Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Christopher P. Newman' 'Gareth W. V. Cave' 'Michael Wong' 'William Errington' 'Nathaniel W. Alcock' 'Jonathan P. Rourke' _publ_contact_author_name 'Dr J Rourke' _publ_contact_author_address ; Dr J Rourke Department of Chemistry University of Warwick Coventry CV4 7AL U.K. ; _publ_contact_author_email 'J.ROURKE@WARWICK.AC.UK' _publ_section_title ; Di-metallated platinum carbonyl complexes: platinum-platinum interactions in the solid state ; data_1 _database_code_CSD 165976 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H35 N O3 Pt' _chemical_formula_weight 652.68 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0566(5) _cell_length_b 11.7161(6) _cell_length_c 13.8432(8) _cell_angle_alpha 68.7940(10) _cell_angle_beta 69.2180(10) _cell_angle_gamma 64.7360(10) _cell_volume 1335.75(12) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method ? _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 5.283 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART area-detector diffractometer' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7048 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4865 _reflns_number_observed 3993 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1996)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0357P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4865 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_obs 0.0354 _refine_ls_wR_factor_all 0.0749 _refine_ls_wR_factor_obs 0.0723 _refine_ls_goodness_of_fit_all 0.935 _refine_ls_goodness_of_fit_obs 1.004 _refine_ls_restrained_S_all 0.935 _refine_ls_restrained_S_obs 1.004 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.09481(2) 0.21349(2) 0.237959(17) 0.03696(9) Uani 1 d . . N1 N 0.2292(5) 0.2773(5) 0.2675(4) 0.0426(13) Uani 1 d . . O1 O 0.5079(4) -0.2146(4) 0.0942(3) 0.0537(12) Uani 1 d . . O2 O -0.4632(5) 0.5689(4) 0.3549(3) 0.0494(11) Uani 1 d . . C1 C 0.3030(7) 0.0764(6) 0.1925(4) 0.0426(15) Uani 1 d . . C2 C 0.3399(6) -0.0293(6) 0.1535(4) 0.0433(16) Uani 1 d . . H2 H 0.2617 -0.0465 0.1441 0.052 Uiso 1 calc R . C3 C 0.4894(7) -0.1112(7) 0.1276(5) 0.0464(16) Uani 1 d . . C4 C 0.6068(7) -0.0862(7) 0.1392(5) 0.0536(18) Uani 1 d . . H4 H 0.7090 -0.1413 0.1213 0.064 Uiso 1 calc R . C5 C 0.5711(7) 0.0197(7) 0.1768(5) 0.0503(17) Uani 1 d . . H5 H 0.6503 0.0374 0.1843 0.060 Uiso 1 calc R . C6 C 0.4247(6) 0.1004(6) 0.2038(4) 0.0428(15) Uani 1 d . . C7 C 0.3825(7) 0.2109(7) 0.2451(5) 0.0494(17) Uani 1 d . . C8 C 0.4740(8) 0.2575(8) 0.2642(5) 0.0594(19) Uani 1 d . . H8 H 0.5807 0.2154 0.2483 0.071 Uiso 1 calc R . C9 C 0.4110(8) 0.3652(8) 0.3064(6) 0.069(2) Uani 1 d . . H9 H 0.4746 0.3952 0.3206 0.083 Uiso 1 calc R . C10 C 0.2534(7) 0.4302(7) 0.3282(5) 0.0570(18) Uani 1 d . . H10 H 0.2105 0.5042 0.3569 0.068 Uiso 1 calc R . C11 C 0.1619(7) 0.3862(6) 0.3078(5) 0.0449(15) Uani 1 d . . C12 C -0.0009(7) 0.4382(6) 0.3221(4) 0.0415(15) Uani 1 d . . C13 C -0.0937(7) 0.5487(7) 0.3623(5) 0.0500(17) Uani 1 d . . H13 H -0.0490 0.5911 0.3822 0.060 Uiso 1 calc R . C14 C -0.2473(7) 0.5965(6) 0.3734(5) 0.0461(15) Uani 1 d . . H14 H -0.3079 0.6724 0.3992 0.055 Uiso 1 calc R . C15 C -0.3134(7) 0.5337(6) 0.3469(4) 0.0412(15) Uani 1 d . . C16 C -0.2228(6) 0.4240(6) 0.3080(4) 0.0397(14) Uani 1 d . . H16 H -0.2704 0.3822 0.2901 0.048 Uiso 1 calc R . C17 C -0.0656(7) 0.3714(6) 0.2936(4) 0.0402(15) Uani 1 d . . C101 C 0.6577(7) -0.3037(7) 0.0671(5) 0.0535(18) Uani 1 d . . H10A H 0.7052 -0.3404 0.1283 0.064 Uiso 1 calc R . H10B H 0.7206 -0.2587 0.0058 0.064 Uiso 1 calc R . C102 C 0.6455(7) -0.4101(7) 0.0388(5) 0.058(2) Uani 1 d . . H10C H 0.5912 -0.3711 -0.0190 0.070 Uiso 1 calc R . H10D H 0.5850 -0.4559 0.1017 0.070 Uiso 1 calc R . C103 C 0.8002(7) -0.5094(7) 0.0025(5) 0.0553(19) Uani 1 d . . H10E H 0.8611 -0.4632 -0.0598 0.066 Uiso 1 calc R . H10F H 0.8539 -0.5489 0.0607 0.066 Uiso 1 calc R . C104 C 0.7899(7) -0.6156(7) -0.0273(5) 0.0573(18) Uani 1 d . . H10G H 0.7304 -0.5756 -0.0822 0.069 Uiso 1 calc R . H10H H 0.7342 -0.6649 0.0363 0.069 Uiso 1 calc R . C105 C 0.9441(8) -0.7115(7) -0.0703(5) 0.064(2) Uani 1 d . . H10I H 1.0005 -0.6626 -0.1337 0.076 Uiso 1 calc R . H10J H 1.0034 -0.7528 -0.0153 0.076 Uiso 1 calc R . C106 C 0.9295(10) -0.8175(9) -0.1009(7) 0.095(3) Uani 1 d . . H10K H 0.8794 -0.8697 -0.0375 0.142 Uiso 1 calc R . H10L H 1.0305 -0.8737 -0.1304 0.142 Uiso 1 calc R . H10M H 0.8694 -0.7772 -0.1545 0.142 Uiso 1 calc R . C201 C -0.5671(7) 0.6833(6) 0.3921(5) 0.0441(15) Uani 1 d . . H20A H -0.5396 0.7608 0.3460 0.053 Uiso 1 calc R . H20B H -0.5655 0.6721 0.4661 0.053 Uiso 1 calc R . C202 C -0.7205(6) 0.6988(6) 0.3875(5) 0.0463(16) Uani 1 d . . H20C H -0.7429 0.6182 0.4313 0.056 Uiso 1 calc R . H20D H -0.7187 0.7089 0.3129 0.056 Uiso 1 calc R . C203 C -0.8475(7) 0.8145(6) 0.4265(5) 0.0431(15) Uani 1 d . . H20E H -0.8269 0.8957 0.3820 0.052 Uiso 1 calc R . H20F H -0.8496 0.8053 0.5009 0.052 Uiso 1 calc R . C204 C -1.0019(7) 0.8251(6) 0.4216(5) 0.0492(16) Uani 1 d . . H20G H -1.0011 0.8398 0.3463 0.059 Uiso 1 calc R . H20H H -1.0186 0.7414 0.4618 0.059 Uiso 1 calc R . C205 C -1.1326(7) 0.9338(7) 0.4664(5) 0.0524(17) Uani 1 d . . H20I H -1.1164 1.0176 0.4255 0.063 Uiso 1 calc R . H20J H -1.1323 0.9197 0.5413 0.063 Uiso 1 calc R . C206 C -1.2873(7) 0.9440(8) 0.4632(6) 0.071(2) Uani 1 d . . H20K H -1.3033 0.8607 0.5017 0.107 Uiso 1 calc R . H20L H -1.2918 0.9652 0.3889 0.107 Uiso 1 calc R . H20M H -1.3662 1.0127 0.4970 0.107 Uiso 1 calc R . C18 C -0.0289(7) 0.1542(6) 0.2140(5) 0.0398(14) Uani 1 d . . O3 O -0.1067(5) 0.1171(5) 0.1983(3) 0.0556(12) Uani 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 0.02890(12) 0.04400(15) 0.03519(13) -0.00649(9) -0.00690(9) -0.01330(10) N1 0.034(3) 0.056(3) 0.045(3) -0.006(3) -0.013(2) -0.024(3) O1 0.033(2) 0.054(3) 0.059(3) -0.018(2) -0.009(2) 0.001(2) O2 0.038(2) 0.046(3) 0.062(3) -0.023(2) -0.011(2) -0.006(2) C1 0.036(3) 0.051(4) 0.032(3) -0.002(3) -0.005(3) -0.016(3) C2 0.029(3) 0.047(4) 0.043(3) -0.007(3) -0.006(3) -0.008(3) C3 0.039(4) 0.049(4) 0.037(3) -0.008(3) -0.004(3) -0.009(3) C4 0.028(3) 0.067(5) 0.048(4) -0.008(3) -0.006(3) -0.007(3) C5 0.034(3) 0.059(5) 0.053(4) -0.009(3) -0.009(3) -0.017(3) C6 0.032(3) 0.047(4) 0.038(3) -0.008(3) -0.005(3) -0.009(3) C7 0.035(3) 0.060(5) 0.041(3) 0.000(3) -0.004(3) -0.021(3) C8 0.032(3) 0.079(5) 0.068(5) -0.019(4) -0.008(3) -0.022(4) C9 0.047(4) 0.091(6) 0.081(5) -0.017(5) -0.014(4) -0.039(4) C10 0.051(4) 0.066(5) 0.066(4) -0.023(4) -0.010(3) -0.028(4) C11 0.046(4) 0.049(4) 0.042(3) -0.007(3) -0.006(3) -0.025(3) C12 0.039(3) 0.053(4) 0.034(3) -0.007(3) -0.007(3) -0.022(3) C13 0.054(4) 0.058(4) 0.049(4) -0.010(3) -0.011(3) -0.033(4) C14 0.048(4) 0.039(4) 0.047(4) -0.016(3) -0.002(3) -0.015(3) C15 0.039(3) 0.042(4) 0.036(3) -0.006(3) -0.008(3) -0.012(3) C16 0.040(3) 0.041(4) 0.038(3) -0.003(3) -0.013(3) -0.017(3) C17 0.042(3) 0.042(4) 0.034(3) -0.002(3) -0.008(3) -0.017(3) C101 0.032(3) 0.057(4) 0.048(4) -0.006(3) -0.008(3) -0.001(3) C102 0.037(4) 0.064(5) 0.047(4) -0.007(3) -0.008(3) 0.000(3) C103 0.037(3) 0.063(5) 0.042(3) -0.011(3) -0.004(3) -0.002(3) C104 0.046(4) 0.058(5) 0.055(4) -0.012(3) -0.014(3) -0.007(4) C105 0.057(4) 0.064(5) 0.050(4) -0.021(4) -0.009(3) -0.001(4) C106 0.097(7) 0.096(7) 0.095(6) -0.058(6) -0.024(5) -0.007(6) C201 0.043(4) 0.042(4) 0.043(3) -0.015(3) -0.006(3) -0.010(3) C202 0.043(4) 0.042(4) 0.047(4) -0.015(3) -0.004(3) -0.010(3) C203 0.047(4) 0.036(3) 0.039(3) -0.013(3) -0.004(3) -0.009(3) C204 0.047(4) 0.049(4) 0.045(3) -0.009(3) -0.006(3) -0.016(3) C205 0.047(4) 0.055(4) 0.042(3) -0.016(3) -0.002(3) -0.009(3) C206 0.038(4) 0.075(5) 0.073(5) -0.012(4) -0.009(3) -0.003(4) C18 0.032(3) 0.042(4) 0.043(3) -0.010(3) -0.008(3) -0.012(3) O3 0.043(3) 0.066(3) 0.063(3) -0.017(2) -0.017(2) -0.019(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C18 1.827(6) . ? Pt1 N1 2.007(5) . ? Pt1 C17 2.055(6) . ? Pt1 C1 2.070(6) . ? N1 C7 1.375(7) . ? N1 C11 1.381(8) . ? O1 C3 1.366(8) . ? O1 C101 1.428(7) . ? O2 C15 1.356(7) . ? O2 C201 1.441(7) . ? C1 C2 1.383(9) . ? C1 C6 1.437(8) . ? C2 C3 1.394(8) . ? C3 C4 1.403(9) . ? C4 C5 1.377(9) . ? C5 C6 1.371(8) . ? C6 C7 1.441(9) . ? C7 C8 1.386(9) . ? C8 C9 1.386(10) . ? C9 C10 1.407(9) . ? C10 C11 1.374(9) . ? C11 C12 1.448(8) . ? C12 C13 1.407(9) . ? C12 C17 1.425(8) . ? C13 C14 1.371(8) . ? C14 C15 1.380(8) . ? C15 C16 1.388(8) . ? C16 C17 1.397(7) . ? C101 C102 1.496(10) . ? C102 C103 1.533(8) . ? C103 C104 1.498(9) . ? C104 C105 1.537(9) . ? C105 C106 1.523(11) . ? C201 C202 1.496(8) . ? C202 C203 1.524(8) . ? C203 C204 1.528(8) . ? C204 C205 1.516(8) . ? C205 C206 1.524(9) . ? C18 O3 1.152(7) . ? 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 C18 Pt1 N1 178.8(2) . . ? C18 Pt1 C17 99.3(2) . . ? N1 Pt1 C17 80.4(2) . . ? C18 Pt1 C1 100.1(3) . . ? N1 Pt1 C1 80.2(2) . . ? C17 Pt1 C1 160.6(2) . . ? C7 N1 C11 124.1(5) . . ? C7 N1 Pt1 118.0(5) . . ? C11 N1 Pt1 117.9(4) . . ? C3 O1 C101 118.3(5) . . ? C15 O2 C201 119.2(5) . . ? C2 C1 C6 117.6(5) . . ? C2 C1 Pt1 130.4(5) . . ? C6 C1 Pt1 111.9(5) . . ? C1 C2 C3 121.4(6) . . ? O1 C3 C2 114.9(6) . . ? O1 C3 C4 124.9(6) . . ? C2 C3 C4 120.2(7) . . ? C5 C4 C3 118.7(6) . . ? C6 C5 C4 122.0(6) . . ? C5 C6 C1 120.1(6) . . ? C5 C6 C7 123.6(6) . . ? C1 C6 C7 116.3(5) . . ? N1 C7 C8 117.3(6) . . ? N1 C7 C6 113.6(6) . . ? C8 C7 C6 129.2(6) . . ? C9 C8 C7 120.5(6) . . ? C8 C9 C10 120.3(7) . . ? C11 C10 C9 119.6(7) . . ? C10 C11 N1 118.1(6) . . ? C10 C11 C12 129.2(6) . . ? N1 C11 C12 112.7(6) . . ? C13 C12 C17 120.4(5) . . ? C13 C12 C11 122.9(6) . . ? C17 C12 C11 116.7(6) . . ? C14 C13 C12 121.4(6) . . ? C13 C14 C15 119.6(6) . . ? O2 C15 C14 126.0(6) . . ? O2 C15 C16 114.6(6) . . ? C14 C15 C16 119.4(6) . . ? C15 C16 C17 123.8(6) . . ? C16 C17 C12 115.5(6) . . ? C16 C17 Pt1 132.2(5) . . ? C12 C17 Pt1 112.3(4) . . ? O1 C101 C102 107.5(5) . . ? C101 C102 C103 112.7(6) . . ? C104 C103 C102 113.3(6) . . ? C103 C104 C105 114.1(6) . . ? C106 C105 C104 112.8(7) . . ? O2 C201 C202 106.2(5) . . ? C201 C202 C203 114.0(5) . . ? C202 C203 C204 112.0(5) . . ? C205 C204 C203 113.7(6) . . ? C204 C205 C206 114.1(6) . . ? O3 C18 Pt1 179.6(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 C18 Pt1 N1 C7 108(11) . . . . ? C17 Pt1 N1 C7 -179.0(4) . . . . ? C1 Pt1 N1 C7 1.1(4) . . . . ? C18 Pt1 N1 C11 -73(12) . . . . ? C17 Pt1 N1 C11 0.1(4) . . . . ? C1 Pt1 N1 C11 -179.7(4) . . . . ? C18 Pt1 C1 C2 0.8(6) . . . . ? N1 Pt1 C1 C2 179.7(6) . . . . ? C17 Pt1 C1 C2 179.3(5) . . . . ? C18 Pt1 C1 C6 -179.9(4) . . . . ? N1 Pt1 C1 C6 -1.1(4) . . . . ? C17 Pt1 C1 C6 -1.4(8) . . . . ? C6 C1 C2 C3 1.0(8) . . . . ? Pt1 C1 C2 C3 -179.7(4) . . . . ? C101 O1 C3 C2 -179.5(5) . . . . ? C101 O1 C3 C4 -1.0(8) . . . . ? C1 C2 C3 O1 177.5(5) . . . . ? C1 C2 C3 C4 -1.1(9) . . . . ? O1 C3 C4 C5 -178.0(6) . . . . ? C2 C3 C4 C5 0.4(9) . . . . ? C3 C4 C5 C6 0.4(9) . . . . ? C4 C5 C6 C1 -0.5(9) . . . . ? C4 C5 C6 C7 178.9(6) . . . . ? C2 C1 C6 C5 -0.3(8) . . . . ? Pt1 C1 C6 C5 -179.6(4) . . . . ? C2 C1 C6 C7 -179.7(5) . . . . ? Pt1 C1 C6 C7 0.9(6) . . . . ? C11 N1 C7 C8 -0.2(8) . . . . ? Pt1 N1 C7 C8 178.9(5) . . . . ? C11 N1 C7 C6 -180.0(5) . . . . ? Pt1 N1 C7 C6 -0.9(6) . . . . ? C5 C6 C7 N1 -179.5(5) . . . . ? C1 C6 C7 N1 -0.1(7) . . . . ? C5 C6 C7 C8 0.8(10) . . . . ? C1 C6 C7 C8 -179.8(6) . . . . ? N1 C7 C8 C9 1.3(9) . . . . ? C6 C7 C8 C9 -178.9(6) . . . . ? C7 C8 C9 C10 -1.4(11) . . . . ? C8 C9 C10 C11 0.2(10) . . . . ? C9 C10 C11 N1 0.9(9) . . . . ? C9 C10 C11 C12 -178.9(6) . . . . ? C7 N1 C11 C10 -1.0(8) . . . . ? Pt1 N1 C11 C10 180.0(4) . . . . ? C7 N1 C11 C12 178.9(5) . . . . ? Pt1 N1 C11 C12 -0.1(6) . . . . ? C10 C11 C12 C13 -0.3(10) . . . . ? N1 C11 C12 C13 179.9(5) . . . . ? C10 C11 C12 C17 179.9(6) . . . . ? N1 C11 C12 C17 0.1(7) . . . . ? C17 C12 C13 C14 -1.2(9) . . . . ? C11 C12 C13 C14 179.0(5) . . . . ? C12 C13 C14 C15 1.4(9) . . . . ? C201 O2 C15 C14 1.3(8) . . . . ? C201 O2 C15 C16 -178.6(5) . . . . ? C13 C14 C15 O2 179.2(5) . . . . ? C13 C14 C15 C16 -0.9(9) . . . . ? O2 C15 C16 C17 180.0(5) . . . . ? C14 C15 C16 C17 0.1(8) . . . . ? C15 C16 C17 C12 0.2(8) . . . . ? C15 C16 C17 Pt1 -179.7(4) . . . . ? C13 C12 C17 C16 0.4(8) . . . . ? C11 C12 C17 C16 -179.8(5) . . . . ? C13 C12 C17 Pt1 -179.7(4) . . . . ? C11 C12 C17 Pt1 0.1(6) . . . . ? C18 Pt1 C17 C16 -1.4(5) . . . . ? N1 Pt1 C17 C16 179.7(5) . . . . ? C1 Pt1 C17 C16 -179.9(5) . . . . ? C18 Pt1 C17 C12 178.7(4) . . . . ? N1 Pt1 C17 C12 -0.1(4) . . . . ? C1 Pt1 C17 C12 0.2(8) . . . . ? C3 O1 C101 C102 177.2(5) . . . . ? O1 C101 C102 C103 177.1(5) . . . . ? C101 C102 C103 C104 -179.3(5) . . . . ? C102 C103 C104 C105 176.5(5) . . . . ? C103 C104 C105 C106 -179.4(6) . . . . ? C15 O2 C201 C202 177.7(5) . . . . ? O2 C201 C202 C203 178.8(5) . . . . ? C201 C202 C203 C204 -179.2(5) . . . . ? C202 C203 C204 C205 176.2(5) . . . . ? C203 C204 C205 C206 -179.2(5) . . . . ? N1 Pt1 C18 O3 174(100) . . . . ? C17 Pt1 C18 O3 101(79) . . . . ? C1 Pt1 C18 O3 -80(79) . . . . ? _refine_diff_density_max 1.911 _refine_diff_density_min -1.671 _refine_diff_density_rms 0.127 #===END data_2 _database_code_CSD 165977 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H31 N O2 Pt' _chemical_formula_weight 656.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.1213(4) _cell_length_b 19.17320(10) _cell_length_c 17.0303(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.5690(10) _cell_angle_gamma 90.00 _cell_volume 10397.0(2) _cell_formula_units_Z 16 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6384 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min ?0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5184 _exptl_absorpt_coefficient_mu 5.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 32811 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 29.20 _reflns_number_total 12731 _reflns_number_gt 7326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0297P)^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 12731 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.002 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 0.244419(6) 0.005941(9) -0.111485(12) 0.02974(6) Uani 1 1 d . . . Pt2 Pt 0.303615(6) -0.003991(10) 0.057798(12) 0.03024(6) Uani 1 1 d . . . C11 C 0.21834(18) 0.0851(3) -0.0820(3) 0.0364(14) Uani 1 1 d . . . C13 C 0.26528(18) 0.0692(3) 0.0993(3) 0.0339(14) Uani 1 1 d . . . C14 C 0.22963(19) 0.0624(3) 0.1379(3) 0.0397(15) Uani 1 1 d . . . H14A H 0.2207 0.0170 0.1504 0.048 Uiso 1 1 calc R . . C15 C 0.2069(2) 0.1194(3) 0.1586(4) 0.0506(17) Uani 1 1 d . . . H15A H 0.1827 0.1128 0.1842 0.061 Uiso 1 1 calc R . . C16 C 0.22003(19) 0.1871(3) 0.1416(4) 0.0469(17) Uani 1 1 d . . . H16A H 0.2045 0.2264 0.1555 0.056 Uiso 1 1 calc R . . C17 C 0.25528(19) 0.1964(3) 0.1048(4) 0.0427(16) Uani 1 1 d . . . H17A H 0.2641 0.2422 0.0937 0.051 Uiso 1 1 calc R . . C18 C 0.27814(17) 0.1394(3) 0.0838(3) 0.0303(13) Uani 1 1 d . . . C19 C 0.31585(17) 0.1457(2) 0.0440(3) 0.0300(13) Uani 1 1 d . . . C21 C 0.27882(18) -0.0836(3) 0.0907(3) 0.0347(14) Uani 1 1 d . . . O22 O 0.26505(14) -0.13297(19) 0.1135(3) 0.0525(12) Uani 1 1 d . . . C110 C 0.36712(17) 0.0764(2) -0.0101(3) 0.0323(13) Uani 1 1 d . . . N110 N 0.33199(14) 0.08272(19) 0.0263(3) 0.0288(10) Uani 1 1 d . . . C112 C 0.38757(17) 0.1362(2) -0.0297(3) 0.0350(14) Uani 1 1 d . . . H11A H 0.4122 0.1325 -0.0547 0.042 Uiso 1 1 calc R . . C113 C 0.37230(17) 0.2020(2) -0.0130(3) 0.0312(13) Uani 1 1 d . . . C114 C 0.33611(17) 0.2062(2) 0.0238(3) 0.0341(14) Uani 1 1 d . . . H11B H 0.3252 0.2506 0.0352 0.041 Uiso 1 1 calc R . . C115 C 0.37852(16) 0.0025(2) -0.0221(3) 0.0329(12) Uani 1 1 d . . . C116 C 0.35179(17) -0.0481(2) 0.0056(3) 0.0326(13) Uani 1 1 d . . . C117 C 0.36124(18) -0.1178(2) -0.0062(3) 0.0377(15) Uani 1 1 d . . . H11C H 0.3443 -0.1531 0.0128 0.045 Uiso 1 1 calc R . . C118 C 0.3949(2) -0.1371(3) -0.0452(4) 0.0444(17) Uani 1 1 d . . . H11D H 0.4004 -0.1851 -0.0534 0.053 Uiso 1 1 calc R . . C119 C 0.4202(2) -0.0865(3) -0.0719(4) 0.0491(17) Uani 1 1 d . . . H11E H 0.4433 -0.1000 -0.0980 0.059 Uiso 1 1 calc R . . C120 C 0.41231(18) -0.0159(3) -0.0613(3) 0.0420(15) Uani 1 1 d . . . H12A H 0.4296 0.0188 -0.0803 0.050 Uiso 1 1 calc R . . C121 C 0.39430(17) 0.2669(2) -0.0332(3) 0.0349(14) Uani 1 1 d . . . C122 C 0.42325(19) 0.2669(3) -0.0870(4) 0.0460(16) Uani 1 1 d . . . H12B H 0.4292 0.2242 -0.1117 0.055 Uiso 1 1 calc R . . C123 C 0.44365(19) 0.3265(3) -0.1059(4) 0.0466(16) Uani 1 1 d . . . H12C H 0.4634 0.3241 -0.1427 0.056 Uiso 1 1 calc R . . C124 C 0.43575(19) 0.3901(3) -0.0718(4) 0.0398(15) Uani 1 1 d . . . C125 C 0.40707(19) 0.3920(3) -0.0173(4) 0.0506(18) Uani 1 1 d . . . H12D H 0.4010 0.4347 0.0069 0.061 Uiso 1 1 calc R . . C126 C 0.38742(18) 0.3305(3) 0.0013(4) 0.0518(18) Uani 1 1 d . . . H12E H 0.3684 0.3324 0.0395 0.062 Uiso 1 1 calc R . . O127 O 0.45699(13) 0.44548(18) -0.0949(3) 0.0528(12) Uani 1 1 d . . . C128 C 0.44739(19) 0.5143(2) -0.0694(4) 0.0481(16) Uani 1 1 d . . . H12F H 0.4538 0.5181 -0.0111 0.058 Uiso 1 1 calc R . . H12G H 0.4173 0.5248 -0.0849 0.058 Uiso 1 1 calc R . . C129 C 0.4743(2) 0.5646(3) -0.1092(4) 0.0489(17) Uani 1 1 d . . . H12H H 0.4669 0.5603 -0.1673 0.059 Uiso 1 1 calc R . . H12I H 0.5041 0.5506 -0.0962 0.059 Uiso 1 1 calc R . . C130 C 0.47032(19) 0.6406(2) -0.0866(4) 0.0440(15) Uani 1 1 d . . . H13A H 0.4759 0.6453 -0.0283 0.053 Uiso 1 1 calc R . . H13B H 0.4413 0.6567 -0.1040 0.053 Uiso 1 1 calc R . . C131 C 0.50097(19) 0.6859(2) -0.1245(4) 0.0425(15) Uani 1 1 d . . . H13C H 0.5298 0.6707 -0.1039 0.051 Uiso 1 1 calc R . . H13D H 0.4968 0.6768 -0.1822 0.051 Uiso 1 1 calc R . . C132 C 0.49823(17) 0.7640(2) -0.1120(3) 0.0393(14) Uani 1 1 d . . . H13E H 0.5005 0.7738 -0.0546 0.047 Uiso 1 1 calc R . . H13F H 0.4705 0.7809 -0.1371 0.047 Uiso 1 1 calc R . . C133 C 0.53255(17) 0.8032(3) -0.1467(3) 0.0369(15) Uani 1 1 d . . . H13G H 0.5310 0.7906 -0.2034 0.044 Uiso 1 1 calc R . . H13H H 0.5600 0.7869 -0.1199 0.044 Uiso 1 1 calc R . . C134 C 0.53125(18) 0.8824(3) -0.1404(4) 0.0417(15) Uani 1 1 d . . . H13I H 0.5330 0.8956 -0.0839 0.050 Uiso 1 1 calc R . . H13J H 0.5040 0.8993 -0.1676 0.050 Uiso 1 1 calc R . . C135 C 0.56681(19) 0.9182(3) -0.1766(4) 0.0490(17) Uani 1 1 d . . . H13K H 0.5643 0.9689 -0.1712 0.074 Uiso 1 1 calc R . . H13L H 0.5650 0.9059 -0.2328 0.074 Uiso 1 1 calc R . . H13M H 0.5939 0.9027 -0.1488 0.074 Uiso 1 1 calc R . . O21 O 0.20170(14) 0.1343(2) -0.0654(3) 0.0548(13) Uani 1 1 d . . . C23 C 0.28889(17) 0.0514(2) -0.1716(3) 0.0334(14) Uani 1 1 d . . . C24 C 0.29882(18) 0.1221(3) -0.1828(3) 0.0381(15) Uani 1 1 d . . . H24A H 0.2821 0.1573 -0.1633 0.046 Uiso 1 1 calc R . . C25 C 0.3325(2) 0.1415(3) -0.2217(4) 0.0442(17) Uani 1 1 d . . . H25A H 0.3390 0.1895 -0.2268 0.053 Uiso 1 1 calc R . . C26 C 0.35626(18) 0.0917(3) -0.2526(3) 0.0427(15) Uani 1 1 d . . . H26A H 0.3790 0.1052 -0.2798 0.051 Uiso 1 1 calc R . . C27 C 0.34725(17) 0.0227(3) -0.2443(3) 0.0360(13) Uani 1 1 d . . . H27A H 0.3637 -0.0115 -0.2662 0.043 Uiso 1 1 calc R . . C28 C 0.31444(16) 0.0020(2) -0.2043(3) 0.0305(11) Uani 1 1 d . . . N29 N 0.27149(13) -0.08026(19) -0.1485(3) 0.0277(10) Uani 1 1 d . . . C29 C 0.30392(17) -0.0723(2) -0.1922(3) 0.0312(13) Uani 1 1 d . . . C210 C 0.25730(16) -0.1435(2) -0.1288(3) 0.0293(13) Uani 1 1 d . . . C211 C 0.27683(17) -0.2025(2) -0.1521(3) 0.0319(13) Uani 1 1 d . . . H21A H 0.2676 -0.2471 -0.1372 0.038 Uiso 1 1 calc R . . C212 C 0.31004(18) -0.1977(2) -0.1973(3) 0.0335(14) Uani 1 1 d . . . C213 C 0.32240(18) -0.1308(2) -0.2173(3) 0.0336(14) Uani 1 1 d . . . H21B H 0.3443 -0.1260 -0.2494 0.040 Uiso 1 1 calc R . . C215 C 0.22245(17) -0.1385(2) -0.0808(3) 0.0295(13) Uani 1 1 d . . . C216 C 0.20965(17) -0.0693(3) -0.0638(3) 0.0302(13) Uani 1 1 d . . . C217 C 0.17731(17) -0.0636(3) -0.0158(3) 0.0355(14) Uani 1 1 d . . . H21C H 0.1679 -0.0185 -0.0032 0.043 Uiso 1 1 calc R . . C218 C 0.15883(18) -0.1213(3) 0.0137(3) 0.0397(14) Uani 1 1 d . . . H21D H 0.1372 -0.1154 0.0461 0.048 Uiso 1 1 calc R . . C219 C 0.17185(18) -0.1881(3) -0.0040(3) 0.0405(15) Uani 1 1 d . . . H21E H 0.1593 -0.2278 0.0166 0.049 Uiso 1 1 calc R . . C220 C 0.20319(18) -0.1963(3) -0.0519(3) 0.0400(15) Uani 1 1 d . . . H22A H 0.2116 -0.2419 -0.0650 0.048 Uiso 1 1 calc R . . C221 C 0.33140(16) -0.2613(2) -0.2212(3) 0.0294(12) Uani 1 1 d . . . C222 C 0.31365(18) -0.3270(2) -0.2200(3) 0.0387(14) Uani 1 1 d . . . H22B H 0.2865 -0.3313 -0.2042 0.046 Uiso 1 1 calc R . . C223 C 0.33390(18) -0.3870(2) -0.2409(3) 0.0372(14) Uani 1 1 d . . . H22C H 0.3209 -0.4313 -0.2386 0.045 Uiso 1 1 calc R . . C224 C 0.37314(18) -0.3815(2) -0.2650(3) 0.0376(14) Uani 1 1 d . . . C225 C 0.39198(19) -0.3165(3) -0.2669(4) 0.0545(19) Uani 1 1 d . . . H22D H 0.4192 -0.3126 -0.2827 0.065 Uiso 1 1 calc R . . C226 C 0.37140(18) -0.2574(3) -0.2459(4) 0.0470(17) Uani 1 1 d . . . H22E H 0.3846 -0.2132 -0.2482 0.056 Uiso 1 1 calc R . . O227 O 0.39589(12) -0.43604(17) -0.2888(3) 0.0504(12) Uani 1 1 d . . . C228 C 0.38066(18) -0.5059(2) -0.2828(4) 0.0440(14) Uani 1 1 d . . . H22F H 0.3528 -0.5111 -0.3147 0.053 Uiso 1 1 calc R . . H22G H 0.3779 -0.5172 -0.2269 0.053 Uiso 1 1 calc R . . C229 C 0.41213(19) -0.5536(2) -0.3134(4) 0.0488(17) Uani 1 1 d . . . H22H H 0.4400 -0.5459 -0.2823 0.059 Uiso 1 1 calc R . . H22I H 0.4143 -0.5414 -0.3692 0.059 Uiso 1 1 calc R . . C230 C 0.40078(18) -0.6307(2) -0.3091(4) 0.0414(15) Uani 1 1 d . . . H23A H 0.3975 -0.6432 -0.2539 0.050 Uiso 1 1 calc R . . H23B H 0.3737 -0.6396 -0.3427 0.050 Uiso 1 1 calc R . . C231 C 0.43491(19) -0.6755(2) -0.3372(4) 0.0475(16) Uani 1 1 d . . . H23C H 0.4621 -0.6634 -0.3056 0.057 Uiso 1 1 calc R . . H23D H 0.4370 -0.6636 -0.3931 0.057 Uiso 1 1 calc R . . C232 C 0.42827(18) -0.7544(2) -0.3315(3) 0.0401(14) Uani 1 1 d . . . H23E H 0.4260 -0.7669 -0.2759 0.048 Uiso 1 1 calc R . . H23F H 0.4015 -0.7673 -0.3641 0.048 Uiso 1 1 calc R . . C233 C 0.46407(19) -0.7959(3) -0.3596(4) 0.0460(17) Uani 1 1 d . . . H23G H 0.4653 -0.7844 -0.4159 0.055 Uiso 1 1 calc R . . H23H H 0.4908 -0.7803 -0.3290 0.055 Uiso 1 1 calc R . . C234 C 0.46098(19) -0.8743(3) -0.3518(4) 0.0458(16) Uani 1 1 d . . . H23I H 0.4344 -0.8905 -0.3825 0.055 Uiso 1 1 calc R . . H23J H 0.4602 -0.8864 -0.2955 0.055 Uiso 1 1 calc R . . C235 C 0.4979(2) -0.9122(3) -0.3814(4) 0.0588(19) Uani 1 1 d . . . H23K H 0.4945 -0.9627 -0.3753 0.088 Uiso 1 1 calc R . . H23L H 0.5242 -0.8971 -0.3504 0.088 Uiso 1 1 calc R . . H23M H 0.4985 -0.9011 -0.4374 0.088 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 0.02998(12) 0.01923(10) 0.04182(13) -0.00165(10) 0.01142(9) 0.00227(9) Pt2 0.03002(12) 0.01967(10) 0.04257(13) 0.00083(9) 0.01058(9) -0.00257(9) C11 0.028(4) 0.036(3) 0.048(4) -0.001(3) 0.014(3) -0.004(3) C13 0.033(4) 0.025(3) 0.044(4) 0.000(2) 0.009(3) -0.003(2) C14 0.042(4) 0.028(3) 0.052(4) -0.002(3) 0.019(3) -0.009(3) C15 0.053(4) 0.035(3) 0.070(5) -0.002(3) 0.030(4) -0.003(3) C16 0.050(4) 0.027(3) 0.071(5) -0.010(3) 0.035(4) -0.003(3) C17 0.050(4) 0.022(3) 0.060(4) -0.005(3) 0.021(3) -0.004(3) C18 0.029(3) 0.027(3) 0.036(3) -0.002(2) 0.009(3) -0.004(2) C19 0.029(3) 0.023(2) 0.039(3) -0.004(2) 0.007(3) -0.002(2) C21 0.037(4) 0.025(3) 0.043(4) -0.002(2) 0.010(3) 0.002(2) O22 0.063(3) 0.031(2) 0.067(3) 0.011(2) 0.023(2) -0.011(2) C110 0.029(3) 0.026(3) 0.041(4) 0.002(2) 0.004(3) 0.000(2) N110 0.029(3) 0.019(2) 0.039(3) 0.0000(19) 0.009(2) -0.0028(18) C112 0.026(3) 0.026(3) 0.055(4) 0.003(3) 0.010(3) -0.004(2) C113 0.027(3) 0.024(2) 0.043(4) 0.003(2) 0.008(3) 0.002(2) C114 0.033(3) 0.018(2) 0.051(4) -0.007(2) 0.006(3) 0.001(2) C115 0.034(3) 0.023(2) 0.043(3) -0.001(3) 0.009(2) -0.001(2) C116 0.037(4) 0.027(3) 0.035(3) -0.002(2) 0.008(3) 0.003(2) C117 0.042(4) 0.019(2) 0.053(4) 0.003(2) 0.011(3) 0.004(2) C118 0.046(4) 0.023(3) 0.065(5) -0.004(3) 0.009(3) 0.006(3) C119 0.049(4) 0.030(3) 0.071(5) -0.002(3) 0.019(4) 0.006(3) C120 0.038(4) 0.028(3) 0.064(4) -0.001(3) 0.020(3) 0.001(2) C121 0.034(4) 0.018(2) 0.053(4) 0.000(2) 0.006(3) -0.004(2) C122 0.060(5) 0.024(3) 0.059(4) -0.001(3) 0.029(3) -0.003(3) C123 0.059(4) 0.025(3) 0.062(4) 0.002(3) 0.033(3) -0.001(3) C124 0.045(4) 0.023(3) 0.053(4) 0.007(3) 0.012(3) -0.005(2) C125 0.051(4) 0.021(3) 0.086(5) -0.003(3) 0.032(4) 0.000(3) C126 0.044(4) 0.032(3) 0.088(5) -0.002(3) 0.040(4) -0.010(3) O127 0.058(3) 0.0245(19) 0.083(3) 0.005(2) 0.033(3) -0.0048(18) C128 0.046(4) 0.024(3) 0.079(5) 0.004(3) 0.025(3) -0.009(3) C129 0.052(4) 0.029(3) 0.069(5) 0.009(3) 0.019(4) -0.009(3) C130 0.045(4) 0.035(3) 0.056(4) 0.005(3) 0.020(3) -0.007(3) C131 0.049(4) 0.030(3) 0.052(4) 0.003(3) 0.017(3) -0.006(3) C132 0.041(4) 0.028(3) 0.052(4) 0.004(3) 0.018(3) -0.005(2) C133 0.038(4) 0.028(3) 0.046(4) 0.002(2) 0.014(3) -0.001(2) C134 0.045(4) 0.030(3) 0.052(4) 0.000(3) 0.013(3) 0.000(3) C135 0.048(4) 0.036(3) 0.068(5) 0.008(3) 0.023(3) -0.010(3) O21 0.062(3) 0.034(2) 0.072(3) -0.012(2) 0.020(3) 0.015(2) C23 0.035(4) 0.020(2) 0.046(4) -0.003(2) 0.008(3) 0.005(2) C24 0.039(4) 0.022(3) 0.055(4) 0.001(3) 0.014(3) 0.004(2) C25 0.044(4) 0.031(3) 0.060(5) -0.003(3) 0.016(3) -0.011(3) C26 0.043(4) 0.035(3) 0.055(4) 0.006(3) 0.025(3) -0.007(3) C27 0.038(3) 0.030(3) 0.043(4) 0.001(2) 0.016(3) 0.001(2) C28 0.034(3) 0.024(2) 0.036(3) 0.002(3) 0.009(2) -0.002(2) N29 0.026(3) 0.020(2) 0.038(3) 0.0004(19) 0.009(2) 0.0023(18) C29 0.032(4) 0.021(2) 0.042(4) 0.002(2) 0.011(3) 0.004(2) C210 0.028(3) 0.024(3) 0.038(3) 0.001(2) 0.012(3) 0.001(2) C211 0.039(4) 0.018(2) 0.040(4) -0.002(2) 0.012(3) 0.000(2) C212 0.041(4) 0.022(2) 0.040(4) 0.000(2) 0.015(3) 0.006(2) C213 0.033(4) 0.032(3) 0.038(4) 0.000(3) 0.013(3) 0.003(2) C215 0.033(3) 0.022(2) 0.035(3) 0.000(2) 0.011(3) -0.001(2) C216 0.025(3) 0.027(3) 0.040(4) 0.005(2) 0.008(3) 0.003(2) C217 0.032(4) 0.029(3) 0.046(4) -0.003(3) 0.010(3) 0.002(2) C218 0.038(4) 0.038(3) 0.049(4) -0.003(3) 0.026(3) 0.000(3) C219 0.042(4) 0.028(3) 0.055(4) 0.001(3) 0.019(3) -0.001(2) C220 0.043(4) 0.024(3) 0.057(4) 0.001(3) 0.019(3) 0.005(2) C221 0.030(3) 0.023(2) 0.036(3) -0.002(2) 0.009(3) 0.004(2) C222 0.040(4) 0.030(3) 0.051(4) -0.009(3) 0.023(3) -0.002(2) C223 0.045(4) 0.022(2) 0.048(4) -0.003(2) 0.021(3) -0.004(2) C224 0.038(4) 0.024(3) 0.052(4) -0.008(3) 0.012(3) 0.002(2) C225 0.036(4) 0.031(3) 0.103(6) -0.003(3) 0.037(4) -0.002(3) C226 0.040(4) 0.022(3) 0.083(5) -0.004(3) 0.025(3) -0.003(2) O227 0.049(3) 0.0213(18) 0.087(3) -0.009(2) 0.031(2) 0.0028(17) C228 0.048(4) 0.024(3) 0.062(4) -0.010(3) 0.013(3) 0.007(3) C229 0.050(4) 0.029(3) 0.071(5) -0.012(3) 0.018(4) 0.007(3) C230 0.040(4) 0.031(3) 0.055(4) -0.012(3) 0.010(3) 0.006(3) C231 0.055(4) 0.028(3) 0.064(4) -0.002(3) 0.024(3) 0.005(3) C232 0.050(4) 0.026(3) 0.047(4) 0.000(3) 0.017(3) 0.007(3) C233 0.052(5) 0.031(3) 0.058(4) -0.011(3) 0.018(3) 0.002(3) C234 0.047(4) 0.030(3) 0.063(5) 0.004(3) 0.016(3) 0.004(3) C235 0.063(5) 0.032(3) 0.086(5) -0.006(3) 0.029(4) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C11 1.836(6) . y Pt1 N29 2.007(4) . y Pt1 C216 2.056(5) . y Pt1 C23 2.058(6) . y Pt2 C21 1.843(5) . y Pt2 N110 2.003(4) . y Pt2 C13 2.053(5) . y Pt2 C116 2.064(5) . y C11 O21 1.137(6) . ? C13 C14 1.400(8) . ? C13 C18 1.442(7) . ? C14 C15 1.385(7) . ? C15 C16 1.406(7) . ? C16 C17 1.376(8) . ? C17 C18 1.389(7) . ? C18 C19 1.469(7) . ? C19 N110 1.363(6) . ? C19 C114 1.395(7) . ? C21 O22 1.135(6) . ? C110 N110 1.363(7) . ? C110 C112 1.385(7) . ? C110 C115 1.483(7) . ? C112 C113 1.396(7) . ? C113 C114 1.394(7) . ? C113 C121 1.493(7) . ? C115 C120 1.392(7) . ? C115 C116 1.417(7) . ? C116 C117 1.393(6) . ? C117 C118 1.390(8) . ? C118 C119 1.382(8) . ? C119 C120 1.394(7) . ? C121 C122 1.389(7) . ? C121 C126 1.385(7) . ? C122 C123 1.376(7) . ? C123 C124 1.389(7) . ? C124 O127 1.347(6) . ? C124 C125 1.391(8) . ? C125 C126 1.393(7) . ? O127 C128 1.435(6) . ? C128 C129 1.515(7) . ? C129 C130 1.516(7) . ? C130 C131 1.519(7) . ? C131 C132 1.516(6) . ? C132 C133 1.517(7) . ? C133 C134 1.522(7) . ? C134 C135 1.530(7) . ? C23 C24 1.411(7) . ? C23 C28 1.415(7) . ? C24 C25 1.391(8) . ? C25 C26 1.371(8) . ? C26 C27 1.366(7) . ? C27 C28 1.386(7) . ? C28 C29 1.484(6) . ? N29 C210 1.352(6) . ? N29 C29 1.366(6) . ? C29 C213 1.365(7) . ? C210 C211 1.378(6) . ? C210 C215 1.474(7) . ? C211 C212 1.398(7) . ? C212 C213 1.398(7) . ? C212 C221 1.483(6) . ? C215 C220 1.391(7) . ? C215 C216 1.430(7) . ? C216 C217 1.408(7) . ? C217 C218 1.380(7) . ? C218 C219 1.393(7) . ? C219 C220 1.385(7) . ? C221 C222 1.385(6) . ? C221 C226 1.405(7) . ? C222 C223 1.390(7) . ? C223 C224 1.380(7) . ? C224 O227 1.367(6) . ? C224 C225 1.388(7) . ? C225 C226 1.383(7) . ? O227 C228 1.434(6) . ? C228 C229 1.507(7) . ? C229 C230 1.526(7) . ? C230 C231 1.519(7) . ? C231 C232 1.533(6) . ? C232 C233 1.526(7) . ? C233 C234 1.514(7) . ? C234 C235 1.531(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pt1 N29 177.5(2) . . y C11 Pt1 C216 100.4(2) . . y N29 Pt1 C216 80.02(19) . . y C11 Pt1 C23 99.1(2) . . y N29 Pt1 C23 80.49(18) . . y C216 Pt1 C23 160.5(2) . . y C21 Pt2 N110 177.7(2) . . y C21 Pt2 C13 99.2(2) . . y N110 Pt2 C13 80.74(19) . . y C21 Pt2 C116 99.8(2) . . y N110 Pt2 C116 80.27(19) . . y C13 Pt2 C116 161.0(2) . . y O21 C11 Pt1 178.4(6) . . ? C14 C13 C18 116.4(5) . . ? C14 C13 Pt2 131.5(4) . . ? C18 C13 Pt2 112.1(4) . . ? C15 C14 C13 122.4(5) . . ? C14 C15 C16 119.6(6) . . ? C17 C16 C15 120.0(5) . . ? C16 C17 C18 120.7(5) . . ? C17 C18 C13 120.9(5) . . ? C17 C18 C19 123.4(5) . . ? C13 C18 C19 115.7(5) . . ? N110 C19 C114 118.6(5) . . ? N110 C19 C18 112.9(4) . . ? C114 C19 C18 128.4(5) . . ? O22 C21 Pt2 176.9(6) . . ? N110 C110 C112 118.9(5) . . ? N110 C110 C115 112.5(4) . . ? C112 C110 C115 128.6(5) . . ? C19 N110 C110 122.8(4) . . ? C19 N110 Pt2 118.5(4) . . ? C110 N110 Pt2 118.7(3) . . ? C110 C112 C113 120.6(5) . . ? C114 C113 C112 118.7(5) . . ? C114 C113 C121 120.2(4) . . ? C112 C113 C121 121.1(5) . . ? C113 C114 C19 120.4(5) . . ? C120 C115 C116 122.1(5) . . ? C120 C115 C110 122.0(5) . . ? C116 C115 C110 115.8(5) . . ? C117 C116 C115 117.1(5) . . ? C117 C116 Pt2 130.2(4) . . ? C115 C116 Pt2 112.7(3) . . ? C118 C117 C116 121.5(5) . . ? C119 C118 C117 119.9(5) . . ? C118 C119 C120 121.0(6) . . ? C119 C120 C115 118.4(5) . . ? C122 C121 C126 116.0(5) . . ? C122 C121 C113 122.0(5) . . ? C126 C121 C113 122.0(5) . . ? C123 C122 C121 122.3(5) . . ? C122 C123 C124 120.9(6) . . ? O127 C124 C123 116.3(5) . . ? O127 C124 C125 125.4(5) . . ? C123 C124 C125 118.3(5) . . ? C126 C125 C124 119.4(5) . . ? C121 C126 C125 123.1(6) . . ? C124 O127 C128 119.9(4) . . ? O127 C128 C129 107.0(5) . . ? C128 C129 C130 115.2(5) . . ? C129 C130 C131 111.1(5) . . ? C132 C131 C130 116.9(5) . . ? C131 C132 C133 112.1(5) . . ? C132 C133 C134 116.0(5) . . ? C133 C134 C135 113.0(5) . . ? C24 C23 C28 115.9(5) . . ? C24 C23 Pt1 131.2(4) . . ? C28 C23 Pt1 112.9(3) . . ? C25 C24 C23 121.7(5) . . ? C26 C25 C24 120.3(5) . . ? C27 C26 C25 119.9(5) . . ? C26 C27 C28 121.0(5) . . ? C27 C28 C23 121.2(4) . . ? C27 C28 C29 123.1(5) . . ? C23 C28 C29 115.7(5) . . ? C210 N29 C29 122.8(4) . . ? C210 N29 Pt1 119.1(4) . . ? C29 N29 Pt1 118.1(3) . . ? C213 C29 N29 118.2(5) . . ? C213 C29 C28 129.0(5) . . ? N29 C29 C28 112.8(4) . . ? N29 C210 C211 119.0(5) . . ? N29 C210 C215 112.6(4) . . ? C211 C210 C215 128.4(5) . . ? C210 C211 C212 120.9(5) . . ? C211 C212 C213 117.2(5) . . ? C211 C212 C221 120.8(4) . . ? C213 C212 C221 122.0(5) . . ? C29 C213 C212 121.9(5) . . ? C220 C215 C216 120.9(5) . . ? C220 C215 C210 123.5(5) . . ? C216 C215 C210 115.6(4) . . ? C217 C216 C215 116.3(5) . . ? C217 C216 Pt1 131.0(4) . . ? C215 C216 Pt1 112.6(4) . . ? C218 C217 C216 122.3(5) . . ? C217 C218 C219 120.2(5) . . ? C220 C219 C218 119.6(5) . . ? C219 C220 C215 120.7(5) . . ? C222 C221 C226 116.6(5) . . ? C222 C221 C212 122.5(5) . . ? C226 C221 C212 120.9(4) . . ? C221 C222 C223 122.8(5) . . ? C224 C223 C222 119.3(5) . . ? O227 C224 C225 115.3(5) . . ? O227 C224 C223 125.1(5) . . ? C225 C224 C223 119.6(5) . . ? C224 C225 C226 120.3(5) . . ? C225 C226 C221 121.4(5) . . ? C224 O227 C228 119.5(4) . . ? O227 C228 C229 107.0(5) . . ? C228 C229 C230 113.3(5) . . ? C231 C230 C229 110.2(5) . . ? C230 C231 C232 115.2(5) . . ? C233 C232 C231 112.2(5) . . ? C234 C233 C232 115.4(5) . . ? C233 C234 C235 112.3(5) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 29.20 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 1.228 _refine_diff_density_min -1.398 _refine_diff_density_rms 0.128 #===END