# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H9 D5 N5 Pt S4' _chemical_formula_weight 664.74 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' 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' D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3331(19) _cell_length_b 27.087(4) _cell_length_c 7.4501(9) _cell_angle_alpha 90.00 _cell_angle_beta 104.149(13) _cell_angle_gamma 90.00 _cell_volume 2413.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 353(2) _cell_measurement_reflns_used 1765 _cell_measurement_theta_min 3.2550 _cell_measurement_theta_max 21.7710 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 6.178 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.322 _exptl_absorpt_correction_T_max 0.350 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 353(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16097 _diffrn_reflns_av_R_equivalents 0.0894 _diffrn_reflns_av_unetI/netI 0.0853 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4477 _reflns_number_gt 2643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4472 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.76841(4) 0.228481(16) 0.04701(6) 0.0683(2) Uani 1 1 d . . . S1 S 0.6259(2) 0.28241(10) -0.0500(4) 0.0747(8) Uani 1 1 d . . . S2 S 0.8883(2) 0.29272(11) 0.1250(4) 0.0769(8) Uani 1 1 d . . . S3 S 0.6535(3) 0.16268(10) -0.0449(4) 0.0801(8) Uani 1 1 d . . . S4 S 0.9138(3) 0.17608(11) 0.1470(4) 0.0836(9) Uani 1 1 d . . . N1 N 0.5638(10) 0.4143(4) -0.1125(18) 0.124(4) Uani 1 1 d . . . N2 N 0.9030(11) 0.4273(4) 0.1114(19) 0.132(5) Uani 1 1 d . . . N3 N 0.6620(11) 0.0289(4) -0.0984(19) 0.132(5) Uani 1 1 d . . . N4 N 0.9998(12) 0.0493(4) 0.1519(19) 0.141(5) Uani 1 1 d . . . N5 N 0.2758(9) 0.0701(3) 0.8653(15) 0.082(3) Uani 1 1 d . . . C1 C 0.6216(12) 0.3814(4) -0.0705(17) 0.090(4) Uani 1 1 d . . . C2 C 0.6930(11) 0.3398(4) -0.0131(13) 0.078(3) Uani 1 1 d . . . C3 C 0.8021(10) 0.3402(5) 0.0595(12) 0.092(5) Uani 1 1 d . . . C4 C 0.8565(12) 0.3922(5) 0.0891(17) 0.097(4) Uani 1 1 d . . . C5 C 0.7009(10) 0.0669(5) -0.0521(18) 0.093(4) Uani 1 1 d . . . C6 C 0.7455(10) 0.1139(4) -0.0003(14) 0.078(3) Uani 1 1 d . . . C7 C 0.8561(11) 0.1200(4) 0.0868(15) 0.078(3) Uani 1 1 d . . . C8 C 0.9318(13) 0.0792(5) 0.1201(19) 0.104(4) Uani 1 1 d . . . C9 C 0.3721(14) 0.0645(5) 0.818(2) 0.117(5) Uani 1 1 d . . . D9A D 0.4390 0.0738 0.8994 0.141 Uiso 1 1 d R . . C10 C 0.3716(18) 0.0453(6) 0.652(3) 0.150(7) Uani 1 1 d . . . D10A D 0.4383 0.0430 0.6152 0.180 Uiso 1 1 d R . . C11 C 0.277(2) 0.0294(6) 0.537(2) 0.134(7) Uani 1 1 d . . . D11A D 0.2777 0.0156 0.4235 0.160 Uiso 1 1 d R . . C12 C 0.1793(15) 0.0338(5) 0.590(3) 0.121(6) Uani 1 1 d . . . D12A D 0.1123 0.0225 0.5149 0.145 Uiso 1 1 d R . . C13 C 0.1824(12) 0.0553(5) 0.759(2) 0.111(5) Uani 1 1 d . . . D13A D 0.1163 0.0593 0.7962 0.133 Uiso 1 1 d R . . C14 C 0.2775(10) 0.0937(5) 1.0460(17) 0.099(4) Uani 1 1 d . . . H14A H 0.3457(10) 0.0843(5) 1.1351(17) 0.119 Uiso 1 1 d R . . H14B H 0.2149(10) 0.0814(5) 1.0904(17) 0.119 Uiso 1 1 d R . . C15 C 0.2709(10) 0.1494(5) 1.0356(13) 0.074(3) Uani 1 1 d . . . C16 C 0.3670(10) 0.1779(5) 1.0811(16) 0.094(4) Uani 1 1 d . . . H16A H 0.4363(10) 0.1626(5) 1.1180(16) 0.113 Uiso 1 1 d R . . C17 C 0.3614(12) 0.2277(5) 1.0729(18) 0.093(4) Uani 1 1 d . . . H17A H 0.4274(12) 0.2459(5) 1.1024(18) 0.112 Uiso 1 1 d R . . C18 C 0.2602(11) 0.2525(5) 1.0217(14) 0.078(3) Uani 1 1 d . . . C19 C 0.1622(10) 0.2229(5) 0.9760(16) 0.087(4) Uani 1 1 d . . . H19A H 0.0923(10) 0.2379(5) 0.9418(16) 0.104 Uiso 1 1 d R . . C20 C 0.1696(10) 0.1725(5) 0.9820(16) 0.085(3) Uani 1 1 d . . . H20A H 0.1047(10) 0.1537(5) 0.9490(16) 0.102 Uiso 1 1 d R . . C21 C 0.2508(10) 0.3073(5) 1.0211(16) 0.114(5) Uani 1 1 d . . . H21A H 0.3242(10) 0.3216(5) 1.0548(16) 0.171 Uiso 1 1 d R . . H21B H 0.2093(10) 0.3173(5) 1.1085(16) 0.171 Uiso 1 1 d R . . H21C H 0.2127(10) 0.3184(5) 0.8996(16) 0.171 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0598(3) 0.0875(4) 0.0569(3) 0.0056(2) 0.0127(2) -0.0002(2) S1 0.0608(19) 0.0883(19) 0.0697(18) 0.0054(15) 0.0056(15) 0.0051(14) S2 0.0607(19) 0.0946(19) 0.0695(17) 0.0010(16) 0.0046(15) -0.0003(16) S3 0.070(2) 0.0883(19) 0.0803(19) 0.0083(16) 0.0162(16) -0.0072(16) S4 0.067(2) 0.098(2) 0.082(2) 0.0043(17) 0.0104(16) 0.0132(16) N1 0.103(10) 0.091(8) 0.170(12) -0.011(8) 0.016(8) 0.016(7) N2 0.119(11) 0.090(8) 0.171(12) -0.031(8) 0.008(9) -0.024(8) N3 0.129(11) 0.104(9) 0.158(12) 0.015(8) 0.027(9) -0.019(8) N4 0.149(13) 0.116(10) 0.150(11) -0.001(9) 0.017(10) 0.042(9) N5 0.062(7) 0.086(6) 0.098(8) -0.007(6) 0.019(6) 0.007(5) C1 0.100(11) 0.069(8) 0.099(9) -0.013(7) 0.018(8) 0.005(7) C2 0.115(10) 0.075(7) 0.048(6) 0.011(5) 0.031(6) 0.036(7) C3 0.080(8) 0.169(13) 0.026(5) 0.009(6) 0.011(5) 0.077(9) C4 0.108(12) 0.086(9) 0.090(9) -0.014(8) 0.007(8) -0.014(8) C5 0.064(8) 0.083(9) 0.121(11) 0.013(8) 0.003(7) -0.004(7) C6 0.101(10) 0.055(7) 0.072(7) 0.004(5) 0.011(7) -0.018(6) C7 0.081(9) 0.079(8) 0.066(7) 0.001(6) 0.005(6) -0.003(7) C8 0.117(13) 0.089(10) 0.100(10) 0.008(8) 0.015(9) 0.011(9) C9 0.104(12) 0.131(12) 0.124(13) -0.015(10) 0.041(10) 0.010(10) C10 0.158(19) 0.142(15) 0.19(2) -0.021(14) 0.110(17) -0.015(13) C11 0.21(2) 0.108(13) 0.092(12) 0.001(9) 0.046(15) 0.000(15) C12 0.110(14) 0.096(10) 0.131(14) -0.024(10) -0.021(11) 0.016(10) C13 0.075(11) 0.095(9) 0.150(14) -0.016(9) 0.000(10) 0.010(8) C14 0.084(10) 0.115(11) 0.097(10) 0.002(8) 0.021(8) 0.001(7) C15 0.071(8) 0.093(8) 0.056(6) -0.002(6) 0.012(6) 0.019(7) C16 0.057(8) 0.128(11) 0.089(9) 0.005(8) 0.001(6) -0.026(8) C17 0.067(9) 0.112(11) 0.096(10) -0.013(8) 0.012(8) -0.029(8) C18 0.096(11) 0.094(9) 0.045(6) 0.000(6) 0.018(6) -0.006(8) C19 0.054(8) 0.119(11) 0.081(8) -0.005(7) 0.004(7) 0.011(7) C20 0.060(8) 0.096(9) 0.095(9) -0.012(7) 0.010(7) -0.001(7) C21 0.155(15) 0.093(10) 0.091(9) 0.003(8) 0.023(9) 0.005(8) _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 S1 2.264(3) . ? Pt1 S4 2.265(3) . ? Pt1 S2 2.266(3) . ? Pt1 S3 2.276(3) . ? S1 C2 1.751(12) . ? S2 C3 1.665(11) . ? S3 C6 1.721(12) . ? S4 C7 1.691(11) . ? N1 C1 1.137(13) . ? N2 C4 1.101(14) . ? N3 C5 1.153(14) . ? N4 C8 1.148(15) . ? N5 C13 1.294(14) . ? N5 C9 1.326(15) . ? N5 C14 1.486(13) . ? C1 C2 1.429(15) . ? C2 C3 1.321(16) . ? C3 C4 1.551(18) . ? C5 C6 1.402(16) . ? C6 C7 1.369(14) . ? C7 C8 1.429(16) . ? C9 C10 1.35(2) . ? C10 C11 1.34(2) . ? C11 C12 1.36(2) . ? C12 C13 1.374(18) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.512(16) . ? C15 C20 1.367(14) . ? C15 C16 1.386(14) . ? C16 H16A 0.9300 . ? C16 C17 1.351(14) . ? C17 H17A 0.9300 . ? C17 C18 1.386(16) . ? C18 C19 1.421(16) . ? C18 C21 1.490(18) . ? C19 H19A 0.9300 . ? C19 C20 1.367(13) . ? C20 H20A 0.9300 . ? C21 H21B 0.9600 . ? C21 H21A 0.9600 . ? C21 H21C 0.9600 . ? 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 S1 Pt1 S4 178.60(11) . . ? S1 Pt1 S2 89.63(11) . . ? S4 Pt1 S2 88.99(11) . . ? S1 Pt1 S3 91.80(11) . . ? S4 Pt1 S3 89.59(11) . . ? S2 Pt1 S3 176.49(11) . . ? C2 S1 Pt1 102.8(4) . . ? C3 S2 Pt1 100.8(6) . . ? C6 S3 Pt1 102.2(4) . . ? C7 S4 Pt1 103.2(4) . . ? C13 N5 C9 121.6(13) . . ? C13 N5 C14 120.2(12) . . ? C9 N5 C14 118.2(12) . . ? N1 C1 C2 178.4(16) . . ? C3 C2 C1 127.4(12) . . ? C3 C2 S1 117.8(9) . . ? C1 C2 S1 114.8(10) . . ? C2 C3 C4 115.3(10) . . ? C2 C3 S2 128.8(12) . . ? C4 C3 S2 115.8(10) . . ? N2 C4 C3 174.4(16) . . ? N3 C5 C6 178.1(15) . . ? C7 C6 C5 121.3(11) . . ? C7 C6 S3 122.1(8) . . ? C5 C6 S3 116.6(9) . . ? C6 C7 C8 121.4(10) . . ? C6 C7 S4 122.7(9) . . ? C8 C7 S4 115.7(10) . . ? N4 C8 C7 174.1(17) . . ? N5 C9 C10 119.0(16) . . ? C11 C10 C9 121.2(19) . . ? C10 C11 C12 119.0(19) . . ? C11 C12 C13 118.2(16) . . ? N5 C13 C12 120.9(14) . . ? H14A C14 H14B 107.7 . . ? H14A C14 N5 108.9(6) . . ? H14B C14 N5 108.9(6) . . ? H14A C14 C15 108.9(6) . . ? H14B C14 C15 108.9(6) . . ? N5 C14 C15 113.3(10) . . ? C20 C15 C16 118.8(12) . . ? C20 C15 C14 120.4(12) . . ? C16 C15 C14 120.8(11) . . ? H16A C16 C17 119.5(8) . . ? H16A C16 C15 119.5(8) . . ? C17 C16 C15 121.0(12) . . ? H17A C17 C16 119.1(8) . . ? H17A C17 C18 119.1(8) . . ? C16 C17 C18 121.9(12) . . ? C17 C18 C19 116.7(12) . . ? C17 C18 C21 123.2(12) . . ? C19 C18 C21 120.0(12) . . ? H19A C19 C20 119.7(7) . . ? H19A C19 C18 119.7(8) . . ? C20 C19 C18 120.6(12) . . ? H20A C20 C15 119.5(8) . . ? H20A C20 C19 119.5(7) . . ? C15 C20 C19 121.1(12) . . ? H21B C21 H21A 109.5 . . ? H21B C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 C18 109.5(6) . . ? H21A C21 C18 109.5(7) . . ? H21C C21 C18 109.5(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.457 _refine_diff_density_min -1.119 _refine_diff_density_rms 0.142 _database_code_depnum_ccdc_archive 'CCDC 935812' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H14 N5 Pt S4' _chemical_formula_weight 659.70 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3066(8) _cell_length_b 27.0522(18) _cell_length_c 7.4248(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.204(6) _cell_angle_gamma 90.00 _cell_volume 2396.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 353(2) _cell_measurement_reflns_used 2571 _cell_measurement_theta_min 2.9210 _cell_measurement_theta_max 22.7220 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 6.222 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.62964 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 353(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16004 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_unetI/netI 0.0616 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4444 _reflns_number_gt 2933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0203P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00139(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4444 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.76870(2) 0.228468(11) 0.04708(4) 0.06333(13) Uani 1 1 d . . . S1 S 0.62543(16) 0.28240(7) -0.0501(3) 0.0706(5) Uani 1 1 d . . . S2 S 0.88866(16) 0.29263(7) 0.1246(2) 0.0717(5) Uani 1 1 d . . . S3 S 0.65376(17) 0.16268(7) -0.0450(3) 0.0755(6) Uani 1 1 d . . . S4 S 0.91413(16) 0.17641(7) 0.1476(3) 0.0788(6) Uani 1 1 d . . . N1 N 0.5627(7) 0.4143(3) -0.1154(11) 0.122(3) Uani 1 1 d . . . N2 N 0.9035(7) 0.4267(3) 0.1147(11) 0.121(3) Uani 1 1 d . . . N3 N 0.6628(7) 0.0285(3) -0.1003(12) 0.128(3) Uani 1 1 d . . . N4 N 0.9998(8) 0.0493(3) 0.1521(12) 0.136(3) Uani 1 1 d . . . N5 N 0.2767(6) 0.0704(2) 0.8673(9) 0.0766(17) Uani 1 1 d . . . C1 C 0.6214(7) 0.3821(3) -0.0706(12) 0.085(2) Uani 1 1 d . . . C2 C 0.6900(6) 0.3395(3) -0.0169(9) 0.066(2) Uani 1 1 d . . . C3 C 0.8019(6) 0.3428(3) 0.0593(8) 0.068(2) Uani 1 1 d . . . C4 C 0.8572(7) 0.3909(3) 0.0885(11) 0.086(2) Uani 1 1 d . . . C5 C 0.7010(7) 0.0659(4) -0.0529(12) 0.089(3) Uani 1 1 d . . . C6 C 0.7458(7) 0.1139(3) 0.0018(9) 0.073(2) Uani 1 1 d . . . C7 C 0.8563(7) 0.1198(3) 0.0867(10) 0.074(2) Uani 1 1 d . . . C8 C 0.9335(8) 0.0794(3) 0.1216(12) 0.095(3) Uani 1 1 d . . . C9 C 0.3710(8) 0.0644(3) 0.8180(14) 0.109(3) Uani 1 1 d . . . H9A H 0.4380 0.0744 0.8981 0.131 Uiso 1 1 calc R . . C10 C 0.3725(12) 0.0438(4) 0.650(2) 0.142(5) Uani 1 1 d . . . H10A H 0.4396 0.0392 0.6165 0.171 Uiso 1 1 calc R . . C11 C 0.2738(14) 0.0302(4) 0.5354(15) 0.126(4) Uani 1 1 d . . . H11A H 0.2716 0.0178 0.4178 0.151 Uiso 1 1 calc R . . C12 C 0.1784(10) 0.0350(4) 0.5931(17) 0.133(4) Uani 1 1 d . . . H12A H 0.1104 0.0243 0.5182 0.160 Uiso 1 1 calc R . . C13 C 0.1828(9) 0.0552(3) 0.7586(15) 0.105(3) Uani 1 1 d . . . H13A H 0.1169 0.0585 0.7976 0.126 Uiso 1 1 calc R . . C14 C 0.2767(7) 0.0940(3) 1.0484(10) 0.095(3) Uani 1 1 d . . . H14A H 0.3446 0.0847 1.1393 0.114 Uiso 1 1 calc R . . H14B H 0.2134 0.0817 1.0913 0.114 Uiso 1 1 calc R . . C15 C 0.2701(7) 0.1490(3) 1.0360(9) 0.0673(19) Uani 1 1 d . . . C16 C 0.3655(7) 0.1773(4) 1.0796(10) 0.089(2) Uani 1 1 d . . . H16A H 0.4351 0.1619 1.1144 0.107 Uiso 1 1 calc R . . C17 C 0.3595(8) 0.2277(4) 1.0726(11) 0.091(3) Uani 1 1 d . . . H17A H 0.4256 0.2459 1.1029 0.109 Uiso 1 1 calc R . . C18 C 0.2591(8) 0.2524(3) 1.0223(10) 0.079(2) Uani 1 1 d . . . C19 C 0.1638(7) 0.2232(3) 0.9763(10) 0.084(2) Uani 1 1 d . . . H19A H 0.0941 0.2384 0.9410 0.101 Uiso 1 1 calc R . . C20 C 0.1691(7) 0.1730(3) 0.9811(10) 0.084(2) Uani 1 1 d . . . H20A H 0.1033 0.1547 0.9467 0.100 Uiso 1 1 calc R . . C21 C 0.2513(7) 0.3083(3) 1.0191(10) 0.116(3) Uani 1 1 d . . . H21A H 0.3252 0.3221 1.0555 0.174 Uiso 1 1 calc R . . H21B H 0.2084 0.3189 1.1039 0.174 Uiso 1 1 calc R . . H21C H 0.2152 0.3191 0.8959 0.174 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 0.0541(2) 0.0822(2) 0.05507(19) 0.00568(15) 0.01599(14) 0.00033(17) S1 0.0525(12) 0.0857(14) 0.0713(12) 0.0039(10) 0.0109(10) 0.0010(11) S2 0.0525(12) 0.0910(14) 0.0676(12) 0.0014(10) 0.0075(10) -0.0008(11) S3 0.0611(13) 0.0863(14) 0.0779(13) 0.0093(11) 0.0148(10) -0.0059(12) S4 0.0584(13) 0.0947(15) 0.0812(13) 0.0014(11) 0.0132(11) 0.0081(12) N1 0.101(7) 0.098(6) 0.159(7) 0.000(5) 0.017(6) 0.033(5) N2 0.100(7) 0.100(6) 0.153(7) -0.016(6) 0.012(5) -0.020(5) N3 0.117(8) 0.090(6) 0.164(8) 0.017(6) 0.010(6) -0.013(6) N4 0.137(9) 0.114(7) 0.143(7) 0.004(5) 0.009(6) 0.042(6) N5 0.065(5) 0.076(4) 0.082(5) 0.005(4) 0.004(4) 0.002(4) C1 0.061(6) 0.084(6) 0.105(6) -0.007(5) 0.010(5) 0.006(5) C2 0.056(5) 0.091(6) 0.051(4) -0.001(4) 0.016(4) -0.007(5) C3 0.067(5) 0.088(6) 0.052(4) -0.006(4) 0.021(4) 0.002(5) C4 0.058(6) 0.092(7) 0.098(6) -0.009(5) 0.001(5) -0.004(5) C5 0.066(6) 0.094(7) 0.099(6) 0.023(6) 0.006(5) 0.006(6) C6 0.078(6) 0.067(5) 0.074(5) 0.001(4) 0.022(5) -0.016(5) C7 0.070(6) 0.080(6) 0.073(5) 0.005(4) 0.023(5) 0.013(5) C8 0.098(8) 0.087(7) 0.096(6) -0.005(5) 0.016(6) 0.013(6) C9 0.069(7) 0.130(8) 0.129(9) -0.021(6) 0.028(6) -0.003(6) C10 0.153(13) 0.141(10) 0.159(12) -0.022(9) 0.088(11) -0.019(9) C11 0.198(16) 0.090(8) 0.091(8) -0.003(6) 0.039(10) 0.006(10) C12 0.123(11) 0.119(9) 0.127(10) -0.023(7) -0.026(8) 0.002(8) C13 0.089(8) 0.103(7) 0.115(8) -0.023(6) 0.009(6) -0.001(6) C14 0.093(7) 0.116(7) 0.075(6) 0.006(5) 0.018(5) -0.001(6) C15 0.060(5) 0.080(6) 0.061(4) 0.005(4) 0.014(4) 0.009(5) C16 0.053(6) 0.128(8) 0.083(6) 0.006(5) 0.008(4) 0.007(6) C17 0.075(7) 0.116(8) 0.081(6) -0.006(5) 0.017(5) -0.026(7) C18 0.086(7) 0.103(7) 0.050(5) -0.003(4) 0.024(5) -0.008(6) C19 0.059(6) 0.098(7) 0.091(6) -0.009(5) 0.012(5) 0.012(5) C20 0.053(6) 0.097(7) 0.096(6) -0.013(5) 0.009(5) -0.004(5) C21 0.164(10) 0.106(7) 0.079(6) -0.007(5) 0.031(6) -0.022(7) _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 S4 2.256(2) . ? Pt1 S2 2.2598(19) . ? Pt1 S1 2.2658(19) . ? Pt1 S3 2.2718(19) . ? S1 C2 1.726(7) . ? S2 C3 1.722(7) . ? S3 C6 1.718(8) . ? S4 C7 1.703(8) . ? N1 C1 1.128(9) . ? N2 C4 1.116(9) . ? N3 C5 1.135(10) . ? N4 C8 1.136(10) . ? N5 C13 1.302(10) . ? N5 C9 1.310(9) . ? N5 C14 1.488(8) . ? C1 C2 1.426(10) . ? C2 C3 1.358(9) . ? C3 C4 1.460(10) . ? C5 C6 1.429(11) . ? C6 C7 1.361(9) . ? C7 C8 1.428(10) . ? C9 C10 1.368(12) . ? C9 H9A 0.9300 . ? C10 C11 1.353(13) . ? C10 H10A 0.9300 . ? C11 C12 1.351(13) . ? C11 H11A 0.9300 . ? C12 C13 1.334(11) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.490(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.372(10) . ? C15 C20 1.374(9) . ? C16 C17 1.368(10) . ? C16 H16A 0.9300 . ? C17 C18 1.374(11) . ? C17 H17A 0.9300 . ? C18 C19 1.386(10) . ? C18 C21 1.513(11) . ? C19 C20 1.359(9) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 Pt1 S2 88.82(7) . . ? S4 Pt1 S1 178.50(7) . . ? S2 Pt1 S1 89.72(7) . . ? S4 Pt1 S3 89.73(7) . . ? S2 Pt1 S3 176.37(6) . . ? S1 Pt1 S3 91.74(7) . . ? C2 S1 Pt1 103.6(3) . . ? C3 S2 Pt1 102.3(3) . . ? C6 S3 Pt1 102.1(3) . . ? C7 S4 Pt1 103.2(3) . . ? C13 N5 C9 120.0(8) . . ? C13 N5 C14 119.9(8) . . ? C9 N5 C14 120.1(8) . . ? N1 C1 C2 176.6(10) . . ? C3 C2 C1 122.2(7) . . ? C3 C2 S1 120.2(6) . . ? C1 C2 S1 117.6(6) . . ? C2 C3 C4 120.6(7) . . ? C2 C3 S2 124.1(6) . . ? C4 C3 S2 115.3(6) . . ? N2 C4 C3 177.0(10) . . ? N3 C5 C6 177.8(10) . . ? C7 C6 C5 120.6(8) . . ? C7 C6 S3 122.6(6) . . ? C5 C6 S3 116.8(6) . . ? C6 C7 C8 122.6(8) . . ? C6 C7 S4 122.2(6) . . ? C8 C7 S4 115.0(7) . . ? N4 C8 C7 176.1(11) . . ? N5 C9 C10 121.0(10) . . ? N5 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C11 C10 C9 118.4(12) . . ? C11 C10 H10A 120.8 . . ? C9 C10 H10A 120.8 . . ? C12 C11 C10 119.3(12) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C13 C12 C11 119.3(12) . . ? C13 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? N5 C13 C12 122.0(10) . . ? N5 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? N5 C14 C15 112.6(6) . . ? N5 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N5 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C20 117.7(8) . . ? C16 C15 C14 120.8(8) . . ? C20 C15 C14 121.5(8) . . ? C17 C16 C15 120.9(8) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 122.2(9) . . ? C16 C17 H17A 118.9 . . ? C18 C17 H17A 118.9 . . ? C17 C18 C19 116.1(8) . . ? C17 C18 C21 122.6(9) . . ? C19 C18 C21 121.3(9) . . ? C20 C19 C18 122.1(8) . . ? C20 C19 H19A 118.9 . . ? C18 C19 H19A 118.9 . . ? C19 C20 C15 121.0(8) . . ? C19 C20 H20A 119.5 . . ? C15 C20 H20A 119.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.773 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.103 _database_code_depnum_ccdc_archive 'CCDC 935813' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H9 D5 N5 Pt S4' _chemical_formula_weight 664.74 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' 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' D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3308(8) _cell_length_b 12.2848(13) _cell_length_c 26.930(3) _cell_angle_alpha 88.479(3) _cell_angle_beta 86.652(4) _cell_angle_gamma 75.563(3) _cell_volume 2344.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3103 _cell_measurement_theta_min 3.0870 _cell_measurement_theta_max 24.9170 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.883 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 6.360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.311 _exptl_absorpt_correction_T_max 0.339 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44144 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_unetI/netI 0.0629 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.76 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8713 _reflns_number_gt 6787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0326P)^2^+89.2530P] 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 8707 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.2112 _refine_ls_wR_factor_gt 0.2044 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.197 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.43585(10) 0.27525(6) 0.23465(3) 0.0439(2) Uani 1 1 d . . . Pt2 Pt 0.94940(10) 0.26943(6) 0.27095(3) 0.0415(2) Uani 1 1 d . . . S1 S 0.8604(8) 0.4165(4) 0.3225(2) 0.0575(13) Uani 1 1 d . . . S2 S 1.0435(7) 0.1540(4) 0.33699(19) 0.0506(12) Uani 1 1 d . . . S3 S 0.8706(7) 0.3895(4) 0.20655(19) 0.0487(12) Uani 1 1 d . . . S4 S 1.0408(7) 0.1255(4) 0.21696(19) 0.0468(11) Uani 1 1 d . . . S5 S 0.3682(7) 0.3959(4) 0.2984(2) 0.0538(13) Uani 1 1 d . . . S6 S 0.5346(7) 0.1312(4) 0.2882(2) 0.0494(12) Uani 1 1 d . . . S7 S 0.3331(8) 0.4215(4) 0.1822(2) 0.0546(13) Uani 1 1 d . . . S8 S 0.5213(9) 0.1587(4) 0.1688(2) 0.0600(14) Uani 1 1 d . . . N1 N 0.866(3) 0.5018(19) 0.4487(8) 0.086(7) Uani 1 1 d . . . N2 N 1.117(4) 0.163(2) 0.4701(8) 0.090(7) Uani 1 1 d . . . N3 N 0.857(3) 0.4047(19) 0.0718(8) 0.095(8) Uani 1 1 d . . . N4 N 1.089(4) 0.0619(19) 0.0841(8) 0.097(8) Uani 1 1 d . . . N5 N 0.410(4) 0.4139(18) 0.4322(9) 0.093(7) Uani 1 1 d . . . N6 N 0.621(3) 0.0706(16) 0.4190(8) 0.081(6) Uani 1 1 d . . . N7 N 0.329(4) 0.501(2) 0.0514(9) 0.104(9) Uani 1 1 d . . . N8 N 0.574(4) 0.163(2) 0.0323(9) 0.103(8) Uani 1 1 d . . . N9 N 0.116(2) 0.7808(13) 0.4300(6) 0.048(4) Uani 1 1 d . . . N10 N 0.627(3) 0.7786(14) 0.0678(6) 0.058(4) Uani 1 1 d . . . C1 C 0.890(3) 0.4355(19) 0.4187(9) 0.064(6) Uani 1 1 d . . . C2 C 0.926(3) 0.3593(17) 0.3795(8) 0.053(5) Uani 1 1 d . . . C3 C 1.004(2) 0.2492(18) 0.3853(8) 0.050(5) Uani 1 1 d . . . C4 C 1.062(3) 0.2003(19) 0.4335(9) 0.061(6) Uani 1 1 d . . . C5 C 0.885(3) 0.3590(17) 0.1098(8) 0.058(5) Uani 1 1 d . . . C6 C 0.925(3) 0.3021(18) 0.1554(8) 0.061(6) Uani 1 1 d . . . C7 C 0.996(2) 0.1928(17) 0.1611(8) 0.048(5) Uani 1 1 d . . . C8 C 1.047(4) 0.1182(19) 0.1172(9) 0.074(7) Uani 1 1 d . . . C9 C 0.424(3) 0.3660(19) 0.3951(8) 0.057(5) Uani 1 1 d . . . C10 C 0.436(3) 0.3128(17) 0.3490(8) 0.055(5) Uani 1 1 d . . . C11 C 0.509(3) 0.1978(14) 0.3440(7) 0.046(5) Uani 1 1 d . . . C12 C 0.570(3) 0.1266(18) 0.3873(9) 0.062(6) Uani 1 1 d . . . C13 C 0.352(4) 0.439(2) 0.0837(10) 0.077(7) Uani 1 1 d . . . C14 C 0.387(3) 0.3594(18) 0.1251(8) 0.058(5) Uani 1 1 d . . . C15 C 0.477(3) 0.249(2) 0.1187(8) 0.062(6) Uani 1 1 d . . . C16 C 0.524(4) 0.200(2) 0.0711(10) 0.071(7) Uani 1 1 d . . . C17 C 0.230(4) 0.6846(18) 0.4434(9) 0.066(6) Uani 1 1 d . . . C18 C 0.397(4) 0.680(2) 0.4641(9) 0.080(8) Uani 1 1 d . . . C19 C 0.455(4) 0.777(3) 0.4685(10) 0.093(9) Uani 1 1 d . . . C20 C 0.334(5) 0.874(3) 0.4537(11) 0.091(9) Uani 1 1 d . . . C21 C 0.169(4) 0.8774(19) 0.4337(9) 0.068(6) Uani 1 1 d . . . C22 C -0.067(3) 0.783(2) 0.4073(9) 0.066(6) Uani 1 1 d . . . H22A H -0.114(3) 0.721(2) 0.4209(9) 0.080 Uiso 1 1 d R . . H22B H -0.159(3) 0.852(2) 0.4168(9) 0.080 Uiso 1 1 d R . . C23 C -0.052(3) 0.7756(16) 0.3528(8) 0.050(5) Uani 1 1 d . . . C24 C 0.007(3) 0.6737(17) 0.3294(8) 0.057(5) Uani 1 1 d . . . H24A H 0.039(3) 0.6075(17) 0.3480(8) 0.068 Uiso 1 1 d R . . C25 C 0.017(3) 0.6707(17) 0.2775(9) 0.059(6) Uani 1 1 d . . . H25A H 0.060(3) 0.6013(17) 0.2622(9) 0.071 Uiso 1 1 d R . . C26 C -0.033(3) 0.7633(19) 0.2483(8) 0.054(5) Uani 1 1 d . . . C27 C -0.090(3) 0.8655(18) 0.2721(9) 0.062(6) Uani 1 1 d . . . H27A H -0.124(3) 0.9314(18) 0.2534(9) 0.074 Uiso 1 1 d R . . C28 C -0.096(3) 0.8706(16) 0.3226(10) 0.063(6) Uani 1 1 d . . . H28A H -0.131(3) 0.9408(16) 0.3375(10) 0.075 Uiso 1 1 d R . . C29 C -0.032(3) 0.757(2) 0.1920(8) 0.076(7) Uani 1 1 d . . . H29A H 0.011(3) 0.680(2) 0.1821(8) 0.114 Uiso 1 1 d R . . H29B H 0.050(3) 0.799(2) 0.1771(8) 0.114 Uiso 1 1 d R . . H29C H -0.158(3) 0.787(2) 0.1814(8) 0.114 Uiso 1 1 d R . . C30 C 0.740(4) 0.684(2) 0.0525(9) 0.081(8) Uani 1 1 d . . . C31 C 0.909(6) 0.681(3) 0.0312(11) 0.122(15) Uani 1 1 d . . . C32 C 0.974(5) 0.781(4) 0.0260(11) 0.111(13) Uani 1 1 d . . . C33 C 0.846(7) 0.872(3) 0.0418(12) 0.116(13) Uani 1 1 d . . . C34 C 0.681(5) 0.875(3) 0.0629(11) 0.097(9) Uani 1 1 d . . . C35 C 0.442(3) 0.780(2) 0.0933(9) 0.068(6) Uani 1 1 d . . . H35A H 0.399(3) 0.717(2) 0.0822(9) 0.082 Uiso 1 1 d R . . H35B H 0.352(3) 0.849(2) 0.0842(9) 0.082 Uiso 1 1 d R . . C36 C 0.453(3) 0.7740(18) 0.1497(9) 0.059(5) Uani 1 1 d . . . C37 C 0.509(3) 0.6716(18) 0.1731(9) 0.065(6) Uani 1 1 d . . . H37A H 0.543(3) 0.6067(18) 0.1542(9) 0.078 Uiso 1 1 d R . . C38 C 0.517(3) 0.6632(17) 0.2242(9) 0.065(6) Uani 1 1 d . . . H38A H 0.552(3) 0.5931(17) 0.2397(9) 0.078 Uiso 1 1 d R . . C39 C 0.470(3) 0.7612(19) 0.2523(9) 0.058(6) Uani 1 1 d . . . C40 C 0.418(3) 0.864(2) 0.2281(10) 0.069(7) Uani 1 1 d . . . H40A H 0.387(3) 0.929(2) 0.2464(10) 0.082 Uiso 1 1 d R . . C41 C 0.412(3) 0.8694(17) 0.1783(10) 0.065(6) Uani 1 1 d . . . H41A H 0.378(3) 0.9395(17) 0.1628(10) 0.078 Uiso 1 1 d R . . C42 C 0.473(3) 0.753(2) 0.3071(9) 0.086(8) Uani 1 1 d . . . H42A H 0.438(3) 0.826(2) 0.3211(9) 0.130 Uiso 1 1 d R . . H42B H 0.598(3) 0.715(2) 0.3162(9) 0.130 Uiso 1 1 d R . . H42C H 0.386(3) 0.710(2) 0.3196(9) 0.130 Uiso 1 1 d R . . D17A D 0.1932 0.6187 0.4385 0.104 Uiso 1 1 d R . . D18A D 0.4692 0.6122 0.4751 0.104 Uiso 1 1 d R . . D20A D 0.3662 0.9419 0.4575 0.104 Uiso 1 1 d R . . D21A D 0.0905 0.9455 0.4227 0.104 Uiso 1 1 d R . . D30A D 0.6982 0.6188 0.0564 0.104 Uiso 1 1 d R . . D31A D 0.9837 0.6133 0.0198 0.104 Uiso 1 1 d R . . D32A D 1.0919 0.7826 0.0127 0.104 Uiso 1 1 d R . . D33A D 0.8770 0.9410 0.0373 0.104 Uiso 1 1 d R . . D34A D 0.5993 0.9437 0.0740 0.104 Uiso 1 1 d R . . D19A D 0.5696 0.7766 0.4810 0.104 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0387(4) 0.0359(4) 0.0592(5) 0.0033(3) -0.0113(3) -0.0120(3) Pt2 0.0376(4) 0.0366(4) 0.0516(5) 0.0009(3) -0.0032(3) -0.0117(3) S1 0.073(4) 0.040(3) 0.057(3) -0.001(2) -0.006(3) -0.007(2) S2 0.055(3) 0.039(3) 0.056(3) 0.004(2) -0.001(2) -0.010(2) S3 0.042(3) 0.041(3) 0.058(3) 0.000(2) -0.008(2) -0.002(2) S4 0.047(3) 0.034(2) 0.057(3) 0.000(2) -0.001(2) -0.007(2) S5 0.053(3) 0.036(2) 0.069(3) 0.004(2) -0.011(3) -0.002(2) S6 0.052(3) 0.033(2) 0.062(3) 0.000(2) -0.012(2) -0.007(2) S7 0.064(3) 0.036(3) 0.064(3) 0.003(2) -0.013(3) -0.010(2) S8 0.076(4) 0.040(3) 0.066(3) -0.001(2) -0.018(3) -0.014(3) N1 0.107(18) 0.077(15) 0.072(14) -0.020(12) -0.004(13) -0.014(13) N2 0.115(19) 0.090(16) 0.057(13) 0.010(12) 0.000(13) -0.013(14) N3 0.103(18) 0.087(16) 0.070(15) 0.003(13) -0.007(13) 0.023(13) N4 0.15(2) 0.076(15) 0.058(13) -0.023(12) 0.006(14) -0.020(15) N5 0.13(2) 0.062(13) 0.076(15) -0.004(12) 0.009(14) 0.000(13) N6 0.109(17) 0.054(12) 0.067(13) 0.012(10) -0.008(12) 0.004(11) N7 0.106(19) 0.099(18) 0.080(16) 0.023(14) -0.002(14) 0.022(15) N8 0.13(2) 0.097(18) 0.066(15) 0.006(14) -0.014(15) -0.003(16) N9 0.053(10) 0.045(9) 0.046(9) -0.011(7) 0.001(7) -0.010(8) N10 0.072(12) 0.046(10) 0.054(11) -0.001(8) -0.012(9) -0.009(9) C1 0.063(14) 0.056(13) 0.067(15) -0.002(12) -0.001(12) -0.006(11) C2 0.061(13) 0.045(11) 0.055(12) -0.007(10) -0.010(10) -0.015(10) C3 0.023(9) 0.065(13) 0.060(12) -0.008(10) 0.015(8) -0.008(9) C4 0.058(13) 0.060(14) 0.061(15) 0.010(12) 0.003(11) -0.011(11) C5 0.071(15) 0.048(12) 0.050(13) 0.005(10) -0.011(11) -0.006(10) C6 0.069(14) 0.058(13) 0.069(15) 0.004(11) -0.021(12) -0.034(12) C7 0.026(9) 0.054(12) 0.066(13) -0.002(10) -0.009(9) -0.012(8) C8 0.11(2) 0.049(13) 0.054(14) 0.008(11) -0.011(13) 0.007(13) C9 0.052(12) 0.060(13) 0.054(13) -0.007(11) 0.001(10) -0.005(10) C10 0.036(10) 0.047(11) 0.078(15) 0.017(11) -0.002(10) -0.002(9) C11 0.056(12) 0.029(9) 0.048(11) -0.009(8) 0.004(9) 0.000(8) C12 0.071(15) 0.046(12) 0.061(14) 0.007(11) 0.008(12) -0.004(11) C13 0.079(17) 0.062(15) 0.078(17) 0.006(13) -0.021(14) 0.011(13) C14 0.050(12) 0.061(13) 0.067(14) 0.010(11) -0.021(10) -0.019(10) C15 0.070(15) 0.065(14) 0.055(13) -0.007(11) -0.014(11) -0.020(12) C16 0.088(18) 0.066(15) 0.058(15) 0.002(12) -0.015(13) -0.013(13) C17 0.079(16) 0.043(12) 0.074(16) -0.011(11) -0.010(13) -0.009(11) C18 0.072(17) 0.087(19) 0.063(16) -0.014(14) -0.006(13) 0.014(15) C19 0.078(19) 0.14(3) 0.062(17) -0.017(19) -0.003(14) -0.04(2) C20 0.10(2) 0.09(2) 0.10(2) -0.007(17) -0.015(18) -0.056(19) C21 0.087(18) 0.051(13) 0.069(15) 0.002(11) -0.007(13) -0.024(12) C22 0.048(13) 0.062(14) 0.086(17) 0.003(12) 0.010(12) -0.012(11) C23 0.038(10) 0.043(11) 0.070(14) -0.004(10) -0.001(9) -0.013(9) C24 0.067(14) 0.044(11) 0.060(14) 0.007(10) -0.015(11) -0.013(10) C25 0.050(12) 0.038(11) 0.085(17) -0.014(11) -0.005(11) -0.001(9) C26 0.041(11) 0.067(14) 0.061(13) 0.007(11) -0.009(9) -0.025(10) C27 0.056(13) 0.044(12) 0.080(17) 0.011(11) 0.000(12) -0.004(10) C28 0.064(14) 0.023(9) 0.100(19) 0.005(11) -0.001(13) -0.010(9) C29 0.052(14) 0.11(2) 0.061(15) 0.002(14) 0.000(11) -0.017(14) C30 0.12(2) 0.051(14) 0.057(15) 0.003(11) -0.002(15) 0.006(15) C31 0.12(3) 0.13(3) 0.066(19) 0.013(19) 0.013(19) 0.06(2) C32 0.08(2) 0.20(4) 0.061(18) 0.01(2) -0.012(16) -0.05(3) C33 0.17(4) 0.11(3) 0.08(2) -0.025(19) 0.04(2) -0.07(3) C34 0.13(3) 0.09(2) 0.08(2) -0.022(17) 0.006(19) -0.04(2) C35 0.060(14) 0.062(14) 0.082(17) -0.005(12) -0.028(13) -0.009(11) C36 0.049(12) 0.052(13) 0.074(15) -0.004(11) -0.010(11) -0.008(10) C37 0.062(14) 0.046(12) 0.085(18) -0.002(12) 0.014(12) -0.015(11) C38 0.066(14) 0.037(11) 0.087(18) 0.007(11) 0.016(13) -0.011(10) C39 0.026(10) 0.068(15) 0.082(16) -0.004(12) 0.010(10) -0.017(10) C40 0.053(13) 0.069(16) 0.088(18) -0.034(14) 0.007(12) -0.021(12) C41 0.057(13) 0.031(10) 0.099(19) -0.001(11) 0.001(13) 0.007(9) C42 0.049(14) 0.12(2) 0.089(19) -0.024(17) 0.017(13) -0.020(14) _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 S5 2.250(6) . ? Pt1 S6 2.253(5) . ? Pt1 S7 2.259(5) . ? Pt1 S8 2.269(6) . ? Pt2 S1 2.248(5) . ? Pt2 S3 2.252(5) . ? Pt2 S4 2.263(5) . ? Pt2 S2 2.274(5) . ? S1 C2 1.72(2) . ? S2 C3 1.73(2) . ? S3 C6 1.73(2) . ? S4 C7 1.71(2) . ? S5 C10 1.70(2) . ? S6 C11 1.710(19) . ? S7 C14 1.72(2) . ? S8 C15 1.72(2) . ? N1 C1 1.14(3) . ? N2 C4 1.13(3) . ? N3 C5 1.16(3) . ? N4 C8 1.12(3) . ? N5 C9 1.16(3) . ? N6 C12 1.11(3) . ? N7 C13 1.13(3) . ? N8 C16 1.15(3) . ? N9 C17 1.32(3) . ? N9 C21 1.34(3) . ? N9 C22 1.50(3) . ? N10 C30 1.31(3) . ? N10 C34 1.34(3) . ? N10 C35 1.48(3) . ? C1 C2 1.40(3) . ? C2 C3 1.34(3) . ? C3 C4 1.46(3) . ? C5 C6 1.41(3) . ? C6 C7 1.32(3) . ? C7 C8 1.49(3) . ? C9 C10 1.41(3) . ? C10 C11 1.39(3) . ? C11 C12 1.46(3) . ? C13 C14 1.46(3) . ? C14 C15 1.36(3) . ? C15 C16 1.42(3) . ? C17 C18 1.36(3) . ? C17 D17A 0.9302 . ? C18 C19 1.37(4) . ? C18 D18A 0.9221 . ? C19 C20 1.36(4) . ? C19 D19A 0.9256 . ? C20 C21 1.35(4) . ? C20 D20A 0.9309 . ? C21 D21A 0.9395 . ? C22 H22B 0.9700 . ? C22 H22A 0.9700 . ? C22 C23 1.47(3) . ? C23 C24 1.37(3) . ? C23 C28 1.38(3) . ? C24 H24A 0.9300 . ? C24 C25 1.40(3) . ? C25 H25A 0.9300 . ? C25 C26 1.35(3) . ? C26 C27 1.38(3) . ? C26 C29 1.52(3) . ? C27 H27A 0.9300 . ? C27 C28 1.36(3) . ? C28 H28A 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.33(5) . ? C30 D30A 0.9288 . ? C31 C32 1.43(5) . ? C31 D31A 0.9221 . ? C32 C33 1.33(5) . ? C32 D32A 0.9229 . ? C33 C34 1.30(5) . ? C33 D33A 0.9363 . ? C34 D34A 0.9448 . ? C35 H35B 0.9700 . ? C35 H35A 0.9700 . ? C35 C36 1.53(3) . ? C36 C37 1.37(3) . ? C36 C41 1.38(3) . ? C37 H37A 0.9300 . ? C37 C38 1.38(3) . ? C38 H38A 0.9300 . ? C38 C39 1.40(3) . ? C39 C40 1.38(3) . ? C39 C42 1.48(3) . ? C40 H40A 0.9300 . ? C40 C41 1.34(3) . ? C41 H41A 0.9300 . ? C42 H42C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? 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 S5 Pt1 S6 90.15(18) . . ? S5 Pt1 S7 88.85(19) . . ? S6 Pt1 S7 178.9(2) . . ? S5 Pt1 S8 176.0(2) . . ? S6 Pt1 S8 91.10(19) . . ? S7 Pt1 S8 89.93(19) . . ? S1 Pt2 S3 88.56(19) . . ? S1 Pt2 S4 178.00(19) . . ? S3 Pt2 S4 89.62(18) . . ? S1 Pt2 S2 89.81(19) . . ? S3 Pt2 S2 176.31(19) . . ? S4 Pt2 S2 91.97(18) . . ? C2 S1 Pt2 103.6(7) . . ? C3 S2 Pt2 101.5(7) . . ? C6 S3 Pt2 103.0(8) . . ? C7 S4 Pt2 101.9(7) . . ? C10 S5 Pt1 103.7(8) . . ? C11 S6 Pt1 102.4(6) . . ? C14 S7 Pt1 102.1(7) . . ? C15 S8 Pt1 102.9(8) . . ? C17 N9 C21 120(2) . . ? C17 N9 C22 120.6(18) . . ? C21 N9 C22 119.1(18) . . ? C30 N10 C34 121(3) . . ? C30 N10 C35 121(2) . . ? C34 N10 C35 119(2) . . ? N1 C1 C2 176(3) . . ? C3 C2 C1 123(2) . . ? C3 C2 S1 121.5(16) . . ? C1 C2 S1 115.2(16) . . ? C2 C3 C4 122(2) . . ? C2 C3 S2 123.4(17) . . ? C4 C3 S2 114.8(16) . . ? N2 C4 C3 176(3) . . ? N3 C5 C6 178(3) . . ? C7 C6 C5 126(2) . . ? C7 C6 S3 120.7(18) . . ? C5 C6 S3 113.6(17) . . ? C6 C7 C8 121(2) . . ? C6 C7 S4 124.7(18) . . ? C8 C7 S4 114.5(15) . . ? N4 C8 C7 179(3) . . ? N5 C9 C10 177(2) . . ? C11 C10 C9 121.7(19) . . ? C11 C10 S5 120.8(18) . . ? C9 C10 S5 117.4(16) . . ? C10 C11 C12 120.8(18) . . ? C10 C11 S6 123.0(16) . . ? C12 C11 S6 116.2(14) . . ? N6 C12 C11 178(2) . . ? N7 C13 C14 178(3) . . ? C15 C14 C13 123(2) . . ? C15 C14 S7 123.7(17) . . ? C13 C14 S7 113.2(17) . . ? C14 C15 C16 123(2) . . ? C14 C15 S8 120.9(18) . . ? C16 C15 S8 116.2(18) . . ? N8 C16 C15 175(3) . . ? N9 C17 C18 122(2) . . ? N9 C17 D17A 118.1 . . ? C18 C17 D17A 120.0 . . ? C17 C18 C19 119(3) . . ? C17 C18 D18A 119.9 . . ? C19 C18 D18A 120.7 . . ? C20 C19 C18 117(3) . . ? C20 C19 D19A 121.7 . . ? C18 C19 D19A 121.7 . . ? C21 C20 C19 123(3) . . ? C21 C20 D20A 117.7 . . ? C19 C20 D20A 119.0 . . ? N9 C21 C20 118(2) . . ? N9 C21 D21A 120.3 . . ? C20 C21 D21A 121.2 . . ? H22B C22 H22A 107.7 . . ? H22B C22 C23 108.9(12) . . ? H22A C22 C23 108.9(12) . . ? H22B C22 N9 108.9(11) . . ? H22A C22 N9 108.9(11) . . ? C23 C22 N9 113.5(17) . . ? C24 C23 C28 117(2) . . ? C24 C23 C22 121.3(19) . . ? C28 C23 C22 122(2) . . ? H24A C24 C23 120.3(13) . . ? H24A C24 C25 120.3(12) . . ? C23 C24 C25 119.4(19) . . ? H25A C25 C26 118.3(13) . . ? H25A C25 C24 118.3(12) . . ? C26 C25 C24 123(2) . . ? C25 C26 C27 117(2) . . ? C25 C26 C29 122(2) . . ? C27 C26 C29 121(2) . . ? H27A C27 C28 119.7(12) . . ? H27A C27 C26 119.7(13) . . ? C28 C27 C26 121(2) . . ? H28A C28 C27 118.7(12) . . ? H28A C28 C23 118.7(13) . . ? C27 C28 C23 123(2) . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? H29A C29 C26 109.5(14) . . ? H29B C29 C26 109.5(12) . . ? H29C C29 C26 109.5(12) . . ? N10 C30 C31 121(3) . . ? N10 C30 D30A 118.4 . . ? C31 C30 D30A 120.1 . . ? C30 C31 C32 120(3) . . ? C30 C31 D31A 119.5 . . ? C32 C31 D31A 120.4 . . ? C33 C32 C31 113(3) . . ? C33 C32 D32A 123.2 . . ? C31 C32 D32A 123.7 . . ? C34 C33 C32 127(4) . . ? C34 C33 D33A 115.8 . . ? C32 C33 D33A 117.4 . . ? C33 C34 N10 118(3) . . ? C33 C34 D34A 121.4 . . ? N10 C34 D34A 120.7 . . ? H35B C35 H35A 107.9 . . ? H35B C35 N10 109.2(11) . . ? H35A C35 N10 109.2(11) . . ? H35B C35 C36 109.2(12) . . ? H35A C35 C36 109.2(12) . . ? N10 C35 C36 112.0(17) . . ? C37 C36 C41 118(2) . . ? C37 C36 C35 120(2) . . ? C41 C36 C35 122(2) . . ? H37A C37 C36 119.4(14) . . ? H37A C37 C38 119.4(13) . . ? C36 C37 C38 121(2) . . ? H38A C38 C37 120.4(13) . . ? H38A C38 C39 120.4(14) . . ? C37 C38 C39 119(2) . . ? C40 C39 C38 119(2) . . ? C40 C39 C42 122(2) . . ? C38 C39 C42 119(2) . . ? H40A C40 C41 119.7(14) . . ? H40A C40 C39 119.6(14) . . ? C41 C40 C39 121(2) . . ? H41A C41 C40 119.2(14) . . ? H41A C41 C36 119.2(14) . . ? C40 C41 C36 122(2) . . ? H42C C42 H42A 109.5 . . ? H42C C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? H42C C42 C39 109.7(13) . . ? H42A C42 C39 109.7(14) . . ? H42B C42 C39 109.0(12) . . ? 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 S3 Pt2 S1 C2 -173.4(8) . . . . ? S4 Pt2 S1 C2 -149(6) . . . . ? S2 Pt2 S1 C2 3.3(8) . . . . ? S1 Pt2 S2 C3 -3.6(6) . . . . ? S3 Pt2 S2 C3 60(3) . . . . ? S4 Pt2 S2 C3 175.5(6) . . . . ? S1 Pt2 S3 C6 179.4(8) . . . . ? S4 Pt2 S3 C6 0.2(8) . . . . ? S2 Pt2 S3 C6 116(3) . . . . ? S1 Pt2 S4 C7 -24(6) . . . . ? S3 Pt2 S4 C7 0.0(6) . . . . ? S2 Pt2 S4 C7 -176.7(6) . . . . ? S6 Pt1 S5 C10 2.0(7) . . . . ? S7 Pt1 S5 C10 -178.5(7) . . . . ? S8 Pt1 S5 C10 -106(3) . . . . ? S5 Pt1 S6 C11 -2.3(7) . . . . ? S7 Pt1 S6 C11 -29(10) . . . . ? S8 Pt1 S6 C11 173.9(7) . . . . ? S5 Pt1 S7 C14 174.2(7) . . . . ? S6 Pt1 S7 C14 -159(10) . . . . ? S8 Pt1 S7 C14 -2.0(7) . . . . ? S5 Pt1 S8 C15 -67(3) . . . . ? S6 Pt1 S8 C15 -175.8(8) . . . . ? S7 Pt1 S8 C15 4.7(8) . . . . ? N1 C1 C2 C3 134(35) . . . . ? N1 C1 C2 S1 -46(37) . . . . ? Pt2 S1 C2 C3 -2.3(19) . . . . ? Pt2 S1 C2 C1 178.3(16) . . . . ? C1 C2 C3 C4 -1(3) . . . . ? S1 C2 C3 C4 179.2(15) . . . . ? C1 C2 C3 S2 178.5(17) . . . . ? S1 C2 C3 S2 -1(3) . . . . ? Pt2 S2 C3 C2 3.5(18) . . . . ? Pt2 S2 C3 C4 -176.6(13) . . . . ? C2 C3 C4 N2 -96(40) . . . . ? S2 C3 C4 N2 85(40) . . . . ? N3 C5 C6 C7 -53(98) . . . . ? N3 C5 C6 S3 127(97) . . . . ? Pt2 S3 C6 C7 -0.5(19) . . . . ? Pt2 S3 C6 C5 179.4(15) . . . . ? C5 C6 C7 C8 2(3) . . . . ? S3 C6 C7 C8 -178.4(17) . . . . ? C5 C6 C7 S4 -179.3(17) . . . . ? S3 C6 C7 S4 1(3) . . . . ? Pt2 S4 C7 C6 -0.3(19) . . . . ? Pt2 S4 C7 C8 178.7(15) . . . . ? C6 C7 C8 N4 104(100) . . . . ? S4 C7 C8 N4 -75(100) . . . . ? N5 C9 C10 C11 -164(50) . . . . ? N5 C9 C10 S5 20(51) . . . . ? Pt1 S5 C10 C11 -1.1(18) . . . . ? Pt1 S5 C10 C9 175.2(15) . . . . ? C9 C10 C11 C12 3(3) . . . . ? S5 C10 C11 C12 179.1(16) . . . . ? C9 C10 C11 S6 -177.1(16) . . . . ? S5 C10 C11 S6 -1(3) . . . . ? Pt1 S6 C11 C10 2.5(19) . . . . ? Pt1 S6 C11 C12 -177.7(15) . . . . ? C10 C11 C12 N6 -139(66) . . . . ? S6 C11 C12 N6 41(67) . . . . ? N7 C13 C14 C15 -57(100) . . . . ? N7 C13 C14 S7 115(100) . . . . ? Pt1 S7 C14 C15 -2(2) . . . . ? Pt1 S7 C14 C13 -174.2(16) . . . . ? C13 C14 C15 C16 -8(4) . . . . ? S7 C14 C15 C16 -178.7(19) . . . . ? C13 C14 C15 S8 178.4(18) . . . . ? S7 C14 C15 S8 7(3) . . . . ? Pt1 S8 C15 C14 -8(2) . . . . ? Pt1 S8 C15 C16 177.9(17) . . . . ? C14 C15 C16 N8 84(33) . . . . ? S8 C15 C16 N8 -101(32) . . . . ? C21 N9 C17 C18 4(4) . . . . ? C22 N9 C17 C18 -180(2) . . . . ? N9 C17 C18 C19 -4(4) . . . . ? C17 C18 C19 C20 3(4) . . . . ? C18 C19 C20 C21 -3(5) . . . . ? C17 N9 C21 C20 -3(4) . . . . ? C22 N9 C21 C20 -179(2) . . . . ? C19 C20 C21 N9 3(4) . . . . ? C17 N9 C22 H22B 148.2(16) . . . . ? C21 N9 C22 H22B -35.8(19) . . . . ? C17 N9 C22 H22A 31(2) . . . . ? C21 N9 C22 H22A -152.9(15) . . . . ? C17 N9 C22 C23 -90(2) . . . . ? C21 N9 C22 C23 86(2) . . . . ? H22B C22 C23 C24 -154.8(16) . . . . ? H22A C22 C23 C24 -38(2) . . . . ? N9 C22 C23 C24 84(2) . . . . ? H22B C22 C23 C28 25(2) . . . . ? H22A C22 C23 C28 142.0(16) . . . . ? N9 C22 C23 C28 -97(2) . . . . ? C28 C23 C24 H24A 179.5(13) . . . . ? C22 C23 C24 H24A -1(2) . . . . ? C28 C23 C24 C25 -1(3) . . . . ? C22 C23 C24 C25 179.1(19) . . . . ? H24A C24 C25 H25A -2.0(14) . . . . ? C23 C24 C25 H25A 178.1(14) . . . . ? H24A C24 C25 C26 178.1(15) . . . . ? C23 C24 C25 C26 -2(3) . . . . ? H25A C25 C26 C27 -177.5(13) . . . . ? C24 C25 C26 C27 2(3) . . . . ? H25A C25 C26 C29 4(2) . . . . ? C24 C25 C26 C29 -176(2) . . . . ? C25 C26 C27 H27A 179.4(13) . . . . ? C29 C26 C27 H27A -2(2) . . . . ? C25 C26 C27 C28 -1(3) . . . . ? C29 C26 C27 C28 178(2) . . . . ? H27A C27 C28 H28A -2.0(15) . . . . ? C26 C27 C28 H28A 178.1(14) . . . . ? H27A C27 C28 C23 178.2(15) . . . . ? C26 C27 C28 C23 -2(3) . . . . ? C24 C23 C28 H28A -177.5(13) . . . . ? C22 C23 C28 H28A 3(2) . . . . ? C24 C23 C28 C27 2(3) . . . . ? C22 C23 C28 C27 -177(2) . . . . ? C25 C26 C29 H29A -2(2) . . . . ? C27 C26 C29 H29A 179.9(15) . . . . ? C25 C26 C29 H29B -121.6(17) . . . . ? C27 C26 C29 H29B 60(2) . . . . ? C25 C26 C29 H29C 118.4(18) . . . . ? C27 C26 C29 H29C -60(2) . . . . ? C34 N10 C30 C31 -1(4) . . . . ? C35 N10 C30 C31 -177(2) . . . . ? N10 C30 C31 C32 2(5) . . . . ? C30 C31 C32 C33 -3(5) . . . . ? C31 C32 C33 C34 4(6) . . . . ? C32 C33 C34 N10 -3(6) . . . . ? C30 N10 C34 C33 1(4) . . . . ? C35 N10 C34 C33 178(3) . . . . ? C30 N10 C35 H35B -145.0(17) . . . . ? C34 N10 C35 H35B 38(2) . . . . ? C30 N10 C35 H35A -27(2) . . . . ? C34 N10 C35 H35A 155.9(19) . . . . ? C30 N10 C35 C36 94(2) . . . . ? C34 N10 C35 C36 -83(3) . . . . ? H35B C35 C36 C37 154.5(17) . . . . ? H35A C35 C36 C37 37(2) . . . . ? N10 C35 C36 C37 -84(3) . . . . ? H35B C35 C36 C41 -27(2) . . . . ? H35A C35 C36 C41 -144.8(18) . . . . ? N10 C35 C36 C41 94(2) . . . . ? C41 C36 C37 H37A -177.1(15) . . . . ? C35 C36 C37 H37A 1(2) . . . . ? C41 C36 C37 C38 3(3) . . . . ? C35 C36 C37 C38 -179(2) . . . . ? H37A C37 C38 H38A -1.6(15) . . . . ? C36 C37 C38 H38A 178.4(15) . . . . ? H37A C37 C38 C39 178.4(14) . . . . ? C36 C37 C38 C39 -2(3) . . . . ? H38A C38 C39 C40 180.0(13) . . . . ? C37 C38 C39 C40 0(3) . . . . ? H38A C38 C39 C42 -1(2) . . . . ? C37 C38 C39 C42 178(2) . . . . ? C38 C39 C40 H40A -179.8(13) . . . . ? C42 C39 C40 H40A 2(2) . . . . ? C38 C39 C40 C41 0(3) . . . . ? C42 C39 C40 C41 -178(2) . . . . ? H40A C40 C41 H41A 1.1(15) . . . . ? C39 C40 C41 H41A -178.9(14) . . . . ? H40A C40 C41 C36 -178.8(16) . . . . ? C39 C40 C41 C36 1(4) . . . . ? C37 C36 C41 H41A 177.4(15) . . . . ? C35 C36 C41 H41A -1(3) . . . . ? C37 C36 C41 C40 -3(3) . . . . ? C35 C36 C41 C40 179(2) . . . . ? C40 C39 C42 H42C 119.0(17) . . . . ? C38 C39 C42 H42C -59.5(19) . . . . ? C40 C39 C42 H42A -1(2) . . . . ? C38 C39 C42 H42A -179.8(15) . . . . ? C40 C39 C42 H42B -121.2(17) . . . . ? C38 C39 C42 H42B 60.3(19) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.655 _refine_diff_density_min -4.424 _refine_diff_density_rms 0.258 _database_code_depnum_ccdc_archive 'CCDC 935814' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H14 N5 Pt S4' _chemical_formula_weight 659.70 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3203(10) _cell_length_b 12.2816(16) _cell_length_c 26.904(4) _cell_angle_alpha 88.500(4) _cell_angle_beta 86.731(4) _cell_angle_gamma 75.421(4) _cell_volume 2337.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2229 _cell_measurement_theta_min 3.1000 _cell_measurement_theta_max 23.2810 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 6.380 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.309 _exptl_absorpt_correction_T_max 0.338 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41038 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_unetI/netI 0.0630 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.76 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8657 _reflns_number_gt 6940 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0565P)^2^+434.5350P] 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 8657 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1495 _refine_ls_R_factor_gt 0.1286 _refine_ls_wR_factor_ref 0.3400 _refine_ls_wR_factor_gt 0.3326 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.43737(17) 0.27521(10) 0.23441(5) 0.0436(4) Uani 1 1 d . . . Pt2 Pt 0.94825(17) 0.26999(10) 0.27088(5) 0.0411(4) Uani 1 1 d . . . S1 S 0.8569(15) 0.4170(7) 0.3225(3) 0.058(2) Uani 1 1 d . . . S2 S 1.0426(13) 0.1536(7) 0.3367(3) 0.051(2) Uani 1 1 d . . . S3 S 0.8721(11) 0.3897(7) 0.2068(4) 0.049(2) Uani 1 1 d . . . S4 S 1.0429(11) 0.1267(6) 0.2167(3) 0.0445(18) Uani 1 1 d . . . S5 S 0.3660(12) 0.3954(7) 0.2981(4) 0.052(2) Uani 1 1 d . . . S6 S 0.5344(12) 0.1310(6) 0.2878(3) 0.0480(19) Uani 1 1 d . . . S7 S 0.3348(14) 0.4226(7) 0.1821(4) 0.057(2) Uani 1 1 d . . . S8 S 0.5254(16) 0.1589(7) 0.1682(4) 0.064(3) Uani 1 1 d . . . N1 N 0.866(6) 0.502(3) 0.4497(14) 0.087(12) Uani 1 1 d . . . N2 N 1.117(7) 0.161(4) 0.4709(15) 0.098(13) Uani 1 1 d . . . N3 N 0.856(5) 0.406(3) 0.0707(14) 0.086(12) Uani 1 1 d . . . N4 N 1.084(7) 0.063(3) 0.0848(14) 0.103(15) Uani 1 1 d . . . N5 N 0.419(7) 0.414(3) 0.4322(15) 0.099(14) Uani 1 1 d . . . N6 N 0.623(7) 0.067(3) 0.4191(14) 0.095(14) Uani 1 1 d . . . N7 N 0.327(6) 0.501(4) 0.0517(15) 0.101(15) Uani 1 1 d . . . N8 N 0.574(7) 0.162(4) 0.0327(15) 0.108(15) Uani 1 1 d . . . N9 N 0.111(4) 0.781(2) 0.4296(10) 0.048(6) Uani 1 1 d . . . N10 N 0.624(5) 0.779(2) 0.0686(11) 0.063(8) Uani 1 1 d . . . C1 C 0.885(6) 0.438(4) 0.4195(18) 0.077(12) Uani 1 1 d . . . C2 C 0.930(6) 0.359(3) 0.3799(14) 0.062(10) Uani 1 1 d . . . C3 C 1.005(4) 0.249(3) 0.3856(14) 0.051(8) Uani 1 1 d . . . C4 C 1.066(5) 0.201(4) 0.4349(16) 0.062(10) Uani 1 1 d . . . C5 C 0.881(5) 0.360(3) 0.1093(14) 0.057(9) Uani 1 1 d . . . C6 C 0.932(6) 0.300(4) 0.1558(16) 0.076(13) Uani 1 1 d . . . C7 C 0.999(4) 0.195(3) 0.1619(12) 0.047(8) Uani 1 1 d . . . C8 C 1.048(7) 0.117(3) 0.1170(16) 0.083(15) Uani 1 1 d . . . C9 C 0.425(5) 0.364(3) 0.3955(15) 0.058(9) Uani 1 1 d . . . C10 C 0.428(4) 0.311(3) 0.3489(16) 0.063(11) Uani 1 1 d . . . C11 C 0.506(5) 0.197(3) 0.3439(12) 0.054(9) Uani 1 1 d . . . C12 C 0.565(7) 0.125(3) 0.3870(17) 0.077(13) Uani 1 1 d . . . C13 C 0.347(7) 0.442(4) 0.0834(19) 0.083(14) Uani 1 1 d . . . C14 C 0.391(5) 0.360(3) 0.1246(14) 0.057(9) Uani 1 1 d . . . C15 C 0.482(7) 0.250(3) 0.1187(15) 0.078(13) Uani 1 1 d . . . C16 C 0.524(8) 0.201(3) 0.0720(16) 0.083(15) Uani 1 1 d . . . C17 C 0.229(6) 0.687(3) 0.4435(16) 0.071(11) Uani 1 1 d . . . H17A H 0.1946 0.6195 0.4396 0.085 Uiso 1 1 calc R . . C18 C 0.394(6) 0.682(4) 0.4627(17) 0.078(13) Uani 1 1 d . . . H18A H 0.4695 0.6123 0.4724 0.094 Uiso 1 1 calc R . . C19 C 0.457(7) 0.781(6) 0.4686(17) 0.099(18) Uani 1 1 d . . . H19A H 0.5724 0.7797 0.4816 0.119 Uiso 1 1 calc R . . C20 C 0.338(8) 0.875(4) 0.454(2) 0.092(16) Uani 1 1 d . . . H20A H 0.3697 0.9425 0.4578 0.111 Uiso 1 1 calc R . . C21 C 0.170(7) 0.877(4) 0.4339(17) 0.080(13) Uani 1 1 d . . . H21A H 0.0948 0.9448 0.4229 0.096 Uiso 1 1 calc R . . C22 C -0.066(5) 0.784(3) 0.4075(14) 0.061(10) Uani 1 1 d . . . H22A H -0.1559 0.8540 0.4168 0.073 Uiso 1 1 calc R . . H22B H -0.1147 0.7230 0.4217 0.073 Uiso 1 1 calc R . . C23 C -0.056(4) 0.775(3) 0.3515(14) 0.049(8) Uani 1 1 d . . . C24 C 0.004(5) 0.674(3) 0.3290(15) 0.061(10) Uani 1 1 d . . . H24A H 0.0372 0.6083 0.3477 0.073 Uiso 1 1 calc R . . C25 C 0.016(4) 0.672(3) 0.2769(15) 0.057(10) Uani 1 1 d . . . H25A H 0.0591 0.6025 0.2617 0.068 Uiso 1 1 calc R . . C26 C -0.031(5) 0.762(3) 0.2480(14) 0.055(9) Uani 1 1 d . . . C27 C -0.094(5) 0.864(3) 0.2723(18) 0.067(12) Uani 1 1 d . . . H27A H -0.1369 0.9297 0.2536 0.081 Uiso 1 1 calc R . . C28 C -0.096(5) 0.871(3) 0.3225(15) 0.057(9) Uani 1 1 d . . . H28A H -0.1257 0.9408 0.3375 0.068 Uiso 1 1 calc R . . C29 C -0.028(5) 0.756(4) 0.1909(14) 0.080(13) Uani 1 1 d . . . H29A H 0.0200 0.6795 0.1808 0.119 Uiso 1 1 calc R . . H29B H 0.0510 0.8012 0.1763 0.119 Uiso 1 1 calc R . . H29C H -0.1545 0.7841 0.1801 0.119 Uiso 1 1 calc R . . C30 C 0.733(7) 0.685(4) 0.0532(15) 0.077(13) Uani 1 1 d . . . H30A H 0.6910 0.6202 0.0559 0.093 Uiso 1 1 calc R . . C31 C 0.908(10) 0.681(6) 0.033(2) 0.13(3) Uani 1 1 d . . . H31A H 0.9831 0.6109 0.0235 0.157 Uiso 1 1 calc R . . C32 C 0.982(8) 0.774(7) 0.0265(19) 0.103(19) Uani 1 1 d . . . H32A H 1.1032 0.7717 0.0132 0.123 Uiso 1 1 calc R . . C33 C 0.854(10) 0.867(5) 0.0420(18) 0.104(19) Uani 1 1 d . . . H33A H 0.8931 0.9339 0.0383 0.125 Uiso 1 1 calc R . . C34 C 0.678(9) 0.878(5) 0.062(2) 0.101(17) Uani 1 1 d . . . H34A H 0.5989 0.9477 0.0709 0.121 Uiso 1 1 calc R . . C35 C 0.440(6) 0.782(3) 0.0938(16) 0.071(11) Uani 1 1 d . . . H35A H 0.3932 0.7205 0.0821 0.085 Uiso 1 1 calc R . . H35B H 0.3509 0.8519 0.0857 0.085 Uiso 1 1 calc R . . C36 C 0.456(5) 0.772(3) 0.1493(16) 0.065(10) Uani 1 1 d . . . C37 C 0.509(5) 0.672(3) 0.1724(17) 0.064(11) Uani 1 1 d . . . H37A H 0.5390 0.6067 0.1535 0.077 Uiso 1 1 calc R . . C38 C 0.519(6) 0.663(3) 0.2238(15) 0.061(10) Uani 1 1 d . . . H38A H 0.5604 0.5923 0.2389 0.073 Uiso 1 1 calc R . . C39 C 0.466(4) 0.762(3) 0.2535(15) 0.055(9) Uani 1 1 d . . . C40 C 0.423(4) 0.863(3) 0.2280(18) 0.066(12) Uani 1 1 d . . . H40A H 0.4013 0.9287 0.2461 0.079 Uiso 1 1 calc R . . C41 C 0.410(5) 0.871(3) 0.1778(16) 0.059(10) Uani 1 1 d . . . H41A H 0.3720 0.9408 0.1624 0.071 Uiso 1 1 calc R . . C42 C 0.473(5) 0.751(4) 0.3072(16) 0.075(13) Uani 1 1 d . . . H42A H 0.4343 0.8239 0.3219 0.113 Uiso 1 1 calc R . . H42B H 0.5991 0.7146 0.3159 0.113 Uiso 1 1 calc R . . H42C H 0.3885 0.7062 0.3194 0.113 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 0.0375(7) 0.0358(6) 0.0594(8) 0.0039(5) -0.0119(6) -0.0114(5) Pt2 0.0363(7) 0.0351(6) 0.0529(8) 0.0008(5) -0.0023(5) -0.0108(5) S1 0.082(7) 0.035(4) 0.052(5) 0.003(4) -0.014(5) -0.002(4) S2 0.053(5) 0.035(4) 0.061(5) 0.002(4) 0.002(4) -0.005(4) S3 0.031(4) 0.044(4) 0.069(6) -0.004(4) -0.006(4) 0.000(3) S4 0.038(4) 0.033(4) 0.059(5) -0.005(3) 0.000(4) -0.002(3) S5 0.045(5) 0.032(4) 0.073(6) 0.007(4) -0.011(4) 0.005(3) S6 0.052(5) 0.029(4) 0.060(5) 0.001(3) -0.010(4) -0.004(3) S7 0.070(6) 0.038(4) 0.062(6) 0.006(4) -0.014(5) -0.008(4) S8 0.086(7) 0.039(5) 0.067(6) 0.001(4) -0.014(5) -0.016(5) N1 0.12(3) 0.07(2) 0.07(2) -0.02(2) 0.01(2) -0.02(2) N2 0.13(4) 0.10(3) 0.06(2) 0.00(2) 0.00(2) -0.01(3) N3 0.09(3) 0.06(2) 0.08(3) -0.003(19) 0.00(2) 0.034(19) N4 0.17(5) 0.07(2) 0.06(2) -0.02(2) 0.03(3) -0.01(3) N5 0.13(4) 0.07(2) 0.07(3) -0.01(2) 0.01(2) 0.02(2) N6 0.14(4) 0.06(2) 0.06(2) 0.023(19) -0.01(2) 0.01(2) N7 0.10(3) 0.10(3) 0.07(3) 0.02(2) 0.00(2) 0.03(2) N8 0.12(4) 0.12(4) 0.06(3) -0.01(2) 0.00(2) 0.00(3) N9 0.048(16) 0.043(15) 0.049(16) -0.012(12) 0.000(12) -0.004(12) N10 0.09(2) 0.043(17) 0.053(18) 0.002(14) -0.011(17) -0.001(16) C1 0.06(3) 0.08(3) 0.08(3) 0.02(3) 0.00(2) 0.00(2) C2 0.09(3) 0.05(2) 0.05(2) -0.002(17) -0.02(2) -0.03(2) C3 0.021(14) 0.051(19) 0.08(2) -0.014(17) 0.016(15) -0.004(13) C4 0.05(2) 0.08(3) 0.06(3) 0.01(2) -0.013(18) -0.017(19) C5 0.06(2) 0.038(18) 0.06(2) 0.014(17) -0.006(18) 0.000(16) C6 0.09(3) 0.09(3) 0.07(3) 0.03(2) -0.04(2) -0.06(3) C7 0.018(14) 0.07(2) 0.048(19) 0.013(16) -0.008(12) -0.002(14) C8 0.12(4) 0.04(2) 0.06(3) 0.008(19) 0.00(2) 0.03(2) C9 0.05(2) 0.06(2) 0.07(3) -0.02(2) 0.004(18) -0.014(17) C10 0.019(15) 0.06(2) 0.09(3) 0.03(2) 0.011(16) 0.006(15) C11 0.07(2) 0.036(17) 0.044(19) -0.005(14) 0.016(17) 0.002(16) C12 0.11(4) 0.05(2) 0.08(3) -0.01(2) 0.03(3) -0.03(2) C13 0.09(3) 0.05(2) 0.09(3) 0.00(2) -0.02(3) 0.02(2) C14 0.07(2) 0.048(19) 0.06(2) 0.015(17) -0.026(18) -0.017(17) C15 0.11(4) 0.06(2) 0.05(2) -0.015(19) 0.01(2) 0.00(2) C16 0.13(4) 0.06(2) 0.05(2) 0.008(19) -0.02(3) 0.00(3) C17 0.09(3) 0.029(17) 0.09(3) -0.012(18) -0.01(2) -0.004(18) C18 0.07(3) 0.07(3) 0.08(3) 0.00(2) 0.00(2) 0.01(2) C19 0.07(3) 0.17(6) 0.06(3) 0.00(3) -0.02(2) -0.03(4) C20 0.11(4) 0.08(3) 0.11(4) 0.01(3) -0.03(3) -0.06(3) C21 0.09(3) 0.08(3) 0.07(3) 0.01(2) -0.01(3) -0.03(3) C22 0.05(2) 0.06(2) 0.07(2) 0.008(18) -0.006(18) -0.003(17) C23 0.037(17) 0.031(16) 0.08(2) -0.005(15) 0.006(16) -0.002(13) C24 0.07(2) 0.041(19) 0.07(3) 0.015(17) -0.03(2) -0.010(17) C25 0.036(17) 0.034(17) 0.09(3) -0.014(18) 0.019(18) 0.003(13) C26 0.042(19) 0.07(2) 0.06(2) 0.017(19) -0.013(16) -0.030(18) C27 0.036(19) 0.05(2) 0.11(4) 0.01(2) 0.01(2) 0.007(15) C28 0.06(2) 0.031(16) 0.07(3) -0.002(16) -0.001(19) 0.003(15) C29 0.05(2) 0.12(4) 0.06(2) -0.01(2) 0.015(19) 0.00(2) C30 0.11(4) 0.06(2) 0.06(3) 0.009(19) 0.00(2) 0.00(2) C31 0.14(6) 0.13(5) 0.07(4) 0.01(3) -0.01(4) 0.07(5) C32 0.09(4) 0.16(6) 0.06(3) 0.00(4) 0.01(3) -0.04(4) C33 0.16(6) 0.11(4) 0.06(3) 0.00(3) 0.01(3) -0.06(4) C34 0.13(5) 0.09(4) 0.09(4) -0.03(3) 0.01(3) -0.04(3) C35 0.07(3) 0.06(2) 0.09(3) 0.00(2) -0.03(2) -0.02(2) C36 0.05(2) 0.05(2) 0.08(3) 0.00(2) -0.01(2) -0.004(18) C37 0.06(2) 0.033(18) 0.09(3) 0.002(18) 0.02(2) -0.009(16) C38 0.07(3) 0.026(16) 0.08(3) 0.006(16) -0.01(2) -0.006(16) C39 0.019(15) 0.06(2) 0.08(3) -0.004(19) -0.004(15) -0.006(14) C40 0.025(16) 0.06(2) 0.11(4) -0.04(2) 0.002(19) -0.008(16) C41 0.040(19) 0.030(16) 0.10(3) -0.014(18) 0.007(19) 0.009(14) C42 0.029(18) 0.11(3) 0.08(3) -0.04(3) 0.010(18) -0.002(19) _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 S5 2.243(9) . ? Pt1 S6 2.249(8) . ? Pt1 S7 2.264(9) . ? Pt1 S8 2.273(10) . ? Pt2 S3 2.239(9) . ? Pt2 S1 2.248(9) . ? Pt2 S4 2.260(8) . ? Pt2 S2 2.272(9) . ? S1 C2 1.74(4) . ? S2 C3 1.75(3) . ? S3 C6 1.74(5) . ? S4 C7 1.68(3) . ? S5 C10 1.70(4) . ? S6 C11 1.71(3) . ? S7 C14 1.73(4) . ? S8 C15 1.71(4) . ? N1 C1 1.12(6) . ? N2 C4 1.12(5) . ? N3 C5 1.17(5) . ? N4 C8 1.09(5) . ? N5 C9 1.17(5) . ? N6 C12 1.14(5) . ? N7 C13 1.10(5) . ? N8 C16 1.17(5) . ? N9 C17 1.32(4) . ? N9 C21 1.36(5) . ? N9 C22 1.44(4) . ? N10 C30 1.28(5) . ? N10 C34 1.38(6) . ? N10 C35 1.47(5) . ? C1 C2 1.42(6) . ? C2 C3 1.33(5) . ? C3 C4 1.49(5) . ? C5 C6 1.45(5) . ? C6 C7 1.28(5) . ? C7 C8 1.53(5) . ? C9 C10 1.43(6) . ? C10 C11 1.37(5) . ? C11 C12 1.46(6) . ? C13 C14 1.47(6) . ? C14 C15 1.35(5) . ? C15 C16 1.39(6) . ? C17 C18 1.33(6) . ? C17 H17A 0.9300 . ? C18 C19 1.42(7) . ? C18 H18A 0.9300 . ? C19 C20 1.33(7) . ? C19 H19A 0.9300 . ? C20 C21 1.36(6) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.51(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.35(5) . ? C23 C28 1.37(5) . ? C24 C25 1.40(5) . ? C24 H24A 0.9300 . ? C25 C26 1.32(5) . ? C25 H25A 0.9300 . ? C26 C27 1.39(5) . ? C26 C29 1.54(5) . ? C27 C28 1.35(6) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.34(8) . ? C30 H30A 0.9300 . ? C31 C32 1.39(9) . ? C31 H31A 0.9300 . ? C32 C33 1.35(8) . ? C32 H32A 0.9300 . ? C33 C34 1.34(8) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.50(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.34(5) . ? C36 C41 1.41(5) . ? C37 C38 1.39(5) . ? C37 H37A 0.9300 . ? C38 C39 1.43(5) . ? C38 H38A 0.9300 . ? C39 C40 1.37(5) . ? C39 C42 1.45(6) . ? C40 C41 1.36(6) . ? C40 H40A 0.9300 . ? C41 H41A 0.9300 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? 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 S5 Pt1 S6 90.3(3) . . ? S5 Pt1 S7 88.5(3) . . ? S6 Pt1 S7 178.6(4) . . ? S5 Pt1 S8 176.2(4) . . ? S6 Pt1 S8 91.2(3) . . ? S7 Pt1 S8 90.1(3) . . ? S3 Pt2 S1 88.6(3) . . ? S3 Pt2 S4 89.5(3) . . ? S1 Pt2 S4 177.8(3) . . ? S3 Pt2 S2 176.1(3) . . ? S1 Pt2 S2 90.1(3) . . ? S4 Pt2 S2 91.7(3) . . ? C2 S1 Pt2 103.4(13) . . ? C3 S2 Pt2 101.4(13) . . ? C6 S3 Pt2 102.1(14) . . ? C7 S4 Pt2 101.3(13) . . ? C10 S5 Pt1 103.4(15) . . ? C11 S6 Pt1 102.3(12) . . ? C14 S7 Pt1 101.6(12) . . ? C15 S8 Pt1 102.5(13) . . ? C17 N9 C21 116(4) . . ? C17 N9 C22 123(3) . . ? C21 N9 C22 121(3) . . ? C30 N10 C34 121(4) . . ? C30 N10 C35 121(4) . . ? C34 N10 C35 119(4) . . ? N1 C1 C2 173(5) . . ? C3 C2 C1 125(4) . . ? C3 C2 S1 121(3) . . ? C1 C2 S1 114(3) . . ? C2 C3 C4 121(3) . . ? C2 C3 S2 124(3) . . ? C4 C3 S2 116(3) . . ? N2 C4 C3 177(5) . . ? N3 C5 C6 175(4) . . ? C7 C6 C5 127(4) . . ? C7 C6 S3 121(3) . . ? C5 C6 S3 112(3) . . ? C6 C7 C8 120(3) . . ? C6 C7 S4 126(3) . . ? C8 C7 S4 113(3) . . ? N4 C8 C7 179(6) . . ? N5 C9 C10 176(4) . . ? C11 C10 C9 121(3) . . ? C11 C10 S5 121(3) . . ? C9 C10 S5 118(3) . . ? C10 C11 C12 121(3) . . ? C10 C11 S6 123(3) . . ? C12 C11 S6 116(3) . . ? N6 C12 C11 175(5) . . ? N7 C13 C14 175(5) . . ? C15 C14 C13 124(4) . . ? C15 C14 S7 124(3) . . ? C13 C14 S7 112(3) . . ? C14 C15 C16 122(4) . . ? C14 C15 S8 122(3) . . ? C16 C15 S8 115(3) . . ? N8 C16 C15 174(6) . . ? N9 C17 C18 124(4) . . ? N9 C17 H17A 118.0 . . ? C18 C17 H17A 118.0 . . ? C17 C18 C19 121(4) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C20 C19 C18 115(4) . . ? C20 C19 H19A 122.7 . . ? C18 C19 H19A 122.7 . . ? C19 C20 C21 123(5) . . ? C19 C20 H20A 118.4 . . ? C21 C20 H20A 118.4 . . ? N9 C21 C20 121(4) . . ? N9 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? N9 C22 C23 116(3) . . ? N9 C22 H22A 108.4 . . ? C23 C22 H22A 108.4 . . ? N9 C22 H22B 108.4 . . ? C23 C22 H22B 108.4 . . ? H22A C22 H22B 107.4 . . ? C24 C23 C28 119(4) . . ? C24 C23 C22 121(3) . . ? C28 C23 C22 120(3) . . ? C23 C24 C25 118(3) . . ? C23 C24 H24A 120.8 . . ? C25 C24 H24A 120.8 . . ? C26 C25 C24 124(3) . . ? C26 C25 H25A 118.0 . . ? C24 C25 H25A 118.0 . . ? C25 C26 C27 116(4) . . ? C25 C26 C29 123(4) . . ? C27 C26 C29 121(4) . . ? C28 C27 C26 122(3) . . ? C28 C27 H27A 119.2 . . ? C26 C27 H27A 119.2 . . ? C27 C28 C23 121(3) . . ? C27 C28 H28A 119.6 . . ? C23 C28 H28A 119.6 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N10 C30 C31 121(5) . . ? N10 C30 H30A 119.5 . . ? C31 C30 H30A 119.5 . . ? C30 C31 C32 124(5) . . ? C30 C31 H31A 118.1 . . ? C32 C31 H31A 118.1 . . ? C33 C32 C31 110(5) . . ? C33 C32 H32A 124.9 . . ? C31 C32 H32A 124.9 . . ? C34 C33 C32 129(6) . . ? C34 C33 H33A 115.5 . . ? C32 C33 H33A 115.5 . . ? C33 C34 N10 115(5) . . ? C33 C34 H34A 122.6 . . ? N10 C34 H34A 122.6 . . ? N10 C35 C36 111(3) . . ? N10 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? N10 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C37 C36 C41 119(4) . . ? C37 C36 C35 122(4) . . ? C41 C36 C35 119(4) . . ? C36 C37 C38 122(4) . . ? C36 C37 H37A 119.1 . . ? C38 C37 H37A 119.1 . . ? C37 C38 C39 120(3) . . ? C37 C38 H38A 120.2 . . ? C39 C38 H38A 120.2 . . ? C40 C39 C38 116(4) . . ? C40 C39 C42 125(4) . . ? C38 C39 C42 119(4) . . ? C41 C40 C39 123(3) . . ? C41 C40 H40A 118.4 . . ? C39 C40 H40A 118.4 . . ? C40 C41 C36 119(4) . . ? C40 C41 H41A 120.3 . . ? C36 C41 H41A 120.3 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 5.032 _refine_diff_density_min -8.593 _refine_diff_density_rms 0.417 _database_code_depnum_ccdc_archive 'CCDC 935815'