Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Suning Wang' 'Youngjin Kang' 'Junghyun Lee' 'Datong Song' _publ_contact_author_name 'Dr Suning Wang' _publ_contact_author_address ; Department of Chemistry Queen's University 90 Queen's crescent Chernoff Hall Kingston Ontario K7L 3N6 CANADA ; _publ_contact_author_email WANGS@CHEM.QUEENSU.CA _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Platinum(II) diimine complexes of Acetylides containing 7-azaindolyl and 2,2'-dipyridylamino Functional groups ; data_compound_1 _database_code_CSD 210583 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H36 N6 Pt' _chemical_formula_weight 867.90 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 Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6498(12) _cell_length_b 16.203(3) _cell_length_c 17.395(4) _cell_angle_alpha 88.544(3) _cell_angle_beta 83.276(4) _cell_angle_gamma 83.331(4) _cell_volume 1848.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 571(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'thin plate' _exptl_crystal_colour yellow _exptl_crystal_size_max .05 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 3.837 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.869 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 571(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13567 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.2815 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.32 _reflns_number_total 8536 _reflns_number_gt 3308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^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 8536 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1488 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 0.695 _refine_ls_restrained_S_all 0.695 _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 0.30339(5) -0.07224(2) -0.08505(2) 0.04652(12) Uani 1 1 d . . . N1 N 0.7093(14) -0.5696(5) -0.2756(5) 0.082(2) Uani 1 1 d . . . N2 N 1.0105(14) -0.6069(5) -0.2144(5) 0.088(3) Uani 1 1 d . . . N3 N 0.1679(11) 0.1335(4) -0.5513(4) 0.057(2) Uani 1 1 d . . . N4 N -0.1748(12) 0.2021(4) -0.5303(4) 0.068(2) Uani 1 1 d . . . N5 N 0.2960(9) -0.1026(5) 0.0305(4) 0.0474(19) Uani 1 1 d . . . N6 N 0.2338(9) 0.0418(4) -0.0335(5) 0.0489(19) Uani 1 1 d . . . C1 C 0.6107(17) -0.6066(8) -0.3292(7) 0.103(4) Uani 1 1 d . . . H1A H 0.4874 -0.5849 -0.3460 0.124 Uiso 1 1 calc R . . C2 C 0.719(2) -0.6783(8) -0.3533(6) 0.104(4) Uani 1 1 d . . . H2B H 0.6846 -0.7141 -0.3894 0.125 Uiso 1 1 calc R . . C3 C 0.8942(19) -0.6897(7) -0.3143(7) 0.089(3) Uani 1 1 d . . . C4 C 1.059(2) -0.7487(7) -0.3122(7) 0.109(4) Uani 1 1 d . . . H4B H 1.0774 -0.7946 -0.3444 0.130 Uiso 1 1 calc R . . C5 C 1.1926(19) -0.7379(7) -0.2619(9) 0.118(5) Uani 1 1 d . . . H5A H 1.3022 -0.7782 -0.2573 0.142 Uiso 1 1 calc R . . C6 C 1.1688(16) -0.6679(8) -0.2173(7) 0.099(4) Uani 1 1 d . . . H6A H 1.2706 -0.6618 -0.1862 0.119 Uiso 1 1 calc R . . C7 C 0.8862(17) -0.6210(7) -0.2637(6) 0.074(3) Uani 1 1 d . . . C8 C 0.6351(16) -0.4901(6) -0.2408(5) 0.069(3) Uani 1 1 d . . . C9 C 0.7690(13) -0.4319(6) -0.2347(5) 0.081(3) Uani 1 1 d . . . H9A H 0.9067 -0.4446 -0.2519 0.097 Uiso 1 1 calc R . . C10 C 0.7000(14) -0.3562(6) -0.2037(5) 0.075(3) Uani 1 1 d . . . H10A H 0.7922 -0.3178 -0.2006 0.090 Uiso 1 1 calc R . . C11 C 0.4959(14) -0.3345(5) -0.1766(5) 0.051(2) Uani 1 1 d . . . C12 C 0.3656(13) -0.3935(6) -0.1844(5) 0.079(3) Uani 1 1 d . . . H12A H 0.2274 -0.3807 -0.1681 0.095 Uiso 1 1 calc R . . C13 C 0.4325(15) -0.4701(6) -0.2154(5) 0.074(3) Uani 1 1 d . . . H13A H 0.3405 -0.5085 -0.2192 0.089 Uiso 1 1 calc R . . C14 C 0.4260(12) -0.2531(6) -0.1463(5) 0.058(3) Uani 1 1 d . . . C15 C 0.3749(12) -0.1849(6) -0.1232(5) 0.051(3) Uani 1 1 d . . . C16 C 0.3089(13) 0.1232(5) -0.6143(6) 0.067(3) Uani 1 1 d . . . H16A H 0.4401 0.0965 -0.6131 0.080 Uiso 1 1 calc R . . C17 C 0.2358(15) 0.1567(6) -0.6796(5) 0.073(3) Uani 1 1 d . . . H17A H 0.3030 0.1564 -0.7296 0.087 Uiso 1 1 calc R . . C18 C 0.0381(15) 0.1914(6) -0.6547(6) 0.065(3) Uani 1 1 d . . . C19 C -0.1198(17) 0.2339(6) -0.6910(6) 0.091(4) Uani 1 1 d . . . H19A H -0.1048 0.2435 -0.7442 0.109 Uiso 1 1 calc R . . C20 C -0.2967(17) 0.2609(7) -0.6466(7) 0.100(4) Uani 1 1 d . . . H20A H -0.4039 0.2896 -0.6696 0.120 Uiso 1 1 calc R . . C21 C -0.3180(13) 0.2459(6) -0.5675(6) 0.086(3) Uani 1 1 d . . . H21A H -0.4384 0.2675 -0.5386 0.103 Uiso 1 1 calc R . . C22 C -0.0060(15) 0.1775(6) -0.5753(6) 0.060(3) Uani 1 1 d . . . C23 C 0.1965(15) 0.1008(5) -0.4749(5) 0.055(2) Uani 1 1 d . . . C24 C 0.0403(13) 0.0649(5) -0.4328(5) 0.054(2) Uani 1 1 d . . . H24A H -0.0837 0.0640 -0.4524 0.065 Uiso 1 1 calc R . . C25 C 0.0692(13) 0.0309(5) -0.3621(5) 0.056(2) Uani 1 1 d . . . H25A H -0.0367 0.0063 -0.3342 0.068 Uiso 1 1 calc R . . C26 C 0.2497(14) 0.0314(5) -0.3300(5) 0.049(2) Uani 1 1 d . . . C27 C 0.4052(13) 0.0684(5) -0.3744(5) 0.062(3) Uani 1 1 d . . . H27A H 0.5291 0.0703 -0.3551 0.074 Uiso 1 1 calc R . . C28 C 0.3775(12) 0.1019(5) -0.4459(5) 0.061(3) Uani 1 1 d . . . H28A H 0.4831 0.1256 -0.4749 0.073 Uiso 1 1 calc R . . C29 C 0.2786(12) -0.0031(6) -0.2544(6) 0.058(3) Uani 1 1 d . . . C30 C 0.2941(11) -0.0307(5) -0.1899(5) 0.053(3) Uani 1 1 d . . . C31 C 0.3229(10) -0.1798(6) 0.0584(5) 0.058(3) Uani 1 1 d . . . H31A H 0.3499 -0.2237 0.0239 0.069 Uiso 1 1 calc R . . C32 C 0.3118(12) -0.1971(7) 0.1386(6) 0.070(3) Uani 1 1 d . . . H32A H 0.3324 -0.2513 0.1573 0.084 Uiso 1 1 calc R . . C33 C 0.2690(13) -0.1302(8) 0.1886(5) 0.075(3) Uani 1 1 d . . . H33A H 0.2590 -0.1391 0.2419 0.090 Uiso 1 1 calc R . . C34 C 0.2420(12) -0.0525(7) 0.1595(6) 0.070(3) Uani 1 1 d . . . H34A H 0.2150 -0.0076 0.1929 0.084 Uiso 1 1 calc R . . C35 C 0.2541(11) -0.0391(7) 0.0809(6) 0.052(2) Uani 1 1 d . . . C36 C 0.2213(11) 0.0414(7) 0.0433(6) 0.055(3) Uani 1 1 d . . . C37 C 0.1762(12) 0.1127(7) 0.0872(6) 0.072(3) Uani 1 1 d . . . H37A H 0.1678 0.1107 0.1409 0.086 Uiso 1 1 calc R . . C38 C 0.1449(12) 0.1859(7) 0.0480(7) 0.077(3) Uani 1 1 d . . . H38A H 0.1119 0.2350 0.0755 0.093 Uiso 1 1 calc R . . C39 C 0.1610(11) 0.1884(6) -0.0314(6) 0.064(3) Uani 1 1 d . . . H39A H 0.1420 0.2386 -0.0581 0.076 Uiso 1 1 calc R . . C40 C 0.2064(10) 0.1138(6) -0.0706(5) 0.052(2) Uani 1 1 d . . . H40A H 0.2178 0.1144 -0.1244 0.062 Uiso 1 1 calc R . . C41 C 0.893(5) -0.4099(17) -0.4657(16) 0.337(13) Uiso 1 1 d . . . C42 C 1.198(4) -0.550(3) -0.486(2) 0.408(16) Uiso 1 1 d . . . C43 C 1.089(4) -0.4754(19) -0.4489(12) 0.257(8) Uiso 1 1 d . . . C49 C 0.030(4) -0.5546(14) -0.0040(14) 0.134(10) Uiso 0.50 1 d P . . C48 C 0.800(3) -0.5947(13) -0.0204(11) 0.103(7) Uiso 0.50 1 d P . . C47 C 0.216(6) -0.501(3) 0.027(2) 0.250(16) Uiso 0.50 1 d P . . C44 C 0.374(4) -0.5820(14) -0.0199(13) 0.127(8) Uiso 0.50 1 d P . . C45 C 0.602(4) -0.5671(15) -0.0255(14) 0.139(9) Uiso 0.50 1 d P . . C46 C 0.184(4) -0.5731(14) -0.0046(12) 0.093(7) Uiso 0.50 1 d P . . 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 0.04158(18) 0.0496(2) 0.0477(2) -0.00154(16) -0.00603(14) -0.00113(14) N1 0.104(7) 0.066(7) 0.075(7) -0.020(5) -0.007(5) -0.001(6) N2 0.097(7) 0.054(6) 0.114(8) -0.017(6) -0.019(6) -0.005(5) N3 0.058(5) 0.057(5) 0.053(6) 0.002(5) 0.007(5) -0.002(4) N4 0.074(5) 0.065(6) 0.062(6) 0.010(5) -0.014(5) 0.007(5) N5 0.042(4) 0.048(5) 0.056(5) 0.007(5) -0.017(4) -0.008(4) N6 0.046(4) 0.051(6) 0.050(5) -0.006(5) -0.009(4) -0.002(4) C1 0.130(10) 0.082(10) 0.104(10) -0.018(8) -0.034(8) -0.014(8) C2 0.131(11) 0.083(10) 0.099(10) -0.025(8) -0.018(8) 0.001(8) C3 0.109(10) 0.061(9) 0.086(9) -0.008(8) 0.018(8) 0.007(8) C4 0.139(12) 0.054(9) 0.127(12) -0.027(8) 0.018(9) -0.016(9) C5 0.125(11) 0.039(8) 0.178(16) -0.020(9) 0.029(10) 0.002(8) C6 0.095(9) 0.072(9) 0.129(11) 0.014(8) -0.022(8) 0.001(7) C7 0.089(8) 0.049(8) 0.077(8) -0.014(7) 0.008(7) 0.001(7) C8 0.086(8) 0.051(7) 0.068(7) -0.014(6) 0.008(6) -0.007(6) C9 0.068(6) 0.060(8) 0.110(9) -0.023(7) 0.004(6) -0.002(6) C10 0.082(7) 0.049(7) 0.095(8) -0.015(6) -0.003(6) -0.020(6) C11 0.063(6) 0.042(6) 0.049(6) -0.004(5) -0.007(5) -0.010(5) C12 0.074(7) 0.051(7) 0.110(9) -0.007(7) -0.014(6) 0.001(6) C13 0.086(8) 0.047(7) 0.091(8) 0.001(6) -0.009(6) -0.013(6) C14 0.059(6) 0.069(8) 0.048(7) -0.010(6) -0.007(5) -0.010(6) C15 0.053(6) 0.074(8) 0.031(6) -0.006(6) -0.012(4) -0.015(5) C16 0.068(6) 0.069(7) 0.060(7) -0.007(6) 0.008(6) -0.007(5) C17 0.084(8) 0.080(8) 0.052(7) -0.003(6) 0.009(6) -0.015(6) C18 0.071(7) 0.060(7) 0.066(8) 0.014(6) -0.014(7) -0.012(6) C19 0.101(8) 0.116(10) 0.063(8) 0.024(7) -0.012(7) -0.045(8) C20 0.092(9) 0.134(11) 0.082(9) 0.062(8) -0.031(7) -0.033(8) C21 0.067(7) 0.097(9) 0.090(9) 0.024(7) -0.011(7) -0.001(6) C22 0.070(7) 0.049(7) 0.062(8) 0.009(6) -0.009(6) -0.012(6) C23 0.076(7) 0.041(6) 0.046(6) 0.008(5) -0.006(6) -0.004(5) C24 0.070(6) 0.052(6) 0.040(6) 0.002(5) -0.014(5) 0.007(5) C25 0.081(7) 0.038(6) 0.048(6) -0.001(5) 0.000(5) -0.005(5) C26 0.061(6) 0.043(6) 0.039(6) -0.005(5) 0.003(5) 0.009(5) C27 0.059(6) 0.061(7) 0.060(7) 0.003(6) -0.008(5) 0.012(5) C28 0.058(6) 0.053(7) 0.070(8) 0.008(6) -0.002(5) -0.009(5) C29 0.054(6) 0.052(7) 0.063(7) -0.013(6) 0.000(6) 0.006(5) C30 0.040(5) 0.041(6) 0.077(8) 0.002(6) -0.014(5) 0.008(4) C31 0.039(5) 0.069(8) 0.066(8) -0.013(6) 0.000(5) -0.010(5) C32 0.062(6) 0.094(9) 0.052(7) 0.026(7) -0.004(5) -0.011(6) C33 0.070(7) 0.108(10) 0.041(7) -0.010(7) 0.010(5) -0.005(7) C34 0.062(6) 0.085(9) 0.061(8) 0.010(7) 0.000(6) -0.006(6) C35 0.034(5) 0.073(8) 0.049(7) -0.009(7) -0.002(5) -0.011(5) C36 0.028(5) 0.062(8) 0.076(8) -0.019(7) -0.007(5) -0.010(5) C37 0.059(6) 0.081(9) 0.077(8) 0.010(8) -0.017(6) -0.010(6) C38 0.056(6) 0.094(10) 0.081(9) -0.043(8) -0.002(7) -0.001(6) C39 0.039(5) 0.054(8) 0.095(9) 0.002(7) 0.002(6) -0.003(5) C40 0.032(5) 0.051(7) 0.071(7) 0.003(6) -0.002(5) -0.008(5) _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 C30 1.934(9) . ? Pt1 C15 1.946(9) . ? Pt1 N5 2.054(7) . ? Pt1 N6 2.055(7) . ? N1 C1 1.386(10) . ? N1 C7 1.393(11) . ? N1 C8 1.445(10) . ? N2 C7 1.300(10) . ? N2 C6 1.355(11) . ? N3 C16 1.357(9) . ? N3 C22 1.388(9) . ? N3 C23 1.443(9) . ? N4 C22 1.319(10) . ? N4 C21 1.340(9) . ? N5 C31 1.330(9) . ? N5 C35 1.350(10) . ? N6 C40 1.323(9) . ? N6 C36 1.329(10) . ? C1 C2 1.345(12) . ? C2 C3 1.407(12) . ? C3 C4 1.370(13) . ? C3 C7 1.429(12) . ? C4 C5 1.347(13) . ? C5 C6 1.374(13) . ? C8 C13 1.372(10) . ? C8 C9 1.384(10) . ? C9 C10 1.360(10) . ? C10 C11 1.392(10) . ? C11 C12 1.382(10) . ? C11 C14 1.438(11) . ? C12 C13 1.370(10) . ? C14 C15 1.183(10) . ? C16 C17 1.362(10) . ? C17 C18 1.393(11) . ? C18 C19 1.393(11) . ? C18 C22 1.396(11) . ? C19 C20 1.363(12) . ? C20 C21 1.385(11) . ? C23 C28 1.361(9) . ? C23 C24 1.376(10) . ? C24 C25 1.361(9) . ? C25 C26 1.382(9) . ? C26 C27 1.399(10) . ? C26 C29 1.441(11) . ? C27 C28 1.367(9) . ? C29 C30 1.207(10) . ? C31 C32 1.411(10) . ? C32 C33 1.390(11) . ? C33 C34 1.345(11) . ? C34 C35 1.375(10) . ? C35 C36 1.449(11) . ? C36 C37 1.384(11) . ? C37 C38 1.359(11) . ? C38 C39 1.373(11) . ? C39 C40 1.388(10) . ? C41 C42 1.32(4) 2_744 ? C41 C43 1.63(3) . ? C42 C41 1.32(4) 2_744 ? C42 C43 1.46(3) . ? C49 C46 1.03(3) . ? C49 C47 1.74(5) . ? C49 C49 1.77(5) 2_545 ? C49 C48 1.78(3) 1_455 ? C49 C47 1.85(4) 2_545 ? C48 C45 1.35(3) . ? C48 C47 1.54(4) 2_645 ? C48 C49 1.78(3) 1_655 ? C47 C46 1.35(4) . ? C47 C48 1.54(4) 2_645 ? C47 C45 1.73(4) 2_645 ? C47 C44 1.74(5) . ? C47 C49 1.85(4) 2_545 ? C44 C46 1.26(3) . ? C44 C45 1.55(3) . ? C45 C47 1.73(4) 2_645 ? 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 C30 Pt1 C15 90.3(3) . . ? C30 Pt1 N5 173.1(4) . . ? C15 Pt1 N5 96.4(3) . . ? C30 Pt1 N6 95.6(3) . . ? C15 Pt1 N6 174.0(4) . . ? N5 Pt1 N6 77.6(3) . . ? C1 N1 C7 108.5(9) . . ? C1 N1 C8 123.5(10) . . ? C7 N1 C8 128.0(9) . . ? C7 N2 C6 110.4(9) . . ? C16 N3 C22 107.3(8) . . ? C16 N3 C23 125.0(8) . . ? C22 N3 C23 127.7(8) . . ? C22 N4 C21 113.8(8) . . ? C31 N5 C35 118.7(8) . . ? C31 N5 Pt1 124.5(7) . . ? C35 N5 Pt1 116.8(7) . . ? C40 N6 C36 118.9(8) . . ? C40 N6 Pt1 125.3(7) . . ? C36 N6 Pt1 115.8(7) . . ? C2 C1 N1 110.1(11) . . ? C1 C2 C3 107.8(11) . . ? C4 C3 C2 136.4(14) . . ? C4 C3 C7 115.8(12) . . ? C2 C3 C7 107.8(11) . . ? C5 C4 C3 117.6(13) . . ? C4 C5 C6 120.7(13) . . ? N2 C6 C5 126.0(11) . . ? N2 C7 N1 124.7(11) . . ? N2 C7 C3 129.4(11) . . ? N1 C7 C3 105.8(11) . . ? C13 C8 C9 118.9(9) . . ? C13 C8 N1 121.3(9) . . ? C9 C8 N1 119.8(9) . . ? C10 C9 C8 120.3(9) . . ? C9 C10 C11 122.1(8) . . ? C12 C11 C10 116.3(8) . . ? C12 C11 C14 122.7(9) . . ? C10 C11 C14 120.9(8) . . ? C13 C12 C11 122.4(9) . . ? C12 C13 C8 120.0(9) . . ? C15 C14 C11 177.3(11) . . ? C14 C15 Pt1 177.5(8) . . ? N3 C16 C17 112.1(8) . . ? C16 C17 C18 104.6(9) . . ? C17 C18 C19 134.6(11) . . ? C17 C18 C22 109.9(9) . . ? C19 C18 C22 115.5(10) . . ? C20 C19 C18 118.2(10) . . ? C19 C20 C21 120.5(10) . . ? N4 C21 C20 123.6(10) . . ? N4 C22 N3 125.7(10) . . ? N4 C22 C18 128.2(10) . . ? N3 C22 C18 106.1(10) . . ? C28 C23 C24 120.1(8) . . ? C28 C23 N3 120.9(9) . . ? C24 C23 N3 118.9(8) . . ? C25 C24 C23 119.2(8) . . ? C24 C25 C26 122.6(8) . . ? C25 C26 C27 116.6(8) . . ? C25 C26 C29 122.5(8) . . ? C27 C26 C29 120.8(8) . . ? C28 C27 C26 121.0(8) . . ? C23 C28 C27 120.5(8) . . ? C30 C29 C26 177.1(10) . . ? C29 C30 Pt1 176.8(8) . . ? N5 C31 C32 122.0(9) . . ? C33 C32 C31 117.6(10) . . ? C34 C33 C32 119.6(10) . . ? C33 C34 C35 120.5(11) . . ? N5 C35 C34 121.5(10) . . ? N5 C35 C36 113.3(9) . . ? C34 C35 C36 125.1(10) . . ? N6 C36 C37 123.3(10) . . ? N6 C36 C35 116.5(9) . . ? C37 C36 C35 120.2(11) . . ? C38 C37 C36 116.9(10) . . ? C37 C38 C39 121.1(11) . . ? C38 C39 C40 118.1(10) . . ? N6 C40 C39 121.7(9) . . ? C42 C41 C43 103(3) 2_744 . ? C41 C42 C43 119(3) 2_744 . ? C42 C43 C41 136(2) . . ? C46 C49 C47 51(2) . . ? C46 C49 C49 112(3) . 2_545 ? C47 C49 C49 63.8(18) . 2_545 ? C46 C49 C48 141(2) . 1_455 ? C47 C49 C48 167(2) . 1_455 ? C49 C49 C48 106(2) 2_545 1_455 ? C46 C49 C47 162(3) . 2_545 ? C47 C49 C47 121(2) . 2_545 ? C49 C49 C47 57.1(19) 2_545 2_545 ? C48 C49 C47 50.2(17) 1_455 2_545 ? C45 C48 C47 72.8(19) . 2_645 ? C45 C48 C49 139(2) . 1_655 ? C47 C48 C49 67.4(16) 2_645 1_655 ? C46 C47 C48 147(3) . 2_645 ? C46 C47 C45 141(3) . 2_645 ? C48 C47 C45 48.5(17) 2_645 2_645 ? C46 C47 C49 36.4(16) . . ? C48 C47 C49 120(3) 2_645 . ? C45 C47 C49 160(3) 2_645 . ? C46 C47 C44 45.9(19) . . ? C48 C47 C44 135(3) 2_645 . ? C45 C47 C44 97(2) 2_645 . ? C49 C47 C44 82(3) . . ? C46 C47 C49 94(3) . 2_545 ? C48 C47 C49 62.4(19) 2_645 2_545 ? C45 C47 C49 110(3) 2_645 2_545 ? C49 C47 C49 59(2) . 2_545 ? C44 C47 C49 131(3) . 2_545 ? C46 C44 C45 162(2) . . ? C46 C44 C47 50.6(17) . . ? C45 C44 C47 112(2) . . ? C48 C45 C44 151(2) . . ? C48 C45 C47 58.7(18) . 2_645 ? C44 C45 C47 149(2) . 2_645 ? C49 C46 C44 165(3) . . ? C49 C46 C47 92(3) . . ? C44 C46 C47 84(2) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.026 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.107 data_compound_4 _database_code_CSD 210584 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H41 Cl2 N8 Pt' _chemical_formula_weight 1043.93 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.154(3) _cell_length_b 13.057(3) _cell_length_c 19.080(5) _cell_angle_alpha 70.846(4) _cell_angle_beta 81.790(5) _cell_angle_gamma 72.416(6) _cell_volume 2275.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1042 _exptl_absorpt_coefficient_mu 3.247 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 1.00 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13823 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.2606 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 28.26 _reflns_number_total 9491 _reflns_number_gt 3924 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^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 9491 _refine_ls_number_parameters 553 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1722 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1171 _refine_ls_goodness_of_fit_ref 0.850 _refine_ls_restrained_S_all 0.850 _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 -0.91509(5) 1.08571(4) -0.92986(3) 0.04242(16) Uani 1 1 d . . . Cl1 Cl 0.1298(5) 0.2002(4) -0.4592(3) 0.1263(16) Uani 1 1 d . . . Cl2 Cl -0.1231(5) 0.2569(4) -0.3726(3) 0.1287(17) Uani 1 1 d . . . N1 N -1.0920(9) 1.1642(8) -0.9886(5) 0.043(2) Uani 1 1 d . . . N2 N -1.0317(9) 0.9725(8) -0.8794(5) 0.046(2) Uani 1 1 d . . . N3 N -0.3594(12) 1.5800(9) -1.1757(5) 0.066(3) Uani 1 1 d . . . N4 N -0.5952(11) 1.6639(8) -1.1854(5) 0.060(3) Uani 1 1 d . . . N5 N -0.6456(12) 1.8226(10) -1.2845(6) 0.080(4) Uani 1 1 d . . . N6 N -0.2437(12) 0.5582(9) -0.4750(7) 0.083(4) Uani 1 1 d . . . N7 N -0.3339(10) 0.6161(9) -0.5929(6) 0.065(3) Uani 1 1 d . . . N8 N -0.1560(12) 0.5619(9) -0.6758(6) 0.072(3) Uani 1 1 d . . . C1 C -1.1200(13) 1.2592(11) -1.0416(7) 0.067(4) Uani 1 1 d . . . H1A H -1.0549 1.3002 -1.0570 0.081 Uiso 1 1 calc R . . C2 C -1.2484(15) 1.3015(12) -1.0763(7) 0.077(4) Uani 1 1 d . . . H2A H -1.2645 1.3680 -1.1156 0.092 Uiso 1 1 calc R . . C3 C -1.3452(13) 1.2479(13) -1.0538(8) 0.072(4) Uani 1 1 d . . . H3A H -1.4286 1.2765 -1.0772 0.086 Uiso 1 1 calc R . . C4 C -1.3224(12) 1.1488(12) -0.9950(7) 0.058(3) Uani 1 1 d . . . C5 C -1.4187(12) 1.0795(14) -0.9634(8) 0.072(4) Uani 1 1 d . . . H5A H -1.5065 1.1036 -0.9818 0.087 Uiso 1 1 calc R . . C6 C -1.3843(15) 0.9850(13) -0.9100(8) 0.075(4) Uani 1 1 d . . . H6A H -1.4491 0.9440 -0.8915 0.090 Uiso 1 1 calc R . . C7 C -1.2558(13) 0.9430(12) -0.8798(7) 0.056(3) Uani 1 1 d . . . C8 C -1.2151(15) 0.8460(12) -0.8238(8) 0.069(4) Uani 1 1 d . . . H8A H -1.2762 0.8019 -0.8040 0.083 Uiso 1 1 calc R . . C9 C -1.0897(17) 0.8118(11) -0.7961(7) 0.074(4) Uani 1 1 d . . . H9A H -1.0644 0.7446 -0.7579 0.089 Uiso 1 1 calc R . . C10 C -0.9983(13) 0.8768(10) -0.8244(7) 0.060(4) Uani 1 1 d . . . H10A H -0.9117 0.8530 -0.8047 0.072 Uiso 1 1 calc R . . C11 C -1.1598(11) 1.0074(10) -0.9068(6) 0.045(3) Uani 1 1 d . . . C12 C -1.1942(11) 1.1108(10) -0.9657(6) 0.046(3) Uani 1 1 d . . . C13 C -0.8263(11) 1.2000(10) -0.9828(6) 0.049(3) Uani 1 1 d . . . C14 C -0.7785(12) 1.2779(11) -1.0193(7) 0.061(4) Uani 1 1 d . . . C15 C -0.7269(11) 1.3753(9) -1.0625(7) 0.049(3) Uani 1 1 d . . . C16 C -0.6733(11) 1.4312(10) -1.0280(6) 0.056(3) Uani 1 1 d . . . H16A H -0.6673 1.4057 -0.9767 0.067 Uiso 1 1 calc R . . C17 C -0.6283(12) 1.5254(10) -1.0694(7) 0.062(4) Uani 1 1 d . . . H17A H -0.5941 1.5625 -1.0451 0.075 Uiso 1 1 calc R . . C18 C -0.6334(12) 1.5642(10) -1.1448(6) 0.050(3) Uani 1 1 d . . . C19 C -0.6820(14) 1.5065(10) -1.1783(7) 0.073(4) Uani 1 1 d . . . H19A H -0.6833 1.5299 -1.2298 0.088 Uiso 1 1 calc R . . C20 C -0.7285(13) 1.4163(10) -1.1392(7) 0.068(4) Uani 1 1 d . . . H20A H -0.7626 1.3807 -1.1646 0.082 Uiso 1 1 calc R . . C21 C -0.4636(15) 1.6728(11) -1.1801(6) 0.058(3) Uani 1 1 d . . . C22 C -0.4433(18) 1.7710(11) -1.1760(7) 0.078(5) Uani 1 1 d . . . H22A H -0.5183 1.8335 -1.1770 0.094 Uiso 1 1 calc R . . C23 C -0.313(2) 1.7754(15) -1.1704(9) 0.102(6) Uani 1 1 d . . . H23A H -0.2990 1.8415 -1.1683 0.122 Uiso 1 1 calc R . . C24 C -0.201(2) 1.6823(17) -1.1679(8) 0.100(6) Uani 1 1 d . . . H24A H -0.1115 1.6843 -1.1654 0.120 Uiso 1 1 calc R . . C25 C -0.2294(14) 1.5882(16) -1.1692(9) 0.103(6) Uani 1 1 d . . . H25A H -0.1556 1.5241 -1.1655 0.123 Uiso 1 1 calc R . . C26 C -0.6929(14) 1.7562(11) -1.2261(7) 0.057(3) Uani 1 1 d . . . C27 C -0.8292(16) 1.7750(11) -1.2038(8) 0.078(4) Uani 1 1 d . . . H27A H -0.8563 1.7250 -1.1608 0.094 Uiso 1 1 calc R . . C28 C -0.9282(16) 1.8663(13) -1.2434(9) 0.083(5) Uani 1 1 d . . . H28A H -1.0219 1.8789 -1.2295 0.099 Uiso 1 1 calc R . . C29 C -0.879(2) 1.9364(12) -1.3038(9) 0.107(6) Uani 1 1 d . . . H29A H -0.9393 2.0008 -1.3327 0.128 Uiso 1 1 calc R . . C30 C -0.734(2) 1.9099(14) -1.3226(9) 0.106(6) Uani 1 1 d . . . H30A H -0.7020 1.9583 -1.3646 0.127 Uiso 1 1 calc R . . C31 C -0.7641(12) 0.9941(10) -0.8616(7) 0.053(3) Uani 1 1 d . . . C32 C -0.6848(13) 0.9312(11) -0.8154(7) 0.058(4) Uani 1 1 d . . . C33 C -0.5955(11) 0.8535(11) -0.7589(6) 0.048(3) Uani 1 1 d . . . C34 C -0.5227(13) 0.8874(10) -0.7178(7) 0.064(4) Uani 1 1 d . . . H34A H -0.5327 0.9638 -0.7271 0.076 Uiso 1 1 calc R . . C35 C -0.4374(12) 0.8110(11) -0.6642(6) 0.060(3) Uani 1 1 d . . . H35A H -0.3885 0.8363 -0.6387 0.072 Uiso 1 1 calc R . . C36 C -0.4222(12) 0.6996(10) -0.6474(7) 0.053(3) Uani 1 1 d . . . C37 C -0.4914(12) 0.6663(10) -0.6883(7) 0.058(3) Uani 1 1 d . . . H37A H -0.4810 0.5899 -0.6792 0.070 Uiso 1 1 calc R . . C38 C -0.5772(12) 0.7446(11) -0.7435(7) 0.061(3) Uani 1 1 d . . . H38A H -0.6231 0.7190 -0.7703 0.073 Uiso 1 1 calc R . . C39 C -0.256(2) 0.5598(14) -0.4042(10) 0.116(7) Uani 1 1 d . . . H39A H -0.1808 0.5215 -0.3741 0.139 Uiso 1 1 calc R . . C40 C -0.374(3) 0.6158(17) -0.3764(9) 0.119(7) Uani 1 1 d . . . H40A H -0.3830 0.6089 -0.3260 0.143 Uiso 1 1 calc R . . C41 C -0.478(2) 0.6806(15) -0.4191(10) 0.117(6) Uani 1 1 d . . . H41A H -0.5555 0.7251 -0.4007 0.141 Uiso 1 1 calc R . . C42 C -0.4668(16) 0.6802(12) -0.4917(8) 0.089(5) Uani 1 1 d . . . H42A H -0.5398 0.7230 -0.5225 0.107 Uiso 1 1 calc R . . C43 C -0.3497(16) 0.6174(11) -0.5191(8) 0.068(4) Uani 1 1 d . . . C44 C -0.2311(13) 0.5277(11) -0.6151(8) 0.056(3) Uani 1 1 d . . . C45 C -0.2173(16) 0.4198(13) -0.5756(8) 0.090(5) Uani 1 1 d . . . H45A H -0.2683 0.3987 -0.5313 0.108 Uiso 1 1 calc R . . C46 C -0.119(2) 0.3389(13) -0.6060(12) 0.115(7) Uani 1 1 d . . . H46A H -0.1054 0.2620 -0.5832 0.138 Uiso 1 1 calc R . . C47 C -0.045(2) 0.378(2) -0.6690(11) 0.117(7) Uani 1 1 d . . . H47A H 0.0214 0.3267 -0.6889 0.140 Uiso 1 1 calc R . . C48 C -0.0655(18) 0.4836(17) -0.7017(11) 0.109(6) Uani 1 1 d . . . H48A H -0.0145 0.5068 -0.7455 0.131 Uiso 1 1 calc R . . C49 C 0.0174(15) 0.3000(13) -0.4239(8) 0.102(5) Uani 1 1 d . . . H49A H -0.0166 0.3675 -0.4645 0.122 Uiso 1 1 calc R . . H49B H 0.0669 0.3193 -0.3923 0.122 Uiso 1 1 calc R . . C50 C 0.2108(14) 0.0662(11) -0.6211(8) 0.091(5) Uiso 1 1 d . . . H50A H 0.1588 0.1183 -0.6627 0.137 Uiso 1 1 calc R . . H50B H 0.1519 0.0603 -0.5767 0.137 Uiso 1 1 calc R . . H50C H 0.2461 -0.0065 -0.6288 0.137 Uiso 1 1 calc R . . C51 C 0.3152(15) 0.1027(12) -0.6142(8) 0.094(5) Uiso 1 1 d . . . H51A H 0.2764 0.1782 -0.6099 0.113 Uiso 1 1 calc R . . H51B H 0.3709 0.1098 -0.6603 0.113 Uiso 1 1 calc R . . C52 C 0.4326(14) 0.0232(11) -0.5386(7) 0.090(4) Uiso 1 1 d . . . H52A H 0.4823 -0.0347 -0.5615 0.108 Uiso 1 1 calc R . . H52B H 0.3646 -0.0098 -0.5053 0.108 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 0.0331(2) 0.0432(3) 0.0488(3) -0.0070(2) -0.0076(2) -0.01226(19) Cl1 0.121(4) 0.098(3) 0.145(4) -0.027(3) -0.005(3) -0.021(3) Cl2 0.105(3) 0.129(4) 0.123(4) -0.005(3) 0.001(3) -0.030(3) N1 0.041(6) 0.043(6) 0.043(6) -0.008(5) -0.018(5) -0.006(5) N2 0.036(5) 0.048(6) 0.057(7) -0.022(6) 0.001(5) -0.010(5) N3 0.078(8) 0.067(8) 0.056(7) -0.020(6) 0.002(7) -0.024(7) N4 0.073(8) 0.046(7) 0.060(7) -0.008(6) 0.000(6) -0.027(6) N5 0.075(8) 0.061(8) 0.058(8) 0.024(6) 0.007(7) -0.005(7) N6 0.086(9) 0.086(9) 0.068(9) -0.016(7) -0.027(8) -0.009(7) N7 0.064(7) 0.072(8) 0.042(7) -0.013(6) -0.012(6) 0.003(6) N8 0.067(8) 0.074(8) 0.063(8) -0.021(7) 0.004(7) -0.005(7) C1 0.060(9) 0.068(10) 0.075(10) -0.018(8) -0.021(8) -0.015(8) C2 0.073(10) 0.074(10) 0.069(10) -0.011(8) -0.026(9) -0.003(9) C3 0.036(7) 0.096(12) 0.091(12) -0.044(10) -0.027(8) -0.002(8) C4 0.029(7) 0.082(10) 0.065(9) -0.034(8) -0.004(7) -0.006(7) C5 0.027(7) 0.122(13) 0.095(12) -0.071(11) -0.013(8) -0.014(9) C6 0.073(11) 0.090(12) 0.078(11) -0.038(9) 0.003(9) -0.034(10) C7 0.047(8) 0.080(10) 0.052(9) -0.029(8) -0.002(7) -0.023(8) C8 0.068(10) 0.079(11) 0.084(11) -0.037(9) 0.028(9) -0.052(9) C9 0.103(12) 0.061(10) 0.067(10) -0.017(8) 0.013(10) -0.043(10) C10 0.061(9) 0.048(8) 0.063(9) -0.003(7) -0.008(7) -0.017(7) C11 0.036(6) 0.061(8) 0.051(8) -0.024(7) 0.002(6) -0.028(6) C12 0.042(7) 0.054(8) 0.038(7) -0.012(6) -0.002(6) -0.011(6) C13 0.040(7) 0.066(9) 0.036(7) -0.004(7) -0.009(6) -0.017(7) C14 0.045(8) 0.070(10) 0.065(9) -0.017(8) -0.024(7) -0.006(7) C15 0.044(7) 0.044(8) 0.058(9) -0.005(7) -0.003(7) -0.020(6) C16 0.067(8) 0.071(9) 0.034(7) -0.003(7) -0.007(6) -0.037(7) C17 0.084(10) 0.064(9) 0.051(9) -0.014(7) -0.010(7) -0.036(8) C18 0.066(8) 0.045(8) 0.034(7) -0.002(6) -0.009(6) -0.016(7) C19 0.123(12) 0.054(9) 0.050(9) -0.001(7) -0.020(8) -0.044(9) C20 0.102(11) 0.063(9) 0.047(9) -0.004(7) -0.029(8) -0.036(8) C21 0.077(10) 0.043(8) 0.048(8) -0.004(7) 0.004(7) -0.021(8) C22 0.119(13) 0.060(10) 0.065(10) -0.003(8) -0.024(10) -0.048(10) C23 0.17(2) 0.084(13) 0.063(11) -0.020(10) 0.001(13) -0.055(14) C24 0.143(17) 0.134(16) 0.058(10) -0.006(12) 0.001(11) -0.115(15) C25 0.042(9) 0.146(16) 0.122(14) -0.052(12) 0.027(9) -0.029(10) C26 0.061(9) 0.060(9) 0.052(9) -0.018(8) 0.000(8) -0.018(8) C27 0.085(11) 0.052(9) 0.083(11) 0.001(8) 0.007(10) -0.027(9) C28 0.081(11) 0.078(11) 0.075(11) -0.021(9) 0.013(10) -0.011(10) C29 0.122(16) 0.068(11) 0.086(13) 0.011(10) -0.027(12) 0.011(11) C30 0.100(14) 0.082(13) 0.109(14) 0.001(11) 0.017(12) -0.029(11) C31 0.045(7) 0.039(8) 0.075(10) -0.020(7) 0.016(7) -0.018(6) C32 0.041(7) 0.066(9) 0.062(9) -0.013(8) -0.003(7) -0.011(7) C33 0.037(7) 0.056(9) 0.045(8) -0.007(7) -0.009(6) -0.007(6) C34 0.066(9) 0.040(7) 0.078(10) -0.019(7) -0.010(8) 0.000(7) C35 0.058(8) 0.061(9) 0.056(8) -0.016(7) -0.027(7) -0.002(7) C36 0.049(7) 0.045(8) 0.051(8) -0.007(7) -0.021(7) 0.005(6) C37 0.060(8) 0.045(8) 0.059(9) -0.005(7) -0.006(7) -0.009(7) C38 0.063(8) 0.060(9) 0.061(9) -0.015(8) -0.017(7) -0.018(7) C39 0.20(2) 0.094(14) 0.059(13) -0.014(11) -0.051(14) -0.029(14) C40 0.18(2) 0.117(17) 0.044(11) -0.029(11) -0.013(13) -0.003(15) C41 0.143(18) 0.127(16) 0.064(13) -0.035(12) 0.027(12) -0.019(14) C42 0.090(12) 0.086(11) 0.063(11) -0.025(9) 0.000(9) 0.018(9) C43 0.079(11) 0.055(9) 0.069(11) -0.016(8) -0.007(9) -0.015(8) C44 0.046(8) 0.055(9) 0.061(9) -0.015(8) -0.025(7) 0.001(7) C45 0.101(12) 0.057(10) 0.080(11) 0.012(9) -0.010(9) -0.009(9) C46 0.143(18) 0.038(10) 0.140(18) -0.020(12) -0.063(15) 0.030(11) C47 0.116(17) 0.128(19) 0.088(15) -0.046(15) 0.012(13) 0.000(15) C48 0.097(14) 0.098(14) 0.116(16) -0.052(14) 0.015(12) 0.009(13) C49 0.096(12) 0.126(14) 0.100(12) -0.054(11) 0.037(10) -0.051(11) _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 C13 1.903(12) . ? Pt1 C31 1.980(14) . ? Pt1 N1 2.059(8) . ? Pt1 N2 2.077(9) . ? Cl1 C49 1.707(14) . ? Cl2 C49 1.742(14) . ? N1 C1 1.300(13) . ? N1 C12 1.365(13) . ? N2 C10 1.328(12) . ? N2 C11 1.361(12) . ? N3 C21 1.333(14) . ? N3 C25 1.382(16) . ? N4 C26 1.387(14) . ? N4 C21 1.396(15) . ? N4 C18 1.414(13) . ? N5 C30 1.290(17) . ? N5 C26 1.299(14) . ? N6 C43 1.339(15) . ? N6 C39 1.344(17) . ? N7 C43 1.401(15) . ? N7 C36 1.415(13) . ? N7 C44 1.438(14) . ? N8 C44 1.317(14) . ? N8 C48 1.329(16) . ? C1 C2 1.419(16) . ? C2 C3 1.318(17) . ? C3 C4 1.389(16) . ? C4 C12 1.374(14) . ? C4 C5 1.465(17) . ? C5 C6 1.303(16) . ? C6 C7 1.383(17) . ? C7 C8 1.355(16) . ? C7 C11 1.410(15) . ? C8 C9 1.339(17) . ? C9 C10 1.380(16) . ? C11 C12 1.428(14) . ? C13 C14 1.222(15) . ? C14 C15 1.471(16) . ? C15 C20 1.384(14) . ? C15 C16 1.386(14) . ? C16 C17 1.394(14) . ? C17 C18 1.363(14) . ? C18 C19 1.360(15) . ? C19 C20 1.350(15) . ? C21 C22 1.387(16) . ? C22 C23 1.36(2) . ? C23 C24 1.38(2) . ? C24 C25 1.350(19) . ? C26 C27 1.361(16) . ? C27 C28 1.380(17) . ? C28 C29 1.353(18) . ? C29 C30 1.43(2) . ? C31 C32 1.194(14) . ? C32 C33 1.421(16) . ? C33 C38 1.313(14) . ? C33 C34 1.397(15) . ? C34 C35 1.360(14) . ? C35 C36 1.348(14) . ? C36 C37 1.363(15) . ? C37 C38 1.388(14) . ? C39 C40 1.34(2) . ? C40 C41 1.32(2) . ? C41 C42 1.375(18) . ? C42 C43 1.368(16) . ? C44 C45 1.337(16) . ? C45 C46 1.43(2) . ? C46 C47 1.35(2) . ? C47 C48 1.28(2) . ? C50 C51 1.325(16) . ? C51 C52 1.828(17) . ? C52 C52 1.97(2) 2_654 ? 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 C13 Pt1 C31 95.7(4) . . ? C13 Pt1 N1 93.8(4) . . ? C31 Pt1 N1 170.2(4) . . ? C13 Pt1 N2 173.4(4) . . ? C31 Pt1 N2 90.9(4) . . ? N1 Pt1 N2 79.5(4) . . ? C1 N1 C12 116.8(10) . . ? C1 N1 Pt1 128.4(9) . . ? C12 N1 Pt1 114.7(7) . . ? C10 N2 C11 118.8(10) . . ? C10 N2 Pt1 128.5(8) . . ? C11 N2 Pt1 112.7(7) . . ? C21 N3 C25 116.3(12) . . ? C26 N4 C21 119.8(10) . . ? C26 N4 C18 119.5(11) . . ? C21 N4 C18 120.5(11) . . ? C30 N5 C26 117.2(13) . . ? C43 N6 C39 119.3(15) . . ? C43 N7 C36 120.9(11) . . ? C43 N7 C44 121.0(11) . . ? C36 N7 C44 118.0(10) . . ? C44 N8 C48 117.7(14) . . ? N1 C1 C2 121.1(13) . . ? C3 C2 C1 121.1(13) . . ? C2 C3 C4 119.9(13) . . ? C12 C4 C3 115.9(12) . . ? C12 C4 C5 117.4(12) . . ? C3 C4 C5 126.7(13) . . ? C6 C5 C4 121.6(13) . . ? C5 C6 C7 122.8(15) . . ? C8 C7 C6 125.3(14) . . ? C8 C7 C11 116.5(12) . . ? C6 C7 C11 118.2(13) . . ? C9 C8 C7 122.0(13) . . ? C8 C9 C10 119.7(13) . . ? N2 C10 C9 121.2(13) . . ? N2 C11 C7 121.8(11) . . ? N2 C11 C12 118.0(10) . . ? C7 C11 C12 120.2(11) . . ? N1 C12 C4 125.2(11) . . ? N1 C12 C11 115.0(10) . . ? C4 C12 C11 119.8(11) . . ? C14 C13 Pt1 175.1(10) . . ? C13 C14 C15 177.4(14) . . ? C20 C15 C16 116.2(11) . . ? C20 C15 C14 122.5(11) . . ? C16 C15 C14 121.3(11) . . ? C15 C16 C17 120.8(11) . . ? C18 C17 C16 121.3(11) . . ? C19 C18 C17 117.4(12) . . ? C19 C18 N4 122.1(11) . . ? C17 C18 N4 120.4(11) . . ? C20 C19 C18 122.3(12) . . ? C19 C20 C15 122.0(12) . . ? N3 C21 C22 121.8(14) . . ? N3 C21 N4 116.3(11) . . ? C22 C21 N4 121.8(13) . . ? C23 C22 C21 119.7(16) . . ? C22 C23 C24 120.3(17) . . ? C25 C24 C23 116.8(17) . . ? C24 C25 N3 124.9(16) . . ? N5 C26 C27 123.4(13) . . ? N5 C26 N4 116.1(12) . . ? C27 C26 N4 120.5(13) . . ? C26 C27 C28 121.5(14) . . ? C29 C28 C27 115.3(15) . . ? C28 C29 C30 119.1(15) . . ? N5 C30 C29 123.5(15) . . ? C32 C31 Pt1 171.6(10) . . ? C31 C32 C33 177.2(13) . . ? C38 C33 C34 116.7(11) . . ? C38 C33 C32 120.6(12) . . ? C34 C33 C32 122.8(12) . . ? C35 C34 C33 121.5(12) . . ? C36 C35 C34 121.4(12) . . ? C35 C36 C37 117.2(11) . . ? C35 C36 N7 124.0(12) . . ? C37 C36 N7 118.8(11) . . ? C36 C37 C38 121.1(12) . . ? C33 C38 C37 122.1(12) . . ? C40 C39 N6 121.0(18) . . ? C41 C40 C39 121.4(18) . . ? C40 C41 C42 118.0(17) . . ? C43 C42 C41 120.6(15) . . ? N6 C43 C42 119.4(14) . . ? N6 C43 N7 118.3(13) . . ? C42 C43 N7 122.3(14) . . ? N8 C44 C45 124.5(13) . . ? N8 C44 N7 115.1(12) . . ? C45 C44 N7 120.4(14) . . ? C44 C45 C46 115.4(15) . . ? C47 C46 C45 118.1(16) . . ? C48 C47 C46 121(2) . . ? C47 C48 N8 123.1(19) . . ? Cl1 C49 Cl2 113.4(9) . . ? C50 C51 C52 120.2(12) . . ? C51 C52 C52 164.7(13) . 2_654 ? _diffrn_measured_fraction_theta_max 0.841 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.841 _refine_diff_density_max 1.758 _refine_diff_density_min -1.344 _refine_diff_density_rms 0.143