# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Juan Fornies' _publ_contact_author_address ; Facultad de Ciencias Zaragoza 50009 ; _publ_contact_author_email juan.fornies@unizar.es loop_ _publ_author_name J.Fornies V.Sicilia data_1 _database_code_depnum_ccdc_archive 'CCDC 798308' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 N2 Pt S2' _chemical_formula_weight 519.54 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 8.9315(5) _cell_length_b 27.8009(7) _cell_length_c 7.7791(4) _cell_angle_alpha 90.00 _cell_angle_beta 122.470(8) _cell_angle_gamma 90.00 _cell_volume 1629.62(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8062 _cell_measurement_theta_min 3.7874 _cell_measurement_theta_max 28.6875 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 8.866 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1380 _exptl_absorpt_correction_T_max 0.4422 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 16.0655 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8221 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 28.81 _reflns_number_total 3232 _reflns_number_gt 3142 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+4.7995P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(8) _refine_ls_number_reflns 3232 _refine_ls_number_parameters 208 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0207 _refine_ls_R_factor_gt 0.0199 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0516 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.08594(6) 0.623260(4) 0.29920(7) 0.01560(6) Uani 1 1 d . . . S1 S 0.26296(17) 0.68080(4) 0.2759(2) 0.0212(3) Uani 1 1 d . . . S2 S 0.37250(19) 0.58997(4) 0.4769(2) 0.0231(3) Uani 1 1 d . . . N1 N -0.1603(6) 0.65267(15) 0.1362(7) 0.0224(9) Uani 1 1 d . . . N2 N 0.6074(6) 0.65311(14) 0.4973(7) 0.0177(8) Uani 1 1 d . . . C1 C -0.0522(6) 0.56867(15) 0.3266(7) 0.0110(8) Uani 1 1 d . . . C2 C 0.0110(8) 0.52762(18) 0.4298(8) 0.0205(10) Uani 1 1 d . . . H2 H 0.1356 0.5226 0.5103 0.025 Uiso 1 1 calc R . . C3 C -0.1035(8) 0.49161(18) 0.4218(9) 0.0256(11) Uani 1 1 d . . . H3 H -0.0554 0.4626 0.4960 0.031 Uiso 1 1 calc R . . C4 C -0.2836(8) 0.49811(18) 0.3079(8) 0.0246(11) Uani 1 1 d . . . H4 H -0.3602 0.4737 0.3030 0.029 Uiso 1 1 calc R . . C5 C -0.3540(8) 0.54081(18) 0.1990(8) 0.0229(11) Uani 1 1 d . . . C6 C -0.5392(8) 0.5520(2) 0.0738(9) 0.0260(12) Uani 1 1 d . . . H6 H -0.6240 0.5292 0.0601 0.031 Uiso 1 1 calc R . . C7 C -0.5957(7) 0.5949(2) -0.0260(9) 0.0251(11) Uani 1 1 d . . . H7 H -0.7196 0.6009 -0.1104 0.030 Uiso 1 1 calc R . . C8 C -0.4743(8) 0.6311(2) -0.0077(9) 0.0205(10) Uani 1 1 d . . . C9 C -0.5252(8) 0.6769(2) -0.1038(9) 0.0244(11) Uani 1 1 d . . . H9 H -0.6472 0.6851 -0.1880 0.029 Uiso 1 1 calc R . . C10 C -0.3972(7) 0.70883(18) -0.0742(8) 0.0218(10) Uani 1 1 d . . . H10 H -0.4310 0.7398 -0.1345 0.026 Uiso 1 1 calc R . . C11 C -0.2173(7) 0.69667(17) 0.0435(8) 0.0201(10) Uani 1 1 d . . . H11 H -0.1318 0.7196 0.0597 0.024 Uiso 1 1 calc R . . C12 C -0.2900(8) 0.62078(17) 0.1110(9) 0.0172(11) Uani 1 1 d . . . C13 C -0.2326(7) 0.57619(18) 0.2133(8) 0.0177(10) Uani 1 1 d . . . C14 C 0.4388(7) 0.64278(19) 0.4260(8) 0.0167(9) Uani 1 1 d . . . C15 C 0.7531(9) 0.62121(17) 0.6369(9) 0.0194(11) Uani 1 1 d . . . H15A H 0.7415 0.5894 0.5736 0.023 Uiso 1 1 calc R . . H15B H 0.7566 0.6167 0.7652 0.023 Uiso 1 1 calc R . . C16 C 0.9190(7) 0.64754(19) 0.6758(9) 0.0232(11) Uani 1 1 d . . . H16A H 0.9554 0.6356 0.5838 0.028 Uiso 1 1 calc R . . H16B H 1.0187 0.6432 0.8187 0.028 Uiso 1 1 calc R . . C17 C 0.8638(7) 0.70062(18) 0.6322(9) 0.0218(10) Uani 1 1 d . . . H17A H 0.8800 0.7167 0.7547 0.026 Uiso 1 1 calc R . . H17B H 0.9339 0.7180 0.5875 0.026 Uiso 1 1 calc R . . C18 C 0.6690(7) 0.69893(17) 0.4629(8) 0.0199(10) Uani 1 1 d . . . H18A H 0.6034 0.7264 0.4728 0.024 Uiso 1 1 calc R . . H18B H 0.6542 0.6995 0.3273 0.024 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 Pt 0.02029(9) 0.01218(7) 0.01908(8) -0.00238(11) 0.01371(7) -0.00317(11) S1 0.0206(6) 0.0170(5) 0.0284(6) -0.0003(5) 0.0147(6) 0.0000(5) S2 0.0310(7) 0.0160(5) 0.0285(7) -0.0020(5) 0.0201(6) -0.0057(5) N1 0.034(3) 0.0155(19) 0.024(2) -0.0022(17) 0.020(2) -0.0014(18) N2 0.022(2) 0.0129(17) 0.023(2) -0.0014(17) 0.0151(18) -0.0020(17) C1 0.018(2) 0.0060(17) 0.016(2) -0.0022(16) 0.0130(19) -0.0026(16) C2 0.030(3) 0.014(2) 0.023(3) 0.0030(19) 0.018(2) 0.001(2) C3 0.044(3) 0.015(2) 0.025(3) -0.001(2) 0.024(3) -0.003(2) C4 0.040(3) 0.019(2) 0.025(3) -0.006(2) 0.025(3) -0.013(2) C5 0.034(3) 0.021(2) 0.024(3) -0.008(2) 0.022(3) -0.009(2) C6 0.027(3) 0.024(2) 0.033(3) -0.006(2) 0.020(3) -0.012(2) C7 0.020(3) 0.028(3) 0.029(3) -0.006(2) 0.014(2) -0.004(2) C8 0.019(3) 0.021(2) 0.019(3) -0.004(2) 0.009(2) -0.002(2) C9 0.022(3) 0.028(3) 0.025(3) 0.000(2) 0.013(2) 0.003(2) C10 0.028(3) 0.018(2) 0.017(2) 0.0032(19) 0.011(2) 0.006(2) C11 0.030(3) 0.014(2) 0.017(2) -0.0006(18) 0.013(2) 0.0005(19) C12 0.024(3) 0.012(2) 0.023(3) -0.0054(18) 0.017(2) -0.0041(18) C13 0.025(3) 0.015(2) 0.021(2) -0.0035(18) 0.018(2) -0.0048(19) C14 0.018(2) 0.015(2) 0.017(2) -0.005(2) 0.009(2) -0.0025(19) C15 0.023(3) 0.013(3) 0.021(3) -0.0022(18) 0.011(2) 0.0033(19) C16 0.024(3) 0.023(2) 0.025(3) -0.002(2) 0.015(2) 0.004(2) C17 0.024(3) 0.020(2) 0.028(3) -0.004(2) 0.019(2) -0.003(2) C18 0.026(3) 0.013(2) 0.025(3) -0.0004(19) 0.016(2) -0.0013(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 Pt N1 2.029(5) . ? Pt C1 2.038(4) . ? Pt S1 2.3236(13) . ? Pt S2 2.3493(16) . ? S1 C14 1.726(6) . ? S2 C14 1.707(6) . ? N1 C11 1.372(6) . ? N1 C12 1.386(7) . ? N2 C14 1.327(7) . ? N2 C15 1.463(7) . ? N2 C18 1.468(6) . ? C1 C2 1.334(6) . ? C1 C13 1.376(7) . ? C2 C3 1.408(7) . ? C2 H2 0.9500 . ? C3 C4 1.369(9) . ? C3 H3 0.9500 . ? C4 C5 1.397(8) . ? C4 H4 0.9500 . ? C5 C13 1.424(7) . ? C5 C6 1.432(8) . ? C6 C7 1.363(8) . ? C6 H6 0.9500 . ? C7 C8 1.431(8) . ? C7 H7 0.9500 . ? C8 C12 1.419(9) . ? C8 C9 1.420(8) . ? C9 C10 1.367(8) . ? C9 H9 0.9500 . ? C10 C11 1.398(8) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.412(7) . ? C15 C16 1.530(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.535(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.518(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? 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 N1 Pt C1 81.46(18) . . ? N1 Pt S1 103.21(13) . . ? C1 Pt S1 175.08(13) . . ? N1 Pt S2 177.68(14) . . ? C1 Pt S2 100.05(14) . . ? S1 Pt S2 75.24(5) . . ? C14 S1 Pt 86.32(18) . . ? C14 S2 Pt 85.91(19) . . ? C11 N1 C12 116.7(5) . . ? C11 N1 Pt 131.3(4) . . ? C12 N1 Pt 111.9(4) . . ? C14 N2 C15 122.5(5) . . ? C14 N2 C18 124.3(5) . . ? C15 N2 C18 112.9(4) . . ? C2 C1 C13 119.2(4) . . ? C2 C1 Pt 128.0(4) . . ? C13 C1 Pt 112.7(3) . . ? C1 C2 C3 121.3(5) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 120.5(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.7(5) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C13 117.6(5) . . ? C4 C5 C6 125.3(5) . . ? C13 C5 C6 117.1(5) . . ? C7 C6 C5 121.1(5) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 122.0(5) . . ? C6 C7 H7 119.0 . . ? C8 C7 H7 119.0 . . ? C12 C8 C9 117.1(5) . . ? C12 C8 C7 118.3(5) . . ? C9 C8 C7 124.5(6) . . ? C10 C9 C8 119.4(5) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 121.1(5) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? N1 C11 C10 122.1(5) . . ? N1 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? N1 C12 C13 117.3(5) . . ? N1 C12 C8 123.5(5) . . ? C13 C12 C8 119.2(5) . . ? C1 C13 C12 116.1(5) . . ? C1 C13 C5 121.7(5) . . ? C12 C13 C5 122.1(5) . . ? N2 C14 S2 123.1(4) . . ? N2 C14 S1 124.5(4) . . ? S2 C14 S1 112.4(3) . . ? N2 C15 C16 103.8(4) . . ? N2 C15 H15A 111.0 . . ? C16 C15 H15A 111.0 . . ? N2 C15 H15B 111.0 . . ? C16 C15 H15B 111.0 . . ? H15A C15 H15B 109.0 . . ? C15 C16 C17 104.7(4) . . ? C15 C16 H16A 110.8 . . ? C17 C16 H16A 110.8 . . ? C15 C16 H16B 110.8 . . ? C17 C16 H16B 110.8 . . ? H16A C16 H16B 108.9 . . ? C18 C17 C16 104.2(4) . . ? C18 C17 H17A 110.9 . . ? C16 C17 H17A 110.9 . . ? C18 C17 H17B 110.9 . . ? C16 C17 H17B 110.9 . . ? H17A C17 H17B 108.9 . . ? N2 C18 C17 103.6(4) . . ? N2 C18 H18A 111.0 . . ? C17 C18 H18A 111.0 . . ? N2 C18 H18B 111.0 . . ? C17 C18 H18B 111.0 . . ? H18A C18 H18B 109.0 . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.841 _refine_diff_density_min -1.308 _refine_diff_density_rms 0.123 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 798309' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H14 N2 Pt S2' _chemical_formula_weight 493.50 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.99202(17) _cell_length_b 9.5990(2) _cell_length_c 22.4903(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.384(2) _cell_angle_gamma 90.00 _cell_volume 1500.11(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11472 _cell_measurement_theta_min 4.1887 _cell_measurement_theta_max 28.8050 _exptl_crystal_description bloc _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 9.625 _exptl_absorpt_correction_T_min 0.1102 _exptl_absorpt_correction_T_max 0.2915 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.0655 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16113 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 4.20 _diffrn_reflns_theta_max 28.81 _diffrn_orient_matrix_UB_11 0.0724124178 _diffrn_orient_matrix_UB_12 -0.0107711012 _diffrn_orient_matrix_UB_13 0.0242634682 _diffrn_orient_matrix_UB_21 0.0129436568 _diffrn_orient_matrix_UB_22 0.0731193419 _diffrn_orient_matrix_UB_23 0.0029084316 _diffrn_orient_matrix_UB_31 -0.0710086942 _diffrn_orient_matrix_UB_32 0.0023811307 _diffrn_orient_matrix_UB_33 0.0202092179 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 17.00 49.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 77.0000 90.0000 32 #__ type_ start__ end____ width___ exp.time_ 2 omega -50.00 33.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 77.0000 -180.0000 83 #__ type_ start__ end____ width___ exp.time_ 3 omega -11.00 92.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 77.0000 -30.0000 103 #__ type_ start__ end____ width___ exp.time_ 4 omega -11.00 95.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 77.0000 90.0000 106 #__ type_ start__ end____ width___ exp.time_ 5 omega 34.00 102.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 179.0000 0.0000 68 #__ type_ start__ end____ width___ exp.time_ 6 omega -6.00 93.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 67.0000 -106.0000 99 #__ type_ start__ end____ width___ exp.time_ 7 omega 34.00 59.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 179.0000 -150.0000 25 #__ type_ start__ end____ width___ exp.time_ 8 omega -51.00 54.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 -37.0000 -30.0000 105 ; _reflns_number_total 3615 _reflns_number_gt 3107 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3615 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0571 _refine_ls_wR_factor_gt 0.0556 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Pt Pt -0.002098(17) 0.156751(13) 0.071803(6) 0.01726(6) Uani 1 1 d . . . S1 S 0.08952(13) 0.23983(10) -0.02085(4) 0.0249(2) Uani 1 1 d . . . S2 S -0.24609(13) 0.30229(10) 0.03497(4) 0.02284(19) Uani 1 1 d . . . N1 N 0.2181(4) 0.0243(3) 0.10083(13) 0.0174(6) Uani 1 1 d . . . N2 N -0.1856(4) 0.4119(3) -0.07217(14) 0.0260(7) Uani 1 1 d . . . C1 C -0.0938(5) 0.1001(4) 0.14944(15) 0.0182(7) Uani 1 1 d . . . C2 C -0.2512(5) 0.1414(3) 0.17750(17) 0.0207(7) Uani 1 1 d . . . H2 H -0.3386 0.2074 0.1583 0.025 Uiso 1 1 calc R . . C3 C -0.2850(5) 0.0879(4) 0.23365(17) 0.0217(7) Uani 1 1 d . . . H3 H -0.3953 0.1180 0.2512 0.026 Uiso 1 1 calc R . . C4 C -0.1617(5) -0.0070(3) 0.26376(17) 0.0214(7) Uani 1 1 d . . . H4 H -0.1878 -0.0424 0.3015 0.026 Uiso 1 1 calc R . . C5 C 0.0035(5) -0.0511(3) 0.23823(15) 0.0175(7) Uani 1 1 d . . . C6 C 0.1453(5) -0.1473(3) 0.26618(17) 0.0204(7) Uani 1 1 d . . . H6 H 0.1282 -0.1853 0.3042 0.025 Uiso 1 1 calc R . . C7 C 0.3026(5) -0.1849(3) 0.23935(17) 0.0207(7) Uani 1 1 d . . . H7 H 0.3932 -0.2481 0.2591 0.025 Uiso 1 1 calc R . . C8 C 0.3340(5) -0.1307(3) 0.18190(17) 0.0183(7) Uani 1 1 d . . . C9 C 0.4928(5) -0.1643(3) 0.15101(18) 0.0235(8) Uani 1 1 d . . . H9 H 0.5882 -0.2279 0.1677 0.028 Uiso 1 1 calc R . . C10 C 0.5075(5) -0.1037(4) 0.09641(18) 0.0254(8) Uani 1 1 d . . . H10 H 0.6129 -0.1260 0.0749 0.031 Uiso 1 1 calc R . . C11 C 0.3690(5) -0.0101(4) 0.07275(17) 0.0241(8) Uani 1 1 d . . . H11 H 0.3822 0.0312 0.0350 0.029 Uiso 1 1 calc R . . C12 C 0.1988(4) -0.0369(3) 0.15470(15) 0.0172(7) Uani 1 1 d . . . C13 C 0.0328(5) 0.0031(3) 0.18195(15) 0.0168(7) Uani 1 1 d . . . C14 C -0.1230(5) 0.3316(4) -0.02690(17) 0.0224(8) Uani 1 1 d . . . C15 C -0.0736(6) 0.4350(4) -0.12248(17) 0.0290(9) Uani 1 1 d . . . H15A H 0.0465 0.3818 -0.1162 0.043 Uiso 1 1 calc R . . H15B H -0.0440 0.5344 -0.1253 0.043 Uiso 1 1 calc R . . H15C H -0.1484 0.4044 -0.1596 0.043 Uiso 1 1 calc R . . C16 C -0.3679(6) 0.4867(4) -0.07428(19) 0.0332(9) Uani 1 1 d . . . H16A H -0.4463 0.4460 -0.0452 0.050 Uiso 1 1 calc R . . H16B H -0.4368 0.4794 -0.1145 0.050 Uiso 1 1 calc R . . H16C H -0.3429 0.5850 -0.0645 0.050 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 Pt 0.01924(8) 0.01844(8) 0.01373(8) -0.00113(5) 0.00015(5) 0.00456(5) S1 0.0261(5) 0.0301(5) 0.0191(5) 0.0035(4) 0.0049(4) 0.0102(4) S2 0.0241(5) 0.0283(5) 0.0159(5) -0.0002(4) 0.0011(3) 0.0099(4) N1 0.0178(14) 0.0193(14) 0.0147(15) -0.0016(12) 0.0000(11) 0.0037(11) N2 0.0303(17) 0.0296(17) 0.0174(17) 0.0014(13) 0.0000(13) 0.0073(14) C1 0.0226(17) 0.0162(16) 0.0148(18) -0.0060(14) -0.0023(14) 0.0006(13) C2 0.0221(18) 0.0172(17) 0.022(2) -0.0037(14) 0.0013(14) 0.0018(13) C3 0.0200(17) 0.0246(18) 0.0210(19) -0.0053(15) 0.0041(14) -0.0007(14) C4 0.0249(18) 0.0207(18) 0.0184(18) -0.0025(14) 0.0015(14) -0.0047(14) C5 0.0197(16) 0.0153(16) 0.0166(17) -0.0036(14) -0.0018(13) -0.0041(13) C6 0.0254(19) 0.0159(17) 0.0188(19) 0.0032(14) -0.0029(14) -0.0052(13) C7 0.0227(18) 0.0146(16) 0.023(2) -0.0011(14) -0.0050(15) 0.0007(13) C8 0.0199(17) 0.0136(16) 0.0202(19) -0.0017(13) -0.0027(14) 0.0008(12) C9 0.0232(18) 0.0214(18) 0.025(2) -0.0017(15) -0.0020(15) 0.0045(14) C10 0.0202(18) 0.034(2) 0.022(2) -0.0042(17) 0.0032(14) 0.0071(15) C11 0.0254(18) 0.031(2) 0.0167(18) -0.0013(15) 0.0041(14) 0.0030(15) C12 0.0176(16) 0.0160(16) 0.0175(18) -0.0050(14) -0.0003(13) -0.0017(13) C13 0.0173(16) 0.0152(16) 0.0169(18) -0.0034(13) -0.0024(13) -0.0028(12) C14 0.0257(19) 0.0247(18) 0.0164(19) -0.0041(14) -0.0003(14) 0.0023(14) C15 0.036(2) 0.034(2) 0.017(2) 0.0053(16) -0.0006(16) 0.0016(17) C16 0.036(2) 0.038(2) 0.024(2) 0.0047(18) -0.0068(17) 0.0142(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C1 2.001(3) . ? Pt N1 2.047(3) . ? Pt S2 2.2878(9) . ? Pt S1 2.3843(9) . ? S1 C14 1.720(4) . ? S2 C14 1.738(4) . ? N1 C11 1.330(4) . ? N1 C12 1.366(4) . ? N2 C14 1.313(5) . ? N2 C16 1.459(5) . ? N2 C15 1.463(5) . ? C1 C2 1.386(5) . ? C1 C13 1.429(5) . ? C2 C3 1.407(5) . ? C3 C4 1.379(5) . ? C4 C5 1.411(5) . ? C5 C13 1.404(5) . ? C5 C6 1.447(5) . ? C6 C7 1.361(5) . ? C7 C8 1.432(5) . ? C8 C12 1.397(5) . ? C8 C9 1.411(5) . ? C9 C10 1.373(5) . ? C10 C11 1.383(5) . ? C12 C13 1.424(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt N1 81.69(12) . . ? C1 Pt S2 100.57(10) . . ? N1 Pt S2 177.39(8) . . ? C1 Pt S1 175.34(10) . . ? N1 Pt S1 102.76(8) . . ? S2 Pt S1 75.01(3) . . ? C14 S1 Pt 85.80(13) . . ? C14 S2 Pt 88.46(13) . . ? C11 N1 C12 118.5(3) . . ? C11 N1 Pt 127.6(2) . . ? C12 N1 Pt 113.9(2) . . ? C14 N2 C16 121.9(3) . . ? C14 N2 C15 121.9(3) . . ? C16 N2 C15 116.2(3) . . ? C2 C1 C13 115.6(3) . . ? C2 C1 Pt 131.9(3) . . ? C13 C1 Pt 112.5(2) . . ? C1 C2 C3 121.7(3) . . ? C4 C3 C2 121.6(3) . . ? C3 C4 C5 119.6(3) . . ? C13 C5 C4 117.6(3) . . ? C13 C5 C6 117.8(3) . . ? C4 C5 C6 124.6(3) . . ? C7 C6 C5 121.7(3) . . ? C6 C7 C8 121.1(3) . . ? C12 C8 C9 117.6(3) . . ? C12 C8 C7 117.7(3) . . ? C9 C8 C7 124.7(3) . . ? C10 C9 C8 119.0(3) . . ? C9 C10 C11 120.0(3) . . ? N1 C11 C10 122.5(3) . . ? N1 C12 C8 122.4(3) . . ? N1 C12 C13 115.6(3) . . ? C8 C12 C13 122.0(3) . . ? C5 C13 C12 119.7(3) . . ? C5 C13 C1 123.9(3) . . ? C12 C13 C1 116.3(3) . . ? N2 C14 S1 124.9(3) . . ? N2 C14 S2 124.3(3) . . ? S1 C14 S2 110.7(2) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.430 _refine_diff_density_min -1.413 _refine_diff_density_rms 0.168 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 798310' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Ag2 Cl2 N4 O10 Pt2 S4' _chemical_formula_weight 1569.87 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 15.0861(4) _cell_length_b 20.0925(6) _cell_length_c 8.0443(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.918(2) _cell_angle_gamma 90.00 _cell_volume 2425.38(11) _cell_formula_units_Z 2 _cell_measurement_temperature 101(2) _cell_measurement_reflns_used 8028 _cell_measurement_theta_min 4.1902 _cell_measurement_theta_max 28.7233 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 6.887 _exptl_absorpt_correction_T_min 0.3003 _exptl_absorpt_correction_T_max 0.7246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 101(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.0655 _diffrn_measurement_method 'w scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12390 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.20 _diffrn_reflns_theta_max 28.72 _diffrn_orient_matrix_UB_11 0.0268077000 _diffrn_orient_matrix_UB_12 -0.0290483000 _diffrn_orient_matrix_UB_13 0.0088147000 _diffrn_orient_matrix_UB_21 0.0374942000 _diffrn_orient_matrix_UB_22 0.0197275000 _diffrn_orient_matrix_UB_23 0.0284366000 _diffrn_orient_matrix_UB_31 -0.0104317000 _diffrn_orient_matrix_UB_32 -0.0036735000 _diffrn_orient_matrix_UB_33 0.0835084000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -92.00 -2.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 -77.0000 -90.0000 90 #__ type_ start__ end____ width___ exp.time_ 2 omega 63.00 89.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 77.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 3 omega -39.00 53.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 -77.0000 90.0000 92 #__ type_ start__ end____ width___ exp.time_ 4 omega -9.00 16.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 77.0000 -60.0000 25 #__ type_ start__ end____ width___ exp.time_ 5 omega -92.00 13.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 -77.0000 120.0000 105 #__ type_ start__ end____ width___ exp.time_ 6 omega -93.00 12.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 -37.0000 -30.0000 105 #__ type_ start__ end____ width___ exp.time_ 7 omega -102.00 -32.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 179.0000 -90.0000 70 #__ type_ start__ end____ width___ exp.time_ 8 omega 34.00 59.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 179.0000 -90.0000 25 #__ type_ start__ end____ width___ exp.time_ 9 omega 34.00 102.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 179.0000 0.0000 68 ; _reflns_number_total 2935 _reflns_number_gt 2500 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Given the symmetry imposed by the spatial group, only half of the benzoquinolinate ligand is present in the asymmetric unit, and thus, the position of the atom bonded to the Pt centre is shared by two atoms, N(1) and C(1), constrained to have the same coordinates and anisotropic thermal parameters and occupancy 0.5. Also, weak restrains were used in the geometry and thermal anisotropic parameters of the acetone molecule coordinated to the Ag Centre. The methylene atoms of the S donor ligand are disordered over two sets of positions refined with partial occupancy 0.5. Unresolved relatively high residual electron density is present in the final model but it does not correspond to unidentified atom sites but rather to residual peaks very close to heavy atoms with no chemical meaning and that probably are due to the quality of the crystal. ; _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^)+(0.0295P)^2^+53.9212P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2935 _refine_ls_number_parameters 178 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.081 _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 Pt Pt 0.00454(2) 0.5000 0.19891(4) 0.01797(12) Uani 1 2 d S . . Ag Ag 0.0000 0.42436(4) 0.5000 0.0536(4) Uani 1 2 d S . . S S -0.11654(12) 0.42810(11) 0.2397(2) 0.0277(4) Uani 1 1 d . A . N1 N 0.1053(4) 0.5668(3) 0.1813(7) 0.0158(12) Uani 0.50 1 d P A 1 N2 N -0.2579(5) 0.5000 0.3089(10) 0.025(2) Uani 1 2 d S . . C1 C 0.1053(4) 0.5668(3) 0.1813(7) 0.0158(12) Uani 0.50 1 d P A 2 C2 C 0.1020(5) 0.6341(4) 0.1719(8) 0.0207(15) Uani 1 1 d . . . H2 H 0.0467 0.6562 0.1763 0.025 Uiso 1 1 calc R A 1 C3 C 0.1788(5) 0.6714(4) 0.1559(8) 0.0235(15) Uani 1 1 d . A . H3 H 0.1748 0.7186 0.1514 0.028 Uiso 1 1 calc R . . C4 C 0.2596(5) 0.6417(4) 0.1467(8) 0.0228(15) Uani 1 1 d . . . H4 H 0.3110 0.6678 0.1344 0.027 Uiso 1 1 calc R A . C5 C 0.2656(4) 0.5712(4) 0.1556(8) 0.0197(15) Uani 1 1 d . A . C6 C 0.1872(4) 0.5355(4) 0.1734(7) 0.0183(14) Uani 1 1 d . . . C7 C 0.3463(4) 0.5338(4) 0.1387(8) 0.0233(15) Uani 1 1 d . . . H7 H 0.4002 0.5570 0.1275 0.028 Uiso 1 1 calc R A . C8 C -0.1763(6) 0.5000 0.2708(12) 0.022(2) Uani 1 2 d S . . C9 C -0.3098(5) 0.4398(5) 0.3308(10) 0.037(2) Uani 1 1 d D . . H9A H -0.2935 0.4180 0.4401 0.045 Uiso 1 1 calc R A 1 H9B H -0.3062 0.4073 0.2391 0.045 Uiso 1 1 calc R A 1 C10 C -0.4018(8) 0.4755(6) 0.321(2) 0.032(4) Uani 0.50 1 d PDU . 1 H10A H -0.4378 0.4603 0.2186 0.038 Uiso 0.50 1 calc PR . 1 H10B H -0.4326 0.4603 0.4175 0.038 Uiso 0.50 1 calc PR . 1 C10' C -0.3979(9) 0.4547(8) 0.400(2) 0.035(4) Uani 0.50 1 d PDU . 2 H10C H -0.3991 0.4366 0.5138 0.043 Uiso 0.50 1 calc PR . 2 H10D H -0.4489 0.4366 0.3262 0.043 Uiso 0.50 1 calc PR . 2 O1 O 0.0402(7) 0.3124(5) 0.5052(13) 0.032(3) Uani 0.50 1 d P . . C11 C 0.0000 0.2551(6) 0.5000 0.053(4) Uani 1 2 d SD . . C12 C -0.0939(9) 0.2401(11) 0.503(2) 0.039(4) Uani 0.50 1 d PDU . . H12A H -0.1028 0.1919 0.4959 0.059 Uiso 0.50 1 calc PR A . H12B H -0.1282 0.2616 0.4076 0.059 Uiso 0.50 1 calc PR . . H12C H -0.1141 0.2567 0.6071 0.059 Uiso 0.50 1 calc PR . . C13 C 0.0692(13) 0.2026(10) 0.506(3) 0.048(5) Uani 0.50 1 d PDU . . H13A H 0.0406 0.1588 0.5021 0.072 Uiso 0.50 1 calc PR A . H13B H 0.1089 0.2068 0.6100 0.072 Uiso 0.50 1 calc PR . . H13C H 0.1038 0.2075 0.4103 0.072 Uiso 0.50 1 calc PR . . Cl Cl 0.0000 0.19557(12) 1.0000 0.0219(5) Uani 1 2 d S . . O2 O 0.0637(6) 0.1554(5) 1.0950(9) 0.080(3) Uani 1 1 d . . . O3 O 0.0443(4) 0.2359(3) 0.8874(6) 0.0287(12) 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 0.00858(16) 0.0336(2) 0.01114(16) 0.000 -0.00158(11) 0.000 Ag 0.1071(10) 0.0174(5) 0.0268(4) 0.000 -0.0394(5) 0.000 S 0.0174(8) 0.0476(13) 0.0170(8) -0.0074(8) -0.0033(6) 0.0066(8) N1 0.015(3) 0.022(3) 0.010(3) -0.002(2) -0.003(2) 0.007(3) N2 0.015(4) 0.041(6) 0.019(4) 0.000 -0.004(3) 0.000 C1 0.015(3) 0.022(3) 0.010(3) -0.002(2) -0.003(2) 0.007(3) C2 0.020(3) 0.025(4) 0.017(3) -0.005(3) -0.001(3) 0.010(3) C3 0.026(4) 0.023(4) 0.020(3) -0.003(3) -0.001(3) -0.001(3) C4 0.017(3) 0.031(4) 0.019(3) -0.001(3) 0.000(3) -0.002(3) C5 0.012(3) 0.033(4) 0.013(3) -0.002(3) -0.001(2) -0.001(3) C6 0.016(3) 0.028(4) 0.010(3) -0.001(3) -0.005(2) -0.001(3) C7 0.011(3) 0.033(4) 0.025(3) 0.000(3) -0.001(2) -0.004(3) C8 0.009(4) 0.039(6) 0.018(4) 0.000 -0.003(3) 0.000 C9 0.019(4) 0.063(6) 0.030(4) -0.004(4) 0.003(3) -0.016(4) C10 0.026(5) 0.038(6) 0.034(5) -0.001(4) 0.011(4) -0.010(4) C10' 0.036(5) 0.040(6) 0.033(5) 0.001(4) 0.013(4) -0.003(4) O1 0.044(6) 0.027(6) 0.025(5) 0.002(5) 0.004(5) 0.005(5) C11 0.131(15) 0.023(7) 0.006(5) 0.000 0.010(6) 0.000 C12 0.040(6) 0.043(6) 0.036(5) -0.002(4) 0.008(4) 0.004(5) C13 0.049(6) 0.051(6) 0.045(6) 0.000(5) 0.007(4) 0.001(5) Cl 0.0270(12) 0.0189(12) 0.0202(11) 0.000 0.0039(9) 0.000 O2 0.107(7) 0.092(6) 0.044(4) 0.032(4) 0.028(4) 0.075(6) O3 0.029(3) 0.029(3) 0.030(3) 0.003(2) 0.013(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt N1 2.044(6) . ? Pt C1 2.044(6) 6_565 ? Pt N1 2.044(6) 6_565 ? Pt S 2.378(2) . ? Pt S 2.378(2) 6_565 ? Pt Ag 2.8661(6) 5_566 ? Pt Ag 2.8661(6) . ? Pt Pt 3.1890(7) 5_565 ? Ag O1 2.328(11) 2_556 ? Ag O1 2.328(11) . ? Ag S 2.5930(17) 2_556 ? Ag S 2.5930(17) . ? Ag Pt 2.8661(6) 5_566 ? Ag Ag 3.0394(18) 5_566 ? S C8 1.735(5) . ? N1 C2 1.355(10) . ? N1 C6 1.393(9) . ? N2 C8 1.299(12) . ? N2 C9 1.462(10) . ? N2 C9 1.462(10) 6_565 ? C2 C3 1.398(10) . ? C2 H2 0.9500 . ? C3 C4 1.366(10) . ? C3 H3 0.9500 . ? C4 C5 1.420(11) . ? C4 H4 0.9500 . ? C5 C6 1.404(9) . ? C5 C7 1.448(10) . ? C6 C6 1.427(15) 6_565 ? C7 C7 1.359(15) 6_565 ? C7 H7 0.9500 . ? C8 S 1.735(5) 6_565 ? C9 C10' 1.520(12) . ? C9 C10 1.557(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C10 0.99(2) 6_565 ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10' C10' 1.82(3) 6_565 ? C10' H10C 0.9900 . ? C10' H10D 0.9900 . ? O1 O1 1.21(2) 2_556 ? O1 C11 1.300(15) . ? O1 C12 1.67(2) 2_556 ? C11 O1 1.300(15) 2_556 ? C11 C12 1.451(14) . ? C11 C12 1.451(14) 2_556 ? C11 C13 1.481(15) 2_556 ? C11 C13 1.481(15) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? Cl O2 1.416(7) 2_557 ? Cl O2 1.416(7) . ? Cl O3 1.431(5) . ? Cl O3 1.431(5) 2_557 ? 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 N1 Pt C1 82.1(3) . 6_565 ? N1 Pt N1 82.1(3) . 6_565 ? C1 Pt N1 0.0(4) 6_565 6_565 ? N1 Pt S 174.86(16) . . ? C1 Pt S 101.43(17) 6_565 . ? N1 Pt S 101.43(17) 6_565 . ? N1 Pt S 101.43(17) . 6_565 ? C1 Pt S 174.86(16) 6_565 6_565 ? N1 Pt S 174.86(16) 6_565 6_565 ? S Pt S 74.82(10) . 6_565 ? N1 Pt Ag 78.07(16) . 5_566 ? C1 Pt Ag 119.31(15) 6_565 5_566 ? N1 Pt Ag 119.31(15) 6_565 5_566 ? S Pt Ag 96.89(5) . 5_566 ? S Pt Ag 58.38(4) 6_565 5_566 ? N1 Pt Ag 119.31(15) . . ? C1 Pt Ag 78.07(16) 6_565 . ? N1 Pt Ag 78.07(16) 6_565 . ? S Pt Ag 58.38(4) . . ? S Pt Ag 96.89(5) 6_565 . ? Ag Pt Ag 64.04(3) 5_566 . ? N1 Pt Pt 83.44(15) . 5_565 ? C1 Pt Pt 83.44(15) 6_565 5_565 ? N1 Pt Pt 83.44(15) 6_565 5_565 ? S Pt Pt 100.61(4) . 5_565 ? S Pt Pt 100.61(4) 6_565 5_565 ? Ag Pt Pt 147.750(16) 5_566 5_565 ? Ag Pt Pt 147.750(16) . 5_565 ? O1 Ag O1 30.0(5) 2_556 . ? O1 Ag S 101.3(3) 2_556 2_556 ? O1 Ag S 81.9(3) . 2_556 ? O1 Ag S 81.9(3) 2_556 . ? O1 Ag S 101.3(3) . . ? S Ag S 176.69(11) 2_556 . ? O1 Ag Pt 119.9(3) 2_556 5_566 ? O1 Ag Pt 121.7(3) . 5_566 ? S Ag Pt 51.35(5) 2_556 5_566 ? S Ag Pt 126.43(5) . 5_566 ? O1 Ag Pt 121.7(3) 2_556 . ? O1 Ag Pt 119.9(3) . . ? S Ag Pt 126.43(5) 2_556 . ? S Ag Pt 51.35(5) . . ? Pt Ag Pt 115.96(3) 5_566 . ? O1 Ag Ag 165.0(3) 2_556 5_566 ? O1 Ag Ag 165.0(3) . 5_566 ? S Ag Ag 88.34(5) 2_556 5_566 ? S Ag Ag 88.34(5) . 5_566 ? Pt Ag Ag 57.979(16) 5_566 5_566 ? Pt Ag Ag 57.979(16) . 5_566 ? C8 S Pt 86.1(3) . . ? C8 S Ag 103.1(3) . . ? Pt S Ag 70.27(5) . . ? C2 N1 C6 118.4(6) . . ? C2 N1 Pt 129.5(5) . . ? C6 N1 Pt 112.1(5) . . ? C8 N2 C9 124.1(4) . . ? C8 N2 C9 124.1(4) . 6_565 ? C9 N2 C9 111.8(9) . 6_565 ? N1 C2 C3 121.0(6) . . ? N1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 121.5(7) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.1(7) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 117.7(6) . . ? C6 C5 C7 118.0(7) . . ? C4 C5 C7 124.3(6) . . ? N1 C6 C5 122.3(7) . . ? N1 C6 C6 116.8(4) . 6_565 ? C5 C6 C6 120.7(4) . 6_565 ? C7 C7 C5 121.3(4) 6_565 . ? C7 C7 H7 119.4 6_565 . ? C5 C7 H7 119.4 . . ? N2 C8 S 123.6(3) . 6_565 ? N2 C8 S 123.6(3) . . ? S C8 S 112.7(5) 6_565 . ? N2 C9 C10' 112.3(9) . . ? N2 C9 C10 95.6(8) . . ? C10' C9 C10 28.3(7) . . ? N2 C9 H9A 112.6 . . ? C10' C9 H9A 84.8 . . ? C10 C9 H9A 112.6 . . ? N2 C9 H9B 112.6 . . ? C10' C9 H9B 121.2 . . ? C10 C9 H9B 112.6 . . ? H9A C9 H9B 110.1 . . ? C10 C10 C9 117.4(6) 6_565 . ? C10 C10 H10A 107.9 6_565 . ? C9 C10 H10A 107.9 . . ? C10 C10 H10B 107.9 6_565 . ? C9 C10 H10B 107.9 . . ? H10A C10 H10B 107.2 . . ? C9 C10' C10' 101.4(7) . 6_565 ? C9 C10' H10C 111.5 . . ? C10' C10' H10C 111.5 6_565 . ? C9 C10' H10D 111.5 . . ? C10' C10' H10D 111.5 6_565 . ? H10C C10' H10D 109.3 . . ? O1 O1 C11 62.4(5) 2_556 . ? O1 O1 C12 119.1(7) 2_556 2_556 ? C11 O1 C12 56.9(7) . 2_556 ? O1 O1 Ag 75.0(3) 2_556 . ? C11 O1 Ag 137.3(8) . . ? C12 O1 Ag 165.3(9) 2_556 . ? O1 C11 O1 55.3(11) . 2_556 ? O1 C11 C12 129.5(12) . . ? O1 C11 C12 74.5(10) 2_556 . ? O1 C11 C12 74.5(10) . 2_556 ? O1 C11 C12 129.5(12) 2_556 2_556 ? C12 C11 C12 156(2) . 2_556 ? O1 C11 C13 163.0(12) . 2_556 ? O1 C11 C13 107.8(10) 2_556 2_556 ? C12 C11 C13 33.6(10) . 2_556 ? C12 C11 C13 122.5(17) 2_556 2_556 ? O1 C11 C13 107.8(10) . . ? O1 C11 C13 163.0(12) 2_556 . ? C12 C11 C13 122.5(17) . . ? C12 C11 C13 33.6(10) 2_556 . ? C13 C11 C13 89.2(19) 2_556 . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 Cl O2 110.5(9) 2_557 . ? O2 Cl O3 108.4(4) 2_557 . ? O2 Cl O3 109.2(4) . . ? O2 Cl O3 109.2(4) 2_557 2_557 ? O2 Cl O3 108.4(4) . 2_557 ? O3 Cl O3 111.0(5) . 2_557 ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.543 _refine_diff_density_min -2.156 _refine_diff_density_rms 0.240 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 798311' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H34 Ag2 Cl2 N4 O9 Pt2 S4' _chemical_formula_weight 1459.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.72036(14) _cell_length_b 12.36498(16) _cell_length_c 15.33482(19) _cell_angle_alpha 85.5909(10) _cell_angle_beta 68.4364(11) _cell_angle_gamma 77.4975(10) _cell_volume 2017.79(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 29993 _cell_measurement_theta_min 4.1461 _cell_measurement_theta_max 28.7517 _exptl_crystal_description block _exptl_crystal_colour 'pale orange' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 8.266 _exptl_absorpt_correction_T_min 0.1773 _exptl_absorpt_correction_T_max 0.4370 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.0655 _diffrn_measurement_method 'w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43606 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.15 _diffrn_reflns_theta_max 28.82 _diffrn_orient_matrix_UB_11 -0.0169651000 _diffrn_orient_matrix_UB_12 0.0405586000 _diffrn_orient_matrix_UB_13 -0.0307707000 _diffrn_orient_matrix_UB_21 0.0591832000 _diffrn_orient_matrix_UB_22 -0.0180415000 _diffrn_orient_matrix_UB_23 -0.0356834000 _diffrn_orient_matrix_UB_31 -0.0250206000 _diffrn_orient_matrix_UB_32 -0.0384957000 _diffrn_orient_matrix_UB_33 -0.0159208000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -86.00 10.30 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 -37.0000 -120.0000 107 #__ type_ start__ end____ width___ exp.time_ 2 omega -91.00 -8.20 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 -77.0000 60.0000 92 #__ type_ start__ end____ width___ exp.time_ 3 omega -48.00 54.60 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 -77.0000 -150.0000 114 #__ type_ start__ end____ width___ exp.time_ 4 omega -22.00 54.50 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 -77.0000 120.0000 85 #__ type_ start__ end____ width___ exp.time_ 5 omega -11.00 68.20 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 77.0000 0.0000 88 #__ type_ start__ end____ width___ exp.time_ 6 omega -92.00 12.40 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 -77.0000 0.0000 116 #__ type_ start__ end____ width___ exp.time_ 7 omega -92.00 12.40 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 -77.0000 -120.0000 116 #__ type_ start__ end____ width___ exp.time_ 8 omega -24.00 23.70 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 -99.0000 176.0000 53 #__ type_ start__ end____ width___ exp.time_ 9 omega -65.00 25.00 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 99.0000 3.0000 100 #__ type_ start__ end____ width___ exp.time_ 10 omega 34.00 101.50 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 179.0000 -180.0000 75 #__ type_ start__ end____ width___ exp.time_ 11 omega 34.00 101.50 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 179.0000 -30.0000 75 #__ type_ start__ end____ width___ exp.time_ 12 omega -10.00 95.30 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 37.0000 -180.0000 117 #__ type_ start__ end____ width___ exp.time_ 13 omega -51.00 53.40 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 -37.0000 -60.0000 116 #__ type_ start__ end____ width___ exp.time_ 14 omega 34.00 61.90 0.9000 15.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 179.0000 -120.0000 31 ; _reflns_number_total 9647 _reflns_number_gt 8420 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The positions of the silver atoms were found to be very diffuse and disordered over several sites. The best model consisted in three different locations for each silver centre, refined with partial occupancy 0.43/0.42/0.15 for Ag(1) and 0.63/0.20/0.17 for Ag(2). The anisotropic thermal parameters of each set of silver positions were constrained to common values. Besides, the Cl(2) perchlorate moiety was also found to be disordered with three of its oxygen atoms refined over two sites with partial occupancy 0.60/0.40. The pairs of analogous oxygen atoms of each disordered sets had their anisotropic thermal parameters constrained to common values. Also, geometrical restrains were used for this disordered perchlorate unit Unresolved relatively high residual electron density is present in the final model but it does not correspond to unidentified atom sites but rather to residual peaks very close to heavy atoms with no chemical meaning and that probably are due to the disorder of the silver atoms and thequality of the crystal. ; _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^)+(0.0276P)^2^+25.7524P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9647 _refine_ls_number_parameters 544 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.00582(2) 0.372681(19) 0.105609(15) 0.01674(6) Uani 1 1 d . . . Pt2 Pt 0.06908(2) 0.358152(18) 0.373098(15) 0.01437(6) Uani 1 1 d . . . Ag1 Ag 0.2118(3) 0.26677(16) 0.18168(19) 0.0345(5) Uani 0.42 1 d P A 1 Ag2 Ag 0.01775(8) 0.17678(8) 0.24513(5) 0.02943(17) Uani 0.63 1 d P A 1 Ag1' Ag 0.1992(2) 0.31750(17) 0.18416(17) 0.0345(5) Uani 0.43 1 d P A 2 Ag2' Ag -0.0429(3) 0.2496(3) 0.2699(2) 0.02943(17) Uani 0.17 1 d P A 2 Ag1" Ag 0.1689(4) 0.3880(4) 0.1926(3) 0.0345(5) Uani 0.15 1 d P A 3 Ag2" Ag -0.0880(3) 0.3003(3) 0.28541(18) 0.02943(17) Uani 0.20 1 d P A 3 S1 S 0.21669(15) 0.29422(13) 0.01480(10) 0.0209(3) Uani 1 1 d . A . S2 S 0.00379(14) 0.18940(13) 0.07964(11) 0.0215(3) Uani 1 1 d . A . S3 S 0.04296(13) 0.17424(12) 0.40456(10) 0.0188(3) Uani 1 1 d . A . S4 S 0.27418(13) 0.25355(12) 0.32615(10) 0.0175(3) Uani 1 1 d . A . N1 N 0.0125(5) 0.5325(5) 0.1239(4) 0.0246(11) Uani 1 1 d . A . N2 N 0.2298(5) 0.0870(4) -0.0379(4) 0.0205(10) Uani 1 1 d . A . N3 N -0.1110(5) 0.4441(5) 0.4205(4) 0.0232(11) Uani 1 1 d . A . N4 N 0.2664(4) 0.0457(4) 0.3926(3) 0.0162(10) Uani 1 1 d . A . C1 C 0.1131(7) 0.5820(6) 0.0966(5) 0.0265(14) Uani 1 1 d . . . H1 H 0.1942 0.5398 0.0638 0.032 Uiso 1 1 calc R A . C2 C 0.0994(7) 0.6939(6) 0.1159(5) 0.0272(14) Uani 1 1 d . A . H2 H 0.1714 0.7259 0.0976 0.033 Uiso 1 1 calc R . . C3 C -0.0168(7) 0.7579(5) 0.1611(5) 0.0255(14) Uani 1 1 d . . . H3 H -0.0249 0.8341 0.1728 0.031 Uiso 1 1 calc R A . C4 C -0.1243(6) 0.7106(5) 0.1901(4) 0.0204(12) Uani 1 1 d . A . C5 C -0.2500(7) 0.7687(6) 0.2372(4) 0.0266(14) Uani 1 1 d . . . H5 H -0.2652 0.8453 0.2507 0.032 Uiso 1 1 calc R A . C6 C -0.3477(7) 0.7160(6) 0.2630(5) 0.0277(14) Uani 1 1 d . A . H6 H -0.4301 0.7572 0.2936 0.033 Uiso 1 1 calc R . . C7 C -0.3305(6) 0.6010(6) 0.2456(5) 0.0254(14) Uani 1 1 d . . . C8 C -0.4273(6) 0.5396(6) 0.2730(5) 0.0316(15) Uani 1 1 d . A . H8 H -0.5118 0.5754 0.3047 0.038 Uiso 1 1 calc R . . C9 C -0.3987(7) 0.4292(7) 0.2538(5) 0.0337(16) Uani 1 1 d . . . H9 H -0.4639 0.3884 0.2736 0.040 Uiso 1 1 calc R A . C10 C -0.2751(6) 0.3740(6) 0.2053(5) 0.0289(14) Uani 1 1 d . A . H10 H -0.2580 0.2973 0.1912 0.035 Uiso 1 1 calc R . . C11 C -0.1791(5) 0.4305(5) 0.1784(4) 0.0192(12) Uani 1 1 d . A . C12 C -0.2072(6) 0.5423(6) 0.1988(4) 0.0214(12) Uani 1 1 d . A . C13 C -0.1050(6) 0.5978(5) 0.1706(4) 0.0202(12) Uani 1 1 d . . . C14 C 0.1623(6) 0.1745(5) 0.0119(4) 0.0189(12) Uani 1 1 d . . . C15 C 0.3660(6) 0.0743(6) -0.0879(5) 0.0246(13) Uani 1 1 d . . . H15A H 0.3927 0.1410 -0.0787 0.037 Uiso 1 1 calc R A . H15B H 0.3860 0.0636 -0.1549 0.037 Uiso 1 1 calc R . . H15C H 0.4098 0.0098 -0.0632 0.037 Uiso 1 1 calc R . . C16 C 0.1724(7) -0.0059(6) -0.0431(5) 0.0302(15) Uani 1 1 d . . . H16A H 0.0822 0.0126 -0.0073 0.045 Uiso 1 1 calc R A . H16B H 0.2103 -0.0725 -0.0168 0.045 Uiso 1 1 calc R . . H16C H 0.1866 -0.0195 -0.1088 0.045 Uiso 1 1 calc R . . C17 C -0.2182(6) 0.4035(6) 0.4565(5) 0.0246(13) Uani 1 1 d . . . H17 H -0.2139 0.3257 0.4589 0.030 Uiso 1 1 calc R A . C18 C -0.3363(6) 0.4772(6) 0.4903(5) 0.0275(14) Uani 1 1 d . A . H18 H -0.4106 0.4482 0.5151 0.033 Uiso 1 1 calc R . . C19 C -0.3449(6) 0.5899(6) 0.4877(5) 0.0275(14) Uani 1 1 d . . . H19 H -0.4247 0.6380 0.5113 0.033 Uiso 1 1 calc R A . C20 C -0.2362(6) 0.6341(5) 0.4502(4) 0.0204(12) Uani 1 1 d . A . C21 C -0.2323(6) 0.7499(5) 0.4410(4) 0.0244(13) Uani 1 1 d . . . H21 H -0.3087 0.8030 0.4619 0.029 Uiso 1 1 calc R A . C22 C -0.1235(7) 0.7854(5) 0.4038(4) 0.0239(13) Uani 1 1 d . A . H22 H -0.1255 0.8628 0.3982 0.029 Uiso 1 1 calc R . . C23 C -0.0038(6) 0.7092(5) 0.3721(4) 0.0206(12) Uani 1 1 d . . . C24 C 0.1124(7) 0.7401(5) 0.3330(4) 0.0240(13) Uani 1 1 d . A . H24 H 0.1169 0.8162 0.3268 0.029 Uiso 1 1 calc R . . C25 C 0.2210(6) 0.6593(5) 0.3034(5) 0.0242(13) Uani 1 1 d . . . H25 H 0.3000 0.6805 0.2767 0.029 Uiso 1 1 calc R A . C26 C 0.2155(6) 0.5468(5) 0.3124(4) 0.0227(13) Uani 1 1 d . A . H26 H 0.2912 0.4927 0.2926 0.027 Uiso 1 1 calc R . . C27 C 0.1035(5) 0.5135(5) 0.3492(4) 0.0146(11) Uani 1 1 d . A . C28 C -0.0052(6) 0.5949(5) 0.3797(4) 0.0170(11) Uani 1 1 d . A . C29 C -0.1201(6) 0.5577(5) 0.4179(4) 0.0188(12) Uani 1 1 d . . . C30 C 0.2061(5) 0.1402(5) 0.3742(4) 0.0162(11) Uani 1 1 d . . . C31 C 0.2019(6) -0.0451(5) 0.4382(5) 0.0226(13) Uani 1 1 d . . . H31A H 0.1125 -0.0222 0.4486 0.034 Uiso 1 1 calc R A . H31B H 0.2126 -0.0625 0.4985 0.034 Uiso 1 1 calc R . . H31C H 0.2378 -0.1109 0.3978 0.034 Uiso 1 1 calc R . . C32 C 0.4022(6) 0.0235(5) 0.3722(5) 0.0234(13) Uani 1 1 d . . . H32A H 0.4360 0.0882 0.3416 0.035 Uiso 1 1 calc R A . H32B H 0.4430 -0.0410 0.3306 0.035 Uiso 1 1 calc R . . H32C H 0.4180 0.0085 0.4309 0.035 Uiso 1 1 calc R . . Cl1 Cl 0.29041(14) -0.04461(12) 0.16931(10) 0.0219(3) Uani 1 1 d . A . O1 O 0.3343(6) 0.0570(4) 0.1473(4) 0.0408(13) Uani 1 1 d . . . O2 O 0.1589(5) -0.0197(6) 0.2217(5) 0.0570(19) Uani 1 1 d . . . O3 O 0.3523(5) -0.1144(4) 0.2246(3) 0.0301(11) Uani 1 1 d . . . O4 O 0.3142(8) -0.1008(5) 0.0854(4) 0.066(2) Uani 1 1 d . . . Cl2 Cl -0.2991(2) 0.10968(18) 0.34239(16) 0.0490(6) Uani 1 1 d D . . O5 O -0.1900(8) 0.1413(10) 0.3380(7) 0.072(3) Uani 0.60 1 d PDU A 1 O6 O -0.3999(10) 0.1966(7) 0.4022(8) 0.096(4) Uani 0.60 1 d PDU A 1 O7 O -0.3176(9) 0.1157(9) 0.2558(4) 0.038(2) Uani 0.60 1 d PDU A 1 O5' O -0.1656(6) 0.0788(12) 0.2904(8) 0.072(3) Uani 0.40 1 d PD A 2 O6' O -0.3207(17) 0.1993(9) 0.4015(9) 0.096(4) Uani 0.40 1 d PD A 2 O7' O -0.3584(12) 0.1380(12) 0.2760(8) 0.038(2) Uani 0.40 1 d PD A 2 O8 O -0.3278(5) 0.0129(4) 0.3924(4) 0.0417(13) Uani 1 1 d DU A . O9 O 0.3795(5) 0.4084(4) 0.1000(4) 0.0359(12) Uani 1 1 d . . . C33 C 0.4746(6) 0.3494(6) 0.0495(5) 0.0274(14) Uani 1 1 d . A . C34 C 0.5477(9) 0.2576(7) 0.0895(6) 0.045(2) Uani 1 1 d . . . H34A H 0.5083 0.2582 0.1581 0.068 Uiso 1 1 calc R A . H34B H 0.6338 0.2683 0.0714 0.068 Uiso 1 1 calc R . . H34C H 0.5486 0.1863 0.0652 0.068 Uiso 1 1 calc R . . C35 C 0.5210(7) 0.3620(6) -0.0550(5) 0.0325(16) Uani 1 1 d . . . H35A H 0.4655 0.4241 -0.0722 0.049 Uiso 1 1 calc R A . H35B H 0.5218 0.2938 -0.0840 0.049 Uiso 1 1 calc R . . H35C H 0.6061 0.3765 -0.0772 0.049 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 0.01540(11) 0.02013(12) 0.01546(11) 0.00162(8) -0.00669(9) -0.00372(8) Pt2 0.01182(10) 0.01690(11) 0.01359(11) -0.00091(8) -0.00380(8) -0.00232(8) Ag1 0.0267(7) 0.0659(15) 0.0135(3) 0.0031(12) -0.0090(4) -0.0129(12) Ag2 0.0349(4) 0.0399(5) 0.0160(3) 0.0054(3) -0.0128(3) -0.0082(3) Ag1' 0.0267(7) 0.0659(15) 0.0135(3) 0.0031(12) -0.0090(4) -0.0129(12) Ag2' 0.0349(4) 0.0399(5) 0.0160(3) 0.0054(3) -0.0128(3) -0.0082(3) Ag1" 0.0267(7) 0.0659(15) 0.0135(3) 0.0031(12) -0.0090(4) -0.0129(12) Ag2" 0.0349(4) 0.0399(5) 0.0160(3) 0.0054(3) -0.0128(3) -0.0082(3) S1 0.0233(7) 0.0261(8) 0.0148(7) 0.0004(6) -0.0051(6) -0.0114(6) S2 0.0158(7) 0.0240(8) 0.0254(8) -0.0013(6) -0.0072(6) -0.0053(6) S3 0.0123(6) 0.0214(7) 0.0198(7) -0.0007(5) -0.0022(5) -0.0040(5) S4 0.0155(6) 0.0187(7) 0.0202(7) 0.0028(5) -0.0075(6) -0.0065(5) N1 0.026(3) 0.028(3) 0.023(3) 0.001(2) -0.013(2) -0.005(2) N2 0.019(3) 0.022(3) 0.021(3) 0.000(2) -0.007(2) -0.004(2) N3 0.020(3) 0.029(3) 0.022(3) -0.003(2) -0.010(2) -0.003(2) N4 0.014(2) 0.016(2) 0.018(2) -0.0012(19) -0.0047(19) -0.0049(19) C1 0.027(3) 0.028(3) 0.027(3) 0.000(3) -0.012(3) -0.006(3) C2 0.034(4) 0.024(3) 0.031(4) 0.004(3) -0.018(3) -0.011(3) C3 0.036(4) 0.021(3) 0.027(3) 0.001(3) -0.018(3) -0.007(3) C4 0.030(3) 0.020(3) 0.012(3) -0.001(2) -0.012(2) 0.000(2) C5 0.036(4) 0.025(3) 0.018(3) -0.003(2) -0.012(3) 0.003(3) C6 0.026(3) 0.033(4) 0.019(3) -0.003(3) -0.009(3) 0.005(3) C7 0.022(3) 0.033(4) 0.021(3) 0.004(3) -0.011(3) -0.002(3) C8 0.017(3) 0.042(4) 0.031(4) -0.002(3) -0.007(3) 0.001(3) C9 0.020(3) 0.045(4) 0.036(4) 0.009(3) -0.008(3) -0.013(3) C10 0.022(3) 0.032(4) 0.031(4) 0.007(3) -0.008(3) -0.006(3) C11 0.014(3) 0.028(3) 0.017(3) 0.004(2) -0.007(2) -0.005(2) C12 0.020(3) 0.031(3) 0.014(3) 0.001(2) -0.008(2) -0.003(3) C13 0.023(3) 0.022(3) 0.018(3) -0.002(2) -0.014(2) 0.001(2) C14 0.021(3) 0.022(3) 0.017(3) 0.003(2) -0.011(2) -0.004(2) C15 0.017(3) 0.030(3) 0.023(3) 0.001(3) -0.006(3) -0.001(3) C16 0.029(4) 0.023(3) 0.038(4) -0.006(3) -0.010(3) -0.005(3) C17 0.018(3) 0.030(3) 0.025(3) -0.006(3) -0.009(3) -0.001(3) C18 0.016(3) 0.035(4) 0.032(4) -0.005(3) -0.009(3) -0.003(3) C19 0.019(3) 0.037(4) 0.024(3) -0.008(3) -0.011(3) 0.007(3) C20 0.018(3) 0.028(3) 0.013(3) -0.003(2) -0.007(2) 0.001(2) C21 0.029(3) 0.023(3) 0.019(3) -0.006(2) -0.013(3) 0.007(3) C22 0.038(4) 0.017(3) 0.020(3) -0.001(2) -0.017(3) 0.001(3) C23 0.029(3) 0.019(3) 0.015(3) -0.001(2) -0.010(3) -0.003(2) C24 0.035(4) 0.020(3) 0.020(3) 0.002(2) -0.013(3) -0.008(3) C25 0.025(3) 0.026(3) 0.021(3) 0.002(2) -0.006(3) -0.011(3) C26 0.023(3) 0.024(3) 0.018(3) 0.000(2) -0.004(2) -0.006(3) C27 0.016(3) 0.015(3) 0.011(2) 0.001(2) -0.002(2) -0.004(2) C28 0.020(3) 0.020(3) 0.011(3) -0.001(2) -0.006(2) -0.001(2) C29 0.018(3) 0.022(3) 0.013(3) -0.004(2) -0.007(2) 0.005(2) C30 0.017(3) 0.018(3) 0.014(3) -0.003(2) -0.005(2) -0.006(2) C31 0.027(3) 0.016(3) 0.026(3) 0.004(2) -0.009(3) -0.009(2) C32 0.016(3) 0.024(3) 0.029(3) 0.000(3) -0.010(3) -0.002(2) Cl1 0.0260(7) 0.0193(7) 0.0187(7) -0.0026(5) -0.0074(6) -0.0015(6) O1 0.045(3) 0.028(3) 0.052(4) 0.012(2) -0.020(3) -0.015(2) O2 0.025(3) 0.058(4) 0.071(5) 0.028(3) -0.006(3) -0.003(3) O3 0.036(3) 0.031(3) 0.027(2) 0.004(2) -0.016(2) -0.006(2) O4 0.135(7) 0.029(3) 0.036(3) -0.013(3) -0.049(4) 0.013(4) Cl2 0.0604(13) 0.0576(13) 0.0603(13) 0.0354(11) -0.0474(12) -0.0430(11) O5 0.067(5) 0.128(8) 0.053(6) 0.023(5) -0.036(5) -0.067(6) O6 0.112(9) 0.058(5) 0.123(8) -0.014(5) -0.048(7) -0.012(7) O7 0.032(6) 0.057(5) 0.030(4) 0.005(4) -0.013(4) -0.018(5) O5' 0.067(5) 0.128(8) 0.053(6) 0.023(5) -0.036(5) -0.067(6) O6' 0.112(9) 0.058(5) 0.123(8) -0.014(5) -0.048(7) -0.012(7) O7' 0.032(6) 0.057(5) 0.030(4) 0.005(4) -0.013(4) -0.018(5) O8 0.044(3) 0.040(3) 0.044(3) 0.009(2) -0.020(3) -0.010(2) O9 0.021(2) 0.025(3) 0.054(3) -0.011(2) -0.002(2) -0.005(2) C33 0.022(3) 0.023(3) 0.039(4) -0.005(3) -0.009(3) -0.010(3) C34 0.048(5) 0.050(5) 0.031(4) -0.011(4) -0.016(4) 0.013(4) C35 0.032(4) 0.027(4) 0.040(4) 0.002(3) -0.011(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C11 2.032(6) . ? Pt1 N1 2.039(6) . ? Pt1 S2 2.3375(16) . ? Pt1 S1 2.3725(16) . ? Pt1 Ag2" 2.726(3) . ? Pt1 Ag1" 2.745(4) . ? Pt1 Ag2' 2.778(3) . ? Pt1 Ag1' 2.875(2) . ? Pt1 Ag1 3.061(3) . ? Pt1 Ag2 3.1211(9) . ? Pt2 C27 2.026(6) . ? Pt2 N3 2.033(5) . ? Pt2 S4 2.3441(15) . ? Pt2 S3 2.3499(15) . ? Pt2 Ag1" 2.611(4) . ? Pt2 Ag1' 2.760(2) . ? Pt2 Ag2" 2.872(3) . ? Pt2 Ag2' 2.940(3) . ? Pt2 Ag1 2.962(3) . ? Ag1 S1 2.536(3) . ? Ag1 S4 2.560(3) . ? Ag1 Ag2 2.581(3) . ? Ag2 O5 2.443(7) . ? Ag2 S3 2.5652(17) . ? Ag2 O2 2.593(6) . ? Ag2 S2 2.5932(18) . ? Ag1' O9 2.488(5) . ? Ag1' S1 2.563(3) . ? Ag1' S4 2.642(3) . ? Ag1' Ag2' 2.933(4) . ? Ag2' S3 2.640(3) . ? Ag2' S2 2.890(3) . ? Ag1" O9 2.410(6) . ? Ag1" S1 2.859(4) . ? Ag1" Ag2" 3.209(5) . ? Ag2" C11 2.562(6) . ? Ag2" S3 2.952(3) . ? S1 C14 1.744(6) . ? S2 C14 1.740(6) . ? S3 C30 1.754(6) . ? S4 C30 1.743(6) . ? N1 C1 1.359(9) . ? N1 C13 1.395(8) . ? N2 C14 1.301(8) . ? N2 C16 1.471(8) . ? N2 C15 1.473(8) . ? N3 C17 1.362(9) . ? N3 C29 1.384(8) . ? N4 C30 1.297(8) . ? N4 C32 1.471(8) . ? N4 C31 1.476(7) . ? C1 C2 1.400(9) . ? C1 H1 0.9500 . ? C2 C3 1.373(10) . ? C2 H2 0.9500 . ? C3 C4 1.413(9) . ? C3 H3 0.9500 . ? C4 C13 1.401(9) . ? C4 C5 1.431(9) . ? C5 C6 1.358(10) . ? C5 H5 0.9500 . ? C6 C7 1.424(10) . ? C6 H6 0.9500 . ? C7 C12 1.412(9) . ? C7 C8 1.419(10) . ? C8 C9 1.362(11) . ? C8 H8 0.9500 . ? C9 C10 1.405(10) . ? C9 H9 0.9500 . ? C10 C11 1.371(9) . ? C10 H10 0.9500 . ? C11 C12 1.383(9) . ? C12 C13 1.422(9) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.420(9) . ? C17 H17 0.9500 . ? C18 C19 1.374(10) . ? C18 H18 0.9500 . ? C19 C20 1.402(10) . ? C19 H19 0.9500 . ? C20 C29 1.418(8) . ? C20 C21 1.437(9) . ? C21 C22 1.346(10) . ? C21 H21 0.9500 . ? C22 C23 1.445(9) . ? C22 H22 0.9500 . ? C23 C24 1.396(9) . ? C23 C28 1.413(8) . ? C24 C25 1.385(9) . ? C24 H24 0.9500 . ? C25 C26 1.400(9) . ? C25 H25 0.9500 . ? C26 C27 1.366(8) . ? C26 H26 0.9500 . ? C27 C28 1.391(8) . ? C28 C29 1.420(9) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? Cl1 O4 1.416(5) . ? Cl1 O2 1.428(6) . ? Cl1 O1 1.430(5) . ? Cl1 O3 1.435(5) . ? Cl2 O5 1.393(5) . ? Cl2 O8 1.406(4) . ? Cl2 O6' 1.407(5) . ? Cl2 O7' 1.416(5) . ? Cl2 O7 1.417(5) . ? Cl2 O5' 1.449(5) . ? Cl2 O6 1.483(5) . ? O9 C33 1.214(8) . ? C33 C35 1.499(10) . ? C33 C34 1.503(11) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pt1 N1 81.2(2) . . ? C11 Pt1 S2 100.47(18) . . ? N1 Pt1 S2 178.03(17) . . ? C11 Pt1 S1 175.24(18) . . ? N1 Pt1 S1 103.02(17) . . ? S2 Pt1 S1 75.28(5) . . ? C11 Pt1 Ag2" 63.19(18) . . ? N1 Pt1 Ag2" 102.48(17) . . ? S2 Pt1 Ag2" 79.27(8) . . ? S1 Pt1 Ag2" 117.43(8) . . ? C11 Pt1 Ag1" 116.62(19) . . ? N1 Pt1 Ag1" 67.26(19) . . ? S2 Pt1 Ag1" 112.68(12) . . ? S1 Pt1 Ag1" 67.47(10) . . ? Ag2" Pt1 Ag1" 71.81(10) . . ? C11 Pt1 Ag2' 76.12(18) . . ? N1 Pt1 Ag2' 113.40(17) . . ? S2 Pt1 Ag2' 68.16(9) . . ? S1 Pt1 Ag2' 103.88(9) . . ? Ag2" Pt1 Ag2' 14.96(8) . . ? Ag1" Pt1 Ag2' 69.28(11) . . ? C11 Pt1 Ag1' 125.68(17) . . ? N1 Pt1 Ag1' 84.48(16) . . ? S2 Pt1 Ag1' 95.35(6) . . ? S1 Pt1 Ag1' 57.52(6) . . ? Ag2" Pt1 Ag1' 69.50(8) . . ? Ag1" Pt1 Ag1' 17.57(10) . . ? Ag2' Pt1 Ag1' 62.49(8) . . ? C11 Pt1 Ag1 128.42(17) . . ? N1 Pt1 Ag1 95.76(16) . . ? S2 Pt1 Ag1 84.05(5) . . ? S1 Pt1 Ag1 53.87(6) . . ? Ag2" Pt1 Ag1 67.49(8) . . ? Ag1" Pt1 Ag1 28.81(11) . . ? Ag2' Pt1 Ag1 57.88(9) . . ? Ag1' Pt1 Ag1 11.31(5) . . ? C11 Pt1 Ag2 92.04(17) . . ? N1 Pt1 Ag2 126.73(15) . . ? S2 Pt1 Ag2 54.46(4) . . ? S1 Pt1 Ag2 87.19(4) . . ? Ag2" Pt1 Ag2 33.68(7) . . ? Ag1" Pt1 Ag2 69.37(10) . . ? Ag2' Pt1 Ag2 18.74(8) . . ? Ag1' Pt1 Ag2 57.31(5) . . ? Ag1 Pt1 Ag2 49.33(5) . . ? C27 Pt2 N3 81.5(2) . . ? C27 Pt2 S4 100.47(16) . . ? N3 Pt2 S4 176.83(16) . . ? C27 Pt2 S3 175.45(17) . . ? N3 Pt2 S3 102.00(16) . . ? S4 Pt2 S3 75.86(5) . . ? C27 Pt2 Ag1" 70.92(19) . . ? N3 Pt2 Ag1" 109.08(18) . . ? S4 Pt2 Ag1" 73.96(11) . . ? S3 Pt2 Ag1" 110.19(12) . . ? C27 Pt2 Ag1' 87.39(16) . . ? N3 Pt2 Ag1' 121.00(16) . . ? S4 Pt2 Ag1' 61.71(6) . . ? S3 Pt2 Ag1' 93.14(6) . . ? Ag1" Pt2 Ag1' 18.32(11) . . ? C27 Pt2 Ag2" 116.35(17) . . ? N3 Pt2 Ag2" 65.16(16) . . ? S4 Pt2 Ag2" 115.67(8) . . ? S3 Pt2 Ag2" 67.98(7) . . ? Ag1" Pt2 Ag2" 71.46(10) . . ? Ag1' Pt2 Ag2" 69.08(8) . . ? C27 Pt2 Ag2' 125.32(17) . . ? N3 Pt2 Ag2' 78.64(17) . . ? S4 Pt2 Ag2' 101.97(9) . . ? S3 Pt2 Ag2' 58.61(8) . . ? Ag1" Pt2 Ag2' 68.61(11) . . ? Ag1' Pt2 Ag2' 61.85(8) . . ? Ag2" Pt2 Ag2' 14.13(7) . . ? C27 Pt2 Ag1 98.47(16) . . ? N3 Pt2 Ag1 126.05(16) . . ? S4 Pt2 Ag1 56.25(6) . . ? S3 Pt2 Ag1 81.82(6) . . ? Ag1" Pt2 Ag1 29.88(12) . . ? Ag1' Pt2 Ag1 11.62(6) . . ? Ag2" Pt2 Ag1 67.13(8) . . ? Ag2' Pt2 Ag1 57.45(9) . . ? S1 Ag1 S4 162.19(13) . . ? S1 Ag1 Ag2 96.81(10) . . ? S4 Ag1 Ag2 100.58(10) . . ? S1 Ag1 Pt2 141.06(10) . . ? S4 Ag1 Pt2 49.58(6) . . ? Ag2 Ag1 Pt2 74.59(7) . . ? S1 Ag1 Pt1 49.06(6) . . ? S4 Ag1 Pt1 143.67(10) . . ? Ag2 Ag1 Pt1 66.55(7) . . ? Pt2 Ag1 Pt1 94.20(7) . . ? O5 Ag2 S3 84.1(2) . . ? O5 Ag2 Ag1 162.1(3) . . ? S3 Ag2 Ag1 85.99(7) . . ? O5 Ag2 O2 102.9(3) . . ? S3 Ag2 O2 85.60(18) . . ? Ag1 Ag2 O2 91.12(15) . . ? O5 Ag2 S2 99.7(2) . . ? S3 Ag2 S2 175.72(6) . . ? Ag1 Ag2 S2 89.85(7) . . ? O2 Ag2 S2 95.52(17) . . ? O5 Ag2 Pt1 112.0(3) . . ? S3 Ag2 Pt1 129.48(5) . . ? Ag1 Ag2 Pt1 64.12(6) . . ? O2 Ag2 Pt1 131.43(15) . . ? S2 Ag2 Pt1 47.18(4) . . ? O9 Ag1' S1 80.35(16) . . ? O9 Ag1' S4 93.91(16) . . ? S1 Ag1' S4 150.66(11) . . ? O9 Ag1' Pt2 119.33(15) . . ? S1 Ag1' Pt2 153.96(11) . . ? S4 Ag1' Pt2 51.38(5) . . ? O9 Ag1' Pt1 112.52(16) . . ? S1 Ag1' Pt1 51.35(6) . . ? S4 Ag1' Pt1 151.14(10) . . ? Pt2 Ag1' Pt1 103.07(8) . . ? O9 Ag1' Ag2' 168.23(17) . . ? S1 Ag1' Ag2' 95.11(10) . . ? S4 Ag1' Ag2' 95.23(10) . . ? Pt2 Ag1' Ag2' 62.09(8) . . ? Pt1 Ag1' Ag2' 57.15(8) . . ? S3 Ag2' Pt1 143.63(14) . . ? S3 Ag2' S2 137.52(16) . . ? Pt1 Ag2' S2 48.66(6) . . ? S3 Ag2' Ag1' 83.61(11) . . ? Pt1 Ag2' Ag1' 60.37(8) . . ? S2 Ag2' Ag1' 83.32(10) . . ? S3 Ag2' Pt2 49.45(6) . . ? Pt1 Ag2' Pt2 100.97(11) . . ? S2 Ag2' Pt2 139.20(13) . . ? Ag1' Ag2' Pt2 56.06(8) . . ? O9 Ag1" Pt2 128.9(2) . . ? O9 Ag1" Pt1 119.9(2) . . ? Pt2 Ag1" Pt1 110.92(14) . . ? O9 Ag1" S1 75.88(17) . . ? Pt2 Ag1" S1 142.9(2) . . ? Pt1 Ag1" S1 50.04(7) . . ? O9 Ag1" Ag2" 164.7(2) . . ? Pt2 Ag1" Ag2" 58.06(9) . . ? Pt1 Ag1" Ag2" 53.81(8) . . ? S1 Ag1" Ag2" 91.71(13) . . ? C11 Ag2" Pt1 45.06(14) . . ? C11 Ag2" Pt2 123.90(18) . . ? Pt1 Ag2" Pt2 104.01(9) . . ? C11 Ag2" S3 171.14(18) . . ? Pt1 Ag2" S3 130.07(12) . . ? Pt2 Ag2" S3 47.57(5) . . ? C11 Ag2" Ag1" 89.32(17) . . ? Pt1 Ag2" Ag1" 54.37(8) . . ? Pt2 Ag2" Ag1" 50.48(8) . . ? S3 Ag2" Ag1" 82.61(11) . . ? C14 S1 Pt1 86.0(2) . . ? C14 S1 Ag1 95.2(2) . . ? Pt1 S1 Ag1 77.07(7) . . ? C14 S1 Ag1' 106.7(2) . . ? Pt1 S1 Ag1' 71.14(7) . . ? Ag1 S1 Ag1' 13.80(6) . . ? C14 S1 Ag1" 118.9(2) . . ? Pt1 S1 Ag1" 62.49(9) . . ? Ag1 S1 Ag1" 31.03(10) . . ? Ag1' S1 Ag1" 17.33(9) . . ? C14 S2 Pt1 87.2(2) . . ? C14 S2 Ag2 99.3(2) . . ? Pt1 S2 Ag2 78.35(5) . . ? C14 S2 Ag2' 110.5(2) . . ? Pt1 S2 Ag2' 63.18(8) . . ? Ag2 S2 Ag2' 20.50(8) . . ? C30 S3 Pt2 85.7(2) . . ? C30 S3 Ag2 102.72(19) . . ? Pt2 S3 Ag2 86.52(5) . . ? C30 S3 Ag2' 117.3(2) . . ? Pt2 S3 Ag2' 71.93(9) . . ? Ag2 S3 Ag2' 22.51(9) . . ? C30 S3 Ag2" 125.1(2) . . ? Pt2 S3 Ag2" 64.45(7) . . ? Ag2 S3 Ag2" 35.81(7) . . ? Ag2' S3 Ag2" 13.31(8) . . ? C30 S4 Pt2 86.1(2) . . ? C30 S4 Ag1 95.0(2) . . ? Pt2 S4 Ag1 74.17(7) . . ? C30 S4 Ag1' 105.1(2) . . ? Pt2 S4 Ag1' 66.91(7) . . ? Ag1 S4 Ag1' 13.42(6) . . ? C1 N1 C13 117.5(6) . . ? C1 N1 Pt1 129.4(5) . . ? C13 N1 Pt1 113.1(4) . . ? C14 N2 C16 120.5(5) . . ? C14 N2 C15 122.2(5) . . ? C16 N2 C15 117.3(5) . . ? C17 N3 C29 118.7(5) . . ? C17 N3 Pt2 128.2(5) . . ? C29 N3 Pt2 113.0(4) . . ? C30 N4 C32 122.3(5) . . ? C30 N4 C31 121.8(5) . . ? C32 N4 C31 115.9(5) . . ? N1 C1 C2 121.3(6) . . ? N1 C1 H1 119.4 . . ? C2 C1 H1 119.4 . . ? C3 C2 C1 120.9(6) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 119.9(6) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C13 C4 C3 116.8(6) . . ? C13 C4 C5 118.1(6) . . ? C3 C4 C5 125.1(6) . . ? C6 C5 C4 121.0(6) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 122.0(6) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C12 C7 C8 116.9(6) . . ? C12 C7 C6 117.8(6) . . ? C8 C7 C6 125.3(6) . . ? C9 C8 C7 119.8(6) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 121.6(7) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C11 C10 C9 120.1(7) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 118.6(6) . . ? C10 C11 Pt1 128.3(5) . . ? C12 C11 Pt1 113.2(4) . . ? C10 C11 Ag2" 87.1(4) . . ? C12 C11 Ag2" 116.3(4) . . ? Pt1 C11 Ag2" 71.75(19) . . ? C11 C12 C7 122.9(6) . . ? C11 C12 C13 116.8(6) . . ? C7 C12 C13 120.2(6) . . ? N1 C13 C4 123.6(6) . . ? N1 C13 C12 115.6(6) . . ? C4 C13 C12 120.8(6) . . ? N2 C14 S2 124.1(5) . . ? N2 C14 S1 124.5(5) . . ? S2 C14 S1 111.3(3) . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 120.1(6) . . ? N3 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 121.0(6) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 120.2(6) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C29 117.0(6) . . ? C19 C20 C21 125.8(6) . . ? C29 C20 C21 117.2(6) . . ? C22 C21 C20 121.9(6) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 121.9(6) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C24 C23 C28 117.8(6) . . ? C24 C23 C22 125.0(6) . . ? C28 C23 C22 117.2(6) . . ? C25 C24 C23 119.8(6) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 120.6(6) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 121.2(6) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 117.9(5) . . ? C26 C27 Pt2 129.4(5) . . ? C28 C27 Pt2 112.7(4) . . ? C27 C28 C23 122.6(6) . . ? C27 C28 C29 116.6(5) . . ? C23 C28 C29 120.7(5) . . ? N3 C29 C20 123.0(6) . . ? N3 C29 C28 116.1(5) . . ? C20 C29 C28 120.9(6) . . ? N4 C30 S4 124.5(4) . . ? N4 C30 S3 124.1(5) . . ? S4 C30 S3 111.2(3) . . ? N4 C31 H31A 109.5 . . ? N4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N4 C32 H32A 109.5 . . ? N4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O4 Cl1 O2 109.9(5) . . ? O4 Cl1 O1 109.6(4) . . ? O2 Cl1 O1 108.6(4) . . ? O4 Cl1 O3 109.2(3) . . ? O2 Cl1 O3 109.0(3) . . ? O1 Cl1 O3 110.6(3) . . ? Cl1 O2 Ag2 125.2(4) . . ? O5 Cl2 O8 117.7(5) . . ? O5 Cl2 O6' 66.3(8) . . ? O8 Cl2 O6' 112.6(6) . . ? O5 Cl2 O7' 125.3(7) . . ? O8 Cl2 O7' 112.7(6) . . ? O6' Cl2 O7' 112.0(7) . . ? O5 Cl2 O7 114.4(5) . . ? O8 Cl2 O7 112.3(5) . . ? O6' Cl2 O7 126.3(8) . . ? O7' Cl2 O7 20.2(7) . . ? O5 Cl2 O5' 42.2(7) . . ? O8 Cl2 O5' 103.3(5) . . ? O6' Cl2 O5' 108.5(6) . . ? O7' Cl2 O5' 107.2(6) . . ? O7 Cl2 O5' 88.1(7) . . ? O5 Cl2 O6 103.2(5) . . ? O8 Cl2 O6 101.8(5) . . ? O6' Cl2 O6 37.5(8) . . ? O7' Cl2 O6 85.6(8) . . ? O7 Cl2 O6 105.2(5) . . ? O5' Cl2 O6 144.4(7) . . ? Cl2 O5 Ag2 149.5(7) . . ? C33 O9 Ag1" 136.4(5) . . ? C33 O9 Ag1' 116.5(4) . . ? Ag1" O9 Ag1' 20.33(13) . . ? O9 C33 C35 121.7(7) . . ? O9 C33 C34 121.0(7) . . ? C35 C33 C34 117.3(6) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 4.166 _refine_diff_density_min -3.580 _refine_diff_density_rms 0.185 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 798312' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H35 Ag Cl N5 O4 Pt2 S4' _chemical_formula_weight 1287.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.9857(2) _cell_length_b 12.3660(2) _cell_length_c 14.5156(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.398(2) _cell_angle_gamma 90.00 _cell_volume 1959.65(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12893 _cell_measurement_theta_min 4.2298 _cell_measurement_theta_max 28.7455 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 7.946 _exptl_absorpt_correction_T_min 0.1920 _exptl_absorpt_correction_T_max 0.6062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.0655 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21819 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 28.81 _diffrn_orient_matrix_UB_11 -0.0430169000 _diffrn_orient_matrix_UB_12 0.0425032000 _diffrn_orient_matrix_UB_13 -0.0089861000 _diffrn_orient_matrix_UB_21 -0.0486768000 _diffrn_orient_matrix_UB_22 -0.0376182000 _diffrn_orient_matrix_UB_23 0.0004184000 _diffrn_orient_matrix_UB_31 -0.0002104000 _diffrn_orient_matrix_UB_32 0.0082333000 _diffrn_orient_matrix_UB_33 0.0483530000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 61.00 102.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 179.0000 -180.0000 41 #__ type_ start__ end____ width___ exp.time_ 2 omega -9.00 78.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 77.0000 -180.0000 87 #__ type_ start__ end____ width___ exp.time_ 3 omega -22.00 81.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 -14.0000 -83.0000 103 #__ type_ start__ end____ width___ exp.time_ 4 omega -102.00 -32.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 179.0000 30.0000 70 #__ type_ start__ end____ width___ exp.time_ 5 omega -102.00 -32.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 179.0000 150.0000 70 #__ type_ start__ end____ width___ exp.time_ 6 omega -10.00 96.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 37.0000 -30.0000 106 #__ type_ start__ end____ width___ exp.time_ 7 omega 34.00 62.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 179.0000 60.0000 28 #__ type_ start__ end____ width___ exp.time_ 8 omega -10.00 96.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 37.0000 90.0000 106 ; _reflns_number_total 8890 _reflns_number_gt 7524 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^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 constr _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 0.007(6) _refine_ls_number_reflns 8890 _refine_ls_number_parameters 497 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.60305(3) -0.32500(2) 0.02112(3) 0.03074(9) Uani 1 1 d . . . Pt2 Pt 0.22314(3) -0.45866(2) 0.09965(2) 0.02554(8) Uani 1 1 d . . . Ag Ag 0.44499(6) -0.49213(5) 0.03566(5) 0.03753(18) Uani 1 1 d . . . S1 S 0.5966(2) -0.3753(2) -0.13158(18) 0.0363(6) Uani 1 1 d . . . S2 S 0.4873(2) -0.18625(19) -0.0629(2) 0.0400(6) Uani 1 1 d . . . S3 S 0.2704(2) -0.27897(17) 0.11526(15) 0.0288(5) Uani 1 1 d . . . S4 S 0.2165(2) -0.42174(17) 0.26121(17) 0.0344(6) Uani 1 1 d . . . N1 N 0.6143(7) -0.2732(6) 0.1549(6) 0.0355(18) Uani 1 1 d . . . N2 N 0.5308(7) -0.2066(6) -0.2426(6) 0.0361(19) Uani 1 1 d . . . N3 N 0.1665(6) -0.6169(5) 0.0893(5) 0.0273(16) Uani 1 1 d . . . N4 N 0.2382(7) -0.2062(6) 0.2860(5) 0.0270(16) Uani 1 1 d . . . C1 C 0.7088(7) -0.4436(6) 0.0791(7) 0.033(2) Uani 1 1 d . . . C2 C 0.7651(8) -0.5286(6) 0.0388(7) 0.035(2) Uani 1 1 d . . . H2 H 0.7525 -0.5381 -0.0265 0.042 Uiso 1 1 calc R . . C3 C 0.8406(8) -0.6006(7) 0.0931(8) 0.038(2) Uani 1 1 d . . . H3 H 0.8747 -0.6606 0.0642 0.046 Uiso 1 1 calc R . . C4 C 0.8666(9) -0.5871(8) 0.1868(11) 0.059(4) Uani 1 1 d . . . H4 H 0.9207 -0.6358 0.2215 0.070 Uiso 1 1 calc R . . C5 C 0.8139(8) -0.5024(7) 0.2314(7) 0.036(2) Uani 1 1 d . . . C6 C 0.8348(9) -0.4799(8) 0.3302(7) 0.044(2) Uani 1 1 d . . . H6 H 0.8869 -0.5266 0.3687 0.053 Uiso 1 1 calc R . . C7 C 0.7831(10) -0.3955(9) 0.3690(8) 0.050(3) Uani 1 1 d . . . H7 H 0.7977 -0.3846 0.4340 0.060 Uiso 1 1 calc R . . C8 C 0.7030(8) -0.3188(9) 0.3110(7) 0.040(2) Uani 1 1 d . . . C9 C 0.6540(9) -0.2235(8) 0.3442(7) 0.044(3) Uani 1 1 d . . . H9 H 0.6661 -0.2065 0.4084 0.053 Uiso 1 1 calc R . . C10 C 0.5879(9) -0.1547(8) 0.2824(8) 0.043(3) Uani 1 1 d . . . H10 H 0.5555 -0.0894 0.3041 0.052 Uiso 1 1 calc R . . C11 C 0.5679(9) -0.1814(7) 0.1854(8) 0.041(2) Uani 1 1 d . . . H11 H 0.5219 -0.1342 0.1432 0.050 Uiso 1 1 calc R . . C12 C 0.6815(8) -0.3414(7) 0.2170(7) 0.036(2) Uani 1 1 d . . . C13 C 0.7346(8) -0.4336(6) 0.1768(8) 0.039(2) Uani 1 1 d . . . C14 C 0.5380(8) -0.2477(7) -0.1599(8) 0.039(2) Uani 1 1 d . . . C15 C 0.5728(10) -0.2661(9) -0.3212(7) 0.046(3) Uani 1 1 d . . . H15A H 0.5230 -0.3318 -0.3360 0.056 Uiso 1 1 calc R . . H15B H 0.6601 -0.2868 -0.3084 0.056 Uiso 1 1 calc R . . C16 C 0.5534(15) -0.1822(12) -0.3998(9) 0.078(4) Uani 1 1 d . . . H16A H 0.6303 -0.1422 -0.4054 0.094 Uiso 1 1 calc R . . H16B H 0.5272 -0.2182 -0.4596 0.094 Uiso 1 1 calc R . . C17 C 0.4559(15) -0.1069(13) -0.3744(9) 0.084(5) Uani 1 1 d . . . H17A H 0.3734 -0.1367 -0.3937 0.100 Uiso 1 1 calc R . . H17B H 0.4631 -0.0353 -0.4038 0.100 Uiso 1 1 calc R . . C18 C 0.4803(11) -0.0981(9) -0.2661(8) 0.053(3) Uani 1 1 d . . . H18A H 0.5402 -0.0404 -0.2467 0.063 Uiso 1 1 calc R . . H18B H 0.4037 -0.0849 -0.2379 0.063 Uiso 1 1 calc R . . C19 C 0.2137(7) -0.4728(8) -0.0399(6) 0.0294(19) Uani 1 1 d . . . C20 C 0.2324(8) -0.3981(7) -0.1079(7) 0.035(2) Uani 1 1 d . . . H20 H 0.2678 -0.3301 -0.0902 0.042 Uiso 1 1 calc R . . C21 C 0.2007(9) -0.4199(8) -0.2025(7) 0.039(2) Uani 1 1 d . . . H21 H 0.2153 -0.3671 -0.2475 0.047 Uiso 1 1 calc R . . C22 C 0.1478(9) -0.5187(9) -0.2307(8) 0.046(3) Uani 1 1 d . . . H22 H 0.1265 -0.5324 -0.2949 0.056 Uiso 1 1 calc R . . C23 C 0.1259(8) -0.5973(8) -0.1663(7) 0.036(2) Uani 1 1 d . . . C24 C 0.0729(8) -0.7016(9) -0.1874(8) 0.044(3) Uani 1 1 d . . . H24 H 0.0500 -0.7203 -0.2504 0.053 Uiso 1 1 calc R . . C25 C 0.0546(8) -0.7738(8) -0.1216(8) 0.043(3) Uani 1 1 d . . . H25 H 0.0192 -0.8417 -0.1395 0.052 Uiso 1 1 calc R . . C26 C 0.0861(7) -0.7520(6) -0.0263(7) 0.033(2) Uani 1 1 d . . . C27 C 0.0654(8) -0.8197(8) 0.0477(8) 0.046(3) Uani 1 1 d . . . H27 H 0.0295 -0.8888 0.0356 0.055 Uiso 1 1 calc R . . C28 C 0.0964(8) -0.7870(8) 0.1368(7) 0.040(2) Uani 1 1 d . . . H28 H 0.0833 -0.8343 0.1863 0.048 Uiso 1 1 calc R . . C29 C 0.1479(8) -0.6834(7) 0.1567(7) 0.035(2) Uani 1 1 d . . . H29 H 0.1690 -0.6620 0.2193 0.042 Uiso 1 1 calc R . . C30 C 0.1402(7) -0.6500(7) -0.0022(6) 0.0260(18) Uani 1 1 d . . . C31 C 0.1616(7) -0.5743(7) -0.0705(6) 0.030(2) Uani 1 1 d . . . C32 C 0.2437(8) -0.2894(7) 0.2300(6) 0.0293(19) Uani 1 1 d . . . C33 C 0.2534(9) -0.0946(7) 0.2578(7) 0.036(2) Uani 1 1 d . . . H33A H 0.1807 -0.0688 0.2174 0.043 Uiso 1 1 calc R . . H33B H 0.3270 -0.0861 0.2249 0.043 Uiso 1 1 calc R . . C34 C 0.2678(11) -0.0343(9) 0.3499(9) 0.054(3) Uani 1 1 d . . . H34A H 0.2368 0.0406 0.3420 0.065 Uiso 1 1 calc R . . H34B H 0.3548 -0.0321 0.3763 0.065 Uiso 1 1 calc R . . C35 C 0.1913(10) -0.0994(8) 0.4121(7) 0.042(2) Uani 1 1 d . . . H35A H 0.2203 -0.0879 0.4784 0.050 Uiso 1 1 calc R . . H35B H 0.1036 -0.0797 0.4008 0.050 Uiso 1 1 calc R . . C36 C 0.2121(10) -0.2148(7) 0.3836(6) 0.038(2) Uani 1 1 d . . . H36A H 0.2822 -0.2472 0.4227 0.045 Uiso 1 1 calc R . . H36B H 0.1382 -0.2594 0.3885 0.045 Uiso 1 1 calc R . . Cl Cl 0.9579(4) -0.2418(3) 0.5801(2) 0.0763(11) Uani 1 1 d . . . O1 O 1.0928(11) -0.2377(8) 0.6073(7) 0.090(3) Uani 1 1 d . . . O2 O 0.9023(9) -0.1594(10) 0.6332(7) 0.092(3) Uani 1 1 d . . . O3 O 0.9224(15) -0.3437(13) 0.5985(10) 0.164(7) Uani 1 1 d . . . O4 O 0.9473(8) -0.2153(6) 0.4873(6) 0.064(2) Uani 1 1 d . . . N5 N 0.5970(16) 0.0517(11) 0.4510(9) 0.100(5) Uani 1 1 d . . . C37 C 0.7018(18) 0.0444(11) 0.4677(8) 0.075(5) Uani 1 1 d . . . C38 C 0.8284(17) 0.0302(12) 0.4887(8) 0.084(4) Uani 1 1 d . . . H38A H 0.8501 0.0356 0.5559 0.126 Uiso 1 1 calc R . . H38B H 0.8719 0.0863 0.4576 0.126 Uiso 1 1 calc R . . H38C H 0.8518 -0.0412 0.4673 0.126 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 0.02116(16) 0.01752(15) 0.0560(2) -0.00613(16) 0.01523(15) -0.00337(14) Pt2 0.02256(16) 0.02124(15) 0.03297(17) -0.00346(15) 0.00373(12) 0.00089(13) Ag 0.0259(4) 0.0241(3) 0.0654(5) -0.0009(3) 0.0176(3) -0.0060(3) S1 0.0248(12) 0.0313(12) 0.0533(16) -0.0102(11) 0.0068(11) 0.0036(9) S2 0.0218(11) 0.0303(11) 0.0689(18) -0.0120(12) 0.0097(11) 0.0025(10) S3 0.0291(11) 0.0267(10) 0.0316(12) -0.0038(9) 0.0086(9) -0.0024(9) S4 0.0455(15) 0.0217(10) 0.0357(14) 0.0022(9) 0.0036(11) 0.0006(9) N1 0.022(4) 0.031(4) 0.056(5) -0.006(4) 0.012(3) -0.005(3) N2 0.024(4) 0.036(4) 0.048(5) -0.004(4) -0.003(3) 0.010(3) N3 0.015(3) 0.026(4) 0.040(4) 0.013(3) 0.002(3) 0.004(3) N4 0.026(4) 0.028(4) 0.027(4) 0.000(3) 0.004(3) -0.003(3) C1 0.015(4) 0.011(4) 0.073(7) -0.002(4) 0.010(4) -0.004(3) C2 0.025(5) 0.019(4) 0.064(7) 0.000(4) 0.022(4) -0.009(3) C3 0.027(5) 0.024(4) 0.066(7) 0.000(5) 0.011(5) 0.003(4) C4 0.025(5) 0.027(5) 0.127(12) 0.007(6) 0.024(6) 0.003(4) C5 0.027(5) 0.030(4) 0.054(6) 0.002(4) 0.018(4) -0.004(4) C6 0.038(5) 0.046(6) 0.052(6) 0.003(5) 0.023(4) 0.005(5) C7 0.043(6) 0.057(7) 0.051(7) -0.001(5) 0.009(5) -0.010(5) C8 0.031(5) 0.037(5) 0.053(6) -0.001(5) 0.013(4) -0.006(5) C9 0.033(5) 0.053(6) 0.048(6) -0.028(5) 0.016(5) -0.008(5) C10 0.034(6) 0.036(5) 0.059(7) -0.027(5) 0.006(5) -0.001(4) C11 0.031(5) 0.025(5) 0.071(7) -0.010(5) 0.016(5) -0.004(4) C12 0.025(5) 0.021(5) 0.065(7) 0.003(4) 0.021(4) -0.004(4) C13 0.030(5) 0.015(4) 0.075(7) -0.001(4) 0.018(5) -0.005(3) C14 0.018(5) 0.028(5) 0.072(8) -0.013(5) 0.005(4) 0.004(4) C15 0.044(6) 0.044(6) 0.051(7) -0.014(5) 0.008(5) 0.002(5) C16 0.106(12) 0.070(9) 0.058(8) 0.017(7) 0.009(8) 0.022(9) C17 0.094(11) 0.098(11) 0.058(9) 0.000(8) 0.003(7) 0.035(9) C18 0.041(6) 0.046(6) 0.068(8) 0.001(6) -0.008(5) 0.019(5) C19 0.018(4) 0.034(5) 0.037(5) 0.000(4) 0.006(3) -0.002(4) C20 0.027(5) 0.033(5) 0.046(6) -0.007(4) 0.004(4) 0.004(4) C21 0.030(5) 0.045(5) 0.044(6) 0.005(4) 0.009(4) 0.017(4) C22 0.026(5) 0.059(7) 0.052(7) -0.030(6) -0.001(5) 0.018(5) C23 0.022(5) 0.046(6) 0.041(6) -0.017(5) 0.002(4) 0.010(4) C24 0.014(4) 0.052(6) 0.066(7) -0.029(6) 0.000(4) 0.006(4) C25 0.021(5) 0.033(5) 0.076(8) -0.022(5) 0.010(5) -0.001(4) C26 0.013(4) 0.017(4) 0.072(7) -0.009(4) 0.009(4) 0.000(3) C27 0.024(4) 0.015(4) 0.104(9) -0.016(5) 0.027(5) 0.002(4) C28 0.026(5) 0.036(5) 0.059(7) -0.002(5) 0.018(4) 0.005(4) C29 0.034(5) 0.024(4) 0.049(6) 0.011(4) 0.017(4) 0.015(4) C30 0.013(4) 0.028(4) 0.037(5) -0.011(4) -0.002(3) 0.008(3) C31 0.013(4) 0.033(5) 0.045(6) -0.014(4) 0.009(4) 0.006(4) C32 0.024(4) 0.026(4) 0.038(5) 0.004(4) 0.000(4) -0.007(3) C33 0.035(5) 0.022(4) 0.054(6) -0.004(4) 0.017(4) 0.000(4) C34 0.045(7) 0.037(6) 0.084(9) -0.021(6) 0.022(6) 0.000(5) C35 0.055(7) 0.033(5) 0.039(6) -0.009(4) 0.012(5) -0.008(5) C36 0.045(6) 0.032(5) 0.036(6) 0.001(4) 0.003(4) 0.002(4) Cl 0.116(3) 0.0574(19) 0.052(2) 0.0055(15) -0.0069(19) -0.0287(19) O1 0.106(9) 0.067(6) 0.089(7) -0.005(5) -0.021(6) -0.005(6) O2 0.078(7) 0.128(9) 0.078(7) -0.004(6) 0.035(5) -0.007(6) O3 0.191(15) 0.143(14) 0.160(13) 0.042(10) 0.036(11) -0.101(12) O4 0.074(6) 0.050(5) 0.072(6) 0.001(4) 0.023(5) -0.015(4) N5 0.144(13) 0.069(8) 0.076(8) 0.032(7) -0.035(9) 0.002(10) C37 0.142(15) 0.037(6) 0.040(6) -0.002(6) -0.021(8) 0.009(10) C38 0.144(15) 0.062(8) 0.045(7) -0.013(7) 0.009(8) 0.014(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 1.997(8) . ? Pt1 N1 2.036(8) . ? Pt1 S1 2.296(3) . ? Pt1 S2 2.388(3) . ? Pt1 Ag 2.7226(7) . ? Pt2 C19 2.024(8) . ? Pt2 N3 2.053(7) . ? Pt2 S3 2.287(2) . ? Pt2 S4 2.398(3) . ? Pt2 Ag 2.7346(7) . ? Ag S2 2.531(2) 2_645 ? Ag C19 2.664(8) . ? S1 C14 1.736(10) . ? S2 C14 1.745(10) . ? S2 Ag 2.531(2) 2_655 ? S3 C32 1.728(9) . ? S4 C32 1.732(8) . ? N1 C11 1.339(12) . ? N1 C12 1.385(12) . ? N2 C14 1.298(13) . ? N2 C15 1.474(12) . ? N2 C18 1.477(12) . ? N3 C29 1.312(11) . ? N3 C30 1.389(11) . ? N4 C32 1.316(11) . ? N4 C33 1.455(11) . ? N4 C36 1.480(11) . ? C1 C2 1.382(12) . ? C1 C13 1.421(14) . ? C2 C3 1.399(13) . ? C2 H2 0.9500 . ? C3 C4 1.368(16) . ? C3 H3 0.9500 . ? C4 C5 1.391(14) . ? C4 H4 0.9500 . ? C5 C13 1.399(13) . ? C5 C6 1.453(14) . ? C6 C7 1.341(15) . ? C6 H6 0.9500 . ? C7 C8 1.490(15) . ? C7 H7 0.9500 . ? C8 C12 1.387(13) . ? C8 C9 1.403(14) . ? C9 C10 1.383(15) . ? C9 H9 0.9500 . ? C10 C11 1.439(14) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.434(12) . ? C15 C16 1.539(16) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.496(19) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.569(16) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.384(12) . ? C19 C31 1.430(12) . ? C20 C21 1.404(13) . ? C20 H20 0.9500 . ? C21 C22 1.394(14) . ? C21 H21 0.9500 . ? C22 C23 1.389(16) . ? C22 H22 0.9500 . ? C23 C31 1.431(13) . ? C23 C24 1.434(14) . ? C24 C25 1.338(15) . ? C24 H24 0.9500 . ? C25 C26 1.414(14) . ? C25 H25 0.9500 . ? C26 C27 1.399(14) . ? C26 C30 1.422(11) . ? C27 C28 1.362(14) . ? C27 H27 0.9500 . ? C28 C29 1.417(13) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.402(13) . ? C33 C34 1.522(14) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.529(15) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.510(13) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? Cl O3 1.355(13) . ? Cl O4 1.379(9) . ? Cl O2 1.453(11) . ? Cl O1 1.491(12) . ? N5 C37 1.15(2) . ? C37 C38 1.40(2) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 N1 81.9(3) . . ? C1 Pt1 S1 99.3(3) . . ? N1 Pt1 S1 176.9(2) . . ? C1 Pt1 S2 173.8(3) . . ? N1 Pt1 S2 103.5(2) . . ? S1 Pt1 S2 75.17(9) . . ? C1 Pt1 Ag 75.9(2) . . ? N1 Pt1 Ag 97.8(2) . . ? S1 Pt1 Ag 85.28(7) . . ? S2 Pt1 Ag 106.09(6) . . ? C19 Pt2 N3 82.2(3) . . ? C19 Pt2 S3 99.7(3) . . ? N3 Pt2 S3 175.1(2) . . ? C19 Pt2 S4 172.4(3) . . ? N3 Pt2 S4 102.2(2) . . ? S3 Pt2 S4 75.50(8) . . ? C19 Pt2 Ag 66.1(2) . . ? N3 Pt2 Ag 96.03(19) . . ? S3 Pt2 Ag 88.83(6) . . ? S4 Pt2 Ag 119.10(7) . . ? S2 Ag C19 113.6(2) 2_645 . ? S2 Ag Pt1 123.58(6) 2_645 . ? C19 Ag Pt1 119.2(2) . . ? S2 Ag Pt2 110.36(6) 2_645 . ? C19 Ag Pt2 44.02(18) . . ? Pt1 Ag Pt2 120.77(2) . . ? C14 S1 Pt1 87.3(4) . . ? C14 S2 Pt1 84.2(4) . . ? C14 S2 Ag 115.1(3) . 2_655 ? Pt1 S2 Ag 118.09(10) . 2_655 ? C32 S3 Pt2 87.8(3) . . ? C32 S4 Pt2 84.2(3) . . ? C11 N1 C12 119.7(9) . . ? C11 N1 Pt1 126.7(7) . . ? C12 N1 Pt1 113.6(6) . . ? C14 N2 C15 121.9(8) . . ? C14 N2 C18 123.5(9) . . ? C15 N2 C18 114.6(9) . . ? C29 N3 C30 119.6(8) . . ? C29 N3 Pt2 127.9(6) . . ? C30 N3 Pt2 112.4(5) . . ? C32 N4 C33 123.6(7) . . ? C32 N4 C36 124.2(7) . . ? C33 N4 C36 112.2(7) . . ? C2 C1 C13 116.1(8) . . ? C2 C1 Pt1 130.3(8) . . ? C13 C1 Pt1 113.5(6) . . ? C1 C2 C3 120.7(10) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 121.8(9) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 120.2(10) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C13 117.4(10) . . ? C4 C5 C6 125.1(10) . . ? C13 C5 C6 117.5(9) . . ? C7 C6 C5 122.4(10) . . ? C7 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C6 C7 C8 120.6(10) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C12 C8 C9 118.5(9) . . ? C12 C8 C7 116.9(9) . . ? C9 C8 C7 124.5(9) . . ? C10 C9 C8 119.2(9) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 120.3(9) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? N1 C11 C10 119.8(10) . . ? N1 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? N1 C12 C8 122.5(8) . . ? N1 C12 C13 115.5(9) . . ? C8 C12 C13 121.9(9) . . ? C5 C13 C1 123.7(8) . . ? C5 C13 C12 120.6(10) . . ? C1 C13 C12 115.5(8) . . ? N2 C14 S1 123.9(8) . . ? N2 C14 S2 125.7(7) . . ? S1 C14 S2 110.4(6) . . ? N2 C15 C16 101.9(9) . . ? N2 C15 H15A 111.4 . . ? C16 C15 H15A 111.4 . . ? N2 C15 H15B 111.4 . . ? C16 C15 H15B 111.4 . . ? H15A C15 H15B 109.2 . . ? C17 C16 C15 106.3(11) . . ? C17 C16 H16A 110.5 . . ? C15 C16 H16A 110.5 . . ? C17 C16 H16B 110.5 . . ? C15 C16 H16B 110.5 . . ? H16A C16 H16B 108.7 . . ? C16 C17 C18 104.1(10) . . ? C16 C17 H17A 110.9 . . ? C18 C17 H17A 110.9 . . ? C16 C17 H17B 110.9 . . ? C18 C17 H17B 110.9 . . ? H17A C17 H17B 109.0 . . ? N2 C18 C17 100.7(9) . . ? N2 C18 H18A 111.6 . . ? C17 C18 H18A 111.6 . . ? N2 C18 H18B 111.6 . . ? C17 C18 H18B 111.6 . . ? H18A C18 H18B 109.4 . . ? C20 C19 C31 116.8(8) . . ? C20 C19 Pt2 131.4(7) . . ? C31 C19 Pt2 111.1(6) . . ? C20 C19 Ag 98.2(6) . . ? C31 C19 Ag 112.3(6) . . ? Pt2 C19 Ag 69.9(2) . . ? C19 C20 C21 121.9(9) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C22 C21 C20 120.4(10) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.9(10) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C31 117.8(9) . . ? C22 C23 C24 125.7(10) . . ? C31 C23 C24 116.5(10) . . ? C25 C24 C23 122.5(10) . . ? C25 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? C24 C25 C26 122.1(9) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C27 C26 C25 126.5(8) . . ? C27 C26 C30 116.1(9) . . ? C25 C26 C30 117.4(9) . . ? C28 C27 C26 120.4(9) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.9(9) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? N3 C29 C28 120.4(9) . . ? N3 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? N3 C30 C31 116.4(7) . . ? N3 C30 C26 122.3(8) . . ? C31 C30 C26 121.1(8) . . ? C30 C31 C19 117.4(8) . . ? C30 C31 C23 120.3(8) . . ? C19 C31 C23 122.2(9) . . ? N4 C32 S3 124.1(6) . . ? N4 C32 S4 123.8(7) . . ? S3 C32 S4 112.1(5) . . ? N4 C33 C34 102.8(8) . . ? N4 C33 H33A 111.2 . . ? C34 C33 H33A 111.2 . . ? N4 C33 H33B 111.2 . . ? C34 C33 H33B 111.2 . . ? H33A C33 H33B 109.1 . . ? C33 C34 C35 104.5(8) . . ? C33 C34 H34A 110.9 . . ? C35 C34 H34A 110.9 . . ? C33 C34 H34B 110.9 . . ? C35 C34 H34B 110.9 . . ? H34A C34 H34B 108.9 . . ? C36 C35 C34 103.1(8) . . ? C36 C35 H35A 111.2 . . ? C34 C35 H35A 111.2 . . ? C36 C35 H35B 111.2 . . ? C34 C35 H35B 111.2 . . ? H35A C35 H35B 109.1 . . ? N4 C36 C35 104.2(7) . . ? N4 C36 H36A 110.9 . . ? C35 C36 H36A 110.9 . . ? N4 C36 H36B 110.9 . . ? C35 C36 H36B 110.9 . . ? H36A C36 H36B 108.9 . . ? O3 Cl O4 114.8(8) . . ? O3 Cl O2 113.6(9) . . ? O4 Cl O2 110.9(6) . . ? O3 Cl O1 106.2(9) . . ? O4 Cl O1 103.0(6) . . ? O2 Cl O1 107.4(6) . . ? N5 C37 C38 177.2(17) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.016 _refine_diff_density_min -1.263 _refine_diff_density_rms 0.162