 
data_73
  
_audit_creation_method            'SHELXL-2018/3' 
_shelx_SHELXL_version_number      '2018/3' 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C30 H36 N4 O11 U, H2 O' 
_chemical_formula_sum 
 'C30 H38 N4 O12 U' 
_chemical_formula_weight          884.67 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'U'  'U'  -9.6767   9.6646 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_space_group_crystal_system       triclinic 
_space_group_IT_number            2 
_space_group_name_H-M_alt         'P -1' 
_space_group_name_Hall            '-P 1' 
  
_shelx_space_group_comment 
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
; 
  
loop_ 
 _space_group_symop_operation_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    9.0575(7) 
_cell_length_b                    9.1343(7) 
_cell_length_c                    23.2937(15) 
_cell_angle_alpha                 79.065(6) 
_cell_angle_beta                  83.148(6) 
_cell_angle_gamma                 62.129(8) 
_cell_volume                      1671.7(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     6400 
_cell_measurement_theta_min       2.5900 
_cell_measurement_theta_max       26.0770 
  
_exptl_crystal_description        'platy needles' 
_exptl_crystal_colour             Yellow 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     1.758 
_exptl_crystal_F_000              868 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.263 
_exptl_crystal_size_mid           0.069 
_exptl_crystal_size_min           0.021 
_exptl_absorpt_coefficient_mu     4.922 
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    analytical 
_exptl_absorpt_correction_T_min   0.497 
_exptl_absorpt_correction_T_max   0.908 
_exptl_absorpt_process_details     
; 
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
; 
_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_source                    'Enhance (Mo) X-ray Source' 
_diffrn_measurement_device_type   'Agilent Xcalibur 3 E' 
_diffrn_measurement_method        'omega scans' 
_diffrn_detector_area_resol_mean  16.0382 
_diffrn_reflns_number             7830 
_diffrn_reflns_av_unetI/netI      0.2153 
_diffrn_reflns_av_R_equivalents   0.0855
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -29 
_diffrn_reflns_limit_l_max        30 
_diffrn_reflns_theta_min          2.545 
_diffrn_reflns_theta_max          28.333 
_diffrn_reflns_theta_full         25.242 
_diffrn_measured_fraction_theta_max   0.847 
_diffrn_measured_fraction_theta_full  0.997 
_diffrn_reflns_Laue_measured_fraction_max    0.847 
_diffrn_reflns_Laue_measured_fraction_full   0.997 
_diffrn_reflns_point_group_measured_fraction_max   0.847 
_diffrn_reflns_point_group_measured_fraction_full  0.997 
_reflns_number_total              7830 
_reflns_number_gt                 4548 
_reflns_threshold_expression      'I > 2σ(I)' 
_reflns_Friedel_coverage          0.000 
_reflns_Friedel_fraction_max      . 
_reflns_Friedel_fraction_full     . 
  
_reflns_special_details 
; 
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. Completness statistics refer to single and 
 composite reflections containing twin component 1 only. 
; 
  
_computing_data_collection        'CrysAlisPro, Rigaku OD' 
_computing_cell_refinement        'CrysAlisPro, Rigaku OD' 
_computing_data_reduction         'CrysAlisPro, Rigaku OD' 
_computing_structure_solution     'SHELXS-2014 (Sheldrick, 2017)' 
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'CIFTAB-2014 (Sheldrick, 2017)' 
_refine_special_details 
; 
 Refined as a 2-component twin. 
; 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.1282P)²] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      ? 
_atom_sites_solution_secondary    ? 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        . 
_refine_ls_number_reflns          7830 
_refine_ls_number_parameters      456 
_refine_ls_number_restraints      181 
_refine_ls_R_factor_all           0.1296 
_refine_ls_R_factor_gt            0.0941 
_refine_ls_wR_factor_ref          0.2527 
_refine_ls_wR_factor_gt           0.2440 
_refine_ls_goodness_of_fit_ref    1.020 
_refine_ls_restrained_S_all       1.012 
_refine_ls_shift/su_max           0.002 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_site_symmetry_order 
 _atom_site_calc_flag 
 _atom_site_refinement_flags_posn 
 _atom_site_refinement_flags_adp 
 _atom_site_refinement_flags_occupancy 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
U1 U 0.39144(12) 0.61998(11) 0.31361(4) 0.0252(3) Uani 1 1 d . . . . . 
N1 N 0.074(2) 1.311(2) 0.3153(9) 0.035(5) Uani 1 1 d . . . . . 
N2 N 0.0689(19) 1.1906(18) 0.2892(8) 0.026(4) Uani 1 1 d . . . . . 
C3 C 0.182(2) 1.029(2) 0.3128(9) 0.024(5) Uani 1 1 d . . . . . 
O3 O 0.2022(18) 0.9013(16) 0.2923(7) 0.041(4) Uani 1 1 d . . . . . 
C4 C 0.261(3) 1.055(2) 0.3548(9) 0.029(5) Uani 1 1 d . . . . . 
C5 C 0.192(2) 1.228(2) 0.3551(9) 0.028(5) Uani 1 1 d . U . . . 
H5 H 0.223759 1.279346 0.379834 0.033 Uiso 1 1 calc R U . . . 
C6 C -0.042(3) 1.239(2) 0.2406(10) 0.033(5) Uani 1 1 d . . . . . 
H6A H -0.152477 1.330296 0.249808 0.040 Uiso 0.592(18) 1 calc R U P A 1 
H6B H -0.057225 1.142391 0.235355 0.040 Uiso 0.592(18) 1 calc R U P A 1 
H6C H -0.137431 1.350125 0.244472 0.040 Uiso 0.408(18) 1 calc R U P A 2 
H6D H -0.086557 1.157660 0.244132 0.040 Uiso 0.408(18) 1 calc R U P A 2 
C7 C 0.031(3) 1.298(3) 0.1852(10) 0.037(9) Uani 0.592(18) 1 d DG U P A 1 
C8 C -0.070(3) 1.450(3) 0.1520(13) 0.054(11) Uani 0.592(18) 1 d DG U P A 1 
H8A H -0.179372 1.518484 0.166298 0.064 Uiso 0.592(18) 1 calc R U P A 1 
C9 C -0.012(4) 1.500(4) 0.0979(13) 0.085(14) Uani 0.592(18) 1 d DG U P A 1 
H9A H -0.081116 1.603943 0.075191 0.103 Uiso 0.592(18) 1 calc R U P A 1 
C10 C 0.147(4) 1.399(4) 0.0769(11) 0.092(14) Uani 0.592(18) 1 d DG U P A 1 
C11 C 0.249(3) 1.248(4) 0.1101(13) 0.070(13) Uani 0.592(18) 1 d DG U P A 1 
H11A H 0.357603 1.178652 0.095773 0.084 Uiso 0.592(18) 1 calc R U P A 1 
C12 C 0.190(3) 1.197(3) 0.1642(12) 0.036(8) Uani 0.592(18) 1 d DG U P A 1 
H12A H 0.259350 1.093190 0.186881 0.044 Uiso 0.592(18) 1 calc R U P A 1 
O13 O 0.210(6) 1.462(6) 0.0244(18) 0.110(13) Uani 0.592(18) 1 d D U P A 1 
C14 C 0.327(6) 1.410(6) 0.001(2) 0.061(11) Uani 0.592(18) 1 d D U P A 1 
H14A H 0.326920 1.489628 -0.033992 0.091 Uiso 0.592(18) 1 calc R U P A 1 
H14B H 0.417730 1.386577 0.025907 0.091 Uiso 0.592(18) 1 calc R U P A 1 
H14C H 0.345180 1.305467 -0.011191 0.091 Uiso 0.592(18) 1 calc R U P A 1 
C7' C 0.039(5) 1.249(5) 0.1801(16) 0.039(11) Uiso 0.408(18) 1 d DG U P A 2 
C8' C 0.032(6) 1.403(5) 0.1542(19) 0.053(14) Uiso 0.408(18) 1 d DG U P A 2 
H8'A H -0.026317 1.497440 0.173819 0.063 Uiso 0.408(18) 1 calc R U P A 2 
C9' C 0.109(7) 1.417(5) 0.100(2) 0.084(14) Uiso 0.408(18) 1 d DG U P A 2 
H9'A H 0.103632 1.522094 0.081993 0.101 Uiso 0.408(18) 1 calc R U P A 2 
C10' C 0.194(7) 1.278(6) 0.0710(17) 0.081(16) Uiso 0.408(18) 1 d DG U P A 2 
C11' C 0.201(6) 1.125(5) 0.0969(18) 0.076(16) Uiso 0.408(18) 1 d DG U P A 2 
H11B H 0.259427 1.029988 0.077332 0.092 Uiso 0.408(18) 1 calc R U P A 2 
C12' C 0.124(6) 1.110(4) 0.1515(18) 0.046(12) Uiso 0.408(18) 1 d DG U P A 2 
H12B H 0.129479 1.005331 0.169158 0.056 Uiso 0.408(18) 1 calc R U P A 2 
O13' O 0.287(7) 1.291(7) 0.019(2) 0.087(13) Uiso 0.408(18) 1 d D U P A 2 
C14' C 0.414(8) 1.266(10) 0.006(3) 0.072(14) Uiso 0.408(18) 1 d D U P A 2 
H14D H 0.422530 1.294927 -0.036997 0.108 Uiso 0.408(18) 1 calc R U P A 2 
H14E H 0.445178 1.334520 0.024502 0.108 Uiso 0.408(18) 1 calc R U P A 2 
H14F H 0.488929 1.147471 0.017453 0.108 Uiso 0.408(18) 1 calc R U P A 2 
C15 C 0.398(3) 0.919(2) 0.3862(9) 0.028(5) Uani 1 1 d . . . . . 
O15 O 0.4510(19) 0.7703(16) 0.3774(7) 0.039(4) Uani 1 1 d . . . . . 
O16 O 0.4646(18) 0.9538(15) 0.4257(6) 0.032(3) Uani 1 1 d . . . . . 
C17 C 0.612(3) 0.819(2) 0.4553(9) 0.033(5) Uani 1 1 d . . . . . 
H17A H 0.678238 0.867064 0.468564 0.040 Uiso 1 1 calc R U . . . 
H17B H 0.683563 0.740799 0.428009 0.040 Uiso 1 1 calc R U . . . 
C18 C 0.557(4) 0.727(3) 0.5074(10) 0.046(7) Uani 1 1 d . . . . . 
H18A H 0.476766 0.696549 0.495005 0.069 Uiso 1 1 calc R U . . . 
H18B H 0.503681 0.800145 0.537459 0.069 Uiso 1 1 calc R U . . . 
H18C H 0.654196 0.625838 0.523477 0.069 Uiso 1 1 calc R U . . . 
N21 N 0.770(2) -0.071(2) 0.3147(8) 0.033(4) Uani 1 1 d . . . . . 
N22 N 0.630(2) 0.0662(19) 0.2904(8) 0.029(4) Uani 1 1 d . . . . . 
C23 C 0.597(3) 0.206(3) 0.3112(10) 0.030(5) Uani 1 1 d . . . . . 
O23 O 0.4772(19) 0.3486(17) 0.2922(7) 0.042(4) Uani 1 1 d . . . . . 
C24 C 0.717(3) 0.160(3) 0.3535(9) 0.031(5) Uani 1 1 d . . . . . 
C25 C 0.821(3) -0.014(2) 0.3516(9) 0.029(5) Uani 1 1 d . U . . . 
H25 H 0.917044 -0.081068 0.374467 0.035 Uiso 1 1 calc R U . . . 
C26 C 0.542(3) 0.049(2) 0.2462(10) 0.035(6) Uani 1 1 d . . . . . 
H26A H 0.423947 0.134638 0.248555 0.043 Uiso 0.58(3) 1 calc R U P B 1 
H26B H 0.543382 -0.061870 0.257065 0.043 Uiso 0.58(3) 1 calc R U P B 1 
H26C H 0.431877 0.148608 0.240329 0.043 Uiso 0.42(3) 1 calc R U P B 3 
H26D H 0.523509 -0.051154 0.258903 0.043 Uiso 0.42(3) 1 calc R U P B 3 
C27 C 0.601(5) 0.063(4) 0.1831(10) 0.047(10) Uani 0.58(3) 1 d DG U P B 1 
C28 C 0.653(5) 0.184(4) 0.1604(13) 0.042(8) Uani 0.58(3) 1 d DG U P B 1 
H28A H 0.646768 0.261092 0.184189 0.050 Uiso 0.58(3) 1 calc R U P B 1 
C29 C 0.714(5) 0.193(4) 0.1029(13) 0.038(9) Uani 0.58(3) 1 d DG U P B 1 
H29A H 0.749768 0.276326 0.087377 0.046 Uiso 0.58(3) 1 calc R U P B 1 
C30 C 0.724(5) 0.081(4) 0.0681(10) 0.065(13) Uani 0.58(3) 1 d DG U P B 1 
C31 C 0.672(5) -0.040(4) 0.0908(11) 0.052(11) Uani 0.58(3) 1 d DG U P B 1 
H31A H 0.678339 -0.116805 0.067077 0.062 Uiso 0.58(3) 1 calc R U P B 1 
C32 C 0.611(5) -0.049(4) 0.1484(12) 0.034(9) Uani 0.58(3) 1 d DG U P B 1 
H32A H 0.575338 -0.132042 0.163889 0.041 Uiso 0.58(3) 1 calc R U P B 1 
O33 O 0.760(5) 0.106(5) 0.0113(13) 0.057(8) Uani 0.58(3) 1 d D U P B 1 
C34 C 0.738(8) 0.010(7) -0.023(2) 0.076(13) Uani 0.58(3) 1 d D U P B 1 
H34A H 0.768280 0.039041 -0.064070 0.115 Uiso 0.58(3) 1 calc R U P B 1 
H34B H 0.809855 -0.109135 -0.009773 0.115 Uiso 0.58(3) 1 calc R U P B 1 
H34C H 0.621022 0.031462 -0.020232 0.115 Uiso 0.58(3) 1 calc R U P B 1 
C27' C 0.649(6) 0.031(6) 0.1876(14) 0.034(12) Uiso 0.42(3) 1 d DG U P B 3 
C28' C 0.679(8) 0.164(6) 0.1602(19) 0.048(12) Uiso 0.42(3) 1 d DG U P B 3 
H28B H 0.654439 0.254214 0.180339 0.058 Uiso 0.42(3) 1 calc R U P B 3 
C29' C 0.746(7) 0.164(5) 0.1032(19) 0.037(10) Uiso 0.42(3) 1 d DG U P B 3 
H29B H 0.766350 0.255413 0.084469 0.045 Uiso 0.42(3) 1 calc R U P B 3 
C30' C 0.782(6) 0.032(5) 0.0737(14) 0.052(14) Uiso 0.42(3) 1 d DG U P B 3 
C31' C 0.752(6) -0.101(5) 0.1011(16) 0.040(12) Uiso 0.42(3) 1 d DG U P B 3 
H31B H 0.777356 -0.191490 0.080913 0.048 Uiso 0.42(3) 1 calc R U P B 3 
C32' C 0.686(6) -0.102(5) 0.1580(15) 0.034(12) Uiso 0.42(3) 1 d DG U P B 3 
H32B H 0.665445 -0.192693 0.176783 0.041 Uiso 0.42(3) 1 calc R U P B 3 
O33' O 0.851(8) 0.028(7) 0.0200(18) 0.067(12) Uiso 0.42(3) 1 d D U P B 3 
C34' C 0.887(12) -0.115(9) -0.004(3) 0.095(18) Uiso 0.42(3) 1 d D U P B 3 
H34D H 0.936944 -0.107503 -0.043145 0.142 Uiso 0.42(3) 1 calc R U P B 3 
H34E H 0.965895 -0.214563 0.021065 0.142 Uiso 0.42(3) 1 calc R U P B 3 
H34F H 0.783884 -0.123549 -0.005577 0.142 Uiso 0.42(3) 1 calc R U P B 3 
C35 C 0.728(3) 0.274(2) 0.3842(9) 0.029(5) Uani 1 1 d . . . . . 
O35 O 0.6274(16) 0.4298(16) 0.3762(6) 0.033(4) Uani 1 1 d . . . . . 
O36 O 0.8356(18) 0.2135(16) 0.4237(7) 0.036(4) Uani 1 1 d . . . . . 
C37 C 0.841(3) 0.330(2) 0.4570(11) 0.035(6) Uani 1 1 d . . . . . 
H37A H 0.730160 0.394024 0.475430 0.042 Uiso 1 1 calc R U . . . 
H37B H 0.872816 0.410926 0.430800 0.042 Uiso 1 1 calc R U . . . 
C38 C 0.970(3) 0.230(3) 0.5037(11) 0.053(8) Uani 1 1 d . . . . . 
H38A H 0.962964 0.304248 0.530495 0.080 Uiso 1 1 calc R U . . . 
H38B H 1.081812 0.182967 0.485119 0.080 Uiso 1 1 calc R U . . . 
H38C H 0.947345 0.139702 0.525533 0.080 Uiso 1 1 calc R U . . . 
O40 O 0.2247(18) 0.6452(16) 0.2378(6) 0.033(3) Uani 1 1 d D . . . . 
C41 C 0.200(6) 0.739(5) 0.1774(16) 0.061(12) Uani 0.55(3) 1 d D U P C 1 
H41A H 0.191095 0.852058 0.176536 0.074 Uiso 0.55(3) 1 calc R U P C 1 
H41B H 0.098496 0.751397 0.160983 0.074 Uiso 0.55(3) 1 calc R U P C 1 
C42 C 0.364(6) 0.626(5) 0.1425(17) 0.050(11) Uani 0.55(3) 1 d D U P C 1 
H42A H 0.389636 0.508226 0.154166 0.076 Uiso 0.55(3) 1 calc R U P C 1 
H42B H 0.457434 0.642907 0.151360 0.076 Uiso 0.55(3) 1 calc R U P C 1 
H42C H 0.344849 0.658228 0.100398 0.076 Uiso 0.55(3) 1 calc R U P C 1 
C41' C 0.278(6) 0.587(5) 0.1800(16) 0.036(10) Uiso 0.45(3) 1 d D U P C 2 
H41C H 0.244974 0.499651 0.176844 0.043 Uiso 0.45(3) 1 calc R U P C 2 
H41D H 0.399886 0.542502 0.173098 0.043 Uiso 0.45(3) 1 calc R U P C 2 
C42' C 0.180(8) 0.753(7) 0.1353(19) 0.064(13) Uiso 0.45(3) 1 d D U P C 2 
H42D H 0.199258 0.725137 0.095516 0.095 Uiso 0.45(3) 1 calc R U P C 2 
H42E H 0.219751 0.834166 0.137368 0.095 Uiso 0.45(3) 1 calc R U P C 2 
H42F H 0.059854 0.800257 0.145463 0.095 Uiso 0.45(3) 1 calc R U P C 2 
O50 O 0.2448(18) 0.5922(19) 0.3657(7) 0.039(4) Uani 1 1 d . U . . . 
O60 O 0.541(2) 0.645(2) 0.2609(7) 0.056(5) Uani 1 1 d . . . . . 
O70 O 0.9501(18) 0.6399(17) 0.2648(7) 0.040(4) Uani 1 1 d . . . . . 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
U1 O50 1.765(16) . ? 
U1 O60 1.785(17) . ? 
U1 O3 2.321(13) . ? 
U1 O23 2.361(13) . ? 
U1 O40 2.368(15) . ? 
U1 O35 2.454(13) . ? 
U1 O15 2.458(13) . ? 
N1 C5 1.33(3) . ? 
N1 N2 1.37(2) . ? 
N2 C3 1.39(2) . ? 
N2 C6 1.46(3) . ? 
C3 O3 1.27(2) . ? 
C3 C4 1.39(3) . ? 
C4 C5 1.41(3) . ? 
C4 C15 1.43(3) . ? 
C6 C7 1.50(3) . ? 
C6 C7' 1.52(4) . ? 
C7 C8 1.3900 . ? 
C7 C12 1.3900 . ? 
C8 C9 1.3900 . ? 
C9 C10 1.3900 . ? 
C10 C11 1.3900 . ? 
C10 O13 1.42(4) . ? 
C11 C12 1.3900 . ? 
O13 C14 1.07(5) . ? 
C7' C8' 1.3900 . ? 
C7' C12' 1.3900 . ? 
C8' C9' 1.3900 . ? 
C9' C10' 1.3900 . ? 
C10' C11' 1.3900 . ? 
C10' O13' 1.42(4) . ? 
C11' C12' 1.3900 . ? 
O13' C14' 1.07(5) . ? 
C15 O15 1.26(2) . ? 
C15 O16 1.32(2) . ? 
O16 C17 1.46(2) . ? 
C17 C18 1.51(3) . ? 
N21 C25 1.31(3) . ? 
N21 N22 1.38(2) . ? 
N22 C23 1.34(2) . ? 
N22 C26 1.44(3) . ? 
C23 O23 1.29(3) . ? 
C23 C24 1.42(3) . ? 
C24 C35 1.41(3) . ? 
C24 C25 1.43(3) . ? 
C26 C27 1.51(3) . ? 
C26 C27' 1.57(4) . ? 
C27 C28 1.3900 . ? 
C27 C32 1.3900 . ? 
C28 C29 1.3900 . ? 
C29 C30 1.3900 . ? 
C30 O33 1.33(3) . ? 
C30 C31 1.3900 . ? 
C31 C32 1.3900 . ? 
O33 C34 1.39(5) . ? 
C27' C28' 1.3900 . ? 
C27' C32' 1.3900 . ? 
C28' C29' 1.3900 . ? 
C29' C30' 1.3900 . ? 
C30' O33' 1.33(3) . ? 
C30' C31' 1.3900 . ? 
C31' C32' 1.3900 . ? 
O33' C34' 1.39(5) . ? 
C35 O35 1.27(2) . ? 
C35 O36 1.28(3) . ? 
O36 C37 1.46(2) . ? 
C37 C38 1.52(3) . ? 
O40 C41' 1.48(4) . ? 
O40 C41 1.48(4) . ? 
C41 C42 1.59(5) . ? 
C41' C42' 1.59(5) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O50 U1 O60 179.2(9) . . ? 
O50 U1 O3 88.9(6) . . ? 
O60 U1 O3 91.8(8) . . ? 
O50 U1 O23 88.8(6) . . ? 
O60 U1 O23 90.4(7) . . ? 
O3 U1 O23 145.0(5) . . ? 
O50 U1 O40 89.5(6) . . ? 
O60 U1 O40 90.6(7) . . ? 
O3 U1 O40 72.8(5) . . ? 
O23 U1 O40 72.2(5) . . ? 
O50 U1 O35 92.6(6) . . ? 
O60 U1 O35 87.0(7) . . ? 
O3 U1 O35 141.2(4) . . ? 
O23 U1 O35 73.8(5) . . ? 
O40 U1 O35 145.9(4) . . ? 
O50 U1 O15 91.2(6) . . ? 
O60 U1 O15 89.2(7) . . ? 
O3 U1 O15 72.9(5) . . ? 
O23 U1 O15 142.0(5) . . ? 
O40 U1 O15 145.7(4) . . ? 
O35 U1 O15 68.3(4) . . ? 
C5 N1 N2 106.1(15) . . ? 
N1 N2 C3 112.0(16) . . ? 
N1 N2 C6 120.4(15) . . ? 
C3 N2 C6 127.6(16) . . ? 
O3 C3 C4 134.3(18) . . ? 
O3 C3 N2 121.5(18) . . ? 
C4 C3 N2 104.1(17) . . ? 
C3 O3 U1 131.6(13) . . ? 
C3 C4 C5 108.1(19) . . ? 
C3 C4 C15 121.8(17) . . ? 
C5 C4 C15 129.9(19) . . ? 
N1 C5 C4 109.8(19) . . ? 
N2 C6 C7 110.5(19) . . ? 
N2 C6 C7' 115(2) . . ? 
C8 C7 C12 120.0 . . ? 
C8 C7 C6 118.6(18) . . ? 
C12 C7 C6 121.2(18) . . ? 
C9 C8 C7 120.0 . . ? 
C8 C9 C10 120.0 . . ? 
C11 C10 C9 120.0 . . ? 
C11 C10 O13 121(3) . . ? 
C9 C10 O13 119(3) . . ? 
C10 C11 C12 120.0 . . ? 
C11 C12 C7 120.0 . . ? 
C14 O13 C10 132(5) . . ? 
C8' C7' C12' 120.0 . . ? 
C8' C7' C6 118(3) . . ? 
C12' C7' C6 122(3) . . ? 
C7' C8' C9' 120.0 . . ? 
C10' C9' C8' 120.0 . . ? 
C9' C10' C11' 120.0 . . ? 
C9' C10' O13' 119(3) . . ? 
C11' C10' O13' 121(3) . . ? 
C10' C11' C12' 120.0 . . ? 
C11' C12' C7' 120.0 . . ? 
C14' O13' C10' 138(6) . . ? 
O15 C15 O16 120.8(19) . . ? 
O15 C15 C4 121.3(18) . . ? 
O16 C15 C4 117.9(16) . . ? 
C15 O15 U1 138.1(14) . . ? 
C15 O16 C17 119.0(15) . . ? 
O16 C17 C18 109.0(19) . . ? 
C25 N21 N22 105.2(15) . . ? 
C23 N22 N21 111.8(18) . . ? 
C23 N22 C26 128.0(18) . . ? 
N21 N22 C26 120.1(15) . . ? 
O23 C23 N22 122(2) . . ? 
O23 C23 C24 131.0(19) . . ? 
N22 C23 C24 107.3(18) . . ? 
C23 O23 U1 131.6(13) . . ? 
C35 C24 C23 124.3(19) . . ? 
C35 C24 C25 132(2) . . ? 
C23 C24 C25 103.1(18) . . ? 
N21 C25 C24 112(2) . . ? 
N22 C26 C27 119(2) . . ? 
N22 C26 C27' 109(2) . . ? 
C28 C27 C32 120.0 . . ? 
C28 C27 C26 120(2) . . ? 
C32 C27 C26 120(2) . . ? 
C29 C28 C27 120.0 . . ? 
C28 C29 C30 120.0 . . ? 
O33 C30 C29 119.1(19) . . ? 
O33 C30 C31 120(2) . . ? 
C29 C30 C31 120.0 . . ? 
C32 C31 C30 120.0 . . ? 
C31 C32 C27 120.0 . . ? 
C30 O33 C34 117(3) . . ? 
C28' C27' C32' 120.0 . . ? 
C28' C27' C26 119(3) . . ? 
C32' C27' C26 120(3) . . ? 
C27' C28' C29' 120.0 . . ? 
C30' C29' C28' 120.0 . . ? 
O33' C30' C29' 121(2) . . ? 
O33' C30' C31' 119(2) . . ? 
C29' C30' C31' 120.0 . . ? 
C32' C31' C30' 120.0 . . ? 
C31' C32' C27' 120.0 . . ? 
C30' O33' C34' 115(4) . . ? 
O35 C35 O36 120.1(18) . . ? 
O35 C35 C24 122(2) . . ? 
O36 C35 C24 117.3(18) . . ? 
C35 O35 U1 136.8(13) . . ? 
C35 O36 C37 117.3(15) . . ? 
O36 C37 C38 108.2(17) . . ? 
C41' O40 U1 129(2) . . ? 
C41 O40 U1 132(2) . . ? 
O40 C41 C42 103(2) . . ? 
O40 C41' C42' 103(2) . . ? 
  
_refine_diff_density_max    5.012 
_refine_diff_density_min   -2.630 
_refine_diff_density_rms    0.310 
  
  
  
# start Validation Reply Form
_vrf_PLAT430_73
;
PROBLEM: Short Inter D...A Contact  O40      ..O70      .       2.51 Ang.  
RESPONSE: ...
The three hydrogen atoms of the O40-based ethanol ligand and O70-based water
molecule could not be located from delta-F maps and so were omitted. See the
supporting information for more details.
;
_vrf_PLAT306_73
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O70 Check 
RESPONSE: ...
see _vrf_PLAT430_73 above
;
_vrf_PLAT342_73
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0325 Ang.  
RESPONSE: ...
The data set was clearly twinned, and although the best results came from a
two component twin model this still used only ca. 44% of the overall spots.
See the supporting information for more details.
;
# end Validation Reply Form

#===END



