# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Datong Song' _publ_contact_author_email DSONG@CHEM.UTORONTO.CA _publ_section_title ; Reductive Dearomatization of a Substituted Benzene Triggered by a Strong Oxidant ; _publ_author_name 'Datong Song' #===>END data_1b _database_code_depnum_ccdc_archive 'CCDC 743627' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H42 F12 N4 O4 Pt2' _chemical_formula_weight 1621.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c 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' '-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 32.542(2) _cell_length_b 11.9573(11) _cell_length_c 21.3780(17) _cell_angle_alpha 90.00 _cell_angle_beta 127.996(4) _cell_angle_gamma 90.00 _cell_volume 6555.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 26365 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 4.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8119 _exptl_absorpt_correction_T_max 0.9181 _exptl_absorpt_process_details 'Bruker Apex 2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26365 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7108 _reflns_number_gt 5084 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0517P)^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 7108 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt -0.500809(8) 0.729784(18) -0.038300(13) 0.02098(8) Uani 1 1 d . . . O1 O -0.43144(16) 1.1629(3) -0.1915(3) 0.0377(11) Uani 1 1 d . . . O2 O -0.26957(16) 1.0373(4) 0.1665(3) 0.0508(11) Uani 1 1 d . A . N1 N -0.46719(16) 0.7630(4) -0.0970(3) 0.0194(9) Uani 1 1 d . . . N2 N -0.41985(18) 0.7129(4) 0.0659(3) 0.0256(11) Uani 1 1 d . . . C1 C -0.4581(2) 0.6688(5) -0.1187(4) 0.0337(15) Uani 1 1 d . . . H1A H -0.4652 0.6006 -0.1041 0.040 Uiso 1 1 calc R . . C2 C -0.4389(3) 0.6622(6) -0.1610(4) 0.0435(18) Uani 1 1 d . . . H2A H -0.4326 0.5915 -0.1740 0.052 Uiso 1 1 calc R . . C3 C -0.4291(3) 0.7590(5) -0.1840(4) 0.0365(16) Uani 1 1 d . . . H3A H -0.4168 0.7566 -0.2144 0.044 Uiso 1 1 calc R . . C4 C -0.4375(2) 0.8611(5) -0.1620(3) 0.0265(13) Uani 1 1 d . . . C5 C -0.4286(2) 0.9609(5) -0.1864(4) 0.0271(13) Uani 1 1 d . . . H5A H -0.4166 0.9587 -0.2172 0.033 Uiso 1 1 calc R . . C6 C -0.4370(2) 1.0595(5) -0.1660(4) 0.0255(13) Uani 1 1 d . . . C7 C -0.4551(2) 1.0653(5) -0.1204(3) 0.0247(13) Uani 1 1 d . . . H7A H -0.4606 1.1363 -0.1068 0.030 Uiso 1 1 calc R . . C8 C -0.46468(18) 0.9702(5) -0.0956(3) 0.0192(11) Uani 1 1 d . . . C9 C -0.45693(19) 0.8633(5) -0.1176(3) 0.0209(12) Uani 1 1 d . . . C10 C -0.3860(3) 1.1860(6) -0.1784(4) 0.0367(15) Uani 1 1 d . . . C11 C -0.4046(2) 0.6067(5) 0.0861(4) 0.0329(15) Uani 1 1 d . . . H11A H -0.4305 0.5506 0.0664 0.039 Uiso 1 1 calc R . . C12 C -0.3524(2) 0.5741(6) 0.1347(4) 0.0406(16) Uani 1 1 d . . . H12A H -0.3432 0.4978 0.1490 0.049 Uiso 1 1 calc R . . C13 C -0.3152(2) 0.6522(6) 0.1612(4) 0.0353(16) Uani 1 1 d . . . H13A H -0.2795 0.6310 0.1932 0.042 Uiso 1 1 calc R . . C14 C -0.3294(2) 0.7662(5) 0.1412(3) 0.0269(13) Uani 1 1 d . . . C15 C -0.2918(2) 0.8505(6) 0.1644(4) 0.0323(15) Uani 1 1 d . . . H15A H -0.2558 0.8324 0.1963 0.039 Uiso 1 1 calc R . . C16 C -0.3077(2) 0.9557(5) 0.1409(4) 0.0316(14) Uani 1 1 d . . . C17 C -0.36057(19) 0.9867(5) 0.0964(3) 0.0241(12) Uani 1 1 d . . . H17A H -0.3704 1.0627 0.0819 0.029 Uiso 1 1 calc R . . C18 C -0.3976(2) 0.9078(5) 0.0741(3) 0.0216(12) Uani 1 1 d . . . C19 C -0.3829(2) 0.7937(5) 0.0940(3) 0.0212(12) Uani 1 1 d . . . C20 C -0.2690(3) 1.0895(7) 0.1148(4) 0.0508(11) Uani 1 1 d . . . C21 C -0.45254(19) 0.9472(4) 0.0330(3) 0.0205(12) Uani 1 1 d . . . C22 C -0.4700(2) 0.9646(4) 0.0775(3) 0.0201(11) Uani 1 1 d . . . H22A H -0.4490 0.9398 0.1311 0.024 Uiso 1 1 calc R . . C23 C -0.48320(19) 0.9835(4) -0.0468(3) 0.0184(11) Uani 1 1 d . . . C24 C -0.5708(2) 0.7189(5) -0.1446(3) 0.0277(13) Uani 1 1 d . . . C25 C -0.6065(2) 0.8053(5) -0.1840(4) 0.0307(14) Uani 1 1 d . . . H25A H -0.5981 0.8762 -0.1588 0.037 Uiso 1 1 calc R . . C26 C -0.6545(2) 0.7925(6) -0.2594(4) 0.0377(16) Uani 1 1 d . . . H26A H -0.6779 0.8541 -0.2839 0.045 Uiso 1 1 calc R . . C27 C -0.6683(2) 0.6909(6) -0.2986(4) 0.0416(17) Uani 1 1 d . . . H27A H -0.7005 0.6816 -0.3500 0.050 Uiso 1 1 calc R . . C28 C -0.6328(2) 0.6023(6) -0.2598(4) 0.0385(16) Uani 1 1 d . . . H28A H -0.6415 0.5315 -0.2852 0.046 Uiso 1 1 calc R . . C29 C -0.5856(2) 0.6151(5) -0.1857(3) 0.0295(14) Uani 1 1 d . . . H29A H -0.5625 0.5532 -0.1614 0.035 Uiso 1 1 calc R . . C30 C -0.5313(2) 0.6847(5) 0.0173(3) 0.0249(12) Uani 1 1 d . . . C31 C -0.5837(2) 0.6767(5) -0.0197(4) 0.0347(15) Uani 1 1 d . . . H31A H -0.6074 0.6929 -0.0749 0.042 Uiso 1 1 calc R . . C32 C -0.6041(3) 0.6457(6) 0.0200(4) 0.0415(17) Uani 1 1 d . . . H32A H -0.6407 0.6411 -0.0079 0.050 Uiso 1 1 calc R . . C33 C -0.5700(3) 0.6225(5) 0.0997(5) 0.0432(18) Uani 1 1 d . . . H33A H -0.5829 0.5992 0.1272 0.052 Uiso 1 1 calc R . . C34 C -0.5173(3) 0.6329(5) 0.1397(4) 0.0384(16) Uani 1 1 d . . . H34A H -0.4938 0.6187 0.1951 0.046 Uiso 1 1 calc R . . C35 C -0.4979(2) 0.6641(5) 0.0994(4) 0.0332(15) Uani 1 1 d . . . H35A H -0.4613 0.6715 0.1281 0.040 Uiso 1 1 calc R . . F1 F -0.38712(18) 1.2907(3) -0.1980(3) 0.0595(12) Uani 1 1 d . . . F2 F -0.37917(16) 1.1237(3) -0.2230(3) 0.0572(12) Uani 1 1 d . . . F3 F -0.34561(16) 1.1709(5) -0.1045(3) 0.0724(14) Uani 1 1 d . . . F4 F -0.2282(4) 1.1660(9) 0.1536(7) 0.0616(10) Uiso 0.50 1 d P A 1 F5 F -0.3093(4) 1.1245(8) 0.0458(6) 0.0616(10) Uiso 0.50 1 d P A 1 F6 F -0.2515(3) 1.0053(8) 0.0850(5) 0.0616(10) Uiso 0.50 1 d P A 1 F4A F -0.2250(4) 1.1359(9) 0.1418(7) 0.0616(10) Uiso 0.50 1 d P A 2 F5A F -0.3072(4) 1.1595(8) 0.0704(6) 0.0616(10) Uiso 0.50 1 d P A 2 F6A F -0.2786(3) 1.0150(8) 0.0527(5) 0.0616(10) Uiso 0.50 1 d P A 2 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 0.02500(12) 0.01949(12) 0.02350(13) 0.00154(10) 0.01748(10) 0.00110(10) O1 0.048(3) 0.029(3) 0.058(3) 0.005(2) 0.043(2) 0.000(2) O2 0.031(2) 0.063(3) 0.042(3) 0.004(2) 0.015(2) -0.0122(19) N1 0.023(2) 0.021(2) 0.024(2) 0.003(2) 0.019(2) 0.0012(19) N2 0.029(3) 0.024(3) 0.028(3) 0.007(2) 0.020(2) 0.005(2) C1 0.048(4) 0.023(4) 0.045(4) 0.003(3) 0.036(4) 0.002(3) C2 0.073(5) 0.027(4) 0.069(5) 0.001(3) 0.063(4) 0.006(3) C3 0.049(4) 0.036(4) 0.048(4) -0.001(3) 0.041(4) 0.008(3) C4 0.027(3) 0.029(3) 0.026(3) 0.004(3) 0.017(3) 0.005(2) C5 0.031(3) 0.030(4) 0.034(3) 0.000(3) 0.027(3) 0.001(3) C6 0.026(3) 0.018(3) 0.034(3) 0.007(3) 0.020(3) -0.001(2) C7 0.027(3) 0.025(3) 0.029(3) 0.001(3) 0.021(3) 0.002(2) C8 0.014(3) 0.026(3) 0.015(3) -0.001(2) 0.007(2) 0.002(2) C9 0.016(3) 0.026(3) 0.023(3) -0.001(2) 0.013(2) 0.001(2) C10 0.051(4) 0.030(4) 0.038(4) -0.008(3) 0.032(4) -0.013(3) C11 0.039(4) 0.026(4) 0.040(4) 0.013(3) 0.027(3) 0.009(3) C12 0.044(4) 0.037(4) 0.043(4) 0.016(3) 0.028(4) 0.014(3) C13 0.026(3) 0.045(4) 0.028(4) 0.019(3) 0.014(3) 0.019(3) C14 0.023(3) 0.034(3) 0.022(3) 0.003(3) 0.013(3) 0.005(3) C15 0.018(3) 0.048(4) 0.027(3) 0.010(3) 0.012(3) 0.012(3) C16 0.029(3) 0.040(4) 0.029(3) -0.009(3) 0.020(3) -0.010(3) C17 0.023(3) 0.030(3) 0.021(3) -0.001(2) 0.014(3) 0.003(2) C18 0.026(3) 0.025(3) 0.018(3) 0.000(2) 0.015(3) 0.002(2) C19 0.025(3) 0.026(4) 0.016(3) 0.003(2) 0.014(2) 0.006(2) C20 0.031(2) 0.063(3) 0.042(3) 0.004(2) 0.015(2) -0.0122(19) C21 0.014(3) 0.020(3) 0.023(3) -0.001(2) 0.009(2) -0.002(2) C22 0.023(3) 0.019(3) 0.016(3) 0.001(2) 0.011(2) 0.001(2) C23 0.022(3) 0.015(3) 0.020(3) 0.000(2) 0.014(2) -0.001(2) C24 0.034(3) 0.032(4) 0.026(3) 0.001(3) 0.023(3) -0.005(3) C25 0.035(3) 0.032(4) 0.033(4) -0.005(3) 0.025(3) -0.002(3) C26 0.025(3) 0.054(5) 0.034(4) 0.004(3) 0.018(3) 0.003(3) C27 0.033(4) 0.062(5) 0.033(4) -0.009(4) 0.022(3) -0.015(3) C28 0.047(4) 0.037(4) 0.040(4) -0.012(3) 0.032(4) -0.021(3) C29 0.040(4) 0.026(3) 0.030(4) 0.000(3) 0.025(3) -0.007(3) C30 0.033(3) 0.016(3) 0.032(3) -0.004(3) 0.023(3) -0.002(2) C31 0.040(4) 0.034(4) 0.038(4) -0.001(3) 0.028(3) -0.007(3) C32 0.048(4) 0.046(4) 0.050(5) 0.001(3) 0.039(4) -0.008(3) C33 0.074(5) 0.022(4) 0.071(5) 0.005(3) 0.064(5) 0.002(3) C34 0.064(5) 0.030(4) 0.037(4) 0.008(3) 0.039(4) 0.008(3) C35 0.043(4) 0.026(4) 0.039(4) 0.002(3) 0.029(3) 0.006(3) F1 0.094(3) 0.033(3) 0.094(4) 0.000(2) 0.079(3) -0.014(2) F2 0.078(3) 0.052(3) 0.082(3) -0.025(2) 0.070(3) -0.023(2) F3 0.057(3) 0.098(4) 0.045(3) -0.002(3) 0.023(2) -0.035(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 C24 1.998(6) . ? Pt1 C30 2.034(5) . ? Pt1 N1 2.150(4) . ? Pt1 N2 2.172(5) . ? O1 C10 1.352(7) . ? O1 C6 1.407(7) . ? O2 C20 1.279(8) . ? O2 C16 1.398(7) . ? N1 C1 1.320(7) . ? N1 C9 1.387(7) . ? N2 C11 1.334(7) . ? N2 C19 1.361(7) . ? C1 C2 1.383(8) . ? C2 C3 1.369(9) . ? C3 C4 1.395(8) . ? C4 C5 1.401(8) . ? C4 C9 1.429(7) . ? C5 C6 1.343(8) . ? C6 C7 1.416(7) . ? C7 C8 1.370(8) . ? C8 C9 1.437(7) . ? C8 C23 1.501(7) . ? C10 F3 1.304(8) . ? C10 F1 1.314(8) . ? C10 F2 1.334(7) . ? C11 C12 1.394(8) . ? C12 C13 1.346(9) . ? C13 C14 1.418(9) . ? C14 C19 1.412(7) . ? C14 C15 1.419(8) . ? C15 C16 1.334(9) . ? C16 C17 1.410(8) . ? C17 C18 1.365(7) . ? C18 C19 1.421(8) . ? C18 C21 1.502(7) . ? C20 F4A 1.294(12) . ? C20 F5 1.299(12) . ? C20 F5A 1.301(12) . ? C20 F4 1.389(13) . ? C20 F6A 1.465(12) . ? C20 F6 1.479(12) . ? C21 C22 1.393(7) . ? C21 C23 1.414(7) . ? C22 C23 1.379(7) 5_475 ? C23 C22 1.379(7) 5_475 ? C24 C25 1.387(9) . ? C24 C29 1.423(8) . ? C25 C26 1.401(8) . ? C26 C27 1.385(10) . ? C27 C28 1.402(10) . ? C28 C29 1.376(8) . ? C30 C31 1.372(8) . ? C30 C35 1.405(8) . ? C31 C32 1.413(8) . ? C32 C33 1.372(10) . ? C33 C34 1.373(9) . ? C34 C35 1.395(8) . ? 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 C24 Pt1 C30 91.3(2) . . ? C24 Pt1 N1 88.93(19) . . ? C30 Pt1 N1 175.23(19) . . ? C24 Pt1 N2 166.8(2) . . ? C30 Pt1 N2 95.5(2) . . ? N1 Pt1 N2 83.36(17) . . ? C10 O1 C6 118.9(5) . . ? C20 O2 C16 118.9(5) . . ? C1 N1 C9 118.5(5) . . ? C1 N1 Pt1 110.6(4) . . ? C9 N1 Pt1 130.8(3) . . ? C11 N2 C19 118.8(5) . . ? C11 N2 Pt1 113.3(4) . . ? C19 N2 Pt1 124.8(4) . . ? N1 C1 C2 124.6(6) . . ? C3 C2 C1 119.0(6) . . ? C2 C3 C4 118.8(6) . . ? C3 C4 C5 119.4(5) . . ? C3 C4 C9 119.9(5) . . ? C5 C4 C9 120.6(5) . . ? C6 C5 C4 119.9(5) . . ? C5 C6 O1 123.1(5) . . ? C5 C6 C7 121.3(5) . . ? O1 C6 C7 115.5(5) . . ? C8 C7 C6 121.1(5) . . ? C7 C8 C9 118.9(5) . . ? C7 C8 C23 117.8(5) . . ? C9 C8 C23 123.3(5) . . ? N1 C9 C4 119.1(5) . . ? N1 C9 C8 122.7(5) . . ? C4 C9 C8 118.2(5) . . ? F3 C10 F1 109.1(5) . . ? F3 C10 F2 107.5(6) . . ? F1 C10 F2 106.7(5) . . ? F3 C10 O1 112.5(5) . . ? F1 C10 O1 108.5(5) . . ? F2 C10 O1 112.4(5) . . ? N2 C11 C12 123.2(6) . . ? C13 C12 C11 119.2(6) . . ? C12 C13 C14 119.8(5) . . ? C19 C14 C13 118.0(5) . . ? C19 C14 C15 120.1(5) . . ? C13 C14 C15 121.8(5) . . ? C16 C15 C14 119.2(5) . . ? C15 C16 O2 117.8(5) . . ? C15 C16 C17 122.0(5) . . ? O2 C16 C17 120.1(6) . . ? C18 C17 C16 120.2(5) . . ? C17 C18 C19 119.8(5) . . ? C17 C18 C21 117.7(5) . . ? C19 C18 C21 122.5(5) . . ? N2 C19 C14 121.0(5) . . ? N2 C19 C18 120.4(5) . . ? C14 C19 C18 118.5(5) . . ? O2 C20 F4A 115.1(8) . . ? O2 C20 F5 126.7(7) . . ? O2 C20 F5A 115.5(7) . . ? F4A C20 F5A 110.2(9) . . ? O2 C20 F4 108.7(7) . . ? F5 C20 F4 113.0(9) . . ? O2 C20 F6A 112.3(7) . . ? F4A C20 F6A 102.9(7) . . ? F5A C20 F6A 98.9(7) . . ? O2 C20 F6 104.7(7) . . ? F5 C20 F6 96.7(7) . . ? F4 C20 F6 103.1(7) . . ? C22 C21 C23 119.8(5) . . ? C22 C21 C18 119.1(5) . . ? C23 C21 C18 120.3(5) . . ? C23 C22 C21 122.5(5) 5_475 . ? C22 C23 C21 117.7(5) 5_475 . ? C22 C23 C8 120.9(5) 5_475 . ? C21 C23 C8 121.3(4) . . ? C25 C24 C29 115.8(6) . . ? C25 C24 Pt1 125.8(5) . . ? C29 C24 Pt1 118.4(4) . . ? C24 C25 C26 122.8(6) . . ? C27 C26 C25 120.5(6) . . ? C26 C27 C28 117.6(6) . . ? C29 C28 C27 121.7(6) . . ? C28 C29 C24 121.5(6) . . ? C31 C30 C35 116.0(5) . . ? C31 C30 Pt1 124.2(4) . . ? C35 C30 Pt1 119.8(4) . . ? C30 C31 C32 123.3(6) . . ? C33 C32 C31 118.6(6) . . ? C32 C33 C34 120.0(6) . . ? C33 C34 C35 120.4(6) . . ? C34 C35 C30 121.5(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.619 _refine_diff_density_min -1.327 _refine_diff_density_rms 0.156 _vrf_PLAT601_1b ; RESPONSE: residue electron density from disordered solvents were removed with SQUEEZE function of PLATON program. The total volume of solvent accessible void in the unit cell is 1097.9 Ang^3, 16.7% of the unit cell volume. In total, 431 electrons were removed per unit cell. The contributions of the solvent molecules are not included in the formula. Elemental Analysis suggests the presence of dichloromethane in the crystal lattice. ; #===>END data_2b _database_code_depnum_ccdc_archive 'CCDC 743628' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H46 Cl6 F12 N4 O4 Pt2' _chemical_formula_weight 1862.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0461(2) _cell_length_b 21.5220(4) _cell_length_c 15.2720(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.6500(10) _cell_angle_gamma 90.00 _cell_volume 3279.78(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28705 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.53 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 4.595 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details 'Bruker Apex 2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28705 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.53 _reflns_number_total 7506 _reflns_number_gt 5621 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0293P)^2^+9.7756P] 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 7506 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 1.034842(19) 0.132312(8) 0.400071(12) 0.01491(6) Uani 1 1 d . . . Cl1 Cl 1.08394(14) 0.21541(6) 0.29963(9) 0.0262(3) Uani 1 1 d . . . Cl2 Cl 0.2695(13) 0.0901(5) 0.0808(7) 0.158(6) Uani 0.50 1 d P A 1 Cl2A Cl 0.3434(9) 0.1153(4) 0.0906(4) 0.099(3) Uani 0.50 1 d P B 2 Cl3 Cl 0.4500(10) 0.1802(5) 0.1636(7) 0.133(4) Uani 0.50 1 d P A 1 Cl3A Cl 0.4888(8) 0.2020(4) 0.2117(5) 0.081(2) Uani 0.50 1 d P B 2 F1 F 1.5304(6) 0.13029(19) 0.8854(3) 0.0855(19) Uani 1 1 d . . . F2 F 1.5074(5) 0.03833(18) 0.9253(2) 0.0620(12) Uani 1 1 d . . . F3 F 1.3366(6) 0.0961(3) 0.8934(3) 0.0931(18) Uani 1 1 d . . . F4 F 0.9992(11) 0.1144(5) 0.8322(7) 0.050(3) Uiso 0.50 1 d P . . F4A F 1.0100(12) 0.1290(6) 0.8207(8) 0.056(4) Uiso 0.50 1 d P . . F5 F 0.8626(9) 0.1035(5) 0.9163(6) 0.052(2) Uiso 0.50 1 d P . . F5A F 0.8465(12) 0.1290(6) 0.9096(8) 0.083(4) Uiso 0.50 1 d P C . F6 F 0.8686(9) 0.1918(5) 0.8592(6) 0.051(2) Uiso 0.50 1 d P . . F6A F 0.8978(13) 0.2047(6) 0.8332(9) 0.090(4) Uiso 0.50 1 d P C . O1 O 1.4462(4) 0.06071(17) 0.7894(2) 0.0342(10) Uani 1 1 d . . . O2A O 0.7807(11) 0.1320(5) 0.7687(7) 0.049(3) Uiso 0.50 1 d P C 2 O2 O 0.7975(8) 0.1091(4) 0.7788(5) 0.0226(19) Uiso 0.50 1 d P C 1 N1 N 1.1325(4) 0.17924(18) 0.5152(3) 0.0177(9) Uani 1 1 d . . . N2A N 0.8531(13) 0.1781(6) 0.4208(8) 0.017(3) Uiso 0.50 1 d P C 2 N2 N 0.8539(12) 0.1770(6) 0.4404(8) 0.016(3) Uiso 0.50 1 d P C 1 C1 C 1.1390(5) 0.2409(2) 0.5083(3) 0.0224(11) Uani 1 1 d . . . H1 H 1.0818 0.2607 0.4629 0.027 Uiso 1 1 calc R C . C1S C 0.3204(19) 0.1245(8) 0.1754(12) 0.068(5) Uiso 0.50 1 d P A 1 H1SA H 0.3545 0.0928 0.2193 0.081 Uiso 0.50 1 calc PR A 1 H1SB H 0.2435 0.1457 0.1976 0.081 Uiso 0.50 1 calc PR A 1 C1SA C 0.3706(15) 0.1439(7) 0.2000(9) 0.041(3) Uiso 0.50 1 d P B 2 H1SC H 0.2850 0.1601 0.2172 0.050 Uiso 0.50 1 calc PR B 2 H1SD H 0.4002 0.1094 0.2404 0.050 Uiso 0.50 1 calc PR B 2 C2 C 1.2258(6) 0.2779(2) 0.5645(4) 0.0264(12) Uani 1 1 d . C . H2 H 1.2268 0.3218 0.5578 0.032 Uiso 1 1 calc R . . C3 C 1.3073(6) 0.2498(2) 0.6279(3) 0.0247(12) Uani 1 1 d . . . H3 H 1.3707 0.2739 0.6644 0.030 Uiso 1 1 calc R C . C4 C 1.3004(5) 0.1842(2) 0.6414(3) 0.0207(11) Uani 1 1 d . C . C5 C 1.3829(6) 0.1554(3) 0.7101(3) 0.0252(12) Uani 1 1 d . . . H5 H 1.4486 0.1784 0.7463 0.030 Uiso 1 1 calc R C . C6 C 1.3664(5) 0.0942(2) 0.7233(3) 0.0240(12) Uani 1 1 d . C . C7 C 1.2730(5) 0.0591(2) 0.6712(3) 0.0211(11) Uani 1 1 d . . . H7 H 1.2626 0.0165 0.6854 0.025 Uiso 1 1 calc R C . C8 C 1.1943(5) 0.0834(2) 0.5994(3) 0.0165(10) Uani 1 1 d . C . C9 C 1.2073(5) 0.1489(2) 0.5839(3) 0.0196(11) Uani 1 1 d . . . C10 C 1.4576(8) 0.0823(3) 0.8714(4) 0.0453(18) Uani 1 1 d . . . C11A C 0.7885(14) 0.2225(6) 0.3784(8) 0.0234(12) Uiso 0.50 1 d P C 2 H11A H 0.8053 0.2297 0.3193 0.028 Uiso 0.50 1 calc PR C 2 C11 C 0.7924(14) 0.2279(6) 0.4014(7) 0.0200(11) Uiso 0.50 1 d P C 1 H11 H 0.8120 0.2410 0.3449 0.024 Uiso 0.50 1 calc PR C 1 C12A C 0.6965(12) 0.2603(6) 0.4127(8) 0.0234(12) Uiso 0.50 1 d P C 2 H12A H 0.6528 0.2926 0.3781 0.028 Uiso 0.50 1 calc PR C 2 C12 C 0.6976(11) 0.2615(5) 0.4465(8) 0.0200(11) Uiso 0.50 1 d P C 1 H12 H 0.6496 0.2953 0.4181 0.024 Uiso 0.50 1 calc PR C 1 C13A C 0.6689(13) 0.2504(6) 0.4980(8) 0.0234(12) Uiso 0.50 1 d P C 2 H13A H 0.6069 0.2759 0.5240 0.028 Uiso 0.50 1 calc PR C 2 C13 C 0.6760(12) 0.2453(5) 0.5293(7) 0.0200(11) Uiso 0.50 1 d P C 1 H13 H 0.6154 0.2685 0.5598 0.024 Uiso 0.50 1 calc PR C 1 C14A C 0.7371(9) 0.2002(4) 0.5463(5) 0.0234(12) Uiso 0.50 1 d PG C 2 C15A C 0.7240(8) 0.1899(4) 0.6347(5) 0.0234(12) Uiso 0.50 1 d PG C 2 H15A H 0.6659 0.2153 0.6641 0.028 Uiso 0.50 1 calc PR C 2 C16A C 0.7960(9) 0.1425(4) 0.6802(4) 0.0234(12) Uiso 0.50 1 d PG C 2 C17A C 0.8811(10) 0.1053(4) 0.6372(5) 0.0234(12) Uiso 0.50 1 d PG C 2 H17A H 0.9303 0.0729 0.6682 0.028 Uiso 0.50 1 calc PR C 2 C18A C 0.8941(11) 0.1156(5) 0.5487(6) 0.0234(12) Uiso 0.50 1 d PG C 2 C19A C 0.8221(11) 0.1630(5) 0.5033(4) 0.0234(12) Uiso 0.50 1 d PG C 2 C14 C 0.7449(8) 0.1932(4) 0.5703(5) 0.0200(11) Uiso 0.50 1 d PG C 1 C15 C 0.7404(8) 0.1776(4) 0.6583(5) 0.0200(11) Uiso 0.50 1 d PG C 1 H15B H 0.6840 0.2002 0.6927 0.024 Uiso 0.50 1 calc PR C 1 C16 C 0.8182(8) 0.1290(4) 0.6958(4) 0.0200(11) Uiso 0.50 1 d PG C 1 C17 C 0.9006(9) 0.0959(4) 0.6453(5) 0.0200(11) Uiso 0.50 1 d PG C 1 H17B H 0.9538 0.0627 0.6710 0.024 Uiso 0.50 1 calc PR C 1 C18 C 0.9052(10) 0.1115(5) 0.5574(5) 0.0200(11) Uiso 0.50 1 d PG C 1 C19 C 0.8274(10) 0.1602(5) 0.5199(4) 0.0200(11) Uiso 0.50 1 d PG C 1 C20A C 0.8942(12) 0.1438(6) 0.8421(8) 0.0234(12) Uiso 0.50 1 d P C 2 C20 C 0.8682(11) 0.1243(5) 0.8316(8) 0.0200(11) Uiso 0.50 1 d P C 1 C21 C 1.2210(5) 0.0969(2) 0.3911(3) 0.0172(10) Uani 1 1 d . C . C22 C 1.3325(5) 0.1356(3) 0.4032(4) 0.0281(12) Uani 1 1 d . . . H22 H 1.3203 0.1791 0.4091 0.034 Uiso 1 1 calc R C . C23 C 1.4626(6) 0.1116(3) 0.4070(5) 0.0447(17) Uani 1 1 d . C . H23 H 1.5375 0.1387 0.4165 0.054 Uiso 1 1 calc R . . C24 C 1.4820(6) 0.0498(3) 0.3972(5) 0.0484(18) Uani 1 1 d . . . H24 H 1.5704 0.0335 0.4010 0.058 Uiso 1 1 calc R C . C25 C 1.3739(6) 0.0105(3) 0.3817(4) 0.0377(15) Uani 1 1 d . C . H25 H 1.3872 -0.0326 0.3720 0.045 Uiso 1 1 calc R . . C26 C 1.2460(5) 0.0340(2) 0.3804(3) 0.0237(12) Uani 1 1 d . . . H26 H 1.1722 0.0062 0.3718 0.028 Uiso 1 1 calc R C . C27 C 0.9447(5) 0.0909(2) 0.2870(3) 0.0231(12) Uani 1 1 d . C . C28A C 0.800(2) 0.0972(11) 0.2689(15) 0.0281(18) Uiso 0.50 1 d P C 2 H28A H 0.7522 0.1158 0.3120 0.034 Uiso 0.50 1 calc PR C 2 C28 C 0.815(2) 0.0933(11) 0.2613(15) 0.0284(18) Uiso 0.50 1 d P C 1 H28 H 0.7573 0.1110 0.2999 0.034 Uiso 0.50 1 calc PR C 1 C29A C 0.7316(14) 0.0771(7) 0.1916(9) 0.0281(18) Uiso 0.50 1 d P C 2 H29A H 0.6374 0.0829 0.1807 0.034 Uiso 0.50 1 calc PR C 2 C29 C 0.7563(15) 0.0698(7) 0.1763(10) 0.0284(18) Uiso 0.50 1 d P C 1 H29 H 0.6621 0.0709 0.1605 0.034 Uiso 0.50 1 calc PR C 1 C30A C 0.7984(13) 0.0488(6) 0.1306(9) 0.0281(18) Uiso 0.50 1 d P C 2 H30A H 0.7519 0.0372 0.0753 0.034 Uiso 0.50 1 calc PR C 2 C30 C 0.8404(14) 0.0457(6) 0.1182(9) 0.0284(18) Uiso 0.50 1 d P C 1 H30 H 0.8035 0.0270 0.0645 0.034 Uiso 0.50 1 calc PR C 1 C31A C 0.9387(14) 0.0364(6) 0.1491(9) 0.0281(18) Uiso 0.50 1 d P C 2 H31A H 0.9849 0.0132 0.1092 0.034 Uiso 0.50 1 calc PR C 2 C31 C 0.9737(13) 0.0491(6) 0.1386(9) 0.0284(18) Uiso 0.50 1 d P C 1 H31 H 1.0304 0.0369 0.0960 0.034 Uiso 0.50 1 calc PR C 1 C32A C 1.0056(14) 0.0595(7) 0.2274(10) 0.0281(18) Uiso 0.50 1 d P C 2 H32A H 1.0994 0.0526 0.2390 0.034 Uiso 0.50 1 calc PR C 2 C32 C 1.0312(15) 0.0702(7) 0.2211(10) 0.0284(18) Uiso 0.50 1 d P C 1 H32 H 1.1259 0.0712 0.2345 0.034 Uiso 0.50 1 calc PR C 1 C33 C 0.9771(5) 0.0683(2) 0.4958(3) 0.0146(10) Uani 1 1 d . . . C34 C 1.0972(5) 0.0413(2) 0.5473(3) 0.0154(10) Uani 1 1 d . . . C35 C 1.1164(5) -0.0209(2) 0.5471(3) 0.0160(10) Uani 1 1 d . . . H35 H 1.1979 -0.0358 0.5776 0.019 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 0.01720(10) 0.01097(9) 0.01668(10) 0.00212(9) 0.00246(7) -0.00005(9) Cl1 0.0336(7) 0.0193(6) 0.0258(7) 0.0107(5) 0.0038(6) -0.0015(6) Cl2 0.295(15) 0.108(7) 0.093(6) 0.002(5) 0.120(9) 0.020(8) Cl2A 0.138(6) 0.126(7) 0.033(2) 0.009(4) 0.013(3) 0.077(6) Cl3 0.119(8) 0.121(8) 0.174(10) 0.095(8) 0.083(7) 0.048(6) Cl3A 0.055(3) 0.095(5) 0.097(5) 0.034(4) 0.029(3) 0.022(3) F1 0.150(5) 0.039(2) 0.052(3) 0.002(2) -0.057(3) -0.035(3) F2 0.096(3) 0.042(2) 0.040(2) 0.0142(19) -0.026(2) 0.003(2) F3 0.111(4) 0.130(5) 0.043(3) 0.016(3) 0.028(3) 0.049(4) O1 0.047(3) 0.024(2) 0.027(2) -0.0009(17) -0.0137(19) 0.0000(19) N1 0.022(2) 0.014(2) 0.017(2) -0.0016(17) 0.0056(17) -0.0027(17) C1 0.029(3) 0.012(2) 0.026(3) 0.001(2) 0.003(2) 0.001(2) C2 0.043(3) 0.008(2) 0.030(3) 0.000(2) 0.008(3) -0.005(2) C3 0.034(3) 0.017(3) 0.023(3) -0.006(2) 0.002(2) -0.005(2) C4 0.027(3) 0.015(3) 0.021(3) -0.008(2) 0.005(2) -0.004(2) C5 0.031(3) 0.024(3) 0.018(3) -0.004(2) -0.005(2) -0.004(2) C6 0.030(3) 0.019(3) 0.021(3) 0.001(2) -0.003(2) -0.002(2) C7 0.030(3) 0.011(2) 0.022(3) -0.001(2) 0.001(2) -0.003(2) C8 0.020(3) 0.014(2) 0.016(2) 0.0009(19) 0.004(2) 0.000(2) C9 0.024(3) 0.015(3) 0.021(3) -0.002(2) 0.008(2) -0.003(2) C10 0.068(5) 0.036(4) 0.028(4) 0.002(3) -0.011(3) 0.005(4) C21 0.021(3) 0.017(3) 0.015(2) 0.003(2) 0.005(2) -0.002(2) C22 0.026(3) 0.025(3) 0.034(3) -0.004(3) 0.007(2) -0.005(3) C23 0.023(3) 0.047(4) 0.066(5) -0.016(4) 0.009(3) -0.009(3) C24 0.021(3) 0.054(5) 0.072(5) -0.004(4) 0.009(3) 0.013(3) C25 0.036(4) 0.025(3) 0.054(4) 0.003(3) 0.013(3) 0.008(3) C26 0.027(3) 0.025(3) 0.021(3) 0.001(2) 0.010(2) -0.002(2) C27 0.032(3) 0.013(2) 0.023(3) 0.007(2) -0.003(2) -0.005(2) C33 0.020(3) 0.009(2) 0.016(2) 0.0017(19) 0.007(2) -0.0014(19) C34 0.020(3) 0.016(2) 0.011(2) 0.0002(19) 0.0060(19) -0.004(2) C35 0.017(3) 0.022(3) 0.009(2) 0.001(2) 0.0047(19) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C21 2.038(5) . ? Pt1 C27 2.057(5) . ? Pt1 N2A 2.131(13) . ? Pt1 C33 2.138(4) . ? Pt1 N1 2.161(4) . ? Pt1 N2 2.206(13) . ? Pt1 Cl1 2.4434(12) . ? Cl2 C1S 1.65(2) . ? Cl2A C1SA 1.772(16) . ? Cl3 C1S 1.79(2) . ? Cl3A C1SA 1.718(17) . ? F1 C10 1.269(8) . ? F2 C10 1.315(7) . ? F3 C10 1.331(9) . ? F4 C20A 1.255(17) . ? F4 C20 1.332(16) . ? F4A C20A 1.286(17) . ? F4A C20 1.457(17) . ? F5 F5A 0.577(15) . ? F5 C20 1.375(15) . ? F5 C20A 1.490(16) . ? F5A C20A 1.227(16) . ? F5A C20 1.239(16) . ? F5A F6 1.584(15) . ? F6 F6A 0.588(15) . ? F6 C20A 1.103(13) . ? F6 C20 1.513(14) . ? F6A C20A 1.318(17) . ? F6A C20 1.755(17) . ? O1 C10 1.328(7) . ? O1 C6 1.412(6) . ? O2A C16A 1.397(12) . ? O2A C20A 1.524(16) . ? O2 C20 1.063(13) . ? O2 C16 1.378(10) . ? N1 C1 1.333(6) . ? N1 C9 1.382(6) . ? N2A C11A 1.286(19) . ? N2A C19A 1.371(14) . ? N2 C19 1.323(14) . ? N2 C11 1.361(19) . ? C1 C2 1.400(7) . ? C2 C3 1.337(7) . ? C3 C4 1.430(7) . ? C4 C5 1.405(7) . ? C4 C9 1.426(7) . ? C5 C6 1.346(7) . ? C6 C7 1.383(7) . ? C7 C8 1.379(7) . ? C8 C9 1.438(7) . ? C8 C34 1.492(7) . ? C11A C12A 1.380(18) . ? C11 C12 1.434(17) . ? C12A C13A 1.380(15) . ? C12 C13 1.353(15) . ? C13A C14A 1.436(13) . ? C13 C14 1.425(12) . ? C14A C15A 1.3900 . ? C14A C19A 1.3900 . ? C15A C16A 1.3900 . ? C16A C17A 1.3900 . ? C17A C18A 1.3900 . ? C18A C19A 1.3900 . ? C18A C33 1.594(7) . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C18 C33 1.559(7) . ? C21 C26 1.390(7) . ? C21 C22 1.390(7) . ? C22 C23 1.400(8) . ? C23 C24 1.356(9) . ? C24 C25 1.375(9) . ? C25 C26 1.379(8) . ? C27 C28 1.32(2) . ? C27 C32A 1.337(16) . ? C27 C28A 1.45(2) . ? C27 C32 1.473(16) . ? C28A C29A 1.37(3) . ? C28 C29 1.45(3) . ? C29A C30A 1.354(17) . ? C29 C30 1.395(16) . ? C30A C31A 1.430(17) . ? C30 C31 1.341(18) . ? C31A C32A 1.39(2) . ? C31 C32 1.40(2) . ? C33 C34 1.480(7) . ? C33 C35 1.486(7) 3_756 ? C34 C35 1.352(7) . ? C35 C33 1.486(7) 3_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Pt1 C27 95.7(2) . . ? C21 Pt1 N2A 172.5(4) . . ? C27 Pt1 N2A 91.3(4) . . ? C21 Pt1 C33 97.40(18) . . ? C27 Pt1 C33 99.60(19) . . ? N2A Pt1 C33 83.8(4) . . ? C21 Pt1 N1 84.02(17) . . ? C27 Pt1 N1 177.37(17) . . ? N2A Pt1 N1 88.8(4) . . ? C33 Pt1 N1 83.03(16) . . ? C21 Pt1 N2 166.8(4) . . ? C27 Pt1 N2 97.3(4) . . ? N2A Pt1 N2 7.7(5) . . ? C33 Pt1 N2 78.0(4) . . ? N1 Pt1 N2 83.1(3) . . ? C21 Pt1 Cl1 88.72(14) . . ? C27 Pt1 Cl1 83.77(14) . . ? N2A Pt1 Cl1 89.6(3) . . ? C33 Pt1 Cl1 172.64(13) . . ? N1 Pt1 Cl1 93.61(11) . . ? N2 Pt1 Cl1 95.1(3) . . ? C10 O1 C6 118.4(5) . . ? C16A O2A C20A 121.9(10) . . ? C20 O2 C16 116.3(10) . . ? C1 N1 C9 120.1(4) . . ? C1 N1 Pt1 115.0(3) . . ? C9 N1 Pt1 123.5(3) . . ? C11A N2A C19A 118.9(12) . . ? C11A N2A Pt1 131.3(10) . . ? C19A N2A Pt1 108.4(8) . . ? C19 N2 C11 119.5(11) . . ? C19 N2 Pt1 113.4(8) . . ? C11 N2 Pt1 125.1(9) . . ? N1 C1 C2 123.5(5) . . ? Cl2 C1S Cl3 111.5(11) . . ? Cl3A C1SA Cl2A 112.3(9) . . ? C3 C2 C1 118.1(5) . . ? C2 C3 C4 121.0(5) . . ? C5 C4 C9 120.8(5) . . ? C5 C4 C3 120.7(5) . . ? C9 C4 C3 118.5(5) . . ? C6 C5 C4 118.1(5) . . ? C5 C6 C7 122.4(5) . . ? C5 C6 O1 122.4(5) . . ? C7 C6 O1 115.1(4) . . ? C8 C7 C6 122.6(5) . . ? C7 C8 C9 116.6(4) . . ? C7 C8 C34 118.2(4) . . ? C9 C8 C34 125.1(4) . . ? N1 C9 C4 118.4(4) . . ? N1 C9 C8 122.4(4) . . ? C4 C9 C8 119.1(5) . . ? F1 C10 F2 108.1(6) . . ? F1 C10 O1 115.4(6) . . ? F2 C10 O1 108.8(5) . . ? F1 C10 F3 107.6(6) . . ? F2 C10 F3 107.1(6) . . ? O1 C10 F3 109.5(6) . . ? N2A C11A C12A 124.6(12) . . ? N2 C11 C12 119.2(11) . . ? C11A C12A C13A 119.0(11) . . ? C13 C12 C11 120.5(11) . . ? C12A C13A C14A 117.6(11) . . ? C12 C13 C14 119.4(10) . . ? C15A C14A C19A 120.0 . . ? C15A C14A C13A 121.7(7) . . ? C19A C14A C13A 118.3(7) . . ? C14A C15A C16A 120.0 . . ? C15A C16A C17A 120.0 . . ? C15A C16A O2A 119.6(7) . . ? C17A C16A O2A 120.4(7) . . ? C18A C17A C16A 120.0 . . ? C17A C18A C19A 120.0 . . ? C17A C18A C33 120.3(6) . . ? C19A C18A C33 119.3(5) . . ? N2A C19A C18A 118.2(8) . . ? N2A C19A C14A 121.0(8) . . ? C18A C19A C14A 120.0 . . ? C15 C14 C19 120.0 . . ? C15 C14 C13 123.1(6) . . ? C19 C14 C13 116.7(6) . . ? C14 C15 C16 120.0 . . ? O2 C16 C17 120.9(6) . . ? O2 C16 C15 118.4(6) . . ? C17 C16 C15 120.0 . . ? C16 C17 C18 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 C33 118.6(5) . . ? C17 C18 C33 120.5(5) . . ? N2 C19 C18 114.9(8) . . ? N2 C19 C14 124.4(8) . . ? C18 C19 C14 120.0 . . ? F5A C20A F4A 127.0(13) . . ? F5A C20A F6A 111.3(13) . . ? F4A C20A F6A 100.6(11) . . ? F4A C20A F5 109.2(11) . . ? F6A C20A F5 131.9(12) . . ? F5A C20A O2A 104.0(11) . . ? F4A C20A O2A 113.2(11) . . ? F6A C20A O2A 96.8(10) . . ? O2 C20 F4 121.9(12) . . ? O2 C20 F5 121.1(11) . . ? F4 C20 F5 95.2(10) . . ? F5 C20 F4A 106.1(10) . . ? O2 C20 F6 119.2(11) . . ? F5A C20 F6 69.5(9) . . ? F4 C20 F6 100.4(9) . . ? F5 C20 F6 92.9(9) . . ? C26 C21 C22 116.3(5) . . ? C26 C21 Pt1 123.5(4) . . ? C22 C21 Pt1 120.0(4) . . ? C21 C22 C23 121.3(5) . . ? C24 C23 C22 120.2(6) . . ? C23 C24 C25 120.1(6) . . ? C24 C25 C26 119.5(6) . . ? C25 C26 C21 122.5(5) . . ? C32A C27 C28A 116.3(11) . . ? C28 C27 C32 116.7(11) . . ? C28 C27 Pt1 123.8(9) . . ? C32A C27 Pt1 126.7(7) . . ? C28A C27 Pt1 116.9(9) . . ? C32 C27 Pt1 117.9(7) . . ? C29A C28A C27 121.9(13) . . ? C27 C28 C29 122.4(13) . . ? C30A C29A C28A 119.7(13) . . ? C30 C29 C28 119.2(13) . . ? C29A C30A C31A 120.2(13) . . ? C31 C30 C29 119.6(13) . . ? C32A C31A C30A 118.0(12) . . ? C30 C31 C32 121.6(12) . . ? C27 C32A C31A 123.4(12) . . ? C31 C32 C27 119.9(11) . . ? C34 C33 C35 113.6(4) . 3_756 ? C34 C33 C18 108.7(5) . . ? C35 C33 C18 111.3(6) 3_756 . ? C34 C33 C18A 115.1(5) . . ? C35 C33 C18A 108.7(6) 3_756 . ? C34 C33 Pt1 110.3(3) . . ? C35 C33 Pt1 110.3(3) 3_756 . ? C18 C33 Pt1 102.1(4) . . ? C18A C33 Pt1 97.7(4) . . ? C35 C34 C33 119.7(4) . . ? C35 C34 C8 121.2(4) . . ? C33 C34 C8 119.1(4) . . ? C34 C35 C33 126.6(4) . 3_756 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.357 _refine_diff_density_min -1.526 _refine_diff_density_rms 0.152 # Attachment 'cif.txt' data_1a _database_code_depnum_ccdc_archive 'CCDC 747774' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H70 N4 O Pt2' _chemical_formula_weight 1469.56 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.8443(8) _cell_length_b 20.5580(13) _cell_length_c 21.3045(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.934(3) _cell_angle_gamma 90.00 _cell_volume 6005.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7264 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920 _exptl_absorpt_coefficient_mu 4.706 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7987 _exptl_absorpt_correction_T_max 0.8717 _exptl_absorpt_process_details 'bruker apex 2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49767 _diffrn_reflns_av_R_equivalents 0.1229 _diffrn_reflns_av_sigmaI/netI 0.1518 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.00 _reflns_number_total 12981 _reflns_number_gt 7264 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0539P)^2^+6.9655P] 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 12981 _refine_ls_number_parameters 680 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1367 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 0.72157(3) 1.392046(18) 0.086080(19) 0.02452(12) Uani 1 1 d . . . N1 N 0.8009(6) 1.3330(4) 0.0257(4) 0.0238(19) Uani 1 1 d . A . C1 C 0.7495(7) 1.3267(5) -0.0317(5) 0.031(3) Uani 1 1 d . . . H1A H 0.6854 1.3443 -0.0378 0.037 Uiso 1 1 calc R . . O1 O 0.9972(15) 1.0757(10) 0.0615(13) 0.200(8) Uani 1 1 d . . . C1S C 0.9649(16) 1.1020(8) 0.1240(10) 0.108(7) Uani 1 1 d . . . H1SA H 0.9906 1.0739 0.1602 0.130 Uiso 1 1 calc R . . H1SB H 0.9893 1.1468 0.1326 0.130 Uiso 1 1 calc R . . Pt2 Pt 1.03098(3) 1.340427(18) 0.344579(19) 0.02189(11) Uani 1 1 d . . . N2 N 0.8089(6) 1.4720(4) 0.0613(4) 0.027(2) Uani 1 1 d . . . C2 C 0.7816(8) 1.2969(5) -0.0829(5) 0.034(3) Uani 1 1 d . A . H2A H 0.7403 1.2937 -0.1223 0.040 Uiso 1 1 calc R . . C2S C 0.8533(17) 1.1010(11) 0.1138(11) 0.135(8) Uani 1 1 d . . . H2SA H 0.8277 1.0595 0.1283 0.162 Uiso 1 1 calc R . . H2SB H 0.8262 1.1376 0.1361 0.162 Uiso 1 1 calc R . . N3 N 0.9517(5) 1.2552(3) 0.3729(4) 0.0208(18) Uani 1 1 d . . . C3 C 0.8721(8) 1.2725(5) -0.0760(5) 0.035(3) Uani 1 1 d . . . H3A H 0.8953 1.2513 -0.1112 0.042 Uiso 1 1 d R A . C3S C 0.8306(14) 1.1084(9) 0.0424(10) 0.105(6) Uani 1 1 d . . . H3SA H 0.7682 1.0869 0.0261 0.126 Uiso 1 1 calc R . . H3SB H 0.8264 1.1550 0.0303 0.126 Uiso 1 1 calc R . . N4 N 0.9396(6) 1.3922(4) 0.3995(4) 0.029(2) Uani 1 1 d . . . C4 C 0.9340(9) 1.2777(6) -0.0179(6) 0.0469(19) Uiso 0.50 1 d P A 1 C4A C 0.9296(9) 1.2769(6) -0.0169(6) 0.0469(19) Uiso 0.50 1 d PR A 2 C4S C 0.9128(12) 1.0767(9) 0.0172(8) 0.080(5) Uani 1 1 d . . . H4SA H 0.8943 1.0315 0.0047 0.096 Uiso 1 1 calc R . . H4SB H 0.9264 1.1001 -0.0213 0.096 Uiso 1 1 calc R . . C5 C 1.0367(12) 1.2560(7) -0.0063(6) 0.031(11) Uiso 0.50 1 d P A 1 H5A H 1.0646 1.2352 -0.0394 0.038 Uiso 0.50 1 calc PR A 1 C5A C 1.0218(12) 1.2491(7) -0.0092(6) 0.034(12) Uiso 0.50 1 d PR A 2 H5AA H 1.0462 1.2320 -0.0453 0.041 Uiso 0.50 1 calc PR A 2 C6 C 1.0928(17) 1.2654(12) 0.0517(12) 0.026(6) Uiso 0.50 1 d P A 1 C6A C 1.0782(16) 1.2453(12) 0.0477(12) 0.023(6) Uiso 0.50 1 d P A 2 C7 C 1.0440(7) 1.2832(5) 0.1013(5) 0.034(3) Uani 1 1 d . . . H7A H 1.0762 1.2766 0.1436 0.041 Uiso 1 1 d R A . C8 C 0.9516(6) 1.3080(4) 0.0948(5) 0.023(2) Uani 1 1 d . A . C9 C 0.8947(8) 1.3064(5) 0.0345(5) 0.0344(9) Uani 1 1 d . . . C10 C 1.2038(18) 1.2465(13) 0.0627(13) 0.0469(19) Uiso 0.50 1 d P A 1 H10A H 1.2334 1.2691 0.1018 0.056 Uiso 0.50 1 d PR A 1 H10B H 1.2068 1.1994 0.0721 0.056 Uiso 0.50 1 d PR A 1 C10A C 1.1755(17) 1.2145(13) 0.0576(13) 0.0469(19) Uiso 0.50 1 d P A 2 H10C H 1.2115 1.2314 0.0976 0.056 Uiso 0.50 1 d PR A 2 H10D H 1.1644 1.1676 0.0642 0.056 Uiso 0.50 1 d PR A 2 C11 C 1.2521(18) 1.2547(12) 0.0268(13) 0.0469(19) Uiso 0.50 1 d P A 1 H11A H 1.3103 1.2274 0.0362 0.070 Uiso 0.50 1 calc PR A 1 H11B H 1.2714 1.3005 0.0272 0.070 Uiso 0.50 1 calc PR A 1 H11C H 1.2177 1.2434 -0.0151 0.070 Uiso 0.50 1 calc PR A 1 C11A C 1.2379(17) 1.2177(12) 0.0084(12) 0.0469(19) Uiso 0.50 1 d P A 2 H11D H 1.3040 1.2037 0.0257 0.070 Uiso 0.50 1 calc PR A 2 H11E H 1.2400 1.2625 -0.0071 0.070 Uiso 0.50 1 calc PR A 2 H11F H 1.2122 1.1890 -0.0267 0.070 Uiso 0.50 1 calc PR A 2 C12 C 0.7658(8) 1.5093(5) 0.0150(5) 0.027(2) Uani 1 1 d . . . H12A H 0.6999 1.5002 -0.0014 0.032 Uiso 1 1 calc R . . C13 C 0.8108(8) 1.5606(5) -0.0107(5) 0.034(3) Uani 1 1 d . . . H13A H 0.7757 1.5860 -0.0435 0.041 Uiso 1 1 calc R . . C14 C 0.9054(9) 1.5748(5) 0.0107(6) 0.040(3) Uani 1 1 d . . . H14A H 0.9380 1.6088 -0.0081 0.047 Uiso 1 1 calc R . . C15 C 0.9554(7) 1.5375(4) 0.0622(5) 0.027(2) Uani 1 1 d . . . C16 C 1.0531(8) 1.5495(5) 0.0871(5) 0.034(3) Uani 1 1 d . . . H16A H 1.0869 1.5838 0.0696 0.040 Uiso 1 1 calc R . . C17 C 1.1002(7) 1.5142(5) 0.1346(5) 0.032(3) Uani 1 1 d . . . C18 C 1.0487(7) 1.4619(5) 0.1605(5) 0.031(3) Uani 1 1 d . . . H18A H 1.0812 1.4367 0.1943 0.037 Uiso 1 1 calc R . . C19 C 0.9535(6) 1.4478(4) 0.1370(5) 0.022(2) Uani 1 1 d . . . C20 C 0.9037(7) 1.4852(4) 0.0861(5) 0.024(2) Uani 1 1 d . . . C21 C 1.2041(7) 1.5292(5) 0.1628(5) 0.0344(9) Uani 1 1 d . . . H21A H 1.2379 1.5477 0.1288 0.041 Uiso 1 1 calc R . . H21B H 1.2024 1.5634 0.1953 0.041 Uiso 1 1 calc R . . C22 C 1.2634(7) 1.4743(5) 0.1921(5) 0.0344(9) Uani 1 1 d . . . H22A H 1.3300 1.4894 0.2063 0.052 Uiso 1 1 calc R . . H22B H 1.2649 1.4394 0.1610 0.052 Uiso 1 1 calc R . . H22C H 1.2346 1.4579 0.2285 0.052 Uiso 1 1 calc R . . C23 C 0.9976(7) 1.2350(5) 0.4296(5) 0.030(3) Uani 1 1 d . . . H23A H 1.0552 1.2574 0.4471 0.036 Uiso 1 1 calc R . . C24 C 0.9662(7) 1.1841(5) 0.4636(5) 0.0344(9) Uani 1 1 d . . . H24A H 1.0029 1.1708 0.5025 0.041 Uiso 1 1 calc R . . C25 C 0.8815(8) 1.1530(5) 0.4405(6) 0.041(3) Uani 1 1 d . . . H25A H 0.8581 1.1183 0.4637 0.049 Uiso 1 1 calc R . . C26 C 0.8287(7) 1.1727(5) 0.3821(5) 0.028(2) Uani 1 1 d . . . C27 C 0.7419(7) 1.1410(5) 0.3574(5) 0.032(3) Uani 1 1 d . . . H27A H 0.7172 1.1069 0.3807 0.038 Uiso 1 1 calc R . . C28 C 0.6930(7) 1.1589(5) 0.3004(5) 0.034(3) Uani 1 1 d . . . C29 C 0.7311(7) 1.2098(5) 0.2655(5) 0.032(3) Uani 1 1 d . . . H29A H 0.6978 1.2206 0.2248 0.038 Uiso 1 1 calc R . . C30 C 0.8140(7) 1.2437(5) 0.2882(5) 0.0344(9) Uani 1 1 d . A . C31 C 0.8664(7) 1.2244(5) 0.3477(5) 0.026(2) Uani 1 1 d . . . C32 C 0.5968(7) 1.1277(5) 0.2751(5) 0.037(3) Uani 1 1 d . . . H32A H 0.5950 1.0845 0.2921 0.044 Uiso 1 1 d R . . H32B H 0.5896 1.1245 0.2297 0.044 Uiso 1 1 d R . . C33 C 0.5125(7) 1.1663(5) 0.2943(5) 0.0344(9) Uani 1 1 d . . . H33A H 0.5028 1.2058 0.2684 0.052 Uiso 1 1 calc R . . H33B H 0.5270 1.1784 0.3391 0.052 Uiso 1 1 calc R . . H33C H 0.4531 1.1398 0.2878 0.052 Uiso 1 1 calc R . . C34 C 0.9808(8) 1.4101(5) 0.4567(5) 0.035(3) Uani 1 1 d . . . H34A H 1.0496 1.4064 0.4666 0.042 Uiso 1 1 calc R . . C35 C 0.9280(8) 1.4344(5) 0.5035(5) 0.0344(9) Uani 1 1 d . B . H35A H 0.9610 1.4475 0.5436 0.041 Uiso 1 1 calc R . . C36 C 0.8314(9) 1.4388(6) 0.4911(6) 0.046(3) Uani 1 1 d . . . H36A H 0.7934 1.4534 0.5227 0.055 Uiso 1 1 d R B . C37 C 0.7877(18) 1.4246(13) 0.4336(13) 0.044(2) Uiso 0.50 1 d P B 1 C37A C 0.7832(9) 1.4129(7) 0.4304(4) 0.044(2) Uiso 0.50 1 d PG B 2 C38 C 0.6835(17) 1.4354(11) 0.4149(12) 0.044(2) Uiso 0.50 1 d P B 1 H38A H 0.6462 1.4543 0.4445 0.053 Uiso 0.50 1 calc PR B 1 C38A C 0.6820(9) 1.4104(8) 0.4175(6) 0.044(2) Uiso 0.50 1 d PG B 2 H38B H 0.6435 1.4207 0.4497 0.053 Uiso 0.50 1 calc PR B 2 C39 C 0.6402(17) 1.4197(11) 0.3583(12) 0.044(2) Uiso 0.50 1 d P B 1 C39A C 0.6374(5) 1.3931(8) 0.3574(8) 0.044(2) Uiso 0.50 1 d PG B 2 C40 C 0.6959(17) 1.3900(12) 0.3107(13) 0.044(2) Uiso 0.50 1 d P B 1 H40A H 0.6622 1.3773 0.2707 0.053 Uiso 0.50 1 calc PR B 1 C40A C 0.6938(6) 1.3781(7) 0.3102(5) 0.044(2) Uiso 0.50 1 d PG B 2 H40B H 0.6633 1.3662 0.2691 0.053 Uiso 0.50 1 calc PR B 2 C41 C 0.7950(6) 1.3805(4) 0.3232(3) 0.025(2) Uani 1 1 d G . . C42 C 0.8396(5) 1.3979(4) 0.3833(4) 0.031(3) Uani 1 1 d G B . C43 C 0.5343(17) 1.4252(12) 0.3373(12) 0.0469(19) Uiso 0.50 1 d P B 1 H43A H 0.5242 1.4571 0.3022 0.056 Uiso 0.50 1 d PR B 1 H43B H 0.5036 1.4432 0.3728 0.056 Uiso 0.50 1 d PR B 1 C43A C 0.5178(17) 1.3776(13) 0.3523(13) 0.0469(19) Uiso 0.50 1 d P B 2 H43C H 0.5056 1.3301 0.3524 0.056 Uiso 0.50 1 d PR B 2 H43D H 0.4902 1.3974 0.3883 0.056 Uiso 0.50 1 d PR B 2 C44 C 0.4824(18) 1.3623(12) 0.3146(13) 0.0469(19) Uiso 0.50 1 d P B 1 H44A H 0.4137 1.3649 0.3209 0.070 Uiso 0.50 1 calc PR B 1 H44B H 0.5135 1.3255 0.3388 0.070 Uiso 0.50 1 calc PR B 1 H44C H 0.4868 1.3560 0.2694 0.070 Uiso 0.50 1 calc PR B 1 C44A C 0.4728(17) 1.4056(12) 0.2938(12) 0.0469(19) Uiso 0.50 1 d P B 2 H44D H 0.4018 1.4018 0.2910 0.070 Uiso 0.50 1 calc PR B 2 H44E H 0.4950 1.3826 0.2582 0.070 Uiso 0.50 1 calc PR B 2 H44F H 0.4909 1.4516 0.2923 0.070 Uiso 0.50 1 calc PR B 2 C45 C 0.6349(7) 1.4561(5) 0.1218(5) 0.030(3) Uani 1 1 d . . . C46 C 0.6562(8) 1.4890(5) 0.1777(5) 0.037(3) Uani 1 1 d . . . H46A H 0.7163 1.4795 0.2033 0.045 Uiso 1 1 calc R . . C47 C 0.5961(9) 1.5352(5) 0.1996(6) 0.042(3) Uani 1 1 d . . . H47A H 0.6140 1.5553 0.2397 0.051 Uiso 1 1 calc R . . C48 C 0.5097(9) 1.5516(6) 0.1624(7) 0.053(4) Uani 1 1 d . . . H48A H 0.4680 1.5838 0.1760 0.064 Uiso 1 1 calc R . . C49 C 0.4856(9) 1.5208(6) 0.1057(7) 0.054(4) Uani 1 1 d . . . H49A H 0.4259 1.5313 0.0801 0.065 Uiso 1 1 calc R . . C50 C 0.5461(8) 1.4744(6) 0.0847(6) 0.051(3) Uani 1 1 d . . . H50A H 0.5278 1.4544 0.0446 0.061 Uiso 1 1 calc R . . C51 C 0.6361(7) 1.3167(5) 0.1055(5) 0.029(3) Uani 1 1 d . . . C52 C 0.5525(8) 1.3216(6) 0.1337(6) 0.043(3) Uani 1 1 d . . . H52A H 0.5361 1.3628 0.1495 0.052 Uiso 1 1 calc R . . C53 C 0.4911(9) 1.2696(7) 0.1401(6) 0.054(4) Uani 1 1 d . . . H53A H 0.4335 1.2763 0.1589 0.064 Uiso 1 1 calc R . . C54 C 0.5125(9) 1.2075(6) 0.1194(5) 0.045(3) Uani 1 1 d . . . H54A H 0.4695 1.1720 0.1225 0.054 Uiso 1 1 calc R . . C55 C 0.5995(9) 1.1993(6) 0.0939(5) 0.041(3) Uani 1 1 d . . . H55A H 0.6181 1.1572 0.0817 0.050 Uiso 1 1 calc R . . C56 C 0.6589(7) 1.2524(5) 0.0863(5) 0.033(3) Uani 1 1 d . . . H56A H 0.7166 1.2458 0.0677 0.040 Uiso 1 1 calc R . . C57 C 1.1165(7) 1.4197(5) 0.3451(5) 0.026(2) Uani 1 1 d . . . C58 C 1.2127(7) 1.4184(5) 0.3745(5) 0.035(3) Uani 1 1 d . . . H58A H 1.2397 1.3787 0.3918 0.042 Uiso 1 1 calc R . . C59 C 1.2692(9) 1.4739(6) 0.3790(6) 0.043(3) Uani 1 1 d . . . H59A H 1.3351 1.4713 0.3985 0.052 Uiso 1 1 calc R . . C60 C 1.2330(9) 1.5328(6) 0.3561(6) 0.043(3) Uani 1 1 d . . . H60A H 1.2737 1.5702 0.3584 0.051 Uiso 1 1 calc R . . C61 C 1.1367(8) 1.5364(5) 0.3297(5) 0.036(3) Uani 1 1 d . . . H61A H 1.1098 1.5769 0.3147 0.043 Uiso 1 1 calc R . . C62 C 1.0782(8) 1.4806(5) 0.3248(5) 0.032(3) Uani 1 1 d . . . H62A H 1.0114 1.4839 0.3074 0.038 Uiso 1 1 calc R . . C63 C 1.1158(6) 1.2863(5) 0.2945(5) 0.023(2) Uani 1 1 d . . . C64 C 1.2008(8) 1.3068(5) 0.2728(5) 0.036(3) Uani 1 1 d . . . H64A H 1.2197 1.3510 0.2788 0.044 Uiso 1 1 calc R . . C65 C 1.2591(8) 1.2659(6) 0.2429(6) 0.045(3) Uani 1 1 d . . . H65A H 1.3174 1.2824 0.2300 0.053 Uiso 1 1 calc R . . C66 C 1.2344(8) 1.2020(6) 0.2315(5) 0.041(3) Uani 1 1 d . . . H66A H 1.2757 1.1737 0.2121 0.049 Uiso 1 1 calc R . . C67 C 1.1489(7) 1.1801(5) 0.2487(5) 0.034(3) Uani 1 1 d . . . H67A H 1.1290 1.1364 0.2400 0.040 Uiso 1 1 calc R . . C68 C 1.0909(7) 1.2215(5) 0.2791(5) 0.029(2) Uani 1 1 d . . . H68A H 1.0313 1.2051 0.2900 0.035 Uiso 1 1 calc R . . C69 C 0.9110(7) 1.3295(5) 0.1536(5) 0.0344(9) Uani 1 1 d . . . C70 C 0.8806(6) 1.2812(4) 0.1930(5) 0.021(2) Uani 1 1 d . A . H70A H 0.8828 1.2369 0.1806 0.025 Uiso 1 1 calc R . . C71 C 0.8477(6) 1.2963(4) 0.2494(5) 0.022(2) Uani 1 1 d . . . C72 C 0.8448(7) 1.3615(5) 0.2681(5) 0.023(2) Uani 1 1 d . A . C73 C 0.8756(6) 1.4092(4) 0.2284(4) 0.020(2) Uani 1 1 d . . . H73A H 0.8736 1.4536 0.2406 0.024 Uiso 1 1 calc R A . C74 C 0.9091(6) 1.3937(5) 0.1718(5) 0.023(2) Uani 1 1 d . A . 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 0.0249(2) 0.0274(2) 0.0203(2) 0.00138(18) -0.00029(16) 0.00103(17) N1 0.027(4) 0.025(5) 0.018(5) 0.003(4) -0.004(4) -0.004(3) C1 0.026(6) 0.033(6) 0.034(7) 0.003(5) 0.006(5) 0.000(4) O1 0.177(19) 0.168(18) 0.26(3) -0.055(17) 0.040(18) 0.004(14) C1S 0.129(18) 0.066(12) 0.110(17) -0.007(11) -0.052(14) 0.012(11) Pt2 0.0244(2) 0.0212(2) 0.0194(2) 0.00039(17) 0.00034(16) -0.00151(16) N2 0.039(5) 0.022(5) 0.022(5) -0.007(4) 0.006(4) -0.003(4) C2 0.040(6) 0.046(7) 0.015(6) -0.007(5) 0.001(5) -0.013(5) C2S 0.15(2) 0.15(2) 0.11(2) -0.049(16) 0.009(17) 0.026(16) N3 0.025(4) 0.019(4) 0.018(5) 0.001(4) 0.003(4) -0.002(3) C3 0.047(7) 0.036(6) 0.026(7) -0.002(5) 0.021(6) -0.003(5) C3S 0.108(15) 0.097(14) 0.102(17) -0.002(12) -0.015(13) 0.022(12) N4 0.035(5) 0.025(5) 0.026(5) 0.000(4) 0.007(4) 0.004(4) C4S 0.067(11) 0.111(14) 0.060(12) -0.012(10) 0.004(9) -0.003(10) C7 0.027(6) 0.053(7) 0.020(6) 0.014(5) 0.001(5) 0.005(5) C8 0.019(5) 0.025(5) 0.026(6) -0.002(4) 0.007(4) -0.004(4) C9 0.033(2) 0.039(2) 0.029(2) 0.0005(18) 0.0000(18) -0.0087(17) C12 0.042(6) 0.021(5) 0.016(6) 0.003(4) 0.000(5) 0.007(4) C13 0.045(7) 0.039(7) 0.018(6) -0.004(5) 0.001(5) 0.006(5) C14 0.058(8) 0.023(6) 0.043(8) 0.006(5) 0.026(6) 0.012(5) C15 0.042(6) 0.016(5) 0.024(6) -0.001(4) 0.008(5) 0.000(4) C16 0.046(7) 0.012(5) 0.041(7) -0.002(5) 0.002(6) -0.010(5) C17 0.031(6) 0.032(6) 0.036(7) -0.008(5) 0.010(5) -0.004(5) C18 0.028(6) 0.036(6) 0.029(7) -0.002(5) 0.003(5) -0.008(5) C19 0.024(5) 0.018(5) 0.025(6) -0.002(4) 0.006(4) -0.004(4) C20 0.037(6) 0.012(5) 0.022(6) -0.006(4) 0.006(5) 0.002(4) C21 0.033(2) 0.039(2) 0.029(2) 0.0005(18) 0.0000(18) -0.0087(17) C22 0.033(2) 0.039(2) 0.029(2) 0.0005(18) 0.0000(18) -0.0087(17) C23 0.033(6) 0.030(6) 0.024(6) 0.000(5) -0.005(5) -0.011(5) C24 0.033(2) 0.039(2) 0.029(2) 0.0005(18) 0.0000(18) -0.0087(17) C25 0.040(7) 0.039(7) 0.043(8) 0.014(6) 0.001(6) 0.000(5) C26 0.027(5) 0.034(6) 0.022(6) 0.008(5) 0.004(5) -0.008(4) C27 0.039(6) 0.036(6) 0.019(6) 0.014(5) 0.002(5) -0.010(5) C28 0.037(6) 0.028(6) 0.041(7) -0.001(5) 0.015(5) -0.017(5) C29 0.035(6) 0.036(6) 0.020(6) 0.002(5) -0.006(5) 0.001(5) C30 0.033(2) 0.039(2) 0.029(2) 0.0005(18) 0.0000(18) -0.0087(17) C31 0.030(6) 0.024(5) 0.023(6) -0.002(4) 0.002(5) -0.003(4) C32 0.041(7) 0.031(6) 0.036(7) 0.010(5) 0.000(5) -0.007(5) C33 0.033(2) 0.039(2) 0.029(2) 0.0005(18) 0.0000(18) -0.0087(17) C34 0.044(7) 0.035(6) 0.026(7) -0.009(5) 0.005(5) -0.006(5) C35 0.033(2) 0.039(2) 0.029(2) 0.0005(18) 0.0000(18) -0.0087(17) C36 0.066(9) 0.045(7) 0.030(7) -0.006(6) 0.015(6) 0.009(6) C41 0.039(6) 0.027(6) 0.014(6) 0.002(4) 0.015(5) 0.000(4) C42 0.036(6) 0.032(6) 0.026(6) 0.003(5) 0.011(5) 0.012(5) C45 0.026(6) 0.036(6) 0.028(7) 0.008(5) 0.001(5) -0.001(4) C46 0.034(6) 0.041(7) 0.036(8) 0.003(6) 0.004(5) 0.006(5) C47 0.064(8) 0.026(6) 0.039(8) 0.000(5) 0.014(6) 0.011(5) C48 0.053(8) 0.031(7) 0.079(11) -0.010(7) 0.019(8) 0.011(6) C49 0.041(7) 0.060(9) 0.060(10) -0.012(7) -0.001(7) 0.027(6) C50 0.044(7) 0.056(8) 0.051(9) -0.015(7) -0.002(7) 0.007(6) C51 0.025(6) 0.031(6) 0.029(7) 0.008(5) -0.007(5) 0.001(4) C52 0.042(7) 0.045(7) 0.047(8) 0.001(6) 0.018(6) -0.006(5) C53 0.046(8) 0.077(10) 0.039(8) 0.016(7) 0.011(6) -0.020(7) C54 0.050(8) 0.061(9) 0.024(7) 0.000(6) 0.007(6) -0.019(6) C55 0.053(8) 0.047(7) 0.023(7) 0.006(5) 0.001(6) -0.015(6) C56 0.028(6) 0.031(6) 0.039(7) 0.007(5) -0.002(5) -0.012(5) C57 0.025(5) 0.039(6) 0.016(6) -0.005(5) 0.006(4) -0.011(4) C58 0.031(6) 0.030(6) 0.039(7) 0.000(5) -0.008(5) -0.012(5) C59 0.047(7) 0.045(8) 0.038(8) -0.010(6) 0.008(6) -0.010(6) C60 0.055(8) 0.039(7) 0.037(8) -0.003(6) 0.013(6) -0.019(6) C61 0.056(8) 0.020(6) 0.033(7) 0.004(5) 0.006(6) -0.010(5) C62 0.043(7) 0.022(6) 0.028(7) 0.002(5) -0.005(5) -0.014(5) C63 0.014(5) 0.028(5) 0.026(6) -0.002(5) -0.009(4) 0.004(4) C64 0.033(6) 0.039(7) 0.037(7) -0.011(5) 0.002(5) -0.005(5) C65 0.025(6) 0.068(9) 0.040(8) -0.006(7) 0.002(5) -0.010(6) C66 0.037(7) 0.044(7) 0.039(8) -0.015(6) -0.007(6) 0.019(5) C67 0.030(6) 0.033(6) 0.036(7) 0.002(5) -0.001(5) 0.005(5) C68 0.032(6) 0.035(6) 0.020(6) 0.009(5) 0.000(5) 0.000(5) C69 0.033(2) 0.039(2) 0.029(2) 0.0005(18) 0.0000(18) -0.0087(17) C70 0.024(5) 0.018(5) 0.021(6) 0.001(4) 0.004(4) -0.005(4) C71 0.016(5) 0.023(5) 0.026(6) 0.006(4) -0.003(4) -0.003(4) C72 0.023(5) 0.028(6) 0.020(6) 0.006(4) 0.007(4) 0.003(4) C73 0.029(5) 0.023(5) 0.008(5) -0.001(4) 0.001(4) -0.001(4) C74 0.023(5) 0.025(5) 0.019(6) -0.001(4) -0.004(4) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C45 2.002(11) . ? Pt1 C51 2.025(10) . ? Pt1 N2 2.149(8) . ? Pt1 N1 2.174(8) . ? Pt1 C74 2.960(9) . ? N1 C1 1.333(12) . ? N1 C9 1.398(13) . ? C1 C2 1.378(14) . ? O1 C4S 1.40(2) . ? O1 C1S 1.56(3) . ? C1S C2S 1.53(3) . ? Pt2 C57 2.014(10) . ? Pt2 C63 2.025(10) . ? Pt2 N4 2.124(8) . ? Pt2 N3 2.196(7) . ? N2 C12 1.325(12) . ? N2 C20 1.373(12) . ? C2 C3 1.340(14) . ? C2S C3S 1.52(3) . ? N3 C23 1.349(12) . ? N3 C31 1.381(11) . ? C3 C4A 1.396(16) . ? C3 C4 1.408(16) . ? C3S C4S 1.48(2) . ? N4 C34 1.323(13) . ? N4 C42 1.384(10) . ? C4 C9 1.436(16) . ? C4 C5 1.479(17) . ? C4A C5A 1.387(16) . ? C4A C9 1.397(16) . ? C5 C6 1.38(3) . ? C5A C6A 1.35(3) . ? C6 C7 1.38(3) . ? C6 C10 1.57(3) . ? C6A C10A 1.48(3) . ? C6A C7 1.51(3) . ? C7 C8 1.366(13) . ? C8 C9 1.412(14) . ? C8 C69 1.507(14) . ? C10 C11 1.10(3) . ? C10A C11A 1.45(3) . ? C12 C13 1.376(14) . ? C13 C14 1.358(15) . ? C14 C15 1.435(14) . ? C15 C16 1.405(14) . ? C15 C20 1.424(13) . ? C16 C17 1.340(14) . ? C17 C18 1.440(14) . ? C17 C21 1.512(14) . ? C18 C19 1.374(13) . ? C19 C20 1.427(13) . ? C19 C74 1.512(13) . ? C21 C22 1.482(14) . ? C23 C24 1.377(14) . ? C24 C25 1.367(14) . ? C25 C26 1.413(14) . ? C26 C27 1.403(13) . ? C26 C31 1.430(13) . ? C27 C28 1.357(14) . ? C28 C29 1.426(14) . ? C28 C32 1.509(14) . ? C29 C30 1.371(13) . ? C30 C31 1.428(14) . ? C30 C71 1.476(14) . ? C32 C33 1.515(14) . ? C34 C35 1.407(14) . ? C35 C36 1.330(15) . ? C36 C37 1.32(3) . ? C36 C37A 1.469(15) . ? C37 C38 1.46(3) . ? C37 C42 1.48(3) . ? C37A C38A 1.3900 . ? C37A C42 1.3900 . ? C38 C39 1.31(3) . ? C38A C39A 1.3900 . ? C39 C43 1.48(3) . ? C39 C40 1.49(3) . ? C39A C40A 1.3900 . ? C39A C43A 1.67(2) . ? C40 C41 1.37(3) . ? C40A C41 1.3900 . ? C41 C42 1.3900 . ? C41 C72 1.492(11) . ? C43 C44 1.52(3) . ? C43A C44A 1.43(3) . ? C45 C46 1.365(15) . ? C45 C50 1.417(15) . ? C46 C47 1.386(14) . ? C47 C48 1.382(16) . ? C48 C49 1.364(17) . ? C49 C50 1.385(15) . ? C51 C52 1.380(14) . ? C51 C56 1.433(14) . ? C52 C53 1.383(15) . ? C53 C54 1.396(17) . ? C54 C55 1.398(15) . ? C55 C56 1.389(14) . ? C57 C58 1.391(13) . ? C57 C62 1.403(14) . ? C58 C59 1.379(14) . ? C59 C60 1.374(15) . ? C60 C61 1.377(15) . ? C61 C62 1.400(13) . ? C63 C64 1.387(14) . ? C63 C68 1.405(13) . ? C64 C65 1.380(15) . ? C65 C66 1.372(15) . ? C66 C67 1.362(15) . ? C67 C68 1.389(14) . ? C69 C74 1.378(13) . ? C69 C70 1.402(13) . ? C70 C71 1.378(13) . ? C71 C72 1.400(13) . ? C72 C73 1.402(12) . ? C73 C74 1.388(13) . ? 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 C45 Pt1 C51 91.6(4) . . ? C45 Pt1 N2 88.7(4) . . ? C51 Pt1 N2 177.5(4) . . ? C45 Pt1 N1 166.1(4) . . ? C51 Pt1 N1 92.9(4) . . ? N2 Pt1 N1 86.2(3) . . ? C45 Pt1 C74 106.2(3) . . ? C51 Pt1 C74 111.7(3) . . ? N2 Pt1 C74 70.6(3) . . ? N1 Pt1 C74 84.3(3) . . ? C1 N1 C9 117.0(9) . . ? C1 N1 Pt1 110.4(6) . . ? C9 N1 Pt1 132.4(7) . . ? N1 C1 C2 125.5(10) . . ? C4S O1 C1S 105.1(16) . . ? C2S C1S O1 106.1(16) . . ? C57 Pt2 C63 93.7(4) . . ? C57 Pt2 N4 89.2(4) . . ? C63 Pt2 N4 176.7(4) . . ? C57 Pt2 N3 163.7(3) . . ? C63 Pt2 N3 93.2(3) . . ? N4 Pt2 N3 83.7(3) . . ? C12 N2 C20 118.8(9) . . ? C12 N2 Pt1 114.5(7) . . ? C20 N2 Pt1 126.6(6) . . ? C3 C2 C1 118.6(10) . . ? C3S C2S C1S 101.8(18) . . ? C23 N3 C31 118.6(8) . . ? C23 N3 Pt2 107.4(6) . . ? C31 N3 Pt2 133.8(6) . . ? C2 C3 C4A 118.9(10) . . ? C2 C3 C4 121.0(10) . . ? C4S C3S C2S 104.9(15) . . ? C34 N4 C42 119.7(8) . . ? C34 N4 Pt2 115.6(7) . . ? C42 N4 Pt2 123.7(6) . . ? C3 C4 C9 117.8(10) . . ? C3 C4 C5 125.3(11) . . ? C9 C4 C5 116.9(11) . . ? C5A C4A C3 118.8(12) . . ? C5A C4A C9 119.9(12) . . ? C3 C4A C9 121.3(11) . . ? O1 C4S C3S 112.0(17) . . ? C6 C5 C4 121.1(14) . . ? C6A C5A C4A 122.7(14) . . ? C5 C6 C7 116.6(18) . . ? C5 C6 C10 121(2) . . ? C7 C6 C10 122(2) . . ? C5A C6A C10A 124(2) . . ? C5A C6A C7 116.4(17) . . ? C10A C6A C7 119.2(19) . . ? C8 C7 C6 125.0(13) . . ? C8 C7 C6A 120.2(12) . . ? C7 C8 C9 118.7(10) . . ? C7 C8 C69 118.5(9) . . ? C9 C8 C69 122.6(9) . . ? C4A C9 N1 118.7(10) . . ? C4A C9 C8 120.9(10) . . ? N1 C9 C8 120.3(9) . . ? N1 C9 C4 120.0(10) . . ? C8 C9 C4 119.6(10) . . ? C11 C10 C6 122(3) . . ? C11A C10A C6A 120(2) . . ? N2 C12 C13 123.9(10) . . ? C14 C13 C12 119.9(10) . . ? C13 C14 C15 118.9(10) . . ? C16 C15 C20 120.2(9) . . ? C16 C15 C14 122.1(10) . . ? C20 C15 C14 117.7(9) . . ? C17 C16 C15 122.2(10) . . ? C16 C17 C18 118.6(10) . . ? C16 C17 C21 121.8(10) . . ? C18 C17 C21 119.6(10) . . ? C19 C18 C17 121.3(10) . . ? C18 C19 C20 120.1(9) . . ? C18 C19 C74 114.3(9) . . ? C20 C19 C74 125.5(8) . . ? N2 C20 C15 120.8(9) . . ? N2 C20 C19 121.5(9) . . ? C15 C20 C19 117.7(9) . . ? C22 C21 C17 117.0(9) . . ? N3 C23 C24 124.1(9) . . ? C25 C24 C23 119.0(10) . . ? C24 C25 C26 119.8(10) . . ? C27 C26 C25 120.7(9) . . ? C27 C26 C31 120.5(9) . . ? C25 C26 C31 118.8(9) . . ? C28 C27 C26 120.4(9) . . ? C27 C28 C29 119.4(9) . . ? C27 C28 C32 120.7(9) . . ? C29 C28 C32 119.9(10) . . ? C30 C29 C28 122.7(10) . . ? C29 C30 C31 118.1(10) . . ? C29 C30 C71 119.2(9) . . ? C31 C30 C71 122.6(9) . . ? N3 C31 C30 121.4(9) . . ? N3 C31 C26 119.7(9) . . ? C30 C31 C26 118.9(9) . . ? C28 C32 C33 110.8(9) . . ? N4 C34 C35 123.4(10) . . ? C36 C35 C34 119.3(11) . . ? C37 C36 C35 119.3(15) . . ? C35 C36 C37A 118.2(11) . . ? C36 C37 C38 122(2) . . ? C36 C37 C42 123.2(19) . . ? C38 C37 C42 115(2) . . ? C38A C37A C42 120.0 . . ? C38A C37A C36 120.7(9) . . ? C42 C37A C36 118.9(9) . . ? C39 C38 C37 121(2) . . ? C39A C38A C37A 120.0 . . ? C38 C39 C43 125(2) . . ? C38 C39 C40 121(2) . . ? C43 C39 C40 114(2) . . ? C40A C39A C38A 120.0 . . ? C40A C39A C43A 124.1(13) . . ? C38A C39A C43A 114.7(13) . . ? C41 C40 C39 122(2) . . ? C39A C40A C41 120.0 . . ? C40 C41 C42 116.5(14) . . ? C42 C41 C40A 120.0 . . ? C40 C41 C72 116.3(13) . . ? C42 C41 C72 126.6(7) . . ? C40A C41 C72 113.4(7) . . ? N4 C42 C41 120.7(7) . . ? N4 C42 C37A 118.7(7) . . ? C41 C42 C37A 120.0 . . ? N4 C42 C37 114.9(12) . . ? C41 C42 C37 124.4(13) . . ? C39 C43 C44 116(2) . . ? C44A C43A C39A 106.7(19) . . ? C46 C45 C50 115.0(10) . . ? C46 C45 Pt1 126.1(8) . . ? C50 C45 Pt1 118.8(8) . . ? C45 C46 C47 124.5(11) . . ? C48 C47 C46 119.1(12) . . ? C49 C48 C47 118.7(11) . . ? C48 C49 C50 121.4(12) . . ? C49 C50 C45 121.3(12) . . ? C52 C51 C56 114.9(10) . . ? C52 C51 Pt1 125.6(8) . . ? C56 C51 Pt1 119.3(8) . . ? C51 C52 C53 123.4(12) . . ? C52 C53 C54 121.0(12) . . ? C53 C54 C55 117.7(11) . . ? C56 C55 C54 120.4(12) . . ? C55 C56 C51 122.4(11) . . ? C58 C57 C62 117.0(9) . . ? C58 C57 Pt2 120.8(8) . . ? C62 C57 Pt2 121.5(7) . . ? C59 C58 C57 120.9(10) . . ? C60 C59 C58 121.9(11) . . ? C59 C60 C61 118.5(10) . . ? C60 C61 C62 120.3(10) . . ? C61 C62 C57 121.2(10) . . ? C64 C63 C68 113.7(9) . . ? C64 C63 Pt2 126.1(7) . . ? C68 C63 Pt2 120.2(7) . . ? C65 C64 C63 123.1(10) . . ? C66 C65 C64 121.1(11) . . ? C67 C66 C65 118.3(10) . . ? C66 C67 C68 120.1(10) . . ? C67 C68 C63 123.5(10) . . ? C74 C69 C70 119.4(10) . . ? C74 C69 C8 122.6(9) . . ? C70 C69 C8 117.8(9) . . ? C71 C70 C69 121.7(9) . . ? C70 C71 C72 119.3(9) . . ? C70 C71 C30 119.4(9) . . ? C72 C71 C30 121.3(9) . . ? C71 C72 C73 118.4(9) . . ? C71 C72 C41 120.6(8) . . ? C73 C72 C41 120.2(8) . . ? C74 C73 C72 122.0(9) . . ? C69 C74 C73 119.1(9) . . ? C69 C74 C19 122.9(9) . . ? C73 C74 C19 117.6(8) . . ? C69 C74 Pt1 82.2(6) . . ? C73 C74 Pt1 99.7(6) . . ? C19 C74 Pt1 95.1(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.422 _refine_diff_density_min -1.735 _refine_diff_density_rms 0.213 #===>END data_2a _database_code_depnum_ccdc_archive 'CCDC 747775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H66 Cl6 N4 Pt2' _chemical_formula_weight 1638.21 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2127(10) _cell_length_b 21.2988(18) _cell_length_c 15.1085(14) _cell_angle_alpha 90.00 _cell_angle_beta 98.108(4) _cell_angle_gamma 90.00 _cell_volume 3253.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28097 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 4.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8030 _exptl_absorpt_correction_T_max 0.8746 _exptl_absorpt_process_details 'Bruker Apex 2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28097 _diffrn_reflns_av_R_equivalents 0.0960 _diffrn_reflns_av_sigmaI/netI 0.1246 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7404 _reflns_number_gt 4612 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+3.1380P] 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 7404 _refine_ls_number_parameters 346 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 1.45019(3) 0.370721(11) 0.607354(18) 0.01518(8) Uani 1 1 d . . . Cl1 Cl 1.39377(18) 0.28923(8) 0.71121(12) 0.0254(4) Uani 1 1 d . . . N1 N 1.6282(5) 0.3213(2) 0.5871(4) 0.0179(13) Uani 1 1 d . . . N2 N 1.3554(5) 0.3219(2) 0.4914(3) 0.0141(12) Uani 1 1 d . . . C1 C 1.6870(7) 0.2743(3) 0.6328(5) 0.0283(18) Uani 1 1 d . . . H1A H 1.6663 0.2658 0.6910 0.034 Uiso 1 1 calc R . . C2 C 1.7791(8) 0.2364(3) 0.5980(6) 0.036(2) Uani 1 1 d . . . H2A H 1.8214 0.2033 0.6334 0.044 Uiso 1 1 calc R . . C3 C 1.8088(7) 0.2461(3) 0.5142(5) 0.0289(9) Uani 1 1 d . . . H3A H 1.8701 0.2196 0.4906 0.035 Uiso 1 1 calc R . . C4 C 1.7482(7) 0.2956(3) 0.4632(5) 0.0266(18) Uani 1 1 d . . . C5 C 1.7651(7) 0.3084(3) 0.3744(5) 0.0304(19) Uani 1 1 d . . . H5A H 1.8287 0.2853 0.3475 0.037 Uiso 1 1 calc R . . C6 C 1.6912(7) 0.3537(3) 0.3257(5) 0.0286(19) Uani 1 1 d . A . C7 C 1.6043(7) 0.3915(3) 0.3684(5) 0.0205(16) Uani 1 1 d . . . H7A H 1.5530 0.4227 0.3345 0.025 Uiso 1 1 calc R . . C8 C 1.5919(6) 0.3845(3) 0.4565(4) 0.0186(8) Uani 1 1 d . . . C9 C 1.6589(6) 0.3343(3) 0.5041(5) 0.0186(8) Uani 1 1 d . . . C10 C 1.7051(7) 0.3652(4) 0.2294(5) 0.0377(19) Uani 1 1 d D . . H10B H 1.7810 0.3425 0.2158 0.045 Uiso 1 1 d R A . H10A H 1.7234 0.4091 0.2236 0.045 Uiso 1 1 d R . . C11 C 1.574(4) 0.362(3) 0.166(4) 0.038(4) Uiso 0.20 1 d PD A 1 H11C H 1.5182 0.3980 0.1767 0.058 Uiso 0.20 1 calc PR A 1 H11B H 1.5275 0.3230 0.1759 0.058 Uiso 0.20 1 calc PR A 1 H11A H 1.5916 0.3633 0.1036 0.058 Uiso 0.20 1 calc PR A 1 C11A C 1.589(3) 0.3323(16) 0.171(3) 0.038(4) Uiso 0.30 1 d PD A 2 H11F H 1.6040 0.2868 0.1727 0.058 Uiso 0.30 1 calc PR A 2 H11E H 1.5835 0.3473 0.1095 0.058 Uiso 0.30 1 calc PR A 2 H11D H 1.5066 0.3418 0.1943 0.058 Uiso 0.30 1 calc PR A 2 C11B C 1.583(2) 0.3486(12) 0.161(2) 0.038(4) Uiso 0.50 1 d PD A 3 H11I H 1.6029 0.3568 0.1006 0.058 Uiso 0.50 1 calc PR A 3 H11H H 1.5080 0.3743 0.1727 0.058 Uiso 0.50 1 calc PR A 3 H11G H 1.5618 0.3041 0.1669 0.058 Uiso 0.50 1 calc PR A 3 C12 C 1.3448(7) 0.2602(3) 0.5009(4) 0.0212(16) Uani 1 1 d . . . H12A H 1.4013 0.2401 0.5478 0.025 Uiso 1 1 calc R . . C13 C 1.2549(7) 0.2236(3) 0.4456(5) 0.0266(18) Uani 1 1 d . . . H13A H 1.2507 0.1795 0.4541 0.032 Uiso 1 1 calc R . . C14 C 1.1737(8) 0.2522(3) 0.3792(5) 0.0273(18) Uani 1 1 d . . . H14A H 1.1071 0.2285 0.3438 0.033 Uiso 1 1 calc R . . C15 C 1.1864(7) 0.3165(3) 0.3621(4) 0.0200(16) Uani 1 1 d . . . C16 C 1.1089(7) 0.3459(3) 0.2893(5) 0.0274(18) Uani 1 1 d . . . H16A H 1.0407 0.3227 0.2545 0.033 Uiso 1 1 calc R . . C17 C 1.1291(7) 0.4063(3) 0.2678(5) 0.0280(19) Uani 1 1 d . B . C18 C 1.2272(7) 0.4398(3) 0.3226(5) 0.0235(17) Uani 1 1 d . . . H18A H 1.2431 0.4818 0.3059 0.028 Uiso 1 1 calc R . . C19 C 1.3032(7) 0.4169(3) 0.3992(5) 0.0289(9) Uani 1 1 d . . . C20 C 1.2840(6) 0.3525(3) 0.4190(4) 0.0175(15) Uani 1 1 d . . . C21 C 1.0476(7) 0.4404(3) 0.1905(4) 0.0304(8) Uani 1 1 d D . . H21B H 1.0909 0.4793 0.1809 0.036 Uiso 1 1 d R B . H21A H 0.9645 0.4505 0.2098 0.036 Uiso 1 1 d R . . C22 C 1.0243(14) 0.4038(6) 0.1018(6) 0.0186(8) Uani 0.50 1 d PD B 1 H22C H 0.9639 0.4276 0.0579 0.028 Uiso 0.50 1 calc PR B 1 H22B H 0.9853 0.3628 0.1118 0.028 Uiso 0.50 1 calc PR B 1 H22A H 1.1088 0.3978 0.0792 0.028 Uiso 0.50 1 calc PR B 1 C22A C 0.9859(13) 0.3961(6) 0.1155(7) 0.0186(8) Uani 0.50 1 d PD B 2 H22F H 0.9386 0.4209 0.0664 0.028 Uiso 0.50 1 calc PR B 2 H22E H 0.9240 0.3675 0.1389 0.028 Uiso 0.50 1 calc PR B 2 H22D H 1.0560 0.3717 0.0933 0.028 Uiso 0.50 1 calc PR B 2 C23 C 1.5357(7) 0.4142(3) 0.7224(4) 0.0214(16) Uani 1 1 d . . . C24 C 1.6704(7) 0.4062(3) 0.7534(5) 0.0216(16) Uani 1 1 d . . . H24A H 1.7240 0.3848 0.7166 0.026 Uiso 1 1 calc R . . C25 C 1.7284(8) 0.4285(3) 0.8363(5) 0.0289(9) Uani 1 1 d . . . H25A H 1.8205 0.4226 0.8545 0.035 Uiso 1 1 calc R . . C26 C 1.6545(7) 0.4589(3) 0.8922(5) 0.0289(9) Uani 1 1 d . . . H26A H 1.6940 0.4726 0.9497 0.035 Uiso 1 1 calc R . . C27 C 1.5233(7) 0.4690(3) 0.8641(5) 0.0304(8) Uani 1 1 d . . . H27A H 1.4720 0.4915 0.9012 0.036 Uiso 1 1 calc R . . C28 C 1.4628(8) 0.4463(4) 0.7801(5) 0.037(2) Uani 1 1 d . . . H28A H 1.3708 0.4529 0.7625 0.044 Uiso 1 1 calc R . . C29 C 1.2678(6) 0.4100(3) 0.6098(4) 0.0181(15) Uani 1 1 d . . . C30 C 1.2440(7) 0.4729(3) 0.6150(4) 0.0231(17) Uani 1 1 d . . . H30A H 1.3168 0.5011 0.6207 0.028 Uiso 1 1 calc R . . C31 C 1.1181(7) 0.4970(3) 0.6124(5) 0.0296(18) Uani 1 1 d . . . H31A H 1.1058 0.5410 0.6168 0.036 Uiso 1 1 calc R . . C32 C 1.0091(8) 0.4573(3) 0.6034(5) 0.0304(8) Uani 1 1 d . . . H32A H 0.9224 0.4738 0.6022 0.036 Uiso 1 1 calc R . . C33 C 1.0287(7) 0.3942(4) 0.5962(5) 0.0325(19) Uani 1 1 d . . . H33A H 0.9550 0.3666 0.5882 0.039 Uiso 1 1 calc R . . C34 C 1.1567(6) 0.3700(3) 0.6006(5) 0.0261(16) Uani 1 1 d . . . H34A H 1.1690 0.3259 0.5973 0.031 Uiso 1 1 calc R . . C35 C 1.5169(7) 0.4308(3) 0.5094(5) 0.0304(8) Uani 1 1 d . . . C36 C 1.4012(6) 0.4592(3) 0.4517(5) 0.0186(8) Uani 1 1 d . . . C37 C 1.3876(8) 0.5219(3) 0.4473(5) 0.0304(8) Uani 1 1 d . . . H37A H 1.3092 0.5376 0.4132 0.036 Uiso 1 1 calc R . . Cl1S Cl 1.5226(3) 0.17898(15) 0.3292(3) 0.0968(11) Uani 1 1 d . . . Cl2S Cl 1.6830(4) 0.08020(18) 0.4185(2) 0.1053(12) Uani 1 1 d . . . C1S C 1.6499(10) 0.1248(5) 0.3229(7) 0.066(3) Uani 1 1 d . . . H1SB H 1.6247 0.0968 0.2711 0.079 Uiso 1 1 calc R . . H1SA H 1.7311 0.1477 0.3130 0.079 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 0.01435(13) 0.01301(13) 0.01868(13) 0.00044(15) 0.00405(9) -0.00073(14) Cl1 0.0271(10) 0.0224(9) 0.0270(10) 0.0084(8) 0.0051(8) -0.0005(7) N1 0.014(3) 0.017(3) 0.023(3) 0.001(3) 0.002(3) 0.002(2) N2 0.013(3) 0.010(3) 0.020(3) 0.001(2) 0.004(2) -0.001(2) C1 0.019(4) 0.025(4) 0.039(5) 0.003(4) -0.001(4) -0.002(3) C2 0.025(5) 0.025(4) 0.056(6) 0.010(4) -0.004(4) 0.011(3) C3 0.028(2) 0.025(2) 0.032(2) -0.0029(18) -0.0018(18) -0.0007(17) C4 0.012(4) 0.024(4) 0.046(5) -0.002(4) 0.010(4) -0.002(3) C5 0.019(4) 0.033(5) 0.042(5) -0.010(4) 0.016(4) 0.000(3) C6 0.026(4) 0.032(5) 0.029(4) -0.012(3) 0.009(4) -0.013(3) C7 0.019(4) 0.020(4) 0.025(4) -0.003(3) 0.013(3) -0.001(3) C8 0.012(2) 0.019(2) 0.026(2) -0.0023(16) 0.0072(16) -0.0032(15) C9 0.012(2) 0.019(2) 0.026(2) -0.0023(16) 0.0072(16) -0.0032(15) C10 0.043(5) 0.039(5) 0.035(5) -0.003(4) 0.018(4) 0.000(4) C12 0.028(4) 0.016(4) 0.019(4) 0.007(3) 0.004(3) 0.000(3) C13 0.030(5) 0.012(4) 0.038(5) 0.001(3) 0.005(4) -0.002(3) C14 0.037(5) 0.019(4) 0.025(4) -0.002(3) 0.002(4) -0.003(3) C15 0.023(4) 0.018(4) 0.021(4) -0.003(3) 0.011(3) 0.000(3) C16 0.030(5) 0.017(4) 0.031(4) 0.000(3) -0.007(4) -0.010(3) C17 0.028(5) 0.024(4) 0.029(4) -0.002(3) -0.006(4) -0.005(3) C18 0.031(5) 0.013(4) 0.027(4) 0.000(3) 0.006(3) -0.008(3) C19 0.028(2) 0.025(2) 0.032(2) -0.0029(18) -0.0018(18) -0.0007(17) C20 0.016(4) 0.012(3) 0.025(4) -0.004(3) 0.003(3) -0.001(3) C21 0.026(2) 0.033(2) 0.031(2) -0.0039(16) 0.0012(16) 0.0021(15) C22 0.012(2) 0.019(2) 0.026(2) -0.0023(16) 0.0072(16) -0.0032(15) C22A 0.012(2) 0.019(2) 0.026(2) -0.0023(16) 0.0072(16) -0.0032(15) C23 0.027(4) 0.019(4) 0.018(4) 0.005(3) 0.000(3) -0.005(3) C24 0.031(5) 0.010(3) 0.024(4) 0.005(3) 0.005(3) -0.001(3) C25 0.028(2) 0.025(2) 0.032(2) -0.0029(18) -0.0018(18) -0.0007(17) C26 0.028(2) 0.025(2) 0.032(2) -0.0029(18) -0.0018(18) -0.0007(17) C27 0.026(2) 0.033(2) 0.031(2) -0.0039(16) 0.0012(16) 0.0021(15) C28 0.028(5) 0.054(5) 0.028(5) -0.006(4) 0.002(4) 0.000(4) C29 0.016(4) 0.020(4) 0.020(4) -0.003(3) 0.007(3) 0.000(3) C30 0.019(4) 0.030(4) 0.023(4) 0.001(3) 0.009(3) -0.001(3) C31 0.033(5) 0.026(4) 0.034(5) -0.003(3) 0.017(4) 0.008(3) C32 0.026(2) 0.033(2) 0.031(2) -0.0039(16) 0.0012(16) 0.0021(15) C33 0.016(4) 0.041(5) 0.040(5) -0.005(4) 0.001(4) -0.008(3) C34 0.022(4) 0.022(4) 0.036(4) -0.003(4) 0.010(3) -0.003(3) C35 0.026(2) 0.033(2) 0.031(2) -0.0039(16) 0.0012(16) 0.0021(15) C36 0.012(2) 0.019(2) 0.026(2) -0.0023(16) 0.0072(16) -0.0032(15) C37 0.026(2) 0.033(2) 0.031(2) -0.0039(16) 0.0012(16) 0.0021(15) Cl1S 0.075(2) 0.083(2) 0.144(3) -0.039(2) 0.055(2) -0.0223(17) Cl2S 0.138(3) 0.126(3) 0.061(2) 0.0087(19) 0.045(2) -0.014(2) C1S 0.064(7) 0.073(7) 0.068(7) -0.014(6) 0.037(5) -0.018(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C29 2.047(7) . ? Pt1 C23 2.052(7) . ? Pt1 C35 2.139(8) . ? Pt1 N2 2.147(5) . ? Pt1 N1 2.159(5) . ? Pt1 Cl1 2.4620(17) . ? N1 C1 1.313(8) . ? N1 C9 1.363(8) . ? N2 C12 1.329(8) . ? N2 C20 1.389(8) . ? C1 C2 1.397(10) . ? C2 C3 1.359(11) . ? C3 C4 1.398(10) . ? C4 C5 1.403(10) . ? C4 C9 1.432(9) . ? C5 C6 1.374(10) . ? C6 C7 1.419(10) . ? C6 C10 1.501(10) . ? C7 C8 1.362(9) . ? C8 C9 1.410(9) . ? C8 C35 1.540(9) . ? C10 C11A 1.5399(10) . ? C10 C11B 1.5399(10) . ? C10 C11 1.5400(10) . ? C12 C13 1.391(9) . ? C13 C14 1.353(9) . ? C14 C15 1.402(9) . ? C15 C16 1.409(9) . ? C15 C20 1.443(9) . ? C16 C17 1.349(9) . ? C17 C18 1.402(9) . ? C17 C21 1.519(9) . ? C18 C19 1.388(9) . ? C19 C20 1.422(9) . ? C19 C36 1.490(9) . ? C21 C22 1.5396(10) . ? C21 C22A 1.5401(10) . ? C23 C24 1.399(9) . ? C23 C28 1.402(10) . ? C24 C25 1.392(9) . ? C25 C26 1.372(10) . ? C26 C27 1.365(10) . ? C27 C28 1.415(10) . ? C29 C30 1.366(9) . ? C29 C34 1.409(9) . ? C30 C31 1.380(9) . ? C31 C32 1.389(10) . ? C32 C33 1.365(10) . ? C33 C34 1.398(10) . ? C35 C37 1.488(10) 3_866 ? C35 C36 1.494(9) . ? C36 C37 1.342(9) . ? C37 C35 1.488(10) 3_866 ? Cl1S C1S 1.751(10) . ? Cl2S C1S 1.722(10) . ? 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 C29 Pt1 C23 94.6(3) . . ? C29 Pt1 C35 98.5(3) . . ? C23 Pt1 C35 100.2(3) . . ? C29 Pt1 N2 84.6(2) . . ? C23 Pt1 N2 176.9(2) . . ? C35 Pt1 N2 82.9(2) . . ? C29 Pt1 N1 171.2(2) . . ? C23 Pt1 N1 94.2(2) . . ? C35 Pt1 N1 80.6(2) . . ? N2 Pt1 N1 86.6(2) . . ? C29 Pt1 Cl1 88.92(19) . . ? C23 Pt1 Cl1 83.59(18) . . ? C35 Pt1 Cl1 171.3(2) . . ? N2 Pt1 Cl1 93.42(14) . . ? N1 Pt1 Cl1 91.40(15) . . ? C1 N1 C9 119.4(6) . . ? C1 N1 Pt1 129.0(5) . . ? C9 N1 Pt1 109.9(4) . . ? C12 N2 C20 120.6(5) . . ? C12 N2 Pt1 115.1(4) . . ? C20 N2 Pt1 122.8(4) . . ? N1 C1 C2 121.7(7) . . ? C3 C2 C1 120.8(7) . . ? C2 C3 C4 119.3(7) . . ? C3 C4 C5 124.6(7) . . ? C3 C4 C9 117.1(7) . . ? C5 C4 C9 118.3(6) . . ? C6 C5 C4 121.0(7) . . ? C5 C6 C7 119.1(7) . . ? C5 C6 C10 120.9(7) . . ? C7 C6 C10 120.0(7) . . ? C8 C7 C6 122.2(6) . . ? C7 C8 C9 118.4(6) . . ? C7 C8 C35 123.9(6) . . ? C9 C8 C35 117.5(6) . . ? N1 C9 C8 117.7(6) . . ? N1 C9 C4 121.6(6) . . ? C8 C9 C4 120.6(6) . . ? C6 C10 C11A 108.0(18) . . ? C6 C10 C11B 115.7(16) . . ? C6 C10 C11 114(3) . . ? N2 C12 C13 123.1(6) . . ? C14 C13 C12 118.5(6) . . ? C13 C14 C15 120.9(7) . . ? C14 C15 C16 121.5(6) . . ? C14 C15 C20 118.9(6) . . ? C16 C15 C20 119.5(6) . . ? C17 C16 C15 121.6(7) . . ? C16 C17 C18 117.6(7) . . ? C16 C17 C21 123.7(6) . . ? C18 C17 C21 118.6(6) . . ? C19 C18 C17 125.6(6) . . ? C18 C19 C20 115.9(6) . . ? C18 C19 C36 119.1(6) . . ? C20 C19 C36 125.0(6) . . ? N2 C20 C19 123.0(6) . . ? N2 C20 C15 117.5(5) . . ? C19 C20 C15 119.5(6) . . ? C17 C21 C22 115.3(8) . . ? C17 C21 C22A 113.3(8) . . ? C24 C23 C28 115.7(6) . . ? C24 C23 Pt1 120.6(5) . . ? C28 C23 Pt1 123.2(5) . . ? C25 C24 C23 122.2(7) . . ? C26 C25 C24 121.0(7) . . ? C27 C26 C25 118.9(7) . . ? C26 C27 C28 120.7(7) . . ? C23 C28 C27 121.4(7) . . ? C30 C29 C34 116.8(6) . . ? C30 C29 Pt1 124.8(5) . . ? C34 C29 Pt1 118.2(5) . . ? C29 C30 C31 122.3(7) . . ? C30 C31 C32 120.5(7) . . ? C33 C32 C31 118.8(7) . . ? C32 C33 C34 120.4(7) . . ? C33 C34 C29 121.1(7) . . ? C37 C35 C36 113.4(6) 3_866 . ? C37 C35 C8 108.6(6) 3_866 . ? C36 C35 C8 111.6(6) . . ? C37 C35 Pt1 110.7(5) 3_866 . ? C36 C35 Pt1 110.1(5) . . ? C8 C35 Pt1 101.9(4) . . ? C37 C36 C19 121.2(6) . . ? C37 C36 C35 120.0(6) . . ? C19 C36 C35 118.8(6) . . ? C36 C37 C35 126.5(7) . 3_866 ? Cl2S C1S Cl1S 112.1(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.780 _refine_diff_density_min -1.363 _refine_diff_density_rms 0.200