Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email GLADYSZ@ORGANIK.UNI-ERLANGEN.DE _publ_contact_author_name 'Prof John A Gladysz' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Institut fur Organische Chemie Universitat Erlangen-Nurnberg Henkestrasse 42 91054 Erlangen GERMANY ; _publ_section_title ; Alkene Metatheses in Transition Metal Coordination Spheres: Dimacrocyclizations that join trans Postitions of Square-Planar Platinum Complexes to give Topologically Novel Diphosphine Ligands ; loop_ _publ_author_name 'John A. Gladysz' 'Eike B. Bauer' 'Frank Hampel' 'Takanori Shima' data_eb01 _database_code_depnum_ccdc_archive 'CCDC 159809' _chemical_name_common 'C46 H66 Cl1 F5 P2 Pt1' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H66 Cl F5 P2 Pt' _chemical_formula_weight 1006.47 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 24.8121(3) _cell_length_b 10.5438(2) _cell_length_c 18.0730(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.6070(10) _cell_angle_gamma 90.00 _cell_volume 4575.32(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 3.246 _exptl_absorpt_correction_type SCALEPACK _exptl_absorpt_correction_T_min 0.4426 _exptl_absorpt_correction_T_max 0.7373 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _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 17699 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0956 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.51 _reflns_number_total 10322 _reflns_number_gt 7022 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement Collect _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0287P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10322 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 0.248597(7) 0.963829(16) 0.240420(8) 0.02153(6) Uani 1 1 d . . . P1 P 0.22358(5) 1.06782(11) 0.12403(6) 0.0228(3) Uani 1 1 d . . . Cl1 Cl 0.24292(5) 0.76817(10) 0.17347(6) 0.0303(3) Uani 1 1 d . . . C1' C 0.17205(19) 0.9805(4) 0.0528(2) 0.0262(10) Uani 1 1 d . . . H1'A H 0.1618 1.0307 0.0050 0.031 Uiso 1 1 calc R . . H1'B H 0.1887 0.8999 0.0413 0.031 Uiso 1 1 calc R . . C1 C 0.28229(19) 1.0909(4) 0.0819(2) 0.0273(10) Uani 1 1 d . . . H1A H 0.2680 1.1184 0.0282 0.033 Uiso 1 1 calc R . . H1B H 0.3061 1.1598 0.1098 0.033 Uiso 1 1 calc R . . P2 P 0.27405(5) 0.85373(11) 0.35427(6) 0.0238(3) Uani 1 1 d . . . C2' C 0.11905(19) 0.9511(4) 0.0792(2) 0.0285(11) Uani 1 1 d . . . H2'A H 0.1301 0.9229 0.1332 0.034 Uiso 1 1 calc R . . H2'B H 0.0973 1.0303 0.0772 0.034 Uiso 1 1 calc R . . C2 C 0.31752(19) 0.9730(4) 0.0838(2) 0.0310(11) Uani 1 1 d . . . H2A H 0.3290 0.9414 0.1370 0.037 Uiso 1 1 calc R . . H2B H 0.2944 0.9065 0.0523 0.037 Uiso 1 1 calc R . . C3 C 0.3692(2) 0.9935(4) 0.0548(2) 0.0328(12) Uani 1 1 d . . . H3A H 0.3923 1.0608 0.0855 0.039 Uiso 1 1 calc R . . H3B H 0.3580 1.0227 0.0010 0.039 Uiso 1 1 calc R . . C3' C 0.08200(19) 0.8507(4) 0.0323(2) 0.0311(11) Uani 1 1 d . . . H3'A H 0.0704 0.8785 -0.0218 0.037 Uiso 1 1 calc R . . H3'B H 0.1033 0.7708 0.0343 0.037 Uiso 1 1 calc R . . C4 C 0.40376(19) 0.8736(5) 0.0593(2) 0.0324(11) Uani 1 1 d . . . H4A H 0.4128 0.8417 0.1126 0.039 Uiso 1 1 calc R . . H4B H 0.3811 0.8080 0.0263 0.039 Uiso 1 1 calc R . . C4' C 0.0311(2) 0.8269(5) 0.0612(3) 0.0379(12) Uani 1 1 d . . . H4'A H 0.0098 0.9070 0.0573 0.045 Uiso 1 1 calc R . . H4'B H 0.0435 0.8046 0.1161 0.045 Uiso 1 1 calc R . . C5' C -0.0078(2) 0.7237(5) 0.0206(3) 0.0495(15) Uani 1 1 d . . . H5'A H 0.0125 0.6420 0.0274 0.059 Uiso 1 1 calc R . . H5'B H -0.0187 0.7428 -0.0348 0.059 Uiso 1 1 calc R . . C5 C 0.45762(19) 0.8921(5) 0.0351(3) 0.0364(12) Uani 1 1 d . . . H5A H 0.4828 0.9463 0.0735 0.044 Uiso 1 1 calc R . . H5B H 0.4491 0.9382 -0.0142 0.044 Uiso 1 1 calc R . . C6' C -0.0602(2) 0.7090(6) 0.0489(3) 0.0603(18) Uani 1 1 d . . . H6'A H -0.0839 0.6425 0.0181 0.072 Uiso 1 1 calc R . . H6'B H -0.0813 0.7896 0.0398 0.072 Uiso 1 1 calc R . . C6 C 0.4880(2) 0.7703(5) 0.0263(3) 0.0476(14) Uani 1 1 d . . . H6A H 0.4661 0.7246 -0.0193 0.057 Uiso 1 1 calc R . . H6B H 0.5243 0.7926 0.0164 0.057 Uiso 1 1 calc R . . C7' C -0.0499(2) 0.6742(6) 0.1337(3) 0.0515(15) Uani 1 1 d . . . H7'A H -0.0241 0.7371 0.1646 0.062 Uiso 1 1 calc R . . H7'B H -0.0856 0.6794 0.1487 0.062 Uiso 1 1 calc R . . C7 C 0.4984(2) 0.6812(5) 0.0937(3) 0.0458(14) Uani 1 1 d . . . H7A H 0.5160 0.6030 0.0806 0.055 Uiso 1 1 calc R . . H7B H 0.4621 0.6571 0.1030 0.055 Uiso 1 1 calc R . . C8' C -0.0257(2) 0.5436(5) 0.1520(3) 0.0507(15) Uani 1 1 d . . . H8'A H 0.0110 0.5402 0.1398 0.061 Uiso 1 1 calc R . . H8'B H -0.0504 0.4813 0.1189 0.061 Uiso 1 1 calc R . . C8 C 0.5350(2) 0.7354(5) 0.1670(3) 0.0387(12) Uani 1 1 d . . . H8A H 0.5173 0.8132 0.1804 0.046 Uiso 1 1 calc R . . H8B H 0.5712 0.7600 0.1576 0.046 Uiso 1 1 calc R . . C9' C -0.0183(3) 0.5046(5) 0.2364(3) 0.0534(16) Uani 1 1 d . . . H9'A H -0.0553 0.5042 0.2478 0.064 Uiso 1 1 calc R . . H9'B H -0.0036 0.4169 0.2432 0.064 Uiso 1 1 calc R . . C9 C 0.5458(2) 0.6432(5) 0.2357(3) 0.0453(14) Uani 1 1 d . . . H9A H 0.5643 0.5663 0.2226 0.054 Uiso 1 1 calc R . . H9B H 0.5719 0.6841 0.2798 0.054 Uiso 1 1 calc R . . C10 C 0.4941(2) 0.6031(5) 0.2598(3) 0.0398(13) Uani 1 1 d . . . H10A H 0.4694 0.5569 0.2167 0.048 Uiso 1 1 calc R . . H10B H 0.5054 0.5427 0.3029 0.048 Uiso 1 1 calc R . . C10' C 0.0207(2) 0.5907(5) 0.2943(3) 0.0389(13) Uani 1 1 d . . . H10C H 0.0018 0.6730 0.2959 0.047 Uiso 1 1 calc R . . H10D H 0.0270 0.5518 0.3456 0.047 Uiso 1 1 calc R . . C11 C 0.4609(2) 0.7082(4) 0.2839(3) 0.0358(12) Uani 1 1 d . . . H11A H 0.4500 0.7698 0.2414 0.043 Uiso 1 1 calc R . . H11B H 0.4850 0.7532 0.3281 0.043 Uiso 1 1 calc R . . C11' C 0.0765(2) 0.6157(5) 0.2782(2) 0.0378(12) Uani 1 1 d . . . H11C H 0.0705 0.6663 0.2307 0.045 Uiso 1 1 calc R . . H11D H 0.0928 0.5334 0.2686 0.045 Uiso 1 1 calc R . . C12 C 0.40874(19) 0.6637(4) 0.3057(2) 0.0309(11) Uani 1 1 d . . . H12A H 0.3857 0.6139 0.2628 0.037 Uiso 1 1 calc R . . H12B H 0.4197 0.6066 0.3504 0.037 Uiso 1 1 calc R . . C12' C 0.11842(19) 0.6840(5) 0.3404(2) 0.0328(12) Uani 1 1 d . . . H12C H 0.1300 0.6274 0.3853 0.039 Uiso 1 1 calc R . . H12D H 0.1005 0.7597 0.3563 0.039 Uiso 1 1 calc R . . C13' C 0.17007(19) 0.7255(4) 0.3152(2) 0.0321(11) Uani 1 1 d . . . H13A H 0.1858 0.6514 0.2943 0.039 Uiso 1 1 calc R . . H13B H 0.1592 0.7893 0.2740 0.039 Uiso 1 1 calc R . . C13 C 0.37394(19) 0.7707(4) 0.3247(3) 0.0320(11) Uani 1 1 d . . . H13C H 0.3624 0.8270 0.2796 0.038 Uiso 1 1 calc R . . H13D H 0.3972 0.8213 0.3670 0.038 Uiso 1 1 calc R . . C14' C 0.21451(19) 0.7819(4) 0.3811(2) 0.0282(11) Uani 1 1 d . . . H14A H 0.2285 0.7142 0.4190 0.034 Uiso 1 1 calc R . . H14B H 0.1968 0.8473 0.4065 0.034 Uiso 1 1 calc R . . C14 C 0.32200(19) 0.7260(4) 0.3478(2) 0.0271(11) Uani 1 1 d . . . H14C H 0.3336 0.6830 0.3981 0.033 Uiso 1 1 calc R . . H14D H 0.3023 0.6630 0.3100 0.033 Uiso 1 1 calc R . . C21 C 0.25187(17) 1.1293(4) 0.2957(2) 0.0222(9) Uani 1 1 d . . . F22 F 0.17683(11) 1.0753(2) 0.34815(15) 0.0403(7) Uani 1 1 d . . . C22 C 0.21489(19) 1.1611(4) 0.3389(2) 0.0279(11) Uani 1 1 d . . . C23 C 0.2137(2) 1.2783(4) 0.3718(2) 0.0293(11) Uani 1 1 d . . . F23 F 0.17663(13) 1.3037(3) 0.41268(16) 0.0500(8) Uani 1 1 d . . . F24 F 0.25044(13) 1.4839(2) 0.39645(15) 0.0430(7) Uani 1 1 d . . . C24 C 0.2513(2) 1.3695(4) 0.3636(2) 0.0318(11) Uani 1 1 d . . . C25' C 0.2894(2) 1.3422(4) 0.3235(3) 0.0312(11) Uani 1 1 d . . . F26 F 0.32726(11) 1.2047(2) 0.25002(15) 0.0402(7) Uani 1 1 d . . . C26' C 0.28857(19) 1.2250(4) 0.2903(2) 0.0267(11) Uani 1 1 d . . . C31' C 0.31045(19) 0.9378(4) 0.4407(2) 0.0262(10) Uani 1 1 d . . . C31 C 0.19322(19) 1.2240(4) 0.1258(2) 0.0251(10) Uani 1 1 d . . . C32' C 0.3498(2) 1.0297(5) 0.4366(3) 0.0348(11) Uani 1 1 d . . . H32A H 0.3567 1.0503 0.3886 0.042 Uiso 1 1 calc R . . C32 C 0.1501(2) 1.2389(4) 0.1617(2) 0.0311(11) Uani 1 1 d . . . H32B H 0.1374 1.1674 0.1846 0.037 Uiso 1 1 calc R . . C33 C 0.1254(2) 1.3560(5) 0.1648(3) 0.0368(12) Uani 1 1 d . . . H33A H 0.0949 1.3636 0.1874 0.044 Uiso 1 1 calc R . . C33' C 0.3789(2) 1.0912(5) 0.5020(3) 0.0440(13) Uani 1 1 d . . . H33B H 0.4063 1.1523 0.4985 0.053 Uiso 1 1 calc R . . C34 C 0.1451(2) 1.4611(5) 0.1352(3) 0.0422(13) Uani 1 1 d . . . H34A H 0.1288 1.5418 0.1384 0.051 Uiso 1 1 calc R . . C34' C 0.3691(2) 1.0660(5) 0.5723(3) 0.0483(15) Uani 1 1 d . . . H34B H 0.3887 1.1104 0.6166 0.058 Uiso 1 1 calc R . . C35' C 0.3304(2) 0.9756(5) 0.5769(3) 0.0399(13) Uani 1 1 d . . . H35A H 0.3234 0.9568 0.6251 0.048 Uiso 1 1 calc R . . C35 C 0.1886(2) 1.4492(5) 0.1005(3) 0.0410(13) Uani 1 1 d . . . H35B H 0.2023 1.5221 0.0804 0.049 Uiso 1 1 calc R . . F35 F 0.32708(13) 1.4305(3) 0.31616(17) 0.0525(8) Uani 1 1 d . . . C36 C 0.2121(2) 1.3319(4) 0.0949(2) 0.0329(11) Uani 1 1 d . . . H36A H 0.2413 1.3245 0.0698 0.039 Uiso 1 1 calc R . . C36' C 0.3011(2) 0.9107(4) 0.5118(2) 0.0309(11) Uani 1 1 d . . . H36B H 0.2747 0.8478 0.5161 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02385(10) 0.01776(9) 0.02468(9) -0.00112(8) 0.00926(7) -0.00093(9) P1 0.0231(6) 0.0230(7) 0.0240(5) -0.0008(5) 0.0092(5) -0.0008(5) Cl1 0.0435(7) 0.0204(6) 0.0289(6) -0.0022(5) 0.0127(5) 0.0003(5) C1' 0.029(3) 0.030(3) 0.022(2) -0.001(2) 0.0117(19) -0.005(2) C1 0.031(3) 0.027(3) 0.026(2) 0.000(2) 0.010(2) -0.002(2) P2 0.0257(7) 0.0200(6) 0.0268(6) 0.0000(5) 0.0086(5) -0.0013(5) C2' 0.034(3) 0.030(3) 0.023(2) -0.003(2) 0.0104(19) -0.007(2) C2 0.032(3) 0.028(3) 0.037(2) 0.003(2) 0.016(2) 0.002(2) C3 0.028(3) 0.041(3) 0.031(2) 0.002(2) 0.010(2) 0.001(2) C3' 0.029(3) 0.038(3) 0.027(2) -0.003(2) 0.009(2) -0.007(2) C4 0.029(3) 0.042(3) 0.029(2) 0.005(2) 0.012(2) 0.003(2) C4' 0.033(3) 0.047(3) 0.035(3) 0.001(2) 0.012(2) -0.010(3) C5' 0.049(4) 0.062(4) 0.036(3) -0.001(3) 0.008(3) -0.023(3) C5 0.030(3) 0.048(3) 0.034(3) 0.002(2) 0.012(2) 0.002(3) C6' 0.035(4) 0.095(5) 0.049(3) 0.022(3) 0.006(3) -0.023(3) C6 0.051(4) 0.060(4) 0.037(3) 0.001(3) 0.019(3) 0.009(3) C7' 0.030(3) 0.065(4) 0.058(3) 0.016(3) 0.008(3) -0.009(3) C7 0.044(4) 0.044(3) 0.052(3) -0.010(3) 0.017(3) 0.006(3) C8' 0.048(4) 0.051(4) 0.047(3) -0.005(3) 0.001(3) -0.023(3) C8 0.028(3) 0.044(3) 0.044(3) 0.005(2) 0.010(2) 0.001(3) C9' 0.047(4) 0.057(4) 0.053(3) 0.009(3) 0.005(3) -0.016(3) C9 0.035(3) 0.056(4) 0.049(3) 0.017(3) 0.019(3) 0.014(3) C10 0.043(3) 0.036(3) 0.047(3) 0.009(2) 0.023(3) 0.006(3) C10' 0.031(3) 0.050(3) 0.035(3) 0.006(2) 0.007(2) -0.009(3) C11 0.035(3) 0.034(3) 0.041(3) 0.006(2) 0.015(2) 0.003(2) C11' 0.038(3) 0.046(3) 0.030(2) -0.002(2) 0.010(2) -0.006(3) C12 0.030(3) 0.030(3) 0.034(2) -0.002(2) 0.010(2) -0.003(2) C12' 0.029(3) 0.042(3) 0.030(2) 0.002(2) 0.012(2) -0.006(2) C13' 0.031(3) 0.037(3) 0.030(2) 0.003(2) 0.011(2) -0.005(2) C13 0.029(3) 0.033(3) 0.035(3) 0.002(2) 0.010(2) 0.002(2) C14' 0.028(3) 0.029(3) 0.028(2) -0.002(2) 0.008(2) -0.003(2) C14 0.032(3) 0.020(2) 0.031(2) 0.0013(19) 0.010(2) 0.002(2) C21 0.017(2) 0.022(2) 0.025(2) 0.0023(19) 0.0000(18) -0.004(2) F22 0.0400(18) 0.0332(16) 0.0580(17) -0.0115(13) 0.0317(15) -0.0128(14) C22 0.031(3) 0.025(3) 0.029(2) -0.004(2) 0.010(2) -0.007(2) C23 0.037(3) 0.027(3) 0.028(2) -0.007(2) 0.017(2) 0.003(2) F23 0.057(2) 0.0435(18) 0.0633(19) -0.0219(15) 0.0403(17) -0.0046(16) F24 0.062(2) 0.0250(15) 0.0441(15) -0.0130(12) 0.0166(15) -0.0044(15) C24 0.044(3) 0.021(3) 0.030(2) -0.006(2) 0.008(2) 0.000(2) C25' 0.037(3) 0.021(3) 0.038(3) -0.001(2) 0.014(2) -0.010(2) F26 0.0376(17) 0.0352(16) 0.0559(17) -0.0131(14) 0.0268(14) -0.0132(14) C26' 0.029(3) 0.031(3) 0.025(2) -0.003(2) 0.014(2) 0.001(2) C31' 0.026(3) 0.022(3) 0.029(2) -0.0030(19) 0.006(2) 0.004(2) C31 0.027(3) 0.024(3) 0.022(2) 0.0016(19) 0.0027(19) 0.004(2) C32' 0.034(3) 0.035(3) 0.037(3) 0.003(2) 0.012(2) -0.001(3) C32 0.033(3) 0.032(3) 0.030(2) -0.001(2) 0.010(2) -0.001(2) C33 0.037(3) 0.034(3) 0.041(3) -0.004(2) 0.013(2) 0.007(3) C33' 0.039(3) 0.038(3) 0.050(3) -0.006(3) 0.003(3) -0.012(3) C34 0.053(4) 0.027(3) 0.047(3) -0.003(3) 0.014(3) 0.013(3) C34' 0.044(4) 0.054(4) 0.041(3) -0.018(3) 0.000(3) 0.000(3) C35' 0.039(3) 0.049(3) 0.030(2) -0.007(2) 0.007(2) 0.005(3) C35 0.053(4) 0.024(3) 0.048(3) 0.003(2) 0.016(3) 0.002(3) F35 0.057(2) 0.0325(17) 0.077(2) -0.0156(15) 0.0325(18) -0.0201(16) C36 0.035(3) 0.027(3) 0.035(3) 0.003(2) 0.008(2) -0.001(2) C36' 0.031(3) 0.032(3) 0.030(2) 0.001(2) 0.009(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C21 2.002(4) . ? Pt1 P2 2.3075(11) . ? Pt1 P1 2.3139(11) . ? Pt1 Cl1 2.3778(11) . ? P1 C31 1.815(4) . ? P1 C1' 1.820(4) . ? P1 C1 1.822(4) . ? C1' C2' 1.540(5) . ? C1 C2 1.515(6) . ? P2 C14 1.820(4) . ? P2 C31' 1.825(4) . ? P2 C14' 1.831(4) . ? C2' C3' 1.514(6) . ? C2 C3 1.518(6) . ? C3 C4 1.518(6) . ? C3' C4' 1.504(6) . ? C4 C5 1.520(6) . ? C4' C5' 1.516(6) . ? C5' C6' 1.521(6) . ? C5 C6 1.518(7) . ? C6' C7' 1.534(6) . ? C6 C7 1.509(7) . ? C7' C8' 1.505(7) . ? C7 C8 1.515(7) . ? C8' C9' 1.545(7) . ? C8 C9 1.547(6) . ? C9' C10' 1.531(7) . ? C9 C10 1.515(6) . ? C10 C11 1.510(6) . ? C10' C11' 1.508(6) . ? C11 C12 1.518(6) . ? C11' C12' 1.508(6) . ? C12 C13 1.513(6) . ? C12' C13' 1.528(6) . ? C13' C14' 1.525(6) . ? C13 C14 1.526(6) . ? C21 C22 1.388(5) . ? C21 C26' 1.379(6) . ? F22 C22 1.349(5) . ? C22 C23 1.375(6) . ? C23 F23 1.343(4) . ? C23 C24 1.374(6) . ? F24 C24 1.346(5) . ? C24 C25' 1.361(6) . ? C25' F35 1.349(5) . ? C25' C26' 1.371(6) . ? F26 C26' 1.360(4) . ? C31' C32' 1.391(6) . ? C31' C36' 1.392(5) . ? C31 C32 1.393(6) . ? C31 C36 1.398(6) . ? C32' C33' 1.382(7) . ? C32 C33 1.386(6) . ? C33 C34 1.372(6) . ? C33' C34' 1.378(6) . ? C34 C35 1.383(6) . ? C34' C35' 1.369(7) . ? C35' C36' 1.396(6) . ? C35 C36 1.382(6) . ? 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 C21 Pt1 P2 91.51(12) . . ? C21 Pt1 P1 90.47(12) . . ? P2 Pt1 P1 177.99(4) . . ? C21 Pt1 Cl1 178.89(13) . . ? P2 Pt1 Cl1 89.14(4) . . ? P1 Pt1 Cl1 88.89(4) . . ? C31 P1 C1' 104.5(2) . . ? C31 P1 C1 105.4(2) . . ? C1' P1 C1 105.38(19) . . ? C31 P1 Pt1 115.57(13) . . ? C1' P1 Pt1 112.54(14) . . ? C1 P1 Pt1 112.55(15) . . ? C2' C1' P1 112.6(3) . . ? C2 C1 P1 113.5(3) . . ? C14 P2 C31' 102.9(2) . . ? C14 P2 C14' 107.2(2) . . ? C31' P2 C14' 103.43(19) . . ? C14 P2 Pt1 110.59(14) . . ? C31' P2 Pt1 118.96(14) . . ? C14' P2 Pt1 112.74(15) . . ? C3' C2' C1' 114.3(3) . . ? C3 C2 C1 114.1(4) . . ? C2 C3 C4 112.2(4) . . ? C4' C3' C2' 111.5(3) . . ? C5 C4 C3 113.7(4) . . ? C3' C4' C5' 116.1(4) . . ? C4' C5' C6' 113.9(4) . . ? C4 C5 C6 114.6(4) . . ? C5' C6' C7' 114.7(5) . . ? C7 C6 C5 115.5(4) . . ? C8' C7' C6' 113.3(5) . . ? C6 C7 C8 114.4(4) . . ? C7' C8' C9' 113.7(5) . . ? C7 C8 C9 114.1(4) . . ? C10' C9' C8' 114.4(4) . . ? C10 C9 C8 114.7(4) . . ? C11 C10 C9 116.2(4) . . ? C11' C10' C9' 115.2(4) . . ? C10 C11 C12 114.2(4) . . ? C10' C11' C12' 115.7(4) . . ? C13 C12 C11 113.6(4) . . ? C11' C12' C13' 112.8(3) . . ? C14' C13' C12' 112.0(3) . . ? C12 C13 C14 113.7(4) . . ? C13' C14' P2 115.3(3) . . ? C13 C14 P2 113.5(3) . . ? C22 C21 C26' 113.9(4) . . ? C22 C21 Pt1 122.8(3) . . ? C26' C21 Pt1 123.2(3) . . ? F22 C22 C23 117.2(4) . . ? F22 C22 C21 119.4(4) . . ? C23 C22 C21 123.4(4) . . ? F23 C23 C22 120.7(4) . . ? F23 C23 C24 119.8(4) . . ? C22 C23 C24 119.6(4) . . ? F24 C24 C25' 121.0(4) . . ? F24 C24 C23 119.6(4) . . ? C25' C24 C23 119.4(4) . . ? F35 C25' C26' 120.9(4) . . ? F35 C25' C24 119.9(4) . . ? C26' C25' C24 119.2(4) . . ? F26 C26' C25' 116.1(4) . . ? F26 C26' C21 119.4(4) . . ? C25' C26' C21 124.5(4) . . ? C32' C31' C36' 118.3(4) . . ? C32' C31' P2 119.7(3) . . ? C36' C31' P2 122.0(3) . . ? C32 C31 C36 117.9(4) . . ? C32 C31 P1 118.7(3) . . ? C36 C31 P1 123.3(3) . . ? C33' C32' C31' 120.3(4) . . ? C33 C32 C31 121.2(4) . . ? C34 C33 C32 119.9(4) . . ? C34' C33' C32' 121.5(5) . . ? C33 C34 C35 119.9(5) . . ? C33' C34' C35' 118.7(5) . . ? C34' C35' C36' 120.9(4) . . ? C36 C35 C34 120.4(5) . . ? C35 C36 C31 120.6(4) . . ? C31' C36' C35' 120.4(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.621 _refine_diff_density_min -1.408 _refine_diff_density_rms 0.136 data_eb03_2 _database_code_depnum_ccdc_archive 'CCDC 227266' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H66 Cl F5 P2 Pt' _chemical_formula_weight 1005.46 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.69470(10) _cell_length_b 13.29450(10) _cell_length_c 14.9666(2) _cell_angle_alpha 88.3340(10) _cell_angle_beta 81.1850(10) _cell_angle_gamma 76.1950(10) _cell_volume 2232.96(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1022 _exptl_absorpt_coefficient_mu 3.325 _exptl_absorpt_correction_type 'empirical (Scalepack)' _exptl_absorpt_correction_T_min 0.7321 _exptl_absorpt_correction_T_max 0.7321 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15379 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7900 _reflns_number_gt 7011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL NT' _computing_publication_material 'SHELXTL NT' _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^)+(0.0393P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7900 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _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 -0.285935(12) 0.584678(10) -0.269380(9) 0.02048(6) Uani 1 1 d . . . P1 P -0.39466(9) 0.46206(7) -0.27110(7) 0.0223(2) Uani 1 1 d . . . Cl1 Cl -0.35723(9) 0.64759(8) -0.40420(7) 0.0295(2) Uani 1 1 d . . . C1 C -0.2370(3) 0.5391(3) -0.1483(3) 0.0231(8) Uani 1 1 d . . . P2 P -0.15930(9) 0.69403(7) -0.27761(7) 0.0210(2) Uani 1 1 d . . . F2 F -0.0703(2) 0.41020(18) -0.21181(16) 0.0364(6) Uani 1 1 d . . . C2 C -0.1363(4) 0.4633(3) -0.1384(3) 0.0274(9) Uani 1 1 d . . . F3 F 0.0026(2) 0.3619(2) -0.05301(17) 0.0462(7) Uani 1 1 d . . . C3 C -0.0976(4) 0.4358(3) -0.0570(3) 0.0320(10) Uani 1 1 d . . . F4 F -0.1225(3) 0.4620(2) 0.10037(16) 0.0512(7) Uani 1 1 d . . . C4 C -0.1606(4) 0.4850(3) 0.0200(3) 0.0346(10) Uani 1 1 d . . . F5 F -0.3264(3) 0.6085(2) 0.09080(17) 0.0536(7) Uani 1 1 d . . . C5 C -0.2636(4) 0.5600(3) 0.0148(3) 0.0329(10) Uani 1 1 d . . . F6 F -0.4041(2) 0.6554(2) -0.06736(16) 0.0414(6) Uani 1 1 d . . . C6 C -0.3010(4) 0.5837(3) -0.0679(3) 0.0286(9) Uani 1 1 d . . . C10 C -0.3379(4) 0.3812(3) -0.3716(3) 0.0240(9) Uani 1 1 d . . . C11 C -0.4087(4) 0.3621(3) -0.4319(3) 0.0271(9) Uani 1 1 d . . . C12 C -0.3589(4) 0.2987(3) -0.5070(3) 0.0302(10) Uani 1 1 d . . . C13 C -0.2390(4) 0.2543(3) -0.5214(3) 0.0305(10) Uani 1 1 d . . . C14 C -0.1675(4) 0.2731(3) -0.4615(3) 0.0310(10) Uani 1 1 d . . . C15 C -0.2161(4) 0.3364(3) -0.3870(3) 0.0271(9) Uani 1 1 d . . . C20 C -0.1768(4) 0.7703(3) -0.1753(3) 0.0277(9) Uani 1 1 d . . . C21 C -0.0828(5) 0.7750(3) -0.1311(3) 0.0431(12) Uani 1 1 d . . . C22 C -0.1031(6) 0.8356(4) -0.0537(4) 0.0600(17) Uani 1 1 d . . . C23 C -0.2153(7) 0.8889(4) -0.0203(3) 0.0643(18) Uani 1 1 d . . . C24 C -0.3093(6) 0.8844(4) -0.0641(4) 0.0589(16) Uani 1 1 d . . . C25 C -0.2906(4) 0.8255(3) -0.1414(3) 0.0419(11) Uani 1 1 d . . . C30 C -0.3828(4) 0.3706(3) -0.1778(3) 0.0292(9) Uani 1 1 d . . . C31 C -0.4162(4) 0.2685(3) -0.1895(3) 0.0387(11) Uani 1 1 d . . . C32 C -0.3875(5) 0.1928(4) -0.1123(3) 0.0525(14) Uani 1 1 d . . . C33 C -0.2608(5) 0.1712(4) -0.0947(3) 0.0472(13) Uani 1 1 d . . . C34 C -0.1665(5) 0.1261(4) -0.1728(3) 0.0490(13) Uani 1 1 d . . . C35 C -0.0418(6) 0.1106(4) -0.1490(4) 0.0586(15) Uani 1 1 d . . . C36 C 0.0582(5) 0.0657(4) -0.2215(4) 0.0621(16) Uani 1 1 d . . . C37 C 0.0795(5) 0.1380(4) -0.3005(4) 0.0519(13) Uani 1 1 d . . . C38 C 0.1419(5) 0.2239(4) -0.2820(3) 0.0491(13) Uani 1 1 d . . . C39 C 0.1373(4) 0.3069(4) -0.3547(3) 0.0421(11) Uani 1 1 d . . . C40 C 0.1848(4) 0.3989(4) -0.3360(3) 0.0428(12) Uani 1 1 d . . . C41 C 0.1543(4) 0.4894(4) -0.3987(3) 0.0426(12) Uani 1 1 d . . . C42 C 0.0258(4) 0.5521(3) -0.3829(3) 0.0329(10) Uani 1 1 d . . . C43 C -0.0034(4) 0.6229(3) -0.2999(3) 0.0282(9) Uani 1 1 d . . . C50 C -0.1781(4) 0.7916(3) -0.3655(3) 0.0265(9) Uani 1 1 d . . . C51 C -0.1153(4) 0.8790(3) -0.3613(3) 0.0301(9) Uani 1 1 d . . . C52 C -0.1379(4) 0.9563(3) -0.4383(3) 0.0362(11) Uani 1 1 d . . . C53 C -0.2676(4) 0.9978(3) -0.4479(3) 0.0345(10) Uani 1 1 d . . . C54 C -0.3433(4) 1.0584(3) -0.3662(3) 0.0377(11) Uani 1 1 d . . . C55 C -0.4746(4) 1.0956(3) -0.3750(3) 0.0417(11) Uani 1 1 d . . . C56 C -0.5429(4) 1.0116(4) -0.3670(3) 0.0397(11) Uani 1 1 d . . . C57 C -0.5667(4) 0.9696(3) -0.2718(3) 0.0371(10) Uani 1 1 d . . . C58 C -0.6337(4) 0.8841(3) -0.2672(3) 0.0347(10) Uani 1 1 d . . . C59 C -0.6665(4) 0.8464(3) -0.1718(3) 0.0362(10) Uani 1 1 d . . . C60 C -0.7525(4) 0.7766(3) -0.1643(3) 0.0370(11) Uani 1 1 d . . . C61 C -0.7126(4) 0.6814(3) -0.2248(3) 0.0319(10) Uani 1 1 d . . . C62 C -0.5969(4) 0.6094(3) -0.2065(3) 0.0311(10) Uani 1 1 d . . . C63 C -0.5511(3) 0.5194(2) -0.2740(2) 0.0280(9) Uani 1 1 d . . . H63A H -0.5963 0.4679 -0.2599 0.034 Uiso 1 1 d R . . H63B H -0.5616 0.5447 -0.3336 0.034 Uiso 1 1 d R . . H11A H -0.4936 0.3916 -0.4203 0.034 Uiso 1 1 d R . . H12A H -0.4091 0.2867 -0.5481 0.034 Uiso 1 1 d R . . H13A H -0.2061 0.2100 -0.5740 0.034 Uiso 1 1 d R . . H14A H -0.0821 0.2427 -0.4712 0.034 Uiso 1 1 d R . . H15A H -0.1663 0.3495 -0.3448 0.034 Uiso 1 1 d R . . H21A H -0.0021 0.7341 -0.1540 0.034 Uiso 1 1 d R . . H22A H -0.0359 0.8396 -0.0217 0.034 Uiso 1 1 d R . . H23A H -0.2289 0.9313 0.0343 0.034 Uiso 1 1 d R . . H24A H -0.3897 0.9240 -0.0400 0.034 Uiso 1 1 d R . . H25A H -0.3575 0.8210 -0.1728 0.034 Uiso 1 1 d R . . H30A H -0.3582 0.3864 -0.1212 0.034 Uiso 1 1 d R . . H31A H -0.3730 0.2382 -0.2455 0.034 Uiso 1 1 d R . . H31B H -0.4996 0.2828 -0.1933 0.034 Uiso 1 1 d R . . H32A H -0.4050 0.1280 -0.1261 0.034 Uiso 1 1 d R . . H32B H -0.4407 0.2193 -0.0575 0.034 Uiso 1 1 d R . . H33A H -0.2496 0.1234 -0.0437 0.034 Uiso 1 1 d R . . H33B H -0.2437 0.2346 -0.0743 0.034 Uiso 1 1 d R . . H34A H -0.1744 0.1739 -0.2231 0.034 Uiso 1 1 d R . . H34B H -0.1783 0.0621 -0.1911 0.034 Uiso 1 1 d R . . H35A H -0.0370 0.0675 -0.0944 0.034 Uiso 1 1 d R . . H35B H -0.0315 0.1775 -0.1290 0.034 Uiso 1 1 d R . . H36A H 0.0450 0.0029 -0.2445 0.034 Uiso 1 1 d R . . H36B H 0.1332 0.0433 -0.1959 0.034 Uiso 1 1 d R . . H37A H 0.0054 0.1705 -0.3201 0.034 Uiso 1 1 d R . . H37B H 0.1287 0.0977 -0.3529 0.034 Uiso 1 1 d R . . H38A H 0.2250 0.1933 -0.2757 0.034 Uiso 1 1 d R . . H38B H 0.1050 0.2561 -0.2237 0.034 Uiso 1 1 d R . . H39A H 0.0554 0.3327 -0.3641 0.034 Uiso 1 1 d R . . H39B H 0.1808 0.2757 -0.4111 0.034 Uiso 1 1 d R . . H40A H 0.2714 0.3767 -0.3388 0.034 Uiso 1 1 d R . . H40B H 0.1550 0.4217 -0.2733 0.034 Uiso 1 1 d R . . H41A H 0.1728 0.4638 -0.4596 0.034 Uiso 1 1 d R . . H41B H 0.2051 0.5364 -0.3935 0.034 Uiso 1 1 d R . . H42A H -0.0256 0.5039 -0.3742 0.034 Uiso 1 1 d R . . H42B H 0.0083 0.5924 -0.4345 0.034 Uiso 1 1 d R . . H43A H 0.0164 0.5823 -0.2467 0.034 Uiso 1 1 d R . . H43B H 0.0468 0.6717 -0.3074 0.034 Uiso 1 1 d R . . H50A H -0.2616 0.8214 -0.3636 0.034 Uiso 1 1 d R . . H50B H -0.1490 0.7575 -0.4228 0.034 Uiso 1 1 d R . . H51A H -0.0316 0.8516 -0.3624 0.034 Uiso 1 1 d R . . H51B H -0.1448 0.9159 -0.3033 0.034 Uiso 1 1 d R . . H52A H -0.0943 0.9232 -0.4929 0.034 Uiso 1 1 d R . . H52B H -0.1039 1.0142 -0.4277 0.034 Uiso 1 1 d R . . H53A H -0.3010 0.9409 -0.4596 0.034 Uiso 1 1 d R . . H53B H -0.2724 1.0424 -0.5003 0.034 Uiso 1 1 d R . . H54A H -0.3092 1.1165 -0.3552 0.034 Uiso 1 1 d R . . H54B H -0.3340 1.0144 -0.3130 0.034 Uiso 1 1 d R . . H55A H -0.4821 1.1308 -0.4318 0.034 Uiso 1 1 d R . . H55B H -0.5132 1.1485 -0.3281 0.034 Uiso 1 1 d R . . H56A H -0.4972 0.9556 -0.4060 0.034 Uiso 1 1 d R . . H56B H -0.6173 1.0374 -0.3881 0.034 Uiso 1 1 d R . . H57A H -0.6112 1.0253 -0.2309 0.034 Uiso 1 1 d R . . H57B H -0.4914 0.9427 -0.2491 0.034 Uiso 1 1 d R . . H58A H -0.5858 0.8268 -0.3037 0.034 Uiso 1 1 d R . . H58B H -0.7054 0.9099 -0.2931 0.034 Uiso 1 1 d R . . H59A H -0.7009 0.9063 -0.1317 0.034 Uiso 1 1 d R . . H59B H -0.5946 0.8103 -0.1488 0.034 Uiso 1 1 d R . . H60A H -0.8278 0.8170 -0.1766 0.034 Uiso 1 1 d R . . H60B H -0.7650 0.7540 -0.1019 0.034 Uiso 1 1 d R . . H61A H -0.7031 0.7032 -0.2872 0.034 Uiso 1 1 d R . . H61B H -0.7748 0.6436 -0.2178 0.034 Uiso 1 1 d R . . H62A H -0.6086 0.5822 -0.1449 0.034 Uiso 1 1 d R . . H62B H -0.5368 0.6490 -0.2064 0.034 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01790(9) 0.02006(9) 0.02377(10) -0.00009(6) -0.00461(6) -0.00411(6) P1 0.0196(5) 0.0197(5) 0.0280(5) -0.0013(4) -0.0032(4) -0.0055(4) Cl1 0.0296(6) 0.0335(5) 0.0291(5) 0.0051(4) -0.0124(4) -0.0099(4) C1 0.022(2) 0.022(2) 0.026(2) -0.0049(16) 0.0001(17) -0.0092(16) P2 0.0202(5) 0.0210(5) 0.0236(5) 0.0004(4) -0.0067(4) -0.0065(4) F2 0.0352(14) 0.0347(13) 0.0314(13) -0.0050(11) -0.0042(11) 0.0073(11) C2 0.029(2) 0.027(2) 0.028(2) 0.0012(18) -0.0068(18) -0.0077(18) F3 0.0475(17) 0.0415(15) 0.0476(16) 0.0087(13) -0.0217(13) 0.0017(13) C3 0.030(2) 0.031(2) 0.035(2) 0.0088(19) -0.012(2) -0.0056(19) F4 0.0603(19) 0.0709(19) 0.0278(14) 0.0156(13) -0.0177(13) -0.0207(15) C4 0.044(3) 0.043(3) 0.024(2) 0.010(2) -0.013(2) -0.019(2) F5 0.0559(19) 0.071(2) 0.0275(14) -0.0077(13) 0.0056(13) -0.0102(15) C5 0.034(3) 0.044(3) 0.021(2) -0.0023(19) 0.0030(19) -0.014(2) F6 0.0312(14) 0.0491(16) 0.0362(14) -0.0037(12) 0.0018(11) 0.0016(12) C6 0.024(2) 0.029(2) 0.032(2) 0.0023(18) -0.0024(18) -0.0052(18) C10 0.025(2) 0.0184(19) 0.029(2) -0.0011(16) -0.0012(17) -0.0079(16) C11 0.024(2) 0.027(2) 0.032(2) 0.0019(18) -0.0064(18) -0.0070(17) C12 0.034(3) 0.033(2) 0.026(2) 0.0031(18) -0.0086(19) -0.012(2) C13 0.038(3) 0.026(2) 0.026(2) -0.0031(18) -0.0008(19) -0.0062(19) C14 0.030(2) 0.028(2) 0.033(2) 0.0018(18) -0.0013(19) -0.0058(18) C15 0.022(2) 0.028(2) 0.031(2) 0.0005(18) -0.0053(18) -0.0049(17) C20 0.038(3) 0.020(2) 0.027(2) 0.0026(17) -0.0091(19) -0.0078(18) C21 0.055(3) 0.031(2) 0.048(3) -0.003(2) -0.025(2) -0.007(2) C22 0.098(5) 0.037(3) 0.054(3) -0.006(3) -0.048(3) -0.010(3) C23 0.124(6) 0.037(3) 0.033(3) -0.007(2) -0.019(3) -0.016(3) C24 0.080(4) 0.035(3) 0.047(3) -0.011(2) 0.016(3) -0.001(3) C25 0.046(3) 0.032(2) 0.043(3) -0.004(2) 0.001(2) -0.005(2) C30 0.041(3) 0.022(2) 0.028(2) -0.0002(17) -0.0049(19) -0.0133(18) C31 0.037(3) 0.028(2) 0.049(3) -0.002(2) 0.007(2) -0.012(2) C32 0.074(4) 0.029(3) 0.047(3) -0.004(2) 0.017(3) -0.014(3) C33 0.082(4) 0.036(3) 0.028(2) 0.005(2) -0.011(3) -0.020(3) C34 0.055(3) 0.055(3) 0.038(3) 0.004(2) -0.014(2) -0.011(3) C35 0.078(4) 0.046(3) 0.056(3) 0.010(3) -0.028(3) -0.013(3) C36 0.063(4) 0.039(3) 0.080(4) 0.000(3) -0.028(3) 0.006(3) C37 0.045(3) 0.047(3) 0.058(3) -0.001(3) -0.011(3) 0.004(2) C38 0.045(3) 0.048(3) 0.043(3) -0.011(2) -0.010(2) 0.014(2) C39 0.033(3) 0.046(3) 0.041(3) -0.010(2) -0.003(2) 0.002(2) C40 0.024(2) 0.044(3) 0.057(3) -0.013(2) -0.008(2) 0.002(2) C41 0.029(3) 0.044(3) 0.052(3) -0.010(2) 0.006(2) -0.009(2) C42 0.031(2) 0.036(2) 0.032(2) -0.0003(19) -0.0030(19) -0.0080(19) C43 0.019(2) 0.031(2) 0.037(2) 0.0018(19) -0.0076(18) -0.0081(17) C50 0.027(2) 0.025(2) 0.027(2) 0.0021(17) -0.0061(18) -0.0066(17) C51 0.030(2) 0.025(2) 0.037(2) -0.0002(18) -0.0035(19) -0.0108(18) C52 0.044(3) 0.030(2) 0.034(2) 0.0012(19) 0.005(2) -0.015(2) C53 0.049(3) 0.027(2) 0.031(2) 0.0065(19) -0.007(2) -0.014(2) C54 0.041(3) 0.032(2) 0.041(3) -0.001(2) -0.004(2) -0.011(2) C55 0.042(3) 0.036(3) 0.048(3) 0.005(2) -0.012(2) -0.008(2) C56 0.037(3) 0.042(3) 0.043(3) 0.001(2) -0.013(2) -0.011(2) C57 0.039(3) 0.035(2) 0.040(3) 0.001(2) -0.011(2) -0.011(2) C58 0.032(2) 0.031(2) 0.037(2) -0.0051(19) -0.002(2) -0.0014(19) C59 0.038(3) 0.029(2) 0.038(3) -0.0045(19) -0.004(2) -0.001(2) C60 0.033(3) 0.034(2) 0.038(3) 0.001(2) 0.000(2) 0.001(2) C61 0.022(2) 0.035(2) 0.038(2) -0.0005(19) -0.0043(19) -0.0044(18) C62 0.026(2) 0.031(2) 0.036(2) -0.0045(19) -0.0030(19) -0.0071(18) C63 0.020(2) 0.029(2) 0.037(2) -0.0018(18) -0.0044(18) -0.0092(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.017(4) . ? Pt1 P1 2.2970(10) . ? Pt1 P2 2.2986(9) . ? Pt1 Cl1 2.3560(10) . ? P1 C63 1.814(3) . ? P1 C10 1.819(4) . ? P1 C30 1.824(4) . ? C1 C2 1.379(6) . ? C1 C6 1.383(5) . ? P2 C20 1.819(4) . ? P2 C50 1.820(4) . ? P2 C43 1.827(4) . ? F2 C2 1.352(5) . ? C2 C3 1.373(6) . ? F3 C3 1.346(5) . ? C3 C4 1.361(6) . ? F4 C4 1.349(5) . ? C4 C5 1.379(6) . ? F5 C5 1.345(5) . ? C5 C6 1.379(6) . ? F6 C6 1.347(5) . ? C10 C11 1.381(5) . ? C10 C15 1.393(6) . ? C11 C12 1.389(6) . ? C12 C13 1.371(6) . ? C13 C14 1.382(6) . ? C14 C15 1.380(6) . ? C20 C21 1.381(6) . ? C20 C25 1.385(6) . ? C21 C22 1.388(7) . ? C22 C23 1.360(9) . ? C23 C24 1.377(9) . ? C24 C25 1.377(7) . ? C30 C31 1.522(6) . ? C31 C32 1.533(7) . ? C32 C33 1.503(8) . ? C33 C34 1.508(7) . ? C34 C35 1.519(8) . ? C35 C36 1.489(8) . ? C36 C37 1.530(8) . ? C37 C38 1.548(7) . ? C38 C39 1.524(7) . ? C39 C40 1.509(7) . ? C40 C41 1.511(7) . ? C41 C42 1.521(6) . ? C42 C43 1.527(6) . ? C50 C51 1.522(5) . ? C51 C52 1.532(6) . ? C52 C53 1.513(7) . ? C53 C54 1.520(6) . ? C54 C55 1.522(7) . ? C55 C56 1.513(6) . ? C56 C57 1.525(6) . ? C57 C58 1.521(6) . ? C58 C59 1.523(6) . ? C59 C60 1.513(6) . ? C60 C61 1.515(6) . ? C61 C62 1.517(6) . ? C62 C63 1.529(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 P1 93.31(10) . . ? C1 Pt1 P2 87.42(10) . . ? P1 Pt1 P2 173.33(3) . . ? C1 Pt1 Cl1 175.18(11) . . ? P1 Pt1 Cl1 86.71(3) . . ? P2 Pt1 Cl1 93.12(3) . . ? C63 P1 C10 107.53(17) . . ? C63 P1 C30 108.42(18) . . ? C10 P1 C30 104.13(18) . . ? C63 P1 Pt1 112.33(11) . . ? C10 P1 Pt1 109.27(12) . . ? C30 P1 Pt1 114.64(13) . . ? C2 C1 C6 114.3(4) . . ? C2 C1 Pt1 123.4(3) . . ? C6 C1 Pt1 122.3(3) . . ? C20 P2 C50 103.30(17) . . ? C20 P2 C43 106.94(19) . . ? C50 P2 C43 105.84(19) . . ? C20 P2 Pt1 113.74(13) . . ? C50 P2 Pt1 114.71(13) . . ? C43 P2 Pt1 111.56(13) . . ? F2 C2 C3 116.2(4) . . ? F2 C2 C1 119.6(3) . . ? C3 C2 C1 124.2(4) . . ? F3 C3 C4 119.9(4) . . ? F3 C3 C2 120.7(4) . . ? C4 C3 C2 119.4(4) . . ? F4 C4 C3 120.7(4) . . ? F4 C4 C5 120.1(4) . . ? C3 C4 C5 119.2(4) . . ? F5 C5 C6 121.0(4) . . ? F5 C5 C4 119.4(4) . . ? C6 C5 C4 119.6(4) . . ? F6 C6 C5 116.2(4) . . ? F6 C6 C1 120.6(4) . . ? C5 C6 C1 123.2(4) . . ? C11 C10 C15 119.2(4) . . ? C11 C10 P1 123.7(3) . . ? C15 C10 P1 117.1(3) . . ? C10 C11 C12 120.3(4) . . ? C13 C12 C11 120.1(4) . . ? C12 C13 C14 119.9(4) . . ? C15 C14 C13 120.3(4) . . ? C14 C15 C10 120.0(4) . . ? C21 C20 C25 119.6(4) . . ? C21 C20 P2 123.2(3) . . ? C25 C20 P2 117.3(3) . . ? C20 C21 C22 119.8(5) . . ? C23 C22 C21 120.4(5) . . ? C22 C23 C24 120.0(5) . . ? C25 C24 C23 120.4(5) . . ? C24 C25 C20 119.8(5) . . ? C31 C30 P1 117.5(3) . . ? C30 C31 C32 112.6(4) . . ? C33 C32 C31 115.0(4) . . ? C32 C33 C34 116.0(4) . . ? C33 C34 C35 111.9(4) . . ? C36 C35 C34 116.2(5) . . ? C35 C36 C37 115.2(4) . . ? C36 C37 C38 115.9(4) . . ? C39 C38 C37 113.6(4) . . ? C40 C39 C38 116.3(4) . . ? C39 C40 C41 114.6(4) . . ? C40 C41 C42 115.9(4) . . ? C41 C42 C43 113.4(4) . . ? C42 C43 P2 113.7(3) . . ? C51 C50 P2 116.5(3) . . ? C50 C51 C52 111.8(3) . . ? C53 C52 C51 114.9(4) . . ? C52 C53 C54 114.6(4) . . ? C53 C54 C55 114.1(4) . . ? C56 C55 C54 114.8(4) . . ? C55 C56 C57 114.8(4) . . ? C58 C57 C56 113.1(4) . . ? C57 C58 C59 114.0(4) . . ? C60 C59 C58 114.4(4) . . ? C59 C60 C61 115.1(4) . . ? C60 C61 C62 113.7(4) . . ? C61 C62 C63 113.2(3) . . ? C62 C63 P1 110.5(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.371 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.184 data_eb11 _database_code_depnum_ccdc_archive 'CCDC 227267' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H66 Cl F5 P2 Pt' _chemical_formula_weight 1006.47 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' Cl Cl 0.1484 0.1585 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.57500(10) _cell_length_b 12.2670(2) _cell_length_c 18.1630(3) _cell_angle_alpha 72.9290(9) _cell_angle_beta 84.6100(8) _cell_angle_gamma 82.4310(8) _cell_volume 2228.93(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9914 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 3.331 _exptl_absorpt_correction_type 'empirical (Scalepack)' _exptl_absorpt_correction_T_min 0.5555 _exptl_absorpt_correction_T_max 0.7317 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19533 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.52 _reflns_number_total 10238 _reflns_number_gt 9428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL NT' _computing_publication_material 'SHELXTL NT' _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^)+(0.0281P)^2^+3.0498P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10238 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0636 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 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 0.172746(9) -0.048117(9) -0.256559(6) 0.02134(4) Uani 1 1 d . . . Cl1 Cl 0.02662(7) -0.17448(7) -0.26190(5) 0.03630(17) Uani 1 1 d . . . P1 P 0.00158(6) 0.09131(6) -0.27280(4) 0.02255(14) Uani 1 1 d . . . P2 P 0.33828(6) -0.19368(6) -0.23053(4) 0.02190(14) Uani 1 1 d . . . C11 C 0.2994(2) 0.0615(2) -0.25696(16) 0.0225(5) Uani 1 1 d . . . F12 F 0.27030(18) 0.03983(16) -0.12286(10) 0.0355(4) Uani 1 1 d . . . C12 C 0.3324(3) 0.0846(2) -0.19163(17) 0.0257(6) Uani 1 1 d . . . F13 F 0.45654(19) 0.16717(18) -0.12478(13) 0.0452(5) Uani 1 1 d . . . C13 C 0.4275(3) 0.1506(3) -0.19040(19) 0.0312(6) Uani 1 1 d . . . F14 F 0.59258(19) 0.25985(18) -0.25983(15) 0.0538(6) Uani 1 1 d . . . C14 C 0.4965(3) 0.1983(3) -0.2588(2) 0.0388(8) Uani 1 1 d . . . F15 F 0.5303(2) 0.2262(2) -0.39249(13) 0.0550(6) Uani 1 1 d . . . C15 C 0.4647(3) 0.1805(3) -0.3256(2) 0.0369(7) Uani 1 1 d . . . F16 F 0.34022(19) 0.10272(18) -0.39229(10) 0.0434(5) Uani 1 1 d . . . C16 C 0.3679(3) 0.1147(3) -0.32390(17) 0.0292(6) Uani 1 1 d . . . C21 C -0.1134(3) 0.0495(2) -0.19165(17) 0.0261(6) Uani 1 1 d . . . C22 C -0.2296(3) 0.0140(3) -0.19760(19) 0.0308(6) Uani 1 1 d . . . H22A H -0.2543 0.0128 -0.2463 0.037 Uiso 1 1 calc R . . C23 C -0.3103(3) -0.0200(3) -0.1322(2) 0.0378(7) Uani 1 1 d . . . H23A H -0.3901 -0.0445 -0.1365 0.045 Uiso 1 1 calc R . . C24 C -0.2766(3) -0.0188(3) -0.0614(2) 0.0406(8) Uani 1 1 d . . . H24A H -0.3330 -0.0416 -0.0171 0.049 Uiso 1 1 calc R . . C25 C -0.1602(4) 0.0158(4) -0.0549(2) 0.0462(9) Uani 1 1 d . . . H25A H -0.1360 0.0168 -0.0061 0.055 Uiso 1 1 calc R . . C26 C -0.0788(3) 0.0491(3) -0.11980(19) 0.0388(8) Uani 1 1 d . . . H26A H 0.0017 0.0719 -0.1150 0.047 Uiso 1 1 calc R . . C31 C 0.0280(3) 0.2353(2) -0.27322(18) 0.0281(6) Uani 1 1 d . . . H31A H 0.0690 0.2300 -0.2253 0.034 Uiso 1 1 calc R . . H31B H 0.0886 0.2658 -0.3172 0.034 Uiso 1 1 calc R . . C32 C -0.0927(3) 0.3213(3) -0.27914(19) 0.0315(6) Uani 1 1 d . . . H32A H -0.1447 0.3147 -0.3199 0.038 Uiso 1 1 calc R . . H32B H -0.1443 0.3023 -0.2296 0.038 Uiso 1 1 calc R . . C33 C -0.0603(3) 0.4440(3) -0.2979(2) 0.0382(7) Uani 1 1 d . . . H33A H -0.0106 0.4626 -0.3482 0.046 Uiso 1 1 calc R . . H33B H -0.0045 0.4485 -0.2583 0.046 Uiso 1 1 calc R . . C34 C -0.1751(4) 0.5352(3) -0.3019(2) 0.0449(8) Uani 1 1 d . . . H34A H -0.2164 0.5242 -0.2494 0.054 Uiso 1 1 calc R . . H34B H -0.1434 0.6116 -0.3179 0.054 Uiso 1 1 calc R . . C35 C -0.2756(3) 0.5350(3) -0.3563(2) 0.0415(8) Uani 1 1 d . . . H35A H -0.3422 0.5999 -0.3566 0.050 Uiso 1 1 calc R . . H35B H -0.3169 0.4634 -0.3357 0.050 Uiso 1 1 calc R . . C36 C -0.2261(3) 0.5443(3) -0.4392(2) 0.0448(8) Uani 1 1 d . . . H36A H -0.1877 0.6173 -0.4611 0.054 Uiso 1 1 calc R . . H36B H -0.1582 0.4806 -0.4395 0.054 Uiso 1 1 calc R . . C37 C -0.3314(4) 0.5401(4) -0.4897(2) 0.0516(10) Uani 1 1 d . . . H37A H -0.3805 0.4753 -0.4620 0.062 Uiso 1 1 calc R . . H37B H -0.3905 0.6115 -0.4967 0.062 Uiso 1 1 calc R . . C38 C -0.2857(4) 0.5268(4) -0.5686(2) 0.0575(11) Uani 1 1 d . . . H38A H -0.2405 0.5938 -0.5973 0.069 Uiso 1 1 calc R . . H38B H -0.3613 0.5282 -0.5972 0.069 Uiso 1 1 calc R . . C39 C -0.1950(4) 0.4151(4) -0.5676(2) 0.0495(9) Uani 1 1 d . . . H39A H -0.1785 0.4100 -0.6211 0.059 Uiso 1 1 calc R . . H39B H -0.1123 0.4203 -0.5482 0.059 Uiso 1 1 calc R . . C40 C -0.2478(4) 0.3073(4) -0.5184(2) 0.0485(9) Uani 1 1 d . . . H40A H -0.3366 0.3089 -0.5320 0.058 Uiso 1 1 calc R . . H40B H -0.2508 0.3069 -0.4637 0.058 Uiso 1 1 calc R . . C41 C -0.1725(3) 0.1972(4) -0.5265(2) 0.0449(8) Uani 1 1 d . . . H41A H -0.2152 0.1324 -0.4918 0.054 Uiso 1 1 calc R . . H41B H -0.1787 0.1945 -0.5799 0.054 Uiso 1 1 calc R . . C42 C -0.0335(3) 0.1767(3) -0.50971(19) 0.0399(8) Uani 1 1 d . . . H42A H 0.0128 0.2326 -0.5505 0.048 Uiso 1 1 calc R . . H42B H 0.0001 0.0991 -0.5133 0.048 Uiso 1 1 calc R . . C43 C -0.0025(3) 0.1860(3) -0.43142(18) 0.0372(7) Uani 1 1 d . . . H43A H -0.0208 0.2672 -0.4312 0.045 Uiso 1 1 calc R . . H43B H 0.0901 0.1635 -0.4249 0.045 Uiso 1 1 calc R . . C44 C -0.0772(3) 0.1115(3) -0.36203(17) 0.0288(6) Uani 1 1 d . . . H44A H -0.0826 0.0359 -0.3701 0.035 Uiso 1 1 calc R . . H44B H -0.1653 0.1491 -0.3578 0.035 Uiso 1 1 calc R . . C51 C 0.4753(3) -0.1698(2) -0.29890(17) 0.0255(6) Uani 1 1 d . . . C52 C 0.5995(3) -0.1719(3) -0.27915(19) 0.0311(6) Uani 1 1 d . . . H52A H 0.6168 -0.1854 -0.2266 0.037 Uiso 1 1 calc R . . C53 C 0.6988(3) -0.1543(3) -0.3360(2) 0.0408(8) Uani 1 1 d . . . H53A H 0.7834 -0.1552 -0.3221 0.049 Uiso 1 1 calc R . . C54 C 0.6748(3) -0.1355(3) -0.4121(2) 0.0430(8) Uani 1 1 d . . . H54A H 0.7428 -0.1235 -0.4507 0.052 Uiso 1 1 calc R . . C55 C 0.5522(4) -0.1342(3) -0.4325(2) 0.0457(9) Uani 1 1 d . . . H55A H 0.5359 -0.1226 -0.4850 0.055 Uiso 1 1 calc R . . C56 C 0.4527(3) -0.1499(3) -0.37626(19) 0.0374(7) Uani 1 1 d . . . H56A H 0.3680 -0.1471 -0.3907 0.045 Uiso 1 1 calc R . . C61 C 0.2997(3) -0.3337(2) -0.23125(19) 0.0295(6) Uani 1 1 d . . . H61A H 0.2194 -0.3500 -0.1994 0.035 Uiso 1 1 calc R . . H61B H 0.2838 -0.3302 -0.2848 0.035 Uiso 1 1 calc R . . C62 C 0.4028(3) -0.4334(3) -0.2014(2) 0.0381(7) Uani 1 1 d . . . H62A H 0.4857 -0.4134 -0.2289 0.046 Uiso 1 1 calc R . . H62B H 0.4112 -0.4436 -0.1459 0.046 Uiso 1 1 calc R . . C63 C 0.3748(4) -0.5458(3) -0.2117(2) 0.0464(9) Uani 1 1 d . . . H63A H 0.3747 -0.5373 -0.2676 0.056 Uiso 1 1 calc R . . H63B H 0.4450 -0.6056 -0.1907 0.056 Uiso 1 1 calc R . . C64 C 0.2496(4) -0.5870(4) -0.1735(3) 0.0668(14) Uani 1 1 d . . . H64A H 0.2423 -0.6627 -0.1809 0.080 Uiso 1 1 calc R . . H64B H 0.1782 -0.5327 -0.1990 0.080 Uiso 1 1 calc R . . C65 C 0.2372(10) -0.5977(6) -0.0853(5) 0.146(4) Uani 1 1 d . . . H65A H 0.3253 -0.6089 -0.0681 0.176 Uiso 1 1 calc R . . H65B H 0.1987 -0.5220 -0.0802 0.176 Uiso 1 1 calc R . . C66 C 0.1754(11) -0.6736(6) -0.0354(5) 0.150(4) Uani 1 1 d . . . H66A H 0.2293 -0.7480 -0.0278 0.180 Uiso 1 1 calc R . . H66B H 0.0981 -0.6801 -0.0599 0.180 Uiso 1 1 calc R . . C67 C 0.1346(9) -0.6625(7) 0.0395(5) 0.128(3) Uani 1 1 d . . . H67A H 0.0741 -0.5919 0.0322 0.154 Uiso 1 1 calc R . . H67B H 0.0852 -0.7277 0.0658 0.154 Uiso 1 1 calc R . . C68 C 0.2226(6) -0.6580(6) 0.0904(4) 0.101(2) Uani 1 1 d . . . H68A H 0.2938 -0.7187 0.0891 0.121 Uiso 1 1 calc R . . H68B H 0.1808 -0.6788 0.1429 0.121 Uiso 1 1 calc R . . C69 C 0.2833(5) -0.5429(5) 0.0791(3) 0.0728(14) Uani 1 1 d . . . H69A H 0.3422 -0.5565 0.1209 0.087 Uiso 1 1 calc R . . H69B H 0.3362 -0.5283 0.0299 0.087 Uiso 1 1 calc R . . C70 C 0.1981(4) -0.4359(5) 0.0777(2) 0.0770(17) Uani 1 1 d . . . H70A H 0.1368 -0.4517 0.1233 0.092 Uiso 1 1 calc R . . H70B H 0.1483 -0.4138 0.0311 0.092 Uiso 1 1 calc R . . C71 C 0.2693(5) -0.3329(4) 0.0780(2) 0.0680(14) Uani 1 1 d . . . H71A H 0.2048 -0.2676 0.0805 0.082 Uiso 1 1 calc R . . H71B H 0.3172 -0.3546 0.1253 0.082 Uiso 1 1 calc R . . C72 C 0.3624(4) -0.2925(3) 0.0083(2) 0.0465(9) Uani 1 1 d . . . H72A H 0.4018 -0.2267 0.0140 0.056 Uiso 1 1 calc R . . H72B H 0.4317 -0.3553 0.0083 0.056 Uiso 1 1 calc R . . C73 C 0.3010(3) -0.2566(3) -0.06901(18) 0.0338(7) Uani 1 1 d . . . H73A H 0.2323 -0.1931 -0.0698 0.041 Uiso 1 1 calc R . . H73B H 0.2619 -0.3220 -0.0754 0.041 Uiso 1 1 calc R . . C74 C 0.3996(3) -0.2176(3) -0.13594(17) 0.0275(6) Uani 1 1 d . . . H74A H 0.4745 -0.2765 -0.1299 0.033 Uiso 1 1 calc R . . H74B H 0.4291 -0.1456 -0.1333 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01903(6) 0.02359(6) 0.02036(6) -0.00493(4) -0.00058(4) -0.00205(4) Cl1 0.0248(3) 0.0306(4) 0.0560(5) -0.0140(4) -0.0084(3) -0.0037(3) P1 0.0199(3) 0.0237(3) 0.0221(3) -0.0037(3) -0.0026(3) -0.0009(3) P2 0.0198(3) 0.0230(3) 0.0226(3) -0.0060(3) -0.0023(3) -0.0016(3) C11 0.0199(12) 0.0205(13) 0.0228(13) -0.0024(11) 0.0011(10) 0.0030(10) F12 0.0415(10) 0.0430(10) 0.0239(9) -0.0111(8) 0.0034(7) -0.0115(8) C12 0.0254(13) 0.0234(14) 0.0266(15) -0.0058(11) 0.0013(11) -0.0022(11) F13 0.0463(11) 0.0449(11) 0.0540(13) -0.0247(10) -0.0125(10) -0.0079(9) C13 0.0299(15) 0.0272(15) 0.0393(17) -0.0142(13) -0.0040(13) -0.0007(12) F14 0.0349(10) 0.0386(11) 0.0903(18) -0.0174(11) 0.0017(11) -0.0187(9) C14 0.0243(15) 0.0292(16) 0.064(2) -0.0147(16) -0.0011(15) -0.0048(12) F15 0.0463(12) 0.0532(13) 0.0528(13) 0.0027(11) 0.0226(10) -0.0194(10) C15 0.0280(15) 0.0285(16) 0.0439(19) 0.0023(14) 0.0122(13) -0.0054(12) F16 0.0482(11) 0.0566(13) 0.0222(9) -0.0059(9) 0.0071(8) -0.0137(10) C16 0.0283(14) 0.0298(15) 0.0258(15) -0.0036(12) 0.0017(11) -0.0026(12) C21 0.0245(13) 0.0252(14) 0.0251(14) -0.0041(11) 0.0020(11) -0.0001(11) C22 0.0279(14) 0.0304(15) 0.0335(16) -0.0088(13) -0.0006(12) -0.0029(12) C23 0.0297(16) 0.0347(17) 0.045(2) -0.0060(15) 0.0025(14) -0.0059(13) C24 0.0368(17) 0.044(2) 0.0332(18) -0.0019(15) 0.0088(14) -0.0033(15) C25 0.045(2) 0.065(2) 0.0257(17) -0.0070(16) 0.0004(14) -0.0100(18) C26 0.0316(16) 0.054(2) 0.0288(17) -0.0071(15) -0.0010(13) -0.0103(15) C31 0.0270(14) 0.0261(14) 0.0294(15) -0.0049(12) -0.0036(12) -0.0026(11) C32 0.0311(15) 0.0283(15) 0.0328(16) -0.0061(13) -0.0005(12) -0.0016(12) C33 0.0438(18) 0.0271(16) 0.0425(19) -0.0063(14) -0.0111(15) -0.0018(14) C34 0.062(2) 0.0270(17) 0.043(2) -0.0073(15) -0.0099(17) 0.0045(16) C35 0.0395(18) 0.0336(18) 0.045(2) -0.0054(15) -0.0030(15) 0.0053(14) C36 0.0412(19) 0.045(2) 0.041(2) -0.0009(16) -0.0063(15) -0.0038(16) C37 0.043(2) 0.056(2) 0.048(2) -0.0027(18) -0.0139(17) 0.0035(17) C38 0.056(2) 0.066(3) 0.040(2) 0.0047(19) -0.0135(18) -0.006(2) C39 0.048(2) 0.063(3) 0.0334(19) -0.0044(17) -0.0013(16) -0.0137(18) C40 0.0415(19) 0.067(3) 0.0311(18) -0.0035(17) -0.0027(15) -0.0106(18) C41 0.0436(19) 0.063(2) 0.0282(17) -0.0085(16) -0.0053(14) -0.0137(17) C42 0.0439(19) 0.046(2) 0.0266(16) -0.0078(14) -0.0019(14) -0.0013(15) C43 0.0315(16) 0.049(2) 0.0269(16) -0.0038(14) -0.0022(13) -0.0073(14) C44 0.0295(14) 0.0305(15) 0.0253(15) -0.0057(12) -0.0051(12) -0.0015(12) C51 0.0226(13) 0.0265(14) 0.0271(14) -0.0082(12) 0.0025(11) -0.0033(11) C52 0.0258(14) 0.0342(16) 0.0346(17) -0.0122(13) -0.0015(12) -0.0027(12) C53 0.0233(15) 0.0400(19) 0.060(2) -0.0156(17) 0.0039(14) -0.0067(13) C54 0.0346(17) 0.044(2) 0.046(2) -0.0109(16) 0.0154(15) -0.0040(15) C55 0.046(2) 0.058(2) 0.0280(17) -0.0096(16) 0.0068(15) -0.0014(17) C56 0.0307(16) 0.052(2) 0.0286(16) -0.0105(15) -0.0010(13) -0.0022(14) C61 0.0293(15) 0.0250(14) 0.0350(16) -0.0091(12) -0.0052(12) -0.0022(12) C62 0.0308(16) 0.0302(16) 0.053(2) -0.0122(15) -0.0052(14) 0.0006(13) C63 0.059(2) 0.0296(17) 0.054(2) -0.0171(16) -0.0115(18) 0.0036(16) C64 0.056(2) 0.034(2) 0.116(4) -0.023(2) -0.022(3) -0.0076(18) C65 0.235(10) 0.078(4) 0.135(7) -0.048(5) 0.097(7) -0.083(6) C66 0.264(12) 0.066(4) 0.119(7) -0.020(4) -0.069(8) 0.013(6) C67 0.154(7) 0.125(6) 0.123(7) -0.039(5) -0.016(6) -0.067(6) C68 0.085(4) 0.091(4) 0.107(5) 0.010(4) -0.028(4) -0.009(3) C69 0.077(3) 0.080(3) 0.063(3) -0.013(3) -0.016(3) -0.025(3) C70 0.039(2) 0.130(5) 0.035(2) 0.018(3) 0.0000(17) -0.008(3) C71 0.091(3) 0.069(3) 0.0252(19) -0.0027(19) 0.009(2) 0.025(3) C72 0.063(2) 0.050(2) 0.0256(17) -0.0103(16) -0.0044(16) -0.0012(18) C73 0.0372(16) 0.0360(17) 0.0253(15) -0.0066(13) -0.0007(13) 0.0010(13) C74 0.0270(14) 0.0298(15) 0.0263(15) -0.0087(12) -0.0050(11) -0.0011(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C11 2.017(3) . ? Pt1 P1 2.2972(7) . ? Pt1 P2 2.3049(7) . ? Pt1 Cl1 2.3554(7) . ? P1 C21 1.816(3) . ? P1 C31 1.822(3) . ? P1 C44 1.829(3) . ? P2 C51 1.814(3) . ? P2 C61 1.820(3) . ? P2 C74 1.823(3) . ? C11 C12 1.383(4) . ? C11 C16 1.386(4) . ? F12 C12 1.353(3) . ? C12 C13 1.377(4) . ? F13 C13 1.336(4) . ? C13 C14 1.391(5) . ? F14 C14 1.339(4) . ? C14 C15 1.372(5) . ? F15 C15 1.348(4) . ? C15 C16 1.378(4) . ? F16 C16 1.355(4) . ? C21 C22 1.381(4) . ? C21 C26 1.387(4) . ? C22 C23 1.388(5) . ? C23 C24 1.370(5) . ? C24 C25 1.380(5) . ? C25 C26 1.384(5) . ? C31 C32 1.535(4) . ? C32 C33 1.520(4) . ? C33 C34 1.530(5) . ? C34 C35 1.519(5) . ? C35 C36 1.524(5) . ? C36 C37 1.522(5) . ? C37 C38 1.517(6) . ? C38 C39 1.562(6) . ? C39 C40 1.504(5) . ? C40 C41 1.513(6) . ? C41 C42 1.503(5) . ? C42 C43 1.528(5) . ? C43 C44 1.541(4) . ? C51 C52 1.389(4) . ? C51 C56 1.392(4) . ? C52 C53 1.392(5) . ? C53 C54 1.377(5) . ? C54 C55 1.377(5) . ? C55 C56 1.388(5) . ? C61 C62 1.533(4) . ? C62 C63 1.515(5) . ? C63 C64 1.512(6) . ? C64 C65 1.564(9) . ? C65 C66 1.291(11) . ? C66 C67 1.428(11) . ? C67 C68 1.388(9) . ? C68 C69 1.578(8) . ? C69 C70 1.487(7) . ? C70 C71 1.554(8) . ? C71 C72 1.531(6) . ? C72 C73 1.524(5) . ? C73 C74 1.532(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pt1 P1 93.69(7) . . ? C11 Pt1 P2 87.72(7) . . ? P1 Pt1 P2 175.54(3) . . ? C11 Pt1 Cl1 177.52(8) . . ? P1 Pt1 Cl1 86.39(3) . . ? P2 Pt1 Cl1 92.38(3) . . ? C21 P1 C31 103.17(14) . . ? C21 P1 C44 108.70(14) . . ? C31 P1 C44 104.77(14) . . ? C21 P1 Pt1 108.22(9) . . ? C31 P1 Pt1 118.49(10) . . ? C44 P1 Pt1 112.79(10) . . ? C51 P2 C61 103.13(14) . . ? C51 P2 C74 105.75(13) . . ? C61 P2 C74 104.77(14) . . ? C51 P2 Pt1 114.09(10) . . ? C61 P2 Pt1 115.32(10) . . ? C74 P2 Pt1 112.71(10) . . ? C12 C11 C16 114.1(3) . . ? C12 C11 Pt1 124.2(2) . . ? C16 C11 Pt1 121.6(2) . . ? F12 C12 C13 115.8(3) . . ? F12 C12 C11 119.7(3) . . ? C13 C12 C11 124.5(3) . . ? F13 C13 C12 121.4(3) . . ? F13 C13 C14 119.6(3) . . ? C12 C13 C14 119.0(3) . . ? F14 C14 C15 120.4(3) . . ? F14 C14 C13 121.0(3) . . ? C15 C14 C13 118.5(3) . . ? F15 C15 C14 119.5(3) . . ? F15 C15 C16 120.3(3) . . ? C14 C15 C16 120.2(3) . . ? F16 C16 C15 116.8(3) . . ? F16 C16 C11 119.6(3) . . ? C15 C16 C11 123.6(3) . . ? C22 C21 C26 119.1(3) . . ? C22 C21 P1 123.4(2) . . ? C26 C21 P1 117.4(2) . . ? C21 C22 C23 119.7(3) . . ? C24 C23 C22 121.1(3) . . ? C23 C24 C25 119.5(3) . . ? C24 C25 C26 119.8(3) . . ? C25 C26 C21 120.8(3) . . ? C32 C31 P1 115.2(2) . . ? C33 C32 C31 111.8(3) . . ? C32 C33 C34 115.3(3) . . ? C35 C34 C33 115.5(3) . . ? C34 C35 C36 115.2(3) . . ? C37 C36 C35 112.1(3) . . ? C38 C37 C36 115.1(3) . . ? C37 C38 C39 115.0(3) . . ? C40 C39 C38 113.6(3) . . ? C39 C40 C41 114.7(3) . . ? C42 C41 C40 118.0(3) . . ? C41 C42 C43 116.1(3) . . ? C42 C43 C44 114.4(3) . . ? C43 C44 P1 110.5(2) . . ? C52 C51 C56 118.7(3) . . ? C52 C51 P2 124.7(2) . . ? C56 C51 P2 116.7(2) . . ? C51 C52 C53 120.3(3) . . ? C54 C53 C52 120.3(3) . . ? C53 C54 C55 120.1(3) . . ? C54 C55 C56 119.9(3) . . ? C55 C56 C51 120.8(3) . . ? C62 C61 P2 115.0(2) . . ? C63 C62 C61 113.5(3) . . ? C64 C63 C62 115.1(3) . . ? C63 C64 C65 112.6(5) . . ? C66 C65 C64 123.2(7) . . ? C65 C66 C67 121.9(8) . . ? C68 C67 C66 120.9(9) . . ? C67 C68 C69 119.5(6) . . ? C70 C69 C68 119.4(5) . . ? C69 C70 C71 114.3(4) . . ? C72 C71 C70 115.3(4) . . ? C73 C72 C71 114.0(3) . . ? C72 C73 C74 111.2(3) . . ? C73 C74 P2 113.5(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.431 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.095 data_ts01_2 _database_code_depnum_ccdc_archive 'CCDC 227268' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H50 Cl F5 P2 Pt' _chemical_formula_weight 894.26 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 23.5432(11) _cell_length_b 15.7182(6) _cell_length_c 21.5805(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.273(2) _cell_angle_gamma 90.00 _cell_volume 7390.2(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23439 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 4.008 _exptl_absorpt_correction_type 'empirical (Scalepack)' _exptl_absorpt_correction_T_min 0.6900 _exptl_absorpt_correction_T_max 0.6900 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source "fine-focus rotating anode'" _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43886 _diffrn_reflns_av_R_equivalents 0.1382 _diffrn_reflns_av_sigmaI/netI 0.1369 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.02 _reflns_number_total 13024 _reflns_number_gt 6875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO_SMN _computing_data_reduction DENZO_SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL NT' _computing_publication_material 'SHELXTL NT' _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^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13024 _refine_ls_number_parameters 847 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1156 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _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 1.040395(18) 0.71528(3) 0.119008(18) 0.03242(12) Uani 1 1 d . . . Pt2 Pt 0.537204(18) 1.21718(3) -0.085131(17) 0.02982(12) Uani 1 1 d . . . P1 P 1.05146(14) 0.70418(18) 0.01704(13) 0.0373(7) Uani 1 1 d . . . P2 P 1.03608(13) 0.71403(19) 0.22479(13) 0.0354(6) Uani 1 1 d . . . P3 P 0.54923(12) 1.21238(18) 0.02626(12) 0.0310(6) Uani 1 1 d . . . P4 P 0.52866(13) 1.20263(18) -0.19449(12) 0.0337(7) Uani 1 1 d . . . Cl1 Cl 0.99136(14) 0.58003(17) 0.09507(13) 0.0454(7) Uani 1 1 d . . . Cl2 Cl 0.48637(13) 1.08390(16) -0.09734(12) 0.0381(6) Uani 1 1 d . . . C1 C 1.0548(5) 0.6096(7) 0.2649(5) 0.041(3) Uani 1 1 d . . . H1A H 1.0594 0.6161 0.3122 0.049 Uiso 1 1 calc R . . H1B H 1.0193 0.5716 0.2430 0.049 Uiso 1 1 calc R . . C2 C 1.1122(5) 0.5648(6) 0.2641(5) 0.035(2) Uani 1 1 d . . . H2A H 1.1165 0.5759 0.2210 0.042 Uiso 1 1 calc R . . H2B H 1.1490 0.5878 0.3004 0.042 Uiso 1 1 calc R . . C3 C 1.1082(5) 0.4696(7) 0.2736(6) 0.043(3) Uani 1 1 d . . . H3A H 1.1037 0.4595 0.3168 0.052 Uiso 1 1 calc R . . H3B H 1.0708 0.4477 0.2376 0.052 Uiso 1 1 calc R . . C4 C 1.1621(6) 0.4203(7) 0.2730(6) 0.053(3) Uani 1 1 d . . . H4A H 1.1587 0.3609 0.2866 0.064 Uiso 1 1 calc R . . H4B H 1.2000 0.4450 0.3065 0.064 Uiso 1 1 calc R . . C5 C 1.1677(7) 0.4195(8) 0.2034(7) 0.069(4) Uani 1 1 d . . . H5A H 1.1739 0.3603 0.1917 0.083 Uiso 1 1 calc R . . H5B H 1.1288 0.4404 0.1691 0.083 Uiso 1 1 calc R . . C6 C 1.2172(6) 0.4710(8) 0.2019(7) 0.066(4) Uani 1 1 d . . . H6A H 1.2558 0.4521 0.2378 0.079 Uiso 1 1 calc R . . H6B H 1.2099 0.5308 0.2111 0.079 Uiso 1 1 calc R . . C7 C 1.2248(6) 0.4662(8) 0.1330(6) 0.058(4) Uani 1 1 d . . . H7A H 1.2604 0.5019 0.1360 0.069 Uiso 1 1 calc R . . H7B H 1.2349 0.4068 0.1261 0.069 Uiso 1 1 calc R . . C8 C 1.1720(6) 0.4929(7) 0.0734(6) 0.054(3) Uani 1 1 d . . . H8A H 1.1374 0.4537 0.0673 0.065 Uiso 1 1 calc R . . H8B H 1.1830 0.4872 0.0337 0.065 Uiso 1 1 calc R . . C9 C 1.1501(6) 0.5852(7) 0.0763(6) 0.048(3) Uani 1 1 d . . . H9A H 1.1421 0.5931 0.1178 0.057 Uiso 1 1 calc R . . H9B H 1.1828 0.6255 0.0775 0.057 Uiso 1 1 calc R . . C10 C 1.0921(6) 0.6045(7) 0.0161(6) 0.045(3) Uani 1 1 d . . . H10A H 1.0631 0.5569 0.0106 0.054 Uiso 1 1 calc R . . H10B H 1.1028 0.6052 -0.0241 0.054 Uiso 1 1 calc R . . C11 C 1.0913(5) 0.7891(7) -0.0072(5) 0.038(3) Uani 1 1 d . . . C12 C 1.0708(5) 0.8707(7) -0.0097(5) 0.039(3) Uani 1 1 d . . . H12A H 1.0365 0.8818 0.0020 0.047 Uiso 1 1 calc R . . C13 C 1.0990(5) 0.9389(7) -0.0291(5) 0.044(3) Uani 1 1 d . . . H13A H 1.0836 0.9950 -0.0305 0.052 Uiso 1 1 calc R . . C14 C 1.1483(6) 0.9247(9) -0.0456(6) 0.059(4) Uani 1 1 d . . . H14A H 1.1671 0.9706 -0.0593 0.071 Uiso 1 1 calc R . . C15 C 1.1709(6) 0.8430(9) -0.0426(6) 0.057(3) Uani 1 1 d . . . H15A H 1.2059 0.8330 -0.0534 0.068 Uiso 1 1 calc R . . C16 C 1.1429(5) 0.7750(7) -0.0239(5) 0.043(3) Uani 1 1 d . . . H16A H 1.1586 0.7191 -0.0224 0.051 Uiso 1 1 calc R . . C20 C 0.9823(6) 0.6889(7) -0.0580(5) 0.050(3) Uani 1 1 d . . . H20A H 0.9949 0.6599 -0.0915 0.060 Uiso 1 1 calc R . . H20B H 0.9556 0.6488 -0.0462 0.060 Uiso 1 1 calc R . . C21 C 0.9439(6) 0.7628(8) -0.0919(5) 0.057(4) Uani 1 1 d . . . H21A H 0.9137 0.7441 -0.1358 0.068 Uiso 1 1 calc R . . H21B H 0.9705 0.8064 -0.1002 0.068 Uiso 1 1 calc R . . C22 C 0.9100(6) 0.8027(8) -0.0529(6) 0.059(4) Uani 1 1 d . . . H22A H 0.9405 0.8226 -0.0095 0.071 Uiso 1 1 calc R . . H22B H 0.8880 0.8534 -0.0777 0.071 Uiso 1 1 calc R . . C23 C 0.8649(6) 0.7466(7) -0.0393(6) 0.053(3) Uani 1 1 d . . . H23A H 0.8875 0.7040 -0.0050 0.064 Uiso 1 1 calc R . . H23B H 0.8405 0.7156 -0.0808 0.064 Uiso 1 1 calc R . . C24 C 0.8218(6) 0.7947(8) -0.0152(6) 0.059(3) Uani 1 1 d . . . H24A H 0.7942 0.8299 -0.0525 0.071 Uiso 1 1 calc R . . H24B H 0.8462 0.8338 0.0211 0.071 Uiso 1 1 calc R . . C26 C 0.7831(6) 0.7388(9) 0.0104(6) 0.068(4) Uani 1 1 d . . . H26A H 0.7554 0.7753 0.0237 0.082 Uiso 1 1 calc R . . H26B H 0.7573 0.7014 -0.0264 0.082 Uiso 1 1 calc R . . C27 C 0.8204(6) 0.6848(8) 0.0688(7) 0.067(4) Uani 1 1 d . . . H27A H 0.8382 0.6367 0.0526 0.081 Uiso 1 1 calc R . . H27B H 0.7932 0.6609 0.0899 0.081 Uiso 1 1 calc R . . C28 C 0.8724(7) 0.7349(9) 0.1215(6) 0.079(5) Uani 1 1 d . . . H28A H 0.9022 0.7527 0.1016 0.094 Uiso 1 1 calc R . . H28B H 0.8550 0.7872 0.1330 0.094 Uiso 1 1 calc R . . C29 C 0.9067(6) 0.6851(9) 0.1860(6) 0.072(4) Uani 1 1 d . . . H29A H 0.8789 0.6743 0.2100 0.086 Uiso 1 1 calc R . . H29B H 0.9203 0.6295 0.1749 0.086 Uiso 1 1 calc R . . C30 C 0.9621(5) 0.7360(8) 0.2304(6) 0.054(3) Uani 1 1 d . . . H30A H 0.9666 0.7269 0.2775 0.064 Uiso 1 1 calc R . . H30B H 0.9528 0.7970 0.2203 0.064 Uiso 1 1 calc R . . C31 C 1.0877(5) 0.7898(7) 0.2821(5) 0.041(3) Uani 1 1 d . . . C32 C 1.0664(6) 0.8610(7) 0.3058(5) 0.051(3) Uani 1 1 d . . . H32A H 1.0236 0.8685 0.2943 0.061 Uiso 1 1 calc R . . C33 C 1.1070(7) 0.9205(8) 0.3457(6) 0.058(4) Uani 1 1 d . . . H33A H 1.0917 0.9683 0.3614 0.069 Uiso 1 1 calc R . . C34 C 1.1702(8) 0.9115(8) 0.3633(6) 0.067(4) Uani 1 1 d . . . H34A H 1.1978 0.9533 0.3900 0.080 Uiso 1 1 calc R . . C35 C 1.1917(6) 0.8415(8) 0.3414(6) 0.059(3) Uani 1 1 d . . . H35A H 1.2347 0.8342 0.3546 0.070 Uiso 1 1 calc R . . C36 C 1.1522(6) 0.7805(8) 0.3004(5) 0.052(3) Uani 1 1 d . . . H36A H 1.1681 0.7332 0.2847 0.062 Uiso 1 1 calc R . . C41 C 1.0827(5) 0.8285(7) 0.1398(4) 0.034(3) Uani 1 1 d . . . F42 F 1.1780(3) 0.7734(4) 0.1491(3) 0.0515(16) Uani 1 1 d . . . C42 C 1.1436(5) 0.8412(7) 0.1515(5) 0.042(3) Uani 1 1 d . . . F43 F 1.2330(3) 0.9257(4) 0.1787(3) 0.064(2) Uani 1 1 d . . . C43 C 1.1728(5) 0.9183(8) 0.1679(5) 0.044(3) Uani 1 1 d . . . F44 F 1.1698(4) 1.0644(4) 0.1913(4) 0.074(2) Uani 1 1 d . . . C44 C 1.1415(7) 0.9891(8) 0.1735(6) 0.054(3) Uani 1 1 d . . . F45 F 1.0486(4) 1.0489(4) 0.1681(3) 0.068(2) Uani 1 1 d . . . C45 C 1.0804(6) 0.9814(7) 0.1624(5) 0.046(3) Uani 1 1 d . . . F46 F 0.9916(3) 0.8987(4) 0.1355(3) 0.0508(17) Uani 1 1 d . . . C46 C 1.0517(5) 0.9028(8) 0.1444(5) 0.043(3) Uani 1 1 d . . . C51 C 0.5957(5) 1.1188(7) 0.0643(5) 0.042(3) Uani 1 1 d . . . H51A H 0.6008 1.1158 0.1120 0.050 Uiso 1 1 calc R . . H51B H 0.5733 1.0672 0.0418 0.050 Uiso 1 1 calc R . . C52 C 0.6591(5) 1.1185(7) 0.0604(5) 0.037(3) Uani 1 1 d . . . H52A H 0.6806 1.1718 0.0805 0.044 Uiso 1 1 calc R . . H52B H 0.6540 1.1179 0.0127 0.044 Uiso 1 1 calc R . . C53 C 0.6990(5) 1.0427(7) 0.0960(5) 0.047(3) Uani 1 1 d . . . H53A H 0.7397 1.0482 0.0928 0.057 Uiso 1 1 calc R . . H53B H 0.7053 1.0445 0.1441 0.057 Uiso 1 1 calc R . . C54 C 0.6718(6) 0.9577(7) 0.0677(6) 0.049(3) Uani 1 1 d . . . H54A H 0.7018 0.9128 0.0910 0.059 Uiso 1 1 calc R . . H54B H 0.6348 0.9484 0.0783 0.059 Uiso 1 1 calc R . . C55 C 0.6539(5) 0.9462(7) -0.0065(5) 0.041(3) Uani 1 1 d . . . H55A H 0.6182 0.9832 -0.0300 0.049 Uiso 1 1 calc R . . H55B H 0.6406 0.8866 -0.0181 0.049 Uiso 1 1 calc R . . C56 C 0.7040(5) 0.9660(7) -0.0329(5) 0.042(3) Uani 1 1 d . . . H56A H 0.7124 1.0279 -0.0286 0.050 Uiso 1 1 calc R . . H56B H 0.7421 0.9363 -0.0046 0.050 Uiso 1 1 calc R . . C57 C 0.6882(5) 0.9405(7) -0.1046(5) 0.043(3) Uani 1 1 d . . . H57A H 0.6853 0.8776 -0.1073 0.052 Uiso 1 1 calc R . . H57B H 0.7225 0.9576 -0.1177 0.052 Uiso 1 1 calc R . . C58 C 0.6289(6) 0.9772(7) -0.1556(5) 0.048(3) Uani 1 1 d . . . H58A H 0.6257 0.9591 -0.2007 0.057 Uiso 1 1 calc R . . H58B H 0.5940 0.9515 -0.1475 0.057 Uiso 1 1 calc R . . C59 C 0.6218(5) 1.0723(6) -0.1562(5) 0.038(3) Uani 1 1 d . . . H59A H 0.6555 1.0993 -0.1659 0.045 Uiso 1 1 calc R . . H59B H 0.6248 1.0917 -0.1114 0.045 Uiso 1 1 calc R . . C60 C 0.5600(5) 1.1007(6) -0.2088(5) 0.033(3) Uani 1 1 d . . . H60A H 0.5295 1.0558 -0.2126 0.040 Uiso 1 1 calc R . . H60B H 0.5645 1.1040 -0.2526 0.040 Uiso 1 1 calc R . . C61 C 0.5664(5) 1.2849(7) -0.2217(4) 0.037(2) Uani 1 1 d . . . C62 C 0.6322(5) 1.2898(7) -0.1944(5) 0.041(3) Uani 1 1 d . . . H62A H 0.6551 1.2463 -0.1650 0.049 Uiso 1 1 calc R . . C63 C 0.6627(6) 1.3559(7) -0.2100(5) 0.049(3) Uani 1 1 d . . . H63A H 0.7063 1.3587 -0.1919 0.059 Uiso 1 1 calc R . . C64 C 0.6272(7) 1.4193(7) -0.2536(5) 0.052(4) Uani 1 1 d . . . H64A H 0.6469 1.4662 -0.2648 0.062 Uiso 1 1 calc R . . C65 C 0.5643(6) 1.4141(7) -0.2803(6) 0.049(3) Uani 1 1 d . . . H65A H 0.5413 1.4577 -0.3095 0.059 Uiso 1 1 calc R . . C66 C 0.5344(6) 1.3479(7) -0.2657(5) 0.047(3) Uani 1 1 d . . . H66A H 0.4909 1.3448 -0.2861 0.056 Uiso 1 1 calc R . . C71 C 0.4476(6) 1.1950(7) -0.2548(6) 0.054(3) Uani 1 1 d . . . H71A H 0.4467 1.2103 -0.2996 0.065 Uiso 1 1 calc R . . H71B H 0.4350 1.1347 -0.2568 0.065 Uiso 1 1 calc R . . C72 C 0.3995(6) 1.2474(8) -0.2426(5) 0.053(3) Uani 1 1 d . . . H72A H 0.4051 1.2416 -0.1950 0.063 Uiso 1 1 calc R . . H72B H 0.4060 1.3079 -0.2507 0.063 Uiso 1 1 calc R . . C73 C 0.3366(6) 1.2243(8) -0.2841(6) 0.060(3) Uani 1 1 d . . . H73A H 0.3312 1.1627 -0.2784 0.072 Uiso 1 1 calc R . . H73B H 0.3303 1.2339 -0.3316 0.072 Uiso 1 1 calc R . . C74 C 0.2877(6) 1.2722(9) -0.2692(7) 0.068(4) Uani 1 1 d . . . H74A H 0.2911 1.3333 -0.2785 0.082 Uiso 1 1 calc R . . H74B H 0.2471 1.2523 -0.3005 0.082 Uiso 1 1 calc R . . C75 C 0.2899(6) 1.2639(8) -0.1995(6) 0.059(4) Uani 1 1 d . . . H75A H 0.3109 1.2099 -0.1804 0.070 Uiso 1 1 calc R . . H75B H 0.2473 1.2601 -0.2014 0.070 Uiso 1 1 calc R . . C76 C 0.3225(6) 1.3364(9) -0.1525(6) 0.061(4) Uani 1 1 d . . . H76A H 0.3573 1.3553 -0.1643 0.073 Uiso 1 1 calc R . . H76B H 0.2936 1.3848 -0.1614 0.073 Uiso 1 1 calc R . . C77 C 0.3463(7) 1.3184(12) -0.0803(7) 0.102(7) Uani 1 1 d . . . H77A H 0.3478 1.3729 -0.0567 0.123 Uiso 1 1 calc R . . H77B H 0.3160 1.2817 -0.0715 0.123 Uiso 1 1 calc R . . C78 C 0.4016(7) 1.2811(11) -0.0520(8) 0.107(7) Uani 1 1 d . . . H78A H 0.4306 1.3147 -0.0654 0.128 Uiso 1 1 calc R . . H78B H 0.3984 1.2244 -0.0730 0.128 Uiso 1 1 calc R . . C79 C 0.4326(5) 1.2676(7) 0.0257(6) 0.052(3) Uani 1 1 d . . . H79A H 0.4535 1.3206 0.0473 0.063 Uiso 1 1 calc R . . H79B H 0.4007 1.2542 0.0438 0.063 Uiso 1 1 calc R . . C80 C 0.4789(5) 1.1952(7) 0.0421(5) 0.040(3) Uani 1 1 d . . . H80A H 0.4579 1.1447 0.0161 0.048 Uiso 1 1 calc R . . H80B H 0.4910 1.1811 0.0901 0.048 Uiso 1 1 calc R . . C81 C 0.5858(5) 1.3002(6) 0.0813(5) 0.033(3) Uani 1 1 d . . . C82 C 0.5689(5) 1.3843(6) 0.0624(5) 0.038(3) Uani 1 1 d . . . H82A H 0.5381 1.3954 0.0196 0.046 Uiso 1 1 calc R . . C83 C 0.5954(6) 1.4520(7) 0.1044(6) 0.054(3) Uani 1 1 d . . . H83A H 0.5832 1.5087 0.0905 0.065 Uiso 1 1 calc R . . C84 C 0.6407(6) 1.4357(9) 0.1676(6) 0.058(4) Uani 1 1 d . . . H84A H 0.6601 1.4814 0.1967 0.070 Uiso 1 1 calc R . . C85 C 0.6570(6) 1.3535(9) 0.1871(5) 0.057(4) Uani 1 1 d . . . H85A H 0.6871 1.3427 0.2304 0.068 Uiso 1 1 calc R . . C86 C 0.6309(5) 1.2871(8) 0.1459(5) 0.042(3) Uani 1 1 d . . . H86A H 0.6432 1.2307 0.1608 0.050 Uiso 1 1 calc R . . C91 C 0.5782(5) 1.3295(6) -0.0777(5) 0.035(3) Uani 1 1 d . . . F92 F 0.6776(3) 1.2796(4) -0.0130(3) 0.0567(17) Uani 1 1 d . . . C92 C 0.6400(6) 1.3463(8) -0.0448(5) 0.045(3) Uani 1 1 d . . . F93 F 0.7286(3) 1.4304(5) -0.0087(3) 0.070(2) Uani 1 1 d . . . C93 C 0.6671(5) 1.4254(8) -0.0420(5) 0.047(3) Uani 1 1 d . . . F94 F 0.6596(3) 1.5689(4) -0.0706(3) 0.061(2) Uani 1 1 d . . . C94 C 0.6331(6) 1.4931(7) -0.0725(6) 0.041(3) Uani 1 1 d . . . F95 F 0.5377(3) 1.5489(4) -0.1381(3) 0.0595(19) Uani 1 1 d . . . C95 C 0.5718(6) 1.4819(7) -0.1061(5) 0.041(3) Uani 1 1 d . . . F96 F 0.4848(3) 1.3972(4) -0.1446(3) 0.0454(15) Uani 1 1 d . . . C96 C 0.5460(5) 1.4031(7) -0.1087(5) 0.034(2) 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 0.0334(3) 0.0325(2) 0.0334(2) 0.0020(2) 0.01496(19) -0.0016(2) Pt2 0.0294(2) 0.0305(2) 0.0313(2) -0.00424(19) 0.01346(18) -0.0038(2) P1 0.0420(18) 0.0352(17) 0.0376(14) 0.0003(13) 0.0185(14) -0.0036(14) P2 0.0385(17) 0.0335(15) 0.0399(14) 0.0050(14) 0.0214(13) 0.0028(15) P3 0.0341(16) 0.0304(14) 0.0316(13) -0.0023(13) 0.0159(12) -0.0023(14) P4 0.0318(16) 0.0383(18) 0.0302(13) -0.0041(12) 0.0107(12) 0.0024(13) Cl1 0.053(2) 0.0391(16) 0.0463(15) 0.0000(12) 0.0216(15) -0.0167(14) Cl2 0.0408(17) 0.0347(15) 0.0430(14) -0.0119(12) 0.0207(13) -0.0131(13) C1 0.044(8) 0.043(7) 0.043(6) 0.011(5) 0.024(6) 0.003(6) C2 0.030(7) 0.036(6) 0.038(6) 0.007(5) 0.012(5) 0.004(5) C3 0.032(7) 0.038(7) 0.058(7) 0.014(5) 0.013(6) 0.004(5) C4 0.057(9) 0.046(8) 0.052(7) 0.014(6) 0.016(7) 0.014(7) C5 0.071(11) 0.035(8) 0.113(12) 0.003(7) 0.049(10) 0.012(7) C6 0.060(10) 0.051(8) 0.081(9) -0.005(7) 0.021(8) 0.014(7) C7 0.077(10) 0.043(7) 0.064(8) -0.008(6) 0.038(8) 0.009(7) C8 0.055(9) 0.045(8) 0.075(9) -0.007(7) 0.039(8) 0.002(6) C9 0.056(9) 0.036(7) 0.059(7) 0.002(6) 0.031(7) 0.002(6) C10 0.057(9) 0.027(6) 0.061(7) 0.000(5) 0.034(7) -0.002(6) C11 0.045(7) 0.043(7) 0.032(5) -0.006(5) 0.020(5) -0.011(6) C12 0.033(7) 0.050(7) 0.036(6) 0.002(5) 0.015(5) -0.006(6) C13 0.047(8) 0.040(7) 0.036(6) 0.007(5) 0.006(6) -0.006(6) C14 0.064(10) 0.063(10) 0.054(8) 0.006(7) 0.026(7) -0.011(8) C15 0.045(8) 0.072(10) 0.055(7) -0.002(7) 0.021(7) -0.019(7) C16 0.042(7) 0.042(7) 0.041(6) 0.001(5) 0.012(5) 0.001(6) C20 0.050(8) 0.058(8) 0.045(6) -0.005(6) 0.020(6) -0.017(6) C21 0.056(9) 0.064(9) 0.042(6) 0.008(6) 0.009(6) -0.014(7) C22 0.042(8) 0.072(10) 0.058(8) 0.007(7) 0.013(7) -0.002(7) C23 0.044(8) 0.052(8) 0.062(8) 0.003(6) 0.018(7) -0.009(6) C24 0.047(8) 0.049(8) 0.079(9) 0.013(7) 0.022(7) 0.019(7) C26 0.055(10) 0.077(11) 0.067(8) -0.014(7) 0.016(8) 0.007(8) C27 0.061(10) 0.053(8) 0.090(10) -0.007(7) 0.031(9) 0.008(7) C28 0.100(13) 0.075(11) 0.052(8) -0.003(7) 0.019(8) -0.012(9) C29 0.053(10) 0.095(12) 0.071(9) 0.002(8) 0.028(8) -0.002(8) C30 0.043(8) 0.068(9) 0.062(7) 0.013(6) 0.033(7) 0.014(7) C31 0.056(8) 0.041(7) 0.036(6) 0.007(5) 0.029(6) 0.000(6) C32 0.072(10) 0.046(7) 0.033(6) 0.000(5) 0.017(6) 0.016(7) C33 0.079(11) 0.052(8) 0.046(7) -0.014(6) 0.029(8) 0.005(8) C34 0.109(14) 0.048(9) 0.037(7) 0.006(6) 0.021(8) -0.009(9) C35 0.059(9) 0.052(8) 0.054(7) 0.003(6) 0.008(7) -0.010(7) C36 0.060(9) 0.053(7) 0.047(6) 0.013(6) 0.025(6) 0.009(7) C41 0.041(7) 0.039(6) 0.023(5) 0.000(4) 0.011(5) -0.001(5) F42 0.040(4) 0.050(4) 0.067(4) 0.004(3) 0.024(3) 0.006(3) C42 0.050(8) 0.041(7) 0.046(6) 0.008(5) 0.032(6) 0.000(6) F43 0.043(5) 0.062(5) 0.073(5) 0.013(4) 0.007(4) -0.019(4) C43 0.031(7) 0.051(8) 0.041(6) 0.015(6) 0.004(6) -0.011(6) F44 0.079(6) 0.047(5) 0.085(5) 0.004(4) 0.017(5) -0.029(4) C44 0.065(10) 0.037(7) 0.051(7) 0.000(6) 0.012(7) -0.016(7) F45 0.085(6) 0.035(4) 0.089(5) -0.007(4) 0.039(5) 0.002(4) C45 0.067(10) 0.033(7) 0.044(6) -0.003(5) 0.029(7) 0.001(6) F46 0.047(5) 0.036(4) 0.073(4) 0.003(3) 0.026(4) 0.005(3) C46 0.039(8) 0.062(8) 0.030(6) 0.002(5) 0.013(6) -0.003(6) C51 0.035(7) 0.044(7) 0.048(6) 0.004(5) 0.017(6) 0.006(5) C52 0.032(7) 0.039(6) 0.039(6) 0.000(5) 0.014(5) 0.002(5) C53 0.047(8) 0.057(8) 0.037(6) 0.009(5) 0.015(6) 0.006(6) C54 0.046(8) 0.037(7) 0.069(8) 0.007(6) 0.026(7) 0.001(6) C55 0.042(7) 0.028(6) 0.060(7) 0.004(5) 0.028(6) -0.002(5) C56 0.020(6) 0.040(7) 0.064(7) -0.006(6) 0.014(6) -0.002(5) C57 0.044(8) 0.035(6) 0.054(7) -0.007(5) 0.022(6) 0.012(6) C58 0.057(9) 0.040(7) 0.054(7) -0.011(6) 0.029(7) -0.006(6) C59 0.035(7) 0.036(6) 0.044(6) -0.007(5) 0.018(6) -0.003(5) C60 0.046(7) 0.028(6) 0.031(5) -0.005(4) 0.020(5) -0.003(5) C61 0.050(7) 0.044(6) 0.022(5) -0.008(5) 0.020(5) -0.002(6) C62 0.055(8) 0.039(6) 0.033(5) -0.004(5) 0.021(5) -0.003(6) C63 0.064(9) 0.051(8) 0.046(7) -0.014(6) 0.036(7) -0.018(7) C64 0.091(12) 0.035(7) 0.044(7) -0.002(6) 0.041(8) -0.016(7) C65 0.062(10) 0.038(7) 0.050(7) 0.005(6) 0.024(7) 0.017(7) C66 0.056(8) 0.041(7) 0.049(7) 0.006(6) 0.025(6) 0.005(6) C71 0.053(8) 0.048(8) 0.051(7) -0.010(5) 0.008(6) 0.019(6) C72 0.047(9) 0.062(8) 0.044(7) 0.009(6) 0.011(6) -0.010(6) C73 0.055(9) 0.050(8) 0.070(8) 0.013(7) 0.016(7) 0.005(7) C74 0.048(9) 0.070(10) 0.084(10) -0.006(8) 0.023(8) -0.012(8) C75 0.040(8) 0.060(9) 0.072(8) 0.016(7) 0.016(7) -0.012(6) C76 0.042(8) 0.083(10) 0.059(8) -0.008(7) 0.021(7) -0.010(7) C77 0.066(12) 0.18(2) 0.058(9) 0.004(10) 0.024(9) -0.050(12) C78 0.063(11) 0.145(16) 0.134(14) 0.114(13) 0.061(11) 0.050(11) C79 0.041(8) 0.042(8) 0.082(9) 0.004(6) 0.033(7) 0.008(6) C80 0.044(7) 0.044(7) 0.030(5) 0.002(5) 0.012(5) -0.005(5) C81 0.035(6) 0.030(6) 0.038(6) -0.013(5) 0.019(5) -0.009(5) C82 0.042(7) 0.032(6) 0.047(6) -0.009(5) 0.025(6) -0.008(5) C83 0.066(10) 0.031(7) 0.073(9) -0.004(6) 0.036(8) -0.009(6) C84 0.068(10) 0.069(10) 0.054(8) -0.029(7) 0.043(8) -0.037(8) C85 0.070(10) 0.069(9) 0.029(6) -0.015(6) 0.016(6) -0.027(8) C86 0.045(7) 0.046(7) 0.036(6) -0.010(6) 0.017(5) -0.015(6) C91 0.046(8) 0.036(6) 0.026(5) -0.013(5) 0.019(5) -0.015(6) F92 0.039(4) 0.057(4) 0.061(4) 0.015(4) 0.005(3) -0.004(4) C92 0.050(8) 0.054(8) 0.035(6) -0.002(6) 0.019(6) -0.008(7) F93 0.046(5) 0.077(6) 0.076(5) 0.012(4) 0.010(4) -0.030(4) C93 0.030(7) 0.065(9) 0.047(7) -0.010(6) 0.017(6) -0.029(7) F94 0.077(6) 0.040(4) 0.069(4) -0.001(3) 0.031(4) -0.022(4) C94 0.052(9) 0.031(6) 0.050(7) -0.002(5) 0.029(7) -0.015(6) F95 0.079(6) 0.035(4) 0.074(5) 0.009(3) 0.040(4) -0.002(4) C95 0.066(9) 0.029(6) 0.037(6) 0.003(5) 0.029(6) 0.000(6) F96 0.043(4) 0.031(3) 0.059(4) 0.005(3) 0.015(3) 0.002(3) C96 0.027(7) 0.036(6) 0.036(6) -0.002(5) 0.008(5) -0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C41 2.005(11) . ? Pt1 P1 2.318(3) . ? Pt1 P2 2.323(2) . ? Pt1 Cl1 2.380(3) . ? Pt2 C91 1.989(10) . ? Pt2 P4 2.303(2) . ? Pt2 P3 2.313(2) . ? Pt2 Cl2 2.377(2) . ? P1 C11 1.818(11) . ? P1 C20 1.825(12) . ? P1 C10 1.840(11) . ? P2 C31 1.813(12) . ? P2 C30 1.825(11) . ? P2 C1 1.830(10) . ? P3 C81 1.812(9) . ? P3 C51 1.832(11) . ? P3 C80 1.832(11) . ? P4 C61 1.789(11) . ? P4 C60 1.839(10) . ? P4 C71 1.863(12) . ? C1 C2 1.529(13) . ? C2 C3 1.517(13) . ? C3 C4 1.491(14) . ? C4 C5 1.558(15) . ? C5 C6 1.430(17) . ? C6 C7 1.565(15) . ? C7 C8 1.470(16) . ? C8 C9 1.549(14) . ? C9 C10 1.515(15) . ? C11 C12 1.365(15) . ? C11 C16 1.408(14) . ? C12 C13 1.405(14) . ? C13 C14 1.355(16) . ? C14 C15 1.383(17) . ? C15 C16 1.393(15) . ? C20 C21 1.484(16) . ? C21 C22 1.497(15) . ? C22 C23 1.494(15) . ? C23 C24 1.506(15) . ? C24 C26 1.513(17) . ? C26 C27 1.497(17) . ? C27 C28 1.536(18) . ? C28 C29 1.533(17) . ? C29 C30 1.520(17) . ? C31 C32 1.399(14) . ? C31 C36 1.424(15) . ? C32 C33 1.379(17) . ? C33 C34 1.396(18) . ? C34 C35 1.367(17) . ? C35 C36 1.394(16) . ? C41 C42 1.374(15) . ? C41 C46 1.400(15) . ? F42 C42 1.351(12) . ? C42 C43 1.371(15) . ? F43 C43 1.351(13) . ? C43 C44 1.366(16) . ? F44 C44 1.341(13) . ? C44 C45 1.370(17) . ? F45 C45 1.330(12) . ? C45 C46 1.391(15) . ? F46 C46 1.355(12) . ? C51 C52 1.526(14) . ? C52 C53 1.532(14) . ? C53 C54 1.508(15) . ? C54 C55 1.505(14) . ? C55 C56 1.523(13) . ? C56 C57 1.502(13) . ? C57 C58 1.525(15) . ? C58 C59 1.504(14) . ? C59 C60 1.533(14) . ? C61 C66 1.381(14) . ? C61 C62 1.435(14) . ? C62 C63 1.377(14) . ? C63 C64 1.408(16) . ? C64 C65 1.371(17) . ? C65 C66 1.360(15) . ? C71 C72 1.500(15) . ? C72 C73 1.456(16) . ? C73 C74 1.509(16) . ? C74 C75 1.490(15) . ? C75 C76 1.526(16) . ? C76 C77 1.471(16) . ? C77 C78 1.345(19) . ? C78 C79 1.569(18) . ? C79 C80 1.522(14) . ? C81 C82 1.396(13) . ? C81 C86 1.410(14) . ? C82 C83 1.383(14) . ? C83 C84 1.401(17) . ? C84 C85 1.367(17) . ? C85 C86 1.359(14) . ? C91 C92 1.381(15) . ? C91 C96 1.407(14) . ? F92 C92 1.376(13) . ? C92 C93 1.388(15) . ? F93 C93 1.353(13) . ? C93 C94 1.344(16) . ? F94 C94 1.337(11) . ? C94 C95 1.361(16) . ? F95 C95 1.346(12) . ? C95 C96 1.370(14) . ? F96 C96 1.357(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 Pt1 P1 93.1(3) . . ? C41 Pt1 P2 89.4(3) . . ? P1 Pt1 P2 173.96(11) . . ? C41 Pt1 Cl1 179.3(3) . . ? P1 Pt1 Cl1 86.94(9) . . ? P2 Pt1 Cl1 90.42(10) . . ? C91 Pt2 P4 91.3(3) . . ? C91 Pt2 P3 94.6(3) . . ? P4 Pt2 P3 172.21(10) . . ? C91 Pt2 Cl2 178.3(3) . . ? P4 Pt2 Cl2 87.37(9) . . ? P3 Pt2 Cl2 86.83(9) . . ? C11 P1 C20 103.0(5) . . ? C11 P1 C10 107.1(5) . . ? C20 P1 C10 99.8(5) . . ? C11 P1 Pt1 118.3(3) . . ? C20 P1 Pt1 118.0(4) . . ? C10 P1 Pt1 108.7(3) . . ? C31 P2 C30 103.9(5) . . ? C31 P2 C1 106.7(5) . . ? C30 P2 C1 101.7(5) . . ? C31 P2 Pt1 113.4(3) . . ? C30 P2 Pt1 117.5(4) . . ? C1 P2 Pt1 112.3(3) . . ? C81 P3 C51 105.3(5) . . ? C81 P3 C80 103.2(5) . . ? C51 P3 C80 103.1(5) . . ? C81 P3 Pt2 119.8(3) . . ? C51 P3 Pt2 108.0(3) . . ? C80 P3 Pt2 115.8(3) . . ? C61 P4 C60 107.1(5) . . ? C61 P4 C71 108.8(5) . . ? C60 P4 C71 101.4(5) . . ? C61 P4 Pt2 113.8(3) . . ? C60 P4 Pt2 112.0(3) . . ? C71 P4 Pt2 113.0(4) . . ? C2 C1 P2 117.6(7) . . ? C3 C2 C1 110.7(8) . . ? C4 C3 C2 114.5(9) . . ? C3 C4 C5 113.3(10) . . ? C6 C5 C4 112.7(12) . . ? C5 C6 C7 112.5(11) . . ? C8 C7 C6 117.0(11) . . ? C7 C8 C9 114.6(10) . . ? C10 C9 C8 111.0(10) . . ? C9 C10 P1 117.7(8) . . ? C12 C11 C16 117.5(10) . . ? C12 C11 P1 119.3(8) . . ? C16 C11 P1 123.2(9) . . ? C11 C12 C13 122.0(10) . . ? C14 C13 C12 120.1(11) . . ? C13 C14 C15 119.5(12) . . ? C14 C15 C16 120.6(12) . . ? C15 C16 C11 120.2(11) . . ? C21 C20 P1 120.4(8) . . ? C20 C21 C22 114.0(10) . . ? C23 C22 C21 115.7(11) . . ? C22 C23 C24 113.2(11) . . ? C23 C24 C26 114.3(11) . . ? C27 C26 C24 113.2(12) . . ? C26 C27 C28 112.4(12) . . ? C29 C28 C27 114.1(12) . . ? C30 C29 C28 109.6(11) . . ? C29 C30 P2 118.1(9) . . ? C32 C31 C36 118.2(11) . . ? C32 C31 P2 122.3(9) . . ? C36 C31 P2 119.3(9) . . ? C33 C32 C31 120.7(13) . . ? C32 C33 C34 121.0(12) . . ? C35 C34 C33 118.9(13) . . ? C34 C35 C36 121.9(14) . . ? C35 C36 C31 119.3(12) . . ? C42 C41 C46 113.6(10) . . ? C42 C41 Pt1 124.5(8) . . ? C46 C41 Pt1 122.0(8) . . ? F42 C42 C43 117.3(11) . . ? F42 C42 C41 118.5(10) . . ? C43 C42 C41 124.2(11) . . ? F43 C43 C44 118.8(11) . . ? F43 C43 C42 120.7(11) . . ? C44 C43 C42 120.5(12) . . ? F44 C44 C43 121.2(13) . . ? F44 C44 C45 120.2(12) . . ? C43 C44 C45 118.6(11) . . ? F45 C45 C44 120.2(11) . . ? F45 C45 C46 120.3(12) . . ? C44 C45 C46 119.5(11) . . ? F46 C46 C45 116.8(11) . . ? F46 C46 C41 119.6(10) . . ? C45 C46 C41 123.5(11) . . ? C52 C51 P3 114.1(7) . . ? C51 C52 C53 113.6(9) . . ? C54 C53 C52 113.6(10) . . ? C55 C54 C53 116.2(9) . . ? C54 C55 C56 115.5(10) . . ? C57 C56 C55 113.9(9) . . ? C56 C57 C58 116.4(9) . . ? C59 C58 C57 116.8(9) . . ? C58 C59 C60 111.5(9) . . ? C59 C60 P4 117.2(7) . . ? C66 C61 C62 117.8(10) . . ? C66 C61 P4 122.3(9) . . ? C62 C61 P4 119.8(8) . . ? C63 C62 C61 121.5(11) . . ? C62 C63 C64 117.7(12) . . ? C65 C64 C63 120.7(11) . . ? C66 C65 C64 121.4(11) . . ? C65 C66 C61 120.8(12) . . ? C72 C71 P4 119.0(8) . . ? C73 C72 C71 114.5(10) . . ? C72 C73 C74 115.2(11) . . ? C75 C74 C73 115.7(12) . . ? C74 C75 C76 114.9(10) . . ? C77 C76 C75 117.0(12) . . ? C78 C77 C76 118.6(14) . . ? C77 C78 C79 121.5(13) . . ? C80 C79 C78 110.5(10) . . ? C79 C80 P3 117.8(7) . . ? C82 C81 C86 116.8(9) . . ? C82 C81 P3 121.2(8) . . ? C86 C81 P3 121.9(8) . . ? C83 C82 C81 122.0(11) . . ? C82 C83 C84 119.0(11) . . ? C85 C84 C83 119.6(11) . . ? C86 C85 C84 121.3(12) . . ? C85 C86 C81 121.3(11) . . ? C92 C91 C96 111.1(10) . . ? C92 C91 Pt2 126.6(9) . . ? C96 C91 Pt2 122.3(8) . . ? F92 C92 C91 117.6(10) . . ? F92 C92 C93 117.6(11) . . ? C91 C92 C93 124.8(12) . . ? C94 C93 F93 122.2(11) . . ? C94 C93 C92 120.6(11) . . ? F93 C93 C92 117.2(12) . . ? F94 C94 C93 120.4(11) . . ? F94 C94 C95 121.3(11) . . ? C93 C94 C95 118.2(10) . . ? F95 C95 C94 118.5(10) . . ? F95 C95 C96 121.2(11) . . ? C94 C95 C96 120.2(11) . . ? F96 C96 C95 116.3(10) . . ? F96 C96 C91 118.7(9) . . ? C95 C96 C91 125.0(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.894 _refine_diff_density_min -1.307 _refine_diff_density_rms 0.224 data_ts02 _database_code_depnum_ccdc_archive 'CCDC 227269' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H34 Cl F5 P2 Pt' _chemical_formula_weight 782.05 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.5572(3) _cell_length_b 10.9033(2) _cell_length_c 28.7856(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5824.33(17) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6873 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 5.071 _exptl_absorpt_correction_type 'empirical (Scalepack)' _exptl_absorpt_correction_T_min 0.3115 _exptl_absorpt_correction_T_max 0.4303 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12286 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6642 _reflns_number_gt 5538 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL NT' _computing_publication_material 'SHELXTL NT' _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^)+(0.0368P)^2^+3.8878P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6642 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0602 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.064589(6) -0.913470(11) 0.138458(5) 0.01862(6) Uani 1 1 d . . . P1 P -0.03505(5) -0.78612(8) 0.14028(3) 0.01994(18) Uani 1 1 d . . . Cl1 Cl 0.12929(4) -0.75043(8) 0.17313(4) 0.0293(2) Uani 1 1 d . . . P2 P 0.17021(5) -1.02471(8) 0.13645(3) 0.02017(19) Uani 1 1 d . . . C11 C 0.00619(17) -1.0496(3) 0.10955(12) 0.0199(7) Uani 1 1 d . . . F12 F -0.06193(10) -1.07542(19) 0.17865(8) 0.0303(5) Uani 1 1 d . . . C12 C -0.0499(2) -1.1052(3) 0.13338(13) 0.0233(8) Uani 1 1 d . . . F13 F -0.15013(12) -1.2387(2) 0.13898(8) 0.0389(6) Uani 1 1 d . . . C13 C -0.09579(18) -1.1902(3) 0.11374(14) 0.0258(8) Uani 1 1 d . . . F14 F -0.12979(12) -1.3085(2) 0.04894(9) 0.0400(6) Uani 1 1 d . . . C14 C -0.08586(19) -1.2245(3) 0.06860(14) 0.0280(8) Uani 1 1 d . . . F15 F -0.01979(12) -1.2110(2) -0.00044(9) 0.0448(6) Uani 1 1 d . . . C15 C -0.02997(19) -1.1752(3) 0.04381(13) 0.0282(8) Uani 1 1 d . . . F16 F 0.06751(10) -1.0426(2) 0.03717(9) 0.0370(6) Uani 1 1 d . . . C16 C 0.01410(18) -1.0888(3) 0.06427(13) 0.0238(7) Uani 1 1 d . . . C21 C -0.01642(19) -0.6467(3) 0.10682(14) 0.0300(8) Uani 1 1 d . . . H21A H 0.0360 -0.6304 0.1089 0.036 Uiso 1 1 calc R . . H21B H -0.0273 -0.6645 0.0738 0.036 Uiso 1 1 calc R . . C22 C -0.0558(2) -0.5286(4) 0.11980(18) 0.0447(11) Uani 1 1 d . . . H22A H -0.0432 -0.4648 0.0967 0.054 Uiso 1 1 calc R . . H22B H -0.1083 -0.5435 0.1174 0.054 Uiso 1 1 calc R . . C23 C -0.0399(3) -0.4789(4) 0.1677(2) 0.0511(13) Uani 1 1 d . . . H23A H -0.0388 -0.3883 0.1657 0.061 Uiso 1 1 calc R . . H23B H 0.0090 -0.5063 0.1767 0.061 Uiso 1 1 calc R . . C24 C -0.0913(2) -0.5142(4) 0.20627(17) 0.0397(10) Uani 1 1 d . . . H24A H -0.1334 -0.4585 0.2051 0.048 Uiso 1 1 calc R . . H24B H -0.0668 -0.5009 0.2364 0.048 Uiso 1 1 calc R . . C25 C -0.11833(19) -0.6459(3) 0.20459(14) 0.0308(9) Uani 1 1 d . . . H25A H -0.1523 -0.6547 0.1783 0.037 Uiso 1 1 calc R . . H25B H -0.1452 -0.6638 0.2335 0.037 Uiso 1 1 calc R . . C26 C -0.05725(18) -0.7405(3) 0.19908(13) 0.0262(8) Uani 1 1 d . . . H26A H -0.0706 -0.8150 0.2167 0.031 Uiso 1 1 calc R . . H26B H -0.0133 -0.7063 0.2136 0.031 Uiso 1 1 calc R . . C31 C -0.11818(17) -0.8483(3) 0.11623(13) 0.0210(7) Uani 1 1 d . . . C32 C -0.1740(2) -0.8910(3) 0.14509(14) 0.0269(8) Uani 1 1 d . . . H32A H -0.1716 -0.8779 0.1777 0.032 Uiso 1 1 calc R . . C33 C -0.23180(19) -0.9515(4) 0.12618(16) 0.0351(9) Uani 1 1 d . . . H33A H -0.2692 -0.9802 0.1459 0.042 Uiso 1 1 calc R . . C34 C -0.23628(19) -0.9711(4) 0.07931(15) 0.0347(9) Uani 1 1 d . . . H34A H -0.2767 -1.0129 0.0667 0.042 Uiso 1 1 calc R . . C35 C -0.1823(2) -0.9302(3) 0.05042(14) 0.0320(9) Uani 1 1 d . . . H35A H -0.1854 -0.9439 0.0179 0.038 Uiso 1 1 calc R . . C36 C -0.12361(19) -0.8693(3) 0.06872(13) 0.0270(8) Uani 1 1 d . . . H36A H -0.0865 -0.8414 0.0486 0.032 Uiso 1 1 calc R . . C41 C 0.16727(19) -1.1906(3) 0.12831(14) 0.0267(8) Uani 1 1 d . . . H41A H 0.1538 -1.2074 0.0956 0.032 Uiso 1 1 calc R . . H41B H 0.2165 -1.2234 0.1331 0.032 Uiso 1 1 calc R . . C42 C 0.1154(2) -1.2619(3) 0.16001(16) 0.0343(9) Uani 1 1 d . . . H42A H 0.0679 -1.2655 0.1445 0.041 Uiso 1 1 calc R . . H42B H 0.1333 -1.3472 0.1626 0.041 Uiso 1 1 calc R . . C43 C 0.1041(2) -1.2126(4) 0.20873(16) 0.0421(11) Uani 1 1 d . . . H43A H 0.0759 -1.2738 0.2265 0.050 Uiso 1 1 calc R . . H43B H 0.0744 -1.1374 0.2065 0.050 Uiso 1 1 calc R . . C44 C 0.1719(2) -1.1817(4) 0.23683(15) 0.0408(10) Uani 1 1 d . . . H44A H 0.1633 -1.2030 0.2698 0.049 Uiso 1 1 calc R . . H44B H 0.2122 -1.2334 0.2256 0.049 Uiso 1 1 calc R . . C45 C 0.1946(2) -1.0472(4) 0.23400(14) 0.0362(9) Uani 1 1 d . . . H45A H 0.2303 -1.0312 0.2588 0.043 Uiso 1 1 calc R . . H45B H 0.1519 -0.9956 0.2405 0.043 Uiso 1 1 calc R . . C46 C 0.22711(18) -1.0065(3) 0.18765(13) 0.0285(8) Uani 1 1 d . . . H46A H 0.2721 -1.0533 0.1825 0.034 Uiso 1 1 calc R . . H46B H 0.2405 -0.9189 0.1903 0.034 Uiso 1 1 calc R . . C51 C 0.22901(18) -0.9725(3) 0.08944(13) 0.0248(7) Uani 1 1 d . . . C52 C 0.29671(19) -1.0251(4) 0.08297(15) 0.0331(9) Uani 1 1 d . . . H52A H 0.3120 -1.0905 0.1024 0.040 Uiso 1 1 calc R . . C53 C 0.3419(2) -0.9817(4) 0.04801(15) 0.0397(10) Uani 1 1 d . . . H53A H 0.3877 -1.0186 0.0434 0.048 Uiso 1 1 calc R . . C54 C 0.3206(2) -0.8857(4) 0.01994(14) 0.0372(9) Uani 1 1 d . . . H54A H 0.3520 -0.8551 -0.0034 0.045 Uiso 1 1 calc R . . C55 C 0.2532(2) -0.8344(3) 0.02612(14) 0.0333(9) Uani 1 1 d . . . H55A H 0.2380 -0.7691 0.0066 0.040 Uiso 1 1 calc R . . C56 C 0.20766(19) -0.8774(3) 0.06046(13) 0.0268(8) Uani 1 1 d . . . H56A H 0.1614 -0.8415 0.0643 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01559(8) 0.01855(8) 0.02171(9) -0.00050(5) 0.00052(5) -0.00040(5) P1 0.0172(4) 0.0204(4) 0.0222(5) 0.0014(3) -0.0003(3) 0.0013(3) Cl1 0.0225(4) 0.0246(4) 0.0408(6) -0.0071(4) -0.0037(4) -0.0024(3) P2 0.0171(4) 0.0206(4) 0.0228(5) -0.0014(4) 0.0016(3) 0.0008(3) C11 0.0183(15) 0.0173(14) 0.0241(19) 0.0001(13) -0.0013(13) -0.0002(13) F12 0.0303(12) 0.0381(12) 0.0226(12) 0.0002(9) 0.0051(9) -0.0070(9) C12 0.0237(17) 0.0226(17) 0.023(2) 0.0021(14) 0.0019(14) 0.0003(14) F13 0.0312(12) 0.0440(13) 0.0414(15) 0.0049(11) 0.0064(10) -0.0180(11) C13 0.0233(17) 0.0233(17) 0.031(2) 0.0047(15) 0.0022(15) -0.0047(14) F14 0.0380(12) 0.0364(12) 0.0456(16) -0.0055(11) -0.0065(11) -0.0173(10) C14 0.0254(17) 0.0241(17) 0.034(2) 0.0003(16) -0.0049(16) -0.0036(14) F15 0.0511(15) 0.0552(15) 0.0282(14) -0.0156(12) 0.0051(11) -0.0171(12) C15 0.0310(19) 0.0308(18) 0.023(2) -0.0049(15) -0.0004(15) -0.0008(15) F16 0.0320(12) 0.0464(13) 0.0327(14) -0.0074(11) 0.0123(10) -0.0143(10) C16 0.0219(17) 0.0274(17) 0.0222(19) -0.0010(14) 0.0016(14) -0.0039(14) C21 0.0270(18) 0.0322(19) 0.031(2) 0.0104(17) 0.0017(16) -0.0009(16) C22 0.046(3) 0.034(2) 0.054(3) 0.014(2) 0.003(2) 0.0046(19) C23 0.052(3) 0.026(2) 0.076(4) -0.003(2) 0.005(3) -0.005(2) C24 0.033(2) 0.037(2) 0.049(3) -0.012(2) -0.008(2) 0.0054(18) C25 0.0279(18) 0.034(2) 0.030(2) -0.0054(16) 0.0008(16) 0.0081(16) C26 0.0256(18) 0.0289(18) 0.0243(19) -0.0003(15) -0.0029(14) 0.0033(14) C31 0.0168(15) 0.0222(16) 0.024(2) 0.0016(14) -0.0017(13) 0.0037(13) C32 0.0235(18) 0.0296(18) 0.028(2) 0.0042(15) 0.0047(15) 0.0051(15) C33 0.0186(18) 0.043(2) 0.044(3) -0.002(2) 0.0073(17) -0.0065(17) C34 0.0215(18) 0.044(2) 0.039(2) -0.0086(19) -0.0058(16) -0.0036(16) C35 0.031(2) 0.039(2) 0.027(2) -0.0024(17) -0.0069(16) 0.0005(16) C36 0.0239(17) 0.0335(18) 0.024(2) 0.0038(16) -0.0001(15) 0.0010(15) C41 0.0232(17) 0.0208(17) 0.036(2) -0.0045(15) 0.0026(15) 0.0019(14) C42 0.0272(19) 0.0242(18) 0.051(3) 0.0082(18) 0.0047(18) 0.0023(15) C43 0.037(2) 0.038(2) 0.051(3) 0.021(2) 0.015(2) 0.0071(18) C44 0.042(2) 0.049(2) 0.031(2) 0.0116(19) 0.0100(19) 0.020(2) C45 0.038(2) 0.046(2) 0.025(2) -0.0045(18) -0.0005(17) 0.0165(19) C46 0.0248(17) 0.0314(19) 0.029(2) -0.0031(16) -0.0040(16) 0.0058(15) C51 0.0230(17) 0.0282(18) 0.0232(19) -0.0009(15) 0.0017(14) -0.0037(14) C52 0.0249(18) 0.038(2) 0.037(2) 0.0032(18) 0.0046(17) 0.0010(16) C53 0.0270(19) 0.054(3) 0.039(3) 0.000(2) 0.0094(18) 0.0003(19) C54 0.035(2) 0.052(2) 0.026(2) 0.0006(18) 0.0064(17) -0.0141(19) C55 0.037(2) 0.035(2) 0.027(2) 0.0043(16) -0.0029(17) -0.0097(18) C56 0.0240(17) 0.0293(17) 0.027(2) -0.0027(16) -0.0017(15) -0.0028(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C11 2.017(3) . ? Pt1 P2 2.3056(9) . ? Pt1 P1 2.3129(9) . ? Pt1 Cl1 2.3660(8) . ? P1 C26 1.812(4) . ? P1 C31 1.822(3) . ? P1 C21 1.832(3) . ? P2 C46 1.824(4) . ? P2 C41 1.825(3) . ? P2 C51 1.829(4) . ? C11 C16 1.380(5) . ? C11 C12 1.387(5) . ? F12 C12 1.361(4) . ? C12 C13 1.379(5) . ? F13 C13 1.351(4) . ? C13 C14 1.364(5) . ? F14 C14 1.351(4) . ? C14 C15 1.369(5) . ? F15 C15 1.346(4) . ? C15 C16 1.379(5) . ? F16 C16 1.358(4) . ? C21 C22 1.527(6) . ? C22 C23 1.510(7) . ? C23 C24 1.513(7) . ? C24 C25 1.523(5) . ? C25 C26 1.540(5) . ? C31 C36 1.390(5) . ? C31 C32 1.407(5) . ? C32 C33 1.373(6) . ? C33 C34 1.369(6) . ? C34 C35 1.377(5) . ? C35 C36 1.380(5) . ? C41 C42 1.537(5) . ? C42 C43 1.516(6) . ? C43 C44 1.533(6) . ? C44 C45 1.527(6) . ? C45 C46 1.530(5) . ? C51 C56 1.389(5) . ? C51 C52 1.394(5) . ? C52 C53 1.392(5) . ? C53 C54 1.381(6) . ? C54 C55 1.382(5) . ? C55 C56 1.382(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pt1 P2 93.41(9) . . ? C11 Pt1 P1 91.23(9) . . ? P2 Pt1 P1 174.84(3) . . ? C11 Pt1 Cl1 177.99(10) . . ? P2 Pt1 Cl1 88.53(3) . . ? P1 Pt1 Cl1 86.85(3) . . ? C26 P1 C31 105.34(16) . . ? C26 P1 C21 107.83(18) . . ? C31 P1 C21 105.58(17) . . ? C26 P1 Pt1 111.59(11) . . ? C31 P1 Pt1 116.42(11) . . ? C21 P1 Pt1 109.59(12) . . ? C46 P2 C41 103.24(17) . . ? C46 P2 C51 102.62(17) . . ? C41 P2 C51 103.38(16) . . ? C46 P2 Pt1 114.50(12) . . ? C41 P2 Pt1 119.95(11) . . ? C51 P2 Pt1 111.21(12) . . ? C16 C11 C12 114.3(3) . . ? C16 C11 Pt1 124.1(2) . . ? C12 C11 Pt1 121.4(3) . . ? F12 C12 C13 116.9(3) . . ? F12 C12 C11 119.5(3) . . ? C13 C12 C11 123.7(4) . . ? F13 C13 C14 120.4(3) . . ? F13 C13 C12 120.2(4) . . ? C14 C13 C12 119.4(3) . . ? F14 C14 C13 120.2(3) . . ? F14 C14 C15 120.3(4) . . ? C13 C14 C15 119.4(3) . . ? F15 C15 C14 119.1(3) . . ? F15 C15 C16 121.3(3) . . ? C14 C15 C16 119.7(4) . . ? F16 C16 C15 116.1(3) . . ? F16 C16 C11 120.3(3) . . ? C15 C16 C11 123.5(3) . . ? C22 C21 P1 118.7(3) . . ? C23 C22 C21 115.7(4) . . ? C22 C23 C24 117.2(4) . . ? C23 C24 C25 115.1(3) . . ? C24 C25 C26 113.1(3) . . ? C25 C26 P1 116.6(3) . . ? C36 C31 C32 118.2(3) . . ? C36 C31 P1 119.8(3) . . ? C32 C31 P1 121.5(3) . . ? C33 C32 C31 120.0(4) . . ? C34 C33 C32 120.9(4) . . ? C33 C34 C35 120.1(3) . . ? C34 C35 C36 120.0(4) . . ? C35 C36 C31 120.8(3) . . ? C42 C41 P2 116.3(3) . . ? C43 C42 C41 117.1(3) . . ? C42 C43 C44 116.9(3) . . ? C45 C44 C43 114.1(3) . . ? C44 C45 C46 115.7(3) . . ? C45 C46 P2 116.4(3) . . ? C56 C51 C52 119.0(3) . . ? C56 C51 P2 120.5(3) . . ? C52 C51 P2 120.6(3) . . ? C53 C52 C51 120.0(4) . . ? C54 C53 C52 120.6(4) . . ? C53 C54 C55 119.4(4) . . ? C54 C55 C56 120.6(4) . . ? C55 C56 C51 120.6(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.893 _refine_diff_density_min -0.996 _refine_diff_density_rms 0.128 data_ts03 _database_code_depnum_ccdc_archive 'CCDC 227270' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H46 Cl F5 P2 Pt' _chemical_formula_weight 890.23 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.64790(10) _cell_length_b 19.0165(3) _cell_length_c 15.0138(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.7190(10) _cell_angle_gamma 90.00 _cell_volume 3731.89(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8701 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 3.968 _exptl_absorpt_correction_type 'empirical (Scalepack)' _exptl_absorpt_correction_T_min 0.3373 _exptl_absorpt_correction_T_max 0.5041 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16508 _diffrn_reflns_av_R_equivalents 0.0130 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8549 _reflns_number_gt 7851 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL NT' _computing_publication_material 'SHELXTL NT' _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^)+(0.0240P)^2^+2.8008P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8549 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0233 _refine_ls_R_factor_gt 0.0199 _refine_ls_wR_factor_ref 0.0505 _refine_ls_wR_factor_gt 0.0491 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 0.682092(6) -0.554836(4) 0.787715(5) 0.01870(3) Uani 1 1 d . . . P1 P 0.59694(4) -0.65583(3) 0.72373(4) 0.02045(11) Uani 1 1 d . . . C1 C 0.46414(17) -0.63658(13) 0.66035(15) 0.0253(5) Uani 1 1 d . . . H1A H 0.4626 -0.6104 0.6029 0.030 Uiso 1 1 calc R . . H1B H 0.4271 -0.6814 0.6417 0.030 Uiso 1 1 calc R . . Cl1 Cl 0.64046(5) -0.51627(3) 0.63138(4) 0.02881(12) Uani 1 1 d . . . C1A C 0.64906(17) -0.69475(12) 0.63519(15) 0.0245(4) Uani 1 1 d . . . H1AA H 0.6309 -0.7453 0.6291 0.029 Uiso 1 1 calc R . . H1AB H 0.6158 -0.6721 0.5747 0.029 Uiso 1 1 calc R . . P2 P 0.76611(4) -0.45087(3) 0.83696(4) 0.02150(12) Uani 1 1 d . . . C2 C 0.40843(17) -0.59335(14) 0.71706(16) 0.0288(5) Uani 1 1 d . . . H2A H 0.4090 -0.6198 0.7740 0.035 Uiso 1 1 calc R . . H2B H 0.4460 -0.5488 0.7365 0.035 Uiso 1 1 calc R . . C2A C 0.76518(17) -0.68786(13) 0.65531(16) 0.0266(5) Uani 1 1 d . . . H2AA H 0.7844 -0.6376 0.6644 0.032 Uiso 1 1 calc R . . H2AB H 0.7992 -0.7131 0.7137 0.032 Uiso 1 1 calc R . . C3 C 0.29778(18) -0.57643(15) 0.66328(17) 0.0315(5) Uani 1 1 d . . . H3A H 0.2608 -0.5614 0.7079 0.038 Uiso 1 1 calc R . . H3B H 0.2646 -0.6198 0.6324 0.038 Uiso 1 1 calc R . . C3A C 0.80305(18) -0.71751(14) 0.57695(17) 0.0310(5) Uani 1 1 d . . . H3AA H 0.7621 -0.6970 0.5173 0.037 Uiso 1 1 calc R . . H3AB H 0.7919 -0.7690 0.5735 0.037 Uiso 1 1 calc R . . C4 C 0.28728(18) -0.51897(14) 0.58976(17) 0.0317(5) Uani 1 1 d . . . H4A H 0.3290 -0.5319 0.5482 0.038 Uiso 1 1 calc R . . H4B H 0.2150 -0.5163 0.5515 0.038 Uiso 1 1 calc R . . C4A C 0.91635(19) -0.70265(14) 0.58927(18) 0.0347(6) Uani 1 1 d . . . H4AA H 0.9574 -0.7218 0.6498 0.042 Uiso 1 1 calc R . . H4AB H 0.9377 -0.7270 0.5396 0.042 Uiso 1 1 calc R . . C5 C 0.3205(2) -0.44793(14) 0.63133(19) 0.0349(6) Uani 1 1 d . . . H5A H 0.2929 -0.4322 0.6791 0.042 Uiso 1 1 calc R . . C5A C 0.93756(19) -0.62586(15) 0.58573(18) 0.0346(6) Uani 1 1 d . . . H5AA H 0.8943 -0.5998 0.5357 0.041 Uiso 1 1 calc R . . C6 C 0.3846(2) -0.40585(14) 0.60688(17) 0.0347(6) Uani 1 1 d . . . H6A H 0.4122 -0.4224 0.5594 0.042 Uiso 1 1 calc R . . C6A C 1.01083(19) -0.59103(15) 0.64571(19) 0.0351(6) Uani 1 1 d . . . H6AA H 1.0573 -0.6177 0.6928 0.042 Uiso 1 1 calc R . . C7 C 0.4191(2) -0.33432(14) 0.6459(2) 0.0408(6) Uani 1 1 d . . . H7A H 0.3972 -0.3267 0.7026 0.049 Uiso 1 1 calc R . . H7B H 0.3858 -0.2980 0.5999 0.049 Uiso 1 1 calc R . . C7A C 1.0276(2) -0.51350(15) 0.6465(2) 0.0375(6) Uani 1 1 d . . . H7AA H 0.9767 -0.4921 0.5927 0.045 Uiso 1 1 calc R . . H7AB H 1.0965 -0.5039 0.6400 0.045 Uiso 1 1 calc R . . C8 C 0.5352(2) -0.32587(14) 0.67013(18) 0.0365(6) Uani 1 1 d . . . H8A H 0.5580 -0.3386 0.6153 0.044 Uiso 1 1 calc R . . H8B H 0.5533 -0.2760 0.6852 0.044 Uiso 1 1 calc R . . C8A C 1.01856(19) -0.47963(15) 0.73594(19) 0.0357(6) Uani 1 1 d . . . H8AA H 1.0654 -0.5036 0.7902 0.043 Uiso 1 1 calc R . . H8AB H 1.0393 -0.4297 0.7376 0.043 Uiso 1 1 calc R . . C9 C 0.59122(18) -0.37159(13) 0.75212(16) 0.0289(5) Uani 1 1 d . . . H9A H 0.5604 -0.4191 0.7440 0.035 Uiso 1 1 calc R . . H9B H 0.5819 -0.3514 0.8099 0.035 Uiso 1 1 calc R . . C9A C 0.90930(18) -0.48427(15) 0.74258(18) 0.0340(6) Uani 1 1 d . . . H9AA H 0.8886 -0.5343 0.7402 0.041 Uiso 1 1 calc R . . H9AB H 0.8627 -0.4601 0.6883 0.041 Uiso 1 1 calc R . . C10 C 0.70575(18) -0.37799(12) 0.76271(15) 0.0261(5) Uani 1 1 d . . . H10A H 0.7400 -0.3336 0.7891 0.031 Uiso 1 1 calc R . . H10B H 0.7157 -0.3843 0.7004 0.031 Uiso 1 1 calc R . . C10A C 0.89801(19) -0.45128(13) 0.83159(18) 0.0308(5) Uani 1 1 d . . . H10C H 0.9236 -0.4023 0.8361 0.037 Uiso 1 1 calc R . . H10D H 0.9410 -0.4776 0.8857 0.037 Uiso 1 1 calc R . . C11 C 0.71490(16) -0.59070(12) 0.91933(14) 0.0215(4) Uani 1 1 d . . . F12 F 0.54904(11) -0.56640(9) 0.93071(10) 0.0395(4) Uani 1 1 d . . . C12 C 0.64434(17) -0.59278(14) 0.96898(16) 0.0289(5) Uani 1 1 d . . . F13 F 0.58975(14) -0.62208(14) 1.10046(12) 0.0717(6) Uani 1 1 d . . . C13 C 0.6626(2) -0.62140(17) 1.05652(18) 0.0424(7) Uani 1 1 d . . . F14 F 0.77695(15) -0.67871(13) 1.18447(12) 0.0706(6) Uani 1 1 d . . . C14 C 0.7574(2) -0.64936(17) 1.09957(18) 0.0438(7) Uani 1 1 d . . . F15 F 0.92339(12) -0.67778(9) 1.09372(12) 0.0497(4) Uani 1 1 d . . . C15 C 0.83109(19) -0.64845(14) 1.05361(18) 0.0355(6) Uani 1 1 d . . . F16 F 0.88489(10) -0.62130(9) 0.92418(11) 0.0398(4) Uani 1 1 d . . . C16 C 0.80918(17) -0.61899(13) 0.96625(16) 0.0267(5) Uani 1 1 d . . . C21 C 0.59490(17) -0.72729(12) 0.80389(15) 0.0234(4) Uani 1 1 d . . . C22 C 0.50465(19) -0.75561(13) 0.81417(16) 0.0302(5) Uani 1 1 d . . . H22A H 0.4406 -0.7393 0.7759 0.036 Uiso 1 1 calc R . . C23 C 0.5077(2) -0.80740(14) 0.87967(19) 0.0387(6) Uani 1 1 d . . . H23A H 0.4456 -0.8260 0.8865 0.046 Uiso 1 1 calc R . . C24 C 0.6004(2) -0.83240(14) 0.93542(18) 0.0387(6) Uani 1 1 d . . . H24A H 0.6020 -0.8676 0.9807 0.046 Uiso 1 1 calc R . . C25 C 0.6908(2) -0.80577(13) 0.92472(17) 0.0342(5) Uani 1 1 d . . . H25A H 0.7546 -0.8233 0.9619 0.041 Uiso 1 1 calc R . . C26 C 0.68799(18) -0.75349(12) 0.85968(16) 0.0271(5) Uani 1 1 d . . . H26A H 0.7503 -0.7352 0.8530 0.032 Uiso 1 1 calc R . . C31 C 0.77390(17) -0.41895(12) 0.95270(15) 0.0236(4) Uani 1 1 d . . . C32 C 0.86313(18) -0.38904(13) 1.01040(16) 0.0294(5) Uani 1 1 d . . . H32A H 0.9242 -0.3895 0.9920 0.035 Uiso 1 1 calc R . . C33 C 0.8631(2) -0.35864(14) 1.09450(17) 0.0364(6) Uani 1 1 d . . . H33A H 0.9243 -0.3387 1.1336 0.044 Uiso 1 1 calc R . . C34 C 0.7750(2) -0.35718(15) 1.12147(17) 0.0402(6) Uani 1 1 d . . . H34A H 0.7749 -0.3357 1.1786 0.048 Uiso 1 1 calc R . . C35 C 0.6862(2) -0.38723(15) 1.06480(17) 0.0385(6) Uani 1 1 d . . . H35A H 0.6253 -0.3863 1.0833 0.046 Uiso 1 1 calc R . . C36 C 0.68585(18) -0.41843(14) 0.98177(16) 0.0294(5) Uani 1 1 d . . . H36A H 0.6250 -0.4397 0.9441 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01791(5) 0.02102(5) 0.01712(5) 0.00074(3) 0.00496(3) -0.00030(3) P1 0.0197(3) 0.0234(3) 0.0184(2) -0.0002(2) 0.0057(2) -0.0003(2) C1 0.0221(11) 0.0316(12) 0.0210(10) -0.0021(9) 0.0042(8) 0.0011(9) Cl1 0.0393(3) 0.0290(3) 0.0183(2) 0.0023(2) 0.0087(2) -0.0009(2) C1A 0.0264(11) 0.0276(12) 0.0201(10) -0.0025(9) 0.0077(9) 0.0016(9) P2 0.0197(3) 0.0238(3) 0.0214(3) 0.0002(2) 0.0066(2) -0.0020(2) C2 0.0241(11) 0.0389(14) 0.0229(11) -0.0005(10) 0.0059(9) 0.0041(10) C2A 0.0263(11) 0.0298(12) 0.0262(11) -0.0020(9) 0.0116(9) 0.0018(9) C3 0.0209(11) 0.0434(14) 0.0300(12) 0.0032(11) 0.0071(9) 0.0037(10) C3A 0.0352(13) 0.0329(13) 0.0281(12) -0.0010(10) 0.0142(10) 0.0045(10) C4 0.0231(11) 0.0409(15) 0.0292(12) 0.0014(11) 0.0045(9) 0.0018(10) C4A 0.0341(13) 0.0406(15) 0.0340(13) 0.0061(11) 0.0172(11) 0.0103(11) C5 0.0315(14) 0.0418(15) 0.0300(13) -0.0018(11) 0.0063(11) 0.0071(10) C5A 0.0308(13) 0.0437(15) 0.0341(13) 0.0099(11) 0.0173(11) 0.0102(11) C6 0.0361(14) 0.0358(14) 0.0271(12) 0.0019(10) 0.0010(10) 0.0028(11) C6A 0.0298(13) 0.0418(15) 0.0386(14) 0.0074(12) 0.0178(11) 0.0125(11) C7 0.0393(14) 0.0328(14) 0.0393(14) 0.0035(12) -0.0061(11) 0.0076(11) C7A 0.0289(13) 0.0439(16) 0.0456(15) 0.0069(12) 0.0200(11) 0.0028(11) C8 0.0438(15) 0.0287(13) 0.0297(12) 0.0035(10) -0.0012(11) -0.0007(11) C8A 0.0263(12) 0.0392(15) 0.0456(15) 0.0012(12) 0.0168(11) -0.0019(10) C9 0.0336(13) 0.0275(12) 0.0242(11) 0.0008(9) 0.0059(9) 0.0048(10) C9A 0.0262(12) 0.0437(15) 0.0365(13) -0.0048(11) 0.0159(10) -0.0046(10) C10 0.0337(12) 0.0221(11) 0.0228(10) -0.0002(9) 0.0083(9) -0.0001(9) C10A 0.0239(12) 0.0342(14) 0.0360(13) -0.0021(10) 0.0116(10) -0.0034(9) C11 0.0209(10) 0.0238(11) 0.0184(10) 0.0012(8) 0.0033(8) -0.0043(8) F12 0.0229(7) 0.0655(11) 0.0315(8) 0.0099(7) 0.0099(6) 0.0059(7) C12 0.0226(11) 0.0401(14) 0.0227(11) 0.0039(10) 0.0046(9) -0.0010(10) F13 0.0523(11) 0.132(2) 0.0400(10) 0.0302(11) 0.0281(9) 0.0077(12) C13 0.0370(14) 0.066(2) 0.0264(12) 0.0112(13) 0.0123(11) -0.0037(13) F14 0.0632(12) 0.1093(18) 0.0333(9) 0.0385(10) 0.0043(8) 0.0021(12) C14 0.0444(16) 0.0574(19) 0.0238(12) 0.0149(12) 0.0007(11) -0.0055(13) F15 0.0326(8) 0.0560(11) 0.0477(9) 0.0209(8) -0.0089(7) 0.0048(7) C15 0.0273(12) 0.0385(14) 0.0315(12) 0.0087(11) -0.0063(10) -0.0038(10) F16 0.0219(7) 0.0538(10) 0.0430(8) 0.0106(7) 0.0084(6) 0.0057(6) C16 0.0208(11) 0.0294(12) 0.0271(11) 0.0032(9) 0.0026(9) -0.0034(9) C21 0.0287(11) 0.0234(11) 0.0200(10) -0.0033(8) 0.0099(9) -0.0029(9) C22 0.0322(13) 0.0312(13) 0.0281(12) -0.0027(10) 0.0100(10) -0.0070(10) C23 0.0477(16) 0.0342(14) 0.0382(14) -0.0021(11) 0.0188(12) -0.0129(12) C24 0.0599(18) 0.0299(13) 0.0300(13) 0.0035(11) 0.0188(12) -0.0058(12) C25 0.0467(15) 0.0300(13) 0.0266(12) 0.0019(10) 0.0115(11) 0.0057(11) C26 0.0303(12) 0.0271(12) 0.0255(11) 0.0002(9) 0.0106(9) -0.0001(9) C31 0.0260(11) 0.0218(11) 0.0213(10) 0.0007(9) 0.0041(8) -0.0012(9) C32 0.0245(12) 0.0310(13) 0.0300(12) 0.0000(10) 0.0033(9) -0.0032(9) C33 0.0384(14) 0.0385(14) 0.0263(12) -0.0033(10) -0.0002(10) -0.0092(11) C34 0.0510(16) 0.0461(16) 0.0225(12) -0.0057(11) 0.0090(11) -0.0102(13) C35 0.0413(15) 0.0516(17) 0.0262(12) -0.0027(11) 0.0154(11) -0.0091(12) C36 0.0279(12) 0.0365(13) 0.0236(11) -0.0014(10) 0.0069(9) -0.0077(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C11 2.015(2) . ? Pt1 P2 2.2984(6) . ? Pt1 P1 2.3064(6) . ? Pt1 Cl1 2.3671(5) . ? P1 C21 1.821(2) . ? P1 C1 1.825(2) . ? P1 C1A 1.834(2) . ? C1 C2 1.533(3) . ? C1A C2A 1.531(3) . ? P2 C31 1.815(2) . ? P2 C10 1.820(2) . ? P2 C10A 1.825(2) . ? C2 C3 1.528(3) . ? C2A C3A 1.523(3) . ? C3 C4 1.530(4) . ? C3A C4A 1.530(3) . ? C4 C5 1.502(4) . ? C4A C5A 1.493(4) . ? C5 C6 1.314(4) . ? C5A C6A 1.316(4) . ? C6 C7 1.502(4) . ? C6A C7A 1.492(4) . ? C7 C8 1.529(4) . ? C7A C8A 1.526(4) . ? C8 C9 1.521(3) . ? C8A C9A 1.525(3) . ? C9 C10 1.530(3) . ? C9A C10A 1.524(3) . ? C11 C12 1.378(3) . ? C11 C16 1.386(3) . ? F12 C12 1.358(3) . ? C12 C13 1.377(3) . ? F13 C13 1.342(3) . ? C13 C14 1.376(4) . ? F14 C14 1.346(3) . ? C14 C15 1.374(4) . ? F15 C15 1.351(3) . ? C15 C16 1.378(3) . ? F16 C16 1.358(3) . ? C21 C22 1.393(3) . ? C21 C26 1.397(3) . ? C22 C23 1.384(4) . ? C23 C24 1.385(4) . ? C24 C25 1.385(4) . ? C25 C26 1.386(3) . ? C31 C36 1.392(3) . ? C31 C32 1.396(3) . ? C32 C33 1.389(4) . ? C33 C34 1.375(4) . ? C34 C35 1.388(4) . ? C35 C36 1.379(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 C11 Pt1 P2 91.50(6) . . ? C11 Pt1 P1 94.00(6) . . ? P2 Pt1 P1 174.41(2) . . ? C11 Pt1 Cl1 178.06(6) . . ? P2 Pt1 Cl1 90.44(2) . . ? P1 Pt1 Cl1 84.062(19) . . ? C21 P1 C1 107.02(11) . . ? C21 P1 C1A 105.11(10) . . ? C1 P1 C1A 103.71(10) . . ? C21 P1 Pt1 116.61(7) . . ? C1 P1 Pt1 110.85(8) . . ? C1A P1 Pt1 112.57(8) . . ? C2 C1 P1 113.24(15) . . ? C2A C1A P1 114.68(15) . . ? C31 P2 C10 102.90(11) . . ? C31 P2 C10A 104.89(11) . . ? C10 P2 C10A 104.74(11) . . ? C31 P2 Pt1 118.83(8) . . ? C10 P2 Pt1 111.22(8) . . ? C10A P2 Pt1 112.90(8) . . ? C3 C2 C1 113.08(19) . . ? C3A C2A C1A 112.21(19) . . ? C2 C3 C4 113.9(2) . . ? C2A C3A C4A 113.2(2) . . ? C5 C4 C3 112.8(2) . . ? C5A C4A C3A 112.1(2) . . ? C6 C5 C4 125.3(2) . . ? C6A C5A C4A 125.8(2) . . ? C5 C6 C7 127.0(3) . . ? C5A C6A C7A 126.0(2) . . ? C6 C7 C8 112.0(2) . . ? C6A C7A C8A 111.9(2) . . ? C9 C8 C7 112.2(2) . . ? C9A C8A C7A 111.2(2) . . ? C8 C9 C10 113.0(2) . . ? C8A C9A C10A 112.4(2) . . ? C9 C10 P2 113.14(16) . . ? C9A C10A P2 112.98(17) . . ? C12 C11 C16 113.9(2) . . ? C12 C11 Pt1 123.21(16) . . ? C16 C11 Pt1 122.81(16) . . ? F12 C12 C11 119.6(2) . . ? F12 C12 C13 116.0(2) . . ? C11 C12 C13 124.4(2) . . ? F13 C13 C14 119.7(2) . . ? F13 C13 C12 121.1(2) . . ? C14 C13 C12 119.3(2) . . ? F14 C14 C13 120.6(3) . . ? F14 C14 C15 120.4(3) . . ? C13 C14 C15 119.0(2) . . ? F15 C15 C16 120.8(2) . . ? F15 C15 C14 119.6(2) . . ? C16 C15 C14 119.6(2) . . ? F16 C16 C15 116.4(2) . . ? F16 C16 C11 119.7(2) . . ? C15 C16 C11 123.9(2) . . ? C22 C21 C26 118.4(2) . . ? C22 C21 P1 122.95(18) . . ? C26 C21 P1 118.58(17) . . ? C23 C22 C21 120.5(2) . . ? C22 C23 C24 120.6(2) . . ? C25 C24 C23 119.6(2) . . ? C26 C25 C24 119.9(2) . . ? C25 C26 C21 120.9(2) . . ? C36 C31 C32 118.7(2) . . ? C36 C31 P2 118.99(17) . . ? C32 C31 P2 122.05(18) . . ? C33 C32 C31 120.4(2) . . ? C34 C33 C32 120.3(2) . . ? C33 C34 C35 119.6(2) . . ? C36 C35 C34 120.4(2) . . ? C35 C36 C31 120.5(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.997 _refine_diff_density_min -0.966 _refine_diff_density_rms 0.085