 H12 H -0.23500 0.04400 0.35600 H13 H 0.01400 -0.25100 0.23300 H14 H -0.02300 -0.12000 0.32900 H15 H 0.02000 -0.05100 0.17600 H16 H 0.13800 -0.16800 0.18900 H17 H 0.22300 -0.22300 -0.00500 H18 H 0.11200 -0.10900 -0.03000 H19 H 0.21400 -0.27000 -0.20600 H20 H 0.17700 -0.35400 -0.15800 H21 H 0.07300 -0.38000 -0.32900 H22 H 0.10900 -0.29500 -0.37700 H23 H -0.10300 -0.15600 -0.36000 H24 H -0.06200 -0.28500 -0.46000 H25 H -0.05100 -0.45000 -0.35500 H26 H -0.15200 -0.41900 -0.44000 H27 H -0.28900 -0.37000 -0.26900 H28 H -0.19500 -0.51400 -0.31900 H29 H -0.22400 -0.53300 -0.12500 H30 H -0.31200 -0.38800 -0.07200 H31 H -0.21400 -0.48000 0.07700 H32 H -0.09200 -0.50600 0.01500 H33 H -0.07600 -0.36100 0.20200 H34 H -0.19700 -0.34800 0.25400 H35? H -0.28900 0.00000 0.27900 H36? H -0.18200 0.00000 0.35700 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rb1 O1 2.887 1_555 1_555 O1 C2 1.429 1_555 1_555 O2 Rb1 2.866 1_555 1_555 O3 Rb1 2.852 1_555 1_555 O4 Rb1 2.928 1_555 1_555 O5 Rb1 2.923 1_555 1_555 O6 Rb1 2.872 1_555 1_555 N1 Rb1 2.997 1_555 1_555 N2 Rb1 2.977 1_555 1_555 C1 N1 1.471 1_555 1_555 C2 C1 1.513 1_555 1_555 C3 O1 1.421 1_555 1_555 C4 O2 1.392 1_555 1_555 C5 O2 1.410 1_555 1_555 C6 N2 1.464 1_555 1_555 C7 N2 1.441 1_555 1_555 C8 O3 1.408 1_555 1_555 C9 O3 1.405 1_555 1_555 C10 O4 1.397 1_555 1_555 C11 O4 1.401 1_555 1_555 C12 N1 1.492 1_555 1_555 C13 N1 1.472 1_555 1_555 C14 O5 1.407 1_555 1_555 C15 O5 1.409 1_555 1_555 C16 O6 1.421 1_555 1_555 C17 O6 1.428 1_555 1_555 C18 N2 1.514 1_555 1_555 H1 C1 0.951 1_555 1_555 H2 C1 0.957 1_555 1_555 H3 C2 0.947 1_555 1_555 H4 C2 0.949 1_555 1_555 H5 C3 0.946 1_555 1_555 H6 C3 0.960 1_555 1_555 H7 C4 0.950 1_555 1_555 H8 C4 0.963 1_555 1_555 H9 C5 0.944 1_555 1_555 H10 C5 0.947 1_555 1_555 H11 C6 0.957 1_555 1_555 H12 C6 0.957 1_555 1_555 H13 C7 0.946 1_555 1_555 H14 C7 0.956 1_555 1_555 H15 C8 0.951 1_555 1_555 H16 C8 0.947 1_555 1_555 H17 C9 0.944 1_555 1_555 H18 C9 0.943 1_555 1_555 H19 C10 0.944 1_555 1_555 H20 C10 0.955 1_555 1_555 H21 C11 0.948 1_555 1_555 H22 C11 0.955 1_555 1_555 H23 C12 0.951 1_555 1_555 H24 C12 0.950 1_555 1_555 H25 C13 0.952 1_555 1_555 H26 C13 0.952 1_555 1_555 H27 C14 0.948 1_555 1_555 H28 C14 0.953 1_555 1_555 H29 C15 0.954 1_555 1_555 H30 C15 0.955 1_555 1_555 H31 C16 0.940 1_555 1_555 H32 C16 0.951 1_555 1_555 H33 C17 0.941 1_555 1_555 H34 C17 0.964 1_555 1_555 C3 C4 1.470 1_555 1_555 C5 C6 1.465 1_555 1_555 C7 C8 1.546 1_555 1_555 C9 C10 1.467 1_555 1_555 C11 C12 1.506 1_555 1_555 C13 C14 1.513 1_555 1_555 C15 C16 1.496 1_555 1_555 C17 C18 1.483 1_555 1_555 #END data_CSD_CIF_JAPVOL _audit_creation_date 1990-02-14 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD JAPVOL _chemical_formula_sum 'C12 H24 O6 Rb2' _chemical_formula_moiety ; C12 H24 O6 Rb1 1+,Rb1 1- ; _journal_coden_Cambridge 4 _journal_volume 111 _journal_year 1989 _journal_page_first 5707 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "R.H.Huang" "D.L.Ward" "J.L.Dye" _chemical_name_systematic ; (18-Crown-6)-rubidium rubidide ; _cell_volume 2302.690 _exptl_crystal_density_diffrn 1.26 _diffrn_ambient_temperature 200 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_gt 0.044 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 -1/2+x,-1/2-y,-1/2+z _cell_length_a 14.852(4) _cell_length_b 8.614(2) _cell_length_c 18.075(4) _cell_angle_alpha 90 _cell_angle_beta 95.26(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 O 0.68 Rb 1.95 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Rb1 Rb 0.75030(9) 0.3521(2) -0.17282(7) Rb2 Rb 0.74750(6) 0.1661(1) 0.07977(5) O1 O 0.8926(4) 0.3229(7) 0.1801(3) O2 O 0.7093(4) 0.4211(7) 0.1791(3) O3 O 0.5774(4) 0.1885(7) 0.1568(3) O4 O 0.6140(5) -0.0803(7) 0.0751(3) O5 O 0.7987(5) -0.1734(7) 0.0765(3) O6 O 0.9323(4) 0.0609(8) 0.0963(3) C1 C 0.8670(6) 0.482(1) 0.1829(5) C2 C 0.7842(7) 0.494(1) 0.2227(5) C3 C 0.6285(6) 0.424(1) 0.2124(5) C4 C 0.5551(6) 0.348(1) 0.1634(5) C5 C 0.5085(7) 0.106(1) 0.1137(6) C6 C 0.5326(7) -0.063(1) 0.1121(6) C7 C 0.6432(7) -0.238(1) 0.0726(6) C8 C 0.7232(8) -0.245(1) 0.0337(6) C9 C 0.8793(7) -0.172(1) 0.0387(6) C10 C 0.9544(7) -0.100(1) 0.0876(6) C11 C 0.9987(6) 0.139(1) 0.1437(5) C12 C 0.9739(6) 0.307(1) 0.1455(6) H1 H 0.85500 0.52200 0.13400 H2 H 0.91400 0.54000 0.20900 H3 H 0.79400 0.44300 0.26900 H4 H 0.77100 0.60000 0.23000 H5 H 0.61200 0.52900 0.22000 H6 H 0.63700 0.37200 0.25900 H7 H 0.50000 0.35700 0.18600 H8 H 0.54900 0.39600 0.11600 H9 H 0.50000 0.14700 0.06500 H10 H 0.45400 0.11500 0.13700 H11 H 0.54100 -0.10600 0.16100 H12 H 0.48500 -0.11600 0.08400 H13 H 0.59700 -0.30100 0.04800 H14 H 0.65700 -0.27400 0.12200 H15 H 0.73700 -0.35100 0.02500 H16 H 0.71200 -0.19200 -0.01200 H17 H 0.86900 -0.11400 -0.00600 H18 H 0.89500 -0.27600 0.02700 H19 H 0.96000 -0.15100 0.13500 H20 H 1.01000 -0.11000 0.06500 H21 H 1.05600 0.12800 0.12500 H22 H 1.00100 0.09700 0.19200 H23 H 1.02100 0.36400 0.17300 H24 H 0.96500 0.34600 0.09600 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rb2 O1 3.007 1_555 1_555 O1 C1 1.424 1_555 1_555 O2 Rb2 2.925 1_555 1_555 O3 Rb2 3.001 1_555 1_555 O4 Rb2 2.900 1_555 1_555 O5 Rb2 3.024 1_555 1_555 O6 Rb2 2.880 1_555 1_555 C1 C2 1.484 1_555 1_555 C2 O2 1.446 1_555 1_555 C3 O2 1.391 1_555 1_555 C4 O3 1.421 1_555 1_555 C5 O3 1.419 1_555 1_555 C6 O4 1.442 1_555 1_555 C7 O4 1.428 1_555 1_555 C8 O5 1.441 1_555 1_555 C9 O5 1.432 1_555 1_555 C10 O6 1.436 1_555 1_555 C11 O6 1.416 1_555 1_555 C12 O1 1.416 1_555 1_555 H1 C1 0.950 1_555 1_555 H2 C1 0.948 1_555 1_555 H3 C2 0.945 1_555 1_555 H4 C2 0.946 1_555 1_555 H5 C3 0.950 1_555 1_555 H6 C3 0.952 1_555 1_555 H7 C4 0.951 1_555 1_555 H8 C4 0.948 1_555 1_555 H9 C5 0.946 1_555 1_555 H10 C5 0.949 1_555 1_555 H11 C6 0.956 1_555 1_555 H12 C6 0.949 1_555 1_555 H13 C7 0.952 1_555 1_555 H14 C7 0.950 1_555 1_555 H15 C8 0.952 1_555 1_555 H16 C8 0.945 1_555 1_555 H17 C9 0.950 1_555 1_555 H18 C9 0.954 1_555 1_555 H19 C10 0.960 1_555 1_555 H20 C10 0.958 1_555 1_555 H21 C11 0.949 1_555 1_555 H22 C11 0.943 1_555 1_555 H23 C12 0.956 1_555 1_555 H24 C12 0.953 1_555 1_555 C3 C4 1.491 1_555 1_555 C5 C6 1.500 1_555 1_555 C7 C8 1.436 1_555 1_555 C9 C10 1.493 1_555 1_555 C11 C12 1.494 1_555 1_555 #END data_CSD_CIF_JEMKIV _audit_creation_date 1991-02-12 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD JEMKIV _database_code_depnum_ccdc_archive 'CCDC 1184624' _chemical_formula_sum 'C52 H76 Li2 N4 O4' _chemical_formula_moiety ; C16 H32 Li1 O4 1+,C36 H44 Li1 N4 1- ; _journal_coden_Cambridge 182 _journal_year 1990 _journal_page_first 976 _journal_name_full 'Chem.Commun. ' loop_ _publ_author_name "J.Arnold" _chemical_name_systematic ; Octaethylporphyrinato-lithium tetrakis(tetrahydrofuran)-lithium ; _cell_volume 4917.550 _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.13 _exptl_special_details ; Moisture-sensitive ; _diffrn_ambient_temperature 188.15 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_gt 0.0543 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,1/2+z 3 1/2-x,y,-z 4 -x,1/2+y,1/2-z 5 -x,-y,-z 6 -1/2-x,-1/2-y,-1/2-z 7 -1/2+x,-y,z 8 x,-1/2-y,-1/2+z _cell_length_a 19.904(4) _cell_length_b 12.693(2) _cell_length_c 20.719(5) _cell_angle_alpha 90 _cell_angle_beta 110.04(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 0.98 N 0.68 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z O1 O 0.1729(2) 0.1203(3) 0.0030(2) O2 O 0.2191(2) -0.0401(3) -0.0827(2) C1 C 0.1264(3) 0.1721(4) -0.0572(3) C2 C 0.1221(3) 0.2858(4) -0.0382(3) C3 C 0.1614(3) 0.2920(4) 0.0380(3) C4 C 0.1698(3) 0.1792(4) 0.0607(2) C5 C 0.1527(3) -0.0953(5) -0.1044(3) C6 C 0.1608(3) -0.1858(4) -0.1441(3) C7 C 0.2347(3) -0.1803(5) -0.1441(3) C8 C 0.2662(3) -0.0882(6) -0.1129(3) Li1 Li 0.25000 0.0357(9) 0.00000 H1 H 0.08020 0.14110 -0.07110 H2 H 0.14530 0.16730 -0.09320 H3 H 0.07370 0.30650 -0.04870 H4 H 0.14430 0.32970 -0.06200 H5 H 0.13420 0.32980 0.06010 H6 H 0.20660 0.32460 0.04750 H7 H 0.21270 0.16990 0.09870 H8 H 0.13020 0.15720 0.07290 H9 H 0.11550 -0.05080 -0.13200 H10 H 0.14150 -0.11820 -0.06560 H11 H 0.12780 -0.18170 -0.18980 H12 H 0.15330 -0.24930 -0.12340 H13 H 0.23440 -0.18150 -0.18980 H14 H 0.26100 -0.23870 -0.11940 H15 H 0.31060 -0.10400 -0.07790 H16 H 0.27380 -0.04280 -0.14570 N1 N 0.5354(2) 0.1487(3) 0.0288(2) N2 N 0.4731(2) 0.0425(3) -0.1007(2) C9 C 0.5646(2) 0.1872(3) 0.0946(2) C10 C 0.5848(2) 0.2975(3) 0.0938(2) C11 C 0.5672(2) 0.3244(3) 0.0263(2) C12 C 0.5361(2) 0.2315(4) -0.0126(2) C13 C 0.5079(2) 0.2256(4) -0.0847(2) C14 C 0.4769(2) 0.1407(4) -0.1260(2) C15 C 0.4447(2) 0.1416(4) -0.2009(2) C16 C 0.4232(2) 0.0417(4) -0.2203(2) C17 C 0.4413(2) -0.0199(4) -0.1571(2) C18 C 0.5743(2) 0.1259(4) 0.1530(2) C19 C 0.6159(3) 0.3669(4) 0.1551(2) C20 C 0.5591(3) 0.4203(4) 0.1778(2) C21 C 0.5833(2) 0.4264(4) -0.0012(2) C22 C 0.6549(3) 0.4254(4) -0.0123(3) C23 C 0.4329(3) 0.2391(4) -0.2451(2) C24 C 0.3659(3) 0.2994(4) -0.2473(3) C25 C 0.3863(2) 0.0006(4) -0.2908(2) C26 C 0.3056(3) -0.0056(5) -0.3095(3) Li2 Li 0.50000 0.00000 0.00000 H17 H 0.51060 0.28890 -0.10840 H18 H 0.59440 0.16140 0.19590 H19 H 0.64400 0.41980 0.14400 H20 H 0.64560 0.32530 0.19200 H21 H 0.58200 0.46310 0.21680 H22 H 0.52960 0.46250 0.14150 H23 H 0.53120 0.36790 0.18940 H24 H 0.58390 0.48080 0.03050 H25 H 0.54670 0.44030 -0.04380 H26 H 0.66230 0.49200 -0.02970 H27 H 0.69180 0.41230 0.03010 H28 H 0.65460 0.37190 -0.04420 H29 H 0.42830 0.21900 -0.29050 H30 H 0.47300 0.28430 -0.22710 H31 H 0.36090 0.35970 -0.27560 H32 H 0.32540 0.25500 -0.26560 H33 H 0.37020 0.32040 -0.20210 H34 H 0.40380 -0.06820 -0.29370 H35 H 0.39680 0.04550 -0.32260 H36 H 0.28530 -0.03210 -0.35480 H37 H 0.29460 -0.05070 -0.27820 H38 H 0.28760 0.06290 -0.30710 O1B O 0.3271(2) 0.1203(3) -0.0030(2) O2B O 0.2809(2) -0.0401(3) 0.0827(2) C1B C 0.3736(3) 0.1721(4) 0.0572(3) C4B C 0.3302(3) 0.1792(4) -0.0607(2) C5B C 0.3473(3) -0.0953(5) 0.1044(3) C8B C 0.2338(3) -0.0882(6) 0.1129(3) C2B C 0.3779(3) 0.2858(4) 0.0382(3) H1B H 0.41980 0.14110 0.07110 H2B H 0.35470 0.16730 0.09320 C3B C 0.3386(3) 0.2920(4) -0.0380(3) H7B H 0.28730 0.16990 -0.09870 H8B H 0.36980 0.15720 -0.07290 C6B C 0.3392(3) -0.1858(4) 0.1441(3) H9B H 0.38450 -0.05080 0.13200 H10B H 0.35850 -0.11820 0.06560 C7B C 0.2653(3) -0.1803(5) 0.1441(3) H15B H 0.18940 -0.10400 0.07790 H16B H 0.22620 -0.04280 0.14570 H3B H 0.42630 0.30650 0.04870 H4B H 0.35570 0.32970 0.06200 H5B H 0.36580 0.32980 -0.06010 H6B H 0.29340 0.32460 -0.04750 H11B H 0.37220 -0.18170 0.18980 H12B H 0.34670 -0.24930 0.12340 H13B H 0.26560 -0.18150 0.18980 H14B H 0.23900 -0.23870 0.11940 C18D C 0.4257(2) -0.1259(4) -0.1530(2) C17D C 0.5587(2) 0.0199(4) 0.1571(2) N1D N 0.4646(2) -0.1487(3) -0.0288(2) N2D N 0.5269(2) -0.0425(3) 0.1007(2) C9D C 0.4354(2) -0.1872(3) -0.0946(2) H18D H 0.40560 -0.16140 -0.19590 C16D C 0.5768(2) -0.0417(4) 0.2203(2) C12D C 0.4639(2) -0.2315(4) 0.0126(2) C14D C 0.5231(2) -0.1407(4) 0.1260(2) C10D C 0.4152(2) -0.2975(3) -0.0938(2) C15D C 0.5553(2) -0.1416(4) 0.2009(2) C25D C 0.6137(2) -0.0006(4) 0.2908(2) C11D C 0.4328(2) -0.3244(3) -0.0263(2) C13D C 0.4921(2) -0.2256(4) 0.0847(2) C19D C 0.3841(3) -0.3669(4) -0.1551(2) C23D C 0.5671(3) -0.2391(4) 0.2451(2) C26D C 0.6944(3) 0.0056(5) 0.3095(3) H34D H 0.59620 0.06820 0.29370 H35D H 0.60320 -0.04550 0.32260 C21D C 0.4167(2) -0.4264(4) 0.0012(2) H17D H 0.48940 -0.28890 0.10840 C20D C 0.4409(3) -0.4203(4) -0.1778(2) H19D H 0.35600 -0.41980 -0.14400 H20D H 0.35440 -0.32530 -0.19200 C24D C 0.6341(3) -0.2994(4) 0.2473(3) H29D H 0.57170 -0.21900 0.29050 H30D H 0.52700 -0.28430 0.22710 H36D H 0.71470 0.03210 0.35480 H37D H 0.70540 0.05070 0.27820 H38D H 0.71240 -0.06290 0.30710 C22D C 0.3451(3) -0.4254(4) 0.0123(3) H24D H 0.41610 -0.48080 -0.03050 H25D H 0.45330 -0.44030 0.04380 H21D H 0.41800 -0.46310 -0.21680 H22D H 0.47040 -0.46250 -0.14150 H23D H 0.46880 -0.36790 -0.18940 H31D H 0.63910 -0.35970 0.27560 H32D H 0.67460 -0.25500 0.26560 H33D H 0.62980 -0.32040 0.20210 H26D H 0.33770 -0.49200 0.02970 H27D H 0.30820 -0.41230 -0.03010 H28D H 0.34540 -0.37190 0.04420 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 O1 C1 1.433 1_555 1_555 O2 C5 1.426 1_555 1_555 C1 C2 1.506 1_555 1_555 C2 C3 1.505 1_555 1_555 C3 C4 1.498 1_555 1_555 C4 O1 1.429 1_555 1_555 C5 C6 1.454 1_555 1_555 C6 C7 1.473 1_555 1_555 C7 C8 1.378 1_555 1_555 C8 O2 1.430 1_555 1_555 Li1 O1 1.891 1_555 1_555 H1 C1 0.950 1_555 1_555 H2 C1 0.945 1_555 1_555 H3 C2 0.949 1_555 1_555 H4 C2 0.948 1_555 1_555 H5 C3 0.950 1_555 1_555 H6 C3 0.948 1_555 1_555 H7 C4 0.950 1_555 1_555 H8 C4 0.949 1_555 1_555 H9 C5 0.951 1_555 1_555 H10 C5 0.950 1_555 1_555 H11 C6 0.951 1_555 1_555 H12 C6 0.949 1_555 1_555 H13 C7 0.945 1_555 1_555 H14 C7 0.950 1_555 1_555 H15 C8 0.953 1_555 1_555 H16 C8 0.942 1_555 1_555 N1 C9 1.376 1_555 1_555 N2 C14 1.364 1_555 1_555 C9 C10 1.458 1_555 1_555 C10 C11 1.364 1_555 1_555 C11 C12 1.443 1_555 1_555 C12 N1 1.360 1_555 1_555 C13 C12 1.406 1_555 1_555 C14 C13 1.383 1_555 1_555 C15 C14 1.462 1_555 1_555 C16 C15 1.355 1_555 1_555 C17 N2 1.374 1_555 1_555 C18 C9 1.395 1_555 1_555 C19 C10 1.494 1_555 1_555 C20 C19 1.524 1_555 1_555 C21 C11 1.493 1_555 1_555 C22 C21 1.519 1_555 1_555 C23 C15 1.509 1_555 1_555 C24 C23 1.525 1_555 1_555 C25 C16 1.487 1_555 1_555 C26 C25 1.520 1_555 1_555 Li2 N1 2.031 1_555 1_555 H17 C13 0.953 1_555 1_555 H18 C18 0.954 1_555 1_555 H19 C19 0.951 1_555 1_555 H20 C19 0.950 1_555 1_555 H21 C20 0.950 1_555 1_555 H22 C20 0.946 1_555 1_555 H23 C20 0.949 1_555 1_555 H24 C21 0.950 1_555 1_555 H25 C21 0.949 1_555 1_555 H26 C22 0.950 1_555 1_555 H27 C22 0.947 1_555 1_555 H28 C22 0.946 1_555 1_555 H29 C23 0.948 1_555 1_555 H30 C23 0.949 1_555 1_555 H31 C24 0.948 1_555 1_555 H32 C24 0.950 1_555 1_555 H33 C24 0.949 1_555 1_555 H34 C25 0.950 1_555 1_555 H35 C25 0.947 1_555 1_555 H36 C26 0.947 1_555 1_555 H37 C26 0.945 1_555 1_555 H38 C26 0.948 1_555 1_555 O1B Li1 1.891 1_555 1_555 O2B Li1 1.876 1_555 1_555 C1B O1B 1.433 1_555 1_555 C4B O1B 1.429 1_555 1_555 C5B O2B 1.426 1_555 1_555 C8B O2B 1.430 1_555 1_555 C2B C1B 1.506 1_555 1_555 H1B C1B 0.950 1_555 1_555 H2B C1B 0.945 1_555 1_555 C3B C4B 1.498 1_555 1_555 H7B C4B 0.950 1_555 1_555 H8B C4B 0.949 1_555 1_555 C6B C5B 1.454 1_555 1_555 H9B C5B 0.951 1_555 1_555 H10B C5B 0.950 1_555 1_555 C7B C8B 1.378 1_555 1_555 H15B C8B 0.953 1_555 1_555 H16B C8B 0.942 1_555 1_555 H3B C2B 0.949 1_555 1_555 H4B C2B 0.948 1_555 1_555 H5B C3B 0.950 1_555 1_555 H6B C3B 0.948 1_555 1_555 H11B C6B 0.951 1_555 1_555 H12B C6B 0.949 1_555 1_555 H13B C7B 0.945 1_555 1_555 H14B C7B 0.950 1_555 1_555 C18D C17 1.390 1_555 1_555 C17D C18 1.390 1_555 1_555 N1D Li2 2.031 1_555 1_555 N2D Li2 2.041 1_555 1_555 C9D C18D 1.395 1_555 1_555 H18D C18D 0.954 1_555 1_555 C16D C17D 1.460 1_555 1_555 C12D N1D 1.360 1_555 1_555 C14D N2D 1.364 1_555 1_555 C10D C9D 1.458 1_555 1_555 C15D C16D 1.355 1_555 1_555 C25D C16D 1.487 1_555 1_555 C11D C12D 1.443 1_555 1_555 C13D C12D 1.406 1_555 1_555 C19D C10D 1.494 1_555 1_555 C23D C15D 1.509 1_555 1_555 C26D C25D 1.520 1_555 1_555 H34D C25D 0.950 1_555 1_555 H35D C25D 0.947 1_555 1_555 C21D C11D 1.493 1_555 1_555 H17D C13D 0.953 1_555 1_555 C20D C19D 1.524 1_555 1_555 H19D C19D 0.951 1_555 1_555 H20D C19D 0.950 1_555 1_555 C24D C23D 1.525 1_555 1_555 H29D C23D 0.948 1_555 1_555 H30D C23D 0.949 1_555 1_555 H36D C26D 0.947 1_555 1_555 H37D C26D 0.945 1_555 1_555 H38D C26D 0.948 1_555 1_555 C22D C21D 1.519 1_555 1_555 H24D C21D 0.950 1_555 1_555 H25D C21D 0.949 1_555 1_555 H21D C20D 0.950 1_555 1_555 H22D C20D 0.946 1_555 1_555 H23D C20D 0.949 1_555 1_555 H31D C24D 0.948 1_555 1_555 H32D C24D 0.950 1_555 1_555 H33D C24D 0.949 1_555 1_555 H26D C22D 0.950 1_555 1_555 H27D C22D 0.947 1_555 1_555 H28D C22D 0.946 1_555 1_555 O2 Li1 1.876 1_555 1_555 N2 Li2 2.041 1_555 1_555 C16 C17 1.460 1_555 1_555 C2B C3B 1.505 1_555 1_555 C6B C7B 1.473 1_555 1_555 C17D N2D 1.374 1_555 1_555 N1D C9D 1.376 1_555 1_555 C14D C15D 1.462 1_555 1_555 C14D C13D 1.383 1_555 1_555 C10D C11D 1.364 1_555 1_555 #END data_CSD_CIF_JEPMEW _audit_creation_date 1991-03-28 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD JEPMEW _chemical_formula_sum 'C20 H40 Cs1 K1 O10' _chemical_formula_moiety ; C20 H40 Cs1 O10 1+,K1 1- ; _journal_coeditor_code "IUCr CR0151" _journal_coden_Cambridge 591 _journal_volume 46 _journal_year 1990 _journal_page_first 1838 _journal_name_full 'Acta Crystallogr.,Sect.C:Cryst.Struct.Commun. ' loop_ _publ_author_name "D.L.Ward" "Rui H.Wang" "J.L.Dye" _chemical_name_systematic ; bis(15-Crown-5)-cesium potassium ; _chemical_name_common ; bis(15-Crown-5)-cesium kalide ; _cell_volume 1676.619 _exptl_crystal_colour 'dark grey' _exptl_crystal_density_diffrn 1.21 _exptl_special_details ; Isostructural with Rb(15C5)2.Na and Rb(15C5)2.Rb ; _diffrn_ambient_temperature 213 _refine_special_details ; C(8a) and C(8b) and their associated hydrogens are all disordered over two sites with equal occupancies. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.067 _refine_ls_wR_factor_gt 0.067 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,z 3 -x,y,-z 4 1/2-x,1/2+y,-z 5 -x,-y,-z 6 -1/2-x,-1/2-y,-z 7 x,-y,z 8 -1/2+x,-1/2-y,z _cell_length_a 11.537(4) _cell_length_b 13.679(3) _cell_length_c 10.624(3) _cell_angle_alpha 90 _cell_angle_beta 90.12(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Cs 2.10 K 1.33 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Cs1 Cs 0.50000 0.00000 0.50000 K1 K 0.50000 0.50000 0.00000 O1 O 0.4754(7) 0.00000 0.2033(8) O2 O 0.5141(5) -0.1790(4) 0.3301(5) O3 O 0.7271(5) -0.1056(4) 0.4388(6) C1 C 0.4117(8) -0.0877(7) 0.1790(8) C2 C 0.4872(9) -0.1710(7) 0.204(1) C3 C 0.614(1) -0.2347(6) 0.3558(9) C4 C 0.7228(8) -0.1789(8) 0.347(1) C5? C 0.828(1) -0.031(1) 0.470(2) C6 C 0.819(1) -0.055(1) 0.384(2) H1 H 0.391(6) -0.073(5) 0.110(7) H2 H 0.369(6) -0.075(5) 0.237(7) H3 H 0.461(6) -0.218(6) 0.179(7) H4 H 0.543(4) -0.154(4) 0.167(4) H5 H 0.600(6) -0.288(5) 0.314(6) H6 H 0.605(5) -0.239(4) 0.420(5) H7 H 0.778(6) -0.209(5) 0.345(6) H8 H 0.734(6) -0.153(6) 0.284(7) H9? H 0.90200 -0.06100 0.46500 H10? H 0.81600 -0.00800 0.55400 H11 H 0.80200 -0.03300 0.30100 H12 H 0.88800 -0.09100 0.38400 O1D O 0.5246(7) 0.00000 0.7967(8) O2D O 0.4859(5) 0.1790(4) 0.6699(5) O2B O 0.4859(5) -0.1790(4) 0.6699(5) O2F O 0.5141(5) 0.1790(4) 0.3301(5) O3D O 0.2729(5) 0.1056(4) 0.5612(6) O3B O 0.2729(5) -0.1056(4) 0.5612(6) O3F O 0.7271(5) 0.1056(4) 0.4388(6) C1F C 0.4117(8) 0.0877(7) 0.1790(8) C6F C 0.819(1) 0.055(1) 0.384(2) C1D C 0.5883(8) 0.0877(7) 0.8210(8) C1B C 0.5883(8) -0.0877(7) 0.8210(8) C2D C 0.5128(9) 0.1710(7) 0.796(1) C3D C 0.386(1) 0.2347(6) 0.6442(9) C2B C 0.5128(9) -0.1710(7) 0.796(1) C3B C 0.386(1) -0.2347(6) 0.6442(9) C2F C 0.4872(9) 0.1710(7) 0.204(1) C3F C 0.614(1) 0.2347(6) 0.3558(9) C4D C 0.2772(8) 0.1789(8) 0.653(1) C6D C 0.181(1) 0.055(1) 0.616(2) C4B C 0.2772(8) -0.1789(8) 0.653(1) C6B C 0.181(1) -0.055(1) 0.616(2) C4F C 0.7228(8) 0.1789(8) 0.347(1) H1F H 0.391(6) 0.073(5) 0.110(7) H2F H 0.369(6) 0.075(5) 0.237(7) H11F H 0.80200 0.03300 0.30100 H12F H 0.88800 0.09100 0.38400 H1D H 0.609(6) 0.073(5) 0.890(7) H2D H 0.631(6) 0.075(5) 0.763(7) H1B H 0.609(6) -0.073(5) 0.890(7) H2B H 0.631(6) -0.075(5) 0.763(7) H3D H 0.539(6) 0.218(6) 0.821(7) H4D H 0.457(4) 0.154(4) 0.833(4) H5D H 0.400(6) 0.288(5) 0.686(6) H6D H 0.395(5) 0.239(4) 0.580(5) H3B H 0.539(6) -0.218(6) 0.821(7) H4B H 0.457(4) -0.154(4) 0.833(4) H5B H 0.400(6) -0.288(5) 0.686(6) H6B H 0.395(5) -0.239(4) 0.580(5) H3F H 0.461(6) 0.218(6) 0.179(7) H4F H 0.543(4) 0.154(4) 0.167(4) H5F H 0.600(6) 0.288(5) 0.314(6) H6F H 0.605(5) 0.239(4) 0.420(5) H7D H 0.222(6) 0.209(5) 0.655(6) H8D H 0.266(6) 0.153(6) 0.716(7) H11D H 0.19800 0.03300 0.69900 H12D H 0.11200 0.09100 0.61600 H7B H 0.222(6) -0.209(5) 0.655(6) H8B H 0.266(6) -0.153(6) 0.716(7) H11B H 0.19800 -0.03300 0.69900 H12B H 0.11200 -0.09100 0.61600 H7F H 0.778(6) 0.209(5) 0.345(6) H8F H 0.734(6) 0.153(6) 0.284(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cs1 O1 3.164 1_555 1_555 O1 C1 1.430 1_555 1_555 O2 Cs1 3.046 1_555 1_555 O3 Cs1 3.063 1_555 1_555 C1 C2 1.458 1_555 1_555 C2 O2 1.379 1_555 1_555 C3 O2 1.408 1_555 1_555 C4 O3 1.400 1_555 1_555 C6 O3 1.395 1_555 1_555 H1 C1 0.796 1_555 1_555 H2 C1 0.809 1_555 1_555 H3 C2 0.758 1_555 1_555 H4 C2 0.790 1_555 1_555 H5 C3 0.869 1_555 1_555 H6 C3 0.693 1_555 1_555 H7 C4 0.759 1_555 1_555 H8 C4 0.768 1_555 1_555 H11 C6 0.952 1_555 1_555 H12 C6 0.936 1_555 1_555 O1D Cs1 3.164 1_555 1_555 O2D Cs1 3.046 1_555 1_555 O2B Cs1 3.046 1_555 1_555 O2F Cs1 3.046 1_555 1_555 O3D Cs1 3.063 1_555 1_555 O3B Cs1 3.063 1_555 1_555 O3F Cs1 3.063 1_555 1_555 C1F O1 1.430 1_555 1_555 C6F C6 1.505 1_555 1_555 C1D O1D 1.430 1_555 1_555 C1B O1D 1.430 1_555 1_555 C2D O2D 1.379 1_555 1_555 C3D O2D 1.408 1_555 1_555 C2B O2B 1.379 1_555 1_555 C3B O2B 1.408 1_555 1_555 C2F O2F 1.379 1_555 1_555 C3F O2F 1.408 1_555 1_555 C4D O3D 1.400 1_555 1_555 C6D O3D 1.395 1_555 1_555 C4B O3B 1.400 1_555 1_555 C6B O3B 1.395 1_555 1_555 C4F O3F 1.400 1_555 1_555 H1F C1F 0.796 1_555 1_555 H2F C1F 0.809 1_555 1_555 H11F C6F 0.952 1_555 1_555 H12F C6F 0.936 1_555 1_555 H1D C1D 0.796 1_555 1_555 H2D C1D 0.809 1_555 1_555 H1B C1B 0.796 1_555 1_555 H2B C1B 0.809 1_555 1_555 H3D C2D 0.758 1_555 1_555 H4D C2D 0.790 1_555 1_555 H5D C3D 0.869 1_555 1_555 H6D C3D 0.693 1_555 1_555 H3B C2B 0.758 1_555 1_555 H4B C2B 0.790 1_555 1_555 H5B C3B 0.869 1_555 1_555 H6B C3B 0.693 1_555 1_555 H3F C2F 0.758 1_555 1_555 H4F C2F 0.790 1_555 1_555 H5F C3F 0.869 1_555 1_555 H6F C3F 0.693 1_555 1_555 H7D C4D 0.759 1_555 1_555 H8D C4D 0.768 1_555 1_555 H11D C6D 0.952 1_555 1_555 H12D C6D 0.936 1_555 1_555 H7B C4B 0.759 1_555 1_555 H8B C4B 0.768 1_555 1_555 H11B C6B 0.952 1_555 1_555 H12B C6B 0.936 1_555 1_555 H7F C4F 0.759 1_555 1_555 H8F C4F 0.768 1_555 1_555 C3 C4 1.472 1_555 1_555 O3F C6F 1.395 1_555 1_555 C1F C2F 1.458 1_555 1_555 C1D C2D 1.458 1_555 1_555 C1B C2B 1.458 1_555 1_555 C3D C4D 1.472 1_555 1_555 C3B C4B 1.472 1_555 1_555 C3F C4F 1.472 1_555 1_555 C6D C6B 1.505 1_555 1_555 #END data_CSD_CIF_JEPMIA _audit_creation_date 1991-03-28 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD JEPMIA _chemical_formula_sum 'C20 H40 O10 Rb2' _chemical_formula_moiety ; C20 H40 O10 Rb1 1+,Rb1 1- ; _journal_coeditor_code "IUCr CR0151" _journal_coden_Cambridge 591 _journal_volume 46 _journal_year 1990 _journal_page_first 1838 _journal_name_full 'Acta Crystallogr.,Sect.C:Cryst.Struct.Commun. ' loop_ _publ_author_name "D.L.Ward" "Rui H.Wang" "J.L.Dye" _chemical_name_systematic ; bis(15-Crown-5)-rubidium rubidide ; _cell_volume 1701.297 _exptl_crystal_colour 'dark grey' _exptl_crystal_density_diffrn 1.19 _exptl_special_details ; monoclinic polymorph Isostructural with Rb(15C5)2.Na and Cs(15C5)2.K ; _diffrn_ambient_temperature 222 _refine_special_details ; C(8a) and C(8b) and their associated hydrogens are all disordered over two sites with equal occupancies. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.05 _refine_ls_wR_factor_gt 0.05 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,z 3 -x,y,-z 4 1/2-x,1/2+y,-z 5 -x,-y,-z 6 -1/2-x,-1/2-y,-z 7 x,-y,z 8 -1/2+x,-1/2-y,z _cell_length_a 11.635(3) _cell_length_b 13.855(5) _cell_length_c 10.556(3) _cell_angle_alpha 90 _cell_angle_beta 88.82(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 O 0.68 Rb 1.99 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Rb1 Rb 0.50000 0.00000 0.50000 Rb2 Rb 0.50000 0.50000 0.00000 O1 O 0.4703(6) 0.00000 0.2112(6) O2 O 0.5127(4) -0.1756(3) 0.3353(4) O3 O 0.7210(4) -0.1041(3) 0.4454(5) C1 C 0.4084(6) -0.0855(5) 0.1857(6) C2 C 0.4878(7) -0.1665(5) 0.2058(6) C3 C 0.6128(6) -0.2293(5) 0.3633(8) C4 C 0.7201(6) -0.1749(6) 0.3492(8) C5 C 0.80770 -0.04680 0.39840 C6? C 0.81240 0.03900 0.47780 H1 H 0.37890 -0.08530 0.10380 H2 H 0.34670 -0.09150 0.24830 H3 H 0.45610 -0.22500 0.17660 H4 H 0.55680 -0.15220 0.15670 H5 H 0.61740 -0.28240 0.30630 H6 H 0.60740 -0.25240 0.44810 H7 H 0.78510 -0.21590 0.35250 H8 H 0.72170 -0.14350 0.26900 H9 H 0.79950 -0.03930 0.30510 H10 H 0.89020 -0.08910 0.38470 H11? H 0.89230 0.04430 0.43880 H12? H 0.81700 -0.00700 0.54470 O1D O 0.5297(6) 0.00000 0.7888(6) O2D O 0.4873(4) 0.1756(3) 0.6647(4) O2B O 0.4873(4) -0.1756(3) 0.6647(4) O2F O 0.5127(4) 0.1756(3) 0.3353(4) O3D O 0.2790(4) 0.1041(3) 0.5546(5) O3B O 0.2790(4) -0.1041(3) 0.5546(5) O3F O 0.7210(4) 0.1041(3) 0.4454(5) C1F C 0.4084(6) 0.0855(5) 0.1857(6) C5F C 0.80770 0.04680 0.39840 C1D C 0.5916(6) 0.0855(5) 0.8143(6) C1B C 0.5916(6) -0.0855(5) 0.8143(6) C2D C 0.5122(7) 0.1665(5) 0.7942(6) C3D C 0.3872(6) 0.2293(5) 0.6367(8) C2B C 0.5122(7) -0.1665(5) 0.7942(6) C3B C 0.3872(6) -0.2293(5) 0.6367(8) C2F C 0.4878(7) 0.1665(5) 0.2058(6) C3F C 0.6128(6) 0.2293(5) 0.3633(8) C4D C 0.2799(6) 0.1749(6) 0.6508(8) C5D C 0.19230 0.04680 0.60160 C4B C 0.2799(6) -0.1749(6) 0.6508(8) C5B C 0.19230 -0.04680 0.60160 C4F C 0.7201(6) 0.1749(6) 0.3492(8) H1F H 0.37890 0.08530 0.10380 H2F H 0.34670 0.09150 0.24830 H9F H 0.79950 0.03930 0.30510 H10F H 0.89020 0.08910 0.38470 H1D H 0.62110 0.08530 0.89620 H2D H 0.65330 0.09150 0.75170 H1B H 0.62110 -0.08530 0.89620 H2B H 0.65330 -0.09150 0.75170 H3D H 0.54390 0.22500 0.82340 H4D H 0.44320 0.15220 0.84330 H5D H 0.38260 0.28240 0.69370 H6D H 0.39260 0.25240 0.55190 H3B H 0.54390 -0.22500 0.82340 H4B H 0.44320 -0.15220 0.84330 H5B H 0.38260 -0.28240 0.69370 H6B H 0.39260 -0.25240 0.55190 H3F H 0.45610 0.22500 0.17660 H4F H 0.55680 0.15220 0.15670 H5F H 0.61740 0.28240 0.30630 H6F H 0.60740 0.25240 0.44810 H7D H 0.21490 0.21590 0.64750 H8D H 0.27830 0.14350 0.73100 H9D H 0.20050 0.03930 0.69490 H10D H 0.10980 0.08910 0.61530 H7B H 0.21490 -0.21590 0.64750 H8B H 0.27830 -0.14350 0.73100 H9B H 0.20050 -0.03930 0.69490 H10B H 0.10980 -0.08910 0.61530 H7F H 0.78510 0.21590 0.35250 H8F H 0.72170 0.14350 0.26900 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rb1 O1 3.075 1_555 1_555 O1 C1 1.415 1_555 1_555 O2 Rb1 2.992 1_555 1_555 O3 Rb1 2.994 1_555 1_555 C1 C2 1.472 1_555 1_555 C2 O2 1.409 1_555 1_555 C3 O2 1.418 1_555 1_555 C4 O3 1.412 1_555 1_555 C5 O3 1.369 1_555 1_555 H1 C1 0.937 1_555 1_555 H2 C1 0.969 1_555 1_555 H3 C2 0.945 1_555 1_555 H4 C2 0.967 1_555 1_555 H5 C3 0.951 1_555 1_555 H6 C3 0.952 1_555 1_555 H7 C4 0.947 1_555 1_555 H8 C4 0.952 1_555 1_555 H9 C5 0.997 1_555 1_555 H10 C5 1.131 1_555 1_555 O1D Rb1 3.075 1_555 1_555 O2D Rb1 2.992 1_555 1_555 O2B Rb1 2.992 1_555 1_555 O2F Rb1 2.992 1_555 1_555 O3D Rb1 2.994 1_555 1_555 O3B Rb1 2.994 1_555 1_555 O3F Rb1 2.994 1_555 1_555 C1F O1 1.415 1_555 1_555 C5F C5 1.297 1_555 1_555 C1D O1D 1.415 1_555 1_555 C1B O1D 1.415 1_555 1_555 C2D O2D 1.409 1_555 1_555 C3D O2D 1.418 1_555 1_555 C2B O2B 1.409 1_555 1_555 C3B O2B 1.418 1_555 1_555 C2F O2F 1.409 1_555 1_555 C3F O2F 1.418 1_555 1_555 C4D O3D 1.412 1_555 1_555 C5D O3D 1.369 1_555 1_555 C4B O3B 1.412 1_555 1_555 C5B O3B 1.369 1_555 1_555 C4F O3F 1.412 1_555 1_555 H1F C1F 0.937 1_555 1_555 H2F C1F 0.969 1_555 1_555 H9F C5F 0.997 1_555 1_555 H10F C5F 1.131 1_555 1_555 H1D C1D 0.937 1_555 1_555 H2D C1D 0.969 1_555 1_555 H1B C1B 0.937 1_555 1_555 H2B C1B 0.969 1_555 1_555 H3D C2D 0.945 1_555 1_555 H4D C2D 0.967 1_555 1_555 H5D C3D 0.951 1_555 1_555 H6D C3D 0.952 1_555 1_555 H3B C2B 0.945 1_555 1_555 H4B C2B 0.967 1_555 1_555 H5B C3B 0.951 1_555 1_555 H6B C3B 0.952 1_555 1_555 H3F C2F 0.945 1_555 1_555 H4F C2F 0.967 1_555 1_555 H5F C3F 0.951 1_555 1_555 H6F C3F 0.952 1_555 1_555 H7D C4D 0.947 1_555 1_555 H8D C4D 0.952 1_555 1_555 H9D C5D 0.997 1_555 1_555 H10D C5D 1.131 1_555 1_555 H7B C4B 0.947 1_555 1_555 H8B C4B 0.952 1_555 1_555 H9B C5B 0.997 1_555 1_555 H10B C5B 1.131 1_555 1_555 H7F C4F 0.947 1_555 1_555 H8F C4F 0.952 1_555 1_555 C3 C4 1.463 1_555 1_555 O3F C5F 1.369 1_555 1_555 C1F C2F 1.472 1_555 1_555 C1D C2D 1.472 1_555 1_555 C1B C2B 1.472 1_555 1_555 C3D C4D 1.463 1_555 1_555 C3B C4B 1.463 1_555 1_555 C3F C4F 1.463 1_555 1_555 C5D C5B 1.297 1_555 1_555 #END data_CSD_CIF_JEPMIB _audit_creation_date 1994-05-24 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD JEPMIB _chemical_formula_sum 'C20 H40 O10 Rb2' _chemical_formula_moiety ; C20 H40 O10 Rb1 1+,Rb1 1- ; _journal_coden_Cambridge 4 _journal_volume 115 _journal_year 1993 _journal_page_first 9542 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "R.H.Huang" "J.L.Eglin" "S.Z.Huang" "L.E.H.McMills" "J.L.Dye" _chemical_name_systematic ; (1,4,7,10,13,16-Hexaoxacyclo-octadecane)-(1,4,7,10-tetraoxacyclododecane)-rubi dium rubidide ; _cell_volume 3392.896 _exptl_special_details ; orthorhombic polymorph ; _diffrn_ambient_temperature 180 _refine_special_details ; The 12-crown-4 ring has imposed disorder. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.031 _refine_ls_wR_factor_gt 0.031 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2+z 3 x,1/2-y,z 4 1/2-x,-y,1/2+z 5 -x,-y,-z 6 -1/2+x,-1/2-y,-1/2-z 7 -x,-1/2+y,-z 8 -1/2+x,y,-1/2-z _cell_length_a 14.063(10) _cell_length_b 14.167(10) _cell_length_c 17.03(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.71 H 0.23 O 0.68 Rb 2.09 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Rb1 Rb 0.3921(1) 0.25000 0.3540(1) Rb2 Rb 0.1032(2) 0.75000 0.3520(1) O1 O 0.5780(8) 0.25000 0.4458(7) O2 O 0.5055(6) 0.0757(6) 0.3906(7) O3 O 0.4250(8) 0.0837(9) 0.2407(8) O4 O 0.343(1) 0.25000 0.184(1) O5 O 0.2070(6) 0.3500(6) 0.3489(6) O6 O 0.2941(6) 0.3520(9) 0.4974(6) C1 C 0.575(1) 0.168(1) 0.491(1) C2 C 0.586(1) 0.083(1) 0.439(1) C3 C 0.516(1) 0.002(1) 0.334(1) C4 C 0.430(2) -0.001(2) 0.284(2) C5 C 0.346(2) 0.082(3) 0.189(1) C6 C 0.353(2) 0.167(3) 0.136(1) C7 C 0.145(2) 0.378(2) 0.398(2) C8? C 0.201(3) 0.423(3) 0.416(2) C9 C 0.223(2) 0.387(2) 0.497(2) C10 C 0.231(2) 0.436(2) 0.449(2) C11 C 0.302(1) 0.271(3) 0.568(1) C12? C 0.242(2) 0.324(2) 0.555(1) C13 C 0.137(1) 0.271(2) 0.2918(9) C14? C 0.128(2) 0.311(2) 0.339(2) H1 H 0.62720 0.17420 0.52850 H2 H 0.51750 0.16970 0.51930 H3 H 0.58890 0.03240 0.47680 H4 H 0.64270 0.09010 0.41340 H5 H 0.57250 0.01820 0.30850 H6 H 0.52770 -0.05170 0.36810 H7 H 0.38000 -0.01380 0.32010 H8 H 0.44390 -0.05790 0.25550 H9 H 0.35070 0.02670 0.16120 H10 H 0.29310 0.08570 0.22140 H11 H 0.30090 0.16000 0.10130 H12 H 0.41060 0.16530 0.10980 H13 H 0.25220 0.47540 0.40790 H14 H 0.14320 0.46200 0.41660 H15 H 0.17660 0.32670 0.51380 H16 H 0.21530 0.42070 0.54800 H17? H 0.37180 0.24310 0.57280 H18 H 0.29390 0.29200 0.62280 H19? H 0.11200 0.29640 0.40460 H20? H 0.07950 0.35820 0.33430 O2B O 0.5055(6) 0.4243(6) 0.3906(7) C2B C 0.586(1) 0.417(1) 0.439(1) C1B C 0.575(1) 0.332(1) 0.491(1) H1B H 0.62720 0.32580 0.52850 H2B H 0.51750 0.33030 0.51930 H3B H 0.58890 0.46760 0.47680 H4B H 0.64270 0.40990 0.41340 C3B C 0.516(1) 0.498(1) 0.334(1) C4B C 0.430(2) 0.501(2) 0.284(2) O3B O 0.4250(8) 0.4163(9) 0.2407(8) O5B O 0.2070(6) 0.1500(6) 0.3489(6) C7B C 0.145(2) 0.122(2) 0.398(2) C10B C 0.231(2) 0.064(2) 0.449(2) O6B O 0.2941(6) 0.1480(9) 0.4974(6) C9B C 0.223(2) 0.113(2) 0.497(2) H13B H 0.25220 0.02460 0.40790 H15B H 0.17660 0.17330 0.51380 H16B H 0.21530 0.07930 0.54800 C11B C 0.302(1) 0.229(3) 0.568(1) H18B H 0.29390 0.20800 0.62280 H14B H 0.14320 0.03800 0.41660 C13B C 0.137(1) 0.229(2) 0.2918(9) C6B C 0.353(2) 0.333(3) 0.136(1) C5B C 0.346(2) 0.418(3) 0.189(1) H9B H 0.35070 0.47330 0.16120 H10B H 0.29310 0.41430 0.22140 H11B H 0.30090 0.34000 0.10130 H12B H 0.41060 0.33470 0.10980 H7B H 0.38000 0.51380 0.32010 H8B H 0.44390 0.55790 0.25550 H5B H 0.57250 0.48180 0.30850 H6B H 0.52770 0.55170 0.36810 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rb1 O1 3.046 1_555 1_555 O1 C1 1.394 1_555 1_555 O2 Rb1 3.005 1_555 1_555 O3 Rb1 3.080 1_555 1_555 O4 Rb1 2.976 1_555 1_555 O5 Rb1 2.965 1_555 1_555 O6 Rb1 3.155 1_555 1_555 C1 C2 1.503 1_555 1_555 C2 O2 1.404 1_555 1_555 C3 O2 1.429 1_555 1_555 C4 O3 1.410 1_555 1_555 C5 O3 1.418 1_555 1_555 C6 O4 1.439 1_555 1_555 C7 O5 1.272 1_555 1_555 C9 O6 1.116 1_555 1_555 C10 O6 1.698 1_555 1_555 C11 O6 1.666 1_555 1_555 C13 O5 1.780 1_555 1_555 H1 C1 0.977 1_555 1_555 H2 C1 0.942 1_555 1_555 H3 C2 0.964 1_555 1_555 H4 C2 0.914 1_555 1_555 H5 C3 0.934 1_555 1_555 H6 C3 0.971 1_555 1_555 H7 C4 0.951 1_555 1_555 H8 C4 0.961 1_555 1_555 H9 C5 0.918 1_555 1_555 H10 C5 0.928 1_555 1_555 H11 C6 0.947 1_555 1_555 H12 C6 0.925 1_555 1_555 H13 C10 0.944 1_555 1_555 H14 C7 1.232 1_555 1_555 H15 C9 1.112 1_555 1_555 H16 C9 0.997 1_555 1_555 H18 C11 0.986 1_555 1_555 O2B Rb1 3.005 1_555 1_555 C2B O2B 1.404 1_555 1_555 C1B O1 1.394 1_555 1_555 H1B C1B 0.977 1_555 1_555 H2B C1B 0.942 1_555 1_555 H3B C2B 0.964 1_555 1_555 H4B C2B 0.914 1_555 1_555 C3B O2B 1.429 1_555 1_555 C4B C3B 1.480 1_555 1_555 O3B Rb1 3.080 1_555 1_555 O5B Rb1 2.965 1_555 1_555 C7B O5B 1.272 1_555 1_555 C10B C7B 1.701 1_555 1_555 O6B Rb1 3.155 1_555 1_555 C9B C10B 1.078 1_555 1_555 H13B C10B 0.944 1_555 1_555 H15B C9B 1.112 1_555 1_555 H16B C9B 0.997 1_555 1_555 C11B C11 0.595 1_555 1_555 H18B C11 1.296 1_555 1_555 H14B C7B 1.232 1_555 1_555 C13B C13 0.595 1_555 1_555 C6B O4 1.439 1_555 1_555 C5B O3B 1.418 1_555 1_555 H9B C5B 0.918 1_555 1_555 H10B C5B 0.928 1_555 1_555 H11B C6B 0.947 1_555 1_555 H12B C6B 0.925 1_555 1_555 H7B C4B 0.951 1_555 1_555 H8B C4B 0.961 1_555 1_555 H5B C3B 0.934 1_555 1_555 H6B C3B 0.971 1_555 1_555 C3 C4 1.480 1_555 1_555 C5 C6 1.508 1_555 1_555 C7 C10 1.701 1_555 1_555 C9 C10 1.078 1_555 1_555 H18 C11B 1.296 1_555 1_555 C2B C1B 1.503 1_555 1_555 C4B O3B 1.410 1_555 1_555 O5B C13B 1.780 1_555 1_555 C10B O6B 1.698 1_555 1_555 O6B C9B 1.116 1_555 1_555 O6B C11B 1.666 1_555 1_555 C11B H18B 0.986 1_555 1_555 C6B C5B 1.508 1_555 1_555 #END data_CSD_CIF_JODLOD _audit_creation_date 1992-05-28 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD JODLOD _database_code_depnum_ccdc_archive 'CCDC 1188069' _chemical_formula_sum 'C44 H86 Li2 N4 O10 S2 Si4' _chemical_formula_moiety ; C16 H32 Li1 O8 1+,C24 H46 Li1 N4 S2 Si4 1-,C4 H8 O2 ; _journal_coden_Cambridge 182 _journal_year 1991 _journal_page_first 1477 _journal_name_full 'Chem.Commun. ' loop_ _publ_author_name "F.Pauer" "J.Rocha" "D.Stalke" _chemical_name_systematic ; bis(12-Crown-4)-lithium bis(N,N'-bis(trimethylsilyl)benzenesulfinamidino)-lithium 1,4-dioxane solvate ; _cell_volume 11417.207 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.189 _exptl_special_details ; air-sensitive ; _diffrn_ambient_temperature 153 _refine_special_details ; One of the lithium co-ordinated crown ethers is disordered. The solvent, presumed to be 1,4-dioxane, is disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_gt 0.0628 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,z 3 -x,y,1/2-z 4 1/2-x,1/2+y,1/2-z 5 -x,-y,-z 6 -1/2-x,-1/2-y,-z 7 x,-y,-1/2+z 8 -1/2+x,-1/2-y,-1/2+z _cell_length_a 17.954(2) _cell_length_b 15.611(2) _cell_length_c 40.833(6) _cell_angle_alpha 90 _cell_angle_beta 93.97(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.21 N 0.68 O 1.03 S 1.02 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.4965(4) 0.2986(5) 0.0938(2) O1 O 0.4241(2) 0.1985(2) 0.1163(1) C1 C 0.4598(5) 0.1418(5) 0.1374(2) C2 C 0.5353(5) 0.1307(4) 0.1294(2) O2 O 0.5760(2) 0.2077(2) 0.1213(1) C3 C 0.6148(5) 0.2469(6) 0.1482(3) C4 C 0.6217(4) 0.3334(4) 0.1471(2) O3 O 0.5592(2) 0.3785(2) 0.1326(1) C5 C 0.5177(4) 0.4171(5) 0.1568(2) C6 C 0.4446(4) 0.4324(6) 0.1477(2) O4 O 0.4053(2) 0.3710(2) 0.1274(1) C7 C 0.3671(4) 0.3121(5) 0.1455(2) C8 C 0.3585(4) 0.2357(6) 0.1298(2) O5 O 0.6006(2) 0.3293(2) 0.0651(1) C9 C 0.5666(3) 0.4751(3) 0.0617(1) C10 C 0.6046(3) 0.4036(3) 0.0452(1) O6 O 0.4988(2) 0.2007(2) 0.0530(1) C11 C 0.6210(3) 0.2529(4) 0.0492(1) C12 C 0.5541(3) 0.2145(3) 0.0302(1) O7 O 0.3896(2) 0.3210(2) 0.0567(1) C13 C 0.4258(3) 0.1850(3) 0.0387(1) C14 C 0.3875(3) 0.2683(3) 0.0283(1) O8 O 0.4918(2) 0.4537(2) 0.0682(1) C15 C 0.3720(3) 0.4085(3) 0.0501(1) C16 C 0.4394(3) 0.4575(3) 0.0409(1) H1 H 0.43090 0.08710 0.13780 H2 H 0.46170 0.16810 0.15970 H3 H 0.53280 0.09140 0.11000 H4 H 0.56480 0.10160 0.14780 H5 H 0.66360 0.21700 0.15280 H6 H 0.58300 0.23380 0.16670 H7 H 0.66680 0.34630 0.13490 H8 H 0.63040 0.35530 0.17010 H9 H 0.54440 0.46990 0.16500 H10 H 0.51640 0.37560 0.17540 H11 H 0.44670 0.48440 0.13340 H12 H 0.41510 0.44780 0.16670 H13 H 0.31650 0.33440 0.14980 H14 H 0.39580 0.30440 0.16720 H15 H 0.34330 0.19300 0.14630 H16 H 0.31650 0.24010 0.11250 H17 H 0.56860 0.53000 0.04910 H18 H 0.59540 0.48270 0.08330 H19 H 0.57400 0.39250 0.02430 H20 H 0.65710 0.41680 0.04010 H21 H 0.64370 0.21000 0.06520 H22 H 0.65890 0.26650 0.03310 H23 H 0.53390 0.25380 0.01240 H24 H 0.56780 0.15900 0.02000 H25 H 0.39560 0.15330 0.05450 H26 H 0.42970 0.14850 0.01880 H27 H 0.41360 0.29650 0.01040 H28 H 0.33460 0.25710 0.02010 H29 H 0.34930 0.43520 0.06930 H30 H 0.33390 0.40900 0.03100 H31 H 0.46090 0.43320 0.02100 H32 H 0.42640 0.51900 0.03670 S1 S 0.1563(1) 0.3778(1) 0.3881(1) C17 C 0.1894(2) 0.4626(3) 0.4160(1) C18 C 0.2311(3) 0.5285(3) 0.4045(1) C19 C 0.2624(3) 0.5904(3) 0.4260(1) C20 C 0.2510(3) 0.5853(3) 0.4590(1) C21 C 0.2088(3) 0.5200(4) 0.4706(1) C22 C 0.1777(3) 0.4583(3) 0.4491(1) N1 N 0.0912(2) 0.3337(2) 0.4069(1) Si1 Si 0.0989(1) 0.2317(1) 0.4214(1) C23 C 0.1242(4) 0.1522(4) 0.3900(2) C24 C 0.1690(3) 0.2181(4) 0.4567(1) C25 C 0.0048(3) 0.2049(3) 0.4355(2) N2 N 0.1144(2) 0.4288(2) 0.3581(1) Si2 Si 0.1445(1) 0.4225(1) 0.3194(1) C26 C 0.0627(3) 0.4457(4) 0.2905(1) C27 C 0.1836(3) 0.3149(4) 0.3095(1) C28 C 0.2182(3) 0.5026(4) 0.3115(1) Li2 Li 0.0086(4) 0.3815(5) 0.3733(2) S2 S -0.1408(1) 0.3693(1) 0.3610(1) C29 C -0.1776(2) 0.4524(3) 0.3332(1) C30 C -0.2396(3) 0.4987(3) 0.3412(1) C31 C -0.2676(3) 0.5637(4) 0.3208(1) C32 C -0.2344(3) 0.5829(3) 0.2923(1) C33 C -0.1732(3) 0.5360(3) 0.2841(1) C34 C -0.1448(3) 0.4704(3) 0.3041(1) N3 N -0.0770(2) 0.3243(2) 0.3414(1) Si3 Si -0.0956(1) 0.2280(1) 0.3227(1) C35 C -0.1777(4) 0.2325(4) 0.2920(2) C36 C -0.1176(3) 0.1422(3) 0.3522(2) C37 C -0.0105(3) 0.1955(4) 0.3020(2) N4 N -0.0947(2) 0.4228(2) 0.3890(1) Si4 Si -0.1251(1) 0.4376(1) 0.4273(1) C38 C -0.0414(3) 0.4621(3) 0.4552(1) C39 C -0.1743(3) 0.3419(3) 0.4435(1) C40 C -0.1911(3) 0.5303(3) 0.4290(1) H33 H 0.24200 0.53320 0.38090 H34 H 0.29250 0.63840 0.41750 H35 H 0.27580 0.62700 0.47480 H36 H 0.19690 0.51880 0.49420 H37 H 0.14720 0.41160 0.45820 H38 H 0.17480 0.16430 0.38230 H39 H 0.12340 0.09310 0.39950 H40 H 0.08590 0.15660 0.37110 H41 H 0.22020 0.23130 0.44980 H42 H 0.15710 0.25710 0.47500 H43 H 0.16720 0.15730 0.46420 H44 H -0.00810 0.24660 0.45280 H45 H -0.03290 0.20900 0.41640 H46 H 0.00460 0.14550 0.44470 H47 H 0.04340 0.50360 0.29600 H48 H 0.07820 0.44580 0.26740 H49 H 0.02260 0.40200 0.29260 H50 H 0.14560 0.26950 0.31280 H51 H 0.19840 0.31260 0.28630 H52 H 0.22850 0.30520 0.32490 H53 H 0.19920 0.56160 0.31550 H54 H 0.26270 0.49070 0.32690 H55 H 0.23270 0.49810 0.28830 H56 H -0.26650 0.48280 0.36100 H57 H -0.31050 0.59820 0.32790 H58 H -0.25540 0.62930 0.27750 H59 H -0.14710 0.54890 0.26380 H60 H -0.10110 0.43570 0.29790 H61 H -0.17150 0.27770 0.27510 H62 H -0.18370 0.17540 0.28110 H63 H -0.22300 0.24540 0.30410 H64 H -0.16380 0.15620 0.36340 H65 H -0.12430 0.08620 0.34050 H66 H -0.07420 0.13820 0.36890 H67 H 0.00170 0.23970 0.28550 H68 H 0.03170 0.19090 0.31930 H69 H -0.01830 0.13890 0.29090 H70 H -0.01530 0.51330 0.44670 H71 H -0.05710 0.47440 0.47780 H72 H -0.00670 0.41190 0.45610 H73 H -0.14090 0.29070 0.44310 H74 H -0.18780 0.35270 0.46650 H75 H -0.22080 0.33110 0.42910 H76 H -0.16710 0.58330 0.42090 H77 H -0.23740 0.51760 0.41480 H78 H -0.20440 0.53920 0.45210 O9? O 0.4953(10) 0.233(1) 0.2302(4) C41? C 0.4429(7) 0.2277(7) 0.2417(3) C42? C 0.38150 0.27100 0.25170 O10? O 0.3897(3) 0.3542(5) 0.2678(1) O11? O 0.3654(23) 0.3303(32) 0.2358(9) C43? C 0.3736(7) 0.4211(10) 0.2486(4) C44? C 0.4339(8) 0.4789(9) 0.2448(3) O12? O 0.4838(6) 0.4667(9) 0.2339(3) H79? H 0.46000 0.19650 0.26230 H80? H 0.41870 0.18260 0.22720 H81? H 0.46000 0.25320 0.22100 H82? H 0.35660 0.23240 0.26710 H83? H 0.34600 0.27790 0.23190 H84? H 0.39220 0.28700 0.27520 H85? H 0.33860 0.23000 0.25070 H86? H 0.33170 0.45250 0.25820 H87? H 0.35470 0.40060 0.22630 H88? H 0.32750 0.45120 0.23950 H89? H 0.36940 0.41850 0.27280 H90? H 0.44810 0.50310 0.26700 H91? H 0.41160 0.52710 0.23130 H92? H 0.41570 0.53680 0.25110 H93? H 0.44250 0.48120 0.22090 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 O1 2.267 1_555 1_555 O1 C1 1.364 1_555 1_555 C1 C2 1.427 1_555 1_555 C2 O2 1.457 1_555 1_555 O2 Li1 2.256 1_555 1_555 C3 O2 1.400 1_555 1_555 C4 C3 1.357 1_555 1_555 O3 Li1 2.255 1_555 1_555 C5 O3 1.413 1_555 1_555 C6 C5 1.360 1_555 1_555 O4 Li1 2.480 1_555 1_555 C7 O4 1.390 1_555 1_555 C8 O1 1.455 1_555 1_555 O5 Li1 2.324 1_555 1_555 C9 C10 1.493 1_555 1_555 C10 O5 1.421 1_555 1_555 O6 Li1 2.263 1_555 1_555 C11 O5 1.418 1_555 1_555 C12 O6 1.424 1_555 1_555 O7 Li1 2.387 1_555 1_555 C13 O6 1.419 1_555 1_555 C14 O7 1.420 1_555 1_555 O8 Li1 2.636 1_555 1_555 C15 O7 1.424 1_555 1_555 C16 O8 1.409 1_555 1_555 H1 C1 1.000 1_555 1_555 H2 C1 0.997 1_555 1_555 H3 C2 1.001 1_555 1_555 H4 C2 0.998 1_555 1_555 H5 C3 0.999 1_555 1_555 H6 C3 0.999 1_555 1_555 H7 C4 1.000 1_555 1_555 H8 C4 1.001 1_555 1_555 H9 C5 1.000 1_555 1_555 H10 C5 1.000 1_555 1_555 H11 C6 1.002 1_555 1_555 H12 C6 0.999 1_555 1_555 H13 C7 1.000 1_555 1_555 H14 C7 1.001 1_555 1_555 H15 C8 0.999 1_555 1_555 H16 C8 0.999 1_555 1_555 H17 C9 1.002 1_555 1_555 H18 C9 0.998 1_555 1_555 H19 C10 0.998 1_555 1_555 H20 C10 1.001 1_555 1_555 H21 C11 1.002 1_555 1_555 H22 C11 1.001 1_555 1_555 H23 C12 1.000 1_555 1_555 H24 C12 0.999 1_555 1_555 H25 C13 1.002 1_555 1_555 H26 C13 0.999 1_555 1_555 H27 C14 0.998 1_555 1_555 H28 C14 1.000 1_555 1_555 H29 C15 0.999 1_555 1_555 H30 C15 1.001 1_555 1_555 H31 C16 0.998 1_555 1_555 H32 C16 1.000 1_555 1_555 S1 C17 1.819 1_555 1_555 C17 C18 1.374 1_555 1_555 C18 C19 1.397 1_555 1_555 C19 C20 1.379 1_555 1_555 C20 C21 1.374 1_555 1_555 C21 C22 1.394 1_555 1_555 C22 C17 1.384 1_555 1_555 N1 S1 1.598 1_555 1_555 Si1 N1 1.701 1_555 1_555 C23 Si1 1.863 1_555 1_555 C24 Si1 1.859 1_555 1_555 C25 Si1 1.870 1_555 1_555 N2 S1 1.604 1_555 1_555 Si2 N2 1.708 1_555 1_555 C26 Si2 1.855 1_555 1_555 C27 Si2 1.875 1_555 1_555 C28 Si2 1.865 1_555 1_555 Li2 N1 2.087 1_555 1_555 S2 C29 1.818 1_555 1_555 C29 C30 1.385 1_555 1_555 C30 C31 1.385 1_555 1_555 C31 C32 1.377 1_555 1_555 C32 C33 1.381 1_555 1_555 C33 C34 1.385 1_555 1_555 C34 C29 1.391 1_555 1_555 N3 Li2 2.140 1_555 1_555 Si3 N3 1.709 1_555 1_555 C35 Si3 1.869 1_555 1_555 C36 Si3 1.862 1_555 1_555 C37 Si3 1.867 1_555 1_555 N4 Li2 2.105 1_555 1_555 Si4 N4 1.707 1_555 1_555 C38 Si4 1.862 1_555 1_555 C39 Si4 1.879 1_555 1_555 C40 Si4 1.875 1_555 1_555 H33 C18 0.999 1_555 1_555 H34 C19 1.000 1_555 1_555 H35 C20 0.999 1_555 1_555 H36 C21 1.002 1_555 1_555 H37 C22 0.999 1_555 1_555 H38 C23 1.000 1_555 1_555 H39 C23 1.001 1_555 1_555 H40 C23 1.000 1_555 1_555 H41 C24 1.001 1_555 1_555 H42 C24 0.998 1_555 1_555 H43 C24 0.999 1_555 1_555 H44 C25 1.000 1_555 1_555 H45 C25 0.999 1_555 1_555 H46 C25 1.001 1_555 1_555 H47 C26 0.999 1_555 1_555 H48 C26 1.002 1_555 1_555 H49 C26 1.000 1_555 1_555 H50 C27 0.999 1_555 1_555 H51 C27 1.002 1_555 1_555 H52 C27 0.999 1_555 1_555 H53 C28 1.000 1_555 1_555 H54 C28 0.999 1_555 1_555 H55 C28 1.002 1_555 1_555 H56 C30 1.001 1_555 1_555 H57 C31 0.999 1_555 1_555 H58 C32 1.000 1_555 1_555 H59 C33 1.001 1_555 1_555 H60 C34 1.000 1_555 1_555 H61 C35 0.999 1_555 1_555 H62 C35 0.999 1_555 1_555 H63 C35 1.001 1_555 1_555 H64 C36 0.999 1_555 1_555 H65 C36 1.000 1_555 1_555 H66 C36 1.001 1_555 1_555 H67 C37 0.999 1_555 1_555 H68 C37 1.002 1_555 1_555 H69 C37 0.998 1_555 1_555 H70 C38 1.001 1_555 1_555 H71 C38 1.002 1_555 1_555 H72 C38 1.000 1_555 1_555 H73 C39 1.000 1_555 1_555 H74 C39 1.000 1_555 1_555 H75 C39 1.002 1_555 1_555 H76 C40 1.000 1_555 1_555 H77 C40 1.000 1_555 1_555 H78 C40 0.999 1_555 1_555 C4 O3 1.419 1_555 1_555 C6 O4 1.422 1_555 1_555 C7 C8 1.358 1_555 1_555 C9 O8 1.427 1_555 1_555 C11 C12 1.508 1_555 1_555 C13 C14 1.518 1_555 1_555 C15 C16 1.501 1_555 1_555 N2 Li2 2.168 1_555 1_555 S2 N3 1.604 1_555 1_555 S2 N4 1.600 1_555 1_555 #END data_CSD_CIF_JUXTAX _audit_creation_date 1993-11-16 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD JUXTAX _chemical_formula_sum 'C46 H42 Cd2 N1 Na1 O6 S6' _chemical_formula_moiety ; C42 H30 Cd2 Na1 O6 S6 1-,C4 H12 N1 1+ ; _journal_coden_Cambridge 9 _journal_volume 32 _journal_year 1993 _journal_page_first 791 _journal_name_full 'Inorg.Chem. ' loop_ _publ_author_name "J.J.Vittal" "P.A.W.Dean" _chemical_name_systematic ; Tetramethylammonium hexakis(\m~2~-thiobenzoato)-di-cadmium-sodium ; _cell_volume 1243.542 _exptl_crystal_colour 'orange-yellow' _exptl_crystal_density_diffrn 1.529 _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; _refine_special_details ; Tetramethylammonium carbon atoms are disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_gt 0.0559 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.026(1) _cell_length_b 11.886(2) _cell_length_c 10.906(1) _cell_angle_alpha 94.32(1) _cell_angle_beta 113.25(1) _cell_angle_gamma 71.53(1) _cell_formula_units_Z 1 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Cd 1.56 N 0.68 Na 1.40 O 0.68 S 1.02 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 0.50000 0.50000 0.50000 Cd1 Cd 0.51664(4) 0.57885(4) 0.20015(4) S1 S 0.7443(2) 0.6170(2) 0.2961(2) S2 S 0.3099(2) 0.7610(2) 0.1253(2) S3 S 0.4731(3) 0.3941(2) 0.0874(2) O1 O 0.6309(6) 0.6216(5) 0.4674(6) O2 O 0.3195(5) 0.6392(4) 0.3186(5) O3 O 0.5656(6) 0.3858(4) 0.3429(4) C1 C 0.7340(6) 0.6432(6) 0.4397(6) C2 C 0.2481(6) 0.7344(6) 0.2262(6) C3 C 0.5231(6) 0.3286(6) 0.2295(6) C4 C 0.8268(7) 0.6911(6) 0.5555(7) C5 C 0.9632(8) 0.6648(7) 0.5688(8) C6 C 1.055(1) 0.7125(10) 0.6703(10) C7 C 1.0056(14) 0.7908(10) 0.751(1) C8 C 0.8652(14) 0.8238(10) 0.7348(10) C9 C 0.7764(9) 0.7687(7) 0.6381(7) C10 C 0.1148(6) 0.8030(6) 0.2354(7) C11 C 0.0194(7) 0.8815(6) 0.1249(8) C12 C -0.1070(9) 0.9488(8) 0.1227(11) C13 C -0.1414(10) 0.9414(10) 0.2271(13) C14 C -0.0485(11) 0.8638(10) 0.3347(12) C15 C 0.0785(10) 0.7965(8) 0.3397(9) C16 C 0.5305(6) 0.2058(5) 0.2582(6) C17 C 0.4708(7) 0.1432(6) 0.1528(8) C18 C 0.4740(9) 0.0274(7) 0.1766(11) C19 C 0.5374(10) -0.0229(7) 0.3027(12) C20 C 0.5946(10) 0.0378(7) 0.4082(11) C21 C 0.5917(8) 0.1522(7) 0.3873(8) N1? N 1.00000 0.50000 0.00000 C22? C 1.05920 0.57990 -0.04050 C23? C 0.85180 0.52400 -0.09130 C24? C 1.01020 0.52180 0.13910 C25? C 1.07880 0.37440 -0.00720 H1 H 0.99500 0.61300 0.50950 H2 H 1.14980 0.69140 0.68250 H3 H 1.06750 0.82410 0.81910 H4 H 0.83160 0.88150 0.78860 H5 H 0.68350 0.78410 0.62990 H6 H 0.04380 0.88800 0.05190 H7 H -0.17140 1.00060 0.04700 H8 H -0.22910 0.98940 0.22600 H9 H -0.07460 0.85650 0.40630 H10 H 0.14240 0.74590 0.41670 H11 H 0.42670 0.17810 0.06430 H12 H 0.43230 -0.01590 0.10400 H13 H 0.54220 -0.10230 0.31670 H14 H 0.63600 0.00210 0.49630 H15 H 0.63180 0.19480 0.46130 O1A O 0.3691(6) 0.3784(5) 0.5326(6) O2A O 0.6805(5) 0.3608(4) 0.6814(5) O3A O 0.4344(6) 0.6142(4) 0.6571(4) C1A C 0.2660(6) 0.3568(6) 0.5603(6) C2A C 0.7519(6) 0.2656(6) 0.7738(6) C3A C 0.4769(6) 0.6714(6) 0.7705(6) S1A S 0.2557(2) 0.3830(2) 0.7039(2) C4A C 0.1732(7) 0.3089(6) 0.4445(7) S2A S 0.6901(2) 0.2390(2) 0.8747(2) C10A C 0.8852(6) 0.1970(6) 0.7646(7) S3A S 0.5269(3) 0.6059(2) 0.9126(2) C16A C 0.4695(6) 0.7942(5) 0.7418(6) Cd1A Cd 0.48336(4) 0.42115(4) 0.79985(4) C5A C 0.0368(8) 0.3352(7) 0.4312(8) C9A C 0.2236(9) 0.2313(7) 0.3619(7) C11A C 0.9806(7) 0.1185(6) 0.8751(8) C15A C 0.9215(10) 0.2035(8) 0.6603(9) C17A C 0.5292(7) 0.8568(6) 0.8472(8) C21A C 0.4083(8) 0.8478(7) 0.6127(8) C6A C -0.055(1) 0.2875(10) 0.3297(10) H1A H 0.00500 0.38700 0.49050 C8A C 0.1348(14) 0.1762(10) 0.2652(10) H5A H 0.31650 0.21590 0.37010 C12A C 1.1070(9) 0.0512(8) 0.8773(11) H6A H 0.95620 0.11200 0.94810 C14A C 1.0485(11) 0.1362(10) 0.6653(12) H10A H 0.85760 0.25410 0.58330 C18A C 0.5260(9) 0.9726(7) 0.8234(11) H11A H 0.57330 0.82190 0.93570 C20A C 0.4054(10) 0.9622(7) 0.5918(11) H15A H 0.36820 0.80520 0.53870 C7A C -0.0056(14) 0.2092(10) 0.249(1) H2A H -0.14980 0.30860 0.31750 H4A H 0.16840 0.11850 0.21140 C13A C 1.1414(10) 0.0586(10) 0.7729(13) H7A H 1.17140 -0.00060 0.95300 H9A H 1.07460 0.14350 0.59370 C19A C 0.4626(10) 1.0229(7) 0.6973(12) H12A H 0.56770 1.01590 0.89600 H14A H 0.36400 0.99790 0.50370 H3A H -0.06750 0.17590 0.18090 H8A H 1.22910 0.01060 0.77400 H13A H 0.45780 1.10230 0.68330 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Na1 O1 2.470 1_555 1_555 Cd1 S1 2.485 1_555 1_555 S1 C1 1.615 1_555 1_555 S2 Cd1 2.494 1_555 1_555 S3 Cd1 2.522 1_555 1_555 O1 C1 1.385 1_555 1_555 O2 Na1 2.431 1_555 1_555 O3 Na1 2.304 1_555 1_555 C1 C4 1.485 1_555 1_555 C2 S2 1.599 1_555 1_555 C3 S3 1.596 1_555 1_555 C4 C5 1.385 1_555 1_555 C5 C6 1.399 1_555 1_555 C6 C7 1.368 1_555 1_555 C7 C8 1.411 1_555 1_555 C8 C9 1.410 1_555 1_555 C9 C4 1.384 1_555 1_555 C10 C2 1.476 1_555 1_555 C11 C10 1.406 1_555 1_555 C12 C11 1.361 1_555 1_555 C13 C12 1.351 1_555 1_555 C14 C13 1.376 1_555 1_555 C15 C10 1.361 1_555 1_555 C16 C3 1.486 1_555 1_555 C17 C16 1.376 1_555 1_555 C18 C17 1.407 1_555 1_555 C19 C18 1.356 1_555 1_555 C20 C19 1.354 1_555 1_555 C21 C16 1.399 1_555 1_555 H1 C5 0.950 1_555 1_555 H2 C6 0.950 1_555 1_555 H3 C7 0.949 1_555 1_555 H4 C8 0.950 1_555 1_555 H5 C9 0.950 1_555 1_555 H6 C11 0.951 1_555 1_555 H7 C12 0.950 1_555 1_555 H8 C13 0.950 1_555 1_555 H9 C14 0.951 1_555 1_555 H10 C15 0.951 1_555 1_555 H11 C17 0.950 1_555 1_555 H12 C18 0.951 1_555 1_555 H13 C19 0.949 1_555 1_555 H14 C20 0.951 1_555 1_555 H15 C21 0.950 1_555 1_555 O1A Na1 2.470 1_555 1_555 O2A Na1 2.431 1_555 1_555 O3A Na1 2.304 1_555 1_555 C1A O1A 1.385 1_555 1_555 C2A O2A 1.377 1_555 1_555 C3A O3A 1.352 1_555 1_555 S1A C1A 1.615 1_555 1_555 C4A C1A 1.485 1_555 1_555 S2A C2A 1.599 1_555 1_555 C10A C2A 1.476 1_555 1_555 S3A C3A 1.596 1_555 1_555 C16A C3A 1.486 1_555 1_555 Cd1A S1A 2.485 1_555 1_555 C5A C4A 1.385 1_555 1_555 C9A C4A 1.384 1_555 1_555 C11A C10A 1.406 1_555 1_555 C15A C10A 1.361 1_555 1_555 C17A C16A 1.376 1_555 1_555 C21A C16A 1.399 1_555 1_555 C6A C5A 1.399 1_555 1_555 H1A C5A 0.950 1_555 1_555 C8A C9A 1.410 1_555 1_555 H5A C9A 0.950 1_555 1_555 C12A C11A 1.361 1_555 1_555 H6A C11A 0.951 1_555 1_555 C14A C15A 1.357 1_555 1_555 H10A C15A 0.951 1_555 1_555 C18A C17A 1.407 1_555 1_555 H11A C17A 0.950 1_555 1_555 C20A C21A 1.384 1_555 1_555 H15A C21A 0.950 1_555 1_555 C7A C6A 1.368 1_555 1_555 H2A C6A 0.950 1_555 1_555 H4A C8A 0.950 1_555 1_555 C13A C12A 1.351 1_555 1_555 H7A C12A 0.950 1_555 1_555 H9A C14A 0.951 1_555 1_555 C19A C18A 1.356 1_555 1_555 H12A C18A 0.951 1_555 1_555 H14A C20A 0.951 1_555 1_555 H3A C7A 0.949 1_555 1_555 H8A C13A 0.950 1_555 1_555 H13A C19A 0.949 1_555 1_555 O2 C2 1.377 1_555 1_555 O3 C3 1.352 1_555 1_555 C14 C15 1.357 1_555 1_555 C20 C21 1.384 1_555 1_555 S2A Cd1A 2.494 1_555 1_555 S3A Cd1A 2.522 1_555 1_555 C8A C7A 1.411 1_555 1_555 C14A C13A 1.376 1_555 1_555 C20A C19A 1.354 1_555 1_555 #END data_CSD_CIF_KIPDOC _audit_creation_date 1991-09-27 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD KIPDOC _database_code_depnum_ccdc_archive 'CCDC 1197273' _database_code_depnum_ccdc_fiz 'CSD 54821' _chemical_formula_sum 'C22 H43 Cl4 Mo1 N3 Na2 O12' _chemical_formula_moiety ; C12 H23 N1 Na1 O5 1+,C10 H20 Cl4 Mo1 N2 Na1 O7 1- ; _journal_coden_Cambridge 29 _journal_volume 592 _journal_year 1991 _journal_page_first 59 _journal_name_full 'Z.Anorg.Allg.Chem. ' loop_ _publ_author_name "E.Rentschler" "W.Massa" "S.Vogler" "K.Dehnicke" "D.Fenske" "G.Baum" _chemical_name_systematic ; Acetonitrile-(15-crown-5)-sodium bis(\m~2~-chloro)-(15-crown-5)-dichloro-dinitrosyl-molybdenum-sodium ; _cell_volume 1758.376 _exptl_crystal_colour 'blue green' _exptl_crystal_density_diffrn 1.55 _exptl_special_details ; z(O6) is -0.0753 not -0.7753 ; _diffrn_ambient_temperature 263.15 _refine_special_details ; The structure is disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.033 _refine_ls_wR_factor_gt 0.033 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,-z _cell_length_a 9.843(5) _cell_length_b 12.511(6) _cell_length_c 14.830(7) _cell_angle_alpha 90 _cell_angle_beta 105.67(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Cl 0.99 Mo 1.47 N 0.68 Na 1.56 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Mo1 Mo 0.44286(5) 0.53261 0.26187(3) Cl1 Cl 0.5601(2) 0.5110(2) 0.1343(1) Cl2 Cl 0.2666(2) 0.6464(2) 0.1524(1) Cl3 Cl 0.2883(2) 0.3795(2) 0.1961(1) Cl4 Cl 0.6161(2) 0.4066(2) 0.3569(2) Na1 Na 0.2892(2) 0.5170(3) -0.0075(2) O1 O 0.3346(6) 0.6886(4) -0.0753(3) O2 O 0.4321(5) 0.4991(4) -0.1334(3) O3 O 0.3278(7) 0.3291(4) -0.0551(4) O4 O 0.0600(6) 0.6225(4) -0.0812(4) O5 O 0.3008(5) 0.5721(4) 0.4071(4) O6 O 0.6228(7) 0.7209(5) 0.3333(4) O7 O 0.060(2) 0.400(2) -0.067(1) N1 N 0.3531(5) 0.5535(4) 0.3552(3) N2 N 0.5543(5) 0.6445(5) 0.3059(3) C1 C 0.404(1) 0.6861(6) -0.1481(6) C2 C 0.5096(9) 0.5977(7) -0.1258(6) C3 C 0.517(1) 0.4056(7) -0.1051(6) C4 C 0.420(1) 0.3133(7) -0.1137(6) C5 C 0.207(1) 0.2618(7) -0.0752(7) C6 C 0.089(1) 0.3038(8) -0.0444(7) C7 C -0.055(1) 0.4572(8) -0.0678(7) C8 C -0.0620(8) 0.5594(8) -0.1196(6) C9 C 0.0831(9) 0.7064(7) -0.1382(6) C10 C 0.218(1) 0.7586(6) -0.0907(6) H1 H 0.337(1) 0.6731(6) -0.2074(6) H2 H 0.451(1) 0.7530(6) -0.1503(6) H3 H 0.5693(9) 0.6059(7) -0.0632(6) H4 H 0.5664(9) 0.5978(7) -0.1692(6) H5 H 0.579(1) 0.3962(7) -0.1446(6) H6 H 0.5271(1) 0.4128(7) -0.0412(6) H7 H 0.475(1) 0.2494(7) -0.0953(6) H8 H 0.365(1) 0.3069(7) -0.1776(6) H9 H 0.178(1) 0.2533(7) -0.1420(7) H10 H 0.234(1) 0.1935(7) -0.0463(7) H11 H -0.1446(8) 0.5978(8) -0.1157(6) H12 H -0.0670(8) 0.5458(8) -0.1842(6) H13 H 0.0887(9) 0.6787(7) -0.1975(6) H14 H 0.00732(9) 0.7571(7) -0.1480(6) H15 H 0.210(1) 0.7840(6) -0.0311(6) H16 H 0.233(1) 0.8179(6) -0.1276(6) Na2 Na 0.8342(3) 0.5531(2) 0.5275(2) O8 O 0.7110(5) 0.4684(4) 0.6371(4) O9 O 0.9520(5) 0.3914(4) 0.6097(3) O10 O 1.0912(5) 0.5817(4) 0.6215(4) O11 O 0.9075(5) 0.7429(4) 0.5584(3) O12 O 0.6387(5) 0.6641(4) 0.5476(3) N3 N 0.9187(6) 0.5589(5) 0.3859(4) C11 C 0.7249(9) 0.3561(6) 0.6260(6) C12 C 0.8785(8) 0.3306(6) 0.6622(5) C13 C 1.0978(8) 0.3961(7) 0.6544(6) C14 C 1.1605(8) 0.4842(6) 0.6109(6) C15 C 1.1379(8) 0.6688(6) 0.5799(5) C16 C 1.0515(7) 0.7639(6) 0.5967(5) C17 C 0.8219(8) 0.7976(6) 0.6025(5) C18 C 0.6724(8) 0.7760(6) 0.5519(5) C19 C 0.5772(8) 0.6268(6) 0.6178(6) C20 C 0.5712(8) 0.5075(6) 0.6126(6) C21 C 0.9364(6) 0.5463(6) 0.3141(5) C22 C 0.9602(7) 0.5295(9) 0.2241(4) H17 H 0.6715(9) 0.3184(6) 0.6613(6) H18 H 0.6916(9) 0.3368(6) 0.5611(6) H19 H 0.8934(8) 0.2556(6) 0.6547(5) H20 H 0.9108(8) 0.3493(6) 0.7272(5) H21 H 1.1124(8) 0.4107(7) 0.7199(6) H22 H 1.1409(8) 0.3291(7) 0.63469(6) H23 H 1.1470(8) 0.4697(6) 0.5455(6) H24 H 1.2596(8) 0.4896(6) 0.6412(6) H25 H 1.2366(8) 0.6813(6) 0.6076(5) H26 H 1.1216(8) 0.6570(6) 0.5138(5) H27 H 1.0775(7) 0.8269(6) 0.5683(5) H28 H 1.0695(7) 0.7750(6) 0.6630(5) H29 H 0.8400(8) 0.7737(6) 0.6661(5) H30 H 0.8401(8) 0.8729(6) 0.6016(5) H31 H 0.6550(8) 0.8028(6) 0.4892(5) H32 H 0.6122(8) 0.8121(6) 0.5833(5) H33 H 0.6343(8) 0.6484(6) 0.6783(6) H34 H 0.4839(8) 0.6555(6) 0.6078(6) H35 H 0.5237(8) 0.4857(6) 0.5500(6) H36 H 0.5214(8) 0.4802(6) 0.6551(6) H37 H 0.8667(7) 0.5066(9) 0.1925(4) H38 H 1.0226(7) 0.45692(9) 0.2341(4) H39 H 0.9910(7) 0.5816(9) 0.1864(4) O13? O 0.068(1) 0.407(1) -0.0932(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mo1 Cl1 2.483 1_555 1_555 Cl1 Na1 2.917 1_555 1_555 Cl2 Mo1 2.480 1_555 1_555 Cl3 Mo1 2.477 1_555 1_555 Cl4 Mo1 2.466 1_555 1_555 Na1 Cl2 2.929 1_555 1_555 O1 Na1 2.462 1_555 1_555 O2 Na1 2.633 1_555 1_555 O3 Na1 2.513 1_555 1_555 O4 Na1 2.587 1_555 1_555 O5 N1 1.061 1_555 1_555 O6 N2 1.177 1_555 1_555 O7 Na1 2.634 1_555 1_555 N1 Mo1 1.851 1_555 1_555 N2 Mo1 1.789 1_555 1_555 C1 O1 1.425 1_555 1_555 C2 O2 1.439 1_555 1_555 C3 O2 1.433 1_555 1_555 C4 O3 1.430 1_555 1_555 C5 O3 1.421 1_555 1_555 C6 O7 1.261 1_555 1_555 C7 O7 1.337 1_555 1_555 C8 O4 1.421 1_555 1_555 C9 O4 1.404 1_555 1_555 C10 O1 1.412 1_555 1_555 H1 C1 0.960 1_555 1_555 H2 C1 0.961 1_555 1_555 H3 C2 0.961 1_555 1_555 H4 C2 0.960 1_555 1_555 H5 C3 0.960 1_555 1_555 H6 C3 0.930 1_555 1_555 H7 C4 0.963 1_555 1_555 H8 C4 0.959 1_555 1_555 H9 C5 0.960 1_555 1_555 H10 C5 0.961 1_555 1_555 H11 C8 0.959 1_555 1_555 H12 C8 0.961 1_555 1_555 H13 C9 0.961 1_555 1_555 H14 C9 0.960 1_555 1_555 H15 C10 0.962 1_555 1_555 H16 C10 0.957 1_555 1_555 Na2 O8 2.510 1_555 1_555 O8 C11 1.425 1_555 1_555 O9 Na2 2.482 1_555 1_555 O10 Na2 2.562 1_555 1_555 O11 Na2 2.488 1_555 1_555 O12 Na2 2.456 1_555 1_555 N3 Na2 2.460 1_555 1_555 C11 C12 1.496 1_555 1_555 C12 O9 1.419 1_555 1_555 C13 O9 1.410 1_555 1_555 C14 O10 1.427 1_555 1_555 C15 O10 1.390 1_555 1_555 C16 O11 1.402 1_555 1_555 C17 O11 1.380 1_555 1_555 C18 O12 1.436 1_555 1_555 C19 O12 1.417 1_555 1_555 C20 O8 1.412 1_555 1_555 C21 N3 1.135 1_555 1_555 C22 C21 1.432 1_555 1_555 H17 C11 0.960 1_555 1_555 H18 C11 0.960 1_555 1_555 H19 C12 0.961 1_555 1_555 H20 C12 0.959 1_555 1_555 H21 C13 0.960 1_555 1_555 H22 C13 1.017 1_555 1_555 H23 C14 0.960 1_555 1_555 H24 C14 0.960 1_555 1_555 H25 C15 0.960 1_555 1_555 H26 C15 0.961 1_555 1_555 H27 C16 0.960 1_555 1_555 H28 C16 0.961 1_555 1_555 H29 C17 0.959 1_555 1_555 H30 C17 0.960 1_555 1_555 H31 C18 0.959 1_555 1_555 H32 C18 0.960 1_555 1_555 H33 C19 0.960 1_555 1_555 H34 C19 0.960 1_555 1_555 H35 C20 0.959 1_555 1_555 H36 C20 0.960 1_555 1_555 H37 C22 0.957 1_555 1_555 H38 C22 1.084 1_555 1_555 H39 C22 0.960 1_555 1_555 C1 C2 1.492 1_555 1_555 C3 C4 1.482 1_555 1_555 C5 C6 1.456 1_555 1_555 C7 C8 1.484 1_555 1_555 C9 C10 1.477 1_555 1_555 C13 C14 1.492 1_555 1_555 C15 C16 1.522 1_555 1_555 C17 C18 1.485 1_555 1_555 C19 C20 1.495 1_555 1_555 #END data_CSD_CIF_KUJFUS _audit_creation_date 2015-04-14 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD KUJFUS _database_code_depnum_ccdc_archive 'CCDC 1047001' _chemical_formula_sum 'C14 H30 K1 N2 O12 Sc1' _chemical_formula_moiety ; (C6 H6 K1 O12 Sc1 2-)n,2(C4 H12 N1 1+) ; _journal_coden_Cambridge 1147 _journal_volume 15 _journal_year 2015 _journal_page_first 2352 _journal_name_full 'Cryst.Growth Des. ' loop_ _publ_author_name "J.Cepeda" "S.Perez-Yanez" "G.Beobide" "O.Castillo" "A.Luque" "P.A.Wright" "S.Sneddon" "S.E.Ashbrook" _chemical_name_systematic ; catena-[bis(tetramethylammonium) hexakis(\m-formato)-potassium] ; _cell_volume 1162.254 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.436 _exptl_crystal_description 'trigonal antiprism' _diffrn_ambient_temperature 100 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_gt 0.0314 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 -1/2+x,-1/2-y,-1/2+z _cell_length_a 9.5369(2) _cell_length_b 9.1544(1) _cell_length_c 13.3131(2) _cell_angle_alpha 90 _cell_angle_beta 90.483(1) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 K 2.03 N 0.68 O 0.68 Sc 1.70 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Sc1 Sc 2.00000 0.00000 0.50000 K1 K 1.50000 -0.50000 0.50000 O1 O 1.81971(11) -0.11032(12) 0.45533(8) C1 C 1.75445(16) -0.22767(17) 0.47194(11) H1 H 1.80320 -0.30060 0.50610 O2 O 1.63367(12) -0.25480(12) 0.44754(8) O3 O 1.90328(11) -0.80358(11) 0.45844(7) C2 C 1.77879(17) -0.75781(17) 0.47021(11) H2 H 1.71590 -0.82180 0.50000 O4 O 1.73391(13) -0.63821(14) 0.44620(9) O5 O 1.58236(12) -0.47941(12) 0.85536(8) C3 C 1.53467(17) -0.48777(16) 0.76651(12) H3 H 1.44140 -0.51580 0.75950 O6 O 1.59753(12) -0.46320(14) 0.68947(8) N1 N 1.51360(12) -0.01459(14) 0.74939(8) C4 C 1.57517(17) -0.08087(18) 0.65723(11) H4 H 1.53220 -0.03820 0.59870 H5 H 1.55860 -0.18430 0.65740 H6 H 1.67430 -0.06270 0.65640 C5 C 1.35846(16) -0.0362(2) 0.74770(12) H7 H 1.31840 0.00770 0.80630 H8 H 1.33780 -0.13890 0.74710 H9 H 1.31940 0.00860 0.68860 C6 C 1.57458(17) -0.08562(18) 0.84072(11) H10 H 1.67390 -0.06890 0.84290 H11 H 1.55660 -0.18870 0.83830 H12 H 1.53240 -0.04490 0.89960 C7 C 1.54646(18) 0.14454(17) 0.75210(11) H13 H 1.50640 0.18730 0.81110 H14 H 1.50780 0.19090 0.69340 H15 H 1.64630 0.15790 0.75350 O1B O 1.18029(11) -0.88968(12) 0.54467(8) C1B C 1.24555(16) -0.77233(17) 0.52806(11) H1B H 1.19680 -0.69940 0.49390 O2B O 1.36633(12) -0.74520(12) 0.55246(8) O3B O 1.09672(11) -0.19642(11) 0.54156(7) C2B C 1.22121(17) -0.24219(17) 0.52979(11) H2B H 1.28410 -0.17820 0.50000 O4B O 1.26609(13) -0.36179(14) 0.55380(9) O5B O 1.41764(12) -0.52059(12) 0.14464(8) C3B C 1.46533(17) -0.51223(16) 0.23349(12) H3B H 1.55860 -0.48420 0.24050 O6B O 1.40247(12) -0.53680(14) 0.31053(8) Sc1* Sc 1.00000 -1.00000 0.50000 Sc1** Sc 1.00000 0.00000 0.50000 Sc1*** Sc 2.00000 -1.00000 0.50000 Sc1A Sc 1.50000 -0.50000 0.00000 Sc1A* Sc 1.50000 -0.50000 1.00000 O1B* O 2.18029(11) 0.11032(12) 0.54467(8) O3* O 1.90328(11) 0.19642(11) 0.45844(7) O3B* O 2.09672(11) -0.19642(11) 0.54156(7) O5A O 1.91764(12) 0.02059(12) 0.64464(8) O5C O 2.08236(12) -0.02059(12) 0.35536(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Sc1 O1 2.077 1_555 1_555 K1 O2 2.677 1_555 1_555 O1 C1 1.262 1_555 1_555 C1 H1 0.930 1_555 1_555 O2 C1 1.220 1_555 1_555 O3 C2 1.270 1_555 1_555 C2 H2 0.930 1_555 1_555 O4 K1 2.668 1_555 1_555 O5 C3 1.266 1_555 1_555 C3 H3 0.930 1_555 1_555 O6 K1 2.702 1_555 1_555 N1 C4 1.493 1_555 1_555 C4 H4 0.960 1_555 1_555 H5 C4 0.960 1_555 1_555 H6 C4 0.960 1_555 1_555 C5 N1 1.493 1_555 1_555 H7 C5 0.960 1_555 1_555 H8 C5 0.961 1_555 1_555 H9 C5 0.960 1_555 1_555 C6 N1 1.492 1_555 1_555 H10 C6 0.960 1_555 1_555 H11 C6 0.960 1_555 1_555 H12 C6 0.959 1_555 1_555 C7 N1 1.490 1_555 1_555 H13 C7 0.960 1_555 1_555 H14 C7 0.960 1_555 1_555 H15 C7 0.960 1_555 1_555 O1B C1B 1.262 1_555 1_555 C1B H1B 0.930 1_555 1_555 O2B K1 2.677 1_555 1_555 O3B C2B 1.270 1_555 1_555 C2B H2B 0.930 1_555 1_555 O4B K1 2.668 1_555 1_555 O5B C3B 1.266 1_555 1_555 C3B H3B 0.930 1_555 1_555 O6B K1 2.702 1_555 1_555 Sc1* O1B 2.077 1_555 1_555 Sc1** O3B 2.093 1_555 1_555 Sc1*** O3 2.093 1_555 1_555 Sc1A O5B 2.094 1_555 1_555 Sc1A* O5 2.094 1_555 1_555 O1B* Sc1 2.077 1_555 1_555 O3* Sc1 2.093 1_555 1_555 O3B* Sc1 2.093 1_555 1_555 O5A Sc1 2.094 1_555 1_555 O5C Sc1 2.094 1_555 1_555 C2 O4 1.217 1_555 1_555 C3 O6 1.213 1_555 1_555 C1B O2B 1.220 1_555 1_555 C2B O4B 1.217 1_555 1_555 C3B O6B 1.213 1_555 1_555 #END data_CSD_CIF_LAHBUR _audit_creation_date 1993-10-28 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD LAHBUR _chemical_formula_sum 'C72 H100 N2 Na2 O6 V2' _chemical_formula_moiety ; C54 H66 N2 Na1 V2 1-,C12 H28 Na1 O6 1+,C6 H6 ; _journal_coden_Cambridge 179 _journal_volume 32 _journal_year 1993 _journal_page_first 396 _journal_name_full 'Angew.Chem.,Int.Ed. ' loop_ _publ_author_name "R.Ferguson" "E.Solari" "C.Floriani" "A.Chiesi-Villa" "C.Rizzoli" _chemical_name_systematic ; bis(Diglyme)-sodium (\m~3~-\h^2^-dinitrogen)-(\m~2~-\h^2^,\h^3^-dimesityl-sodium)-bis(dimesityl-va nadium) benzene solvate ; _cell_volume 7345.596 _exptl_crystal_colour 'red' _exptl_crystal_density_diffrn 1.119 _exptl_special_details ; Absolute configuration ; _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; _refine_special_details ; The sodium atom is disordered over two positions. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.081 _refine_ls_wR_factor_gt 0.081 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_Int_Tables_number 20 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,z 3 x,-y,-z 4 1/2+x,1/2-y,-z 5 -x,y,1/2-z 6 1/2-x,1/2+y,1/2-z 7 -x,-y,1/2+z 8 1/2-x,1/2-y,1/2+z _cell_length_a 11.823(4) _cell_length_b 21.651(2) _cell_length_c 28.696(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.64 H 0.23 N 0.68 Na 1.56 O 0.68 V 1.33 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z V1 V -0.0183(4) -0.2226(2) -0.1667(1) Na1 Na -0.0572(16) -0.1134(9) -0.2486(11) Na2 Na -0.1785(14) -0.50000 0.00000 O1 O -0.0363(43) -0.5684(15) -0.0364(12) O2 O -0.1667(39) -0.5957(14) 0.0398(10) O3 O -0.3223(29) -0.5115(17) 0.0566(10) N1 N -0.0088(26) -0.2250(8) -0.2280(5) C1 C -0.1907(13) -0.2413(9) -0.1502(7) C2 C -0.2201(13) -0.2277(9) -0.1043(7) C3 C -0.3293(13) -0.2397(9) -0.0884(7) C4 C -0.4092(13) -0.2655(9) -0.1185(7) C5 C -0.3798(13) -0.2791(9) -0.1644(7) C6 C -0.2705(13) -0.2670(9) -0.1803(7) C7 C -0.1398(31) -0.2000(17) -0.0724(13) C8 C -0.5238(46) -0.2806(22) -0.1012(15) C9 C -0.2523(26) -0.2854(14) -0.2296(9) C10 C 0.0820(13) -0.2868(8) -0.1255(6) C11 C 0.0823(13) -0.3478(8) -0.1413(6) C12 C 0.1445(13) -0.3926(8) -0.1176(6) C13 C 0.2063(13) -0.3765(8) -0.0780(6) C14 C 0.2060(13) -0.3156(8) -0.0622(6) C15 C 0.1439(13) -0.2708(8) -0.0859(6) C16 C 0.0131(27) -0.3689(11) -0.1806(8) C17 C 0.2825(36) -0.429(2) -0.0553(14) C18 C 0.1521(24) -0.2056(13) -0.0654(10) C19 C 0.0273(21) -0.1251(7) -0.1657(6) C20 C -0.1412(21) -0.1186(7) -0.3226(6) C21 C -0.1833(21) -0.0611(7) -0.3093(6) C22 C -0.1114(21) -0.0100(7) -0.3076(6) C23 C 0.0025(21) -0.0165(7) -0.3193(6) C24 C -0.0445(21) -0.0740(7) -0.1673(6) C25 C -0.2355(31) -0.1615(16) -0.3261(13) C26 C -0.1398(38) 0.0552(19) -0.2918(14) C27 C -0.1550(29) -0.0807(15) -0.1553(11) C28 C -0.0133(63) -0.5612(26) -0.0785(19) C29 C -0.0267(64) -0.6153(28) -0.0158(24) C30 C -0.0811(40) -0.6300(19) 0.0240(18) C31 C -0.2190(57) -0.6005(28) 0.0737(22) C32 C -0.3038(67) -0.5647(36) 0.0796(23) C33 C -0.4092(43) -0.4737(24) 0.0585(17) C34 C 0.00000 -0.5279(20) -0.25000 C35 C 0.0531(26) -0.5566(13) -0.2149(10) C36 C 0.0509(25) -0.6251(13) -0.2139(10) C37 C 0.00000 -0.6523(19) -0.25000 H1 H -0.34880 -0.22770 -0.05440 H2 H -0.43990 -0.29820 -0.18620 H3 H -0.15480 -0.18760 -0.03580 H4 H -0.06730 -0.22920 -0.06840 H5 H -0.10560 -0.15670 -0.08470 H6 H -0.59710 -0.30270 -0.11930 H7 H -0.52480 -0.31370 -0.07000 H8 H -0.57260 -0.24230 -0.08450 H9 H -0.16790 -0.27870 -0.24370 H10 H -0.26070 -0.33580 -0.23230 H11 H -0.30670 -0.26690 -0.25330 H12 H 0.14510 -0.43850 -0.12840 H13 H 0.25630 -0.30340 -0.03300 H14 H 0.00990 -0.41570 -0.19340 H15 H -0.07290 -0.35990 -0.17300 H16 H 0.03480 -0.34360 -0.21020 H17 H 0.32800 -0.41580 -0.02290 H18 H 0.22520 -0.46250 -0.04180 H19 H 0.33740 -0.44570 -0.07650 H20 H 0.11630 -0.17390 -0.08240 H21 H 0.13710 -0.20830 -0.03010 H22 H 0.24830 -0.19560 -0.06630 H23 H -0.26510 -0.04890 -0.30180 H24 H 0.06580 0.02040 -0.31860 H25 H -0.32310 -0.15560 -0.31600 H26 H -0.23820 -0.17820 -0.35830 H27 H -0.21280 -0.19850 -0.30210 H28 H -0.10380 0.09570 -0.28920 H29 H -0.22700 0.07060 -0.31200 H30 H -0.19100 0.05190 -0.25640 H31 H -0.19890 -0.12190 -0.14400 H32 H -0.17920 -0.04960 -0.12370 H33 H -0.22110 -0.06120 -0.17970 H34 H -0.03060 -0.52070 -0.09830 H35 H -0.05600 -0.59440 -0.09500 H36 H 0.07050 -0.56440 -0.07840 H37 H 0.06160 -0.61380 0.00170 H38 H -0.02800 -0.65640 -0.03160 H39 H -0.02830 -0.63050 0.05400 H40 H -0.11970 -0.67150 0.02040 H41 H -0.18100 -0.60230 0.10400 H42 H -0.26510 -0.64700 0.06990 H43 H -0.30730 -0.55570 0.11300 H44 H -0.37820 -0.59050 0.06880 H45 H -0.42330 -0.42970 0.04170 H46 H -0.42480 -0.46360 0.09270 H47 H -0.47670 -0.49930 0.04450 H48 H 0.00020 -0.47970 -0.25000 H49 H 0.09880 -0.53230 -0.18410 H50 H 0.09190 -0.65370 -0.18700 H51 H 0.00010 -0.69930 -0.25010 Na1D Na 0.0572(16) -0.1134(9) -0.2514(11) N1D N 0.0088(26) -0.2250(8) -0.2720(5) V1D V 0.0183(4) -0.2226(2) -0.3333(1) C1D C 0.1907(13) -0.2413(9) -0.3498(7) C2D C 0.2201(13) -0.2277(9) -0.3957(7) C3D C 0.3293(13) -0.2397(9) -0.4116(7) C4D C 0.4092(13) -0.2655(9) -0.3815(7) C5D C 0.3798(13) -0.2791(9) -0.3356(7) C6D C 0.2705(13) -0.2670(9) -0.3197(7) C9D C 0.2523(26) -0.2854(14) -0.2704(9) H9D H 0.16790 -0.27870 -0.25630 H10D H 0.26070 -0.33580 -0.26770 H11D H 0.30670 -0.26690 -0.24670 H2D H 0.43990 -0.29820 -0.31380 C8D C 0.5238(46) -0.2806(22) -0.3988(15) H6D H 0.59710 -0.30270 -0.38070 H7D H 0.52480 -0.31370 -0.43000 H8D H 0.57260 -0.24230 -0.41550 H1D H 0.34880 -0.22770 -0.44560 C7D C 0.1398(31) -0.2000(17) -0.4276(13) H3D H 0.15480 -0.18760 -0.46420 H4D H 0.06730 -0.22920 -0.43160 H5D H 0.10560 -0.15670 -0.41530 C10D C -0.0820(13) -0.2868(8) -0.3745(6) C11D C -0.0823(13) -0.3478(8) -0.3587(6) C12D C -0.1445(13) -0.3926(8) -0.3824(6) C13D C -0.2063(13) -0.3765(8) -0.4220(6) C14D C -0.2060(13) -0.3156(8) -0.4378(6) C15D C -0.1439(13) -0.2708(8) -0.4141(6) C18D C -0.1521(24) -0.2056(13) -0.4346(10) H20D H -0.11630 -0.17390 -0.41760 H21D H -0.13710 -0.20830 -0.46990 H22D H -0.24830 -0.19560 -0.43370 H13D H -0.25630 -0.30340 -0.46700 C17D C -0.2825(36) -0.429(2) -0.4447(14) H17D H -0.32800 -0.41580 -0.47710 H18D H -0.22520 -0.46250 -0.45820 H19D H -0.33740 -0.44570 -0.42350 H12D H -0.14510 -0.43850 -0.37160 C16D C -0.0131(27) -0.3689(11) -0.3194(8) H14D H -0.00990 -0.41570 -0.30660 H15D H 0.07290 -0.35990 -0.32700 H16D H -0.03480 -0.34360 -0.28980 C19D C -0.0273(21) -0.1251(7) -0.3343(6) C20D C 0.1412(21) -0.1186(7) -0.1774(6) C24D C 0.0445(21) -0.0740(7) -0.3327(6) C21D C 0.1833(21) -0.0611(7) -0.1907(6) C25D C 0.2355(31) -0.1615(16) -0.1739(13) H25D H 0.32310 -0.15560 -0.18400 H26D H 0.23820 -0.17820 -0.14170 H27D H 0.21280 -0.19850 -0.19790 C22D C 0.1114(21) -0.0100(7) -0.1924(6) C23D C -0.0025(21) -0.0165(7) -0.1807(6) H24D H -0.06580 0.02040 -0.18140 C26D C 0.1398(38) 0.0552(19) -0.2082(14) H28D H 0.10380 0.09570 -0.21080 H29D H 0.22700 0.07060 -0.18800 H30D H 0.19100 0.05190 -0.24360 H23D H 0.26510 -0.04890 -0.19820 C27D C 0.1550(29) -0.0807(15) -0.3447(11) H31D H 0.19890 -0.12190 -0.35600 H32D H 0.17920 -0.04960 -0.37630 H33D H 0.22110 -0.06120 -0.32030 O1B O -0.0363(43) -0.4316(15) 0.0364(12) C28B C -0.0133(63) -0.4388(26) 0.0785(19) H34B H -0.03060 -0.47930 0.09830 H35B H -0.05600 -0.40560 0.09500 H36B H 0.07050 -0.43560 0.07840 C29B C -0.0267(64) -0.3847(28) 0.0158(24) C30B C -0.0811(40) -0.3700(19) -0.0240(18) O2B O -0.1667(39) -0.4043(14) -0.0398(10) O3B O -0.3223(29) -0.4885(17) -0.0566(10) C32B C -0.3038(67) -0.4353(36) -0.0796(23) C31B C -0.2190(57) -0.3995(28) -0.0737(22) H41B H -0.18100 -0.39770 -0.10400 H42B H -0.26510 -0.35300 -0.06990 H43B H -0.30730 -0.44430 -0.11300 H44B H -0.37820 -0.40950 -0.06880 C33B C -0.4092(43) -0.5263(24) -0.0585(17) H45B H -0.42330 -0.57030 -0.04170 H46B H -0.42480 -0.53640 -0.09270 H47B H -0.47670 -0.50070 -0.04450 H39B H -0.02830 -0.36950 -0.05400 H40B H -0.11970 -0.32850 -0.02040 H37B H 0.06160 -0.38620 -0.00170 H38B H -0.02800 -0.34360 0.03160 C36D C -0.0509(25) -0.6251(13) -0.2861(10) C35D C -0.0531(26) -0.5566(13) -0.2851(10) H49D H -0.09880 -0.53230 -0.31590 H50D H -0.09190 -0.65370 -0.31300 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 V1 N1 1.763 1_555 1_555 Na1 N1 2.552 1_555 1_555 Na2 O1 2.472 1_555 1_555 O1 C28 1.248 1_555 1_555 O2 Na2 2.370 1_555 1_555 O3 Na2 2.364 1_555 1_555 N1 Na1D 2.626 1_555 1_555 C1 V1 2.131 1_555 1_555 C2 C1 1.394 1_555 1_555 C3 C2 1.394 1_555 1_555 C4 C3 1.397 1_555 1_555 C5 C4 1.394 1_555 1_555 C6 C1 1.395 1_555 1_555 C7 C2 1.449 1_555 1_555 C8 C4 1.480 1_555 1_555 C9 C6 1.485 1_555 1_555 C10 V1 2.176 1_555 1_555 C11 C10 1.396 1_555 1_555 C12 C11 1.394 1_555 1_555 C13 C12 1.395 1_555 1_555 C14 C13 1.394 1_555 1_555 C15 C10 1.395 1_555 1_555 C16 C11 1.466 1_555 1_555 C17 C13 1.590 1_555 1_555 C18 C15 1.532 1_555 1_555 C19 V1 2.179 1_555 1_555 C20 Na1 2.347 1_555 1_555 C21 Na1 2.557 1_555 1_555 C22 C21 1.396 1_555 1_555 C23 C22 1.395 1_555 1_555 C24 Na1 2.489 1_555 1_555 C25 C20 1.455 1_555 1_555 C26 C22 1.520 1_555 1_555 C27 C24 1.359 1_555 1_555 C28 H34 1.065 1_555 1_555 C29 O1 1.180 1_555 1_555 C30 O2 1.335 1_555 1_555 C31 O2 1.157 1_555 1_555 C32 O3 1.345 1_555 1_555 C33 O3 1.315 1_555 1_555 C34 C35 1.340 1_555 1_555 C35 C36 1.484 1_555 1_555 C36 C37 1.335 1_555 1_555 C37 H51 1.018 1_555 1_555 H1 C3 1.036 1_555 1_555 H2 C5 1.033 1_555 1_555 H3 C7 1.098 1_555 1_555 H4 C7 1.071 1_555 1_555 H5 C7 1.080 1_555 1_555 H6 C8 1.118 1_555 1_555 H7 C8 1.147 1_555 1_555 H8 C8 1.118 1_555 1_555 H9 C9 1.086 1_555 1_555 H10 C9 1.098 1_555 1_555 H11 C9 1.018 1_555 1_555 H12 C12 1.041 1_555 1_555 H13 C14 1.061 1_555 1_555 H14 C16 1.078 1_555 1_555 H15 C16 1.058 1_555 1_555 H16 C16 1.043 1_555 1_555 H17 C17 1.112 1_555 1_555 H18 C17 1.065 1_555 1_555 H19 C17 0.960 1_555 1_555 H20 C18 0.942 1_555 1_555 H21 C18 1.030 1_555 1_555 H22 C18 1.158 1_555 1_555 H23 C21 1.025 1_555 1_555 H24 C23 1.095 1_555 1_555 H25 C25 1.083 1_555 1_555 H26 C25 0.993 1_555 1_555 H27 C25 1.090 1_555 1_555 H28 C26 0.978 1_555 1_555 H29 C26 1.229 1_555 1_555 H30 C26 1.185 1_555 1_555 H31 C27 1.082 1_555 1_555 H32 C27 1.165 1_555 1_555 H33 C27 1.131 1_555 1_555 H35 C28 0.998 1_555 1_555 H36 C28 0.993 1_555 1_555 H37 C29 1.159 1_555 1_555 H38 C29 0.999 1_555 1_555 H39 C30 1.063 1_555 1_555 H40 C30 1.013 1_555 1_555 H41 C31 0.979 1_555 1_555 H42 C31 1.150 1_555 1_555 H43 C32 0.979 1_555 1_555 H44 C32 1.087 1_555 1_555 H45 C33 1.081 1_555 1_555 H46 C33 1.022 1_555 1_555 H47 C33 1.051 1_555 1_555 H48 C34 1.044 1_555 1_555 H49 C35 1.162 1_555 1_555 H50 C36 1.102 1_555 1_555 Na1D Na1 1.355 1_555 1_555 N1D Na1 2.626 1_555 1_555 V1D N1D 1.763 1_555 1_555 C1D V1D 2.131 1_555 1_555 C2D C1D 1.394 1_555 1_555 C3D C2D 1.394 1_555 1_555 C4D C3D 1.397 1_555 1_555 C5D C4D 1.394 1_555 1_555 C6D C1D 1.395 1_555 1_555 C9D C6D 1.485 1_555 1_555 H9D C9D 1.086 1_555 1_555 H10D C9D 1.098 1_555 1_555 H11D C9D 1.018 1_555 1_555 H2D C5D 1.033 1_555 1_555 C8D C4D 1.480 1_555 1_555 H6D C8D 1.118 1_555 1_555 H7D C8D 1.147 1_555 1_555 H8D C8D 1.118 1_555 1_555 H1D C3D 1.036 1_555 1_555 C7D C2D 1.449 1_555 1_555 H3D C7D 1.098 1_555 1_555 H4D C7D 1.071 1_555 1_555 H5D C7D 1.080 1_555 1_555 C10D V1D 2.176 1_555 1_555 C11D C10D 1.396 1_555 1_555 C12D C11D 1.394 1_555 1_555 C13D C12D 1.395 1_555 1_555 C14D C13D 1.394 1_555 1_555 C15D C10D 1.395 1_555 1_555 C18D C15D 1.532 1_555 1_555 H20D C18D 0.942 1_555 1_555 H21D C18D 1.030 1_555 1_555 H22D C18D 1.158 1_555 1_555 H13D C14D 1.061 1_555 1_555 C17D C13D 1.590 1_555 1_555 H17D C17D 1.112 1_555 1_555 H18D C17D 1.065 1_555 1_555 H19D C17D 0.960 1_555 1_555 H12D C12D 1.041 1_555 1_555 C16D C11D 1.466 1_555 1_555 H14D C16D 1.078 1_555 1_555 H15D C16D 1.058 1_555 1_555 H16D C16D 1.043 1_555 1_555 C19D Na1 2.497 1_555 1_555 C20D C19 1.395 1_555 1_555 C24D C23 1.394 1_555 1_555 C21D Na1D 2.557 1_555 1_555 C25D C20D 1.455 1_555 1_555 H25D C25D 1.083 1_555 1_555 H26D C25D 0.993 1_555 1_555 H27D C25D 1.090 1_555 1_555 C22D C21D 1.396 1_555 1_555 C23D C24 1.394 1_555 1_555 H24D C23D 1.095 1_555 1_555 C26D C22D 1.520 1_555 1_555 H28D C26D 0.978 1_555 1_555 H29D C26D 1.229 1_555 1_555 H30D C26D 1.185 1_555 1_555 H23D C21D 1.025 1_555 1_555 C27D C24D 1.359 1_555 1_555 H31D C27D 1.082 1_555 1_555 H32D C27D 1.165 1_555 1_555 H33D C27D 1.131 1_555 1_555 O1B Na2 2.472 1_555 1_555 C28B O1B 1.248 1_555 1_555 H34B C28B 1.065 1_555 1_555 H35B C28B 0.998 1_555 1_555 H36B C28B 0.993 1_555 1_555 C29B O1B 1.180 1_555 1_555 C30B C29B 1.349 1_555 1_555 O2B Na2 2.370 1_555 1_555 O3B Na2 2.364 1_555 1_555 C32B O3B 1.345 1_555 1_555 C31B O2B 1.157 1_555 1_555 H41B C31B 0.979 1_555 1_555 H42B C31B 1.150 1_555 1_555 H43B C32B 0.979 1_555 1_555 H44B C32B 1.087 1_555 1_555 C33B O3B 1.315 1_555 1_555 H45B C33B 1.081 1_555 1_555 H46B C33B 1.022 1_555 1_555 H47B C33B 1.051 1_555 1_555 H39B C30B 1.063 1_555 1_555 H40B C30B 1.013 1_555 1_555 H37B C29B 1.159 1_555 1_555 H38B C29B 0.999 1_555 1_555 C36D C37 1.335 1_555 1_555 C35D C34 1.340 1_555 1_555 H49D C35D 1.162 1_555 1_555 H50D C36D 1.102 1_555 1_555 Na1 C19 2.593 1_555 1_555 N1 N1D 1.280 1_555 1_555 C5 C6 1.395 1_555 1_555 C14 C15 1.394 1_555 1_555 C19 C24 1.395 1_555 1_555 C19 Na1D 2.497 1_555 1_555 C20 C19D 1.395 1_555 1_555 C20 C21 1.394 1_555 1_555 C29 C30 1.349 1_555 1_555 C31 C32 1.279 1_555 1_555 Na1D N1D 2.552 1_555 1_555 Na1D C20D 2.347 1_555 1_555 Na1D C19D 2.593 1_555 1_555 Na1D C24D 2.489 1_555 1_555 V1D C19D 2.179 1_555 1_555 C5D C6D 1.395 1_555 1_555 C14D C15D 1.394 1_555 1_555 C19D C24D 1.395 1_555 1_555 C20D C21D 1.394 1_555 1_555 C22D C23D 1.395 1_555 1_555 C30B O2B 1.335 1_555 1_555 C32B C31B 1.279 1_555 1_555 C36D C35D 1.484 1_555 1_555 #END data_CSD_CIF_LAHBUR01 _audit_creation_date 1998-07-29 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD LAHBUR01 _chemical_formula_sum 'C72 H100 N2 Na2 O6 V2' _chemical_formula_moiety ; C54 H66 N2 Na1 V2 1-,C12 H28 Na1 O6 1+,C6 H6 ; _journal_coden_Cambridge 4 _journal_volume 119 _journal_year 1997 _journal_page_first 10104 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "R.Ferguson" "E.Solari" "C.Floriani" "D.Osella" "M.Ravera" "N.Re" "A.Chiesi-Villa" "C.Rizzoli" _chemical_name_systematic ; bis(Diglyme)-sodium (\m~3~-\h^2^-dinitrogen)-(\m~2~-\h^2^,\h^3^-dimesityl-sodium)-bis(dimesityl-va nadium) benzene solvate ; _cell_volume 7345.596 _exptl_crystal_colour 'red' _exptl_crystal_density_diffrn 1.119 _exptl_crystal_description 'irregular prism' _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; _refine_special_details ; One sodium atom is equally disordered over two sites. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.045 _refine_ls_wR_factor_gt 0.045 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_Int_Tables_number 20 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,1/2+z 3 x,-y,-z 4 -x,y,1/2-z 5 1/2+x,1/2+y,z 6 1/2-x,1/2-y,1/2+z 7 1/2+x,1/2-y,-z 8 1/2-x,1/2+y,1/2-z _cell_length_a 11.823(4) _cell_length_b 21.651(2) _cell_length_c 28.696(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 N 0.68 Na 1.53 O 0.68 V 1.33 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z V1 V -0.0173(2) -0.2226(1) -0.1670(1) Na1 Na -0.0581(10) -0.1147(4) -0.2470(5) Na2 Na -0.1783(6) -0.50000 0.00000 O1 O -0.0492(15) -0.5683(7) -0.0355(8) O2 O -0.1653(18) -0.5947(6) 0.0376(5) O3 O -0.3233(11) -0.5138(7) 0.0539(4) N1 N -0.0081(10) -0.2247(3) -0.2281(2) C1 C -0.1890(7) -0.2401(4) -0.1498(4) C2 C -0.219(1) -0.2265(4) -0.1041(4) C3 C -0.3276(12) -0.2395(4) -0.0883(3) C4 C -0.4061(7) -0.2662(4) -0.1182(6) C5 C -0.3762(10) -0.2798(4) -0.1639(5) C6 C -0.2676(12) -0.2667(4) -0.1797(3) C7 C -0.1403(12) -0.1992(8) -0.0717(5) C8 C -0.5266(14) -0.2801(7) -0.1029(7) C9 C -0.2484(12) -0.2849(6) -0.2296(4) C10 C 0.0802(6) -0.2879(4) -0.1259(3) C11 C 0.0826(7) -0.3491(4) -0.1407(2) C12 C 0.1466(8) -0.3923(3) -0.1164(4) C13 C 0.2082(7) -0.3744(5) -0.0775(4) C14 C 0.2059(7) -0.3132(5) -0.0627(2) C15 C 0.1419(7) -0.2700(3) -0.0870(3) C16 C 0.0172(13) -0.3688(5) -0.1815(4) C17 C 0.2787(13) -0.4265(8) -0.0542(6) C18 C 0.1514(11) -0.2079(6) -0.0645(4) C19 C 0.0284(12) -0.1245(4) -0.1646(3) C20 C -0.1409(10) -0.1157(4) -0.3229(3) C21 C -0.1782(9) -0.0575(6) -0.3095(3) C22 C -0.1032(13) -0.0081(4) -0.3085(3) C23 C 0.0093(11) -0.0169(4) -0.3210(3) C24 C -0.0466(8) -0.0751(6) -0.1656(3) C25 C -0.2296(13) -0.1618(7) -0.3235(6) C26 C -0.1466(21) 0.0546(7) -0.2922(5) C27 C -0.1627(13) -0.0822(5) -0.1559(6) C28 C -0.0054(22) -0.5582(10) -0.0805(8) C29 C -0.0198(31) -0.6134(17) -0.0242(16) C30 C -0.0729(20) -0.6281(11) 0.0212(11) C31 C -0.2267(27) -0.6039(10) 0.0743(9) C32 C -0.3172(31) -0.5630(9) 0.0779(9) C33 C -0.3986(23) -0.4714(11) 0.0614(8) C34 C 0.00000 -0.5267(8) -0.25000 C35 C 0.0534(11) -0.5575(6) -0.2170(4) C36 C 0.0540(13) -0.6239(7) -0.2141(5) C37 C 0.00000 -0.6513(9) -0.25000 H1 H -0.34880 -0.22770 -0.05440 H2 H -0.43990 -0.29820 -0.18620 H3 H -0.15480 -0.18760 -0.03580 H4 H -0.06730 -0.22920 -0.06840 H5 H -0.10560 -0.15680 -0.08470 H6 H -0.59710 -0.30270 -0.11930 H7 H -0.52480 -0.31370 -0.07000 H8 H -0.57260 -0.24230 -0.08450 H9 H -0.16790 -0.27870 -0.24370 H10 H -0.26070 -0.33580 -0.23230 H11 H -0.30670 -0.26690 -0.25330 H12 H 0.14510 -0.43850 -0.12840 H13 H 0.25630 -0.30340 -0.03300 H14 H 0.00990 -0.41570 -0.19340 H15 H -0.07290 -0.35990 -0.17300 H16 H 0.03470 -0.34360 -0.21020 H17 H 0.32800 -0.41580 -0.02290 H18 H 0.22520 -0.46250 -0.04180 H19 H 0.33740 -0.44570 -0.07650 H20 H 0.11630 -0.17390 -0.08240 H21 H 0.13710 -0.20830 -0.03010 H22 H 0.24830 -0.19560 -0.06630 H23 H -0.26510 -0.04890 -0.30180 H24 H 0.06580 0.02040 -0.31860 H25 H -0.32310 -0.15560 -0.31600 H26 H -0.23820 -0.17820 -0.35830 H27 H -0.21280 -0.19850 -0.30210 H28 H -0.10380 0.09570 -0.28920 H29 H -0.22700 0.07060 -0.31200 H30 H -0.19100 0.05190 -0.25640 H31 H -0.19890 -0.12180 -0.14400 H32 H -0.17920 -0.04960 -0.12370 H33 H -0.22120 -0.06120 -0.17970 H34 H -0.03060 -0.52070 -0.09830 H35 H -0.05600 -0.59440 -0.09500 H36 H 0.07050 -0.56440 -0.07840 H37 H 0.06160 -0.61380 0.00170 H38 H -0.02800 -0.65640 -0.03160 H39 H -0.02830 -0.63050 0.05400 H40 H -0.11970 -0.67150 0.02040 H41 H -0.18100 -0.60230 0.10400 H42 H -0.26510 -0.64700 0.06990 H43 H -0.30730 -0.55570 0.11310 H44 H -0.37820 -0.59040 0.06880 H45 H -0.42330 -0.42970 0.04170 H46 H -0.42480 -0.46360 0.09270 H47 H -0.47670 -0.49930 0.04450 H48 H 0.00000 -0.48310 -0.25000 H49 H 0.09420 -0.53330 -0.19330 H50 H 0.09010 -0.64770 -0.19000 H51 H 0.00000 -0.69590 -0.25000 Na1C Na 0.0581(10) -0.1147(4) -0.2530(5) N1C N 0.0081(10) -0.2247(3) -0.2719(2) V1C V 0.0173(2) -0.2226(1) -0.3330(1) C1C C 0.1890(7) -0.2401(4) -0.3502(4) C2C C 0.219(1) -0.2265(4) -0.3959(4) C3C C 0.3276(12) -0.2395(4) -0.4117(3) C4C C 0.4061(7) -0.2662(4) -0.3818(6) C5C C 0.3762(10) -0.2798(4) -0.3361(5) C6C C 0.2676(12) -0.2667(4) -0.3203(3) C9C C 0.2484(12) -0.2849(6) -0.2704(4) H9C H 0.16790 -0.27870 -0.25630 H10C H 0.26070 -0.33580 -0.26770 H11C H 0.30670 -0.26690 -0.24670 H2C H 0.43990 -0.29820 -0.31380 C8C C 0.5266(14) -0.2801(7) -0.3971(7) H6C H 0.59710 -0.30270 -0.38070 H7C H 0.52480 -0.31370 -0.43000 H8C H 0.57260 -0.24230 -0.41550 H1C H 0.34880 -0.22770 -0.44560 C7C C 0.1403(12) -0.1992(8) -0.4283(5) H3C H 0.15480 -0.18760 -0.46420 H4C H 0.06730 -0.22920 -0.43160 H5C H 0.10560 -0.15680 -0.41530 C10C C -0.0802(6) -0.2879(4) -0.3741(3) C11C C -0.0826(7) -0.3491(4) -0.3593(2) C12C C -0.1466(8) -0.3923(3) -0.3836(4) C13C C -0.2082(7) -0.3744(5) -0.4225(4) C14C C -0.2059(7) -0.3132(5) -0.4373(2) C15C C -0.1419(7) -0.2700(3) -0.4130(3) C18C C -0.1514(11) -0.2079(6) -0.4355(4) H20C H -0.11630 -0.17390 -0.41760 H21C H -0.13710 -0.20830 -0.46990 H22C H -0.24830 -0.19560 -0.43370 H13C H -0.25630 -0.30340 -0.46700 C17C C -0.2787(13) -0.4265(8) -0.4458(6) H17C H -0.32800 -0.41580 -0.47710 H18C H -0.22520 -0.46250 -0.45820 H19C H -0.33740 -0.44570 -0.42350 H12C H -0.14510 -0.43850 -0.37160 C16C C -0.0172(13) -0.3688(5) -0.3185(4) H14C H -0.00990 -0.41570 -0.30660 H15C H 0.07290 -0.35990 -0.32700 H16C H -0.03470 -0.34360 -0.28980 C19C C -0.0284(12) -0.1245(4) -0.3354(3) C20C C 0.1409(10) -0.1157(4) -0.1771(3) C24C C 0.0466(8) -0.0751(6) -0.3344(3) C21C C 0.1782(9) -0.0575(6) -0.1905(3) C25C C 0.2296(13) -0.1618(7) -0.1765(6) H25C H 0.32310 -0.15560 -0.18400 H26C H 0.23820 -0.17820 -0.14170 H27C H 0.21280 -0.19850 -0.19790 C22C C 0.1032(13) -0.0081(4) -0.1915(3) C23C C -0.0093(11) -0.0169(4) -0.1790(3) H24C H -0.06580 0.02040 -0.18140 C26C C 0.1466(21) 0.0546(7) -0.2078(5) H28C H 0.10380 0.09570 -0.21080 H29C H 0.22700 0.07060 -0.18800 H30C H 0.19100 0.05190 -0.24360 H23C H 0.26510 -0.04890 -0.19820 C27C C 0.1627(13) -0.0822(5) -0.3441(6) H31C H 0.19890 -0.12180 -0.35600 H32C H 0.17920 -0.04960 -0.37630 H33C H 0.22120 -0.06120 -0.32030 O1B O -0.0492(15) -0.4317(7) 0.0355(8) C28B C -0.0054(22) -0.4418(10) 0.0805(8) H34B H -0.03060 -0.47930 0.09830 H35B H -0.05600 -0.40560 0.09500 H36B H 0.07050 -0.43560 0.07840 C29B C -0.0198(31) -0.3866(17) 0.0242(16) C30B C -0.0729(20) -0.3719(11) -0.0212(11) O2B O -0.1653(18) -0.4053(6) -0.0376(5) O3B O -0.3233(11) -0.4862(7) -0.0539(4) C32B C -0.3172(31) -0.4370(9) -0.0779(9) C31B C -0.2267(27) -0.3961(10) -0.0743(9) H41B H -0.18100 -0.39770 -0.10400 H42B H -0.26510 -0.35300 -0.06990 H43B H -0.30730 -0.44430 -0.11310 H44B H -0.37820 -0.40960 -0.06880 C33B C -0.3986(23) -0.5286(11) -0.0614(8) H45B H -0.42330 -0.57030 -0.04170 H46B H -0.42480 -0.53640 -0.09270 H47B H -0.47670 -0.50070 -0.04450 H39B H -0.02830 -0.36950 -0.05400 H40B H -0.11970 -0.32850 -0.02040 H37B H 0.06160 -0.38620 -0.00170 H38B H -0.02800 -0.34360 0.03160 C36C C -0.0540(13) -0.6239(7) -0.2859(5) C35C C -0.0534(11) -0.5575(6) -0.2830(4) H49C H -0.09420 -0.53330 -0.30670 H50C H -0.09010 -0.64770 -0.31000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 V1 N1 1.757 1_555 1_555 Na1 N1 2.513 1_555 1_555 Na2 O1 2.357 1_555 1_555 O1 C28 1.408 1_555 1_555 O2 Na2 2.322 1_555 1_555 O3 Na2 2.328 1_555 1_555 N1 Na1C 2.607 1_555 1_555 C1 V1 2.123 1_555 1_555 C2 C1 1.390 1_555 1_555 C3 C2 1.390 1_555 1_555 C4 C3 1.390 1_555 1_555 C5 C4 1.390 1_555 1_555 C6 C1 1.390 1_555 1_555 C7 C2 1.442 1_555 1_555 C8 C4 1.521 1_555 1_555 C9 C6 1.502 1_555 1_555 C10 V1 2.172 1_555 1_555 C11 C10 1.392 1_555 1_555 C12 C11 1.391 1_555 1_555 C13 C12 1.388 1_555 1_555 C14 C13 1.392 1_555 1_555 C15 C10 1.389 1_555 1_555 C16 C11 1.466 1_555 1_555 C17 C13 1.554 1_555 1_555 C18 C15 1.496 1_555 1_555 C19 V1 2.193 1_555 1_555 C20 Na1 2.388 1_555 1_555 C21 Na1 2.601 1_555 1_555 C22 C21 1.390 1_555 1_555 C23 C22 1.391 1_555 1_555 C24 Na1 2.492 1_555 1_555 C25 C20 1.448 1_555 1_555 C26 C22 1.525 1_555 1_555 C27 C24 1.409 1_555 1_555 C28 H34 1.004 1_555 1_555 C29 O1 1.086 1_555 1_555 C30 O2 1.392 1_555 1_555 C31 O2 1.295 1_555 1_555 C32 O3 1.271 1_555 1_555 C33 O3 1.297 1_555 1_555 C34 C35 1.319 1_555 1_555 C35 C36 1.440 1_555 1_555 C36 C37 1.349 1_555 1_555 C37 H51 0.966 1_555 1_555 H1 C3 1.037 1_555 1_555 H2 C5 1.066 1_555 1_555 H3 C7 1.074 1_555 1_555 H4 C7 1.084 1_555 1_555 H5 C7 1.072 1_555 1_555 H6 C8 1.075 1_555 1_555 H7 C8 1.192 1_555 1_555 H8 C8 1.116 1_555 1_555 H9 C9 1.043 1_555 1_555 H10 C9 1.114 1_555 1_555 H11 C9 1.044 1_555 1_555 H12 C12 1.058 1_555 1_555 H13 C14 1.061 1_555 1_555 H14 C16 1.075 1_555 1_555 H15 C16 1.110 1_555 1_555 H16 C16 1.009 1_555 1_555 H17 C17 1.096 1_555 1_555 H18 C17 1.065 1_555 1_555 H19 C17 1.031 1_555 1_555 H20 C18 0.989 1_555 1_555 H21 C18 1.002 1_555 1_555 H22 C18 1.177 1_555 1_555 H23 C21 1.067 1_555 1_555 H24 C23 1.050 1_555 1_555 H25 C25 1.134 1_555 1_555 H26 C25 1.065 1_555 1_555 H27 C25 1.024 1_555 1_555 H28 C26 1.027 1_555 1_555 H29 C26 1.160 1_555 1_555 H30 C26 1.155 1_555 1_555 H31 C27 1.017 1_555 1_555 H32 C27 1.179 1_555 1_555 H33 C27 1.073 1_555 1_555 H35 C28 1.070 1_555 1_555 H36 C28 0.909 1_555 1_555 H37 C29 1.216 1_555 1_555 H38 C29 0.960 1_555 1_555 H39 C30 1.080 1_555 1_555 H40 C30 1.091 1_555 1_555 H41 C31 1.010 1_555 1_555 H42 C31 1.045 1_555 1_555 H43 C32 1.029 1_555 1_555 H44 C32 0.970 1_555 1_555 H45 C33 1.105 1_555 1_555 H46 C33 0.965 1_555 1_555 H47 C33 1.205 1_555 1_555 H48 C34 0.944 1_555 1_555 H49 C35 0.985 1_555 1_555 H50 C36 0.962 1_555 1_555 Na1C Na1 1.385 1_555 1_555 N1C Na1 2.607 1_555 1_555 V1C N1C 1.757 1_555 1_555 C1C V1C 2.123 1_555 1_555 C2C C1C 1.390 1_555 1_555 C3C C2C 1.390 1_555 1_555 C4C C3C 1.390 1_555 1_555 C5C C4C 1.390 1_555 1_555 C6C C1C 1.390 1_555 1_555 C9C C6C 1.502 1_555 1_555 H9C C9C 1.043 1_555 1_555 H10C C9C 1.114 1_555 1_555 H11C C9C 1.044 1_555 1_555 H2C C5C 1.066 1_555 1_555 C8C C4C 1.521 1_555 1_555 H6C C8C 1.075 1_555 1_555 H7C C8C 1.192 1_555 1_555 H8C C8C 1.116 1_555 1_555 H1C C3C 1.037 1_555 1_555 C7C C2C 1.442 1_555 1_555 H3C C7C 1.074 1_555 1_555 H4C C7C 1.084 1_555 1_555 H5C C7C 1.072 1_555 1_555 C10C V1C 2.172 1_555 1_555 C11C C10C 1.392 1_555 1_555 C12C C11C 1.391 1_555 1_555 C13C C12C 1.388 1_555 1_555 C14C C13C 1.392 1_555 1_555 C15C C10C 1.389 1_555 1_555 C18C C15C 1.496 1_555 1_555 H20C C18C 0.989 1_555 1_555 H21C C18C 1.002 1_555 1_555 H22C C18C 1.177 1_555 1_555 H13C C14C 1.061 1_555 1_555 C17C C13C 1.554 1_555 1_555 H17C C17C 1.096 1_555 1_555 H18C C17C 1.065 1_555 1_555 H19C C17C 1.031 1_555 1_555 H12C C12C 1.058 1_555 1_555 C16C C11C 1.466 1_555 1_555 H14C C16C 1.075 1_555 1_555 H15C C16C 1.110 1_555 1_555 H16C C16C 1.009 1_555 1_555 C19C Na1 2.570 1_555 1_555 C20C C19 1.391 1_555 1_555 C24C C23 1.389 1_555 1_555 C21C Na1C 2.601 1_555 1_555 C25C C20C 1.448 1_555 1_555 H25C C25C 1.134 1_555 1_555 H26C C25C 1.065 1_555 1_555 H27C C25C 1.024 1_555 1_555 C22C C21C 1.390 1_555 1_555 C23C C24 1.389 1_555 1_555 H24C C23C 1.050 1_555 1_555 C26C C22C 1.525 1_555 1_555 H28C C26C 1.027 1_555 1_555 H29C C26C 1.160 1_555 1_555 H30C C26C 1.155 1_555 1_555 H23C C21C 1.067 1_555 1_555 C27C C24C 1.409 1_555 1_555 H31C C27C 1.017 1_555 1_555 H32C C27C 1.179 1_555 1_555 H33C C27C 1.073 1_555 1_555 O1B Na2 2.357 1_555 1_555 C28B O1B 1.408 1_555 1_555 H34B C28B 1.004 1_555 1_555 H35B C28B 1.070 1_555 1_555 H36B C28B 0.909 1_555 1_555 C29B O1B 1.086 1_555 1_555 C30B C29B 1.481 1_555 1_555 O2B Na2 2.322 1_555 1_555 O3B Na2 2.328 1_555 1_555 C32B O3B 1.271 1_555 1_555 C31B O2B 1.295 1_555 1_555 H41B C31B 1.010 1_555 1_555 H42B C31B 1.045 1_555 1_555 H43B C32B 1.029 1_555 1_555 H44B C32B 0.970 1_555 1_555 C33B O3B 1.297 1_555 1_555 H45B C33B 1.105 1_555 1_555 H46B C33B 0.965 1_555 1_555 H47B C33B 1.205 1_555 1_555 H39B C30B 1.080 1_555 1_555 H40B C30B 1.091 1_555 1_555 H37B C29B 1.216 1_555 1_555 H38B C29B 0.960 1_555 1_555 C36C C37 1.349 1_555 1_555 C35C C34 1.319 1_555 1_555 H49C C35C 0.985 1_555 1_555 H50C C36C 0.962 1_555 1_555 Na1 C19 2.585 1_555 1_555 N1 N1C 1.271 1_555 1_555 C5 C6 1.391 1_555 1_555 C14 C15 1.391 1_555 1_555 C19 C24 1.390 1_555 1_555 C19 Na1C 2.570 1_555 1_555 C20 C19C 1.391 1_555 1_555 C20 C21 1.389 1_555 1_555 C29 C30 1.481 1_555 1_555 C31 C32 1.393 1_555 1_555 Na1C N1C 2.513 1_555 1_555 Na1C C20C 2.388 1_555 1_555 Na1C C19C 2.585 1_555 1_555 Na1C C24C 2.492 1_555 1_555 V1C C19C 2.193 1_555 1_555 C5C C6C 1.391 1_555 1_555 C14C C15C 1.391 1_555 1_555 C19C C24C 1.390 1_555 1_555 C20C C21C 1.389 1_555 1_555 C22C C23C 1.391 1_555 1_555 C30B O2B 1.392 1_555 1_555 C32B C31B 1.393 1_555 1_555 C36C C35C 1.440 1_555 1_555 #END data_CSD_CIF_LONYES _audit_creation_date 2000-12-08 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD LONYES _database_code_depnum_ccdc_archive 'CCDC 144780' _chemical_formula_sum 'C32 H78 Li2 O3 Si6' _chemical_formula_moiety ; C12 H24 Li1 O3 1+,C20 H54 Li1 Si6 1- ; _journal_coden_Cambridge 29 _journal_volume 626 _journal_year 2000 _journal_page_first 2040 _journal_name_full 'Z.Anorg.Allg.Chem. ' loop_ _publ_author_name "T.Viefhaus" "A.Walz" "M.Niemeyer" "W.Schwarz" "J.Weidlein" _chemical_name_systematic ; tris(Tetrahydrofuran-O)-lithium bis(tris(trimethylsilyl)methyl)-lithium ; _cell_volume 4572.938 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.007 _exptl_crystal_description 'plate' _diffrn_ambient_temperature 173 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_gt 0.0559 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 -x,1/2+y,1/2-z 4 1/2+x,1/2-y,-z _cell_length_a 13.645(3) _cell_length_b 17.168(4) _cell_length_c 19.521(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.12 O 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.1967(6) 0.8715(5) 0.2297(4) Li2 Li 0.6269(5) 0.8141(5) 0.2580(3) O1 O 0.1259(3) 0.9197(2) 0.15718(16) O2 O 0.1813(3) 0.9211(2) 0.31464(16) O3 O 0.1608(3) 0.7660(2) 0.23756(18) Si1 Si 0.49304(9) 0.90706(6) 0.15626(5) Si2 Si 0.68349(10) 0.83947(10) 0.10024(6) Si3 Si 0.51326(9) 0.73055(7) 0.13548(7) Si4 Si 0.56382(10) 0.79652(8) 0.41504(6) Si5 Si 0.75261(9) 0.71901(7) 0.36537(6) Si6 Si 0.74334(10) 0.89635(7) 0.37878(6) C1 C 0.5746(3) 0.8234(2) 0.15324(19) C2 C 0.6756(3) 0.8060(2) 0.36329(18) C3 C 0.1506(5) 0.9300(4) 0.0856(3) H1 H 0.16790 0.87950 0.06420 H2 H 0.20630 0.96640 0.08030 C4 C 0.0596(6) 0.9629(4) 0.0544(3) H3 H 0.07600 0.99910 0.01670 H4 H 0.01760 0.92070 0.03610 C5 C 0.0091(5) 1.0045(4) 0.1103(3) H5 H 0.03510 1.05800 0.11590 H6 H -0.06250 1.00720 0.10220 C6 C 0.0320(5) 0.9558(5) 0.1703(3) H7 H 0.03530 0.98810 0.21230 H8 H -0.01910 0.91550 0.17680 C7 C 0.2312(5) 0.9896(3) 0.3389(3) H9 H 0.22250 1.03340 0.30640 H10 H 0.30220 0.97930 0.34430 C8 C 0.1864(6) 1.0081(5) 0.4053(4) H11 H 0.22880 0.99030 0.44340 H12 H 0.17600 1.06500 0.40990 C9 C 0.0924(6) 0.9667(5) 0.4063(4) H13 H 0.03980 0.99850 0.38530 H14 H 0.07310 0.95280 0.45360 C10 C 0.1129(5) 0.8966(4) 0.3652(3) H15 H 0.14120 0.85490 0.39410 H16 H 0.05220 0.87690 0.34350 C11 C 0.1173(8) 0.7235(4) 0.1821(3) H17 H 0.05480 0.74840 0.16860 H18 H 0.16170 0.72410 0.14200 C12 C 0.0998(8) 0.6456(4) 0.2028(6) H19 H 0.11690 0.60880 0.16570 H20 H 0.03010 0.63810 0.21530 C13 C 0.1637(7) 0.6340(4) 0.2626(4) H21 H 0.22760 0.61190 0.24860 H22 H 0.13260 0.59830 0.29600 C14 C 0.1767(6) 0.7125(4) 0.2927(3) H23 H 0.12870 0.72140 0.32990 H24 H 0.24360 0.71850 0.31160 C15 C 0.3661(4) 0.8855(3) 0.1920(3) H25 H 0.379(4) 0.867(3) 0.236(3) H26 H 0.329(3) 0.848(3) 0.162(2) H27 H 0.335(4) 0.933(3) 0.188(2) C16 C 0.5382(4) 0.9881(3) 0.2131(3) H28 H 0.60260 1.00570 0.19710 H29 H 0.54360 0.96910 0.26030 H30 H 0.49180 1.03170 0.21150 C17 C 0.4620(4) 0.9529(3) 0.0711(2) H31 H 0.52070 0.97760 0.05190 H32 H 0.41080 0.99220 0.07750 H33 H 0.43840 0.91260 0.03950 C18 C 0.7310(4) 0.9424(4) 0.1011(3) H34 H 0.75010 0.95660 0.14780 H35 H 0.67950 0.97790 0.08510 H36 H 0.78800 0.94640 0.07070 C19 C 0.7924(4) 0.7803(4) 0.1269(3) H37 H 0.80880 0.79210 0.17470 H38 H 0.84830 0.79310 0.09750 H39 H 0.77710 0.72480 0.12250 C20 C 0.6645(4) 0.8195(5) 0.0058(2) H40 H 0.64490 0.76500 -0.00060 H41 H 0.72570 0.82930 -0.01900 H42 H 0.61290 0.85380 -0.01190 C21 C 0.4370(4) 0.6940(3) 0.2086(3) H43 H 0.47840 0.68760 0.24920 H44 H 0.40780 0.64370 0.19630 H45 H 0.38480 0.73160 0.21850 C22 C 0.4277(4) 0.7307(4) 0.0594(3) H46 H 0.46440 0.74430 0.01790 H47 H 0.37550 0.76900 0.06680 H48 H 0.39870 0.67880 0.05390 C23 C 0.5975(5) 0.6472(3) 0.1174(3) H49 H 0.64370 0.64120 0.15550 H50 H 0.63380 0.65740 0.07510 H51 H 0.55910 0.59930 0.11230 C24 C 0.5817(4) 0.8172(4) 0.5097(2) H52 H 0.59650 0.87250 0.51610 H53 H 0.63620 0.78570 0.52710 H54 H 0.52160 0.80390 0.53460 C25 C 0.4620(4) 0.8635(4) 0.3873(3) H55 H 0.43540 0.84550 0.34340 H56 H 0.48760 0.91650 0.38210 H57 H 0.41000 0.86320 0.42190 C26 C 0.5068(5) 0.6968(4) 0.4119(3) H58 H 0.49410 0.68240 0.36410 H59 H 0.44490 0.69720 0.43740 H60 H 0.55160 0.65880 0.43260 C27 C 0.7740(4) 0.6762(3) 0.4535(2) H61 H 0.71160 0.65780 0.47240 H62 H 0.80160 0.71620 0.48370 H63 H 0.81980 0.63240 0.45010 C28 C 0.7049(5) 0.6361(3) 0.3127(3) H64 H 0.69830 0.65270 0.26490 H65 H 0.64070 0.62000 0.33030 H66 H 0.75060 0.59220 0.31550 C29 C 0.8801(4) 0.7333(3) 0.3290(3) H67 H 0.87540 0.74710 0.28040 H68 H 0.91760 0.68490 0.33390 H69 H 0.91330 0.77530 0.35400 C30 C 0.8330(4) 0.8932(3) 0.4526(3) H70 H 0.79810 0.87920 0.49480 H71 H 0.86350 0.94440 0.45820 H72 H 0.88370 0.85420 0.44320 C31 C 0.8183(4) 0.9274(3) 0.3021(3) H73 H 0.77440 0.94540 0.26570 H74 H 0.85680 0.88310 0.28550 H75 H 0.86250 0.96980 0.31540 C32 C 0.6672(5) 0.9852(3) 0.3983(3) H76 H 0.62950 0.99990 0.35760 H77 H 0.71040 1.02830 0.41140 H78 H 0.62220 0.97360 0.43610 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 O1 1.903 1_555 1_555 Li2 C1 2.172 1_555 1_555 O1 C3 1.448 1_555 1_555 O2 Li1 1.876 1_555 1_555 O3 Li1 1.883 1_555 1_555 Si1 C1 1.818 1_555 1_555 Si2 C1 1.831 1_555 1_555 Si3 C1 1.834 1_555 1_555 Si4 C2 1.837 1_555 1_555 Si5 C2 1.827 1_555 1_555 Si6 C2 1.831 1_555 1_555 C2 Li2 2.165 1_555 1_555 C3 H1 0.991 1_555 1_555 H2 C3 0.989 1_555 1_555 C4 C3 1.494 1_555 1_555 H3 C4 0.989 1_555 1_555 H4 C4 0.990 1_555 1_555 C5 C4 1.475 1_555 1_555 H5 C5 0.991 1_555 1_555 H6 C5 0.991 1_555 1_555 C6 O1 1.446 1_555 1_555 H7 C6 0.991 1_555 1_555 H8 C6 0.990 1_555 1_555 C7 O2 1.439 1_555 1_555 H9 C7 0.991 1_555 1_555 H10 C7 0.990 1_555 1_555 C8 C7 1.468 1_555 1_555 H11 C8 0.991 1_555 1_555 H12 C8 0.991 1_555 1_555 C9 C8 1.467 1_555 1_555 H13 C9 0.991 1_555 1_555 H14 C9 0.989 1_555 1_555 C10 O2 1.422 1_555 1_555 H15 C10 0.990 1_555 1_555 H16 C10 0.990 1_555 1_555 C11 O3 1.434 1_555 1_555 H17 C11 0.990 1_555 1_555 H18 C11 0.990 1_555 1_555 C12 C11 1.417 1_555 1_555 H19 C12 0.989 1_555 1_555 H20 C12 0.990 1_555 1_555 C13 C12 1.471 1_555 1_555 H21 C13 0.989 1_555 1_555 H22 C13 0.990 1_555 1_555 C14 O3 1.432 1_555 1_555 H23 C14 0.990 1_555 1_555 H24 C14 0.990 1_555 1_555 C15 Si1 1.904 1_555 1_555 H25 C15 0.933 1_555 1_555 H26 C15 1.007 1_555 1_555 H27 C15 0.923 1_555 1_555 C16 Si1 1.883 1_555 1_555 H28 C16 0.980 1_555 1_555 H29 C16 0.980 1_555 1_555 H30 C16 0.981 1_555 1_555 C17 Si1 1.887 1_555 1_555 H31 C17 0.981 1_555 1_555 H32 C17 0.979 1_555 1_555 H33 C17 0.981 1_555 1_555 C18 Si2 1.882 1_555 1_555 H34 C18 0.979 1_555 1_555 H35 C18 0.981 1_555 1_555 H36 C18 0.981 1_555 1_555 C19 Si2 1.874 1_555 1_555 H37 C19 0.981 1_555 1_555 H38 C19 0.980 1_555 1_555 H39 C19 0.979 1_555 1_555 C20 Si2 1.893 1_555 1_555 H40 C20 0.981 1_555 1_555 H41 C20 0.980 1_555 1_555 H42 C20 0.981 1_555 1_555 C21 Si3 1.875 1_555 1_555 H43 C21 0.979 1_555 1_555 H44 C21 0.981 1_555 1_555 H45 C21 0.980 1_555 1_555 C22 Si3 1.889 1_555 1_555 H46 C22 0.981 1_555 1_555 H47 C22 0.980 1_555 1_555 H48 C22 0.981 1_555 1_555 C23 Si3 1.869 1_555 1_555 H49 C23 0.980 1_555 1_555 H50 C23 0.979 1_555 1_555 H51 C23 0.980 1_555 1_555 C24 Si4 1.897 1_555 1_555 H52 C24 0.979 1_555 1_555 H53 C24 0.980 1_555 1_555 H54 C24 0.980 1_555 1_555 C25 Si4 1.883 1_555 1_555 H55 C25 0.981 1_555 1_555 H56 C25 0.980 1_555 1_555 H57 C25 0.980 1_555 1_555 C26 Si4 1.881 1_555 1_555 H58 C26 0.981 1_555 1_555 H59 C26 0.980 1_555 1_555 H60 C26 0.981 1_555 1_555 C27 Si5 1.893 1_555 1_555 H61 C27 0.980 1_555 1_555 H62 C27 0.980 1_555 1_555 H63 C27 0.980 1_555 1_555 C28 Si5 1.873 1_555 1_555 H64 C28 0.980 1_555 1_555 H65 C28 0.981 1_555 1_555 H66 C28 0.980 1_555 1_555 C29 Si5 1.895 1_555 1_555 H67 C29 0.980 1_555 1_555 H68 C29 0.981 1_555 1_555 H69 C29 0.981 1_555 1_555 C30 Si6 1.891 1_555 1_555 H70 C30 0.981 1_555 1_555 H71 C30 0.979 1_555 1_555 H72 C30 0.980 1_555 1_555 C31 Si6 1.890 1_555 1_555 H73 C31 0.979 1_555 1_555 H74 C31 0.979 1_555 1_555 H75 C31 0.980 1_555 1_555 C32 Si6 1.885 1_555 1_555 H76 C32 0.980 1_555 1_555 H77 C32 0.980 1_555 1_555 H78 C32 0.980 1_555 1_555 C5 C6 1.473 1_555 1_555 C9 C10 1.473 1_555 1_555 C13 C14 1.481 1_555 1_555 #END data_CSD_CIF_MIVVAO _audit_creation_date 2002-06-26 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD MIVVAO _database_code_depnum_ccdc_archive 'CCDC 184336' _chemical_formula_sum 'C22 H34 Na2 O6' _chemical_formula_moiety ; C12 H24 Na1 O6 1+,C10 H10 Na1 1- ; _journal_coden_Cambridge 1078 _journal_year 2002 _journal_name_full 'CSD Communication(Private Communication) ' loop_ _publ_author_name "T.Kaehler" "F.Olbrich" _chemical_name_systematic ; (1,4,7,10,13,16-Hexaoxacyclooctadecane)-sodium bis(\h^5^-cyclopentadienyl)-sodium ; _cell_volume 1182.045 _exptl_crystal_colour 'red' _exptl_crystal_density_diffrn 1.238 _exptl_special_details ; contribution from Institut fur Anorganische und Angewandte Chemie der Universitat Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg, Germany ; _exptl_crystal_description 'block' _diffrn_ambient_temperature 173 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_gt 0.0486 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,z 3 x,-y,z 4 1/2+x,1/2-y,z 5 -x,-y,-z 6 -1/2-x,-1/2-y,-z 7 -x,y,-z 8 -1/2-x,-1/2+y,-z _cell_length_a 12.417(3) _cell_length_b 12.3388(19) _cell_length_c 9.1041(12) _cell_angle_alpha 90 _cell_angle_beta 122.066(12) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Na 1.77 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 0.50000 0.00000 0.00000 Na2 Na 0.00000 0.00000 -0.50000 C1 C 0.25937(13) 0.05660(13) -0.22390(19) H1 H 0.24170 0.10190 -0.31860 C2 C 0.29003(14) 0.09162(13) -0.0596(2) H2 H 0.29630 0.16480 -0.02350 C3 C 0.3097(2) 0.00000 0.0417(3) H3 H 0.33260 0.00000 0.15920 O1 O 0.07565(15) 0.00000 -0.7243(2) O2 O 0.06033(10) 0.19887(9) -0.59191(13) C4 C 0.13092(17) 0.09635(17) -0.7421(2) H4 H 0.13420 0.09240 -0.84820 H5 H 0.21870 0.10480 -0.64120 C5 C 0.05260(17) 0.18959(15) -0.7527(2) H6 H 0.08420 0.25680 -0.77680 H7 H -0.03680 0.17840 -0.84770 C6 C -0.00546(16) 0.29000(12) -0.5862(2) H8 H -0.09590 0.28650 -0.68120 H9 H 0.03190 0.35720 -0.60000 C1B C 0.25937(13) -0.05660(13) -0.22390(19) C1D C 0.74063(13) -0.05660(13) 0.22390(19) C1F C 0.74063(13) 0.05660(13) 0.22390(19) C2B C 0.29003(14) -0.09162(13) -0.0596(2) H1B H 0.24170 -0.10190 -0.31860 H2B H 0.29630 -0.16480 -0.02350 C2D C 0.70997(14) -0.09162(13) 0.0596(2) H1D H 0.75830 -0.10190 0.31860 H2D H 0.70370 -0.16480 0.02350 C3D C 0.6903(2) 0.00000 -0.0417(3) C2F C 0.70997(14) 0.09162(13) 0.0596(2) H1F H 0.75830 0.10190 0.31860 H2F H 0.70370 0.16480 0.02350 H3D H 0.66740 0.00000 -0.15920 O1D O -0.07565(15) 0.00000 -0.2757(2) C4D C -0.13092(17) -0.09635(17) -0.2579(2) H4D H -0.13420 -0.09240 -0.15180 H5D H -0.21870 -0.10480 -0.35880 C5D C -0.05260(17) -0.18959(15) -0.2473(2) O2D O -0.06033(10) -0.19887(9) -0.40809(13) O2B O 0.06033(10) -0.19887(9) -0.59191(13) C5B C 0.05260(17) -0.18959(15) -0.7527(2) C4B C 0.13092(17) -0.09635(17) -0.7421(2) H4B H 0.13420 -0.09240 -0.84820 H5B H 0.21870 -0.10480 -0.64120 H6B H 0.08420 -0.25680 -0.77680 H7B H -0.03680 -0.17840 -0.84770 C6B C -0.00546(16) -0.29000(12) -0.5862(2) C6D C 0.00546(16) -0.29000(12) -0.4138(2) H8D H 0.09590 -0.28650 -0.31880 H9D H -0.03190 -0.35720 -0.40000 H8B H -0.09590 -0.28650 -0.68120 H9B H 0.03190 -0.35720 -0.60000 O2F O -0.06033(10) 0.19887(9) -0.40809(13) C5F C -0.05260(17) 0.18959(15) -0.2473(2) C4F C -0.13092(17) 0.09635(17) -0.2579(2) H4F H -0.13420 0.09240 -0.15180 H5F H -0.21870 0.10480 -0.35880 H6F H -0.08420 0.25680 -0.22320 H7F H 0.03680 0.17840 -0.15230 C6F C 0.00546(16) 0.29000(12) -0.4138(2) H8F H 0.09590 0.28650 -0.31880 H9F H -0.03190 0.35720 -0.40000 H6D H -0.08420 -0.25680 -0.22320 H7D H 0.03680 -0.17840 -0.15230 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Na1 C1 2.665 1_555 1_555 Na2 O1 2.663 1_555 1_555 C1 H1 0.950 1_555 1_555 C2 Na1 2.621 1_555 1_555 H2 C2 0.950 1_555 1_555 C3 Na1 2.585 1_555 1_555 H3 C3 0.950 1_555 1_555 O1 C4 1.424 1_555 1_555 O2 Na2 2.819 1_555 1_555 C4 H4 0.989 1_555 1_555 H5 C4 0.990 1_555 1_555 C5 O2 1.420 1_555 1_555 H6 C5 0.991 1_555 1_555 H7 C5 0.990 1_555 1_555 C6 O2 1.407 1_555 1_555 H8 C6 0.990 1_555 1_555 H9 C6 0.990 1_555 1_555 C1B Na1 2.665 1_555 1_555 C1D Na1 2.665 1_555 1_555 C1F Na1 2.665 1_555 1_555 C2B Na1 2.621 1_555 1_555 H1B C1B 0.950 1_555 1_555 H2B C2B 0.950 1_555 1_555 C2D Na1 2.621 1_555 1_555 H1D C1D 0.950 1_555 1_555 H2D C2D 0.950 1_555 1_555 C3D Na1 2.585 1_555 1_555 C2F Na1 2.621 1_555 1_555 H1F C1F 0.950 1_555 1_555 H2F C2F 0.950 1_555 1_555 H3D C3D 0.950 1_555 1_555 O1D Na2 2.663 1_555 1_555 C4D O1D 1.424 1_555 1_555 H4D C4D 0.989 1_555 1_555 H5D C4D 0.990 1_555 1_555 C5D C4D 1.476 1_555 1_555 O2D Na2 2.819 1_555 1_555 O2B Na2 2.819 1_555 1_555 C5B O2B 1.420 1_555 1_555 C4B O1 1.424 1_555 1_555 H4B C4B 0.989 1_555 1_555 H5B C4B 0.990 1_555 1_555 H6B C5B 0.991 1_555 1_555 H7B C5B 0.990 1_555 1_555 C6B O2B 1.407 1_555 1_555 C6D O2D 1.407 1_555 1_555 H8D C6D 0.990 1_555 1_555 H9D C6D 0.990 1_555 1_555 H8B C6B 0.990 1_555 1_555 H9B C6B 0.990 1_555 1_555 O2F Na2 2.819 1_555 1_555 C5F O2F 1.420 1_555 1_555 C4F O1D 1.424 1_555 1_555 H4F C4F 0.989 1_555 1_555 H5F C4F 0.990 1_555 1_555 H6F C5F 0.991 1_555 1_555 H7F C5F 0.990 1_555 1_555 C6F C6 1.502 1_555 1_555 H8F C6F 0.990 1_555 1_555 H9F C6F 0.990 1_555 1_555 H6D C5D 0.991 1_555 1_555 H7D C5D 0.990 1_555 1_555 C1 C1B 1.397 1_555 1_555 C1 C2 1.402 1_555 1_555 C2 C3 1.396 1_555 1_555 C3 C2B 1.396 1_555 1_555 C4 C5 1.476 1_555 1_555 C1B C2B 1.402 1_555 1_555 C1D C1F 1.397 1_555 1_555 C1D C2D 1.402 1_555 1_555 C1F C2F 1.402 1_555 1_555 C2D C3D 1.396 1_555 1_555 C3D C2F 1.396 1_555 1_555 C5D O2D 1.420 1_555 1_555 C5B C4B 1.476 1_555 1_555 C6B C6D 1.502 1_555 1_555 O2F C6F 1.407 1_555 1_555 C5F C4F 1.476 1_555 1_555 #END data_CSD_CIF_MOQWOE _audit_creation_date 2002-10-17 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD MOQWOE _chemical_formula_sum 'C48 H70 Li2 O4 Si2' _chemical_formula_moiety ; C16 H32 Li1 O4 1+,C32 H38 Li1 Si2 1- ; _journal_coden_Cambridge 579 _journal_volume 21 _journal_year 2002 _journal_page_first 220 _journal_name_full 'Organometallics ' loop_ _publ_author_name "M.S.Hill" "P.B.Hitchcock" _chemical_name_systematic ; tetrakis(Tetrahydrofuran)-lithium bis(diphenyl(trimethylsilyl)methyl)-lithium ; _cell_volume 2365.838 _exptl_crystal_colour 'orange-yellow' _exptl_crystal_density_diffrn 1.1 _exptl_special_details ; pyrophoric; air- and moisture-sensitive ; _exptl_crystal_preparation 'hexane' _diffrn_ambient_temperature 173 _refine_special_details ; The tetrahydrofuran ligands are disordered over two sites. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.085 _refine_ls_wR_factor_gt 0.085 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,-1/2+z _cell_length_a 11.7682(12) _cell_length_b 10.3345(10) _cell_length_c 19.558(2) _cell_angle_alpha 90 _cell_angle_beta 95.941(5) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.38 O 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.00000 0.00000 0.00000 Li2 Li 0.50000 0.5555(13) 0.25000 Si1 Si 0.2024(1) -0.1642(1) -0.0686(1) O1 O 0.4671(3) 0.6442(4) 0.3323(2) O2 O 0.6381(3) 0.4622(4) 0.2788(2) C1 C 0.1751(4) -0.0188(4) -0.0192(2) C2 C 0.1528(3) 0.1067(5) -0.0513(2) C3 C 0.1322(4) 0.2194(5) -0.0129(2) C4 C 0.1016(4) 0.3367(5) -0.0428(3) C5 C 0.0889(4) 0.3516(5) -0.1131(3) C6 C 0.1086(4) 0.2445(5) -0.1527(3) C7 C 0.1398(4) 0.1270(5) -0.1236(2) C8 C 0.2159(4) -0.0197(5) 0.0557(2) C9 C 0.3111(4) 0.0528(6) 0.0829(3) C10 C 0.3482(6) 0.0536(8) 0.1516(3) C11 C 0.2931(6) -0.0196(8) 0.1967(3) C12 C 0.2002(6) -0.0912(7) 0.1726(3) C13 C 0.1627(4) -0.0930(5) 0.1030(5) C14 C 0.3411(4) -0.1547(5) -0.1082(3) C15 C 0.2159(5) -0.3093(5) -0.0117(3) C16 C 0.0863(5) -0.2032(6) -0.1391(3) C17 C 0.4812(15) 0.5681(13) 0.3959(7) C18 C 0.4392(5) 0.6646(7) 0.4493(3) C19 C 0.4571(5) 0.7972(7) 0.4203(3) C20 C 0.4335(12) 0.7637(15) 0.3410(7) C21 C 0.7374(12) 0.5342(17) 0.2825(12) C22 C 0.8321(7) 0.4470(12) 0.2977(7) C23 C 0.7694(14) 0.321(2) 0.3182(12) C24 C 0.6497(10) 0.3365(12) 0.2958(6) C25? C 0.4051(11) 0.6002(14) 0.3883(7) C26? C 0.5053(12) 0.7812(13) 0.3537(7) C27? C 0.7295(13) 0.427(2) 0.2456(6) C28? C 0.8111(10) 0.4612(18) 0.3550(6) C29? C 0.6957(10) 0.4560(13) 0.3591(5) H1 H 0.13980 0.21360 0.03590 H2 H 0.08900 0.40880 -0.01440 H3 H 0.06750 0.43240 -0.13370 H4 H 0.10020 0.25240 -0.20140 H5 H 0.15320 0.05660 -0.15290 H6 H 0.35110 0.10300 0.05250 H7 H 0.41220 0.10490 0.16820 H8 H 0.31950 -0.02030 0.24430 H9 H 0.16080 -0.14030 0.20370 H10 H 0.09910 -0.14550 0.08710 H11 H 0.35190 -0.23420 -0.13410 H12 H 0.40440 -0.14490 -0.07180 H13 H 0.33950 -0.08020 -0.13920 H14 H 0.23040 -0.38590 -0.03910 H15 H 0.14490 -0.32150 0.00960 H16 H 0.27950 -0.29690 0.02410 H17 H 0.10680 -0.28160 -0.16320 H18 H 0.07740 -0.13090 -0.17170 H19 H 0.01430 -0.21750 -0.11920 H20 H 0.56210 0.54350 0.40810 H21 H 0.43360 0.48890 0.39190 H22 H 0.35750 0.65010 0.45480 H23 H 0.48420 0.65420 0.49460 H24 H 0.53590 0.82910 0.43260 H25 H 0.40170 0.86100 0.43500 H26 H 0.35100 0.77220 0.32560 H27 H 0.47610 0.82380 0.31360 H28 H 0.73710 0.60040 0.31910 H29 H 0.74380 0.57870 0.23830 H30 H 0.88600 0.47930 0.33610 H31 H 0.87380 0.43250 0.25690 H32 H 0.80030 0.24460 0.29590 H33 H 0.78080 0.30850 0.36870 H34 H 0.62670 0.28060 0.25560 H35 H 0.60250 0.31440 0.33320 H36? H 0.32230 0.61440 0.37590 H37? H 0.41760 0.50620 0.39500 H38? H 0.51070 0.62830 0.47290 H39? H 0.37890 0.66440 0.48100 H40? H 0.38350 0.84420 0.41340 H41? H 0.51030 0.84770 0.45260 H42? H 0.58960 0.78850 0.35940 H43? H 0.47360 0.84610 0.31970 H44? H 0.73490 0.48090 0.20440 H45? H 0.72330 0.33470 0.23130 H46? H 0.88360 0.37150 0.29610 H47? H 0.87420 0.52410 0.28400 H48? H 0.84090 0.54590 0.37230 H49? H 0.84940 0.39270 0.38430 H50? H 0.67040 0.53020 0.38580 H51? H 0.67460 0.37470 0.38140 C1B C -0.1751(4) 0.0188(4) 0.0192(2) Si1B Si -0.2024(1) 0.1642(1) 0.0686(1) C14B C -0.3411(4) 0.1547(5) 0.1082(3) H11B H -0.35190 0.23420 0.13410 H12B H -0.40440 0.14490 0.07180 H13B H -0.33950 0.08020 0.13920 C15B C -0.2159(5) 0.3093(5) 0.0117(3) H14B H -0.23040 0.38590 0.03910 H15B H -0.14490 0.32150 -0.00960 H16B H -0.27950 0.29690 -0.02410 C16B C -0.0863(5) 0.2032(6) 0.1391(3) H17B H -0.10680 0.28160 0.16320 H18B H -0.07740 0.13090 0.17170 H19B H -0.01430 0.21750 0.11920 C2B C -0.1528(3) -0.1067(5) 0.0513(2) C3B C -0.1322(4) -0.2194(5) 0.0129(2) C4B C -0.1016(4) -0.3367(5) 0.0428(3) C5B C -0.0889(4) -0.3516(5) 0.1131(3) C6B C -0.1086(4) -0.2445(5) 0.1527(3) C7B C -0.1398(4) -0.1270(5) 0.1236(2) H5B H -0.15320 -0.05660 0.15290 H4B H -0.10020 -0.25240 0.20140 H3B H -0.06750 -0.43240 0.13370 H2B H -0.08900 -0.40880 0.01440 H1B H -0.13980 -0.21360 -0.03590 C8B C -0.2159(4) 0.0197(5) -0.0557(2) C9B C -0.3111(4) -0.0528(6) -0.0829(3) C10B C -0.3482(6) -0.0536(8) -0.1516(3) C11B C -0.2931(6) 0.0196(8) -0.1967(3) C12B C -0.2002(6) 0.0912(7) -0.1726(3) C13B C -0.1627(4) 0.0930(5) -0.1030(5) H10B H -0.09910 0.14550 -0.08710 H9B H -0.16080 0.14030 -0.20370 H8B H -0.31950 0.02030 -0.24430 H7B H -0.41220 -0.10490 -0.16820 H6B H -0.35110 -0.10300 -0.05250 O1A O 0.5329(3) 0.6442(4) 0.1677(2) C17A C 0.5188(15) 0.5681(13) 0.1041(7) C18A C 0.5608(5) 0.6646(7) 0.0507(3) C19A C 0.5429(5) 0.7972(7) 0.0797(3) C20A C 0.5665(12) 0.7637(15) 0.1590(7) H26A H 0.64900 0.77220 0.17440 H27A H 0.52390 0.82380 0.18640 H24A H 0.46410 0.82910 0.06740 H25A H 0.59830 0.86100 0.06500 H22A H 0.64250 0.65010 0.04520 H23A H 0.51580 0.65420 0.00540 H20A H 0.43790 0.54350 0.09190 H21A H 0.56640 0.48890 0.10810 O2A O 0.3619(3) 0.4622(4) 0.2212(2) C21A C 0.2626(12) 0.5342(17) 0.2175(12) C22A C 0.1679(7) 0.4470(12) 0.2023(7) C23A C 0.2306(14) 0.321(2) 0.1818(12) C24A C 0.3503(10) 0.3365(12) 0.2042(6) H34A H 0.37330 0.28060 0.24440 H35A H 0.39750 0.31440 0.16680 H32A H 0.19970 0.24460 0.20410 H33A H 0.21920 0.30850 0.13130 H30A H 0.11400 0.47930 0.16390 H31A H 0.12620 0.43250 0.24310 H28A H 0.26290 0.60040 0.18090 H29A H 0.25620 0.57870 0.26170 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 C1 2.141 1_555 1_555 Li2 O1 1.926 1_555 1_555 Si1 C1 1.833 1_555 1_555 O1 C17 1.466 1_555 1_555 O2 Li2 1.923 1_555 1_555 C1 C2 1.453 1_555 1_555 C2 Li1 2.414 1_555 1_555 C3 C2 1.420 1_555 1_555 C4 C3 1.378 1_555 1_555 C5 C4 1.376 1_555 1_555 C6 C5 1.384 1_555 1_555 C7 C2 1.422 1_555 1_555 C8 C1 1.494 1_555 1_555 C9 C8 1.406 1_555 1_555 C10 C9 1.369 1_555 1_555 C11 C10 1.374 1_555 1_555 C12 C11 1.363 1_555 1_555 C13 C8 1.393 1_555 1_555 C14 Si1 1.880 1_555 1_555 C15 Si1 1.864 1_555 1_555 C16 Si1 1.882 1_555 1_555 C17 C18 1.561 1_555 1_555 C18 C19 1.506 1_555 1_555 C19 C20 1.585 1_555 1_555 C20 O1 1.313 1_555 1_555 C21 O2 1.381 1_555 1_555 C22 C21 1.440 1_555 1_555 C23 C22 1.569 1_555 1_555 C24 O2 1.344 1_555 1_555 H1 C3 0.951 1_555 1_555 H2 C4 0.950 1_555 1_555 H3 C5 0.950 1_555 1_555 H4 C6 0.951 1_555 1_555 H5 C7 0.949 1_555 1_555 H6 C9 0.950 1_555 1_555 H7 C10 0.950 1_555 1_555 H8 C11 0.950 1_555 1_555 H9 C12 0.949 1_555 1_555 H10 C13 0.950 1_555 1_555 H11 C14 0.980 1_555 1_555 H12 C14 0.981 1_555 1_555 H13 C14 0.979 1_555 1_555 H14 C15 0.981 1_555 1_555 H15 C15 0.980 1_555 1_555 H16 C15 0.979 1_555 1_555 H17 C16 0.980 1_555 1_555 H18 C16 0.981 1_555 1_555 H19 C16 0.980 1_555 1_555 H20 C17 0.990 1_555 1_555 H21 C17 0.990 1_555 1_555 H22 C18 0.990 1_555 1_555 H23 C18 0.990 1_555 1_555 H24 C19 0.990 1_555 1_555 H25 C19 0.991 1_555 1_555 H26 C20 0.990 1_555 1_555 H27 C20 0.990 1_555 1_555 H28 C21 0.990 1_555 1_555 H29 C21 0.989 1_555 1_555 H30 C22 0.990 1_555 1_555 H31 C22 0.990 1_555 1_555 H32 C23 0.989 1_555 1_555 H33 C23 0.991 1_555 1_555 H34 C24 0.991 1_555 1_555 H35 C24 0.990 1_555 1_555 C1B Li1 2.141 1_555 1_555 Si1B C1B 1.833 1_555 1_555 C14B Si1B 1.880 1_555 1_555 H11B C14B 0.980 1_555 1_555 H12B C14B 0.981 1_555 1_555 H13B C14B 0.979 1_555 1_555 C15B Si1B 1.864 1_555 1_555 H14B C15B 0.981 1_555 1_555 H15B C15B 0.980 1_555 1_555 H16B C15B 0.979 1_555 1_555 C16B Si1B 1.882 1_555 1_555 H17B C16B 0.980 1_555 1_555 H18B C16B 0.981 1_555 1_555 H19B C16B 0.980 1_555 1_555 C2B Li1 2.414 1_555 1_555 C3B C2B 1.420 1_555 1_555 C4B C3B 1.378 1_555 1_555 C5B C4B 1.376 1_555 1_555 C6B C5B 1.384 1_555 1_555 C7B C2B 1.422 1_555 1_555 H5B C7B 0.949 1_555 1_555 H4B C6B 0.951 1_555 1_555 H3B C5B 0.950 1_555 1_555 H2B C4B 0.950 1_555 1_555 H1B C3B 0.951 1_555 1_555 C8B C1B 1.494 1_555 1_555 C9B C8B 1.406 1_555 1_555 C10B C9B 1.369 1_555 1_555 C11B C10B 1.374 1_555 1_555 C12B C11B 1.363 1_555 1_555 C13B C8B 1.393 1_555 1_555 H10B C13B 0.950 1_555 1_555 H9B C12B 0.949 1_555 1_555 H8B C11B 0.950 1_555 1_555 H7B C10B 0.950 1_555 1_555 H6B C9B 0.950 1_555 1_555 O1A Li2 1.926 1_555 1_555 C17A O1A 1.466 1_555 1_555 C18A C17A 1.561 1_555 1_555 C19A C18A 1.506 1_555 1_555 C20A O1A 1.313 1_555 1_555 H26A C20A 0.990 1_555 1_555 H27A C20A 0.990 1_555 1_555 H24A C19A 0.990 1_555 1_555 H25A C19A 0.991 1_555 1_555 H22A C18A 0.990 1_555 1_555 H23A C18A 0.990 1_555 1_555 H20A C17A 0.990 1_555 1_555 H21A C17A 0.990 1_555 1_555 O2A Li2 1.923 1_555 1_555 C21A O2A 1.381 1_555 1_555 C22A C21A 1.440 1_555 1_555 C23A C22A 1.569 1_555 1_555 C24A O2A 1.344 1_555 1_555 H34A C24A 0.991 1_555 1_555 H35A C24A 0.990 1_555 1_555 H32A C23A 0.989 1_555 1_555 H33A C23A 0.991 1_555 1_555 H30A C22A 0.990 1_555 1_555 H31A C22A 0.990 1_555 1_555 H28A C21A 0.990 1_555 1_555 H29A C21A 0.989 1_555 1_555 C6 C7 1.375 1_555 1_555 C12 C13 1.387 1_555 1_555 C23 C24 1.440 1_555 1_555 C1B C2B 1.453 1_555 1_555 C6B C7B 1.375 1_555 1_555 C12B C13B 1.387 1_555 1_555 C19A C20A 1.585 1_555 1_555 C23A C24A 1.440 1_555 1_555 #END data_CSD_CIF_MOQWUK _audit_creation_date 2002-10-17 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD MOQWUK _chemical_formula_sum 'C58 H74 Li2 O4 Si2' _chemical_formula_moiety ; C16 H32 Li1 O4 1+,C42 H42 Li1 Si2 1- ; _journal_coden_Cambridge 579 _journal_volume 21 _journal_year 2002 _journal_page_first 220 _journal_name_full 'Organometallics ' loop_ _publ_author_name "M.S.Hill" "P.B.Hitchcock" _chemical_name_systematic ; tetrakis(Tetrahydrofuran)-lithium bis(diphenyl(dimethyl(phenyl)silyl)methyl)-lithium ; _cell_volume 5473.616 _exptl_crystal_colour 'orange-yellow' _exptl_crystal_density_diffrn 1.1 _exptl_special_details ; air- and moisture-sensitive ; _exptl_crystal_description 'blocks' _exptl_crystal_preparation 'hexane/toluene' _diffrn_ambient_temperature 173 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.066 _refine_ls_wR_factor_gt 0.066 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 1/2+x,1/2+y,z 4 1/2-x,1/2+y,1/2-z 5 -x,-y,-z 6 x,-y,-1/2+z 7 -1/2-x,-1/2-y,-z 8 -1/2+x,-1/2-y,-1/2+z _cell_length_a 16.5808(7) _cell_length_b 13.4857(7) _cell_length_c 24.7299(11) _cell_angle_alpha 90 _cell_angle_beta 98.167(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.28 O 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.25000 0.25000 0.50000 Li2 Li 0.50000 0.3019(7) 0.25000 Si1 Si 0.2655(1) 0.4778(1) 0.5483(1) O1 O 0.4137(2) 0.3825(2) 0.2691(1) O2 O 0.4561(2) 0.2177(2) 0.1907(1) C1 C 0.2333(2) 0.3525(2) 0.5627(1) C2 C 0.1491(2) 0.3186(2) 0.5469(1) C3 C 0.1253(2) 0.2193(2) 0.5546(1) C4 C 0.0479(2) 0.1835(3) 0.5354(1) C5 C -0.0097(2) 0.2447(3) 0.5066(1) C6 C 0.0108(2) 0.3418(3) 0.4986(1) C7 C 0.0872(2) 0.3789(3) 0.5181(1) C8 C 0.2845(2) 0.2966(2) 0.6068(1) C9 C 0.3645(2) 0.2687(2) 0.6022(1) C10 C 0.4131(2) 0.2210(3) 0.6443(2) C11 C 0.3846(2) 0.1990(3) 0.6924(2) C12 C 0.3053(2) 0.2239(3) 0.6980(1) C13 C 0.2567(2) 0.2714(2) 0.6562(1) C14 C 0.3766(2) 0.5000(3) 0.5717(2) C15 C 0.2463(3) 0.5143(3) 0.4740(1) C16 C 0.2125(2) 0.5729(2) 0.5872(1) C17 C 0.2168(2) 0.6749(3) 0.5786(1) C18 C 0.1817(2) 0.7430(3) 0.6097(2) C19 C 0.1406(2) 0.7114(3) 0.6509(2) C20 C 0.1343(2) 0.6121(3) 0.6602(1) C21 C 0.1693(2) 0.5436(2) 0.6288(1) C22 C 0.3624(3) 0.4459(6) 0.2317(2) C23 C 0.3219(5) 0.5138(5) 0.2656(3) C24 C 0.3668(7) 0.5052(6) 0.3205(3) C25 C 0.4163(3) 0.4231(4) 0.3219(2) C26 C 0.3778(3) 0.1748(7) 0.1889(3) C27 C 0.3768(4) 0.0800(5) 0.1634(3) C28 C 0.4479(3) 0.0767(5) 0.1361(3) C29 C 0.4996(3) 0.1594(4) 0.1568(2) H1 H 0.16390 0.17530 0.57390 H2 H 0.03460 0.11650 0.54200 H3 H -0.06230 0.22020 0.49270 H4 H -0.02860 0.38460 0.47920 H5 H 0.09860 0.44670 0.51200 H6 H 0.38580 0.28280 0.56940 H7 H 0.46720 0.20310 0.63980 H8 H 0.41870 0.16720 0.72140 H9 H 0.28430 0.20820 0.73070 H10 H 0.20230 0.28770 0.66080 H11 H 0.39040 0.56830 0.56300 H12 H 0.40890 0.45370 0.55310 H13 H 0.38830 0.48970 0.61120 H14 H 0.26540 0.58230 0.46990 H15 H 0.18780 0.51040 0.46080 H16 H 0.27580 0.46910 0.45270 H17 H 0.24490 0.69840 0.55020 H18 H 0.18600 0.81190 0.60270 H19 H 0.11680 0.75810 0.67260 H20 H 0.10560 0.58980 0.68860 H21 H 0.16360 0.47490 0.63590 H22 H 0.32160 0.40600 0.20790 H23 H 0.39550 0.48340 0.20840 H24 H 0.32400 0.58270 0.25210 H25 H 0.26420 0.49470 0.26530 H26 H 0.40020 0.56540 0.32970 H27 H 0.32840 0.49810 0.34750 H28 H 0.39810 0.37280 0.34670 H29 H 0.47300 0.44190 0.33640 H30 H 0.33640 0.21830 0.16810 H31 H 0.36440 0.16760 0.22650 H32 H 0.32660 0.07190 0.13680 H33 H 0.37880 0.02660 0.19100 H34 H 0.43200 0.08280 0.09610 H35 H 0.47710 0.01310 0.14380 H36 H 0.55070 0.13450 0.17800 H37 H 0.51370 0.19980 0.12610 C1F C 0.2667(2) 0.1475(2) 0.4373(1) Si1F Si 0.2345(1) 0.0222(1) 0.4517(1) C14F C 0.1234(2) 0.0000(3) 0.4283(2) H11F H 0.10960 -0.06830 0.43700 H12F H 0.09110 0.04630 0.44690 H13F H 0.11170 0.01030 0.38880 C15F C 0.2537(3) -0.0143(3) 0.5260(1) H14F H 0.23460 -0.08230 0.53010 H15F H 0.31220 -0.01040 0.53920 H16F H 0.22420 0.03090 0.54730 C16F C 0.2875(2) -0.0729(2) 0.4128(1) C17F C 0.2832(2) -0.1749(3) 0.4214(1) C18F C 0.3183(2) -0.2430(3) 0.3903(2) C19F C 0.3594(2) -0.2114(3) 0.3491(2) C20F C 0.3657(2) -0.1121(3) 0.3398(1) C21F C 0.3307(2) -0.0436(2) 0.3712(1) H21F H 0.33640 0.02510 0.36410 H20F H 0.39440 -0.08980 0.31140 H19F H 0.38320 -0.25810 0.32740 H18F H 0.31400 -0.31190 0.39730 H17F H 0.25510 -0.19840 0.44980 C2F C 0.3509(2) 0.1814(2) 0.4531(1) C3F C 0.3747(2) 0.2807(2) 0.4454(1) C4F C 0.4521(2) 0.3165(3) 0.4646(1) C5F C 0.5097(2) 0.2553(3) 0.4934(1) C6F C 0.4892(2) 0.1582(3) 0.5014(1) C7F C 0.4128(2) 0.1211(3) 0.4819(1) H5F H 0.40140 0.05330 0.48800 H4F H 0.52860 0.11540 0.52080 H3F H 0.56230 0.27980 0.50730 H2F H 0.46540 0.38350 0.45800 H1F H 0.33610 0.32470 0.42610 C8F C 0.2155(2) 0.2034(2) 0.3932(1) C9F C 0.1355(2) 0.2313(2) 0.3978(1) C10F C 0.0869(2) 0.2790(3) 0.3557(2) C11F C 0.1154(2) 0.3010(3) 0.3076(2) C12F C 0.1947(2) 0.2761(3) 0.3020(1) C13F C 0.2433(2) 0.2286(2) 0.3438(1) H10F H 0.29770 0.21230 0.33920 H9F H 0.21570 0.29180 0.26930 H8F H 0.08130 0.33280 0.27860 H7F H 0.03280 0.29690 0.36020 H6F H 0.11420 0.21720 0.43060 O1A O 0.5863(2) 0.3825(2) 0.2309(1) C22A C 0.6376(3) 0.4459(6) 0.2683(2) C23A C 0.6781(5) 0.5138(5) 0.2344(3) C24A C 0.6332(7) 0.5052(6) 0.1795(3) C25A C 0.5837(3) 0.4231(4) 0.1781(2) H28A H 0.60190 0.37280 0.15330 H29A H 0.52700 0.44190 0.16360 H26A H 0.59980 0.56540 0.17030 H27A H 0.67160 0.49810 0.15250 H24A H 0.67600 0.58270 0.24790 H25A H 0.73580 0.49470 0.23470 H22A H 0.67840 0.40600 0.29210 H23A H 0.60450 0.48340 0.29160 O2A O 0.5439(2) 0.2177(2) 0.3093(1) C26A C 0.6222(3) 0.1748(7) 0.3111(3) C27A C 0.6232(4) 0.0800(5) 0.3366(3) C28A C 0.5521(3) 0.0767(5) 0.3639(3) C29A C 0.5004(3) 0.1594(4) 0.3432(2) H36A H 0.44930 0.13450 0.32200 H37A H 0.48630 0.19980 0.37390 H34A H 0.56800 0.08280 0.40390 H35A H 0.52290 0.01310 0.35620 H32A H 0.67340 0.07190 0.36320 H33A H 0.62120 0.02660 0.30900 H30A H 0.66360 0.21830 0.33190 H31A H 0.63560 0.16760 0.27350 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 C1 2.125 1_555 1_555 Li2 O1 1.909 1_555 1_555 Si1 C1 1.822 1_555 1_555 O1 C22 1.444 1_555 1_555 O2 Li2 1.915 1_555 1_555 C1 C2 1.468 1_555 1_555 C2 Li1 2.356 1_555 1_555 C3 C2 1.417 1_555 1_555 C4 C3 1.390 1_555 1_555 C5 C4 1.381 1_555 1_555 C6 C5 1.374 1_555 1_555 C7 C2 1.419 1_555 1_555 C8 C1 1.488 1_555 1_555 C9 C8 1.399 1_555 1_555 C10 C9 1.382 1_555 1_555 C11 C10 1.373 1_555 1_555 C12 C11 1.383 1_555 1_555 C13 C8 1.407 1_555 1_555 C14 Si1 1.875 1_555 1_555 C15 Si1 1.885 1_555 1_555 C16 Si1 1.893 1_555 1_555 C17 C16 1.395 1_555 1_555 C18 C17 1.379 1_555 1_555 C19 C18 1.372 1_555 1_555 C20 C19 1.365 1_555 1_555 C21 C16 1.392 1_555 1_555 C22 C23 1.467 1_555 1_555 C23 C24 1.457 1_555 1_555 C24 C25 1.376 1_555 1_555 C25 O1 1.411 1_555 1_555 C26 O2 1.416 1_555 1_555 C27 C26 1.425 1_555 1_555 C28 C27 1.440 1_555 1_555 C29 O2 1.419 1_555 1_555 H1 C3 0.950 1_555 1_555 H2 C4 0.950 1_555 1_555 H3 C5 0.950 1_555 1_555 H4 C6 0.949 1_555 1_555 H5 C7 0.950 1_555 1_555 H6 C9 0.949 1_555 1_555 H7 C10 0.951 1_555 1_555 H8 C11 0.950 1_555 1_555 H9 C12 0.949 1_555 1_555 H10 C13 0.951 1_555 1_555 H11 C14 0.980 1_555 1_555 H12 C14 0.979 1_555 1_555 H13 C14 0.978 1_555 1_555 H14 C15 0.980 1_555 1_555 H15 C15 0.980 1_555 1_555 H16 C15 0.981 1_555 1_555 H17 C17 0.951 1_555 1_555 H18 C18 0.950 1_555 1_555 H19 C19 0.949 1_555 1_555 H20 C20 0.951 1_555 1_555 H21 C21 0.950 1_555 1_555 H22 C22 0.990 1_555 1_555 H23 C22 0.989 1_555 1_555 H24 C23 0.990 1_555 1_555 H25 C23 0.990 1_555 1_555 H26 C24 0.991 1_555 1_555 H27 C24 0.991 1_555 1_555 H28 C25 0.990 1_555 1_555 H29 C25 0.990 1_555 1_555 H30 C26 0.990 1_555 1_555 H31 C26 0.991 1_555 1_555 H32 C27 0.991 1_555 1_555 H33 C27 0.990 1_555 1_555 H34 C28 0.990 1_555 1_555 H35 C28 0.990 1_555 1_555 H36 C29 0.990 1_555 1_555 H37 C29 0.989 1_555 1_555 C1F Li1 2.125 1_555 1_555 Si1F C1F 1.822 1_555 1_555 C14F Si1F 1.875 1_555 1_555 H11F C14F 0.980 1_555 1_555 H12F C14F 0.979 1_555 1_555 H13F C14F 0.978 1_555 1_555 C15F Si1F 1.885 1_555 1_555 H14F C15F 0.980 1_555 1_555 H15F C15F 0.980 1_555 1_555 H16F C15F 0.981 1_555 1_555 C16F Si1F 1.893 1_555 1_555 C17F C16F 1.395 1_555 1_555 C18F C17F 1.379 1_555 1_555 C19F C18F 1.372 1_555 1_555 C20F C19F 1.365 1_555 1_555 C21F C16F 1.392 1_555 1_555 H21F C21F 0.950 1_555 1_555 H20F C20F 0.951 1_555 1_555 H19F C19F 0.949 1_555 1_555 H18F C18F 0.950 1_555 1_555 H17F C17F 0.951 1_555 1_555 C2F Li1 2.356 1_555 1_555 C3F C2F 1.417 1_555 1_555 C4F C3F 1.390 1_555 1_555 C5F C4F 1.381 1_555 1_555 C6F C5F 1.374 1_555 1_555 C7F C2F 1.419 1_555 1_555 H5F C7F 0.950 1_555 1_555 H4F C6F 0.949 1_555 1_555 H3F C5F 0.950 1_555 1_555 H2F C4F 0.950 1_555 1_555 H1F C3F 0.950 1_555 1_555 C8F C1F 1.488 1_555 1_555 C9F C8F 1.399 1_555 1_555 C10F C9F 1.382 1_555 1_555 C11F C10F 1.373 1_555 1_555 C12F C11F 1.383 1_555 1_555 C13F C8F 1.407 1_555 1_555 H10F C13F 0.951 1_555 1_555 H9F C12F 0.949 1_555 1_555 H8F C11F 0.950 1_555 1_555 H7F C10F 0.951 1_555 1_555 H6F C9F 0.949 1_555 1_555 O1A Li2 1.909 1_555 1_555 C22A O1A 1.444 1_555 1_555 C23A C22A 1.467 1_555 1_555 C24A C23A 1.457 1_555 1_555 C25A O1A 1.411 1_555 1_555 H28A C25A 0.990 1_555 1_555 H29A C25A 0.990 1_555 1_555 H26A C24A 0.991 1_555 1_555 H27A C24A 0.991 1_555 1_555 H24A C23A 0.990 1_555 1_555 H25A C23A 0.990 1_555 1_555 H22A C22A 0.990 1_555 1_555 H23A C22A 0.989 1_555 1_555 O2A Li2 1.915 1_555 1_555 C26A O2A 1.416 1_555 1_555 C27A C26A 1.425 1_555 1_555 C28A C27A 1.440 1_555 1_555 C29A O2A 1.419 1_555 1_555 H36A C29A 0.990 1_555 1_555 H37A C29A 0.989 1_555 1_555 H34A C28A 0.990 1_555 1_555 H35A C28A 0.990 1_555 1_555 H32A C27A 0.991 1_555 1_555 H33A C27A 0.990 1_555 1_555 H30A C26A 0.990 1_555 1_555 H31A C26A 0.991 1_555 1_555 C6 C7 1.383 1_555 1_555 C12 C13 1.375 1_555 1_555 C20 C21 1.386 1_555 1_555 C28 C29 1.455 1_555 1_555 C1F C2F 1.468 1_555 1_555 C20F C21F 1.386 1_555 1_555 C6F C7F 1.383 1_555 1_555 C12F C13F 1.375 1_555 1_555 C24A C25A 1.376 1_555 1_555 C28A C29A 1.455 1_555 1_555 #END data_CSD_CIF_MUJCIF _audit_creation_date 2015-06-02 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD MUJCIF _database_code_depnum_ccdc_archive 'CCDC 1028726' _chemical_formula_sum 'C52 H106 B4 K2 O18' _chemical_formula_moiety ; C32 H66 B4 K1 O10 1-,C20 H40 K1 O8 1+ ; _journal_coden_Cambridge 1220 _journal_volume 21 _journal_year 2015 _journal_page_first 7082 _journal_name_full 'Chem.-Eur.J. ' loop_ _publ_author_name "S.Pietsch" "E.C.Neeve" "D.C.Apperley" "R.Bertermann" "Fanyang Mo" "Di Qiu" "Man Sing Cheung" "Li Dang" "Jianbo Wang" "U.Radius" "C.Kleeberg" "Zhenyang Lin" "T.B.Marder" _chemical_name_systematic ; (18-Crown-6)-bis(tetrahydrofuran)-potassium bis(2-t-butoxy-4,4,4',4',5,5,5',5'-octamethyl-2,2'-bi-1,3,2-dioxaborolane)-pot assium ; _cell_volume 1612.056 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.179 _exptl_crystal_description 'block' _diffrn_ambient_temperature 120 _refine_special_details ; C10,C11,C12,C7,C8,C9,O3 and C10',C11',C12',C7',C8',C9',O3' disordered over two sites with occupancies 0.656:0.344. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.058 _refine_ls_wR_factor_gt 0.058 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 9.8484(2) _cell_length_b 13.0033(3) _cell_length_c 14.0924(3) _cell_angle_alpha 74.7327(8) _cell_angle_beta 78.2436(8) _cell_angle_gamma 68.8727(7) _cell_formula_units_Z 1 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 B 0.83 K 2.03 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z C1 C 0.7654(3) -0.0203(2) 0.36055(18) C2 C 0.8376(3) -0.0971(2) 0.28537(19) C3 C 0.7928(4) -0.0726(3) 0.4668(2) H1 H 0.89850 -0.10120 0.47090 H2 H 0.75260 -0.13490 0.49110 H3 H 0.74500 -0.01560 0.50750 C4 C 0.5998(3) 0.0347(2) 0.3577(2) H4 H 0.56200 0.09310 0.39720 H5 H 0.55150 -0.02260 0.38500 H6 H 0.58000 0.06880 0.28900 C5 C 0.9878(3) -0.1803(3) 0.3113(3) H7 H 1.04110 -0.21380 0.25420 H8 H 0.97430 -0.23990 0.36790 H9 H 1.04400 -0.14040 0.32830 C6 C 0.7464(4) -0.1603(3) 0.2672(2) H10 H 0.65510 -0.10640 0.24290 H11 H 0.72320 -0.20990 0.32930 H12 H 0.80160 -0.20560 0.21770 O1 O 1.1125(3) 0.0821(3) 0.1143(2) C7 C 1.2200(7) 0.1368(5) 0.0994(4) C8 C 1.1467(3) 0.2182(4) 0.1730(3) C9 C 1.3702(4) 0.0503(4) 0.1211(3) H13 H 1.36140 0.00430 0.18800 H14 H 1.44010 0.08980 0.11670 H15 H 1.40510 0.00160 0.07270 C10 C 1.2342(6) 0.1995(4) -0.0083(3) H16 H 1.26400 0.14580 -0.05210 H17 H 1.30800 0.23670 -0.01840 H18 H 1.13950 0.25610 -0.02340 C11 C 1.1860(4) 0.1559(4) 0.2796(3) H19 H 1.29060 0.13990 0.28170 H20 H 1.16410 0.08490 0.29730 H21 H 1.12800 0.20350 0.32680 C12 C 1.1856(9) 0.3257(6) 0.1469(5) H22 H 1.29160 0.30690 0.14550 H23 H 1.13370 0.37140 0.19660 H24 H 1.15660 0.36830 0.08150 C13 C 0.7485(4) 0.2929(2) 0.0346(2) C14 C 0.6766(5) 0.2737(3) -0.0414(3) H25 H 0.74360 0.26880 -0.10310 H26 H 0.58590 0.33660 -0.05420 H27 H 0.65380 0.20330 -0.01620 C15 C 0.6466(4) 0.2977(3) 0.1319(2) H28 H 0.62060 0.22840 0.15440 H29 H 0.55730 0.36280 0.12160 H30 H 0.69630 0.30510 0.18200 C16 C 0.7781(6) 0.4061(3) -0.0018(3) H31 H 0.82220 0.41870 0.04870 H32 H 0.68550 0.46720 -0.01370 H33 H 0.84540 0.40450 -0.06350 B1 B 0.8767(3) 0.0737(2) 0.2225(2) B2 B 0.9578(3) 0.1622(3) 0.1353(2) O2 O 0.82938(17) 0.06915(14) 0.32254(12) O3 O 0.86443(19) -0.01788(14) 0.19534(12) O4 O 0.98643(19) 0.25046(14) 0.16895(12) O5 O 0.8847(2) 0.20496(15) 0.04312(12) K1 K 1.00000 0.00000 0.00000 C17 C 0.8284(3) 0.3068(2) 0.39398(19) H34 H 0.89980 0.32440 0.42210 H35 H 0.88130 0.26850 0.33860 C18 C 0.7712(3) 0.4806(2) 0.27841(19) H36 H 0.82780 0.43880 0.22580 H37 H 0.83720 0.50890 0.30130 C19 C 0.6441(3) 0.5770(2) 0.23883(18) H38 H 0.67980 0.62970 0.18360 H39 H 0.58060 0.54890 0.21340 C20 C 0.4456(3) 0.7319(2) 0.2848(2) H40 H 0.37330 0.71120 0.26060 H41 H 0.48290 0.78400 0.23000 C21 C 0.3746(3) 0.7877(2) 0.3704(2) H42 H 0.44940 0.80110 0.39870 H43 H 0.30110 0.86160 0.34760 C22 C 0.2405(3) 0.7684(2) 0.5282(2) H44 H 0.16520 0.84220 0.50790 H45 H 0.31660 0.78160 0.55530 C23 C 0.3901(3) 0.3643(3) 0.3493(2) H46 H 0.36500 0.30370 0.33390 H47 H 0.49320 0.35730 0.32200 C24 C 0.2891(4) 0.4775(3) 0.3079(2) H48 H 0.25680 0.47780 0.24580 H49 H 0.33610 0.53630 0.29520 C25 C 0.1622(4) 0.4947(3) 0.3901(3) H50 H 0.13310 0.57130 0.40340 H51 H 0.07650 0.48510 0.37140 C26 C 0.2145(3) 0.4093(3) 0.4775(2) H52 H 0.19500 0.44450 0.53530 H53 H 0.16440 0.35200 0.49360 O6 O 0.71610(17) 0.40840(14) 0.35867(12) O7 O 0.56328(18) 0.63355(14) 0.31648(12) O8 O 0.30495(17) 0.71834(13) 0.44441(12) O9 O 0.3684(2) 0.35858(18) 0.45328(14) K2 K 0.50000 0.50000 0.50000 O10? O 1.1020(6) 0.1010(7) 0.0818(5) C27? C 1.1964(16) 0.1364(9) 0.1217(9) C28? C 1.1216(7) 0.2651(6) 0.1164(5) C29? C 1.2267(9) 0.0646(8) 0.2227(6) H54? H 1.13460 0.07460 0.26730 H55? H 1.29420 0.08710 0.24880 H56? H 1.27090 -0.01480 0.21790 C30? C 1.3354(8) 0.1131(7) 0.0472(7) H57? H 1.38420 0.03150 0.05500 H58? H 1.40190 0.14770 0.05940 H59? H 1.30900 0.14500 -0.02030 C31? C 1.168(2) 0.3086(14) 0.1892(9) H60? H 1.11320 0.38890 0.18470 H61? H 1.27340 0.29810 0.17380 H62? H 1.14860 0.26700 0.25650 C32? C 1.1138(9) 0.3395(6) 0.0171(5) H63? H 1.07420 0.31090 -0.02510 H64? H 1.21230 0.34120 -0.01240 H65? H 1.04980 0.41590 0.02290 C1A C 1.2346(3) 0.0203(2) -0.36055(18) C2A C 1.1624(3) 0.0971(2) -0.28537(19) C3A C 1.2072(4) 0.0726(3) -0.4668(2) H1A H 1.10150 0.10120 -0.47090 H2A H 1.24740 0.13490 -0.49110 H3A H 1.25500 0.01560 -0.50750 C4A C 1.4002(3) -0.0347(2) -0.3577(2) H4A H 1.43800 -0.09310 -0.39720 H5A H 1.44850 0.02260 -0.38500 H6A H 1.42000 -0.06880 -0.28900 C5A C 1.0122(3) 0.1803(3) -0.3113(3) H7A H 0.95890 0.21380 -0.25420 H8A H 1.02570 0.23990 -0.36790 H9A H 0.95600 0.14040 -0.32830 C6A C 1.2536(4) 0.1603(3) -0.2672(2) H10A H 1.34490 0.10640 -0.24290 H11A H 1.27680 0.20990 -0.32930 H12A H 1.19840 0.20560 -0.21770 O1A O 0.8875(3) -0.0821(3) -0.1143(2) C7A C 0.7800(7) -0.1368(5) -0.0994(4) C8A C 0.8533(3) -0.2182(4) -0.1730(3) C9A C 0.6298(4) -0.0503(4) -0.1211(3) H13A H 0.63860 -0.00430 -0.18800 H14A H 0.55990 -0.08980 -0.11670 H15A H 0.59490 -0.00160 -0.07270 C10A C 0.7658(6) -0.1995(4) 0.0083(3) H16A H 0.73600 -0.14580 0.05210 H17A H 0.69200 -0.23670 0.01840 H18A H 0.86050 -0.25610 0.02340 C11A C 0.8140(4) -0.1559(4) -0.2796(3) H19A H 0.70940 -0.13990 -0.28170 H20A H 0.83590 -0.08490 -0.29730 H21A H 0.87200 -0.20350 -0.32680 C12A C 0.8144(9) -0.3257(6) -0.1469(5) H22A H 0.70840 -0.30690 -0.14550 H23A H 0.86630 -0.37140 -0.19660 H24A H 0.84340 -0.36830 -0.08150 C13A C 1.2515(4) -0.2929(2) -0.0346(2) C14A C 1.3234(5) -0.2737(3) 0.0414(3) H25A H 1.25640 -0.26880 0.10310 H26A H 1.41410 -0.33660 0.05420 H27A H 1.34620 -0.20330 0.01620 C15A C 1.3534(4) -0.2977(3) -0.1319(2) H28A H 1.37940 -0.22840 -0.15440 H29A H 1.44270 -0.36280 -0.12160 H30A H 1.30370 -0.30510 -0.18200 C16A C 1.2219(6) -0.4061(3) 0.0018(3) H31A H 1.17780 -0.41870 -0.04870 H32A H 1.31450 -0.46720 0.01370 H33A H 1.15460 -0.40450 0.06350 B1A B 1.1233(3) -0.0737(2) -0.2225(2) B2A B 1.0422(3) -0.1622(3) -0.1353(2) O2A O 1.17062(17) -0.06915(14) -0.32254(12) O3A O 1.13557(19) 0.01788(14) -0.19534(12) O4A O 1.01357(19) -0.25046(14) -0.16895(12) O5A O 1.1153(2) -0.20496(15) -0.04312(12) C17A C 0.1716(3) 0.6932(2) 0.60602(19) H34A H 0.10020 0.67560 0.57790 H35A H 0.11870 0.73150 0.66140 C18A C 0.2288(3) 0.5194(2) 0.72159(19) H36A H 0.17220 0.56120 0.77420 H37A H 0.16280 0.49110 0.69870 C19A C 0.3559(3) 0.4230(2) 0.76117(18) H38A H 0.32020 0.37030 0.81640 H39A H 0.41940 0.45110 0.78660 C20A C 0.5544(3) 0.2681(2) 0.7152(2) H40A H 0.62670 0.28880 0.73940 H41A H 0.51710 0.21600 0.77000 C21A C 0.6254(3) 0.2123(2) 0.6296(2) H42A H 0.55060 0.19890 0.60130 H43A H 0.69890 0.13840 0.65240 C22A C 0.7595(3) 0.2316(2) 0.4718(2) H44A H 0.83480 0.15780 0.49210 H45A H 0.68340 0.21840 0.44470 O6A O 0.28390(17) 0.59160(14) 0.64133(12) O7A O 0.43672(18) 0.36645(14) 0.68352(12) O8A O 0.69505(17) 0.28166(13) 0.55559(12) C23A C 0.6099(3) 0.6357(3) 0.6507(2) H46A H 0.63500 0.69630 0.66610 H47A H 0.50680 0.64270 0.67800 C24A C 0.7109(4) 0.5225(3) 0.6921(2) H48A H 0.74320 0.52220 0.75420 H49A H 0.66390 0.46370 0.70480 C25A C 0.8378(4) 0.5053(3) 0.6099(3) H50A H 0.86690 0.42870 0.59660 H51A H 0.92350 0.51490 0.62860 C26A C 0.7855(3) 0.5907(3) 0.5225(2) H52A H 0.80500 0.55550 0.46470 H53A H 0.83560 0.64800 0.50640 O9A O 0.6316(2) 0.64142(18) 0.54672(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 C1 C2 1.537 1_555 1_555 C2 C5 1.533 1_555 1_555 C3 C1 1.508 1_555 1_555 H1 C3 0.979 1_555 1_555 H2 C3 0.980 1_555 1_555 H3 C3 0.981 1_555 1_555 C4 C1 1.531 1_555 1_555 H4 C4 0.980 1_555 1_555 H5 C4 0.979 1_555 1_555 H6 C4 0.980 1_555 1_555 C5 H7 0.980 1_555 1_555 H8 C5 0.980 1_555 1_555 H9 C5 0.980 1_555 1_555 C6 C2 1.511 1_555 1_555 H10 C6 0.981 1_555 1_555 H11 C6 0.981 1_555 1_555 H12 C6 0.980 1_555 1_555 O1 C7 1.430 1_555 1_555 C7 C8 1.562 1_555 1_555 C8 C11 1.560 1_555 1_555 C9 C7 1.533 1_555 1_555 H13 C9 0.980 1_555 1_555 H14 C9 0.981 1_555 1_555 H15 C9 0.979 1_555 1_555 C10 C7 1.527 1_555 1_555 H16 C10 0.980 1_555 1_555 H17 C10 0.979 1_555 1_555 H18 C10 0.980 1_555 1_555 C11 H19 0.980 1_555 1_555 H20 C11 0.981 1_555 1_555 H21 C11 0.979 1_555 1_555 C12 C8 1.515 1_555 1_555 H22 C12 0.980 1_555 1_555 H23 C12 0.979 1_555 1_555 H24 C12 0.981 1_555 1_555 C13 C14 1.513 1_555 1_555 C14 H25 0.980 1_555 1_555 H26 C14 0.980 1_555 1_555 H27 C14 0.979 1_555 1_555 C15 C13 1.527 1_555 1_555 H28 C15 0.980 1_555 1_555 H29 C15 0.981 1_555 1_555 H30 C15 0.979 1_555 1_555 C16 C13 1.538 1_555 1_555 H31 C16 0.980 1_555 1_555 H32 C16 0.980 1_555 1_555 H33 C16 0.980 1_555 1_555 B1 B2 1.729 1_555 1_555 B2 O1 1.526 1_555 1_555 O2 C1 1.449 1_555 1_555 O3 C2 1.453 1_555 1_555 O4 C8 1.489 1_555 1_555 O5 C13 1.417 1_555 1_555 K1 O1 2.729 1_555 1_555 C17 H34 0.991 1_555 1_555 H35 C17 0.990 1_555 1_555 C18 H36 0.991 1_555 1_555 H37 C18 0.991 1_555 1_555 C19 C18 1.495 1_555 1_555 H38 C19 0.990 1_555 1_555 H39 C19 0.989 1_555 1_555 C20 H40 0.991 1_555 1_555 H41 C20 0.989 1_555 1_555 C21 C20 1.491 1_555 1_555 H42 C21 0.990 1_555 1_555 H43 C21 0.991 1_555 1_555 C22 H44 0.991 1_555 1_555 H45 C22 0.990 1_555 1_555 C23 H46 0.991 1_555 1_555 H47 C23 0.990 1_555 1_555 C24 C23 1.492 1_555 1_555 H48 C24 0.989 1_555 1_555 H49 C24 0.990 1_555 1_555 C25 C24 1.516 1_555 1_555 H50 C25 0.990 1_555 1_555 H51 C25 0.991 1_555 1_555 C26 C25 1.463 1_555 1_555 H52 C26 0.989 1_555 1_555 H53 C26 0.990 1_555 1_555 O6 C17 1.429 1_555 1_555 O7 C19 1.421 1_555 1_555 O8 C21 1.425 1_555 1_555 O9 C23 1.423 1_555 1_555 K2 O6 2.759 1_555 1_555 C1A C2A 1.537 1_555 1_555 C2A C5A 1.533 1_555 1_555 C3A C1A 1.508 1_555 1_555 H1A C3A 0.979 1_555 1_555 H2A C3A 0.980 1_555 1_555 H3A C3A 0.981 1_555 1_555 C4A C1A 1.531 1_555 1_555 H4A C4A 0.980 1_555 1_555 H5A C4A 0.979 1_555 1_555 H6A C4A 0.980 1_555 1_555 C5A H7A 0.980 1_555 1_555 H8A C5A 0.980 1_555 1_555 H9A C5A 0.980 1_555 1_555 C6A C2A 1.511 1_555 1_555 H10A C6A 0.981 1_555 1_555 H11A C6A 0.981 1_555 1_555 H12A C6A 0.980 1_555 1_555 O1A K1 2.729 1_555 1_555 C7A O1A 1.430 1_555 1_555 C8A C7A 1.562 1_555 1_555 C9A C7A 1.533 1_555 1_555 H13A C9A 0.980 1_555 1_555 H14A C9A 0.981 1_555 1_555 H15A C9A 0.979 1_555 1_555 C10A C7A 1.527 1_555 1_555 H16A C10A 0.980 1_555 1_555 H17A C10A 0.979 1_555 1_555 H18A C10A 0.980 1_555 1_555 C11A C8A 1.560 1_555 1_555 H19A C11A 0.980 1_555 1_555 H20A C11A 0.981 1_555 1_555 H21A C11A 0.979 1_555 1_555 C12A C8A 1.515 1_555 1_555 H22A C12A 0.980 1_555 1_555 H23A C12A 0.979 1_555 1_555 H24A C12A 0.981 1_555 1_555 C13A C14A 1.513 1_555 1_555 C14A H25A 0.980 1_555 1_555 H26A C14A 0.980 1_555 1_555 H27A C14A 0.979 1_555 1_555 C15A C13A 1.527 1_555 1_555 H28A C15A 0.980 1_555 1_555 H29A C15A 0.981 1_555 1_555 H30A C15A 0.979 1_555 1_555 C16A C13A 1.538 1_555 1_555 H31A C16A 0.980 1_555 1_555 H32A C16A 0.980 1_555 1_555 H33A C16A 0.980 1_555 1_555 B1A B2A 1.729 1_555 1_555 B2A O1A 1.526 1_555 1_555 O2A C1A 1.449 1_555 1_555 O3A K1 2.793 1_555 1_555 O4A C8A 1.489 1_555 1_555 O5A K1 2.674 1_555 1_555 C17A C22 1.493 1_555 1_555 H34A C17A 0.991 1_555 1_555 H35A C17A 0.990 1_555 1_555 C18A H36A 0.991 1_555 1_555 H37A C18A 0.991 1_555 1_555 C19A C18A 1.495 1_555 1_555 H38A C19A 0.990 1_555 1_555 H39A C19A 0.989 1_555 1_555 C20A H40A 0.991 1_555 1_555 H41A C20A 0.989 1_555 1_555 C21A C20A 1.491 1_555 1_555 H42A C21A 0.990 1_555 1_555 H43A C21A 0.991 1_555 1_555 C22A C17 1.493 1_555 1_555 H44A C22A 0.991 1_555 1_555 H45A C22A 0.990 1_555 1_555 O6A K2 2.759 1_555 1_555 O7A K2 2.802 1_555 1_555 O8A K2 2.806 1_555 1_555 C23A H46A 0.991 1_555 1_555 H47A C23A 0.990 1_555 1_555 C24A C23A 1.492 1_555 1_555 H48A C24A 0.989 1_555 1_555 H49A C24A 0.990 1_555 1_555 C25A C24A 1.516 1_555 1_555 H50A C25A 0.990 1_555 1_555 H51A C25A 0.991 1_555 1_555 C26A C25A 1.463 1_555 1_555 H52A C26A 0.989 1_555 1_555 H53A C26A 0.990 1_555 1_555 O9A K2 2.863 1_555 1_555 B1 O2 1.384 1_555 1_555 B1 O3 1.393 1_555 1_555 B2 O4 1.482 1_555 1_555 B2 O5 1.492 1_555 1_555 O3 K1 2.793 1_555 1_555 O5 K1 2.674 1_555 1_555 C18 O6 1.419 1_555 1_555 C20 O7 1.421 1_555 1_555 C22 O8 1.422 1_555 1_555 C26 O9 1.427 1_555 1_555 O7 K2 2.802 1_555 1_555 O8 K2 2.806 1_555 1_555 O9 K2 2.863 1_555 1_555 C2A O3A 1.453 1_555 1_555 C13A O5A 1.417 1_555 1_555 B1A O2A 1.384 1_555 1_555 B1A O3A 1.393 1_555 1_555 B2A O4A 1.482 1_555 1_555 B2A O5A 1.492 1_555 1_555 C17A O6A 1.429 1_555 1_555 C18A O6A 1.419 1_555 1_555 C19A O7A 1.421 1_555 1_555 C20A O7A 1.421 1_555 1_555 C21A O8A 1.425 1_555 1_555 C22A O8A 1.422 1_555 1_555 C23A O9A 1.423 1_555 1_555 C26A O9A 1.427 1_555 1_555 #END data_CSD_CIF_NAKCUX _audit_creation_date 1997-01-09 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD NAKCUX _database_code_depnum_ccdc_archive 'CCDC 1216260' _database_code_depnum_ccdc_journal 182/202 _chemical_formula_sum 'C114 H132 Li8 N12 O36 Ti4' _chemical_formula_moiety ; 2(C48 H45 Li3 N3 O15 Ti2 1-),C18 H42 Li2 N6 O6 2+ ; _journal_coden_Cambridge 182 _journal_year 1996 _journal_page_first 2309 _journal_name_full 'Chem.Commun. ' loop_ _publ_author_name "M.Albrecht" "S.Kotila" _chemical_name_systematic ; bis(tris(\m~4~-bis(2,3-Dihydroxyphenyl)methane)-tris(dimethylformamide)-di-tit anium-tri-lithium) bis(\m~2~-dimethylformamide)-tetrakis(dimethylformamide)-di-lithium ; _cell_volume 2957.017 _exptl_crystal_colour 'red' _exptl_crystal_density_diffrn 1.4 _diffrn_ambient_temperature 173 _refine_special_details ; Three dimethylformamide were refined over two positions with occupancies 0.52:0.48 and 0.557;0.443. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_gt 0.0371 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 12.524(2) _cell_length_b 12.562(1) _cell_length_c 22.425(2) _cell_angle_alpha 75.97(1) _cell_angle_beta 73.91(1) _cell_angle_gamma 61.63(1) _cell_formula_units_Z 1 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.35 N 0.68 O 0.68 Ti 1.47 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Ti1 Ti 0.73950(4) 0.80807(4) 0.32879(2) Ti2 Ti 0.83758(4) 0.79211(4) 0.07639(2) C1 C 0.5674(2) 0.6243(2) 0.28719(12) C2 C 0.6037(2) 0.6958(2) 0.30800(11) O1 O 0.70593(15) 0.71478(15) 0.28071(8) C3 C 0.5372(2) 0.7525(2) 0.36217(11) O2 O 0.5872(2) 0.8123(2) 0.37888(8) C4 C 0.4299(2) 0.7435(3) 0.39522(12) H1 H 0.3846(2) 0.7823(3) 0.43171(12) C5 C 0.3904(2) 0.6759(3) 0.37335(14) H2 H 0.3159(2) 0.6703(3) 0.39466(14) C6 C 0.4582(2) 0.6167(3) 0.32088(13) H3 H 0.4299(2) 0.5700(3) 0.30748(13) C7 C 0.6467(2) 0.5497(2) 0.23388(12) H4 H 0.7343(2) 0.5278(2) 0.23274(12) H5 H 0.6380(2) 0.4728(2) 0.24290(12) C8 C 0.6171(2) 0.6115(2) 0.16976(12) C9 C 0.6735(2) 0.6835(2) 0.13206(11) O3 O 0.7524(2) 0.7104(2) 0.14948(8) C10 C 0.6513(2) 0.7350(2) 0.07092(11) O4 O 0.7158(2) 0.7981(2) 0.03854(8) C11 C 0.5665(3) 0.7202(3) 0.04886(13) H6 H 0.5485(3) 0.7578(3) 0.00838(13) C12 C 0.5079(3) 0.6494(3) 0.08658(14) H7 H 0.4506(3) 0.6381(3) 0.07161(14) C13 C 0.5336(2) 0.5960(2) 0.14579(14) H8 H 0.4937(2) 0.5476(2) 0.17089(14) C14 C 1.1235(2) 0.6279(2) 0.26449(12) C15 C 1.0002(2) 0.6712(2) 0.29493(11) O5 O 0.90269(15) 0.7563(2) 0.26816(8) C16 C 0.9671(2) 0.6299(2) 0.35839(12) O6 O 0.8454(2) 0.6829(2) 0.38258(8) C17 C 1.0569(3) 0.5425(3) 0.39170(14) H9 H 1.0350(3) 0.5149(3) 0.43458(14) C18 C 1.1804(3) 0.4957(3) 0.36080(15) H10 H 1.2428(3) 0.4341(3) 0.38257(15) C19 C 1.2123(2) 0.5382(3) 0.29918(14) H11 H 1.2969(2) 0.5059(3) 0.27948(14) C20 C 1.1619(2) 0.6784(2) 0.19800(12) H12 H 1.2448(2) 0.6740(2) 0.19342(12) H13 H 1.1034(2) 0.7656(2) 0.19056(12) C21 C 1.1661(2) 0.6126(2) 0.14821(11) C22 C 1.0648(2) 0.6515(2) 0.12077(11) O7 O 0.95267(14) 0.74583(15) 0.13681(8) C23 C 1.0725(2) 0.5949(2) 0.07168(11) O8 O 0.9708(2) 0.6495(2) 0.04540(8) C24 C 1.1794(2) 0.4930(2) 0.05268(12) H14 H 1.1838(2) 0.4524(2) 0.02079(12) C25 C 1.2797(2) 0.4519(2) 0.08145(13) H15 H 1.3532(2) 0.3819(2) 0.06927(13) C26 C 1.2743(2) 0.5111(2) 0.12746(12) H16 H 1.3451(2) 0.4827(2) 0.14542(12) C27 C 0.5953(2) 1.1639(2) 0.23460(12) C28 C 0.6521(2) 1.0546(2) 0.27135(11) O9 O 0.6826(2) 0.94239(14) 0.25810(8) C29 C 0.6792(2) 1.0520(2) 0.32903(11) O10 O 0.7281(2) 0.9400(2) 0.36156(8) C30 C 0.6529(3) 1.1593(3) 0.34917(13) H17 H 0.6734(3) 1.1577(3) 0.38723(13) C31 C 0.5960(3) 1.2692(2) 0.31253(13) H18 H 0.5763(3) 1.3437(2) 0.32594(13) C32 C 0.5678(3) 1.2712(2) 0.25656(13) H19 H 0.5287(3) 1.3476(2) 0.23238(13) C33 C 0.5573(2) 1.1690(2) 0.17510(12) H20 H 0.4847(2) 1.2483(2) 0.16888(12) H21 H 0.5298(2) 1.1043(2) 0.18170(12) C34 C 0.6533(2) 1.1546(2) 0.11470(11) C35 C 0.7304(2) 1.0413(2) 0.09445(11) O11 O 0.73604(15) 0.93295(15) 0.12776(8) C36 C 0.8091(2) 1.0305(2) 0.03569(11) O12 O 0.8727(2) 0.9159(2) 0.02011(8) C37 C 0.8172(2) 1.1332(2) -0.00222(12) H22 H 0.8732(2) 1.1258(2) -0.04122(12) C38 C 0.7418(3) 1.2464(3) 0.01821(13) H23 H 0.7458(3) 1.3173(3) -0.00728(13) C39 C 0.6606(2) 1.2575(2) 0.07541(13) H24 H 0.6091(2) 1.3361(2) 0.08818(13) Li1 Li 0.8528(4) 0.6487(4) 0.2139(2) O13 O 0.9487(2) 0.4825(2) 0.23861(10) C40 C 1.0567(12) 0.4089(24) 0.2243(12) H25 H 1.1018(12) 0.4220(24) 0.1838(12) N1 N 1.1130(11) 0.3114(18) 0.2633(9) C41 C 1.0503(16) 0.2932(18) 0.3272(9) H26 H 1.1022(29) 0.2806(55) 0.3563(9) H27 H 1.0351(50) 0.2213(37) 0.3330(13) H28 H 0.9714(30) 0.3653(29) 0.3354(12) C42 C 1.2427(11) 0.2301(16) 0.2447(12) H29 H 1.2546(17) 0.1453(16) 0.2553(38) H30 H 1.2924(14) 0.2429(57) 0.2667(33) H31 H 1.2686(24) 0.2474(56) 0.1994(14) Li2 Li 0.8744(4) 0.8794(4) 0.1898(2) O14 O 0.9294(2) 1.0003(2) 0.18081(9) C43 C 0.9314(2) 1.0878(2) 0.14151(13) H32 H 0.9385(2) 1.0821(2) 0.09898(13) N2 N 0.9243(2) 1.1884(2) 0.15403(11) C44 C 0.9057(3) 1.2063(3) 0.21801(15) H33 H 0.8396(16) 1.2880(9) 0.2250(3) H34 H 0.9823(7) 1.1985(22) 0.2260(4) H35 H 0.8826(22) 1.1447(14) 0.24645(15) C45 C 0.9276(4) 1.2877(3) 0.1055(2) H36 H 0.9972(15) 1.3029(16) 0.1059(8) H37 H 0.8502(11) 1.3615(7) 0.1131(7) H38 H 0.9378(25) 1.2656(10) 0.0645(2) Li3 Li 0.6381(4) 0.8770(4) 0.2012(2) O15 O 0.4724(2) 0.9350(2) 0.19463(9) C46 C 0.4043(21) 0.9242(13) 0.1673(10) H39 H 0.4049(21) 0.8461(13) 0.1761(10) N3 N 0.3329(10) 1.0021(7) 0.1289(6) C47 C 0.2679(20) 0.9687(18) 0.0977(10) H40 H 0.2954(43) 0.9813(53) 0.0523(10) H41 H 0.1788(20) 1.0195(39) 0.1085(23) H42 H 0.2857(47) 0.8826(23) 0.1112(23) C48 C 0.3071(10) 1.1298(6) 0.1192(4) H43 H 0.2298(29) 1.1748(11) 0.1469(19) H44 H 0.2992(52) 1.1634(15) 0.0755(8) H45 H 0.3749(26) 1.1374(8) 0.1285(26) Li4 Li 0.8919(5) 1.0125(5) 0.4878(2) O16 O 0.8302(3) 0.8992(3) 0.51439(12) C49 C 0.7758(3) 0.8468(4) 0.50430(14) H46 H 0.8114(3) 0.8030(4) 0.46922(14) N4 N 0.6719(2) 0.8480(2) 0.53911(12) C50 C 0.6125(4) 0.7850(4) 0.5240(2) H47 H 0.5311(12) 0.8445(5) 0.5147(14) H48 H 0.6029(26) 0.7253(20) 0.5597(6) H49 H 0.6637(14) 0.7429(23) 0.4874(9) C51 C 0.6105(4) 0.9140(5) 0.5924(3) H50 H 0.6206(34) 0.8561(5) 0.6310(3) H51 H 0.5224(9) 0.9621(31) 0.5911(11) H52 H 0.6468(27) 0.9685(29) 0.5914(11) O17 O 1.0559(2) 0.9769(2) 0.43789(9) C52 C 1.1229(3) 0.9594(2) 0.38569(13) H53 H 1.1983(3) 0.9656(2) 0.37836(13) N5 N 1.0978(2) 0.9331(2) 0.33968(11) C53 C 0.9852(3) 0.9199(4) 0.3475(2) H54 H 0.9944(9) 0.8412(11) 0.3723(10) H55 H 0.9698(13) 0.9237(24) 0.3064(2) H56 H 0.9154(5) 0.9861(14) 0.3692(11) C54 C 1.1874(3) 0.9049(4) 0.28111(15) H57 H 1.1479(8) 0.9574(17) 0.2458(2) H58 H 1.2170(19) 0.8192(7) 0.2766(6) H59 H 1.2574(12) 0.9194(24) 0.2817(6) O18 O 0.7914(2) 1.1785(2) 0.46117(11) C55 C 0.8155(4) 1.2575(4) 0.4702(2) H60 H 0.8867(4) 1.2318(4) 0.4874(2) N6 N 0.7470(9) 1.3756(4) 0.4572(7) C56 C 0.6374(8) 1.4172(6) 0.4312(5) H61 H 0.6622(8) 1.3980(63) 0.3881(13) H62 H 0.5892(38) 1.5056(13) 0.4312(34) H63 H 0.5870(35) 1.3759(53) 0.4566(21) C57 C 0.7720(8) 1.4662(6) 0.4719(4) H64 H 0.7066(31) 1.5083(39) 0.5056(20) H65 H 0.7746(58) 1.5256(33) 0.4347(9) H66 H 0.8518(28) 1.4264(9) 0.4855(28) C58? C 1.0578(12) 0.4091(29) 0.2357(12) H67? H 1.1141(12) 0.4183(29) 0.1988(12) N7? N 1.1039(13) 0.3178(21) 0.2798(10) C59? C 1.0226(25) 0.2956(27) 0.3364(11) H68? H 1.0241(67) 0.3318(72) 0.3701(15) H69? H 1.0507(49) 0.2075(27) 0.3486(25) H70? H 0.9382(27) 0.3326(70) 0.3287(15) C60? C 1.2368(13) 0.2454(13) 0.2743(11) H71? H 1.2571(14) 0.1589(14) 0.2773(34) H72? H 1.2640(17) 0.2573(53) 0.3081(23) H73? H 1.2787(13) 0.2711(45) 0.2338(18) C61? C 0.4223(28) 0.9011(17) 0.1669(13) H74? H 0.4247(28) 0.8222(17) 0.1778(13) N8? N 0.3668(13) 0.9784(11) 0.1226(8) C62? C 0.2927(25) 0.9546(28) 0.0925(14) H75? H 0.3463(27) 0.9056(68) 0.0586(29) H76? H 0.2310(54) 1.0321(28) 0.0754(36) H77? H 0.2506(66) 0.9099(73) 0.1233(17) C63? C 0.4032(13) 1.0740(11) 0.0890(5) H78? H 0.3367(30) 1.1384(34) 0.0681(29) H79? H 0.4784(40) 1.0398(18) 0.0577(24) H80? H 0.4190(68) 1.1084(48) 0.1186(7) C64? C 0.7403(10) 1.2909(7) 0.4451(5) H81? H 0.6731(10) 1.3230(7) 0.4239(5) N9? N 0.7748(23) 1.3671(7) 0.4559(18) C65? C 0.8789(10) 1.3238(11) 0.4866(6) H82? H 0.8906(10) 1.3934(11) 0.4905(6) H83? H 0.9538(10) 1.2678(11) 0.4616(6) H84? H 0.8625(10) 1.2810(11) 0.5283(6) C66? C 0.7039(16) 1.4981(7) 0.443(1) H85? H 0.7440(16) 1.5395(7) 0.454(1) H86? H 0.6201(16) 1.5226(7) 0.4679(10) H87? H 0.6999(16) 1.5208(7) 0.3984(10) Li4A Li 1.1081(5) 0.9875(5) 0.5122(2) O16A O 1.1698(3) 1.1008(3) 0.48561(12) C49A C 1.2242(3) 1.1532(4) 0.49570(14) H46A H 1.1886(3) 1.1970(4) 0.53078(14) N4A N 1.3281(2) 1.1520(2) 0.46089(12) C50A C 1.3875(4) 1.2150(4) 0.4760(2) H47A H 1.4689(12) 1.1555(5) 0.4853(14) H48A H 1.3971(26) 1.2747(20) 0.4403(6) H49A H 1.3363(14) 1.2571(23) 0.5126(9) C51A C 1.3895(4) 1.0860(5) 0.4076(3) H50A H 1.3794(34) 1.1439(5) 0.3690(3) H51A H 1.4776(9) 1.0379(31) 0.4089(11) H52A H 1.3532(27) 1.0315(29) 0.4086(11) O17A O 0.9441(2) 1.0231(2) 0.56211(9) O18A O 1.2086(2) 0.8215(2) 0.53883(11) C55A C 1.1845(4) 0.7425(4) 0.5298(2) H60A H 1.1133(4) 0.7682(4) 0.5126(2) N6A N 1.2530(9) 0.6244(4) 0.5428(7) C56A C 1.3626(8) 0.5828(6) 0.5688(5) H61A H 1.3378(8) 0.6020(63) 0.6119(13) H62A H 1.4108(38) 0.4944(13) 0.5688(34) H63A H 1.4130(35) 0.6241(53) 0.5434(21) C57A C 1.2280(8) 0.5338(6) 0.5281(4) H64A H 1.2934(31) 0.4917(39) 0.4944(20) H65A H 1.2254(58) 0.4744(33) 0.5653(9) H66A H 1.1482(28) 0.5736(9) 0.5145(28) C52A C 0.8771(3) 1.0406(2) 0.61431(13) H53A H 0.8017(3) 1.0344(2) 0.62164(13) N5A N 0.9022(2) 1.0669(2) 0.66032(11) C53A C 1.0148(3) 1.0801(4) 0.6525(2) H54A H 1.0056(9) 1.1588(11) 0.6277(10) H55A H 1.0302(13) 1.0763(24) 0.6936(2) H56A H 1.0846(5) 1.0139(14) 0.6308(11) C54A C 0.8126(3) 1.0951(4) 0.71889(15) H57A H 0.8521(8) 1.0426(17) 0.7542(2) H58A H 0.7830(19) 1.1808(7) 0.7234(6) H59A H 0.7426(12) 1.0806(24) 0.7183(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ti1 O1 2.011 1_555 1_555 Ti2 O3 2.033 1_555 1_555 C1 C2 1.393 1_555 1_555 C2 O1 1.362 1_555 1_555 O1 Li1 1.985 1_555 1_555 C3 C2 1.404 1_555 1_555 O2 Ti1 1.910 1_555 1_555 C4 C3 1.386 1_555 1_555 H1 C4 0.950 1_555 1_555 C5 C4 1.394 1_555 1_555 H2 C5 0.950 1_555 1_555 C6 C1 1.402 1_555 1_555 H3 C6 0.950 1_555 1_555 C7 C1 1.515 1_555 1_555 H4 C7 0.990 1_555 1_555 H5 C7 0.989 1_555 1_555 C8 C7 1.513 1_555 1_555 C9 C8 1.392 1_555 1_555 O3 C9 1.356 1_555 1_555 C10 C9 1.409 1_555 1_555 O4 Ti2 1.905 1_555 1_555 C11 C10 1.389 1_555 1_555 H6 C11 0.950 1_555 1_555 C12 C11 1.399 1_555 1_555 H7 C12 0.949 1_555 1_555 C13 C8 1.406 1_555 1_555 H8 C13 0.950 1_555 1_555 C14 C15 1.394 1_555 1_555 C15 O5 1.360 1_555 1_555 O5 Ti1 2.018 1_555 1_555 C16 C15 1.409 1_555 1_555 O6 Ti1 1.916 1_555 1_555 C17 C16 1.387 1_555 1_555 H9 C17 0.950 1_555 1_555 C18 C17 1.399 1_555 1_555 H10 C18 0.949 1_555 1_555 C19 C14 1.405 1_555 1_555 H11 C19 0.949 1_555 1_555 C20 C14 1.514 1_555 1_555 H12 C20 0.990 1_555 1_555 H13 C20 0.990 1_555 1_555 C21 C20 1.519 1_555 1_555 C22 C21 1.387 1_555 1_555 O7 Ti2 2.039 1_555 1_555 C23 C22 1.408 1_555 1_555 O8 Ti2 1.896 1_555 1_555 C24 C23 1.390 1_555 1_555 H14 C24 0.950 1_555 1_555 C25 C24 1.390 1_555 1_555 H15 C25 0.950 1_555 1_555 C26 C21 1.405 1_555 1_555 H16 C26 0.950 1_555 1_555 C27 C28 1.385 1_555 1_555 C28 O9 1.360 1_555 1_555 O9 Ti1 2.014 1_555 1_555 C29 C28 1.415 1_555 1_555 O10 Ti1 1.901 1_555 1_555 C30 C29 1.386 1_555 1_555 H17 C30 0.950 1_555 1_555 C31 C30 1.389 1_555 1_555 H18 C31 0.950 1_555 1_555 C32 C27 1.402 1_555 1_555 H19 C32 0.950 1_555 1_555 C33 C27 1.514 1_555 1_555 H20 C33 0.990 1_555 1_555 H21 C33 0.990 1_555 1_555 C34 C33 1.524 1_555 1_555 C35 C34 1.389 1_555 1_555 O11 Ti2 2.028 1_555 1_555 C36 C35 1.402 1_555 1_555 O12 Ti2 1.896 1_555 1_555 C37 C36 1.394 1_555 1_555 H22 C37 0.950 1_555 1_555 C38 C37 1.387 1_555 1_555 H23 C38 0.950 1_555 1_555 C39 C34 1.404 1_555 1_555 H24 C39 0.950 1_555 1_555 Li1 O3 1.951 1_555 1_555 O13 Li1 1.880 1_555 1_555 C40 O13 1.226 1_555 1_555 H25 C40 0.950 1_555 1_555 N1 C40 1.328 1_555 1_555 C41 N1 1.453 1_555 1_555 H26 C41 0.980 1_555 1_555 H27 C41 0.981 1_555 1_555 H28 C41 0.980 1_555 1_555 C42 N1 1.453 1_555 1_555 H29 C42 0.980 1_555 1_555 H30 C42 0.980 1_555 1_555 H31 C42 0.981 1_555 1_555 Li2 O5 2.028 1_555 1_555 O14 Li2 1.895 1_555 1_555 C43 O14 1.237 1_555 1_555 H32 C43 0.950 1_555 1_555 N2 C43 1.317 1_555 1_555 C44 N2 1.444 1_555 1_555 H33 C44 0.981 1_555 1_555 H34 C44 0.980 1_555 1_555 H35 C44 0.980 1_555 1_555 C45 N2 1.452 1_555 1_555 H36 C45 0.980 1_555 1_555 H37 C45 0.979 1_555 1_555 H38 C45 0.982 1_555 1_555 Li3 O1 2.342 1_555 1_555 O15 Li3 1.881 1_555 1_555 C46 O15 1.250 1_555 1_555 H39 C46 0.949 1_555 1_555 N3 C46 1.298 1_555 1_555 C47 N3 1.453 1_555 1_555 H40 C47 0.980 1_555 1_555 H41 C47 0.980 1_555 1_555 H42 C47 0.980 1_555 1_555 C48 N3 1.450 1_555 1_555 H43 C48 0.980 1_555 1_555 H44 C48 0.981 1_555 1_555 H45 C48 0.979 1_555 1_555 Li4 O16 1.832 1_555 1_555 O16 C49 1.238 1_555 1_555 C49 H46 0.950 1_555 1_555 N4 C49 1.314 1_555 1_555 C50 N4 1.457 1_555 1_555 H47 C50 0.980 1_555 1_555 H48 C50 0.979 1_555 1_555 H49 C50 0.980 1_555 1_555 C51 N4 1.439 1_555 1_555 H50 C51 0.981 1_555 1_555 H51 C51 0.979 1_555 1_555 H52 C51 0.979 1_555 1_555 O17 Li4 1.941 1_555 1_555 C52 O17 1.236 1_555 1_555 H53 C52 0.950 1_555 1_555 N5 C52 1.310 1_555 1_555 C53 N5 1.455 1_555 1_555 H54 C53 0.980 1_555 1_555 H55 C53 0.978 1_555 1_555 H56 C53 0.981 1_555 1_555 C54 N5 1.463 1_555 1_555 H57 C54 0.980 1_555 1_555 H58 C54 0.979 1_555 1_555 H59 C54 0.980 1_555 1_555 O18 Li4 1.899 1_555 1_555 C55 O18 1.238 1_555 1_555 H60 C55 0.951 1_555 1_555 N6 C55 1.320 1_555 1_555 C56 N6 1.453 1_555 1_555 H61 C56 0.982 1_555 1_555 H62 C56 0.980 1_555 1_555 H63 C56 0.980 1_555 1_555 C57 N6 1.442 1_555 1_555 H64 C57 0.980 1_555 1_555 H65 C57 0.980 1_555 1_555 H66 C57 0.981 1_555 1_555 Li4A O17 2.004 1_555 1_555 O16A Li4A 1.832 1_555 1_555 C49A O16A 1.238 1_555 1_555 H46A C49A 0.950 1_555 1_555 N4A C49A 1.314 1_555 1_555 C50A N4A 1.457 1_555 1_555 H47A C50A 0.980 1_555 1_555 H48A C50A 0.979 1_555 1_555 H49A C50A 0.980 1_555 1_555 C51A N4A 1.439 1_555 1_555 H50A C51A 0.981 1_555 1_555 H51A C51A 0.979 1_555 1_555 H52A C51A 0.979 1_555 1_555 O17A Li4 2.004 1_555 1_555 O18A Li4A 1.899 1_555 1_555 C55A O18A 1.238 1_555 1_555 H60A C55A 0.951 1_555 1_555 N6A C55A 1.320 1_555 1_555 C56A N6A 1.453 1_555 1_555 H61A C56A 0.982 1_555 1_555 H62A C56A 0.980 1_555 1_555 H63A C56A 0.980 1_555 1_555 C57A N6A 1.442 1_555 1_555 H64A C57A 0.980 1_555 1_555 H65A C57A 0.980 1_555 1_555 H66A C57A 0.981 1_555 1_555 C52A O17A 1.236 1_555 1_555 H53A C52A 0.950 1_555 1_555 N5A C52A 1.310 1_555 1_555 C53A N5A 1.455 1_555 1_555 H54A C53A 0.980 1_555 1_555 H55A C53A 0.978 1_555 1_555 H56A C53A 0.981 1_555 1_555 C54A N5A 1.463 1_555 1_555 H57A C54A 0.980 1_555 1_555 H58A C54A 0.979 1_555 1_555 H59A C54A 0.980 1_555 1_555 C3 O2 1.346 1_555 1_555 C5 C6 1.389 1_555 1_555 O3 Li3 2.277 1_555 1_555 C10 O4 1.346 1_555 1_555 C12 C13 1.384 1_555 1_555 O5 Li1 2.392 1_555 1_555 C16 O6 1.347 1_555 1_555 C18 C19 1.376 1_555 1_555 C22 O7 1.360 1_555 1_555 O7 Li1 2.296 1_555 1_555 O7 Li2 1.987 1_555 1_555 C23 O8 1.353 1_555 1_555 C25 C26 1.381 1_555 1_555 O9 Li2 2.342 1_555 1_555 O9 Li3 1.988 1_555 1_555 C29 O10 1.348 1_555 1_555 C31 C32 1.387 1_555 1_555 C35 O11 1.364 1_555 1_555 O11 Li2 2.273 1_555 1_555 O11 Li3 1.962 1_555 1_555 C36 O12 1.352 1_555 1_555 C38 C39 1.388 1_555 1_555 Li4A O17A 1.941 1_555 1_555 #END data_CSD_CIF_OBABOK _audit_creation_date 2011-11-29 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD OBABOK _database_code_depnum_ccdc_archive 'CCDC 827712' _chemical_formula_sum 'C22 H38 Li2 O6' _chemical_formula_moiety ; C12 H28 Li1 O6 1+,C10 H10 Li1 1- ; _journal_coden_Cambridge 579 _journal_volume 30 _journal_year 2011 _journal_page_first 4379 _journal_name_full 'Organometallics ' loop_ _publ_author_name "R.Michel" "R.Herbst-Irmer" "D.Stalke" _chemical_name_systematic ; bis(bis(2-Methoxyethyl) ether)-lithium bis(\h^5^-cyclopentadienyl)-lithium ; _cell_volume 1231.073 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.113 _exptl_crystal_description 'block' _diffrn_ambient_temperature 100 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_gt 0.0353 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 8.619(2) _cell_length_b 9.165(2) _cell_length_c 16.009(3) _cell_angle_alpha 89.43(2) _cell_angle_beta 79.81(2) _cell_angle_gamma 81.58(2) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.34 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.50000 1.00000 0.50000 C1 C 0.85751(10) 0.21999(9) 0.04323(6) H1 H 0.91060 0.30430 0.03850 C2 C 0.72280(9) 0.03798(9) 0.01224(6) H2 H 0.66880 -0.02260 -0.01710 C3 C 0.78760(9) 0.16366(10) -0.02006(5) H3 H 0.78460 0.20330 -0.07490 C4 C 0.75211(10) 0.01791(10) 0.09566(6) H4 H 0.72090 -0.05840 0.13260 C5 C 0.83541(10) 0.13027(11) 0.11474(6) H5 H 0.87060 0.14330 0.16680 C6 C 0.77271(9) 0.93766(9) 0.47349(5) H6 H 0.83110 0.93950 0.51840 C7 C 0.73336(9) 1.05656(9) 0.42076(5) H7 H 0.76050 1.15290 0.42420 C8 C 0.70975(9) 0.81553(9) 0.44742(5) H8 H 0.71820 0.72040 0.47190 C9 C 0.64703(9) 1.00798(9) 0.36224(5) H9 H 0.60610 1.06550 0.31920 C10 C 0.63213(9) 0.85915(9) 0.37877(5) H10 H 0.57910 0.79860 0.34890 O1 O 0.37414(7) 0.32499(6) 0.20006(4) C11 C 0.45959(10) 0.33724(9) 0.11553(5) H11 H 0.38510 0.35210 0.07470 H12 H 0.53660 0.24680 0.09880 C12 C 0.54502(9) 0.46819(9) 0.11723(5) H13 H 0.62720 0.44850 0.15360 H14 H 0.59810 0.48900 0.05920 C13 C 0.28498(11) 0.20525(9) 0.21000(6) H15 H 0.35700 0.11010 0.20000 H16 H 0.21020 0.21250 0.16930 O2 O 0.42981(6) 0.59113(6) 0.15023(4) O3 O 0.11406(7) 0.36341(6) 0.31265(4) C14 C 0.50048(11) 0.72094(10) 0.15374(6) H17 H 0.58140 0.70460 0.19010 H18 H 0.41830 0.80280 0.17710 H19 H 0.55050 0.74510 0.09640 C15 C 0.00938(11) 0.38458(10) 0.39207(6) H20 H -0.07580 0.32400 0.39370 H21 H -0.03720 0.48880 0.39950 H22 H 0.06890 0.35550 0.43790 C16 C 0.19481(11) 0.21601(9) 0.30000(6) H23 H 0.11730 0.14510 0.30860 H24 H 0.26930 0.19380 0.34050 Li2 Li 0.25671(16) 0.52300(15) 0.24901(9) O4 O 0.07462(6) 0.60511(6) 0.17993(4) O5 O 0.13145(6) 0.69351(6) 0.32514(4) O6 O 0.41035(7) 0.55028(6) 0.34170(4) C17 C 0.32009(9) 0.63260(9) 0.41356(5) H25 H 0.39190 0.67130 0.44700 H26 H 0.25420 0.56930 0.45060 C18 C -0.04525(9) 0.70894(9) 0.22922(5) H27 H -0.12260 0.65690 0.26680 H28 H -0.10340 0.77390 0.19160 C19 C 0.21531(9) 0.75787(9) 0.38046(5) H29 H 0.13980 0.81150 0.42790 H30 H 0.28070 0.82810 0.34940 C20 C 0.03684(9) 0.79838(8) 0.28106(5) H31 H 0.10500 0.85970 0.24390 H32 H -0.04220 0.86390 0.32170 C21 C 0.00736(11) 0.51329(11) 0.12967(6) H33 H -0.05900 0.45220 0.16680 H34 H 0.09290 0.44960 0.09280 H35 H -0.05820 0.57470 0.09480 C22 C 0.52698(11) 0.43769(10) 0.36436(6) H36 H 0.60400 0.48270 0.39010 H37 H 0.58250 0.38110 0.31340 H38 H 0.47480 0.37180 0.40510 Li3 Li 1.00000 0.00000 0.00000 C1A C 1.14249(10) -0.21999(9) -0.04323(6) H1A H 1.08940 -0.30430 -0.03850 C2A C 1.27720(9) -0.03798(9) -0.01224(6) H2A H 1.33120 0.02260 0.01710 C3A C 1.21240(9) -0.16366(10) 0.02006(5) H3A H 1.21540 -0.20330 0.07490 C4A C 1.24789(10) -0.01791(10) -0.09566(6) H4A H 1.27910 0.05840 -0.13260 C5A C 1.16459(10) -0.13027(11) -0.11474(6) H5A H 1.12940 -0.14330 -0.16680 C6A C 0.22729(9) 1.06234(9) 0.52651(5) H6A H 0.16890 1.06050 0.48160 C7A C 0.26664(9) 0.94344(9) 0.57924(5) H7A H 0.23950 0.84710 0.57580 C8A C 0.29025(9) 1.18447(9) 0.55258(5) H8A H 0.28180 1.27960 0.52810 C9A C 0.35297(9) 0.99202(9) 0.63776(5) H9A H 0.39390 0.93450 0.68080 C10A C 0.36787(9) 1.14085(9) 0.62123(5) H10A H 0.42090 1.20140 0.65110 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 C6 2.300 1_555 1_555 C1 H1 0.950 1_555 1_555 C2 H2 0.951 1_555 1_555 C3 C1 1.405 1_555 1_555 H3 C3 0.950 1_555 1_555 C4 C2 1.408 1_555 1_555 H4 C4 0.950 1_555 1_555 C5 C1 1.405 1_555 1_555 H5 C5 0.950 1_555 1_555 C6 H6 0.949 1_555 1_555 C7 Li1 2.305 1_555 1_555 H7 C7 0.950 1_555 1_555 C8 Li1 2.330 1_555 1_555 H8 C8 0.951 1_555 1_555 C9 Li1 2.347 1_555 1_555 H9 C9 0.949 1_555 1_555 C10 Li1 2.359 1_555 1_555 H10 C10 0.950 1_555 1_555 O1 C11 1.433 1_555 1_555 C11 H11 0.990 1_555 1_555 H12 C11 0.990 1_555 1_555 C12 C11 1.500 1_555 1_555 H13 C12 0.990 1_555 1_555 H14 C12 0.990 1_555 1_555 C13 O1 1.421 1_555 1_555 H15 C13 0.990 1_555 1_555 H16 C13 0.990 1_555 1_555 O2 C12 1.426 1_555 1_555 O3 C15 1.420 1_555 1_555 C14 O2 1.420 1_555 1_555 H17 C14 0.979 1_555 1_555 H18 C14 0.980 1_555 1_555 H19 C14 0.981 1_555 1_555 C15 H20 0.980 1_555 1_555 H21 C15 0.980 1_555 1_555 H22 C15 0.981 1_555 1_555 C16 C13 1.508 1_555 1_555 H23 C16 0.990 1_555 1_555 H24 C16 0.990 1_555 1_555 Li2 O1 2.035 1_555 1_555 O4 Li2 2.122 1_555 1_555 O5 Li2 2.042 1_555 1_555 O6 Li2 2.195 1_555 1_555 C17 O6 1.424 1_555 1_555 H25 C17 0.990 1_555 1_555 H26 C17 0.991 1_555 1_555 C18 O4 1.426 1_555 1_555 H27 C18 0.990 1_555 1_555 H28 C18 0.990 1_555 1_555 C19 O5 1.420 1_555 1_555 H29 C19 0.990 1_555 1_555 H30 C19 0.990 1_555 1_555 C20 O5 1.431 1_555 1_555 H31 C20 0.991 1_555 1_555 H32 C20 0.990 1_555 1_555 C21 O4 1.419 1_555 1_555 H33 C21 0.980 1_555 1_555 H34 C21 0.980 1_555 1_555 H35 C21 0.980 1_555 1_555 C22 O6 1.423 1_555 1_555 H36 C22 0.980 1_555 1_555 H37 C22 0.980 1_555 1_555 H38 C22 0.980 1_555 1_555 Li3 C1 2.248 1_555 1_555 C1A Li3 2.248 1_555 1_555 H1A C1A 0.950 1_555 1_555 C2A Li3 2.337 1_555 1_555 H2A C2A 0.951 1_555 1_555 C3A Li3 2.258 1_555 1_555 H3A C3A 0.950 1_555 1_555 C4A Li3 2.384 1_555 1_555 H4A C4A 0.950 1_555 1_555 C5A Li3 2.332 1_555 1_555 H5A C5A 0.950 1_555 1_555 C6A Li1 2.300 1_555 1_555 H6A C6A 0.949 1_555 1_555 C7A Li1 2.305 1_555 1_555 H7A C7A 0.950 1_555 1_555 C8A Li1 2.330 1_555 1_555 H8A C8A 0.951 1_555 1_555 C9A Li1 2.347 1_555 1_555 H9A C9A 0.949 1_555 1_555 C10A Li1 2.359 1_555 1_555 H10A C10A 0.950 1_555 1_555 C2 C3 1.407 1_555 1_555 C2 Li3 2.337 1_555 1_555 C3 Li3 2.258 1_555 1_555 C4 C5 1.403 1_555 1_555 C4 Li3 2.384 1_555 1_555 C5 Li3 2.332 1_555 1_555 C6 C7 1.411 1_555 1_555 C6 C8 1.410 1_555 1_555 C7 C9 1.408 1_555 1_555 C8 C10 1.410 1_555 1_555 C9 C10 1.407 1_555 1_555 O2 Li2 2.130 1_555 1_555 O3 C16 1.425 1_555 1_555 O3 Li2 2.178 1_555 1_555 C17 C19 1.506 1_555 1_555 C18 C20 1.501 1_555 1_555 C1A C3A 1.405 1_555 1_555 C1A C5A 1.405 1_555 1_555 C2A C3A 1.407 1_555 1_555 C2A C4A 1.408 1_555 1_555 C4A C5A 1.403 1_555 1_555 C6A C7A 1.411 1_555 1_555 C6A C8A 1.410 1_555 1_555 C7A C9A 1.408 1_555 1_555 C8A C10A 1.410 1_555 1_555 C9A C10A 1.407 1_555 1_555 #END data_CSD_CIF_PEGBAE _audit_creation_date 1993-11-16 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD PEGBAE _chemical_formula_sum 'C74 H88 Li2 N4 O18' _chemical_formula_moiety ; C12 H24 Li1 O4 1+,C56 H52 Li1 N4 O12 1-,2(C3 H6 O1) ; _journal_coden_Cambridge 4 _journal_volume 115 _journal_year 1993 _journal_page_first 2707 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "J.Arnold" "D.Y.Dawson" "C.G.Hoffman" _chemical_name_systematic ; (Diacetone alcohol-lithium) meso-tetrakis(3,4,5-trimethoxy-phenyl)porphyrinato-lithium acetone solvate ; _cell_volume 1790.156 _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.23 _diffrn_ambient_temperature 188.15 _refine_special_details ; One lithium atom and an acetone molcule are disordered, the former with equal occupancies. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_gt 0.0614 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 12.420(2) _cell_length_b 12.965(2) _cell_length_c 13.998(2) _cell_angle_alpha 66.294(13) _cell_angle_beta 60.207(15) _cell_angle_gamma 77.003(15) _cell_formula_units_Z 1 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.16 N 0.68 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z O1 O -0.1445(3) -0.6668(2) 0.2484(2) O2 O -0.2171(2) -0.7229(2) 0.4773(2) O3 O -0.2296(3) -0.5728(2) 0.5670(2) O4 O -0.6821(2) 0.1921(3) 0.4154(2) O5 O -0.8229(3) 0.1874(3) 0.3204(2) O6 O -0.7161(2) 0.1710(2) 0.1078(2) O7 O 0.0966(2) -0.0960(2) -0.5869(2) O8 O -0.0752(4) 0.0743(4) -0.6141(4) O9? O 0.1364(4) -0.0228(4) -0.4495(4) N1 N -0.1630(2) -0.0791(2) 0.1179(2) N2 N 0.0935(2) -0.1516(2) 0.0290(2) C1 C -0.2796(3) -0.0301(3) 0.1497(2) C2 C -0.3713(3) -0.1139(3) 0.2356(3) C3 C -0.3093(3) -0.2141(3) 0.2564(3) C4 C -0.1789(3) -0.1919(3) 0.1822(2) C5 C -0.0825(3) -0.2750(3) 0.1772(2) C6 C 0.0446(3) -0.2542(3) 0.1050(2) C7 C 0.1428(3) -0.3399(3) 0.1015(3) C8 C 0.2509(3) -0.2873(3) 0.0222(3) C9 C 0.2200(3) -0.1691(3) -0.0221(2) C10 C -0.3066(3) 0.0853(3) 0.1060(2) C11 C -0.1188(3) -0.3928(3) 0.2564(3) C12 C -0.1141(3) -0.4725(3) 0.2113(3) C13 C -0.1482(3) -0.5826(3) 0.2853(3) C14 C -0.1887(3) -0.6132(3) 0.4038(3) C15 C -0.1915(3) -0.5337(3) 0.4490(3) C16 C -0.1568(3) -0.4243(3) 0.3749(3) C17 C -0.0792(6) -0.6462(4) 0.1238(4) C18 C -0.3364(4) -0.7555(4) 0.5116(4) C19 C -0.2091(5) -0.5026(4) 0.6131(3) C20 C -0.4417(3) 0.1215(3) 0.1567(3) C21 C -0.4950(3) 0.1418(3) 0.2612(3) C22 C -0.6207(3) 0.1692(3) 0.3131(3) C23 C -0.6926(3) 0.1736(4) 0.2612(3) C24 C -0.6384(3) 0.1586(3) 0.1546(3) C25 C -0.5123(3) 0.1319(3) 0.1017(3) C26 C -0.6118(4) 0.1829(4) 0.4724(3) C27 C -0.8604(5) 0.2984(5) 0.2821(4) C28 C -0.6600(3) 0.1533(4) -0.0001(3) C29 C 0.0900(4) -0.1160(3) -0.6766(3) C30 C 0.0410(4) -0.0074(4) -0.7413(4) C31 C -0.0844(4) 0.0322(3) -0.6676(3) C32 C 0.0058(4) -0.2107(4) -0.6241(3) C33 C 0.2209(4) -0.1431(4) -0.7598(4) C34 C -0.1846(4) 0.0541(4) -0.7005(4) C35 C 0.370(1) -0.543(1) 0.911(1) C36 C 0.429(1) -0.491(1) 0.779(1) C37 C 0.273(1) -0.556(1) 0.963(1) C38? C 0.444(3) -0.516(3) 0.836(2) C39 C 0.455(1) -0.536(1) 0.717(1) C40 C 0.493(2) -0.531(2) 0.895(2) C41 C 0.431(2) -0.388(2) 0.747(1) C42 C 0.413(2) -0.555(2) 0.986(2) C43 C 0.507(3) -0.428(3) 0.806(2) Li1 Li 0.00000 0.00000 0.00000 Li2 Li -0.052(1) -0.042(1) -0.449(1) H1 H 0.13767 -0.18750 -0.54297 H2 H -0.45874 -0.10122 0.27096 H3 H -0.34480 -0.28524 0.30950 H4 H 0.13293 -0.41810 0.14626 H5 H 0.33184 -0.32142 -0.00030 H6 H -0.08753 -0.45168 0.12976 H7 H -0.15922 -0.37026 0.40600 H8 H -0.08318 -0.71060 0.10942 H9 H -0.11641 -0.58289 0.08507 H10 H 0.00524 -0.63172 0.09478 H11 H -0.39819 -0.70903 0.55175 H12 H -0.34794 -0.83190 0.56183 H13 H -0.34287 -0.74698 0.44393 H14 H -0.23914 -0.53841 0.69544 H15 H -0.12276 -0.49099 0.57741 H16 H -0.25184 -0.43219 0.59722 H17 H -0.44545 0.17060 0.29729 H18 H -0.47486 0.12107 0.02835 H19 H -0.54577 0.23410 0.42173 H20 H -0.66338 0.20059 0.54184 H21 H -0.57869 0.10823 0.49179 H22 H -0.94827 0.30520 0.32325 H23 H -0.83537 0.32236 0.20051 H24 H -0.82361 0.34393 0.29618 H25 H -0.63286 0.07835 0.00849 H26 H -0.60214 0.20493 -0.05848 H27 H -0.72971 0.16450 -0.02248 H28 H 0.03714 -0.01919 -0.80222 H29 H 0.09771 0.05022 -0.77434 H30 H -0.07504 -0.19157 -0.57249 H31 H 0.00219 -0.22333 -0.68483 H32 H 0.03623 -0.27721 -0.58188 H33 H 0.25278 -0.20914 -0.71843 H34 H 0.21874 -0.15527 -0.82138 H35 H 0.27259 -0.08185 -0.79168 H36 H -0.16095 0.11084 -0.77556 H37 H -0.20041 -0.01323 -0.70267 H38 H -0.25774 0.07843 -0.64438 C9A C -0.2200(3) 0.1691(3) 0.0221(2) N2A N -0.0935(2) 0.1516(2) -0.0290(2) C6A C -0.0446(3) 0.2542(3) -0.1050(2) C5A C 0.0825(3) 0.2750(3) -0.1772(2) C4A C 0.1789(3) 0.1919(3) -0.1822(2) N1A N 0.1630(2) 0.0791(2) -0.1179(2) C1A C 0.2796(3) 0.0301(3) -0.1497(2) C2A C 0.3713(3) 0.1139(3) -0.2356(3) C3A C 0.3093(3) 0.2141(3) -0.2564(3) H3A H 0.34480 0.28524 -0.30950 H2A H 0.45874 0.10122 -0.27096 C10A C 0.3066(3) -0.0853(3) -0.1060(2) C20A C 0.4417(3) -0.1215(3) -0.1567(3) C21A C 0.4950(3) -0.1418(3) -0.2612(3) C22A C 0.6207(3) -0.1692(3) -0.3131(3) O4A O 0.6821(2) -0.1921(3) -0.4154(2) C26A C 0.6118(4) -0.1829(4) -0.4724(3) H19A H 0.54577 -0.23410 -0.42173 H20A H 0.66338 -0.20059 -0.54184 H21A H 0.57869 -0.10823 -0.49179 C23A C 0.6926(3) -0.1736(4) -0.2612(3) O5A O 0.8229(3) -0.1874(3) -0.3204(2) C27A C 0.8604(5) -0.2984(5) -0.2821(4) H22A H 0.94827 -0.30520 -0.32325 H23A H 0.83537 -0.32236 -0.20051 H24A H 0.82361 -0.34393 -0.29618 C24A C 0.6384(3) -0.1586(3) -0.1546(3) O6A O 0.7161(2) -0.1710(2) -0.1078(2) C28A C 0.6600(3) -0.1533(4) 0.0001(3) H25A H 0.63286 -0.07835 -0.00849 H26A H 0.60214 -0.20493 0.05848 H27A H 0.72971 -0.16450 0.02248 C25A C 0.5123(3) -0.1319(3) -0.1017(3) H18A H 0.47486 -0.12107 -0.02835 H17A H 0.44545 -0.17060 -0.29729 C11A C 0.1188(3) 0.3928(3) -0.2564(3) C12A C 0.1141(3) 0.4725(3) -0.2113(3) C13A C 0.1482(3) 0.5826(3) -0.2853(3) O1A O 0.1445(3) 0.6668(2) -0.2484(2) C17A C 0.0792(6) 0.6462(4) -0.1238(4) H8A H 0.08318 0.71060 -0.10942 H9A H 0.11641 0.58289 -0.08507 H10A H -0.00524 0.63172 -0.09478 C14A C 0.1887(3) 0.6132(3) -0.4038(3) O2A O 0.2171(2) 0.7229(2) -0.4773(2) C18A C 0.3364(4) 0.7555(4) -0.5116(4) H11A H 0.39819 0.70903 -0.55175 H12A H 0.34794 0.83190 -0.56183 H13A H 0.34287 0.74698 -0.44393 C15A C 0.1915(3) 0.5337(3) -0.4490(3) O3A O 0.2296(3) 0.5728(2) -0.5670(2) C19A C 0.2091(5) 0.5026(4) -0.6131(3) H14A H 0.23914 0.53841 -0.69544 H15A H 0.12276 0.49099 -0.57741 H16A H 0.25184 0.43219 -0.59722 C16A C 0.1568(3) 0.4243(3) -0.3749(3) H7A H 0.15922 0.37026 -0.40600 H6A H 0.08753 0.45168 -0.12976 C7A C -0.1428(3) 0.3399(3) -0.1015(3) C8A C -0.2509(3) 0.2873(3) -0.0222(3) H5A H -0.33184 0.32142 0.00030 H4A H -0.13293 0.41810 -0.14626 Li2A Li 0.052(1) 0.042(1) -0.551(1) O7A O -0.0966(2) 0.0960(2) -0.4131(2) C29A C -0.0900(4) 0.1160(3) -0.3234(3) C30A C -0.0410(4) 0.0074(4) -0.2587(4) C31A C 0.0844(4) -0.0322(3) -0.3324(3) O8A O 0.0752(4) -0.0743(4) -0.3859(4) H1A H -0.13767 0.18750 -0.45703 C34A C 0.1846(4) -0.0541(4) -0.2995(4) H36A H 0.16095 -0.11084 -0.22444 H37A H 0.20041 0.01323 -0.29733 H38A H 0.25774 -0.07843 -0.35562 H28A H -0.03714 0.01919 -0.19778 H29A H -0.09771 -0.05022 -0.22566 C32A C -0.0058(4) 0.2107(4) -0.3759(3) H30A H 0.07504 0.19157 -0.42751 H31A H -0.00219 0.22333 -0.31517 H32A H -0.03623 0.27721 -0.41812 C33A C -0.2209(4) 0.1431(4) -0.2402(4) H33A H -0.25278 0.20914 -0.28157 H34A H -0.21874 0.15527 -0.17862 H35A H -0.27259 0.08185 -0.20832 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 O1 C13 1.367 1_555 1_555 O2 C14 1.376 1_555 1_555 O3 C15 1.366 1_555 1_555 O4 C22 1.369 1_555 1_555 O5 C23 1.412 1_555 1_555 O6 C24 1.364 1_555 1_555 O7 C29 1.423 1_555 1_555 O8 C31 1.146 1_555 1_555 N1 C1 1.368 1_555 1_555 N2 C6 1.361 1_555 1_555 C1 C2 1.438 1_555 1_555 C2 C3 1.354 1_555 1_555 C3 C4 1.443 1_555 1_555 C4 N1 1.372 1_555 1_555 C5 C4 1.413 1_555 1_555 C6 C5 1.405 1_555 1_555 C7 C6 1.449 1_555 1_555 C8 C7 1.350 1_555 1_555 C9 N2 1.373 1_555 1_555 C10 C1 1.403 1_555 1_555 C11 C5 1.489 1_555 1_555 C12 C11 1.389 1_555 1_555 C13 C12 1.392 1_555 1_555 C14 C13 1.376 1_555 1_555 C15 C14 1.397 1_555 1_555 C16 C11 1.380 1_555 1_555 C17 O1 1.445 1_555 1_555 C18 O2 1.420 1_555 1_555 C19 O3 1.432 1_555 1_555 C20 C10 1.507 1_555 1_555 C21 C20 1.384 1_555 1_555 C22 C21 1.386 1_555 1_555 C23 C22 1.385 1_555 1_555 C24 C23 1.376 1_555 1_555 C25 C20 1.383 1_555 1_555 C26 O4 1.408 1_555 1_555 C27 O5 1.379 1_555 1_555 C28 O6 1.407 1_555 1_555 C29 C30 1.520 1_555 1_555 C30 C31 1.491 1_555 1_555 C31 C34 1.465 1_555 1_555 C32 C29 1.493 1_555 1_555 C33 C29 1.521 1_555 1_555 C34 H36 0.949 1_555 1_555 C35 C36 1.510 1_555 1_555 C36 C39 1.114 1_555 1_555 C37 C35 1.063 1_555 1_555 C40 C35 1.465 1_555 1_555 C41 C36 1.228 1_555 1_555 C42 C35 1.342 1_555 1_555 C43 C36 1.648 1_555 1_555 Li1 N1 2.031 1_555 1_555 Li2 O7 2.142 1_555 1_555 H1 O7 1.224 1_555 1_555 H2 C2 0.950 1_555 1_555 H3 C3 0.951 1_555 1_555 H4 C7 0.951 1_555 1_555 H5 C8 0.950 1_555 1_555 H6 C12 0.950 1_555 1_555 H7 C16 0.951 1_555 1_555 H8 C17 0.951 1_555 1_555 H9 C17 0.950 1_555 1_555 H10 C17 0.951 1_555 1_555 H11 C18 0.951 1_555 1_555 H12 C18 0.949 1_555 1_555 H13 C18 0.950 1_555 1_555 H14 C19 0.951 1_555 1_555 H15 C19 0.950 1_555 1_555 H16 C19 0.949 1_555 1_555 H17 C21 1.156 1_555 1_555 H18 C25 0.950 1_555 1_555 H19 C26 0.951 1_555 1_555 H20 C26 0.950 1_555 1_555 H21 C26 0.949 1_555 1_555 H22 C27 0.951 1_555 1_555 H23 C27 0.950 1_555 1_555 H24 C27 0.949 1_555 1_555 H25 C28 0.933 1_555 1_555 H26 C28 0.908 1_555 1_555 H27 C28 1.022 1_555 1_555 H28 C30 0.950 1_555 1_555 H29 C30 0.950 1_555 1_555 H30 C32 0.950 1_555 1_555 H31 C32 0.951 1_555 1_555 H32 C32 0.949 1_555 1_555 H33 C33 0.950 1_555 1_555 H34 C33 0.950 1_555 1_555 H35 C33 0.950 1_555 1_555 H37 C34 0.952 1_555 1_555 H38 C34 0.950 1_555 1_555 C9A C10 1.400 1_555 1_555 N2A Li1 2.044 1_555 1_555 C6A N2A 1.361 1_555 1_555 C5A C6A 1.405 1_555 1_555 C4A C5A 1.413 1_555 1_555 N1A Li1 2.031 1_555 1_555 C1A N1A 1.368 1_555 1_555 C2A C1A 1.438 1_555 1_555 C3A C4A 1.443 1_555 1_555 H3A C3A 0.951 1_555 1_555 H2A C2A 0.950 1_555 1_555 C10A C9 1.400 1_555 1_555 C20A C10A 1.507 1_555 1_555 C21A C20A 1.384 1_555 1_555 C22A C21A 1.386 1_555 1_555 O4A C22A 1.369 1_555 1_555 C26A O4A 1.408 1_555 1_555 H19A C26A 0.951 1_555 1_555 H20A C26A 0.950 1_555 1_555 H21A C26A 0.949 1_555 1_555 C23A C22A 1.385 1_555 1_555 O5A C23A 1.412 1_555 1_555 C27A O5A 1.379 1_555 1_555 H22A C27A 0.951 1_555 1_555 H23A C27A 0.950 1_555 1_555 H24A C27A 0.949 1_555 1_555 C24A C23A 1.376 1_555 1_555 O6A C24A 1.364 1_555 1_555 C28A O6A 1.407 1_555 1_555 H25A C28A 0.933 1_555 1_555 H26A C28A 0.908 1_555 1_555 H27A C28A 1.022 1_555 1_555 C25A C20A 1.383 1_555 1_555 H18A C25A 0.950 1_555 1_555 H17A C21A 1.156 1_555 1_555 C11A C5A 1.489 1_555 1_555 C12A C11A 1.389 1_555 1_555 C13A C12A 1.392 1_555 1_555 O1A C13A 1.367 1_555 1_555 C17A O1A 1.445 1_555 1_555 H8A C17A 0.951 1_555 1_555 H9A C17A 0.950 1_555 1_555 H10A C17A 0.951 1_555 1_555 C14A C13A 1.376 1_555 1_555 O2A C14A 1.376 1_555 1_555 C18A O2A 1.420 1_555 1_555 H11A C18A 0.951 1_555 1_555 H12A C18A 0.949 1_555 1_555 H13A C18A 0.950 1_555 1_555 C15A C14A 1.397 1_555 1_555 O3A C15A 1.366 1_555 1_555 C19A O3A 1.432 1_555 1_555 H14A C19A 0.951 1_555 1_555 H15A C19A 0.950 1_555 1_555 H16A C19A 0.949 1_555 1_555 C16A C11A 1.380 1_555 1_555 H7A C16A 0.951 1_555 1_555 H6A C12A 0.950 1_555 1_555 C7A C6A 1.449 1_555 1_555 C8A C9A 1.445 1_555 1_555 H5A C8A 0.950 1_555 1_555 H4A C7A 0.951 1_555 1_555 Li2A O7 1.939 1_555 1_555 O7A Li2 1.939 1_555 1_555 C29A O7A 1.423 1_555 1_555 C30A C29A 1.520 1_555 1_555 C31A C30A 1.491 1_555 1_555 O8A Li2 2.060 1_555 1_555 H1A O7A 1.224 1_555 1_555 C34A C31A 1.465 1_555 1_555 H36A C34A 0.949 1_555 1_555 H37A C34A 0.952 1_555 1_555 H38A C34A 0.950 1_555 1_555 H28A C30A 0.950 1_555 1_555 H29A C30A 0.950 1_555 1_555 C32A C29A 1.493 1_555 1_555 H30A C32A 0.950 1_555 1_555 H31A C32A 0.951 1_555 1_555 H32A C32A 0.949 1_555 1_555 C33A C29A 1.521 1_555 1_555 H33A C33A 0.950 1_555 1_555 H34A C33A 0.950 1_555 1_555 H35A C33A 0.950 1_555 1_555 O8 Li2A 2.060 1_555 1_555 N2 Li1 2.044 1_555 1_555 C8 C9 1.445 1_555 1_555 C15 C16 1.386 1_555 1_555 C24 C25 1.390 1_555 1_555 C40 C43 1.385 1_555 1_555 C40 C42 1.127 1_555 1_555 C41 C43 1.433 1_555 1_555 Li2 Li2A 1.563 1_555 1_555 C9A N2A 1.373 1_555 1_555 C4A N1A 1.372 1_555 1_555 C1A C10A 1.403 1_555 1_555 C2A C3A 1.354 1_555 1_555 C24A C25A 1.390 1_555 1_555 C15A C16A 1.386 1_555 1_555 C7A C8A 1.350 1_555 1_555 Li2A O7A 2.142 1_555 1_555 C31A O8A 1.146 1_555 1_555 #END data_CSD_CIF_PEJROL _audit_creation_date 1994-02-10 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD PEJROL _chemical_formula_sum 'C64 H112 N4 Na2 O7 P2 Si4' _chemical_formula_moiety ; C24 H48 Na1 O6 1+,C36 H56 N4 Na1 P2 Si4 1-,C4 H8 O1 ; _journal_coden_Cambridge 9 _journal_volume 32 _journal_year 1993 _journal_page_first 1977 _journal_name_full 'Inorg.Chem. ' loop_ _publ_author_name "A.Steiner" "D.Stalke" _chemical_name_systematic ; hexakis(Tetrahydrofuran)-sodium bis(diphenyl-(trimethylsilylamino)-(trimethylsilylimino)phosphorane-N,N')-sodi um tetrahydrofuran solvate ; _chemical_melting_point 253.15 _cell_volume 4080.918 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.033 _diffrn_ambient_temperature 153 _refine_special_details ; Some tetrahydrofuran molecules are disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0931 _refine_ls_wR_factor_gt 0.0931 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,-z _cell_length_a 13.473(2) _cell_length_b 17.273(2) _cell_length_c 18.188(2) _cell_angle_alpha 90 _cell_angle_beta 105.39(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 N 0.68 Na 1.35 O 0.68 P 1.05 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na -0.1084(2) 0.75590 -0.2257(2) P1 P 0.1064(1) 0.7561(2) -0.2277(1) N1 N 0.0188(4) 0.7165(4) -0.2907(3) Si1 Si -0.0013(2) 0.6388(2) -0.3476(1) C1 C 0.0708(8) 0.6448(7) -0.4225(6) C2 C -0.1421(7) 0.6321(7) -0.3979(6) C3 C 0.0346(7) 0.5466(5) -0.2954(6) N2 N 0.0645(4) 0.8012(4) -0.1670(4) Si2 Si 0.0949(2) 0.8747(2) -0.1050(1) C4 C -0.0141(9) 0.8875(6) -0.0600(7) C5 C 0.1060(7) 0.9692(5) -0.1516(6) C6 C 0.2202(8) 0.8622(6) -0.0309(6) C7 C 0.2014(5) 0.6839(4) -0.1811(4) C8 C 0.2727(5) 0.6522(5) -0.2158(5) C9 C 0.3373(5) 0.5912(5) -0.1820(5) C10 C 0.3335(7) 0.5626(5) -0.1145(5) C11 C 0.2627(7) 0.5931(6) -0.0796(5) C12 C 0.1984(6) 0.6525(5) -0.1107(4) C13 C 0.1828(5) 0.8175(4) -0.2744(5) C14 C 0.2802(5) 0.8447(5) -0.2327(5) C15 C 0.3386(7) 0.8901(5) -0.2677(7) C16 C 0.3002(9) 0.9078(5) -0.3437(8) C17 C 0.2034(9) 0.8824(6) -0.3860(7) C18 C 0.1469(6) 0.8376(5) -0.3492(5) P2 P -0.3224(1) 0.7387(2) -0.2226(1) N3 N -0.2793(4) 0.8070(3) -0.2623(3) Si3 Si -0.3079(1) 0.8854(2) -0.3178(1) C19 C -0.3783(9) 0.9612(6) -0.2773(7) C20 C -0.1834(7) 0.9279(6) -0.3257(6) C21 C -0.3863(9) 0.8668(8) -0.4155(6) N4 N -0.2350(4) 0.6789(3) -0.1856(3) Si4 Si -0.2021(2) 0.6130(2) -0.1159(2) C22 C -0.1673(12) 0.5182(7) -0.1547(8) C23 C -0.0814(13) 0.6369(10) -0.0473(9) C24 C -0.2987(11) 0.5897(8) -0.0644(9) C25 C -0.3831(5) 0.7783(4) -0.1521(4) C26 C -0.4669(5) 0.7435(6) -0.1340(5) C27 C -0.5087(6) 0.7738(7) -0.0782(5) C28 C -0.4714(7) 0.8376(8) -0.0418(5) C29 C -0.3860(8) 0.8755(6) -0.0576(5) C30 C -0.3446(6) 0.8444(6) -0.1124(5) C31 C -0.4299(5) 0.6892(4) -0.2892(4) C32 C -0.5206(5) 0.7280(5) -0.3211(4) C33 C -0.6026(6) 0.6906(6) -0.3745(5) C34 C -0.5922(7) 0.6167(6) -0.3930(5) C35 C -0.5012(8) 0.5756(6) -0.3629(6) C36 C -0.4212(6) 0.6123(5) -0.3099(4) Na2 Na -0.7112(2) 0.2430(2) -0.2787(2) O1 O -0.8519(4) 0.1591(3) -0.3203(3) C37 C -0.9440(8) 0.1617(7) -0.2946(6) C38 C -1.0217(7) 0.1132(6) -0.3502(7) C39 C -0.9519(7) 0.0529(6) -0.3713(6) C40 C -0.8601(7) 0.0974(6) -0.3713(6) O2 O -0.6247(4) 0.1877(3) -0.3649(3) C41 C -0.5628(9) 0.1183(7) -0.3549(7) C42 C -0.5778(22) 0.0929(10) -0.4393(12) C43? C -0.4980(34) 0.1324(36) -0.4154(18) C44 C -0.5733(10) 0.1723(9) -0.4788(8) C45 C -0.6249(9) 0.2232(7) -0.4352(6) O3 O -0.5698(4) 0.3285(3) -0.2398(3) C46 C -0.5587(9) 0.3774(8) -0.1791(7) C47 C -0.4574(12) 0.4019(11) -0.152(1) C48 C -0.4094(16) 0.3717(13) -0.1916(11) C49 C -0.4758(9) 0.3270(8) -0.2605(8) O4 O -0.6261(4) 0.1543(3) -0.1842(3) C50 C -0.6664(10) 0.0852(8) -0.1642(10) C51 C -0.5920(11) 0.0442(8) -0.1081(8) C52 C -0.5075(14) 0.0875(10) -0.0947(12) C53 C -0.5278(11) 0.1642(8) -0.1316(9) O5 O -0.7949(5) 0.2992(4) -0.1928(3) C54 C -0.789(1) 0.2685(9) -0.1194(7) C55 C -0.8631(16) 0.3183(13) -0.0893(14) C56 C -0.8879(15) 0.3849(11) -0.1396(9) C57 C -0.8471(12) 0.3742(8) -0.2044(9) O6 O -0.7918(4) 0.3362(4) -0.3711(3) C58 C -0.7505(9) 0.4112(6) -0.3861(7) C59 C -0.8089(9) 0.4403(8) -0.4592(7) C60 C -0.9007(10) 0.3859(8) -0.4783(8) C61 C -0.8888(9) 0.3271(7) -0.4292(9) O7 O -0.1504(14) 0.3145(16) -0.3758(16) C62 C -0.2244(27) 0.2851(13) -0.4171(16) C63 C -0.3193(14) 0.3338(18) -0.4347(14) C64 C -0.2799(23) 0.4051(14) -0.3981(16) C65 C -0.1786(23) 0.3824(22) -0.3620(2) O8 O -0.1786(19) 0.1001(14) -0.1129(12) C66 C -0.1218(14) 0.1205(13) -0.1646(14) C67 C -0.1943(21) 0.1541(16) -0.2362(11) C68 C -0.2811(16) 0.1853(14) -0.2059(15) C69 C -0.2441(19) 0.1646(17) -0.1218(13) H1 H 0.14340 0.64760 -0.39880 H2 H 0.05620 0.59960 -0.45430 H3 H 0.04930 0.69010 -0.45310 H4 H -0.18130 0.62900 -0.36090 H5 H -0.16190 0.67750 -0.42860 H6 H -0.15500 0.58690 -0.42980 H7 H -0.00050 0.54130 -0.25610 H8 H 0.01530 0.50480 -0.33110 H9 H 0.10760 0.54540 -0.27310 H10 H -0.07760 0.89400 -0.09870 H11 H -0.01850 0.84250 -0.03000 H12 H -0.00150 0.93240 -0.02760 H13 H 0.04350 0.97820 -0.19080 H14 H 0.11580 1.00990 -0.11440 H15 H 0.16310 0.96820 -0.17380 H16 H 0.27530 0.85590 -0.05470 H17 H 0.23300 0.90710 0.00150 H18 H 0.21600 0.81720 -0.00090 H19 H 0.27790 0.67250 -0.26380 H20 H 0.38460 0.56890 -0.20740 H21 H 0.38110 0.52290 -0.09070 H22 H 0.25580 0.56970 -0.03330 H23 H 0.15270 0.67440 -0.08370 H24 H 0.30680 0.83190 -0.17970 H25 H 0.40460 0.90890 -0.23910 H26 H 0.34250 0.93790 -0.36790 H27 H 0.17670 0.89680 -0.43860 H28 H 0.08080 0.81820 -0.37690 H29 H -0.44270 0.94060 -0.27300 H30 H -0.33710 0.97610 -0.22780 H31 H -0.39080 1.00560 -0.31030 H32 H -0.18470 0.93520 -0.37830 H33 H -0.12700 0.89420 -0.30280 H34 H -0.17520 0.97670 -0.29970 H35 H -0.35420 0.82810 -0.43940 H36 H -0.45230 0.84850 -0.41230 H37 H -0.39500 0.91350 -0.44510 H38 H -0.22940 0.50180 -0.19100 H39 H -0.11330 0.52350 -0.17980 H40 H -0.14780 0.48050 -0.11470 H41 H -0.08650 0.68570 -0.02320 H42 H -0.06370 0.59710 -0.00920 H43 H -0.02920 0.64010 -0.07420 H44 H -0.31310 0.63690 -0.04140 H45 H -0.36160 0.56860 -0.09590 H46 H -0.26800 0.55310 -0.02520 H47 H -0.49580 0.69740 -0.16070 H48 H -0.56520 0.74820 -0.06550 H49 H -0.50290 0.85830 -0.00450 H50 H -0.35870 0.92140 -0.02980 H51 H -0.28720 0.86970 -0.12420 H52 H -0.52800 0.78050 -0.30610 H53 H -0.66380 0.71890 -0.39890 H54 H -0.64990 0.59110 -0.42660 H55 H -0.49470 0.52320 -0.37840 H56 H -0.35880 0.58470 -0.28700 H57 H -0.96780 0.21410 -0.29520 H58 H -0.93240 0.14130 -0.24390 H59 H -1.05560 0.14240 -0.39470 H60 H -1.07240 0.09100 -0.32810 H61 H -0.98250 0.02890 -0.41960 H62 H -0.93540 0.01380 -0.33240 H63 H -0.79920 0.06590 -0.35770 H64 H -0.86730 0.11820 -0.42140 H65 H -0.58540 0.07920 -0.32550 H66 H -0.49190 0.13040 -0.33140 H67? H -0.60430 0.07240 -0.36250 H68? H -0.51600 0.11650 -0.30490 H69 H -0.64380 0.06890 -0.45890 H70 H -0.52490 0.05810 -0.44520 H71? H -0.48170 0.08320 -0.43380 H72? H -0.43550 0.16100 -0.39570 H73 H -0.61050 0.16990 -0.53160 H74 H -0.50380 0.18820 -0.47470 H75? H -0.62230 0.13830 -0.51110 H76? H -0.53750 0.20070 -0.50920 H77 H -0.59110 0.27270 -0.42760 H78 H -0.69510 0.23110 -0.46380 H79 H -0.58230 0.35220 -0.13980 H80 H -0.60160 0.42170 -0.19610 H81 H -0.43200 0.38690 -0.09950 H82 H -0.45160 0.45710 -0.15570 H83 H -0.36500 0.33360 -0.16120 H84 H -0.36690 0.40890 -0.20810 H85 H -0.48170 0.35630 -0.30630 H86 H -0.45370 0.27520 -0.26720 H87 H -0.68710 0.05410 -0.20940 H88 H -0.72610 0.09600 -0.14660 H89 H -0.58650 -0.00870 -0.12280 H90 H -0.61040 0.04490 -0.06060 H91 H -0.46810 0.06210 -0.12450 H92 H -0.46770 0.08820 -0.04240 H93 H -0.53190 0.19860 -0.09110 H94 H -0.47850 0.18390 -0.15660 H95 H -0.72180 0.27720 -0.08570 H96 H -0.80310 0.21390 -0.12220 H97 H -0.84220 0.32700 -0.03520 H98 H -0.92750 0.29100 -0.10210 H99 H -0.84190 0.42280 -0.11020 H100 H -0.95690 0.40460 -0.15040 H101 H -0.90760 0.36900 -0.24620 H102 H -0.80470 0.41460 -0.21600 H103 H -0.67840 0.40810 -0.38320 H104 H -0.75960 0.44570 -0.34710 H105 H -0.77030 0.43360 -0.49610 H106 H -0.82740 0.49380 -0.45760 H107 H -0.91550 0.36840 -0.53010 H108 H -0.95890 0.41500 -0.47250 H109 H -0.94320 0.32370 -0.40430 H110 H -0.88870 0.28030 -0.45770 H111 H -0.23760 0.23720 -0.39470 H112 H -0.20920 0.27440 -0.46480 H113 H -0.36940 0.31360 -0.41080 H114 H -0.35160 0.34160 -0.48800 H115 H -0.32250 0.42700 -0.36880 H116 H -0.27220 0.44220 -0.43560 H117 H -0.12800 0.42140 -0.36270 H118 H -0.18260 0.37580 -0.31050 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Na1 N1 2.423 1_555 1_555 P1 N1 1.567 1_555 1_555 N1 Si1 1.672 1_555 1_555 Si1 C1 1.874 1_555 1_555 C1 H1 0.960 1_555 1_555 C2 Si1 1.878 1_555 1_555 C3 Si1 1.851 1_555 1_555 N2 Na1 2.420 1_555 1_555 Si2 N2 1.675 1_555 1_555 C4 Si2 1.874 1_555 1_555 C5 Si2 1.863 1_555 1_555 C6 Si2 1.872 1_555 1_555 C7 P1 1.826 1_555 1_555 C8 C7 1.394 1_555 1_555 C9 C8 1.401 1_555 1_555 C10 C9 1.337 1_555 1_555 C11 C10 1.383 1_555 1_555 C12 C7 1.401 1_555 1_555 C13 P1 1.836 1_555 1_555 C14 C13 1.411 1_555 1_555 C15 C14 1.380 1_555 1_555 C16 C15 1.376 1_555 1_555 C17 C16 1.397 1_555 1_555 C18 C13 1.362 1_555 1_555 P2 N3 1.573 1_555 1_555 N3 Na1 2.390 1_555 1_555 Si3 N3 1.672 1_555 1_555 C19 Si3 1.878 1_555 1_555 C20 Si3 1.871 1_555 1_555 C21 Si3 1.839 1_555 1_555 N4 Na1 2.423 1_555 1_555 Si4 N4 1.674 1_555 1_555 C22 Si4 1.891 1_555 1_555 C23 Si4 1.815 1_555 1_555 C24 Si4 1.839 1_555 1_555 C25 P2 1.827 1_555 1_555 C26 C25 1.393 1_555 1_555 C27 C26 1.387 1_555 1_555 C28 C27 1.315 1_555 1_555 C29 C28 1.418 1_555 1_555 C30 C25 1.377 1_555 1_555 C31 P2 1.834 1_555 1_555 C32 C31 1.379 1_555 1_555 C33 C32 1.418 1_555 1_555 C34 C33 1.337 1_555 1_555 C35 C34 1.397 1_555 1_555 C36 C31 1.394 1_555 1_555 Na2 O1 2.346 1_555 1_555 O1 C37 1.438 1_555 1_555 C37 C38 1.503 1_555 1_555 C38 C39 1.519 1_555 1_555 C39 C40 1.456 1_555 1_555 C40 O1 1.398 1_555 1_555 O2 Na2 2.387 1_555 1_555 C41 O2 1.444 1_555 1_555 C42 C41 1.557 1_555 1_555 C44 C42 1.557 1_555 1_555 C45 O2 1.417 1_555 1_555 O3 Na2 2.365 1_555 1_555 C46 O3 1.366 1_555 1_555 C47 C46 1.388 1_555 1_555 C48 C47 1.207 1_555 1_555 C49 O3 1.414 1_555 1_555 O4 Na2 2.360 1_555 1_555 C50 O4 1.399 1_555 1_555 C51 C50 1.416 1_555 1_555 C52 C51 1.330 1_555 1_555 C53 O4 1.423 1_555 1_555 O5 Na2 2.364 1_555 1_555 C54 O5 1.419 1_555 1_555 C55 C54 1.525 1_555 1_555 C56 C55 1.452 1_555 1_555 C57 O5 1.462 1_555 1_555 O6 Na2 2.372 1_555 1_555 C58 O6 1.464 1_555 1_555 C59 C58 1.444 1_555 1_555 C60 C59 1.518 1_555 1_555 C61 O6 1.455 1_555 1_555 O7 C62 1.191 1_555 1_555 C62 C63 1.493 1_555 1_555 C63 C64 1.433 1_555 1_555 C64 C65 1.404 1_555 1_555 C65 O7 1.278 1_555 1_555 O8 C66 1.406 1_555 1_555 C66 C67 1.520 1_555 1_555 C67 C68 1.518 1_555 1_555 C68 C69 1.520 1_555 1_555 C69 O8 1.404 1_555 1_555 H2 C1 0.960 1_555 1_555 H3 C1 0.959 1_555 1_555 H4 C2 0.961 1_555 1_555 H5 C2 0.959 1_555 1_555 H6 C2 0.961 1_555 1_555 H7 C3 0.960 1_555 1_555 H8 C3 0.960 1_555 1_555 H9 C3 0.959 1_555 1_555 H10 C4 0.959 1_555 1_555 H11 C4 0.961 1_555 1_555 H12 C4 0.961 1_555 1_555 H13 C5 0.961 1_555 1_555 H14 C5 0.960 1_555 1_555 H15 C5 0.959 1_555 1_555 H16 C6 0.960 1_555 1_555 H17 C6 0.962 1_555 1_555 H18 C6 0.960 1_555 1_555 H19 C8 0.960 1_555 1_555 H20 C9 0.961 1_555 1_555 H21 C10 0.960 1_555 1_555 H22 C11 0.961 1_555 1_555 H23 C12 0.961 1_555 1_555 H24 C14 0.961 1_555 1_555 H25 C15 0.960 1_555 1_555 H26 C16 0.960 1_555 1_555 H27 C17 0.961 1_555 1_555 H28 C18 0.960 1_555 1_555 H29 C19 0.960 1_555 1_555 H30 C19 0.959 1_555 1_555 H31 C19 0.961 1_555 1_555 H32 C20 0.961 1_555 1_555 H33 C20 0.960 1_555 1_555 H34 C20 0.958 1_555 1_555 H35 C21 0.961 1_555 1_555 H36 C21 0.960 1_555 1_555 H37 C21 0.960 1_555 1_555 H38 C22 0.961 1_555 1_555 H39 C22 0.960 1_555 1_555 H40 C22 0.960 1_555 1_555 H41 C23 0.961 1_555 1_555 H42 C23 0.960 1_555 1_555 H43 C23 0.959 1_555 1_555 H44 C24 0.959 1_555 1_555 H45 C24 0.960 1_555 1_555 H46 C24 0.960 1_555 1_555 H47 C26 0.960 1_555 1_555 H48 C27 0.960 1_555 1_555 H49 C28 0.960 1_555 1_555 H50 C29 0.960 1_555 1_555 H51 C30 0.961 1_555 1_555 H52 C32 0.960 1_555 1_555 H53 C33 0.960 1_555 1_555 H54 C34 0.960 1_555 1_555 H55 C35 0.959 1_555 1_555 H56 C36 0.960 1_555 1_555 H57 C37 0.959 1_555 1_555 H58 C37 0.960 1_555 1_555 H59 C38 0.960 1_555 1_555 H60 C38 0.960 1_555 1_555 H61 C39 0.960 1_555 1_555 H62 C39 0.961 1_555 1_555 H63 C40 0.961 1_555 1_555 H64 C40 0.960 1_555 1_555 H65 C41 0.960 1_555 1_555 H66 C41 0.960 1_555 1_555 H69 C42 0.960 1_555 1_555 H70 C42 0.960 1_555 1_555 H73 C44 0.959 1_555 1_555 H74 C44 0.960 1_555 1_555 H77 C45 0.961 1_555 1_555 H78 C45 0.961 1_555 1_555 H79 C46 0.960 1_555 1_555 H80 C46 0.959 1_555 1_555 H81 C47 0.961 1_555 1_555 H82 C47 0.960 1_555 1_555 H83 C48 0.960 1_555 1_555 H84 C48 0.960 1_555 1_555 H85 C49 0.960 1_555 1_555 H86 C49 0.961 1_555 1_555 H87 C50 0.959 1_555 1_555 H88 C50 0.960 1_555 1_555 H89 C51 0.960 1_555 1_555 H90 C51 0.960 1_555 1_555 H91 C52 0.960 1_555 1_555 H92 C52 0.960 1_555 1_555 H93 C53 0.959 1_555 1_555 H94 C53 0.961 1_555 1_555 H95 C54 0.961 1_555 1_555 H96 C54 0.961 1_555 1_555 H97 C55 0.961 1_555 1_555 H98 C55 0.960 1_555 1_555 H99 C56 0.961 1_555 1_555 H100 C56 0.960 1_555 1_555 H101 C57 0.960 1_555 1_555 H102 C57 0.960 1_555 1_555 H103 C58 0.960 1_555 1_555 H104 C58 0.959 1_555 1_555 H105 C59 0.959 1_555 1_555 H106 C59 0.960 1_555 1_555 H107 C60 0.959 1_555 1_555 H108 C60 0.960 1_555 1_555 H109 C61 0.960 1_555 1_555 H110 C61 0.960 1_555 1_555 H111 C62 0.959 1_555 1_555 H112 C62 0.961 1_555 1_555 H113 C63 0.960 1_555 1_555 H114 C63 0.961 1_555 1_555 H115 C64 0.959 1_555 1_555 H116 C64 0.961 1_555 1_555 H117 C65 0.961 1_555 1_555 H118 C65 0.959 1_555 1_555 P1 N2 1.573 1_555 1_555 C11 C12 1.365 1_555 1_555 C17 C18 1.377 1_555 1_555 P2 N4 1.577 1_555 1_555 C29 C30 1.374 1_555 1_555 C35 C36 1.393 1_555 1_555 C44 C45 1.476 1_555 1_555 C48 C49 1.540 1_555 1_555 C52 C53 1.477 1_555 1_555 C56 C57 1.438 1_555 1_555 C60 C61 1.334 1_555 1_555 #END data_CSD_CIF_PEYLIO _audit_creation_date 1994-05-24 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD PEYLIO _chemical_formula_sum 'C32 H86 Li2 N4 Si6' _chemical_formula_moiety ; C12 H32 Li1 N4 1+,C20 H54 Li1 Si6 1- ; _journal_coden_Cambridge 186 _journal_year 1993 _journal_page_first 3259 _journal_name_full 'J.Chem.Soc.,Dalton Trans. ' loop_ _publ_author_name "A.G.Avent" "C.Eaborn" "P.B.Hitchcock" "G.A.Lawless" "P.D.Lickiss" "M.Mallien" "J.D.Smith" "A.D.Webb" "B.Wrackmeyer" _chemical_name_systematic ; bis(N,N,N',N'-Tetramethylethylenediamine)-lithium bis(tris(trimethylsilyl)methyl)-lithium ; _cell_volume 4899.153 _exptl_crystal_density_diffrn 0.96 _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; _refine_special_details ; The anion is disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.093 _refine_ls_wR_factor_gt 0.093 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I b a 2' _symmetry_Int_Tables_number 45 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,1/2+z 3 1/2-x,1/2+y,z 4 -x,y,1/2+z 5 1/2+x,1/2-y,z 6 x,-y,1/2+z 7 -x,-y,z 8 1/2-x,1/2-y,1/2+z _cell_length_a 19.252(2) _cell_length_b 14.006(2) _cell_length_c 18.169(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 Li 1.14 N 0.77 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Si1 Si 0.3888(3) 0.1451(4) 0.0611(4) Si2 Si 0.3394(3) -0.0589(5) 0.0339(4) Si3 Si 0.3724(4) 0.0703(5) -0.0993(4) Si4? Si 0.6260(3) -0.0723(6) 0.0887(4) Si5? Si 0.6605(3) 0.0580(4) -0.0396(3) Si6? Si 0.6054(3) -0.1445(5) -0.0715(5) Li1 Li 0.5000(1) 0.00000 0.00290 C1 C 0.3895(4) 0.0425(6) -0.0036(9) C2 C 0.2996(7) 0.1644(9) 0.0956(7) C3 C 0.4482(8) 0.1258(10) 0.1371(8) C4 C 0.4277(6) 0.2620(8) -0.0228(16) C5 C 0.3704(6) -0.1793(7) -0.0049(13) C6 C 0.2418(5) -0.0535(7) -0.0096(12) C7 C 0.3396(8) -0.0557(12) 0.1371(7) C8 C 0.3029(6) 0.1819(11) -0.1204(9) C9 C 0.4531(6) 0.1287(11) -0.1517(8) C10 C 0.3479(9) -0.0546(12) -0.1603(8) Li2 Li 0.50000 0.50000 0.2536(15) N1 N 0.4188(5) 0.5726(11) 0.1793(7) N2 N 0.4167(5) 0.4294(6) 0.2994(5) C11 C 0.3562(7) 0.4797(12) 0.2845(7) C12 C 0.3568(6) 0.5079(14) 0.205(1) C13 C 0.4220(8) 0.5583(12) 0.1000(7) C14 C 0.4218(9) 0.6791(11) 0.2156(13) C15 C 0.4040(7) 0.3317(9) 0.2822(8) C16 C 0.4232(12) 0.4101(14) 0.3836(10) C1F C 0.6105(4) -0.0425(6) -0.0036(9) Si1F Si 0.6112(3) -0.1451(4) 0.0611(4) Si2F Si 0.6606(3) 0.0589(5) 0.0339(4) Si3F Si 0.6276(4) -0.0703(5) -0.0993(4) C2F C 0.7004(7) -0.1644(9) 0.0956(7) C3F C 0.5518(8) -0.1258(10) 0.1371(8) C5F C 0.6296(6) 0.1793(7) -0.0049(13) C6F C 0.7582(5) 0.0535(7) -0.0096(12) C7F C 0.6604(8) 0.0557(12) 0.1371(7) C8F C 0.6971(6) -0.1819(11) -0.1204(9) C9F C 0.5469(6) -0.1287(11) -0.1517(8) C10F C 0.6521(9) 0.0546(12) -0.1603(8) N1F N 0.5812(5) 0.4274(11) 0.1793(7) N2F N 0.5833(5) 0.5706(6) 0.2994(5) C12F C 0.6432(6) 0.4921(14) 0.205(1) C13F C 0.5780(8) 0.4417(12) 0.1000(7) C14F C 0.5782(9) 0.3209(11) 0.2156(13) C11F C 0.6438(7) 0.5203(12) 0.2845(7) C15F C 0.5960(7) 0.6683(9) 0.2822(8) C16F C 0.5768(12) 0.5899(14) 0.3836(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Si1 C1 1.857 1_555 1_555 Si2 C1 1.847 1_555 1_555 Si3 C1 1.812 1_555 1_555 Li1 C1 2.212 1_555 1_555 C2 Si1 1.848 1_555 1_555 C3 Si1 1.813 1_555 1_555 C5 Si2 1.923 1_555 1_555 C6 Si2 2.040 1_555 1_555 C7 Si2 1.876 1_555 1_555 C8 Si3 2.093 1_555 1_555 C9 Si3 1.997 1_555 1_555 C10 Si3 2.124 1_555 1_555 Li2 N1 2.302 1_555 1_555 N1 C12 1.570 1_555 1_555 N2 Li2 2.060 1_555 1_555 C11 N2 1.388 1_555 1_555 C12 C11 1.498 1_555 1_555 C13 N1 1.456 1_555 1_555 C14 N1 1.632 1_555 1_555 C15 N2 1.425 1_555 1_555 C16 N2 1.559 1_555 1_555 C1F Li1 2.212 1_555 1_555 Si1F C1F 1.857 1_555 1_555 Si2F C1F 1.847 1_555 1_555 Si3F C1F 1.812 1_555 1_555 C2F Si1F 1.848 1_555 1_555 C3F Si1F 1.813 1_555 1_555 C5F Si2F 1.923 1_555 1_555 C6F Si2F 2.040 1_555 1_555 C7F Si2F 1.876 1_555 1_555 C8F Si3F 2.093 1_555 1_555 C9F Si3F 1.997 1_555 1_555 C10F Si3F 2.124 1_555 1_555 N1F Li2 2.302 1_555 1_555 N2F Li2 2.060 1_555 1_555 C12F N1F 1.570 1_555 1_555 C13F N1F 1.456 1_555 1_555 C14F N1F 1.632 1_555 1_555 C11F N2F 1.388 1_555 1_555 C15F N2F 1.425 1_555 1_555 C16F N2F 1.559 1_555 1_555 C12F C11F 1.498 1_555 1_555 #END data_CSD_CIF_PEZPAL _audit_creation_date 1994-05-24 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD PEZPAL _chemical_formula_sum 'C20 H40 K1 Na1 O10' _chemical_formula_moiety ; C20 H40 K1 O10 1+,Na1 1- ; _journal_coden_Cambridge 4 _journal_volume 115 _journal_year 1993 _journal_page_first 9542 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "R.H.Huang" "J.L.Eglin" "S.Z.Huang" "L.E.H.McMills" "J.L.Dye" _chemical_name_systematic ; 1,4,7,10,13,16-Hexaoxacyclo-octadecane-1,4,7,10-tetra-oxacyclododecane-potassi um sodide ; _cell_volume 3172.372 _diffrn_ambient_temperature 210 _refine_special_details ; The 12-crown-4 moeity is disordered with two C atoms having respective occupancies of 0.65,0.35,0.525 and 0.475, whilst the remainder have occupancies of 0.5. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.047 _refine_ls_wR_factor_gt 0.047 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2+z 3 x,1/2-y,z 4 1/2-x,-y,1/2+z 5 -x,-y,-z 6 -1/2+x,-1/2-y,-1/2-z 7 -x,-1/2+y,-z 8 -1/2+x,y,-1/2-z _cell_length_a 13.735(5) _cell_length_b 13.679(5) _cell_length_c 16.885(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 K 2.06 Na 0.97 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z K1 K 0.3937(1) 0.25000 0.3461(1) Na1 Na 0.1075(3) 0.75000 0.3607(2) O1 O 0.5717(3) 0.25000 0.4411(3) O2 O 0.5031(3) 0.0676(3) 0.3843(3) O3 O 0.4254(3) 0.0780(4) 0.2334(3) O4 O 0.3477(4) 0.25000 0.1738(4) O5 O 0.2159(3) 0.3523(3) 0.3411(2) O6 O 0.3009(3) 0.3535(4) 0.4933(3) C1 C 0.5696(5) 0.1625(6) 0.4872(4) C2 C 0.5828(5) 0.0782(6) 0.4337(5) C3 C 0.5177(7) -0.0069(6) 0.3266(5) C4 C 0.4322(7) -0.0113(7) 0.2744(6) C5 C 0.3474(7) 0.0772(8) 0.1795(6) C6 C 0.3578(6) 0.162(1) 0.1289(5) C7 C 0.16550 0.39470 0.39620 C8? C 0.20980 0.43940 0.40620 C9 C 0.22250 0.39750 0.48870 C10? C 0.23950 0.06430 0.43660 C11 C 0.29670 0.27380 0.56610 C12? C 0.24750 0.17310 0.54850 C13 C 0.14200 0.28060 0.29740 C14? C 0.13460 0.18390 0.34360 H1 H 0.618(4) 0.169(4) 0.527(3) H2 H 0.509(4) 0.159(3) 0.516(2) H3 H 0.594(4) 0.029(4) 0.462(4) H4 H 0.648(4) 0.075(4) 0.398(3) H5 H 0.586(4) 0.006(4) 0.299(3) H6 H 0.530(4) -0.068(4) 0.350(3) H7 H 0.367(5) -0.033(5) 0.297(4) H8 H 0.450(4) -0.063(5) 0.236(4) H9 H 0.344(6) 0.022(5) 0.160(4) H10 H 0.269(6) 0.074(5) 0.212(4) H11 H 0.313(3) 0.175(4) 0.095(3) H12 H 0.418(4) 0.171(4) 0.103(3) H13? H 0.25990 0.48570 0.39620 H14 H 0.14820 0.47070 0.40250 H15 H 0.17080 0.35330 0.49950 H16 H 0.22150 0.44910 0.52630 H17? H 0.36180 0.26110 0.58210 H18 H 0.26210 0.30320 0.60860 H19 H 0.07960 0.31040 0.29480 H20? H 0.16470 0.26780 0.24530 O2B O 0.5031(3) 0.4324(3) 0.3843(3) C2B C 0.5828(5) 0.4218(6) 0.4337(5) C1B C 0.5696(5) 0.3375(6) 0.4872(4) H1B H 0.618(4) 0.331(4) 0.527(3) H2B H 0.509(4) 0.341(3) 0.516(2) H3B H 0.594(4) 0.471(4) 0.462(4) H4B H 0.648(4) 0.425(4) 0.398(3) C3B C 0.5177(7) 0.5069(6) 0.3266(5) C4B C 0.4322(7) 0.5113(7) 0.2744(6) O3B O 0.4254(3) 0.4220(4) 0.2334(3) O5B O 0.2159(3) 0.1477(3) 0.3411(2) C7B C 0.16550 0.10530 0.39620 C9B C 0.22250 0.10250 0.48870 O6B O 0.3009(3) 0.1465(4) 0.4933(3) C11B C 0.29670 0.22620 0.56610 H18B H 0.26210 0.19680 0.60860 H15B H 0.17080 0.14670 0.49950 H16B H 0.22150 0.05090 0.52630 H14B H 0.14820 0.02930 0.40250 C13B C 0.14200 0.21940 0.29740 H19B H 0.07960 0.18960 0.29480 C6B C 0.3578(6) 0.338(1) 0.1289(5) C5B C 0.3474(7) 0.4228(8) 0.1795(6) H9B H 0.344(6) 0.478(5) 0.160(4) H10B H 0.269(6) 0.426(5) 0.212(4) H11B H 0.313(3) 0.325(4) 0.095(3) H12B H 0.418(4) 0.329(4) 0.103(3) H7B H 0.367(5) 0.533(5) 0.297(4) H8B H 0.450(4) 0.563(5) 0.236(4) H5B H 0.586(4) 0.494(4) 0.299(3) H6B H 0.530(4) 0.568(4) 0.350(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 K1 O1 2.924 1_555 1_555 O1 C1 1.428 1_555 1_555 O2 K1 2.983 1_555 1_555 O3 K1 3.057 1_555 1_555 O4 K1 2.977 1_555 1_555 O5 K1 2.816 1_555 1_555 O6 K1 3.132 1_555 1_555 C1 C2 1.476 1_555 1_555 C2 O2 1.384 1_555 1_555 C3 O2 1.424 1_555 1_555 C4 O3 1.407 1_555 1_555 C5 O3 1.406 1_555 1_555 C6 O4 1.429 1_555 1_555 C7 O5 1.297 1_555 1_555 C9 O6 1.236 1_555 1_555 C11 O6 1.644 1_555 1_555 C13 O5 1.593 1_555 1_555 H1 C1 0.949 1_555 1_555 H2 C1 0.965 1_555 1_555 H3 C2 0.840 1_555 1_555 H4 C2 1.080 1_555 1_555 H5 C3 1.062 1_555 1_555 H6 C3 0.940 1_555 1_555 H7 C4 1.018 1_555 1_555 H8 C4 0.990 1_555 1_555 H9 C5 0.825 1_555 1_555 H10 C5 1.209 1_555 1_555 H11 C6 0.859 1_555 1_555 H12 C6 0.943 1_555 1_555 H14 C7 1.072 1_555 1_555 H15 C9 0.950 1_555 1_555 H16 C9 0.949 1_555 1_555 H18 C11 0.950 1_555 1_555 H19 C13 0.950 1_555 1_555 O2B K1 2.983 1_555 1_555 C2B O2B 1.384 1_555 1_555 C1B O1 1.428 1_555 1_555 H1B C1B 0.949 1_555 1_555 H2B C1B 0.965 1_555 1_555 H3B C2B 0.840 1_555 1_555 H4B C2B 1.080 1_555 1_555 C3B O2B 1.424 1_555 1_555 C4B C3B 1.470 1_555 1_555 O3B K1 3.057 1_555 1_555 O5B K1 2.816 1_555 1_555 C7B O5B 1.297 1_555 1_555 C9B C7B 1.748 1_555 1_555 O6B K1 3.132 1_555 1_555 C11B C11 0.651 1_555 1_555 H18B C11B 0.950 1_555 1_555 H15B C9B 0.950 1_555 1_555 H16B C9B 0.949 1_555 1_555 H14B C7B 1.072 1_555 1_555 C13B C13 0.837 1_555 1_555 H19B C13B 0.950 1_555 1_555 C6B O4 1.429 1_555 1_555 C5B O3B 1.406 1_555 1_555 H9B C5B 0.825 1_555 1_555 H10B C5B 1.209 1_555 1_555 H11B C6B 0.859 1_555 1_555 H12B C6B 0.943 1_555 1_555 H7B C4B 1.018 1_555 1_555 H8B C4B 0.990 1_555 1_555 H5B C3B 1.062 1_555 1_555 H6B C3B 0.940 1_555 1_555 C3 C4 1.470 1_555 1_555 C5 C6 1.448 1_555 1_555 C7 C9 1.748 1_555 1_555 C2B C1B 1.476 1_555 1_555 C4B O3B 1.407 1_555 1_555 O5B C13B 1.593 1_555 1_555 C9B O6B 1.236 1_555 1_555 O6B C11B 1.644 1_555 1_555 C6B C5B 1.448 1_555 1_555 #END data_CSD_CIF_PEZPEP _audit_creation_date 1994-05-24 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD PEZPEP _chemical_formula_sum 'C20 H40 K2 O10' _chemical_formula_moiety ; C20 H40 K1 O10 1+,K1 1- ; _journal_coden_Cambridge 4 _journal_volume 115 _journal_year 1993 _journal_page_first 9542 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "R.H.Huang" "J.L.Eglin" "S.Z.Huang" "L.E.H.McMills" "J.L.Dye" _chemical_name_systematic ; 1,4,7,10,13,16-Hexaoxacyclo-octadecane-1,4,7,10-tetraoxacyclododecane-potassiu m potasside ; _cell_volume 3315.784 _exptl_crystal_colour 'red' _diffrn_ambient_temperature 210 _refine_special_details ; The 12-crown-4 moeity is disordered with occupancies of 0.5. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.037 _refine_ls_wR_factor_gt 0.037 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2+z 3 x,1/2-y,z 4 1/2-x,-y,1/2+z 5 -x,-y,-z 6 -1/2+x,-1/2-y,-1/2-z 7 -x,-1/2+y,-z 8 -1/2+x,y,-1/2-z _cell_length_a 13.795(26) _cell_length_b 14.090(24) _cell_length_c 17.059(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 K 2.06 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z K1 K 0.3927(1) 0.25000 0.3507(1) K2 K 0.1054(2) 0.75000 0.3550(2) O1 O 0.5705(4) 0.25000 0.4441(4) O2 O 0.5024(3) 0.0741(3) 0.3888(3) O3 O 0.4232(3) 0.0827(4) 0.2387(3) O4 O 0.3444(5) 0.25000 0.1796(4) O5 O 0.2148(3) 0.3489(3) 0.3472(3) O6 O 0.3033(3) 0.3484(4) 0.4985(3) C1 C 0.5683(6) 0.1659(6) 0.4904(4) C2 C 0.5830(6) 0.0842(6) 0.4384(5) C3 C 0.5175(7) 0.0034(6) 0.3316(6) C4 C 0.4312(7) -0.0031(6) 0.2797(6) C5 C 0.3450(6) 0.0845(8) 0.1834(5) C6 C 0.3535(6) 0.1686(8) 0.1335(5) C7? C 0.156(1) 0.390(1) 0.3979(8) C8 C 0.222(1) 0.424(1) 0.4152(7) C9 C 0.227(1) 0.383(1) 0.5053(9) C10? C 0.243(1) 0.424(1) 0.4553(7) C11 C 0.3044(9) 0.276(1) 0.5692(6) C12? C 0.244(1) 0.325(1) 0.5531(7) C13 C 0.1425(7) 0.2810(8) 0.3047(5) C14? C 0.130(1) 0.315(1) 0.3564(7) H1 H 0.61750 0.16790 0.52890 H2 H 0.50640 0.16090 0.51570 H3 H 0.58980 0.02760 0.46850 H4 H 0.63910 0.09330 0.40740 H5 H 0.57240 0.01910 0.30160 H6 H 0.52630 -0.05560 0.35700 H7 H 0.37370 -0.01300 0.30940 H8 H 0.43880 -0.05340 0.24310 H9 H 0.34740 0.02800 0.15160 H10 H 0.28440 0.08540 0.21010 H11 H 0.30540 0.16710 0.09410 H12 H 0.41630 0.16770 0.10910 H13 H 0.22560 0.48310 0.39050 H14 H 0.15340 0.42190 0.43850 H15? H 0.18950 0.45990 0.48040 H16? H 0.28170 0.48300 0.43190 H17? H 0.37050 0.26300 0.59210 H18? H 0.26950 0.29850 0.61910 H19 H 0.07240 0.29790 0.30720 H20? H 0.15490 0.26510 0.25170 O2B O 0.5024(3) 0.4259(3) 0.3888(3) C2B C 0.5830(6) 0.4158(6) 0.4384(5) C1B C 0.5683(6) 0.3341(6) 0.4904(4) H1B H 0.61750 0.33210 0.52890 H2B H 0.50640 0.33910 0.51570 H3B H 0.58980 0.47240 0.46850 H4B H 0.63910 0.40670 0.40740 C3B C 0.5175(7) 0.4966(6) 0.3316(6) C4B C 0.4312(7) 0.5031(6) 0.2797(6) O3B O 0.4232(3) 0.4173(4) 0.2387(3) O5B O 0.2148(3) 0.1511(3) 0.3472(3) C8B C 0.222(1) 0.076(1) 0.4152(7) C9B C 0.227(1) 0.117(1) 0.5053(9) O6B O 0.3033(3) 0.1516(4) 0.4985(3) C11B C 0.3044(9) 0.224(1) 0.5692(6) H13B H 0.22560 0.01690 0.39050 H14B H 0.15340 0.07810 0.43850 C13B C 0.1425(7) 0.2190(8) 0.3047(5) H19B H 0.07240 0.20210 0.30720 C6B C 0.3535(6) 0.3314(8) 0.1335(5) C5B C 0.3450(6) 0.4155(8) 0.1834(5) H9B H 0.34740 0.47200 0.15160 H10B H 0.28440 0.41460 0.21010 H11B H 0.30540 0.33290 0.09410 H12B H 0.41630 0.33230 0.10910 H7B H 0.37370 0.51300 0.30940 H8B H 0.43880 0.55340 0.24310 H5B H 0.57240 0.48090 0.30160 H6B H 0.52630 0.55560 0.35700 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 K1 O1 2.925 1_555 1_555 O1 C1 1.424 1_555 1_555 O2 K1 2.976 1_555 1_555 O3 K1 3.063 1_555 1_555 O4 K1 2.994 1_555 1_555 O5 K1 2.823 1_555 1_555 O6 K1 3.131 1_555 1_555 C1 C2 1.467 1_555 1_555 C2 O2 1.404 1_555 1_555 C3 O2 1.410 1_555 1_555 C4 O3 1.401 1_555 1_555 C5 O3 1.433 1_555 1_555 C6 O4 1.396 1_555 1_555 C8 O5 1.573 1_555 1_555 C9 O6 1.166 1_555 1_555 C11 O6 1.580 1_555 1_555 C13 O5 1.561 1_555 1_555 H1 C1 0.945 1_555 1_555 H2 C1 0.959 1_555 1_555 H3 C2 0.953 1_555 1_555 H4 C2 0.946 1_555 1_555 H5 C3 0.940 1_555 1_555 H6 C3 0.945 1_555 1_555 H7 C4 0.951 1_555 1_555 H8 C4 0.950 1_555 1_555 H9 C5 0.964 1_555 1_555 H10 C5 0.952 1_555 1_555 H11 C6 0.945 1_555 1_555 H12 C6 0.961 1_555 1_555 H13 C8 0.935 1_555 1_555 H14 C8 1.027 1_555 1_555 H19 C13 0.997 1_555 1_555 O2B K1 2.976 1_555 1_555 C2B O2B 1.404 1_555 1_555 C1B O1 1.424 1_555 1_555 H1B C1B 0.945 1_555 1_555 H2B C1B 0.959 1_555 1_555 H3B C2B 0.953 1_555 1_555 H4B C2B 0.946 1_555 1_555 C3B O2B 1.410 1_555 1_555 C4B C3B 1.486 1_555 1_555 O3B K1 3.063 1_555 1_555 O5B K1 2.823 1_555 1_555 C8B O5B 1.573 1_555 1_555 C9B C8B 1.643 1_555 1_555 O6B K1 3.131 1_555 1_555 C11B C11 0.733 1_555 1_555 H13B C8B 0.935 1_555 1_555 H14B C8B 1.027 1_555 1_555 C13B C13 0.874 1_555 1_555 H19B C13B 0.997 1_555 1_555 C6B O4 1.396 1_555 1_555 C5B O3B 1.433 1_555 1_555 H9B C5B 0.964 1_555 1_555 H10B C5B 0.952 1_555 1_555 H11B C6B 0.945 1_555 1_555 H12B C6B 0.961 1_555 1_555 H7B C4B 0.951 1_555 1_555 H8B C4B 0.950 1_555 1_555 H5B C3B 0.940 1_555 1_555 H6B C3B 0.945 1_555 1_555 C3 C4 1.486 1_555 1_555 C5 C6 1.464 1_555 1_555 C8 C9 1.643 1_555 1_555 C2B C1B 1.467 1_555 1_555 C4B O3B 1.401 1_555 1_555 O5B C13B 1.561 1_555 1_555 C9B O6B 1.166 1_555 1_555 O6B C11B 1.580 1_555 1_555 C6B C5B 1.464 1_555 1_555 #END data_CSD_CIF_PEZPIT _audit_creation_date 1994-05-24 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD PEZPIT _chemical_formula_sum 'C32 H64 K2 O16' _chemical_formula_moiety ; C20 H40 K1 O10 1+,K1 1-,C12 H24 O6 ; _journal_coden_Cambridge 4 _journal_volume 115 _journal_year 1993 _journal_page_first 9542 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "R.H.Huang" "J.L.Eglin" "S.Z.Huang" "L.E.H.McMills" "J.L.Dye" _chemical_name_systematic ; 1,4,7,10,13,16-Hexaoxacyclo-octadecane-1,4,7,10-tetraoxacyclododecane-potassiu m potasside 1,4,7,10,13,17-hexaoxacylo-octadecane ; _cell_volume 4852.812 _diffrn_ambient_temperature 210 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.055 _refine_ls_wR_factor_gt 0.055 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,-1/2-y,-1/2+z _cell_length_a 15.857(8) _cell_length_b 21.059(13) _cell_length_c 14.535(7) _cell_angle_alpha 90 _cell_angle_beta 88.898(40) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 K 2.10 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z K1 K 0.7421(2) 0.8037(1) 0.1583(2) K2 K 0.2423(3) 0.6308(2) -0.0050(3) O1 O 0.8504(5) 0.8595(3) 0.3074(5) O2 O 0.6729(5) 0.8643(3) 0.3443(5) O3 O 0.5600(4) 0.7977(3) 0.2351(5) O4 O 0.6264(5) 0.6842(3) 0.1624(5) O5 O 0.8003(4) 0.6701(3) 0.1230(5) O6 O 0.9087(5) 0.7487(3) 0.2239(5) O7 O 0.7071(5) 0.9315(4) 0.1219(5) O8 O 0.8669(5) 0.8827(3) 0.0676(6) O9 O 0.8029(5) 0.7949(4) -0.0491(6) O10 O 0.6371(6) 0.8369(4) 0.0057(5) O11 O 0.3756(5) 0.9106(3) 0.0558(5) O12 O 0.4691(4) 0.9903(3) 0.1840(5) O13 O 0.5579(5) 1.1023(3) 0.1273(5) O14 O 0.8871(5) 1.0983(3) 0.0738(5) O15 O 0.9169(5) 1.0729(4) -0.1203(5) O16 O 0.9891(5) 0.9538(4) -0.1893(5) C1 C 0.8135(7) 0.8888(5) 0.3868(8) C2 C 0.7278(7) 0.9155(5) 0.3625(8) C3 C 0.5880(8) 0.8855(5) 0.3292(8) C4 C 0.5357(8) 0.8273(5) 0.3174(8) C5 C 0.5078(7) 0.7438(5) 0.2178(8) C6 C 0.5453(7) 0.7099(5) 0.1377(8) C7 C 0.6586(8) 0.6407(5) 0.0963(8) C8 C 0.7420(7) 0.6191(5) 0.1277(8) C9 C 0.8841(7) 0.6526(5) 0.1429(7) C10 C 0.9375(7) 0.7110(5) 0.1483(8) C11 C 0.9628(7) 0.8010(5) 0.2413(8) C12 C 0.9300(7) 0.8335(5) 0.3285(8) C13 C 0.7778(8) 0.9690(6) 0.113(1) C14 C 0.8492(9) 0.9462(6) 0.079(1) C15 C 0.899(1) 0.8711(8) -0.0189(8) C16 C 0.861(1) 0.8348(7) -0.0795(9) C17 C 0.7311(9) 0.7940(7) -0.106(1) C18 C 0.6554(9) 0.817(1) -0.076(1) C19 C 0.604(1) 0.8995(6) 0.020(1) C20 C 0.6429(9) 0.9432(7) 0.0624(9) C21 C 0.3816(8) 0.9002(6) 0.1510(8) C22 C 0.3889(7) 0.9632(6) 0.2007(8) C23 C 0.4843(8) 1.0435(5) 0.2429(8) C24 C 0.5665(8) 1.0736(5) 0.2135(7) C25 C 0.6309(7) 1.1325(5) 0.0940(8) C26 C 0.3768(8) 0.8526(5) 0.0050(8) C27 C 0.8719(8) 1.1411(5) 0.0017(9) C28 C 0.8471(7) 1.1074(6) -0.0847(8) C29 C 0.8907(8) 1.0401(6) -0.2005(9) C30 C 0.9687(9) 1.0085(6) -0.2431(9) C31 C 1.0627(8) 0.9238(6) -0.2232(8) C32 C 0.9082(7) 1.1277(5) 0.1594(8) H1 H 0.84800 0.92300 0.40700 H2 H 0.80600 0.85900 0.43500 H3 H 0.70500 0.94100 0.41000 H4 H 0.73500 0.94000 0.30800 H5 H 0.58600 0.91100 0.27500 H6 H 0.56900 0.91000 0.38100 H7 H 0.54300 0.79900 0.36800 H8 H 0.47800 0.84000 0.31500 H9 H 0.45200 0.75700 0.20500 H10 H 0.50700 0.71600 0.26900 H11 H 0.51000 0.67600 0.11900 H12 H 0.55200 0.73900 0.08800 H13 H 0.66600 0.66100 0.03900 H14 H 0.62100 0.60600 0.09000 H15 H 0.73600 0.60500 0.18900 H16 H 0.76300 0.58500 0.09000 H17 H 0.90500 0.62500 0.09600 H18 H 0.88600 0.63200 0.20100 H19 H 0.99500 0.70000 0.15600 H20 H 0.93200 0.73400 0.09300 H21 H 0.96500 0.83000 0.19100 H22 H 1.01700 0.78400 0.25200 H23 H 0.92500 0.80400 0.37800 H24 H 0.96700 0.86700 0.34500 H25 H 0.78800 0.98500 0.17300 H26 H 0.76200 1.00300 0.07400 H27 H 0.85700 0.96500 0.02000 H28 H 0.89100 0.96200 0.12000 H29 H 0.95400 0.85500 -0.01100 H30 H 0.90300 0.91100 -0.04900 H31 H 0.83600 0.86100 -0.12500 H32 H 0.90400 0.80900 -0.10800 H33 H 0.80200 1.08300 -0.07100 H34 H 0.83000 1.14100 -0.13000 H35 H 0.86800 1.06400 -0.23800 H36 H 0.85400 1.00400 -0.17900 H37 H 0.71960 0.75300 -0.11500 H38 H 0.75100 0.81400 -0.16400 H39 H 0.65300 0.85800 -0.11100 H40 H 0.61000 0.79300 -0.09800 H41 H 0.55900 0.88700 0.06500 H42 H 0.58100 0.91000 -0.03400 H43 H 0.67000 0.96600 0.01000 H44 H 0.60300 0.97100 0.09000 H45 H 0.33300 0.87700 0.17500 H46 H 0.43100 0.87700 0.16400 H47 H 0.37900 0.95700 0.26400 H48 H 0.34500 0.99000 0.17600 H49 H 0.95700 1.00000 -0.30500 H50 H 1.01600 1.03500 -0.22700 H51 H 0.33200 0.82600 0.02600 H52 H 0.42900 0.83200 0.01400 H53 H 0.44100 1.07500 0.23200 H54 H 0.48400 1.03100 0.30200 H55 H 0.60700 1.04300 0.21400 H56 H 0.58000 1.10700 0.26000 H57 H 1.05400 0.90600 -0.28200 H58 H 1.10800 0.95300 -0.22600 H59 H 0.86100 1.15000 0.18400 H60 H 0.95300 1.15600 0.15200 H61 H 0.64200 1.16900 0.13000 H62 H 0.68000 1.10300 0.10200 H63 H 0.92000 1.16500 -0.01300 H64 H 0.82700 1.17000 0.02000 C26B C 0.6232(8) 1.1474(5) -0.0050(8) C25B C 0.3691(7) 0.8675(5) -0.0940(8) O11B O 0.6244(5) 1.0894(3) -0.0558(5) H51B H 0.66800 1.17400 -0.02600 H52B H 0.57100 1.16800 -0.01400 O13B O 0.4421(5) 0.8977(3) -0.1273(5) H61B H 0.35800 0.83100 -0.13000 H62B H 0.32000 0.89700 -0.10200 C21B C 0.6184(8) 1.0998(6) -0.1510(8) C24B C 0.4335(8) 0.9264(5) -0.2135(7) C22B C 0.6111(7) 1.0368(6) -0.2007(8) H45B H 0.66700 1.12300 -0.17500 H46B H 0.56900 1.12300 -0.16400 C23B C 0.5157(8) 0.9565(5) -0.2429(8) H55B H 0.39300 0.95700 -0.21400 H56B H 0.42000 0.89300 -0.26000 O12B O 0.5309(4) 1.0097(3) -0.1840(5) H47B H 0.62100 1.04300 -0.26400 H48B H 0.65500 1.01000 -0.17600 H53B H 0.55900 0.92500 -0.23200 H54B H 0.51600 0.96900 -0.30200 C32B C 1.0918(7) 0.8723(5) -0.1594(8) C31B C 0.9373(8) 1.0762(6) 0.2232(8) O14B O 1.1129(5) 0.9017(3) -0.0738(5) H59B H 1.13900 0.85000 -0.18400 H60B H 1.04700 0.84400 -0.15200 O16B O 1.0109(5) 1.0462(4) 0.1893(5) H57B H 0.94600 1.09400 0.28200 H58B H 0.89200 1.04700 0.22600 C27B C 1.1281(8) 0.8589(5) -0.0017(9) C30B C 1.0313(9) 0.9915(6) 0.2431(9) C28B C 1.1529(7) 0.8926(6) 0.0847(8) H63B H 1.08000 0.83500 0.01300 H64B H 1.17300 0.83000 -0.02000 C29B C 1.1093(8) 0.9599(6) 0.2005(9) H49B H 1.04300 1.00000 0.30500 H50B H 0.98400 0.96500 0.22700 O15B O 1.0831(5) 0.9271(4) 0.1203(5) H33B H 1.19800 0.91700 0.07100 H34B H 1.17000 0.85900 0.13000 H35B H 1.13200 0.93600 0.23800 H36B H 1.14600 0.99600 0.17900 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 K1 O1 3.028 1_555 1_555 O1 C1 1.424 1_555 1_555 O2 K1 3.167 1_555 1_555 O3 K1 3.078 1_555 1_555 O4 K1 3.114 1_555 1_555 O5 K1 3.002 1_555 1_555 O6 K1 3.054 1_555 1_555 O7 K1 2.800 1_555 1_555 O8 K1 2.885 1_555 1_555 O9 K1 3.153 1_555 1_555 O10 K1 2.885 1_555 1_555 O11 C21 1.406 1_555 1_555 O12 C22 1.411 1_555 1_555 O13 C24 1.400 1_555 1_555 O14 C27 1.407 1_555 1_555 O15 C28 1.414 1_555 1_555 O16 C30 1.433 1_555 1_555 C1 C2 1.519 1_555 1_555 C2 O2 1.414 1_555 1_555 C3 O2 1.439 1_555 1_555 C4 O3 1.397 1_555 1_555 C5 O3 1.430 1_555 1_555 C6 O4 1.447 1_555 1_555 C7 O4 1.416 1_555 1_555 C8 O5 1.418 1_555 1_555 C9 O5 1.414 1_555 1_555 C10 O6 1.424 1_555 1_555 C11 O6 1.422 1_555 1_555 C12 O1 1.415 1_555 1_555 C13 O7 1.375 1_555 1_555 C14 O8 1.376 1_555 1_555 C15 O8 1.369 1_555 1_555 C16 O9 1.317 1_555 1_555 C17 O9 1.420 1_555 1_555 C18 O10 1.287 1_555 1_555 C19 O10 1.433 1_555 1_555 C20 O7 1.371 1_555 1_555 C21 C22 1.516 1_555 1_555 C22 H47 0.939 1_555 1_555 C23 O12 1.433 1_555 1_555 C24 C23 1.504 1_555 1_555 C25 O13 1.399 1_555 1_555 C26 O11 1.427 1_555 1_555 C27 C28 1.501 1_555 1_555 C28 H33 0.900 1_555 1_555 C29 O15 1.424 1_555 1_555 C30 C29 1.525 1_555 1_555 C31 O16 1.408 1_555 1_555 C32 O14 1.435 1_555 1_555 H1 C1 0.954 1_555 1_555 H2 C1 0.946 1_555 1_555 H3 C2 0.941 1_555 1_555 H4 C2 0.950 1_555 1_555 H5 C3 0.954 1_555 1_555 H6 C3 0.957 1_555 1_555 H7 C4 0.955 1_555 1_555 H8 C4 0.955 1_555 1_555 H9 C5 0.949 1_555 1_555 H10 C5 0.947 1_555 1_555 H11 C6 0.950 1_555 1_555 H12 C6 0.952 1_555 1_555 H13 C7 0.941 1_555 1_555 H14 C7 0.949 1_555 1_555 H15 C8 0.942 1_555 1_555 H16 C8 0.959 1_555 1_555 H17 C9 0.951 1_555 1_555 H18 C9 0.950 1_555 1_555 H19 C10 0.949 1_555 1_555 H20 C10 0.944 1_555 1_555 H21 C11 0.953 1_555 1_555 H22 C11 0.947 1_555 1_555 H23 C12 0.953 1_555 1_555 H24 C12 0.951 1_555 1_555 H25 C13 0.952 1_555 1_555 H26 C13 0.950 1_555 1_555 H27 C14 0.950 1_555 1_555 H28 C14 0.959 1_555 1_555 H29 C15 0.945 1_555 1_555 H30 C15 0.949 1_555 1_555 H31 C16 0.953 1_555 1_555 H32 C16 0.960 1_555 1_555 H34 C28 1.007 1_555 1_555 H35 C29 0.829 1_555 1_555 H36 C29 1.004 1_555 1_555 H37 C17 0.893 1_555 1_555 H38 C17 0.989 1_555 1_555 H39 C18 1.003 1_555 1_555 H40 C18 0.941 1_555 1_555 H41 C19 0.994 1_555 1_555 H42 C19 0.899 1_555 1_555 H43 C20 0.991 1_555 1_555 H44 C20 0.946 1_555 1_555 H45 C21 0.972 1_555 1_555 H46 C21 0.945 1_555 1_555 H48 C22 0.970 1_555 1_555 H49 C30 0.939 1_555 1_555 H50 C30 0.967 1_555 1_555 H51 C26 0.950 1_555 1_555 H52 C26 0.946 1_555 1_555 H53 C23 0.970 1_555 1_555 H54 C23 0.898 1_555 1_555 H55 C24 0.910 1_555 1_555 H56 C24 1.001 1_555 1_555 H57 C31 0.946 1_555 1_555 H58 C31 0.946 1_555 1_555 H59 C32 0.948 1_555 1_555 H60 C32 0.932 1_555 1_555 H61 C25 0.948 1_555 1_555 H62 C25 1.005 1_555 1_555 H63 C27 0.935 1_555 1_555 H64 C27 0.970 1_555 1_555 C26B C25 1.480 1_555 1_555 C25B C26 1.480 1_555 1_555 O11B C26B 1.427 1_555 1_555 H51B C26B 0.950 1_555 1_555 H52B C26B 0.946 1_555 1_555 O13B C25B 1.399 1_555 1_555 H61B C25B 0.948 1_555 1_555 H62B C25B 1.005 1_555 1_555 C21B O11B 1.406 1_555 1_555 C24B O13B 1.400 1_555 1_555 C22B C21B 1.516 1_555 1_555 H45B C21B 0.972 1_555 1_555 H46B C21B 0.945 1_555 1_555 C23B C24B 1.504 1_555 1_555 H55B C24B 0.910 1_555 1_555 H56B C24B 1.001 1_555 1_555 O12B C22B 1.411 1_555 1_555 H47B C22B 0.939 1_555 1_555 H48B C22B 0.970 1_555 1_555 H53B C23B 0.970 1_555 1_555 H54B C23B 0.898 1_555 1_555 C32B C31 1.505 1_555 1_555 C31B C32 1.505 1_555 1_555 O14B C32B 1.435 1_555 1_555 H59B C32B 0.948 1_555 1_555 H60B C32B 0.932 1_555 1_555 O16B C31B 1.408 1_555 1_555 H57B C31B 0.946 1_555 1_555 H58B C31B 0.946 1_555 1_555 C27B O14B 1.407 1_555 1_555 C30B O16B 1.433 1_555 1_555 C28B C27B 1.501 1_555 1_555 H63B C27B 0.935 1_555 1_555 H64B C27B 0.970 1_555 1_555 C29B C30B 1.525 1_555 1_555 H49B C30B 0.939 1_555 1_555 H50B C30B 0.967 1_555 1_555 O15B C28B 1.414 1_555 1_555 H33B C28B 0.900 1_555 1_555 H34B C28B 1.007 1_555 1_555 H35B C29B 0.829 1_555 1_555 H36B C29B 1.004 1_555 1_555 C3 C4 1.492 1_555 1_555 C5 C6 1.481 1_555 1_555 C7 C8 1.479 1_555 1_555 C9 C10 1.496 1_555 1_555 C11 C12 1.523 1_555 1_555 C13 C14 1.317 1_555 1_555 C15 C16 1.320 1_555 1_555 C17 C18 1.358 1_555 1_555 C19 C20 1.274 1_555 1_555 C23B O12B 1.433 1_555 1_555 C29B O15B 1.424 1_555 1_555 #END data_CSD_CIF_QOMCOK _audit_creation_date 2001-08-08 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD QOMCOK _database_code_depnum_ccdc_archive 'CCDC 164839' _chemical_formula_sum 'C54 H112 B20 Li4 O7 Si2' _chemical_formula_moiety ; C16 H32 Li1 O4 1+,C34 H72 B20 Li3 O2 Si2 1-,C4 H8 O1 ; _journal_coden_Cambridge 579 _journal_volume 20 _journal_year 2001 _journal_page_first 2359 _journal_name_full 'Organometallics ' loop_ _publ_author_name "Guofu Zi" "Qingchuan Yang" "T.C.W.Mak" "Zuowei Xie" _chemical_name_systematic ; tetrakis(Tetrahydrofuran-O)-lithium bis(\m~2~-\h^5^,\h^5^-(1-(2,3,4,5-tetramethyl-cyclopentadienyl)dimethylsilyl)- 1,2-dicarbadodecaboran-2-yl)-bis(tetrahydrofuran-O)-tri-lithium tetrahydrofuran solvate ; _cell_volume 7407.788 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.052 _exptl_crystal_description 'block' _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.1092 _refine_ls_wR_factor_gt 0.1092 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x,-y,1/2+z 3 1/2+x,1/2+y,z 4 1/2+x,1/2-y,1/2+z _cell_length_a 38.213(8) _cell_length_b 10.460(2) _cell_length_c 18.533(4) _cell_angle_alpha 90 _cell_angle_beta 90.00(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.73 H 0.23 B 0.83 Li 1.37 O 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Si1 Si 0.27764(3) 0.95134(10) 0.41826(5) Si2 Si 0.17372(2) 1.55084(10) 0.30471(5) Li1 Li 0.30502(18) 1.2178(6) 0.5021(4) Li2 Li 0.14795(15) 1.2825(6) 0.2236(3) Li3 Li 0.22383(15) 1.2451(6) 0.3704(3) O1 O 0.31345(8) 1.3331(3) 0.58394(15) O2 O 0.13688(7) 1.1692(3) 0.14052(15) C1 C 0.31824(8) 0.9260(3) 0.47345(17) C2 C 0.33433(7) 1.0463(3) 0.51434(12) B1 B 0.35487(10) 0.9933(5) 0.44465(19) H1 H 0.35740 1.04440 0.39300 B2 B 0.34916(9) 0.8136(3) 0.4583(2) H2 H 0.34800 0.74540 0.41320 B3 B 0.32304(10) 0.7889(5) 0.5287(2) H3 H 0.30360 0.71140 0.53130 B4 B 0.31400(9) 0.9443(3) 0.56505(18) H4 H 0.28940 0.97220 0.59140 B5 B 0.37750(12) 1.0333(3) 0.5282(2) H5 H 0.39470 1.11760 0.53150 B6 B 0.39003(11) 0.8920(4) 0.4854(3) H6 H 0.41520 0.88290 0.45710 B7 B 0.36852(8) 0.7607(3) 0.53476(15) H7 H 0.38010 0.66480 0.53910 B8 B 0.34558(11) 0.8321(2) 0.6000(2) H8 H 0.34110 0.77800 0.65000 B9 B 0.35187(12) 0.9907(3) 0.5998(3) H9 H 0.35220 1.04310 0.65130 B10 B 0.38785(14) 0.8934(2) 0.5807(3) H10 H 0.41130 0.88410 0.61480 C3 C 0.13275(8) 1.5881(3) 0.24339(14) C4 C 0.11395(10) 1.4424(4) 0.2022(2) B11 B 0.09266(9) 1.5296(4) 0.2753(2) H11 H 0.08900 1.48120 0.32750 B12 B 0.10158(12) 1.6972(5) 0.2772(3) H12 H 0.10300 1.75320 0.32730 B13 B 0.12870(13) 1.7211(4) 0.1994(3) H13 H 0.14730 1.80120 0.20080 B14 B 0.13648(16) 1.5684(5) 0.15809(17) H14 H 0.16220 1.55390 0.13270 B15 B 0.06872(8) 1.4808(3) 0.20025(16) H15 H 0.04820 1.40740 0.20470 B16 B 0.06191(11) 1.6376(4) 0.2382(3) H16 H 0.03730 1.66630 0.26440 B17 B 0.08372(13) 1.7473(6) 0.1874(3) H17 H 0.07410 1.84500 0.17810 B18 B 0.10462(13) 1.6563(6) 0.1127(3) H18 H 0.10840 1.69190 0.05740 B19 B 0.09429(11) 1.4858(5) 0.12725(19) H19 H 0.09140 1.41520 0.08370 B20 B 0.06452(13) 1.6087(3) 0.1468(2) H20 H 0.04130 1.61990 0.11230 C5 C 0.26743(9) 1.1274(3) 0.4269(2) C6 C 0.24483(9) 1.1893(4) 0.47586(17) C7 C 0.24995(8) 1.3327(3) 0.47000(17) C8 C 0.27297(8) 1.3413(3) 0.41033(18) C9 C 0.28303(9) 1.2181(4) 0.38065(19) C10 C 0.22161(9) 1.1368(4) 0.5314(3) H21 H 0.19840 1.12800 0.51210 H22 H 0.22110 1.19350 0.57210 H23 H 0.23010 1.05460 0.54630 C11 C 0.23521(10) 1.4348(3) 0.5084(2) H24 H 0.21460 1.46420 0.48390 H25 H 0.25190 1.50330 0.51160 H26 H 0.22910 1.40680 0.55610 C12 C 0.28417(11) 1.4712(4) 0.3794(3) H27 H 0.26790 1.49690 0.34260 H28 H 0.30720 1.46400 0.35890 H29 H 0.28440 1.53380 0.41720 C13 C 0.30707(9) 1.2204(4) 0.31885(19) H30 H 0.29380 1.22170 0.27480 H31 H 0.32160 1.14550 0.31990 H32 H 0.32150 1.29540 0.32140 C14 C 0.24065(10) 0.8383(4) 0.4560(3) H33 H 0.23380 0.86670 0.50320 H34 H 0.24940 0.75230 0.45900 H35 H 0.22080 0.84070 0.42430 C15 C 0.28913(10) 0.8916(4) 0.3254(2) H36 H 0.30690 0.94520 0.30490 H37 H 0.26870 0.89380 0.29530 H38 H 0.29760 0.80540 0.32870 C16 C 0.30144(13) 1.2965(5) 0.6597(2) H39 H 0.27630 1.30540 0.66540 H40 H 0.30850 1.21030 0.67250 C17 C 0.32073(18) 1.3931(9) 0.7011(5) H41 H 0.30420 1.45600 0.71910 H42 H 0.33140 1.35200 0.74260 C18 C 0.34230(17) 1.4455(6) 0.6690(3) H43 H 0.36410 1.43750 0.69550 H44 H 0.33640 1.53570 0.66750 C19 C 0.34965(15) 1.3937(6) 0.5802(4) H45 H 0.35170 1.46240 0.54530 H46 H 0.36860 1.33280 0.57530 C20 C 0.18586(7) 1.3807(3) 0.30530(17) C21 C 0.16646(8) 1.2719(3) 0.33861(18) C22 C 0.17582(9) 1.1550(4) 0.3088(2) C23 C 0.20101(9) 1.1932(3) 0.2537(2) C24 C 0.20510(8) 1.3145(4) 0.2487(2) C25 C 0.14350(11) 1.3005(4) 0.4072(2) H47 H 0.11950 1.31020 0.39310 H48 H 0.15150 1.37790 0.42960 H49 H 0.14550 1.23090 0.44070 C26 C 0.16406(11) 1.0233(4) 0.3357(2) H50 H 0.14470 0.99400 0.30710 H51 H 0.15700 1.02940 0.38530 H52 H 0.18310 0.96390 0.33160 C27 C 0.21975(10) 1.0907(4) 0.2039(2) H53 H 0.20690 1.08170 0.15970 H54 H 0.22050 1.00990 0.22840 H55 H 0.24320 1.11860 0.19350 C28 C 0.22888(10) 1.3817(4) 0.19119(19) H56 H 0.21590 1.39350 0.14740 H57 H 0.24900 1.32950 0.18180 H58 H 0.23630 1.46340 0.20920 C29 C 0.16601(12) 1.6147(5) 0.3975(3) H59 H 0.18600 1.59670 0.42730 H60 H 0.14570 1.57470 0.41790 H61 H 0.16240 1.70540 0.39520 C30 C 0.20848(9) 1.6520(4) 0.2671(3) H62 H 0.22960 1.64050 0.29460 H63 H 0.20140 1.74000 0.26930 H64 H 0.21270 1.62840 0.21780 C31 C 0.15064(12) 1.1718(6) 0.0757(3) H65 H 0.17030 1.11330 0.07430 H66 H 0.15950 1.25710 0.06640 C32 C 0.12406(12) 1.1343(4) 0.0135(2) H67 H 0.13430 1.07850 -0.02260 H68 H 0.11320 1.20790 -0.00920 C33 C 0.09808(14) 1.0599(5) 0.0689(3) H69 H 0.07460 1.09520 0.06700 H70 H 0.09710 0.96930 0.05790 C34 C 0.11347(15) 1.0813(5) 0.1361(2) H71 H 0.09500 1.10190 0.17000 H72 H 0.12400 1.00170 0.15190 Li4 Li -0.0089(2) 0.9233(8) 0.4660(6) O3 O -0.01713(9) 1.0185(4) 0.5565(2) C35 C -0.0453(2) 1.0023(5) 0.6006(2) H73 H -0.04390 0.91640 0.62010 H74 H -0.06600 1.00520 0.57040 C36 C -0.05166(7) 1.0924(4) 0.6640(2) H75 H -0.04910 1.05370 0.71130 H76 H -0.07280 1.14350 0.66050 C37 C -0.01841(9) 1.1566(4) 0.6341(4) C38 C 0.00696(8) 1.0429(4) 0.6259(3) O4 O -0.05315(9) 0.9151(4) 0.41497(19) C39 C -0.05807(15) 0.8575(7) 0.3550(3) H77 H -0.04340 0.78180 0.35360 H78 H -0.05070 0.91320 0.31600 C40 C -0.0923(3) 0.8221(5) 0.3437(2) H79 H -0.09900 0.82610 0.29330 H80 H -0.09770 0.73840 0.36340 C41 C -0.10643(16) 0.9209(7) 0.3843(5) H81 H -0.13010 0.89710 0.39730 H82 H -0.10800 0.99570 0.35360 C42 C -0.08864(19) 0.9574(5) 0.4488(2) H83 H -0.09540 0.90770 0.49070 H84 H -0.08990 1.04830 0.45890 O5 O 0.00190(8) 0.7526(3) 0.4768(2) C43 C 0.0307(2) 0.6690(9) 0.4523(7) H85 H 0.03540 0.69120 0.40240 H86 H 0.05130 0.69270 0.47980 C44 C 0.0282(2) 0.5440(8) 0.4552(5) H87 H 0.04720 0.50660 0.48290 H88 H 0.02770 0.50620 0.40740 C45 C -0.00652(13) 0.5299(5) 0.4932(4) H89 H -0.00640 0.46340 0.52970 H90 H -0.02590 0.51740 0.46020 C46 C -0.0053(2) 0.6752(6) 0.5277(4) H91 H -0.02780 0.69660 0.54890 H92 H 0.01240 0.68000 0.56510 O6 O 0.02364(9) 1.0246(4) 0.4119(3) C47 C 0.0321(3) 1.1336(5) 0.4517(3) H93 H 0.05150 1.12190 0.48470 H94 H 0.01230 1.17300 0.47560 C48 C 0.0421(3) 1.1960(14) 0.3810(7) H95 H 0.02170 1.24500 0.36630 H96 H 0.06000 1.25800 0.39290 C49 C 0.0529(2) 1.1393(8) 0.3235(4) H97 H 0.07710 1.15890 0.31180 H98 H 0.03800 1.15420 0.28200 C50 C 0.04769(17) 0.9923(5) 0.3598(2) H99 H 0.03840 0.93150 0.32530 H100 H 0.06920 0.95960 0.38030 O7 O -0.06842(15) 1.4829(7) 0.2824(3) C51 C -0.08488(9) 1.3254(6) 0.2667(5) H101 H -0.09010 1.28490 0.31260 H102 H -0.10640 1.33050 0.23920 C52 C -0.06364(14) 1.2610(7) 0.2339(3) H103 H -0.07380 1.21820 0.19250 H104 H -0.05190 1.19930 0.26460 C53 C -0.0391(2) 1.3762(11) 0.2118(5) H105 H -0.01770 1.34600 0.18920 H106 H -0.05100 1.43430 0.17920 C54 C -0.03209(11) 1.4350(7) 0.2783(6) H107 H -0.01470 1.50240 0.27520 H108 H -0.02620 1.37500 0.31630 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Si1 C1 1.877 1_555 1_555 Si2 C3 1.973 1_555 1_555 Li1 O1 1.964 1_555 1_555 Li2 O2 1.989 1_555 1_555 Li3 C5 2.321 1_555 1_555 O1 C16 1.526 1_555 1_555 O2 C31 1.312 1_555 1_555 C1 C2 1.592 1_555 1_555 C2 Li1 2.127 1_555 1_555 B1 C1 1.655 1_555 1_555 H1 B1 1.101 1_555 1_555 B2 C1 1.690 1_555 1_555 H2 B2 1.100 1_555 1_555 B3 C1 1.772 1_555 1_555 H3 B3 1.101 1_555 1_555 B4 C1 1.716 1_555 1_555 H4 B4 1.099 1_555 1_555 B5 C2 1.675 1_555 1_555 H5 B5 1.101 1_555 1_555 B6 B1 1.870 1_555 1_555 H6 B6 1.100 1_555 1_555 B7 B2 1.692 1_555 1_555 H7 B7 1.099 1_555 1_555 B8 B3 1.641 1_555 1_555 H8 B8 1.099 1_555 1_555 B9 C2 1.815 1_555 1_555 H9 B9 1.101 1_555 1_555 B10 B5 1.801 1_555 1_555 H10 B10 1.101 1_555 1_555 C3 C4 1.850 1_555 1_555 C4 Li2 2.155 1_555 1_555 B11 C3 1.752 1_555 1_555 H11 B11 1.101 1_555 1_555 B12 C3 1.765 1_555 1_555 H12 B12 1.099 1_555 1_555 B13 C3 1.620 1_555 1_555 H13 B13 1.099 1_555 1_555 B14 C3 1.601 1_555 1_555 H14 B14 1.100 1_555 1_555 B15 C4 1.775 1_555 1_555 H15 B15 1.101 1_555 1_555 B16 B11 1.769 1_555 1_555 H16 B16 1.100 1_555 1_555 B17 B12 1.874 1_555 1_555 H17 B17 1.100 1_555 1_555 B18 B13 1.972 1_555 1_555 H18 B18 1.100 1_555 1_555 B19 C4 1.643 1_555 1_555 H19 B19 1.100 1_555 1_555 B20 B15 1.672 1_555 1_555 H20 B20 1.100 1_555 1_555 C5 Si1 1.889 1_555 1_555 C6 Li1 2.370 1_555 1_555 C7 Li1 2.495 1_555 1_555 C8 Li1 2.462 1_555 1_555 C9 Li1 2.403 1_555 1_555 C10 C6 1.466 1_555 1_555 H21 C10 0.961 1_555 1_555 H22 C10 0.960 1_555 1_555 H23 C10 0.960 1_555 1_555 C11 C7 1.402 1_555 1_555 H24 C11 0.960 1_555 1_555 H25 C11 0.961 1_555 1_555 H26 C11 0.960 1_555 1_555 C12 C8 1.536 1_555 1_555 H27 C12 0.961 1_555 1_555 H28 C12 0.962 1_555 1_555 H29 C12 0.959 1_555 1_555 C13 C9 1.468 1_555 1_555 H30 C13 0.961 1_555 1_555 H31 C13 0.960 1_555 1_555 H32 C13 0.960 1_555 1_555 C14 Si1 1.971 1_555 1_555 H33 C14 0.960 1_555 1_555 H34 C14 0.961 1_555 1_555 H35 C14 0.960 1_555 1_555 C15 Si1 1.883 1_555 1_555 H36 C15 0.959 1_555 1_555 H37 C15 0.960 1_555 1_555 H38 C15 0.960 1_555 1_555 C16 H39 0.971 1_555 1_555 H40 C16 0.971 1_555 1_555 C17 C16 1.467 1_555 1_555 H41 C17 0.971 1_555 1_555 H42 C17 0.971 1_555 1_555 C18 C17 1.155 1_555 1_555 H43 C18 0.971 1_555 1_555 H44 C18 0.970 1_555 1_555 C19 O1 1.523 1_555 1_555 H45 C19 0.970 1_555 1_555 H46 C19 0.969 1_555 1_555 C20 Si2 1.839 1_555 1_555 C21 Li2 2.249 1_555 1_555 C22 Li2 2.325 1_555 1_555 C23 Li2 2.301 1_555 1_555 C24 Li2 2.258 1_555 1_555 C25 C21 1.573 1_555 1_555 H47 C25 0.959 1_555 1_555 H48 C25 0.960 1_555 1_555 H49 C25 0.960 1_555 1_555 C26 C22 1.532 1_555 1_555 H50 C26 0.960 1_555 1_555 H51 C26 0.960 1_555 1_555 H52 C26 0.960 1_555 1_555 C27 C23 1.586 1_555 1_555 H53 C27 0.960 1_555 1_555 H54 C27 0.960 1_555 1_555 H55 C27 0.962 1_555 1_555 C28 C24 1.567 1_555 1_555 H56 C28 0.959 1_555 1_555 H57 C28 0.959 1_555 1_555 H58 C28 0.960 1_555 1_555 C29 Si2 1.868 1_555 1_555 H59 C29 0.961 1_555 1_555 H60 C29 0.959 1_555 1_555 H61 C29 0.960 1_555 1_555 C30 Si2 1.836 1_555 1_555 H62 C30 0.962 1_555 1_555 H63 C30 0.960 1_555 1_555 H64 C30 0.960 1_555 1_555 C31 H65 0.969 1_555 1_555 H66 C31 0.970 1_555 1_555 C32 C31 1.586 1_555 1_555 H67 C32 0.970 1_555 1_555 H68 C32 0.971 1_555 1_555 C33 C32 1.626 1_555 1_555 H69 C33 0.971 1_555 1_555 H70 C33 0.970 1_555 1_555 C34 O2 1.285 1_555 1_555 H71 C34 0.969 1_555 1_555 H72 C34 0.970 1_555 1_555 Li4 O3 1.976 1_555 1_555 O3 C35 1.362 1_555 1_555 C35 H73 0.970 1_555 1_555 H74 C35 0.969 1_555 1_555 C36 C35 1.526 1_555 1_555 H75 C36 0.971 1_555 1_555 H76 C36 0.971 1_555 1_555 C37 C36 1.540 1_555 1_555 C38 O3 1.602 1_555 1_555 O4 Li4 1.939 1_555 1_555 C39 O4 1.278 1_555 1_555 H77 C39 0.971 1_555 1_555 H78 C39 0.970 1_555 1_555 C40 C39 1.375 1_555 1_555 H79 C40 0.969 1_555 1_555 H80 C40 0.971 1_555 1_555 C41 C40 1.388 1_555 1_555 H81 C41 0.969 1_555 1_555 H82 C41 0.969 1_555 1_555 C42 O4 1.558 1_555 1_555 H83 C42 0.970 1_555 1_555 H84 C42 0.970 1_555 1_555 O5 Li4 1.843 1_555 1_555 C43 O5 1.477 1_555 1_555 H85 C43 0.970 1_555 1_555 H86 C43 0.970 1_555 1_555 C44 C43 1.312 1_555 1_555 H87 C44 0.971 1_555 1_555 H88 C44 0.970 1_555 1_555 C45 C44 1.509 1_555 1_555 H89 C45 0.970 1_555 1_555 H90 C45 0.969 1_555 1_555 C46 O5 1.273 1_555 1_555 H91 C46 0.971 1_555 1_555 H92 C46 0.970 1_555 1_555 O6 Li4 1.917 1_555 1_555 C47 O6 1.396 1_555 1_555 H93 C47 0.969 1_555 1_555 H94 C47 0.969 1_555 1_555 C48 C47 1.513 1_555 1_555 H95 C48 0.972 1_555 1_555 H96 C48 0.968 1_555 1_555 C49 C48 1.288 1_555 1_555 H97 C49 0.972 1_555 1_555 H98 C49 0.970 1_555 1_555 C50 O6 1.375 1_555 1_555 H99 C50 0.969 1_555 1_555 H100 C50 0.968 1_555 1_555 O7 C51 1.787 1_555 1_555 C51 H101 0.971 1_555 1_555 H102 C51 0.969 1_555 1_555 C52 C51 1.217 1_555 1_555 H103 C52 0.969 1_555 1_555 H104 C52 0.970 1_555 1_555 C53 C52 1.581 1_555 1_555 H105 C53 0.972 1_555 1_555 H106 C53 0.970 1_555 1_555 C54 O7 1.478 1_555 1_555 H107 C54 0.971 1_555 1_555 H108 C54 0.970 1_555 1_555 Li1 C5 2.214 1_555 1_555 Li2 C20 2.334 1_555 1_555 Li3 C6 2.192 1_555 1_555 Li3 C7 2.290 1_555 1_555 Li3 C8 2.255 1_555 1_555 Li3 C9 2.288 1_555 1_555 Li3 C20 2.361 1_555 1_555 Li3 C21 2.287 1_555 1_555 Li3 C22 2.357 1_555 1_555 Li3 C23 2.394 1_555 1_555 Li3 C24 2.475 1_555 1_555 C2 B1 1.610 1_555 1_555 C2 B4 1.620 1_555 1_555 B1 B2 1.909 1_555 1_555 B1 B5 1.822 1_555 1_555 B2 B3 1.663 1_555 1_555 B2 B6 1.834 1_555 1_555 B3 B4 1.793 1_555 1_555 B3 B7 1.766 1_555 1_555 B4 B8 1.804 1_555 1_555 B4 B9 1.657 1_555 1_555 B5 B6 1.744 1_555 1_555 B5 B9 1.708 1_555 1_555 B6 B7 1.844 1_555 1_555 B6 B10 1.768 1_555 1_555 B7 B8 1.670 1_555 1_555 B7 B10 1.788 1_555 1_555 B8 B9 1.676 1_555 1_555 B8 B10 1.774 1_555 1_555 B9 B10 1.747 1_555 1_555 C4 B11 1.825 1_555 1_555 C4 B14 1.774 1_555 1_555 B11 B12 1.786 1_555 1_555 B11 B15 1.741 1_555 1_555 B12 B13 1.793 1_555 1_555 B12 B16 1.791 1_555 1_555 B13 B14 1.796 1_555 1_555 B13 B17 1.755 1_555 1_555 B14 B18 1.742 1_555 1_555 B14 B19 1.916 1_555 1_555 B15 B16 1.803 1_555 1_555 B15 B19 1.670 1_555 1_555 B16 B17 1.702 1_555 1_555 B16 B20 1.724 1_555 1_555 B17 B18 1.860 1_555 1_555 B17 B20 1.791 1_555 1_555 B18 B19 1.846 1_555 1_555 B18 B20 1.731 1_555 1_555 B19 B20 1.754 1_555 1_555 C5 C6 1.410 1_555 1_555 C5 C9 1.411 1_555 1_555 C6 C7 1.517 1_555 1_555 C7 C8 1.416 1_555 1_555 C8 C9 1.453 1_555 1_555 C18 C19 1.755 1_555 1_555 C20 C21 1.492 1_555 1_555 C20 C24 1.456 1_555 1_555 C21 C22 1.389 1_555 1_555 C22 C23 1.459 1_555 1_555 C23 C24 1.282 1_555 1_555 C33 C34 1.395 1_555 1_555 C37 C38 1.542 1_555 1_555 C41 C42 1.427 1_555 1_555 C45 C46 1.650 1_555 1_555 C49 C50 1.690 1_555 1_555 C53 C54 1.403 1_555 1_555 #END data_CSD_CIF_QUGCAY _audit_creation_date 2015-06-08 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD QUGCAY _database_code_depnum_ccdc_archive 'CCDC 1048216' _chemical_formula_sum 'C16 H14 Co1 N8 Na1 O1' _chemical_formula_moiety ; (C6 H2 Co1 N6 Na1 O1 2-)n,2(C5 H6 N1 1+) ; _journal_coden_Cambridge 179 _journal_volume 54 _journal_year 2015 _journal_page_first 6206 _journal_name_full 'Angew.Chem.,Int.Ed. ' loop_ _publ_author_name "Chao Shi" "Xi Zhang" "Ying Cai" "Ye-Feng Yao" "Wen Zhang" _chemical_name_systematic ; catena-[bis(pyridinium) tetrakis(cyano)-dicyano-aqua-cobalt-sodium] ; _cell_volume 939.079 _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.472 _exptl_crystal_description 'block' _diffrn_ambient_temperature 133 _refine_special_details ; C4,C4',C5,C5',C6',N6 disordered by symmetry over two configurations with occupancy 0.50. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_gt 0.0675 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P m m n' _symmetry_Int_Tables_number 59 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2-y,z 3 -x,1/2+y,-z 4 1/2+x,-y,-z 5 -x,-y,-z 6 -1/2+x,-1/2+y,-z 7 x,-1/2-y,z 8 -1/2-x,y,z _cell_length_a 11.127(8) _cell_length_b 8.763(6) _cell_length_c 9.631(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Co 1.26 N 0.68 Na 1.66 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Co1 Co 0.75000 0.75000 0.65408(11) Na1 Na 0.75000 0.25000 0.3133(3) N1 N 0.75000 0.4938(6) 0.4378(5) C1 C 0.75000 0.5947(7) 0.5165(6) C2 C 0.5797(5) 0.75000 0.6604(6) N2 N 0.4766(4) 0.75000 0.6715(5) O1 O 0.75000 0.25000 0.0707(7) N3 N 0.75000 0.9944(7) 0.8796(6) C3 C 0.75000 0.9038(7) 0.7937(6) H1 H 0.75040 0.16920 0.00460 C4? C 0.5303(14) 0.8844(16) 0.187(2) C5? C 0.471(3) 0.830(3) 0.308(3) C6? C 0.5834(10) 0.7762(18) 0.1000(12) C7? C 0.5794(13) 0.8773(18) 0.1356(14) N4? N 0.5223(10) 0.9199(12) 0.2526(13) C8? C 0.470(4) 0.823(4) 0.339(4) H1A H 0.74960 0.33080 0.00460 N1A N 0.75000 0.0062(6) 0.4378(5) C1A C 0.75000 -0.0947(7) 0.5165(6) C2A C 0.9203(5) 0.75000 0.6604(6) N2A N 1.0234(4) 0.75000 0.6715(5) N3A N 0.75000 0.5056(7) 0.8796(6) C3A C 0.75000 0.5962(7) 0.7937(6) Co1* Co 0.75000 -0.25000 0.65408(11) Na1B Na 0.25000 0.75000 0.6867(3) Na1B* Na 1.25000 0.75000 0.6867(3) C1A* C 0.75000 0.9053(7) 0.5165(6) N2B N 0.5234(4) 0.25000 0.3285(5) N2C N 0.9766(4) 0.25000 0.3285(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Co1 C1 1.899 1_555 1_555 Na1 N1 2.450 1_555 1_555 N1 C1 1.165 1_555 1_555 C2 Co1 1.896 1_555 1_555 N2 C2 1.152 1_555 1_555 O1 Na1 2.336 1_555 1_555 N3 C3 1.147 1_555 1_555 C3 Co1 1.904 1_555 1_555 H1 O1 0.952 1_555 1_555 H1A O1 0.952 1_555 1_555 N1A Na1 2.450 1_555 1_555 C1A N1A 1.165 1_555 1_555 C2A Co1 1.896 1_555 1_555 N2A C2A 1.152 1_555 1_555 N3A C3A 1.147 1_555 1_555 C3A Co1 1.904 1_555 1_555 Co1* C1A 1.899 1_555 1_555 Na1B N2 2.526 1_555 1_555 Na1B* N2A 2.526 1_555 1_555 C1A* Co1 1.899 1_555 1_555 N2B Na1 2.526 1_555 1_555 N2C Na1 2.526 1_555 1_555 #END data_CSD_CIF_REGCAH _audit_creation_date 2001-11-22 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD REGCAH _chemical_formula_sum 'C16 H32 K1 Na1 O8' _chemical_formula_moiety ; C16 H32 K1 O8 1+,Na1 1- ; _journal_coden_Cambridge 211 _journal_volume 46 _journal_year 1998 _journal_page_first 13 _journal_name_full 'J.Coord.Chem. ' loop_ _publ_author_name "R.H.Huang" "S.Z.Huang" "J.L.Dye" _chemical_name_systematic ; bis(12-Crown-4)-potassium sodide ; _cell_volume 2589.443 _exptl_special_details ; air- and moisture-sensitive ; _exptl_crystal_preparation 'dimethyl ether' _diffrn_ambient_temperature 213 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.04 _refine_ls_wR_factor_gt 0.04 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,-1/2-y,-1/2+z _cell_length_a 11.0527(25) _cell_length_b 15.3311(34) _cell_length_c 15.3115(36) _cell_angle_alpha 90 _cell_angle_beta 93.59(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 K 1.72 Na 0.97 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z K1 K -0.00375(5) 0.24205(4) 0.51658(4) Na1 Na 0.5036(1) 0.5392(1) 0.25341(9) O1 O -0.1239(2) 0.0844(1) 0.5275(1) O2 O -0.0829(2) 0.1593(1) 0.3634(1) O3 O -0.1907(2) 0.3163(1) 0.4169(1) O4 O -0.2337(2) 0.2407(1) 0.5799(1) O5 O 0.2267(2) 0.1816(1) 0.5590(1) O6 O 0.1906(2) 0.3262(1) 0.4465(1) O7 O 0.0552(2) 0.4083(1) 0.5746(1) O8 O 0.0907(2) 0.2623(1) 0.6861(1) C1 C -0.1727(3) 0.0452(2) 0.4495(2) C2 C -0.0927(3) 0.0666(2) 0.3796(2) C3 C -0.1823(3) 0.1958(2) 0.3141(2) C4 C -0.1807(3) 0.2909(2) 0.3269(2) C5 C -0.3096(3) 0.3120(2) 0.4447(2) C6 C -0.3014(3) 0.3140(2) 0.5410(2) C7 C -0.2981(3) 0.1618(2) 0.5804(2) C8 C -0.2098(3) 0.0898(2) 0.5956(2) C9 C 0.3064(3) 0.2031(2) 0.4906(2) C10 C 0.3092(3) 0.2996(2) 0.4729(2) C11 C 0.1713(3) 0.4192(2) 0.4516(2) C12 C 0.1577(3) 0.4494(2) 0.5435(2) C13 C 0.0504(3) 0.4119(2) 0.6683(2) C14 C 0.1293(3) 0.3450(2) 0.7146(2) C15 C 0.1797(3) 0.1946(2) 0.7054(2) C16 C 0.2790(3) 0.1961(2) 0.6441(2) H1 H -0.253(3) 0.066(2) 0.435(2) H2 H -0.176(3) -0.016(2) 0.457(2) H3 H -0.014(3) 0.043(2) 0.393(2) H4 H -0.126(3) 0.040(2) 0.327(2) H5 H -0.256(2) 0.173(2) 0.334(2) H6 H -0.178(3) 0.182(2) 0.254(2) H7 H -0.105(3) 0.312(2) 0.308(2) H8 H -0.245(3) 0.317(2) 0.292(2) H9 H -0.347(3) 0.259(2) 0.425(2) H10 H -0.355(3) 0.360(2) 0.422(2) H11 H -0.261(3) 0.366(2) 0.560(2) H12 H -0.381(2) 0.315(2) 0.561(2) H13 H -0.342(3) 0.154(2) 0.526(2) H14 H -0.353(3) 0.162(2) 0.626(2) H15 H -0.167(2) 0.098(2) 0.651(2) H16 H -0.254(3) 0.036(2) 0.597(2) H17 H 0.279(3) 0.174(2) 0.439(2) H18 H 0.386(3) 0.184(2) 0.508(2) H19 H 0.337(2) 0.330(2) 0.525(2) H20 H 0.362(3) 0.311(2) 0.428(2) H21 H 0.099(3) 0.434(2) 0.417(2) H22 H 0.238(2) 0.449(2) 0.429(2) H23 H 0.228(2) 0.433(2) 0.578(2) H24 H 0.148(3) 0.511(2) 0.545(2) H25 H -0.030(2) 0.402(2) 0.683(2) H26 H 0.076(3) 0.468(2) 0.688(2) H27 H 0.211(2) 0.354(2) 0.701(2) H28 H 0.124(3) 0.350(2) 0.776(2) H29 H 0.139(3) 0.140(2) 0.699(2) H30 H 0.213(3) 0.200(2) 0.764(2) H31 H 0.317(3) 0.251(2) 0.648(2) H32 H 0.336(3) 0.152(2) 0.659(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 K1 O1 2.768 1_555 1_555 O1 C1 1.413 1_555 1_555 O2 K1 2.760 1_555 1_555 O3 K1 2.739 1_555 1_555 O4 K1 2.776 1_555 1_555 O5 K1 2.750 1_555 1_555 O6 K1 2.778 1_555 1_555 O7 K1 2.764 1_555 1_555 O8 K1 2.754 1_555 1_555 C1 C2 1.467 1_555 1_555 C2 O2 1.448 1_555 1_555 C3 O2 1.409 1_555 1_555 C4 O3 1.443 1_555 1_555 C5 O3 1.408 1_555 1_555 C6 O4 1.457 1_555 1_555 C7 O4 1.404 1_555 1_555 C8 O1 1.456 1_555 1_555 C9 O5 1.448 1_555 1_555 C10 O6 1.408 1_555 1_555 C11 O6 1.444 1_555 1_555 C12 O7 1.405 1_555 1_555 C13 O7 1.440 1_555 1_555 C14 O8 1.399 1_555 1_555 C15 O8 1.448 1_555 1_555 C16 O5 1.410 1_555 1_555 H1 C1 0.956 1_555 1_555 H2 C1 0.946 1_555 1_555 H3 C2 0.953 1_555 1_555 H4 C2 0.956 1_555 1_555 H5 C3 0.954 1_555 1_555 H6 C3 0.948 1_555 1_555 H7 C4 0.959 1_555 1_555 H8 C4 0.950 1_555 1_555 H9 C5 0.952 1_555 1_555 H10 C5 0.945 1_555 1_555 H11 C6 0.950 1_555 1_555 H12 C6 0.950 1_555 1_555 H13 C7 0.945 1_555 1_555 H14 C7 0.953 1_555 1_555 H15 C8 0.953 1_555 1_555 H16 C8 0.960 1_555 1_555 H17 C9 0.941 1_555 1_555 H18 C9 0.949 1_555 1_555 H19 C10 0.958 1_555 1_555 H20 C10 0.946 1_555 1_555 H21 C11 0.958 1_555 1_555 H22 C11 0.951 1_555 1_555 H23 C12 0.946 1_555 1_555 H24 C12 0.951 1_555 1_555 H25 C13 0.943 1_555 1_555 H26 C13 0.949 1_555 1_555 H27 C14 0.949 1_555 1_555 H28 C14 0.949 1_555 1_555 H29 C15 0.952 1_555 1_555 H30 C15 0.952 1_555 1_555 H31 C16 0.941 1_555 1_555 H32 C16 0.942 1_555 1_555 C3 C4 1.471 1_555 1_555 C5 C6 1.472 1_555 1_555 C7 C8 1.482 1_555 1_555 C9 C10 1.505 1_555 1_555 C11 C12 1.498 1_555 1_555 C13 C14 1.496 1_555 1_555 C15 C16 1.488 1_555 1_555 #END data_CSD_CIF_REGCEL _audit_creation_date 2001-11-22 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD REGCEL _chemical_formula_sum 'C16 H32 N2 Na2 O5' _chemical_formula_moiety ; C16 H32 N2 Na1 O5 1+,Na1 1- ; _journal_coden_Cambridge 211 _journal_volume 46 _journal_year 1998 _journal_page_first 13 _journal_name_full 'J.Coord.Chem. ' loop_ _publ_author_name "R.H.Huang" "S.Z.Huang" "J.L.Dye" _chemical_name_systematic ; (4,7,13,16,21-Pentaoxa-1,10-diazabicyclo(8.8.5)tricosane)-sodium sodide ; _chemical_name_common ; (2.2.1-Cryptand)-sodium sodide ; _cell_volume 2533.197 _exptl_special_details ; air-sensitive and moisture-sensitive ; _exptl_crystal_preparation 'dimethyl ether/diethyl ether' _diffrn_ambient_temperature 210 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.03 _refine_ls_wR_factor_gt 0.03 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,-1/2-y,-1/2+z _cell_length_a 8.4976(36) _cell_length_b 13.0383(59) _cell_length_c 22.9368(93) _cell_angle_alpha 90 _cell_angle_beta 94.567(34) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 N 0.68 Na 1.57 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 0.4527(1) 0.72519(7) 0.41419(4) Na2 Na 0.0791(2) 0.7282(1) 0.17797(5) O1 O 0.6691(2) 0.7029(1) 0.34835(6) O2 O 0.4372(2) 0.5578(1) 0.36617(6) O3 O 0.4822(2) 0.6567(1) 0.51493(6) O4 O 0.5746(2) 0.8518(1) 0.48490(7) O5 O 0.2218(2) 0.8145(1) 0.37927(7) N1 N 0.5230(2) 0.8987(2) 0.36338(8) N2 N 0.2010(2) 0.6244(2) 0.43769(9) C1 C 0.6471(3) 0.8787(2) 0.3239(1) C2 C 0.6380(3) 0.7714(2) 0.2999(1) C3 C 0.6816(3) 0.5979(2) 0.3308(1) C4 C 0.5247(3) 0.5489(2) 0.3162(1) C5 C 0.2803(3) 0.5185(2) 0.3566(1) C6 C 0.2088(3) 0.5195(2) 0.4144(1) C7 C 0.2002(3) 0.6247(2) 0.5015(1) C8 C 0.3554(3) 0.5940(2) 0.5324(1) C9 C 0.5363(4) 0.7300(2) 0.5578(1) C10 C 0.6543(3) 0.7969(2) 0.5323(1) C11 C 0.6732(3) 0.9229(2) 0.4582(1) C12 C 0.5759(3) 0.9732(2) 0.4085(1) C13 C 0.3765(3) 0.9321(2) 0.3303(1) C14 C 0.2339(3) 0.9200(2) 0.3641(1) C15 C 0.0867(3) 0.7935(2) 0.4100(1) C16 C 0.0634(3) 0.6794(3) 0.4101(1) H1 H 0.746(2) 0.887(2) 0.3452(9) H2 H 0.636(2) 0.926(2) 0.2927(9) H3 H 0.535(2) 0.760(2) 0.2822(9) H4 H 0.713(3) 0.762(2) 0.2718(9) H5 H 0.735(3) 0.561(2) 0.3621(9) H6 H 0.742(2) 0.596(2) 0.2977(8) H7 H 0.471(2) 0.583(2) 0.2839(9) H8 H 0.538(2) 0.479(2) 0.3074(9) H9 H 0.285(3) 0.451(2) 0.3426(9) H10 H 0.220(2) 0.561(2) 0.3299(9) H11 H 0.105(3) 0.492(2) 0.409(1) H12 H 0.272(2) 0.479(2) 0.4411(9) H13 H 0.120(3) 0.578(2) 0.5122(9) H14 H 0.176(2) 0.692(2) 0.5135(9) H15 H 0.349(3) 0.601(2) 0.573(1) H16 H 0.376(2) 0.525(2) 0.5232(9) H17 H 0.581(3) 0.696(2) 0.591(1) H18 H 0.450(3) 0.771(2) 0.568(1) H19 H 0.699(3) 0.844(2) 0.561(1) H20 H 0.736(3) 0.756(2) 0.5182(9) H21 H 0.761(3) 0.888(2) 0.444(1) H22 H 0.710(3) 0.973(2) 0.4856(9) H23 H 0.487(2) 1.005(2) 0.4232(8) H24 H 0.639(3) 1.023(2) 0.391(1) H25 H 0.361(3) 0.890(2) 0.2968(9) H26 H 0.386(3) 1.001(2) 0.320(1) H27 H 0.249(3) 0.962(2) 0.399(1) H28 H 0.142(3) 0.942(2) 0.342(1) H29 H -0.002(3) 0.825(2) 0.391(1) H30 H 0.101(3) 0.818(2) 0.449(1) H31 H -0.028(3) 0.663(2) 0.430(1) H32 H 0.046(2) 0.657(2) 0.3707(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Na1 O1 2.488 1_555 1_555 O1 C2 1.434 1_555 1_555 O2 Na1 2.443 1_555 1_555 O3 Na1 2.471 1_555 1_555 O4 Na1 2.482 1_555 1_555 O5 Na1 2.366 1_555 1_555 N1 Na1 2.635 1_555 1_555 N2 Na1 2.603 1_555 1_555 C1 N1 1.467 1_555 1_555 C2 C1 1.503 1_555 1_555 C3 O1 1.433 1_555 1_555 C4 O2 1.420 1_555 1_555 C5 O2 1.429 1_555 1_555 C6 N2 1.472 1_555 1_555 C7 N2 1.464 1_555 1_555 C8 O3 1.435 1_555 1_555 C9 O3 1.421 1_555 1_555 C10 O4 1.427 1_555 1_555 C11 O4 1.421 1_555 1_555 C12 N1 1.464 1_555 1_555 C13 N1 1.471 1_555 1_555 C14 O5 1.425 1_555 1_555 C15 O5 1.421 1_555 1_555 C16 N2 1.471 1_555 1_555 H1 C1 0.944 1_555 1_555 H2 C1 0.944 1_555 1_555 H3 C2 0.947 1_555 1_555 H4 C2 0.950 1_555 1_555 H5 C3 0.949 1_555 1_555 H6 C3 0.950 1_555 1_555 H7 C4 0.949 1_555 1_555 H8 C4 0.942 1_555 1_555 H9 C5 0.939 1_555 1_555 H10 C5 0.946 1_555 1_555 H11 C6 0.951 1_555 1_555 H12 C6 0.943 1_555 1_555 H13 C7 0.960 1_555 1_555 H14 C7 0.947 1_555 1_555 H15 C8 0.942 1_555 1_555 H16 C8 0.944 1_555 1_555 H17 C9 0.935 1_555 1_555 H18 C9 0.952 1_555 1_555 H19 C10 0.957 1_555 1_555 H20 C10 0.952 1_555 1_555 H21 C11 0.953 1_555 1_555 H22 C11 0.942 1_555 1_555 H23 C12 0.947 1_555 1_555 H24 C12 0.951 1_555 1_555 H25 C13 0.945 1_555 1_555 H26 C13 0.934 1_555 1_555 H27 C14 0.970 1_555 1_555 H28 C14 0.941 1_555 1_555 H29 C15 0.935 1_555 1_555 H30 C15 0.949 1_555 1_555 H31 C16 0.956 1_555 1_555 H32 C16 0.950 1_555 1_555 C3 C4 1.492 1_555 1_555 C5 C6 1.502 1_555 1_555 C7 C8 1.501 1_555 1_555 C9 C10 1.484 1_555 1_555 C11 C12 1.504 1_555 1_555 C13 C14 1.498 1_555 1_555 C15 C16 1.501 1_555 1_555 #END data_CSD_CIF_REGCIP _audit_creation_date 2001-11-22 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD REGCIP _chemical_formula_sum 'C13 H29 N1 Na1 O6 Rb1' _chemical_formula_moiety ; C13 H29 N1 O6 Rb1 1+,Na1 1- ; _journal_coden_Cambridge 211 _journal_volume 46 _journal_year 1998 _journal_page_first 13 _journal_name_full 'J.Coord.Chem. ' loop_ _publ_author_name "R.H.Huang" "S.Z.Huang" "J.L.Dye" _chemical_name_systematic ; (18-Crown-6)-methylamine-rubidium sodide ; _cell_volume 2308.602 _exptl_crystal_colour 'red-bronze' _exptl_special_details ; air-sensitive and moisture-sensitive ; _exptl_crystal_preparation 'methylamine/diethyl ether' _diffrn_ambient_temperature 200 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.037 _refine_ls_wR_factor_gt 0.037 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,1/2+y,1/2-z _cell_length_a 8.3919(61) _cell_length_b 12.4835(84) _cell_length_c 22.037(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 N 0.68 Na 0.97 O 0.68 Rb 1.97 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Rb1 Rb 0.2527(1) 0.41238(5) 0.60542(3) Na1 Na 0.3309(5) 0.7628(3) 0.6570(2) O1 O 0.5062(6) 0.2798(4) 0.5578(2) O2 O 0.4055(6) 0.4522(3) 0.4825(2) O3 O 0.1360(6) 0.5653(4) 0.5195(2) O4 O -0.0976(6) 0.4667(4) 0.5881(2) O5 O 0.0016(6) 0.2931(4) 0.6601(2) O6 O 0.2755(6) 0.1765(4) 0.6271(2) N1 N 0.366(1) 0.4412(6) 0.7335(3) C1 C 0.5760(9) 0.3054(5) 0.5005(3) C2 C 0.5676(9) 0.4243(6) 0.4910(3) C3 C 0.391(1) 0.5657(6) 0.4755(3) C4 C 0.2187(9) 0.5931(6) 0.4651(3) C5 C -0.024(1) 0.6014(6) 0.5190(4) C6 C -0.096(1) 0.5788(6) 0.5786(4) C7 C -0.171(1) 0.4357(8) 0.6431(4) C8 C -0.1619(9) 0.3204(8) 0.6515(4) C9 C 0.023(1) 0.1839(7) 0.6754(3) C10 C 0.195(1) 0.1598(6) 0.6838(3) C11 C 0.436(1) 0.1497(6) 0.6306(3) C12 C 0.5124(9) 0.1702(5) 0.5700(3) C13 C 0.235(1) 0.4473(8) 0.7724(4) H1 H 0.68520 0.28090 0.49950 H2 H 0.52170 0.26830 0.46700 H3 H 0.628(7) 0.444(4) 0.456(2) H4 H 0.610(8) 0.460(5) 0.526(3) H5 H 0.43(1) 0.601(7) 0.512(4) H6 H 0.453(8) 0.588(5) 0.442(3) H7 H 0.17840 0.55140 0.43220 H8 H 0.205(9) 0.667(6) 0.456(3) H9 H -0.026(7) 0.676(4) 0.511(2) H10 H -0.083(9) 0.565(5) 0.488(3) H11 H -0.20180 0.60680 0.57950 H12 H -0.034(8) 0.613(5) 0.609(3) H13 H -0.116(8) 0.468(5) 0.676(3) H14 H -0.28(1) 0.456(7) 0.643(4) H15 H -0.20510 0.28320 0.61630 H16 H -0.219(7) 0.299(5) 0.686(3) H17 H -0.034(9) 0.169(6) 0.711(3) H18 H -0.011(9) 0.142(6) 0.643(3) H19 H 0.211(6) 0.089(4) 0.697(2) H20 H 0.236(7) 0.208(4) 0.713(2) H21 H 0.44660 0.07620 0.64110 H22 H 0.485(6) 0.194(4) 0.658(2) H23 H 0.454(7) 0.132(4) 0.540(2) H24 H 0.620(8) 0.149(5) 0.569(2) H25 H 0.429(9) 0.504(6) 0.736(3) H26 H 0.42660 0.38120 0.74510 H27 H 0.26(1) 0.456(7) 0.814(4) H28 H 0.16050 0.50420 0.76180 H29 H 0.16760 0.38100 0.77050 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rb1 O1 2.892 1_555 1_555 O1 C1 1.428 1_555 1_555 O2 Rb1 3.038 1_555 1_555 O3 Rb1 2.862 1_555 1_555 O4 Rb1 3.041 1_555 1_555 O5 Rb1 2.848 1_555 1_555 O6 Rb1 2.989 1_555 1_555 N1 Rb1 3.000 1_555 1_555 C1 C2 1.501 1_555 1_555 C2 O2 1.417 1_555 1_555 C3 O2 1.430 1_555 1_555 C4 O3 1.428 1_555 1_555 C5 O3 1.416 1_555 1_555 C6 O4 1.415 1_555 1_555 C7 O4 1.414 1_555 1_555 C8 O5 1.426 1_555 1_555 C9 O5 1.416 1_555 1_555 C10 O6 1.436 1_555 1_555 C11 O6 1.390 1_555 1_555 C12 O1 1.395 1_555 1_555 C13 N1 1.396 1_555 1_555 H1 C1 0.966 1_555 1_555 H2 C1 0.983 1_555 1_555 H3 C2 0.955 1_555 1_555 H4 C2 0.959 1_555 1_555 H5 C3 0.974 1_555 1_555 H6 C3 0.945 1_555 1_555 H7 C4 0.954 1_555 1_555 H8 C4 0.951 1_555 1_555 H9 C5 0.948 1_555 1_555 H10 C5 0.958 1_555 1_555 H11 C6 0.954 1_555 1_555 H12 C6 0.950 1_555 1_555 H13 C7 0.949 1_555 1_555 H14 C7 0.949 1_555 1_555 H15 C8 0.974 1_555 1_555 H16 C8 0.938 1_555 1_555 H17 C9 0.937 1_555 1_555 H18 C9 0.930 1_555 1_555 H19 C10 0.940 1_555 1_555 H20 C10 0.946 1_555 1_555 H21 C11 0.950 1_555 1_555 H22 C11 0.916 1_555 1_555 H23 C12 0.951 1_555 1_555 H24 C12 0.941 1_555 1_555 H25 N1 0.947 1_555 1_555 H26 N1 0.941 1_555 1_555 H27 C13 0.947 1_555 1_555 H28 C13 0.975 1_555 1_555 H29 C13 1.003 1_555 1_555 C3 C4 1.503 1_555 1_555 C5 C6 1.473 1_555 1_555 C7 C8 1.453 1_555 1_555 C9 C10 1.486 1_555 1_555 C11 C12 1.503 1_555 1_555 #END data_CSD_CIF_REGDEM _audit_creation_date 2001-11-22 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD REGDEM _chemical_formula_sum 'C50 H106 K1 N2 Na1 O24' _chemical_formula_moiety ; C14 H34 K1 N2 O6 1+,Na1 1-,3(C12 H24 O6) ; _journal_coden_Cambridge 211 _journal_volume 46 _journal_year 1998 _journal_page_first 13 _journal_name_full 'J.Coord.Chem. ' loop_ _publ_author_name "R.H.Huang" "S.Z.Huang" "J.L.Dye" _chemical_name_systematic ; (18-Crown-6)-bis(methylamine)-potassium sodide tris(18-crown-6) ; _cell_volume 5018.772 _exptl_special_details ; air- and moisture-sensitive ; _exptl_crystal_preparation 'methylamine/diethyl ether/dimethyl ether' _diffrn_ambient_temperature 180 _refine_special_details ; The methylamine ligands are crystallographically disordered about a three-fold axis. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.054 _refine_ls_wR_factor_gt 0.054 _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R -3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 1/3+x,2/3+y,2/3+z 5 1/3-y,2/3+x-y,2/3+z 6 1/3-x+y,2/3-x,2/3+z 7 2/3+x,1/3+y,1/3+z 8 2/3-y,1/3+x-y,1/3+z 9 2/3-x+y,1/3-x,1/3+z 10 -x,-y,-z 11 y,-x+y,-z 12 x-y,x,-z 13 -1/3-x,-2/3-y,-2/3-z 14 -1/3+y,-2/3-x+y,-2/3-z 15 -1/3+x-y,-2/3+x,-2/3-z 16 -2/3-x,-1/3-y,-1/3-z 17 -2/3+y,-1/3-x+y,-1/3-z 18 -2/3+x-y,-1/3+x,-1/3-z _cell_length_a 18.4033(42) _cell_length_b 18.4033(42) _cell_length_c 17.111(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 K 1.80 N 0.68 Na 0.97 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z K1 K 0.00000 0.00000 0.50000 Na1 Na 0.00000 0.00000 0.00000 O1 O -0.0194(1) 0.1403(1) 0.5123(1) O2 O 0.0320(2) 0.4052(2) 0.3992(2) O3 O 0.2454(2) 0.4505(2) 0.4112(1) O4 O 0.3444(2) 0.3751(2) 0.4078(1) N1 N 0.0520(7) 0.0238(7) 0.3398(6) C1 C 0.0452(2) 0.2120(2) 0.4732(2) C2 C -0.1002(2) 0.1285(2) 0.4946(3) C3 C 0.1103(2) 0.4162(2) 0.3717(2) C4 C 0.1709(3) 0.4475(3) 0.4393(2) C5 C 0.3061(3) 0.4654(3) 0.4709(2) C6 C 0.3764(3) 0.4585(3) 0.4347(2) C7 C 0.4024(3) 0.3659(3) 0.3605(3) C8 C -0.0277(3) 0.3891(3) 0.3391(3) C9 C 0.002(2) 0.030(1) 0.301(1) H1 H 0.044(2) 0.199(2) 0.407(2) H2 H 0.037(2) 0.265(2) 0.481(2) H3 H -0.107(3) 0.129(3) 0.434(2) H4 H -0.103(3) 0.173(3) 0.520(2) H5 H 0.103(2) 0.360(2) 0.350(2) H6 H 0.135(2) 0.451(2) 0.318(2) H7 H 0.146(2) 0.412(2) 0.487(2) H8 H 0.175(2) 0.496(2) 0.462(2) H9 H 0.324(2) 0.523(2) 0.497(2) H10 H 0.284(2) 0.430(2) 0.516(2) H11 H 0.392(3) 0.489(3) 0.380(3) H12 H 0.425(3) 0.469(3) 0.477(2) H13 H 0.451(3) 0.377(3) 0.400(2) H14 H 0.422(2) 0.410(2) 0.316(2) H15 H -0.079(3) 0.392(2) 0.372(2) H16 H -0.001(2) 0.428(2) 0.294(2) H17 H 0.10750 0.07190 0.33560 H18 H 0.05190 -0.02370 0.32040 H19 H 0.08020 -0.00500 0.32790 H20 H 0.01820 0.04560 0.25310 H21 H 0.01040 -0.04020 0.31280 C2J C 0.1285(2) 0.2287(2) 0.5054(3) O1J O 0.1403(1) 0.1597(1) 0.4877(1) O1A O -0.1403(1) -0.1597(1) 0.5123(1) C1A C -0.2120(2) -0.1668(2) 0.4732(2) C2K C -0.2287(2) -0.1002(2) 0.5054(3) O1K O -0.1597(1) -0.0194(1) 0.4877(1) O1B O 0.1597(1) 0.0194(1) 0.5123(1) C1B C 0.1668(2) -0.0452(2) 0.4732(2) C2I C 0.1002(2) -0.1285(2) 0.5054(3) O1I O 0.0194(1) -0.1403(1) 0.4877(1) N1A N -0.0238(7) 0.0282(7) 0.3398(6) N1B N -0.0282(7) -0.0520(7) 0.3398(6) C9A C -0.030(2) -0.028(1) 0.301(1) C9B C 0.028(2) -0.002(1) 0.301(1) H18B H -0.07560 -0.05190 0.32040 H17B H -0.03560 -0.10750 0.33560 H19B H -0.08520 -0.08020 0.32790 H20A H -0.04560 -0.02740 0.25310 H20B H 0.02740 -0.01820 0.25310 H21A H 0.04020 0.05060 0.31280 H17A H -0.07190 0.03560 0.33560 H18A H 0.02370 0.07560 0.32040 H19A H 0.00500 0.08520 0.32790 H21B H -0.05060 -0.01040 0.31280 N1I N -0.0520(7) -0.0238(7) 0.6602(6) N1J N 0.0238(7) -0.0282(7) 0.6602(6) N1K N 0.0282(7) 0.0520(7) 0.6602(6) C9I C -0.002(2) -0.030(1) 0.699(1) C9J C 0.030(2) 0.028(1) 0.699(1) C9K C -0.028(2) 0.002(1) 0.699(1) H18K H 0.07560 0.05190 0.67960 H17K H 0.03560 0.10750 0.66440 H19K H 0.08520 0.08020 0.67210 H20J H 0.04560 0.02740 0.74690 H18I H -0.05190 0.02370 0.67960 H17I H -0.10750 -0.07190 0.66440 H19I H -0.08020 0.00500 0.67210 H20K H -0.02740 0.01820 0.74690 H21I H -0.01040 0.04020 0.68720 H21J H -0.04020 -0.05060 0.68720 H17J H 0.07190 -0.03560 0.66440 H18J H -0.02370 -0.07560 0.67960 H19J H -0.00500 -0.08520 0.67210 H21K H 0.05060 0.01040 0.68720 H20I H -0.01820 -0.04560 0.74690 C1I C -0.0452(2) -0.2120(2) 0.5268(2) C2A C -0.1285(2) -0.2287(2) 0.4946(3) H3A H -0.129(3) -0.236(3) 0.434(2) H4A H -0.173(3) -0.276(3) 0.520(2) H1I H -0.044(2) -0.199(2) 0.593(2) H2I H -0.037(2) -0.265(2) 0.519(2) H3I H 0.107(3) -0.129(3) 0.566(2) H4I H 0.103(3) -0.173(3) 0.480(2) H1B H 0.155(2) -0.044(2) 0.407(2) H2B H 0.228(2) -0.037(2) 0.481(2) C2B C 0.2287(2) 0.1002(2) 0.4946(3) C1J C 0.2120(2) 0.1668(2) 0.5268(2) H1J H 0.199(2) 0.155(2) 0.593(2) H2J H 0.265(2) 0.228(2) 0.519(2) H3B H 0.236(3) 0.107(3) 0.434(2) H4B H 0.276(3) 0.103(3) 0.520(2) C1K C -0.1668(2) 0.0452(2) 0.5268(2) H1K H -0.155(2) 0.044(2) 0.593(2) H2K H -0.228(2) 0.037(2) 0.519(2) H3K H -0.236(3) -0.107(3) 0.566(2) H4K H -0.276(3) -0.103(3) 0.480(2) H1A H -0.199(2) -0.155(2) 0.407(2) H2A H -0.265(2) -0.228(2) 0.481(2) H3J H 0.129(3) 0.236(3) 0.566(2) H4J H 0.173(3) 0.276(3) 0.480(2) C8O C 0.361033(300) 0.277567(300) 0.327567(300) O2O O 0.301333(200) 0.261467(200) 0.267467(200) C3O C 0.223033(200) 0.250467(200) 0.294967(200) C4O C 0.162433(300) 0.219167(300) 0.227367(200) O3O O 0.087933(200) 0.216167(200) 0.255467(100) C5O C 0.027233(300) 0.201267(300) 0.195767(200) C6O C -0.043067(300) 0.208167(300) 0.231967(200) O4O O -0.011067(200) 0.291567(200) 0.258867(100) C7O C -0.069067(300) 0.300767(300) 0.306167(300) H13O H -0.117667(3000) 0.289667(3000) 0.266667(2000) H14O H -0.088667(2000) 0.256667(2000) 0.350667(2000) H11O H -0.058667(3000) 0.177667(3000) 0.286667(3000) H12O H -0.091667(3000) 0.197667(3000) 0.189667(2000) H9O H 0.009333(2000) 0.143667(2000) 0.169667(2000) H10O H 0.049333(2000) 0.236667(2000) 0.150667(2000) H7O H 0.187333(2000) 0.254667(2000) 0.179667(2000) H8O H 0.158333(2000) 0.170667(2000) 0.204667(2000) H5O H 0.230333(2000) 0.306667(2000) 0.316667(2000) H6O H 0.198333(2000) 0.215667(2000) 0.348667(2000) H15O H 0.412333(3000) 0.274667(2000) 0.294667(2000) H16O H 0.334333(2000) 0.238667(2000) 0.372667(2000) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 K1 O1 2.786 1_555 1_555 O1 C1 1.426 1_555 1_555 O2 C3 1.431 1_555 1_555 O3 C4 1.428 1_555 1_555 O4 C6 1.418 1_555 1_555 N1 K1 2.864 1_555 1_555 C1 H1 1.156 1_555 1_555 C2 O1 1.424 1_555 1_555 C3 C4 1.507 1_555 1_555 C4 H7 1.002 1_555 1_555 C5 O3 1.435 1_555 1_555 C6 C5 1.496 1_555 1_555 C7 O4 1.416 1_555 1_555 C8 O2 1.424 1_555 1_555 C9 N1 1.186 1_555 1_555 H2 C1 1.067 1_555 1_555 H3 C2 1.045 1_555 1_555 H4 C2 0.951 1_555 1_555 H5 C3 1.042 1_555 1_555 H6 C3 1.082 1_555 1_555 H8 C4 0.941 1_555 1_555 H9 C5 1.040 1_555 1_555 H10 C5 0.959 1_555 1_555 H11 C6 1.055 1_555 1_555 H12 C6 1.090 1_555 1_555 H13 C7 1.056 1_555 1_555 H14 C7 1.037 1_555 1_555 H15 C8 1.123 1_555 1_555 H16 C8 0.999 1_555 1_555 H17 N1 0.963 1_555 1_555 H18 N1 0.934 1_555 1_555 H19 N1 0.931 1_555 1_555 H20 C9 0.870 1_555 1_555 H21 N1 1.134 1_555 1_555 C2J C1 1.509 1_555 1_555 O1J K1 2.786 1_555 1_555 O1A K1 2.786 1_555 1_555 C1A O1A 1.426 1_555 1_555 C2K C1A 1.509 1_555 1_555 O1K K1 2.786 1_555 1_555 O1B K1 2.786 1_555 1_555 C1B O1B 1.426 1_555 1_555 C2I C1B 1.509 1_555 1_555 O1I K1 2.786 1_555 1_555 N1A K1 2.864 1_555 1_555 N1B K1 2.864 1_555 1_555 C9A N1 1.479 1_555 1_555 C9B N1 0.807 1_555 1_555 H18B N1B 0.934 1_555 1_555 H17B N1B 0.963 1_555 1_555 H19B N1B 0.931 1_555 1_555 H20A C9 1.277 1_555 1_555 H20B C9A 1.277 1_555 1_555 H21A N1 0.782 1_555 1_555 H17A N1A 0.963 1_555 1_555 H18A C9 0.799 1_555 1_555 H19A C9 1.091 1_555 1_555 H21B C9 0.900 1_555 1_555 N1I K1 2.864 1_555 1_555 N1J K1 2.864 1_555 1_555 N1K K1 2.864 1_555 1_555 C9I N1I 1.186 1_555 1_555 C9J N1I 1.479 1_555 1_555 C9K N1I 0.807 1_555 1_555 H18K N1K 0.934 1_555 1_555 H17K N1K 0.963 1_555 1_555 H19K N1K 0.931 1_555 1_555 H20J C9I 1.277 1_555 1_555 H18I N1I 0.934 1_555 1_555 H17I N1I 0.963 1_555 1_555 H19I N1I 0.931 1_555 1_555 H20K C9J 1.277 1_555 1_555 H21I N1I 1.134 1_555 1_555 H21J N1I 0.782 1_555 1_555 H17J N1J 0.963 1_555 1_555 H18J N1J 0.934 1_555 1_555 H19J N1J 0.931 1_555 1_555 H21K N1J 0.782 1_555 1_555 H20I C9I 0.870 1_555 1_555 C1I O1I 1.426 1_555 1_555 C2A O1A 1.424 1_555 1_555 H3A C2A 1.045 1_555 1_555 H4A C2A 0.951 1_555 1_555 H1I C1I 1.156 1_555 1_555 H2I C1I 1.067 1_555 1_555 H3I C2I 1.045 1_555 1_555 H4I C2I 0.951 1_555 1_555 H1B C1B 1.156 1_555 1_555 H2B C1B 1.067 1_555 1_555 C2B O1B 1.424 1_555 1_555 C1J O1J 1.426 1_555 1_555 H1J C1J 1.156 1_555 1_555 H2J C1J 1.067 1_555 1_555 H3B C2B 1.045 1_555 1_555 H4B C2B 0.951 1_555 1_555 C1K C2 1.509 1_555 1_555 H1K C1K 1.156 1_555 1_555 H2K C1K 1.067 1_555 1_555 H3K C2K 1.045 1_555 1_555 H4K C2K 0.951 1_555 1_555 H1A C1A 1.156 1_555 1_555 H2A C1A 1.067 1_555 1_555 H3J C2J 1.045 1_555 1_555 H4J C2J 0.951 1_555 1_555 C8O C7 1.517 1_555 1_555 O2O C8O 1.424 1_555 1_555 C3O O2O 1.431 1_555 1_555 C4O C3O 1.507 1_555 1_555 O3O C4O 1.428 1_555 1_555 C5O O3O 1.435 1_555 1_555 C6O C5O 1.496 1_555 1_555 O4O C6O 1.418 1_555 1_555 C7O C8 1.517 1_555 1_555 H13O C7O 1.056 1_555 1_555 H14O C7O 1.037 1_555 1_555 H11O C6O 1.055 1_555 1_555 H12O C6O 1.090 1_555 1_555 H9O C5O 1.040 1_555 1_555 H10O C5O 0.959 1_555 1_555 H7O C4O 1.002 1_555 1_555 H8O C4O 0.941 1_555 1_555 H5O C3O 1.042 1_555 1_555 H6O C3O 1.082 1_555 1_555 H15O C8O 1.123 1_555 1_555 H16O C8O 0.999 1_555 1_555 N1 N1A 1.437 1_555 1_555 N1 N1B 1.437 1_555 1_555 C9 N1B 1.479 1_555 1_555 C9 N1A 0.807 1_555 1_555 C9 C9A 0.926 1_555 1_555 C9 C9B 0.926 1_555 1_555 C9 H21A 0.642 1_555 1_555 H18 C9B 0.799 1_555 1_555 H18 H21 0.679 1_555 1_555 H18 H19 0.476 1_555 1_555 H19 C9B 1.091 1_555 1_555 H20 C9B 1.277 1_555 1_555 H21 C9A 0.900 1_555 1_555 H21 N1B 0.782 1_555 1_555 H21 C9B 0.642 1_555 1_555 C2J O1J 1.424 1_555 1_555 C2K O1K 1.424 1_555 1_555 O1K C1K 1.426 1_555 1_555 C2I O1I 1.424 1_555 1_555 N1A C9A 1.186 1_555 1_555 N1A H18A 0.934 1_555 1_555 N1A H21B 0.782 1_555 1_555 N1A N1B 1.437 1_555 1_555 N1A C9B 1.479 1_555 1_555 N1A H21A 1.134 1_555 1_555 N1A H19A 0.931 1_555 1_555 N1B C9B 1.186 1_555 1_555 N1B C9A 0.807 1_555 1_555 N1B H21B 1.134 1_555 1_555 C9A H18B 0.799 1_555 1_555 C9A H20A 0.870 1_555 1_555 C9A C9B 0.926 1_555 1_555 C9A H19B 1.091 1_555 1_555 C9A H21B 0.642 1_555 1_555 C9B H20B 0.870 1_555 1_555 C9B H21A 0.900 1_555 1_555 H18B H21B 0.679 1_555 1_555 H18B H19B 0.476 1_555 1_555 H21A H18A 0.679 1_555 1_555 H18A H19A 0.476 1_555 1_555 N1I N1J 1.437 1_555 1_555 N1I N1K 1.437 1_555 1_555 N1J C9J 1.186 1_555 1_555 N1J N1K 1.437 1_555 1_555 N1J C9K 1.479 1_555 1_555 N1J C9I 0.807 1_555 1_555 N1J H21J 1.134 1_555 1_555 N1K C9I 1.479 1_555 1_555 N1K C9K 1.186 1_555 1_555 N1K C9J 0.807 1_555 1_555 N1K H21K 1.134 1_555 1_555 N1K H21I 0.782 1_555 1_555 C9I H19J 1.091 1_555 1_555 C9I C9J 0.926 1_555 1_555 C9I C9K 0.926 1_555 1_555 C9I H18J 0.799 1_555 1_555 C9I H21K 0.900 1_555 1_555 C9I H21J 0.642 1_555 1_555 C9J H18K 0.799 1_555 1_555 C9J H20J 0.870 1_555 1_555 C9J H21I 0.900 1_555 1_555 C9J C9K 0.926 1_555 1_555 C9J H19K 1.091 1_555 1_555 C9J H21K 0.642 1_555 1_555 C9K H18I 0.799 1_555 1_555 C9K H20K 0.870 1_555 1_555 C9K H20I 1.277 1_555 1_555 C9K H19I 1.091 1_555 1_555 C9K H21I 0.642 1_555 1_555 C9K H21J 0.900 1_555 1_555 H18K H21K 0.679 1_555 1_555 H18K H19K 0.476 1_555 1_555 H18I H21I 0.679 1_555 1_555 H18I H19I 0.476 1_555 1_555 H21J H18J 0.679 1_555 1_555 H18J H19J 0.476 1_555 1_555 C1I C2A 1.509 1_555 1_555 C2B C1J 1.509 1_555 1_555 O4O C7O 1.416 1_555 1_555 #END data_CSD_CIF_REGVUU _audit_creation_date 2001-11-22 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD REGVUU _chemical_formula_sum 'C20 H40 Cs1 N2 Na1 O7' _chemical_formula_moiety ; C20 H40 Cs1 N2 O7 1+,Na1 1- ; _journal_coden_Cambridge 211 _journal_volume 46 _journal_year 1998 _journal_page_first 13 _journal_name_full 'J.Coord.Chem. ' loop_ _publ_author_name "R.H.Huang" "S.Z.Huang" "J.L.Dye" _chemical_name_systematic ; (4,7,10,16,19,24,27-Heptaoxa-1,13-diazabicyclo(11.8.8)nonacosane)-cesium sodide ; _chemical_name_common ; (3.2.2-Cryptand)-cesium sodide ; _cell_volume 3057.731 _exptl_special_details ; air- and moisture-sensitive ; _exptl_crystal_preparation 'dimethyl ether/diethyl ether' _diffrn_ambient_temperature 170 _refine_special_details ; Atoms C11, C12, C14, C15, C28 and C29 of the cryptand are each disordered over two positions. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.045 _refine_ls_wR_factor_gt 0.045 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 -1/2+x,-1/2-y,-1/2+z _cell_length_a 12.2637(22) _cell_length_b 17.0657(39) _cell_length_c 15.6607(42) _cell_angle_alpha 90 _cell_angle_beta 111.106(17) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Cs 2.28 N 0.68 Na 0.97 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Cs1 Cs 0.2394(1) 0.10937(9) 0.48491(9) Na1 Na 0.2769(9) 0.1185(7) 0.0334(6) O1 O 0.183(1) -0.0670(8) 0.5203(9) O2 O 0.052(1) -0.0103(9) 0.336(1) O3 O 0.084(1) 0.139(1) 0.281(1) O4 O 0.263(1) 0.2880(9) 0.550(1) O5 O 0.204(1) 0.1756(7) 0.662(1) O6 O 0.502(1) 0.0920(8) 0.6116(8) O7 O 0.452(1) 0.1499(7) 0.429(1) N1 N 0.324(1) 0.026(1) 0.687(1) N2 N 0.258(1) 0.265(1) 0.362(1) C1 C 0.311(2) -0.058(1) 0.679(1) C2 C 0.197(2) -0.090(1) 0.612(1) C3 C 0.083(2) -0.101(2) 0.465(2) C4 C 0.073(2) -0.092(1) 0.364(2) C5 C 0.054(2) 0.005(2) 0.251(1) C6 C 0.014(2) 0.087(2) 0.222(2) C7 C 0.04950 0.22530 0.26480 C8? C 0.07480 0.20880 0.22180 C9 C 0.11960 0.26570 0.28210 C10? C 0.16040 0.26420 0.25070 C11 C 0.28530 0.34090 0.40340 C12? C 0.21730 0.34030 0.39610 C13 C 0.31260 0.34950 0.50400 C14? C 0.23850 0.35200 0.48480 C15 C 0.173(2) 0.298(1) 0.572(2) C16 C 0.190(2) 0.257(1) 0.662(1) C17 C 0.254(3) 0.140(1) 0.750(2) C18 C 0.257(2) 0.054(1) 0.741(2) C19 C 0.450(2) 0.042(1) 0.738(1) C20 C 0.525(2) 0.034(1) 0.679(1) C21 C 0.585(2) 0.096(2) 0.565(2) C22 C 0.563(2) 0.163(1) 0.505(2) C23 C 0.44810 0.21270 0.36460 C24? C 0.40800 0.18660 0.32900 C25 C 0.38590 0.27660 0.36020 C26? C 0.33960 0.24910 0.31400 H1 H 0.37080 -0.07870 0.66280 H2 H 0.31740 -0.07700 0.73870 H3 H 0.13290 -0.06880 0.62750 H4 H 0.19600 -0.14500 0.61700 H5 H 0.08580 -0.15690 0.47430 H6 H 0.01610 -0.08050 0.47190 H7 H 0.00650 -0.11820 0.31950 H8 H 0.14020 -0.10450 0.35090 H9 H 0.12930 -0.00500 0.24820 H10 H 0.00120 -0.02960 0.20480 H11 H -0.06540 0.09200 0.21440 H12 H 0.01830 0.09540 0.16010 H13 H 0.00420 0.23200 0.20170 H14 H 0.00330 0.23780 0.30040 H15 H 0.08670 0.31220 0.29600 H16 H 0.13210 0.27250 0.22610 H17 H 0.35180 0.35890 0.39160 H18 H 0.22060 0.37420 0.37350 H19 H 0.28350 0.39900 0.51380 H20 H 0.39530 0.34870 0.53320 H21 H 0.15810 0.35600 0.59140 H22 H 0.09380 0.28250 0.53890 H23 H 0.11510 0.27150 0.66780 H24 H 0.24930 0.28430 0.70510 H25 H 0.33300 0.15780 0.77490 H26 H 0.21170 0.15410 0.78470 H27 H 0.17860 0.03410 0.71410 H28 H 0.28980 0.03180 0.80200 H29 H 0.46230 0.09500 0.76130 H30 H 0.48280 0.00760 0.78990 H31 H 0.50940 -0.01690 0.65040 H32 H 0.60700 0.03480 0.71720 H33 H 0.65830 0.10200 0.61190 H34 H 0.57670 0.05060 0.53310 H35 H 0.62320 0.16920 0.48300 H36 H 0.55430 0.21080 0.53580 H37 H 0.52640 0.22940 0.37800 H38 H 0.41900 0.18980 0.30540 H39 H 0.37860 0.30290 0.30490 H40 H 0.42820 0.30870 0.41090 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cs1 O1 3.181 1_555 1_555 O1 C2 1.438 1_555 1_555 O2 Cs1 3.321 1_555 1_555 O3 Cs1 3.115 1_555 1_555 O4 Cs1 3.194 1_555 1_555 O5 Cs1 3.166 1_555 1_555 O6 Cs1 3.130 1_555 1_555 O7 Cs1 3.112 1_555 1_555 N1 Cs1 3.279 1_555 1_555 N2 Cs1 3.336 1_555 1_555 C1 N1 1.443 1_555 1_555 C2 C1 1.516 1_555 1_555 C3 O1 1.351 1_555 1_555 C4 O2 1.456 1_555 1_555 C5 O2 1.365 1_555 1_555 C6 O3 1.344 1_555 1_555 C7 O3 1.528 1_555 1_555 C9 N2 1.708 1_555 1_555 C11 N2 1.433 1_555 1_555 C13 O4 1.519 1_555 1_555 C15 O4 1.281 1_555 1_555 C16 O5 1.400 1_555 1_555 C17 O5 1.427 1_555 1_555 C18 N1 1.456 1_555 1_555 C19 N1 1.487 1_555 1_555 C20 O6 1.400 1_555 1_555 C21 O6 1.452 1_555 1_555 C22 O7 1.467 1_555 1_555 C23 O7 1.461 1_555 1_555 C25 N2 1.591 1_555 1_555 H1 C1 0.928 1_555 1_555 H2 C1 0.966 1_555 1_555 H3 C2 0.972 1_555 1_555 H4 C2 0.942 1_555 1_555 H5 C3 0.964 1_555 1_555 H6 C3 0.933 1_555 1_555 H7 C4 0.970 1_555 1_555 H8 C4 0.943 1_555 1_555 H9 C5 0.956 1_555 1_555 H10 C5 0.977 1_555 1_555 H11 C6 0.941 1_555 1_555 H12 C6 1.000 1_555 1_555 H13 C7 0.950 1_555 1_555 H14 C7 0.951 1_555 1_555 H15 C9 0.950 1_555 1_555 H16 C9 0.950 1_555 1_555 H17 C11 0.950 1_555 1_555 H18 C11 0.951 1_555 1_555 H19 C13 0.951 1_555 1_555 H20 C13 0.951 1_555 1_555 H21 C15 1.070 1_555 1_555 H22 C15 0.959 1_555 1_555 H23 C16 0.987 1_555 1_555 H24 C16 0.921 1_555 1_555 H25 C17 0.954 1_555 1_555 H26 C17 0.908 1_555 1_555 H27 C18 0.962 1_555 1_555 H28 C18 0.970 1_555 1_555 H29 C19 0.967 1_555 1_555 H30 C19 0.965 1_555 1_555 H31 C20 0.964 1_555 1_555 H32 C20 0.968 1_555 1_555 H33 C21 0.939 1_555 1_555 H34 C21 0.908 1_555 1_555 H35 C22 0.926 1_555 1_555 H36 C22 0.973 1_555 1_555 H37 C23 0.950 1_555 1_555 H38 C23 0.949 1_555 1_555 H39 C25 0.951 1_555 1_555 H40 C25 0.950 1_555 1_555 C3 C4 1.549 1_555 1_555 C5 C6 1.498 1_555 1_555 C7 C9 1.058 1_555 1_555 C11 C13 1.495 1_555 1_555 C15 C16 1.519 1_555 1_555 C17 C18 1.476 1_555 1_555 C19 C20 1.527 1_555 1_555 C21 C22 1.442 1_555 1_555 C23 C25 1.318 1_555 1_555 #END data_CSD_CIF_REGXAC _audit_creation_date 2001-11-22 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD REGXAC _chemical_formula_sum 'C17.5 H39.5 Li1 N5.5 Na1' _chemical_formula_moiety ; C17 H37 Li1 N5 1+,Na1 1-,0.5(C1 H5 N1) ; _journal_coden_Cambridge 211 _journal_volume 46 _journal_year 1998 _journal_page_first 13 _journal_name_full 'J.Coord.Chem. ' loop_ _publ_author_name "R.H.Huang" "S.Z.Huang" "J.L.Dye" _chemical_name_systematic ; (5,12,17-Trimethyl-1,5,9,12,17-penta-azabicyclo(7.5.5)nonadecane-N,N',N'',N''' ,N'''')-lithium sodide methylamine solvate ; _cell_volume 2283.446 _exptl_special_details ; air-sensitive and moisture-sensitive ; _diffrn_ambient_temperature 175 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.07 _refine_ls_wR_factor_gt 0.07 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P c' _symmetry_Int_Tables_number 7 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x,-y,1/2+z _cell_length_a 9.2280(36) _cell_length_b 15.3977(59) _cell_length_c 16.0970(67) _cell_angle_alpha 90 _cell_angle_beta 93.293(32) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.53 N 0.68 Na 0.97 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 0.6962(4) 0.4741(2) 0.5858(2) Na2 Na 0.2094(2) 0.03362(8) 0.85625(9) Li1 Li 0.7184(12) 0.1332(7) 0.3233(6) Li2 Li 1.1982(14) 0.3562(7) 0.8596(8) N1 N 0.9958(6) 0.3070(4) 0.8396(3) N2 N 1.2011(6) 0.3071(4) 0.9889(3) N3 N 1.4050(6) 0.3166(4) 0.8600(3) N4 N 1.2041(6) 0.2970(3) 0.7085(3) N5 N 1.1974(7) 0.4859(3) 0.8483(3) N6 N 0.8510(6) 0.1484(4) 0.2197(3) N7 N 0.7068(6) -0.0028(4) 0.2871(3) N8 N 0.6882(6) 0.0885(4) 0.4465(3) N9 N 0.9067(6) 0.2043(4) 0.3879(3) N10 N 0.5300(6) 0.1996(4) 0.2898(3) N11 N 0.2268(13) 0.0295(8) 0.6107(6) C1 C 0.9599(8) 0.2779(6) 0.9232(4) C2 C 1.0925(9) 0.2396(5) 0.9708(4) C3 C 1.3474(9) 0.2698(6) 1.0031(4) C4 C 1.4177(9) 0.2461(5) 0.9209(4) C5 C 1.4475(8) 0.2855(5) 0.7780(4) C6 C 1.3223(9) 0.2383(5) 0.7324(4) C7 C 1.0621(8) 0.2540(5) 0.7002(4) C8 C 0.9978(8) 0.2330(5) 0.7813(4) C9 C 0.8929(8) 0.3742(5) 0.8082(5) C10 C 0.9280(9) 0.4650(5) 0.8391(5) C11 C 1.0644(10) 0.5037(5) 0.8014(5) C12 C 1.3241(10) 0.4985(6) 0.7956(5) C13 C 1.4715(9) 0.4760(5) 0.8361(5) C14 C 1.4891(8) 0.3943(5) 0.8898(4) C15 C 1.1667(11) 0.3572(6) 1.0611(5) C16 C 1.2327(11) 0.3402(6) 0.6292(4) C17 C 1.2114(12) 0.5452(6) 0.9223(6) C18 C 0.8334(8) 0.0660(5) 0.1739(4) C19 C 0.8320(8) -0.0103(5) 0.2338(4) C20 C 0.7313(9) -0.0468(4) 0.3678(4) C21 C 0.6424(10) -0.0024(5) 0.4321(4) C22 C 0.8342(9) 0.0940(7) 0.4910(4) C23 C 0.9536(9) 0.1265(6) 0.4360(5) C24 C 1.0127(9) 0.2237(6) 0.3247(5) C25 C 1.0024(7) 0.1580(5) 0.2537(4) C26 C 0.8093(9) 0.2235(5) 0.1661(4) C27 C 0.6484(3) 0.2410(6) 0.1576(4) C28 C 0.5823(9) 0.2710(5) 0.2379(5) C29 C 0.4841(10) 0.2377(5) 0.3696(5) C30 C 0.4484(9) 0.1689(6) 0.4344(5) C31 C 0.5778(10) 0.1380(6) 0.4901(4) C32 C 0.5724(10) -0.0347(5) 0.2438(5) C33 C 0.8987(13) 0.2801(6) 0.4419(6) C34 C 0.4020(8) 0.1611(6) 0.2474(5) C35 C 0.2851(20) -0.0398(7) 0.5680(6) H1 H 0.884(11) 0.2344(57) 0.9181(49) H2 H 0.9238(94) 0.3267(57) 0.954(5) H3 H 1.0637(9) 0.2141(55) 1.0224(51) H4 H 1.1339(93) 0.1941(56) 0.9379(50) H5 H 1.3414(96) 0.2180(59) 1.0370(51) H6 H 1.4089(96) 0.3113(56) 1.0336(49) H7 H 1.520(11) 0.2327(55) 0.9328(50) H8 H 1.3710(97) 0.1945(58) 0.8973(50) H9 H 1.5299(12) 0.2466(58) 0.7855(48) H10 H 1.4766(93) 0.3345(57) 0.7449(49) H11 H 1.3566(95) 0.2108(54) 0.6830(53) H12 H 1.2870(95) 0.1932(55) 0.7680(51) H13 H 1.0721(93) 0.2005(57) 0.6692(50) H14 H 0.9952(99) 0.2912(56) 0.6681(51) H15 H 0.8991(98) 0.2128(51) 0.7701(45) H16 H 1.0527(93) 0.1860(56) 0.8079(45) H17 H 0.797(10) 0.3588(53) 0.8243(49) H18 H 0.8908(91) 0.3742(51) 0.7479(54) H19 H 0.943(11) 0.4638(58) 0.8992(61) H20 H 0.846(11) 0.5025(63) 0.8253(52) H21 H 1.071(11) 0.4809(59) 0.7456(62) H22 H 1.053(11) 0.5661(69) 0.7969(53) H23 H 1.309(10) 0.4635(56) 0.7458(59) H24 H 1.326(10) 0.5588(65) 0.7783(53) H25 H 1.503(11) 0.5251(59) 0.8704(53) H26 H 1.539(11) 0.4713(55) 0.7921(56) H27 H 1.591(10) 0.3789(54) 0.8942(47) H28 H 1.4608(86) 0.4086(52) 0.9454(51) H29 H 1.067(14) 0.3748(71) 1.0557(66) H30 H 1.228(13) 0.4078(73) 1.0651(62) H31 H 1.183(12) 0.3225(69) 1.1102(70) H32 H 1.1521(26) 0.3769(71) 0.6124(61) H33 H 1.246(11) 0.2971(69) 0.5872(67) H34 H 1.319(13) 0.3748(72) 0.6365(60) H35 H 1.303(15) 0.5355(73) 0.9520(75) H36 H 1.134(14) 0.5336(70) 0.9584(72) H37 H 1.206(13) 0.6045(80) 0.9039(66) H38 H 0.9125(95) 0.0590(55) 0.1373(48) H39 H 0.7432(99) 0.0671(53) 0.1398(49) H40 H 0.8253(87) -0.0643(54) 0.2027(45) H41 H 0.922(10) -0.0112(50) 0.2684(49) H42 H 0.834(11) -0.0444(54) 0.3854(50) H43 H 0.7031(95) -0.1073(56) 0.3625(46) H44 H 0.541(11) -0.0036(59) 0.4132(52) H45 H 0.653(10) -0.0342(53) 0.4841(55) H46 H 0.861(11) 0.0370(62) 0.5123(61) H47 H 0.829(10) 0.1328(59) 0.5382(56) H48 H 1.040(11) 0.1404(57) 0.4708(55) H49 H 0.979(10) 0.0808(60) 0.3979(54) H50 H 1.110(11) 0.2227(58) 0.3508(54) H51 H 0.995(10) 0.2815(65) 0.3026(51) H52 H 1.0629(91) 0.1769(49) 0.2098(50) H53 H 1.0382(87) 0.1021(57) 0.2738(46) H54 H 0.8439(95) 0.2135(55) 0.1111(55) H55 H 0.858(10) 0.2749(61) 0.1887(50) H56 H 0.5993(99) 0.1884(64) 0.1384(48) H57 H 0.6301(94) 0.2851(57) 0.1153(53) H58 H 0.655(10) 0.3041(59) 0.2706(51) H59 H 0.502(10) 0.3097(60) 0.2235(49) H60 H 0.399(11) 0.2738(60) 0.3579(51) H61 H 0.561(11) 0.2747(59) 0.3928(53) H62 H 0.376(11) 0.1925(61) 0.4695(56) H63 H 0.406(10) 0.1190(66) 0.4055(56) H64 H 0.624(11) 0.1883(64) 0.5164(57) H65 H 0.542(11) 0.1018(64) 0.5338(58) H66 H 0.554(11) -0.0029(69) 0.1929(61) H67 H 0.493(12) -0.0266(61) 0.2788(61) H68 H 0.582(11) -0.0953(69) 0.2315(56) H69 H 0.842(14) 0.2663(80) 0.4881(76) H70 H 0.854(14) 0.3274(84) 0.4110(73) H71 H 0.995(14) 0.2964(80) 0.4620(72) H72 H 0.359(11) 0.1201(68) 0.2836(60) H73 H 0.429(11) 0.1320(63) 0.1979(63) H74 H 0.333(12) 0.2060(67) 0.2326(59) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 N6 2.137 1_555 1_555 Li2 N1 2.024 1_555 1_555 N1 C1 1.474 1_555 1_555 N2 Li2 2.213 1_555 1_555 N3 Li2 2.003 1_555 1_555 N4 Li2 2.601 1_555 1_555 N5 Li2 2.005 1_555 1_555 N6 C18 1.472 1_555 1_555 N7 Li1 2.175 1_555 1_555 N8 Li1 2.133 1_555 1_555 N9 Li1 2.256 1_555 1_555 N10 Li1 2.062 1_555 1_555 N11 C35 1.394 1_555 1_555 C1 C2 1.525 1_555 1_555 C2 N2 1.461 1_555 1_555 C3 N2 1.473 1_555 1_555 C4 N3 1.463 1_555 1_555 C5 N3 1.478 1_555 1_555 C6 N4 1.451 1_555 1_555 C7 N4 1.467 1_555 1_555 C8 N1 1.477 1_555 1_555 C9 N1 1.474 1_555 1_555 C10 C9 1.513 1_555 1_555 C11 N5 1.430 1_555 1_555 C12 N5 1.496 1_555 1_555 C13 C12 1.514 1_555 1_555 C14 N3 1.490 1_555 1_555 C15 N2 1.445 1_555 1_555 C16 N4 1.477 1_555 1_555 C17 N5 1.501 1_555 1_555 C18 C19 1.520 1_555 1_555 C19 N7 1.483 1_555 1_555 C20 N7 1.471 1_555 1_555 C21 N8 1.477 1_555 1_555 C22 N8 1.492 1_555 1_555 C23 N9 1.478 1_555 1_555 C24 N9 1.482 1_555 1_555 C25 N6 1.478 1_555 1_555 C26 N6 1.480 1_555 1_555 C27 C26 1.508 1_555 1_555 C28 N10 1.478 1_555 1_555 C29 N10 1.495 1_555 1_555 C30 C29 1.536 1_555 1_555 C31 N8 1.481 1_555 1_555 C32 N7 1.472 1_555 1_555 C33 N9 1.460 1_555 1_555 C34 N10 1.456 1_555 1_555 H1 C1 0.969 1_555 1_555 H2 C1 0.970 1_555 1_555 H3 C2 0.970 1_555 1_555 H4 C2 0.970 1_555 1_555 H5 C3 0.970 1_555 1_555 H6 C3 0.969 1_555 1_555 H7 C4 0.975 1_555 1_555 H8 C4 0.971 1_555 1_555 H9 C5 0.970 1_555 1_555 H10 C5 0.970 1_555 1_555 H11 C6 0.970 1_555 1_555 H12 C6 0.969 1_555 1_555 H13 C7 0.970 1_555 1_555 H14 C7 0.969 1_555 1_555 H15 C8 0.970 1_555 1_555 H16 C8 0.969 1_555 1_555 H17 C9 0.966 1_555 1_555 H18 C9 0.970 1_555 1_555 H19 C10 0.970 1_555 1_555 H20 C10 0.967 1_555 1_555 H21 C11 0.970 1_555 1_555 H22 C11 0.969 1_555 1_555 H23 C12 0.969 1_555 1_555 H24 C12 0.970 1_555 1_555 H25 C13 0.971 1_555 1_555 H26 C13 0.972 1_555 1_555 H27 C14 0.968 1_555 1_555 H28 C14 0.972 1_555 1_555 H29 C15 0.958 1_555 1_555 H30 C15 0.963 1_555 1_555 H31 C15 0.959 1_555 1_555 H32 C16 0.961 1_555 1_555 H33 C16 0.960 1_555 1_555 H34 C16 0.960 1_555 1_555 H35 C17 0.959 1_555 1_555 H36 C17 0.963 1_555 1_555 H37 C17 0.960 1_555 1_555 H38 C18 0.970 1_555 1_555 H39 C18 0.971 1_555 1_555 H40 C19 0.971 1_555 1_555 H41 C19 0.973 1_555 1_555 H42 C20 0.974 1_555 1_555 H43 C20 0.970 1_555 1_555 H44 C21 0.967 1_555 1_555 H45 C21 0.970 1_555 1_555 H46 C22 0.969 1_555 1_555 H47 C22 0.970 1_555 1_555 H48 C23 0.972 1_555 1_555 H49 C23 0.971 1_555 1_555 H50 C24 0.969 1_555 1_555 H51 C24 0.969 1_555 1_555 H52 C25 0.970 1_555 1_555 H53 C25 0.971 1_555 1_555 H54 C26 0.971 1_555 1_555 H55 C26 0.971 1_555 1_555 H56 C27 0.970 1_555 1_555 H57 C27 0.970 1_555 1_555 H58 C28 0.973 1_555 1_555 H59 C28 0.969 1_555 1_555 H60 C29 0.972 1_555 1_555 H61 C29 0.968 1_555 1_555 H62 C30 0.970 1_555 1_555 H63 C30 0.969 1_555 1_555 H64 C31 0.970 1_555 1_555 H65 C31 0.970 1_555 1_555 H66 C32 0.961 1_555 1_555 H67 C32 0.958 1_555 1_555 H68 C32 0.959 1_555 1_555 H69 C33 0.957 1_555 1_555 H70 C33 0.961 1_555 1_555 H71 C33 0.961 1_555 1_555 H72 C34 0.960 1_555 1_555 H73 C34 0.959 1_555 1_555 H74 C34 0.961 1_555 1_555 C3 C4 1.550 1_555 1_555 C5 C6 1.518 1_555 1_555 C7 C8 1.500 1_555 1_555 C10 C11 1.548 1_555 1_555 C13 C14 1.530 1_555 1_555 C20 C21 1.520 1_555 1_555 C22 C23 1.536 1_555 1_555 C24 C25 1.525 1_555 1_555 C27 C28 1.532 1_555 1_555 C30 C31 1.527 1_555 1_555 #END data_CSD_CIF_REHBUC _audit_creation_date 2006-06-21 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD REHBUC _database_code_depnum_ccdc_archive 'CCDC 605222' _chemical_formula_sum 'C146 H112 Li8 N32 O12' _chemical_formula_moiety ; C6 H20 Li2 O6 2+,C12 H28 Li2 O6 2+,4(C32 H16 Li1 N8 1-) ; _journal_coeditor_code "IUCr XU6105" _journal_coden_Cambridge 1370 _journal_volume 62 _journal_year 2006 _journal_page_first m827 _journal_name_full 'Acta Crystallogr.,Sect.E:Struct.Rep.Online ' loop_ _publ_author_name "D.A.Grossie" "W.A.Feld" "L.Scanlon" "G.Sandi" "Z.Wawrzak" _chemical_name_systematic ; bis(\m~2~-Acetone-O,O)-bis(acetone-O)-diaqua-di-lithium(i) bis(\m~2~-acetone-O,O)-tetra-aqua-di-lithium(i) tetrakis((phthalocyaninato-N,N',N'',N''')-lithium(i)) ; _cell_volume 3118.748 _exptl_crystal_colour 'purple' _exptl_crystal_density_diffrn 1.364 _exptl_crystal_description 'block' _diffrn_ambient_temperature 100 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.049 _refine_ls_wR_factor_gt 0.049 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 12.8017(6) _cell_length_b 14.3637(7) _cell_length_c 17.3859(8) _cell_angle_alpha 101.5838(9) _cell_angle_beta 94.1351(9) _cell_angle_gamma 92.3054(9) _cell_formula_units_Z 1 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.00 N 0.68 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.51818(14) 0.95205(13) 0.06887(11) N1 N 0.63594(7) 0.87772(6) 0.02443(5) N2 N 0.42809(7) 0.88277(6) -0.02491(5) N3 N 0.39241(7) 0.98926(6) 0.12432(5) N4 N 0.60172(7) 0.99048(6) 0.17084(5) N5 N 0.55504(7) 0.79554(6) -0.10245(5) N6 N 0.25786(7) 0.92698(6) 0.01849(5) N7 N 0.47216(7) 1.07087(6) 0.25146(5) N8 N 0.76920(7) 0.92923(6) 0.13275(5) C1 C 0.91086(8) 0.81084(7) 0.01437(6) C2 C 0.80507(8) 0.82906(7) 0.00680(6) C3 C 0.73572(8) 0.88376(7) 0.06007(6) C4 C 0.95097(8) 0.75106(8) -0.04869(6) C5 C 0.88799(9) 0.71209(8) -0.11808(6) C6 C 0.78270(8) 0.73159(7) -0.12614(6) C7 C 0.74215(8) 0.78990(7) -0.06255(6) C8 C 0.63717(8) 0.82283(7) -0.04891(6) C9 C 0.35380(9) 0.72500(7) -0.21886(6) C10 C 0.36664(8) 0.78553(7) -0.14500(6) C11 C 0.45806(8) 0.82259(7) -0.08982(6) C12 C 0.25205(9) 0.70552(8) -0.25454(7) C13 C 0.16585(9) 0.74582(8) -0.21762(7) C14 C 0.17871(8) 0.80576(8) -0.14387(6) C15 C 0.28013(8) 0.82463(7) -0.10836(6) C16 C 0.32113(8) 0.88364(7) -0.03288(6) C17 C 0.11182(8) 1.03022(8) 0.13601(6) C18 C 0.22005(8) 1.02365(7) 0.14426(6) C19 C 0.29237(8) 0.97605(7) 0.09026(6) C20 C 0.06521(9) 1.08280(8) 0.19914(7) C21 C 0.12563(9) 1.12829(8) 0.26778(7) C22 C 0.23408(9) 1.12171(8) 0.27567(6) C23 C 0.28122(8) 1.06797(7) 0.21296(6) C24 C 0.38983(8) 1.04333(7) 0.19806(6) C25 C 0.66046(8) 1.07138(7) 0.29700(6) C26 C 0.57066(8) 1.04546(7) 0.23774(6) C27 C 0.67386(9) 1.12744(8) 0.37277(6) C28 C 0.77320(9) 1.13621(8) 0.41220(6) C29 C 0.85765(9) 1.08972(9) 0.37742(7) C30 C 0.84495(8) 1.03419(8) 0.30188(6) C31 C 0.74570(8) 1.02659(7) 0.26195(6) C32 C 0.70627(8) 0.97780(7) 0.18267(6) H1 H 0.9549(12) 0.8383(10) 0.0626(9) H2 H 1.0249(12) 0.7337(11) -0.0447(9) H3 H 0.9181(12) 0.6697(11) -0.1633(9) H4 H 0.7410(12) 0.7057(10) -0.1741(9) H5 H 0.4112(12) 0.6993(11) -0.2454(9) H6 H 0.2413(12) 0.6652(11) -0.3067(9) H7 H 0.0962(13) 0.7333(11) -0.2444(9) H8 H 0.1212(12) 0.8343(11) -0.1173(9) H9 H 0.0718(12) 0.999(1) 0.0885(9) H10 H -0.0111(12) 1.0913(11) 0.1949(9) H11 H 0.0943(12) 1.1675(11) 0.3124(9) H12 H 0.2745(12) 1.1540(11) 0.3244(9) H13 H 0.6159(13) 1.1605(11) 0.3985(9) H14 H 0.7843(12) 1.1759(11) 0.4656(9) H15 H 0.9273(12) 1.0952(11) 0.4063(9) H16 H 0.9043(12) 1.0012(11) 0.2770(9) Li2 Li 0.44807(15) 0.49472(14) 0.32510(11) N9 N 0.53655(7) 0.43865(6) 0.39811(5) N10 N 0.32584(7) 0.42041(6) 0.34707(5) N11 N 0.36108(7) 0.54287(6) 0.24357(5) N12 N 0.57151(7) 0.55941(6) 0.29369(5) N13 N 0.40588(7) 0.34355(6) 0.44681(5) N14 N 0.19029(7) 0.47960(6) 0.26819(5) N15 N 0.49130(7) 0.64017(6) 0.19686(5) N16 N 0.70517(7) 0.51148(6) 0.38258(5) C33 C 0.77810(9) 0.40703(8) 0.51683(6) C34 C 0.67998(8) 0.40838(7) 0.47709(6) C35 C 0.64186(8) 0.45774(7) 0.41539(6) C36 C 0.78536(9) 0.35386(8) 0.57569(7) C37 C 0.69772(10) 0.30438(8) 0.59444(7) C38 C 0.59950(9) 0.30575(8) 0.55446(6) C39 C 0.59222(8) 0.35821(7) 0.49545(6) C40 C 0.50377(8) 0.37909(7) 0.44414(6) C41 C 0.17125(9) 0.29347(8) 0.46889(6) C42 C 0.21545(8) 0.34094(7) 0.41571(6) C43 C 0.32379(8) 0.36762(7) 0.40382(6) C44 C 0.06234(9) 0.28541(9) 0.46659(7) C45 C -0.00089(9) 0.32470(8) 0.41352(7) C46 C 0.04334(8) 0.37428(8) 0.36180(6) C47 C 0.15210(8) 0.38095(7) 0.36305(6) C48 C 0.22452(8) 0.43007(7) 0.32099(6) C49 C 0.11086(9) 0.61068(8) 0.15932(7) C50 C 0.21320(8) 0.59495(7) 0.18457(6) C51 C 0.25404(8) 0.53282(7) 0.23479(6) C52 C 0.09706(9) 0.67776(9) 0.11241(7) C53 C 0.18349(9) 0.72861(8) 0.09228(7) C54 C 0.28565(9) 0.71284(8) 0.11748(7) C55 C 0.30025(8) 0.64439(7) 0.16372(6) C56 C 0.39216(8) 0.60931(7) 0.20208(6) C57 C 0.72687(9) 0.71874(8) 0.19702(7) C58 C 0.68169(8) 0.65420(7) 0.23707(6) C59 C 0.57383(8) 0.61618(7) 0.23964(6) C60 C 0.83358(9) 0.74302(9) 0.21344(7) C61 C 0.89446(9) 0.70356(9) 0.26774(7) C62 C 0.85002(9) 0.63964(8) 0.30814(7) C63 C 0.74292(8) 0.61615(7) 0.29237(6) C64 C 0.67117(8) 0.55715(7) 0.32637(6) H17 H 0.8384(11) 0.4428(10) 0.5039(8) H18 H 0.8536(12) 0.3546(11) 0.6049(9) H19 H 0.7029(12) 0.2697(11) 0.6376(9) H20 H 0.5435(13) 0.2720(11) 0.5695(9) H21 H 0.2138(12) 0.2676(11) 0.5075(9) H22 H 0.0281(13) 0.2523(12) 0.5037(10) H23 H -0.0771(12) 0.3188(10) 0.4124(9) H24 H 0.0017(11) 0.4044(10) 0.3267(8) H25 H 0.0519(12) 0.5766(11) 0.1734(9) H26 H 0.0252(12) 0.6902(11) 0.0934(9) H27 H 0.1723(13) 0.7765(12) 0.0605(10) H28 H 0.3422(12) 0.7493(11) 0.1044(9) H29 H 0.6872(12) 0.7456(11) 0.1580(9) H30 H 0.8651(12) 0.7885(11) 0.1873(9) H31 H 0.9684(13) 0.7219(12) 0.276(1) H32 H 0.8921(13) 0.6123(11) 0.3453(9) Li3 Li 0.47969(17) 0.41601(15) 0.03018(12) O1 O 0.45711(7) 0.39829(6) 0.13103(5) O2 O 0.47560(7) 0.30728(6) -0.05210(5) O3 O 0.60733(7) 0.49545(6) 0.01914(5) C65 C 0.73898(13) 0.43906(11) 0.09823(10) C66 C 0.70069(9) 0.49722(8) 0.04084(7) C67 C 0.77953(11) 0.5570(1) 0.01056(9) H33 H 0.4609(14) 0.2493(14) -0.0529(11) H34 H 0.4492(13) 0.3383(13) 0.1387(10) H35 H 0.4853(15) 0.3175(14) -0.1003(12) H36 H 0.4312(15) 0.4329(14) 0.1686(12) H37 H 0.6831(19) 0.4173(17) 0.1244(14) H38 H 0.7875(19) 0.4765(17) 0.1416(14) H39 H 0.776(2) 0.3895(18) 0.0730(14) H40 H 0.747(2) 0.5857(19) -0.0280(15) H41 H 0.8308(18) 0.5181(16) -0.0148(13) H42 H 0.814(2) 0.6021(18) 0.0522(15) Li4 Li 0.41436(17) 1.02150(15) 0.44798(12) O4 O 0.42815(7) 1.13473(6) 0.41009(5) O5 O 0.54188(7) 0.94715(6) 0.43774(5) O6 O 0.28914(8) 0.95264(7) 0.40014(6) C68 C 0.68804(12) 0.86134(11) 0.39528(9) C69 C 0.57976(10) 0.89366(8) 0.38390(7) C70 C 0.51837(11) 0.85763(9) 0.30706(7) C71 C 0.18547(14) 0.87296(11) 0.28622(9) C72 C 0.20223(10) 0.92880(9) 0.36823(8) C73 C 0.10675(16) 0.9553(2) 0.41007(12) H43 H 0.12760 0.98620 0.46490 H44 H 0.06210 0.89790 0.40880 H45 H 0.06790 0.99930 0.38400 H46 H 0.4242(14) 1.1974(14) 0.4278(11) H47 H 0.4389(16) 1.1230(14) 0.3556(12) H48 H 0.7153(14) 0.8793(13) 0.4500(11) H49 H 0.730(2) 0.882(2) 0.3595(17) H50 H 0.6850(16) 0.7933(16) 0.3830(12) H51 H 0.4566(13) 0.8951(12) 0.3029(10) H52 H 0.4963(15) 0.7918(14) 0.3039(11) H53 H 0.5644(14) 0.8594(12) 0.2617(10) H54 H 0.2566(19) 0.8672(16) 0.2627(13) H55 H 0.1374(16) 0.9056(15) 0.2557(12) H56 H 0.1505(16) 0.8125(16) 0.2826(12) Li3A Li 0.52031(17) 0.58399(15) -0.03018(12) O1A O 0.54289(7) 0.60171(6) -0.13103(5) O2A O 0.52440(7) 0.69272(6) 0.05210(5) O3A O 0.39267(7) 0.50455(6) -0.01914(5) C65A C 0.26102(13) 0.56094(11) -0.09823(10) C66A C 0.29931(9) 0.50278(8) -0.04084(7) C67A C 0.22047(11) 0.4430(1) -0.01056(9) H33A H 0.5391(14) 0.7507(14) 0.0529(11) H34A H 0.5508(13) 0.6617(13) -0.1387(10) H35A H 0.5147(15) 0.6825(14) 0.1003(12) H36A H 0.5688(15) 0.5671(14) -0.1686(12) H37A H 0.3169(19) 0.5827(17) -0.1244(14) H38A H 0.2125(19) 0.5235(17) -0.1416(14) H39A H 0.224(2) 0.6105(18) -0.0730(14) H40A H 0.253(2) 0.4143(19) 0.0280(15) H41A H 0.1692(18) 0.4819(16) 0.0148(13) H42A H 0.186(2) 0.3979(18) -0.0522(15) Li4A Li 0.58564(17) 0.97850(15) 0.55202(12) O4A O 0.57185(7) 0.86527(6) 0.58991(5) O5A O 0.45812(7) 1.05285(6) 0.56226(5) O6A O 0.71086(8) 1.04736(7) 0.59986(6) C68A C 0.31196(12) 1.13866(11) 0.60472(9) C69A C 0.42024(10) 1.10634(8) 0.61610(7) C70A C 0.48163(11) 1.14237(9) 0.69294(7) C71A C 0.81453(14) 1.12704(11) 0.71378(9) C72A C 0.79777(10) 1.07120(9) 0.63177(8) C73A C 0.89325(16) 1.0447(2) 0.58993(12) H43A H 0.87240 1.01380 0.53510 H44A H 0.93790 1.10210 0.59120 H45A H 0.93210 1.00070 0.61600 H46A H 0.5758(14) 0.8026(14) 0.5722(11) H47A H 0.5611(16) 0.8770(14) 0.6444(12) H48A H 0.2847(14) 1.1207(13) 0.5500(11) H49A H 0.270(2) 1.118(2) 0.6405(17) H50A H 0.3150(16) 1.2067(16) 0.6170(12) H51A H 0.5434(13) 1.1049(12) 0.6971(10) H52A H 0.5037(15) 1.2082(14) 0.6961(11) H53A H 0.4356(14) 1.1406(12) 0.7383(10) H54A H 0.7434(19) 1.1328(16) 0.7373(13) H55A H 0.8626(16) 1.0944(15) 0.7443(12) H56A H 0.8495(16) 1.1875(16) 0.7174(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 N1 1.994 1_555 1_555 N1 C3 1.371 1_555 1_555 N2 Li1 1.991 1_555 1_555 N3 Li1 1.973 1_555 1_555 N4 Li1 1.969 1_555 1_555 N5 C8 1.343 1_555 1_555 N6 C16 1.328 1_555 1_555 N7 C24 1.344 1_555 1_555 N8 C3 1.332 1_555 1_555 C1 C2 1.392 1_555 1_555 C2 C3 1.465 1_555 1_555 C4 C1 1.393 1_555 1_555 C5 C4 1.404 1_555 1_555 C6 C5 1.391 1_555 1_555 C7 C2 1.404 1_555 1_555 C8 N1 1.359 1_555 1_555 C9 C10 1.393 1_555 1_555 C10 C11 1.468 1_555 1_555 C11 N2 1.366 1_555 1_555 C12 C9 1.394 1_555 1_555 C13 C12 1.403 1_555 1_555 C14 C13 1.388 1_555 1_555 C15 C10 1.399 1_555 1_555 C16 N2 1.367 1_555 1_555 C17 C18 1.392 1_555 1_555 C18 C19 1.458 1_555 1_555 C19 N3 1.361 1_555 1_555 C20 C17 1.389 1_555 1_555 C21 C20 1.401 1_555 1_555 C22 C21 1.394 1_555 1_555 C23 C18 1.402 1_555 1_555 C24 N3 1.362 1_555 1_555 C25 C26 1.471 1_555 1_555 C26 N4 1.363 1_555 1_555 C27 C25 1.394 1_555 1_555 C28 C27 1.389 1_555 1_555 C29 C28 1.404 1_555 1_555 C30 C29 1.388 1_555 1_555 C31 C25 1.404 1_555 1_555 C32 N4 1.364 1_555 1_555 H1 C1 0.979 1_555 1_555 H2 C4 0.990 1_555 1_555 H3 C5 1.004 1_555 1_555 H4 C6 0.956 1_555 1_555 H5 C9 0.944 1_555 1_555 H6 C12 0.970 1_555 1_555 H7 C13 0.968 1_555 1_555 H8 C14 0.960 1_555 1_555 H9 C17 0.958 1_555 1_555 H10 C20 0.989 1_555 1_555 H11 C21 0.984 1_555 1_555 H12 C22 0.980 1_555 1_555 H13 C27 0.983 1_555 1_555 H14 C28 0.984 1_555 1_555 H15 C29 0.983 1_555 1_555 H16 C30 0.991 1_555 1_555 Li2 N9 1.954 1_555 1_555 N9 C35 1.364 1_555 1_555 N10 Li2 1.962 1_555 1_555 N11 Li2 1.989 1_555 1_555 N12 Li2 1.967 1_555 1_555 N13 C40 1.341 1_555 1_555 N14 C48 1.330 1_555 1_555 N15 C56 1.343 1_555 1_555 N16 C35 1.331 1_555 1_555 C33 C34 1.392 1_555 1_555 C34 C35 1.466 1_555 1_555 C36 C33 1.395 1_555 1_555 C37 C36 1.397 1_555 1_555 C38 C37 1.395 1_555 1_555 C39 C34 1.401 1_555 1_555 C40 N9 1.358 1_555 1_555 C41 C42 1.392 1_555 1_555 C42 C43 1.464 1_555 1_555 C43 N10 1.361 1_555 1_555 C44 C41 1.391 1_555 1_555 C45 C44 1.401 1_555 1_555 C46 C45 1.391 1_555 1_555 C47 C42 1.403 1_555 1_555 C48 N10 1.365 1_555 1_555 C49 C50 1.393 1_555 1_555 C50 C51 1.455 1_555 1_555 C51 N11 1.366 1_555 1_555 C52 C49 1.390 1_555 1_555 C53 C52 1.405 1_555 1_555 C54 C53 1.391 1_555 1_555 C55 C50 1.406 1_555 1_555 C56 N11 1.370 1_555 1_555 C57 C58 1.397 1_555 1_555 C58 C59 1.471 1_555 1_555 C59 N12 1.363 1_555 1_555 C60 C57 1.391 1_555 1_555 C61 C60 1.402 1_555 1_555 C62 C61 1.391 1_555 1_555 C63 C58 1.405 1_555 1_555 C64 N12 1.363 1_555 1_555 H17 C33 0.975 1_555 1_555 H18 C36 0.977 1_555 1_555 H19 C37 0.980 1_555 1_555 H20 C38 0.931 1_555 1_555 H21 C41 0.974 1_555 1_555 H22 C44 0.991 1_555 1_555 H23 C45 0.974 1_555 1_555 H24 C46 0.960 1_555 1_555 H25 C49 0.956 1_555 1_555 H26 C52 0.990 1_555 1_555 H27 C53 0.974 1_555 1_555 H28 C54 0.944 1_555 1_555 H29 C57 0.969 1_555 1_555 H30 C60 0.959 1_555 1_555 H31 C61 0.965 1_555 1_555 H32 C62 0.965 1_555 1_555 Li3 O1 1.863 1_555 1_555 O1 H34 0.901 1_555 1_555 O2 Li3 1.890 1_555 1_555 O3 Li3 1.998 1_555 1_555 C65 C66 1.494 1_555 1_555 C66 O3 1.225 1_555 1_555 C67 C66 1.490 1_555 1_555 H33 O2 0.844 1_555 1_555 H35 O2 0.896 1_555 1_555 H36 O1 0.835 1_555 1_555 H37 C65 0.950 1_555 1_555 H38 C65 0.993 1_555 1_555 H39 C65 0.925 1_555 1_555 H40 C67 0.937 1_555 1_555 H41 C67 0.954 1_555 1_555 H42 C67 0.939 1_555 1_555 Li4 O4 1.880 1_555 1_555 O4 H46 0.896 1_555 1_555 O5 Li4 1.986 1_555 1_555 O6 Li4 1.895 1_555 1_555 C68 C69 1.492 1_555 1_555 C69 O5 1.228 1_555 1_555 C70 C69 1.486 1_555 1_555 C71 C72 1.485 1_555 1_555 C72 O6 1.211 1_555 1_555 C73 C72 1.491 1_555 1_555 H43 C73 0.980 1_555 1_555 H44 C73 0.980 1_555 1_555 H45 C73 0.980 1_555 1_555 H47 O4 0.949 1_555 1_555 H48 C68 0.969 1_555 1_555 H49 C68 0.934 1_555 1_555 H50 C68 0.956 1_555 1_555 H51 C70 0.981 1_555 1_555 H52 C70 0.966 1_555 1_555 H53 C70 1.022 1_555 1_555 H54 C71 1.024 1_555 1_555 H55 C71 0.978 1_555 1_555 H56 C71 0.949 1_555 1_555 Li3A O3 2.002 1_555 1_555 O1A Li3A 1.863 1_555 1_555 O2A Li3A 1.890 1_555 1_555 O3A Li3 2.002 1_555 1_555 C65A C66A 1.494 1_555 1_555 C66A O3A 1.225 1_555 1_555 C67A C66A 1.490 1_555 1_555 H33A O2A 0.844 1_555 1_555 H34A O1A 0.901 1_555 1_555 H35A O2A 0.896 1_555 1_555 H36A O1A 0.835 1_555 1_555 H37A C65A 0.950 1_555 1_555 H38A C65A 0.993 1_555 1_555 H39A C65A 0.925 1_555 1_555 H40A C67A 0.937 1_555 1_555 H41A C67A 0.954 1_555 1_555 H42A C67A 0.939 1_555 1_555 Li4A O5 1.981 1_555 1_555 O4A Li4A 1.880 1_555 1_555 O5A Li4 1.981 1_555 1_555 O6A Li4A 1.895 1_555 1_555 C68A C69A 1.492 1_555 1_555 C69A O5A 1.228 1_555 1_555 C70A C69A 1.486 1_555 1_555 C71A C72A 1.485 1_555 1_555 C72A O6A 1.211 1_555 1_555 C73A C72A 1.491 1_555 1_555 H43A C73A 0.980 1_555 1_555 H44A C73A 0.980 1_555 1_555 H45A C73A 0.980 1_555 1_555 H46A O4A 0.896 1_555 1_555 H47A O4A 0.949 1_555 1_555 H48A C68A 0.969 1_555 1_555 H49A C68A 0.934 1_555 1_555 H50A C68A 0.956 1_555 1_555 H51A C70A 0.981 1_555 1_555 H52A C70A 0.966 1_555 1_555 H53A C70A 1.022 1_555 1_555 H54A C71A 1.024 1_555 1_555 H55A C71A 0.978 1_555 1_555 H56A C71A 0.949 1_555 1_555 N5 C11 1.336 1_555 1_555 N6 C19 1.338 1_555 1_555 N7 C26 1.351 1_555 1_555 N8 C32 1.339 1_555 1_555 C6 C7 1.393 1_555 1_555 C7 C8 1.462 1_555 1_555 C14 C15 1.389 1_555 1_555 C15 C16 1.461 1_555 1_555 C22 C23 1.394 1_555 1_555 C23 C24 1.477 1_555 1_555 C30 C31 1.393 1_555 1_555 C31 C32 1.459 1_555 1_555 N13 C43 1.342 1_555 1_555 N14 C51 1.336 1_555 1_555 N15 C59 1.344 1_555 1_555 N16 C64 1.339 1_555 1_555 C38 C39 1.390 1_555 1_555 C39 C40 1.469 1_555 1_555 C46 C47 1.390 1_555 1_555 C47 C48 1.464 1_555 1_555 C54 C55 1.399 1_555 1_555 C55 C56 1.467 1_555 1_555 C62 C63 1.393 1_555 1_555 C63 C64 1.459 1_555 1_555 Li3A O3A 1.998 1_555 1_555 Li4A O5A 1.986 1_555 1_555 #END data_CSD_CIF_REJBAK _audit_creation_date 2006-10-19 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD REJBAK _database_code_depnum_ccdc_archive 'CCDC 614723' _chemical_formula_sum 'C14 H28 Cs1 Li1 N2 O4' _chemical_formula_moiety ; C14 H28 Li1 N2 O4 1+,Cs1 1- ; _journal_coden_Cambridge 1278 _journal_volume 110 _journal_year 2006 _journal_page_first 12293 _journal_name_full 'J.Phys.Chem.B ' loop_ _publ_author_name "A.S.Ichimura" "R.H.Huang" "Qingshan Xie" "P.Morganelli" "A.Burns" "J.L.Dye" _chemical_name_systematic ; (2.1.1)Cryptand-lithium ceside ; _cell_volume 2534.589 _exptl_crystal_density_diffrn 1.122 _diffrn_ambient_temperature 173 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.1194 _refine_ls_wR_factor_gt 0.1194 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,z 3 -x,y,-z 4 1/2-x,1/2+y,-z 5 -x,-y,-z 6 -1/2-x,-1/2-y,-z 7 x,-y,z 8 -1/2+x,-1/2-y,z _cell_length_a 23.748(15) _cell_length_b 13.434(8) _cell_length_c 8.212(12) _cell_angle_alpha 90 _cell_angle_beta 75.34(9) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Cs 1.67 Li 1.16 N 0.68 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Cs1 Cs 0.40513(7) 0.00000 0.8213(3) Li1 Li 0.1016(9) 0.00000 0.6788(29) O1 O 0.0279(4) 0.0956(8) 0.7277(11) O2 O 0.1485(5) 0.00000 0.4177(14) O3 O 0.1414(5) 0.00000 0.8843(12) N1 N 0.1407(7) 0.1521(14) 0.6527(16) C1 C 0.0965(13) 0.2258(17) 0.6775(23) H1 H 0.1002(13) 0.2680(17) 0.7702(23) H2 H 0.1038(13) 0.2672(17) 0.5776(23) C2 C 0.0383(18) 0.1916(19) 0.7117(51) H3 H 0.0168(18) 0.2234(19) 0.8149(51) H4 H 0.0219(18) 0.2156(19) 0.6222(51) C3 C -0.0262(6) 0.0492(15) 0.7605(20) H5 H -0.0490(6) 0.0716(15) 0.8696(20) H6 H -0.0459(6) 0.0716(15) 0.6772(20) C4 C 0.1815(11) 0.1581(19) 0.4884(31) H7 H 0.1752(11) 0.2205(19) 0.4361(31) H8 H 0.2207(11) 0.1595(19) 0.5037(31) C5 C 0.1780(12) 0.0864(30) 0.3872(23) H9 H 0.2180(12) 0.0671(30) 0.3375(23) H10 H 0.1646(12) 0.1175(30) 0.2973(23) C6 C 0.1721(10) 0.0886(24) 0.8798(24) H11 H 0.1581(10) 0.1179(24) 0.9906(24) H12 H 0.2121(10) 0.0692(24) 0.8708(24) C7 C 0.1748(15) 0.1602(21) 0.7760(43) H13 H 0.2153(15) 0.1686(21) 0.7154(43) H14 H 0.1630(15) 0.2206(21) 0.8404(43) O1F O 0.0279(4) -0.0956(8) 0.7277(11) N1F N 0.1407(7) -0.1521(14) 0.6527(16) C1F C 0.0965(13) -0.2258(17) 0.6775(23) H1F H 0.1002(13) -0.2680(17) 0.7702(23) H2F H 0.1038(13) -0.2672(17) 0.5776(23) C2F C 0.0383(18) -0.1916(19) 0.7117(51) H3F H 0.0168(18) -0.2234(19) 0.8149(51) H4F H 0.0219(18) -0.2156(19) 0.6222(51) C3F C -0.0262(6) -0.0492(15) 0.7605(20) H5F H -0.0490(6) -0.0716(15) 0.8696(20) H6F H -0.0459(6) -0.0716(15) 0.6772(20) C4F C 0.1815(11) -0.1581(19) 0.4884(31) H7F H 0.1752(11) -0.2205(19) 0.4361(31) H8F H 0.2207(11) -0.1595(19) 0.5037(31) C5F C 0.1780(12) -0.0864(30) 0.3872(23) H9F H 0.2180(12) -0.0671(30) 0.3375(23) H10F H 0.1646(12) -0.1175(30) 0.2973(23) C6F C 0.1721(10) -0.0886(24) 0.8798(24) H11F H 0.1581(10) -0.1179(24) 0.9906(24) H12F H 0.2121(10) -0.0692(24) 0.8708(24) C7F C 0.1748(15) -0.1602(21) 0.7760(43) H13F H 0.2153(15) -0.1686(21) 0.7154(43) H14F H 0.1630(15) -0.2206(21) 0.8404(43) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 O1 2.126 1_555 1_555 O1 C2 1.313 1_555 1_555 O2 Li1 2.152 1_555 1_555 O3 Li1 2.133 1_555 1_555 N1 Li1 2.232 1_555 1_555 C1 N1 1.420 1_555 1_555 H1 C1 0.971 1_555 1_555 H2 C1 0.970 1_555 1_555 C2 C1 1.416 1_555 1_555 H3 C2 0.971 1_555 1_555 H4 C2 0.970 1_555 1_555 C3 O1 1.392 1_555 1_555 H5 C3 0.970 1_555 1_555 H6 C3 0.969 1_555 1_555 C4 N1 1.451 1_555 1_555 H7 C4 0.971 1_555 1_555 H8 C4 0.971 1_555 1_555 C5 O2 1.346 1_555 1_555 H9 C5 0.969 1_555 1_555 H10 C5 0.969 1_555 1_555 C6 O3 1.391 1_555 1_555 H11 C6 0.970 1_555 1_555 H12 C6 0.970 1_555 1_555 C7 N1 1.452 1_555 1_555 H13 C7 0.971 1_555 1_555 H14 C7 0.970 1_555 1_555 O1F Li1 2.126 1_555 1_555 N1F Li1 2.232 1_555 1_555 C1F N1F 1.420 1_555 1_555 H1F C1F 0.971 1_555 1_555 H2F C1F 0.970 1_555 1_555 C2F O1F 1.313 1_555 1_555 H3F C2F 0.971 1_555 1_555 H4F C2F 0.970 1_555 1_555 C3F C3 1.322 1_555 1_555 H5F C3F 0.970 1_555 1_555 H6F C3F 0.969 1_555 1_555 C4F N1F 1.451 1_555 1_555 H7F C4F 0.971 1_555 1_555 H8F C4F 0.971 1_555 1_555 C5F O2 1.346 1_555 1_555 H9F C5F 0.969 1_555 1_555 H10F C5F 0.969 1_555 1_555 C6F O3 1.391 1_555 1_555 H11F C6F 0.970 1_555 1_555 H12F C6F 0.970 1_555 1_555 C7F N1F 1.452 1_555 1_555 H13F C7F 0.971 1_555 1_555 H14F C7F 0.970 1_555 1_555 C4 C5 1.289 1_555 1_555 C6 C7 1.276 1_555 1_555 O1F C3F 1.392 1_555 1_555 C1F C2F 1.416 1_555 1_555 C4F C5F 1.289 1_555 1_555 C6F C7F 1.276 1_555 1_555 #END data_CSD_CIF_RESYAP _audit_creation_date 1997-10-02 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD RESYAP _database_code_depnum_ccdc_fiz 'CSD 406754' _chemical_formula_sum 'C52 H60 Li1 N9 O1' _chemical_formula_moiety ; C32 H16 Li1 N8 1-,C16 H36 N1 1+,C4 H8 O1 ; _journal_coden_Cambridge 29 _journal_volume 623 _journal_year 1997 _journal_page_first 1281 _journal_name_full 'Z.Anorg.Allg.Chem. ' loop_ _publ_author_name "B.Latte" "B.Assmann" "H.Homborg" _chemical_name_systematic ; Tetra-n-butylammonium (phthalocyaninato)-lithium tetrahydrofuran solvate ; _cell_volume 4679.548 _exptl_crystal_colour 'blue' _exptl_crystal_density_diffrn 1.184 _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_gt 0.0634 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x,1/2-y,1/2+z 3 -x,-y,-z 4 -x,-1/2+y,-1/2-z _cell_length_a 12.455(5) _cell_length_b 23.396(5) _cell_length_c 16.120(5) _cell_angle_alpha 90 _cell_angle_beta 94.986(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.28 N 0.68 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.4681(5) 0.1156(3) 0.1537(4) N1 N 0.3229(2) 0.13350(11) 0.1046(2) N2 N 0.4059(2) 0.06366(11) 0.2329(2) N3 N 0.6124(2) 0.10030(11) 0.2087(2) N4 N 0.5269(2) 0.17517(11) 0.0862(2) N5 N 0.3638(2) 0.20986(11) 0.0103(2) N6 N 0.7160(2) 0.16726(12) 0.1336(2) N7 N 0.5684(2) 0.03351(11) 0.3152(2) N8 N 0.2170(2) 0.07069(11) 0.1844(2) N9 N 0.4648(2) 0.33362(12) 0.2409(2) C1 C 0.2294(3) 0.10917(14) 0.1248(2) C2 C 0.1374(3) 0.13327(14) 0.0743(2) C3 C 0.0273(3) 0.1238(2) 0.0706(2) H1 H -0.0013(3) 0.0959(2) 0.1033(2) C4 C -0.0383(3) 0.1569(2) 0.0168(3) H2 H -0.1125(3) 0.1512(2) 0.0135(3) C5 C 0.0033(3) 0.1989(2) -0.0326(2) H3 H -0.0432(3) 0.2205(2) -0.0684(2) C6 C 0.1137(3) 0.2088(2) -0.0290(2) H4 H 0.1419(3) 0.2369(2) -0.0616(2) C7 C 0.1802(3) 0.17556(14) 0.0245(2) C8 C 0.2963(3) 0.17407(14) 0.0451(2) C9 C 0.4707(3) 0.20929(14) 0.0303(2) C10 C 0.5437(3) 0.24812(14) -0.0088(2) C11 C 0.5268(3) 0.29194(14) -0.0670(2) H5 H 0.4578(3) 0.30204(14) -0.0887(2) C12 C 0.6172(3) 0.3199(2) -0.0914(2) H6 H 0.6085(3) 0.3484(2) -0.1316(2) C13 C 0.7201(3) 0.3064(2) -0.0574(2) H7 H 0.7787(3) 0.3265(2) -0.0746(2) C14 C 0.7372(3) 0.26355(15) 0.0019(2) H8 H 0.8062(3) 0.25449(15) 0.0249(2) C15 C 0.6470(3) 0.23466(14) 0.0256(2) C16 C 0.6332(3) 0.18881(14) 0.0859(2) C17 C 0.7045(3) 0.12734(14) 0.1910(2) C18 C 0.7944(3) 0.10870(15) 0.2485(2) C19 C 0.9019(3) 0.1244(2) 0.2599(2) H9 H 0.9301(3) 0.1516(2) 0.2258(2) C20 C 0.9658(3) 0.0988(2) 0.3231(2) H10 H 1.0383(3) 0.1088(2) 0.3315(2) C21 C 0.9239(3) 0.0580(2) 0.3750(2) H11 H 0.9689(3) 0.0409(2) 0.4169(2) C22 C 0.8165(3) 0.0428(2) 0.3648(2) H12 H 0.7882(3) 0.0164(2) 0.4001(2) C23 C 0.7518(3) 0.06803(14) 0.3007(2) C24 C 0.6368(3) 0.06479(14) 0.2741(2) C25 C 0.4615(3) 0.03500(13) 0.2960(2) C26 C 0.3869(3) 0.00256(13) 0.3434(2) C27 C 0.4022(3) -0.03113(15) 0.4149(2) H13 H 0.4706(3) -0.03723(15) 0.4414(2) C28 C 0.3122(3) -0.0549(2) 0.4445(2) H14 H 0.3198(3) -0.0774(2) 0.4923(2) C29 C 0.2099(3) -0.0462(2) 0.4046(2) H15 H 0.1508(3) -0.0635(2) 0.4257(2) C30 C 0.1939(3) -0.0122(2) 0.3341(2) H16 H 0.1255(3) -0.0060(2) 0.3077(2) C31 C 0.2854(3) 0.01239(14) 0.3046(2) C32 C 0.2989(3) 0.05147(14) 0.2351(2) C33 C 0.3786(3) 0.30079(14) 0.2821(2) H17 H 0.4026(3) 0.29571(14) 0.3404(2) H18 H 0.3136(3) 0.32384(14) 0.2792(2) C34 C 0.3503(3) 0.2427(2) 0.2448(2) H19 H 0.4125(3) 0.2177(2) 0.2528(2) H20 H 0.3315(3) 0.2466(2) 0.1854(2) C35 C 0.2560(3) 0.2163(2) 0.2856(2) H21 H 0.2543(3) 0.1756(2) 0.2743(2) H22 H 0.2680(3) 0.2213(2) 0.3454(2) C36 C 0.1482(3) 0.2414(2) 0.2565(3) H23 H 0.0930(3) 0.2229(2) 0.2846(3) H24 H 0.1345(3) 0.2358(2) 0.1975(3) H25 H 0.1483(3) 0.2816(2) 0.2687(3) C37 C 0.4781(3) 0.39151(14) 0.2833(2) H26 H 0.5285(3) 0.41398(14) 0.2542(2) H27 H 0.4092(3) 0.41109(14) 0.2773(2) C38 C 0.5171(4) 0.3900(2) 0.3742(3) H28 H 0.5737(4) 0.3617(2) 0.3834(3) H29 H 0.4582(4) 0.3792(2) 0.4065(3) C39 C 0.5597(5) 0.4477(2) 0.4025(4) H30 H 0.5788(5) 0.4679(2) 0.3534(4) H31 H 0.5002(5) 0.4684(2) 0.4234(4) C40 C 0.6362(8) 0.4519(3) 0.4550(7) H32 H 0.6520(8) 0.4916(3) 0.4653(7) H33 H 0.6980(8) 0.4335(3) 0.4353(7) H34 H 0.6188(8) 0.4340(3) 0.5057(7) C41 C 0.5693(3) 0.2991(2) 0.2506(2) H35 H 0.5837(3) 0.2888(2) 0.3088(2) H36 H 0.5582(3) 0.2638(2) 0.2193(2) C42 C 0.6683(3) 0.3284(2) 0.2226(2) H37 H 0.6623(3) 0.3313(2) 0.1624(2) H38 H 0.6736(3) 0.3668(2) 0.2454(2) C43 C 0.7684(3) 0.2948(2) 0.2517(3) H39 H 0.7738(3) 0.2925(2) 0.3120(3) H40 H 0.7610(3) 0.2562(2) 0.2301(3) C44 C 0.8696(4) 0.3202(2) 0.2250(4) H41 H 0.9299(4) 0.2971(2) 0.2453(4) H42 H 0.8784(4) 0.3582(2) 0.2473(4) H43 H 0.8656(4) 0.3218(2) 0.1653(4) C45 C 0.4339(3) 0.3429(2) 0.1488(2) H44 H 0.4884(3) 0.3668(2) 0.1269(2) H45 H 0.4358(3) 0.3062(2) 0.1209(2) C46 C 0.3254(3) 0.3697(2) 0.1261(2) H46 H 0.2699(3) 0.3473(2) 0.1496(2) H47 H 0.3241(3) 0.4079(2) 0.1493(2) C47 C 0.3024(4) 0.3725(2) 0.0330(3) H48 H 0.3525(4) 0.3992(2) 0.0111(3) H49 H 0.3160(4) 0.3352(2) 0.0098(3) C48 C 0.1923(5) 0.3900(3) 0.0042(3) H50 H 0.1844(5) 0.3908(3) -0.0555(3) H51 H 0.1785(5) 0.4274(3) 0.0254(3) H52 H 0.1419(5) 0.3633(3) 0.0241(3) O1 O 0.2118(3) 0.4183(2) 0.3099(2) C49 C 0.1029(4) 0.4216(2) 0.2878(4) H53 H 0.0705(4) 0.3841(2) 0.2919(4) H54 H 0.0903(4) 0.4346(2) 0.2307(4) C50 C 0.0553(4) 0.4607(3) 0.3421(4) H55 H -0.0004(4) 0.4414(3) 0.3701(4) H56 H 0.0223(4) 0.4922(3) 0.3101(4) C51 C 0.1383(4) 0.4822(2) 0.4032(3) H57 H 0.1226(4) 0.4723(2) 0.4593(3) H58 H 0.1454(4) 0.5234(2) 0.3990(3) C52 C 0.2382(4) 0.4524(2) 0.3799(3) H59 H 0.2920(4) 0.4804(2) 0.3677(3) H60 H 0.2678(4) 0.4290(2) 0.4259(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 N1 1.955 1_555 1_555 N1 C1 1.361 1_555 1_555 N2 Li1 1.969 1_555 1_555 N3 Li1 1.967 1_555 1_555 N4 Li1 1.950 1_555 1_555 N5 C8 1.343 1_555 1_555 N6 C16 1.331 1_555 1_555 N7 C24 1.341 1_555 1_555 N8 C1 1.335 1_555 1_555 N9 C33 1.519 1_555 1_555 C1 C2 1.460 1_555 1_555 C2 C3 1.385 1_555 1_555 C3 H1 0.929 1_555 1_555 C4 C3 1.377 1_555 1_555 H2 C4 0.931 1_555 1_555 C5 C4 1.393 1_555 1_555 H3 C5 0.930 1_555 1_555 C6 C5 1.391 1_555 1_555 H4 C6 0.929 1_555 1_555 C7 C2 1.408 1_555 1_555 C8 N1 1.369 1_555 1_555 C9 N4 1.353 1_555 1_555 C10 C9 1.466 1_555 1_555 C11 C10 1.393 1_555 1_555 H5 C11 0.930 1_555 1_555 C12 C11 1.388 1_555 1_555 H6 C12 0.930 1_555 1_555 C13 C12 1.386 1_555 1_555 H7 C13 0.931 1_555 1_555 C14 C13 1.389 1_555 1_555 H8 C14 0.930 1_555 1_555 C15 C10 1.392 1_555 1_555 C16 N4 1.362 1_555 1_555 C17 N3 1.362 1_555 1_555 C18 C17 1.457 1_555 1_555 C19 C18 1.385 1_555 1_555 H9 C19 0.930 1_555 1_555 C20 C19 1.374 1_555 1_555 H10 C20 0.931 1_555 1_555 C21 C20 1.400 1_555 1_555 H11 C21 0.930 1_555 1_555 C22 C21 1.380 1_555 1_555 H12 C22 0.930 1_555 1_555 C23 C18 1.404 1_555 1_555 C24 N3 1.356 1_555 1_555 C25 N2 1.357 1_555 1_555 C26 C25 1.465 1_555 1_555 C27 C26 1.396 1_555 1_555 H13 C27 0.930 1_555 1_555 C28 C27 1.373 1_555 1_555 H14 C28 0.931 1_555 1_555 C29 C28 1.391 1_555 1_555 H15 C29 0.930 1_555 1_555 C30 C29 1.387 1_555 1_555 H16 C30 0.930 1_555 1_555 C31 C26 1.380 1_555 1_555 C32 N2 1.366 1_555 1_555 C33 H17 0.968 1_555 1_555 H18 C33 0.970 1_555 1_555 C34 C33 1.515 1_555 1_555 H19 C34 0.970 1_555 1_555 H20 C34 0.970 1_555 1_555 C35 C34 1.526 1_555 1_555 H21 C35 0.969 1_555 1_555 H22 C35 0.970 1_555 1_555 C36 C35 1.503 1_555 1_555 H23 C36 0.959 1_555 1_555 H24 C36 0.961 1_555 1_555 H25 C36 0.961 1_555 1_555 C37 N9 1.520 1_555 1_555 H26 C37 0.970 1_555 1_555 H27 C37 0.970 1_555 1_555 C38 C37 1.504 1_555 1_555 H28 C38 0.969 1_555 1_555 H29 C38 0.969 1_555 1_555 C39 C38 1.507 1_555 1_555 H30 C39 0.969 1_555 1_555 H31 C39 0.970 1_555 1_555 C40 C39 1.222 1_555 1_555 H32 C40 0.961 1_555 1_555 H33 C40 0.960 1_555 1_555 H34 C40 0.960 1_555 1_555 C41 N9 1.528 1_555 1_555 H35 C41 0.970 1_555 1_555 H36 C41 0.971 1_555 1_555 C42 C41 1.514 1_555 1_555 H37 C42 0.969 1_555 1_555 H38 C42 0.971 1_555 1_555 C43 C42 1.514 1_555 1_555 H39 C43 0.970 1_555 1_555 H40 C43 0.969 1_555 1_555 C44 C43 1.490 1_555 1_555 H41 C44 0.959 1_555 1_555 H42 C44 0.962 1_555 1_555 H43 C44 0.960 1_555 1_555 C45 N9 1.517 1_555 1_555 H44 C45 0.969 1_555 1_555 H45 C45 0.971 1_555 1_555 C46 C45 1.506 1_555 1_555 H46 C46 0.970 1_555 1_555 H47 C46 0.969 1_555 1_555 C47 C46 1.505 1_555 1_555 H48 C47 0.971 1_555 1_555 H49 C47 0.970 1_555 1_555 C48 C47 1.467 1_555 1_555 H50 C48 0.959 1_555 1_555 H51 C48 0.960 1_555 1_555 H52 C48 0.960 1_555 1_555 O1 C49 1.374 1_555 1_555 C49 H53 0.970 1_555 1_555 H54 C49 0.969 1_555 1_555 C50 C49 1.430 1_555 1_555 H55 C50 0.971 1_555 1_555 H56 C50 0.970 1_555 1_555 C51 C50 1.454 1_555 1_555 H57 C51 0.970 1_555 1_555 H58 C51 0.971 1_555 1_555 C52 O1 1.398 1_555 1_555 H59 C52 0.969 1_555 1_555 H60 C52 0.968 1_555 1_555 N5 C9 1.342 1_555 1_555 N6 C17 1.331 1_555 1_555 N7 C25 1.341 1_555 1_555 N8 C32 1.329 1_555 1_555 C6 C7 1.382 1_555 1_555 C7 C8 1.456 1_555 1_555 C14 C15 1.393 1_555 1_555 C15 C16 1.468 1_555 1_555 C22 C23 1.386 1_555 1_555 C23 C24 1.461 1_555 1_555 C30 C31 1.396 1_555 1_555 C31 C32 1.467 1_555 1_555 C51 C52 1.502 1_555 1_555 #END data_CSD_CIF_RESYET _audit_creation_date 1997-10-02 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD RESYET _database_code_depnum_ccdc_fiz 'CSD 406755' _chemical_formula_sum 'C64 H89 F1 Li1 N10 O0.5' _chemical_formula_moiety ; C32 H16 Li1 N8 1-,2(C16 H36 N1 1+),F1 1-,0.5(H2 O1) ; _journal_coden_Cambridge 29 _journal_volume 623 _journal_year 1997 _journal_page_first 1281 _journal_name_full 'Z.Anorg.Allg.Chem. ' loop_ _publ_author_name "B.Latte" "B.Assmann" "H.Homborg" _chemical_name_systematic ; bis(Tetra-n-butylammonium) phthalocyaninato-lithium fluoride hemihydrate ; _cell_volume 1553.402 _exptl_crystal_colour 'blue' _exptl_crystal_density_diffrn 1.103 _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; _refine_special_details ; The F anion and the hydrate are disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.1327 _refine_ls_wR_factor_gt 0.1327 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 8.648(1) _cell_length_b 12.620(2) _cell_length_c 14.866(5) _cell_angle_alpha 82.44(2) _cell_angle_beta 87.01(2) _cell_angle_gamma 75.020(12) _cell_formula_units_Z 1 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 F 0.64 Li 1.29 N 0.68 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 1.00000 0.00000 0.00000 N1 N 1.1456(12) -0.1379(8) 0.0586(6) N2 N 1.0605(11) -0.0497(7) -0.1194(6) N3 N 1.2358(12) -0.2284(8) -0.0750(6) N4 N 1.0901(12) -0.1109(8) 0.2172(6) C1 C 1.1557(14) -0.1705(10) 0.1500(8) C2 C 1.2414(14) -0.2862(9) 0.1658(7) C3 C 1.2775(14) -0.3577(11) 0.2436(8) H1 H 1.2508(14) -0.3336(11) 0.3002(8) C4 C 1.3554(16) -0.4680(12) 0.2360(8) H2 H 1.3830(16) -0.5179(12) 0.2880(8) C5 C 1.3924(16) -0.5037(11) 0.1494(9) H3 H 1.4445(16) -0.5773(11) 0.1452(9) C6 C 1.3522(15) -0.4308(12) 0.0698(8) H4 H 1.3740(15) -0.4544(12) 0.0128(8) C7 C 1.2777(14) -0.3209(11) 0.0803(8) C8 C 1.2190(15) -0.2253(10) 0.0148(8) C9 C 1.1660(14) -0.1450(9) -0.1369(7) C10 C 1.1894(15) -0.1475(10) -0.2333(7) C11 C 1.2900(16) -0.2259(11) -0.2840(8) H5 H 1.3592(16) -0.2901(11) -0.2572(8) C12 C 1.2770(19) -0.1990(14) -0.3779(9) H6 H 1.3396(19) -0.2487(14) -0.4144(9) C13 C 1.1767(20) -0.1027(14) -0.4206(10) H7 H 1.1731(20) -0.0895(14) -0.4836(10) C14 C 1.0818(15) -0.0264(11) -0.3677(8) H8 H 1.0149(15) 0.0387(11) -0.3949(8) C15 C 1.0885(15) -0.0489(10) -0.2738(8) C16 C 1.0094(15) 0.0093(10) -0.2006(7) N5 N 0.7250(12) -0.2596(8) 0.2511(6) C17 C 0.7593(14) -0.1942(11) 0.1629(7) H9 H 0.7524(14) -0.1193(11) 0.1748(7) H10 H 0.8689(14) -0.2259(11) 0.1444(7) C18 C 0.6533(16) -0.1881(11) 0.0847(9) H11 H 0.5452(16) -0.1470(11) 0.0983(9) H12 H 0.6502(16) -0.2621(11) 0.0751(9) C19 C 0.7163(18) -0.1319(12) -0.0002(8) H13 H 0.8273(18) -0.1701(12) -0.0102(8) H14 H 0.7129(18) -0.0567(12) 0.0089(8) C20 C 0.6216(20) -0.1298(13) -0.0845(10) H15 H 0.6666(20) -0.0932(13) -0.1361(10) H16 H 0.512(2) -0.0907(13) -0.0757(10) H17 H 0.6266(20) -0.2041(13) -0.0949(10) C21 C 0.5585(15) -0.2042(11) 0.2875(8) H18 H 0.4798(15) -0.2032(11) 0.2430(8) H19 H 0.5356(15) -0.2491(11) 0.3422(8) C22 C 0.5376(16) -0.0859(11) 0.3094(9) H20 H 0.6197(16) -0.0845(11) 0.3509(9) H21 H 0.5491(16) -0.0381(11) 0.2541(9) C23 C 0.3818(18) -0.0466(13) 0.3499(11) H22 H 0.3722(18) -0.0952(13) 0.4050(11) H23 H 0.3012(18) -0.0508(13) 0.3085(11) C24 C 0.3482(20) 0.0694(13) 0.3726(12) H24 H 0.2426(20) 0.0900(13) 0.3990(12) H25 H 0.3549(20) 0.1185(13) 0.3183(12) H26 H 0.4254(20) 0.0741(13) 0.4150(12) C25 C 0.8565(16) -0.2622(11) 0.3193(8) H27 H 0.9587(16) -0.3033(11) 0.2967(8) H28 H 0.8635(16) -0.1871(11) 0.3214(8) C26 C 0.8292(17) -0.3129(12) 0.4149(8) H29 H 0.7284(17) -0.2721(12) 0.4393(8) H30 H 0.8245(17) -0.3889(12) 0.4146(8) C27 C 0.9658(20) -0.3093(14) 0.4732(9) H31 H 0.9722(20) -0.2333(14) 0.4706(9) H32 H 1.0655(20) -0.3513(14) 0.4486(9) C28 C 0.9471(23) -0.3554(13) 0.5716(10) H33 H 1.0366(23) -0.3513(13) 0.6054(10) H34 H 0.9429(23) -0.4310(13) 0.5748(10) H35 H 0.8499(23) -0.3129(13) 0.5969(10) C29 C 0.7261(17) -0.3786(10) 0.2385(9) H36 H 0.7047(17) -0.417(1) 0.2969(9) H37 H 0.6398(17) -0.3765(10) 0.1986(9) C30 C 0.8821(19) -0.4442(12) 0.1995(11) H38 H 0.9099(19) -0.4030(12) 0.1440(11) H39 H 0.9670(19) -0.4543(12) 0.2423(11) C31 C 0.8693(21) -0.5508(15) 0.1805(13) H40 H 0.7839(21) -0.5402(15) 0.1378(13) H41 H 0.8406(21) -0.5914(15) 0.2362(13) C32 C 1.0186(25) -0.6170(16) 0.1427(19) H42 H 1.0033(25) -0.6866(16) 0.1311(19) H43 H 1.1030(25) -0.6296(16) 0.1853(19) H44 H 1.0467(25) -0.5779(16) 0.0870(19) F1 F 1.50000 -0.50000 0.50000 F2? F 0.4468(37) -0.3901(23) 0.4537(19) O1? O 0.4468(37) -0.3901(23) 0.4537(19) F3? F 0.6070(32) -0.5189(21) 0.4231(17) O2? O 0.6070(32) -0.5189(21) 0.4231(17) F4? F 1.3996(49) -0.5532(32) 0.4546(26) O3 O 1.3996(49) -0.5532(32) 0.4546(26) C16A C 0.9906(15) -0.0093(10) 0.2006(7) N2A N 0.9395(11) 0.0497(7) 0.1194(6) N1A N 0.8544(12) 0.1379(8) -0.0586(6) C1A C 0.8443(14) 0.1705(10) -0.1500(8) N4A N 0.9099(12) 0.1109(8) -0.2172(6) C2A C 0.7586(14) 0.2862(9) -0.1658(7) C3A C 0.7225(14) 0.3577(11) -0.2436(8) H1A H 0.7492(14) 0.3336(11) -0.3002(8) C4A C 0.6446(16) 0.4680(12) -0.2360(8) H2A H 0.6170(16) 0.5179(12) -0.2880(8) C5A C 0.6076(16) 0.5037(11) -0.1494(9) H3A H 0.5555(16) 0.5773(11) -0.1452(9) C6A C 0.6478(15) 0.4308(12) -0.0698(8) H4A H 0.6260(15) 0.4544(12) -0.0128(8) C7A C 0.7223(14) 0.3209(11) -0.0803(8) C8A C 0.7810(15) 0.2253(10) -0.0148(8) N3A N 0.7642(12) 0.2284(8) 0.0750(6) C9A C 0.8340(14) 0.1450(9) 0.1369(7) C10A C 0.8106(15) 0.1475(10) 0.2333(7) C11A C 0.7100(16) 0.2259(11) 0.2840(8) H5A H 0.6408(16) 0.2901(11) 0.2572(8) C12A C 0.7230(19) 0.1990(14) 0.3779(9) H6A H 0.6604(19) 0.2487(14) 0.4144(9) C13A C 0.8233(20) 0.1027(14) 0.4206(10) H7A H 0.8269(20) 0.0895(14) 0.4836(10) C14A C 0.9182(15) 0.0264(11) 0.3677(8) H8A H 0.9851(15) -0.0387(11) 0.3949(8) C15A C 0.9115(15) 0.0489(10) 0.2738(8) O3A O 1.6004(49) -0.4468(32) 0.5454(26) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 N1 1.989 1_555 1_555 N1 C1 1.367 1_555 1_555 N2 Li1 1.961 1_555 1_555 N3 C8 1.340 1_555 1_555 N4 C1 1.343 1_555 1_555 C1 C2 1.451 1_555 1_555 C2 C3 1.366 1_555 1_555 C3 H1 0.930 1_555 1_555 C4 C3 1.397 1_555 1_555 H2 C4 0.930 1_555 1_555 C5 C4 1.413 1_555 1_555 H3 C5 0.930 1_555 1_555 C6 C5 1.400 1_555 1_555 H4 C6 0.929 1_555 1_555 C7 C2 1.393 1_555 1_555 C8 N1 1.352 1_555 1_555 C9 N2 1.355 1_555 1_555 C10 C9 1.440 1_555 1_555 C11 C10 1.410 1_555 1_555 H5 C11 0.929 1_555 1_555 C12 C11 1.396 1_555 1_555 H6 C12 0.930 1_555 1_555 C13 C12 1.393 1_555 1_555 H7 C13 0.930 1_555 1_555 C14 C13 1.394 1_555 1_555 H8 C14 0.930 1_555 1_555 C15 C10 1.403 1_555 1_555 C16 N2 1.362 1_555 1_555 N5 C17 1.513 1_555 1_555 C17 H9 0.971 1_555 1_555 H10 C17 0.969 1_555 1_555 C18 C17 1.500 1_555 1_555 H11 C18 0.970 1_555 1_555 H12 C18 0.970 1_555 1_555 C19 C18 1.512 1_555 1_555 H13 C19 0.970 1_555 1_555 H14 C19 0.969 1_555 1_555 C20 C19 1.526 1_555 1_555 H15 C20 0.960 1_555 1_555 H16 C20 0.960 1_555 1_555 H17 C20 0.960 1_555 1_555 C21 N5 1.534 1_555 1_555 H18 C21 0.970 1_555 1_555 H19 C21 0.970 1_555 1_555 C22 C21 1.533 1_555 1_555 H20 C22 0.970 1_555 1_555 H21 C22 0.970 1_555 1_555 C23 C22 1.440 1_555 1_555 H22 C23 0.970 1_555 1_555 H23 C23 0.969 1_555 1_555 C24 C23 1.497 1_555 1_555 H24 C24 0.960 1_555 1_555 H25 C24 0.960 1_555 1_555 H26 C24 0.960 1_555 1_555 C25 N5 1.554 1_555 1_555 H27 C25 0.970 1_555 1_555 H28 C25 0.970 1_555 1_555 C26 C25 1.513 1_555 1_555 H29 C26 0.970 1_555 1_555 H30 C26 0.971 1_555 1_555 C27 C26 1.514 1_555 1_555 H31 C27 0.971 1_555 1_555 H32 C27 0.970 1_555 1_555 C28 C27 1.518 1_555 1_555 H33 C28 0.960 1_555 1_555 H34 C28 0.959 1_555 1_555 H35 C28 0.961 1_555 1_555 C29 N5 1.535 1_555 1_555 H36 C29 0.970 1_555 1_555 H37 C29 0.970 1_555 1_555 C30 C29 1.519 1_555 1_555 H38 C30 0.969 1_555 1_555 H39 C30 0.969 1_555 1_555 C31 C30 1.443 1_555 1_555 H40 C31 0.970 1_555 1_555 H41 C31 0.971 1_555 1_555 C32 C31 1.473 1_555 1_555 H42 C32 0.960 1_555 1_555 H43 C32 0.960 1_555 1_555 H44 C32 0.960 1_555 1_555 C16A N4 1.347 1_555 1_555 N2A Li1 1.961 1_555 1_555 N1A Li1 1.989 1_555 1_555 C1A N1A 1.367 1_555 1_555 N4A C16 1.347 1_555 1_555 C2A C1A 1.451 1_555 1_555 C3A C2A 1.366 1_555 1_555 H1A C3A 0.930 1_555 1_555 C4A C3A 1.397 1_555 1_555 H2A C4A 0.930 1_555 1_555 C5A C4A 1.413 1_555 1_555 H3A C5A 0.930 1_555 1_555 C6A C5A 1.400 1_555 1_555 H4A C6A 0.929 1_555 1_555 C7A C2A 1.393 1_555 1_555 C8A N1A 1.352 1_555 1_555 N3A C8A 1.340 1_555 1_555 C9A N2A 1.355 1_555 1_555 C10A C9A 1.440 1_555 1_555 C11A C10A 1.410 1_555 1_555 H5A C11A 0.929 1_555 1_555 C12A C11A 1.396 1_555 1_555 H6A C12A 0.930 1_555 1_555 C13A C12A 1.393 1_555 1_555 H7A C13A 0.930 1_555 1_555 C14A C13A 1.394 1_555 1_555 H8A C14A 0.930 1_555 1_555 C15A C16A 1.437 1_555 1_555 N3 C9 1.339 1_555 1_555 C6 C7 1.396 1_555 1_555 C7 C8 1.445 1_555 1_555 C14 C15 1.389 1_555 1_555 C15 C16 1.437 1_555 1_555 C16A N2A 1.362 1_555 1_555 C1A N4A 1.343 1_555 1_555 C6A C7A 1.396 1_555 1_555 C7A C8A 1.445 1_555 1_555 N3A C9A 1.339 1_555 1_555 C10A C15A 1.403 1_555 1_555 C14A C15A 1.389 1_555 1_555 #END data_CSD_CIF_ROGDEW _audit_creation_date 1998-01-15 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD ROGDEW _chemical_formula_sum 'C14 H28 Li1 N2 Na1 O4' _chemical_formula_moiety ; C14 H28 Li1 N2 O4 1+,Na1 1- ; _journal_coden_Cambridge 4 _journal_volume 119 _journal_year 1997 _journal_page_first 3765 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "R.H.Huang" "M.J.Wagner" "D.J.Gilbert" "K.A.Reidy-Cedergren" "D.L.Ward" "M.K.Faber" "J.L.Dye" _chemical_name_systematic ; Cryptand(2.1.1)-lithium sodide ; _cell_volume 2125.280 _diffrn_ambient_temperature 200 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_gt 0.032 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,1/2+z 3 1/2-x,1/2+y,1/2+z 4 1/2+x,1/2-y,z _cell_length_a 9.639(5) _cell_length_b 22.924(17) _cell_length_c 9.6182(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.23 N 0.68 Na 0.97 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 0.95240 0.61867 0.46197 O1 O 0.50330 0.30502 0.27135 O2 O 0.34830 0.43598 0.43537 O3 O 0.69238 0.41491 0.46576 O4 O 0.57431 0.33185 0.61320 N1 N 0.54857 0.42310 0.22458 N2 N 0.31762 0.31797 0.49361 C1 C 0.56996 0.37939 0.11566 C2 C 0.47862 0.32707 0.13378 C3 C 0.41337 0.25758 0.30654 C4 C 0.28320 0.28063 0.37575 C5 C 0.20881 0.36013 0.52697 C6 C 0.21090 0.41118 0.42851 C7 C 0.37066 0.48196 0.33989 C8 C 0.42273 0.45876 0.20204 C9 C 0.67238 0.46002 0.24717 C10 C 0.77016 0.42932 0.34621 C11 C 0.77364 0.38658 0.57052 C12 C 0.67530 0.36700 0.68016 C13 C 0.46260 0.31669 0.70430 C14 C 0.35868 0.28376 0.61877 Li1 Li 0.50400 0.37115 0.42304 H1 H 0.66399 0.36704 0.11825 H2 H 0.55073 0.39663 0.02793 H3 H 0.38405 0.33798 0.12399 H4 H 0.50096 0.29822 0.06649 H5 H 0.46003 0.23200 0.36861 H6 H 0.38891 0.23699 0.22440 H7 H 0.23096 0.30239 0.30994 H8 H 0.23053 0.24846 0.40872 H9 H 0.22262 0.37399 0.61901 H10 H 0.18163 0.34114 0.51839 H11 H 0.19178 0.39833 0.33657 H12 H 0.14383 0.43935 0.45553 H13 H 0.43737 0.50812 0.37724 H14 H 0.28572 0.50205 0.32521 H15 H 0.35283 0.43538 0.16030 H16 H 0.44439 0.49053 0.14244 H17 H 0.64496 0.49636 0.28588 H18 H 0.71792 0.46651 0.16095 H19 H 0.80591 0.39495 0.30427 H20 H 0.84466 0.45446 0.37049 H21 H 0.83927 0.41309 0.60846 H22 H 0.82089 0.35400 0.53200 H23 H 0.72304 0.34491 0.74867 H24 H 0.63227 0.39972 0.72275 H25 H 0.42151 0.35099 0.74143 H26 H 0.49555 0.29291 0.77815 H27 H 0.39842 0.24782 0.58987 H28 H 0.27871 0.27628 0.67367 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 O1 C2 1.436 1_555 1_555 O2 C6 1.443 1_555 1_555 O3 C10 1.412 1_555 1_555 O4 C12 1.418 1_555 1_555 N1 C1 1.464 1_555 1_555 N2 C4 1.459 1_555 1_555 C1 C2 1.498 1_555 1_555 C2 H3 0.950 1_555 1_555 C3 O1 1.431 1_555 1_555 C4 C3 1.515 1_555 1_555 C5 N2 1.462 1_555 1_555 C6 C5 1.506 1_555 1_555 C7 O2 1.415 1_555 1_555 C8 N1 1.479 1_555 1_555 C9 N1 1.479 1_555 1_555 C10 C9 1.514 1_555 1_555 C11 O3 1.432 1_555 1_555 C12 C11 1.487 1_555 1_555 C13 O4 1.431 1_555 1_555 C14 N2 1.490 1_555 1_555 Li1 O1 2.104 1_555 1_555 H1 C1 0.950 1_555 1_555 H2 C1 0.950 1_555 1_555 H4 C2 0.950 1_555 1_555 H5 C3 0.950 1_555 1_555 H6 C3 0.950 1_555 1_555 H7 C4 0.950 1_555 1_555 H8 C4 0.950 1_555 1_555 H9 C5 0.950 1_555 1_555 H10 C5 0.515 1_555 1_555 H11 C6 0.950 1_555 1_555 H12 C6 0.950 1_555 1_555 H13 C7 0.950 1_555 1_555 H14 C7 0.950 1_555 1_555 H15 C8 0.950 1_555 1_555 H16 C8 0.950 1_555 1_555 H17 C9 0.950 1_555 1_555 H18 C9 0.950 1_555 1_555 H19 C10 0.950 1_555 1_555 H20 C10 0.950 1_555 1_555 H21 C11 0.950 1_555 1_555 H22 C11 0.950 1_555 1_555 H23 C12 0.950 1_555 1_555 H24 C12 0.950 1_555 1_555 H25 C13 0.950 1_555 1_555 H26 C13 0.950 1_555 1_555 H27 C14 0.950 1_555 1_555 H28 C14 0.950 1_555 1_555 O2 Li1 2.115 1_555 1_555 O3 Li1 2.115 1_555 1_555 O4 Li1 2.149 1_555 1_555 N1 Li1 2.291 1_555 1_555 N2 Li1 2.275 1_555 1_555 C7 C8 1.514 1_555 1_555 C13 C14 1.500 1_555 1_555 #END data_CSD_CIF_SIHHOH _audit_creation_date 2007-12-12 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD SIHHOH _database_code_depnum_ccdc_archive 'CCDC 637966' _chemical_formula_sum 'C89 H137 Li5 N24 O2 V4' _chemical_formula_moiety ; C66 H106 Li3 N24 V4 1+,C15 H15 Li2 1-,2(C4 H8 O1) ; _journal_coden_Cambridge 179 _journal_volume 46 _journal_year 2007 _journal_page_first 5425 _journal_name_full 'Angew.Chem.,Int.Ed. ' loop_ _publ_author_name "C.Fernandez-Cortabitarte" "F.Garcia" "J.V.Morey" "M.McPartlin" "S.Singh" "A.E.H.Wheatley" "D.S.Wright" _chemical_name_systematic ; tetrakis(\m~3~-\h^3^-3,4,7,8-tetrahydro-2H,6H-pyrimido[1,2-a]pyrimidin-1-yl)-t etrakis(\m~2~-3,4,7,8-tetrahydro-2H,6H-pyrimido[1,2-a]pyrimidin-1-yl)-bis(\m~2 ~-\h^5^,\h^5^-cyclopentadienyl)-tri-lithium-tetra-vanadium(ii) (\m~2~-\h^5^,\h^5^-cyclopentadienyl)-bis(\h^5^-cyclopentadienyl)-di-lithium tetrahydrofuran solvate ; _chemical_melting_point 493.15 _cell_volume 2315.304 _exptl_crystal_colour 'brown' _exptl_crystal_density_diffrn 1.301 _exptl_special_details ; magnetic properties ; _exptl_crystal_description 'plate' _diffrn_ambient_temperature 180 _refine_special_details ; The bridging cyclopentadienyl anion ligand is disordered by symmetry. Two cation C atoms are disordered with occupancies of 0.616:0.384 and 0.632:0.368. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_gt 0.0766 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 10.868(2) _cell_length_b 13.783(3) _cell_length_c 16.716(3) _cell_angle_alpha 105.75(3) _cell_angle_beta 103.41(3) _cell_angle_gamma 94.80(3) _cell_formula_units_Z 1 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.43 N 0.68 O 0.68 V 1.13 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z V1 V 0.12560(7) 0.30343(6) -0.28261(5) V2 V 0.28169(7) 0.34341(6) -0.19012(5) N1 N 0.2166(4) 0.3073(3) -0.3788(3) N2 N 0.3996(4) 0.3625(3) -0.2710(3) N3 N 0.0919(4) 0.4522(3) -0.2707(3) N4 N 0.2756(4) 0.4979(3) -0.1602(3) N5 N 0.0043(4) 0.2884(3) -0.2073(3) N6 N 0.1885(4) 0.3309(3) -0.0975(3) N7 N 0.1346(4) 0.1460(3) -0.3072(3) N8 N 0.3248(4) 0.1958(3) -0.2058(3) C1 C 0.1426(6) 0.2961(5) -0.4667(4) H1 H 0.05010 0.28370 -0.47030 H2 H 0.16260 0.23590 -0.50680 C2 C 0.1708(7) 0.3886(6) -0.4939(5) H3 H 0.14200 0.44770 -0.45830 H4 H 0.12400 0.37640 -0.55490 C3 C 0.3130(6) 0.4116(6) -0.4830(4) H5 H 0.33880 0.35830 -0.52620 H6 H 0.33390 0.47810 -0.49260 N9 N 0.3830(4) 0.4146(4) -0.3968(3) C4 C 0.51529(10) 0.46924(8) -0.36773(7) H7 H 0.56220 0.43820 -0.40990 H8 H 0.51320 0.54100 -0.36740 H9? H 0.51600 0.54330 -0.34320 H10? H 0.55380 0.45900 -0.41700 C5 C 0.58095(10) 0.46839(8) -0.28840(7) H11 H 0.61240 0.54070 -0.25430 H12? H 0.65770 0.43710 -0.29630 C6? C 0.59365(10) 0.42639(8) -0.29780(7) H13? H 0.60950 0.35730 -0.32600 H14 H 0.67770 0.47070 -0.26990 C7 C 0.52869(10) 0.42092(8) -0.23288(7) H15 H 0.52790 0.47510 -0.18020 H16 H 0.58720 0.37480 -0.21490 H17? H 0.52330 0.49090 -0.19920 H18? H 0.57880 0.38840 -0.19280 C8 C 0.33468(10) 0.36394(8) -0.34845(7) C9 C -0.01841(10) 0.47957(8) -0.32488(7) H19 H -0.08750 0.41990 -0.35060 H20 H 0.00710 0.49870 -0.37240 C10 C -0.0682(1) 0.56954(8) -0.27092(7) H21 H -0.14180 0.58810 -0.30800 H22 H -0.09710 0.55000 -0.22470 C11 C 0.04065(10) 0.66036(8) -0.23154(7) H23 H 0.05680 0.68910 -0.27700 H24 H 0.01650 0.71440 -0.18800 N10 N 0.15746(10) 0.62585(8) -0.19065(7) C12 C 0.25555(10) 0.71185(8) -0.13213(7) H25 H 0.22730 0.74300 -0.08000 H26 H 0.26580 0.76450 -0.16120 C13 C 0.38566(10) 0.67561(8) -0.10540(7) H27 H 0.42790 0.66440 -0.15290 H28 H 0.44300 0.72750 -0.05410 C14 C 0.35746(10) 0.57525(8) -0.08482(7) H29 H 0.43890 0.55080 -0.06530 H30 H 0.31490 0.58740 -0.03750 C15 C 0.17376(10) 0.52597(8) -0.20818(7) C16 C -0.13407(10) 0.28130(8) -0.23436(7) H31 H -0.16580 0.24430 -0.29670 H32 H -0.15740 0.35070 -0.22480 C17 C -0.19617(10) 0.22523(8) -0.18333(7) H33 H -0.29060 0.21760 -0.20350 H34 H -0.17160 0.15640 -0.19140 C18 C -0.15091(10) 0.28667(8) -0.08976(7) H35 H -0.19570 0.34670 -0.07950 H36 H -0.17200 0.24450 -0.05390 N11 N -0.01017(10) 0.32140(8) -0.06441(7) C19 C 0.04304(10) 0.36503(8) 0.02848(7) H37 H 0.04050 0.31050 0.05660 H38 H -0.00900 0.41570 0.05180 C20 C 0.18119(10) 0.41650(8) 0.04814(7) H39 H 0.18230 0.48280 0.03570 H40 H 0.22440 0.42960 0.10990 C21 C 0.25043(10) 0.34861(8) -0.00619(7) H41 H 0.34060 0.38090 0.00730 H42 H 0.24990 0.28270 0.00680 C22 C 0.05952(10) 0.31306(8) -0.12262(7) C23 C 0.01998(10) 0.07035(8) -0.35560(7) H43 H -0.05680 0.10410 -0.35440 H44 H 0.02230 0.04470 -0.41650 H45? H -0.00060 0.07150 -0.41620 H46? H -0.05210 0.09280 -0.33220 C24 C 0.01015(10) -0.00261(8) -0.32690(7) H47 H -0.04030 -0.05930 -0.37750 H48 H -0.04790 0.01530 -0.28930 C25? C 0.02525(10) -0.03921(8) -0.35600(7) H49? H -0.06280 -0.07340 -0.36490 H50? H 0.05650 -0.07460 -0.40560 C26 C 0.10351(10) -0.05068(8) -0.28073(7) H51 H 0.13140 -0.10540 -0.32150 H52 H 0.06690 -0.08070 -0.24220 H53? H 0.13820 -0.11530 -0.29690 H54? H 0.04860 -0.05850 -0.24250 N12 N 0.21141(10) 0.03052(8) -0.23046(7) C27 C 0.31454(10) 0.00439(8) -0.16822(7) H55 H 0.37260 -0.03220 -0.19900 H56 H 0.27660 -0.04130 -0.14070 C28 C 0.3891(1) 0.09970(8) -0.10044(7) H57 H 0.46400 0.08300 -0.06300 H58 H 0.33450 0.13150 -0.06410 C29 C 0.43426(10) 0.17432(8) -0.14599(7) H59 H 0.48020 0.23890 -0.10220 H60 H 0.49450 0.14430 -0.17830 C30 C 0.22219(10) 0.12255(8) -0.24753(7) C31 C -0.3447(5) -0.0670(4) -0.1838(4) H61 H -0.38510 -0.00860 -0.16900 C32 C -0.3516(5) -0.1519(5) -0.1514(3) H62 H -0.39740 -0.16030 -0.11120 C33 C -0.2780(6) -0.2221(3) -0.1898(4) H63 H -0.26590 -0.28560 -0.17980 C34 C -0.2257(5) -0.1805(4) -0.2459(3) H64 H -0.17240 -0.21140 -0.28000 C35 C -0.2669(5) -0.0847(3) -0.2422(3) H65 H -0.24610 -0.04020 -0.27340 C36 C 0.4719(8) 0.0590(6) -0.3627(3) H66 H 0.51670 0.03790 -0.31600 C37 C 0.5152(4) 0.1432(4) -0.3881(4) H67 H 0.59410 0.18820 -0.36150 C38 C 0.4199(6) 0.1482(4) -0.4604(4) H68 H 0.42380 0.19720 -0.49060 C39 C 0.3177(4) 0.0672(5) -0.4797(4) H69 H 0.24120 0.05250 -0.52500 C40 C 0.3498(7) 0.0121(4) -0.4193(5) H70 H 0.29860 -0.04600 -0.41710 C41 C -0.0590(14) 0.0620(13) 0.0211(11) H71 H -0.10730 0.11460 0.03790 C42 C -0.0573(15) -0.0252(18) 0.0476(9) H72 H -0.10280 -0.04190 0.08540 C43 C 0.0241(18) -0.084(1) 0.0083(12) H73 H 0.04310 -0.14810 0.01440 C44 C 0.0725(11) -0.0308(16) -0.0416(9) H74 H 0.13060 -0.05290 -0.07480 C45 C 0.0204(17) 0.0611(13) -0.0342(10) H75 H -0.03610 -0.11160 0.06110 O1 O 0.5867(7) 0.3185(6) -0.5440(6) C46 C 0.5588(10) 0.2564(7) -0.6221(8) H76 H 0.47770 0.26820 -0.65710 H77 H 0.54850 0.18470 -0.62130 C47 C 0.6686(13) 0.2776(9) -0.6601(6) H78 H 0.66150 0.33760 -0.68170 H79 H 0.67420 0.21770 -0.70710 C48 C 0.7850(9) 0.2993(9) -0.5783(8) H80 H 0.83630 0.24290 -0.58250 H81 H 0.84120 0.36440 -0.56750 C49 C 0.7127(9) 0.3051(9) -0.5115(6) H82 H 0.71240 0.24150 -0.49470 H83 H 0.75520 0.36290 -0.45950 Li1 Li -0.1490(11) -0.0725(9) -0.1054(8) Li2 Li 0.50000 0.00000 -0.50000 Li3 Li 0.3244(10) 0.1888(8) -0.3411(7) V1A V 0.87440(7) -0.30343(6) -0.71739(5) V2A V 0.71831(7) -0.34341(6) -0.80988(5) N1A N 0.7834(4) -0.3073(3) -0.6212(3) N2A N 0.6004(4) -0.3625(3) -0.7290(3) N3A N 0.9081(4) -0.4522(3) -0.7293(3) N4A N 0.7244(4) -0.4979(3) -0.8398(3) N5A N 0.9957(4) -0.2884(3) -0.7927(3) N6A N 0.8115(4) -0.3309(3) -0.9025(3) N7A N 0.8654(4) -0.1460(3) -0.6928(3) N8A N 0.6752(4) -0.1958(3) -0.7942(3) C1A C 0.8574(6) -0.2961(5) -0.5333(4) H1A H 0.94990 -0.28370 -0.52970 H2A H 0.83740 -0.23590 -0.49320 C2A C 0.8292(7) -0.3886(6) -0.5061(5) H3A H 0.85800 -0.44770 -0.54170 H4A H 0.87600 -0.37640 -0.44510 C3A C 0.6870(6) -0.4116(6) -0.5170(4) H5A H 0.66120 -0.35830 -0.47380 H6A H 0.66610 -0.47810 -0.50740 N9A N 0.6170(4) -0.4146(4) -0.6032(3) C4A C 0.48471(10) -0.46924(8) -0.63227(7) H7A H 0.43780 -0.43820 -0.59010 H8A H 0.48680 -0.54100 -0.63260 C5A C 0.41905(10) -0.46839(8) -0.71160(7) H11A H 0.38760 -0.54070 -0.74570 H14A H 0.32230 -0.47070 -0.73010 C7A C 0.47131(10) -0.42092(8) -0.76712(7) H15A H 0.47210 -0.47510 -0.81980 H16A H 0.41280 -0.37480 -0.78510 C8A C 0.66532(10) -0.36394(8) -0.65155(7) C9A C 1.01841(10) -0.47957(8) -0.67512(7) H19A H 1.08750 -0.41990 -0.64940 H20A H 0.99290 -0.49870 -0.62760 C10A C 1.0682(1) -0.56954(8) -0.72908(7) H21A H 1.14180 -0.58810 -0.69200 H22A H 1.09710 -0.55000 -0.77530 C11A C 0.95935(10) -0.66036(8) -0.76846(7) H23A H 0.94320 -0.68910 -0.72300 H24A H 0.98350 -0.71440 -0.81200 N10A N 0.84254(10) -0.62585(8) -0.80935(7) C12A C 0.74445(10) -0.71185(8) -0.86787(7) H25A H 0.77270 -0.74300 -0.92000 H26A H 0.73420 -0.76450 -0.83880 C13A C 0.61434(10) -0.67561(8) -0.89460(7) H27A H 0.57210 -0.66440 -0.84710 H28A H 0.55700 -0.72750 -0.94590 C14A C 0.64254(10) -0.57525(8) -0.91518(7) H29A H 0.56110 -0.55080 -0.93470 H30A H 0.68510 -0.58740 -0.96250 C15A C 0.82624(10) -0.52597(8) -0.79182(7) C16A C 1.13407(10) -0.28130(8) -0.76564(7) H31A H 1.16580 -0.24430 -0.70330 H32A H 1.15740 -0.35070 -0.77520 C17A C 1.19617(10) -0.22523(8) -0.81667(7) H33A H 1.29060 -0.21760 -0.79650 H34A H 1.17160 -0.15640 -0.80860 C18A C 1.15091(10) -0.28667(8) -0.91024(7) H35A H 1.19570 -0.34670 -0.92050 H36A H 1.17200 -0.24450 -0.94610 N11A N 1.01017(10) -0.32140(8) -0.93559(7) C19A C 0.95696(10) -0.36503(8) -1.02848(7) H37A H 0.95950 -0.31050 -1.05660 H38A H 1.00900 -0.41570 -1.05180 C20A C 0.81881(10) -0.41650(8) -1.04814(7) H39A H 0.81770 -0.48280 -1.03570 H40A H 0.77560 -0.42960 -1.10990 C21A C 0.74957(10) -0.34861(8) -0.99381(7) H41A H 0.65940 -0.38090 -1.00730 H42A H 0.75010 -0.28270 -1.00680 C22A C 0.94048(10) -0.31306(8) -0.87738(7) C23A C 0.98002(10) -0.07035(8) -0.64440(7) H43A H 1.05680 -0.10410 -0.64560 H44A H 0.97770 -0.04470 -0.58350 C24A C 0.98985(10) 0.00261(8) -0.67310(7) H47A H 1.04030 0.05930 -0.62250 H48A H 1.04790 -0.01530 -0.71070 C26A C 0.89649(10) 0.05068(8) -0.71927(7) H51A H 0.86860 0.10540 -0.67850 H52A H 0.93310 0.08070 -0.75780 N12A N 0.78859(10) -0.03052(8) -0.76954(7) C27A C 0.68546(10) -0.00439(8) -0.83178(7) H55A H 0.62740 0.03220 -0.80100 H56A H 0.72340 0.04130 -0.85930 C28A C 0.6109(1) -0.09970(8) -0.89956(7) H57A H 0.53600 -0.08300 -0.93700 H58A H 0.66550 -0.13150 -0.93590 C29A C 0.56574(10) -0.17432(8) -0.85401(7) H59A H 0.51980 -0.23890 -0.89780 H60A H 0.50550 -0.14430 -0.82170 C30A C 0.77781(10) -0.12255(8) -0.75247(7) C31A C 0.3447(5) 0.0670(4) 0.1838(4) H61A H 0.38510 0.00860 0.16900 C32A C 0.3516(5) 0.1519(5) 0.1514(3) H62A H 0.39740 0.16030 0.11120 C33A C 0.2780(6) 0.2221(3) 0.1898(4) H63A H 0.26590 0.28560 0.17980 C34A C 0.2257(5) 0.1805(4) 0.2459(3) H64A H 0.17240 0.21140 0.28000 C35A C 0.2669(5) 0.0847(3) 0.2422(3) H65A H 0.24610 0.04020 0.27340 C36A C 0.5281(8) -0.0590(6) -0.6373(3) H66A H 0.48330 -0.03790 -0.68400 C37A C 0.4848(4) -0.1432(4) -0.6119(4) H67A H 0.40590 -0.18820 -0.63850 C38A C 0.5801(6) -0.1482(4) -0.5396(4) H68A H 0.57620 -0.19720 -0.50940 C39A C 0.6823(4) -0.0672(5) -0.5203(4) H69A H 0.75880 -0.05250 -0.47500 C40A C 0.6502(7) -0.0121(4) -0.5807(5) H70A H 0.70140 0.04600 -0.58290 C41A C 0.0590(14) -0.0620(13) -0.0211(11) H71A H 0.10730 -0.11460 -0.03790 C42A C 0.0573(15) 0.0252(18) -0.0476(9) H72A H 0.10280 0.04190 -0.08540 C43A C -0.0241(18) 0.084(1) -0.0083(12) H73A H -0.04310 0.14810 -0.01440 C44A C -0.0725(11) 0.0308(16) 0.0416(9) H74A H -0.13060 0.05290 0.07480 C45A C -0.0204(17) -0.0611(13) 0.0342(10) H75A H 0.03610 0.11160 -0.06110 Li1A Li 0.1490(11) 0.0725(9) 0.1054(8) Li3A Li 0.6756(10) -0.1888(8) -0.6589(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 V1 V2 1.933 1_555 1_555 V2 N2 2.116 1_555 1_555 N1 V1 2.084 1_555 1_555 N2 C7 1.463 1_555 1_555 N3 V1 2.078 1_555 1_555 N4 V2 2.061 1_555 1_555 N5 V1 2.057 1_555 1_555 N6 V2 2.073 1_555 1_555 N7 V1 2.111 1_555 1_555 N8 V2 2.087 1_555 1_555 C1 N1 1.462 1_555 1_555 H1 C1 0.990 1_555 1_555 H2 C1 0.990 1_555 1_555 C2 C1 1.497 1_555 1_555 H3 C2 0.991 1_555 1_555 H4 C2 0.989 1_555 1_555 C3 C2 1.509 1_555 1_555 H5 C3 0.990 1_555 1_555 H6 C3 0.990 1_555 1_555 N9 C3 1.453 1_555 1_555 C4 N9 1.472 1_555 1_555 H7 C4 0.990 1_555 1_555 H8 C4 0.990 1_555 1_555 C5 C4 1.356 1_555 1_555 H11 C5 0.990 1_555 1_555 H14 C5 1.020 1_555 1_555 C7 C5 1.457 1_555 1_555 H15 C7 0.990 1_555 1_555 H16 C7 0.991 1_555 1_555 C8 N1 1.352 1_555 1_555 C9 N3 1.469 1_555 1_555 H19 C9 0.990 1_555 1_555 H20 C9 0.990 1_555 1_555 C10 C9 1.541 1_555 1_555 H21 C10 0.990 1_555 1_555 H22 C10 0.990 1_555 1_555 C11 C10 1.531 1_555 1_555 H23 C11 0.989 1_555 1_555 H24 C11 0.990 1_555 1_555 N10 C11 1.477 1_555 1_555 C12 N10 1.474 1_555 1_555 H25 C12 0.990 1_555 1_555 H26 C12 0.989 1_555 1_555 C13 C12 1.548 1_555 1_555 H27 C13 0.990 1_555 1_555 H28 C13 0.990 1_555 1_555 C14 N4 1.452 1_555 1_555 H29 C14 0.989 1_555 1_555 H30 C14 0.989 1_555 1_555 C15 N3 1.326 1_555 1_555 C16 N5 1.453 1_555 1_555 H31 C16 0.990 1_555 1_555 H32 C16 0.991 1_555 1_555 C17 C16 1.522 1_555 1_555 H33 C17 0.990 1_555 1_555 H34 C17 0.990 1_555 1_555 C18 C17 1.503 1_555 1_555 H35 C18 0.990 1_555 1_555 H36 C18 0.990 1_555 1_555 N11 C18 1.488 1_555 1_555 C19 N11 1.458 1_555 1_555 H37 C19 0.990 1_555 1_555 H38 C19 0.990 1_555 1_555 C20 C19 1.527 1_555 1_555 H39 C20 0.990 1_555 1_555 H40 C20 0.989 1_555 1_555 C21 N6 1.462 1_555 1_555 H41 C21 0.990 1_555 1_555 H42 C21 0.990 1_555 1_555 C22 N5 1.338 1_555 1_555 C23 N7 1.467 1_555 1_555 H43 C23 0.990 1_555 1_555 H44 C23 0.990 1_555 1_555 C24 C23 1.233 1_555 1_555 H47 C24 0.990 1_555 1_555 H48 C24 0.990 1_555 1_555 C26 C24 1.446 1_555 1_555 H51 C26 0.990 1_555 1_555 H52 C26 0.990 1_555 1_555 N12 C26 1.465 1_555 1_555 C27 N12 1.483 1_555 1_555 H55 C27 0.990 1_555 1_555 H56 C27 0.990 1_555 1_555 C28 C27 1.501 1_555 1_555 H57 C28 0.990 1_555 1_555 H58 C28 0.990 1_555 1_555 C29 N8 1.473 1_555 1_555 H59 C29 0.990 1_555 1_555 H60 C29 0.990 1_555 1_555 C30 N7 1.339 1_555 1_555 C31 H61 0.950 1_555 1_555 C32 C31 1.420 1_555 1_555 H62 C32 0.949 1_555 1_555 C33 C32 1.421 1_555 1_555 H63 C33 0.949 1_555 1_555 C34 C33 1.420 1_555 1_555 H64 C34 0.951 1_555 1_555 C35 C31 1.420 1_555 1_555 H65 C35 0.951 1_555 1_555 C36 H66 0.950 1_555 1_555 C37 C36 1.420 1_555 1_555 H67 C37 0.950 1_555 1_555 C38 C37 1.419 1_555 1_555 H68 C38 0.950 1_555 1_555 C39 C38 1.419 1_555 1_555 H69 C39 0.950 1_555 1_555 C40 C36 1.420 1_555 1_555 H70 C40 0.950 1_555 1_555 C41 H71 0.950 1_555 1_555 H71 C44A 1.258 1_555 1_555 C42 C41 1.389 1_555 1_555 H72 C42 0.950 1_555 1_555 C43 C42 1.404 1_555 1_555 H73 C43 0.950 1_555 1_555 C44 C43 1.408 1_555 1_555 H74 C44 0.950 1_555 1_555 C45 C41 1.402 1_555 1_555 H75 C42 1.300 1_555 1_555 O1 C46 1.302 1_555 1_555 C46 H76 0.991 1_555 1_555 H77 C46 0.989 1_555 1_555 C47 C46 1.519 1_555 1_555 H78 C47 0.990 1_555 1_555 H79 C47 0.990 1_555 1_555 C48 C47 1.572 1_555 1_555 H80 C48 0.991 1_555 1_555 H81 C48 0.990 1_555 1_555 C49 O1 1.399 1_555 1_555 H82 C49 0.990 1_555 1_555 H83 C49 0.990 1_555 1_555 Li1 C31 2.244 1_555 1_555 Li2 C36 2.319 1_555 1_555 Li3 N1 2.230 1_555 1_555 V1A V2A 1.933 1_555 1_555 V2A N2A 2.116 1_555 1_555 N1A V1A 2.084 1_555 1_555 N2A C7A 1.463 1_555 1_555 N3A V1A 2.078 1_555 1_555 N4A V2A 2.061 1_555 1_555 N5A V1A 2.057 1_555 1_555 N6A V2A 2.073 1_555 1_555 N7A V1A 2.111 1_555 1_555 N8A V2A 2.087 1_555 1_555 C1A N1A 1.462 1_555 1_555 H1A C1A 0.990 1_555 1_555 H2A C1A 0.990 1_555 1_555 C2A C1A 1.497 1_555 1_555 H3A C2A 0.991 1_555 1_555 H4A C2A 0.989 1_555 1_555 C3A C2A 1.509 1_555 1_555 H5A C3A 0.990 1_555 1_555 H6A C3A 0.990 1_555 1_555 N9A C3A 1.453 1_555 1_555 C4A N9A 1.472 1_555 1_555 H7A C4A 0.990 1_555 1_555 H8A C4A 0.990 1_555 1_555 C5A C4A 1.356 1_555 1_555 H11A C5A 0.990 1_555 1_555 H14A C5A 1.020 1_555 1_555 C7A C5A 1.457 1_555 1_555 H15A C7A 0.990 1_555 1_555 H16A C7A 0.991 1_555 1_555 C8A N1A 1.352 1_555 1_555 C9A N3A 1.469 1_555 1_555 H19A C9A 0.990 1_555 1_555 H20A C9A 0.990 1_555 1_555 C10A C9A 1.541 1_555 1_555 H21A C10A 0.990 1_555 1_555 H22A C10A 0.990 1_555 1_555 C11A C10A 1.531 1_555 1_555 H23A C11A 0.989 1_555 1_555 H24A C11A 0.990 1_555 1_555 N10A C11A 1.477 1_555 1_555 C12A N10A 1.474 1_555 1_555 H25A C12A 0.990 1_555 1_555 H26A C12A 0.989 1_555 1_555 C13A C12A 1.548 1_555 1_555 H27A C13A 0.990 1_555 1_555 H28A C13A 0.990 1_555 1_555 C14A N4A 1.452 1_555 1_555 H29A C14A 0.989 1_555 1_555 H30A C14A 0.989 1_555 1_555 C15A N3A 1.326 1_555 1_555 C16A N5A 1.453 1_555 1_555 H31A C16A 0.990 1_555 1_555 H32A C16A 0.991 1_555 1_555 C17A C16A 1.522 1_555 1_555 H33A C17A 0.990 1_555 1_555 H34A C17A 0.990 1_555 1_555 C18A C17A 1.503 1_555 1_555 H35A C18A 0.990 1_555 1_555 H36A C18A 0.990 1_555 1_555 N11A C18A 1.488 1_555 1_555 C19A N11A 1.458 1_555 1_555 H37A C19A 0.990 1_555 1_555 H38A C19A 0.990 1_555 1_555 C20A C19A 1.527 1_555 1_555 H39A C20A 0.990 1_555 1_555 H40A C20A 0.989 1_555 1_555 C21A N6A 1.462 1_555 1_555 H41A C21A 0.990 1_555 1_555 H42A C21A 0.990 1_555 1_555 C22A N5A 1.338 1_555 1_555 C23A N7A 1.467 1_555 1_555 H43A C23A 0.990 1_555 1_555 H44A C23A 0.990 1_555 1_555 C24A C23A 1.233 1_555 1_555 H47A C24A 0.990 1_555 1_555 H48A C24A 0.990 1_555 1_555 C26A C24A 1.446 1_555 1_555 H51A C26A 0.990 1_555 1_555 H52A C26A 0.990 1_555 1_555 N12A C26A 1.465 1_555 1_555 C27A N12A 1.483 1_555 1_555 H55A C27A 0.990 1_555 1_555 H56A C27A 0.990 1_555 1_555 C28A C27A 1.501 1_555 1_555 H57A C28A 0.990 1_555 1_555 H58A C28A 0.990 1_555 1_555 C29A N8A 1.473 1_555 1_555 H59A C29A 0.990 1_555 1_555 H60A C29A 0.990 1_555 1_555 C30A N7A 1.339 1_555 1_555 C31A H61A 0.950 1_555 1_555 C32A C31A 1.420 1_555 1_555 H62A C32A 0.949 1_555 1_555 C33A C32A 1.421 1_555 1_555 H63A C33A 0.949 1_555 1_555 C34A C33A 1.420 1_555 1_555 H64A C34A 0.951 1_555 1_555 C35A C31A 1.420 1_555 1_555 H65A C35A 0.951 1_555 1_555 C36A Li2 2.319 1_555 1_555 H66A C36A 0.950 1_555 1_555 C37A Li2 2.285 1_555 1_555 H67A C37A 0.950 1_555 1_555 C38A Li2 2.280 1_555 1_555 H68A C38A 0.950 1_555 1_555 C39A Li2 2.312 1_555 1_555 H69A C39A 0.950 1_555 1_555 C40A Li2 2.336 1_555 1_555 H70A C40A 0.950 1_555 1_555 C41A C43 0.791 1_555 1_555 H71A C44 1.258 1_555 1_555 C42A C44 0.830 1_555 1_555 H72A C42A 0.950 1_555 1_555 C43A C41 0.791 1_555 1_555 H73A C43A 0.950 1_555 1_555 C44A C41 0.645 1_555 1_555 H74A C44A 0.950 1_555 1_555 C45A C42 0.686 1_555 1_555 H75A C45 0.949 1_555 1_555 Li1A C41 2.340 1_555 1_555 Li3A N1A 2.230 1_555 1_555 N2 C8 1.329 1_555 1_555 N2 Li3 2.341 1_555 1_555 N4 C15 1.359 1_555 1_555 N6 C22 1.347 1_555 1_555 N7 Li3 2.333 1_555 1_555 N8 C30 1.348 1_555 1_555 N8 Li3 2.236 1_555 1_555 N9 C8 1.363 1_555 1_555 C8 Li3 2.445 1_555 1_555 N10 C15 1.363 1_555 1_555 C13 C14 1.537 1_555 1_555 N11 C22 1.353 1_555 1_555 C20 C21 1.497 1_555 1_555 N12 C30 1.375 1_555 1_555 C28 C29 1.547 1_555 1_555 C30 Li3 2.434 1_555 1_555 C32 Li1 2.234 1_555 1_555 C33 Li1 2.286 1_555 1_555 C34 C35 1.420 1_555 1_555 C34 Li1 2.327 1_555 1_555 C35 Li1 2.301 1_555 1_555 C36 Li3 2.510 1_555 1_555 C37 Li2 2.285 1_555 1_555 C37 Li3 2.453 1_555 1_555 C38 Li2 2.280 1_555 1_555 C38 Li3 2.412 1_555 1_555 C39 C40 1.420 1_555 1_555 C39 Li2 2.312 1_555 1_555 C39 Li3 2.444 1_555 1_555 C40 Li2 2.336 1_555 1_555 C40 Li3 2.504 1_555 1_555 C41 Li1 2.340 1_555 1_555 C42 Li1 2.401 1_555 1_555 C42 C44A 0.830 1_555 1_555 C42 Li1A 2.357 1_555 1_555 C43 Li1 2.394 1_555 1_555 C43 C45A 0.755 1_555 1_555 C43 Li1A 2.391 1_555 1_555 C44 C45 1.417 1_555 1_555 C44 Li1 2.347 1_555 1_555 C44 C41A 0.645 1_555 1_555 C44 Li1A 2.390 1_555 1_555 C45 Li1 2.329 1_555 1_555 C45 C42A 0.686 1_555 1_555 C45 C43A 0.755 1_555 1_555 C45 Li1A 2.382 1_555 1_555 H75 C45A 0.949 1_555 1_555 C48 C49 1.497 1_555 1_555 Li1 C41A 2.340 1_555 1_555 Li1 C42A 2.357 1_555 1_555 Li1 C43A 2.391 1_555 1_555 Li1 C44A 2.390 1_555 1_555 Li1 C45A 2.382 1_555 1_555 N2A C8A 1.329 1_555 1_555 N2A Li3A 2.341 1_555 1_555 N4A C15A 1.359 1_555 1_555 N6A C22A 1.347 1_555 1_555 N7A Li3A 2.333 1_555 1_555 N8A C30A 1.348 1_555 1_555 N8A Li3A 2.236 1_555 1_555 N9A C8A 1.363 1_555 1_555 C8A Li3A 2.445 1_555 1_555 N10A C15A 1.363 1_555 1_555 C13A C14A 1.537 1_555 1_555 N11A C22A 1.353 1_555 1_555 C20A C21A 1.497 1_555 1_555 N12A C30A 1.375 1_555 1_555 C28A C29A 1.547 1_555 1_555 C30A Li3A 2.434 1_555 1_555 C31A Li1A 2.244 1_555 1_555 C32A Li1A 2.234 1_555 1_555 C33A Li1A 2.286 1_555 1_555 C34A C35A 1.420 1_555 1_555 C34A Li1A 2.327 1_555 1_555 C35A Li1A 2.301 1_555 1_555 C36A C37A 1.420 1_555 1_555 C36A C40A 1.420 1_555 1_555 C36A Li3A 2.510 1_555 1_555 C37A C38A 1.419 1_555 1_555 C37A Li3A 2.453 1_555 1_555 C38A C39A 1.419 1_555 1_555 C38A Li3A 2.412 1_555 1_555 C39A C40A 1.420 1_555 1_555 C39A Li3A 2.444 1_555 1_555 C40A Li3A 2.504 1_555 1_555 C41A H71A 0.950 1_555 1_555 C41A C42A 1.389 1_555 1_555 C41A C45A 1.402 1_555 1_555 C41A Li1A 2.340 1_555 1_555 C42A C43A 1.404 1_555 1_555 C42A H75A 1.300 1_555 1_555 C42A Li1A 2.401 1_555 1_555 C43A C44A 1.408 1_555 1_555 C43A Li1A 2.394 1_555 1_555 C44A C45A 1.417 1_555 1_555 C44A Li1A 2.347 1_555 1_555 C45A Li1A 2.329 1_555 1_555 #END data_CSD_CIF_SUMSUO _audit_creation_date 1994-07-28 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD SUMSUO _chemical_formula_sum 'C38 H50 Li2 N4 O8' _chemical_formula_moiety ; C22 H18 Li1 N4 1-,C16 H32 Li1 O8 1+ ; _journal_coden_Cambridge 179 _journal_volume 33 _journal_year 1994 _journal_page_first 693 _journal_name_full 'Angew.Chem.,Int.Ed. ' loop_ _publ_author_name "H.Gornitzka" "D.Stalke" _chemical_name_systematic ; bis(12-Crown-4)-lithium bis(bis(2-pyridyl)methane)-lithium ; _chemical_melting_point 466.15 _cell_volume 3713.585 _exptl_crystal_colour 'yellow' _exptl_crystal_density_diffrn 1.26 _diffrn_ambient_temperature 153 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_gt 0.0502 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,-1/2-y,-1/2+z _cell_length_a 11.941(6) _cell_length_b 24.049(12) _cell_length_c 13.208(7) _cell_angle_alpha 90 _cell_angle_beta 101.74(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.46 N 0.68 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.2651(3) 0.3853(2) 0.8328(3) C1 C 0.2574(2) 0.32919(10) 1.0566(2) H1 H 0.2471(20) 0.3119(10) 1.1205(15) C2 C 0.2702(2) 0.38777(10) 1.0604(2) C3 C 0.2659(2) 0.41659(11) 1.1533(2) H2 H 0.258(2) 0.3953(9) 1.2125(14) C4 C 0.2811(3) 0.47251(12) 1.1608(2) H3 H 0.2832(21) 0.4908(10) 1.2261(14) C5 C 0.3014(3) 0.50227(12) 1.0761(2) H4 H 0.3187(25) 0.5421(7) 1.0799(22) C6 C 0.3042(2) 0.47295(11) 0.9879(2) H5 H 0.3196(21) 0.4916(10) 0.9240(14) N1 N 0.2885(2) 0.41759(8) 0.97635(14) C7 C 0.2767(2) 0.29077(10) 0.9819(2) C8 C 0.2791(2) 0.23265(11) 1.0054(2) H6 H 0.2627(20) 0.2215(10) 1.0703(13) C9 C 0.3082(2) 0.19427(11) 0.9397(2) H7 H 0.3109(24) 0.1555(7) 0.958(2) C10 C 0.3333(2) 0.21182(11) 0.8459(2) H8 H 0.3527(21) 0.1852(9) 0.7957(16) C11 C 0.3250(2) 0.26764(11) 0.8243(2) H9 H 0.3424(20) 0.2814(10) 0.7573(14) N2 N 0.2967(2) 0.30684(8) 0.88729(15) C12 C 0.1748(2) 0.43693(10) 0.5976(2) H10 H 0.1505(20) 0.4516(10) 0.5281(15) C13 C 0.2936(2) 0.42891(9) 0.6259(2) C14 C 0.3641(3) 0.44442(10) 0.5548(2) H11 H 0.3279(19) 0.4593(10) 0.4892(13) C15 C 0.4799(3) 0.43848(11) 0.5797(2) H12 H 0.5264(21) 0.4480(11) 0.5306(17) C16 C 0.5309(2) 0.41709(12) 0.6760(3) H13 H 0.6134(14) 0.4111(11) 0.6982(19) C17 C 0.4598(2) 0.40275(11) 0.7408(2) H14 H 0.4931(21) 0.3863(11) 0.8103(13) N3 N 0.3456(2) 0.40766(8) 0.72038(15) C18 C 0.0877(2) 0.42916(9) 0.6543(2) C19 C -0.0284(2) 0.44185(11) 0.6088(2) H15 H -0.0446(19) 0.4527(9) 0.5375(11) C20 C -0.1131(2) 0.43609(11) 0.6628(2) H16 H -0.1903(14) 0.4448(10) 0.6282(17) C21 C -0.0869(2) 0.41795(10) 0.7655(2) H17 H -0.1449(18) 0.414(1) 0.8077(17) C22 C 0.0258(2) 0.40615(10) 0.8056(2) H18 H 0.0480(18) 0.3945(9) 0.8799(12) N4 N 0.1118(2) 0.41023(7) 0.75442(14) Li2 Li 0.2048(4) 0.6629(2) 0.7873(4) O1 O 0.26478(14) 0.63374(7) 0.62996(13) C23 C 0.2925(2) 0.68089(12) 0.5740(2) H19 H 0.2211(2) 0.69875(12) 0.5370(2) H20 H 0.3363(2) 0.66861(12) 0.5220(2) C24 C 0.3617(2) 0.72217(11) 0.6454(2) H21 H 0.4356(2) 0.70547(11) 0.6794(2) H22 H 0.3776(2) 0.75529(11) 0.6061(2) O2 O 0.29804(13) 0.73768(7) 0.72083(13) C25 C 0.3626(2) 0.76863(10) 0.8053(2) H23 H 0.3095(2) 0.78976(10) 0.8396(2) H24 H 0.4120(2) 0.7957(1) 0.7787(2) C26 C 0.4357(2) 0.73151(10) 0.8831(2) H25 H 0.4935(2) 0.71238(10) 0.8516(2) H26 H 0.4758(2) 0.75358(10) 0.9429(2) O3 O 0.36177(13) 0.69200(7) 0.91580(12) C27 C 0.4202(2) 0.64388(11) 0.9640(2) H27 H 0.3749(2) 0.62688(11) 1.0109(2) H28 H 0.4953(2) 0.65503(11) 1.0059(2) C28 C 0.4377(2) 0.60214(11) 0.8847(2) H29 H 0.4876(2) 0.61772(11) 0.8404(2) H30 H 0.4743(2) 0.56818(11) 0.9187(2) O4 O 0.32764(13) 0.58927(7) 0.82407(12) C29 C 0.3319(2) 0.5566(1) 0.7343(2) H31 H 0.2589(2) 0.53616(10) 0.7129(2) H32 H 0.3943(2) 0.52895(10) 0.7514(2) C30 C 0.3516(2) 0.59233(11) 0.6467(2) H33 H 0.4281(2) 0.60991(11) 0.6643(2) H34 H 0.3476(2) 0.56963(11) 0.5836(2) O5 O 0.07876(13) 0.59450(7) 0.74835(12) C31 C -0.0280(2) 0.60809(11) 0.6841(2) H35 H -0.0804(2) 0.62374(11) 0.7259(2) H36 H -0.0638(2) 0.57450(11) 0.6480(2) C32 C -0.0043(2) 0.65041(10) 0.6070(2) H37 H 0.0434(2) 0.63332(10) 0.5622(2) H38 H -0.0774(2) 0.66233(10) 0.5625(2) O6 O 0.05356(13) 0.69781(7) 0.65844(12) C33 C -0.0200(2) 0.73622(11) 0.6957(2) H39 H -0.0786(2) 0.71600(11) 0.7246(2) H40 H -0.0593(2) 0.76040(11) 0.6388(2) C34 C 0.0543(2) 0.77050(9) 0.7784(2) H41 H 0.1092(2) 0.79231(9) 0.7475(2) H42 H 0.0060(2) 0.79693(9) 0.8079(2) O7 O 0.11565(12) 0.73575(6) 0.85891(12) C35 C 0.0504(2) 0.71992(10) 0.9332(2) H43 H -0.0233(2) 0.70352(10) 0.8981(2) H44 H 0.0343(2) 0.75283(10) 0.9729(2) C36 C 0.1186(2) 0.67806(10) 1.0043(2) H45 H 0.1909(2) 0.69537(10) 1.0406(2) H46 H 0.0750(2) 0.66665(10) 1.0570(2) O8 O 0.14417(13) 0.63009(7) 0.94948(12) C37 C 0.0515(2) 0.59163(10) 0.9246(2) H47 H -0.0222(2) 0.6118(1) 0.9080(2) H48 H 0.0503(2) 0.56663(10) 0.9839(2) C38 C 0.0694(2) 0.55876(10) 0.8330(2) H49 H 0.1400(2) 0.53632(10) 0.8525(2) H50 H 0.0044(2) 0.53292(10) 0.8113(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 N1 2.015 1_555 1_555 C1 H1 0.971 1_555 1_555 C2 C1 1.417 1_555 1_555 C3 C2 1.419 1_555 1_555 H2 C3 0.955 1_555 1_555 C4 C3 1.358 1_555 1_555 H3 C4 0.964 1_555 1_555 C5 C4 1.390 1_555 1_555 H4 C5 0.979 1_555 1_555 C6 C5 1.368 1_555 1_555 H5 C6 1.005 1_555 1_555 N1 C2 1.376 1_555 1_555 C7 C1 1.405 1_555 1_555 C8 C7 1.431 1_555 1_555 H6 C8 0.956 1_555 1_555 C9 C8 1.360 1_555 1_555 H7 C9 0.962 1_555 1_555 C10 C9 1.398 1_555 1_555 H8 C10 0.983 1_555 1_555 C11 C10 1.372 1_555 1_555 H9 C11 1.005 1_555 1_555 N2 Li1 2.027 1_555 1_555 C12 H10 0.971 1_555 1_555 C13 C12 1.405 1_555 1_555 C14 C13 1.432 1_555 1_555 H11 C14 0.956 1_555 1_555 C15 C14 1.362 1_555 1_555 H12 C15 0.963 1_555 1_555 C16 C15 1.392 1_555 1_555 H13 C16 0.980 1_555 1_555 C17 C16 1.367 1_555 1_555 H14 C17 1.004 1_555 1_555 N3 Li1 2.000 1_555 1_555 C18 C12 1.412 1_555 1_555 C19 C18 1.427 1_555 1_555 H15 C19 0.958 1_555 1_555 C20 C19 1.358 1_555 1_555 H16 C20 0.965 1_555 1_555 C21 C20 1.398 1_555 1_555 H17 C21 0.978 1_555 1_555 C22 C21 1.372 1_555 1_555 H18 C22 1.003 1_555 1_555 N4 Li1 2.003 1_555 1_555 Li2 O1 2.435 1_555 1_555 O1 C23 1.429 1_555 1_555 C23 H19 0.990 1_555 1_555 H20 C23 0.989 1_555 1_555 C24 C23 1.497 1_555 1_555 H21 C24 0.990 1_555 1_555 H22 C24 0.990 1_555 1_555 O2 Li2 2.375 1_555 1_555 C25 O2 1.429 1_555 1_555 H23 C25 0.991 1_555 1_555 H24 C25 0.990 1_555 1_555 C26 C25 1.500 1_555 1_555 H25 C26 0.989 1_555 1_555 H26 C26 0.990 1_555 1_555 O3 Li2 2.364 1_555 1_555 C27 O3 1.432 1_555 1_555 H27 C27 0.990 1_555 1_555 H28 C27 0.990 1_555 1_555 C28 C27 1.496 1_555 1_555 H29 C28 0.990 1_555 1_555 H30 C28 0.990 1_555 1_555 O4 Li2 2.288 1_555 1_555 C29 O4 1.432 1_555 1_555 H31 C29 0.991 1_555 1_555 H32 C29 0.990 1_555 1_555 C30 O1 1.422 1_555 1_555 H33 C30 0.990 1_555 1_555 H34 C30 0.989 1_555 1_555 O5 Li2 2.218 1_555 1_555 C31 O5 1.418 1_555 1_555 H35 C31 0.989 1_555 1_555 H36 C31 0.990 1_555 1_555 C32 C31 1.507 1_555 1_555 H37 C32 0.990 1_555 1_555 H38 C32 0.990 1_555 1_555 O6 Li2 2.369 1_555 1_555 C33 O6 1.429 1_555 1_555 H39 C33 0.990 1_555 1_555 H40 C33 0.990 1_555 1_555 C34 C33 1.505 1_555 1_555 H41 C34 0.990 1_555 1_555 H42 C34 0.990 1_555 1_555 O7 Li2 2.347 1_555 1_555 C35 O7 1.423 1_555 1_555 H43 C35 0.989 1_555 1_555 H44 C35 0.990 1_555 1_555 C36 C35 1.499 1_555 1_555 H45 C36 0.990 1_555 1_555 H46 C36 0.989 1_555 1_555 O8 Li2 2.523 1_555 1_555 C37 O8 1.428 1_555 1_555 H47 C37 0.990 1_555 1_555 H48 C37 0.990 1_555 1_555 C38 O5 1.433 1_555 1_555 H49 C38 0.990 1_555 1_555 H50 C38 0.990 1_555 1_555 C6 N1 1.349 1_555 1_555 C7 N2 1.375 1_555 1_555 C11 N2 1.345 1_555 1_555 C13 N3 1.374 1_555 1_555 C17 N3 1.340 1_555 1_555 C18 N4 1.373 1_555 1_555 C22 N4 1.343 1_555 1_555 C24 O2 1.420 1_555 1_555 C26 O3 1.423 1_555 1_555 C28 O4 1.427 1_555 1_555 C29 C30 1.498 1_555 1_555 C32 O6 1.431 1_555 1_555 C34 O7 1.431 1_555 1_555 C36 O8 1.428 1_555 1_555 C37 C38 1.497 1_555 1_555 #END data_CSD_CIF_SUMTAV _audit_creation_date 1994-07-28 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD SUMTAV _chemical_formula_sum 'C50 H74 Li1 N4 Na1 O7' _chemical_formula_moiety ; C22 H18 Li1 N4 1-,C24 H48 Na1 O6 1+,C4 H8 O1 ; _journal_coden_Cambridge 179 _journal_volume 33 _journal_year 1994 _journal_page_first 693 _journal_name_full 'Angew.Chem.,Int.Ed. ' loop_ _publ_author_name "H.Gornitzka" "D.Stalke" _chemical_name_systematic ; hexakis(Tetrahydrofuran)-sodium bis(bis(2-pyridyl)methane)-lithium tetrahydrofuran solvate ; _chemical_melting_point 243.15 _cell_volume 2468.678 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.175 _diffrn_ambient_temperature 153 _refine_special_details ; Three of the THF species are disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_gt 0.0554 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.324(5) _cell_length_b 14.073(7) _cell_length_c 17.885(9) _cell_angle_alpha 93.49(2) _cell_angle_beta 106.73(2) _cell_angle_gamma 112.76(2) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 0.94 N 0.68 Na 1.33 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.3005(5) 0.1434(4) 0.1947(3) C1 C 0.4761(3) 0.0381(2) 0.1333(2) H1 H 0.5289(27) 0.0127(21) 0.1161(15) C2 C 0.4356(3) -0.0025(2) 0.1952(2) C3 C 0.4790(3) -0.0783(2) 0.2294(2) H2 H 0.5343(27) -0.0967(22) 0.2056(16) C4 C 0.4402(3) -0.1202(3) 0.2891(2) H3 H 0.4734(33) -0.1696(22) 0.3115(19) C5 C 0.3577(4) -0.0891(3) 0.3190(2) H4 H 0.3294(34) -0.1134(26) 0.3629(16) C6 C 0.3189(3) -0.0171(2) 0.2847(2) H5 H 0.2602(27) 0.0056(22) 0.3041(17) N1 N 0.3543(2) 0.0271(2) 0.22538(13) C7 C 0.4414(3) 0.1061(2) 0.0856(2) C8 C 0.4963(3) 0.1330(2) 0.0242(2) H6 H 0.5599(26) 0.1040(21) 0.0172(17) C9 C 0.4619(3) 0.1960(3) -0.0241(2) H7 H 0.5027(31) 0.2160(24) -0.0640(16) C10 C 0.3715(3) 0.2354(2) -0.0124(2) H8 H 0.345(3) 0.2800(21) -0.0446(16) C11 C 0.3229(3) 0.2084(2) 0.0480(2) H9 H 0.2665(27) 0.2367(22) 0.0637(17) N2 N 0.3545(2) 0.1468(2) 0.09745(13) C12 C 0.2167(3) 0.3019(2) 0.2902(2) H10 H 0.1952(26) 0.3465(19) 0.3197(15) C13 C 0.1060(3) 0.2167(2) 0.2343(2) C14 C -0.0291(3) 0.2061(2) 0.2239(2) H11 H -0.0386(27) 0.2563(18) 0.2576(14) C15 C -0.1393(3) 0.1269(2) 0.1706(2) H12 H -0.2276(22) 0.1219(23) 0.1656(17) C16 C -0.1224(3) 0.0541(2) 0.1242(2) H13 H -0.1953(24) -0.0009(18) 0.0836(14) C17 C 0.0083(3) 0.0663(2) 0.1359(2) H14 H 0.0289(22) 0.0199(16) 0.1044(12) N3 N 0.1212(2) 0.1439(2) 0.18868(13) C18 C 0.3578(3) 0.3325(2) 0.3101(2) C19 C 0.4510(3) 0.4257(2) 0.3676(2) H15 H 0.4130(28) 0.4646(21) 0.3916(16) C20 C 0.5878(3) 0.4575(2) 0.3872(2) H16 H 0.6422(28) 0.5199(18) 0.4257(15) C21 C 0.6372(3) 0.3986(2) 0.3513(2) H17 H 0.7344(22) 0.4188(25) 0.3615(19) C22 C 0.5440(3) 0.3102(2) 0.2966(2) H18 H 0.5715(27) 0.2672(20) 0.2680(15) N4 N 0.4086(2) 0.2758(2) 0.27533(13) Na1 Na 0.00000 0.50000 0.00000 O1 O 0.1287(2) 0.5422(2) -0.08631(12) C23 C 0.0862(3) 0.5734(3) -0.1598(2) H19 H 0.0411(3) 0.6201(3) -0.1546(2) H20 H 0.0213(3) 0.5112(3) -0.2020(2) C24 C 0.2117(3) 0.6302(3) -0.1796(2) H21 H 0.2569(3) 0.7055(3) -0.1540(2) H22 H 0.1910(3) 0.6239(3) -0.2378(2) C25 C 0.2980(3) 0.5736(3) -0.1455(2) H23 H 0.2764(3) 0.5108(3) -0.1841(2) H24 H 0.3961(3) 0.6205(3) -0.1301(2) C26 C 0.2598(3) 0.5432(3) -0.0738(2) H25 H 0.2564(3) 0.4729(3) -0.0677(2) H26 H 0.3275(3) 0.5946(3) -0.0250(2) O2 O 0.1943(2) 0.5076(2) 0.10340(13) C27 C 0.2984(12) 0.5992(7) 0.1568(8) H27 H 0.2708(12) 0.6145(7) 0.2021(8) H28 H 0.3153(12) 0.6598(7) 0.1295(8) C28 C 0.4220(11) 0.5825(11) 0.1855(8) H29 H 0.4472(11) 0.5832(11) 0.2434(8) H30 H 0.4984(11) 0.6384(11) 0.1755(8) C29 C 0.3912(11) 0.4773(14) 0.1406(18) H31 H 0.4291(11) 0.4849(14) 0.0967(18) H32 H 0.4281(11) 0.4369(14) 0.1763(18) C30 C 0.2402(4) 0.4260(3) 0.1093(2) H33 H 0.2075(4) 0.3809(3) 0.0564(2) H34 H 0.2049(4) 0.3817(3) 0.1458(2) C31? C 0.2752(18) 0.5871(13) 0.1728(10) H35? H 0.2239(18) 0.5820(13) 0.210(1) H36? H 0.2995(18) 0.6574(13) 0.1584(10) C32? C 0.3996(14) 0.5725(13) 0.2108(8) H37? H 0.4025(14) 0.5540(13) 0.2636(8) H38? H 0.4821(14) 0.6371(13) 0.2174(8) C33? C 0.3900(18) 0.4836(21) 0.1545(21) H39? H 0.4414(18) 0.5105(21) 0.1182(21) H40? H 0.4253(18) 0.4375(21) 0.1840(21) O3 O 0.0693(2) 0.6792(2) 0.05402(13) C34 C 0.1295(4) 0.7704(3) 0.0232(3) H41 H 0.0996(4) 0.7529(3) -0.0356(3) H42 H 0.2300(4) 0.7985(3) 0.0446(3) C35 C 0.0837(3) 0.8491(2) 0.0486(2) H43 H 0.0141(3) 0.8552(2) 0.0033(2) H44 H 0.1613(3) 0.9190(2) 0.0707(2) C36 C 0.0243(4) 0.8070(3) 0.1120(2) H45 H 0.0853(4) 0.8499(3) 0.1654(2) H46 H -0.0657(4) 0.8083(3) 0.1017(2) C37 C 0.0114(20) 0.7009(11) 0.1077(11) H47 H 0.0575(20) 0.6915(11) 0.1609(11) H48 H -0.086(2) 0.6514(11) 0.0905(11) C38? C 0.0716(6) 0.7237(5) 0.1302(4) H49? H 0.1648(6) 0.7536(5) 0.1697(4) H50? H 0.0098(6) 0.6697(5) 0.1511(4) Na2 Na 0.00000 0.00000 0.50000 O4 O 0.1237(2) -0.10253(15) 0.54473(12) C39 C 0.2605(3) -0.0794(3) 0.5484(2) H51 H 0.3221(3) -0.0063(3) 0.5768(2) H52 H 0.2649(3) -0.0872(3) 0.4940(2) C40 C 0.3025(3) -0.1554(3) 0.5922(2) H53 H 0.2914(3) -0.2154(3) 0.5546(2) H54 H 0.3983(3) -0.1204(3) 0.6282(2) C41 C 0.2072(3) -0.1904(3) 0.6381(2) H55 H 0.2423(3) -0.1415(3) 0.6896(2) H56 H 0.1912(3) -0.2621(3) 0.6481(2) C42 C 0.0785(3) -0.1883(2) 0.5828(2) H57 H 0.0234(3) -0.2549(2) 0.5432(2) H58 H 0.0226(3) -0.1781(2) 0.6134(2) O5 O 0.0534(2) 0.08594(15) 0.63113(11) C43 C 0.1187(5) 0.0609(3) 0.7027(2) H59 H 0.1727(5) 0.0236(3) 0.6927(2) H60 H 0.0505(5) 0.0154(3) 0.7245(2) C44 C 0.2092(4) 0.1627(3) 0.7594(2) H61 H 0.3043(4) 0.1858(3) 0.7606(2) H62 H 0.2069(4) 0.1563(3) 0.8138(2) C45 C 0.1527(3) 0.2390(2) 0.7279(2) H63 H 0.1261(3) 0.2696(2) 0.7681(2) H64 H 0.2201(3) 0.2965(2) 0.7128(2) C46 C 0.0307(3) 0.1731(2) 0.6564(2) H65 H -0.0532(3) 0.1490(2) 0.6705(2) H66 H 0.0212(3) 0.2139(2) 0.6136(2) O6 O 0.1954(2) 0.13564(15) 0.49284(12) C47 C 0.2850(11) 0.2238(8) 0.5547(6) H67 H 0.3094(11) 0.2008(8) 0.6059(6) H68 H 0.2410(11) 0.2712(8) 0.5601(6) C48? C 0.2670(13) 0.2462(9) 0.5296(8) H69? H 0.2624(13) 0.2569(9) 0.5838(8) H70? H 0.2258(13) 0.2874(9) 0.4976(8) C49 C 0.4093(3) 0.2793(3) 0.5335(2) H71 H 0.4925(3) 0.3068(3) 0.5812(2) H72 H 0.4040(3) 0.3382(3) 0.5072(2) C50 C 0.4080(3) 0.1945(3) 0.4769(2) H73 H 0.4543(3) 0.1541(3) 0.5061(2) H74 H 0.4525(3) 0.2246(3) 0.4383(2) C51 C 0.2581(3) 0.1265(2) 0.4357(2) H75 H 0.2221(3) 0.1516(2) 0.3875(2) H76 H 0.2415(3) 0.0526(2) 0.4200(2) O7 O 0.0133(3) 0.5193(2) 0.6138(2) C52 C 0.0003(4) 0.4169(3) 0.6210(3) H77 H 0.0742(4) 0.4199(3) 0.6684(3) H78 H 0.0077(4) 0.3831(3) 0.5735(3) C53 C -0.1318(5) 0.3556(3) 0.6288(3) H79 H -0.1229(5) 0.3485(3) 0.6846(3) H80 H -0.1773(5) 0.2848(3) 0.5945(3) C54 C -0.2092(4) 0.4240(3) 0.6000(3) H81 H -0.2949(4) 0.3826(3) 0.5552(3) H82 H -0.2307(4) 0.4524(3) 0.6438(3) C55 C -0.1146(4) 0.5084(3) 0.5744(3) H83 H -0.1356(4) 0.4910(3) 0.5162(3) H84 H -0.1223(4) 0.5748(3) 0.5868(3) O1A O -0.1287(2) 0.4578(2) 0.08631(12) O2A O -0.1943(2) 0.4924(2) -0.10340(13) O3A O -0.0693(2) 0.3208(2) -0.05402(13) C23A C -0.0862(3) 0.4266(3) 0.1598(2) C26A C -0.2598(3) 0.4568(3) 0.0738(2) C27A C -0.2984(12) 0.4008(7) -0.1568(8) C30A C -0.2402(4) 0.5740(3) -0.1093(2) C34A C -0.1295(4) 0.2296(3) -0.0232(3) C37A C -0.0114(20) 0.2991(11) -0.1077(11) H19A H -0.0411(3) 0.3799(3) 0.1546(2) H20A H -0.0213(3) 0.4888(3) 0.2020(2) C24A C -0.2117(3) 0.3698(3) 0.1796(2) C25A C -0.2980(3) 0.4264(3) 0.1455(2) H25A H -0.2564(3) 0.5271(3) 0.0677(2) H26A H -0.3275(3) 0.4054(3) 0.0250(2) H27A H -0.2708(12) 0.3855(7) -0.2021(8) H28A H -0.3153(12) 0.3402(7) -0.1295(8) C28A C -0.4220(11) 0.4175(11) -0.1855(8) C29A C -0.3912(11) 0.5227(14) -0.1406(18) H33A H -0.2075(4) 0.6191(3) -0.0564(2) H34A H -0.2049(4) 0.6183(3) -0.1458(2) H41A H -0.0996(4) 0.2471(3) 0.0356(3) H42A H -0.2300(4) 0.2015(3) -0.0446(3) C35A C -0.0837(3) 0.1509(2) -0.0486(2) C36A C -0.0243(4) 0.1930(3) -0.1120(2) H47A H -0.0575(20) 0.3085(11) -0.1609(11) H48A H 0.086(2) 0.3486(11) -0.0905(11) H21A H -0.2569(3) 0.2945(3) 0.1540(2) H22A H -0.1910(3) 0.3761(3) 0.2378(2) H23A H -0.2764(3) 0.4892(3) 0.1841(2) H24A H -0.3961(3) 0.3795(3) 0.1301(2) H29A H -0.4472(11) 0.4168(11) -0.2434(8) H30A H -0.4984(11) 0.3616(11) -0.1755(8) H31A H -0.4291(11) 0.5151(14) -0.0967(18) H32A H -0.4281(11) 0.5631(14) -0.1763(18) H43A H -0.0141(3) 0.1448(2) -0.0033(2) H44A H -0.1613(3) 0.0810(2) -0.0707(2) H45A H -0.0853(4) 0.1501(3) -0.1654(2) H46A H 0.0657(4) 0.1917(3) -0.1017(2) O4A O -0.1237(2) 0.10253(15) 0.45527(12) O5A O -0.0534(2) -0.08594(15) 0.36887(11) O6A O -0.1954(2) -0.13564(15) 0.50716(12) C39A C -0.2605(3) 0.0794(3) 0.4516(2) C42A C -0.0785(3) 0.1883(2) 0.4172(2) C43A C -0.1187(5) -0.0609(3) 0.2973(2) C46A C -0.0307(3) -0.1731(2) 0.3436(2) C47A C -0.2850(11) -0.2238(8) 0.4453(6) C51A C -0.2581(3) -0.1265(2) 0.5643(2) H51A H -0.3221(3) 0.0063(3) 0.4232(2) H52A H -0.2649(3) 0.0872(3) 0.5060(2) C40A C -0.3025(3) 0.1554(3) 0.4078(2) C41A C -0.2072(3) 0.1904(3) 0.3619(2) H57A H -0.0234(3) 0.2549(2) 0.4568(2) H58A H -0.0226(3) 0.1781(2) 0.3866(2) H59A H -0.1727(5) -0.0236(3) 0.3073(2) H60A H -0.0505(5) -0.0154(3) 0.2755(2) C44A C -0.2092(4) -0.1627(3) 0.2406(2) C45A C -0.1527(3) -0.2390(2) 0.2721(2) H65A H 0.0532(3) -0.1490(2) 0.3295(2) H66A H -0.0212(3) -0.2139(2) 0.3864(2) H67A H -0.3094(11) -0.2008(8) 0.3941(6) H68A H -0.2410(11) -0.2712(8) 0.4399(6) C49A C -0.4093(3) -0.2793(3) 0.4665(2) C50A C -0.4080(3) -0.1945(3) 0.5231(2) H75A H -0.2221(3) -0.1516(2) 0.6125(2) H76A H -0.2415(3) -0.0526(2) 0.5800(2) H53A H -0.2914(3) 0.2154(3) 0.4454(2) H54A H -0.3983(3) 0.1204(3) 0.3718(2) H55A H -0.2423(3) 0.1415(3) 0.3104(2) H56A H -0.1912(3) 0.2621(3) 0.3519(2) H61A H -0.3043(4) -0.1858(3) 0.2394(2) H62A H -0.2069(4) -0.1563(3) 0.1862(2) H63A H -0.1261(3) -0.2696(2) 0.2319(2) H64A H -0.2201(3) -0.2965(2) 0.2872(2) H71A H -0.4925(3) -0.3068(3) 0.4188(2) H72A H -0.4040(3) -0.3382(3) 0.4928(2) H73A H -0.4543(3) -0.1541(3) 0.4939(2) H74A H -0.4525(3) -0.2246(3) 0.5617(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 N1 2.010 1_555 1_555 C1 H1 0.915 1_555 1_555 C2 C1 1.389 1_555 1_555 C3 C2 1.437 1_555 1_555 H2 C3 0.952 1_555 1_555 C4 C3 1.352 1_555 1_555 H3 C4 0.967 1_555 1_555 C5 C4 1.388 1_555 1_555 H4 C5 0.964 1_555 1_555 C6 C5 1.364 1_555 1_555 H5 C6 0.974 1_555 1_555 N1 C2 1.367 1_555 1_555 C7 C1 1.413 1_555 1_555 C8 C7 1.413 1_555 1_555 H6 C8 0.987 1_555 1_555 C9 C8 1.360 1_555 1_555 H7 C9 0.957 1_555 1_555 C10 C9 1.396 1_555 1_555 H8 C10 0.952 1_555 1_555 C11 C10 1.358 1_555 1_555 H9 C11 0.965 1_555 1_555 N2 Li1 2.000 1_555 1_555 C12 H10 0.940 1_555 1_555 C13 C12 1.406 1_555 1_555 C14 C13 1.433 1_555 1_555 H11 C14 0.958 1_555 1_555 C15 C14 1.348 1_555 1_555 H12 C15 0.952 1_555 1_555 C16 C15 1.384 1_555 1_555 H13 C16 0.949 1_555 1_555 C17 C16 1.373 1_555 1_555 H14 C17 0.973 1_555 1_555 N3 Li1 2.005 1_555 1_555 C18 C12 1.409 1_555 1_555 C19 C18 1.425 1_555 1_555 H15 C19 0.964 1_555 1_555 C20 C19 1.362 1_555 1_555 H16 C20 0.943 1_555 1_555 C21 C20 1.383 1_555 1_555 H17 C21 0.981 1_555 1_555 C22 C21 1.364 1_555 1_555 H18 C22 0.962 1_555 1_555 N4 Li1 1.985 1_555 1_555 Na1 O1 2.366 1_555 1_555 O1 C23 1.422 1_555 1_555 C23 H19 0.990 1_555 1_555 H20 C23 0.989 1_555 1_555 C24 C23 1.493 1_555 1_555 H21 C24 0.990 1_555 1_555 H22 C24 0.989 1_555 1_555 C25 C24 1.510 1_555 1_555 H23 C25 0.989 1_555 1_555 H24 C25 0.990 1_555 1_555 C26 O1 1.431 1_555 1_555 H25 C26 0.989 1_555 1_555 H26 C26 0.991 1_555 1_555 O2 Na1 2.392 1_555 1_555 C27 O2 1.411 1_555 1_555 H27 C27 0.988 1_555 1_555 H28 C27 0.990 1_555 1_555 C28 C27 1.461 1_555 1_555 H29 C28 0.990 1_555 1_555 H30 C28 0.989 1_555 1_555 C29 C28 1.501 1_555 1_555 H31 C29 0.990 1_555 1_555 H32 C29 0.990 1_555 1_555 C30 O2 1.430 1_555 1_555 H33 C30 0.989 1_555 1_555 H34 C30 0.991 1_555 1_555 O3 Na1 2.376 1_555 1_555 C34 O3 1.429 1_555 1_555 H41 C34 0.990 1_555 1_555 H42 C34 0.990 1_555 1_555 C35 C34 1.490 1_555 1_555 H43 C35 0.989 1_555 1_555 H44 C35 0.990 1_555 1_555 C36 C35 1.517 1_555 1_555 H45 C36 0.990 1_555 1_555 H46 C36 0.990 1_555 1_555 C37 O3 1.388 1_555 1_555 H47 C37 0.989 1_555 1_555 H48 C37 0.990 1_555 1_555 Na2 O4 2.397 1_555 1_555 O4 C39 1.435 1_555 1_555 C39 H51 0.990 1_555 1_555 H52 C39 0.990 1_555 1_555 C40 C39 1.505 1_555 1_555 H53 C40 0.990 1_555 1_555 H54 C40 0.990 1_555 1_555 C41 C40 1.493 1_555 1_555 H55 C41 0.990 1_555 1_555 H56 C41 0.991 1_555 1_555 C42 O4 1.416 1_555 1_555 H57 C42 0.991 1_555 1_555 H58 C42 0.990 1_555 1_555 O5 Na2 2.367 1_555 1_555 C43 O5 1.422 1_555 1_555 H59 C43 0.991 1_555 1_555 H60 C43 0.990 1_555 1_555 C44 C43 1.490 1_555 1_555 H61 C44 0.990 1_555 1_555 H62 C44 0.989 1_555 1_555 C45 C44 1.509 1_555 1_555 H63 C45 0.990 1_555 1_555 H64 C45 0.989 1_555 1_555 C46 O5 1.421 1_555 1_555 H65 C46 0.990 1_555 1_555 H66 C46 0.991 1_555 1_555 O6 Na2 2.341 1_555 1_555 C47 O6 1.416 1_555 1_555 H67 C47 0.990 1_555 1_555 H68 C47 0.990 1_555 1_555 C49 C47 1.493 1_555 1_555 H71 C49 0.990 1_555 1_555 H72 C49 0.991 1_555 1_555 C50 C49 1.510 1_555 1_555 H73 C50 0.990 1_555 1_555 H74 C50 0.990 1_555 1_555 C51 O6 1.427 1_555 1_555 H75 C51 0.990 1_555 1_555 H76 C51 0.989 1_555 1_555 O7 C52 1.409 1_555 1_555 C52 H77 0.990 1_555 1_555 H78 C52 0.989 1_555 1_555 C53 C52 1.462 1_555 1_555 H79 C53 0.989 1_555 1_555 H80 C53 0.990 1_555 1_555 C54 C53 1.554 1_555 1_555 H81 C54 0.991 1_555 1_555 H82 C54 0.990 1_555 1_555 C55 O7 1.358 1_555 1_555 H83 C55 0.991 1_555 1_555 H84 C55 0.989 1_555 1_555 O1A Na1 2.366 1_555 1_555 O2A Na1 2.392 1_555 1_555 O3A Na1 2.376 1_555 1_555 C23A O1A 1.422 1_555 1_555 C26A O1A 1.431 1_555 1_555 C27A O2A 1.411 1_555 1_555 C30A O2A 1.430 1_555 1_555 C34A O3A 1.429 1_555 1_555 C37A O3A 1.388 1_555 1_555 H19A C23A 0.990 1_555 1_555 H20A C23A 0.989 1_555 1_555 C24A C23A 1.493 1_555 1_555 C25A C26A 1.503 1_555 1_555 H25A C26A 0.989 1_555 1_555 H26A C26A 0.991 1_555 1_555 H27A C27A 0.988 1_555 1_555 H28A C27A 0.990 1_555 1_555 C28A C27A 1.461 1_555 1_555 C29A C30A 1.484 1_555 1_555 H33A C30A 0.989 1_555 1_555 H34A C30A 0.991 1_555 1_555 H41A C34A 0.990 1_555 1_555 H42A C34A 0.990 1_555 1_555 C35A C34A 1.490 1_555 1_555 C36A C37A 1.438 1_555 1_555 H47A C37A 0.989 1_555 1_555 H48A C37A 0.990 1_555 1_555 H21A C24A 0.990 1_555 1_555 H22A C24A 0.989 1_555 1_555 H23A C25A 0.989 1_555 1_555 H24A C25A 0.990 1_555 1_555 H29A C28A 0.990 1_555 1_555 H30A C28A 0.989 1_555 1_555 H31A C29A 0.990 1_555 1_555 H32A C29A 0.990 1_555 1_555 H43A C35A 0.989 1_555 1_555 H44A C35A 0.990 1_555 1_555 H45A C36A 0.990 1_555 1_555 H46A C36A 0.990 1_555 1_555 O4A Na2 2.397 1_555 1_555 O5A Na2 2.367 1_555 1_555 O6A Na2 2.341 1_555 1_555 C39A O4A 1.435 1_555 1_555 C42A O4A 1.416 1_555 1_555 C43A O5A 1.422 1_555 1_555 C46A O5A 1.421 1_555 1_555 C47A O6A 1.416 1_555 1_555 C51A O6A 1.427 1_555 1_555 H51A C39A 0.990 1_555 1_555 H52A C39A 0.990 1_555 1_555 C40A C39A 1.505 1_555 1_555 C41A C42A 1.520 1_555 1_555 H57A C42A 0.991 1_555 1_555 H58A C42A 0.990 1_555 1_555 H59A C43A 0.991 1_555 1_555 H60A C43A 0.990 1_555 1_555 C44A C43A 1.490 1_555 1_555 C45A C46A 1.500 1_555 1_555 H65A C46A 0.990 1_555 1_555 H66A C46A 0.991 1_555 1_555 H67A C47A 0.990 1_555 1_555 H68A C47A 0.990 1_555 1_555 C49A C47A 1.493 1_555 1_555 C50A C51A 1.509 1_555 1_555 H75A C51A 0.990 1_555 1_555 H76A C51A 0.989 1_555 1_555 H53A C40A 0.990 1_555 1_555 H54A C40A 0.990 1_555 1_555 H55A C41A 0.990 1_555 1_555 H56A C41A 0.991 1_555 1_555 H61A C44A 0.990 1_555 1_555 H62A C44A 0.989 1_555 1_555 H63A C45A 0.990 1_555 1_555 H64A C45A 0.989 1_555 1_555 H71A C49A 0.990 1_555 1_555 H72A C49A 0.991 1_555 1_555 H73A C50A 0.990 1_555 1_555 H74A C50A 0.990 1_555 1_555 C6 N1 1.344 1_555 1_555 C7 N2 1.372 1_555 1_555 C11 N2 1.346 1_555 1_555 C13 N3 1.364 1_555 1_555 C17 N3 1.348 1_555 1_555 C18 N4 1.362 1_555 1_555 C22 N4 1.341 1_555 1_555 C25 C26 1.503 1_555 1_555 C29 C30 1.484 1_555 1_555 C36 C37 1.438 1_555 1_555 C41 C42 1.520 1_555 1_555 C45 C46 1.500 1_555 1_555 C50 C51 1.509 1_555 1_555 C54 C55 1.460 1_555 1_555 C24A C25A 1.510 1_555 1_555 C28A C29A 1.501 1_555 1_555 C35A C36A 1.517 1_555 1_555 C40A C41A 1.493 1_555 1_555 C44A C45A 1.509 1_555 1_555 C49A C50A 1.510 1_555 1_555 #END data_CSD_CIF_SURLOG _audit_creation_date 1996-01-18 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD SURLOG _chemical_formula_sum 'C16 H28 Li1 N3 S1' _chemical_formula_moiety ; C6 H18 N3 S1 1+,C10 H10 Li1 1- ; _journal_coden_Cambridge 179 _journal_volume 34 _journal_year 1995 _journal_page_first 2376 _journal_name_full 'Angew.Chem.,Int.Ed. ' loop_ _publ_author_name "J.Wessel" "E.Lork" "R.Mews" _chemical_name_systematic ; tris(Dimethylamino)sulfonium bis(\h^5^-cyclopentadienyl)-lithium ; _chemical_name_common ; tris(Dimethylamino)sulfonium lithiocenide ; _chemical_melting_point 380.15 _cell_volume 917.794 _exptl_crystal_colour 'red' _exptl_crystal_density_diffrn 1.091 _diffrn_ambient_temperature 173 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_gt 0.0364 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 7.754(1) _cell_length_b 8.175(1) _cell_length_c 16.400(2) _cell_angle_alpha 81.98(1) _cell_angle_beta 85.46(1) _cell_angle_gamma 63.09(1) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.28 N 0.68 S 1.02 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z S1 S 0.40676(8) 0.48936(7) 0.73005(4) N1 N 0.6230(2) 0.4877(2) 0.74046(10) C1 C 0.7496(3) 0.4330(3) 0.66661(15) H1 H 0.7578(16) 0.3171(10) 0.6524(5) H2 H 0.8792(6) 0.4157(19) 0.6782(3) H3 H 0.6956(11) 0.5299(9) 0.6204(3) C2 C 0.6052(3) 0.6639(3) 0.76184(15) H4 H 0.5232(17) 0.697(1) 0.8114(5) H5 H 0.5466(19) 0.7610(5) 0.7161(4) H6 H 0.7337(4) 0.6510(6) 0.7723(9) N2 N 0.3171(2) 0.5458(2) 0.81982(11) C3 C 0.4157(3) 0.4517(4) 0.89801(14) H7 H 0.5559(4) 0.4031(17) 0.8892(2) H8 H 0.3840(16) 0.3496(13) 0.9180(5) H9 H 0.3729(16) 0.5396(6) 0.9389(3) C4 C 0.1042(3) 0.6224(3) 0.82641(14) H10 H 0.0481(3) 0.6807(17) 0.7723(2) H11 H 0.0547(3) 0.7145(14) 0.8655(6) H12 H 0.0685(3) 0.5226(4) 0.8458(8) N3 N 0.4845(3) 0.2725(2) 0.72015(12) C5 C 0.6133(4) 0.1201(3) 0.7785(2) H13 H 0.6959(15) 0.1594(7) 0.8044(7) H14 H 0.6943(15) 0.0135(8) 0.7490(2) H15 H 0.5356(4) 0.0856(13) 0.8210(5) C6 C 0.3670(4) 0.2277(3) 0.6710(2) H16 H 0.2826(15) 0.3386(5) 0.6358(7) H17 H 0.2879(15) 0.1821(18) 0.7075(2) H18 H 0.4515(4) 0.1321(14) 0.6365(6) C7 C 0.2779(4) 0.7261(3) 0.5344(2) C8 C 0.1170(4) 0.6936(3) 0.5515(2) C9 C 0.0066(4) 0.8025(3) 0.6122(2) C10 C 0.0989(4) 0.9022(3) 0.6326(2) C11 C 0.2663(4) 0.8545(3) 0.58412(15) C12 C 0.0119(3) 0.2016(3) 0.8848(2) C13 C 0.1681(3) 0.0289(3) 0.8768(2) C14 C 0.2871(4) -0.0155(4) 0.9433(2) C15 C 0.2074(4) 0.1268(4) 0.9921(2) C16 C 0.0355(4) 0.2626(3) 0.9562(2) Li1 Li 0.00000 1.00000 0.50000 Li2 Li 0.00000 0.00000 1.00000 H19 H 0.3721(32) 0.6711(28) 0.4928(13) H20 H 0.0972(31) 0.6171(31) 0.5218(13) H21 H -0.1057(35) 0.8042(29) 0.6324(13) H22 H 0.0651(31) 0.9843(31) 0.6741(14) H23 H 0.3589(32) 0.9031(28) 0.5832(12) H24 H -0.0877(35) 0.2681(30) 0.8448(14) H25 H 0.1887(29) -0.0450(28) 0.8318(13) H26 H 0.4117(43) -0.1304(40) 0.9523(16) H27 H 0.2563(37) 0.1308(33) 1.0414(16) H28 H -0.0447(38) 0.3754(37) 0.9774(15) C7A C -0.2779(4) 1.2739(3) 0.4656(2) C8A C -0.1170(4) 1.3064(3) 0.4485(2) C9A C -0.0066(4) 1.1975(3) 0.3878(2) C10A C -0.0989(4) 1.0978(3) 0.3674(2) C11A C -0.2663(4) 1.1455(3) 0.41588(15) H19A H -0.3721(32) 1.3289(28) 0.5072(13) H20A H -0.0972(31) 1.3829(31) 0.4782(13) H21A H 0.1057(35) 1.1958(29) 0.3676(13) H22A H -0.0651(31) 1.0157(31) 0.3259(14) H23A H -0.3589(32) 1.0969(28) 0.4168(12) C12A C -0.0119(3) -0.2016(3) 1.1152(2) C13A C -0.1681(3) -0.0289(3) 1.1232(2) C14A C -0.2871(4) 0.0155(4) 1.0567(2) C15A C -0.2074(4) -0.1268(4) 1.0079(2) C16A C -0.0355(4) -0.2626(3) 1.0438(2) H24A H 0.0877(35) -0.2681(30) 1.1552(14) H25A H -0.1887(29) 0.0450(28) 1.1682(13) H26A H -0.4117(43) 0.1304(40) 1.0477(16) H27A H -0.2563(37) -0.1308(33) 0.9586(16) H28A H 0.0447(38) -0.3754(37) 1.0226(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 S1 N1 1.693 1_555 1_555 N1 C1 1.482 1_555 1_555 C1 H1 0.980 1_555 1_555 H2 C1 0.980 1_555 1_555 H3 C1 0.980 1_555 1_555 C2 N1 1.473 1_555 1_555 H4 C2 0.981 1_555 1_555 H5 C2 0.980 1_555 1_555 H6 C2 0.980 1_555 1_555 N2 S1 1.613 1_555 1_555 C3 N2 1.472 1_555 1_555 H7 C3 0.980 1_555 1_555 H8 C3 0.980 1_555 1_555 H9 C3 0.980 1_555 1_555 C4 N2 1.478 1_555 1_555 H10 C4 0.979 1_555 1_555 H11 C4 0.979 1_555 1_555 H12 C4 0.981 1_555 1_555 N3 S1 1.622 1_555 1_555 C5 N3 1.469 1_555 1_555 H13 C5 0.980 1_555 1_555 H14 C5 0.981 1_555 1_555 H15 C5 0.980 1_555 1_555 C6 N3 1.454 1_555 1_555 H16 C6 0.980 1_555 1_555 H17 C6 0.980 1_555 1_555 H18 C6 0.981 1_555 1_555 C7 C8 1.389 1_555 1_555 C8 C9 1.392 1_555 1_555 C9 C10 1.389 1_555 1_555 C10 C11 1.391 1_555 1_555 C11 C7 1.384 1_555 1_555 C12 C13 1.399 1_555 1_555 C13 C14 1.385 1_555 1_555 C14 C15 1.381 1_555 1_555 C15 C16 1.399 1_555 1_555 C16 C12 1.390 1_555 1_555 Li1 C7 2.334 1_555 1_555 Li2 C12 2.353 1_555 1_555 H19 C7 0.954 1_555 1_555 H20 C8 0.914 1_555 1_555 H21 C9 0.902 1_555 1_555 H22 C10 0.960 1_555 1_555 H23 C11 0.964 1_555 1_555 H24 C12 0.961 1_555 1_555 H25 C13 0.976 1_555 1_555 H26 C14 1.000 1_555 1_555 H27 C15 0.930 1_555 1_555 H28 C16 0.946 1_555 1_555 C7A Li1 2.334 1_555 1_555 C8A Li1 2.299 1_555 1_555 C9A Li1 2.260 1_555 1_555 C10A Li1 2.276 1_555 1_555 C11A Li1 2.313 1_555 1_555 H19A C7A 0.954 1_555 1_555 H20A C8A 0.914 1_555 1_555 H21A C9A 0.902 1_555 1_555 H22A C10A 0.960 1_555 1_555 H23A C11A 0.964 1_555 1_555 C12A Li2 2.353 1_555 1_555 C13A Li2 2.359 1_555 1_555 C14A Li2 2.299 1_555 1_555 C15A Li2 2.262 1_555 1_555 C16A Li2 2.296 1_555 1_555 H24A C12A 0.961 1_555 1_555 H25A C13A 0.976 1_555 1_555 H26A C14A 1.000 1_555 1_555 H27A C15A 0.930 1_555 1_555 H28A C16A 0.946 1_555 1_555 C8 Li1 2.299 1_555 1_555 C9 Li1 2.260 1_555 1_555 C10 Li1 2.276 1_555 1_555 C11 Li1 2.313 1_555 1_555 C13 Li2 2.359 1_555 1_555 C14 Li2 2.299 1_555 1_555 C15 Li2 2.262 1_555 1_555 C16 Li2 2.296 1_555 1_555 C7A C8A 1.389 1_555 1_555 C7A C11A 1.384 1_555 1_555 C8A C9A 1.392 1_555 1_555 C9A C10A 1.389 1_555 1_555 C10A C11A 1.391 1_555 1_555 C12A C13A 1.399 1_555 1_555 C12A C16A 1.390 1_555 1_555 C13A C14A 1.385 1_555 1_555 C14A C15A 1.381 1_555 1_555 C15A C16A 1.399 1_555 1_555 #END data_CSD_CIF_SURLUM _audit_creation_date 1996-01-18 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD SURLUM _chemical_formula_sum 'C27 H51 N6 Na1 S2' _chemical_formula_moiety ; 2(C6 H18 N3 S1 1+),C5 H5 1-,C10 H10 Na1 1- ; _journal_coden_Cambridge 179 _journal_volume 34 _journal_year 1995 _journal_page_first 2376 _journal_name_full 'Angew.Chem.,Int.Ed. ' loop_ _publ_author_name "J.Wessel" "E.Lork" "R.Mews" _chemical_name_systematic ; bis(tris(Dimethylamino)sulfonium) cyclopentadienide bis(\h^5^-cyclopentadienyl)-sodium ; _chemical_name_common ; bis(tris(Dimethylamino)sulfonium) cyclopentadienide sodiocenide ; _chemical_melting_point 358.15 _cell_volume 802.554 _exptl_crystal_colour 'violet' _exptl_crystal_density_diffrn 1.131 _diffrn_ambient_temperature 173 _refine_special_details ; The enclosed cyclopentadienide is crystallographically disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_gt 0.0642 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 8.067(1) _cell_length_b 8.283(1) _cell_length_c 14.470(2) _cell_angle_alpha 92.48(1) _cell_angle_beta 104.40(1) _cell_angle_gamma 119.12(1) _cell_formula_units_Z 1 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 N 0.68 Na 1.56 S 1.02 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z S1 S 0.38654(8) 0.81343(8) 0.67656(4) N1 N 0.1789(3) 0.8049(3) 0.68789(15) C1 C 0.0004(4) 0.6854(4) 0.6039(2) H1 H -0.0220(19) 0.5576(9) 0.5944(10) H2 H 0.0202(14) 0.7377(17) 0.5455(4) H3 H -0.1158(7) 0.6811(25) 0.6160(7) C2 C 0.2054(4) 0.9931(4) 0.7106(2) H4 H 0.3249(19) 1.0700(11) 0.7665(10) H5 H 0.0884(15) 0.9800(4) 0.7260(16) H6 H 0.2204(32) 1.0541(13) 0.6542(6) N2 N 0.5390(3) 0.9386(3) 0.78347(15) C3 C 0.7512(4) 1.0237(4) 0.7902(2) H7 H 0.7665(6) 1.0407(28) 0.7256(3) H8 H 0.7991(9) 0.9408(15) 0.8150(15) H9 H 0.8292(6) 1.1464(14) 0.8346(12) C4 C 0.4961(5) 0.9006(5) 0.8755(2) H10 H 0.3519(6) 0.8381(28) 0.8641(3) H11 H 0.5637(27) 1.0196(6) 0.9222(6) H12 H 0.5443(30) 0.8187(25) 0.9018(8) N3 N 0.3056(4) 0.5875(3) 0.6666(2) C5 C 0.4188(5) 0.5286(4) 0.6241(2) H13 H 0.4773(27) 0.6143(18) 0.5816(13) H14 H 0.3296(8) 0.4001(12) 0.5861(13) H15 H 0.5254(21) 0.532(3) 0.6762(2) C6 C 0.2221(5) 0.4775(4) 0.7375(3) H16 H 0.1481(28) 0.5251(21) 0.7620(12) H17 H 0.3307(6) 0.4895(25) 0.7917(8) H18 H 0.1319(26) 0.3447(7) 0.7059(5) Na1 Na 1.00000 0.50000 1.00000 C7 C 0.8933(4) 0.6367(4) 0.8509(2) H19 H 0.9691(51) 0.6636(47) 0.8087(26) C8 C 0.7235(4) 0.4615(4) 0.8429(2) H20 H 0.6561(52) 0.345(5) 0.7916(26) C9 C 0.6589(5) 0.4778(6) 0.9231(3) H21 H 0.5358(78) 0.3692(72) 0.9264(39) C10 C 0.7883(6) 0.6598(6) 0.9787(3) H22 H 0.7705(73) 0.7045(68) 1.0409(38) C11 C 0.9322(5) 0.7567(4) 0.9343(2) H23 H 1.0333(61) 0.8829(58) 0.9582(30) C12? C 0.3993(28) 1.0653(21) 0.5092(10) H24? H 0.3029(47) 1.1069(43) 0.5045(18) C13? C 0.6013(26) 1.1386(12) 0.5516(5) H25? H 0.6812(47) 1.2543(16) 0.5994(7) C14? C 0.6480(14) 1.0102(32) 0.5205(11) H26? H 0.7743(17) 1.0519(50) 0.5518(16) C15? C 0.4749(32) 0.8576(16) 0.4590(8) H27? H 0.4388(56) 0.7434(22) 0.4209(13) C16? C 0.3212(9) 0.8917(17) 0.4520(5) H28? H 0.2053(13) 0.8275(31) 0.4143(9) C7A C 1.1067(4) 0.3633(4) 1.1491(2) C8A C 1.2765(4) 0.5385(4) 1.1571(2) C9A C 1.3411(5) 0.5222(6) 1.0769(3) C10A C 1.2117(6) 0.3402(6) 1.0213(3) C11A C 1.0678(5) 0.2433(4) 1.0657(2) H19A H 1.0309(51) 0.3364(47) 1.1913(26) H20A H 1.3439(52) 0.655(5) 1.2084(26) H21A H 1.4642(78) 0.6308(72) 1.0736(39) H22A H 1.2295(73) 0.2955(68) 0.9591(38) H23A H 0.9667(61) 0.1171(58) 1.0418(30) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 S1 N1 1.691 1_555 1_555 N1 C1 1.473 1_555 1_555 C1 H1 0.980 1_555 1_555 H2 C1 0.979 1_555 1_555 H3 C1 0.980 1_555 1_555 C2 N1 1.477 1_555 1_555 H4 C2 0.979 1_555 1_555 H5 C2 0.979 1_555 1_555 H6 C2 0.980 1_555 1_555 N2 S1 1.629 1_555 1_555 C3 N2 1.474 1_555 1_555 H7 C3 0.980 1_555 1_555 H8 C3 0.980 1_555 1_555 H9 C3 0.981 1_555 1_555 C4 N2 1.467 1_555 1_555 H10 C4 0.980 1_555 1_555 H11 C4 0.981 1_555 1_555 H12 C4 0.981 1_555 1_555 N3 S1 1.640 1_555 1_555 C5 N3 1.462 1_555 1_555 H13 C5 0.980 1_555 1_555 H14 C5 0.980 1_555 1_555 H15 C5 0.980 1_555 1_555 C6 N3 1.471 1_555 1_555 H16 C6 0.980 1_555 1_555 H17 C6 0.979 1_555 1_555 H18 C6 0.980 1_555 1_555 Na1 C7 2.629 1_555 1_555 C7 H19 0.928 1_555 1_555 C8 Na1 2.640 1_555 1_555 H20 C8 1.002 1_555 1_555 C9 Na1 2.610 1_555 1_555 H21 C9 0.977 1_555 1_555 C10 Na1 2.596 1_555 1_555 H22 C10 1.027 1_555 1_555 C11 Na1 2.602 1_555 1_555 H23 C11 0.936 1_555 1_555 C7A Na1 2.629 1_555 1_555 C8A Na1 2.640 1_555 1_555 C9A Na1 2.610 1_555 1_555 C10A Na1 2.596 1_555 1_555 C11A Na1 2.602 1_555 1_555 H19A C7A 0.928 1_555 1_555 H20A C8A 1.002 1_555 1_555 H21A C9A 0.977 1_555 1_555 H22A C10A 1.027 1_555 1_555 H23A C11A 0.936 1_555 1_555 C7 C8 1.403 1_555 1_555 C7 C11 1.395 1_555 1_555 C8 C9 1.411 1_555 1_555 C9 C10 1.398 1_555 1_555 C10 C11 1.383 1_555 1_555 C7A C8A 1.403 1_555 1_555 C7A C11A 1.395 1_555 1_555 C8A C9A 1.411 1_555 1_555 C9A C10A 1.398 1_555 1_555 C10A C11A 1.383 1_555 1_555 #END data_CSD_CIF_TAFJOZ _audit_creation_date 1991-05-01 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD TAFJOZ _chemical_formula_sum 'C18 H44 Li2 N7 Na1' _chemical_formula_moiety ; C18 H44 Li2 N7 1+,Na1 1- ; _journal_coeditor_code "IUCr CR0153" _journal_coden_Cambridge 591 _journal_volume 46 _journal_year 1990 _journal_page_first 1835 _journal_name_full 'Acta Crystallogr.,Sect.C:Cryst.Struct.Commun. ' loop_ _publ_author_name "R.H.Huang" "D.L.Ward" "J.L.Dye" _chemical_name_systematic ; (\m~2~-1,4-Dimethyl-1,4,7-triazacyclononamido) (methylamine)(1,4,7-trimethyl-1,4,7-triazacyclo-nonane) dilithium natride ; _cell_volume 5942.619 _exptl_crystal_density_diffrn 0.884 _diffrn_ambient_temperature 203 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.078 _refine_ls_wR_factor_gt 0.078 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,z 3 x,1/2-y,1/2+z 4 1/2-x,-y,1/2+z 5 -x,-y,-z 6 -1/2+x,-1/2-y,-z 7 -x,-1/2+y,-1/2-z 8 -1/2+x,y,-1/2-z _cell_length_a 25.271(8) _cell_length_b 10.904(3) _cell_length_c 21.566(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.08 N 0.68 Na 0.97 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 0.5999(3) 0.6300(8) 0.6043(5) N1 N 0.3412(4) 0.719(1) 0.6417(6) N2 N 0.3157(5) 0.809(1) 0.5160(6) N3 N 0.3901(6) 0.938(1) 0.5924(6) N4 N 0.3180(6) 0.508(2) 0.7641(6) N5 N 0.3841(5) 0.414(1) 0.6698(6) N6 N 0.4259(5) 0.572(1) 0.7616(8) N7 N 0.4442(5) 0.673(1) 0.5184(6) C1 C 0.2925(6) 0.694(2) 0.6125(7) C2 C 0.2735(7) 0.782(2) 0.5627(8) C3 C 0.3260(7) 0.939(2) 0.5067(8) C4 C 0.3447(7) 1.004(2) 0.5617(8) C5 C 0.3862(7) 0.919(2) 0.6584(7) C6 C 0.3408(6) 0.836(1) 0.6765(7) C7 C 0.3055(7) 0.744(2) 0.4589(8) C8 C 0.4392(7) 1.005(2) 0.5774(9) C9 C 0.3091(9) 0.384(2) 0.736(1) C10 C 0.3494(8) 0.336(2) 0.7017(9) C11 C 0.4409(8) 0.408(2) 0.687(1) C12 C 0.4552(8) 0.464(2) 0.743(1) C13 C 0.3952(8) 0.560(2) 0.8209(9) C14 C 0.3481(8) 0.502(2) 0.818(1) C15 C 0.2682(8) 0.571(2) 0.7763(9) C16 C 0.3780(8) 0.392(2) 0.6036(8) C17 C 0.4606(7) 0.671(2) 0.7643(9) C18 C 0.4638(7) 0.746(2) 0.4664(9) Li1 Li 0.364(1) 0.590(3) 0.694(1) Li2 Li 0.382(1) 0.757(3) 0.566(1) H1 H 0.29700 0.61600 0.59300 H2 H 0.26600 0.68800 0.64400 H3 H 0.26100 0.85500 0.58100 H4 H 0.24500 0.74300 0.54100 H5 H 0.35400 0.94200 0.47700 H6 H 0.29600 0.97900 0.49100 H7 H 0.31600 1.00700 0.59100 H8 H 0.35500 1.08500 0.55100 H9 H 0.41800 0.88100 0.67300 H10 H 0.38200 0.99600 0.67800 H11 H 0.30800 0.87600 0.66800 H12 H 0.34300 0.81800 0.72000 H13 H 0.27700 0.77900 0.43700 H14 H 0.33600 0.74400 0.43400 H15 H 0.29700 0.66200 0.47000 H16 H 0.43800 1.08200 0.59800 H17 H 0.46900 0.96000 0.59200 H18 H 0.44200 1.01700 0.53400 H19 H 0.28000 0.39000 0.70900 H20 H 0.30100 0.32900 0.76900 H21 H 0.36900 0.29000 0.73100 H22 H 0.33500 0.28300 0.67100 H23 H 0.46000 0.45200 0.65600 H24 H 0.45100 0.32400 0.68600 H25 H 0.44900 0.40400 0.77400 H26 H 0.49200 0.48300 0.74200 H27 H 0.39000 0.63900 0.83800 H28 H 0.41600 0.51200 0.84900 H29 H 0.35300 0.41800 0.82600 H30 H 0.32700 0.53700 0.84900 H31 H 0.24900 0.52400 0.80600 H32 H 0.24800 0.58100 0.74000 H33 H 0.27600 0.64900 0.79300 H34 H 0.39100 0.31200 0.59400 H35 H 0.39600 0.45100 0.57900 H36 H 0.34100 0.39600 0.59500 H37 H 0.48400 0.66300 0.79800 H38 H 0.44000 0.74300 0.77000 H39 H 0.48000 0.67800 0.72700 H40 H 0.47200 0.65900 0.54700 H41 H 0.43200 0.59800 0.50200 H42 H 0.49200 0.70200 0.44700 H43 H 0.43700 0.76100 0.43700 H44 H 0.47700 0.82200 0.48100 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 N1 C1 1.409 1_555 1_555 N2 C2 1.496 1_555 1_555 N3 C4 1.508 1_555 1_555 N4 C9 1.499 1_555 1_555 N5 C10 1.402 1_555 1_555 N6 C12 1.448 1_555 1_555 N7 C18 1.462 1_555 1_555 C1 C2 1.518 1_555 1_555 C2 H3 0.943 1_555 1_555 C3 N2 1.455 1_555 1_555 C4 C3 1.460 1_555 1_555 C5 N3 1.442 1_555 1_555 C6 N1 1.480 1_555 1_555 C7 N2 1.444 1_555 1_555 C8 N3 1.476 1_555 1_555 C9 C10 1.363 1_555 1_555 C10 H21 0.947 1_555 1_555 C11 N5 1.484 1_555 1_555 C12 C11 1.401 1_555 1_555 C13 N6 1.502 1_555 1_555 C14 N4 1.391 1_555 1_555 C15 N4 1.458 1_555 1_555 C16 N5 1.456 1_555 1_555 C17 N6 1.392 1_555 1_555 C18 H42 0.956 1_555 1_555 Li1 N1 1.893 1_555 1_555 Li2 N1 1.975 1_555 1_555 H1 C1 0.956 1_555 1_555 H2 C1 0.956 1_555 1_555 H4 C2 0.958 1_555 1_555 H5 C3 0.955 1_555 1_555 H6 C3 0.938 1_555 1_555 H7 C4 0.962 1_555 1_555 H8 C4 0.949 1_555 1_555 H9 C5 0.957 1_555 1_555 H10 C5 0.946 1_555 1_555 H11 C6 0.954 1_555 1_555 H12 C6 0.960 1_555 1_555 H13 C7 0.942 1_555 1_555 H14 C7 0.939 1_555 1_555 H15 C7 0.950 1_555 1_555 H16 C8 0.950 1_555 1_555 H17 C8 0.952 1_555 1_555 H18 C8 0.948 1_555 1_555 H19 C9 0.940 1_555 1_555 H20 C9 0.953 1_555 1_555 H22 C10 0.951 1_555 1_555 H23 C11 0.954 1_555 1_555 H24 C11 0.951 1_555 1_555 H25 C12 0.948 1_555 1_555 H26 C12 0.953 1_555 1_555 H27 C13 0.946 1_555 1_555 H28 C13 0.958 1_555 1_555 H29 C14 0.940 1_555 1_555 H30 C14 0.936 1_555 1_555 H31 C15 0.953 1_555 1_555 H32 C15 0.941 1_555 1_555 H33 C15 0.944 1_555 1_555 H34 C16 0.955 1_555 1_555 H35 C16 0.950 1_555 1_555 H36 C16 0.954 1_555 1_555 H37 C17 0.941 1_555 1_555 H38 C17 0.950 1_555 1_555 H39 C17 0.945 1_555 1_555 H40 N7 0.947 1_555 1_555 H41 N7 0.943 1_555 1_555 H43 C18 0.942 1_555 1_555 H44 C18 0.947 1_555 1_555 N2 Li2 2.072 1_555 1_555 N3 Li2 2.064 1_555 1_555 N4 Li1 2.106 1_555 1_555 N5 Li1 2.053 1_555 1_555 N6 Li1 2.147 1_555 1_555 N7 Li2 2.089 1_555 1_555 C5 C6 1.513 1_555 1_555 C13 C14 1.349 1_555 1_555 #END data_CSD_CIF_TAFLAN _audit_creation_date 1991-05-01 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD TAFLAN _chemical_formula_sum 'C18 H36 K1 N2 Na1 O6' _chemical_formula_moiety ; C18 H36 K1 N2 O6 1+,Na1 1- ; _journal_coeditor_code "IUCr CR0152" _journal_coden_Cambridge 591 _journal_volume 46 _journal_year 1990 _journal_page_first 1833 _journal_name_full 'Acta Crystallogr.,Sect.C:Cryst.Struct.Commun. ' loop_ _publ_author_name "D.L.Ward" "R.H.Huang" "J.L.Dye" _chemical_name_systematic ; Cryptand(2.2.2)-potassium natride ; _cell_volume 5500.786 _exptl_crystal_colour 'dark grey' _exptl_crystal_density_diffrn 1.06 _diffrn_ambient_temperature 206 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.021 _refine_ls_wR_factor_gt 0.021 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x,1/2+y,1/2+z 3 1/2+x,y,1/2+z 4 1/2+x,1/2+y,z 5 1/4-x,1/4+y,1/4+z 6 1/4-x,3/4+y,3/4+z 7 3/4-x,1/4+y,3/4+z 8 3/4-x,3/4+y,1/4+z 9 1/4+x,1/4-y,1/4+z 10 1/4+x,3/4-y,3/4+z 11 3/4+x,1/4-y,3/4+z 12 3/4+x,3/4-y,1/4+z 13 1/2-x,-y,1/2+z 14 1/2-x,1/2-y,z 15 -x,-y,z 16 -x,1/2-y,1/2+z _cell_length_a 15.769(7) _cell_length_b 25.245(7) _cell_length_c 13.818(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 K 1.90 N 0.68 Na 0.97 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z K1 K 0.00000 0.00000 0.00000 Na1 Na 0.00000 0.00000 0.4151(1) O1 O -0.0007(1) 0.09556(6) 0.0989(1) O2 O -0.1552(1) 0.04284(6) 0.0677(1) O3 O 0.06218(9) 0.04014(6) -0.1801(1) N1 N 0.1544(1) 0.06749(7) -0.0041(2) C1 C 0.1485(2) 0.10556(9) 0.0771(2) C2 C 0.0643(2) 0.13368(9) 0.0834(2) C3 C -0.0800(2) 0.1207(1) 0.1173(2) C4 C -0.1438(2) 0.0792(1) 0.1457(2) C5 C -0.2226(2) 0.0064(1) 0.0884(2) C6 C 0.2300(1) 0.03334(9) 0.0088(2) C7 C 0.1605(1) 0.09597(9) -0.0963(2) C8 C 0.1457(1) 0.06197(9) -0.1840(2) C9 C 0.0458(1) 0.00877(9) -0.2633(2) H1 H 0.196(12) 0.133(1) 0.074(2) H2 H 0.157(1) 0.0848(9) 0.134(2) H3 H 0.066(2) 0.1558(9) 0.144(2) H4 H 0.051(1) 0.1562(8) 0.023(2) H5 H -0.101(1) 0.1427(8) 0.057(2) H6 H -0.073(1) 0.1455(8) 0.168(2) H7 H -0.126(1) 0.0602(9) 0.205(2) H8 H -0.197(2) 0.095(1) 0.155(2) H9 H -0.277(1) 0.0258(9) 0.095(2) H10 H -0.211(1) -0.0102(8) 0.151(2) H11 H 0.236(1) 0.0137(8) -0.053(2) H12 H 0.283(1) 0.0561(9) 0.021(2) H13 H 0.215(1) 0.1138(9) -0.107(2) H14 H 0.117(1) 0.1218(8) -0.093(2) H15 H 0.151(1) 0.0837(8) -0.241(2) H16 H 0.189(1) 0.0341(9) -0.190(2) H17 H 0.085(1) -0.0222(8) -0.263(2) H18 H 0.053(1) 0.0303(8) -0.327(2) O1N O 0.0007(1) -0.09556(6) 0.0989(1) O2N O 0.1552(1) -0.04284(6) 0.0677(1) O3N O -0.06218(9) -0.04014(6) -0.1801(1) N1N N -0.1544(1) -0.06749(7) -0.0041(2) C6N C -0.2300(1) -0.03334(9) 0.0088(2) C5N C 0.2226(2) -0.0064(1) 0.0884(2) C9N C -0.0458(1) -0.00877(9) -0.2633(2) C2N C -0.0643(2) -0.13368(9) 0.0834(2) C3N C 0.0800(2) -0.1207(1) 0.1173(2) C4N C 0.1438(2) -0.0792(1) 0.1457(2) C8N C -0.1457(1) -0.06197(9) -0.1840(2) C1N C -0.1485(2) -0.10556(9) 0.0771(2) C7N C -0.1605(1) -0.09597(9) -0.0963(2) H11N H -0.236(1) -0.0137(8) -0.053(2) H12N H -0.283(1) -0.0561(9) 0.021(2) H9N H 0.277(1) -0.0258(9) 0.095(2) H10N H 0.211(1) 0.0102(8) 0.151(2) H17N H -0.085(1) 0.0222(8) -0.263(2) H18N H -0.053(1) -0.0303(8) -0.327(2) H3N H -0.066(2) -0.1558(9) 0.144(2) H4N H -0.051(1) -0.1562(8) 0.023(2) H5N H 0.101(1) -0.1427(8) 0.057(2) H6N H 0.073(1) -0.1455(8) 0.168(2) H7N H 0.126(1) -0.0602(9) 0.205(2) H8N H 0.197(2) -0.095(1) 0.155(2) H15N H -0.151(1) -0.0837(8) -0.241(2) H16N H -0.189(1) -0.0341(9) -0.190(2) H1N H -0.196(12) -0.133(1) 0.074(2) H2N H -0.157(1) -0.0848(9) 0.134(2) H13N H -0.215(1) -0.1138(9) -0.107(2) H14N H -0.117(1) -0.1218(8) -0.093(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 K1 O1 2.773 1_555 1_555 O1 C2 1.422 1_555 1_555 O2 K1 2.834 1_555 1_555 O3 K1 2.860 1_555 1_555 N1 K1 2.972 1_555 1_555 C1 N1 1.480 1_555 1_555 C2 C1 1.508 1_555 1_555 C3 O1 1.425 1_555 1_555 C4 O2 1.427 1_555 1_555 C5 O2 1.434 1_555 1_555 C6 N1 1.482 1_555 1_555 C7 N1 1.466 1_555 1_555 C8 O3 1.429 1_555 1_555 C9 O3 1.420 1_555 1_555 H1 C1 1.021 1_555 1_555 H2 C1 0.954 1_555 1_555 H3 C2 1.007 1_555 1_555 H4 C2 1.031 1_555 1_555 H5 C3 1.055 1_555 1_555 H6 C3 0.946 1_555 1_555 H7 C4 0.990 1_555 1_555 H8 C4 0.938 1_555 1_555 H9 C5 0.992 1_555 1_555 H10 C5 0.978 1_555 1_555 H11 C6 0.992 1_555 1_555 H12 C6 1.028 1_555 1_555 H13 C7 0.981 1_555 1_555 H14 C7 0.948 1_555 1_555 H15 C8 0.963 1_555 1_555 H16 C8 0.984 1_555 1_555 H17 C9 0.997 1_555 1_555 H18 C9 1.041 1_555 1_555 O1N K1 2.773 1_555 1_555 O2N K1 2.834 1_555 1_555 O3N K1 2.860 1_555 1_555 N1N K1 2.972 1_555 1_555 C6N C5 1.493 1_555 1_555 C5N C6 1.493 1_555 1_555 C9N C9 1.511 1_555 1_555 C2N O1N 1.422 1_555 1_555 C3N O1N 1.425 1_555 1_555 C4N O2N 1.427 1_555 1_555 C8N O3N 1.429 1_555 1_555 C1N N1N 1.480 1_555 1_555 C7N N1N 1.466 1_555 1_555 H11N C6N 0.992 1_555 1_555 H12N C6N 1.028 1_555 1_555 H9N C5N 0.992 1_555 1_555 H10N C5N 0.978 1_555 1_555 H17N C9N 0.997 1_555 1_555 H18N C9N 1.041 1_555 1_555 H3N C2N 1.007 1_555 1_555 H4N C2N 1.031 1_555 1_555 H5N C3N 1.055 1_555 1_555 H6N C3N 0.946 1_555 1_555 H7N C4N 0.990 1_555 1_555 H8N C4N 0.938 1_555 1_555 H15N C8N 0.963 1_555 1_555 H16N C8N 0.984 1_555 1_555 H1N C1N 1.021 1_555 1_555 H2N C1N 0.954 1_555 1_555 H13N C7N 0.981 1_555 1_555 H14N C7N 0.948 1_555 1_555 C3 C4 1.505 1_555 1_555 C7 C8 1.503 1_555 1_555 O2N C5N 1.434 1_555 1_555 O3N C9N 1.420 1_555 1_555 N1N C6N 1.482 1_555 1_555 C2N C1N 1.508 1_555 1_555 C3N C4N 1.505 1_555 1_555 C8N C7N 1.503 1_555 1_555 #END data_CSD_CIF_TEQLAC _audit_creation_date 1997-02-21 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD TEQLAC _chemical_formula_sum 'C28 H78 B8 Li2 N4 Si4' _chemical_formula_moiety ; C16 H46 B8 Li1 Si4 1-,C12 H32 Li1 N4 1+ ; _journal_coden_Cambridge 4 _journal_volume 118 _journal_year 1996 _journal_page_first 5150 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "N.S.Hosmane" "Jimin Yang" "Hongming Zhang" "J.A.Maguire" _chemical_name_systematic ; bis(Tetramethylethylenediamine)-lithium commo-1,1'-lithia-bis(2,3-bis(trimethylsilyl)-2,3-dicarbahexaborane(5)) ; _chemical_melting_point 423.15 _cell_volume 9739.575 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 0.932 _exptl_special_details ; Melting point range 423.15-425.15K ; _diffrn_ambient_temperature 220 _refine_special_details ; Si3, Si4, C39, C42, H37-H42 were refined at occupancies 0.5279:0.4721. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_gt 0.0738 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_Int_Tables_number 56 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2-y,z 3 1/2+x,-y,1/2-z 4 -x,1/2+y,1/2-z 5 -x,-y,-z 6 -1/2+x,-1/2+y,-z 7 -1/2-x,y,-1/2+z 8 x,-1/2-y,-1/2+z _cell_length_a 12.050(3) _cell_length_b 20.894(4) _cell_length_c 38.684(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.20 B 1.02 Li 1.31 N 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.00000 0.50000 0.00000 Li2 Li 0.25000 0.75000 -0.2436(8) Li3 Li 0.25000 0.25000 -0.1265(7) Li4 Li 0.25000 0.25000 0.1243(7) Si1 Si 0.2046(3) 0.5548(2) 0.0617(1) Si2 Si 0.2726(3) 0.5656(2) -0.0358(1) Si3 Si 0.2260(7) 0.6171(3) -0.1824(2) Si4? Si 0.2090(9) 0.5902(4) -0.2071(2) Si5 Si 0.2178(6) 0.5722(3) -0.2796(2) Si6? Si 0.2309(7) 0.6214(4) -0.3051(2) C1 C 0.1635(8) 0.4993(5) 0.0253(3) C2 C 0.1860(9) 0.5045(6) -0.0124(3) B1 B 0.1565(10) 0.4420(8) -0.0316(4) B2 B 0.1155(11) 0.3870(7) 0.0005(4) B3 B 0.1200(11) 0.4304(7) 0.0357(4) B4 B 0.2338(12) 0.4355(7) 0.0069(4) C3 C 0.1614(10) 0.6624(6) -0.2258(4) C4 C 0.1663(11) 0.6596(7) -0.2635(5) B5 B 0.0890(15) 0.7088(11) -0.2803(4) B6 B 0.0229(11) 0.7454(8) -0.2475(4) B7 B 0.0808(12) 0.7129(7) -0.2126(4) B8 B 0.0373(10) 0.6631(8) -0.2480(5) C5 C 0.1947(11) 0.6411(5) 0.0505(3) C6 C 0.1030(9) 0.5429(6) 0.0975(3) C7 C 0.3466(9) 0.5363(6) 0.0783(3) C8 C 0.3197(11) 0.5306(6) -0.0780(3) C9 C 0.1885(11) 0.6373(5) -0.0460(3) C10 C 0.4017(9) 0.5882(6) -0.0127(3) C11 C 0.1302(13) 0.5713(9) -0.1649(4) C12 C 0.3585(11) 0.5871(7) -0.1947(3) C13 C 0.2569(19) 0.6754(11) -0.1490(5) C14? C 0.1713(31) 0.5131(16) -0.2269(10) C15 C 0.3658(11) 0.5803(7) -0.2895(3) C16 C 0.1414(12) 0.5610(7) -0.3210(3) C17 C 0.1812(20) 0.4986(12) -0.2535(7) C18? C 0.2672(22) 0.6744(12) -0.3409(6) N1 N 0.2347(12) 0.3336(5) -0.1554(4) N2 N 0.3837(11) 0.2864(7) -0.0975(4) C19 C 0.3162(23) 0.3707(10) -0.1386(7) C20 C 0.3943(18) 0.3485(11) -0.1139(8) C21 C 0.2694(16) 0.3305(7) -0.1894(4) C22 C 0.1300(13) 0.3646(7) -0.1550(5) C23 C 0.4861(11) 0.2522(8) -0.0985(4) C24 C 0.3620(16) 0.2994(9) -0.0625(5) N3 N 0.1071(9) 0.2229(6) 0.0971(3) N4 N 0.2324(10) 0.1647(5) 0.1533(3) C25 C 0.0774(15) 0.1645(8) 0.1141(6) C26 C 0.1430(17) 0.1348(8) 0.1348(5) C27 C 0.1257(11) 0.2099(7) 0.0619(4) C28 C 0.0178(10) 0.2680(6) 0.0981(3) C29 C 0.3283(12) 0.1227(6) 0.1526(4) C30 C 0.2030(13) 0.1705(6) 0.1888(4) H1 H 0.19690 0.41800 -0.06080 H2 H 0.11600 0.32450 -0.00770 H3 H 0.13130 0.41880 0.06920 H4 H 0.31760 0.40520 0.02230 H5 H 0.04740 0.42190 -0.02200 H6 H 0.08060 0.73170 -0.31490 H7 H -0.05450 0.78510 -0.24640 H8 H 0.06290 0.73800 -0.18070 H9 H -0.05720 0.63850 -0.24010 H10 H 0.09640 0.77430 -0.26850 H11 H 0.12140 0.65070 0.04230 H12 H 0.20970 0.66590 0.07090 H13 H 0.24790 0.65150 0.03300 H14 H 0.10300 0.49890 0.10450 H15 H 0.12330 0.56940 0.11670 H16 H 0.03030 0.55460 0.08960 H17 H 0.35020 0.49150 0.08360 H18 H 0.40040 0.54630 0.06080 H19 H 0.36210 0.56070 0.09880 H20 H 0.25620 0.51810 -0.09140 H21 H 0.36210 0.56160 -0.09070 H22 H 0.36490 0.49380 -0.07340 H23 H 0.12270 0.62400 -0.05800 H24 H 0.16810 0.65890 -0.02510 H25 H 0.23060 0.66580 -0.06040 H26 H 0.38290 0.60710 0.00920 H27 H 0.44590 0.55060 -0.00890 H28 H 0.44310 0.61840 -0.02620 H29 H 0.15030 0.54720 -0.14320 H30 H 0.05870 0.59300 -0.15780 H31 H 0.10200 0.53570 -0.18030 H32? H 0.12970 0.60060 -0.14650 H33? H 0.04570 0.56240 -0.16960 H34? H 0.15100 0.52810 -0.15460 H35 H 0.39900 0.56250 -0.17560 H36 H 0.35480 0.55450 -0.21350 H37 H 0.41100 0.61890 -0.20220 H38? H 0.40910 0.59550 -0.21440 H39? H 0.38200 0.61200 -0.17580 H40? H 0.37990 0.54060 -0.18830 H41 H 0.28460 0.65460 -0.12810 H42 H 0.31260 0.70370 -0.15750 H43 H 0.19160 0.69950 -0.14270 H44? H 0.20490 0.51260 -0.24670 H45? H 0.19840 0.47710 -0.21100 H46? H 0.09310 0.51140 -0.22600 H47 H 0.40010 0.53950 -0.29750 H48 H 0.38230 0.61130 -0.30770 H49 H 0.41070 0.59330 -0.26940 H50? H 0.40740 0.56000 -0.30920 H51? H 0.42020 0.61200 -0.28030 H52? H 0.35560 0.54840 -0.27260 H53 H 0.15480 0.51860 -0.33170 H54 H 0.05800 0.56110 -0.31720 H55 H 0.15490 0.59260 -0.33820 H56? H 0.06840 0.57930 -0.32950 H57? H 0.17030 0.53800 -0.34120 H58? H 0.12040 0.52920 -0.30410 H59 H 0.21200 0.46260 -0.26430 H60 H 0.21580 0.50430 -0.23060 H61 H 0.10330 0.49460 -0.25030 H62? H 0.20110 0.69530 -0.34890 H63? H 0.31930 0.70680 -0.33310 H64? H 0.30040 0.65110 -0.35960 H65 H 0.27220 0.39850 -0.12440 H66 H 0.35270 0.39720 -0.15540 H67 H 0.45980 0.34460 -0.12790 H68 H 0.41070 0.37940 -0.09630 H69 H 0.26010 0.37070 -0.20110 H70 H 0.34620 0.31830 -0.19000 H71 H 0.22560 0.29830 -0.20070 H72 H 0.13030 0.40270 -0.16890 H73 H 0.07790 0.33450 -0.16440 H74 H 0.10890 0.37520 -0.13180 H75 H 0.54150 0.27270 -0.08460 H76 H 0.47420 0.20940 -0.09040 H77 H 0.51080 0.25090 -0.12210 H78 H 0.42400 0.31640 -0.04990 H79 H 0.30090 0.32880 -0.06120 H80 H 0.34050 0.25910 -0.05270 H81 H 0.05490 0.13590 0.09600 H82 H 0.01200 0.17390 0.12740 H83 H 0.09730 0.11370 0.15160 H84 H 0.17690 0.10190 0.12100 H85 H 0.05830 0.19810 0.05040 H86 H 0.15630 0.24740 0.05120 H87 H 0.17810 0.17540 0.06040 H88 H -0.04330 0.25190 0.08470 H89 H -0.00520 0.27370 0.12160 H90 H 0.04140 0.30840 0.08870 H91 H 0.31470 0.08490 0.16600 H92 H 0.34390 0.11100 0.12910 H93 H 0.39070 0.14530 0.16210 H94 H 0.19660 0.12940 0.19980 H95 H 0.25830 0.19540 0.20050 H96 H 0.13290 0.19220 0.18990 C1D C -0.1635(8) 0.5007(5) -0.0253(3) Si1D Si -0.2046(3) 0.4452(2) -0.0617(1) C5D C -0.1947(11) 0.3589(5) -0.0505(3) H11D H -0.12140 0.34930 -0.04230 H12D H -0.20970 0.33410 -0.07090 H13D H -0.24790 0.34850 -0.03300 C6D C -0.1030(9) 0.4571(6) -0.0975(3) H14D H -0.10300 0.50110 -0.10450 H15D H -0.12330 0.43060 -0.11670 H16D H -0.03030 0.44540 -0.08960 C7D C -0.3466(9) 0.4637(6) -0.0783(3) H17D H -0.35020 0.50850 -0.08360 H18D H -0.40040 0.45370 -0.06080 H19D H -0.36210 0.43930 -0.09880 C2D C -0.1860(9) 0.4955(6) 0.0124(3) B1D B -0.1565(10) 0.5580(8) 0.0316(4) Si2D Si -0.2726(3) 0.4344(2) 0.0358(1) C8D C -0.3197(11) 0.4694(6) 0.0780(3) H20D H -0.25620 0.48190 0.09140 H21D H -0.36210 0.43840 0.09070 H22D H -0.36490 0.50620 0.07340 C9D C -0.1885(11) 0.3627(5) 0.0460(3) H23D H -0.12270 0.37600 0.05800 H24D H -0.16810 0.34110 0.02510 H25D H -0.23060 0.33420 0.06040 C10D C -0.4017(9) 0.4118(6) 0.0127(3) H26D H -0.38290 0.39290 -0.00920 H27D H -0.44590 0.44940 0.00890 H28D H -0.44310 0.38160 0.02620 B4D B -0.2338(12) 0.5645(7) -0.0069(4) B3D B -0.1200(11) 0.5696(7) -0.0357(4) B2D B -0.1155(11) 0.6130(7) -0.0005(4) H4D H -0.31760 0.59480 -0.02230 H3D H -0.13130 0.58120 -0.06920 H2D H -0.11600 0.67550 0.00770 H5D H -0.04740 0.57810 0.02200 H1D H -0.19690 0.58200 0.06080 C3A C 0.3386(10) 0.8376(6) -0.2258(4) Si3A Si 0.2740(7) 0.8829(3) -0.1824(2) C11A C 0.3698(13) 0.9287(9) -0.1649(4) H29A H 0.34970 0.95280 -0.14320 H30A H 0.44130 0.90700 -0.15780 H31A H 0.39800 0.96430 -0.18030 C12A C 0.1415(11) 0.9129(7) -0.1947(3) H35A H 0.10100 0.93750 -0.17560 H36A H 0.14520 0.94550 -0.21350 H37A H 0.08900 0.88110 -0.20220 C13A C 0.2431(19) 0.8246(11) -0.1490(5) H41A H 0.21540 0.84540 -0.12810 H42A H 0.18740 0.79630 -0.15750 H43A H 0.30840 0.80050 -0.14270 C4A C 0.3337(11) 0.8404(7) -0.2635(5) B5A B 0.4110(15) 0.7912(11) -0.2803(4) Si5A Si 0.2822(6) 0.9278(3) -0.2796(2) C15A C 0.1342(11) 0.9197(7) -0.2895(3) H47A H 0.09990 0.96050 -0.29750 H48A H 0.11770 0.88870 -0.30770 H49A H 0.08930 0.90670 -0.26940 C16A C 0.3586(12) 0.9390(7) -0.3210(3) H53A H 0.34520 0.98140 -0.33170 H54A H 0.44200 0.93890 -0.31720 H55A H 0.34510 0.90740 -0.33820 C17A C 0.3188(20) 1.0014(12) -0.2535(7) H59A H 0.28800 1.03740 -0.26430 H60A H 0.28420 0.99570 -0.23060 H61A H 0.39670 1.00540 -0.25030 B8A B 0.4627(10) 0.8369(8) -0.2480(5) B7A B 0.4192(12) 0.7871(7) -0.2126(4) B6A B 0.4771(11) 0.7546(8) -0.2475(4) H9A H 0.55720 0.86150 -0.24010 H8A H 0.43710 0.76200 -0.18070 H7A H 0.55450 0.71490 -0.24640 H10A H 0.40360 0.72570 -0.26850 H6A H 0.41940 0.76830 -0.31490 N1A N 0.2653(12) 0.1664(5) -0.1554(4) C19A C 0.1838(23) 0.1293(10) -0.1386(7) C20A C 0.1057(18) 0.1515(11) -0.1139(8) N2A N 0.1163(11) 0.2136(7) -0.0975(4) C23A C 0.0139(11) 0.2478(8) -0.0985(4) H75A H -0.04150 0.22730 -0.08460 H76A H 0.02580 0.29060 -0.09040 H77A H -0.01080 0.24910 -0.12210 C24A C 0.1380(16) 0.2006(9) -0.0625(5) H78A H 0.07600 0.18360 -0.04990 H79A H 0.19910 0.17120 -0.06120 H80A H 0.15950 0.24090 -0.05270 H67A H 0.04020 0.15540 -0.12790 H68A H 0.08930 0.12060 -0.09630 H65A H 0.22780 0.10150 -0.12440 H66A H 0.14730 0.10280 -0.15540 C21A C 0.2306(16) 0.1695(7) -0.1894(4) H69A H 0.23990 0.12930 -0.20110 H70A H 0.15380 0.18170 -0.19000 H71A H 0.27440 0.20170 -0.20070 C22A C 0.3700(13) 0.1354(7) -0.1550(5) H72A H 0.36970 0.09730 -0.16890 H73A H 0.42210 0.16550 -0.16440 H74A H 0.39110 0.12480 -0.13180 N3A N 0.3929(9) 0.2771(6) 0.0971(3) C25A C 0.4226(15) 0.3355(8) 0.1141(6) C26A C 0.3570(17) 0.3652(8) 0.1348(5) N4A N 0.2676(10) 0.3353(5) 0.1533(3) C29A C 0.1717(12) 0.3773(6) 0.1526(4) H91A H 0.18530 0.41510 0.16600 H92A H 0.15610 0.38900 0.12910 H93A H 0.10930 0.35470 0.16210 C30A C 0.2970(13) 0.3295(6) 0.1888(4) H94A H 0.30340 0.37060 0.19980 H95A H 0.24170 0.30460 0.20050 H96A H 0.36710 0.30780 0.18990 H83A H 0.40270 0.38630 0.15160 H84A H 0.32310 0.39810 0.12100 H81A H 0.44510 0.36410 0.09600 H82A H 0.48800 0.32610 0.12740 C27A C 0.3743(11) 0.2901(7) 0.0619(4) H85A H 0.44170 0.30190 0.05040 H86A H 0.34370 0.25260 0.05120 H87A H 0.32190 0.32460 0.06040 C28A C 0.4822(10) 0.2320(6) 0.0981(3) H88A H 0.54330 0.24810 0.08470 H89A H 0.50520 0.22630 0.12160 H90A H 0.45860 0.19160 0.08870 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 C1 2.200 1_555 1_555 Li2 C3 2.228 1_555 1_555 Li3 N1 2.082 1_555 1_555 Li4 N3 2.096 1_555 1_555 Si1 C1 1.890 1_555 1_555 Si2 C2 1.881 1_555 1_555 Si3 C3 2.079 1_555 1_555 Si5 C4 2.027 1_555 1_555 C1 C2 1.487 1_555 1_555 C2 Li1 2.294 1_555 1_555 B1 Li1 2.553 1_555 1_555 B2 Li1 2.741 1_555 1_555 B3 Li1 2.472 1_555 1_555 B4 C1 1.732 1_555 1_555 C3 C4 1.461 1_555 1_555 C4 Li2 2.275 1_555 1_555 B5 Li2 2.554 1_555 1_555 B6 Li2 2.742 1_555 1_555 B7 Li2 2.489 1_555 1_555 B8 C3 1.725 1_555 1_555 C5 Si1 1.858 1_555 1_555 C6 Si1 1.865 1_555 1_555 C7 Si1 1.868 1_555 1_555 C8 Si2 1.877 1_555 1_555 C9 Si2 1.851 1_555 1_555 C10 Si2 1.855 1_555 1_555 C11 Si3 1.645 1_555 1_555 C12 Si3 1.780 1_555 1_555 C13 Si3 1.814 1_555 1_555 C15 Si5 1.832 1_555 1_555 C16 Si5 1.862 1_555 1_555 C17 Si5 1.892 1_555 1_555 N1 C19 1.410 1_555 1_555 N2 Li3 2.105 1_555 1_555 C19 C20 1.419 1_555 1_555 C20 N2 1.450 1_555 1_555 C21 N1 1.382 1_555 1_555 C22 N1 1.418 1_555 1_555 C23 N2 1.426 1_555 1_555 C24 N2 1.405 1_555 1_555 N3 C25 1.432 1_555 1_555 N4 Li4 2.117 1_555 1_555 C25 C26 1.285 1_555 1_555 C26 N4 1.436 1_555 1_555 C27 N3 1.406 1_555 1_555 C28 N3 1.431 1_555 1_555 C29 N4 1.451 1_555 1_555 C30 N4 1.423 1_555 1_555 H1 B1 1.328 1_555 1_555 H2 B2 1.344 1_555 1_555 H3 B3 1.325 1_555 1_555 H4 B4 1.332 1_555 1_555 H5 B1 1.429 1_555 1_555 H6 B5 1.425 1_555 1_555 H7 B6 1.249 1_555 1_555 H8 B7 1.358 1_555 1_555 H9 B8 1.286 1_555 1_555 H10 B5 1.445 1_555 1_555 H11 C5 0.960 1_555 1_555 H12 C5 0.961 1_555 1_555 H13 C5 0.957 1_555 1_555 H14 C6 0.958 1_555 1_555 H15 C6 0.958 1_555 1_555 H16 C6 0.959 1_555 1_555 H17 C7 0.959 1_555 1_555 H18 C7 0.960 1_555 1_555 H19 C7 0.961 1_555 1_555 H20 C8 0.960 1_555 1_555 H21 C8 0.960 1_555 1_555 H22 C8 0.959 1_555 1_555 H23 C9 0.960 1_555 1_555 H24 C9 0.958 1_555 1_555 H25 C9 0.960 1_555 1_555 H26 C10 0.962 1_555 1_555 H27 C10 0.960 1_555 1_555 H28 C10 0.959 1_555 1_555 H29 C11 1.008 1_555 1_555 H30 C11 1.012 1_555 1_555 H31 C11 1.012 1_555 1_555 H35 C12 1.024 1_555 1_555 H36 C12 0.997 1_555 1_555 H37 C12 0.962 1_555 1_555 H41 C13 0.977 1_555 1_555 H42 C13 0.953 1_555 1_555 H43 C13 0.965 1_555 1_555 H47 C15 0.997 1_555 1_555 H48 C15 0.977 1_555 1_555 H49 C15 0.985 1_555 1_555 H53 C16 0.991 1_555 1_555 H54 C16 1.016 1_555 1_555 H55 C16 0.951 1_555 1_555 H59 C17 0.937 1_555 1_555 H60 C17 0.986 1_555 1_555 H61 C17 0.951 1_555 1_555 H65 C19 0.959 1_555 1_555 H66 C19 0.960 1_555 1_555 H67 C20 0.961 1_555 1_555 H68 C20 0.959 1_555 1_555 H69 C21 0.961 1_555 1_555 H70 C21 0.960 1_555 1_555 H71 C21 0.960 1_555 1_555 H72 C22 0.961 1_555 1_555 H73 C22 0.960 1_555 1_555 H74 C22 0.959 1_555 1_555 H75 C23 0.958 1_555 1_555 H76 C23 0.958 1_555 1_555 H77 C23 0.961 1_555 1_555 H78 C24 0.960 1_555 1_555 H79 C24 0.960 1_555 1_555 H80 C24 0.959 1_555 1_555 H81 C25 0.960 1_555 1_555 H82 C25 0.961 1_555 1_555 H83 C26 0.959 1_555 1_555 H84 C26 0.961 1_555 1_555 H85 C27 0.958 1_555 1_555 H86 C27 0.960 1_555 1_555 H87 C27 0.960 1_555 1_555 H88 C28 0.961 1_555 1_555 H89 C28 0.958 1_555 1_555 H90 C28 0.962 1_555 1_555 H91 C29 0.959 1_555 1_555 H92 C29 0.960 1_555 1_555 H93 C29 0.961 1_555 1_555 H94 C30 0.961 1_555 1_555 H95 C30 0.959 1_555 1_555 H96 C30 0.960 1_555 1_555 C1D Li1 2.200 1_555 1_555 Si1D C1D 1.890 1_555 1_555 C5D Si1D 1.858 1_555 1_555 H11D C5D 0.960 1_555 1_555 H12D C5D 0.961 1_555 1_555 H13D C5D 0.957 1_555 1_555 C6D Si1D 1.865 1_555 1_555 H14D C6D 0.958 1_555 1_555 H15D C6D 0.958 1_555 1_555 H16D C6D 0.959 1_555 1_555 C7D Si1D 1.868 1_555 1_555 H17D C7D 0.959 1_555 1_555 H18D C7D 0.960 1_555 1_555 H19D C7D 0.961 1_555 1_555 C2D Li1 2.294 1_555 1_555 B1D Li1 2.553 1_555 1_555 Si2D C2D 1.881 1_555 1_555 C8D Si2D 1.877 1_555 1_555 H20D C8D 0.960 1_555 1_555 H21D C8D 0.960 1_555 1_555 H22D C8D 0.959 1_555 1_555 C9D Si2D 1.851 1_555 1_555 H23D C9D 0.960 1_555 1_555 H24D C9D 0.958 1_555 1_555 H25D C9D 0.960 1_555 1_555 C10D Si2D 1.855 1_555 1_555 H26D C10D 0.962 1_555 1_555 H27D C10D 0.960 1_555 1_555 H28D C10D 0.959 1_555 1_555 B4D C1D 1.732 1_555 1_555 B3D Li1 2.472 1_555 1_555 B2D Li1 2.741 1_555 1_555 H4D B4D 1.332 1_555 1_555 H3D B3D 1.325 1_555 1_555 H2D B2D 1.344 1_555 1_555 H5D B1D 1.429 1_555 1_555 H1D B1D 1.328 1_555 1_555 C3A Li2 2.228 1_555 1_555 Si3A C3A 2.079 1_555 1_555 C11A Si3A 1.645 1_555 1_555 H29A C11A 1.008 1_555 1_555 H30A C11A 1.012 1_555 1_555 H31A C11A 1.012 1_555 1_555 C12A Si3A 1.780 1_555 1_555 H35A C12A 1.024 1_555 1_555 H36A C12A 0.997 1_555 1_555 H37A C12A 0.962 1_555 1_555 C13A Si3A 1.814 1_555 1_555 H41A C13A 0.977 1_555 1_555 H42A C13A 0.953 1_555 1_555 H43A C13A 0.965 1_555 1_555 C4A Li2 2.275 1_555 1_555 B5A Li2 2.554 1_555 1_555 Si5A C4A 2.027 1_555 1_555 C15A Si5A 1.832 1_555 1_555 H47A C15A 0.997 1_555 1_555 H48A C15A 0.977 1_555 1_555 H49A C15A 0.985 1_555 1_555 C16A Si5A 1.862 1_555 1_555 H53A C16A 0.991 1_555 1_555 H54A C16A 1.016 1_555 1_555 H55A C16A 0.951 1_555 1_555 C17A Si5A 1.892 1_555 1_555 H59A C17A 0.937 1_555 1_555 H60A C17A 0.986 1_555 1_555 H61A C17A 0.951 1_555 1_555 B8A C3A 1.725 1_555 1_555 B7A Li2 2.489 1_555 1_555 B6A Li2 2.742 1_555 1_555 H9A B8A 1.286 1_555 1_555 H8A B7A 1.358 1_555 1_555 H7A B6A 1.249 1_555 1_555 H10A B5A 1.445 1_555 1_555 H6A B5A 1.425 1_555 1_555 N1A Li3 2.082 1_555 1_555 C19A N1A 1.410 1_555 1_555 C20A C19A 1.419 1_555 1_555 N2A Li3 2.105 1_555 1_555 C23A N2A 1.426 1_555 1_555 H75A C23A 0.958 1_555 1_555 H76A C23A 0.958 1_555 1_555 H77A C23A 0.961 1_555 1_555 C24A N2A 1.405 1_555 1_555 H78A C24A 0.960 1_555 1_555 H79A C24A 0.960 1_555 1_555 H80A C24A 0.959 1_555 1_555 H67A C20A 0.961 1_555 1_555 H68A C20A 0.959 1_555 1_555 H65A C19A 0.959 1_555 1_555 H66A C19A 0.960 1_555 1_555 C21A N1A 1.382 1_555 1_555 H69A C21A 0.961 1_555 1_555 H70A C21A 0.960 1_555 1_555 H71A C21A 0.960 1_555 1_555 C22A N1A 1.418 1_555 1_555 H72A C22A 0.961 1_555 1_555 H73A C22A 0.960 1_555 1_555 H74A C22A 0.959 1_555 1_555 N3A Li4 2.096 1_555 1_555 C25A N3A 1.432 1_555 1_555 C26A C25A 1.285 1_555 1_555 N4A Li4 2.117 1_555 1_555 C29A N4A 1.451 1_555 1_555 H91A C29A 0.959 1_555 1_555 H92A C29A 0.960 1_555 1_555 H93A C29A 0.961 1_555 1_555 C30A N4A 1.423 1_555 1_555 H94A C30A 0.961 1_555 1_555 H95A C30A 0.959 1_555 1_555 H96A C30A 0.960 1_555 1_555 H83A C26A 0.959 1_555 1_555 H84A C26A 0.961 1_555 1_555 H81A C25A 0.960 1_555 1_555 H82A C25A 0.961 1_555 1_555 C27A N3A 1.406 1_555 1_555 H85A C27A 0.958 1_555 1_555 H86A C27A 0.960 1_555 1_555 H87A C27A 0.960 1_555 1_555 C28A N3A 1.431 1_555 1_555 H88A C28A 0.961 1_555 1_555 H89A C28A 0.958 1_555 1_555 H90A C28A 0.962 1_555 1_555 C1 B3 1.584 1_555 1_555 C2 B4 1.723 1_555 1_555 C2 B1 1.544 1_555 1_555 B1 B2 1.763 1_555 1_555 B1 B4 1.762 1_555 1_555 B2 H5 1.401 1_555 1_555 B2 B4 1.766 1_555 1_555 B2 B3 1.637 1_555 1_555 B3 B4 1.770 1_555 1_555 C3 B7 1.522 1_555 1_555 C4 B8 1.668 1_555 1_555 C4 B5 1.532 1_555 1_555 B5 B6 1.682 1_555 1_555 B5 B8 1.691 1_555 1_555 B6 H10 1.345 1_555 1_555 B6 B8 1.728 1_555 1_555 B6 B7 1.665 1_555 1_555 B7 B8 1.798 1_555 1_555 C1D C2D 1.487 1_555 1_555 C1D B3D 1.584 1_555 1_555 C2D B4D 1.723 1_555 1_555 C2D B1D 1.544 1_555 1_555 B1D B2D 1.763 1_555 1_555 B1D B4D 1.762 1_555 1_555 B4D B2D 1.766 1_555 1_555 B4D B3D 1.770 1_555 1_555 B3D B2D 1.637 1_555 1_555 B2D H5D 1.401 1_555 1_555 C3A C4A 1.461 1_555 1_555 C3A B7A 1.522 1_555 1_555 C4A B8A 1.668 1_555 1_555 C4A B5A 1.532 1_555 1_555 B5A B6A 1.682 1_555 1_555 B5A B8A 1.691 1_555 1_555 B8A B6A 1.728 1_555 1_555 B8A B7A 1.798 1_555 1_555 B7A B6A 1.665 1_555 1_555 B6A H10A 1.345 1_555 1_555 C20A N2A 1.450 1_555 1_555 C26A N4A 1.436 1_555 1_555 #END data_CSD_CIF_TIWCUZ _audit_creation_date 2014-02-17 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD TIWCUZ _database_code_depnum_ccdc_archive 'CCDC 895864' _chemical_formula_sum 'C10 H12 D4 Co1 K1 N8' _chemical_formula_moiety ; (C6 Co1 K1 N6 2-)n,2n(C2 H6 D2 N1 1+) ; _journal_coden_Cambridge 4 _journal_volume 135 _journal_year 2013 _journal_page_first 5230 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "Wen Zhang" "Heng-Yun Ye" "R.Graf" "H.W.Spiess" "Ye-Feng Yao" "Run-Qiang Zhu" "Ren-Gen Xiong" _chemical_name_systematic ; catena-[bis(N,N-dideuterodiemthylammonium) hexakis(\m~2~-cyano)-potassium-cobalt] ; _cell_volume 796.208 _exptl_crystal_colour 'yellow' _exptl_crystal_density_diffrn 1.462 _exptl_crystal_description 'block' _diffrn_ambient_temperature 280 _refine_special_details ; C3 and C3' disordered over two sites with occupancies 0.59:0.41; N3 and N3' disordered over two sites with occupancies 0.297:0.203. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_gt 0.0487 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/m n c' _symmetry_Int_Tables_number 128 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,z 3 -y,x,z 4 y,-x,z 5 1/2-x,1/2+y,1/2-z 6 1/2+x,1/2-y,1/2-z 7 1/2+y,1/2+x,1/2-z 8 1/2-y,1/2-x,1/2-z 9 -x,-y,-z 10 x,y,-z 11 y,-x,-z 12 -y,x,-z 13 -1/2+x,-1/2-y,-1/2+z 14 -1/2-x,-1/2+y,-1/2+z 15 -1/2-y,-1/2-x,-1/2+z 16 -1/2+y,-1/2+x,-1/2+z _cell_length_a 8.277(5) _cell_length_b 8.277(5) _cell_length_c 11.622(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Co 1.26 D 0.23 K 2.03 N 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Co1 Co 0.00000 1.00000 0.00000 K1 K 0.50000 0.50000 0.00000 C1 C 0.1897(5) 0.8710(5) 0.00000 C2 C 0.00000 1.00000 0.1626(5) N1 N 0.3060(7) 0.7981(7) 0.00000 N2 N 0.00000 1.00000 0.2608(5) C3? C 0.3995(8) 0.1005(8) 0.25000 H1? H 0.334(3) 0.167(3) 0.19890 H2? H 0.329(3) 0.039(3) 0.29760 H3? H 0.463(3) 0.172(3) 0.29760 N3? N 0.50000 0.00000 0.181(3) D1? D 0.56190 0.06190 0.13530 N4? N 0.5650(13) 0.0650(13) 0.25000 C4? C 0.3995(8) 0.1005(8) 0.25000 H4? H 0.3867(8) 0.2180(8) 0.25000 H5? H 0.3495(8) 0.0585(8) 0.18250 H6? H 0.3495(8) 0.0585(8) 0.31750 D2? D 0.61050 0.10950 0.31240 C1A C -0.1897(5) 1.1290(5) 0.00000 N1A N -0.3060(7) 1.2019(7) 0.00000 C1B C 0.1290(5) 0.1897(5) 0.00000 N1B N 0.2019(7) 0.3060(7) 0.00000 C1C C -0.1290(5) 0.8103(5) 0.00000 N1C N -0.2019(7) 0.6940(7) 0.00000 C2H C 0.00000 1.00000 -0.1626(5) N2H N 0.00000 1.00000 -0.2608(5) Co1* Co 0.00000 0.00000 0.00000 K1* K -0.50000 0.50000 0.00000 K1** K -0.50000 1.50000 0.00000 K1D K 0.00000 1.00000 -0.50000 K1D* K 0.00000 1.00000 0.50000 C1B* C 0.1290(5) 1.1897(5) 0.00000 N1A* N 0.6940(7) 0.2019(7) 0.00000 N1C* N 0.7981(7) 0.6940(7) 0.00000 N2D N 0.50000 0.50000 0.2392(5) N2L N 0.50000 0.50000 -0.2392(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Co1 C1 1.899 1_555 1_555 K1 N1 2.944 1_555 1_555 C1 N1 1.136 1_555 1_555 C2 Co1 1.890 1_555 1_555 N2 C2 1.141 1_555 1_555 C1A Co1 1.899 1_555 1_555 N1A C1A 1.136 1_555 1_555 C1B N1B 1.136 1_555 1_555 N1B K1 2.944 1_555 1_555 C1C Co1 1.899 1_555 1_555 N1C C1C 1.136 1_555 1_555 C2H Co1 1.890 1_555 1_555 N2H C2H 1.141 1_555 1_555 Co1* C1B 1.899 1_555 1_555 K1* N1C 2.944 1_555 1_555 K1** N1A 2.944 1_555 1_555 K1D N2H 2.780 1_555 1_555 K1D* N2 2.780 1_555 1_555 C1B* Co1 1.899 1_555 1_555 N1A* K1 2.944 1_555 1_555 N1C* K1 2.944 1_555 1_555 N2D K1 2.780 1_555 1_555 N2L K1 2.780 1_555 1_555 #END data_CSD_CIF_TIWCUZ01 _audit_creation_date 2014-02-17 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD TIWCUZ01 _database_code_depnum_ccdc_archive 'CCDC 895862' _chemical_formula_sum 'C10 H16 Co1 K1 N8' _chemical_formula_moiety ; (C6 Co1 K1 N6 2-)n,2n(C2 H8 N1 1+) ; _journal_coden_Cambridge 4 _journal_volume 135 _journal_year 2013 _journal_page_first 5230 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "Wen Zhang" "Heng-Yun Ye" "R.Graf" "H.W.Spiess" "Ye-Feng Yao" "Run-Qiang Zhu" "Ren-Gen Xiong" _chemical_name_systematic ; catena-[bis(diemthylammonium) hexakis(\m~2~-cyano)-potassium-cobalt] ; _cell_volume 798.546 _exptl_crystal_colour 'yellow' _exptl_crystal_density_diffrn 1.44 _exptl_crystal_description 'block' _diffrn_ambient_temperature 293 _refine_special_details ; C3 and C3' disordered over two sites with occupancies 0.61:0.39; N3 and N3' disordered over two sites with occupancies 0.303:0.197. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_gt 0.0344 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/m n c' _symmetry_Int_Tables_number 128 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,z 3 -y,x,z 4 y,-x,z 5 1/2-x,1/2+y,1/2-z 6 1/2+x,1/2-y,1/2-z 7 1/2+y,1/2+x,1/2-z 8 1/2-y,1/2-x,1/2-z 9 -x,-y,-z 10 x,y,-z 11 y,-x,-z 12 -y,x,-z 13 -1/2+x,-1/2-y,-1/2+z 14 -1/2-x,-1/2+y,-1/2+z 15 -1/2-y,-1/2-x,-1/2+z 16 -1/2+y,-1/2+x,-1/2+z _cell_length_a 8.2895(13) _cell_length_b 8.2895(13) _cell_length_c 11.621(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Co 1.26 K 2.03 N 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Co1 Co 0.00000 1.00000 0.00000 K1 K 0.50000 0.50000 0.00000 C1 C 0.1920(3) 0.8737(3) 0.00000 C2 C 0.00000 1.00000 0.1629(4) N1 N 0.3088(4) 0.8009(4) 0.00000 N2 N 0.00000 1.00000 0.2608(3) C3 C 0.3990(5) 0.1010(5) 0.25000 H1 H 0.38610 0.21800 0.25000 H2 H 0.34900 0.05850 0.18260 H3 H 0.34900 0.05850 0.31750 N3 N 0.5638(10) 0.0638(10) 0.25000 H4 H 0.60930 0.10950 0.31240 C4? C 0.3990(5) 0.1010(5) 0.25000 H5? H 0.33250 0.16730 0.19890 H6? H 0.32760 0.03850 0.29760 H7? H 0.46130 0.17220 0.29760 N4? N 0.50000 0.00000 0.1855(19) H8? H 0.56190 0.06190 0.13970 C1A C -0.1920(3) 1.1263(3) 0.00000 N1A N -0.3088(4) 1.1991(4) 0.00000 C1B C 0.1263(3) 0.1920(3) 0.00000 N1B N 0.1991(4) 0.3088(4) 0.00000 C1C C -0.1263(3) 0.8080(3) 0.00000 N1C N -0.1991(4) 0.6912(4) 0.00000 C2H C 0.00000 1.00000 -0.1629(4) N2H N 0.00000 1.00000 -0.2608(3) Co1* Co 0.00000 0.00000 0.00000 K1* K -0.50000 0.50000 0.00000 K1** K -0.50000 1.50000 0.00000 K1D K 0.00000 1.00000 -0.50000 K1D* K 0.00000 1.00000 0.50000 C1B* C 0.1263(3) 1.1920(3) 0.00000 N1A* N 0.6912(4) 0.1991(4) 0.00000 N1C* N 0.8009(4) 0.6912(4) 0.00000 N2D N 0.50000 0.50000 0.2392(3) N2L N 0.50000 0.50000 -0.2392(3) C3A C 0.6010(5) -0.1010(5) 0.25000 H1A H 0.61390 -0.21800 0.25000 H2A H 0.65100 -0.05850 0.18260 H3A H 0.65100 -0.05850 0.31750 N3A N 0.4362(10) -0.0638(10) 0.25000 H4A H 0.39070 -0.10950 0.31240 H1F H 0.71800 -0.11390 0.25000 H2F H 0.55850 -0.15100 0.31740 H3F H 0.55850 -0.15100 0.18250 H4F H 0.60950 0.10930 0.18760 H1G H 0.28200 0.11390 0.25000 H2G H 0.44150 0.15100 0.31740 H3G H 0.44150 0.15100 0.18250 H4G H 0.39050 -0.10930 0.18760 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Co1 C1 1.905 1_555 1_555 K1 N1 2.955 1_555 1_555 C1 N1 1.141 1_555 1_555 C2 Co1 1.893 1_555 1_555 N2 C2 1.138 1_555 1_555 C3 H1 0.976 1_555 1_555 H2 C3 0.954 1_555 1_555 H3 C3 0.955 1_555 1_555 N3 C3 1.400 1_555 1_555 H4 N3 0.901 1_555 1_555 C1A Co1 1.905 1_555 1_555 N1A C1A 1.141 1_555 1_555 C1B N1B 1.141 1_555 1_555 N1B K1 2.955 1_555 1_555 C1C Co1 1.905 1_555 1_555 N1C C1C 1.141 1_555 1_555 C2H Co1 1.893 1_555 1_555 N2H C2H 1.138 1_555 1_555 Co1* C1B 1.905 1_555 1_555 K1* N1C 2.955 1_555 1_555 K1** N1A 2.955 1_555 1_555 K1D N2H 2.780 1_555 1_555 K1D* N2 2.780 1_555 1_555 C1B* Co1 1.905 1_555 1_555 N1A* K1 2.955 1_555 1_555 N1C* K1 2.955 1_555 1_555 N2D K1 2.780 1_555 1_555 N2L K1 2.780 1_555 1_555 C3A N3 1.400 1_555 1_555 H1A C3A 0.976 1_555 1_555 H2A C3A 0.954 1_555 1_555 H3A C3A 0.955 1_555 1_555 N3A C3 1.400 1_555 1_555 H4A N3A 0.901 1_555 1_555 H1F C3A 0.976 1_555 1_555 H2F C3A 0.954 1_555 1_555 H3F C3A 0.955 1_555 1_555 H4F N3 0.901 1_555 1_555 H1G C3 0.976 1_555 1_555 H2G C3 0.954 1_555 1_555 H3G C3 0.955 1_555 1_555 H4G N3A 0.901 1_555 1_555 N3 N3A 1.496 1_555 1_555 C3A N3A 1.400 1_555 1_555 #END data_CSD_CIF_TIWCUZ02 _audit_creation_date 2014-02-17 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD TIWCUZ02 _database_code_depnum_ccdc_archive 'CCDC 895863' _chemical_formula_sum 'C10 H16 Co1 K1 N8' _chemical_formula_moiety ; (C6 Co1 K1 N6 2-)n,2(C2 H8 N1 1+) ; _journal_coden_Cambridge 4 _journal_volume 135 _journal_year 2013 _journal_page_first 5230 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "Wen Zhang" "Heng-Yun Ye" "R.Graf" "H.W.Spiess" "Ye-Feng Yao" "Run-Qiang Zhu" "Ren-Gen Xiong" _chemical_name_systematic ; catena-[bis(N,N-dideuterodiemthylammonium) hexakis(\m~2~-cyano)-potassium-cobalt] ; _cell_volume 787.058 _exptl_crystal_colour 'yellow' _exptl_crystal_density_diffrn 1.478 _exptl_crystal_description 'block' _diffrn_ambient_temperature 113 _refine_special_details ; N3 disordered by symmetry over two sites with occupancy 0.50. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0926 _refine_ls_wR_factor_gt 0.0926 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/m n c' _symmetry_Int_Tables_number 128 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x,z 3 -x,-y,z 4 y,-x,z 5 1/2+x,1/2-y,1/2-z 6 1/2+y,1/2+x,1/2-z 7 1/2-x,1/2+y,1/2-z 8 1/2-y,1/2-x,1/2-z 9 -x,-y,-z 10 y,-x,-z 11 x,y,-z 12 -y,x,-z 13 -1/2-x,-1/2+y,-1/2+z 14 -1/2-y,-1/2-x,-1/2+z 15 -1/2+x,-1/2-y,-1/2+z 16 -1/2+y,-1/2+x,-1/2+z _cell_length_a 8.2371(13) _cell_length_b 8.2371(13) _cell_length_c 11.600(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Co 1.26 D 0.23 K 2.03 N 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Co1 Co 0.00000 0.00000 0.50000 K1 K 0.00000 0.00000 0.00000 N1 N 0.00000 0.00000 0.2386(13) N2 N 0.1954(14) 0.3130(15) 0.50000 C1 C 0.00000 0.00000 0.3373(11) C2 C 0.1273(11) 0.1958(11) 0.50000 C3 C -0.1039(12) 0.3961(12) 0.25000 H1? H -0.2198(12) 0.3841(12) 0.25000 H2? H -0.0598(12) 0.3448(12) 0.18230 H3? H -0.0598(12) 0.3448(12) 0.31770 N3? N -0.0620(14) 0.5620(14) 0.25000 D1? D -0.10780 0.60910 0.31250 N2A N -0.3130(14) 0.1954(15) 0.50000 C2A C -0.1958(11) 0.1273(11) 0.50000 N2B N -0.1954(14) -0.3130(15) 0.50000 C2B C -0.1273(11) -0.1958(11) 0.50000 N2C N 0.3130(14) -0.1954(15) 0.50000 C2C C 0.1958(11) -0.1273(11) 0.50000 N1H N 0.00000 0.00000 -0.2386(13) C1H C 0.00000 0.00000 -0.3373(11) Co1* Co 0.00000 0.00000 -0.50000 K1D K -0.50000 -0.50000 0.50000 K1D* K -0.50000 0.50000 0.50000 K1D** K 0.50000 -0.50000 0.50000 K1D*** K 0.50000 0.50000 0.50000 N2D N -0.3046(14) 0.1870(15) 0.00000 N2E N -0.1870(14) -0.3046(15) 0.00000 N2F N 0.3046(14) -0.1870(15) 0.00000 N2G N 0.1870(14) 0.3046(15) 0.00000 C1H* C 0.00000 0.00000 0.6627(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Co1 C1 1.887 1_555 1_555 K1 N1 2.768 1_555 1_555 N1 C1 1.145 1_555 1_555 N2 C2 1.117 1_555 1_555 C2 Co1 1.924 1_555 1_555 N2A C2A 1.117 1_555 1_555 C2A Co1 1.924 1_555 1_555 N2B C2B 1.117 1_555 1_555 C2B Co1 1.924 1_555 1_555 N2C C2C 1.117 1_555 1_555 C2C Co1 1.924 1_555 1_555 N1H K1 2.768 1_555 1_555 C1H N1H 1.145 1_555 1_555 Co1* C1H 1.887 1_555 1_555 K1D N2B 2.944 1_555 1_555 K1D* N2A 2.944 1_555 1_555 K1D** N2C 2.944 1_555 1_555 K1D*** N2 2.944 1_555 1_555 N2D K1 2.944 1_555 1_555 N2E K1 2.944 1_555 1_555 N2F K1 2.944 1_555 1_555 N2G K1 2.944 1_555 1_555 C1H* Co1 1.887 1_555 1_555 #END data_CSD_CIF_TOXHUJ _audit_creation_date 1997-05-19 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD TOXHUJ _chemical_formula_sum 'C18 H54 Al2 N2 Na2 Si4' _chemical_formula_moiety ; C18 H54 Al2 N2 Na1 Si4 1-,Na1 1+ ; _journal_coden_Cambridge 579 _journal_volume 15 _journal_year 1996 _journal_page_first 4107 _journal_name_full 'Organometallics ' loop_ _publ_author_name "M.Niemeyer" "P.P.Power" _chemical_name_systematic ; Sodium bis((\m~2~-bis(trimethylsilyl)amido)-trimethyl-aluminium)-sodium ; _chemical_melting_point 460.15 _cell_volume 1570.475 _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.08 _exptl_special_details ; Melts with decomposition. ; _diffrn_ambient_temperature 130 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.059 _refine_ls_wR_factor_gt 0.059 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 8.812(2) _cell_length_b 12.642(2) _cell_length_c 15.436(3) _cell_angle_alpha 74.894(13) _cell_angle_beta 86.924(14) _cell_angle_gamma 71.173(13) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Al 1.28 N 0.68 Na 1.44 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 0.1924(2) 0.2609(1) 0.9863(1) Na2 Na 0.2315(2) 0.7530(1) 0.7752(1) N1 N 0.2685(4) 0.5662(3) 0.7350(2) Si1 Si 0.4731(1) 0.4911(1) 0.7541(1) C1 C 0.5984(6) 0.5085(5) 0.6525(3) C2 C 0.5588(6) 0.5440(5) 0.8362(4) C3 C 0.5160(6) 0.3312(4) 0.7980(4) Si2 Si 0.1869(1) 0.5939(1) 0.6272(1) C4 C -0.0365(6) 0.6599(4) 0.6211(3) C5 C 0.2307(6) 0.4595(4) 0.5875(3) C6 C 0.2591(8) 0.7020(5) 0.5433(4) N2 N 0.2222(3) 0.9559(3) 0.7580(2) Si3 Si 0.0215(1) 1.0368(1) 0.7303(1) C7 C -0.0137(6) 1.1961(4) 0.6921(3) C8 C -0.0603(6) 0.9908(4) 0.6412(3) C9 C -0.1125(5) 1.0164(4) 0.8274(3) Si4 Si 0.3636(1) 0.9838(1) 0.6795(1) C10 C 0.5365(5) 0.8494(4) 0.6834(3) C11 C 0.4410(6) 1.0972(4) 0.6987(3) C12 C 0.2855(6) 1.0338(5) 0.5598(3) Al1 Al 0.1321(1) 0.5292(1) 0.8311(1) C13 C 0.0402(5) 0.4092(4) 0.8195(3) C14 C 0.2445(6) 0.4745(4) 0.9518(3) C15 C -0.0386(5) 0.6767(4) 0.8401(3) Al2 Al 0.2874(1) 0.9269(1) 0.8820(1) C16 C 0.2258(5) 1.0732(4) 0.9215(3) C17 C 0.5237(5) 0.8548(4) 0.9089(3) C18 C 0.2006(6) 0.8086(4) 0.9597(3) H1 H 0.5959(56) 0.5850(47) 0.6326(33) H2 H 0.5656(57) 0.4825(43) 0.6082(35) H3 H 0.7112(71) 0.4582(49) 0.6716(38) H4 H 0.5534(70) 0.6166(59) 0.8097(42) H5 H 0.6705(73) 0.5118(49) 0.8449(38) H6 H 0.5053(87) 0.5367(63) 0.8889(53) H7 H 0.4721(63) 0.3148(47) 0.8564(41) H8 H 0.6242(75) 0.3002(51) 0.8068(39) H9 H 0.4840(62) 0.3025(46) 0.7525(38) H10 H -0.0775(51) 0.7345(42) 0.6311(29) H11 H -0.0889(54) 0.6134(42) 0.6604(32) H12 H -0.0755(51) 0.6673(38) 0.5581(32) H13 H 0.3462(77) 0.4259(53) 0.5863(42) H14 H 0.1876(51) 0.4802(38) 0.5299(35) H15 H 0.1706(56) 0.4179(41) 0.6261(33) H16 H 0.2207(78) 0.7726(61) 0.5575(44) H17 H 0.2158(66) 0.7193(49) 0.4906(43) H18 H 0.3566(70) 0.6802(48) 0.5321(36) H19 H 0.0398(58) 1.2187(41) 0.6403(36) H20 H 0.0113(56) 1.2250(41) 0.7435(34) H21 H -0.1210(64) 1.2355(45) 0.6816(34) H22 H -0.0698(86) 0.9192(71) 0.6668(50) H23 H 0.0015(80) 1.0049(58) 0.5881(48) H24 H -0.1667(90) 1.0163(61) 0.6329(47) H25 H -0.1182(52) 0.9404(44) 0.8448(30) H26 H -0.2147(70) 1.073(5) 0.8088(37) H27 H -0.0867(49) 1.0402(36) 0.8790(31) H28 H 0.5027(68) 0.8013(51) 0.6612(40) H29 H 0.5843(58) 0.8162(43) 0.7389(37) H30 H 0.6169(64) 0.8691(45) 0.6429(37) H31 H 0.3603(57) 1.1655(45) 0.6972(31) H32 H 0.5100(63) 1.1088(44) 0.6529(37) H33 H 0.4877(50) 1.0741(37) 0.7577(33) H34 H 0.1954(60) 1.1006(45) 0.5563(32) H35 H 0.2712(67) 0.9756(54) 0.5391(41) H36 H 0.3613(64) 1.0651(45) 0.5314(36) H37 H -0.0247(54) 0.4312(40) 0.7664(33) H38 H 0.1215(53) 0.3371(41) 0.8124(29) H39 H -0.0307(59) 0.3844(42) 0.8671(35) H40 H 0.1657(61) 0.4554(43) 1.0006(35) H41 H 0.2756(62) 0.5255(49) 0.9675(36) H42 H 0.3382(64) 0.4115(47) 0.9606(34) H43 H -0.1353(59) 0.6584(40) 0.8591(32) H44 H -0.0764(53) 0.7366(43) 0.7936(34) H45 H -0.0078(61) 0.7045(46) 0.8866(37) H46 H 0.2911(65) 1.1105(46) 0.8965(37) H47 H 0.2503(50) 1.0566(38) 0.9870(33) H48 H 0.1137(57) 1.1284(39) 0.9056(30) H49 H 0.5684(49) 0.7833(41) 0.9074(28) H50 H 0.5302(53) 0.8497(40) 0.9705(36) H51 H 0.5928(49) 0.9016(37) 0.8751(29) H52 H 0.2457(73) 0.7315(58) 0.9558(40) H53 H 0.2342(59) 0.7968(43) 1.0154(39) H54 H 0.0979(73) 0.8229(49) 0.9607(37) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Na2 N1 2.513 1_555 1_555 N1 Si1 1.745 1_555 1_555 Si1 C1 1.876 1_555 1_555 C1 H1 0.929 1_555 1_555 C2 Si1 1.869 1_555 1_555 C3 Si1 1.873 1_555 1_555 Si2 N1 1.752 1_555 1_555 C4 Si2 1.871 1_555 1_555 C5 Si2 1.872 1_555 1_555 C6 Si2 1.871 1_555 1_555 N2 Na2 2.484 1_555 1_555 Si3 N2 1.744 1_555 1_555 C7 Si3 1.870 1_555 1_555 C8 Si3 1.882 1_555 1_555 C9 Si3 1.874 1_555 1_555 Si4 N2 1.745 1_555 1_555 C10 Si4 1.870 1_555 1_555 C11 Si4 1.866 1_555 1_555 C12 Si4 1.880 1_555 1_555 Al1 N1 1.917 1_555 1_555 C13 Al1 1.985 1_555 1_555 C14 Al1 2.004 1_555 1_555 C15 Al1 2.015 1_555 1_555 Al2 N2 1.935 1_555 1_555 C16 Al2 1.998 1_555 1_555 C17 Al2 2.002 1_555 1_555 C18 Al2 1.991 1_555 1_555 H2 C1 0.927 1_555 1_555 H3 C1 1.003 1_555 1_555 H4 C2 0.889 1_555 1_555 H5 C2 0.938 1_555 1_555 H6 C2 0.917 1_555 1_555 H7 C3 0.960 1_555 1_555 H8 C3 0.909 1_555 1_555 H9 C3 0.962 1_555 1_555 H10 C4 0.945 1_555 1_555 H11 C4 0.941 1_555 1_555 H12 C4 1.020 1_555 1_555 H13 C5 0.969 1_555 1_555 H14 C5 0.924 1_555 1_555 H15 C5 0.946 1_555 1_555 H16 C6 0.926 1_555 1_555 H17 C6 0.861 1_555 1_555 H18 C6 0.837 1_555 1_555 H19 C7 0.933 1_555 1_555 H20 C7 1.017 1_555 1_555 H21 C7 0.916 1_555 1_555 H22 C8 0.917 1_555 1_555 H23 C8 0.969 1_555 1_555 H24 C8 0.892 1_555 1_555 H25 C9 0.945 1_555 1_555 H26 C9 0.954 1_555 1_555 H27 C9 0.982 1_555 1_555 H28 C10 0.901 1_555 1_555 H29 C10 0.908 1_555 1_555 H30 C10 0.970 1_555 1_555 H31 C11 0.920 1_555 1_555 H32 C11 0.921 1_555 1_555 H33 C11 0.953 1_555 1_555 H34 C12 0.946 1_555 1_555 H35 C12 0.920 1_555 1_555 H36 C12 0.919 1_555 1_555 H37 C13 0.951 1_555 1_555 H38 C13 0.989 1_555 1_555 H39 C13 0.993 1_555 1_555 H40 C14 1.032 1_555 1_555 H41 C14 0.867 1_555 1_555 H42 C14 0.930 1_555 1_555 H43 C15 0.965 1_555 1_555 H44 C15 0.883 1_555 1_555 H45 C15 0.962 1_555 1_555 H46 C16 0.871 1_555 1_555 H47 C16 0.998 1_555 1_555 H48 C16 1.007 1_555 1_555 H49 C17 0.868 1_555 1_555 H50 C17 0.940 1_555 1_555 H51 C17 1.015 1_555 1_555 H52 C18 0.943 1_555 1_555 H53 C18 0.884 1_555 1_555 H54 C18 0.864 1_555 1_555 #END data_CSD_CIF_UDORIQ _audit_creation_date 2013-07-31 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD UDORIQ _database_code_depnum_ccdc_archive 'CCDC 938237' _chemical_formula_sum 'C74.5 H78 B4 Li1 O4 P1' _chemical_formula_moiety ; C52 H40 B4 Li1 O4 1-,C12 H26 P1 1+,1.5(C7 H8) ; _journal_coden_Cambridge 1078 _journal_year 2013 _journal_name_full 'CSD Communication(Private Communication) ' loop_ _publ_author_name "M.Bolte" _chemical_name_systematic ; 1,1-Di-t-butylphospholanium (7',7''-oxybis(5,7'-dihydrospiro[dibenzo[b,d]borole-5,5'-dibenzo[c,e][1,2,7]ox adiborepine]))-tetrahydrofuran-lithium toluene solvate ; _cell_volume 3121.292 _exptl_crystal_density_diffrn 1.19 _exptl_crystal_description 'plate' _diffrn_ambient_temperature 173 _refine_special_details ; C201,C203,C205 disordered by symmetry over two sites with occupancy 0.50; C83',C84',C85' and C83,C84,C85 disordered over two sites with occupancies 0.515:0.485. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.1096 _refine_ls_wR_factor_gt 0.1096 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 13.690(3) _cell_length_b 14.090(3) _cell_length_c 17.523(5) _cell_angle_alpha 68.938(18) _cell_angle_beta 83.344(18) _cell_angle_gamma 83.014(16) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 B 0.83 Li 1.28 O 0.68 P 1.05 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.2385(14) 0.1507(12) 0.7404(12) O1 O 0.2248(5) 0.2727(4) 0.7677(4) B1 B 0.2933(10) 0.2835(7) 0.8155(7) O2 O 0.3793(5) 0.2280(4) 0.8273(4) B2 B 0.4279(9) 0.1504(7) 0.7985(7) O3 O 0.3766(4) 0.1132(4) 0.7558(4) B3 B 0.1279(9) 0.3380(7) 0.7472(8) B4 B 0.4178(9) 0.0225(6) 0.7284(6) C1 C 0.2691(7) 0.3633(6) 0.8619(6) C2 C 0.2262(7) 0.4616(6) 0.8283(6) C3 C 0.2071(8) 0.5213(7) 0.8793(7) H1 H 0.17430 0.58770 0.85800 C4 C 0.2339(8) 0.4874(8) 0.9574(7) H2 H 0.22280 0.53080 0.98900 C5 C 0.2776(9) 0.3893(7) 0.9907(7) H3 H 0.29450 0.36390 1.04590 C6 C 0.2965(8) 0.3285(7) 0.9434(7) H4 H 0.32860 0.26190 0.96600 C7 C 0.1521(7) 0.4567(7) 0.7014(7) C8 C 0.2022(8) 0.5067(6) 0.7426(6) C9 C 0.2344(9) 0.6054(7) 0.6982(7) H5 H 0.27240 0.63730 0.72270 C10 C 0.2077(10) 0.6555(8) 0.6149(8) H6 H 0.22820 0.72170 0.58480 C11 C 0.1559(9) 0.6127(9) 0.5790(8) H7 H 0.13780 0.64840 0.52470 C12 C 0.1276(8) 0.5127(7) 0.6227(7) H8 H 0.08980 0.48280 0.59650 C13 C 0.0382(8) 0.3199(6) 0.8216(7) C14 C -0.0439(8) 0.2788(7) 0.8019(7) C15 C -0.1276(10) 0.2606(8) 0.8531(9) H9 H -0.17950 0.23280 0.83860 C16 C -0.1405(12) 0.2809(10) 0.9256(9) H10 H -0.20040 0.26880 0.95940 C17 C -0.0637(9) 0.3193(8) 0.9475(7) H11 H -0.06960 0.33320 0.99710 C18 C 0.0230(9) 0.3371(7) 0.8948(8) H12 H 0.07490 0.36310 0.91080 C19 C 0.0771(8) 0.2942(6) 0.6875(7) C20 C -0.0197(8) 0.2628(6) 0.7242(7) C21 C -0.0773(9) 0.2238(7) 0.6840(9) H13 H -0.14120 0.20410 0.70700 C22 C -0.0401(12) 0.2141(7) 0.6093(9) H14 H -0.07820 0.18530 0.58250 C23 C 0.0520(11) 0.2459(8) 0.5734(8) H15 H 0.07560 0.24040 0.52190 C24 C 0.1093(8) 0.2857(7) 0.6127(7) H16 H 0.17190 0.30740 0.58770 C25 C 0.5303(7) 0.1078(6) 0.8306(6) C26 C 0.6074(8) 0.0705(6) 0.7853(6) C27 C 0.6961(9) 0.0270(8) 0.8228(7) H17 H 0.74870 0.00100 0.79350 C28 C 0.7071(9) 0.0221(8) 0.9009(7) H18 H 0.76620 -0.00980 0.92610 C29 C 0.6333(8) 0.0629(7) 0.9431(6) H19 H 0.64220 0.06200 0.99630 C30 C 0.5453(8) 0.1055(6) 0.9069(6) H20 H 0.49440 0.13370 0.93610 C31 C 0.5181(7) 0.0495(6) 0.6736(6) C32 C 0.6039(8) 0.0745(6) 0.6996(6) C33 C 0.6876(8) 0.1028(7) 0.6447(6) H21 H 0.74210 0.12200 0.66330 C34 C 0.6943(8) 0.1041(7) 0.5664(6) H22 H 0.75240 0.12340 0.53140 C35 C 0.6156(8) 0.0769(6) 0.5379(6) H23 H 0.61990 0.07310 0.48450 C36 C 0.5311(8) 0.0557(6) 0.5891(6) H24 H 0.47570 0.04390 0.56670 C37 C 0.4179(7) -0.0875(6) 0.8049(5) C38 C 0.3528(8) -0.1482(6) 0.7913(7) C39 C 0.3395(9) -0.2483(7) 0.8465(7) H25 H 0.29310 -0.28750 0.83770 C40 C 0.3959(9) -0.2880(7) 0.9139(6) H26 H 0.38850 -0.35550 0.95110 C41 C 0.4618(9) -0.2313(7) 0.9274(6) H27 H 0.50060 -0.25950 0.97320 C42 C 0.4720(7) -0.1293(6) 0.8721(6) H28 H 0.51700 -0.08960 0.88210 C43 C 0.3307(7) 0.0061(6) 0.6794(6) C44 C 0.2998(7) -0.0946(6) 0.7204(6) C45 C 0.2269(8) -0.1285(7) 0.6902(7) H29 H 0.20720 -0.19560 0.71730 C46 C 0.1828(8) -0.0641(8) 0.6203(7) H30 H 0.13430 -0.08850 0.59910 C47 C 0.2083(8) 0.0357(7) 0.5808(7) H31 H 0.17590 0.08070 0.53450 C48 C 0.2828(7) 0.0673(6) 0.6112(6) H32 H 0.30170 0.13460 0.58360 O4 O 0.1541(5) 0.0604(5) 0.8160(4) C49 C 0.0769(8) 0.0020(7) 0.8118(7) H33 H 0.10410 -0.06570 0.81020 H34 H 0.03960 0.03850 0.76290 C50 C 0.0133(13) -0.0083(16) 0.8888(10) H35 H -0.00690 -0.07860 0.91480 H36 H -0.04670 0.03990 0.87720 C51 C 0.0760(12) 0.0166(14) 0.9449(9) H37 H 0.04970 0.08130 0.95280 H38 H 0.07760 -0.03880 0.99910 C52 C 0.1782(14) 0.026(2) 0.8997(9) H39 H 0.21380 0.07670 0.91020 H40 H 0.21830 -0.04040 0.91490 P1 P 0.6621(2) 0.57677(18) 0.70357(17) C53 C 0.6369(8) 0.7152(7) 0.6789(7) C54 C 0.6274(10) 0.7427(9) 0.7556(9) H41 H 0.57230 0.70950 0.79250 H42 H 0.61490 0.81690 0.74050 H43 H 0.68860 0.71960 0.78330 C55 C 0.5417(9) 0.7539(8) 0.6323(8) H44 H 0.48490 0.72330 0.66830 H45 H 0.54860 0.73420 0.58350 H46 H 0.53150 0.82840 0.61560 C56 C 0.7225(10) 0.7670(7) 0.6185(8) H47 H 0.78460 0.74510 0.64530 H48 H 0.70980 0.84130 0.60220 H49 H 0.72750 0.74740 0.56980 C57 C 0.5791(10) 0.4959(8) 0.7838(8) C58 C 0.6004(12) 0.4938(9) 0.8681(8) H50 H 0.67040 0.47270 0.87640 H51 H 0.56000 0.44520 0.91070 H52 H 0.58440 0.56200 0.87130 C59 C 0.604(1) 0.3837(8) 0.7818(10) H53 H 0.67420 0.36290 0.78940 H54 H 0.58900 0.38260 0.72880 H55 H 0.56420 0.33640 0.82600 C60 C 0.4733(10) 0.5274(9) 0.7731(9) H56 H 0.45800 0.52840 0.71950 H57 H 0.45780 0.59570 0.77620 H58 H 0.43370 0.47890 0.81660 C61 C 0.7873(10) 0.5392(7) 0.7284(9) H59 H 0.81540 0.59220 0.74200 H60 H 0.79260 0.47390 0.77520 C62 C 0.8420(11) 0.5269(11) 0.6452(11) H61 H 0.85890 0.59400 0.60510 H62 H 0.90340 0.48090 0.65720 C63 C 0.7702(14) 0.4824(11) 0.6126(10) H63 H 0.76430 0.40990 0.64720 H64 H 0.79270 0.48600 0.55590 C64 C 0.6698(11) 0.545(1) 0.6136(8) H65 H 0.61500 0.50420 0.61550 H66 H 0.66660 0.60760 0.56410 C65 C -0.0656(11) 0.8266(13) 0.7156(17) C66 C -0.0975(11) 0.8266(15) 0.7925(18) H67 H -0.12720 0.88770 0.79970 C67 C -0.0856(16) 0.731(2) 0.8646(14) H68 H -0.10330 0.72900 0.91920 C68 C -0.0488(14) 0.6508(13) 0.8471(16) H69 H -0.04670 0.58710 0.89120 C69 C -0.0124(13) 0.6500(17) 0.7693(19) H70 H 0.02110 0.59020 0.76230 C70 C -0.0270(12) 0.7407(16) 0.7019(12) H71 H -0.00990 0.74160 0.64750 C71 C -0.0821(16) 0.9235(13) 0.6364(16) H72 H -0.11030 0.98160 0.65240 H73 H -0.12760 0.90970 0.60310 H74 H -0.01880 0.93940 0.60440 H75? H 0.08490 -0.01320 0.76040 H76? H 0.01070 0.03750 0.81660 C72? C 0.0936(14) -0.0939(11) 0.886(1) H77? H 0.12650 -0.15050 0.86910 H78? H 0.03010 -0.11500 0.91740 C73? C 0.1600(14) -0.0649(10) 0.938(1) H79? H 0.22860 -0.09530 0.93350 H80? H 0.13480 -0.08800 0.99650 C74? C 0.155(2) 0.0529(13) 0.9006(9) H81? H 0.09390 0.08570 0.92010 H82? H 0.21350 0.08060 0.91030 H83? H 0.60670 0.40020 0.47030 H84? H 0.50610 0.29250 0.58880 H85? H 0.45310 0.35110 0.64760 H86? H 0.39390 0.33950 0.57830 C75? C 0.4585(19) 0.3492(15) 0.5919(12) H87? H 0.44020 0.28460 0.62870 C76? C 0.515(2) 0.563(3) 0.460(2) H88? H 0.59100 0.32240 0.52730 C77? C 0.544(5) 0.378(2) 0.526(3) C78? C 0.5681(12) 0.4599(19) 0.4728(13) C79? C 0.592(3) 0.537(3) 0.425(2) H89? H 0.64950 0.53050 0.39060 H90? H 0.62420 0.45870 0.43570 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 O1 1.926 1_555 1_555 O1 B1 1.383 1_555 1_555 B1 O2 1.325 1_555 1_555 O2 B2 1.426 1_555 1_555 B2 O3 1.349 1_555 1_555 O3 Li1 1.923 1_555 1_555 B3 O1 1.520 1_555 1_555 B4 O3 1.544 1_555 1_555 C1 B1 1.593 1_555 1_555 C2 C1 1.381 1_555 1_555 C3 C2 1.417 1_555 1_555 H1 C3 0.950 1_555 1_555 C4 C3 1.356 1_555 1_555 H2 C4 0.951 1_555 1_555 C5 C4 1.382 1_555 1_555 H3 C5 0.949 1_555 1_555 C6 C1 1.413 1_555 1_555 H4 C6 0.951 1_555 1_555 C7 B3 1.631 1_555 1_555 C8 C2 1.464 1_555 1_555 C9 C8 1.423 1_555 1_555 H5 C9 0.951 1_555 1_555 C10 C9 1.443 1_555 1_555 H6 C10 0.950 1_555 1_555 C11 C10 1.320 1_555 1_555 H7 C11 0.949 1_555 1_555 C12 C7 1.378 1_555 1_555 H8 C12 0.950 1_555 1_555 C13 B3 1.655 1_555 1_555 C14 C13 1.452 1_555 1_555 C15 C14 1.361 1_555 1_555 H9 C15 0.951 1_555 1_555 C16 C15 1.387 1_555 1_555 H10 C16 0.949 1_555 1_555 C17 C16 1.388 1_555 1_555 H11 C17 0.950 1_555 1_555 C18 C13 1.377 1_555 1_555 H12 C18 0.949 1_555 1_555 C19 B3 1.642 1_555 1_555 C20 C14 1.453 1_555 1_555 C21 C20 1.390 1_555 1_555 H13 C21 0.950 1_555 1_555 C22 C21 1.396 1_555 1_555 H14 C22 0.950 1_555 1_555 C23 C22 1.392 1_555 1_555 H15 C23 0.949 1_555 1_555 C24 C19 1.376 1_555 1_555 H16 C24 0.949 1_555 1_555 C25 B2 1.542 1_555 1_555 C26 C25 1.411 1_555 1_555 C27 C26 1.413 1_555 1_555 H17 C27 0.950 1_555 1_555 C28 C27 1.370 1_555 1_555 H18 C28 0.950 1_555 1_555 C29 C28 1.374 1_555 1_555 H19 C29 0.949 1_555 1_555 C30 C25 1.364 1_555 1_555 H20 C30 0.949 1_555 1_555 C31 B4 1.585 1_555 1_555 C32 C26 1.489 1_555 1_555 C33 C32 1.406 1_555 1_555 H21 C33 0.951 1_555 1_555 C34 C33 1.358 1_555 1_555 H22 C34 0.950 1_555 1_555 C35 C34 1.386 1_555 1_555 H23 C35 0.951 1_555 1_555 C36 C31 1.443 1_555 1_555 H24 C36 0.951 1_555 1_555 C37 B4 1.645 1_555 1_555 C38 C37 1.401 1_555 1_555 C39 C38 1.414 1_555 1_555 H25 C39 0.950 1_555 1_555 C40 C39 1.391 1_555 1_555 H26 C40 0.950 1_555 1_555 C41 C40 1.367 1_555 1_555 H27 C41 0.950 1_555 1_555 C42 C37 1.371 1_555 1_555 H28 C42 0.950 1_555 1_555 C43 B4 1.631 1_555 1_555 C44 C38 1.429 1_555 1_555 C45 C44 1.387 1_555 1_555 H29 C45 0.950 1_555 1_555 C46 C45 1.388 1_555 1_555 H30 C46 0.950 1_555 1_555 C47 C46 1.394 1_555 1_555 H31 C47 0.950 1_555 1_555 C48 C43 1.380 1_555 1_555 H32 C48 0.949 1_555 1_555 O4 Li1 1.871 1_555 1_555 C49 O4 1.440 1_555 1_555 H33 C49 0.990 1_555 1_555 H34 C49 0.990 1_555 1_555 C50 C49 1.489 1_555 1_555 H35 C50 0.989 1_555 1_555 H36 C50 0.990 1_555 1_555 C51 C50 1.531 1_555 1_555 H37 C51 0.990 1_555 1_555 H38 C51 0.990 1_555 1_555 C52 O4 1.434 1_555 1_555 H39 C52 0.991 1_555 1_555 H40 C52 0.989 1_555 1_555 P1 C53 1.837 1_555 1_555 C53 C54 1.515 1_555 1_555 C54 H41 0.980 1_555 1_555 H42 C54 0.980 1_555 1_555 H43 C54 0.979 1_555 1_555 C55 C53 1.555 1_555 1_555 H44 C55 0.980 1_555 1_555 H45 C55 0.981 1_555 1_555 H46 C55 0.980 1_555 1_555 C56 C53 1.546 1_555 1_555 H47 C56 0.981 1_555 1_555 H48 C56 0.980 1_555 1_555 H49 C56 0.980 1_555 1_555 C57 P1 1.833 1_555 1_555 C58 C57 1.528 1_555 1_555 H50 C58 0.980 1_555 1_555 H51 C58 0.980 1_555 1_555 H52 C58 0.979 1_555 1_555 C59 C57 1.588 1_555 1_555 H53 C59 0.980 1_555 1_555 H54 C59 0.980 1_555 1_555 H55 C59 0.980 1_555 1_555 C60 C57 1.475 1_555 1_555 H56 C60 0.981 1_555 1_555 H57 C60 0.979 1_555 1_555 H58 C60 0.981 1_555 1_555 C61 P1 1.787 1_555 1_555 H59 C61 0.991 1_555 1_555 H60 C61 0.990 1_555 1_555 C62 C61 1.617 1_555 1_555 H61 C62 0.990 1_555 1_555 H62 C62 0.991 1_555 1_555 C63 C62 1.491 1_555 1_555 H63 C63 0.991 1_555 1_555 H64 C63 0.991 1_555 1_555 C64 P1 1.776 1_555 1_555 H65 C64 0.990 1_555 1_555 H66 C64 0.991 1_555 1_555 C65 C66 1.368 1_555 1_555 C66 H67 0.950 1_555 1_555 C67 C66 1.486 1_555 1_555 H68 C67 0.950 1_555 1_555 C68 C67 1.304 1_555 1_555 H69 C68 0.951 1_555 1_555 C69 C68 1.400 1_555 1_555 H70 C69 0.950 1_555 1_555 C70 C65 1.351 1_555 1_555 H71 C70 0.951 1_555 1_555 C71 C65 1.574 1_555 1_555 H72 C71 0.980 1_555 1_555 H73 C71 0.981 1_555 1_555 H74 C71 0.980 1_555 1_555 C5 C6 1.376 1_555 1_555 C7 C8 1.444 1_555 1_555 C11 C12 1.418 1_555 1_555 C17 C18 1.406 1_555 1_555 C19 C20 1.451 1_555 1_555 C23 C24 1.383 1_555 1_555 C29 C30 1.393 1_555 1_555 C31 C32 1.432 1_555 1_555 C35 C36 1.372 1_555 1_555 C41 C42 1.428 1_555 1_555 C43 C44 1.432 1_555 1_555 C47 C48 1.389 1_555 1_555 C51 C52 1.522 1_555 1_555 C63 C64 1.542 1_555 1_555 C69 C70 1.406 1_555 1_555 #END data_CSD_CIF_VACNOC _audit_creation_date 1989-07-31 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD VACNOC _database_code_depnum_ccdc_archive 'CCDC 1278754' _chemical_formula_sum 'C48 H110 Cd2 Cl4 Li2 O7 Si6' _chemical_formula_moiety ; C28 H70 Cd2 Cl4 Li1 O2 Si6 1+,C16 H32 Li1 O4 1-,C4 H8 O1 ; _journal_coden_Cambridge 182 _journal_year 1988 _journal_page_first 1389 _journal_name_full 'Chem.Commun. ' loop_ _publ_author_name "S.S.Al-Juaid" "N.H.Buttrus" "C.Eaborn" "P.B.Hitchcock" "J.D.Smith" "K.Tavakkoli" _chemical_name_systematic ; (bis(Tetrahydrofuran)-lithium)-tetrakis(\m~2~-chloro)-bis(tris(trimethylsilyl) methyl)-di-cadmium(ii) tetrakis(tetrahydrofuran)-lithium tetrahydrofuran solvate ; _cell_volume 3483.767 _exptl_crystal_density_diffrn 1.29 _exptl_special_details ; Tetrahydrofuran solvent is easily lost on exposure to air ; _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; _refine_special_details ; A free tetrahydrofuran molecule appears to be disordered across the mirror plane of the cation, whose nature is uncertain, but which appears to be a lithium atom tetrahedrally surrounded by 4 O atoms. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.083 _refine_ls_wR_factor_gt 0.083 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,-z 3 -x,-y,-z 4 x,-1/2-y,z _cell_length_a 12.691(2) _cell_length_b 19.656(3) _cell_length_c 14.154(3) _cell_angle_alpha 90 _cell_angle_beta 99.36(1) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 Cd 1.62 Cl 0.99 Li 1.09 O 0.68 Si 1.18 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li -0.0364(5) 0.25000 0.8210(46) Cd1 Cd 0.2333(1) 0.3431(1) 0.7650(1) Cl1 Cl 0.0760(4) 0.3481(3) 0.8535(4) Cl2 Cl 0.3405(7) 0.25000 0.8668(6) Cl3 Cl 0.1621(7) 0.25000 0.6425(6) Si1 Si 0.3134(7) 0.4930(4) 0.8337(6) Si2 Si 0.2120(7) 0.4705(5) 0.6201(6) Si3 Si 0.4397(6) 0.4170(5) 0.6967(6) O1 O -0.1311(23) 0.25000 0.7120(19) O2 O -0.135(2) 0.25000 0.9188(17) C1 C 0.3068(14) 0.4383(11) 0.7247(14) C2 C 0.3540(23) 0.4459(16) 0.9514(16) C3 C 0.1804(22) 0.5348(15) 0.8509(24) C4 C 0.4143(25) 0.5649(13) 0.8455(21) C5 C 0.2344(30) 0.4197(21) 0.5020(19) C6 C 0.0645(19) 0.4520(17) 0.6333(21) C7 C 0.2315(26) 0.5669(16) 0.5929(24) C8 C 0.5384(20) 0.3986(18) 0.8167(22) C9 C 0.5064(20) 0.4862(16) 0.6328(17) C10 C 0.4409(23) 0.3329(17) 0.6192(21) C11 C -0.1508(28) 0.1931(19) 0.6571(26) C12 C -0.2353(31) 0.2152(20) 0.5801(26) C13 C -0.1704(34) 0.1936(22) 0.9832(30) C14 C -0.2675(32) 0.2216(22) 0.9979(26) Li2? Li 0.1960(69) 0.2893(44) 0.1945(60) O3? O 0.3469(29) 0.25000 0.2474(25) O4? O 0.0891(30) 0.25000 0.2856(26) O5? O 0.1634(21) 0.25000 0.0670(19) O6? O 0.1741(17) 0.3886(12) 0.1573(15) C15? C 0.0899(24) 0.4290(16) 0.0947(20) C16? C 0.1298(27) 0.5004(19) 0.1188(23) C17? C 0.2005(29) 0.4971(20) 0.2090(25) C18? C 0.2479(28) 0.4283(20) 0.2164(24) C19? C 0.4329(46) 0.25000 0.1791(41) C20? C 0.5247(49) 0.25000 0.2742(43) C21? C 0.5177(64) 0.75000 0.6441(55) C22? C 0.3732(66) 0.25000 0.3662(57) Cl1C Cl 0.0760(4) 0.1519(3) 0.8535(4) Cd1C Cd 0.2333(1) 0.1569(1) 0.7650(1) C11C C -0.1508(28) 0.3069(19) 0.6571(26) C13C C -0.1704(34) 0.3064(22) 0.9832(30) C12C C -0.2353(31) 0.2848(20) 0.5801(26) C14C C -0.2675(32) 0.2784(22) 0.9979(26) C1C C 0.3068(14) 0.0617(11) 0.7247(14) Si1C Si 0.3134(7) 0.0070(4) 0.8337(6) Si2C Si 0.2120(7) 0.0295(5) 0.6201(6) Si3C Si 0.4397(6) 0.0830(5) 0.6967(6) C2C C 0.3540(23) 0.0541(16) 0.9514(16) C3C C 0.1804(22) -0.0348(15) 0.8509(24) C4C C 0.4143(25) -0.0649(13) 0.8455(21) C5C C 0.2344(30) 0.0803(21) 0.5020(19) C6C C 0.0645(19) 0.0480(17) 0.6333(21) C7C C 0.2315(26) -0.0669(16) 0.5929(24) C8C C 0.5384(20) 0.1014(18) 0.8167(22) C9C C 0.5064(20) 0.0138(16) 0.6328(17) C10C C 0.4409(23) 0.1671(17) 0.6192(21) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 Cl1 2.398 1_555 1_555 Cd1 Cl1 2.525 1_555 1_555 Cl2 Cd1 2.576 1_555 1_555 Cl3 Cd1 2.581 1_555 1_555 Si1 C1 1.871 1_555 1_555 Si2 C1 1.860 1_555 1_555 Si3 C1 1.842 1_555 1_555 O1 Li1 1.795 1_555 1_555 O2 Li1 2.011 1_555 1_555 C1 Cd1 2.207 1_555 1_555 C2 Si1 1.902 1_555 1_555 C3 Si1 1.928 1_555 1_555 C4 Si1 1.896 1_555 1_555 C5 Si2 2.007 1_555 1_555 C6 Si2 1.946 1_555 1_555 C7 Si2 1.957 1_555 1_555 C8 Si3 1.973 1_555 1_555 C9 Si3 1.906 1_555 1_555 C10 Si3 1.985 1_555 1_555 C11 O1 1.362 1_555 1_555 C12 C11 1.465 1_555 1_555 C13 O2 1.548 1_555 1_555 C14 C13 1.396 1_555 1_555 Cl1C Li1 2.398 1_555 1_555 Cd1C Cl2 2.576 1_555 1_555 C11C O1 1.362 1_555 1_555 C13C O2 1.548 1_555 1_555 C12C C12 1.368 1_555 1_555 C14C C14 1.116 1_555 1_555 C1C Cd1C 2.207 1_555 1_555 Si1C C1C 1.871 1_555 1_555 Si2C C1C 1.860 1_555 1_555 Si3C C1C 1.842 1_555 1_555 C2C Si1C 1.902 1_555 1_555 C3C Si1C 1.928 1_555 1_555 C4C Si1C 1.896 1_555 1_555 C5C Si2C 2.007 1_555 1_555 C6C Si2C 1.946 1_555 1_555 C7C Si2C 1.957 1_555 1_555 C8C Si3C 1.973 1_555 1_555 C9C Si3C 1.906 1_555 1_555 C10C Si3C 1.985 1_555 1_555 Cl3 Cd1C 2.581 1_555 1_555 Cl1C Cd1C 2.525 1_555 1_555 C11C C12C 1.465 1_555 1_555 C13C C14C 1.396 1_555 1_555 #END data_CSD_CIF_VOJVUL _audit_creation_date 1992-06-24 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD VOJVUL _database_code_depnum_ccdc_fiz 'CSD 54838' _chemical_formula_sum 'C7 H12 K0.5 Mn0.5 N4' _chemical_formula_moiety ; (C4 H12 N1 1+)n,0.25n(C12 K2 Mn2 N12 4-) ; _journal_coden_Cambridge 29 _journal_volume 600 _journal_year 1991 _journal_page_first 239 _journal_name_full 'Z.Anorg.Allg.Chem. ' loop_ _publ_author_name "B.Ziegler" "M.Witzel" "D.Babel" _chemical_name_systematic ; catena-(bis(Tetramethylammonium) hexakis(\m~2~-cyano)-manganese-potassium) ; _cell_volume 956.825 _exptl_crystal_colour 'yellow' _exptl_crystal_density_diffrn 1.38 _exptl_special_details ; Isostructural with the rubidium cobalt analogue CSD 54838 adds no new information ; _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_gt 0.0445 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 4/m' _symmetry_Int_Tables_number 87 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,1/2+z 3 -y,x,z 4 1/2-y,1/2+x,1/2+z 5 -x,-y,z 6 1/2-x,1/2-y,1/2+z 7 y,-x,z 8 1/2+y,1/2-x,1/2+z 9 -x,-y,-z 10 -1/2-x,-1/2-y,-1/2-z 11 y,-x,-z 12 -1/2+y,-1/2-x,-1/2-z 13 x,y,-z 14 -1/2+x,-1/2+y,-1/2-z 15 -y,x,-z 16 -1/2-y,-1/2+x,-1/2-z _cell_length_a 8.848(2) _cell_length_b 8.848(2) _cell_length_c 12.222(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 K 2.07 Mn 1.35 N 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z K1 K 0.00000 0.00000 0.50000 Mn1 Mn 0.00000 0.00000 0.00000 C1 C 0.00000 0.00000 0.1641(6) N1 N 0.00000 0.00000 0.2590(6) C2 C 0.1822(6) 0.1379(6) 0.00000 N2 N -0.2154(5) -0.2811(6) 0.50000 N3 N 0.00000 0.50000 0.25000 C3 C 0.1118(5) 0.4198(5) 0.1792(3) H1 H 0.2123(5) 0.4495(5) 0.1995(3) H2 H 0.0941(5) 0.4457(5) 0.1040(3) H3 H 0.1008(5) 0.3127(5) 0.1886(3) N1H N 0.00000 0.00000 0.7410(6) N2D N 0.2154(5) 0.2811(6) 0.50000 N2B N 0.2811(5) -0.2154(6) 0.50000 N2F N -0.2811(5) 0.2154(6) 0.50000 C1H C 0.00000 0.00000 -0.1641(6) C2D C -0.1822(6) -0.1379(6) 0.00000 C2B C -0.1379(6) 0.1822(6) 0.00000 C2F C 0.1379(6) -0.1822(6) 0.00000 N2A N 0.2846(5) 0.2189(6) 0.00000 C2A C -0.3178(6) -0.3621(6) 0.50000 C1H* C 0.00000 0.00000 0.8359(6) C2E C 0.3178(6) 0.3621(6) 0.50000 C2C C 0.3621(6) -0.3178(6) 0.50000 C2G C -0.3621(6) 0.3178(6) 0.50000 N1H* N 0.00000 0.00000 -0.2590(6) N2E N -0.2846(5) -0.2189(6) 0.00000 N2C N -0.2189(5) 0.2846(6) 0.00000 K1A K 0.50000 0.50000 0.00000 Mn1A Mn -0.50000 -0.50000 0.50000 Mn1A* Mn 0.50000 0.50000 0.50000 Mn1A** Mn 0.50000 -0.50000 0.50000 Mn1A*** Mn -0.50000 0.50000 0.50000 K1A* K -0.50000 -0.50000 0.00000 K1A** K -0.50000 0.50000 0.00000 N1A N 0.50000 0.50000 -0.2410(6) N1I N 0.50000 0.50000 0.2410(6) N2E* N 0.7154(5) 0.7811(6) 0.00000 N2C* N 0.7811(5) 0.2846(6) 0.00000 N2G N 0.2189(5) 0.7154(6) 0.00000 C1A C -0.50000 -0.50000 0.6641(6) C1I C -0.50000 -0.50000 0.3359(6) C2E* C -0.6822(6) -0.6379(6) 0.50000 C2C* C -0.6379(6) -0.3178(6) 0.50000 C2G* C -0.3621(6) -0.6822(6) 0.50000 N1A* N -0.50000 -0.50000 0.7590(6) N1I* N -0.50000 -0.50000 0.2410(6) C3K C -0.0802(5) 0.3882(5) 0.3208(3) C3D C -0.1118(5) 0.5802(5) 0.1792(3) C3O C 0.0802(5) 0.6118(5) 0.3208(3) H1K H -0.0505(5) 0.2877(5) 0.3005(3) H2K H -0.0543(5) 0.4059(5) 0.3960(3) H3K H -0.1873(5) 0.3992(5) 0.3114(3) H1D H -0.2123(5) 0.5505(5) 0.1995(3) H2D H -0.0941(5) 0.5543(5) 0.1040(3) H3D H -0.1008(5) 0.6873(5) 0.1886(3) H1O H 0.0505(5) 0.7123(5) 0.3005(3) H2O H 0.0543(5) 0.5941(5) 0.3960(3) H3O H 0.1873(5) 0.6008(5) 0.3114(3) Mn1* Mn 0.00000 0.00000 1.00000 K1* K 0.00000 0.00000 -0.50000 K1A*** K -0.50000 -0.50000 1.00000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 K1 N1 2.946 1_555 1_555 Mn1 C1 2.006 1_555 1_555 C1 N1 1.160 1_555 1_555 C2 Mn1 2.022 1_555 1_555 N2 K1 3.133 1_555 1_555 N3 C3 1.494 1_555 1_555 C3 H1 0.960 1_555 1_555 H2 C3 0.960 1_555 1_555 H3 C3 0.960 1_555 1_555 N1H K1 2.946 1_555 1_555 N2D K1 3.133 1_555 1_555 N2B K1 3.133 1_555 1_555 N2F K1 3.133 1_555 1_555 C1H Mn1 2.006 1_555 1_555 C2D Mn1 2.022 1_555 1_555 C2B Mn1 2.022 1_555 1_555 C2F Mn1 2.022 1_555 1_555 N2A C2 1.155 1_555 1_555 C2A N2 1.155 1_555 1_555 C1H* N1H 1.160 1_555 1_555 C2E N2D 1.155 1_555 1_555 C2C N2B 1.155 1_555 1_555 C2G N2F 1.155 1_555 1_555 N1H* C1H 1.160 1_555 1_555 N2E C2D 1.155 1_555 1_555 N2C C2B 1.155 1_555 1_555 K1A N2A 3.133 1_555 1_555 Mn1A C2A 2.022 1_555 1_555 Mn1A* C2E 2.022 1_555 1_555 Mn1A** C2C 2.022 1_555 1_555 Mn1A*** C2G 2.022 1_555 1_555 K1A* N2E 3.133 1_555 1_555 K1A** N2C 3.133 1_555 1_555 N1A K1A 2.946 1_555 1_555 N1I K1A 2.946 1_555 1_555 N2E* K1A 3.133 1_555 1_555 N2C* K1A 3.133 1_555 1_555 N2G K1A 3.133 1_555 1_555 C1A Mn1A 2.006 1_555 1_555 C1I Mn1A 2.006 1_555 1_555 C2E* Mn1A 2.022 1_555 1_555 C2C* Mn1A 2.022 1_555 1_555 C2G* Mn1A 2.022 1_555 1_555 N1A* C1A 1.160 1_555 1_555 N1I* K1A* 2.946 1_555 1_555 C3K N3 1.494 1_555 1_555 C3D N3 1.494 1_555 1_555 C3O N3 1.494 1_555 1_555 H1K C3K 0.960 1_555 1_555 H2K C3K 0.960 1_555 1_555 H3K C3K 0.960 1_555 1_555 H1D C3D 0.960 1_555 1_555 H2D C3D 0.960 1_555 1_555 H3D C3D 0.960 1_555 1_555 H1O C3O 0.960 1_555 1_555 H2O C3O 0.960 1_555 1_555 H3O C3O 0.960 1_555 1_555 Mn1* C1H* 2.006 1_555 1_555 K1* N1H* 2.946 1_555 1_555 K1A*** N1A* 2.946 1_555 1_555 C1I N1I* 1.160 1_555 1_555 #END data_CSD_CIF_VOJWAS _audit_creation_date 1992-06-24 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD VOJWAS _database_code_depnum_ccdc_fiz 'CSD 54838' _chemical_formula_sum 'C7 H12 Co0.5 N4 Rb0.5' _chemical_formula_moiety ; (C4 H12 N1 1+)n,0.25n(C12 Co2 N12 Rb2 4-) ; _journal_coden_Cambridge 29 _journal_volume 600 _journal_year 1991 _journal_page_first 239 _journal_name_full 'Z.Anorg.Allg.Chem. ' loop_ _publ_author_name "B.Ziegler" "M.Witzel" "D.Babel" _chemical_name_systematic ; catena-(bis(Tetramethylammonium) hexakis(\m~2~-cyano)-cobalt-rubidium) ; _cell_volume 965.140 _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.54 _exptl_special_details ; Isostructural with the potassium manganese analogue CSD 54838 adds no new information ; _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_gt 0.0437 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 4/m' _symmetry_Int_Tables_number 87 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,1/2+z 3 -y,x,z 4 1/2-y,1/2+x,1/2+z 5 -x,-y,z 6 1/2-x,1/2-y,1/2+z 7 y,-x,z 8 1/2+y,1/2-x,1/2+z 9 -x,-y,-z 10 -1/2-x,-1/2-y,-1/2-z 11 y,-x,-z 12 -1/2+y,-1/2-x,-1/2-z 13 x,y,-z 14 -1/2+x,-1/2+y,-1/2-z 15 -y,x,-z 16 -1/2-y,-1/2+x,-1/2-z _cell_length_a 8.847(1) _cell_length_b 8.847(1) _cell_length_c 12.331(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Co 1.33 N 0.68 Rb 2.18 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Rb1 Rb 0.00000 0.00000 0.50000 Co1 Co 0.00000 0.00000 0.00000 C1 C 0.00000 0.00000 0.1542(7) N1 N 0.00000 0.00000 0.2476(11) C2 C 0.1710(8) 0.1317(8) 0.00000 N2 N -0.2269(7) -0.2883(7) 0.50000 N3 N 0.00000 0.50000 0.25000 C3 C 0.1149(8) 0.4234(8) 0.1810(6) H1 H 0.2185(8) 0.4520(8) 0.2061(6) H2 H 0.1013(8) 0.4553(8) 0.1038(6) H3 H 0.1021(8) 0.3113(8) 0.1867(6) N1H N 0.00000 0.00000 0.7524(11) N2D N 0.2269(7) 0.2883(7) 0.50000 N2B N 0.2883(7) -0.2269(7) 0.50000 N2F N -0.2883(7) 0.2269(7) 0.50000 C1H C 0.00000 0.00000 -0.1542(7) C2D C -0.1710(8) -0.1317(8) 0.00000 C2B C -0.1317(8) 0.1710(8) 0.00000 C2F C 0.1317(8) -0.1710(8) 0.00000 N2A N 0.2731(7) 0.2117(7) 0.00000 C2A C -0.3290(8) -0.3683(8) 0.50000 C1H* C 0.00000 0.00000 0.8458(7) C2E C 0.3290(8) 0.3683(8) 0.50000 C2C C 0.3683(8) -0.3290(8) 0.50000 C2G C -0.3683(8) 0.3290(8) 0.50000 N1H* N 0.00000 0.00000 -0.2476(11) N2E N -0.2731(7) -0.2117(7) 0.00000 N2C N -0.2117(7) 0.2731(7) 0.00000 Rb1A Rb 0.50000 0.50000 0.00000 Co1A Co -0.50000 -0.50000 0.50000 Co1A* Co 0.50000 0.50000 0.50000 Co1A** Co 0.50000 -0.50000 0.50000 Co1A*** Co -0.50000 0.50000 0.50000 Rb1A* Rb -0.50000 -0.50000 0.00000 Rb1A** Rb -0.50000 0.50000 0.00000 N1A N 0.50000 0.50000 -0.2524(11) N1I N 0.50000 0.50000 0.2524(11) N2E* N 0.7269(7) 0.7883(7) 0.00000 N2C* N 0.7883(7) 0.2731(7) 0.00000 N2G N 0.2117(7) 0.7269(7) 0.00000 C1A C -0.50000 -0.50000 0.6542(7) C1I C -0.50000 -0.50000 0.3458(7) C2E* C -0.6710(8) -0.6317(8) 0.50000 C2C* C -0.6317(8) -0.3290(8) 0.50000 C2G* C -0.3683(8) -0.6710(8) 0.50000 N1A* N -0.50000 -0.50000 0.7476(11) N1I* N -0.50000 -0.50000 0.2524(11) C3K C -0.0766(8) 0.3851(8) 0.3190(6) C3D C -0.1149(8) 0.5766(8) 0.1810(6) C3O C 0.0766(8) 0.6149(8) 0.3190(6) H1K H -0.0480(8) 0.2815(8) 0.2939(6) H2K H -0.0447(8) 0.3987(8) 0.3962(6) H3K H -0.1887(8) 0.3979(8) 0.3133(6) H1D H -0.2185(8) 0.5480(8) 0.2061(6) H2D H -0.1013(8) 0.5447(8) 0.1038(6) H3D H -0.1021(8) 0.6887(8) 0.1867(6) H1O H 0.0480(8) 0.7185(8) 0.2939(6) H2O H 0.0447(8) 0.6013(8) 0.3962(6) H3O H 0.1887(8) 0.6021(8) 0.3133(6) Co1* Co 0.00000 0.00000 1.00000 Rb1* Rb 0.00000 0.00000 -0.50000 Rb1A*** Rb -0.50000 -0.50000 1.00000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rb1 N1 3.112 1_555 1_555 Co1 C1 1.901 1_555 1_555 C1 N1 1.152 1_555 1_555 C2 Co1 1.910 1_555 1_555 N2 Rb1 3.246 1_555 1_555 N3 C3 1.489 1_555 1_555 C3 H1 1.000 1_555 1_555 H2 C3 1.000 1_555 1_555 H3 C3 1.001 1_555 1_555 N1H Rb1 3.112 1_555 1_555 N2D Rb1 3.246 1_555 1_555 N2B Rb1 3.246 1_555 1_555 N2F Rb1 3.246 1_555 1_555 C1H Co1 1.901 1_555 1_555 C2D Co1 1.910 1_555 1_555 C2B Co1 1.910 1_555 1_555 C2F Co1 1.910 1_555 1_555 N2A C2 1.148 1_555 1_555 C2A N2 1.148 1_555 1_555 C1H* N1H 1.152 1_555 1_555 C2E N2D 1.148 1_555 1_555 C2C N2B 1.148 1_555 1_555 C2G N2F 1.148 1_555 1_555 N1H* C1H 1.152 1_555 1_555 N2E C2D 1.148 1_555 1_555 N2C C2B 1.148 1_555 1_555 Rb1A N2A 3.246 1_555 1_555 Co1A C2A 1.910 1_555 1_555 Co1A* C2E 1.910 1_555 1_555 Co1A** C2C 1.910 1_555 1_555 Co1A*** C2G 1.910 1_555 1_555 Rb1A* N2E 3.246 1_555 1_555 Rb1A** N2C 3.246 1_555 1_555 N1A Rb1A 3.112 1_555 1_555 N1I Rb1A 3.112 1_555 1_555 N2E* Rb1A 3.246 1_555 1_555 N2C* Rb1A 3.246 1_555 1_555 N2G Rb1A 3.246 1_555 1_555 C1A Co1A 1.901 1_555 1_555 C1I Co1A 1.901 1_555 1_555 C2E* Co1A 1.910 1_555 1_555 C2C* Co1A 1.910 1_555 1_555 C2G* Co1A 1.910 1_555 1_555 N1A* C1A 1.152 1_555 1_555 N1I* Rb1A* 3.112 1_555 1_555 C3K N3 1.489 1_555 1_555 C3D N3 1.489 1_555 1_555 C3O N3 1.489 1_555 1_555 H1K C3K 1.000 1_555 1_555 H2K C3K 1.000 1_555 1_555 H3K C3K 1.001 1_555 1_555 H1D C3D 1.000 1_555 1_555 H2D C3D 1.000 1_555 1_555 H3D C3D 1.001 1_555 1_555 H1O C3O 1.000 1_555 1_555 H2O C3O 1.000 1_555 1_555 H3O C3O 1.001 1_555 1_555 Co1* C1H* 1.901 1_555 1_555 Rb1* N1H* 3.112 1_555 1_555 Rb1A*** N1A* 3.112 1_555 1_555 C1I N1I* 1.152 1_555 1_555 #END data_CSD_CIF_VOSJIW _audit_creation_date 1992-11-02 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD VOSJIW _database_code_depnum_ccdc_fiz 'CSD 55793' _chemical_formula_sum 'C46 H100 Li2 N2 O9 Si3' _chemical_formula_moiety ; C30 H68 Li1 N2 O1 Si3 1-,C16 H32 Li1 O8 1+ ; _journal_coden_Cambridge 36 _journal_volume 426 _journal_year 1992 _journal_page_first 287 _journal_name_full 'J.Organomet.Chem. ' loop_ _publ_author_name "B.Tecklenburg" "U.Klingebiel" "D.Schmidt-Base" _chemical_name_systematic ; Lithium-bis(12-crown-4) (di-t-butylsilylbis(di-t-butyl(methyl)silyl)diamide-N,N)tetrahydrofuran-lithiu m ; _cell_volume 3241.039 _exptl_special_details ; Dx reported as 1.1; we calculate 0.95 ; _diffrn_ambient_temperature 153.15 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_gt 0.0487 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 13.689(2) _cell_length_b 15.102(3) _cell_length_c 16.618(3) _cell_angle_alpha 81.08(1) _cell_angle_beta 74.70(1) _cell_angle_gamma 79.92(1) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.36 N 0.68 O 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Si1 Si 0.2824(1) 0.2397(1) 0.3440(1) N1 N 0.4075(2) 0.2450(1) 0.3144(1) Si2 Si 0.5201(1) 0.2508(1) 0.2414(1) N2 N 0.6059(2) 0.2683(1) 0.2931(1) Si3 Si 0.7117(1) 0.3049(1) 0.2974(1) Li1 Li 0.4907(3) 0.2511(3) 0.3935(3) Li2 Li 0.1213(4) 0.2490(3) -0.0825(3) C1 C 0.2237(2) 0.2138(2) 0.2600(2) C2 C 0.2035(2) 0.3540(2) 0.3781(2) C3 C 0.2555(2) 0.3954(2) 0.4310(2) C4 C 0.0920(2) 0.3484(2) 0.4274(2) C5 C 0.1979(2) 0.4208(2) 0.2986(2) C6 C 0.2456(2) 0.1419(2) 0.4333(2) C7 C 0.2444(2) 0.1628(2) 0.5207(2) C8 C 0.1402(2) 0.1145(2) 0.4389(2) C9 C 0.3246(2) 0.0587(2) 0.4135(2) C10 C 0.5068(2) 0.3479(2) 0.1497(2) C11 C 0.6014(2) 0.3521(2) 0.0748(2) C12 C 0.4154(2) 0.3460(2) 0.1125(2) C13 C 0.4888(2) 0.4377(2) 0.1871(2) C14 C 0.5664(2) 0.1351(2) 0.1937(2) C15 C 0.4839(2) 0.1040(2) 0.1619(2) C16 C 0.6638(2) 0.1339(2) 0.1228(2) C17 C 0.5900(2) 0.0635(2) 0.2655(2) C18 C 0.7849(2) 0.3637(2) 0.1960(2) C19 C 0.8125(2) 0.2064(2) 0.3272(2) C20 C 0.9041(2) 0.2370(2) 0.3470(2) C21 C 0.7645(2) 0.1419(2) 0.4029(2) C22 C 0.8554(2) 0.1515(2) 0.2520(2) C23 C 0.6852(2) 0.3967(2) 0.3747(2) C24 C 0.5856(2) 0.4582(2) 0.3675(2) C25 C 0.6721(3) 0.3560(2) 0.4672(2) C26 C 0.7697(3) 0.4582(2) 0.3556(2) O1 O 0.4729(1) 0.2307(1) 0.5167(1) C27 C 0.5022(2) 0.1477(2) 0.5649(2) C28 C 0.5286(4) 0.1749(3) 0.6382(3) C29 C 0.4796(3) 0.2712(2) 0.6463(2) C30 C 0.4267(2) 0.2962(2) 0.5750(2) O2 O -0.0451(1) 0.3141(2) -0.0746(1) C31 C -0.0702(3) 0.3564(3) -0.1515(2) C32 C 0.0197(3) 0.4026(2) -0.2000(2) O3 O 0.1121(2) 0.3421(1) -0.2122(1) C33 C 0.1283(3) 0.2892(2) -0.2791(2) C34 C 0.2082(3) 0.2114(2) -0.2652(2) O4 O 0.1764(2) 0.1597(1) -0.1860(1) C35 C 0.1142(3) 0.0944(2) -0.1888(2) C36 C 0.0717(3) 0.0583(2) -0.0993(2) O5 O 0.0183(2) 0.1294(2) -0.0504(1) C37 C -0.0821(3) 0.1605(3) -0.0600(2) C38 C -0.1131(2) 0.2513(3) -0.0280(2) O6 O 0.2950(2) 0.2849(1) -0.1316(1) C39 C 0.3690(2) 0.2297(2) -0.0926(2) C40 C 0.3401(2) 0.1355(2) -0.0742(2) O7 O 0.2386(2) 0.1339(1) -0.0247(1) C41 C 0.2268(2) 0.1383(2) 0.0624(2) C42 C 0.1148(2) 0.1563(2) 0.0999(2) O8 O 0.0713(2) 0.2413(1) 0.0630(1) C43 C 0.0838(2) 0.3170(2) 0.0990(2) C44 C 0.0620(3) 0.3990(2) 0.0391(2) O9 O 0.1278(2) 0.3921(1) -0.0428(1) C45 C 0.2286(3) 0.4113(2) -0.0507(2) C46 C 0.2925(3) 0.3799(2) -0.1313(2) O10 O 0.9261(2) 0.1680(1) 0.6800(1) C47 C 0.9048(3) 0.0766(2) 0.6917(3) C48 C 0.7972(3) 0.0664(2) 0.7431(2) O11 O 0.7916(2) 0.0778(1) 0.8269(2) C49 C 0.6904(3) 0.1028(2) 0.8749(2) C50 C 0.6611(3) 0.2039(2) 0.8723(2) O12 O 0.6399(2) 0.2387(1) 0.7948(1) C51 C 0.6339(3) 0.3356(2) 0.7786(2) C52 C 0.7030(3) 0.3609(2) 0.6955(2) O13 O 0.8052(2) 0.3417(1) 0.7038(1) C53 C 0.8776(2) 0.3193(2) 0.6276(2) C54 C 0.8858(3) 0.2235(2) 0.6155(2) H1 H 0.23760 0.26000 0.20980 H2 H 0.25460 0.15220 0.24330 H3 H 0.14820 0.21550 0.28270 H4 H 0.21390 0.45390 0.44790 H5 H 0.26140 0.35270 0.48250 H6 H 0.32530 0.40670 0.39750 H7 H 0.05760 0.40990 0.44220 H8 H 0.05480 0.32590 0.39210 H9 H 0.09110 0.30580 0.48000 H10 H 0.15750 0.47980 0.31530 H11 H 0.26860 0.43070 0.26630 H12 H 0.16390 0.39520 0.26290 H13 H 0.22500 0.11010 0.56300 H14 H 0.31390 0.17440 0.52130 H15 H 0.19350 0.21770 0.53520 H16 H 0.12580 0.06450 0.48560 H17 H 0.08600 0.16780 0.45020 H18 H 0.14070 0.09340 0.38470 H19 H 0.30770 0.00750 0.45830 H20 H 0.32410 0.04120 0.35800 H21 H 0.39410 0.07280 0.41120 H22 H 0.58670 0.40360 0.03200 H23 H 0.66110 0.36150 0.09490 H24 H 0.61760 0.29410 0.04900 H25 H 0.41300 0.39680 0.06640 H26 H 0.42350 0.28700 0.08960 H27 H 0.35050 0.35280 0.15750 H28 H 0.48150 0.48920 0.14240 H29 H 0.42490 0.44040 0.23330 H30 H 0.54820 0.44210 0.21000 H31 H 0.51130 0.04510 0.13830 H32 H 0.42250 0.09620 0.20950 H33 H 0.46410 0.15060 0.11700 H34 H 0.68200 0.07290 0.10220 H35 H 0.65210 0.18100 0.07560 H36 H 0.72100 0.14680 0.14420 H37 H 0.61400 0.00320 0.24390 H38 H 0.64470 0.08100 0.28710 H39 H 0.52670 0.05990 0.31190 H40 H 0.80290 0.32240 0.15110 H41 H 0.74160 0.42020 0.17860 H42 H 0.84900 0.37960 0.20470 H43 H 0.95210 0.18260 0.36170 H44 H 0.94050 0.27450 0.29670 H45 H 0.87940 0.27370 0.39540 H46 H 0.81860 0.09220 0.41630 H47 H 0.73390 0.17620 0.45260 H48 H 0.71000 0.11520 0.38890 H49 H 0.90760 0.10020 0.26590 H50 H 0.79860 0.12690 0.23930 H51 H 0.88800 0.19140 0.20190 H52 H 0.57090 0.50560 0.40670 H53 H 0.59270 0.48800 0.30860 H54 H 0.52810 0.42130 0.38270 H55 H 0.65880 0.40580 0.50350 H56 H 0.61310 0.32070 0.48410 H57 H 0.73590 0.31490 0.47400 H58 H 0.75130 0.50330 0.39720 H59 H 0.83640 0.42030 0.35950 H60 H 0.77620 0.49080 0.29770 H61 H 0.56270 0.11120 0.53080 H62 H 0.44460 0.11080 0.58400 H63 H 0.60450 0.16990 0.62900 H64 H 0.50170 0.13490 0.69050 H65 H 0.53240 0.31140 0.64070 H66 H 0.42910 0.27630 0.70180 H67 H 0.35160 0.29370 0.59620 H68 H 0.43690 0.35880 0.54740 H69 H -0.13370 0.40150 -0.13970 H70 H -0.08160 0.31020 -0.18380 H71 H 0.02570 0.45240 -0.16910 H72 H 0.00790 0.43030 -0.25590 H73 H 0.15220 0.32570 -0.33420 H74 H 0.06360 0.26700 -0.27880 H75 H 0.27310 0.23470 -0.26770 H76 H 0.22220 0.17160 -0.31100 H77 H 0.15590 0.04450 -0.22140 H78 H 0.05760 0.12320 -0.21600 H79 H 0.12890 0.02510 -0.07460 H80 H 0.02400 0.01440 -0.09750 H81 H -0.12980 0.11740 -0.02710 H82 H -0.08340 0.16600 -0.12040 H83 H -0.18440 0.27560 -0.03270 H84 H -0.11250 0.24460 0.03270 H85 H 0.36880 0.25300 -0.03950 H86 H 0.43890 0.22950 -0.13100 H87 H 0.38840 0.09530 -0.04390 H88 H 0.34700 0.11110 -0.12840 H89 H 0.26160 0.18810 0.07040 H90 H 0.25710 0.07990 0.08930 H91 H 0.10230 0.15730 0.16190 H92 H 0.08090 0.10650 0.09060 H93 H 0.15510 0.31120 0.10590 H94 H 0.03490 0.32140 0.15520 H95 H 0.07170 0.45420 0.06070 H96 H 0.01090 0.40580 0.03560 H97 H 0.25620 0.37860 -0.00250 H98 H 0.22790 0.47780 -0.05140 H99 H 0.26420 0.41370 -0.17880 H100 H 0.36380 0.39350 -0.14020 H101 H 0.95490 0.03670 0.72050 H102 H 0.91450 0.05580 0.63550 H103 H 0.78110 0.00500 0.74030 H104 H 0.74660 0.11290 0.72060 H105 H 0.68490 0.07580 0.93460 H106 H 0.64130 0.07720 0.85290 H107 H 0.71840 0.23190 0.88030 H108 H 0.59940 0.21860 0.91870 H109 H 0.65420 0.35950 0.82380 H110 H 0.56190 0.36320 0.77870 H111 H 0.68610 0.42670 0.67700 H112 H 0.69410 0.32540 0.65240 H113 H 0.94630 0.33270 0.62860 H114 H 0.85640 0.35830 0.57890 H115 H 0.81680 0.20850 0.61750 H116 H 0.93180 0.21200 0.55930 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Si1 N1 1.665 1_555 1_555 N1 Si2 1.698 1_555 1_555 Si2 N2 1.703 1_555 1_555 N2 Si3 1.660 1_555 1_555 Si3 C18 1.894 1_555 1_555 Li1 N1 1.974 1_555 1_555 Li2 O2 2.296 1_555 1_555 C1 Si1 1.902 1_555 1_555 C2 Si1 1.948 1_555 1_555 C3 C2 1.525 1_555 1_555 C4 C2 1.540 1_555 1_555 C5 C2 1.543 1_555 1_555 C6 Si1 1.955 1_555 1_555 C7 C6 1.529 1_555 1_555 C8 C6 1.545 1_555 1_555 C9 C6 1.524 1_555 1_555 C10 Si2 1.966 1_555 1_555 C11 C10 1.544 1_555 1_555 C12 C10 1.541 1_555 1_555 C13 C10 1.533 1_555 1_555 C14 Si2 1.965 1_555 1_555 C15 C14 1.534 1_555 1_555 C16 C14 1.528 1_555 1_555 C17 C14 1.542 1_555 1_555 C18 H40 1.000 1_555 1_555 C19 Si3 1.943 1_555 1_555 C20 C19 1.537 1_555 1_555 C21 C19 1.540 1_555 1_555 C22 C19 1.535 1_555 1_555 C23 Si3 1.958 1_555 1_555 C24 C23 1.531 1_555 1_555 C25 C23 1.540 1_555 1_555 C26 C23 1.547 1_555 1_555 O1 Li1 1.978 1_555 1_555 C27 O1 1.434 1_555 1_555 C28 C27 1.491 1_555 1_555 C29 C28 1.502 1_555 1_555 C30 O1 1.439 1_555 1_555 O2 C31 1.436 1_555 1_555 C31 C32 1.501 1_555 1_555 C32 O3 1.412 1_555 1_555 O3 Li2 2.404 1_555 1_555 C33 O3 1.417 1_555 1_555 C34 C33 1.493 1_555 1_555 O4 Li2 2.242 1_555 1_555 C35 O4 1.424 1_555 1_555 C36 C35 1.500 1_555 1_555 O5 Li2 2.394 1_555 1_555 C37 O5 1.415 1_555 1_555 C38 O2 1.438 1_555 1_555 O6 Li2 2.430 1_555 1_555 C39 O6 1.423 1_555 1_555 C40 C39 1.507 1_555 1_555 O7 Li2 2.417 1_555 1_555 C41 O7 1.424 1_555 1_555 C42 C41 1.488 1_555 1_555 O8 Li2 2.323 1_555 1_555 C43 O8 1.424 1_555 1_555 C44 C43 1.503 1_555 1_555 O9 Li2 2.378 1_555 1_555 C45 O9 1.428 1_555 1_555 C46 O6 1.430 1_555 1_555 O10 C47 1.434 1_555 1_555 C47 C48 1.516 1_555 1_555 C48 O11 1.410 1_555 1_555 O11 C49 1.423 1_555 1_555 C49 C50 1.506 1_555 1_555 C50 O12 1.398 1_555 1_555 O12 C51 1.438 1_555 1_555 C51 C52 1.490 1_555 1_555 C52 O13 1.417 1_555 1_555 O13 C53 1.433 1_555 1_555 C53 C54 1.472 1_555 1_555 C54 O10 1.424 1_555 1_555 H1 C1 1.001 1_555 1_555 H2 C1 1.001 1_555 1_555 H3 C1 1.000 1_555 1_555 H4 C3 1.000 1_555 1_555 H5 C3 1.001 1_555 1_555 H6 C3 0.999 1_555 1_555 H7 C4 1.001 1_555 1_555 H8 C4 0.999 1_555 1_555 H9 C4 1.000 1_555 1_555 H10 C5 1.000 1_555 1_555 H11 C5 0.999 1_555 1_555 H12 C5 0.999 1_555 1_555 H13 C7 1.000 1_555 1_555 H14 C7 1.000 1_555 1_555 H15 C7 1.001 1_555 1_555 H16 C8 1.000 1_555 1_555 H17 C8 0.999 1_555 1_555 H18 C8 0.999 1_555 1_555 H19 C9 0.999 1_555 1_555 H20 C9 1.000 1_555 1_555 H21 C9 1.001 1_555 1_555 H22 C11 1.000 1_555 1_555 H23 C11 0.999 1_555 1_555 H24 C11 0.999 1_555 1_555 H25 C12 0.999 1_555 1_555 H26 C12 1.000 1_555 1_555 H27 C12 1.000 1_555 1_555 H28 C13 1.000 1_555 1_555 H29 C13 1.000 1_555 1_555 H30 C13 1.000 1_555 1_555 H31 C15 1.000 1_555 1_555 H32 C15 1.000 1_555 1_555 H33 C15 1.001 1_555 1_555 H34 C16 1.000 1_555 1_555 H35 C16 1.000 1_555 1_555 H36 C16 1.000 1_555 1_555 H37 C17 1.000 1_555 1_555 H38 C17 1.000 1_555 1_555 H39 C17 1.000 1_555 1_555 H41 C18 1.000 1_555 1_555 H42 C18 1.000 1_555 1_555 H43 C20 1.000 1_555 1_555 H44 C20 1.000 1_555 1_555 H45 C20 0.999 1_555 1_555 H46 C21 1.001 1_555 1_555 H47 C21 1.000 1_555 1_555 H48 C21 1.000 1_555 1_555 H49 C22 1.001 1_555 1_555 H50 C22 1.000 1_555 1_555 H51 C22 0.999 1_555 1_555 H52 C24 1.001 1_555 1_555 H53 C24 0.999 1_555 1_555 H54 C24 0.999 1_555 1_555 H55 C25 0.999 1_555 1_555 H56 C25 1.000 1_555 1_555 H57 C25 1.001 1_555 1_555 H58 C26 1.000 1_555 1_555 H59 C26 1.001 1_555 1_555 H60 C26 1.000 1_555 1_555 H61 C27 1.000 1_555 1_555 H62 C27 1.000 1_555 1_555 H63 C28 1.000 1_555 1_555 H64 C28 1.001 1_555 1_555 H65 C29 1.000 1_555 1_555 H66 C29 1.001 1_555 1_555 H67 C30 1.000 1_555 1_555 H68 C30 1.001 1_555 1_555 H69 C31 1.001 1_555 1_555 H70 C31 0.999 1_555 1_555 H71 C32 1.000 1_555 1_555 H72 C32 1.000 1_555 1_555 H73 C33 0.999 1_555 1_555 H74 C33 0.999 1_555 1_555 H75 C34 1.000 1_555 1_555 H76 C34 1.001 1_555 1_555 H77 C35 1.000 1_555 1_555 H78 C35 1.000 1_555 1_555 H79 C36 1.001 1_555 1_555 H80 C36 1.001 1_555 1_555 H81 C37 0.999 1_555 1_555 H82 C37 0.999 1_555 1_555 H83 C38 1.000 1_555 1_555 H84 C38 1.000 1_555 1_555 H85 C39 0.999 1_555 1_555 H86 C39 1.000 1_555 1_555 H87 C40 1.000 1_555 1_555 H88 C40 1.001 1_555 1_555 H89 C41 1.000 1_555 1_555 H90 C41 0.999 1_555 1_555 H91 C42 1.001 1_555 1_555 H92 C42 1.000 1_555 1_555 H93 C43 1.000 1_555 1_555 H94 C43 0.999 1_555 1_555 H95 C44 0.999 1_555 1_555 H96 C44 0.705 1_555 1_555 H97 C45 1.000 1_555 1_555 H98 C45 1.001 1_555 1_555 H99 C46 1.000 1_555 1_555 H100 C46 1.001 1_555 1_555 H101 C47 1.001 1_555 1_555 H102 C47 1.000 1_555 1_555 H103 C48 1.000 1_555 1_555 H104 C48 0.999 1_555 1_555 H105 C49 1.001 1_555 1_555 H106 C49 1.000 1_555 1_555 H107 C50 1.000 1_555 1_555 H108 C50 1.000 1_555 1_555 H109 C51 1.001 1_555 1_555 H110 C51 1.000 1_555 1_555 H111 C52 0.999 1_555 1_555 H112 C52 1.002 1_555 1_555 H113 C53 1.001 1_555 1_555 H114 C53 1.001 1_555 1_555 H115 C54 1.000 1_555 1_555 H116 C54 1.000 1_555 1_555 Si2 Li1 2.453 1_555 1_555 N2 Li1 1.990 1_555 1_555 C29 C30 1.513 1_555 1_555 C34 O4 1.425 1_555 1_555 C36 O5 1.425 1_555 1_555 C37 C38 1.499 1_555 1_555 C40 O7 1.418 1_555 1_555 C42 O8 1.435 1_555 1_555 C44 O9 1.428 1_555 1_555 C45 C46 1.489 1_555 1_555 #END data_CSD_CIF_WELBEV _audit_creation_date 2006-11-14 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD WELBEV _database_code_depnum_ccdc_archive 'CCDC 619432' _chemical_formula_sum 'C162 H198 K2 N10 O8 Th2' _chemical_formula_moiety ; C16 H40 K1 O8 1+,C122 H102 K1 N10 Th2 1-,4(C6 H14) ; _journal_coden_Cambridge 579 _journal_volume 25 _journal_year 2006 _journal_page_first 3856 _journal_name_full 'Organometallics ' loop_ _publ_author_name "A.Arunachalampillai" "P.Crewdson" "I.Korobkov" "S.Gambarotta" _chemical_name_systematic ; tetrakis(Dimethoxyethane)-potassium bis(\m~2~-\h^5^,\h^2^-2,5-bis(2-pyrrolyl(diphenyl)methyl)-N-methylpyrrolide)-( \m~2~-\h^5^,\h^5^-7-(2-pyrrolyl)-7,7-diphenyl-2-azahepta-3,5-dien-2-yl)-potass ium-di-thorium hexane solvate ; _cell_volume 13414.805 _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.444 _exptl_crystal_description 'plate' _diffrn_ambient_temperature 208 _refine_special_details ; The four dimethoxyethane ligands and the hexane solvent molecules have been removed using SQUEEZE/PLATON. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_gt 0.0768 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,z 3 -x,y,1/2-z 4 1/2-x,1/2+y,1/2-z 5 -x,-y,-z 6 -1/2-x,-1/2-y,-z 7 x,-y,-1/2+z 8 -1/2+x,-1/2-y,-1/2+z _cell_length_a 17.67(7) _cell_length_b 29.83(14) _cell_length_c 25.61(15) _cell_angle_alpha 90 _cell_angle_beta 96.4(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.82 H 0.23 K 2.27 N 0.68 Th 1.99 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Th1 Th 0.72261(2) 0.526097(19) 0.664354(18) K1 K 1.00000 0.57425(18) 0.75000 K2 K 0.50000 0.77389(19) 0.75000 N1 N 0.6996(5) 0.4508(3) 0.7017(4) N2 N 0.7511(5) 0.4531(4) 0.5920(3) N3 N 0.8384(5) 0.5461(4) 0.6240(4) N4 N 0.6369(7) 0.5807(5) 0.6241(4) N5 N 0.8253(5) 0.5264(4) 0.7392(4) C1 C 0.7216(8) 0.4436(6) 0.7546(5) H1 H 0.73930 0.46590 0.77890 C2 C 0.7138(8) 0.3993(6) 0.7663(5) H2 H 0.72350 0.38620 0.79970 C3 C 0.6883(7) 0.3765(5) 0.7186(5) H3 H 0.67950 0.34570 0.71340 C4 C 0.6796(6) 0.4113(4) 0.6811(4) C5 C 0.6426(6) 0.4085(5) 0.6244(4) C6 C 0.6740(7) 0.4461(5) 0.5953(4) C7 C 0.6364(7) 0.4776(5) 0.5647(5) H4 H 0.58330 0.48200 0.56040 C8 C 0.6898(7) 0.5028(5) 0.5405(4) H5 H 0.67860 0.52650 0.51670 C9 C 0.7603(6) 0.4870(4) 0.5573(4) C10 C 0.8130(7) 0.4259(5) 0.6181(5) H6 H 0.82400 0.40140 0.59520 H7 H 0.79790 0.41390 0.65060 H8 H 0.85810 0.44430 0.62580 C11 C 0.8380(7) 0.5008(4) 0.5408(4) C12 C 0.8809(7) 0.5278(5) 0.5865(4) C13 C 0.9471(7) 0.5503(5) 0.5867(5) H9 H 0.98520 0.54460 0.56480 C14 C 0.9489(7) 0.5838(5) 0.6258(5) H10 H 0.98830 0.60450 0.63490 C15 C 0.8821(8) 0.5803(5) 0.6475(5) H11 H 0.86800 0.59850 0.67470 C16 C 0.5242(7) 0.4358(5) 0.6635(5) H12 H 0.55640 0.44550 0.69300 C17 C 0.4465(7) 0.4418(5) 0.6615(6) H13 H 0.42560 0.45290 0.69110 C18 C 0.3988(7) 0.4316(5) 0.6161(6) H14 H 0.34670 0.43890 0.61320 C19 C 0.4299(9) 0.4106(6) 0.5754(5) H15 H 0.39850 0.40040 0.54570 C20 C 0.5068(7) 0.4050(5) 0.5791(5) H16 H 0.52810 0.39310 0.55010 C21 C 0.5543(6) 0.4157(5) 0.6226(5) C22 C 0.6239(8) 0.3228(6) 0.6188(5) H17 H 0.59640 0.32440 0.64810 C23 C 0.6333(9) 0.2830(6) 0.5967(6) H18 H 0.61400 0.25760 0.61250 C24 C 0.6688(8) 0.2768(5) 0.5531(6) H19 H 0.67370 0.24830 0.53820 C25 C 0.6964(8) 0.3139(6) 0.5323(6) H20 H 0.72060 0.31080 0.50150 C26 C 0.6912(7) 0.3576(6) 0.5541(5) H21 H 0.71230 0.38250 0.53850 C27 C 0.6538(7) 0.3627(5) 0.5998(5) C28 C 0.8375(7) 0.4303(5) 0.4914(5) H22 H 0.78640 0.43650 0.47930 C29 C 0.8685(8) 0.3918(5) 0.4761(5) H23 H 0.83920 0.37230 0.45310 C30 C 0.9442(9) 0.3804(7) 0.4943(6) H24 H 0.96580 0.35360 0.48370 C31 C 0.9856(8) 0.4093(6) 0.5275(6) H25 H 1.03610 0.40210 0.54030 C32 C 0.9528(8) 0.4503(5) 0.5431(5) H26 H 0.98100 0.47030 0.56590 C33 C 0.8769(6) 0.4600(4) 0.5231(4) C34 C 0.8326(7) 0.5266(5) 0.4438(5) H27 H 0.84820 0.49770 0.43520 C35 C 0.8203(7) 0.5592(6) 0.4045(6) H28 H 0.82620 0.55180 0.36950 C36 C 0.7999(8) 0.6012(6) 0.4167(5) H29 H 0.79180 0.62320 0.39040 C37 C 0.7909(7) 0.6116(5) 0.4679(5) H30 H 0.77610 0.64080 0.47640 C38 C 0.8030(7) 0.5805(5) 0.5063(5) H31 H 0.79840 0.58900 0.54110 C39 C 0.8218(6) 0.5369(5) 0.4965(5) C40 C 0.6215(9) 0.6039(6) 0.5745(5) H32 H 0.57850 0.62400 0.57590 H33 H 0.60960 0.58220 0.54660 H34 H 0.66590 0.62110 0.56770 C41 C 0.5765(8) 0.5635(5) 0.6435(6) H35 H 0.54250 0.54640 0.61740 C42 C 0.5747(7) 0.5492(5) 0.6934(5) H36 H 0.54030 0.52370 0.69790 C43 C 0.6289(7) 0.5604(5) 0.7396(5) H37 H 0.62500 0.53790 0.76760 C44 C 0.7028(6) 0.5718(5) 0.7378(4) C45 C 0.7591(7) 0.5850(5) 0.7840(5) C46 C 0.8176(7) 0.5474(5) 0.7847(5) C47 C 0.8725(7) 0.5338(5) 0.8240(5) H38 H 0.87170 0.53850 0.86230 C48 C 0.9159(7) 0.5017(5) 0.7999(5) H39 H 0.94240 0.47670 0.81980 C49 C 0.8848(7) 0.4972(5) 0.7487(5) H40 H 0.88910 0.46940 0.72820 C50 C 0.7022(7) 0.5492(5) 0.8611(5) H41 H 0.71880 0.52130 0.84960 C51 C 0.6598(7) 0.5500(7) 0.9046(5) H42 H 0.64790 0.52320 0.92110 C52 C 0.6363(8) 0.5900(6) 0.9223(5) H43 H 0.60860 0.59140 0.95150 C53 C 0.6537(8) 0.6281(7) 0.8967(6) H44 H 0.63810 0.65600 0.90910 C54 C 0.6945(8) 0.6271(7) 0.8522(6) H45 H 0.70380 0.65380 0.83450 C55 C 0.7204(7) 0.5870(6) 0.8348(5) C56 C 0.8593(10) 0.6404(5) 0.8114(7) H46 H 0.87160 0.62280 0.84160 C57 C 0.9012(10) 0.6780(6) 0.8033(8) H47 H 0.93950 0.68720 0.82950 C58 C 0.8887(10) 0.7018(8) 0.7592(11) H48 H 0.91960 0.72630 0.75270 C59 C 0.8280(13) 0.6888(7) 0.7230(8) H49 H 0.81640 0.70600 0.69240 C60 C 0.7854(9) 0.6524(6) 0.7305(6) H50 H 0.74610 0.64390 0.70460 C61 C 0.7988(7) 0.6282(5) 0.7748(6) Th1B Th 1.27739(2) 0.526097(19) 0.835646(18) N1B N 1.3004(5) 0.4508(3) 0.7983(4) N2B N 1.2489(5) 0.4531(4) 0.9080(3) N3B N 1.1616(5) 0.5461(4) 0.8760(4) N4B N 1.3631(7) 0.5807(5) 0.8759(4) N5B N 1.1747(5) 0.5264(4) 0.7608(4) C1B C 1.2784(8) 0.4436(6) 0.7454(5) H1B H 1.26070 0.46590 0.72110 C2B C 1.2862(8) 0.3993(6) 0.7337(5) H2B H 1.27650 0.38620 0.70030 C3B C 1.3117(7) 0.3765(5) 0.7814(5) H3B H 1.32050 0.34570 0.78660 C4B C 1.3204(6) 0.4113(4) 0.8189(4) C5B C 1.3574(6) 0.4085(5) 0.8756(4) C6B C 1.3260(7) 0.4461(5) 0.9047(4) C7B C 1.3636(7) 0.4776(5) 0.9353(5) H4B H 1.41670 0.48200 0.93960 C8B C 1.3102(7) 0.5028(5) 0.9595(4) H5B H 1.32140 0.52650 0.98330 C9B C 1.2397(6) 0.4870(4) 0.9427(4) C10B C 1.1870(7) 0.4259(5) 0.8819(5) H6B H 1.17600 0.40140 0.90480 H7B H 1.20210 0.41390 0.84940 H8B H 1.14190 0.44430 0.87420 C11B C 1.1620(7) 0.5008(4) 0.9592(4) C12B C 1.1191(7) 0.5278(5) 0.9135(4) C13B C 1.0529(7) 0.5503(5) 0.9133(5) H9B H 1.01480 0.54460 0.93520 C14B C 1.0511(7) 0.5838(5) 0.8742(5) H10B H 1.01170 0.60450 0.86510 C15B C 1.1179(8) 0.5803(5) 0.8525(5) H11B H 1.13200 0.59850 0.82530 C16B C 1.4758(7) 0.4358(5) 0.8365(5) H12B H 1.44360 0.44550 0.80700 C17B C 1.5535(7) 0.4418(5) 0.8385(6) H13B H 1.57440 0.45290 0.80890 C18B C 1.6012(7) 0.4316(5) 0.8839(6) H14B H 1.65330 0.43890 0.88680 C19B C 1.5701(9) 0.4106(6) 0.9246(5) H15B H 1.60150 0.40040 0.95430 C20B C 1.4932(7) 0.4050(5) 0.9209(5) H16B H 1.47190 0.39310 0.94990 C21B C 1.4457(6) 0.4157(5) 0.8774(5) C22B C 1.3761(8) 0.3228(6) 0.8812(5) H17B H 1.40360 0.32440 0.85190 C23B C 1.3667(9) 0.2830(6) 0.9033(6) H18B H 1.38600 0.25760 0.88750 C24B C 1.3312(8) 0.2768(5) 0.9469(6) H19B H 1.32630 0.24830 0.96180 C25B C 1.3036(8) 0.3139(6) 0.9677(6) H20B H 1.27940 0.31080 0.99850 C26B C 1.3088(7) 0.3576(6) 0.9459(5) H21B H 1.28770 0.38250 0.96150 C27B C 1.3462(7) 0.3627(5) 0.9002(5) C28B C 1.1625(7) 0.4303(5) 1.0086(5) H22B H 1.21360 0.43650 1.02070 C29B C 1.1315(8) 0.3918(5) 1.0239(5) H23B H 1.16080 0.37230 1.04690 C30B C 1.0558(9) 0.3804(7) 1.0057(6) H24B H 1.03420 0.35360 1.01630 C31B C 1.0144(8) 0.4093(6) 0.9725(6) H25B H 0.96390 0.40210 0.95970 C32B C 1.0472(8) 0.4503(5) 0.9569(5) H26B H 1.01900 0.47030 0.93410 C33B C 1.1231(6) 0.4600(4) 0.9769(4) C34B C 1.1674(7) 0.5266(5) 1.0562(5) H27B H 1.15180 0.49770 1.06480 C35B C 1.1797(7) 0.5592(6) 1.0955(6) H28B H 1.17380 0.55180 1.13050 C36B C 1.2001(8) 0.6012(6) 1.0833(5) H29B H 1.20820 0.62320 1.10960 C37B C 1.2091(7) 0.6116(5) 1.0321(5) H30B H 1.22390 0.64080 1.02360 C38B C 1.1970(7) 0.5805(5) 0.9937(5) H31B H 1.20160 0.58900 0.95890 C39B C 1.1782(6) 0.5369(5) 1.0035(5) C40B C 1.3785(9) 0.6039(6) 0.9255(5) H32B H 1.42150 0.62400 0.92410 H33B H 1.39040 0.58220 0.95340 H34B H 1.33410 0.62110 0.93230 C41B C 1.4235(8) 0.5635(5) 0.8565(6) H35B H 1.45750 0.54640 0.88260 C42B C 1.4253(7) 0.5492(5) 0.8066(5) H36B H 1.45970 0.52370 0.80210 C43B C 1.3711(7) 0.5604(5) 0.7604(5) H37B H 1.37500 0.53790 0.73240 C44B C 1.2972(6) 0.5718(5) 0.7622(4) C45B C 1.2409(7) 0.5850(5) 0.7160(5) C46B C 1.1824(7) 0.5474(5) 0.7153(5) C47B C 1.1275(7) 0.5338(5) 0.6760(5) H38B H 1.12830 0.53850 0.63770 C48B C 1.0841(7) 0.5017(5) 0.7001(5) H39B H 1.05760 0.47670 0.68020 C49B C 1.1152(7) 0.4972(5) 0.7513(5) H40B H 1.11090 0.46940 0.77180 C50B C 1.2978(7) 0.5492(5) 0.6389(5) H41B H 1.28120 0.52130 0.65040 C51B C 1.3402(7) 0.5500(7) 0.5954(5) H42B H 1.35210 0.52320 0.57890 C52B C 1.3637(8) 0.5900(6) 0.5777(5) H43B H 1.39140 0.59140 0.54850 C53B C 1.3463(8) 0.6281(7) 0.6033(6) H44B H 1.36190 0.65600 0.59090 C54B C 1.3055(8) 0.6271(7) 0.6478(6) H45B H 1.29620 0.65380 0.66550 C55B C 1.2796(7) 0.5870(6) 0.6652(5) C56B C 1.1407(10) 0.6404(5) 0.6886(7) H46B H 1.12840 0.62280 0.65840 C57B C 1.0988(10) 0.6780(6) 0.6967(8) H47B H 1.06050 0.68720 0.67050 C58B C 1.1113(10) 0.7018(8) 0.7408(11) H48B H 1.08040 0.72630 0.74730 C59B C 1.1720(13) 0.6888(7) 0.7770(8) H49B H 1.18360 0.70600 0.80760 C60B C 1.2146(9) 0.6524(6) 0.7695(6) H50B H 1.25390 0.64390 0.79540 C61B C 1.2012(7) 0.6282(5) 0.7252(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Th1 N1 2.492 1_555 1_555 K1 N5 3.384 1_555 1_555 N1 C1 1.384 1_555 1_555 N2 Th1 2.939 1_555 1_555 N3 Th1 2.466 1_555 1_555 N4 Th1 2.379 1_555 1_555 N5 Th1 2.488 1_555 1_555 C1 H1 0.940 1_555 1_555 C2 C1 1.365 1_555 1_555 H2 C2 0.939 1_555 1_555 C3 C2 1.427 1_555 1_555 H3 C3 0.939 1_555 1_555 C4 N1 1.323 1_555 1_555 C5 C4 1.527 1_555 1_555 C6 Th1 3.037 1_555 1_555 C7 Th1 3.172 1_555 1_555 H4 C7 0.942 1_555 1_555 C8 Th1 3.236 1_555 1_555 H5 C8 0.940 1_555 1_555 C9 Th1 3.119 1_555 1_555 C10 N2 1.462 1_555 1_555 H6 C10 0.970 1_555 1_555 H7 C10 0.970 1_555 1_555 H8 C10 0.970 1_555 1_555 C11 C9 1.537 1_555 1_555 C12 N3 1.395 1_555 1_555 C13 C12 1.348 1_555 1_555 H9 C13 0.939 1_555 1_555 C14 K1 3.221 1_555 1_555 H10 C14 0.940 1_555 1_555 C15 K1 3.169 1_555 1_555 H11 C15 0.938 1_555 1_555 C16 H12 0.939 1_555 1_555 C17 C16 1.380 1_555 1_555 H13 C17 0.940 1_555 1_555 C18 C17 1.392 1_555 1_555 H14 C18 0.941 1_555 1_555 C19 C18 1.382 1_555 1_555 H15 C19 0.941 1_555 1_555 C20 C19 1.362 1_555 1_555 H16 C20 0.939 1_555 1_555 C21 C5 1.571 1_555 1_555 C22 H17 0.940 1_555 1_555 C23 C22 1.334 1_555 1_555 H18 C23 0.941 1_555 1_555 C24 C23 1.353 1_555 1_555 H19 C24 0.940 1_555 1_555 C25 C24 1.343 1_555 1_555 H20 C25 0.943 1_555 1_555 C26 C25 1.425 1_555 1_555 H21 C26 0.940 1_555 1_555 C27 C5 1.527 1_555 1_555 C28 H22 0.940 1_555 1_555 C29 C28 1.349 1_555 1_555 H23 C29 0.941 1_555 1_555 C30 C29 1.408 1_555 1_555 H24 C30 0.939 1_555 1_555 C31 C30 1.365 1_555 1_555 H25 C31 0.941 1_555 1_555 C32 C31 1.429 1_555 1_555 H26 C32 0.938 1_555 1_555 C33 C11 1.493 1_555 1_555 C34 H27 0.939 1_555 1_555 C35 C34 1.399 1_555 1_555 H28 C35 0.940 1_555 1_555 C36 C35 1.350 1_555 1_555 H29 C36 0.940 1_555 1_555 C37 C36 1.374 1_555 1_555 H30 C37 0.942 1_555 1_555 C38 C37 1.352 1_555 1_555 H31 C38 0.939 1_555 1_555 C39 C11 1.567 1_555 1_555 C40 N4 1.446 1_555 1_555 H32 C40 0.972 1_555 1_555 H33 C40 0.970 1_555 1_555 H34 C40 0.969 1_555 1_555 C41 Th1 2.809 1_555 1_555 H35 C41 0.989 1_555 1_555 C42 Th1 2.880 1_555 1_555 H36 C42 0.988 1_555 1_555 C43 Th1 2.866 1_555 1_555 H37 C43 0.990 1_555 1_555 C44 Th1 2.380 1_555 1_555 C45 C44 1.511 1_555 1_555 C46 K1 3.530 1_555 1_555 C47 K1 3.328 1_555 1_555 H38 C47 0.992 1_555 1_555 C48 K1 2.991 1_555 1_555 H39 C48 0.991 1_555 1_555 C49 K1 3.068 1_555 1_555 H40 C49 0.989 1_555 1_555 C50 H41 0.941 1_555 1_555 C51 C50 1.410 1_555 1_555 H42 C51 0.939 1_555 1_555 C52 C51 1.358 1_555 1_555 H43 C52 0.939 1_555 1_555 C53 C52 1.364 1_555 1_555 H44 C53 0.943 1_555 1_555 C54 C53 1.415 1_555 1_555 H45 C54 0.940 1_555 1_555 C55 C45 1.537 1_555 1_555 C56 H46 0.940 1_555 1_555 C57 C56 1.372 1_555 1_555 H47 C57 0.939 1_555 1_555 C58 C57 1.331 1_555 1_555 H48 C58 0.938 1_555 1_555 C59 C58 1.392 1_555 1_555 H49 C59 0.940 1_555 1_555 C60 C59 1.347 1_555 1_555 H50 C60 0.940 1_555 1_555 C61 C45 1.498 1_555 1_555 Th1B N1B 2.492 1_555 1_555 N1B C1B 1.384 1_555 1_555 N2B Th1B 2.939 1_555 1_555 N3B Th1B 2.466 1_555 1_555 N4B Th1B 2.379 1_555 1_555 N5B K1 3.384 1_555 1_555 C1B H1B 0.940 1_555 1_555 C2B C1B 1.365 1_555 1_555 H2B C2B 0.939 1_555 1_555 C3B C2B 1.427 1_555 1_555 H3B C3B 0.939 1_555 1_555 C4B N1B 1.323 1_555 1_555 C5B C4B 1.527 1_555 1_555 C6B Th1B 3.037 1_555 1_555 C7B Th1B 3.172 1_555 1_555 H4B C7B 0.942 1_555 1_555 C8B Th1B 3.236 1_555 1_555 H5B C8B 0.940 1_555 1_555 C9B Th1B 3.119 1_555 1_555 C10B N2B 1.462 1_555 1_555 H6B C10B 0.970 1_555 1_555 H7B C10B 0.970 1_555 1_555 H8B C10B 0.970 1_555 1_555 C11B C9B 1.537 1_555 1_555 C12B N3B 1.395 1_555 1_555 C13B C12B 1.348 1_555 1_555 H9B C13B 0.939 1_555 1_555 C14B K1 3.221 1_555 1_555 H10B C14B 0.940 1_555 1_555 C15B K1 3.169 1_555 1_555 H11B C15B 0.938 1_555 1_555 C16B H12B 0.939 1_555 1_555 C17B C16B 1.380 1_555 1_555 H13B C17B 0.940 1_555 1_555 C18B C17B 1.392 1_555 1_555 H14B C18B 0.941 1_555 1_555 C19B C18B 1.382 1_555 1_555 H15B C19B 0.941 1_555 1_555 C20B C19B 1.362 1_555 1_555 H16B C20B 0.939 1_555 1_555 C21B C5B 1.571 1_555 1_555 C22B H17B 0.940 1_555 1_555 C23B C22B 1.334 1_555 1_555 H18B C23B 0.941 1_555 1_555 C24B C23B 1.353 1_555 1_555 H19B C24B 0.940 1_555 1_555 C25B C24B 1.343 1_555 1_555 H20B C25B 0.943 1_555 1_555 C26B C25B 1.425 1_555 1_555 H21B C26B 0.940 1_555 1_555 C27B C5B 1.527 1_555 1_555 C28B H22B 0.940 1_555 1_555 C29B C28B 1.349 1_555 1_555 H23B C29B 0.941 1_555 1_555 C30B C29B 1.408 1_555 1_555 H24B C30B 0.939 1_555 1_555 C31B C30B 1.365 1_555 1_555 H25B C31B 0.941 1_555 1_555 C32B C31B 1.429 1_555 1_555 H26B C32B 0.938 1_555 1_555 C33B C11B 1.493 1_555 1_555 C34B H27B 0.939 1_555 1_555 C35B C34B 1.399 1_555 1_555 H28B C35B 0.940 1_555 1_555 C36B C35B 1.350 1_555 1_555 H29B C36B 0.940 1_555 1_555 C37B C36B 1.374 1_555 1_555 H30B C37B 0.942 1_555 1_555 C38B C37B 1.352 1_555 1_555 H31B C38B 0.939 1_555 1_555 C39B C11B 1.567 1_555 1_555 C40B N4B 1.446 1_555 1_555 H32B C40B 0.972 1_555 1_555 H33B C40B 0.970 1_555 1_555 H34B C40B 0.969 1_555 1_555 C41B Th1B 2.809 1_555 1_555 H35B C41B 0.989 1_555 1_555 C42B Th1B 2.880 1_555 1_555 H36B C42B 0.988 1_555 1_555 C43B Th1B 2.866 1_555 1_555 H37B C43B 0.990 1_555 1_555 C44B Th1B 2.380 1_555 1_555 C45B C44B 1.511 1_555 1_555 C46B K1 3.530 1_555 1_555 C47B K1 3.328 1_555 1_555 H38B C47B 0.992 1_555 1_555 C48B K1 2.991 1_555 1_555 H39B C48B 0.991 1_555 1_555 C49B K1 3.068 1_555 1_555 H40B C49B 0.989 1_555 1_555 C50B H41B 0.941 1_555 1_555 C51B C50B 1.410 1_555 1_555 H42B C51B 0.939 1_555 1_555 C52B C51B 1.358 1_555 1_555 H43B C52B 0.939 1_555 1_555 C53B C52B 1.364 1_555 1_555 H44B C53B 0.943 1_555 1_555 C54B C53B 1.415 1_555 1_555 H45B C54B 0.940 1_555 1_555 C55B C45B 1.537 1_555 1_555 C56B H46B 0.940 1_555 1_555 C57B C56B 1.372 1_555 1_555 H47B C57B 0.939 1_555 1_555 C58B C57B 1.331 1_555 1_555 H48B C58B 0.938 1_555 1_555 C59B C58B 1.392 1_555 1_555 H49B C59B 0.940 1_555 1_555 C60B C59B 1.347 1_555 1_555 H50B C60B 0.940 1_555 1_555 C61B C45B 1.498 1_555 1_555 N2 C6 1.390 1_555 1_555 N2 C9 1.368 1_555 1_555 N3 C15 1.377 1_555 1_555 N4 C41 1.329 1_555 1_555 N5 C46 1.343 1_555 1_555 N5 C49 1.366 1_555 1_555 C3 C4 1.411 1_555 1_555 C5 C6 1.488 1_555 1_555 C6 C7 1.350 1_555 1_555 C7 C8 1.404 1_555 1_555 C8 C9 1.356 1_555 1_555 C11 C12 1.548 1_555 1_555 C13 C14 1.413 1_555 1_555 C14 C15 1.364 1_555 1_555 C16 C21 1.365 1_555 1_555 C20 C21 1.356 1_555 1_555 C22 C27 1.411 1_555 1_555 C26 C27 1.415 1_555 1_555 C28 C33 1.343 1_555 1_555 C32 C33 1.411 1_555 1_555 C34 C39 1.418 1_555 1_555 C38 C39 1.372 1_555 1_555 C41 C42 1.351 1_555 1_555 C42 C43 1.475 1_555 1_555 C43 C44 1.355 1_555 1_555 C45 C46 1.524 1_555 1_555 C46 C47 1.379 1_555 1_555 C47 C48 1.411 1_555 1_555 C48 C49 1.371 1_555 1_555 C50 C55 1.370 1_555 1_555 C54 C55 1.373 1_555 1_555 C56 C61 1.389 1_555 1_555 C60 C61 1.343 1_555 1_555 Th1B N5B 2.488 1_555 1_555 N2B C6B 1.390 1_555 1_555 N2B C9B 1.368 1_555 1_555 N3B C15B 1.377 1_555 1_555 N4B C41B 1.329 1_555 1_555 N5B C46B 1.343 1_555 1_555 N5B C49B 1.366 1_555 1_555 C3B C4B 1.411 1_555 1_555 C5B C6B 1.488 1_555 1_555 C6B C7B 1.350 1_555 1_555 C7B C8B 1.404 1_555 1_555 C8B C9B 1.356 1_555 1_555 C11B C12B 1.548 1_555 1_555 C13B C14B 1.413 1_555 1_555 C14B C15B 1.364 1_555 1_555 C16B C21B 1.365 1_555 1_555 C20B C21B 1.356 1_555 1_555 C22B C27B 1.411 1_555 1_555 C26B C27B 1.415 1_555 1_555 C28B C33B 1.343 1_555 1_555 C32B C33B 1.411 1_555 1_555 C34B C39B 1.418 1_555 1_555 C38B C39B 1.372 1_555 1_555 C41B C42B 1.351 1_555 1_555 C42B C43B 1.475 1_555 1_555 C43B C44B 1.355 1_555 1_555 C45B C46B 1.524 1_555 1_555 C46B C47B 1.379 1_555 1_555 C47B C48B 1.411 1_555 1_555 C48B C49B 1.371 1_555 1_555 C50B C55B 1.370 1_555 1_555 C54B C55B 1.373 1_555 1_555 C56B C61B 1.389 1_555 1_555 C60B C61B 1.343 1_555 1_555 #END data_CSD_CIF_WUSXOX _audit_creation_date 2003-05-15 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD WUSXOX _database_code_depnum_ccdc_archive 'CCDC 181615' _chemical_formula_sum 'C72 H106 Li2 N2 O5 P2 Si4' _chemical_formula_moiety ; C52 H66 Li1 N2 P2 Si4 1-,C16 H32 Li1 O4 1+,C4 H8 O1 ; _journal_coden_Cambridge 179 _journal_volume 42 _journal_year 2003 _journal_page_first 435 _journal_name_full 'Angew.Chem.,Int.Ed. ' loop_ _publ_author_name "S.Ekici" "M.Nieger" "R.Glaum" "E.Niecke" _chemical_name_systematic ; tetrakis(tetrahydrofuran)-lithium (2,11-di(bis(trimethylsilyl)methylene)-2,11-diphospha-1,3,10,12-tetraphenyl(3. 3)(2,6)pyridinophane-N,N',P,P')-lithium tetrahydrofuran solvate ; _cell_volume 7320.142 _exptl_crystal_colour 'red' _exptl_crystal_density_diffrn 1.15 _exptl_crystal_description 'blocks' _diffrn_ambient_temperature 123 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_gt 0.0766 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 -x,1/2+y,1/2-z 4 1/2+x,1/2-y,-z _cell_length_a 16.8587(2) _cell_length_b 20.3906(3) _cell_length_c 21.2944(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.08 N 0.68 O 0.68 P 1.05 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.5720(4) 0.6282(3) 0.4973(3) N1 N 0.6730(2) 0.56830(16) 0.49392(18) C1 C 0.7108(3) 0.5648(2) 0.4379(2) C2 C 0.7921(3) 0.5588(2) 0.4332(3) H1 H 0.81690 0.55670 0.39330 C3 C 0.8368(3) 0.5560(2) 0.4875(3) H2 H 0.89290 0.55220 0.48540 C4 C 0.7994(3) 0.5587(2) 0.5441(3) H3 H 0.82970 0.55600 0.58160 C5 C 0.7170(3) 0.5655(2) 0.5477(2) C6 C 0.6733(3) 0.5669(2) 0.6098(2) H4 H 0.71180 0.57880 0.64370 C7 C 0.6383(3) 0.5002(2) 0.6245(2) C8 C 0.5918(4) 0.4673(3) 0.5829(3) H5 H 0.58130 0.48570 0.54280 C9 C 0.5595(4) 0.4066(3) 0.5991(3) H6 H 0.52630 0.38480 0.56970 C10 C 0.5741(4) 0.3774(3) 0.6556(4) H7 H 0.55270 0.33560 0.66530 C11 C 0.6212(4) 0.4110(3) 0.6985(4) H8 H 0.63060 0.39290 0.73900 C12 C 0.6545(3) 0.4708(3) 0.6822(3) H9 H 0.68900 0.49210 0.71100 P1 P 0.58687(7) 0.62863(5) 0.61155(5) C13 C 0.5356(3) 0.6217(2) 0.6823(2) Si1 Si 0.57716(11) 0.63588(7) 0.75989(6) C14 C 0.5606(7) 0.5645(4) 0.8163(3) H10 H 0.58470 0.57480 0.85700 H11 H 0.58500 0.52480 0.79910 H12 H 0.50350 0.55740 0.82190 C15 C 0.6853(4) 0.6535(3) 0.7639(3) H13 H 0.70100 0.65950 0.80790 H14 H 0.69700 0.69350 0.74020 H15 H 0.71490 0.61670 0.74590 C16 C 0.5280(5) 0.7091(4) 0.7988(3) H16 H 0.55100 0.71590 0.84060 H17 H 0.47090 0.70100 0.80280 H18 H 0.53670 0.74840 0.77310 Si2 Si 0.43255(10) 0.60164(9) 0.67223(8) C17 C 0.4017(4) 0.5877(4) 0.5890(4) H19 H 0.34530 0.57640 0.58760 H20 H 0.43290 0.55160 0.57110 H21 H 0.41090 0.62770 0.56450 C18 C 0.3633(5) 0.6684(5) 0.7008(4) H22 H 0.30820 0.65460 0.69440 H23 H 0.37330 0.70880 0.67720 H24 H 0.37250 0.67630 0.74560 C19 C 0.4019(5) 0.5253(5) 0.7146(5) H25 H 0.34550 0.51690 0.70700 H26 H 0.41100 0.53080 0.75970 H27 H 0.43320 0.48810 0.69920 C20 C 0.6465(3) 0.7079(2) 0.6122(2) H28 H 0.68690 0.70450 0.64640 C21 C 0.5934(3) 0.7664(2) 0.6269(2) C22 C 0.5200(3) 0.7746(2) 0.5975(2) H29 H 0.50150 0.74230 0.56890 C23 C 0.4750(3) 0.8281(3) 0.6094(3) H30 H 0.42480 0.83230 0.58960 C24 C 0.5005(4) 0.8766(3) 0.6497(3) H31 H 0.46850 0.91410 0.65740 C25 C 0.5743(5) 0.8699(3) 0.6790(3) H32 H 0.59390 0.90290 0.70640 C26 C 0.6184(4) 0.8134(2) 0.6671(2) H33 H 0.66770 0.80770 0.68790 C27 C 0.6906(3) 0.7190(2) 0.5504(2) C28 C 0.7692(3) 0.7401(2) 0.5508(2) H34 H 0.79620 0.74700 0.58930 C29 C 0.8073(3) 0.7510(2) 0.4942(3) H35 H 0.86100 0.76500 0.49310 C30 C 0.7651(3) 0.7409(2) 0.4391(2) H36 H 0.78990 0.74820 0.39970 C31 C 0.6875(3) 0.7204(2) 0.4415(2) N2 N 0.6507(2) 0.70917(15) 0.49723(17) C32 C 0.6405(3) 0.7096(2) 0.3818(2) H37 H 0.67850 0.70820 0.34580 C33 C 0.5833(3) 0.7657(2) 0.3711(2) C34 C 0.5233(3) 0.7809(2) 0.4135(2) H38 H 0.51930 0.75640 0.45130 C35 C 0.4689(3) 0.8311(2) 0.4020(2) H39 H 0.42820 0.84020 0.43160 C36 C 0.4745(3) 0.8672(3) 0.3481(3) H40 H 0.43800 0.90160 0.34020 C37 C 0.5330(4) 0.8535(3) 0.3052(3) H41 H 0.53670 0.87890 0.26790 C38 C 0.5865(4) 0.8035(2) 0.3155(2) H42 H 0.62600 0.79440 0.28490 P2 P 0.57821(7) 0.63123(5) 0.38003(5) C39 C 0.5307(3) 0.6266(2) 0.3078(2) Si3 Si 0.57931(9) 0.62739(6) 0.23173(6) C40 C 0.6852(3) 0.6553(3) 0.2299(2) H43 H 0.70490 0.65410 0.18660 H44 H 0.71750 0.62630 0.25620 H45 H 0.68870 0.70030 0.24600 C41 C 0.5289(4) 0.6833(3) 0.1730(3) H46 H 0.55770 0.68190 0.13310 H47 H 0.52870 0.72830 0.18920 H48 H 0.47420 0.66860 0.16640 C42 C 0.5830(4) 0.5441(3) 0.1918(3) H49 H 0.60960 0.54820 0.15110 H50 H 0.52890 0.52790 0.18550 H51 H 0.61230 0.51320 0.21840 Si4 Si 0.42313(9) 0.62631(7) 0.31057(6) C43 C 0.3793(4) 0.5599(3) 0.2574(3) H52 H 0.32120 0.56120 0.25990 H53 H 0.39820 0.51670 0.27110 H54 H 0.39590 0.56760 0.21400 C44 C 0.3808(4) 0.6103(3) 0.3918(3) H55 H 0.32270 0.61100 0.38980 H56 H 0.39920 0.64430 0.42080 H57 H 0.39860 0.56730 0.40670 C45 C 0.3740(3) 0.7056(3) 0.2847(3) H58 H 0.31630 0.70100 0.28770 H59 H 0.38880 0.71510 0.24110 H60 H 0.39160 0.74150 0.31190 C46 C 0.6579(3) 0.5652(2) 0.3801(2) H61 H 0.69250 0.57270 0.34260 C47 C 0.6202(3) 0.4981(2) 0.3732(2) C48 C 0.6487(4) 0.4526(3) 0.3312(3) H62 H 0.69230 0.46320 0.30490 C49 C 0.6128(5) 0.3898(3) 0.3273(3) H63 H 0.63290 0.35840 0.29850 C50 C 0.5492(4) 0.3740(3) 0.3648(3) H64 H 0.52640 0.33150 0.36190 C51 C 0.5184(4) 0.4184(3) 0.4062(3) H65 H 0.47380 0.40750 0.43140 C52 C 0.5540(3) 0.4801(3) 0.4106(3) H66 H 0.53320 0.51110 0.43960 Li2 Li 0.2336(11) 0.3135(8) 0.4893(9) O1 O 0.2685(3) 0.22246(19) 0.4985(2) C53 C 0.2657(6) 0.1797(3) 0.5500(3) H67 H 0.22340 0.19320 0.57950 H68 H 0.31700 0.18000 0.57260 C54 C 0.2491(6) 0.1134(3) 0.5246(3) H69 H 0.19150 0.10380 0.52490 H70 H 0.27730 0.07910 0.54870 C55 C 0.2799(5) 0.1180(3) 0.4592(3) H71 H 0.33700 0.10660 0.45760 H72 H 0.25030 0.08840 0.43080 C56 C 0.2675(5) 0.1859(3) 0.4423(3) H73 H 0.31010 0.20100 0.41370 H74 H 0.21590 0.19110 0.42070 O2 O 0.2806(5) 0.3634(3) 0.4235(2) C57 C 0.2969(7) 0.3434(3) 0.3606(3) H75 H 0.25440 0.31440 0.34480 H76 H 0.34800 0.31950 0.35850 C58 C 0.3008(6) 0.4037(3) 0.3234(3) H77 H 0.27790 0.39700 0.28100 H78 H 0.35610 0.41920 0.31910 C59 C 0.2529(6) 0.4504(4) 0.3601(3) H79 H 0.27180 0.49600 0.35410 H80 H 0.19610 0.44780 0.34840 C60 C 0.2655(6) 0.4286(3) 0.4246(3) H81 H 0.31070 0.45240 0.44340 H82 H 0.21760 0.43750 0.45010 O3 O 0.2580(3) 0.3679(4) 0.5648(2) C61 C 0.2222(4) 0.3490(6) 0.6204(4) H83 H 0.19780 0.30510 0.61580 H84 H 0.18030 0.38060 0.63220 C62 C 0.2842(5) 0.3475(8) 0.6680(4) H85 H 0.27660 0.38370 0.69840 H86 H 0.28280 0.30540 0.69110 C63 C 0.3593(5) 0.3548(8) 0.6358(5) H87 H 0.38510 0.31170 0.62950 H88 H 0.39560 0.38360 0.65980 C64 C 0.3380(5) 0.3847(7) 0.5755(4) H89 H 0.34430 0.43290 0.57740 H90 H 0.37220 0.36740 0.54150 O4 O 0.1213(4) 0.3042(4) 0.4805(4) C65 C 0.0728(5) 0.2580(5) 0.5113(6) H91 H 0.07820 0.26240 0.55740 H92 H 0.08820 0.21290 0.49910 C66 C -0.0098(5) 0.2716(4) 0.4917(5) H93 H -0.04820 0.25930 0.52490 H94 H -0.02350 0.24840 0.45240 C67 C -0.0067(6) 0.3441(5) 0.4824(6) H95 H -0.04640 0.35860 0.45110 H96 H -0.01600 0.36770 0.52240 C68 C 0.0739(5) 0.3547(4) 0.4596(7) H97 H 0.07420 0.35610 0.41320 H98 H 0.09440 0.39710 0.47550 O5 O 0.0785(7) 0.5282(8) 0.4884(6) C69 C 0.1282(9) 0.4907(5) 0.5261(6) H99 H 0.17120 0.47050 0.50100 H100 H 0.09830 0.45570 0.54790 C70 C 0.1602(9) 0.5391(6) 0.5713(5) H101 H 0.20720 0.52210 0.59410 H102 H 0.11960 0.55380 0.60180 C71 C 0.1815(9) 0.5913(6) 0.5259(6) H103 H 0.17390 0.63520 0.54490 H104 H 0.23750 0.58690 0.51260 C72 C 0.1283(11) 0.5821(8) 0.4729(6) H105 H 0.09630 0.62210 0.46570 H106 H 0.15900 0.57250 0.43430 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 N1 2.097 1_555 1_555 N1 C1 1.354 1_555 1_555 C1 C2 1.380 1_555 1_555 C2 H1 0.948 1_555 1_555 C3 C2 1.381 1_555 1_555 H2 C3 0.950 1_555 1_555 C4 C3 1.361 1_555 1_555 H3 C4 0.950 1_555 1_555 C5 N1 1.366 1_555 1_555 C6 C5 1.514 1_555 1_555 H4 C6 1.001 1_555 1_555 C7 C6 1.515 1_555 1_555 C8 C7 1.360 1_555 1_555 H5 C8 0.949 1_555 1_555 C9 C8 1.396 1_555 1_555 H6 C9 0.950 1_555 1_555 C10 C9 1.365 1_555 1_555 H7 C10 0.948 1_555 1_555 C11 C10 1.391 1_555 1_555 H8 C11 0.951 1_555 1_555 C12 C7 1.394 1_555 1_555 H9 C12 0.950 1_555 1_555 P1 Li1 2.446 1_555 1_555 C13 P1 1.743 1_555 1_555 Si1 C13 1.818 1_555 1_555 C14 Si1 1.908 1_555 1_555 H10 C14 0.980 1_555 1_555 H11 C14 0.979 1_555 1_555 H12 C14 0.981 1_555 1_555 C15 Si1 1.860 1_555 1_555 H13 C15 0.981 1_555 1_555 H14 C15 0.979 1_555 1_555 H15 C15 0.979 1_555 1_555 C16 Si1 1.898 1_555 1_555 H16 C16 0.981 1_555 1_555 H17 C16 0.980 1_555 1_555 H18 C16 0.981 1_555 1_555 Si2 C13 1.798 1_555 1_555 C17 Si2 1.869 1_555 1_555 H19 C17 0.979 1_555 1_555 H20 C17 0.982 1_555 1_555 H21 C17 0.981 1_555 1_555 C18 Si2 1.894 1_555 1_555 H22 C18 0.980 1_555 1_555 H23 C18 0.980 1_555 1_555 H24 C18 0.980 1_555 1_555 C19 Si2 1.872 1_555 1_555 H25 C19 0.980 1_555 1_555 H26 C19 0.979 1_555 1_555 H27 C19 0.980 1_555 1_555 C20 P1 1.904 1_555 1_555 H28 C20 1.000 1_555 1_555 C21 C20 1.524 1_555 1_555 C22 C21 1.397 1_555 1_555 H29 C22 0.950 1_555 1_555 C23 C22 1.353 1_555 1_555 H30 C23 0.949 1_555 1_555 C24 C23 1.378 1_555 1_555 H31 C24 0.950 1_555 1_555 C25 C24 1.399 1_555 1_555 H32 C25 0.950 1_555 1_555 C26 C21 1.352 1_555 1_555 H33 C26 0.949 1_555 1_555 C27 C20 1.528 1_555 1_555 C28 C27 1.393 1_555 1_555 H34 C28 0.948 1_555 1_555 C29 C28 1.384 1_555 1_555 H35 C29 0.950 1_555 1_555 C30 C29 1.388 1_555 1_555 H36 C30 0.949 1_555 1_555 C31 C30 1.374 1_555 1_555 N2 Li1 2.118 1_555 1_555 C32 C31 1.514 1_555 1_555 H37 C32 0.999 1_555 1_555 C33 C32 1.513 1_555 1_555 C34 C33 1.391 1_555 1_555 H38 C34 0.950 1_555 1_555 C35 C34 1.396 1_555 1_555 H39 C35 0.950 1_555 1_555 C36 C35 1.367 1_555 1_555 H40 C36 0.948 1_555 1_555 C37 C36 1.373 1_555 1_555 H41 C37 0.950 1_555 1_555 C38 C33 1.414 1_555 1_555 H42 C38 0.950 1_555 1_555 P2 Li1 2.500 1_555 1_555 C39 P2 1.737 1_555 1_555 Si3 C39 1.815 1_555 1_555 C40 Si3 1.874 1_555 1_555 H43 C40 0.980 1_555 1_555 H44 C40 0.980 1_555 1_555 H45 C40 0.981 1_555 1_555 C41 Si3 1.894 1_555 1_555 H46 C41 0.979 1_555 1_555 H47 C41 0.980 1_555 1_555 H48 C41 0.980 1_555 1_555 C42 Si3 1.900 1_555 1_555 H49 C42 0.979 1_555 1_555 H50 C42 0.979 1_555 1_555 H51 C42 0.981 1_555 1_555 Si4 C39 1.814 1_555 1_555 C43 Si4 1.914 1_555 1_555 H52 C43 0.981 1_555 1_555 H53 C43 0.981 1_555 1_555 H54 C43 0.978 1_555 1_555 C44 Si4 1.899 1_555 1_555 H55 C44 0.981 1_555 1_555 H56 C44 0.979 1_555 1_555 H57 C44 0.980 1_555 1_555 C45 Si4 1.898 1_555 1_555 H58 C45 0.979 1_555 1_555 H59 C45 0.981 1_555 1_555 H60 C45 0.979 1_555 1_555 C46 C1 1.520 1_555 1_555 H61 C46 1.001 1_555 1_555 C47 C46 1.516 1_555 1_555 C48 C47 1.375 1_555 1_555 H62 C48 0.949 1_555 1_555 C49 C48 1.419 1_555 1_555 H63 C49 0.949 1_555 1_555 C50 C49 1.375 1_555 1_555 H64 C50 0.950 1_555 1_555 C51 C50 1.366 1_555 1_555 H65 C51 0.950 1_555 1_555 C52 C47 1.419 1_555 1_555 H66 C52 0.951 1_555 1_555 Li2 O1 1.957 1_555 1_555 O1 C53 1.402 1_555 1_555 C53 H67 0.989 1_555 1_555 H68 C53 0.990 1_555 1_555 C54 C53 1.483 1_555 1_555 H69 C54 0.991 1_555 1_555 H70 C54 0.989 1_555 1_555 C55 C54 1.489 1_555 1_555 H71 C55 0.991 1_555 1_555 H72 C55 0.989 1_555 1_555 C56 O1 1.410 1_555 1_555 H73 C56 0.991 1_555 1_555 H74 C56 0.990 1_555 1_555 O2 Li2 1.904 1_555 1_555 C57 O2 1.427 1_555 1_555 H75 C57 0.988 1_555 1_555 H76 C57 0.991 1_555 1_555 C58 C57 1.464 1_555 1_555 H77 C58 0.991 1_555 1_555 H78 C58 0.989 1_555 1_555 C59 C58 1.473 1_555 1_555 H79 C59 0.991 1_555 1_555 H80 C59 0.991 1_555 1_555 C60 O2 1.354 1_555 1_555 H81 C60 0.988 1_555 1_555 H82 C60 0.990 1_555 1_555 O3 Li2 1.996 1_555 1_555 C61 O3 1.384 1_555 1_555 H83 C61 0.990 1_555 1_555 H84 C61 0.989 1_555 1_555 C62 C61 1.456 1_555 1_555 H85 C62 0.990 1_555 1_555 H86 C62 0.990 1_555 1_555 C63 C62 1.448 1_555 1_555 H87 C63 0.990 1_555 1_555 H88 C63 0.990 1_555 1_555 C64 O3 1.410 1_555 1_555 H89 C64 0.989 1_555 1_555 H90 C64 0.990 1_555 1_555 O4 Li2 1.912 1_555 1_555 C65 O4 1.409 1_555 1_555 H91 C65 0.990 1_555 1_555 H92 C65 0.990 1_555 1_555 C66 C65 1.480 1_555 1_555 H93 C66 0.991 1_555 1_555 H94 C66 0.989 1_555 1_555 C67 C66 1.492 1_555 1_555 H95 C67 0.990 1_555 1_555 H96 C67 0.991 1_555 1_555 C68 O4 1.377 1_555 1_555 H97 C68 0.988 1_555 1_555 H98 C68 0.991 1_555 1_555 O5 C69 1.390 1_555 1_555 C69 H99 0.990 1_555 1_555 H100 C69 0.989 1_555 1_555 C70 C69 1.480 1_555 1_555 H101 C70 0.992 1_555 1_555 H102 C70 0.990 1_555 1_555 C71 C70 1.482 1_555 1_555 H103 C71 0.991 1_555 1_555 H104 C71 0.990 1_555 1_555 C72 O5 1.422 1_555 1_555 H105 C72 0.990 1_555 1_555 H106 C72 0.991 1_555 1_555 C4 C5 1.398 1_555 1_555 C6 P1 1.926 1_555 1_555 C11 C12 1.387 1_555 1_555 C25 C26 1.394 1_555 1_555 C27 N2 1.332 1_555 1_555 C31 N2 1.359 1_555 1_555 C32 P2 1.913 1_555 1_555 C37 C38 1.379 1_555 1_555 P2 C46 1.902 1_555 1_555 C51 C52 1.397 1_555 1_555 C55 C56 1.446 1_555 1_555 C59 C60 1.459 1_555 1_555 C63 C64 1.466 1_555 1_555 C67 C68 1.459 1_555 1_555 C71 C72 1.454 1_555 1_555 #END data_CSD_CIF_WUSXUD _audit_creation_date 2003-05-15 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD WUSXUD _database_code_depnum_ccdc_archive 'CCDC 181616' _chemical_formula_sum 'C55 H115 Cl1 Fe1 Li3 N7 P2 Si6' _chemical_formula_moiety ; C37 H67 Fe1 Li1 N1 P2 Si6 1-,C12 H32 Li1 N4 1+,0.5(C12 H32 Cl2 Li2 N4) ; _journal_coden_Cambridge 179 _journal_volume 42 _journal_year 2003 _journal_page_first 435 _journal_name_full 'Angew.Chem.,Int.Ed. ' loop_ _publ_author_name "S.Ekici" "M.Nieger" "R.Glaum" "E.Niecke" _chemical_name_systematic ; bis(N,N,N',N'-tetramethylethylenediamine)-lithium (1,10-bis(bis(trimethylsilyl)methylene)-1,9-bis(trimethylsilyl)-1,10-diphospha (2)(2,6)pyridino(2)(1,1')-ferrocenophane-N,P,P')-lithium bis((\m~2~-chloro)-(tetramethylethane-1,2-diamine)-lithium) ; _cell_volume 3647.287 _exptl_crystal_colour 'red' _exptl_crystal_density_diffrn 1.108 _exptl_crystal_description 'blocks' _diffrn_ambient_temperature 123 _refine_special_details ; The anion is disordered with atoms refined equally over two positions. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_gt 0.0406 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 13.6549(1) _cell_length_b 14.6901(2) _cell_length_c 19.2675(2) _cell_angle_alpha 102.043(1) _cell_angle_beta 92.848(1) _cell_angle_gamma 103.988(1) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Cl 0.99 Fe 1.34 Li 1.08 N 0.68 P 1.05 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Li1 Li 0.4823(3) 0.3253(3) 0.2123(2) Fe1 Fe 0.71008(2) 0.49034(2) 0.354492(17) P1 P 0.44654(4) 0.45783(4) 0.29017(3) P2 P 0.63841(4) 0.28104(4) 0.20363(3) Si1 Si 0.23978(5) 0.32205(5) 0.31241(4) Si2 Si 0.37509(5) 0.64528(5) 0.34531(4) Si3 Si 0.36689(5) 0.55023(5) 0.18291(4) Si4 Si 0.67817(5) 0.29490(5) 0.05682(4) Si5 Si 0.83987(5) 0.23658(5) 0.14938(4) Si6 Si 0.50392(5) 0.06393(5) 0.17605(4) N1 N 0.47465(14) 0.26574(13) 0.29908(10) C1 C 0.52863(17) 0.20083(16) 0.30477(13) C2 C 0.53218(18) 0.16498(17) 0.36586(13) H1 H 0.56630 0.11620 0.36790 C3 C 0.48553(19) 0.20110(18) 0.42362(14) H2 H 0.48690 0.17700 0.46560 C4 C 0.43686(18) 0.27254(17) 0.41980(13) H3 H 0.40720 0.29990 0.45990 C5 C 0.43185(17) 0.30386(16) 0.35662(12) C6 C 0.37830(17) 0.38015(17) 0.34880(13) H4 H 0.38010 0.42210 0.39720 C7 C 0.2256(2) 0.2785(2) 0.21306(14) H5 H 0.26960 0.23540 0.19970 H6 H 0.24500 0.33370 0.19100 H7 H 0.15480 0.24370 0.19650 C8 C 0.1971(2) 0.2156(2) 0.35295(16) H8 H 0.24060 0.17160 0.34070 H9 H 0.12660 0.18200 0.33440 H10 H 0.20190 0.23750 0.40490 C9 C 0.1556(2) 0.4040(2) 0.33680(18) H11 H 0.16250 0.42720 0.38880 H12 H 0.08490 0.36890 0.32000 H13 H 0.17510 0.45900 0.31450 C10 C 0.38611(18) 0.54481(17) 0.27591(13) C11 C 0.3546(2) 0.6156(2) 0.43465(14) H14 H 0.34940 0.67320 0.46910 H15 H 0.41190 0.59350 0.45120 H16 H 0.29170 0.56460 0.43030 C12 C 0.2664(2) 0.6945(2) 0.31959(16) H17 H 0.26200 0.74860 0.35780 H18 H 0.20280 0.64370 0.31220 H19 H 0.27790 0.71670 0.27540 C13 C 0.4883(2) 0.75402(19) 0.36521(15) H20 H 0.47520 0.80410 0.40320 H21 H 0.49980 0.77890 0.32210 H22 H 0.54860 0.73540 0.38070 C14 C 0.2300(2) 0.5278(2) 0.14706(15) H23 H 0.22630 0.53200 0.09690 H24 H 0.20040 0.57630 0.17490 H25 H 0.19220 0.46350 0.15070 C15 C 0.4189(2) 0.4623(2) 0.11920(14) H26 H 0.40590 0.46930 0.07040 H27 H 0.38580 0.39640 0.12240 H28 H 0.49220 0.47530 0.13160 C16 C 0.4316(3) 0.6707(2) 0.16585(17) H29 H 0.41870 0.66960 0.11510 H30 H 0.50480 0.68460 0.17900 H31 H 0.40490 0.72080 0.19450 C17 C 0.56493(17) 0.51812(16) 0.34866(12) C18 C 0.59892(18) 0.51472(18) 0.41931(12) H32 H 0.56480 0.47180 0.44630 C19 C 0.69223(19) 0.58611(18) 0.44258(13) H33 H 0.73030 0.59970 0.48780 C20 C 0.71856(19) 0.63339(17) 0.38665(15) H34 H 0.77700 0.68440 0.38770 C21 C 0.64149(18) 0.59059(17) 0.32874(14) H35 H 0.64090 0.60750 0.28380 C22 C 0.73578(18) 0.35815(17) 0.35564(13) H36 H 0.69600 0.31150 0.37740 C23 C 0.81993(18) 0.43417(18) 0.39031(14) H37 H 0.84690 0.44640 0.43870 C24 C 0.85703(18) 0.48898(19) 0.34010(14) H38 H 0.91330 0.54400 0.34870 C25 C 0.79461(18) 0.44634(17) 0.27464(14) H39 H 0.80110 0.46960 0.23220 C26 C 0.72039(17) 0.36291(16) 0.28262(12) C27 C 0.71556(18) 0.25813(17) 0.13645(12) C28 C 0.5381(2) 0.2557(2) 0.02695(15) H40 H 0.52490 0.27850 -0.01600 H41 H 0.50130 0.28290 0.06500 H42 H 0.51510 0.18520 0.01640 C29 C 0.7136(2) 0.4297(2) 0.06548(18) H43 H 0.69110 0.44400 0.02080 H44 H 0.78740 0.45480 0.07560 H45 H 0.68060 0.46020 0.10450 C30 C 0.7389(3) 0.2445(3) -0.02340(15) H46 H 0.71660 0.26610 -0.06490 H47 H 0.71860 0.17390 -0.03340 H48 H 0.81290 0.26720 -0.01350 C31 C 0.8561(2) 0.1248(2) 0.08621(15) H49 H 0.92460 0.11760 0.09610 H50 H 0.84630 0.13100 0.03680 H51 H 0.80590 0.06810 0.09300 C32 C 0.8731(2) 0.2187(2) 0.24038(14) H52 H 0.94090 0.20760 0.24310 H53 H 0.82340 0.16290 0.24910 H54 H 0.87220 0.27630 0.27650 C33 C 0.9478(2) 0.3375(2) 0.13626(19) H55 H 1.01230 0.32130 0.14400 H56 H 0.94780 0.39720 0.17040 H57 H 0.93900 0.34650 0.08750 C34 C 0.58720(18) 0.17251(16) 0.24292(13) H58 H 0.64650 0.15290 0.26190 C35 C 0.5740(2) 0.0176(2) 0.10232(16) H59 H 0.63380 0.00200 0.12220 H60 H 0.59560 0.06680 0.07490 H61 H 0.52970 -0.04060 0.07090 C36 C 0.3895(2) 0.0941(2) 0.13954(18) H62 H 0.35320 0.11850 0.17900 H63 H 0.34470 0.03620 0.10820 H64 H 0.41060 0.14360 0.11220 C37 C 0.4580(3) -0.0343(2) 0.22439(19) H65 H 0.42070 -0.01100 0.26360 H66 H 0.51630 -0.05270 0.24360 H67 H 0.41310 -0.09030 0.19120 Cl1 Cl 0.02821(7) 0.05138(7) 0.59698(4) Li2 Li 0.0740(4) -0.0520(4) 0.5032(3) C38 C -0.0134(3) -0.2650(3) 0.4777(2) H68 H -0.07430 -0.25520 0.49980 H69 H -0.00460 -0.32840 0.48050 H70 H -0.02080 -0.26150 0.42750 C39 C 0.0819(3) -0.1932(3) 0.59052(17) H71 H 0.01880 -0.18490 0.60980 H72 H 0.13920 -0.14160 0.61720 H73 H 0.09170 -0.25570 0.59500 N2 N 0.07615(17) -0.18934(17) 0.51562(12) C40 C 0.1674(3) -0.2012(2) 0.4846(2) H74 H 0.15340 -0.21700 0.43190 H75 H 0.18650 -0.25640 0.49840 C41 C 0.2525(2) -0.1166(2) 0.50618(19) H76 H 0.31110 -0.12890 0.48110 H77 H 0.27200 -0.10550 0.55800 N3 N 0.22999(19) -0.02792(18) 0.49082(13) C42 C 0.2468(3) -0.0256(3) 0.41610(18) H78 H 0.20300 -0.08360 0.38420 H79 H 0.31800 -0.02320 0.40940 H80 H 0.23070 0.03160 0.40500 C43 C 0.2954(4) 0.0585(3) 0.5372(2) H81 H 0.28490 0.05770 0.58710 H82 H 0.27910 0.11540 0.52570 H83 H 0.36650 0.06060 0.53020 Li3 Li 0.0885(3) 0.1818(3) 0.8471(2) C44 C -0.0839(3) 0.0551(4) 0.8961(2) H84 H -0.08350 0.11580 0.92900 H85 H -0.03890 0.02320 0.91740 H86 H -0.15300 0.01300 0.88670 C45 C -0.0500(3) -0.0168(2) 0.7821(2) H87 H -0.02630 -0.00500 0.73680 H88 H -0.11930 -0.05850 0.77330 H89 H -0.00520 -0.04840 0.80400 N4 N -0.04873(16) 0.07445(15) 0.82987(12) C46 C -0.1157(3) 0.1191(3) 0.7947(3) H90 H -0.11900 0.09310 0.74270 H91 H -0.18460 0.09620 0.80870 C47 C -0.0954(3) 0.2165(3) 0.8056(3) H92 H -0.12330 0.24040 0.85030 H93 H -0.13420 0.23110 0.76630 N5 N 0.00900(18) 0.27305(18) 0.81037(14) C48 C 0.0151(4) 0.3651(4) 0.8583(3) H94 H 0.08450 0.40610 0.86340 H95 H -0.00320 0.35480 0.90510 H96 H -0.03190 0.39660 0.83880 C49 C 0.0333(3) 0.2903(4) 0.7408(2) H97 H 0.02960 0.22880 0.70760 H98 H 0.10210 0.33240 0.74530 H99 H -0.01530 0.32120 0.72260 C50 C 0.2102(3) 0.0559(2) 0.76616(19) H100 H 0.18770 0.01410 0.79890 H101 H 0.27600 0.04870 0.75130 H102 H 0.16020 0.03790 0.72410 C51 C 0.2534(3) 0.2166(3) 0.7524(2) H103 H 0.26040 0.28420 0.77580 H104 H 0.20320 0.19790 0.71040 H105 H 0.31900 0.20870 0.73750 N6 N 0.21999(16) 0.15571(17) 0.80209(12) C52 C 0.2941(2) 0.1834(3) 0.86574(18) H106 H 0.34370 0.14420 0.85650 H107 H 0.33160 0.25140 0.87020 H108? H 0.29590 0.12440 0.88240 H109? H 0.36200 0.20930 0.85140 C53 C 0.2608(4) 0.1753(4) 0.9305(3) H110 H 0.31860 0.20470 0.96810 H111 H 0.23710 0.10620 0.93080 N7 N 0.17393(17) 0.22400(19) 0.94891(12) C54 C 0.1362(6) 0.1690(5) 1.0040(4) H112 H 0.11750 0.09980 0.98240 H113 H 0.07670 0.18810 1.02230 H114? H 0.18980 0.18330 1.04340 C55 C 0.2011(6) 0.3227(4) 0.9787(4) H115 H 0.22530 0.35750 0.94210 H116 H 0.25520 0.33750 1.01780 H117 H 0.14200 0.34240 0.99700 C56? C 0.2764(4) 0.2533(4) 0.9251(3) H118? H 0.28420 0.31570 0.91110 H119? H 0.32830 0.26290 0.96550 C57? C 0.1642(6) 0.1570(5) 0.9921(4) H120? H 0.09470 0.14170 1.00530 H121 H 0.21190 0.18430 1.03530 H122? H 0.17910 0.09800 0.96580 C58? C 0.1550(6) 0.3165(4) 0.9946(4) H123? H 0.16110 0.36550 0.96630 H124? H 0.20520 0.34090 1.03670 H125? H 0.08670 0.30200 1.00990 Cl1A Cl -0.02821(7) -0.05138(7) 0.40302(4) Li2A Li -0.0740(4) 0.0520(4) 0.4968(3) N2A N -0.07615(17) 0.18934(17) 0.48438(12) C38A C 0.0134(3) 0.2650(3) 0.5223(2) H68A H 0.07430 0.25520 0.50020 H69A H 0.00460 0.32840 0.51950 H70A H 0.02080 0.26150 0.57250 C39A C -0.0819(3) 0.1932(3) 0.40948(17) H71A H -0.01880 0.18490 0.39020 H72A H -0.13920 0.14160 0.38280 H73A H -0.09170 0.25570 0.40500 C40A C -0.1674(3) 0.2012(2) 0.5154(2) H74A H -0.15340 0.21700 0.56810 H75A H -0.18650 0.25640 0.50160 C41A C -0.2525(2) 0.1166(2) 0.49382(19) H76A H -0.31110 0.12890 0.51890 H77A H -0.27200 0.10550 0.44200 N3A N -0.22999(19) 0.02792(18) 0.50918(13) C42A C -0.2468(3) 0.0256(3) 0.58390(18) H78A H -0.20300 0.08360 0.61580 H79A H -0.31800 0.02320 0.59060 H80A H -0.23070 -0.03160 0.59500 C43A C -0.2954(4) -0.0585(3) 0.4628(2) H81A H -0.28490 -0.05770 0.41290 H82A H -0.27910 -0.11540 0.47430 H83A H -0.36650 -0.06060 0.46980 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Li1 P1 2.365 1_555 1_555 Fe1 C17 2.120 1_555 1_555 P1 C6 1.891 1_555 1_555 P2 Li1 2.378 1_555 1_555 Si1 C6 1.907 1_555 1_555 Si2 C10 1.815 1_555 1_555 Si3 C10 1.819 1_555 1_555 Si4 C27 1.819 1_555 1_555 Si5 C27 1.815 1_555 1_555 Si6 C34 1.902 1_555 1_555 N1 Li1 2.039 1_555 1_555 C1 N1 1.356 1_555 1_555 C2 C1 1.389 1_555 1_555 H1 C2 0.950 1_555 1_555 C3 C2 1.383 1_555 1_555 H2 C3 0.949 1_555 1_555 C4 C3 1.383 1_555 1_555 H3 C4 0.950 1_555 1_555 C5 N1 1.359 1_555 1_555 C6 C5 1.506 1_555 1_555 H4 C6 1.000 1_555 1_555 C7 Si1 1.872 1_555 1_555 H5 C7 0.979 1_555 1_555 H6 C7 0.980 1_555 1_555 H7 C7 0.980 1_555 1_555 C8 Si1 1.873 1_555 1_555 H8 C8 0.981 1_555 1_555 H9 C8 0.980 1_555 1_555 H10 C8 0.979 1_555 1_555 C9 Si1 1.865 1_555 1_555 H11 C9 0.981 1_555 1_555 H12 C9 0.980 1_555 1_555 H13 C9 0.980 1_555 1_555 C10 P1 1.739 1_555 1_555 C11 Si2 1.880 1_555 1_555 H14 C11 0.980 1_555 1_555 H15 C11 0.980 1_555 1_555 H16 C11 0.981 1_555 1_555 C12 Si2 1.888 1_555 1_555 H17 C12 0.980 1_555 1_555 H18 C12 0.981 1_555 1_555 H19 C12 0.980 1_555 1_555 C13 Si2 1.892 1_555 1_555 H20 C13 0.980 1_555 1_555 H21 C13 0.980 1_555 1_555 H22 C13 0.980 1_555 1_555 C14 Si3 1.886 1_555 1_555 H23 C14 0.981 1_555 1_555 H24 C14 0.980 1_555 1_555 H25 C14 0.979 1_555 1_555 C15 Si3 1.884 1_555 1_555 H26 C15 0.979 1_555 1_555 H27 C15 0.981 1_555 1_555 H28 C15 0.980 1_555 1_555 C16 Si3 1.881 1_555 1_555 H29 C16 0.981 1_555 1_555 H30 C16 0.980 1_555 1_555 H31 C16 0.980 1_555 1_555 C17 P1 1.838 1_555 1_555 C18 Fe1 2.063 1_555 1_555 H32 C18 0.951 1_555 1_555 C19 Fe1 2.032 1_555 1_555 H33 C19 0.949 1_555 1_555 C20 Fe1 2.036 1_555 1_555 H34 C20 0.950 1_555 1_555 C21 Fe1 2.054 1_555 1_555 H35 C21 0.950 1_555 1_555 C22 Fe1 2.059 1_555 1_555 H36 C22 0.950 1_555 1_555 C23 Fe1 2.035 1_555 1_555 H37 C23 0.949 1_555 1_555 C24 Fe1 2.044 1_555 1_555 H38 C24 0.950 1_555 1_555 C25 Fe1 2.059 1_555 1_555 H39 C25 0.950 1_555 1_555 C26 Fe1 2.123 1_555 1_555 C27 P2 1.739 1_555 1_555 C28 Si4 1.882 1_555 1_555 H40 C28 0.980 1_555 1_555 H41 C28 0.980 1_555 1_555 H42 C28 0.980 1_555 1_555 C29 Si4 1.891 1_555 1_555 H43 C29 0.980 1_555 1_555 H44 C29 0.980 1_555 1_555 H45 C29 0.980 1_555 1_555 C30 Si4 1.890 1_555 1_555 H46 C30 0.980 1_555 1_555 H47 C30 0.981 1_555 1_555 H48 C30 0.980 1_555 1_555 C31 Si5 1.896 1_555 1_555 H49 C31 0.980 1_555 1_555 H50 C31 0.981 1_555 1_555 H51 C31 0.979 1_555 1_555 C32 Si5 1.876 1_555 1_555 H52 C32 0.979 1_555 1_555 H53 C32 0.980 1_555 1_555 H54 C32 0.980 1_555 1_555 C33 Si5 1.890 1_555 1_555 H55 C33 0.979 1_555 1_555 H56 C33 0.980 1_555 1_555 H57 C33 0.981 1_555 1_555 C34 P2 1.903 1_555 1_555 H58 C34 1.000 1_555 1_555 C35 Si6 1.856 1_555 1_555 H59 C35 0.981 1_555 1_555 H60 C35 0.980 1_555 1_555 H61 C35 0.980 1_555 1_555 C36 Si6 1.868 1_555 1_555 H62 C36 0.981 1_555 1_555 H63 C36 0.980 1_555 1_555 H64 C36 0.981 1_555 1_555 C37 Si6 1.877 1_555 1_555 H65 C37 0.981 1_555 1_555 H66 C37 0.980 1_555 1_555 H67 C37 0.979 1_555 1_555 Cl1 Li2 2.321 1_555 1_555 Li2 N2 2.088 1_555 1_555 C38 H68 0.980 1_555 1_555 H69 C38 0.979 1_555 1_555 H70 C38 0.981 1_555 1_555 C39 H71 0.979 1_555 1_555 H72 C39 0.981 1_555 1_555 H73 C39 0.980 1_555 1_555 N2 C38 1.476 1_555 1_555 C40 N2 1.441 1_555 1_555 H74 C40 0.991 1_555 1_555 H75 C40 0.991 1_555 1_555 C41 C40 1.451 1_555 1_555 H76 C41 0.989 1_555 1_555 H77 C41 0.989 1_555 1_555 N3 Li2 2.107 1_555 1_555 C42 N3 1.475 1_555 1_555 H78 C42 0.980 1_555 1_555 H79 C42 0.980 1_555 1_555 H80 C42 0.980 1_555 1_555 C43 N3 1.452 1_555 1_555 H81 C43 0.981 1_555 1_555 H82 C43 0.980 1_555 1_555 H83 C43 0.981 1_555 1_555 Li3 N4 2.098 1_555 1_555 C44 H84 0.979 1_555 1_555 H85 C44 0.980 1_555 1_555 H86 C44 0.980 1_555 1_555 C45 H87 0.980 1_555 1_555 H88 C45 0.980 1_555 1_555 H89 C45 0.980 1_555 1_555 N4 C44 1.444 1_555 1_555 C46 N4 1.463 1_555 1_555 H90 C46 0.990 1_555 1_555 H91 C46 0.991 1_555 1_555 C47 C46 1.358 1_555 1_555 H92 C47 0.991 1_555 1_555 H93 C47 0.991 1_555 1_555 N5 Li3 2.121 1_555 1_555 C48 N5 1.451 1_555 1_555 H94 C48 0.980 1_555 1_555 H95 C48 0.980 1_555 1_555 H96 C48 0.979 1_555 1_555 C49 N5 1.455 1_555 1_555 H97 C49 0.981 1_555 1_555 H98 C49 0.980 1_555 1_555 H99 C49 0.979 1_555 1_555 C50 H100 0.979 1_555 1_555 H101 C50 0.979 1_555 1_555 H102 C50 0.980 1_555 1_555 C51 H103 0.981 1_555 1_555 H104 C51 0.980 1_555 1_555 H105 C51 0.980 1_555 1_555 N6 Li3 2.115 1_555 1_555 C52 N6 1.471 1_555 1_555 H106 C52 0.990 1_555 1_555 H107 C52 0.990 1_555 1_555 C53 C52 1.367 1_555 1_555 H110 C53 0.991 1_555 1_555 H111 C53 0.989 1_555 1_555 N7 Li3 2.123 1_555 1_555 C54 N7 1.502 1_555 1_555 H112 C54 0.979 1_555 1_555 H113 C54 0.980 1_555 1_555 C55 N7 1.393 1_555 1_555 H115 C55 0.980 1_555 1_555 H116 C55 0.979 1_555 1_555 H117 C55 0.979 1_555 1_555 H121 C54 1.119 1_555 1_555 Cl1A Li2 2.328 1_555 1_555 Li2A Cl1 2.328 1_555 1_555 N2A Li2A 2.088 1_555 1_555 C38A N2A 1.476 1_555 1_555 H68A C38A 0.980 1_555 1_555 H69A C38A 0.979 1_555 1_555 H70A C38A 0.981 1_555 1_555 C39A N2A 1.455 1_555 1_555 H71A C39A 0.979 1_555 1_555 H72A C39A 0.981 1_555 1_555 H73A C39A 0.980 1_555 1_555 C40A N2A 1.441 1_555 1_555 H74A C40A 0.991 1_555 1_555 H75A C40A 0.991 1_555 1_555 C41A C40A 1.451 1_555 1_555 H76A C41A 0.989 1_555 1_555 H77A C41A 0.989 1_555 1_555 N3A Li2A 2.107 1_555 1_555 C42A N3A 1.475 1_555 1_555 H78A C42A 0.980 1_555 1_555 H79A C42A 0.980 1_555 1_555 H80A C42A 0.980 1_555 1_555 C43A N3A 1.452 1_555 1_555 H81A C43A 0.981 1_555 1_555 H82A C43A 0.980 1_555 1_555 H83A C43A 0.981 1_555 1_555 P2 C26 1.853 1_555 1_555 C1 C34 1.510 1_555 1_555 C4 C5 1.392 1_555 1_555 C17 C18 1.431 1_555 1_555 C17 C21 1.430 1_555 1_555 C18 C19 1.423 1_555 1_555 C19 C20 1.415 1_555 1_555 C20 C21 1.421 1_555 1_555 C22 C23 1.416 1_555 1_555 C22 C26 1.431 1_555 1_555 C23 C24 1.420 1_555 1_555 C24 C25 1.420 1_555 1_555 C25 C26 1.431 1_555 1_555 C39 N2 1.455 1_555 1_555 C41 N3 1.491 1_555 1_555 C45 N4 1.455 1_555 1_555 C47 N5 1.454 1_555 1_555 C50 N6 1.456 1_555 1_555 C51 N6 1.459 1_555 1_555 C53 N7 1.546 1_555 1_555 Cl1A Li2A 2.321 1_555 1_555 C41A N3A 1.491 1_555 1_555 #END data_CSD_CIF_XIDGIA _audit_creation_date 2002-05-23 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD XIDGIA _chemical_formula_sum 'C36 H70 Li2 N6' _chemical_formula_moiety ; C12 H32 Li1 N4 1+,C24 H38 Li1 N2 1- ; _journal_coden_Cambridge 579 _journal_volume 20 _journal_year 2001 _journal_page_first 1689 _journal_name_full 'Organometallics ' loop_ _publ_author_name "U.J.Bildmann" "G.Muller" _chemical_name_systematic ; bis(N,N,N',N'-Tetramethylethylenediamine-N,N')-lithium bis(3,5-dimethylbenzyl)-(N,N,N',N'-tetramethylethylenediamine-N,N')-lithium ; _chemical_melting_point 331.15 _cell_volume 4025.385 _exptl_crystal_colour 'deep red' _exptl_crystal_density_diffrn 0.992 _exptl_special_details ; Melting point range 331.15-335.15K extremely air-sensitive ; _diffrn_ambient_temperature 188 _refine_special_details ; C511-C561, from a ethylenediamine ligand, are disordered over two sites with occupancies 0.6:0.4. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_gt 0.0643 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,1/2+y,1/2-z _cell_length_a 8.8000(9) _cell_length_b 14.309(2) _cell_length_c 31.968(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.48 N 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z N1 N 0.6877(4) 0.2833(2) 0.08052(10) N2 N 0.9641(4) 0.3885(3) 0.09999(10) N3 N 0.7146(4) 0.3406(2) 0.19180(9) N4 N 0.6246(4) 0.5035(21) 0.14221(10) C1 C 0.6661(8) 0.2458(4) 0.20225(19) C2 C 0.8549(7) 0.3587(5) 0.21479(16) C3 C 0.5927(6) 0.4050(3) 0.20461(15) C4 C 0.6142(6) 0.5003(3) 0.18825(14) C5 C 0.4751(6) 0.4944(4) 0.12253(19) C6 C 0.6891(7) 0.5917(3) 0.12983(16) C7 C 0.5243(8) 0.2964(5) 0.0607(2) C8 C 0.6919(9) 0.1875(5) 0.0960(2) C9 C 0.7897(7) 0.2988(5) 0.04777(19) C10 C 0.9459(8) 0.3032(5) 0.0670(2) C11 C 1.0913(8) 0.3668(5) 0.1252(2) C12 C 0.9776(10) 0.4675(5) 0.0754(2) Li1 Li 0.7499(6) 0.3782(4) 0.12832(17) C13? C 0.8661(10) 0.2707(7) 0.0642(3) C14? C 0.6448(11) 0.1916(6) 0.0954(3) C15? C 0.6053(16) 0.3209(10) 0.0487(4) C16? C 0.0864(11) 0.3455(7) 0.1258(3) C17? C 0.9518(12) 0.3624(7) 0.0602(3) C18? C 1.0235(13) 0.4951(7) 0.0979(3) N5 N 0.1613(3) 0.8438(2) 0.11706(8) N6 N 0.4436(3) 0.93170(19) 0.14537(9) C19 C 0.2405(4) 0.9864(3) 0.02218(10) C20 C 0.2720(5) 0.9029(3) 0.00051(12) C21 C 0.1567(6) 0.8494(3) -0.01819(11) C22 C 0.0080(6) 0.8790(3) -0.01648(12) C23 C -0.0273(4) 0.9611(3) 0.00420(11) C24 C 0.0847(4) 1.0134(3) 0.02258(10) C25 C 0.3526(5) 1.0369(4) 0.04366(13) C26 C 0.1960(8) 0.7596(3) -0.03985(15) C27 C -0.1917(6) 0.9942(5) 0.00695(19) C28 C 0.0838(4) 1.1077(2) 0.17772(11) C29 C 0.1777(4) 1.1684(3) 0.20214(12) C30 C 0.1557(4) 1.1848(2) 0.24417(11) C31 C 0.0366(4) 1.1389(3) 0.26502(11) C32 C -0.0562(4) 1.0786(3) 0.24266(11) C33 C -0.0328(4) 1.0645(3) 0.20084(13) C34 C 0.1101(5) 1.0923(3) 0.13488(12) C35 C 0.2551(5) 1.2523(3) 0.26754(13) C36 C -0.1881(5) 1.0320(3) 0.26499(14) C37 C -0.0054(5) 0.8502(4) 0.12154(18) C38 C 0.1951(6) 0.7711(3) 0.08790(14) C39 C 0.2262(5) 0.8295(3) 0.15825(12) C40 C 0.3922(5) 0.8412(3) 0.16004(15) C41 C 0.4491(6) 0.9989(3) 0.17887(14) C42 C 0.5955(5) 0.9252(3) 0.12707(15) Li2 Li 0.2626(7) 0.9784(4) 0.10438(17) H1 H 0.43090 0.43640 0.13020 H2 H 0.51350 0.35880 0.05100 H3 H 0.44910 0.28400 0.08130 H4 H 0.68180 0.14540 0.07320 H5 H 0.61070 0.17800 0.11510 H6 H 0.78590 0.17660 0.10980 H7 H 0.76660 0.35590 0.03390 H8 H 0.78420 0.24940 0.02800 H9 H 1.01910 0.31030 0.04540 H10 H 0.96620 0.24590 0.08090 H11 H 1.18140 0.37260 0.10900 H12 H 1.08240 0.30460 0.13520 H13 H 1.09550 0.40880 0.14820 H14 H 0.88700 0.47600 0.05970 H15 H 1.06120 0.46030 0.05680 H16 H 0.99390 0.52040 0.09270 H17 H 0.645(4) 0.241(3) 0.2312(13) H18 H 0.748(5) 0.204(3) 0.1928(12) H19 H 0.580(5) 0.237(3) 0.1856(12) H20 H 0.921(5) 0.306(3) 0.2064(12) H21 H 0.889(4) 0.420(3) 0.2050(12) H22 H 0.842(5) 0.368(3) 0.2398(13) H23 H 0.583(4) 0.406(3) 0.2338(13) H24 H 0.495(5) 0.384(2) 0.1883(11) H25 H 0.715(5) 0.526(2) 0.2024(11) H26 H 0.523(5) 0.540(3) 0.1979(11) H27 H 0.48590 0.49710 0.09300 H28 H 0.41140 0.54410 0.13160 H29 H 0.78590 0.59910 0.14260 H30 H 0.62400 0.64100 0.13820 H31 H 0.70010 0.59320 0.10030 H32? H 0.51220 0.25440 0.03800 H33? H 0.61610 0.15370 0.07230 H34? H 0.56160 0.19720 0.11410 H35? H 0.72840 0.16380 0.10940 H36? H 0.61720 0.28370 0.02430 H37? H 0.64020 0.38250 0.04320 H38? H 0.50100 0.32280 0.05630 H39? H 0.91780 0.23140 0.08330 H40? H 0.86540 0.24040 0.03770 H41? H 1.04870 0.35360 0.04780 H42? H 0.89600 0.40680 0.04440 H43? H 0.95090 0.53240 0.08360 H44? H 1.11760 0.49730 0.08340 H45? H 1.03690 0.51840 0.12550 H46? H 1.17590 0.33900 0.10950 H47? H 1.05440 0.28570 0.13530 H48? H 1.10700 0.38440 0.14930 H49 H 0.30260 0.74960 -0.03830 H50 H 0.16590 0.76310 -0.06830 H51 H 0.14440 0.70930 -0.02660 H52 H 0.237(5) 1.198(3) 0.1894(12) H53 H 0.22380 1.25500 0.29600 H54 H 0.24660 1.31260 0.25530 H55 H 0.35770 1.23190 0.26610 H56 H -0.18750 1.04950 0.29370 H57 H -0.17840 0.96600 0.26280 H58 H -0.28100 1.05120 0.25250 H59 H -0.049(4) 0.875(3) 0.0951(12) H60 H 0.14940 0.78510 0.06170 H61 H 0.15640 0.71350 0.09810 H62 H 0.30210 0.76640 0.08450 H63 H 0.20150 0.76820 0.16740 H64 H 0.18060 0.87240 0.17720 H65 H 0.59480 0.88110 0.10490 H66 H 0.66570 0.90560 0.14790 H67 H 0.62490 0.98460 0.11660 H68 H 0.383(4) 0.884(3) -0.0039(11) H69 H -0.069(4) 0.842(3) -0.0299(11) H70 H 0.054(4) 1.070(3) 0.0350(11) H71 H 0.321(5) 1.094(3) 0.0479(12) H72 H 0.436(5) 1.024(3) 0.0374(12) H73 H -0.245(4) 0.992(2) 0.0402(12) H74 H -0.192(4) 1.060(3) 0.0011(12) H75 H -0.250(5) 0.958(3) -0.0038(12) H76 H 0.028(4) 1.153(2) 0.2934(12) H77 H -0.087(5) 1.030(3) 0.1898(12) H78 H 0.039(5) 1.069(3) 0.1190(12) H79 H 0.187(4) 1.136(3) 0.1208(11) H80 H -0.042(4) 0.790(3) 0.1294(11) H81 H -0.020(4) 0.906(3) 0.1434(11) H82 H 0.429(4) 0.831(2) 0.1891(12) H83 H 0.429(4) 0.794(3) 0.1420(12) H84 H 0.364(5) 1.000(3) 0.1926(12) H85 H 0.513(5) 0.977(3) 0.1999(12) H86 H 0.482(4) 1.063(3) 0.1671(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 N1 C7 1.582 1_555 1_555 N2 C10 1.621 1_555 1_555 N3 C1 1.461 1_555 1_555 N4 C4 1.475 1_555 1_555 C1 H17 0.946 1_555 1_555 C2 N3 1.460 1_555 1_555 C3 N3 1.472 1_555 1_555 C4 C3 1.473 1_555 1_555 C5 N4 1.464 1_555 1_555 C6 N4 1.439 1_555 1_555 C7 H2 0.950 1_555 1_555 C8 N1 1.458 1_555 1_555 C9 N1 1.397 1_555 1_555 C10 C9 1.507 1_555 1_555 C11 N2 1.414 1_555 1_555 C12 N2 1.382 1_555 1_555 Li1 N1 2.116 1_555 1_555 N5 C37 1.477 1_555 1_555 N6 C40 1.450 1_555 1_555 C19 C20 1.409 1_555 1_555 C20 C21 1.405 1_555 1_555 C21 C22 1.376 1_555 1_555 C22 C23 1.383 1_555 1_555 C23 C24 1.370 1_555 1_555 C24 C19 1.424 1_555 1_555 C25 C19 1.402 1_555 1_555 C26 C21 1.500 1_555 1_555 C27 C23 1.525 1_555 1_555 C28 C29 1.431 1_555 1_555 C29 C30 1.378 1_555 1_555 C30 C31 1.405 1_555 1_555 C31 C32 1.386 1_555 1_555 C32 C33 1.368 1_555 1_555 C33 C28 1.408 1_555 1_555 C34 C28 1.406 1_555 1_555 C35 C30 1.502 1_555 1_555 C36 C32 1.517 1_555 1_555 C37 H59 0.994 1_555 1_555 C38 N5 1.428 1_555 1_555 C39 N5 1.450 1_555 1_555 C40 C39 1.471 1_555 1_555 C41 N6 1.440 1_555 1_555 C42 N6 1.462 1_555 1_555 Li2 N5 2.161 1_555 1_555 H1 C5 0.949 1_555 1_555 H3 C7 0.950 1_555 1_555 H4 C8 0.950 1_555 1_555 H5 C8 0.950 1_555 1_555 H6 C8 0.950 1_555 1_555 H7 C9 0.952 1_555 1_555 H8 C9 0.949 1_555 1_555 H9 C10 0.950 1_555 1_555 H10 C10 0.950 1_555 1_555 H11 C11 0.951 1_555 1_555 H12 C11 0.949 1_555 1_555 H13 C11 0.950 1_555 1_555 H14 C12 0.950 1_555 1_555 H15 C12 0.952 1_555 1_555 H16 C12 0.948 1_555 1_555 H18 C1 0.984 1_555 1_555 H19 C1 0.934 1_555 1_555 H20 C2 0.989 1_555 1_555 H21 C2 0.978 1_555 1_555 H22 C2 0.818 1_555 1_555 H23 C3 0.937 1_555 1_555 H24 C3 1.049 1_555 1_555 H25 C4 1.061 1_555 1_555 H26 C4 1.031 1_555 1_555 H27 C5 0.950 1_555 1_555 H28 C5 0.951 1_555 1_555 H29 C6 0.951 1_555 1_555 H30 C6 0.947 1_555 1_555 H31 C6 0.949 1_555 1_555 H49 C26 0.950 1_555 1_555 H50 C26 0.949 1_555 1_555 H51 C26 0.951 1_555 1_555 H52 C29 0.786 1_555 1_555 H53 C35 0.951 1_555 1_555 H54 C35 0.950 1_555 1_555 H55 C35 0.950 1_555 1_555 H56 C36 0.951 1_555 1_555 H57 C36 0.951 1_555 1_555 H58 C36 0.950 1_555 1_555 H60 C38 0.950 1_555 1_555 H61 C38 0.950 1_555 1_555 H62 C38 0.950 1_555 1_555 H63 C39 0.950 1_555 1_555 H64 C39 0.951 1_555 1_555 H65 C42 0.949 1_555 1_555 H66 C42 0.951 1_555 1_555 H67 C42 0.949 1_555 1_555 H68 C20 1.023 1_555 1_555 H69 C22 0.961 1_555 1_555 H70 C24 0.942 1_555 1_555 H71 C25 0.874 1_555 1_555 H72 C25 0.783 1_555 1_555 H73 C27 1.162 1_555 1_555 H74 C27 0.960 1_555 1_555 H75 C27 0.806 1_555 1_555 H76 C31 0.932 1_555 1_555 H77 C33 0.772 1_555 1_555 H78 C34 0.872 1_555 1_555 H79 C34 1.025 1_555 1_555 H80 C37 0.953 1_555 1_555 H81 C37 1.069 1_555 1_555 H82 C40 0.995 1_555 1_555 H83 C40 0.945 1_555 1_555 H84 C41 0.868 1_555 1_555 H85 C41 0.931 1_555 1_555 H86 C41 1.033 1_555 1_555 N2 Li1 2.096 1_555 1_555 N3 Li1 2.122 1_555 1_555 N4 Li1 2.151 1_555 1_555 N6 Li2 2.168 1_555 1_555 C25 Li2 2.257 1_555 1_555 C34 Li2 2.325 1_555 1_555 #END data_CSD_CIF_XUDCAC _audit_creation_date 2015-04-04 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD XUDCAC _database_code_depnum_ccdc_archive 'CCDC 1037635' _chemical_formula_sum 'C61 H100 Li2 N6 P4' _chemical_formula_moiety ; C42 H60 Li1 N2 P4 1-,C12 H32 Li1 N4 1+,C7 H8 ; _journal_coden_Cambridge 1290 _journal_year 2015 _journal_page_first 2041 _journal_name_full 'Eur.J.Inorg.Chem. ' loop_ _publ_author_name "L.S.H.Dixon" "P.D.Matthews" "S.A.Solomon" "D.S.Wright" _chemical_name_systematic ; bis(N,N,N',N'-tetramethylethane-1,2-diamine)-lithium (1,2,3,4-tetramesityltetraphosphanato)-(N,N,N',N'-tetramethylethane-1,2-diamin e)-lithium toluene solvate ; _cell_volume 3276.639 _exptl_crystal_colour 'orange' _exptl_crystal_density_diffrn 1.07 _exptl_special_details ; Air-sensitive, Moisture-sensitive ; _exptl_crystal_description 'block' _exptl_crystal_preparation 'Toluene' _diffrn_ambient_temperature 240 _refine_special_details ; C51,C52,C53,C54,C55,C56,C57 disordered by symmetry over two configurations with occupancy 0.50. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0947 _refine_ls_wR_factor_gt 0.0947 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,y,1/2-z 3 -x,-y,-z 4 -1/2+x,-y,-1/2+z _cell_length_a 16.1229(7) _cell_length_b 12.2196(6) _cell_length_c 17.0599(8) _cell_angle_alpha 90 _cell_angle_beta 102.869(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.28 N 0.68 P 1.05 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z P1 P 0.74083(11) 0.77708(14) 0.13494(10) P2 P 0.77738(10) 0.93316(13) 0.19491(9) Li1 Li 0.75000 0.6412(13) 0.25000 N1 N 0.8432(4) 0.5133(5) 0.2633(4) C1 C 0.7939(6) 0.4189(7) 0.2765(6) H1 H 0.78940 0.41780 0.33290 H2 H 0.82360 0.35220 0.26650 C2 C 0.8760(6) 0.4979(7) 0.1902(5) H3 H 0.91320 0.43460 0.19670 H4 H 0.90760 0.56240 0.18100 H5 H 0.82880 0.48660 0.14450 C3 C 0.9171(7) 0.5326(11) 0.3313(6) H6 H 0.95780 0.47360 0.33390 H7 H 0.89780 0.53540 0.38120 H8 H 0.94390 0.60150 0.32330 C4 C 0.8252(4) 0.7400(5) 0.0824(3) C5 C 0.7979(4) 0.6676(5) 0.0158(3) C6 C 0.8540(5) 0.6341(6) -0.0303(4) H9 H 0.83360 0.58760 -0.07420 C7 C 0.9392(5) 0.6658(6) -0.0148(4) C8 C 0.9661(4) 0.7318(6) 0.0516(4) H10 H 1.02350 0.75370 0.06470 C9 C 0.9128(4) 0.7679(5) 0.1004(4) C10 C 0.7068(4) 1.0389(5) 0.1363(3) C11 C 0.6173(4) 1.0336(6) 0.1108(3) C12 C 0.5730(5) 1.1187(7) 0.0650(4) H11 H 0.51340 1.11410 0.04880 C13 C 0.6134(6) 1.2091(6) 0.0426(4) C14 C 0.7011(5) 1.2150(6) 0.0691(4) H12 H 0.73000 1.27670 0.05590 C15 C 0.7473(4) 1.1324(5) 0.1146(3) C16 C 0.7093(5) 0.6230(6) -0.0043(4) H13 H 0.69920 0.58660 -0.05610 H14 H 0.66900 0.68250 -0.00650 H15 H 0.70220 0.57100 0.03670 C17 C 0.9994(5) 0.6255(7) -0.0648(5) H16 H 1.05750 0.64150 -0.03730 H17 H 0.98670 0.66200 -0.11660 H18 H 0.99260 0.54710 -0.07270 C18 C 0.9555(4) 0.8288(8) 0.1769(5) H19 H 1.01600 0.81350 0.18940 H20 H 0.93110 0.80470 0.22110 H21 H 0.94640 0.90690 0.16890 C19 C 0.5667(4) 0.9384(7) 0.1322(4) H22 H 0.50700 0.94810 0.10690 H23 H 0.57340 0.93520 0.19010 H24 H 0.58720 0.87080 0.11340 C20 C 0.5644(7) 1.3004(8) -0.0085(6) H25 H 0.50800 1.30610 0.00230 H26 H 0.55970 1.28390 -0.06500 H27 H 0.59440 1.36910 0.00460 C21 C 0.8428(5) 1.1494(6) 0.1419(5) H28 H 0.85770 1.22120 0.12520 H29 H 0.87230 1.09380 0.11790 H30 H 0.85940 1.14390 0.20000 Li2 Li 0.75000 0.9209(13) -0.25000 N2 N 0.7677(5) 1.0027(6) -0.1360(4) N3 N 0.6480(4) 0.8367(6) -0.2175(4) C22 C 0.6878(8) 0.9764(11) -0.1126(6) H31 H 0.69490 0.98930 -0.05480 H32 H 0.64310 1.02560 -0.14100 C23 C 0.6610(7) 0.8648(9) -0.1303(6) H33 H 0.60770 0.85240 -0.11300 H34 H 0.70410 0.81560 -0.09910 C24 C 0.7734(9) 1.1220(8) -0.1400(6) H35 H 0.78000 1.15250 -0.08650 H36 H 0.72180 1.15060 -0.17450 H37 H 0.82200 1.14210 -0.16170 C25 C 0.8415(8) 0.9659(9) -0.0755(6) H38 H 0.84060 0.99950 -0.02420 H39 H 0.89320 0.98690 -0.09180 H40 H 0.83970 0.88690 -0.07040 C26 C 0.6508(6) 0.7177(8) -0.2229(6) H41 H 0.60430 0.68630 -0.20280 H42 H 0.70450 0.69120 -0.19100 H43 H 0.64550 0.69640 -0.27860 C27 C 0.5669(6) 0.8736(11) -0.2630(7) H44 H 0.52200 0.84370 -0.23980 H45 H 0.55920 0.84910 -0.31820 H46 H 0.56480 0.95290 -0.26160 C28 C 0.8015(8) 0.3997(14) -0.2617(9) C29 C 0.7216(10) 0.4009(16) -0.3134(7) H47 H 0.71670 0.40380 -0.36930 C30 C 0.6489(8) 0.3977(19) -0.2823(10) H48 H 0.59480 0.39840 -0.31720 C31 C 0.6561(9) 0.3933(18) -0.1996(10) H49 H 0.60700 0.39110 -0.17860 C32 C 0.7361(11) 0.3921(19) -0.1480(7) H50 H 0.74100 0.38910 -0.09210 C33 C 0.8088(9) 0.3953(18) -0.1791(8) H51 H 0.86290 0.39450 -0.14410 C34 C 0.8782(14) 0.407(2) -0.2864(12) H52 H 0.86690 0.40970 -0.34460 H53 H 0.91340 0.34440 -0.26700 H54 H 0.90770 0.47370 -0.26460 P1A P 0.75917(11) 0.77708(14) 0.36506(10) P2A P 0.72262(10) 0.93316(13) 0.30509(9) C4A C 0.6748(4) 0.7400(5) 0.4176(3) C5A C 0.7021(4) 0.6676(5) 0.4842(3) C6A C 0.6460(5) 0.6341(6) 0.5303(4) H9A H 0.66640 0.58760 0.57420 C7A C 0.5608(5) 0.6658(6) 0.5148(4) C8A C 0.5339(4) 0.7318(6) 0.4484(4) H10A H 0.47650 0.75370 0.43530 C9A C 0.5872(4) 0.7679(5) 0.3996(4) C10A C 0.7932(4) 1.0389(5) 0.3637(3) C11A C 0.8827(4) 1.0336(6) 0.3892(3) C12A C 0.9270(5) 1.1187(7) 0.4350(4) H11A H 0.98660 1.11410 0.45120 C13A C 0.8866(6) 1.2091(6) 0.4574(4) C14A C 0.7989(5) 1.2150(6) 0.4309(4) H12A H 0.77000 1.27670 0.44410 C15A C 0.7527(4) 1.1324(5) 0.3854(3) C16A C 0.7907(5) 0.6230(6) 0.5043(4) H13A H 0.80080 0.58660 0.55610 H14A H 0.83100 0.68250 0.50650 H15A H 0.79780 0.57100 0.46330 C17A C 0.5006(5) 0.6255(7) 0.5648(5) H16A H 0.44250 0.64150 0.53730 H17A H 0.51330 0.66200 0.61660 H18A H 0.50740 0.54710 0.57270 C18A C 0.5445(4) 0.8288(8) 0.3231(5) H19A H 0.48400 0.81350 0.31060 H20A H 0.56890 0.80470 0.27890 H21A H 0.55360 0.90690 0.33110 C19A C 0.9333(4) 0.9384(7) 0.3678(4) H22A H 0.99300 0.94810 0.39310 H23A H 0.92660 0.93520 0.30990 H24A H 0.91280 0.87080 0.38660 C20A C 0.9356(7) 1.3004(8) 0.5085(6) H25A H 0.99200 1.30610 0.49770 H26A H 0.94030 1.28390 0.56500 H27A H 0.90560 1.36910 0.49540 C21A C 0.6572(5) 1.1494(6) 0.3581(5) H28A H 0.64230 1.22120 0.37480 H29A H 0.62770 1.09380 0.38210 H30A H 0.64060 1.14390 0.30000 N1A N 0.6568(4) 0.5133(5) 0.2367(4) C1A C 0.7061(6) 0.4189(7) 0.2235(6) H1A H 0.71060 0.41780 0.16710 H2A H 0.67640 0.35220 0.23350 C2A C 0.6240(6) 0.4979(7) 0.3098(5) H3A H 0.58680 0.43460 0.30330 H4A H 0.59240 0.56240 0.31900 H5A H 0.67120 0.48660 0.35550 C3A C 0.5829(7) 0.5326(11) 0.1687(6) H6A H 0.54220 0.47360 0.16610 H7A H 0.60220 0.53540 0.11880 H8A H 0.55610 0.60150 0.17670 N2A N 0.7323(5) 1.0027(6) -0.3640(4) N3A N 0.8520(4) 0.8367(6) -0.2825(4) C22A C 0.8122(8) 0.9764(11) -0.3874(6) H31A H 0.80510 0.98930 -0.44520 H32A H 0.85690 1.02560 -0.35900 C23A C 0.8390(7) 0.8648(9) -0.3697(6) H33A H 0.89230 0.85240 -0.38700 H34A H 0.79590 0.81560 -0.40090 C24A C 0.7266(9) 1.1220(8) -0.3600(6) H35A H 0.72000 1.15250 -0.41350 H36A H 0.77820 1.15060 -0.32550 H37A H 0.67800 1.14210 -0.33830 C25A C 0.6585(8) 0.9659(9) -0.4245(6) H38A H 0.65940 0.99950 -0.47580 H39A H 0.60680 0.98690 -0.40820 H40A H 0.66030 0.88690 -0.42960 C26A C 0.8492(6) 0.7177(8) -0.2771(6) H41A H 0.89570 0.68630 -0.29720 H42A H 0.79550 0.69120 -0.30900 H43A H 0.85450 0.69640 -0.22140 C27A C 0.9331(6) 0.8736(11) -0.2370(7) H44A H 0.97800 0.84370 -0.26020 H45A H 0.94080 0.84910 -0.18180 H46A H 0.93520 0.95290 -0.23840 C28A C 0.6985(8) 0.3997(14) -0.2383(9) C29A C 0.7784(10) 0.4009(16) -0.1866(7) H47A H 0.78330 0.40380 -0.13070 C30A C 0.8511(8) 0.3977(19) -0.2177(10) H48A H 0.90520 0.39840 -0.18280 C31A C 0.8439(9) 0.3933(18) -0.3004(10) H49A H 0.89300 0.39110 -0.32140 C32A C 0.7639(11) 0.3921(19) -0.3520(7) H50A H 0.75900 0.38910 -0.40790 C33A C 0.6912(9) 0.3953(18) -0.3209(8) H51A H 0.63710 0.39450 -0.35590 C34A C 0.6218(14) 0.407(2) -0.2136(12) H52A H 0.63310 0.40970 -0.15540 H53A H 0.58660 0.34440 -0.23300 H54A H 0.59230 0.47370 -0.23540 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 P1 P2 2.182 1_555 1_555 P2 C10 1.859 1_555 1_555 Li1 P1 2.550 1_555 1_555 N1 Li1 2.145 1_555 1_555 C1 N1 1.447 1_555 1_555 H1 C1 0.981 1_555 1_555 H2 C1 0.979 1_555 1_555 C2 N1 1.471 1_555 1_555 H3 C2 0.970 1_555 1_555 H4 C2 0.970 1_555 1_555 H5 C2 0.970 1_555 1_555 C3 N1 1.485 1_555 1_555 H6 C3 0.969 1_555 1_555 H7 C3 0.970 1_555 1_555 H8 C3 0.970 1_555 1_555 C4 P1 1.845 1_555 1_555 C5 C4 1.430 1_555 1_555 C6 C5 1.386 1_555 1_555 H9 C6 0.939 1_555 1_555 C7 C6 1.395 1_555 1_555 C8 C7 1.379 1_555 1_555 H10 C8 0.941 1_555 1_555 C9 C4 1.418 1_555 1_555 C10 C11 1.413 1_555 1_555 C11 C12 1.398 1_555 1_555 C12 H11 0.941 1_555 1_555 C13 C12 1.379 1_555 1_555 C14 C13 1.387 1_555 1_555 H12 C14 0.940 1_555 1_555 C15 C10 1.406 1_555 1_555 C16 C5 1.496 1_555 1_555 H13 C16 0.970 1_555 1_555 H14 C16 0.970 1_555 1_555 H15 C16 0.970 1_555 1_555 C17 C7 1.510 1_555 1_555 H16 C17 0.970 1_555 1_555 H17 C17 0.970 1_555 1_555 H18 C17 0.970 1_555 1_555 C18 C9 1.527 1_555 1_555 H19 C18 0.969 1_555 1_555 H20 C18 0.971 1_555 1_555 H21 C18 0.971 1_555 1_555 C19 C11 1.512 1_555 1_555 H22 C19 0.970 1_555 1_555 H23 C19 0.970 1_555 1_555 H24 C19 0.970 1_555 1_555 C20 C13 1.524 1_555 1_555 H25 C20 0.970 1_555 1_555 H26 C20 0.971 1_555 1_555 H27 C20 0.970 1_555 1_555 C21 C15 1.520 1_555 1_555 H28 C21 0.969 1_555 1_555 H29 C21 0.971 1_555 1_555 H30 C21 0.970 1_555 1_555 Li2 N2 2.148 1_555 1_555 N2 C22 1.467 1_555 1_555 N3 Li2 2.116 1_555 1_555 C22 H31 0.980 1_555 1_555 H32 C22 0.980 1_555 1_555 C23 N3 1.495 1_555 1_555 H33 C23 0.981 1_555 1_555 H34 C23 0.981 1_555 1_555 C24 N2 1.463 1_555 1_555 H35 C24 0.970 1_555 1_555 H36 C24 0.971 1_555 1_555 H37 C24 0.970 1_555 1_555 C25 N2 1.462 1_555 1_555 H38 C25 0.970 1_555 1_555 H39 C25 0.970 1_555 1_555 H40 C25 0.970 1_555 1_555 C26 N3 1.458 1_555 1_555 H41 C26 0.970 1_555 1_555 H42 C26 0.970 1_555 1_555 H43 C26 0.970 1_555 1_555 C27 N3 1.436 1_555 1_555 H44 C27 0.970 1_555 1_555 H45 C27 0.969 1_555 1_555 H46 C27 0.970 1_555 1_555 C28 C29 1.390 1_555 1_555 C29 H47 0.940 1_555 1_555 H47 C32A 0.766 1_555 1_555 C30 C29 1.391 1_555 1_555 H48 C30 0.940 1_555 1_555 C31 H49 0.939 1_555 1_555 H49 C34A 0.717 1_555 1_555 C32 C31 1.390 1_555 1_555 H50 C32 0.940 1_555 1_555 C33 C28 1.389 1_555 1_555 H51 C33 0.941 1_555 1_555 C34 H52 0.969 1_555 1_555 H52 C31A 0.933 1_555 1_555 H53 C34 0.966 1_555 1_555 H54 C34 0.975 1_555 1_555 P1A Li1 2.550 1_555 1_555 P2A P2 2.248 1_555 1_555 C4A P1A 1.845 1_555 1_555 C5A C4A 1.430 1_555 1_555 C6A C5A 1.386 1_555 1_555 H9A C6A 0.939 1_555 1_555 C7A C6A 1.395 1_555 1_555 C8A C7A 1.379 1_555 1_555 H10A C8A 0.941 1_555 1_555 C9A C4A 1.418 1_555 1_555 C10A P2A 1.859 1_555 1_555 C11A C10A 1.413 1_555 1_555 C12A C11A 1.398 1_555 1_555 H11A C12A 0.941 1_555 1_555 C13A C12A 1.379 1_555 1_555 C14A C13A 1.387 1_555 1_555 H12A C14A 0.940 1_555 1_555 C15A C10A 1.406 1_555 1_555 C16A C5A 1.496 1_555 1_555 H13A C16A 0.970 1_555 1_555 H14A C16A 0.970 1_555 1_555 H15A C16A 0.970 1_555 1_555 C17A C7A 1.510 1_555 1_555 H16A C17A 0.970 1_555 1_555 H17A C17A 0.970 1_555 1_555 H18A C17A 0.970 1_555 1_555 C18A C9A 1.527 1_555 1_555 H19A C18A 0.969 1_555 1_555 H20A C18A 0.971 1_555 1_555 H21A C18A 0.971 1_555 1_555 C19A C11A 1.512 1_555 1_555 H22A C19A 0.970 1_555 1_555 H23A C19A 0.970 1_555 1_555 H24A C19A 0.970 1_555 1_555 C20A C13A 1.524 1_555 1_555 H25A C20A 0.970 1_555 1_555 H26A C20A 0.971 1_555 1_555 H27A C20A 0.970 1_555 1_555 C21A C15A 1.520 1_555 1_555 H28A C21A 0.969 1_555 1_555 H29A C21A 0.971 1_555 1_555 H30A C21A 0.970 1_555 1_555 N1A Li1 2.145 1_555 1_555 C1A C1 1.500 1_555 1_555 H1A C1A 0.981 1_555 1_555 H2A C1A 0.979 1_555 1_555 C2A N1A 1.471 1_555 1_555 H3A C2A 0.970 1_555 1_555 H4A C2A 0.970 1_555 1_555 H5A C2A 0.970 1_555 1_555 C3A N1A 1.485 1_555 1_555 H6A C3A 0.969 1_555 1_555 H7A C3A 0.970 1_555 1_555 H8A C3A 0.970 1_555 1_555 N2A Li2 2.148 1_555 1_555 N3A Li2 2.116 1_555 1_555 C22A N2A 1.467 1_555 1_555 H31A C22A 0.980 1_555 1_555 H32A C22A 0.980 1_555 1_555 C23A N3A 1.495 1_555 1_555 H33A C23A 0.981 1_555 1_555 H34A C23A 0.981 1_555 1_555 C24A N2A 1.463 1_555 1_555 H35A C24A 0.970 1_555 1_555 H36A C24A 0.971 1_555 1_555 H37A C24A 0.970 1_555 1_555 C25A N2A 1.462 1_555 1_555 H38A C25A 0.970 1_555 1_555 H39A C25A 0.970 1_555 1_555 H40A C25A 0.970 1_555 1_555 C26A N3A 1.458 1_555 1_555 H41A C26A 0.970 1_555 1_555 H42A C26A 0.970 1_555 1_555 H43A C26A 0.970 1_555 1_555 C27A N3A 1.436 1_555 1_555 H44A C27A 0.970 1_555 1_555 H45A C27A 0.969 1_555 1_555 H46A C27A 0.970 1_555 1_555 C28A C28 1.792 1_555 1_555 C29A C28 1.412 1_555 1_555 H47A C32 0.766 1_555 1_555 C30A C28 0.968 1_555 1_555 H48A C30A 0.940 1_555 1_555 C31A C28 1.054 1_555 1_555 H49A C34 0.717 1_555 1_555 C32A C28 1.528 1_555 1_555 H50A C32A 0.940 1_555 1_555 C33A H47 1.006 1_555 1_555 H51A C30 1.228 1_555 1_555 C34A C30 1.344 1_555 1_555 H52A C31 0.933 1_555 1_555 H53A C31 1.286 1_555 1_555 H54A C34A 0.975 1_555 1_555 C8 C9 1.395 1_555 1_555 C14 C15 1.385 1_555 1_555 C22 C23 1.442 1_555 1_555 C29 C28A 1.412 1_555 1_555 C29 C32A 1.054 1_555 1_555 C30 C28A 0.968 1_555 1_555 C30 C33A 1.049 1_555 1_555 C31 C28A 1.054 1_555 1_555 C31 C34A 0.576 1_555 1_555 C32 C33 1.391 1_555 1_555 C32 C28A 1.528 1_555 1_555 C32 C29A 1.054 1_555 1_555 C33 H47A 1.006 1_555 1_555 C33 C30A 1.049 1_555 1_555 H51 C30A 1.228 1_555 1_555 C34 C30A 1.344 1_555 1_555 C34 C31A 0.576 1_555 1_555 H53 C31A 1.286 1_555 1_555 P1A P2A 2.182 1_555 1_555 C8A C9A 1.395 1_555 1_555 C14A C15A 1.385 1_555 1_555 N1A C1A 1.447 1_555 1_555 C22A C23A 1.442 1_555 1_555 C28A C29A 1.390 1_555 1_555 C28A C33A 1.389 1_555 1_555 C29A H47A 0.940 1_555 1_555 C29A C30A 1.391 1_555 1_555 C31A H49A 0.939 1_555 1_555 C31A C32A 1.390 1_555 1_555 C32A C33A 1.391 1_555 1_555 C33A H51A 0.941 1_555 1_555 C34A H52A 0.969 1_555 1_555 C34A H53A 0.966 1_555 1_555 #END data_CSD_CIF_YEHTOU _audit_creation_date 1995-03-22 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD YEHTOU _chemical_formula_sum 'C36 H54 Li2 O8' _chemical_formula_moiety ; C20 H22 Li1 1-,C16 H32 Li1 O8 1+ ; _journal_coden_Cambridge 4 _journal_volume 116 _journal_year 1994 _journal_page_first 6466 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "F.Zaegel" "J.C.Gallucci" "P.Meunier" "B.Gautheron" "M.R.Sivik" "L.A.Paquette" _chemical_name_systematic ; bis(\h^5^-Isodicyclopentadiene)-lithium bis(12-crown-4)-lithium ; _cell_volume 1703.610 _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.23 _exptl_special_details ; becomes green on exposure to light or air ; _diffrn_ambient_temperature 203 _refine_special_details ; One of the crown molecules is disordered over two positions with occupancy factors of 0.69 and 0.31. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.054 _refine_ls_wR_factor_gt 0.054 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.818(1) _cell_length_b 16.129(2) _cell_length_c 9.871(1) _cell_angle_alpha 107.05(1) _cell_angle_beta 108.23(1) _cell_angle_gamma 88.70(1) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.53 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z O1 O 0.5565(2) 0.1981(1) 0.4620(2) O2 O 0.5289(2) 0.3706(1) 0.4776(2) O3 O 0.3235(2) 0.3212(1) 0.2361(2) O4 O 0.3495(2) 0.1495(1) 0.2224(2) C1 C 0.5619(3) 0.2578(2) 0.6002(3) C2 C 0.6034(3) 0.3438(2) 0.6020(3) C3 C 0.4203(3) 0.4012(2) 0.4956(4) C4 C 0.3429(3) 0.4050(2) 0.3466(4) C5 C 0.2254(3) 0.2690(3) 0.2323(5) C6 C 0.2362(3) 0.1786(3) 0.1595(4) C7 C 0.3605(3) 0.1246(2) 0.3532(4) C8 C 0.4879(3) 0.1179(2) 0.4251(4) O5 O 0.6981(4) 0.2693(3) 0.3098(5) O6 O 0.5636(4) 0.1187(3) 0.1241(6) O7 O 0.4290(5) 0.2350(4) 0.0008(6) O8 O 0.5636(4) 0.3886(3) 0.1870(5) C9 C 0.7475(5) 0.1851(4) 0.2972(6) C10 C 0.6884(6) 0.1236(3) 0.1469(7) C11 C 0.4906(6) 0.0951(3) -0.0296(6) C12 C 0.4766(5) 0.1688(3) -0.0926(5) C13 C 0.4176(5) 0.3143(5) -0.0395(7) C14 C 0.5307(5) 0.3703(3) 0.0285(6) C15 C 0.6910(5) 0.4030(3) 0.2600(7) C16 C 0.7514(4) 0.3216(3) 0.2487(5) O9? O 0.418(1) 0.2045(7) -0.010(2) O10? O 0.5172(8) 0.3716(7) 0.150(1) O11? O 0.701(1) 0.2988(7) 0.316(2) O12? O 0.603(1) 0.1308(8) 0.162(1) C17? C 0.438(1) 0.2595(8) -0.085(1) C18? C 0.432(2) 0.355(1) 0.007(2) C19? C 0.635(1) 0.3906(7) 0.157(1) C20? C 0.714(1) 0.382(1) 0.307(1) C21? C 0.7709(9) 0.2355(7) 0.253(1) C22? C 0.723(1) 0.146(1) 0.240(2) C23? C 0.576(1) 0.1074(6) 0.004(1) C24? C 0.442(1) 0.1170(9) -0.066(1) Li1 Li 0.5005(5) 0.2556(4) 0.2523(6) C25 C 0.0734(2) -0.0013(2) 0.3103(3) C26 C 0.0808(3) 0.0865(2) 0.3961(4) C27 C 0.1637(3) 0.0941(2) 0.5378(3) C28 C 0.2097(3) 0.0130(2) 0.5397(3) C29 C 0.1514(2) -0.0462(2) 0.3978(3) C30 C 0.1524(2) -0.1365(2) 0.2967(3) C31 C 0.2174(3) -0.1281(2) 0.1861(3) C32 C 0.1313(3) -0.0789(2) 0.0884(3) C33 C 0.0264(3) -0.0638(2) 0.1544(3) C34 C 0.0228(3) -0.1500(2) 0.1921(3) Li2 Li 0.00000 0.00000 0.50000 C35 C 0.8699(2) 0.5573(2) 0.1283(3) C36 C 0.8016(2) 0.4954(2) -0.0043(3) C37 C 0.8460(3) 0.4140(2) 0.0011(3) C38 C 0.9383(3) 0.4251(2) 0.1381(4) C39 C 0.9533(2) 0.5146(2) 0.2152(3) C40 C 1.0106(3) 0.5812(2) 0.3652(3) C41 C 0.9154(3) 0.6012(2) 0.4458(3) C42 C 0.8217(3) 0.6469(2) 0.3479(3) C43 C 0.8761(3) 0.6499(2) 0.2248(3) C44 C 1.0093(3) 0.6637(2) 0.3169(3) Li3 Li 1.00000 0.50000 0.00000 H1 H 0.03670 0.13320 0.36350 H2 H 0.18610 0.14770 0.62220 H3 H 0.27040 0.00020 0.62330 H4 H 0.17900 -0.18110 0.34660 H5 H 0.29490 -0.09490 0.24000 H6 H 0.22910 -0.18560 0.12490 H7 H 0.16990 -0.02350 0.09750 H8 H 0.10340 -0.11420 -0.01690 H9 H -0.04880 -0.05040 0.08990 H10 H 0.00850 -0.20150 0.10440 H11 H -0.03550 -0.15260 0.24320 H12 H 0.73590 0.50650 -0.08500 H13 H 0.81720 0.35860 -0.07770 H14 H 0.98320 0.37920 0.17270 H15 H 1.08870 0.56850 0.42440 H16 H 0.87970 0.54750 0.44800 H17 H 0.95000 0.63980 0.54820 H18 H 0.74410 0.61320 0.30390 H19 H 0.81240 0.70570 0.40680 H20 H 0.84540 0.69250 0.17170 H21 H 1.02910 0.71720 0.40130 H22 H 1.06140 0.66250 0.25630 H23 H 0.48250 0.26030 0.61210 H24 H 0.61800 0.24010 0.68170 H25 H 0.68510 0.34120 0.59760 H26 H 0.60280 0.38690 0.69540 H27 H 0.38230 0.36130 0.52950 H28 H 0.43450 0.45920 0.56870 H29 H 0.38150 0.44600 0.31560 H30 H 0.26570 0.42500 0.35430 H31 H 0.22630 0.27610 0.33470 H32 H 0.15010 0.28750 0.17660 H33 H 0.22390 0.17110 0.05360 H34 H 0.17430 0.14310 0.16850 H35 H 0.32920 0.16850 0.42170 H36 H 0.31610 0.06830 0.32530 H37 H 0.51710 0.07230 0.35660 H38 H 0.49800 0.10260 0.51700 H39 H 0.83330 0.19190 0.31330 H40 H 0.73480 0.16190 0.37310 H41 H 0.71870 0.06610 0.14120 H42 H 0.70410 0.14470 0.07040 H43 H 0.52720 0.04910 -0.08780 H44 H 0.41130 0.07320 -0.03770 H45 H 0.42160 0.15100 -0.19540 H46 H 0.55420 0.18980 -0.09140 H47 H 0.39480 0.29980 -0.14860 H48 H 0.35530 0.34630 -0.00510 H49 H 0.51930 0.42470 0.00200 H50 H 0.59340 0.34000 -0.00760 H51 H 0.72410 0.43830 0.21380 H52 H 0.70630 0.43450 0.36610 H53 H 0.83670 0.33450 0.30520 H54 H 0.74140 0.29090 0.14360 H55? H 0.51760 0.25230 -0.09650 H56? H 0.37750 0.24610 -0.18410 H57? H 0.35150 0.36250 0.01600 H58? H 0.44870 0.39480 -0.04350 H59? H 0.65510 0.34920 0.07410 H60? H 0.64530 0.44990 0.15250 H61? H 0.69190 0.42360 0.38700 H62? H 0.79780 0.39520 0.31810 H63? H 0.76560 0.23830 0.15290 H64? H 0.85450 0.24630 0.31690 H65? H 0.73580 0.14200 0.34110 H66? H 0.76560 0.10170 0.18850 H67? H 0.62380 0.14580 -0.02110 H68? H 0.59380 0.04690 -0.03400 H69? H 0.39400 0.07900 -0.03990 H70? H 0.42110 0.10090 -0.17520 C25A C -0.0734(2) 0.0013(2) 0.6897(3) C26A C -0.0808(3) -0.0865(2) 0.6039(4) C27A C -0.1637(3) -0.0941(2) 0.4622(3) C28A C -0.2097(3) -0.0130(2) 0.4603(3) C29A C -0.1514(2) 0.0462(2) 0.6022(3) C33A C -0.0264(3) 0.0638(2) 0.8456(3) H1A H -0.03670 -0.13320 0.63650 H2A H -0.18610 -0.14770 0.37780 H3A H -0.27040 -0.00020 0.37670 C30A C -0.1524(2) 0.1365(2) 0.7033(3) C32A C -0.1313(3) 0.0789(2) 0.9116(3) C34A C -0.0228(3) 0.1500(2) 0.8079(3) H9A H 0.04880 0.05040 0.91010 C31A C -0.2174(3) 0.1281(2) 0.8139(3) H4A H -0.17900 0.18110 0.65340 H7A H -0.16990 0.02350 0.90250 H8A H -0.10340 0.11420 1.01690 H10A H -0.00850 0.20150 0.89560 H11A H 0.03550 0.15260 0.75680 H5A H -0.29490 0.09490 0.76000 H6A H -0.22910 0.18560 0.87510 C35A C 1.1301(2) 0.4427(2) -0.1283(3) C36A C 1.1984(2) 0.5046(2) 0.0043(3) C37A C 1.1540(3) 0.5860(2) -0.0011(3) C38A C 1.0617(3) 0.5749(2) -0.1381(4) C39A C 1.0467(2) 0.4854(2) -0.2152(3) C43A C 1.1239(3) 0.3501(2) -0.2248(3) H12A H 1.26410 0.49350 0.08500 H13A H 1.18280 0.64140 0.07770 H14A H 1.01680 0.62080 -0.17270 C40A C 0.9894(3) 0.4188(2) -0.3652(3) C42A C 1.1783(3) 0.3531(2) -0.3479(3) C44A C 0.9907(3) 0.3363(2) -0.3169(3) H20A H 1.15460 0.30750 -0.17170 C41A C 1.0846(3) 0.3988(2) -0.4458(3) H15A H 0.91130 0.43150 -0.42440 H18A H 1.25590 0.38680 -0.30390 H19A H 1.18760 0.29430 -0.40680 H21A H 0.97090 0.28280 -0.40130 H22A H 0.93860 0.33750 -0.25630 H16A H 1.12030 0.45250 -0.44800 H17A H 1.05000 0.36020 -0.54820 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 O1 C1 1.404 1_555 1_555 O2 C2 1.445 1_555 1_555 O3 C4 1.436 1_555 1_555 O4 C6 1.422 1_555 1_555 C1 C2 1.475 1_555 1_555 C2 H25 0.979 1_555 1_555 C3 O2 1.409 1_555 1_555 C4 C3 1.487 1_555 1_555 C5 O3 1.433 1_555 1_555 C6 C5 1.447 1_555 1_555 C7 O4 1.429 1_555 1_555 C8 O1 1.432 1_555 1_555 O5 C9 1.453 1_555 1_555 O6 C10 1.421 1_555 1_555 O7 C12 1.424 1_555 1_555 O8 C14 1.428 1_555 1_555 C9 C10 1.481 1_555 1_555 C10 H41 0.979 1_555 1_555 C11 O6 1.431 1_555 1_555 C12 C11 1.479 1_555 1_555 C13 O7 1.439 1_555 1_555 C14 C13 1.480 1_555 1_555 C15 O8 1.442 1_555 1_555 C16 O5 1.426 1_555 1_555 Li1 O1 2.413 1_555 1_555 C25 C26 1.409 1_555 1_555 C26 C27 1.407 1_555 1_555 C27 C28 1.408 1_555 1_555 C28 C29 1.411 1_555 1_555 C29 C25 1.399 1_555 1_555 C30 C29 1.507 1_555 1_555 C31 C30 1.555 1_555 1_555 C32 C31 1.547 1_555 1_555 C33 C25 1.508 1_555 1_555 C34 C30 1.534 1_555 1_555 Li2 C25 2.292 1_555 1_555 C35 C36 1.404 1_555 1_555 C36 C37 1.412 1_555 1_555 C37 C38 1.412 1_555 1_555 C38 C39 1.406 1_555 1_555 C39 C35 1.403 1_555 1_555 C40 C39 1.509 1_555 1_555 C41 C40 1.548 1_555 1_555 C42 C41 1.554 1_555 1_555 C43 C35 1.507 1_555 1_555 C44 C40 1.538 1_555 1_555 Li3 C35 2.300 1_555 1_555 H1 C26 0.981 1_555 1_555 H2 C27 0.981 1_555 1_555 H3 C28 0.980 1_555 1_555 H4 C30 0.980 1_555 1_555 H5 C31 0.979 1_555 1_555 H6 C31 0.981 1_555 1_555 H7 C32 0.980 1_555 1_555 H8 C32 0.980 1_555 1_555 H9 C33 0.980 1_555 1_555 H10 C34 0.980 1_555 1_555 H11 C34 0.981 1_555 1_555 H12 C36 0.980 1_555 1_555 H13 C37 0.980 1_555 1_555 H14 C38 0.982 1_555 1_555 H15 C40 0.980 1_555 1_555 H16 C41 0.981 1_555 1_555 H17 C41 0.980 1_555 1_555 H18 C42 0.980 1_555 1_555 H19 C42 0.981 1_555 1_555 H20 C43 0.979 1_555 1_555 H21 C44 0.979 1_555 1_555 H22 C44 0.980 1_555 1_555 H23 C1 0.980 1_555 1_555 H24 C1 0.980 1_555 1_555 H26 C2 0.980 1_555 1_555 H27 C3 0.980 1_555 1_555 H28 C3 0.980 1_555 1_555 H29 C4 0.979 1_555 1_555 H30 C4 0.979 1_555 1_555 H31 C5 0.980 1_555 1_555 H32 C5 0.980 1_555 1_555 H33 C6 0.980 1_555 1_555 H34 C6 0.980 1_555 1_555 H35 C7 0.979 1_555 1_555 H36 C7 0.980 1_555 1_555 H37 C8 0.980 1_555 1_555 H38 C8 0.980 1_555 1_555 H39 C9 0.980 1_555 1_555 H40 C9 0.980 1_555 1_555 H42 C10 0.981 1_555 1_555 H43 C11 0.979 1_555 1_555 H44 C11 0.980 1_555 1_555 H45 C12 0.980 1_555 1_555 H46 C12 0.980 1_555 1_555 H47 C13 0.980 1_555 1_555 H48 C13 0.980 1_555 1_555 H49 C14 0.982 1_555 1_555 H50 C14 0.981 1_555 1_555 H51 C15 0.979 1_555 1_555 H52 C15 0.980 1_555 1_555 H53 C16 0.980 1_555 1_555 H54 C16 0.980 1_555 1_555 C25A Li2 2.292 1_555 1_555 C26A Li2 2.329 1_555 1_555 C27A Li2 2.353 1_555 1_555 C28A Li2 2.389 1_555 1_555 C29A Li2 2.324 1_555 1_555 C33A C25A 1.508 1_555 1_555 H1A C26A 0.981 1_555 1_555 H2A C27A 0.981 1_555 1_555 H3A C28A 0.980 1_555 1_555 C30A C29A 1.507 1_555 1_555 C32A C33A 1.555 1_555 1_555 C34A C33A 1.546 1_555 1_555 H9A C33A 0.980 1_555 1_555 C31A C30A 1.555 1_555 1_555 H4A C30A 0.980 1_555 1_555 H7A C32A 0.980 1_555 1_555 H8A C32A 0.980 1_555 1_555 H10A C34A 0.980 1_555 1_555 H11A C34A 0.981 1_555 1_555 H5A C31A 0.979 1_555 1_555 H6A C31A 0.981 1_555 1_555 C35A Li3 2.300 1_555 1_555 C36A Li3 2.334 1_555 1_555 C37A Li3 2.318 1_555 1_555 C38A Li3 2.340 1_555 1_555 C39A Li3 2.304 1_555 1_555 C43A C35A 1.507 1_555 1_555 H12A C36A 0.980 1_555 1_555 H13A C37A 0.980 1_555 1_555 H14A C38A 0.982 1_555 1_555 C40A C39A 1.509 1_555 1_555 C42A C43A 1.555 1_555 1_555 C44A C43A 1.535 1_555 1_555 H20A C43A 0.979 1_555 1_555 C41A C40A 1.548 1_555 1_555 H15A C40A 0.980 1_555 1_555 H18A C42A 0.980 1_555 1_555 H19A C42A 0.981 1_555 1_555 H21A C44A 0.979 1_555 1_555 H22A C44A 0.980 1_555 1_555 H16A C41A 0.981 1_555 1_555 H17A C41A 0.980 1_555 1_555 O2 Li1 2.375 1_555 1_555 O3 Li1 2.304 1_555 1_555 O4 Li1 2.390 1_555 1_555 C7 C8 1.467 1_555 1_555 O5 Li1 2.224 1_555 1_555 O6 Li1 2.431 1_555 1_555 O7 Li1 2.281 1_555 1_555 O8 Li1 2.600 1_555 1_555 C15 C16 1.472 1_555 1_555 C26 Li2 2.329 1_555 1_555 C27 Li2 2.353 1_555 1_555 C28 Li2 2.389 1_555 1_555 C29 Li2 2.324 1_555 1_555 C32 C33 1.555 1_555 1_555 C33 C34 1.546 1_555 1_555 C36 Li3 2.334 1_555 1_555 C37 Li3 2.318 1_555 1_555 C38 Li3 2.340 1_555 1_555 C39 Li3 2.304 1_555 1_555 C42 C43 1.555 1_555 1_555 C43 C44 1.535 1_555 1_555 C25A C26A 1.409 1_555 1_555 C25A C29A 1.399 1_555 1_555 C26A C27A 1.407 1_555 1_555 C27A C28A 1.408 1_555 1_555 C28A C29A 1.411 1_555 1_555 C30A C34A 1.534 1_555 1_555 C32A C31A 1.547 1_555 1_555 C35A C36A 1.404 1_555 1_555 C35A C39A 1.403 1_555 1_555 C36A C37A 1.412 1_555 1_555 C37A C38A 1.412 1_555 1_555 C38A C39A 1.406 1_555 1_555 C40A C44A 1.538 1_555 1_555 C42A C41A 1.554 1_555 1_555 #END data_CSD_CIF_YEHTOU10 _audit_creation_date 1996-09-23 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD YEHTOU10 _database_code_depnum_ccdc_archive 'CCDC 126911' _chemical_formula_sum 'C36 H54 Li2 O8' _chemical_formula_moiety ; C20 H22 Li1 1-,C16 H32 Li1 O8 1+ ; _journal_coeditor_code "IUCr BK1216" _journal_coden_Cambridge 591 _journal_volume 52 _journal_year 1996 _journal_page_first 1673 _journal_name_full 'Acta Crystallogr.,Sect.C:Cryst.Struct.Commun. ' loop_ _publ_author_name "J.C.Gallucci" "M.R.Sivik" "L.A.Paquette" "F.Zaegel" "P.Meunier" "B.Gautheron" _chemical_name_systematic ; bis(1,4,7,10-Tetraoxacyclododecane)-lithium bis((1,2,3,3a,7a-\h^5^)-4,5,6,7-tetrahydro-4,7-methanoindenido)-lithium ; _cell_volume 1703.610 _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.225 _diffrn_ambient_temperature 203 _refine_special_details ; One of the crown ether molecules is disordered over two orientations with occupancies 0.69:0.31. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.054 _refine_ls_wR_factor_gt 0.054 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.818(1) _cell_length_b 16.129(2) _cell_length_c 9.871(1) _cell_angle_alpha 107.05(1) _cell_angle_beta 108.23(1) _cell_angle_gamma 88.70(1) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.53 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z O1 O 0.5565(2) 0.1981(1) 0.4620(2) O2 O 0.5289(2) 0.3706(1) 0.4776(2) O3 O 0.3235(2) 0.3212(1) 0.2361(2) O4 O 0.3495(2) 0.1495(1) 0.2224(2) C1 C 0.5619(3) 0.2578(2) 0.6002(3) C2 C 0.6034(3) 0.3438(2) 0.6020(3) C3 C 0.4203(3) 0.4012(2) 0.4956(4) C4 C 0.3429(3) 0.4050(2) 0.3466(4) C5 C 0.2254(3) 0.2690(3) 0.2323(5) C6 C 0.2362(3) 0.1786(3) 0.1595(4) C7 C 0.3605(3) 0.1246(2) 0.3532(4) C8 C 0.4879(3) 0.1179(2) 0.4251(4) O5 O 0.6981(4) 0.2693(3) 0.3098(5) O6 O 0.5636(4) 0.1187(3) 0.1241(5) O7 O 0.4290(5) 0.2350(4) 0.0008(6) O8 O 0.5636(4) 0.3887(3) 0.1870(5) C9 C 0.7475(5) 0.1851(4) 0.2972(6) C10 C 0.6884(6) 0.1236(3) 0.1469(7) C11 C 0.4906(6) 0.0951(3) -0.0296(6) C12 C 0.4766(5) 0.1688(3) -0.0926(5) C13 C 0.4176(5) 0.3143(5) -0.0395(7) C14 C 0.5307(5) 0.3703(3) 0.0285(6) C15 C 0.6910(5) 0.4030(3) 0.2600(7) C16 C 0.7514(4) 0.3216(3) 0.2487(5) O9? O 0.418(1) 0.2045(7) -0.010(2) O10? O 0.5172(8) 0.3716(7) 0.150(1) O11? O 0.701(1) 0.2988(7) 0.316(2) O12? O 0.603(1) 0.1308(8) 0.162(1) C17? C 0.438(1) 0.2595(8) -0.085(1) C18? C 0.432(2) 0.3547(10) 0.007(2) C19? C 0.635(1) 0.3906(7) 0.157(1) C20? C 0.714(1) 0.3821(9) 0.307(1) C21? C 0.7709(9) 0.2355(7) 0.253(1) C22? C 0.723(1) 0.146(1) 0.240(2) C23? C 0.576(1) 0.1074(6) 0.004(1) C24? C 0.442(1) 0.1170(9) -0.066(1) Li1 Li 0.5005(5) 0.2556(4) 0.2523(6) C25 C 0.0734(2) -0.0013(2) 0.3103(3) C26 C 0.0808(3) 0.0865(2) 0.3961(3) C27 C 0.1637(3) 0.0941(2) 0.5378(3) C28 C 0.2097(3) 0.0130(2) 0.5397(3) C29 C 0.1514(2) -0.0462(2) 0.3978(3) C30 C 0.1524(3) -0.1365(2) 0.2967(3) C31 C 0.2174(3) -0.1281(2) 0.1861(3) C32 C 0.1313(3) -0.0789(2) 0.0884(3) C33 C 0.0264(3) -0.0638(2) 0.1544(3) C34 C 0.0228(3) -0.1500(2) 0.1921(3) Li2 Li 0.00000 0.00000 0.50000 C35 C 0.8699(2) 0.5573(2) 0.1283(3) C36 C 0.8016(2) 0.4954(2) -0.0043(3) C37 C 0.8460(3) 0.4140(2) 0.0011(3) C38 C 0.9383(3) 0.4251(2) 0.1381(4) C39 C 0.9533(2) 0.5146(2) 0.2152(3) C40 C 1.0106(3) 0.5812(2) 0.3652(3) C41 C 0.9154(3) 0.6012(2) 0.4458(3) C42 C 0.8217(3) 0.6469(2) 0.3479(3) C43 C 0.8761(3) 0.6499(2) 0.2248(3) C44 C 1.0093(3) 0.6637(2) 0.3169(3) Li3 Li 1.00000 0.50000 0.00000 H1 H 0.03670 0.13320 0.36350 H2 H 0.18610 0.14770 0.62220 H3 H 0.27040 0.00020 0.62330 H4 H 0.17900 -0.18110 0.34660 H5 H 0.29490 -0.09490 0.24000 H6 H 0.22910 -0.18560 0.12490 H7 H 0.16990 -0.02350 0.09750 H8 H 0.10340 -0.11420 -0.01690 H9 H -0.04880 -0.05040 0.08990 H10 H 0.00850 -0.20150 0.10440 H11 H -0.03550 -0.15260 0.24320 H12 H 0.73590 0.50650 -0.08500 H13 H 0.81720 0.35860 -0.07770 H14 H 0.98320 0.37920 0.17270 H15 H 1.08870 0.56850 0.42440 H16 H 0.87970 0.54750 0.44800 H17 H 0.95000 0.63980 0.54820 H18 H 0.74410 0.61320 0.30390 H19 H 0.81240 0.70570 0.40680 H20 H 0.84540 0.69250 0.17170 H21 H 1.02910 0.71720 0.40130 H22 H 1.06140 0.66250 0.25630 H23 H 0.48250 0.26030 0.61210 H24 H 0.61800 0.24010 0.68170 H25 H 0.68510 0.34120 0.59760 H26 H 0.60280 0.38680 0.69540 H27 H 0.38230 0.36130 0.52950 H28 H 0.43450 0.45920 0.56870 H29 H 0.38150 0.44600 0.31560 H30 H 0.26570 0.42500 0.35430 H31 H 0.22630 0.27610 0.33470 H32 H 0.15010 0.28750 0.17660 H33 H 0.22390 0.17110 0.05360 H34 H 0.17430 0.14310 0.16850 H35 H 0.32920 0.16850 0.42170 H36 H 0.31610 0.06830 0.32530 H37 H 0.51710 0.07230 0.35660 H38 H 0.49800 0.10260 0.51700 H39 H 0.83330 0.19190 0.31330 H40 H 0.73480 0.16190 0.37310 H41 H 0.71870 0.06610 0.14120 H42 H 0.70410 0.14470 0.07040 H43 H 0.52720 0.04910 -0.08780 H44 H 0.41130 0.07320 -0.03770 H45 H 0.42160 0.15100 -0.19540 H46 H 0.55420 0.18980 -0.09140 H47 H 0.39480 0.29980 -0.14860 H48 H 0.35530 0.34630 -0.00510 H49 H 0.51930 0.42470 0.00200 H50 H 0.59340 0.34000 -0.00760 H51 H 0.72410 0.43830 0.21380 H52 H 0.70630 0.43450 0.36610 H53 H 0.83670 0.33450 0.30520 H54 H 0.74140 0.29090 0.14360 H55? H 0.51760 0.25230 -0.09650 H56? H 0.37750 0.24610 -0.18410 H57? H 0.35150 0.36250 0.01600 H58? H 0.44870 0.39480 -0.04350 H59? H 0.65510 0.34920 0.07410 H60? H 0.64530 0.44990 0.15250 H61? H 0.69190 0.42360 0.38700 H62? H 0.79780 0.39520 0.31810 H63? H 0.76560 0.23830 0.15290 H64? H 0.85450 0.24630 0.31690 H65? H 0.73580 0.14200 0.34110 H66? H 0.76560 0.10170 0.18850 H67? H 0.62380 0.14580 -0.02110 H68? H 0.59380 0.04690 -0.03400 H69? H 0.39400 0.07900 -0.03990 H70? H 0.42110 0.10090 -0.17520 C25A C -0.0734(2) 0.0013(2) 0.6897(3) C26A C -0.0808(3) -0.0865(2) 0.6039(3) C27A C -0.1637(3) -0.0941(2) 0.4622(3) C28A C -0.2097(3) -0.0130(2) 0.4603(3) C29A C -0.1514(2) 0.0462(2) 0.6022(3) C33A C -0.0264(3) 0.0638(2) 0.8456(3) C32A C -0.1313(3) 0.0789(2) 0.9116(3) C31A C -0.2174(3) 0.1281(2) 0.8139(3) C30A C -0.1524(3) 0.1365(2) 0.7033(3) H1A H -0.03670 -0.13320 0.63650 H2A H -0.18610 -0.14770 0.37780 H3A H -0.27040 -0.00020 0.37670 C34A C -0.0228(3) 0.1500(2) 0.8079(3) H9A H 0.04880 0.05040 0.91010 H10A H -0.00850 0.20150 0.89560 H11A H 0.03550 0.15260 0.75680 H4A H -0.17900 0.18110 0.65340 H5A H -0.29490 0.09490 0.76000 H6A H -0.22910 0.18560 0.87510 H7A H -0.16990 0.02350 0.90250 H8A H -0.10340 0.11420 1.01690 C35A C 1.1301(2) 0.4427(2) -0.1283(3) C36A C 1.1984(2) 0.5046(2) 0.0043(3) C37A C 1.1540(3) 0.5860(2) -0.0011(3) C38A C 1.0617(3) 0.5749(2) -0.1381(4) C39A C 1.0467(2) 0.4854(2) -0.2152(3) C43A C 1.1239(3) 0.3501(2) -0.2248(3) C42A C 1.1783(3) 0.3531(2) -0.3479(3) C41A C 1.0846(3) 0.3988(2) -0.4458(3) C40A C 0.9894(3) 0.4188(2) -0.3652(3) H12A H 1.26410 0.49350 0.08500 H13A H 1.18280 0.64140 0.07770 H14A H 1.01680 0.62080 -0.17270 C44A C 0.9907(3) 0.3363(2) -0.3169(3) H20A H 1.15460 0.30750 -0.17170 H21A H 0.97090 0.28280 -0.40130 H22A H 0.93860 0.33750 -0.25630 H15A H 0.91130 0.43150 -0.42440 H16A H 1.12030 0.45250 -0.44800 H17A H 1.05000 0.36020 -0.54820 H18A H 1.25590 0.38680 -0.30390 H19A H 1.18760 0.29430 -0.40680 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 O1 C1 1.404 1_555 1_555 O2 C2 1.445 1_555 1_555 O3 C4 1.436 1_555 1_555 O4 C6 1.422 1_555 1_555 C1 C2 1.475 1_555 1_555 C2 H25 0.979 1_555 1_555 C3 O2 1.409 1_555 1_555 C4 C3 1.487 1_555 1_555 C5 O3 1.433 1_555 1_555 C6 C5 1.447 1_555 1_555 C7 O4 1.429 1_555 1_555 C8 O1 1.432 1_555 1_555 O5 C9 1.453 1_555 1_555 O6 C10 1.421 1_555 1_555 O7 C12 1.424 1_555 1_555 O8 C14 1.428 1_555 1_555 C9 C10 1.481 1_555 1_555 C10 H41 0.979 1_555 1_555 C11 O6 1.431 1_555 1_555 C12 C11 1.479 1_555 1_555 C13 O7 1.439 1_555 1_555 C14 C13 1.480 1_555 1_555 C15 O8 1.442 1_555 1_555 C16 O5 1.426 1_555 1_555 Li1 O1 2.413 1_555 1_555 C25 C26 1.409 1_555 1_555 C26 C27 1.407 1_555 1_555 C27 C28 1.408 1_555 1_555 C28 C29 1.411 1_555 1_555 C29 C25 1.399 1_555 1_555 C30 C29 1.507 1_555 1_555 C31 C30 1.555 1_555 1_555 C32 C31 1.547 1_555 1_555 C33 C25 1.508 1_555 1_555 C34 C30 1.534 1_555 1_555 Li2 C25 2.292 1_555 1_555 C35 C36 1.404 1_555 1_555 C36 C37 1.412 1_555 1_555 C37 C38 1.412 1_555 1_555 C38 C39 1.406 1_555 1_555 C39 C35 1.403 1_555 1_555 C40 C39 1.509 1_555 1_555 C41 C40 1.548 1_555 1_555 C42 C41 1.554 1_555 1_555 C43 C35 1.507 1_555 1_555 C44 C40 1.538 1_555 1_555 Li3 C35 2.300 1_555 1_555 H1 C26 0.981 1_555 1_555 H2 C27 0.981 1_555 1_555 H3 C28 0.980 1_555 1_555 H4 C30 0.980 1_555 1_555 H5 C31 0.979 1_555 1_555 H6 C31 0.981 1_555 1_555 H7 C32 0.980 1_555 1_555 H8 C32 0.980 1_555 1_555 H9 C33 0.980 1_555 1_555 H10 C34 0.980 1_555 1_555 H11 C34 0.981 1_555 1_555 H12 C36 0.980 1_555 1_555 H13 C37 0.980 1_555 1_555 H14 C38 0.982 1_555 1_555 H15 C40 0.980 1_555 1_555 H16 C41 0.981 1_555 1_555 H17 C41 0.980 1_555 1_555 H18 C42 0.980 1_555 1_555 H19 C42 0.981 1_555 1_555 H20 C43 0.979 1_555 1_555 H21 C44 0.979 1_555 1_555 H22 C44 0.980 1_555 1_555 H23 C1 0.980 1_555 1_555 H24 C1 0.980 1_555 1_555 H26 C2 0.980 1_555 1_555 H27 C3 0.980 1_555 1_555 H28 C3 0.980 1_555 1_555 H29 C4 0.979 1_555 1_555 H30 C4 0.979 1_555 1_555 H31 C5 0.980 1_555 1_555 H32 C5 0.980 1_555 1_555 H33 C6 0.980 1_555 1_555 H34 C6 0.980 1_555 1_555 H35 C7 0.979 1_555 1_555 H36 C7 0.980 1_555 1_555 H37 C8 0.980 1_555 1_555 H38 C8 0.980 1_555 1_555 H39 C9 0.980 1_555 1_555 H40 C9 0.980 1_555 1_555 H42 C10 0.981 1_555 1_555 H43 C11 0.979 1_555 1_555 H44 C11 0.980 1_555 1_555 H45 C12 0.980 1_555 1_555 H46 C12 0.980 1_555 1_555 H47 C13 0.980 1_555 1_555 H48 C13 0.980 1_555 1_555 H49 C14 0.982 1_555 1_555 H50 C14 0.981 1_555 1_555 H51 C15 0.979 1_555 1_555 H52 C15 0.980 1_555 1_555 H53 C16 0.980 1_555 1_555 H54 C16 0.980 1_555 1_555 C25A Li2 2.292 1_555 1_555 C26A Li2 2.329 1_555 1_555 C27A Li2 2.353 1_555 1_555 C28A Li2 2.389 1_555 1_555 C29A Li2 2.324 1_555 1_555 C33A C25A 1.508 1_555 1_555 C32A C33A 1.555 1_555 1_555 C31A C32A 1.547 1_555 1_555 C30A C29A 1.507 1_555 1_555 H1A C26A 0.981 1_555 1_555 H2A C27A 0.981 1_555 1_555 H3A C28A 0.980 1_555 1_555 C34A C33A 1.546 1_555 1_555 H9A C33A 0.980 1_555 1_555 H10A C34A 0.980 1_555 1_555 H11A C34A 0.981 1_555 1_555 H4A C30A 0.980 1_555 1_555 H5A C31A 0.979 1_555 1_555 H6A C31A 0.981 1_555 1_555 H7A C32A 0.980 1_555 1_555 H8A C32A 0.980 1_555 1_555 C35A Li3 2.300 1_555 1_555 C36A Li3 2.334 1_555 1_555 C37A Li3 2.318 1_555 1_555 C38A Li3 2.340 1_555 1_555 C39A Li3 2.304 1_555 1_555 C43A C35A 1.507 1_555 1_555 C42A C43A 1.555 1_555 1_555 C41A C42A 1.554 1_555 1_555 C40A C39A 1.509 1_555 1_555 H12A C36A 0.980 1_555 1_555 H13A C37A 0.980 1_555 1_555 H14A C38A 0.982 1_555 1_555 C44A C43A 1.535 1_555 1_555 H20A C43A 0.979 1_555 1_555 H21A C44A 0.979 1_555 1_555 H22A C44A 0.980 1_555 1_555 H15A C40A 0.980 1_555 1_555 H16A C41A 0.981 1_555 1_555 H17A C41A 0.980 1_555 1_555 H18A C42A 0.980 1_555 1_555 H19A C42A 0.981 1_555 1_555 O2 Li1 2.375 1_555 1_555 O3 Li1 2.304 1_555 1_555 O4 Li1 2.390 1_555 1_555 C7 C8 1.467 1_555 1_555 O5 Li1 2.224 1_555 1_555 O6 Li1 2.431 1_555 1_555 O7 Li1 2.281 1_555 1_555 O8 Li1 2.601 1_555 1_555 C15 C16 1.472 1_555 1_555 C26 Li2 2.329 1_555 1_555 C27 Li2 2.353 1_555 1_555 C28 Li2 2.389 1_555 1_555 C29 Li2 2.324 1_555 1_555 C32 C33 1.555 1_555 1_555 C33 C34 1.546 1_555 1_555 C36 Li3 2.334 1_555 1_555 C37 Li3 2.318 1_555 1_555 C38 Li3 2.340 1_555 1_555 C39 Li3 2.304 1_555 1_555 C42 C43 1.555 1_555 1_555 C43 C44 1.535 1_555 1_555 C25A C26A 1.409 1_555 1_555 C25A C29A 1.399 1_555 1_555 C26A C27A 1.407 1_555 1_555 C27A C28A 1.408 1_555 1_555 C28A C29A 1.411 1_555 1_555 C31A C30A 1.555 1_555 1_555 C30A C34A 1.534 1_555 1_555 C35A C36A 1.404 1_555 1_555 C35A C39A 1.403 1_555 1_555 C36A C37A 1.412 1_555 1_555 C37A C38A 1.412 1_555 1_555 C38A C39A 1.406 1_555 1_555 C41A C40A 1.548 1_555 1_555 C40A C44A 1.538 1_555 1_555 #END data_CSD_CIF_YOSTUV10 _audit_creation_date 1996-10-31 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD YOSTUV10 _chemical_formula_sum 'C43 H111 B8 Cl2 Er1 Li3 N8 Si4' _chemical_formula_moiety ; C28 H76 B8 Cl2 Er1 Li2 N4 Si4 1-,C12 H32 Li1 N4 1+,0.5(C6 H6) ; _journal_coden_Cambridge 579 _journal_volume 15 _journal_year 1996 _journal_page_first 1006 _journal_name_full 'Organometallics ' loop_ _publ_author_name "N.S.Hosmane" "Ying Wang" "Hongming Zhang" "J.A.Maguire" "M.McInnis" "T.G.Gray" "J.D.Collins" "R.K.Kremer" "H.Binder" "E.Waldhor" "W.Kaim" _chemical_name_systematic ; bis(Tetramethylethylenediamine)-lithium 1-chloro-1-(\m~2~-chloro)-2,2',3,3'-tetrakis(trimethylsilyl)-5,6-(bis(\m~2~-hy drido)-tetramethylethylenediamine-lithium)-4,4',5'-(tris(\m~2~-hydrido)-(tetra methylethylenediamine)-lithium)-1,1'-commo-erbium(iii)-bis(2,3-dicarbahexabora ne) benzene solvate ; _cell_volume 6979.635 _exptl_crystal_density_diffrn 1.14 _exptl_special_details ; Air-sensitive ; _diffrn_ambient_temperature 230 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.056 _refine_ls_wR_factor_gt 0.056 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_Int_Tables_number 18 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,z 3 1/2+x,1/2-y,-z 4 1/2-x,1/2+y,-z _cell_length_a 21.051(6) _cell_length_b 23.435(6) _cell_length_c 14.148(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.72 H 0.23 B 0.83 Cl 0.99 Er 1.73 Li 1.44 N 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Er1 Er 0.7308(1) 0.3550(1) 0.2452(1) Cl1 Cl 0.7692(3) 0.4589(2) 0.2663(4) Cl2 Cl 0.8451(3) 0.3078(2) 0.2238(5) Si1 Si 0.8011(4) 0.3945(4) 0.5110(6) Si2 Si 0.6236(4) 0.4284(3) 0.4724(6) Si3 Si 0.7884(4) 0.3954(4) -0.0246(6) Si4 Si 0.6417(4) 0.4723(4) 0.0693(6) C1 C 0.7407(11) 0.359(1) 0.4329(14) C2 C 0.6707(10) 0.3729(9) 0.4123(14) B1 B 0.6399(13) 0.3201(11) 0.3688(16) B2 B 0.6934(12) 0.271(1) 0.3590(17) B3 B 0.7569(13) 0.2988(10) 0.4044(16) B4 B 0.6815(12) 0.3106(11) 0.4703(19) C3 C 0.7278(12) 0.3667(10) 0.0565(14) C4 C 0.6722(10) 0.3993(10) 0.0933(15) B5 B 0.6224(13) 0.3572(12) 0.1434(18) B6 B 0.6533(13) 0.2932(12) 0.1274(17) B7 B 0.7215(14) 0.3014(12) 0.0730(18) B8 B 0.6566(12) 0.3428(10) 0.0354(19) C5 C 0.7879(11) 0.4753(10) 0.5418(19) C6 C 0.8789(11) 0.3873(10) 0.4538(18) C7 C 0.8054(14) 0.3547(12) 0.6292(15) C8 C 0.6389(13) 0.5027(10) 0.4288(21) C9 C 0.6257(19) 0.4254(13) 0.5983(26) C10 C 0.5401(11) 0.4154(10) 0.4472(26) C11 C 0.8431(14) 0.4451(12) 0.0364(19) C12 C 0.7544(12) 0.4282(14) -0.1308(18) C13 C 0.8388(13) 0.3379(12) -0.0612(19) C14 C 0.7006(12) 0.5299(9) 0.0548(18) C15 C 0.5865(16) 0.4733(14) -0.0400(2) C16 C 0.5939(14) 0.4961(11) 0.1621(23) Li1 Li 0.5695(18) 0.2767(16) 0.2504(47) N1 N 0.4709(9) 0.2957(10) 0.2082(18) N2 N 0.5329(9) 0.2009(9) 0.2950(14) C17 C 0.4357(9) 0.2506(9) 0.2515(29) C18 C 0.4716(10) 0.1974(10) 0.2557(27) C19 C 0.4452(10) 0.3517(11) 0.2502(28) C20 C 0.4681(13) 0.2954(17) 0.1034(17) C21 C 0.5693(12) 0.1512(10) 0.2748(23) C22 C 0.5294(15) 0.2028(12) 0.3971(21) Li2 Li 0.7995(15) 0.2247(13) 0.3009(22) N3 N 0.7990(8) 0.1561(5) 0.2062(11) N4 N 0.8437(9) 0.1701(7) 0.4047(13) C23 C 0.8200(12) 0.1052(8) 0.2610(16) C24 C 0.8652(12) 0.1209(10) 0.3462(13) C25 C 0.7363(9) 0.1439(9) 0.1618(17) C26 C 0.8464(10) 0.1684(10) 0.1306(16) C27 C 0.7931(12) 0.1505(10) 0.471(2) C28 C 0.8985(12) 0.1923(12) 0.4603(22) Li3 Li 0.1060(8) 0.3347(7) 0.2060(13) N5 N 0.1997(9) 0.3119(9) 0.2155(16) N6 N 0.0725(10) 0.2602(8) 0.2633(18) C29 C 0.1832(13) 0.2501(11) 0.2176(27) C30 C 0.1355(9) 0.244(2) 0.3032(24) C31 C 0.2366(14) 0.3243(11) 0.1279(16) C32 C 0.2393(22) 0.3260(19) 0.2996(17) C33 C 0.0233(13) 0.2553(15) 0.3385(23) C34 C 0.0564(19) 0.2208(20) 0.1843(25) N7 N 0.0648(10) 0.3750(8) 0.0932(12) N8 N 0.0755(15) 0.4046(9) 0.2800(18) C35 C 0.0391(12) 0.4314(10) 0.1233(18) C36 C 0.0833(16) 0.4503(11) 0.2078(16) C37 C 0.1149(14) 0.3841(14) 0.0202(25) C38 C 0.0125(14) 0.3402(14) 0.0518(30) C39 C 0.0096(16) 0.4066(18) 0.3182(22) C40 C 0.1214(19) 0.4144(21) 0.3586(29) C41 C 0.5243(15) -0.0078(18) 0.1477(21) C42 C 0.5630(13) -0.0162(12) 0.2285(16) C43 C 0.5390(15) -0.0125(16) 0.3219(21) H1 H 0.58880 0.31740 0.34790 H2 H 0.68690 0.22780 0.32750 H3 H 0.80380 0.27650 0.41420 H4 H 0.66510 0.29620 0.54140 H5 H 0.57670 0.36790 0.18020 H6 H 0.63130 0.25260 0.15030 H7 H 0.75610 0.26770 0.05160 H8 H 0.63060 0.33920 -0.03380 H9 H 0.78550 0.49700 0.48440 H10 H 0.74900 0.47950 0.57650 H11 H 0.82270 0.48890 0.57950 H12 H 0.88620 0.34800 0.43830 H13 H 0.87960 0.40980 0.39700 H14 H 0.91160 0.40030 0.49590 H15 H 0.81190 0.31480 0.61800 H16 H 0.84000 0.36950 0.66600 H17 H 0.76630 0.36010 0.66300 H18 H 0.61280 0.52900 0.46330 H19 H 0.68280 0.51200 0.43810 H20 H 0.62890 0.50490 0.36270 H21 H 0.61770 0.38700 0.61900 H22 H 0.66670 0.43740 0.62030 H23 H 0.59360 0.45020 0.62340 H24 H 0.52860 0.37780 0.46770 H25 H 0.51460 0.44300 0.48000 H26 H 0.53290 0.41880 0.38040 H27 H 0.87390 0.45920 -0.00780 H28 H 0.81940 0.47650 0.06210 H29 H 0.86440 0.42530 0.08670 H30 H 0.72620 0.40160 -0.16090 H31 H 0.73120 0.46190 -0.11330 H32 H 0.78790 0.43830 -0.17370 H33 H 0.81390 0.30980 -0.09390 H34 H 0.87120 0.35230 -0.10260 H35 H 0.85830 0.32080 -0.00680 H36 H 0.72860 0.53010 0.10840 H37 H 0.72470 0.52350 -0.00180 H38 H 0.67920 0.56590 0.05050 H39 H 0.57150 0.51150 -0.05070 H40 H 0.60950 0.46040 -0.09460 H41 H 0.55090 0.44850 -0.02900 H42 H 0.61810 0.49690 0.21960 H43 H 0.57860 0.53380 0.14830 H44 H 0.55840 0.47070 0.16950 H45 H 0.39720 0.24430 0.21650 H46 H 0.42410 0.26170 0.31450 H47 H 0.44750 0.17020 0.29160 H48 H 0.47540 0.18280 0.19260 H49 H 0.40240 0.35740 0.22910 H50 H 0.44600 0.34980 0.31790 H51 H 0.47120 0.38300 0.22940 H52 H 0.42540 0.30350 0.08340 H53 H 0.49630 0.32380 0.07850 H54 H 0.48040 0.25840 0.08040 H55 H 0.54770 0.11820 0.29880 H56 H 0.57440 0.14760 0.20760 H57 H 0.61030 0.15420 0.30400 H58 H 0.51230 0.16750 0.42030 H59 H 0.57120 0.20840 0.42260 H60 H 0.50250 0.23380 0.41600 H61 H 0.84180 0.07950 0.21930 H62 H 0.78330 0.08580 0.28510 H63 H 0.86920 0.08800 0.38640 H64 H 0.90660 0.12940 0.32150 H65 H 0.74020 0.11210 0.11950 H66 H 0.70590 0.13500 0.21030 H67 H 0.72220 0.17690 0.12730 H68 H 0.84690 0.13730 0.08630 H69 H 0.83500 0.20300 0.09850 H70 H 0.88780 0.17260 0.15820 H71 H 0.81160 0.12600 0.51800 H72 H 0.77410 0.18300 0.50120 H73 H 0.76120 0.12990 0.43650 H74 H 0.91320 0.16340 0.50320 H75 H 0.93220 0.20260 0.41800 H76 H 0.88530 0.22530 0.49550 C41A C 0.4757(15) 0.0078(18) 0.1477(21) C42A C 0.4370(13) 0.0162(12) 0.2285(16) C43A C 0.4610(15) 0.0125(16) 0.3219(21) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Er1 Cl1 2.583 1_555 1_555 Cl2 Er1 2.665 1_555 1_555 Si1 C1 1.879 1_555 1_555 Si2 C2 1.843 1_555 1_555 Si3 C3 1.843 1_555 1_555 Si4 C4 1.859 1_555 1_555 C1 Er1 2.665 1_555 1_555 C2 Er1 2.714 1_555 1_555 B1 Er1 2.718 1_555 1_555 B2 Er1 2.662 1_555 1_555 B3 Er1 2.666 1_555 1_555 B4 C1 1.766 1_555 1_555 C3 Er1 2.685 1_555 1_555 C4 Er1 2.687 1_555 1_555 B5 Er1 2.699 1_555 1_555 B6 Er1 2.745 1_555 1_555 B7 Er1 2.748 1_555 1_555 B8 C3 1.628 1_555 1_555 C5 Si1 1.963 1_555 1_555 C6 Si1 1.835 1_555 1_555 C7 Si1 1.917 1_555 1_555 C8 Si2 1.875 1_555 1_555 C9 Si2 1.783 1_555 1_555 C10 Si2 1.819 1_555 1_555 C11 Si3 1.851 1_555 1_555 C12 Si3 1.833 1_555 1_555 C13 Si3 1.792 1_555 1_555 C14 Si4 1.844 1_555 1_555 C15 Si4 1.934 1_555 1_555 C16 Si4 1.746 1_555 1_555 Li1 B1 2.457 1_555 1_555 N1 Li1 2.205 1_555 1_555 N2 Li1 2.036 1_555 1_555 C17 N1 1.429 1_555 1_555 C18 N2 1.408 1_555 1_555 C19 N1 1.539 1_555 1_555 C20 N1 1.484 1_555 1_555 C21 N2 1.423 1_555 1_555 C22 N2 1.447 1_555 1_555 Li2 Cl2 2.430 1_555 1_555 N3 Li2 2.093 1_555 1_555 N4 Li2 2.159 1_555 1_555 C23 N3 1.490 1_555 1_555 C24 N4 1.490 1_555 1_555 C25 N3 1.489 1_555 1_555 C26 N3 1.491 1_555 1_555 C27 N4 1.492 1_555 1_555 C28 N4 1.490 1_555 1_555 Li3 N5 2.048 1_555 1_555 N5 C29 1.490 1_555 1_555 N6 Li3 2.050 1_555 1_555 C29 C30 1.580 1_555 1_555 C30 N6 1.491 1_555 1_555 C31 N5 1.491 1_555 1_555 C32 N5 1.490 1_555 1_555 C33 N6 1.489 1_555 1_555 C34 N6 1.489 1_555 1_555 N7 Li3 2.047 1_555 1_555 N8 Li3 2.047 1_555 1_555 C35 N7 1.490 1_555 1_555 C36 N8 1.489 1_555 1_555 C37 N7 1.491 1_555 1_555 C38 N7 1.490 1_555 1_555 C39 N8 1.490 1_555 1_555 C40 N8 1.491 1_555 1_555 C41 C42 1.417 1_555 1_555 C42 C43 1.417 1_555 1_555 C43 C43A 1.743 1_555 1_555 H1 B1 1.117 1_555 1_555 H2 B2 1.115 1_555 1_555 H3 B3 1.126 1_555 1_555 H4 B4 1.116 1_555 1_555 H5 B5 1.122 1_555 1_555 H6 B6 1.107 1_555 1_555 H7 B7 1.116 1_555 1_555 H8 B8 1.125 1_555 1_555 H9 C5 0.960 1_555 1_555 H10 C5 0.960 1_555 1_555 H11 C5 0.961 1_555 1_555 H12 C6 0.959 1_555 1_555 H13 C6 0.961 1_555 1_555 H14 C6 0.960 1_555 1_555 H15 C7 0.958 1_555 1_555 H16 C7 0.960 1_555 1_555 H17 C7 0.960 1_555 1_555 H18 C8 0.959 1_555 1_555 H19 C8 0.959 1_555 1_555 H20 C8 0.960 1_555 1_555 H21 C9 0.961 1_555 1_555 H22 C9 0.960 1_555 1_555 H23 C9 0.959 1_555 1_555 H24 C10 0.959 1_555 1_555 H25 C10 0.960 1_555 1_555 H26 C10 0.960 1_555 1_555 H27 C11 0.959 1_555 1_555 H28 C11 0.961 1_555 1_555 H29 C11 0.961 1_555 1_555 H30 C12 0.960 1_555 1_555 H31 C12 0.961 1_555 1_555 H32 C12 0.960 1_555 1_555 H33 C13 0.960 1_555 1_555 H34 C13 0.960 1_555 1_555 H35 C13 0.960 1_555 1_555 H36 C14 0.960 1_555 1_555 H37 C14 0.960 1_555 1_555 H38 C14 0.958 1_555 1_555 H39 C15 0.961 1_555 1_555 H40 C15 0.960 1_555 1_555 H41 C15 0.961 1_555 1_555 H42 C16 0.960 1_555 1_555 H43 C16 0.960 1_555 1_555 H44 C16 0.961 1_555 1_555 H45 C17 0.961 1_555 1_555 H46 C17 0.960 1_555 1_555 H47 C18 0.960 1_555 1_555 H48 C18 0.959 1_555 1_555 H49 C19 0.959 1_555 1_555 H50 C19 0.959 1_555 1_555 H51 C19 0.961 1_555 1_555 H52 C20 0.961 1_555 1_555 H53 C20 0.959 1_555 1_555 H54 C20 0.962 1_555 1_555 H55 C21 0.959 1_555 1_555 H56 C21 0.961 1_555 1_555 H57 C21 0.959 1_555 1_555 H58 C22 0.960 1_555 1_555 H59 C22 0.960 1_555 1_555 H60 C22 0.959 1_555 1_555 H61 C23 0.960 1_555 1_555 H62 C23 0.959 1_555 1_555 H63 C24 0.962 1_555 1_555 H64 C24 0.960 1_555 1_555 H65 C25 0.959 1_555 1_555 H66 C25 0.961 1_555 1_555 H67 C25 0.961 1_555 1_555 H68 C26 0.961 1_555 1_555 H69 C26 0.960 1_555 1_555 H70 C26 0.960 1_555 1_555 H71 C27 0.961 1_555 1_555 H72 C27 0.961 1_555 1_555 H73 C27 0.960 1_555 1_555 H74 C28 0.961 1_555 1_555 H75 C28 0.959 1_555 1_555 H76 C28 0.961 1_555 1_555 C41A C41 1.086 1_555 1_555 C42A C41A 1.417 1_555 1_555 C43A C42A 1.417 1_555 1_555 C1 C2 1.537 1_555 1_555 C1 B3 1.506 1_555 1_555 C2 B4 1.690 1_555 1_555 C2 B1 1.527 1_555 1_555 B1 B2 1.616 1_555 1_555 B1 B4 1.697 1_555 1_555 B2 B4 1.845 1_555 1_555 B2 B3 1.620 1_555 1_555 B2 Li2 2.616 1_555 1_555 B3 B4 1.861 1_555 1_555 B3 Li2 2.442 1_555 1_555 C3 C4 1.492 1_555 1_555 C3 B7 1.554 1_555 1_555 C4 B8 1.591 1_555 1_555 C4 B5 1.605 1_555 1_555 B5 Li1 2.663 1_555 1_555 B5 B6 1.650 1_555 1_555 B5 B8 1.722 1_555 1_555 B6 B7 1.640 1_555 1_555 B6 B8 1.746 1_555 1_555 B6 Li1 2.508 1_555 1_555 B7 B8 1.758 1_555 1_555 Li1 H1 1.726 1_555 1_555 Li1 H6 2.004 1_555 1_555 Li1 H5 2.362 1_555 1_555 C17 C18 1.459 1_555 1_555 Li2 H3 2.013 1_555 1_555 Li2 H2 2.401 1_555 1_555 C23 C24 1.579 1_555 1_555 C35 C36 1.578 1_555 1_555 #END data_CSD_CIF_YUCGOS _audit_creation_date 1996-04-04 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD YUCGOS _chemical_formula_sum 'C28 H64 La2 Na3 O50 S4 Tb1' _chemical_formula_moiety ; (C28 H32 La2 O34 S4 Tb1 3+)n,3n(Na1 1-),16n(H2 O1) ; _journal_coden_Cambridge 580 _journal_volume 14 _journal_year 1995 _journal_page_first 1201 _journal_name_full 'Polyhedron ' loop_ _publ_author_name "Hong-Ye Sun" "Chun-Hui Huang" "Xiang-Lin Jin" "Guang-Xiang Xu" _chemical_name_systematic ; catena-(trisodium bis(\m~3~-5-sulfonatosalicylato-O,O')-bis(\m~2~-5-sulfonatosalicylato-O,O')-de ca-aqua-di-lanthanum-terbium hexadecahydrate) ; _cell_volume 6358.517 _exptl_crystal_density_diffrn 1.917 _exptl_special_details ; Coordinates of the Na and a sulfonato O are not available ; _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.064 _refine_ls_wR_factor_gt 0.064 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 1/2+x,1/2+y,z 4 1/2-x,1/2+y,1/2-z 5 -x,-y,-z 6 x,-y,-1/2+z 7 -1/2-x,-1/2-y,-z 8 -1/2+x,-1/2-y,-1/2+z _cell_length_a 16.319(10) _cell_length_b 18.374(8) _cell_length_c 22.075(8) _cell_angle_alpha 90 _cell_angle_beta 106.13(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 La 1.67 Na 1.15 O 0.68 S 1.02 Tb 1.76 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 0.50000 0.00000 0.00000 Na2 Na 0.2304(5) 0.2179(5) 0.0720(3) O1 O -0.1334(7) 0.2856(6) 0.1019(5) O2 O 0.3336(10) 0.2969(9) 0.0456(7) O3 O 0.5671(15) 0.1166(13) 0.0025(11) O4 O 0.5682(14) -0.0259(13) 0.1098(10) O5 O 0.3310(11) 0.3256(9) 0.2384(8) O6 O 0.00000 -0.1282(15) 0.25000 O7 O 0.4700(12) 0.1617(11) 0.1516(9) O8 O 0.00000 0.2895(28) 0.25000 O9 O 0.1457(28) 0.3235(25) 0.0689(20) O10 O 0.1389(33) 0.3221(29) 0.2159(23) Tb1 Tb 0.00000 0.0769(1) 0.25000 La1 La 0.2405(1) 0.0758(1) 0.2095(1) S1 S -0.1001(2) 0.2114(2) -0.0916(2) O11 O -0.1604(7) 0.1608(6) -0.1313(4) O12 O -0.0157(7) 0.2064(7) -0.0990(5) O13 O -0.0850(6) 0.1544(5) 0.1744(4) O14 O 0.1411(5) 0.1547(6) 0.1162(4) O15 O 0.0866(5) 0.1322(5) 0.1936(4) C1 C -0.0934(9) 0.1898(8) -0.0125(6) C2 C -0.1661(10) 0.1866(9) 0.0066(6) C3 C -0.1635(9) 0.1735(9) 0.0680(7) C4 C -0.0844(8) 0.1639(7) 0.1144(6) C5 C -0.0105(8) 0.1659(7) 0.0947(6) C6 C -0.0166(9) 0.1802(8) 0.0305(6) C7 C 0.0759(8) 0.1511(7) 0.1367(6) S2 S -0.3132(3) -0.0320(3) -0.0596(2) O16 O -0.3277(12) 0.0533(8) -0.0820(7) O17 O -0.3843(7) -0.0473(11) -0.0411(5) O18 O -0.2869(6) -0.0623(7) -0.1083(4) O19 O -0.0198(5) -0.0056(5) 0.1658(4) O20 O -0.2706(6) 0.0088(7) 0.1806(4) O21 O -0.1368(5) 0.0220(5) 0.2297(4) C8 C -0.2255(8) -0.0261(8) 0.0073(6) C9 C -0.1417(9) -0.0325(9) 0.0037(6) C10 C -0.0760(9) -0.0256(8) 0.0561(6) C11 C -0.0883(8) -0.0123(7) 0.1166(6) C12 C -0.1722(8) -0.0085(7) 0.1198(6) C13 C -0.2398(9) -0.0157(8) 0.0655(6) C14 C -0.1946(8) 0.0071(8) 0.1793(6) O22 O 0.1316(6) -0.0103(5) 0.1413(5) O23 O 0.2337(6) 0.1728(6) 0.2917(4) O24 O 0.3169(7) 0.1948(6) 0.1838(5) O25 O 0.4004(7) 0.0807(9) 0.2688(6) O26 O 0.3104(8) -0.0509(7) 0.2074(6) S1A S 0.1001(2) 0.2114(2) 0.5916(2) O11A O 0.1604(7) 0.1608(6) 0.6313(4) O12A O 0.0157(7) 0.2064(7) 0.5990(5) O13A O 0.0850(6) 0.1544(5) 0.3256(4) O14A O -0.1411(5) 0.1547(6) 0.3838(4) O15A O -0.0866(5) 0.1322(5) 0.3064(4) C1A C 0.0934(9) 0.1898(8) 0.5125(6) C2A C 0.1661(10) 0.1866(9) 0.4934(6) C3A C 0.1635(9) 0.1735(9) 0.4320(7) C4A C 0.0844(8) 0.1639(7) 0.3856(6) C5A C 0.0105(8) 0.1659(7) 0.4053(6) C6A C 0.0166(9) 0.1802(8) 0.4695(6) C7A C -0.0759(8) 0.1511(7) 0.3633(6) S2A S 0.3132(3) -0.0320(3) 0.5596(2) O16A O 0.3277(12) 0.0533(8) 0.5820(7) O17A O 0.3843(7) -0.0473(11) 0.5411(5) O18A O 0.2869(6) -0.0623(7) 0.6083(4) O19A O 0.0198(5) -0.0056(5) 0.3342(4) O20A O 0.2706(6) 0.0088(7) 0.3194(4) O21A O 0.1368(5) 0.0220(5) 0.2703(4) C8A C 0.2255(8) -0.0261(8) 0.4927(6) C9A C 0.1417(9) -0.0325(9) 0.4963(6) C10A C 0.0760(9) -0.0256(8) 0.4439(6) C11A C 0.0883(8) -0.0123(7) 0.3834(6) C12A C 0.1722(8) -0.0085(7) 0.3802(6) C13A C 0.2398(9) -0.0157(8) 0.4345(6) C14A C 0.1946(8) 0.0071(8) 0.3207(6) La1A La -0.2405(1) 0.0758(1) 0.2905(1) O22A O -0.1316(6) -0.0103(5) 0.3587(5) O23A O -0.2337(6) 0.1728(6) 0.2083(4) O24A O -0.3169(7) 0.1948(6) 0.3162(5) O25A O -0.4004(7) 0.0807(9) 0.2312(6) O26A O -0.3104(8) -0.0509(7) 0.2926(6) O18D O 0.2869(6) 0.0623(7) 0.1083(4) La1D La -0.2405(1) -0.0758(1) -0.2095(1) La1E La 0.2405(1) -0.0758(1) 0.7095(1) O18E O -0.2869(6) 0.0623(7) 0.3917(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Tb1 O13 2.335 1_555 1_555 La1 O14 2.668 1_555 1_555 S1 O11 1.457 1_555 1_555 O12 S1 1.434 1_555 1_555 O13 C4 1.339 1_555 1_555 O14 C7 1.268 1_555 1_555 O15 Tb1 2.357 1_555 1_555 C1 S1 1.764 1_555 1_555 C2 C1 1.366 1_555 1_555 C3 C2 1.366 1_555 1_555 C4 C3 1.418 1_555 1_555 C5 C4 1.391 1_555 1_555 C6 C1 1.357 1_555 1_555 C7 O15 1.268 1_555 1_555 S2 O16 1.641 1_555 1_555 O17 S2 1.362 1_555 1_555 O18 S2 1.381 1_555 1_555 O19 Tb1 2.350 1_555 1_555 O20 C14 1.249 1_555 1_555 O21 Tb1 2.376 1_555 1_555 C8 S2 1.751 1_555 1_555 C9 C8 1.397 1_555 1_555 C10 C9 1.347 1_555 1_555 C11 O19 1.330 1_555 1_555 C12 C11 1.392 1_555 1_555 C13 C8 1.381 1_555 1_555 C14 O21 1.273 1_555 1_555 O22 La1 2.538 1_555 1_555 O23 La1 2.568 1_555 1_555 O24 La1 2.655 1_555 1_555 O25 La1 2.575 1_555 1_555 O26 La1 2.599 1_555 1_555 S1A O11A 1.457 1_555 1_555 O12A S1A 1.434 1_555 1_555 O13A Tb1 2.335 1_555 1_555 O14A C7A 1.268 1_555 1_555 O15A Tb1 2.357 1_555 1_555 C1A S1A 1.764 1_555 1_555 C2A C1A 1.366 1_555 1_555 C3A C2A 1.366 1_555 1_555 C4A O13A 1.339 1_555 1_555 C5A C4A 1.391 1_555 1_555 C6A C1A 1.357 1_555 1_555 C7A O15A 1.268 1_555 1_555 S2A O16A 1.641 1_555 1_555 O17A S2A 1.362 1_555 1_555 O18A S2A 1.381 1_555 1_555 O19A Tb1 2.350 1_555 1_555 O20A La1 2.642 1_555 1_555 O21A Tb1 2.376 1_555 1_555 C8A S2A 1.751 1_555 1_555 C9A C8A 1.397 1_555 1_555 C10A C9A 1.347 1_555 1_555 C11A O19A 1.330 1_555 1_555 C12A C11A 1.392 1_555 1_555 C13A C8A 1.381 1_555 1_555 C14A O20A 1.249 1_555 1_555 La1A O20 2.642 1_555 1_555 O22A La1A 2.538 1_555 1_555 O23A La1A 2.568 1_555 1_555 O24A La1A 2.655 1_555 1_555 O25A La1A 2.575 1_555 1_555 O26A La1A 2.599 1_555 1_555 O18D La1 2.562 1_555 1_555 La1D O18 2.562 1_555 1_555 La1E O18A 2.562 1_555 1_555 O18E La1A 2.562 1_555 1_555 La1 O15 2.649 1_555 1_555 La1 O21A 2.628 1_555 1_555 C5 C6 1.417 1_555 1_555 C5 C7 1.482 1_555 1_555 O21 La1A 2.628 1_555 1_555 C10 C11 1.426 1_555 1_555 C12 C13 1.392 1_555 1_555 C12 C14 1.486 1_555 1_555 O14A La1A 2.668 1_555 1_555 O15A La1A 2.649 1_555 1_555 C3A C4A 1.418 1_555 1_555 C5A C6A 1.417 1_555 1_555 C5A C7A 1.482 1_555 1_555 O21A C14A 1.273 1_555 1_555 C10A C11A 1.426 1_555 1_555 C12A C13A 1.392 1_555 1_555 C12A C14A 1.486 1_555 1_555 #END data_CSD_CIF_YUPJIC _audit_creation_date 1996-05-02 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD YUPJIC _chemical_formula_sum 'C106 H160 Li4 N8 O8 Ti2' _chemical_formula_moiety ; 2(C16 H32 Li1 O4 1+),C74 H96 Li2 N8 Ti2 2- ; _journal_coden_Cambridge 179 _journal_volume 34 _journal_year 1995 _journal_page_first 1092 _journal_name_full 'Angew.Chem.,Int.Ed. ' loop_ _publ_author_name "S.DeAngelis" "E.Solari" "C.Floriani" "A.Chiesi-Villa" "C.Rizzoli" _chemical_name_systematic ; bis(tetrakis(Tetrahydrofuran)-lithium) (\m~4~-ethylene-1,2-dienyl)-(\h^3^,\h^3^-5,5,10,10,15,15,20,20-octaethylporphy rinogen)-di-lithium-di-titanium benzene solvate ; _cell_volume 5440.138 _diffrn_ambient_temperature ? _diffrn_special_details ; The study was carried out at room temperature,in the range 283-303K ; _refine_special_details ; Six tetrahydrofuran molecules are disordered as are a number of ethyl groups with occupancies of 0.6:0.4 for C32 and C34; and 0.5 occupancies for C29-32, C51-56 and C60-72. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.092 _refine_ls_wR_factor_gt 0.092 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 16.648(2) _cell_length_b 22.144(3) _cell_length_c 15.948(2) _cell_angle_alpha 97.97(1) _cell_angle_beta 108.95(1) _cell_angle_gamma 79.02(1) _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Li 1.66 N 0.68 O 0.59 Ti 1.14 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Ti1 Ti 0.18013(12) 0.27536(9) -0.12192(13) N1 N 0.0846(5) 0.3435(4) -0.0900(6) N2 N 0.1891(5) 0.3398(4) -0.2045(6) N3 N 0.2210(6) 0.2073(4) -0.2127(6) N4 N 0.1075(6) 0.2100(4) -0.1093(6) C1 C 0.0606(7) 0.3299(5) -0.0191(8) C2 C 0.0747(7) 0.3772(7) 0.0479(8) C3 C 0.1029(8) 0.4237(6) 0.0145(9) C4 C 0.1086(7) 0.4008(5) -0.0682(8) C5 C 0.1230(8) 0.4368(5) -0.1334(8) C6 C 0.1346(7) 0.3964(5) -0.2128(8) C7 C 0.1169(8) 0.4133(5) -0.2980(8) C8 C 0.1625(8) 0.3659(7) -0.3425(8) C9 C 0.2066(8) 0.3219(5) -0.2838(8) C10 C 0.2820(8) 0.2739(6) -0.2858(8) C11 C 0.2900(8) 0.2194(5) -0.2346(8) C12 C 0.3564(8) 0.1727(7) -0.2128(8) C13 C 0.3317(9) 0.1290(6) -0.1790(9) C14 C 0.2489(9) 0.1503(6) -0.1794(8) C15 C 0.1883(9) 0.1138(6) -0.1630(9) C16 C 0.1030(9) 0.1529(6) -0.1577(7) C17 C 0.0263(10) 0.1362(6) -0.1749(9) C18 C -0.0230(8) 0.1824(7) -0.1364(10) C19 C 0.0275(8) 0.2253(6) -0.0940(8) C20 C 0.0171(8) 0.2773(6) -0.0206(9) C21 C 0.0479(11) 0.4877(6) -0.1608(10) C22 C -0.0406(11) 0.4660(8) -0.1979(10) C23 C 0.206(1) 0.4664(7) -0.0852(10) C24 C 0.2299(12) 0.5076(8) -0.1357(12) C25 C 0.2816(11) 0.2511(8) -0.3819(10) C26 C 0.2107(11) 0.2121(9) -0.4287(10) C27 C 0.3681(9) 0.3051(8) -0.2405(10) C28 C 0.3748(10) 0.3596(9) -0.2823(12) C29 C 0.1695(12) 0.0616(7) -0.2385(13) Ti2 Ti 0.42643(12) 0.27837(9) 0.14564(13) N5 N 0.3749(6) 0.3217(4) 0.2478(6) N6 N 0.4425(6) 0.1951(4) 0.2064(6) N7 N 0.5313(5) 0.2338(5) 0.0984(6) N8 N 0.4746(6) 0.3601(5) 0.1525(7) C30 C 0.3330(9) 0.3817(6) 0.2354(7) C31 C 0.2522(10) 0.3882(7) 0.2377(10) C32 C 0.2422(8) 0.3318(8) 0.2561(10) C33 C 0.3163(8) 0.2913(6) 0.2615(7) C34 C 0.3405(8) 0.2274(6) 0.2955(8) C35 C 0.4246(8) 0.1944(5) 0.2847(8) C36 C 0.4831(9) 0.1507(6) 0.3361(8) C37 C 0.5384(8) 0.1216(5) 0.2864(8) C38 C 0.5114(7) 0.1484(5) 0.2065(8) C39 C 0.5300(7) 0.1240(5) 0.1211(8) C40 C 0.5257(7) 0.1736(6) 0.0665(8) C41 C 0.5292(8) 0.1675(7) -0.0203(8) C42 C 0.5378(9) 0.2245(8) -0.0414(10) C43 C 0.5408(7) 0.2660(7) 0.0345(10) C44 C 0.5642(8) 0.3271(8) 0.0517(11) C45 C 0.5466(9) 0.3623(7) 0.1323(11) C46 C 0.5867(10) 0.409(1) 0.1798(14) C47 C 0.5333(13) 0.4407(7) 0.2331(11) C48 C 0.4658(9) 0.4106(6) 0.2146(9) C49 C 0.3795(10) 0.4334(6) 0.2298(8) C50 C 0.3453(10) 0.2342(8) 0.3963(10) C51 C 0.4032(12) 0.2776(8) 0.4554(10) C52 C 0.2686(9) 0.1891(7) 0.2416(10) C53 C 0.2796(11) 0.1238(9) 0.2655(12) C54 C 0.6201(9) 0.0834(6) 0.1413(9) C55 C 0.6957(10) 0.1175(8) 0.1836(12) C56 C 0.4593(9) 0.0831(6) 0.0664(8) C57 C 0.4495(10) 0.0300(6) 0.1122(9) C58 C 0.6659(22) 0.3287(14) 0.0781(24) C59? C 0.6462(18) 0.3194(13) 0.0227(22) C60 C 0.1302(13) 0.0813(9) -0.3285(12) C61 C 0.2361(11) 0.0807(8) -0.0762(11) C62 C 0.2292(18) 0.1134(12) 0.0125(14) C63? C 0.1847(22) 0.0543(17) -0.0297(25) C64 C -0.0814(10) 0.3005(9) -0.0334(15) C65 C -0.1233(19) 0.3467(14) -0.1039(18) C66? C -0.1228(32) 0.3539(23) -0.0073(33) C67 C 0.0604(13) 0.2473(8) 0.0714(10) C68 C 0.0229(16) 0.1941(11) 0.0840(12) Li1 Li 0.3801(14) 0.2177(10) -0.0625(15) C69 C 0.2721(6) 0.2761(4) -0.0228(7) Li2 Li -0.3195(19) 0.1231(16) -0.2970(21) O1 O -0.2494(9) 0.0932(7) -0.1808(9) O2 O -0.4257(9) 0.0962(6) -0.3326(8) O3 O -0.2587(9) 0.0950(7) -0.3847(9) O4 O -0.3370(9) 0.2108(6) -0.2904(10) C70 C -0.2603(28) 0.1175(18) -0.0919(24) C71 C -0.1925(41) 0.0969(20) -0.0189(28) C72 C -0.1321(22) 0.0551(18) -0.0600(24) C73 C -0.1706(18) 0.0476(11) -0.1621(23) C74 C -0.4506(18) 0.0502(12) -0.2967(17) C75 C -0.4971(16) 0.1224(11) -0.4006(17) C76 C -0.5394(18) 0.0356(10) -0.3567(18) C77 C -0.5670(19) 0.0826(12) -0.4251(15) C78 C -0.1701(13) 0.1025(15) -0.3758(17) C79 C -0.1640(21) 0.0781(15) -0.4692(18) C80 C -0.2331(30) 0.0360(22) -0.5113(37) C81 C -0.2776(35) 0.0369(15) -0.4403(32) C82 C 0.7504(26) 0.2725(17) 0.1246(29) C83? C 0.7286(22) 0.2808(18) 0.0752(27) C84 C 0.5418(21) 0.3764(16) -0.0121(23) C85? C 0.5003(17) 0.3578(11) -0.0385(15) C86 C 0.4448(18) 0.4010(15) -0.0245(20) C87? C 0.5023(23) 0.4288(13) -0.0361(23) C88 C 0.3944(15) 0.4750(9) 0.3177(16) C89 C 0.4414(17) 0.4458(12) 0.3973(16) C90 C 0.3216(10) 0.4736(7) 0.1534(11) C91 C 0.3490(14) 0.5279(8) 0.1403(13) Li3 Li 0.2251(14) 0.3366(10) 0.0869(14) C92 C 0.3371(5) 0.2771(4) 0.0495(5) Li4 Li -0.1590(15) 0.3556(11) -0.5511(18) O5 O -0.1840(9) 0.4416(6) -0.5316(9) O6 O -0.2606(7) 0.3217(6) -0.5962(8) O7 O -0.1002(8) 0.3164(7) -0.4452(8) O8 O -0.0847(8) 0.3394(7) -0.6247(9) C93 C -0.1695(44) 0.4714(16) -0.4401(15) C94? C -0.130(2) 0.4829(16) -0.4659(28) C95 C -0.3915(14) 0.2993(12) -0.5868(17) C96 C -0.3349(15) 0.3507(11) -0.5647(21) C97 C -0.3746(23) 0.2604(18) -0.6681(21) C98 C -0.2859(25) 0.2718(16) -0.6669(23) C99? C -0.3495(15) 0.3149(25) -0.6522(18) C100? C -0.3364(26) 0.2397(15) -0.6123(33) C101? C -0.2517(27) 0.2539(9) -0.6197(33) C102 C -0.119(3) 0.3353(19) -0.3599(18) C103 C -0.0557(31) 0.2849(18) -0.3040(26) C104 C -0.0360(34) 0.2290(18) -0.3679(29) C105? C -0.2438(24) 0.0682(32) -0.5484(26) C106? C -0.2953(29) 0.0917(24) -0.4826(12) C107 C -0.2802(25) 0.2471(15) -0.3108(34) C108 C -0.4203(17) 0.2502(17) -0.2922(31) C109 C -0.4098(22) 0.3149(19) -0.3083(41) C110 C -0.3131(22) 0.3157(16) -0.2902(27) C111? C -0.3167(32) 0.2512(18) -0.2066(19) C112? C -0.3771(29) 0.3108(19) -0.2396(28) C113? C -0.3785(51) 0.3136(26) -0.3363(29) C114? C -0.3654(44) 0.2450(24) -0.3712(24) C115 C -0.2478(15) 0.4807(10) -0.5984(14) C116 C -0.2804(20) 0.5312(14) -0.5360(21) C117 C -0.1979(25) 0.5396(15) -0.4592(23) C118 C -0.022(2) 0.2696(16) -0.4315(29) C119? C -0.1516(25) 0.3008(23) -0.3929(28) C120? C -0.0927(23) 0.2500(25) -0.3344(41) C121? C -0.0025(21) 0.2621(17) -0.3279(23) C122? C -0.0282(24) 0.3262(17) -0.3640(22) C123 C -0.0867(33) 0.3059(21) -0.7124(21) C124 C -0.0266(27) 0.3392(20) -0.7389(28) C125 C 0.0337(30) 0.2879(21) -0.6835(28) C126 C 0.0069(14) 0.3107(21) -0.5994(28) C127? C -0.1153(28) 0.3470(24) -0.7214(13) C128? C -0.0495(30) 0.3868(28) -0.7227(44) C129? C 0.0348(26) 0.3524(20) -0.6643(29) C130? C -0.0213(23) 0.3823(16) -0.6046(28) H1 H 0.06650 0.37850 0.10250 H2 H 0.11510 0.46140 0.04410 H3 H 0.08150 0.44910 -0.32140 H4 H 0.16190 0.36440 -0.40100 H5 H 0.41040 0.17120 -0.21950 H6 H 0.36380 0.09180 -0.15960 H7 H 0.00790 0.09990 -0.20630 H8 H -0.08060 0.18380 -0.13900 H9 H 0.05720 0.50890 -0.20590 H10 H 0.04870 0.51700 -0.10990 H11 H -0.08390 0.50140 -0.21420 H12 H -0.05000 0.44610 -0.15390 H13 H -0.04150 0.43800 -0.25000 H14 H 0.19850 0.48910 -0.03190 H15 H 0.25320 0.43300 -0.06900 H16 H 0.28140 0.52340 -0.09920 H17 H 0.18430 0.54250 -0.15200 H18 H 0.23950 0.48620 -0.18900 H19 H 0.27330 0.28630 -0.41530 H20 H 0.33680 0.22670 -0.38050 H21 H 0.21330 0.19900 -0.48820 H22 H 0.15610 0.23640 -0.43160 H23 H 0.21960 0.17680 -0.39670 H24 H 0.37110 0.31800 -0.17850 H25 H 0.41690 0.27420 -0.24040 H26 H 0.42740 0.37510 -0.24930 H27 H 0.32700 0.39230 -0.28050 H28 H 0.37340 0.34830 -0.34240 H29 H 0.22220 0.03370 -0.23610 H30 H 0.13040 0.03820 -0.22720 H31 H 0.12120 0.04560 -0.36990 H32 H 0.16930 0.10300 -0.34140 H33 H 0.07730 0.10770 -0.33240 H34 H 0.12100 0.23360 0.07820 H35 H 0.05720 0.27940 0.11910 H36 H 0.05420 0.18040 0.14200 H37 H 0.02840 0.16190 0.03940 H38 H -0.03600 0.20790 0.08000 H39 H 0.21090 0.42380 0.22860 H40 H 0.19280 0.32320 0.26400 H41 H 0.48660 0.14170 0.39280 H42 H 0.58410 0.08990 0.30390 H43 H 0.52650 0.13110 -0.05770 H44 H 0.54090 0.23220 -0.09600 H45 H 0.63830 0.41940 0.17980 H46 H 0.54340 0.47580 0.27320 H47 H 0.28860 0.24850 0.40120 H48 H 0.36530 0.19400 0.41950 H49 H 0.40260 0.27810 0.51560 H50 H 0.38410 0.31800 0.43570 H51 H 0.46120 0.26350 0.45350 H52 H 0.21440 0.21020 0.24770 H53 H 0.26450 0.18650 0.17890 H54 H 0.23190 0.10390 0.22800 H55 H 0.28160 0.12400 0.32660 H56 H 0.33200 0.10020 0.25770 H57 H 0.62300 0.05250 0.18000 H58 H 0.62680 0.06230 0.08610 H59 H 0.74790 0.08920 0.19450 H60 H 0.69090 0.13820 0.24050 H61 H 0.69470 0.14790 0.14640 H62 H 0.40420 0.11000 0.04950 H63 H 0.47180 0.06590 0.01190 H64 H 0.40440 0.00890 0.07280 H65 H 0.43470 0.04640 0.16530 H66 H 0.50240 0.00210 0.12730 H67 H 0.41980 0.50870 0.31310 H68 H 0.33600 0.49270 0.32310 H69 H 0.44580 0.47510 0.44840 H70 H 0.49920 0.42940 0.39470 H71 H 0.41530 0.41230 0.40370 H72 H 0.31100 0.44690 0.09850 H73 H 0.26580 0.48640 0.16410 H74 H 0.30740 0.54800 0.09010 H75 H 0.40330 0.51640 0.12620 H76 H 0.35750 0.55620 0.19180 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ti1 N1 2.113 1_555 1_555 N1 C1 1.401 1_555 1_555 N2 Ti1 2.127 1_555 1_555 N3 Ti1 2.115 1_555 1_555 N4 Ti1 2.122 1_555 1_555 C1 C2 1.384 1_555 1_555 C2 C3 1.436 1_555 1_555 C3 C4 1.372 1_555 1_555 C4 N1 1.368 1_555 1_555 C5 C4 1.496 1_555 1_555 C6 N2 1.395 1_555 1_555 C7 C6 1.383 1_555 1_555 C8 C7 1.422 1_555 1_555 C9 N2 1.378 1_555 1_555 C10 C9 1.488 1_555 1_555 C11 N3 1.385 1_555 1_555 C12 C11 1.352 1_555 1_555 C13 C12 1.355 1_555 1_555 C14 N3 1.376 1_555 1_555 C15 C14 1.510 1_555 1_555 C16 N4 1.389 1_555 1_555 C17 C16 1.329 1_555 1_555 C18 C17 1.389 1_555 1_555 C19 N4 1.402 1_555 1_555 C20 C1 1.478 1_555 1_555 C21 C5 1.506 1_555 1_555 C22 C21 1.542 1_555 1_555 C23 C5 1.564 1_555 1_555 C24 C23 1.480 1_555 1_555 C25 C10 1.544 1_555 1_555 C26 C25 1.528 1_555 1_555 C27 C10 1.619 1_555 1_555 C28 C27 1.495 1_555 1_555 C29 C15 1.546 1_555 1_555 Ti2 N5 2.115 1_555 1_555 N5 C30 1.386 1_555 1_555 N6 Ti2 2.133 1_555 1_555 N7 Ti2 2.140 1_555 1_555 N8 Ti2 2.091 1_555 1_555 C30 C31 1.337 1_555 1_555 C31 C32 1.373 1_555 1_555 C32 C33 1.365 1_555 1_555 C33 N5 1.372 1_555 1_555 C34 C33 1.521 1_555 1_555 C35 N6 1.377 1_555 1_555 C36 C35 1.378 1_555 1_555 C37 C36 1.413 1_555 1_555 C38 N6 1.390 1_555 1_555 C39 C38 1.500 1_555 1_555 C40 N7 1.369 1_555 1_555 C41 C40 1.391 1_555 1_555 C42 C41 1.395 1_555 1_555 C43 N7 1.386 1_555 1_555 C44 C43 1.444 1_555 1_555 C45 N8 1.349 1_555 1_555 C46 C45 1.344 1_555 1_555 C47 C46 1.447 1_555 1_555 C48 N8 1.406 1_555 1_555 C49 C30 1.526 1_555 1_555 C50 C34 1.571 1_555 1_555 C51 C50 1.501 1_555 1_555 C52 C34 1.552 1_555 1_555 C53 C52 1.509 1_555 1_555 C54 C39 1.554 1_555 1_555 C55 C54 1.510 1_555 1_555 C56 C39 1.577 1_555 1_555 C57 C56 1.527 1_555 1_555 C58 C44 1.613 1_555 1_555 C60 C29 1.461 1_555 1_555 C61 C15 1.559 1_555 1_555 C62 C61 1.526 1_555 1_555 C64 C20 1.577 1_555 1_555 C65 C64 1.528 1_555 1_555 C67 C20 1.586 1_555 1_555 C68 C67 1.498 1_555 1_555 Li1 C11 2.668 1_555 1_555 C69 Ti1 1.809 1_555 1_555 Li2 O1 1.969 1_555 1_555 O1 C70 1.500 1_555 1_555 O2 Li2 1.860 1_555 1_555 O3 Li2 1.951 1_555 1_555 O4 Li2 1.901 1_555 1_555 C70 C71 1.391 1_555 1_555 C71 C72 1.484 1_555 1_555 C72 C73 1.542 1_555 1_555 C73 O1 1.468 1_555 1_555 C74 O2 1.419 1_555 1_555 C75 O2 1.414 1_555 1_555 C76 C74 1.544 1_555 1_555 C77 C75 1.511 1_555 1_555 C78 O3 1.475 1_555 1_555 C79 C78 1.541 1_555 1_555 C80 C79 1.542 1_555 1_555 C81 O3 1.482 1_555 1_555 C82 C58 1.729 1_555 1_555 C84 C44 1.508 1_555 1_555 C86 C84 1.559 1_555 1_555 C88 C49 1.542 1_555 1_555 C89 C88 1.425 1_555 1_555 C90 C49 1.555 1_555 1_555 C91 C90 1.428 1_555 1_555 Li3 C1 2.731 1_555 1_555 C92 Ti2 1.757 1_555 1_555 Li4 O5 1.875 1_555 1_555 O5 C93 1.479 1_555 1_555 O6 Li4 1.867 1_555 1_555 O7 Li4 1.890 1_555 1_555 O8 Li4 1.922 1_555 1_555 C93 C117 1.536 1_555 1_555 C95 C96 1.546 1_555 1_555 C96 O6 1.485 1_555 1_555 C97 C95 1.529 1_555 1_555 C98 O6 1.481 1_555 1_555 C102 O7 1.481 1_555 1_555 C103 C102 1.539 1_555 1_555 C104 C103 1.546 1_555 1_555 C107 O4 1.486 1_555 1_555 C108 O4 1.485 1_555 1_555 C109 C108 1.541 1_555 1_555 C110 C107 1.542 1_555 1_555 C115 O5 1.478 1_555 1_555 C116 C115 1.532 1_555 1_555 C117 C116 1.537 1_555 1_555 C118 O7 1.477 1_555 1_555 C123 O8 1.483 1_555 1_555 C124 C123 1.538 1_555 1_555 C125 C124 1.532 1_555 1_555 C126 O8 1.481 1_555 1_555 H1 C2 0.920 1_555 1_555 H2 C3 0.924 1_555 1_555 H3 C7 0.936 1_555 1_555 H4 C8 0.926 1_555 1_555 H5 C12 0.933 1_555 1_555 H6 C13 0.925 1_555 1_555 H7 C17 0.934 1_555 1_555 H8 C18 0.941 1_555 1_555 H9 C21 0.977 1_555 1_555 H10 C21 0.965 1_555 1_555 H11 C22 0.960 1_555 1_555 H12 C22 0.946 1_555 1_555 H13 C22 0.963 1_555 1_555 H14 C23 0.958 1_555 1_555 H15 C23 0.965 1_555 1_555 H16 C24 0.964 1_555 1_555 H17 C24 0.972 1_555 1_555 H18 C24 0.959 1_555 1_555 H19 C25 0.968 1_555 1_555 H20 C25 0.968 1_555 1_555 H21 C26 0.965 1_555 1_555 H22 C26 0.955 1_555 1_555 H23 C26 0.954 1_555 1_555 H24 C27 0.978 1_555 1_555 H25 C27 0.957 1_555 1_555 H26 C28 0.963 1_555 1_555 H27 C28 0.974 1_555 1_555 H28 C28 0.950 1_555 1_555 H29 C29 0.965 1_555 1_555 H30 C29 0.977 1_555 1_555 H31 C60 0.959 1_555 1_555 H32 C60 0.965 1_555 1_555 H33 C60 0.948 1_555 1_555 H34 C67 0.971 1_555 1_555 H35 C67 0.974 1_555 1_555 H36 C68 0.961 1_555 1_555 H37 C68 0.948 1_555 1_555 H38 C68 0.954 1_555 1_555 H39 C31 0.936 1_555 1_555 H40 C32 0.928 1_555 1_555 H41 C36 0.934 1_555 1_555 H42 C37 0.929 1_555 1_555 H43 C41 0.933 1_555 1_555 H44 C42 0.929 1_555 1_555 H45 C46 0.931 1_555 1_555 H46 C47 0.940 1_555 1_555 H47 C50 0.962 1_555 1_555 H48 C50 0.969 1_555 1_555 H49 C51 0.962 1_555 1_555 H50 C51 0.951 1_555 1_555 H51 C51 0.966 1_555 1_555 H52 C52 0.962 1_555 1_555 H53 C52 0.974 1_555 1_555 H54 C53 0.967 1_555 1_555 H55 C53 0.964 1_555 1_555 H56 C53 0.964 1_555 1_555 H57 C54 0.968 1_555 1_555 H58 C54 0.967 1_555 1_555 H59 C55 0.950 1_555 1_555 H60 C55 0.979 1_555 1_555 H61 C55 0.952 1_555 1_555 H62 C56 0.972 1_555 1_555 H63 C56 0.969 1_555 1_555 H64 C57 0.961 1_555 1_555 H65 C57 0.962 1_555 1_555 H66 C57 0.955 1_555 1_555 H67 C88 0.947 1_555 1_555 H68 C88 1.003 1_555 1_555 H69 C89 0.961 1_555 1_555 H70 C89 0.974 1_555 1_555 H71 C89 0.960 1_555 1_555 H72 C90 0.971 1_555 1_555 H73 C90 0.981 1_555 1_555 H74 C91 0.970 1_555 1_555 H75 C91 0.980 1_555 1_555 H76 C91 0.950 1_555 1_555 C2 Li3 2.398 1_555 1_555 C3 Li3 2.606 1_555 1_555 C5 C6 1.490 1_555 1_555 C8 C9 1.378 1_555 1_555 C10 C11 1.511 1_555 1_555 C12 Li1 2.402 1_555 1_555 C13 C14 1.368 1_555 1_555 C13 Li1 2.565 1_555 1_555 C15 C16 1.537 1_555 1_555 C18 C19 1.350 1_555 1_555 C19 C20 1.552 1_555 1_555 C30 Li3 2.664 1_555 1_555 C31 Li3 2.454 1_555 1_555 C32 Li3 2.635 1_555 1_555 C34 C35 1.502 1_555 1_555 C37 C38 1.383 1_555 1_555 C39 C40 1.471 1_555 1_555 C40 Li1 2.735 1_555 1_555 C41 Li1 2.433 1_555 1_555 C42 C43 1.408 1_555 1_555 C42 Li1 2.567 1_555 1_555 C44 C45 1.492 1_555 1_555 C47 C48 1.345 1_555 1_555 C48 C49 1.515 1_555 1_555 Li1 C69 2.221 1_555 1_555 Li1 C92 2.292 1_555 1_555 C69 Li3 2.304 1_555 1_555 C69 C92 1.301 1_555 1_555 C76 C77 1.514 1_555 1_555 C80 C81 1.538 1_555 1_555 Li3 C92 2.266 1_555 1_555 C97 C98 1.538 1_555 1_555 C104 C118 1.542 1_555 1_555 C109 C110 1.544 1_555 1_555 C125 C126 1.539 1_555 1_555 #END data_CSD_CIF_ZEBZEO _audit_creation_date 2017-07-06 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD ZEBZEO _database_code_depnum_ccdc_archive 'CCDC 1560730' _chemical_formula_sum 'C54 H72 Dy1 Fe3 Li3 O6' _chemical_formula_moiety ; C38 H40 Dy1 Fe3 Li2 O2 1-,C16 H32 Li1 O4 1+ ; _journal_coden_Cambridge 4 _journal_volume 139 _journal_year 2017 _journal_page_first 8058 _journal_name_full 'J.Am.Chem.Soc. ' loop_ _publ_author_name "T.P.Latendresse" "N.S.Bhuvanesh" "M.Nippe" _chemical_name_systematic ; tetrakis(tetrahydrofuran)-lithium tris(\m-ferrocene-1,1,1',1'-tetrayl)-bis(tetrahydrofuran)-dysprosium-di-lithiu m ; _cell_volume 9937.871 _exptl_crystal_colour 'orange' _exptl_crystal_density_diffrn 1.561 _exptl_crystal_description 'plate' _diffrn_ambient_temperature 100 _refine_special_details ; C105,C106,C107,C108,O12 and C1A,C1B,C1C,C1D,O12A disordered over two sites with occupancies 0.638:0.362. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_gt 0.0589 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,-1/2-y,-1/2+z _cell_length_a 11.3810(9) _cell_length_b 63.671(5) _cell_length_c 13.7280(11) _cell_angle_alpha 90 _cell_angle_beta 92.567(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Dy 1.92 Fe 1.52 Li 1.28 O 0.68 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Dy1 Dy -0.15217(2) 0.56388(2) 0.28224(2) Fe1 Fe 0.07469(6) 0.58808(2) 0.37772(5) Fe2 Fe -0.41160(6) 0.57276(2) 0.35552(5) Fe3 Fe -0.12089(6) 0.53110(2) 0.10624(5) Li1 Li -0.1825(7) 0.59558(14) 0.1496(6) Li2 Li -0.1222(8) 0.53266(14) 0.4167(7) O1 O -0.1847(3) 0.62208(6) 0.0804(3) O2 O -0.1027(3) 0.51617(6) 0.5338(3) C1 C -0.0216(4) 0.59527(8) 0.2485(4) C2 C -0.0272(4) 0.61176(8) 0.3208(4) H1 H -0.09800 0.61680 0.34630 C3 C 0.0875(4) 0.61945(8) 0.3492(4) H2 H 0.10560 0.63020 0.39560 C4 C 0.1688(5) 0.60803(9) 0.2948(4) H3 H 0.25190 0.60960 0.29820 C5 C 0.1037(5) 0.59375(8) 0.2341(4) H4 H 0.13790 0.58440 0.18970 C6 C -0.0027(5) 0.56028(8) 0.4240(4) C7 C -0.0039(5) 0.57668(9) 0.4974(4) H5 H -0.07310 0.58190 0.52480 C8 C 0.1124(5) 0.58391(9) 0.5232(4) H6 H 0.13290 0.59470 0.56890 C9 C 0.1911(5) 0.57210(9) 0.4683(4) H7 H 0.27430 0.57340 0.47010 C10 C 0.1219(5) 0.55782(8) 0.4096(4) H8 H 0.15370 0.54790 0.36630 C11 C -0.3159(4) 0.59099(8) 0.2589(4) C12 C -0.4241(4) 0.58250(8) 0.2140(4) H9 H -0.42700 0.57370 0.15810 C13 C -0.5259(4) 0.58904(8) 0.2642(4) H10 H -0.60530 0.58540 0.24790 C14 C -0.4849(5) 0.60201(8) 0.3433(4) H11 H -0.53180 0.60860 0.39000 C15 C -0.3590(4) 0.60320(8) 0.3390(4) H12 H -0.31000 0.61110 0.38330 C16 C -0.2940(4) 0.54899(8) 0.4022(4) C17 C -0.4015(5) 0.54083(8) 0.3582(4) H13 H -0.40460 0.53180 0.30310 C18 C -0.5035(4) 0.54779(8) 0.4065(4) H14 H -0.58310 0.54440 0.38950 C19 C -0.4618(5) 0.56077(8) 0.4848(4) H15 H -0.50870 0.56780 0.53030 C20 C -0.3368(4) 0.56140(8) 0.4827(4) H16 H -0.28740 0.56890 0.52800 C21 C -0.1750(4) 0.56248(8) 0.0966(4) C22 C -0.0705(5) 0.55850(8) 0.0434(4) H17 H 0.00240 0.56550 0.05510 C23 C -0.0910(6) 0.54273(9) -0.0290(4) H18 H -0.03510 0.53750 -0.07230 C24 C -0.2095(5) 0.53626(9) -0.0247(4) H19 H -0.24810 0.52600 -0.06470 C25 C -0.2602(5) 0.54811(8) 0.0507(4) H20 H -0.33950 0.54680 0.06880 C26 C -0.1031(4) 0.52547(8) 0.2571(4) C27 C 0.0060(5) 0.52227(8) 0.2082(4) H21 H 0.07700 0.52960 0.22430 C28 C -0.0062(5) 0.50679(8) 0.1330(4) H22 H 0.05320 0.50230 0.09130 C29 C -0.1240(5) 0.49939(8) 0.1323(4) H23 H -0.15820 0.48890 0.09070 C30 C -0.1811(5) 0.51075(8) 0.2065(4) H24 H -0.26130 0.50890 0.22090 C31 C -0.2066(5) 0.64031(9) 0.1390(4) H25 H -0.23540 0.63600 0.20310 H26 H -0.26700 0.64930 0.10600 C32 C -0.0914(5) 0.65215(10) 0.1527(5) H27 H -0.06200 0.65170 0.22160 H28 H -0.10110 0.66700 0.13260 C33 C -0.0075(5) 0.64072(10) 0.0870(5) H29 H 0.03800 0.65080 0.04880 H30 H 0.04780 0.63170 0.12570 C34 C -0.0892(5) 0.62760(9) 0.0206(4) H31 H -0.11770 0.63580 -0.03690 H32 H -0.04860 0.61490 -0.00210 C35 C -0.2001(5) 0.51024(10) 0.5908(4) H33 H -0.19630 0.49510 0.60680 H34 H -0.27550 0.51310 0.55450 C36 C -0.1900(5) 0.52339(10) 0.6833(4) H35 H -0.19630 0.51440 0.74180 H36 H -0.25250 0.53420 0.68320 C37 C -0.0677(5) 0.53369(10) 0.6818(4) H37 H -0.07400 0.54880 0.66520 H38 H -0.02440 0.53220 0.74560 C38 C -0.0082(5) 0.52153(9) 0.6029(4) H39 H 0.05150 0.53030 0.57190 H40 H 0.03030 0.50870 0.63000 Dy2 Dy 0.42947(2) 0.67859(2) 0.74002(2) Fe4 Fe 0.44562(6) 0.64488(2) 0.56974(5) Fe5 Fe 0.65967(6) 0.69739(2) 0.85267(5) Fe6 Fe 0.17251(6) 0.69642(2) 0.79631(5) Li3 Li 0.4441(8) 0.70963(13) 0.6071(6) Li4 Li 0.4146(8) 0.64785(15) 0.8762(6) O3 O 0.4335(3) 0.73431(6) 0.5239(3) O4 O 0.4000(3) 0.62991(6) 0.9894(3) C39 C 0.4325(5) 0.67743(9) 0.5548(4) C40 C 0.5350(5) 0.66912(8) 0.5105(4) H41 H 0.61330 0.67330 0.52780 C41 C 0.5054(5) 0.65393(8) 0.4379(4) H42 H 0.55880 0.64640 0.39980 C42 C 0.3809(5) 0.65215(9) 0.4329(4) H43 H 0.33540 0.64320 0.39080 C43 C 0.3368(5) 0.66634(8) 0.5024(4) H44 H 0.25570 0.66830 0.51330 C44 C 0.4393(5) 0.63910(8) 0.7200(4) C45 C 0.5460(5) 0.63120(8) 0.6801(4) H45 H 0.62290 0.63520 0.70270 C46 C 0.5216(5) 0.61668(8) 0.6029(4) H46 H 0.57790 0.60970 0.56540 C47 C 0.3975(5) 0.61456(8) 0.5923(4) H47 H 0.35510 0.60580 0.54690 C48 C 0.3489(5) 0.62806(8) 0.6630(4) H48 H 0.26700 0.62960 0.67160 C49 C 0.5880(4) 0.70629(8) 0.7165(4) C50 C 0.5999(5) 0.72397(8) 0.7819(4) H49 H 0.53670 0.73270 0.79960 C51 C 0.7185(5) 0.72663(9) 0.8165(4) H50 H 0.74680 0.73720 0.86040 C52 C 0.7868(5) 0.71084(9) 0.7745(4) H51 H 0.86890 0.70870 0.78510 C53 C 0.7080(5) 0.69870(9) 0.7124(4) H52 H 0.73130 0.68720 0.67370 C54 C 0.5552(5) 0.67223(8) 0.8949(4) C55 C 0.5540(5) 0.68947(9) 0.9635(4) H53 H 0.48490 0.69660 0.98150 C56 C 0.6703(5) 0.69446(10) 1.0007(4) H54 H 0.69140 0.70530 1.04590 C57 C 0.7481(5) 0.68016(10) 0.9572(4) H55 H 0.83120 0.67970 0.96770 C58 C 0.6781(5) 0.66661(9) 0.8945(4) H56 H 0.70860 0.65540 0.85760 C59 C 0.2940(5) 0.70965(8) 0.7024(4) C60 C 0.1808(5) 0.70573(8) 0.6547(4) H57 H 0.16830 0.69680 0.59990 C61 C 0.0907(5) 0.71693(9) 0.7002(4) H58 H 0.00970 0.71700 0.68020 C62 C 0.1422(5) 0.72789(9) 0.7799(4) H59 H 0.10280 0.73660 0.82430 C63 C 0.2654(5) 0.72341(8) 0.7815(4) H60 H 0.32120 0.72880 0.82860 C64 C 0.2610(5) 0.66968(8) 0.8509(4) C65 C 0.1505(5) 0.66442(8) 0.8005(4) H61 H 0.14310 0.65520 0.74610 C66 C 0.0538(5) 0.67480(9) 0.8428(4) H62 H -0.02660 0.67390 0.82130 C67 C 0.1000(5) 0.68673(9) 0.9230(4) H63 H 0.05640 0.69520 0.96540 C68 C 0.2248(5) 0.68358(8) 0.9281(4) H64 H 0.27710 0.68980 0.97570 C69 C 0.3170(5) 0.73739(9) 0.4815(4) H65 H 0.27060 0.72430 0.48490 H66 H 0.32040 0.74160 0.41230 C70 C 0.2610(5) 0.75478(9) 0.5412(4) H67 H 0.20070 0.74890 0.58320 H68 H 0.22400 0.76550 0.49780 C71 C 0.3639(5) 0.76422(9) 0.6032(4) H69 H 0.36510 0.77970 0.59770 H70 H 0.35890 0.76030 0.67270 C72 C 0.4718(5) 0.75455(8) 0.5596(5) H71 H 0.49950 0.76340 0.50580 H72 H 0.53650 0.75300 0.60980 C73 C 0.3003(6) 0.63268(12) 1.0490(5) H73 H 0.27320 0.61900 1.07380 H74 H 0.23450 0.63950 1.01130 C74 C 0.3441(7) 0.64663(12) 1.1322(5) H75 H 0.30750 0.64270 1.19360 H76 H 0.32680 0.66160 1.11780 C75 C 0.4773(6) 0.64268(11) 1.1391(5) H77 H 0.52120 0.65590 1.13130 H78 H 0.50140 0.63630 1.20270 C76 C 0.4994(6) 0.62778(10) 1.0570(4) H79 H 0.57310 0.63150 1.02540 H80 H 0.50580 0.61320 1.08140 Li5 Li 0.8530(8) 0.69953(15) 0.4258(7) O5 O 0.7064(3) 0.69983(6) 0.3475(3) O6 O 0.9840(3) 0.69746(6) 0.3385(3) O7 O 0.8599(3) 0.72710(6) 0.4908(3) O8 O 0.8700(3) 0.67389(6) 0.5039(3) C77 C 0.6656(5) 0.68774(10) 0.2642(4) H81 H 0.64910 0.67310 0.28310 H82 H 0.72490 0.68770 0.21360 C78 C 0.5542(6) 0.69865(11) 0.2275(4) H83 H 0.57190 0.71060 0.18420 H84 H 0.50050 0.68880 0.19190 C79 C 0.5027(5) 0.70615(9) 0.3205(4) H85 H 0.44820 0.71810 0.30820 H86 H 0.46050 0.69470 0.35300 C80 C 0.6103(5) 0.71282(9) 0.3798(4) H87 H 0.62720 0.72790 0.36870 H88 H 0.59890 0.71060 0.45010 C81 C 1.0916(5) 0.68667(10) 0.3652(5) H89 H 1.07570 0.67180 0.38130 H90 H 1.13170 0.69340 0.42240 C82 C 1.1657(6) 0.68808(15) 0.2783(6) H91 H 1.24990 0.68950 0.29880 H92 H 1.15560 0.67540 0.23710 C83 C 1.1256(7) 0.70625(18) 0.2268(7) H93 H 1.13490 0.70450 0.15590 H94 H 1.17060 0.71880 0.24930 C84 C 0.9982(5) 0.70857(10) 0.2482(5) H95 H 0.97730 0.72360 0.25530 H96 H 0.94760 0.70240 0.19520 C85 C 0.7752(5) 0.73766(9) 0.5497(4) H97 H 0.73760 0.72760 0.59360 H98 H 0.71340 0.74450 0.50800 C86 C 0.8458(5) 0.75364(9) 0.6073(4) H99 H 0.88630 0.74720 0.66530 H100 H 0.79580 0.76540 0.62840 C87 C 0.9334(5) 0.76097(9) 0.5339(5) H101 H 0.90010 0.77240 0.49250 H102 H 1.00740 0.76590 0.56710 C88 C 0.9542(5) 0.74141(10) 0.4739(5) H103 H 0.95520 0.74500 0.40380 H104 H 1.03060 0.73500 0.49400 C89 C 0.8384(5) 0.65396(9) 0.4588(4) H105 H 0.89620 0.65000 0.41020 H106 H 0.75960 0.65490 0.42540 C90 C 0.8382(7) 0.63799(10) 0.5396(5) H107 H 0.88630 0.62560 0.52320 H108 H 0.75700 0.63320 0.55050 C91 C 0.8903(6) 0.64899(10) 0.6296(5) H109 H 0.95120 0.64020 0.66340 H110 H 0.82870 0.65240 0.67570 C92 C 0.9438(5) 0.66879(9) 0.5886(4) H111 H 0.94360 0.68030 0.63690 H112 H 1.02570 0.66620 0.57030 Li6 Li 0.3899(9) 0.55486(16) 0.8563(7) O9 O 0.5373(3) 0.56941(6) 0.8432(3) O10 O 0.3737(4) 0.54460(7) 0.9869(3) O11 O 0.3858(3) 0.53333(6) 0.7602(3) C93 C 0.5834(5) 0.58596(10) 0.9056(5) H113 H 0.59020 0.58110 0.97420 H114 H 0.53100 0.59840 0.90180 C94 C 0.7042(6) 0.59144(11) 0.8692(5) H115 H 0.71240 0.60680 0.86110 H116 H 0.76730 0.58640 0.91540 C95 C 0.7101(6) 0.58047(12) 0.7729(5) H117 H 0.76570 0.56850 0.77760 H118 H 0.73550 0.59030 0.72200 C96 C 0.5861(5) 0.57285(10) 0.7501(4) H119 H 0.54010 0.58350 0.71250 H120 H 0.58660 0.55970 0.71200 C97 C 0.3947(5) 0.52366(9) 1.0220(5) H121 H 0.47950 0.52140 1.03790 H122 H 0.36790 0.51320 0.97250 C98 C 0.3235(6) 0.52183(11) 1.1135(5) H123 H 0.24110 0.51770 1.09710 H124 H 0.35930 0.51160 1.16020 C99 C 0.3307(6) 0.54376(11) 1.1530(5) H125 H 0.26470 0.54680 1.19550 H126 H 0.40600 0.54620 1.19030 C100 C 0.3227(7) 0.55675(11) 1.0629(5) H127 H 0.23960 0.56010 1.04500 H128 H 0.36630 0.57010 1.07310 C101 C 0.3098(5) 0.53402(10) 0.6723(4) H129 H 0.31330 0.54800 0.64130 H130 H 0.22730 0.53110 0.68780 C102 C 0.3551(6) 0.51734(10) 0.6053(4) H131 H 0.34760 0.52190 0.53630 H132 H 0.31230 0.50390 0.61270 C103 C 0.4828(6) 0.51513(10) 0.6390(5) H133 H 0.51380 0.50110 0.62330 H134 H 0.53210 0.52600 0.60920 C104 C 0.4779(5) 0.51823(9) 0.7471(5) H135 H 0.45980 0.50480 0.77970 H136 H 0.55400 0.52360 0.77460 O12 O 0.2572(8) 0.57318(17) 0.830(3) C105 C 0.2581(10) 0.5947(2) 0.8202(15) H137 H 0.29960 0.59860 0.76100 H138 H 0.30080 0.60110 0.87730 C106 C 0.1364(9) 0.60291(17) 0.8128(10) H139 H 0.12110 0.61180 0.87000 H140 H 0.12460 0.61150 0.75320 C107 C 0.0575(11) 0.5851(2) 0.8091(11) H141 H 0.01560 0.58350 0.87040 H142 H -0.00050 0.58600 0.75340 C108 C 0.1394(9) 0.56814(18) 0.7966(11) H143 H 0.11270 0.55570 0.83260 H144 H 0.13930 0.56440 0.72660 O13? O 0.2603(14) 0.5739(3) 0.841(5) C109? C 0.1427(15) 0.5671(3) 0.855(2) H145? H 0.13580 0.56090 0.92050 H146? H 0.11780 0.55660 0.80510 C110? C 0.0712(17) 0.5862(3) 0.845(2) H147? H 0.05010 0.58910 0.77540 H148? H -0.00180 0.58490 0.88090 C111? C 0.1459(14) 0.6027(3) 0.8862(19) H149? H 0.13640 0.60410 0.95730 H150? H 0.12850 0.61640 0.85450 C112? C 0.2632(14) 0.5954(3) 0.8655(13) H151? H 0.29360 0.60360 0.81070 H152? H 0.31680 0.59760 0.92340 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Dy1 C1 2.545 1_555 1_555 Fe1 C1 2.094 1_555 1_555 Fe2 C11 2.103 1_555 1_555 Fe3 C21 2.093 1_555 1_555 Li1 O1 1.936 1_555 1_555 Li2 O2 1.925 1_555 1_555 O1 C31 1.440 1_555 1_555 O2 C35 1.436 1_555 1_555 C1 Li1 2.230 1_555 1_555 C2 Fe1 2.037 1_555 1_555 H1 C2 0.949 1_555 1_555 C3 Fe1 2.042 1_555 1_555 H2 C3 0.951 1_555 1_555 C4 Fe1 2.041 1_555 1_555 H3 C4 0.950 1_555 1_555 C5 Fe1 2.046 1_555 1_555 H4 C5 0.948 1_555 1_555 C6 Dy1 2.537 1_555 1_555 C7 Fe1 2.039 1_555 1_555 H5 C7 0.948 1_555 1_555 C8 Fe1 2.041 1_555 1_555 H6 C8 0.952 1_555 1_555 C9 Fe1 2.047 1_555 1_555 H7 C9 0.950 1_555 1_555 C10 Fe1 2.042 1_555 1_555 H8 C10 0.950 1_555 1_555 C11 Dy1 2.550 1_555 1_555 C12 Fe2 2.038 1_555 1_555 H9 C12 0.950 1_555 1_555 C13 Fe2 2.047 1_555 1_555 H10 C13 0.950 1_555 1_555 C14 Fe2 2.045 1_555 1_555 H11 C14 0.950 1_555 1_555 C15 Fe2 2.044 1_555 1_555 H12 C15 0.951 1_555 1_555 C16 Dy1 2.541 1_555 1_555 C17 Fe2 2.037 1_555 1_555 H13 C17 0.950 1_555 1_555 C18 Fe2 2.044 1_555 1_555 H14 C18 0.950 1_555 1_555 C19 Fe2 2.037 1_555 1_555 H15 C19 0.951 1_555 1_555 C20 Fe2 2.040 1_555 1_555 H16 C20 0.948 1_555 1_555 C21 Dy1 2.552 1_555 1_555 C22 Fe3 2.040 1_555 1_555 H17 C22 0.949 1_555 1_555 C23 Fe3 2.041 1_555 1_555 H18 C23 0.950 1_555 1_555 C24 Fe3 2.048 1_555 1_555 H19 C24 0.949 1_555 1_555 C25 Fe3 2.040 1_555 1_555 H20 C25 0.950 1_555 1_555 C26 Dy1 2.536 1_555 1_555 C27 Fe3 2.044 1_555 1_555 H21 C27 0.951 1_555 1_555 C28 Fe3 2.047 1_555 1_555 H22 C28 0.949 1_555 1_555 C29 Fe3 2.051 1_555 1_555 H23 C29 0.951 1_555 1_555 C30 Fe3 2.032 1_555 1_555 H24 C30 0.950 1_555 1_555 C31 H25 0.991 1_555 1_555 H26 C31 0.989 1_555 1_555 C32 C31 1.517 1_555 1_555 H27 C32 0.989 1_555 1_555 H28 C32 0.990 1_555 1_555 C33 C32 1.527 1_555 1_555 H29 C33 0.990 1_555 1_555 H30 C33 0.989 1_555 1_555 C34 O1 1.435 1_555 1_555 H31 C34 0.989 1_555 1_555 H32 C34 0.989 1_555 1_555 C35 H33 0.989 1_555 1_555 H34 C35 0.990 1_555 1_555 C36 C35 1.521 1_555 1_555 H35 C36 0.991 1_555 1_555 H36 C36 0.990 1_555 1_555 C37 C36 1.540 1_555 1_555 H37 C37 0.991 1_555 1_555 H38 C37 0.990 1_555 1_555 C38 O2 1.443 1_555 1_555 H39 C38 0.990 1_555 1_555 H40 C38 0.992 1_555 1_555 Dy2 C39 2.546 1_555 1_555 Fe4 C39 2.087 1_555 1_555 Fe5 C49 2.084 1_555 1_555 Fe6 C59 2.108 1_555 1_555 Li3 O3 1.943 1_555 1_555 Li4 O4 1.942 1_555 1_555 O3 C69 1.437 1_555 1_555 O4 C73 1.439 1_555 1_555 C39 Li3 2.174 1_555 1_555 C40 Fe4 2.038 1_555 1_555 H41 C40 0.950 1_555 1_555 C41 Fe4 2.045 1_555 1_555 H42 C41 0.949 1_555 1_555 C42 Fe4 2.040 1_555 1_555 H43 C42 0.949 1_555 1_555 C43 Fe4 2.038 1_555 1_555 H44 C43 0.950 1_555 1_555 C44 Dy2 2.532 1_555 1_555 C45 Fe4 2.050 1_555 1_555 H45 C45 0.950 1_555 1_555 C46 Fe4 2.036 1_555 1_555 H46 C46 0.950 1_555 1_555 C47 Fe4 2.034 1_555 1_555 H47 C47 0.952 1_555 1_555 C48 Fe4 2.031 1_555 1_555 H48 C48 0.950 1_555 1_555 C49 Dy2 2.554 1_555 1_555 C50 Fe5 2.052 1_555 1_555 H49 C50 0.949 1_555 1_555 C51 Fe5 2.047 1_555 1_555 H50 C51 0.950 1_555 1_555 C52 Fe5 2.029 1_555 1_555 H51 C52 0.949 1_555 1_555 C53 Fe5 2.028 1_555 1_555 H52 C53 0.949 1_555 1_555 C54 Dy2 2.542 1_555 1_555 C55 Fe5 2.044 1_555 1_555 H53 C55 0.950 1_555 1_555 C56 Fe5 2.039 1_555 1_555 H54 C56 0.952 1_555 1_555 C57 Fe5 2.036 1_555 1_555 H55 C57 0.951 1_555 1_555 C58 Fe5 2.050 1_555 1_555 H56 C58 0.950 1_555 1_555 C59 Dy2 2.546 1_555 1_555 C60 Fe6 2.039 1_555 1_555 H57 C60 0.949 1_555 1_555 C61 Fe6 2.050 1_555 1_555 H58 C61 0.950 1_555 1_555 C62 Fe6 2.044 1_555 1_555 H59 C62 0.951 1_555 1_555 C63 Fe6 2.033 1_555 1_555 H60 C63 0.950 1_555 1_555 C64 Dy2 2.564 1_555 1_555 C65 Fe6 2.054 1_555 1_555 H61 C65 0.951 1_555 1_555 C66 Fe6 2.051 1_555 1_555 H62 C66 0.951 1_555 1_555 C67 Fe6 2.053 1_555 1_555 H63 C67 0.950 1_555 1_555 C68 Fe6 2.049 1_555 1_555 H64 C68 0.950 1_555 1_555 C69 H65 0.989 1_555 1_555 H66 C69 0.989 1_555 1_555 C70 C69 1.533 1_555 1_555 H67 C70 0.989 1_555 1_555 H68 C70 0.988 1_555 1_555 C71 C70 1.539 1_555 1_555 H69 C71 0.989 1_555 1_555 H70 C71 0.990 1_555 1_555 C72 O3 1.439 1_555 1_555 H71 C72 0.992 1_555 1_555 H72 C72 0.991 1_555 1_555 C73 H73 0.990 1_555 1_555 H74 C73 0.991 1_555 1_555 C74 C73 1.514 1_555 1_555 H75 C74 0.989 1_555 1_555 H76 C74 0.991 1_555 1_555 C75 C74 1.535 1_555 1_555 H77 C75 0.987 1_555 1_555 H78 C75 0.991 1_555 1_555 C76 O4 1.437 1_555 1_555 H79 C76 0.990 1_555 1_555 H80 C76 0.988 1_555 1_555 Li5 O5 1.944 1_555 1_555 O5 C77 1.438 1_555 1_555 O6 Li5 1.959 1_555 1_555 O7 Li5 1.969 1_555 1_555 O8 Li5 1.958 1_555 1_555 C77 H81 0.988 1_555 1_555 H82 C77 0.990 1_555 1_555 C78 C77 1.512 1_555 1_555 H83 C78 0.992 1_555 1_555 H84 C78 0.989 1_555 1_555 C79 C78 1.506 1_555 1_555 H85 C79 0.991 1_555 1_555 H86 C79 0.990 1_555 1_555 C80 O5 1.456 1_555 1_555 H87 C80 0.992 1_555 1_555 H88 C80 0.990 1_555 1_555 C81 O6 1.437 1_555 1_555 H89 C81 0.991 1_555 1_555 H90 C81 0.988 1_555 1_555 C82 C81 1.494 1_555 1_555 H91 C82 0.991 1_555 1_555 H92 C82 0.989 1_555 1_555 C83 C82 1.420 1_555 1_555 H93 C83 0.990 1_555 1_555 H94 C83 0.991 1_555 1_555 C84 O6 1.443 1_555 1_555 H95 C84 0.992 1_555 1_555 H96 C84 0.989 1_555 1_555 C85 O7 1.451 1_555 1_555 H97 C85 0.990 1_555 1_555 H98 C85 0.988 1_555 1_555 C86 C85 1.500 1_555 1_555 H99 C86 0.991 1_555 1_555 H100 C86 0.992 1_555 1_555 C87 C86 1.522 1_555 1_555 H101 C87 0.988 1_555 1_555 H102 C87 0.991 1_555 1_555 C88 O7 1.435 1_555 1_555 H103 C88 0.990 1_555 1_555 H104 C88 0.989 1_555 1_555 C89 O8 1.450 1_555 1_555 H105 C89 0.990 1_555 1_555 H106 C89 0.991 1_555 1_555 C90 C89 1.505 1_555 1_555 H107 C90 0.992 1_555 1_555 H108 C90 0.991 1_555 1_555 C91 C90 1.518 1_555 1_555 H109 C91 0.990 1_555 1_555 H110 C91 0.989 1_555 1_555 C92 O8 1.441 1_555 1_555 H111 C92 0.988 1_555 1_555 H112 C92 0.990 1_555 1_555 Li6 O9 1.932 1_555 1_555 O9 C93 1.442 1_555 1_555 O10 Li6 1.925 1_555 1_555 O11 Li6 1.902 1_555 1_555 C93 H113 0.991 1_555 1_555 H114 C93 0.991 1_555 1_555 C94 C93 1.524 1_555 1_555 H115 C94 0.989 1_555 1_555 H116 C94 0.990 1_555 1_555 C95 C94 1.499 1_555 1_555 H117 C95 0.991 1_555 1_555 H118 C95 0.991 1_555 1_555 C96 O9 1.433 1_555 1_555 H119 C96 0.988 1_555 1_555 H120 C96 0.987 1_555 1_555 C97 O10 1.434 1_555 1_555 H121 C97 0.990 1_555 1_555 H122 C97 0.990 1_555 1_555 C98 C97 1.529 1_555 1_555 H123 C98 0.990 1_555 1_555 H124 C98 0.989 1_555 1_555 C99 C98 1.499 1_555 1_555 H125 C99 0.991 1_555 1_555 H126 C99 0.991 1_555 1_555 C100 O10 1.442 1_555 1_555 H127 C100 0.990 1_555 1_555 H128 C100 0.991 1_555 1_555 C101 O11 1.454 1_555 1_555 H129 C101 0.988 1_555 1_555 H130 C101 0.990 1_555 1_555 C102 C101 1.511 1_555 1_555 H131 C102 0.991 1_555 1_555 H132 C102 0.992 1_555 1_555 C103 C102 1.512 1_555 1_555 H133 C103 0.988 1_555 1_555 H134 C103 0.991 1_555 1_555 C104 O11 1.440 1_555 1_555 H135 C104 0.991 1_555 1_555 H136 C104 0.990 1_555 1_555 O12 Li6 1.930 1_555 1_555 C105 O12 1.377 1_555 1_555 H137 C105 0.990 1_555 1_555 H138 C105 0.991 1_555 1_555 C106 C105 1.480 1_555 1_555 H139 C106 0.990 1_555 1_555 H140 C106 0.988 1_555 1_555 C107 C106 1.446 1_555 1_555 H141 C107 0.991 1_555 1_555 H142 C107 0.989 1_555 1_555 C108 O12 1.434 1_555 1_555 H143 C108 0.989 1_555 1_555 H144 C108 0.990 1_555 1_555 Fe1 C6 2.089 1_555 1_555 Fe2 C16 2.101 1_555 1_555 Fe3 C26 2.103 1_555 1_555 Li1 C11 2.201 1_555 1_555 Li1 C21 2.232 1_555 1_555 Li2 C6 2.223 1_555 1_555 Li2 C16 2.216 1_555 1_555 Li2 C26 2.258 1_555 1_555 C1 C2 1.448 1_555 1_555 C1 C5 1.452 1_555 1_555 C2 C3 1.432 1_555 1_555 C3 C4 1.416 1_555 1_555 C4 C5 1.419 1_555 1_555 C6 C7 1.452 1_555 1_555 C6 C10 1.449 1_555 1_555 C7 C8 1.431 1_555 1_555 C8 C9 1.413 1_555 1_555 C9 C10 1.428 1_555 1_555 C11 C12 1.456 1_555 1_555 C11 C15 1.450 1_555 1_555 C12 C13 1.436 1_555 1_555 C13 C14 1.426 1_555 1_555 C14 C15 1.439 1_555 1_555 C16 C17 1.437 1_555 1_555 C16 C20 1.460 1_555 1_555 C17 C18 1.433 1_555 1_555 C18 C19 1.421 1_555 1_555 C19 C20 1.425 1_555 1_555 C21 C22 1.446 1_555 1_555 C21 C25 1.456 1_555 1_555 C22 C23 1.425 1_555 1_555 C23 C24 1.414 1_555 1_555 C24 C25 1.424 1_555 1_555 C26 C27 1.452 1_555 1_555 C26 C30 1.447 1_555 1_555 C27 C28 1.430 1_555 1_555 C28 C29 1.421 1_555 1_555 C29 C30 1.429 1_555 1_555 C33 C34 1.522 1_555 1_555 C37 C38 1.516 1_555 1_555 Fe4 C44 2.100 1_555 1_555 Fe5 C54 2.092 1_555 1_555 Fe6 C64 2.099 1_555 1_555 Li3 C49 2.182 1_555 1_555 Li3 C59 2.198 1_555 1_555 Li4 C44 2.245 1_555 1_555 Li4 C54 2.236 1_555 1_555 Li4 C64 2.248 1_555 1_555 C39 C40 1.440 1_555 1_555 C39 C43 1.460 1_555 1_555 C40 C41 1.418 1_555 1_555 C41 C42 1.420 1_555 1_555 C42 C43 1.422 1_555 1_555 C44 C45 1.445 1_555 1_555 C44 C48 1.447 1_555 1_555 C45 C46 1.424 1_555 1_555 C46 C47 1.420 1_555 1_555 C47 C48 1.426 1_555 1_555 C49 C50 1.442 1_555 1_555 C49 C53 1.452 1_555 1_555 C50 C51 1.421 1_555 1_555 C51 C52 1.410 1_555 1_555 C52 C53 1.435 1_555 1_555 C54 C55 1.447 1_555 1_555 C54 C58 1.444 1_555 1_555 C55 C56 1.433 1_555 1_555 C56 C57 1.420 1_555 1_555 C57 C58 1.435 1_555 1_555 C59 C60 1.441 1_555 1_555 C59 C63 1.444 1_555 1_555 C60 C61 1.417 1_555 1_555 C61 C62 1.404 1_555 1_555 C62 C63 1.430 1_555 1_555 C64 C65 1.447 1_555 1_555 C64 C68 1.454 1_555 1_555 C65 C66 1.429 1_555 1_555 C66 C67 1.419 1_555 1_555 C67 C68 1.433 1_555 1_555 C71 C72 1.520 1_555 1_555 C75 C76 1.503 1_555 1_555 C79 C80 1.501 1_555 1_555 C83 C84 1.500 1_555 1_555 C87 C88 1.518 1_555 1_555 C91 C92 1.519 1_555 1_555 C95 C96 1.512 1_555 1_555 C99 C100 1.487 1_555 1_555 C103 C104 1.501 1_555 1_555 C107 C108 1.442 1_555 1_555 #END data_CSD_CIF_ZOQPUQ _audit_creation_date 1996-09-23 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD ZOQPUQ _chemical_formula_sum 'C34 H30 Na1 P1' _chemical_formula_moiety ; C10 H10 Na1 1-,C24 H20 P1 1+ ; _journal_coden_Cambridge 579 _journal_volume 15 _journal_year 1996 _journal_page_first 118 _journal_name_full 'Organometallics ' loop_ _publ_author_name "S.Harder" "M.H.Prosenc" "U.Rief" _chemical_name_systematic ; Tetraphenylphosphonium bis(\h^5^-cyclopentadienyl)-sodium ; _cell_volume 1348.318 _exptl_crystal_colour 'orange-brown' _exptl_crystal_density_diffrn 1.213 _exptl_special_details ; Atomic coordinates for cation not reported ; _diffrn_ambient_temperature 233.15 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.042 _refine_ls_wR_factor_gt 0.042 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,-1/2+z _cell_length_a 10.974(4) _cell_length_b 7.007(3) _cell_length_c 17.961(6) _cell_angle_alpha 90 _cell_angle_beta 102.51(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 Na 1.61 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Na1 Na 1.00000 0.50000 0.50000 C1 C 0.8252(3) 0.4720(5) 0.5784(2) C2 C 0.9268(3) 0.4050(6) 0.6275(1) C3 C 0.9604(2) 0.2375(5) 0.5994(2) C4 C 0.8769(3) 0.2038(5) 0.5322(2) C5 C 0.7953(2) 0.3487(7) 0.5209(2) C1B C 1.1748(3) 0.5280(5) 0.4216(2) C2B C 1.0732(3) 0.5950(6) 0.3725(1) C3B C 1.0396(2) 0.7625(5) 0.4006(2) C4B C 1.1231(3) 0.7962(5) 0.4678(2) C5B C 1.2047(2) 0.6513(7) 0.4791(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Na1 C1 2.621 1_555 1_555 C1 C2 1.347 1_555 1_555 C2 Na1 2.670 1_555 1_555 C3 Na1 2.664 1_555 1_555 C4 Na1 2.609 1_555 1_555 C5 Na1 2.584 1_555 1_555 C1B Na1 2.621 1_555 1_555 C2B Na1 2.670 1_555 1_555 C3B Na1 2.664 1_555 1_555 C4B Na1 2.609 1_555 1_555 C5B Na1 2.584 1_555 1_555 C1 C5 1.332 1_555 1_555 C2 C3 1.360 1_555 1_555 C3 C4 1.369 1_555 1_555 C4 C5 1.340 1_555 1_555 C1B C2B 1.347 1_555 1_555 C1B C5B 1.332 1_555 1_555 C2B C3B 1.360 1_555 1_555 C3B C4B 1.369 1_555 1_555 C4B C5B 1.340 1_555 1_555 #END data_CSD_CIF_ZOZPUZ10 _audit_creation_date 1996-10-31 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD ZOZPUZ10 _chemical_formula_sum 'C43 H111 B8 Cl2 Ho1 Li3 N8 Si4' _chemical_formula_moiety ; C28 H76 B8 Cl2 Ho1 Li2 N4 Si4 1-,C12 H32 Li1 N4 1+,0.5(C6 H6) ; _journal_coden_Cambridge 579 _journal_volume 15 _journal_year 1996 _journal_page_first 1006 _journal_name_full 'Organometallics ' loop_ _publ_author_name "N.S.Hosmane" "Ying Wang" "Hongming Zhang" "J.A.Maguire" "M.McInnis" "T.G.Gray" "J.D.Collins" "R.K.Kremer" "H.Binder" "E.Waldhor" "W.Kaim" _chemical_name_systematic ; bis(Tetramethylethylenediamine)-lithium 1-chloro-1-(\m~2~-chloro)-2,2',3,3'-tetrakis(trimethylsilyl)-5,6-(bis(\m~2~-hy drido)-tetramethylethylenediamine-lithium)-4,4',5'-(tris(\m~2~-hydrido)-(tetra methylethylenediamine)-lithium)-1,1'-commo-holmium(iii)-bis(2,3-dicarbahexabor ane) benzene solvate ; _cell_volume 7164.697 _exptl_crystal_density_diffrn 1.109 _exptl_special_details ; Air-sensitive ; _diffrn_ambient_temperature 230 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.05 _refine_ls_wR_factor_gt 0.05 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 -1/2+x,-1/2-y,-1/2+z _cell_length_a 14.708(2) _cell_length_b 21.098(4) _cell_length_c 23.127(3) _cell_angle_alpha 90 _cell_angle_beta 93.29(1) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 B 0.83 Cl 0.99 Ho 1.74 Li 1.44 N 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Ho1 Ho 0.02952(2) 0.241539(13) 0.850762(13) Cl1 Cl 0.04919(13) 0.28578(9) 0.95626(8) Cl2 Cl 0.02419(13) 0.35310(8) 0.79623(8) Si1 Si 0.29582(14) 0.29591(10) 0.89669(9) Si2 Si 0.2299(2) 0.12479(10) 0.94137(11) Si3 Si -0.22011(15) 0.32435(10) 0.86488(11) Si4 Si -0.1636(2) 0.17855(12) 0.96194(10) C1 C 0.2147(4) 0.2376(3) 0.8619(3) C2 C 0.1849(5) 0.1724(3) 0.8776(3) B1 B 0.1330(6) 0.1396(4) 0.8248(4) H1 H 0.12040 0.08310 0.82170 B2 B 0.1367(6) 0.1889(5) 0.7697(4) H2 H 0.12610 0.17680 0.71620 B3 B 0.1884(5) 0.2526(4) 0.7975(3) H3 H 0.20300 0.29680 0.77600 B4 B 0.2387(7) 0.1793(4) 0.8149(4) H4 H 0.30510 0.16010 0.80260 C3 C -0.1514(4) 0.2525(3) 0.8498(3) C4 C -0.1270(4) 0.1977(3) 0.8881(3) B5 B -0.0867(6) 0.1430(4) 0.8542(3) H5 H -0.06680 0.08840 0.86520 B6 B -0.0908(6) 0.1658(4) 0.7855(4) H6 H -0.07830 0.13680 0.73920 B7 B -0.1301(5) 0.2376(4) 0.7859(3) H7 H -0.15800 0.25680 0.74480 B8 B -0.1882(6) 0.1809(4) 0.8255(4) H8 H -0.25820 0.16200 0.81780 C5 C 0.3260(6) 0.2862(4) 0.9760(3) H9 H 0.3532(6) 0.2449(4) 0.9829(3) H10 H 0.2713(6) 0.2899(4) 0.9973(3) H11 H 0.3690(6) 0.3189(4) 0.9887(3) C6 C 0.2452(5) 0.3760(3) 0.8899(3) H12 H 0.2869(5) 0.4068(3) 0.9079(3) H13 H 0.1882(5) 0.3769(3) 0.9090(3) H14 H 0.2339(5) 0.3864(3) 0.8493(3) C7 C 0.4039(5) 0.2946(4) 0.8578(4) H15 H 0.4310(5) 0.2528(4) 0.8611(4) H16 H 0.4459(5) 0.3257(4) 0.8749(4) H17 H 0.3907(5) 0.3046(4) 0.8172(4) C8 C 0.1985(6) 0.1560(4) 1.0131(3) H18 H 0.2220(6) 0.1987(4) 1.0183(3) H19 H 0.2244(6) 0.1289(4) 1.0436(3) H20 H 0.1327(6) 0.1566(4) 1.0145(3) C9 C 0.3571(6) 0.1162(5) 0.9406(4) H21 H 0.3730(6) 0.0999(5) 0.9032(4) H22 H 0.3783(6) 0.0869(5) 0.9708(4) H23 H 0.3856(6) 0.1571(5) 0.9473(4) C10 C 0.1808(8) 0.0432(4) 0.9370(4) H24 H 0.1947(8) 0.0239(4) 0.9005(4) H25 H 0.1153(8) 0.0454(4) 0.9396(4) H26 H 0.2070(8) 0.0178(4) 0.9687(4) C11 C -0.1593(6) 0.3790(4) 0.9172(4) H27 H -0.1464(6) 0.3572(4) 0.9537(4) H28 H -0.1973(6) 0.4157(4) 0.9235(4) H29 H -0.1027(6) 0.3927(4) 0.9017(4) C12 C -0.3358(5) 0.3043(5) 0.8897(4) H30 H -0.3293(5) 0.2791(5) 0.9248(4) H31 H -0.3694(5) 0.2803(5) 0.8597(4) H32 H -0.3684(5) 0.3430(5) 0.8974(4) C13 C -0.2399(6) 0.3722(4) 0.7980(4) H33 H -0.2717(6) 0.3467(4) 0.7684(4) H34 H -0.1819(6) 0.3859(4) 0.7844(4) H35 H -0.2766(6) 0.4090(4) 0.8063(4) C14 C -0.1809(6) 0.2478(4) 1.0096(3) H36 H -0.2267(6) 0.2756(4) 0.9914(3) H37 H -0.1240(6) 0.2707(4) 1.0158(3) H38 H -0.2012(6) 0.2332(4) 1.0466(3) C15 C -0.2718(7) 0.1308(5) 0.9545(4) H39 H -0.3190(7) 0.1555(5) 0.9340(4) H40 H -0.2911(7) 0.1199(5) 0.9927(4) H41 H -0.2611(7) 0.0923(5) 0.9330(4) C16 C -0.0756(7) 0.1296(4) 1.0012(4) H42 H -0.0633(7) 0.0923(4) 0.9784(4) H43 H -0.0973(7) 0.1167(4) 1.0382(4) H44 H -0.0202(7) 0.1541(4) 1.0075(4) Li1 Li 0.0056(9) 0.0779(6) 0.7848(6) Li2 Li 0.0918(9) 0.2976(7) 0.7212(6) Li3 Li 0.0479(8) 0.3836(5) 1.1667(6) N1 N -0.0495(5) -0.0160(3) 0.8083(3) N2 N 0.0452(6) 0.0292(4) 0.7084(4) C17 C -0.0148(9) -0.0588(4) 0.7647(6) H45 H -0.0545(9) -0.0961(4) 0.7611(6) H46 H 0.0462(9) -0.0733(4) 0.7780(6) C18 C -0.0100(9) -0.0284(6) 0.7067(6) H47 H 0.0158(9) -0.0587(6) 0.6800(6) H48 H -0.0718(9) -0.0180(6) 0.6916(6) C19 C -0.0229(8) -0.0416(4) 0.8658(5) H49 H -0.0452(8) -0.0139(4) 0.8953(5) H50 H 0.0429(8) -0.0443(4) 0.8704(5) H51 H -0.0489(8) -0.0835(4) 0.8696(5) C20 C -0.1491(6) -0.0108(4) 0.8023(4) H52 H -0.1699(6) 0.0178(4) 0.8316(4) H53 H -0.1760(6) -0.0523(4) 0.8071(4) H54 H -0.1673(6) 0.0056(4) 0.7642(4) C21 C 0.0244(9) 0.0636(6) 0.6529(5) H55 H -0.0406(9) 0.0715(6) 0.6482(5) H56 H 0.0434(9) 0.0381(6) 0.6209(5) H57 H 0.0569(9) 0.1037(6) 0.6536(5) C22 C 0.1424(7) 0.0180(5) 0.7146(5) H58 H 0.1744(7) 0.0582(5) 0.7154(5) H59 H 0.1610(7) -0.0071(5) 0.6822(5) H60 H 0.1568(7) -0.0047(5) 0.7505(5) N3 N 0.0059(6) 0.2966(5) 0.6425(3) N4 N 0.1834(5) 0.3506(4) 0.6697(3) C23 C 0.0650(9) 0.3177(7) 0.5978(4) H61 H 0.0978(9) 0.2810(7) 0.5835(4) H62 H 0.0272(9) 0.3350(7) 0.5653(4) C24 C 0.1297(9) 0.3646(7) 0.6171(5) H63 H 0.0969(9) 0.4043(7) 0.6228(5) H64 H 0.1713(9) 0.3717(7) 0.5862(5) C25 C -0.0329(9) 0.2361(6) 0.6303(4) H65 H 0.0153(9) 0.2053(6) 0.6263(4) H66 H -0.0706(9) 0.2381(6) 0.5946(4) H67 H -0.0698(9) 0.2236(6) 0.6618(4) C26 C -0.0688(8) 0.3411(6) 0.6481(5) H68 H -0.0445(8) 0.3831(6) 0.6564(5) H69 H -0.1055(8) 0.3277(6) 0.6794(5) H70 H -0.1063(8) 0.3422(6) 0.6122(5) C27 C 0.2621(8) 0.3128(7) 0.6590(5) H71 H 0.2428(8) 0.2738(7) 0.6398(5) H72 H 0.2950(8) 0.3030(7) 0.6954(5) H73 H 0.3015(8) 0.3362(7) 0.6344(5) C28 C 0.2130(8) 0.4085(5) 0.6982(5) H74 H 0.1604(8) 0.4343(5) 0.7056(5) H75 H 0.2526(8) 0.4317(5) 0.6735(5) H76 H 0.2460(8) 0.3985(5) 0.7345(5) N5 N -0.0720(5) 0.4280(4) 1.1327(4) N6 N 0.0309(6) 0.4317(4) 1.2467(3) C29 C -0.0886(9) 0.4741(7) 1.1761(9) H77 H -0.0584(9) 0.5136(7) 1.1657(9) H78 H -0.1542(9) 0.4826(7) 1.1748(9) C30 C -0.0604(11) 0.4592(7) 1.2330(6) H79 H -0.1051(11) 0.4296(7) 1.2474(6) H80 H -0.0644(11) 0.4982(7) 1.2558(6) C31 C -0.1453(8) 0.3846(6) 1.1242(6) H81 H -0.1313(8) 0.3542(6) 1.0945(6) H82 H -0.2003(8) 0.4075(6) 1.1121(6) H83 H -0.1544(8) 0.3624(6) 1.1601(6) C32 C -0.0659(10) 0.4610(8) 1.0774(7) H84 H -0.0166(10) 0.4915(8) 1.0805(7) H85 H -0.1228(10) 0.4828(8) 1.0677(7) H86 H -0.0543(10) 0.4304(8) 1.0473(7) C33 C 0.0227(7) 0.3941(6) 1.2983(4) H87 H -0.0248(7) 0.3626(6) 1.2914(4) H88 H 0.0072(7) 0.4214(6) 1.3300(4) H89 H 0.0801(7) 0.3730(6) 1.3081(4) C34 C 0.1012(10) 0.4795(6) 1.2551(6) H90 H 0.1052(10) 0.5039(6) 1.2198(6) H91 H 0.1593(10) 0.4590(6) 1.2646(6) H92 H 0.0864(10) 0.5074(6) 1.2864(6) N7 N 0.1689(5) 0.3894(4) 1.1212(3) N8 N 0.0677(6) 0.2854(3) 1.1695(4) C35 C 0.1901(10) 0.3209(7) 1.1150(6) H93 H 0.1663(10) 0.3072(7) 1.0766(6) H94 H 0.2565(10) 0.3163(7) 1.1159(6) C36 C 0.1582(12) 0.2801(7) 1.1546(9) H95 H 0.1970(12) 0.2845(7) 1.1903(9) H96 H 0.1668(12) 0.2370(7) 1.1402(9) C37 C 0.1585(8) 0.4169(5) 1.0640(4) H97 H 0.1113(8) 0.3943(5) 1.0413(4) H98 H 0.2156(8) 0.4137(5) 1.0452(4) H99 H 0.1415(8) 0.4611(5) 1.0671(4) C38 C 0.2400(7) 0.4242(7) 1.1541(5) H100 H 0.2481(7) 0.4064(7) 1.1928(5) H101 H 0.2225(7) 0.4684(7) 1.1568(5) H102 H 0.2966(7) 0.4209(7) 1.1348(5) C39 C 0.0075(8) 0.2516(4) 1.1294(5) H103 H -0.0547(8) 0.2560(4) 1.1407(5) H104 H 0.0241(8) 0.2071(4) 1.1295(5) H105 H 0.0124(8) 0.2688(4) 1.0908(5) C40 C 0.0663(12) 0.2554(5) 1.2266(5) H106 H 0.0051(12) 0.2571(5) 1.2400(5) H107 H 0.1077(12) 0.2776(5) 1.2537(5) H108 H 0.0852(12) 0.2115(5) 1.2237(5) C41 C 0.5790(6) 0.5328(7) -0.0006(6) H109 H 0.6333(6) 0.5560(7) -0.0026(6) C42 C 0.5019(11) 0.5622(3) 0.0142(6) H110 H 0.5037(11) 0.6050(3) 0.0258(6) C43 C 0.5779(7) 0.4700(7) -0.0124(6) H111 H 0.6324(7) 0.4487(7) -0.0193(6) C43B C 0.4221(7) 0.5300(7) 0.0124(6) C41B C 0.4210(6) 0.4672(7) 0.0006(6) H109B H 0.3667(6) 0.4440(7) 0.0026(6) C42B C 0.4981(11) 0.4378(3) -0.0142(6) H110B H 0.4963(11) 0.3950(3) -0.0258(6) H111B H 0.3676(7) 0.5513(7) 0.0193(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ho1 Cl1 2.613 1_555 1_555 Cl2 Ho1 2.669 1_555 1_555 Si1 C1 1.864 1_555 1_555 Si2 C2 1.874 1_555 1_555 Si3 C3 1.866 1_555 1_555 Si4 C4 1.864 1_555 1_555 C1 Ho1 2.722 1_555 1_555 C2 Ho1 2.752 1_555 1_555 B1 Ho1 2.722 1_555 1_555 H1 B1 1.208 1_555 1_555 B2 Ho1 2.752 1_555 1_555 H2 B2 1.264 1_555 1_555 B3 Ho1 2.713 1_555 1_555 H3 B3 1.084 1_555 1_555 B4 C1 1.692 1_555 1_555 H4 B4 1.109 1_555 1_555 C3 Ho1 2.670 1_555 1_555 C4 Ho1 2.670 1_555 1_555 B5 Ho1 2.696 1_555 1_555 H5 B5 1.212 1_555 1_555 B6 Ho1 2.767 1_555 1_555 H6 B6 1.256 1_555 1_555 B7 Ho1 2.714 1_555 1_555 H7 B7 1.091 1_555 1_555 B8 C3 1.690 1_555 1_555 H8 B8 1.109 1_555 1_555 C5 Si1 1.873 1_555 1_555 H9 C5 0.968 1_555 1_555 H10 C5 0.970 1_555 1_555 H11 C5 0.970 1_555 1_555 C6 Si1 1.850 1_555 1_555 H12 C6 0.971 1_555 1_555 H13 C6 0.970 1_555 1_555 H14 C6 0.969 1_555 1_555 C7 Si1 1.871 1_555 1_555 H15 C7 0.969 1_555 1_555 H16 C7 0.970 1_555 1_555 H17 C7 0.971 1_555 1_555 C8 Si2 1.867 1_555 1_555 H18 C8 0.970 1_555 1_555 H19 C8 0.969 1_555 1_555 H20 C8 0.970 1_555 1_555 C9 Si2 1.881 1_555 1_555 H21 C9 0.972 1_555 1_555 H22 C9 0.971 1_555 1_555 H23 C9 0.968 1_555 1_555 C10 Si2 1.867 1_555 1_555 H24 C10 0.970 1_555 1_555 H25 C10 0.970 1_555 1_555 H26 C10 0.970 1_555 1_555 C11 Si3 1.863 1_555 1_555 H27 C11 0.970 1_555 1_555 H28 C11 0.971 1_555 1_555 H29 C11 0.969 1_555 1_555 C12 Si3 1.875 1_555 1_555 H30 C12 0.970 1_555 1_555 H31 C12 0.971 1_555 1_555 H32 C12 0.969 1_555 1_555 C13 Si3 1.856 1_555 1_555 H33 C13 0.970 1_555 1_555 H34 C13 0.970 1_555 1_555 H35 C13 0.971 1_555 1_555 C14 Si4 1.856 1_555 1_555 H36 C14 0.971 1_555 1_555 H37 C14 0.970 1_555 1_555 H38 C14 0.972 1_555 1_555 C15 Si4 1.883 1_555 1_555 H39 C15 0.970 1_555 1_555 H40 C15 0.971 1_555 1_555 H41 C15 0.970 1_555 1_555 C16 Si4 1.852 1_555 1_555 H42 C16 0.970 1_555 1_555 H43 C16 0.969 1_555 1_555 H44 C16 0.969 1_555 1_555 Li1 B1 2.421 1_555 1_555 Li2 Cl2 2.360 1_555 1_555 Li3 N5 2.109 1_555 1_555 N1 Li1 2.220 1_555 1_555 N2 Li1 2.153 1_555 1_555 C17 N1 1.467 1_555 1_555 H45 C17 0.981 1_555 1_555 H46 C17 0.981 1_555 1_555 C18 N2 1.461 1_555 1_555 H47 C18 0.980 1_555 1_555 H48 C18 0.980 1_555 1_555 C19 N1 1.467 1_555 1_555 H49 C19 0.970 1_555 1_555 H50 C19 0.969 1_555 1_555 H51 C19 0.969 1_555 1_555 C20 N1 1.468 1_555 1_555 H52 C20 0.970 1_555 1_555 H53 C20 0.970 1_555 1_555 H54 C20 0.970 1_555 1_555 C21 N2 1.491 1_555 1_555 H55 C21 0.970 1_555 1_555 H56 C21 0.969 1_555 1_555 H57 C21 0.971 1_555 1_555 C22 N2 1.448 1_555 1_555 H58 C22 0.970 1_555 1_555 H59 C22 0.970 1_555 1_555 H60 C22 0.971 1_555 1_555 N3 Li2 2.155 1_555 1_555 N4 Li2 2.161 1_555 1_555 C23 N3 1.458 1_555 1_555 H61 C23 0.980 1_555 1_555 H62 C23 0.979 1_555 1_555 C24 N4 1.442 1_555 1_555 H63 C24 0.979 1_555 1_555 H64 C24 0.979 1_555 1_555 C25 N3 1.420 1_555 1_555 H65 C25 0.970 1_555 1_555 H66 C25 0.969 1_555 1_555 H67 C25 0.970 1_555 1_555 C26 N3 1.457 1_555 1_555 H68 C26 0.971 1_555 1_555 H69 C26 0.970 1_555 1_555 H70 C26 0.970 1_555 1_555 C27 N4 1.439 1_555 1_555 H71 C27 0.970 1_555 1_555 H72 C27 0.969 1_555 1_555 H73 C27 0.970 1_555 1_555 C28 N4 1.443 1_555 1_555 H74 C28 0.969 1_555 1_555 H75 C28 0.971 1_555 1_555 H76 C28 0.969 1_555 1_555 N5 C29 1.429 1_555 1_555 N6 Li3 2.137 1_555 1_555 C29 H77 0.981 1_555 1_555 H78 C29 0.980 1_555 1_555 C30 N6 1.480 1_555 1_555 H79 C30 0.979 1_555 1_555 H80 C30 0.981 1_555 1_555 C31 N5 1.420 1_555 1_555 H81 C31 0.970 1_555 1_555 H82 C31 0.970 1_555 1_555 H83 C31 0.969 1_555 1_555 C32 N5 1.463 1_555 1_555 H84 C32 0.969 1_555 1_555 H85 C32 0.970 1_555 1_555 H86 C32 0.972 1_555 1_555 C33 N6 1.444 1_555 1_555 H87 C33 0.971 1_555 1_555 H88 C33 0.970 1_555 1_555 H89 C33 0.970 1_555 1_555 C34 N6 1.449 1_555 1_555 H90 C34 0.970 1_555 1_555 H91 C34 0.972 1_555 1_555 H92 C34 0.967 1_555 1_555 N7 Li3 2.122 1_555 1_555 N8 Li3 2.093 1_555 1_555 C35 N7 1.487 1_555 1_555 H93 C35 0.979 1_555 1_555 H94 C35 0.980 1_555 1_555 C36 N8 1.398 1_555 1_555 H95 C36 0.981 1_555 1_555 H96 C36 0.979 1_555 1_555 C37 N7 1.445 1_555 1_555 H97 C37 0.971 1_555 1_555 H98 C37 0.970 1_555 1_555 H99 C37 0.969 1_555 1_555 C38 N7 1.456 1_555 1_555 H100 C38 0.972 1_555 1_555 H101 C38 0.970 1_555 1_555 H102 C38 0.969 1_555 1_555 C39 N8 1.435 1_555 1_555 H103 C39 0.970 1_555 1_555 H104 C39 0.970 1_555 1_555 H105 C39 0.970 1_555 1_555 C40 N8 1.466 1_555 1_555 H106 C40 0.969 1_555 1_555 H107 C40 0.969 1_555 1_555 H108 C40 0.970 1_555 1_555 C41 H109 0.940 1_555 1_555 C42 C41 1.354 1_555 1_555 H110 C42 0.942 1_555 1_555 C43 C41 1.353 1_555 1_555 H111 C43 0.941 1_555 1_555 C43B C42 1.355 1_555 1_555 C41B C43B 1.353 1_555 1_555 H109B C41B 0.940 1_555 1_555 C42B C43 1.355 1_555 1_555 H110B C42B 0.942 1_555 1_555 H111B C43B 0.941 1_555 1_555 C1 C2 1.495 1_555 1_555 C1 B3 1.550 1_555 1_555 C2 B4 1.698 1_555 1_555 C2 B1 1.564 1_555 1_555 B1 B2 1.648 1_555 1_555 B1 B4 1.792 1_555 1_555 H1 Li1 1.851 1_555 1_555 B2 B4 1.790 1_555 1_555 B2 B3 1.656 1_555 1_555 B2 Li2 2.621 1_555 1_555 H2 Li2 2.602 1_555 1_555 B3 Li2 2.397 1_555 1_555 B3 B4 1.751 1_555 1_555 H3 Li2 2.011 1_555 1_555 C3 C4 1.488 1_555 1_555 C3 B7 1.560 1_555 1_555 C4 B8 1.698 1_555 1_555 C4 B5 1.533 1_555 1_555 B5 Li1 2.560 1_555 1_555 B5 B6 1.658 1_555 1_555 B5 B8 1.787 1_555 1_555 H5 Li1 2.206 1_555 1_555 B6 B7 1.622 1_555 1_555 B6 Li1 2.335 1_555 1_555 B6 B8 1.778 1_555 1_555 H6 Li1 2.007 1_555 1_555 B7 B8 1.758 1_555 1_555 C17 C18 1.492 1_555 1_555 C23 C24 1.427 1_555 1_555 C29 C30 1.393 1_555 1_555 C35 C36 1.360 1_555 1_555 C41B C42B 1.354 1_555 1_555 #END data_CSD_CIF_ZUPBAN _audit_creation_date 1996-10-31 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD ZUPBAN _chemical_formula_sum 'C43 H111 B8 Cl2 Li3 N8 Si4 Sm1' _chemical_formula_moiety ; C28 H76 B8 Cl2 Li2 N4 Si4 Sm1 1-,C12 H32 Li1 N4 1+,0.5(C6 H6) ; _journal_coden_Cambridge 579 _journal_volume 15 _journal_year 1996 _journal_page_first 1006 _journal_name_full 'Organometallics ' loop_ _publ_author_name "N.S.Hosmane" "Ying Wang" "Hongming Zhang" "J.A.Maguire" "M.McInnis" "T.G.Gray" "J.D.Collins" "R.K.Kremer" "H.Binder" "E.Waldhor" "W.Kaim" _chemical_name_systematic ; bis(Tetramethylethylenediamine)-lithium 1-chloro-1-(\m~2~-chloro)-2,2',3,3'-tetrakis(trimethylsilyl)-5,6-(bis(\m~2~-hy drido)-tetramethylethylenediamine-lithium)-4,4',5'-(tris(\m~2~-hydrido)-(tetra methylethylenediamine)-lithium)-1,1'-commo-samarium(iii)-bis(2,3-dicarbahexabo rane) benzene solvate ; _cell_volume 7285.948 _exptl_crystal_density_diffrn 1.077 _exptl_special_details ; Air-sensitive ; _diffrn_ambient_temperature 230 _refine_special_details ; The benzene solvent is disordered. ; #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.055 _refine_ls_wR_factor_gt 0.055 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 -1/2+x,-1/2-y,-1/2+z _cell_length_a 14.830(4) _cell_length_b 21.196(6) _cell_length_c 23.215(4) _cell_angle_alpha 90 _cell_angle_beta 93.20(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.63 H 0.23 B 0.85 Cl 0.99 Li 1.44 N 0.68 Si 1.20 Sm 1.94 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Sm1 Sm 0.0279(1) 0.2565(11) 0.8533(1) Cl1 Cl 0.0460(3) 0.2902(3) 0.9614(2) Cl2 Cl 0.0233(4) 0.3556(3) 0.7933(2) Si1 Si 0.2956(4) 0.2964(4) 0.8977(3) Si2 Si 0.2290(4) 0.1253(3) 0.9417(3) Si3 Si -0.2248(4) 0.3245(3) 0.8628(3) Si4 Si -0.1701(5) 0.1790(4) 0.9612(3) C1 C 0.2155(10) 0.2385(13) 0.8624(7) C2 C 0.1847(14) 0.1719(12) 0.8784(9) B1 B 0.1305(19) 0.1398(14) 0.8249(12) B2 B 0.1376(18) 0.1885(14) 0.7702(12) B3 B 0.1892(12) 0.2612(19) 0.7969(8) B4 B 0.2376(19) 0.1762(14) 0.8124(12) C3 C -0.1572(9) 0.2567(25) 0.8493(6) C4 C -0.1332(12) 0.1978(9) 0.8880(8) B5 B -0.0885(16) 0.1404(12) 0.8548(10) B6 B -0.0936(17) 0.1652(12) 0.7851(11) B7 B -0.1334(11) 0.2364(11) 0.7843(7) B8 B -0.1919(20) 0.1820(14) 0.8247(13) C5 C 0.3229(14) 0.2856(11) 0.9772(8) C6 C 0.2444(17) 0.3768(12) 0.8898(12) C7 C 0.4026(16) 0.2970(13) 0.8589(11) C8 C 0.1941(17) 0.1555(13) 1.013(1) C9 C 0.3571(17) 0.1169(14) 0.9435(12) C10 C 0.1856(22) 0.0427(15) 0.9391(14) C11 C -0.1657(15) 0.3812(11) 0.9155(9) C12 C -0.3389(17) 0.3035(14) 0.8867(12) C13 C -0.2427(17) 0.3702(13) 0.7968(10) C14 C -0.1872(12) 0.2561(30) 1.0086(8) C15 C -0.2770(16) 0.1310(13) 0.9555(11) C16 C -0.0802(19) 0.1317(15) 1.0020(13) Li1 Li -0.0004(29) 0.0792(23) 0.7881(18) N1 N -0.0483(14) -0.0142(11) 0.8109(10) N2 N 0.0454(14) 0.0279(11) 0.7086(9) C17 C -0.0091(44) -0.0543(29) 0.7689(22) C18 C -0.0037(28) -0.0315(20) 0.7105(17) C19 C -0.0249(23) -0.0385(17) 0.8678(14) C20 C -0.1495(17) -0.0111(14) 0.8060(12) C21 C 0.0319(22) 0.0622(16) 0.6554(13) C22 C 0.1451(20) 0.0187(16) 0.7132(14) Li2 Li 0.0970(22) 0.3008(18) 0.7197(14) N3 N 0.0074(15) 0.2957(12) 0.6406(9) N4 N 0.1859(13) 0.3502(10) 0.6701(8) C23 C 0.0681(20) 0.3132(16) 0.6010(13) C24 C 0.1292(22) 0.3631(16) 0.6165(14) C25 C -0.0303(21) 0.2356(22) 0.6313(15) C26 C -0.0638(17) 0.3386(14) 0.6469(11) C27 C 0.2630(19) 0.3100(15) 0.6623(13) C28 C 0.2133(23) 0.4066(16) 0.6951(14) Li3 Li 0.0461(24) 0.3805(19) 1.1679(16) N5 N -0.0689(15) 0.4297(12) 1.1301(10) N6 N 0.0257(21) 0.4340(16) 1.2442(14) C29 C -0.0871(26) 0.4717(18) 1.1724(15) C30 C -0.0689(23) 0.4576(18) 1.2328(14) C31 C -0.1417(25) 0.3854(19) 1.1224(17) C32 C -0.0625(29) 0.4612(21) 1.0763(18) C33 C 0.0221(20) 0.3917(15) 1.2960(13) C34 C 0.0906(26) 0.4789(19) 1.2517(18) N7 N 0.1727(13) 0.3878(9) 1.1236(8) N8 N 0.0665(14) 0.2865(9) 1.1676(9) C35 C 0.1870(23) 0.3165(16) 1.1205(14) C36 C 0.1501(26) 0.2701(39) 1.1569(18) C37 C 0.1641(19) 0.4173(14) 1.0682(10) C38 C 0.2435(19) 0.4175(15) 1.1581(11) C39 C 0.0062(13) 0.2563(21) 1.1261(8) C40 C 0.0620(19) 0.2561(23) 1.2223(10) C41? C -0.7333(25) 0.0291(23) 0.5011(7) C42? C 0.0051(33) 0.0622(11) 0.4875(17) C43? C 0.0890(31) 0.0309(26) 0.4897(20) H1 H 0.26860 0.28540 0.99790 H2 H 0.35320 0.24580 0.98250 H3 H 0.36190 0.31880 0.99160 H4 H 0.22890 0.38460 0.84970 H5 H 0.19110 0.37950 0.91130 H6 H 0.28750 0.40770 0.90400 H7 H 0.38960 0.30360 0.81830 H8 H 0.44120 0.33020 0.87390 H9 H 0.43250 0.25710 0.86470 H10 H 0.12950 0.15920 1.01250 H11 H 0.21450 0.12720 1.04330 H12 H 0.22100 0.19620 1.01950 H13 H 0.37490 0.10070 0.90730 H14 H 0.38370 0.15770 0.95020 H15 H 0.37720 0.08880 0.97400 H16 H 0.12090 0.04450 0.93810 H17 H 0.20430 0.02310 0.90440 H18 H 0.20750 0.01850 0.97190 H19 H -0.10790 0.39220 0.90180 H20 H -0.20150 0.41860 0.91880 H21 H -0.15760 0.36120 0.95250 H22 H -0.36830 0.27500 0.85960 H23 H -0.33120 0.28340 0.92370 H24 H -0.37510 0.34080 0.89000 H25 H -0.27290 0.34530 0.76710 H26 H -0.27880 0.40640 0.80470 H27 H -0.18520 0.38380 0.78430 H28 H -0.13210 0.27990 1.01180 H29 H -0.23420 0.28150 0.99040 H30 H -0.20400 0.24390 1.04640 H31 H -0.26770 0.09400 0.93260 H32 H -0.29390 0.11860 0.99320 H33 H -0.32420 0.15620 0.93720 H34 H -0.06790 0.09360 0.98150 H35 H -0.02610 0.15650 1.00660 H36 H -0.10110 0.12140 1.03920 H37 H -0.06240 -0.07930 0.76150 H38 H 0.04010 -0.08160 0.78080 H39 H 0.02470 -0.06020 0.68520 H40 H -0.06020 -0.01950 0.69150 H41 H -0.05040 -0.07950 0.87360 H42 H 0.03970 -0.04100 0.87180 H43 H -0.04620 -0.00970 0.89590 H44 H -0.17500 -0.05130 0.81520 H45 H -0.16890 0.02010 0.83270 H46 H -0.16940 0.00070 0.76750 H47 H 0.05050 0.03900 0.62260 H48 H -0.03130 0.07180 0.65040 H49 H 0.06570 0.10080 0.65900 H50 H 0.16560 -0.00410 0.68070 H51 H 0.17270 0.05970 0.71490 H52 H 0.16130 -0.00410 0.74800 H53 H 0.03560 0.32210 0.56490 H54 H 0.10640 0.27750 0.59510 H55 H 0.16580 0.37370 0.58510 H56 H 0.09110 0.39860 0.62340 H57 H -0.06700 0.23720 0.59590 H58 H 0.01400 0.20290 0.62900 H59 H -0.06780 0.22700 0.66280 H60 H -0.10460 0.33810 0.61330 H61 H -0.09570 0.32710 0.68020 H62 H -0.03910 0.38020 0.65210 H63 H 0.30380 0.33320 0.63960 H64 H 0.29280 0.29900 0.69870 H65 H 0.24430 0.27220 0.64220 H66 H 0.25430 0.42920 0.67210 H67 H 0.15920 0.43090 0.69830 H68 H 0.24110 0.39930 0.73280 H69 H -0.14980 0.48280 1.16720 H70 H -0.05270 0.50930 1.16660 H71 H -0.08350 0.49090 1.25870 H72 H -0.10480 0.42130 1.24090 H73 H -0.19540 0.40490 1.10560 H74 H -0.12300 0.35230 1.09750 H75 H -0.15400 0.36800 1.15940 H76 H -0.11900 0.48100 1.06510 H77 H -0.01540 0.49240 1.07820 H78 H -0.04900 0.42970 1.04830 H79 H 0.00700 0.41330 1.33050 H80 H -0.01660 0.35570 1.29010 H81 H 0.08390 0.37810 1.29980 H82 H 0.08380 0.50770 1.28310 H83 H 0.13760 0.44920 1.26200 H84 H 0.10610 0.50200 1.21810 H85 H 0.25050 0.30880 1.11830 H86 H 0.15850 0.30380 1.08420 H87 H 0.15670 0.22700 1.14540 H88 H 0.18540 0.27630 1.19240 H89 H 0.22240 0.41750 1.05210 H90 H 0.12260 0.39330 1.04370 H91 H 0.14260 0.45980 1.07110 H92 H 0.29970 0.41960 1.13960 H93 H 0.22160 0.45940 1.16450 H94 H 0.25250 0.39610 1.19440 H95 H 0.01750 0.21170 1.12720 H96 H -0.05520 0.26430 1.13500 H97 H 0.01630 0.27220 1.08820 H98 H 0.07270 0.21150 1.21960 H99 H 0.10580 0.27450 1.24930 H100 H 0.00240 0.26320 1.23520 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Sm1 Cl1 2.609 1_555 1_555 Cl2 Sm1 2.519 1_555 1_555 Si1 C1 1.865 1_555 1_555 Si2 C2 1.860 1_555 1_555 Si3 C3 1.790 1_555 1_555 Si4 C4 1.857 1_555 1_555 C1 Sm1 2.804 1_555 1_555 C2 Sm1 2.968 1_555 1_555 B1 Sm1 2.997 1_555 1_555 B2 Sm1 2.966 1_555 1_555 B3 Sm1 2.792 1_555 1_555 B4 C1 1.800 1_555 1_555 C3 Sm1 2.741 1_555 1_555 C4 Sm1 2.850 1_555 1_555 B5 Sm1 3.007 1_555 1_555 B6 Sm1 3.030 1_555 1_555 B7 Sm1 2.836 1_555 1_555 B8 C3 1.751 1_555 1_555 C5 Si1 1.881 1_555 1_555 C6 Si1 1.871 1_555 1_555 C7 Si1 1.868 1_555 1_555 C8 Si2 1.874 1_555 1_555 C9 Si2 1.906 1_555 1_555 C10 Si2 1.865 1_555 1_555 C11 Si3 1.895 1_555 1_555 C12 Si3 1.864 1_555 1_555 C13 Si3 1.820 1_555 1_555 C14 Si4 1.994 1_555 1_555 C15 Si4 1.882 1_555 1_555 C16 Si4 1.881 1_555 1_555 Li1 B1 2.442 1_555 1_555 N1 Li1 2.179 1_555 1_555 N2 Li1 2.278 1_555 1_555 C17 N1 1.440 1_555 1_555 C18 N2 1.456 1_555 1_555 C19 N1 1.442 1_555 1_555 C20 N1 1.500 1_555 1_555 C21 N2 1.437 1_555 1_555 C22 N2 1.489 1_555 1_555 Li2 Cl2 2.382 1_555 1_555 N3 Li2 2.208 1_555 1_555 N4 Li2 2.081 1_555 1_555 C23 N3 1.373 1_555 1_555 C24 N4 1.488 1_555 1_555 C25 N3 1.403 1_555 1_555 C26 N3 1.407 1_555 1_555 C27 N4 1.445 1_555 1_555 C28 N4 1.380 1_555 1_555 Li3 N5 2.145 1_555 1_555 N5 C29 1.364 1_555 1_555 N6 Li3 2.139 1_555 1_555 C29 C30 1.444 1_555 1_555 C30 N6 1.499 1_555 1_555 C31 N5 1.434 1_555 1_555 C32 N5 1.424 1_555 1_555 C33 N6 1.503 1_555 1_555 C34 N6 1.358 1_555 1_555 N7 Li3 2.196 1_555 1_555 N8 Li3 2.015 1_555 1_555 C35 N7 1.528 1_555 1_555 C36 N8 1.324 1_555 1_555 C37 N7 1.429 1_555 1_555 C38 N7 1.430 1_555 1_555 C39 N8 1.429 1_555 1_555 C40 N8 1.429 1_555 1_555 H1 C5 0.961 1_555 1_555 H2 C5 0.960 1_555 1_555 H3 C5 0.959 1_555 1_555 H4 C6 0.961 1_555 1_555 H5 C6 0.960 1_555 1_555 H6 C6 0.961 1_555 1_555 H7 C7 0.962 1_555 1_555 H8 C7 0.960 1_555 1_555 H9 C7 0.961 1_555 1_555 H10 C8 0.961 1_555 1_555 H11 C8 0.960 1_555 1_555 H12 C8 0.959 1_555 1_555 H13 C9 0.958 1_555 1_555 H14 C9 0.960 1_555 1_555 H15 C9 0.960 1_555 1_555 H16 C10 0.959 1_555 1_555 H17 C10 0.961 1_555 1_555 H18 C10 0.960 1_555 1_555 H19 C11 0.960 1_555 1_555 H20 C11 0.960 1_555 1_555 H21 C11 0.959 1_555 1_555 H22 C12 0.959 1_555 1_555 H23 C12 0.960 1_555 1_555 H24 C12 0.961 1_555 1_555 H25 C13 0.959 1_555 1_555 H26 C13 0.959 1_555 1_555 H27 C13 0.960 1_555 1_555 H28 C14 0.960 1_555 1_555 H29 C14 0.960 1_555 1_555 H30 C14 0.961 1_555 1_555 H31 C15 0.962 1_555 1_555 H32 C15 0.960 1_555 1_555 H33 C15 0.960 1_555 1_555 H34 C16 0.960 1_555 1_555 H35 C16 0.960 1_555 1_555 H36 C16 0.959 1_555 1_555 H37 C17 0.959 1_555 1_555 H38 C17 0.960 1_555 1_555 H39 C18 0.959 1_555 1_555 H40 C18 0.959 1_555 1_555 H41 C19 0.960 1_555 1_555 H42 C19 0.959 1_555 1_555 H43 C19 0.960 1_555 1_555 H44 C20 0.961 1_555 1_555 H45 C20 0.961 1_555 1_555 H46 C20 0.959 1_555 1_555 H47 C21 0.960 1_555 1_555 H48 C21 0.960 1_555 1_555 H49 C21 0.961 1_555 1_555 H50 C22 0.960 1_555 1_555 H51 C22 0.960 1_555 1_555 H52 C22 0.960 1_555 1_555 H53 C23 0.962 1_555 1_555 H54 C23 0.961 1_555 1_555 H55 C24 0.959 1_555 1_555 H56 C24 0.960 1_555 1_555 H57 C25 0.961 1_555 1_555 H58 C25 0.959 1_555 1_555 H59 C25 0.961 1_555 1_555 H60 C26 0.960 1_555 1_555 H61 C26 0.960 1_555 1_555 H62 C26 0.960 1_555 1_555 H63 C27 0.960 1_555 1_555 H64 C27 0.960 1_555 1_555 H65 C27 0.960 1_555 1_555 H66 C28 0.959 1_555 1_555 H67 C28 0.960 1_555 1_555 H68 C28 0.959 1_555 1_555 H69 C29 0.960 1_555 1_555 H70 C29 0.960 1_555 1_555 H71 C30 0.960 1_555 1_555 H72 C30 0.960 1_555 1_555 H73 C31 0.960 1_555 1_555 H74 C31 0.960 1_555 1_555 H75 C31 0.962 1_555 1_555 H76 C32 0.960 1_555 1_555 H77 C32 0.961 1_555 1_555 H78 C32 0.961 1_555 1_555 H79 C33 0.960 1_555 1_555 H80 C33 0.960 1_555 1_555 H81 C33 0.960 1_555 1_555 H82 C34 0.960 1_555 1_555 H83 C34 0.960 1_555 1_555 H84 C34 0.960 1_555 1_555 H85 C35 0.960 1_555 1_555 H86 C35 0.960 1_555 1_555 H87 C36 0.958 1_555 1_555 H88 C36 0.960 1_555 1_555 H89 C37 0.961 1_555 1_555 H90 C37 0.960 1_555 1_555 H91 C37 0.959 1_555 1_555 H92 C38 0.960 1_555 1_555 H93 C38 0.960 1_555 1_555 H94 C38 0.960 1_555 1_555 H95 C39 0.960 1_555 1_555 H96 C39 0.960 1_555 1_555 H97 C39 0.962 1_555 1_555 H98 C40 0.961 1_555 1_555 H99 C40 0.960 1_555 1_555 H100 C40 0.961 1_555 1_555 C1 C2 1.536 1_555 1_555 C1 B3 1.622 1_555 1_555 C2 B4 1.762 1_555 1_555 C2 B1 1.594 1_555 1_555 B1 B2 1.644 1_555 1_555 B1 B4 1.804 1_555 1_555 B2 B4 1.751 1_555 1_555 B2 B3 1.814 1_555 1_555 B2 Li2 2.706 1_555 1_555 B3 B4 1.965 1_555 1_555 B3 Li2 2.348 1_555 1_555 C3 C4 1.567 1_555 1_555 C3 B7 1.627 1_555 1_555 C4 B8 1.699 1_555 1_555 C4 B5 1.603 1_555 1_555 B5 Li1 2.452 1_555 1_555 B5 B6 1.699 1_555 1_555 B5 B8 1.870 1_555 1_555 B6 B7 1.620 1_555 1_555 B6 B8 1.802 1_555 1_555 B6 Li1 2.286 1_555 1_555 B7 B8 1.747 1_555 1_555 C17 C18 1.446 1_555 1_555 C23 C24 1.426 1_555 1_555 C35 C36 1.426 1_555 1_555 #END data_CSD_CIF_ZUPBER _audit_creation_date 1996-10-31 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD ZUPBER _chemical_formula_sum 'C43 H111 B8 Cl2 Gd1 Li3 N8 Si4' _chemical_formula_moiety ; C28 H76 B8 Cl2 Gd1 Li2 N4 Si4 1-,C12 H32 Li1 N4 1+,0.5(C6 H6) ; _journal_coden_Cambridge 579 _journal_volume 15 _journal_year 1996 _journal_page_first 1006 _journal_name_full 'Organometallics ' loop_ _publ_author_name "N.S.Hosmane" "Ying Wang" "Hongming Zhang" "J.A.Maguire" "M.McInnis" "T.G.Gray" "J.D.Collins" "R.K.Kremer" "H.Binder" "E.Waldhor" "W.Kaim" _chemical_name_systematic ; bis(Tetramethylethylenediamine)-lithium 1-chloro-1-(\m~2~-chloro)-2,2',3,3'-tetrakis(trimethylsilyl)-5,6-(bis(\m~2~-hy drido)-tetramethylethylenediamine-lithium)-4,4',5'-(tris(\m~2~-hydrido)-(tetra methylethylenediamine)-lithium)-1,1'-commo-gadolinium(iii)-bis(2,3-dicarbahexa borane) benzene solvate ; _cell_volume 7241.588 _exptl_crystal_density_diffrn 1.09 _exptl_special_details ; Air-sensitive z(C73) is 1.1711 not 1.1171 ; _diffrn_ambient_temperature 230 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.048 _refine_ls_wR_factor_gt 0.048 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 -1/2+x,-1/2-y,-1/2+z _cell_length_a 14.793(3) _cell_length_b 21.149(5) _cell_length_c 23.183(5) _cell_angle_alpha 90 _cell_angle_beta 93.21(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.25 B 0.83 Cl 0.99 Gd 1.79 Li 1.44 N 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Gd1 Gd 0.0283(1) 0.2432(1) 0.8521(1) Cl1 Cl 0.0468(2) 0.2883(1) 0.9596(1) Cl2 Cl 0.0232(2) 0.3548(1) 0.7942(1) Si1 Si 0.2956(2) 0.2966(2) 0.8973(1) Si2 Si 0.2291(2) 0.1253(2) 0.9420(2) Si3 Si -0.2235(2) 0.3242(2) 0.8637(2) Si4 Si -0.1682(3) 0.1792(2) 0.9615(2) C1 C 0.2165(7) 0.2379(6) 0.8626(4) C2 C 0.1833(7) 0.1724(5) 0.8780(5) B1 B 0.1332(10) 0.1395(7) 0.8251(6) B2 B 0.1379(10) 0.1887(7) 0.7708(6) B3 B 0.1909(7) 0.2527(7) 0.7975(5) B4 B 0.240(1) 0.1776(8) 0.8152(7) C3 C -0.1553(6) 0.2525(5) 0.8490(4) C4 C -0.1303(6) 0.1978(5) 0.8882(4) B5 B -0.0882(8) 0.1434(5) 0.8546(5) B6 B -0.0932(8) 0.1652(6) 0.7861(6) B7 B -0.1315(8) 0.2380(6) 0.7847(5) B8 B -0.1895(9) 0.1803(5) 0.8259(6) C5 C 0.3237(9) 0.2870(6) 0.9758(5) C6 C 0.2438(8) 0.3772(5) 0.8902(5) C7 C 0.4033(8) 0.2965(7) 0.8597(6) C8 C 0.1972(8) 0.1555(6) 1.0130(5) C9 C 0.3540(9) 0.1167(7) 0.9412(6) C10 C 0.1834(11) 0.0448(6) 0.9375(6) C11 C -0.1632(8) 0.3801(5) 0.9153(5) C12 C -0.3388(8) 0.3051(8) 0.8863(6) C13 C -0.2408(9) 0.3721(6) 0.7959(6) C14 C -0.1865(9) 0.2489(6) 1.0092(5) C15 C -0.2731(10) 0.1308(8) 0.9541(6) C16 C -0.0801(10) 0.1309(6) 1.0003(5) Li1 Li 0.0039(14) 0.0779(10) 0.7857(10) N1 N -0.0491(8) -0.0161(5) 0.8107(5) N2 N 0.0478(9) 0.0279(7) 0.7116(6) C17 C -0.0128(15) -0.0577(8) 0.7676(9) C18 C -0.0082(13) -0.0301(9) 0.7100(9) C19 C -0.0218(11) -0.0413(6) 0.8669(7) C20 C -0.1484(10) -0.0117(7) 0.8036(7) C21 C 0.0283(12) 0.0611(9) 0.6551(7) C22 C 0.1425(10) 0.0190(8) 0.7159(7) Li2 Li 0.0932(14) 0.298(1) 0.7195(8) N3 N 0.0099(10) 0.2958(7) 0.6427(5) N4 N 0.1828(9) 0.3493(7) 0.6697(5) C23 C 0.0683(13) 0.3177(11) 0.5986(6) C24 C 0.1323(12) 0.3639(10) 0.6174(8) C25 C -0.0319(13) 0.2360(9) 0.6306(6) C26 C -0.0652(12) 0.3389(10) 0.6458(7) C27 C 0.2619(12) 0.3119(11) 0.6593(7) C28 C 0.2142(11) 0.4070(8) 0.6969(7) Li3 Li 0.0486(12) 0.3833(9) 1.1659(9) N5 N -0.0708(8) 0.4271(6) 1.1321(7) N6 N 0.0269(8) 0.4315(5) 1.2443(5) C29 C -0.0850(13) 0.4764(9) 1.1711(12) C30 C -0.0646(14) 0.4570(9) 1.2319(9) C31 C -0.1424(11) 0.3878(8) 1.1231(9) C32 C -0.0638(15) 0.4590(11) 1.0775(10) C33 C 0.0213(11) 0.3956(9) 1.2979(6) C34 C 0.0912(14) 0.4777(9) 1.2559(9) N7 N 0.1704(7) 0.3893(6) 1.1236(5) N8 N 0.0659(9) 0.2852(5) 1.1695(5) C35 C 0.1881(15) 0.3176(12) 1.1165(8) C36 C 0.1576(17) 0.2806(10) 1.1577(12) C37 C 0.1621(11) 0.4155(7) 1.0658(6) C38 C 0.2413(11) 0.4210(11) 1.1574(7) C39 C 0.0070(11) 0.2516(7) 1.1292(6) C40 C 0.0668(17) 0.2558(8) 1.2244(7) C41 C 0.577(2) 0.5300(25) -0.001(1) C42 C 0.5005(32) 0.5631(8) 0.0153(10) C43 C 0.5846(24) 0.4662(18) -0.0110(11) H1 H 0.13110 0.08210 0.83170 H2 H 0.12080 0.18460 0.71680 H3 H 0.18460 0.30580 0.77970 H4? H 0.31610 0.14910 0.82570 H5 H -0.07820 0.09780 0.87670 H6 H -0.08210 0.13260 0.73920 H7 H -0.15570 0.27130 0.74250 H8 H -0.26460 0.15960 0.81890 H9 H 0.35090 0.24630 0.98290 H10 H 0.26950 0.29030 0.99650 H11 H 0.36540 0.31950 0.98880 H12 H 0.22740 0.38560 0.85030 H13 H 0.28680 0.40830 0.90450 H14 H 0.19080 0.37900 0.91220 H15 H 0.39040 0.30140 0.81890 H16 H 0.43430 0.25720 0.86700 H17 H 0.44080 0.33080 0.87380 H18 H 0.21930 0.19790 1.01820 H19 H 0.22340 0.12890 1.04310 H20 H 0.13250 0.15520 1.01440 H21 H 0.37810 0.10520 0.97900 H22 H 0.38010 0.15600 0.92990 H23 H 0.36830 0.08430 0.91410 H24 H 0.19660 0.02330 0.97350 H25 H 0.21070 0.02230 0.90700 H26 H 0.11910 0.04660 0.92970 H27 H -0.15130 0.35950 0.95180 H28 H -0.20040 0.41670 0.92050 H29 H -0.10710 0.39290 0.90000 H30 H -0.33430 0.28040 0.92110 H31 H -0.37080 0.28140 0.85630 H32 H -0.37100 0.34360 0.89320 H33 H -0.27070 0.41100 0.80440 H34 H -0.27740 0.34860 0.76790 H35 H -0.18320 0.38110 0.78070 H36 H -0.23200 0.27590 0.99110 H37 H -0.13090 0.27200 1.01510 H38 H -0.20610 0.23460 1.04570 H39 H -0.32020 0.15470 0.93410 H40 H -0.29170 0.11950 0.99180 H41 H -0.26150 0.09310 0.93270 H42 H -0.07880 0.14050 1.04080 H43 H -0.02210 0.14030 0.98570 H44 H -0.09350 0.08690 0.99460 H45 H 0.04740 -0.06970 0.78090 H46 H -0.05040 -0.09460 0.76430 H47 H 0.01780 -0.06040 0.68500 H48 H -0.06840 -0.01970 0.69540 H49 H -0.04490 -0.01480 0.89640 H50 H 0.04300 -0.04260 0.87140 H51 H -0.04560 -0.08330 0.87050 H52 H -0.16530 0.00510 0.76610 H53 H -0.17020 0.01580 0.83270 H54 H -0.17440 -0.05300 0.80730 H55 H -0.03560 0.06860 0.64960 H56 H 0.04810 0.03530 0.62420 H57 H 0.05990 0.10080 0.65540 H58 H 0.15940 -0.00220 0.75150 H59 H 0.17220 0.05930 0.71520 H60 H 0.16040 -0.00610 0.68400 H61 H 0.03080 0.33550 0.56760 H62 H 0.10050 0.28190 0.58470 H63 H 0.17430 0.36920 0.58760 H64 H 0.10070 0.40290 0.62290 H65 H 0.01390 0.20430 0.62780 H66 H -0.06740 0.23840 0.59470 H67 H -0.07030 0.22530 0.66110 H68 H -0.04270 0.38070 0.65390 H69 H -0.10280 0.32580 0.67600 H70 H -0.09990 0.33900 0.60950 H71 H 0.24350 0.27280 0.64110 H72 H 0.29460 0.30320 0.69540 H73 H 0.30010 0.33480 0.63450 H74 H 0.16330 0.43320 0.70450 H75 H 0.25290 0.42900 0.67170 H76 H 0.24740 0.39730 0.73260 H77 H -0.04650 0.51120 1.16230 H78 H -0.14710 0.48940 1.16670 H79 H -0.10750 0.42520 1.24140 H80 H -0.07170 0.49340 1.25600 H81 H -0.15170 0.36450 1.15780 H82 H -0.13070 0.35890 1.09250 H83 H -0.19560 0.41210 1.11260 H84 H -0.01400 0.48810 1.08030 H85 H -0.11890 0.48170 1.06800 H86 H -0.05400 0.42850 1.04790 H87 H -0.02270 0.36250 1.29230 H88 H 0.00370 0.42330 1.32810 H89 H 0.07930 0.37740 1.30850 H90 H 0.09770 0.50290 1.22200 H91 H 0.14810 0.45830 1.26720 H92 H 0.07250 0.50420 1.28680 H93 H 0.25230 0.31140 1.11590 H94 H 0.15970 0.30450 1.08020 H95 H 0.16850 0.23760 1.14670 H96 H 0.19230 0.29000 1.19290 H97 H 0.11470 0.39400 1.04380 H98 H 0.21820 0.41020 1.04750 H99 H 0.14790 0.45970 1.06790 H100 H 0.24610 0.40330 1.19550 H101 H 0.22730 0.46520 1.15980 H102 H 0.29770 0.41570 1.13940 H103 H 0.00680 0.27180 1.09220 H104 H -0.05330 0.25160 1.14260 H105 H 0.02790 0.20880 1.12590 H106 H 0.00670 0.25570 1.23790 H107 H 0.10640 0.27860 1.25110 H108 H 0.08780 0.21300 1.22130 C43B C 0.4154(24) 0.5338(18) 0.0110(11) C41B C 0.423(2) 0.4700(25) 0.001(1) C42B C 0.4995(32) 0.4369(8) -0.0153(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Gd1 Cl1 2.668 1_555 1_555 Cl2 Gd1 2.714 1_555 1_555 Si1 C1 1.858 1_555 1_555 Si2 C2 1.882 1_555 1_555 Si3 C3 1.863 1_555 1_555 Si4 C4 1.861 1_555 1_555 C1 Gd1 2.783 1_555 1_555 C2 Gd1 2.776 1_555 1_555 B1 Gd1 2.778 1_555 1_555 B2 Gd1 2.802 1_555 1_555 B3 Gd1 2.787 1_555 1_555 B4 C1 1.731 1_555 1_555 C3 Gd1 2.720 1_555 1_555 C4 Gd1 2.710 1_555 1_555 B5 Gd1 2.728 1_555 1_555 B6 Gd1 2.826 1_555 1_555 B7 Gd1 2.762 1_555 1_555 B8 C3 1.686 1_555 1_555 C5 Si1 1.855 1_555 1_555 C6 Si1 1.872 1_555 1_555 C7 Si1 1.858 1_555 1_555 C8 Si2 1.851 1_555 1_555 C9 Si2 1.858 1_555 1_555 C10 Si2 1.833 1_555 1_555 C11 Si3 1.872 1_555 1_555 C12 Si3 1.857 1_555 1_555 C13 Si3 1.875 1_555 1_555 C14 Si4 1.872 1_555 1_555 C15 Si4 1.859 1_555 1_555 C16 Si4 1.849 1_555 1_555 Li1 B1 2.448 1_555 1_555 N1 Li1 2.226 1_555 1_555 N2 Li1 2.148 1_555 1_555 C17 N1 1.456 1_555 1_555 C18 N2 1.479 1_555 1_555 C19 N1 1.444 1_555 1_555 C20 N1 1.472 1_555 1_555 C21 N2 1.500 1_555 1_555 C22 N2 1.411 1_555 1_555 Li2 Cl2 2.391 1_555 1_555 N3 Li2 2.108 1_555 1_555 N4 Li2 2.107 1_555 1_555 C23 N3 1.451 1_555 1_555 C24 N4 1.422 1_555 1_555 C25 N3 1.429 1_555 1_555 C26 N3 1.442 1_555 1_555 C27 N4 1.444 1_555 1_555 C28 N4 1.439 1_555 1_555 Li3 N5 2.106 1_555 1_555 N5 C29 1.404 1_555 1_555 N6 Li3 2.124 1_555 1_555 C29 C30 1.483 1_555 1_555 C30 N6 1.470 1_555 1_555 C31 N5 1.353 1_555 1_555 C32 N5 1.443 1_555 1_555 C33 N6 1.463 1_555 1_555 C34 N6 1.380 1_555 1_555 N7 Li3 2.103 1_555 1_555 N8 Li3 2.092 1_555 1_555 C35 N7 1.549 1_555 1_555 C36 N8 1.402 1_555 1_555 C37 N7 1.449 1_555 1_555 C38 N7 1.439 1_555 1_555 C39 N8 1.430 1_555 1_555 C40 N8 1.416 1_555 1_555 C41 C42 1.400 1_555 1_555 C42 C43B 1.402 1_555 1_555 C43 C41 1.375 1_555 1_555 H1 B1 1.224 1_555 1_555 H2 B2 1.266 1_555 1_555 H3 B3 1.198 1_555 1_555 H5 B5 1.098 1_555 1_555 H6 B6 1.306 1_555 1_555 H7 B7 1.242 1_555 1_555 H8 B8 1.197 1_555 1_555 H9 C5 0.960 1_555 1_555 H10 C5 0.960 1_555 1_555 H11 C5 0.961 1_555 1_555 H12 C6 0.960 1_555 1_555 H13 C6 0.961 1_555 1_555 H14 C6 0.960 1_555 1_555 H15 C7 0.960 1_555 1_555 H16 C7 0.960 1_555 1_555 H17 C7 0.959 1_555 1_555 H18 C8 0.960 1_555 1_555 H19 C8 0.961 1_555 1_555 H20 C8 0.959 1_555 1_555 H21 C9 0.959 1_555 1_555 H22 C9 0.959 1_555 1_555 H23 C9 0.961 1_555 1_555 H24 C10 0.961 1_555 1_555 H25 C10 0.960 1_555 1_555 H26 C10 0.959 1_555 1_555 H27 C11 0.959 1_555 1_555 H28 C11 0.961 1_555 1_555 H29 C11 0.960 1_555 1_555 H30 C12 0.960 1_555 1_555 H31 C12 0.960 1_555 1_555 H32 C12 0.961 1_555 1_555 H33 C13 0.960 1_555 1_555 H34 C13 0.960 1_555 1_555 H35 C13 0.959 1_555 1_555 H36 C14 0.961 1_555 1_555 H37 C14 0.960 1_555 1_555 H38 C14 0.959 1_555 1_555 H39 C15 0.959 1_555 1_555 H40 C15 0.961 1_555 1_555 H41 C15 0.960 1_555 1_555 H42 C16 0.960 1_555 1_555 H43 C16 0.961 1_555 1_555 H44 C16 0.959 1_555 1_555 H45 C17 0.960 1_555 1_555 H46 C17 0.959 1_555 1_555 H47 C18 0.959 1_555 1_555 H48 C18 0.960 1_555 1_555 H49 C19 0.962 1_555 1_555 H50 C19 0.959 1_555 1_555 H51 C19 0.961 1_555 1_555 H52 C20 0.959 1_555 1_555 H53 C20 0.960 1_555 1_555 H54 C20 0.960 1_555 1_555 H55 C21 0.960 1_555 1_555 H56 C21 0.959 1_555 1_555 H57 C21 0.961 1_555 1_555 H58 C22 0.960 1_555 1_555 H59 C22 0.959 1_555 1_555 H60 C22 0.960 1_555 1_555 H61 C23 0.960 1_555 1_555 H62 C23 0.960 1_555 1_555 H63 C24 0.961 1_555 1_555 H64 C24 0.960 1_555 1_555 H65 C25 0.958 1_555 1_555 H66 C25 0.960 1_555 1_555 H67 C25 0.959 1_555 1_555 H68 C26 0.959 1_555 1_555 H69 C26 0.959 1_555 1_555 H70 C26 0.961 1_555 1_555 H71 C27 0.961 1_555 1_555 H72 C27 0.961 1_555 1_555 H73 C27 0.960 1_555 1_555 H74 C28 0.959 1_555 1_555 H75 C28 0.961 1_555 1_555 H76 C28 0.961 1_555 1_555 H77 C29 0.960 1_555 1_555 H78 C29 0.959 1_555 1_555 H79 C30 0.959 1_555 1_555 H80 C30 0.960 1_555 1_555 H81 C31 0.960 1_555 1_555 H82 C31 0.959 1_555 1_555 H83 C31 0.960 1_555 1_555 H84 C32 0.959 1_555 1_555 H85 C32 0.961 1_555 1_555 H86 C32 0.959 1_555 1_555 H87 C33 0.960 1_555 1_555 H88 C33 0.960 1_555 1_555 H89 C33 0.960 1_555 1_555 H90 C34 0.959 1_555 1_555 H91 C34 0.960 1_555 1_555 H92 C34 0.962 1_555 1_555 H93 C35 0.960 1_555 1_555 H94 C35 0.960 1_555 1_555 H95 C36 0.961 1_555 1_555 H96 C36 0.960 1_555 1_555 H97 C37 0.958 1_555 1_555 H98 C37 0.960 1_555 1_555 H99 C37 0.960 1_555 1_555 H100 C38 0.958 1_555 1_555 H101 C38 0.960 1_555 1_555 H102 C38 0.960 1_555 1_555 H103 C39 0.958 1_555 1_555 H104 C39 0.961 1_555 1_555 H105 C39 0.961 1_555 1_555 H106 C40 0.959 1_555 1_555 H107 C40 0.958 1_555 1_555 H108 C40 0.961 1_555 1_555 C43B C41B 1.375 1_555 1_555 C41B C42B 1.400 1_555 1_555 C42B C43 1.402 1_555 1_555 C1 C2 1.519 1_555 1_555 C1 B3 1.567 1_555 1_555 C2 B4 1.724 1_555 1_555 C2 B1 1.561 1_555 1_555 B1 B2 1.638 1_555 1_555 B1 B4 1.800 1_555 1_555 B2 B4 1.795 1_555 1_555 B2 B3 1.666 1_555 1_555 B2 Li2 2.666 1_555 1_555 B3 B4 1.785 1_555 1_555 B3 Li2 2.446 1_555 1_555 C3 C4 1.504 1_555 1_555 C3 B7 1.581 1_555 1_555 C4 B8 1.688 1_555 1_555 C4 B5 1.540 1_555 1_555 B5 Li1 2.563 1_555 1_555 B5 B6 1.651 1_555 1_555 B5 B8 1.785 1_555 1_555 B6 B7 1.640 1_555 1_555 B6 B8 1.769 1_555 1_555 B6 Li1 2.340 1_555 1_555 B7 B8 1.797 1_555 1_555 Li1 H6 1.991 1_555 1_555 Li1 H1 2.112 1_555 1_555 Li1 H5 2.528 1_555 1_555 C17 C18 1.462 1_555 1_555 Li2 H3 1.895 1_555 1_555 Li2 H2 2.434 1_555 1_555 C23 C24 1.412 1_555 1_555 C35 C36 1.333 1_555 1_555 #END data_CSD_CIF_ZUPBIV _audit_creation_date 1996-10-31 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD ZUPBIV _chemical_formula_sum 'C43 H111 B8 Cl2 Dy1 Li3 N8 Si4' _chemical_formula_moiety ; C28 H76 B8 Cl2 Dy1 Li2 N4 Si4 1-,C12 H32 Li1 N4 1+,0.5(C6 H6) ; _journal_coden_Cambridge 579 _journal_volume 15 _journal_year 1996 _journal_page_first 1006 _journal_name_full 'Organometallics ' loop_ _publ_author_name "N.S.Hosmane" "Ying Wang" "Hongming Zhang" "J.A.Maguire" "M.McInnis" "T.G.Gray" "J.D.Collins" "R.K.Kremer" "H.Binder" "E.Waldhor" "W.Kaim" _chemical_name_systematic ; bis(Tetramethylethylenediamine)-lithium 1-chloro-1-(\m~2~-chloro)-2,2',3,3'-tetrakis(trimethylsilyl)-5,6-(bis(\m~2~-hy drido)-tetramethylethylenediamine-lithium)-4,4',5'-(tris(\m~2~-hydrido)-(tetra methylethylenediamine)-lithium)-1,1'-commo-dysprosium(iii)-bis(2,3-dicarbahexa borane) benzene solvate ; _cell_volume 7121.000 _exptl_crystal_density_diffrn 1.113 _exptl_special_details ; Air-sensitive ; _diffrn_ambient_temperature 230 #These two values have been output from a single CSD field. _refine_ls_R_factor_gt 0.055 _refine_ls_wR_factor_gt 0.055 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 -1/2+x,-1/2-y,-1/2+z _cell_length_a 14.679(2) _cell_length_b 21.062(4) _cell_length_c 23.068(4) _cell_angle_alpha 90 _cell_angle_beta 93.17(1) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.25 B 0.83 Cl 0.99 Dy 1.75 Li 1.44 N 0.68 Si 1.20 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Dy1 Dy 0.0286(1) 0.2416(1) 0.8512(1) Cl1 Cl 0.0478(3) 0.2859(2) 0.9575(2) Cl2 Cl 0.0233(3) 0.3536(2) 0.7962(2) Si1 Si 0.2953(3) 0.2959(2) 0.8965(2) Si2 Si 0.2294(3) 0.1243(2) 0.9411(2) Si3 Si -0.2219(3) 0.3242(2) 0.8654(2) Si4 Si -0.1652(3) 0.1782(3) 0.9616(2) C1 C 0.2142(9) 0.2374(8) 0.8616(6) C2 C 0.1834(10) 0.1729(8) 0.8772(6) B1 B 0.1319(11) 0.1406(9) 0.8250(9) B2 B 0.1375(11) 0.1885(10) 0.7718(8) B3 B 0.1891(10) 0.2527(9) 0.7969(7) B4 B 0.2384(13) 0.1775(10) 0.8156(9) C3 C -0.1523(8) 0.2527(7) 0.8497(5) C4 C -0.1295(9) 0.1979(7) 0.8885(6) B5 B -0.0881(11) 0.1434(8) 0.8524(8) B6 B -0.0901(11) 0.1673(8) 0.7863(7) B7 B -0.1305(11) 0.2380(9) 0.7860(8) B8 B -0.1899(11) 0.1801(8) 0.8250(8) C5 C 0.3231(11) 0.2849(7) 0.9767(6) C6 C 0.2427(10) 0.3756(7) 0.8899(7) C7 C 0.4029(9) 0.2938(8) 0.8583(7) C8 C 0.1971(11) 0.1541(8) 1.0117(6) C9 C 0.3551(11) 0.1178(9) 0.9414(8) C10 C 0.1815(14) 0.0444(8) 0.9365(8) C11 C -0.1608(11) 0.3787(7) 0.9172(7) C12 C -0.3352(10) 0.3030(9) 0.8901(8) C13 C -0.2420(12) 0.3703(7) 0.7988(7) C14 C -0.1825(12) 0.2485(8) 1.0103(6) C15 C -0.2711(12) 0.1309(9) 0.9556(8) C16 C -0.0777(12) 0.1314(8) 1.0012(7) Li1 Li 0.0067(19) 0.0787(12) 0.7860(12) N1 N -0.0498(11) -0.0166(7) 0.8089(9) N2 N 0.0453(13) 0.0285(9) 0.7090(9) C17 C -0.0133(16) -0.0588(9) 0.7649(10) C18 C -0.0093(16) -0.0298(11) 0.7081(10) C19 C -0.0203(14) -0.0430(9) 0.8632(9) C20 C -0.1457(13) -0.0090(8) 0.8020(8) C21 C 0.0269(17) 0.0613(12) 0.6546(10) C22 C 0.1412(15) 0.0172(9) 0.7151(9) Li2 Li 0.0929(19) 0.2974(12) 0.7205(11) N3 N 0.0063(14) 0.2967(10) 0.6441(7) N4 N 0.1820(12) 0.3529(9) 0.6704(8) C23 C 0.0619(17) 0.3188(14) 0.5989(9) C24 C 0.1280(18) 0.3638(14) 0.6182(10) C25 C -0.0324(16) 0.2358(10) 0.6294(8) C26 C -0.0688(16) 0.3403(11) 0.6482(8) C27 C 0.2571(15) 0.3141(12) 0.6591(8) C28 C 0.2127(16) 0.4097(10) 0.6973(10) Li3 Li 0.0479(16) 0.3828(11) 1.1683(12) N5 N -0.0732(12) 0.4267(9) 1.1327(10) N6 N 0.0338(11) 0.4312(8) 1.2460(7) C29 C -0.0908(19) 0.4647(17) 1.1822(18) C30 C -0.0530(23) 0.4638(13) 1.2348(12) C31 C -0.1453(14) 0.3851(10) 1.1236(11) C32 C -0.0636(20) 0.4630(15) 1.0866(15) C33 C 0.0237(13) 0.3953(10) 1.2963(8) C34 C 0.1004(19) 0.4780(11) 1.2565(11) N7 N 0.1672(11) 0.3909(9) 1.1212(8) N8 N 0.0673(14) 0.2858(7) 1.1683(8) C35 C 0.1904(17) 0.3219(17) 1.1167(10) C36 C 0.1546(23) 0.2801(13) 1.1537(17) C37 C 0.1605(15) 0.415(1) 1.0657(10) C38 C 0.2393(14) 0.4223(12) 1.1557(9) C39 C 0.0083(14) 0.2508(9) 1.1293(8) C40 C 0.0702(21) 0.2572(10) 1.2231(11) C41 C 0.5797(26) 0.5292(31) -0.0011(12) C42 C 0.5020(49) 0.5648(15) 0.0128(12) C43 C 0.5830(32) 0.4670(25) -0.0137(13) H1 H 0.09760 0.09510 0.82520 H2 H 0.10920 0.17210 0.72300 H3 H 0.22070 0.30690 0.78670 H4 H 0.31890 0.16460 0.81070 H5 H -0.08080 0.08880 0.87100 H6 H -0.08620 0.13810 0.74030 H7 H -0.16930 0.27120 0.75100 H8 H -0.26370 0.16330 0.84280 H9 H 0.36490 0.31740 0.99030 H10 H 0.26840 0.28740 0.99750 H11 H 0.35080 0.24400 0.98300 H12 H 0.28350 0.40630 0.90790 H13 H 0.23180 0.38600 0.84960 H14 H 0.18600 0.37600 0.90870 H15 H 0.44540 0.32370 0.87600 H16 H 0.42840 0.25190 0.86110 H17 H 0.39090 0.30460 0.81820 H18 H 0.13190 0.15750 1.01180 H19 H 0.21840 0.12470 1.04120 H20 H 0.22410 0.19500 1.01930 H21 H 0.37730 0.09280 0.97400 H22 H 0.37150 0.09770 0.90610 H23 H 0.38180 0.15940 0.94390 H24 H 0.11620 0.04670 0.93660 H25 H 0.19870 0.02410 0.90140 H26 H 0.20450 0.02030 0.96940 H27 H -0.19870 0.41480 0.92420 H28 H -0.14670 0.35690 0.95310 H29 H -0.10530 0.39280 0.90120 H30 H -0.36850 0.34100 0.89790 H31 H -0.36770 0.27920 0.86000 H32 H -0.32880 0.27780 0.92470 H33 H -0.27750 0.40710 0.80700 H34 H -0.18490 0.38320 0.78420 H35 H -0.27480 0.34460 0.77030 H36 H -0.12760 0.27330 1.01370 H37 H -0.23160 0.27410 0.99420 H38 H -0.19710 0.23360 1.04810 H39 H -0.26250 0.09510 0.93070 H40 H -0.28570 0.11620 0.99340 H41 H -0.32010 0.15670 0.93950 H42 H -0.06370 0.09420 0.97910 H43 H -0.02280 0.15650 1.00720 H44 H -0.09860 0.11880 1.03810 H45 H -0.05190 -0.09550 0.76150 H46 H 0.04630 -0.07280 0.77860 H47 H 0.01850 -0.05990 0.68340 H48 H -0.06970 -0.02130 0.69180 H49 H -0.04920 -0.08340 0.86790 H50 H 0.04470 -0.04850 0.86430 H51 H -0.03600 -0.01510 0.89400 H52 H -0.17490 -0.04830 0.81100 H53 H -0.16520 0.02370 0.82740 H54 H -0.16190 0.00250 0.76240 H55 H 0.04560 0.03500 0.62350 H56 H -0.03690 0.07080 0.64880 H57 H 0.06130 0.10010 0.65540 H58 H 0.16090 -0.00510 0.68180 H59 H 0.17300 0.05690 0.71890 H60 H 0.15410 -0.00800 0.74930 H61 H 0.02330 0.33920 0.56950 H62 H 0.09100 0.28370 0.58100 H63 H 0.16870 0.36930 0.58740 H64 H 0.09840 0.40390 0.62340 H65 H -0.07020 0.23880 0.59420 H66 H 0.01420 0.20450 0.62490 H67 H -0.06910 0.22380 0.66080 H68 H -0.10690 0.33980 0.61300 H69 H -0.10410 0.32800 0.68020 H70 H -0.04500 0.38230 0.65480 H71 H 0.29940 0.33730 0.63680 H72 H 0.28670 0.30130 0.69530 H73 H 0.23640 0.27720 0.63770 H74 H 0.25330 0.43170 0.67290 H75 H 0.16010 0.43570 0.70280 H76 H 0.24350 0.40110 0.73420 H77 H -0.15590 0.46600 1.18420 H78 H -0.07300 0.50640 1.17020 H79 H -0.05060 0.50560 1.25140 H80 H -0.09670 0.44000 1.25540 H81 H -0.19750 0.40780 1.10750 H82 H -0.12920 0.35220 1.09730 H83 H -0.15940 0.36670 1.16010 H84 H -0.12140 0.48080 1.07380 H85 H -0.02110 0.49660 1.09590 H86 H -0.04080 0.43720 1.05630 H87 H 0.01750 0.42290 1.32900 H88 H -0.02930 0.36880 1.29140 H89 H 0.07690 0.36930 1.30290 H90 H 0.08990 0.49840 1.29280 H91 H 0.15980 0.45880 1.25870 H92 H 0.09690 0.50880 1.22590 H93 H 0.25500 0.31670 1.12400 H94 H 0.17610 0.30780 1.07770 H95 H 0.15730 0.23850 1.13670 H96 H 0.19250 0.27870 1.18890 H97 H 0.21970 0.41560 1.04990 H98 H 0.11990 0.38930 1.04170 H99 H 0.13710 0.45760 1.06690 H100 H 0.29300 0.42530 1.13390 H101 H 0.21930 0.46420 1.16540 H102 H 0.25290 0.39860 1.19060 H103 H 0.02130 0.20630 1.13330 H104 H -0.05410 0.25850 1.13760 H105 H 0.01820 0.26410 1.09040 H106 H 0.07900 0.21240 1.21800 H107 H 0.11970 0.27410 1.24730 H108 H 0.01370 0.26450 1.24110 C43B C 0.4170(32) 0.5330(25) 0.0137(13) C41B C 0.4203(26) 0.4708(31) 0.0011(12) C42B C 0.4980(49) 0.4352(15) -0.0128(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Dy1 Cl1 2.624 1_555 1_555 Cl2 Dy1 2.678 1_555 1_555 Si1 C1 1.865 1_555 1_555 Si2 C2 1.889 1_555 1_555 Si3 C3 1.866 1_555 1_555 Si4 C4 1.841 1_555 1_555 C1 Dy1 2.723 1_555 1_555 C2 Dy1 2.732 1_555 1_555 B1 Dy1 2.700 1_555 1_555 B2 Dy1 2.736 1_555 1_555 B3 Dy1 2.739 1_555 1_555 B4 C1 1.699 1_555 1_555 C3 Dy1 2.664 1_555 1_555 C4 Dy1 2.682 1_555 1_555 B5 Dy1 2.687 1_555 1_555 B6 Dy1 2.727 1_555 1_555 B7 Dy1 2.708 1_555 1_555 B8 C3 1.712 1_555 1_555 C5 Si1 1.887 1_555 1_555 C6 Si1 1.850 1_555 1_555 C7 Si1 1.851 1_555 1_555 C8 Si2 1.832 1_555 1_555 C9 Si2 1.850 1_555 1_555 C10 Si2 1.825 1_555 1_555 C11 Si3 1.852 1_555 1_555 C12 Si3 1.843 1_555 1_555 C13 Si3 1.828 1_555 1_555 C14 Si4 1.884 1_555 1_555 C15 Si4 1.845 1_555 1_555 C16 Si4 1.824 1_555 1_555 Li1 B1 2.388 1_555 1_555 N1 Li1 2.246 1_555 1_555 N2 Li1 2.169 1_555 1_555 C17 N1 1.472 1_555 1_555 C18 N2 1.466 1_555 1_555 C19 N1 1.416 1_555 1_555 C20 N1 1.417 1_555 1_555 C21 N2 1.445 1_555 1_555 C22 N2 1.427 1_555 1_555 Li2 Cl2 2.386 1_555 1_555 N3 Li2 2.115 1_555 1_555 N4 Li2 2.140 1_555 1_555 C23 N3 1.437 1_555 1_555 C24 N4 1.423 1_555 1_555 C25 N3 1.436 1_555 1_555 C26 N3 1.442 1_555 1_555 C27 N4 1.408 1_555 1_555 C28 N4 1.410 1_555 1_555 Li3 N5 2.128 1_555 1_555 N5 C29 1.430 1_555 1_555 N6 Li3 2.082 1_555 1_555 C29 C30 1.306 1_555 1_555 C30 N6 1.458 1_555 1_555 C31 N5 1.381 1_555 1_555 C32 N5 1.324 1_555 1_555 C33 N6 1.400 1_555 1_555 C34 N6 1.400 1_555 1_555 N7 Li3 2.118 1_555 1_555 N8 Li3 2.063 1_555 1_555 C35 N7 1.498 1_555 1_555 C36 N8 1.348 1_555 1_555 C37 N7 1.376 1_555 1_555 C38 N7 1.448 1_555 1_555 C39 N8 1.420 1_555 1_555 C40 N8 1.399 1_555 1_555 C41 C42 1.416 1_555 1_555 C42 C43B 1.417 1_555 1_555 C43 C41 1.343 1_555 1_555 H1 B1 1.083 1_555 1_555 H2 B2 1.228 1_555 1_555 H3 B3 1.259 1_555 1_555 H4 B4 1.224 1_555 1_555 H5 B5 1.230 1_555 1_555 H6 B6 1.231 1_555 1_555 H7 B7 1.189 1_555 1_555 H8 B8 1.231 1_555 1_555 H9 C5 0.960 1_555 1_555 H10 C5 0.959 1_555 1_555 H11 C5 0.960 1_555 1_555 H12 C6 0.960 1_555 1_555 H13 C6 0.960 1_555 1_555 H14 C6 0.960 1_555 1_555 H15 C7 0.961 1_555 1_555 H16 C7 0.959 1_555 1_555 H17 C7 0.959 1_555 1_555 H18 C8 0.960 1_555 1_555 H19 C8 0.960 1_555 1_555 H20 C8 0.960 1_555 1_555 H21 C9 0.960 1_555 1_555 H22 C9 0.960 1_555 1_555 H23 C9 0.960 1_555 1_555 H24 C10 0.960 1_555 1_555 H25 C10 0.962 1_555 1_555 H26 C10 0.959 1_555 1_555 H27 C11 0.961 1_555 1_555 H28 C11 0.959 1_555 1_555 H29 C11 0.960 1_555 1_555 H30 C12 0.960 1_555 1_555 H31 C12 0.961 1_555 1_555 H32 C12 0.959 1_555 1_555 H33 C13 0.959 1_555 1_555 H34 C13 0.960 1_555 1_555 H35 C13 0.960 1_555 1_555 H36 C14 0.960 1_555 1_555 H37 C14 0.958 1_555 1_555 H38 C14 0.962 1_555 1_555 H39 C15 0.960 1_555 1_555 H40 C15 0.961 1_555 1_555 H41 C15 0.960 1_555 1_555 H42 C16 0.963 1_555 1_555 H43 C16 0.967 1_555 1_555 H44 C16 0.958 1_555 1_555 H45 C17 0.959 1_555 1_555 H46 C17 0.960 1_555 1_555 H47 C18 0.959 1_555 1_555 H48 C18 0.961 1_555 1_555 H49 C19 0.960 1_555 1_555 H50 C19 0.960 1_555 1_555 H51 C19 0.960 1_555 1_555 H52 C20 0.960 1_555 1_555 H53 C20 0.958 1_555 1_555 H54 C20 0.962 1_555 1_555 H55 C21 0.958 1_555 1_555 H56 C21 0.960 1_555 1_555 H57 C21 0.960 1_555 1_555 H58 C22 0.959 1_555 1_555 H59 C22 0.959 1_555 1_555 H60 C22 0.961 1_555 1_555 H61 C23 0.961 1_555 1_555 H62 C23 0.959 1_555 1_555 H63 C24 0.960 1_555 1_555 H64 C24 0.960 1_555 1_555 H65 C25 0.960 1_555 1_555 H66 C25 0.960 1_555 1_555 H67 C25 0.960 1_555 1_555 H68 C26 0.960 1_555 1_555 H69 C26 0.961 1_555 1_555 H70 C26 0.960 1_555 1_555 H71 C27 0.961 1_555 1_555 H72 C27 0.958 1_555 1_555 H73 C27 0.961 1_555 1_555 H74 C28 0.961 1_555 1_555 H75 C28 0.961 1_555 1_555 H76 C28 0.959 1_555 1_555 H77 C29 0.960 1_555 1_555 H78 C29 0.961 1_555 1_555 H79 C30 0.960 1_555 1_555 H80 C30 0.960 1_555 1_555 H81 C31 0.960 1_555 1_555 H82 C31 0.959 1_555 1_555 H83 C31 0.960 1_555 1_555 H84 C32 0.959 1_555 1_555 H85 C32 0.960 1_555 1_555 H86 C32 0.960 1_555 1_555 H87 C33 0.961 1_555 1_555 H88 C33 0.959 1_555 1_555 H89 C33 0.959 1_555 1_555 H90 C34 0.961 1_555 1_555 H91 C34 0.960 1_555 1_555 H92 C34 0.958 1_555 1_555 H93 C35 0.960 1_555 1_555 H94 C35 0.960 1_555 1_555 H95 C36 0.962 1_555 1_555 H96 C36 0.959 1_555 1_555 H97 C37 0.961 1_555 1_555 H98 C37 0.958 1_555 1_555 H99 C37 0.962 1_555 1_555 H100 C38 0.960 1_555 1_555 H101 C38 0.960 1_555 1_555 H102 C38 0.959 1_555 1_555 H103 C39 0.960 1_555 1_555 H104 C39 0.960 1_555 1_555 H105 C39 0.959 1_555 1_555 H106 C40 0.960 1_555 1_555 H107 C40 0.960 1_555 1_555 H108 C40 0.960 1_555 1_555 C43B C41B 1.343 1_555 1_555 C41B C42B 1.416 1_555 1_555 C42B C43 1.417 1_555 1_555 C1 C2 1.482 1_555 1_555 C1 B3 1.551 1_555 1_555 C2 B4 1.675 1_555 1_555 C2 B1 1.544 1_555 1_555 B1 B2 1.594 1_555 1_555 B1 B4 1.770 1_555 1_555 B2 B4 1.761 1_555 1_555 B2 B3 1.640 1_555 1_555 B2 Li2 2.647 1_555 1_555 B3 B4 1.784 1_555 1_555 B3 Li2 2.390 1_555 1_555 C3 C4 1.487 1_555 1_555 C3 B7 1.552 1_555 1_555 C4 B8 1.711 1_555 1_555 C4 B5 1.561 1_555 1_555 B5 Li1 2.525 1_555 1_555 B5 B6 1.604 1_555 1_555 B5 B8 1.768 1_555 1_555 B6 B7 1.603 1_555 1_555 B6 B8 1.778 1_555 1_555 B6 Li1 2.346 1_555 1_555 B7 B8 1.773 1_555 1_555 Li1 H1 1.607 1_555 1_555 Li1 H6 2.092 1_555 1_555 Li1 H5 2.412 1_555 1_555 C17 C18 1.450 1_555 1_555 Li2 H2 2.650 1_555 1_555 Li2 H3 2.361 1_555 1_555 C23 C24 1.411 1_555 1_555 C35 C36 1.353 1_555 1_555 #END