# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Dr Claire Carmalt' _publ_contact_author_address ; Department of Chemistry University College London Christopher Ingold Laboratories 20 Gordon Street London WC1H 0AJ UNITED KINGDOM ; _publ_contact_author_email C.J.CARMALT@UCL.AC.UK _publ_section_title ; Reactivity of tetrakisdimethylamido-titanium(IV) and -zirconium(IV) with thiols ; loop_ _publ_author_name 'Claire Carmalt' 'Ivan P. Parkin' 'Emily S. Peters' 'Derek A. Tocher' data_str0145 _database_code_depnum_ccdc_archive 'CCDC 248661' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H36 F18 N2 S6 Ti' _chemical_formula_weight 886.77 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' F F 0.0171 0.0103 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.173(6) _cell_length_b 10.794(8) _cell_length_c 10.913(8) _cell_angle_alpha 69.848(13) _cell_angle_beta 85.759(13) _cell_angle_gamma 82.043(13) _cell_volume 894.7(11) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 450 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7387 _exptl_absorpt_correction_T_max 0.9461 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7839 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.46 _reflns_number_total 4106 _reflns_number_gt 3675 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+0.6631P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4106 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.0000 1.0000 0.5000 0.01630(13) Uani 1 2 d S . . S1 S 0.13414(6) 1.15880(5) 0.55723(5) 0.02073(13) Uani 1 1 d . . . S2 S 0.24216(6) 0.83924(5) 0.51624(5) 0.02054(13) Uani 1 1 d . . . S3 S 0.07428(7) 1.07991(5) 0.26941(5) 0.02150(13) Uani 1 1 d . . . C1 C 0.3369(3) 1.0868(3) 0.6231(2) 0.0289(5) Uani 1 1 d . . . H1A H 0.3446 0.9887 0.6510 0.035 Uiso 1 1 calc R . . H1B H 0.4226 1.1162 0.5538 0.035 Uiso 1 1 calc R . . C2 C 0.3698(3) 1.1260(2) 0.7364(2) 0.0312(5) Uani 1 1 d . . . C3 C 0.2530(4) 0.7122(3) 0.6768(3) 0.0416(7) Uani 1 1 d . . . H3A H 0.2687 0.7535 0.7426 0.050 Uiso 1 1 calc R . . H3B H 0.1470 0.6737 0.6982 0.050 Uiso 1 1 calc R . . C4 C 0.3890(3) 0.6049(2) 0.6847(2) 0.0332(5) Uani 1 1 d . . . C5 C 0.2181(3) 1.2012(2) 0.2364(2) 0.0315(5) Uani 1 1 d . . . H5A H 0.1914 1.2535 0.2956 0.038 Uiso 1 1 calc R . . H5B H 0.3313 1.1544 0.2550 0.038 Uiso 1 1 calc R . . C6 C 0.2137(4) 1.2928(3) 0.0993(3) 0.0482(8) Uani 1 1 d . . . F1 F 0.3764(3) 1.25462(18) 0.7046(2) 0.0644(6) Uani 1 1 d . . . F2 F 0.2577(2) 1.0937(2) 0.83277(16) 0.0573(5) Uani 1 1 d . . . F3 F 0.51676(19) 1.06654(18) 0.78854(17) 0.0460(4) Uani 1 1 d . . . F4 F 0.4009(2) 0.51335(17) 0.80313(16) 0.0558(5) Uani 1 1 d . . . F5 F 0.5366(2) 0.6471(2) 0.6545(2) 0.0732(7) Uani 1 1 d . . . F6 F 0.3747(3) 0.54094(17) 0.60317(19) 0.0682(6) Uani 1 1 d . . . F7 F 0.2525(3) 1.2331(2) 0.01216(18) 0.0761(7) Uani 1 1 d . . . F8 F 0.0637(3) 1.3615(2) 0.0667(2) 0.0819(7) Uani 1 1 d . . . F9 F 0.3191(4) 1.3828(2) 0.07890(18) 0.0854(9) Uani 1 1 d . . . N1 N 0.8417(2) 0.22419(19) 0.75517(19) 0.0274(4) Uani 1 1 d . . . H1C H 0.9365 0.1931 0.7186 0.033 Uiso 1 1 calc R . . H1D H 0.7563 0.1852 0.7388 0.033 Uiso 1 1 calc R . . C7 C 0.8085(4) 0.3707(3) 0.6871(3) 0.0427(7) Uani 1 1 d . . . H7A H 0.7052 0.4055 0.7239 0.051 Uiso 1 1 calc R . . H7B H 0.7923 0.3886 0.5933 0.051 Uiso 1 1 calc R . . C8 C 0.8611(4) 0.1786(3) 0.8994(2) 0.0368(6) Uani 1 1 d . . . H8A H 0.9605 0.2114 0.9181 0.044 Uiso 1 1 calc R . . H8B H 0.8786 0.0803 0.9337 0.044 Uiso 1 1 calc R . . C9 C 0.9471(5) 0.4419(3) 0.7010(3) 0.0568(9) Uani 1 1 d . . . H9A H 0.9503 0.4383 0.7917 0.085 Uiso 1 1 calc R . . H9B H 0.9296 0.5349 0.6435 0.085 Uiso 1 1 calc R . . H9C H 1.0521 0.3992 0.6767 0.085 Uiso 1 1 calc R . . C10 C 0.7123(5) 0.2270(4) 0.9694(3) 0.0587(9) Uani 1 1 d . . . H10A H 0.7026 0.3240 0.9440 0.088 Uiso 1 1 calc R . . H10B H 0.7259 0.1871 1.0640 0.088 Uiso 1 1 calc R . . H10C H 0.6122 0.2011 0.9456 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0159(2) 0.0153(2) 0.0192(2) -0.00771(19) 0.00012(18) -0.00219(18) S1 0.0218(3) 0.0211(2) 0.0231(3) -0.0112(2) 0.00054(19) -0.00578(19) S2 0.0190(3) 0.0198(2) 0.0226(3) -0.00829(19) -0.00023(18) 0.00126(18) S3 0.0252(3) 0.0206(2) 0.0207(3) -0.00936(19) 0.00172(19) -0.00432(19) C1 0.0173(10) 0.0414(13) 0.0374(13) -0.0251(11) -0.0006(9) -0.0046(9) C2 0.0260(12) 0.0360(13) 0.0382(13) -0.0199(11) -0.0051(10) -0.0046(9) C3 0.0502(16) 0.0330(13) 0.0285(12) -0.0018(10) 0.0059(11) 0.0126(12) C4 0.0366(13) 0.0254(11) 0.0330(13) -0.0052(10) -0.0066(10) 0.0023(10) C5 0.0413(14) 0.0315(12) 0.0250(11) -0.0108(9) 0.0051(10) -0.0156(10) C6 0.077(2) 0.0482(17) 0.0257(13) -0.0116(12) 0.0114(13) -0.0359(16) F1 0.0813(14) 0.0386(9) 0.0888(15) -0.0338(10) -0.0383(12) -0.0071(9) F2 0.0414(9) 0.1025(15) 0.0317(8) -0.0283(9) 0.0021(7) -0.0075(10) F3 0.0319(8) 0.0615(11) 0.0543(10) -0.0312(9) -0.0167(7) 0.0006(7) F4 0.0703(12) 0.0391(9) 0.0366(9) 0.0072(7) -0.0058(8) 0.0142(8) F5 0.0322(9) 0.0610(12) 0.0975(16) 0.0110(11) -0.0165(10) -0.0006(9) F6 0.1151(18) 0.0332(9) 0.0575(12) -0.0227(9) -0.0251(12) 0.0186(10) F7 0.1116(18) 0.1054(17) 0.0375(10) -0.0450(11) 0.0370(11) -0.0658(15) F8 0.114(2) 0.0443(11) 0.0639(14) 0.0146(10) -0.0232(13) -0.0064(12) F9 0.149(2) 0.0868(15) 0.0347(10) -0.0135(10) 0.0215(12) -0.0920(16) N1 0.0283(10) 0.0290(10) 0.0304(10) -0.0175(8) -0.0010(8) -0.0017(8) C7 0.0589(18) 0.0326(13) 0.0371(14) -0.0162(11) -0.0144(13) 0.0114(12) C8 0.0481(15) 0.0350(13) 0.0290(12) -0.0141(10) -0.0037(11) -0.0014(11) C9 0.085(3) 0.0291(14) 0.061(2) -0.0204(14) 0.0043(18) -0.0123(15) C10 0.068(2) 0.076(2) 0.0460(18) -0.0385(17) 0.0199(16) -0.0179(18) _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 Ti1 S2 2.4183(14) 2_576 ? Ti1 S2 2.4183(14) . ? Ti1 S3 2.4224(17) . ? Ti1 S3 2.4224(17) 2_576 ? Ti1 S1 2.4267(13) 2_576 ? Ti1 S1 2.4267(13) . ? S1 C1 1.817(3) . ? S2 C3 1.815(3) . ? S3 C5 1.806(3) . ? C1 C2 1.490(3) . ? C2 F1 1.318(3) . ? C2 F2 1.327(3) . ? C2 F3 1.347(3) . ? C3 C4 1.474(4) . ? C4 F6 1.320(3) . ? C4 F5 1.327(3) . ? C4 F4 1.330(3) . ? C5 C6 1.482(4) . ? C6 F7 1.319(3) . ? C6 F9 1.338(3) . ? C6 F8 1.345(4) . ? N1 C7 1.492(3) . ? N1 C8 1.492(3) . ? C7 C9 1.498(5) . ? C8 C10 1.516(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 _geom_angle_publ_flag S2 Ti1 S2 180.000(1) 2_576 . ? S2 Ti1 S3 95.35(3) 2_576 . ? S2 Ti1 S3 84.65(3) . . ? S2 Ti1 S3 84.65(3) 2_576 2_576 ? S2 Ti1 S3 95.35(3) . 2_576 ? S3 Ti1 S3 180.0 . 2_576 ? S2 Ti1 S1 96.37(5) 2_576 2_576 ? S2 Ti1 S1 83.63(5) . 2_576 ? S3 Ti1 S1 83.86(4) . 2_576 ? S3 Ti1 S1 96.14(4) 2_576 2_576 ? S2 Ti1 S1 83.63(6) 2_576 . ? S2 Ti1 S1 96.37(6) . . ? S3 Ti1 S1 96.14(4) . . ? S3 Ti1 S1 83.86(4) 2_576 . ? S1 Ti1 S1 180.000(1) 2_576 . ? C1 S1 Ti1 111.28(9) . . ? C3 S2 Ti1 111.32(9) . . ? C5 S3 Ti1 110.36(8) . . ? C2 C1 S1 111.95(16) . . ? F1 C2 F2 106.7(2) . . ? F1 C2 F3 105.6(2) . . ? F2 C2 F3 106.3(2) . . ? F1 C2 C1 113.0(2) . . ? F2 C2 C1 113.3(2) . . ? F3 C2 C1 111.4(2) . . ? C4 C3 S2 112.33(19) . . ? F6 C4 F5 104.0(2) . . ? F6 C4 F4 106.4(2) . . ? F5 C4 F4 106.1(2) . . ? F6 C4 C3 113.2(2) . . ? F5 C4 C3 113.7(2) . . ? F4 C4 C3 112.7(2) . . ? C6 C5 S3 112.37(19) . . ? F7 C6 F9 106.8(2) . . ? F7 C6 F8 105.4(3) . . ? F9 C6 F8 106.5(3) . . ? F7 C6 C5 114.0(3) . . ? F9 C6 C5 110.8(2) . . ? F8 C6 C5 112.7(3) . . ? C7 N1 C8 116.48(19) . . ? N1 C7 C9 112.0(2) . . ? N1 C8 C10 112.6(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Ti1 S1 C1 167.41(9) 2_576 . . . ? S2 Ti1 S1 C1 -12.59(9) . . . . ? S3 Ti1 S1 C1 -97.87(9) . . . . ? S3 Ti1 S1 C1 82.13(9) 2_576 . . . ? S1 Ti1 S1 C1 34(100) 2_576 . . . ? S2 Ti1 S2 C3 38(100) 2_576 . . . ? S3 Ti1 S2 C3 -170.41(12) . . . . ? S3 Ti1 S2 C3 9.59(12) 2_576 . . . ? S1 Ti1 S2 C3 -86.02(12) 2_576 . . . ? S1 Ti1 S2 C3 93.98(12) . . . . ? S2 Ti1 S3 C5 92.58(11) 2_576 . . . ? S2 Ti1 S3 C5 -87.42(11) . . . . ? S3 Ti1 S3 C5 136(100) 2_576 . . . ? S1 Ti1 S3 C5 -171.57(10) 2_576 . . . ? S1 Ti1 S3 C5 8.43(10) . . . . ? Ti1 S1 C1 C2 -139.11(16) . . . . ? S1 C1 C2 F1 -64.5(3) . . . . ? S1 C1 C2 F2 57.0(3) . . . . ? S1 C1 C2 F3 176.80(17) . . . . ? Ti1 S2 C3 C4 173.59(18) . . . . ? S2 C3 C4 F6 -61.1(3) . . . . ? S2 C3 C4 F5 57.3(3) . . . . ? S2 C3 C4 F4 178.1(2) . . . . ? Ti1 S3 C5 C6 -155.7(2) . . . . ? S3 C5 C6 F7 -60.7(3) . . . . ? S3 C5 C6 F9 178.8(2) . . . . ? S3 C5 C6 F8 59.5(3) . . . . ? C8 N1 C7 C9 61.8(3) . . . . ? C7 N1 C8 C10 56.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.763 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.075 #===END data_str0222 _database_code_depnum_ccdc_archive 'CCDC 248662' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H93 Cl4 N S9 Zr2' _chemical_formula_weight 1200.93 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8588(6) _cell_length_b 18.7448(10) _cell_length_c 27.2112(14) _cell_angle_alpha 90.00 _cell_angle_beta 94.2710(10) _cell_angle_gamma 90.00 _cell_volume 6032.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6778 _exptl_absorpt_correction_T_max 0.7703 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52874 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 28.32 _reflns_number_total 14128 _reflns_number_gt 12313 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+10.8183P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14128 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.19570(2) 0.453689(14) 0.183133(10) 0.01426(7) Uani 1 1 d . . . Zr2 Zr 0.28081(2) 0.451665(14) 0.322807(10) 0.01434(7) Uani 1 1 d . . . S1 S 0.34856(7) 0.47657(4) 0.13020(3) 0.02519(17) Uani 1 1 d . . . S2 S 0.04014(7) 0.53286(4) 0.15248(3) 0.02338(16) Uani 1 1 d . . . S3 S 0.13207(6) 0.32926(4) 0.15533(3) 0.02038(15) Uani 1 1 d . . . S4 S 0.20863(6) 0.55158(4) 0.25563(2) 0.01550(13) Uani 1 1 d . . . S5 S 0.36261(6) 0.39140(4) 0.24322(3) 0.01589(14) Uani 1 1 d . . . S6 S 0.11164(5) 0.39796(4) 0.26360(3) 0.01511(13) Uani 1 1 d . . . S7 S 0.43266(6) 0.53780(4) 0.34598(3) 0.02327(16) Uani 1 1 d . . . S8 S 0.15351(8) 0.46114(5) 0.38955(3) 0.03016(19) Uani 1 1 d . . . S9 S 0.33460(6) 0.32589(4) 0.35091(3) 0.02081(15) Uani 1 1 d . . . C1 C 0.3557(3) 0.53561(18) 0.07565(12) 0.0255(7) Uani 1 1 d . . . C2 C 0.4826(3) 0.5439(3) 0.06933(17) 0.0495(11) Uani 1 1 d . . . H2A H 0.4933 0.5747 0.0410 0.074 Uiso 1 1 calc R . . H2B H 0.5157 0.4969 0.0639 0.074 Uiso 1 1 calc R . . H2C H 0.5198 0.5653 0.0991 0.074 Uiso 1 1 calc R . . C3 C 0.3002(4) 0.5006(3) 0.03077(15) 0.0530(12) Uani 1 1 d . . . H3A H 0.3045 0.5322 0.0023 0.080 Uiso 1 1 calc R . . H3B H 0.2208 0.4908 0.0360 0.080 Uiso 1 1 calc R . . H3C H 0.3390 0.4556 0.0246 0.080 Uiso 1 1 calc R . . C4 C 0.3052(4) 0.6079(2) 0.08440(16) 0.0527(12) Uani 1 1 d . . . H4A H 0.3102 0.6376 0.0550 0.079 Uiso 1 1 calc R . . H4B H 0.3468 0.6307 0.1126 0.079 Uiso 1 1 calc R . . H4C H 0.2257 0.6023 0.0912 0.079 Uiso 1 1 calc R . . C5 C -0.0637(3) 0.51975(19) 0.09859(12) 0.0284(7) Uani 1 1 d . . . C6 C -0.1805(3) 0.5206(3) 0.11798(15) 0.0450(10) Uani 1 1 d . . . H6A H -0.2378 0.5139 0.0905 0.068 Uiso 1 1 calc R . . H6B H -0.1928 0.5665 0.1340 0.068 Uiso 1 1 calc R . . H6C H -0.1862 0.4819 0.1419 0.068 Uiso 1 1 calc R . . C7 C -0.0504(4) 0.5830(2) 0.06436(15) 0.0465(11) Uani 1 1 d . . . H7A H -0.1039 0.5783 0.0353 0.070 Uiso 1 1 calc R . . H7B H 0.0269 0.5841 0.0540 0.070 Uiso 1 1 calc R . . H7C H -0.0658 0.6274 0.0818 0.070 Uiso 1 1 calc R . . C8 C -0.0438(3) 0.4508(2) 0.07194(14) 0.0361(8) Uani 1 1 d . . . H8A H -0.1000 0.4459 0.0439 0.054 Uiso 1 1 calc R . . H8B H -0.0507 0.4106 0.0945 0.054 Uiso 1 1 calc R . . H8C H 0.0323 0.4511 0.0601 0.054 Uiso 1 1 calc R . . C9 C 0.1912(3) 0.28322(17) 0.10237(12) 0.0257(7) Uani 1 1 d . . . C10 C 0.1374(4) 0.2092(2) 0.10048(16) 0.0430(10) Uani 1 1 d . . . H10A H 0.1655 0.1820 0.0731 0.065 Uiso 1 1 calc R . . H10B H 0.0551 0.2139 0.0956 0.065 Uiso 1 1 calc R . . H10C H 0.1573 0.1842 0.1316 0.065 Uiso 1 1 calc R . . C11 C 0.1605(4) 0.3226(2) 0.05475(13) 0.0400(9) Uani 1 1 d . . . H11A H 0.1924 0.2975 0.0274 0.060 Uiso 1 1 calc R . . H11B H 0.1912 0.3712 0.0571 0.060 Uiso 1 1 calc R . . H11C H 0.0780 0.3248 0.0489 0.060 Uiso 1 1 calc R . . C12 C 0.3187(3) 0.2770(2) 0.11055(15) 0.0374(9) Uani 1 1 d . . . H12A H 0.3484 0.2526 0.0824 0.056 Uiso 1 1 calc R . . H12B H 0.3382 0.2497 0.1407 0.056 Uiso 1 1 calc R . . H12C H 0.3519 0.3248 0.1139 0.056 Uiso 1 1 calc R . . C13 C 0.2738(2) 0.64054(15) 0.24404(11) 0.0180(6) Uani 1 1 d . . . C14 C 0.2681(3) 0.68538(17) 0.29053(12) 0.0286(7) Uani 1 1 d . . . H14A H 0.3018 0.7323 0.2854 0.043 Uiso 1 1 calc R . . H14B H 0.3098 0.6613 0.3182 0.043 Uiso 1 1 calc R . . H14C H 0.1889 0.6913 0.2978 0.043 Uiso 1 1 calc R . . C15 C 0.2003(3) 0.67568(16) 0.20231(12) 0.0234(6) Uani 1 1 d . . . H15A H 0.2316 0.7225 0.1950 0.035 Uiso 1 1 calc R . . H15B H 0.1232 0.6814 0.2123 0.035 Uiso 1 1 calc R . . H15C H 0.1990 0.6456 0.1728 0.035 Uiso 1 1 calc R . . C16 C 0.3943(3) 0.63336(17) 0.22968(13) 0.0252(7) Uani 1 1 d . . . H16A H 0.4254 0.6808 0.2239 0.038 Uiso 1 1 calc R . . H16B H 0.3951 0.6049 0.1995 0.038 Uiso 1 1 calc R . . H16C H 0.4403 0.6097 0.2563 0.038 Uiso 1 1 calc R . . C17 C 0.5197(2) 0.39600(16) 0.23790(11) 0.0192(6) Uani 1 1 d . . . C18 C 0.5746(3) 0.36089(18) 0.28392(12) 0.0247(7) Uani 1 1 d . . . H18A H 0.6569 0.3620 0.2828 0.037 Uiso 1 1 calc R . . H18B H 0.5490 0.3113 0.2855 0.037 Uiso 1 1 calc R . . H18C H 0.5531 0.3868 0.3131 0.037 Uiso 1 1 calc R . . C19 C 0.5611(3) 0.47252(17) 0.23333(13) 0.0247(7) Uani 1 1 d . . . H19A H 0.6430 0.4725 0.2306 0.037 Uiso 1 1 calc R . . H19B H 0.5435 0.4997 0.2626 0.037 Uiso 1 1 calc R . . H19C H 0.5234 0.4946 0.2039 0.037 Uiso 1 1 calc R . . C20 C 0.5445(3) 0.35330(18) 0.19235(12) 0.0251(7) Uani 1 1 d . . . H20A H 0.6259 0.3544 0.1882 0.038 Uiso 1 1 calc R . . H20B H 0.5035 0.3742 0.1632 0.038 Uiso 1 1 calc R . . H20C H 0.5201 0.3038 0.1962 0.038 Uiso 1 1 calc R . . C21 C -0.0416(2) 0.41497(17) 0.27168(11) 0.0210(6) Uani 1 1 d . . . C22 C -0.0671(3) 0.49408(18) 0.27776(13) 0.0275(7) Uani 1 1 d . . . H22A H -0.1479 0.5004 0.2819 0.041 Uiso 1 1 calc R . . H22B H -0.0471 0.5201 0.2484 0.041 Uiso 1 1 calc R . . H22C H -0.0229 0.5126 0.3068 0.041 Uiso 1 1 calc R . . C23 C -0.0711(3) 0.37341(19) 0.31717(12) 0.0287(7) Uani 1 1 d . . . H23A H -0.1510 0.3809 0.3226 0.043 Uiso 1 1 calc R . . H23B H -0.0239 0.3902 0.3460 0.043 Uiso 1 1 calc R . . H23C H -0.0573 0.3225 0.3121 0.043 Uiso 1 1 calc R . . C24 C -0.1062(3) 0.3844(2) 0.22586(12) 0.0287(7) Uani 1 1 d . . . H24A H -0.1875 0.3916 0.2281 0.043 Uiso 1 1 calc R . . H24B H -0.0903 0.3332 0.2235 0.043 Uiso 1 1 calc R . . H24C H -0.0822 0.4086 0.1965 0.043 Uiso 1 1 calc R . . C25 C 0.5419(3) 0.52523(18) 0.39794(12) 0.0242(6) Uani 1 1 d . . . C26 C 0.5205(3) 0.45869(19) 0.42715(13) 0.0330(8) Uani 1 1 d . . . H26A H 0.5795 0.4538 0.4541 0.049 Uiso 1 1 calc R . . H26B H 0.5217 0.4169 0.4055 0.049 Uiso 1 1 calc R . . H26C H 0.4464 0.4622 0.4407 0.049 Uiso 1 1 calc R . . C27 C 0.5369(3) 0.5908(2) 0.43054(15) 0.0395(9) Uani 1 1 d . . . H27A H 0.5934 0.5865 0.4586 0.059 Uiso 1 1 calc R . . H27B H 0.4614 0.5947 0.4427 0.059 Uiso 1 1 calc R . . H27C H 0.5528 0.6335 0.4114 0.059 Uiso 1 1 calc R . . C28 C 0.6566(3) 0.5214(2) 0.37615(15) 0.0384(9) Uani 1 1 d . . . H28A H 0.7162 0.5148 0.4027 0.058 Uiso 1 1 calc R . . H28B H 0.6701 0.5658 0.3585 0.058 Uiso 1 1 calc R . . H28C H 0.6573 0.4811 0.3532 0.058 Uiso 1 1 calc R . . C29 C 0.1307(3) 0.54339(18) 0.42522(12) 0.0272(7) Uani 1 1 d . . . C30 C 0.0068(3) 0.5419(2) 0.43619(15) 0.0385(9) Uani 1 1 d . . . H30A H -0.0107 0.5844 0.4551 0.058 Uiso 1 1 calc R . . H30B H -0.0080 0.4991 0.4554 0.058 Uiso 1 1 calc R . . H30C H -0.0407 0.5412 0.4052 0.058 Uiso 1 1 calc R . . C31 C 0.1563(4) 0.6092(2) 0.39616(16) 0.0417(9) Uani 1 1 d . . . H31A H 0.1435 0.6518 0.4159 0.063 Uiso 1 1 calc R . . H31B H 0.1066 0.6106 0.3657 0.063 Uiso 1 1 calc R . . H31C H 0.2353 0.6080 0.3880 0.063 Uiso 1 1 calc R . . C32 C 0.2057(4) 0.5387(3) 0.47289(14) 0.0473(11) Uani 1 1 d . . . H32A H 0.1956 0.5816 0.4927 0.071 Uiso 1 1 calc R . . H32B H 0.2850 0.5350 0.4653 0.071 Uiso 1 1 calc R . . H32C H 0.1850 0.4965 0.4915 0.071 Uiso 1 1 calc R . . C33 C 0.2908(3) 0.28231(17) 0.40809(12) 0.0271(7) Uani 1 1 d . . . C34 C 0.3304(3) 0.3242(2) 0.45401(13) 0.0369(9) Uani 1 1 d . . . H34A H 0.3058 0.2998 0.4832 0.055 Uiso 1 1 calc R . . H34B H 0.2979 0.3722 0.4520 0.055 Uiso 1 1 calc R . . H34C H 0.4131 0.3275 0.4564 0.055 Uiso 1 1 calc R . . C35 C 0.3496(4) 0.2094(2) 0.40935(15) 0.0416(9) Uani 1 1 d . . . H35A H 0.3303 0.1831 0.4387 0.062 Uiso 1 1 calc R . . H35B H 0.4316 0.2163 0.4104 0.062 Uiso 1 1 calc R . . H35C H 0.3243 0.1823 0.3797 0.062 Uiso 1 1 calc R . . C36 C 0.1633(3) 0.2726(2) 0.40469(14) 0.0352(8) Uani 1 1 d . . . H36A H 0.1408 0.2498 0.4348 0.053 Uiso 1 1 calc R . . H36B H 0.1404 0.2426 0.3762 0.053 Uiso 1 1 calc R . . H36C H 0.1265 0.3193 0.4008 0.053 Uiso 1 1 calc R . . N1 N 0.2221(2) 0.23808(14) 0.25371(10) 0.0252(6) Uani 1 1 d . . . H1A H 0.2095 0.2670 0.2265 0.030 Uiso 1 1 calc R . . H1B H 0.2414 0.2669 0.2804 0.030 Uiso 1 1 calc R . . C37 C 0.3177(3) 0.1902(2) 0.24584(15) 0.0391(9) Uani 1 1 d . . . H37A H 0.3849 0.2187 0.2403 0.059 Uiso 1 1 calc R . . H37B H 0.2986 0.1600 0.2170 0.059 Uiso 1 1 calc R . . H37C H 0.3332 0.1601 0.2750 0.059 Uiso 1 1 calc R . . C38 C 0.1164(3) 0.2000(2) 0.26232(16) 0.0375(9) Uani 1 1 d . . . H38A H 0.0566 0.2348 0.2674 0.056 Uiso 1 1 calc R . . H38B H 0.1285 0.1698 0.2916 0.056 Uiso 1 1 calc R . . H38C H 0.0938 0.1703 0.2336 0.056 Uiso 1 1 calc R . . Cl1 Cl 0.88721(13) 0.24646(8) 0.98519(4) 0.0681(4) Uani 1 1 d . . . Cl2 Cl 0.71977(12) 0.19181(8) 0.91170(5) 0.0708(4) Uani 1 1 d . . . C39 C 0.8572(4) 0.2227(3) 0.92419(17) 0.0578(13) Uani 1 1 d . . . H39A H 0.9107 0.1850 0.9155 0.069 Uiso 1 1 calc R . . H39B H 0.8692 0.2646 0.9031 0.069 Uiso 1 1 calc R . . Cl3 Cl 0.76813(15) 0.30692(9) 0.10063(6) 0.0893(5) Uani 1 1 d . . . Cl4 Cl 0.56557(19) 0.3089(2) 0.03500(10) 0.1868(17) Uani 1 1 d . . . C40 C 0.6447(5) 0.2649(3) 0.0785(2) 0.0741(16) Uani 1 1 d . . . H40A H 0.6647 0.2179 0.0650 0.089 Uiso 1 1 calc R . . H40B H 0.5981 0.2561 0.1066 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.01378(13) 0.01463(13) 0.01402(13) -0.00042(10) -0.00124(9) 0.00037(10) Zr2 0.01344(13) 0.01499(13) 0.01420(13) 0.00072(10) -0.00154(9) -0.00088(10) S1 0.0221(4) 0.0299(4) 0.0243(4) 0.0073(3) 0.0060(3) 0.0033(3) S2 0.0226(4) 0.0217(4) 0.0244(4) -0.0009(3) -0.0077(3) 0.0044(3) S3 0.0214(3) 0.0173(3) 0.0220(4) -0.0042(3) -0.0015(3) -0.0014(3) S4 0.0169(3) 0.0131(3) 0.0161(3) 0.0000(3) -0.0011(2) -0.0012(2) S5 0.0121(3) 0.0176(3) 0.0175(3) -0.0001(3) -0.0011(2) 0.0017(2) S6 0.0115(3) 0.0160(3) 0.0176(3) -0.0001(3) -0.0005(2) -0.0013(2) S7 0.0222(4) 0.0205(4) 0.0256(4) 0.0019(3) -0.0081(3) -0.0047(3) S8 0.0384(5) 0.0282(4) 0.0256(4) -0.0046(3) 0.0143(3) -0.0076(4) S9 0.0228(4) 0.0173(3) 0.0218(4) 0.0041(3) -0.0025(3) -0.0003(3) C1 0.0257(16) 0.0304(17) 0.0209(15) 0.0053(13) 0.0055(12) -0.0013(13) C2 0.034(2) 0.061(3) 0.054(3) 0.017(2) 0.0100(19) -0.008(2) C3 0.061(3) 0.063(3) 0.033(2) 0.003(2) -0.006(2) -0.018(2) C4 0.072(3) 0.046(2) 0.043(2) 0.018(2) 0.022(2) 0.015(2) C5 0.0279(17) 0.0292(17) 0.0263(17) -0.0021(14) -0.0099(13) 0.0074(13) C6 0.0277(19) 0.066(3) 0.040(2) -0.008(2) -0.0109(16) 0.0139(18) C7 0.065(3) 0.035(2) 0.036(2) 0.0076(17) -0.022(2) 0.0070(19) C8 0.038(2) 0.0342(19) 0.0341(19) -0.0103(16) -0.0117(15) 0.0089(16) C9 0.0271(16) 0.0223(15) 0.0276(16) -0.0110(13) 0.0006(13) 0.0004(13) C10 0.050(2) 0.0264(18) 0.053(2) -0.0168(17) 0.0064(19) -0.0087(17) C11 0.052(2) 0.041(2) 0.0266(18) -0.0097(16) -0.0007(16) 0.0116(18) C12 0.0315(19) 0.038(2) 0.043(2) -0.0147(17) 0.0021(16) 0.0087(16) C13 0.0210(14) 0.0115(12) 0.0212(14) 0.0011(11) -0.0002(11) -0.0031(11) C14 0.043(2) 0.0160(14) 0.0267(17) -0.0041(13) -0.0001(14) -0.0032(13) C15 0.0239(15) 0.0179(14) 0.0278(16) 0.0076(12) -0.0022(12) 0.0002(12) C16 0.0225(15) 0.0198(15) 0.0332(17) 0.0043(13) 0.0013(13) -0.0029(12) C17 0.0103(12) 0.0224(14) 0.0245(15) 0.0004(12) -0.0003(10) 0.0029(11) C18 0.0157(14) 0.0290(16) 0.0288(17) 0.0018(13) -0.0027(12) 0.0053(12) C19 0.0161(14) 0.0242(15) 0.0338(18) 0.0011(13) 0.0020(12) -0.0016(12) C20 0.0167(14) 0.0296(16) 0.0289(17) -0.0027(14) 0.0016(12) 0.0069(12) C21 0.0095(12) 0.0283(16) 0.0255(15) 0.0008(13) 0.0019(11) -0.0014(11) C22 0.0190(15) 0.0293(17) 0.0348(18) 0.0000(14) 0.0055(13) 0.0059(13) C23 0.0220(16) 0.0354(18) 0.0290(17) 0.0022(14) 0.0046(13) -0.0074(14) C24 0.0142(14) 0.0409(19) 0.0300(17) -0.0025(15) -0.0049(12) -0.0030(13) C25 0.0217(15) 0.0285(16) 0.0210(15) -0.0016(13) -0.0079(12) -0.0054(12) C26 0.0339(19) 0.0331(19) 0.0302(18) 0.0051(15) -0.0085(14) -0.0056(15) C27 0.046(2) 0.033(2) 0.038(2) -0.0077(16) -0.0061(17) -0.0096(17) C28 0.0210(17) 0.052(2) 0.042(2) 0.0015(18) -0.0035(15) -0.0056(16) C29 0.0267(16) 0.0292(17) 0.0263(16) -0.0029(14) 0.0064(13) 0.0036(13) C30 0.0305(19) 0.045(2) 0.041(2) 0.0099(18) 0.0134(16) 0.0083(16) C31 0.049(2) 0.0262(18) 0.053(2) 0.0003(17) 0.0227(19) 0.0011(16) C32 0.047(2) 0.066(3) 0.029(2) -0.0172(19) -0.0044(17) 0.004(2) C33 0.0338(18) 0.0228(15) 0.0240(16) 0.0107(13) -0.0029(13) -0.0052(13) C34 0.049(2) 0.038(2) 0.0232(17) 0.0096(15) -0.0057(15) -0.0114(17) C35 0.054(2) 0.0275(19) 0.042(2) 0.0153(17) -0.0048(18) 0.0014(17) C36 0.037(2) 0.0339(19) 0.0340(19) 0.0101(16) 0.0007(15) -0.0130(16) N1 0.0265(14) 0.0188(13) 0.0300(15) -0.0007(11) -0.0011(11) -0.0015(11) C37 0.036(2) 0.034(2) 0.047(2) 0.0006(17) 0.0002(17) 0.0107(16) C38 0.0326(19) 0.0291(18) 0.051(2) 0.0017(17) 0.0040(17) -0.0090(15) Cl1 0.0846(9) 0.0790(9) 0.0390(6) 0.0031(6) -0.0071(6) -0.0222(7) Cl2 0.0646(8) 0.0739(9) 0.0733(9) -0.0163(7) 0.0016(7) -0.0252(7) C39 0.053(3) 0.081(4) 0.041(2) -0.010(2) 0.007(2) -0.013(3) Cl3 0.1090(12) 0.0778(10) 0.0867(11) -0.0354(8) 0.0440(9) -0.0460(9) Cl4 0.0945(15) 0.318(4) 0.152(2) 0.166(3) 0.0401(14) 0.047(2) C40 0.087(4) 0.058(3) 0.075(4) 0.016(3) -0.008(3) -0.010(3) _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 S1 2.4360(8) . ? Zr1 S2 2.4641(8) . ? Zr1 S3 2.5489(8) . ? Zr1 S6 2.6842(7) . ? Zr1 S4 2.6902(7) . ? Zr1 S5 2.7336(7) . ? Zr2 S8 2.4531(9) . ? Zr2 S7 2.4654(8) . ? Zr2 S9 2.5451(8) . ? Zr2 S6 2.6743(7) . ? Zr2 S5 2.6871(8) . ? Zr2 S4 2.7110(7) . ? S1 C1 1.858(3) . ? S2 C5 1.860(3) . ? S3 C9 1.861(3) . ? S4 C13 1.874(3) . ? S5 C17 1.881(3) . ? S6 C21 1.874(3) . ? S7 C25 1.860(3) . ? S8 C29 1.852(3) . ? S9 C33 1.865(3) . ? C1 C3 1.496(5) . ? C1 C4 1.507(5) . ? C1 C2 1.536(5) . ? C5 C8 1.509(5) . ? C5 C6 1.519(5) . ? C5 C7 1.523(5) . ? C9 C11 1.512(5) . ? C9 C12 1.516(5) . ? C9 C10 1.526(5) . ? C13 C16 1.516(4) . ? C13 C14 1.524(4) . ? C13 C15 1.528(4) . ? C17 C18 1.518(4) . ? C17 C20 1.522(4) . ? C17 C19 1.524(4) . ? C21 C22 1.525(4) . ? C21 C23 1.525(4) . ? C21 C24 1.526(4) . ? C25 C26 1.511(5) . ? C25 C27 1.520(5) . ? C25 C28 1.525(5) . ? C29 C31 1.508(5) . ? C29 C32 1.520(5) . ? C29 C30 1.521(5) . ? C33 C36 1.519(5) . ? C33 C34 1.520(5) . ? C33 C35 1.532(5) . ? N1 C37 1.474(4) . ? N1 C38 1.477(4) . ? Cl1 C39 1.730(5) . ? Cl2 C39 1.739(5) . ? Cl3 C40 1.730(6) . ? Cl4 C40 1.672(6) . ? 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 S1 Zr1 S2 105.38(3) . . ? S1 Zr1 S3 101.68(3) . . ? S2 Zr1 S3 104.66(3) . . ? S1 Zr1 S6 152.73(3) . . ? S2 Zr1 S6 101.32(3) . . ? S3 Zr1 S6 76.49(2) . . ? S1 Zr1 S4 108.01(3) . . ? S2 Zr1 S4 80.66(2) . . ? S3 Zr1 S4 147.28(3) . . ? S6 Zr1 S4 70.83(2) . . ? S1 Zr1 S5 83.76(3) . . ? S2 Zr1 S5 161.84(3) . . ? S3 Zr1 S5 88.39(2) . . ? S6 Zr1 S5 69.03(2) . . ? S4 Zr1 S5 81.58(2) . . ? S8 Zr2 S7 103.96(3) . . ? S8 Zr2 S9 89.94(3) . . ? S7 Zr2 S9 111.59(3) . . ? S8 Zr2 S6 89.88(3) . . ? S7 Zr2 S6 154.35(3) . . ? S9 Zr2 S6 89.56(2) . . ? S8 Zr2 S5 154.98(3) . . ? S7 Zr2 S5 100.42(3) . . ? S9 Zr2 S5 75.83(2) . . ? S6 Zr2 S5 69.87(2) . . ? S8 Zr2 S4 105.57(3) . . ? S7 Zr2 S4 84.72(2) . . ? S9 Zr2 S4 154.43(2) . . ? S6 Zr2 S4 70.66(2) . . ? S5 Zr2 S4 82.06(2) . . ? C1 S1 Zr1 131.09(11) . . ? C5 S2 Zr1 128.49(11) . . ? C9 S3 Zr1 122.26(11) . . ? C13 S4 Zr1 119.03(9) . . ? C13 S4 Zr2 127.93(9) . . ? Zr1 S4 Zr2 91.21(2) . . ? C17 S5 Zr2 117.50(10) . . ? C17 S5 Zr1 127.70(10) . . ? Zr2 S5 Zr1 90.78(2) . . ? C21 S6 Zr2 123.76(10) . . ? C21 S6 Zr1 116.85(10) . . ? Zr2 S6 Zr1 92.14(2) . . ? C25 S7 Zr2 124.44(11) . . ? C29 S8 Zr2 124.75(11) . . ? C33 S9 Zr2 125.26(11) . . ? C3 C1 C4 111.6(4) . . ? C3 C1 C2 109.2(3) . . ? C4 C1 C2 109.3(3) . . ? C3 C1 S1 110.3(3) . . ? C4 C1 S1 111.5(2) . . ? C2 C1 S1 104.6(2) . . ? C8 C5 C6 110.8(3) . . ? C8 C5 C7 110.2(3) . . ? C6 C5 C7 110.1(3) . . ? C8 C5 S2 112.0(2) . . ? C6 C5 S2 107.0(2) . . ? C7 C5 S2 106.7(2) . . ? C11 C9 C12 109.7(3) . . ? C11 C9 C10 110.0(3) . . ? C12 C9 C10 110.2(3) . . ? C11 C9 S3 110.9(2) . . ? C12 C9 S3 110.5(2) . . ? C10 C9 S3 105.5(2) . . ? C16 C13 C14 111.3(3) . . ? C16 C13 C15 110.1(3) . . ? C14 C13 C15 108.7(3) . . ? C16 C13 S4 111.9(2) . . ? C14 C13 S4 107.9(2) . . ? C15 C13 S4 106.82(19) . . ? C18 C17 C20 110.3(2) . . ? C18 C17 C19 110.8(3) . . ? C20 C17 C19 110.2(3) . . ? C18 C17 S5 106.4(2) . . ? C20 C17 S5 106.9(2) . . ? C19 C17 S5 112.1(2) . . ? C22 C21 C23 110.4(3) . . ? C22 C21 C24 111.2(3) . . ? C23 C21 C24 109.9(3) . . ? C22 C21 S6 112.4(2) . . ? C23 C21 S6 106.9(2) . . ? C24 C21 S6 105.8(2) . . ? C26 C25 C27 110.2(3) . . ? C26 C25 C28 110.8(3) . . ? C27 C25 C28 109.9(3) . . ? C26 C25 S7 111.7(2) . . ? C27 C25 S7 106.6(2) . . ? C28 C25 S7 107.5(2) . . ? C31 C29 C32 111.5(3) . . ? C31 C29 C30 110.7(3) . . ? C32 C29 C30 110.1(3) . . ? C31 C29 S8 111.3(2) . . ? C32 C29 S8 107.5(3) . . ? C30 C29 S8 105.6(2) . . ? C36 C33 C34 110.9(3) . . ? C36 C33 C35 110.1(3) . . ? C34 C33 C35 109.3(3) . . ? C36 C33 S9 109.8(2) . . ? C34 C33 S9 111.8(2) . . ? C35 C33 S9 104.7(3) . . ? C37 N1 C38 113.6(3) . . ? Cl1 C39 Cl2 113.3(3) . . ? Cl4 C40 Cl3 116.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Zr1 S1 C1 -2.84(15) . . . . ? S3 Zr1 S1 C1 106.11(15) . . . . ? S6 Zr1 S1 C1 -170.76(14) . . . . ? S4 Zr1 S1 C1 -87.82(15) . . . . ? S5 Zr1 S1 C1 -166.84(15) . . . . ? S1 Zr1 S2 C5 80.09(16) . . . . ? S3 Zr1 S2 C5 -26.71(16) . . . . ? S6 Zr1 S2 C5 -105.53(16) . . . . ? S4 Zr1 S2 C5 -173.67(16) . . . . ? S5 Zr1 S2 C5 -161.46(16) . . . . ? S1 Zr1 S3 C9 -5.50(13) . . . . ? S2 Zr1 S3 C9 104.01(13) . . . . ? S6 Zr1 S3 C9 -157.60(13) . . . . ? S4 Zr1 S3 C9 -160.44(13) . . . . ? S5 Zr1 S3 C9 -88.79(13) . . . . ? S1 Zr1 S4 C13 27.09(11) . . . . ? S2 Zr1 S4 C13 -76.15(11) . . . . ? S3 Zr1 S4 C13 -178.76(11) . . . . ? S6 Zr1 S4 C13 178.31(11) . . . . ? S5 Zr1 S4 C13 107.67(11) . . . . ? S1 Zr1 S4 Zr2 -108.54(3) . . . . ? S2 Zr1 S4 Zr2 148.22(3) . . . . ? S3 Zr1 S4 Zr2 45.60(5) . . . . ? S6 Zr1 S4 Zr2 42.68(2) . . . . ? S5 Zr1 S4 Zr2 -27.96(2) . . . . ? S8 Zr2 S4 C13 103.64(12) . . . . ? S7 Zr2 S4 C13 0.59(12) . . . . ? S9 Zr2 S4 C13 -130.93(13) . . . . ? S6 Zr2 S4 C13 -172.11(12) . . . . ? S5 Zr2 S4 C13 -100.73(12) . . . . ? S8 Zr2 S4 Zr1 -127.18(3) . . . . ? S7 Zr2 S4 Zr1 129.77(3) . . . . ? S9 Zr2 S4 Zr1 -1.75(7) . . . . ? S6 Zr2 S4 Zr1 -42.93(2) . . . . ? S5 Zr2 S4 Zr1 28.45(2) . . . . ? S8 Zr2 S5 C17 -143.82(12) . . . . ? S7 Zr2 S5 C17 23.10(11) . . . . ? S9 Zr2 S5 C17 -86.74(11) . . . . ? S6 Zr2 S5 C17 178.44(11) . . . . ? S4 Zr2 S5 C17 106.20(11) . . . . ? S8 Zr2 S5 Zr1 82.03(7) . . . . ? S7 Zr2 S5 Zr1 -111.05(2) . . . . ? S9 Zr2 S5 Zr1 139.10(3) . . . . ? S6 Zr2 S5 Zr1 44.29(2) . . . . ? S4 Zr2 S5 Zr1 -27.96(2) . . . . ? S1 Zr1 S5 C17 11.08(12) . . . . ? S2 Zr1 S5 C17 -110.41(14) . . . . ? S3 Zr1 S5 C17 113.02(12) . . . . ? S6 Zr1 S5 C17 -170.84(12) . . . . ? S4 Zr1 S5 C17 -98.23(12) . . . . ? S1 Zr1 S5 Zr2 137.54(3) . . . . ? S2 Zr1 S5 Zr2 16.05(9) . . . . ? S3 Zr1 S5 Zr2 -120.53(2) . . . . ? S6 Zr1 S5 Zr2 -44.39(2) . . . . ? S4 Zr1 S5 Zr2 28.23(2) . . . . ? S8 Zr2 S6 C21 24.98(12) . . . . ? S7 Zr2 S6 C21 -98.59(13) . . . . ? S9 Zr2 S6 C21 114.92(12) . . . . ? S5 Zr2 S6 C21 -170.02(12) . . . . ? S4 Zr2 S6 C21 -81.59(12) . . . . ? S8 Zr2 S6 Zr1 149.64(3) . . . . ? S7 Zr2 S6 Zr1 26.08(7) . . . . ? S9 Zr2 S6 Zr1 -120.42(2) . . . . ? S5 Zr2 S6 Zr1 -45.36(2) . . . . ? S4 Zr2 S6 Zr1 43.07(2) . . . . ? S1 Zr1 S6 C21 178.83(12) . . . . ? S2 Zr1 S6 C21 10.71(11) . . . . ? S3 Zr1 S6 C21 -91.84(11) . . . . ? S4 Zr1 S6 C21 86.53(11) . . . . ? S5 Zr1 S6 C21 174.65(11) . . . . ? S1 Zr1 S6 Zr2 48.87(7) . . . . ? S2 Zr1 S6 Zr2 -119.26(2) . . . . ? S3 Zr1 S6 Zr2 138.19(3) . . . . ? S4 Zr1 S6 Zr2 -43.43(2) . . . . ? S5 Zr1 S6 Zr2 44.69(2) . . . . ? S8 Zr2 S7 C25 71.21(14) . . . . ? S9 Zr2 S7 C25 -24.36(14) . . . . ? S6 Zr2 S7 C25 -167.95(13) . . . . ? S5 Zr2 S7 C25 -103.13(13) . . . . ? S4 Zr2 S7 C25 175.97(14) . . . . ? S7 Zr2 S8 C29 30.88(14) . . . . ? S9 Zr2 S8 C29 143.14(14) . . . . ? S6 Zr2 S8 C29 -127.30(14) . . . . ? S5 Zr2 S8 C29 -162.38(14) . . . . ? S4 Zr2 S8 C29 -57.45(14) . . . . ? S8 Zr2 S9 C33 -7.10(13) . . . . ? S7 Zr2 S9 C33 97.91(13) . . . . ? S6 Zr2 S9 C33 -96.98(13) . . . . ? S5 Zr2 S9 C33 -166.31(13) . . . . ? S4 Zr2 S9 C33 -135.39(13) . . . . ? Zr1 S1 C1 C3 -79.9(3) . . . . ? Zr1 S1 C1 C4 44.7(3) . . . . ? Zr1 S1 C1 C2 162.8(2) . . . . ? Zr1 S2 C5 C8 -0.5(3) . . . . ? Zr1 S2 C5 C6 121.0(2) . . . . ? Zr1 S2 C5 C7 -121.2(2) . . . . ? Zr1 S3 C9 C11 -64.9(3) . . . . ? Zr1 S3 C9 C12 57.0(3) . . . . ? Zr1 S3 C9 C10 176.1(2) . . . . ? Zr1 S4 C13 C16 -58.2(2) . . . . ? Zr2 S4 C13 C16 59.3(2) . . . . ? Zr1 S4 C13 C14 178.99(17) . . . . ? Zr2 S4 C13 C14 -63.4(2) . . . . ? Zr1 S4 C13 C15 62.3(2) . . . . ? Zr2 S4 C13 C15 179.85(15) . . . . ? Zr2 S5 C17 C18 57.7(2) . . . . ? Zr1 S5 C17 C18 172.62(16) . . . . ? Zr2 S5 C17 C20 175.56(17) . . . . ? Zr1 S5 C17 C20 -69.5(2) . . . . ? Zr2 S5 C17 C19 -63.6(2) . . . . ? Zr1 S5 C17 C19 51.4(3) . . . . ? Zr2 S6 C21 C22 49.8(3) . . . . ? Zr1 S6 C21 C22 -63.1(2) . . . . ? Zr2 S6 C21 C23 -71.6(2) . . . . ? Zr1 S6 C21 C23 175.54(18) . . . . ? Zr2 S6 C21 C24 171.35(17) . . . . ? Zr1 S6 C21 C24 58.5(2) . . . . ? Zr2 S7 C25 C26 -5.0(3) . . . . ? Zr2 S7 C25 C27 -125.4(2) . . . . ? Zr2 S7 C25 C28 116.8(2) . . . . ? Zr2 S8 C29 C31 24.8(3) . . . . ? Zr2 S8 C29 C32 -97.6(3) . . . . ? Zr2 S8 C29 C30 144.93(19) . . . . ? Zr2 S9 C33 C36 64.6(3) . . . . ? Zr2 S9 C33 C34 -59.0(3) . . . . ? Zr2 S9 C33 C35 -177.19(19) . . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.680 _refine_diff_density_min -1.461 _refine_diff_density_rms 0.091 #===END