 
data_33
  
_audit_creation_method            'SHELXL-2018/3' 
_shelx_SHELXL_version_number      '2018/3' 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety
 'C56 H60 N8 O16 Zr' 
_chemical_formula_sum 
 'C56 H60 N8 O16 Zr' 
_chemical_formula_weight          1192.34 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 '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'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Zr'  'Zr'  -0.1862   2.2449 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_space_group_crystal_system       monoclinic 
_space_group_IT_number            15 
_space_group_name_H-M_alt         'I 2/a' 
_space_group_name_Hall            '-I 2ya' 
  
_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+1/2, y, -z' 
 'x+1/2, y+1/2, z+1/2' 
 '-x+1, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y, z' 
 '-x+1/2, -y+1/2, -z+1/2' 
 'x, -y+1/2, z+1/2' 
  
_cell_length_a                    22.5461(10) 
_cell_length_b                    12.3749(5) 
_cell_length_c                    41.985(2) 
_cell_angle_alpha                 90 
_cell_angle_beta                  99.689(5) 
_cell_angle_gamma                 90 
_cell_volume                      11547.0(10) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     7273 
_cell_measurement_theta_min       3.7250 
_cell_measurement_theta_max       73.4010 
  
_exptl_crystal_description        plates 
_exptl_crystal_colour             Colourless 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     1.372 
_exptl_crystal_F_000              4960 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.203 
_exptl_crystal_size_mid           0.147 
_exptl_crystal_size_min           0.086 
_exptl_absorpt_coefficient_mu     2.191 
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    analytical 
_exptl_absorpt_correction_T_min   0.660 
_exptl_absorpt_correction_T_max   0.842 
_exptl_absorpt_process_details     
; 
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 
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      1.54184 
_diffrn_radiation_type            CuK\a 
_diffrn_source                    'Enhance Ultra (Cu) X-ray Source' 
_diffrn_measurement_device_type   'Agilent Xcalibur PX Ultra A' 
_diffrn_measurement_method        'omega scans' 
_diffrn_detector_area_resol_mean  10.4115 
_diffrn_reflns_number             19117 
_diffrn_reflns_av_unetI/netI      0.0581 
_diffrn_reflns_av_R_equivalents   0.0471 
_diffrn_reflns_limit_h_min        -27 
_diffrn_reflns_limit_h_max        25 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -52 
_diffrn_reflns_limit_l_max        51 
_diffrn_reflns_theta_min          3.728 
_diffrn_reflns_theta_max          73.899 
_diffrn_reflns_theta_full         67.684 
_diffrn_measured_fraction_theta_max   0.943 
_diffrn_measured_fraction_theta_full  0.984 
_diffrn_reflns_Laue_measured_fraction_max    0.943 
_diffrn_reflns_Laue_measured_fraction_full   0.984 
_diffrn_reflns_point_group_measured_fraction_max   0.943 
_diffrn_reflns_point_group_measured_fraction_full  0.984 
_reflns_number_total              11053 
_reflns_number_gt                 9404 
_reflns_threshold_expression      'I > 2σ(I)' 
_reflns_Friedel_coverage          0.000 
_reflns_Friedel_fraction_max      . 
_reflns_Friedel_fraction_full     . 
  
_reflns_special_details 
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _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. 
; 
  
_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           ? 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.0163P)²+41.3136P] 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      'SHELXL-2018/3 (Sheldrick 2018)' 
_refine_ls_extinction_coef        0.000029(3) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          11053 
_refine_ls_number_parameters      763 
_refine_ls_number_restraints      69 
_refine_ls_R_factor_all           0.0672 
_refine_ls_R_factor_gt            0.0542 
_refine_ls_wR_factor_ref          0.1208 
_refine_ls_wR_factor_gt           0.1121 
_refine_ls_goodness_of_fit_ref    1.071 
_refine_ls_restrained_S_all       1.076 
_refine_ls_shift/su_max           0.001 
_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 
Zr1 Zr 0.40125(2) 0.73856(2) 0.12216(2) 0.03087(9) Uani 1 1 d . . . . . 
N1 N 0.19651(15) 0.6247(3) 0.04822(8) 0.0508(9) Uani 1 1 d . . . . . 
N2 N 0.23045(14) 0.6083(3) 0.07877(8) 0.0418(7) Uani 1 1 d . . . . . 
C3 C 0.27557(15) 0.6796(3) 0.08526(8) 0.0345(7) Uani 1 1 d . . . . . 
O3 O 0.31259(11) 0.6800(2) 0.11267(5) 0.0364(5) Uani 1 1 d . . . . . 
C4 C 0.27231(16) 0.7475(3) 0.05838(8) 0.0369(8) Uani 1 1 d . . . . . 
C5 C 0.22196(17) 0.7091(4) 0.03674(10) 0.0473(9) Uani 1 1 d . . . . . 
H5A H 0.207923 0.740511 0.016203 0.057 Uiso 1 1 calc R U . . . 
C6 C 0.21694(18) 0.5193(3) 0.09905(10) 0.0463(9) Uani 1 1 d . . . . . 
H6A H 0.174512 0.497305 0.092098 0.056 Uiso 1 1 calc R U . . . 
H6B H 0.221208 0.544874 0.121659 0.056 Uiso 1 1 calc R U . . . 
C7 C 0.25686(18) 0.4217(3) 0.09796(10) 0.0455(9) Uani 1 1 d . . . . . 
C8 C 0.2380(2) 0.3345(4) 0.07773(11) 0.0558(11) Uani 1 1 d . . . . . 
H8A H 0.199573 0.336278 0.064364 0.067 Uiso 1 1 calc R U . . . 
C9 C 0.2747(2) 0.2457(4) 0.07697(12) 0.0653(13) Uani 1 1 d . . . . . 
H9A H 0.260968 0.186427 0.063323 0.078 Uiso 1 1 calc R U . . . 
C10 C 0.3313(2) 0.2416(4) 0.09579(13) 0.0616(12) Uani 1 1 d . . . . . 
C11 C 0.3502(2) 0.3267(4) 0.11607(13) 0.0634(13) Uani 1 1 d . . . . . 
H11A H 0.388722 0.324574 0.129377 0.076 Uiso 1 1 calc R U . . . 
C12 C 0.3130(2) 0.4160(4) 0.11707(12) 0.0554(11) Uani 1 1 d . . . . . 
H12A H 0.326421 0.474218 0.131198 0.066 Uiso 1 1 calc R U . . . 
O13 O 0.3632(2) 0.1491(3) 0.09293(11) 0.0853(12) Uani 1 1 d . . . . . 
C14 C 0.4223(3) 0.1412(5) 0.1121(2) 0.106(3) Uani 1 1 d . . . . . 
H14A H 0.447394 0.200855 0.106657 0.159 Uiso 1 1 calc R U . . . 
H14B H 0.440684 0.072222 0.107723 0.159 Uiso 1 1 calc R U . . . 
H14C H 0.419162 0.145238 0.135102 0.159 Uiso 1 1 calc R U . . . 
C15 C 0.31715(16) 0.8269(3) 0.05614(8) 0.0339(7) Uani 1 1 d . . . . . 
O15 O 0.36334(11) 0.8381(2) 0.07669(5) 0.0362(5) Uani 1 1 d . . . . . 
O16 O 0.30761(12) 0.8877(2) 0.02955(6) 0.0439(6) Uani 1 1 d D . . . . 
C17 C 0.3567(4) 0.9601(8) 0.02444(19) 0.0462(18) Uani 0.86(3) 1 d D . P A 1 
H17A H 0.393100 0.917717 0.022328 0.055 Uiso 0.86(3) 1 calc R U P A 1 
H17B H 0.366789 1.010184 0.042943 0.055 Uiso 0.86(3) 1 calc R U P A 1 
C18 C 0.3354(4) 1.0223(9) -0.00606(16) 0.080(3) Uani 0.86(3) 1 d D . P A 1 
H18A H 0.367197 1.071676 -0.010239 0.120 Uiso 0.86(3) 1 calc R U P A 1 
H18B H 0.325642 0.971880 -0.024184 0.120 Uiso 0.86(3) 1 calc R U P A 1 
H18C H 0.299444 1.063950 -0.003657 0.120 Uiso 0.86(3) 1 calc R U P A 1 
C17' C 0.346(2) 0.983(3) 0.0282(9) 0.033(11) Uiso 0.14(3) 1 d D . P A 2 
H17C H 0.381905 0.978943 0.045035 0.040 Uiso 0.14(3) 1 calc R U P A 2 
H17D H 0.323135 1.049653 0.031624 0.040 Uiso 0.14(3) 1 calc R U P A 2 
C18' C 0.363(4) 0.983(6) -0.0050(15) 0.12(3) Uiso 0.14(3) 1 d D . P A 2 
H18D H 0.388307 1.045990 -0.007160 0.175 Uiso 0.14(3) 1 calc R U P A 2 
H18E H 0.384752 0.916841 -0.008055 0.175 Uiso 0.14(3) 1 calc R U P A 2 
H18F H 0.326281 0.987191 -0.021398 0.175 Uiso 0.14(3) 1 calc R U P A 2 
N21 N 0.56523(18) 0.7607(3) 0.04345(9) 0.0579(10) Uani 1 1 d . . . . . 
N22 N 0.55136(15) 0.8039(3) 0.07184(8) 0.0428(7) Uani 1 1 d . . . . . 
C23 C 0.49967(15) 0.7624(3) 0.07909(8) 0.0341(7) Uani 1 1 d . . . . . 
O23 O 0.47840(11) 0.7911(2) 0.10440(6) 0.0366(5) Uani 1 1 d . . . . . 
C24 C 0.47907(17) 0.6867(3) 0.05505(9) 0.0384(8) Uani 1 1 d . . . . . 
C25 C 0.5221(2) 0.6907(4) 0.03388(11) 0.0536(11) Uani 1 1 d . . . . . 
H25A H 0.519847 0.647681 0.014974 0.064 Uiso 1 1 calc R U . . . 
C26 C 0.58668(18) 0.8904(3) 0.08794(11) 0.0474(9) Uani 1 1 d D . . . . 
H26A H 0.629367 0.878595 0.086027 0.057 Uiso 0.816(9) 1 calc R U P B 1 
H26B H 0.583765 0.888314 0.111201 0.057 Uiso 0.816(9) 1 calc R U P B 1 
H26C H 0.628531 0.881898 0.084046 0.057 Uiso 0.184(9) 1 calc R U P B 2 
H26D H 0.587432 0.882513 0.111473 0.057 Uiso 0.184(9) 1 calc R U P B 2 
C27 C 0.56780(19) 1.0019(2) 0.07479(10) 0.043(2) Uani 0.816(9) 1 d DG U P B 1 
C28 C 0.51931(19) 1.0170(3) 0.04998(12) 0.0589(18) Uani 0.816(9) 1 d G U P B 1 
H28A H 0.497943 0.956335 0.040028 0.071 Uiso 0.816(9) 1 calc R U P B 1 
C29 C 0.50209(19) 1.1209(3) 0.03972(12) 0.065(2) Uani 0.816(9) 1 d G U P B 1 
H29A H 0.468953 1.131200 0.022766 0.078 Uiso 0.816(9) 1 calc R U P B 1 
C30 C 0.5334(2) 1.2096(2) 0.05428(12) 0.052(2) Uani 0.816(9) 1 d DG U P B 1 
C31 C 0.5819(2) 1.1945(3) 0.07910(11) 0.0534(15) Uani 0.816(9) 1 d G U P B 1 
H31A H 0.603223 1.255185 0.089047 0.064 Uiso 0.816(9) 1 calc R U P B 1 
C32 C 0.5991(2) 1.0906(3) 0.08935(10) 0.0541(15) Uani 0.816(9) 1 d G U P B 1 
H32A H 0.632213 1.080321 0.106309 0.065 Uiso 0.816(9) 1 calc R U P B 1 
O33 O 0.5105(3) 1.3089(4) 0.0435(2) 0.0631(19) Uani 0.816(9) 1 d D U P B 1 
C34 C 0.5447(4) 1.4020(7) 0.0522(3) 0.059(2) Uani 0.816(9) 1 d D U P B 1 
H34A H 0.522507 1.465561 0.042778 0.088 Uiso 0.816(9) 1 calc R U P B 1 
H34B H 0.552533 1.408845 0.075837 0.088 Uiso 0.816(9) 1 calc R U P B 1 
H34C H 0.583005 1.396754 0.044240 0.088 Uiso 0.816(9) 1 calc R U P B 1 
C27' C 0.5660(8) 1.0050(10) 0.0782(5) 0.033(7) Uiso 0.184(9) 1 d DG U P B 2 
C28' C 0.5055(7) 1.0298(12) 0.0688(6) 0.060(6) Uiso 0.184(9) 1 d G U P B 2 
H28B H 0.475858 0.975274 0.068778 0.072 Uiso 0.184(9) 1 calc R U P B 2 
C29' C 0.4883(6) 1.1345(14) 0.0594(6) 0.059(6) Uiso 0.184(9) 1 d G U P B 2 
H29B H 0.446968 1.151494 0.052951 0.070 Uiso 0.184(9) 1 calc R U P B 2 
C30' C 0.5317(9) 1.2144(10) 0.0594(5) 0.035(6) Uiso 0.184(9) 1 d DG U P B 2 
C31' C 0.5922(7) 1.1895(13) 0.0689(5) 0.042(6) Uiso 0.184(9) 1 d G U P B 2 
H31B H 0.621888 1.244121 0.068911 0.050 Uiso 0.184(9) 1 calc R U P B 2 
C32' C 0.6094(6) 1.0849(15) 0.0783(5) 0.041(6) Uiso 0.184(9) 1 d G U P B 2 
H32B H 0.650780 1.067902 0.084737 0.049 Uiso 0.184(9) 1 calc R U P B 2 
O33' O 0.5122(16) 1.3191(17) 0.0529(7) 0.052(7) Uiso 0.184(9) 1 d D U P B 2 
C34' C 0.5569(18) 1.399(4) 0.0584(12) 0.047(8) Uiso 0.184(9) 1 d D U P B 2 
H34D H 0.538702 1.470271 0.053080 0.070 Uiso 0.184(9) 1 calc R U P B 2 
H34E H 0.576037 1.398046 0.081135 0.070 Uiso 0.184(9) 1 calc R U P B 2 
H34F H 0.587305 1.385268 0.044696 0.070 Uiso 0.184(9) 1 calc R U P B 2 
C35 C 0.42678(15) 0.6236(3) 0.05590(8) 0.0323(7) Uani 1 1 d . . . . . 
O35 O 0.39618(11) 0.6321(2) 0.07768(6) 0.0352(5) Uani 1 1 d . . . . . 
O36 O 0.41214(12) 0.5514(2) 0.03223(6) 0.0422(6) Uani 1 1 d . . . . . 
C37 C 0.35757(19) 0.4877(4) 0.03341(10) 0.0500(10) Uani 1 1 d . . . . . 
H37A H 0.321467 0.534253 0.028661 0.060 Uiso 1 1 calc R U . . . 
H37B H 0.359096 0.455842 0.055167 0.060 Uiso 1 1 calc R U . . . 
C38 C 0.3549(2) 0.4012(4) 0.00890(12) 0.0616(12) Uani 1 1 d . . . . . 
H38A H 0.356727 0.433399 -0.012237 0.092 Uiso 1 1 calc R U . . . 
H38B H 0.317186 0.360953 0.007829 0.092 Uiso 1 1 calc R U . . . 
H38C H 0.389013 0.352008 0.014874 0.092 Uiso 1 1 calc R U . . . 
N41 N 0.37039(16) 1.0634(3) 0.20139(9) 0.0541(9) Uani 1 1 d . . . . . 
N42 N 0.34751(13) 1.0183(3) 0.17160(8) 0.0396(7) Uani 1 1 d . . . . . 
C43 C 0.38334(15) 0.9397(3) 0.16329(8) 0.0344(7) Uani 1 1 d . . . . . 
O43 O 0.37035(10) 0.8876(2) 0.13632(6) 0.0345(5) Uani 1 1 d . . . . . 
C44 C 0.43260(16) 0.9318(4) 0.18820(9) 0.0410(8) Uani 1 1 d . . . . . 
C45 C 0.42169(18) 1.0106(4) 0.21069(10) 0.0535(11) Uani 1 1 d . . . . . 
H45A H 0.448125 1.024425 0.230380 0.064 Uiso 1 1 calc R U . . . 
C46 C 0.28932(16) 1.0523(3) 0.15324(10) 0.0430(9) Uani 1 1 d . . . . . 
H46A H 0.289972 1.043809 0.129861 0.052 Uiso 1 1 calc R U . . . 
H46B H 0.282912 1.129827 0.157456 0.052 Uiso 1 1 calc R U . . . 
C47 C 0.23751(16) 0.9872(3) 0.16218(10) 0.0429(9) Uani 1 1 d . . . . . 
C48 C 0.23115(17) 0.8779(3) 0.15438(11) 0.0461(9) Uani 1 1 d . . . . . 
H48A H 0.259788 0.844059 0.143445 0.055 Uiso 1 1 calc R U . . . 
C49 C 0.18388(17) 0.8175(3) 0.16225(11) 0.0486(10) Uani 1 1 d . . . . . 
H49A H 0.180536 0.742861 0.156985 0.058 Uiso 1 1 calc R U . . . 
C50 C 0.14150(17) 0.8667(3) 0.17785(11) 0.0483(10) Uani 1 1 d . . . . . 
C51 C 0.1469(2) 0.9755(4) 0.18541(14) 0.0653(14) Uani 1 1 d . . . . . 
H51A H 0.117809 1.010036 0.195845 0.078 Uiso 1 1 calc R U . . . 
C52 C 0.1950(2) 1.0336(4) 0.17768(13) 0.0594(12) Uani 1 1 d . . . . . 
H52A H 0.198687 1.108002 0.183280 0.071 Uiso 1 1 calc R U . . . 
O53 O 0.09596(13) 0.8009(3) 0.18444(9) 0.0615(9) Uani 1 1 d . . . . . 
C54 C 0.0493(2) 0.8497(4) 0.19864(17) 0.0792(18) Uani 1 1 d . . . . . 
H54A H 0.029257 0.905503 0.184113 0.119 Uiso 1 1 calc R U . . . 
H54B H 0.066708 0.882615 0.219347 0.119 Uiso 1 1 calc R U . . . 
H54C H 0.019956 0.794539 0.202218 0.119 Uiso 1 1 calc R U . . . 
C55 C 0.47766(15) 0.8532(4) 0.18684(8) 0.0404(9) Uani 1 1 d . . . . . 
O55 O 0.47434(11) 0.7836(2) 0.16540(5) 0.0385(6) Uani 1 1 d . . . . . 
O56 O 0.52562(12) 0.8569(3) 0.21029(7) 0.0634(10) Uani 1 1 d D . . . . 
C57 C 0.5654(4) 0.7531(9) 0.20842(19) 0.048(2) Uani 0.513(9) 1 d D U P C 1 
H57A H 0.541323 0.686584 0.209216 0.057 Uiso 0.513(9) 1 calc R U P C 1 
H57B H 0.582733 0.752779 0.188254 0.057 Uiso 0.513(9) 1 calc R U P C 1 
C58 C 0.6139(4) 0.7604(7) 0.2373(2) 0.055(2) Uani 0.513(9) 1 d D U P C 1 
H58A H 0.640691 0.697896 0.237718 0.083 Uiso 0.513(9) 1 calc R U P C 1 
H58B H 0.636965 0.826969 0.236085 0.083 Uiso 0.513(9) 1 calc R U P C 1 
H58C H 0.595818 0.761193 0.256914 0.083 Uiso 0.513(9) 1 calc R U P C 1 
C57' C 0.5778(4) 0.7943(8) 0.2118(3) 0.045(3) Uiso 0.487(9) 1 d D U P C 2 
H57C H 0.613566 0.833159 0.223255 0.054 Uiso 0.487(9) 1 calc R U P C 2 
H57D H 0.584861 0.773890 0.189979 0.054 Uiso 0.487(9) 1 calc R U P C 2 
C58' C 0.5635(4) 0.6969(7) 0.2306(2) 0.051(2) Uiso 0.487(9) 1 d D U P C 2 
H58D H 0.597597 0.646632 0.233224 0.076 Uiso 0.487(9) 1 calc R U P C 2 
H58E H 0.556079 0.719687 0.251971 0.076 Uiso 0.487(9) 1 calc R U P C 2 
H58F H 0.527613 0.660912 0.218973 0.076 Uiso 0.487(9) 1 calc R U P C 2 
N61 N 0.49445(17) 0.4147(3) 0.19983(9) 0.0532(9) Uani 1 1 d . . . . . 
N62 N 0.49352(15) 0.4584(3) 0.16941(8) 0.0442(8) Uani 1 1 d . . . . . 
C63 C 0.45338(16) 0.5398(3) 0.16300(8) 0.0359(7) Uani 1 1 d . . . . . 
O63 O 0.44503(11) 0.5915(2) 0.13579(6) 0.0389(6) Uani 1 1 d . . . . . 
C64 C 0.42507(16) 0.5483(3) 0.19024(9) 0.0376(8) Uani 1 1 d . . . . . 
C65 C 0.45278(19) 0.4687(4) 0.21162(10) 0.0487(10) Uani 1 1 d . . . . . 
H65A H 0.442540 0.455344 0.232312 0.058 Uiso 1 1 calc R U . . . 
C66 C 0.5382(2) 0.4281(4) 0.14933(12) 0.0560(11) Uani 1 1 d . . . . . 
H66A H 0.520363 0.436216 0.126253 0.067 Uiso 1 1 calc R U . . . 
H66B H 0.549304 0.351189 0.153201 0.067 Uiso 1 1 calc R U . . . 
C67 C 0.5938(2) 0.4966(4) 0.15664(12) 0.0551(11) Uani 1 1 d . . . . . 
C68 C 0.6003(2) 0.5901(4) 0.13905(13) 0.0638(14) Uani 1 1 d . . . . . 
H68A H 0.569659 0.609506 0.121582 0.077 Uiso 1 1 calc R U . . . 
C69 C 0.6503(2) 0.6549(4) 0.14653(14) 0.0667(15) Uani 1 1 d . . . . . 
H69A H 0.654015 0.717936 0.134110 0.080 Uiso 1 1 calc R U . . . 
C70 C 0.6949(2) 0.6286(4) 0.17199(15) 0.0696(15) Uani 1 1 d . . . . . 
C71 C 0.6899(2) 0.5347(4) 0.18971(15) 0.0730(15) Uani 1 1 d . . . . . 
H71A H 0.720867 0.514916 0.206963 0.088 Uiso 1 1 calc R U . . . 
C72 C 0.6390(2) 0.4705(4) 0.18180(14) 0.0656(14) Uani 1 1 d . . . . . 
H72A H 0.635239 0.407124 0.194061 0.079 Uiso 1 1 calc R U . . . 
O73 O 0.74230(17) 0.6986(3) 0.17782(12) 0.0863(13) Uani 1 1 d . . . . . 
C74 C 0.7909(3) 0.6724(5) 0.2028(2) 0.108(3) Uani 1 1 d . . . . . 
H74A H 0.808656 0.603363 0.197884 0.162 Uiso 1 1 calc R U . . . 
H74B H 0.776145 0.666491 0.223415 0.162 Uiso 1 1 calc R U . . . 
H74C H 0.821545 0.729277 0.204435 0.162 Uiso 1 1 calc R U . . . 
C75 C 0.38031(16) 0.6277(3) 0.19148(8) 0.0387(8) Uani 1 1 d . . . . . 
O75 O 0.36593(11) 0.6980(2) 0.17075(6) 0.0406(6) Uani 1 1 d . . . . . 
O76 O 0.35323(13) 0.6199(3) 0.21779(6) 0.0519(7) Uani 1 1 d . . . . . 
C77 C 0.3056(2) 0.6958(5) 0.22047(12) 0.0715(15) Uani 1 1 d . . . . . 
H77A H 0.277868 0.663418 0.233736 0.086 Uiso 1 1 calc R U . . . 
H77B H 0.282472 0.710256 0.198690 0.086 Uiso 1 1 calc R U . . . 
C78 C 0.3290(3) 0.7974(5) 0.23509(16) 0.0857(18) Uani 1 1 d . . . . . 
H78A H 0.355540 0.830777 0.221665 0.129 Uiso 1 1 calc R U . . . 
H78B H 0.351647 0.783477 0.256729 0.129 Uiso 1 1 calc R U . . . 
H78C H 0.295405 0.846304 0.236691 0.129 Uiso 1 1 calc R U . . . 
  
  
_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 
Zr1 O43 2.093(2) . ? 
Zr1 O3 2.100(2) . ? 
Zr1 O63 2.103(2) . ? 
Zr1 O23 2.107(2) . ? 
Zr1 O35 2.273(2) . ? 
Zr1 O55 2.305(2) . ? 
Zr1 O15 2.312(2) . ? 
Zr1 O75 2.365(2) . ? 
N1 C5 1.321(5) . ? 
N1 N2 1.394(4) . ? 
N2 C3 1.339(5) . ? 
N2 C6 1.456(5) . ? 
C3 O3 1.303(4) . ? 
C3 C4 1.400(5) . ? 
C4 C5 1.412(5) . ? 
C4 C15 1.424(5) . ? 
C6 C7 1.511(6) . ? 
C7 C12 1.381(6) . ? 
C7 C8 1.394(6) . ? 
C8 C9 1.380(7) . ? 
C9 C10 1.383(7) . ? 
C10 O13 1.368(6) . ? 
C10 C11 1.376(7) . ? 
C11 C12 1.393(7) . ? 
O13 C14 1.441(8) . ? 
C15 O15 1.243(4) . ? 
C15 O16 1.333(4) . ? 
O16 C17' 1.464(18) . ? 
O16 C17 1.468(5) . ? 
C17 C18 1.502(8) . ? 
C17' C18' 1.51(2) . ? 
N21 C25 1.315(6) . ? 
N21 N22 1.389(5) . ? 
N22 C23 1.354(5) . ? 
N22 C26 1.434(5) . ? 
C23 O23 1.288(4) . ? 
C23 C24 1.398(5) . ? 
C24 C35 1.419(5) . ? 
C24 C25 1.422(5) . ? 
C26 C27 1.520(5) . ? 
C26 C27' 1.526(11) . ? 
C27 C28 1.3900 . ? 
C27 C32 1.3900 . ? 
C28 C29 1.3900 . ? 
C29 C30 1.3900 . ? 
C30 O33 1.378(5) . ? 
C30 C31 1.3900 . ? 
C31 C32 1.3900 . ? 
O33 C34 1.400(7) . ? 
C27' C28' 1.3900 . ? 
C27' C32' 1.3900 . ? 
C28' C29' 1.3900 . ? 
C29' C30' 1.3900 . ? 
C30' O33' 1.381(17) . ? 
C30' C31' 1.3900 . ? 
C31' C32' 1.3900 . ? 
O33' C34' 1.405(18) . ? 
C35 O35 1.239(4) . ? 
C35 O36 1.336(4) . ? 
O36 C37 1.469(5) . ? 
C37 C38 1.478(6) . ? 
N41 C45 1.329(6) . ? 
N41 N42 1.388(4) . ? 
N42 C43 1.347(5) . ? 
N42 C46 1.467(5) . ? 
C43 O43 1.293(4) . ? 
C43 C44 1.395(5) . ? 
C44 C45 1.407(6) . ? 
C44 C55 1.415(6) . ? 
C46 C47 1.517(6) . ? 
C47 C52 1.372(6) . ? 
C47 C48 1.393(6) . ? 
C48 C49 1.386(6) . ? 
C49 C50 1.387(6) . ? 
C50 O53 1.374(5) . ? 
C50 C51 1.384(6) . ? 
C51 C52 1.385(6) . ? 
O53 C54 1.427(6) . ? 
C55 O55 1.239(5) . ? 
C55 O56 1.335(4) . ? 
O56 C57' 1.401(10) . ? 
O56 C57 1.577(9) . ? 
C57 C58 1.490(9) . ? 
C57' C58' 1.506(11) . ? 
N61 C65 1.316(6) . ? 
N61 N62 1.384(5) . ? 
N62 C63 1.350(5) . ? 
N62 C66 1.468(5) . ? 
C63 O63 1.296(4) . ? 
C63 C64 1.404(5) . ? 
C64 C65 1.407(5) . ? 
C64 C75 1.415(6) . ? 
C66 C67 1.501(7) . ? 
C67 C72 1.377(7) . ? 
C67 C68 1.394(6) . ? 
C68 C69 1.375(8) . ? 
C69 C70 1.379(8) . ? 
C70 O73 1.365(7) . ? 
C70 C71 1.394(7) . ? 
C71 C72 1.390(7) . ? 
O73 C74 1.422(8) . ? 
C75 O75 1.235(5) . ? 
C75 O76 1.353(4) . ? 
O76 C77 1.445(6) . ? 
C77 C78 1.459(8) . ? 
  
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 
O43 Zr1 O3 90.36(10) . . ? 
O43 Zr1 O63 148.07(9) . . ? 
O3 Zr1 O63 98.12(10) . . ? 
O43 Zr1 O23 99.35(10) . . ? 
O3 Zr1 O23 148.78(9) . . ? 
O63 Zr1 O23 89.18(10) . . ? 
O43 Zr1 O35 140.45(9) . . ? 
O3 Zr1 O35 74.31(9) . . ? 
O63 Zr1 O35 71.25(9) . . ? 
O23 Zr1 O35 79.54(9) . . ? 
O43 Zr1 O55 77.95(9) . . ? 
O3 Zr1 O55 139.83(9) . . ? 
O63 Zr1 O55 75.78(10) . . ? 
O23 Zr1 O55 71.39(9) . . ? 
O35 Zr1 O55 135.87(9) . . ? 
O43 Zr1 O15 70.76(9) . . ? 
O3 Zr1 O15 79.59(9) . . ? 
O63 Zr1 O15 141.00(9) . . ? 
O23 Zr1 O15 75.86(9) . . ? 
O35 Zr1 O15 70.70(9) . . ? 
O55 Zr1 O15 129.60(9) . . ? 
O43 Zr1 O75 76.44(10) . . ? 
O3 Zr1 O75 69.06(9) . . ? 
O63 Zr1 O75 78.03(9) . . ? 
O23 Zr1 O75 142.04(9) . . ? 
O35 Zr1 O75 127.47(9) . . ? 
O55 Zr1 O75 70.85(9) . . ? 
O15 Zr1 O75 133.95(9) . . ? 
C5 N1 N2 104.3(3) . . ? 
C3 N2 N1 111.8(3) . . ? 
C3 N2 C6 127.3(3) . . ? 
N1 N2 C6 120.8(3) . . ? 
O3 C3 N2 122.3(3) . . ? 
O3 C3 C4 130.4(3) . . ? 
N2 C3 C4 107.3(3) . . ? 
C3 O3 Zr1 128.1(2) . . ? 
C3 C4 C5 104.1(3) . . ? 
C3 C4 C15 121.7(3) . . ? 
C5 C4 C15 133.9(3) . . ? 
N1 C5 C4 112.5(3) . . ? 
N2 C6 C7 113.8(3) . . ? 
C12 C7 C8 118.0(4) . . ? 
C12 C7 C6 121.0(4) . . ? 
C8 C7 C6 121.0(4) . . ? 
C9 C8 C7 120.5(4) . . ? 
C8 C9 C10 121.0(5) . . ? 
O13 C10 C11 125.6(5) . . ? 
O13 C10 C9 115.4(5) . . ? 
C11 C10 C9 119.1(5) . . ? 
C10 C11 C12 120.0(4) . . ? 
C7 C12 C11 121.4(5) . . ? 
C10 O13 C14 117.3(5) . . ? 
O15 C15 O16 121.1(3) . . ? 
O15 C15 C4 123.5(3) . . ? 
O16 C15 C4 115.3(3) . . ? 
C15 O15 Zr1 131.6(2) . . ? 
C15 O16 C17' 118.3(18) . . ? 
C15 O16 C17 116.6(3) . . ? 
O16 C17 C18 107.3(5) . . ? 
O16 C17' C18' 106.3(18) . . ? 
C25 N21 N22 104.7(3) . . ? 
C23 N22 N21 111.9(3) . . ? 
C23 N22 C26 127.4(3) . . ? 
N21 N22 C26 120.3(3) . . ? 
O23 C23 N22 122.3(3) . . ? 
O23 C23 C24 131.0(3) . . ? 
N22 C23 C24 106.6(3) . . ? 
C23 O23 Zr1 130.6(2) . . ? 
C23 C24 C35 121.8(3) . . ? 
C23 C24 C25 104.4(3) . . ? 
C35 C24 C25 133.7(4) . . ? 
N21 C25 C24 112.3(4) . . ? 
N22 C26 C27 114.0(3) . . ? 
N22 C26 C27' 116.6(8) . . ? 
C28 C27 C32 120.0 . . ? 
C28 C27 C26 122.1(3) . . ? 
C32 C27 C26 117.8(3) . . ? 
C29 C28 C27 120.0 . . ? 
C28 C29 C30 120.0 . . ? 
O33 C30 C31 124.7(4) . . ? 
O33 C30 C29 115.2(4) . . ? 
C31 C30 C29 120.0 . . ? 
C30 C31 C32 120.0 . . ? 
C31 C32 C27 120.0 . . ? 
C30 O33 C34 119.3(6) . . ? 
C28' C27' C32' 120.0 . . ? 
C28' C27' C26 121.5(12) . . ? 
C32' C27' C26 118.5(12) . . ? 
C29' C28' C27' 120.0 . . ? 
C28' C29' C30' 120.0 . . ? 
O33' C30' C29' 117.8(19) . . ? 
O33' C30' C31' 121.9(19) . . ? 
C29' C30' C31' 120.0 . . ? 
C32' C31' C30' 120.0 . . ? 
C31' C32' C27' 120.0 . . ? 
C30' O33' C34' 116(3) . . ? 
O35 C35 O36 120.5(3) . . ? 
O35 C35 C24 122.7(3) . . ? 
O36 C35 C24 116.9(3) . . ? 
C35 O35 Zr1 134.3(2) . . ? 
C35 O36 C37 115.9(3) . . ? 
O36 C37 C38 107.5(3) . . ? 
C45 N41 N42 103.8(3) . . ? 
C43 N42 N41 112.1(3) . . ? 
C43 N42 C46 126.4(3) . . ? 
N41 N42 C46 121.4(3) . . ? 
O43 C43 N42 122.0(3) . . ? 
O43 C43 C44 131.0(3) . . ? 
N42 C43 C44 107.0(3) . . ? 
C43 O43 Zr1 130.6(2) . . ? 
C43 C44 C45 104.3(3) . . ? 
C43 C44 C55 120.3(3) . . ? 
C45 C44 C55 135.3(3) . . ? 
N41 C45 C44 112.7(3) . . ? 
N42 C46 C47 112.0(3) . . ? 
C52 C47 C48 117.8(4) . . ? 
C52 C47 C46 121.5(4) . . ? 
C48 C47 C46 120.7(4) . . ? 
C49 C48 C47 121.3(4) . . ? 
C48 C49 C50 119.7(4) . . ? 
O53 C50 C51 124.7(4) . . ? 
O53 C50 C49 115.7(4) . . ? 
C51 C50 C49 119.6(4) . . ? 
C50 C51 C52 119.6(4) . . ? 
C47 C52 C51 122.0(4) . . ? 
C50 O53 C54 117.5(4) . . ? 
O55 C55 O56 120.1(4) . . ? 
O55 C55 C44 123.5(3) . . ? 
O56 C55 C44 116.4(4) . . ? 
C55 O55 Zr1 133.5(2) . . ? 
C55 O56 C57' 125.8(6) . . ? 
C55 O56 C57 109.4(4) . . ? 
C58 C57 O56 104.8(7) . . ? 
O56 C57' C58' 102.4(7) . . ? 
C65 N61 N62 104.3(3) . . ? 
C63 N62 N61 112.4(3) . . ? 
C63 N62 C66 125.4(3) . . ? 
N61 N62 C66 121.6(3) . . ? 
O63 C63 N62 122.5(3) . . ? 
O63 C63 C64 131.5(3) . . ? 
N62 C63 C64 106.0(3) . . ? 
C63 O63 Zr1 131.3(2) . . ? 
C63 C64 C65 104.7(3) . . ? 
C63 C64 C75 120.5(3) . . ? 
C65 C64 C75 134.9(4) . . ? 
N61 C65 C64 112.6(4) . . ? 
N62 C66 C67 111.6(4) . . ? 
C72 C67 C68 118.1(5) . . ? 
C72 C67 C66 120.6(4) . . ? 
C68 C67 C66 121.3(4) . . ? 
C69 C68 C67 121.2(5) . . ? 
C68 C69 C70 120.2(4) . . ? 
O73 C70 C69 115.9(4) . . ? 
O73 C70 C71 124.4(5) . . ? 
C69 C70 C71 119.7(5) . . ? 
C72 C71 C70 119.2(5) . . ? 
C67 C72 C71 121.6(4) . . ? 
C70 O73 C74 118.1(4) . . ? 
O75 C75 O76 121.6(4) . . ? 
O75 C75 C64 124.6(3) . . ? 
O76 C75 C64 113.8(3) . . ? 
C75 O75 Zr1 132.1(2) . . ? 
C75 O76 C77 117.4(3) . . ? 
O76 C77 C78 111.9(4) . . ? 
  
_refine_diff_density_max    0.745 
_refine_diff_density_min   -1.239 
_refine_diff_density_rms    0.068 
  
  
  
#===END

