Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'David Milstein' _publ_contact_author_address ; Department of Organic Chemistry The Weizmann Institute of Science Rehovot 76100 76100 ISRAEL ; _publ_contact_author_email DAVID.MILSTEIN@WEIZMANN.AC.IL _publ_section_title ; Reactivity and Stability of Platinum(II) Formyl Complexes Based on PCP-Type Ligands. The Significance of Sterics ; loop_ _publ_author_name 'David Milstein' 'Yael Diskin-Posner' 'Gregory Leitus' 'Elena Poverenov' 'Linda Shimon' ; D.Vuzman ; # Attachment 'compound6_new.cif' data_m716a _database_code_depnum_ccdc_archive 'CCDC 653982' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H43 Cl P2 Pt' _chemical_formula_sum 'C24 H43 Cl P2 Pt' _chemical_formula_weight 624.06 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.965(3) _cell_length_b 13.853(3) _cell_length_c 14.642(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2629.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3801 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 30.51 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 5.567 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2142 _exptl_absorpt_correction_T_max 0.2859 _exptl_absorpt_process_details 'SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14714 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 30.49 _reflns_number_total 4426 _reflns_number_gt 3623 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect Package (Bruker Nonius)' _computing_cell_refinement HKL _computing_data_reduction HKL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^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 riding _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 0.508(12) _refine_ls_number_reflns 4426 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 1.886159(17) 0.502233(14) 0.186436(13) 0.01233(7) Uani 1 1 d . . . P2 P 1.71061(12) 0.49536(13) 0.16969(9) 0.0124(3) Uani 1 1 d . . . P3 P 2.06132(13) 0.48641(11) 0.17625(10) 0.0128(3) Uani 1 1 d . . . Cl1 Cl 1.88822(15) 0.62547(12) 0.30227(12) 0.0273(4) Uani 1 1 d . . . C11 C 1.8851(6) 0.3975(4) 0.0907(4) 0.0156(12) Uani 1 1 d . . . C12 C 1.7929(5) 0.3722(4) 0.0440(4) 0.0137(12) Uani 1 1 d . . . C13 C 1.7914(7) 0.2965(4) -0.0187(4) 0.0216(16) Uani 1 1 d . . . H13 H 1.7294 0.2807 -0.0499 0.026 Uiso 1 1 calc R . . C14 C 1.8813(7) 0.2443(5) -0.0353(5) 0.0265(17) Uani 1 1 d . . . H14 H 1.8796 0.1911 -0.0763 0.032 Uiso 1 1 calc R . . C15 C 1.9724(6) 0.2686(5) 0.0067(5) 0.0253(17) Uani 1 1 d . . . H15 H 2.0337 0.2342 -0.0078 0.030 Uiso 1 1 calc R . . C16 C 1.9759(5) 0.3447(4) 0.0714(4) 0.0159(13) Uani 1 1 d . . . C31 C 2.0756(6) 0.3686(5) 0.1198(5) 0.0207(15) Uani 1 1 d . . . H31A H 2.1330 0.3710 0.0753 0.025 Uiso 1 1 calc R . . H31B H 2.0915 0.3182 0.1657 0.025 Uiso 1 1 calc R . . C21 C 1.6980(6) 0.4325(5) 0.0590(5) 0.0190(14) Uani 1 1 d . . . H21A H 1.6359 0.3908 0.0595 0.023 Uiso 1 1 calc R . . H21B H 1.6905 0.4802 0.0091 0.023 Uiso 1 1 calc R . . C22 C 1.6463(6) 0.4169(5) 0.2564(4) 0.0173(14) Uani 1 1 d . . . C23 C 1.6405(6) 0.6117(4) 0.1517(5) 0.0202(15) Uani 1 1 d . . . C24 C 1.6877(8) 0.3125(5) 0.2409(6) 0.035(2) Uani 1 1 d . . . H24A H 1.6628 0.2703 0.2899 0.053 Uiso 1 1 calc R . . H24B H 1.7632 0.3133 0.2411 0.053 Uiso 1 1 calc R . . H24C H 1.6630 0.2883 0.1819 0.053 Uiso 1 1 calc R . . C25 C 1.6834(7) 0.4477(5) 0.3523(5) 0.0257(17) Uani 1 1 d . . . H25A H 1.6614 0.5142 0.3644 0.039 Uiso 1 1 calc R . . H25B H 1.7588 0.4439 0.3551 0.039 Uiso 1 1 calc R . . H25C H 1.6535 0.4046 0.3983 0.039 Uiso 1 1 calc R . . C26 C 1.5298(6) 0.4152(6) 0.2513(6) 0.0287(18) Uani 1 1 d . . . H26A H 1.5083 0.3902 0.1917 0.043 Uiso 1 1 calc R . . H26B H 1.5031 0.4809 0.2592 0.043 Uiso 1 1 calc R . . H26C H 1.5026 0.3736 0.2997 0.043 Uiso 1 1 calc R . . C27 C 1.5383(7) 0.5989(6) 0.1001(6) 0.036(2) Uani 1 1 d . . . H27A H 1.4925 0.5567 0.1353 0.054 Uiso 1 1 calc R . . H27B H 1.5518 0.5698 0.0402 0.054 Uiso 1 1 calc R . . H27C H 1.5054 0.6620 0.0918 0.054 Uiso 1 1 calc R . . C28 C 1.7156(7) 0.6755(5) 0.0954(5) 0.0277(18) Uani 1 1 d . . . H28A H 1.6856 0.7399 0.0872 0.042 Uiso 1 1 calc R . . H28B H 1.7273 0.6459 0.0355 0.042 Uiso 1 1 calc R . . H28C H 1.7814 0.6811 0.1279 0.042 Uiso 1 1 calc R . . C29 C 1.6217(7) 0.6612(5) 0.2439(5) 0.0303(18) Uani 1 1 d . . . H29A H 1.5958 0.7268 0.2336 0.045 Uiso 1 1 calc R . . H29B H 1.6866 0.6642 0.2782 0.045 Uiso 1 1 calc R . . H29C H 1.5707 0.6243 0.2788 0.045 Uiso 1 1 calc R . . C32 C 2.1391(6) 0.4734(5) 0.2845(5) 0.0208(15) Uani 1 1 d . . . C33 C 2.1186(6) 0.5767(5) 0.0969(5) 0.0187(14) Uani 1 1 d . . . C34 C 2.2410(6) 0.4187(5) 0.2697(6) 0.0264(17) Uani 1 1 d . . . H34A H 2.2854 0.4557 0.2284 0.040 Uiso 1 1 calc R . . H34B H 2.2265 0.3553 0.2429 0.040 Uiso 1 1 calc R . . H34C H 2.2760 0.4103 0.3285 0.040 Uiso 1 1 calc R . . C35 C 2.0699(7) 0.4128(6) 0.3481(5) 0.034(2) Uani 1 1 d . . . H35A H 2.1079 0.3972 0.4041 0.052 Uiso 1 1 calc R . . H35B H 2.0500 0.3530 0.3171 0.052 Uiso 1 1 calc R . . H35C H 2.0080 0.4498 0.3637 0.052 Uiso 1 1 calc R . . C36 C 2.1596(7) 0.5719(5) 0.3300(5) 0.0268(16) Uani 1 1 d . . . H36A H 2.0941 0.6056 0.3395 0.040 Uiso 1 1 calc R . . H36B H 2.2042 0.6108 0.2904 0.040 Uiso 1 1 calc R . . H36C H 2.1937 0.5619 0.3890 0.040 Uiso 1 1 calc R . . C37 C 2.0684(7) 0.5569(5) 0.0023(5) 0.0282(17) Uani 1 1 d . . . H37A H 2.0884 0.6078 -0.0406 0.042 Uiso 1 1 calc R . . H37B H 1.9931 0.5561 0.0087 0.042 Uiso 1 1 calc R . . H37C H 2.0919 0.4943 -0.0207 0.042 Uiso 1 1 calc R . . C38 C 2.0844(7) 0.6768(5) 0.1264(5) 0.0257(17) Uani 1 1 d . . . H38A H 2.1078 0.6889 0.1890 0.039 Uiso 1 1 calc R . . H38B H 2.0090 0.6809 0.1239 0.039 Uiso 1 1 calc R . . H38C H 2.1145 0.7251 0.0854 0.039 Uiso 1 1 calc R . . C39 C 2.2354(6) 0.5744(6) 0.0881(6) 0.0291(19) Uani 1 1 d . . . H39A H 2.2569 0.6166 0.0378 0.044 Uiso 1 1 calc R . . H39B H 2.2581 0.5082 0.0758 0.044 Uiso 1 1 calc R . . H39C H 2.2667 0.5971 0.1452 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01054(11) 0.01060(10) 0.01585(11) -0.00218(10) -0.00004(8) -0.00023(13) P2 0.0079(6) 0.0128(6) 0.0165(6) -0.0017(8) -0.0006(5) 0.0020(8) P3 0.0090(7) 0.0136(7) 0.0159(7) -0.0009(6) -0.0002(6) 0.0001(6) Cl1 0.0191(9) 0.0286(8) 0.0343(9) -0.0190(7) 0.0013(9) -0.0012(7) C11 0.013(3) 0.014(3) 0.019(3) 0.000(2) -0.003(3) 0.001(3) C12 0.013(3) 0.013(3) 0.015(3) -0.001(2) -0.001(3) -0.003(2) C13 0.029(4) 0.015(3) 0.021(3) -0.004(2) -0.003(3) -0.005(3) C14 0.034(5) 0.018(3) 0.027(4) -0.012(3) -0.006(4) 0.002(3) C15 0.025(4) 0.017(3) 0.034(4) -0.008(3) -0.002(4) 0.006(3) C16 0.015(3) 0.014(3) 0.019(3) 0.004(2) -0.001(3) -0.003(2) C31 0.017(4) 0.018(3) 0.027(4) -0.003(3) 0.002(3) 0.007(3) C21 0.016(4) 0.023(3) 0.018(3) -0.011(3) -0.003(3) 0.003(3) C22 0.016(4) 0.019(3) 0.017(3) 0.001(2) -0.002(3) -0.004(3) C23 0.016(4) 0.015(3) 0.029(4) 0.000(2) -0.002(3) 0.007(3) C24 0.039(6) 0.026(4) 0.042(5) 0.011(3) 0.003(4) -0.001(4) C25 0.022(4) 0.037(4) 0.019(3) 0.004(3) 0.003(3) -0.007(3) C26 0.019(4) 0.031(4) 0.036(4) -0.005(3) 0.006(4) -0.014(3) C27 0.017(4) 0.045(5) 0.046(5) -0.002(4) -0.011(4) 0.012(4) C28 0.033(5) 0.016(3) 0.034(4) 0.002(3) -0.006(4) 0.010(3) C29 0.030(5) 0.020(3) 0.041(4) -0.012(3) -0.001(4) 0.013(3) C32 0.018(4) 0.022(3) 0.023(3) 0.002(2) -0.003(3) -0.004(3) C33 0.014(3) 0.020(3) 0.023(3) 0.005(2) 0.001(3) 0.005(3) C34 0.014(4) 0.024(4) 0.041(4) 0.001(3) -0.014(3) 0.003(3) C35 0.020(4) 0.051(5) 0.032(4) 0.021(4) -0.002(4) -0.008(4) C36 0.028(4) 0.032(4) 0.020(3) -0.002(3) -0.003(4) -0.005(4) C37 0.032(5) 0.031(4) 0.021(3) 0.004(3) -0.005(4) -0.007(4) C38 0.023(4) 0.025(3) 0.030(4) 0.006(3) -0.001(3) -0.006(3) C39 0.019(4) 0.039(4) 0.029(4) 0.004(3) 0.016(3) 0.000(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 Pt1 C11 2.017(6) . ? Pt1 P3 2.2863(18) . ? Pt1 P2 2.2911(16) . ? Pt1 Cl1 2.4066(15) . ? P2 C21 1.847(6) . ? P2 C22 1.868(7) . ? P2 C23 1.869(6) . ? P3 C31 1.839(6) . ? P3 C33 1.862(7) . ? P3 C32 1.887(7) . ? C11 C16 1.415(9) . ? C11 C12 1.420(10) . ? C12 C13 1.394(8) . ? C12 C21 1.504(9) . ? C13 C14 1.394(11) . ? C13 H13 0.9500 . ? C14 C15 1.374(11) . ? C14 H14 0.9500 . ? C15 C16 1.418(9) . ? C15 H15 0.9500 . ? C16 C31 1.511(10) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C26 1.512(12) . ? C22 C25 1.544(9) . ? C22 C24 1.559(10) . ? C23 C29 1.534(9) . ? C23 C27 1.536(11) . ? C23 C28 1.553(11) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C32 C34 1.538(10) . ? C32 C36 1.542(9) . ? C32 C35 1.542(10) . ? C33 C38 1.518(9) . ? C33 C39 1.521(11) . ? C33 C37 1.554(10) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? 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 C11 Pt1 P3 83.8(2) . . ? C11 Pt1 P2 83.6(2) . . ? P3 Pt1 P2 167.35(5) . . ? C11 Pt1 Cl1 179.17(18) . . ? P3 Pt1 Cl1 95.91(6) . . ? P2 Pt1 Cl1 96.66(6) . . ? C21 P2 C22 106.4(3) . . ? C21 P2 C23 103.9(3) . . ? C22 P2 C23 112.4(3) . . ? C21 P2 Pt1 101.6(2) . . ? C22 P2 Pt1 113.3(2) . . ? C23 P2 Pt1 117.5(2) . . ? C31 P3 C33 106.0(3) . . ? C31 P3 C32 103.8(3) . . ? C33 P3 C32 112.0(3) . . ? C31 P3 Pt1 102.4(3) . . ? C33 P3 Pt1 111.9(2) . . ? C32 P3 Pt1 119.0(2) . . ? C16 C11 C12 118.4(5) . . ? C16 C11 Pt1 120.3(5) . . ? C12 C11 Pt1 121.2(5) . . ? C13 C12 C11 121.0(6) . . ? C13 C12 C21 120.1(6) . . ? C11 C12 C21 118.8(5) . . ? C14 C13 C12 119.6(7) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.9(5) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 120.6(7) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C11 C16 C15 119.5(6) . . ? C11 C16 C31 120.3(6) . . ? C15 C16 C31 120.2(6) . . ? C16 C31 P3 108.6(5) . . ? C16 C31 H31A 110.0 . . ? P3 C31 H31A 110.0 . . ? C16 C31 H31B 110.0 . . ? P3 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? C12 C21 P2 108.5(5) . . ? C12 C21 H21A 110.0 . . ? P2 C21 H21A 110.0 . . ? C12 C21 H21B 110.0 . . ? P2 C21 H21B 110.0 . . ? H21A C21 H21B 108.4 . . ? C26 C22 C25 111.1(6) . . ? C26 C22 C24 108.8(6) . . ? C25 C22 C24 106.4(6) . . ? C26 C22 P2 114.9(5) . . ? C25 C22 P2 108.6(4) . . ? C24 C22 P2 106.7(5) . . ? C29 C23 C27 110.4(7) . . ? C29 C23 C28 108.2(6) . . ? C27 C23 C28 110.2(6) . . ? C29 C23 P2 109.8(5) . . ? C27 C23 P2 112.9(5) . . ? C28 C23 P2 105.1(5) . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C23 C29 H29A 109.5 . . ? C23 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C23 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C34 C32 C36 110.4(6) . . ? C34 C32 C35 108.4(6) . . ? C36 C32 C35 108.7(7) . . ? C34 C32 P3 112.8(5) . . ? C36 C32 P3 111.8(5) . . ? C35 C32 P3 104.4(5) . . ? C38 C33 C39 109.5(7) . . ? C38 C33 C37 107.0(6) . . ? C39 C33 C37 109.8(7) . . ? C38 C33 P3 108.7(5) . . ? C39 C33 P3 115.8(5) . . ? C37 C33 P3 105.7(5) . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C36 H36A 109.5 . . ? C32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C37 H37A 109.5 . . ? C33 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C33 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C33 C39 H39A 109.5 . . ? C33 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C33 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? 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 C11 Pt1 P2 C21 -17.8(3) . . . . ? P3 Pt1 P2 C21 -10.3(4) . . . . ? Cl1 Pt1 P2 C21 163.0(2) . . . . ? C11 Pt1 P2 C22 95.9(3) . . . . ? P3 Pt1 P2 C22 103.4(3) . . . . ? Cl1 Pt1 P2 C22 -83.3(2) . . . . ? C11 Pt1 P2 C23 -130.3(3) . . . . ? P3 Pt1 P2 C23 -122.9(3) . . . . ? Cl1 Pt1 P2 C23 50.5(3) . . . . ? C11 Pt1 P3 C31 -17.4(3) . . . . ? P2 Pt1 P3 C31 -24.8(4) . . . . ? Cl1 Pt1 P3 C31 161.8(2) . . . . ? C11 Pt1 P3 C33 95.7(3) . . . . ? P2 Pt1 P3 C33 88.3(3) . . . . ? Cl1 Pt1 P3 C33 -85.0(2) . . . . ? C11 Pt1 P3 C32 -131.0(3) . . . . ? P2 Pt1 P3 C32 -138.5(3) . . . . ? Cl1 Pt1 P3 C32 48.2(2) . . . . ? P3 Pt1 C11 C16 13.3(5) . . . . ? P2 Pt1 C11 C16 -168.3(5) . . . . ? Cl1 Pt1 C11 C16 -59(16) . . . . ? P3 Pt1 C11 C12 -169.4(5) . . . . ? P2 Pt1 C11 C12 9.0(5) . . . . ? Cl1 Pt1 C11 C12 119(15) . . . . ? C16 C11 C12 C13 0.6(9) . . . . ? Pt1 C11 C12 C13 -176.7(4) . . . . ? C16 C11 C12 C21 -175.6(6) . . . . ? Pt1 C11 C12 C21 7.0(8) . . . . ? C11 C12 C13 C14 0.6(10) . . . . ? C21 C12 C13 C14 176.8(6) . . . . ? C12 C13 C14 C15 -2.5(11) . . . . ? C13 C14 C15 C16 3.1(11) . . . . ? C12 C11 C16 C15 0.0(9) . . . . ? Pt1 C11 C16 C15 177.3(5) . . . . ? C12 C11 C16 C31 -179.6(6) . . . . ? Pt1 C11 C16 C31 -2.2(8) . . . . ? C14 C15 C16 C11 -1.8(10) . . . . ? C14 C15 C16 C31 177.8(7) . . . . ? C11 C16 C31 P3 -14.0(8) . . . . ? C15 C16 C31 P3 166.5(5) . . . . ? C33 P3 C31 C16 -96.8(5) . . . . ? C32 P3 C31 C16 145.0(5) . . . . ? Pt1 P3 C31 C16 20.6(5) . . . . ? C13 C12 C21 P2 160.9(5) . . . . ? C11 C12 C21 P2 -22.8(8) . . . . ? C22 P2 C21 C12 -93.3(5) . . . . ? C23 P2 C21 C12 147.9(5) . . . . ? Pt1 P2 C21 C12 25.4(5) . . . . ? C21 P2 C22 C26 -72.8(6) . . . . ? C23 P2 C22 C26 40.3(6) . . . . ? Pt1 P2 C22 C26 176.4(4) . . . . ? C21 P2 C22 C25 162.2(5) . . . . ? C23 P2 C22 C25 -84.8(6) . . . . ? Pt1 P2 C22 C25 51.4(6) . . . . ? C21 P2 C22 C24 47.9(6) . . . . ? C23 P2 C22 C24 161.0(5) . . . . ? Pt1 P2 C22 C24 -62.9(5) . . . . ? C21 P2 C23 C29 166.4(5) . . . . ? C22 P2 C23 C29 51.8(6) . . . . ? Pt1 P2 C23 C29 -82.3(6) . . . . ? C21 P2 C23 C27 42.8(6) . . . . ? C22 P2 C23 C27 -71.8(6) . . . . ? Pt1 P2 C23 C27 154.1(5) . . . . ? C21 P2 C23 C28 -77.4(5) . . . . ? C22 P2 C23 C28 168.0(4) . . . . ? Pt1 P2 C23 C28 33.9(5) . . . . ? C31 P3 C32 C34 40.6(6) . . . . ? C33 P3 C32 C34 -73.4(5) . . . . ? Pt1 P3 C32 C34 153.5(4) . . . . ? C31 P3 C32 C36 165.7(5) . . . . ? C33 P3 C32 C36 51.7(6) . . . . ? Pt1 P3 C32 C36 -81.4(5) . . . . ? C31 P3 C32 C35 -77.0(6) . . . . ? C33 P3 C32 C35 169.1(5) . . . . ? Pt1 P3 C32 C35 35.9(6) . . . . ? C31 P3 C33 C38 165.0(5) . . . . ? C32 P3 C33 C38 -82.4(6) . . . . ? Pt1 P3 C33 C38 54.2(6) . . . . ? C31 P3 C33 C39 -71.3(7) . . . . ? C32 P3 C33 C39 41.3(7) . . . . ? Pt1 P3 C33 C39 177.9(5) . . . . ? C31 P3 C33 C37 50.4(6) . . . . ? C32 P3 C33 C37 163.0(5) . . . . ? Pt1 P3 C33 C37 -60.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.389 _refine_diff_density_min -1.839 _refine_diff_density_rms 0.204 data_m745a _database_code_depnum_ccdc_archive 'CCDC 653983' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H55 F3 O5 P2 Pt S' _chemical_formula_weight 853.84 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 15.8240(2) _cell_length_b 11.37500(10) _cell_length_c 20.0930(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.4580(8) _cell_angle_gamma 90.00 _cell_volume 3586.10(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8383 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 4.111 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5249 _exptl_absorpt_correction_T_max 0.6839 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Nonius Kappa CCD' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8214 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8214 _reflns_number_gt 6720 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect package Bruker - Nonius' _computing_cell_refinement HKL _computing_data_reduction HKL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.6481P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8214 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0678 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.747272(7) 0.207885(9) 0.236068(5) 0.01476(5) Uani 1 1 d . . . P2 P 0.76993(5) 0.32827(7) 0.32881(4) 0.01521(16) Uani 1 1 d . . . P3 P 0.74643(5) 0.12923(7) 0.13048(4) 0.01492(16) Uani 1 1 d . . . C4 C 0.8143(2) 0.2297(3) 0.09024(15) 0.0184(7) Uani 1 1 d . . . H4A H 0.8729 0.1977 0.0936 0.022 Uiso 1 1 calc R . . H4B H 0.7921 0.2383 0.0421 0.022 Uiso 1 1 calc R . . C5 C 0.81565(19) 0.3482(3) 0.12457(15) 0.0175(6) Uani 1 1 d . . . C6 C 0.84338(19) 0.4480(3) 0.09334(15) 0.0206(7) Uani 1 1 d . . . H6 H 0.8567 0.4431 0.0487 0.025 Uiso 1 1 calc R . . C7 C 0.8516(2) 0.5539(3) 0.12717(16) 0.0239(7) Uani 1 1 d . . . H7 H 0.8716 0.6212 0.1060 0.029 Uiso 1 1 calc R . . C8 C 0.8305(2) 0.5623(3) 0.19221(15) 0.0206(7) Uani 1 1 d . . . H8 H 0.8366 0.6350 0.2155 0.025 Uiso 1 1 calc R . . C9 C 0.80058(19) 0.4638(3) 0.22288(14) 0.0179(6) Uani 1 1 d . . . C10 C 0.7741(2) 0.4756(2) 0.29249(14) 0.0175(6) Uani 1 1 d . . . H10A H 0.7174 0.5135 0.2897 0.021 Uiso 1 1 calc R . . H10B H 0.8157 0.5249 0.3211 0.021 Uiso 1 1 calc R . . C11 C 0.79246(18) 0.3548(2) 0.19009(14) 0.0147(6) Uani 1 1 d . . . C12 C 0.7995(2) -0.0179(3) 0.12869(15) 0.0208(7) Uani 1 1 d . . . C13 C 0.8337(2) -0.0411(3) 0.06167(16) 0.0251(7) Uani 1 1 d . . . H13A H 0.8724 0.0226 0.0527 0.038 Uiso 1 1 calc R . . H13B H 0.7859 -0.0447 0.0254 0.038 Uiso 1 1 calc R . . H13C H 0.8646 -0.1160 0.0642 0.038 Uiso 1 1 calc R . . C14 C 0.8758(2) -0.0149(3) 0.18489(16) 0.0269(8) Uani 1 1 d . . . H14A H 0.8552 -0.0003 0.2281 0.040 Uiso 1 1 calc R . . H14B H 0.9151 0.0479 0.1757 0.040 Uiso 1 1 calc R . . H14C H 0.9056 -0.0906 0.1866 0.040 Uiso 1 1 calc R . . C15 C 0.7389(2) -0.1168(3) 0.14355(17) 0.0260(7) Uani 1 1 d . . . H15A H 0.7177 -0.1012 0.1864 0.039 Uiso 1 1 calc R . . H15B H 0.7694 -0.1919 0.1461 0.039 Uiso 1 1 calc R . . H15C H 0.6907 -0.1203 0.1076 0.039 Uiso 1 1 calc R . . C16 C 0.63828(19) 0.1354(3) 0.07923(15) 0.0184(6) Uani 1 1 d . . . C17 C 0.5718(2) 0.0836(3) 0.12009(16) 0.0243(7) Uani 1 1 d . . . H17A H 0.5839 0.0000 0.1286 0.036 Uiso 1 1 calc R . . H17B H 0.5148 0.0922 0.0949 0.036 Uiso 1 1 calc R . . H17C H 0.5742 0.1253 0.1629 0.036 Uiso 1 1 calc R . . C18 C 0.6342(2) 0.0716(3) 0.01174(15) 0.0239(7) Uani 1 1 d . . . H18A H 0.6475 -0.0118 0.0195 0.036 Uiso 1 1 calc R . . H18B H 0.6758 0.1065 -0.0146 0.036 Uiso 1 1 calc R . . H18C H 0.5768 0.0794 -0.0129 0.036 Uiso 1 1 calc R . . C19 C 0.6177(2) 0.2667(3) 0.06688(17) 0.0251(7) Uani 1 1 d . . . H19A H 0.6598 0.3016 0.0410 0.038 Uiso 1 1 calc R . . H19B H 0.6195 0.3074 0.1100 0.038 Uiso 1 1 calc R . . H19C H 0.5606 0.2746 0.0417 0.038 Uiso 1 1 calc R . . C20 C 0.8777(2) 0.3020(3) 0.37708(16) 0.0199(7) Uani 1 1 d . . . C21 C 0.8888(2) 0.1715(3) 0.39393(17) 0.0270(8) Uani 1 1 d . . . H21A H 0.8785 0.1251 0.3526 0.041 Uiso 1 1 calc R . . H21B H 0.8481 0.1484 0.4243 0.041 Uiso 1 1 calc R . . H21C H 0.9470 0.1573 0.4157 0.041 Uiso 1 1 calc R . . C22 C 0.9439(2) 0.3363(3) 0.33083(17) 0.0257(7) Uani 1 1 d . . . H22A H 0.9345 0.2895 0.2896 0.039 Uiso 1 1 calc R . . H22B H 1.0013 0.3212 0.3538 0.039 Uiso 1 1 calc R . . H22C H 0.9380 0.4200 0.3196 0.039 Uiso 1 1 calc R . . C23 C 0.8937(2) 0.3766(3) 0.44094(16) 0.0296(8) Uani 1 1 d . . . H23A H 0.8522 0.3558 0.4711 0.044 Uiso 1 1 calc R . . H23B H 0.8878 0.4601 0.4291 0.044 Uiso 1 1 calc R . . H23C H 0.9515 0.3617 0.4634 0.044 Uiso 1 1 calc R . . C24 C 0.6812(2) 0.3351(3) 0.38226(16) 0.0213(7) Uani 1 1 d . . . C25 C 0.6814(2) 0.4486(3) 0.42424(17) 0.0287(8) Uani 1 1 d . . . H25A H 0.6797 0.5171 0.3945 0.043 Uiso 1 1 calc R . . H25B H 0.7333 0.4515 0.4567 0.043 Uiso 1 1 calc R . . H25C H 0.6313 0.4495 0.4483 0.043 Uiso 1 1 calc R . . C26 C 0.5982(2) 0.3315(3) 0.33319(17) 0.0258(7) Uani 1 1 d . . . H26A H 0.5959 0.3998 0.3033 0.039 Uiso 1 1 calc R . . H26B H 0.5493 0.3332 0.3585 0.039 Uiso 1 1 calc R . . H26C H 0.5965 0.2592 0.3065 0.039 Uiso 1 1 calc R . . C27 C 0.6834(2) 0.2281(3) 0.42914(17) 0.0252(7) Uani 1 1 d . . . H27A H 0.7360 0.2298 0.4609 0.038 Uiso 1 1 calc R . . H27B H 0.6818 0.1557 0.4025 0.038 Uiso 1 1 calc R . . H27C H 0.6341 0.2304 0.4539 0.038 Uiso 1 1 calc R . . C28 C 0.7045(2) 0.0663(3) 0.27887(14) 0.0194(7) Uani 1 1 d . . . H28 H 0.7418 -0.0011 0.2986 0.024(9) Uiso 1 1 d R . . O29 O 0.62664(14) 0.0427(2) 0.28219(11) 0.0254(5) Uani 1 1 d . . . C30 C 0.6019(2) -0.0668(3) 0.31322(17) 0.0293(8) Uani 1 1 d . . . H30A H 0.5397 -0.0699 0.3110 0.044 Uiso 1 1 calc R . . H30B H 0.6278 -0.0694 0.3602 0.044 Uiso 1 1 calc R . . H30C H 0.6217 -0.1342 0.2891 0.044 Uiso 1 1 calc R . . C31 C 0.0766(3) 0.7946(4) 0.1090(3) 0.0522(12) Uani 1 1 d . . . F32 F 0.05089(18) 0.8844(3) 0.14299(18) 0.0868(10) Uani 1 1 d . . . F33 F 0.0429(2) 0.8070(3) 0.04496(19) 0.0915(12) Uani 1 1 d . . . F34 F 0.0457(2) 0.6958(3) 0.1315(2) 0.1055(15) Uani 1 1 d . . . S35 S 0.19106(6) 0.78869(7) 0.11681(4) 0.02501(18) Uani 1 1 d . . . O36 O 0.21254(16) 0.9005(2) 0.09019(13) 0.0376(6) Uani 1 1 d . . . O37 O 0.21667(18) 0.7747(2) 0.18792(13) 0.0371(7) Uani 1 1 d . . . O38 O 0.2078(3) 0.6894(3) 0.07687(15) 0.0618(10) Uani 1 1 d . . . O39 O 0.55205(19) -0.2440(3) 0.17197(14) 0.0413(7) Uani 1 1 d . . . C40 C 0.6007(2) -0.3356(3) 0.2068(2) 0.0363(9) Uani 1 1 d . . . H40A H 0.5827 -0.3480 0.2516 0.044 Uiso 1 1 calc R . . H40B H 0.6621 -0.3156 0.2126 0.044 Uiso 1 1 calc R . . C41 C 0.5849(3) -0.4424(4) 0.1654(2) 0.0490(11) Uani 1 1 d . . . H41A H 0.5336 -0.4846 0.1760 0.059 Uiso 1 1 calc R . . H41B H 0.6344 -0.4963 0.1719 0.059 Uiso 1 1 calc R . . C42 C 0.5716(3) -0.3942(4) 0.0948(2) 0.0556(12) Uani 1 1 d . . . H42A H 0.5374 -0.4485 0.0636 0.067 Uiso 1 1 calc R . . H42B H 0.6265 -0.3779 0.0780 0.067 Uiso 1 1 calc R . . C43 C 0.5236(4) -0.2825(4) 0.1049(2) 0.0540(14) Uani 1 1 d . . . H43A H 0.5360 -0.2221 0.0721 0.065 Uiso 1 1 calc R . . H43B H 0.4615 -0.2975 0.0991 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01613(7) 0.01515(7) 0.01313(7) 0.00045(4) 0.00236(5) -0.00064(4) P2 0.0178(4) 0.0158(4) 0.0122(3) 0.0013(3) 0.0026(3) -0.0005(3) P3 0.0149(4) 0.0162(4) 0.0138(3) -0.0017(3) 0.0024(3) 0.0008(3) C4 0.0166(16) 0.0239(17) 0.0151(15) -0.0027(12) 0.0034(12) -0.0020(13) C5 0.0133(15) 0.0189(16) 0.0197(15) 0.0000(12) -0.0002(12) -0.0005(12) C6 0.0175(16) 0.0266(17) 0.0184(15) 0.0062(13) 0.0049(12) 0.0007(13) C7 0.0270(18) 0.0226(17) 0.0228(16) 0.0076(13) 0.0053(14) -0.0036(14) C8 0.0236(16) 0.0163(15) 0.0214(16) 0.0022(12) 0.0012(13) -0.0024(13) C9 0.0172(15) 0.0213(16) 0.0148(14) 0.0005(12) 0.0006(12) 0.0017(12) C10 0.0237(16) 0.0141(14) 0.0146(14) 0.0019(12) 0.0022(12) -0.0001(12) C11 0.0113(14) 0.0175(15) 0.0158(14) 0.0029(12) 0.0043(11) 0.0004(11) C12 0.0237(17) 0.0204(16) 0.0189(15) -0.0012(13) 0.0045(13) 0.0017(13) C13 0.0282(18) 0.0239(17) 0.0239(17) -0.0046(14) 0.0064(14) 0.0055(14) C14 0.0239(17) 0.0339(19) 0.0225(17) 0.0008(14) 0.0009(14) 0.0112(15) C15 0.0331(19) 0.0173(16) 0.0291(18) -0.0011(14) 0.0094(15) 0.0023(14) C16 0.0172(15) 0.0177(15) 0.0193(15) -0.0024(12) -0.0013(12) 0.0006(12) C17 0.0184(16) 0.0276(17) 0.0267(17) -0.0034(14) 0.0018(13) -0.0020(13) C18 0.0232(17) 0.0286(17) 0.0189(15) -0.0046(13) -0.0008(13) -0.0009(14) C19 0.0245(18) 0.0233(17) 0.0260(18) 0.0003(14) -0.0029(14) 0.0049(14) C20 0.0191(16) 0.0213(16) 0.0183(15) 0.0008(12) -0.0012(13) 0.0025(12) C21 0.0261(18) 0.0262(17) 0.0267(17) 0.0036(15) -0.0042(15) 0.0052(15) C22 0.0173(16) 0.0310(18) 0.0282(17) 0.0019(15) 0.0004(14) -0.0012(14) C23 0.039(2) 0.0286(18) 0.0196(16) -0.0012(14) -0.0043(15) -0.0041(16) C24 0.0278(18) 0.0167(15) 0.0212(16) 0.0001(13) 0.0100(13) 0.0001(13) C25 0.037(2) 0.0224(17) 0.0291(18) -0.0044(14) 0.0148(15) -0.0019(15) C26 0.0211(17) 0.0248(16) 0.0331(18) 0.0035(15) 0.0096(14) 0.0027(14) C27 0.032(2) 0.0248(18) 0.0201(16) 0.0007(13) 0.0095(14) -0.0033(14) C28 0.0258(17) 0.0180(15) 0.0144(14) -0.0056(12) 0.0027(13) -0.0026(13) O29 0.0220(12) 0.0308(13) 0.0249(12) 0.0004(10) 0.0085(9) -0.0056(10) C30 0.0306(19) 0.0264(18) 0.0326(19) 0.0006(15) 0.0105(15) -0.0050(15) C31 0.035(2) 0.060(3) 0.061(3) -0.005(2) 0.001(2) -0.014(2) F32 0.0404(16) 0.107(3) 0.120(3) -0.017(2) 0.0356(17) 0.0199(17) F33 0.065(2) 0.106(3) 0.089(2) 0.002(2) -0.0451(19) -0.0027(18) F34 0.071(2) 0.113(3) 0.130(3) 0.026(2) 0.004(2) -0.066(2) S35 0.0301(5) 0.0256(4) 0.0201(4) 0.0034(3) 0.0061(3) 0.0067(3) O36 0.0382(15) 0.0377(15) 0.0378(15) 0.0171(12) 0.0078(12) 0.0002(12) O37 0.0457(17) 0.0422(16) 0.0218(13) 0.0112(11) -0.0019(12) -0.0070(12) O38 0.112(3) 0.0422(17) 0.0336(16) 0.0002(13) 0.0175(18) 0.0386(18) O39 0.0444(17) 0.0375(14) 0.0401(16) -0.0028(13) -0.0015(13) 0.0150(13) C40 0.029(2) 0.034(2) 0.044(2) 0.0079(18) -0.0002(17) -0.0004(16) C41 0.044(2) 0.043(2) 0.055(3) -0.007(2) -0.013(2) 0.006(2) C42 0.082(4) 0.045(3) 0.042(2) -0.016(2) 0.016(2) 0.002(2) C43 0.067(3) 0.042(3) 0.045(3) -0.0033(19) -0.024(2) 0.007(2) _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 C28 1.986(3) . ? Pt1 C11 2.081(3) . ? Pt1 P3 2.3010(7) . ? Pt1 P2 2.3029(8) . ? P2 C10 1.832(3) . ? P2 C20 1.873(3) . ? P2 C24 1.877(3) . ? P3 C4 1.827(3) . ? P3 C12 1.875(3) . ? P3 C16 1.881(3) . ? C4 C5 1.513(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.396(4) . ? C5 C11 1.414(4) . ? C6 C7 1.381(4) . ? C6 H6 0.9500 . ? C7 C8 1.393(5) . ? C7 H7 0.9500 . ? C8 C9 1.391(4) . ? C8 H8 0.9500 . ? C9 C11 1.402(4) . ? C9 C10 1.517(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C12 C15 1.533(4) . ? C12 C13 1.538(4) . ? C12 C14 1.542(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.532(4) . ? C16 C17 1.534(4) . ? C16 C19 1.542(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.528(4) . ? C20 C23 1.532(4) . ? C20 C22 1.538(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.537(4) . ? C24 C27 1.537(4) . ? C24 C25 1.542(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 O29 1.271(4) . ? C28 H28 1.0161 . ? O29 C30 1.469(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 F32 1.322(5) . ? C31 F34 1.328(5) . ? C31 F33 1.334(6) . ? C31 S35 1.799(5) . ? S35 O38 1.430(3) . ? S35 O36 1.437(3) . ? S35 O37 1.442(3) . ? O39 C40 1.424(4) . ? O39 C43 1.433(5) . ? C40 C41 1.475(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.508(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.508(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C28 Pt1 C11 179.19(12) . . ? C28 Pt1 P3 97.03(8) . . ? C11 Pt1 P3 82.19(8) . . ? C28 Pt1 P2 99.08(8) . . ? C11 Pt1 P2 81.68(8) . . ? P3 Pt1 P2 163.54(3) . . ? C10 P2 C20 105.94(14) . . ? C10 P2 C24 104.97(14) . . ? C20 P2 C24 114.14(15) . . ? C10 P2 Pt1 103.37(10) . . ? C20 P2 Pt1 111.09(10) . . ? C24 P2 Pt1 115.98(10) . . ? C4 P3 C12 105.00(14) . . ? C4 P3 C16 106.25(14) . . ? C12 P3 C16 113.65(14) . . ? C4 P3 Pt1 103.38(10) . . ? C12 P3 Pt1 114.56(10) . . ? C16 P3 Pt1 112.72(10) . . ? C5 C4 P3 109.2(2) . . ? C5 C4 H4A 109.8 . . ? P3 C4 H4A 109.8 . . ? C5 C4 H4B 109.8 . . ? P3 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? C6 C5 C11 120.7(3) . . ? C6 C5 C4 120.4(3) . . ? C11 C5 C4 118.8(3) . . ? C7 C6 C5 120.2(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.2(3) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 119.8(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C11 121.3(3) . . ? C8 C9 C10 119.2(3) . . ? C11 C9 C10 119.5(3) . . ? C9 C10 P2 108.4(2) . . ? C9 C10 H10A 110.0 . . ? P2 C10 H10A 110.0 . . ? C9 C10 H10B 110.0 . . ? P2 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C9 C11 C5 117.8(3) . . ? C9 C11 Pt1 121.2(2) . . ? C5 C11 Pt1 121.1(2) . . ? C15 C12 C13 110.2(3) . . ? C15 C12 C14 108.9(3) . . ? C13 C12 C14 108.3(3) . . ? C15 C12 P3 110.9(2) . . ? C13 C12 P3 112.3(2) . . ? C14 C12 P3 106.1(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C17 109.8(3) . . ? C18 C16 C19 109.4(3) . . ? C17 C16 C19 108.2(3) . . ? C18 C16 P3 113.4(2) . . ? C17 C16 P3 109.3(2) . . ? C19 C16 P3 106.4(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C23 110.6(3) . . ? C21 C20 C22 108.2(3) . . ? C23 C20 C22 108.3(3) . . ? C21 C20 P2 109.9(2) . . ? C23 C20 P2 112.7(2) . . ? C22 C20 P2 107.0(2) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C27 108.8(3) . . ? C26 C24 C25 108.3(3) . . ? C27 C24 C25 109.3(3) . . ? C26 C24 P2 105.8(2) . . ? C27 C24 P2 111.0(2) . . ? C25 C24 P2 113.5(2) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O29 C28 Pt1 125.5(2) . . ? O29 C28 H28 109.8 . . ? Pt1 C28 H28 124.6 . . ? C28 O29 C30 121.0(3) . . ? O29 C30 H30A 109.5 . . ? O29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? F32 C31 F34 109.0(5) . . ? F32 C31 F33 107.8(4) . . ? F34 C31 F33 107.4(4) . . ? F32 C31 S35 110.9(3) . . ? F34 C31 S35 110.4(3) . . ? F33 C31 S35 111.1(4) . . ? O38 S35 O36 114.83(19) . . ? O38 S35 O37 114.85(17) . . ? O36 S35 O37 114.62(16) . . ? O38 S35 C31 103.8(2) . . ? O36 S35 C31 102.61(19) . . ? O37 S35 C31 104.0(2) . . ? C40 O39 C43 108.7(3) . . ? O39 C40 C41 106.5(3) . . ? O39 C40 H40A 110.4 . . ? C41 C40 H40A 110.4 . . ? O39 C40 H40B 110.4 . . ? C41 C40 H40B 110.4 . . ? H40A C40 H40B 108.6 . . ? C40 C41 C42 102.9(3) . . ? C40 C41 H41A 111.2 . . ? C42 C41 H41A 111.2 . . ? C40 C41 H41B 111.2 . . ? C42 C41 H41B 111.2 . . ? H41A C41 H41B 109.1 . . ? C41 C42 C43 101.0(4) . . ? C41 C42 H42A 111.6 . . ? C43 C42 H42A 111.6 . . ? C41 C42 H42B 111.6 . . ? C43 C42 H42B 111.6 . . ? H42A C42 H42B 109.4 . . ? O39 C43 C42 106.4(3) . . ? O39 C43 H43A 110.5 . . ? C42 C43 H43A 110.5 . . ? O39 C43 H43B 110.5 . . ? C42 C43 H43B 110.5 . . ? H43A C43 H43B 108.6 . . ? 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 C28 Pt1 P2 C10 -161.26(14) . . . . ? C11 Pt1 P2 C10 19.01(13) . . . . ? P3 Pt1 P2 C10 30.56(15) . . . . ? C28 Pt1 P2 C20 85.52(15) . . . . ? C11 Pt1 P2 C20 -94.21(14) . . . . ? P3 Pt1 P2 C20 -82.66(15) . . . . ? C28 Pt1 P2 C24 -46.98(15) . . . . ? C11 Pt1 P2 C24 133.30(14) . . . . ? P3 Pt1 P2 C24 144.85(13) . . . . ? C28 Pt1 P3 C4 -163.03(14) . . . . ? C11 Pt1 P3 C4 16.74(13) . . . . ? P2 Pt1 P3 C4 5.20(15) . . . . ? C28 Pt1 P3 C12 -49.37(15) . . . . ? C11 Pt1 P3 C12 130.40(14) . . . . ? P2 Pt1 P3 C12 118.87(14) . . . . ? C28 Pt1 P3 C16 82.67(14) . . . . ? C11 Pt1 P3 C16 -97.56(13) . . . . ? P2 Pt1 P3 C16 -109.10(14) . . . . ? C12 P3 C4 C5 -144.1(2) . . . . ? C16 P3 C4 C5 95.2(2) . . . . ? Pt1 P3 C4 C5 -23.7(2) . . . . ? P3 C4 C5 C6 -162.9(2) . . . . ? P3 C4 C5 C11 20.2(3) . . . . ? C11 C5 C6 C7 2.5(4) . . . . ? C4 C5 C6 C7 -174.3(3) . . . . ? C5 C6 C7 C8 -1.3(5) . . . . ? C6 C7 C8 C9 -0.5(5) . . . . ? C7 C8 C9 C11 1.2(5) . . . . ? C7 C8 C9 C10 -177.2(3) . . . . ? C8 C9 C10 P2 -162.8(2) . . . . ? C11 C9 C10 P2 18.8(3) . . . . ? C20 P2 C10 C9 92.2(2) . . . . ? C24 P2 C10 C9 -146.7(2) . . . . ? Pt1 P2 C10 C9 -24.7(2) . . . . ? C8 C9 C11 C5 -0.1(4) . . . . ? C10 C9 C11 C5 178.3(3) . . . . ? C8 C9 C11 Pt1 -179.8(2) . . . . ? C10 C9 C11 Pt1 -1.4(4) . . . . ? C6 C5 C11 C9 -1.7(4) . . . . ? C4 C5 C11 C9 175.1(3) . . . . ? C6 C5 C11 Pt1 178.0(2) . . . . ? C4 C5 C11 Pt1 -5.2(4) . . . . ? C28 Pt1 C11 C9 -173(100) . . . . ? P3 Pt1 C11 C9 170.7(2) . . . . ? P2 Pt1 C11 C9 -12.6(2) . . . . ? C28 Pt1 C11 C5 7(8) . . . . ? P3 Pt1 C11 C5 -9.0(2) . . . . ? P2 Pt1 C11 C5 167.7(2) . . . . ? C4 P3 C12 C15 -165.0(2) . . . . ? C16 P3 C12 C15 -49.3(3) . . . . ? Pt1 P3 C12 C15 82.3(2) . . . . ? C4 P3 C12 C13 -41.3(3) . . . . ? C16 P3 C12 C13 74.4(3) . . . . ? Pt1 P3 C12 C13 -153.96(19) . . . . ? C4 P3 C12 C14 76.9(2) . . . . ? C16 P3 C12 C14 -167.4(2) . . . . ? Pt1 P3 C12 C14 -35.8(2) . . . . ? C4 P3 C16 C18 73.7(2) . . . . ? C12 P3 C16 C18 -41.3(3) . . . . ? Pt1 P3 C16 C18 -173.77(19) . . . . ? C4 P3 C16 C17 -163.4(2) . . . . ? C12 P3 C16 C17 81.7(2) . . . . ? Pt1 P3 C16 C17 -50.8(2) . . . . ? C4 P3 C16 C19 -46.7(2) . . . . ? C12 P3 C16 C19 -161.6(2) . . . . ? Pt1 P3 C16 C19 65.9(2) . . . . ? C10 P2 C20 C21 -165.3(2) . . . . ? C24 P2 C20 C21 79.7(3) . . . . ? Pt1 P2 C20 C21 -53.7(3) . . . . ? C10 P2 C20 C23 70.9(3) . . . . ? C24 P2 C20 C23 -44.1(3) . . . . ? Pt1 P2 C20 C23 -177.5(2) . . . . ? C10 P2 C20 C22 -48.0(2) . . . . ? C24 P2 C20 C22 -163.0(2) . . . . ? Pt1 P2 C20 C22 63.6(2) . . . . ? C10 P2 C24 C26 75.7(2) . . . . ? C20 P2 C24 C26 -168.8(2) . . . . ? Pt1 P2 C24 C26 -37.7(2) . . . . ? C10 P2 C24 C27 -166.4(2) . . . . ? C20 P2 C24 C27 -50.9(3) . . . . ? Pt1 P2 C24 C27 80.2(2) . . . . ? C10 P2 C24 C25 -42.9(3) . . . . ? C20 P2 C24 C25 72.6(3) . . . . ? Pt1 P2 C24 C25 -156.32(19) . . . . ? C11 Pt1 C28 O29 -107(8) . . . . ? P3 Pt1 C28 O29 -90.4(3) . . . . ? P2 Pt1 C28 O29 93.0(2) . . . . ? Pt1 C28 O29 C30 178.0(2) . . . . ? F32 C31 S35 O38 -179.1(3) . . . . ? F34 C31 S35 O38 59.9(4) . . . . ? F33 C31 S35 O38 -59.2(4) . . . . ? F32 C31 S35 O36 -59.3(4) . . . . ? F34 C31 S35 O36 179.7(4) . . . . ? F33 C31 S35 O36 60.6(3) . . . . ? F32 C31 S35 O37 60.4(4) . . . . ? F34 C31 S35 O37 -60.6(4) . . . . ? F33 C31 S35 O37 -179.7(3) . . . . ? C43 O39 C40 C41 -13.3(5) . . . . ? O39 C40 C41 C42 32.2(4) . . . . ? C40 C41 C42 C43 -37.3(5) . . . . ? C40 O39 C43 C42 -11.1(5) . . . . ? C41 C42 C43 O39 30.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.956 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.114 data_m765a _database_code_depnum_ccdc_archive 'CCDC 653984' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H35 O P2 Pt, 0.5(C6 H6), C F3 O3 S' _chemical_formula_sum 'C25 H38 F3 O4 P2 Pt S' _chemical_formula_weight 748.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.430(3) _cell_length_b 15.667(3) _cell_length_c 15.472(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.73(3) _cell_angle_gamma 90.00 _cell_volume 3002.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7426 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 4.895 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3214 _exptl_absorpt_correction_T_max 0.6403 _exptl_absorpt_process_details 'SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37774 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 28.26 _reflns_number_total 7410 _reflns_number_gt 6285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect package (Bruker Nonius)' _computing_cell_refinement HKL _computing_data_reduction HKL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+3.6674P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7410 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0565 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.031255(8) 0.729838(6) 0.334262(7) 0.01416(4) Uani 1 1 d . . . P1 P -0.13154(6) 0.70309(5) 0.21287(5) 0.01401(14) Uani 1 1 d . . . P2 P 0.21010(6) 0.73100(4) 0.43600(5) 0.01422(14) Uani 1 1 d . . . O1 O -0.05851(18) 0.84742(14) 0.44383(15) 0.0256(5) Uani 1 1 d . . . C1 C -0.0250(2) 0.80233(18) 0.40464(19) 0.0161(6) Uani 1 1 d . . . C2 C 0.0910(2) 0.65555(17) 0.25641(19) 0.0155(6) Uani 1 1 d . . . C3 C -0.1000(2) 0.61474(18) 0.1503(2) 0.0198(6) Uani 1 1 d . . . H3A H -0.1285 0.5607 0.1649 0.024 Uiso 1 1 calc R . . H3B H -0.1347 0.6246 0.0819 0.024 Uiso 1 1 calc R . . C4 C 0.0208(2) 0.60798(17) 0.17933(19) 0.0171(6) Uani 1 1 d . . . C5 C 0.0628(3) 0.55273(18) 0.1313(2) 0.0201(6) Uani 1 1 d . . . H5 H 0.0150 0.5205 0.0800 0.024 Uiso 1 1 calc R . . C6 C 0.1733(3) 0.54415(19) 0.1574(2) 0.0231(7) Uani 1 1 d . . . H6 H 0.2010 0.5052 0.1252 0.028 Uiso 1 1 calc R . . C7 C 0.2435(3) 0.5928(2) 0.2308(2) 0.0233(7) Uani 1 1 d . . . H7 H 0.3192 0.5884 0.2473 0.028 Uiso 1 1 calc R . . C8 C 0.2036(2) 0.64802(18) 0.28048(19) 0.0179(6) Uani 1 1 d . . . C9 C 0.2801(2) 0.7013(2) 0.3598(2) 0.0221(6) Uani 1 1 d . . . H9A H 0.3015 0.7532 0.3347 0.026 Uiso 1 1 calc R . . H9B H 0.3460 0.6682 0.3955 0.026 Uiso 1 1 calc R . . C10 C -0.1830(3) 0.79248(18) 0.1323(2) 0.0197(6) Uani 1 1 d . . . H10 H -0.2508 0.7739 0.0800 0.024 Uiso 1 1 calc R . . C11 C -0.2099(3) 0.8678(2) 0.1824(2) 0.0272(7) Uani 1 1 d . . . H11A H -0.1434 0.8896 0.2310 0.041 Uiso 1 1 calc R . . H11B H -0.2594 0.8489 0.2114 0.041 Uiso 1 1 calc R . . H11C H -0.2442 0.9131 0.1370 0.041 Uiso 1 1 calc R . . C12 C -0.1011(3) 0.8190(2) 0.0909(3) 0.0357(8) Uani 1 1 d . . . H12A H -0.1298 0.8673 0.0483 0.054 Uiso 1 1 calc R . . H12B H -0.0879 0.7709 0.0562 0.054 Uiso 1 1 calc R . . H12C H -0.0333 0.8356 0.1415 0.054 Uiso 1 1 calc R . . C13 C -0.2406(2) 0.66782(19) 0.2479(2) 0.0194(6) Uani 1 1 d . . . H13 H -0.2611 0.7175 0.2781 0.023 Uiso 1 1 calc R . . C14 C -0.2014(3) 0.5966(2) 0.3211(3) 0.0346(8) Uani 1 1 d . . . H14A H -0.2564 0.5853 0.3467 0.052 Uiso 1 1 calc R . . H14B H -0.1341 0.6142 0.3718 0.052 Uiso 1 1 calc R . . H14C H -0.1885 0.5446 0.2917 0.052 Uiso 1 1 calc R . . C15 C -0.3411(3) 0.6409(2) 0.1641(2) 0.0324(8) Uani 1 1 d . . . H15A H -0.3240 0.5916 0.1333 0.049 Uiso 1 1 calc R . . H15B H -0.3655 0.6883 0.1195 0.049 Uiso 1 1 calc R . . H15C H -0.3985 0.6255 0.1856 0.049 Uiso 1 1 calc R . . C16 C 0.2437(3) 0.64977(19) 0.5281(2) 0.0211(6) Uani 1 1 d . . . H16 H 0.3237 0.6507 0.5635 0.025 Uiso 1 1 calc R . . C17 C 0.1905(3) 0.6700(3) 0.5972(3) 0.0386(9) Uani 1 1 d . . . H17A H 0.1121 0.6730 0.5635 0.058 Uiso 1 1 calc R . . H17B H 0.2173 0.7250 0.6276 0.058 Uiso 1 1 calc R . . H17C H 0.2082 0.6250 0.6448 0.058 Uiso 1 1 calc R . . C18 C 0.2127(3) 0.5609(2) 0.4855(3) 0.0366(9) Uani 1 1 d . . . H18A H 0.2322 0.5183 0.5358 0.055 Uiso 1 1 calc R . . H18B H 0.2512 0.5486 0.4445 0.055 Uiso 1 1 calc R . . H18C H 0.1347 0.5587 0.4489 0.055 Uiso 1 1 calc R . . C19 C 0.2653(2) 0.83162(18) 0.4942(2) 0.0212(6) Uani 1 1 d . . . H19 H 0.2304 0.8433 0.5396 0.025 Uiso 1 1 calc R . . C20 C 0.3870(3) 0.8270(2) 0.5509(2) 0.0295(7) Uani 1 1 d . . . H20A H 0.4238 0.8119 0.5092 0.044 Uiso 1 1 calc R . . H20B H 0.4021 0.7835 0.5998 0.044 Uiso 1 1 calc R . . H20C H 0.4130 0.8825 0.5798 0.044 Uiso 1 1 calc R . . C21 C 0.2359(3) 0.9058(2) 0.4244(3) 0.0336(8) Uani 1 1 d . . . H21A H 0.2571 0.9598 0.4586 0.050 Uiso 1 1 calc R . . H21B H 0.1578 0.9058 0.3880 0.050 Uiso 1 1 calc R . . H21C H 0.2739 0.8993 0.3820 0.050 Uiso 1 1 calc R . . S1 S 0.40081(8) 0.32276(7) 0.13198(7) 0.0408(2) Uani 1 1 d . . . O2 O 0.4471(3) 0.26719(17) 0.0841(3) 0.0602(10) Uani 1 1 d . A . O3 O 0.4171(3) 0.3006(2) 0.2268(2) 0.0686(11) Uani 1 1 d . A . O4A O 0.2957(6) 0.3753(8) 0.0639(6) 0.051(3) Uiso 0.44(2) 1 d P A 1 O4B O 0.2949(5) 0.3367(6) 0.0833(5) 0.050(2) Uiso 0.56(2) 1 d P A 2 C31 C 0.4810(3) 0.4183(2) 0.1492(2) 0.0324(8) Uani 1 1 d . A . F1 F 0.5827(2) 0.40420(19) 0.2043(2) 0.0664(8) Uani 1 1 d . . . F2 F 0.4459(3) 0.48056(14) 0.18880(18) 0.0595(7) Uani 1 1 d . . . F3 F 0.4815(3) 0.44869(15) 0.06905(18) 0.0652(8) Uani 1 1 d . . . C32 C 0.4850(3) 0.4566(3) 0.4179(3) 0.0374(9) Uani 1 1 d . . . H32 H 0.4747 0.4269 0.3615 0.045 Uiso 1 1 calc R . . C33 C 0.4688(3) 0.4154(2) 0.4903(3) 0.0371(9) Uani 1 1 d . . . H33 H 0.4474 0.3571 0.4840 0.044 Uiso 1 1 calc R . . C34 C 0.4838(3) 0.4591(3) 0.5721(3) 0.0374(9) Uani 1 1 d . . . H34 H 0.4724 0.4306 0.6218 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01263(6) 0.01497(6) 0.01404(6) -0.00201(4) 0.00423(4) 0.00037(4) P1 0.0121(3) 0.0152(3) 0.0122(3) -0.0016(3) 0.0019(3) -0.0008(3) P2 0.0111(3) 0.0152(3) 0.0147(3) -0.0008(3) 0.0032(3) 0.0010(3) O1 0.0301(13) 0.0262(11) 0.0233(11) -0.0061(9) 0.0135(10) 0.0033(10) C1 0.0134(14) 0.0174(12) 0.0144(13) 0.0021(11) 0.0020(11) -0.0029(11) C2 0.0200(15) 0.0145(13) 0.0138(13) 0.0026(10) 0.0085(12) 0.0032(11) C3 0.0215(16) 0.0165(13) 0.0196(14) -0.0049(12) 0.0059(12) 0.0003(12) C4 0.0226(16) 0.0141(13) 0.0145(13) 0.0026(11) 0.0070(12) 0.0044(11) C5 0.0294(17) 0.0169(14) 0.0146(13) -0.0006(11) 0.0091(13) 0.0032(12) C6 0.0330(18) 0.0224(15) 0.0190(14) 0.0014(12) 0.0157(14) 0.0096(13) C7 0.0225(17) 0.0287(16) 0.0221(15) 0.0049(13) 0.0123(13) 0.0080(13) C8 0.0196(15) 0.0181(13) 0.0159(13) 0.0010(11) 0.0068(12) 0.0021(12) C9 0.0142(15) 0.0303(16) 0.0214(15) -0.0042(13) 0.0065(12) 0.0017(12) C10 0.0204(16) 0.0192(14) 0.0150(13) 0.0025(11) 0.0019(12) 0.0010(11) C11 0.0305(19) 0.0194(15) 0.0302(17) 0.0045(13) 0.0100(15) 0.0079(13) C12 0.053(2) 0.0285(18) 0.0350(19) 0.0058(15) 0.0275(18) 0.0043(17) C13 0.0138(15) 0.0236(15) 0.0198(14) -0.0009(12) 0.0055(12) -0.0027(11) C14 0.030(2) 0.0393(19) 0.0317(19) 0.0116(16) 0.0092(16) -0.0092(16) C15 0.0165(16) 0.041(2) 0.0340(18) 0.0007(16) 0.0031(14) -0.0087(15) C16 0.0207(16) 0.0227(15) 0.0171(14) 0.0039(12) 0.0041(12) 0.0034(12) C17 0.049(2) 0.045(2) 0.0298(18) 0.0105(16) 0.0238(18) 0.0107(18) C18 0.052(2) 0.0179(15) 0.0340(19) 0.0056(14) 0.0097(18) -0.0017(15) C19 0.0167(15) 0.0174(14) 0.0252(15) -0.0042(12) 0.0032(13) 0.0009(11) C20 0.0188(17) 0.0253(16) 0.0348(18) -0.0047(14) -0.0003(14) -0.0032(13) C21 0.0242(18) 0.0198(15) 0.046(2) 0.0041(15) 0.0021(16) -0.0013(13) S1 0.0377(5) 0.0515(6) 0.0427(5) -0.0190(5) 0.0262(5) -0.0190(4) O2 0.092(3) 0.0335(15) 0.078(2) -0.0187(15) 0.059(2) -0.0121(16) O3 0.110(3) 0.0587(19) 0.061(2) -0.0087(17) 0.059(2) -0.039(2) C31 0.046(2) 0.0293(18) 0.0292(18) 0.0050(14) 0.0225(17) 0.0056(16) F1 0.0321(14) 0.087(2) 0.0722(19) -0.0042(16) 0.0110(14) -0.0198(14) F2 0.112(2) 0.0299(12) 0.0551(15) -0.0032(11) 0.0524(17) 0.0110(13) F3 0.127(3) 0.0422(13) 0.0513(15) 0.0133(12) 0.0613(17) 0.0070(15) C32 0.0250(19) 0.048(2) 0.0293(19) -0.0040(17) -0.0006(15) 0.0062(17) C33 0.0198(18) 0.0306(18) 0.046(2) 0.0076(16) -0.0036(16) 0.0019(14) C34 0.0226(19) 0.055(2) 0.0314(19) 0.0176(17) 0.0069(15) 0.0053(17) _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 C1 1.919(3) . ? Pt1 C2 2.048(3) . ? Pt1 P1 2.3044(12) . ? Pt1 P2 2.3077(11) . ? P1 C10 1.824(3) . ? P1 C3 1.830(3) . ? P1 C13 1.832(3) . ? P2 C19 1.825(3) . ? P2 C9 1.829(3) . ? P2 C16 1.832(3) . ? O1 C1 1.132(3) . ? C2 C4 1.413(4) . ? C2 C8 1.416(4) . ? C3 C4 1.510(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.394(4) . ? C5 C6 1.386(4) . ? C5 H5 0.9500 . ? C6 C7 1.390(5) . ? C6 H6 0.9500 . ? C7 C8 1.394(4) . ? C7 H7 0.9500 . ? C8 C9 1.512(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C12 1.529(5) . ? C10 C11 1.530(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.526(4) . ? C13 C14 1.532(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.528(4) . ? C16 C17 1.532(4) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.529(4) . ? C19 C21 1.530(4) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? S1 O4B 1.345(6) . ? S1 O2 1.432(3) . ? S1 O3 1.440(3) . ? S1 O4A 1.622(10) . ? S1 C31 1.803(4) . ? C31 F1 1.321(4) . ? C31 F3 1.330(4) . ? C31 F2 1.331(4) . ? C32 C34 1.377(6) 3_666 ? C32 C33 1.381(5) . ? C32 H32 0.9500 . ? C33 C34 1.383(6) . ? C33 H33 0.9500 . ? C34 C32 1.377(6) 3_666 ? C34 H34 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 C2 178.23(11) . . ? C1 Pt1 P1 96.47(9) . . ? C2 Pt1 P1 83.18(8) . . ? C1 Pt1 P2 98.18(9) . . ? C2 Pt1 P2 82.22(9) . . ? P1 Pt1 P2 165.25(3) . . ? C10 P1 C3 108.88(14) . . ? C10 P1 C13 107.36(14) . . ? C3 P1 C13 107.64(14) . . ? C10 P1 Pt1 114.01(10) . . ? C3 P1 Pt1 103.17(10) . . ? C13 P1 Pt1 115.41(10) . . ? C19 P2 C9 108.99(15) . . ? C19 P2 C16 106.59(14) . . ? C9 P2 C16 106.93(15) . . ? C19 P2 Pt1 117.43(10) . . ? C9 P2 Pt1 102.53(10) . . ? C16 P2 Pt1 113.81(11) . . ? O1 C1 Pt1 177.5(2) . . ? C4 C2 C8 118.3(3) . . ? C4 C2 Pt1 120.7(2) . . ? C8 C2 Pt1 120.9(2) . . ? C4 C3 P1 109.7(2) . . ? C4 C3 H3A 109.7 . . ? P1 C3 H3A 109.7 . . ? C4 C3 H3B 109.7 . . ? P1 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C2 120.1(3) . . ? C5 C4 C3 119.6(3) . . ? C2 C4 C3 120.2(2) . . ? C6 C5 C4 120.9(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 119.8(3) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C8 120.5(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C2 120.4(3) . . ? C7 C8 C9 120.3(3) . . ? C2 C8 C9 119.3(3) . . ? C8 C9 P2 107.8(2) . . ? C8 C9 H9A 110.1 . . ? P2 C9 H9A 110.1 . . ? C8 C9 H9B 110.1 . . ? P2 C9 H9B 110.1 . . ? H9A C9 H9B 108.5 . . ? C12 C10 C11 110.6(3) . . ? C12 C10 P1 110.6(2) . . ? C11 C10 P1 110.3(2) . . ? C12 C10 H10 108.4 . . ? C11 C10 H10 108.4 . . ? P1 C10 H10 108.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 111.4(3) . . ? C15 C13 P1 112.2(2) . . ? C14 C13 P1 110.7(2) . . ? C15 C13 H13 107.4 . . ? C14 C13 H13 107.4 . . ? P1 C13 H13 107.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C17 111.5(3) . . ? C18 C16 P2 110.7(2) . . ? C17 C16 P2 111.0(2) . . ? C18 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? P2 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 111.6(3) . . ? C20 C19 P2 112.5(2) . . ? C21 C19 P2 111.3(2) . . ? C20 C19 H19 107.0 . . ? C21 C19 H19 107.0 . . ? P2 C19 H19 107.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O4B S1 O2 112.6(3) . . ? O4B S1 O3 108.7(4) . . ? O2 S1 O3 117.1(2) . . ? O2 S1 O4A 114.6(3) . . ? O3 S1 O4A 122.4(3) . . ? O4B S1 C31 112.9(5) . . ? O2 S1 C31 103.15(17) . . ? O3 S1 C31 101.70(18) . . ? O4A S1 C31 89.7(4) . . ? F1 C31 F3 106.6(3) . . ? F1 C31 F2 106.7(3) . . ? F3 C31 F2 107.3(3) . . ? F1 C31 S1 111.5(3) . . ? F3 C31 S1 112.2(3) . . ? F2 C31 S1 112.3(3) . . ? C34 C32 C33 119.6(3) 3_666 . ? C34 C32 H32 120.2 3_666 . ? C33 C32 H32 120.2 . . ? C32 C33 C34 119.9(3) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C32 C34 C33 120.5(3) 3_666 . ? C32 C34 H34 119.7 3_666 . ? C33 C34 H34 119.7 . . ? 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 C1 Pt1 P1 C10 74.60(14) . . . . ? C2 Pt1 P1 C10 -103.65(14) . . . . ? P2 Pt1 P1 C10 -111.76(14) . . . . ? C1 Pt1 P1 C3 -167.49(13) . . . . ? C2 Pt1 P1 C3 14.26(13) . . . . ? P2 Pt1 P1 C3 6.15(15) . . . . ? C1 Pt1 P1 C13 -50.37(14) . . . . ? C2 Pt1 P1 C13 131.37(13) . . . . ? P2 Pt1 P1 C13 123.26(14) . . . . ? C1 Pt1 P2 C19 -38.96(15) . . . . ? C2 Pt1 P2 C19 139.29(14) . . . . ? P1 Pt1 P2 C19 147.42(14) . . . . ? C1 Pt1 P2 C9 -158.37(14) . . . . ? C2 Pt1 P2 C9 19.89(13) . . . . ? P1 Pt1 P2 C9 28.01(16) . . . . ? C1 Pt1 P2 C16 86.53(14) . . . . ? C2 Pt1 P2 C16 -95.21(13) . . . . ? P1 Pt1 P2 C16 -87.08(15) . . . . ? P1 Pt1 C2 C4 -11.5(2) . . . . ? P2 Pt1 C2 C4 166.4(2) . . . . ? P1 Pt1 C2 C8 170.9(2) . . . . ? P2 Pt1 C2 C8 -11.2(2) . . . . ? C10 P1 C3 C4 104.8(2) . . . . ? C13 P1 C3 C4 -139.1(2) . . . . ? Pt1 P1 C3 C4 -16.6(2) . . . . ? C8 C2 C4 C5 2.5(4) . . . . ? Pt1 C2 C4 C5 -175.2(2) . . . . ? C8 C2 C4 C3 -179.3(3) . . . . ? Pt1 C2 C4 C3 3.0(4) . . . . ? P1 C3 C4 C5 -171.2(2) . . . . ? P1 C3 C4 C2 10.5(3) . . . . ? C2 C4 C5 C6 -0.7(4) . . . . ? C3 C4 C5 C6 -178.9(3) . . . . ? C4 C5 C6 C7 -1.7(4) . . . . ? C5 C6 C7 C8 2.2(4) . . . . ? C6 C7 C8 C2 -0.3(4) . . . . ? C6 C7 C8 C9 -179.5(3) . . . . ? C4 C2 C8 C7 -2.0(4) . . . . ? Pt1 C2 C8 C7 175.7(2) . . . . ? C4 C2 C8 C9 177.2(3) . . . . ? Pt1 C2 C8 C9 -5.2(4) . . . . ? C7 C8 C9 P2 -157.8(2) . . . . ? C2 C8 C9 P2 23.0(3) . . . . ? C19 P2 C9 C8 -152.4(2) . . . . ? C16 P2 C9 C8 92.8(2) . . . . ? Pt1 P2 C9 C8 -27.2(2) . . . . ? C3 P1 C10 C12 -57.1(3) . . . . ? C13 P1 C10 C12 -173.4(2) . . . . ? Pt1 P1 C10 C12 57.5(2) . . . . ? C3 P1 C10 C11 -179.8(2) . . . . ? C13 P1 C10 C11 63.9(2) . . . . ? Pt1 P1 C10 C11 -65.2(2) . . . . ? C10 P1 C13 C15 58.8(3) . . . . ? C3 P1 C13 C15 -58.3(3) . . . . ? Pt1 P1 C13 C15 -172.9(2) . . . . ? C10 P1 C13 C14 -176.1(2) . . . . ? C3 P1 C13 C14 66.9(3) . . . . ? Pt1 P1 C13 C14 -47.7(2) . . . . ? C19 P2 C16 C18 -173.3(2) . . . . ? C9 P2 C16 C18 -56.8(3) . . . . ? Pt1 P2 C16 C18 55.7(3) . . . . ? C19 P2 C16 C17 62.3(3) . . . . ? C9 P2 C16 C17 178.8(2) . . . . ? Pt1 P2 C16 C17 -68.7(3) . . . . ? C9 P2 C19 C20 -57.6(3) . . . . ? C16 P2 C19 C20 57.5(3) . . . . ? Pt1 P2 C19 C20 -173.51(19) . . . . ? C9 P2 C19 C21 68.5(3) . . . . ? C16 P2 C19 C21 -176.4(2) . . . . ? Pt1 P2 C19 C21 -47.4(3) . . . . ? O4B S1 C31 F1 174.2(4) . . . . ? O2 S1 C31 F1 -63.9(3) . . . . ? O3 S1 C31 F1 57.9(3) . . . . ? O4A S1 C31 F1 -179.1(4) . . . . ? O4B S1 C31 F3 -66.4(4) . . . . ? O2 S1 C31 F3 55.5(3) . . . . ? O3 S1 C31 F3 177.3(3) . . . . ? O4A S1 C31 F3 -59.7(4) . . . . ? O4B S1 C31 F2 54.6(4) . . . . ? O2 S1 C31 F2 176.5(3) . . . . ? O3 S1 C31 F2 -61.8(3) . . . . ? O4A S1 C31 F2 61.3(4) . . . . ? C34 C32 C33 C34 0.1(6) 3_666 . . . ? C32 C33 C34 C32 -0.1(6) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.169 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.117 # Attachment 'compound8a_new.cif' data_m755 _database_code_depnum_ccdc_archive 'CCDC 654331' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H43 O P2 Pt, B F4' _chemical_formula_sum 'C25 H43 B F4 O P2 Pt' _chemical_formula_weight 703.43 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' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7910(2) _cell_length_b 26.9261(4) _cell_length_c 21.0591(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.5884(6) _cell_angle_gamma 90.00 _cell_volume 8378.5(2) _cell_formula_units_Z 12 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 14469 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'Leaf shape' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4200 _exptl_absorpt_coefficient_mu 5.182 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.0178 _exptl_absorpt_correction_T_max 0.1815 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Nonius Kappa CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48040 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0936 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 28.27 _reflns_number_total 20527 _reflns_number_gt 13643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect package Bruker - Nonius' _computing_cell_refinement HKL _computing_data_reduction HKL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20527 _refine_ls_number_parameters 926 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1491 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.045955(17) 0.627574(11) 0.635072(12) 0.01653(8) Uani 1 1 d . . . P2 P 0.16036(11) 0.67224(8) 0.58927(8) 0.0173(4) Uani 1 1 d . . . P3 P -0.09185(12) 0.59659(8) 0.66613(9) 0.0202(4) Uani 1 1 d . . . C4 C -0.1678(5) 0.6498(3) 0.6534(4) 0.0236(17) Uani 1 1 d . . . H4A H -0.2263 0.6384 0.6339 0.028 Uiso 1 1 calc R . . H4B H -0.1794 0.6657 0.6946 0.028 Uiso 1 1 calc R . . C5 C -0.1256(5) 0.6868(3) 0.6105(3) 0.0238(17) Uani 1 1 d . . . C6 C -0.1772(4) 0.7277(3) 0.5884(3) 0.0211(16) Uani 1 1 d . . . H6 H -0.2388 0.7303 0.5990 0.025 Uiso 1 1 calc R . . C7 C -0.1401(4) 0.7637(3) 0.5516(3) 0.0239(17) Uani 1 1 d . . . H7 H -0.1758 0.7911 0.5370 0.029 Uiso 1 1 calc R . . C8 C -0.0495(4) 0.7602(3) 0.5356(3) 0.0204(16) Uani 1 1 d . . . H8 H -0.0233 0.7854 0.5106 0.025 Uiso 1 1 calc R . . C9 C 0.0021(4) 0.7197(3) 0.5564(3) 0.0213(17) Uani 1 1 d . . . C10 C -0.0342(4) 0.6828(3) 0.5957(3) 0.0162(15) Uani 1 1 d . . . C11 C 0.0984(4) 0.7140(3) 0.5351(3) 0.0252(18) Uani 1 1 d . . . H11A H 0.1286 0.7468 0.5349 0.030 Uiso 1 1 calc R . . H11B H 0.0975 0.7003 0.4914 0.030 Uiso 1 1 calc R . . C12 C 0.2239(4) 0.7121(3) 0.6477(3) 0.0210(16) Uani 1 1 d . . . C13 C 0.1534(4) 0.7477(3) 0.6755(4) 0.0264(18) Uani 1 1 d . . . H13A H 0.1076 0.7284 0.6969 0.040 Uiso 1 1 calc R . . H13B H 0.1241 0.7672 0.6410 0.040 Uiso 1 1 calc R . . H13C H 0.1839 0.7702 0.7061 0.040 Uiso 1 1 calc R . . C14 C 0.2647(5) 0.6811(3) 0.7035(3) 0.031(2) Uani 1 1 d . . . H14A H 0.3078 0.6570 0.6874 0.046 Uiso 1 1 calc R . . H14B H 0.2162 0.6634 0.7243 0.046 Uiso 1 1 calc R . . H14C H 0.2961 0.7031 0.7343 0.046 Uiso 1 1 calc R . . C15 C 0.2992(5) 0.7420(3) 0.6177(4) 0.0308(19) Uani 1 1 d . . . H15A H 0.3249 0.7657 0.6489 0.046 Uiso 1 1 calc R . . H15B H 0.2741 0.7601 0.5805 0.046 Uiso 1 1 calc R . . H15C H 0.3467 0.7194 0.6045 0.046 Uiso 1 1 calc R . . C16 C 0.2322(4) 0.6342(3) 0.5366(3) 0.0213(17) Uani 1 1 d . . . C17 C 0.1675(5) 0.6010(3) 0.4962(4) 0.035(2) Uani 1 1 d . . . H17A H 0.2021 0.5819 0.4660 0.053 Uiso 1 1 calc R . . H17B H 0.1229 0.6218 0.4729 0.053 Uiso 1 1 calc R . . H17C H 0.1362 0.5781 0.5241 0.053 Uiso 1 1 calc R . . C18 C 0.2863(5) 0.6680(3) 0.4917(4) 0.032(2) Uani 1 1 d . . . H18A H 0.3356 0.6844 0.5162 0.048 Uiso 1 1 calc R . . H18B H 0.2458 0.6932 0.4724 0.048 Uiso 1 1 calc R . . H18C H 0.3115 0.6477 0.4582 0.048 Uiso 1 1 calc R . . C19 C 0.2973(5) 0.6012(3) 0.5753(4) 0.032(2) Uani 1 1 d . . . H19A H 0.2631 0.5801 0.6037 0.047 Uiso 1 1 calc R . . H19B H 0.3397 0.6219 0.6007 0.047 Uiso 1 1 calc R . . H19C H 0.3310 0.5802 0.5466 0.047 Uiso 1 1 calc R . . C20 C -0.0965(5) 0.5821(3) 0.7525(3) 0.0263(18) Uani 1 1 d . . . C21 C -0.0534(5) 0.5322(3) 0.7702(4) 0.035(2) Uani 1 1 d . . . H21A H -0.0511 0.5283 0.8165 0.052 Uiso 1 1 calc R . . H21B H 0.0081 0.5309 0.7549 0.052 Uiso 1 1 calc R . . H21C H -0.0896 0.5053 0.7506 0.052 Uiso 1 1 calc R . . C22 C -0.1939(5) 0.5828(4) 0.7749(4) 0.043(3) Uani 1 1 d . . . H22A H -0.2268 0.5539 0.7575 0.064 Uiso 1 1 calc R . . H22B H -0.2242 0.6133 0.7600 0.064 Uiso 1 1 calc R . . H22C H -0.1928 0.5816 0.8214 0.064 Uiso 1 1 calc R . . C23 C -0.0427(6) 0.6238(4) 0.7867(4) 0.042(2) Uani 1 1 d . . . H23A H -0.0455 0.6195 0.8328 0.062 Uiso 1 1 calc R . . H23B H -0.0689 0.6560 0.7744 0.062 Uiso 1 1 calc R . . H23C H 0.0205 0.6225 0.7747 0.062 Uiso 1 1 calc R . . C24 C -0.1315(5) 0.5464(3) 0.6116(4) 0.0265(18) Uani 1 1 d . . . C25 C -0.0624(5) 0.5039(3) 0.6101(4) 0.039(2) Uani 1 1 d . . . H25A H -0.0585 0.4873 0.6516 0.058 Uiso 1 1 calc R . . H25B H -0.0029 0.5173 0.6006 0.058 Uiso 1 1 calc R . . H25C H -0.0816 0.4799 0.5772 0.058 Uiso 1 1 calc R . . C26 C -0.1432(5) 0.5692(4) 0.5447(4) 0.041(2) Uani 1 1 d . . . H26A H -0.1620 0.5433 0.5142 0.061 Uiso 1 1 calc R . . H26B H -0.0856 0.5835 0.5325 0.061 Uiso 1 1 calc R . . H26C H -0.1894 0.5952 0.5447 0.061 Uiso 1 1 calc R . . C27 C -0.2234(5) 0.5244(3) 0.6293(4) 0.037(2) Uani 1 1 d . . . H27A H -0.2460 0.5021 0.5953 0.055 Uiso 1 1 calc R . . H27B H -0.2669 0.5513 0.6347 0.055 Uiso 1 1 calc R . . H27C H -0.2157 0.5057 0.6691 0.055 Uiso 1 1 calc R . . C28 C 0.1234(4) 0.5812(3) 0.6811(3) 0.0239(18) Uani 1 1 d . . . O29 O 0.1677(3) 0.5561(2) 0.7110(2) 0.0337(15) Uani 1 1 d . . . Pt30 Pt 0.305366(16) 0.390218(12) 0.694506(12) 0.01738(8) Uani 1 1 d . . . P31 P 0.44575(11) 0.42570(8) 0.67853(9) 0.0183(4) Uani 1 1 d . . . P32 P 0.18530(11) 0.33853(8) 0.71565(9) 0.0200(4) Uani 1 1 d . A . C33 C 0.2402(5) 0.2830(3) 0.7480(5) 0.045(3) Uani 1 1 d . . . H33A H 0.2181 0.2762 0.7908 0.055 Uiso 1 1 calc R . . H33B H 0.2242 0.2542 0.7205 0.055 Uiso 1 1 calc R . . C34 C 0.3420(5) 0.2890(3) 0.7525(3) 0.0237(17) Uani 1 1 d . . . C35 C 0.3935(5) 0.2495(3) 0.7757(3) 0.0248(17) Uani 1 1 d . . . H35 H 0.3648 0.2205 0.7907 0.030 Uiso 1 1 calc R . . C36 C 0.4878(5) 0.2524(3) 0.7772(3) 0.0277(18) Uani 1 1 d . . . H36 H 0.5234 0.2252 0.7924 0.033 Uiso 1 1 calc R . . C37 C 0.5294(5) 0.2954(3) 0.7563(3) 0.0266(19) Uani 1 1 d . . . H37 H 0.5936 0.2972 0.7570 0.032 Uiso 1 1 calc R . . C38 C 0.4783(5) 0.3354(3) 0.7346(3) 0.0230(17) Uani 1 1 d . . . C39 C 0.3824(4) 0.3325(3) 0.7319(3) 0.0187(16) Uani 1 1 d . . . C40 C 0.5259(4) 0.3826(3) 0.7176(3) 0.0262(19) Uani 1 1 d . . . H40A H 0.5752 0.3750 0.6887 0.031 Uiso 1 1 calc R . . H40B H 0.5532 0.3981 0.7565 0.031 Uiso 1 1 calc R . . C41 C 0.4685(5) 0.4265(3) 0.5922(3) 0.0249(17) Uani 1 1 d . . . C42 C 0.4764(5) 0.3709(3) 0.5721(4) 0.035(2) Uani 1 1 d . . . H42A H 0.4818 0.3689 0.5259 0.052 Uiso 1 1 calc R . . H42B H 0.4222 0.3529 0.5841 0.052 Uiso 1 1 calc R . . H42C H 0.5300 0.3561 0.5935 0.052 Uiso 1 1 calc R . . C43 C 0.5558(5) 0.4533(4) 0.5774(4) 0.040(2) Uani 1 1 d . . . H43A H 0.5681 0.4487 0.5324 0.060 Uiso 1 1 calc R . . H43B H 0.6060 0.4397 0.6038 0.060 Uiso 1 1 calc R . . H43C H 0.5493 0.4888 0.5863 0.060 Uiso 1 1 calc R . . C44 C 0.3902(5) 0.4495(3) 0.5529(3) 0.035(2) Uani 1 1 d . . . H44A H 0.3793 0.4833 0.5681 0.052 Uiso 1 1 calc R . . H44B H 0.3356 0.4294 0.5573 0.052 Uiso 1 1 calc R . . H44C H 0.4053 0.4506 0.5081 0.052 Uiso 1 1 calc R . . C45 C 0.4658(4) 0.4862(3) 0.7206(3) 0.0242(18) Uani 1 1 d . . . C46 C 0.4124(5) 0.5281(3) 0.6886(4) 0.034(2) Uani 1 1 d . . . H46A H 0.4158 0.5576 0.7157 0.051 Uiso 1 1 calc R . . H46B H 0.3491 0.5179 0.6818 0.051 Uiso 1 1 calc R . . H46C H 0.4380 0.5356 0.6476 0.051 Uiso 1 1 calc R . . C47 C 0.4323(5) 0.4789(4) 0.7879(4) 0.039(2) Uani 1 1 d . . . H47A H 0.4419 0.5096 0.8124 0.059 Uiso 1 1 calc R . . H47B H 0.4660 0.4518 0.8089 0.059 Uiso 1 1 calc R . . H47C H 0.3677 0.4708 0.7854 0.059 Uiso 1 1 calc R . . C48 C 0.5672(5) 0.4999(4) 0.7253(4) 0.034(2) Uani 1 1 d . . . H48A H 0.5890 0.5049 0.6826 0.052 Uiso 1 1 calc R . . H48B H 0.6014 0.4729 0.7464 0.052 Uiso 1 1 calc R . . H48C H 0.5755 0.5305 0.7500 0.052 Uiso 1 1 calc R . . C49 C 0.1257(5) 0.3160(3) 0.6410(4) 0.031(2) Uani 1 1 d . . . C50 C 0.0614(5) 0.2734(4) 0.6509(4) 0.052(3) Uani 1 1 d . A . H50A H 0.0359 0.2621 0.6097 0.077 Uiso 1 1 calc R . . H50B H 0.0124 0.2846 0.6773 0.077 Uiso 1 1 calc R . . H50C H 0.0941 0.2460 0.6722 0.077 Uiso 1 1 calc R . . C51A C 0.0548(18) 0.3615(9) 0.6149(12) 0.036(6) Uani 0.47(4) 1 d P A 1 H51A H 0.0884 0.3928 0.6123 0.053 Uiso 0.47(4) 1 calc PR A 1 H51B H 0.0060 0.3654 0.6445 0.053 Uiso 0.47(4) 1 calc PR A 1 H51C H 0.0288 0.3529 0.5727 0.053 Uiso 0.47(4) 1 calc PR A 1 C52A C 0.1937(13) 0.3095(10) 0.5892(10) 0.035(7) Uani 0.53(4) 1 d P A 1 H52A H 0.2368 0.2832 0.6016 0.053 Uiso 0.53(4) 1 calc PR A 1 H52B H 0.2265 0.3407 0.5836 0.053 Uiso 0.53(4) 1 calc PR A 1 H52C H 0.1616 0.3004 0.5492 0.053 Uiso 0.53(4) 1 calc PR A 1 C51B C 0.089(2) 0.3534(11) 0.6020(12) 0.057(8) Uiso 0.53(4) 1 d P A 2 H51D H 0.0588 0.3385 0.5643 0.086 Uiso 0.53(4) 1 calc PR A 2 H51E H 0.1376 0.3754 0.5889 0.086 Uiso 0.53(4) 1 calc PR A 2 H51F H 0.0451 0.3725 0.6254 0.086 Uiso 0.53(4) 1 calc PR A 2 C52B C 0.2069(16) 0.2852(14) 0.6101(15) 0.057(8) Uiso 0.47(4) 1 d P A 2 H52D H 0.2272 0.2587 0.6393 0.086 Uiso 0.47(4) 1 calc PR A 2 H52E H 0.2575 0.3076 0.6028 0.086 Uiso 0.47(4) 1 calc PR A 2 H52F H 0.1851 0.2706 0.5696 0.086 Uiso 0.47(4) 1 calc PR A 2 C53 C 0.1132(5) 0.3632(3) 0.7782(3) 0.0272(18) Uani 1 1 d . . . C54 C 0.0416(5) 0.3253(3) 0.7986(4) 0.037(2) Uani 1 1 d . A . H54A H 0.0170 0.3359 0.8388 0.056 Uiso 1 1 calc R . . H54B H 0.0697 0.2925 0.8041 0.056 Uiso 1 1 calc R . . H54C H -0.0074 0.3234 0.7658 0.056 Uiso 1 1 calc R . . C55 C 0.1794(6) 0.3735(4) 0.8353(4) 0.063(4) Uani 1 1 d . A . H55A H 0.2290 0.3945 0.8218 0.094 Uiso 1 1 calc R . . H55B H 0.2039 0.3420 0.8518 0.094 Uiso 1 1 calc R . . H55C H 0.1473 0.3905 0.8688 0.094 Uiso 1 1 calc R . . C56 C 0.0669(6) 0.4111(3) 0.7576(5) 0.052(3) Uani 1 1 d . A . H56A H 0.0352 0.4251 0.7934 0.078 Uiso 1 1 calc R . . H56B H 0.0232 0.4044 0.7223 0.078 Uiso 1 1 calc R . . H56C H 0.1122 0.4349 0.7438 0.078 Uiso 1 1 calc R . . C57 C 0.2331(4) 0.4429(3) 0.6550(3) 0.0266(19) Uani 1 1 d . . . O58 O 0.1923(3) 0.4718(2) 0.6299(3) 0.0325(14) Uani 1 1 d . . . Pt59 Pt 0.632312(16) 0.379371(12) 1.022992(12) 0.01852(8) Uani 1 1 d . . . P60 P 0.51412(11) 0.33103(8) 1.05704(8) 0.0184(4) Uani 1 1 d . . . P61 P 0.77134(12) 0.41728(8) 1.00765(9) 0.0212(4) Uani 1 1 d . . . C62 C 0.8529(4) 0.3695(3) 1.0345(4) 0.029(2) Uani 1 1 d . . . H62A H 0.8787 0.3533 0.9973 0.035 Uiso 1 1 calc R . . H62B H 0.9030 0.3851 1.0602 0.035 Uiso 1 1 calc R . . C63 C 0.8072(4) 0.3320(3) 1.0733(3) 0.0222(17) Uani 1 1 d . . . C64 C 0.8581(5) 0.2979(3) 1.1098(3) 0.0237(17) Uani 1 1 d . . . H64 H 0.9221 0.3012 1.1124 0.028 Uiso 1 1 calc R . . C65 C 0.8187(5) 0.2598(3) 1.1423(3) 0.0246(17) Uani 1 1 d . . . H65 H 0.8552 0.2380 1.1679 0.030 Uiso 1 1 calc R . . C66 C 0.7258(4) 0.2535(3) 1.1375(3) 0.0237(17) Uani 1 1 d . . . H66 H 0.6984 0.2265 1.1584 0.028 Uiso 1 1 calc R . . C67 C 0.6722(4) 0.2874(3) 1.1015(3) 0.0183(15) Uani 1 1 d . . . C68 C 0.7117(4) 0.3272(3) 1.0697(3) 0.0176(15) Uani 1 1 d . . . C69 C 0.5719(4) 0.2770(3) 1.0938(4) 0.030(2) Uani 1 1 d . . . H69A H 0.5472 0.2702 1.1358 0.036 Uiso 1 1 calc R . . H69B H 0.5615 0.2473 1.0667 0.036 Uiso 1 1 calc R . . C70 C 0.4383(4) 0.3037(3) 0.9924(3) 0.0244(18) Uani 1 1 d . . . C71 C 0.3806(5) 0.2611(3) 1.0170(4) 0.034(2) Uani 1 1 d . . . H71A H 0.3335 0.2746 1.0433 0.051 Uiso 1 1 calc R . . H71B H 0.4191 0.2383 1.0424 0.051 Uiso 1 1 calc R . . H71C H 0.3522 0.2431 0.9809 0.051 Uiso 1 1 calc R . . C72 C 0.5022(5) 0.2836(4) 0.9426(4) 0.055(3) Uani 1 1 d . . . H72A H 0.5422 0.2583 0.9622 0.083 Uiso 1 1 calc R . . H72B H 0.5387 0.3108 0.9266 0.083 Uiso 1 1 calc R . . H72C H 0.4663 0.2687 0.9072 0.083 Uiso 1 1 calc R . . C73 C 0.3772(5) 0.3429(4) 0.9608(4) 0.038(2) Uani 1 1 d . . . H73A H 0.3399 0.3276 0.9265 0.058 Uiso 1 1 calc R . . H73B H 0.4144 0.3693 0.9433 0.058 Uiso 1 1 calc R . . H73C H 0.3378 0.3572 0.9923 0.058 Uiso 1 1 calc R . . C74 C 0.4526(5) 0.3622(3) 1.1220(3) 0.0214(16) Uani 1 1 d . . . C75 C 0.5241(5) 0.3685(3) 1.1770(3) 0.032(2) Uani 1 1 d . . . H75A H 0.5734 0.3896 1.1630 0.048 Uiso 1 1 calc R . . H75B H 0.5482 0.3359 1.1897 0.048 Uiso 1 1 calc R . . H75C H 0.4961 0.3841 1.2133 0.048 Uiso 1 1 calc R . . C76 C 0.3734(5) 0.3311(3) 1.1444(3) 0.031(2) Uani 1 1 d . . . H76A H 0.3533 0.3444 1.1847 0.046 Uiso 1 1 calc R . . H76B H 0.3929 0.2966 1.1505 0.046 Uiso 1 1 calc R . . H76C H 0.3233 0.3325 1.1124 0.046 Uiso 1 1 calc R . . C77 C 0.4201(5) 0.4131(3) 1.1009(4) 0.0307(19) Uani 1 1 d . . . H77A H 0.3771 0.4098 1.0643 0.046 Uiso 1 1 calc R . . H77B H 0.4720 0.4331 1.0887 0.046 Uiso 1 1 calc R . . H77C H 0.3904 0.4295 1.1358 0.046 Uiso 1 1 calc R . . C78 C 0.7899(5) 0.4705(3) 1.0626(4) 0.0264(18) Uani 1 1 d . . . C79 C 0.7138(5) 0.5081(3) 1.0542(4) 0.032(2) Uani 1 1 d . . . H79A H 0.7223 0.5346 1.0859 0.048 Uiso 1 1 calc R . . H79B H 0.6557 0.4916 1.0598 0.048 Uiso 1 1 calc R . . H79C H 0.7144 0.5225 1.0114 0.048 Uiso 1 1 calc R . . C80 C 0.7887(5) 0.4495(3) 1.1308(3) 0.036(2) Uani 1 1 d . . . H80A H 0.8370 0.4248 1.1370 0.053 Uiso 1 1 calc R . . H80B H 0.7301 0.4338 1.1372 0.053 Uiso 1 1 calc R . . H80C H 0.7984 0.4765 1.1615 0.053 Uiso 1 1 calc R . . C81 C 0.8812(5) 0.4960(3) 1.0544(4) 0.036(2) Uani 1 1 d . . . H81A H 0.8823 0.5105 1.0117 0.054 Uiso 1 1 calc R . . H81B H 0.9300 0.4716 1.0599 0.054 Uiso 1 1 calc R . . H81C H 0.8897 0.5223 1.0863 0.054 Uiso 1 1 calc R . . C82 C 0.7958(5) 0.4290(3) 0.9227(3) 0.0286(19) Uani 1 1 d . . . C83 C 0.7622(6) 0.3838(4) 0.8864(4) 0.050(3) Uani 1 1 d . . . H83A H 0.7765 0.3872 0.8416 0.076 Uiso 1 1 calc R . . H83B H 0.6966 0.3809 0.8897 0.076 Uiso 1 1 calc R . . H83C H 0.7918 0.3541 0.9042 0.076 Uiso 1 1 calc R . . C84 C 0.8963(5) 0.4367(4) 0.9124(4) 0.041(2) Uani 1 1 d . . . H84A H 0.9063 0.4375 0.8667 0.061 Uiso 1 1 calc R . . H84B H 0.9311 0.4094 0.9321 0.061 Uiso 1 1 calc R . . H84C H 0.9161 0.4682 0.9318 0.061 Uiso 1 1 calc R . . C85 C 0.7444(5) 0.4749(3) 0.8959(4) 0.036(2) Uani 1 1 d . . . H85A H 0.7665 0.5048 0.9182 0.054 Uiso 1 1 calc R . . H85B H 0.6795 0.4710 0.9022 0.054 Uiso 1 1 calc R . . H85C H 0.7544 0.4781 0.8504 0.054 Uiso 1 1 calc R . . C86 C 0.5583(5) 0.4282(3) 0.9777(4) 0.0286(19) Uani 1 1 d . . . O87 O 0.5162(3) 0.4566(2) 0.9520(3) 0.0390(16) Uani 1 1 d . . . B88 B 0.4334(5) 0.1319(4) 0.8767(5) 0.031(2) Uani 1 1 d . . . F89 F 0.3935(4) 0.1240(2) 0.8175(2) 0.0500(15) Uani 1 1 d . . . F90 F 0.4525(3) 0.08790(19) 0.9074(2) 0.0424(13) Uani 1 1 d . . . F91 F 0.3759(4) 0.1603(3) 0.9120(3) 0.072(2) Uani 1 1 d . . . F92 F 0.5135(4) 0.1564(3) 0.8697(3) 0.085(2) Uani 1 1 d . . . B93 B 1.1213(6) 0.3838(4) 1.0396(4) 0.025(2) Uani 1 1 d . . . F94 F 1.0727(3) 0.4225(2) 1.0690(2) 0.0497(14) Uiso 1 1 d . . . F95 F 1.0852(4) 0.3791(2) 0.9790(3) 0.0594(16) Uiso 1 1 d . . . F96 F 1.1111(4) 0.3406(2) 1.0730(3) 0.0635(17) Uiso 1 1 d . . . F97 F 1.2081(5) 0.3972(3) 1.0392(3) 0.089(2) Uiso 1 1 d . . . B98 B 0.7899(7) 0.3823(4) 0.6997(4) 0.033(2) Uani 1 1 d . . . F99 F 0.8669(5) 0.3628(3) 0.6727(4) 0.104(3) Uiso 1 1 d . . . F100 F 0.7512(4) 0.3453(2) 0.7342(3) 0.0586(16) Uiso 1 1 d . . . F101 F 0.7330(4) 0.3944(2) 0.6500(3) 0.0609(16) Uiso 1 1 d . . . F102 F 0.8130(4) 0.4217(3) 0.7354(3) 0.081(2) Uiso 1 1 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 0.01325(13) 0.01829(17) 0.01805(14) 0.00192(11) 0.00087(9) 0.00213(11) P2 0.0133(8) 0.0172(11) 0.0214(9) -0.0005(8) 0.0017(7) -0.0004(8) P3 0.0162(8) 0.0212(12) 0.0235(10) 0.0059(8) 0.0041(7) -0.0011(8) C4 0.024(4) 0.008(4) 0.040(4) 0.007(3) 0.007(3) 0.006(3) C5 0.024(4) 0.024(5) 0.024(4) 0.007(3) -0.001(3) 0.006(3) C6 0.013(3) 0.022(5) 0.028(4) 0.002(3) 0.001(3) 0.002(3) C7 0.018(3) 0.019(5) 0.033(4) 0.000(3) -0.008(3) 0.003(3) C8 0.022(3) 0.017(4) 0.022(4) 0.002(3) -0.002(3) 0.001(3) C9 0.016(3) 0.029(5) 0.019(4) 0.001(3) -0.001(3) 0.005(3) C10 0.017(3) 0.007(4) 0.024(4) -0.001(3) 0.002(3) 0.001(3) C11 0.016(3) 0.036(5) 0.024(4) 0.009(3) 0.003(3) -0.001(3) C12 0.022(4) 0.017(4) 0.024(4) -0.002(3) -0.001(3) 0.001(3) C13 0.024(4) 0.019(5) 0.037(5) -0.010(4) 0.004(3) 0.001(3) C14 0.028(4) 0.035(6) 0.028(4) 0.003(4) -0.001(3) 0.001(4) C15 0.027(4) 0.031(5) 0.035(5) -0.007(4) 0.002(3) -0.007(4) C16 0.011(3) 0.033(5) 0.021(4) -0.003(3) 0.007(3) 0.001(3) C17 0.031(4) 0.048(6) 0.028(4) -0.022(4) 0.009(3) -0.002(4) C18 0.037(4) 0.024(5) 0.036(5) 0.010(4) 0.014(4) 0.008(4) C19 0.033(4) 0.029(5) 0.034(5) 0.004(4) 0.016(3) 0.010(4) C20 0.026(4) 0.031(5) 0.022(4) 0.005(3) 0.003(3) 0.004(4) C21 0.027(4) 0.046(6) 0.031(5) 0.018(4) 0.006(3) 0.000(4) C22 0.041(5) 0.054(7) 0.034(5) 0.022(4) 0.023(4) 0.007(5) C23 0.049(5) 0.049(7) 0.027(5) -0.005(4) 0.007(4) -0.008(5) C24 0.023(4) 0.029(5) 0.028(4) 0.002(4) 0.000(3) -0.010(4) C25 0.031(4) 0.041(6) 0.044(5) -0.017(4) 0.004(4) -0.003(4) C26 0.039(5) 0.053(7) 0.029(5) -0.001(4) -0.004(4) -0.022(5) C27 0.026(4) 0.026(5) 0.058(6) -0.002(4) -0.003(4) -0.007(4) C28 0.017(3) 0.034(5) 0.021(4) -0.002(3) 0.004(3) -0.004(4) O29 0.029(3) 0.043(4) 0.029(3) 0.014(3) -0.001(2) 0.019(3) Pt30 0.01241(12) 0.01778(17) 0.02177(14) 0.00120(12) -0.00119(9) 0.00049(11) P31 0.0138(8) 0.0196(11) 0.0217(10) 0.0036(8) 0.0020(7) -0.0004(8) P32 0.0127(8) 0.0184(11) 0.0289(10) 0.0011(8) 0.0007(7) -0.0022(8) C33 0.019(4) 0.022(5) 0.094(8) 0.010(5) -0.006(4) -0.003(4) C34 0.023(4) 0.021(5) 0.027(4) 0.003(3) 0.001(3) -0.001(3) C35 0.031(4) 0.024(5) 0.019(4) 0.002(3) -0.001(3) 0.002(4) C36 0.031(4) 0.027(5) 0.024(4) -0.001(3) -0.005(3) 0.004(4) C37 0.016(3) 0.034(5) 0.029(4) 0.008(4) -0.003(3) 0.015(4) C38 0.022(4) 0.024(5) 0.022(4) 0.002(3) -0.001(3) 0.000(3) C39 0.018(3) 0.017(4) 0.020(4) 0.006(3) 0.000(3) 0.014(3) C40 0.011(3) 0.035(5) 0.033(4) 0.010(4) -0.004(3) 0.000(3) C41 0.035(4) 0.020(5) 0.020(4) 0.005(3) 0.008(3) 0.003(4) C42 0.029(4) 0.025(5) 0.051(5) -0.007(4) 0.015(4) 0.001(4) C43 0.038(5) 0.038(6) 0.047(5) 0.003(4) 0.029(4) -0.006(4) C44 0.038(4) 0.042(6) 0.023(4) 0.003(4) 0.002(3) 0.012(4) C45 0.016(3) 0.034(5) 0.023(4) -0.001(3) 0.000(3) -0.005(3) C46 0.022(4) 0.027(5) 0.052(5) -0.006(4) -0.003(3) 0.002(4) C47 0.044(5) 0.040(6) 0.034(5) -0.013(4) 0.006(4) -0.019(5) C48 0.024(4) 0.043(6) 0.036(5) -0.003(4) -0.003(3) -0.001(4) C49 0.026(4) 0.029(5) 0.037(5) -0.009(4) 0.002(3) -0.015(4) C50 0.035(5) 0.051(7) 0.067(7) 0.003(5) -0.016(4) -0.036(5) C51A 0.032(13) 0.038(14) 0.035(11) -0.006(10) -0.021(9) -0.011(11) C52A 0.044(10) 0.038(15) 0.025(10) -0.020(9) 0.016(7) -0.012(10) C53 0.034(4) 0.025(5) 0.024(4) -0.002(3) 0.012(3) -0.006(4) C54 0.030(4) 0.041(6) 0.042(5) 0.008(4) 0.007(4) -0.003(4) C55 0.059(6) 0.103(11) 0.027(5) -0.017(5) 0.008(4) -0.053(7) C56 0.064(6) 0.022(6) 0.075(7) -0.001(5) 0.043(5) -0.004(5) C57 0.015(3) 0.038(6) 0.027(4) 0.005(4) -0.003(3) 0.000(4) O58 0.029(3) 0.024(4) 0.044(4) 0.004(3) -0.010(2) 0.002(3) Pt59 0.01389(13) 0.02181(18) 0.01978(15) 0.00336(11) -0.00006(10) 0.00179(11) P60 0.0144(8) 0.0202(12) 0.0205(9) -0.0012(8) -0.0006(7) 0.0007(8) P61 0.0179(9) 0.0214(12) 0.0246(10) 0.0044(8) 0.0043(7) 0.0009(8) C62 0.011(3) 0.030(5) 0.048(5) 0.013(4) 0.007(3) 0.006(3) C63 0.015(3) 0.026(5) 0.026(4) 0.001(3) 0.003(3) 0.006(3) C64 0.019(3) 0.022(5) 0.030(4) 0.003(3) -0.003(3) 0.010(3) C65 0.024(4) 0.024(5) 0.025(4) 0.003(3) -0.004(3) 0.008(3) C66 0.026(4) 0.026(5) 0.019(4) 0.003(3) 0.003(3) 0.005(4) C67 0.022(3) 0.011(4) 0.023(4) -0.005(3) 0.003(3) -0.003(3) C68 0.014(3) 0.021(4) 0.018(3) 0.002(3) -0.004(2) 0.010(3) C69 0.023(4) 0.036(6) 0.032(4) 0.007(4) -0.004(3) -0.004(4) C70 0.018(3) 0.029(5) 0.026(4) -0.005(3) -0.003(3) 0.000(3) C71 0.029(4) 0.023(5) 0.049(5) -0.011(4) -0.008(4) -0.008(4) C72 0.040(5) 0.086(9) 0.040(6) -0.042(6) 0.008(4) -0.009(6) C73 0.027(4) 0.047(7) 0.040(5) 0.005(4) -0.010(3) -0.009(4) C74 0.027(4) 0.015(4) 0.023(4) 0.003(3) 0.005(3) 0.003(3) C75 0.035(4) 0.035(6) 0.026(4) -0.009(4) 0.006(3) -0.006(4) C76 0.025(4) 0.039(6) 0.029(4) -0.003(4) 0.012(3) -0.005(4) C77 0.040(4) 0.025(5) 0.028(4) 0.003(4) 0.012(3) 0.008(4) C78 0.024(4) 0.028(5) 0.027(4) 0.007(3) 0.001(3) 0.007(4) C79 0.027(4) 0.030(5) 0.039(5) -0.011(4) 0.001(3) 0.006(4) C80 0.040(5) 0.046(6) 0.020(4) 0.001(4) -0.008(3) -0.006(4) C81 0.024(4) 0.033(6) 0.052(6) -0.001(4) 0.003(4) 0.001(4) C82 0.036(4) 0.029(5) 0.021(4) -0.001(3) 0.009(3) -0.012(4) C83 0.067(7) 0.048(7) 0.038(5) -0.010(5) 0.016(5) -0.014(6) C84 0.032(4) 0.052(7) 0.041(5) 0.013(5) 0.022(4) 0.006(5) C85 0.038(5) 0.047(6) 0.024(4) 0.015(4) 0.005(3) 0.001(4) C86 0.023(4) 0.032(5) 0.030(4) 0.008(4) 0.000(3) -0.005(4) O87 0.029(3) 0.039(4) 0.047(4) 0.019(3) -0.010(3) 0.013(3) B88 0.010(4) 0.035(7) 0.047(6) 0.000(5) 0.002(4) 0.005(4) F89 0.060(3) 0.042(4) 0.048(3) 0.001(3) 0.008(3) 0.005(3) F90 0.053(3) 0.025(3) 0.049(3) 0.003(2) 0.006(2) 0.001(3) F91 0.059(4) 0.079(5) 0.077(4) -0.040(4) -0.011(3) 0.034(4) F92 0.046(3) 0.062(5) 0.144(6) 0.060(5) -0.015(4) -0.015(3) B93 0.024(4) 0.018(5) 0.032(5) 0.004(4) 0.005(3) -0.007(4) B98 0.049(6) 0.030(6) 0.019(5) -0.011(4) 0.007(4) -0.005(5) _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 C28 1.926(8) . ? Pt1 C10 2.053(7) . ? Pt1 P2 2.3211(18) . ? Pt1 P3 2.3235(17) . ? P2 C11 1.819(7) . ? P2 C12 1.856(7) . ? P2 C16 1.875(7) . ? P3 C4 1.833(7) . ? P3 C24 1.851(8) . ? P3 C20 1.865(7) . ? C4 C5 1.498(10) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.405(9) . ? C5 C6 1.407(10) . ? C6 C7 1.373(10) . ? C6 H6 0.9500 . ? C7 C8 1.400(9) . ? C7 H7 0.9500 . ? C8 C9 1.391(10) . ? C8 H8 0.9500 . ? C9 C10 1.415(10) . ? C9 C11 1.520(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C15 1.535(10) . ? C12 C14 1.542(10) . ? C12 C13 1.551(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C19 1.521(10) . ? C16 C17 1.538(10) . ? C16 C18 1.559(10) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.527(11) . ? C20 C22 1.536(9) . ? C20 C23 1.536(11) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.536(11) . ? C24 C26 1.540(10) . ? C24 C27 1.544(10) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 O29 1.116(9) . ? Pt30 C57 1.940(8) . ? Pt30 C39 2.061(7) . ? Pt30 P32 2.3153(18) . ? Pt30 P31 2.3239(17) . ? P31 C40 1.828(7) . ? P31 C41 1.864(7) . ? P31 C45 1.872(8) . ? P32 C33 1.820(9) . ? P32 C53 1.855(7) . ? P32 C49 1.869(8) . ? C33 C34 1.513(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.386(10) . ? C34 C39 1.393(10) . ? C35 C36 1.396(9) . ? C35 H35 0.9500 . ? C36 C37 1.390(11) . ? C36 H36 0.9500 . ? C37 C38 1.383(10) . ? C37 H37 0.9500 . ? C38 C39 1.420(9) . ? C38 C40 1.503(10) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C44 1.525(10) . ? C41 C43 1.525(10) . ? C41 C42 1.560(11) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.516(11) . ? C45 C47 1.534(10) . ? C45 C48 1.544(9) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C51B 1.39(3) . ? C49 C50 1.509(11) . ? C49 C52A 1.528(16) . ? C49 C52B 1.62(3) . ? C49 C51A 1.69(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51A H51A 0.9800 . ? C51A H51B 0.9800 . ? C51A H51C 0.9800 . ? C52A H52A 0.9800 . ? C52A H52B 0.9800 . ? C52A H52C 0.9800 . ? C51B H51D 0.9800 . ? C51B H51E 0.9800 . ? C51B H51F 0.9800 . ? C52B H52D 0.9800 . ? C52B H52E 0.9800 . ? C52B H52F 0.9800 . ? C53 C56 1.516(12) . ? C53 C55 1.541(10) . ? C53 C54 1.546(10) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 O58 1.105(9) . ? Pt59 C86 1.934(8) . ? Pt59 C68 2.054(7) . ? Pt59 P60 2.3189(19) . ? Pt59 P61 2.3312(18) . ? P60 C69 1.841(8) . ? P60 C70 1.874(7) . ? P60 C74 1.875(7) . ? P61 C62 1.835(7) . ? P61 C78 1.855(9) . ? P61 C82 1.867(7) . ? C62 C63 1.482(10) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.395(10) . ? C63 C68 1.416(9) . ? C64 C65 1.377(10) . ? C64 H64 0.9500 . ? C65 C66 1.383(9) . ? C65 H65 0.9500 . ? C66 C67 1.407(10) . ? C66 H66 0.9500 . ? C67 C68 1.405(10) . ? C67 C69 1.511(9) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C73 1.524(11) . ? C70 C71 1.534(11) . ? C70 C72 1.543(10) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C77 1.513(10) . ? C74 C76 1.530(10) . ? C74 C75 1.543(10) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C79 1.519(10) . ? C78 C81 1.532(10) . ? C78 C80 1.543(10) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.509(12) . ? C82 C84 1.526(10) . ? C82 C85 1.546(11) . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 O87 1.111(9) . ? B88 F92 1.370(10) . ? B88 F89 1.372(10) . ? B88 F90 1.373(11) . ? B88 F91 1.385(10) . ? B93 F97 1.335(10) . ? B93 F95 1.366(10) . ? B93 F96 1.372(10) . ? B93 F94 1.423(10) . ? B98 F102 1.336(11) . ? B98 F101 1.353(10) . ? B98 F100 1.373(11) . ? B98 F99 1.398(11) . ? 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 C28 Pt1 C10 172.7(3) . . ? C28 Pt1 P2 96.7(2) . . ? C10 Pt1 P2 82.87(19) . . ? C28 Pt1 P3 97.8(2) . . ? C10 Pt1 P3 82.84(19) . . ? P2 Pt1 P3 165.53(7) . . ? C11 P2 C12 106.6(4) . . ? C11 P2 C16 104.4(3) . . ? C12 P2 C16 115.1(3) . . ? C11 P2 Pt1 103.0(2) . . ? C12 P2 Pt1 112.4(2) . . ? C16 P2 Pt1 114.0(3) . . ? C4 P3 C24 107.8(4) . . ? C4 P3 C20 104.9(3) . . ? C24 P3 C20 115.3(4) . . ? C4 P3 Pt1 102.5(2) . . ? C24 P3 Pt1 110.2(2) . . ? C20 P3 Pt1 114.9(2) . . ? C5 C4 P3 109.8(5) . . ? C5 C4 H4A 109.7 . . ? P3 C4 H4A 109.7 . . ? C5 C4 H4B 109.7 . . ? P3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C10 C5 C6 120.0(7) . . ? C10 C5 C4 120.9(6) . . ? C6 C5 C4 119.0(6) . . ? C7 C6 C5 121.0(6) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 120.0(7) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 119.7(7) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 121.2(6) . . ? C8 C9 C11 119.6(7) . . ? C10 C9 C11 119.2(6) . . ? C5 C10 C9 118.1(6) . . ? C5 C10 Pt1 120.7(5) . . ? C9 C10 Pt1 121.1(5) . . ? C9 C11 P2 109.2(5) . . ? C9 C11 H11A 109.8 . . ? P2 C11 H11A 109.8 . . ? C9 C11 H11B 109.8 . . ? P2 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? C15 C12 C14 109.4(6) . . ? C15 C12 C13 110.0(6) . . ? C14 C12 C13 107.1(6) . . ? C15 C12 P2 112.7(5) . . ? C14 C12 P2 111.2(5) . . ? C13 C12 P2 106.2(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C16 C17 108.6(7) . . ? C19 C16 C18 109.7(5) . . ? C17 C16 C18 109.2(6) . . ? C19 C16 P2 111.3(5) . . ? C17 C16 P2 106.8(4) . . ? C18 C16 P2 111.1(6) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 108.8(7) . . ? C21 C20 C23 109.1(7) . . ? C22 C20 C23 108.7(7) . . ? C21 C20 P3 112.9(5) . . ? C22 C20 P3 111.9(5) . . ? C23 C20 P3 105.2(5) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C26 109.0(7) . . ? C25 C24 C27 108.2(7) . . ? C26 C24 C27 108.0(6) . . ? C25 C24 P3 111.4(5) . . ? C26 C24 P3 107.2(6) . . ? C27 C24 P3 112.9(6) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O29 C28 Pt1 175.9(7) . . ? C57 Pt30 C39 177.0(3) . . ? C57 Pt30 P32 96.3(2) . . ? C39 Pt30 P32 83.6(2) . . ? C57 Pt30 P31 96.7(2) . . ? C39 Pt30 P31 83.3(2) . . ? P32 Pt30 P31 166.68(7) . . ? C40 P31 C41 107.7(4) . . ? C40 P31 C45 104.7(3) . . ? C41 P31 C45 114.9(4) . . ? C40 P31 Pt30 103.9(2) . . ? C41 P31 Pt30 110.3(3) . . ? C45 P31 Pt30 114.4(2) . . ? C33 P32 C53 106.8(4) . . ? C33 P32 C49 103.5(4) . . ? C53 P32 C49 116.7(4) . . ? C33 P32 Pt30 103.5(3) . . ? C53 P32 Pt30 113.1(3) . . ? C49 P32 Pt30 111.8(3) . . ? C34 C33 P32 111.1(6) . . ? C34 C33 H33A 109.4 . . ? P32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? P32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C39 121.3(6) . . ? C35 C34 C33 118.0(7) . . ? C39 C34 C33 120.7(7) . . ? C34 C35 C36 119.8(8) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C37 C36 C35 119.8(7) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C38 C37 C36 120.7(7) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C39 120.1(7) . . ? C37 C38 C40 118.9(6) . . ? C39 C38 C40 121.0(7) . . ? C34 C39 C38 118.4(7) . . ? C34 C39 Pt30 121.0(5) . . ? C38 C39 Pt30 120.5(6) . . ? C38 C40 P31 110.0(5) . . ? C38 C40 H40A 109.7 . . ? P31 C40 H40A 109.7 . . ? C38 C40 H40B 109.7 . . ? P31 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C44 C41 C43 109.0(7) . . ? C44 C41 C42 107.9(7) . . ? C43 C41 C42 109.0(6) . . ? C44 C41 P31 111.6(5) . . ? C43 C41 P31 113.4(5) . . ? C42 C41 P31 105.9(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C47 108.8(7) . . ? C46 C45 C48 109.6(7) . . ? C47 C45 C48 108.9(6) . . ? C46 C45 P31 111.6(5) . . ? C47 C45 P31 106.0(6) . . ? C48 C45 P31 111.7(5) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C51B C49 C50 113.6(14) . . ? C51B C49 C52A 85(2) . . ? C50 C49 C52A 116.8(10) . . ? C51B C49 C52B 114(2) . . ? C50 C49 C52B 98.6(14) . . ? C52A C49 C52B 29.6(10) . . ? C51B C49 C51A 20.7(13) . . ? C50 C49 C51A 102.2(10) . . ? C52A C49 C51A 106(2) . . ? C52B C49 C51A 135(2) . . ? C51B C49 P32 114.6(13) . . ? C50 C49 P32 114.0(6) . . ? C52A C49 P32 109.7(8) . . ? C52B C49 P32 100.0(10) . . ? C51A C49 P32 107.4(9) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51A H51A 109.5 . . ? C49 C51A H51B 109.5 . . ? C49 C51A H51C 109.5 . . ? C49 C52A H52A 109.5 . . ? C49 C52A H52B 109.5 . . ? C49 C52A H52C 109.5 . . ? C49 C51B H51D 109.5 . . ? C49 C51B H51E 109.5 . . ? H51D C51B H51E 109.5 . . ? C49 C51B H51F 109.5 . . ? H51D C51B H51F 109.5 . . ? H51E C51B H51F 109.5 . . ? C49 C52B H52D 109.5 . . ? C49 C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? C49 C52B H52F 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? C56 C53 C55 109.5(8) . . ? C56 C53 C54 109.5(7) . . ? C55 C53 C54 108.7(7) . . ? C56 C53 P32 111.6(5) . . ? C55 C53 P32 104.7(5) . . ? C54 C53 P32 112.6(6) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O58 C57 Pt30 176.8(8) . . ? C86 Pt59 C68 179.1(3) . . ? C86 Pt59 P60 96.7(2) . . ? C68 Pt59 P60 83.7(2) . . ? C86 Pt59 P61 96.7(2) . . ? C68 Pt59 P61 82.9(2) . . ? P60 Pt59 P61 166.07(7) . . ? C69 P60 C70 104.3(4) . . ? C69 P60 C74 106.2(3) . . ? C70 P60 C74 114.3(3) . . ? C69 P60 Pt59 103.4(2) . . ? C70 P60 Pt59 115.5(2) . . ? C74 P60 Pt59 111.9(3) . . ? C62 P61 C78 105.8(4) . . ? C62 P61 C82 105.1(4) . . ? C78 P61 C82 116.0(4) . . ? C62 P61 Pt59 102.8(2) . . ? C78 P61 Pt59 111.0(2) . . ? C82 P61 Pt59 114.6(2) . . ? C63 C62 P61 109.8(5) . . ? C63 C62 H62A 109.7 . . ? P61 C62 H62A 109.7 . . ? C63 C62 H62B 109.7 . . ? P61 C62 H62B 109.7 . . ? H62A C62 H62B 108.2 . . ? C64 C63 C68 118.8(7) . . ? C64 C63 C62 120.2(6) . . ? C68 C63 C62 120.7(6) . . ? C65 C64 C63 122.2(7) . . ? C65 C64 H64 118.9 . . ? C63 C64 H64 118.9 . . ? C64 C65 C66 119.8(7) . . ? C64 C65 H65 120.1 . . ? C66 C65 H65 120.1 . . ? C65 C66 C67 119.5(7) . . ? C65 C66 H66 120.2 . . ? C67 C66 H66 120.2 . . ? C68 C67 C66 121.0(6) . . ? C68 C67 C69 121.2(6) . . ? C66 C67 C69 117.6(7) . . ? C67 C68 C63 118.6(6) . . ? C67 C68 Pt59 120.6(5) . . ? C63 C68 Pt59 120.7(6) . . ? C67 C69 P60 109.5(5) . . ? C67 C69 H69A 109.8 . . ? P60 C69 H69A 109.8 . . ? C67 C69 H69B 109.8 . . ? P60 C69 H69B 109.8 . . ? H69A C69 H69B 108.2 . . ? C73 C70 C71 109.7(6) . . ? C73 C70 C72 108.4(7) . . ? C71 C70 C72 109.5(7) . . ? C73 C70 P60 111.7(6) . . ? C71 C70 P60 111.9(5) . . ? C72 C70 P60 105.5(5) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C77 C74 C76 110.4(6) . . ? C77 C74 C75 108.5(7) . . ? C76 C74 C75 109.7(6) . . ? C77 C74 P60 110.4(5) . . ? C76 C74 P60 112.6(5) . . ? C75 C74 P60 105.0(5) . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C74 C76 H76A 109.5 . . ? C74 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C74 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C74 C77 H77A 109.5 . . ? C74 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C74 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C79 C78 C81 109.8(7) . . ? C79 C78 C80 108.3(6) . . ? C81 C78 C80 108.5(6) . . ? C79 C78 P61 110.7(5) . . ? C81 C78 P61 112.5(5) . . ? C80 C78 P61 106.9(6) . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C78 C80 H80A 109.5 . . ? C78 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C78 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C78 C81 H81A 109.5 . . ? C78 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C78 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C84 109.8(7) . . ? C83 C82 C85 108.3(7) . . ? C84 C82 C85 107.8(7) . . ? C83 C82 P61 106.0(6) . . ? C84 C82 P61 113.1(5) . . ? C85 C82 P61 111.8(5) . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C82 C85 H85A 109.5 . . ? C82 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C82 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? O87 C86 Pt59 179.3(8) . . ? F92 B88 F89 108.4(8) . . ? F92 B88 F90 107.9(7) . . ? F89 B88 F90 111.4(8) . . ? F92 B88 F91 110.3(9) . . ? F89 B88 F91 108.9(7) . . ? F90 B88 F91 110.0(8) . . ? F97 B93 F95 110.7(7) . . ? F97 B93 F96 111.1(8) . . ? F95 B93 F96 110.6(8) . . ? F97 B93 F94 108.1(8) . . ? F95 B93 F94 106.9(7) . . ? F96 B93 F94 109.3(7) . . ? F102 B98 F101 112.3(9) . . ? F102 B98 F100 112.4(7) . . ? F101 B98 F100 108.9(8) . . ? F102 B98 F99 109.6(8) . . ? F101 B98 F99 105.4(7) . . ? F100 B98 F99 108.0(9) . . ? 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 C28 Pt1 P2 C11 173.2(4) . . . . ? C10 Pt1 P2 C11 -14.1(3) . . . . ? P3 Pt1 P2 C11 -4.9(4) . . . . ? C28 Pt1 P2 C12 -72.5(3) . . . . ? C10 Pt1 P2 C12 100.2(3) . . . . ? P3 Pt1 P2 C12 109.3(4) . . . . ? C28 Pt1 P2 C16 60.8(3) . . . . ? C10 Pt1 P2 C16 -126.5(3) . . . . ? P3 Pt1 P2 C16 -117.4(3) . . . . ? C28 Pt1 P3 C4 158.1(3) . . . . ? C10 Pt1 P3 C4 -14.6(3) . . . . ? P2 Pt1 P3 C4 -23.7(4) . . . . ? C28 Pt1 P3 C24 -87.4(4) . . . . ? C10 Pt1 P3 C24 99.9(3) . . . . ? P2 Pt1 P3 C24 90.8(4) . . . . ? C28 Pt1 P3 C20 44.9(4) . . . . ? C10 Pt1 P3 C20 -127.8(4) . . . . ? P2 Pt1 P3 C20 -136.9(4) . . . . ? C24 P3 C4 C5 -98.8(6) . . . . ? C20 P3 C4 C5 137.9(5) . . . . ? Pt1 P3 C4 C5 17.5(6) . . . . ? P3 C4 C5 C10 -11.7(9) . . . . ? P3 C4 C5 C6 172.4(6) . . . . ? C10 C5 C6 C7 0.8(11) . . . . ? C4 C5 C6 C7 176.8(7) . . . . ? C5 C6 C7 C8 0.0(11) . . . . ? C6 C7 C8 C9 0.9(11) . . . . ? C7 C8 C9 C10 -2.6(11) . . . . ? C7 C8 C9 C11 175.6(6) . . . . ? C6 C5 C10 C9 -2.5(11) . . . . ? C4 C5 C10 C9 -178.3(7) . . . . ? C6 C5 C10 Pt1 173.6(5) . . . . ? C4 C5 C10 Pt1 -2.3(10) . . . . ? C8 C9 C10 C5 3.4(11) . . . . ? C11 C9 C10 C5 -174.9(6) . . . . ? C8 C9 C10 Pt1 -172.6(5) . . . . ? C11 C9 C10 Pt1 9.1(9) . . . . ? P2 Pt1 C10 C5 -170.9(6) . . . . ? P3 Pt1 C10 C5 11.4(6) . . . . ? P2 Pt1 C10 C9 5.0(6) . . . . ? P3 Pt1 C10 C9 -172.7(6) . . . . ? C8 C9 C11 P2 160.3(6) . . . . ? C10 C9 C11 P2 -21.4(9) . . . . ? C12 P2 C11 C9 -96.6(6) . . . . ? C16 P2 C11 C9 141.1(5) . . . . ? Pt1 P2 C11 C9 21.8(6) . . . . ? C11 P2 C12 C15 -67.5(6) . . . . ? C16 P2 C12 C15 47.7(7) . . . . ? Pt1 P2 C12 C15 -179.6(5) . . . . ? C11 P2 C12 C14 169.3(5) . . . . ? C16 P2 C12 C14 -75.5(6) . . . . ? Pt1 P2 C12 C14 57.2(5) . . . . ? C11 P2 C12 C13 53.0(6) . . . . ? C16 P2 C12 C13 168.3(5) . . . . ? Pt1 P2 C12 C13 -59.0(5) . . . . ? C11 P2 C16 C19 173.2(5) . . . . ? C12 P2 C16 C19 56.8(6) . . . . ? Pt1 P2 C16 C19 -75.2(5) . . . . ? C11 P2 C16 C17 -68.3(6) . . . . ? C12 P2 C16 C17 175.2(5) . . . . ? Pt1 P2 C16 C17 43.3(6) . . . . ? C11 P2 C16 C18 50.7(6) . . . . ? C12 P2 C16 C18 -65.8(6) . . . . ? Pt1 P2 C16 C18 162.3(4) . . . . ? C4 P3 C20 C21 167.9(5) . . . . ? C24 P3 C20 C21 49.5(6) . . . . ? Pt1 P3 C20 C21 -80.3(6) . . . . ? C4 P3 C20 C22 44.8(7) . . . . ? C24 P3 C20 C22 -73.6(7) . . . . ? Pt1 P3 C20 C22 156.6(5) . . . . ? C4 P3 C20 C23 -73.2(6) . . . . ? C24 P3 C20 C23 168.4(5) . . . . ? Pt1 P3 C20 C23 38.6(6) . . . . ? C4 P3 C24 C25 169.6(5) . . . . ? C20 P3 C24 C25 -73.6(6) . . . . ? Pt1 P3 C24 C25 58.5(6) . . . . ? C4 P3 C24 C26 50.5(6) . . . . ? C20 P3 C24 C26 167.2(5) . . . . ? Pt1 P3 C24 C26 -60.7(5) . . . . ? C4 P3 C24 C27 -68.4(6) . . . . ? C20 P3 C24 C27 48.4(7) . . . . ? Pt1 P3 C24 C27 -179.5(5) . . . . ? C57 Pt30 P31 C40 176.7(4) . . . . ? C39 Pt30 P31 C40 -6.3(3) . . . . ? P32 Pt30 P31 C40 -17.2(4) . . . . ? C57 Pt30 P31 C41 -68.2(4) . . . . ? C39 Pt30 P31 C41 108.8(3) . . . . ? P32 Pt30 P31 C41 97.9(4) . . . . ? C57 Pt30 P31 C45 63.2(4) . . . . ? C39 Pt30 P31 C45 -119.8(3) . . . . ? P32 Pt30 P31 C45 -130.7(4) . . . . ? C57 Pt30 P32 C33 175.5(4) . . . . ? C39 Pt30 P32 C33 -1.5(4) . . . . ? P31 Pt30 P32 C33 9.4(5) . . . . ? C57 Pt30 P32 C53 -69.3(4) . . . . ? C39 Pt30 P32 C53 113.7(3) . . . . ? P31 Pt30 P32 C53 124.6(4) . . . . ? C57 Pt30 P32 C49 64.8(4) . . . . ? C39 Pt30 P32 C49 -112.2(4) . . . . ? P31 Pt30 P32 C49 -101.3(4) . . . . ? C53 P32 C33 C34 -117.7(7) . . . . ? C49 P32 C33 C34 118.6(6) . . . . ? Pt30 P32 C33 C34 1.8(7) . . . . ? P32 C33 C34 C35 -179.4(6) . . . . ? P32 C33 C34 C39 -1.3(11) . . . . ? C39 C34 C35 C36 -1.8(11) . . . . ? C33 C34 C35 C36 176.3(7) . . . . ? C34 C35 C36 C37 1.1(11) . . . . ? C35 C36 C37 C38 0.5(11) . . . . ? C36 C37 C38 C39 -1.6(11) . . . . ? C36 C37 C38 C40 175.0(7) . . . . ? C35 C34 C39 C38 0.7(11) . . . . ? C33 C34 C39 C38 -177.3(7) . . . . ? C35 C34 C39 Pt30 177.9(5) . . . . ? C33 C34 C39 Pt30 -0.1(10) . . . . ? C37 C38 C39 C34 0.9(11) . . . . ? C40 C38 C39 C34 -175.6(7) . . . . ? C37 C38 C39 Pt30 -176.2(6) . . . . ? C40 C38 C39 Pt30 7.3(9) . . . . ? P32 Pt30 C39 C34 1.1(6) . . . . ? P31 Pt30 C39 C34 -176.4(6) . . . . ? P32 Pt30 C39 C38 178.2(6) . . . . ? P31 Pt30 C39 C38 0.7(5) . . . . ? C37 C38 C40 P31 170.9(6) . . . . ? C39 C38 C40 P31 -12.5(9) . . . . ? C41 P31 C40 C38 -105.9(6) . . . . ? C45 P31 C40 C38 131.4(5) . . . . ? Pt30 P31 C40 C38 11.1(6) . . . . ? C40 P31 C41 C44 164.1(6) . . . . ? C45 P31 C41 C44 -79.6(6) . . . . ? Pt30 P31 C41 C44 51.4(6) . . . . ? C40 P31 C41 C43 -72.4(7) . . . . ? C45 P31 C41 C43 43.9(7) . . . . ? Pt30 P31 C41 C43 174.9(5) . . . . ? C40 P31 C41 C42 47.0(6) . . . . ? C45 P31 C41 C42 163.3(5) . . . . ? Pt30 P31 C41 C42 -65.7(5) . . . . ? C40 P31 C45 C46 172.9(5) . . . . ? C41 P31 C45 C46 55.0(6) . . . . ? Pt30 P31 C45 C46 -74.1(5) . . . . ? C40 P31 C45 C47 -68.8(5) . . . . ? C41 P31 C45 C47 173.3(5) . . . . ? Pt30 P31 C45 C47 44.2(6) . . . . ? C40 P31 C45 C48 49.7(6) . . . . ? C41 P31 C45 C48 -68.2(6) . . . . ? Pt30 P31 C45 C48 162.8(4) . . . . ? C33 P32 C49 C51B -170.8(16) . . . . ? C53 P32 C49 C51B 72.2(16) . . . . ? Pt30 P32 C49 C51B -60.1(16) . . . . ? C33 P32 C49 C50 56.0(7) . . . . ? C53 P32 C49 C50 -61.0(8) . . . . ? Pt30 P32 C49 C50 166.7(6) . . . . ? C33 P32 C49 C52A -77.2(14) . . . . ? C53 P32 C49 C52A 165.8(13) . . . . ? Pt30 P32 C49 C52A 33.5(14) . . . . ? C33 P32 C49 C52B -48.3(15) . . . . ? C53 P32 C49 C52B -165.2(15) . . . . ? Pt30 P32 C49 C52B 62.5(15) . . . . ? C33 P32 C49 C51A 168.4(11) . . . . ? C53 P32 C49 C51A 51.4(12) . . . . ? Pt30 P32 C49 C51A -80.9(11) . . . . ? C33 P32 C53 C56 177.5(6) . . . . ? C49 P32 C53 C56 -67.3(7) . . . . ? Pt30 P32 C53 C56 64.4(6) . . . . ? C33 P32 C53 C55 59.1(7) . . . . ? C49 P32 C53 C55 174.3(6) . . . . ? Pt30 P32 C53 C55 -54.0(7) . . . . ? C33 P32 C53 C54 -58.8(6) . . . . ? C49 P32 C53 C54 56.3(7) . . . . ? Pt30 P32 C53 C54 -172.0(5) . . . . ? C86 Pt59 P60 C69 173.2(4) . . . . ? C68 Pt59 P60 C69 -6.0(3) . . . . ? P61 Pt59 P60 C69 -22.7(4) . . . . ? C86 Pt59 P60 C70 60.0(4) . . . . ? C68 Pt59 P60 C70 -119.2(3) . . . . ? P61 Pt59 P60 C70 -135.9(4) . . . . ? C86 Pt59 P60 C74 -73.0(3) . . . . ? C68 Pt59 P60 C74 107.9(3) . . . . ? P61 Pt59 P60 C74 91.1(4) . . . . ? C86 Pt59 P61 C62 -169.4(4) . . . . ? C68 Pt59 P61 C62 9.7(3) . . . . ? P60 Pt59 P61 C62 26.5(4) . . . . ? C86 Pt59 P61 C78 77.9(4) . . . . ? C68 Pt59 P61 C78 -103.0(3) . . . . ? P60 Pt59 P61 C78 -86.2(4) . . . . ? C86 Pt59 P61 C82 -55.9(4) . . . . ? C68 Pt59 P61 C82 123.2(4) . . . . ? P60 Pt59 P61 C82 140.0(4) . . . . ? C78 P61 C62 C63 99.5(6) . . . . ? C82 P61 C62 C63 -137.3(6) . . . . ? Pt59 P61 C62 C63 -17.0(6) . . . . ? P61 C62 C63 C64 -166.6(6) . . . . ? P61 C62 C63 C68 18.9(10) . . . . ? C68 C63 C64 C65 0.2(12) . . . . ? C62 C63 C64 C65 -174.4(8) . . . . ? C63 C64 C65 C66 2.1(12) . . . . ? C64 C65 C66 C67 -2.6(11) . . . . ? C65 C66 C67 C68 0.8(11) . . . . ? C65 C66 C67 C69 175.7(7) . . . . ? C66 C67 C68 C63 1.5(11) . . . . ? C69 C67 C68 C63 -173.3(7) . . . . ? C66 C67 C68 Pt59 -175.3(5) . . . . ? C69 C67 C68 Pt59 9.9(10) . . . . ? C64 C63 C68 C67 -2.0(11) . . . . ? C62 C63 C68 C67 172.6(7) . . . . ? C64 C63 C68 Pt59 174.8(6) . . . . ? C62 C63 C68 Pt59 -10.6(10) . . . . ? P60 Pt59 C68 C67 -0.8(5) . . . . ? P61 Pt59 C68 C67 175.2(6) . . . . ? P60 Pt59 C68 C63 -177.6(6) . . . . ? P61 Pt59 C68 C63 -1.6(5) . . . . ? C68 C67 C69 P60 -14.5(9) . . . . ? C66 C67 C69 P60 170.5(5) . . . . ? C70 P60 C69 C67 132.8(5) . . . . ? C74 P60 C69 C67 -106.2(5) . . . . ? Pt59 P60 C69 C67 11.7(6) . . . . ? C69 P60 C70 C73 174.1(5) . . . . ? C74 P60 C70 C73 58.7(6) . . . . ? Pt59 P60 C70 C73 -73.2(5) . . . . ? C69 P60 C70 C71 50.7(6) . . . . ? C74 P60 C70 C71 -64.8(6) . . . . ? Pt59 P60 C70 C71 163.4(5) . . . . ? C69 P60 C70 C72 -68.3(7) . . . . ? C74 P60 C70 C72 176.3(6) . . . . ? Pt59 P60 C70 C72 44.4(7) . . . . ? C69 P60 C74 C77 167.3(5) . . . . ? C70 P60 C74 C77 -78.4(6) . . . . ? Pt59 P60 C74 C77 55.2(6) . . . . ? C69 P60 C74 C76 -68.8(6) . . . . ? C70 P60 C74 C76 45.5(6) . . . . ? Pt59 P60 C74 C76 179.1(4) . . . . ? C69 P60 C74 C75 50.5(6) . . . . ? C70 P60 C74 C75 164.9(5) . . . . ? Pt59 P60 C74 C75 -61.5(5) . . . . ? C62 P61 C78 C79 -168.1(5) . . . . ? C82 P61 C78 C79 75.9(6) . . . . ? Pt59 P61 C78 C79 -57.3(6) . . . . ? C62 P61 C78 C81 68.6(6) . . . . ? C82 P61 C78 C81 -47.5(7) . . . . ? Pt59 P61 C78 C81 179.4(5) . . . . ? C62 P61 C78 C80 -50.3(6) . . . . ? C82 P61 C78 C80 -166.4(5) . . . . ? Pt59 P61 C78 C80 60.5(5) . . . . ? C62 P61 C82 C83 72.2(7) . . . . ? C78 P61 C82 C83 -171.4(6) . . . . ? Pt59 P61 C82 C83 -39.9(7) . . . . ? C62 P61 C82 C84 -48.1(7) . . . . ? C78 P61 C82 C84 68.3(7) . . . . ? Pt59 P61 C82 C84 -160.2(5) . . . . ? C62 P61 C82 C85 -170.0(6) . . . . ? C78 P61 C82 C85 -53.5(7) . . . . ? Pt59 P61 C82 C85 77.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 4.097 _refine_diff_density_min -3.182 _refine_diff_density_rms 0.250