# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_address 'University of Western Ontario' _publ_contact_author_address 'University of Western Ontario' _publ_contact_author_email pudd@uwo.ca _publ_contact_author_phone 519-661-2111 #TrackingRef '- allcifs.cif' _publ_contact_author_name Puddephatt _publ_author_name R.J.Puddephatt #===END data_1 _database_code_depnum_ccdc_archive 'CCDC 869542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H23 Cl N4 Pt' _chemical_formula_sum 'C21 H23 Cl N4 Pt' _chemical_formula_weight 561.97 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)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.164(4) _cell_length_b 12.904(3) _cell_length_c 8.2595(16) _cell_angle_alpha 90.00 _cell_angle_beta 93.249(7) _cell_angle_gamma 90.00 _cell_volume 1932.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2592 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 19.52 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 7.411 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7711 _exptl_absorpt_correction_T_max 0.8720 _exptl_absorpt_process_details 'SADABS (Bruker, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44599 _diffrn_reflns_av_R_equivalents 0.1391 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3802 _reflns_number_gt 2679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.8675P] 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 3802 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0501 _refine_ls_wR_factor_gt 0.0425 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.310143(14) 0.37917(2) 0.44254(3) 0.01781(7) Uani 1 1 d . . . Cl1 Cl 0.37321(9) 0.53449(12) 0.46261(18) 0.0253(4) Uani 1 1 d . . . N1 N 0.2652(3) 0.2392(4) 0.4186(5) 0.0160(12) Uani 1 1 d . . . N2 N 0.1967(3) 0.2288(4) 0.3550(6) 0.0207(13) Uani 1 1 d . . . N3 N 0.3961(3) 0.2860(4) 0.5400(5) 0.0183(12) Uani 1 1 d . . . N4 N 0.0494(3) 0.0667(4) 0.3298(6) 0.0303(14) Uani 1 1 d . . . C1 C 0.1729(3) 0.1343(5) 0.3156(6) 0.0177(14) Uani 1 1 d . . . C2 C 0.2178(4) 0.0448(5) 0.3221(7) 0.0188(15) Uani 1 1 d . . . C3 C 0.1904(4) -0.0544(4) 0.2422(7) 0.0226(16) Uani 1 1 d . . . H3A H 0.2325 -0.0883 0.1923 0.027 Uiso 1 1 calc R . . H3B H 0.1537 -0.0363 0.1536 0.027 Uiso 1 1 calc R . . C4 C 0.1552(4) -0.1332(5) 0.3543(7) 0.0299(16) Uani 1 1 d . . . H4A H 0.1077 -0.1045 0.3872 0.036 Uiso 1 1 calc R . . H4B H 0.1440 -0.1972 0.2915 0.036 Uiso 1 1 calc R . . C5 C 0.2018(4) -0.1623(5) 0.5072(7) 0.037(2) Uani 1 1 d . . . H5A H 0.2048 -0.1009 0.5791 0.044 Uiso 1 1 calc R . . H5B H 0.1752 -0.2170 0.5645 0.044 Uiso 1 1 calc R . . C6 C 0.2798(4) -0.2004(5) 0.4864(8) 0.037(2) Uani 1 1 d . . . H6A H 0.2826 -0.2278 0.3750 0.044 Uiso 1 1 calc R . . H6B H 0.2901 -0.2586 0.5625 0.044 Uiso 1 1 calc R . . C7 C 0.3405(3) -0.1175(5) 0.5156(6) 0.0307(16) Uani 1 1 d . . . H7A H 0.3338 -0.0847 0.6221 0.037 Uiso 1 1 calc R . . H7B H 0.3888 -0.1531 0.5228 0.037 Uiso 1 1 calc R . . C8 C 0.3434(4) -0.0310(5) 0.3873(7) 0.0257(17) Uani 1 1 d . . . H8A H 0.3933 -0.0001 0.3967 0.031 Uiso 1 1 calc R . . H8B H 0.3375 -0.0638 0.2790 0.031 Uiso 1 1 calc R . . C9 C 0.2884(3) 0.0557(4) 0.3921(6) 0.0164(15) Uani 1 1 d . . . C10 C 0.3094(4) 0.1554(4) 0.4513(7) 0.0161(13) Uani 1 1 d . . . C11 C 0.3799(3) 0.1827(5) 0.5408(7) 0.0189(15) Uani 1 1 d . . . C12 C 0.4590(4) 0.3197(5) 0.6139(7) 0.0249(16) Uani 1 1 d . . . H12 H 0.4709 0.3912 0.6085 0.030 Uiso 1 1 calc R . . C13 C 0.5070(4) 0.2539(5) 0.6974(7) 0.0265(17) Uani 1 1 d . . . H13 H 0.5520 0.2796 0.7460 0.032 Uiso 1 1 calc R . . C14 C 0.4896(4) 0.1509(5) 0.7104(7) 0.0265(17) Uani 1 1 d . . . H14 H 0.5211 0.1051 0.7722 0.032 Uiso 1 1 calc R . . C15 C 0.4250(3) 0.1149(5) 0.6311(6) 0.0222(14) Uani 1 1 d . . . H15 H 0.4118 0.0440 0.6388 0.027 Uiso 1 1 calc R . . C16 C 0.0943(3) 0.1321(5) 0.2568(7) 0.0243(15) Uani 1 1 d . . . C17 C -0.0214(4) 0.0639(5) 0.2749(8) 0.0352(19) Uani 1 1 d . . . H17 H -0.0536 0.0184 0.3273 0.042 Uiso 1 1 calc R . . C18 C -0.0505(3) 0.1222(6) 0.1481(7) 0.0299(16) Uani 1 1 d . . . H18 H -0.1011 0.1167 0.1130 0.036 Uiso 1 1 calc R . . C19 C -0.0040(4) 0.1894(6) 0.0731(8) 0.038(2) Uani 1 1 d . . . H19 H -0.0222 0.2305 -0.0157 0.046 Uiso 1 1 calc R . . C20 C 0.0679(4) 0.1964(5) 0.1268(8) 0.0329(18) Uani 1 1 d . . . H20 H 0.1000 0.2437 0.0779 0.040 Uiso 1 1 calc R . . C21 C 0.2182(3) 0.4559(4) 0.3461(6) 0.0150(14) Uani 1 1 d . . . H21A H 0.2084 0.4346 0.2331 0.023 Uiso 1 1 calc R . . H21B H 0.2269 0.5308 0.3507 0.023 Uiso 1 1 calc R . . H21C H 0.1756 0.4387 0.4088 0.023 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 0.01809(13) 0.01659(12) 0.01890(12) 0.00138(15) 0.00231(9) 0.00005(16) Cl1 0.0323(11) 0.0199(9) 0.0236(9) -0.0017(7) 0.0022(8) -0.0055(8) N1 0.012(3) 0.015(3) 0.021(3) 0.002(2) 0.005(2) 0.001(2) N2 0.017(3) 0.017(3) 0.028(3) 0.006(2) 0.000(3) 0.000(3) N3 0.015(3) 0.022(3) 0.017(3) -0.002(2) 0.001(2) -0.001(3) N4 0.020(4) 0.032(4) 0.039(4) 0.007(3) 0.003(3) -0.011(3) C1 0.019(4) 0.020(4) 0.015(3) 0.004(3) 0.004(3) 0.000(3) C2 0.029(4) 0.014(4) 0.014(3) 0.007(3) 0.005(3) 0.001(3) C3 0.030(4) 0.011(3) 0.028(4) -0.001(3) 0.010(3) 0.002(3) C4 0.043(4) 0.015(4) 0.033(4) -0.002(3) 0.006(3) -0.004(4) C5 0.064(6) 0.018(4) 0.030(4) 0.002(3) 0.009(4) -0.007(4) C6 0.068(6) 0.013(4) 0.030(4) 0.002(3) 0.007(4) 0.000(4) C7 0.045(5) 0.023(4) 0.022(3) 0.000(4) -0.006(3) 0.011(4) C8 0.031(4) 0.028(4) 0.018(4) -0.004(3) -0.001(3) 0.014(3) C9 0.023(4) 0.015(4) 0.012(3) 0.004(3) 0.006(3) 0.003(3) C10 0.018(3) 0.019(3) 0.012(3) 0.006(3) 0.005(2) 0.001(3) C11 0.016(4) 0.022(4) 0.019(3) -0.001(3) 0.005(3) 0.001(3) C12 0.021(4) 0.028(4) 0.026(4) 0.001(3) 0.003(3) -0.005(3) C13 0.021(4) 0.032(5) 0.026(4) -0.004(3) -0.003(3) 0.005(3) C14 0.027(4) 0.035(5) 0.017(3) 0.003(3) -0.001(3) 0.008(3) C15 0.024(4) 0.024(4) 0.019(3) 0.007(3) 0.004(3) 0.003(4) C16 0.027(4) 0.024(4) 0.021(3) -0.009(3) -0.003(3) -0.004(4) C17 0.032(5) 0.026(4) 0.049(5) 0.002(4) 0.011(4) -0.013(4) C18 0.017(4) 0.039(4) 0.033(4) -0.014(4) -0.005(3) -0.005(4) C19 0.027(5) 0.054(5) 0.034(4) 0.012(4) -0.002(4) -0.001(4) C20 0.024(4) 0.030(4) 0.045(5) 0.013(4) 0.005(4) 0.000(4) C21 0.014(4) 0.008(3) 0.023(3) 0.002(3) 0.000(3) 0.003(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 N1 1.988(5) . ? Pt1 C21 2.062(5) . ? Pt1 N3 2.095(5) . ? Pt1 Cl1 2.3099(16) . ? N1 N2 1.329(6) . ? N1 C10 1.365(7) . ? N2 C1 1.328(7) . ? N3 C12 1.337(7) . ? N3 C11 1.366(7) . ? N4 C16 1.340(8) . ? N4 C17 1.340(8) . ? C1 C2 1.413(8) . ? C1 C16 1.481(8) . ? C2 C9 1.384(8) . ? C2 C3 1.511(8) . ? C3 C4 1.539(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.528(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.518(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.544(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.542(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.503(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.421(7) . ? C10 C11 1.484(8) . ? C11 C15 1.387(8) . ? C12 C13 1.374(8) . ? C12 H12 0.9500 . ? C13 C14 1.371(8) . ? C13 H13 0.9500 . ? C14 C15 1.391(8) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C20 1.420(8) . ? C17 C18 1.372(8) . ? C17 H17 0.9500 . ? C18 C19 1.382(9) . ? C18 H18 0.9500 . ? C19 C20 1.357(9) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 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 N1 Pt1 C21 94.5(2) . . ? N1 Pt1 N3 79.0(2) . . ? C21 Pt1 N3 173.5(2) . . ? N1 Pt1 Cl1 174.28(15) . . ? C21 Pt1 Cl1 89.93(16) . . ? N3 Pt1 Cl1 96.56(15) . . ? N2 N1 C10 121.8(5) . . ? N2 N1 Pt1 120.0(4) . . ? C10 N1 Pt1 117.8(4) . . ? C1 N2 N1 118.2(5) . . ? C12 N3 C11 119.6(5) . . ? C12 N3 Pt1 126.0(4) . . ? C11 N3 Pt1 113.9(4) . . ? C16 N4 C17 117.5(6) . . ? N2 C1 C2 124.2(6) . . ? N2 C1 C16 113.1(6) . . ? C2 C1 C16 122.6(6) . . ? C9 C2 C1 116.8(5) . . ? C9 C2 C3 122.9(6) . . ? C1 C2 C3 120.1(6) . . ? C2 C3 C4 115.8(5) . . ? C2 C3 H3A 108.3 . . ? C4 C3 H3A 108.3 . . ? C2 C3 H3B 108.3 . . ? C4 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? C5 C4 C3 115.5(5) . . ? C5 C4 H4A 108.4 . . ? C3 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? C3 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? C6 C5 C4 117.6(5) . . ? C6 C5 H5A 107.9 . . ? C4 C5 H5A 107.9 . . ? C6 C5 H5B 107.9 . . ? C4 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? C5 C6 C7 114.9(5) . . ? C5 C6 H6A 108.6 . . ? C7 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? C7 C6 H6B 108.6 . . ? H6A C6 H6B 107.5 . . ? C8 C7 C6 116.5(5) . . ? C8 C7 H7A 108.2 . . ? C6 C7 H7A 108.2 . . ? C8 C7 H7B 108.2 . . ? C6 C7 H7B 108.2 . . ? H7A C7 H7B 107.3 . . ? C9 C8 C7 118.2(5) . . ? C9 C8 H8A 107.8 . . ? C7 C8 H8A 107.8 . . ? C9 C8 H8B 107.8 . . ? C7 C8 H8B 107.8 . . ? H8A C8 H8B 107.1 . . ? C2 C9 C10 117.5(6) . . ? C2 C9 C8 121.0(5) . . ? C10 C9 C8 121.1(6) . . ? N1 C10 C9 120.3(6) . . ? N1 C10 C11 113.1(5) . . ? C9 C10 C11 126.5(5) . . ? N3 C11 C15 119.8(6) . . ? N3 C11 C10 114.2(5) . . ? C15 C11 C10 125.8(6) . . ? N3 C12 C13 122.0(6) . . ? N3 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C14 C13 C12 119.7(6) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 118.6(6) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C11 C15 C14 120.0(6) . . ? C11 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? N4 C16 C20 121.3(6) . . ? N4 C16 C1 117.7(6) . . ? C20 C16 C1 121.0(6) . . ? N4 C17 C18 124.4(6) . . ? N4 C17 H17 117.8 . . ? C18 C17 H17 117.8 . . ? C17 C18 C19 117.8(6) . . ? C17 C18 H18 121.1 . . ? C19 C18 H18 121.1 . . ? C20 C19 C18 119.8(7) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C16 119.1(6) . . ? C19 C20 H20 120.5 . . ? C16 C20 H20 120.5 . . ? Pt1 C21 H21A 109.5 . . ? Pt1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Pt1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Pt1 N1 N2 0.3(4) . . . . ? N3 Pt1 N1 N2 179.3(4) . . . . ? C21 Pt1 N1 C10 172.7(4) . . . . ? N3 Pt1 N1 C10 -8.2(4) . . . . ? C10 N1 N2 C1 -3.3(8) . . . . ? Pt1 N1 N2 C1 168.8(4) . . . . ? N1 Pt1 N3 C12 -173.0(5) . . . . ? Cl1 Pt1 N3 C12 10.7(5) . . . . ? N1 Pt1 N3 C11 -0.7(4) . . . . ? Cl1 Pt1 N3 C11 -177.0(4) . . . . ? N1 N2 C1 C2 -6.5(8) . . . . ? N1 N2 C1 C16 176.0(5) . . . . ? N2 C1 C2 C9 7.9(8) . . . . ? C16 C1 C2 C9 -174.8(5) . . . . ? N2 C1 C2 C3 -167.0(5) . . . . ? C16 C1 C2 C3 10.4(8) . . . . ? C9 C2 C3 C4 89.1(7) . . . . ? C1 C2 C3 C4 -96.4(7) . . . . ? C2 C3 C4 C5 -52.7(8) . . . . ? C3 C4 C5 C6 -53.5(8) . . . . ? C4 C5 C6 C7 98.7(7) . . . . ? C5 C6 C7 C8 -70.2(7) . . . . ? C6 C7 C8 C9 78.3(7) . . . . ? C1 C2 C9 C10 0.1(8) . . . . ? C3 C2 C9 C10 174.9(5) . . . . ? C1 C2 C9 C8 -172.7(5) . . . . ? C3 C2 C9 C8 2.1(9) . . . . ? C7 C8 C9 C2 -82.6(7) . . . . ? C7 C8 C9 C10 104.8(7) . . . . ? N2 N1 C10 C9 11.2(9) . . . . ? Pt1 N1 C10 C9 -161.1(4) . . . . ? N2 N1 C10 C11 -172.7(5) . . . . ? Pt1 N1 C10 C11 15.0(6) . . . . ? C2 C9 C10 N1 -9.2(9) . . . . ? C8 C9 C10 N1 163.6(5) . . . . ? C2 C9 C10 C11 175.3(6) . . . . ? C8 C9 C10 C11 -11.9(9) . . . . ? C12 N3 C11 C15 6.2(8) . . . . ? Pt1 N3 C11 C15 -166.6(4) . . . . ? C12 N3 C11 C10 -178.6(5) . . . . ? Pt1 N3 C11 C10 8.5(6) . . . . ? N1 C10 C11 N3 -15.1(7) . . . . ? C9 C10 C11 N3 160.7(6) . . . . ? N1 C10 C11 C15 159.7(5) . . . . ? C9 C10 C11 C15 -24.5(10) . . . . ? C11 N3 C12 C13 -2.8(9) . . . . ? Pt1 N3 C12 C13 169.1(4) . . . . ? N3 C12 C13 C14 -1.9(10) . . . . ? C12 C13 C14 C15 3.1(9) . . . . ? N3 C11 C15 C14 -4.9(9) . . . . ? C10 C11 C15 C14 -179.5(6) . . . . ? C13 C14 C15 C11 0.3(9) . . . . ? C17 N4 C16 C20 0.3(9) . . . . ? C17 N4 C16 C1 -179.1(6) . . . . ? N2 C1 C16 N4 -126.4(6) . . . . ? C2 C1 C16 N4 56.0(8) . . . . ? N2 C1 C16 C20 54.1(8) . . . . ? C2 C1 C16 C20 -123.5(7) . . . . ? C16 N4 C17 C18 0.9(10) . . . . ? N4 C17 C18 C19 -0.8(11) . . . . ? C17 C18 C19 C20 -0.6(10) . . . . ? C18 C19 C20 C16 1.7(10) . . . . ? N4 C16 C20 C19 -1.6(10) . . . . ? C1 C16 C20 C19 177.8(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.266 _refine_diff_density_min -1.196 _refine_diff_density_rms 0.205 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 869543' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H26 N4 Pt' _chemical_formula_sum 'C22 H26 N4 Pt' _chemical_formula_weight 541.56 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' 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)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4230(15) _cell_length_b 18.826(2) _cell_length_c 8.6433(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.068(4) _cell_angle_gamma 90.00 _cell_volume 1951.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3309 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 19.66 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 7.203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7866 _exptl_absorpt_correction_T_max 0.9315 _exptl_absorpt_process_details 'SADABS (Bruker, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46180 _diffrn_reflns_av_R_equivalents 0.1466 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.09 _reflns_number_total 4299 _reflns_number_gt 2973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+2.2256P] 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 4299 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0585 _refine_ls_wR_factor_gt 0.0512 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 1.09382(2) 0.119471(12) 0.78557(3) 0.01693(7) Uani 1 1 d . . . N1 N 1.1100(4) 0.0123(2) 0.7259(6) 0.0177(12) Uani 1 1 d . . . N2 N 0.9450(4) 0.0750(2) 0.7987(5) 0.0147(11) Uani 1 1 d . . . N4 N 0.6056(4) 0.1391(3) 0.8875(6) 0.0304(14) Uani 1 1 d . . . C23 C 1.2494(4) 0.1605(2) 0.7848(6) 0.0045(11) Uani 1 1 d . . . H23A H 1.2402 0.1974 0.7025 0.007 Uiso 1 1 calc R . . H23B H 1.2965 0.1223 0.7614 0.007 Uiso 1 1 calc R . . H23C H 1.2846 0.1810 0.8900 0.007 Uiso 1 1 calc R . . C1 C 1.0179(5) -0.0292(3) 0.7122(7) 0.0132(13) Uani 1 1 d . . . C2 C 0.9269(5) 0.0045(3) 0.7729(7) 0.0138(13) Uani 1 1 d . . . N3 N 0.8737(4) 0.1158(3) 0.8499(5) 0.0198(11) Uani 1 1 d . . . C4 C 0.7840(5) 0.0865(3) 0.8816(7) 0.0174(14) Uani 1 1 d . . . C5 C 0.7591(5) 0.0137(3) 0.8637(7) 0.0175(14) Uani 1 1 d . . . C6 C 0.6634(5) -0.0164(3) 0.9208(7) 0.0214(15) Uani 1 1 d . . . H6A H 0.6477 0.0166 1.0016 0.026 Uiso 1 1 calc R . . H6B H 0.6878 -0.0620 0.9756 0.026 Uiso 1 1 calc R . . C7 C 0.5532(5) -0.0294(3) 0.7907(8) 0.0272(16) Uani 1 1 d . . . H7A H 0.4931 -0.0357 0.8455 0.033 Uiso 1 1 calc R . . H7B H 0.5358 0.0141 0.7247 0.033 Uiso 1 1 calc R . . C8 C 0.5486(5) -0.0920(3) 0.6781(8) 0.0312(17) Uani 1 1 d . . . H8A H 0.4709 -0.0976 0.6125 0.037 Uiso 1 1 calc R . . H8B H 0.5686 -0.1357 0.7431 0.037 Uiso 1 1 calc R . . C9 C 0.6255(5) -0.0860(3) 0.5645(7) 0.0259(16) Uani 1 1 d . . . H9A H 0.5842 -0.1035 0.4575 0.031 Uiso 1 1 calc R . . H9B H 0.6419 -0.0351 0.5529 0.031 Uiso 1 1 calc R . . C10 C 0.7363(5) -0.1261(3) 0.6156(6) 0.0217(14) Uani 1 1 d . . . H10A H 0.7796 -0.1163 0.5366 0.026 Uiso 1 1 calc R . . H10B H 0.7203 -0.1777 0.6119 0.026 Uiso 1 1 calc R . . C11 C 0.8090(5) -0.1075(3) 0.7838(7) 0.0174(14) Uani 1 1 d . . . H11A H 0.7705 -0.1233 0.8646 0.021 Uiso 1 1 calc R . . H11B H 0.8802 -0.1339 0.8031 0.021 Uiso 1 1 calc R . . C12 C 0.8339(5) -0.0290(3) 0.8058(6) 0.0136(13) Uani 1 1 d . . . C13 C 0.7177(5) 0.1414(3) 0.9415(7) 0.0179(14) Uani 1 1 d . . . C14 C 0.5480(6) 0.1900(3) 0.9380(9) 0.0381(19) Uani 1 1 d . . . H14 H 0.4691 0.1898 0.8992 0.046 Uiso 1 1 calc R . . C15 C 0.5973(7) 0.2429(4) 1.0440(9) 0.0335(17) Uani 1 1 d . . . H15 H 0.5527 0.2771 1.0792 0.040 Uiso 1 1 calc R . . C16 C 0.7120(6) 0.2454(3) 1.0980(8) 0.0287(17) Uani 1 1 d . . . H16 H 0.7482 0.2813 1.1702 0.034 Uiso 1 1 calc R . . C17 C 0.7724(5) 0.1939(3) 1.0435(7) 0.0203(14) Uani 1 1 d . . . H17 H 0.8516 0.1947 1.0761 0.024 Uiso 1 1 calc R . . C18 C 1.0137(5) -0.0956(3) 0.6403(7) 0.0186(15) Uani 1 1 d . . . H18 H 0.9488 -0.1241 0.6265 0.022 Uiso 1 1 calc R . . C19 C 1.1031(5) -0.1204(4) 0.5885(6) 0.0229(13) Uani 1 1 d . . . H19 H 1.0998 -0.1656 0.5386 0.027 Uiso 1 1 calc R . . C20 C 1.1963(5) -0.0789(3) 0.6103(7) 0.0222(15) Uani 1 1 d . . . H20 H 1.2600 -0.0956 0.5797 0.027 Uiso 1 1 calc R . . C21 C 1.1961(5) -0.0127(3) 0.6774(7) 0.0216(15) Uani 1 1 d . . . H21 H 1.2601 0.0165 0.6896 0.026 Uiso 1 1 calc R . . C22 C 1.0553(5) 0.2217(3) 0.8265(8) 0.0284(17) Uani 1 1 d . . . H22A H 1.0516 0.2503 0.7306 0.043 Uiso 1 1 calc R . . H22B H 1.1128 0.2410 0.9167 0.043 Uiso 1 1 calc R . . H22C H 0.9829 0.2230 0.8520 0.043 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 0.01771(12) 0.01379(11) 0.01872(12) 0.00022(14) 0.00373(8) -0.00169(15) N1 0.015(3) 0.020(3) 0.018(3) 0.002(2) 0.004(2) -0.001(2) N2 0.014(3) 0.011(3) 0.019(3) 0.001(2) 0.004(2) 0.002(2) N4 0.022(3) 0.022(3) 0.046(4) -0.006(3) 0.006(3) 0.002(3) C23 0.008(3) 0.003(3) 0.003(3) 0.001(2) 0.001(2) -0.001(2) C1 0.017(3) 0.011(3) 0.011(3) 0.004(2) 0.001(3) 0.001(3) C2 0.015(4) 0.010(3) 0.014(3) -0.002(2) 0.000(3) 0.000(3) N3 0.016(3) 0.016(3) 0.027(3) 0.003(3) 0.006(2) 0.004(3) C4 0.021(4) 0.016(3) 0.014(3) 0.002(3) 0.004(3) 0.001(3) C5 0.018(4) 0.019(3) 0.017(3) 0.000(3) 0.008(3) 0.000(3) C6 0.026(4) 0.019(3) 0.022(4) 0.001(3) 0.010(3) -0.001(3) C7 0.016(4) 0.034(4) 0.034(4) -0.005(3) 0.010(3) 0.000(3) C8 0.019(4) 0.034(4) 0.040(4) -0.012(3) 0.008(3) -0.009(3) C9 0.021(4) 0.028(4) 0.026(4) -0.009(3) 0.003(3) -0.003(3) C10 0.020(3) 0.016(3) 0.026(3) -0.002(3) 0.000(3) -0.005(3) C11 0.020(3) 0.013(4) 0.020(3) 0.003(3) 0.007(3) 0.003(3) C12 0.013(3) 0.018(3) 0.008(3) 0.002(2) -0.001(3) -0.001(3) C13 0.025(4) 0.013(3) 0.018(3) 0.004(2) 0.010(3) 0.003(3) C14 0.023(4) 0.033(4) 0.057(5) -0.004(4) 0.009(4) 0.005(3) C15 0.041(4) 0.021(4) 0.046(4) -0.001(3) 0.025(4) 0.010(3) C16 0.042(5) 0.022(4) 0.024(4) -0.005(3) 0.012(4) -0.001(3) C17 0.019(4) 0.024(4) 0.016(3) 0.001(3) 0.001(3) 0.000(3) C18 0.021(4) 0.015(3) 0.020(4) 0.002(3) 0.006(3) 0.002(3) C19 0.027(4) 0.021(3) 0.020(3) 0.000(3) 0.005(3) 0.010(4) C20 0.019(4) 0.024(4) 0.027(4) 0.003(3) 0.012(3) 0.007(3) C21 0.017(4) 0.021(4) 0.027(4) 0.003(3) 0.007(3) -0.001(3) C22 0.029(4) 0.011(3) 0.048(5) -0.006(3) 0.016(4) -0.008(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 C22 2.037(5) . ? Pt1 N2 2.060(5) . ? Pt1 C23 2.082(5) . ? Pt1 N1 2.105(5) . ? N1 C21 1.333(7) . ? N1 C1 1.365(7) . ? N2 N3 1.332(6) . ? N2 C2 1.354(6) . ? N4 C14 1.335(8) . ? N4 C13 1.349(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C1 C18 1.391(7) . ? C1 C2 1.505(8) . ? C2 C12 1.409(8) . ? N3 C4 1.334(7) . ? C4 C5 1.404(7) . ? C4 C13 1.496(8) . ? C5 C12 1.415(8) . ? C5 C6 1.510(8) . ? C6 C7 1.549(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.520(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.542(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.531(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.539(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.512(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 C17 1.380(8) . ? C14 C15 1.385(9) . ? C14 H14 0.9500 . ? C15 C16 1.380(9) . ? C15 H15 0.9500 . ? C16 C17 1.381(8) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.382(8) . ? C18 H18 0.9500 . ? C19 C20 1.369(8) . ? C19 H19 0.9500 . ? C20 C21 1.375(8) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 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 C22 Pt1 N2 96.9(2) . . ? C22 Pt1 C23 84.9(2) . . ? N2 Pt1 C23 176.34(18) . . ? C22 Pt1 N1 172.0(2) . . ? N2 Pt1 N1 76.58(18) . . ? C23 Pt1 N1 101.95(19) . . ? C21 N1 C1 119.6(5) . . ? C21 N1 Pt1 123.5(4) . . ? C1 N1 Pt1 116.1(4) . . ? N3 N2 C2 121.6(5) . . ? N3 N2 Pt1 117.9(3) . . ? C2 N2 Pt1 120.1(4) . . ? C14 N4 C13 117.1(6) . . ? Pt1 C23 H23A 109.5 . . ? Pt1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Pt1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C1 C18 119.1(5) . . ? N1 C1 C2 114.6(5) . . ? C18 C1 C2 126.2(5) . . ? N2 C2 C12 121.0(5) . . ? N2 C2 C1 111.3(5) . . ? C12 C2 C1 127.7(5) . . ? N2 N3 C4 119.5(5) . . ? N3 C4 C5 123.6(5) . . ? N3 C4 C13 110.5(5) . . ? C5 C4 C13 125.9(5) . . ? C4 C5 C12 116.5(5) . . ? C4 C5 C6 120.0(5) . . ? C12 C5 C6 123.2(5) . . ? C5 C6 C7 116.4(5) . . ? C5 C6 H6A 108.2 . . ? C7 C6 H6A 108.2 . . ? C5 C6 H6B 108.2 . . ? C7 C6 H6B 108.2 . . ? H6A C6 H6B 107.3 . . ? C8 C7 C6 117.8(5) . . ? C8 C7 H7A 107.8 . . ? C6 C7 H7A 107.8 . . ? C8 C7 H7B 107.8 . . ? C6 C7 H7B 107.8 . . ? H7A C7 H7B 107.2 . . ? C7 C8 C9 115.1(5) . . ? C7 C8 H8A 108.5 . . ? C9 C8 H8A 108.5 . . ? C7 C8 H8B 108.5 . . ? C9 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C10 C9 C8 116.0(5) . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? C8 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C11 115.1(5) . . ? C9 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? C9 C10 H10B 108.5 . . ? C11 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C12 C11 C10 113.1(5) . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C2 C12 C5 117.8(5) . . ? C2 C12 C11 124.3(5) . . ? C5 C12 C11 118.0(5) . . ? N4 C13 C17 122.5(5) . . ? N4 C13 C4 118.0(5) . . ? C17 C13 C4 119.5(6) . . ? N4 C14 C15 123.4(7) . . ? N4 C14 H14 118.3 . . ? C15 C14 H14 118.3 . . ? C16 C15 C14 119.2(6) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 117.8(6) . . ? C15 C16 H16 121.1 . . ? C17 C16 H16 121.1 . . ? C13 C17 C16 119.9(6) . . ? C13 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C18 C1 120.6(6) . . ? C19 C18 H18 119.7 . . ? C1 C18 H18 119.7 . . ? C20 C19 C18 119.0(6) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 118.7(6) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? N1 C21 C20 122.9(6) . . ? N1 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? Pt1 C22 H22A 109.5 . . ? Pt1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Pt1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pt1 N1 C21 174.2(5) . . . . ? C23 Pt1 N1 C21 -9.2(5) . . . . ? N2 Pt1 N1 C1 5.3(4) . . . . ? C23 Pt1 N1 C1 -178.2(4) . . . . ? C22 Pt1 N2 N3 -9.5(4) . . . . ? N1 Pt1 N2 N3 175.3(4) . . . . ? C22 Pt1 N2 C2 177.7(4) . . . . ? N1 Pt1 N2 C2 2.4(4) . . . . ? C21 N1 C1 C18 -3.2(8) . . . . ? Pt1 N1 C1 C18 166.2(4) . . . . ? C21 N1 C1 C2 179.3(5) . . . . ? Pt1 N1 C1 C2 -11.3(6) . . . . ? N3 N2 C2 C12 -2.7(8) . . . . ? Pt1 N2 C2 C12 169.9(4) . . . . ? N3 N2 C2 C1 178.8(5) . . . . ? Pt1 N2 C2 C1 -8.7(6) . . . . ? N1 C1 C2 N2 12.8(7) . . . . ? C18 C1 C2 N2 -164.5(5) . . . . ? N1 C1 C2 C12 -165.7(6) . . . . ? C18 C1 C2 C12 17.0(9) . . . . ? C2 N2 N3 C4 2.2(8) . . . . ? Pt1 N2 N3 C4 -170.6(4) . . . . ? N2 N3 C4 C5 -0.1(9) . . . . ? N2 N3 C4 C13 178.4(5) . . . . ? N3 C4 C5 C12 -1.3(9) . . . . ? C13 C4 C5 C12 -179.6(5) . . . . ? N3 C4 C5 C6 172.7(5) . . . . ? C13 C4 C5 C6 -5.6(9) . . . . ? C4 C5 C6 C7 100.4(7) . . . . ? C12 C5 C6 C7 -85.9(7) . . . . ? C5 C6 C7 C8 73.5(7) . . . . ? C6 C7 C8 C9 -66.1(8) . . . . ? C7 C8 C9 C10 99.2(7) . . . . ? C8 C9 C10 C11 -55.5(7) . . . . ? C9 C10 C11 C12 -55.4(7) . . . . ? N2 C2 C12 C5 1.1(8) . . . . ? C1 C2 C12 C5 179.5(5) . . . . ? N2 C2 C12 C11 -178.6(5) . . . . ? C1 C2 C12 C11 -0.3(9) . . . . ? C4 C5 C12 C2 0.7(8) . . . . ? C6 C5 C12 C2 -173.1(5) . . . . ? C4 C5 C12 C11 -179.5(5) . . . . ? C6 C5 C12 C11 6.7(9) . . . . ? C10 C11 C12 C2 -90.1(7) . . . . ? C10 C11 C12 C5 90.1(6) . . . . ? C14 N4 C13 C17 -0.6(9) . . . . ? C14 N4 C13 C4 -177.8(5) . . . . ? N3 C4 C13 N4 138.5(5) . . . . ? C5 C4 C13 N4 -43.0(8) . . . . ? N3 C4 C13 C17 -38.7(7) . . . . ? C5 C4 C13 C17 139.8(6) . . . . ? C13 N4 C14 C15 -1.4(10) . . . . ? N4 C14 C15 C16 2.0(11) . . . . ? C14 C15 C16 C17 -0.4(10) . . . . ? N4 C13 C17 C16 2.1(9) . . . . ? C4 C13 C17 C16 179.2(5) . . . . ? C15 C16 C17 C13 -1.5(9) . . . . ? N1 C1 C18 C19 2.4(8) . . . . ? C2 C1 C18 C19 179.6(5) . . . . ? C1 C18 C19 C20 0.5(9) . . . . ? C18 C19 C20 C21 -2.5(9) . . . . ? C1 N1 C21 C20 1.2(9) . . . . ? Pt1 N1 C21 C20 -167.4(4) . . . . ? C19 C20 C21 N1 1.7(9) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.09 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.923 _refine_diff_density_min -0.986 _refine_diff_density_rms 0.198 #===END data_4b _database_code_depnum_ccdc_archive 'CCDC 869544' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H46 N8 Pt2, 2(C F3 O3 S), C3 H6 O' _chemical_formula_sum 'C47 H52 F6 N8 O7 Pt2 S2' _chemical_formula_weight 1409.26 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' 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/n _symmetry_space_group_name_Hall '-P 2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 10.6068(11) _cell_length_b 8.7983(9) _cell_length_c 26.434(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.805(2) _cell_angle_gamma 90.00 _cell_volume 2466.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4999 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 26.46 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 5.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6960 _exptl_absorpt_correction_T_max 0.9176 _exptl_absorpt_process_details 'SADABS (Bruker, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26302 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.46 _reflns_number_total 4999 _reflns_number_gt 3723 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The disordered triflate anion was refined isotropically. When made anisotropic, thetriflate group atoms would become non-positive definites. It was decided that the model for the disorder was adequate and the anion was best left isotropic. The methyl group bonded to the platinum atom was also refined isotropically. When refined anisotropically the carbon atom, C21 would become a non-positive definite. There are no similar carbon atoms to model this atom against and therefore EADP could not be used as in the case of N4 and C1. ; _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^)+(0.0000P)^2^+49.3811P] 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 4999 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1257 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 1.251 _refine_ls_restrained_S_all 1.251 _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 0.11452(4) 0.62621(6) 0.309126(15) 0.01928(12) Uani 1 1 d . . . N1 N 0.0742(8) 0.3972(10) 0.3247(3) 0.0200(14) Uani 1 1 d . . . N2 N 0.0703(8) 0.5470(11) 0.2400(3) 0.020(2) Uani 1 1 d . . . N4 N 0.1973(8) 0.6975(10) 0.3745(3) 0.0200(14) Uani 1 1 d . . . C1 C 0.0560(10) 0.3346(12) 0.3711(4) 0.021(3) Uani 1 1 d . . . H1A H 0.0959 0.3807 0.3996 0.025 Uiso 1 1 calc R . . C2 C -0.0173(11) 0.2079(15) 0.3788(4) 0.029(3) Uani 1 1 d . . . H2B H -0.0272 0.1678 0.4119 0.035 Uiso 1 1 calc R . . C3 C -0.0751(10) 0.1413(15) 0.3384(4) 0.028(3) Uani 1 1 d . . . H3A H -0.1288 0.0561 0.3431 0.033 Uiso 1 1 calc R . . C4 C -0.0554(10) 0.1988(14) 0.2898(4) 0.025(3) Uani 1 1 d . . . H4A H -0.0954 0.1529 0.2613 0.030 Uiso 1 1 calc R . . C5 C 0.0223(9) 0.3223(12) 0.2836(4) 0.018(2) Uani 1 1 d . . . C6 C 0.0504(9) 0.3998(12) 0.2348(4) 0.018(2) Uani 1 1 d . . . C7 C 0.0674(10) 0.3234(13) 0.1881(4) 0.021(2) Uani 1 1 d . . . C8 C 0.4010(10) 0.4151(12) 0.3531(4) 0.019(2) Uani 1 1 d . . . C9 C 0.3812(10) 0.5680(13) 0.3437(4) 0.021(2) Uani 1 1 d . . . C10 C 0.3222(10) 0.6731(12) 0.3816(4) 0.021(2) Uani 1 1 d . . . C11 C 0.3891(11) 0.7406(14) 0.4203(4) 0.027(3) Uani 1 1 d . . . H11A H 0.4771 0.7227 0.4241 0.033 Uiso 1 1 calc R . . C12 C 0.3268(11) 0.8359(13) 0.4541(4) 0.028(3) Uani 1 1 d . . . H12A H 0.3715 0.8857 0.4807 0.033 Uiso 1 1 calc R . . C13 C 0.1994(12) 0.8555(16) 0.4477(4) 0.034(3) Uani 1 1 d . . . H13A H 0.1540 0.9152 0.4712 0.041 Uiso 1 1 calc R . . C14 C 0.1371(11) 0.7891(14) 0.4076(4) 0.024(3) Uani 1 1 d . . . H14A H 0.0495 0.8079 0.4029 0.029 Uiso 1 1 calc R . . C16 C 0.5540(13) 0.0769(14) 0.3376(5) 0.035(2) Uani 1 1 d . . . H16A H 0.6265 0.1123 0.3175 0.043 Uiso 1 1 calc R . . H16B H 0.5466 -0.0342 0.3323 0.043 Uiso 1 1 calc R . . C17 C 0.5851(14) 0.1050(19) 0.3939(5) 0.052(5) Uani 1 1 d . . . H17A H 0.5117 0.0718 0.4138 0.063 Uiso 1 1 calc R . . H17B H 0.6568 0.0385 0.4036 0.063 Uiso 1 1 calc R . . C18 C 0.6175(12) 0.2635(19) 0.4096(5) 0.045(4) Uani 1 1 d . . . H18A H 0.6446 0.3204 0.3793 0.054 Uiso 1 1 calc R . . H18B H 0.6903 0.2593 0.4334 0.054 Uiso 1 1 calc R . . C19 C 0.5103(12) 0.3531(18) 0.4350(4) 0.039(3) Uani 1 1 d . . . H19A H 0.4968 0.3107 0.4691 0.047 Uiso 1 1 calc R . . H19B H 0.5373 0.4602 0.4391 0.047 Uiso 1 1 calc R . . C20 C 0.3840(10) 0.3500(15) 0.4054(4) 0.026(3) Uani 1 1 d . . . H20A H 0.3532 0.2440 0.4027 0.031 Uiso 1 1 calc R . . H20B H 0.3203 0.4102 0.4237 0.031 Uiso 1 1 calc R . . C25 C -0.2524(14) -0.303(2) 0.2016(7) 0.068(5) Uani 1 1 d . . . H25A H -0.2519 -0.4125 0.2086 0.102 Uiso 1 1 calc R . . H25B H -0.1780 -0.2765 0.1819 0.102 Uiso 1 1 calc R . . H25C H -0.3288 -0.2768 0.1823 0.102 Uiso 1 1 calc R . . C24 C -0.2500 -0.218(3) 0.2500 0.051(6) Uani 1 2 d S . . O7 O -0.2500 -0.0786(16) 0.2500 0.052(4) Uani 1 2 d S . . N3 N 0.3977(8) 0.6378(12) 0.2989(3) 0.0202(19) Uani 1 1 d . . . C15 C 0.4340(13) 0.1524(14) 0.3161(5) 0.035(2) Uani 1 1 d . . . H15A H 0.4179 0.1101 0.2819 0.043 Uiso 1 1 calc R . . H15B H 0.3626 0.1217 0.3375 0.043 Uiso 1 1 calc R . . C21 C 0.1129(11) 0.8487(14) 0.2899(4) 0.032(3) Uiso 1 1 d . . . H21A H 0.1972 0.8918 0.2953 0.048 Uiso 1 1 calc R . . H21B H 0.0521 0.9030 0.3108 0.048 Uiso 1 1 calc R . . H21C H 0.0886 0.8590 0.2541 0.048 Uiso 1 1 calc R . . S1 S 0.8004(6) 0.7936(7) 0.4715(3) 0.0219(18) Uiso 0.489(13) 1 d P A 1 C22 C 0.815(3) 0.590(4) 0.4544(13) 0.051(9) Uiso 0.489(13) 1 d P A 1 O1 O 0.869(2) 0.793(3) 0.5176(9) 0.070(8) Uiso 0.489(13) 1 d P A 1 O2 O 0.8470(18) 0.873(3) 0.4242(8) 0.028(5) Uiso 0.489(13) 1 d P A 1 O3 O 0.663(2) 0.809(3) 0.4768(9) 0.049(6) Uiso 0.489(13) 1 d P A 1 F1 F 0.730(3) 0.584(3) 0.4111(10) 0.114(10) Uiso 0.489(13) 1 d P A 1 F2 F 0.804(2) 0.517(2) 0.4986(7) 0.046(6) Uiso 0.489(13) 1 d P A 1 F3 F 0.9414(18) 0.564(2) 0.4488(7) 0.048(5) Uiso 0.489(13) 1 d P A 1 S2 S 0.7653(7) 0.7869(8) 0.4502(3) 0.033(2) Uiso 0.511(13) 1 d P A 2 C23 C 0.862(2) 0.633(3) 0.4731(9) 0.026(5) Uiso 0.511(13) 1 d P A 2 O4 O 0.686(2) 0.712(3) 0.4114(8) 0.063(7) Uiso 0.511(13) 1 d P A 2 O5 O 0.8598(18) 0.901(2) 0.4376(7) 0.028(5) Uiso 0.511(13) 1 d P A 2 O6 O 0.6985(18) 0.838(2) 0.4938(7) 0.039(5) Uiso 0.511(13) 1 d P A 2 F4 F 0.9447(18) 0.682(2) 0.5063(7) 0.072(6) Uiso 0.511(13) 1 d P A 2 F5 F 0.7651(16) 0.5110(19) 0.4872(6) 0.030(4) Uiso 0.511(13) 1 d P A 2 F6 F 0.9017(15) 0.5519(18) 0.4288(6) 0.034(4) Uiso 0.511(13) 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 0.01881(19) 0.0204(2) 0.01875(19) -0.0020(2) 0.00417(13) -0.0002(2) N1 0.022(3) 0.013(4) 0.024(3) -0.001(3) 0.005(3) 0.005(3) N2 0.016(5) 0.021(5) 0.023(5) 0.005(4) 0.003(4) 0.004(4) N4 0.022(3) 0.013(4) 0.024(3) -0.001(3) 0.005(3) 0.005(3) C1 0.022(5) 0.019(7) 0.022(5) -0.001(5) 0.005(4) 0.000(4) C2 0.033(7) 0.028(7) 0.026(6) 0.005(6) 0.011(5) 0.001(6) C3 0.032(6) 0.022(7) 0.029(6) 0.000(6) 0.009(5) -0.006(6) C4 0.027(6) 0.029(7) 0.020(6) -0.007(5) 0.004(5) -0.005(5) C5 0.017(5) 0.017(6) 0.020(5) -0.005(4) 0.001(4) 0.000(4) C6 0.018(5) 0.008(6) 0.028(5) 0.001(5) 0.006(4) 0.000(4) C7 0.018(5) 0.026(7) 0.019(5) 0.001(5) 0.000(4) -0.005(5) C8 0.018(5) 0.015(6) 0.024(5) 0.001(4) 0.004(4) 0.002(4) C9 0.016(5) 0.026(6) 0.021(5) 0.000(5) 0.002(4) 0.006(5) C10 0.025(6) 0.015(6) 0.022(5) 0.001(4) 0.006(4) 0.000(4) C11 0.031(6) 0.030(7) 0.021(6) -0.001(5) 0.003(5) -0.004(5) C12 0.041(7) 0.019(7) 0.023(6) -0.008(5) 0.001(5) -0.004(5) C13 0.041(7) 0.032(8) 0.029(6) -0.005(6) 0.012(5) 0.006(6) C14 0.031(6) 0.024(7) 0.019(5) -0.004(5) 0.007(5) 0.000(5) C16 0.054(6) 0.020(5) 0.033(5) 0.004(4) 0.011(4) 0.013(4) C17 0.061(9) 0.061(12) 0.035(7) 0.026(8) 0.010(6) 0.041(9) C18 0.034(7) 0.074(12) 0.026(7) 0.010(7) 0.003(6) 0.020(8) C19 0.046(8) 0.048(10) 0.024(6) 0.013(7) -0.006(5) 0.006(7) C20 0.030(6) 0.027(8) 0.020(5) 0.003(5) 0.005(4) 0.008(5) C25 0.038(9) 0.068(12) 0.098(14) -0.028(11) 0.002(9) 0.000(9) C24 0.011(9) 0.056(16) 0.085(18) 0.000 0.000(10) 0.000 O7 0.062(10) 0.030(9) 0.064(10) 0.000 0.021(8) 0.000 N3 0.024(4) 0.015(5) 0.022(4) 0.004(5) 0.003(3) 0.002(4) C15 0.054(6) 0.020(5) 0.033(5) 0.004(4) 0.011(4) 0.013(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 N2 2.005(9) . ? Pt1 C21 2.023(13) . ? Pt1 N4 2.028(9) . ? Pt1 N1 2.102(9) . ? N1 C1 1.362(13) . ? N1 C5 1.378(13) . ? N2 C6 1.319(14) . ? N2 N3 1.349(12) 2 ? N4 C10 1.352(14) . ? N4 C14 1.356(13) . ? C1 C2 1.376(16) . ? C1 H1A 0.9500 . ? C2 C3 1.358(16) . ? C2 H2B 0.9500 . ? C3 C4 1.400(15) . ? C3 H3A 0.9500 . ? C4 C5 1.374(15) . ? C4 H4A 0.9500 . ? C5 C6 1.494(14) . ? C6 C7 1.419(15) . ? C7 C8 1.399(15) 2 ? C7 C15 1.508(16) 2 ? C8 C9 1.383(15) . ? C8 C7 1.399(15) 2 ? C8 C20 1.509(14) . ? C9 N3 1.347(13) . ? C9 C10 1.507(15) . ? C10 C11 1.373(16) . ? C11 C12 1.398(15) . ? C11 H11A 0.9500 . ? C12 C13 1.371(17) . ? C12 H12A 0.9500 . ? C13 C14 1.372(16) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C16 C15 1.538(17) . ? C16 C17 1.541(18) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.49(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.544(17) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.542(16) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C25 C24 1.483(19) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C24 O7 1.23(3) . ? C24 C25 1.483(19) 2_455 ? N3 N2 1.349(12) 2 ? C15 C7 1.509(16) 2 ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? S1 O1 1.41(3) . ? S1 O3 1.48(2) . ? S1 O2 1.52(2) . ? S1 C22 1.85(4) . ? C22 F2 1.34(4) . ? C22 F3 1.37(4) . ? C22 F1 1.45(4) . ? S2 O6 1.44(2) . ? S2 O5 1.46(2) . ? S2 O4 1.47(2) . ? S2 C23 1.80(3) . ? C23 F4 1.31(3) . ? C23 F6 1.44(3) . ? C23 F5 1.53(3) . ? 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 N2 Pt1 C21 96.1(4) . . ? N2 Pt1 N4 167.8(3) . . ? C21 Pt1 N4 85.3(4) . . ? N2 Pt1 N1 78.4(4) . . ? C21 Pt1 N1 167.4(4) . . ? N4 Pt1 N1 102.5(4) . . ? C1 N1 C5 117.2(9) . . ? C1 N1 Pt1 126.6(7) . . ? C5 N1 Pt1 112.6(7) . . ? C6 N2 N3 122.9(9) . 2 ? C6 N2 Pt1 118.1(7) . . ? N3 N2 Pt1 115.5(7) 2 . ? C10 N4 C14 118.4(10) . . ? C10 N4 Pt1 118.7(7) . . ? C14 N4 Pt1 122.1(8) . . ? N1 C1 C2 123.3(11) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C3 C2 C1 118.9(11) . . ? C3 C2 H2B 120.6 . . ? C1 C2 H2B 120.6 . . ? C2 C3 C4 119.6(11) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 119.5(11) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 N1 121.2(10) . . ? C4 C5 C6 126.2(10) . . ? N1 C5 C6 112.3(9) . . ? N2 C6 C7 122.3(10) . . ? N2 C6 C5 113.0(9) . . ? C7 C6 C5 124.4(10) . . ? C8 C7 C6 116.0(10) 2 . ? C8 C7 C15 121.4(10) 2 2 ? C6 C7 C15 122.3(10) . 2 ? C9 C8 C7 117.2(10) . 2 ? C9 C8 C20 121.0(10) . . ? C7 C8 C20 121.8(10) 2 . ? N3 C9 C8 125.5(10) . . ? N3 C9 C10 111.3(10) . . ? C8 C9 C10 122.7(10) . . ? N4 C10 C11 122.0(10) . . ? N4 C10 C9 114.9(9) . . ? C11 C10 C9 123.1(10) . . ? C10 C11 C12 119.5(11) . . ? C10 C11 H11A 120.3 . . ? C12 C11 H11A 120.3 . . ? C13 C12 C11 118.1(11) . . ? C13 C12 H12A 121.0 . . ? C11 C12 H12A 121.0 . . ? C12 C13 C14 120.3(11) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? N4 C14 C13 121.7(11) . . ? N4 C14 H14A 119.2 . . ? C13 C14 H14A 119.2 . . ? C15 C16 C17 116.9(10) . . ? C15 C16 H16A 108.1 . . ? C17 C16 H16A 108.1 . . ? C15 C16 H16B 108.1 . . ? C17 C16 H16B 108.1 . . ? H16A C16 H16B 107.3 . . ? C18 C17 C16 117.6(11) . . ? C18 C17 H17A 107.9 . . ? C16 C17 H17A 107.9 . . ? C18 C17 H17B 107.9 . . ? C16 C17 H17B 107.9 . . ? H17A C17 H17B 107.2 . . ? C17 C18 C19 115.4(12) . . ? C17 C18 H18A 108.4 . . ? C19 C18 H18A 108.4 . . ? C17 C18 H18B 108.4 . . ? C19 C18 H18B 108.4 . . ? H18A C18 H18B 107.5 . . ? C20 C19 C18 114.3(11) . . ? C20 C19 H19A 108.7 . . ? C18 C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? C18 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C8 C20 C19 110.1(9) . . ? C8 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? C8 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O7 C24 C25 120.4(12) . 2_455 ? O7 C24 C25 120.4(12) . . ? C25 C24 C25 119(2) 2_455 . ? C9 N3 N2 115.9(10) . 2 ? C7 C15 C16 117.8(11) 2 . ? C7 C15 H15A 107.9 2 . ? C16 C15 H15A 107.9 . . ? C7 C15 H15B 107.9 2 . ? C16 C15 H15B 107.9 . . ? H15A C15 H15B 107.2 . . ? Pt1 C21 H21A 109.5 . . ? Pt1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Pt1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 S1 O3 114.8(14) . . ? O1 S1 O2 122.8(14) . . ? O3 S1 O2 111.6(13) . . ? O1 S1 C22 99.6(17) . . ? O3 S1 C22 101.4(15) . . ? O2 S1 C22 102.3(14) . . ? F2 C22 F3 96(3) . . ? F2 C22 F1 127(3) . . ? F3 C22 F1 120(3) . . ? F2 C22 S1 104(2) . . ? F3 C22 S1 106(2) . . ? F1 C22 S1 100(2) . . ? O6 S2 O5 108.3(13) . . ? O6 S2 O4 114.8(13) . . ? O5 S2 O4 122.4(13) . . ? O6 S2 C23 104.6(12) . . ? O5 S2 C23 101.9(12) . . ? O4 S2 C23 102.2(14) . . ? F4 C23 F6 120(2) . . ? F4 C23 F5 121(2) . . ? F6 C23 F5 93.3(19) . . ? F4 C23 S2 111(2) . . ? F6 C23 S2 105.7(16) . . ? F5 C23 S2 103.3(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pt1 N1 C1 -166.9(9) . . . . ? C21 Pt1 N1 C1 -102(2) . . . . ? N4 Pt1 N1 C1 25.5(9) . . . . ? N2 Pt1 N1 C5 -9.2(7) . . . . ? C21 Pt1 N1 C5 56(2) . . . . ? N4 Pt1 N1 C5 -176.8(7) . . . . ? C21 Pt1 N2 C6 -174.7(8) . . . . ? N4 Pt1 N2 C6 89.7(19) . . . . ? N1 Pt1 N2 C6 -6.1(7) . . . . ? C21 Pt1 N2 N3 25.6(8) . . . 2 ? N4 Pt1 N2 N3 -70(2) . . . 2 ? N1 Pt1 N2 N3 -165.8(7) . . . 2 ? N2 Pt1 N4 C10 -9(2) . . . . ? C21 Pt1 N4 C10 -105.4(9) . . . . ? N1 Pt1 N4 C10 84.6(8) . . . . ? N2 Pt1 N4 C14 160.7(15) . . . . ? C21 Pt1 N4 C14 63.9(9) . . . . ? N1 Pt1 N4 C14 -106.1(9) . . . . ? C5 N1 C1 C2 -4.3(15) . . . . ? Pt1 N1 C1 C2 152.6(9) . . . . ? N1 C1 C2 C3 -0.2(17) . . . . ? C1 C2 C3 C4 2.4(18) . . . . ? C2 C3 C4 C5 -0.1(18) . . . . ? C3 C4 C5 N1 -4.6(17) . . . . ? C3 C4 C5 C6 -178.2(10) . . . . ? C1 N1 C5 C4 6.6(15) . . . . ? Pt1 N1 C5 C4 -153.4(9) . . . . ? C1 N1 C5 C6 -178.9(9) . . . . ? Pt1 N1 C5 C6 21.1(10) . . . . ? N3 N2 C6 C7 3.4(16) 2 . . . ? Pt1 N2 C6 C7 -154.7(8) . . . . ? N3 N2 C6 C5 177.2(8) 2 . . . ? Pt1 N2 C6 C5 19.1(11) . . . . ? C4 C5 C6 N2 147.7(11) . . . . ? N1 C5 C6 N2 -26.4(13) . . . . ? C4 C5 C6 C7 -38.6(16) . . . . ? N1 C5 C6 C7 147.3(10) . . . . ? N2 C6 C7 C8 -4.0(15) . . . 2 ? C5 C6 C7 C8 -177.1(10) . . . 2 ? N2 C6 C7 C15 169.6(11) . . . 2 ? C5 C6 C7 C15 -3.6(17) . . . 2 ? C7 C8 C9 N3 -4.6(17) 2 . . . ? C20 C8 C9 N3 177.8(10) . . . . ? C7 C8 C9 C10 167.5(10) 2 . . . ? C20 C8 C9 C10 -10.1(17) . . . . ? C14 N4 C10 C11 -1.4(16) . . . . ? Pt1 N4 C10 C11 168.4(9) . . . . ? C14 N4 C10 C9 179.0(10) . . . . ? Pt1 N4 C10 C9 -11.3(12) . . . . ? N3 C9 C10 N4 75.8(12) . . . . ? C8 C9 C10 N4 -97.3(13) . . . . ? N3 C9 C10 C11 -103.8(12) . . . . ? C8 C9 C10 C11 83.1(15) . . . . ? N4 C10 C11 C12 0.9(17) . . . . ? C9 C10 C11 C12 -179.5(10) . . . . ? C10 C11 C12 C13 1.4(17) . . . . ? C11 C12 C13 C14 -3.3(19) . . . . ? C10 N4 C14 C13 -0.6(17) . . . . ? Pt1 N4 C14 C13 -169.9(9) . . . . ? C12 C13 C14 N4 3.0(19) . . . . ? C15 C16 C17 C18 -65.7(17) . . . . ? C16 C17 C18 C19 101.0(14) . . . . ? C17 C18 C19 C20 -50.1(16) . . . . ? C9 C8 C20 C19 -91.9(13) . . . . ? C7 C8 C20 C19 90.6(13) 2 . . . ? C18 C19 C20 C8 -58.9(15) . . . . ? C8 C9 N3 N2 3.7(16) . . . 2 ? C10 C9 N3 N2 -169.1(8) . . . 2 ? C17 C16 C15 C7 67.8(16) . . . 2 ? O1 S1 C22 F2 39(3) . . . . ? O3 S1 C22 F2 -79(3) . . . . ? O2 S1 C22 F2 166(2) . . . . ? O1 S1 C22 F3 -62(2) . . . . ? O3 S1 C22 F3 -180(2) . . . . ? O2 S1 C22 F3 65(2) . . . . ? O1 S1 C22 F1 172(2) . . . . ? O3 S1 C22 F1 54(2) . . . . ? O2 S1 C22 F1 -61(2) . . . . ? O6 S2 C23 F4 -64.1(19) . . . . ? O5 S2 C23 F4 49(2) . . . . ? O4 S2 C23 F4 175.9(17) . . . . ? O6 S2 C23 F6 164.1(16) . . . . ? O5 S2 C23 F6 -83.2(19) . . . . ? O4 S2 C23 F6 44.1(19) . . . . ? O6 S2 C23 F5 66.8(19) . . . . ? O5 S2 C23 F5 179.5(14) . . . . ? O4 S2 C23 F5 -53.3(17) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.626 _refine_diff_density_min -3.841 _refine_diff_density_rms 0.217 #===END data_4a _database_code_depnum_ccdc_archive 'CCDC 869545' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H46 N8 Pt2, 2(C3 H6 O), 2(C F3 O3 S), O' _chemical_formula_sum 'C50 H58 F6 N8 O9 Pt2 S2' _chemical_formula_weight 1483.34 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.493(3) _cell_length_b 14.767(3) _cell_length_c 15.879(3) _cell_angle_alpha 77.96(3) _cell_angle_beta 76.62(3) _cell_angle_gamma 76.14(3) _cell_volume 2730.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12484 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 27.60 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 5.276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5171 _exptl_absorpt_correction_T_max 0.7025 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22922 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 27.60 _reflns_number_total 12484 _reflns_number_gt 8998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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. H2 of H2O not found due to poor diffraction data surrounding the O atom ; _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^)+(0.1002P)^2^+3.4963P] 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 12484 _refine_ls_number_parameters 598 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1763 _refine_ls_wR_factor_gt 0.1352 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _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 0.37032(2) 0.57187(2) -0.67104(2) 0.02302(11) Uani 1 1 d . . . C1 C 0.6345(8) 1.0022(7) -0.9149(7) 0.036(2) Uani 1 1 d . . . H1A H 0.7140 0.9941 -0.9302 0.043 Uiso 1 1 calc R . . C2 C 0.5730(9) 1.0923(7) -0.9064(6) 0.039(2) Uani 1 1 d . . . H2A H 0.6087 1.1445 -0.9159 0.046 Uiso 1 1 calc R . . C3 C 0.4565(8) 1.1032(7) -0.8834(6) 0.035(2) Uani 1 1 d . . . H3A H 0.4109 1.1637 -0.8763 0.043 Uiso 1 1 calc R . . C4 C 0.4075(8) 1.0250(6) -0.8708(6) 0.033(2) Uani 1 1 d . . . H4A H 0.3281 1.0322 -0.8571 0.040 Uiso 1 1 calc R . . C5 C 0.4744(7) 0.9372(6) -0.8782(5) 0.0236(18) Uani 1 1 d . . . C6 C 0.4316(6) 0.8485(6) -0.8680(5) 0.0227(17) Uani 1 1 d . . . C7 C 0.3202(6) 0.8345(6) -0.8333(5) 0.0209(17) Uani 1 1 d . . . C8 C 0.3001(7) 0.7467(6) -0.8371(5) 0.0253(18) Uani 1 1 d . . . C9 C 0.3904(6) 0.6766(6) -0.8668(5) 0.0218(17) Uani 1 1 d . . . C10 C 0.3821(6) 0.5768(6) -0.8632(5) 0.0228(17) Uani 1 1 d . . . C11 C 0.3825(7) 0.5409(6) -0.9360(6) 0.0269(19) Uani 1 1 d . . . H11A H 0.3834 0.5808 -0.9913 0.032 Uiso 1 1 calc R . . C12 C 0.3815(7) 0.4460(7) -0.9287(6) 0.034(2) Uani 1 1 d . . . H12A H 0.3827 0.4196 -0.9787 0.041 Uiso 1 1 calc R . . C13 C 0.3787(8) 0.3907(7) -0.8471(7) 0.036(2) Uani 1 1 d . . . H13A H 0.3799 0.3251 -0.8407 0.043 Uiso 1 1 calc R . . C14 C 0.3742(7) 0.4298(7) -0.7763(7) 0.033(2) Uani 1 1 d . . . H14A H 0.3705 0.3908 -0.7204 0.039 Uiso 1 1 calc R . . C15 C 0.2280(7) 0.9050(6) -0.7868(6) 0.0282(19) Uani 1 1 d . . . H15A H 0.2636 0.9438 -0.7619 0.034 Uiso 1 1 calc R . . H15B H 0.1826 0.8695 -0.7372 0.034 Uiso 1 1 calc R . . C16 C 0.1477(8) 0.9726(7) -0.8449(7) 0.036(2) Uani 1 1 d . . . H16A H 0.1035 1.0236 -0.8117 0.043 Uiso 1 1 calc R . . H16B H 0.1945 1.0025 -0.8975 0.043 Uiso 1 1 calc R . . C17 C 0.0653(8) 0.9316(7) -0.8759(7) 0.036(2) Uani 1 1 d . . . H17A H 0.0151 0.9844 -0.9061 0.043 Uiso 1 1 calc R . . H17B H 0.0181 0.9014 -0.8237 0.043 Uiso 1 1 calc R . . C18 C 0.1189(8) 0.8582(7) -0.9385(6) 0.032(2) Uani 1 1 d . . . H18A H 0.0744 0.8709 -0.9853 0.038 Uiso 1 1 calc R . . H18B H 0.1954 0.8683 -0.9668 0.038 Uiso 1 1 calc R . . C19 C 0.1273(7) 0.7564(6) -0.8975(6) 0.0279(19) Uani 1 1 d . . . H19A H 0.1706 0.7170 -0.9423 0.033 Uiso 1 1 calc R . . H19B H 0.0507 0.7427 -0.8808 0.033 Uiso 1 1 calc R . . C20 C 0.18297(3) 0.72564(2) -0.81541(2) 0.0237(18) Uani 1 1 d . . . H20A H 0.1366 0.7598 -0.7677 0.028 Uiso 1 1 calc R . . H20B H 0.1871 0.6571 -0.7946 0.028 Uiso 1 1 calc R . . N1 N 0.58946(3) 0.92592(2) -0.90288(2) 0.0289(16) Uani 1 1 d R . . N2 N 0.51157(3) 0.77818(2) -0.89871(2) 0.0227(15) Uani 1 1 d R . . N3 N 0.49347(3) 0.69230(2) -0.89999(2) 0.0228(15) Uani 1 1 d R . . N4 N 0.37484(3) 0.52141(2) -0.78223(2) 0.0238(15) Uani 1 1 d R . . Pt2 Pt 0.67772(3) 0.79870(2) -0.92571(2) 0.02533(11) Uani 1 1 d R . . C22 C 0.29421(3) 0.62633(2) -0.49246(2) 0.033(2) Uani 1 1 d R . . H22A H 0.2224 0.6198 -0.4979 0.040 Uiso 1 1 calc R . . C23 C 0.3062(8) 0.6432(7) -0.4157(6) 0.039(2) Uani 1 1 d . . . H23A H 0.2440 0.6495 -0.3684 0.047 Uiso 1 1 calc R . . C24 C 0.4116(8) 0.6514(7) -0.4068(6) 0.037(2) Uani 1 1 d . . . H24A H 0.4239 0.6603 -0.3525 0.045 Uiso 1 1 calc R . . C25 C 0.4967(7) 0.6461(6) -0.4781(6) 0.029(2) Uani 1 1 d . . . H25A H 0.5690 0.6514 -0.4727 0.035 Uiso 1 1 calc R . . C26 C 0.4813(7) 0.6334(6) -0.5577(5) 0.0267(19) Uani 1 1 d . . . C27 C 0.5672(6) 0.6271(6) -0.6386(5) 0.0212(17) Uani 1 1 d . . . C28 C 0.6702(6) 0.6591(6) -0.6601(5) 0.0234(18) Uani 1 1 d . . . C29 C 0.7379(7) 0.6429(6) -0.7402(6) 0.0255(18) Uani 1 1 d . . . C30 C 0.6954(7) 0.6025(6) -0.7966(5) 0.0248(18) Uani 1 1 d . . . C31 C 0.7579(7) 0.5894(6) -0.8879(6) 0.0265(19) Uani 1 1 d . . . C32 C 0.8086(7) 0.5014(7) -0.9088(6) 0.032(2) Uani 1 1 d . . . H32A H 0.8053 0.4473 -0.8645 0.038 Uiso 1 1 calc R . . C33 C 0.8642(8) 0.4901(8) -0.9929(7) 0.037(2) Uani 1 1 d . . . H33A H 0.8976 0.4291 -1.0075 0.045 Uiso 1 1 calc R . . C34 C 0.8695(7) 0.5690(8) -1.0542(7) 0.039(2) Uani 1 1 d . . . H34A H 0.9096 0.5636 -1.1122 0.047 Uiso 1 1 calc R . . C35 C 0.8169(7) 0.6574(7) -1.0326(6) 0.031(2) Uani 1 1 d . . . H35A H 0.8212 0.7118 -1.0764 0.037 Uiso 1 1 calc R . . C36 C 0.7024(7) 0.7142(6) -0.6043(6) 0.0256(18) Uani 1 1 d . . . H36A H 0.6326 0.7482 -0.5709 0.031 Uiso 1 1 calc R . . H36B H 0.7418 0.7625 -0.6436 0.031 Uiso 1 1 calc R . . C37 C 0.7769(7) 0.6578(7) -0.5394(6) 0.031(2) Uani 1 1 d . . . H37A H 0.7404 0.6060 -0.5038 0.038 Uiso 1 1 calc R . . H37B H 0.7788 0.6999 -0.4990 0.038 Uiso 1 1 calc R . . C38 C 0.8987(7) 0.6143(7) -0.5774(6) 0.030(2) Uani 1 1 d . . . H38A H 0.9353 0.6658 -0.6138 0.036 Uiso 1 1 calc R . . H38B H 0.9390 0.5871 -0.5282 0.036 Uiso 1 1 calc R . . C39 C 0.9136(7) 0.5381(6) -0.6328(6) 0.030(2) Uani 1 1 d . . . H39A H 0.8446 0.5117 -0.6169 0.035 Uiso 1 1 calc R . . H39B H 0.9761 0.4865 -0.6170 0.035 Uiso 1 1 calc R . . C40 C 0.9379(7) 0.5696(7) -0.7331(6) 0.030(2) Uani 1 1 d . . . H40A H 1.0153 0.5814 -0.7513 0.036 Uiso 1 1 calc R . . H40B H 0.9341 0.5174 -0.7620 0.036 Uiso 1 1 calc R . . C41 C 0.85663(12) 0.65855(10) -0.76543(9) 0.0260(19) Uani 1 1 d . . . H41A H 0.8624 0.7121 -0.7394 0.031 Uiso 1 1 calc R . . H41B H 0.8771 0.6748 -0.8300 0.031 Uiso 1 1 calc R . . N5 N 0.37876(12) 0.61824(10) -0.56214(9) 0.0278(16) Uani 1 1 d R . . N6 N 0.53686(12) 0.58886(10) -0.69764(9) 0.0222(15) Uani 1 1 d R . . N7 N 0.59901(12) 0.57385(10) -0.77548(9) 0.0249(15) Uani 1 1 d R . . N8 N 0.75926(12) 0.66783(10) -0.95022(9) 0.0262(16) Uani 1 1 d R . . S1 S 0.31291(12) 0.74059(10) -0.18314(9) 0.0403(6) Uani 1 1 d R . . O1 O 0.29168(12) 0.66330(10) -0.21454(9) 0.080(3) Uani 1 1 d R . . O2 O 0.31002(12) 0.72685(10) -0.09022(9) 0.051(2) Uani 1 1 d R . . O3 O 0.40272(12) 0.78381(10) -0.23675(9) 0.052(2) Uani 1 1 d R . . C43 C 0.18670(12) 0.83221(10) -0.19634(9) 0.073(4) Uani 1 1 d R . . F1 F 0.17880(12) 0.85225(10) -0.28083(9) 0.134(4) Uani 1 1 d R . . F2 F 0.09594(12) 0.80399(10) -0.14662(9) 0.127(4) Uani 1 1 d R . . F3 F 0.19436(12) 0.91142(10) -0.17270(9) 0.099(3) Uani 1 1 d R . . S2 S 0.83352(12) 0.83143(10) -1.30091(9) 0.0456(7) Uani 1 1 d R . . O4 O 0.75680(12) 0.84634(10) -1.35702(9) 0.111(4) Uani 1 1 d R . . O5 O 0.79586(12) 0.81758(10) -1.20893(9) 0.087(4) Uani 1 1 d R . . O6 O 0.90780(12) 0.89768(10) -1.33092(9) 0.066(3) Uani 1 1 d R . . C44 C 0.92219(12) 0.71847(10) -1.31934(9) 0.058(3) Uani 1 1 d R . . F4 F 0.86665(12) 0.64900(10) -1.29400(9) 0.097(3) Uani 1 1 d R . . F5 F 1.00247(12) 0.69320(10) -1.27503(9) 0.105(3) Uani 1 1 d R . . F6 F 0.96710(12) 0.71798(10) -1.40386(9) 0.101(3) Uani 1 1 d R . . O8 O 0.97979(12) 0.82407(10) -0.65344(9) 0.102(4) Uani 1 1 d R . . C48 C 1.06063(12) 0.88306(10) -0.55990(9) 0.092(6) Uani 1 1 d R . . H48A H 1.1278 0.8369 -0.5797 0.138 Uiso 1 1 calc R . . H48B H 1.0381 0.8687 -0.4960 0.138 Uiso 1 1 calc R . . H48C H 1.0771 0.9467 -0.5764 0.138 Uiso 1 1 calc R . . C49 C 0.9679(16) 0.8782(10) -0.6018(9) 0.088(6) Uani 1 1 d . . . C50 C 0.8558(16) 0.9426(12) -0.5790(12) 0.121(8) Uani 1 1 d . . . H50A H 0.7981 0.9207 -0.5975 0.182 Uiso 1 1 calc R . . H50B H 0.8597 1.0071 -0.6093 0.182 Uiso 1 1 calc R . . H50C H 0.8367 0.9421 -0.5155 0.182 Uiso 1 1 calc R . . O9 O 0.5775(7) 0.7816(7) -0.3887(6) 0.071(3) Uani 1 1 d . . . O7 O 0.4638(8) 0.8423(6) 0.3193(6) 0.069(3) Uani 1 1 d . . . C46 C 0.4582(11) 0.8988(9) 0.3646(9) 0.061(3) Uani 1 1 d . . . C45 C 0.5392(8) 0.9644(7) 0.3385(7) 0.0429(15) Uani 1 1 d . . . H45A H 0.5896 0.9516 0.2832 0.064 Uiso 1 1 calc R . . H45B H 0.5834 0.9547 0.3844 0.064 Uiso 1 1 calc R . . H45C H 0.4976 1.0299 0.3310 0.064 Uiso 1 1 calc R . . C47 C 0.3788(15) 0.9099(13) 0.4444(12) 0.114(7) Uani 1 1 d . . . H47A H 0.3301 0.8639 0.4560 0.171 Uiso 1 1 calc R . . H47B H 0.3330 0.9740 0.4391 0.171 Uiso 1 1 calc R . . H47C H 0.4189 0.8994 0.4930 0.171 Uiso 1 1 calc R . . C21 C 0.2014(8) 0.5608(8) -0.6346(7) 0.0429(15) Uani 1 1 d . . . H21A H 0.1830 0.5292 -0.6764 0.064 Uiso 1 1 calc R . . H21B H 0.1539 0.6241 -0.6348 0.064 Uiso 1 1 calc R . . H21C H 0.1883 0.5238 -0.5757 0.064 Uiso 1 1 calc R . . C42 C 0.8350(8) 0.8324(8) -0.9462(7) 0.0429(15) Uani 1 1 d . . . H42A H 0.8916 0.7847 -0.9756 0.064 Uiso 1 1 calc R . . H42B H 0.8529 0.8339 -0.8897 0.064 Uiso 1 1 calc R . . H42C H 0.8345 0.8946 -0.9831 0.064 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 0.01886(18) 0.02518(19) 0.02464(18) 0.00023(13) -0.00443(13) -0.00712(13) C1 0.031(5) 0.034(5) 0.048(6) -0.004(4) -0.016(4) -0.013(4) C2 0.057(6) 0.033(5) 0.031(5) 0.000(4) -0.007(5) -0.026(5) C3 0.039(5) 0.034(5) 0.036(5) -0.013(4) -0.002(4) -0.010(4) C4 0.039(5) 0.026(5) 0.035(5) 0.000(4) -0.006(4) -0.011(4) C5 0.028(4) 0.026(4) 0.016(4) 0.000(3) -0.001(3) -0.011(4) C6 0.015(4) 0.027(4) 0.027(4) -0.002(3) -0.013(3) 0.000(3) C7 0.021(4) 0.022(4) 0.019(4) 0.000(3) -0.004(3) -0.006(3) C8 0.021(4) 0.032(5) 0.023(4) -0.002(3) -0.003(3) -0.008(4) C9 0.017(4) 0.033(5) 0.016(4) -0.002(3) -0.007(3) -0.005(3) C10 0.013(4) 0.026(4) 0.028(4) -0.006(3) 0.000(3) -0.004(3) C11 0.027(5) 0.027(5) 0.028(4) -0.007(4) -0.005(4) -0.006(4) C12 0.026(5) 0.041(6) 0.042(5) -0.020(4) -0.009(4) -0.004(4) C13 0.035(5) 0.029(5) 0.047(6) -0.005(4) -0.013(4) -0.010(4) C14 0.031(5) 0.029(5) 0.044(6) -0.006(4) -0.015(4) -0.008(4) C15 0.023(4) 0.027(5) 0.031(5) -0.007(4) -0.001(4) 0.000(4) C16 0.027(5) 0.028(5) 0.047(6) -0.004(4) -0.010(4) 0.007(4) C17 0.027(5) 0.029(5) 0.051(6) -0.001(4) -0.014(4) -0.002(4) C18 0.029(5) 0.035(5) 0.031(5) -0.001(4) -0.011(4) -0.003(4) C19 0.021(4) 0.032(5) 0.028(5) -0.005(4) -0.002(4) -0.003(4) C20 0.019(4) 0.020(4) 0.029(4) 0.001(3) -0.004(3) -0.003(3) N1 0.035(4) 0.029(4) 0.026(4) -0.002(3) -0.010(3) -0.012(3) N2 0.015(3) 0.028(4) 0.026(4) -0.001(3) -0.006(3) -0.006(3) N3 0.021(3) 0.027(4) 0.020(3) 0.002(3) -0.003(3) -0.010(3) N4 0.020(3) 0.026(4) 0.028(4) -0.003(3) -0.007(3) -0.008(3) Pt2 0.02057(18) 0.0289(2) 0.02567(19) 0.00192(14) -0.00461(13) -0.00854(14) C22 0.023(4) 0.052(6) 0.025(5) -0.005(4) 0.003(4) -0.017(4) C23 0.037(5) 0.047(6) 0.031(5) -0.007(4) 0.003(4) -0.012(5) C24 0.036(5) 0.050(6) 0.027(5) -0.013(4) -0.002(4) -0.008(5) C25 0.025(4) 0.033(5) 0.031(5) -0.003(4) -0.004(4) -0.009(4) C26 0.022(4) 0.036(5) 0.020(4) -0.004(4) -0.003(3) -0.004(4) C27 0.012(4) 0.026(4) 0.025(4) 0.003(3) -0.007(3) -0.006(3) C28 0.016(4) 0.032(5) 0.023(4) 0.000(3) -0.007(3) -0.007(3) C29 0.020(4) 0.026(5) 0.028(4) 0.005(3) -0.009(3) -0.004(3) C30 0.024(4) 0.022(4) 0.023(4) -0.002(3) 0.000(3) 0.000(3) C31 0.017(4) 0.030(5) 0.030(5) 0.000(4) -0.004(3) -0.006(3) C32 0.026(5) 0.033(5) 0.036(5) -0.002(4) -0.010(4) -0.005(4) C33 0.029(5) 0.042(6) 0.042(6) -0.018(5) -0.006(4) 0.001(4) C34 0.021(5) 0.060(7) 0.034(5) -0.013(5) -0.002(4) -0.005(4) C35 0.016(4) 0.049(6) 0.027(5) -0.002(4) -0.006(3) -0.008(4) C36 0.022(4) 0.029(5) 0.031(5) -0.010(4) -0.010(4) -0.006(3) C37 0.024(4) 0.044(6) 0.028(5) -0.007(4) -0.010(4) -0.005(4) C38 0.025(4) 0.033(5) 0.032(5) 0.000(4) -0.011(4) -0.002(4) C39 0.019(4) 0.033(5) 0.034(5) 0.002(4) -0.005(4) -0.007(4) C40 0.020(4) 0.034(5) 0.033(5) 0.000(4) -0.005(4) -0.004(4) C41 0.018(4) 0.038(5) 0.022(4) 0.005(4) -0.002(3) -0.014(4) N5 0.024(4) 0.032(4) 0.027(4) -0.003(3) -0.002(3) -0.009(3) N6 0.012(3) 0.033(4) 0.023(4) -0.002(3) -0.002(3) -0.011(3) N7 0.023(4) 0.023(4) 0.026(4) -0.001(3) -0.001(3) -0.005(3) N8 0.025(4) 0.026(4) 0.022(4) 0.001(3) 0.001(3) -0.004(3) S1 0.0503(15) 0.0368(14) 0.0306(12) -0.0079(10) 0.0078(11) -0.0152(12) O1 0.136(9) 0.070(6) 0.043(5) -0.027(4) 0.030(5) -0.070(6) O2 0.074(5) 0.045(5) 0.033(4) -0.007(3) -0.007(4) -0.011(4) O3 0.056(5) 0.057(5) 0.041(4) -0.009(4) 0.011(4) -0.022(4) C43 0.049(8) 0.115(14) 0.062(9) -0.022(8) -0.016(7) -0.016(8) F1 0.124(9) 0.194(13) 0.088(7) -0.030(7) -0.066(6) 0.012(8) F2 0.048(5) 0.240(14) 0.102(7) -0.068(8) 0.007(5) -0.034(7) F3 0.111(7) 0.065(6) 0.110(7) -0.029(5) -0.041(6) 0.033(5) S2 0.0466(15) 0.0402(15) 0.0444(15) -0.0054(12) -0.0060(12) -0.0015(12) O4 0.088(8) 0.099(9) 0.163(12) -0.012(8) -0.082(8) -0.005(7) O5 0.123(8) 0.045(5) 0.050(5) 0.000(4) 0.035(5) 0.008(5) O6 0.090(7) 0.044(5) 0.065(6) -0.008(4) 0.006(5) -0.036(5) C44 0.049(7) 0.056(8) 0.066(8) -0.016(6) 0.002(6) -0.010(6) F4 0.118(7) 0.045(5) 0.115(7) -0.019(4) 0.034(6) -0.042(5) F5 0.061(5) 0.081(7) 0.171(10) -0.029(6) -0.043(6) 0.019(5) F6 0.158(9) 0.057(5) 0.068(5) -0.027(4) 0.044(5) -0.029(5) O8 0.154(10) 0.054(6) 0.080(7) -0.034(5) 0.053(7) -0.042(6) C48 0.133(15) 0.069(11) 0.058(9) -0.008(8) 0.025(10) -0.034(10) C49 0.143(15) 0.042(8) 0.058(9) -0.012(6) 0.043(9) -0.032(9) C50 0.150(18) 0.070(12) 0.097(13) -0.021(10) 0.016(12) 0.035(11) O9 0.064(5) 0.091(7) 0.072(6) -0.044(5) 0.021(5) -0.046(5) O7 0.101(7) 0.052(5) 0.061(5) -0.010(4) -0.047(5) 0.005(5) C46 0.072(9) 0.043(7) 0.067(9) -0.005(6) -0.038(7) 0.013(6) C45 0.030(3) 0.045(4) 0.053(4) 0.007(3) -0.015(3) -0.012(3) C47 0.110(15) 0.098(14) 0.096(13) -0.013(11) 0.011(11) 0.019(11) C21 0.030(3) 0.045(4) 0.053(4) 0.007(3) -0.015(3) -0.012(3) C42 0.030(3) 0.045(4) 0.053(4) 0.007(3) -0.015(3) -0.012(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 N5 2.0208(15) . ? Pt1 N4 2.0390 . ? Pt1 N6 2.0904(15) . ? Pt1 C21 2.091(9) . ? C1 N1 1.337(9) . ? C1 C2 1.383(14) . ? C1 H1A 0.9500 . ? C2 C3 1.394(14) . ? C2 H2A 0.9500 . ? C3 C4 1.391(13) . ? C3 H3A 0.9500 . ? C4 C5 1.376(12) . ? C4 H4A 0.9500 . ? C5 N1 1.378(8) . ? C5 C6 1.495(11) . ? C6 N2 1.343(8) . ? C6 C7 1.421(11) . ? C7 C8 1.393(12) . ? C7 C15 1.519(11) . ? C8 C9 1.402(11) . ? C8 C20 1.515(8) . ? C9 N3 1.330(8) . ? C9 C10 1.490(12) . ? C10 C11 1.367(12) . ? C10 N4 1.369(8) . ? C11 C12 1.385(13) . ? C11 H11A 0.9500 . ? C12 C13 1.377(14) . ? C12 H12A 0.9500 . ? C13 C14 1.351(13) . ? C13 H13A 0.9500 . ? C14 N4 1.339(9) . ? C14 H14A 0.9500 . ? C15 C16 1.555(12) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.524(13) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.552(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.497(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.553(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N1 Pt2 1.9958 . ? N2 N3 1.3454 . ? N2 Pt2 2.1023 . ? Pt2 N8 2.0275(15) . ? Pt2 C42 2.078(9) . ? C22 C23 1.341(10) . ? C22 N5 1.3447(14) . ? C22 H22A 0.9500 . ? C23 C24 1.392(14) . ? C23 H23A 0.9500 . ? C24 C25 1.363(12) . ? C24 H24A 0.9500 . ? C25 C26 1.377(12) . ? C25 H25A 0.9500 . ? C26 N5 1.373(9) . ? C26 C27 1.475(11) . ? C27 N6 1.352(9) . ? C27 C28 1.419(10) . ? C28 C29 1.387(12) . ? C28 C36 1.494(11) . ? C29 C30 1.427(12) . ? C29 C41 1.504(8) . ? C30 N7 1.319(9) . ? C30 C31 1.507(11) . ? C31 N8 1.358(9) . ? C31 C32 1.374(13) . ? C32 C33 1.379(13) . ? C32 H32A 0.9500 . ? C33 C34 1.357(14) . ? C33 H33A 0.9500 . ? C34 C35 1.388(14) . ? C34 H34A 0.9500 . ? C35 N8 1.360(9) . ? C35 H35A 0.9500 . ? C36 C37 1.530(12) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.537(12) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.520(13) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.543(12) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.529(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? N6 N7 1.3295 . ? S1 O1 1.4370 . ? S1 O3 1.4371 . ? S1 O2 1.4400 . ? S1 C43 1.8366 . ? C43 F2 1.3257 . ? C43 F3 1.3310 . ? C43 F1 1.3338 . ? S2 O4 1.4047 . ? S2 O5 1.4142 . ? S2 O6 1.4426 . ? S2 C44 1.8065 . ? C44 F5 1.2954 . ? C44 F4 1.3173 . ? C44 F6 1.3303 . ? O8 C49 1.222(15) . ? C48 C49 1.48(2) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.51(2) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? O7 C46 1.190(15) . ? C46 C47 1.43(2) . ? C46 C45 1.498(17) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 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 N5 Pt1 N4 175.6 . . ? N5 Pt1 N6 78.24(6) . . ? N4 Pt1 N6 97.7 . . ? N5 Pt1 C21 96.7(3) . . ? N4 Pt1 C21 87.4(3) . . ? N6 Pt1 C21 174.9(3) . . ? N1 C1 C2 124.3(8) . . ? N1 C1 H1A 117.8 . . ? C2 C1 H1A 117.8 . . ? C1 C2 C3 117.3(9) . . ? C1 C2 H2A 121.4 . . ? C3 C2 H2A 121.4 . . ? C4 C3 C2 119.5(9) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C5 C4 C3 119.8(9) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 N1 121.1(7) . . ? C4 C5 C6 124.7(8) . . ? N1 C5 C6 114.1(6) . . ? N2 C6 C7 120.3(7) . . ? N2 C6 C5 112.3(6) . . ? C7 C6 C5 127.4(7) . . ? C8 C7 C6 116.1(7) . . ? C8 C7 C15 119.8(7) . . ? C6 C7 C15 124.0(7) . . ? C7 C8 C9 119.1(7) . . ? C7 C8 C20 122.5(7) . . ? C9 C8 C20 118.3(7) . . ? N3 C9 C8 123.1(7) . . ? N3 C9 C10 112.9(6) . . ? C8 C9 C10 124.0(7) . . ? C11 C10 N4 120.9(7) . . ? C11 C10 C9 122.8(8) . . ? N4 C10 C9 116.3(7) . . ? C10 C11 C12 119.7(8) . . ? C10 C11 H11A 120.2 . . ? C12 C11 H11A 120.2 . . ? C13 C12 C11 118.4(9) . . ? C13 C12 H12A 120.8 . . ? C11 C12 H12A 120.8 . . ? C14 C13 C12 120.1(9) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? N4 C14 C13 122.3(9) . . ? N4 C14 H14A 118.8 . . ? C13 C14 H14A 118.8 . . ? C7 C15 C16 115.5(7) . . ? C7 C15 H15A 108.4 . . ? C16 C15 H15A 108.4 . . ? C7 C15 H15B 108.4 . . ? C16 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C17 C16 C15 118.5(8) . . ? C17 C16 H16A 107.7 . . ? C15 C16 H16A 107.7 . . ? C17 C16 H16B 107.7 . . ? C15 C16 H16B 107.7 . . ? H16A C16 H16B 107.1 . . ? C16 C17 C18 115.7(8) . . ? C16 C17 H17A 108.4 . . ? C18 C17 H17A 108.4 . . ? C16 C17 H17B 108.4 . . ? C18 C17 H17B 108.4 . . ? H17A C17 H17B 107.4 . . ? C19 C18 C17 116.2(8) . . ? C19 C18 H18A 108.2 . . ? C17 C18 H18A 108.2 . . ? C19 C18 H18B 108.2 . . ? C17 C18 H18B 108.2 . . ? H18A C18 H18B 107.4 . . ? C18 C19 C20 115.7(7) . . ? C18 C19 H19A 108.3 . . ? C20 C19 H19A 108.3 . . ? C18 C19 H19B 108.3 . . ? C20 C19 H19B 108.3 . . ? H19A C19 H19B 107.4 . . ? C8 C20 C19 110.5(4) . . ? C8 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? C8 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C1 N1 C5 117.9(6) . . ? C1 N1 Pt2 123.9(4) . . ? C5 N1 Pt2 118.1(4) . . ? C6 N2 N3 123.9(4) . . ? C6 N2 Pt2 116.4(4) . . ? N3 N2 Pt2 118.9 . . ? C9 N3 N2 117.2(4) . . ? C14 N4 C10 118.5(6) . . ? C14 N4 Pt1 118.8(4) . . ? C10 N4 Pt1 122.6(4) . . ? N1 Pt2 N8 176.7 . . ? N1 Pt2 C42 96.1(3) . . ? N8 Pt2 C42 87.1(3) . . ? N1 Pt2 N2 77.9 . . ? N8 Pt2 N2 99.0 . . ? C42 Pt2 N2 173.7(3) . . ? C23 C22 N5 123.3(4) . . ? C23 C22 H22A 118.4 . . ? N5 C22 H22A 118.4 . . ? C22 C23 C24 118.7(8) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? C25 C24 C23 118.1(9) . . ? C25 C24 H24A 120.9 . . ? C23 C24 H24A 120.9 . . ? C24 C25 C26 122.2(9) . . ? C24 C25 H25A 118.9 . . ? C26 C25 H25A 118.9 . . ? N5 C26 C25 117.9(7) . . ? N5 C26 C27 115.4(7) . . ? C25 C26 C27 126.6(8) . . ? N6 C27 C28 119.8(7) . . ? N6 C27 C26 112.5(6) . . ? C28 C27 C26 127.7(8) . . ? C29 C28 C27 116.5(8) . . ? C29 C28 C36 120.2(7) . . ? C27 C28 C36 123.1(7) . . ? C28 C29 C30 117.9(7) . . ? C28 C29 C41 122.3(7) . . ? C30 C29 C41 119.6(7) . . ? N7 C30 C29 124.4(7) . . ? N7 C30 C31 113.4(7) . . ? C29 C30 C31 122.2(7) . . ? N8 C31 C32 120.7(7) . . ? N8 C31 C30 117.5(7) . . ? C32 C31 C30 121.7(8) . . ? C31 C32 C33 121.2(9) . . ? C31 C32 H32A 119.4 . . ? C33 C32 H32A 119.4 . . ? C34 C33 C32 117.9(9) . . ? C34 C33 H33A 121.0 . . ? C32 C33 H33A 121.0 . . ? C33 C34 C35 120.3(9) . . ? C33 C34 H34A 119.8 . . ? C35 C34 H34A 119.8 . . ? N8 C35 C34 121.5(8) . . ? N8 C35 H35A 119.3 . . ? C34 C35 H35A 119.3 . . ? C28 C36 C37 116.5(8) . . ? C28 C36 H36A 108.2 . . ? C37 C36 H36A 108.2 . . ? C28 C36 H36B 108.2 . . ? C37 C36 H36B 108.2 . . ? H36A C36 H36B 107.3 . . ? C36 C37 C38 117.4(7) . . ? C36 C37 H37A 108.0 . . ? C38 C37 H37A 108.0 . . ? C36 C37 H37B 108.0 . . ? C38 C37 H37B 108.0 . . ? H37A C37 H37B 107.2 . . ? C39 C38 C37 115.9(8) . . ? C39 C38 H38A 108.3 . . ? C37 C38 H38A 108.3 . . ? C39 C38 H38B 108.3 . . ? C37 C38 H38B 108.3 . . ? H38A C38 H38B 107.4 . . ? C38 C39 C40 116.1(8) . . ? C38 C39 H39A 108.3 . . ? C40 C39 H39A 108.3 . . ? C38 C39 H39B 108.3 . . ? C40 C39 H39B 108.3 . . ? H39A C39 H39B 107.4 . . ? C41 C40 C39 113.9(6) . . ? C41 C40 H40A 108.8 . . ? C39 C40 H40A 108.8 . . ? C41 C40 H40B 108.8 . . ? C39 C40 H40B 108.8 . . ? H40A C40 H40B 107.7 . . ? C29 C41 C40 110.4(5) . . ? C29 C41 H41A 109.6 . . ? C40 C41 H41A 109.6 . . ? C29 C41 H41B 109.6 . . ? C40 C41 H41B 109.6 . . ? H41A C41 H41B 108.1 . . ? C22 N5 C26 119.3(4) . . ? C22 N5 Pt1 123.99(10) . . ? C26 N5 Pt1 116.4(4) . . ? N7 N6 C27 125.1(3) . . ? N7 N6 Pt1 117.9 . . ? C27 N6 Pt1 116.3(3) . . ? C30 N7 N6 116.1(4) . . ? C31 N8 C35 118.2(6) . . ? C31 N8 Pt2 122.8(4) . . ? C35 N8 Pt2 119.0(4) . . ? O1 S1 O3 115.5 . . ? O1 S1 O2 115.4 . . ? O3 S1 O2 114.7 . . ? O1 S1 C43 102.5 . . ? O3 S1 C43 103.5 . . ? O2 S1 C43 102.5 . . ? F2 C43 F3 108.1 . . ? F2 C43 F1 111.3 . . ? F3 C43 F1 107.4 . . ? F2 C43 S1 110.6 . . ? F3 C43 S1 110.5 . . ? F1 C43 S1 109.0 . . ? O4 S2 O5 120.1 . . ? O4 S2 O6 110.6 . . ? O5 S2 O6 113.2 . . ? O4 S2 C44 103.5 . . ? O5 S2 C44 102.7 . . ? O6 S2 C44 104.5 . . ? F5 C44 F4 104.1 . . ? F5 C44 F6 108.5 . . ? F4 C44 F6 106.7 . . ? F5 C44 S2 113.1 . . ? F4 C44 S2 112.3 . . ? F6 C44 S2 111.6 . . ? C49 C48 H48A 109.5 . . ? C49 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C49 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O8 C49 C48 122.4(13) . . ? O8 C49 C50 119.5(18) . . ? C48 C49 C50 118.1(13) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O7 C46 C47 125.0(16) . . ? O7 C46 C45 119.4(13) . . ? C47 C46 C45 115.6(14) . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Pt1 C21 H21A 109.5 . . ? Pt1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Pt1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Pt2 C42 H42A 109.5 . . ? Pt2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Pt2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.3(14) . . . . ? C1 C2 C3 C4 -0.5(14) . . . . ? C2 C3 C4 C5 2.2(14) . . . . ? C3 C4 C5 N1 -3.7(13) . . . . ? C3 C4 C5 C6 -178.6(8) . . . . ? C4 C5 C6 N2 165.1(7) . . . . ? N1 C5 C6 N2 -10.2(9) . . . . ? C4 C5 C6 C7 -13.1(13) . . . . ? N1 C5 C6 C7 171.6(7) . . . . ? N2 C6 C7 C8 -2.7(11) . . . . ? C5 C6 C7 C8 175.3(8) . . . . ? N2 C6 C7 C15 172.0(7) . . . . ? C5 C6 C7 C15 -10.0(13) . . . . ? C6 C7 C8 C9 5.5(11) . . . . ? C15 C7 C8 C9 -169.4(7) . . . . ? C6 C7 C8 C20 -170.7(6) . . . . ? C15 C7 C8 C20 14.4(11) . . . . ? C7 C8 C9 N3 -6.9(12) . . . . ? C20 C8 C9 N3 169.5(5) . . . . ? C7 C8 C9 C10 172.0(8) . . . . ? C20 C8 C9 C10 -11.6(11) . . . . ? N3 C9 C10 C11 -74.8(9) . . . . ? C8 C9 C10 C11 106.3(10) . . . . ? N3 C9 C10 N4 104.7(7) . . . . ? C8 C9 C10 N4 -74.2(10) . . . . ? N4 C10 C11 C12 -3.4(12) . . . . ? C9 C10 C11 C12 176.0(8) . . . . ? C10 C11 C12 C13 0.8(13) . . . . ? C11 C12 C13 C14 1.6(14) . . . . ? C12 C13 C14 N4 -1.5(14) . . . . ? C8 C7 C15 C16 -88.9(10) . . . . ? C6 C7 C15 C16 96.6(10) . . . . ? C7 C15 C16 C17 70.3(11) . . . . ? C15 C16 C17 C18 -64.4(11) . . . . ? C16 C17 C18 C19 99.5(10) . . . . ? C17 C18 C19 C20 -51.5(10) . . . . ? C7 C8 C20 C19 85.9(8) . . . . ? C9 C8 C20 C19 -90.4(8) . . . . ? C18 C19 C20 C8 -57.1(8) . . . . ? C2 C1 N1 C5 -1.8(12) . . . . ? C2 C1 N1 Pt2 174.3(7) . . . . ? C4 C5 N1 C1 3.4(10) . . . . ? C6 C5 N1 C1 178.9(7) . . . . ? C4 C5 N1 Pt2 -172.8(6) . . . . ? C6 C5 N1 Pt2 2.6(7) . . . . ? C7 C6 N2 N3 0.8(9) . . . . ? C5 C6 N2 N3 -177.6(4) . . . . ? C7 C6 N2 Pt2 -168.7(5) . . . . ? C5 C6 N2 Pt2 13.0(7) . . . . ? C8 C9 N3 N2 4.7(9) . . . . ? C10 C9 N3 N2 -174.3(5) . . . . ? C6 N2 N3 C9 -1.6(6) . . . . ? Pt2 N2 N3 C9 167.6(4) . . . . ? C13 C14 N4 C10 -1.1(11) . . . . ? C13 C14 N4 Pt1 -179.0(7) . . . . ? C11 C10 N4 C14 3.6(9) . . . . ? C9 C10 N4 C14 -175.9(6) . . . . ? C11 C10 N4 Pt1 -178.6(5) . . . . ? C9 C10 N4 Pt1 1.9(8) . . . . ? N5 Pt1 N4 C14 83.2(7) . . . . ? N6 Pt1 N4 C14 107.2(4) . . . . ? C21 Pt1 N4 C14 -73.4(5) . . . . ? N5 Pt1 N4 C10 -94.7(7) . . . . ? N6 Pt1 N4 C10 -70.6(4) . . . . ? C21 Pt1 N4 C10 108.8(5) . . . . ? C1 N1 Pt2 N8 -153.0(9) . . . . ? C5 N1 Pt2 N8 23.0(8) . . . . ? C1 N1 Pt2 C42 8.9(6) . . . . ? C5 N1 Pt2 C42 -175.1(5) . . . . ? C1 N1 Pt2 N2 -172.9(5) . . . . ? C5 N1 Pt2 N2 3.2(4) . . . . ? C6 N2 Pt2 N1 -9.3(4) . . . . ? N3 N2 Pt2 N1 -179.3 . . . . ? C6 N2 Pt2 N8 171.8(4) . . . . ? N3 N2 Pt2 N8 1.8 . . . . ? C6 N2 Pt2 C42 7(3) . . . . ? N3 N2 Pt2 C42 -163(3) . . . . ? N5 C22 C23 C24 -1.0(11) . . . . ? C22 C23 C24 C25 3.0(15) . . . . ? C23 C24 C25 C26 0.2(15) . . . . ? C24 C25 C26 N5 -5.2(13) . . . . ? C24 C25 C26 C27 179.8(9) . . . . ? N5 C26 C27 N6 -12.5(10) . . . . ? C25 C26 C27 N6 162.6(8) . . . . ? N5 C26 C27 C28 164.9(7) . . . . ? C25 C26 C27 C28 -20.0(14) . . . . ? N6 C27 C28 C29 -4.1(11) . . . . ? C26 C27 C28 C29 178.7(8) . . . . ? N6 C27 C28 C36 171.1(7) . . . . ? C26 C27 C28 C36 -6.1(13) . . . . ? C27 C28 C29 C30 4.6(11) . . . . ? C36 C28 C29 C30 -170.8(7) . . . . ? C27 C28 C29 C41 -170.0(6) . . . . ? C36 C28 C29 C41 14.6(12) . . . . ? C28 C29 C30 N7 -4.5(12) . . . . ? C41 C29 C30 N7 170.2(6) . . . . ? C28 C29 C30 C31 174.9(8) . . . . ? C41 C29 C30 C31 -10.4(11) . . . . ? N7 C30 C31 N8 106.0(8) . . . . ? C29 C30 C31 N8 -73.4(10) . . . . ? N7 C30 C31 C32 -71.7(10) . . . . ? C29 C30 C31 C32 108.9(10) . . . . ? N8 C31 C32 C33 1.3(13) . . . . ? C30 C31 C32 C33 179.0(8) . . . . ? C31 C32 C33 C34 1.5(14) . . . . ? C32 C33 C34 C35 -2.3(14) . . . . ? C33 C34 C35 N8 0.3(14) . . . . ? C29 C28 C36 C37 -89.1(10) . . . . ? C27 C28 C36 C37 95.9(10) . . . . ? C28 C36 C37 C38 69.2(11) . . . . ? C36 C37 C38 C39 -64.9(11) . . . . ? C37 C38 C39 C40 100.3(9) . . . . ? C38 C39 C40 C41 -49.8(10) . . . . ? C28 C29 C41 C40 87.5(9) . . . . ? C30 C29 C41 C40 -87.0(8) . . . . ? C39 C40 C41 C29 -59.4(8) . . . . ? C23 C22 N5 C26 -4.1(7) . . . . ? C23 C22 N5 Pt1 169.5(5) . . . . ? C25 C26 N5 C22 7.1(9) . . . . ? C27 C26 N5 C22 -177.4(5) . . . . ? C25 C26 N5 Pt1 -167.0(6) . . . . ? C27 C26 N5 Pt1 8.5(8) . . . . ? N4 Pt1 N5 C22 -151.6(5) . . . . ? N6 Pt1 N5 C22 -175.96(7) . . . . ? C21 Pt1 N5 C22 4.8(3) . . . . ? N4 Pt1 N5 C26 22.2(8) . . . . ? N6 Pt1 N5 C26 -2.2(4) . . . . ? C21 Pt1 N5 C26 178.6(5) . . . . ? C28 C27 N6 N7 3.3(9) . . . . ? C26 C27 N6 N7 -179.1(4) . . . . ? C28 C27 N6 Pt1 -167.0(6) . . . . ? C26 C27 N6 Pt1 10.6(7) . . . . ? N5 Pt1 N6 N7 -176.0 . . . . ? N4 Pt1 N6 N7 5.8 . . . . ? C21 Pt1 N6 N7 -168(3) . . . . ? N5 Pt1 N6 C27 -5.1(4) . . . . ? N4 Pt1 N6 C27 176.8(4) . . . . ? C21 Pt1 N6 C27 3(3) . . . . ? C29 C30 N7 N6 3.3(9) . . . . ? C31 C30 N7 N6 -176.1(5) . . . . ? C27 N6 N7 C30 -2.7(6) . . . . ? Pt1 N6 N7 C30 167.4(4) . . . . ? C32 C31 N8 C35 -3.3(10) . . . . ? C30 C31 N8 C35 178.9(7) . . . . ? C32 C31 N8 Pt2 175.9(6) . . . . ? C30 C31 N8 Pt2 -1.8(9) . . . . ? C34 C35 N8 C31 2.5(10) . . . . ? C34 C35 N8 Pt2 -176.8(6) . . . . ? N1 Pt2 N8 C31 -85.1(8) . . . . ? C42 Pt2 N8 C31 113.0(5) . . . . ? N2 Pt2 N8 C31 -65.4(4) . . . . ? N1 Pt2 N8 C35 94.2(8) . . . . ? C42 Pt2 N8 C35 -67.8(5) . . . . ? N2 Pt2 N8 C35 113.8(4) . . . . ? O1 S1 C43 F2 62.6 . . . . ? O3 S1 C43 F2 -177.0 . . . . ? O2 S1 C43 F2 -57.4 . . . . ? O1 S1 C43 F3 -177.8 . . . . ? O3 S1 C43 F3 -57.3 . . . . ? O2 S1 C43 F3 62.2 . . . . ? O1 S1 C43 F1 -60.1 . . . . ? O3 S1 C43 F1 60.4 . . . . ? O2 S1 C43 F1 179.9 . . . . ? O4 S2 C44 F5 177.7 . . . . ? O5 S2 C44 F5 -56.7 . . . . ? O6 S2 C44 F5 61.7 . . . . ? O4 S2 C44 F4 -64.9 . . . . ? O5 S2 C44 F4 60.8 . . . . ? O6 S2 C44 F4 179.2 . . . . ? O4 S2 C44 F6 54.9 . . . . ? O5 S2 C44 F6 -179.4 . . . . ? O6 S2 C44 F6 -61.0 . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.974 _refine_diff_density_min -2.584 _refine_diff_density_rms 0.385 #===END data_4c _database_code_depnum_ccdc_archive 'CCDC 869546' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H46 N8 Pt2, 2(C F3 O3 S), C H2 Cl2' _chemical_formula_sum 'C45 H48 Cl2 F6 N8 O6 Pt2 S2' _chemical_formula_weight 1436.11 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.6348(8) _cell_length_b 22.0849(13) _cell_length_c 19.8889(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5549.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6960 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 28.44 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 5.278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4183 _exptl_absorpt_correction_T_max 0.7254 _exptl_absorpt_process_details 'SADABS (Bruker, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 90903 _diffrn_reflns_av_R_equivalents 0.1022 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.44 _reflns_number_total 6960 _reflns_number_gt 4322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Residual electron density associated with a disordered solvent molecule was eliminated using squeeze as an acceptable model for the disordered solvent molecule was unable to be found. The electron density related to this molecule was removed from the reflection data using SQUEEZE (PLATON), leaving a void of about 212 cubic angstrom. The triflate anions were modelled anisotropically however the trifluoromethyl group exhibits elongated ellipsoids for the fluorine atoms do to unmodelled disorder. ; _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^)+(0.0493P)^2^+34.8135P] 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 6960 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.15330(2) 0.045778(14) 0.129979(14) 0.02772(10) Uani 1 1 d . . . N1 N 0.1066(5) -0.0282(3) 0.0791(3) 0.0284(16) Uani 1 1 d . . . N2 N -0.0081(5) 0.0448(3) 0.1494(3) 0.0216(13) Uani 1 1 d . . . N3 N -0.0487(5) 0.0880(3) 0.1887(3) 0.0274(15) Uani 1 1 d . . . N4 N -0.1904(5) 0.1233(3) 0.3215(3) 0.0298(16) Uani 1 1 d . . . C1 C 0.1706(6) -0.0610(4) 0.0403(4) 0.035(2) Uani 1 1 d . . . H1A H 0.2443 -0.0525 0.0405 0.042 Uiso 1 1 calc R . . C2 C 0.1331(7) -0.1069(4) -0.0003(4) 0.039(2) Uani 1 1 d . . . H2A H 0.1804 -0.1295 -0.0276 0.047 Uiso 1 1 calc R . . C3 C 0.0282(7) -0.1193(3) -0.0009(4) 0.0304(18) Uani 1 1 d . . . H3B H 0.0006 -0.1499 -0.0294 0.036 Uiso 1 1 calc R . . C4 C -0.0379(6) -0.0866(4) 0.0407(4) 0.0274(17) Uani 1 1 d . . . H4B H -0.1118 -0.0947 0.0407 0.033 Uiso 1 1 calc R . . C5 C 0.0028(6) -0.0421(4) 0.0825(4) 0.0268(17) Uani 1 1 d . . . C6 C -0.0618(5) -0.0049(3) 0.1300(4) 0.0229(15) Uani 1 1 d . . . C7 C -0.1654(6) -0.0157(4) 0.1542(4) 0.0246(16) Uani 1 1 d . . . C8 C -0.2096(6) 0.0289(3) 0.1950(4) 0.0246(17) Uani 1 1 d . . . C9 C -0.1474(6) 0.0796(4) 0.2112(4) 0.0240(16) Uani 1 1 d . . . C10 C -0.1831(6) 0.1313(4) 0.2543(4) 0.0273(18) Uani 1 1 d . . . C11 C -0.2076(7) 0.1856(4) 0.2241(5) 0.037(2) Uani 1 1 d . . . H11A H -0.2042 0.1897 0.1766 0.045 Uiso 1 1 calc R . . C12 C -0.2375(9) 0.2348(4) 0.2642(5) 0.052(3) Uani 1 1 d . . . H12A H -0.2534 0.2729 0.2446 0.062 Uiso 1 1 calc R . . C13 C -0.2432(9) 0.2268(4) 0.3316(5) 0.048(2) Uani 1 1 d . . . H13A H -0.2642 0.2596 0.3596 0.057 Uiso 1 1 calc R . . C14 C -0.2191(8) 0.1720(5) 0.3600(5) 0.046(2) Uani 1 1 d . . . H14A H -0.2222 0.1676 0.4075 0.055 Uiso 1 1 calc R . . C15 C -0.2237(6) -0.0743(4) 0.1414(3) 0.0251(17) Uani 1 1 d . . . H15A H -0.2648 -0.0848 0.1821 0.030 Uiso 1 1 calc R . . H15B H -0.1710 -0.1068 0.1341 0.030 Uiso 1 1 calc R . . C16 C -0.2999(6) -0.0730(4) 0.0807(4) 0.035(2) Uani 1 1 d . . . H16A H -0.2614 -0.0557 0.0418 0.043 Uiso 1 1 calc R . . H16B H -0.3185 -0.1152 0.0691 0.043 Uiso 1 1 calc R . . C17 C -0.4034(8) -0.0369(4) 0.0902(5) 0.048(3) Uani 1 1 d . . . H17A H -0.4508 -0.0460 0.0518 0.058 Uiso 1 1 calc R . . H17B H -0.4387 -0.0517 0.1315 0.058 Uiso 1 1 calc R . . C18 C -0.3916(7) 0.0303(4) 0.0954(4) 0.037(2) Uani 1 1 d . . . H18A H -0.4473 0.0495 0.0675 0.044 Uiso 1 1 calc R . . H18B H -0.3224 0.0417 0.0757 0.044 Uiso 1 1 calc R . . C19 C -0.3981(6) 0.0570(4) 0.1667(4) 0.034(2) Uani 1 1 d . . . H19A H -0.4719 0.0533 0.1828 0.041 Uiso 1 1 calc R . . H19B H -0.3808 0.1006 0.1644 0.041 Uiso 1 1 calc R . . C20 C -0.3237(6) 0.0264(4) 0.2185(4) 0.031(2) Uani 1 1 d . . . H20A H -0.3302 0.0472 0.2624 0.037 Uiso 1 1 calc R . . H20B H -0.3451 -0.0164 0.2247 0.037 Uiso 1 1 calc R . . C21 C 0.3130(6) 0.0390(4) 0.1072(4) 0.0324(19) Uani 1 1 d . . . H21A H 0.3500 0.0751 0.1235 0.049 Uiso 1 1 calc R . . H21B H 0.3219 0.0357 0.0584 0.049 Uiso 1 1 calc R . . H21C H 0.3425 0.0029 0.1290 0.049 Uiso 1 1 calc R . . S1 S -0.1363(2) 0.25671(11) 0.56324(12) 0.0443(6) Uani 1 1 d . . . O1 O -0.1457(7) 0.2274(5) 0.5007(4) 0.097(3) Uani 1 1 d . . . O2 O -0.1998(6) 0.3094(3) 0.5739(4) 0.065(2) Uani 1 1 d . . . O3 O -0.1392(8) 0.2164(4) 0.6193(4) 0.088(3) Uani 1 1 d . . . C22 C -0.0008(13) 0.2890(11) 0.5663(10) 0.120(7) Uani 1 1 d . . . F1 F 0.0146(8) 0.3074(4) 0.6339(6) 0.140(4) Uani 1 1 d . . . F2 F 0.0679(6) 0.2443(4) 0.5559(7) 0.171(6) Uani 1 1 d . . . F3 F 0.0159(10) 0.3305(5) 0.5270(9) 0.186(8) Uani 1 1 d . . . C23 C 0.0000 -0.1712(6) 0.2500 0.051(4) Uani 1 2 d S . . H23A H 0.0351 -0.1976 0.2835 0.061 Uiso 0.50 1 calc PR . . H23B H -0.0351 -0.1976 0.2165 0.061 Uiso 0.50 1 calc PR . . Cl1 Cl 0.0957(3) -0.12736(14) 0.20958(15) 0.0729(9) 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 Pt1 0.02226(14) 0.03659(17) 0.02431(15) 0.00443(14) -0.00120(14) -0.00148(15) N1 0.017(3) 0.052(5) 0.016(3) 0.008(3) -0.002(3) 0.010(3) N2 0.017(3) 0.029(3) 0.019(3) 0.002(3) -0.002(2) 0.003(3) N3 0.029(4) 0.034(4) 0.019(3) -0.004(3) -0.009(3) 0.008(3) N4 0.025(3) 0.039(4) 0.025(4) -0.010(3) -0.005(3) 0.000(3) C1 0.022(4) 0.045(6) 0.038(5) 0.000(4) 0.007(3) 0.000(4) C2 0.045(6) 0.043(5) 0.029(5) 0.001(4) 0.013(4) 0.013(4) C3 0.044(5) 0.020(4) 0.027(4) -0.002(3) 0.003(4) 0.004(4) C4 0.023(4) 0.031(5) 0.028(4) 0.006(3) -0.001(3) 0.000(4) C5 0.030(4) 0.029(4) 0.021(4) 0.006(4) 0.002(3) 0.006(4) C6 0.021(3) 0.025(4) 0.023(4) 0.004(3) -0.008(3) 0.001(3) C7 0.025(4) 0.031(4) 0.018(3) 0.003(3) -0.006(3) 0.004(4) C8 0.020(4) 0.033(5) 0.022(4) 0.006(3) -0.005(3) 0.007(3) C9 0.017(3) 0.035(4) 0.020(4) 0.002(3) 0.000(3) 0.000(4) C10 0.023(4) 0.040(5) 0.019(4) -0.003(3) 0.000(3) 0.004(4) C11 0.036(5) 0.033(5) 0.043(5) -0.006(4) -0.008(4) 0.009(4) C12 0.067(7) 0.029(5) 0.058(7) -0.007(5) -0.007(6) 0.009(5) C13 0.060(7) 0.033(5) 0.050(6) -0.010(4) -0.003(5) 0.012(5) C14 0.047(6) 0.055(6) 0.034(5) -0.020(5) 0.004(4) 0.007(5) C15 0.026(4) 0.034(4) 0.016(4) -0.002(3) -0.001(3) 0.000(3) C16 0.024(4) 0.050(6) 0.032(5) 0.000(4) -0.011(4) 0.000(4) C17 0.060(6) 0.049(6) 0.036(5) -0.015(4) -0.024(5) 0.014(5) C18 0.029(4) 0.061(7) 0.020(4) -0.004(4) 0.003(3) 0.000(4) C19 0.011(4) 0.052(6) 0.039(5) -0.009(4) -0.002(3) -0.005(4) C20 0.018(4) 0.047(5) 0.028(4) -0.007(4) 0.000(3) 0.001(3) C21 0.020(3) 0.058(6) 0.019(3) -0.001(4) 0.002(3) 0.001(4) S1 0.0490(15) 0.0476(14) 0.0364(12) -0.0004(10) -0.0095(11) 0.0135(12) O1 0.092(7) 0.143(9) 0.054(5) -0.051(5) -0.039(5) 0.048(6) O2 0.071(5) 0.075(5) 0.050(4) -0.002(4) 0.002(4) 0.046(4) O3 0.146(9) 0.054(5) 0.063(5) 0.014(4) -0.015(6) 0.027(5) C22 0.073(11) 0.17(2) 0.112(14) -0.080(14) -0.015(10) 0.042(13) F1 0.105(7) 0.123(8) 0.193(11) -0.073(8) -0.066(7) 0.028(6) F2 0.047(5) 0.125(8) 0.341(17) -0.128(10) 0.002(7) 0.011(5) F3 0.137(10) 0.108(9) 0.31(2) 0.051(10) 0.115(12) -0.009(7) C23 0.073(10) 0.030(7) 0.050(9) 0.000 -0.035(8) 0.000 Cl1 0.098(2) 0.0628(19) 0.0584(18) 0.0196(14) -0.0330(17) -0.0131(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 Pt1 N1 2.010(7) . ? Pt1 N4 2.020(7) 3 ? Pt1 C21 2.073(7) . ? Pt1 N2 2.076(6) . ? N1 C1 1.333(10) . ? N1 C5 1.349(10) . ? N2 N3 1.336(8) . ? N2 C6 1.346(9) . ? N3 C9 1.338(10) . ? N4 C10 1.352(10) . ? N4 C14 1.368(11) . ? N4 Pt1 2.020(7) 3 ? C1 C2 1.379(12) . ? C1 H1A 0.9500 . ? C2 C3 1.354(12) . ? C2 H2A 0.9500 . ? C3 C4 1.378(11) . ? C3 H3B 0.9500 . ? C4 C5 1.386(11) . ? C4 H4B 0.9500 . ? C5 C6 1.496(10) . ? C6 C7 1.414(10) . ? C7 C8 1.393(10) . ? C7 C15 1.511(11) . ? C8 C9 1.406(11) . ? C8 C20 1.516(10) . ? C9 C10 1.496(11) . ? C10 C11 1.377(12) . ? C11 C12 1.400(12) . ? C11 H11A 0.9500 . ? C12 C13 1.354(14) . ? C12 H12A 0.9500 . ? C13 C14 1.371(13) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.544(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.543(13) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.496(12) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.537(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.551(11) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? S1 O1 1.407(7) . ? S1 O3 1.427(8) . ? S1 O2 1.430(7) . ? S1 C22 1.86(2) . ? C22 F3 1.22(2) . ? C22 F2 1.331(18) . ? C22 F1 1.418(18) . ? C23 Cl1 1.745(8) . ? C23 Cl1 1.745(8) 3 ? C23 H23A 0.9900 . ? C23 H23B 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 Pt1 N4 175.7(2) . 3 ? N1 Pt1 C21 96.7(3) . . ? N4 Pt1 C21 86.5(3) 3 . ? N1 Pt1 N2 78.3(3) . . ? N4 Pt1 N2 98.5(3) 3 . ? C21 Pt1 N2 174.9(3) . . ? C1 N1 C5 119.6(7) . . ? C1 N1 Pt1 123.7(6) . . ? C5 N1 Pt1 116.5(5) . . ? N3 N2 C6 123.9(6) . . ? N3 N2 Pt1 118.6(5) . . ? C6 N2 Pt1 116.7(5) . . ? N2 N3 C9 117.0(6) . . ? C10 N4 C14 117.9(8) . . ? C10 N4 Pt1 124.5(6) . 3 ? C14 N4 Pt1 117.4(6) . 3 ? N1 C1 C2 122.0(8) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C3 C2 C1 119.3(8) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 118.9(8) . . ? C2 C3 H3B 120.6 . . ? C4 C3 H3B 120.6 . . ? C3 C4 C5 120.4(8) . . ? C3 C4 H4B 119.8 . . ? C5 C4 H4B 119.8 . . ? N1 C5 C4 119.5(7) . . ? N1 C5 C6 115.9(7) . . ? C4 C5 C6 124.5(7) . . ? N2 C6 C7 120.4(7) . . ? N2 C6 C5 110.8(6) . . ? C7 C6 C5 128.8(7) . . ? C8 C7 C6 116.8(7) . . ? C8 C7 C15 120.5(7) . . ? C6 C7 C15 122.6(7) . . ? C7 C8 C9 118.2(7) . . ? C7 C8 C20 122.3(7) . . ? C9 C8 C20 119.4(7) . . ? N3 C9 C8 123.7(7) . . ? N3 C9 C10 111.5(7) . . ? C8 C9 C10 124.8(7) . . ? N4 C10 C11 122.0(8) . . ? N4 C10 C9 119.2(7) . . ? C11 C10 C9 118.9(7) . . ? C10 C11 C12 119.2(9) . . ? C10 C11 H11A 120.4 . . ? C12 C11 H11A 120.4 . . ? C13 C12 C11 118.6(9) . . ? C13 C12 H12A 120.7 . . ? C11 C12 H12A 120.7 . . ? C12 C13 C14 120.6(9) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? N4 C14 C13 121.6(8) . . ? N4 C14 H14A 119.2 . . ? C13 C14 H14A 119.2 . . ? C7 C15 C16 114.8(7) . . ? C7 C15 H15A 108.6 . . ? C16 C15 H15A 108.6 . . ? C7 C15 H15B 108.6 . . ? C16 C15 H15B 108.6 . . ? H15A C15 H15B 107.5 . . ? C17 C16 C15 116.2(7) . . ? C17 C16 H16A 108.2 . . ? C15 C16 H16A 108.2 . . ? C17 C16 H16B 108.2 . . ? C15 C16 H16B 108.2 . . ? H16A C16 H16B 107.4 . . ? C18 C17 C16 115.8(9) . . ? C18 C17 H17A 108.3 . . ? C16 C17 H17A 108.3 . . ? C18 C17 H17B 108.3 . . ? C16 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C17 C18 C19 116.0(8) . . ? C17 C18 H18A 108.3 . . ? C19 C18 H18A 108.3 . . ? C17 C18 H18B 108.3 . . ? C19 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? C18 C19 C20 114.4(7) . . ? C18 C19 H19A 108.6 . . ? C20 C19 H19A 108.6 . . ? C18 C19 H19B 108.6 . . ? C20 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? C8 C20 C19 110.8(7) . . ? C8 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? C8 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? Pt1 C21 H21A 109.5 . . ? Pt1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Pt1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 S1 O3 113.7(6) . . ? O1 S1 O2 117.2(5) . . ? O3 S1 O2 112.2(5) . . ? O1 S1 C22 106.5(7) . . ? O3 S1 C22 103.7(9) . . ? O2 S1 C22 101.5(7) . . ? F3 C22 F2 110.1(17) . . ? F3 C22 F1 111.6(19) . . ? F2 C22 F1 105.8(15) . . ? F3 C22 S1 115.2(15) . . ? F2 C22 S1 108.1(14) . . ? F1 C22 S1 105.5(13) . . ? Cl1 C23 Cl1 112.7(7) . 3 ? Cl1 C23 H23A 109.1 . . ? Cl1 C23 H23A 109.1 3 . ? Cl1 C23 H23B 109.1 . . ? Cl1 C23 H23B 109.1 3 . ? H23A C23 H23B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Pt1 N1 C1 133(3) 3 . . . ? C21 Pt1 N1 C1 -5.9(7) . . . . ? N2 Pt1 N1 C1 175.2(7) . . . . ? N4 Pt1 N1 C5 -43(4) 3 . . . ? C21 Pt1 N1 C5 178.1(6) . . . . ? N2 Pt1 N1 C5 -0.8(5) . . . . ? N1 Pt1 N2 N3 179.2(5) . . . . ? N4 Pt1 N2 N3 -3.7(5) 3 . . . ? C21 Pt1 N2 N3 167(3) . . . . ? N1 Pt1 N2 C6 9.2(5) . . . . ? N4 Pt1 N2 C6 -173.7(5) 3 . . . ? C21 Pt1 N2 C6 -3(3) . . . . ? C6 N2 N3 C9 2.2(10) . . . . ? Pt1 N2 N3 C9 -167.0(5) . . . . ? C5 N1 C1 C2 4.1(12) . . . . ? Pt1 N1 C1 C2 -171.8(6) . . . . ? N1 C1 C2 C3 -0.1(13) . . . . ? C1 C2 C3 C4 -1.7(13) . . . . ? C2 C3 C4 C5 -0.4(12) . . . . ? C1 N1 C5 C4 -6.1(11) . . . . ? Pt1 N1 C5 C4 170.1(5) . . . . ? C1 N1 C5 C6 177.0(7) . . . . ? Pt1 N1 C5 C6 -6.8(8) . . . . ? C3 C4 C5 N1 4.3(11) . . . . ? C3 C4 C5 C6 -179.1(7) . . . . ? N3 N2 C6 C7 -3.7(10) . . . . ? Pt1 N2 C6 C7 165.7(5) . . . . ? N3 N2 C6 C5 176.0(6) . . . . ? Pt1 N2 C6 C5 -14.6(7) . . . . ? N1 C5 C6 N2 13.9(9) . . . . ? C4 C5 C6 N2 -162.7(7) . . . . ? N1 C5 C6 C7 -166.4(7) . . . . ? C4 C5 C6 C7 16.9(12) . . . . ? N2 C6 C7 C8 3.7(10) . . . . ? C5 C6 C7 C8 -175.9(7) . . . . ? N2 C6 C7 C15 -171.9(6) . . . . ? C5 C6 C7 C15 8.5(11) . . . . ? C6 C7 C8 C9 -2.5(10) . . . . ? C15 C7 C8 C9 173.2(6) . . . . ? C6 C7 C8 C20 173.6(7) . . . . ? C15 C7 C8 C20 -10.7(10) . . . . ? N2 N3 C9 C8 -0.9(10) . . . . ? N2 N3 C9 C10 -179.8(6) . . . . ? C7 C8 C9 N3 1.2(11) . . . . ? C20 C8 C9 N3 -175.0(7) . . . . ? C7 C8 C9 C10 180.0(7) . . . . ? C20 C8 C9 C10 3.8(11) . . . . ? C14 N4 C10 C11 -2.7(12) . . . . ? Pt1 N4 C10 C11 -178.7(6) 3 . . . ? C14 N4 C10 C9 177.4(7) . . . . ? Pt1 N4 C10 C9 1.4(10) 3 . . . ? N3 C9 C10 N4 -106.8(8) . . . . ? C8 C9 C10 N4 74.3(10) . . . . ? N3 C9 C10 C11 73.3(9) . . . . ? C8 C9 C10 C11 -105.6(9) . . . . ? N4 C10 C11 C12 2.3(13) . . . . ? C9 C10 C11 C12 -177.8(8) . . . . ? C10 C11 C12 C13 -1.2(15) . . . . ? C11 C12 C13 C14 0.8(17) . . . . ? C10 N4 C14 C13 2.2(13) . . . . ? Pt1 N4 C14 C13 178.5(8) 3 . . . ? C12 C13 C14 N4 -1.3(16) . . . . ? C8 C7 C15 C16 88.5(8) . . . . ? C6 C7 C15 C16 -96.1(9) . . . . ? C7 C15 C16 C17 -73.3(10) . . . . ? C15 C16 C17 C18 68.9(11) . . . . ? C16 C17 C18 C19 -101.8(9) . . . . ? C17 C18 C19 C20 51.7(10) . . . . ? C7 C8 C20 C19 -88.1(9) . . . . ? C9 C8 C20 C19 87.9(8) . . . . ? C18 C19 C20 C8 56.6(9) . . . . ? O1 S1 C22 F3 67.8(16) . . . . ? O3 S1 C22 F3 -171.9(14) . . . . ? O2 S1 C22 F3 -55.4(15) . . . . ? O1 S1 C22 F2 -55.8(16) . . . . ? O3 S1 C22 F2 64.5(15) . . . . ? O2 S1 C22 F2 -179.0(13) . . . . ? O1 S1 C22 F1 -168.6(11) . . . . ? O3 S1 C22 F1 -48.3(14) . . . . ? O2 S1 C22 F1 68.2(14) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.44 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.245 _refine_diff_density_min -1.766 _refine_diff_density_rms 0.173 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.321 0.250 212 94 ' ' 2 0.000 0.679 0.750 212 94 ' ' 3 0.500 0.821 0.250 212 95 ' ' 4 0.500 0.179 0.750 212 92 ' ' _platon_squeeze_details ; ; _iucr_refine_instructions_details ; TITL B11172a in Pbcn CELL 0.71073 12.6348 22.0849 19.8889 90.000 90.000 90.000 ZERR 4.00 0.0008 0.0013 0.0012 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, 0.5-Y, 0.5+Z SYMM -X, Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O F S PT Cl UNIT 180 192 32 24 24 8 8 8 TEMP -123.130 ACTA BOND $H CONF HTAB SIZE 0.200 0.072 0.065 L.S. 4 BOND FMAP 2 PLAN 20 WGHT 0.049300 34.813496 FVAR 0.47406 PT1 7 0.153296 0.045778 0.129979 11.00000 0.02226 0.03659 = 0.02431 0.00443 -0.00120 -0.00148 N1 3 0.106585 -0.028193 0.079135 11.00000 0.01688 0.05192 = 0.01632 0.00779 -0.00200 0.01042 N2 3 -0.008147 0.044793 0.149445 11.00000 0.01741 0.02862 = 0.01878 0.00198 -0.00230 0.00259 N3 3 -0.048685 0.088046 0.188725 11.00000 0.02944 0.03350 = 0.01917 -0.00390 -0.00926 0.00762 N4 3 -0.190440 0.123278 0.321522 11.00000 0.02457 0.03926 = 0.02549 -0.00971 -0.00490 -0.00033 C1 1 0.170604 -0.061000 0.040261 11.00000 0.02165 0.04546 = 0.03797 -0.00010 0.00701 -0.00039 AFIX 43 H1A 2 0.244318 -0.052522 0.040517 11.00000 -1.20000 AFIX 0 C2 1 0.133107 -0.106875 -0.000320 11.00000 0.04512 0.04273 = 0.02919 0.00069 0.01317 0.01265 AFIX 43 H2A 2 0.180423 -0.129538 -0.027610 11.00000 -1.20000 AFIX 0 C3 1 0.028195 -0.119269 -0.000860 11.00000 0.04359 0.02002 = 0.02747 -0.00178 0.00267 0.00363 AFIX 43 H3B 2 0.000590 -0.149942 -0.029390 11.00000 -1.20000 AFIX 0 C4 1 -0.037903 -0.086634 0.040686 11.00000 0.02337 0.03073 = 0.02824 0.00600 -0.00144 -0.00036 AFIX 43 H4B 2 -0.111766 -0.094680 0.040661 11.00000 -1.20000 AFIX 0 C5 1 0.002762 -0.042150 0.082499 11.00000 0.02975 0.02945 = 0.02120 0.00611 0.00188 0.00623 C6 1 -0.061848 -0.004880 0.130023 11.00000 0.02058 0.02494 = 0.02314 0.00403 -0.00768 0.00137 C7 1 -0.165361 -0.015674 0.154205 11.00000 0.02503 0.03074 = 0.01804 0.00324 -0.00622 0.00445 C8 1 -0.209636 0.028921 0.195017 11.00000 0.01961 0.03259 = 0.02164 0.00628 -0.00532 0.00660 C9 1 -0.147421 0.079627 0.211213 11.00000 0.01730 0.03494 = 0.01980 0.00170 -0.00035 -0.00008 C10 1 -0.183088 0.131266 0.254263 11.00000 0.02314 0.03953 = 0.01928 -0.00338 -0.00035 0.00432 C11 1 -0.207590 0.185614 0.224079 11.00000 0.03573 0.03261 = 0.04329 -0.00614 -0.00754 0.00902 AFIX 43 H11A 2 -0.204239 0.189684 0.176576 11.00000 -1.20000 AFIX 0 C12 1 -0.237486 0.234777 0.264220 11.00000 0.06748 0.02948 = 0.05825 -0.00713 -0.00745 0.00854 AFIX 43 H12A 2 -0.253404 0.272917 0.244582 11.00000 -1.20000 AFIX 0 C13 1 -0.243245 0.226843 0.331634 11.00000 0.06019 0.03324 = 0.04998 -0.01021 -0.00309 0.01163 AFIX 43 H13A 2 -0.264245 0.259610 0.359556 11.00000 -1.20000 AFIX 0 C14 1 -0.219055 0.171964 0.359976 11.00000 0.04728 0.05547 = 0.03417 -0.02018 0.00379 0.00717 AFIX 43 H14A 2 -0.222242 0.167645 0.407456 11.00000 -1.20000 AFIX 0 C15 1 -0.223715 -0.074265 0.141385 11.00000 0.02577 0.03379 = 0.01584 -0.00220 -0.00120 -0.00039 AFIX 23 H15A 2 -0.264774 -0.084774 0.182143 11.00000 -1.20000 H15B 2 -0.171048 -0.106806 0.134129 11.00000 -1.20000 AFIX 0 C16 1 -0.299853 -0.072962 0.080668 11.00000 0.02379 0.05022 = 0.03249 0.00050 -0.01090 0.00017 AFIX 23 H16A 2 -0.261420 -0.055683 0.041765 11.00000 -1.20000 H16B 2 -0.318524 -0.115230 0.069087 11.00000 -1.20000 AFIX 0 C17 1 -0.403393 -0.036926 0.090172 11.00000 0.05974 0.04902 = 0.03607 -0.01454 -0.02374 0.01410 AFIX 23 H17A 2 -0.450807 -0.045994 0.051844 11.00000 -1.20000 H17B 2 -0.438737 -0.051675 0.131468 11.00000 -1.20000 AFIX 0 C18 1 -0.391557 0.030332 0.095365 11.00000 0.02891 0.06100 = 0.01997 -0.00351 0.00306 -0.00023 AFIX 23 H18A 2 -0.447277 0.049455 0.067547 11.00000 -1.20000 H18B 2 -0.322367 0.041747 0.075741 11.00000 -1.20000 AFIX 0 C19 1 -0.398122 0.056975 0.166653 11.00000 0.01082 0.05203 = 0.03896 -0.00906 -0.00193 -0.00511 AFIX 23 H19A 2 -0.471943 0.053337 0.182844 11.00000 -1.20000 H19B 2 -0.380767 0.100643 0.164434 11.00000 -1.20000 AFIX 0 C20 1 -0.323683 0.026380 0.218502 11.00000 0.01754 0.04666 = 0.02825 -0.00709 -0.00019 0.00072 AFIX 23 H20A 2 -0.330192 0.047208 0.262385 11.00000 -1.20000 H20B 2 -0.345070 -0.016377 0.224742 11.00000 -1.20000 AFIX 0 C21 1 0.312988 0.038985 0.107235 11.00000 0.02047 0.05808 = 0.01877 -0.00126 0.00180 0.00135 AFIX 33 H21A 2 0.350001 0.075113 0.123534 11.00000 -1.50000 H21B 2 0.321900 0.035689 0.058425 11.00000 -1.50000 H21C 2 0.342550 0.002943 0.128995 11.00000 -1.50000 AFIX 0 S1 6 -0.136338 0.256712 0.563244 11.00000 0.04900 0.04756 = 0.03644 -0.00040 -0.00949 0.01351 O1 4 -0.145731 0.227441 0.500719 11.00000 0.09237 0.14346 = 0.05431 -0.05101 -0.03931 0.04762 O2 4 -0.199839 0.309421 0.573882 11.00000 0.07106 0.07489 = 0.05011 -0.00156 0.00213 0.04587 O3 4 -0.139229 0.216408 0.619299 11.00000 0.14602 0.05449 = 0.06345 0.01422 -0.01474 0.02724 C22 1 -0.000784 0.289014 0.566338 11.00000 0.07323 0.17416 = 0.11166 -0.08021 -0.01488 0.04196 F1 5 0.014551 0.307392 0.633947 11.00000 0.10537 0.12265 = 0.19304 -0.07304 -0.06623 0.02792 F2 5 0.067909 0.244294 0.555856 11.00000 0.04672 0.12512 = 0.34056 -0.12833 0.00243 0.01128 F3 5 0.015876 0.330494 0.527000 11.00000 0.13654 0.10788 = 0.31446 0.05122 0.11464 -0.00924 C23 1 0.000000 -0.171158 0.250000 10.50000 0.07272 0.03047 = 0.04979 0.00000 -0.03458 0.00000 AFIX 23 H23A 2 0.035053 -0.197565 0.283496 10.50000 -1.20000 H23B 2 -0.035054 -0.197563 0.216502 10.50000 -1.20000 AFIX 0 CL1 8 0.095723 -0.127365 0.209575 11.00000 0.09757 0.06279 = 0.05840 0.01958 -0.03298 -0.01314 HKLF 4 REM B11172a in Pbcn REM R1 = 0.0570 for 4322 Fo > 4sig(Fo) and 0.1051 for all 6960 data REM 321 parameters refined using 0 restraints END WGHT 0.0493 34.8290 REM Highest difference peak 2.245, deepest hole -1.766, 1-sigma level 0.173 Q1 1 -0.4611 -0.0465 0.1115 11.00000 0.05 2.25 Q2 1 0.1497 0.0068 0.1259 11.00000 0.05 1.81 Q3 1 0.1542 -0.0476 0.1097 11.00000 0.05 1.45 Q4 1 -0.1505 0.1011 0.3685 11.00000 0.05 1.07 Q5 1 -0.4666 0.0491 0.1282 11.00000 0.05 0.90 Q6 1 -0.1510 0.2225 0.3791 11.00000 0.05 0.79 Q7 1 0.3631 -0.1260 0.1670 11.00000 0.05 0.78 Q8 1 -0.0547 0.3274 0.4893 11.00000 0.05 0.77 Q9 1 0.2084 0.0500 0.1289 11.00000 0.05 0.76 Q10 1 -0.0193 0.2921 0.5241 11.00000 0.05 0.76 Q11 1 0.1616 0.0434 0.0626 11.00000 0.05 0.72 Q12 1 0.0362 0.3291 0.5378 11.00000 0.05 0.72 Q13 1 -0.1560 0.0916 0.3209 11.00000 0.05 0.66 Q14 1 0.1618 -0.0062 0.0779 11.00000 0.05 0.65 Q15 1 -0.1486 -0.0418 -0.0135 11.00000 0.05 0.65 Q16 1 0.0782 0.0278 0.1724 11.00000 0.05 0.64 Q17 1 0.2206 0.0536 0.1853 11.00000 0.05 0.61 Q18 1 0.1547 -0.1373 0.0730 11.00000 0.05 0.60 Q19 1 0.0791 0.0482 0.1803 11.00000 0.05 0.58 Q20 1 -0.3402 0.0562 0.1659 11.00000 0.05 0.57 ; #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 869547' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H38 N4 P Pt, C F3 O3 S' _chemical_formula_sum 'C40 H38 F3 N4 O3 P Pt S' _chemical_formula_weight 937.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8817(2) _cell_length_b 11.1700(2) _cell_length_c 18.5352(3) _cell_angle_alpha 83.1270(10) _cell_angle_beta 78.9850(10) _cell_angle_gamma 66.7850(10) _cell_volume 1843.37(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11312 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 30.61 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 3.966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8263 _exptl_absorpt_correction_T_max 0.8263 _exptl_absorpt_process_details 'SADABS (Bruker, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45958 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 30.61 _reflns_number_total 11312 _reflns_number_gt 10178 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+0.2627P] 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 11312 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0472 _refine_ls_wR_factor_gt 0.0459 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.005 _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 0.680629(8) 0.742813(7) 0.707753(4) 0.01732(2) Uani 1 1 d . . . N1 N 0.74397(17) 0.81091(16) 0.79090(9) 0.0187(3) Uani 1 1 d . . . N2 N 0.54938(17) 0.70046(15) 0.80209(8) 0.0168(3) Uani 1 1 d . . . N3 N 0.44987(17) 0.65063(16) 0.79695(8) 0.0175(3) Uani 1 1 d . . . N4 N 0.1993(2) 0.52040(18) 0.89966(9) 0.0251(4) Uani 1 1 d . . . C1 C 0.8504(2) 0.8598(2) 0.78228(12) 0.0255(4) Uani 1 1 d . . . H1A H 0.8932 0.8770 0.7337 0.031 Uiso 1 1 calc R . . C2 C 0.9010(2) 0.8865(2) 0.84086(13) 0.0300(5) Uani 1 1 d . . . H2A H 0.9733 0.9249 0.8328 0.036 Uiso 1 1 calc R . . C3 C 0.8437(2) 0.8560(2) 0.91106(12) 0.0288(5) Uani 1 1 d . . . H3B H 0.8796 0.8689 0.9523 0.035 Uiso 1 1 calc R . . C4 C 0.7331(2) 0.8064(2) 0.92078(12) 0.0255(4) Uani 1 1 d . . . H4B H 0.6938 0.7837 0.9689 0.031 Uiso 1 1 calc R . . C5 C 0.6791(2) 0.78954(19) 0.86012(10) 0.0188(4) Uani 1 1 d . . . C6 C 0.5533(2) 0.74707(18) 0.86506(10) 0.0167(3) Uani 1 1 d . . . C7 C 0.4365(2) 0.76496(18) 0.92521(10) 0.0167(3) Uani 1 1 d . . . C8 C 0.3322(2) 0.71093(18) 0.92123(10) 0.0172(3) Uani 1 1 d . . . C9 C 0.3486(2) 0.64919(18) 0.85612(10) 0.0168(3) Uani 1 1 d . . . C10 C 0.2458(2) 0.58897(18) 0.84285(10) 0.0180(3) Uani 1 1 d . . . C11 C 0.1994(2) 0.6071(2) 0.77500(11) 0.0231(4) Uani 1 1 d . . . H11A H 0.2374 0.6532 0.7353 0.028 Uiso 1 1 calc R . . C12 C 0.0965(2) 0.5565(2) 0.76635(12) 0.0272(4) Uani 1 1 d . . . H12A H 0.0616 0.5687 0.7206 0.033 Uiso 1 1 calc R . . C13 C 0.0451(2) 0.4885(2) 0.82435(12) 0.0272(4) Uani 1 1 d . . . H13A H -0.0267 0.4541 0.8199 0.033 Uiso 1 1 calc R . . C14 C 0.1012(3) 0.4716(2) 0.88944(12) 0.0285(4) Uani 1 1 d . . . H14A H 0.0680 0.4226 0.9291 0.034 Uiso 1 1 calc R . . C15 C 0.4111(2) 0.8548(2) 0.98527(10) 0.0222(4) Uani 1 1 d . . . H15A H 0.3034 0.9101 0.9940 0.027 Uiso 1 1 calc R . . H15B H 0.4647 0.9134 0.9663 0.027 Uiso 1 1 calc R . . C16 C 0.4573(3) 0.7947(3) 1.06017(11) 0.0335(5) Uani 1 1 d . . . H16A H 0.5579 0.7251 1.0510 0.040 Uiso 1 1 calc R . . H16B H 0.4656 0.8629 1.0865 0.040 Uiso 1 1 calc R . . C17 C 0.3556(3) 0.7367(3) 1.11129(12) 0.0349(5) Uani 1 1 d . . . H17A H 0.3868 0.7178 1.1605 0.042 Uiso 1 1 calc R . . H17B H 0.2524 0.8029 1.1168 0.042 Uiso 1 1 calc R . . C18 C 0.3555(3) 0.6127(2) 1.08542(12) 0.0305(5) Uani 1 1 d . . . H18A H 0.3546 0.5515 1.1287 0.037 Uiso 1 1 calc R . . H18B H 0.4498 0.5714 1.0516 0.037 Uiso 1 1 calc R . . C19 C 0.2259(2) 0.6301(2) 1.04634(11) 0.0262(4) Uani 1 1 d . . . H19A H 0.1336 0.6558 1.0830 0.031 Uiso 1 1 calc R . . H19B H 0.2424 0.5444 1.0289 0.031 Uiso 1 1 calc R . . C20 C 0.1996(2) 0.7299(2) 0.98073(10) 0.0205(4) Uani 1 1 d . . . H20A H 0.1175 0.7270 0.9586 0.025 Uiso 1 1 calc R . . H20B H 0.1661 0.8181 0.9994 0.025 Uiso 1 1 calc R . . C21 C 0.8150(3) 0.8036(3) 0.62654(12) 0.0375(6) Uani 1 1 d . . . H21A H 0.8676 0.8445 0.6486 0.056 Uiso 1 1 calc R . . H21B H 0.7539 0.8669 0.5927 0.056 Uiso 1 1 calc R . . H21C H 0.8877 0.7285 0.5995 0.056 Uiso 1 1 calc R . . P1 P 0.59958(5) 0.66436(5) 0.62677(3) 0.01752(9) Uani 1 1 d . . . C22 C 0.6213(2) 0.49545(19) 0.65023(10) 0.0196(4) Uani 1 1 d . . . C23 C 0.7457(2) 0.4149(2) 0.68179(11) 0.0249(4) Uani 1 1 d . . . H23A H 0.8106 0.4506 0.6942 0.030 Uiso 1 1 calc R . . C24 C 0.7755(3) 0.2826(2) 0.69521(12) 0.0306(5) Uani 1 1 d . . . H24A H 0.8615 0.2277 0.7158 0.037 Uiso 1 1 calc R . . C25 C 0.6797(3) 0.2313(2) 0.67851(13) 0.0329(5) Uani 1 1 d . . . H25A H 0.6996 0.1410 0.6881 0.040 Uiso 1 1 calc R . . C26 C 0.5557(3) 0.3100(2) 0.64813(13) 0.0329(5) Uani 1 1 d . . . H26A H 0.4904 0.2738 0.6368 0.039 Uiso 1 1 calc R . . C27 C 0.5253(2) 0.4424(2) 0.63384(11) 0.0259(4) Uani 1 1 d . . . H27A H 0.4393 0.4966 0.6130 0.031 Uiso 1 1 calc R . . C28 C 0.6910(2) 0.6599(2) 0.53124(10) 0.0215(4) Uani 1 1 d . . . C29 C 0.7932(3) 0.5463(2) 0.49974(11) 0.0311(5) Uani 1 1 d . . . H29A H 0.8140 0.4653 0.5272 0.037 Uiso 1 1 calc R . . C30 C 0.8656(3) 0.5508(3) 0.42757(13) 0.0441(7) Uani 1 1 d . . . H30A H 0.9351 0.4725 0.4060 0.053 Uiso 1 1 calc R . . C31 C 0.8373(3) 0.6670(3) 0.38753(12) 0.0412(6) Uani 1 1 d . . . H31A H 0.8870 0.6691 0.3384 0.049 Uiso 1 1 calc R . . C32 C 0.7374(3) 0.7800(3) 0.41851(12) 0.0365(6) Uani 1 1 d . . . H32A H 0.7184 0.8606 0.3908 0.044 Uiso 1 1 calc R . . C33 C 0.6635(3) 0.7781(2) 0.49011(11) 0.0287(5) Uani 1 1 d . . . H33A H 0.5943 0.8571 0.5111 0.034 Uiso 1 1 calc R . . C34 C 0.4060(2) 0.7602(2) 0.61643(10) 0.0206(4) Uani 1 1 d . . . C35 C 0.3168(2) 0.8559(2) 0.66533(11) 0.0225(4) Uani 1 1 d . . . H35A H 0.3553 0.8677 0.7060 0.027 Uiso 1 1 calc R . . C36 C 0.1712(2) 0.9350(2) 0.65541(13) 0.0288(5) Uani 1 1 d . . . H36A H 0.1108 1.0000 0.6893 0.035 Uiso 1 1 calc R . . C37 C 0.1147(3) 0.9185(2) 0.59593(14) 0.0337(5) Uani 1 1 d . . . H37A H 0.0160 0.9731 0.5887 0.040 Uiso 1 1 calc R . . C38 C 0.2022(3) 0.8224(3) 0.54725(14) 0.0358(5) Uani 1 1 d . . . H38A H 0.1624 0.8102 0.5072 0.043 Uiso 1 1 calc R . . C39 C 0.3475(2) 0.7438(2) 0.55641(12) 0.0289(5) Uani 1 1 d . . . H39A H 0.4074 0.6792 0.5222 0.035 Uiso 1 1 calc R . . S1 S 0.16419(6) 1.10678(5) 0.83934(3) 0.02372(10) Uani 1 1 d . . . O1 O 0.1439(2) 1.14753(18) 0.91264(9) 0.0380(4) Uani 1 1 d . . . O2 O 0.06039(18) 1.19410(17) 0.79357(10) 0.0364(4) Uani 1 1 d . . . O3 O 0.19570(18) 0.97046(15) 0.83363(9) 0.0333(4) Uani 1 1 d . . . C40 C 0.3404(2) 1.1208(2) 0.79703(11) 0.0230(4) Uani 1 1 d . . . F1 F 0.45213(14) 1.04000(13) 0.83151(8) 0.0347(3) Uani 1 1 d . . . F2 F 0.33736(15) 1.24011(12) 0.79859(8) 0.0374(3) Uani 1 1 d . . . F3 F 0.37804(17) 1.08825(16) 0.72700(7) 0.0412(3) 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 Pt1 0.01792(4) 0.02252(4) 0.01510(3) -0.00279(2) -0.00203(2) -0.01121(3) N1 0.0162(7) 0.0195(8) 0.0208(8) -0.0056(6) -0.0042(6) -0.0053(6) N2 0.0185(7) 0.0178(8) 0.0153(7) -0.0023(6) -0.0036(6) -0.0074(6) N3 0.0179(7) 0.0188(8) 0.0168(7) -0.0003(6) -0.0038(6) -0.0077(6) N4 0.0276(9) 0.0283(9) 0.0230(8) 0.0016(7) -0.0030(7) -0.0157(8) C1 0.0211(9) 0.0290(11) 0.0302(10) -0.0071(8) -0.0022(8) -0.0128(9) C2 0.0207(10) 0.0342(12) 0.0402(12) -0.0149(10) -0.0040(9) -0.0124(9) C3 0.0215(10) 0.0335(12) 0.0327(11) -0.0134(9) -0.0109(8) -0.0053(9) C4 0.0218(9) 0.0312(11) 0.0235(10) -0.0073(8) -0.0072(8) -0.0068(9) C5 0.0162(8) 0.0199(9) 0.0198(9) -0.0052(7) -0.0044(7) -0.0045(7) C6 0.0176(8) 0.0168(9) 0.0160(8) -0.0003(6) -0.0063(6) -0.0053(7) C7 0.0179(8) 0.0163(8) 0.0140(8) 0.0004(6) -0.0055(6) -0.0035(7) C8 0.0159(8) 0.0163(9) 0.0159(8) 0.0020(7) -0.0036(6) -0.0028(7) C9 0.0158(8) 0.0158(8) 0.0175(8) 0.0004(6) -0.0045(6) -0.0040(7) C10 0.0169(8) 0.0166(9) 0.0196(8) -0.0033(7) -0.0006(7) -0.0057(7) C11 0.0281(10) 0.0246(10) 0.0202(9) 0.0000(7) -0.0050(8) -0.0135(9) C12 0.0325(11) 0.0281(11) 0.0269(10) -0.0032(8) -0.0092(9) -0.0153(9) C13 0.0263(10) 0.0273(11) 0.0337(11) -0.0066(9) -0.0038(9) -0.0151(9) C14 0.0332(11) 0.0307(11) 0.0277(10) -0.0008(9) -0.0010(9) -0.0204(10) C15 0.0258(10) 0.0227(10) 0.0190(9) -0.0053(7) -0.0039(7) -0.0087(8) C16 0.0440(13) 0.0491(14) 0.0160(9) -0.0031(9) -0.0065(9) -0.0256(12) C17 0.0456(14) 0.0451(14) 0.0156(9) 0.0004(9) -0.0058(9) -0.0189(12) C18 0.0344(12) 0.0311(12) 0.0213(10) 0.0066(8) -0.0067(8) -0.0086(10) C19 0.0291(10) 0.0294(11) 0.0181(9) 0.0012(8) 0.0006(8) -0.0114(9) C20 0.0171(8) 0.0224(10) 0.0183(8) -0.0027(7) -0.0004(7) -0.0043(8) C21 0.0451(14) 0.0626(17) 0.0231(10) -0.0028(10) -0.0002(9) -0.0419(13) P1 0.0189(2) 0.0220(2) 0.0139(2) -0.00229(17) -0.00214(17) -0.00990(19) C22 0.0225(9) 0.0245(10) 0.0134(8) -0.0040(7) -0.0001(7) -0.0110(8) C23 0.0243(10) 0.0302(11) 0.0223(9) -0.0012(8) -0.0054(8) -0.0120(9) C24 0.0332(11) 0.0271(11) 0.0280(11) 0.0023(9) -0.0065(9) -0.0080(9) C25 0.0485(14) 0.0237(11) 0.0291(11) 0.0000(9) -0.0051(10) -0.0173(10) C26 0.0423(13) 0.0348(13) 0.0312(11) -0.0038(9) -0.0051(10) -0.0245(11) C27 0.0279(10) 0.0302(11) 0.0247(10) -0.0021(8) -0.0057(8) -0.0154(9) C28 0.0219(9) 0.0308(11) 0.0155(8) -0.0016(7) -0.0033(7) -0.0139(8) C29 0.0312(11) 0.0378(13) 0.0190(9) -0.0017(9) -0.0017(8) -0.0085(10) C30 0.0381(13) 0.0572(17) 0.0219(11) -0.0061(11) 0.0025(10) -0.0045(13) C31 0.0351(13) 0.074(2) 0.0173(10) 0.0028(11) -0.0010(9) -0.0260(13) C32 0.0452(14) 0.0529(16) 0.0241(11) 0.0118(10) -0.0102(10) -0.0340(13) C33 0.0390(12) 0.0307(11) 0.0222(10) 0.0012(8) -0.0066(9) -0.0192(10) C34 0.0209(9) 0.0239(10) 0.0199(9) 0.0000(7) -0.0040(7) -0.0115(8) C35 0.0243(9) 0.0227(10) 0.0226(9) 0.0002(8) -0.0041(8) -0.0115(8) C36 0.0223(10) 0.0257(11) 0.0360(12) 0.0031(9) -0.0014(8) -0.0093(9) C37 0.0224(10) 0.0358(13) 0.0439(13) 0.0081(10) -0.0102(9) -0.0129(10) C38 0.0335(12) 0.0476(15) 0.0337(12) 0.0028(11) -0.0157(10) -0.0198(11) C39 0.0294(11) 0.0368(12) 0.0247(10) -0.0028(9) -0.0088(8) -0.0148(10) S1 0.0230(2) 0.0229(2) 0.0260(2) 0.00060(19) -0.00603(19) -0.0089(2) O1 0.0409(10) 0.0416(10) 0.0272(8) -0.0077(7) 0.0021(7) -0.0129(8) O2 0.0285(8) 0.0340(9) 0.0485(10) 0.0061(8) -0.0192(7) -0.0101(7) O3 0.0347(9) 0.0239(8) 0.0448(10) 0.0020(7) -0.0092(7) -0.0145(7) C40 0.0245(10) 0.0212(10) 0.0236(9) -0.0016(7) -0.0071(8) -0.0076(8) F1 0.0259(6) 0.0319(7) 0.0454(8) 0.0020(6) -0.0162(6) -0.0063(6) F2 0.0333(7) 0.0238(7) 0.0576(9) -0.0031(6) -0.0049(6) -0.0141(6) F3 0.0513(9) 0.0584(10) 0.0222(6) -0.0071(6) 0.0011(6) -0.0313(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C21 2.047(2) . ? Pt1 N1 2.0905(16) . ? Pt1 N2 2.0934(15) . ? Pt1 P1 2.2339(5) . ? N1 C1 1.341(3) . ? N1 C5 1.359(2) . ? N2 N3 1.329(2) . ? N2 C6 1.347(2) . ? N3 C9 1.339(2) . ? N4 C14 1.335(3) . ? N4 C10 1.344(2) . ? C1 C2 1.385(3) . ? C1 H1A 0.9500 . ? C2 C3 1.376(3) . ? C2 H2A 0.9500 . ? C3 C4 1.383(3) . ? C3 H3B 0.9500 . ? C4 C5 1.394(3) . ? C4 H4B 0.9500 . ? C5 C6 1.480(3) . ? C6 C7 1.412(3) . ? C7 C8 1.400(3) . ? C7 C15 1.507(3) . ? C8 C9 1.412(3) . ? C8 C20 1.505(3) . ? C9 C10 1.490(3) . ? C10 C11 1.385(3) . ? C11 C12 1.385(3) . ? C11 H11A 0.9500 . ? C12 C13 1.375(3) . ? C12 H12A 0.9500 . ? C13 C14 1.384(3) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.537(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.526(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.520(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.525(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.535(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? P1 C22 1.821(2) . ? P1 C34 1.822(2) . ? P1 C28 1.824(2) . ? C22 C23 1.393(3) . ? C22 C27 1.393(3) . ? C23 C24 1.388(3) . ? C23 H23A 0.9500 . ? C24 C25 1.379(3) . ? C24 H24A 0.9500 . ? C25 C26 1.373(3) . ? C25 H25A 0.9500 . ? C26 C27 1.391(3) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C29 1.383(3) . ? C28 C33 1.398(3) . ? C29 C30 1.397(3) . ? C29 H29A 0.9500 . ? C30 C31 1.370(4) . ? C30 H30A 0.9500 . ? C31 C32 1.368(4) . ? C31 H31A 0.9500 . ? C32 C33 1.389(3) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 C35 1.388(3) . ? C34 C39 1.408(3) . ? C35 C36 1.394(3) . ? C35 H35A 0.9500 . ? C36 C37 1.388(3) . ? C36 H36A 0.9500 . ? C37 C38 1.384(4) . ? C37 H37A 0.9500 . ? C38 C39 1.388(3) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? S1 O1 1.4371(17) . ? S1 O2 1.4384(16) . ? S1 O3 1.4418(17) . ? S1 C40 1.827(2) . ? C40 F2 1.324(2) . ? C40 F3 1.333(2) . ? C40 F1 1.337(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Pt1 N1 92.78(8) . . ? C21 Pt1 N2 170.39(8) . . ? N1 Pt1 N2 77.91(6) . . ? C21 Pt1 P1 92.33(7) . . ? N1 Pt1 P1 174.88(5) . . ? N2 Pt1 P1 96.98(4) . . ? C1 N1 C5 118.91(17) . . ? C1 N1 Pt1 126.17(14) . . ? C5 N1 Pt1 114.55(12) . . ? N3 N2 C6 122.17(15) . . ? N3 N2 Pt1 120.79(11) . . ? C6 N2 Pt1 116.05(12) . . ? N2 N3 C9 118.66(16) . . ? C14 N4 C10 117.35(18) . . ? N1 C1 C2 123.1(2) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C3 C2 C1 118.3(2) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C2 C3 C4 119.17(19) . . ? C2 C3 H3B 120.4 . . ? C4 C3 H3B 120.4 . . ? C3 C4 C5 120.2(2) . . ? C3 C4 H4B 119.9 . . ? C5 C4 H4B 119.9 . . ? N1 C5 C4 120.00(18) . . ? N1 C5 C6 115.74(16) . . ? C4 C5 C6 124.26(18) . . ? N2 C6 C7 120.85(17) . . ? N2 C6 C5 113.27(16) . . ? C7 C6 C5 125.51(17) . . ? C8 C7 C6 116.88(17) . . ? C8 C7 C15 120.85(17) . . ? C6 C7 C15 121.62(17) . . ? C7 C8 C9 117.34(16) . . ? C7 C8 C20 121.04(17) . . ? C9 C8 C20 121.34(17) . . ? N3 C9 C8 122.89(17) . . ? N3 C9 C10 112.89(16) . . ? C8 C9 C10 123.89(16) . . ? N4 C10 C11 122.83(18) . . ? N4 C10 C9 116.93(16) . . ? C11 C10 C9 120.23(17) . . ? C12 C11 C10 118.41(18) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? C13 C12 C11 119.58(19) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C12 C13 C14 117.98(19) . . ? C12 C13 H13A 121.0 . . ? C14 C13 H13A 121.0 . . ? N4 C14 C13 123.79(19) . . ? N4 C14 H14A 118.1 . . ? C13 C14 H14A 118.1 . . ? C7 C15 C16 118.64(18) . . ? C7 C15 H15A 107.7 . . ? C16 C15 H15A 107.7 . . ? C7 C15 H15B 107.7 . . ? C16 C15 H15B 107.7 . . ? H15A C15 H15B 107.1 . . ? C17 C16 C15 117.26(19) . . ? C17 C16 H16A 108.0 . . ? C15 C16 H16A 108.0 . . ? C17 C16 H16B 108.0 . . ? C15 C16 H16B 108.0 . . ? H16A C16 H16B 107.2 . . ? C18 C17 C16 114.6(2) . . ? C18 C17 H17A 108.6 . . ? C16 C17 H17A 108.6 . . ? C18 C17 H17B 108.6 . . ? C16 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? C17 C18 C19 115.69(19) . . ? C17 C18 H18A 108.4 . . ? C19 C18 H18A 108.4 . . ? C17 C18 H18B 108.4 . . ? C19 C18 H18B 108.4 . . ? H18A C18 H18B 107.4 . . ? C18 C19 C20 116.84(18) . . ? C18 C19 H19A 108.1 . . ? C20 C19 H19A 108.1 . . ? C18 C19 H19B 108.1 . . ? C20 C19 H19B 108.1 . . ? H19A C19 H19B 107.3 . . ? C8 C20 C19 115.52(16) . . ? C8 C20 H20A 108.4 . . ? C19 C20 H20A 108.4 . . ? C8 C20 H20B 108.4 . . ? C19 C20 H20B 108.4 . . ? H20A C20 H20B 107.5 . . ? Pt1 C21 H21A 109.5 . . ? Pt1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Pt1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 P1 C34 108.78(9) . . ? C22 P1 C28 103.20(9) . . ? C34 P1 C28 101.03(9) . . ? C22 P1 Pt1 111.86(6) . . ? C34 P1 Pt1 113.32(7) . . ? C28 P1 Pt1 117.59(7) . . ? C23 C22 C27 119.23(19) . . ? C23 C22 P1 117.59(15) . . ? C27 C22 P1 123.05(15) . . ? C24 C23 C22 120.4(2) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C25 C24 C23 119.8(2) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C26 C25 C24 120.4(2) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C25 C26 C27 120.4(2) . . ? C25 C26 H26A 119.8 . . ? C27 C26 H26A 119.8 . . ? C26 C27 C22 119.8(2) . . ? C26 C27 H27A 120.1 . . ? C22 C27 H27A 120.1 . . ? C29 C28 C33 118.99(19) . . ? C29 C28 P1 122.81(16) . . ? C33 C28 P1 118.05(17) . . ? C28 C29 C30 119.9(2) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 120.7(3) . . ? C31 C30 H30A 119.6 . . ? C29 C30 H30A 119.6 . . ? C32 C31 C30 119.7(2) . . ? C32 C31 H31A 120.1 . . ? C30 C31 H31A 120.1 . . ? C31 C32 C33 120.7(2) . . ? C31 C32 H32A 119.6 . . ? C33 C32 H32A 119.6 . . ? C32 C33 C28 119.9(2) . . ? C32 C33 H33A 120.0 . . ? C28 C33 H33A 120.0 . . ? C35 C34 C39 119.07(19) . . ? C35 C34 P1 120.19(15) . . ? C39 C34 P1 120.63(16) . . ? C34 C35 C36 120.67(19) . . ? C34 C35 H35A 119.7 . . ? C36 C35 H35A 119.7 . . ? C37 C36 C35 119.9(2) . . ? C37 C36 H36A 120.1 . . ? C35 C36 H36A 120.1 . . ? C38 C37 C36 119.9(2) . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C37 C38 C39 120.6(2) . . ? C37 C38 H38A 119.7 . . ? C39 C38 H38A 119.7 . . ? C38 C39 C34 119.9(2) . . ? C38 C39 H39A 120.1 . . ? C34 C39 H39A 120.1 . . ? O1 S1 O2 115.37(11) . . ? O1 S1 O3 115.49(10) . . ? O2 S1 O3 114.70(10) . . ? O1 S1 C40 102.73(10) . . ? O2 S1 C40 103.15(10) . . ? O3 S1 C40 102.73(10) . . ? F2 C40 F3 107.56(17) . . ? F2 C40 F1 107.29(16) . . ? F3 C40 F1 106.21(17) . . ? F2 C40 S1 112.75(14) . . ? F3 C40 S1 111.78(14) . . ? F1 C40 S1 110.91(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Pt1 N1 C1 -6.47(18) . . . . ? N2 Pt1 N1 C1 175.93(17) . . . . ? P1 Pt1 N1 C1 174.4(4) . . . . ? C21 Pt1 N1 C5 -179.43(15) . . . . ? N2 Pt1 N1 C5 2.97(13) . . . . ? P1 Pt1 N1 C5 1.4(6) . . . . ? C21 Pt1 N2 N3 161.6(5) . . . . ? N1 Pt1 N2 N3 176.10(15) . . . . ? P1 Pt1 N2 N3 -4.04(14) . . . . ? C21 Pt1 N2 C6 -7.3(6) . . . . ? N1 Pt1 N2 C6 7.25(13) . . . . ? P1 Pt1 N2 C6 -172.89(12) . . . . ? C6 N2 N3 C9 1.3(3) . . . . ? Pt1 N2 N3 C9 -166.87(12) . . . . ? C5 N1 C1 C2 1.9(3) . . . . ? Pt1 N1 C1 C2 -170.82(16) . . . . ? N1 C1 C2 C3 2.9(3) . . . . ? C1 C2 C3 C4 -3.2(3) . . . . ? C2 C3 C4 C5 -1.0(3) . . . . ? C1 N1 C5 C4 -6.2(3) . . . . ? Pt1 N1 C5 C4 167.32(15) . . . . ? C1 N1 C5 C6 174.57(17) . . . . ? Pt1 N1 C5 C6 -11.9(2) . . . . ? C3 C4 C5 N1 5.8(3) . . . . ? C3 C4 C5 C6 -175.00(19) . . . . ? N3 N2 C6 C7 -10.6(3) . . . . ? Pt1 N2 C6 C7 158.10(13) . . . . ? N3 N2 C6 C5 176.03(15) . . . . ? Pt1 N2 C6 C5 -15.3(2) . . . . ? N1 C5 C6 N2 18.0(2) . . . . ? C4 C5 C6 N2 -161.21(18) . . . . ? N1 C5 C6 C7 -155.03(17) . . . . ? C4 C5 C6 C7 25.8(3) . . . . ? N2 C6 C7 C8 11.1(3) . . . . ? C5 C6 C7 C8 -176.35(17) . . . . ? N2 C6 C7 C15 -159.75(17) . . . . ? C5 C6 C7 C15 12.8(3) . . . . ? C6 C7 C8 C9 -3.1(2) . . . . ? C15 C7 C8 C9 167.87(16) . . . . ? C6 C7 C8 C20 -177.08(16) . . . . ? C15 C7 C8 C20 -6.1(3) . . . . ? N2 N3 C9 C8 7.1(3) . . . . ? N2 N3 C9 C10 -179.17(15) . . . . ? C7 C8 C9 N3 -6.0(3) . . . . ? C20 C8 C9 N3 168.00(17) . . . . ? C7 C8 C9 C10 -178.98(16) . . . . ? C20 C8 C9 C10 -5.0(3) . . . . ? C14 N4 C10 C11 -1.8(3) . . . . ? C14 N4 C10 C9 176.69(19) . . . . ? N3 C9 C10 N4 145.26(17) . . . . ? C8 C9 C10 N4 -41.1(3) . . . . ? N3 C9 C10 C11 -36.2(2) . . . . ? C8 C9 C10 C11 137.4(2) . . . . ? N4 C10 C11 C12 2.5(3) . . . . ? C9 C10 C11 C12 -175.97(19) . . . . ? C10 C11 C12 C13 -1.0(3) . . . . ? C11 C12 C13 C14 -1.0(3) . . . . ? C10 N4 C14 C13 -0.4(3) . . . . ? C12 C13 C14 N4 1.8(4) . . . . ? C8 C7 C15 C16 84.6(2) . . . . ? C6 C7 C15 C16 -104.9(2) . . . . ? C7 C15 C16 C17 -76.7(3) . . . . ? C15 C16 C17 C18 69.5(3) . . . . ? C16 C17 C18 C19 -98.7(2) . . . . ? C17 C18 C19 C20 53.6(3) . . . . ? C7 C8 C20 C19 -86.8(2) . . . . ? C9 C8 C20 C19 99.5(2) . . . . ? C18 C19 C20 C8 54.3(3) . . . . ? C21 Pt1 P1 C22 127.41(11) . . . . ? N1 Pt1 P1 C22 -53.5(5) . . . . ? N2 Pt1 P1 C22 -54.96(8) . . . . ? C21 Pt1 P1 C34 -109.16(11) . . . . ? N1 Pt1 P1 C34 70.0(5) . . . . ? N2 Pt1 P1 C34 68.46(8) . . . . ? C21 Pt1 P1 C28 8.24(11) . . . . ? N1 Pt1 P1 C28 -172.6(5) . . . . ? N2 Pt1 P1 C28 -174.13(9) . . . . ? C34 P1 C22 C23 -161.11(15) . . . . ? C28 P1 C22 C23 92.19(16) . . . . ? Pt1 P1 C22 C23 -35.16(17) . . . . ? C34 P1 C22 C27 23.06(19) . . . . ? C28 P1 C22 C27 -83.64(18) . . . . ? Pt1 P1 C22 C27 149.01(15) . . . . ? C27 C22 C23 C24 1.5(3) . . . . ? P1 C22 C23 C24 -174.54(17) . . . . ? C22 C23 C24 C25 -1.3(3) . . . . ? C23 C24 C25 C26 0.5(4) . . . . ? C24 C25 C26 C27 0.0(4) . . . . ? C25 C26 C27 C22 0.2(3) . . . . ? C23 C22 C27 C26 -0.9(3) . . . . ? P1 C22 C27 C26 174.85(17) . . . . ? C22 P1 C28 C29 -19.9(2) . . . . ? C34 P1 C28 C29 -132.42(18) . . . . ? Pt1 P1 C28 C29 103.73(18) . . . . ? C22 P1 C28 C33 164.48(16) . . . . ? C34 P1 C28 C33 51.98(18) . . . . ? Pt1 P1 C28 C33 -71.86(17) . . . . ? C33 C28 C29 C30 -0.8(3) . . . . ? P1 C28 C29 C30 -176.31(19) . . . . ? C28 C29 C30 C31 0.4(4) . . . . ? C29 C30 C31 C32 0.1(4) . . . . ? C30 C31 C32 C33 -0.4(4) . . . . ? C31 C32 C33 C28 0.0(3) . . . . ? C29 C28 C33 C32 0.5(3) . . . . ? P1 C28 C33 C32 176.30(17) . . . . ? C22 P1 C34 C35 114.07(16) . . . . ? C28 P1 C34 C35 -137.75(16) . . . . ? Pt1 P1 C34 C35 -11.03(18) . . . . ? C22 P1 C34 C39 -69.88(18) . . . . ? C28 P1 C34 C39 38.31(19) . . . . ? Pt1 P1 C34 C39 165.02(15) . . . . ? C39 C34 C35 C36 0.1(3) . . . . ? P1 C34 C35 C36 176.17(15) . . . . ? C34 C35 C36 C37 -0.3(3) . . . . ? C35 C36 C37 C38 0.9(3) . . . . ? C36 C37 C38 C39 -1.3(4) . . . . ? C37 C38 C39 C34 1.1(3) . . . . ? C35 C34 C39 C38 -0.5(3) . . . . ? P1 C34 C39 C38 -176.58(17) . . . . ? O1 S1 C40 F2 -57.79(16) . . . . ? O2 S1 C40 F2 62.47(16) . . . . ? O3 S1 C40 F2 -178.01(14) . . . . ? O1 S1 C40 F3 -179.11(15) . . . . ? O2 S1 C40 F3 -58.86(17) . . . . ? O3 S1 C40 F3 60.67(16) . . . . ? O1 S1 C40 F1 62.56(16) . . . . ? O2 S1 C40 F1 -177.19(15) . . . . ? O3 S1 C40 F1 -57.66(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.61 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.972 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.089 data_6-dppd _database_code_depnum_ccdc_archive 'CCDC 892425' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 N4' _chemical_formula_sum 'C20 H20 N4' _chemical_formula_weight 316.40 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0827(14) _cell_length_b 7.2540(15) _cell_length_c 16.885(3) _cell_angle_alpha 97.29(3) _cell_angle_beta 98.24(3) _cell_angle_gamma 100.83(3) _cell_volume 832.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9670 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 39.59 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9661 _exptl_absorpt_correction_T_max 0.9939 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; Addition of H202 to PtMe2(6-dppd) resulted in loss of ligand ; _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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16546 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0795 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 39.59 _reflns_number_total 9670 _reflns_number_gt 5569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0909P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9670 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1225 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1787 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 C1 C -0.22805(18) 1.03209(17) 0.44482(7) 0.0301(2) Uani 1 1 d . . . H1 H -0.172(2) 1.032(2) 0.5033(10) 0.045(4) Uiso 1 1 d . . . C2 C -0.39409(18) 1.10382(16) 0.42330(7) 0.0293(2) Uani 1 1 d . . . H2 H -0.464(2) 1.160(2) 0.4651(10) 0.045(4) Uiso 1 1 d . . . C3 C -0.46554(17) 1.09555(16) 0.34090(7) 0.0279(2) Uani 1 1 d . . . H3 H -0.590(3) 1.135(2) 0.3230(10) 0.050(5) Uiso 1 1 d . . . C4 C -0.36520(15) 1.02147(15) 0.28309(6) 0.02374(19) Uani 1 1 d . . . H4 H -0.409(2) 1.011(2) 0.2232(9) 0.030(4) Uiso 1 1 d . . . C5 C -0.19743(14) 0.95529(13) 0.31029(6) 0.01993(17) Uani 1 1 d . . . C6 C -0.07753(13) 0.88547(13) 0.25080(6) 0.01925(17) Uani 1 1 d . . . C7 C -0.02310(13) 0.70576(13) 0.24759(5) 0.01786(16) Uani 1 1 d . . . C8 C 0.09835(13) 0.66715(13) 0.19110(5) 0.01784(16) Uani 1 1 d . . . C9 C 0.14654(13) 0.80614(13) 0.14032(6) 0.01893(16) Uani 1 1 d . . . C10 C 0.26621(14) 0.78118(13) 0.07419(6) 0.01949(17) Uani 1 1 d . . . C11 C 0.19209(15) 0.80064(15) -0.00573(6) 0.02425(19) Uani 1 1 d . . . H11 H 0.060(2) 0.832(2) -0.0173(9) 0.034(4) Uiso 1 1 d . . . C12 C 0.30943(17) 0.78465(16) -0.06551(6) 0.0276(2) Uani 1 1 d . . . H12 H 0.260(2) 0.801(2) -0.1222(9) 0.032(4) Uiso 1 1 d . . . C13 C 0.49625(17) 0.75192(16) -0.04360(7) 0.0275(2) Uani 1 1 d . . . H13 H 0.591(2) 0.744(2) -0.0825(10) 0.049(5) Uiso 1 1 d . . . C14 C 0.55770(16) 0.73467(16) 0.03769(7) 0.0262(2) Uani 1 1 d . . . H14 H 0.692(2) 0.713(2) 0.0547(10) 0.041(4) Uiso 1 1 d . . . C15 C -0.10936(14) 0.55953(14) 0.29746(6) 0.02136(18) Uani 1 1 d . . . H15A H -0.237(2) 0.5927(19) 0.3101(8) 0.027(3) Uiso 1 1 d . . . H15B H -0.1495(18) 0.4344(19) 0.2627(8) 0.022(3) Uiso 1 1 d . . . C16 C 0.01786(16) 0.53668(16) 0.37700(6) 0.0248(2) Uani 1 1 d . . . H16A H -0.078(2) 0.459(2) 0.4085(9) 0.033(4) Uiso 1 1 d . . . H16B H 0.058(2) 0.666(2) 0.4107(9) 0.035(4) Uiso 1 1 d . . . C17 C 0.19036(16) 0.43832(16) 0.36779(7) 0.0255(2) Uani 1 1 d . . . H17A H 0.139(2) 0.309(2) 0.3334(9) 0.031(4) Uiso 1 1 d . . . H17B H 0.242(2) 0.414(2) 0.4256(9) 0.041(4) Uiso 1 1 d . . . C18 C 0.35743(15) 0.55403(17) 0.33248(7) 0.0262(2) Uani 1 1 d . . . H18B H 0.487(2) 0.549(2) 0.3643(9) 0.029(3) Uiso 1 1 d . . . H18A H 0.352(2) 0.692(2) 0.3442(8) 0.027(3) Uiso 1 1 d . . . C19 C 0.36109(15) 0.49216(16) 0.24181(7) 0.0254(2) Uani 1 1 d . . . H19A H 0.392(2) 0.358(2) 0.2334(9) 0.035(4) Uiso 1 1 d . . . H19B H 0.471(2) 0.584(2) 0.2239(9) 0.034(4) Uiso 1 1 d . . . C20 C 0.16956(14) 0.48264(14) 0.18331(6) 0.02118(18) Uani 1 1 d . . . H20A H 0.0652(19) 0.3780(18) 0.1914(8) 0.023(3) Uiso 1 1 d . . . H20B H 0.186(2) 0.4474(19) 0.1263(8) 0.026(3) Uiso 1 1 d . . . N1 N -0.12946(14) 0.95808(14) 0.38987(5) 0.02662(18) Uani 1 1 d . . . N2 N -0.02792(13) 1.01086(12) 0.20053(5) 0.02300(17) Uani 1 1 d . . . N3 N 0.08297(13) 0.97047(12) 0.14421(5) 0.02325(17) Uani 1 1 d . . . N4 N 0.44630(12) 0.74759(13) 0.09607(5) 0.02315(17) 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 C1 0.0367(6) 0.0346(6) 0.0226(5) 0.0026(4) 0.0089(4) 0.0142(5) C2 0.0371(6) 0.0270(5) 0.0308(5) 0.0063(4) 0.0176(4) 0.0141(4) C3 0.0297(5) 0.0280(5) 0.0346(5) 0.0121(4) 0.0149(4) 0.0155(4) C4 0.0254(4) 0.0256(5) 0.0249(5) 0.0082(4) 0.0080(4) 0.0114(4) C5 0.0216(4) 0.0187(4) 0.0215(4) 0.0040(3) 0.0066(3) 0.0065(3) C6 0.0189(4) 0.0206(4) 0.0200(4) 0.0039(3) 0.0050(3) 0.0068(3) C7 0.0164(3) 0.0195(4) 0.0190(4) 0.0044(3) 0.0042(3) 0.0052(3) C8 0.0165(4) 0.0187(4) 0.0193(4) 0.0037(3) 0.0038(3) 0.0050(3) C9 0.0192(4) 0.0195(4) 0.0194(4) 0.0040(3) 0.0049(3) 0.0055(3) C10 0.0218(4) 0.0185(4) 0.0201(4) 0.0044(3) 0.0069(3) 0.0057(3) C11 0.0264(5) 0.0272(5) 0.0210(4) 0.0060(4) 0.0050(3) 0.0082(4) C12 0.0366(5) 0.0288(5) 0.0193(4) 0.0051(4) 0.0087(4) 0.0076(4) C13 0.0345(5) 0.0255(5) 0.0267(5) 0.0045(4) 0.0158(4) 0.0084(4) C14 0.0252(5) 0.0279(5) 0.0291(5) 0.0055(4) 0.0116(4) 0.0090(4) C15 0.0188(4) 0.0219(4) 0.0261(4) 0.0068(3) 0.0084(3) 0.0057(3) C16 0.0270(5) 0.0277(5) 0.0243(5) 0.0089(4) 0.0100(4) 0.0100(4) C17 0.0260(5) 0.0290(5) 0.0273(5) 0.0125(4) 0.0093(4) 0.0111(4) C18 0.0203(4) 0.0327(5) 0.0275(5) 0.0100(4) 0.0049(3) 0.0062(4) C19 0.0225(4) 0.0314(5) 0.0290(5) 0.0130(4) 0.0096(4) 0.0130(4) C20 0.0226(4) 0.0191(4) 0.0245(4) 0.0047(3) 0.0075(3) 0.0076(3) N1 0.0289(4) 0.0319(5) 0.0213(4) 0.0026(3) 0.0048(3) 0.0129(3) N2 0.0276(4) 0.0228(4) 0.0233(4) 0.0067(3) 0.0098(3) 0.0107(3) N3 0.0279(4) 0.0232(4) 0.0232(4) 0.0069(3) 0.0100(3) 0.0104(3) N4 0.0215(4) 0.0278(4) 0.0229(4) 0.0064(3) 0.0076(3) 0.0074(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 C1 N1 1.3553(14) . ? C1 C2 1.3933(17) . ? C1 H1 1.011(17) . ? C2 C3 1.4005(17) . ? C2 H2 1.007(17) . ? C3 C4 1.3986(15) . ? C3 H3 0.997(18) . ? C4 C5 1.4026(14) . ? C4 H4 1.004(14) . ? C5 N1 1.3572(14) . ? C5 C6 1.5045(13) . ? C6 N2 1.3539(13) . ? C6 C7 1.4240(13) . ? C7 C8 1.4094(13) . ? C7 C15 1.5291(13) . ? C8 C9 1.4290(13) . ? C8 C20 1.5136(13) . ? C9 N3 1.3484(13) . ? C9 C10 1.5086(13) . ? C10 N4 1.3518(13) . ? C10 C11 1.4106(14) . ? C11 C12 1.4036(15) . ? C11 H11 1.000(15) . ? C12 C13 1.3943(17) . ? C12 H12 1.001(14) . ? C13 C14 1.4077(16) . ? C13 H13 1.006(17) . ? C14 N4 1.3530(13) . ? C14 H14 0.998(16) . ? C15 C16 1.5520(15) . ? C15 H15A 1.024(14) . ? C15 H15B 0.985(13) . ? C16 C17 1.5426(15) . ? C16 H16A 1.045(14) . ? C16 H16B 1.003(16) . ? C17 C18 1.5545(15) . ? C17 H17A 1.011(15) . ? C17 H17B 1.040(15) . ? C18 C19 1.5452(16) . ? C18 H18B 1.006(14) . ? C18 H18A 1.002(14) . ? C19 C20 1.5441(15) . ? C19 H19A 1.034(15) . ? C19 H19B 1.030(14) . ? C20 H20A 0.993(13) . ? C20 H20B 0.993(13) . ? N2 N3 1.3553(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.20(10) . . ? N1 C1 H1 115.0(9) . . ? C2 C1 H1 121.8(9) . . ? C1 C2 C3 118.59(10) . . ? C1 C2 H2 122.0(9) . . ? C3 C2 H2 119.4(9) . . ? C4 C3 C2 119.23(10) . . ? C4 C3 H3 119.7(10) . . ? C2 C3 H3 120.9(10) . . ? C3 C4 C5 118.28(10) . . ? C3 C4 H4 123.0(8) . . ? C5 C4 H4 118.7(8) . . ? N1 C5 C4 123.07(9) . . ? N1 C5 C6 116.59(8) . . ? C4 C5 C6 120.27(9) . . ? N2 C6 C7 123.66(8) . . ? N2 C6 C5 112.95(8) . . ? C7 C6 C5 123.39(8) . . ? C8 C7 C6 115.97(8) . . ? C8 C7 C15 123.15(8) . . ? C6 C7 C15 120.63(8) . . ? C7 C8 C9 117.44(8) . . ? C7 C8 C20 120.90(8) . . ? C9 C8 C20 121.63(8) . . ? N3 C9 C8 123.50(8) . . ? N3 C9 C10 112.71(8) . . ? C8 C9 C10 123.74(8) . . ? N4 C10 C11 122.85(9) . . ? N4 C10 C9 117.07(8) . . ? C11 C10 C9 120.04(9) . . ? C12 C11 C10 118.97(10) . . ? C12 C11 H11 122.2(8) . . ? C10 C11 H11 118.8(8) . . ? C13 C12 C11 118.78(10) . . ? C13 C12 H12 121.4(8) . . ? C11 C12 H12 119.8(8) . . ? C12 C13 C14 118.21(10) . . ? C12 C13 H13 123.4(10) . . ? C14 C13 H13 118.3(10) . . ? N4 C14 C13 123.99(10) . . ? N4 C14 H14 116.7(9) . . ? C13 C14 H14 119.3(9) . . ? C7 C15 C16 118.27(9) . . ? C7 C15 H15A 107.0(7) . . ? C16 C15 H15A 109.4(7) . . ? C7 C15 H15B 108.7(7) . . ? C16 C15 H15B 108.2(7) . . ? H15A C15 H15B 104.5(11) . . ? C17 C16 C15 116.61(9) . . ? C17 C16 H16A 109.7(8) . . ? C15 C16 H16A 105.7(8) . . ? C17 C16 H16B 113.2(9) . . ? C15 C16 H16B 106.4(9) . . ? H16A C16 H16B 104.3(12) . . ? C16 C17 C18 114.62(9) . . ? C16 C17 H17A 108.8(8) . . ? C18 C17 H17A 110.4(8) . . ? C16 C17 H17B 105.6(9) . . ? C18 C17 H17B 110.4(9) . . ? H17A C17 H17B 106.7(12) . . ? C19 C18 C17 116.02(10) . . ? C19 C18 H18B 108.0(8) . . ? C17 C18 H18B 109.7(8) . . ? C19 C18 H18A 111.3(8) . . ? C17 C18 H18A 107.8(8) . . ? H18B C18 H18A 103.2(11) . . ? C20 C19 C18 115.59(9) . . ? C20 C19 H19A 106.5(8) . . ? C18 C19 H19A 109.6(8) . . ? C20 C19 H19B 108.0(8) . . ? C18 C19 H19B 109.5(8) . . ? H19A C19 H19B 107.3(11) . . ? C8 C20 C19 113.17(9) . . ? C8 C20 H20A 109.4(7) . . ? C19 C20 H20A 110.8(7) . . ? C8 C20 H20B 108.8(8) . . ? C19 C20 H20B 110.6(8) . . ? H20A C20 H20B 103.8(11) . . ? C1 N1 C5 117.60(9) . . ? C6 N2 N3 120.22(8) . . ? C9 N3 N2 119.09(8) . . ? C10 N4 C14 117.20(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 1.44(18) . . . . ? C1 C2 C3 C4 -1.99(17) . . . . ? C2 C3 C4 C5 0.98(16) . . . . ? C3 C4 C5 N1 0.70(15) . . . . ? C3 C4 C5 C6 -176.24(9) . . . . ? N1 C5 C6 N2 -125.48(10) . . . . ? C4 C5 C6 N2 51.65(13) . . . . ? N1 C5 C6 C7 54.85(13) . . . . ? C4 C5 C6 C7 -128.02(11) . . . . ? N2 C6 C7 C8 3.70(14) . . . . ? C5 C6 C7 C8 -176.66(9) . . . . ? N2 C6 C7 C15 -170.78(9) . . . . ? C5 C6 C7 C15 8.86(14) . . . . ? C6 C7 C8 C9 -3.02(13) . . . . ? C15 C7 C8 C9 171.30(8) . . . . ? C6 C7 C8 C20 178.68(8) . . . . ? C15 C7 C8 C20 -6.99(14) . . . . ? C7 C8 C9 N3 0.36(14) . . . . ? C20 C8 C9 N3 178.64(9) . . . . ? C7 C8 C9 C10 -176.78(8) . . . . ? C20 C8 C9 C10 1.50(14) . . . . ? N3 C9 C10 N4 125.45(10) . . . . ? C8 C9 C10 N4 -57.13(13) . . . . ? N3 C9 C10 C11 -52.06(13) . . . . ? C8 C9 C10 C11 125.35(11) . . . . ? N4 C10 C11 C12 0.00(15) . . . . ? C9 C10 C11 C12 177.36(9) . . . . ? C10 C11 C12 C13 -0.64(16) . . . . ? C11 C12 C13 C14 0.58(16) . . . . ? C12 C13 C14 N4 0.12(17) . . . . ? C8 C7 C15 C16 84.08(12) . . . . ? C6 C7 C15 C16 -101.85(11) . . . . ? C7 C15 C16 C17 -72.28(12) . . . . ? C15 C16 C17 C18 67.98(13) . . . . ? C16 C17 C18 C19 -101.32(12) . . . . ? C17 C18 C19 C20 53.84(13) . . . . ? C7 C8 C20 C19 -87.76(11) . . . . ? C9 C8 C20 C19 94.01(11) . . . . ? C18 C19 C20 C8 55.25(12) . . . . ? C2 C1 N1 C5 0.19(17) . . . . ? C4 C5 N1 C1 -1.28(16) . . . . ? C6 C5 N1 C1 175.76(10) . . . . ? C7 C6 N2 N3 -1.42(15) . . . . ? C5 C6 N2 N3 178.90(8) . . . . ? C8 C9 N3 N2 2.04(15) . . . . ? C10 C9 N3 N2 179.46(9) . . . . ? C6 N2 N3 C9 -1.51(14) . . . . ? C11 C10 N4 C14 0.68(14) . . . . ? C9 C10 N4 C14 -176.76(9) . . . . ? C13 C14 N4 C10 -0.74(16) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 39.59 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.437 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.068