Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Armando Pombeiro' _publ_contact_author_address ; Centro de Quimica Estrutural, Complexo I Instituto Superior Tecnico, TU Lisbon Av. Rovisco Pais, S/N Lisbon 1049-001 PORTUGAL ; _publ_contact_author_email POMBEIRO@IST.UTL.PT _publ_section_title ; Microwave Synthesis of Mono- and Bis-Tetrazolato Complexes via 1,3-Dipolar Cycloaddition of Organonitriles with Platinum(II)-bound Azides ; loop_ _publ_author_name 'Armando J. L. Pombeiro' 'Adilia Charmier' 'M.F.C.G.da Silva' 'Jamal Lasri' ; S.Mukhopadhyay ; data_sm_c66 _database_code_depnum_ccdc_archive 'CCDC 652528' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H35 N5 P2 Pt' _chemical_formula_sum 'C40 H35 N5 P2 Pt' _chemical_formula_weight 842.76 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' P P 0.1023 0.0942 '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 Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 9.3467(5) _cell_length_b 15.5678(9) _cell_length_c 12.3442(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.967(3) _cell_angle_gamma 90.00 _cell_volume 1774.22(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8657 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 30.50 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 4.081 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.7361 _exptl_absorpt_correction_T_max 0.8220 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26752 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8860 _reflns_number_gt 8121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 mixed _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 -0.004(4) _refine_ls_number_reflns 8860 _refine_ls_number_parameters 433 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0515 _refine_ls_wR_factor_gt 0.0501 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.039 _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 C1 C 1.0143(5) 0.4907(2) 0.4251(3) 0.0279(9) Uani 1 1 d . . . C2 C 0.9668(6) 0.3985(2) 0.4088(4) 0.0378(11) Uani 1 1 d . . . H2A H 0.9714 0.3815 0.3322 0.045 Uiso 1 1 calc R . . H2B H 0.8647 0.3935 0.4206 0.045 Uiso 1 1 calc R . . C3 C 1.0592(7) 0.3370(3) 0.4860(4) 0.0483(14) Uani 1 1 d . . . H3A H 1.0233 0.2782 0.4723 0.072 Uiso 1 1 calc R . . H3B H 1.0540 0.3529 0.5621 0.072 Uiso 1 1 calc R . . H3C H 1.1600 0.3403 0.4732 0.072 Uiso 1 1 calc R . . C101 C 0.8135(6) 0.8306(3) 0.2119(3) 0.0288(10) Uani 1 1 d . . . C102 C 0.8214(6) 0.8601(3) 0.1064(4) 0.0432(12) Uani 1 1 d . . . H102 H 0.9100 0.8560 0.0781 0.052 Uiso 1 1 calc R . . C103 C 0.7001(9) 0.8953(4) 0.0427(5) 0.061(2) Uani 1 1 d . . . H103 H 0.7066 0.9168 -0.0284 0.073 Uiso 1 1 calc R . . C104 C 0.5701(8) 0.8992(3) 0.0825(6) 0.071(2) Uani 1 1 d . . . H104 H 0.4883 0.9256 0.0401 0.085 Uiso 1 1 calc R . . C105 C 0.5592(6) 0.8651(4) 0.1827(5) 0.0599(16) Uani 1 1 d . . . H105 H 0.4679 0.8637 0.2074 0.072 Uiso 1 1 calc R . . C106 C 0.6813(6) 0.8324(3) 0.2490(4) 0.0414(12) Uani 1 1 d . . . H106 H 0.6738 0.8113 0.3201 0.050 Uiso 1 1 calc R . . C111 C 1.0319(4) 0.7039(2) 0.2091(3) 0.0220(8) Uani 1 1 d . . . C112 C 0.9281(5) 0.6498(2) 0.1530(3) 0.0319(9) Uani 1 1 d . . . H112 H 0.8294 0.6556 0.1620 0.038 Uiso 1 1 calc R . . C113 C 0.9686(6) 0.5866(3) 0.0830(4) 0.0397(12) Uani 1 1 d . . . H113 H 0.8975 0.5496 0.0441 0.048 Uiso 1 1 calc R . . C114 C 1.1098(6) 0.5785(3) 0.0709(3) 0.0382(11) Uani 1 1 d . . . H114 H 1.1371 0.5358 0.0230 0.046 Uiso 1 1 calc R . . C115 C 1.2146(6) 0.6316(3) 0.1274(3) 0.0376(11) Uani 1 1 d . . . H115 H 1.3133 0.6257 0.1186 0.045 Uiso 1 1 calc R . . C116 C 1.1738(5) 0.6936(3) 0.1969(3) 0.0314(10) Uani 1 1 d . . . H116 H 1.2455 0.7295 0.2369 0.038 Uiso 1 1 calc R . . C121 C 1.1176(5) 0.8650(2) 0.3163(3) 0.0267(8) Uani 1 1 d . . . C122 C 1.2297(6) 0.8493(3) 0.4024(4) 0.0398(11) Uani 1 1 d . . . H122 H 1.2236 0.8015 0.4493 0.048 Uiso 1 1 calc R . . C123 C 1.3500(6) 0.9024(3) 0.4205(4) 0.0539(14) Uani 1 1 d . . . H123 H 1.4257 0.8913 0.4797 0.065 Uiso 1 1 calc R . . C124 C 1.3589(7) 0.9711(3) 0.3521(4) 0.0566(16) Uani 1 1 d . . . H124 H 1.4413 1.0077 0.3642 0.068 Uiso 1 1 calc R . . C125 C 1.2501(7) 0.9876(3) 0.2665(5) 0.0523(15) Uani 1 1 d . . . H125 H 1.2578 1.0351 0.2194 0.063 Uiso 1 1 calc R . . C126 C 1.1278(6) 0.9347(2) 0.2485(4) 0.0386(11) Uani 1 1 d . . . H126 H 1.0519 0.9466 0.1897 0.046 Uiso 1 1 calc R . . C201 C 0.7270(4) 0.7244(2) 0.6665(3) 0.0215(7) Uani 1 1 d . . . C202 C 0.6776(5) 0.7814(2) 0.7395(3) 0.0278(9) Uani 1 1 d . . . H202 H 0.7452 0.8125 0.7903 0.033 Uiso 1 1 calc R . . C203 C 0.5304(5) 0.7928(3) 0.7383(4) 0.0380(10) Uani 1 1 d . . . H203 H 0.4974 0.8322 0.7878 0.046 Uiso 1 1 calc R . . C204 C 0.4311(6) 0.7472(2) 0.6651(4) 0.0400(11) Uani 1 1 d . . . H204 H 0.3302 0.7556 0.6641 0.048 Uiso 1 1 calc R . . C205 C 0.4788(5) 0.6894(3) 0.5938(4) 0.0375(10) Uani 1 1 d . . . H205 H 0.4109 0.6571 0.5448 0.045 Uiso 1 1 calc R . . C206 C 0.6258(5) 0.6786(2) 0.5938(3) 0.0293(9) Uani 1 1 d . . . H206 H 0.6581 0.6395 0.5436 0.035 Uiso 1 1 calc R . . C211 C 1.0219(4) 0.7855(2) 0.7493(3) 0.0213(7) Uani 1 1 d . . . C212 C 1.0437(6) 0.7642(2) 0.8606(3) 0.0350(10) Uani 1 1 d . . . H212 H 0.9998 0.7142 0.8847 0.042 Uiso 1 1 calc R . . C213 C 1.1296(6) 0.8163(3) 0.9364(4) 0.0492(14) Uani 1 1 d . . . H213 H 1.1439 0.8018 1.0121 0.059 Uiso 1 1 calc R . . C214 C 1.1931(7) 0.8880(4) 0.9017(5) 0.0483(16) Uani 1 1 d . . . H214 H 1.2502 0.9237 0.9539 0.058 Uiso 1 1 calc R . . C215 C 1.1759(5) 0.9092(2) 0.7932(4) 0.0392(11) Uani 1 1 d . . . H215 H 1.2218 0.9589 0.7701 0.047 Uiso 1 1 calc R . . C216 C 1.0897(5) 0.8571(3) 0.7154(4) 0.0274(10) Uani 1 1 d . . . H216 H 1.0784 0.8713 0.6397 0.033 Uiso 1 1 calc R . . C221 C 0.9729(4) 0.6080(2) 0.7044(3) 0.0192(7) Uani 1 1 d . . . C222 C 1.1130(4) 0.5824(2) 0.6947(3) 0.0218(8) Uani 1 1 d . . . H222 H 1.1716 0.6180 0.6570 0.026 Uiso 1 1 calc R . . C223 C 1.1674(5) 0.5057(3) 0.7392(3) 0.0260(9) Uani 1 1 d . . . H223 H 1.2629 0.4886 0.7318 0.031 Uiso 1 1 calc R . . C224 C 1.0839(5) 0.4538(2) 0.7943(3) 0.0279(9) Uani 1 1 d . . . H224 H 1.1220 0.4011 0.8251 0.033 Uiso 1 1 calc R . . C225 C 0.9441(5) 0.4782(2) 0.8051(3) 0.0278(9) Uani 1 1 d . . . H225 H 0.8865 0.4420 0.8429 0.033 Uiso 1 1 calc R . . C226 C 0.8882(5) 0.5557(2) 0.7607(3) 0.0240(8) Uani 1 1 d . . . H226 H 0.7929 0.5729 0.7687 0.029 Uiso 1 1 calc R . . N1 N 0.9248(4) 0.55459(16) 0.4408(2) 0.0211(7) Uani 1 1 d . . . N11 N 1.0113(4) 0.62343(18) 0.4478(3) 0.0207(7) Uani 1 1 d . . . N12 N 1.1452(4) 0.6028(2) 0.4387(3) 0.0271(7) Uani 1 1 d . . . N13 N 1.1497(4) 0.5177(2) 0.4244(3) 0.0308(8) Uani 1 1 d . . . C21 C 0.8564(6) 0.8581(2) 0.4940(3) 0.0312(11) Uani 1 1 d . . . N21 N 0.8087(6) 0.9232(2) 0.5076(3) 0.0488(12) Uani 1 1 d . . . P1 P 0.97138(14) 0.78637(6) 0.29762(9) 0.0216(2) Uani 1 1 d . . . P2 P 0.91525(13) 0.71341(5) 0.65208(9) 0.01797(19) Uani 1 1 d . . . Pt1 Pt 0.93717(4) 0.743432(6) 0.47167(3) 0.01914(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(3) 0.0255(18) 0.0214(18) 0.0005(14) 0.0038(18) 0.0056(17) C2 0.053(3) 0.0200(17) 0.038(2) -0.0066(16) 0.000(2) 0.0062(18) C3 0.063(4) 0.032(2) 0.047(3) 0.0014(19) -0.001(3) 0.010(2) C101 0.033(3) 0.026(2) 0.027(2) -0.0011(17) 0.0061(19) 0.0072(19) C102 0.042(3) 0.049(3) 0.037(2) 0.015(2) -0.001(2) 0.002(2) C103 0.076(6) 0.047(4) 0.049(4) 0.020(3) -0.024(4) -0.004(3) C104 0.065(5) 0.045(3) 0.085(5) -0.013(3) -0.039(4) 0.021(3) C105 0.027(3) 0.076(4) 0.073(4) -0.034(3) -0.003(3) 0.012(3) C106 0.031(3) 0.054(3) 0.037(2) -0.020(2) -0.001(2) 0.008(2) C111 0.027(2) 0.0219(16) 0.0177(16) 0.0036(13) 0.0053(15) 0.0037(15) C112 0.031(3) 0.033(2) 0.034(2) -0.0024(17) 0.0131(19) -0.0041(18) C113 0.053(4) 0.032(2) 0.035(2) -0.0093(18) 0.012(2) -0.010(2) C114 0.052(4) 0.034(2) 0.031(2) -0.0038(17) 0.013(2) 0.011(2) C115 0.034(3) 0.047(2) 0.034(2) 0.0012(19) 0.012(2) 0.013(2) C116 0.027(3) 0.039(2) 0.027(2) -0.0049(16) 0.0031(18) 0.0028(18) C121 0.027(2) 0.0259(17) 0.029(2) -0.0026(15) 0.0110(17) -0.0053(16) C122 0.036(3) 0.049(3) 0.037(2) -0.0014(19) 0.013(2) -0.015(2) C123 0.047(4) 0.070(3) 0.044(3) -0.008(2) 0.005(3) -0.025(3) C124 0.064(4) 0.054(3) 0.059(3) -0.023(3) 0.032(3) -0.039(3) C125 0.074(5) 0.028(2) 0.063(3) -0.004(2) 0.035(3) -0.015(2) C126 0.054(3) 0.0250(19) 0.040(2) 0.0060(17) 0.015(2) -0.002(2) C201 0.022(2) 0.0192(15) 0.0237(17) 0.0039(13) 0.0046(15) 0.0019(14) C202 0.027(3) 0.0234(17) 0.035(2) 0.0001(15) 0.0119(19) 0.0022(16) C203 0.031(3) 0.034(2) 0.052(3) 0.0009(19) 0.016(2) 0.0097(19) C204 0.024(2) 0.038(2) 0.059(3) 0.019(2) 0.008(2) 0.0063(19) C205 0.024(3) 0.042(2) 0.045(3) 0.0050(19) -0.002(2) -0.0033(19) C206 0.025(2) 0.0331(19) 0.030(2) -0.0028(16) 0.0066(18) -0.0041(17) C211 0.019(2) 0.0183(16) 0.0263(18) -0.0029(14) 0.0037(15) 0.0028(15) C212 0.045(3) 0.0287(19) 0.029(2) -0.0027(15) 0.000(2) -0.0019(18) C213 0.064(4) 0.040(2) 0.036(2) -0.0111(19) -0.013(3) 0.008(2) C214 0.032(3) 0.041(3) 0.065(4) -0.021(3) -0.015(3) 0.007(2) C215 0.027(3) 0.0199(18) 0.070(3) -0.0069(19) 0.002(2) -0.0028(17) C216 0.022(3) 0.023(2) 0.038(2) -0.0021(17) 0.0048(19) 0.0019(17) C221 0.020(2) 0.0227(16) 0.0152(16) -0.0023(12) 0.0039(14) 0.0005(14) C222 0.020(2) 0.0245(17) 0.0206(17) 0.0009(13) 0.0013(15) -0.0014(15) C223 0.022(3) 0.0317(19) 0.023(2) 0.0017(17) 0.0023(17) 0.0098(16) C224 0.036(3) 0.0221(17) 0.0238(19) 0.0027(14) -0.0008(18) 0.0039(16) C225 0.032(3) 0.0250(17) 0.027(2) 0.0056(15) 0.0069(18) -0.0042(17) C226 0.021(2) 0.0258(17) 0.0261(19) -0.0007(14) 0.0064(16) -0.0032(15) N1 0.0212(19) 0.0202(12) 0.0213(16) -0.0016(10) 0.0014(16) 0.0004(13) N11 0.020(2) 0.0233(14) 0.0193(16) 0.0018(11) 0.0050(14) 0.0010(12) N12 0.0170(19) 0.0354(17) 0.0304(18) 0.0069(13) 0.0083(15) 0.0030(14) N13 0.027(2) 0.0366(17) 0.0308(18) 0.0033(14) 0.0116(16) 0.0131(15) C21 0.048(3) 0.0283(19) 0.0178(19) 0.0021(15) 0.0070(19) 0.0048(19) N21 0.080(4) 0.0333(19) 0.032(2) 0.0023(16) 0.007(2) 0.018(2) P1 0.0259(6) 0.0201(4) 0.0197(5) 0.0023(3) 0.0064(4) 0.0009(4) P2 0.0194(5) 0.0168(4) 0.0182(4) 0.0009(3) 0.0045(4) -0.0013(4) Pt1 0.02446(6) 0.01604(5) 0.01769(5) 0.00098(12) 0.00573(4) -0.00009(14) _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 N13 1.335(6) . ? C1 N1 1.333(5) . ? C1 C2 1.507(5) . ? C2 C3 1.521(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C101 C106 1.383(7) . ? C101 C102 1.393(6) . ? C101 P1 1.812(5) . ? C102 C103 1.387(8) . ? C102 H102 0.9500 . ? C103 C104 1.382(10) . ? C103 H103 0.9500 . ? C104 C105 1.365(9) . ? C104 H104 0.9500 . ? C105 C106 1.393(7) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C111 C116 1.368(6) . ? C111 C112 1.386(5) . ? C111 P1 1.831(4) . ? C112 C113 1.400(6) . ? C112 H112 0.9500 . ? C113 C114 1.357(7) . ? C113 H113 0.9500 . ? C114 C115 1.386(7) . ? C114 H114 0.9500 . ? C115 C116 1.383(6) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C126 1.382(5) . ? C121 C122 1.393(6) . ? C121 P1 1.823(4) . ? C122 C123 1.385(7) . ? C122 H122 0.9500 . ? C123 C124 1.374(7) . ? C123 H123 0.9500 . ? C124 C125 1.371(8) . ? C124 H124 0.9500 . ? C125 C126 1.398(7) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C201 C202 1.393(6) . ? C201 C206 1.394(5) . ? C201 P2 1.804(4) . ? C202 C203 1.385(6) . ? C202 H202 0.9500 . ? C203 C204 1.386(7) . ? C203 H203 0.9500 . ? C204 C205 1.380(7) . ? C204 H204 0.9500 . ? C205 C206 1.384(6) . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? C211 C216 1.380(5) . ? C211 C212 1.396(5) . ? C211 P2 1.822(4) . ? C212 C213 1.394(6) . ? C212 H212 0.9500 . ? C213 C214 1.364(8) . ? C213 H213 0.9500 . ? C214 C215 1.365(7) . ? C214 H214 0.9500 . ? C215 C216 1.409(6) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C222 1.392(5) . ? C221 C226 1.394(5) . ? C221 P2 1.814(3) . ? C222 C223 1.378(5) . ? C222 H222 0.9500 . ? C223 C224 1.375(6) . ? C223 H223 0.9500 . ? C224 C225 1.386(6) . ? C224 H224 0.9500 . ? C225 C226 1.394(5) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? N1 N11 1.337(4) . ? N11 N12 1.314(5) . ? N11 Pt1 2.030(3) . ? N12 N13 1.338(4) . ? C21 N21 1.130(5) . ? C21 Pt1 1.973(4) . ? P1 Pt1 2.3193(13) . ? P2 Pt1 2.3156(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N13 C1 N1 112.5(3) . . ? N13 C1 C2 124.0(4) . . ? N1 C1 C2 123.5(4) . . ? C1 C2 C3 112.9(4) . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C106 C101 C102 118.9(5) . . ? C106 C101 P1 120.2(3) . . ? C102 C101 P1 120.9(4) . . ? C101 C102 C103 120.2(6) . . ? C101 C102 H102 119.9 . . ? C103 C102 H102 119.9 . . ? C104 C103 C102 120.2(6) . . ? C104 C103 H103 119.9 . . ? C102 C103 H103 119.9 . . ? C105 C104 C103 119.9(5) . . ? C105 C104 H104 120.0 . . ? C103 C104 H104 120.0 . . ? C104 C105 C106 120.3(6) . . ? C104 C105 H105 119.8 . . ? C106 C105 H105 119.8 . . ? C101 C106 C105 120.4(5) . . ? C101 C106 H106 119.8 . . ? C105 C106 H106 119.8 . . ? C116 C111 C112 119.3(4) . . ? C116 C111 P1 122.9(3) . . ? C112 C111 P1 117.8(3) . . ? C111 C112 C113 120.0(4) . . ? C111 C112 H112 120.0 . . ? C113 C112 H112 120.0 . . ? C114 C113 C112 119.7(4) . . ? C114 C113 H113 120.2 . . ? C112 C113 H113 120.2 . . ? C113 C114 C115 120.8(4) . . ? C113 C114 H114 119.6 . . ? C115 C114 H114 119.6 . . ? C116 C115 C114 119.2(5) . . ? C116 C115 H115 120.4 . . ? C114 C115 H115 120.4 . . ? C111 C116 C115 121.1(4) . . ? C111 C116 H116 119.5 . . ? C115 C116 H116 119.5 . . ? C126 C121 C122 119.1(4) . . ? C126 C121 P1 124.9(4) . . ? C122 C121 P1 116.0(3) . . ? C123 C122 C121 120.8(4) . . ? C123 C122 H122 119.6 . . ? C121 C122 H122 119.6 . . ? C124 C123 C122 119.4(5) . . ? C124 C123 H123 120.3 . . ? C122 C123 H123 120.3 . . ? C125 C124 C123 120.7(5) . . ? C125 C124 H124 119.7 . . ? C123 C124 H124 119.7 . . ? C124 C125 C126 120.1(4) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C121 C126 C125 119.8(5) . . ? C121 C126 H126 120.1 . . ? C125 C126 H126 120.1 . . ? C202 C201 C206 118.8(4) . . ? C202 C201 P2 123.4(3) . . ? C206 C201 P2 117.5(3) . . ? C203 C202 C201 120.2(4) . . ? C203 C202 H202 119.9 . . ? C201 C202 H202 119.9 . . ? C202 C203 C204 120.3(4) . . ? C202 C203 H203 119.9 . . ? C204 C203 H203 119.9 . . ? C205 C204 C203 119.9(5) . . ? C205 C204 H204 120.0 . . ? C203 C204 H204 120.0 . . ? C204 C205 C206 119.9(4) . . ? C204 C205 H205 120.0 . . ? C206 C205 H205 120.0 . . ? C205 C206 C201 120.7(4) . . ? C205 C206 H206 119.6 . . ? C201 C206 H206 119.6 . . ? C216 C211 C212 119.1(4) . . ? C216 C211 P2 121.9(3) . . ? C212 C211 P2 118.9(3) . . ? C211 C212 C213 120.2(4) . . ? C211 C212 H212 119.9 . . ? C213 C212 H212 119.9 . . ? C214 C213 C212 119.9(5) . . ? C214 C213 H213 120.1 . . ? C212 C213 H213 120.1 . . ? C213 C214 C215 121.0(5) . . ? C213 C214 H214 119.5 . . ? C215 C214 H214 119.5 . . ? C214 C215 C216 119.8(4) . . ? C214 C215 H215 120.1 . . ? C216 C215 H215 120.1 . . ? C211 C216 C215 120.0(4) . . ? C211 C216 H216 120.0 . . ? C215 C216 H216 120.0 . . ? C222 C221 C226 119.4(3) . . ? C222 C221 P2 117.4(3) . . ? C226 C221 P2 123.0(3) . . ? C223 C222 C221 120.5(4) . . ? C223 C222 H222 119.8 . . ? C221 C222 H222 119.8 . . ? C222 C223 C224 120.2(4) . . ? C222 C223 H223 119.9 . . ? C224 C223 H223 119.9 . . ? C223 C224 C225 120.2(3) . . ? C223 C224 H224 119.9 . . ? C225 C224 H224 119.9 . . ? C224 C225 C226 120.0(4) . . ? C224 C225 H225 120.0 . . ? C226 C225 H225 120.0 . . ? C225 C226 C221 119.6(4) . . ? C225 C226 H226 120.2 . . ? C221 C226 H226 120.2 . . ? N11 N1 C1 102.8(3) . . ? N12 N11 N1 111.9(3) . . ? N12 N11 Pt1 126.0(2) . . ? N1 N11 Pt1 122.1(3) . . ? N11 N12 N13 107.6(3) . . ? C1 N13 N12 105.2(3) . . ? N21 C21 Pt1 179.0(4) . . ? C101 P1 C121 110.2(2) . . ? C101 P1 C111 102.53(19) . . ? C121 P1 C111 104.55(19) . . ? C101 P1 Pt1 115.65(16) . . ? C121 P1 Pt1 106.58(13) . . ? C111 P1 Pt1 116.79(11) . . ? C201 P2 C221 106.93(17) . . ? C201 P2 C211 108.58(17) . . ? C221 P2 C211 102.73(17) . . ? C201 P2 Pt1 108.02(12) . . ? C221 P2 Pt1 117.33(12) . . ? C211 P2 Pt1 112.83(13) . . ? C21 Pt1 N11 177.5(2) . . ? C21 Pt1 P2 87.44(12) . . ? N11 Pt1 P2 92.12(9) . . ? C21 Pt1 P1 88.82(12) . . ? N11 Pt1 P1 91.81(9) . . ? P2 Pt1 P1 174.10(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 N13 C1 C2 C3 52.7(6) . . . . ? N1 C1 C2 C3 -127.9(4) . . . . ? C106 C101 C102 C103 3.8(7) . . . . ? P1 C101 C102 C103 -178.7(4) . . . . ? C101 C102 C103 C104 -1.7(9) . . . . ? C102 C103 C104 C105 -2.8(9) . . . . ? C103 C104 C105 C106 5.1(8) . . . . ? C102 C101 C106 C105 -1.5(7) . . . . ? P1 C101 C106 C105 -179.0(3) . . . . ? C104 C105 C106 C101 -3.0(7) . . . . ? C116 C111 C112 C113 -1.4(6) . . . . ? P1 C111 C112 C113 179.0(3) . . . . ? C111 C112 C113 C114 0.3(6) . . . . ? C112 C113 C114 C115 0.3(7) . . . . ? C113 C114 C115 C116 0.1(7) . . . . ? C112 C111 C116 C115 1.8(6) . . . . ? P1 C111 C116 C115 -178.6(3) . . . . ? C114 C115 C116 C111 -1.1(6) . . . . ? C126 C121 C122 C123 0.1(7) . . . . ? P1 C121 C122 C123 176.6(4) . . . . ? C121 C122 C123 C124 -0.4(8) . . . . ? C122 C123 C124 C125 0.1(8) . . . . ? C123 C124 C125 C126 0.5(8) . . . . ? C122 C121 C126 C125 0.5(7) . . . . ? P1 C121 C126 C125 -175.6(4) . . . . ? C124 C125 C126 C121 -0.8(7) . . . . ? C206 C201 C202 C203 -0.9(6) . . . . ? P2 C201 C202 C203 173.4(3) . . . . ? C201 C202 C203 C204 0.6(6) . . . . ? C202 C203 C204 C205 0.6(6) . . . . ? C203 C204 C205 C206 -1.4(6) . . . . ? C204 C205 C206 C201 1.1(6) . . . . ? C202 C201 C206 C205 0.1(6) . . . . ? P2 C201 C206 C205 -174.5(3) . . . . ? C216 C211 C212 C213 1.8(7) . . . . ? P2 C211 C212 C213 177.4(4) . . . . ? C211 C212 C213 C214 -0.2(8) . . . . ? C212 C213 C214 C215 -1.1(9) . . . . ? C213 C214 C215 C216 0.8(8) . . . . ? C212 C211 C216 C215 -2.0(6) . . . . ? P2 C211 C216 C215 -177.5(3) . . . . ? C214 C215 C216 C211 0.7(7) . . . . ? C226 C221 C222 C223 0.6(5) . . . . ? P2 C221 C222 C223 175.6(3) . . . . ? C221 C222 C223 C224 -0.4(6) . . . . ? C222 C223 C224 C225 0.2(6) . . . . ? C223 C224 C225 C226 -0.4(6) . . . . ? C224 C225 C226 C221 0.7(6) . . . . ? C222 C221 C226 C225 -0.8(5) . . . . ? P2 C221 C226 C225 -175.5(3) . . . . ? N13 C1 N1 N11 1.1(4) . . . . ? C2 C1 N1 N11 -178.3(3) . . . . ? C1 N1 N11 N12 -0.9(4) . . . . ? C1 N1 N11 Pt1 179.8(2) . . . . ? N1 N11 N12 N13 0.4(4) . . . . ? Pt1 N11 N12 N13 179.7(2) . . . . ? N1 C1 N13 N12 -0.9(4) . . . . ? C2 C1 N13 N12 178.5(3) . . . . ? N11 N12 N13 C1 0.3(4) . . . . ? C106 C101 P1 C121 -124.7(4) . . . . ? C102 C101 P1 C121 57.9(4) . . . . ? C106 C101 P1 C111 124.5(4) . . . . ? C102 C101 P1 C111 -53.0(4) . . . . ? C106 C101 P1 Pt1 -3.7(4) . . . . ? C102 C101 P1 Pt1 178.8(3) . . . . ? C126 C121 P1 C101 -20.4(4) . . . . ? C122 C121 P1 C101 163.4(3) . . . . ? C126 C121 P1 C111 89.1(4) . . . . ? C122 C121 P1 C111 -87.1(3) . . . . ? C126 C121 P1 Pt1 -146.6(3) . . . . ? C122 C121 P1 Pt1 37.2(4) . . . . ? C116 C111 P1 C101 134.9(3) . . . . ? C112 C111 P1 C101 -45.5(3) . . . . ? C116 C111 P1 C121 19.9(4) . . . . ? C112 C111 P1 C121 -160.5(3) . . . . ? C116 C111 P1 Pt1 -97.6(3) . . . . ? C112 C111 P1 Pt1 82.0(3) . . . . ? C202 C201 P2 C221 111.7(3) . . . . ? C206 C201 P2 C221 -74.0(3) . . . . ? C202 C201 P2 C211 1.5(4) . . . . ? C206 C201 P2 C211 175.8(3) . . . . ? C202 C201 P2 Pt1 -121.2(3) . . . . ? C206 C201 P2 Pt1 53.1(3) . . . . ? C222 C221 P2 C201 175.6(3) . . . . ? C226 C221 P2 C201 -9.6(3) . . . . ? C222 C221 P2 C211 -70.2(3) . . . . ? C226 C221 P2 C211 104.6(3) . . . . ? C222 C221 P2 Pt1 54.2(3) . . . . ? C226 C221 P2 Pt1 -131.0(3) . . . . ? C216 C211 P2 C201 -110.8(4) . . . . ? C212 C211 P2 C201 73.7(4) . . . . ? C216 C211 P2 C221 136.2(4) . . . . ? C212 C211 P2 C221 -39.4(4) . . . . ? C216 C211 P2 Pt1 8.9(4) . . . . ? C212 C211 P2 Pt1 -166.6(3) . . . . ? N21 C21 Pt1 N11 39(28) . . . . ? N21 C21 Pt1 P2 -41(26) . . . . ? N21 C21 Pt1 P1 143(26) . . . . ? N12 N11 Pt1 C21 173(4) . . . . ? N1 N11 Pt1 C21 -8(4) . . . . ? N12 N11 Pt1 P2 -107.2(3) . . . . ? N1 N11 Pt1 P2 72.0(3) . . . . ? N12 N11 Pt1 P1 68.3(3) . . . . ? N1 N11 Pt1 P1 -112.4(3) . . . . ? C201 P2 Pt1 C21 59.24(19) . . . . ? C221 P2 Pt1 C21 -179.9(2) . . . . ? C211 P2 Pt1 C21 -60.8(2) . . . . ? C201 P2 Pt1 N11 -118.30(15) . . . . ? C221 P2 Pt1 N11 2.56(18) . . . . ? C211 P2 Pt1 N11 121.68(17) . . . . ? C201 P2 Pt1 P1 110.0(6) . . . . ? C221 P2 Pt1 P1 -129.1(5) . . . . ? C211 P2 Pt1 P1 -10.0(6) . . . . ? C101 P1 Pt1 C21 -52.6(2) . . . . ? C121 P1 Pt1 C21 70.2(2) . . . . ? C111 P1 Pt1 C21 -173.4(2) . . . . ? C101 P1 Pt1 N11 124.98(19) . . . . ? C121 P1 Pt1 N11 -112.18(17) . . . . ? C111 P1 Pt1 N11 4.18(19) . . . . ? C101 P1 Pt1 P2 -103.3(6) . . . . ? C121 P1 Pt1 P2 19.5(6) . . . . ? C111 P1 Pt1 P2 135.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.520 _refine_diff_density_min -1.022 _refine_diff_density_rms 0.104 data_sm_c67 _database_code_depnum_ccdc_archive 'CCDC 652529' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H40 N8 P2 Pt' _chemical_formula_sum 'C50 H40 N8 P2 Pt' _chemical_formula_weight 1009.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 8.45380(10) _cell_length_b 11.6212(2) _cell_length_c 11.9546(2) _cell_angle_alpha 69.5140(10) _cell_angle_beta 81.6740(10) _cell_angle_gamma 83.3340(10) _cell_volume 1085.88(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4806 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.78 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 3.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_T_max 0.771 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18352 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 29.57 _reflns_number_total 5974 _reflns_number_gt 5634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^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 calc _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5974 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0512 _refine_ls_wR_factor_gt 0.0476 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4343(2) 0.7686(2) 0.64493(18) 0.0266(4) Uani 1 1 d . . . C2 C 0.3569(2) 0.8248(2) 0.73382(19) 0.0283(5) Uani 1 1 d . . . C7 C 0.2753(3) 0.7524(3) 0.8406(2) 0.0368(5) Uani 1 1 d . . . H7 H 0.2703 0.6668 0.8563 0.044 Uiso 1 1 calc R . . C6 C 0.2016(3) 0.8053(3) 0.9238(2) 0.0405(6) Uani 1 1 d . . . H6 H 0.1459 0.7557 0.9964 0.049 Uiso 1 1 calc R . . C5 C 0.2082(3) 0.9285(3) 0.9023(2) 0.0412(6) Uani 1 1 d . . . H5 H 0.1567 0.9642 0.9597 0.049 Uiso 1 1 calc R . . C4 C 0.2894(3) 1.0004(3) 0.7976(2) 0.0388(6) Uani 1 1 d . . . H4 H 0.2951 1.0856 0.7834 0.047 Uiso 1 1 calc R . . C3 C 0.3632(3) 0.9495(2) 0.7123(2) 0.0334(5) Uani 1 1 d . . . H3 H 0.4178 0.9999 0.6395 0.040 Uiso 1 1 calc R . . C101 C 0.7497(2) 0.2554(2) 0.66209(18) 0.0287(5) Uani 1 1 d . . . C102 C 0.3098(3) 0.8522(3) 0.3327(2) 0.0399(6) Uani 1 1 d . . . H102 H 0.4219 0.8610 0.3156 0.048 Uiso 1 1 calc R . . C103 C 0.2082(3) 0.9477(3) 0.3520(3) 0.0513(7) Uani 1 1 d . . . H103 H 0.2504 1.0213 0.3488 0.062 Uiso 1 1 calc R . . C104 C 0.0449(3) 0.9348(3) 0.3760(3) 0.0525(8) Uani 1 1 d . . . H104 H -0.0255 1.0002 0.3884 0.063 Uiso 1 1 calc R . . C105 C -0.0155(3) 0.8292(3) 0.3821(3) 0.0511(8) Uani 1 1 d . . . H105 H -0.1277 0.8209 0.4000 0.061 Uiso 1 1 calc R . . C106 C 0.9152(3) 0.2665(3) 0.6377(2) 0.0401(6) Uani 1 1 d . . . H106 H 0.9587 0.3394 0.6347 0.048 Uiso 1 1 calc R . . C111 C 0.4572(2) 0.3128(2) 0.79577(18) 0.0274(5) Uani 1 1 d . . . C112 C 0.5029(3) 0.7852(2) 0.1027(2) 0.0340(5) Uani 1 1 d . . . H112 H 0.3947 0.8176 0.0974 0.041 Uiso 1 1 calc R . . C113 C 0.6193(3) 0.8355(3) 0.0096(2) 0.0383(6) Uani 1 1 d . . . H113 H 0.5910 0.9010 -0.0601 0.046 Uiso 1 1 calc R . . C114 C 0.7778(3) 0.7899(3) 0.0187(2) 0.0411(6) Uani 1 1 d . . . H114 H 0.8586 0.8254 -0.0442 0.049 Uiso 1 1 calc R . . C115 C 0.8187(3) 0.6926(3) 0.1194(2) 0.0424(6) Uani 1 1 d . . . H115 H 0.9272 0.6611 0.1247 0.051 Uiso 1 1 calc R . . C116 C 0.2978(3) 0.3587(2) 0.7880(2) 0.0345(5) Uani 1 1 d . . . H116 H 0.2692 0.4251 0.7191 0.041 Uiso 1 1 calc R . . C121 C 0.7181(3) 0.4739(2) 0.7325(2) 0.0304(5) Uani 1 1 d . . . C122 C 0.6840(3) 0.4762(3) 0.8499(2) 0.0394(6) Uani 1 1 d . . . H122 H 0.6016 0.4293 0.9029 0.047 Uiso 1 1 calc R . . C123 C 0.7696(4) 0.5461(3) 0.8892(3) 0.0522(7) Uani 1 1 d . . . H123 H 0.7455 0.5475 0.9689 0.063 Uiso 1 1 calc R . . C124 C 0.8897(4) 0.6139(3) 0.8132(3) 0.0530(8) Uani 1 1 d . . . H124 H 0.9494 0.6607 0.8412 0.064 Uiso 1 1 calc R . . C125 C 0.9239(3) 0.6143(3) 0.6969(3) 0.0487(7) Uani 1 1 d . . . H125 H 1.0071 0.6612 0.6449 0.058 Uiso 1 1 calc R . . C126 C 0.8365(3) 0.5462(3) 0.6557(2) 0.0388(6) Uani 1 1 d . . . H126 H 0.8577 0.5488 0.5746 0.047 Uiso 1 1 calc R . . N1 N 0.3933(2) 0.66322(19) 0.64120(16) 0.0286(4) Uani 1 1 d . . . N11 N 0.4928(2) 0.64836(18) 0.54860(16) 0.0273(4) Uani 1 1 d . . . N12 N 0.5886(2) 0.7390(2) 0.49902(17) 0.0334(4) Uani 1 1 d . . . N13 N 0.5530(2) 0.8173(2) 0.55954(17) 0.0336(4) Uani 1 1 d . . . P1 P 0.61008(6) 0.38295(6) 0.67621(5) 0.02548(12) Uani 1 1 d . . . Pt1 Pt 0.5000 0.5000 0.5000 0.02397(4) Uani 1 2 d S . . 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 0.0291(9) 0.0205(12) 0.0298(10) -0.0064(9) -0.0054(8) -0.0039(9) C2 0.0271(9) 0.0264(13) 0.0323(10) -0.0103(10) -0.0047(8) -0.0033(9) C7 0.0376(11) 0.0322(15) 0.0388(12) -0.0092(11) -0.0012(9) -0.0085(11) C6 0.0356(11) 0.0466(18) 0.0375(12) -0.0125(12) 0.0029(9) -0.0092(11) C5 0.0333(11) 0.053(2) 0.0442(13) -0.0274(13) -0.0031(10) 0.0025(12) C4 0.0424(12) 0.0306(15) 0.0486(14) -0.0202(12) -0.0078(10) 0.0011(11) C3 0.0376(11) 0.0280(14) 0.0355(11) -0.0116(10) -0.0026(9) -0.0049(10) C101 0.0271(9) 0.0304(14) 0.0276(10) -0.0087(9) -0.0050(8) 0.0014(9) C102 0.0305(11) 0.0369(16) 0.0553(15) -0.0197(13) -0.0075(10) 0.0011(11) C103 0.0486(15) 0.0415(19) 0.0719(19) -0.0301(16) -0.0138(13) 0.0081(13) C104 0.0447(14) 0.052(2) 0.0610(17) -0.0259(16) -0.0064(12) 0.0163(14) C105 0.0303(11) 0.058(2) 0.0560(16) -0.0122(15) -0.0009(11) 0.0065(13) C106 0.0290(10) 0.0410(17) 0.0450(13) -0.0081(12) -0.0032(9) -0.0038(11) C111 0.0283(9) 0.0268(13) 0.0286(10) -0.0104(9) -0.0018(8) -0.0059(9) C112 0.0334(11) 0.0338(15) 0.0330(11) -0.0076(10) -0.0063(9) -0.0042(10) C113 0.0480(13) 0.0345(16) 0.0296(11) -0.0066(10) -0.0017(9) -0.0080(11) C114 0.0442(13) 0.0422(18) 0.0354(12) -0.0139(12) 0.0111(10) -0.0140(12) C115 0.0321(11) 0.0447(18) 0.0471(14) -0.0146(13) 0.0038(10) -0.0027(11) C116 0.0308(10) 0.0314(15) 0.0368(11) -0.0071(10) -0.0015(9) -0.0024(10) C121 0.0307(10) 0.0267(14) 0.0347(11) -0.0092(10) -0.0073(8) -0.0055(9) C122 0.0461(13) 0.0379(17) 0.0373(12) -0.0146(11) -0.0022(10) -0.0121(12) C123 0.0739(19) 0.048(2) 0.0456(15) -0.0225(14) -0.0108(13) -0.0194(16) C124 0.0619(17) 0.046(2) 0.0632(18) -0.0246(16) -0.0185(14) -0.0199(15) C125 0.0423(13) 0.0462(19) 0.0582(16) -0.0131(14) -0.0062(12) -0.0196(13) C126 0.0393(12) 0.0397(17) 0.0392(12) -0.0122(12) -0.0049(10) -0.0124(11) N1 0.0294(8) 0.0253(11) 0.0307(9) -0.0093(8) -0.0013(7) -0.0041(8) N11 0.0280(8) 0.0217(11) 0.0319(9) -0.0080(8) -0.0046(7) -0.0029(8) N12 0.0365(9) 0.0262(12) 0.0379(10) -0.0114(9) 0.0032(8) -0.0109(8) N13 0.0368(9) 0.0271(12) 0.0385(10) -0.0127(9) 0.0011(8) -0.0099(9) P1 0.0236(2) 0.0256(3) 0.0272(2) -0.0081(2) -0.00294(19) -0.0044(2) Pt1 0.02398(6) 0.02146(8) 0.02685(6) -0.00803(5) -0.00275(4) -0.00373(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.327(3) . ? C1 N13 1.342(3) . ? C1 C2 1.473(3) . ? C2 C3 1.386(4) . ? C2 C7 1.393(3) . ? C7 C6 1.384(3) . ? C7 H7 0.9500 . ? C6 C5 1.370(4) . ? C6 H6 0.9500 . ? C5 C4 1.374(4) . ? C5 H5 0.9500 . ? C4 C3 1.390(3) . ? C4 H4 0.9500 . ? C3 H3 0.9500 . ? C101 C102 1.379(4) 2_666 ? C101 C106 1.399(3) . ? C101 P1 1.825(2) . ? C102 C101 1.379(4) 2_666 ? C102 C103 1.387(4) . ? C102 H102 0.9500 . ? C103 C104 1.384(4) . ? C103 H103 0.9500 . ? C104 C105 1.358(5) . ? C104 H104 0.9500 . ? C105 C106 1.385(4) 2_666 ? C105 H105 0.9500 . ? C106 C105 1.385(4) 2_666 ? C106 H106 0.9500 . ? C111 C116 1.395(3) . ? C111 C112 1.395(3) 2_666 ? C111 P1 1.809(2) . ? C112 C113 1.382(3) . ? C112 C111 1.395(3) 2_666 ? C112 H112 0.9500 . ? C113 C114 1.387(4) . ? C113 H113 0.9500 . ? C114 C115 1.387(4) . ? C114 H114 0.9500 . ? C115 C116 1.381(3) 2_666 ? C115 H115 0.9500 . ? C116 C115 1.381(3) 2_666 ? C116 H116 0.9500 . ? C121 C126 1.393(3) . ? C121 C122 1.400(3) . ? C121 P1 1.818(2) . ? C122 C123 1.381(4) . ? C122 H122 0.9500 . ? C123 C124 1.376(4) . ? C123 H123 0.9500 . ? C124 C125 1.377(4) . ? C124 H124 0.9500 . ? C125 C126 1.390(4) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? N1 N11 1.339(2) . ? N11 N12 1.318(3) . ? N11 Pt1 1.9951(19) . ? N12 N13 1.333(3) . ? P1 Pt1 2.3284(5) . ? Pt1 N11 1.9951(19) 2_666 ? Pt1 P1 2.3284(5) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N13 112.73(19) . . ? N1 C1 C2 123.1(2) . . ? N13 C1 C2 124.2(2) . . ? C3 C2 C7 119.4(2) . . ? C3 C2 C1 120.8(2) . . ? C7 C2 C1 119.9(2) . . ? C6 C7 C2 119.9(3) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C5 C6 C7 120.6(2) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C5 C4 119.9(2) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C4 C3 120.5(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C2 C3 C4 119.7(2) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C102 C101 C106 118.8(2) 2_666 . ? C102 C101 P1 119.23(16) 2_666 . ? C106 C101 P1 121.8(2) . . ? C101 C102 C103 121.0(2) 2_666 . ? C101 C102 H102 119.5 2_666 . ? C103 C102 H102 119.5 . . ? C104 C103 C102 119.3(3) . . ? C104 C103 H103 120.4 . . ? C102 C103 H103 120.4 . . ? C105 C104 C103 120.5(3) . . ? C105 C104 H104 119.8 . . ? C103 C104 H104 119.8 . . ? C104 C105 C106 120.7(3) . 2_666 ? C104 C105 H105 119.7 . . ? C106 C105 H105 119.7 2_666 . ? C105 C106 C101 119.8(3) 2_666 . ? C105 C106 H106 120.1 2_666 . ? C101 C106 H106 120.1 . . ? C116 C111 C112 119.3(2) . 2_666 ? C116 C111 P1 119.81(17) . . ? C112 C111 P1 120.86(16) 2_666 . ? C113 C112 C111 120.6(2) . 2_666 ? C113 C112 H112 119.7 . . ? C111 C112 H112 119.7 2_666 . ? C112 C113 C114 119.5(2) . . ? C112 C113 H113 120.2 . . ? C114 C113 H113 120.2 . . ? C113 C114 C115 120.3(2) . . ? C113 C114 H114 119.9 . . ? C115 C114 H114 119.9 . . ? C116 C115 C114 120.3(2) 2_666 . ? C116 C115 H115 119.9 2_666 . ? C114 C115 H115 119.9 . . ? C115 C116 C111 120.0(2) 2_666 . ? C115 C116 H116 120.0 2_666 . ? C111 C116 H116 120.0 . . ? C126 C121 C122 118.7(2) . . ? C126 C121 P1 119.03(17) . . ? C122 C121 P1 122.30(19) . . ? C123 C122 C121 120.4(3) . . ? C123 C122 H122 119.8 . . ? C121 C122 H122 119.8 . . ? C124 C123 C122 120.1(3) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C125 C124 C123 120.5(3) . . ? C125 C124 H124 119.8 . . ? C123 C124 H124 119.8 . . ? C124 C125 C126 119.9(3) . . ? C124 C125 H125 120.1 . . ? C126 C125 H125 120.1 . . ? C125 C126 C121 120.4(2) . . ? C125 C126 H126 119.8 . . ? C121 C126 H126 119.8 . . ? C1 N1 N11 102.47(18) . . ? N12 N11 N1 112.22(19) . . ? N12 N11 Pt1 124.94(14) . . ? N1 N11 Pt1 122.75(16) . . ? N11 N12 N13 107.36(18) . . ? N12 N13 C1 105.21(19) . . ? C111 P1 C121 106.32(10) . . ? C111 P1 C101 105.20(11) . . ? C121 P1 C101 106.36(10) . . ? C111 P1 Pt1 111.60(7) . . ? C121 P1 Pt1 112.61(8) . . ? C101 P1 Pt1 114.14(7) . . ? N11 Pt1 N11 180.0 . 2_666 ? N11 Pt1 P1 89.11(5) . . ? N11 Pt1 P1 90.89(5) 2_666 . ? N11 Pt1 P1 90.89(5) . 2_666 ? N11 Pt1 P1 89.11(5) 2_666 2_666 ? P1 Pt1 P1 180.000(1) . 2_666 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.852 _refine_diff_density_min -2.681 _refine_diff_density_rms 0.184 # Attachment '3e.cif' data_smc80 _database_code_depnum_ccdc_archive 'CCDC 652530' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H38 Cl2 N8 P2 Pt' _chemical_formula_sum 'C50 H38 Cl2 N8 P2 Pt' _chemical_formula_weight 1078.81 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8240(13) _cell_length_b 10.4480(13) _cell_length_c 12.0130(16) _cell_angle_alpha 66.379(6) _cell_angle_beta 83.021(7) _cell_angle_gamma 79.276(7) _cell_volume 1108.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8183 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 29.54 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 3.404 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.7271 _exptl_absorpt_correction_T_max 0.8482 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22011 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4052 _reflns_number_gt 4051 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'WinGX v.1.70.01 (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+0.2512P] 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 4052 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0155 _refine_ls_R_factor_gt 0.0155 _refine_ls_wR_factor_ref 0.0396 _refine_ls_wR_factor_gt 0.0396 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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 0.7336(2) 0.0836(2) 0.18807(19) 0.0207(4) Uani 1 1 d . . . C2 C 0.8096(2) 0.1779(2) 0.0835(2) 0.0249(5) Uani 1 1 d . . . C3 C 0.8771(3) 0.1318(3) -0.0043(2) 0.0307(5) Uani 1 1 d . . . H3 H 0.8694 0.0407 -0.0001 0.037 Uiso 1 1 calc R . . C4 C 0.9564(3) 0.2178(3) -0.0989(2) 0.0350(6) Uani 1 1 d . . . H4 H 1.0050 0.1849 -0.1581 0.042 Uiso 1 1 calc R . . C5 C 0.9636(3) 0.3494(3) -0.1058(2) 0.0325(6) Uani 1 1 d . . . C6 C 0.8906(3) 0.4017(3) -0.0236(2) 0.0362(6) Uani 1 1 d . . . H6 H 0.8926 0.4960 -0.0327 0.043 Uiso 1 1 calc R . . C7 C 0.8143(3) 0.3150(3) 0.0722(2) 0.0327(5) Uani 1 1 d . . . H7 H 0.7651 0.3490 0.1304 0.039 Uiso 1 1 calc R . . C101 C 0.4119(2) 0.3657(2) 0.35501(18) 0.0185(4) Uani 1 1 d . . . C102 C 0.5441(2) 0.3670(2) 0.38367(19) 0.0226(5) Uani 1 1 d . . . H102 H 0.6059 0.2809 0.4161 0.027 Uiso 1 1 calc R . . C103 C 0.5863(3) 0.4947(2) 0.3648(2) 0.0283(5) Uani 1 1 d . . . H103 H 0.6767 0.4954 0.3849 0.034 Uiso 1 1 calc R . . C104 C 0.4974(3) 0.6200(2) 0.3173(2) 0.0311(5) Uani 1 1 d . . . H104 H 0.5264 0.7067 0.3052 0.037 Uiso 1 1 calc R . . C105 C 0.3662(3) 0.6197(2) 0.2874(2) 0.0311(5) Uani 1 1 d . . . H105 H 0.3057 0.7063 0.2534 0.037 Uiso 1 1 calc R . . C106 C 0.3225(2) 0.4931(2) 0.3067(2) 0.0252(5) Uani 1 1 d . . . H106 H 0.2316 0.4932 0.2871 0.030 Uiso 1 1 calc R . . C111 C 0.1759(2) 0.2179(2) 0.42572(19) 0.0200(4) Uani 1 1 d . . . C112 C 0.1327(2) 0.2770(2) 0.5117(2) 0.0266(5) Uani 1 1 d . . . H112 H 0.1981 0.3097 0.5423 0.032 Uiso 1 1 calc R . . C113 C -0.0047(2) 0.2885(3) 0.5528(2) 0.0315(5) Uani 1 1 d . . . H113 H -0.0335 0.3300 0.6108 0.038 Uiso 1 1 calc R . . C114 C -0.1004(2) 0.2403(3) 0.5101(2) 0.0324(6) Uani 1 1 d . . . H114 H -0.1945 0.2469 0.5399 0.039 Uiso 1 1 calc R . . C115 C -0.0593(2) 0.1824(3) 0.4242(2) 0.0340(6) Uani 1 1 d . . . H115 H -0.1253 0.1500 0.3943 0.041 Uiso 1 1 calc R . . C116 C 0.0780(2) 0.1716(2) 0.3816(2) 0.0280(5) Uani 1 1 d . . . H116 H 0.1056 0.1324 0.3219 0.034 Uiso 1 1 calc R . . C121 C 0.3606(2) 0.1989(2) 0.22363(19) 0.0204(4) Uani 1 1 d . . . C122 C 0.3456(2) 0.0730(2) 0.2142(2) 0.0270(5) Uani 1 1 d . . . H122 H 0.3355 -0.0090 0.2857 0.032 Uiso 1 1 calc R . . C123 C 0.3454(3) 0.0681(3) 0.1007(2) 0.0366(6) Uani 1 1 d . . . H123 H 0.3341 -0.0171 0.0944 0.044 Uiso 1 1 calc R . . C124 C 0.3617(3) 0.1862(3) -0.0031(2) 0.0406(6) Uani 1 1 d . . . H124 H 0.3599 0.1826 -0.0807 0.049 Uiso 1 1 calc R . . C125 C 0.3804(3) 0.3094(3) 0.0052(2) 0.0392(6) Uani 1 1 d . . . H125 H 0.3938 0.3899 -0.0667 0.047 Uiso 1 1 calc R . . C126 C 0.3797(3) 0.3162(2) 0.1183(2) 0.0290(5) Uani 1 1 d . . . H126 H 0.3923 0.4016 0.1236 0.035 Uiso 1 1 calc R . . N1 N 0.67748(18) 0.11806(18) 0.28069(16) 0.0210(4) Uani 1 1 d . . . N11 N 0.62081(18) 0.00454(17) 0.35257(15) 0.0176(4) Uani 1 1 d . . . N12 N 0.6397(2) -0.09376(18) 0.30700(16) 0.0234(4) Uani 1 1 d . . . N13 N 0.7128(2) -0.04539(19) 0.20184(17) 0.0256(4) Uani 1 1 d . . . P1 P 0.35875(5) 0.20022(5) 0.37471(5) 0.01637(11) Uani 1 1 d . . . Cl1 Cl 1.06418(7) 0.45774(7) -0.22300(6) 0.04444(17) Uani 1 1 d . . . Pt1 Pt 0.5000 0.0000 0.5000 0.01429(5) Uani 1 2 d S . . 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 0.0171(11) 0.0262(10) 0.0202(11) -0.0105(9) 0.0001(9) -0.0041(8) C2 0.0220(12) 0.0293(11) 0.0213(11) -0.0073(9) 0.0018(9) -0.0063(9) C3 0.0335(14) 0.0328(12) 0.0257(12) -0.0121(10) 0.0062(10) -0.0077(10) C4 0.0349(14) 0.0421(14) 0.0233(12) -0.0108(11) 0.0078(10) -0.0052(11) C5 0.0246(13) 0.0376(13) 0.0259(12) -0.0010(10) 0.0009(10) -0.0100(10) C6 0.0356(15) 0.0317(13) 0.0371(14) -0.0082(11) 0.0042(11) -0.0108(11) C7 0.0327(14) 0.0319(12) 0.0318(13) -0.0123(10) 0.0086(11) -0.0077(10) C101 0.0226(11) 0.0210(10) 0.0141(10) -0.0087(8) 0.0032(8) -0.0071(8) C102 0.0215(11) 0.0268(11) 0.0235(11) -0.0133(9) 0.0027(9) -0.0078(9) C103 0.0272(13) 0.0369(12) 0.0292(12) -0.0187(10) 0.0078(10) -0.0172(10) C104 0.0456(15) 0.0281(12) 0.0256(12) -0.0144(10) 0.0116(11) -0.0193(11) C105 0.0409(15) 0.0219(11) 0.0282(12) -0.0089(10) 0.0031(11) -0.0044(10) C106 0.0284(12) 0.0229(10) 0.0241(11) -0.0083(9) -0.0029(9) -0.0043(9) C111 0.0168(11) 0.0204(10) 0.0201(10) -0.0046(8) -0.0012(8) -0.0036(8) C112 0.0217(12) 0.0344(12) 0.0236(11) -0.0115(10) -0.0015(9) -0.0035(9) C113 0.0244(13) 0.0438(14) 0.0240(12) -0.0135(11) 0.0017(10) -0.0006(10) C114 0.0179(12) 0.0396(13) 0.0310(13) -0.0059(11) 0.0024(10) -0.0044(10) C115 0.0217(13) 0.0371(13) 0.0435(15) -0.0123(11) -0.0035(11) -0.0113(10) C116 0.0255(13) 0.0284(11) 0.0336(13) -0.0143(10) -0.0024(10) -0.0067(9) C121 0.0183(11) 0.0257(10) 0.0197(10) -0.0115(9) -0.0024(8) -0.0020(8) C122 0.0287(13) 0.0285(11) 0.0270(12) -0.0130(10) -0.0034(10) -0.0053(9) C123 0.0412(15) 0.0413(14) 0.0398(15) -0.0278(12) -0.0082(12) -0.0043(11) C124 0.0519(17) 0.0517(16) 0.0254(13) -0.0238(12) -0.0091(12) 0.0006(13) C125 0.0557(18) 0.0388(14) 0.0196(12) -0.0102(10) -0.0002(11) -0.0029(12) C126 0.0376(14) 0.0282(11) 0.0221(12) -0.0111(9) -0.0010(10) -0.0041(10) N1 0.0202(9) 0.0235(9) 0.0207(9) -0.0094(7) 0.0047(7) -0.0082(7) N11 0.0169(9) 0.0197(8) 0.0180(9) -0.0091(7) 0.0003(7) -0.0041(7) N12 0.0290(10) 0.0227(9) 0.0215(9) -0.0120(8) 0.0039(8) -0.0063(7) N13 0.0308(11) 0.0269(9) 0.0212(9) -0.0124(8) 0.0060(8) -0.0069(8) P1 0.0163(3) 0.0176(2) 0.0163(3) -0.0071(2) -0.0007(2) -0.0040(2) Cl1 0.0394(4) 0.0500(4) 0.0310(3) 0.0000(3) 0.0082(3) -0.0188(3) Pt1 0.01460(7) 0.01591(6) 0.01362(6) -0.00660(4) 0.00116(4) -0.00455(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.330(3) . ? C1 N13 1.342(3) . ? C1 C2 1.469(3) . ? C2 C3 1.380(3) . ? C2 C7 1.393(3) . ? C3 C4 1.390(3) . ? C4 C5 1.359(4) . ? C5 C6 1.379(4) . ? C5 Cl1 1.743(2) . ? C6 C7 1.384(3) . ? C101 C102 1.387(3) . ? C101 C106 1.396(3) . ? C101 P1 1.815(2) . ? C102 C103 1.395(3) . ? C103 C104 1.378(4) . ? C104 C105 1.380(4) . ? C105 C106 1.388(3) . ? C111 C112 1.392(3) . ? C111 C116 1.394(3) . ? C111 P1 1.827(2) . ? C112 C113 1.380(3) . ? C113 C114 1.379(4) . ? C114 C115 1.379(4) . ? C115 C116 1.384(3) . ? C121 C126 1.387(3) . ? C121 C122 1.400(3) . ? C121 P1 1.818(2) . ? C122 C123 1.386(3) . ? C123 C124 1.376(4) . ? C124 C125 1.377(4) . ? C125 C126 1.388(3) . ? N1 N11 1.331(2) . ? N11 N12 1.321(2) . ? N11 Pt1 1.9976(17) . ? N12 N13 1.330(3) . ? P1 Pt1 2.3390(6) . ? Pt1 N11 1.9976(17) 2_656 ? Pt1 P1 2.3390(6) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N13 112.35(18) . . ? N1 C1 C2 122.93(19) . . ? N13 C1 C2 124.7(2) . . ? C3 C2 C7 119.2(2) . . ? C3 C2 C1 120.5(2) . . ? C7 C2 C1 120.2(2) . . ? C2 C3 C4 120.5(2) . . ? C5 C4 C3 119.2(2) . . ? C4 C5 C6 121.7(2) . . ? C4 C5 Cl1 119.7(2) . . ? C6 C5 Cl1 118.6(2) . . ? C5 C6 C7 119.1(2) . . ? C6 C7 C2 120.2(2) . . ? C102 C101 C106 119.40(19) . . ? C102 C101 P1 120.02(16) . . ? C106 C101 P1 120.54(17) . . ? C101 C102 C103 120.0(2) . . ? C104 C103 C102 120.3(2) . . ? C105 C104 C103 120.1(2) . . ? C104 C105 C106 120.2(2) . . ? C105 C106 C101 120.1(2) . . ? C112 C111 C116 118.8(2) . . ? C112 C111 P1 119.69(16) . . ? C116 C111 P1 121.46(17) . . ? C113 C112 C111 120.3(2) . . ? C112 C113 C114 120.5(2) . . ? C115 C114 C113 119.8(2) . . ? C114 C115 C116 120.1(2) . . ? C115 C116 C111 120.4(2) . . ? C126 C121 C122 119.1(2) . . ? C126 C121 P1 122.56(17) . . ? C122 C121 P1 118.28(16) . . ? C123 C122 C121 120.0(2) . . ? C124 C123 C122 120.3(2) . . ? C125 C124 C123 120.2(2) . . ? C124 C125 C126 120.2(2) . . ? C125 C126 C121 120.2(2) . . ? N11 N1 C1 102.67(17) . . ? N12 N11 N1 112.36(16) . . ? N12 N11 Pt1 125.08(14) . . ? N1 N11 Pt1 122.06(13) . . ? N11 N12 N13 107.19(17) . . ? N12 N13 C1 105.42(17) . . ? C101 P1 C121 106.77(10) . . ? C101 P1 C111 104.41(10) . . ? C121 P1 C111 105.42(10) . . ? C101 P1 Pt1 113.74(7) . . ? C121 P1 Pt1 110.32(7) . . ? C111 P1 Pt1 115.47(7) . . ? N11 Pt1 N11 180.0 . 2_656 ? N11 Pt1 P1 88.33(5) . . ? N11 Pt1 P1 91.67(5) 2_656 . ? N11 Pt1 P1 91.67(5) . 2_656 ? N11 Pt1 P1 88.33(5) 2_656 2_656 ? P1 Pt1 P1 180.0 . 2_656 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.516 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.069 # Attachment '5d.cif' data_sm-68 _database_code_depnum_ccdc_archive 'CCDC 652531' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 N10 Pt, C3 H7 N O' _chemical_formula_sum 'C27 H25 N11 O Pt' _chemical_formula_weight 714.67 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' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1290(7) _cell_length_b 7.4829(5) _cell_length_c 35.429(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.151(4) _cell_angle_gamma 90.00 _cell_volume 2669.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5936 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 24.09 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 5.300 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6193 _exptl_absorpt_correction_T_max 0.7080 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29536 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 30.44 _reflns_number_total 8022 _reflns_number_gt 5975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0877P)^2^+3.8245P] 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 8022 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1661 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.079 _refine_ls_shift/su_mean 0.001 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 0.4321(10) 0.6050(16) 0.1498(4) 0.086(3) Uani 1 1 d . . . H1A H 0.4160 0.5644 0.1752 0.128 Uiso 1 1 calc R . . H1B H 0.3769 0.5359 0.1307 0.128 Uiso 1 1 calc R . . H1C H 0.4097 0.7321 0.1471 0.128 Uiso 1 1 calc R . . C2 C 0.6594(12) 0.5162(16) 0.1760(3) 0.082(3) Uani 1 1 d . . . H2A H 0.6106 0.4888 0.1977 0.124 Uiso 1 1 calc R . . H2B H 0.7260 0.6085 0.1832 0.124 Uiso 1 1 calc R . . H2C H 0.7036 0.4079 0.1682 0.124 Uiso 1 1 calc R . . C3 C 0.6136(10) 0.6231(15) 0.1125(3) 0.068(2) Uani 1 1 d . . . C205 C 0.5908(9) 0.9706(13) 0.2107(2) 0.061(2) Uani 1 1 d . . . H205 H 0.6450 0.9186 0.2314 0.073 Uiso 1 1 calc R . . N1 N 0.5679(7) 0.5800(10) 0.1448(2) 0.0553(16) Uani 1 1 d . . . O1 O 0.5425(10) 0.6812(13) 0.0852(2) 0.095(3) Uani 1 1 d . . . H3 H 0.723(13) 0.681(17) 0.120(4) 0.114 Uiso 1 1 d . . . C11 C 0.9653(7) 1.2025(9) -0.0264(2) 0.0384(14) Uani 1 1 d . . . C12 C 0.9419(8) 1.1531(11) -0.0642(2) 0.0483(17) Uani 1 1 d . . . H12 H 1.0107 1.1609 -0.0804 0.058 Uiso 1 1 calc R . . C13 C 0.8180(8) 1.0924(11) -0.0781(2) 0.054(2) Uani 1 1 d . . . H13 H 0.7997 1.0585 -0.1040 0.065 Uiso 1 1 calc R . . C14 C 0.7226(8) 1.0820(11) -0.0542(2) 0.0519(19) Uani 1 1 d . . . H14 H 0.6367 1.0402 -0.0636 0.062 Uiso 1 1 calc R . . C15 C 0.7470(7) 1.1305(10) -0.0168(2) 0.0465(17) Uani 1 1 d . . . H15 H 0.6783 1.1219 -0.0006 0.056 Uiso 1 1 calc R . . C21 C 1.0927(7) 1.2745(9) -0.0088(2) 0.0387(15) Uani 1 1 d . . . C22 C 1.2064(9) 1.2934(12) -0.0270(3) 0.0528(19) Uani 1 1 d . . . H22 H 1.2062 1.2585 -0.0528 0.063 Uiso 1 1 calc R . . C23 C 1.3190(7) 1.3627(13) -0.0075(3) 0.058(2) Uani 1 1 d . . . H23 H 1.3977 1.3747 -0.0196 0.069 Uiso 1 1 calc R . . C24 C 1.3177(7) 1.4147(11) 0.0296(2) 0.0497(18) Uani 1 1 d . . . H24 H 1.3943 1.4656 0.0433 0.060 Uiso 1 1 calc R . . C25 C 1.2032(7) 1.3914(10) 0.0465(2) 0.0435(16) Uani 1 1 d . . . H25 H 1.2030 1.4249 0.0723 0.052 Uiso 1 1 calc R . . C100 C 1.0499(6) 1.5113(10) 0.15068(18) 0.0373(14) Uani 1 1 d . . . C101 C 1.0618(7) 1.6602(11) 0.1781(2) 0.0399(15) Uani 1 1 d . . . C102 C 1.1389(8) 1.6366(13) 0.2125(2) 0.055(2) Uani 1 1 d . . . H102 H 1.1828 1.5262 0.2182 0.066 Uiso 1 1 calc R . . C103 C 1.1513(11) 1.7768(14) 0.2385(3) 0.066(3) Uani 1 1 d . . . H103 H 1.2038 1.7606 0.2621 0.079 Uiso 1 1 calc R . . C104 C 1.0901(9) 1.9361(14) 0.2309(3) 0.062(2) Uani 1 1 d . . . H104 H 1.0992 2.0300 0.2490 0.075 Uiso 1 1 calc R . . C105 C 1.0145(8) 1.9599(13) 0.1965(2) 0.058(2) Uani 1 1 d . . . H105 H 0.9722 2.0717 0.1911 0.069 Uiso 1 1 calc R . . C106 C 0.9986(8) 1.8256(13) 0.1696(2) 0.0529(19) Uani 1 1 d . . . H106 H 0.9464 1.8442 0.1460 0.063 Uiso 1 1 calc R . . C200 C 0.6236(7) 1.1379(10) 0.1122(2) 0.0403(15) Uani 1 1 d . . . C201 C 0.5665(7) 1.0859(10) 0.1472(2) 0.0424(16) Uani 1 1 d . . . C202 C 0.4336(7) 1.1198(11) 0.1510(2) 0.0490(18) Uani 1 1 d . . . H202 H 0.3784 1.1691 0.1303 0.059 Uiso 1 1 calc R . . C203 C 0.3802(9) 1.0835(14) 0.1843(3) 0.063(2) Uani 1 1 d . . . H203 H 0.2899 1.1104 0.1867 0.076 Uiso 1 1 calc R . . C204 C 0.4595(11) 1.0076(15) 0.2142(3) 0.073(3) Uani 1 1 d . . . H204 H 0.4234 0.9808 0.2372 0.087 Uiso 1 1 calc R . . C206 C 0.6442(8) 1.0088(12) 0.1771(2) 0.0514(19) Uani 1 1 d . . . H206 H 0.7346 0.9818 0.1748 0.062 Uiso 1 1 calc R . . N10 N 0.9952(5) 1.3544(8) 0.10291(15) 0.0359(12) Uani 1 1 d . . . N11 N 0.8675(5) 1.1899(8) -0.00292(16) 0.0369(12) Uani 1 1 d . . . N12 N 1.0917(5) 1.3237(8) 0.02834(16) 0.0344(11) Uani 1 1 d . . . N20 N 1.0811(8) 1.2598(9) 0.1254(2) 0.0567(19) Uani 1 1 d . . . N30 N 1.1164(7) 1.3591(10) 0.15560(17) 0.0530(17) Uani 1 1 d . . . N40 N 0.7552(6) 1.2077(8) 0.07328(18) 0.0411(13) Uani 1 1 d . . . N50 N 0.6345(7) 1.2416(9) 0.0568(2) 0.0553(19) Uani 1 1 d . . . N60 N 0.5484(6) 1.1974(10) 0.0808(2) 0.0515(16) Uani 1 1 d . . . N100 N 0.9714(5) 1.5129(8) 0.11727(15) 0.0389(12) Uani 1 1 d . . . N200 N 0.7516(6) 1.1425(9) 0.10850(17) 0.0438(14) Uani 1 1 d . . . Pt1 Pt 0.92320(2) 1.26977(4) 0.051241(7) 0.03599(11) 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 0.065(6) 0.073(7) 0.122(10) -0.004(7) 0.027(7) -0.005(5) C2 0.105(9) 0.078(7) 0.058(6) -0.004(5) -0.023(6) 0.008(6) C3 0.059(6) 0.078(7) 0.065(6) -0.005(5) -0.004(5) 0.009(5) C205 0.064(6) 0.075(6) 0.041(4) 0.001(4) -0.002(4) -0.010(5) N1 0.053(4) 0.059(4) 0.052(4) -0.004(3) -0.003(3) 0.001(3) O1 0.124(7) 0.101(6) 0.055(4) -0.001(4) -0.007(5) 0.027(6) C11 0.039(3) 0.039(4) 0.036(3) 0.004(3) -0.005(3) 0.002(3) C12 0.054(4) 0.050(4) 0.039(4) -0.002(3) -0.004(3) 0.005(4) C13 0.059(5) 0.056(5) 0.043(4) -0.007(3) -0.017(4) 0.004(4) C14 0.048(4) 0.058(5) 0.044(4) -0.007(3) -0.020(3) 0.003(4) C15 0.040(4) 0.049(4) 0.048(4) -0.001(3) -0.008(3) -0.004(3) C21 0.034(3) 0.037(3) 0.044(4) 0.002(3) -0.001(3) 0.001(3) C22 0.049(4) 0.061(5) 0.049(5) 0.008(4) 0.009(4) -0.002(4) C23 0.031(4) 0.075(6) 0.068(6) 0.014(5) 0.008(4) -0.005(4) C24 0.037(4) 0.062(5) 0.046(4) 0.017(4) -0.011(3) -0.005(3) C25 0.038(3) 0.053(4) 0.036(4) 0.010(3) -0.014(3) -0.004(3) C100 0.032(3) 0.053(4) 0.027(3) 0.001(3) 0.000(3) -0.002(3) C101 0.033(3) 0.052(4) 0.034(3) 0.002(3) 0.003(3) 0.001(3) C102 0.053(5) 0.073(6) 0.037(4) -0.001(4) -0.011(3) -0.002(4) C103 0.063(6) 0.092(8) 0.039(4) -0.014(4) -0.010(4) -0.014(5) C104 0.061(5) 0.069(6) 0.056(5) -0.028(4) 0.004(4) -0.016(4) C105 0.050(5) 0.065(6) 0.057(5) -0.010(4) 0.003(4) 0.006(4) C106 0.041(4) 0.066(5) 0.050(5) -0.005(4) -0.001(3) 0.000(4) C200 0.032(3) 0.044(4) 0.043(4) -0.001(3) -0.002(3) -0.002(3) C201 0.033(3) 0.038(4) 0.056(4) -0.004(3) 0.002(3) -0.006(3) C202 0.036(4) 0.056(5) 0.054(5) 0.001(4) 0.002(3) 0.001(3) C203 0.044(4) 0.089(7) 0.060(5) 0.005(5) 0.016(4) 0.004(4) C204 0.073(6) 0.097(8) 0.049(5) 0.002(5) 0.017(5) -0.012(6) C206 0.039(4) 0.060(5) 0.055(5) 0.003(4) 0.001(4) 0.002(3) N10 0.027(2) 0.051(3) 0.028(3) 0.003(2) -0.008(2) 0.000(2) N11 0.032(3) 0.039(3) 0.037(3) 0.003(2) -0.009(2) -0.001(2) N12 0.028(2) 0.037(3) 0.036(3) 0.006(2) -0.008(2) -0.004(2) N20 0.062(5) 0.058(4) 0.044(4) -0.003(3) -0.021(3) 0.016(3) N30 0.058(4) 0.066(5) 0.030(3) -0.006(3) -0.018(3) 0.016(3) N40 0.029(3) 0.049(3) 0.044(3) 0.003(3) -0.003(2) 0.000(2) N50 0.029(3) 0.086(6) 0.049(4) 0.012(3) -0.004(3) 0.000(3) N60 0.035(3) 0.068(4) 0.049(4) 0.010(3) -0.004(3) -0.001(3) N100 0.031(3) 0.052(4) 0.031(3) 0.002(2) -0.010(2) 0.002(2) N200 0.035(3) 0.056(4) 0.040(3) 0.006(3) -0.001(2) -0.001(3) Pt1 0.02894(14) 0.04134(17) 0.03592(15) 0.00245(10) -0.00478(10) -0.00103(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.417(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.444(12) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 O1 1.223(12) . ? C3 N1 1.321(12) . ? C3 H3 1.19(13) . ? C205 C204 1.376(13) . ? C205 C206 1.388(11) . ? C205 H205 0.9500 . ? C11 N11 1.363(9) . ? C11 C12 1.386(10) . ? C11 C21 1.474(10) . ? C12 C13 1.375(11) . ? C12 H12 0.9500 . ? C13 C14 1.353(12) . ? C13 H13 0.9500 . ? C14 C15 1.372(10) . ? C14 H14 0.9500 . ? C15 N11 1.342(9) . ? C15 H15 0.9500 . ? C21 N12 1.367(9) . ? C21 C22 1.386(11) . ? C22 C23 1.371(12) . ? C22 H22 0.9500 . ? C23 C24 1.373(12) . ? C23 H23 0.9500 . ? C24 C25 1.372(10) . ? C24 H24 0.9500 . ? C25 N12 1.337(8) . ? C25 H25 0.9500 . ? C100 N30 1.325(9) . ? C100 N100 1.354(8) . ? C100 C101 1.474(10) . ? C101 C102 1.387(11) . ? C101 C106 1.411(12) . ? C102 C103 1.393(13) . ? C102 H102 0.9500 . ? C103 C104 1.357(14) . ? C103 H103 0.9500 . ? C104 C105 1.379(12) . ? C104 H104 0.9500 . ? C105 C106 1.382(12) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C200 N200 1.317(8) . ? C200 N60 1.353(9) . ? C200 C201 1.476(10) . ? C201 C206 1.377(11) . ? C201 C202 1.392(10) . ? C202 C203 1.375(11) . ? C202 H202 0.9500 . ? C203 C204 1.380(13) . ? C203 H203 0.9500 . ? C204 H204 0.9500 . ? C206 H206 0.9500 . ? N10 N20 1.320(8) . ? N10 N100 1.323(8) . ? N10 Pt1 1.999(5) . ? N11 Pt1 2.031(6) . ? N12 Pt1 2.008(5) . ? N20 N30 1.321(9) . ? N40 N50 1.323(9) . ? N40 N200 1.344(8) . ? N40 Pt1 2.001(6) . ? N50 N60 1.326(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 N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C3 N1 122.8(10) . . ? O1 C3 H3 120(6) . . ? N1 C3 H3 107(6) . . ? C204 C205 C206 120.2(9) . . ? C204 C205 H205 119.9 . . ? C206 C205 H205 119.9 . . ? C3 N1 C1 120.8(9) . . ? C3 N1 C2 119.1(9) . . ? C1 N1 C2 120.0(9) . . ? N11 C11 C12 120.8(7) . . ? N11 C11 C21 115.3(6) . . ? C12 C11 C21 123.9(7) . . ? C13 C12 C11 119.3(8) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 118.7(8) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 121.5(7) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? N11 C15 C14 120.3(7) . . ? N11 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? N12 C21 C22 120.8(7) . . ? N12 C21 C11 114.2(6) . . ? C22 C21 C11 125.0(7) . . ? C23 C22 C21 119.5(8) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 119.8(7) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 118.5(7) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? N12 C25 C24 123.2(7) . . ? N12 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? N30 C100 N100 111.4(6) . . ? N30 C100 C101 124.0(6) . . ? N100 C100 C101 124.6(7) . . ? C102 C101 C106 119.9(8) . . ? C102 C101 C100 118.7(7) . . ? C106 C101 C100 121.3(7) . . ? C101 C102 C103 119.2(9) . . ? C101 C102 H102 120.4 . . ? C103 C102 H102 120.4 . . ? C104 C103 C102 121.6(9) . . ? C104 C103 H103 119.2 . . ? C102 C103 H103 119.2 . . ? C103 C104 C105 119.2(8) . . ? C103 C104 H104 120.4 . . ? C105 C104 H104 120.4 . . ? C104 C105 C106 121.8(9) . . ? C104 C105 H105 119.1 . . ? C106 C105 H105 119.1 . . ? C105 C106 C101 118.3(8) . . ? C105 C106 H106 120.8 . . ? C101 C106 H106 120.8 . . ? N200 C200 N60 112.6(6) . . ? N200 C200 C201 124.6(6) . . ? N60 C200 C201 122.7(6) . . ? C206 C201 C202 118.7(7) . . ? C206 C201 C200 121.0(6) . . ? C202 C201 C200 120.3(7) . . ? C203 C202 C201 121.4(8) . . ? C203 C202 H202 119.3 . . ? C201 C202 H202 119.3 . . ? C202 C203 C204 119.2(8) . . ? C202 C203 H203 120.4 . . ? C204 C203 H203 120.4 . . ? C205 C204 C203 120.2(8) . . ? C205 C204 H204 119.9 . . ? C203 C204 H204 119.9 . . ? C201 C206 C205 120.2(8) . . ? C201 C206 H206 119.9 . . ? C205 C206 H206 119.9 . . ? N20 N10 N100 112.6(5) . . ? N20 N10 Pt1 122.3(5) . . ? N100 N10 Pt1 124.9(4) . . ? C15 N11 C11 119.4(6) . . ? C15 N11 Pt1 126.4(5) . . ? C11 N11 Pt1 114.2(4) . . ? C25 N12 C21 118.2(6) . . ? C25 N12 Pt1 126.3(5) . . ? C21 N12 Pt1 115.4(4) . . ? N10 N20 N30 106.9(6) . . ? N20 N30 C100 106.7(6) . . ? N50 N40 N200 111.4(6) . . ? N50 N40 Pt1 124.6(5) . . ? N200 N40 Pt1 123.8(5) . . ? N40 N50 N60 108.0(6) . . ? N50 N60 C200 105.0(6) . . ? N10 N100 C100 102.4(5) . . ? C200 N200 N40 103.1(6) . . ? N10 Pt1 N40 87.6(2) . . ? N10 Pt1 N12 93.6(2) . . ? N40 Pt1 N12 178.1(2) . . ? N10 Pt1 N11 174.4(2) . . ? N40 Pt1 N11 98.0(2) . . ? N12 Pt1 N11 80.8(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.44 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 3.483 _refine_diff_density_min -3.897 _refine_diff_density_rms 0.223