# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'M Schroder' 'Alexander Blake' 'E Stephen Davies' 'Jonathan McMaster' 'Emma Stephen' _publ_contact_author_name 'M Schroder' _publ_contact_author_email M.SCHRODER@NOTTINGHAM.AC.UK _publ_section_title ; The Structural Characterisation and Elucidation of the Electronic Structure of the Mononuclear Pt(III) Complex [Pt([9]aneS3)2]3+ ([9]aneS3 = 1,4,7-trithiacyclononane) ; # Attachment 'PT9S3P1.CIF' data_pt9s3p _database_code_depnum_ccdc_archive 'CCDC 694378' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Pt S6 2+, 2(P F6 -), 2(C2 H3 N)' _chemical_formula_sum 'C16 H30 F12 N2 P2 Pt S6' _chemical_formula_weight 927.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 11.9244(8) _cell_length_b 21.6165(14) _cell_length_c 11.3781(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2932.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11102 _cell_measurement_theta_min 4.9 _cell_measurement_theta_max 55 _exptl_crystal_description Block _exptl_crystal_colour Red/Orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 5.411 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.414 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details '(SADABS version 2.05; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25895 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_av_sigmaI/netI 0.015 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3371 _reflns_number_gt 2884 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.014P)^2^+23.57P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00135(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3371 _refine_ls_number_parameters 182 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.13 _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 Pt Pt 0.5000 1.0000 0.5000 0.01079(8) Uani 1 2 d SU . . S1 S 0.33067(9) 0.98574(5) 0.30010(10) 0.0197(2) Uani 1 1 d U . . C2 C 0.2444(4) 0.9438(2) 0.4052(4) 0.0196(8) Uani 1 1 d U . . H2A H 0.2101 0.9748 0.4584 0.024 Uiso 1 1 calc R . . H2B H 0.1824 0.9243 0.3608 0.024 Uiso 1 1 calc R . . C3 C 0.2973(4) 0.89407(19) 0.4816(4) 0.0179(8) Uani 1 1 d U . . H3A H 0.3317 0.8627 0.4294 0.021 Uiso 1 1 calc R . . H3B H 0.2368 0.8733 0.5262 0.021 Uiso 1 1 calc R . . S4 S 0.40377(8) 0.92013(4) 0.58600(9) 0.0138(2) Uani 1 1 d U . . C5 C 0.5070(4) 0.8590(2) 0.5712(4) 0.0205(9) Uani 1 1 d U . . H5A H 0.5689 0.8667 0.6273 0.025 Uiso 1 1 calc R . . H5B H 0.4717 0.8191 0.5927 0.025 Uiso 1 1 calc R . . C6 C 0.5554(4) 0.85357(19) 0.4486(4) 0.0195(8) Uani 1 1 d U . . H6A H 0.4980 0.8362 0.3951 0.023 Uiso 1 1 calc R . . H6B H 0.6200 0.8248 0.4498 0.023 Uiso 1 1 calc R . . S7 S 0.60128(8) 0.92904(5) 0.39320(9) 0.0150(2) Uani 1 1 d U . . C8 C 0.5423(4) 0.9320(2) 0.2460(4) 0.0193(8) Uani 1 1 d U . . H8A H 0.5659 0.9717 0.2103 0.023 Uiso 1 1 calc R . . H8B H 0.5779 0.8986 0.1997 0.023 Uiso 1 1 calc R . . C9 C 0.4154(4) 0.9263(2) 0.2296(4) 0.0221(9) Uani 1 1 d U . . H9A H 0.3915 0.8855 0.2602 0.027 Uiso 1 1 calc R . . H9B H 0.3990 0.9269 0.1444 0.027 Uiso 1 1 calc R . . P1 P 0.2500 0.7500 0.23806(13) 0.0142(3) Uani 1 2 d SDU . . F1 F 0.2955(2) 0.68030(11) 0.2391(3) 0.0266(6) Uani 1 1 d DU . . F2 F 0.1635(5) 0.7329(2) 0.1411(5) 0.111(2) Uani 1 1 d DU . . F3 F 0.1625(5) 0.73260(18) 0.3334(5) 0.111(2) Uani 1 1 d DU . . P2 P 0.7500 0.7500 0.20780(15) 0.0225(3) Uani 1 2 d SDU . . F4 F 0.6168(2) 0.75650(16) 0.2076(3) 0.0352(7) Uani 1 1 d DU . . F5 F 0.7500 0.7500 0.3413(5) 0.176(4) Uani 1 2 d SDU . . F6 F 0.7603(4) 0.82001(19) 0.2084(11) 0.183(3) Uani 1 1 d DU . . F7 F 0.7500 0.7500 0.0745(5) 0.187(5) Uani 1 2 d SDU . . C1S C 0.9745(5) 0.8235(2) 0.4497(5) 0.0334(11) Uani 1 1 d U . . H1S1 H 1.0344 0.8182 0.5077 0.050 Uiso 1 1 calc R . . H1S2 H 0.9975 0.8050 0.3748 0.050 Uiso 1 1 calc R . . H1S3 H 0.9061 0.8032 0.4778 0.050 Uiso 1 1 calc R . . C2S C 0.9530(4) 0.8892(2) 0.4328(5) 0.0297(11) Uani 1 1 d U . . N3S N 0.9373(6) 0.9404(3) 0.4216(6) 0.0590(17) Uani 1 1 d U . . 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 Pt 0.01067(12) 0.00993(12) 0.01177(12) -0.00054(7) 0.00050(8) -0.00185(7) S1 0.0171(5) 0.0203(5) 0.0216(5) 0.0036(4) -0.0043(4) -0.0012(4) C2 0.0116(18) 0.023(2) 0.024(2) 0.0004(17) -0.0016(16) -0.0022(16) C3 0.0151(19) 0.0163(19) 0.022(2) -0.0004(15) -0.0002(16) -0.0049(15) S4 0.0144(5) 0.0119(4) 0.0149(4) 0.0017(3) 0.0016(4) -0.0021(4) C5 0.022(2) 0.0158(19) 0.024(2) 0.0067(16) -0.0005(17) 0.0029(16) C6 0.019(2) 0.0101(17) 0.029(2) 0.0006(16) 0.0031(18) 0.0027(15) S7 0.0125(4) 0.0144(5) 0.0182(5) -0.0021(4) 0.0022(4) -0.0002(4) C8 0.023(2) 0.021(2) 0.0139(18) -0.0033(15) 0.0036(16) -0.0023(17) C9 0.026(2) 0.024(2) 0.016(2) -0.0033(17) -0.0026(16) -0.0048(18) P1 0.0149(7) 0.0109(6) 0.0168(7) 0.000 0.000 -0.0002(6) F1 0.0292(14) 0.0139(12) 0.0369(16) -0.0037(11) 0.0053(12) 0.0054(11) F2 0.119(4) 0.067(3) 0.146(4) -0.058(3) -0.108(4) 0.047(3) F3 0.141(5) 0.040(2) 0.151(4) 0.051(3) 0.125(4) 0.049(3) P2 0.0156(7) 0.0326(9) 0.0193(8) 0.000 0.000 -0.0040(7) F4 0.0172(13) 0.0503(19) 0.0381(16) 0.0078(15) -0.0037(12) -0.0038(13) F5 0.027(3) 0.469(14) 0.033(3) 0.000 0.000 0.029(7) F6 0.033(2) 0.042(2) 0.474(10) -0.003(4) 0.036(5) -0.002(2) F7 0.055(4) 0.477(14) 0.030(3) 0.000 0.000 0.085(8) C1S 0.033(3) 0.032(2) 0.035(3) -0.001(2) -0.003(2) -0.001(2) C2S 0.024(2) 0.035(2) 0.030(3) 0.003(2) -0.008(2) -0.005(2) N3S 0.066(4) 0.036(2) 0.075(4) 0.007(3) -0.031(3) -0.004(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 Pt S4 2.2925(10) . ? Pt S7 2.2995(10) . ? S1 C2 1.819(5) . ? S1 C9 1.820(5) . ? C2 C3 1.520(6) . ? C3 S4 1.828(4) . ? S4 C5 1.814(4) . ? C5 C6 1.514(6) . ? C6 S7 1.832(4) . ? S7 C8 1.817(4) . ? C8 C9 1.530(6) . ? P1 F1 1.601(2) . ? P1 F2 1.555(4) . ? P1 F3 1.552(4) . ? P2 F4 1.594(3) . ? P2 F5 1.519(5) . ? P2 F6 1.518(4) . ? P2 F7 1.517(5) . ? C1S C2S 1.456(7) . ? C2S N3S 1.128(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 S4 Pt S7 89.20(4) . . ? C2 S1 C9 104.6(2) . . ? C3 C2 S1 119.6(3) . . ? C2 C3 S4 116.2(3) . . ? C5 S4 C3 100.8(2) . . ? C5 S4 Pt 99.75(15) . . ? C3 S4 Pt 107.61(14) . . ? C6 C5 S4 113.6(3) . . ? C5 C6 S7 111.2(3) . . ? C8 S7 C6 103.5(2) . . ? C8 S7 Pt 105.08(15) . . ? C6 S7 Pt 104.80(15) . . ? C9 C8 S7 119.5(3) . . ? C8 C9 S1 116.0(3) . . ? F3 P1 F3 91.2(6) 2_565 . ? F3 P1 F2 179.2(4) 2_565 . ? F3 P1 F2 89.6(4) . . ? F3 P1 F1 89.73(17) 2_565 . ? F3 P1 F1 89.67(17) . . ? F2 P1 F1 90.36(19) . . ? F2 P1 F1 90.24(19) 2_565 . ? F1 P1 F1 179.1(2) 2_565 . ? F7 P2 F6 90.3(5) . . ? F6 P2 F6 179.5(9) 2_665 . ? F6 P2 F5 89.7(5) . . ? F7 P2 F4 89.91(13) . . ? F6 P2 F4 90.4(2) 2_665 . ? F6 P2 F4 89.6(2) . . ? F5 P2 F4 90.09(13) . . ? F4 P2 F4 179.8(3) . 2_665 ? N3S C2S C1S 178.7(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.26 _refine_diff_density_min -0.98 _refine_diff_density_rms 0.13 #===END of CIF # Attachment 'S3PTPF.CIF' data_s3ptpf _database_code_depnum_ccdc_archive 'CCDC 694379' _refine_special_details ; ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Pt S6 3+, 3(P F6 -), C2 H3 N' _chemical_formula_sum 'C14 H27 F18 N P3 Pt S6' _chemical_formula_weight 1031.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.2153(5) _cell_length_b 17.3138(9) _cell_length_c 18.8681(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3010.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11984 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1996 _exptl_absorpt_coefficient_mu 5.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.438 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details '(SADABS 2007/2; Sheldrick, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18675 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.054 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.53 _reflns_number_total 6785 _reflns_number_gt 6379 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)' _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^)+(0.039P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'MeCN H atoms from delta-F; others placed geometrically' _refine_ls_hydrogen_treatment 'rigid rotor; riding model' _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 0.012(5) _refine_ls_number_reflns 6785 _refine_ls_number_parameters 404 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.011 _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 Pt Pt 0.52420(2) 0.131726(11) 0.767898(11) 0.01801(6) Uani 1 1 d . . . S1 S 0.24808(15) 0.15616(8) 0.76054(9) 0.0239(3) Uani 1 1 d . . . S4 S 0.54694(16) 0.21084(8) 0.66752(8) 0.0258(3) Uani 1 1 d . . . S7 S 0.48974(15) 0.02520(7) 0.69325(7) 0.0206(3) Uani 1 1 d . . . C2 C 0.2424(7) 0.2157(4) 0.6809(3) 0.0311(14) Uani 1 1 d . . . H6A H 0.2301 0.1817 0.6391 0.037 Uiso 1 1 calc R . . H6B H 0.1569 0.2502 0.6835 0.037 Uiso 1 1 calc R . . C3 C 0.3771(7) 0.2644(3) 0.6707(4) 0.0307(14) Uani 1 1 d . . . H5A H 0.3827 0.3022 0.7100 0.037 Uiso 1 1 calc R . . H5B H 0.3668 0.2938 0.6261 0.037 Uiso 1 1 calc R . . C5 C 0.5243(7) 0.1435(3) 0.5935(3) 0.0276(12) Uani 1 1 d . . . H4A H 0.4206 0.1413 0.5799 0.033 Uiso 1 1 calc R . . H4B H 0.5801 0.1623 0.5522 0.033 Uiso 1 1 calc R . . C6 C 0.5760(7) 0.0637(3) 0.6135(3) 0.0250(12) Uani 1 1 d . . . H3A H 0.6823 0.0652 0.6209 0.030 Uiso 1 1 calc R . . H3B H 0.5566 0.0281 0.5735 0.030 Uiso 1 1 calc R . . C8 C 0.2965(6) 0.0261(4) 0.6706(4) 0.0280(13) Uani 1 1 d . . . H2A H 0.2833 0.0560 0.6263 0.034 Uiso 1 1 calc R . . H2B H 0.2647 -0.0275 0.6613 0.034 Uiso 1 1 calc R . . C9 C 0.1993(6) 0.0607(3) 0.7279(4) 0.0286(12) Uani 1 1 d . . . H1A H 0.1982 0.0248 0.7687 0.034 Uiso 1 1 calc R . . H1B H 0.0992 0.0633 0.7091 0.034 Uiso 1 1 calc R . . S1' S 0.79985(14) 0.10701(8) 0.76958(9) 0.0266(3) Uani 1 1 d . . . S4' S 0.50636(17) 0.05217(8) 0.86807(7) 0.0252(3) Uani 1 1 d . . . S7' S 0.56438(16) 0.23792(8) 0.84243(8) 0.0249(3) Uani 1 1 d . . . C2' C 0.8095(7) 0.0467(4) 0.8485(4) 0.0333(15) Uani 1 1 d . . . H1'A H 0.8943 0.0119 0.8442 0.040 Uiso 1 1 calc R . . H1'B H 0.8258 0.0803 0.8902 0.040 Uiso 1 1 calc R . . C3' C 0.6755(7) -0.0016(4) 0.8614(4) 0.0324(14) Uani 1 1 d . . . H2'A H 0.6894 -0.0311 0.9058 0.039 Uiso 1 1 calc R . . H2'B H 0.6663 -0.0394 0.8223 0.039 Uiso 1 1 calc R . . C5' C 0.5373(7) 0.1185(3) 0.9421(3) 0.0304(13) Uani 1 1 d . . . H3'A H 0.4839 0.0999 0.9843 0.037 Uiso 1 1 calc R . . H3'B H 0.6420 0.1193 0.9538 0.037 Uiso 1 1 calc R . . C6' C 0.4877(7) 0.1997(4) 0.9243(3) 0.0327(14) Uani 1 1 d . . . H4'A H 0.5146 0.2344 0.9639 0.039 Uiso 1 1 calc R . . H4'B H 0.3806 0.1999 0.9204 0.039 Uiso 1 1 calc R . . C8' C 0.7603(6) 0.2361(4) 0.8604(4) 0.0306(14) Uani 1 1 d . . . H5'A H 0.7937 0.2894 0.8698 0.037 Uiso 1 1 calc R . . H5'B H 0.7778 0.2053 0.9038 0.037 Uiso 1 1 calc R . . C9' C 0.8497(6) 0.2025(3) 0.8006(4) 0.0307(14) Uani 1 1 d . . . H6'A H 0.9522 0.2008 0.8162 0.037 Uiso 1 1 calc R . . H6'B H 0.8443 0.2385 0.7599 0.037 Uiso 1 1 calc R . . P P 0.5442(2) -0.15090(12) 1.03051(10) 0.0401(5) Uani 1 1 d D . . F1 F 0.4852(4) -0.1368(3) 0.9522(2) 0.0612(13) Uani 1 1 d D . . F2 F 0.6734(6) -0.2011(4) 1.0001(3) 0.099(2) Uani 1 1 d D . . F3 F 0.6405(7) -0.0776(4) 1.0245(3) 0.103(3) Uani 1 1 d D . . F4 F 0.4545(6) -0.2286(3) 1.0368(3) 0.0775(17) Uani 1 1 d D . . F5 F 0.4126(6) -0.1057(3) 1.0616(3) 0.082(2) Uani 1 1 d D . . F6 F 0.6037(6) -0.1653(3) 1.1080(2) 0.0621(14) Uani 1 1 d D . . P' P 0.87027(15) -0.11995(8) 0.66367(9) 0.0315(4) Uani 1 1 d D . . F1' F 0.7859(13) -0.0654(7) 0.7147(2) 0.039(3) Uiso 0.379(18) 1 d PD A 1 F2' F 0.7502(9) -0.1830(6) 0.6717(5) 0.035(3) Uiso 0.379(18) 1 d PD A 1 F3' F 0.7867(4) -0.0854(2) 0.5993(2) 0.0565(12) Uani 1 1 d D A . F4' F 0.9537(4) -0.1555(2) 0.72816(19) 0.0645(13) Uani 1 1 d D . . F5' F 0.9906(10) -0.0577(7) 0.6552(6) 0.060(4) Uiso 0.379(18) 1 d PD A 1 F6' F 0.9555(13) -0.1741(7) 0.6124(2) 0.040(3) Uiso 0.379(18) 1 d PD A 1 F11' F 0.8375(15) -0.0464(5) 0.7074(4) 0.051(3) Uiso 0.435(18) 1 d PD A 2 F12' F 0.7273(6) -0.1590(8) 0.6897(5) 0.057(4) Uiso 0.435(18) 1 d PD A 2 F15' F 1.0144(6) -0.0840(8) 0.6359(5) 0.057(4) Uiso 0.435(18) 1 d PD A 2 F16' F 0.9054(16) -0.1941(5) 0.6188(4) 0.054(4) Uiso 0.435(18) 1 d PD A 2 F21' F 0.926(3) -0.0384(4) 0.6840(10) 0.110(14) Uiso 0.188(11) 1 d PD A 3 F22' F 0.7350(13) -0.1068(17) 0.7114(5) 0.075(10) Uiso 0.188(11) 1 d PD A 3 F25' F 1.0051(12) -0.1327(16) 0.6163(5) 0.057(8) Uiso 0.188(11) 1 d PD A 3 F26' F 0.812(3) -0.2013(4) 0.6442(10) 0.081(11) Uiso 0.188(11) 1 d PD A 3 P" P 0.11234(18) 0.09517(10) 0.98680(9) 0.0277(3) Uani 1 1 d . . . F1" F -0.0211(5) 0.1504(2) 0.9662(2) 0.0419(9) Uani 1 1 d . . . F2" F 0.1633(6) 0.0925(2) 0.9053(2) 0.0507(12) Uani 1 1 d . . . F3" F 0.2103(4) 0.1698(2) 1.0010(2) 0.0407(10) Uani 1 1 d . . . F4" F 0.0108(5) 0.0210(2) 0.97364(19) 0.0396(9) Uani 1 1 d . . . F5" F 0.0628(4) 0.0979(2) 1.0676(2) 0.0392(9) Uani 1 1 d . . . F6" F 0.2432(5) 0.0398(3) 1.0077(3) 0.0510(11) Uani 1 1 d . . . C1S C 0.1670(8) -0.1292(5) 0.8924(5) 0.055(2) Uani 1 1 d . . . H1S1 H 0.1863 -0.1792 0.9148 0.082 Uiso 1 1 calc R . . H1S2 H 0.0648 -0.1266 0.8783 0.082 Uiso 1 1 calc R . . H1S3 H 0.1883 -0.0876 0.9260 0.082 Uiso 1 1 calc R . . C2S C 0.2582(8) -0.1208(4) 0.8302(4) 0.0409(17) Uani 1 1 d . . . N3S N 0.3298(8) -0.1156(4) 0.7821(4) 0.0576(19) 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 Pt 0.01782(9) 0.01698(9) 0.01924(10) -0.00043(8) -0.00046(8) -0.00123(7) S1 0.0241(6) 0.0238(6) 0.0238(7) -0.0002(6) 0.0013(6) 0.0028(5) S4 0.0294(8) 0.0203(6) 0.0277(7) 0.0028(6) 0.0028(6) -0.0015(6) S7 0.0206(6) 0.0196(6) 0.0217(6) -0.0021(5) 0.0004(6) -0.0001(5) C2 0.032(3) 0.036(3) 0.026(3) 0.004(3) -0.005(3) 0.013(3) C3 0.035(3) 0.025(3) 0.032(3) 0.006(3) 0.005(3) 0.009(3) C5 0.033(3) 0.034(3) 0.016(2) 0.001(2) 0.002(2) -0.006(3) C6 0.026(3) 0.028(3) 0.021(3) -0.006(2) 0.004(2) 0.001(2) C8 0.019(2) 0.028(3) 0.037(4) -0.004(3) -0.006(3) -0.004(2) C9 0.023(2) 0.029(3) 0.034(3) -0.001(3) 0.004(3) -0.003(2) S1' 0.0237(6) 0.0279(7) 0.0283(7) -0.0048(7) 0.0014(7) 0.0004(5) S4' 0.0284(8) 0.0251(6) 0.0221(6) 0.0021(5) -0.0015(6) -0.0052(6) S7' 0.0236(7) 0.0221(6) 0.0292(8) -0.0069(6) 0.0018(6) -0.0016(5) C2' 0.031(3) 0.035(3) 0.034(4) -0.002(3) -0.006(3) 0.010(3) C3' 0.038(3) 0.031(3) 0.029(3) 0.002(3) -0.006(3) 0.006(3) C5' 0.033(3) 0.037(3) 0.022(3) -0.005(2) 0.005(2) -0.007(3) C6' 0.032(3) 0.039(3) 0.027(3) -0.007(2) 0.010(3) -0.008(3) C8' 0.020(3) 0.029(3) 0.043(4) -0.010(3) -0.003(3) -0.009(2) C9' 0.020(3) 0.031(3) 0.041(4) -0.007(3) 0.002(3) -0.004(2) P 0.0305(9) 0.0571(12) 0.0325(9) -0.0186(8) 0.0043(7) -0.0067(8) F1 0.039(2) 0.102(4) 0.043(2) -0.018(2) -0.009(2) 0.014(3) F2 0.051(3) 0.178(7) 0.067(4) -0.003(5) 0.008(3) 0.053(4) F3 0.117(5) 0.125(6) 0.065(4) 0.038(4) -0.026(4) -0.084(5) F4 0.079(4) 0.046(3) 0.108(5) -0.025(3) -0.026(4) -0.009(3) F5 0.093(4) 0.076(4) 0.075(4) 0.012(3) 0.052(4) 0.037(3) F6 0.085(4) 0.067(3) 0.034(3) -0.004(2) -0.008(3) -0.024(3) P' 0.0265(7) 0.0223(8) 0.0457(10) 0.0016(7) 0.0023(7) 0.0023(6) F3' 0.051(3) 0.057(3) 0.062(3) 0.014(2) -0.008(2) 0.010(2) F4' 0.062(3) 0.075(3) 0.056(3) 0.007(3) -0.012(3) 0.012(2) P" 0.0316(8) 0.0255(8) 0.0260(8) 0.0001(6) 0.0016(7) -0.0007(7) F1" 0.045(2) 0.0308(19) 0.050(2) -0.0026(16) -0.021(2) 0.0055(18) F2" 0.079(3) 0.043(2) 0.031(2) -0.0018(18) 0.019(2) -0.013(2) F3" 0.038(2) 0.036(2) 0.048(3) -0.0050(19) 0.008(2) -0.0099(18) F4" 0.054(2) 0.0292(18) 0.0356(19) -0.0022(15) 0.004(2) -0.0108(19) F5" 0.048(2) 0.041(2) 0.0283(19) -0.0014(17) 0.0003(18) -0.0103(19) F6" 0.048(2) 0.045(3) 0.060(3) -0.005(2) -0.009(2) 0.016(2) C1S 0.045(4) 0.061(5) 0.059(5) -0.001(5) 0.004(4) 0.009(4) C2S 0.038(3) 0.023(3) 0.061(5) 0.006(3) -0.010(4) 0.001(3) N3S 0.061(4) 0.048(4) 0.064(5) 0.020(3) 0.013(4) 0.010(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 Pt S1 2.5832(14) . ? Pt S4 2.3467(15) . ? Pt S7 2.3423(13) . ? Pt S1' 2.5762(13) . ? Pt S4' 2.3445(14) . ? Pt S7' 2.3442(14) . ? S1 C9 1.819(6) . ? S1 C2 1.822(6) . ? S4 C3 1.820(6) . ? S4 C5 1.831(6) . ? S7 C6 1.828(6) . ? S7 C8 1.831(6) . ? C2 C3 1.512(9) . ? C2 H6A 0.9900 . ? C2 H6B 0.9900 . ? C3 H5A 0.9900 . ? C3 H5B 0.9900 . ? C5 C6 1.510(8) . ? C5 H4A 0.9900 . ? C5 H4B 0.9900 . ? C6 H3A 0.9900 . ? C6 H3B 0.9900 . ? C8 C9 1.527(8) . ? C8 H2A 0.9900 . ? C8 H2B 0.9900 . ? C9 H1A 0.9900 . ? C9 H1B 0.9900 . ? S1' C9' 1.814(6) . ? S1' C2' 1.821(7) . ? S4' C3' 1.820(7) . ? S4' C5' 1.831(6) . ? S7' C6' 1.824(6) . ? S7' C8' 1.837(6) . ? C2' C3' 1.511(9) . ? C2' H1'A 0.9900 . ? C2' H1'B 0.9900 . ? C3' H2'A 0.9900 . ? C3' H2'B 0.9900 . ? C5' C6' 1.514(9) . ? C5' H3'A 0.9900 . ? C5' H3'B 0.9900 . ? C6' H4'A 0.9900 . ? C6' H4'B 0.9900 . ? C8' C9' 1.513(9) . ? C8' H5'A 0.9900 . ? C8' H5'B 0.9900 . ? C9' H6'A 0.9900 . ? C9' H6'B 0.9900 . ? P F1 1.593(4) . ? P F2 1.582(5) . ? P F3 1.553(5) . ? P F4 1.583(5) . ? P F5 1.558(5) . ? P F6 1.581(5) . ? P' F25' 1.546(4) . ? P' F11' 1.548(4) . ? P' F21' 1.549(5) . ? P' F26' 1.551(5) . ? P' F22' 1.554(5) . ? P' F5' 1.555(4) . ? P' F1' 1.556(4) . ? P' F15' 1.557(4) . ? P' F3' 1.558(3) . ? P' F6' 1.559(4) . ? P' F12' 1.560(4) . ? P' F2' 1.562(4) . ? P" F6" 1.589(4) . ? P" F5" 1.593(4) . ? P" F3" 1.599(4) . ? P" F1" 1.605(4) . ? P" F2" 1.608(4) . ? P" F4" 1.608(4) . ? C1S C2S 1.450(11) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S N3S 1.126(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S7 Pt S7' 178.70(5) . . ? S7 Pt S4' 90.72(5) . . ? S7' Pt S4' 89.33(5) . . ? S7 Pt S4 89.22(5) . . ? S7' Pt S4 90.70(6) . . ? S4' Pt S4 178.88(6) . . ? S7 Pt S1' 90.59(5) . . ? S7' Pt S1' 88.12(5) . . ? S4' Pt S1' 87.80(5) . . ? S4 Pt S1' 91.08(5) . . ? S7 Pt S1 87.88(5) . . ? S7' Pt S1 93.41(5) . . ? S4' Pt S1 94.04(5) . . ? S4 Pt S1 87.08(5) . . ? S1' Pt S1 177.62(6) . . ? C9 S1 C2 103.2(3) . . ? C9 S1 Pt 96.47(18) . . ? C2 S1 Pt 99.5(2) . . ? C3 S4 C5 104.6(3) . . ? C3 S4 Pt 101.2(2) . . ? C5 S4 Pt 103.51(18) . . ? C6 S7 C8 103.1(3) . . ? C6 S7 Pt 98.60(19) . . ? C8 S7 Pt 105.4(2) . . ? C3 C2 S1 113.4(4) . . ? C3 C2 H6A 108.9 . . ? S1 C2 H6A 108.9 . . ? C3 C2 H6B 108.9 . . ? S1 C2 H6B 108.9 . . ? H6A C2 H6B 107.7 . . ? C2 C3 S4 115.2(4) . . ? C2 C3 H5A 108.5 . . ? S4 C3 H5A 108.5 . . ? C2 C3 H5B 108.5 . . ? S4 C3 H5B 108.5 . . ? H5A C3 H5B 107.5 . . ? C6 C5 S4 110.9(4) . . ? C6 C5 H4A 109.5 . . ? S4 C5 H4A 109.5 . . ? C6 C5 H4B 109.5 . . ? S4 C5 H4B 109.5 . . ? H4A C5 H4B 108.0 . . ? C5 C6 S7 113.7(4) . . ? C5 C6 H3A 108.8 . . ? S7 C6 H3A 108.8 . . ? C5 C6 H3B 108.8 . . ? S7 C6 H3B 108.8 . . ? H3A C6 H3B 107.7 . . ? C9 C8 S7 114.1(4) . . ? C9 C8 H2A 108.7 . . ? S7 C8 H2A 108.7 . . ? C9 C8 H2B 108.7 . . ? S7 C8 H2B 108.7 . . ? H2A C8 H2B 107.6 . . ? C8 C9 S1 116.8(4) . . ? C8 C9 H1A 108.1 . . ? S1 C9 H1A 108.1 . . ? C8 C9 H1B 108.1 . . ? S1 C9 H1B 108.1 . . ? H1A C9 H1B 107.3 . . ? C9' S1' C2' 104.3(3) . . ? C9' S1' Pt 95.86(19) . . ? C2' S1' Pt 98.8(2) . . ? C3' S4' C5' 103.9(3) . . ? C3' S4' Pt 100.6(2) . . ? C5' S4' Pt 103.6(2) . . ? C6' S7' C8' 102.6(3) . . ? C6' S7' Pt 99.3(2) . . ? C8' S7' Pt 104.6(2) . . ? C3' C2' S1' 114.1(5) . . ? C3' C2' H1'A 108.7 . . ? S1' C2' H1'A 108.7 . . ? C3' C2' H1'B 108.7 . . ? S1' C2' H1'B 108.7 . . ? H1'A C2' H1'B 107.6 . . ? C2' C3' S4' 115.3(4) . . ? C2' C3' H2'A 108.4 . . ? S4' C3' H2'A 108.4 . . ? C2' C3' H2'B 108.4 . . ? S4' C3' H2'B 108.4 . . ? H2'A C3' H2'B 107.5 . . ? C6' C5' S4' 111.5(4) . . ? C6' C5' H3'A 109.3 . . ? S4' C5' H3'A 109.3 . . ? C6' C5' H3'B 109.3 . . ? S4' C5' H3'B 109.3 . . ? H3'A C5' H3'B 108.0 . . ? C5' C6' S7' 114.0(4) . . ? C5' C6' H4'A 108.7 . . ? S7' C6' H4'A 108.7 . . ? C5' C6' H4'B 108.7 . . ? S7' C6' H4'B 108.7 . . ? H4'A C6' H4'B 107.6 . . ? C9' C8' S7' 113.8(4) . . ? C9' C8' H5'A 108.8 . . ? S7' C8' H5'A 108.8 . . ? C9' C8' H5'B 108.8 . . ? S7' C8' H5'B 108.8 . . ? H5'A C8' H5'B 107.7 . . ? C8' C9' S1' 116.9(4) . . ? C8' C9' H6'A 108.1 . . ? S1' C9' H6'A 108.1 . . ? C8' C9' H6'B 108.1 . . ? S1' C9' H6'B 108.1 . . ? H6'A C9' H6'B 107.3 . . ? F3 P F5 93.5(4) . . ? F3 P F6 89.9(3) . . ? F5 P F6 90.0(3) . . ? F3 P F2 89.6(4) . . ? F5 P F2 176.8(4) . . ? F6 P F2 89.3(3) . . ? F3 P F4 176.6(4) . . ? F5 P F4 89.6(3) . . ? F6 P F4 88.7(3) . . ? F2 P F4 87.3(3) . . ? F3 P F1 90.1(3) . . ? F5 P F1 90.4(3) . . ? F6 P F1 179.5(3) . . ? F2 P F1 90.2(3) . . ? F4 P F1 91.2(3) . . ? F25' P' F21' 90.4(5) . . ? F25' P' F26' 90.6(5) . . ? F21' P' F26' 179.0(6) . . ? F25' P' F22' 179.7(6) . . ? F21' P' F22' 89.3(5) . . ? F26' P' F22' 89.7(5) . . ? F5' P' F1' 90.0(4) . . ? F11' P' F15' 91.0(4) . . ? F5' P' F3' 90.06(18) . . ? F11' P' F3' 90.21(18) . . ? F21' P' F3' 90.38(18) . . ? F26' P' F3' 89.64(18) . . ? F22' P' F3' 89.97(18) . . ? F5' P' F3' 90.38(18) . . ? F1' P' F3' 90.16(17) . . ? F15' P' F3' 90.35(18) . . ? F5' P' F6' 89.6(4) . . ? F1' P' F6' 179.6(5) . . ? F3' P' F6' 89.74(18) . . ? F11' P' F12' 91.4(4) . . ? F15' P' F12' 177.6(4) . . ? F3' P' F12' 89.67(18) . . ? F5' P' F2' 179.4(5) . . ? F1' P' F2' 90.6(4) . . ? F3' P' F2' 89.64(17) . . ? F6' P' F2' 89.8(4) . . ? F6" P" F5" 89.9(2) . . ? F6" P" F3" 91.0(2) . . ? F5" P" F3" 88.7(2) . . ? F6" P" F1" 179.3(3) . . ? F5" P" F1" 89.7(2) . . ? F3" P" F1" 89.5(2) . . ? F6" P" F2" 89.9(3) . . ? F5" P" F2" 179.7(3) . . ? F3" P" F2" 91.1(2) . . ? F1" P" F2" 90.5(3) . . ? F6" P" F4" 89.9(2) . . ? F5" P" F4" 90.3(2) . . ? F3" P" F4" 178.6(2) . . ? F1" P" F4" 89.6(2) . . ? F2" P" F4" 90.0(2) . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? N3S C2S C1S 178.8(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 S1 C2 C3 -130.1(5) . . . . ? S1 C2 C3 S4 56.9(6) . . . . ? C5 S4 C3 C2 58.4(5) . . . . ? C3 S4 C5 C6 -135.0(4) . . . . ? S4 C5 C6 S7 55.1(5) . . . . ? C8 S7 C6 C5 58.6(5) . . . . ? C6 S7 C8 C9 -132.7(5) . . . . ? S7 C8 C9 S1 52.6(6) . . . . ? C2 S1 C9 C8 59.0(5) . . . . ? C9' S1' C2' C3' 129.2(5) . . . . ? S1' C2' C3' S4' -56.6(6) . . . . ? C5' S4' C3' C2' -58.8(6) . . . . ? C3' S4' C5' C6' 134.2(5) . . . . ? S4' C5' C6' S7' -53.3(6) . . . . ? C8' S7' C6' C5' -60.3(5) . . . . ? C6' S7' C8' C9' 133.6(5) . . . . ? S7' C8' C9' S1' -54.3(6) . . . . ? C2' S1' C9' C8' -56.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.95 _refine_diff_density_min -1.30 _refine_diff_density_rms 0.16 #===END of CIF