# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_txy _database_code_depnum_ccdc_archive 'CCDC 888633' #TrackingRef '12208_web_deposit_cif_file_0_Jing-YuLiu_1340755455.2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H39 Cl F2 O5 P2 Zr' _chemical_formula_weight 886.37 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.9957(8) _cell_length_b 15.2366(9) _cell_length_c 20.3856(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4036.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.473 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8789 _exptl_absorpt_correction_T_max 0.9367 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22739 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_av_sigmaI/netI 0.0902 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.04 _reflns_number_total 7142 _reflns_number_gt 5395 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0383P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(5) _refine_ls_number_reflns 7142 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 O3 O 0.6659(2) 0.4989(2) 0.03648(15) 0.0310(8) Uani 1 1 d . . . Zr1 Zr 0.79079(4) 0.49393(3) 0.10078(2) 0.02626(13) Uani 1 1 d . . . P1 P 1.04614(10) 0.45289(7) 0.10324(7) 0.0257(3) Uani 1 1 d . . . P2 P 0.83391(11) 0.54336(9) -0.05955(7) 0.0313(3) Uani 1 1 d . . . Cl1 Cl 0.79715(13) 0.65793(8) 0.11547(7) 0.0485(4) Uani 1 1 d . . . C40 C 0.6883(6) 0.5235(5) 0.2069(3) 0.060(2) Uani 1 1 d . . . H40A H 0.6668 0.5827 0.2230 0.072 Uiso 1 1 calc R . . O2 O 0.9502(2) 0.4933(2) 0.13298(14) 0.0261(7) Uani 1 1 d . . . F2 F 0.4652(2) 0.53508(19) 0.02617(16) 0.0458(9) Uani 1 1 d . . . O4 O 0.8697(3) 0.5355(2) 0.01066(15) 0.0300(9) Uani 1 1 d . . . O1 O 0.8344(3) 0.3731(2) 0.06274(18) 0.0318(9) Uani 1 1 d . . . C25 C 0.9021(4) 0.6296(3) -0.1008(3) 0.0344(13) Uani 1 1 d . . . F1 F 0.8088(2) 0.21359(18) 0.01120(17) 0.0501(9) Uani 1 1 d . . . C8 C 1.1642(4) 0.4975(4) -0.0060(3) 0.0417(13) Uani 1 1 d . . . H8A H 1.1694 0.4364 -0.0144 0.050 Uiso 1 1 calc R . . C19 C 0.6362(4) 0.5412(3) -0.0137(3) 0.0317(13) Uani 1 1 d . . . C6 C 1.0184(4) 0.3505(3) 0.0650(2) 0.0251(12) Uani 1 1 d . . . C1 C 0.9166(4) 0.3254(3) 0.0504(2) 0.0262(12) Uani 1 1 d . . . C13 C 1.1385(4) 0.4297(3) 0.1674(2) 0.0293(12) Uani 1 1 d . . . C31 C 0.8575(4) 0.4428(3) -0.1030(3) 0.0328(12) Uani 1 1 d . . . C14 C 1.2389(4) 0.4602(4) 0.1661(3) 0.0416(15) Uani 1 1 d . . . H14A H 1.2614 0.4968 0.1312 0.050 Uiso 1 1 calc R . . C4 C 1.0857(5) 0.2146(4) 0.0191(3) 0.0407(15) Uani 1 1 d . . . H4A H 1.1424 0.1782 0.0078 0.049 Uiso 1 1 calc R . . C32 C 0.9559(5) 0.4161(4) -0.1124(3) 0.0547(18) Uani 1 1 d . . . H32A H 1.0110 0.4534 -0.0997 0.066 Uiso 1 1 calc R . . C20 C 0.5308(4) 0.5630(3) -0.0215(3) 0.0357(14) Uani 1 1 d . . . C30 C 0.9173(5) 0.6267(4) -0.1682(3) 0.0432(16) Uani 1 1 d . . . H30A H 0.8969 0.5765 -0.1926 0.052 Uiso 1 1 calc R . . C9 C 1.2125(5) 0.5564(4) -0.0471(3) 0.0508(16) Uani 1 1 d . . . H9A H 1.2501 0.5358 -0.0840 0.061 Uiso 1 1 calc R . . C3 C 0.9861(5) 0.1878(3) 0.0058(3) 0.0381(15) Uani 1 1 d . . . H3A H 0.9735 0.1326 -0.0144 0.046 Uiso 1 1 calc R . . C24 C 0.7000(4) 0.5711(3) -0.0654(2) 0.0336(12) Uani 1 1 d . . . C37 C 0.6806(6) 0.3903(5) 0.1655(3) 0.0560(19) Uani 1 1 d . . . H37A H 0.6504 0.3344 0.1485 0.067 Uiso 1 1 calc R . . C26 C 0.9313(6) 0.7012(4) -0.0668(3) 0.068(2) Uani 1 1 d . . . H26A H 0.9197 0.7046 -0.0208 0.081 Uiso 1 1 calc R . . C5 C 1.1016(4) 0.2948(3) 0.0490(3) 0.0344(14) Uani 1 1 d . . . H5A H 1.1698 0.3128 0.0589 0.041 Uiso 1 1 calc R . . C2 C 0.9060(4) 0.2416(3) 0.0221(3) 0.0349(14) Uani 1 1 d . . . C17 C 1.1763(5) 0.3546(4) 0.2679(3) 0.0490(18) Uani 1 1 d . . . H17A H 1.1549 0.3177 0.3029 0.059 Uiso 1 1 calc R . . C38 C 0.7714(5) 0.3971(4) 0.2002(3) 0.0497(17) Uani 1 1 d . . . H38A H 0.8177 0.3471 0.2122 0.060 Uiso 1 1 calc R . . C16 C 1.2741(5) 0.3851(4) 0.2663(3) 0.0553(19) Uani 1 1 d . . . H16A H 1.3205 0.3701 0.3005 0.066 Uiso 1 1 calc R . . C33 C 0.9771(6) 0.3349(4) -0.1405(3) 0.067(2) Uani 1 1 d . . . H33A H 1.0462 0.3165 -0.1470 0.081 Uiso 1 1 calc R . . C22 C 0.5577(5) 0.6404(4) -0.1216(3) 0.0473(17) Uani 1 1 d . . . H22A H 0.5318 0.6736 -0.1574 0.057 Uiso 1 1 calc R . . C10 C 1.2061(5) 0.6444(4) -0.0346(3) 0.0558(18) Uani 1 1 d . . . H10A H 1.2383 0.6852 -0.0632 0.067 Uiso 1 1 calc R . . C35 C 0.7989(6) 0.3077(4) -0.1502(3) 0.0621(19) Uani 1 1 d . . . H35A H 0.7443 0.2703 -0.1636 0.074 Uiso 1 1 calc R . . C41 C 0.6297(5) 0.4691(5) 0.1696(3) 0.058(2) Uani 1 1 d . . . H41A H 0.5573 0.4805 0.1553 0.070 Uiso 1 1 calc R . . C15 C 1.3066(5) 0.4374(4) 0.2160(3) 0.0519(17) Uani 1 1 d . . . H15A H 1.3756 0.4581 0.2151 0.062 Uiso 1 1 calc R . . C21 C 0.4935(5) 0.6124(4) -0.0732(3) 0.0457(16) Uani 1 1 d . . . H21A H 0.4225 0.6269 -0.0749 0.055 Uiso 1 1 calc R . . C29 C 0.9615(5) 0.6964(4) -0.1991(3) 0.0560(18) Uani 1 1 d . . . H29A H 0.9706 0.6952 -0.2453 0.067 Uiso 1 1 calc R . . C34 C 0.8975(6) 0.2826(4) -0.1582(3) 0.063(2) Uani 1 1 d . . . H34A H 0.9117 0.2267 -0.1768 0.076 Uiso 1 1 calc R . . C12 C 1.1033(5) 0.6146(4) 0.0599(3) 0.0469(16) Uani 1 1 d . . . H12A H 1.0656 0.6357 0.0966 0.056 Uiso 1 1 calc R . . C23 C 0.6614(5) 0.6196(4) -0.1178(3) 0.0429(16) Uani 1 1 d . . . H23A H 0.7067 0.6387 -0.1515 0.052 Uiso 1 1 calc R . . C36 C 0.7784(5) 0.3882(4) -0.1224(3) 0.0461(16) Uani 1 1 d . . . H36A H 0.7091 0.4063 -0.1165 0.055 Uiso 1 1 calc R . . C28 C 0.9927(6) 0.7675(4) -0.1645(4) 0.071(2) Uani 1 1 d . . . H28A H 1.0245 0.8154 -0.1863 0.086 Uiso 1 1 calc R . . C27 C 0.9787(7) 0.7702(4) -0.0997(4) 0.096(3) Uani 1 1 d . . . H27A H 1.0014 0.8200 -0.0757 0.115 Uiso 1 1 calc R . . C42 C 0.8266(9) 0.1754(5) 0.2475(5) 0.105(3) Uani 1 1 d . . . H42A H 0.7703 0.2192 0.2476 0.126 Uiso 1 1 calc R . . H42B H 0.8190 0.1365 0.2861 0.126 Uiso 1 1 calc R . . C43 C 0.8281(11) 0.1247(8) 0.1859(5) 0.152(6) Uani 1 1 d . . . H43A H 0.7792 0.0750 0.1886 0.183 Uiso 1 1 calc R . . H43B H 0.8079 0.1626 0.1486 0.183 Uiso 1 1 calc R . . C39 C 0.7771(5) 0.4798(4) 0.2252(3) 0.0481(16) Uani 1 1 d . . . H39A H 0.8290 0.5012 0.2578 0.058 Uiso 1 1 calc R . . C18 C 1.1069(5) 0.3766(4) 0.2186(3) 0.0424(16) Uani 1 1 d . . . H18A H 1.0382 0.3554 0.2201 0.051 Uiso 1 1 calc R . . C11 C 1.1540(5) 0.6732(4) 0.0185(4) 0.064(2) Uani 1 1 d . . . H11A H 1.1519 0.7343 0.0278 0.077 Uiso 1 1 calc R . . C45 C 0.9904(8) 0.1580(6) 0.2163(6) 0.129(4) Uani 1 1 d . . . H45A H 1.0322 0.1274 0.2499 0.154 Uiso 1 1 calc R . . H45B H 1.0376 0.1914 0.1875 0.154 Uiso 1 1 calc R . . C7 C 1.1080(4) 0.5268(3) 0.0475(2) 0.0273(13) Uani 1 1 d . . . O5 O 0.9213(5) 0.2154(3) 0.2468(3) 0.0893(17) Uani 1 1 d . . . C44 C 0.9315(14) 0.0927(7) 0.1768(6) 0.193(9) Uani 1 1 d . . . H44A H 0.9520 0.0938 0.1300 0.232 Uiso 1 1 calc R . . H44B H 0.9398 0.0324 0.1942 0.232 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 O3 0.0292(19) 0.0353(19) 0.0284(19) 0.0035(19) 0.0066(15) 0.000(2) Zr1 0.0268(2) 0.0263(2) 0.0257(2) 0.0016(2) 0.0031(2) 0.0062(3) P1 0.0264(7) 0.0223(6) 0.0283(7) -0.0009(7) -0.0007(7) -0.0006(6) P2 0.0313(8) 0.0357(8) 0.0269(8) -0.0044(6) 0.0014(7) -0.0005(7) Cl1 0.0724(11) 0.0276(7) 0.0456(9) -0.0025(6) 0.0055(9) 0.0131(8) C40 0.069(5) 0.067(5) 0.043(4) 0.019(3) 0.036(4) 0.030(4) O2 0.0264(18) 0.0234(17) 0.0284(17) -0.0015(16) 0.0013(14) 0.0046(18) F2 0.0302(18) 0.053(2) 0.054(2) 0.0033(16) 0.0063(16) -0.0012(16) O4 0.030(2) 0.039(2) 0.0206(19) -0.0001(15) 0.0019(16) -0.0030(16) O1 0.021(2) 0.0266(18) 0.048(2) -0.0076(17) -0.0022(18) 0.0013(16) C25 0.036(3) 0.037(3) 0.030(3) 0.001(3) -0.002(3) -0.009(3) F1 0.035(2) 0.0359(17) 0.079(2) -0.0144(16) -0.0135(18) -0.0048(16) C8 0.042(3) 0.034(3) 0.049(3) 0.001(3) 0.005(3) -0.007(3) C19 0.028(3) 0.028(3) 0.039(3) -0.008(3) 0.000(3) -0.004(3) C6 0.025(3) 0.024(3) 0.026(3) 0.001(2) 0.002(2) 0.007(2) C1 0.027(3) 0.027(3) 0.025(3) 0.002(2) 0.003(2) 0.002(2) C13 0.030(3) 0.027(3) 0.031(3) -0.007(2) 0.001(3) 0.010(3) C31 0.036(3) 0.039(3) 0.023(3) -0.006(3) 0.007(3) -0.003(3) C14 0.040(4) 0.042(3) 0.043(3) -0.006(3) -0.009(3) 0.007(3) C4 0.042(4) 0.035(3) 0.045(4) -0.011(3) 0.000(3) 0.016(3) C32 0.043(4) 0.055(4) 0.066(5) -0.022(4) -0.010(4) -0.007(3) C20 0.036(4) 0.038(3) 0.033(3) -0.003(3) 0.008(3) -0.005(3) C30 0.042(4) 0.052(4) 0.036(4) -0.001(3) 0.006(3) -0.014(3) C9 0.048(4) 0.049(4) 0.055(4) 0.003(3) 0.026(4) -0.012(4) C3 0.046(4) 0.016(3) 0.052(4) -0.008(3) -0.005(3) 0.005(3) C24 0.031(3) 0.039(3) 0.030(3) -0.010(2) -0.002(3) -0.002(3) C37 0.063(5) 0.065(4) 0.040(4) 0.006(3) 0.017(4) -0.025(4) C26 0.112(7) 0.057(5) 0.034(4) -0.004(3) 0.009(4) -0.010(5) C5 0.032(4) 0.028(3) 0.043(4) -0.004(3) -0.004(3) 0.002(3) C2 0.033(4) 0.022(3) 0.049(4) -0.003(3) -0.005(3) -0.004(3) C17 0.053(5) 0.054(4) 0.040(4) 0.011(3) 0.005(3) 0.025(4) C38 0.055(5) 0.046(4) 0.048(4) 0.026(3) 0.014(4) 0.005(3) C16 0.047(5) 0.074(5) 0.045(4) -0.015(3) -0.012(4) 0.031(4) C33 0.059(5) 0.061(5) 0.082(6) -0.027(4) 0.019(4) 0.009(4) C22 0.040(4) 0.066(4) 0.035(4) 0.008(3) -0.012(3) -0.002(3) C10 0.060(5) 0.044(4) 0.063(4) 0.014(3) 0.014(4) -0.018(4) C35 0.073(5) 0.053(4) 0.060(4) -0.017(3) 0.017(4) -0.018(4) C41 0.036(4) 0.101(7) 0.038(4) 0.025(4) 0.011(3) 0.001(4) C15 0.028(4) 0.070(4) 0.058(4) -0.014(4) -0.009(3) 0.000(3) C21 0.031(4) 0.057(4) 0.049(4) 0.004(3) -0.013(3) -0.002(3) C29 0.059(5) 0.069(5) 0.041(4) 0.012(3) -0.003(4) -0.023(4) C34 0.085(6) 0.045(4) 0.059(5) -0.018(3) 0.035(5) -0.004(4) C12 0.057(5) 0.034(3) 0.050(4) 0.003(3) 0.011(4) -0.002(3) C23 0.046(4) 0.052(4) 0.031(4) 0.003(3) -0.007(3) -0.001(3) C36 0.051(4) 0.042(3) 0.046(4) -0.010(3) 0.012(3) -0.012(3) C28 0.093(6) 0.054(4) 0.067(5) 0.015(4) 0.004(5) -0.036(4) C27 0.175(9) 0.050(4) 0.063(5) -0.008(5) -0.007(7) -0.038(5) C42 0.140(11) 0.053(5) 0.121(9) 0.027(5) 0.019(7) -0.002(6) C43 0.257(18) 0.135(11) 0.064(7) 0.000(7) -0.017(10) -0.115(11) C39 0.052(4) 0.066(5) 0.026(3) 0.008(3) 0.006(3) -0.009(4) C18 0.041(4) 0.046(4) 0.041(4) 0.000(3) 0.001(3) 0.012(3) C11 0.072(5) 0.028(3) 0.091(6) 0.002(4) 0.013(5) -0.008(4) C45 0.135(10) 0.060(6) 0.191(12) -0.023(7) 0.015(9) 0.044(6) C7 0.025(3) 0.025(3) 0.032(3) 0.001(2) -0.005(2) -0.001(2) O5 0.096(5) 0.059(3) 0.113(5) -0.016(3) -0.016(4) -0.001(3) C44 0.42(3) 0.048(6) 0.116(10) -0.005(6) 0.115(14) 0.008(10) _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 O3 C19 1.269(6) . ? O3 Zr1 2.088(3) . ? Zr1 O1 2.076(3) . ? Zr1 O2 2.173(3) . ? Zr1 O4 2.198(3) . ? Zr1 C37 2.507(6) . ? Zr1 Cl1 2.5180(13) . ? Zr1 C38 2.520(5) . ? Zr1 C41 2.548(6) . ? Zr1 C39 2.552(5) . ? Zr1 C40 2.580(5) . ? P1 O2 1.517(3) . ? P1 C6 1.780(5) . ? P1 C7 1.791(5) . ? P1 C13 1.810(5) . ? P2 O4 1.510(3) . ? P2 C25 1.794(5) . ? P2 C24 1.795(6) . ? P2 C31 1.797(5) . ? C40 C41 1.357(9) . ? C40 C39 1.384(8) . ? C40 H40A 1.0000 . ? F2 C20 1.361(6) . ? O1 C1 1.317(6) . ? C25 C26 1.347(7) . ? C25 C30 1.389(8) . ? F1 C2 1.353(6) . ? C8 C9 1.378(7) . ? C8 C7 1.385(7) . ? C8 H8A 0.9500 . ? C19 C24 1.416(7) . ? C19 C20 1.418(7) . ? C6 C1 1.410(7) . ? C6 C5 1.413(7) . ? C1 C2 1.407(7) . ? C13 C18 1.383(7) . ? C13 C14 1.386(7) . ? C31 C32 1.355(7) . ? C31 C36 1.380(7) . ? C14 C15 1.389(7) . ? C14 H14A 0.9500 . ? C4 C5 1.381(7) . ? C4 C3 1.384(7) . ? C4 H4A 0.9500 . ? C32 C33 1.390(8) . ? C32 H32A 0.9500 . ? C20 C21 1.382(7) . ? C30 C29 1.363(8) . ? C30 H30A 0.9500 . ? C9 C10 1.368(8) . ? C9 H9A 0.9500 . ? C3 C2 1.366(7) . ? C3 H3A 0.9500 . ? C24 C23 1.393(7) . ? C37 C41 1.374(9) . ? C37 C38 1.380(9) . ? C37 H37A 1.0000 . ? C26 C27 1.391(9) . ? C26 H26A 0.9500 . ? C5 H5A 0.9500 . ? C17 C16 1.354(9) . ? C17 C18 1.392(8) . ? C17 H17A 0.9500 . ? C38 C39 1.362(8) . ? C38 H38A 1.0000 . ? C16 C15 1.365(8) . ? C16 H16A 0.9500 . ? C33 C34 1.355(9) . ? C33 H33A 0.9500 . ? C22 C21 1.360(8) . ? C22 C23 1.386(8) . ? C22 H22A 0.9500 . ? C10 C11 1.349(9) . ? C10 H10A 0.9500 . ? C35 C34 1.347(9) . ? C35 C36 1.378(8) . ? C35 H35A 0.9500 . ? C41 H41A 1.0000 . ? C15 H15A 0.9500 . ? C21 H21A 0.9500 . ? C29 C28 1.354(9) . ? C29 H29A 0.9500 . ? C34 H34A 0.9500 . ? C12 C7 1.362(7) . ? C12 C11 1.395(8) . ? C12 H12A 0.9500 . ? C23 H23A 0.9500 . ? C36 H36A 0.9500 . ? C28 C27 1.334(10) . ? C28 H28A 0.9500 . ? C27 H27A 0.9500 . ? C42 O5 1.374(10) . ? C42 C43 1.475(13) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.442(17) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C39 H39A 1.0000 . ? C18 H18A 0.9500 . ? C11 H11A 0.9500 . ? C45 O5 1.398(9) . ? C45 C44 1.493(16) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? 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 C19 O3 Zr1 139.5(3) . . ? O1 Zr1 O3 90.55(14) . . ? O1 Zr1 O2 81.30(13) . . ? O3 Zr1 O2 158.60(11) . . ? O1 Zr1 O4 79.40(13) . . ? O3 Zr1 O4 80.08(12) . . ? O2 Zr1 O4 78.98(12) . . ? O1 Zr1 C37 78.1(2) . . ? O3 Zr1 C37 84.78(19) . . ? O2 Zr1 C37 112.5(2) . . ? O4 Zr1 C37 152.68(18) . . ? O1 Zr1 Cl1 156.24(11) . . ? O3 Zr1 Cl1 93.70(11) . . ? O2 Zr1 Cl1 86.40(9) . . ? O4 Zr1 Cl1 78.34(9) . . ? C37 Zr1 Cl1 125.53(17) . . ? O1 Zr1 C38 78.97(18) . . ? O3 Zr1 C38 116.65(19) . . ? O2 Zr1 C38 81.34(18) . . ? O4 Zr1 C38 152.63(17) . . ? C37 Zr1 C38 31.9(2) . . ? Cl1 Zr1 C38 119.25(16) . . ? O1 Zr1 C41 107.4(2) . . ? O3 Zr1 C41 73.27(17) . . ? O2 Zr1 C41 128.03(18) . . ? O4 Zr1 C41 152.44(17) . . ? C37 Zr1 C41 31.5(2) . . ? Cl1 Zr1 C41 96.24(19) . . ? C38 Zr1 C41 52.3(2) . . ? O1 Zr1 C39 108.40(17) . . ? O3 Zr1 C39 124.96(17) . . ? O2 Zr1 C39 76.44(17) . . ? O4 Zr1 C39 152.59(17) . . ? C37 Zr1 C39 52.0(2) . . ? Cl1 Zr1 C39 88.14(14) . . ? C38 Zr1 C39 31.14(18) . . ? C41 Zr1 C39 51.9(2) . . ? O1 Zr1 C40 127.50(18) . . ? O3 Zr1 C40 96.8(2) . . ? O2 Zr1 C40 103.9(2) . . ? O4 Zr1 C40 153.08(17) . . ? C37 Zr1 C40 51.2(2) . . ? Cl1 Zr1 C40 75.17(16) . . ? C38 Zr1 C40 51.4(2) . . ? C41 Zr1 C40 30.69(19) . . ? C39 Zr1 C40 31.28(18) . . ? O2 P1 C6 111.4(2) . . ? O2 P1 C7 111.6(2) . . ? C6 P1 C7 111.4(2) . . ? O2 P1 C13 109.6(2) . . ? C6 P1 C13 106.2(2) . . ? C7 P1 C13 106.5(2) . . ? O4 P2 C25 110.4(2) . . ? O4 P2 C24 112.4(2) . . ? C25 P2 C24 106.0(3) . . ? O4 P2 C31 110.3(2) . . ? C25 P2 C31 108.0(2) . . ? C24 P2 C31 109.5(2) . . ? C41 C40 C39 109.0(6) . . ? C41 C40 Zr1 73.4(4) . . ? C39 C40 Zr1 73.3(3) . . ? C41 C40 H40A 125.3 . . ? C39 C40 H40A 125.3 . . ? Zr1 C40 H40A 125.3 . . ? P1 O2 Zr1 131.66(18) . . ? P2 O4 Zr1 132.2(2) . . ? C1 O1 Zr1 141.5(3) . . ? C26 C25 C30 119.6(5) . . ? C26 C25 P2 119.5(5) . . ? C30 C25 P2 120.7(4) . . ? C9 C8 C7 120.6(5) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? O3 C19 C24 125.9(5) . . ? O3 C19 C20 120.2(5) . . ? C24 C19 C20 114.0(5) . . ? C1 C6 C5 120.4(4) . . ? C1 C6 P1 121.4(4) . . ? C5 C6 P1 118.2(4) . . ? O1 C1 C2 120.1(5) . . ? O1 C1 C6 124.8(4) . . ? C2 C1 C6 115.1(5) . . ? C18 C13 C14 119.4(5) . . ? C18 C13 P1 117.5(4) . . ? C14 C13 P1 123.1(4) . . ? C32 C31 C36 118.8(5) . . ? C32 C31 P2 119.1(4) . . ? C36 C31 P2 121.9(4) . . ? C13 C14 C15 119.9(6) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C5 C4 C3 119.1(5) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C31 C32 C33 120.8(6) . . ? C31 C32 H32A 119.6 . . ? C33 C32 H32A 119.6 . . ? F2 C20 C21 119.6(5) . . ? F2 C20 C19 116.9(5) . . ? C21 C20 C19 123.5(5) . . ? C29 C30 C25 119.5(6) . . ? C29 C30 H30A 120.3 . . ? C25 C30 H30A 120.3 . . ? C10 C9 C8 119.8(6) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C2 C3 C4 119.2(5) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C23 C24 C19 122.1(5) . . ? C23 C24 P2 121.7(4) . . ? C19 C24 P2 116.2(4) . . ? C41 C37 C38 108.4(6) . . ? C41 C37 Zr1 75.9(4) . . ? C38 C37 Zr1 74.6(3) . . ? C41 C37 H37A 125.3 . . ? C38 C37 H37A 125.3 . . ? Zr1 C37 H37A 125.3 . . ? C25 C26 C27 119.3(6) . . ? C25 C26 H26A 120.4 . . ? C27 C26 H26A 120.4 . . ? C4 C5 C6 121.3(5) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? F1 C2 C3 118.8(5) . . ? F1 C2 C1 116.4(5) . . ? C3 C2 C1 124.7(5) . . ? C16 C17 C18 120.5(6) . . ? C16 C17 H17A 119.7 . . ? C18 C17 H17A 119.7 . . ? C39 C38 C37 107.9(6) . . ? C39 C38 Zr1 75.7(3) . . ? C37 C38 Zr1 73.6(3) . . ? C39 C38 H38A 125.6 . . ? C37 C38 H38A 125.6 . . ? Zr1 C38 H38A 125.6 . . ? C17 C16 C15 120.6(6) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C34 C33 C32 118.8(7) . . ? C34 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C21 C22 C23 118.9(6) . . ? C21 C22 H22A 120.5 . . ? C23 C22 H22A 120.5 . . ? C11 C10 C9 120.0(6) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C34 C35 C36 119.1(7) . . ? C34 C35 H35A 120.5 . . ? C36 C35 H35A 120.5 . . ? C40 C41 C37 107.3(6) . . ? C40 C41 Zr1 75.9(4) . . ? C37 C41 Zr1 72.6(4) . . ? C40 C41 H41A 125.9 . . ? C37 C41 H41A 125.9 . . ? Zr1 C41 H41A 125.9 . . ? C16 C15 C14 120.0(6) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C22 C21 C20 120.6(6) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C28 C29 C30 120.6(6) . . ? C28 C29 H29A 119.7 . . ? C30 C29 H29A 119.7 . . ? C35 C34 C33 121.8(6) . . ? C35 C34 H34A 119.1 . . ? C33 C34 H34A 119.1 . . ? C7 C12 C11 119.7(6) . . ? C7 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C22 C23 C24 120.9(6) . . ? C22 C23 H23A 119.5 . . ? C24 C23 H23A 119.5 . . ? C35 C36 C31 120.7(6) . . ? C35 C36 H36A 119.6 . . ? C31 C36 H36A 119.6 . . ? C27 C28 C29 120.0(6) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C28 C27 C26 121.0(7) . . ? C28 C27 H27A 119.5 . . ? C26 C27 H27A 119.5 . . ? O5 C42 C43 102.2(9) . . ? O5 C42 H42A 111.3 . . ? C43 C42 H42A 111.3 . . ? O5 C42 H42B 111.3 . . ? C43 C42 H42B 111.3 . . ? H42A C42 H42B 109.2 . . ? C44 C43 C42 107.4(12) . . ? C44 C43 H43A 110.2 . . ? C42 C43 H43A 110.2 . . ? C44 C43 H43B 110.2 . . ? C42 C43 H43B 110.2 . . ? H43A C43 H43B 108.5 . . ? C38 C39 C40 107.4(6) . . ? C38 C39 Zr1 73.1(3) . . ? C40 C39 Zr1 75.5(3) . . ? C38 C39 H39A 125.8 . . ? C40 C39 H39A 125.8 . . ? Zr1 C39 H39A 125.8 . . ? C13 C18 C17 119.6(6) . . ? C13 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C10 C11 C12 120.9(6) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? O5 C45 C44 109.1(10) . . ? O5 C45 H45A 109.9 . . ? C44 C45 H45A 109.9 . . ? O5 C45 H45B 109.9 . . ? C44 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? C12 C7 C8 119.1(5) . . ? C12 C7 P1 118.6(4) . . ? C8 C7 P1 122.2(4) . . ? C42 O5 C45 107.6(7) . . ? C43 C44 C45 100.5(9) . . ? C43 C44 H44A 111.7 . . ? C45 C44 H44A 111.7 . . ? C43 C44 H44B 111.7 . . ? C45 C44 H44B 111.7 . . ? H44A C44 H44B 109.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.562 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.071 data_u080 _database_code_depnum_ccdc_archive 'CCDC 888634' #TrackingRef '12209_web_deposit_cif_file_1_Jing-YuLiu_1340755455.2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H49 Cl O4 P2 Zr' _chemical_formula_weight 890.49 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' P P 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3191(6) _cell_length_b 12.4318(7) _cell_length_c 17.7473(10) _cell_angle_alpha 73.0780(10) _cell_angle_beta 80.5820(10) _cell_angle_gamma 63.6480(10) _cell_volume 2139.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 2460 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 23.98 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8907 _exptl_absorpt_correction_T_max 0.9616 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11172 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.04 _reflns_number_total 8233 _reflns_number_gt 5867 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0847P)^2^+1.7524P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8233 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1643 _refine_ls_wR_factor_gt 0.1467 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.70077(4) 0.65391(4) 0.67782(3) 0.02919(15) Uani 1 1 d . . . Cl1 Cl 0.45644(12) 0.73966(13) 0.71175(8) 0.0505(4) Uani 1 1 d . . . O1 O 0.8931(3) 0.6325(3) 0.66794(18) 0.0311(7) Uani 1 1 d . . . O2 O 0.6676(3) 0.8360(3) 0.60444(17) 0.0306(7) Uani 1 1 d . . . O3 O 0.7279(3) 0.5222(3) 0.78576(19) 0.0342(7) Uani 1 1 d . . . O4 O 0.6928(3) 0.7633(3) 0.75860(18) 0.0353(7) Uani 1 1 d . . . P1 P 0.76236(11) 0.89699(10) 0.57566(7) 0.0273(3) Uani 1 1 d . . . P2 P 0.68058(13) 0.74643(12) 0.84534(7) 0.0358(3) Uani 1 1 d . . . C37 C 0.8239(6) 0.4940(6) 0.5948(4) 0.0571(15) Uani 1 1 d . . . H37A H 0.9189 0.4341 0.5991 0.069 Uiso 1 1 calc R . . C38 C 0.7225(6) 0.4692(5) 0.6307(3) 0.0479(13) Uani 1 1 d . . . H38A H 0.7308 0.3875 0.6663 0.058 Uiso 1 1 calc R . . C39 C 0.6048(6) 0.5655(6) 0.6015(4) 0.0597(16) Uani 1 1 d . . . H39A H 0.5157 0.5646 0.6106 0.072 Uiso 1 1 calc R . . C40 C 0.6397(7) 0.6530(6) 0.5454(4) 0.0617(17) Uani 1 1 d . . . H40A H 0.5790 0.7267 0.5074 0.074 Uiso 1 1 calc R . . C41 C 0.7755(8) 0.6062(6) 0.5411(4) 0.0648(18) Uani 1 1 d . . . H41A H 0.8294 0.6414 0.5001 0.078 Uiso 1 1 calc R . . C1 C 0.9618(4) 0.6970(4) 0.6659(2) 0.0283(10) Uani 1 1 d . . . C2 C 1.0881(4) 0.6377(4) 0.7007(3) 0.0302(10) Uani 1 1 d . . . C3 C 1.1530(5) 0.7112(5) 0.6953(3) 0.0381(11) Uani 1 1 d . . . H3A H 1.2370 0.6736 0.7178 0.046 Uiso 1 1 calc R . . C4 C 1.1031(5) 0.8354(5) 0.6591(3) 0.0390(12) Uani 1 1 d . . . H4A H 1.1519 0.8816 0.6575 0.047 Uiso 1 1 calc R . . C5 C 0.9817(5) 0.8932(5) 0.6251(3) 0.0373(11) Uani 1 1 d . . . H5A H 0.9468 0.9790 0.5996 0.045 Uiso 1 1 calc R . . C6 C 0.9112(4) 0.8237(4) 0.6286(2) 0.0287(10) Uani 1 1 d . . . C42 C 1.1478(5) 0.4984(5) 0.7396(3) 0.0386(11) Uani 1 1 d . . . C44 C 1.0591(5) 0.4678(5) 0.8104(3) 0.0506(14) Uani 1 1 d . . . H44A H 0.9713 0.4928 0.7923 0.076 Uiso 1 1 calc R . . H44B H 1.0516 0.5127 0.8494 0.076 Uiso 1 1 calc R . . H44C H 1.0981 0.3785 0.8345 0.076 Uiso 1 1 calc R . . C43 C 1.2832(5) 0.4564(5) 0.7723(4) 0.0542(15) Uani 1 1 d . . . H43A H 1.3435 0.4735 0.7292 0.081 Uiso 1 1 calc R . . H43B H 1.3190 0.3674 0.7971 0.081 Uiso 1 1 calc R . . H43C H 1.2733 0.5017 0.8116 0.081 Uiso 1 1 calc R . . C45 C 1.1663(6) 0.4246(5) 0.6796(4) 0.0611(17) Uani 1 1 d . . . H45A H 1.0809 0.4496 0.6582 0.092 Uiso 1 1 calc R . . H45B H 1.2027 0.3359 0.7055 0.092 Uiso 1 1 calc R . . H45C H 1.2273 0.4411 0.6366 0.092 Uiso 1 1 calc R . . C13 C 0.8080(4) 0.8962(4) 0.4740(3) 0.0290(10) Uani 1 1 d . . . C18 C 0.9389(5) 0.8383(4) 0.4483(3) 0.0378(11) Uani 1 1 d . . . H18A H 1.0076 0.8039 0.4842 0.045 Uiso 1 1 calc R . . C17 C 0.9691(5) 0.8308(5) 0.3709(3) 0.0445(13) Uani 1 1 d . . . H17A H 1.0584 0.7935 0.3530 0.053 Uiso 1 1 calc R . . C16 C 0.8681(5) 0.8780(5) 0.3194(3) 0.0450(13) Uani 1 1 d . . . H16A H 0.8888 0.8693 0.2668 0.054 Uiso 1 1 calc R . . C15 C 0.7388(5) 0.9370(5) 0.3429(3) 0.0432(12) Uani 1 1 d . . . H15A H 0.6709 0.9714 0.3064 0.052 Uiso 1 1 calc R . . C14 C 0.7077(5) 0.9462(4) 0.4206(3) 0.0346(11) Uani 1 1 d . . . H14A H 0.6183 0.9865 0.4374 0.042 Uiso 1 1 calc R . . C7 C 0.6807(4) 1.0544(4) 0.5841(3) 0.0305(10) Uani 1 1 d . . . C12 C 0.7112(5) 1.1480(4) 0.5338(3) 0.0400(12) Uani 1 1 d . . . H12A H 0.7716 1.1330 0.4901 0.048 Uiso 1 1 calc R . . C11 C 0.6498(6) 1.2658(5) 0.5495(4) 0.0529(15) Uani 1 1 d . . . H11A H 0.6693 1.3315 0.5161 0.064 Uiso 1 1 calc R . . C10 C 0.5622(6) 1.2868(5) 0.6123(4) 0.0554(15) Uani 1 1 d . . . H10A H 0.5216 1.3669 0.6223 0.066 Uiso 1 1 calc R . . C9 C 0.5327(6) 1.1931(6) 0.6608(4) 0.0551(15) Uani 1 1 d . . . H9A H 0.4707 1.2086 0.7038 0.066 Uiso 1 1 calc R . . C8 C 0.5930(5) 1.0763(5) 0.6474(3) 0.0419(12) Uani 1 1 d . . . H8A H 0.5739 1.0110 0.6817 0.050 Uiso 1 1 calc R . . C19 C 0.7052(4) 0.5086(4) 0.8588(3) 0.0298(10) Uani 1 1 d . . . C20 C 0.7064(5) 0.3916(4) 0.9088(3) 0.0343(11) Uani 1 1 d . . . C21 C 0.6778(5) 0.3803(5) 0.9895(3) 0.0431(12) Uani 1 1 d . . . H21A H 0.6789 0.3039 1.0214 0.052 Uiso 1 1 calc R . . C22 C 0.6478(5) 0.4754(5) 1.0257(3) 0.0471(13) Uani 1 1 d . . . H22A H 0.6297 0.4633 1.0810 0.056 Uiso 1 1 calc R . . C23 C 0.6446(5) 0.5872(5) 0.9803(3) 0.0435(12) Uani 1 1 d . . . H23A H 0.6229 0.6532 1.0041 0.052 Uiso 1 1 calc R . . C24 C 0.6736(5) 0.6036(4) 0.8984(3) 0.0380(11) Uani 1 1 d . . . C46 C 0.7338(5) 0.2846(5) 0.8724(3) 0.0393(11) Uani 1 1 d . . . C47 C 0.6196(6) 0.3243(5) 0.8198(3) 0.0505(14) Uani 1 1 d . . . H47A H 0.5365 0.3456 0.8512 0.076 Uiso 1 1 calc R . . H47B H 0.6340 0.2560 0.7972 0.076 Uiso 1 1 calc R . . H47C H 0.6153 0.3966 0.7771 0.076 Uiso 1 1 calc R . . C48 C 0.8671(5) 0.2494(5) 0.8249(3) 0.0505(14) Uani 1 1 d . . . H48A H 0.9384 0.2237 0.8600 0.076 Uiso 1 1 calc R . . H48B H 0.8650 0.3212 0.7825 0.076 Uiso 1 1 calc R . . H48C H 0.8824 0.1810 0.8023 0.076 Uiso 1 1 calc R . . C49 C 0.7414(6) 0.1675(5) 0.9332(3) 0.0544(15) Uani 1 1 d . . . H49A H 0.6584 0.1850 0.9648 0.082 Uiso 1 1 calc R . . H49B H 0.8145 0.1381 0.9677 0.082 Uiso 1 1 calc R . . H49C H 0.7561 0.1036 0.9065 0.082 Uiso 1 1 calc R . . C25 C 0.5327(5) 0.8735(5) 0.8703(3) 0.0439(12) Uani 1 1 d . . . C26 C 0.4109(6) 0.8787(6) 0.8613(3) 0.0537(14) Uani 1 1 d . . . H26A H 0.4055 0.8126 0.8476 0.064 Uiso 1 1 calc R . . C27 C 0.2976(6) 0.9801(6) 0.8722(3) 0.0636(17) Uani 1 1 d . . . H27A H 0.2144 0.9841 0.8648 0.076 Uiso 1 1 calc R . . C28 C 0.3022(8) 1.0764(6) 0.8939(4) 0.076(2) Uani 1 1 d . . . H28A H 0.2231 1.1450 0.9021 0.092 Uiso 1 1 calc R . . C29 C 0.4218(9) 1.0715(7) 0.9033(5) 0.091(3) Uani 1 1 d . . . H29A H 0.4260 1.1367 0.9187 0.110 Uiso 1 1 calc R . . C30 C 0.5387(7) 0.9706(6) 0.8904(5) 0.080(2) Uani 1 1 d . . . H30A H 0.6218 0.9689 0.8955 0.096 Uiso 1 1 calc R . . C31 C 0.8180(5) 0.7570(5) 0.8780(3) 0.0379(11) Uani 1 1 d . . . C32 C 0.8775(6) 0.6884(6) 0.9473(3) 0.0532(14) Uani 1 1 d . . . H32A H 0.8480 0.6301 0.9819 0.064 Uiso 1 1 calc R . . C33 C 0.9821(6) 0.7040(6) 0.9674(4) 0.0663(18) Uani 1 1 d . . . H33A H 1.0255 0.6554 1.0153 0.080 Uiso 1 1 calc R . . C34 C 1.0221(6) 0.7913(6) 0.9167(4) 0.0666(18) Uani 1 1 d . . . H34A H 1.0917 0.8038 0.9309 0.080 Uiso 1 1 calc R . . C35 C 0.9628(6) 0.8598(6) 0.8466(4) 0.0592(16) Uani 1 1 d . . . H35A H 0.9922 0.9180 0.8118 0.071 Uiso 1 1 calc R . . C36 C 0.8605(6) 0.8433(5) 0.8271(3) 0.0493(14) Uani 1 1 d . . . H36A H 0.8184 0.8910 0.7787 0.059 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 0.0277(3) 0.0290(2) 0.0330(3) -0.00071(18) -0.00614(18) -0.01632(19) Cl1 0.0302(7) 0.0546(8) 0.0647(9) -0.0090(7) -0.0007(6) -0.0200(6) O1 0.0250(16) 0.0287(16) 0.0410(18) -0.0057(14) -0.0080(13) -0.0120(14) O2 0.0257(16) 0.0315(17) 0.0344(17) -0.0011(13) -0.0053(13) -0.0147(14) O3 0.0319(18) 0.0291(17) 0.0420(19) -0.0084(14) -0.0001(14) -0.0140(14) O4 0.0406(19) 0.0330(18) 0.0321(17) 0.0000(14) -0.0033(14) -0.0195(15) P1 0.0266(6) 0.0270(6) 0.0283(6) -0.0011(5) -0.0034(5) -0.0139(5) P2 0.0416(8) 0.0341(7) 0.0342(7) -0.0093(5) -0.0014(5) -0.0174(6) C37 0.066(4) 0.052(4) 0.065(4) -0.027(3) -0.004(3) -0.026(3) C38 0.057(4) 0.053(3) 0.043(3) -0.021(3) -0.005(3) -0.024(3) C39 0.051(4) 0.069(4) 0.080(4) -0.030(4) -0.006(3) -0.035(3) C40 0.090(5) 0.050(4) 0.052(4) -0.002(3) -0.036(3) -0.031(4) C41 0.103(6) 0.068(4) 0.049(4) -0.025(3) 0.013(4) -0.057(4) C1 0.026(2) 0.037(3) 0.026(2) -0.0100(19) 0.0033(18) -0.016(2) C2 0.025(2) 0.037(3) 0.032(2) -0.012(2) -0.0007(19) -0.014(2) C3 0.024(2) 0.051(3) 0.041(3) -0.010(2) -0.005(2) -0.017(2) C4 0.035(3) 0.045(3) 0.047(3) -0.008(2) -0.003(2) -0.027(2) C5 0.037(3) 0.037(3) 0.042(3) 0.000(2) -0.006(2) -0.024(2) C6 0.026(2) 0.034(2) 0.028(2) -0.0012(19) -0.0055(18) -0.016(2) C42 0.026(3) 0.039(3) 0.046(3) -0.011(2) -0.009(2) -0.007(2) C44 0.042(3) 0.043(3) 0.053(3) 0.009(3) -0.013(3) -0.014(3) C43 0.036(3) 0.044(3) 0.077(4) -0.015(3) -0.021(3) -0.005(3) C45 0.045(3) 0.049(3) 0.089(5) -0.036(3) -0.019(3) -0.002(3) C13 0.032(3) 0.025(2) 0.032(2) -0.0060(19) -0.0010(19) -0.015(2) C18 0.031(3) 0.032(3) 0.045(3) -0.007(2) -0.003(2) -0.009(2) C17 0.036(3) 0.042(3) 0.045(3) -0.011(2) 0.011(2) -0.012(2) C16 0.055(4) 0.042(3) 0.037(3) -0.016(2) 0.008(2) -0.020(3) C15 0.048(3) 0.049(3) 0.036(3) -0.006(2) -0.006(2) -0.024(3) C14 0.028(3) 0.037(3) 0.036(3) -0.008(2) 0.001(2) -0.013(2) C7 0.029(2) 0.030(2) 0.035(2) -0.0071(19) -0.0054(19) -0.013(2) C12 0.041(3) 0.032(3) 0.045(3) -0.006(2) -0.004(2) -0.015(2) C11 0.058(4) 0.037(3) 0.070(4) -0.003(3) -0.020(3) -0.025(3) C10 0.047(3) 0.049(3) 0.076(4) -0.039(3) -0.009(3) -0.009(3) C9 0.045(3) 0.059(4) 0.062(4) -0.029(3) 0.002(3) -0.016(3) C8 0.034(3) 0.048(3) 0.045(3) -0.016(2) 0.002(2) -0.017(2) C19 0.024(2) 0.022(2) 0.040(3) -0.0042(19) -0.013(2) -0.0049(18) C20 0.033(3) 0.035(3) 0.036(3) -0.006(2) -0.004(2) -0.017(2) C21 0.050(3) 0.040(3) 0.038(3) -0.001(2) -0.002(2) -0.023(3) C22 0.054(3) 0.055(3) 0.031(3) -0.006(2) 0.001(2) -0.026(3) C23 0.049(3) 0.043(3) 0.037(3) -0.009(2) 0.001(2) -0.019(3) C24 0.044(3) 0.036(3) 0.034(3) -0.005(2) 0.003(2) -0.020(2) C46 0.042(3) 0.035(3) 0.038(3) -0.005(2) -0.002(2) -0.017(2) C47 0.055(4) 0.057(4) 0.049(3) -0.013(3) -0.003(3) -0.032(3) C48 0.047(3) 0.041(3) 0.057(3) -0.012(3) 0.007(3) -0.015(3) C49 0.069(4) 0.039(3) 0.053(3) -0.007(3) 0.004(3) -0.025(3) C25 0.055(3) 0.039(3) 0.035(3) -0.009(2) 0.004(2) -0.018(3) C26 0.051(4) 0.061(4) 0.038(3) -0.007(3) -0.002(3) -0.017(3) C27 0.056(4) 0.064(4) 0.041(3) -0.005(3) -0.001(3) -0.004(3) C28 0.078(5) 0.044(4) 0.064(4) -0.006(3) 0.012(4) 0.003(4) C29 0.088(6) 0.054(4) 0.130(7) -0.041(5) 0.005(5) -0.019(4) C30 0.063(5) 0.065(4) 0.118(6) -0.048(4) 0.015(4) -0.023(4) C31 0.038(3) 0.038(3) 0.043(3) -0.017(2) -0.001(2) -0.017(2) C32 0.059(4) 0.061(4) 0.048(3) -0.010(3) -0.008(3) -0.032(3) C33 0.066(4) 0.076(5) 0.066(4) -0.014(4) -0.021(3) -0.033(4) C34 0.062(4) 0.079(5) 0.077(5) -0.024(4) -0.014(4) -0.039(4) C35 0.066(4) 0.067(4) 0.062(4) -0.024(3) 0.003(3) -0.039(4) C36 0.062(4) 0.055(3) 0.044(3) -0.015(3) 0.000(3) -0.034(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 O1 2.056(3) . ? Zr1 O3 2.090(3) . ? Zr1 O2 2.157(3) . ? Zr1 O4 2.212(3) . ? Zr1 Cl1 2.5216(13) . ? Zr1 C40 2.559(6) . ? Zr1 C38 2.565(5) . ? Zr1 C39 2.576(5) . ? Zr1 C37 2.577(6) . ? Zr1 C41 2.583(6) . ? O1 C1 1.332(5) . ? O2 P1 1.518(3) . ? O3 C19 1.256(5) . ? O4 P2 1.484(3) . ? P1 C6 1.791(4) . ? P1 C13 1.795(5) . ? P1 C7 1.796(5) . ? P2 C24 1.781(5) . ? P2 C31 1.814(5) . ? P2 C25 1.819(5) . ? C37 C38 1.334(8) . ? C37 C41 1.367(8) . ? C37 H37A 1.0000 . ? C38 C39 1.388(8) . ? C38 H38A 1.0000 . ? C39 C40 1.397(8) . ? C39 H39A 1.0000 . ? C40 C41 1.379(9) . ? C40 H40A 1.0000 . ? C41 H41A 1.0000 . ? C1 C6 1.401(6) . ? C1 C2 1.435(6) . ? C2 C3 1.380(6) . ? C2 C42 1.532(7) . ? C3 C4 1.372(7) . ? C3 H3A 0.9500 . ? C4 C5 1.382(6) . ? C4 H4A 0.9500 . ? C5 C6 1.398(6) . ? C5 H5A 0.9500 . ? C42 C45 1.531(7) . ? C42 C43 1.537(7) . ? C42 C44 1.543(7) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C13 C18 1.394(6) . ? C13 C14 1.399(6) . ? C18 C17 1.381(7) . ? C18 H18A 0.9500 . ? C17 C16 1.386(7) . ? C17 H17A 0.9500 . ? C16 C15 1.371(7) . ? C16 H16A 0.9500 . ? C15 C14 1.392(7) . ? C15 H15A 0.9500 . ? C14 H14A 0.9500 . ? C7 C8 1.376(7) . ? C7 C12 1.386(6) . ? C12 C11 1.405(7) . ? C12 H12A 0.9500 . ? C11 C10 1.368(8) . ? C11 H11A 0.9500 . ? C10 C9 1.371(8) . ? C10 H10A 0.9500 . ? C9 C8 1.378(7) . ? C9 H9A 0.9500 . ? C8 H8A 0.9500 . ? C19 C24 1.429(7) . ? C19 C20 1.462(6) . ? C20 C21 1.396(7) . ? C20 C46 1.533(7) . ? C21 C22 1.392(7) . ? C21 H21A 0.9500 . ? C22 C23 1.376(7) . ? C22 H22A 0.9500 . ? C23 C24 1.412(7) . ? C23 H23A 0.9500 . ? C46 C49 1.516(7) . ? C46 C47 1.532(7) . ? C46 C48 1.545(7) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C25 C26 1.385(8) . ? C25 C30 1.386(8) . ? C26 C27 1.379(8) . ? C26 H26A 0.9500 . ? C27 C28 1.383(10) . ? C27 H27A 0.9500 . ? C28 C29 1.363(10) . ? C28 H28A 0.9500 . ? C29 C30 1.404(10) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.359(7) . ? C31 C36 1.397(7) . ? C32 C33 1.397(8) . ? C32 H32A 0.9500 . ? C33 C34 1.389(9) . ? C33 H33A 0.9500 . ? C34 C35 1.368(9) . ? C34 H34A 0.9500 . ? C35 C36 1.374(8) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? 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 O1 Zr1 O3 93.23(12) . . ? O1 Zr1 O2 82.58(11) . . ? O3 Zr1 O2 153.60(12) . . ? O1 Zr1 O4 79.28(12) . . ? O3 Zr1 O4 79.27(11) . . ? O2 Zr1 O4 74.34(11) . . ? O1 Zr1 Cl1 159.60(9) . . ? O3 Zr1 Cl1 87.98(9) . . ? O2 Zr1 Cl1 87.31(8) . . ? O4 Zr1 Cl1 80.95(9) . . ? O1 Zr1 C40 108.31(19) . . ? O3 Zr1 C40 129.68(16) . . ? O2 Zr1 C40 75.85(16) . . ? O4 Zr1 C40 147.93(16) . . ? Cl1 Zr1 C40 86.13(18) . . ? O1 Zr1 C38 101.78(15) . . ? O3 Zr1 C38 80.37(15) . . ? O2 Zr1 C38 126.02(15) . . ? O4 Zr1 C38 159.63(15) . . ? Cl1 Zr1 C38 98.50(13) . . ? C40 Zr1 C38 51.41(18) . . ? O1 Zr1 C39 125.27(17) . . ? O3 Zr1 C39 99.23(17) . . ? O2 Zr1 C39 104.45(17) . . ? O4 Zr1 C39 155.37(17) . . ? Cl1 Zr1 C39 74.42(15) . . ? C40 Zr1 C39 31.58(19) . . ? C38 Zr1 C39 31.32(18) . . ? O1 Zr1 C37 74.84(16) . . ? O3 Zr1 C37 94.98(17) . . ? O2 Zr1 C37 108.85(16) . . ? O4 Zr1 C37 153.13(17) . . ? Cl1 Zr1 C37 125.38(14) . . ? C40 Zr1 C37 51.3(2) . . ? C38 Zr1 C37 30.06(17) . . ? C39 Zr1 C37 51.2(2) . . ? O1 Zr1 C41 78.25(18) . . ? O3 Zr1 C41 125.60(17) . . ? O2 Zr1 C41 79.21(17) . . ? O4 Zr1 C41 147.12(15) . . ? Cl1 Zr1 C41 117.23(17) . . ? C40 Zr1 C41 31.1(2) . . ? C38 Zr1 C41 50.40(18) . . ? C39 Zr1 C41 51.4(2) . . ? C37 Zr1 C41 30.73(19) . . ? C1 O1 Zr1 139.9(3) . . ? P1 O2 Zr1 130.13(17) . . ? C19 O3 Zr1 143.8(3) . . ? P2 O4 Zr1 135.14(18) . . ? O2 P1 C6 114.70(18) . . ? O2 P1 C13 108.87(18) . . ? C6 P1 C13 107.6(2) . . ? O2 P1 C7 108.87(19) . . ? C6 P1 C7 107.5(2) . . ? C13 P1 C7 109.1(2) . . ? O4 P2 C24 113.5(2) . . ? O4 P2 C31 109.5(2) . . ? C24 P2 C31 109.4(2) . . ? O4 P2 C25 109.2(2) . . ? C24 P2 C25 108.9(2) . . ? C31 P2 C25 106.0(2) . . ? C38 C37 C41 108.5(6) . . ? C38 C37 Zr1 74.5(3) . . ? C41 C37 Zr1 74.9(4) . . ? C38 C37 H37A 125.3 . . ? C41 C37 H37A 125.3 . . ? Zr1 C37 H37A 125.3 . . ? C37 C38 C39 109.9(6) . . ? C37 C38 Zr1 75.5(3) . . ? C39 C38 Zr1 74.8(3) . . ? C37 C38 H38A 124.7 . . ? C39 C38 H38A 124.7 . . ? Zr1 C38 H38A 124.7 . . ? C38 C39 C40 105.9(5) . . ? C38 C39 Zr1 73.9(3) . . ? C40 C39 Zr1 73.6(3) . . ? C38 C39 H39A 126.5 . . ? C40 C39 H39A 126.5 . . ? Zr1 C39 H39A 126.5 . . ? C41 C40 C39 107.5(6) . . ? C41 C40 Zr1 75.4(3) . . ? C39 C40 Zr1 74.9(3) . . ? C41 C40 H40A 125.6 . . ? C39 C40 H40A 125.6 . . ? Zr1 C40 H40A 125.6 . . ? C37 C41 C40 108.2(6) . . ? C37 C41 Zr1 74.4(3) . . ? C40 C41 Zr1 73.5(3) . . ? C37 C41 H41A 125.5 . . ? C40 C41 H41A 125.5 . . ? Zr1 C41 H41A 125.5 . . ? O1 C1 C6 119.8(4) . . ? O1 C1 C2 120.7(4) . . ? C6 C1 C2 119.5(4) . . ? C3 C2 C1 116.8(4) . . ? C3 C2 C42 122.5(4) . . ? C1 C2 C42 120.6(4) . . ? C4 C3 C2 123.7(4) . . ? C4 C3 H3A 118.2 . . ? C2 C3 H3A 118.2 . . ? C3 C4 C5 119.9(4) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 119.1(4) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C5 C6 C1 121.0(4) . . ? C5 C6 P1 118.1(3) . . ? C1 C6 P1 120.6(3) . . ? C45 C42 C2 110.4(4) . . ? C45 C42 C43 108.1(4) . . ? C2 C42 C43 111.1(4) . . ? C45 C42 C44 110.5(5) . . ? C2 C42 C44 110.3(4) . . ? C43 C42 C44 106.4(4) . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C18 C13 C14 119.3(4) . . ? C18 C13 P1 122.0(4) . . ? C14 C13 P1 118.4(3) . . ? C17 C18 C13 120.3(5) . . ? C17 C18 H18A 119.9 . . ? C13 C18 H18A 119.9 . . ? C18 C17 C16 119.5(5) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C15 C16 C17 121.2(5) . . ? C15 C16 H16A 119.4 . . ? C17 C16 H16A 119.4 . . ? C16 C15 C14 119.5(5) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? C15 C14 C13 120.0(4) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C8 C7 C12 121.0(5) . . ? C8 C7 P1 116.5(4) . . ? C12 C7 P1 122.3(4) . . ? C7 C12 C11 117.9(5) . . ? C7 C12 H12A 121.1 . . ? C11 C12 H12A 121.1 . . ? C10 C11 C12 120.7(5) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C11 C10 C9 120.3(5) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C9 C8 120.1(6) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C7 C8 C9 120.0(5) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? O3 C19 C24 124.0(4) . . ? O3 C19 C20 120.4(4) . . ? C24 C19 C20 115.6(4) . . ? C21 C20 C19 119.0(4) . . ? C21 C20 C46 120.6(4) . . ? C19 C20 C46 120.3(4) . . ? C22 C21 C20 123.3(5) . . ? C22 C21 H21A 118.3 . . ? C20 C21 H21A 118.3 . . ? C23 C22 C21 119.1(5) . . ? C23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? C22 C23 C24 120.0(5) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C19 122.8(4) . . ? C23 C24 P2 117.1(4) . . ? C19 C24 P2 119.9(3) . . ? C49 C46 C47 106.9(4) . . ? C49 C46 C20 113.2(4) . . ? C47 C46 C20 108.2(4) . . ? C49 C46 C48 106.4(4) . . ? C47 C46 C48 111.1(4) . . ? C20 C46 C48 111.0(4) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C26 C25 C30 119.4(5) . . ? C26 C25 P2 118.5(4) . . ? C30 C25 P2 121.8(5) . . ? C27 C26 C25 119.7(6) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 121.5(7) . . ? C26 C27 H27A 119.3 . . ? C28 C27 H27A 119.3 . . ? C29 C28 C27 119.1(6) . . ? C29 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? C28 C29 C30 120.4(7) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C25 C30 C29 119.9(7) . . ? C25 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C32 C31 C36 120.3(5) . . ? C32 C31 P2 124.0(4) . . ? C36 C31 P2 115.7(4) . . ? C31 C32 C33 119.7(6) . . ? C31 C32 H32A 120.1 . . ? C33 C32 H32A 120.1 . . ? C34 C33 C32 119.3(6) . . ? C34 C33 H33A 120.3 . . ? C32 C33 H33A 120.3 . . ? C35 C34 C33 121.0(6) . . ? C35 C34 H34A 119.5 . . ? C33 C34 H34A 119.5 . . ? C34 C35 C36 119.3(6) . . ? C34 C35 H35A 120.3 . . ? C36 C35 H35A 120.3 . . ? C35 C36 C31 120.4(5) . . ? C35 C36 H36A 119.8 . . ? C31 C36 H36A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.281 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.094 data_txy1 _database_code_depnum_ccdc_archive 'CCDC 888635' #TrackingRef '12210_web_deposit_cif_file_2_Jing-YuLiu_1340755455.2f.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H49 Cl O2 P2 S2 Si2 Zr' _chemical_formula_weight 954.77 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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)/n 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' _cell_length_a 10.782(2) _cell_length_b 27.167(5) _cell_length_c 18.915(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.846(3) _cell_angle_gamma 90.00 _cell_volume 5488.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8748 _exptl_absorpt_correction_T_max 0.9303 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32047 _diffrn_reflns_av_R_equivalents 0.1018 _diffrn_reflns_av_sigmaI/netI 0.1246 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.07 _reflns_number_total 9699 _reflns_number_gt 5862 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1629P)^2^+21.6259P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9699 _refine_ls_number_parameters 514 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1513 _refine_ls_R_factor_gt 0.1062 _refine_ls_wR_factor_ref 0.3065 _refine_ls_wR_factor_gt 0.2847 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _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 0.19385(7) 0.20331(3) 0.76692(5) 0.0220(3) Uani 1 1 d . . . P2 P 0.4723(2) 0.24132(9) 0.71905(14) 0.0264(6) Uani 1 1 d . . . S3 S 0.2725(2) 0.16122(9) 0.65555(13) 0.0285(6) Uani 1 1 d . . . S1 S 0.1942(2) 0.24347(10) 0.89266(13) 0.0310(6) Uani 1 1 d . . . Cl1 Cl 0.1257(2) 0.28235(10) 0.70722(14) 0.0380(6) Uani 1 1 d . . . P1 P 0.3755(2) 0.15009(10) 0.90919(14) 0.0314(6) Uani 1 1 d . . . Si1 Si 0.2949(3) 0.35336(11) 0.95242(16) 0.0377(7) Uani 1 1 d . . . Si2 Si 0.3575(3) 0.05265(12) 0.60297(19) 0.0458(8) Uani 1 1 d . . . O4 O 0.3733(5) 0.2409(2) 0.7682(3) 0.0248(14) Uani 1 1 d . . . O2 O 0.3224(6) 0.1526(2) 0.8310(3) 0.0316(16) Uani 1 1 d . . . C6 C 0.4247(9) 0.2074(4) 0.9468(6) 0.036(2) Uani 1 1 d . . . C41 C 0.0229(9) 0.1486(5) 0.7033(7) 0.052(3) Uani 1 1 d . . . H41A H 0.0250 0.1319 0.6564 0.062 Uiso 1 1 calc R . . C25 C 0.4288(8) 0.2726(4) 0.6354(5) 0.031(2) Uani 1 1 d . . . C5 C 0.5442(9) 0.2115(4) 0.9905(6) 0.042(3) Uani 1 1 d . . . H5A H 0.5970 0.1835 0.9978 0.050 Uiso 1 1 calc R . . C20 C 0.4691(9) 0.0999(4) 0.6513(6) 0.033(2) Uani 1 1 d . . . C1 C 0.3484(9) 0.2498(4) 0.9376(5) 0.030(2) Uani 1 1 d . . . C32 C 0.6990(9) 0.2910(4) 0.7217(6) 0.039(3) Uani 1 1 d . . . H32A H 0.6903 0.2864 0.6715 0.047 Uiso 1 1 calc R . . C30 C 0.3731(9) 0.3192(4) 0.6352(6) 0.037(2) Uani 1 1 d . . . H30A H 0.3525 0.3336 0.6779 0.045 Uiso 1 1 calc R . . C24 C 0.5224(7) 0.1815(4) 0.6997(5) 0.028(2) Uani 1 1 d . . . C19 C 0.4340(8) 0.1459(4) 0.6698(5) 0.030(2) Uani 1 1 d . . . C13 C 0.5109(10) 0.1108(4) 0.9177(5) 0.040(3) Uani 1 1 d . . . C7 C 0.2697(11) 0.1216(4) 0.9614(6) 0.044(3) Uani 1 1 d U . . C14 C 0.5414(11) 0.0779(4) 0.9750(6) 0.051(3) Uani 1 1 d . . . H14A H 0.4874 0.0748 1.0105 0.061 Uiso 1 1 calc R . . C26 C 0.4602(9) 0.2517(5) 0.5722(6) 0.043(3) Uani 1 1 d . . . H26A H 0.5009 0.2207 0.5720 0.052 Uiso 1 1 calc R . . C2 C 0.3900(9) 0.2948(4) 0.9688(6) 0.036(2) Uani 1 1 d . . . C4 C 0.5822(9) 0.2550(4) 1.0214(6) 0.039(3) Uani 1 1 d . . . H4A H 0.6600 0.2569 1.0517 0.047 Uiso 1 1 calc R . . C21 C 0.5995(9) 0.0877(4) 0.6635(5) 0.033(2) Uani 1 1 d . . . H21A H 0.6266 0.0560 0.6509 0.040 Uiso 1 1 calc R . . C35 C 0.7191(12) 0.3090(5) 0.8703(7) 0.063(4) Uani 1 1 d . . . H35A H 0.7240 0.3163 0.9197 0.075 Uiso 1 1 calc R . . C39 C -0.0317(8) 0.1993(4) 0.7890(6) 0.041(3) Uani 1 1 d . . . H39A H -0.0752 0.2257 0.8131 0.050 Uiso 1 1 calc R . . C23 C 0.6509(8) 0.1679(4) 0.7105(6) 0.035(2) Uani 1 1 d . . . H23A H 0.7127 0.1910 0.7298 0.042 Uiso 1 1 calc R . . C29 C 0.3491(10) 0.3433(5) 0.5703(6) 0.046(3) Uani 1 1 d . . . H29A H 0.3122 0.3751 0.5697 0.055 Uiso 1 1 calc R . . C42 C 0.1392(11) 0.3503(5) 0.9883(7) 0.051(3) Uani 1 1 d . . . H42A H 0.0944 0.3815 0.9786 0.077 Uiso 1 1 calc R . . H42B H 0.1538 0.3445 1.0399 0.077 Uiso 1 1 calc R . . H42C H 0.0889 0.3233 0.9649 0.077 Uiso 1 1 calc R . . C40 C -0.0373(8) 0.1942(4) 0.7136(6) 0.042(3) Uani 1 1 d . . . H40A H -0.0851 0.2154 0.6761 0.050 Uiso 1 1 calc R . . C10 C 0.1050(13) 0.0726(5) 1.0388(9) 0.071(4) Uani 1 1 d . . . H10A H 0.0511 0.0558 1.0664 0.086 Uiso 1 1 calc R . . C31 C 0.6074(8) 0.2742(4) 0.7613(6) 0.035(2) Uani 1 1 d . . . C36 C 0.6198(10) 0.2842(4) 0.8354(6) 0.040(3) Uani 1 1 d . . . H36A H 0.5561 0.2732 0.8617 0.048 Uiso 1 1 calc R . . C37 C 0.0600(8) 0.1276(4) 0.7705(6) 0.035(3) Uani 1 1 d . . . H37A H 0.0927 0.0933 0.7788 0.042 Uiso 1 1 calc R . . C22 C 0.6851(9) 0.1215(4) 0.6931(6) 0.041(3) Uani 1 1 d . . . H22A H 0.7709 0.1124 0.7018 0.049 Uiso 1 1 calc R . . C3 C 0.5083(10) 0.2965(4) 1.0091(6) 0.045(3) Uani 1 1 d . . . H3A H 0.5390 0.3271 1.0286 0.054 Uiso 1 1 calc R . . C8 C 0.2359(12) 0.1393(4) 1.0209(6) 0.051(3) Uani 1 1 d U . . H8A H 0.2646 0.1713 1.0353 0.061 Uiso 1 1 calc R . . C38 C 0.0221(9) 0.1577(5) 0.8225(6) 0.046(3) Uani 1 1 d . . . H38A H 0.0243 0.1493 0.8741 0.055 Uiso 1 1 calc R . . C43 C 0.3839(13) 0.4042(5) 1.0033(7) 0.065(4) Uani 1 1 d . . . H43A H 0.4659 0.4078 0.9869 0.098 Uiso 1 1 calc R . . H43B H 0.3956 0.3963 1.0543 0.098 Uiso 1 1 calc R . . H43C H 0.3370 0.4350 0.9952 0.098 Uiso 1 1 calc R . . C15 C 0.6479(11) 0.0507(5) 0.9797(7) 0.055(3) Uani 1 1 d . . . H15A H 0.6672 0.0286 1.0185 0.066 Uiso 1 1 calc R . . C16 C 0.7272(12) 0.0543(5) 0.9302(7) 0.062(4) Uani 1 1 d . . . H16A H 0.7999 0.0342 0.9338 0.075 Uiso 1 1 calc R . . C18 C 0.5955(10) 0.1147(4) 0.8684(7) 0.052(3) Uani 1 1 d . . . H18A H 0.5779 0.1371 0.8298 0.062 Uiso 1 1 calc R . . C11 C 0.1248(12) 0.0543(5) 0.9745(8) 0.056(3) Uani 1 1 d . . . H11A H 0.0820 0.0253 0.9566 0.068 Uiso 1 1 calc R . . C33 C 0.8035(10) 0.3147(5) 0.7577(8) 0.056(3) Uani 1 1 d . . . H33A H 0.8686 0.3251 0.7320 0.067 Uiso 1 1 calc R . . C34 C 0.8141(11) 0.3234(5) 0.8311(8) 0.061(4) Uani 1 1 d . . . H34A H 0.8867 0.3393 0.8547 0.074 Uiso 1 1 calc R . . C12 C 0.2100(11) 0.0782(4) 0.9329(7) 0.051(3) Uani 1 1 d . . . H12A H 0.2253 0.0654 0.8882 0.061 Uiso 1 1 calc R . . C9 C 0.1622(14) 0.1151(5) 1.0639(8) 0.072(4) Uani 1 1 d . . . H9A H 0.1517 0.1276 1.1097 0.086 Uiso 1 1 calc R . . C47 C 0.2317(14) 0.0334(6) 0.6559(8) 0.093(6) Uani 1 1 d . . . H47A H 0.1770 0.0093 0.6286 0.139 Uiso 1 1 calc R . . H47B H 0.1823 0.0622 0.6659 0.139 Uiso 1 1 calc R . . H47C H 0.2696 0.0186 0.7009 0.139 Uiso 1 1 calc R . . C17 C 0.7021(11) 0.0876(6) 0.8740(7) 0.066(4) Uani 1 1 d . . . H17A H 0.7587 0.0912 0.8401 0.079 Uiso 1 1 calc R . . C28 C 0.3742(11) 0.3251(5) 0.5090(7) 0.055(3) Uani 1 1 d . . . H28A H 0.3555 0.3431 0.4659 0.066 Uiso 1 1 calc R . . C44 C 0.2705(15) 0.3666(5) 0.8542(7) 0.073(4) Uani 1 1 d . . . H44A H 0.3518 0.3684 0.8367 0.109 Uiso 1 1 calc R . . H44B H 0.2265 0.3981 0.8454 0.109 Uiso 1 1 calc R . . H44C H 0.2203 0.3403 0.8291 0.109 Uiso 1 1 calc R . . C27 C 0.4283(12) 0.2789(6) 0.5097(7) 0.063(4) Uani 1 1 d . . . H27A H 0.4446 0.2652 0.4657 0.076 Uiso 1 1 calc R . . C45 C 0.4479(13) -0.0046(5) 0.5962(9) 0.078(5) Uani 1 1 d . . . H45A H 0.3933 -0.0298 0.5713 0.116 Uiso 1 1 calc R . . H45B H 0.4805 -0.0163 0.6441 0.116 Uiso 1 1 calc R . . H45C H 0.5178 0.0019 0.5694 0.116 Uiso 1 1 calc R . . C46 C 0.2940(11) 0.0760(5) 0.5117(6) 0.060(4) Uani 1 1 d . . . H46A H 0.2367 0.0516 0.4871 0.090 Uiso 1 1 calc R . . H46B H 0.3634 0.0817 0.4842 0.090 Uiso 1 1 calc R . . H46C H 0.2489 0.1069 0.5161 0.090 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 0.0115(4) 0.0282(5) 0.0260(5) 0.0002(4) 0.0011(3) 0.0001(4) P2 0.0160(11) 0.0303(14) 0.0319(14) -0.0022(11) -0.0006(10) -0.0004(10) S3 0.0163(10) 0.0388(15) 0.0294(13) -0.0069(11) -0.0008(9) 0.0016(10) S1 0.0216(11) 0.0382(15) 0.0326(14) -0.0041(11) 0.0022(10) 0.0045(10) Cl1 0.0302(12) 0.0390(15) 0.0439(16) 0.0065(12) 0.0023(11) 0.0070(11) P1 0.0271(13) 0.0284(14) 0.0362(15) 0.0038(11) -0.0043(11) 0.0022(11) Si1 0.0413(16) 0.0322(16) 0.0372(17) -0.0058(13) -0.0037(13) 0.0073(13) Si2 0.0386(16) 0.0342(18) 0.064(2) -0.0135(15) 0.0055(15) -0.0008(14) O4 0.018(3) 0.031(4) 0.024(3) -0.003(3) -0.003(3) -0.003(3) O2 0.035(4) 0.030(4) 0.030(4) 0.012(3) 0.007(3) 0.002(3) C6 0.022(5) 0.045(7) 0.040(6) -0.006(5) 0.005(4) 0.001(5) C41 0.020(5) 0.082(9) 0.051(7) -0.012(7) -0.004(5) -0.019(6) C25 0.012(4) 0.038(6) 0.042(6) 0.000(5) 0.004(4) -0.007(4) C5 0.029(5) 0.039(7) 0.053(7) 0.001(5) -0.013(5) 0.006(5) C20 0.031(5) 0.027(6) 0.041(6) 0.006(4) 0.003(5) 0.005(4) C1 0.031(5) 0.046(6) 0.016(5) 0.001(4) 0.008(4) 0.005(5) C32 0.028(5) 0.046(7) 0.043(6) -0.001(5) 0.004(5) -0.011(5) C30 0.036(5) 0.026(6) 0.052(7) 0.009(5) 0.013(5) 0.003(5) C24 0.008(4) 0.037(6) 0.036(6) 0.005(4) -0.003(4) 0.005(4) C19 0.017(4) 0.040(6) 0.034(6) -0.006(5) 0.004(4) -0.005(4) C13 0.045(6) 0.041(7) 0.032(6) -0.014(5) -0.007(5) 0.015(5) C7 0.059(6) 0.023(5) 0.053(6) 0.014(4) 0.023(5) 0.015(5) C14 0.059(7) 0.047(7) 0.050(7) 0.015(6) 0.015(6) 0.021(6) C26 0.030(5) 0.058(8) 0.043(7) -0.002(6) 0.013(5) -0.020(5) C2 0.029(5) 0.035(6) 0.044(6) -0.005(5) 0.008(5) -0.008(5) C4 0.018(5) 0.053(7) 0.044(7) -0.003(5) -0.004(4) -0.005(5) C21 0.026(5) 0.036(6) 0.036(6) -0.004(5) 0.000(4) 0.006(4) C35 0.058(8) 0.067(9) 0.056(8) -0.017(7) -0.018(7) -0.010(7) C39 0.006(4) 0.054(7) 0.064(8) -0.009(6) 0.005(4) 0.003(4) C23 0.012(4) 0.041(6) 0.052(7) 0.003(5) 0.000(4) 0.000(4) C29 0.028(5) 0.055(8) 0.053(8) 0.021(6) 0.002(5) 0.007(5) C42 0.046(7) 0.050(8) 0.060(8) 0.001(6) 0.019(6) 0.011(6) C40 0.012(4) 0.063(8) 0.051(7) -0.006(6) 0.006(4) 0.004(5) C10 0.068(9) 0.037(8) 0.116(14) 0.025(8) 0.038(9) -0.004(7) C31 0.011(4) 0.036(6) 0.056(7) 0.002(5) 0.002(4) -0.006(4) C36 0.036(6) 0.051(7) 0.034(6) -0.005(5) 0.010(5) -0.011(5) C37 0.015(4) 0.036(6) 0.056(7) 0.016(5) 0.011(5) 0.000(4) C22 0.020(5) 0.053(7) 0.052(7) 0.014(6) 0.010(5) 0.015(5) C3 0.039(6) 0.045(7) 0.048(7) -0.012(6) -0.004(5) -0.009(5) C8 0.076(7) 0.022(5) 0.066(6) 0.020(5) 0.050(6) 0.026(5) C38 0.024(5) 0.065(8) 0.049(7) -0.002(6) 0.011(5) -0.019(5) C43 0.069(9) 0.052(8) 0.067(9) -0.006(7) -0.018(7) 0.019(7) C15 0.048(7) 0.060(8) 0.057(8) 0.016(6) 0.006(6) 0.030(6) C16 0.053(8) 0.060(9) 0.070(9) 0.008(7) -0.009(7) 0.031(7) C18 0.040(6) 0.048(7) 0.070(9) 0.025(6) 0.011(6) 0.017(6) C11 0.057(8) 0.037(7) 0.072(9) 0.017(7) -0.001(7) -0.008(6) C33 0.033(6) 0.064(9) 0.075(9) 0.001(7) 0.023(6) -0.017(6) C34 0.031(6) 0.068(9) 0.080(10) -0.019(8) -0.009(6) -0.016(6) C12 0.064(8) 0.028(6) 0.062(8) -0.001(6) 0.012(6) -0.001(6) C9 0.085(10) 0.060(10) 0.079(11) -0.001(8) 0.043(9) 0.003(8) C47 0.079(10) 0.118(14) 0.091(12) -0.041(10) 0.047(9) -0.067(10) C17 0.044(7) 0.089(11) 0.064(9) 0.014(8) 0.009(6) 0.032(7) C28 0.046(7) 0.067(9) 0.051(8) 0.036(7) 0.006(6) 0.005(6) C44 0.102(11) 0.059(9) 0.064(9) 0.031(7) 0.036(8) 0.030(8) C27 0.061(8) 0.093(11) 0.037(7) 0.006(7) 0.008(6) -0.016(8) C45 0.061(9) 0.058(9) 0.113(13) -0.047(9) 0.010(8) 0.007(7) C46 0.049(7) 0.073(9) 0.053(8) -0.018(7) -0.012(6) -0.001(7) _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_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.034 0.000 0.500 682 257 ' ' 2 -0.035 0.500 1.000 682 255 ' ' 3 0.200 0.744 0.405 21 5 ' ' 4 0.300 0.244 0.095 21 3 ' ' 5 0.699 0.756 0.905 21 5 ' ' 6 0.800 0.256 0.595 20 4 ' ' _platon_squeeze_details ; ; 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 O4 2.185(6) . ? Zr1 O2 2.197(6) . ? Zr1 Cl1 2.490(3) . ? Zr1 C37 2.519(10) . ? Zr1 C39 2.525(9) . ? Zr1 C41 2.539(10) . ? Zr1 C38 2.569(10) . ? Zr1 C40 2.569(9) . ? Zr1 S1 2.616(3) . ? Zr1 S3 2.636(3) . ? P2 O4 1.509(6) . ? P2 C24 1.767(10) . ? P2 C31 1.799(9) . ? P2 C25 1.800(10) . ? S3 C19 1.775(9) . ? S1 C1 1.769(10) . ? P1 O2 1.513(7) . ? P1 C6 1.764(11) . ? P1 C7 1.783(11) . ? P1 C13 1.798(10) . ? Si1 C43 1.872(13) . ? Si1 C44 1.876(13) . ? Si1 C2 1.895(11) . ? Si1 C42 1.896(11) . ? Si2 C45 1.850(13) . ? Si2 C47 1.866(13) . ? Si2 C46 1.879(13) . ? Si2 C20 1.905(11) . ? C6 C1 1.412(14) . ? C6 C5 1.436(13) . ? C41 C37 1.401(15) . ? C41 C40 1.424(17) . ? C41 H41A 1.0000 . ? C25 C30 1.402(14) . ? C25 C26 1.406(15) . ? C5 C4 1.357(15) . ? C5 H5A 0.9500 . ? C20 C19 1.366(14) . ? C20 C21 1.432(13) . ? C1 C2 1.403(14) . ? C32 C33 1.392(15) . ? C32 C31 1.396(14) . ? C32 H32A 0.9500 . ? C30 C29 1.385(15) . ? C30 H30A 0.9500 . ? C24 C19 1.419(13) . ? C24 C23 1.421(11) . ? C13 C18 1.393(16) . ? C13 C14 1.408(15) . ? C7 C8 1.321(15) . ? C7 C12 1.415(16) . ? C14 C15 1.359(15) . ? C14 H14A 0.9500 . ? C26 C27 1.398(17) . ? C26 H26A 0.9500 . ? C2 C3 1.395(14) . ? C4 C3 1.383(15) . ? C4 H4A 0.9500 . ? C21 C22 1.365(14) . ? C21 H21A 0.9500 . ? C35 C36 1.358(15) . ? C35 C34 1.399(19) . ? C35 H35A 0.9500 . ? C39 C38 1.383(16) . ? C39 C40 1.425(15) . ? C39 H39A 1.0000 . ? C23 C22 1.368(15) . ? C23 H23A 0.9500 . ? C29 C28 1.322(17) . ? C29 H29A 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C40 H40A 1.0000 . ? C10 C11 1.359(19) . ? C10 C9 1.362(19) . ? C10 H10A 0.9500 . ? C31 C36 1.417(14) . ? C36 H36A 0.9500 . ? C37 C38 1.383(15) . ? C37 H37A 1.0000 . ? C22 H22A 0.9500 . ? C3 H3A 0.9500 . ? C8 C9 1.380(17) . ? C8 H8A 0.9500 . ? C38 H38A 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C15 C16 1.355(17) . ? C15 H15A 0.9500 . ? C16 C17 1.393(18) . ? C16 H16A 0.9500 . ? C18 C17 1.358(15) . ? C18 H18A 0.9500 . ? C11 C12 1.443(17) . ? C11 H11A 0.9500 . ? C33 C34 1.397(18) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C12 H12A 0.9500 . ? C9 H9A 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C17 H17A 0.9500 . ? C28 C27 1.382(19) . ? C28 H28A 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C27 H27A 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? 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 O4 Zr1 O2 78.2(2) . . ? O4 Zr1 Cl1 78.92(17) . . ? O2 Zr1 Cl1 156.30(19) . . ? O4 Zr1 C37 153.0(3) . . ? O2 Zr1 C37 78.1(3) . . ? Cl1 Zr1 C37 125.6(2) . . ? O4 Zr1 C39 152.8(3) . . ? O2 Zr1 C39 115.5(3) . . ? Cl1 Zr1 C39 83.2(3) . . ? C37 Zr1 C39 52.6(3) . . ? O4 Zr1 C41 149.7(3) . . ? O2 Zr1 C41 104.9(3) . . ? Cl1 Zr1 C41 98.0(3) . . ? C37 Zr1 C41 32.2(4) . . ? C39 Zr1 C41 53.1(4) . . ? O4 Zr1 C38 155.1(3) . . ? O2 Zr1 C38 84.7(3) . . ? Cl1 Zr1 C38 114.6(3) . . ? C37 Zr1 C38 31.5(3) . . ? C39 Zr1 C38 31.5(4) . . ? C41 Zr1 C38 52.7(4) . . ? O4 Zr1 C40 149.2(3) . . ? O2 Zr1 C40 131.4(3) . . ? Cl1 Zr1 C40 72.2(3) . . ? C37 Zr1 C40 53.4(3) . . ? C39 Zr1 C40 32.5(3) . . ? C41 Zr1 C40 32.4(4) . . ? C38 Zr1 C40 53.1(4) . . ? O4 Zr1 S1 84.45(17) . . ? O2 Zr1 S1 80.65(18) . . ? Cl1 Zr1 S1 90.94(9) . . ? C37 Zr1 S1 104.2(3) . . ? C39 Zr1 S1 75.5(3) . . ? C41 Zr1 S1 125.8(3) . . ? C38 Zr1 S1 75.0(3) . . ? C40 Zr1 S1 106.1(3) . . ? O4 Zr1 S3 80.27(17) . . ? O2 Zr1 S3 85.49(18) . . ? Cl1 Zr1 S3 96.82(9) . . ? C37 Zr1 S3 85.2(3) . . ? C39 Zr1 S3 122.4(3) . . ? C41 Zr1 S3 70.1(3) . . ? C38 Zr1 S3 116.5(3) . . ? C40 Zr1 S3 92.6(2) . . ? S1 Zr1 S3 161.17(8) . . ? O4 P2 C24 112.5(4) . . ? O4 P2 C31 109.1(4) . . ? C24 P2 C31 107.3(4) . . ? O4 P2 C25 115.1(4) . . ? C24 P2 C25 107.6(5) . . ? C31 P2 C25 104.7(5) . . ? C19 S3 Zr1 113.3(3) . . ? C1 S1 Zr1 111.3(3) . . ? O2 P1 C6 114.0(4) . . ? O2 P1 C7 112.1(5) . . ? C6 P1 C7 109.8(5) . . ? O2 P1 C13 108.0(4) . . ? C6 P1 C13 107.0(5) . . ? C7 P1 C13 105.5(5) . . ? C43 Si1 C44 111.1(7) . . ? C43 Si1 C2 107.9(5) . . ? C44 Si1 C2 108.8(5) . . ? C43 Si1 C42 105.4(6) . . ? C44 Si1 C42 110.6(6) . . ? C2 Si1 C42 113.0(5) . . ? C45 Si2 C47 103.3(8) . . ? C45 Si2 C46 110.5(7) . . ? C47 Si2 C46 112.8(7) . . ? C45 Si2 C20 107.2(5) . . ? C47 Si2 C20 112.9(6) . . ? C46 Si2 C20 109.9(5) . . ? P2 O4 Zr1 134.2(4) . . ? P1 O2 Zr1 133.9(4) . . ? C1 C6 C5 118.0(10) . . ? C1 C6 P1 122.2(7) . . ? C5 C6 P1 119.8(8) . . ? C37 C41 C40 108.0(11) . . ? C37 C41 Zr1 73.1(6) . . ? C40 C41 Zr1 75.0(6) . . ? C37 C41 H41A 125.6 . . ? C40 C41 H41A 125.6 . . ? Zr1 C41 H41A 125.6 . . ? C30 C25 C26 121.0(10) . . ? C30 C25 P2 119.3(8) . . ? C26 C25 P2 119.5(8) . . ? C4 C5 C6 120.6(10) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C19 C20 C21 118.0(9) . . ? C19 C20 Si2 124.1(7) . . ? C21 C20 Si2 117.7(7) . . ? C2 C1 C6 120.7(9) . . ? C2 C1 S1 120.8(8) . . ? C6 C1 S1 118.2(8) . . ? C33 C32 C31 118.3(11) . . ? C33 C32 H32A 120.9 . . ? C31 C32 H32A 120.9 . . ? C29 C30 C25 117.3(11) . . ? C29 C30 H30A 121.4 . . ? C25 C30 H30A 121.4 . . ? C19 C24 C23 118.0(9) . . ? C19 C24 P2 120.1(6) . . ? C23 C24 P2 121.8(7) . . ? C20 C19 C24 122.1(8) . . ? C20 C19 S3 118.4(7) . . ? C24 C19 S3 119.5(7) . . ? C18 C13 C14 117.3(10) . . ? C18 C13 P1 119.5(8) . . ? C14 C13 P1 123.1(9) . . ? C8 C7 C12 117.7(11) . . ? C8 C7 P1 125.9(10) . . ? C12 C7 P1 116.3(9) . . ? C15 C14 C13 120.1(11) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C27 C26 C25 116.5(12) . . ? C27 C26 H26A 121.8 . . ? C25 C26 H26A 121.8 . . ? C3 C2 C1 118.3(10) . . ? C3 C2 Si1 119.7(8) . . ? C1 C2 Si1 121.9(7) . . ? C5 C4 C3 120.3(9) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C22 C21 C20 120.3(9) . . ? C22 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C36 C35 C34 117.8(12) . . ? C36 C35 H35A 121.1 . . ? C34 C35 H35A 121.1 . . ? C38 C39 C40 109.7(10) . . ? C38 C39 Zr1 76.0(5) . . ? C40 C39 Zr1 75.5(5) . . ? C38 C39 H39A 124.6 . . ? C40 C39 H39A 124.6 . . ? Zr1 C39 H39A 124.6 . . ? C22 C23 C24 119.6(9) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C28 C29 C30 124.3(12) . . ? C28 C29 H29A 117.8 . . ? C30 C29 H29A 117.8 . . ? Si1 C42 H42A 109.5 . . ? Si1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C40 C39 105.2(10) . . ? C41 C40 Zr1 72.6(5) . . ? C39 C40 Zr1 72.0(5) . . ? C41 C40 H40A 127.1 . . ? C39 C40 H40A 127.1 . . ? Zr1 C40 H40A 127.1 . . ? C11 C10 C9 120.3(13) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C32 C31 C36 119.3(9) . . ? C32 C31 P2 120.9(8) . . ? C36 C31 P2 119.8(7) . . ? C35 C36 C31 122.6(11) . . ? C35 C36 H36A 118.7 . . ? C31 C36 H36A 118.7 . . ? C38 C37 C41 109.1(10) . . ? C38 C37 Zr1 76.2(6) . . ? C41 C37 Zr1 74.7(6) . . ? C38 C37 H37A 124.9 . . ? C41 C37 H37A 124.9 . . ? Zr1 C37 H37A 124.9 . . ? C21 C22 C23 121.9(9) . . ? C21 C22 H22A 119.0 . . ? C23 C22 H22A 119.0 . . ? C4 C3 C2 121.8(10) . . ? C4 C3 H3A 119.1 . . ? C2 C3 H3A 119.1 . . ? C7 C8 C9 125.2(13) . . ? C7 C8 H8A 117.4 . . ? C9 C8 H8A 117.4 . . ? C37 C38 C39 107.7(10) . . ? C37 C38 Zr1 72.3(6) . . ? C39 C38 Zr1 72.5(6) . . ? C37 C38 H38A 126.0 . . ? C39 C38 H38A 126.0 . . ? Zr1 C38 H38A 126.0 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C16 C15 C14 121.5(12) . . ? C16 C15 H15A 119.2 . . ? C14 C15 H15A 119.2 . . ? C15 C16 C17 120.0(11) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C17 C18 C13 122.1(11) . . ? C17 C18 H18A 119.0 . . ? C13 C18 H18A 119.0 . . ? C10 C11 C12 120.8(12) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C32 C33 C34 121.0(10) . . ? C32 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C33 C34 C35 120.9(10) . . ? C33 C34 H34A 119.6 . . ? C35 C34 H34A 119.6 . . ? C7 C12 C11 117.3(11) . . ? C7 C12 H12A 121.3 . . ? C11 C12 H12A 121.3 . . ? C10 C9 C8 117.9(14) . . ? C10 C9 H9A 121.0 . . ? C8 C9 H9A 121.0 . . ? Si2 C47 H47A 109.5 . . ? Si2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C18 C17 C16 119.1(12) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? C29 C28 C27 118.0(11) . . ? C29 C28 H28A 121.0 . . ? C27 C28 H28A 121.0 . . ? Si1 C44 H44A 109.5 . . ? Si1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C28 C27 C26 122.9(13) . . ? C28 C27 H27A 118.6 . . ? C26 C27 H27A 118.6 . . ? Si2 C45 H45A 109.5 . . ? Si2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si2 C46 H46A 109.5 . . ? Si2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.988 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.155