data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wai-Yeung (Raymond) Wong.' _publ_contact_author_email RWYWONG@HKBU.EDU.HK _publ_section_title ; A versatile color tuning strategy for iridium(III) and platinum(II) electrophosphors by shifting the charge-transfer states with an electron-deficient core ; loop_ _publ_author_name 'Wai-Yeung Wong.' 'Zhenyang Lin.' 'Dongge Ma.' 'Qi Wang.' 'Lixiang Wang.' ; Gui-Jiang Zhou ; data_wy1174wc _database_code_depnum_ccdc_archive 'CCDC 639790' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H37 Cl3 N2 O2 Pt' _chemical_formula_weight 879.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 24.1106(15) _cell_length_b 13.6691(9) _cell_length_c 13.1241(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.2780(10) _cell_angle_gamma 90.00 _cell_volume 4325.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 3.461 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.5735 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20919 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7563 _reflns_number_gt 5598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Burker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+3.3587P] 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 7563 _refine_ls_number_parameters 469 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1322 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5273(2) 0.4510(4) 0.8971(3) 0.0566(13) Uani 1 1 d . . . H1A H 0.5318 0.3911 0.9298 0.068 Uiso 1 1 calc R . . C2 C 0.5657(2) 0.5210(4) 0.9119(4) 0.0600(14) Uani 1 1 d . . . H2A H 0.5964 0.5092 0.9533 0.072 Uiso 1 1 calc R . . C3 C 0.5589(2) 0.6123(4) 0.8638(4) 0.0609(15) Uani 1 1 d . . . H3A H 0.5848 0.6621 0.8731 0.073 Uiso 1 1 calc R . . C4 C 0.5129(2) 0.6260(3) 0.8024(4) 0.0536(13) Uani 1 1 d . . . H4A H 0.5072 0.6860 0.7707 0.064 Uiso 1 1 calc R . . C5 C 0.47515(18) 0.5504(3) 0.7879(3) 0.0443(11) Uani 1 1 d . . . C6 C 0.42575(18) 0.5522(3) 0.7222(3) 0.0456(11) Uani 1 1 d . . . C7 C 0.39411(19) 0.4658(3) 0.7246(3) 0.0481(12) Uani 1 1 d . . . C8 C 0.3464(2) 0.4596(4) 0.6642(3) 0.0541(13) Uani 1 1 d . . . H8A H 0.3248 0.4032 0.6646 0.065 Uiso 1 1 calc R . . C9 C 0.33129(19) 0.5396(4) 0.6031(3) 0.0529(13) Uani 1 1 d . . . C10 C 0.2830(2) 0.5535(4) 0.5362(4) 0.0587(14) Uani 1 1 d . . . C11 C 0.2390(2) 0.4911(5) 0.5149(4) 0.0779(17) Uani 1 1 d . . . H11A H 0.2372 0.4291 0.5440 0.094 Uiso 1 1 calc R . . C12 C 0.1980(2) 0.5238(5) 0.4491(4) 0.0802(18) Uani 1 1 d . . . H12A H 0.1677 0.4838 0.4354 0.096 Uiso 1 1 calc R . . C13 C 0.2012(2) 0.6172(4) 0.4021(4) 0.0672(16) Uani 1 1 d . . . C14 C 0.2458(2) 0.6762(4) 0.4240(3) 0.0581(14) Uani 1 1 d . . . H14A H 0.2484 0.7378 0.3943 0.070 Uiso 1 1 calc R . . C15 C 0.2871(2) 0.6444(4) 0.4900(4) 0.0543(13) Uani 1 1 d . . . C16 C 0.33909(18) 0.6995(3) 0.5252(3) 0.0482(12) Uani 1 1 d . . . C17 C 0.36411(19) 0.6241(3) 0.5983(3) 0.0472(12) Uani 1 1 d . . . C18 C 0.41146(19) 0.6318(3) 0.6587(3) 0.0466(12) Uani 1 1 d . . . H18A H 0.4332 0.6880 0.6573 0.056 Uiso 1 1 calc R . . C19 C 0.3780(2) 0.7225(4) 0.4371(4) 0.0588(14) Uani 1 1 d . . . H19A H 0.3609 0.7730 0.3955 0.071 Uiso 1 1 calc R . . H19B H 0.4120 0.7494 0.4651 0.071 Uiso 1 1 calc R . . C20 C 0.3930(3) 0.6376(4) 0.3684(4) 0.0736(18) Uani 1 1 d . . . H20A H 0.4172 0.6601 0.3155 0.110 Uiso 1 1 calc R . . H20B H 0.3598 0.6110 0.3384 0.110 Uiso 1 1 calc R . . H20C H 0.4114 0.5879 0.4077 0.110 Uiso 1 1 calc R . . C21 C 0.3242(2) 0.7944(4) 0.5808(4) 0.0676(16) Uani 1 1 d . . . H21A H 0.3581 0.8228 0.6079 0.081 Uiso 1 1 calc R . . H21B H 0.3091 0.8401 0.5315 0.081 Uiso 1 1 calc R . . C22 C 0.2836(3) 0.7841(5) 0.6664(5) 0.095(2) Uani 1 1 d . . . H22A H 0.2770 0.8469 0.6966 0.143 Uiso 1 1 calc R . . H22B H 0.2984 0.7403 0.7169 0.143 Uiso 1 1 calc R . . H22C H 0.2493 0.7583 0.6403 0.143 Uiso 1 1 calc R . . C23 C 0.1411(2) 0.7431(5) 0.3378(5) 0.089(2) Uani 1 1 d . . . C24 C 0.1297(3) 0.7902(8) 0.4337(7) 0.141(4) Uani 1 1 d . . . H24A H 0.1341 0.7585 0.4959 0.170 Uiso 1 1 calc R . . C25 C 0.1111(4) 0.8898(8) 0.4263(10) 0.209(5) Uani 1 1 d . . . H25A H 0.1022 0.9235 0.4855 0.251 Uiso 1 1 calc R . . C26 C 0.1057(4) 0.9410(12) 0.3251(16) 0.327(10) Uani 1 1 d . . . H26A H 0.0935 1.0053 0.3197 0.393 Uiso 1 1 calc R . . C27 C 0.1181(5) 0.8941(8) 0.2535(11) 0.183(5) Uani 1 1 d . . . H27A H 0.1182 0.9270 0.1914 0.219 Uiso 1 1 calc R . . C28 C 0.1325(3) 0.7950(7) 0.2501(6) 0.122(3) Uani 1 1 d . . . H28A H 0.1364 0.7641 0.1874 0.147 Uiso 1 1 calc R . . C29 C 0.1297(2) 0.5797(5) 0.2754(5) 0.083(2) Uani 1 1 d . . . C30 C 0.0737(3) 0.5829(7) 0.2655(6) 0.115(3) Uani 1 1 d . . . H30A H 0.0543 0.6323 0.2986 0.138 Uiso 1 1 calc R . . C31 C 0.0434(3) 0.5134(7) 0.2063(7) 0.140(4) Uani 1 1 d . . . H31A H 0.0049 0.5154 0.2025 0.168 Uiso 1 1 calc R . . C32 C 0.0724(4) 0.4447(8) 0.1560(7) 0.152(4) Uani 1 1 d . . . H32A H 0.0533 0.4016 0.1138 0.182 Uiso 1 1 calc R . . C33 C 0.1286(4) 0.4354(7) 0.1642(6) 0.137(3) Uani 1 1 d . . . H33A H 0.1478 0.3848 0.1328 0.165 Uiso 1 1 calc R . . C34 C 0.1564(3) 0.5087(6) 0.2244(5) 0.107(3) Uani 1 1 d . . . H34A H 0.1949 0.5067 0.2283 0.128 Uiso 1 1 calc R . . C35 C 0.4688(3) 0.1254(4) 1.0201(5) 0.0759(18) Uani 1 1 d . . . H35A H 0.5015 0.1610 1.0397 0.114 Uiso 1 1 calc R . . H35B H 0.4793 0.0636 0.9914 0.114 Uiso 1 1 calc R . . H35C H 0.4461 0.1146 1.0790 0.114 Uiso 1 1 calc R . . C36 C 0.4363(2) 0.1842(4) 0.9414(4) 0.0570(13) Uani 1 1 d . . . C37 C 0.3863(3) 0.1481(4) 0.9035(5) 0.0704(17) Uani 1 1 d . . . H37A H 0.3732 0.0908 0.9330 0.084 Uiso 1 1 calc R . . C38 C 0.3542(2) 0.1879(4) 0.8273(4) 0.0640(15) Uani 1 1 d . . . C39 C 0.3046(3) 0.1306(5) 0.7878(6) 0.098(2) Uani 1 1 d . . . H39A H 0.2861 0.1676 0.7356 0.147 Uiso 1 1 calc R . . H39B H 0.2794 0.1184 0.8427 0.147 Uiso 1 1 calc R . . H39C H 0.3170 0.0694 0.7600 0.147 Uiso 1 1 calc R . . C40 C 0.2684(4) 0.4124(7) 0.8829(7) 0.098(4) Uani 0.50 1 d PD . . H40A H 0.3027 0.4013 0.8449 0.118 Uiso 0.50 1 calc PR . . C41 C 0.0555(5) 0.3417(10) 0.4426(11) 0.311(15) Uani 0.50 1 d PD . . H41 H 0.0548 0.3967 0.3948 0.373 Uiso 0.50 1 calc PR . . Cl1 Cl 0.21449(17) 0.3598(3) 0.8147(4) 0.1370(18) Uani 0.50 1 d PD . . Cl2 Cl 0.2569(2) 0.5337(3) 0.8866(5) 0.218(3) Uani 0.50 1 d PD . . Cl3 Cl 0.2752(3) 0.3548(7) 0.9999(4) 0.273(6) Uani 0.50 1 d PD . . Cl4 Cl 0.0704(4) 0.3786(8) 0.5646(7) 0.383(6) Uani 0.50 1 d PD . . Cl5 Cl -0.0048(3) 0.2746(9) 0.4382(9) 0.347(7) Uani 0.50 1 d PD . . Cl6 Cl 0.1069(4) 0.2612(6) 0.4155(8) 0.355(5) Uani 0.50 1 d PD . . N1 N 0.48203(15) 0.4642(3) 0.8364(3) 0.0478(10) Uani 1 1 d . . . N2 N 0.1587(2) 0.6476(4) 0.3353(4) 0.0761(15) Uani 1 1 d . . . O1 O 0.45984(14) 0.2643(2) 0.9164(2) 0.0574(9) Uani 1 1 d . . . O2 O 0.36064(14) 0.2707(2) 0.7837(3) 0.0632(10) Uani 1 1 d . . . Pt1 Pt 0.423562(8) 0.363370(13) 0.815397(13) 0.04793(5) 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 0.063(3) 0.053(3) 0.054(3) 0.003(2) -0.004(2) 0.007(2) C2 0.060(3) 0.057(3) 0.063(3) -0.006(2) -0.012(2) 0.008(3) C3 0.056(3) 0.062(3) 0.065(3) 0.000(2) -0.010(2) -0.003(2) C4 0.063(3) 0.045(3) 0.053(3) 0.005(2) -0.004(2) -0.005(2) C5 0.053(2) 0.040(2) 0.040(2) 0.0026(19) 0.0000(19) 0.003(2) C6 0.048(2) 0.049(2) 0.040(2) 0.0025(19) -0.0038(19) 0.003(2) C7 0.059(3) 0.046(2) 0.040(2) 0.0000(19) 0.004(2) 0.007(2) C8 0.061(3) 0.052(3) 0.050(2) 0.008(2) -0.004(2) -0.013(2) C9 0.056(3) 0.054(3) 0.049(2) 0.008(2) -0.010(2) -0.006(2) C10 0.059(3) 0.064(3) 0.054(3) 0.005(2) -0.011(2) -0.009(3) C11 0.071(3) 0.085(4) 0.077(3) 0.027(3) -0.019(3) -0.027(3) C12 0.067(3) 0.097(4) 0.076(3) 0.013(3) -0.021(3) -0.021(3) C13 0.056(3) 0.085(4) 0.060(3) 0.004(3) -0.013(2) -0.005(3) C14 0.066(3) 0.061(3) 0.047(2) 0.004(2) -0.010(2) 0.004(3) C15 0.058(3) 0.060(3) 0.045(2) 0.006(2) -0.004(2) 0.007(2) C16 0.053(2) 0.046(3) 0.046(2) 0.001(2) -0.011(2) 0.000(2) C17 0.051(2) 0.049(3) 0.041(2) 0.0026(19) -0.0061(19) 0.002(2) C18 0.050(2) 0.044(2) 0.046(2) 0.002(2) -0.002(2) -0.004(2) C19 0.067(3) 0.054(3) 0.055(3) 0.014(2) -0.011(2) -0.008(3) C20 0.078(4) 0.077(4) 0.066(3) -0.002(3) 0.001(3) -0.005(3) C21 0.076(3) 0.057(3) 0.070(3) -0.002(3) -0.019(3) 0.016(3) C22 0.087(4) 0.112(5) 0.086(4) -0.020(4) 0.002(3) 0.023(4) C23 0.048(3) 0.114(5) 0.105(5) -0.014(4) -0.020(3) 0.009(3) C24 0.078(4) 0.208(9) 0.137(6) -0.072(6) -0.018(4) 0.012(6) C25 0.095(6) 0.187(7) 0.344(12) -0.187(7) -0.019(7) 0.035(6) C26 0.136(6) 0.239(14) 0.60(3) -0.125(15) -0.190(11) 0.111(8) C27 0.157(9) 0.133(8) 0.257(12) 0.067(8) -0.068(9) 0.025(7) C28 0.126(6) 0.127(7) 0.115(5) 0.030(5) -0.035(5) 0.028(5) C29 0.059(3) 0.104(5) 0.085(4) 0.005(4) -0.026(3) -0.001(3) C30 0.071(4) 0.137(7) 0.137(6) -0.003(6) -0.019(4) -0.012(5) C31 0.089(5) 0.166(9) 0.165(8) 0.014(7) -0.046(5) -0.032(6) C32 0.144(7) 0.163(9) 0.147(7) -0.001(6) -0.066(6) -0.062(6) C33 0.159(7) 0.140(7) 0.113(6) -0.029(5) -0.031(6) -0.037(6) C34 0.108(5) 0.118(6) 0.094(5) 0.004(4) -0.027(4) -0.022(5) C35 0.087(4) 0.062(3) 0.080(4) 0.025(3) 0.003(3) 0.014(3) C36 0.068(3) 0.050(3) 0.053(3) 0.007(2) 0.004(2) 0.012(3) C37 0.080(4) 0.052(3) 0.079(4) 0.018(3) -0.003(3) -0.008(3) C38 0.068(3) 0.054(3) 0.070(3) 0.009(3) -0.004(3) -0.013(3) C39 0.101(5) 0.080(4) 0.113(5) 0.014(4) -0.021(4) -0.036(4) C40 0.051(6) 0.136(10) 0.107(8) -0.069(8) 0.024(6) -0.020(7) C41 0.41(3) 0.085(13) 0.44(4) 0.007(17) 0.27(3) -0.083(17) Cl1 0.084(2) 0.110(3) 0.217(5) -0.063(3) -0.025(3) -0.004(2) Cl2 0.104(3) 0.134(3) 0.417(7) -0.173(4) -0.016(4) 0.004(3) Cl3 0.210(6) 0.534(17) 0.076(3) 0.032(5) 0.042(4) 0.047(8) Cl4 0.359(10) 0.491(15) 0.300(11) -0.134(9) 0.144(9) -0.261(9) Cl5 0.154(5) 0.420(15) 0.467(16) 0.061(12) -0.115(7) -0.107(8) Cl6 0.417(10) 0.216(7) 0.435(12) 0.130(7) 0.241(9) 0.154(7) N1 0.051(2) 0.046(2) 0.0460(19) 0.0009(17) -0.0024(17) 0.0033(18) N2 0.066(3) 0.087(4) 0.075(3) -0.002(2) -0.026(2) 0.009(3) O1 0.068(2) 0.0462(18) 0.0576(18) 0.0116(15) -0.0026(16) 0.0001(17) O2 0.076(2) 0.0473(19) 0.066(2) 0.0092(16) -0.0111(17) -0.0092(18) Pt1 0.05759(11) 0.03965(10) 0.04651(10) 0.00473(8) -0.00358(8) 0.00029(9) _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 C2 1.346(7) . ? C1 N1 1.359(6) . ? C1 H1A 0.9300 . ? C2 C3 1.408(7) . ? C2 H2A 0.9300 . ? C3 C4 1.380(7) . ? C3 H3A 0.9300 . ? C4 C5 1.390(6) . ? C4 H4A 0.9300 . ? C5 N1 1.349(5) . ? C5 C6 1.467(6) . ? C6 C7 1.406(6) . ? C6 C18 1.413(6) . ? C7 C8 1.397(6) . ? C7 Pt1 1.969(4) . ? C8 C9 1.402(6) . ? C8 H8A 0.9300 . ? C9 C17 1.402(6) . ? C9 C10 1.468(6) . ? C10 C15 1.386(7) . ? C10 C11 1.388(7) . ? C11 C12 1.383(7) . ? C11 H11A 0.9300 . ? C12 C13 1.420(8) . ? C12 H12A 0.9300 . ? C13 C14 1.373(7) . ? C13 N2 1.409(7) . ? C14 C15 1.386(7) . ? C14 H14A 0.9300 . ? C15 C16 1.532(7) . ? C16 C19 1.525(6) . ? C16 C17 1.530(6) . ? C16 C21 1.532(7) . ? C17 C18 1.390(6) . ? C18 H18A 0.9300 . ? C19 C20 1.514(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.501(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C28 1.367(10) . ? C23 N2 1.374(8) . ? C23 C24 1.441(10) . ? C24 C25 1.436(14) . ? C24 H24A 0.9300 . ? C25 C26 1.51(2) . ? C25 H25A 0.9300 . ? C26 C27 1.18(2) . ? C26 H26A 0.9300 . ? C27 C28 1.400(14) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C29 C34 1.344(10) . ? C29 C30 1.358(8) . ? C29 N2 1.401(8) . ? C30 C31 1.427(11) . ? C30 H30A 0.9300 . ? C31 C32 1.345(14) . ? C31 H31A 0.9300 . ? C32 C33 1.365(12) . ? C32 H32A 0.9300 . ? C33 C34 1.439(11) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.523(7) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O1 1.276(6) . ? C36 C37 1.393(8) . ? C37 C38 1.374(8) . ? C37 H37A 0.9300 . ? C38 O2 1.277(6) . ? C38 C39 1.519(8) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 Cl2 1.683(10) . ? C40 Cl1 1.730(10) . ? C40 Cl3 1.731(11) . ? C40 H40A 0.9800 . ? C41 Cl6 1.696(13) . ? C41 Cl4 1.715(14) . ? C41 Cl5 1.720(13) . ? C41 H41 0.9800 . ? N1 Pt1 1.990(4) . ? O1 Pt1 2.085(3) . ? O2 Pt1 2.018(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 C2 C1 N1 122.7(5) . . ? C2 C1 H1A 118.6 . . ? N1 C1 H1A 118.6 . . ? C1 C2 C3 119.2(5) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? C4 C3 C2 118.2(5) . . ? C4 C3 H3A 120.9 . . ? C2 C3 H3A 120.9 . . ? C3 C4 C5 120.2(4) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? N1 C5 C4 120.4(4) . . ? N1 C5 C6 113.0(4) . . ? C4 C5 C6 126.7(4) . . ? C7 C6 C18 121.9(4) . . ? C7 C6 C5 114.3(4) . . ? C18 C6 C5 123.7(4) . . ? C8 C7 C6 118.9(4) . . ? C8 C7 Pt1 126.4(4) . . ? C6 C7 Pt1 114.6(3) . . ? C7 C8 C9 119.2(4) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C8 C9 C17 121.6(4) . . ? C8 C9 C10 130.2(4) . . ? C17 C9 C10 108.2(4) . . ? C15 C10 C11 121.3(5) . . ? C15 C10 C9 108.6(4) . . ? C11 C10 C9 130.0(5) . . ? C12 C11 C10 118.0(5) . . ? C12 C11 H11A 121.0 . . ? C10 C11 H11A 121.0 . . ? C11 C12 C13 121.5(5) . . ? C11 C12 H12A 119.3 . . ? C13 C12 H12A 119.3 . . ? C14 C13 N2 121.6(5) . . ? C14 C13 C12 118.7(5) . . ? N2 C13 C12 119.7(5) . . ? C13 C14 C15 120.4(5) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C10 C15 C14 120.1(5) . . ? C10 C15 C16 111.7(4) . . ? C14 C15 C16 128.2(4) . . ? C19 C16 C17 111.9(4) . . ? C19 C16 C15 112.2(4) . . ? C17 C16 C15 100.2(4) . . ? C19 C16 C21 109.5(4) . . ? C17 C16 C21 111.3(4) . . ? C15 C16 C21 111.5(4) . . ? C18 C17 C9 119.9(4) . . ? C18 C17 C16 128.8(4) . . ? C9 C17 C16 111.3(4) . . ? C17 C18 C6 118.4(4) . . ? C17 C18 H18A 120.8 . . ? C6 C18 H18A 120.8 . . ? C20 C19 C16 116.3(4) . . ? C20 C19 H19A 108.2 . . ? C16 C19 H19A 108.2 . . ? C20 C19 H19B 108.2 . . ? C16 C19 H19B 108.2 . . ? H19A C19 H19B 107.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C16 115.6(5) . . ? C22 C21 H21A 108.4 . . ? C16 C21 H21A 108.4 . . ? C22 C21 H21B 108.4 . . ? C16 C21 H21B 108.4 . . ? H21A C21 H21B 107.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 N2 121.2(7) . . ? C28 C23 C24 118.4(8) . . ? N2 C23 C24 120.4(7) . . ? C25 C24 C23 115.1(9) . . ? C25 C24 H24A 122.4 . . ? C23 C24 H24A 122.4 . . ? C24 C25 C26 121.7(11) . . ? C24 C25 H25A 119.1 . . ? C26 C25 H25A 119.1 . . ? C27 C26 C25 115.5(14) . . ? C27 C26 H26A 122.2 . . ? C25 C26 H26A 122.2 . . ? C26 C27 C28 128.0(15) . . ? C26 C27 H27A 116.0 . . ? C28 C27 H27A 116.0 . . ? C23 C28 C27 120.8(9) . . ? C23 C28 H28A 119.6 . . ? C27 C28 H28A 119.6 . . ? C34 C29 C30 116.9(7) . . ? C34 C29 N2 121.3(6) . . ? C30 C29 N2 121.7(7) . . ? C29 C30 C31 122.5(8) . . ? C29 C30 H30A 118.7 . . ? C31 C30 H30A 118.7 . . ? C32 C31 C30 117.7(8) . . ? C32 C31 H31A 121.1 . . ? C30 C31 H31A 121.1 . . ? C31 C32 C33 123.0(9) . . ? C31 C32 H32A 118.5 . . ? C33 C32 H32A 118.5 . . ? C32 C33 C34 116.0(9) . . ? C32 C33 H33A 122.0 . . ? C34 C33 H33A 122.0 . . ? C29 C34 C33 123.6(8) . . ? C29 C34 H34A 118.2 . . ? C33 C34 H34A 118.2 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O1 C36 C37 126.6(5) . . ? O1 C36 C35 113.5(4) . . ? C37 C36 C35 119.8(5) . . ? C38 C37 C36 127.1(5) . . ? C38 C37 H37A 116.4 . . ? C36 C37 H37A 116.4 . . ? O2 C38 C37 127.4(5) . . ? O2 C38 C39 113.7(5) . . ? C37 C38 C39 118.9(5) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Cl2 C40 Cl1 107.5(6) . . ? Cl2 C40 Cl3 115.9(7) . . ? Cl1 C40 Cl3 109.8(6) . . ? Cl2 C40 H40A 107.8 . . ? Cl1 C40 H40A 107.8 . . ? Cl3 C40 H40A 107.8 . . ? Cl6 C41 Cl4 103.7(9) . . ? Cl6 C41 Cl5 105.4(8) . . ? Cl4 C41 Cl5 111.2(9) . . ? Cl6 C41 H41 112.0 . . ? Cl4 C41 H41 112.0 . . ? Cl5 C41 H41 112.0 . . ? C5 N1 C1 119.3(4) . . ? C5 N1 Pt1 117.0(3) . . ? C1 N1 Pt1 123.7(3) . . ? C23 N2 C29 119.4(5) . . ? C23 N2 C13 119.3(5) . . ? C29 N2 C13 120.9(5) . . ? C36 O1 Pt1 122.4(3) . . ? C38 O2 Pt1 123.8(3) . . ? C7 Pt1 N1 81.07(17) . . ? C7 Pt1 O2 93.04(17) . . ? N1 Pt1 O2 174.10(14) . . ? C7 Pt1 O1 174.83(16) . . ? N1 Pt1 O1 93.84(14) . . ? O2 Pt1 O1 92.05(13) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.136 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.134 # Attachment 'compound 2.cif' data_wy1393wm _database_code_depnum_ccdc_archive 'CCDC 639791' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H40 N2 O2 Pt' _chemical_formula_weight 787.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.7385(5) _cell_length_b 11.2842(5) _cell_length_c 31.6544(15) _cell_angle_alpha 90.00 _cell_angle_beta 94.9410(10) _cell_angle_gamma 90.00 _cell_volume 3465.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 4.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7623 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20129 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.27 _reflns_number_total 7979 _reflns_number_gt 6760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+2.4500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7979 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.003 _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 0.1254(4) 0.9835(4) 1.06450(11) 0.0573(10) Uani 1 1 d . . . H1A H 0.0659 0.9650 1.0850 0.069 Uiso 1 1 calc R . . C2 C 0.2124(5) 1.0779(4) 1.07079(12) 0.0630(11) Uani 1 1 d . . . H2A H 0.2107 1.1236 1.0952 0.076 Uiso 1 1 calc R . . C3 C 0.3017(4) 1.1054(4) 1.04137(13) 0.0639(11) Uani 1 1 d . . . H3A H 0.3621 1.1689 1.0458 0.077 Uiso 1 1 calc R . . C4 C 0.3014(4) 1.0377(4) 1.00495(12) 0.0583(10) Uani 1 1 d . . . H4A H 0.3611 1.0559 0.9845 0.070 Uiso 1 1 calc R . . C5 C 0.2118(4) 0.9429(3) 0.99910(11) 0.0458(8) Uani 1 1 d . . . C6 C 0.1975(4) 0.8631(3) 0.96227(10) 0.0444(7) Uani 1 1 d . . . C7 C 0.0965(4) 0.7736(3) 0.96484(10) 0.0419(7) Uani 1 1 d . . . C8 C 0.0784(4) 0.6926(3) 0.93106(10) 0.0428(7) Uani 1 1 d . . . H8A H 0.0146 0.6315 0.9320 0.051 Uiso 1 1 calc R . . C9 C 0.1546(4) 0.7034(3) 0.89646(11) 0.0413(7) Uani 1 1 d . . . C10 C 0.1558(3) 0.6333(3) 0.85730(10) 0.0395(7) Uani 1 1 d . . . C11 C 0.0827(4) 0.5331(3) 0.84350(11) 0.0468(8) Uani 1 1 d . . . H11A H 0.0224 0.4971 0.8608 0.056 Uiso 1 1 calc R . . C12 C 0.1002(4) 0.4872(3) 0.80375(10) 0.0478(8) Uani 1 1 d . . . H12A H 0.0502 0.4207 0.7942 0.057 Uiso 1 1 calc R . . C13 C 0.1924(4) 0.5394(3) 0.77766(10) 0.0446(8) Uani 1 1 d . . . C14 C 0.2684(3) 0.6373(3) 0.79199(10) 0.0437(7) Uani 1 1 d . . . H14A H 0.3316 0.6713 0.7752 0.052 Uiso 1 1 calc R . . C15 C 0.2494(3) 0.6843(3) 0.83154(10) 0.0409(7) Uani 1 1 d . . . C16 C 0.3241(3) 0.7889(3) 0.85366(11) 0.0425(7) Uani 1 1 d . . . C17 C 0.2526(4) 0.7961(3) 0.89412(11) 0.0430(7) Uani 1 1 d . . . C18 C 0.2741(4) 0.8746(3) 0.92715(11) 0.0480(8) Uani 1 1 d . . . H18A H 0.3389 0.9349 0.9261 0.058 Uiso 1 1 calc R . . C19 C 0.3073(4) 0.9033(3) 0.82718(11) 0.0491(8) Uani 1 1 d . . . H19A H 0.3527 0.9674 0.8433 0.059 Uiso 1 1 calc R . . H19B H 0.3545 0.8930 0.8017 0.059 Uiso 1 1 calc R . . C20 C 0.1605(4) 0.9398(4) 0.81443(14) 0.0647(11) Uani 1 1 d . . . H20A H 0.1601 1.0121 0.7984 0.097 Uiso 1 1 calc R . . H20B H 0.1128 0.9519 0.8394 0.097 Uiso 1 1 calc R . . H20C H 0.1152 0.8786 0.7974 0.097 Uiso 1 1 calc R . . C21 C 0.4787(4) 0.7627(3) 0.86285(12) 0.0521(9) Uani 1 1 d . . . H21A H 0.5190 0.7547 0.8360 0.063 Uiso 1 1 calc R . . H21B H 0.5218 0.8304 0.8775 0.063 Uiso 1 1 calc R . . C22 C 0.5131(4) 0.6526(4) 0.88914(14) 0.0692(11) Uani 1 1 d . . . H22A H 0.6113 0.6434 0.8933 0.104 Uiso 1 1 calc R . . H22B H 0.4734 0.5844 0.8746 0.104 Uiso 1 1 calc R . . H22C H 0.4762 0.6602 0.9162 0.104 Uiso 1 1 calc R . . C23 C 0.2271(4) 0.5699(3) 0.70269(10) 0.0425(7) Uani 1 1 d . . . C24 C 0.3345(4) 0.5548(3) 0.67757(11) 0.0496(8) Uani 1 1 d . . . H24A H 0.3947 0.4913 0.6825 0.060 Uiso 1 1 calc R . . C25 C 0.3536(4) 0.6338(4) 0.64492(12) 0.0594(10) Uani 1 1 d . . . H25A H 0.4264 0.6218 0.6282 0.071 Uiso 1 1 calc R . . C26 C 0.2675(5) 0.7293(4) 0.63674(13) 0.0634(11) Uani 1 1 d . . . C27 C 0.1600(5) 0.7424(4) 0.66190(15) 0.0649(11) Uani 1 1 d . . . H27A H 0.0996 0.8057 0.6567 0.078 Uiso 1 1 calc R . . C28 C 0.1384(4) 0.6650(3) 0.69455(13) 0.0569(9) Uani 1 1 d . . . H28A H 0.0648 0.6767 0.7110 0.068 Uiso 1 1 calc R . . C29 C 0.2896(7) 0.8150(5) 0.60099(15) 0.0934(18) Uani 1 1 d . . . H29A H 0.2202 0.8756 0.6000 0.140 Uiso 1 1 calc R . . H29B H 0.2834 0.7730 0.5745 0.140 Uiso 1 1 calc R . . H29C H 0.3791 0.8507 0.6058 0.140 Uiso 1 1 calc R . . C30 C 0.2378(3) 0.3691(3) 0.73227(10) 0.0396(7) Uani 1 1 d . . . C31 C 0.1862(4) 0.3089(3) 0.69593(12) 0.0472(8) Uani 1 1 d . . . H31A H 0.1290 0.3481 0.6754 0.057 Uiso 1 1 calc R . . C32 C 0.2191(4) 0.1917(3) 0.69016(13) 0.0526(9) Uani 1 1 d . . . H32A H 0.1833 0.1530 0.6657 0.063 Uiso 1 1 calc R . . C33 C 0.3038(4) 0.1301(3) 0.71976(12) 0.0552(9) Uani 1 1 d . . . C34 C 0.3527(4) 0.1902(3) 0.75590(13) 0.0570(10) Uani 1 1 d . . . H34A H 0.4084 0.1504 0.7766 0.068 Uiso 1 1 calc R . . C35 C 0.3210(4) 0.3081(3) 0.76219(11) 0.0493(8) Uani 1 1 d . . . H35A H 0.3561 0.3464 0.7868 0.059 Uiso 1 1 calc R . . C36 C 0.3422(7) 0.0034(4) 0.71274(16) 0.0882(16) Uani 1 1 d . . . H36A H 0.2994 -0.0231 0.6859 0.132 Uiso 1 1 calc R . . H36B H 0.3113 -0.0448 0.7350 0.132 Uiso 1 1 calc R . . H36C H 0.4405 -0.0030 0.7127 0.132 Uiso 1 1 calc R . . C37 C -0.2533(6) 0.7606(5) 1.12317(16) 0.0813(15) Uani 1 1 d . . . H37A H -0.2047 0.8274 1.1359 0.122 Uiso 1 1 calc R . . H37B H -0.2421 0.6937 1.1419 0.122 Uiso 1 1 calc R . . H37C H -0.3495 0.7794 1.1182 0.122 Uiso 1 1 calc R . . C38 C -0.1965(5) 0.7312(4) 1.08177(13) 0.0608(10) Uani 1 1 d . . . C39 C -0.2527(5) 0.6355(4) 1.05761(13) 0.0673(11) Uani 1 1 d . . . H39A H -0.3235 0.5939 1.0689 0.081 Uiso 1 1 calc R . . C40 C -0.2137(4) 0.5963(4) 1.01873(12) 0.0546(9) Uani 1 1 d . . . C41 C -0.2876(5) 0.4939(4) 0.99690(13) 0.0684(11) Uani 1 1 d . . . H41A H -0.2486 0.4780 0.9706 0.103 Uiso 1 1 calc R . . H41B H -0.3835 0.5130 0.9913 0.103 Uiso 1 1 calc R . . H41C H -0.2780 0.4251 1.0148 0.103 Uiso 1 1 calc R . . N1 N 0.1242(3) 0.9165(3) 1.02909(8) 0.0460(7) Uani 1 1 d . . . N2 N 0.2070(3) 0.4910(2) 0.73676(8) 0.0492(7) Uani 1 1 d . . . O1 O -0.0979(3) 0.7969(2) 1.07230(8) 0.0621(7) Uani 1 1 d . . . O2 O -0.1182(3) 0.6397(2) 0.99813(7) 0.0538(6) Uani 1 1 d . . . Pt1 Pt -0.000803(14) 0.778386(13) 1.016402(4) 0.04670(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 0.068(3) 0.064(2) 0.0396(18) -0.0082(17) 0.0014(17) 0.014(2) C2 0.077(3) 0.068(3) 0.043(2) -0.0162(18) -0.0061(19) 0.010(2) C3 0.069(3) 0.063(2) 0.057(2) -0.014(2) -0.010(2) 0.000(2) C4 0.064(2) 0.059(2) 0.051(2) -0.0121(17) 0.0025(18) -0.0018(19) C5 0.0476(19) 0.0497(19) 0.0391(17) -0.0061(14) -0.0021(15) 0.0070(15) C6 0.0467(19) 0.0481(19) 0.0386(17) -0.0052(14) 0.0045(14) 0.0033(15) C7 0.0481(19) 0.0438(17) 0.0341(15) -0.0001(13) 0.0053(13) 0.0059(15) C8 0.0466(18) 0.0413(17) 0.0418(17) -0.0054(13) 0.0107(14) -0.0027(14) C9 0.0427(18) 0.0406(18) 0.0415(17) -0.0047(13) 0.0091(14) -0.0004(13) C10 0.0417(17) 0.0416(17) 0.0365(16) -0.0047(13) 0.0116(13) -0.0011(13) C11 0.055(2) 0.0411(18) 0.0472(19) -0.0026(14) 0.0185(15) -0.0055(15) C12 0.058(2) 0.0409(18) 0.0457(18) -0.0040(15) 0.0113(15) -0.0074(15) C13 0.055(2) 0.0408(17) 0.0391(17) -0.0049(13) 0.0119(15) 0.0038(15) C14 0.0463(19) 0.0461(19) 0.0405(17) -0.0012(14) 0.0142(14) -0.0041(14) C15 0.0415(18) 0.0396(16) 0.0425(17) -0.0040(13) 0.0093(14) -0.0023(13) C16 0.0403(17) 0.0441(18) 0.0444(17) -0.0057(14) 0.0112(14) -0.0058(14) C17 0.0442(18) 0.0424(18) 0.0433(18) -0.0041(13) 0.0089(14) -0.0020(14) C18 0.0463(19) 0.053(2) 0.0456(19) -0.0083(15) 0.0069(15) -0.0066(15) C19 0.049(2) 0.048(2) 0.052(2) -0.0036(16) 0.0131(16) -0.0082(15) C20 0.052(2) 0.064(3) 0.077(3) 0.010(2) 0.004(2) 0.0037(19) C21 0.0422(19) 0.064(2) 0.051(2) -0.0068(17) 0.0092(15) -0.0022(16) C22 0.062(3) 0.076(3) 0.069(3) 0.002(2) 0.004(2) 0.012(2) C23 0.0518(19) 0.0378(17) 0.0379(17) -0.0031(13) 0.0049(14) -0.0026(14) C24 0.051(2) 0.053(2) 0.0446(19) 0.0032(15) 0.0063(15) 0.0017(16) C25 0.067(3) 0.065(3) 0.048(2) -0.0001(18) 0.0137(18) -0.012(2) C26 0.091(3) 0.052(2) 0.045(2) 0.0049(17) -0.004(2) -0.018(2) C27 0.083(3) 0.044(2) 0.066(3) 0.0085(18) -0.003(2) 0.0094(19) C28 0.061(2) 0.050(2) 0.061(2) -0.0029(18) 0.0126(18) 0.0082(18) C29 0.138(5) 0.079(3) 0.060(3) 0.024(2) -0.004(3) -0.031(3) C30 0.0435(18) 0.0370(16) 0.0392(16) -0.0032(13) 0.0089(13) -0.0022(13) C31 0.0411(18) 0.051(2) 0.0494(19) -0.0080(15) 0.0034(15) -0.0006(14) C32 0.052(2) 0.049(2) 0.059(2) -0.0172(17) 0.0149(17) -0.0121(16) C33 0.071(3) 0.0404(19) 0.058(2) -0.0007(16) 0.0265(19) -0.0053(17) C34 0.074(3) 0.0442(19) 0.054(2) 0.0105(16) 0.0123(19) 0.0073(18) C35 0.061(2) 0.048(2) 0.0388(17) -0.0016(14) 0.0042(16) -0.0040(16) C36 0.138(5) 0.049(2) 0.083(3) -0.001(2) 0.039(3) 0.011(3) C37 0.103(4) 0.082(3) 0.064(3) -0.004(2) 0.040(3) 0.009(3) C38 0.073(3) 0.066(3) 0.047(2) 0.0086(19) 0.0219(19) 0.020(2) C39 0.075(3) 0.068(3) 0.063(3) 0.003(2) 0.033(2) 0.001(2) C40 0.055(2) 0.056(2) 0.054(2) 0.0077(17) 0.0117(17) 0.0082(17) C41 0.070(3) 0.074(3) 0.064(2) 0.003(2) 0.018(2) -0.003(2) N1 0.0485(16) 0.0519(17) 0.0366(14) -0.0075(12) -0.0023(12) 0.0121(13) N2 0.072(2) 0.0388(15) 0.0383(14) -0.0022(12) 0.0130(13) 0.0039(13) O1 0.078(2) 0.0665(18) 0.0451(14) -0.0055(12) 0.0250(13) 0.0080(14) O2 0.0630(16) 0.0603(16) 0.0401(13) -0.0067(11) 0.0164(11) -0.0009(12) Pt1 0.05311(9) 0.05311(9) 0.03516(7) -0.00286(6) 0.01106(5) 0.00870(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 N1 1.351(4) . ? C1 C2 1.364(6) . ? C1 H1A 0.9300 . ? C2 C3 1.364(6) . ? C2 H2A 0.9300 . ? C3 C4 1.383(5) . ? C3 H3A 0.9300 . ? C4 C5 1.383(5) . ? C4 H4A 0.9300 . ? C5 N1 1.362(5) . ? C5 C6 1.471(4) . ? C6 C18 1.397(5) . ? C6 C7 1.417(5) . ? C7 C8 1.406(5) . ? C7 Pt1 1.958(3) . ? C8 C9 1.380(5) . ? C8 H8A 0.9300 . ? C9 C17 1.422(5) . ? C9 C10 1.471(4) . ? C10 C11 1.387(5) . ? C10 C15 1.399(4) . ? C11 C12 1.385(4) . ? C11 H11A 0.9300 . ? C12 C13 1.401(5) . ? C12 H12A 0.9300 . ? C13 C14 1.385(5) . ? C13 N2 1.424(4) . ? C14 C15 1.386(4) . ? C14 H14A 0.9300 . ? C15 C16 1.524(5) . ? C16 C17 1.512(5) . ? C16 C21 1.537(5) . ? C16 C19 1.541(5) . ? C17 C18 1.373(5) . ? C18 H18A 0.9300 . ? C19 C20 1.509(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.517(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.378(5) . ? C23 C28 1.388(5) . ? C23 N2 1.425(4) . ? C24 C25 1.389(5) . ? C24 H24A 0.9300 . ? C25 C26 1.377(6) . ? C25 H25A 0.9300 . ? C26 C27 1.377(7) . ? C26 C29 1.518(6) . ? C27 C28 1.383(6) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C35 1.376(5) . ? C30 C31 1.393(5) . ? C30 N2 1.417(4) . ? C31 C32 1.376(5) . ? C31 H31A 0.9300 . ? C32 C33 1.382(6) . ? C32 H32A 0.9300 . ? C33 C34 1.378(6) . ? C33 C36 1.500(5) . ? C34 C35 1.384(5) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.503(6) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 O1 1.270(5) . ? C38 C39 1.406(6) . ? C39 C40 1.391(5) . ? C39 H39A 0.9300 . ? C40 O2 1.278(4) . ? C40 C41 1.499(6) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? N1 Pt1 1.997(3) . ? O1 Pt1 2.087(3) . ? O2 Pt1 1.994(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 N1 C1 C2 121.3(4) . . ? N1 C1 H1A 119.4 . . ? C2 C1 H1A 119.4 . . ? C3 C2 C1 120.1(4) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C2 C3 C4 119.2(4) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C3 C4 C5 119.7(4) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? N1 C5 C4 120.1(3) . . ? N1 C5 C6 113.4(3) . . ? C4 C5 C6 126.5(3) . . ? C18 C6 C7 122.2(3) . . ? C18 C6 C5 123.6(3) . . ? C7 C6 C5 114.2(3) . . ? C8 C7 C6 117.5(3) . . ? C8 C7 Pt1 127.9(3) . . ? C6 C7 Pt1 114.6(2) . . ? C9 C8 C7 120.4(3) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C17 121.0(3) . . ? C8 C9 C10 131.7(3) . . ? C17 C9 C10 107.3(3) . . ? C11 C10 C15 119.7(3) . . ? C11 C10 C9 131.5(3) . . ? C15 C10 C9 108.9(3) . . ? C12 C11 C10 119.4(3) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? C11 C12 C13 120.9(3) . . ? C11 C12 H12A 119.5 . . ? C13 C12 H12A 119.5 . . ? C14 C13 C12 119.6(3) . . ? C14 C13 N2 120.8(3) . . ? C12 C13 N2 119.6(3) . . ? C13 C14 C15 119.5(3) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C14 C15 C10 120.9(3) . . ? C14 C15 C16 128.0(3) . . ? C10 C15 C16 111.1(3) . . ? C17 C16 C15 101.2(3) . . ? C17 C16 C21 111.4(3) . . ? C15 C16 C21 111.1(3) . . ? C17 C16 C19 112.4(3) . . ? C15 C16 C19 112.0(3) . . ? C21 C16 C19 108.7(3) . . ? C18 C17 C9 119.6(3) . . ? C18 C17 C16 128.9(3) . . ? C9 C17 C16 111.4(3) . . ? C17 C18 C6 119.3(3) . . ? C17 C18 H18A 120.4 . . ? C6 C18 H18A 120.4 . . ? C20 C19 C16 115.3(3) . . ? C20 C19 H19A 108.4 . . ? C16 C19 H19A 108.4 . . ? C20 C19 H19B 108.4 . . ? C16 C19 H19B 108.4 . . ? H19A C19 H19B 107.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C16 115.3(3) . . ? C22 C21 H21A 108.4 . . ? C16 C21 H21A 108.4 . . ? C22 C21 H21B 108.4 . . ? C16 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 118.7(3) . . ? C24 C23 N2 121.3(3) . . ? C28 C23 N2 120.0(3) . . ? C23 C24 C25 120.4(4) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C26 C25 C24 121.6(4) . . ? C26 C25 H25A 119.2 . . ? C24 C25 H25A 119.2 . . ? C25 C26 C27 117.2(4) . . ? C25 C26 C29 121.1(5) . . ? C27 C26 C29 121.7(5) . . ? C26 C27 C28 122.4(4) . . ? C26 C27 H27A 118.8 . . ? C28 C27 H27A 118.8 . . ? C27 C28 C23 119.7(4) . . ? C27 C28 H28A 120.2 . . ? C23 C28 H28A 120.2 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 118.2(3) . . ? C35 C30 N2 122.3(3) . . ? C31 C30 N2 119.5(3) . . ? C32 C31 C30 120.5(3) . . ? C32 C31 H31A 119.8 . . ? C30 C31 H31A 119.8 . . ? C31 C32 C33 121.7(3) . . ? C31 C32 H32A 119.2 . . ? C33 C32 H32A 119.2 . . ? C34 C33 C32 117.3(3) . . ? C34 C33 C36 121.3(4) . . ? C32 C33 C36 121.4(4) . . ? C33 C34 C35 121.8(4) . . ? C33 C34 H34A 119.1 . . ? C35 C34 H34A 119.1 . . ? C30 C35 C34 120.5(3) . . ? C30 C35 H35A 119.8 . . ? C34 C35 H35A 119.8 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O1 C38 C39 125.9(4) . . ? O1 C38 C37 114.8(4) . . ? C39 C38 C37 119.3(4) . . ? C40 C39 C38 127.0(4) . . ? C40 C39 H39A 116.5 . . ? C38 C39 H39A 116.5 . . ? O2 C40 C39 126.6(4) . . ? O2 C40 C41 113.7(3) . . ? C39 C40 C41 119.8(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C1 N1 C5 119.6(3) . . ? C1 N1 Pt1 124.4(3) . . ? C5 N1 Pt1 116.0(2) . . ? C30 N2 C13 120.1(3) . . ? C30 N2 C23 119.1(3) . . ? C13 N2 C23 118.6(3) . . ? C38 O1 Pt1 123.3(3) . . ? C40 O2 Pt1 125.2(2) . . ? C7 Pt1 O2 92.47(12) . . ? C7 Pt1 N1 81.88(13) . . ? O2 Pt1 N1 174.32(10) . . ? C7 Pt1 O1 175.45(13) . . ? O2 Pt1 O1 91.95(11) . . ? N1 Pt1 O1 93.69(12) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 1.110 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.077 # Attachment 'compound 3.cif' data_wy1361wm _database_code_depnum_ccdc_archive 'CCDC 639792' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H27 N O2 Pt' _chemical_formula_weight 592.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.1679(5) _cell_length_b 26.7111(15) _cell_length_c 10.9458(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.2510(10) _cell_angle_gamma 90.00 _cell_volume 2280.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 6.176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5981 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13355 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 28.30 _reflns_number_total 5267 _reflns_number_gt 4832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+2.6110P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5267 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_restrained_S_all 1.176 _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 -0.0606(6) 0.25667(18) -0.5126(4) 0.0569(11) Uani 1 1 d . . . H1A H -0.1666 0.2710 -0.5084 0.085 Uiso 1 1 calc R . . H1B H -0.0664 0.2209 -0.5078 0.085 Uiso 1 1 calc R . . H1C H -0.0412 0.2660 -0.5919 0.085 Uiso 1 1 calc R . . C2 C 0.0839(5) 0.27571(14) -0.4030(4) 0.0444(9) Uani 1 1 d . . . C3 C 0.2505(6) 0.25985(15) -0.3900(4) 0.0498(10) Uani 1 1 d . . . H3A H 0.2634 0.2370 -0.4506 0.060 Uiso 1 1 calc R . . C4 C 0.3980(5) 0.27393(14) -0.2983(4) 0.0437(9) Uani 1 1 d . . . C5 C 0.5696(6) 0.25319(18) -0.3007(5) 0.0608(12) Uani 1 1 d . . . H5A H 0.6587 0.2668 -0.2304 0.091 Uiso 1 1 calc R . . H5B H 0.5901 0.2622 -0.3798 0.091 Uiso 1 1 calc R . . H5C H 0.5687 0.2174 -0.2934 0.091 Uiso 1 1 calc R . . C6 C -0.1320(5) 0.38039(16) -0.2002(4) 0.0461(9) Uani 1 1 d . . . H6A H -0.1662 0.3605 -0.2732 0.055 Uiso 1 1 calc R . . C7 C -0.2514(5) 0.40933(18) -0.1677(4) 0.0502(10) Uani 1 1 d . . . H7A H -0.3654 0.4090 -0.2179 0.060 Uiso 1 1 calc R . . C8 C -0.2013(5) 0.43886(16) -0.0603(4) 0.0470(9) Uani 1 1 d . . . H8A H -0.2805 0.4590 -0.0377 0.056 Uiso 1 1 calc R . . C9 C -0.0313(5) 0.43829(15) 0.0141(4) 0.0409(8) Uani 1 1 d . . . H9A H 0.0038 0.4578 0.0877 0.049 Uiso 1 1 calc R . . C10 C 0.0861(4) 0.40864(13) -0.0215(3) 0.0316(7) Uani 1 1 d . . . C11 C 0.2688(4) 0.40362(12) 0.0455(3) 0.0310(7) Uani 1 1 d . . . C12 C 0.3589(4) 0.37185(12) -0.0150(3) 0.0298(7) Uani 1 1 d . . . C13 C 0.5332(4) 0.36410(12) 0.0428(3) 0.0328(7) Uani 1 1 d . . . H13A H 0.5955 0.3438 0.0038 0.039 Uiso 1 1 calc R . . C14 C 0.6132(4) 0.38687(12) 0.1593(3) 0.0313(7) Uani 1 1 d . . . C15 C 0.5230(4) 0.41825(13) 0.2183(3) 0.0315(7) Uani 1 1 d . . . C16 C 0.3512(4) 0.42720(13) 0.1620(3) 0.0341(7) Uani 1 1 d . . . H16A H 0.2909 0.4485 0.2005 0.041 Uiso 1 1 calc R . . C17 C 0.7906(4) 0.38276(13) 0.2426(3) 0.0335(7) Uani 1 1 d . . . C18 C 0.9290(5) 0.35568(15) 0.2291(4) 0.0433(9) Uani 1 1 d . . . H18A H 0.9181 0.3364 0.1563 0.052 Uiso 1 1 calc R . . C19 C 1.0835(5) 0.35768(18) 0.3251(5) 0.0534(11) Uani 1 1 d . . . H19A H 1.1769 0.3394 0.3174 0.064 Uiso 1 1 calc R . . C20 C 1.0993(5) 0.38668(18) 0.4324(4) 0.0530(11) Uani 1 1 d . . . H20A H 1.2036 0.3877 0.4966 0.064 Uiso 1 1 calc R . . C21 C 0.9625(5) 0.41433(16) 0.4460(4) 0.0464(9) Uani 1 1 d . . . H21A H 0.9749 0.4341 0.5182 0.056 Uiso 1 1 calc R . . C22 C 0.8067(4) 0.41230(14) 0.3507(3) 0.0356(7) Uani 1 1 d . . . C23 C 0.6389(4) 0.43778(14) 0.3455(3) 0.0350(7) Uani 1 1 d . . . C24 C 0.5745(5) 0.42113(16) 0.4581(3) 0.0430(9) Uani 1 1 d . . . H24A H 0.6504 0.4350 0.5365 0.052 Uiso 1 1 calc R . . H24B H 0.4616 0.4353 0.4464 0.052 Uiso 1 1 calc R . . C25 C 0.5641(5) 0.36522(17) 0.4740(4) 0.0520(10) Uani 1 1 d . . . H25A H 0.5233 0.3582 0.5460 0.078 Uiso 1 1 calc R . . H25B H 0.6758 0.3508 0.4882 0.078 Uiso 1 1 calc R . . H25C H 0.4865 0.3511 0.3981 0.078 Uiso 1 1 calc R . . C26 C 0.6537(6) 0.49527(15) 0.3458(4) 0.0473(9) Uani 1 1 d . . . H26A H 0.5417 0.5094 0.3382 0.057 Uiso 1 1 calc R . . H26B H 0.7303 0.5057 0.4278 0.057 Uiso 1 1 calc R . . C27 C 0.7183(8) 0.51711(18) 0.2408(5) 0.0701(14) Uani 1 1 d . . . H27A H 0.7231 0.5529 0.2482 0.105 Uiso 1 1 calc R . . H27B H 0.6420 0.5079 0.1589 0.105 Uiso 1 1 calc R . . H27C H 0.8309 0.5043 0.2488 0.105 Uiso 1 1 calc R . . N1 N 0.0341(4) 0.38003(11) -0.1288(3) 0.0341(6) Uani 1 1 d . . . O1 O 0.0405(3) 0.30669(10) -0.3304(2) 0.0450(6) Uani 1 1 d . . . O2 O 0.4107(3) 0.30377(10) -0.2044(3) 0.0451(6) Uani 1 1 d . . . Pt1 Pt 0.213576(17) 0.339847(5) -0.172352(12) 0.03393(5) 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 0.061(3) 0.055(3) 0.046(2) -0.019(2) 0.002(2) -0.009(2) C2 0.057(2) 0.0347(19) 0.036(2) -0.0054(16) 0.0047(17) -0.0048(17) C3 0.059(2) 0.041(2) 0.041(2) -0.0171(18) 0.0032(18) 0.0057(18) C4 0.055(2) 0.0310(18) 0.041(2) -0.0076(16) 0.0084(18) 0.0048(16) C5 0.060(3) 0.051(3) 0.066(3) -0.018(2) 0.010(2) 0.010(2) C6 0.040(2) 0.054(2) 0.037(2) -0.0015(18) 0.0013(16) -0.0031(17) C7 0.037(2) 0.065(3) 0.042(2) 0.0038(19) 0.0015(17) 0.0038(18) C8 0.040(2) 0.053(2) 0.047(2) 0.0090(19) 0.0132(18) 0.0085(17) C9 0.0410(19) 0.044(2) 0.0366(19) -0.0012(16) 0.0095(16) 0.0032(16) C10 0.0355(17) 0.0312(17) 0.0261(16) 0.0031(13) 0.0058(13) -0.0014(13) C11 0.0360(17) 0.0291(16) 0.0267(16) 0.0025(13) 0.0074(13) -0.0004(13) C12 0.0394(17) 0.0253(15) 0.0221(15) -0.0018(12) 0.0051(13) -0.0018(13) C13 0.0399(18) 0.0280(17) 0.0307(17) -0.0021(13) 0.0110(14) 0.0007(13) C14 0.0336(16) 0.0293(16) 0.0303(17) 0.0012(13) 0.0086(13) 0.0007(13) C15 0.0343(16) 0.0327(17) 0.0259(15) -0.0026(13) 0.0066(13) -0.0021(13) C16 0.0361(17) 0.0343(18) 0.0319(17) -0.0044(14) 0.0099(14) 0.0047(14) C17 0.0344(17) 0.0354(18) 0.0322(17) 0.0009(14) 0.0123(14) -0.0022(14) C18 0.041(2) 0.045(2) 0.045(2) -0.0009(17) 0.0138(17) 0.0013(16) C19 0.036(2) 0.059(3) 0.066(3) 0.004(2) 0.017(2) 0.0048(18) C20 0.0294(18) 0.071(3) 0.052(2) 0.000(2) 0.0020(17) -0.0057(18) C21 0.0343(18) 0.057(2) 0.044(2) -0.0074(18) 0.0057(16) -0.0107(17) C22 0.0334(17) 0.0379(19) 0.0335(18) 0.0000(14) 0.0070(14) -0.0040(14) C23 0.0355(17) 0.0384(19) 0.0293(17) -0.0083(14) 0.0071(14) -0.0016(14) C24 0.0384(19) 0.059(2) 0.0302(18) -0.0018(17) 0.0089(15) 0.0022(17) C25 0.041(2) 0.064(3) 0.049(2) 0.012(2) 0.0102(18) 0.0012(19) C26 0.057(2) 0.036(2) 0.044(2) -0.0123(17) 0.0084(19) -0.0024(17) C27 0.099(4) 0.042(2) 0.073(3) 0.004(2) 0.032(3) -0.012(3) N1 0.0378(15) 0.0322(15) 0.0302(15) 0.0012(12) 0.0067(12) -0.0033(12) O1 0.0472(15) 0.0448(15) 0.0362(14) -0.0122(12) 0.0019(12) -0.0021(12) O2 0.0468(15) 0.0424(15) 0.0409(15) -0.0125(12) 0.0047(12) 0.0048(12) Pt1 0.04091(8) 0.03094(8) 0.02610(8) -0.00288(5) 0.00403(5) -0.00153(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.500(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.269(5) . ? C2 C3 1.392(6) . ? C3 C4 1.372(6) . ? C3 H3A 0.9300 . ? C4 O2 1.280(4) . ? C4 C5 1.515(6) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N1 1.350(5) . ? C6 C7 1.372(6) . ? C6 H6A 0.9300 . ? C7 C8 1.374(6) . ? C7 H7A 0.9300 . ? C8 C9 1.385(5) . ? C8 H8A 0.9300 . ? C9 C10 1.386(5) . ? C9 H9A 0.9300 . ? C10 N1 1.360(4) . ? C10 C11 1.461(5) . ? C11 C16 1.403(5) . ? C11 C12 1.410(5) . ? C12 C13 1.391(5) . ? C12 Pt1 1.973(3) . ? C13 C14 1.388(5) . ? C13 H13A 0.9300 . ? C14 C15 1.395(5) . ? C14 C17 1.470(5) . ? C15 C16 1.376(5) . ? C15 C23 1.525(5) . ? C16 H16A 0.9300 . ? C17 C18 1.387(5) . ? C17 C22 1.395(5) . ? C18 C19 1.383(6) . ? C18 H18A 0.9300 . ? C19 C20 1.380(6) . ? C19 H19A 0.9300 . ? C20 C21 1.384(6) . ? C20 H20A 0.9300 . ? C21 C22 1.386(5) . ? C21 H21A 0.9300 . ? C22 C23 1.517(5) . ? C23 C26 1.540(5) . ? C23 C24 1.542(5) . ? C24 C25 1.509(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.517(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N1 Pt1 1.985(3) . ? O1 Pt1 2.080(2) . ? O2 Pt1 1.995(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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 125.5(4) . . ? O1 C2 C1 115.0(4) . . ? C3 C2 C1 119.5(4) . . ? C4 C3 C2 127.7(4) . . ? C4 C3 H3A 116.2 . . ? C2 C3 H3A 116.2 . . ? O2 C4 C3 127.1(4) . . ? O2 C4 C5 112.7(4) . . ? C3 C4 C5 120.2(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 121.6(4) . . ? N1 C6 H6A 119.2 . . ? C7 C6 H6A 119.2 . . ? C6 C7 C8 119.4(4) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? C7 C8 C9 119.3(4) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C8 C9 C10 119.8(4) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? N1 C10 C9 120.0(3) . . ? N1 C10 C11 113.1(3) . . ? C9 C10 C11 126.9(3) . . ? C16 C11 C12 121.4(3) . . ? C16 C11 C10 123.9(3) . . ? C12 C11 C10 114.7(3) . . ? C13 C12 C11 118.8(3) . . ? C13 C12 Pt1 127.0(2) . . ? C11 C12 Pt1 114.1(2) . . ? C14 C13 C12 119.5(3) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C13 C14 C15 121.2(3) . . ? C13 C14 C17 130.3(3) . . ? C15 C14 C17 108.4(3) . . ? C16 C15 C14 120.4(3) . . ? C16 C15 C23 128.6(3) . . ? C14 C15 C23 111.0(3) . . ? C15 C16 C11 118.7(3) . . ? C15 C16 H16A 120.7 . . ? C11 C16 H16A 120.7 . . ? C18 C17 C22 120.7(3) . . ? C18 C17 C14 131.1(3) . . ? C22 C17 C14 108.2(3) . . ? C19 C18 C17 119.2(4) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? C20 C19 C18 120.2(4) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C19 C20 C21 121.1(4) . . ? C19 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? C20 C21 C22 119.2(4) . . ? C20 C21 H21A 120.4 . . ? C22 C21 H21A 120.4 . . ? C21 C22 C17 119.6(3) . . ? C21 C22 C23 128.9(3) . . ? C17 C22 C23 111.4(3) . . ? C22 C23 C15 101.0(3) . . ? C22 C23 C26 112.2(3) . . ? C15 C23 C26 111.7(3) . . ? C22 C23 C24 111.0(3) . . ? C15 C23 C24 111.4(3) . . ? C26 C23 C24 109.3(3) . . ? C25 C24 C23 115.0(3) . . ? C25 C24 H24A 108.5 . . ? C23 C24 H24A 108.5 . . ? C25 C24 H24B 108.5 . . ? C23 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C23 115.2(3) . . ? C27 C26 H26A 108.5 . . ? C23 C26 H26A 108.5 . . ? C27 C26 H26B 108.5 . . ? C23 C26 H26B 108.5 . . ? H26A C26 H26B 107.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C6 N1 C10 119.9(3) . . ? C6 N1 Pt1 123.5(3) . . ? C10 N1 Pt1 116.6(2) . . ? C2 O1 Pt1 123.5(3) . . ? C4 O2 Pt1 124.3(3) . . ? C12 Pt1 N1 81.49(13) . . ? C12 Pt1 O2 93.15(12) . . ? N1 Pt1 O2 174.40(11) . . ? C12 Pt1 O1 174.34(12) . . ? N1 Pt1 O1 93.54(11) . . ? O2 Pt1 O1 91.89(11) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.946 _refine_diff_density_min -1.754 _refine_diff_density_rms 0.096 # Attachment 'cif_Pt-1.doc' data_wy1350wm _database_code_depnum_ccdc_archive 'CCDC 698299' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H17 N O3 Pt' _chemical_formula_weight 550.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.6884(7) _cell_length_b 7.8986(6) _cell_length_c 23.7456(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.0830(10) _cell_angle_gamma 90.00 _cell_volume 1810.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8447 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.020 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 7.777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3462 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8447 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3170 _reflns_number_gt 2909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+2.9457P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3170 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0694 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 0.8656(5) 0.8237(6) 0.40704(19) 0.0276(10) Uani 1 1 d . . . C2 C 0.7704(5) 0.8483(6) 0.3599(2) 0.0296(10) Uani 1 1 d . . . H2A H 0.7954 0.9087 0.3287 0.036 Uiso 1 1 calc R . . C3 C 0.6390(5) 0.7815(6) 0.3603(2) 0.0295(10) Uani 1 1 d . . . C4 C 0.5199(5) 0.7839(7) 0.3164(2) 0.0319(10) Uani 1 1 d . . . C5 C 0.5054(5) 0.8541(7) 0.2634(2) 0.0404(13) Uani 1 1 d . . . H5A H 0.5779 0.9136 0.2495 0.048 Uiso 1 1 calc R . . C6 C 0.3798(6) 0.8344(8) 0.2310(2) 0.0479(14) Uani 1 1 d . . . H6A H 0.3684 0.8817 0.1951 0.057 Uiso 1 1 calc R . . C7 C 0.2719(6) 0.7462(8) 0.2512(3) 0.0521(16) Uani 1 1 d . . . H7A H 0.1897 0.7315 0.2283 0.062 Uiso 1 1 calc R . . C8 C 0.2850(5) 0.6794(8) 0.3051(3) 0.0449(13) Uani 1 1 d . . . H8A H 0.2116 0.6226 0.3194 0.054 Uiso 1 1 calc R . . C9 C 0.4089(5) 0.6987(7) 0.3372(2) 0.0353(11) Uani 1 1 d . . . C10 C 0.4533(5) 0.6370(6) 0.3958(2) 0.0353(11) Uani 1 1 d . . . C11 C 0.5993(5) 0.6930(6) 0.4073(2) 0.0314(10) Uani 1 1 d . . . C12 C 0.6897(5) 0.6701(6) 0.4549(2) 0.0312(10) Uani 1 1 d . . . H12A H 0.6626 0.6130 0.4864 0.037 Uiso 1 1 calc R . . C13 C 0.8231(5) 0.7359(6) 0.4542(2) 0.0281(10) Uani 1 1 d . . . C14 C 0.9313(5) 0.7177(6) 0.50085(19) 0.0288(10) Uani 1 1 d . . . C15 C 0.9198(5) 0.6348(6) 0.5524(2) 0.0334(11) Uani 1 1 d . . . H15A H 0.8365 0.5847 0.5598 0.040 Uiso 1 1 calc R . . C16 C 1.0301(6) 0.6278(7) 0.5913(2) 0.0411(13) Uani 1 1 d . . . H16A H 1.0228 0.5741 0.6257 0.049 Uiso 1 1 calc R . . C17 C 1.1547(6) 0.7013(8) 0.5795(2) 0.0439(13) Uani 1 1 d . . . H17A H 1.2311 0.6980 0.6061 0.053 Uiso 1 1 calc R . . C18 C 1.1637(5) 0.7777(7) 0.5289(2) 0.0387(12) Uani 1 1 d . . . H18A H 1.2477 0.8252 0.5210 0.046 Uiso 1 1 calc R . . C19 C 1.1126(6) 1.1588(10) 0.2611(3) 0.0593(18) Uani 1 1 d . . . H19A H 1.0211 1.1231 0.2472 0.089 Uiso 1 1 calc R . . H19B H 1.1786 1.1149 0.2370 0.089 Uiso 1 1 calc R . . H19C H 1.1169 1.2802 0.2613 0.089 Uiso 1 1 calc R . . C20 C 1.1455(6) 1.0937(7) 0.3197(2) 0.0401(13) Uani 1 1 d . . . C21 C 1.2735(6) 1.1314(7) 0.3474(3) 0.0453(14) Uani 1 1 d . . . H21A H 1.3304 1.2024 0.3285 0.054 Uiso 1 1 calc R . . C22 C 1.3271(5) 1.0742(6) 0.4010(3) 0.0370(12) Uani 1 1 d . . . C23 C 1.4705(6) 1.1279(7) 0.4233(3) 0.0480(15) Uani 1 1 d . . . H23A H 1.4929 1.0794 0.4600 0.072 Uiso 1 1 calc R . . H23B H 1.4743 1.2491 0.4260 0.072 Uiso 1 1 calc R . . H23C H 1.5361 1.0895 0.3980 0.072 Uiso 1 1 calc R . . N1 N 1.0548(4) 0.7871(5) 0.48962(17) 0.0304(9) Uani 1 1 d . . . O1 O 0.3832(4) 0.5570(6) 0.42645(19) 0.0531(11) Uani 1 1 d . . . O2 O 1.0478(3) 1.0074(5) 0.33871(14) 0.0382(8) Uani 1 1 d . . . O3 O 1.2633(3) 0.9803(5) 0.43330(15) 0.0391(8) Uani 1 1 d . . . Pt1 Pt 1.059614(17) 0.90032(2) 0.415319(7) 0.02905(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 0.031(2) 0.027(2) 0.026(2) -0.0037(19) 0.0083(19) 0.0009(19) C2 0.032(2) 0.034(3) 0.024(2) -0.0005(19) 0.010(2) -0.004(2) C3 0.027(2) 0.032(3) 0.030(3) -0.005(2) 0.009(2) -0.0003(19) C4 0.029(2) 0.039(3) 0.028(3) -0.005(2) 0.006(2) 0.000(2) C5 0.032(3) 0.055(3) 0.036(3) -0.001(2) 0.008(2) -0.005(2) C6 0.041(3) 0.068(4) 0.034(3) -0.002(3) -0.003(2) -0.001(3) C7 0.032(3) 0.073(4) 0.050(4) -0.007(3) -0.004(3) -0.003(3) C8 0.028(3) 0.055(4) 0.052(4) -0.007(3) 0.004(2) -0.002(2) C9 0.028(2) 0.038(3) 0.042(3) -0.007(2) 0.009(2) 0.000(2) C10 0.029(3) 0.036(3) 0.042(3) 0.003(2) 0.009(2) -0.004(2) C11 0.027(2) 0.033(3) 0.035(3) 0.001(2) 0.009(2) -0.003(2) C12 0.034(3) 0.034(3) 0.027(3) 0.002(2) 0.011(2) -0.003(2) C13 0.027(2) 0.033(3) 0.026(2) -0.0034(19) 0.0085(19) 0.0005(18) C14 0.031(2) 0.030(2) 0.026(2) -0.0059(19) 0.0082(19) 0.0000(19) C15 0.038(3) 0.032(3) 0.032(3) 0.006(2) 0.012(2) 0.002(2) C16 0.047(3) 0.045(3) 0.032(3) 0.004(2) 0.005(2) 0.002(2) C17 0.044(3) 0.050(3) 0.036(3) 0.001(3) -0.004(2) 0.005(3) C18 0.034(3) 0.046(3) 0.035(3) 0.000(2) 0.000(2) -0.003(2) C19 0.046(3) 0.083(5) 0.051(4) 0.027(3) 0.015(3) 0.004(3) C20 0.036(3) 0.048(3) 0.038(3) 0.006(2) 0.016(2) 0.001(2) C21 0.032(3) 0.048(3) 0.057(4) 0.012(3) 0.015(3) -0.007(2) C22 0.028(3) 0.036(3) 0.049(3) -0.005(2) 0.012(2) 0.000(2) C23 0.030(3) 0.049(3) 0.066(4) -0.006(3) 0.008(3) -0.009(2) N1 0.027(2) 0.035(2) 0.030(2) -0.0014(18) 0.0055(17) 0.0001(17) O1 0.038(2) 0.063(3) 0.059(3) 0.020(2) 0.010(2) -0.0129(19) O2 0.0287(17) 0.052(2) 0.0349(19) 0.0054(17) 0.0087(15) -0.0068(16) O3 0.0284(17) 0.042(2) 0.047(2) 0.0021(17) 0.0039(16) -0.0040(16) Pt1 0.02450(13) 0.03548(14) 0.02799(13) -0.00050(7) 0.00702(8) -0.00385(7) _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 C2 1.400(7) . ? C1 C13 1.409(7) . ? C1 Pt1 1.968(5) . ? C2 C3 1.379(6) . ? C2 H2A 0.9300 . ? C3 C11 1.398(7) . ? C3 C4 1.486(6) . ? C4 C5 1.370(7) . ? C4 C9 1.396(7) . ? C5 C6 1.389(7) . ? C5 H5A 0.9300 . ? C6 C7 1.377(8) . ? C6 H6A 0.9300 . ? C7 C8 1.380(9) . ? C7 H7A 0.9300 . ? C8 C9 1.372(7) . ? C8 H8A 0.9300 . ? C9 C10 1.502(7) . ? C10 O1 1.216(6) . ? C10 C11 1.484(7) . ? C11 C12 1.380(7) . ? C12 C13 1.395(6) . ? C12 H12A 0.9300 . ? C13 C14 1.464(6) . ? C14 N1 1.363(6) . ? C14 C15 1.401(7) . ? C15 C16 1.350(8) . ? C15 H15A 0.9300 . ? C16 C17 1.390(8) . ? C16 H16A 0.9300 . ? C17 C18 1.355(8) . ? C17 H17A 0.9300 . ? C18 N1 1.346(6) . ? C18 H18A 0.9300 . ? C19 C20 1.491(8) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 O2 1.280(6) . ? C20 C21 1.384(8) . ? C21 C22 1.405(8) . ? C21 H21A 0.9300 . ? C22 O3 1.266(6) . ? C22 C23 1.503(7) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? N1 Pt1 1.982(4) . ? O2 Pt1 2.000(3) . ? O3 Pt1 2.080(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 C2 C1 C13 119.0(4) . . ? C2 C1 Pt1 126.4(4) . . ? C13 C1 Pt1 114.6(3) . . ? C3 C2 C1 119.0(4) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C2 C3 C11 121.1(4) . . ? C2 C3 C4 130.5(5) . . ? C11 C3 C4 108.4(4) . . ? C5 C4 C9 120.0(5) . . ? C5 C4 C3 131.3(5) . . ? C9 C4 C3 108.7(4) . . ? C4 C5 C6 118.5(5) . . ? C4 C5 H5A 120.8 . . ? C6 C5 H5A 120.8 . . ? C7 C6 C5 121.3(6) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C6 C7 C8 120.3(5) . . ? C6 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C9 C8 C7 118.5(5) . . ? C9 C8 H8A 120.8 . . ? C7 C8 H8A 120.8 . . ? C8 C9 C4 121.4(5) . . ? C8 C9 C10 130.0(5) . . ? C4 C9 C10 108.5(4) . . ? O1 C10 C11 128.3(5) . . ? O1 C10 C9 126.4(5) . . ? C11 C10 C9 105.3(4) . . ? C12 C11 C3 121.3(4) . . ? C12 C11 C10 129.5(5) . . ? C3 C11 C10 109.2(4) . . ? C11 C12 C13 117.5(4) . . ? C11 C12 H12A 121.2 . . ? C13 C12 H12A 121.2 . . ? C12 C13 C1 122.0(4) . . ? C12 C13 C14 123.8(4) . . ? C1 C13 C14 114.2(4) . . ? N1 C14 C15 119.8(4) . . ? N1 C14 C13 113.3(4) . . ? C15 C14 C13 126.9(4) . . ? C16 C15 C14 119.8(5) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C15 C16 C17 119.6(5) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 119.3(5) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? N1 C18 C17 122.1(5) . . ? N1 C18 H18A 119.0 . . ? C17 C18 H18A 119.0 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O2 C20 C21 127.3(5) . . ? O2 C20 C19 114.1(5) . . ? C21 C20 C19 118.6(5) . . ? C20 C21 C22 127.3(5) . . ? C20 C21 H21A 116.4 . . ? C22 C21 H21A 116.4 . . ? O3 C22 C21 125.1(5) . . ? O3 C22 C23 116.0(5) . . ? C21 C22 C23 118.9(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 . . ? C18 N1 C14 119.3(4) . . ? C18 N1 Pt1 124.2(3) . . ? C14 N1 Pt1 116.4(3) . . ? C20 O2 Pt1 124.1(3) . . ? C22 O3 Pt1 124.0(3) . . ? C1 Pt1 N1 81.53(17) . . ? C1 Pt1 O2 93.55(16) . . ? N1 Pt1 O2 175.07(14) . . ? C1 Pt1 O3 173.91(16) . . ? N1 Pt1 O3 92.92(15) . . ? O2 Pt1 O3 92.01(14) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.720 _refine_diff_density_min -1.537 _refine_diff_density_rms 0.122 # Attachment 'cif_Ir-1.doc' data_wy1358wm _database_code_depnum_ccdc_archive 'CCDC 698300' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H31 Cl4 Ir N2 O4' _chemical_formula_weight 973.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2247(18) _cell_length_b 13.728(2) _cell_length_c 13.838(2) _cell_angle_alpha 63.248(2) _cell_angle_beta 74.128(2) _cell_angle_gamma 74.473(3) _cell_volume 1966.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11580 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 28.31 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 3.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3651 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11580 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.31 _reflns_number_total 8501 _reflns_number_gt 7481 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0802P)^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_number_reflns 8501 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1124 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.008 _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 0.1918(4) 0.1152(4) 0.3705(4) 0.0332(9) Uani 1 1 d . . . C2 C 0.2295(4) 0.1713(4) 0.4169(4) 0.0394(10) Uani 1 1 d . . . H2A H 0.3078 0.1708 0.4081 0.047 Uiso 1 1 calc R . . C3 C 0.1497(4) 0.2265(4) 0.4748(4) 0.0398(11) Uani 1 1 d . . . C4 C 0.1672(5) 0.2916(5) 0.5296(5) 0.0474(12) Uani 1 1 d . . . C5 C 0.2648(6) 0.3139(6) 0.5393(5) 0.0584(15) Uani 1 1 d . . . H5A H 0.3374 0.2855 0.5099 0.070 Uiso 1 1 calc R . . C6 C 0.2527(7) 0.3806(7) 0.5948(7) 0.072(2) Uani 1 1 d . . . H6A H 0.3186 0.3982 0.6003 0.086 Uiso 1 1 calc R . . C7 C 0.1476(7) 0.4209(7) 0.6413(7) 0.072(2) Uani 1 1 d . . . H7A H 0.1429 0.4624 0.6805 0.086 Uiso 1 1 calc R . . C8 C 0.0469(7) 0.3999(7) 0.6303(6) 0.0674(18) Uani 1 1 d . . . H8A H -0.0252 0.4296 0.6592 0.081 Uiso 1 1 calc R . . C9 C 0.0569(5) 0.3340(5) 0.5754(5) 0.0496(13) Uani 1 1 d . . . C10 C -0.0336(5) 0.2979(5) 0.5515(5) 0.0488(13) Uani 1 1 d . . . C11 C 0.0315(4) 0.2292(4) 0.4880(4) 0.0411(11) Uani 1 1 d . . . C12 C -0.0097(4) 0.1741(4) 0.4464(4) 0.0391(10) Uani 1 1 d . . . H12A H -0.0882 0.1741 0.4574 0.047 Uiso 1 1 calc R . . C13 C 0.0718(4) 0.1182(4) 0.3869(4) 0.0349(10) Uani 1 1 d . . . C14 C 0.0412(4) 0.0594(4) 0.3344(4) 0.0363(10) Uani 1 1 d . . . C15 C -0.0700(5) 0.0522(5) 0.3338(5) 0.0462(12) Uani 1 1 d . . . H15A H -0.1334 0.0868 0.3688 0.055 Uiso 1 1 calc R . . C16 C -0.0862(5) -0.0059(6) 0.2814(5) 0.0534(14) Uani 1 1 d . . . H16A H -0.1604 -0.0096 0.2796 0.064 Uiso 1 1 calc R . . C17 C 0.0085(5) -0.0592(6) 0.2312(5) 0.0531(14) Uani 1 1 d . . . H17A H -0.0006 -0.1000 0.1963 0.064 Uiso 1 1 calc R . . C18 C 0.1166(5) -0.0497(5) 0.2347(4) 0.0452(12) Uani 1 1 d . . . H18A H 0.1807 -0.0856 0.2017 0.054 Uiso 1 1 calc R . . C19 C 0.2810(4) 0.1812(4) 0.1501(4) 0.0334(9) Uani 1 1 d . . . C20 C 0.1946(4) 0.2305(4) 0.0858(4) 0.0378(10) Uani 1 1 d . . . H20A H 0.1369 0.1916 0.0982 0.045 Uiso 1 1 calc R . . C21 C 0.1941(4) 0.3352(4) 0.0049(4) 0.0390(10) Uani 1 1 d . . . C22 C 0.1072(5) 0.4093(4) -0.0661(4) 0.0417(11) Uani 1 1 d . . . C23 C 0.0038(5) 0.3923(5) -0.0721(5) 0.0486(12) Uani 1 1 d . . . H23A H -0.0189 0.3233 -0.0322 0.058 Uiso 1 1 calc R . . C24 C -0.0652(6) 0.4799(6) -0.1386(5) 0.0587(16) Uani 1 1 d . . . H24A H -0.1370 0.4708 -0.1408 0.070 Uiso 1 1 calc R . . C25 C -0.0295(5) 0.5823(5) -0.2028(5) 0.0520(14) Uani 1 1 d . . . H25A H -0.0761 0.6391 -0.2498 0.062 Uiso 1 1 calc R . . C26 C 0.0746(6) 0.6003(5) -0.1974(5) 0.0529(14) Uani 1 1 d . . . H26A H 0.0976 0.6691 -0.2377 0.063 Uiso 1 1 calc R . . C27 C 0.1424(5) 0.5120(5) -0.1298(4) 0.0458(12) Uani 1 1 d . . . C28 C 0.2541(5) 0.5089(5) -0.1028(5) 0.0490(13) Uani 1 1 d . . . C29 C 0.2804(4) 0.3951(4) -0.0167(4) 0.0396(11) Uani 1 1 d . . . C30 C 0.3704(4) 0.3483(4) 0.0422(4) 0.0428(11) Uani 1 1 d . . . H30A H 0.4295 0.3868 0.0264 0.051 Uiso 1 1 calc R . . C31 C 0.3697(4) 0.2424(4) 0.1253(4) 0.0378(10) Uani 1 1 d . . . C32 C 0.4562(4) 0.1866(4) 0.1971(4) 0.0375(10) Uani 1 1 d . . . C33 C 0.5485(5) 0.2301(5) 0.1945(5) 0.0515(13) Uani 1 1 d . . . H33A H 0.5616 0.2996 0.1411 0.062 Uiso 1 1 calc R . . C34 C 0.6195(5) 0.1710(6) 0.2699(6) 0.0585(16) Uani 1 1 d . . . H34A H 0.6804 0.2003 0.2686 0.070 Uiso 1 1 calc R . . C35 C 0.6004(5) 0.0678(6) 0.3478(6) 0.0571(16) Uani 1 1 d . . . H35A H 0.6466 0.0274 0.4012 0.069 Uiso 1 1 calc R . . C36 C 0.5103(5) 0.0245(5) 0.3453(5) 0.0463(12) Uani 1 1 d . . . H36A H 0.5001 -0.0471 0.3951 0.056 Uiso 1 1 calc R . . C37 C 0.3610(8) -0.3074(6) 0.5231(6) 0.077(2) Uani 1 1 d . . . H37A H 0.3160 -0.2840 0.5800 0.115 Uiso 1 1 calc R . . H37B H 0.4380 -0.3391 0.5376 0.115 Uiso 1 1 calc R . . H37C H 0.3266 -0.3618 0.5216 0.115 Uiso 1 1 calc R . . C38 C 0.3647(5) -0.2092(5) 0.4135(5) 0.0500(13) Uani 1 1 d . . . C39 C 0.4251(6) -0.2244(5) 0.3200(6) 0.0629(17) Uani 1 1 d . . . H39A H 0.4646 -0.2957 0.3316 0.075 Uiso 1 1 calc R . . C40 C 0.4356(5) -0.1472(5) 0.2094(6) 0.0531(14) Uani 1 1 d . . . C41 C 0.5053(7) -0.1875(8) 0.1217(8) 0.081(2) Uani 1 1 d . . . H41A H 0.5049 -0.1271 0.0506 0.122 Uiso 1 1 calc R . . H41B H 0.4719 -0.2448 0.1247 0.122 Uiso 1 1 calc R . . H41C H 0.5833 -0.2162 0.1342 0.122 Uiso 1 1 calc R . . C42 C 0.6911(10) 0.4425(10) 0.7228(8) 0.115(4) Uani 1 1 d . . . H42A H 0.7449 0.4939 0.6932 0.139 Uiso 1 1 calc R . . H42B H 0.6997 0.4122 0.6693 0.139 Uiso 1 1 calc R . . C43 C 0.7107(13) 0.9802(12) 0.0745(11) 0.150(5) Uani 1 1 d . . . H43A H 0.7002 0.9729 0.0112 0.180 Uiso 1 1 calc R . . H43B H 0.6350 1.0001 0.1130 0.180 Uiso 1 1 calc R . . Cl1 Cl 0.7312(5) 0.3366(4) 0.8399(4) 0.206(3) Uani 1 1 d . . . Cl2 Cl 0.5609(5) 0.5123(5) 0.7330(6) 0.268(4) Uani 1 1 d . . . Cl3 Cl 0.7773(6) 0.8547(4) 0.1608(4) 0.212(3) Uani 1 1 d . . . Cl4 Cl 0.7881(5) 1.0826(3) 0.0307(3) 0.1595(15) Uani 1 1 d . . . Ir1 Ir 0.291091(14) 0.036577(14) 0.279008(13) 0.03299(8) Uani 1 1 d . . . N1 N 0.1341(4) 0.0089(3) 0.2837(3) 0.0363(8) Uani 1 1 d . . . N2 N 0.4384(3) 0.0832(4) 0.2732(4) 0.0384(9) Uani 1 1 d . . . O1 O -0.1378(4) 0.3195(4) 0.5774(4) 0.0721(14) Uani 1 1 d . . . O2 O 0.3067(5) 0.5848(4) -0.1402(5) 0.0734(14) Uani 1 1 d . . . O3 O 0.3112(3) -0.1182(3) 0.4188(3) 0.0465(9) Uani 1 1 d . . . O4 O 0.3882(3) -0.0468(3) 0.1752(3) 0.0480(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 0.035(2) 0.027(2) 0.025(2) -0.0002(17) -0.0047(17) -0.0051(18) C2 0.037(2) 0.040(3) 0.039(2) -0.015(2) -0.0069(19) -0.006(2) C3 0.043(3) 0.037(3) 0.038(2) -0.016(2) -0.008(2) -0.002(2) C4 0.054(3) 0.044(3) 0.044(3) -0.020(2) -0.008(2) -0.005(2) C5 0.057(4) 0.066(4) 0.062(4) -0.036(3) -0.013(3) -0.005(3) C6 0.075(5) 0.081(5) 0.080(5) -0.047(4) -0.015(4) -0.019(4) C7 0.086(5) 0.073(5) 0.081(5) -0.055(4) -0.016(4) -0.008(4) C8 0.072(4) 0.077(5) 0.062(4) -0.044(4) -0.008(3) -0.002(4) C9 0.056(3) 0.044(3) 0.044(3) -0.020(3) -0.009(2) 0.003(3) C10 0.050(3) 0.045(3) 0.043(3) -0.019(3) -0.003(2) -0.001(2) C11 0.042(3) 0.036(3) 0.037(2) -0.012(2) -0.007(2) 0.003(2) C12 0.036(2) 0.036(2) 0.034(2) -0.008(2) -0.0060(18) -0.0006(19) C13 0.033(2) 0.031(2) 0.032(2) -0.0064(19) -0.0074(17) -0.0028(18) C14 0.038(2) 0.033(2) 0.031(2) -0.0065(19) -0.0078(18) -0.0049(19) C15 0.037(3) 0.047(3) 0.045(3) -0.010(2) -0.011(2) -0.004(2) C16 0.042(3) 0.064(4) 0.058(3) -0.023(3) -0.016(2) -0.012(3) C17 0.050(3) 0.061(4) 0.059(3) -0.028(3) -0.012(3) -0.015(3) C18 0.050(3) 0.047(3) 0.040(3) -0.016(2) -0.008(2) -0.013(2) C19 0.034(2) 0.033(2) 0.032(2) -0.0149(19) -0.0036(17) -0.0032(18) C20 0.040(2) 0.037(3) 0.037(2) -0.013(2) -0.0068(19) -0.011(2) C21 0.046(3) 0.036(3) 0.033(2) -0.015(2) -0.0070(19) -0.004(2) C22 0.046(3) 0.036(3) 0.035(2) -0.011(2) -0.009(2) 0.000(2) C23 0.053(3) 0.045(3) 0.044(3) -0.014(2) -0.013(2) -0.005(2) C24 0.057(3) 0.070(4) 0.048(3) -0.025(3) -0.023(3) 0.009(3) C25 0.057(3) 0.049(3) 0.044(3) -0.016(3) -0.020(3) 0.004(3) C26 0.066(4) 0.039(3) 0.044(3) -0.008(2) -0.014(3) -0.006(3) C27 0.059(3) 0.039(3) 0.035(2) -0.012(2) -0.009(2) -0.006(2) C28 0.055(3) 0.038(3) 0.046(3) -0.011(2) -0.004(2) -0.012(2) C29 0.043(3) 0.031(2) 0.038(2) -0.009(2) -0.004(2) -0.008(2) C30 0.040(3) 0.039(3) 0.047(3) -0.014(2) -0.004(2) -0.012(2) C31 0.035(2) 0.033(2) 0.039(2) -0.013(2) -0.0041(19) -0.0038(19) C32 0.034(2) 0.037(3) 0.041(2) -0.018(2) -0.0037(19) -0.0062(19) C33 0.040(3) 0.044(3) 0.068(4) -0.017(3) -0.015(3) -0.008(2) C34 0.042(3) 0.059(4) 0.078(4) -0.023(3) -0.022(3) -0.011(3) C35 0.037(3) 0.063(4) 0.065(4) -0.018(3) -0.018(3) -0.005(3) C36 0.039(3) 0.045(3) 0.048(3) -0.015(2) -0.010(2) -0.003(2) C37 0.097(6) 0.044(4) 0.073(5) -0.009(3) -0.030(4) 0.003(4) C38 0.048(3) 0.034(3) 0.061(3) -0.011(3) -0.020(3) 0.001(2) C39 0.059(4) 0.047(3) 0.082(5) -0.034(3) -0.022(3) 0.015(3) C40 0.041(3) 0.052(3) 0.068(4) -0.029(3) -0.010(3) -0.001(2) C41 0.067(5) 0.085(6) 0.103(6) -0.065(5) 0.005(4) -0.002(4) C42 0.129(9) 0.101(8) 0.102(8) -0.046(7) -0.023(7) 0.015(7) C43 0.160(12) 0.146(12) 0.121(10) 0.002(9) -0.061(9) -0.056(10) Cl1 0.210(4) 0.174(4) 0.202(4) 0.034(3) -0.112(4) -0.105(4) Cl2 0.202(5) 0.158(4) 0.251(6) -0.031(4) 0.063(4) 0.071(4) Cl3 0.324(7) 0.132(3) 0.206(4) 0.009(3) -0.182(5) -0.084(4) Cl4 0.259(5) 0.118(3) 0.107(2) -0.037(2) -0.055(3) -0.033(3) Ir1 0.03214(11) 0.02969(11) 0.03291(11) -0.01017(8) -0.00590(7) -0.00313(7) N1 0.036(2) 0.032(2) 0.037(2) -0.0091(17) -0.0070(16) -0.0079(16) N2 0.0286(19) 0.041(2) 0.043(2) -0.018(2) -0.0051(16) -0.0025(17) O1 0.051(3) 0.083(4) 0.090(4) -0.055(3) -0.006(2) 0.005(2) O2 0.078(3) 0.046(3) 0.080(3) 0.001(2) -0.026(3) -0.022(2) O3 0.050(2) 0.0365(19) 0.043(2) -0.0056(16) -0.0119(16) -0.0065(16) O4 0.045(2) 0.047(2) 0.052(2) -0.0267(19) 0.0001(17) -0.0041(17) _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 C13 1.415(7) . ? C1 C2 1.419(7) . ? C1 Ir1 1.982(5) . ? C2 C3 1.375(7) . ? C2 H2A 0.9300 . ? C3 C11 1.398(8) . ? C3 C4 1.491(8) . ? C4 C5 1.363(9) . ? C4 C9 1.416(8) . ? C5 C6 1.396(9) . ? C5 H5A 0.9300 . ? C6 C7 1.363(11) . ? C6 H6A 0.9300 . ? C7 C8 1.397(10) . ? C7 H7A 0.9300 . ? C8 C9 1.385(9) . ? C8 H8A 0.9300 . ? C9 C10 1.491(9) . ? C10 O1 1.217(7) . ? C10 C11 1.502(7) . ? C11 C12 1.381(8) . ? C12 C13 1.403(7) . ? C12 H12A 0.9300 . ? C13 C14 1.470(7) . ? C14 N1 1.358(6) . ? C14 C15 1.392(7) . ? C15 C16 1.374(8) . ? C15 H15A 0.9300 . ? C16 C17 1.386(9) . ? C16 H16A 0.9300 . ? C17 C18 1.378(8) . ? C17 H17A 0.9300 . ? C18 N1 1.347(7) . ? C18 H18A 0.9300 . ? C19 C20 1.397(7) . ? C19 C31 1.423(7) . ? C19 Ir1 1.985(5) . ? C20 C21 1.369(7) . ? C20 H20A 0.9300 . ? C21 C29 1.395(7) . ? C21 C22 1.489(7) . ? C22 C23 1.376(8) . ? C22 C27 1.396(8) . ? C23 C24 1.375(8) . ? C23 H23A 0.9300 . ? C24 C25 1.395(10) . ? C24 H24A 0.9300 . ? C25 C26 1.386(9) . ? C25 H25A 0.9300 . ? C26 C27 1.377(8) . ? C26 H26A 0.9300 . ? C27 C28 1.496(9) . ? C28 O2 1.208(7) . ? C28 C29 1.493(8) . ? C29 C30 1.389(8) . ? C30 C31 1.390(7) . ? C30 H30A 0.9300 . ? C31 C32 1.465(7) . ? C32 N2 1.366(7) . ? C32 C33 1.397(7) . ? C33 C34 1.361(9) . ? C33 H33A 0.9300 . ? C34 C35 1.374(10) . ? C34 H34A 0.9300 . ? C35 C36 1.399(8) . ? C35 H35A 0.9300 . ? C36 N2 1.340(7) . ? C36 H36A 0.9300 . ? C37 C38 1.509(9) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 O3 1.270(7) . ? C38 C39 1.379(9) . ? C39 C40 1.410(10) . ? C39 H39A 0.9300 . ? C40 O4 1.263(7) . ? C40 C41 1.513(9) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 Cl2 1.629(11) . ? C42 Cl1 1.706(11) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 Cl4 1.693(13) . ? C43 Cl3 1.729(14) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? Ir1 N1 2.033(4) . ? Ir1 N2 2.037(4) . ? Ir1 O3 2.144(4) . ? Ir1 O4 2.145(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 C13 C1 C2 117.7(4) . . ? C13 C1 Ir1 115.9(4) . . ? C2 C1 Ir1 126.3(4) . . ? C3 C2 C1 119.7(5) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C11 121.1(5) . . ? C2 C3 C4 129.8(5) . . ? C11 C3 C4 109.1(4) . . ? C5 C4 C9 120.9(6) . . ? C5 C4 C3 131.6(5) . . ? C9 C4 C3 107.5(5) . . ? C4 C5 C6 118.0(6) . . ? C4 C5 H5A 121.0 . . ? C6 C5 H5A 121.0 . . ? C7 C6 C5 122.2(7) . . ? C7 C6 H6A 118.9 . . ? C5 C6 H6A 118.9 . . ? C6 C7 C8 120.2(6) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C9 C8 C7 118.6(6) . . ? C9 C8 H8A 120.7 . . ? C7 C8 H8A 120.7 . . ? C8 C9 C4 120.1(6) . . ? C8 C9 C10 130.5(6) . . ? C4 C9 C10 109.4(5) . . ? O1 C10 C9 127.6(5) . . ? O1 C10 C11 127.3(6) . . ? C9 C10 C11 105.1(5) . . ? C12 C11 C3 121.6(5) . . ? C12 C11 C10 129.6(5) . . ? C3 C11 C10 108.8(5) . . ? C11 C12 C13 117.3(5) . . ? C11 C12 H12A 121.3 . . ? C13 C12 H12A 121.3 . . ? C12 C13 C1 122.6(5) . . ? C12 C13 C14 123.7(4) . . ? C1 C13 C14 113.7(4) . . ? N1 C14 C15 120.4(5) . . ? N1 C14 C13 113.5(4) . . ? C15 C14 C13 126.0(5) . . ? C16 C15 C14 119.9(5) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 119.8(5) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C18 C17 C16 117.7(6) . . ? C18 C17 H17A 121.1 . . ? C16 C17 H17A 121.1 . . ? N1 C18 C17 123.3(6) . . ? N1 C18 H18A 118.4 . . ? C17 C18 H18A 118.4 . . ? C20 C19 C31 117.5(4) . . ? C20 C19 Ir1 127.4(4) . . ? C31 C19 Ir1 115.1(3) . . ? C21 C20 C19 120.7(5) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C29 121.0(5) . . ? C20 C21 C22 131.0(5) . . ? C29 C21 C22 107.8(4) . . ? C23 C22 C27 120.3(5) . . ? C23 C22 C21 130.8(5) . . ? C27 C22 C21 108.9(5) . . ? C24 C23 C22 118.3(6) . . ? C24 C23 H23A 120.9 . . ? C22 C23 H23A 120.9 . . ? C23 C24 C25 121.3(6) . . ? C23 C24 H24A 119.4 . . ? C25 C24 H24A 119.4 . . ? C26 C25 C24 120.9(6) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C27 C26 C25 117.2(6) . . ? C27 C26 H26A 121.4 . . ? C25 C26 H26A 121.4 . . ? C26 C27 C22 122.0(6) . . ? C26 C27 C28 128.9(5) . . ? C22 C27 C28 108.9(5) . . ? O2 C28 C29 128.8(6) . . ? O2 C28 C27 126.3(6) . . ? C29 C28 C27 104.8(5) . . ? C30 C29 C21 120.5(5) . . ? C30 C29 C28 129.7(5) . . ? C21 C29 C28 109.7(5) . . ? C29 C30 C31 118.3(5) . . ? C29 C30 H30A 120.9 . . ? C31 C30 H30A 120.9 . . ? C30 C31 C19 122.0(5) . . ? C30 C31 C32 123.4(5) . . ? C19 C31 C32 114.6(4) . . ? N2 C32 C33 120.3(5) . . ? N2 C32 C31 113.4(4) . . ? C33 C32 C31 126.4(5) . . ? C34 C33 C32 120.2(6) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C33 C34 C35 119.6(6) . . ? C33 C34 H34A 120.2 . . ? C35 C34 H34A 120.2 . . ? C34 C35 C36 118.9(6) . . ? C34 C35 H35A 120.6 . . ? C36 C35 H35A 120.6 . . ? N2 C36 C35 121.8(6) . . ? N2 C36 H36A 119.1 . . ? C35 C36 H36A 119.1 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O3 C38 C39 126.6(6) . . ? O3 C38 C37 114.2(6) . . ? C39 C38 C37 119.1(6) . . ? C38 C39 C40 129.1(6) . . ? C38 C39 H39A 115.4 . . ? C40 C39 H39A 115.4 . . ? O4 C40 C39 125.9(6) . . ? O4 C40 C41 115.9(6) . . ? C39 C40 C41 118.1(6) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Cl2 C42 Cl1 117.4(7) . . ? Cl2 C42 H42A 108.0 . . ? Cl1 C42 H42A 108.0 . . ? Cl2 C42 H42B 108.0 . . ? Cl1 C42 H42B 108.0 . . ? H42A C42 H42B 107.2 . . ? Cl4 C43 Cl3 112.2(8) . . ? Cl4 C43 H43A 109.2 . . ? Cl3 C43 H43A 109.2 . . ? Cl4 C43 H43B 109.2 . . ? Cl3 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? C1 Ir1 C19 87.56(18) . . ? C1 Ir1 N1 80.03(19) . . ? C19 Ir1 N1 94.88(18) . . ? C1 Ir1 N2 94.36(18) . . ? C19 Ir1 N2 80.50(19) . . ? N1 Ir1 N2 172.94(15) . . ? C1 Ir1 O3 92.83(17) . . ? C19 Ir1 O3 176.75(15) . . ? N1 Ir1 O3 88.36(16) . . ? N2 Ir1 O3 96.25(16) . . ? C1 Ir1 O4 176.01(16) . . ? C19 Ir1 O4 91.11(17) . . ? N1 Ir1 O4 96.34(16) . . ? N2 Ir1 O4 89.12(16) . . ? O3 Ir1 O4 88.71(16) . . ? C18 N1 C14 118.8(4) . . ? C18 N1 Ir1 124.5(4) . . ? C14 N1 Ir1 116.5(3) . . ? C36 N2 C32 119.1(5) . . ? C36 N2 Ir1 124.3(4) . . ? C32 N2 Ir1 116.2(3) . . ? C38 O3 Ir1 124.5(4) . . ? C40 O4 Ir1 124.8(4) . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 2.234 _refine_diff_density_min -1.737 _refine_diff_density_rms 0.146