# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_20121214d_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H26 N2 Pt' _chemical_formula_sum 'C31 H26 N2 Pt' _chemical_formula_weight 621.63 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 Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.2934(4) _cell_length_b 11.9839(8) _cell_length_c 32.646(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2462.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5259 _cell_measurement_theta_min 2.528 _cell_measurement_theta_max 23.8935 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 5.720 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3289 _exptl_absorpt_correction_T_max 0.4613 _exptl_absorpt_process_details SADABS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Smart Aepex CCD' _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 16877 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5646 _reflns_number_gt 5065 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART,(Bruker,2000) _computing_cell_refinement SMART _computing_data_reduction SAINT(Bruker,2000) _computing_structure_solution 'SHELXTL(Bruker,2000) ' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0118P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(8) _chemical_absolute_configuration unk _refine_ls_number_reflns 5646 _refine_ls_number_parameters 303 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0558 _refine_ls_wR_factor_gt 0.0540 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.010 _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 0.4845(8) 0.1549(3) 0.75120(15) 0.0439(12) Uani 1 1 d . . . C2 C 0.4161(9) 0.0981(4) 0.84008(14) 0.0471(13) Uani 1 1 d . . . C3 C 0.6722(9) 0.0931(4) 0.74947(16) 0.0542(13) Uani 1 1 d U . . H3 H 0.7271 0.0587 0.7727 0.065 Uiso 1 1 calc R . . C4 C 0.7716(12) 0.0848(3) 0.71286(15) 0.0671(17) Uani 1 1 d U . . H4 H 0.8896 0.0382 0.7122 0.081 Uiso 1 1 calc R . . C5 C 0.7237(11) 0.1335(4) 0.67862(18) 0.0667(15) Uani 1 1 d U . . H5 H 0.8105 0.1275 0.6557 0.080 Uiso 1 1 calc R . . C6 C 0.5375(9) 0.1949(4) 0.67772(15) 0.0559(13) Uani 1 1 d . . . H6 H 0.4917 0.2281 0.6535 0.067 Uiso 1 1 calc R . . C7 C 0.4203(8) 0.2062(4) 0.71355(14) 0.0461(12) Uani 1 1 d . . . C8 C 0.2249(8) 0.2750(4) 0.71572(14) 0.0450(11) Uani 1 1 d . . . C9 C 0.1282(10) 0.3382(4) 0.68539(15) 0.0539(14) Uani 1 1 d . . . H9 H 0.1872 0.3419 0.6593 0.065 Uiso 1 1 calc R . . C10 C -0.0553(10) 0.3952(4) 0.69418(15) 0.0561(15) Uani 1 1 d . . . H10 H -0.1206 0.4368 0.6737 0.067 Uiso 1 1 calc R . . C11 C -0.1459(9) 0.3921(4) 0.73302(15) 0.0501(13) Uani 1 1 d . . . H11 H -0.2715 0.4299 0.7387 0.060 Uiso 1 1 calc R . . C12 C -0.0420(8) 0.3306(3) 0.76303(14) 0.0439(11) Uani 1 1 d . . . C13 C -0.1023(7) 0.3218(4) 0.80665(13) 0.0441(11) Uani 1 1 d . . . C14 C -0.2707(9) 0.3765(4) 0.82412(14) 0.0498(12) Uani 1 1 d . . . H14 H -0.3623 0.4175 0.8076 0.060 Uiso 1 1 calc R . . C15 C -0.3062(9) 0.3719(4) 0.86547(16) 0.0516(12) Uani 1 1 d . . . C16 C -0.1658(8) 0.3080(4) 0.88978(14) 0.0504(11) Uani 1 1 d . . . C17 C -0.0044(9) 0.2518(4) 0.87059(15) 0.0509(13) Uani 1 1 d . . . H17 H 0.0851 0.2073 0.8863 0.061 Uiso 1 1 calc R . . C18 C -0.4784(10) 0.4349(6) 0.88753(17) 0.0729(17) Uani 1 1 d . . . H18A H -0.6160 0.4107 0.8775 0.088 Uiso 1 1 calc R . . H18B H -0.4642 0.5140 0.8818 0.088 Uiso 1 1 calc R . . C19 C -0.4663(11) 0.4156(5) 0.93393(18) 0.0744(13) Uani 1 1 d . . . H19 H -0.5761 0.4533 0.9501 0.089 Uiso 1 1 calc R . . C20 C -0.4431(10) 0.2890(5) 0.94209(18) 0.0744(13) Uani 1 1 d . . . H20A H -0.5110 0.2418 0.9218 0.089 Uiso 1 1 calc R . . H20B H -0.4801 0.2663 0.9697 0.089 Uiso 1 1 calc R . . C21 C -0.2023(9) 0.3074(4) 0.93506(15) 0.0604(13) Uani 1 1 d . . . H21 H -0.1055 0.2615 0.9515 0.073 Uiso 1 1 calc R . . C22 C -0.2362(10) 0.4311(5) 0.94966(16) 0.0653(15) Uani 1 1 d . . . C23 C -0.0941(12) 0.5215(5) 0.9313(2) 0.081(2) Uani 1 1 d . . . H23A H -0.0995 0.5172 0.9019 0.122 Uiso 1 1 calc R . . H23B H 0.0495 0.5105 0.9403 0.122 Uiso 1 1 calc R . . H23C H -0.1431 0.5935 0.9400 0.122 Uiso 1 1 calc R . . C24 C -0.2280(13) 0.4388(5) 0.99668(17) 0.096(2) Uani 1 1 d . . . H24A H -0.0833 0.4330 1.0057 0.144 Uiso 1 1 calc R . . H24B H -0.3100 0.3792 1.0084 0.144 Uiso 1 1 calc R . . H24C H -0.2858 0.5092 1.0053 0.144 Uiso 1 1 calc R . . C25 C 0.4741(9) 0.0386(4) 0.86763(15) 0.0504(13) Uani 1 1 d . . . C26 C 0.5288(9) -0.0378(4) 0.90007(13) 0.0488(13) Uani 1 1 d . . . C27 C 0.3866(11) -0.1216(4) 0.91128(15) 0.0629(16) Uani 1 1 d . . . H27 H 0.2544 -0.1249 0.8986 0.076 Uiso 1 1 calc R . . C28 C 0.4373(13) -0.1994(6) 0.94065(17) 0.086(2) Uani 1 1 d . . . H28 H 0.3409 -0.2553 0.9474 0.103 Uiso 1 1 calc R . . C29 C 0.6298(16) -0.1943(7) 0.9599(2) 0.100(3) Uani 1 1 d . . . H29 H 0.6631 -0.2465 0.9800 0.120 Uiso 1 1 calc R . . C30 C 0.7735(15) -0.1134(6) 0.9500(2) 0.098(3) Uani 1 1 d . . . H30 H 0.9039 -0.1101 0.9633 0.118 Uiso 1 1 calc R . . C31 C 0.7231(12) -0.0356(5) 0.91945(17) 0.0754(17) Uani 1 1 d . . . H31 H 0.8223 0.0184 0.9122 0.090 Uiso 1 1 calc R . . N1 N 0.1388(7) 0.2763(3) 0.75378(11) 0.0418(9) Uani 1 1 d . . . N2 N 0.0304(7) 0.2580(3) 0.83005(12) 0.0449(10) Uani 1 1 d . . . Pt1 Pt 0.28635(3) 0.188585(13) 0.796922(5) 0.04094(6) 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 0.048(3) 0.033(2) 0.051(3) 0.004(2) -0.011(2) -0.004(2) C2 0.059(4) 0.038(2) 0.044(3) -0.003(2) -0.009(2) 0.004(2) C3 0.050(4) 0.040(2) 0.072(3) 0.002(2) -0.009(2) 0.004(2) C4 0.116(5) 0.0212(19) 0.064(3) -0.005(2) 0.022(3) -0.005(3) C5 0.065(4) 0.058(3) 0.076(4) -0.018(3) 0.015(3) 0.004(3) C6 0.065(4) 0.051(3) 0.052(3) 0.005(3) -0.001(2) 0.000(3) C7 0.045(3) 0.042(3) 0.052(3) 0.003(2) -0.004(2) -0.004(2) C8 0.046(3) 0.041(2) 0.048(3) 0.0057(19) -0.008(2) -0.009(2) C9 0.066(4) 0.050(3) 0.045(3) 0.009(2) -0.015(2) -0.003(3) C10 0.069(4) 0.054(3) 0.045(3) 0.009(2) -0.026(3) 0.009(3) C11 0.050(3) 0.043(3) 0.057(3) -0.003(2) -0.022(2) 0.009(2) C12 0.047(3) 0.033(3) 0.051(3) 0.001(2) -0.015(2) -0.005(2) C13 0.042(3) 0.040(2) 0.050(3) 0.003(2) -0.015(2) -0.002(2) C14 0.045(3) 0.051(3) 0.054(3) 0.006(2) -0.013(2) 0.002(2) C15 0.040(3) 0.053(3) 0.062(3) -0.003(2) -0.002(3) -0.006(3) C16 0.053(3) 0.041(2) 0.058(3) -0.004(3) -0.006(2) -0.004(3) C17 0.061(4) 0.041(3) 0.050(3) 0.008(2) -0.016(3) -0.003(3) C18 0.044(4) 0.099(4) 0.076(4) -0.004(4) -0.001(3) 0.005(4) C19 0.072(3) 0.083(3) 0.068(3) -0.003(2) 0.010(2) -0.001(3) C20 0.072(3) 0.083(3) 0.068(3) -0.003(2) 0.010(2) -0.001(3) C21 0.072(4) 0.055(3) 0.054(3) 0.002(3) -0.005(3) 0.005(4) C22 0.065(4) 0.062(3) 0.068(3) -0.014(3) -0.006(3) 0.011(3) C23 0.072(5) 0.058(3) 0.113(5) -0.022(4) -0.009(4) -0.004(3) C24 0.106(6) 0.099(4) 0.082(4) -0.033(4) -0.015(4) 0.030(5) C25 0.062(4) 0.040(3) 0.049(3) -0.003(2) -0.012(2) 0.008(2) C26 0.067(4) 0.046(3) 0.034(3) -0.006(2) -0.007(2) 0.015(3) C27 0.082(5) 0.065(3) 0.041(3) 0.002(3) 0.001(3) 0.004(3) C28 0.134(7) 0.073(4) 0.051(3) 0.015(3) 0.010(4) -0.002(5) C29 0.155(9) 0.085(5) 0.060(4) 0.014(4) -0.010(5) 0.042(6) C30 0.110(7) 0.115(5) 0.070(4) 0.010(4) -0.041(5) 0.034(6) C31 0.081(5) 0.074(4) 0.071(4) 0.001(3) -0.020(4) 0.019(4) N1 0.042(2) 0.0300(17) 0.053(2) 0.0036(16) -0.0134(19) -0.0037(17) N2 0.048(3) 0.038(2) 0.049(2) 0.0017(18) -0.0116(19) 0.0026(19) Pt1 0.04387(10) 0.03158(8) 0.04737(9) 0.00531(8) -0.01210(8) 0.00007(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 C1 C3 1.395(7) . ? C1 C7 1.433(6) . ? C1 Pt1 1.986(5) . ? C2 C25 1.204(6) . ? C2 Pt1 1.957(5) . ? C3 C4 1.353(7) . ? C3 H3 0.9300 . ? C4 C5 1.297(7) . ? C4 H4 0.9300 . ? C5 C6 1.384(8) . ? C5 H5 0.9300 . ? C6 C7 1.390(7) . ? C6 H6 0.9300 . ? C7 C8 1.482(7) . ? C8 N1 1.356(6) . ? C8 C9 1.387(6) . ? C9 C10 1.372(8) . ? C9 H9 0.9300 . ? C10 C11 1.391(7) . ? C10 H10 0.9300 . ? C11 C12 1.390(6) . ? C11 H11 0.9300 . ? C12 N1 1.345(6) . ? C12 C13 1.478(6) . ? C13 N2 1.365(6) . ? C13 C14 1.371(7) . ? C14 C15 1.370(7) . ? C14 H14 0.9300 . ? C15 C16 1.413(7) . ? C15 C18 1.504(8) . ? C16 C17 1.371(7) . ? C16 C21 1.496(6) . ? C17 N2 1.343(6) . ? C17 H17 0.9300 . ? C18 C19 1.534(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.547(9) . ? C19 C22 1.548(9) . ? C19 H19 0.9800 . ? C20 C21 1.549(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.571(7) . ? C21 H21 0.9800 . ? C22 C23 1.527(9) . ? C22 C24 1.539(7) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.442(6) . ? C26 C31 1.377(8) . ? C26 C27 1.394(7) . ? C27 C28 1.375(8) . ? C27 H27 0.9300 . ? C28 C29 1.366(11) . ? C28 H28 0.9300 . ? C29 C30 1.365(11) . ? C29 H29 0.9300 . ? C30 C31 1.402(8) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? N1 Pt1 1.988(4) . ? N2 Pt1 2.111(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C1 C7 115.6(5) . . ? C3 C1 Pt1 132.1(4) . . ? C7 C1 Pt1 112.4(4) . . ? C25 C2 Pt1 172.9(5) . . ? C4 C3 C1 117.8(5) . . ? C4 C3 H3 121.1 . . ? C1 C3 H3 121.1 . . ? C5 C4 C3 128.4(6) . . ? C5 C4 H4 115.8 . . ? C3 C4 H4 115.8 . . ? C4 C5 C6 117.0(6) . . ? C4 C5 H5 121.5 . . ? C6 C5 H5 121.5 . . ? C5 C6 C7 118.9(5) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C6 C7 C1 122.1(5) . . ? C6 C7 C8 122.3(4) . . ? C1 C7 C8 115.6(4) . . ? N1 C8 C9 118.2(5) . . ? N1 C8 C7 112.4(4) . . ? C9 C8 C7 129.3(5) . . ? C10 C9 C8 119.5(5) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 121.5(4) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C12 C11 C10 117.6(5) . . ? C12 C11 H11 121.2 . . ? C10 C11 H11 121.2 . . ? N1 C12 C11 119.8(5) . . ? N1 C12 C13 113.5(4) . . ? C11 C12 C13 126.6(5) . . ? N2 C13 C14 120.5(4) . . ? N2 C13 C12 115.0(4) . . ? C14 C13 C12 124.4(4) . . ? C15 C14 C13 121.1(5) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 118.2(5) . . ? C14 C15 C18 124.7(5) . . ? C16 C15 C18 117.0(5) . . ? C17 C16 C15 118.2(5) . . ? C17 C16 C21 124.3(5) . . ? C15 C16 C21 117.5(5) . . ? N2 C17 C16 122.9(5) . . ? N2 C17 H17 118.5 . . ? C16 C17 H17 118.5 . . ? C15 C18 C19 111.2(5) . . ? C15 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? C15 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C20 108.8(5) . . ? C18 C19 C22 110.8(5) . . ? C20 C19 C22 88.4(5) . . ? C18 C19 H19 115.2 . . ? C20 C19 H19 115.2 . . ? C22 C19 H19 115.2 . . ? C19 C20 C21 85.8(5) . . ? C19 C20 H20A 114.4 . . ? C21 C20 H20A 114.4 . . ? C19 C20 H20B 114.4 . . ? C21 C20 H20B 114.4 . . ? H20A C20 H20B 111.5 . . ? C16 C21 C20 107.3(4) . . ? C16 C21 C22 108.4(4) . . ? C20 C21 C22 87.5(5) . . ? C16 C21 H21 116.6 . . ? C20 C21 H21 116.6 . . ? C22 C21 H21 116.6 . . ? C23 C22 C24 109.2(5) . . ? C23 C22 C19 120.2(5) . . ? C24 C22 C19 111.7(5) . . ? C23 C22 C21 118.1(5) . . ? C24 C22 C21 110.8(5) . . ? C19 C22 C21 85.0(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C2 C25 C26 175.5(6) . . ? C31 C26 C27 117.6(5) . . ? C31 C26 C25 122.5(6) . . ? C27 C26 C25 119.8(5) . . ? C28 C27 C26 121.5(6) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C29 C28 C27 119.8(7) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C30 C29 C28 120.6(7) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 119.5(7) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C26 C31 C30 121.0(7) . . ? C26 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C12 N1 C8 123.3(4) . . ? C12 N1 Pt1 119.5(3) . . ? C8 N1 Pt1 117.2(3) . . ? C17 N2 C13 118.8(4) . . ? C17 N2 Pt1 127.4(3) . . ? C13 N2 Pt1 113.6(3) . . ? C2 Pt1 C1 99.6(2) . . ? C2 Pt1 N1 176.7(2) . . ? C1 Pt1 N1 82.44(18) . . ? C2 Pt1 N2 99.68(19) . . ? C1 Pt1 N2 160.75(16) . . ? N1 Pt1 N2 78.35(16) . . ? 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 C7 C1 C3 C4 -1.8(6) . . . . ? Pt1 C1 C3 C4 179.5(4) . . . . ? C1 C3 C4 C5 5.1(9) . . . . ? C3 C4 C5 C6 -6.0(9) . . . . ? C4 C5 C6 C7 3.6(8) . . . . ? C5 C6 C7 C1 -1.0(8) . . . . ? C5 C6 C7 C8 177.0(4) . . . . ? C3 C1 C7 C6 0.1(7) . . . . ? Pt1 C1 C7 C6 179.1(4) . . . . ? C3 C1 C7 C8 -178.0(4) . . . . ? Pt1 C1 C7 C8 1.0(5) . . . . ? C6 C7 C8 N1 -178.6(4) . . . . ? C1 C7 C8 N1 -0.5(6) . . . . ? C6 C7 C8 C9 -0.9(8) . . . . ? C1 C7 C8 C9 177.2(5) . . . . ? N1 C8 C9 C10 -3.0(7) . . . . ? C7 C8 C9 C10 179.4(5) . . . . ? C8 C9 C10 C11 0.7(8) . . . . ? C9 C10 C11 C12 1.1(8) . . . . ? C10 C11 C12 N1 -0.4(7) . . . . ? C10 C11 C12 C13 175.9(5) . . . . ? N1 C12 C13 N2 -1.8(6) . . . . ? C11 C12 C13 N2 -178.3(4) . . . . ? N1 C12 C13 C14 174.9(4) . . . . ? C11 C12 C13 C14 -1.6(7) . . . . ? N2 C13 C14 C15 2.2(7) . . . . ? C12 C13 C14 C15 -174.3(4) . . . . ? C13 C14 C15 C16 -0.7(7) . . . . ? C13 C14 C15 C18 176.0(5) . . . . ? C14 C15 C16 C17 -1.6(7) . . . . ? C18 C15 C16 C17 -178.5(5) . . . . ? C14 C15 C16 C21 177.8(4) . . . . ? C18 C15 C16 C21 0.8(7) . . . . ? C15 C16 C17 N2 2.5(7) . . . . ? C21 C16 C17 N2 -176.9(5) . . . . ? C14 C15 C18 C19 -177.0(5) . . . . ? C16 C15 C18 C19 -0.3(7) . . . . ? C15 C18 C19 C20 -47.7(7) . . . . ? C15 C18 C19 C22 47.9(7) . . . . ? C18 C19 C20 C21 84.2(5) . . . . ? C22 C19 C20 C21 -27.3(4) . . . . ? C17 C16 C21 C20 -134.7(5) . . . . ? C15 C16 C21 C20 45.9(6) . . . . ? C17 C16 C21 C22 132.0(5) . . . . ? C15 C16 C21 C22 -47.3(6) . . . . ? C19 C20 C21 C16 -81.6(5) . . . . ? C19 C20 C21 C22 26.9(4) . . . . ? C18 C19 C22 C23 37.1(8) . . . . ? C20 C19 C22 C23 146.6(5) . . . . ? C18 C19 C22 C24 167.0(5) . . . . ? C20 C19 C22 C24 -83.5(5) . . . . ? C18 C19 C22 C21 -82.6(6) . . . . ? C20 C19 C22 C21 26.9(4) . . . . ? C16 C21 C22 C23 -41.2(7) . . . . ? C20 C21 C22 C23 -148.6(6) . . . . ? C16 C21 C22 C24 -168.2(5) . . . . ? C20 C21 C22 C24 84.4(6) . . . . ? C16 C21 C22 C19 80.5(5) . . . . ? C20 C21 C22 C19 -26.9(4) . . . . ? Pt1 C2 C25 C26 26(9) . . . . ? C2 C25 C26 C31 170(7) . . . . ? C2 C25 C26 C27 -6(7) . . . . ? C31 C26 C27 C28 0.1(8) . . . . ? C25 C26 C27 C28 176.7(5) . . . . ? C26 C27 C28 C29 1.0(9) . . . . ? C27 C28 C29 C30 -0.8(11) . . . . ? C28 C29 C30 C31 -0.5(11) . . . . ? C27 C26 C31 C30 -1.3(8) . . . . ? C25 C26 C31 C30 -177.9(5) . . . . ? C29 C30 C31 C26 1.5(10) . . . . ? C11 C12 N1 C8 -2.2(6) . . . . ? C13 C12 N1 C8 -178.9(4) . . . . ? C11 C12 N1 Pt1 180.0(3) . . . . ? C13 C12 N1 Pt1 3.2(5) . . . . ? C9 C8 N1 C12 3.9(7) . . . . ? C7 C8 N1 C12 -178.1(4) . . . . ? C9 C8 N1 Pt1 -178.2(3) . . . . ? C7 C8 N1 Pt1 -0.2(5) . . . . ? C16 C17 N2 C13 -1.0(7) . . . . ? C16 C17 N2 Pt1 174.1(4) . . . . ? C14 C13 N2 C17 -1.4(7) . . . . ? C12 C13 N2 C17 175.5(4) . . . . ? C14 C13 N2 Pt1 -177.1(3) . . . . ? C12 C13 N2 Pt1 -0.2(5) . . . . ? C25 C2 Pt1 C1 -135(3) . . . . ? C25 C2 Pt1 N1 -7(6) . . . . ? C25 C2 Pt1 N2 46(3) . . . . ? C3 C1 Pt1 C2 -4.7(5) . . . . ? C7 C1 Pt1 C2 176.5(3) . . . . ? C3 C1 Pt1 N1 177.9(5) . . . . ? C7 C1 Pt1 N1 -0.9(3) . . . . ? C3 C1 Pt1 N2 174.1(4) . . . . ? C7 C1 Pt1 N2 -4.7(7) . . . . ? C12 N1 Pt1 C2 50(3) . . . . ? C8 N1 Pt1 C2 -128(3) . . . . ? C12 N1 Pt1 C1 178.6(3) . . . . ? C8 N1 Pt1 C1 0.6(3) . . . . ? C12 N1 Pt1 N2 -2.6(3) . . . . ? C8 N1 Pt1 N2 179.4(3) . . . . ? C17 N2 Pt1 C2 8.8(4) . . . . ? C13 N2 Pt1 C2 -175.9(3) . . . . ? C17 N2 Pt1 C1 -170.0(5) . . . . ? C13 N2 Pt1 C1 5.3(7) . . . . ? C17 N2 Pt1 N1 -173.8(4) . . . . ? C13 N2 Pt1 N1 1.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.792 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.082 _database_code_depnum_ccdc_archive 'CCDC 952002' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_20130322e_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H26 N2 Pt' _chemical_formula_sum 'C31 H26 N2 Pt' _chemical_formula_weight 621.63 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 Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.0349(4) _cell_length_b 15.7571(11) _cell_length_c 25.3332(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2409.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7577 _cell_measurement_theta_min 2.585 _cell_measurement_theta_max 26.825 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 5.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2644 _exptl_absorpt_correction_T_max 0.4547 _exptl_absorpt_process_details SADABS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Smart Aepex CCD' _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 16468 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5513 _reflns_number_gt 5102 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART,(Bruker,2000) _computing_cell_refinement SMART _computing_data_reduction SAINT(Bruker,2000) _computing_structure_solution 'SHELXTL(Bruker,2000) ' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(6) _chemical_absolute_configuration unk _refine_ls_number_reflns 5513 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0248 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0435 _refine_ls_wR_factor_gt 0.0425 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 C1 C 0.8070(7) 0.4686(2) 0.89665(14) 0.0543(9) Uani 1 1 d . . . C2 C 0.8796(6) 0.4933(2) 0.77992(14) 0.0501(9) Uani 1 1 d . . . C3 C 0.9945(9) 0.5168(2) 0.90784(17) 0.0641(11) Uani 1 1 d . . . H3 H 1.0791 0.5378 0.8801 0.077 Uiso 1 1 calc R . . C4 C 1.0589(9) 0.5344(3) 0.9596(2) 0.0795(15) Uani 1 1 d . . . H4 H 1.1850 0.5667 0.9661 0.095 Uiso 1 1 calc R . . C5 C 0.9354(10) 0.5038(3) 1.00083(18) 0.0867(16) Uani 1 1 d . . . H5 H 0.9786 0.5157 1.0353 0.104 Uiso 1 1 calc R . . C6 C 0.7489(8) 0.4559(3) 0.99212(17) 0.0767(13) Uani 1 1 d . . . H6 H 0.6666 0.4361 1.0206 0.092 Uiso 1 1 calc R . . C7 C 0.6818(7) 0.4368(2) 0.94033(13) 0.0588(9) Uani 1 1 d . . . C8 C 0.4877(8) 0.3855(2) 0.92788(15) 0.0578(10) Uani 1 1 d . . . C9 C 0.3364(10) 0.3468(3) 0.96061(17) 0.0725(12) Uani 1 1 d . . . H9 H 0.3535 0.3503 0.9970 0.087 Uiso 1 1 calc R . . C10 C 0.1592(10) 0.3028(3) 0.93959(18) 0.0760(13) Uani 1 1 d . . . H10 H 0.0577 0.2770 0.9621 0.091 Uiso 1 1 calc R . . C11 C 0.1309(7) 0.2966(2) 0.88588(17) 0.0648(11) Uani 1 1 d . . . H11 H 0.0104 0.2677 0.8717 0.078 Uiso 1 1 calc R . . C12 C 0.2860(6) 0.3346(2) 0.85346(15) 0.0524(9) Uani 1 1 d . . . C13 C 0.2873(6) 0.3345(2) 0.79535(14) 0.0468(8) Uani 1 1 d . . . C14 C 0.1345(6) 0.2918(2) 0.76454(15) 0.0548(9) Uani 1 1 d . . . H14 H 0.0189 0.2626 0.7806 0.066 Uiso 1 1 calc R . . C15 C 0.1514(7) 0.2919(2) 0.71021(16) 0.0517(9) Uani 1 1 d . . . C16 C 0.3242(7) 0.3392(2) 0.68732(13) 0.0511(8) Uani 1 1 d . . . C17 C 0.4704(7) 0.3809(2) 0.71989(14) 0.0491(8) Uani 1 1 d . . . H17 H 0.5846 0.4119 0.7045 0.059 Uiso 1 1 calc R . . C18 C 0.0016(6) 0.2433(2) 0.67427(18) 0.0664(10) Uani 1 1 d . . . H18A H -0.1505 0.2607 0.6802 0.080 Uiso 1 1 calc R . . H18B H 0.0127 0.1832 0.6822 0.080 Uiso 1 1 calc R . . C19 C 0.0621(8) 0.2581(3) 0.6164(2) 0.0691(13) Uani 1 1 d . . . H19 H -0.0340 0.2299 0.5907 0.083 Uiso 1 1 calc R . . C20 C 0.0969(9) 0.3541(3) 0.6076(2) 0.0886(17) Uani 1 1 d . . . H20A H 0.0066 0.3901 0.6301 0.106 Uiso 1 1 calc R . . H20B H 0.0890 0.3717 0.5710 0.106 Uiso 1 1 calc R . . C21 C 0.3377(8) 0.3392(2) 0.62850(14) 0.0602(10) Uani 1 1 d . . . H21 H 0.4547 0.3739 0.6127 0.072 Uiso 1 1 calc R . . C22 C 0.3157(8) 0.2457(2) 0.60759(15) 0.0579(9) Uani 1 1 d . . . C23 C 0.4310(6) 0.1757(2) 0.63690(17) 0.0649(11) Uani 1 1 d . . . H23A H 0.3858 0.1219 0.6228 0.097 Uiso 1 1 calc R . . H23B H 0.3926 0.1786 0.6736 0.097 Uiso 1 1 calc R . . H23C H 0.5884 0.1819 0.6330 0.097 Uiso 1 1 calc R . . C24 C 0.3758(10) 0.2399(3) 0.54919(17) 0.0946(17) Uani 1 1 d . . . H24A H 0.5337 0.2437 0.5452 0.142 Uiso 1 1 calc R . . H24B H 0.3066 0.2857 0.5304 0.142 Uiso 1 1 calc R . . H24C H 0.3248 0.1867 0.5352 0.142 Uiso 1 1 calc R . . C25 C 0.9958(7) 0.5268(2) 0.74890(14) 0.0486(8) Uani 1 1 d . . . C26 C 1.1408(6) 0.5639(2) 0.71003(13) 0.0459(7) Uani 1 1 d . . . C27 C 1.0796(7) 0.5700(3) 0.65754(14) 0.0622(10) Uani 1 1 d . . . H27 H 0.9401 0.5516 0.6469 0.075 Uiso 1 1 calc R . . C28 C 1.2262(10) 0.6034(4) 0.6206(2) 0.0852(17) Uani 1 1 d . . . H28 H 1.1840 0.6070 0.5854 0.102 Uiso 1 1 calc R . . C29 C 1.4304(10) 0.6309(3) 0.6355(2) 0.0866(16) Uani 1 1 d . . . H29 H 1.5272 0.6533 0.6105 0.104 Uiso 1 1 calc R . . C30 C 1.4920(8) 0.6257(3) 0.6865(2) 0.0781(14) Uani 1 1 d . . . H30 H 1.6318 0.6446 0.6966 0.094 Uiso 1 1 calc R . . C31 C 1.3511(8) 0.5928(2) 0.72385(17) 0.0592(10) Uani 1 1 d . . . H31 H 1.3968 0.5897 0.7589 0.071 Uiso 1 1 calc R . . N1 N 0.4563(6) 0.37705(18) 0.87515(11) 0.0481(7) Uani 1 1 d . . . N2 N 0.4565(5) 0.37906(17) 0.77287(11) 0.0453(7) Uani 1 1 d . . . Pt1 Pt 0.67244(2) 0.434694(7) 0.828055(5) 0.04421(4) 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 0.069(2) 0.0451(18) 0.049(2) -0.0025(15) -0.013(2) 0.0130(19) C2 0.060(2) 0.0445(19) 0.045(2) -0.0064(15) -0.0086(18) 0.0000(17) C3 0.081(3) 0.052(2) 0.059(2) -0.0008(18) -0.017(2) 0.007(2) C4 0.101(4) 0.063(3) 0.075(3) -0.013(2) -0.029(3) 0.010(3) C5 0.124(5) 0.084(3) 0.052(3) -0.011(2) -0.022(3) 0.017(3) C6 0.105(4) 0.077(3) 0.048(2) -0.002(2) -0.001(2) 0.016(2) C7 0.079(2) 0.0553(19) 0.0425(18) -0.0005(17) 0.0001(19) 0.015(3) C8 0.073(3) 0.050(2) 0.050(2) 0.0064(17) 0.013(2) 0.015(2) C9 0.100(3) 0.065(2) 0.053(2) 0.0083(19) 0.016(3) 0.018(3) C10 0.087(3) 0.064(3) 0.076(3) 0.018(2) 0.035(3) 0.005(3) C11 0.065(3) 0.053(2) 0.076(3) 0.008(2) 0.023(2) 0.004(2) C12 0.058(2) 0.0423(18) 0.057(2) 0.0019(16) 0.0133(19) 0.0077(17) C13 0.045(2) 0.0381(17) 0.058(2) 0.0005(15) 0.0108(17) 0.0013(15) C14 0.048(2) 0.048(2) 0.069(2) -0.0009(17) 0.0085(19) -0.0095(17) C15 0.043(2) 0.0441(18) 0.068(2) -0.0071(17) 0.000(2) 0.0001(19) C16 0.057(2) 0.0406(17) 0.055(2) 0.0021(14) -0.010(2) -0.0066(19) C17 0.055(2) 0.0397(18) 0.052(2) 0.0057(15) 0.0041(18) -0.0090(17) C18 0.0422(18) 0.068(2) 0.089(3) -0.012(2) -0.008(3) -0.0079(18) C19 0.063(3) 0.069(3) 0.075(3) -0.005(2) -0.023(2) -0.011(2) C20 0.113(4) 0.070(3) 0.083(3) 0.013(2) -0.042(3) 0.000(3) C21 0.073(2) 0.059(2) 0.048(2) 0.0086(16) -0.012(2) -0.021(2) C22 0.062(2) 0.062(2) 0.050(2) -0.0059(17) -0.005(2) -0.017(2) C23 0.052(2) 0.062(2) 0.081(3) -0.015(2) -0.012(2) -0.0060(19) C24 0.113(4) 0.111(4) 0.059(3) -0.014(3) -0.002(3) -0.042(3) C25 0.054(2) 0.0445(19) 0.047(2) -0.0018(15) -0.0024(19) -0.0050(17) C26 0.049(2) 0.0370(15) 0.0520(18) -0.0059(16) -0.0017(16) 0.003(2) C27 0.057(2) 0.074(3) 0.056(2) 0.005(2) -0.0037(17) -0.006(2) C28 0.097(4) 0.108(4) 0.051(3) 0.016(3) 0.005(3) 0.008(3) C29 0.085(4) 0.086(4) 0.089(4) 0.020(3) 0.027(3) -0.015(3) C30 0.058(3) 0.065(3) 0.112(4) -0.008(2) 0.008(3) -0.019(2) C31 0.060(3) 0.056(2) 0.062(2) -0.0088(17) -0.004(2) -0.008(2) N1 0.061(2) 0.0433(16) 0.0406(16) 0.0019(12) 0.0070(15) 0.0062(15) N2 0.0515(18) 0.0360(15) 0.0485(18) 0.0018(12) 0.0034(14) -0.0055(13) Pt1 0.05266(7) 0.03814(6) 0.04184(7) 0.00099(6) 0.00110(7) 0.00066(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C3 1.392(6) . ? C1 C7 1.430(5) . ? C1 Pt1 1.991(4) . ? C2 C25 1.178(5) . ? C2 Pt1 1.975(4) . ? C3 C4 1.396(6) . ? C3 H3 0.9300 . ? C4 C5 1.370(7) . ? C4 H4 0.9300 . ? C5 C6 1.373(7) . ? C5 H5 0.9300 . ? C6 C7 1.406(5) . ? C6 H6 0.9300 . ? C7 C8 1.458(6) . ? C8 N1 1.356(5) . ? C8 C9 1.376(6) . ? C9 C10 1.381(7) . ? C9 H9 0.9300 . ? C10 C11 1.375(6) . ? C10 H10 0.9300 . ? C11 C12 1.382(5) . ? C11 H11 0.9300 . ? C12 N1 1.344(5) . ? C12 C13 1.472(5) . ? C13 N2 1.364(4) . ? C13 C14 1.383(5) . ? C14 C15 1.380(5) . ? C14 H14 0.9300 . ? C15 C16 1.407(6) . ? C15 C18 1.494(5) . ? C16 C17 1.375(5) . ? C16 C21 1.492(5) . ? C17 N2 1.345(4) . ? C17 H17 0.9300 . ? C18 C19 1.528(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.544(6) . ? C19 C22 1.559(6) . ? C19 H19 0.9800 . ? C20 C21 1.564(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.570(5) . ? C21 H21 0.9800 . ? C22 C23 1.500(6) . ? C22 C24 1.526(6) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.441(5) . ? C26 C27 1.383(5) . ? C26 C31 1.393(6) . ? C27 C28 1.392(6) . ? C27 H27 0.9300 . ? C28 C29 1.359(7) . ? C28 H28 0.9300 . ? C29 C30 1.348(7) . ? C29 H29 0.9300 . ? C30 C31 1.374(6) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? N1 Pt1 1.988(3) . ? N2 Pt1 2.103(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 C3 C1 C7 117.6(4) . . ? C3 C1 Pt1 131.0(3) . . ? C7 C1 Pt1 111.5(3) . . ? C25 C2 Pt1 176.3(3) . . ? C1 C3 C4 121.8(5) . . ? C1 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C5 C4 C3 119.6(5) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.1(4) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C7 120.3(4) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C1 119.7(4) . . ? C6 C7 C8 123.5(4) . . ? C1 C7 C8 116.8(3) . . ? N1 C8 C9 117.2(4) . . ? N1 C8 C7 112.3(3) . . ? C9 C8 C7 130.4(4) . . ? C8 C9 C10 120.2(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 120.9(4) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 118.3(4) . . ? C10 C11 H11 120.9 . . ? C12 C11 H11 120.9 . . ? N1 C12 C11 119.4(4) . . ? N1 C12 C13 113.9(3) . . ? C11 C12 C13 126.7(4) . . ? N2 C13 C14 120.9(3) . . ? N2 C13 C12 114.9(3) . . ? C14 C13 C12 124.2(4) . . ? C15 C14 C13 120.9(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 117.8(3) . . ? C14 C15 C18 124.2(4) . . ? C16 C15 C18 118.0(3) . . ? C17 C16 C15 118.8(3) . . ? C17 C16 C21 124.3(4) . . ? C15 C16 C21 116.9(3) . . ? N2 C17 C16 123.3(3) . . ? N2 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? C15 C18 C19 111.2(3) . . ? C15 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? C15 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C20 108.7(4) . . ? C18 C19 C22 110.7(4) . . ? C20 C19 C22 88.2(4) . . ? C18 C19 H19 115.4 . . ? C20 C19 H19 115.4 . . ? C22 C19 H19 115.4 . . ? C19 C20 C21 86.0(3) . . ? C19 C20 H20A 114.3 . . ? C21 C20 H20A 114.3 . . ? C19 C20 H20B 114.3 . . ? C21 C20 H20B 114.3 . . ? H20A C20 H20B 111.5 . . ? C16 C21 C20 106.7(4) . . ? C16 C21 C22 109.4(3) . . ? C20 C21 C22 87.1(3) . . ? C16 C21 H21 116.6 . . ? C20 C21 H21 116.6 . . ? C22 C21 H21 116.6 . . ? C23 C22 C24 109.0(4) . . ? C23 C22 C19 118.4(4) . . ? C24 C22 C19 112.3(4) . . ? C23 C22 C21 118.9(3) . . ? C24 C22 C21 111.3(3) . . ? C19 C22 C21 85.3(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C2 C25 C26 177.3(4) . . ? C27 C26 C31 117.5(4) . . ? C27 C26 C25 121.5(3) . . ? C31 C26 C25 120.9(3) . . ? C26 C27 C28 120.2(4) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 120.7(5) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C30 C29 C28 119.8(5) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 120.9(5) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C30 C31 C26 120.9(4) . . ? C30 C31 H31 119.5 . . ? C26 C31 H31 119.5 . . ? C12 N1 C8 124.0(3) . . ? C12 N1 Pt1 118.9(2) . . ? C8 N1 Pt1 117.1(3) . . ? C17 N2 C13 118.3(3) . . ? C17 N2 Pt1 128.0(2) . . ? C13 N2 Pt1 113.6(2) . . ? C2 Pt1 N1 178.23(15) . . ? C2 Pt1 C1 98.95(17) . . ? N1 Pt1 C1 82.31(15) . . ? C2 Pt1 N2 100.16(13) . . ? N1 Pt1 N2 78.57(11) . . ? C1 Pt1 N2 160.88(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 C7 C1 C3 C4 -0.4(6) . . . . ? Pt1 C1 C3 C4 179.0(3) . . . . ? C1 C3 C4 C5 -0.1(6) . . . . ? C3 C4 C5 C6 0.1(7) . . . . ? C4 C5 C6 C7 0.4(7) . . . . ? C5 C6 C7 C1 -1.0(6) . . . . ? C5 C6 C7 C8 179.2(4) . . . . ? C3 C1 C7 C6 0.9(5) . . . . ? Pt1 C1 C7 C6 -178.6(3) . . . . ? C3 C1 C7 C8 -179.2(3) . . . . ? Pt1 C1 C7 C8 1.3(4) . . . . ? C6 C7 C8 N1 179.2(4) . . . . ? C1 C7 C8 N1 -0.7(5) . . . . ? C6 C7 C8 C9 0.0(7) . . . . ? C1 C7 C8 C9 -179.8(4) . . . . ? N1 C8 C9 C10 -1.1(6) . . . . ? C7 C8 C9 C10 178.0(4) . . . . ? C8 C9 C10 C11 0.2(7) . . . . ? C9 C10 C11 C12 0.9(6) . . . . ? C10 C11 C12 N1 -1.0(5) . . . . ? C10 C11 C12 C13 179.3(4) . . . . ? N1 C12 C13 N2 -1.6(4) . . . . ? C11 C12 C13 N2 178.1(3) . . . . ? N1 C12 C13 C14 177.0(3) . . . . ? C11 C12 C13 C14 -3.2(6) . . . . ? N2 C13 C14 C15 1.2(5) . . . . ? C12 C13 C14 C15 -177.4(4) . . . . ? C13 C14 C15 C16 -2.1(5) . . . . ? C13 C14 C15 C18 176.2(4) . . . . ? C14 C15 C16 C17 1.6(5) . . . . ? C18 C15 C16 C17 -176.8(4) . . . . ? C14 C15 C16 C21 -179.3(4) . . . . ? C18 C15 C16 C21 2.3(5) . . . . ? C15 C16 C17 N2 -0.2(6) . . . . ? C21 C16 C17 N2 -179.1(4) . . . . ? C14 C15 C18 C19 179.1(4) . . . . ? C16 C15 C18 C19 -2.6(5) . . . . ? C15 C18 C19 C20 -46.0(5) . . . . ? C15 C18 C19 C22 49.2(5) . . . . ? C18 C19 C20 C21 83.8(4) . . . . ? C22 C19 C20 C21 -27.5(4) . . . . ? C17 C16 C21 C20 -135.6(4) . . . . ? C15 C16 C21 C20 45.4(4) . . . . ? C17 C16 C21 C22 131.6(4) . . . . ? C15 C16 C21 C22 -47.4(5) . . . . ? C19 C20 C21 C16 -82.1(4) . . . . ? C19 C20 C21 C22 27.3(4) . . . . ? C18 C19 C22 C23 38.5(5) . . . . ? C20 C19 C22 C23 147.8(4) . . . . ? C18 C19 C22 C24 167.0(3) . . . . ? C20 C19 C22 C24 -83.7(4) . . . . ? C18 C19 C22 C21 -81.9(4) . . . . ? C20 C19 C22 C21 27.4(3) . . . . ? C16 C21 C22 C23 -40.3(6) . . . . ? C20 C21 C22 C23 -147.0(4) . . . . ? C16 C21 C22 C24 -168.3(4) . . . . ? C20 C21 C22 C24 85.1(5) . . . . ? C16 C21 C22 C19 79.6(4) . . . . ? C20 C21 C22 C19 -27.0(4) . . . . ? Pt1 C2 C25 C26 -67(12) . . . . ? C2 C25 C26 C27 77(9) . . . . ? C2 C25 C26 C31 -101(9) . . . . ? C31 C26 C27 C28 0.4(6) . . . . ? C25 C26 C27 C28 -177.8(4) . . . . ? C26 C27 C28 C29 -0.3(8) . . . . ? C27 C28 C29 C30 0.1(9) . . . . ? C28 C29 C30 C31 0.1(8) . . . . ? C29 C30 C31 C26 0.0(7) . . . . ? C27 C26 C31 C30 -0.3(6) . . . . ? C25 C26 C31 C30 177.9(4) . . . . ? C11 C12 N1 C8 0.1(5) . . . . ? C13 C12 N1 C8 179.8(3) . . . . ? C11 C12 N1 Pt1 -177.9(3) . . . . ? C13 C12 N1 Pt1 1.9(4) . . . . ? C9 C8 N1 C12 1.0(5) . . . . ? C7 C8 N1 C12 -178.3(3) . . . . ? C9 C8 N1 Pt1 179.0(3) . . . . ? C7 C8 N1 Pt1 -0.3(4) . . . . ? C16 C17 N2 C13 -0.8(5) . . . . ? C16 C17 N2 Pt1 177.2(3) . . . . ? C14 C13 N2 C17 0.4(5) . . . . ? C12 C13 N2 C17 179.1(3) . . . . ? C14 C13 N2 Pt1 -178.0(3) . . . . ? C12 C13 N2 Pt1 0.7(4) . . . . ? C25 C2 Pt1 N1 -40(8) . . . . ? C25 C2 Pt1 C1 -175(5) . . . . ? C25 C2 Pt1 N2 4(5) . . . . ? C12 N1 Pt1 C2 43(4) . . . . ? C8 N1 Pt1 C2 -135(4) . . . . ? C12 N1 Pt1 C1 178.9(3) . . . . ? C8 N1 Pt1 C1 0.8(3) . . . . ? C12 N1 Pt1 N2 -1.2(2) . . . . ? C8 N1 Pt1 N2 -179.3(3) . . . . ? C3 C1 Pt1 C2 -1.8(4) . . . . ? C7 C1 Pt1 C2 177.7(3) . . . . ? C3 C1 Pt1 N1 179.5(4) . . . . ? C7 C1 Pt1 N1 -1.1(3) . . . . ? C3 C1 Pt1 N2 179.3(3) . . . . ? C7 C1 Pt1 N2 -1.3(6) . . . . ? C17 N2 Pt1 C2 3.3(3) . . . . ? C13 N2 Pt1 C2 -178.6(2) . . . . ? C17 N2 Pt1 N1 -178.0(3) . . . . ? C13 N2 Pt1 N1 0.2(2) . . . . ? C17 N2 Pt1 C1 -177.8(4) . . . . ? C13 N2 Pt1 C1 0.3(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.704 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.062 _database_code_depnum_ccdc_archive 'CCDC 952003' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo_20130412a_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H26 N2 Pt' _chemical_formula_sum 'C31 H26 N2 Pt' _chemical_formula_weight 621.63 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 Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.2882(15) _cell_length_b 11.994(3) _cell_length_c 32.734(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2468.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3988 _cell_measurement_theta_min 2.489 _cell_measurement_theta_max 23.0625 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 5.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2794 _exptl_absorpt_correction_T_max 0.4816 _exptl_absorpt_process_details SADABS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Smart Aepex CCD' _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 17028 _diffrn_reflns_av_R_equivalents 0.1742 _diffrn_reflns_av_sigmaI/netI 0.1358 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4803 _reflns_number_gt 3569 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART,(Bruker,2000) _computing_cell_refinement SMART _computing_data_reduction SAINT(Bruker,2000) _computing_structure_solution 'SHELXTL(Bruker,2000) ' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0500P)^2^+0.5500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(3) _chemical_absolute_configuration unk _refine_ls_number_reflns 4803 _refine_ls_number_parameters 279 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.1629 _refine_ls_wR_factor_gt 0.1559 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 C2 C 0.5759(18) 0.9021(10) 0.1599(3) 0.044(3) Uani 1 1 d . . . C1 C 0.5185(10) 0.8442(5) 0.25033(17) 0.043(3) Uani 1 1 d GU . . C3 C 0.3347(11) 0.9085(6) 0.2506(2) 0.063(2) Uani 1 1 d GU . . H3 H 0.2903 0.9443 0.2269 0.076 Uiso 1 1 calc R . . C4 C 0.2172(11) 0.9194(7) 0.2864(2) 0.063(2) Uani 1 1 d GU . . H4 H 0.0943 0.9625 0.2866 0.076 Uiso 1 1 calc R . . C5 C 0.2836(13) 0.8659(8) 0.3218(2) 0.067(3) Uani 1 1 d GU . . H5 H 0.2050 0.8732 0.3457 0.080 Uiso 1 1 calc R . . C6 C 0.4674(13) 0.8015(7) 0.32152(18) 0.062(3) Uani 1 1 d GU . . H6 H 0.5118 0.7657 0.3452 0.075 Uiso 1 1 calc R . . C7 C 0.5849(11) 0.7907(6) 0.2858(2) 0.046(3) Uani 1 1 d GU . . C8 C 0.7725(17) 0.7221(10) 0.2832(4) 0.055(4) Uani 1 1 d . . . C9 C 0.873(2) 0.6637(13) 0.3133(4) 0.065(4) Uani 1 1 d . . . H9 H 0.8188 0.6644 0.3397 0.078 Uiso 1 1 calc R . . C10 C 1.055(2) 0.6038(11) 0.3050(4) 0.058(4) Uani 1 1 d . . . H10 H 1.1177 0.5611 0.3254 0.070 Uiso 1 1 calc R . . C11 C 1.1451(19) 0.6069(9) 0.2661(4) 0.046(3) Uani 1 1 d . . . H11 H 1.2691 0.5682 0.2599 0.055 Uiso 1 1 calc R . . C12 C 1.0422(18) 0.6696(10) 0.2379(3) 0.046(3) Uani 1 1 d . . . C13 C 1.1002(15) 0.6746(11) 0.1934(4) 0.048(3) Uani 1 1 d . . . C14 C 1.2677(18) 0.6244(10) 0.1764(4) 0.052(3) Uani 1 1 d . . . H14 H 1.3621 0.5858 0.1931 0.062 Uiso 1 1 calc R . . C15 C 1.305(2) 0.6276(11) 0.1353(5) 0.062(4) Uani 1 1 d . . . C16 C 1.1624(16) 0.6925(11) 0.1116(4) 0.053(3) Uani 1 1 d . . . C17 C 1.0025(19) 0.7486(12) 0.1290(4) 0.061(4) Uani 1 1 d . . . H17 H 0.9118 0.7911 0.1128 0.073 Uiso 1 1 calc R . . C18 C 1.478(2) 0.5666(16) 0.1116(4) 0.080(4) Uani 1 1 d . . . H18A H 1.6160 0.5926 0.1209 0.096 Uiso 1 1 calc R . . H18B H 1.4690 0.4875 0.1176 0.096 Uiso 1 1 calc R . . C19 C 1.465(2) 0.5826(15) 0.0665(5) 0.080(4) Uani 1 1 d . . . H19 H 1.5744 0.5445 0.0505 0.096 Uiso 1 1 calc R . . C20 C 1.441(3) 0.7127(15) 0.0580(5) 0.091(6) Uani 1 1 d . . . H20A H 1.5086 0.7602 0.0782 0.110 Uiso 1 1 calc R . . H20B H 1.4767 0.7355 0.0304 0.110 Uiso 1 1 calc R . . C21 C 1.199(2) 0.6910(12) 0.0655(4) 0.069(4) Uani 1 1 d . . . H21 H 1.1007 0.7358 0.0491 0.083 Uiso 1 1 calc R . . C22 C 1.236(2) 0.5690(14) 0.0507(5) 0.073(4) Uani 1 1 d . . . C23 C 1.092(3) 0.4809(16) 0.0680(6) 0.103(7) Uani 1 1 d . . . H23A H 1.1199 0.4722 0.0966 0.155 Uiso 1 1 calc R . . H23B H 1.1171 0.4115 0.0542 0.155 Uiso 1 1 calc R . . H23C H 0.9465 0.5029 0.0641 0.155 Uiso 1 1 calc R . . C24 C 1.225(3) 0.5574(17) 0.0034(5) 0.116(7) Uani 1 1 d . . . H24A H 1.0813 0.5675 -0.0055 0.173 Uiso 1 1 calc R . . H24B H 1.2740 0.4846 -0.0044 0.173 Uiso 1 1 calc R . . H24C H 1.3143 0.6130 -0.0090 0.173 Uiso 1 1 calc R . . C25 C 0.526(2) 0.9608(14) 0.1344(5) 0.074(5) Uani 1 1 d . . . C26 C 0.467(2) 1.0392(11) 0.1006(4) 0.051(3) Uani 1 1 d . . . C27 C 0.610(3) 1.1209(13) 0.0890(4) 0.076(5) Uani 1 1 d . . . H27 H 0.7424 1.1230 0.1017 0.091 Uiso 1 1 calc R . . C28 C 0.563(3) 1.2030(16) 0.0582(5) 0.093(6) Uani 1 1 d . . . H28 H 0.6578 1.2596 0.0515 0.112 Uiso 1 1 calc R . . C29 C 0.371(3) 1.1923(18) 0.0396(5) 0.104(5) Uani 1 1 d . . . H29 H 0.3409 1.2397 0.0178 0.125 Uiso 1 1 calc R . . C30 C 0.211(4) 1.1119(16) 0.0513(5) 0.104(5) Uani 1 1 d . . . H30 H 0.0763 1.1106 0.0396 0.125 Uiso 1 1 calc R . . C31 C 0.271(3) 1.0382(14) 0.0808(4) 0.087(5) Uani 1 1 d . . . H31 H 0.1747 0.9831 0.0882 0.105 Uiso 1 1 calc R . . N1 N 0.8596(15) 0.7238(9) 0.2456(3) 0.049(3) Uani 1 1 d . . . N2 N 0.9703(16) 0.7441(10) 0.1713(3) 0.055(3) Uani 1 1 d . . . Pt1 Pt 0.71320(7) 0.81152(4) 0.203226(15) 0.04586(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.040(6) 0.061(8) 0.031(6) -0.011(5) -0.001(5) -0.013(6) C1 0.061(6) 0.039(7) 0.028(5) -0.009(4) -0.005(5) -0.005(5) C3 0.074(5) 0.043(5) 0.071(5) -0.003(4) 0.008(4) 0.007(4) C4 0.074(5) 0.043(5) 0.071(5) -0.003(4) 0.008(4) 0.007(4) C5 0.066(6) 0.080(9) 0.056(6) -0.019(5) -0.008(6) 0.013(6) C6 0.065(6) 0.072(9) 0.050(6) 0.008(6) 0.001(5) 0.003(6) C7 0.045(5) 0.035(7) 0.057(6) -0.019(4) -0.020(4) -0.006(4) C8 0.029(5) 0.042(7) 0.093(10) 0.016(6) -0.007(6) 0.009(5) C9 0.049(6) 0.090(12) 0.057(8) 0.007(7) -0.022(7) 0.004(7) C10 0.075(8) 0.049(8) 0.051(9) 0.009(6) -0.028(7) -0.002(6) C11 0.048(7) 0.033(7) 0.056(8) 0.000(5) -0.007(6) 0.013(5) C12 0.054(6) 0.046(8) 0.038(7) -0.006(5) -0.011(6) -0.003(6) C13 0.033(5) 0.053(8) 0.060(8) -0.002(6) -0.022(5) -0.010(5) C14 0.029(6) 0.044(7) 0.082(9) -0.005(6) -0.010(6) -0.011(5) C15 0.032(6) 0.066(8) 0.087(10) -0.026(7) -0.012(7) 0.015(6) C16 0.037(6) 0.052(7) 0.068(8) -0.021(7) 0.002(6) -0.007(6) C17 0.040(7) 0.066(10) 0.075(10) 0.001(7) -0.016(7) 0.005(6) C18 0.043(5) 0.127(10) 0.069(7) -0.002(7) 0.000(6) 0.016(6) C19 0.043(5) 0.127(10) 0.069(7) -0.002(7) 0.000(6) 0.016(6) C20 0.096(11) 0.110(16) 0.069(11) 0.012(9) 0.033(9) -0.007(11) C21 0.062(7) 0.077(9) 0.068(8) 0.026(7) -0.017(7) 0.001(10) C22 0.059(9) 0.080(10) 0.080(10) -0.014(8) -0.003(8) 0.015(8) C23 0.094(13) 0.108(16) 0.107(15) -0.001(11) 0.002(12) 0.016(11) C24 0.102(13) 0.179(18) 0.066(11) -0.044(11) 0.002(11) 0.016(15) C25 0.050(7) 0.093(12) 0.078(10) -0.038(8) -0.040(7) 0.032(7) C26 0.056(7) 0.059(8) 0.037(7) -0.013(6) -0.017(6) 0.003(6) C27 0.084(10) 0.090(11) 0.055(9) 0.031(8) -0.004(9) 0.017(9) C28 0.101(12) 0.093(14) 0.085(12) 0.006(10) 0.014(10) 0.005(12) C29 0.136(12) 0.119(11) 0.058(7) 0.013(7) -0.014(8) 0.034(10) C30 0.136(12) 0.119(11) 0.058(7) 0.013(7) -0.014(8) 0.034(10) C31 0.086(10) 0.128(14) 0.047(8) -0.012(8) -0.036(9) 0.021(11) N1 0.038(5) 0.066(8) 0.043(6) 0.004(4) 0.009(5) -0.011(5) N2 0.035(5) 0.083(8) 0.048(7) -0.006(6) 0.007(5) -0.007(5) Pt1 0.03539(18) 0.0490(2) 0.0532(3) 0.0046(2) -0.0158(2) 0.0005(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 C2 C25 1.135(19) . ? C2 Pt1 1.985(12) . ? C1 C3 1.3900 . ? C1 C7 1.3900 . ? C1 Pt1 2.007(6) . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 C8 1.441(12) . ? C8 N1 1.349(15) . ? C8 C9 1.364(18) . ? C9 C10 1.376(19) . ? C9 H9 0.9300 . ? C10 C11 1.393(17) . ? C10 H10 0.9300 . ? C11 C12 1.356(16) . ? C11 H11 0.9300 . ? C12 N1 1.343(15) . ? C12 C13 1.502(16) . ? C13 C14 1.336(16) . ? C13 N2 1.372(15) . ? C14 C15 1.366(19) . ? C14 H14 0.9300 . ? C15 C16 1.418(18) . ? C15 C18 1.525(19) . ? C16 C17 1.337(17) . ? C16 C21 1.527(17) . ? C17 N2 1.403(16) . ? C17 H17 0.9300 . ? C18 C19 1.49(2) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C22 1.53(2) . ? C19 C20 1.59(2) . ? C19 H19 0.9800 . ? C20 C21 1.56(2) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.56(2) . ? C21 H21 0.9800 . ? C22 C23 1.50(2) . ? C22 C24 1.56(2) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.50(2) . ? C26 C27 1.383(19) . ? C26 C31 1.390(19) . ? C27 C28 1.44(2) . ? C27 H27 0.9300 . ? C28 C29 1.36(2) . ? C28 H28 0.9300 . ? C29 C30 1.45(3) . ? C29 H29 0.9300 . ? C30 C31 1.36(2) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? N1 Pt1 1.968(10) . ? N2 Pt1 2.088(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C25 C2 Pt1 169.9(12) . . ? C3 C1 C7 120.0 . . ? C3 C1 Pt1 128.4(3) . . ? C7 C1 Pt1 111.6(3) . . ? C4 C3 C1 120.0 . . ? C4 C3 H3 120.0 . . ? C1 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C1 120.0 . . ? C6 C7 C8 122.5(7) . . ? C1 C7 C8 117.4(7) . . ? N1 C8 C9 118.6(11) . . ? N1 C8 C7 112.2(10) . . ? C9 C8 C7 129.2(12) . . ? C8 C9 C10 120.8(13) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 120.2(12) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 116.3(11) . . ? C12 C11 H11 121.9 . . ? C10 C11 H11 121.9 . . ? N1 C12 C11 123.4(11) . . ? N1 C12 C13 111.6(10) . . ? C11 C12 C13 124.5(11) . . ? C14 C13 N2 121.5(11) . . ? C14 C13 C12 125.3(11) . . ? N2 C13 C12 113.0(10) . . ? C13 C14 C15 122.3(12) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C14 C15 C16 116.4(11) . . ? C14 C15 C18 127.7(13) . . ? C16 C15 C18 115.9(13) . . ? C17 C16 C15 121.4(12) . . ? C17 C16 C21 122.6(12) . . ? C15 C16 C21 116.0(11) . . ? C16 C17 N2 120.6(12) . . ? C16 C17 H17 119.7 . . ? N2 C17 H17 119.7 . . ? C19 C18 C15 113.7(13) . . ? C19 C18 H18A 108.8 . . ? C15 C18 H18A 108.8 . . ? C19 C18 H18B 108.8 . . ? C15 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C18 C19 C22 111.9(12) . . ? C18 C19 C20 107.7(14) . . ? C22 C19 C20 87.7(12) . . ? C18 C19 H19 115.4 . . ? C22 C19 H19 115.4 . . ? C20 C19 H19 115.4 . . ? C21 C20 C19 84.2(11) . . ? C21 C20 H20A 114.6 . . ? C19 C20 H20A 114.6 . . ? C21 C20 H20B 114.6 . . ? C19 C20 H20B 114.6 . . ? H20A C20 H20B 111.7 . . ? C16 C21 C22 109.9(11) . . ? C16 C21 C20 107.5(11) . . ? C22 C21 C20 87.8(12) . . ? C16 C21 H21 116.0 . . ? C22 C21 H21 116.0 . . ? C20 C21 H21 116.0 . . ? C23 C22 C19 120.9(14) . . ? C23 C22 C24 106.6(14) . . ? C19 C22 C24 112.7(13) . . ? C23 C22 C21 116.9(13) . . ? C19 C22 C21 86.3(11) . . ? C24 C22 C21 112.7(13) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C2 C25 C26 178.2(15) . . ? C27 C26 C31 117.0(13) . . ? C27 C26 C25 119.0(12) . . ? C31 C26 C25 123.9(13) . . ? C26 C27 C28 122.8(15) . . ? C26 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? C29 C28 C27 115.7(18) . . ? C29 C28 H28 122.2 . . ? C27 C28 H28 122.2 . . ? C28 C29 C30 124.2(17) . . ? C28 C29 H29 117.9 . . ? C30 C29 H29 117.9 . . ? C31 C30 C29 115.2(19) . . ? C31 C30 H30 122.4 . . ? C29 C30 H30 122.4 . . ? C30 C31 C26 124.8(18) . . ? C30 C31 H31 117.6 . . ? C26 C31 H31 117.6 . . ? C12 N1 C8 120.7(10) . . ? C12 N1 Pt1 121.8(8) . . ? C8 N1 Pt1 117.5(8) . . ? C13 N2 C17 117.3(11) . . ? C13 N2 Pt1 115.6(8) . . ? C17 N2 Pt1 126.2(9) . . ? N1 Pt1 C2 177.9(4) . . ? N1 Pt1 C1 81.3(3) . . ? C2 Pt1 C1 100.2(4) . . ? N1 Pt1 N2 77.4(4) . . ? C2 Pt1 N2 101.0(5) . . ? C1 Pt1 N2 158.8(4) . . ? 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 C7 C1 C3 C4 0.0 . . . . ? Pt1 C1 C3 C4 178.5(4) . . . . ? C1 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C1 0.0 . . . . ? C5 C6 C7 C8 -177.8(8) . . . . ? C3 C1 C7 C6 0.0 . . . . ? Pt1 C1 C7 C6 -178.7(4) . . . . ? C3 C1 C7 C8 177.9(8) . . . . ? Pt1 C1 C7 C8 -0.8(7) . . . . ? C6 C7 C8 N1 179.7(7) . . . . ? C1 C7 C8 N1 1.8(12) . . . . ? C6 C7 C8 C9 -4.1(17) . . . . ? C1 C7 C8 C9 178.1(12) . . . . ? N1 C8 C9 C10 -3(2) . . . . ? C7 C8 C9 C10 -178.9(11) . . . . ? C8 C9 C10 C11 4(2) . . . . ? C9 C10 C11 C12 -1.1(18) . . . . ? C10 C11 C12 N1 -2.1(18) . . . . ? C10 C11 C12 C13 -173.4(11) . . . . ? N1 C12 C13 C14 -176.9(11) . . . . ? C11 C12 C13 C14 -4.7(19) . . . . ? N1 C12 C13 N2 7.5(14) . . . . ? C11 C12 C13 N2 179.7(12) . . . . ? N2 C13 C14 C15 -8.2(18) . . . . ? C12 C13 C14 C15 176.5(11) . . . . ? C13 C14 C15 C16 3.2(18) . . . . ? C13 C14 C15 C18 -174.6(13) . . . . ? C14 C15 C16 C17 1.1(19) . . . . ? C18 C15 C16 C17 179.2(13) . . . . ? C14 C15 C16 C21 -177.2(11) . . . . ? C18 C15 C16 C21 0.9(17) . . . . ? C15 C16 C17 N2 -1(2) . . . . ? C21 C16 C17 N2 177.6(12) . . . . ? C14 C15 C18 C19 176.0(13) . . . . ? C16 C15 C18 C19 -2(2) . . . . ? C15 C18 C19 C22 -46(2) . . . . ? C15 C18 C19 C20 49.2(17) . . . . ? C18 C19 C20 C21 -84.6(12) . . . . ? C22 C19 C20 C21 27.7(11) . . . . ? C17 C16 C21 C22 -132.4(13) . . . . ? C15 C16 C21 C22 45.9(15) . . . . ? C17 C16 C21 C20 133.5(14) . . . . ? C15 C16 C21 C20 -48.3(16) . . . . ? C19 C20 C21 C16 83.0(13) . . . . ? C19 C20 C21 C22 -27.2(10) . . . . ? C18 C19 C22 C23 -39(2) . . . . ? C20 C19 C22 C23 -147.0(15) . . . . ? C18 C19 C22 C24 -166.5(15) . . . . ? C20 C19 C22 C24 85.4(15) . . . . ? C18 C19 C22 C21 80.4(15) . . . . ? C20 C19 C22 C21 -27.7(10) . . . . ? C16 C21 C22 C23 43.4(17) . . . . ? C20 C21 C22 C23 151.2(14) . . . . ? C16 C21 C22 C19 -79.6(12) . . . . ? C20 C21 C22 C19 28.2(11) . . . . ? C16 C21 C22 C24 167.4(12) . . . . ? C20 C21 C22 C24 -84.8(14) . . . . ? Pt1 C2 C25 C26 12(58) . . . . ? C2 C25 C26 C27 -22(53) . . . . ? C2 C25 C26 C31 161(52) . . . . ? C31 C26 C27 C28 0(2) . . . . ? C25 C26 C27 C28 -177.0(14) . . . . ? C26 C27 C28 C29 -3(2) . . . . ? C27 C28 C29 C30 6(3) . . . . ? C28 C29 C30 C31 -6(3) . . . . ? C29 C30 C31 C26 3(3) . . . . ? C27 C26 C31 C30 -1(2) . . . . ? C25 C26 C31 C30 176.7(15) . . . . ? C11 C12 N1 C8 2.9(19) . . . . ? C13 C12 N1 C8 175.2(10) . . . . ? C11 C12 N1 Pt1 -178.8(9) . . . . ? C13 C12 N1 Pt1 -6.5(14) . . . . ? C9 C8 N1 C12 -0.3(18) . . . . ? C7 C8 N1 C12 176.4(10) . . . . ? C9 C8 N1 Pt1 -178.7(10) . . . . ? C7 C8 N1 Pt1 -2.0(12) . . . . ? C14 C13 N2 C17 8.4(17) . . . . ? C12 C13 N2 C17 -175.8(10) . . . . ? C14 C13 N2 Pt1 178.6(9) . . . . ? C12 C13 N2 Pt1 -5.6(13) . . . . ? C16 C17 N2 C13 -4.1(18) . . . . ? C16 C17 N2 Pt1 -173.1(10) . . . . ? C12 N1 Pt1 C2 -41(13) . . . . ? C8 N1 Pt1 C2 138(13) . . . . ? C12 N1 Pt1 C1 -177.0(10) . . . . ? C8 N1 Pt1 C1 1.3(8) . . . . ? C12 N1 Pt1 N2 2.9(9) . . . . ? C8 N1 Pt1 N2 -178.8(9) . . . . ? C25 C2 Pt1 N1 -11(18) . . . . ? C25 C2 Pt1 C1 125(7) . . . . ? C25 C2 Pt1 N2 -54(7) . . . . ? C3 C1 Pt1 N1 -178.8(5) . . . . ? C7 C1 Pt1 N1 -0.2(4) . . . . ? C3 C1 Pt1 C2 2.7(5) . . . . ? C7 C1 Pt1 C2 -178.7(4) . . . . ? C3 C1 Pt1 N2 -179.0(9) . . . . ? C7 C1 Pt1 N2 -0.4(11) . . . . ? C13 N2 Pt1 N1 1.9(9) . . . . ? C17 N2 Pt1 N1 171.1(11) . . . . ? C13 N2 Pt1 C2 -179.6(9) . . . . ? C17 N2 Pt1 C2 -10.4(11) . . . . ? C13 N2 Pt1 C1 2.1(16) . . . . ? C17 N2 Pt1 C1 171.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.061 _refine_diff_density_min -2.309 _refine_diff_density_rms 0.248 _database_code_depnum_ccdc_archive 'CCDC 952004' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo_20130330c_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H26 N2 Pt' _chemical_formula_sum 'C31 H26 N2 Pt' _chemical_formula_weight 621.63 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 Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.018(3) _cell_length_b 15.716(8) _cell_length_c 25.260(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2389(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3608 _cell_measurement_theta_min 2.592 _cell_measurement_theta_max 22.6415 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 5.895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2990 _exptl_absorpt_correction_T_max 0.4523 _exptl_absorpt_process_details SADABS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Smart Aepex CCD' _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 16636 _diffrn_reflns_av_R_equivalents 0.1698 _diffrn_reflns_av_sigmaI/netI 0.1302 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4191 _reflns_number_gt 3240 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART,(Bruker,2000) _computing_cell_refinement SMART _computing_data_reduction SAINT(Bruker,2000) _computing_structure_solution 'SHELXTL(Bruker,2000) ' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0450P)^2^+0.5500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _chemical_absolute_configuration unk _refine_ls_number_reflns 4191 _refine_ls_number_parameters 309 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 C1 C 0.702(2) 0.9683(6) 0.8980(4) 0.057(3) Uani 1 1 d U . . C2 C 0.6218(17) 0.9944(6) 0.7805(4) 0.046(3) Uani 1 1 d . . . C3 C 0.502(2) 1.0176(7) 0.9072(5) 0.065(3) Uani 1 1 d . . . H3 H 0.4189 1.0381 0.8789 0.078 Uiso 1 1 calc R . . C4 C 0.436(2) 1.0339(8) 0.9589(5) 0.069(4) Uani 1 1 d . . . H4 H 0.3058 1.0639 0.9659 0.083 Uiso 1 1 calc R . . C5 C 0.570(3) 1.0042(8) 1.0003(5) 0.086(5) Uani 1 1 d . . . H5 H 0.5321 1.0189 1.0348 0.103 Uiso 1 1 calc R . . C6 C 0.756(2) 0.9535(7) 0.9921(5) 0.073(4) Uani 1 1 d . . . H6 H 0.8362 0.9308 1.0202 0.087 Uiso 1 1 calc R . . C7 C 0.8161(19) 0.9388(8) 0.9407(3) 0.058(2) Uani 1 1 d U . . C8 C 1.014(2) 0.8855(6) 0.9264(5) 0.057(3) Uani 1 1 d . . . C9 C 1.163(3) 0.8467(7) 0.9606(4) 0.069(3) Uani 1 1 d . . . H9 H 1.1426 0.8501 0.9971 0.083 Uiso 1 1 calc R . . C10 C 1.340(2) 0.8031(8) 0.9398(5) 0.078(4) Uani 1 1 d . . . H10 H 1.4409 0.7771 0.9624 0.094 Uiso 1 1 calc R . . C11 C 1.3692(17) 0.7971(6) 0.8858(4) 0.054(3) Uani 1 1 d . . . H11 H 1.4897 0.7682 0.8714 0.065 Uiso 1 1 calc R . . C12 C 1.2141(18) 0.8357(6) 0.8542(4) 0.052(3) Uani 1 1 d . . . C13 C 1.2143(16) 0.8359(6) 0.7959(4) 0.047(3) Uani 1 1 d . . . C14 C 1.3637(18) 0.7924(6) 0.7653(4) 0.055(3) Uani 1 1 d . . . H14 H 1.4765 0.7619 0.7819 0.067 Uiso 1 1 calc R . . C15 C 1.3524(18) 0.7922(5) 0.7110(4) 0.046(3) Uani 1 1 d . . . C16 C 1.179(2) 0.8396(6) 0.6878(4) 0.049(3) Uani 1 1 d . . . C17 C 1.0292(19) 0.8802(6) 0.7199(4) 0.047(3) Uani 1 1 d . . . H17 H 0.9132 0.9100 0.7042 0.056 Uiso 1 1 calc R . . C18 C 1.5009(19) 0.7422(6) 0.6738(5) 0.062(3) Uani 1 1 d . . . H18A H 1.6544 0.7582 0.6799 0.075 Uiso 1 1 calc R . . H18B H 1.4863 0.6820 0.6815 0.075 Uiso 1 1 calc R . . C19 C 1.444(2) 0.7575(8) 0.6173(6) 0.076(4) Uani 1 1 d . . . H19 H 1.5405 0.7293 0.5914 0.091 Uiso 1 1 calc R . . C20 C 1.403(2) 0.8524(9) 0.6078(6) 0.089(5) Uani 1 1 d . . . H20A H 1.4088 0.8691 0.5708 0.106 Uiso 1 1 calc R . . H20B H 1.4927 0.8898 0.6296 0.106 Uiso 1 1 calc R . . C21 C 1.165(2) 0.8384(7) 0.6289(4) 0.059(3) Uani 1 1 d . . . H21 H 1.0477 0.8732 0.6129 0.071 Uiso 1 1 calc R . . C22 C 1.185(2) 0.7449(7) 0.6085(4) 0.059(3) Uani 1 1 d . . . C23 C 1.0690(16) 0.6748(7) 0.6397(5) 0.061(3) Uani 1 1 d . . . H23A H 1.0589 0.6911 0.6763 0.091 Uiso 1 1 calc R . . H23B H 1.1526 0.6230 0.6368 0.091 Uiso 1 1 calc R . . H23C H 0.9224 0.6662 0.6257 0.091 Uiso 1 1 calc R . . C24 C 1.123(3) 0.7403(11) 0.5492(6) 0.101(5) Uani 1 1 d . . . H24A H 1.1471 0.6836 0.5364 0.151 Uiso 1 1 calc R . . H24B H 1.2133 0.7794 0.5296 0.151 Uiso 1 1 calc R . . H24C H 0.9690 0.7551 0.5449 0.151 Uiso 1 1 calc R . . C25 C 0.5066(18) 1.0267(7) 0.7482(4) 0.049(3) Uani 1 1 d . . . C26 C 0.3560(16) 1.0623(7) 0.7093(4) 0.045(2) Uani 1 1 d . . . C27 C 0.4182(16) 1.0687(8) 0.6573(4) 0.058(3) Uani 1 1 d . . . H27 H 0.5581 1.0501 0.6467 0.069 Uiso 1 1 calc R . . C28 C 0.274(2) 1.1024(10) 0.6207(5) 0.079(5) Uani 1 1 d . . . H28 H 0.3166 1.1048 0.5853 0.095 Uiso 1 1 calc R . . C29 C 0.070(2) 1.1327(10) 0.6353(7) 0.088(5) Uani 1 1 d . . . H29 H -0.0247 1.1565 0.6104 0.106 Uiso 1 1 calc R . . C30 C 0.009(2) 1.1272(8) 0.6871(6) 0.084(5) Uani 1 1 d . . . H30 H -0.1298 1.1472 0.6977 0.101 Uiso 1 1 calc R . . C31 C 0.1486(19) 1.0926(6) 0.7233(5) 0.058(3) Uani 1 1 d . . . H31 H 0.1038 1.0892 0.7585 0.070 Uiso 1 1 calc R . . N1 N 1.0416(15) 0.8763(5) 0.8745(3) 0.044(2) Uani 1 1 d . . . N2 N 1.0414(16) 0.8792(5) 0.7730(4) 0.050(2) Uani 1 1 d . . . Pt1 Pt 0.82782(6) 0.93471(2) 0.828069(15) 0.04260(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 C1 0.100(8) 0.040(4) 0.031(5) -0.006(4) 0.017(5) -0.026(5) C2 0.061(7) 0.044(5) 0.033(5) -0.008(4) 0.012(5) -0.004(4) C3 0.093(8) 0.045(6) 0.057(7) -0.005(5) 0.019(6) -0.025(6) C4 0.080(8) 0.052(6) 0.074(9) -0.007(6) 0.023(6) -0.011(6) C5 0.137(13) 0.067(7) 0.054(8) -0.002(7) 0.020(8) -0.014(8) C6 0.090(9) 0.061(7) 0.067(8) -0.012(6) -0.003(6) -0.005(5) C7 0.072(6) 0.068(6) 0.032(5) -0.005(5) 0.011(4) -0.016(7) C8 0.075(7) 0.029(4) 0.068(8) 0.007(4) -0.015(6) -0.020(5) C9 0.102(8) 0.067(6) 0.038(6) 0.012(5) -0.019(7) -0.022(8) C10 0.083(7) 0.071(7) 0.080(8) 0.007(7) -0.046(7) -0.011(8) C11 0.056(6) 0.039(5) 0.066(7) 0.001(5) -0.025(5) -0.002(5) C12 0.064(7) 0.041(5) 0.051(6) 0.002(5) -0.012(5) -0.013(5) C13 0.043(6) 0.037(4) 0.062(7) -0.004(5) -0.010(5) -0.004(4) C14 0.053(6) 0.038(5) 0.075(7) -0.001(5) -0.013(5) 0.006(5) C15 0.047(6) 0.027(4) 0.065(7) -0.009(4) -0.012(5) 0.010(4) C16 0.055(5) 0.038(4) 0.055(6) 0.006(4) 0.015(5) -0.002(5) C17 0.063(6) 0.037(5) 0.040(6) 0.003(4) -0.007(5) 0.008(5) C18 0.056(6) 0.054(5) 0.077(7) -0.020(6) -0.001(7) 0.010(5) C19 0.059(7) 0.052(6) 0.117(12) 0.000(7) 0.025(7) 0.020(5) C20 0.101(11) 0.078(9) 0.088(10) 0.008(8) 0.035(7) -0.008(7) C21 0.058(6) 0.053(5) 0.066(7) 0.010(5) 0.019(6) 0.020(6) C22 0.058(6) 0.071(7) 0.047(6) -0.005(5) 0.009(6) 0.015(6) C23 0.037(5) 0.049(6) 0.097(9) -0.014(6) 0.007(5) -0.008(4) C24 0.102(12) 0.114(12) 0.087(10) -0.029(9) -0.016(9) 0.026(9) C25 0.050(6) 0.049(5) 0.048(7) -0.002(5) 0.004(5) 0.000(5) C26 0.043(5) 0.044(4) 0.047(5) -0.002(5) 0.003(4) 0.014(6) C27 0.040(5) 0.076(7) 0.057(7) 0.013(7) 0.004(4) 0.011(6) C28 0.088(11) 0.095(10) 0.055(8) 0.015(7) -0.006(6) 0.005(7) C29 0.083(9) 0.074(9) 0.107(12) 0.003(8) -0.026(8) 0.028(7) C30 0.061(7) 0.055(6) 0.135(14) -0.013(7) -0.019(8) 0.019(6) C31 0.040(6) 0.057(6) 0.077(8) -0.014(5) 0.006(6) 0.019(5) N1 0.065(5) 0.046(4) 0.022(4) -0.002(3) -0.003(4) -0.008(4) N2 0.070(6) 0.023(4) 0.056(6) -0.002(3) -0.011(4) 0.009(4) Pt1 0.04876(17) 0.03747(13) 0.04157(18) 0.00103(18) -0.00090(18) -0.00046(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 C1 C7 1.363(15) . ? C1 C3 1.450(18) . ? C1 Pt1 1.993(10) . ? C2 C25 1.185(14) . ? C2 Pt1 1.965(10) . ? C3 C4 1.389(17) . ? C3 H3 0.9300 . ? C4 C5 1.399(19) . ? C4 H4 0.9300 . ? C5 C6 1.392(19) . ? C5 H5 0.9300 . ? C6 C7 1.365(16) . ? C6 H6 0.9300 . ? C7 C8 1.502(17) . ? C8 N1 1.329(13) . ? C8 C9 1.385(17) . ? C9 C10 1.37(2) . ? C9 H9 0.9300 . ? C10 C11 1.379(16) . ? C10 H10 0.9300 . ? C11 C12 1.369(14) . ? C11 H11 0.9300 . ? C12 N1 1.322(14) . ? C12 C13 1.474(13) . ? C13 C14 1.369(15) . ? C13 N2 1.372(13) . ? C14 C15 1.375(14) . ? C14 H14 0.9300 . ? C15 C16 1.411(15) . ? C15 C18 1.515(15) . ? C16 C17 1.369(15) . ? C16 C21 1.490(14) . ? C17 N2 1.342(13) . ? C17 H17 0.9300 . ? C18 C19 1.487(19) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.532(19) . ? C19 C22 1.589(18) . ? C19 H19 0.9800 . ? C20 C21 1.543(19) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.560(15) . ? C21 H21 0.9800 . ? C22 C23 1.523(16) . ? C22 C24 1.546(17) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.448(15) . ? C26 C27 1.372(13) . ? C26 C31 1.381(14) . ? C27 C28 1.371(17) . ? C27 H27 0.9300 . ? C28 C29 1.368(19) . ? C28 H28 0.9300 . ? C29 C30 1.36(2) . ? C29 H29 0.9300 . ? C30 C31 1.357(18) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? N1 Pt1 1.968(8) . ? N2 Pt1 2.086(9) . ? 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 C7 C1 C3 118.3(10) . . ? C7 C1 Pt1 114.8(9) . . ? C3 C1 Pt1 126.9(8) . . ? C25 C2 Pt1 174.2(9) . . ? C4 C3 C1 119.2(12) . . ? C4 C3 H3 120.4 . . ? C1 C3 H3 120.4 . . ? C3 C4 C5 118.4(13) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C6 C5 C4 123.0(12) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C7 C6 C5 116.8(12) . . ? C7 C6 H6 121.6 . . ? C5 C6 H6 121.6 . . ? C1 C7 C6 124.2(12) . . ? C1 C7 C8 113.6(9) . . ? C6 C7 C8 122.2(10) . . ? N1 C8 C9 119.3(11) . . ? N1 C8 C7 113.3(9) . . ? C9 C8 C7 127.4(11) . . ? C10 C9 C8 118.8(11) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 120.9(11) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 117.3(11) . . ? C12 C11 H11 121.4 . . ? C10 C11 H11 121.4 . . ? N1 C12 C11 121.6(10) . . ? N1 C12 C13 112.7(9) . . ? C11 C12 C13 125.7(10) . . ? C14 C13 N2 120.5(10) . . ? C14 C13 C12 124.3(10) . . ? N2 C13 C12 115.1(9) . . ? C13 C14 C15 122.1(10) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C14 C15 C16 116.7(9) . . ? C14 C15 C18 126.2(9) . . ? C16 C15 C18 117.0(9) . . ? C17 C16 C15 119.2(9) . . ? C17 C16 C21 124.1(10) . . ? C15 C16 C21 116.6(9) . . ? N2 C17 C16 123.3(10) . . ? N2 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? C19 C18 C15 112.0(9) . . ? C19 C18 H18A 109.2 . . ? C15 C18 H18A 109.2 . . ? C19 C18 H18B 109.2 . . ? C15 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C18 C19 C20 110.3(12) . . ? C18 C19 C22 109.9(10) . . ? C20 C19 C22 86.5(10) . . ? C18 C19 H19 115.6 . . ? C20 C19 H19 115.6 . . ? C22 C19 H19 115.6 . . ? C19 C20 C21 87.5(10) . . ? C19 C20 H20A 114.1 . . ? C21 C20 H20A 114.1 . . ? C19 C20 H20B 114.1 . . ? C21 C20 H20B 114.1 . . ? H20A C20 H20B 111.2 . . ? C16 C21 C20 107.0(11) . . ? C16 C21 C22 109.7(8) . . ? C20 C21 C22 87.1(9) . . ? C16 C21 H21 116.4 . . ? C20 C21 H21 116.4 . . ? C22 C21 H21 116.4 . . ? C23 C22 C24 110.8(11) . . ? C23 C22 C21 118.3(9) . . ? C24 C22 C21 110.2(10) . . ? C23 C22 C19 117.9(10) . . ? C24 C22 C19 112.3(11) . . ? C21 C22 C19 85.0(9) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C2 C25 C26 176.6(12) . . ? C27 C26 C31 117.8(10) . . ? C27 C26 C25 120.4(9) . . ? C31 C26 C25 121.7(9) . . ? C28 C27 C26 120.1(11) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C27 121.3(13) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C30 C29 C28 118.8(14) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C31 C30 C29 120.2(13) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C26 121.8(12) . . ? C30 C31 H31 119.1 . . ? C26 C31 H31 119.1 . . ? C12 N1 C8 122.1(9) . . ? C12 N1 Pt1 120.5(6) . . ? C8 N1 Pt1 117.2(7) . . ? C17 N2 C13 118.0(9) . . ? C17 N2 Pt1 128.9(7) . . ? C13 N2 Pt1 113.1(7) . . ? C2 Pt1 N1 178.3(4) . . ? C2 Pt1 C1 100.1(5) . . ? N1 Pt1 C1 81.1(4) . . ? C2 Pt1 N2 100.4(4) . . ? N1 Pt1 N2 78.5(3) . . ? C1 Pt1 N2 159.5(4) . . ? 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 C7 C1 C3 C4 0.8(15) . . . . ? Pt1 C1 C3 C4 178.8(8) . . . . ? C1 C3 C4 C5 2.0(16) . . . . ? C3 C4 C5 C6 -5.0(19) . . . . ? C4 C5 C6 C7 5.0(19) . . . . ? C3 C1 C7 C6 -0.8(17) . . . . ? Pt1 C1 C7 C6 -179.1(9) . . . . ? C3 C1 C7 C8 177.6(9) . . . . ? Pt1 C1 C7 C8 -0.7(12) . . . . ? C5 C6 C7 C1 -1.9(18) . . . . ? C5 C6 C7 C8 179.8(11) . . . . ? C1 C7 C8 N1 -0.5(13) . . . . ? C6 C7 C8 N1 178.0(10) . . . . ? C1 C7 C8 C9 -179.9(11) . . . . ? C6 C7 C8 C9 -1.5(18) . . . . ? N1 C8 C9 C10 3.1(17) . . . . ? C7 C8 C9 C10 -177.5(11) . . . . ? C8 C9 C10 C11 -0.6(18) . . . . ? C9 C10 C11 C12 -0.7(17) . . . . ? C10 C11 C12 N1 -0.6(15) . . . . ? C10 C11 C12 C13 -179.3(10) . . . . ? N1 C12 C13 C14 -174.3(9) . . . . ? C11 C12 C13 C14 4.6(17) . . . . ? N1 C12 C13 N2 1.4(13) . . . . ? C11 C12 C13 N2 -179.8(9) . . . . ? N2 C13 C14 C15 2.3(15) . . . . ? C12 C13 C14 C15 177.7(9) . . . . ? C13 C14 C15 C16 0.2(14) . . . . ? C13 C14 C15 C18 -176.3(10) . . . . ? C14 C15 C16 C17 -2.1(14) . . . . ? C18 C15 C16 C17 174.7(10) . . . . ? C14 C15 C16 C21 -179.2(9) . . . . ? C18 C15 C16 C21 -2.4(14) . . . . ? C15 C16 C17 N2 1.7(15) . . . . ? C21 C16 C17 N2 178.5(10) . . . . ? C14 C15 C18 C19 -179.5(10) . . . . ? C16 C15 C18 C19 4.1(14) . . . . ? C15 C18 C19 C20 43.2(14) . . . . ? C15 C18 C19 C22 -50.4(12) . . . . ? C18 C19 C20 C21 -82.1(11) . . . . ? C22 C19 C20 C21 27.7(10) . . . . ? C17 C16 C21 C20 137.5(11) . . . . ? C15 C16 C21 C20 -45.6(12) . . . . ? C17 C16 C21 C22 -129.4(11) . . . . ? C15 C16 C21 C22 47.5(14) . . . . ? C19 C20 C21 C16 81.5(11) . . . . ? C19 C20 C21 C22 -28.3(10) . . . . ? C16 C21 C22 C23 39.3(15) . . . . ? C20 C21 C22 C23 146.3(11) . . . . ? C16 C21 C22 C24 168.3(11) . . . . ? C20 C21 C22 C24 -84.7(13) . . . . ? C16 C21 C22 C19 -79.8(11) . . . . ? C20 C21 C22 C19 27.3(10) . . . . ? C18 C19 C22 C23 -36.7(14) . . . . ? C20 C19 C22 C23 -147.0(11) . . . . ? C18 C19 C22 C24 -167.4(11) . . . . ? C20 C19 C22 C24 82.3(12) . . . . ? C18 C19 C22 C21 82.8(10) . . . . ? C20 C19 C22 C21 -27.5(10) . . . . ? Pt1 C2 C25 C26 96(21) . . . . ? C2 C25 C26 C27 -120(19) . . . . ? C2 C25 C26 C31 62(19) . . . . ? C31 C26 C27 C28 -1.4(19) . . . . ? C25 C26 C27 C28 179.9(12) . . . . ? C26 C27 C28 C29 2(2) . . . . ? C27 C28 C29 C30 -1(2) . . . . ? C28 C29 C30 C31 0(2) . . . . ? C29 C30 C31 C26 0(2) . . . . ? C27 C26 C31 C30 0.4(18) . . . . ? C25 C26 C31 C30 179.0(11) . . . . ? C11 C12 N1 C8 3.2(15) . . . . ? C13 C12 N1 C8 -177.9(9) . . . . ? C11 C12 N1 Pt1 177.7(7) . . . . ? C13 C12 N1 Pt1 -3.4(11) . . . . ? C9 C8 N1 C12 -4.5(15) . . . . ? C7 C8 N1 C12 176.1(9) . . . . ? C9 C8 N1 Pt1 -179.1(8) . . . . ? C7 C8 N1 Pt1 1.5(11) . . . . ? C16 C17 N2 C13 0.8(14) . . . . ? C16 C17 N2 Pt1 -178.7(8) . . . . ? C14 C13 N2 C17 -2.7(14) . . . . ? C12 C13 N2 C17 -178.5(9) . . . . ? C14 C13 N2 Pt1 176.9(8) . . . . ? C12 C13 N2 Pt1 1.0(10) . . . . ? C25 C2 Pt1 N1 55(18) . . . . ? C25 C2 Pt1 C1 -173(9) . . . . ? C25 C2 Pt1 N2 8(9) . . . . ? C12 N1 Pt1 C2 -43(13) . . . . ? C8 N1 Pt1 C2 131(13) . . . . ? C12 N1 Pt1 C1 -176.1(8) . . . . ? C8 N1 Pt1 C1 -1.5(7) . . . . ? C12 N1 Pt1 N2 3.2(7) . . . . ? C8 N1 Pt1 N2 177.9(8) . . . . ? C7 C1 Pt1 C2 -177.6(8) . . . . ? C3 C1 Pt1 C2 4.3(10) . . . . ? C7 C1 Pt1 N1 1.1(8) . . . . ? C3 C1 Pt1 N1 -177.0(9) . . . . ? C7 C1 Pt1 N2 -0.8(16) . . . . ? C3 C1 Pt1 N2 -178.9(9) . . . . ? C17 N2 Pt1 C2 -3.9(9) . . . . ? C13 N2 Pt1 C2 176.6(7) . . . . ? C17 N2 Pt1 N1 177.4(9) . . . . ? C13 N2 Pt1 N1 -2.1(6) . . . . ? C17 N2 Pt1 C1 179.3(10) . . . . ? C13 N2 Pt1 C1 -0.2(14) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.661 _refine_diff_density_min -1.280 _refine_diff_density_rms 0.185 _database_code_depnum_ccdc_archive 'CCDC 952005'