Supplementary Material (ESI) for J. Chem. Soc., Dalton Trans. This journal is (C) The Royal Society of Chemistry 2002 data_global #====================================== _journal_coden_Cambridge 186 loop_ _publ_author_name 'Gregory J. Grant' 'David F. Galas' 'Ivan M. Poullaos' 'Shawn M. Carter' 'Donald G. VanDerveer' _publ_contact_author_name 'Gregory J Grant' _publ_contact_author_address ; Department of Chemistry The University of Tennessee at Chattanooga 615 McCallie Avenue Chattanooga TN 37403-2598 UNITED STATES OF AMERICA ; _publ_contact_author_email '?' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthetic and Structural Studies of Heteroleptic Platinum(II) Complexes Containing Crown Trithioether and Diphosphine Ligands1 ; _publ_section_references ; Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. and White, P.S. (1989) J. Appl. Cryst., 22, 384-387. Flack, H., (1983) Acta Cryst., A39, 876-881. International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Larson, A.C., (1970) p.293, Crystallographic Computing, Munksgaard, Copenhagen. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. Rogers, D., (1981) Acta Cryst., A37, 734-741. ; data_compound1 _database_code_CSD 180861 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common ? _chemical_formula_moiety 'Pt C32 H36 P4 S3 F11.95 ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Pt C32 H36 P4 S3 F11.95 ' _chemical_formula_weight 1062.82 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt ? -5.233 6.925 'International Tables Vol. IV Table 2.2B' C ? 0.017 0.009 'International Tables Vol. IV Table 2.2B' H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B' P ? 0.283 0.434 'International Tables Vol. IV Table 2.2B' S ? 0.319 0.557 'International Tables Vol. IV Table 2.2B' Cl ? 0.348 0.702 'International Tables Vol. IV Table 2.2B' F ? 0.069 0.053 'International Tables Vol. IV Table 2.2B' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,1/2+y,1/2-z x,1/2-y,1/2+z _cell_length_a 11.1790(21) _cell_length_b 17.711(2) _cell_length_c 20.511(3) _cell_angle_alpha 90.0 _cell_angle_beta 103.480(*) _cell_angle_gamma 90.0 _cell_volume 3949.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.30 _cell_measurement_theta_max 32.71 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_method ? _exptl_crystal_F_000 2080.63 _exptl_absorpt_coefficient_mu 10.49 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0431 _exptl_absorpt_correction_T_max 0.1523 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54056 _diffrn_radiation_type 'Copper K\a' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius CAD-4' _diffrn_measurement_method 'Theta/2theta scan b/P/b ' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 9228 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 73.78 _diffrn_reflns_reduction_process ? _reflns_number_total 7993 _reflns_number_observed 6528 _reflns_observed_criterion 'Inet > 2.5\s(Inet)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'NRCVAX SOLVER' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_molecular_graphics 'NRCVAX' _computing_publication_material 'NRCVAX TABLES Jan 94 Version' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; ? #Insert any special details here. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 1/(\s^2^(F)+0.0003F^2^) _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Larson _refine_ls_extinction_coef 4232( 363) _refine_ls_number_reflns 6528 _refine_ls_number_parameters 506 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.040 _refine_ls_R_factor_obs 0.040 _refine_ls_wR_factor_all 0.053 _refine_ls_wR_factor_obs 0.053 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.91 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean ? _refine_diff_density_max 15.10 _refine_diff_density_min -19.50 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Pt 0.381025(21) 0.205965(12) 0.212953(11) 0.04336(13) Uij ? . Pt S1 0.43305(18) 0.22844(10) 0.09045(9) 0.0669(9) Uij ? . S C2 0.4616(7) 0.1309(4) 0.0685(4) 0.071(4) Uij ? . C C3 0.5184(7) 0.0829(4) 0.1294(4) 0.067(4) Uij ? . C S4 0.43359(14) 0.07919(8) 0.19565(8) 0.0528(7) Uij ? . S C5 0.2894(6) 0.0374(4) 0.1506(3) 0.062(4) Uij ? . C C6 0.1759(6) 0.0792(4) 0.1605(4) 0.064(4) Uij ? . C S7 0.18035(14) 0.18029(9) 0.14866(8) 0.0551(7) Uij ? . S C8 0.1807(7) 0.1894(4) 0.0597(3) 0.067(4) Uij ? . C C9 0.2759(8) 0.2418(5) 0.0455(4) 0.071(4) Uij ? . C P1 0.32429(15) 0.31805(8) 0.24842(8) 0.0520(8) Uij ? . P P2 0.55815(14) 0.22601(8) 0.29020(7) 0.0475(7) Uij ? . P C10 0.4569(7) 0.3624(4) 0.3065(4) 0.063(4) Uij ? . C C11 0.5783(6) 0.3281(3) 0.2985(4) 0.061(3) Uij ? . C C12 0.2718(7) 0.3804(4) 0.1777(4) 0.066(4) Uij ? . C C13 0.3581(8) 0.4187(4) 0.1502(4) 0.074(5) Uij ? . C C14 0.3191(10) 0.4593(5) 0.0919(5) 0.089(6) Uij ? . C C15 0.1953(11) 0.4617(5) 0.0604(5) 0.101(7) Uij ? . C C16 0.1085(9) 0.4239(6) 0.0869(4) 0.094(6) Uij ? . C C17 0.1480(8) 0.3834(5) 0.1459(4) 0.078(5) Uij ? . C C18 0.2056(6) 0.3156(4) 0.2952(3) 0.058(3) Uij ? . C C19 0.1673(9) 0.3834(5) 0.3184(5) 0.086(5) Uij ? . C C20 0.0812(10) 0.3821(7) 0.3574(5) 0.101(7) Uij ? . C C21 0.0360(9) 0.3144(7) 0.3734(5) 0.096(7) Uij ? . C C22 0.0747(9) 0.2465(6) 0.3524(4) 0.093(6) Uij ? . C C23 0.1596(8) 0.2481(5) 0.3124(4) 0.072(4) Uij ? . C C24 0.5554(6) 0.1903(4) 0.3724(3) 0.057(3) Uij ? . C C25 0.4604(7) 0.1454(4) 0.3813(3) 0.065(4) Uij ? . C C26 0.4612(8) 0.1170(5) 0.4445(4) 0.080(5) Uij ? . C C27 0.5558(9) 0.1347(5) 0.4979(4) 0.083(6) Uij ? . C C28 0.6496(10) 0.1767(6) 0.4896(4) 0.091(6) Uij ? . C C29 0.6526(8) 0.2071(5) 0.4269(4) 0.074(4) Uij ? . C C30 0.6935(6) 0.1873(3) 0.2693(3) 0.053(3) Uij ? . C C31 0.7408(7) 0.1192(4) 0.2969(4) 0.064(4) Uij ? . C C32 0.8375(8) 0.0866(5) 0.2756(5) 0.081(5) Uij ? . C C33 0.8880(7) 0.1207(6) 0.2288(5) 0.085(5) Uij ? . C C34 0.8410(8) 0.1893(5) 0.2020(4) 0.079(5) Uij ? . C C35 0.7430(7) 0.2231(4) 0.2206(4) 0.065(4) Uij ? . C P3 0.20898(21) 0.95415(14) 0.33008(11) 0.0783(12) Uij ? . P F1 0.1945(7) 0.9252(4) 0.2541(3) 0.129(5) Uij ? . F F2 0.2319(9) 0.9789(4) 0.4032(3) 0.160(7) Uij ? . F F3 0.1596(8) 0.8771(4) 0.3498(4) 0.149(6) Uij ? . F F4 0.0775(7) 0.9811(5) 0.3059(5) 0.185(8) Uij ? . F F5 0.3352(7) 0.9136(7) 0.3455(4) 0.203(9) Uij ? . F F6 0.2599(10) 1.0288(5) 0.3100(3) 0.212(8) Uij ? . F P4 0.79525(20) 0.08211(13) 0.01396(10) 0.0726(11) Uij ? . P F7 0.8350(12) 0.0014(5) -0.0032(4) 0.162(7) Uij ? . F F8 0.7345(7) 0.1512(5) 0.0405(4) 0.147(6) Uij ? . F F9 0.9179(7) 0.0888(7) 0.0613(5) 0.185(8) Uij ? . F F10 0.6572(10) 0.0559(10) -0.0235(9) 0.166(12) Uij ? . F F11 0.1876(16) 0.8897(9) 0.0529(6) 0.130(10) Uij ? . F F12 0.7674(18) 0.0551(9) 0.0815(6) 0.159(14) Uij ? . F F13 0.1384(18) 0.8339(10) -0.0057(12) 0.125(14) Uij ? . F F14 0.7311(21) 0.0230(17) 0.039(3) 0.24(4) Uij ? . F F15 0.3066(24) 0.8978(12) 0.0481(9) 0.114(14) Uij ? . F F16 0.1268(23) 0.9385(19) 0.0434(17) 0.135(21) Uij ? . F H2a 0.521 0.130 0.036 0.0849 Uiso ? . H H2b 0.380 0.105 0.044 0.0849 Uiso ? . H H3a 0.532 0.028 0.115 0.0774 Uiso ? . H H3b 0.606 0.106 0.151 0.0774 Uiso ? . H H5a 0.287 -0.019 0.165 0.0686 Uiso ? . H H5b 0.287 0.038 0.099 0.0686 Uiso ? . H H6a 0.098 0.057 0.128 0.0737 Uiso ? . H H6b 0.168 0.068 0.210 0.0737 Uiso ? . H H8a 0.094 0.206 0.033 0.0752 Uiso ? . H H8b 0.199 0.136 0.042 0.0752 Uiso ? . H H9a 0.271 0.239 -0.006 0.0796 Uiso ? . H H9b 0.248 0.296 0.056 0.0796 Uiso ? . H H10a 0.449 0.353 0.356 0.0705 Uiso ? . H H10b 0.456 0.419 0.298 0.0705 Uiso ? . H H11a 0.602 0.350 0.257 0.0721 Uiso ? . H H11b 0.649 0.341 0.340 0.0721 Uiso ? . H H13 0.453 0.417 0.174 0.0876 Uiso ? . H H14 0.380 0.489 0.071 0.1070 Uiso ? . H H15 0.167 0.491 0.015 0.1089 Uiso ? . H H16 0.016 0.429 0.064 0.1011 Uiso ? . H H17 0.081 0.355 0.168 0.0858 Uiso ? . H H19 0.200 0.435 0.305 0.0936 Uiso ? . H H20 0.054 0.432 0.377 0.1092 Uiso ? . H H21 -0.032 0.313 0.402 0.1032 Uiso ? . H H22 0.039 0.195 0.364 0.1082 Uiso ? . H H23 0.188 0.197 0.295 0.0803 Uiso ? . H H25 0.386 0.133 0.340 0.0754 Uiso ? . H H26 0.389 0.082 0.452 0.0873 Uiso ? . H H27 0.552 0.113 0.544 0.0897 Uiso ? . H H28 0.721 0.188 0.532 0.0967 Uiso ? . H H29 0.728 0.241 0.421 0.0811 Uiso ? . H H31 0.706 0.093 0.334 0.0717 Uiso ? . H H32 0.875 0.035 0.297 0.0856 Uiso ? . H H33 0.960 0.096 0.213 0.0892 Uiso ? . H H34 0.883 0.216 0.167 0.0890 Uiso ? . H H35 0.705 0.273 0.199 0.0743 Uiso ? . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Pt 0.05079(14) 0.03716(13) 0.04136(13) 0.00172(9) 0.00920(9) -0.00105(9) Pt S1 0.0804(11) 0.0633(9) 0.0615(9) -0.0078(8) 0.0258(8) 0.0072(8) S C2 0.082(5) 0.075(5) 0.065(4) -0.001(4) 0.038(4) -0.010(4) C C3 0.076(4) 0.065(4) 0.067(4) 0.004(3) 0.028(3) -0.012(3) C S4 0.0628(8) 0.0415(6) 0.0535(7) 0.0043(6) 0.0124(6) -0.0039(6) S C5 0.073(4) 0.048(3) 0.063(4) -0.010(3) 0.014(3) -0.011(3) C C6 0.065(4) 0.060(4) 0.065(4) -0.014(3) 0.009(3) 0.003(3) C S7 0.0557(8) 0.0576(8) 0.0497(7) 0.0023(6) 0.0074(6) -0.0007(6) S C8 0.074(4) 0.074(4) 0.048(3) 0.000(3) 0.007(3) 0.002(3) C C9 0.089(5) 0.074(4) 0.052(4) 0.006(4) 0.018(3) 0.013(3) C P1 0.0633(9) 0.0402(7) 0.0530(8) 0.0065(6) 0.0145(7) -0.0018(6) P P2 0.0547(7) 0.0407(6) 0.0455(7) -0.0020(6) 0.0083(6) -0.0003(5) P C10 0.075(4) 0.045(3) 0.067(4) -0.002(3) 0.010(3) -0.011(3) C C11 0.066(4) 0.042(3) 0.071(4) -0.005(3) 0.005(3) -0.003(3) C C12 0.087(5) 0.049(3) 0.063(4) 0.018(3) 0.022(4) 0.007(3) C C13 0.102(6) 0.045(3) 0.080(5) 0.007(3) 0.032(4) 0.010(3) C C14 0.137(8) 0.059(4) 0.087(6) 0.010(5) 0.058(6) 0.011(4) C C15 0.141(9) 0.086(6) 0.083(6) 0.043(6) 0.038(6) 0.033(5) C C16 0.102(6) 0.105(7) 0.075(5) 0.044(6) 0.023(5) 0.030(5) C C17 0.088(5) 0.080(5) 0.067(4) 0.030(4) 0.016(4) 0.012(4) C C18 0.064(4) 0.061(3) 0.049(3) 0.010(3) 0.011(3) -0.005(3) C C19 0.110(6) 0.073(5) 0.081(5) 0.028(5) 0.032(5) -0.002(4) C C20 0.109(7) 0.109(7) 0.095(7) 0.036(6) 0.044(6) -0.020(6) C C21 0.077(5) 0.148(9) 0.067(5) 0.013(6) 0.024(4) -0.012(6) C C22 0.108(7) 0.115(7) 0.070(5) -0.028(6) 0.045(5) -0.017(5) C C23 0.084(5) 0.072(5) 0.067(4) -0.004(4) 0.032(4) -0.014(4) C C24 0.071(4) 0.051(3) 0.047(3) 0.003(3) 0.010(3) -0.003(3) C C25 0.073(4) 0.066(4) 0.056(4) -0.002(3) 0.016(3) 0.004(3) C C26 0.095(6) 0.085(5) 0.066(4) -0.006(4) 0.031(4) 0.013(4) C C27 0.121(7) 0.080(5) 0.051(4) 0.011(5) 0.029(4) 0.004(4) C C28 0.120(7) 0.089(6) 0.049(4) 0.004(5) -0.008(4) -0.001(4) C C29 0.085(5) 0.075(5) 0.055(4) -0.015(4) 0.002(3) -0.001(3) C C30 0.053(3) 0.052(3) 0.051(3) 0.0023(24) 0.0072(25) -0.0036(25) C C31 0.069(4) 0.056(3) 0.066(4) 0.008(3) 0.013(3) 0.004(3) C C32 0.077(5) 0.074(5) 0.089(6) 0.020(4) 0.011(4) 0.001(4) C C33 0.062(4) 0.105(7) 0.093(6) 0.008(4) 0.025(4) -0.018(5) C C34 0.083(5) 0.086(5) 0.076(5) -0.002(4) 0.030(4) -0.005(4) C C35 0.063(4) 0.069(4) 0.064(4) -0.003(3) 0.017(3) -0.001(3) C P3 0.0751(12) 0.0887(14) 0.0705(12) 0.0031(10) 0.0157(10) 0.0206(11) P F1 0.175(6) 0.125(5) 0.083(4) -0.007(5) 0.018(4) 0.012(4) F F2 0.306(11) 0.102(5) 0.078(4) 0.016(6) 0.057(5) -0.008(3) F F3 0.214(8) 0.103(5) 0.143(6) -0.011(5) 0.069(6) 0.038(4) F F4 0.135(6) 0.171(8) 0.244(10) 0.072(6) 0.034(7) 0.051(7) F F5 0.123(5) 0.369(15) 0.116(5) 0.098(8) 0.023(4) 0.018(7) F F6 0.332(12) 0.188(8) 0.086(4) -0.181(8) -0.010(6) 0.023(5) F P4 0.0751(11) 0.0792(12) 0.0580(10) 0.0092(10) 0.0046(8) -0.0135(9) P F7 0.223(10) 0.124(6) 0.112(6) 0.076(7) -0.017(6) -0.046(5) F F8 0.125(6) 0.138(7) 0.166(7) 0.031(5) 0.010(5) -0.075(6) F F9 0.091(5) 0.247(11) 0.178(8) 0.020(6) -0.045(5) -0.107(8) F F10 0.094(7) 0.191(14) 0.216(16) -0.027(9) 0.039(9) -0.115(12) F F11 0.164(13) 0.147(12) 0.095(7) 0.011(10) 0.061(8) 0.035(8) F F12 0.254(20) 0.169(14) 0.078(7) -0.032(12) 0.087(10) -0.035(8) F F13 0.119(14) 0.086(11) 0.162(18) -0.021(10) 0.019(13) -0.016(12) F F14 0.073(11) 0.139(22) 0.48(6) 0.004(14) 0.02(3) 0.18(3) F F15 0.128(18) 0.105(14) 0.074(10) 0.022(12) -0.044(12) -0.013(9) F F16 0.110(17) 0.138(22) 0.18(3) 0.010(16) 0.084(18) -0.037(20) F #=============================================================================== # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt S4 2.3685(14) C30-C31 1 ? ? ? Pt S7 2.3662(16) C30-C35 1 ? ? ? Pt P1 2.2555(15) C31-C32 1 ? ? ? Pt P2 2.2570(16) C31-H31 1 ? ? ? S1 C2 1.831(8) C32-C33 1 ? ? ? S1 C9 1.799(8) C32-H32 1 ? ? ? C2 C3 1.523(11) C33-C34 1 ? ? ? C2 H2a 1.051(6) C33-H33 1 ? ? ? C2 H2b 1.039(8) C34-C35 1 ? ? ? C3 S4 1.830(7) C34-H34 1 ? ? ? C3 H3a 1.028(7) C35-H35 1 ? ? ? C3 H3b 1.056(8) P3-F1 1 ? ? ? S4 C5 1.819(7) P3-F2 1 ? ? ? C5 C6 1.524(10) P3-F3 1 ? ? ? C5 H5a 1.039(7) P3-F4 1 ? ? ? C5 H5b 1.055(7) P3-F5 1 ? ? ? C6 S7 1.808(7) P3-F6 1 ? ? ? C6 H6a 1.045(7) F1-F4 2 ? ? ? C6 H6b 1.052(7) F1-F5 2 ? ? ? S7 C8 1.832(7) F1-F6 2 ? ? ? C8 C9 1.490(11) F2-F3 2 ? ? ? C8 H8a 1.032(7) F2-F5 2 ? ? ? C8 H8b 1.054(8) F2-F6 2 ? ? ? C9 H9a 1.045(7) F3-F4 2 ? ? ? C9 H9b 1.051(8) F3-F5 2 ? ? ? P1 C10 1.846(7) F4-F6 2 ? ? ? P1 C12 1.810(7) P4-F7 1 ? ? ? P1 C18 1.809(7) P4-F8 1 ? ? ? P2 C11 1.826(6) P4-F9 1 ? ? ? P2 C24 1.807(7) P4-F10 1 ? ? ? P2 C30 1.801(6) P4-F11a 1 ? ? ? C10 C11 1.530(10) P4-F12 1 ? ? ? C10 H10a 1.052(7) P4-F13a 1 ? ? ? C10 H10b 1.024(6) P4-F14 1 ? ? ? C11 H11a 1.035(7) P4-F15a 1 ? ? ? C11 H11b 1.046(7) P4-F16a 1 ? ? ? C12 C13 1.400(11) F7-F9 2 ? ? ? C12 C17 1.387(11) F7-F10 2 ? ? ? C13 C14 1.375(12) F7-F11a 2 ? ? ? C13 H13 1.059(9) F7-F14 1 ? ? ? C14 C15 1.386(17) F7-F16a 1 ? ? ? C14 H14 1.029(9) F8-F10 2 ? ? ? C15 C16 1.389(16) F8-F12 1 ? ? ? C15 H15 1.042(9) F8-F13a 1 ? ? ? C16 C17 1.388(11) F8-F15a 1 ? ? ? C16 H16 1.041(9) F9-F12 1 ? ? ? C17 H17 1.089(9) F9-F13a 1 ? ? ? C18 C19 1.396(10) F9-F16a 2 ? ? ? C18 C23 1.379(11) F10-F11a 2 ? ? ? C19 C20 1.388(13) F10-F14 1 ? ? ? C19 H19 1.044(10) F10-F15a 1 ? ? ? C20 C21 1.370(18) F11-P4a 1 ? ? ? C20 H20 1.043(9) F11-F7a 2 ? ? ? C21 C22 1.380(16) F11-F10a 2 ? ? ? C21 H21 1.059(9) F11-F13 1 ? ? ? C22 C23 1.392(11) F11-F15 1 ? ? ? C22 H22 1.050(10) F11-F16 1 ? ? ? C23 H23 1.054(8) F12-F14 1 ? ? ? C24 C25 1.374(10) F13-P4a 1 ? ? ? C24 C29 1.397(10) F13-F8a 1 ? ? ? C25 C26 1.388(10) F13-F9a 1 ? ? ? C25 H25 1.060(7) F13-F16 2 ? ? ? C26 C27 1.370(13) F15-P4a 1 ? ? ? C26 H26 1.059(8) F15-F8a 1 ? ? ? C27 C28 1.330(15) F15-F10a 1 ? ? ? C27 H27 1.037(8) F15-F16 2 ? ? ? C28 C29 1.401(12) F16-P4a 1 ? ? ? C28 H28 1.051(8) F16-F7a 1 ? ? ? C29 H29 1.062(8) F16-F9a 2 ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Pt S7 88.30(5) F4 F3 F5 91.8(5) ? ? ? ? S4 Pt P1 168.79(6) P3 F4 F1 49.4(3) ? ? ? ? S4 Pt P2 92.67(5) P3 F4 F3 46.3(3) ? ? ? ? S7 Pt P1 92.73(6) P3 F4 F6 44.4(4) ? ? ? ? S7 Pt P2 169.75(6) F1 F4 F3 63.7(3) ? ? ? ? P1 Pt P2 84.36(6) F1 F4 F6 61.3(4) ? ? ? ? C2 S1 C9 101.7(4) F3 F4 F6 90.7(4) ? ? ? ? S1 C2 C3 112.9(5) P3 F5 F1 48.2(3) ? ? ? ? S1 C2 H2a 110.0(6) P3 F5 F2 44.7(3) ? ? ? ? S1 C2 H2b 110.5(6) P3 F5 F3 48.0(3) ? ? ? ? C3 C2 H2a 108.3(6) F1 F5 F2 92.9(4) ? ? ? ? C3 C2 H2b 107.8(7) F1 F5 F3 64.2(4) ? ? ? ? H2a C2 H2b 107.2(6) F2 F5 F3 61.1(4) ? ? ? ? C2 C3 S4 116.1(5) P3 F6 F1 47.2(3) ? ? ? ? C2 C3 H3a 110.5(6) P3 F6 F2 44.0(3) ? ? ? ? C2 C3 H3b 107.4(6) P3 F6 F4 43.7(3) ? ? ? ? S4 C3 H3a 108.2(6) F1 F6 F2 91.1(3) ? ? ? ? S4 C3 H3b 106.7(5) F1 F6 F4 57.6(4) ? ? ? ? H3a C3 H3b 107.6(6) F2 F6 F4 63.7(4) ? ? ? ? Pt S4 C3 105.50(24) F7 P4 F8 165.5(7) ? ? ? ? Pt S4 C5 103.93(22) F7 P4 F9 87.3(5) ? ? ? ? C3 S4 C5 100.9(3) F7 P4 F10 85.4(7) ? ? ? ? S4 C5 C6 113.6(4) F7 P4 F11a 89.7(8) ? ? ? ? S4 C5 H5a 109.1(5) F7 P4 F12 92.6(8) ? ? ? ? S4 C5 H5b 108.4(5) F7 P4 F13a 129.0(9) ? ? ? ? C6 C5 H5a 110.7(6) F7 P4 F14 66.5(19) ? ? ? ? C6 C5 H5b 107.9(6) F7 P4 F15a 102.7(8) ? ? ? ? H5a C5 H5b 106.9(5) F7 P4 F16a 54.2(13) ? ? ? ? C5 C6 S7 114.4(5) F8 P4 F9 96.9(5) ? ? ? ? C5 C6 H6a 109.2(6) F8 P4 F10 86.9(6) ? ? ? ? C5 C6 H6b 107.3(6) F8 P4 F11a 102.4(7) ? ? ? ? S7 C6 H6a 109.7(5) F8 P4 F12 74.8(7) ? ? ? ? S7 C6 H6b 109.3(5) F8 P4 F13a 65.2(8) ? ? ? ? H6a C6 H6b 106.6(6) F8 P4 F14 99.0(19) ? ? ? ? Pt S7 C6 99.66(22) F8 P4 F15a 79.0(9) ? ? ? ? Pt S7 C8 108.4(3) F8 P4 F16a 139.8(13) ? ? ? ? C6 S7 C8 103.2(3) F9 P4 F10 163.9(10) ? ? ? ? S7 C8 C9 114.7(5) F9 P4 F11a 105.9(8) ? ? ? ? S7 C8 H8a 109.2(6) F9 P4 F12 77.9(8) ? ? ? ? S7 C8 H8b 107.9(5) F9 P4 F13a 68.7(9) ? ? ? ? C9 C8 H8a 110.2(6) F9 P4 F14 106.8(16) ? ? ? ? C9 C8 H8b 107.0(7) F9 P4 F15a 155.9(13) ? ? ? ? H8a C8 H8b 107.5(6) F9 P4 F16a 85.6(12) ? ? ? ? S1 C9 C8 118.3(5) F10 P4 F11a 88.4(10) ? ? ? ? S1 C9 H9a 108.9(6) F10 P4 F12 88.1(10) ? ? ? ? S1 C9 H9b 108.7(6) F10 P4 F13a 126.6(11) ? ? ? ? C8 C9 H9a 107.7(7) F10 P4 F14 57.1(17) ? ? ? ? C8 C9 H9b 105.9(7) F10 P4 F15a 40.2(14) ? ? ? ? H9a C9 H9b 106.7(6) F10 P4 F16a 101.6(11) ? ? ? ? Pt P1 C10 109.79(22) F11a P4 F12 175.7(10) ? ? ? ? Pt P1 C12 109.98(22) F11a P4 F13a 57.8(10) ? ? ? ? Pt P1 C18 116.46(23) F11a P4 F14 138.1(24) ? ? ? ? C10 P1 C12 108.6(3) F11a P4 F15a 53.1(14) ? ? ? ? C10 P1 C18 104.3(3) F11a P4 F16a 39.8(15) ? ? ? ? C12 P1 C18 107.4(3) F12 P4 F13a 122.8(10) ? ? ? ? Pt P2 C11 106.86(22) F12 P4 F14 40.6(25) ? ? ? ? Pt P2 C24 113.38(23) F12 P4 F15a 122.8(14) ? ? ? ? Pt P2 C30 114.89(20) F12 P4 F16a 143.8(15) ? ? ? ? C11 P2 C24 106.7(3) F13a P4 F14 162.0(25) ? ? ? ? C11 P2 C30 107.9(3) F13a P4 F15a 88.3(13) ? ? ? ? C24 P2 C30 106.7(3) F13a P4 F16a 78.9(13) ? ? ? ? P1 C10 C11 111.2(4) F14 P4 F15a 97.3(19) ? ? ? ? P1 C10 H10a 108.5(5) F14 P4 F16a 118.7(24) ? ? ? ? P1 C10 H10b 109.6(5) F15a P4 F16a 82.7(16) ? ? ? ? C11 C10 H10a 108.6(6) P4 F7 F9 44.9(3) ? ? ? ? C11 C10 H10b 110.6(6) P4 F7 F10 48.5(4) ? ? ? ? H10a C10 H10b 108.3(6) P4 F7 F11a 44.2(5) ? ? ? ? P2 C11 C10 108.0(4) P4 F7 F14 52.8(9) ? ? ? ? P2 C11 H11a 110.5(5) P4 F7 F16a 66.3(10) ? ? ? ? P2 C11 H11b 109.9(5) F9 F7 F10 92.5(5) ? ? ? ? C10 C11 H11a 110.0(6) F9 F7 F11a 68.1(6) ? ? ? ? C10 C11 H11b 110.5(6) F9 F7 F14 76.2(15) ? ? ? ? H11a C11 H11b 107.9(6) F9 F7 F16a 71.1(12) ? ? ? ? P1 C12 C13 119.6(6) F10 F7 F11a 60.7(7) ? ? ? ? P1 C12 C17 120.0(6) F10 F7 F14 42.7(14) ? ? ? ? C13 C12 C17 119.9(7) F10 F7 F16a 86.7(12) ? ? ? ? C12 C13 C14 119.6(8) F11a F7 F14 91.1(9) ? ? ? ? C12 C13 H13 120.5(7) F11a F7 F16a 27.0(11) ? ? ? ? C14 C13 H13 119.9(8) F14 F7 F16a 117.2(13) ? ? ? ? C13 C14 C15 120.1(8) P4 F8 F10 47.8(4) ? ? ? ? C13 C14 H14 121.3(10) P4 F8 F12 52.7(4) ? ? ? ? C15 C14 H14 118.6(9) P4 F8 F13a 61.0(7) ? ? ? ? C14 C15 C16 121.0(8) P4 F8 F15a 50.1(6) ? ? ? ? C14 C15 H15 119.2(10) F10 F8 F12 65.3(7) ? ? ? ? C16 C15 H15 119.8(11) F10 F8 F13a 96.7(8) ? ? ? ? C15 C16 C17 118.8(9) F10 F8 F15a 29.8(10) ? ? ? ? C15 C16 H16 119.4(8) F12 F8 F13a 103.0(9) ? ? ? ? C17 C16 H16 121.7(9) F12 F8 F15a 89.6(8) ? ? ? ? C12 C17 C16 120.6(8) F13a F8 F15a 74.2(12) ? ? ? ? C12 C17 H17 119.9(7) P4 F9 F7 47.8(3) ? ? ? ? C16 C17 H17 119.5(8) P4 F9 F12 52.8(5) ? ? ? ? P1 C18 C19 118.8(6) P4 F9 F13a 60.9(7) ? ? ? ? P1 C18 C23 121.4(5) P4 F9 F16a 50.5(7) ? ? ? ? C19 C18 C23 119.6(7) F7 F9 F12 68.1(6) ? ? ? ? C18 C19 C20 119.6(9) F7 F9 F13a 97.1(8) ? ? ? ? C18 C19 H19 120.5(8) F7 F9 F16a 40.5(10) ? ? ? ? C20 C19 H19 119.9(8) F12 F9 F13a 100.3(9) ? ? ? ? C19 C20 C21 119.7(8) F12 F9 F16a 97.7(8) ? ? ? ? C19 C20 H20 120.6(11) F13a F9 F16a 64.6(12) ? ? ? ? C21 C20 H20 119.6(9) P4 F10 F7 46.1(5) ? ? ? ? C20 C21 C22 121.9(8) P4 F10 F8 45.3(3) ? ? ? ? C20 C21 H21 119.9(10) P4 F10 F11a 43.7(5) ? ? ? ? C22 C21 H21 118.2(11) P4 F10 F14 54.7(10) ? ? ? ? C21 C22 C23 118.2(9) P4 F10 F15a 65.7(11) ? ? ? ? C21 C22 H22 121.5(9) F7 F10 F8 90.7(5) ? ? ? ? C23 C22 H22 120.3(9) F7 F10 F11a 59.8(6) ? ? ? ? C18 C23 C22 121.0(8) F7 F10 F14 49.4(18) ? ? ? ? C18 C23 H23 119.7(7) F7 F10 F15a 90.1(14) ? ? ? ? C22 C23 H23 119.2(8) F8 F10 F11a 66.3(6) ? ? ? ? P2 C24 C25 120.6(5) F8 F10 F14 73.9(18) ? ? ? ? P2 C24 C29 119.5(6) F8 F10 F15a 63.9(11) ? ? ? ? C25 C24 C29 119.8(6) F11a F10 F14 95.3(11) ? ? ? ? C24 C25 C26 119.9(7) F11a F10 F15a 30.3(13) ? ? ? ? C24 C25 H25 120.0(6) F14 F10 F15a 120.4(15) ? ? ? ? C26 C25 H25 120.1(7) P4a F11 F7a 46.0(4) ? ? ? ? C25 C26 C27 120.0(8) P4a F11 F10a 47.8(6) ? ? ? ? C25 C26 H26 120.4(8) P4a F11 F13 66.8(9) ? ? ? ? C27 C26 H26 119.6(7) P4a F11 F15 64.4(9) ? ? ? ? C26 C27 C28 120.7(7) P4a F11 F16 77.3(17) ? ? ? ? C26 C27 H27 117.5(9) F7a F11 F10a 59.4(7) ? ? ? ? C28 C27 H27 121.8(9) F7a F11 F13 102.7(10) ? ? ? ? C27 C28 C29 121.4(8) F7a F11 F15 83.1(11) ? ? ? ? C27 C28 H28 118.2(9) F7a F11 F16 37.8(16) ? ? ? ? C29 C28 H28 120.3(10) F10a F11 F13 103.1(10) ? ? ? ? C24 C29 C28 118.2(8) F10a F11 F15 23.7(10) ? ? ? ? C24 C29 H29 120.7(7) F10a F11 F16 95.9(17) ? ? ? ? C28 C29 H29 121.1(7) F13 F11 F15 100.8(14) ? ? ? ? P2 C30 C31 119.7(5) F13 F11 F16 105.8(21) ? ? ? ? P2 C30 C35 119.4(5) F15 F11 F16 118.8(20) ? ? ? ? C31 C30 C35 120.6(6) P4 F12 F8 52.5(6) ? ? ? ? C30 C31 C32 119.1(7) P4 F12 F9 49.3(5) ? ? ? ? C30 C31 H31 120.6(6) P4 F12 F14 62.7(17) ? ? ? ? C32 C31 H31 120.3(7) F8 F12 F9 73.4(7) ? ? ? ? C31 C32 C33 121.3(8) F8 F12 F14 96.8(16) ? ? ? ? C31 C32 H32 119.3(9) F9 F12 F14 100.1(19) ? ? ? ? C33 C32 H32 119.3(8) P4a F13 F8a 53.8(6) ? ? ? ? C32 C33 C34 119.2(7) P4a F13 F9a 50.4(6) ? ? ? ? C32 C33 H33 120.7(10) P4a F13 F11 55.4(7) ? ? ? ? C34 C33 H33 120.1(9) P4a F13 F16 50.0(9) ? ? ? ? C33 C34 C35 121.5(8) F8a F13 F9a 79.9(10) ? ? ? ? C33 C34 H34 118.1(8) F8a F13 F11 92.5(11) ? ? ? ? C35 C34 H34 120.4(9) F8a F13 F16 101.9(10) ? ? ? ? C30 C35 C34 118.3(7) F9a F13 F11 90.8(10) ? ? ? ? C30 C35 H35 120.2(7) F9a F13 F16 65.5(12) ? ? ? ? C34 C35 H35 121.5(7) F11 F13 F16 29.5(12) ? ? ? ? F1 P3 F2 175.8(5) P4 F14 F7 60.7(15) ? ? ? ? F1 P3 F3 90.6(4) P4 F14 F10 68.2(15) ? ? ? ? F1 P3 F4 85.0(5) P4 F14 F12 76.7(19) ? ? ? ? F1 P3 F5 86.0(4) F7 F14 F10 87(3) ? ? ? ? F1 P3 F6 88.5(4) F7 F14 F12 112.5(20) ? ? ? ? F2 P3 F3 89.1(4) F10 F14 F12 122(3) ? ? ? ? F2 P3 F4 99.1(6) P4a F15 F8a 50.9(5) ? ? ? ? F2 P3 F5 89.8(5) P4a F15 F10a 74.1(13) ? ? ? ? F2 P3 F6 91.7(4) P4a F15 F11 62.5(10) ? ? ? ? F3 P3 F4 89.1(5) P4a F15 F16 51.1(11) ? ? ? ? F3 P3 F5 84.4(6) F8a F15 F10a 86.3(15) ? ? ? ? F3 P3 F6 178.6(6) F8a F15 F11 89.9(11) ? ? ? ? F4 P3 F5 168.9(6) F8a F15 F16 95.3(11) ? ? ? ? F4 P3 F6 91.9(6) F10a F15 F11 126.0(18) ? ? ? ? F5 P3 F6 94.4(7) F10a F15 F16 100.1(17) ? ? ? ? P3 F1 F4 45.5(3) F11 F15 F16 26.8(12) ? ? ? ? P3 F1 F5 45.7(3) P4a F16 F7a 59.5(10) ? ? ? ? P3 F1 F6 44.3(3) P4a F16 F9a 43.8(7) ? ? ? ? F4 F1 F5 91.1(4) P4a F16 F11 62.8(11) ? ? ? ? F4 F1 F6 61.1(5) P4a F16 F13 51.2(9) ? ? ? ? F5 F1 F6 62.6(5) P4a F16 F15 46.2(8) ? ? ? ? P3 F2 F3 46.1(3) F7a F16 F9a 68.4(13) ? ? ? ? P3 F2 F5 45.5(3) F7a F16 F11 115.1(18) ? ? ? ? P3 F2 F6 44.3(3) F7a F16 F13 107.9(15) ? ? ? ? F3 F2 F5 57.6(4) F7a F16 F15 82.8(13) ? ? ? ? F3 F2 F6 90.4(3) F9a F16 F11 89.5(16) ? ? ? ? F5 F2 F6 62.4(5) F9a F16 F13 49.8(9) ? ? ? ? P3 F3 F2 44.8(3) F9a F16 F15 88.1(9) ? ? ? ? P3 F3 F4 44.6(3) F11 F16 F13 44.7(14) ? ? ? ? P3 F3 F5 47.6(4) F11 F16 F15 34.4(13) ? ? ? ? F2 F3 F4 64.7(4) F13 F16 F15 64.1(10) ? ? ? ? F2 F3 F5 61.3(4) ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? #=============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #=============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./ #1 ==== END #=============================================================================== data_compound2 _database_code_CSD 180862 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common ? _chemical_formula_moiety 'C33 H38 S3 P4 F12 Pt ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H38 S3 P4 F12 Pt ' _chemical_formula_weight 1077.80 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.017 0.009 'International Tables Vol. IV Table 2.2B' H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B' S ? 0.319 0.557 'International Tables Vol. IV Table 2.2B' P ? 0.283 0.434 'International Tables Vol. IV Table 2.2B' F ? 0.069 0.053 'International Tables Vol. IV Table 2.2B' Pt ? -5.233 6.925 'International Tables Vol. IV Table 2.2B' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,1/2+y,1/2-z x,1/2-y,1/2+z _cell_length_a 10.9130(13) _cell_length_b 29.8500(22) _cell_length_c 12.4053(16) _cell_angle_alpha 90.0 _cell_angle_beta 100.138(10) _cell_angle_gamma 90.0 _cell_volume 3978.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.60 _cell_measurement_theta_max 44.15 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method ? _exptl_crystal_F_000 2114.52 _exptl_absorpt_coefficient_mu 10.43 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0476 _exptl_absorpt_correction_T_max 0.2038 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54056 _diffrn_radiation_type 'Copper K\a ' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method 'Theta/2theta scan b/P/b ' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 9293 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 74.89 _diffrn_reflns_reduction_process ? _reflns_number_total 7913 _reflns_number_observed 6631 _reflns_observed_criterion 'Inet > 2.5\s(Inet)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'NRCVAX SOLVER' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_molecular_graphics 'NRCVAX' _computing_publication_material 'NRCVAX TABLES Jan 94 Version' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; ? #Insert any special details here. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 1/(\s^2^(F)+0.0003F^2^) _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Larson _refine_ls_extinction_coef '3292( 419)' _refine_ls_number_reflns 6631 _refine_ls_number_parameters 479 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.049 _refine_ls_R_factor_obs 0.040 _refine_ls_wR_factor_all 0.055 _refine_ls_wR_factor_obs 0.054 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.96 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean ? _refine_diff_density_max 1.74 _refine_diff_density_min -1.17 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Pt 0.165585(20) 0.137591(7) 0.243284(18) 0.04391(13) Uij ? . Pt S1 0.20382(14) 0.20988(4) 0.17789(12) 0.0523(7) Uij ? . S C2 0.1460(6) 0.24931(20) 0.2685(6) 0.064(4) Uij ? . C C3 0.1812(7) 0.24113(22) 0.3909(6) 0.069(4) Uij ? . C S4 0.14388(17) 0.18556(6) 0.43466(14) 0.0671(9) Uij ? . S C5 0.2939(8) 0.16719(25) 0.5114(6) 0.074(4) Uij ? . C C6 0.4027(7) 0.16610(24) 0.4518(6) 0.070(4) Uij ? . C S7 0.37840(14) 0.13484(5) 0.32376(13) 0.0547(7) Uij ? . S C8 0.4414(6) 0.17241(23) 0.2323(6) 0.065(3) Uij ? . C C9 0.3731(6) 0.21691(22) 0.2128(6) 0.063(4) Uij ? . C P1 0.15635(13) 0.06356(4) 0.28574(13) 0.0485(7) Uij ? . P P2 -0.02224(13) 0.13777(4) 0.12869(12) 0.0481(7) Uij ? . P C10 0.0039(6) 0.03621(19) 0.2603(6) 0.062(3) Uij ? . C C11 -0.0733(6) 0.04609(21) 0.1482(6) 0.066(4) Uij ? . C C12 -0.1302(5) 0.09295(20) 0.1456(6) 0.059(3) Uij ? . C C13 0.2142(6) 0.05382(18) 0.4294(5) 0.053(3) Uij ? . C C14 0.1381(6) 0.05780(22) 0.5062(6) 0.066(4) Uij ? . C C15 0.1850(8) 0.0539(3) 0.6169(6) 0.078(5) Uij ? . C C16 0.3101(8) 0.0463(3) 0.6523(6) 0.081(5) Uij ? . C C17 0.3887(7) 0.0425(3) 0.5773(6) 0.077(4) Uij ? . C C18 0.3423(6) 0.04588(21) 0.4658(6) 0.062(3) Uij ? . C C19 0.2493(6) 0.02966(19) 0.2101(5) 0.056(3) Uij ? . C C20 0.2748(7) -0.01470(20) 0.2403(6) 0.067(4) Uij ? . C C21 0.3371(7) -0.04190(23) 0.1792(8) 0.080(5) Uij ? . C C22 0.3709(8) -0.0262(3) 0.0844(8) 0.087(5) Uij ? . C C23 0.3486(8) 0.0172(3) 0.0529(7) 0.089(5) Uij ? . C C24 0.2870(7) 0.04559(23) 0.1158(6) 0.069(4) Uij ? . C C25 -0.0070(6) 0.13532(18) -0.0146(5) 0.053(3) Uij ? . C C26 0.1062(6) 0.13441(20) -0.0479(5) 0.057(3) Uij ? . C C27 0.1136(7) 0.13257(23) -0.1585(6) 0.065(4) Uij ? . C C28 0.0041(8) 0.1313(3) -0.2354(6) 0.074(4) Uij ? . C C29 -0.1099(7) 0.1315(3) -0.2035(6) 0.076(4) Uij ? . C C30 -0.1160(7) 0.13437(25) -0.0932(6) 0.068(4) Uij ? . C C31 -0.1094(5) 0.18892(19) 0.1426(5) 0.054(3) Uij ? . C C32 -0.1207(7) 0.22270(22) 0.0652(6) 0.065(4) Uij ? . C C33 -0.1855(8) 0.26142(24) 0.0810(7) 0.079(5) Uij ? . C C34 -0.2405(8) 0.2664(3) 0.1725(7) 0.085(5) Uij ? . C C35 -0.2265(7) 0.2330(3) 0.2504(7) 0.076(4) Uij ? . C C36 -0.1621(5) 0.19405(23) 0.2369(5) 0.059(3) Uij ? . C P3 0.25334(16) 0.59803(6) 0.03304(15) 0.0617(8) Uij ? . P F1 0.3734(5) 0.57232(22) 0.0274(7) 0.144(5) Uij ? . F F2 0.1316(5) 0.6223(3) 0.0466(9) 0.200(8) Uij ? . F F3 0.1758(5) 0.56598(23) -0.0533(6) 0.133(5) Uij ? . F F4 0.3248(5) 0.6320(3) 0.1152(6) 0.156(5) Uij ? . F F5 0.2218(9) 0.5655(4) 0.1198(7) 0.206(9) Uij ? . F F6 0.2819(12) 0.6283(3) -0.0577(7) 0.219(9) Uij ? . F P4 0.50906(16) 0.83154(6) 0.09966(17) 0.0681(10) Uij ? . P F7 0.5575(7) 0.88096(21) 0.1089(8) 0.172(6) Uij ? . F F8 0.4155(7) 0.8439(3) 0.1738(6) 0.172(7) Uij ? . F F9 0.4087(5) 0.84334(25) -0.0031(5) 0.128(4) Uij ? . F F10 0.6075(6) 0.8214(3) 0.0284(5) 0.167(7) Uij ? . F F11 0.6125(4) 0.81896(16) 0.2023(4) 0.093(3) Uij ? . F F12 0.4641(7) 0.78294(20) 0.0960(8) 0.192(7) Uij ? . F HC2a 0.196 0.278 0.251 0.0700 Uiso ? . H HC2b 0.051 0.246 0.242 0.0700 Uiso ? . H HC3a 0.143 0.266 0.438 0.0750 Uiso ? . H HC3b 0.265 0.252 0.413 0.0750 Uiso ? . H HC5a 0.270 0.139 0.538 0.0750 Uiso ? . H HC5b 0.325 0.188 0.573 0.0750 Uiso ? . H HC6a 0.424 0.201 0.436 0.0700 Uiso ? . H HC6b 0.476 0.149 0.503 0.0750 Uiso ? . H HC8a 0.412 0.157 0.155 0.0700 Uiso ? . H HC8b 0.527 0.178 0.282 0.0700 Uiso ? . H HC9a 0.405 0.232 0.147 0.0700 Uiso ? . H HC9b 0.397 0.237 0.274 0.0700 Uiso ? . H HC10a 0.029 0.007 0.260 0.0650 Uiso ? . H HC10b -0.047 0.044 0.313 0.0650 Uiso ? . H HC11a -0.024 0.040 0.088 0.0700 Uiso ? . H HC11b -0.130 0.023 0.139 0.0700 Uiso ? . H HC12a -0.198 0.096 0.067 0.0650 Uiso ? . H HC12b -0.169 0.105 0.214 0.0650 Uiso ? . H HC14 0.038 0.068 0.489 0.0700 Uiso ? . H HC15 0.119 0.053 0.674 0.0800 Uiso ? . H HC16 0.341 0.045 0.737 0.0800 Uiso ? . H HC17 0.483 0.034 0.610 0.0800 Uiso ? . H HC18 0.415 0.041 0.414 0.0700 Uiso ? . H HC20 0.249 -0.026 0.310 0.0700 Uiso ? . H HC21 0.347 -0.076 0.203 0.0800 Uiso ? . H HC22 0.412 -0.047 0.045 0.0850 Uiso ? . H HC23 0.375 0.029 -0.020 0.1000 Uiso ? . H HC24 0.271 0.079 0.093 0.0750 Uiso ? . H HC26 0.191 0.139 0.007 0.0600 Uiso ? . H HC27 0.187 0.132 -0.198 0.0700 Uiso ? . H HC28 0.011 0.124 -0.314 0.0750 Uiso ? . H HC29 -0.202 0.136 -0.260 0.0750 Uiso ? . H HC30 -0.203 0.135 -0.068 0.0750 Uiso ? . H HC32 -0.095 0.211 -0.005 0.0700 Uiso ? . H HC33 -0.195 0.287 0.022 0.0850 Uiso ? . H HC34 -0.301 0.295 0.187 0.0800 Uiso ? . H HC35 -0.265 0.237 0.322 0.0850 Uiso ? . H HC36 -0.137 0.173 0.307 0.0650 Uiso ? . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Pt 0.04424(15) 0.03484(12) 0.05105(14) -0.00086(8) 0.00398(9) 0.00171(8) Pt S1 0.0593(8) 0.0380(6) 0.0581(7) -0.0024(5) 0.0056(6) 0.0035(5) S C2 0.069(4) 0.043(3) 0.081(4) -0.006(3) 0.013(3) -0.006(3) C C3 0.082(5) 0.050(3) 0.075(4) -0.008(3) 0.015(3) -0.016(3) C S4 0.0753(10) 0.0618(9) 0.0671(9) -0.0081(8) 0.0203(8) -0.0066(7) S C5 0.093(5) 0.068(4) 0.057(4) -0.018(4) 0.006(3) -0.003(3) C C6 0.071(4) 0.065(4) 0.066(4) -0.005(3) -0.008(3) -0.004(3) C S7 0.0476(7) 0.0499(7) 0.0633(8) -0.0019(5) 0.0012(6) 0.0059(6) S C8 0.058(3) 0.064(4) 0.072(4) -0.007(3) 0.007(3) 0.009(3) C C9 0.061(4) 0.056(3) 0.073(4) -0.011(3) 0.012(3) 0.000(3) C P1 0.0499(7) 0.0344(6) 0.0619(8) 0.0004(5) 0.0112(6) 0.0055(6) P P2 0.0441(7) 0.0441(6) 0.0542(7) 0.0002(5) 0.0032(6) 0.0019(6) P C10 0.050(3) 0.048(3) 0.088(4) -0.0075(24) 0.013(3) 0.009(3) C C11 0.059(4) 0.049(3) 0.088(5) -0.012(3) 0.010(3) -0.006(3) C C12 0.049(3) 0.051(3) 0.075(4) -0.0070(24) 0.008(3) 0.003(3) C C13 0.062(3) 0.0390(24) 0.060(3) 0.0018(23) 0.015(3) 0.0052(23) C C14 0.068(4) 0.057(3) 0.077(4) 0.006(3) 0.025(3) 0.005(3) C C15 0.099(6) 0.071(4) 0.070(4) 0.002(4) 0.034(4) 0.008(4) C C16 0.103(6) 0.080(5) 0.058(4) 0.006(4) 0.009(4) 0.008(4) C C17 0.082(5) 0.077(4) 0.067(4) 0.008(4) 0.000(4) 0.013(4) C C18 0.063(4) 0.052(3) 0.070(4) 0.009(3) 0.008(3) 0.009(3) C C19 0.055(3) 0.044(3) 0.070(4) 0.0030(23) 0.011(3) -0.002(3) C C20 0.079(4) 0.040(3) 0.084(5) 0.007(3) 0.020(4) 0.003(3) C C21 0.080(5) 0.050(3) 0.110(6) 0.005(3) 0.015(4) -0.010(4) C C22 0.081(5) 0.073(5) 0.110(7) 0.013(4) 0.022(5) -0.023(5) C C23 0.098(6) 0.087(5) 0.092(6) 0.010(5) 0.041(5) 0.000(5) C C24 0.075(4) 0.054(3) 0.082(5) 0.009(3) 0.024(4) 0.005(3) C C25 0.057(3) 0.047(3) 0.052(3) 0.0030(23) 0.0015(25) 0.0002(23) C C26 0.055(3) 0.054(3) 0.062(3) -0.0022(24) 0.005(3) -0.005(3) C C27 0.066(4) 0.065(4) 0.066(4) 0.000(3) 0.013(3) -0.007(3) C C28 0.087(5) 0.082(5) 0.051(3) 0.002(4) 0.007(3) -0.008(3) C C29 0.070(4) 0.092(5) 0.060(4) 0.003(4) -0.006(3) -0.012(4) C C30 0.053(4) 0.084(5) 0.065(4) 0.005(3) 0.005(3) -0.006(3) C C31 0.047(3) 0.049(3) 0.062(3) 0.0063(23) -0.0009(25) -0.001(3) C C32 0.076(4) 0.054(3) 0.063(4) 0.010(3) 0.005(3) 0.004(3) C C33 0.096(5) 0.055(3) 0.081(5) 0.019(4) 0.005(4) 0.004(3) C C34 0.088(5) 0.067(4) 0.097(6) 0.025(4) 0.009(4) -0.012(4) C C35 0.078(5) 0.068(4) 0.087(5) 0.005(4) 0.027(4) -0.017(4) C C36 0.055(3) 0.061(3) 0.064(4) 0.005(3) 0.014(3) 0.000(3) C P3 0.0576(9) 0.0615(9) 0.0661(9) 0.0015(7) 0.0116(7) -0.0082(8) P F1 0.076(3) 0.122(5) 0.233(8) 0.021(3) 0.028(4) -0.038(5) F F2 0.061(3) 0.159(6) 0.363(13) 0.021(3) -0.010(5) -0.151(8) F F3 0.097(4) 0.148(5) 0.155(5) -0.016(4) 0.024(4) -0.087(5) F F4 0.068(3) 0.212(8) 0.182(7) -0.026(4) 0.009(4) -0.122(6) F F5 0.228(9) 0.250(11) 0.164(7) -0.027(8) 0.101(7) 0.070(7) F F6 0.311(14) 0.196(9) 0.130(6) -0.055(9) -0.015(8) 0.082(6) F P4 0.0552(9) 0.0609(9) 0.0882(12) 0.0137(7) 0.0125(8) 0.0109(9) P F7 0.146(6) 0.076(4) 0.263(10) -0.002(4) -0.049(6) 0.043(5) F F8 0.119(5) 0.258(10) 0.148(6) 0.072(6) 0.048(5) 0.015(6) F F9 0.081(3) 0.164(6) 0.127(5) 0.021(4) -0.013(3) 0.053(4) F F10 0.110(4) 0.307(11) 0.088(4) 0.076(6) 0.032(3) 0.005(5) F F11 0.091(3) 0.083(3) 0.097(3) 0.0156(25) -0.005(3) 0.014(3) F F12 0.173(7) 0.079(4) 0.272(10) -0.037(4) -0.104(7) 0.028(5) F #=============================================================================== # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ? ? ? ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? #=============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #=============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./ #2 === END data_grant6 _database_code_CSD 180863 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H40 F12 P4 Pt S3' _chemical_formula_weight 1091.81 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' '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 ? _symmetry_space_group_name_H-M ? 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 10.63670(10) _cell_length_b 28.9211(3) _cell_length_c 12.98850(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.6650(10) _cell_angle_gamma 90.00 _cell_volume 3938.87(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 3.968 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34807 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 28.26 _reflns_number_total 9302 _reflns_number_gt 8321 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+2.5760P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00170(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9302 _refine_ls_number_parameters 521 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0517 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 -0.128752(9) 0.136338(3) -0.228494(7) 0.01505(4) Uani 1 1 d . . . P1 P -0.14290(6) 0.05965(2) -0.27274(5) 0.01628(13) Uani 1 1 d . . . P2 P 0.06643(6) 0.13307(2) -0.11972(5) 0.01743(13) Uani 1 1 d . . . S1 S -0.08671(7) 0.18914(3) -0.40483(6) 0.02794(16) Uani 1 1 d . . . S4 S -0.34406(6) 0.13924(2) -0.31448(5) 0.02015(13) Uani 1 1 d . . . S7 S -0.16126(6) 0.21179(2) -0.16078(5) 0.02093(13) Uani 1 1 d . . . C2 C -0.2372(3) 0.17305(11) -0.4857(2) 0.0304(7) Uani 1 1 d . . . H2A H -0.2512 0.1932 -0.5442 0.035(6) Uiso 1 1 calc R . . H2B H -0.2283 0.1427 -0.5115 0.035(6) Uiso 1 1 calc R . . C3 C -0.3558(3) 0.17397(11) -0.4342(2) 0.0285(6) Uani 1 1 d . . . H3A H -0.4262 0.1631 -0.4831 0.030(6) Uiso 1 1 calc R . . H3B H -0.3730 0.2051 -0.4180 0.030(6) Uiso 1 1 calc R . . C5 C -0.4106(2) 0.17818(10) -0.2278(2) 0.0241(6) Uani 1 1 d . . . H5A H -0.4944 0.1865 -0.2600 0.029(6) Uiso 1 1 calc R . . H5B H -0.4174 0.1620 -0.1653 0.029(6) Uiso 1 1 calc R . . C6 C -0.3344(3) 0.22195(10) -0.1996(2) 0.0260(6) Uani 1 1 d . . . H6A H -0.3655 0.2369 -0.1438 0.029(6) Uiso 1 1 calc R . . H6B H -0.3476 0.2423 -0.2579 0.029(6) Uiso 1 1 calc R . . C8 C -0.0954(3) 0.25397(9) -0.2421(2) 0.0256(6) Uani 1 1 d . . . H8A H -0.1259 0.2837 -0.2271 0.037(7) Uiso 1 1 calc R . . H8B H -0.0054 0.2543 -0.2214 0.037(7) Uiso 1 1 calc R . . C9 C -0.1247(3) 0.24678(10) -0.3608(2) 0.0307(7) Uani 1 1 d . . . H9A H -0.0781 0.2690 -0.3930 0.027(6) Uiso 1 1 calc R . . H9B H -0.2128 0.2525 -0.3840 0.027(6) Uiso 1 1 calc R . . C10 C -0.0070(3) 0.02051(9) -0.2405(2) 0.0223(5) Uani 1 1 d . . . H10A H -0.0320 -0.0097 -0.2645 0.026(6) Uiso 1 1 calc R . . H10B H 0.0595 0.0304 -0.2760 0.026(6) Uiso 1 1 calc R . . C11 C 0.0442(3) 0.01864(10) -0.1221(2) 0.0251(6) Uani 1 1 d . . . H11A H -0.0148 0.0337 -0.0859 0.025(5) Uiso 1 1 calc R . . H11B H 0.0498 -0.0128 -0.1003 0.025(5) Uiso 1 1 calc R . . C12 C 0.1748(3) 0.04126(10) -0.0919(2) 0.0295(6) Uani 1 1 d . . . H12A H 0.2371 0.0216 -0.1135 0.047(7) Uiso 1 1 calc R . . H12B H 0.1936 0.0436 -0.0180 0.047(7) Uiso 1 1 calc R . . C13 C 0.1871(2) 0.08963(10) -0.1386(2) 0.0248(6) Uani 1 1 d . . . H13A H 0.1854 0.0861 -0.2116 0.033(6) Uiso 1 1 calc R . . H13B H 0.2685 0.1016 -0.1098 0.033(6) Uiso 1 1 calc R . . C14 C -0.1906(2) 0.05377(9) -0.41347(19) 0.0196(5) Uani 1 1 d . . . C15 C -0.3186(3) 0.04824(10) -0.4595(2) 0.0249(6) Uani 1 1 d . . . H15 H -0.3825 0.0451 -0.4169 0.022(7) Uiso 1 1 calc R . . C16 C -0.3520(3) 0.04744(12) -0.5677(2) 0.0364(7) Uani 1 1 d . . . H16 H -0.4388 0.0438 -0.5989 0.047(10) Uiso 1 1 calc R . . C17 C -0.2591(3) 0.05195(12) -0.6301(2) 0.0403(8) Uani 1 1 d . . . H17 H -0.2827 0.0516 -0.7040 0.045(10) Uiso 1 1 calc R . . C18 C -0.1320(3) 0.05702(11) -0.5854(2) 0.0334(7) Uani 1 1 d . . . H18 H -0.0686 0.0596 -0.6287 0.039(9) Uiso 1 1 calc R . . C19 C -0.0970(3) 0.05834(10) -0.4771(2) 0.0245(6) Uani 1 1 d . . . H19 H -0.0101 0.0623 -0.4465 0.021(7) Uiso 1 1 calc R . . C20 C -0.2682(2) 0.03135(9) -0.21494(19) 0.0194(5) Uani 1 1 d . . . C21 C -0.3325(3) 0.05451(10) -0.1448(2) 0.0234(6) Uani 1 1 d . . . H21 H -0.3069 0.0848 -0.1218 0.030(8) Uiso 1 1 calc R . . C22 C -0.4341(3) 0.03314(11) -0.1085(2) 0.0296(6) Uani 1 1 d . . . H22 H -0.4793 0.0492 -0.0624 0.037(9) Uiso 1 1 calc R . . C23 C -0.4693(3) -0.01140(11) -0.1394(2) 0.0302(6) Uani 1 1 d . . . H23 H -0.5392 -0.0257 -0.1151 0.039(9) Uiso 1 1 calc R . . C24 C -0.4028(3) -0.03540(10) -0.2061(2) 0.0275(6) Uani 1 1 d . . . H24 H -0.4254 -0.0664 -0.2252 0.024(8) Uiso 1 1 calc R . . C25 C -0.3032(3) -0.01401(10) -0.2447(2) 0.0238(6) Uani 1 1 d . . . H25 H -0.2589 -0.0302 -0.2912 0.026(8) Uiso 1 1 calc R . . C26 C 0.1530(2) 0.18669(9) -0.1342(2) 0.0218(5) Uani 1 1 d . . . C27 C 0.2006(3) 0.19315(10) -0.2278(2) 0.0262(6) Uani 1 1 d . . . H27 H 0.1879 0.1701 -0.2806 0.030(8) Uiso 1 1 calc R . . C28 C 0.2666(3) 0.23359(11) -0.2425(3) 0.0354(7) Uani 1 1 d . . . H28 H 0.2985 0.2381 -0.3059 0.037(9) Uiso 1 1 calc R . . C29 C 0.2861(3) 0.26722(12) -0.1657(3) 0.0430(8) Uani 1 1 d . . . H29 H 0.3325 0.2944 -0.1759 0.061(12) Uiso 1 1 calc R . . C30 C 0.2377(3) 0.26114(11) -0.0734(3) 0.0416(8) Uani 1 1 d . . . H30 H 0.2498 0.2845 -0.0212 0.042(10) Uiso 1 1 calc R . . C31 C 0.1716(3) 0.22088(10) -0.0575(2) 0.0308(6) Uani 1 1 d . . . H31 H 0.1392 0.2167 0.0057 0.033(9) Uiso 1 1 calc R . . C32 C 0.0547(3) 0.12888(9) 0.0181(2) 0.0202(5) Uani 1 1 d . . . C33 C 0.1672(3) 0.12965(10) 0.0917(2) 0.0276(6) Uani 1 1 d . . . H33 H 0.2474 0.1319 0.0689 0.034(9) Uiso 1 1 calc R . . C34 C 0.1622(3) 0.12717(10) 0.1975(2) 0.0294(6) Uani 1 1 d . . . H34 H 0.2388 0.1277 0.2471 0.045(10) Uiso 1 1 calc R . . C35 C 0.0450(3) 0.12395(11) 0.2310(2) 0.0293(6) Uani 1 1 d . . . H35 H 0.0417 0.1230 0.3036 0.041(9) Uiso 1 1 calc R . . C36 C -0.0671(3) 0.12212(11) 0.1591(2) 0.0297(6) Uani 1 1 d . . . H36 H -0.1467 0.1190 0.1824 0.047(10) Uiso 1 1 calc R . . C37 C -0.0629(3) 0.12488(10) 0.0520(2) 0.0225(6) Uani 1 1 d . . . H37 H -0.1397 0.1240 0.0026 0.027(8) Uiso 1 1 calc R . . P3 P 0.27927(7) 0.09984(3) -0.47172(6) 0.02723(16) Uani 1 1 d . . . P4 P -0.44139(7) 0.16438(3) 0.09688(6) 0.02835(16) Uani 1 1 d . . . F1 F 0.1626(2) 0.13462(9) -0.5000(3) 0.0915(11) Uani 1 1 d . . . F2 F 0.2137(2) 0.07985(13) -0.38145(17) 0.0981(12) Uani 1 1 d . . . F3 F 0.3429(3) 0.12122(10) -0.56367(19) 0.0760(8) Uani 1 1 d . . . F4 F 0.20112(19) 0.06354(7) -0.55025(16) 0.0489(5) Uani 1 1 d . . . F5 F 0.3535(2) 0.13855(9) -0.3961(2) 0.0729(8) Uani 1 1 d . . . F6 F 0.3940(2) 0.06573(9) -0.4461(3) 0.0809(9) Uani 1 1 d . . . F7 F -0.3397(2) 0.17566(10) 0.02295(16) 0.0658(7) Uani 1 1 d . . . F8 F -0.4855(2) 0.21678(7) 0.0940(2) 0.0670(7) Uani 1 1 d . . . F9 F -0.5398(2) 0.15212(9) 0.17250(17) 0.0609(6) Uani 1 1 d . . . F10 F -0.54678(18) 0.15314(8) -0.00328(16) 0.0500(5) Uani 1 1 d . . . F11 F -0.33418(16) 0.17582(6) 0.19669(14) 0.0351(4) Uani 1 1 d . . . F12 F -0.3939(2) 0.11161(8) 0.1033(2) 0.0651(7) Uani 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 0.01470(5) 0.01404(5) 0.01624(5) -0.00022(4) 0.00205(3) 0.00090(4) P1 0.0170(3) 0.0153(3) 0.0168(3) -0.0010(2) 0.0036(2) -0.0002(2) P2 0.0150(3) 0.0183(3) 0.0186(3) -0.0009(3) 0.0019(2) 0.0004(3) S1 0.0293(4) 0.0253(4) 0.0318(4) 0.0054(3) 0.0127(3) 0.0065(3) S4 0.0173(3) 0.0214(3) 0.0209(3) -0.0010(2) 0.0007(2) 0.0025(3) S7 0.0220(3) 0.0159(3) 0.0248(3) -0.0015(2) 0.0037(3) 0.0015(3) C2 0.0396(17) 0.0321(16) 0.0200(13) 0.0061(12) 0.0060(12) 0.0098(14) C3 0.0294(15) 0.0316(16) 0.0226(13) 0.0040(12) -0.0008(11) 0.0091(13) C5 0.0170(13) 0.0295(15) 0.0269(13) -0.0017(12) 0.0068(11) 0.0059(11) C6 0.0217(14) 0.0247(15) 0.0324(15) -0.0008(12) 0.0066(12) 0.0065(11) C8 0.0236(14) 0.0149(13) 0.0385(16) 0.0023(11) 0.0057(12) 0.0002(11) C9 0.0345(17) 0.0224(15) 0.0375(16) 0.0089(12) 0.0124(13) 0.0047(12) C10 0.0227(13) 0.0173(13) 0.0272(13) -0.0021(10) 0.0046(11) 0.0027(11) C11 0.0296(15) 0.0189(14) 0.0261(13) 0.0044(11) 0.0030(11) 0.0044(11) C12 0.0275(15) 0.0267(15) 0.0318(15) 0.0000(12) -0.0024(12) 0.0102(12) C13 0.0163(13) 0.0274(15) 0.0304(14) -0.0041(12) 0.0033(11) 0.0041(11) C14 0.0236(13) 0.0174(13) 0.0181(12) -0.0032(10) 0.0045(10) -0.0010(10) C15 0.0238(14) 0.0271(15) 0.0239(13) -0.0017(11) 0.0040(11) -0.0037(11) C16 0.0346(18) 0.045(2) 0.0265(15) -0.0042(13) -0.0039(13) -0.0055(15) C17 0.053(2) 0.049(2) 0.0180(13) -0.0057(14) 0.0035(13) -0.0038(17) C18 0.0436(19) 0.0341(17) 0.0271(14) -0.0030(13) 0.0191(13) -0.0012(14) C19 0.0233(14) 0.0236(14) 0.0283(14) -0.0015(11) 0.0090(11) -0.0007(11) C20 0.0203(13) 0.0194(13) 0.0185(12) 0.0018(10) 0.0035(10) -0.0015(10) C21 0.0272(14) 0.0224(14) 0.0215(12) -0.0007(11) 0.0067(11) -0.0019(11) C22 0.0296(15) 0.0360(17) 0.0262(14) 0.0008(12) 0.0132(12) -0.0008(13) C23 0.0261(15) 0.0375(17) 0.0277(14) 0.0048(13) 0.0070(12) -0.0080(13) C24 0.0312(16) 0.0218(14) 0.0279(14) 0.0021(11) 0.0008(12) -0.0085(12) C25 0.0285(15) 0.0214(14) 0.0221(13) -0.0016(11) 0.0061(11) -0.0028(11) C26 0.0162(12) 0.0214(14) 0.0266(13) 0.0022(11) 0.0003(10) -0.0008(10) C27 0.0203(13) 0.0277(15) 0.0311(14) 0.0026(12) 0.0059(11) 0.0027(11) C28 0.0254(16) 0.0353(18) 0.0474(19) 0.0153(15) 0.0119(14) 0.0015(13) C29 0.0363(18) 0.0273(17) 0.062(2) 0.0154(16) -0.0009(16) -0.0085(15) C30 0.048(2) 0.0256(17) 0.0462(19) -0.0039(15) -0.0068(16) -0.0064(15) C31 0.0346(17) 0.0261(15) 0.0298(15) -0.0012(12) 0.0002(13) -0.0031(13) C32 0.0218(13) 0.0185(13) 0.0197(12) -0.0003(10) 0.0016(10) 0.0004(10) C33 0.0207(14) 0.0354(17) 0.0257(14) 0.0012(12) 0.0009(11) -0.0012(12) C34 0.0298(16) 0.0315(16) 0.0234(13) 0.0022(12) -0.0050(12) -0.0012(13) C35 0.0372(17) 0.0306(16) 0.0201(13) 0.0027(12) 0.0048(12) 0.0015(13) C36 0.0274(15) 0.0353(17) 0.0283(14) 0.0027(12) 0.0104(12) 0.0031(13) C37 0.0180(13) 0.0254(14) 0.0235(13) -0.0008(11) 0.0019(10) 0.0016(11) P3 0.0210(4) 0.0361(4) 0.0254(3) -0.0059(3) 0.0061(3) -0.0003(3) P4 0.0212(4) 0.0279(4) 0.0365(4) -0.0074(3) 0.0062(3) -0.0092(3) F1 0.0368(14) 0.0495(16) 0.177(3) -0.0304(17) -0.0136(16) 0.0119(11) F2 0.0627(16) 0.205(4) 0.0299(11) 0.0026(16) 0.0155(11) -0.0620(19) F3 0.0752(18) 0.101(2) 0.0541(14) 0.0149(14) 0.0182(13) -0.0359(16) F4 0.0417(11) 0.0533(13) 0.0527(12) -0.0283(10) 0.0112(9) -0.0097(10) F5 0.0336(12) 0.109(2) 0.0757(17) -0.0561(15) 0.0084(11) -0.0237(12) F6 0.0303(12) 0.0607(16) 0.145(3) 0.0243(16) -0.0041(14) 0.0115(11) F7 0.0362(12) 0.122(2) 0.0408(11) 0.0029(13) 0.0109(9) -0.0267(13) F8 0.0601(15) 0.0332(12) 0.0939(18) -0.0029(12) -0.0267(13) 0.0068(11) F9 0.0375(12) 0.0945(18) 0.0534(13) -0.0028(12) 0.0154(10) -0.0251(12) F10 0.0321(11) 0.0723(15) 0.0436(11) -0.0156(10) 0.0000(9) -0.0175(10) F11 0.0279(9) 0.0328(10) 0.0426(10) -0.0067(8) 0.0001(8) -0.0051(8) F12 0.0618(15) 0.0326(12) 0.0940(19) -0.0204(12) -0.0069(13) -0.0021(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2896(7) . ? Pt1 P2 2.3087(7) . ? Pt1 S4 2.3749(6) . ? Pt1 S7 2.3995(6) . ? Pt1 S1 2.8498(7) . ? P1 C14 1.821(3) . ? P1 C10 1.828(3) . ? P1 C20 1.829(3) . ? P2 C32 1.819(3) . ? P2 C26 1.829(3) . ? P2 C13 1.842(3) . ? S1 C2 1.821(3) . ? S1 C9 1.830(3) . ? S4 C5 1.818(3) . ? S4 C3 1.838(3) . ? S7 C8 1.828(3) . ? S7 C6 1.849(3) . ? C2 C3 1.525(4) . ? C5 C6 1.514(4) . ? C8 C9 1.535(4) . ? C10 C11 1.544(4) . ? C11 C12 1.526(4) . ? C12 C13 1.539(4) . ? C14 C15 1.402(4) . ? C14 C19 1.403(3) . ? C15 C16 1.390(4) . ? C16 C17 1.386(4) . ? C17 C18 1.387(5) . ? C18 C19 1.394(4) . ? C20 C21 1.398(3) . ? C20 C25 1.400(4) . ? C21 C22 1.394(4) . ? C22 C23 1.382(4) . ? C23 C24 1.392(4) . ? C24 C25 1.391(4) . ? C26 C31 1.394(4) . ? C26 C27 1.406(4) . ? C27 C28 1.394(4) . ? C28 C29 1.384(5) . ? C29 C30 1.393(5) . ? C30 C31 1.394(4) . ? C32 C37 1.399(4) . ? C32 C33 1.401(4) . ? C33 C34 1.386(4) . ? C34 C35 1.391(4) . ? C35 C36 1.387(4) . ? C36 C37 1.401(4) . ? P3 F6 1.561(2) . ? P3 F2 1.572(2) . ? P3 F1 1.592(2) . ? P3 F3 1.593(2) . ? P3 F4 1.596(2) . ? P3 F5 1.606(2) . ? P4 F8 1.585(2) . ? P4 F9 1.591(2) . ? P4 F7 1.596(2) . ? P4 F10 1.602(2) . ? P4 F12 1.606(2) . ? P4 F11 1.6106(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 97.38(2) . . ? P1 Pt1 S4 84.18(2) . . ? P2 Pt1 S4 170.50(2) . . ? P1 Pt1 S7 164.90(2) . . ? P2 Pt1 S7 89.03(2) . . ? S4 Pt1 S7 87.32(2) . . ? P1 Pt1 S1 109.26(2) . . ? P2 Pt1 S1 105.51(2) . . ? S4 Pt1 S1 82.66(2) . . ? S7 Pt1 S1 81.89(2) . . ? C14 P1 C10 104.37(12) . . ? C14 P1 C20 105.72(12) . . ? C10 P1 C20 103.39(12) . . ? C14 P1 Pt1 109.75(9) . . ? C10 P1 Pt1 121.74(9) . . ? C20 P1 Pt1 110.62(9) . . ? C32 P2 C26 106.05(12) . . ? C32 P2 C13 104.50(12) . . ? C26 P2 C13 100.99(13) . . ? C32 P2 Pt1 113.67(9) . . ? C26 P2 Pt1 108.59(9) . . ? C13 P2 Pt1 121.43(9) . . ? C2 S1 C9 101.21(14) . . ? C2 S1 Pt1 94.91(9) . . ? C9 S1 Pt1 99.45(9) . . ? C5 S4 C3 101.95(13) . . ? C5 S4 Pt1 100.11(9) . . ? C3 S4 Pt1 109.90(10) . . ? C8 S7 C6 101.36(13) . . ? C8 S7 Pt1 107.61(9) . . ? C6 S7 Pt1 104.04(9) . . ? C3 C2 S1 117.0(2) . . ? C2 C3 S4 114.72(19) . . ? C6 C5 S4 114.80(18) . . ? C5 C6 S7 113.66(19) . . ? C9 C8 S7 117.2(2) . . ? C8 C9 S1 114.81(19) . . ? C11 C10 P1 112.50(18) . . ? C12 C11 C10 113.2(2) . . ? C11 C12 C13 115.0(2) . . ? C12 C13 P2 117.39(19) . . ? C15 C14 C19 119.6(2) . . ? C15 C14 P1 121.72(19) . . ? C19 C14 P1 118.5(2) . . ? C16 C15 C14 119.9(3) . . ? C17 C16 C15 120.3(3) . . ? C16 C17 C18 120.4(3) . . ? C17 C18 C19 120.1(3) . . ? C18 C19 C14 119.8(3) . . ? C21 C20 C25 119.5(2) . . ? C21 C20 P1 121.5(2) . . ? C25 C20 P1 118.98(19) . . ? C22 C21 C20 120.0(3) . . ? C23 C22 C21 120.2(3) . . ? C22 C23 C24 120.3(3) . . ? C25 C24 C23 120.0(3) . . ? C24 C25 C20 120.1(2) . . ? C31 C26 C27 119.7(3) . . ? C31 C26 P2 122.8(2) . . ? C27 C26 P2 117.5(2) . . ? C28 C27 C26 119.6(3) . . ? C29 C28 C27 120.5(3) . . ? C28 C29 C30 120.0(3) . . ? C29 C30 C31 120.1(3) . . ? C30 C31 C26 120.1(3) . . ? C37 C32 C33 119.6(2) . . ? C37 C32 P2 121.9(2) . . ? C33 C32 P2 118.6(2) . . ? C34 C33 C32 120.3(3) . . ? C33 C34 C35 120.0(3) . . ? C36 C35 C34 120.4(3) . . ? C35 C36 C37 119.9(3) . . ? C32 C37 C36 119.8(3) . . ? F6 P3 F2 92.16(18) . . ? F6 P3 F1 178.94(19) . . ? F2 P3 F1 88.76(19) . . ? F6 P3 F3 89.43(16) . . ? F2 P3 F3 178.39(19) . . ? F1 P3 F3 89.65(18) . . ? F6 P3 F4 91.44(14) . . ? F2 P3 F4 89.20(13) . . ? F1 P3 F4 88.04(13) . . ? F3 P3 F4 90.99(13) . . ? F6 P3 F5 91.37(15) . . ? F2 P3 F5 91.98(15) . . ? F1 P3 F5 89.13(14) . . ? F3 P3 F5 87.74(14) . . ? F4 P3 F5 176.91(15) . . ? F8 P4 F9 90.30(15) . . ? F8 P4 F7 91.03(15) . . ? F9 P4 F7 178.29(15) . . ? F8 P4 F10 90.62(13) . . ? F9 P4 F10 90.74(11) . . ? F7 P4 F10 90.32(11) . . ? F8 P4 F12 178.20(14) . . ? F9 P4 F12 89.43(14) . . ? F7 P4 F12 89.20(15) . . ? F10 P4 F12 91.16(13) . . ? F8 P4 F11 89.40(11) . . ? F9 P4 F11 89.95(11) . . ? F7 P4 F11 88.99(11) . . ? F10 P4 F11 179.31(12) . . ? F12 P4 F11 88.82(11) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.813 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.087 #3 === END data_grant10 _database_code_CSD 180864 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H42 F12 P4 Pt S3' _chemical_formula_weight 1105.84 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' '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 ? _symmetry_space_group_name_H-M ? 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 10.719(4) _cell_length_b 29.648(8) _cell_length_c 12.968(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.05(3) _cell_angle_gamma 90.00 _cell_volume 4058(2) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.810 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 3.852 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5071 _exptl_absorpt_correction_T_max 0.6224 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25868 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.1140 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.32 _reflns_number_total 9578 _reflns_number_gt 5568 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00065(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9578 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1145 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _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 1.61997(2) 0.861760(7) 1.240005(16) 0.03076(8) Uani 1 1 d . . . P1 P 1.42465(13) 0.86157(5) 1.13310(11) 0.0339(3) Uani 1 1 d . . . P2 P 1.63126(14) 0.93676(5) 1.28762(11) 0.0312(3) Uani 1 1 d . . . S1 S 1.59224(18) 0.80928(6) 1.42039(14) 0.0567(5) Uani 1 1 d . . . S4 S 1.83596(13) 0.86040(5) 1.32062(11) 0.0406(4) Uani 1 1 d . . . S7 S 1.65487(15) 0.78896(5) 1.17325(12) 0.0441(4) Uani 1 1 d . . . C2 C 1.7458(7) 0.8242(2) 1.4948(5) 0.064(2) Uani 1 1 d . . . H2A H 1.7379 0.8532 1.5259 0.053(9) Uiso 1 1 calc R . . H2B H 1.7655 0.8029 1.5510 0.053(9) Uiso 1 1 calc R . . C3 C 1.8567(6) 0.8261(2) 1.4389(5) 0.0587(19) Uani 1 1 d . . . H3A H 1.8769 0.7959 1.4208 0.072(15) Uiso 1 1 calc R . . H3B H 1.9283 0.8376 1.4867 0.072(15) Uiso 1 1 calc R . . C5 C 1.8984(6) 0.8233(2) 1.2316(5) 0.0518(18) Uani 1 1 d . . . H5A H 1.9011 0.8396 1.1680 0.068(14) Uiso 1 1 calc R . . H5B H 1.9840 0.8158 1.2620 0.068(14) Uiso 1 1 calc R . . C6 C 1.8272(6) 0.7807(2) 1.2044(5) 0.0547(18) Uani 1 1 d . . . H6A H 1.8462 0.7601 1.2622 0.081(16) Uiso 1 1 calc R . . H6B H 1.8554 0.7672 1.1453 0.081(16) Uiso 1 1 calc R . . C8 C 1.5983(6) 0.74688(18) 1.2556(5) 0.0555(19) Uani 1 1 d . . . H8A H 1.5081 0.7446 1.2345 0.078(15) Uiso 1 1 calc R . . H8B H 1.6336 0.7183 1.2408 0.078(15) Uiso 1 1 calc R . . C9 C 1.6254(7) 0.75360(19) 1.3723(5) 0.064(2) Uani 1 1 d . . . H9A H 1.7133 0.7470 1.3967 0.098(19) Uiso 1 1 calc R . . H9B H 1.5769 0.7319 1.4035 0.098(19) Uiso 1 1 calc R . . C10 C 1.3011(5) 0.90187(17) 1.1519(4) 0.0406(15) Uani 1 1 d . . . H10A H 1.2212 0.8864 1.1383 0.053(9) Uiso 1 1 calc R . . H10B H 1.3157 0.9105 1.2243 0.053(9) Uiso 1 1 calc R . . C11 C 1.2879(6) 0.9452(2) 1.0857(5) 0.0502(17) Uani 1 1 d . . . H11A H 1.2504 0.9372 1.0154 0.050(12) Uiso 1 1 calc R . . H11B H 1.2292 0.9647 1.1121 0.050(12) Uiso 1 1 calc R . . C12 C 1.4065(6) 0.97224(19) 1.0806(4) 0.0457(16) Uani 1 1 d . . . H12A H 1.4723 0.9517 1.0702 0.052(13) Uiso 1 1 calc R . . H12B H 1.3900 0.9915 1.0204 0.052(13) Uiso 1 1 calc R . . C13 C 1.4550(6) 1.00071(19) 1.1743(4) 0.0460(17) Uani 1 1 d . . . H13A H 1.3898 1.0218 1.1834 0.059(13) Uiso 1 1 calc R . . H13B H 1.5256 1.0179 1.1592 0.059(13) Uiso 1 1 calc R . . C14 C 1.4972(5) 0.97627(18) 1.2784(4) 0.0400(15) Uani 1 1 d . . . H14A H 1.4258 0.9599 1.2945 0.034(10) Uiso 1 1 calc R . . H14B H 1.5189 0.9987 1.3319 0.034(10) Uiso 1 1 calc R . . C15 C 1.3443(5) 0.80876(18) 1.1490(4) 0.0362(14) Uani 1 1 d . . . C16 C 1.3267(6) 0.7752(2) 1.0748(6) 0.0603(19) Uani 1 1 d . . . H16 H 1.3628 0.7785 1.0125 0.040(17) Uiso 1 1 calc R . . C17 C 1.2584(8) 0.7367(2) 1.0876(7) 0.077(3) Uani 1 1 d . . . H17 H 1.2460 0.7139 1.0343 0.10(3) Uiso 1 1 calc R . . C18 C 1.2080(8) 0.7315(3) 1.1778(7) 0.077(2) Uani 1 1 d . . . H18 H 1.1595 0.7050 1.1873 0.15(4) Uiso 1 1 calc R . . C19 C 1.2275(7) 0.7642(3) 1.2539(7) 0.071(2) Uani 1 1 d . . . H19 H 1.1935 0.7603 1.3171 0.06(2) Uiso 1 1 calc R . . C20 C 1.2958(6) 0.8027(2) 1.2400(5) 0.0504(17) Uani 1 1 d . . . H20 H 1.3096 0.8253 1.2939 0.022(14) Uiso 1 1 calc R . . C21 C 1.4361(5) 0.86403(18) 0.9960(4) 0.0339(13) Uani 1 1 d . . . C22 C 1.5500(5) 0.86823(17) 0.9606(4) 0.0366(14) Uani 1 1 d . . . H22 H 1.6276 0.8695 1.0104 0.026(13) Uiso 1 1 calc R . . C23 C 1.5539(6) 0.87066(18) 0.8556(5) 0.0477(16) Uani 1 1 d . . . H23 H 1.6339 0.8733 0.8323 0.032(14) Uiso 1 1 calc R . . C24 C 1.4437(6) 0.8693(2) 0.7838(5) 0.0523(17) Uani 1 1 d . . . H24 H 1.4468 0.8711 0.7104 0.063(19) Uiso 1 1 calc R . . C25 C 1.3304(6) 0.8656(2) 0.8159(5) 0.0538(17) Uani 1 1 d . . . H25 H 1.2536 0.8650 0.7652 0.11(3) Uiso 1 1 calc R . . C26 C 1.3250(5) 0.8626(2) 0.9214(4) 0.0465(15) Uani 1 1 d . . . H26 H 1.2445 0.8595 0.9436 0.042(15) Uiso 1 1 calc R . . C27 C 1.6907(6) 0.93924(17) 1.4270(4) 0.0354(14) Uani 1 1 d . . . C28 C 1.6055(6) 0.93166(18) 1.4948(4) 0.0440(16) Uani 1 1 d . . . H28 H 1.5178 0.9260 1.4673 0.046(17) Uiso 1 1 calc R . . C29 C 1.6476(7) 0.9323(2) 1.6025(5) 0.0588(19) Uani 1 1 d . . . H29 H 1.5892 0.9272 1.6496 0.07(2) Uiso 1 1 calc R . . C30 C 1.7722(7) 0.9401(2) 1.6407(5) 0.069(2) Uani 1 1 d . . . H30 H 1.8013 0.9400 1.7151 0.058(18) Uiso 1 1 calc R . . C31 C 1.8573(7) 0.9483(2) 1.5748(5) 0.067(2) Uani 1 1 d . . . H31 H 1.9446 0.9541 1.6032 0.054(18) Uiso 1 1 calc R . . C32 C 1.8168(6) 0.94808(19) 1.4680(5) 0.0463(16) Uani 1 1 d . . . H32 H 1.8759 0.9541 1.4219 0.050(18) Uiso 1 1 calc R . . C33 C 1.7475(5) 0.96625(18) 1.2255(4) 0.0349(14) Uani 1 1 d . . . C34 C 1.7838(6) 1.00969(19) 1.2553(5) 0.0467(17) Uani 1 1 d . . . H34 H 1.7457 1.0247 1.3075 0.046(18) Uiso 1 1 calc R . . C35 C 1.8744(6) 1.0315(2) 1.2105(5) 0.0508(17) Uani 1 1 d . . . H35 H 1.8990 1.0618 1.2312 0.051(18) Uiso 1 1 calc R . . C36 C 1.9291(7) 1.0100(2) 1.1366(5) 0.0602(19) Uani 1 1 d . . . H36 H 1.9935 1.0252 1.1068 0.08(2) Uiso 1 1 calc R . . C37 C 1.8938(7) 0.9673(2) 1.1044(5) 0.0615(19) Uani 1 1 d . . . H37 H 1.9324 0.9525 1.0521 0.07(2) Uiso 1 1 calc R . . C38 C 1.8025(6) 0.9460(2) 1.1480(4) 0.0451(16) Uani 1 1 d . . . H38 H 1.7758 0.9163 1.1244 0.041(16) Uiso 1 1 calc R . . P3 P 1.21757(19) 0.90089(7) 0.47467(16) 0.0607(5) Uani 1 1 d . . . F1 F 1.285(3) 0.9439(10) 0.510(4) 0.167(19) Uani 0.324(19) 1 d P . . F1' F 1.3080(14) 0.9286(5) 0.5613(9) 0.101(5) Uani 0.676(19) 1 d P . . F2 F 1.1071(5) 0.9336(2) 0.4734(6) 0.169(3) Uani 1 1 d . . . F3 F 1.121(2) 0.8847(17) 0.3729(19) 0.138(18) Uani 0.324(19) 1 d P . . F3' F 1.1446(12) 0.8609(5) 0.4160(12) 0.113(5) Uani 0.676(19) 1 d P . . F4 F 1.316(2) 0.8694(8) 0.541(2) 0.104(10) Uani 0.324(19) 1 d P . . F4' F 1.3283(10) 0.8707(6) 0.460(2) 0.192(10) Uani 0.676(19) 1 d P . . F5 F 1.1629(8) 0.8787(2) 0.5657(5) 0.192(3) Uani 1 1 d . . . F6 F 1.196(7) 0.9308(15) 0.373(3) 0.26(3) Uani 0.324(19) 1 d P . . F6' F 1.2862(12) 0.9175(9) 0.3922(7) 0.166(9) Uani 0.676(19) 1 d P . . P4 P 0.93821(18) 0.83673(7) -0.09277(16) 0.0609(5) Uani 1 1 d . . . F7 F 1.0392(4) 0.84661(16) 0.0076(3) 0.1048(16) Uani 1 1 d . . . F8 F 0.8347(10) 0.8262(8) -0.0275(9) 0.078(6) Uani 0.55(3) 1 d P . . F8' F 0.897(4) 0.7914(11) -0.0327(19) 0.165(15) Uani 0.45(3) 1 d P . . F9 F 0.8346(4) 0.82606(13) -0.1932(3) 0.0828(13) Uani 1 1 d . . . F10 F 1.0262(13) 0.8506(10) -0.1712(10) 0.101(8) Uani 0.55(3) 1 d P . . F10' F 0.993(4) 0.8779(11) -0.133(2) 0.185(18) Uani 0.45(3) 1 d P . . F11 F 0.9798(19) 0.7879(5) -0.0964(19) 0.109(7) Uani 0.55(3) 1 d P . . F11' F 1.041(2) 0.8063(14) -0.132(2) 0.151(14) Uani 0.45(3) 1 d P . . F12 F 0.8831(19) 0.8879(4) -0.1069(17) 0.103(6) Uani 0.55(3) 1 d P . . F12' F 0.8494(19) 0.8643(14) -0.034(2) 0.149(15) Uani 0.45(3) 1 d P . . 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 0.03083(12) 0.02954(12) 0.03127(12) 0.00071(12) 0.00361(8) 0.00134(13) P1 0.0321(8) 0.0356(8) 0.0337(8) -0.0005(8) 0.0051(7) -0.0024(8) P2 0.0321(8) 0.0313(8) 0.0302(8) -0.0018(7) 0.0056(7) 0.0004(7) S1 0.0631(12) 0.0504(10) 0.0614(12) 0.0131(9) 0.0245(10) 0.0114(9) S4 0.0334(8) 0.0423(8) 0.0436(8) 0.0003(8) -0.0002(7) 0.0069(8) S7 0.0500(10) 0.0327(8) 0.0487(10) -0.0026(7) 0.0066(8) 0.0031(8) C2 0.085(6) 0.065(5) 0.045(4) 0.014(3) 0.015(4) 0.020(4) C3 0.058(5) 0.068(5) 0.046(4) 0.015(4) -0.003(4) 0.015(4) C5 0.043(4) 0.058(4) 0.056(5) -0.003(4) 0.016(3) 0.015(4) C6 0.048(4) 0.051(4) 0.067(5) -0.009(4) 0.015(4) 0.017(4) C8 0.065(5) 0.030(3) 0.071(5) 0.005(3) 0.007(4) 0.000(3) C9 0.084(6) 0.038(4) 0.073(5) 0.018(4) 0.026(4) 0.003(4) C10 0.028(3) 0.047(4) 0.049(4) -0.004(3) 0.012(3) 0.006(3) C11 0.048(4) 0.049(4) 0.050(4) 0.004(3) -0.003(3) 0.005(4) C12 0.051(4) 0.042(4) 0.043(4) 0.011(3) 0.005(3) 0.002(4) C13 0.054(4) 0.035(4) 0.047(4) 0.001(3) 0.005(3) 0.009(3) C14 0.040(4) 0.039(3) 0.039(4) -0.007(3) 0.004(3) 0.004(3) C15 0.029(3) 0.038(3) 0.040(4) 0.001(3) 0.003(3) -0.001(3) C16 0.069(5) 0.049(4) 0.062(5) -0.006(4) 0.010(4) -0.014(4) C17 0.102(7) 0.043(5) 0.078(6) -0.003(5) -0.010(5) -0.020(4) C18 0.072(6) 0.057(5) 0.093(7) 0.026(5) -0.005(5) -0.018(5) C19 0.060(5) 0.072(6) 0.084(6) 0.025(5) 0.020(5) 0.000(5) C20 0.049(4) 0.043(4) 0.061(5) 0.005(4) 0.014(4) -0.005(3) C21 0.026(3) 0.041(3) 0.034(3) 0.002(3) 0.002(2) -0.007(3) C22 0.035(3) 0.039(4) 0.035(3) -0.001(3) 0.004(3) -0.003(3) C23 0.041(4) 0.059(5) 0.045(4) -0.001(3) 0.015(3) -0.003(3) C24 0.069(5) 0.055(5) 0.033(4) 0.001(3) 0.011(3) 0.000(4) C25 0.055(4) 0.070(5) 0.035(4) -0.007(4) 0.001(3) -0.003(4) C26 0.035(3) 0.069(4) 0.037(3) -0.007(4) 0.011(3) -0.006(4) C27 0.045(4) 0.035(3) 0.026(3) -0.005(3) 0.007(3) 0.003(3) C28 0.049(4) 0.049(4) 0.036(4) -0.002(3) 0.012(3) 0.000(3) C29 0.068(5) 0.070(5) 0.042(4) 0.003(4) 0.021(4) 0.005(4) C30 0.077(6) 0.093(6) 0.033(4) -0.004(4) -0.001(4) 0.003(5) C31 0.050(5) 0.103(6) 0.044(4) -0.010(4) -0.003(4) -0.007(4) C32 0.044(4) 0.064(4) 0.031(3) -0.001(3) 0.008(3) 0.001(4) C33 0.031(3) 0.037(3) 0.034(3) 0.009(3) 0.001(3) -0.002(3) C34 0.055(4) 0.038(4) 0.047(4) -0.002(3) 0.008(4) -0.008(3) C35 0.046(4) 0.043(4) 0.061(4) 0.008(3) 0.002(4) -0.015(3) C36 0.055(5) 0.077(5) 0.051(5) 0.016(4) 0.016(4) -0.016(4) C37 0.068(5) 0.077(5) 0.046(4) -0.002(4) 0.030(4) -0.007(4) C38 0.053(4) 0.047(4) 0.038(4) -0.002(3) 0.017(3) -0.005(3) P3 0.0484(12) 0.0771(14) 0.0602(13) -0.0113(11) 0.0194(11) -0.0032(12) F1 0.10(2) 0.054(14) 0.34(6) -0.06(3) 0.01(3) -0.015(13) F1' 0.075(6) 0.143(15) 0.078(6) -0.061(6) -0.002(5) 0.013(7) F2 0.085(4) 0.161(6) 0.261(9) 0.017(6) 0.029(5) 0.046(4) F3 0.033(9) 0.32(5) 0.050(14) -0.06(2) -0.012(9) 0.01(2) F3' 0.066(7) 0.148(10) 0.114(11) -0.057(8) -0.012(6) -0.039(7) F4 0.104(17) 0.078(16) 0.107(16) 0.039(12) -0.043(14) -0.006(11) F4' 0.069(6) 0.188(14) 0.31(2) -0.191(15) 0.026(12) 0.031(8) F5 0.225(9) 0.217(7) 0.148(6) 0.051(5) 0.072(6) -0.036(7) F6 0.43(7) 0.21(3) 0.17(3) 0.12(3) 0.16(4) 0.18(4) F6' 0.093(9) 0.36(3) 0.050(5) 0.009(10) 0.039(6) -0.096(12) P4 0.0422(11) 0.0650(14) 0.0772(15) -0.0191(11) 0.0153(11) -0.0156(11) F7 0.059(3) 0.159(4) 0.092(3) -0.034(3) 0.002(3) -0.032(3) F8 0.051(6) 0.122(14) 0.067(7) 0.015(8) 0.023(5) -0.008(8) F8' 0.19(3) 0.14(2) 0.147(17) 0.054(16) -0.028(17) -0.11(2) F9 0.061(3) 0.098(3) 0.085(3) -0.022(2) 0.002(2) -0.020(2) F10 0.058(7) 0.17(2) 0.077(7) -0.020(10) 0.026(5) -0.054(11) F10' 0.25(4) 0.13(2) 0.15(3) 0.046(16) -0.02(2) -0.13(2) F11 0.088(13) 0.063(8) 0.165(18) 0.009(9) -0.010(11) 0.026(9) F11' 0.098(15) 0.20(4) 0.15(2) -0.08(2) 0.032(12) 0.041(18) F12 0.135(13) 0.054(7) 0.113(12) -0.005(6) 0.006(11) -0.022(8) F12' 0.091(14) 0.20(3) 0.15(2) -0.10(2) -0.007(12) 0.080(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.3007(17) . ? Pt1 P2 2.3053(15) . ? Pt1 S4 2.3686(17) . ? Pt1 S7 2.3794(15) . ? Pt1 S1 2.8677(17) . ? P1 C21 1.805(5) . ? P1 C15 1.816(6) . ? P1 C10 1.831(5) . ? P2 C27 1.810(5) . ? P2 C33 1.821(6) . ? P2 C14 1.841(5) . ? S1 C2 1.811(7) . ? S1 C9 1.822(6) . ? S4 C5 1.804(6) . ? S4 C3 1.821(6) . ? S7 C8 1.814(6) . ? S7 C6 1.837(6) . ? C2 C3 1.498(9) . ? C5 C6 1.487(7) . ? C8 C9 1.504(8) . ? C10 C11 1.538(7) . ? C11 C12 1.513(8) . ? C12 C13 1.495(7) . ? C13 C14 1.530(7) . ? C15 C16 1.375(8) . ? C15 C20 1.382(8) . ? C16 C17 1.380(9) . ? C17 C18 1.380(10) . ? C18 C19 1.373(10) . ? C19 C20 1.385(8) . ? C21 C22 1.382(7) . ? C21 C26 1.398(7) . ? C22 C23 1.372(7) . ? C23 C24 1.371(8) . ? C24 C25 1.355(8) . ? C25 C26 1.382(7) . ? C27 C32 1.389(7) . ? C27 C28 1.392(8) . ? C28 C29 1.391(7) . ? C29 C30 1.361(9) . ? C30 C31 1.376(9) . ? C31 C32 1.377(8) . ? C33 C34 1.381(7) . ? C33 C38 1.387(8) . ? C34 C35 1.376(8) . ? C35 C36 1.366(8) . ? C36 C37 1.366(8) . ? C37 C38 1.368(8) . ? P3 F6' 1.484(9) . ? P3 F1 1.50(3) . ? P3 F4' 1.525(10) . ? P3 F2 1.528(6) . ? P3 F3' 1.546(12) . ? P3 F5 1.552(6) . ? P3 F4 1.555(18) . ? P3 F6 1.58(3) . ? P3 F1' 1.580(13) . ? P3 F3 1.60(2) . ? F1 F1' 0.81(5) . ? F1 F6' 1.71(5) . ? F1' F4 1.78(3) . ? F2 F6 1.75(4) . ? F3 F3' 0.91(4) . ? F3 F6 1.59(8) . ? F4 F4' 1.09(2) . ? F4 F5 1.75(3) . ? F4' F6' 1.66(4) . ? F6 F6' 1.03(5) . ? P4 F10' 1.490(18) . ? P4 F11 1.517(13) . ? P4 F8 1.540(11) . ? P4 F12' 1.550(13) . ? P4 F10 1.558(12) . ? P4 F7 1.568(4) . ? P4 F11' 1.577(18) . ? P4 F9 1.589(4) . ? P4 F12 1.627(13) . ? P4 F8' 1.650(16) . ? F8 F12' 1.14(3) . ? F8 F8' 1.24(3) . ? F8' F11 1.32(3) . ? F10 F10' 1.04(3) . ? F10 F11' 1.41(3) . ? F10' F12 1.32(4) . ? F11 F11' 1.02(3) . ? F12 F12' 1.28(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 99.41(5) . . ? P1 Pt1 S4 169.31(5) . . ? P2 Pt1 S4 84.07(5) . . ? P1 Pt1 S7 87.87(6) . . ? P2 Pt1 S7 165.52(6) . . ? S4 Pt1 S7 86.65(5) . . ? P1 Pt1 S1 106.10(6) . . ? P2 Pt1 S1 108.23(5) . . ? S4 Pt1 S1 82.13(6) . . ? S7 Pt1 S1 81.37(5) . . ? C21 P1 C15 105.2(3) . . ? C21 P1 C10 106.2(2) . . ? C15 P1 C10 100.3(3) . . ? C21 P1 Pt1 112.48(18) . . ? C15 P1 Pt1 109.48(18) . . ? C10 P1 Pt1 121.44(19) . . ? C27 P2 C33 105.9(3) . . ? C27 P2 C14 100.0(2) . . ? C33 P2 C14 104.6(3) . . ? C27 P2 Pt1 107.43(17) . . ? C33 P2 Pt1 110.6(2) . . ? C14 P2 Pt1 126.33(19) . . ? C2 S1 C9 100.9(3) . . ? C2 S1 Pt1 95.1(2) . . ? C9 S1 Pt1 99.1(2) . . ? C5 S4 C3 101.2(3) . . ? C5 S4 Pt1 99.8(2) . . ? C3 S4 Pt1 110.4(2) . . ? C8 S7 C6 101.9(3) . . ? C8 S7 Pt1 108.6(2) . . ? C6 S7 Pt1 104.9(2) . . ? C3 C2 S1 118.5(5) . . ? C2 C3 S4 116.0(5) . . ? C6 C5 S4 115.9(4) . . ? C5 C6 S7 113.2(4) . . ? C9 C8 S7 118.4(4) . . ? C8 C9 S1 116.7(4) . . ? C11 C10 P1 118.0(4) . . ? C12 C11 C10 118.1(5) . . ? C13 C12 C11 116.0(5) . . ? C12 C13 C14 117.2(5) . . ? C13 C14 P2 117.8(4) . . ? C16 C15 C20 118.5(6) . . ? C16 C15 P1 123.7(5) . . ? C20 C15 P1 117.7(5) . . ? C15 C16 C17 121.7(7) . . ? C18 C17 C16 119.3(7) . . ? C19 C18 C17 119.7(8) . . ? C18 C19 C20 120.4(8) . . ? C15 C20 C19 120.3(7) . . ? C22 C21 C26 117.9(5) . . ? C22 C21 P1 123.1(4) . . ? C26 C21 P1 119.0(4) . . ? C23 C22 C21 121.1(5) . . ? C24 C23 C22 120.0(6) . . ? C25 C24 C23 120.4(6) . . ? C24 C25 C26 120.3(6) . . ? C25 C26 C21 120.4(6) . . ? C32 C27 C28 119.4(5) . . ? C32 C27 P2 122.6(5) . . ? C28 C27 P2 118.0(5) . . ? C29 C28 C27 119.9(6) . . ? C30 C29 C28 119.6(7) . . ? C29 C30 C31 121.2(7) . . ? C30 C31 C32 119.9(7) . . ? C31 C32 C27 120.0(6) . . ? C34 C33 C38 118.2(6) . . ? C34 C33 P2 120.3(5) . . ? C38 C33 P2 121.5(5) . . ? C35 C34 C33 120.4(6) . . ? C36 C35 C34 119.8(6) . . ? C35 C36 C37 121.1(7) . . ? C36 C37 C38 118.8(7) . . ? C37 C38 C33 121.7(6) . . ? F6' P3 F1 70(2) . . ? F6' P3 F4' 67.2(15) . . ? F1 P3 F4' 101.0(14) . . ? F6' P3 F2 105.2(10) . . ? F1 P3 F2 78.3(13) . . ? F4' P3 F2 171.8(13) . . ? F6' P3 F3' 99.9(8) . . ? F1 P3 F3' 168(2) . . ? F4' P3 F3' 80.0(7) . . ? F2 P3 F3' 99.1(6) . . ? F6' P3 F5 171.5(9) . . ? F1 P3 F5 111(2) . . ? F4' P3 F5 104.5(12) . . ? F2 P3 F5 83.2(4) . . ? F3' P3 F5 79.9(6) . . ? F6' P3 F4 103.1(15) . . ? F1 P3 F4 95.6(16) . . ? F4' P3 F4 41.3(8) . . ? F2 P3 F4 146.7(14) . . ? F3' P3 F4 92.8(12) . . ? F5 P3 F4 68.4(11) . . ? F6' P3 F6 39.3(19) . . ? F1 P3 F6 77(2) . . ? F4' P3 F6 103(2) . . ? F2 P3 F6 68.6(16) . . ? F3' P3 F6 92(3) . . ? F5 P3 F6 149(2) . . ? F4 P3 F6 142(3) . . ? F6' P3 F1' 91.1(8) . . ? F1 P3 F1' 30.4(19) . . ? F4' P3 F1' 90.0(7) . . ? F2 P3 F1' 93.2(6) . . ? F3' P3 F1' 160.7(10) . . ? F5 P3 F1' 86.9(7) . . ? F4 P3 F1' 69.2(9) . . ? F6 P3 F1' 107(3) . . ? F6' P3 F3 80.7(14) . . ? F1 P3 F3 136(3) . . ? F4' P3 F3 97.4(16) . . ? F2 P3 F3 78.0(14) . . ? F3' P3 F3 33.5(16) . . ? F5 P3 F3 102.9(15) . . ? F4 P3 F3 124(2) . . ? F6 P3 F3 60(3) . . ? F1' P3 F3 166(2) . . ? F1' F1 P3 81(3) . . ? F1' F1 F6' 116(3) . . ? P3 F1 F6' 54.6(14) . . ? F1 F1' P3 69(3) . . ? F1 F1' F4 116(3) . . ? P3 F1' F4 54.8(7) . . ? P3 F2 F6 57.0(11) . . ? F3' F3 F6 125(3) . . ? F3' F3 P3 69.7(16) . . ? F6 F3 P3 59(2) . . ? F3 F3' P3 77(2) . . ? F4' F4 P3 67.9(12) . . ? F4' F4 F5 116.5(17) . . ? P3 F4 F5 55.7(10) . . ? F4' F4 F1' 97.0(16) . . ? P3 F4 F1' 56.1(8) . . ? F5 F4 F1' 75.3(15) . . ? F4 F4' P3 70.9(13) . . ? F4 F4' F6' 118.4(19) . . ? P3 F4' F6' 55.3(8) . . ? P3 F5 F4 55.9(6) . . ? F6' F6 P3 65.5(18) . . ? F6' F6 F3 97(3) . . ? P3 F6 F3 60.9(19) . . ? F6' F6 F2 116(3) . . ? P3 F6 F2 54.4(11) . . ? F3 F6 F2 72(3) . . ? F6 F6' P3 75(2) . . ? F6 F6' F4' 127(3) . . ? P3 F6' F4' 57.6(9) . . ? F6 F6' F1 84(3) . . ? P3 F6' F1 55.3(14) . . ? F4' F6' F1 87.3(13) . . ? F10' P4 F11 129.4(16) . . ? F10' P4 F8 136.5(16) . . ? F11 P4 F8 93.9(7) . . ? F10' P4 F12' 93.1(13) . . ? F11 P4 F12' 136.6(14) . . ? F8 P4 F12' 43.5(12) . . ? F10' P4 F10 40.0(14) . . ? F11 P4 F10 90.9(8) . . ? F8 P4 F10 171.2(8) . . ? F12' P4 F10 132.4(14) . . ? F10' P4 F7 83.0(10) . . ? F11 P4 F7 92.3(6) . . ? F8 P4 F7 92.3(5) . . ? F12' P4 F7 83.7(6) . . ? F10 P4 F7 94.8(5) . . ? F10' P4 F11' 90.8(14) . . ? F11 P4 F11' 38.6(10) . . ? F8 P4 F11' 132.3(13) . . ? F12' P4 F11' 169.8(12) . . ? F10 P4 F11' 53.3(11) . . ? F7 P4 F11' 87.5(8) . . ? F10' P4 F9 98.1(10) . . ? F11 P4 F9 87.2(6) . . ? F8 P4 F9 86.7(5) . . ? F12' P4 F9 96.0(6) . . ? F10 P4 F9 86.2(5) . . ? F7 P4 F9 178.9(3) . . ? F11' P4 F9 92.7(8) . . ? F10' P4 F12 49.8(16) . . ? F11 P4 F12 171.4(9) . . ? F8 P4 F12 88.2(6) . . ? F12' P4 F12 47.3(13) . . ? F10 P4 F12 86.0(8) . . ? F7 P4 F12 96.0(6) . . ? F11' P4 F12 139.3(14) . . ? F9 P4 F12 84.6(6) . . ? F10' P4 F8' 170.7(13) . . ? F11 P4 F8' 48.9(10) . . ? F8 P4 F8' 45.5(12) . . ? F12' P4 F8' 87.8(12) . . ? F10 P4 F8' 139.8(13) . . ? F7 P4 F8' 87.9(6) . . ? F11' P4 F8' 86.9(12) . . ? F9 P4 F8' 91.1(6) . . ? F12 P4 F8' 133.7(14) . . ? F12' F8 F8' 137.2(16) . . ? F12' F8 P4 68.7(12) . . ? F8' F8 P4 71.9(11) . . ? F8 F8' F11 122.0(15) . . ? F8 F8' P4 62.5(9) . . ? F11 F8' P4 60.3(8) . . ? F10' F10 F11' 125(2) . . ? F10' F10 P4 66.5(16) . . ? F11' F10 P4 64.0(9) . . ? F10 F10' F12 133(2) . . ? F10 F10' P4 73.5(14) . . ? F12 F10' P4 70.5(15) . . ? F11' F11 F8' 143(2) . . ? F11' F11 P4 73.9(16) . . ? F8' F11 P4 70.9(11) . . ? F11 F11' F10 128(2) . . ? F11 F11' P4 67.6(14) . . ? F10 F11' P4 62.7(11) . . ? F12' F12 F10' 116.6(17) . . ? F12' F12 P4 63.2(9) . . ? F10' F12 P4 59.7(10) . . ? F8 F12' F12 131.2(16) . . ? F8 F12' P4 67.8(9) . . ? F12 F12' P4 69.5(12) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.751 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.136 #4 === END data_grant9 _database_code_CSD 180865 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 F12 P4 Pt S3' _chemical_formula_weight 1111.80 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' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 21.6418(9) _cell_length_b 8.7316(4) _cell_length_c 20.9904(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3966.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 3.942 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24135 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.31 _reflns_number_total 9093 _reflns_number_gt 7631 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0026P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00005(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(4) _refine_ls_number_reflns 9093 _refine_ls_number_parameters 535 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0555 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.141241(7) -0.133460(15) -0.082040(11) 0.01714(4) Uani 1 1 d . . . P1 P 0.05247(5) -0.26170(12) -0.06391(5) 0.0173(3) Uani 1 1 d . . . P2 P 0.14675(6) -0.26179(13) -0.17608(5) 0.0182(3) Uani 1 1 d . . . S1 S 0.11217(7) 0.15327(13) -0.12257(6) 0.0293(3) Uani 1 1 d . . . S4 S 0.24454(5) -0.04037(11) -0.08458(9) 0.0286(3) Uani 1 1 d . . . S7 S 0.13371(6) -0.03396(13) 0.02134(6) 0.0236(3) Uani 1 1 d . . . C2 C 0.1885(3) 0.2409(6) -0.1218(3) 0.0391(14) Uani 1 1 d . . . H2A H 0.1898 0.3193 -0.1546 0.051(11) Uiso 1 1 calc R . . H2B H 0.1943 0.2915 -0.0811 0.051(11) Uiso 1 1 calc R . . C3 C 0.2426(3) 0.1314(6) -0.1325(3) 0.0389(14) Uani 1 1 d . . . H3A H 0.2802 0.1869 -0.1251 0.039(11) Uiso 1 1 calc R . . H3B H 0.2424 0.1014 -0.1765 0.039(11) Uiso 1 1 calc R . . C5 C 0.2564(3) 0.0400(6) -0.0049(3) 0.0379(14) Uani 1 1 d . . . H5A H 0.2987 0.0250 0.0073 0.045(13) Uiso 1 1 calc R . . H5B H 0.2488 0.1483 -0.0063 0.045(13) Uiso 1 1 calc R . . C6 C 0.2152(3) -0.0306(6) 0.0444(2) 0.0343(13) Uani 1 1 d . . . H6A H 0.2193 0.0256 0.0834 0.058(13) Uiso 1 1 calc R . . H6B H 0.2287 -0.1337 0.0522 0.058(13) Uiso 1 1 calc R . . C8 C 0.1166(3) 0.1710(5) 0.0130(2) 0.0295(12) Uani 1 1 d . . . H8A H 0.0934 0.2032 0.0496 0.042(11) Uiso 1 1 calc R . . H8B H 0.1549 0.2263 0.0133 0.042(11) Uiso 1 1 calc R . . C9 C 0.0810(3) 0.2162(5) -0.0463(2) 0.0297(12) Uani 1 1 d . . . H9A H 0.0779 0.3259 -0.0471 0.030(10) Uiso 1 1 calc R . . H9B H 0.0397 0.1767 -0.0424 0.030(10) Uiso 1 1 calc R . . C10 C 0.0372(2) -0.3853(5) -0.1316(2) 0.0193(10) Uani 1 1 d . . . C11 C 0.0797(3) -0.3887(5) -0.1810(2) 0.0185(11) Uani 1 1 d . . . C12 C 0.0707(3) -0.4876(5) -0.2336(2) 0.0271(12) Uani 1 1 d . . . H12 H 0.0990 -0.4897 -0.2670 0.033(18) Uiso 1 1 calc R . . C13 C 0.0192(3) -0.5811(6) -0.2344(3) 0.0298(13) Uani 1 1 d . . . H13 H 0.0134 -0.6480 -0.2684 0.023(13) Uiso 1 1 calc R . . C14 C -0.0240(2) -0.5768(6) -0.1855(2) 0.0277(12) Uani 1 1 d . . . H14 H -0.0589 -0.6387 -0.1873 0.047(17) Uiso 1 1 calc R . . C15 C -0.0150(2) -0.4804(5) -0.1342(2) 0.0251(11) Uani 1 1 d . . . H15 H -0.0436 -0.4786 -0.1012 0.021(13) Uiso 1 1 calc R . . C16 C 0.0513(3) -0.3782(5) 0.0070(2) 0.0191(11) Uani 1 1 d . . . C17 C 0.1056(3) -0.4160(5) 0.0383(2) 0.0243(11) Uani 1 1 d . . . H17 H 0.1432 -0.3835 0.0217 0.004(10) Uiso 1 1 calc R . . C18 C 0.1049(3) -0.5011(6) 0.0938(3) 0.0329(14) Uani 1 1 d . . . H18 H 0.1416 -0.5229 0.1150 0.019(12) Uiso 1 1 calc R . . C19 C 0.0489(3) -0.5538(6) 0.1177(2) 0.0367(14) Uani 1 1 d . . . H19 H 0.0481 -0.6126 0.1546 0.053(18) Uiso 1 1 calc R . . C20 C -0.0042(3) -0.5196(6) 0.0872(3) 0.0345(14) Uani 1 1 d . . . H20 H -0.0413 -0.5558 0.1038 0.033(15) Uiso 1 1 calc R . . C21 C -0.0054(3) -0.4323(5) 0.0322(2) 0.0299(12) Uani 1 1 d . . . H21 H -0.0427 -0.4098 0.0121 0.08(2) Uiso 1 1 calc R . . C22 C -0.0115(2) -0.1289(5) -0.0543(2) 0.0206(10) Uani 1 1 d . . . C23 C -0.0238(2) -0.0679(5) 0.0062(2) 0.0238(11) Uani 1 1 d . . . H23 H -0.0045 -0.1084 0.0421 0.029 Uiso 1 1 calc R . . C24 C -0.0651(2) 0.0541(6) 0.0124(2) 0.0291(12) Uani 1 1 d . . . H24 H -0.0731 0.0959 0.0523 0.07(2) Uiso 1 1 calc R . . C25 C -0.0941(3) 0.1128(6) -0.0414(3) 0.0333(13) Uani 1 1 d . . . H25 H -0.1212 0.1949 -0.0374 0.041(17) Uiso 1 1 calc R . . C26 C -0.0832(3) 0.0507(6) -0.1005(2) 0.0295(13) Uani 1 1 d . . . H26 H -0.1039 0.0887 -0.1360 0.010(13) Uiso 1 1 calc R . . C27 C -0.0413(2) -0.0689(6) -0.1074(2) 0.0251(11) Uani 1 1 d . . . H27 H -0.0332 -0.1088 -0.1476 0.012(13) Uiso 1 1 calc R . . C28 C 0.1415(2) -0.1324(5) -0.2435(2) 0.0239(10) Uani 1 1 d . . . C29 C 0.0846(3) -0.0834(6) -0.2648(2) 0.0270(11) Uani 1 1 d . . . H29 H 0.0487 -0.1293 -0.2496 0.021(13) Uiso 1 1 calc R . . C30 C 0.0806(3) 0.0341(8) -0.3088(3) 0.0382(16) Uani 1 1 d . . . H30 H 0.0421 0.0659 -0.3234 0.032(17) Uiso 1 1 calc R . . C31 C 0.1335(3) 0.1045(7) -0.3313(3) 0.0331(16) Uani 1 1 d . . . H31 H 0.1305 0.1849 -0.3602 0.06(2) Uiso 1 1 calc R . . C32 C 0.1906(3) 0.0551(6) -0.3107(3) 0.0348(13) Uani 1 1 d . . . H32 H 0.2262 0.1023 -0.3259 0.044(17) Uiso 1 1 calc R . . C33 C 0.1952(2) -0.0649(6) -0.2674(2) 0.0278(12) Uani 1 1 d . . . H33 H 0.2338 -0.0999 -0.2545 0.035(16) Uiso 1 1 calc R . . C34 C 0.2161(2) -0.3755(5) -0.1885(2) 0.0206(10) Uani 1 1 d . . . C35 C 0.2295(3) -0.4343(7) -0.2493(2) 0.0281(13) Uani 1 1 d . . . H35 H 0.2043 -0.4097 -0.2837 0.025(14) Uiso 1 1 calc R . . C36 C 0.2800(3) -0.5287(6) -0.2580(3) 0.0341(13) Uani 1 1 d . . . H36 H 0.2878 -0.5718 -0.2977 0.006(10) Uiso 1 1 calc R . . C37 C 0.3201(3) -0.5592(7) -0.2060(3) 0.0364(15) Uani 1 1 d . . . H37 H 0.3549 -0.6201 -0.2118 0.07(3) Uiso 1 1 calc R . . C38 C 0.3073(2) -0.4989(5) -0.1469(3) 0.0289(12) Uani 1 1 d . . . H38 H 0.3339 -0.5179 -0.1129 0.034(15) Uiso 1 1 calc R . . C39 C 0.2545(2) -0.4087(5) -0.1378(2) 0.0215(11) Uani 1 1 d . . . H39 H 0.2452 -0.3711 -0.0975 0.013(11) Uiso 1 1 calc R . . P3 P -0.20337(9) -0.4766(2) 0.05460(9) 0.0432(4) Uani 1 1 d . . . F1 F -0.1786(3) -0.6109(5) 0.0143(2) 0.130(3) Uani 1 1 d . . . F2 F -0.1596(2) -0.3599(6) 0.0190(2) 0.0908(17) Uani 1 1 d . . . F3 F -0.15499(19) -0.4998(5) 0.10854(19) 0.0774(13) Uani 1 1 d . . . F4 F -0.2336(2) -0.3402(4) 0.09382(19) 0.0694(12) Uani 1 1 d . . . F5 F -0.25508(19) -0.4441(4) 0.00193(17) 0.0622(11) Uani 1 1 d . . . F6 F -0.2486(2) -0.5932(4) 0.0897(2) 0.0706(14) Uani 1 1 d . . . P4 P -0.60919(7) 0.03577(17) -0.29187(7) 0.0360(4) Uani 1 1 d . . . F7 F -0.56199(18) 0.0355(5) -0.34979(17) 0.0518(11) Uani 1 1 d . . . F8 F -0.64723(18) -0.0987(4) -0.32402(18) 0.0596(10) Uani 1 1 d . . . F9 F -0.57122(15) 0.1742(3) -0.25909(14) 0.0407(8) Uani 1 1 d . . . F10 F -0.65077(16) 0.1593(4) -0.3295(2) 0.0436(10) Uani 1 1 d . . . F11 F -0.56706(17) -0.0847(4) -0.25485(16) 0.0530(9) Uani 1 1 d . . . F12 F -0.65688(16) 0.0381(4) -0.23393(15) 0.0496(9) Uani 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 0.01679(7) 0.01701(6) 0.01764(7) -0.00267(12) 0.00217(14) -0.00079(7) P1 0.0173(6) 0.0187(5) 0.0158(7) -0.0007(4) 0.0000(4) -0.0007(5) P2 0.0180(6) 0.0198(5) 0.0169(6) -0.0017(4) 0.0037(5) -0.0011(5) S1 0.0347(8) 0.0204(6) 0.0327(7) 0.0008(5) -0.0022(6) -0.0021(6) S4 0.0198(5) 0.0259(5) 0.0402(7) -0.0118(8) 0.0048(9) -0.0049(4) S7 0.0253(7) 0.0242(6) 0.0213(6) -0.0067(5) 0.0006(6) 0.0000(5) C2 0.049(4) 0.026(3) 0.042(3) -0.003(2) 0.011(3) -0.018(3) C3 0.041(4) 0.032(3) 0.044(3) -0.007(3) 0.009(3) -0.017(3) C5 0.021(3) 0.040(3) 0.053(4) -0.017(3) -0.004(3) 0.002(3) C6 0.032(3) 0.038(3) 0.033(3) -0.010(2) -0.013(3) 0.008(3) C8 0.033(3) 0.026(3) 0.030(3) -0.009(2) 0.006(3) 0.004(2) C9 0.029(3) 0.018(2) 0.043(3) -0.004(2) 0.002(3) 0.002(2) C10 0.024(3) 0.019(2) 0.015(2) 0.0007(19) -0.003(2) 0.005(2) C11 0.017(3) 0.019(2) 0.019(3) -0.002(2) -0.001(2) 0.004(2) C12 0.034(3) 0.023(3) 0.024(3) -0.004(2) 0.002(3) 0.001(2) C13 0.037(3) 0.018(2) 0.034(3) -0.005(2) -0.013(3) -0.003(2) C14 0.023(3) 0.024(2) 0.036(3) -0.002(2) -0.005(2) -0.005(2) C15 0.017(2) 0.029(3) 0.030(3) -0.001(2) 0.001(2) -0.003(2) C16 0.023(3) 0.017(2) 0.017(3) -0.002(2) 0.002(2) 0.004(2) C17 0.032(3) 0.019(2) 0.022(3) 0.002(2) 0.002(2) 0.002(2) C18 0.041(4) 0.032(3) 0.026(3) 0.002(2) -0.010(3) 0.011(3) C19 0.061(4) 0.028(3) 0.020(3) 0.007(2) 0.010(3) 0.009(3) C20 0.039(4) 0.032(3) 0.032(3) 0.009(3) 0.016(3) 0.000(3) C21 0.032(3) 0.029(3) 0.029(3) 0.007(2) 0.009(3) 0.007(2) C22 0.018(2) 0.021(2) 0.023(2) -0.001(2) 0.007(2) -0.008(2) C23 0.023(3) 0.029(3) 0.019(2) -0.002(2) 0.003(2) 0.001(2) C24 0.026(3) 0.032(3) 0.030(3) -0.006(2) 0.010(2) -0.001(2) C25 0.020(3) 0.027(3) 0.052(4) -0.002(3) 0.006(3) 0.003(2) C26 0.025(3) 0.031(3) 0.033(3) 0.006(2) -0.001(2) 0.006(2) C27 0.021(3) 0.028(3) 0.026(3) -0.001(2) -0.002(2) 0.006(2) C28 0.029(3) 0.024(2) 0.019(2) 0.0001(19) 0.002(2) 0.000(2) C29 0.024(3) 0.032(3) 0.025(3) 0.004(2) 0.004(2) -0.002(2) C30 0.040(4) 0.043(4) 0.032(3) 0.008(3) -0.008(3) 0.006(3) C31 0.045(4) 0.030(3) 0.024(3) 0.005(2) 0.001(3) -0.010(3) C32 0.040(4) 0.034(3) 0.030(3) 0.006(2) 0.008(3) -0.007(3) C33 0.023(3) 0.033(3) 0.027(3) 0.004(2) 0.003(2) 0.000(2) C34 0.023(3) 0.021(2) 0.018(2) 0.0007(19) 0.007(2) -0.003(2) C35 0.033(3) 0.034(3) 0.017(3) -0.004(2) 0.001(2) 0.000(3) C36 0.039(4) 0.031(3) 0.032(3) -0.007(3) 0.010(3) 0.000(3) C37 0.027(3) 0.029(3) 0.054(4) -0.003(3) 0.013(3) 0.006(3) C38 0.025(3) 0.020(2) 0.041(3) 0.003(2) 0.001(3) -0.002(2) C39 0.019(3) 0.016(2) 0.029(3) -0.004(2) 0.001(2) -0.0017(19) P3 0.0383(10) 0.0490(10) 0.0423(10) 0.0007(8) -0.0019(9) 0.0063(9) F1 0.223(7) 0.107(4) 0.062(3) -0.017(3) 0.007(4) 0.115(5) F2 0.040(2) 0.132(4) 0.100(4) 0.066(3) 0.015(3) 0.001(3) F3 0.056(3) 0.115(4) 0.061(3) 0.024(2) -0.008(2) -0.001(3) F4 0.083(3) 0.058(2) 0.067(3) -0.014(2) 0.014(2) 0.003(2) F5 0.066(3) 0.060(2) 0.061(2) 0.0067(19) -0.023(2) 0.007(2) F6 0.076(4) 0.054(3) 0.082(3) 0.016(2) -0.013(3) -0.016(3) P4 0.0309(8) 0.0451(9) 0.0319(8) 0.0029(6) 0.0001(7) 0.0045(8) F7 0.044(3) 0.079(3) 0.033(2) -0.0020(19) 0.0008(19) 0.013(2) F8 0.067(3) 0.053(2) 0.059(2) -0.0016(18) -0.012(2) -0.008(2) F9 0.0352(18) 0.0492(19) 0.0377(17) -0.0048(14) -0.0103(16) 0.0038(16) F10 0.036(2) 0.049(2) 0.046(2) 0.0068(18) -0.0128(18) 0.0108(17) F11 0.053(2) 0.058(2) 0.049(2) 0.0120(17) -0.0005(19) 0.0154(19) F12 0.040(2) 0.072(2) 0.0370(19) 0.0067(17) 0.0096(17) 0.0070(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2559(12) . ? Pt1 P2 2.2729(11) . ? Pt1 S7 2.3432(11) . ? Pt1 S4 2.3794(11) . ? Pt1 S1 2.7180(12) . ? P1 C16 1.803(5) . ? P1 C10 1.814(5) . ? P1 C22 1.818(5) . ? P2 C28 1.814(5) . ? P2 C34 1.817(5) . ? P2 C11 1.829(5) . ? S1 C2 1.822(5) . ? S1 C9 1.823(5) . ? S4 C3 1.807(5) . ? S4 C5 1.831(6) . ? S7 C6 1.828(5) . ? S7 C8 1.836(5) . ? C2 C3 1.527(8) . ? C5 C6 1.499(8) . ? C8 C9 1.516(7) . ? C10 C11 1.387(7) . ? C10 C15 1.402(7) . ? C11 C12 1.415(7) . ? C12 C13 1.381(7) . ? C13 C14 1.389(7) . ? C14 C15 1.381(7) . ? C16 C17 1.388(7) . ? C16 C21 1.417(7) . ? C17 C18 1.381(7) . ? C18 C19 1.389(8) . ? C19 C20 1.349(8) . ? C20 C21 1.384(7) . ? C22 C27 1.389(6) . ? C22 C23 1.404(6) . ? C23 C24 1.396(7) . ? C24 C25 1.390(7) . ? C25 C26 1.374(7) . ? C26 C27 1.390(7) . ? C28 C29 1.379(7) . ? C28 C33 1.397(7) . ? C29 C30 1.383(8) . ? C30 C31 1.382(9) . ? C31 C32 1.378(8) . ? C32 C33 1.390(7) . ? C34 C39 1.381(7) . ? C34 C35 1.405(7) . ? C35 C36 1.383(8) . ? C36 C37 1.420(8) . ? C37 C38 1.375(8) . ? C38 C39 1.402(7) . ? P3 F1 1.543(4) . ? P3 F3 1.556(4) . ? P3 F2 1.578(4) . ? P3 F4 1.589(4) . ? P3 F6 1.593(5) . ? P3 F5 1.599(4) . ? P4 F8 1.585(4) . ? P4 F7 1.588(4) . ? P4 F11 1.594(4) . ? P4 F12 1.595(4) . ? P4 F10 1.612(4) . ? P4 F9 1.615(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 86.93(4) . . ? P1 Pt1 S7 88.20(4) . . ? P2 Pt1 S7 172.19(4) . . ? P1 Pt1 S4 166.77(5) . . ? P2 Pt1 S4 95.72(5) . . ? S7 Pt1 S4 87.68(5) . . ? P1 Pt1 S1 108.24(4) . . ? P2 Pt1 S1 101.21(4) . . ? S7 Pt1 S1 86.11(4) . . ? S4 Pt1 S1 84.02(4) . . ? C16 P1 C10 107.9(2) . . ? C16 P1 C22 104.9(2) . . ? C10 P1 C22 109.1(2) . . ? C16 P1 Pt1 115.58(19) . . ? C10 P1 Pt1 108.59(17) . . ? C22 P1 Pt1 110.54(14) . . ? C28 P2 C34 106.2(2) . . ? C28 P2 C11 106.5(2) . . ? C34 P2 C11 108.4(2) . . ? C28 P2 Pt1 111.55(15) . . ? C34 P2 Pt1 115.93(16) . . ? C11 P2 Pt1 107.81(17) . . ? C2 S1 C9 101.7(2) . . ? C2 S1 Pt1 100.05(18) . . ? C9 S1 Pt1 95.08(16) . . ? C3 S4 C5 101.2(3) . . ? C3 S4 Pt1 105.9(2) . . ? C5 S4 Pt1 104.00(19) . . ? C6 S7 C8 101.8(2) . . ? C6 S7 Pt1 100.58(17) . . ? C8 S7 Pt1 106.68(16) . . ? C3 C2 S1 115.5(3) . . ? C2 C3 S4 117.1(4) . . ? C6 C5 S4 112.9(4) . . ? C5 C6 S7 113.4(4) . . ? C9 C8 S7 115.8(3) . . ? C8 C9 S1 117.0(4) . . ? C11 C10 C15 119.5(4) . . ? C11 C10 P1 118.5(4) . . ? C15 C10 P1 122.0(4) . . ? C10 C11 C12 120.3(5) . . ? C10 C11 P2 118.2(4) . . ? C12 C11 P2 121.5(4) . . ? C13 C12 C11 118.8(5) . . ? C12 C13 C14 121.2(5) . . ? C15 C14 C13 119.9(5) . . ? C14 C15 C10 120.3(5) . . ? C17 C16 C21 118.5(5) . . ? C17 C16 P1 120.9(4) . . ? C21 C16 P1 120.6(4) . . ? C18 C17 C16 121.2(5) . . ? C17 C18 C19 119.4(6) . . ? C20 C19 C18 120.0(5) . . ? C19 C20 C21 122.2(6) . . ? C20 C21 C16 118.6(6) . . ? C27 C22 C23 119.7(4) . . ? C27 C22 P1 120.4(3) . . ? C23 C22 P1 119.1(4) . . ? C24 C23 C22 119.6(5) . . ? C25 C24 C23 119.7(5) . . ? C26 C25 C24 120.7(5) . . ? C25 C26 C27 120.1(5) . . ? C22 C27 C26 120.2(4) . . ? C29 C28 C33 119.7(4) . . ? C29 C28 P2 120.1(4) . . ? C33 C28 P2 119.4(4) . . ? C28 C29 C30 120.1(5) . . ? C31 C30 C29 120.5(6) . . ? C32 C31 C30 119.7(6) . . ? C31 C32 C33 120.4(5) . . ? C32 C33 C28 119.5(5) . . ? C39 C34 C35 119.9(5) . . ? C39 C34 P2 120.0(3) . . ? C35 C34 P2 120.0(4) . . ? C36 C35 C34 120.1(5) . . ? C35 C36 C37 119.5(5) . . ? C38 C37 C36 120.0(5) . . ? C37 C38 C39 120.1(5) . . ? C34 C39 C38 120.3(4) . . ? F1 P3 F3 93.8(3) . . ? F1 P3 F2 91.3(3) . . ? F3 P3 F2 91.4(3) . . ? F1 P3 F4 175.9(3) . . ? F3 P3 F4 89.9(3) . . ? F2 P3 F4 90.4(3) . . ? F1 P3 F6 88.9(3) . . ? F3 P3 F6 89.6(2) . . ? F2 P3 F6 178.9(3) . . ? F4 P3 F6 89.2(2) . . ? F1 P3 F5 90.0(3) . . ? F3 P3 F5 176.3(3) . . ? F2 P3 F5 88.7(2) . . ? F4 P3 F5 86.4(2) . . ? F6 P3 F5 90.2(2) . . ? F8 P4 F7 90.4(2) . . ? F8 P4 F11 90.9(2) . . ? F7 P4 F11 90.3(2) . . ? F8 P4 F12 89.9(2) . . ? F7 P4 F12 179.3(2) . . ? F11 P4 F12 90.38(19) . . ? F8 P4 F10 89.8(2) . . ? F7 P4 F10 89.1(2) . . ? F11 P4 F10 179.1(2) . . ? F12 P4 F10 90.2(2) . . ? F8 P4 F9 179.2(2) . . ? F7 P4 F9 90.0(2) . . ? F11 P4 F9 89.73(19) . . ? F12 P4 F9 89.71(19) . . ? F10 P4 F9 89.54(18) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.108 _refine_diff_density_min -2.078 _refine_diff_density_rms 0.101 #5 === END data_grant5 _database_code_CSD 180866 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H36 F12 N O2 P4 Pt S3' _chemical_formula_weight 1121.78 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.58810(10) _cell_length_b 16.3447(2) _cell_length_c 18.681 _cell_angle_alpha 90.00 _cell_angle_beta 105.5280(10) _cell_angle_gamma 90.00 _cell_volume 4291.73(6) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2204 _exptl_absorpt_coefficient_mu 3.648 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.2756 _exptl_absorpt_correction_T_max 0.5760 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27078 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.35 _reflns_number_total 10157 _reflns_number_gt 8441 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+3.1905P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00246(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10157 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.004 _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 0.763848(9) 0.852061(8) 0.036898(7) 0.02894(6) Uani 1 1 d . . . S1 S 0.90087(7) 0.93850(6) 0.00404(6) 0.0423(2) Uani 1 1 d . . . C2 C 0.8408(3) 1.0365(2) -0.0105(3) 0.0482(10) Uani 1 1 d . . . H2A H 0.8539 1.0645 0.0376 0.054(9) Uiso 1 1 calc R . . H2B H 0.8696 1.0693 -0.0427 0.054(9) Uiso 1 1 calc R . . C3 C 0.7345(3) 1.0364(2) -0.0441(2) 0.0429(9) Uani 1 1 d . . . H3A H 0.7208 1.0174 -0.0956 0.034(7) Uiso 1 1 calc R . . H3B H 0.7108 1.0925 -0.0448 0.034(7) Uiso 1 1 calc R . . S4 S 0.67069(7) 0.97164(6) 0.00607(5) 0.0365(2) Uani 1 1 d . . . C5 C 0.5624(3) 0.9481(3) -0.0658(2) 0.0447(9) Uani 1 1 d . . . H5A H 0.5246 0.9108 -0.0441 0.048(8) Uiso 1 1 calc R . . H5B H 0.5259 0.9990 -0.0777 0.048(8) Uiso 1 1 calc R . . C6 C 0.5695(3) 0.9108(3) -0.1382(2) 0.0509(10) Uani 1 1 d . . . H6A H 0.6101 0.9464 -0.1590 0.060(10) Uiso 1 1 calc R . . H6B H 0.5059 0.9114 -0.1730 0.060(10) Uiso 1 1 calc R . . C7 C 0.6083(3) 0.8242(3) -0.1351(2) 0.0485(10) Uani 1 1 d . . . H7A H 0.5977 0.8050 -0.1863 0.056(9) Uiso 1 1 calc R . . H7B H 0.5695 0.7896 -0.1117 0.056(9) Uiso 1 1 calc R . . S8 S 0.73212(7) 0.80543(6) -0.08733(5) 0.0367(2) Uani 1 1 d . . . C9 C 0.7958(3) 0.8725(3) -0.1357(2) 0.0459(10) Uani 1 1 d . . . H9A H 0.8045 0.8437 -0.1794 0.056(9) Uiso 1 1 calc R . . H9B H 0.7565 0.9209 -0.1533 0.056(9) Uiso 1 1 calc R . . C10 C 0.8919(3) 0.9002(3) -0.0886(2) 0.0476(10) Uani 1 1 d . . . H10A H 0.9148 0.9432 -0.1160 0.054(9) Uiso 1 1 calc R . . H10B H 0.9359 0.8539 -0.0840 0.054(9) Uiso 1 1 calc R . . P1 P 0.84326(6) 0.73287(6) 0.07162(5) 0.03081(18) Uani 1 1 d . . . P2 P 0.77354(7) 0.86872(6) 0.15950(5) 0.0362(2) Uani 1 1 d . . . C11 C 0.8980(3) 0.7388(3) 0.1714(2) 0.0428(9) Uani 1 1 d . . . H11A H 0.9171 0.6842 0.1914 0.058(9) Uiso 1 1 calc R . . H11B H 0.9547 0.7736 0.1815 0.058(9) Uiso 1 1 calc R . . C12 C 0.8250(3) 0.7750(3) 0.2077(2) 0.0472(10) Uani 1 1 d . . . H12A H 0.8556 0.7873 0.2599 0.046(8) Uiso 1 1 calc R . . H12B H 0.7743 0.7350 0.2058 0.046(8) Uiso 1 1 calc R . . C13 C 0.7697(3) 0.6420(2) 0.0572(2) 0.0385(8) Uani 1 1 d . . . C14 C 0.8112(3) 0.5653(3) 0.0701(3) 0.0541(11) Uani 1 1 d . . . H14 H 0.8807 0.5602 0.0852 0.051(12) Uiso 1 1 calc R . . C15 C 0.7552(4) 0.4963(3) 0.0619(3) 0.0662(14) Uani 1 1 d . . . H15 H 0.7850 0.4422 0.0712 0.071(15) Uiso 1 1 calc R . . C16 C 0.6584(4) 0.5029(4) 0.0409(4) 0.092(2) Uani 1 1 d . . . H16 H 0.6188 0.4538 0.0369 0.12(2) Uiso 1 1 calc R . . C17 C 0.6164(4) 0.5784(4) 0.0254(5) 0.098(2) Uani 1 1 d . . . H17 H 0.5469 0.5830 0.0088 0.12(2) Uiso 1 1 calc R . . C18 C 0.6719(3) 0.6479(3) 0.0332(3) 0.0616(14) Uani 1 1 d . . . H18 H 0.6418 0.7016 0.0217 0.084(18) Uiso 1 1 calc R . . C19 C 0.9354(2) 0.7151(2) 0.0251(2) 0.0337(7) Uani 1 1 d . . . C20 C 1.0239(3) 0.7524(2) 0.0507(2) 0.0407(8) Uani 1 1 d . . . H20 H 1.0392 0.7836 0.0972 0.061(14) Uiso 1 1 calc R . . C21 C 1.0904(3) 0.7452(3) 0.0101(3) 0.0491(10) Uani 1 1 d . . . H21 H 1.1532 0.7705 0.0286 0.051(12) Uiso 1 1 calc R . . C22 C 1.0690(3) 0.7028(3) -0.0556(3) 0.0541(11) Uani 1 1 d . . . H22 H 1.1161 0.6988 -0.0844 0.073(16) Uiso 1 1 calc R . . C23 C 0.9813(3) 0.6658(3) -0.0815(3) 0.0541(11) Uani 1 1 d . . . H23 H 0.9665 0.6352 -0.1283 0.056(14) Uiso 1 1 calc R . . C24 C 0.9141(3) 0.6717(3) -0.0416(2) 0.0433(9) Uani 1 1 d . . . H24 H 0.8518 0.6455 -0.0602 0.063(15) Uiso 1 1 calc R . . C25 C 0.6605(3) 0.8799(3) 0.1818(2) 0.0425(9) Uani 1 1 d . . . C26 C 0.5829(3) 0.8360(3) 0.1410(3) 0.0536(11) Uani 1 1 d . . . H26 H 0.5878 0.8038 0.0979 0.073(16) Uiso 1 1 calc R . . C27 C 0.4985(4) 0.8378(4) 0.1611(3) 0.0667(14) Uani 1 1 d . . . H27 H 0.4439 0.8059 0.1327 0.092(19) Uiso 1 1 calc R . . C28 C 0.4903(4) 0.8835(4) 0.2204(3) 0.0707(15) Uani 1 1 d . . . H28 H 0.4299 0.8849 0.2339 0.071(15) Uiso 1 1 calc R . . C29 C 0.5665(4) 0.9272(4) 0.2607(3) 0.0699(15) Uani 1 1 d . . . H29 H 0.5603 0.9600 0.3031 0.069(15) Uiso 1 1 calc R . . C30 C 0.6524(3) 0.9257(3) 0.2424(3) 0.0588(12) Uani 1 1 d . . . H30 H 0.7070 0.9567 0.2720 0.065(15) Uiso 1 1 calc R . . C31 C 0.8456(3) 0.9545(3) 0.2040(2) 0.0507(10) Uani 1 1 d . . . C32 C 0.8134(4) 1.0333(3) 0.1850(3) 0.0649(13) Uani 1 1 d . . . H32 H 0.7526 1.0416 0.1477 0.079(18) Uiso 1 1 calc R . . C33 C 0.8663(5) 1.1010(4) 0.2181(4) 0.092(2) Uani 1 1 d . . . H33 H 0.8430 1.1566 0.2045 0.09(2) Uiso 1 1 calc R . . C34 C 0.9522(6) 1.0883(5) 0.2705(5) 0.119(3) Uani 1 1 d . . . H34 H 0.9909 1.1352 0.2933 0.13(3) Uiso 1 1 calc R . . C35 C 0.9834(5) 1.0101(6) 0.2907(5) 0.124(3) Uani 1 1 d . . . H35 H 1.0427 1.0017 0.3297 0.12(3) Uiso 1 1 calc R . . C36 C 0.9317(4) 0.9432(4) 0.2564(4) 0.092(2) Uani 1 1 d . . . H36 H 0.9561 0.8877 0.2693 0.09(2) Uiso 1 1 calc R . . P3 P 0.64275(9) 0.24430(8) 0.06554(7) 0.0534(3) Uani 1 1 d . . . F1 F 0.6588(3) 0.2982(3) 0.0007(2) 0.1232(16) Uani 1 1 d . . . F2 F 0.5771(4) 0.1839(4) 0.0102(2) 0.151(2) Uani 1 1 d . . . F3 F 0.6282(3) 0.1889(2) 0.13130(17) 0.0846(10) Uani 1 1 d . . . F4 F 0.7151(3) 0.2992(3) 0.1221(2) 0.1140(15) Uani 1 1 d . . . F5 F 0.7304(3) 0.1890(3) 0.0612(3) 0.1222(15) Uani 1 1 d . . . F6 F 0.5607(4) 0.2978(4) 0.0737(4) 0.186(3) Uani 1 1 d . . . P4 P 0.70517(9) 0.62859(9) -0.26368(7) 0.0573(3) Uani 1 1 d . . . F7 F 0.6208(3) 0.5787(4) -0.3129(3) 0.165(3) Uani 1 1 d . . . F8 F 0.6363(3) 0.7026(3) -0.2667(2) 0.144(2) Uani 1 1 d . . . F9 F 0.6850(3) 0.6008(3) -0.1894(2) 0.1198(14) Uani 1 1 d . . . F10 F 0.7763(3) 0.5557(2) -0.2627(3) 0.1097(14) Uani 1 1 d . . . F11 F 0.7279(3) 0.6577(2) -0.3387(2) 0.0994(13) Uani 1 1 d . . . F12 F 0.7893(3) 0.6818(3) -0.2184(2) 0.1074(13) Uani 1 1 d . . . N N 1.1222(5) 0.5755(4) 0.1434(4) 0.0912(17) Uani 1 1 d . . . O1 O 1.0753(6) 0.5349(5) 0.0924(5) 0.190(4) Uani 1 1 d . . . O2 O 1.0941(7) 0.5980(5) 0.1905(4) 0.184(4) Uani 1 1 d . . . C37 C 1.2160(6) 0.5928(7) 0.1359(7) 0.160(5) Uani 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 0.03300(8) 0.02825(8) 0.02722(8) 0.00181(5) 0.01092(5) 0.00078(5) S1 0.0385(5) 0.0395(5) 0.0507(6) 0.0080(4) 0.0149(4) -0.0050(4) C2 0.052(2) 0.033(2) 0.063(3) 0.0018(18) 0.022(2) -0.0076(17) C3 0.054(2) 0.032(2) 0.046(2) 0.0046(15) 0.0189(19) 0.0024(16) S4 0.0428(5) 0.0329(5) 0.0369(5) 0.0025(4) 0.0160(4) 0.0064(4) C5 0.0360(19) 0.047(2) 0.051(2) 0.0078(18) 0.0121(17) 0.0082(17) C6 0.043(2) 0.060(3) 0.045(2) 0.002(2) 0.0026(18) 0.011(2) C7 0.047(2) 0.053(3) 0.040(2) -0.0051(19) 0.0018(18) 0.0024(19) S8 0.0433(5) 0.0356(5) 0.0313(4) -0.0017(3) 0.0102(4) 0.0032(4) C9 0.060(3) 0.048(2) 0.034(2) 0.0067(17) 0.0204(18) 0.0098(19) C10 0.048(2) 0.048(2) 0.056(3) 0.0108(19) 0.030(2) 0.0069(18) P1 0.0314(4) 0.0294(4) 0.0317(4) 0.0035(3) 0.0085(3) 0.0008(3) P2 0.0375(5) 0.0445(5) 0.0281(5) 0.0002(4) 0.0115(4) 0.0026(4) C11 0.043(2) 0.050(2) 0.0327(19) 0.0072(16) 0.0053(16) 0.0062(17) C12 0.053(2) 0.059(3) 0.032(2) 0.0121(18) 0.0141(17) 0.008(2) C13 0.038(2) 0.032(2) 0.047(2) 0.0055(15) 0.0134(16) -0.0021(14) C14 0.047(2) 0.036(2) 0.076(3) 0.013(2) 0.010(2) 0.0002(18) C15 0.067(3) 0.033(2) 0.095(4) 0.012(2) 0.016(3) -0.003(2) C16 0.067(4) 0.048(3) 0.153(6) 0.009(4) 0.018(4) -0.021(3) C17 0.042(3) 0.053(3) 0.190(8) 0.017(4) 0.014(4) -0.012(2) C18 0.041(2) 0.042(3) 0.098(4) 0.011(2) 0.013(2) -0.0021(18) C19 0.0332(17) 0.0310(18) 0.0365(19) 0.0045(14) 0.0089(14) 0.0032(14) C20 0.0379(19) 0.038(2) 0.046(2) -0.0018(16) 0.0107(16) -0.0003(16) C21 0.036(2) 0.045(2) 0.069(3) 0.008(2) 0.0185(19) 0.0001(17) C22 0.047(2) 0.059(3) 0.064(3) 0.002(2) 0.029(2) 0.008(2) C23 0.055(3) 0.065(3) 0.046(2) -0.011(2) 0.020(2) 0.006(2) C24 0.040(2) 0.046(2) 0.045(2) -0.0063(18) 0.0124(17) -0.0013(17) C25 0.044(2) 0.054(2) 0.034(2) 0.0054(17) 0.0180(17) 0.0074(18) C26 0.045(2) 0.077(3) 0.042(2) -0.006(2) 0.0152(19) -0.001(2) C27 0.046(3) 0.104(4) 0.051(3) 0.006(3) 0.015(2) -0.004(3) C28 0.052(3) 0.111(5) 0.059(3) 0.017(3) 0.033(2) 0.016(3) C29 0.068(3) 0.098(4) 0.055(3) -0.006(3) 0.036(3) 0.012(3) C30 0.053(3) 0.081(4) 0.046(2) -0.010(2) 0.019(2) 0.000(2) C31 0.045(2) 0.065(3) 0.044(2) -0.015(2) 0.0148(18) -0.003(2) C32 0.078(3) 0.057(3) 0.055(3) -0.010(2) 0.009(3) -0.012(3) C33 0.112(5) 0.063(4) 0.096(5) -0.026(3) 0.018(4) -0.018(4) C34 0.094(5) 0.099(6) 0.156(8) -0.072(6) 0.020(5) -0.032(5) C35 0.064(4) 0.121(7) 0.156(8) -0.073(6) -0.021(4) -0.001(4) C36 0.060(3) 0.090(5) 0.112(5) -0.051(4) -0.004(3) 0.009(3) P3 0.0561(7) 0.0520(7) 0.0554(7) -0.0070(5) 0.0206(6) -0.0117(5) F1 0.166(4) 0.124(4) 0.084(3) 0.029(2) 0.042(3) -0.043(3) F2 0.182(5) 0.187(5) 0.065(2) -0.012(3) 0.000(3) -0.125(4) F3 0.108(3) 0.087(2) 0.0620(19) -0.0002(17) 0.0283(18) -0.033(2) F4 0.137(3) 0.114(3) 0.100(3) -0.049(2) 0.048(3) -0.073(3) F5 0.119(3) 0.097(3) 0.176(4) -0.018(3) 0.085(3) 0.012(3) F6 0.128(4) 0.150(5) 0.321(8) 0.094(5) 0.134(5) 0.080(4) P4 0.0482(7) 0.0701(8) 0.0495(7) -0.0196(6) 0.0060(5) 0.0127(6) F7 0.107(3) 0.243(7) 0.152(4) -0.128(4) 0.048(3) -0.086(4) F8 0.142(4) 0.176(5) 0.095(3) -0.039(3) 0.000(3) 0.107(4) F9 0.134(4) 0.148(4) 0.095(3) 0.007(3) 0.062(3) -0.015(3) F10 0.124(3) 0.081(3) 0.140(4) 0.026(2) 0.062(3) 0.048(2) F11 0.131(3) 0.112(3) 0.059(2) -0.0015(18) 0.031(2) 0.024(2) F12 0.095(3) 0.139(4) 0.086(3) -0.045(3) 0.020(2) -0.035(3) N 0.130(5) 0.063(3) 0.076(4) 0.013(3) 0.021(4) 0.026(3) O1 0.214(8) 0.119(6) 0.193(8) -0.012(5) -0.020(6) 0.001(5) O2 0.287(10) 0.175(7) 0.126(5) 0.056(5) 0.115(6) 0.124(7) C37 0.089(6) 0.194(11) 0.202(11) 0.104(9) 0.048(6) 0.031(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2707(9) . ? Pt1 P2 2.2730(9) . ? Pt1 S4 2.3621(9) . ? Pt1 S8 2.3676(9) . ? Pt1 S1 2.6505(9) . ? S1 C2 1.811(4) . ? S1 C10 1.812(4) . ? C2 C3 1.510(6) . ? C3 S4 1.824(4) . ? S4 C5 1.819(4) . ? C5 C6 1.513(6) . ? C6 C7 1.520(6) . ? C7 S8 1.814(4) . ? S8 C9 1.825(4) . ? C9 C10 1.512(6) . ? P1 C19 1.809(4) . ? P1 C13 1.810(4) . ? P1 C11 1.823(4) . ? P2 C31 1.815(5) . ? P2 C25 1.815(4) . ? P2 C12 1.832(4) . ? C11 C12 1.527(6) . ? C13 C18 1.380(6) . ? C13 C14 1.384(5) . ? C14 C15 1.378(6) . ? C15 C16 1.365(7) . ? C16 C17 1.374(8) . ? C17 C18 1.380(7) . ? C19 C20 1.392(5) . ? C19 C24 1.394(5) . ? C20 C21 1.387(6) . ? C21 C22 1.371(7) . ? C22 C23 1.380(6) . ? C23 C24 1.385(6) . ? C25 C26 1.384(6) . ? C25 C30 1.388(6) . ? C26 C27 1.381(7) . ? C27 C28 1.367(8) . ? C28 C29 1.365(8) . ? C29 C30 1.385(6) . ? C31 C36 1.382(7) . ? C31 C32 1.383(7) . ? C32 C33 1.396(7) . ? C33 C34 1.383(10) . ? C34 C35 1.375(12) . ? C35 C36 1.385(9) . ? P3 F6 1.522(4) . ? P3 F2 1.559(4) . ? P3 F4 1.562(3) . ? P3 F1 1.565(4) . ? P3 F3 1.586(3) . ? P3 F5 1.586(4) . ? P4 F7 1.555(4) . ? P4 F12 1.557(4) . ? P4 F9 1.562(4) . ? P4 F8 1.563(4) . ? P4 F10 1.577(4) . ? P4 F11 1.596(4) . ? N O2 1.126(7) . ? N O1 1.212(8) . ? N C37 1.440(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 85.73(3) . . ? P1 Pt1 S4 174.75(3) . . ? P2 Pt1 S4 91.32(3) . . ? P1 Pt1 S8 87.40(3) . . ? P2 Pt1 S8 165.77(4) . . ? S4 Pt1 S8 94.51(3) . . ? P1 Pt1 S1 99.48(3) . . ? P2 Pt1 S1 108.79(4) . . ? S4 Pt1 S1 85.58(3) . . ? S8 Pt1 S1 84.62(3) . . ? C2 S1 C10 104.7(2) . . ? C2 S1 Pt1 98.16(13) . . ? C10 S1 Pt1 99.84(14) . . ? C3 C2 S1 117.6(3) . . ? C2 C3 S4 113.4(3) . . ? C5 S4 C3 101.85(19) . . ? C5 S4 Pt1 109.53(14) . . ? C3 S4 Pt1 105.41(13) . . ? C6 C5 S4 119.4(3) . . ? C5 C6 C7 117.0(4) . . ? C6 C7 S8 119.2(3) . . ? C7 S8 C9 103.1(2) . . ? C7 S8 Pt1 109.59(14) . . ? C9 S8 Pt1 107.48(14) . . ? C10 C9 S8 114.0(3) . . ? C9 C10 S1 118.6(3) . . ? C19 P1 C13 106.44(18) . . ? C19 P1 C11 108.73(17) . . ? C13 P1 C11 106.0(2) . . ? C19 P1 Pt1 112.88(12) . . ? C13 P1 Pt1 115.16(13) . . ? C11 P1 Pt1 107.25(14) . . ? C31 P2 C25 105.5(2) . . ? C31 P2 C12 108.1(2) . . ? C25 P2 C12 104.41(19) . . ? C31 P2 Pt1 115.21(15) . . ? C25 P2 Pt1 115.36(13) . . ? C12 P2 Pt1 107.54(14) . . ? C12 C11 P1 107.9(3) . . ? C11 C12 P2 110.4(3) . . ? C18 C13 C14 119.1(4) . . ? C18 C13 P1 120.7(3) . . ? C14 C13 P1 120.2(3) . . ? C15 C14 C13 120.2(4) . . ? C16 C15 C14 120.3(5) . . ? C15 C16 C17 120.0(5) . . ? C16 C17 C18 120.1(5) . . ? C13 C18 C17 120.2(4) . . ? C20 C19 C24 119.7(3) . . ? C20 C19 P1 120.3(3) . . ? C24 C19 P1 119.6(3) . . ? C21 C20 C19 119.6(4) . . ? C22 C21 C20 120.5(4) . . ? C21 C22 C23 120.1(4) . . ? C22 C23 C24 120.3(4) . . ? C23 C24 C19 119.7(4) . . ? C26 C25 C30 119.5(4) . . ? C26 C25 P2 118.7(3) . . ? C30 C25 P2 121.5(3) . . ? C27 C26 C25 119.8(4) . . ? C28 C27 C26 120.6(5) . . ? C29 C28 C27 119.9(5) . . ? C28 C29 C30 120.7(5) . . ? C29 C30 C25 119.4(5) . . ? C36 C31 C32 119.2(5) . . ? C36 C31 P2 121.7(4) . . ? C32 C31 P2 119.1(4) . . ? C31 C32 C33 121.0(5) . . ? C34 C33 C32 118.9(7) . . ? C35 C34 C33 120.3(6) . . ? C34 C35 C36 120.5(7) . . ? C31 C36 C35 120.0(7) . . ? F6 P3 F2 94.0(4) . . ? F6 P3 F4 90.5(4) . . ? F2 P3 F4 175.2(3) . . ? F6 P3 F1 92.2(3) . . ? F2 P3 F1 92.1(2) . . ? F4 P3 F1 89.2(2) . . ? F6 P3 F3 88.7(3) . . ? F2 P3 F3 88.1(2) . . ? F4 P3 F3 90.6(2) . . ? F1 P3 F3 179.0(3) . . ? F6 P3 F5 177.3(4) . . ? F2 P3 F5 88.0(3) . . ? F4 P3 F5 87.4(3) . . ? F1 P3 F5 89.5(3) . . ? F3 P3 F5 89.5(2) . . ? F7 P4 F12 176.6(3) . . ? F7 P4 F9 93.8(3) . . ? F12 P4 F9 89.3(2) . . ? F7 P4 F8 89.1(3) . . ? F12 P4 F8 89.6(3) . . ? F9 P4 F8 89.1(3) . . ? F7 P4 F10 91.5(3) . . ? F12 P4 F10 89.7(3) . . ? F9 P4 F10 92.9(3) . . ? F8 P4 F10 177.9(3) . . ? F7 P4 F11 87.4(3) . . ? F12 P4 F11 89.5(2) . . ? F9 P4 F11 178.8(3) . . ? F8 P4 F11 91.1(3) . . ? F10 P4 F11 86.8(2) . . ? O2 N O1 123.1(10) . . ? O2 N C37 124.4(10) . . ? O1 N C37 112.5(9) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.514 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.195 #=== END