Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Clerac, Rodolphe' 'Gabbai, F.' 'Gardinier, James R.' _publ_contact_author_name 'Dr F Gabbai' _publ_contact_author_address ; Department of Chemistry Texas A&M University College Station Texas 77843-3255 USA ; _publ_contact_author_email 'FRANCOIS@TAMU.EDU' _publ_section_title ; Preparation, Structural Studies, and Magnetic Properties of Co-ordination Complexes of Bimetallic Arylplatinum Compounds and Pyridyl Nitronyl Nitroxide Radicals ; data_compound_1 _database_code_CSD 171201 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1,4-bis((PEt3)2Platinumiodide)benzene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H64 I2 P4 Pt2' _chemical_formula_weight 1192.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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 7.4670(15) _cell_length_b 15.906(3) _cell_length_c 16.692(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.37(3) _cell_angle_gamma 90.00 _cell_volume 1950.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.031 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 8.931 _exptl_absorpt_correction_type SADABST _exptl_absorpt_correction_T_min 0.436641 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16791 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 24.00 _reflns_number_total 3059 _reflns_number_gt 2983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+5.4802P] 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 3059 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.257 _refine_ls_restrained_S_all 1.257 _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 0.59142(2) 0.838575(11) 0.140470(10) 0.01573(9) Uani 1 1 d . . . I1 I 0.67873(5) 0.71958(2) 0.257475(19) 0.02561(11) Uani 1 1 d . . . P1 P 0.64213(16) 0.75294(8) 0.03578(7) 0.0176(3) Uani 1 1 d . . . P2 P 0.48137(16) 0.92124(8) 0.23369(7) 0.0180(3) Uani 1 1 d . . . C1 C 0.5365(6) 0.9325(3) 0.0581(3) 0.0177(10) Uani 1 1 d . . . C3 C 0.6639(7) 0.9963(3) 0.0534(3) 0.0202(10) Uani 1 1 d . . . H2A H 0.7752 0.9951 0.0889 0.024 Uiso 1 1 calc R . . C2 C 0.3720(6) 0.9384(3) 0.0031(3) 0.0211(10) Uani 1 1 d . . . H3A H 0.2834 0.8975 0.0042 0.025 Uiso 1 1 calc R . . C4 C 0.7116(7) 0.8006(3) -0.0532(3) 0.0252(11) Uani 1 1 d . . . H4A H 0.7014 0.7589 -0.0961 0.030 Uiso 1 1 calc R . . H4B H 0.6281 0.8460 -0.0726 0.030 Uiso 1 1 calc R . . C5 C 0.9054(8) 0.8354(3) -0.0375(3) 0.0305(13) Uani 1 1 d . . . H5A H 0.9321 0.8593 -0.0868 0.046 Uiso 1 1 calc R . . H5B H 0.9896 0.7907 -0.0197 0.046 Uiso 1 1 calc R . . H5C H 0.9162 0.8779 0.0039 0.046 Uiso 1 1 calc R . . C6 C 0.8002(8) 0.6658(3) 0.0616(3) 0.0266(12) Uani 1 1 d . . . H6A H 0.9197 0.6889 0.0825 0.032 Uiso 1 1 calc R . . H6B H 0.7626 0.6340 0.1053 0.032 Uiso 1 1 calc R . . C7 C 0.8181(8) 0.6046(4) -0.0078(3) 0.0330(13) Uani 1 1 d . . . H7A H 0.9036 0.5612 0.0125 0.049 Uiso 1 1 calc R . . H7B H 0.8602 0.6345 -0.0508 0.049 Uiso 1 1 calc R . . H7C H 0.7016 0.5798 -0.0283 0.049 Uiso 1 1 calc R . . C8 C 0.4271(7) 0.7031(3) -0.0106(3) 0.0261(11) Uani 1 1 d . . . H8A H 0.3411 0.7467 -0.0325 0.031 Uiso 1 1 calc R . . H8B H 0.4483 0.6685 -0.0559 0.031 Uiso 1 1 calc R . . C9 C 0.3415(8) 0.6486(4) 0.0477(4) 0.0363(14) Uani 1 1 d . . . H9A H 0.2301 0.6247 0.0191 0.054 Uiso 1 1 calc R . . H9B H 0.3164 0.6825 0.0919 0.054 Uiso 1 1 calc R . . H9C H 0.4242 0.6044 0.0686 0.054 Uiso 1 1 calc R . . C10 C 0.2775(7) 0.8730(4) 0.2591(3) 0.0276(11) Uani 1 1 d . . . H10A H 0.3094 0.8193 0.2853 0.033 Uiso 1 1 calc R . . H10B H 0.2298 0.9086 0.2974 0.033 Uiso 1 1 calc R . . C11 C 0.1304(8) 0.8594(4) 0.1842(4) 0.0420(15) Uani 1 1 d . . . H11A H 0.0254 0.8344 0.2004 0.063 Uiso 1 1 calc R . . H11B H 0.1758 0.8228 0.1468 0.063 Uiso 1 1 calc R . . H11C H 0.0974 0.9125 0.1584 0.063 Uiso 1 1 calc R . . C12 C 0.6315(7) 0.9347(3) 0.3324(3) 0.0234(11) Uani 1 1 d . . . H12A H 0.5771 0.9746 0.3649 0.028 Uiso 1 1 calc R . . H12B H 0.6434 0.8813 0.3611 0.028 Uiso 1 1 calc R . . C13 C 0.8189(7) 0.9657(4) 0.3233(3) 0.0327(12) Uani 1 1 d . . . H13A H 0.8933 0.9721 0.3762 0.049 Uiso 1 1 calc R . . H13B H 0.8078 1.0189 0.2957 0.049 Uiso 1 1 calc R . . H13C H 0.8743 0.9257 0.2923 0.049 Uiso 1 1 calc R . . C14 C 0.4132(7) 1.0284(3) 0.2022(3) 0.0262(11) Uani 1 1 d . . . H14A H 0.5214 1.0595 0.1956 0.031 Uiso 1 1 calc R . . H14B H 0.3345 1.0258 0.1493 0.031 Uiso 1 1 calc R . . C15 C 0.3152(8) 1.0779(4) 0.2596(3) 0.0362(13) Uani 1 1 d . . . H15A H 0.2854 1.1329 0.2374 0.054 Uiso 1 1 calc R . . H15B H 0.3929 1.0830 0.3118 0.054 Uiso 1 1 calc R . . H15C H 0.2055 1.0490 0.2655 0.054 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 0.01884(13) 0.01404(13) 0.01455(13) 0.00114(6) 0.00370(8) 0.00049(6) I1 0.0390(2) 0.01912(19) 0.01882(18) 0.00391(12) 0.00554(14) 0.00387(13) P1 0.0201(6) 0.0176(6) 0.0152(6) -0.0003(5) 0.0037(5) 0.0003(5) P2 0.0203(6) 0.0178(6) 0.0164(6) 0.0004(5) 0.0043(5) 0.0016(5) C1 0.021(2) 0.018(2) 0.016(2) -0.0025(19) 0.0094(19) 0.0008(19) C3 0.021(2) 0.018(2) 0.021(2) 0.000(2) 0.0030(19) 0.0032(19) C2 0.018(2) 0.022(3) 0.023(3) -0.001(2) 0.005(2) -0.003(2) C4 0.037(3) 0.021(3) 0.016(2) -0.001(2) 0.000(2) 0.013(2) C5 0.033(3) 0.035(3) 0.028(3) 0.004(2) 0.015(2) -0.002(2) C6 0.040(3) 0.018(3) 0.017(3) -0.0016(19) -0.006(2) 0.009(2) C7 0.040(3) 0.032(3) 0.026(3) -0.001(2) 0.003(2) 0.011(3) C8 0.030(3) 0.025(3) 0.025(3) -0.001(2) 0.007(2) -0.002(2) C9 0.033(3) 0.040(3) 0.033(3) -0.005(3) 0.000(3) -0.012(3) C10 0.025(3) 0.034(3) 0.027(3) -0.002(2) 0.013(2) -0.002(2) C11 0.023(3) 0.062(4) 0.042(4) -0.012(3) 0.010(3) -0.010(3) C12 0.030(3) 0.023(3) 0.017(2) -0.003(2) 0.003(2) 0.003(2) C13 0.032(3) 0.029(3) 0.036(3) -0.006(2) 0.002(2) -0.004(2) C14 0.033(3) 0.020(3) 0.025(3) 0.004(2) 0.001(2) 0.008(2) C15 0.045(3) 0.032(3) 0.032(3) -0.004(2) 0.007(3) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.021(5) . ? Pt1 P2 2.2991(13) . ? Pt1 P1 2.3002(12) . ? Pt1 I1 2.7136(6) . ? P1 C6 1.821(5) . ? P1 C4 1.824(5) . ? P1 C8 1.833(5) . ? P2 C10 1.822(5) . ? P2 C14 1.829(5) . ? P2 C12 1.831(5) . ? C1 C2 1.398(7) . ? C1 C3 1.404(7) . ? C3 C2 1.395(7) 3_675 ? C2 C3 1.395(7) 3_675 ? C4 C5 1.527(8) . ? C6 C7 1.537(7) . ? C8 C9 1.526(8) . ? C10 C11 1.523(8) . ? C12 C13 1.518(7) . ? C14 C15 1.524(7) . ? 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 P2 89.11(13) . . ? C1 Pt1 P1 87.80(13) . . ? P2 Pt1 P1 168.71(4) . . ? C1 Pt1 I1 176.32(13) . . ? P2 Pt1 I1 88.89(3) . . ? P1 Pt1 I1 94.74(3) . . ? C6 P1 C4 104.0(3) . . ? C6 P1 C8 104.6(3) . . ? C4 P1 C8 101.0(2) . . ? C6 P1 Pt1 117.36(17) . . ? C4 P1 Pt1 118.82(17) . . ? C8 P1 Pt1 109.00(17) . . ? C10 P2 C14 105.0(3) . . ? C10 P2 C12 104.0(2) . . ? C14 P2 C12 104.1(2) . . ? C10 P2 Pt1 109.38(18) . . ? C14 P2 Pt1 116.98(17) . . ? C12 P2 Pt1 116.14(17) . . ? C2 C1 C3 116.0(4) . . ? C2 C1 Pt1 122.9(3) . . ? C3 C1 Pt1 121.1(4) . . ? C2 C3 C1 121.8(5) 3_675 . ? C3 C2 C1 122.2(4) 3_675 . ? C5 C4 P1 114.2(4) . . ? C7 C6 P1 116.4(4) . . ? C9 C8 P1 114.3(4) . . ? C11 C10 P2 112.2(4) . . ? C13 C12 P2 111.9(4) . . ? C15 C14 P2 116.2(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.396 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.175 #===END data_compound_2 _database_code_CSD 171202 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1,4-bis(bis(PEt3)platinumiodide)benzene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H64 I2 P4 Pt2' _chemical_formula_weight 1192.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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 Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 10.2652(15) _cell_length_b 10.2652(15) _cell_length_c 38.177(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4022.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 8.659 _exptl_absorpt_correction_type SADABST _exptl_absorpt_correction_T_min 0.604206 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25115 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 24.00 _reflns_number_total 3163 _reflns_number_gt 3097 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+14.9881P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.044(8) _refine_ls_number_reflns 3163 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _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 0.21370(3) 0.83065(3) 0.028218(8) 0.02446(11) Uani 1 1 d . . . I1 I 0.46285(5) 0.79379(6) 0.048880(14) 0.03387(16) Uani 1 1 d . . . P1 P 0.25879(18) 0.7165(2) -0.02233(5) 0.0252(4) Uani 1 1 d . . . P2 P 0.1673(2) 0.9164(2) 0.08224(5) 0.0270(5) Uani 1 1 d . . . C1 C 0.0303(8) 0.8716(8) 0.01138(19) 0.0229(17) Uani 1 1 d . . . C2 C -0.0676(7) 0.7788(8) 0.0115(2) 0.0249(16) Uani 1 1 d . . . H2A H -0.0487 0.6954 0.0196 0.030 Uiso 1 1 calc R . . C3 C -0.1937(7) 0.8063(7) 0.0000 0.028(3) Uani 1 2 d S . . H3A H -0.2578 0.7422 0.0000 0.034 Uiso 1 2 calc SR . . C4 C -0.0034(8) 0.9966(8) 0.0000 0.025(2) Uani 1 2 d S . . H4A H 0.0606 1.0606 0.0000 0.030 Uiso 1 2 calc SR . . C5 C 0.3962(8) 0.7792(9) -0.0476(2) 0.0318(18) Uani 1 1 d . . . H5A H 0.4721 0.7841 -0.0325 0.038 Uiso 1 1 calc R . . H5B H 0.4158 0.7185 -0.0664 0.038 Uiso 1 1 calc R . . C6 C 0.3708(10) 0.9134(10) -0.0634(3) 0.047(3) Uani 1 1 d . . . H6A H 0.4458 0.9411 -0.0764 0.070 Uiso 1 1 calc R . . H6B H 0.3537 0.9746 -0.0449 0.070 Uiso 1 1 calc R . . H6C H 0.2967 0.9091 -0.0787 0.070 Uiso 1 1 calc R . . C7 C 0.3064(9) 0.5482(8) -0.0118(2) 0.038(2) Uani 1 1 d . . . H7A H 0.3234 0.5014 -0.0334 0.045 Uiso 1 1 calc R . . H7B H 0.3865 0.5496 0.0017 0.045 Uiso 1 1 calc R . . C8 C 0.2025(10) 0.4760(8) 0.0089(3) 0.043(2) Uani 1 1 d . . . H8A H 0.2318 0.3891 0.0138 0.065 Uiso 1 1 calc R . . H8B H 0.1235 0.4726 -0.0045 0.065 Uiso 1 1 calc R . . H8C H 0.1865 0.5209 0.0306 0.065 Uiso 1 1 calc R . . C9 C 0.1287(7) 0.6962(9) -0.0541(2) 0.0299(19) Uani 1 1 d . . . H9A H 0.0583 0.6487 -0.0430 0.036 Uiso 1 1 calc R . . H9B H 0.0956 0.7817 -0.0602 0.036 Uiso 1 1 calc R . . C10 C 0.1660(9) 0.6250(8) -0.0880(2) 0.036(2) Uani 1 1 d . . . H10A H 0.0911 0.6191 -0.1029 0.053 Uiso 1 1 calc R . . H10B H 0.1964 0.5390 -0.0824 0.053 Uiso 1 1 calc R . . H10C H 0.2337 0.6724 -0.0997 0.053 Uiso 1 1 calc R . . C11 C 0.2036(9) 0.8031(8) 0.1183(2) 0.038(2) Uani 1 1 d . . . H11A H 0.2972 0.7947 0.1209 0.045 Uiso 1 1 calc R . . H11B H 0.1693 0.8383 0.1400 0.045 Uiso 1 1 calc R . . C12 C 0.1439(13) 0.6682(10) 0.1118(3) 0.067(4) Uani 1 1 d . . . H12A H 0.1651 0.6113 0.1309 0.100 Uiso 1 1 calc R . . H12B H 0.1783 0.6328 0.0904 0.100 Uiso 1 1 calc R . . H12C H 0.0510 0.6760 0.1099 0.100 Uiso 1 1 calc R . . C13 C 0.2624(9) 1.0595(8) 0.0941(2) 0.034(2) Uani 1 1 d . . . H13A H 0.2415 1.0836 0.1180 0.040 Uiso 1 1 calc R . . H13B H 0.3542 1.0370 0.0934 0.040 Uiso 1 1 calc R . . C14 C 0.2395(9) 1.1764(9) 0.0705(2) 0.040(2) Uani 1 1 d . . . H14A H 0.2929 1.2477 0.0782 0.059 Uiso 1 1 calc R . . H14B H 0.1495 1.2013 0.0717 0.059 Uiso 1 1 calc R . . H14C H 0.2617 1.1541 0.0469 0.059 Uiso 1 1 calc R . . C15 C -0.0007(8) 0.9651(10) 0.0898(2) 0.037(2) Uani 1 1 d . . . H15A H -0.0230 1.0302 0.0724 0.044 Uiso 1 1 calc R . . H15B H -0.0555 0.8898 0.0855 0.044 Uiso 1 1 calc R . . C16 C -0.0362(9) 1.0191(9) 0.1253(2) 0.039(2) Uani 1 1 d . . . H16A H -0.1272 1.0405 0.1257 0.058 Uiso 1 1 calc R . . H16B H 0.0142 1.0961 0.1298 0.058 Uiso 1 1 calc R . . H16C H -0.0181 0.9551 0.1430 0.058 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 0.02063(17) 0.02355(17) 0.02922(17) 0.00126(13) 0.00154(13) 0.00191(12) I1 0.0227(3) 0.0446(3) 0.0343(3) 0.0012(3) -0.0009(2) 0.0041(2) P1 0.0215(10) 0.0239(10) 0.0303(10) 0.0005(9) 0.0025(8) 0.0033(8) P2 0.0265(11) 0.0243(11) 0.0302(11) 0.0038(8) 0.0019(9) 0.0012(9) C1 0.024(4) 0.025(4) 0.020(4) -0.005(3) 0.007(3) 0.004(3) C2 0.020(4) 0.025(4) 0.030(4) -0.001(3) -0.003(3) 0.006(3) C3 0.025(4) 0.025(4) 0.035(6) -0.011(3) 0.011(3) -0.004(5) C4 0.024(4) 0.024(4) 0.026(6) 0.001(3) -0.001(3) -0.002(5) C5 0.022(4) 0.040(5) 0.034(4) -0.005(4) 0.004(4) 0.006(4) C6 0.054(7) 0.045(6) 0.040(5) 0.006(5) 0.003(5) -0.007(5) C7 0.048(6) 0.023(5) 0.042(5) 0.000(4) 0.007(4) 0.004(4) C8 0.052(6) 0.023(4) 0.054(6) 0.007(4) 0.015(5) 0.005(4) C9 0.020(4) 0.034(5) 0.036(5) -0.003(4) -0.005(3) 0.007(3) C10 0.036(5) 0.034(5) 0.036(5) -0.007(4) 0.001(4) -0.016(4) C11 0.044(5) 0.039(5) 0.029(4) 0.010(4) 0.006(4) 0.013(4) C12 0.105(10) 0.032(5) 0.063(7) 0.012(5) 0.045(7) 0.005(6) C13 0.039(5) 0.025(4) 0.037(5) -0.001(4) 0.000(4) -0.001(4) C14 0.045(5) 0.032(5) 0.042(5) 0.004(4) -0.001(4) -0.003(4) C15 0.016(4) 0.052(6) 0.042(5) -0.006(4) 0.004(4) -0.006(4) C16 0.028(5) 0.041(5) 0.047(5) -0.005(4) -0.001(4) 0.000(4) _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 2.034(8) . ? Pt1 P2 2.292(2) . ? Pt1 P1 2.304(2) . ? Pt1 I1 2.7031(7) . ? P1 C9 1.815(8) . ? P1 C5 1.826(8) . ? P1 C7 1.841(9) . ? P2 C15 1.819(9) . ? P2 C13 1.821(9) . ? P2 C11 1.841(8) . ? C1 C2 1.385(11) . ? C1 C4 1.397(9) . ? C2 C3 1.396(9) . ? C3 C2 1.396(9) 7_465 ? C4 C1 1.397(9) 7_465 ? C5 C6 1.526(13) . ? C7 C8 1.520(12) . ? C9 C10 1.535(11) . ? C11 C12 1.536(14) . ? C13 C14 1.518(12) . ? C15 C16 1.510(12) . ? 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 P2 90.7(2) . . ? C1 Pt1 P1 91.5(2) . . ? P2 Pt1 P1 172.02(7) . . ? C1 Pt1 I1 175.8(2) . . ? P2 Pt1 I1 89.30(6) . . ? P1 Pt1 I1 89.04(5) . . ? C9 P1 C5 104.8(4) . . ? C9 P1 C7 103.5(4) . . ? C5 P1 C7 103.9(4) . . ? C9 P1 Pt1 118.0(3) . . ? C5 P1 Pt1 114.8(3) . . ? C7 P1 Pt1 110.3(3) . . ? C15 P2 C13 104.3(4) . . ? C15 P2 C11 104.3(4) . . ? C13 P2 C11 102.4(4) . . ? C15 P2 Pt1 116.5(3) . . ? C13 P2 Pt1 115.0(3) . . ? C11 P2 Pt1 112.9(3) . . ? C2 C1 C4 116.9(8) . . ? C2 C1 Pt1 121.9(6) . . ? C4 C1 Pt1 121.2(6) . . ? C1 C2 C3 122.1(8) . . ? C2 C3 C2 118.3(10) 7_465 . ? C1 C4 C1 123.4(10) 7_465 . ? C6 C5 P1 113.2(6) . . ? C8 C7 P1 112.6(6) . . ? C10 C9 P1 115.8(6) . . ? C12 C11 P2 111.5(7) . . ? C14 C13 P2 114.0(6) . . ? C16 C15 P2 118.2(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.508 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.154 #===END <> data_compound_4 _database_code_CSD 171203 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H102 F12 N6 O6 P6 Pt2' _chemical_formula_weight 1747.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 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 13.772(3) _cell_length_b 14.307(3) _cell_length_c 36.198(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.30(3) _cell_angle_gamma 90.00 _cell_volume 7121(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 4.139 _exptl_absorpt_correction_type SADABST _exptl_absorpt_correction_T_min 0.743377 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43624 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 24.00 _reflns_number_total 11201 _reflns_number_gt 9370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+22.1985P] 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 11201 _refine_ls_number_parameters 787 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.656501(17) 0.638451(18) 0.092345(7) 0.02517(9) Uani 1 1 d . . . Pt2 Pt 0.302260(17) 0.884364(17) 0.103180(7) 0.02431(9) Uani 1 1 d . . . P1 P 0.56813(13) 0.50136(12) 0.09215(5) 0.0278(4) Uani 1 1 d . . . P2 P 0.75082(12) 0.77170(12) 0.08724(5) 0.0260(4) Uani 1 1 d . . . P3 P 0.21659(12) 0.74585(12) 0.10330(5) 0.0255(4) Uani 1 1 d . . . P4 P 0.40615(12) 1.01051(12) 0.10642(5) 0.0267(4) Uani 1 1 d . . . P5 P -0.00632(16) 0.77030(17) 0.23962(7) 0.0497(6) Uani 1 1 d . . . P6 P 0.0000 1.0000 0.0000 0.0392(7) Uani 1 2 d S . . P7 P 1.0000 0.5000 0.0000 0.0415(7) Uani 1 2 d S . . F1 F 0.0576(7) 0.7210(9) 0.2127(3) 0.182(5) Uani 1 1 d . . . F2 F 0.0770(8) 0.8364(9) 0.2505(3) 0.208(7) Uani 1 1 d . . . F3 F -0.0397(4) 0.8385(5) 0.2071(2) 0.101(2) Uani 1 1 d . . . F4 F -0.0751(8) 0.8164(6) 0.2666(3) 0.154(4) Uani 1 1 d . . . F5 F -0.0949(6) 0.7059(6) 0.2284(2) 0.125(3) Uani 1 1 d . . . F6 F 0.0249(5) 0.7022(6) 0.2710(2) 0.117(3) Uani 1 1 d . . . F7 F 0.1102(3) 1.0055(5) 0.01503(14) 0.0736(17) Uani 1 1 d . . . F8 F -0.0166(4) 0.9237(6) 0.0290(3) 0.138(4) Uani 1 1 d . . . F9 F -0.0313(5) 1.0723(7) 0.0287(2) 0.133(4) Uani 1 1 d . . . F10 F 1.1146(4) 0.5039(4) 0.0045(2) 0.086(2) Uani 1 1 d . . . F11 F 0.9923(3) 0.5699(3) 0.03423(14) 0.0539(13) Uani 1 1 d . . . F12 F 0.9987(6) 0.4133(4) 0.02692(16) 0.089(2) Uani 1 1 d . . . O1 O 0.9709(4) 0.4151(4) 0.23121(14) 0.0375(12) Uani 1 1 d . . . O2 O 1.1272(4) 0.4313(4) 0.12123(16) 0.0465(14) Uani 1 1 d . . . O3 O 0.0291(4) 1.1047(4) 0.24321(15) 0.0421(13) Uani 1 1 d . . . O4 O -0.1656(4) 1.0753(4) 0.13543(15) 0.0433(13) Uani 1 1 d . . . O5 O -0.2891(6) 1.1916(5) 0.0884(2) 0.085(2) Uani 1 1 d . . . H5B H -0.2631 1.1557 0.1049 0.128 Uiso 1 1 d R . . O6 O 1.1021(10) 0.2302(10) 0.0725(4) 0.075(5) Uiso 0.513(13) 1 d P A 1 H60A H 1.0731 0.1712 0.0657 0.113 Uiso 0.513(13) 1 d PR A 1 H60B H 1.1445 0.2495 0.0537 0.113 Uiso 0.513(13) 1 d PR A 1 O7 O 1.1905(7) 0.2731(6) 0.0793(3) 0.031(3) Uiso 0.487(13) 1 d P A 2 H70A H 1.2478 0.3097 0.0851 0.046 Uiso 0.487(13) 1 d PR A 2 H70B H 1.1874 0.2226 0.0967 0.046 Uiso 0.487(13) 1 d PR A 2 N1 N 1.0353(4) 0.4121(4) 0.20708(17) 0.0311(14) Uani 1 1 d . . . N2 N 1.1078(4) 0.4148(4) 0.15497(18) 0.0359(15) Uani 1 1 d . . . N3 N 0.7782(4) 0.5657(4) 0.11762(16) 0.0287(13) Uani 1 1 d . . . N4 N -0.1341(4) 1.0976(4) 0.16795(17) 0.0324(14) Uani 1 1 d . . . N5 N -0.0443(4) 1.1049(4) 0.21984(17) 0.0316(14) Uani 1 1 d . . . N6 N 0.1912(4) 0.9551(4) 0.13059(16) 0.0273(13) Uani 1 1 d . . . C1 C 0.5427(5) 0.7105(5) 0.06879(19) 0.0268(15) Uani 1 1 d . . . C2 C 0.4773(4) 0.7605(4) 0.09018(19) 0.0235(15) Uani 1 1 d . . . H2A H 0.4848 0.7573 0.1158 0.028 Uiso 1 1 calc R . . C3 C 0.4008(5) 0.8153(4) 0.0738(2) 0.0262(15) Uani 1 1 d . . . C4 C 0.3928(5) 0.8186(5) 0.03530(19) 0.0263(15) Uani 1 1 d . . . H4A H 0.3442 0.8550 0.0237 0.032 Uiso 1 1 calc R . . C5 C 0.4551(5) 0.7694(5) 0.0138(2) 0.0304(16) Uani 1 1 d . . . H5A H 0.4477 0.7728 -0.0118 0.036 Uiso 1 1 calc R . . C6 C 0.5286(5) 0.7150(5) 0.0304(2) 0.0296(16) Uani 1 1 d . . . H6A H 0.5691 0.6810 0.0157 0.036 Uiso 1 1 calc R . . C7 C 0.5578(6) 0.4490(5) 0.1377(2) 0.0373(18) Uani 1 1 d . . . H7A H 0.5215 0.3911 0.1351 0.045 Uiso 1 1 calc R . . H7B H 0.6224 0.4340 0.1482 0.045 Uiso 1 1 calc R . . C8 C 0.5075(6) 0.5132(6) 0.1643(2) 0.047(2) Uani 1 1 d . . . H8A H 0.5036 0.4826 0.1877 0.070 Uiso 1 1 calc R . . H8B H 0.4431 0.5273 0.1543 0.070 Uiso 1 1 calc R . . H8C H 0.5440 0.5700 0.1675 0.070 Uiso 1 1 calc R . . C9 C 0.6290(6) 0.4096(5) 0.0665(2) 0.0411(19) Uani 1 1 d . . . H9A H 0.6906 0.3941 0.0793 0.049 Uiso 1 1 calc R . . H9B H 0.5889 0.3538 0.0655 0.049 Uiso 1 1 calc R . . C10 C 0.6469(7) 0.4413(6) 0.0271(2) 0.054(2) Uani 1 1 d . . . H10A H 0.6787 0.3922 0.0144 0.082 Uiso 1 1 calc R . . H10B H 0.6874 0.4960 0.0281 0.082 Uiso 1 1 calc R . . H10C H 0.5859 0.4557 0.0142 0.082 Uiso 1 1 calc R . . C11 C 0.4446(5) 0.5068(5) 0.0713(2) 0.0394(19) Uani 1 1 d . . . H11A H 0.4075 0.5488 0.0862 0.047 Uiso 1 1 calc R . . H11B H 0.4475 0.5350 0.0471 0.047 Uiso 1 1 calc R . . C12 C 0.3880(6) 0.4161(6) 0.0668(2) 0.046(2) Uani 1 1 d . . . H12A H 0.3245 0.4288 0.0556 0.069 Uiso 1 1 calc R . . H12B H 0.3819 0.3879 0.0906 0.069 Uiso 1 1 calc R . . H12C H 0.4219 0.3742 0.0513 0.069 Uiso 1 1 calc R . . C13 C 0.8104(5) 0.8119(5) 0.1304(2) 0.0337(17) Uani 1 1 d . . . H13A H 0.8495 0.7613 0.1411 0.040 Uiso 1 1 calc R . . H13B H 0.8541 0.8627 0.1250 0.040 Uiso 1 1 calc R . . C14 C 0.7411(6) 0.8453(6) 0.1586(2) 0.0402(19) Uani 1 1 d . . . H14A H 0.7776 0.8656 0.1806 0.060 Uiso 1 1 calc R . . H14B H 0.6988 0.7950 0.1647 0.060 Uiso 1 1 calc R . . H14C H 0.7031 0.8964 0.1485 0.060 Uiso 1 1 calc R . . C15 C 0.8499(5) 0.7487(5) 0.0570(2) 0.0364(18) Uani 1 1 d . . . H15A H 0.8912 0.8036 0.0566 0.044 Uiso 1 1 calc R . . H15B H 0.8889 0.6975 0.0673 0.044 Uiso 1 1 calc R . . C16 C 0.8155(6) 0.7245(6) 0.0177(2) 0.051(2) Uani 1 1 d . . . H16A H 0.8707 0.7133 0.0033 0.077 Uiso 1 1 calc R . . H16B H 0.7781 0.7754 0.0071 0.077 Uiso 1 1 calc R . . H16C H 0.7758 0.6693 0.0178 0.077 Uiso 1 1 calc R . . C17 C 0.6894(5) 0.8737(5) 0.0669(2) 0.0307(16) Uani 1 1 d . . . H17A H 0.6578 0.8553 0.0434 0.037 Uiso 1 1 calc R . . H17B H 0.6388 0.8924 0.0830 0.037 Uiso 1 1 calc R . . C18 C 0.7521(6) 0.9576(5) 0.0604(3) 0.047(2) Uani 1 1 d . . . H18A H 0.7126 1.0070 0.0497 0.070 Uiso 1 1 calc R . . H18B H 0.8014 0.9411 0.0439 0.070 Uiso 1 1 calc R . . H18C H 0.7823 0.9782 0.0836 0.070 Uiso 1 1 calc R . . C19 C 0.2802(5) 0.6602(5) 0.1333(2) 0.0312(16) Uani 1 1 d . . . H19A H 0.2427 0.6028 0.1331 0.037 Uiso 1 1 calc R . . H19B H 0.3427 0.6463 0.1235 0.037 Uiso 1 1 calc R . . C20 C 0.2966(6) 0.6940(5) 0.1734(2) 0.0404(19) Uani 1 1 d . . . H20A H 0.3301 0.6465 0.1879 0.061 Uiso 1 1 calc R . . H20B H 0.2350 0.7066 0.1835 0.061 Uiso 1 1 calc R . . H20C H 0.3350 0.7501 0.1739 0.061 Uiso 1 1 calc R . . C21 C 0.1996(5) 0.6862(5) 0.0593(2) 0.0353(17) Uani 1 1 d . . . H21A H 0.2627 0.6738 0.0498 0.042 Uiso 1 1 calc R . . H21B H 0.1682 0.6266 0.0631 0.042 Uiso 1 1 calc R . . C22 C 0.1380(6) 0.7428(6) 0.0304(2) 0.043(2) Uani 1 1 d . . . H22A H 0.1313 0.7081 0.0077 0.065 Uiso 1 1 calc R . . H22B H 0.1694 0.8013 0.0261 0.065 Uiso 1 1 calc R . . H22C H 0.0748 0.7541 0.0394 0.065 Uiso 1 1 calc R . . C23 C 0.0956(5) 0.7546(5) 0.1214(2) 0.0350(17) Uani 1 1 d . . . H23A H 0.1013 0.7853 0.1453 0.042 Uiso 1 1 calc R . . H23B H 0.0551 0.7935 0.1049 0.042 Uiso 1 1 calc R . . C24 C 0.0458(5) 0.6610(5) 0.1257(2) 0.0394(19) Uani 1 1 d . . . H24A H -0.0170 0.6706 0.1352 0.059 Uiso 1 1 calc R . . H24B H 0.0845 0.6225 0.1425 0.059 Uiso 1 1 calc R . . H24C H 0.0384 0.6307 0.1020 0.059 Uiso 1 1 calc R . . C25 C 0.5136(5) 0.9823(5) 0.1364(2) 0.0298(16) Uani 1 1 d . . . H25A H 0.5441 0.9269 0.1268 0.036 Uiso 1 1 calc R . . H25B H 0.5598 1.0333 0.1354 0.036 Uiso 1 1 calc R . . C26 C 0.4918(6) 0.9652(6) 0.1765(2) 0.050(2) Uani 1 1 d . . . H26A H 0.5511 0.9508 0.1906 0.074 Uiso 1 1 calc R . . H26B H 0.4474 0.9137 0.1778 0.074 Uiso 1 1 calc R . . H26C H 0.4631 1.0202 0.1864 0.074 Uiso 1 1 calc R . . C27 C 0.4551(5) 1.0449(5) 0.0628(2) 0.0383(18) Uani 1 1 d . . . H27A H 0.5043 1.0926 0.0674 0.046 Uiso 1 1 calc R . . H27B H 0.4859 0.9913 0.0519 0.046 Uiso 1 1 calc R . . C28 C 0.3758(7) 1.0825(7) 0.0356(3) 0.063(3) Uani 1 1 d . . . H28A H 0.4039 1.1000 0.0130 0.095 Uiso 1 1 calc R . . H28B H 0.3460 1.1362 0.0462 0.095 Uiso 1 1 calc R . . H28C H 0.3276 1.0350 0.0307 0.095 Uiso 1 1 calc R . . C29 C 0.3586(5) 1.1174(5) 0.1259(3) 0.0408(19) Uani 1 1 d . . . H29A H 0.3052 1.1397 0.1095 0.049 Uiso 1 1 calc R . . H29B H 0.3324 1.1026 0.1495 0.049 Uiso 1 1 calc R . . C30 C 0.4328(6) 1.1964(5) 0.1317(3) 0.050(2) Uani 1 1 d . . . H30A H 0.4019 1.2496 0.1421 0.075 Uiso 1 1 calc R . . H30B H 0.4577 1.2133 0.1084 0.075 Uiso 1 1 calc R . . H30C H 0.4853 1.1758 0.1483 0.075 Uiso 1 1 calc R . . C31 C 0.8412(5) 0.5171(5) 0.0977(2) 0.0290(16) Uani 1 1 d . . . H31A H 0.8313 0.5157 0.0720 0.035 Uiso 1 1 calc R . . C32 C 0.9202(5) 0.4691(5) 0.1141(2) 0.0319(16) Uani 1 1 d . . . H32A H 0.9617 0.4353 0.0997 0.038 Uiso 1 1 calc R . . C33 C 0.9363(5) 0.4726(5) 0.15230(19) 0.0262(15) Uani 1 1 d . . . C34 C 0.8712(5) 0.5227(5) 0.1728(2) 0.0295(16) Uani 1 1 d . . . H34A H 0.8798 0.5259 0.1985 0.035 Uiso 1 1 calc R . . C35 C 0.7944(5) 0.5669(5) 0.1547(2) 0.0300(16) Uani 1 1 d . . . H35A H 0.7511 0.5996 0.1686 0.036 Uiso 1 1 calc R . . C36 C 1.0235(5) 0.4316(5) 0.1706(2) 0.0294(16) Uani 1 1 d . . . C37 C 1.1795(5) 0.3662(5) 0.1810(2) 0.0363(18) Uani 1 1 d . . . C38 C 1.1417(5) 0.3965(5) 0.2185(2) 0.0367(18) Uani 1 1 d . . . C39 C 1.1512(6) 0.3245(6) 0.2491(2) 0.0424(19) Uani 1 1 d . . . H39A H 1.1257 0.3496 0.2712 0.064 Uiso 1 1 calc R . . H39B H 1.2185 0.3088 0.2539 0.064 Uiso 1 1 calc R . . H39C H 1.1154 0.2694 0.2417 0.064 Uiso 1 1 calc R . . C40 C 1.1794(5) 0.4911(6) 0.2327(2) 0.046(2) Uani 1 1 d . . . H40A H 1.1527 0.5045 0.2561 0.069 Uiso 1 1 calc R . . H40B H 1.1601 0.5390 0.2152 0.069 Uiso 1 1 calc R . . H40C H 1.2491 0.4893 0.2358 0.069 Uiso 1 1 calc R . . C41 C 1.1696(6) 0.2615(5) 0.1740(2) 0.045(2) Uani 1 1 d . . . H41A H 1.1941 0.2465 0.1504 0.068 Uiso 1 1 calc R . . H41B H 1.1024 0.2440 0.1741 0.068 Uiso 1 1 calc R . . H41C H 1.2062 0.2280 0.1931 0.068 Uiso 1 1 calc R . . C42 C 1.2814(5) 0.4005(6) 0.1742(3) 0.047(2) Uani 1 1 d . . . H42A H 1.2995 0.3792 0.1504 0.070 Uiso 1 1 calc R . . H42B H 1.3264 0.3764 0.1930 0.070 Uiso 1 1 calc R . . H42C H 1.2825 0.4676 0.1748 0.070 Uiso 1 1 calc R . . C43 C 0.1165(5) 0.9948(5) 0.1106(2) 0.0299(16) Uani 1 1 d . . . H43A H 0.1176 0.9952 0.0849 0.036 Uiso 1 1 calc R . . C44 C 0.0376(5) 1.0351(5) 0.1270(2) 0.0307(16) Uani 1 1 d . . . H44A H -0.0128 1.0616 0.1123 0.037 Uiso 1 1 calc R . . C45 C 0.0345(5) 1.0356(5) 0.1651(2) 0.0297(16) Uani 1 1 d . . . C46 C 0.1134(5) 0.9954(5) 0.1857(2) 0.0290(16) Uani 1 1 d . . . H46A H 0.1153 0.9950 0.2114 0.035 Uiso 1 1 calc R . . C47 C 0.1868(5) 0.9571(5) 0.1673(2) 0.0287(16) Uani 1 1 d . . . H47A H 0.2380 0.9302 0.1814 0.034 Uiso 1 1 calc R . . C48 C -0.0459(5) 1.0781(5) 0.1838(2) 0.0305(16) Uani 1 1 d . . . C49 C -0.1941(5) 1.1558(5) 0.1929(2) 0.0361(18) Uani 1 1 d . . . C50 C -0.1451(5) 1.1303(5) 0.2309(2) 0.0358(18) Uani 1 1 d . . . C51 C -0.1392(6) 1.2083(6) 0.2592(2) 0.045(2) Uani 1 1 d . . . H51A H -0.1079 1.1857 0.2819 0.068 Uiso 1 1 calc R . . H51B H -0.2036 1.2294 0.2638 0.068 Uiso 1 1 calc R . . H51C H -0.1023 1.2593 0.2500 0.068 Uiso 1 1 calc R . . C52 C -0.1857(6) 1.0402(6) 0.2474(2) 0.045(2) Uani 1 1 d . . . H52A H -0.1525 1.0278 0.2709 0.068 Uiso 1 1 calc R . . H52B H -0.1760 0.9889 0.2309 0.068 Uiso 1 1 calc R . . H52C H -0.2540 1.0477 0.2506 0.068 Uiso 1 1 calc R . . C53 C -0.3004(5) 1.1295(6) 0.1876(3) 0.046(2) Uani 1 1 d . . . H53A H -0.3249 1.1482 0.1634 0.069 Uiso 1 1 calc R . . H53B H -0.3365 1.1605 0.2059 0.069 Uiso 1 1 calc R . . H53C H -0.3073 1.0631 0.1902 0.069 Uiso 1 1 calc R . . C54 C -0.1787(6) 1.2577(5) 0.1816(2) 0.044(2) Uani 1 1 d . . . H54A H -0.2110 1.2688 0.1578 0.066 Uiso 1 1 calc R . . H54B H -0.1104 1.2697 0.1803 0.066 Uiso 1 1 calc R . . H54C H -0.2051 1.2985 0.1995 0.066 Uiso 1 1 calc R . . C55 C -0.2177(8) 1.2164(7) 0.0624(3) 0.079(3) Uani 1 1 d . . . H55A H -0.2316 1.1838 0.0395 0.119 Uiso 1 1 calc R . . H55B H -0.1541 1.1993 0.0724 0.119 Uiso 1 1 calc R . . H55C H -0.2199 1.2825 0.0580 0.119 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 0.02193(15) 0.02747(15) 0.02611(17) -0.00079(11) 0.00149(11) 0.00247(10) Pt2 0.01998(14) 0.02620(15) 0.02687(17) 0.00033(11) 0.00243(11) 0.00155(10) P1 0.0302(9) 0.0252(9) 0.0279(10) -0.0017(8) -0.0001(8) -0.0007(7) P2 0.0213(8) 0.0279(9) 0.0288(10) 0.0000(8) 0.0020(8) 0.0003(7) P3 0.0207(8) 0.0245(9) 0.0313(11) -0.0013(8) 0.0021(8) -0.0009(7) P4 0.0256(9) 0.0242(9) 0.0305(11) -0.0002(8) 0.0036(8) -0.0023(7) P5 0.0456(12) 0.0628(15) 0.0411(14) 0.0044(11) 0.0053(11) -0.0143(11) P6 0.0345(14) 0.0474(17) 0.0359(17) 0.0070(14) 0.0041(13) -0.0023(12) P7 0.0390(15) 0.0471(17) 0.0391(18) -0.0111(14) 0.0082(14) -0.0042(13) F1 0.167(8) 0.283(14) 0.104(7) 0.057(8) 0.091(7) 0.118(9) F2 0.202(10) 0.275(12) 0.133(8) 0.118(9) -0.113(8) -0.193(10) F3 0.065(4) 0.134(6) 0.100(5) 0.058(5) -0.029(4) -0.033(4) F4 0.247(11) 0.085(5) 0.142(8) -0.017(5) 0.107(8) 0.012(6) F5 0.145(7) 0.117(6) 0.114(6) 0.003(5) 0.004(5) -0.080(5) F6 0.106(5) 0.147(7) 0.101(6) 0.078(5) 0.023(5) 0.022(5) F7 0.039(3) 0.140(5) 0.041(3) 0.012(3) -0.002(2) -0.009(3) F8 0.057(4) 0.154(7) 0.205(9) 0.131(7) 0.035(5) 0.015(4) F9 0.080(5) 0.186(8) 0.133(7) -0.101(7) -0.002(5) 0.021(5) F10 0.044(3) 0.097(5) 0.117(5) -0.055(4) 0.005(3) -0.004(3) F11 0.055(3) 0.061(3) 0.047(3) -0.021(2) 0.011(2) -0.005(2) F12 0.159(6) 0.058(3) 0.051(4) -0.004(3) 0.018(4) -0.013(4) O1 0.040(3) 0.045(3) 0.027(3) 0.009(2) 0.004(2) 0.003(2) O2 0.045(3) 0.057(4) 0.038(3) 0.007(3) 0.009(3) 0.017(3) O3 0.033(3) 0.055(3) 0.038(3) -0.008(3) 0.001(3) 0.003(2) O4 0.035(3) 0.058(4) 0.036(3) -0.009(3) -0.001(2) 0.008(3) O5 0.099(6) 0.093(6) 0.064(5) 0.014(4) 0.010(4) 0.039(5) N1 0.028(3) 0.033(3) 0.032(4) 0.003(3) 0.000(3) 0.000(3) N2 0.035(3) 0.036(3) 0.036(4) -0.004(3) 0.001(3) 0.008(3) N3 0.027(3) 0.030(3) 0.029(4) -0.002(3) 0.004(3) 0.002(2) N4 0.030(3) 0.039(3) 0.029(4) -0.007(3) 0.001(3) 0.004(3) N5 0.027(3) 0.036(3) 0.032(4) -0.009(3) 0.008(3) 0.000(3) N6 0.028(3) 0.021(3) 0.033(4) -0.001(3) 0.003(3) -0.001(2) C1 0.023(3) 0.031(4) 0.026(4) 0.001(3) 0.002(3) 0.000(3) C2 0.017(3) 0.026(3) 0.028(4) -0.001(3) 0.001(3) -0.001(3) C3 0.024(3) 0.023(3) 0.032(4) -0.002(3) 0.008(3) -0.003(3) C4 0.026(3) 0.030(4) 0.023(4) 0.001(3) 0.003(3) 0.000(3) C5 0.024(3) 0.041(4) 0.026(4) 0.002(3) 0.002(3) -0.008(3) C6 0.023(3) 0.031(4) 0.036(4) -0.005(3) 0.007(3) 0.002(3) C7 0.041(4) 0.037(4) 0.034(5) 0.005(3) -0.003(4) -0.005(3) C8 0.041(4) 0.063(5) 0.037(5) 0.008(4) 0.007(4) -0.004(4) C9 0.043(4) 0.032(4) 0.048(5) -0.005(4) 0.006(4) 0.001(3) C10 0.072(6) 0.046(5) 0.045(6) -0.013(4) 0.002(5) 0.002(4) C11 0.036(4) 0.043(4) 0.039(5) 0.003(4) -0.002(4) -0.004(3) C12 0.039(4) 0.056(5) 0.042(5) -0.004(4) 0.002(4) -0.017(4) C13 0.030(4) 0.031(4) 0.040(5) 0.001(3) -0.002(3) -0.002(3) C14 0.044(4) 0.043(4) 0.033(5) -0.009(4) -0.003(4) 0.007(4) C15 0.021(3) 0.038(4) 0.051(5) 0.005(4) 0.012(3) 0.003(3) C16 0.054(5) 0.066(6) 0.034(5) -0.004(4) 0.009(4) 0.014(4) C17 0.032(4) 0.036(4) 0.024(4) 0.000(3) 0.001(3) 0.008(3) C18 0.045(5) 0.033(4) 0.062(6) 0.010(4) -0.004(4) -0.003(4) C19 0.028(4) 0.035(4) 0.031(4) 0.002(3) 0.001(3) 0.005(3) C20 0.047(4) 0.036(4) 0.038(5) -0.003(4) 0.002(4) -0.002(3) C21 0.039(4) 0.034(4) 0.032(4) -0.004(3) 0.003(3) -0.003(3) C22 0.043(4) 0.050(5) 0.037(5) 0.003(4) -0.001(4) -0.007(4) C23 0.027(4) 0.035(4) 0.043(5) 0.000(3) 0.001(3) 0.000(3) C24 0.025(4) 0.043(4) 0.051(5) 0.002(4) 0.011(4) 0.003(3) C25 0.028(4) 0.028(4) 0.034(4) -0.002(3) 0.009(3) 0.002(3) C26 0.042(5) 0.059(5) 0.047(6) 0.004(4) 0.000(4) -0.009(4) C27 0.043(4) 0.037(4) 0.034(5) 0.004(3) 0.004(4) -0.014(3) C28 0.075(6) 0.067(6) 0.046(6) 0.022(5) -0.012(5) -0.016(5) C29 0.038(4) 0.030(4) 0.055(6) -0.003(4) 0.006(4) 0.003(3) C30 0.051(5) 0.034(4) 0.067(6) -0.008(4) 0.019(5) -0.002(4) C31 0.027(3) 0.026(4) 0.033(4) -0.002(3) 0.002(3) 0.000(3) C32 0.032(4) 0.031(4) 0.032(4) 0.002(3) 0.003(3) 0.000(3) C33 0.024(3) 0.028(4) 0.026(4) 0.001(3) 0.007(3) 0.000(3) C34 0.034(4) 0.033(4) 0.022(4) 0.001(3) 0.003(3) -0.001(3) C35 0.026(3) 0.033(4) 0.032(4) 0.003(3) 0.009(3) 0.006(3) C36 0.033(4) 0.031(4) 0.024(4) -0.002(3) 0.001(3) -0.005(3) C37 0.031(4) 0.038(4) 0.040(5) 0.007(3) 0.000(3) 0.006(3) C38 0.033(4) 0.039(4) 0.038(5) 0.005(4) -0.005(3) 0.004(3) C39 0.046(5) 0.046(5) 0.034(5) 0.006(4) -0.010(4) 0.003(4) C40 0.034(4) 0.051(5) 0.051(6) -0.009(4) -0.013(4) 0.002(4) C41 0.049(5) 0.042(5) 0.045(5) -0.001(4) 0.000(4) 0.019(4) C42 0.027(4) 0.058(5) 0.056(6) 0.010(4) 0.003(4) 0.012(4) C43 0.031(4) 0.034(4) 0.025(4) 0.001(3) 0.000(3) 0.005(3) C44 0.032(4) 0.036(4) 0.025(4) 0.001(3) 0.002(3) 0.007(3) C45 0.027(3) 0.030(4) 0.032(4) -0.003(3) 0.002(3) -0.002(3) C46 0.027(4) 0.035(4) 0.024(4) 0.001(3) 0.000(3) 0.003(3) C47 0.025(3) 0.033(4) 0.028(4) 0.004(3) 0.005(3) 0.000(3) C48 0.030(4) 0.035(4) 0.028(4) -0.002(3) 0.005(3) 0.001(3) C49 0.031(4) 0.038(4) 0.040(5) -0.018(4) 0.005(3) 0.002(3) C50 0.030(4) 0.045(4) 0.033(5) -0.006(3) 0.011(3) -0.002(3) C51 0.050(5) 0.049(5) 0.037(5) -0.014(4) 0.009(4) 0.000(4) C52 0.046(5) 0.053(5) 0.037(5) -0.002(4) 0.014(4) -0.010(4) C53 0.028(4) 0.061(5) 0.049(5) -0.014(4) 0.005(4) 0.001(4) C54 0.044(4) 0.044(5) 0.044(5) -0.008(4) -0.001(4) 0.008(4) C55 0.095(8) 0.070(7) 0.078(8) 0.023(6) 0.040(7) 0.030(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.023(6) . ? Pt1 N3 2.134(5) . ? Pt1 P1 2.3081(18) . ? Pt1 P2 2.3203(18) . ? Pt2 C3 2.028(7) . ? Pt2 N6 2.127(5) . ? Pt2 P4 2.3019(17) . ? Pt2 P3 2.3065(17) . ? P1 C11 1.823(7) . ? P1 C7 1.825(8) . ? P1 C9 1.838(8) . ? P2 C13 1.815(7) . ? P2 C17 1.821(7) . ? P2 C15 1.827(7) . ? P3 C21 1.810(7) . ? P3 C19 1.827(7) . ? P3 C23 1.829(7) . ? P4 C29 1.820(7) . ? P4 C27 1.821(8) . ? P4 C25 1.829(7) . ? P5 F2 1.521(7) . ? P5 F1 1.524(8) . ? P5 F6 1.539(7) . ? P5 F4 1.546(8) . ? P5 F5 1.564(7) . ? P5 F3 1.577(6) . ? P6 F8 1.540(6) 3_575 ? P6 F8 1.540(6) . ? P6 F9 1.546(7) . ? P6 F9 1.546(7) 3_575 ? P6 F7 1.584(5) 3_575 ? P6 F7 1.584(5) . ? P7 F12 1.578(6) 3_765 ? P7 F12 1.578(6) . ? P7 F10 1.579(5) . ? P7 F10 1.579(5) 3_765 ? P7 F11 1.600(4) 3_765 ? P7 F11 1.600(4) . ? O1 N1 1.281(7) . ? O2 N2 1.287(8) . ? O3 N5 1.280(8) . ? O4 N4 1.272(8) . ? O5 C55 1.444(12) . ? N1 C36 1.351(9) . ? N1 C38 1.516(9) . ? N2 C36 1.342(9) . ? N2 C37 1.496(9) . ? N3 C35 1.346(9) . ? N3 C31 1.353(9) . ? N4 C48 1.342(9) . ? N4 C49 1.510(9) . ? N5 C48 1.358(9) . ? N5 C50 1.512(9) . ? N6 C47 1.335(9) . ? N6 C43 1.350(8) . ? C1 C6 1.392(10) . ? C1 C2 1.415(9) . ? C2 C3 1.415(9) . ? C3 C4 1.393(10) . ? C4 C5 1.382(10) . ? C5 C6 1.386(9) . ? C7 C8 1.524(11) . ? C9 C10 1.527(12) . ? C11 C12 1.517(10) . ? C13 C14 1.515(10) . ? C15 C16 1.514(11) . ? C17 C18 1.505(10) . ? C19 C20 1.533(10) . ? C21 C22 1.539(10) . ? C23 C24 1.516(10) . ? C25 C26 1.520(11) . ? C27 C28 1.524(11) . ? C29 C30 1.531(10) . ? C31 C32 1.391(9) . ? C32 C33 1.389(10) . ? C33 C34 1.395(9) . ? C33 C36 1.460(9) . ? C34 C35 1.368(9) . ? C37 C42 1.519(10) . ? C37 C41 1.524(10) . ? C37 C38 1.546(11) . ? C38 C39 1.513(10) . ? C38 C40 1.529(10) . ? C43 C44 1.393(10) . ? C44 C45 1.385(10) . ? C45 C46 1.405(9) . ? C45 C48 1.463(10) . ? C46 C47 1.357(9) . ? C49 C53 1.513(10) . ? C49 C54 1.534(11) . ? C49 C50 1.541(11) . ? C50 C51 1.514(10) . ? C50 C52 1.539(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 C1 Pt1 N3 178.6(2) . . ? C1 Pt1 P1 92.06(19) . . ? N3 Pt1 P1 89.30(16) . . ? C1 Pt1 P2 88.37(19) . . ? N3 Pt1 P2 90.31(16) . . ? P1 Pt1 P2 174.56(7) . . ? C3 Pt2 N6 175.7(2) . . ? C3 Pt2 P4 88.61(18) . . ? N6 Pt2 P4 93.72(15) . . ? C3 Pt2 P3 86.59(18) . . ? N6 Pt2 P3 91.50(15) . . ? P4 Pt2 P3 171.91(6) . . ? C11 P1 C7 105.8(4) . . ? C11 P1 C9 105.3(4) . . ? C7 P1 C9 103.0(4) . . ? C11 P1 Pt1 116.4(3) . . ? C7 P1 Pt1 114.5(3) . . ? C9 P1 Pt1 110.7(3) . . ? C13 P2 C17 105.7(3) . . ? C13 P2 C15 104.8(3) . . ? C17 P2 C15 104.3(3) . . ? C13 P2 Pt1 114.8(3) . . ? C17 P2 Pt1 116.2(2) . . ? C15 P2 Pt1 109.9(3) . . ? C21 P3 C19 103.9(3) . . ? C21 P3 C23 105.8(4) . . ? C19 P3 C23 104.4(3) . . ? C21 P3 Pt2 116.3(3) . . ? C19 P3 Pt2 110.4(2) . . ? C23 P3 Pt2 114.8(2) . . ? C29 P4 C27 105.5(4) . . ? C29 P4 C25 104.7(4) . . ? C27 P4 C25 104.3(3) . . ? C29 P4 Pt2 116.2(3) . . ? C27 P4 Pt2 115.3(3) . . ? C25 P4 Pt2 109.7(2) . . ? F2 P5 F1 90.0(7) . . ? F2 P5 F6 91.6(5) . . ? F1 P5 F6 91.8(5) . . ? F2 P5 F4 92.9(7) . . ? F1 P5 F4 177.1(7) . . ? F6 P5 F4 87.7(5) . . ? F2 P5 F5 177.6(7) . . ? F1 P5 F5 91.7(6) . . ? F6 P5 F5 90.0(5) . . ? F4 P5 F5 85.4(5) . . ? F2 P5 F3 89.5(4) . . ? F1 P5 F3 87.9(5) . . ? F6 P5 F3 178.9(5) . . ? F4 P5 F3 92.5(5) . . ? F5 P5 F3 88.9(4) . . ? F8 P6 F8 180.0(5) 3_575 . ? F8 P6 F9 92.4(6) 3_575 . ? F8 P6 F9 87.6(6) . . ? F8 P6 F9 87.6(6) 3_575 3_575 ? F8 P6 F9 92.4(6) . 3_575 ? F9 P6 F9 180.0(5) . 3_575 ? F8 P6 F7 88.7(3) 3_575 3_575 ? F8 P6 F7 91.3(3) . 3_575 ? F9 P6 F7 88.1(3) . 3_575 ? F9 P6 F7 91.9(3) 3_575 3_575 ? F8 P6 F7 91.3(3) 3_575 . ? F8 P6 F7 88.7(3) . . ? F9 P6 F7 92.0(3) . . ? F9 P6 F7 88.0(3) 3_575 . ? F7 P6 F7 180.0(4) 3_575 . ? F12 P7 F12 180.0(4) 3_765 . ? F12 P7 F10 89.4(4) 3_765 . ? F12 P7 F10 90.6(4) . . ? F12 P7 F10 90.6(4) 3_765 3_765 ? F12 P7 F10 89.4(4) . 3_765 ? F10 P7 F10 180.0 . 3_765 ? F12 P7 F11 90.5(3) 3_765 3_765 ? F12 P7 F11 89.5(3) . 3_765 ? F10 P7 F11 89.5(3) . 3_765 ? F10 P7 F11 90.5(3) 3_765 3_765 ? F12 P7 F11 89.5(3) 3_765 . ? F12 P7 F11 90.5(3) . . ? F10 P7 F11 90.5(3) . . ? F10 P7 F11 89.5(3) 3_765 . ? F11 P7 F11 180.0(3) 3_765 . ? O1 N1 C36 127.7(6) . . ? O1 N1 C38 121.0(6) . . ? C36 N1 C38 110.9(6) . . ? O2 N2 C36 126.7(6) . . ? O2 N2 C37 121.2(6) . . ? C36 N2 C37 112.0(6) . . ? C35 N3 C31 117.7(6) . . ? C35 N3 Pt1 120.1(4) . . ? C31 N3 Pt1 122.2(5) . . ? O4 N4 C48 126.6(6) . . ? O4 N4 C49 121.5(5) . . ? C48 N4 C49 111.8(6) . . ? O3 N5 C48 127.0(6) . . ? O3 N5 C50 121.8(6) . . ? C48 N5 C50 111.0(6) . . ? C47 N6 C43 116.7(6) . . ? C47 N6 Pt2 123.4(4) . . ? C43 N6 Pt2 119.7(5) . . ? C6 C1 C2 117.8(6) . . ? C6 C1 Pt1 120.3(5) . . ? C2 C1 Pt1 121.9(5) . . ? C3 C2 C1 122.2(6) . . ? C4 C3 C2 116.9(6) . . ? C4 C3 Pt2 119.4(5) . . ? C2 C3 Pt2 123.7(5) . . ? C5 C4 C3 122.0(6) . . ? C4 C5 C6 120.2(7) . . ? C5 C6 C1 121.0(7) . . ? C8 C7 P1 112.6(5) . . ? C10 C9 P1 111.2(5) . . ? C12 C11 P1 118.0(6) . . ? C14 C13 P2 114.2(5) . . ? C16 C15 P2 113.6(5) . . ? C18 C17 P2 116.4(5) . . ? C20 C19 P3 113.0(5) . . ? C22 C21 P3 112.9(5) . . ? C24 C23 P3 113.8(5) . . ? C26 C25 P4 113.8(5) . . ? C28 C27 P4 111.6(6) . . ? C30 C29 P4 114.9(5) . . ? N3 C31 C32 122.4(7) . . ? C33 C32 C31 118.9(7) . . ? C32 C33 C34 118.6(6) . . ? C32 C33 C36 121.1(6) . . ? C34 C33 C36 120.1(6) . . ? C35 C34 C33 119.0(7) . . ? N3 C35 C34 123.5(6) . . ? N2 C36 N1 108.4(6) . . ? N2 C36 C33 126.2(7) . . ? N1 C36 C33 125.1(6) . . ? N2 C37 C42 109.3(6) . . ? N2 C37 C41 107.7(6) . . ? C42 C37 C41 111.5(7) . . ? N2 C37 C38 100.3(6) . . ? C42 C37 C38 114.4(7) . . ? C41 C37 C38 112.9(6) . . ? C39 C38 N1 110.0(6) . . ? C39 C38 C40 110.1(7) . . ? N1 C38 C40 105.4(6) . . ? C39 C38 C37 115.7(6) . . ? N1 C38 C37 99.9(6) . . ? C40 C38 C37 114.8(7) . . ? N6 C43 C44 122.3(7) . . ? C45 C44 C43 119.8(6) . . ? C44 C45 C46 117.4(6) . . ? C44 C45 C48 122.1(6) . . ? C46 C45 C48 120.5(7) . . ? C47 C46 C45 118.7(7) . . ? N6 C47 C46 125.1(6) . . ? N4 C48 N5 108.5(6) . . ? N4 C48 C45 125.4(7) . . ? N5 C48 C45 126.2(6) . . ? N4 C49 C53 110.3(6) . . ? N4 C49 C54 106.0(6) . . ? C53 C49 C54 110.5(6) . . ? N4 C49 C50 100.2(5) . . ? C53 C49 C50 115.2(7) . . ? C54 C49 C50 113.8(6) . . ? N5 C50 C51 110.0(6) . . ? N5 C50 C52 105.1(6) . . ? C51 C50 C52 111.2(7) . . ? N5 C50 C49 100.4(6) . . ? C51 C50 C49 115.7(6) . . ? C52 C50 C49 113.2(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.974 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.166 data_compound_3 _database_code_CSD 171204 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H100 Cl4 F12 N6 O4 P6 Pt2' _chemical_formula_weight 1867.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.634(2) _cell_length_b 23.791(5) _cell_length_c 14.159(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.15(3) _cell_angle_gamma 90.00 _cell_volume 3745.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 4.077 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.069 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17035 _diffrn_reflns_av_R_equivalents 0.0988 _diffrn_reflns_av_sigmaI/netI 0.1509 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5285 _reflns_number_gt 3243 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+-1.00000exp(-12.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+5.0000*P+(0.0000P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _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 5285 _refine_ls_number_parameters 406 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1177 _refine_ls_R_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.1600 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.082 _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 0.45022(5) 0.857670(17) 0.01884(5) 0.0304(2) Uani 1 1 d . . . Cl1 Cl 0.9316(4) 0.3370(2) 0.9770(5) 0.0748(14) Uani 1 1 d . . . Cl2 Cl 1.0275(5) 0.3877(3) 0.8294(5) 0.0912(17) Uani 1 1 d . . . P1 P 0.6538(3) 0.85184(14) 0.0866(3) 0.0356(8) Uani 1 1 d . . . P2 P 0.2457(3) 0.87178(14) -0.0474(3) 0.0399(10) Uani 1 1 d . . . P3 P 0.1934(4) 0.80293(15) 0.3053(4) 0.0506(12) Uani 1 1 d . . . F1 F 0.2944(11) 0.7578(4) 0.3114(14) 0.116(6) Uani 1 1 d . . . F2 F 0.2798(12) 0.8499(4) 0.2897(13) 0.103(5) Uani 1 1 d . . . F3 F 0.1449(11) 0.7912(5) 0.1910(9) 0.093(4) Uani 1 1 d . . . F4 F 0.1067(9) 0.7553(4) 0.3219(8) 0.069(3) Uani 1 1 d . . . F5 F 0.2441(16) 0.8134(8) 0.4176(12) 0.133(6) Uani 1 1 d . . . F6 F 0.0891(15) 0.8460(4) 0.2943(19) 0.146(8) Uani 1 1 d . . . O1 O 0.3598(13) 0.5962(4) 0.2401(11) 0.072(4) Uani 1 1 d . . . O2 O 0.3517(10) 0.5629(4) -0.0851(9) 0.048(3) Uani 1 1 d . . . N1 N 0.3480(13) 0.5721(5) 0.1562(13) 0.059(4) Uani 1 1 d . . . N2 N 0.3420(11) 0.5567(4) 0.0016(12) 0.045(4) Uani 1 1 d . . . N3 N 0.4294(9) 0.7699(4) 0.0353(9) 0.033(3) Uani 1 1 d . . . C1 C 0.4748(11) 0.9410(5) 0.0067(10) 0.029(3) Uani 1 1 d . . . C2 C 0.4937(12) 0.9780(5) 0.0877(12) 0.037(3) Uani 1 1 d . . . H2A H 0.4893 0.9641 0.1479 0.045 Uiso 1 1 calc R . . C3 C 0.4818(12) 0.9668(5) -0.0804(12) 0.039(4) Uani 1 1 d . . . H3A H 0.4688 0.9446 -0.1366 0.047 Uiso 1 1 calc R . . C4 C 0.7065(12) 0.8750(7) 0.2195(10) 0.044(4) Uani 1 1 d DU . . H4A H 0.7905 0.8648 0.2472 0.052 Uiso 1 1 calc R . . H4B H 0.7007 0.9156 0.2221 0.052 Uiso 1 1 calc R . . C5 C 0.6342(17) 0.8489(7) 0.2829(12) 0.067(5) Uani 1 1 d DU . . H5A H 0.6639 0.8628 0.3493 0.100 Uiso 1 1 calc R . . H5B H 0.6424 0.8087 0.2830 0.100 Uiso 1 1 calc R . . H5C H 0.5509 0.8588 0.2560 0.100 Uiso 1 1 calc R . . C6 C 0.7141(10) 0.7784(6) 0.0896(16) 0.059(5) Uani 1 1 d DU . . H6A H 0.6762 0.7550 0.1280 0.070 Uiso 1 1 calc R . . H6B H 0.6912 0.7638 0.0227 0.070 Uiso 1 1 calc R . . C7 C 0.8512(12) 0.7733(10) 0.133(2) 0.105(9) Uani 1 1 d DU . . H7A H 0.8743 0.7346 0.1337 0.158 Uiso 1 1 calc R . . H7B H 0.8751 0.7876 0.1998 0.158 Uiso 1 1 calc R . . H7C H 0.8899 0.7947 0.0939 0.158 Uiso 1 1 calc R . . C8 C 0.7460(16) 0.8947(9) 0.0330(11) 0.071(6) Uani 1 1 d DU . . H8A H 0.7257 0.9341 0.0355 0.086 Uiso 1 1 calc R . . H8B H 0.8305 0.8897 0.0685 0.086 Uiso 1 1 calc R . . C9 C 0.7200(17) 0.8752(8) -0.0738(12) 0.081(8) Uani 1 1 d DU . . H9A H 0.7672 0.8968 -0.1060 0.122 Uiso 1 1 calc R . . H9B H 0.6361 0.8803 -0.1078 0.122 Uiso 1 1 calc R . . H9C H 0.7403 0.8362 -0.0749 0.122 Uiso 1 1 calc R . . C10 C 0.2016(16) 0.8883(9) -0.178(2) 0.099(9) Uani 1 1 d DU . . H10A H 0.1163 0.8969 -0.1988 0.119 Uiso 1 1 calc R . . H10B H 0.2443 0.9218 -0.1872 0.119 Uiso 1 1 calc R . . C11 C 0.226(3) 0.8414(15) -0.2436(16) 0.139(13) Uani 1 1 d DU . . H11A H 0.1996 0.8533 -0.3114 0.209 Uiso 1 1 calc R . . H11B H 0.1826 0.8082 -0.2359 0.209 Uiso 1 1 calc R . . H11C H 0.3105 0.8334 -0.2248 0.209 Uiso 1 1 calc R . . C12 C 0.1564(10) 0.8109(7) -0.0375(15) 0.056(4) Uani 1 1 d DU . . H12A H 0.1769 0.7807 -0.0756 0.067 Uiso 1 1 calc R . . H12B H 0.1803 0.7990 0.0311 0.067 Uiso 1 1 calc R . . C13 C 0.0190(11) 0.8178(9) -0.0714(17) 0.077(6) Uani 1 1 d DU . . H13A H -0.0180 0.7830 -0.0622 0.115 Uiso 1 1 calc R . . H13B H -0.0071 0.8279 -0.1401 0.115 Uiso 1 1 calc R . . H13C H -0.0036 0.8467 -0.0332 0.115 Uiso 1 1 calc R . . C14 C 0.187(3) 0.9379(14) -0.028(3) 0.165(17) Uani 1 1 d DU . . H14A H 0.2375 0.9685 -0.0383 0.198 Uiso 1 1 calc R . . H14B H 0.1058 0.9431 -0.0700 0.198 Uiso 1 1 calc R . . C15 C 0.192(2) 0.9328(17) 0.081(3) 0.18(2) Uani 1 1 d DU . . H15A H 0.1595 0.9662 0.1011 0.263 Uiso 1 1 calc R . . H15B H 0.2743 0.9283 0.1208 0.263 Uiso 1 1 calc R . . H15C H 0.1462 0.9008 0.0896 0.263 Uiso 1 1 calc R . . C16 C 0.3980(12) 0.7518(6) 0.1162(12) 0.044(4) Uani 1 1 d . . . H16A H 0.3874 0.7780 0.1617 0.053 Uiso 1 1 calc R . . C17 C 0.3816(11) 0.6950(5) 0.1318(12) 0.036(3) Uani 1 1 d . . . H17A H 0.3650 0.6832 0.1890 0.043 Uiso 1 1 calc R . . C18 C 0.3901(10) 0.6563(5) 0.0617(11) 0.031(3) Uani 1 1 d . . . C19 C 0.4234(12) 0.6752(5) -0.0199(12) 0.039(3) Uani 1 1 d . . . H19A H 0.4339 0.6499 -0.0668 0.046 Uiso 1 1 calc R . . C20 C 0.4402(11) 0.7313(5) -0.0295(12) 0.037(3) Uani 1 1 d . . . H20A H 0.4606 0.7434 -0.0849 0.044 Uiso 1 1 calc R . . C21 C 0.3651(12) 0.5961(5) 0.0733(12) 0.036(3) Uani 1 1 d . . . C22 C 0.3268(18) 0.5113(6) 0.1433(17) 0.064(5) Uani 1 1 d . . . C23 C 0.2882(15) 0.5041(5) 0.0308(19) 0.068(6) Uani 1 1 d . . . C24 C 0.3386(13) 0.4530(5) -0.0054(16) 0.056(5) Uani 1 1 d . . . H24A H 0.3110 0.4519 -0.0763 0.084 Uiso 1 1 calc R . . H24B H 0.3120 0.4198 0.0206 0.084 Uiso 1 1 calc R . . H24C H 0.4248 0.4546 0.0165 0.084 Uiso 1 1 calc R . . C25 C 0.1521(15) 0.5096(6) -0.019(2) 0.103(10) Uani 1 1 d . . . H25A H 0.1223 0.5423 0.0054 0.154 Uiso 1 1 calc R . . H25B H 0.1119 0.4768 -0.0053 0.154 Uiso 1 1 calc R . . H25C H 0.1371 0.5131 -0.0895 0.154 Uiso 1 1 calc R . . C26 C 0.4469(19) 0.4831(6) 0.1967(17) 0.076(6) Uani 1 1 d . . . H26A H 0.4644 0.4887 0.2666 0.114 Uiso 1 1 calc R . . H26B H 0.5097 0.4994 0.1743 0.114 Uiso 1 1 calc R . . H26C H 0.4417 0.4436 0.1825 0.114 Uiso 1 1 calc R . . C27 C 0.229(3) 0.4940(7) 0.194(2) 0.113(10) Uani 1 1 d . . . H27A H 0.1538 0.5115 0.1595 0.169 Uiso 1 1 calc R . . H27B H 0.2535 0.5060 0.2614 0.169 Uiso 1 1 calc R . . H27C H 0.2194 0.4539 0.1909 0.169 Uiso 1 1 calc R . . C28 C 0.9191(19) 0.3439(8) 0.8460(17) 0.081(7) Uani 1 1 d . . . H28A H 0.9272 0.3072 0.8189 0.097 Uiso 1 1 calc R . . H28B H 0.8404 0.3586 0.8109 0.097 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 0.0346(3) 0.0181(2) 0.0410(3) -0.0019(3) 0.0151(2) -0.0030(2) Cl1 0.064(2) 0.068(2) 0.089(4) 0.005(3) 0.017(3) 0.010(2) Cl2 0.092(3) 0.097(4) 0.077(4) 0.006(3) 0.014(3) -0.031(3) P1 0.0319(16) 0.0369(17) 0.036(2) -0.0018(17) 0.0063(18) -0.0062(15) P2 0.0325(16) 0.0324(17) 0.053(3) 0.0008(18) 0.010(2) 0.0017(14) P3 0.060(2) 0.0299(17) 0.066(3) -0.007(2) 0.025(3) -0.0019(17) F1 0.102(8) 0.053(6) 0.205(17) 0.032(9) 0.063(11) 0.026(6) F2 0.112(8) 0.047(5) 0.132(12) 0.023(7) 0.008(10) -0.034(6) F3 0.106(9) 0.112(9) 0.068(8) 0.007(7) 0.035(8) -0.041(7) F4 0.079(6) 0.066(5) 0.086(8) -0.003(6) 0.063(6) -0.008(5) F5 0.145(13) 0.160(13) 0.093(11) -0.049(10) 0.032(11) -0.063(11) F6 0.144(12) 0.050(6) 0.24(2) -0.021(10) 0.054(15) 0.029(7) O1 0.127(11) 0.031(5) 0.090(9) -0.005(6) 0.081(9) -0.004(6) O2 0.066(6) 0.026(5) 0.046(7) -0.001(5) 0.006(7) 0.012(4) N1 0.081(9) 0.031(6) 0.093(12) 0.014(8) 0.067(10) 0.020(6) N2 0.041(6) 0.025(5) 0.058(10) -0.004(6) -0.004(8) -0.004(5) N3 0.031(5) 0.039(6) 0.032(7) -0.007(6) 0.014(5) -0.003(5) C1 0.033(6) 0.030(6) 0.028(8) -0.007(6) 0.015(6) 0.001(5) C2 0.046(7) 0.030(6) 0.042(9) -0.001(6) 0.023(8) 0.003(6) C3 0.050(8) 0.023(6) 0.050(10) -0.016(7) 0.025(8) -0.008(6) C4 0.038(7) 0.062(9) 0.025(8) -0.010(7) 0.001(7) -0.006(7) C5 0.093(13) 0.066(11) 0.032(10) 0.012(8) 0.004(11) -0.010(10) C6 0.043(7) 0.042(7) 0.090(14) 0.003(9) 0.020(9) -0.001(7) C7 0.071(12) 0.111(17) 0.11(2) 0.000(16) -0.009(15) 0.028(13) C8 0.054(9) 0.092(13) 0.053(12) -0.015(11) -0.009(10) -0.022(9) C9 0.069(11) 0.073(11) 0.070(13) -0.026(11) -0.029(11) 0.062(10) C10 0.041(9) 0.100(15) 0.14(2) 0.070(15) -0.006(13) -0.026(10) C11 0.108(19) 0.28(4) 0.034(13) 0.024(18) 0.034(15) 0.03(2) C12 0.047(8) 0.059(9) 0.064(12) 0.007(9) 0.021(9) -0.021(7) C13 0.050(9) 0.098(14) 0.074(14) 0.034(12) 0.004(10) -0.021(9) C14 0.072(15) 0.13(3) 0.28(4) -0.12(3) 0.03(3) 0.000(16) C15 0.047(12) 0.18(3) 0.29(5) 0.12(4) 0.04(3) 0.033(16) C16 0.048(8) 0.034(7) 0.045(10) -0.010(7) 0.004(8) -0.009(6) C17 0.041(7) 0.024(6) 0.047(10) 0.006(6) 0.018(8) 0.004(5) C18 0.026(6) 0.023(6) 0.041(9) -0.002(6) 0.007(7) 0.002(5) C19 0.047(7) 0.028(6) 0.048(9) 0.005(7) 0.024(8) 0.010(6) C20 0.043(7) 0.017(5) 0.057(9) 0.000(6) 0.026(8) -0.006(5) C21 0.039(7) 0.022(6) 0.055(10) 0.008(7) 0.025(8) 0.000(5) C22 0.096(13) 0.020(6) 0.108(17) 0.001(9) 0.079(14) 0.013(8) C23 0.060(9) 0.012(6) 0.14(2) -0.004(9) 0.040(13) -0.004(6) C24 0.056(8) 0.024(6) 0.107(15) -0.005(8) 0.052(11) 0.006(6) C25 0.062(10) 0.030(8) 0.22(3) 0.010(13) 0.044(16) -0.018(8) C26 0.123(15) 0.022(6) 0.096(16) 0.014(9) 0.053(15) 0.020(9) C27 0.19(2) 0.024(7) 0.18(3) -0.004(12) 0.14(2) -0.019(11) C28 0.077(12) 0.078(12) 0.070(15) -0.025(11) -0.003(13) 0.020(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 C1 2.017(12) . ? Pt1 N3 2.122(11) . ? Pt1 P1 2.282(3) . ? Pt1 P2 2.310(4) . ? Cl1 C28 1.82(3) . ? Cl2 C28 1.71(3) . ? P1 C8 1.80(2) . ? P1 C6 1.878(15) . ? P1 C4 1.881(14) . ? P2 C14 1.77(3) . ? P2 C10 1.80(3) . ? P2 C12 1.812(14) . ? P3 F5 1.543(17) . ? P3 F6 1.561(14) . ? P3 F2 1.562(12) . ? P3 F3 1.574(13) . ? P3 F1 1.576(11) . ? P3 F4 1.579(10) . ? O1 N1 1.289(19) . ? O2 N2 1.274(18) . ? N1 C21 1.37(2) . ? N1 C22 1.471(19) . ? N2 C21 1.351(19) . ? N2 C23 1.51(2) . ? N3 C20 1.331(18) . ? N3 C16 1.37(2) . ? C1 C3 1.40(2) . ? C1 C2 1.410(19) . ? C2 C3 1.355(17) 3_675 ? C3 C2 1.355(17) 3_675 ? C4 C5 1.531(10) . ? C6 C7 1.536(10) . ? C8 C9 1.525(10) . ? C10 C11 1.534(10) . ? C12 C13 1.536(9) . ? C14 C15 1.530(10) . ? C16 C17 1.393(18) . ? C17 C18 1.38(2) . ? C18 C19 1.40(2) . ? C18 C21 1.479(16) . ? C19 C20 1.362(17) . ? C22 C23 1.53(3) . ? C22 C26 1.53(3) . ? C22 C27 1.57(3) . ? C23 C24 1.50(2) . ? C23 C25 1.54(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 N3 178.2(5) . . ? C1 Pt1 P1 86.6(4) . . ? N3 Pt1 P1 91.8(3) . . ? C1 Pt1 P2 88.7(4) . . ? N3 Pt1 P2 92.9(3) . . ? P1 Pt1 P2 175.09(12) . . ? C8 P1 C6 105.7(9) . . ? C8 P1 C4 101.3(6) . . ? C6 P1 C4 103.9(8) . . ? C8 P1 Pt1 117.5(6) . . ? C6 P1 Pt1 113.6(4) . . ? C4 P1 Pt1 113.2(5) . . ? C14 P2 C10 87.7(17) . . ? C14 P2 C12 116.4(14) . . ? C10 P2 C12 104.9(9) . . ? C14 P2 Pt1 117.5(10) . . ? C10 P2 Pt1 113.3(7) . . ? C12 P2 Pt1 113.4(5) . . ? F5 P3 F6 92.7(13) . . ? F5 P3 F2 88.0(9) . . ? F6 P3 F2 91.7(9) . . ? F5 P3 F3 178.4(10) . . ? F6 P3 F3 88.9(11) . . ? F2 P3 F3 91.8(8) . . ? F5 P3 F1 90.0(10) . . ? F6 P3 F1 176.9(10) . . ? F2 P3 F1 89.7(7) . . ? F3 P3 F1 88.3(9) . . ? F5 P3 F4 91.7(8) . . ? F6 P3 F4 88.5(8) . . ? F2 P3 F4 179.6(8) . . ? F3 P3 F4 88.5(6) . . ? F1 P3 F4 90.1(6) . . ? O1 N1 C21 126.9(12) . . ? O1 N1 C22 121.4(14) . . ? C21 N1 C22 111.4(15) . . ? O2 N2 C21 126.1(12) . . ? O2 N2 C23 121.4(13) . . ? C21 N2 C23 112.1(16) . . ? C20 N3 C16 117.5(12) . . ? C20 N3 Pt1 124.5(10) . . ? C16 N3 Pt1 117.9(9) . . ? C3 C1 C2 113.9(11) . . ? C3 C1 Pt1 123.5(9) . . ? C2 C1 Pt1 122.4(10) . . ? C3 C2 C1 122.0(15) 3_675 . ? C2 C3 C1 124.1(14) 3_675 . ? C5 C4 P1 113.2(10) . . ? C7 C6 P1 114.8(12) . . ? C9 C8 P1 106.1(13) . . ? C11 C10 P2 114.6(14) . . ? C13 C12 P2 117.2(11) . . ? C15 C14 P2 101(3) . . ? N3 C16 C17 121.3(14) . . ? C18 C17 C16 119.5(15) . . ? C17 C18 C19 118.5(11) . . ? C17 C18 C21 120.5(14) . . ? C19 C18 C21 121.0(13) . . ? C20 C19 C18 118.7(14) . . ? N3 C20 C19 124.3(15) . . ? N2 C21 N1 107.9(12) . . ? N2 C21 C18 126.2(14) . . ? N1 C21 C18 125.5(14) . . ? N1 C22 C23 103.0(14) . . ? N1 C22 C26 105.9(15) . . ? C23 C22 C26 114.1(15) . . ? N1 C22 C27 108.7(13) . . ? C23 C22 C27 114.5(19) . . ? C26 C22 C27 109.9(17) . . ? C24 C23 N2 110.0(16) . . ? C24 C23 C22 114.9(15) . . ? N2 C23 C22 100.1(13) . . ? C24 C23 C25 111.3(15) . . ? N2 C23 C25 104.9(13) . . ? C22 C23 C25 115(2) . . ? Cl2 C28 Cl1 110.8(11) . . ? _diffrn_measured_fraction_theta_max 0.803 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.803 _refine_diff_density_max 3.490 _refine_diff_density_min -1.261 _refine_diff_density_rms 0.203