# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1836 data_10 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C60 H80 Cl2 N O4 P Pd' _chemical_formula_weight 1087.52 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 22.871(4) _cell_length_b 13.852(3) _cell_length_c 18.117(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.104(12) _cell_angle_gamma 90.00 _cell_volume 5731.4(17) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method ? _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 0.490 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6036 _exptl_absorpt_correction_T_max 0.8296 _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11314 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 23.30 _reflns_number_total 7145 _reflns_number_observed 6986 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+19.6000P] 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 0.01(3) _refine_ls_number_reflns 7145 _refine_ls_number_parameters 630 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_obs 0.0447 _refine_ls_wR_factor_all 0.1182 _refine_ls_wR_factor_obs 0.1163 _refine_ls_goodness_of_fit_all 1.029 _refine_ls_goodness_of_fit_obs 1.024 _refine_ls_restrained_S_all 1.053 _refine_ls_restrained_S_obs 1.049 _refine_ls_shift/esd_max -1.535 _refine_ls_shift/esd_mean 0.029 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.49998(2) -0.13537(3) 1.24994(2) 0.03297(13) Uani 1 d . . Cl1 Cl 0.47364(10) -0.28880(12) 1.21468(10) 0.0613(5) Uani 1 d . . Cl2 Cl 0.45340(9) -0.15352(13) 1.36174(10) 0.0477(5) Uani 1 d . . P1 P 0.54882(7) -0.12395(11) 1.14808(9) 0.0305(4) Uani 1 d . . O1 O 0.4744(2) -0.0216(3) 0.9681(2) 0.0443(10) Uani 1 d . . H1A H 0.4976(2) 0.0243(3) 0.9617(2) 0.053 Uiso 1 calc R . O2 O 0.5244(2) -0.1639(3) 1.0719(2) 0.0327(8) Uani 1 d . . O3 O 0.6093(2) -0.1761(3) 1.1642(2) 0.0355(9) Uani 1 d . . O4 O 0.5642(2) -0.0139(3) 1.1318(2) 0.0327(8) Uani 1 d . . C1 C 0.4461(2) -0.0067(4) 1.0320(3) 0.0369(14) Uani 1 d . . C2 C 0.4563(2) 0.0730(4) 1.0763(3) 0.0363(13) Uani 1 d . . C3 C 0.4243(3) 0.0842(5) 1.1391(3) 0.0416(15) Uani 1 d . . H3A H 0.4313(3) 0.1394(5) 1.1695(3) 0.050 Uiso 1 calc R . C4 C 0.3818(3) 0.0162(5) 1.1593(4) 0.049(2) Uani 1 d . . C5 C 0.3770(3) -0.0660(5) 1.1160(4) 0.049(2) Uani 1 d . . H5A H 0.3512(3) -0.1157(5) 1.1299(4) 0.059 Uiso 1 calc R . C6 C 0.4080(3) -0.0788(5) 1.0536(4) 0.0428(15) Uani 1 d . . C7 C 0.3415(3) 0.0387(7) 1.2223(4) 0.064(2) Uani 1 d . . C8 C 0.3744(4) 0.0883(8) 1.2870(5) 0.081(3) Uani 1 d . . H8A H 0.3876(23) 0.1521(19) 1.2715(10) 0.097 Uiso 1 calc R . H8B H 0.4084(15) 0.0491(22) 1.3033(22) 0.097 Uiso 1 calc R . H8C H 0.3483(9) 0.0956(40) 1.3278(13) 0.097 Uiso 1 calc R . C9 C 0.2921(4) 0.1053(8) 1.1919(5) 0.088(3) Uani 1 d . . H9A H 0.3089(5) 0.1663(18) 1.1755(33) 0.106 Uiso 1 calc R . H9B H 0.2650(16) 0.1183(40) 1.2308(12) 0.106 Uiso 1 calc R . H9C H 0.2709(18) 0.0739(20) 1.1500(23) 0.106 Uiso 1 calc R . C10 C 0.3158(4) -0.0538(8) 1.2519(6) 0.088(3) Uani 1 d . . H10A H 0.2946(23) -0.0393(10) 1.2961(20) 0.106 Uiso 1 calc R . H10B H 0.3475(5) -0.0995(19) 1.2646(33) 0.106 Uiso 1 calc R . H10C H 0.2889(21) -0.0823(24) 1.2141(13) 0.106 Uiso 1 calc R . C11 C 0.4005(4) -0.1667(6) 1.0056(5) 0.059(2) Uani 1 d . . H11A H 0.3978(4) -0.1438(6) 0.9538(5) 0.071 Uiso 1 calc R . H11B H 0.3619(4) -0.1946(6) 1.0155(5) 0.071 Uiso 1 calc R . C12 C 0.5001(3) -0.2524(4) 1.0442(3) 0.0415(14) Uani 1 d . . C13 C 0.4436(3) -0.2487(5) 1.0088(4) 0.050(2) Uani 1 d . . C14 C 0.4253(4) -0.3323(5) 0.9701(4) 0.062(2) Uani 1 d . . H14A H 0.3880(4) -0.3304(5) 0.9444(4) 0.074 Uiso 1 calc R . C15 C 0.4565(4) -0.4157(5) 0.9663(4) 0.068(2) Uani 1 d . . C16 C 0.5096(4) -0.4162(5) 1.0083(5) 0.067(2) Uani 1 d . . H16A H 0.5319(4) -0.4741(5) 1.0097(5) 0.080 Uiso 1 calc R . C17 C 0.5320(3) -0.3374(5) 1.0482(4) 0.048(2) Uani 1 d . . C18 C 0.4362(6) -0.5020(7) 0.9203(6) 0.105(4) Uani 1 d . . C19 C 0.3689(6) -0.5160(9) 0.9236(8) 0.135(5) Uani 1 d . . H19A H 0.3487(6) -0.4578(28) 0.9050(48) 0.162 Uiso 1 calc R . H19B H 0.3592(7) -0.5276(66) 0.9748(11) 0.162 Uiso 1 calc R . H19C H 0.3565(9) -0.5714(43) 0.8929(42) 0.162 Uiso 1 calc R . C20 C 0.4632(9) -0.5940(10) 0.9420(13) 0.241(13) Uani 1 d . . H20A H 0.4440(62) -0.6464(20) 0.9135(85) 0.289 Uiso 1 calc R . H20B H 0.4588(76) -0.6050(69) 0.9948(30) 0.289 Uiso 1 calc R . H20C H 0.5049(23) -0.5924(55) 0.9321(102) 0.289 Uiso 1 calc R . C21 C 0.4516(10) -0.4787(13) 0.8414(9) 0.209(11) Uani 1 d . . H21A H 0.4407(66) -0.5332(49) 0.8090(19) 0.250 Uiso 1 calc R . H21B H 0.4938(12) -0.4669(110) 0.8402(18) 0.250 Uiso 1 calc R . H21C H 0.4302(51) -0.4209(68) 0.8242(32) 0.250 Uiso 1 calc R . C22 C 0.5875(3) -0.3543(4) 1.0963(4) 0.049(2) Uani 1 d . . H22A H 0.5788(3) -0.3413(4) 1.1483(4) 0.059 Uiso 1 calc R . H22B H 0.5982(3) -0.4233(4) 1.0929(4) 0.059 Uiso 1 calc R . C23 C 0.6472(3) -0.2044(4) 1.1086(3) 0.0388(14) Uani 1 d . . C24 C 0.6400(3) -0.2947(4) 1.0780(3) 0.0434(15) Uani 1 d . . C25 C 0.6811(3) -0.3268(5) 1.0301(4) 0.051(2) Uani 1 d . . H25A H 0.6767(3) -0.3889(5) 1.0083(4) 0.061 Uiso 1 calc R . C26 C 0.7289(3) -0.2699(5) 1.0135(3) 0.046(2) Uani 1 d . . C27 C 0.7319(3) -0.1769(5) 1.0427(4) 0.046(2) Uani 1 d . . H27A H 0.7630(3) -0.1358(5) 1.0299(4) 0.055 Uiso 1 calc R . C28 C 0.6909(3) -0.1423(4) 1.0900(4) 0.0403(14) Uani 1 d . . C29 C 0.7765(4) -0.3066(6) 0.9641(4) 0.065(2) Uani 1 d . . C30 C 0.7690(4) -0.2559(6) 0.8876(4) 0.068(2) Uani 1 d . . H30A H 0.7654(21) -0.1861(7) 0.8947(4) 0.081 Uiso 1 calc R . H30B H 0.7337(12) -0.2804(25) 0.8608(11) 0.081 Uiso 1 calc R . H30C H 0.8033(10) -0.2694(29) 0.8590(11) 0.081 Uiso 1 calc R . C31 C 0.7775(5) -0.4148(7) 0.9551(6) 0.092(3) Uani 1 d . . H31A H 0.8133(14) -0.4339(8) 0.9315(32) 0.110 Uiso 1 calc R . H31B H 0.7432(15) -0.4353(8) 0.9241(29) 0.110 Uiso 1 calc R . H31C H 0.7766(28) -0.4456(7) 1.0037(6) 0.110 Uiso 1 calc R . C32 C 0.8377(4) -0.2801(8) 0.9985(5) 0.084(3) Uani 1 d . . H32A H 0.8410(10) -0.2097(8) 1.0029(31) 0.100 Uiso 1 calc R . H32B H 0.8679(4) -0.3043(39) 0.9669(18) 0.100 Uiso 1 calc R . H32C H 0.8430(11) -0.3094(37) 1.0477(15) 0.100 Uiso 1 calc R . C33 C 0.6913(2) -0.0406(4) 1.1178(4) 0.0419(14) Uani 1 d . . H33A H 0.7320(2) -0.0161(4) 1.1203(4) 0.050 Uiso 1 calc R . H33B H 0.6772(2) -0.0397(4) 1.1685(4) 0.050 Uiso 1 calc R . C34 C 0.5934(2) 0.0389(4) 1.0773(3) 0.0308(12) Uani 1 d . . C35 C 0.6531(2) 0.0260(4) 1.0688(3) 0.0356(13) Uani 1 d . . C36 C 0.6788(3) 0.0791(4) 1.0154(4) 0.046(2) Uani 1 d . . H36A H 0.7193(3) 0.0697(4) 1.0089(4) 0.055 Uiso 1 calc R . C37 C 0.6484(3) 0.1464(4) 0.9701(4) 0.046(2) Uani 1 d . . C38 C 0.5905(3) 0.1622(5) 0.9853(4) 0.041(2) Uani 1 d . . H38A H 0.5691(3) 0.2101(5) 0.9577(4) 0.049 Uiso 1 calc R . C39 C 0.5621(3) 0.1109(4) 1.0393(3) 0.0360(13) Uani 1 d . . C40 C 0.6782(3) 0.2020(6) 0.9083(5) 0.064(2) Uani 1 d . . C41 C 0.6380(5) 0.2709(11) 0.8674(7) 0.124(5) Uani 1 d . . H41A H 0.6025(17) 0.2367(16) 0.8494(41) 0.149 Uiso 1 calc R . H41B H 0.6577(15) 0.2980(49) 0.8253(29) 0.149 Uiso 1 calc R . H41C H 0.6274(30) 0.3232(33) 0.9005(15) 0.149 Uiso 1 calc R . C42 C 0.7358(5) 0.2400(12) 0.9349(7) 0.146(6) Uani 1 d . . H42A H 0.7561(20) 0.2665(72) 0.8931(11) 0.176 Uiso 1 calc R . H42B H 0.7592(17) 0.1877(18) 0.9578(52) 0.176 Uiso 1 calc R . H42C H 0.7304(6) 0.2910(51) 0.9714(43) 0.176 Uiso 1 calc R . C43 C 0.6906(7) 0.1282(9) 0.8447(6) 0.118(4) Uani 1 d . . H43A H 0.6541(10) 0.1149(44) 0.8156(27) 0.141 Uiso 1 calc R . H43B H 0.7060(33) 0.0680(23) 0.8664(7) 0.141 Uiso 1 calc R . H43C H 0.7193(27) 0.1559(26) 0.8125(26) 0.141 Uiso 1 calc R . C44 C 0.5019(3) 0.1471(4) 1.0587(4) 0.0378(14) Uani 1 d . . H44A H 0.5073(3) 0.1907(4) 1.1018(4) 0.045 Uiso 1 calc R . H44B H 0.4859(3) 0.1865(4) 1.0167(4) 0.045 Uiso 1 calc R . N1 N 0.5472(2) 0.0611(4) 1.3047(3) 0.0416(12) Uani 1 d . . C50 C 0.5285(3) -0.0108(4) 1.2827(3) 0.0371(14) Uani 1 d . . C51 C 0.5752(3) 0.1506(4) 1.3311(4) 0.046(2) Uani 1 d . . C52 C 0.6196(4) 0.1753(7) 1.2770(4) 0.078(3) Uani 1 d . . H52A H 0.6492(14) 0.1241(21) 1.2767(24) 0.094 Uiso 1 calc R . H52B H 0.6384(19) 0.2366(22) 1.2910(19) 0.094 Uiso 1 calc R . H52C H 0.6003(6) 0.1813(42) 1.2275(7) 0.094 Uiso 1 calc R . C53 C 0.5287(4) 0.2262(6) 1.3354(5) 0.077(2) Uani 1 d . . H53A H 0.5003(14) 0.2059(20) 1.3709(23) 0.093 Uiso 1 calc R . H53B H 0.5087(17) 0.2345(29) 1.2866(8) 0.093 Uiso 1 calc R . H53C H 0.5466(5) 0.2874(12) 1.3515(31) 0.093 Uiso 1 calc R . C54 C 0.6027(4) 0.1302(5) 1.4085(4) 0.059(2) Uani 1 d . . H54A H 0.5775(11) 0.0861(28) 1.4346(10) 0.070 Uiso 1 calc R . H54B H 0.6069(20) 0.1909(7) 1.4361(10) 0.070 Uiso 1 calc R . H54C H 0.6413(9) 0.1007(32) 1.4044(4) 0.070 Uiso 1 calc R . C70 C 0.5916(6) 0.5228(8) 0.7394(7) 0.103(4) Uani 1 d . . H70A H 0.5856(6) 0.4834(8) 0.7813(7) 0.124 Uiso 1 calc R . C71 C 0.5448(6) 0.5513(10) 0.6973(10) 0.123(5) Uani 1 d . . H71A H 0.5065(6) 0.5303(10) 0.7077(10) 0.147 Uiso 1 calc R . C72 C 0.5534(8) 0.6107(10) 0.6399(10) 0.129(7) Uani 1 d . . H72A H 0.5208(8) 0.6329(10) 0.6099(10) 0.155 Uiso 1 calc R . C73 C 0.6078(10) 0.6389(9) 0.6248(9) 0.138(6) Uani 1 d . . H73A H 0.6132(10) 0.6807(9) 0.5842(9) 0.165 Uiso 1 calc R . C74 C 0.6557(8) 0.6078(10) 0.6673(11) 0.146(6) Uani 1 d . . H74A H 0.6941(8) 0.6278(10) 0.6571(11) 0.175 Uiso 1 calc R . C75 C 0.6462(6) 0.5474(9) 0.7248(8) 0.111(4) Uani 1 d . . H75A H 0.6783(6) 0.5228(9) 0.7545(8) 0.133 Uiso 1 calc R . C80 C 0.8120(15) 0.0734(16) 0.7328(18) 0.122(10) Uiso 0.422(14) d PD 1 H80A H 0.8287(87) 0.1051(48) 0.7775(32) 0.147 Uiso 0.422(14) calc PR 1 H80B H 0.7767(22) 0.1083(45) 0.7147(112) 0.147 Uiso 0.422(14) calc PR 1 H80C H 0.8407(71) 0.0737(17) 0.6947(85) 0.147 Uiso 0.422(14) calc PR 1 C81 C 0.7965(12) -0.0263(17) 0.7501(14) 0.109(9) Uiso 0.422(14) d PD 1 H81A H 0.7535(12) -0.0332(17) 0.7429(14) 0.130 Uiso 0.422(14) calc PR 1 H81B H 0.8070(12) -0.0380(17) 0.8031(14) 0.130 Uiso 0.422(14) calc PR 1 C82 C 0.8250(15) -0.1048(15) 0.7054(16) 0.132(12) Uiso 0.422(14) d PD 1 H82A H 0.7948(15) -0.1489(15) 0.6832(16) 0.159 Uiso 0.422(14) calc PR 1 H82B H 0.8527(15) -0.1431(15) 0.7375(16) 0.159 Uiso 0.422(14) calc PR 1 C83 C 0.8574(5) -0.0539(7) 0.6448(6) 0.096(3) Uiso 0.422(14) d PD 1 H83A H 0.8969(5) -0.0831(7) 0.6442(6) 0.115 Uiso 0.422(14) calc PR 1 H83B H 0.8368(5) -0.0698(7) 0.5969(6) 0.115 Uiso 0.422(14) calc PR 1 C84 C 0.8645(7) 0.0439(10) 0.6471(9) 0.134(5) Uiso 0.422(14) d PD 1 H84A H 0.9053(25) 0.0600(13) 0.6380(129) 0.160 Uiso 0.422(14) calc PR 1 H84B H 0.8550(99) 0.0680(23) 0.6958(44) 0.160 Uiso 0.422(14) calc PR 1 H84C H 0.8385(75) 0.0739(15) 0.6090(86) 0.160 Uiso 0.422(14) calc PR 1 C90 C 0.7751(6) -0.1909(9) 0.6622(8) 0.065(4) Uiso 0.578(14) d PD 2 H90A H 0.7432(15) -0.1817(46) 0.6245(27) 0.077 Uiso 0.578(14) calc PR 2 H90B H 0.7615(24) -0.1733(42) 0.7108(22) 0.077 Uiso 0.578(14) calc PR 2 H90C H 0.7873(11) -0.2587(10) 0.6627(46) 0.077 Uiso 0.578(14) calc PR 2 C91 C 0.8222(11) -0.1326(15) 0.6459(20) 0.156(11) Uiso 0.578(14) d PD 2 H91A H 0.8531(11) -0.1790(15) 0.6624(20) 0.187 Uiso 0.578(14) calc PR 2 H91B H 0.8186(11) -0.1421(15) 0.5917(20) 0.187 Uiso 0.578(14) calc PR 2 C92 C 0.8574(5) -0.0539(7) 0.6448(6) 0.096(3) Uiso 0.578(14) d PD 2 H92A H 0.8775(17) -0.0678(17) 0.5989(22) 0.115 Uiso 0.578(14) calc PR 2 H92B H 0.8865(17) -0.0723(17) 0.6848(22) 0.115 Uiso 0.578(14) calc PR 2 C93 C 0.8645(7) 0.0439(10) 0.6471(9) 0.134(5) Uiso 0.578(14) d PD 2 H93A H 0.9078(17) 0.0467(17) 0.6487(22) 0.160 Uiso 0.578(14) calc PR 2 H93B H 0.8527(17) 0.0591(17) 0.5950(22) 0.160 Uiso 0.578(14) calc PR 2 C94 C 0.8542(17) 0.1279(17) 0.6768(22) 0.220(19) Uiso 0.578(14) d PD 2 H94A H 0.8276(112) 0.1195(33) 0.7170(116) 0.264 Uiso 0.578(14) calc PR 2 H94B H 0.8360(125) 0.1708(73) 0.6391(46) 0.264 Uiso 0.578(14) calc PR 2 H94C H 0.8911(26) 0.1562(104) 0.6964(155) 0.264 Uiso 0.578(14) calc PR 2 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 Pd1 0.0328(2) 0.0362(2) 0.0300(2) -0.0001(2) 0.00275(15) -0.0031(2) Cl1 0.0917(14) 0.0436(8) 0.0501(10) -0.0046(7) 0.0183(9) -0.0261(9) Cl2 0.0517(11) 0.0568(9) 0.0357(10) -0.0012(8) 0.0131(8) -0.0095(8) P1 0.0300(9) 0.0354(8) 0.0258(9) 0.0003(6) 0.0000(7) -0.0004(6) O1 0.046(3) 0.044(2) 0.044(3) 0.003(2) 0.011(2) -0.004(2) O2 0.041(2) 0.030(2) 0.027(2) -0.002(2) 0.005(2) -0.004(2) O3 0.040(2) 0.032(2) 0.036(2) 0.001(2) 0.006(2) 0.008(2) O4 0.032(2) 0.033(2) 0.033(2) -0.002(2) 0.004(2) -0.004(2) C1 0.029(3) 0.047(3) 0.035(3) 0.004(3) -0.003(3) 0.008(2) C2 0.029(3) 0.044(3) 0.037(3) 0.004(3) 0.008(3) 0.007(2) C3 0.032(3) 0.054(4) 0.039(4) 0.004(3) 0.002(3) 0.005(3) C4 0.034(3) 0.076(5) 0.038(4) 0.022(3) 0.000(3) 0.009(3) C5 0.032(3) 0.059(4) 0.055(4) 0.019(3) -0.006(3) -0.008(3) C6 0.033(3) 0.051(4) 0.043(4) 0.010(3) -0.001(3) -0.001(3) C7 0.032(4) 0.118(6) 0.043(4) 0.020(4) 0.008(3) 0.021(4) C8 0.060(5) 0.133(8) 0.052(5) -0.015(5) 0.013(4) 0.018(5) C9 0.053(5) 0.153(9) 0.061(5) 0.031(6) 0.021(4) 0.041(5) C10 0.060(5) 0.129(8) 0.077(6) 0.036(6) 0.019(5) 0.001(5) C11 0.052(5) 0.051(4) 0.073(6) 0.009(4) -0.020(4) -0.014(4) C12 0.051(4) 0.038(3) 0.036(3) -0.006(3) 0.005(3) -0.010(3) C13 0.055(4) 0.048(4) 0.048(4) -0.003(3) 0.003(3) -0.019(3) C14 0.070(5) 0.063(5) 0.050(4) -0.002(3) -0.009(4) -0.032(4) C15 0.096(6) 0.050(4) 0.060(5) -0.021(4) 0.016(5) -0.023(4) C16 0.087(6) 0.046(4) 0.068(5) -0.013(4) 0.007(5) -0.017(4) C17 0.064(4) 0.036(3) 0.046(4) -0.013(3) 0.008(3) -0.008(3) C18 0.149(11) 0.076(7) 0.089(8) -0.030(5) -0.008(7) -0.033(6) C19 0.125(10) 0.118(9) 0.157(12) -0.044(8) -0.036(9) -0.058(8) C20 0.272(22) 0.089(10) 0.344(29) -0.127(15) -0.154(21) 0.011(12) C21 0.281(24) 0.188(17) 0.159(16) -0.125(14) 0.036(16) -0.116(17) C22 0.064(5) 0.031(3) 0.053(4) -0.002(3) 0.005(3) -0.007(3) C23 0.040(3) 0.044(3) 0.032(3) 0.003(2) 0.004(3) 0.015(3) C24 0.050(4) 0.038(3) 0.042(3) 0.001(3) 0.001(3) 0.011(3) C25 0.066(5) 0.044(3) 0.043(4) 0.007(3) 0.006(3) 0.020(3) C26 0.050(4) 0.052(4) 0.037(4) 0.007(3) 0.010(3) 0.020(3) C27 0.037(4) 0.054(4) 0.047(4) 0.009(3) 0.007(3) 0.011(3) C28 0.036(3) 0.045(3) 0.040(3) 0.004(3) -0.001(3) 0.005(3) C29 0.079(6) 0.072(5) 0.045(4) 0.009(4) 0.020(4) 0.037(4) C30 0.069(5) 0.088(6) 0.047(4) 0.006(4) 0.008(4) 0.023(4) C31 0.129(9) 0.072(6) 0.080(6) 0.003(5) 0.049(6) 0.045(6) C32 0.060(5) 0.127(8) 0.066(5) 0.006(5) 0.021(4) 0.051(5) C33 0.022(3) 0.047(3) 0.057(4) 0.000(3) 0.002(3) -0.002(2) C34 0.030(3) 0.032(3) 0.031(3) -0.002(2) 0.006(2) -0.002(2) C35 0.032(3) 0.030(3) 0.044(3) -0.001(2) 0.000(3) -0.005(2) C36 0.027(3) 0.046(3) 0.066(4) -0.004(3) 0.006(3) -0.003(3) C37 0.040(4) 0.049(4) 0.049(4) 0.006(3) 0.010(3) -0.008(3) C38 0.038(4) 0.044(3) 0.041(4) 0.011(3) 0.012(3) -0.009(3) C39 0.031(3) 0.035(3) 0.043(3) -0.003(2) 0.004(3) -0.004(2) C40 0.055(4) 0.066(4) 0.074(5) 0.028(4) 0.023(4) -0.005(4) C41 0.083(7) 0.189(13) 0.100(9) 0.078(9) 0.012(6) -0.020(8) C42 0.110(9) 0.224(15) 0.102(9) 0.074(9) -0.025(7) -0.114(10) C43 0.149(12) 0.139(11) 0.066(7) 0.002(6) 0.021(7) -0.040(8) C44 0.034(3) 0.036(3) 0.043(4) 0.005(2) 0.003(3) 0.005(2) N1 0.051(3) 0.041(3) 0.033(3) -0.002(2) 0.001(2) -0.001(2) C50 0.036(3) 0.053(4) 0.022(3) -0.003(3) -0.004(3) 0.001(3) C51 0.059(4) 0.042(3) 0.036(4) -0.004(3) -0.002(3) -0.013(3) C52 0.091(6) 0.094(6) 0.048(5) 0.002(4) -0.004(4) -0.046(5) C53 0.102(7) 0.050(4) 0.078(6) -0.009(4) -0.008(5) -0.001(4) C54 0.073(5) 0.054(4) 0.048(4) -0.004(3) -0.010(4) -0.013(3) C70 0.128(10) 0.090(7) 0.091(8) 0.001(6) 0.015(7) 0.044(7) C71 0.119(10) 0.094(8) 0.154(13) -0.033(9) -0.009(10) 0.046(8) C72 0.163(14) 0.071(7) 0.145(13) -0.056(9) -0.066(12) 0.075(9) C73 0.209(19) 0.079(8) 0.124(12) 0.025(7) 0.008(13) 0.039(11) C74 0.176(16) 0.083(8) 0.178(16) 0.005(10) -0.004(13) -0.004(9) C75 0.098(9) 0.094(8) 0.137(11) -0.009(8) -0.018(8) 0.018(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 Pd1 C50 1.927(6) . ? Pd1 P1 2.214(2) . ? Pd1 Cl1 2.291(2) . ? Pd1 Cl2 2.353(2) . ? P1 O2 1.562(4) . ? P1 O3 1.573(4) . ? P1 O4 1.595(4) . ? O1 C1 1.371(7) . ? O2 C12 1.426(7) . ? O3 C23 1.420(7) . ? O4 C34 1.425(7) . ? C1 C2 1.378(8) . ? C1 C6 1.395(9) . ? C2 C3 1.395(9) . ? C2 C44 1.508(8) . ? C3 C4 1.416(9) . ? C4 C5 1.383(10) . ? C4 C7 1.538(10) . ? C5 C6 1.380(10) . ? C6 C11 1.500(10) . ? C7 C10 1.520(12) . ? C7 C8 1.520(12) . ? C7 C9 1.538(10) . ? C11 C13 1.503(11) . ? C12 C17 1.387(9) . ? C12 C13 1.411(9) . ? C13 C14 1.405(10) . ? C14 C15 1.362(12) . ? C15 C16 1.399(12) . ? C15 C18 1.516(11) . ? C16 C17 1.390(10) . ? C17 C22 1.518(10) . ? C18 C20 1.46(2) . ? C18 C21 1.52(2) . ? C18 C19 1.55(2) . ? C22 C24 1.508(10) . ? C23 C28 1.373(9) . ? C23 C24 1.374(9) . ? C24 C25 1.388(9) . ? C25 C26 1.394(10) . ? C26 C27 1.392(10) . ? C26 C29 1.533(10) . ? C27 C28 1.390(9) . ? C28 C33 1.497(8) . ? C29 C31 1.509(13) . ? C29 C32 1.546(13) . ? C29 C30 1.555(11) . ? C33 C35 1.522(8) . ? C34 C39 1.388(8) . ? C34 C35 1.395(8) . ? C35 C36 1.372(9) . ? C36 C37 1.402(9) . ? C37 C38 1.384(10) . ? C37 C40 1.547(10) . ? C38 C39 1.398(9) . ? C39 C44 1.523(8) . ? C40 C42 1.474(12) . ? C40 C41 1.495(13) . ? C40 C43 1.578(14) . ? N1 C50 1.147(8) . ? N1 C51 1.464(8) . ? C51 C52 1.488(11) . ? C51 C53 1.498(11) . ? C51 C54 1.532(10) . ? C70 C75 1.33(2) . ? C70 C71 1.34(2) . ? C71 C72 1.35(2) . ? C72 C73 1.35(2) . ? C73 C74 1.37(2) . ? C74 C75 1.36(2) . ? C80 C81 1.46(2) . ? C81 C82 1.52(2) . ? C82 C83 1.53(2) . ? C83 C84 1.365(12) . ? C90 C91 1.39(2) . ? C91 C92 1.357(15) . ? C92 C93 1.365(12) . ? C93 C94 1.31(2) . ? 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 C50 Pd1 P1 90.9(2) . . ? C50 Pd1 Cl1 175.1(2) . . ? P1 Pd1 Cl1 88.33(6) . . ? C50 Pd1 Cl2 89.5(2) . . ? P1 Pd1 Cl2 176.14(8) . . ? Cl1 Pd1 Cl2 90.94(7) . . ? O2 P1 O3 105.7(2) . . ? O2 P1 O4 104.3(2) . . ? O3 P1 O4 105.8(2) . . ? O2 P1 Pd1 122.6(2) . . ? O3 P1 Pd1 106.9(2) . . ? O4 P1 Pd1 110.4(2) . . ? C12 O2 P1 136.9(4) . . ? C23 O3 P1 124.1(3) . . ? C34 O4 P1 137.3(3) . . ? O1 C1 C2 122.6(5) . . ? O1 C1 C6 117.3(5) . . ? C2 C1 C6 120.0(6) . . ? C1 C2 C3 119.0(6) . . ? C1 C2 C44 121.3(5) . . ? C3 C2 C44 119.7(5) . . ? C2 C3 C4 122.3(6) . . ? C5 C4 C3 115.9(6) . . ? C5 C4 C7 123.7(7) . . ? C3 C4 C7 120.3(7) . . ? C6 C5 C4 122.8(6) . . ? C5 C6 C1 119.6(6) . . ? C5 C6 C11 122.1(6) . . ? C1 C6 C11 118.2(6) . . ? C10 C7 C8 107.1(7) . . ? C10 C7 C9 110.0(7) . . ? C8 C7 C9 109.2(8) . . ? C10 C7 C4 110.5(8) . . ? C8 C7 C4 111.9(6) . . ? C9 C7 C4 108.3(6) . . ? C6 C11 C13 122.5(6) . . ? C17 C12 C13 121.4(6) . . ? C17 C12 O2 121.1(5) . . ? C13 C12 O2 117.4(5) . . ? C14 C13 C12 116.0(7) . . ? C14 C13 C11 115.2(6) . . ? C12 C13 C11 128.8(6) . . ? C15 C14 C13 125.5(7) . . ? C14 C15 C16 114.8(6) . . ? C14 C15 C18 123.4(9) . . ? C16 C15 C18 121.8(9) . . ? C17 C16 C15 124.3(8) . . ? C12 C17 C16 117.4(7) . . ? C12 C17 C22 125.6(5) . . ? C16 C17 C22 116.8(7) . . ? C20 C18 C15 115.3(10) . . ? C20 C18 C21 108.7(15) . . ? C15 C18 C21 105.6(9) . . ? C20 C18 C19 106.6(12) . . ? C15 C18 C19 110.6(10) . . ? C21 C18 C19 110.0(12) . . ? C24 C22 C17 116.1(5) . . ? C28 C23 C24 123.0(6) . . ? C28 C23 O3 118.8(5) . . ? C24 C23 O3 118.2(5) . . ? C23 C24 C25 118.2(6) . . ? C23 C24 C22 119.3(6) . . ? C25 C24 C22 122.5(6) . . ? C24 C25 C26 121.3(6) . . ? C27 C26 C25 117.7(6) . . ? C27 C26 C29 120.4(7) . . ? C25 C26 C29 121.9(7) . . ? C28 C27 C26 122.1(7) . . ? C23 C28 C27 117.4(6) . . ? C23 C28 C33 119.9(6) . . ? C27 C28 C33 122.6(6) . . ? C31 C29 C26 114.1(7) . . ? C31 C29 C32 105.2(7) . . ? C26 C29 C32 110.0(7) . . ? C31 C29 C30 110.7(7) . . ? C26 C29 C30 108.9(6) . . ? C32 C29 C30 107.8(8) . . ? C28 C33 C35 112.4(5) . . ? C39 C34 C35 121.3(5) . . ? C39 C34 O4 117.7(5) . . ? C35 C34 O4 120.6(5) . . ? C36 C35 C34 117.9(5) . . ? C36 C35 C33 118.8(5) . . ? C34 C35 C33 123.3(5) . . ? C35 C36 C37 123.5(6) . . ? C38 C37 C36 115.9(6) . . ? C38 C37 C40 122.0(6) . . ? C36 C37 C40 122.1(6) . . ? C37 C38 C39 123.1(7) . . ? C34 C39 C38 117.7(6) . . ? C34 C39 C44 124.8(5) . . ? C38 C39 C44 117.1(6) . . ? C42 C40 C41 116.8(9) . . ? C42 C40 C37 111.2(7) . . ? C41 C40 C37 113.1(7) . . ? C42 C40 C43 106.1(10) . . ? C41 C40 C43 100.4(9) . . ? C37 C40 C43 108.0(7) . . ? C2 C44 C39 117.9(5) . . ? C50 N1 C51 175.9(7) . . ? N1 C50 Pd1 176.7(5) . . ? N1 C51 C52 106.3(6) . . ? N1 C51 C53 108.0(6) . . ? C52 C51 C53 112.7(7) . . ? N1 C51 C54 107.1(5) . . ? C52 C51 C54 112.7(6) . . ? C53 C51 C54 109.8(6) . . ? C75 C70 C71 122.6(14) . . ? C70 C71 C72 118.3(16) . . ? C73 C72 C71 120.5(13) . . ? C72 C73 C74 120.8(15) . . ? C75 C74 C73 117.8(17) . . ? C70 C75 C74 119.9(14) . . ? C80 C81 C82 116.5(16) . . ? C81 C82 C83 106.9(12) . . ? C84 C83 C82 119.8(11) . . ? C92 C91 C90 159.6(26) . . ? C91 C92 C93 150.1(16) . . ? C94 C93 C92 150.6(22) . . ? _refine_diff_density_max 0.688 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.069 data_8b _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C94 H112 Cl24 O8 P2 Pd2' _chemical_formula_weight 2495.38 _chemical_melting_point ? _chemical_compound_source ? 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' 'Pd' 'Pd' -0.9988 1.0072 '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 13.312(3) _cell_length_b 13.923(3) _cell_length_c 16.352(3) _cell_angle_alpha 106.68(3) _cell_angle_beta 95.68(3) _cell_angle_gamma 107.47(3) _cell_volume 2711.8(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method ? _exptl_crystal_F_000 1270 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10006 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9555 _reflns_number_observed 7268 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SMART (Siemens, 1995b)' _computing_data_reduction 'SMART (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 on F^2^ for ALL reflections except for 10 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+6.4000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9545 _refine_ls_number_parameters 714 _refine_ls_number_restraints 399 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_obs 0.0507 _refine_ls_wR_factor_all 0.1482 _refine_ls_wR_factor_obs 0.1260 _refine_ls_goodness_of_fit_all 1.090 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_all 1.159 _refine_ls_restrained_S_obs 1.161 _refine_ls_shift/esd_max -0.288 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.92893(3) 0.51327(3) 0.58226(3) 0.02781(13) Uani 1 d . . Cl1 Cl 1.06221(12) 0.62649(10) 0.53945(10) 0.0471(4) Uani 1 d . . Cl2 Cl 0.79575(11) 0.39475(10) 0.61549(9) 0.0410(3) Uani 1 d . . P1 P 0.90584(9) 0.64187(9) 0.68387(8) 0.0227(3) Uani 1 d . . O1 O 1.0842(3) 0.7573(3) 0.9142(2) 0.0407(9) Uani 1 d . . H1 H 1.1099(43) 0.8199(9) 0.9135(28) 0.049 Uiso 1 calc R . O2 O 0.8898(2) 0.6345(2) 0.7763(2) 0.0254(7) Uani 1 d . . O3 O 0.8019(3) 0.6603(2) 0.6456(2) 0.0250(7) Uani 1 d . . O4 O 1.0038(3) 0.7478(2) 0.7033(2) 0.0257(7) Uani 1 d . . C1 C 1.1157(4) 0.6900(4) 0.8509(3) 0.0321(11) Uani 1 d . . C2 C 1.1847(4) 0.7275(4) 0.8000(3) 0.0299(11) Uani 1 d . . C3 C 1.2206(4) 0.6547(4) 0.7434(4) 0.0360(12) Uani 1 d . . H3A H 1.2690(4) 0.6800(4) 0.7091(4) 0.043 Uiso 1 calc R . C4 C 1.1893(4) 0.5481(4) 0.7349(4) 0.0408(13) Uani 1 d . . C5 C 1.1117(4) 0.5124(4) 0.7811(4) 0.0403(13) Uani 1 d . . H5A H 1.0840(4) 0.4383(4) 0.7731(4) 0.048 Uiso 1 calc R . C6 C 1.0736(4) 0.5816(4) 0.8383(4) 0.0361(12) Uani 1 d . . C7 C 1.2414(5) 0.4732(5) 0.6817(5) 0.054(2) Uani 1 d . . C8 C 1.3057(9) 0.5217(7) 0.6232(7) 0.101(3) Uani 1 d . . H8A H 1.3643(30) 0.5873(28) 0.6590(7) 0.121 Uiso 1 calc R . H8B H 1.2587(13) 0.5385(46) 0.5836(28) 0.121 Uiso 1 calc R . H8C H 1.3358(44) 0.4708(21) 0.5892(31) 0.121 Uiso 1 calc R . C9 C 1.1590(7) 0.3704(7) 0.6237(8) 0.112(4) Uani 1 d . . H9A H 1.1084(34) 0.3849(8) 0.5853(31) 0.134 Uiso 1 calc R . H9B H 1.1200(38) 0.3324(26) 0.6593(8) 0.134 Uiso 1 calc R . H9C H 1.1946(9) 0.3262(25) 0.5884(34) 0.134 Uiso 1 calc R . C10 C 1.3187(7) 0.4551(7) 0.7442(6) 0.085(3) Uani 1 d . . H10A H 1.3775(24) 0.5225(12) 0.7755(27) 0.102 Uiso 1 calc R . H10B H 1.3480(35) 0.4025(34) 0.7117(7) 0.102 Uiso 1 calc R . H10C H 1.2809(12) 0.4284(42) 0.7860(23) 0.102 Uiso 1 calc R . C11 C 0.9956(4) 0.5435(5) 0.8919(4) 0.0463(15) Uani 1 d . . H11A H 1.0191(4) 0.5976(5) 0.9510(4) 0.056 Uiso 1 calc R . H11B H 1.0038(4) 0.4773(5) 0.8979(4) 0.056 Uiso 1 calc R . C12 C 0.8252(4) 0.5574(4) 0.8080(3) 0.0252(10) Uani 1 d . . C13 C 0.8757(4) 0.5202(4) 0.8633(3) 0.0283(10) Uani 1 d . . C14 C 0.8109(4) 0.4539(4) 0.9024(3) 0.0306(11) Uani 1 d . . H14A H 0.8453(4) 0.4286(4) 0.9412(3) 0.037 Uiso 1 calc R . C15 C 0.7009(4) 0.4235(4) 0.8880(3) 0.0306(11) Uani 1 d . . C16 C 0.6545(4) 0.4605(4) 0.8297(3) 0.0302(11) Uani 1 d . . H16A H 0.5782(4) 0.4393(4) 0.8170(3) 0.036 Uiso 1 calc R . C17 C 0.7121(4) 0.5267(4) 0.7885(3) 0.0257(10) Uani 1 d . . C18 C 0.6320(5) 0.3523(5) 0.9313(4) 0.0406(13) Uani 1 d . . C19 C 0.5507(6) 0.2500(6) 0.8588(6) 0.056(2) Uani 0.844(8) d P 1 H19A H 0.5061(28) 0.2710(6) 0.8208(20) 0.067 Uiso 0.844(8) calc PR 1 H19B H 0.5047(28) 0.2044(20) 0.8861(6) 0.067 Uiso 0.844(8) calc PR 1 H19C H 0.5906(6) 0.2105(22) 0.8242(22) 0.067 Uiso 0.844(8) calc PR 1 C20 C 0.6963(6) 0.3151(8) 0.9893(6) 0.056(2) Uani 0.844(8) d P 1 H20A H 0.7439(32) 0.2844(40) 0.9570(13) 0.068 Uiso 0.844(8) calc PR 1 H20B H 0.6472(7) 0.2608(33) 1.0076(31) 0.068 Uiso 0.844(8) calc PR 1 H20C H 0.7396(35) 0.3759(11) 1.0408(18) 0.068 Uiso 0.844(8) calc PR 1 C21 C 0.5676(7) 0.4109(7) 0.9840(6) 0.059(2) Uani 0.844(8) d P 1 H21A H 0.5201(31) 0.4281(38) 0.9452(8) 0.071 Uiso 0.844(8) calc PR 1 H21B H 0.6168(7) 0.4770(22) 1.0282(23) 0.071 Uiso 0.844(8) calc PR 1 H21C H 0.5243(33) 0.3654(18) 1.0128(29) 0.071 Uiso 0.844(8) calc PR 1 C19' C 0.6586(36) 0.4345(32) 1.0357(29) 0.056(2) Uani 0.156(8) d P 2 H19D H 0.7229(133) 0.4315(168) 1.0681(54) 0.067 Uiso 0.156(8) calc PR 2 H19E H 0.5973(97) 0.4117(137) 1.0629(62) 0.067 Uiso 0.156(8) calc PR 2 H19F H 0.6709(220) 0.5078(47) 1.0366(30) 0.067 Uiso 0.156(8) calc PR 2 C20' C 0.5177(33) 0.3118(40) 0.8985(32) 0.056(2) Uani 0.156(8) d P 2 H20D H 0.4881(47) 0.3687(76) 0.9198(153) 0.068 Uiso 0.156(8) calc PR 2 H20E H 0.4839(44) 0.2523(154) 0.9186(157) 0.068 Uiso 0.156(8) calc PR 2 H20F H 0.5031(34) 0.2868(210) 0.8346(32) 0.068 Uiso 0.156(8) calc PR 2 C21' C 0.6770(44) 0.2679(41) 0.9396(38) 0.059(2) Uani 0.156(8) d P 2 H21D H 0.7419(149) 0.3004(62) 0.9857(142) 0.071 Uiso 0.156(8) calc PR 2 H21E H 0.6951(240) 0.2350(175) 0.8842(71) 0.071 Uiso 0.156(8) calc PR 2 H21F H 0.6234(102) 0.2132(140) 0.9543(208) 0.071 Uiso 0.156(8) calc PR 2 C22 C 0.6480(4) 0.5537(4) 0.7223(3) 0.0276(10) Uani 1 d . . H22A H 0.6600(4) 0.5195(4) 0.6638(3) 0.033 Uiso 1 calc R . H22B H 0.5707(4) 0.5218(4) 0.7220(3) 0.033 Uiso 1 calc R . C23 C 0.7516(4) 0.7220(4) 0.6998(3) 0.0256(10) Uani 1 d . . C24 C 0.6737(4) 0.6707(4) 0.7368(3) 0.0245(10) Uani 1 d . . C25 C 0.6215(4) 0.7320(4) 0.7876(3) 0.0287(11) Uani 1 d . . H25A H 0.5668(4) 0.6986(4) 0.8139(3) 0.034 Uiso 1 calc R . C26 C 0.6474(4) 0.8396(4) 0.8005(3) 0.0280(10) Uani 1 d . . C27 C 0.7271(4) 0.8872(4) 0.7614(3) 0.0283(10) Uani 1 d . . H27A H 0.7443(4) 0.9609(4) 0.7687(3) 0.034 Uiso 1 calc R . C28 C 0.7824(4) 0.8296(4) 0.7117(3) 0.0251(10) Uani 1 d . . C29 C 0.5891(4) 0.9085(4) 0.8541(4) 0.0361(12) Uani 1 d . . C30 C 0.5152(6) 0.8485(5) 0.9020(5) 0.056(2) Uani 1 d . . H30A H 0.5559(9) 0.8209(29) 0.9371(21) 0.067 Uiso 1 calc R . H30B H 0.4559(19) 0.7889(21) 0.8596(5) 0.067 Uiso 1 calc R . H30C H 0.4861(27) 0.8971(10) 0.9402(21) 0.067 Uiso 1 calc R . C31 C 0.6729(6) 1.0099(5) 0.9212(4) 0.055(2) Uani 1 d . . H31A H 0.7194(22) 1.0505(17) 0.8909(5) 0.066 Uiso 1 calc R . H31B H 0.7167(22) 0.9898(5) 0.9607(17) 0.066 Uiso 1 calc R . H31C H 0.6361(6) 1.0540(17) 0.9549(19) 0.066 Uiso 1 calc R . C32 C 0.5223(5) 0.9416(6) 0.7932(5) 0.053(2) Uani 1 d . . H32A H 0.5695(7) 0.9826(29) 0.7636(21) 0.064 Uiso 1 calc R . H32B H 0.4856(27) 0.9856(28) 0.8271(6) 0.064 Uiso 1 calc R . H32C H 0.4688(22) 0.8776(6) 0.7498(17) 0.064 Uiso 1 calc R . C33 C 0.8777(4) 0.8827(4) 0.6781(3) 0.0276(10) Uani 1 d . . H33A H 0.8676(4) 0.9440(4) 0.6637(3) 0.033 Uiso 1 calc R . H33B H 0.8840(4) 0.8314(4) 0.6243(3) 0.033 Uiso 1 calc R . C34 C 1.0382(4) 0.8566(4) 0.7568(3) 0.0262(10) Uani 1 d . . C35 C 0.9792(4) 0.9211(4) 0.7470(3) 0.0261(10) Uani 1 d . . C36 C 1.0155(4) 1.0260(4) 0.8028(4) 0.0326(11) Uani 1 d . . H36A H 0.9738(4) 1.0696(4) 0.7984(4) 0.039 Uiso 1 calc R . C37 C 1.1101(4) 1.0697(4) 0.8648(4) 0.0382(13) Uani 1 d . . C38 C 1.1717(4) 1.0045(4) 0.8649(4) 0.0360(12) Uani 1 d . . H38A H 1.2392(4) 1.0338(4) 0.9042(4) 0.043 Uiso 1 calc R . C39 C 1.1398(4) 0.8999(4) 0.8107(3) 0.0301(11) Uani 1 d . . C40 C 1.1453(5) 1.1831(5) 0.9314(5) 0.062(2) Uani 1 d . . C41 C 1.1318(9) 1.1710(8) 1.0216(5) 0.106(4) Uani 1 d . . H41A H 1.0552(9) 1.1404(48) 1.0215(15) 0.127 Uiso 1 calc R . H41B H 1.1629(47) 1.2413(11) 1.0671(7) 0.127 Uiso 1 calc R . H41C H 1.1688(45) 1.1237(43) 1.0330(19) 0.127 Uiso 1 calc R . C42 C 1.2612(7) 1.2427(6) 0.9410(9) 0.128(5) Uani 1 d . . H42A H 1.3041(7) 1.2035(34) 0.9592(50) 0.154 Uiso 1 calc R . H42B H 1.2809(17) 1.3136(26) 0.9851(40) 0.154 Uiso 1 calc R . H42C H 1.2750(13) 1.2505(55) 0.8850(17) 0.154 Uiso 1 calc R . C43 C 1.0746(7) 1.2444(6) 0.9126(6) 0.090(3) Uani 1 d . . H43A H 0.9998(11) 1.2048(24) 0.9118(38) 0.108 Uiso 1 calc R . H43B H 1.0803(37) 1.2535(41) 0.8558(19) 0.108 Uiso 1 calc R . H43C H 1.0980(32) 1.3147(20) 0.9581(22) 0.108 Uiso 1 calc R . C44 C 1.2214(4) 0.8430(4) 0.8066(4) 0.0365(12) Uani 1 d . . H44A H 1.2545(4) 0.8489(4) 0.7559(4) 0.044 Uiso 1 calc R . H44B H 1.2790(4) 0.8831(4) 0.8594(4) 0.044 Uiso 1 calc R . C45 C 1.2362(14) 0.0210(10) 0.6032(10) 0.115(7) Uani 0.659(8) d PD 1 H45 H 1.2794(14) 0.0289(10) 0.5574(10) 0.138 Uiso 0.659(8) calc PR 1 Cl3 Cl 1.1363(12) 0.0718(11) 0.5951(12) 0.239(7) Uani 0.659(8) d PDU 1 Cl4 Cl 1.3124(13) 0.0909(12) 0.7032(7) 0.295(9) Uani 0.659(8) d PDU 1 Cl5 Cl 1.1681(6) -0.1146(4) 0.5870(4) 0.094(2) Uani 0.659(8) d PDU 1 C45' C 1.2035(14) 0.0255(13) 0.6542(13) 0.059(6) Uani 0.341(8) d PD 2 H45' H 1.1624(14) 0.0248(13) 0.7021(13) 0.070 Uiso 0.341(8) calc PR 2 Cl3' Cl 1.1822(13) 0.1077(16) 0.5990(19) 0.160(7) Uani 0.341(8) d PDU 2 Cl4' Cl 1.3436(7) 0.0533(11) 0.6903(10) 0.099(4) Uani 0.341(8) d PDU 2 Cl5' Cl 1.1642(31) -0.0985(15) 0.5727(14) 0.274(14) Uani 0.341(8) d PDU 2 C46 C 0.8032(9) 1.1699(7) 0.6613(8) 0.129(5) Uani 0.659(8) d PD 1 H46 H 0.7868(9) 1.2260(7) 0.6412(8) 0.154 Uiso 0.659(8) calc PR 1 Cl6 Cl 0.9252(5) 1.1613(7) 0.6442(5) 0.103(3) Uani 0.659(8) d PDU 1 Cl7 Cl 0.7011(5) 1.0365(4) 0.6059(4) 0.0903(15) Uani 0.659(8) d PDU 1 Cl8 Cl 0.8155(6) 1.2015(4) 0.7825(6) 0.140(3) Uani 0.659(8) d PDU 1 C46' C 0.8032(9) 1.1699(7) 0.6613(8) 0.129(5) Uani 0.341(8) d PD 2 H46' H 0.8032(14) 1.2232(16) 0.6313(16) 0.154 Uiso 0.341(8) calc PR 2 Cl6' Cl 0.9103(14) 1.1456(16) 0.6409(16) 0.163(9) Uani 0.341(8) d PDU 2 Cl7' Cl 0.6924(14) 1.0830(17) 0.6168(14) 0.207(11) Uani 0.341(8) d PDU 2 Cl8' Cl 0.7956(15) 1.2321(9) 0.7557(7) 0.147(6) Uani 0.341(8) d PDU 2 C47 C 0.4689(8) 0.7284(8) 0.4811(6) 0.102(3) Uani 0.659(8) d PD 1 H47 H 0.4010(8) 0.6652(8) 0.4630(6) 0.123 Uiso 0.659(8) calc PR 1 Cl9 Cl 0.5027(7) 0.7489(5) 0.3914(3) 0.139(3) Uani 0.659(8) d PDU 1 ClA Cl 0.4403(7) 0.8393(7) 0.5450(5) 0.176(4) Uani 0.659(8) d PDU 1 ClB Cl 0.5540(7) 0.7061(7) 0.5440(6) 0.194(4) Uani 0.659(8) d PDU 1 C47' C 0.4689(8) 0.7284(8) 0.4811(6) 0.102(3) Uani 0.341(8) d PD 2 H47' H 0.4096(12) 0.6577(12) 0.4551(8) 0.123 Uiso 0.341(8) calc PR 2 Cl9' Cl 0.4788(12) 0.7894(12) 0.5845(8) 0.161(6) Uani 0.341(8) d PDU 2 ClA' Cl 0.5845(16) 0.7416(12) 0.4332(16) 0.213(9) Uani 0.341(8) d PDU 2 ClB' Cl 0.4514(27) 0.8327(25) 0.4442(21) 0.494(21) Uani 0.341(8) d PDU 2 Cl20 Cl 0.5065(14) 0.5805(15) 0.5098(11) 0.080(4) Uiso 0.15 d P 3 Cl21 Cl 0.6580(30) 1.1745(29) 0.6808(25) 0.237(14) Uiso 0.20 d P 3 Cl22 Cl 0.5329(18) 0.6367(18) 0.5155(14) 0.170(8) Uiso 0.30 d P 3 Cl23 Cl 1.2973(55) -0.0306(56) 0.6277(43) 0.357(30) Uiso 0.20 d P 3 Cl24 Cl 0.5700(59) 0.8929(55) 0.5595(46) 0.330(30) Uiso 0.15 d P 3 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 Pd1 0.0291(2) 0.0181(2) 0.0316(2) 0.00080(14) 0.0123(2) 0.00683(14) Cl1 0.0549(9) 0.0204(6) 0.0523(9) -0.0037(6) 0.0336(7) 0.0019(6) Cl2 0.0454(8) 0.0244(6) 0.0474(8) 0.0061(6) 0.0226(6) 0.0054(6) P1 0.0227(6) 0.0193(6) 0.0241(6) 0.0030(5) 0.0070(5) 0.0077(5) O1 0.040(2) 0.049(2) 0.036(2) 0.010(2) 0.016(2) 0.021(2) O2 0.021(2) 0.025(2) 0.028(2) 0.0075(14) 0.0068(13) 0.0068(13) O3 0.026(2) 0.024(2) 0.026(2) 0.0047(13) 0.0077(13) 0.0111(13) O4 0.027(2) 0.017(2) 0.029(2) 0.0014(13) 0.0092(14) 0.0067(13) C1 0.025(2) 0.041(3) 0.032(3) 0.010(2) 0.008(2) 0.015(2) C2 0.022(2) 0.031(3) 0.035(3) 0.007(2) 0.005(2) 0.011(2) C3 0.026(3) 0.039(3) 0.043(3) 0.010(2) 0.013(2) 0.014(2) C4 0.031(3) 0.033(3) 0.057(4) 0.009(3) 0.010(3) 0.016(2) C5 0.030(3) 0.032(3) 0.061(4) 0.018(3) 0.005(3) 0.011(2) C6 0.025(3) 0.045(3) 0.045(3) 0.022(3) 0.007(2) 0.016(2) C7 0.049(4) 0.043(3) 0.074(5) 0.010(3) 0.020(3) 0.028(3) C8 0.132(8) 0.084(6) 0.125(8) 0.035(6) 0.091(7) 0.072(6) C9 0.070(6) 0.064(5) 0.152(10) -0.037(6) 0.010(6) 0.027(5) C10 0.072(5) 0.088(6) 0.116(7) 0.028(5) 0.029(5) 0.059(5) C11 0.030(3) 0.062(4) 0.059(4) 0.037(3) 0.010(3) 0.015(3) C12 0.025(2) 0.024(2) 0.026(2) 0.005(2) 0.010(2) 0.009(2) C13 0.027(2) 0.026(2) 0.032(3) 0.008(2) 0.007(2) 0.011(2) C14 0.031(3) 0.031(3) 0.031(3) 0.012(2) 0.006(2) 0.011(2) C15 0.030(3) 0.026(2) 0.035(3) 0.010(2) 0.008(2) 0.008(2) C16 0.024(2) 0.024(2) 0.040(3) 0.008(2) 0.009(2) 0.006(2) C17 0.023(2) 0.019(2) 0.033(3) 0.005(2) 0.006(2) 0.007(2) C18 0.038(3) 0.040(3) 0.050(3) 0.024(3) 0.019(3) 0.012(3) C19 0.050(4) 0.038(4) 0.065(5) 0.021(4) 0.008(4) -0.007(3) C20 0.046(4) 0.064(5) 0.068(6) 0.044(5) 0.012(4) 0.009(4) C21 0.067(5) 0.057(5) 0.073(6) 0.036(4) 0.047(5) 0.024(4) C19' 0.050(4) 0.038(4) 0.065(5) 0.021(4) 0.008(4) -0.007(3) C20' 0.046(4) 0.064(5) 0.068(6) 0.044(5) 0.012(4) 0.009(4) C21' 0.067(5) 0.057(5) 0.073(6) 0.036(4) 0.047(5) 0.024(4) C22 0.021(2) 0.023(2) 0.037(3) 0.009(2) 0.004(2) 0.006(2) C23 0.019(2) 0.030(2) 0.026(2) 0.005(2) 0.001(2) 0.011(2) C24 0.019(2) 0.025(2) 0.029(2) 0.008(2) 0.003(2) 0.008(2) C25 0.024(2) 0.033(3) 0.034(3) 0.015(2) 0.011(2) 0.011(2) C26 0.025(2) 0.031(3) 0.031(3) 0.011(2) 0.007(2) 0.013(2) C27 0.033(3) 0.023(2) 0.031(3) 0.009(2) 0.009(2) 0.012(2) C28 0.024(2) 0.028(2) 0.023(2) 0.009(2) 0.003(2) 0.008(2) C29 0.039(3) 0.035(3) 0.047(3) 0.018(2) 0.019(3) 0.023(2) C30 0.062(4) 0.054(4) 0.081(5) 0.034(4) 0.052(4) 0.037(3) C31 0.072(5) 0.046(4) 0.051(4) 0.008(3) 0.027(3) 0.030(3) C32 0.048(4) 0.061(4) 0.074(5) 0.032(4) 0.028(3) 0.037(3) C33 0.027(2) 0.026(2) 0.032(3) 0.011(2) 0.009(2) 0.010(2) C34 0.029(2) 0.018(2) 0.027(2) 0.001(2) 0.010(2) 0.006(2) C35 0.026(2) 0.024(2) 0.027(2) 0.006(2) 0.010(2) 0.007(2) C36 0.030(3) 0.022(2) 0.046(3) 0.008(2) 0.014(2) 0.010(2) C37 0.038(3) 0.023(3) 0.042(3) 0.000(2) 0.007(2) 0.006(2) C38 0.028(3) 0.028(3) 0.039(3) -0.001(2) 0.000(2) 0.005(2) C39 0.025(2) 0.028(3) 0.036(3) 0.007(2) 0.010(2) 0.010(2) C40 0.049(4) 0.031(3) 0.076(5) -0.019(3) -0.010(3) 0.016(3) C41 0.139(9) 0.096(7) 0.061(5) -0.031(5) -0.009(6) 0.073(7) C42 0.055(5) 0.037(4) 0.218(13) -0.037(6) 0.012(6) -0.006(4) C43 0.095(6) 0.036(4) 0.106(7) -0.024(4) -0.015(5) 0.032(4) C44 0.022(2) 0.030(3) 0.050(3) 0.004(2) 0.003(2) 0.008(2) C45 0.155(18) 0.072(10) 0.095(12) 0.020(9) 0.056(13) 0.005(11) Cl3 0.283(15) 0.181(11) 0.337(14) 0.099(10) 0.175(13) 0.148(11) Cl4 0.344(16) 0.217(12) 0.113(6) 0.023(7) -0.019(9) -0.146(10) Cl5 0.162(4) 0.042(2) 0.057(2) 0.014(2) 0.033(3) 0.005(2) C45' 0.072(14) 0.049(12) 0.075(15) 0.032(11) 0.050(13) 0.029(11) Cl3' 0.127(9) 0.127(10) 0.311(19) 0.147(12) 0.088(11) 0.077(8) Cl4' 0.062(4) 0.103(7) 0.131(10) 0.072(8) -0.001(5) 0.001(4) Cl5' 0.456(29) 0.143(14) 0.116(11) 0.057(10) 0.098(15) -0.073(16) C46 0.148(11) 0.090(8) 0.213(15) 0.105(9) 0.089(11) 0.063(8) Cl6 0.078(3) 0.124(6) 0.087(3) 0.055(3) 0.012(2) -0.009(3) Cl7 0.081(3) 0.094(3) 0.107(3) 0.063(3) 0.009(2) 0.021(2) Cl8 0.143(5) 0.064(3) 0.215(8) 0.019(3) 0.072(5) 0.053(3) C46' 0.148(11) 0.090(8) 0.213(15) 0.105(9) 0.089(11) 0.063(8) Cl6' 0.194(18) 0.090(8) 0.235(18) 0.110(10) 0.039(14) 0.039(10) Cl7' 0.104(10) 0.301(25) 0.242(20) 0.188(20) -0.003(11) 0.025(15) Cl8' 0.306(17) 0.090(7) 0.088(6) 0.026(5) 0.079(8) 0.118(9) C47 0.092(7) 0.097(7) 0.080(6) 0.007(5) -0.010(5) 0.011(6) Cl9 0.189(7) 0.117(4) 0.088(3) 0.033(3) 0.049(4) 0.015(4) ClA 0.202(7) 0.175(7) 0.110(5) -0.032(4) -0.017(4) 0.101(6) ClB 0.198(8) 0.190(8) 0.174(7) 0.048(6) -0.070(6) 0.085(7) C47' 0.092(7) 0.097(7) 0.080(6) 0.007(5) -0.010(5) 0.011(6) Cl9' 0.158(11) 0.152(11) 0.124(9) -0.018(8) 0.041(8) 0.040(9) ClA' 0.229(17) 0.132(10) 0.293(22) 0.054(12) 0.180(16) 0.060(11) ClB' 0.444(33) 0.409(31) 0.452(34) 0.061(30) 0.013(31) 0.004(29) _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 Pd1 P1 2.1874(14) . ? Pd1 Cl2 2.261(2) . ? Pd1 Cl1 2.307(2) . ? Pd1 Cl1 2.392(2) 2_766 ? Cl1 Pd1 2.392(2) 2_766 ? P1 O4 1.573(3) . ? P1 O2 1.574(3) . ? P1 O3 1.583(3) . ? O1 C1 1.374(6) . ? O2 C12 1.419(6) . ? O3 C23 1.414(5) . ? O4 C34 1.418(5) . ? C1 C2 1.386(7) . ? C1 C6 1.387(8) . ? C2 C3 1.398(7) . ? C2 C44 1.502(7) . ? C3 C4 1.377(8) . ? C4 C5 1.394(8) . ? C4 C7 1.536(8) . ? C5 C6 1.389(8) . ? C6 C11 1.499(8) . ? C7 C9 1.492(10) . ? C7 C10 1.504(11) . ? C7 C8 1.512(11) . ? C11 C13 1.525(7) . ? C12 C13 1.378(7) . ? C12 C17 1.411(7) . ? C13 C14 1.405(7) . ? C14 C15 1.371(7) . ? C15 C16 1.383(7) . ? C15 C18 1.521(7) . ? C16 C17 1.388(7) . ? C17 C22 1.512(7) . ? C18 C20' 1.44(4) . ? C18 C21' 1.50(5) . ? C18 C20 1.513(10) . ? C18 C21 1.519(9) . ? C18 C19 1.568(9) . ? C18 C19' 1.69(4) . ? C22 C24 1.502(6) . ? C23 C24 1.371(7) . ? C23 C28 1.377(7) . ? C24 C25 1.402(7) . ? C25 C26 1.379(7) . ? C26 C27 1.389(7) . ? C26 C29 1.545(7) . ? C27 C28 1.395(7) . ? C28 C33 1.505(6) . ? C29 C30 1.523(8) . ? C29 C32 1.526(8) . ? C29 C31 1.538(9) . ? C33 C35 1.516(7) . ? C34 C35 1.391(7) . ? C34 C39 1.392(7) . ? C35 C36 1.387(7) . ? C36 C37 1.384(8) . ? C37 C38 1.394(8) . ? C37 C40 1.538(7) . ? C38 C39 1.379(7) . ? C39 C44 1.521(7) . ? C40 C42 1.484(11) . ? C40 C43 1.511(10) . ? C40 C41 1.553(13) . ? C45 Cl4 1.68(2) . ? C45 Cl3 1.69(2) . ? C45 Cl5 1.759(13) . ? C45' Cl3' 1.72(2) . ? C45' Cl5' 1.74(2) . ? C45' Cl4' 1.79(2) . ? C46 Cl6 1.708(12) . ? C46 Cl7 1.842(12) . ? C46 Cl8 1.882(13) . ? C46' Cl7' 1.54(2) . ? C46' Cl8' 1.567(14) . ? C46' Cl6' 1.61(2) . ? C47 ClB 1.613(11) . ? C47 Cl9 1.652(11) . ? C47 ClA 1.768(11) . ? C47' Cl9' 1.632(13) . ? C47' ClA' 1.779(14) . ? C47' ClB' 1.79(2) . ? ClA' ClB' 2.46(3) . ? Cl20 Cl22 0.73(2) . ? Cl20 Cl20 2.12(4) 2_666 ? 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 P1 Pd1 Cl2 88.73(6) . . ? P1 Pd1 Cl1 94.54(5) . . ? Cl2 Pd1 Cl1 176.34(5) . . ? P1 Pd1 Cl1 173.53(6) . 2_766 ? Cl2 Pd1 Cl1 90.54(6) . 2_766 ? Cl1 Pd1 Cl1 86.02(5) . 2_766 ? Pd1 Cl1 Pd1 93.98(5) . 2_766 ? O4 P1 O2 104.9(2) . . ? O4 P1 O3 107.5(2) . . ? O2 P1 O3 104.8(2) . . ? O4 P1 Pd1 109.19(13) . . ? O2 P1 Pd1 122.53(13) . . ? O3 P1 Pd1 107.11(13) . . ? C12 O2 P1 135.8(3) . . ? C23 O3 P1 121.5(3) . . ? C34 O4 P1 138.7(3) . . ? O1 C1 C2 122.0(5) . . ? O1 C1 C6 117.2(5) . . ? C2 C1 C6 120.8(5) . . ? C1 C2 C3 117.9(5) . . ? C1 C2 C44 121.2(5) . . ? C3 C2 C44 121.0(5) . . ? C4 C3 C2 123.1(5) . . ? C3 C4 C5 116.6(5) . . ? C3 C4 C7 121.9(5) . . ? C5 C4 C7 121.4(5) . . ? C6 C5 C4 122.2(5) . . ? C1 C6 C5 118.7(5) . . ? C1 C6 C11 119.3(5) . . ? C5 C6 C11 121.8(5) . . ? C9 C7 C10 111.3(7) . . ? C9 C7 C8 106.5(8) . . ? C10 C7 C8 107.1(7) . . ? C9 C7 C4 111.5(6) . . ? C10 C7 C4 108.2(6) . . ? C8 C7 C4 112.1(6) . . ? C6 C11 C13 120.7(5) . . ? C13 C12 C17 121.2(4) . . ? C13 C12 O2 118.4(4) . . ? C17 C12 O2 120.2(4) . . ? C12 C13 C14 117.6(4) . . ? C12 C13 C11 129.0(5) . . ? C14 C13 C11 113.3(4) . . ? C15 C14 C13 123.9(5) . . ? C14 C15 C16 115.9(5) . . ? C14 C15 C18 123.2(5) . . ? C16 C15 C18 120.9(5) . . ? C15 C16 C17 124.1(5) . . ? C16 C17 C12 117.2(4) . . ? C16 C17 C22 117.0(4) . . ? C12 C17 C22 125.6(4) . . ? C20' C18 C21' 113.6(29) . . ? C20 C18 C21 109.6(6) . . ? C20' C18 C15 116.8(17) . . ? C21' C18 C15 110.9(17) . . ? C20 C18 C15 113.4(5) . . ? C21 C18 C15 109.6(5) . . ? C20 C18 C19 107.2(6) . . ? C21 C18 C19 108.0(6) . . ? C15 C18 C19 108.9(5) . . ? C20' C18 C19' 108.9(27) . . ? C21' C18 C19' 102.7(28) . . ? C15 C18 C19' 102.4(14) . . ? C24 C22 C17 115.5(4) . . ? C24 C23 C28 123.7(4) . . ? C24 C23 O3 117.9(4) . . ? C28 C23 O3 118.5(4) . . ? C23 C24 C25 117.2(4) . . ? C23 C24 C22 119.8(4) . . ? C25 C24 C22 123.0(4) . . ? C26 C25 C24 121.7(4) . . ? C25 C26 C27 118.4(4) . . ? C25 C26 C29 122.8(4) . . ? C27 C26 C29 118.7(4) . . ? C26 C27 C28 121.7(4) . . ? C23 C28 C27 117.2(4) . . ? C23 C28 C33 120.5(4) . . ? C27 C28 C33 122.1(4) . . ? C30 C29 C32 108.7(5) . . ? C30 C29 C31 108.8(5) . . ? C32 C29 C31 108.6(5) . . ? C30 C29 C26 111.9(4) . . ? C32 C29 C26 109.4(5) . . ? C31 C29 C26 109.4(4) . . ? C28 C33 C35 109.5(4) . . ? C35 C34 C39 120.9(4) . . ? C35 C34 O4 120.9(4) . . ? C39 C34 O4 117.6(4) . . ? C36 C35 C34 118.1(5) . . ? C36 C35 C33 118.6(4) . . ? C34 C35 C33 123.3(4) . . ? C37 C36 C35 122.7(5) . . ? C36 C37 C38 116.3(5) . . ? C36 C37 C40 122.3(5) . . ? C38 C37 C40 121.3(5) . . ? C39 C38 C37 123.4(5) . . ? C38 C39 C34 117.6(4) . . ? C38 C39 C44 118.1(5) . . ? C34 C39 C44 124.0(4) . . ? C42 C40 C43 112.4(8) . . ? C42 C40 C37 111.9(6) . . ? C43 C40 C37 112.4(5) . . ? C42 C40 C41 105.9(8) . . ? C43 C40 C41 106.7(7) . . ? C37 C40 C41 107.0(6) . . ? C2 C44 C39 119.1(4) . . ? Cl4 C45 Cl3 105.7(14) . . ? Cl4 C45 Cl5 114.3(10) . . ? Cl3 C45 Cl5 104.0(10) . . ? Cl3' C45' Cl5' 103.3(16) . . ? Cl3' C45' Cl4' 111.8(12) . . ? Cl5' C45' Cl4' 102.7(17) . . ? Cl6 C46 Cl7 107.5(6) . . ? Cl6 C46 Cl8 103.7(7) . . ? Cl7 C46 Cl8 108.7(6) . . ? Cl7' C46' Cl8' 107.8(11) . . ? Cl7' C46' Cl6' 119.4(13) . . ? Cl8' C46' Cl6' 121.7(14) . . ? ClB C47 Cl9 117.7(8) . . ? ClB C47 ClA 107.1(6) . . ? Cl9 C47 ClA 109.6(7) . . ? Cl9' C47' ClA' 121.4(12) . . ? Cl9' C47' ClB' 96.5(12) . . ? ClA' C47' ClB' 87.2(11) . . ? C47' ClA' ClB' 46.6(7) . . ? C47' ClB' ClA' 46.2(7) . . ? Cl22 Cl20 Cl20 157.0(34) . 2_666 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pd1 Cl1 Pd1 -173.53(6) . . . 2_766 ? Cl2 Pd1 Cl1 Pd1 -20.3(10) . . . 2_766 ? Cl1 Pd1 Cl1 Pd1 0.0 2_766 . . 2_766 ? Cl2 Pd1 P1 O4 166.51(15) . . . . ? Cl1 Pd1 P1 O4 -15.14(15) . . . . ? Cl1 Pd1 P1 O4 -109.9(4) 2_766 . . . ? Cl2 Pd1 P1 O2 43.5(2) . . . . ? Cl1 Pd1 P1 O2 -138.1(2) . . . . ? Cl1 Pd1 P1 O2 127.1(4) 2_766 . . . ? Cl2 Pd1 P1 O3 -77.40(14) . . . . ? Cl1 Pd1 P1 O3 100.95(14) . . . . ? Cl1 Pd1 P1 O3 6.2(5) 2_766 . . . ? O4 P1 O2 C12 -172.6(4) . . . . ? O3 P1 O2 C12 74.3(4) . . . . ? Pd1 P1 O2 C12 -47.7(5) . . . . ? O4 P1 O3 C23 -76.0(4) . . . . ? O2 P1 O3 C23 35.2(4) . . . . ? Pd1 P1 O3 C23 166.7(3) . . . . ? O2 P1 O4 C34 -49.1(5) . . . . ? O3 P1 O4 C34 62.0(5) . . . . ? Pd1 P1 O4 C34 177.9(4) . . . . ? O1 C1 C2 C3 173.8(5) . . . . ? C6 C1 C2 C3 -7.7(8) . . . . ? O1 C1 C2 C44 -5.1(8) . . . . ? C6 C1 C2 C44 173.4(5) . . . . ? C1 C2 C3 C4 1.2(8) . . . . ? C44 C2 C3 C4 -179.9(5) . . . . ? C2 C3 C4 C5 5.0(9) . . . . ? C2 C3 C4 C7 -171.6(5) . . . . ? C3 C4 C5 C6 -5.0(9) . . . . ? C7 C4 C5 C6 171.6(6) . . . . ? O1 C1 C6 C5 -173.7(5) . . . . ? C2 C1 C6 C5 7.7(8) . . . . ? O1 C1 C6 C11 1.2(7) . . . . ? C2 C1 C6 C11 -177.4(5) . . . . ? C4 C5 C6 C1 -1.1(8) . . . . ? C4 C5 C6 C11 -175.9(5) . . . . ? C3 C4 C7 C9 -134.4(8) . . . . ? C5 C4 C7 C9 49.2(10) . . . . ? C3 C4 C7 C10 102.8(8) . . . . ? C5 C4 C7 C10 -73.6(8) . . . . ? C3 C4 C7 C8 -15.0(10) . . . . ? C5 C4 C7 C8 168.6(7) . . . . ? C1 C6 C11 C13 86.2(7) . . . . ? C5 C6 C11 C13 -99.0(7) . . . . ? P1 O2 C12 C13 121.5(4) . . . . ? P1 O2 C12 C17 -63.5(6) . . . . ? C17 C12 C13 C14 -2.4(7) . . . . ? O2 C12 C13 C14 172.5(4) . . . . ? C17 C12 C13 C11 179.8(5) . . . . ? O2 C12 C13 C11 -5.3(8) . . . . ? C6 C11 C13 C12 -21.8(9) . . . . ? C6 C11 C13 C14 160.3(5) . . . . ? C12 C13 C14 C15 0.7(8) . . . . ? C11 C13 C14 C15 178.8(5) . . . . ? C13 C14 C15 C16 1.3(8) . . . . ? C13 C14 C15 C18 -179.6(5) . . . . ? C14 C15 C16 C17 -1.7(8) . . . . ? C18 C15 C16 C17 179.2(5) . . . . ? C15 C16 C17 C12 0.1(7) . . . . ? C15 C16 C17 C22 176.1(5) . . . . ? C13 C12 C17 C16 2.1(7) . . . . ? O2 C12 C17 C16 -172.8(4) . . . . ? C13 C12 C17 C22 -173.6(4) . . . . ? O2 C12 C17 C22 11.6(7) . . . . ? C14 C15 C18 C20' -169.2(26) . . . . ? C16 C15 C18 C20' 9.8(26) . . . . ? C14 C15 C18 C21' -37.1(27) . . . . ? C16 C15 C18 C21' 142.0(26) . . . . ? C14 C15 C18 C20 -2.1(9) . . . . ? C16 C15 C18 C20 176.9(6) . . . . ? C14 C15 C18 C21 120.7(7) . . . . ? C16 C15 C18 C21 -60.2(7) . . . . ? C14 C15 C18 C19 -121.3(6) . . . . ? C16 C15 C18 C19 57.7(7) . . . . ? C14 C15 C18 C19' 71.9(18) . . . . ? C16 C15 C18 C19' -109.1(18) . . . . ? C16 C17 C22 C24 125.9(5) . . . . ? C12 C17 C22 C24 -58.4(6) . . . . ? P1 O3 C23 C24 -89.1(5) . . . . ? P1 O3 C23 C28 91.7(5) . . . . ? C28 C23 C24 C25 1.6(7) . . . . ? O3 C23 C24 C25 -177.5(4) . . . . ? C28 C23 C24 C22 -178.1(4) . . . . ? O3 C23 C24 C22 2.8(6) . . . . ? C17 C22 C24 C23 90.2(6) . . . . ? C17 C22 C24 C25 -89.5(6) . . . . ? C23 C24 C25 C26 -0.3(7) . . . . ? C22 C24 C25 C26 179.4(5) . . . . ? C24 C25 C26 C27 0.3(7) . . . . ? C24 C25 C26 C29 178.3(5) . . . . ? C25 C26 C27 C28 -1.5(7) . . . . ? C29 C26 C27 C28 -179.6(5) . . . . ? C24 C23 C28 C27 -2.8(7) . . . . ? O3 C23 C28 C27 176.3(4) . . . . ? C24 C23 C28 C33 172.5(4) . . . . ? O3 C23 C28 C33 -8.4(6) . . . . ? C26 C27 C28 C23 2.7(7) . . . . ? C26 C27 C28 C33 -172.5(5) . . . . ? C25 C26 C29 C30 9.5(8) . . . . ? C27 C26 C29 C30 -172.5(5) . . . . ? C25 C26 C29 C32 -111.1(6) . . . . ? C27 C26 C29 C32 66.9(6) . . . . ? C25 C26 C29 C31 130.1(5) . . . . ? C27 C26 C29 C31 -51.9(6) . . . . ? C23 C28 C33 C35 -88.7(5) . . . . ? C27 C28 C33 C35 86.4(5) . . . . ? P1 O4 C34 C35 -62.7(7) . . . . ? P1 O4 C34 C39 126.0(5) . . . . ? C39 C34 C35 C36 -10.6(7) . . . . ? O4 C34 C35 C36 178.4(4) . . . . ? C39 C34 C35 C33 169.0(4) . . . . ? O4 C34 C35 C33 -2.0(7) . . . . ? C28 C33 C35 C36 -94.8(5) . . . . ? C28 C33 C35 C34 85.6(5) . . . . ? C34 C35 C36 C37 3.0(8) . . . . ? C33 C35 C36 C37 -176.7(5) . . . . ? C35 C36 C37 C38 4.1(8) . . . . ? C35 C36 C37 C40 -175.0(6) . . . . ? C36 C37 C38 C39 -3.8(9) . . . . ? C40 C37 C38 C39 175.2(6) . . . . ? C37 C38 C39 C34 -3.4(8) . . . . ? C37 C38 C39 C44 170.4(5) . . . . ? C35 C34 C39 C38 10.8(7) . . . . ? O4 C34 C39 C38 -177.9(4) . . . . ? C35 C34 C39 C44 -162.6(5) . . . . ? O4 C34 C39 C44 8.7(7) . . . . ? C36 C37 C40 C42 -135.9(8) . . . . ? C38 C37 C40 C42 45.1(11) . . . . ? C36 C37 C40 C43 -8.3(10) . . . . ? C38 C37 C40 C43 172.8(7) . . . . ? C36 C37 C40 C41 108.5(7) . . . . ? C38 C37 C40 C41 -70.5(8) . . . . ? C1 C2 C44 C39 -43.9(7) . . . . ? C3 C2 C44 C39 137.2(5) . . . . ? C38 C39 C44 C2 141.7(5) . . . . ? C34 C39 C44 C2 -45.0(8) . . . . ? Cl9' C47' ClA' ClB' -95.9(15) . . . . ? ClB' C47' ClA' ClB' 0.000(13) . . . . ? Cl9' C47' ClB' ClA' 121.3(12) . . . . ? ClA' C47' ClB' ClA' 0.000(12) . . . . ? C47' ClA' ClB' C47' 0.00(2) . . . . ? _refine_diff_density_max 0.464 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.090 data_13a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H36 Cl Ir O4 P' _chemical_formula_weight 827.30 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.914(2) _cell_length_b 10.115(2) _cell_length_c 18.556(3) _cell_angle_alpha 82.27(2) _cell_angle_beta 84.47(2) _cell_angle_gamma 71.912(14) _cell_volume 1573.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method ? _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 4.422 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10208 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6990 _reflns_number_observed 6531 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SMART (Siemens, 1995b)' _computing_data_reduction 'SMART (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 on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+5.5201P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6989 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_obs 0.0288 _refine_ls_wR_factor_all 0.0724 _refine_ls_wR_factor_obs 0.0672 _refine_ls_goodness_of_fit_all 1.152 _refine_ls_goodness_of_fit_obs 1.109 _refine_ls_restrained_S_all 1.152 _refine_ls_restrained_S_obs 1.109 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ir1 Ir -0.22163(2) 0.26600(2) 0.359075(8) 0.01919(5) Uani 1 d . . Cl1 Cl -0.38349(12) 0.40856(11) 0.26748(6) 0.0288(2) Uani 1 d . . P1 P -0.04349(11) 0.13814(10) 0.28010(5) 0.0161(2) Uani 1 d . . O1 O 0.3444(4) 0.2667(4) 0.1954(2) 0.0420(9) Uani 1 d . . H1 H 0.4337(4) 0.2582(63) 0.2098(22) 0.063 Uiso 1 calc R . O2 O 0.0001(3) 0.1949(3) 0.19808(14) 0.0187(5) Uani 1 d . . O3 O -0.0876(3) 0.0008(3) 0.26811(14) 0.0192(5) Uani 1 d . . O4 O 0.1247(3) 0.0778(3) 0.31478(14) 0.0182(5) Uani 1 d . . C1 C 0.2291(5) 0.3422(4) 0.2410(2) 0.0243(8) Uani 1 d . . C2 C 0.2369(5) 0.3158(4) 0.3166(2) 0.0241(8) Uani 1 d . . C3 C 0.1232(6) 0.4058(5) 0.3587(3) 0.0315(10) Uani 1 d . . H3 H 0.1298(6) 0.3938(5) 0.4101(3) 0.038 Uiso 1 calc R . C4 C 0.0010(6) 0.5122(5) 0.3275(3) 0.0362(11) Uani 1 d . . H4 H -0.0723(6) 0.5757(5) 0.3570(3) 0.043 Uiso 1 calc R . C5 C -0.0141(6) 0.5257(5) 0.2530(3) 0.0311(9) Uani 1 d . . H5 H -0.1020(6) 0.5948(5) 0.2319(3) 0.037 Uiso 1 calc R . C6 C 0.0983(5) 0.4391(4) 0.2092(2) 0.0232(8) Uani 1 d . . C7 C 0.0759(5) 0.4403(4) 0.1298(2) 0.0262(9) Uani 1 d . . H7A H 0.1695(5) 0.3720(4) 0.1085(2) 0.031 Uiso 1 calc R . H7B H 0.0706(5) 0.5341(4) 0.1045(2) 0.031 Uiso 1 calc R . C8 C -0.1045(5) 0.2826(4) 0.1457(2) 0.0218(8) Uani 1 d . . C9 C -0.0704(5) 0.4053(4) 0.1155(2) 0.0236(8) Uani 1 d . . C10 C -0.1764(6) 0.4970(5) 0.0668(3) 0.0338(10) Uani 1 d . . H10 H -0.1583(6) 0.5826(5) 0.0468(3) 0.041 Uiso 1 calc R . C11 C -0.3063(6) 0.4664(5) 0.0472(3) 0.0409(12) Uani 1 d . . H11 H -0.3789(6) 0.5318(5) 0.0157(3) 0.049 Uiso 1 calc R . C12 C -0.3294(6) 0.3413(5) 0.0735(3) 0.0354(10) Uani 1 d . . H12 H -0.4165(6) 0.3190(5) 0.0583(3) 0.042 Uiso 1 calc R . C13 C -0.2283(5) 0.2447(5) 0.1225(2) 0.0260(8) Uani 1 d . . C14 C -0.2617(6) 0.1069(5) 0.1461(3) 0.0312(10) Uani 1 d . . H14A H -0.3105(6) 0.1083(5) 0.1964(3) 0.037 Uiso 1 calc R . H14B H -0.3391(6) 0.0970(5) 0.1139(3) 0.037 Uiso 1 calc R . C15 C -0.0282(5) -0.0663(4) 0.2049(2) 0.0217(8) Uani 1 d . . C16 C -0.1171(6) -0.0174(5) 0.1439(2) 0.0272(9) Uani 1 d . . C17 C -0.0604(7) -0.0852(5) 0.0817(3) 0.0372(11) Uani 1 d . . H17 H -0.1184(7) -0.0569(5) 0.0390(3) 0.045 Uiso 1 calc R . C18 C 0.0797(7) -0.1933(5) 0.0818(3) 0.0394(12) Uani 1 d . . H18 H 0.1177(7) -0.2371(5) 0.0386(3) 0.047 Uiso 1 calc R . C19 C 0.1668(6) -0.2396(5) 0.1438(3) 0.0333(10) Uani 1 d . . H19 H 0.2624(6) -0.3147(5) 0.1429(3) 0.040 Uiso 1 calc R . C20 C 0.1119(5) -0.1740(4) 0.2076(2) 0.0256(9) Uani 1 d . . C21 C 0.2006(5) -0.2169(4) 0.2767(2) 0.0267(9) Uani 1 d . . H21A H 0.2562(5) -0.3186(4) 0.2798(2) 0.032 Uiso 1 calc R . H21B H 0.1229(5) -0.2005(4) 0.3189(2) 0.032 Uiso 1 calc R . C22 C 0.2817(5) -0.0035(4) 0.3019(2) 0.0196(7) Uani 1 d . . C23 C 0.3203(5) -0.1408(4) 0.2828(2) 0.0246(8) Uani 1 d . . C24 C 0.4815(6) -0.2139(5) 0.2743(3) 0.0341(10) Uani 1 d . . H24 H 0.5116(6) -0.3053(5) 0.2594(3) 0.041 Uiso 1 calc R . C25 C 0.5976(6) -0.1578(6) 0.2868(3) 0.0402(12) Uani 1 d . . H25 H 0.7060(6) -0.2086(6) 0.2792(3) 0.048 Uiso 1 calc R . C26 C 0.5550(5) -0.0273(5) 0.3105(3) 0.0311(10) Uani 1 d . . H26 H 0.6353(5) 0.0091(5) 0.3215(3) 0.037 Uiso 1 calc R . C27 C 0.3965(5) 0.0534(4) 0.3189(2) 0.0225(8) Uani 1 d . . C28 C 0.3607(5) 0.1913(5) 0.3504(2) 0.0271(9) Uani 1 d . . H28A H 0.3284(5) 0.1761(5) 0.4026(2) 0.032 Uiso 1 calc R . H28B H 0.4604(5) 0.2159(5) 0.3478(2) 0.032 Uiso 1 calc R . C101 C -0.1053(6) 0.2693(6) 0.5113(3) 0.0396(12) Uani 1 d . . H10A H -0.1554(6) 0.2247(6) 0.5535(3) 0.048 Uiso 1 calc R . H10B H -0.0031(6) 0.2734(6) 0.5260(3) 0.048 Uiso 1 calc R . C102 C -0.2115(6) 0.4178(6) 0.4917(3) 0.0405(12) Uani 1 d . . H10C H -0.2719(6) 0.4537(6) 0.5363(3) 0.049 Uiso 1 calc R . H10D H -0.1446(6) 0.4784(6) 0.4733(3) 0.049 Uiso 1 calc R . C103 C -0.3264(5) 0.4274(5) 0.4348(3) 0.0319(10) Uani 1 d . . H103 H -0.3730(5) 0.5239(5) 0.4102(3) 0.038 Uiso 1 calc R . C104 C -0.4232(5) 0.3425(5) 0.4392(2) 0.0282(9) Uani 1 d . . H104 H -0.5271(5) 0.3885(5) 0.4169(2) 0.034 Uiso 1 calc R . C105 C -0.4274(6) 0.2310(6) 0.5023(3) 0.0380(11) Uani 1 d . . H10E H -0.5363(6) 0.2246(6) 0.5110(3) 0.046 Uiso 1 calc R . H10F H -0.3980(6) 0.2585(6) 0.5469(3) 0.046 Uiso 1 calc R . C106 C -0.3147(6) 0.0879(5) 0.4873(3) 0.0354(10) Uani 1 d . . H10G H -0.2811(6) 0.0329(5) 0.5345(3) 0.042 Uiso 1 calc R . H10H H -0.3728(6) 0.0379(5) 0.4638(3) 0.042 Uiso 1 calc R . C107 C -0.1683(6) 0.0928(5) 0.4394(2) 0.0290(9) Uani 1 d . . H107 H -0.1082(6) 0.0021(5) 0.4203(2) 0.035 Uiso 1 calc R . C108 C -0.0738(5) 0.1787(5) 0.4484(2) 0.0299(9) Uani 1 d . . H108 H 0.0407(5) 0.1384(5) 0.4337(2) 0.036 Uiso 1 calc R . C203 C -0.4758(8) -0.1195(6) 0.0484(4) 0.053(2) Uani 1 d . . H203 H -0.4594(8) -0.2021(6) 0.0816(4) 0.064 Uiso 1 calc R . C201 C -0.6111(7) 0.1222(6) 0.0171(3) 0.0483(13) Uani 1 d . . H201 H -0.6882(7) 0.2064(6) 0.0288(3) 0.058 Uiso 1 calc R . C202 C -0.5864(8) 0.0025(7) 0.0660(3) 0.0513(14) Uani 1 d . . H202 H -0.6454(8) 0.0045(7) 0.1115(3) 0.062 Uiso 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 Ir1 0.01770(8) 0.01977(8) 0.02064(8) -0.00434(5) -0.00075(5) -0.00563(5) Cl1 0.0245(5) 0.0255(5) 0.0315(5) 0.0016(4) -0.0033(4) -0.0020(4) P1 0.0158(4) 0.0171(4) 0.0168(4) 0.0004(3) -0.0021(3) -0.0076(3) O1 0.030(2) 0.044(2) 0.035(2) 0.006(2) 0.0101(14) 0.006(2) O2 0.0227(14) 0.0180(13) 0.0174(13) 0.0014(10) -0.0039(10) -0.0093(11) O3 0.0234(14) 0.0194(13) 0.0177(13) -0.0004(10) 0.0005(10) -0.0120(11) O4 0.0165(13) 0.0188(13) 0.0197(13) -0.0012(10) -0.0007(10) -0.0063(10) C1 0.022(2) 0.024(2) 0.028(2) -0.002(2) 0.003(2) -0.011(2) C2 0.024(2) 0.025(2) 0.028(2) -0.003(2) -0.003(2) -0.015(2) C3 0.037(2) 0.030(2) 0.034(2) -0.012(2) -0.005(2) -0.013(2) C4 0.039(3) 0.028(2) 0.039(3) -0.015(2) 0.000(2) -0.004(2) C5 0.032(2) 0.020(2) 0.039(3) -0.003(2) -0.004(2) -0.005(2) C6 0.024(2) 0.019(2) 0.030(2) 0.001(2) -0.004(2) -0.012(2) C7 0.032(2) 0.020(2) 0.028(2) 0.003(2) -0.004(2) -0.011(2) C8 0.027(2) 0.020(2) 0.019(2) -0.0003(14) -0.0015(15) -0.007(2) C9 0.026(2) 0.021(2) 0.023(2) 0.0004(15) -0.001(2) -0.007(2) C10 0.041(3) 0.026(2) 0.032(2) 0.009(2) -0.009(2) -0.010(2) C11 0.042(3) 0.037(3) 0.040(3) 0.012(2) -0.017(2) -0.008(2) C12 0.033(2) 0.041(3) 0.033(2) 0.005(2) -0.014(2) -0.013(2) C13 0.028(2) 0.027(2) 0.024(2) 0.001(2) -0.005(2) -0.011(2) C14 0.035(2) 0.037(2) 0.029(2) 0.004(2) -0.014(2) -0.022(2) C15 0.033(2) 0.020(2) 0.017(2) -0.0022(14) 0.000(2) -0.016(2) C16 0.041(2) 0.028(2) 0.022(2) 0.001(2) -0.005(2) -0.024(2) C17 0.065(3) 0.035(3) 0.025(2) -0.001(2) -0.007(2) -0.034(3) C18 0.070(4) 0.031(2) 0.026(2) -0.011(2) 0.008(2) -0.029(2) C19 0.048(3) 0.026(2) 0.030(2) -0.010(2) 0.009(2) -0.019(2) C20 0.036(2) 0.018(2) 0.026(2) -0.002(2) 0.005(2) -0.016(2) C21 0.034(2) 0.017(2) 0.028(2) -0.001(2) 0.000(2) -0.006(2) C22 0.020(2) 0.020(2) 0.016(2) 0.0029(14) -0.0007(14) -0.0048(15) C23 0.024(2) 0.023(2) 0.023(2) -0.001(2) 0.004(2) -0.004(2) C24 0.031(2) 0.022(2) 0.041(3) -0.001(2) 0.005(2) 0.002(2) C25 0.020(2) 0.042(3) 0.047(3) 0.002(2) 0.004(2) 0.004(2) C26 0.018(2) 0.039(3) 0.034(2) 0.006(2) -0.003(2) -0.009(2) C27 0.019(2) 0.026(2) 0.020(2) 0.0044(15) -0.0011(14) -0.007(2) C28 0.023(2) 0.033(2) 0.029(2) -0.001(2) -0.006(2) -0.013(2) C101 0.032(3) 0.060(3) 0.028(2) -0.015(2) -0.007(2) -0.011(2) C102 0.034(3) 0.053(3) 0.041(3) -0.028(2) 0.000(2) -0.015(2) C103 0.030(2) 0.030(2) 0.036(2) -0.017(2) 0.000(2) -0.004(2) C104 0.022(2) 0.034(2) 0.026(2) -0.014(2) 0.007(2) -0.004(2) C105 0.034(3) 0.051(3) 0.029(2) -0.010(2) 0.007(2) -0.014(2) C106 0.037(3) 0.040(3) 0.025(2) 0.004(2) 0.003(2) -0.011(2) C107 0.035(2) 0.029(2) 0.019(2) 0.002(2) -0.003(2) -0.005(2) C108 0.023(2) 0.042(3) 0.020(2) -0.006(2) -0.007(2) -0.001(2) C203 0.072(4) 0.039(3) 0.057(4) 0.004(3) -0.021(3) -0.026(3) C201 0.054(3) 0.038(3) 0.052(3) -0.006(2) -0.014(3) -0.009(3) C202 0.057(4) 0.061(4) 0.046(3) -0.011(3) -0.003(3) -0.032(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 Ir1 C107 2.106(4) . ? Ir1 C108 2.137(4) . ? Ir1 C103 2.220(4) . ? Ir1 C104 2.230(4) . ? Ir1 P1 2.2644(11) . ? Ir1 Cl1 2.3605(11) . ? P1 O4 1.596(3) . ? P1 O3 1.604(3) . ? P1 O2 1.608(3) . ? O1 C1 1.370(5) . ? O2 C8 1.425(5) . ? O3 C15 1.410(5) . ? O4 C22 1.402(5) . ? C1 C6 1.391(6) . ? C1 C2 1.395(6) . ? C2 C3 1.390(6) . ? C2 C28 1.502(6) . ? C3 C4 1.380(7) . ? C4 C5 1.386(7) . ? C5 C6 1.386(6) . ? C6 C7 1.505(6) . ? C7 C9 1.508(6) . ? C8 C13 1.396(6) . ? C8 C9 1.401(6) . ? C9 C10 1.401(6) . ? C10 C11 1.380(7) . ? C11 C12 1.363(7) . ? C12 C13 1.402(6) . ? C13 C14 1.514(6) . ? C14 C16 1.497(7) . ? C15 C20 1.379(6) . ? C15 C16 1.390(6) . ? C16 C17 1.395(7) . ? C17 C18 1.381(8) . ? C18 C19 1.395(7) . ? C19 C20 1.407(6) . ? C20 C21 1.514(6) . ? C21 C23 1.517(6) . ? C22 C27 1.399(6) . ? C22 C23 1.408(6) . ? C23 C24 1.402(6) . ? C24 C25 1.377(8) . ? C25 C26 1.375(7) . ? C26 C27 1.401(6) . ? C27 C28 1.515(6) . ? C101 C102 1.523(8) . ? C101 C108 1.531(6) . ? C102 C103 1.513(7) . ? C103 C104 1.385(7) . ? C104 C105 1.518(7) . ? C105 C106 1.527(7) . ? C106 C107 1.517(6) . ? C107 C108 1.419(7) . ? C203 C202 1.375(9) . ? C203 C201 1.376(9) 2_455 ? C201 C203 1.376(9) 2_455 ? C201 C202 1.384(9) . ? 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 C107 Ir1 C108 39.1(2) . . ? C107 Ir1 C103 96.5(2) . . ? C108 Ir1 C103 80.2(2) . . ? C107 Ir1 C104 81.2(2) . . ? C108 Ir1 C104 88.5(2) . . ? C103 Ir1 C104 36.3(2) . . ? C107 Ir1 P1 89.66(13) . . ? C108 Ir1 P1 92.44(12) . . ? C103 Ir1 P1 158.98(13) . . ? C104 Ir1 P1 164.30(12) . . ? C107 Ir1 Cl1 150.92(13) . . ? C108 Ir1 Cl1 167.70(13) . . ? C103 Ir1 Cl1 89.79(13) . . ? C104 Ir1 Cl1 87.51(12) . . ? P1 Ir1 Cl1 94.51(4) . . ? O4 P1 O3 103.89(15) . . ? O4 P1 O2 102.95(14) . . ? O3 P1 O2 101.93(14) . . ? O4 P1 Ir1 109.72(11) . . ? O3 P1 Ir1 111.07(11) . . ? O2 P1 Ir1 125.12(11) . . ? C8 O2 P1 128.0(3) . . ? C15 O3 P1 119.8(2) . . ? C22 O4 P1 143.5(3) . . ? O1 C1 C6 117.2(4) . . ? O1 C1 C2 121.3(4) . . ? C6 C1 C2 121.3(4) . . ? C3 C2 C1 117.6(4) . . ? C3 C2 C28 121.8(4) . . ? C1 C2 C28 120.6(4) . . ? C4 C3 C2 121.5(4) . . ? C3 C4 C5 119.5(4) . . ? C4 C5 C6 120.5(4) . . ? C5 C6 C1 118.7(4) . . ? C5 C6 C7 121.6(4) . . ? C1 C6 C7 119.5(4) . . ? C6 C7 C9 114.0(4) . . ? C13 C8 C9 121.7(4) . . ? C13 C8 O2 122.1(3) . . ? C9 C8 O2 116.1(3) . . ? C8 C9 C10 117.2(4) . . ? C8 C9 C7 123.9(4) . . ? C10 C9 C7 118.8(4) . . ? C11 C10 C9 121.8(4) . . ? C12 C11 C10 119.3(4) . . ? C11 C12 C13 121.9(4) . . ? C8 C13 C12 117.6(4) . . ? C8 C13 C14 125.0(4) . . ? C12 C13 C14 117.4(4) . . ? C16 C14 C13 113.3(4) . . ? C20 C15 C16 124.9(4) . . ? C20 C15 O3 118.5(4) . . ? C16 C15 O3 116.6(4) . . ? C15 C16 C17 116.8(4) . . ? C15 C16 C14 120.0(4) . . ? C17 C16 C14 123.1(4) . . ? C18 C17 C16 120.3(5) . . ? C17 C18 C19 121.6(4) . . ? C18 C19 C20 119.4(5) . . ? C15 C20 C19 117.0(4) . . ? C15 C20 C21 120.4(4) . . ? C19 C20 C21 122.6(4) . . ? C20 C21 C23 114.9(3) . . ? C27 C22 O4 115.3(3) . . ? C27 C22 C23 122.2(4) . . ? O4 C22 C23 122.0(3) . . ? C24 C23 C22 116.8(4) . . ? C24 C23 C21 118.6(4) . . ? C22 C23 C21 124.5(4) . . ? C25 C24 C23 122.2(4) . . ? C26 C25 C24 119.3(4) . . ? C25 C26 C27 121.9(4) . . ? C22 C27 C26 117.3(4) . . ? C22 C27 C28 124.5(4) . . ? C26 C27 C28 118.1(4) . . ? C2 C28 C27 118.3(3) . . ? C102 C101 C108 113.0(4) . . ? C103 C102 C101 113.2(4) . . ? C104 C103 C102 123.8(5) . . ? C104 C103 Ir1 72.2(2) . . ? C102 C103 Ir1 110.4(3) . . ? C103 C104 C105 123.6(4) . . ? C103 C104 Ir1 71.5(2) . . ? C105 C104 Ir1 111.5(3) . . ? C104 C105 C106 111.9(4) . . ? C107 C106 C105 114.6(4) . . ? C108 C107 C106 124.1(4) . . ? C108 C107 Ir1 71.7(2) . . ? C106 C107 Ir1 110.7(3) . . ? C107 C108 C101 122.5(4) . . ? C107 C108 Ir1 69.3(2) . . ? C101 C108 Ir1 114.9(3) . . ? C202 C203 C201 120.2(6) . 2_455 ? C203 C201 C202 120.1(6) 2_455 . ? C203 C202 C201 119.7(6) . . ? _refine_diff_density_max 1.336 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.122 data_5b _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C98 H120 Cl12 O8 P2 Pt2' _chemical_formula_weight 2303.46 _chemical_melting_point ? _chemical_compound_source ? 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6605(14) _cell_length_b 13.821(2) _cell_length_c 14.660(2) _cell_angle_alpha 104.270(11) _cell_angle_beta 101.943(12) _cell_angle_gamma 104.796(8) _cell_volume 2483.4(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1162 _exptl_absorpt_coefficient_mu 3.222 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15724 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.1600 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10877 _reflns_number_observed 6301 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SMART (Siemens, 1995b)' _computing_data_reduction 'SMART (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 on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0334P)^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_number_reflns 10877 _refine_ls_number_parameters 546 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_obs 0.0476 _refine_ls_wR_factor_all 0.1096 _refine_ls_wR_factor_obs 0.1037 _refine_ls_goodness_of_fit_all 0.789 _refine_ls_goodness_of_fit_obs 0.996 _refine_ls_restrained_S_all 0.791 _refine_ls_restrained_S_obs 0.999 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.43657(2) 0.36325(2) 0.44954(2) 0.03475(10) Uani 1 d . . Cl1 Cl 0.4462(2) 0.23186(14) 0.51523(12) 0.0472(5) Uani 1 d . . Cl2 Cl 0.4429(2) 0.51152(15) 0.39980(13) 0.0620(7) Uani 1 d . . P1 P 0.34139(13) 0.25574(14) 0.30514(12) 0.0282(4) Uani 1 d . . O1 O 0.0392(4) 0.1879(3) 0.2216(3) 0.0372(12) Uani 1 d . . H1 H 0.0452(50) 0.1280(17) 0.2168(14) 0.056 Uiso 1 calc R . O2 O 0.2493(3) 0.1494(3) 0.2870(3) 0.0297(10) Uani 1 d . . O3 O 0.4185(3) 0.2183(3) 0.2479(3) 0.0350(11) Uani 1 d . . O4 O 0.2871(3) 0.3181(3) 0.2465(3) 0.0331(11) Uani 1 d . . C1 C 0.0905(5) 0.2549(5) 0.3178(4) 0.031(2) Uani 1 d . . C2 C 0.1056(5) 0.2125(5) 0.3946(5) 0.029(2) Uani 1 d . . C3 C 0.1508(5) 0.2839(5) 0.4896(4) 0.033(2) Uani 1 d . . H3A H 0.1622(5) 0.2570(5) 0.5432(4) 0.040 Uiso 1 calc R . C4 C 0.1795(6) 0.3924(5) 0.5093(5) 0.037(2) Uani 1 d . . C5 C 0.1691(6) 0.4278(5) 0.4278(4) 0.036(2) Uani 1 d . . H5A H 0.1934(6) 0.5017(5) 0.4388(4) 0.044 Uiso 1 calc R . C6 C 0.1256(5) 0.3621(5) 0.3326(4) 0.031(2) Uani 1 d . . C7 C 0.2188(7) 0.4691(6) 0.6158(5) 0.048(2) Uani 1 d . . C8 C 0.2805(9) 0.4252(7) 0.6867(5) 0.098(4) Uani 1 d . . H8A H 0.2354(9) 0.3562(7) 0.6838(5) 0.148 Uiso 1 calc R . H8B H 0.3020(9) 0.4739(7) 0.7539(5) 0.148 Uiso 1 calc R . H8C H 0.3435(9) 0.4176(7) 0.6676(5) 0.148 Uiso 1 calc R . C9 C 0.1229(8) 0.4824(8) 0.6457(6) 0.099(4) Uani 1 d . . H9A H 0.0762(8) 0.4136(8) 0.6413(6) 0.148 Uiso 1 calc R . H9B H 0.0851(8) 0.5126(8) 0.6017(6) 0.148 Uiso 1 calc R . H9C H 0.1450(8) 0.5298(8) 0.7134(6) 0.148 Uiso 1 calc R . C10 C 0.2902(8) 0.5743(6) 0.6224(5) 0.075(3) Uani 1 d . . H10A H 0.3527(8) 0.5655(6) 0.6029(5) 0.113 Uiso 1 calc R . H10B H 0.3123(8) 0.6216(6) 0.6902(5) 0.113 Uiso 1 calc R . H10C H 0.2524(8) 0.6044(6) 0.5785(5) 0.113 Uiso 1 calc R . C11 C 0.0778(5) 0.0956(5) 0.3765(5) 0.033(2) Uani 1 d . . H11A H 0.0237(5) 0.0600(5) 0.3119(5) 0.039 Uiso 1 calc R . H11B H 0.0440(5) 0.0790(5) 0.4268(5) 0.039 Uiso 1 calc R . C12 C 0.2440(5) 0.0671(5) 0.3321(4) 0.0275(15) Uani 1 d . . C13 C 0.3139(5) 0.0083(5) 0.3263(4) 0.029(2) Uani 1 d . . C14 C 0.3051(5) -0.0678(5) 0.3731(4) 0.034(2) Uani 1 d . . H14A H 0.3526(5) -0.1074(5) 0.3709(4) 0.040 Uiso 1 calc R . C15 C 0.2297(5) -0.0896(5) 0.4236(4) 0.030(2) Uani 1 d . . C16 C 0.1607(5) -0.0319(5) 0.4225(4) 0.030(2) Uani 1 d . . H16A H 0.1075(5) -0.0463(5) 0.4546(4) 0.036 Uiso 1 calc R . C17 C 0.1643(5) 0.0464(5) 0.3771(4) 0.0264(15) Uani 1 d . . C18 C 0.2278(5) -0.1730(5) 0.4760(5) 0.037(2) Uani 1 d . . C19 C 0.1334(6) -0.1927(6) 0.5183(5) 0.055(2) Uani 1 d . . H19A H 0.0674(6) -0.2174(6) 0.4649(5) 0.083 Uiso 1 calc R . H19B H 0.1377(6) -0.1269(6) 0.5659(5) 0.083 Uiso 1 calc R . H19C H 0.1350(6) -0.2463(6) 0.5511(5) 0.083 Uiso 1 calc R . C20 C 0.2244(7) -0.2769(6) 0.4045(5) 0.061(3) Uani 1 d . . H20A H 0.1599(7) -0.3031(6) 0.3492(5) 0.092 Uiso 1 calc R . H20B H 0.2249(7) -0.3293(6) 0.4388(5) 0.092 Uiso 1 calc R . H20C H 0.2864(7) -0.2644(6) 0.3797(5) 0.092 Uiso 1 calc R . C21 C 0.3284(6) -0.1350(6) 0.5602(5) 0.052(2) Uani 1 d . . H21A H 0.3278(6) -0.1879(6) 0.5941(5) 0.078 Uiso 1 calc R . H21B H 0.3327(6) -0.0683(6) 0.6065(5) 0.078 Uiso 1 calc R . H21C H 0.3897(6) -0.1241(6) 0.5345(5) 0.078 Uiso 1 calc R . C22 C 0.4021(5) 0.0242(6) 0.2775(5) 0.038(2) Uani 1 d . . H22A H 0.4592(5) 0.0904(6) 0.3190(5) 0.046 Uiso 1 calc R . H22B H 0.4316(5) -0.0344(6) 0.2759(5) 0.046 Uiso 1 calc R . C23 C 0.3776(5) 0.1286(6) 0.1617(5) 0.037(2) Uani 1 d . . C24 C 0.3511(5) 0.1439(6) 0.0714(5) 0.038(2) Uani 1 d . . C25 C 0.3203(5) 0.0542(6) -0.0107(5) 0.044(2) Uani 1 d . . H25A H 0.3015(5) 0.0617(6) -0.0741(5) 0.052 Uiso 1 calc R . C26 C 0.3160(6) -0.0445(6) -0.0044(5) 0.045(2) Uani 1 d . . C27 C 0.3404(5) -0.0550(6) 0.0900(5) 0.041(2) Uani 1 d . . H27A H 0.3358(5) -0.1228(6) 0.0959(5) 0.049 Uiso 1 calc R . C28 C 0.3708(5) 0.0297(6) 0.1739(5) 0.034(2) Uani 1 d . . C29 C 0.2874(7) -0.1419(7) -0.0949(5) 0.055(2) Uani 1 d . . C30 C 0.2524(9) -0.1182(8) -0.1903(6) 0.109(4) Uani 1 d . . H30A H 0.3093(9) -0.0611(8) -0.1945(6) 0.163 Uiso 1 calc R . H30B H 0.1892(9) -0.0966(8) -0.1916(6) 0.163 Uiso 1 calc R . H30C H 0.2360(9) -0.1816(8) -0.2463(6) 0.163 Uiso 1 calc R . C31 C 0.3861(7) -0.1735(8) -0.0944(7) 0.108(4) Uani 1 d . . H31A H 0.4435(7) -0.1137(8) -0.0939(7) 0.162 Uiso 1 calc R . H31B H 0.3715(7) -0.2332(8) -0.1532(7) 0.162 Uiso 1 calc R . H31C H 0.4071(7) -0.1938(8) -0.0356(7) 0.162 Uiso 1 calc R . C32 C 0.1956(7) -0.2294(7) -0.0957(6) 0.075(3) Uani 1 d . . H32A H 0.1342(7) -0.2050(7) -0.0960(6) 0.112 Uiso 1 calc R . H32B H 0.2141(7) -0.2504(7) -0.0369(6) 0.112 Uiso 1 calc R . H32C H 0.1785(7) -0.2899(7) -0.1546(6) 0.112 Uiso 1 calc R . C33 C 0.3543(5) 0.2525(6) 0.0658(5) 0.041(2) Uani 1 d . . H33A H 0.4125(5) 0.3058(6) 0.1218(5) 0.050 Uiso 1 calc R . H33B H 0.3710(5) 0.2592(6) 0.0046(5) 0.050 Uiso 1 calc R . C34 C 0.2236(5) 0.3107(5) 0.1540(4) 0.030(2) Uani 1 d . . C35 C 0.1402(5) 0.3501(5) 0.1549(4) 0.033(2) Uani 1 d . . C36 C 0.0784(5) 0.3457(5) 0.0652(5) 0.039(2) Uani 1 d . . H36A H 0.0193(5) 0.3702(5) 0.0642(5) 0.047 Uiso 1 calc R . C37 C 0.0991(6) 0.3067(5) -0.0243(5) 0.038(2) Uani 1 d . . C38 C 0.1864(6) 0.2764(5) -0.0200(4) 0.040(2) Uani 1 d . . H38A H 0.2036(6) 0.2533(5) -0.0795(4) 0.048 Uiso 1 calc R . C39 C 0.2530(5) 0.2773(5) 0.0676(5) 0.036(2) Uani 1 d . . C40 C 0.0288(7) 0.3079(7) -0.1199(5) 0.054(2) Uani 1 d . . C41 C -0.0875(8) 0.2617(12) -0.1263(7) 0.167(7) Uani 1 d . . H41A H -0.1020(8) 0.1891(12) -0.1245(7) 0.251 Uiso 1 calc R . H41B H -0.1320(8) 0.2620(12) -0.1879(7) 0.251 Uiso 1 calc R . H41C H -0.1033(8) 0.3044(12) -0.0706(7) 0.251 Uiso 1 calc R . C42 C 0.0511(8) 0.2432(7) -0.2089(5) 0.083(3) Uani 1 d . . H42A H 0.0363(8) 0.1700(7) -0.2091(5) 0.124 Uiso 1 calc R . H42B H 0.1255(8) 0.2727(7) -0.2057(5) 0.124 Uiso 1 calc R . H42C H 0.0060(8) 0.2455(7) -0.2692(5) 0.124 Uiso 1 calc R . C43 C 0.0524(9) 0.4184(7) -0.1225(6) 0.103(4) Uani 1 d . . H43A H 0.0387(9) 0.4620(7) -0.0659(6) 0.154 Uiso 1 calc R . H43B H 0.0072(9) 0.4194(7) -0.1834(6) 0.154 Uiso 1 calc R . H43C H 0.1268(9) 0.4466(7) -0.1199(6) 0.154 Uiso 1 calc R . C44 C 0.1194(6) 0.4064(5) 0.2475(4) 0.039(2) Uani 1 d . . H44A H 0.0478(6) 0.4122(5) 0.2284(4) 0.047 Uiso 1 calc R . H44B H 0.1700(6) 0.4791(5) 0.2728(4) 0.047 Uiso 1 calc R . C45 C -0.4272(21) 0.4317(14) -0.1679(15) 0.265(17) Uani 1 d . . H45A H -0.4093(21) 0.5011(14) -0.1790(15) 0.319 Uiso 1 calc R . H45B H -0.4949(21) 0.3817(14) -0.2145(15) 0.319 Uiso 1 calc R . Cl3 Cl -0.4097(18) 0.4369(10) -0.0420(13) 0.756(18) Uani 1 d . . Cl4 Cl -0.3135(9) 0.3750(9) -0.1493(9) 0.440(7) Uani 1 d . . C46 C 0.6657(12) -0.1652(13) 0.3123(15) 0.207(9) Uani 1 d . . H46A H 0.6581(12) -0.1269(13) 0.3757(15) 0.248 Uiso 1 calc R . H46B H 0.6532(12) -0.2398(13) 0.3092(15) 0.248 Uiso 1 calc R . Cl5 Cl 0.7940(3) -0.1114(3) 0.3082(3) 0.1397(13) Uani 1 d . . Cl6 Cl 0.5704(3) -0.1587(3) 0.2163(3) 0.167(2) Uani 1 d . . C47 C -0.0761(9) 0.0201(10) -0.0750(9) 0.084(4) Uani 1 d D . C48 C 0.0379(14) 0.0198(9) -0.0807(14) 0.249(13) Uani 1 d D . C49 C 0.0737(25) -0.0015(26) 0.0304(21) 0.280(19) Uiso 1 d D . 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 0.0337(2) 0.0371(2) 0.02251(13) 0.01109(11) 0.00018(11) -0.00212(12) Cl1 0.0596(13) 0.0424(12) 0.0318(9) 0.0147(8) 0.0014(9) 0.0101(10) Cl2 0.077(2) 0.0420(12) 0.0334(10) 0.0175(9) -0.0198(10) -0.0133(11) P1 0.0208(9) 0.0352(11) 0.0233(8) 0.0097(8) 0.0042(8) 0.0016(8) O1 0.043(3) 0.029(3) 0.029(2) 0.000(2) 0.003(2) 0.009(2) O2 0.023(2) 0.032(3) 0.026(2) 0.006(2) 0.002(2) 0.001(2) O3 0.024(2) 0.045(3) 0.029(2) 0.004(2) 0.011(2) 0.004(2) O4 0.035(3) 0.035(3) 0.021(2) 0.008(2) 0.003(2) 0.002(2) C1 0.033(4) 0.029(4) 0.028(3) 0.007(3) 0.009(3) 0.009(3) C2 0.028(4) 0.028(4) 0.035(4) 0.012(3) 0.014(3) 0.009(3) C3 0.044(4) 0.039(5) 0.028(3) 0.019(3) 0.018(3) 0.020(4) C4 0.052(5) 0.034(4) 0.028(4) 0.012(3) 0.016(4) 0.012(4) C5 0.058(5) 0.022(4) 0.028(3) 0.008(3) 0.014(4) 0.011(4) C6 0.039(4) 0.030(4) 0.024(3) 0.008(3) 0.011(3) 0.011(3) C7 0.075(6) 0.036(5) 0.027(4) 0.007(3) 0.021(4) 0.007(4) C8 0.181(12) 0.064(7) 0.028(4) 0.011(5) 0.011(6) 0.023(7) C9 0.117(9) 0.097(8) 0.047(5) -0.030(5) 0.039(6) 0.014(7) C10 0.119(8) 0.054(6) 0.026(4) -0.004(4) 0.017(5) 0.002(6) C11 0.028(4) 0.030(4) 0.042(4) 0.015(3) 0.015(3) 0.006(3) C12 0.031(4) 0.025(4) 0.022(3) 0.010(3) 0.001(3) 0.006(3) C13 0.027(4) 0.034(4) 0.022(3) 0.007(3) 0.001(3) 0.011(3) C14 0.028(4) 0.047(5) 0.024(3) 0.006(3) 0.001(3) 0.019(3) C15 0.030(4) 0.028(4) 0.022(3) 0.004(3) -0.003(3) 0.003(3) C16 0.028(4) 0.034(4) 0.023(3) 0.008(3) 0.007(3) 0.004(3) C17 0.022(3) 0.024(4) 0.025(3) 0.005(3) 0.002(3) 0.001(3) C18 0.038(4) 0.037(4) 0.029(4) 0.008(3) 0.000(3) 0.013(4) C19 0.056(5) 0.069(6) 0.058(5) 0.046(5) 0.020(4) 0.021(5) C20 0.104(7) 0.039(5) 0.042(4) 0.017(4) 0.009(5) 0.030(5) C21 0.053(5) 0.072(6) 0.036(4) 0.027(4) 0.009(4) 0.021(5) C22 0.033(4) 0.049(5) 0.037(4) 0.016(4) 0.014(3) 0.017(4) C23 0.026(4) 0.054(5) 0.030(4) 0.010(3) 0.014(3) 0.008(4) C24 0.028(4) 0.061(5) 0.029(4) 0.016(4) 0.014(3) 0.015(4) C25 0.036(4) 0.069(6) 0.027(4) 0.013(4) 0.014(3) 0.015(4) C26 0.039(4) 0.059(6) 0.034(4) 0.005(4) 0.020(4) 0.013(4) C27 0.039(4) 0.054(5) 0.037(4) 0.013(4) 0.020(4) 0.021(4) C28 0.025(4) 0.050(5) 0.031(4) 0.013(3) 0.013(3) 0.016(3) C29 0.059(6) 0.064(6) 0.035(4) 0.002(4) 0.019(4) 0.017(5) C30 0.173(12) 0.096(8) 0.036(5) 0.005(5) 0.035(7) 0.019(8) C31 0.058(7) 0.117(9) 0.091(7) -0.055(7) 0.026(6) 0.012(6) C32 0.065(6) 0.074(7) 0.057(5) -0.013(5) 0.018(5) 0.006(5) C33 0.040(4) 0.057(5) 0.028(4) 0.018(4) 0.012(3) 0.010(4) C34 0.033(4) 0.023(4) 0.021(3) 0.008(3) -0.003(3) -0.002(3) C35 0.039(4) 0.029(4) 0.022(3) 0.010(3) 0.001(3) 0.003(3) C36 0.041(4) 0.043(5) 0.030(4) 0.017(3) 0.002(3) 0.010(4) C37 0.040(4) 0.040(5) 0.028(4) 0.015(3) 0.002(3) 0.005(4) C38 0.052(5) 0.044(5) 0.021(3) 0.014(3) 0.013(3) 0.005(4) C39 0.031(4) 0.043(5) 0.028(3) 0.016(3) 0.007(3) -0.002(3) C40 0.066(6) 0.070(6) 0.025(4) 0.018(4) 0.002(4) 0.022(5) C41 0.067(8) 0.359(22) 0.071(7) 0.111(11) -0.001(7) 0.036(11) C42 0.130(9) 0.087(7) 0.028(4) 0.009(5) 0.000(5) 0.055(7) C43 0.201(12) 0.095(8) 0.037(5) 0.036(5) 0.020(7) 0.086(8) C44 0.056(5) 0.040(4) 0.026(3) 0.014(3) 0.011(4) 0.021(4) C45 0.298(27) 0.132(15) 0.223(21) 0.120(16) -0.132(21) -0.064(17) Cl3 1.082(39) 0.323(14) 0.717(26) -0.010(16) 0.626(29) -0.141(18) Cl4 0.405(14) 0.399(14) 0.390(14) 0.106(11) 0.102(12) -0.053(11) C46 0.181(15) 0.238(18) 0.400(27) 0.250(20) 0.213(18) 0.151(14) Cl5 0.177(4) 0.119(3) 0.136(3) 0.030(2) 0.085(3) 0.048(3) Cl6 0.145(4) 0.162(4) 0.189(4) 0.035(3) 0.078(3) 0.040(3) C47 0.054(7) 0.081(8) 0.068(7) -0.036(6) -0.024(6) 0.031(6) C48 0.228(21) 0.036(8) 0.311(24) 0.028(11) -0.152(19) -0.030(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 Pt1 P1 2.169(2) . ? Pt1 Cl1 2.275(2) . ? Pt1 Cl2 2.326(2) . ? Pt1 Cl2 2.396(2) 2_666 ? Cl2 Pt1 2.396(2) 2_666 ? P1 O4 1.569(4) . ? P1 O3 1.584(5) . ? P1 O2 1.593(4) . ? O1 C1 1.396(7) . ? O2 C12 1.444(7) . ? O3 C23 1.425(8) . ? O4 C34 1.413(6) . ? C1 C6 1.382(8) . ? C1 C2 1.395(8) . ? C2 C3 1.397(8) . ? C2 C11 1.502(8) . ? C3 C4 1.386(9) . ? C4 C5 1.393(8) . ? C4 C7 1.548(9) . ? C5 C6 1.372(8) . ? C6 C44 1.514(8) . ? C7 C10 1.498(10) . ? C7 C9 1.504(12) . ? C7 C8 1.539(11) . ? C11 C17 1.507(9) . ? C12 C17 1.391(8) . ? C12 C13 1.406(8) . ? C13 C14 1.384(8) . ? C13 C22 1.520(9) . ? C14 C15 1.402(9) . ? C15 C16 1.380(9) . ? C15 C18 1.533(8) . ? C16 C17 1.400(8) . ? C18 C21 1.516(8) . ? C18 C19 1.534(10) . ? C18 C20 1.539(9) . ? C22 C28 1.516(8) . ? C23 C24 1.381(8) . ? C23 C28 1.404(9) . ? C24 C25 1.396(9) . ? C24 C33 1.513(9) . ? C25 C26 1.378(10) . ? C26 C27 1.406(9) . ? C26 C29 1.537(10) . ? C27 C28 1.374(9) . ? C29 C32 1.499(10) . ? C29 C31 1.519(11) . ? C29 C30 1.525(10) . ? C33 C39 1.512(9) . ? C34 C35 1.384(9) . ? C34 C39 1.412(9) . ? C35 C36 1.385(8) . ? C35 C44 1.511(9) . ? C36 C37 1.405(9) . ? C37 C38 1.356(10) . ? C37 C40 1.533(9) . ? C38 C39 1.408(8) . ? C40 C43 1.490(11) . ? C40 C42 1.525(11) . ? C40 C41 1.527(12) . ? C45 Cl3 1.79(2) . ? C45 Cl4 1.91(3) . ? Cl3 Cl4 2.39(2) . ? C46 Cl5 1.740(13) . ? C46 Cl6 1.74(2) . ? C47 C49 0.76(3) 2 ? C47 C48 1.58(2) . ? C48 C49 1.72(2) . ? C48 C49 1.81(4) 2 ? C49 C47 0.76(3) 2 ? C49 C48 1.81(4) 2 ? 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 P1 Pt1 Cl1 93.98(7) . . ? P1 Pt1 Cl2 92.92(6) . . ? Cl1 Pt1 Cl2 172.94(6) . . ? P1 Pt1 Cl2 173.39(7) . 2_666 ? Cl1 Pt1 Cl2 89.00(6) . 2_666 ? Cl2 Pt1 Cl2 83.99(6) . 2_666 ? Pt1 Cl2 Pt1 96.01(6) . 2_666 ? O4 P1 O3 106.6(2) . . ? O4 P1 O2 104.5(2) . . ? O3 P1 O2 104.0(2) . . ? O4 P1 Pt1 108.6(2) . . ? O3 P1 Pt1 108.0(2) . . ? O2 P1 Pt1 124.0(2) . . ? C12 O2 P1 131.6(3) . . ? C23 O3 P1 120.2(4) . . ? C34 O4 P1 144.0(4) . . ? C6 C1 C2 122.4(6) . . ? C6 C1 O1 117.8(5) . . ? C2 C1 O1 119.8(6) . . ? C1 C2 C3 116.9(6) . . ? C1 C2 C11 122.0(6) . . ? C3 C2 C11 121.1(6) . . ? C4 C3 C2 123.0(6) . . ? C3 C4 C5 116.1(6) . . ? C3 C4 C7 121.7(6) . . ? C5 C4 C7 122.2(6) . . ? C6 C5 C4 123.8(6) . . ? C5 C6 C1 117.4(6) . . ? C5 C6 C44 120.7(6) . . ? C1 C6 C44 121.8(6) . . ? C10 C7 C9 109.5(7) . . ? C10 C7 C8 107.8(7) . . ? C9 C7 C8 109.7(7) . . ? C10 C7 C4 111.3(6) . . ? C9 C7 C4 107.4(6) . . ? C8 C7 C4 111.2(6) . . ? C2 C11 C17 118.9(5) . . ? C17 C12 C13 122.2(6) . . ? C17 C12 O2 116.9(6) . . ? C13 C12 O2 120.8(6) . . ? C14 C13 C12 117.3(6) . . ? C14 C13 C22 116.8(6) . . ? C12 C13 C22 125.8(6) . . ? C13 C14 C15 123.4(6) . . ? C16 C15 C14 116.1(6) . . ? C16 C15 C18 124.0(6) . . ? C14 C15 C18 119.9(6) . . ? C15 C16 C17 124.0(6) . . ? C12 C17 C16 116.9(6) . . ? C12 C17 C11 126.2(5) . . ? C16 C17 C11 116.8(6) . . ? C21 C18 C15 109.0(5) . . ? C21 C18 C19 108.1(5) . . ? C15 C18 C19 111.9(6) . . ? C21 C18 C20 107.9(6) . . ? C15 C18 C20 109.9(5) . . ? C19 C18 C20 109.8(6) . . ? C28 C22 C13 115.7(5) . . ? C24 C23 C28 123.9(7) . . ? C24 C23 O3 118.6(6) . . ? C28 C23 O3 117.4(6) . . ? C23 C24 C25 116.0(7) . . ? C23 C24 C33 120.0(7) . . ? C25 C24 C33 124.0(6) . . ? C26 C25 C24 123.2(7) . . ? C25 C26 C27 117.7(7) . . ? C25 C26 C29 123.1(7) . . ? C27 C26 C29 119.2(7) . . ? C28 C27 C26 122.2(7) . . ? C27 C28 C23 116.9(6) . . ? C27 C28 C22 124.6(7) . . ? C23 C28 C22 118.4(6) . . ? C32 C29 C31 112.8(8) . . ? C32 C29 C30 105.3(7) . . ? C31 C29 C30 108.3(8) . . ? C32 C29 C26 111.3(7) . . ? C31 C29 C26 107.5(6) . . ? C30 C29 C26 111.8(7) . . ? C39 C33 C24 114.6(6) . . ? C35 C34 C39 122.2(6) . . ? C35 C34 O4 116.4(6) . . ? C39 C34 O4 120.9(6) . . ? C34 C35 C36 117.4(6) . . ? C34 C35 C44 123.9(6) . . ? C36 C35 C44 118.5(6) . . ? C35 C36 C37 123.0(7) . . ? C38 C37 C36 117.1(6) . . ? C38 C37 C40 123.1(7) . . ? C36 C37 C40 119.6(7) . . ? C37 C38 C39 123.6(7) . . ? C38 C39 C34 116.3(7) . . ? C38 C39 C33 119.3(6) . . ? C34 C39 C33 124.2(6) . . ? C43 C40 C42 107.7(7) . . ? C43 C40 C41 110.3(9) . . ? C42 C40 C41 108.9(8) . . ? C43 C40 C37 109.3(6) . . ? C42 C40 C37 110.7(7) . . ? C41 C40 C37 110.0(7) . . ? C35 C44 C6 120.1(6) . . ? Cl3 C45 Cl4 80.2(11) . . ? C45 Cl3 Cl4 52.1(10) . . ? C45 Cl4 Cl3 47.7(8) . . ? Cl5 C46 Cl6 112.7(8) . . ? C49 C47 C48 95.5(28) 2 . ? C47 C48 C49 94.7(18) . . ? C47 C48 C49 24.5(10) . 2 ? C49 C48 C49 70.5(21) . 2 ? C47 C49 C48 166.3(42) 2 . ? C47 C49 C48 59.9(26) 2 2 ? C48 C49 C48 109.5(21) . 2 ? _refine_diff_density_max 1.488 _refine_diff_density_min -1.727 _refine_diff_density_rms 0.140