#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/94/4339447.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4339447
loop_
_publ_author_name
'Cohen, Ad'
'Yeori, Adi'
'Goldberg, Israel'
'Kol, Moshe'
_publ_section_title
;
 Group 4 complexes of a new [OSSO]-type dianionic ligand. Coordination
 chemistry and preliminary polymerization catalysis studies.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8114
_journal_page_last               8116
_journal_paper_doi               10.1021/ic701370t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C40 H66 O4 S2 Zr, C2.5 H5.5'
_chemical_formula_sum            'C42.5 H71.5 O4 S2 Zr'
_chemical_formula_weight         801.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.0593(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0206(2)
_cell_length_b                   17.7528(2)
_cell_length_c                   19.5067(4)
_cell_measurement_reflns_used    10275
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      1.41
_cell_volume                     4502.59(13)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40493
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1722
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         10709
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0717P)²+0.7764P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                7745
_reflns_number_total             10709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701370t-file003.cif
_cod_data_source_block           mk176
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C42.50 H71.50 O4 S2 Zr'
_cod_database_code               4339447
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.384696(18) 0.100454(12) 0.273130(12) 0.01964(8) Uani 1 1 d . . .
S2 S 0.35355(5) 0.01339(3) 0.39291(4) 0.02688(16) Uani 1 1 d . . .
S3 S 0.28355(5) -0.03273(3) 0.22735(4) 0.02884(16) Uani 1 1 d . . .
O4 O 0.23516(13) 0.12401(9) 0.28788(9) 0.0226(4) Uani 1 1 d . . .
O5 O 0.44794(13) 0.17777(9) 0.33079(9) 0.0256(4) Uani 1 1 d . . .
O6 O 0.50557(14) 0.02799(9) 0.27411(9) 0.0232(4) Uani 1 1 d . . .
O7 O 0.38853(14) 0.13760(10) 0.18048(9) 0.0269(4) Uani 1 1 d . . .
C8 C 0.2749(2) -0.06793(15) 0.36954(16) 0.0338(7) Uani 1 1 d . . .
H8A H 0.2927 -0.1088 0.4026 0.041 Uiso 1 1 calc R . .
H8B H 0.2021 -0.0544 0.3753 0.041 Uiso 1 1 calc R . .
C9 C 0.2830(2) -0.09945(13) 0.29724(16) 0.0332(7) Uani 1 1 d . . .
H9A H 0.2247 -0.1345 0.2880 0.040 Uiso 1 1 calc R . .
H9B H 0.3469 -0.1296 0.2967 0.040 Uiso 1 1 calc R . .
C10 C 0.1510(2) -0.00027(15) 0.21667(15) 0.0304(6) Uani 1 1 d . . .
H10A H 0.1475 0.0383 0.1800 0.036 Uiso 1 1 calc R . .
H10B H 0.1081 -0.0433 0.2002 0.036 Uiso 1 1 calc R . .
C11 C 0.4824(2) -0.02529(14) 0.40811(14) 0.0264(6) Uani 1 1 d . . .
H11A H 0.5307 0.0172 0.4164 0.032 Uiso 1 1 calc R . .
H11B H 0.4833 -0.0555 0.4508 0.032 Uiso 1 1 calc R . .
C12 C 0.52284(19) -0.07380(14) 0.35213(13) 0.0221(5) Uani 1 1 d . . .
C13 C 0.5466(2) -0.14866(13) 0.36633(13) 0.0233(5) Uani 1 1 d . . .
H13 H 0.5350 -0.1685 0.4105 0.028 Uiso 1 1 calc R . .
C14 C 0.5869(2) -0.19511(13) 0.31718(14) 0.0248(5) Uani 1 1 d . A .
C15 C 0.60685(19) -0.16211(13) 0.25448(13) 0.0229(5) Uani 1 1 d . . .
H15 H 0.6375 -0.1927 0.2212 0.027 Uiso 1 1 calc R . .
C16 C 0.58496(19) -0.08724(13) 0.23716(13) 0.0212(5) Uani 1 1 d . . .
C17 C 0.53744(19) -0.04311(13) 0.28707(13) 0.0202(5) Uani 1 1 d . . .
C18 C 0.1032(2) 0.03241(13) 0.27854(14) 0.0251(6) Uani 1 1 d . . .
C19 C 0.0141(2) -0.00015(14) 0.30241(15) 0.0271(6) Uani 1 1 d . . .
H19 H -0.0127 -0.0445 0.2810 0.032 Uiso 1 1 calc R . .
C20 C -0.0358(2) 0.03092(14) 0.35670(14) 0.0255(6) Uani 1 1 d . . .
C21 C 0.0058(2) 0.09668(13) 0.38560(14) 0.0243(5) Uani 1 1 d . . .
H21 H -0.0283 0.1191 0.4223 0.029 Uiso 1 1 calc R . .
C22 C 0.09515(19) 0.13197(13) 0.36385(13) 0.0221(5) Uani 1 1 d . . .
C23 C 0.14607(19) 0.09679(12) 0.31047(13) 0.0214(5) Uani 1 1 d . . .
C24 C 0.6116(2) -0.27827(14) 0.33396(14) 0.0319(6) Uani 1 1 d D . .
C25 C 0.6313(3) -0.32429(15) 0.27051(16) 0.0402(7) Uani 1 1 d . A .
H25A H 0.6923 -0.3047 0.2491 0.060 Uiso 1 1 calc R . .
H25B H 0.5716 -0.3209 0.2379 0.060 Uiso 1 1 calc R . .
H25C H 0.6429 -0.3771 0.2836 0.060 Uiso 1 1 calc R . .
C26A C 0.7212(5) -0.2773(4) 0.3669(5) 0.051(2) Uiso 0.538(16) 1 d PD A 1
H26A H 0.7145 -0.2483 0.4092 0.076 Uiso 0.538(16) 1 d PR A 1
H26B H 0.7750 -0.2549 0.3401 0.076 Uiso 0.538(16) 1 d PR A 1
H26C H 0.7397 -0.3295 0.3785 0.076 Uiso 0.538(16) 1 d PR A 1
C26B C 0.6879(5) -0.2861(3) 0.3928(3) 0.025(2) Uiso 0.462(16) 1 d PD A 2
H26D H 0.6607 -0.2605 0.4325 0.038 Uiso 0.462(16) 1 d PR A 2
H26E H 0.7545 -0.2641 0.3828 0.038 Uiso 0.462(16) 1 d PR A 2
H26F H 0.6967 -0.3398 0.4032 0.038 Uiso 0.462(16) 1 d PR A 2
C27A C 0.5126(3) -0.3158(2) 0.3572(3) 0.0380(14) Uiso 0.677(10) 1 d PD A 1
H27A H 0.5273 -0.3684 0.3694 0.057 Uiso 0.677(10) 1 d PR A 1
H27B H 0.4582 -0.3139 0.3205 0.057 Uiso 0.677(10) 1 d PR A 1
H27C H 0.4898 -0.2890 0.3976 0.057 Uiso 0.677(10) 1 d PR A 1
C27B C 0.5602(8) -0.3102(5) 0.3942(4) 0.038(3) Uiso 0.323(10) 1 d PD A 2
H27D H 0.5810 -0.3628 0.4015 0.058 Uiso 0.323(10) 1 d PR A 2
H27E H 0.4850 -0.3071 0.3897 0.058 Uiso 0.323(10) 1 d PR A 2
H27F H 0.5857 -0.2797 0.4333 0.058 Uiso 0.323(10) 1 d PR A 2
C28 C 0.6106(2) -0.05521(13) 0.16686(13) 0.0236(5) Uani 1 1 d . . .
C29 C 0.6794(2) -0.10924(14) 0.12820(15) 0.0304(6) Uani 1 1 d . . .
H29A H 0.7425 -0.1193 0.1563 0.046 Uiso 1 1 calc R . .
H29B H 0.6969 -0.0862 0.0847 0.046 Uiso 1 1 calc R . .
H29C H 0.6425 -0.1566 0.1190 0.046 Uiso 1 1 calc R . .
C30 C 0.5115(2) -0.04241(15) 0.12224(14) 0.0296(6) Uani 1 1 d . . .
H30A H 0.4726 -0.0896 0.1184 0.044 Uiso 1 1 calc R . .
H30B H 0.5290 -0.0257 0.0764 0.044 Uiso 1 1 calc R . .
H30C H 0.4697 -0.0038 0.1434 0.044 Uiso 1 1 calc R . .
C31 C 0.6712(2) 0.01927(14) 0.17513(15) 0.0322(6) Uani 1 1 d . . .
H31A H 0.6306 0.0558 0.1999 0.048 Uiso 1 1 calc R . .
H31B H 0.6847 0.0394 0.1297 0.048 Uiso 1 1 calc R . .
H31C H 0.7365 0.0099 0.2010 0.048 Uiso 1 1 calc R . .
C32 C -0.1360(2) -0.00258(16) 0.38316(16) 0.0325(6) Uani 1 1 d . . .
C33 C -0.1665(2) -0.07698(17) 0.3471(2) 0.0488(9) Uani 1 1 d . . .
H33A H -0.2310 -0.0955 0.3646 0.073 Uiso 1 1 calc R . .
H33B H -0.1121 -0.1144 0.3562 0.073 Uiso 1 1 calc R . .
H33C H -0.1757 -0.0684 0.2975 0.073 Uiso 1 1 calc R . .
C34 C -0.1252(3) -0.0169(2) 0.45991(19) 0.0603(11) Uani 1 1 d . . .
H34A H -0.1069 0.0302 0.4838 0.090 Uiso 1 1 calc R . .
H34B H -0.0711 -0.0544 0.4697 0.090 Uiso 1 1 calc R . .
H34C H -0.1905 -0.0357 0.4759 0.090 Uiso 1 1 calc R . .
C35 C -0.2244(2) 0.05329(17) 0.36856(18) 0.0413(7) Uani 1 1 d . . .
H35A H -0.2077 0.1013 0.3913 0.062 Uiso 1 1 calc R . .
H35B H -0.2878 0.0329 0.3861 0.062 Uiso 1 1 calc R . .
H35C H -0.2340 0.0613 0.3189 0.062 Uiso 1 1 calc R . .
C36 C 0.1332(2) 0.20697(13) 0.39588(14) 0.0244(6) Uani 1 1 d . . .
C37 C 0.2385(2) 0.19648(14) 0.43456(14) 0.0281(6) Uani 1 1 d . . .
H37A H 0.2328 0.1580 0.4702 0.042 Uiso 1 1 calc R . .
H37B H 0.2603 0.2443 0.4558 0.042 Uiso 1 1 calc R . .
H37C H 0.2893 0.1805 0.4022 0.042 Uiso 1 1 calc R . .
C38 C 0.1432(2) 0.26613(13) 0.33880(15) 0.0291(6) Uani 1 1 d . . .
H38A H 0.1932 0.2487 0.3065 0.044 Uiso 1 1 calc R . .
H38B H 0.1666 0.3140 0.3592 0.044 Uiso 1 1 calc R . .
H38C H 0.0762 0.2734 0.3143 0.044 Uiso 1 1 calc R . .
C39 C 0.0592(2) 0.23839(15) 0.44714(16) 0.0347(7) Uani 1 1 d . . .
H39A H -0.0092 0.2446 0.4244 0.052 Uiso 1 1 calc R . .
H39B H 0.0844 0.2873 0.4642 0.052 Uiso 1 1 calc R . .
H39C H 0.0550 0.2034 0.4857 0.052 Uiso 1 1 calc R . .
C40 C 0.5203(2) 0.23030(14) 0.35911(15) 0.0292(6) Uani 1 1 d . . .
C41 C 0.5428(3) 0.2105(2) 0.43407(17) 0.0502(9) Uani 1 1 d . . .
H41A H 0.4782 0.2088 0.4576 0.075 Uiso 1 1 calc R . .
H41B H 0.5882 0.2488 0.4556 0.075 Uiso 1 1 calc R . .
H41C H 0.5765 0.1612 0.4374 0.075 Uiso 1 1 calc R . .
C42 C 0.4719(3) 0.30874(15) 0.35182(19) 0.0472(8) Uani 1 1 d . . .
H42A H 0.4547 0.3192 0.3032 0.071 Uiso 1 1 calc R . .
H42B H 0.5208 0.3466 0.3701 0.071 Uiso 1 1 calc R . .
H42C H 0.4092 0.3106 0.3774 0.071 Uiso 1 1 calc R . .
C43 C 0.6165(2) 0.22546(18) 0.31843(19) 0.0451(8) Uani 1 1 d . . .
H43A H 0.6421 0.1735 0.3193 0.068 Uiso 1 1 calc R . .
H43B H 0.6694 0.2590 0.3390 0.068 Uiso 1 1 calc R . .
H43C H 0.5999 0.2407 0.2708 0.068 Uiso 1 1 calc R . .
C44 C 0.3734(2) 0.18369(14) 0.12184(14) 0.0279(6) Uani 1 1 d . . .
C45 C 0.2591(3) 0.20233(18) 0.11239(19) 0.0478(8) Uani 1 1 d . . .
H45A H 0.2197 0.1556 0.1058 0.072 Uiso 1 1 calc R . .
H45B H 0.2474 0.2347 0.0721 0.072 Uiso 1 1 calc R . .
H45C H 0.2369 0.2286 0.1532 0.072 Uiso 1 1 calc R . .
C46 C 0.4375(3) 0.25526(16) 0.13261(17) 0.0422(8) Uani 1 1 d . . .
H46A H 0.4155 0.2820 0.1733 0.063 Uiso 1 1 calc R . .
H46B H 0.4276 0.2879 0.0922 0.063 Uiso 1 1 calc R . .
H46C H 0.5104 0.2418 0.1392 0.063 Uiso 1 1 calc R . .
C47 C 0.4094(3) 0.14080(17) 0.05976(16) 0.0442(8) Uani 1 1 d . . .
H47A H 0.4825 0.1284 0.0671 0.066 Uiso 1 1 calc R . .
H47B H 0.3993 0.1722 0.0186 0.066 Uiso 1 1 calc R . .
H47C H 0.3694 0.0943 0.0537 0.066 Uiso 1 1 calc R . .
C48 C 0.4571(3) 0.4773(2) 0.48267(19) 0.0582(10) Uani 1 1 d . . .
H48A H 0.4579 0.4857 0.4325 0.070 Uiso 1 1 calc R . .
H48B H 0.4713 0.4232 0.4912 0.070 Uiso 1 1 calc R . .
C49 C 0.3514(4) 0.4945(3) 0.5050(3) 0.0773(14) Uani 1 1 d . . .
H49A H 0.3347 0.5475 0.4932 0.093 Uiso 1 1 calc R . .
H49B H 0.3515 0.4897 0.5556 0.093 Uiso 1 1 calc R . .
C50 C 0.2684(6) 0.4446(4) 0.4734(4) 0.0557(19) Uani 0.50 1 d P . .
H50A H 0.2667 0.4496 0.4233 0.084 Uiso 0.50 1 calc PR . .
H50B H 0.2018 0.4596 0.4901 0.084 Uiso 0.50 1 calc PR . .
H50C H 0.2828 0.3921 0.4862 0.084 Uiso 0.50 1 calc PR . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O7 Zr1 O5 105.75(8) . .
O7 Zr1 O4 97.80(7) . .
O5 Zr1 O4 98.84(7) . .
O7 Zr1 O6 99.59(7) . .
O5 Zr1 O6 97.96(7) . .
O4 Zr1 O6 151.48(7) . .
O7 Zr1 S3 91.42(6) . .
O5 Zr1 S3 162.80(6) . .
O4 Zr1 S3 77.45(5) . .
O6 Zr1 S3 79.69(5) . .
O7 Zr1 S2 165.23(6) . .
O5 Zr1 S2 89.02(6) . .
O4 Zr1 S2 79.38(5) . .
O6 Zr1 S2 78.04(5) . .
S3 Zr1 S2 73.80(2) . .
C8 S2 C11 104.11(12) . .
C8 S2 Zr1 109.20(10) . .
C11 S2 Zr1 99.65(9) . .
C9 S3 C10 104.58(13) . .
C9 S3 Zr1 109.30(9) . .
C10 S3 Zr1 101.19(8) . .
C23 O4 Zr1 145.07(15) . .
C40 O5 Zr1 161.64(17) . .
C17 O6 Zr1 145.57(15) . .
C44 O7 Zr1 161.61(16) . .
C9 C8 S2 117.25(18) . .
C9 C8 H8A 108.0 . .
S2 C8 H8A 108.0 . .
C9 C8 H8B 108.0 . .
S2 C8 H8B 108.0 . .
H8A C8 H8B 107.2 . .
C8 C9 S3 117.41(17) . .
C8 C9 H9A 107.9 . .
S3 C9 H9A 107.9 . .
C8 C9 H9B 107.9 . .
S3 C9 H9B 107.9 . .
H9A C9 H9B 107.2 . .
C18 C10 S3 117.4(2) . .
C18 C10 H10A 107.9 . .
S3 C10 H10A 107.9 . .
C18 C10 H10B 107.9 . .
S3 C10 H10B 107.9 . .
H10A C10 H10B 107.2 . .
C12 C11 S2 116.83(19) . .
C12 C11 H11A 108.1 . .
S2 C11 H11A 108.1 . .
C12 C11 H11B 108.1 . .
S2 C11 H11B 108.1 . .
H11A C11 H11B 107.3 . .
C13 C12 C17 120.8(2) . .
C13 C12 C11 119.0(2) . .
C17 C12 C11 120.2(2) . .
C14 C13 C12 121.2(2) . .
C14 C13 H13 119.4 . .
C12 C13 H13 119.4 . .
C13 C14 C15 116.8(2) . .
C13 C14 C24 120.3(2) . .
C15 C14 C24 122.8(2) . .
C14 C15 C16 124.6(2) . .
C14 C15 H15 117.7 . .
C16 C15 H15 117.7 . .
C15 C16 C17 116.8(2) . .
C15 C16 C28 121.1(2) . .
C17 C16 C28 122.1(2) . .
O6 C17 C12 118.5(2) . .
O6 C17 C16 122.0(2) . .
C12 C17 C16 119.5(2) . .
C19 C18 C23 120.4(2) . .
C19 C18 C10 119.6(2) . .
C23 C18 C10 119.9(2) . .
C20 C19 C18 121.4(2) . .
C20 C19 H19 119.3 . .
C18 C19 H19 119.3 . .
C19 C20 C21 117.0(2) . .
C19 C20 C32 122.7(2) . .
C21 C20 C32 120.3(2) . .
C20 C21 C22 124.1(2) . .
C20 C21 H21 117.9 . .
C22 C21 H21 117.9 . .
C21 C22 C23 117.0(2) . .
C21 C22 C36 121.0(2) . .
C23 C22 C36 121.9(2) . .
O4 C23 C18 118.3(2) . .
O4 C23 C22 121.9(2) . .
C18 C23 C22 119.8(2) . .
C27B C24 C26B 70.4(6) . .
C27B C24 C26A 96.9(6) . .
C26B C24 C26A 26.8(3) . .
C27B C24 C25 122.7(4) . .
C26B C24 C25 116.5(3) . .
C26A C24 C25 98.8(4) . .
C27B C24 C27A 35.7(4) . .
C26B C24 C27A 105.5(4) . .
C26A C24 C27A 131.0(5) . .
C25 C24 C27A 100.8(3) . .
C27B C24 C14 115.7(4) . .
C26B C24 C14 112.2(3) . .
C26A C24 C14 104.9(3) . .
C25 C24 C14 112.6(2) . .
C27A C24 C14 108.0(2) . .
C24 C25 H25A 109.5 . .
C24 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
C24 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C24 C26A H26A 103.6 . .
C24 C26A H26B 117.2 . .
H26A C26A H26B 109.5 . .
C24 C26A H26C 107.3 . .
H26A C26A H26C 109.5 . .
H26B C26A H26C 109.5 . .
C24 C26B H26D 108.2 . .
C24 C26B H26E 111.8 . .
H26D C26B H26E 109.5 . .
C24 C26B H26F 108.5 . .
H26D C26B H26F 109.5 . .
H26E C26B H26F 109.5 . .
C24 C27A H27A 109.1 . .
C24 C27A H27B 110.6 . .
H27A C27A H27B 109.5 . .
C24 C27A H27C 108.7 . .
H27A C27A H27C 109.5 . .
H27B C27A H27C 109.5 . .
C24 C27B H27D 110.2 . .
H27D C27B H27E 109.5 . .
C24 C27B H27F 104.8 . .
H27D C27B H27F 109.5 . .
H27E C27B H27F 109.5 . .
C16 C28 C30 110.2(2) . .
C16 C28 C29 111.5(2) . .
C30 C28 C29 108.0(2) . .
C16 C28 C31 111.0(2) . .
C30 C28 C31 110.0(2) . .
C29 C28 C31 106.2(2) . .
C28 C29 H29A 109.5 . .
C28 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C28 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C28 C30 H30A 109.5 . .
C28 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
C28 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C28 C31 H31A 109.5 . .
C28 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C28 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C34 C32 C35 108.7(3) . .
C34 C32 C33 108.4(3) . .
C35 C32 C33 107.3(2) . .
C34 C32 C20 111.0(2) . .
C35 C32 C20 109.1(2) . .
C33 C32 C20 112.2(2) . .
C32 C33 H33A 109.5 . .
C32 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C32 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C32 C34 H34A 109.5 . .
C32 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C32 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C32 C35 H35A 109.5 . .
C32 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
C32 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
C39 C36 C37 107.4(2) . .
C39 C36 C38 107.7(2) . .
C37 C36 C38 109.2(2) . .
C39 C36 C22 112.3(2) . .
C37 C36 C22 110.63(19) . .
C38 C36 C22 109.5(2) . .
C36 C37 H37A 109.5 . .
C36 C37 H37B 109.5 . .
H37A C37 H37B 109.5 . .
C36 C37 H37C 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
C36 C38 H38A 109.5 . .
C36 C38 H38B 109.5 . .
H38A C38 H38B 109.5 . .
C36 C38 H38C 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
C36 C39 H39A 109.5 . .
C36 C39 H39B 109.5 . .
H39A C39 H39B 109.5 . .
C36 C39 H39C 109.5 . .
H39A C39 H39C 109.5 . .
H39B C39 H39C 109.5 . .
O5 C40 C41 108.3(2) . .
O5 C40 C43 108.0(2) . .
C41 C40 C43 111.6(3) . .
O5 C40 C42 107.5(2) . .
C41 C40 C42 110.9(3) . .
C43 C40 C42 110.4(2) . .
C40 C41 H41A 109.5 . .
C40 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
C40 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C40 C42 H42A 109.5 . .
C40 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
C40 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C40 C43 H43A 109.5 . .
C40 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
C40 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
O7 C44 C47 108.6(2) . .
O7 C44 C46 108.6(2) . .
C47 C44 C46 109.6(2) . .
O7 C44 C45 108.4(2) . .
C47 C44 C45 110.5(3) . .
C46 C44 C45 111.0(2) . .
C44 C45 H45A 109.5 . .
C44 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
C44 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
C44 C46 H46A 109.5 . .
C44 C46 H46B 109.5 . .
H46A C46 H46B 109.5 . .
C44 C46 H46C 109.5 . .
H46A C46 H46C 109.5 . .
H46B C46 H46C 109.5 . .
C44 C47 H47A 109.5 . .
C44 C47 H47B 109.5 . .
H47A C47 H47B 109.5 . .
C44 C47 H47C 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
C49 C48 C48 115.5(4) . 3_666
C49 C48 H48A 108.4 . .
C48 C48 H48A 108.4 3_666 .
C49 C48 H48B 108.4 . .
C48 C48 H48B 108.4 3_666 .
H48A C48 H48B 107.5 . .
C48 C49 C50 114.3(5) . .
C48 C49 H49A 108.7 . .
C50 C49 H49A 108.7 . .
C48 C49 H49B 108.7 . .
C50 C49 H49B 108.7 . .
H49A C49 H49B 107.6 . .
C49 C50 H50A 109.5 . .
C49 C50 H50B 109.5 . .
H50A C50 H50B 109.5 . .
C49 C50 H50C 109.5 . .
H50A C50 H50C 109.5 . .
H50B C50 H50C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O7 1.9269(18) .
Zr1 O5 1.9309(17) .
Zr1 O4 2.0270(17) .
Zr1 O6 2.0320(17) .
Zr1 S3 2.8279(7) .
Zr1 S2 2.8485(7) .
S2 C8 1.814(3) .
S2 C11 1.823(3) .
S3 C9 1.806(3) .
S3 C10 1.821(3) .
O4 C23 1.352(3) .
O5 C40 1.417(3) .
O6 C17 1.348(3) .
O7 C44 1.412(3) .
C8 C9 1.526(4) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C18 1.504(4) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.507(3) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.389(3) .
C12 C17 1.403(3) .
C13 C14 1.389(3) .
C13 H13 0.9500 .
C14 C15 1.393(4) .
C14 C24 1.542(3) .
C15 C16 1.397(3) .
C15 H15 0.9500 .
C16 C17 1.417(3) .
C16 C28 1.538(3) .
C18 C19 1.397(4) .
C18 C23 1.403(3) .
C19 C20 1.387(4) .
C19 H19 0.9500 .
C20 C21 1.394(4) .
C20 C32 1.547(4) .
C21 C22 1.407(3) .
C21 H21 0.9500 .
C22 C23 1.410(3) .
C22 C36 1.541(3) .
C24 C27B 1.494(4) .
C24 C26B 1.484(4) .
C24 C26A 1.533(4) .
C24 C25 1.516(4) .
C24 C27A 1.542(3) .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
C26A H26A 0.9800 .
C26A H26B 0.9800 .
C26A H26C 0.9800 .
C26B H26D 0.9800 .
C26B H26E 0.9800 .
C26B H26F 0.9800 .
C27A H27A 0.9800 .
C27A H27B 0.9800 .
C27A H27C 0.9800 .
C27B H27D 0.9800 .
C27B H27E 0.9800 .
C27B H27F 0.9800 .
C28 C30 1.534(4) .
C28 C29 1.537(3) .
C28 C31 1.543(3) .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 C34 1.518(5) .
C32 C35 1.534(4) .
C32 C33 1.538(4) .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
C35 H35A 0.9800 .
C35 H35B 0.9800 .
C35 H35C 0.9800 .
C36 C39 1.530(3) .
C36 C37 1.541(4) .
C36 C38 1.541(3) .
C37 H37A 0.9800 .
C37 H37B 0.9800 .
C37 H37C 0.9800 .
C38 H38A 0.9800 .
C38 H38B 0.9800 .
C38 H38C 0.9800 .
C39 H39A 0.9800 .
C39 H39B 0.9800 .
C39 H39C 0.9800 .
C40 C41 1.517(4) .
C40 C43 1.520(4) .
C40 C42 1.532(4) .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C43 H43A 0.9800 .
C43 H43B 0.9800 .
C43 H43C 0.9800 .
C44 C47 1.525(4) .
C44 C46 1.528(4) .
C44 C45 1.527(4) .
C45 H45A 0.9800 .
C45 H45B 0.9800 .
C45 H45C 0.9800 .
C46 H46A 0.9800 .
C46 H46B 0.9800 .
C46 H46C 0.9800 .
C47 H47A 0.9800 .
C47 H47B 0.9800 .
C47 H47C 0.9800 .
C48 C49 1.497(5) .
C48 C48 1.508(8) 3_666
C48 H48A 0.9900 .
C48 H48B 0.9900 .
C49 C50 1.504(9) .
C49 H49A 0.9900 .
C49 H49B 0.9900 .
C50 H50A 0.9800 .
C50 H50B 0.9800 .
C50 H50C 0.9800 .
