# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1604 # Paper Ref. # # Biarylphosphonites: a class of monodentate phosphorus(III) ligands # that outperform their chelating analogues in asymmetric # hydrogenation catalyses # #============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Dr P.G. Pringle, School of Chemistry, Cantocks Close, University of Bristol. Bristol. BS8 1TS. ; _publ_contact_author_phone '0117 928 8114' _publ_contact_author_fax '0117 929 0509' _publ_contact_author_email 'Paul.Pringle@bris.ac.uk' _publ_requested_journal 'Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Phosphonites: the most enantioselective monodentate phosphorus(III) ligands for asymmetric hydrogenations. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Claver, Carmen' ; Universitat Rovira i Virgili Department de Quimica Fisica Inorganica Placa Imperial Tarraco,1, Tarragona, Spain ; 'Fernandez, Elena' ; Universitat Rovira i Virgili Department de Quimica Fisica Inorganica Placa Imperial Tarraco,1, Tarragona, Spain ; 'Gillon, Amy L.' ; School of Chemistry University of Bristol Cantock's Close BS8 1TS. Bristol, UK ; 'Heslop, Katie M.' ; School of Chemistry University of Bristol Cantock's Close BS8 1TS. Bristol, UK ; 'Hyett, David J.' ; School of Chemistry University of Bristol Cantock's Close BS8 1TS. Bristol, UK ; 'Martorell, Aina' ; School of Chemistry University of Bristol Cantock's Close BS8 1TS. Bristol, UK ; 'Orpen, A. Guy' ; School of Chemistry University of Bristol Cantock's Close BS8 1TS. Bristol, UK ; 'Pringle, Paul G.' ; School of Chemistry University of Bristol Cantock's Close BS8 1TS. Bristol, UK ; #============================================================================== # 4. TEXT # # # # data_R,R-7.thf.(CHCl3)0.76 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72.76 H50.76 Cl4.27 O5 P2 Pt' _chemical_formula_weight 1413.38 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' 'Pt' 'Pt' -1.7033 8.3905 '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 13.3036(19) _cell_length_b 19.602(4) _cell_length_c 23.287(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6072.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 132 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'Not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 2.605 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.584882 _exptl_absorpt_correction_T_max 0.694168 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 33374 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0955 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10674 _reflns_number_gt 8024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXTL (Siemens, 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _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^)+(0.0382P)^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 mixed _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 -0.020(6) _refine_ls_number_reflns 10674 _refine_ls_number_parameters 776 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.979 _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 Pt1 Pt 0.74015(2) 0.344370(15) 0.376583(13) 0.02332(8) Uani 1 1 d . . . Cl1 Cl 0.71490(16) 0.25856(11) 0.44538(10) 0.0344(6) Uani 1 1 d . . . Cl2 Cl 0.76946(18) 0.25990(10) 0.30746(10) 0.0363(6) Uani 1 1 d . . . P1 P 0.70719(15) 0.41479(11) 0.44777(10) 0.0243(5) Uani 1 1 d . . . P2 P 0.76920(17) 0.41659(10) 0.30644(9) 0.0257(5) Uani 1 1 d . . . O11 O 0.7923(3) 0.4155(3) 0.4963(2) 0.0228(13) Uani 1 1 d . . . O12 O 0.6989(4) 0.4938(2) 0.4303(2) 0.0216(14) Uani 1 1 d . . . O21 O 0.7721(4) 0.4956(2) 0.3256(3) 0.0244(14) Uani 1 1 d . . . O22 O 0.6857(4) 0.4153(3) 0.2568(2) 0.0246(13) Uani 1 1 d . . . C101 C 0.5967(6) 0.3964(4) 0.4881(4) 0.029(2) Uani 1 1 d . . . C102 C 0.5146(6) 0.3676(5) 0.4593(5) 0.039(3) Uani 1 1 d . . . H102 H 0.5181 0.3577 0.4194 0.047 Uiso 1 1 calc R . . C103 C 0.4282(7) 0.3538(6) 0.4905(5) 0.048(3) Uani 1 1 d . . . H103 H 0.3737 0.3316 0.4718 0.058 Uiso 1 1 calc R . . C104 C 0.4184(7) 0.3705(5) 0.5462(5) 0.055(3) Uani 1 1 d . . . H104 H 0.3572 0.3617 0.5658 0.066 Uiso 1 1 calc R . . C105 C 0.4996(7) 0.4012(5) 0.5753(4) 0.044(3) Uani 1 1 d . . . H105 H 0.4935 0.4128 0.6148 0.053 Uiso 1 1 calc R . . C106 C 0.5885(6) 0.4144(5) 0.5462(4) 0.031(2) Uani 1 1 d . . . H106 H 0.6433 0.4354 0.5655 0.037 Uiso 1 1 calc R . . C107 C 0.8805(6) 0.4536(4) 0.4841(3) 0.0192(19) Uani 1 1 d . . . C108 C 0.9672(6) 0.4143(5) 0.4677(4) 0.030(2) Uani 1 1 d . . . C109 C 0.9667(5) 0.3434(5) 0.4651(3) 0.027(2) Uani 1 1 d . . . H109 H 0.9069 0.3191 0.4739 0.033 Uiso 1 1 calc R . . C110 C 1.0520(6) 0.3081(5) 0.4499(4) 0.033(2) Uani 1 1 d . . . H110 H 1.0512 0.2597 0.4480 0.039 Uiso 1 1 calc R . . C111 C 1.1379(6) 0.3434(6) 0.4375(4) 0.040(2) Uani 1 1 d . . . H111 H 1.1970 0.3191 0.4272 0.048 Uiso 1 1 calc R . . C112 C 1.1403(6) 0.4117(5) 0.4397(4) 0.034(2) Uani 1 1 d . . . H112 H 1.2015 0.4341 0.4306 0.041 Uiso 1 1 calc R . . C113 C 1.0570(6) 0.4516(5) 0.4548(4) 0.030(2) Uani 1 1 d . . . C114 C 1.0561(6) 0.5252(5) 0.4577(4) 0.030(2) Uani 1 1 d . . . C115 C 1.1427(7) 0.5649(5) 0.4454(4) 0.039(2) Uani 1 1 d . . . H115 H 1.2037 0.5422 0.4363 0.046 Uiso 1 1 calc R . . C116 C 1.1414(7) 0.6332(5) 0.4463(4) 0.038(2) Uani 1 1 d . . . H116 H 1.2009 0.6580 0.4377 0.045 Uiso 1 1 calc R . . C117 C 1.0531(7) 0.6679(5) 0.4596(4) 0.040(3) Uani 1 1 d . . . H117 H 1.0523 0.7164 0.4601 0.048 Uiso 1 1 calc R . . C118 C 0.9670(7) 0.6320(5) 0.4723(4) 0.038(3) Uani 1 1 d . . . H118 H 0.9069 0.6563 0.4804 0.046 Uiso 1 1 calc R . . C119 C 0.9657(6) 0.5605(5) 0.4735(4) 0.027(2) Uani 1 1 d . . . C120 C 0.8769(6) 0.5223(5) 0.4884(4) 0.023(2) Uani 1 1 d . . . C121 C 0.7805(6) 0.5555(4) 0.5047(3) 0.0239(19) Uani 1 1 d . . . C122 C 0.7728(6) 0.6015(4) 0.5538(3) 0.0241(18) Uani 1 1 d . . . C123 C 0.8548(7) 0.6128(5) 0.5902(4) 0.037(2) Uani 1 1 d . . . H123 H 0.9166 0.5904 0.5826 0.045 Uiso 1 1 calc R . . C124 C 0.8478(6) 0.6553(6) 0.6362(4) 0.039(2) Uani 1 1 d . . . H124 H 0.9041 0.6614 0.6608 0.047 Uiso 1 1 calc R . . C125 C 0.7570(7) 0.6904(4) 0.6475(3) 0.038(2) Uani 1 1 d . . . H125 H 0.7525 0.7218 0.6785 0.046 Uiso 1 1 calc R . . C126 C 0.6771(6) 0.6784(4) 0.6133(4) 0.035(2) Uani 1 1 d . . . H126 H 0.6159 0.7016 0.6213 0.042 Uiso 1 1 calc R . . C127 C 0.6800(6) 0.6331(4) 0.5661(4) 0.026(2) Uani 1 1 d . . . C128 C 0.5914(6) 0.6200(4) 0.5311(4) 0.028(2) Uani 1 1 d . . . C129 C 0.4979(6) 0.6486(5) 0.5400(4) 0.036(2) Uani 1 1 d . . . H129 H 0.4899 0.6791 0.5714 0.043 Uiso 1 1 calc R . . C130 C 0.4179(7) 0.6357(5) 0.5069(5) 0.045(3) Uani 1 1 d . . . H130 H 0.3546 0.6554 0.5159 0.055 Uiso 1 1 calc R . . C131 C 0.4277(7) 0.5928(5) 0.4587(4) 0.038(2) Uani 1 1 d . . . H131 H 0.3723 0.5855 0.4337 0.046 Uiso 1 1 calc R . . C132 C 0.5160(6) 0.5624(5) 0.4485(4) 0.031(2) Uani 1 1 d . . . H132 H 0.5221 0.5323 0.4167 0.038 Uiso 1 1 calc R . . C133 C 0.6007(6) 0.5742(5) 0.4842(4) 0.028(2) Uani 1 1 d . . . C134 C 0.6956(6) 0.5426(4) 0.4753(4) 0.026(2) Uani 1 1 d . . . C201 C 0.8838(6) 0.4051(5) 0.2669(4) 0.032(2) Uani 1 1 d . . . C202 C 0.8958(6) 0.4307(4) 0.2122(4) 0.031(2) Uani 1 1 d . . . H202 H 0.8404 0.4498 0.1921 0.038 Uiso 1 1 calc R . . C203 C 0.9913(8) 0.4281(5) 0.1865(5) 0.048(3) Uani 1 1 d . . . H203 H 1.0011 0.4466 0.1493 0.058 Uiso 1 1 calc R . . C204 C 1.0708(7) 0.3986(6) 0.2154(5) 0.053(3) Uani 1 1 d . . . H204 H 1.1344 0.3951 0.1970 0.064 Uiso 1 1 calc R . . C205 C 1.0595(7) 0.3746(6) 0.2694(5) 0.051(3) Uani 1 1 d . . . H205 H 1.1154 0.3558 0.2893 0.061 Uiso 1 1 calc R . . C206 C 0.9668(7) 0.3775(5) 0.2955(5) 0.038(3) Uani 1 1 d . . . H206 H 0.9590 0.3604 0.3334 0.045 Uiso 1 1 calc R . . C207 C 0.7737(6) 0.5456(4) 0.2805(3) 0.0254(19) Uani 1 1 d . . . C208 C 0.8633(6) 0.5830(5) 0.2737(4) 0.029(2) Uani 1 1 d . . . C209 C 0.9472(6) 0.5732(5) 0.3109(4) 0.037(2) Uani 1 1 d . . . H209 H 0.9441 0.5407 0.3411 0.045 Uiso 1 1 calc R . . C210 C 1.0312(7) 0.6107(6) 0.3026(5) 0.054(3) Uani 1 1 d . . . H210 H 1.0871 0.6042 0.3274 0.065 Uiso 1 1 calc R . . C211 C 1.0380(7) 0.6587(7) 0.2587(4) 0.056(3) Uani 1 1 d . . . H211 H 1.0983 0.6840 0.2537 0.068 Uiso 1 1 calc R . . C212 C 0.9574(7) 0.6698(5) 0.2223(4) 0.046(3) Uani 1 1 d . . . H212 H 0.9623 0.7031 0.1928 0.055 Uiso 1 1 calc R . . C213 C 0.8673(6) 0.6317(4) 0.2288(4) 0.026(2) Uani 1 1 d . . . C214 C 0.7819(6) 0.6377(4) 0.1902(3) 0.030(2) Uani 1 1 d . . . C215 C 0.7858(6) 0.6801(4) 0.1401(3) 0.032(2) Uani 1 1 d . . . H215 H 0.8443 0.7062 0.1321 0.039 Uiso 1 1 calc R . . C216 C 0.7059(7) 0.6828(4) 0.1043(4) 0.040(3) Uani 1 1 d . . . H216 H 0.7099 0.7100 0.0706 0.048 Uiso 1 1 calc R . . C217 C 0.6179(6) 0.6465(5) 0.1154(4) 0.037(2) Uani 1 1 d . . . H217 H 0.5620 0.6500 0.0902 0.044 Uiso 1 1 calc R . . C218 C 0.6131(6) 0.6061(4) 0.1630(4) 0.030(2) Uani 1 1 d . . . H218 H 0.5540 0.5804 0.1705 0.035 Uiso 1 1 calc R . . C219 C 0.6934(6) 0.6022(4) 0.2005(4) 0.028(2) Uani 1 1 d . . . C220 C 0.6876(6) 0.5555(4) 0.2503(4) 0.027(2) Uani 1 1 d . . . C221 C 0.5932(6) 0.5187(5) 0.2670(4) 0.026(2) Uani 1 1 d . . . C222 C 0.5023(6) 0.5546(4) 0.2812(3) 0.024(2) Uani 1 1 d . . . C223 C 0.4997(7) 0.6266(5) 0.2840(4) 0.033(2) Uani 1 1 d . . . H223 H 0.5588 0.6524 0.2768 0.040 Uiso 1 1 calc R . . C224 C 0.4119(6) 0.6588(5) 0.2972(4) 0.036(2) Uani 1 1 d . . . H224 H 0.4109 0.7072 0.2986 0.043 Uiso 1 1 calc R . . C225 C 0.3241(7) 0.6232(5) 0.3085(5) 0.045(3) Uani 1 1 d . . . H225 H 0.2636 0.6468 0.3172 0.054 Uiso 1 1 calc R . . C226 C 0.3262(6) 0.5529(5) 0.3068(4) 0.037(2) Uani 1 1 d . . . H226 H 0.2658 0.5284 0.3139 0.044 Uiso 1 1 calc R . . C227 C 0.4150(6) 0.5161(5) 0.2950(4) 0.027(2) Uani 1 1 d . . . C228 C 0.4194(6) 0.4420(4) 0.2949(4) 0.029(2) Uani 1 1 d . . . C229 C 0.3323(6) 0.4017(5) 0.3081(5) 0.050(3) Uani 1 1 d . . . H229 H 0.2694 0.4229 0.3154 0.060 Uiso 1 1 calc R . . C230 C 0.3415(7) 0.3309(5) 0.3099(4) 0.047(3) Uani 1 1 d . . . H230 H 0.2845 0.3037 0.3190 0.056 Uiso 1 1 calc R . . C231 C 0.4318(7) 0.2998(5) 0.2989(4) 0.045(3) Uani 1 1 d . . . H231 H 0.4367 0.2515 0.3006 0.054 Uiso 1 1 calc R . . C232 C 0.5157(6) 0.3379(5) 0.2853(4) 0.033(2) Uani 1 1 d . . . H232 H 0.5777 0.3156 0.2776 0.039 Uiso 1 1 calc R . . C233 C 0.5101(6) 0.4088(5) 0.2828(4) 0.027(2) Uani 1 1 d . . . C234 C 0.5951(6) 0.4498(5) 0.2690(4) 0.026(2) Uani 1 1 d . . . O1 O 0.3794(12) 0.2468(12) 0.1140(12) 0.331(14) Uani 1 1 d DU . . C1 C 0.3013(19) 0.2489(13) 0.0745(8) 0.215(11) Uani 1 1 d DU . . H1A H 0.3186 0.2221 0.0398 0.258 Uiso 1 1 calc R . . H1B H 0.2874 0.2966 0.0629 0.258 Uiso 1 1 calc R . . C2 C 0.2158(16) 0.2200(14) 0.1028(11) 0.314(19) Uani 1 1 d DU . . H2A H 0.1525 0.2352 0.0844 0.377 Uiso 1 1 calc R . . H2B H 0.2186 0.1696 0.1021 0.377 Uiso 1 1 calc R . . C3 C 0.2226(17) 0.2437(10) 0.1565(10) 0.212(12) Uani 1 1 d DU . . H3A H 0.2263 0.2044 0.1831 0.254 Uiso 1 1 calc R . . H3B H 0.1604 0.2693 0.1656 0.254 Uiso 1 1 calc R . . C4 C 0.305(2) 0.2863(14) 0.1667(12) 0.38(2) Uani 1 1 d DU . . H4A H 0.3329 0.2813 0.2059 0.452 Uiso 1 1 calc R . . H4B H 0.2911 0.3349 0.1583 0.452 Uiso 1 1 calc R . . C99 C 0.332(2) 0.5179(13) 0.1115(11) 0.190(17) Uani 0.756(7) 1 d PU . . H99 H 0.3691 0.5331 0.0764 0.229 Uiso 0.756(7) 1 calc PR . . Cl99 Cl 0.2261(6) 0.4827(3) 0.0841(3) 0.151(3) Uani 0.756(7) 1 d P . . Cl98 Cl 0.3133(6) 0.5835(5) 0.1426(4) 0.234(6) Uani 0.756(7) 1 d PU . . Cl97 Cl 0.4057(6) 0.4665(5) 0.1388(5) 0.237(6) Uani 0.756(7) 1 d PU . . 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 Pt1 0.02295(15) 0.02138(13) 0.02562(14) 0.00090(17) 0.00284(15) 0.00205(15) Cl1 0.0396(15) 0.0270(12) 0.0367(13) 0.0075(10) 0.0048(10) 0.0008(9) Cl2 0.0399(16) 0.0284(11) 0.0406(13) -0.0038(9) 0.0123(12) 0.0062(11) P1 0.0193(13) 0.0262(13) 0.0275(13) 0.0001(10) 0.0004(9) 0.0021(9) P2 0.0258(14) 0.0247(11) 0.0267(12) -0.0013(9) 0.0029(11) 0.0028(10) O11 0.016(3) 0.030(3) 0.022(3) 0.002(3) 0.001(2) 0.001(2) O12 0.029(3) 0.023(3) 0.013(3) 0.001(2) 0.001(2) 0.002(2) O21 0.018(3) 0.020(3) 0.035(4) 0.001(2) 0.005(3) -0.001(2) O22 0.023(3) 0.027(4) 0.024(3) -0.002(3) -0.001(2) 0.008(2) C101 0.020(5) 0.026(6) 0.041(6) -0.001(4) 0.003(4) 0.001(4) C102 0.022(5) 0.043(7) 0.052(7) -0.003(5) 0.000(4) -0.009(4) C103 0.024(5) 0.046(7) 0.074(8) -0.005(7) 0.000(5) -0.002(5) C104 0.032(6) 0.064(8) 0.069(9) -0.008(6) 0.026(5) 0.000(5) C105 0.048(6) 0.040(6) 0.045(7) 0.002(5) 0.017(5) 0.003(5) C106 0.028(5) 0.040(6) 0.025(5) 0.007(4) 0.007(4) 0.004(4) C107 0.016(5) 0.022(5) 0.019(5) 0.001(4) -0.003(3) -0.004(3) C108 0.026(5) 0.029(6) 0.034(6) 0.004(5) -0.010(4) 0.010(4) C109 0.023(4) 0.033(6) 0.026(5) 0.005(5) 0.003(3) 0.007(5) C110 0.031(6) 0.035(6) 0.032(6) -0.007(4) -0.007(4) 0.006(4) C111 0.022(5) 0.047(6) 0.051(6) 0.003(6) -0.001(4) 0.020(5) C112 0.016(5) 0.044(7) 0.043(6) 0.002(5) 0.006(4) -0.002(4) C113 0.023(5) 0.045(6) 0.022(5) 0.003(4) 0.004(4) 0.001(4) C114 0.024(5) 0.033(6) 0.033(6) -0.003(5) -0.008(4) -0.002(4) C115 0.024(5) 0.042(7) 0.050(7) 0.006(5) 0.006(4) -0.002(4) C116 0.037(6) 0.036(7) 0.039(6) 0.001(5) 0.005(4) -0.016(4) C117 0.040(6) 0.018(6) 0.063(7) 0.009(5) 0.004(5) 0.001(4) C118 0.032(6) 0.034(7) 0.048(7) 0.011(5) -0.005(4) 0.000(4) C119 0.028(5) 0.022(5) 0.030(6) 0.008(4) 0.000(4) -0.001(4) C120 0.016(5) 0.034(6) 0.020(5) -0.004(4) -0.005(3) 0.000(4) C121 0.023(5) 0.025(5) 0.023(5) 0.003(4) 0.000(4) -0.001(3) C122 0.024(5) 0.015(4) 0.033(5) -0.001(3) 0.004(4) -0.002(3) C123 0.029(5) 0.045(6) 0.038(6) 0.004(5) -0.003(4) -0.002(4) C124 0.042(5) 0.044(6) 0.031(6) -0.010(6) -0.007(4) -0.003(5) C125 0.049(6) 0.033(5) 0.032(5) -0.003(4) 0.000(5) -0.005(5) C126 0.035(5) 0.022(5) 0.046(7) 0.000(5) 0.007(4) -0.004(3) C127 0.030(5) 0.024(5) 0.025(5) -0.001(4) 0.003(4) 0.003(3) C128 0.026(5) 0.021(5) 0.036(6) 0.002(4) 0.012(4) 0.004(4) C129 0.032(5) 0.029(5) 0.047(6) 0.002(5) 0.003(4) -0.004(5) C130 0.027(6) 0.049(8) 0.061(7) -0.005(6) 0.010(5) 0.007(4) C131 0.029(5) 0.043(7) 0.043(7) -0.003(5) -0.006(4) 0.012(4) C132 0.030(5) 0.037(6) 0.027(6) -0.010(5) -0.001(4) 0.001(4) C133 0.029(5) 0.023(6) 0.032(6) 0.002(4) 0.005(4) 0.000(4) C134 0.028(5) 0.023(5) 0.026(5) 0.003(4) 0.006(4) 0.005(4) C201 0.022(5) 0.035(6) 0.039(6) 0.006(5) 0.001(4) -0.012(4) C202 0.025(5) 0.030(5) 0.039(6) -0.002(4) 0.009(4) 0.000(4) C203 0.055(7) 0.043(7) 0.047(7) -0.012(5) 0.021(6) -0.013(5) C204 0.019(6) 0.060(8) 0.081(9) 0.008(7) 0.025(5) 0.009(5) C205 0.019(6) 0.066(8) 0.068(9) 0.007(6) 0.012(5) 0.007(5) C206 0.027(6) 0.041(7) 0.045(7) 0.000(5) 0.006(5) 0.005(4) C207 0.039(6) 0.021(4) 0.016(4) -0.004(3) -0.002(4) -0.008(4) C208 0.026(5) 0.028(6) 0.033(6) 0.008(4) 0.011(4) 0.000(4) C209 0.034(6) 0.046(6) 0.032(6) 0.003(5) 0.001(4) -0.005(4) C210 0.033(6) 0.061(8) 0.068(9) 0.017(7) -0.006(5) -0.016(5) C211 0.038(6) 0.078(9) 0.053(7) 0.003(8) -0.005(5) -0.029(7) C212 0.050(6) 0.037(7) 0.051(7) 0.013(5) 0.008(5) -0.015(5) C213 0.022(5) 0.020(5) 0.036(5) 0.005(4) 0.012(4) -0.003(3) C214 0.039(5) 0.023(5) 0.029(5) -0.003(4) 0.001(4) -0.004(4) C215 0.041(5) 0.027(5) 0.028(5) 0.000(4) 0.003(4) -0.005(4) C216 0.067(7) 0.022(5) 0.030(6) 0.001(4) 0.006(5) 0.000(4) C217 0.045(5) 0.039(6) 0.027(5) -0.008(5) -0.008(4) 0.001(4) C218 0.038(5) 0.022(5) 0.029(6) 0.005(4) 0.001(4) -0.008(4) C219 0.030(5) 0.024(5) 0.030(5) 0.002(4) 0.009(4) 0.002(4) C220 0.030(5) 0.023(5) 0.028(5) -0.003(4) 0.005(4) 0.002(4) C221 0.017(5) 0.031(6) 0.030(5) -0.006(4) 0.006(4) -0.009(4) C222 0.021(5) 0.029(6) 0.023(5) 0.003(4) 0.003(4) 0.006(4) C223 0.029(6) 0.033(6) 0.037(6) 0.006(5) -0.002(4) -0.005(4) C224 0.040(5) 0.024(5) 0.043(6) 0.011(5) 0.004(4) 0.010(5) C225 0.024(5) 0.037(6) 0.075(8) 0.007(6) 0.010(5) 0.007(4) C226 0.026(5) 0.036(6) 0.049(6) -0.004(5) 0.005(4) 0.009(4) C227 0.018(5) 0.031(5) 0.032(6) -0.003(4) 0.000(4) 0.002(4) C228 0.029(5) 0.018(5) 0.041(6) 0.005(4) -0.002(4) -0.008(4) C229 0.021(5) 0.038(7) 0.091(9) 0.005(6) 0.006(5) 0.000(4) C230 0.033(5) 0.027(6) 0.079(8) 0.007(5) 0.013(5) -0.013(4) C231 0.048(7) 0.026(6) 0.061(8) -0.007(5) 0.001(5) -0.002(5) C232 0.035(5) 0.024(6) 0.040(6) 0.006(5) 0.006(4) -0.007(5) C233 0.026(5) 0.021(6) 0.033(6) 0.000(4) 0.000(4) -0.004(4) C234 0.021(5) 0.026(6) 0.032(6) 0.008(4) 0.009(4) 0.004(4) O1 0.31(2) 0.33(3) 0.35(3) 0.04(2) -0.026(18) 0.16(2) C1 0.21(2) 0.26(2) 0.174(15) 0.163(15) 0.096(14) 0.032(19) C2 0.34(3) 0.22(2) 0.39(4) -0.18(3) -0.07(3) -0.12(2) C3 0.33(3) 0.098(14) 0.21(2) -0.067(14) 0.15(2) -0.067(17) C4 0.50(4) 0.19(3) 0.44(3) -0.19(3) 0.00(3) 0.01(3) C99 0.29(3) 0.14(2) 0.14(2) -0.098(19) -0.15(2) 0.15(2) Cl99 0.142(6) 0.140(5) 0.170(7) -0.004(5) -0.044(5) -0.024(5) Cl98 0.231(9) 0.208(9) 0.263(11) -0.126(8) -0.146(8) 0.096(7) Cl97 0.157(7) 0.307(12) 0.247(12) -0.148(11) -0.052(7) 0.091(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_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.196(2) . ? Pt1 P1 2.201(2) . ? Pt1 Cl2 2.342(2) . ? Pt1 Cl1 2.347(2) . ? P1 O11 1.599(5) . ? P1 O12 1.606(5) . ? P1 C101 1.781(9) . ? P2 O22 1.604(6) . ? P2 O21 1.613(5) . ? P2 C201 1.795(9) . ? O11 C107 1.419(9) . ? O12 C134 1.420(9) . ? O21 C207 1.435(9) . ? O22 C234 1.410(9) . ? C101 C106 1.401(12) . ? C101 C102 1.402(12) . ? C102 C103 1.388(12) . ? C103 C104 1.343(14) . ? C104 C105 1.410(13) . ? C105 C106 1.387(11) . ? C107 C120 1.351(12) . ? C107 C108 1.440(12) . ? C108 C109 1.390(13) . ? C108 C113 1.433(12) . ? C109 C110 1.375(11) . ? C110 C111 1.367(12) . ? C111 C112 1.340(13) . ? C112 C113 1.401(12) . ? C113 C114 1.444(13) . ? C114 C115 1.420(12) . ? C114 C119 1.435(12) . ? C115 C116 1.338(12) . ? C116 C117 1.393(12) . ? C117 C118 1.377(11) . ? C118 C119 1.402(12) . ? C119 C120 1.440(11) . ? C120 C121 1.487(11) . ? C121 C134 1.345(10) . ? C121 C122 1.461(10) . ? C122 C123 1.399(11) . ? C122 C127 1.410(10) . ? C123 C124 1.358(12) . ? C124 C125 1.415(12) . ? C125 C126 1.350(12) . ? C126 C127 1.414(11) . ? C127 C128 1.456(12) . ? C128 C129 1.381(11) . ? C128 C133 1.420(12) . ? C129 C130 1.339(12) . ? C130 C131 1.408(13) . ? C131 C132 1.339(12) . ? C132 C133 1.419(12) . ? C133 C134 1.420(11) . ? C201 C202 1.380(12) . ? C201 C206 1.398(13) . ? C202 C203 1.404(12) . ? C203 C204 1.380(14) . ? C204 C205 1.351(14) . ? C205 C206 1.377(12) . ? C207 C220 1.358(11) . ? C207 C208 1.409(11) . ? C208 C213 1.417(11) . ? C208 C209 1.425(12) . ? C209 C210 1.352(13) . ? C210 C211 1.392(15) . ? C211 C212 1.384(13) . ? C212 C213 1.420(11) . ? C213 C214 1.453(11) . ? C214 C219 1.389(11) . ? C214 C215 1.433(11) . ? C215 C216 1.353(11) . ? C216 C217 1.394(11) . ? C217 C218 1.364(11) . ? C218 C219 1.382(11) . ? C219 C220 1.478(12) . ? C220 C221 1.501(11) . ? C221 C234 1.350(12) . ? C221 C222 1.437(11) . ? C222 C223 1.415(12) . ? C222 C227 1.422(11) . ? C223 C224 1.362(12) . ? C224 C225 1.386(12) . ? C225 C226 1.380(12) . ? C226 C227 1.412(11) . ? C227 C228 1.454(11) . ? C228 C233 1.400(12) . ? C228 C229 1.436(12) . ? C229 C230 1.394(13) . ? C230 C231 1.371(12) . ? C231 C232 1.378(12) . ? C232 C233 1.393(12) . ? C233 C234 1.425(11) . ? O1 C1 1.39(3) . ? O1 C4 1.76(3) . ? C1 C2 1.431(17) . ? C2 C3 1.338(16) . ? C3 C4 1.400(17) . ? C99 Cl98 1.497(19) . ? C99 Cl97 1.54(2) . ? C99 Cl99 1.70(3) . ? 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 P2 Pt1 P1 101.01(8) . . ? P2 Pt1 Cl2 85.14(7) . . ? P1 Pt1 Cl2 173.78(8) . . ? P2 Pt1 Cl1 174.26(8) . . ? P1 Pt1 Cl1 84.66(8) . . ? Cl2 Pt1 Cl1 89.21(8) . . ? O11 P1 O12 102.6(3) . . ? O11 P1 C101 102.3(4) . . ? O12 P1 C101 105.8(4) . . ? O11 P1 Pt1 113.4(2) . . ? O12 P1 Pt1 115.3(2) . . ? C101 P1 Pt1 115.8(3) . . ? O22 P2 O21 103.3(3) . . ? O22 P2 C201 102.6(4) . . ? O21 P2 C201 104.0(4) . . ? O22 P2 Pt1 113.9(2) . . ? O21 P2 Pt1 114.7(2) . . ? C201 P2 Pt1 116.8(3) . . ? C107 O11 P1 116.7(5) . . ? C134 O12 P1 117.7(5) . . ? C207 O21 P2 116.9(5) . . ? C234 O22 P2 116.1(5) . . ? C106 C101 C102 120.2(8) . . ? C106 C101 P1 121.6(7) . . ? C102 C101 P1 118.1(8) . . ? C103 C102 C101 118.3(10) . . ? C104 C103 C102 122.6(10) . . ? C103 C104 C105 119.6(9) . . ? C106 C105 C104 119.8(9) . . ? C105 C106 C101 119.5(9) . . ? C120 C107 O11 118.7(7) . . ? C120 C107 C108 125.6(7) . . ? O11 C107 C108 115.7(7) . . ? C109 C108 C113 120.4(8) . . ? C109 C108 C107 122.9(8) . . ? C113 C108 C107 116.7(8) . . ? C110 C109 C108 120.7(8) . . ? C111 C110 C109 119.3(9) . . ? C112 C111 C110 121.2(8) . . ? C111 C112 C113 123.3(8) . . ? C112 C113 C108 115.2(9) . . ? C112 C113 C114 125.2(8) . . ? C108 C113 C114 119.6(8) . . ? C115 C114 C119 117.9(9) . . ? C115 C114 C113 122.1(8) . . ? C119 C114 C113 120.0(8) . . ? C116 C115 C114 122.3(9) . . ? C115 C116 C117 120.2(9) . . ? C118 C117 C116 120.0(9) . . ? C117 C118 C119 121.7(9) . . ? C118 C119 C114 117.8(8) . . ? C118 C119 C120 122.3(8) . . ? C114 C119 C120 119.9(8) . . ? C107 C120 C119 118.1(7) . . ? C107 C120 C121 119.0(7) . . ? C119 C120 C121 122.8(8) . . ? C134 C121 C122 117.1(7) . . ? C134 C121 C120 120.8(7) . . ? C122 C121 C120 122.1(7) . . ? C123 C122 C127 119.4(7) . . ? C123 C122 C121 121.1(7) . . ? C127 C122 C121 119.4(7) . . ? C124 C123 C122 121.4(8) . . ? C123 C124 C125 120.2(8) . . ? C126 C125 C124 118.5(8) . . ? C125 C126 C127 123.2(8) . . ? C122 C127 C126 117.2(8) . . ? C122 C127 C128 121.2(7) . . ? C126 C127 C128 121.6(7) . . ? C129 C128 C133 116.9(8) . . ? C129 C128 C127 125.0(8) . . ? C133 C128 C127 118.2(7) . . ? C130 C129 C128 123.5(9) . . ? C129 C130 C131 119.9(9) . . ? C132 C131 C130 119.3(9) . . ? C131 C132 C133 121.4(9) . . ? C132 C133 C128 119.0(8) . . ? C132 C133 C134 123.4(8) . . ? C128 C133 C134 117.7(8) . . ? C121 C134 O12 118.4(7) . . ? C121 C134 C133 126.2(8) . . ? O12 C134 C133 115.4(7) . . ? C202 C201 C206 119.3(9) . . ? C202 C201 P2 121.8(7) . . ? C206 C201 P2 118.4(8) . . ? C201 C202 C203 119.0(9) . . ? C204 C203 C202 120.1(10) . . ? C205 C204 C203 120.9(9) . . ? C204 C205 C206 119.8(10) . . ? C205 C206 C201 120.8(10) . . ? C220 C207 C208 125.5(8) . . ? C220 C207 O21 117.7(7) . . ? C208 C207 O21 116.7(7) . . ? C207 C208 C213 117.7(8) . . ? C207 C208 C209 121.6(8) . . ? C213 C208 C209 120.6(8) . . ? C210 C209 C208 119.2(9) . . ? C209 C210 C211 121.7(10) . . ? C212 C211 C210 120.4(9) . . ? C211 C212 C213 120.4(9) . . ? C208 C213 C212 117.7(8) . . ? C208 C213 C214 118.8(7) . . ? C212 C213 C214 123.4(8) . . ? C219 C214 C215 117.5(8) . . ? C219 C214 C213 121.0(8) . . ? C215 C214 C213 121.5(7) . . ? C216 C215 C214 119.8(8) . . ? C215 C216 C217 121.7(8) . . ? C218 C217 C216 119.1(8) . . ? C217 C218 C219 120.6(8) . . ? C218 C219 C214 121.2(8) . . ? C218 C219 C220 119.2(7) . . ? C214 C219 C220 119.4(8) . . ? C207 C220 C219 116.8(7) . . ? C207 C220 C221 120.1(8) . . ? C219 C220 C221 123.1(8) . . ? C234 C221 C222 119.9(7) . . ? C234 C221 C220 118.3(8) . . ? C222 C221 C220 121.9(8) . . ? C223 C222 C227 120.0(8) . . ? C223 C222 C221 121.3(8) . . ? C227 C222 C221 118.6(8) . . ? C224 C223 C222 119.6(9) . . ? C223 C224 C225 122.2(10) . . ? C226 C225 C224 118.7(9) . . ? C225 C226 C227 122.2(9) . . ? C226 C227 C222 117.1(9) . . ? C226 C227 C228 123.0(8) . . ? C222 C227 C228 119.8(7) . . ? C233 C228 C229 118.9(8) . . ? C233 C228 C227 120.0(7) . . ? C229 C228 C227 121.1(8) . . ? C230 C229 C228 118.9(8) . . ? C231 C230 C229 120.9(8) . . ? C230 C231 C232 120.8(9) . . ? C231 C232 C233 120.4(8) . . ? C232 C233 C228 120.0(8) . . ? C232 C233 C234 122.1(8) . . ? C228 C233 C234 117.9(8) . . ? C221 C234 O22 119.3(7) . . ? C221 C234 C233 123.8(8) . . ? O22 C234 C233 116.9(8) . . ? C1 O1 C4 91.7(13) . . ? O1 C1 C2 106.2(16) . . ? C3 C2 C1 103.8(13) . . ? C2 C3 C4 114.8(16) . . ? C3 C4 O1 93.4(12) . . ? Cl98 C99 Cl97 118.0(14) . . ? Cl98 C99 Cl99 113.1(16) . . ? Cl97 C99 Cl99 114.7(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.313 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.108 data_S,S-8.3thf.2CHCl3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H50 Cl8 O7 P2 Pt' _chemical_formula_weight 1567.75 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' 'Pt' 'Pt' -1.7033 8.3905 '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 14.8155(16) _cell_length_b 19.132(3) _cell_length_c 23.690(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6714.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 275 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'Not measured' _exptl_crystal_F_000 3128 _exptl_absorpt_coefficient_mu 2.510 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.585651 _exptl_absorpt_correction_T_max 0.694170 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 32962 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.00 _reflns_number_total 10534 _reflns_number_gt 8197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXTL (Siemens, 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _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^)+(0.0522P)^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 mixed _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 0.000(7) _refine_ls_number_reflns 10534 _refine_ls_number_parameters 767 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.002 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 Pt1 Pt -1.10432(2) -1.40181(2) 0.412087(15) 0.02438(10) Uani 1 1 d . . . P1 P -1.21642(14) -1.40653(15) 0.35203(9) 0.0212(5) Uani 1 1 d . . . P2 P -1.03073(16) -1.34744(13) 0.34550(10) 0.0223(6) Uani 1 1 d . . . Cl1 Cl -0.98368(17) -1.38878(16) 0.47565(10) 0.0432(8) Uani 1 1 d . . . Cl2 Cl -1.18272(19) -1.47161(17) 0.47652(11) 0.0466(8) Uani 1 1 d . . . O1 O -1.3175(4) -1.3867(3) 0.3697(2) 0.0239(15) Uani 1 1 d . . . O2 O -1.2259(4) -1.4842(3) 0.3262(2) 0.0225(15) Uani 1 1 d . . . O3 O -1.0017(4) -1.2683(3) 0.3599(2) 0.0238(15) Uani 1 1 d . . . O4 O -0.9380(4) -1.3829(3) 0.3231(3) 0.0237(16) Uani 1 1 d . . . C1 C -1.1969(6) -1.3469(6) 0.2943(4) 0.030(2) Uani 1 1 d . . . H1A H -1.2321 -1.3617 0.2608 0.037 Uiso 1 1 calc R . . H1B H -1.2163 -1.2992 0.3050 0.037 Uiso 1 1 calc R . . C2 C -1.0948(6) -1.3471(5) 0.2801(3) 0.023(2) Uani 1 1 d . . . H2A H -1.0794 -1.3051 0.2577 0.028 Uiso 1 1 calc R . . H2B H -1.0797 -1.3890 0.2575 0.028 Uiso 1 1 calc R . . C3 C -1.3711(5) -1.4360(4) 0.3989(3) 0.019(2) Uani 1 1 d . . . C4 C -1.3955(6) -1.4172(4) 0.4553(3) 0.020(2) Uani 1 1 d . . . C5 C -1.3759(6) -1.3513(5) 0.4782(4) 0.025(2) Uani 1 1 d . . . H5 H -1.3401 -1.3190 0.4576 0.030 Uiso 1 1 calc R . . C6 C -1.4086(7) -1.3337(5) 0.5305(4) 0.028(2) Uani 1 1 d . . . H6 H -1.3945 -1.2894 0.5464 0.033 Uiso 1 1 calc R . . C7 C -1.4613(7) -1.3797(5) 0.5599(4) 0.032(3) Uani 1 1 d . . . H7 H -1.4854 -1.3662 0.5954 0.039 Uiso 1 1 calc R . . C8 C -1.4801(6) -1.4448(5) 0.5390(4) 0.031(3) Uani 1 1 d . . . H8 H -1.5161 -1.4762 0.5604 0.037 Uiso 1 1 calc R . . C9 C -1.4459(6) -1.4658(5) 0.4853(4) 0.024(2) Uani 1 1 d . . . C10 C -1.4641(6) -1.5353(5) 0.4614(4) 0.023(2) Uani 1 1 d . . . C11 C -1.4993(6) -1.5919(6) 0.4938(4) 0.034(2) Uani 1 1 d . . . H11 H -1.5110 -1.5849 0.5328 0.041 Uiso 1 1 calc R . . C12 C -1.5166(8) -1.6549(6) 0.4710(5) 0.044(3) Uani 1 1 d . . . H12 H -1.5398 -1.6915 0.4939 0.053 Uiso 1 1 calc R . . C13 C -1.5000(6) -1.6667(5) 0.4123(5) 0.039(3) Uani 1 1 d . . . H13 H -1.5142 -1.7105 0.3956 0.047 Uiso 1 1 calc R . . C14 C -1.4632(6) -1.6136(5) 0.3800(4) 0.029(3) Uani 1 1 d . . . H14 H -1.4499 -1.6219 0.3413 0.035 Uiso 1 1 calc R . . C15 C -1.4451(6) -1.5471(5) 0.4035(4) 0.021(2) Uani 1 1 d . . . C16 C -1.4017(6) -1.4936(4) 0.3703(4) 0.023(2) Uani 1 1 d . . . C17 C -1.2969(6) -1.4983(5) 0.2892(4) 0.021(2) Uani 1 1 d . . . C18 C -1.2723(6) -1.5085(4) 0.2315(4) 0.020(2) Uani 1 1 d . . . C19 C -1.1823(7) -1.5097(5) 0.2138(4) 0.025(2) Uani 1 1 d . . . H19 H -1.1358 -1.5032 0.2409 0.030 Uiso 1 1 calc R . . C20 C -1.1595(7) -1.5199(5) 0.1587(4) 0.030(2) Uani 1 1 d . . . H20 H -1.0979 -1.5212 0.1477 0.036 Uiso 1 1 calc R . . C21 C -1.2298(7) -1.5287(5) 0.1172(4) 0.034(3) Uani 1 1 d . . . H21 H -1.2150 -1.5362 0.0787 0.041 Uiso 1 1 calc R . . C22 C -1.3168(7) -1.5260(5) 0.1337(4) 0.027(2) Uani 1 1 d . . . H22 H -1.3627 -1.5305 0.1060 0.032 Uiso 1 1 calc R . . C23 C -1.3424(7) -1.5169(5) 0.1908(4) 0.026(2) Uani 1 1 d . . . C24 C -1.4357(7) -1.5151(5) 0.2102(4) 0.026(2) Uani 1 1 d . . . C25 C -1.5107(7) -1.5207(5) 0.1730(4) 0.035(3) Uani 1 1 d . . . H25 H -1.4997 -1.5272 0.1338 0.042 Uiso 1 1 calc R . . C26 C -1.5964(8) -1.5171(6) 0.1910(4) 0.044(3) Uani 1 1 d . . . H26 H -1.6442 -1.5208 0.1645 0.053 Uiso 1 1 calc R . . C27 C -1.6165(8) -1.5081(5) 0.2485(4) 0.039(3) Uani 1 1 d . . . H27 H -1.6773 -1.5046 0.2607 0.047 Uiso 1 1 calc R . . C28 C -1.5473(7) -1.5043(6) 0.2866(4) 0.037(3) Uani 1 1 d . . . H28 H -1.5607 -1.4980 0.3255 0.045 Uiso 1 1 calc R . . C29 C -1.4556(6) -1.5098(5) 0.2690(4) 0.026(2) Uani 1 1 d . . . C30 C -1.3835(7) -1.5022(4) 0.3094(3) 0.023(2) Uani 1 1 d . . . C31 C -0.9560(6) -1.2326(5) 0.3160(4) 0.023(2) Uani 1 1 d . . . C32 C -1.0075(6) -1.1784(5) 0.2889(4) 0.026(2) Uani 1 1 d . . . C33 C -1.0946(7) -1.1591(5) 0.3081(4) 0.027(2) Uani 1 1 d . . . H33 H -1.1229 -1.1846 0.3376 0.033 Uiso 1 1 calc R . . C34 C -1.1369(6) -1.1044(6) 0.2842(4) 0.039(3) Uani 1 1 d . . . H34 H -1.1951 -1.0909 0.2972 0.047 Uiso 1 1 calc R . . C35 C -1.0946(9) -1.0664(6) 0.2395(5) 0.055(3) Uani 1 1 d . . . H35 H -1.1238 -1.0267 0.2238 0.066 Uiso 1 1 calc R . . C36 C -1.0143(7) -1.0865(6) 0.2198(4) 0.042(3) Uani 1 1 d . . . H36 H -0.9889 -1.0621 0.1887 0.050 Uiso 1 1 calc R . . C37 C -0.9666(7) -1.1419(5) 0.2434(4) 0.029(2) Uani 1 1 d . . . C38 C -0.8786(7) -1.1661(5) 0.2222(4) 0.029(3) Uani 1 1 d . . . C39 C -0.8412(7) -1.1397(5) 0.1728(4) 0.029(2) Uani 1 1 d . . . H39 H -0.8733 -1.1054 0.1519 0.035 Uiso 1 1 calc R . . C40 C -0.7584(7) -1.1623(6) 0.1536(4) 0.042(3) Uani 1 1 d . . . H40 H -0.7340 -1.1436 0.1197 0.051 Uiso 1 1 calc R . . C41 C -0.7102(7) -1.2126(6) 0.1837(4) 0.044(3) Uani 1 1 d . . . H41 H -0.6531 -1.2282 0.1705 0.053 Uiso 1 1 calc R . . C42 C -0.7459(7) -1.2394(5) 0.2325(4) 0.034(3) Uani 1 1 d . . . H42 H -0.7127 -1.2735 0.2529 0.041 Uiso 1 1 calc R . . C43 C -0.8303(7) -1.2178(5) 0.2532(4) 0.028(2) Uani 1 1 d . . . C44 C -0.8700(6) -1.2490(5) 0.3039(4) 0.027(2) Uani 1 1 d . . . C45 C -0.8546(6) -1.3675(5) 0.3463(4) 0.028(2) Uani 1 1 d . . . C46 C -0.8083(7) -1.4225(5) 0.3742(4) 0.027(3) Uani 1 1 d . . . C47 C -0.8451(7) -1.4866(5) 0.3833(4) 0.029(2) Uani 1 1 d . . . H47 H -0.9063 -1.4939 0.3729 0.034 Uiso 1 1 calc R . . C48 C -0.7985(7) -1.5416(5) 0.4068(5) 0.039(3) Uani 1 1 d . . . H48 H -0.8267 -1.5856 0.4127 0.047 Uiso 1 1 calc R . . C49 C -0.7087(7) -1.5307(5) 0.4216(4) 0.037(3) Uani 1 1 d . . . H49 H -0.6741 -1.5685 0.4359 0.044 Uiso 1 1 calc R . . C50 C -0.6687(6) -1.4654(5) 0.4158(4) 0.031(2) Uani 1 1 d . . . H50 H -0.6080 -1.4587 0.4275 0.038 Uiso 1 1 calc R . . C51 C -0.7178(6) -1.4091(6) 0.3926(4) 0.027(2) Uani 1 1 d . . . C52 C -0.6814(6) -1.3383(5) 0.3907(4) 0.021(2) Uani 1 1 d . . . C53 C -0.5983(7) -1.3198(5) 0.4165(4) 0.033(2) Uani 1 1 d . . . H53 H -0.5617 -1.3551 0.4329 0.040 Uiso 1 1 calc R . . C54 C -0.5706(6) -1.2517(6) 0.4179(5) 0.041(3) Uani 1 1 d . . . H54 H -0.5144 -1.2402 0.4349 0.049 Uiso 1 1 calc R . . C55 C -0.6226(6) -1.1999(6) 0.3950(4) 0.042(3) Uani 1 1 d . . . H55 H -0.6039 -1.1526 0.3984 0.050 Uiso 1 1 calc R . . C56 C -0.7026(7) -1.2154(5) 0.3669(4) 0.035(3) Uani 1 1 d . . . H56 H -0.7359 -1.1791 0.3491 0.042 Uiso 1 1 calc R . . C57 C -0.7345(7) -1.2854(6) 0.3646(4) 0.032(3) Uani 1 1 d . . . C58 C -0.8201(6) -1.3018(5) 0.3378(4) 0.024(2) Uani 1 1 d . . . Cl3 Cl -0.5987(4) -1.4142(4) 0.0414(2) 0.178(3) Uani 1 1 d . . . Cl4 Cl -0.4219(5) -1.3689(3) 0.0647(3) 0.175(3) Uani 1 1 d . . . Cl5 Cl -0.4869(4) -1.3629(3) -0.0464(2) 0.1281(18) Uani 1 1 d . . . C100 C -0.4960(10) -1.4094(8) 0.0168(6) 0.080(4) Uani 1 1 d . . . H100 H -0.4739 -1.4580 0.0099 0.096 Uiso 1 1 calc R . . Cl6 Cl -0.2124(4) -0.2396(3) 0.04672(19) 0.123(2) Uani 1 1 d . . . Cl7 Cl -0.1609(5) -0.2174(3) 0.1607(2) 0.149(3) Uani 1 1 d . . . Cl8 Cl -0.1970(4) -0.3559(2) 0.1224(2) 0.1204(18) Uani 1 1 d . . . C101 C -0.2245(2) -0.26940(18) 0.11399(13) 0.100(6) Uani 1 1 d . . . H101 H -0.2895 -0.2640 0.1245 0.120 Uiso 1 1 calc R . . O79 O -0.4036(2) -1.16512(18) -0.13032(13) 0.209(8) Uani 1 1 d R . . C75 C -0.3133(2) -1.14733(18) -0.09205(13) 0.080(4) Uani 1 1 d R . . H75 H -0.2768 -1.1760 -0.0685 0.097 Uiso 1 1 calc R . . C76 C -0.3074(2) -1.06967(18) -0.10688(13) 0.148(9) Uani 1 1 d R . . H76 H -0.2565 -1.0405 -0.1007 0.178 Uiso 1 1 calc R . . C77 C -0.3878(2) -1.04900(18) -0.13064(13) 0.100(6) Uani 1 1 d R . . H77 H -0.4183 -1.0065 -0.1224 0.120 Uiso 1 1 calc R . . C78 C -0.4160(2) -1.09633(18) -0.16626(13) 0.195(14) Uani 1 1 d R . . H78 H -0.4381 -1.0908 -0.2037 0.234 Uiso 1 1 calc R . . O89 O -0.7659(2) -0.73825(18) 0.10060(13) 0.045(2) Uani 1 1 d R . . C85 C -0.6908(2) -0.69165(18) 0.11330(13) 0.066(4) Uani 1 1 d R . . H85 H -0.6414 -0.6999 0.1380 0.079 Uiso 1 1 calc R . . C86 C -0.7092(2) -0.62723(18) 0.07831(13) 0.102(6) Uani 1 1 d R . . H86 H -0.6894 -0.5811 0.0863 0.123 Uiso 1 1 calc R . . C87 C -0.7617(2) -0.64856(18) 0.03114(13) 0.130(8) Uani 1 1 d R . . H87 H -0.7674 -0.6249 -0.0039 0.156 Uiso 1 1 calc R . . C88 C -0.8078(2) -0.71791(18) 0.04815(13) 0.043(3) Uani 1 1 d R . . H88 H -0.8540 -0.7420 0.0283 0.052 Uiso 1 1 calc R . . O99 O -1.6016(2) -1.77122(18) 0.30510(13) 0.103(4) Uani 1 1 d R . . C95 C -1.6043(2) -1.71046(18) 0.27102(13) 0.068(4) Uani 1 1 d R . . H95 H -1.6472 -1.6736 0.2721 0.082 Uiso 1 1 calc R . . C96 C -1.5233(2) -1.71758(18) 0.23242(13) 0.073(4) Uani 1 1 d R . . H96 H -1.4855 -1.6819 0.2176 0.088 Uiso 1 1 calc R . . C97 C -1.5175(2) -1.79580(18) 0.22340(13) 0.084(5) Uani 1 1 d R . . H97 H -1.4971 -1.8207 0.1911 0.101 Uiso 1 1 calc R . . C98 C -1.5532(2) -1.82503(18) 0.28002(13) 0.082(5) Uani 1 1 d R . . H98 H -1.5438 -1.8707 0.2947 0.099 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 Pt1 0.02069(17) 0.03498(19) 0.01747(16) 0.0003(2) -0.00203(19) 0.0029(2) P1 0.0176(12) 0.0271(14) 0.0189(12) 0.0007(13) 0.0001(10) -0.0036(13) P2 0.0165(13) 0.0300(15) 0.0205(13) -0.0042(11) -0.0031(11) -0.0008(11) Cl1 0.0306(14) 0.070(2) 0.0293(14) -0.0088(14) -0.0120(11) 0.0118(15) Cl2 0.0307(16) 0.076(2) 0.0327(15) 0.0277(15) 0.0056(13) 0.0099(15) O1 0.017(3) 0.026(4) 0.029(3) 0.003(3) 0.001(3) 0.002(3) O2 0.025(4) 0.027(4) 0.016(3) -0.006(3) 0.002(3) 0.001(3) O3 0.022(4) 0.026(4) 0.024(4) -0.003(3) 0.000(3) -0.002(3) O4 0.016(3) 0.023(4) 0.033(4) 0.000(3) 0.007(3) 0.000(3) C1 0.028(6) 0.047(7) 0.016(5) 0.007(5) 0.001(5) -0.012(5) C2 0.023(5) 0.028(5) 0.018(5) -0.006(4) -0.015(5) -0.001(5) C3 0.018(5) 0.019(5) 0.018(5) 0.006(4) 0.007(4) -0.002(4) C4 0.015(4) 0.026(6) 0.020(4) 0.000(4) -0.013(5) -0.003(5) C5 0.022(6) 0.028(5) 0.026(5) 0.008(4) -0.004(4) 0.000(4) C6 0.030(6) 0.031(6) 0.022(5) -0.011(4) 0.003(5) 0.005(5) C7 0.038(6) 0.036(7) 0.023(5) 0.002(5) -0.004(5) 0.011(5) C8 0.026(6) 0.030(6) 0.036(6) 0.003(5) 0.008(5) -0.006(5) C9 0.020(5) 0.040(6) 0.013(5) 0.003(5) -0.005(4) 0.007(5) C10 0.014(5) 0.024(6) 0.031(6) 0.002(5) 0.001(4) -0.001(4) C11 0.033(6) 0.037(7) 0.031(5) 0.007(6) 0.000(4) -0.002(6) C12 0.058(8) 0.034(7) 0.041(7) 0.008(6) 0.003(6) -0.001(6) C13 0.030(6) 0.042(6) 0.046(6) -0.006(6) -0.005(6) -0.012(5) C14 0.021(5) 0.035(7) 0.032(6) 0.011(5) 0.007(4) -0.003(5) C15 0.012(5) 0.031(6) 0.020(6) -0.006(5) 0.001(4) 0.005(4) C16 0.008(5) 0.028(5) 0.032(5) 0.004(4) 0.001(5) 0.003(5) C17 0.023(6) 0.021(5) 0.017(5) -0.001(4) -0.006(4) 0.004(4) C18 0.017(5) 0.014(5) 0.028(5) 0.009(4) 0.008(4) -0.001(4) C19 0.023(6) 0.023(6) 0.029(6) -0.004(4) -0.010(5) -0.001(4) C20 0.031(6) 0.033(6) 0.028(6) -0.004(5) 0.002(5) 0.002(5) C21 0.049(7) 0.029(7) 0.025(6) -0.009(5) 0.013(6) -0.001(5) C22 0.040(7) 0.025(6) 0.015(5) -0.004(4) 0.001(5) -0.004(5) C23 0.031(6) 0.020(6) 0.027(6) -0.002(5) -0.006(5) 0.000(5) C24 0.032(6) 0.022(6) 0.025(6) 0.000(4) -0.006(5) -0.001(4) C25 0.032(7) 0.049(7) 0.024(6) -0.009(5) -0.005(5) -0.012(5) C26 0.028(6) 0.062(8) 0.043(7) 0.002(6) -0.016(6) -0.018(7) C27 0.028(6) 0.056(7) 0.033(6) -0.004(5) 0.001(6) 0.001(6) C28 0.031(7) 0.046(7) 0.035(7) -0.003(5) -0.002(5) -0.006(5) C29 0.024(6) 0.022(6) 0.032(6) 0.000(5) 0.005(5) -0.006(4) C30 0.030(6) 0.023(5) 0.016(5) 0.004(4) 0.002(5) 0.004(5) C31 0.030(6) 0.017(5) 0.021(5) 0.005(4) 0.002(5) -0.001(4) C32 0.027(6) 0.022(6) 0.028(6) -0.006(4) -0.011(5) 0.004(5) C33 0.028(6) 0.034(6) 0.020(5) -0.002(4) 0.001(5) 0.000(5) C34 0.028(6) 0.053(7) 0.036(6) 0.000(6) -0.005(4) 0.023(6) C35 0.052(8) 0.052(7) 0.061(8) 0.023(6) 0.004(7) 0.027(7) C36 0.039(7) 0.057(9) 0.029(6) 0.004(6) -0.010(5) 0.002(6) C37 0.038(6) 0.040(7) 0.010(5) 0.003(5) -0.002(5) 0.002(5) C38 0.034(7) 0.019(5) 0.035(6) -0.004(4) -0.005(5) 0.002(5) C39 0.032(6) 0.022(6) 0.034(6) 0.005(5) 0.000(5) -0.002(5) C40 0.043(7) 0.051(8) 0.032(6) 0.015(6) -0.008(6) -0.012(6) C41 0.034(7) 0.062(8) 0.037(7) 0.007(6) 0.008(6) 0.010(6) C42 0.033(6) 0.038(7) 0.033(6) 0.002(5) -0.009(5) -0.004(5) C43 0.024(6) 0.030(6) 0.029(6) -0.006(5) 0.000(5) -0.009(5) C44 0.018(6) 0.030(6) 0.034(6) -0.012(5) -0.009(4) -0.006(4) C45 0.013(5) 0.039(7) 0.031(6) -0.008(5) -0.001(5) -0.012(5) C46 0.026(6) 0.040(7) 0.016(5) 0.006(4) 0.008(4) 0.001(5) C47 0.029(6) 0.029(6) 0.028(6) -0.003(5) 0.001(5) 0.000(5) C48 0.041(7) 0.036(6) 0.040(6) -0.007(6) 0.002(6) 0.000(5) C49 0.044(7) 0.028(6) 0.039(7) 0.003(5) -0.009(6) 0.019(5) C50 0.029(6) 0.029(6) 0.036(6) -0.007(6) -0.013(6) 0.010(4) C51 0.030(5) 0.025(6) 0.026(5) 0.002(5) 0.005(4) 0.000(5) C52 0.016(5) 0.020(5) 0.028(5) 0.006(4) 0.008(4) 0.006(4) C53 0.021(5) 0.038(6) 0.040(6) 0.011(5) 0.000(6) 0.005(5) C54 0.025(5) 0.050(7) 0.048(7) 0.008(6) -0.006(6) -0.008(5) C55 0.030(7) 0.038(6) 0.056(7) 0.008(5) -0.016(5) -0.006(5) C56 0.040(7) 0.030(6) 0.035(6) 0.012(5) -0.008(5) -0.010(5) C57 0.030(6) 0.038(7) 0.027(6) -0.007(5) 0.001(5) -0.010(5) C58 0.015(5) 0.030(6) 0.026(5) -0.004(5) -0.006(4) 0.001(5) Cl3 0.121(4) 0.287(8) 0.125(4) 0.047(5) 0.020(4) 0.047(7) Cl4 0.201(7) 0.161(6) 0.163(5) -0.035(4) -0.080(5) -0.018(5) Cl5 0.131(4) 0.154(5) 0.099(4) 0.010(3) 0.023(3) -0.003(4) C100 0.101(12) 0.054(9) 0.084(10) -0.009(9) 0.021(9) 0.006(9) Cl6 0.175(5) 0.116(4) 0.078(3) 0.019(3) -0.025(3) -0.053(4) Cl7 0.277(8) 0.082(3) 0.090(3) 0.008(3) -0.061(4) -0.034(4) Cl8 0.165(5) 0.054(3) 0.141(4) 0.000(3) -0.014(4) 0.001(3) C101 0.150(17) 0.061(11) 0.089(12) -0.015(9) 0.032(12) -0.043(11) O79 0.33(2) 0.166(14) 0.134(12) -0.058(11) 0.016(16) 0.119(17) C75 0.069(9) 0.101(12) 0.072(10) -0.015(10) -0.010(10) 0.019(9) C76 0.115(16) 0.087(14) 0.24(3) 0.010(16) -0.013(18) -0.044(12) C77 0.159(17) 0.070(11) 0.070(10) 0.020(8) -0.004(13) 0.046(13) C78 0.40(4) 0.116(16) 0.071(12) -0.036(12) -0.102(18) 0.09(3) O89 0.049(5) 0.052(5) 0.034(5) 0.010(4) -0.001(4) 0.005(4) C85 0.044(8) 0.084(11) 0.069(9) -0.028(8) -0.021(7) 0.002(7) C86 0.138(15) 0.111(13) 0.058(10) 0.011(9) -0.001(10) -0.090(12) C87 0.173(19) 0.109(14) 0.108(14) 0.068(12) -0.066(14) -0.094(14) C88 0.046(7) 0.056(8) 0.027(6) 0.018(5) -0.014(5) -0.001(6) O99 0.177(11) 0.060(6) 0.072(6) 0.001(5) 0.036(9) 0.007(8) C95 0.083(10) 0.050(8) 0.072(9) 0.011(7) 0.004(10) 0.005(9) C96 0.064(10) 0.076(11) 0.079(10) 0.012(9) -0.014(8) -0.021(8) C97 0.097(13) 0.087(12) 0.069(10) -0.011(9) 0.016(9) -0.005(10) C98 0.119(13) 0.049(9) 0.079(11) -0.010(8) 0.014(10) 0.037(9) _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 Pt1 P2 2.181(3) . ? Pt1 P1 2.189(2) . ? Pt1 Cl2 2.337(3) . ? Pt1 Cl1 2.350(2) . ? P1 O1 1.600(6) . ? P1 O2 1.612(6) . ? P1 C1 1.804(9) . ? P2 O3 1.610(6) . ? P2 O4 1.621(6) . ? P2 C2 1.817(8) . ? O1 C3 1.414(9) . ? O2 C17 1.397(10) . ? O3 C31 1.416(10) . ? O4 C45 1.385(10) . ? C1 C2 1.549(13) . ? C3 C16 1.370(12) . ? C3 C4 1.430(12) . ? C4 C9 1.388(12) . ? C4 C5 1.403(12) . ? C5 C6 1.372(12) . ? C6 C7 1.367(13) . ? C7 C8 1.368(13) . ? C8 C9 1.427(12) . ? C9 C10 1.470(13) . ? C10 C15 1.417(13) . ? C10 C11 1.427(13) . ? C11 C12 1.345(14) . ? C12 C13 1.431(15) . ? C13 C14 1.384(13) . ? C14 C15 1.414(12) . ? C15 C16 1.444(12) . ? C16 C30 1.476(12) . ? C17 C30 1.371(13) . ? C17 C18 1.427(12) . ? C18 C19 1.398(13) . ? C18 C23 1.425(13) . ? C19 C20 1.363(12) . ? C20 C21 1.442(13) . ? C21 C22 1.348(13) . ? C22 C23 1.416(13) . ? C23 C24 1.456(13) . ? C24 C25 1.423(13) . ? C24 C29 1.427(13) . ? C25 C26 1.341(15) . ? C26 C27 1.404(14) . ? C27 C28 1.367(14) . ? C28 C29 1.426(13) . ? C29 C30 1.443(13) . ? C31 C44 1.344(13) . ? C31 C32 1.439(13) . ? C32 C33 1.417(14) . ? C32 C37 1.421(13) . ? C33 C34 1.345(13) . ? C34 C35 1.429(15) . ? C35 C36 1.335(15) . ? C36 C37 1.392(14) . ? C37 C38 1.472(14) . ? C38 C39 1.391(13) . ? C38 C43 1.425(13) . ? C39 C40 1.378(14) . ? C40 C41 1.395(14) . ? C41 C42 1.371(14) . ? C42 C43 1.404(14) . ? C43 C44 1.465(13) . ? C44 C58 1.487(13) . ? C45 C58 1.371(13) . ? C45 C46 1.418(13) . ? C46 C47 1.360(13) . ? C46 C51 1.433(13) . ? C47 C48 1.375(13) . ? C48 C49 1.392(13) . ? C49 C50 1.388(13) . ? C50 C51 1.413(13) . ? C51 C52 1.459(13) . ? C52 C53 1.418(13) . ? C52 C57 1.423(13) . ? C53 C54 1.367(13) . ? C54 C55 1.367(13) . ? C55 C56 1.391(13) . ? C56 C57 1.421(14) . ? C57 C58 1.452(13) . ? Cl3 C100 1.631(15) . ? Cl4 C100 1.760(15) . ? Cl5 C100 1.746(15) . ? Cl6 C101 1.702(5) . ? Cl7 C101 1.762(6) . ? Cl8 C101 1.717(6) . ? O79 C78 1.5783 . ? O79 C75 1.6524 . ? C75 C76 1.5292 . ? C76 C77 1.3763 . ? C77 C78 1.3066 . ? O89 C88 1.4428 . ? O89 C85 1.4570 . ? C85 C86 1.5103 . ? C86 C87 1.4212 . ? C87 C88 1.5460 . ? O99 C98 1.3885 . ? O99 C95 1.4158 . ? C95 C96 1.5150 . ? C96 C97 1.5141 . ? C97 C98 1.5463 . ? 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 P2 Pt1 P1 85.92(9) . . ? P2 Pt1 Cl2 173.25(11) . . ? P1 Pt1 Cl2 91.37(9) . . ? P2 Pt1 Cl1 91.87(9) . . ? P1 Pt1 Cl1 176.25(11) . . ? Cl2 Pt1 Cl1 91.15(10) . . ? O1 P1 O2 103.7(3) . . ? O1 P1 C1 101.5(4) . . ? O2 P1 C1 108.0(4) . . ? O1 P1 Pt1 122.0(2) . . ? O2 P1 Pt1 110.5(3) . . ? C1 P1 Pt1 110.2(3) . . ? O3 P2 O4 103.6(3) . . ? O3 P2 C2 108.5(4) . . ? O4 P2 C2 99.5(4) . . ? O3 P2 Pt1 115.4(2) . . ? O4 P2 Pt1 117.4(2) . . ? C2 P2 Pt1 110.9(3) . . ? C3 O1 P1 119.7(5) . . ? C17 O2 P1 118.8(6) . . ? C31 O3 P2 115.2(5) . . ? C45 O4 P2 122.5(5) . . ? C2 C1 P1 108.6(6) . . ? C1 C2 P2 109.0(6) . . ? C16 C3 O1 118.7(7) . . ? C16 C3 C4 125.5(8) . . ? O1 C3 C4 115.5(7) . . ? C9 C4 C5 121.0(8) . . ? C9 C4 C3 116.5(7) . . ? C5 C4 C3 122.4(8) . . ? C6 C5 C4 119.8(9) . . ? C7 C6 C5 120.2(9) . . ? C6 C7 C8 121.3(10) . . ? C7 C8 C9 120.4(9) . . ? C4 C9 C8 117.3(9) . . ? C4 C9 C10 120.4(8) . . ? C8 C9 C10 122.2(9) . . ? C15 C10 C11 118.1(9) . . ? C15 C10 C9 118.8(8) . . ? C11 C10 C9 123.1(9) . . ? C12 C11 C10 122.2(9) . . ? C11 C12 C13 120.0(10) . . ? C14 C13 C12 119.3(10) . . ? C13 C14 C15 121.1(9) . . ? C14 C15 C10 119.2(8) . . ? C14 C15 C16 120.5(8) . . ? C10 C15 C16 120.1(8) . . ? C3 C16 C15 116.7(8) . . ? C3 C16 C30 120.8(8) . . ? C15 C16 C30 122.3(8) . . ? C30 C17 O2 119.6(8) . . ? C30 C17 C18 124.5(8) . . ? O2 C17 C18 115.8(8) . . ? C19 C18 C23 119.4(8) . . ? C19 C18 C17 122.2(9) . . ? C23 C18 C17 118.4(8) . . ? C20 C19 C18 121.7(9) . . ? C19 C20 C21 119.4(9) . . ? C22 C21 C20 119.2(9) . . ? C21 C22 C23 122.6(10) . . ? C22 C23 C18 117.7(9) . . ? C22 C23 C24 123.9(9) . . ? C18 C23 C24 118.4(8) . . ? C25 C24 C29 116.6(9) . . ? C25 C24 C23 123.0(9) . . ? C29 C24 C23 120.4(9) . . ? C26 C25 C24 122.5(10) . . ? C25 C26 C27 121.1(11) . . ? C28 C27 C26 119.2(11) . . ? C27 C28 C29 121.1(10) . . ? C28 C29 C24 119.3(9) . . ? C28 C29 C30 120.2(9) . . ? C24 C29 C30 120.2(9) . . ? C17 C30 C29 117.7(8) . . ? C17 C30 C16 120.5(9) . . ? C29 C30 C16 121.6(9) . . ? C44 C31 O3 119.8(9) . . ? C44 C31 C32 125.2(9) . . ? O3 C31 C32 114.9(8) . . ? C33 C32 C37 120.3(9) . . ? C33 C32 C31 121.8(9) . . ? C37 C32 C31 117.8(9) . . ? C34 C33 C32 119.5(9) . . ? C33 C34 C35 120.2(9) . . ? C36 C35 C34 120.3(10) . . ? C35 C36 C37 122.1(10) . . ? C36 C37 C32 117.5(9) . . ? C36 C37 C38 123.6(9) . . ? C32 C37 C38 118.8(9) . . ? C39 C38 C43 119.1(9) . . ? C39 C38 C37 121.7(9) . . ? C43 C38 C37 119.2(9) . . ? C40 C39 C38 121.2(10) . . ? C39 C40 C41 120.3(10) . . ? C42 C41 C40 119.4(10) . . ? C41 C42 C43 121.9(10) . . ? C42 C43 C38 118.2(9) . . ? C42 C43 C44 121.6(9) . . ? C38 C43 C44 120.2(9) . . ? C31 C44 C43 117.4(9) . . ? C31 C44 C58 121.0(9) . . ? C43 C44 C58 121.4(8) . . ? C58 C45 O4 117.9(9) . . ? C58 C45 C46 124.7(8) . . ? O4 C45 C46 117.3(9) . . ? C47 C46 C45 123.3(9) . . ? C47 C46 C51 119.2(9) . . ? C45 C46 C51 117.4(9) . . ? C46 C47 C48 123.6(10) . . ? C47 C48 C49 117.8(10) . . ? C50 C49 C48 121.2(9) . . ? C49 C50 C51 120.3(9) . . ? C50 C51 C46 117.6(9) . . ? C50 C51 C52 122.0(8) . . ? C46 C51 C52 120.3(9) . . ? C53 C52 C57 119.4(8) . . ? C53 C52 C51 122.6(8) . . ? C57 C52 C51 117.9(8) . . ? C54 C53 C52 120.6(9) . . ? C53 C54 C55 120.8(10) . . ? C54 C55 C56 121.1(10) . . ? C55 C56 C57 120.2(10) . . ? C56 C57 C52 117.9(9) . . ? C56 C57 C58 120.8(10) . . ? C52 C57 C58 121.3(9) . . ? C45 C58 C57 117.3(9) . . ? C45 C58 C44 121.1(8) . . ? C57 C58 C44 121.5(9) . . ? Cl3 C100 Cl5 114.0(9) . . ? Cl3 C100 Cl4 112.1(8) . . ? Cl5 C100 Cl4 106.3(8) . . ? Cl6 C101 Cl8 114.0(3) . . ? Cl6 C101 Cl7 110.0(3) . . ? Cl8 C101 Cl7 110.2(3) . . ? C78 O79 C75 102.6 . . ? C76 C75 O79 96.9 . . ? C77 C76 C75 108.9 . . ? C78 C77 C76 110.0 . . ? C77 C78 O79 101.1 . . ? C88 O89 C85 110.0 . . ? O89 C85 C86 104.3 . . ? C87 C86 C85 107.2 . . ? C86 C87 C88 106.4 . . ? O89 C88 C87 105.4 . . ? C98 O99 C95 112.3 . . ? O99 C95 C96 104.4 . . ? C97 C96 C95 102.6 . . ? C96 C97 C98 102.5 . . ? O99 C98 C97 106.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.901 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.120