# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Lan-Chang Liang' _publ_contact_author_address ; Department of Chemistry National Sun Yat-sen University Kaohsiung 80424 TAIWAN ; _publ_contact_author_email LCLIANG@MAIL.NSYSU.EDU.TW _publ_section_title ; Benzene C-H Activation by Platinum(II) Complexes of Bis(2-diphenylphosphinophenyl)amide ; loop_ _publ_author_name 'Lan-Chang Liang' 'Wei-Ying Lee' 'Jia-Ming Lin' data_3465 _database_code_depnum_ccdc_archive 'CCDC 261442' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H41 F3 N2 O3 P2 Pt S' _chemical_formula_weight 1051.93 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' F F 0.0171 0.0103 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.1140(2) _cell_length_b 17.6950(3) _cell_length_c 16.9010(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.9800(10) _cell_angle_gamma 90.00 _cell_volume 4345.38(12) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 3.409 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32860 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7654 _reflns_number_gt 6260 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^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 SHELXL _refine_ls_extinction_coef 0.0076(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7654 _refine_ls_number_parameters 560 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.291269(15) 0.402435(14) 0.143938(14) 0.01842(14) Uani 1 1 d . . . S1 S 0.96137(13) 0.39700(10) 0.25383(13) 0.0311(5) Uani 1 1 d . . . P1 P 0.24357(11) 0.30569(10) 0.05167(10) 0.0206(4) Uani 1 1 d . . . P2 P 0.36852(11) 0.48143(10) 0.24568(10) 0.0191(4) Uani 1 1 d . . . F1 F 0.9942(4) 0.4740(3) 0.3913(3) 0.0651(16) Uani 1 1 d . . . F2 F 0.8639(3) 0.4168(3) 0.3591(4) 0.0569(15) Uani 1 1 d . . . F3 F 0.9878(4) 0.3545(3) 0.4070(3) 0.0591(14) Uani 1 1 d . . . O1 O 0.9205(4) 0.4628(3) 0.2101(4) 0.0495(16) Uani 1 1 d . . . O2 O 1.0587(4) 0.3903(3) 0.2669(4) 0.0467(16) Uani 1 1 d . . . O3 O 0.9099(4) 0.3283(3) 0.2294(4) 0.0459(15) Uani 1 1 d . . . N1 N 0.3998(3) 0.3338(3) 0.1924(3) 0.0214(12) Uani 1 1 d . . . N2 N 0.1879(4) 0.4791(3) 0.0971(3) 0.0218(12) Uani 1 1 d . . . C1 C 0.1284(4) 0.2666(4) 0.0360(4) 0.0217(14) Uani 1 1 d . . . C2 C 0.0875(5) 0.2719(4) 0.1006(4) 0.0246(15) Uani 1 1 d . . . H2 H 0.1188 0.2985 0.1499 0.030 Uiso 1 1 d R . . C3 C 0.0015(5) 0.2403(4) 0.0918(5) 0.0309(17) Uani 1 1 d . . . H3 H -0.0261 0.2425 0.1365 0.037 Uiso 1 1 d R . . C4 C -0.0429(5) 0.2041(4) 0.0193(5) 0.0309(16) Uani 1 1 d . . . H4 H -0.1028 0.1832 0.0145 0.037 Uiso 1 1 d R . . C5 C -0.0028(5) 0.1982(4) -0.0440(5) 0.0334(17) Uani 1 1 d . . . H5 H -0.0354 0.1727 -0.0937 0.040 Uiso 1 1 d R . . C6 C 0.0836(5) 0.2297(4) -0.0360(4) 0.0263(15) Uani 1 1 d . . . H6 H 0.1125 0.2258 -0.0798 0.032 Uiso 1 1 d R . . C7 C 0.2560(5) 0.3205(4) -0.0505(4) 0.0243(15) Uani 1 1 d . . . C8 C 0.2108(6) 0.3812(5) -0.0963(5) 0.044(2) Uani 1 1 d . . . H8 H 0.1724 0.4119 -0.0725 0.052 Uiso 1 1 d R . . C9 C 0.2198(8) 0.3973(5) -0.1739(6) 0.060(3) Uani 1 1 d . . . H9 H 0.1869 0.4393 -0.2041 0.072 Uiso 1 1 d R . . C10 C 0.2764(7) 0.3523(5) -0.2058(5) 0.049(2) Uani 1 1 d . . . H10 H 0.2848 0.3635 -0.2588 0.059 Uiso 1 1 d R . . C11 C 0.3211(5) 0.2913(4) -0.1622(4) 0.0328(17) Uani 1 1 d . . . H11 H 0.3595 0.2595 -0.1849 0.039 Uiso 1 1 d R . . C12 C 0.3106(5) 0.2751(4) -0.0845(4) 0.0268(16) Uani 1 1 d . . . H12 H 0.3413 0.2323 -0.0540 0.032 Uiso 1 1 d R . . C13 C 0.3229(4) 0.2332(4) 0.1034(4) 0.0203(14) Uani 1 1 d . . . C14 C 0.3114(5) 0.1571(4) 0.0801(4) 0.0267(16) Uani 1 1 d . . . H14 H 0.2620 0.1427 0.0333 0.032 Uiso 1 1 d R . . C15 C 0.3701(5) 0.1034(4) 0.1248(5) 0.0274(17) Uani 1 1 d . . . H15 H 0.3669 0.0516 0.1075 0.033 Uiso 1 1 d R . . C16 C 0.4370(5) 0.1258(4) 0.1968(4) 0.0271(15) Uani 1 1 d . . . H16 H 0.4751 0.0880 0.2304 0.033 Uiso 1 1 d R . . C17 C 0.4474(5) 0.1999(4) 0.2203(4) 0.0257(15) Uani 1 1 d . . . H17 H 0.4929 0.2143 0.2699 0.031 Uiso 1 1 d R . . C18 C 0.3923(4) 0.2570(4) 0.1721(4) 0.0203(14) Uani 1 1 d . . . C19 C 0.4837(4) 0.3679(4) 0.2333(4) 0.0237(15) Uani 1 1 d . . . C20 C 0.5712(4) 0.3349(4) 0.2438(4) 0.0254(16) Uani 1 1 d . . . H20 H 0.5746 0.2840 0.2252 0.031 Uiso 1 1 d R . . C21 C 0.6501(5) 0.3742(4) 0.2795(4) 0.0279(16) Uani 1 1 d . . . H21 H 0.7089 0.3506 0.2862 0.034 Uiso 1 1 d R . . C22 C 0.6474(4) 0.4485(4) 0.3069(4) 0.0287(17) Uani 1 1 d . . . H22 H 0.7030 0.4759 0.3316 0.034 Uiso 1 1 d R . . C23 C 0.5634(5) 0.4823(4) 0.2989(4) 0.0268(16) Uani 1 1 d . . . H23 H 0.5599 0.5331 0.3175 0.032 Uiso 1 1 d R . . C24 C 0.4822(4) 0.4430(4) 0.2623(4) 0.0205(14) Uani 1 1 d . . . C25 C 0.3394(4) 0.4761(4) 0.3426(4) 0.0201(14) Uani 1 1 d . . . C26 C 0.2701(4) 0.4267(4) 0.3518(4) 0.0232(15) Uani 1 1 d . . . H26 H 0.2372 0.3960 0.3063 0.028 Uiso 1 1 d R . . C27 C 0.2494(5) 0.4220(4) 0.4258(4) 0.0265(16) Uani 1 1 d . . . H27 H 0.2008 0.3894 0.4315 0.032 Uiso 1 1 d R . . C28 C 0.2981(5) 0.4647(4) 0.4920(4) 0.0268(16) Uani 1 1 d . . . H28 H 0.2837 0.4601 0.5437 0.032 Uiso 1 1 d R . . C29 C 0.3666(4) 0.5147(4) 0.4839(4) 0.0254(15) Uani 1 1 d . . . H29 H 0.3998 0.5449 0.5297 0.030 Uiso 1 1 d R . . C30 C 0.3871(4) 0.5205(4) 0.4100(4) 0.0217(14) Uani 1 1 d . . . H30 H 0.4342 0.5545 0.4038 0.026 Uiso 1 1 d R . . C31 C 0.3648(5) 0.5812(4) 0.2201(4) 0.0226(15) Uani 1 1 d . . . C32 C 0.4235(5) 0.6124(4) 0.1779(4) 0.0292(17) Uani 1 1 d . . . H32 H 0.4718 0.5816 0.1682 0.035 Uiso 1 1 d R . . C33 C 0.4133(6) 0.6855(5) 0.1520(5) 0.0368(19) Uani 1 1 d . . . H33 H 0.4551 0.7064 0.1242 0.044 Uiso 1 1 d R . . C34 C 0.3433(6) 0.7288(4) 0.1666(5) 0.0378(19) Uani 1 1 d . . . H34 H 0.3355 0.7799 0.1471 0.045 Uiso 1 1 d R . . C35 C 0.2845(5) 0.6990(4) 0.2076(4) 0.0306(16) Uani 1 1 d . . . H35 H 0.2367 0.7295 0.2185 0.037 Uiso 1 1 d R . . C36 C 0.2946(5) 0.6252(4) 0.2343(4) 0.0280(15) Uani 1 1 d . . . H36 H 0.2529 0.6037 0.2618 0.034 Uiso 1 1 d R . . C37 C 0.2017(5) 0.5343(4) 0.0452(4) 0.0277(16) Uani 1 1 d . . . H37 H 0.2566 0.5334 0.0272 0.033 Uiso 1 1 d R . . C38 C 0.1400(5) 0.5916(4) 0.0187(5) 0.0313(18) Uani 1 1 d . . . H38 H 0.1496 0.6285 -0.0199 0.038 Uiso 1 1 d R . . C39 C 0.0620(5) 0.5955(4) 0.0471(5) 0.0285(17) Uani 1 1 d . . . H39 H 0.0189 0.6362 0.0298 0.034 Uiso 1 1 d R . . C40 C 0.0485(5) 0.5400(4) 0.1007(4) 0.0277(16) Uani 1 1 d . . . H40 H -0.0044 0.5412 0.1216 0.033 Uiso 1 1 d R . . C41 C 0.1126(4) 0.4834(4) 0.1245(4) 0.0247(15) Uani 1 1 d . . . H41 H 0.1018 0.4455 0.1613 0.030 Uiso 1 1 d R . . C42 C 0.9514(5) 0.4124(4) 0.3578(5) 0.037(2) Uani 1 1 d . . . C43 C 0.1415(12) 0.3433(13) 0.5881(12) 0.068(5) Uani 0.55 1 d P . . H44A H 0.1024 0.0510 0.5615 0.080 Uiso 0.45 1 d P . . C43' C 0.082(3) 0.0332(14) 0.5670(17) 0.109(13) Uani 0.45 1 d P . . H47A H 0.1450 0.3143 0.5834 0.080 Uiso 0.55 1 d P . . C44 C 0.1117(9) 0.1042(9) 0.5658(7) 0.086(5) Uani 1 1 d . . . C45 C 0.1950(7) 0.1322(9) 0.5959(5) 0.076(4) Uani 1 1 d . . . H45 H 0.2467 0.0991 0.6159 0.091 Uiso 1 1 d R . . C46 C 0.2088(7) 0.2154(9) 0.5988(7) 0.081(4) Uani 1 1 d . . . H46 H 0.2699 0.2359 0.6161 0.098 Uiso 1 1 d R . . C47 C 0.1370(8) 0.2611(8) 0.5782(6) 0.077(4) Uani 1 1 d . . . C48 C 0.0475(7) 0.2295(10) 0.5482(6) 0.081(4) Uani 1 1 d . . . H48 H -0.0059 0.2614 0.5330 0.097 Uiso 1 1 d R . . C49 C 0.0361(7) 0.1549(10) 0.5406(6) 0.074(4) Uani 1 1 d . . . H49 H -0.0256 0.1377 0.5161 0.089 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01740(19) 0.0173(2) 0.01941(19) -0.00042(10) 0.00313(12) 0.00216(9) S1 0.0223(9) 0.0277(11) 0.0421(11) 0.0093(8) 0.0070(8) -0.0016(7) P1 0.0192(8) 0.0206(10) 0.0205(8) -0.0023(7) 0.0029(7) 0.0030(7) P2 0.0196(8) 0.0171(9) 0.0201(8) 0.0006(7) 0.0044(7) 0.0013(7) F1 0.071(4) 0.057(4) 0.070(4) -0.013(3) 0.025(3) -0.039(3) F2 0.027(2) 0.073(4) 0.076(4) -0.020(3) 0.021(3) -0.006(2) F3 0.063(3) 0.067(4) 0.052(3) 0.025(3) 0.023(3) 0.010(3) O1 0.042(3) 0.037(4) 0.063(4) 0.020(3) 0.005(3) 0.006(3) O2 0.021(3) 0.070(4) 0.050(4) 0.025(3) 0.012(3) 0.005(3) O3 0.052(3) 0.037(4) 0.056(4) -0.004(3) 0.027(3) -0.015(3) N1 0.020(3) 0.025(3) 0.017(3) 0.000(2) 0.000(2) 0.005(2) N2 0.024(3) 0.021(3) 0.021(3) 0.002(2) 0.006(2) 0.001(2) C1 0.023(3) 0.012(3) 0.026(3) 0.002(3) 0.002(3) 0.005(3) C2 0.029(4) 0.019(4) 0.026(3) 0.001(3) 0.007(3) -0.003(3) C3 0.031(4) 0.026(4) 0.038(4) 0.005(3) 0.012(3) 0.000(3) C4 0.023(4) 0.020(4) 0.046(4) -0.001(3) 0.003(3) -0.003(3) C5 0.033(4) 0.027(4) 0.035(4) -0.012(3) -0.001(3) 0.000(3) C6 0.028(4) 0.024(4) 0.025(4) -0.004(3) 0.004(3) 0.003(3) C7 0.027(3) 0.025(4) 0.023(3) -0.003(3) 0.009(3) -0.001(3) C8 0.057(5) 0.043(5) 0.034(4) 0.004(4) 0.020(4) 0.023(4) C9 0.091(8) 0.055(7) 0.040(5) 0.017(4) 0.032(6) 0.038(5) C10 0.081(6) 0.036(5) 0.041(5) 0.013(4) 0.037(5) 0.017(5) C11 0.040(4) 0.029(4) 0.036(4) -0.008(3) 0.021(3) 0.004(3) C12 0.025(4) 0.025(4) 0.030(4) -0.001(3) 0.007(3) 0.003(3) C13 0.022(3) 0.013(4) 0.027(3) 0.000(3) 0.008(3) 0.003(3) C14 0.025(3) 0.022(4) 0.032(4) -0.002(3) 0.008(3) 0.000(3) C15 0.023(4) 0.016(4) 0.039(4) -0.003(3) 0.003(3) 0.005(3) C16 0.031(4) 0.018(4) 0.032(4) -0.001(3) 0.008(3) 0.003(3) C17 0.026(3) 0.031(4) 0.022(3) 0.002(3) 0.008(3) 0.006(3) C18 0.019(3) 0.016(4) 0.029(3) -0.002(3) 0.011(3) 0.003(3) C19 0.021(3) 0.033(4) 0.014(3) -0.001(3) 0.002(3) 0.003(3) C20 0.021(3) 0.032(4) 0.023(3) 0.000(3) 0.005(3) 0.009(3) C21 0.021(4) 0.035(4) 0.024(4) 0.000(3) 0.001(3) 0.008(3) C22 0.015(3) 0.040(5) 0.029(4) -0.004(3) 0.002(3) -0.002(3) C23 0.029(4) 0.031(4) 0.018(3) -0.005(3) 0.002(3) -0.004(3) C24 0.018(3) 0.025(4) 0.018(3) 0.000(3) 0.004(3) 0.001(3) C25 0.023(3) 0.018(4) 0.018(3) 0.002(3) 0.004(3) 0.005(3) C26 0.019(3) 0.021(4) 0.030(4) 0.000(3) 0.009(3) 0.002(3) C27 0.024(4) 0.025(4) 0.029(4) -0.002(3) 0.005(3) -0.002(3) C28 0.032(4) 0.028(4) 0.021(3) 0.002(3) 0.007(3) 0.005(3) C29 0.026(4) 0.025(4) 0.021(3) -0.004(3) 0.002(3) 0.000(3) C30 0.019(3) 0.017(4) 0.027(3) 0.003(3) 0.004(3) -0.001(3) C31 0.022(3) 0.025(4) 0.018(3) -0.004(3) 0.001(3) -0.003(3) C32 0.036(4) 0.027(4) 0.028(4) -0.005(3) 0.013(3) -0.002(3) C33 0.048(5) 0.029(5) 0.040(4) 0.002(4) 0.023(4) -0.001(4) C34 0.054(5) 0.023(4) 0.035(4) 0.009(3) 0.011(4) 0.000(4) C35 0.037(4) 0.024(4) 0.028(4) -0.001(3) 0.005(3) 0.005(3) C36 0.029(4) 0.026(4) 0.027(4) -0.007(3) 0.004(3) -0.005(3) C37 0.021(3) 0.030(4) 0.031(4) 0.002(3) 0.007(3) 0.003(3) C38 0.035(4) 0.030(5) 0.030(4) 0.011(3) 0.011(4) 0.007(3) C39 0.028(4) 0.025(4) 0.031(4) 0.004(3) 0.005(3) 0.009(3) C40 0.020(3) 0.032(4) 0.029(4) -0.001(3) 0.005(3) 0.003(3) C41 0.024(3) 0.023(4) 0.027(3) -0.002(3) 0.007(3) -0.002(3) C42 0.025(4) 0.032(5) 0.055(5) -0.001(4) 0.010(4) -0.012(3) C43 0.055(11) 0.071(15) 0.068(12) 0.013(11) 0.001(9) -0.023(10) C43' 0.27(4) 0.026(13) 0.075(17) 0.004(12) 0.12(2) -0.007(19) C44 0.062(8) 0.158(16) 0.041(6) -0.025(7) 0.020(6) -0.002(8) C45 0.039(6) 0.163(13) 0.029(5) -0.011(7) 0.015(4) 0.024(7) C46 0.042(6) 0.131(13) 0.072(7) -0.032(8) 0.018(5) 0.005(7) C47 0.063(7) 0.128(12) 0.042(6) -0.002(6) 0.018(5) 0.000(7) C48 0.045(6) 0.159(15) 0.038(6) 0.013(7) 0.010(5) 0.011(8) C49 0.047(6) 0.141(13) 0.031(5) 0.005(7) 0.006(4) 0.033(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.025(5) . ? Pt1 N2 2.056(5) . ? Pt1 P2 2.2735(17) . ? Pt1 P1 2.2941(17) . ? S1 O1 1.426(6) . ? S1 O2 1.431(6) . ? S1 O3 1.442(6) . ? S1 C42 1.825(9) . ? P1 C7 1.807(6) . ? P1 C13 1.808(6) . ? P1 C1 1.823(7) . ? P2 C24 1.797(6) . ? P2 C25 1.811(6) . ? P2 C31 1.815(7) . ? F1 C42 1.313(9) . ? F2 C42 1.331(9) . ? F3 C42 1.340(10) . ? N1 C18 1.398(8) . ? N1 C19 1.402(8) . ? N2 C41 1.344(8) . ? N2 C37 1.366(9) . ? C1 C6 1.383(9) . ? C1 C2 1.399(9) . ? C2 C3 1.384(10) . ? C2 H2 0.9605 . ? C3 C4 1.383(10) . ? C3 H3 0.9591 . ? C4 C5 1.371(10) . ? C4 H4 0.9605 . ? C5 C6 1.392(10) . ? C5 H5 0.9613 . ? C6 H6 0.9600 . ? C7 C12 1.385(9) . ? C7 C8 1.388(11) . ? C8 C9 1.385(13) . ? C8 H8 0.9604 . ? C9 C10 1.382(12) . ? C9 H9 0.9594 . ? C10 C11 1.376(11) . ? C10 H10 0.9594 . ? C11 C12 1.395(10) . ? C11 H11 0.9609 . ? C12 H12 0.9607 . ? C13 C18 1.398(9) . ? C13 C14 1.401(9) . ? C14 C15 1.375(10) . ? C14 H14 0.9607 . ? C15 C16 1.407(10) . ? C15 H15 0.9593 . ? C16 C17 1.367(10) . ? C16 H16 0.9599 . ? C17 C18 1.415(9) . ? C17 H17 0.9608 . ? C19 C20 1.411(9) . ? C19 C24 1.419(10) . ? C20 C21 1.370(10) . ? C20 H20 0.9600 . ? C21 C22 1.398(11) . ? C21 H21 0.9600 . ? C22 C23 1.377(10) . ? C22 H22 0.9604 . ? C23 C24 1.398(9) . ? C23 H23 0.9585 . ? C25 C26 1.405(9) . ? C25 C30 1.408(9) . ? C26 C27 1.374(9) . ? C26 H26 0.9608 . ? C27 C28 1.381(10) . ? C27 H27 0.9594 . ? C28 C29 1.398(10) . ? C28 H28 0.9603 . ? C29 C30 1.370(9) . ? C29 H29 0.9606 . ? C30 H30 0.9596 . ? C31 C36 1.390(10) . ? C31 C32 1.396(10) . ? C32 C33 1.360(11) . ? C32 H32 0.9606 . ? C33 C34 1.382(11) . ? C33 H33 0.9592 . ? C34 C35 1.374(10) . ? C34 H34 0.9585 . ? C35 C36 1.375(10) . ? C35 H35 0.9594 . ? C36 H36 0.9588 . ? C37 C38 1.368(10) . ? C37 H37 0.9593 . ? C38 C39 1.392(10) . ? C38 H38 0.9618 . ? C39 C40 1.388(10) . ? C39 H39 0.9611 . ? C40 C41 1.374(10) . ? C40 H40 0.9592 . ? C41 H41 0.9587 . ? C43 C47 1.46(2) . ? C43 H47A 0.52(2) . ? C43' C44 1.34(3) . ? C43' H44A 0.47(3) . ? C44 C45 1.318(17) . ? C44 C49 1.423(17) . ? C44 H44A 0.952(15) . ? C45 C46 1.486(18) . ? C45 H45 0.9604 . ? C46 C47 1.320(16) . ? C46 H46 0.9598 . ? C47 C48 1.422(16) . ? C47 H47A 0.949(15) . ? C48 C49 1.333(18) . ? C48 H48 0.9601 . ? C49 H49 0.9597 . ? 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 Pt1 N2 175.6(2) . . ? N1 Pt1 P2 82.68(16) . . ? N2 Pt1 P2 93.60(16) . . ? N1 Pt1 P1 84.00(16) . . ? N2 Pt1 P1 99.65(15) . . ? P2 Pt1 P1 166.60(6) . . ? O1 S1 O2 115.3(3) . . ? O1 S1 O3 114.8(4) . . ? O2 S1 O3 115.1(4) . . ? O1 S1 C42 103.8(4) . . ? O2 S1 C42 102.6(4) . . ? O3 S1 C42 102.8(3) . . ? C7 P1 C13 109.6(3) . . ? C7 P1 C1 105.2(3) . . ? C13 P1 C1 106.3(3) . . ? C7 P1 Pt1 116.5(2) . . ? C13 P1 Pt1 99.1(2) . . ? C1 P1 Pt1 119.4(2) . . ? C24 P2 C25 107.4(3) . . ? C24 P2 C31 111.8(3) . . ? C25 P2 C31 105.5(3) . . ? C24 P2 Pt1 98.9(2) . . ? C25 P2 Pt1 116.7(2) . . ? C31 P2 Pt1 116.3(2) . . ? C18 N1 C19 122.7(5) . . ? C18 N1 Pt1 118.8(4) . . ? C19 N1 Pt1 117.6(4) . . ? C41 N2 C37 118.3(6) . . ? C41 N2 Pt1 122.1(4) . . ? C37 N2 Pt1 119.0(4) . . ? C6 C1 C2 120.3(6) . . ? C6 C1 P1 121.6(5) . . ? C2 C1 P1 118.1(5) . . ? C3 C2 C1 119.5(7) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 119.7(7) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 121.1(7) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 118.0 . . ? C4 C5 C6 119.9(7) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 121.0 . . ? C1 C6 C5 119.6(6) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 120.7 . . ? C12 C7 C8 118.4(6) . . ? C12 C7 P1 122.8(5) . . ? C8 C7 P1 118.7(5) . . ? C9 C8 C7 121.8(7) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 117.7 . . ? C10 C9 C8 118.9(8) . . ? C10 C9 H9 121.7 . . ? C8 C9 H9 119.5 . . ? C11 C10 C9 120.6(7) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0(6) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 119.6 . . ? C7 C12 C11 120.4(7) . . ? C7 C12 H12 119.4 . . ? C11 C12 H12 120.2 . . ? C18 C13 C14 122.0(6) . . ? C18 C13 P1 115.7(5) . . ? C14 C13 P1 122.1(5) . . ? C15 C14 C13 119.9(6) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 118.8(6) . . ? C14 C15 H15 121.4 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 121.2(7) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 121.1(6) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 118.6 . . ? N1 C18 C13 119.2(6) . . ? N1 C18 C17 123.9(6) . . ? C13 C18 C17 116.8(6) . . ? N1 C19 C20 125.0(6) . . ? N1 C19 C24 118.4(5) . . ? C20 C19 C24 116.5(6) . . ? C21 C20 C19 121.2(7) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 118.7 . . ? C20 C21 C22 121.5(6) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 118.7 . . ? C23 C22 C21 119.1(6) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 121.1 . . ? C22 C23 C24 120.0(7) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 119.4 . . ? C23 C24 C19 121.6(6) . . ? C23 C24 P2 124.5(5) . . ? C19 C24 P2 113.9(4) . . ? C26 C25 C30 119.3(6) . . ? C26 C25 P2 120.4(5) . . ? C30 C25 P2 120.3(5) . . ? C27 C26 C25 120.1(6) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.0(7) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 119.9 . . ? C27 C28 C29 120.7(6) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 119.7(6) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 120.7 . . ? C29 C30 C25 120.1(6) . . ? C29 C30 H30 120.4 . . ? C25 C30 H30 119.4 . . ? C36 C31 C32 119.3(7) . . ? C36 C31 P2 118.7(5) . . ? C32 C31 P2 121.6(5) . . ? C33 C32 C31 120.6(7) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 118.8 . . ? C32 C33 C34 119.6(7) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 120.9 . . ? C35 C34 C33 120.7(7) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 119.3 . . ? C34 C35 C36 120.1(7) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 119.7(7) . . ? C35 C36 H36 120.5 . . ? C31 C36 H36 119.8 . . ? N2 C37 C38 122.0(6) . . ? N2 C37 H37 119.3 . . ? C38 C37 H37 118.7 . . ? C37 C38 C39 119.3(7) . . ? C37 C38 H38 120.6 . . ? C39 C38 H38 120.1 . . ? C40 C39 C38 118.8(6) . . ? C40 C39 H39 121.3 . . ? C38 C39 H39 119.9 . . ? C41 C40 C39 119.2(6) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.8 . . ? N2 C41 C40 122.5(6) . . ? N2 C41 H41 119.7 . . ? C40 C41 H41 117.8 . . ? F1 C42 F2 108.6(7) . . ? F1 C42 F3 107.3(7) . . ? F2 C42 F3 106.0(6) . . ? F1 C42 S1 112.2(5) . . ? F2 C42 S1 111.8(6) . . ? F3 C42 S1 110.8(6) . . ? C47 C43 H47A 9.3(13) . . ? C44 C43' H44A 29(2) . . ? C45 C44 C43' 130(2) . . ? C45 C44 C49 118.8(15) . . ? C43' C44 C49 110(2) . . ? C45 C44 H44A 120.4(14) . . ? C43' C44 H44A 13.8(14) . . ? C49 C44 H44A 120.8(13) . . ? C44 C45 C46 119.7(12) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.0 . . ? C47 C46 C45 120.0(11) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 119.9 . . ? C46 C47 C48 119.0(14) . . ? C46 C47 C43 124.7(13) . . ? C48 C47 C43 116.2(14) . . ? C46 C47 H47A 120.5(13) . . ? C48 C47 H47A 120.4(13) . . ? C43 C47 H47A 5.1(8) . . ? C49 C48 C47 120.6(13) . . ? C49 C48 H48 118.6 . . ? C47 C48 H48 120.8 . . ? C48 C49 C44 121.5(13) . . ? C48 C49 H49 116.2 . . ? C44 C49 H49 122.3 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.573 _refine_diff_density_min -1.605 _refine_diff_density_rms 0.411 data_2861 _database_code_depnum_ccdc_archive 'CCDC 261443' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H31 N1 P2 Pt1' _chemical_formula_sum 'C37 H31 N P2 Pt' _chemical_formula_weight 746.66 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 orthorhombic _symmetry_space_group_name_H-M 'F 2 d d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' 'x+1/4, -y+1/4, z+1/4' 'x+1/4, y+1/4, -z+1/4' 'x, y+1/2, z+1/2' 'x, -y+1/2, -z+1/2' 'x+1/4, -y+3/4, z+3/4' 'x+1/4, y+3/4, -z+3/4' 'x+1/2, y, z+1/2' 'x+1/2, -y, -z+1/2' 'x+3/4, -y+1/4, z+3/4' 'x+3/4, y+1/4, -z+3/4' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' 'x+3/4, -y+3/4, z+1/4' 'x+3/4, y+3/4, -z+1/4' _cell_length_a 9.9610(2) _cell_length_b 18.6010(4) _cell_length_c 32.7250(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6063.4(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13597 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 4.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.32 _exptl_absorpt_correction_T_max 0.5427 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7661 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2559 _reflns_number_gt 2334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0910P)^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 fixed _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 0.295(18) _refine_ls_number_reflns 2559 _refine_ls_number_parameters 187 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.73210(13) 0.0000 0.0000 0.03912(17) Uani 1 2 d S . . P1 P 0.7016(2) 0.07046(10) 0.05601(5) 0.0393(4) Uani 1 1 d . . . N1 N 0.522(2) 0.0000 0.0000 0.046(6) Uani 1 2 d S . . C1 C 0.944(3) 0.0000 0.0000 0.059(9) Uani 1 2 d S . . C2 C 0.4555(10) 0.0146(4) 0.0363(3) 0.042(2) Uani 1 1 d . . . C3 C 0.3219(12) -0.0047(4) 0.0465(4) 0.056(3) Uani 1 1 d . . . H3 H 0.2680 -0.0286 0.0264 0.068 Uiso 1 1 d R . . C4 C 0.2670(12) 0.0110(6) 0.0841(4) 0.064(3) Uani 1 1 d . . . H4 H 0.1786 -0.0048 0.0915 0.077 Uiso 1 1 d R . . C5 C 0.3363(11) 0.0457(6) 0.1133(3) 0.060(3) Uani 1 1 d . . . H5 H 0.2955 0.0592 0.1387 0.072 Uiso 1 1 d R . . C6 C 0.4705(10) 0.0645(4) 0.1060(2) 0.050(2) Uani 1 1 d . . . H6 H 0.5229 0.0884 0.1265 0.060 Uiso 1 1 d R . . C7 C 0.5285(8) 0.0485(4) 0.0681(2) 0.0384(18) Uani 1 1 d . . . C8 C 0.6961(10) 0.1666(4) 0.0462(2) 0.0401(18) Uani 1 1 d . . . C9 C 0.5777(11) 0.2001(5) 0.0359(3) 0.053(2) Uani 1 1 d . . . H9 H 0.4954 0.1732 0.0355 0.064 Uiso 1 1 d R . . C10 C 0.5771(15) 0.2727(6) 0.0265(4) 0.068(3) Uani 1 1 d . . . H10 H 0.4922 0.2951 0.0208 0.081 Uiso 1 1 d R . . C11 C 0.6896(15) 0.3121(5) 0.0264(3) 0.067(3) Uani 1 1 d . . . H11 H 0.6898 0.3614 0.0177 0.081 Uiso 1 1 d R . . C12 C 0.8073(14) 0.2810(6) 0.0376(3) 0.066(3) Uani 1 1 d . . . H12 H 0.8860 0.3108 0.0382 0.079 Uiso 1 1 d R . . C13 C 0.8141(12) 0.2084(6) 0.0476(3) 0.059(3) Uani 1 1 d . . . H13 H 0.8973 0.1869 0.0560 0.071 Uiso 1 1 d R . . C14 C 0.7978(9) 0.0591(5) 0.1024(3) 0.045(2) Uani 1 1 d . . . C15 C 0.8083(10) 0.1123(5) 0.1326(3) 0.052(2) Uani 1 1 d . . . H15 H 0.7671 0.1583 0.1285 0.062 Uiso 1 1 d R . . C16 C 0.8765(10) 0.1002(5) 0.1677(3) 0.055(2) Uani 1 1 d . . . H16 H 0.8784 0.1365 0.1886 0.066 Uiso 1 1 d R . . C17 C 0.9404(11) 0.0346(6) 0.1742(3) 0.063(3) Uani 1 1 d . . . H17 H 0.9958 0.0277 0.1978 0.076 Uiso 1 1 d R . . C18 C 0.9317(12) -0.0191(7) 0.1454(4) 0.065(3) Uani 1 1 d . . . H18 H 0.9663 -0.0664 0.1504 0.078 Uiso 1 1 d R . . C19 C 0.8633(12) -0.0065(5) 0.1093(4) 0.055(3) Uani 1 1 d . . . H19 H 0.8638 -0.0425 0.0882 0.066 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0361(2) 0.0486(2) 0.0326(2) -0.00564(19) 0.000 0.000 P1 0.0427(11) 0.0441(10) 0.0313(9) -0.0024(8) -0.0002(9) -0.0026(10) N1 0.040(14) 0.066(14) 0.031(11) -0.007(4) 0.000 0.000 C1 0.030(16) 0.08(2) 0.07(2) -0.015(6) 0.000 0.000 C2 0.038(5) 0.035(3) 0.053(6) -0.004(4) 0.005(4) 0.001(4) C3 0.045(7) 0.066(7) 0.059(7) -0.006(4) 0.009(5) -0.008(4) C4 0.051(9) 0.076(8) 0.065(7) 0.004(5) 0.015(5) 0.000(5) C5 0.063(7) 0.076(7) 0.042(5) 0.004(5) 0.016(5) 0.013(5) C6 0.058(6) 0.051(4) 0.042(4) 0.002(4) 0.004(5) -0.004(5) C7 0.036(5) 0.039(4) 0.040(4) -0.004(3) 0.002(3) 0.005(3) C8 0.051(5) 0.043(4) 0.026(4) 0.000(3) 0.001(4) -0.006(4) C9 0.068(7) 0.044(5) 0.048(5) 0.003(4) -0.007(5) -0.007(5) C10 0.093(9) 0.053(5) 0.057(7) 0.007(5) -0.018(6) 0.003(6) C11 0.094(9) 0.050(5) 0.057(6) 0.003(5) -0.009(6) -0.023(6) C12 0.085(9) 0.058(6) 0.055(6) 0.004(5) 0.002(6) -0.031(7) C13 0.065(7) 0.065(6) 0.048(6) 0.008(5) -0.011(5) -0.024(5) C14 0.044(5) 0.049(5) 0.042(5) 0.004(4) 0.003(4) -0.006(4) C15 0.065(6) 0.050(5) 0.041(5) -0.008(4) -0.006(4) 0.002(4) C16 0.066(6) 0.060(6) 0.037(5) -0.006(4) -0.014(4) -0.016(5) C17 0.055(6) 0.096(7) 0.039(5) 0.008(5) -0.004(5) -0.004(6) C18 0.062(7) 0.071(5) 0.061(7) 0.014(6) -0.011(6) 0.018(6) C19 0.051(7) 0.063(6) 0.050(6) -0.005(4) 0.000(5) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.09(2) . ? Pt1 C1 2.11(3) . ? Pt1 P1 2.2737(18) 2 ? Pt1 P1 2.2737(18) . ? P1 C14 1.807(9) . ? P1 C7 1.816(8) . ? P1 C8 1.818(8) . ? N1 C2 1.389(15) . ? N1 C2 1.389(15) 2 ? C2 C7 1.418(12) . ? C2 C3 1.418(15) . ? C3 C4 1.378(19) . ? C3 H3 0.9586 . ? C4 C5 1.344(17) . ? C4 H4 0.9594 . ? C5 C6 1.403(16) . ? C5 H5 0.9587 . ? C6 C7 1.399(11) . ? C6 H6 0.9599 . ? C8 C9 1.375(14) . ? C8 C13 1.410(14) . ? C9 C10 1.385(15) . ? C9 H9 0.9605 . ? C10 C11 1.339(18) . ? C10 H10 0.9611 . ? C11 C12 1.358(19) . ? C11 H11 0.9600 . ? C12 C13 1.391(19) . ? C12 H12 0.9603 . ? C13 H13 0.9604 . ? C14 C19 1.402(13) . ? C14 C15 1.405(12) . ? C15 C16 1.354(12) . ? C15 H15 0.9581 . ? C16 C17 1.392(15) . ? C16 H16 0.9613 . ? C17 C18 1.375(17) . ? C17 H17 0.9576 . ? C18 C19 1.383(17) . ? C18 H18 0.9591 . ? C19 H19 0.9619 . ? 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 Pt1 C1 180.0 . . ? N1 Pt1 P1 82.31(7) . 2 ? C1 Pt1 P1 97.69(7) . 2 ? N1 Pt1 P1 82.31(7) . . ? C1 Pt1 P1 97.69(7) . . ? P1 Pt1 P1 164.63(13) 2 . ? C14 P1 C7 107.1(4) . . ? C14 P1 C8 106.2(4) . . ? C7 P1 C8 103.4(4) . . ? C14 P1 Pt1 122.6(3) . . ? C7 P1 Pt1 100.0(3) . . ? C8 P1 Pt1 115.3(2) . . ? C2 N1 C2 123(2) . 2 ? C2 N1 Pt1 118.6(10) . . ? C2 N1 Pt1 118.6(10) 2 . ? N1 C2 C7 118.0(12) . . ? N1 C2 C3 126.9(12) . . ? C7 C2 C3 114.9(9) . . ? C4 C3 C2 121.9(11) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 118.8 . . ? C5 C4 C3 122.2(11) . . ? C5 C4 H4 116.1 . . ? C3 C4 H4 121.6 . . ? C4 C5 C6 119.2(9) . . ? C4 C5 H5 121.6 . . ? C6 C5 H5 119.1 . . ? C5 C6 C7 119.4(9) . . ? C5 C6 H6 121.0 . . ? C7 C6 H6 119.6 . . ? C6 C7 C2 122.2(8) . . ? C6 C7 P1 122.5(6) . . ? C2 C7 P1 115.3(6) . . ? C9 C8 C13 118.3(8) . . ? C9 C8 P1 120.9(7) . . ? C13 C8 P1 120.7(8) . . ? C8 C9 C10 119.9(10) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 122.1(11) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 118.0 . . ? C10 C11 C12 119.2(10) . . ? C10 C11 H11 121.8 . . ? C12 C11 H11 119.0 . . ? C11 C12 C13 121.3(10) . . ? C11 C12 H12 117.7 . . ? C13 C12 H12 121.0 . . ? C12 C13 C8 119.1(10) . . ? C12 C13 H13 120.9 . . ? C8 C13 H13 120.0 . . ? C19 C14 C15 117.6(9) . . ? C19 C14 P1 119.0(7) . . ? C15 C14 P1 123.3(7) . . ? C16 C15 C14 121.2(9) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.3(8) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 120.2(10) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 119.5(10) . . ? C17 C18 H18 121.7 . . ? C19 C18 H18 118.6 . . ? C18 C19 C14 121.0(10) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.4 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.698 _refine_diff_density_min -1.607 _refine_diff_density_rms 0.334 data_3256 _database_code_depnum_ccdc_archive 'CCDC 261444' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H58 Cl1 N1 P2 Pt1' _chemical_formula_sum 'C66 H58 Cl N P2 Pt' _chemical_formula_weight 1157.61 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' 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.3780(5) _cell_length_b 12.7050(4) _cell_length_c 25.5550(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.5820(10) _cell_angle_gamma 90.00 _cell_volume 5460.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 62886 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 2.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3757 _exptl_absorpt_correction_T_max 0.6606 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21551 _diffrn_reflns_av_R_equivalents 0.1316 _diffrn_reflns_av_sigmaI/netI 0.0944 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 24.96 _reflns_number_total 9430 _reflns_number_gt 7957 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1576P)^2^+13.6693P] 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 SHELXL _refine_ls_extinction_coef 0.0025(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9430 _refine_ls_number_parameters 641 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.2174 _refine_ls_wR_factor_gt 0.2004 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.584452(17) 0.11500(2) 0.170035(11) 0.02456(19) Uani 1 1 d . . . Cl1 Cl 0.46150(12) 0.18831(18) 0.16769(9) 0.0366(5) Uani 1 1 d . . . P1 P 0.58639(12) -0.00948(17) 0.23486(8) 0.0260(5) Uani 1 1 d . . . P2 P 0.60957(12) 0.22423(17) 0.10602(8) 0.0263(5) Uani 1 1 d . . . N1 N 0.6905(4) 0.0510(5) 0.1685(3) 0.0266(15) Uani 1 1 d . . . C1 C 0.6081(5) 0.0366(7) 0.3043(3) 0.0296(18) Uani 1 1 d . . . C2 C 0.5481(6) 0.0946(8) 0.3185(4) 0.036(2) Uani 1 1 d . . . H2 H 0.4991 0.1075 0.2920 0.043 Uiso 1 1 d R . . C3 C 0.5600(6) 0.1316(8) 0.3707(4) 0.038(2) Uani 1 1 d . . . H3 H 0.5181 0.1696 0.3806 0.045 Uiso 1 1 d R . . C4 C 0.6325(6) 0.1135(7) 0.4087(4) 0.036(2) Uani 1 1 d . . . H4 H 0.6415 0.1399 0.4449 0.043 Uiso 1 1 d R . . C5 C 0.6914(5) 0.0574(7) 0.3939(3) 0.0322(19) Uani 1 1 d . . . H5 H 0.7411 0.0459 0.4200 0.039 Uiso 1 1 d R . . C6 C 0.6801(5) 0.0182(7) 0.3416(4) 0.0334(19) Uani 1 1 d . . . H6 H 0.7214 -0.0217 0.3319 0.040 Uiso 1 1 d R . . C7 C 0.5017(5) -0.0955(6) 0.2297(4) 0.0286(18) Uani 1 1 d . . . C8 C 0.4937(5) -0.1548(8) 0.2748(4) 0.036(2) Uani 1 1 d . . . H8 H 0.5311 -0.1455 0.3092 0.043 Uiso 1 1 d R . . C9 C 0.4315(6) -0.2247(9) 0.2684(5) 0.047(2) Uani 1 1 d . . . H9 H 0.4263 -0.2668 0.2985 0.057 Uiso 1 1 d R . . C10 C 0.3764(6) -0.2378(8) 0.2189(5) 0.049(3) Uani 1 1 d . . . H10 H 0.3340 -0.2879 0.2151 0.059 Uiso 1 1 d R . . C11 C 0.3840(5) -0.1774(8) 0.1760(4) 0.043(2) Uani 1 1 d . . . H11 H 0.3458 -0.1848 0.1418 0.051 Uiso 1 1 d R . . C12 C 0.4449(6) -0.1066(7) 0.1807(4) 0.037(2) Uani 1 1 d . . . H12 H 0.4485 -0.0641 0.1503 0.044 Uiso 1 1 d R . . C13 C 0.6664(5) -0.0913(7) 0.2248(3) 0.0271(18) Uani 1 1 d . . . C14 C 0.6821(5) -0.1921(7) 0.2464(3) 0.0270(17) Uani 1 1 d . . . H14 H 0.6548 -0.2172 0.2724 0.032 Uiso 1 1 d R . . C15 C 0.7357(5) -0.2563(7) 0.2312(3) 0.0335(19) Uani 1 1 d . . . H15 H 0.7461 -0.3253 0.2467 0.040 Uiso 1 1 d R . . C16 C 0.7756(5) -0.2186(7) 0.1931(3) 0.0296(18) Uani 1 1 d . . . H16 H 0.8121 -0.2633 0.1809 0.036 Uiso 1 1 d R . . C17 C 0.7623(5) -0.1175(6) 0.1726(4) 0.030(2) Uani 1 1 d . . . H17 H 0.7905 -0.0927 0.1471 0.036 Uiso 1 1 d R . . C18 C 0.7084(5) -0.0520(6) 0.1886(3) 0.0272(17) Uani 1 1 d . . . C19 C 0.7433(5) 0.1118(6) 0.1474(3) 0.0253(17) Uani 1 1 d . . . C20 C 0.8278(5) 0.0957(7) 0.1605(4) 0.0306(19) Uani 1 1 d . . . H20 H 0.8510 0.0387 0.1839 0.037 Uiso 1 1 d R . . C21 C 0.8750(5) 0.1591(7) 0.1394(4) 0.0317(18) Uani 1 1 d . . . H21 H 0.9314 0.1481 0.1488 0.038 Uiso 1 1 d R . . C22 C 0.8446(5) 0.2434(7) 0.1048(3) 0.0321(19) Uani 1 1 d . . . H22 H 0.8793 0.2862 0.0899 0.039 Uiso 1 1 d R . . C23 C 0.7637(5) 0.2609(7) 0.0927(3) 0.0307(18) Uani 1 1 d . . . H23 H 0.7416 0.3177 0.0689 0.037 Uiso 1 1 d R . . C24 C 0.7138(5) 0.1985(7) 0.1145(3) 0.0278(17) Uani 1 1 d . . . C25 C 0.5565(5) 0.1899(6) 0.0374(3) 0.0273(17) Uani 1 1 d . . . C26 C 0.5897(6) 0.1188(7) 0.0075(4) 0.033(2) Uani 1 1 d . . . H26 H 0.6437 0.0960 0.0216 0.039 Uiso 1 1 d R . . C27 C 0.5448(6) 0.0822(9) -0.0421(4) 0.041(2) Uani 1 1 d . . . H27 H 0.5672 0.0332 -0.0628 0.049 Uiso 1 1 d R . . C28 C 0.4668(6) 0.1152(7) -0.0616(4) 0.040(2) Uani 1 1 d . . . H28 H 0.4360 0.0885 -0.0956 0.048 Uiso 1 1 d R . . C29 C 0.4337(5) 0.1862(7) -0.0327(3) 0.0342(19) Uani 1 1 d . . . H29 H 0.3802 0.2107 -0.0472 0.041 Uiso 1 1 d R . . C30 C 0.4780(5) 0.2232(7) 0.0179(3) 0.0335(19) Uani 1 1 d . . . H30 H 0.4541 0.2700 0.0387 0.040 Uiso 1 1 d R . . C31 C 0.6000(5) 0.3652(7) 0.1130(4) 0.0289(18) Uani 1 1 d . . . C32 C 0.5898(5) 0.4336(7) 0.0690(3) 0.0309(18) Uani 1 1 d . . . H32 H 0.5843 0.4049 0.0335 0.037 Uiso 1 1 d R . . C33 C 0.5877(5) 0.5402(8) 0.0761(4) 0.037(2) Uani 1 1 d . . . H33 H 0.5795 0.5862 0.0454 0.045 Uiso 1 1 d R . . C34 C 0.5969(6) 0.5830(8) 0.1291(4) 0.043(2) Uani 1 1 d . . . H34 H 0.5977 0.6575 0.1354 0.052 Uiso 1 1 d R . . C35 C 0.6075(6) 0.5129(8) 0.1717(4) 0.039(2) Uani 1 1 d . . . H35 H 0.6123 0.5407 0.2073 0.046 Uiso 1 1 d R . . C36 C 0.6088(6) 0.4063(7) 0.1648(4) 0.0320(19) Uani 1 1 d . . . H36 H 0.6163 0.3595 0.1952 0.038 Uiso 1 1 d R . . C37 C 0.5195(8) 0.4100(10) 0.3539(6) 0.065(3) Uani 1 1 d . . . H37 H 0.5636 0.3838 0.3814 0.078 Uiso 1 1 d R . . C38 C 0.5157(7) 0.3824(8) 0.3014(6) 0.053(3) Uani 1 1 d . . . H38 H 0.5526 0.3327 0.2932 0.064 Uiso 1 1 d R . . C39 C 0.4586(7) 0.4257(10) 0.2604(5) 0.058(3) Uani 1 1 d . . . H39 H 0.4567 0.4092 0.2234 0.070 Uiso 1 1 d R . . C40 C 0.4046(8) 0.4922(10) 0.2724(8) 0.078(5) Uani 1 1 d . . . H40 H 0.3633 0.5222 0.2440 0.094 Uiso 1 1 d R . . C41 C 0.4055(9) 0.5169(11) 0.3247(8) 0.078(5) Uani 1 1 d . . . H41 H 0.3674 0.5657 0.3321 0.094 Uiso 1 1 d R . . C42 C 0.4638(9) 0.4753(11) 0.3663(7) 0.073(4) Uani 1 1 d . . . H42 H 0.4655 0.4872 0.4036 0.088 Uiso 1 1 d R . . C43 C 0.3399(7) 0.1889(11) 0.2644(5) 0.063(3) Uani 1 1 d . . . H43 H 0.3512 0.2336 0.2369 0.076 Uiso 1 1 d R . . C44 C 0.3251(6) 0.0834(12) 0.2515(5) 0.061(3) Uani 1 1 d . . . H44 H 0.3283 0.0552 0.2173 0.073 Uiso 1 1 d R . . C45 C 0.3069(7) 0.0188(10) 0.2906(6) 0.062(3) Uani 1 1 d . . . H45 H 0.2979 -0.0550 0.2834 0.074 Uiso 1 1 d R . . C46 C 0.3005(7) 0.0606(11) 0.3395(5) 0.062(3) Uani 1 1 d . . . H46 H 0.2831 0.0173 0.3651 0.075 Uiso 1 1 d R . . C47 C 0.3177(6) 0.1648(10) 0.3509(5) 0.054(3) Uani 1 1 d . . . H47 H 0.3174 0.1927 0.3857 0.064 Uiso 1 1 d R . . C48 C 0.3371(6) 0.2291(10) 0.3132(4) 0.051(3) Uani 1 1 d . . . H48 H 0.3494 0.3017 0.3219 0.061 Uiso 1 1 d R . . C49 C 0.3352(7) 0.4167(10) 0.0806(5) 0.054(3) Uani 1 1 d . . . H49 H 0.3482 0.3454 0.0917 0.064 Uiso 1 1 d R . . C50 C 0.2625(7) 0.4412(11) 0.0467(4) 0.059(3) Uani 1 1 d . . . H50 H 0.2232 0.3871 0.0355 0.071 Uiso 1 1 d R . . C51 C 0.2497(7) 0.5458(12) 0.0295(4) 0.063(4) Uani 1 1 d . . . H51 H 0.1992 0.5647 0.0060 0.075 Uiso 1 1 d R . . C52 C 0.3063(7) 0.6223(9) 0.0458(5) 0.048(3) Uani 1 1 d . . . H52 H 0.2971 0.6931 0.0327 0.057 Uiso 1 1 d R . . C53 C 0.3788(7) 0.5971(11) 0.0805(5) 0.061(3) Uani 1 1 d . . . H53 H 0.4189 0.6495 0.0935 0.073 Uiso 1 1 d R . . C54 C 0.3917(6) 0.4946(10) 0.0983(4) 0.053(3) Uani 1 1 d . . . H54 H 0.4414 0.4790 0.1236 0.063 Uiso 1 1 d R . . C55 C 0.2408(9) 0.0818(13) -0.0093(6) 0.074(4) Uani 1 1 d . . . H55 H 0.2459 0.1252 -0.0390 0.089 Uiso 1 1 d R . . C56 C 0.2820(9) 0.1012(11) 0.0411(7) 0.073(4) Uani 1 1 d . . . H56 H 0.3190 0.1585 0.0456 0.087 Uiso 1 1 d R . . C57 C 0.2728(7) 0.0480(13) 0.0829(5) 0.070(4) Uani 1 1 d . . . H57 H 0.3035 0.0670 0.1184 0.084 Uiso 1 1 d R . . C58 C 0.2214(9) -0.0349(13) 0.0792(8) 0.090(5) Uani 1 1 d . . . H58 H 0.2162 -0.0697 0.1115 0.108 Uiso 1 1 d R . . C59 C 0.1778(8) -0.0609(11) 0.0226(10) 0.095(6) Uani 1 1 d . . . H59 H 0.1418 -0.1194 0.0144 0.114 Uiso 1 1 d R . . C60 C 0.1916(8) -0.0001(12) -0.0175(6) 0.066(3) Uani 1 1 d . . . H60 H 0.1651 -0.0159 -0.0544 0.080 Uiso 1 1 d R . . C61 C 0.0812(9) 0.2130(11) 0.0451(7) 0.079(4) Uani 1 1 d . . . H61 H 0.1091 0.1476 0.0459 0.094 Uiso 1 1 d R . . C62 C 0.0196(10) 0.2377(12) -0.0007(6) 0.079(5) Uani 1 1 d . . . H62 H 0.0090 0.1928 -0.0319 0.095 Uiso 1 1 d R . . C63 C -0.0256(7) 0.3316(12) -0.0011(5) 0.066(4) Uani 1 1 d . . . H63 H -0.0663 0.3501 -0.0327 0.080 Uiso 1 1 d R . . C64 C -0.0092(8) 0.3927(9) 0.0421(6) 0.056(3) Uani 1 1 d . . . H64 H -0.0408 0.4543 0.0428 0.067 Uiso 1 1 d R . . C65 C 0.0514(9) 0.3677(12) 0.0862(6) 0.070(4) Uani 1 1 d . . . H65 H 0.0640 0.4136 0.1170 0.085 Uiso 1 1 d R . . C66 C 0.0960(9) 0.2802(14) 0.0864(6) 0.079(4) Uani 1 1 d . . . H66 H 0.1392 0.2632 0.1168 0.095 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0290(3) 0.0258(3) 0.0155(2) 0.00154(11) -0.00088(15) 0.00088(11) Cl1 0.0348(11) 0.0409(13) 0.0332(12) 0.0077(9) 0.0067(9) 0.0085(9) P1 0.0301(10) 0.0274(11) 0.0174(10) 0.0015(8) -0.0002(8) -0.0012(8) P2 0.0314(10) 0.0274(11) 0.0167(10) 0.0026(8) -0.0002(8) 0.0005(8) N1 0.030(3) 0.027(4) 0.020(3) 0.009(3) 0.000(3) 0.010(3) C1 0.029(4) 0.034(5) 0.021(4) 0.009(4) -0.003(3) -0.005(3) C2 0.034(5) 0.040(5) 0.029(5) -0.001(4) 0.002(4) 0.002(4) C3 0.043(5) 0.048(6) 0.021(5) -0.008(4) 0.006(4) 0.004(4) C4 0.041(5) 0.033(5) 0.027(5) 0.001(4) -0.002(4) -0.006(4) C5 0.032(4) 0.038(5) 0.021(4) 0.001(4) -0.004(3) 0.005(4) C6 0.035(4) 0.038(5) 0.023(4) -0.001(4) -0.001(3) -0.004(4) C7 0.035(4) 0.022(4) 0.025(5) -0.005(3) 0.002(4) -0.002(3) C8 0.037(5) 0.041(5) 0.027(5) 0.011(4) 0.002(4) -0.009(4) C9 0.047(6) 0.047(6) 0.044(6) 0.011(5) 0.005(5) -0.007(5) C10 0.034(5) 0.040(6) 0.065(7) 0.004(5) -0.007(5) -0.011(4) C11 0.032(5) 0.051(6) 0.036(5) -0.002(5) -0.009(4) -0.004(4) C12 0.047(6) 0.039(6) 0.021(5) 0.000(4) 0.001(4) -0.002(4) C13 0.036(4) 0.029(4) 0.013(4) -0.001(3) 0.001(3) 0.001(4) C14 0.029(4) 0.032(5) 0.019(4) 0.002(3) 0.003(3) -0.004(3) C15 0.032(4) 0.033(5) 0.027(5) 0.001(4) -0.006(3) -0.001(4) C16 0.033(4) 0.029(5) 0.023(4) 0.000(4) 0.000(3) 0.000(3) C17 0.030(4) 0.030(5) 0.026(5) 0.002(3) 0.000(4) -0.001(3) C18 0.032(4) 0.028(4) 0.018(4) -0.007(3) 0.000(3) -0.011(3) C19 0.031(4) 0.028(5) 0.016(4) 0.001(3) 0.004(3) 0.002(3) C20 0.033(4) 0.027(4) 0.027(5) 0.000(4) 0.000(4) 0.002(3) C21 0.034(4) 0.031(5) 0.029(5) -0.004(4) 0.007(3) 0.000(4) C22 0.042(5) 0.030(5) 0.022(4) 0.001(4) 0.004(4) -0.003(4) C23 0.040(5) 0.031(5) 0.020(4) 0.004(4) 0.005(3) 0.005(4) C24 0.035(4) 0.033(5) 0.011(4) 0.000(3) -0.001(3) 0.001(3) C25 0.031(4) 0.025(4) 0.021(4) 0.006(3) -0.002(3) 0.001(3) C26 0.043(5) 0.038(5) 0.013(4) 0.005(3) -0.001(4) 0.002(4) C27 0.048(5) 0.050(6) 0.018(4) 0.002(4) -0.003(4) 0.015(5) C28 0.054(6) 0.038(6) 0.019(5) 0.000(4) -0.008(4) -0.007(4) C29 0.036(4) 0.039(5) 0.021(4) 0.006(4) -0.003(3) -0.002(4) C30 0.045(5) 0.031(5) 0.022(4) 0.005(4) 0.003(4) 0.003(4) C31 0.030(4) 0.025(4) 0.026(5) 0.004(3) -0.001(3) -0.002(3) C32 0.038(4) 0.033(5) 0.019(4) -0.002(4) 0.003(3) -0.004(4) C33 0.035(5) 0.037(5) 0.031(5) 0.005(4) -0.008(4) 0.002(4) C34 0.047(5) 0.025(5) 0.048(6) 0.000(5) -0.008(4) -0.004(4) C35 0.040(5) 0.045(6) 0.023(5) -0.005(4) -0.005(4) 0.009(4) C36 0.042(5) 0.025(4) 0.023(5) 0.005(4) -0.002(4) 0.003(4) C37 0.069(8) 0.055(7) 0.063(9) 0.013(7) 0.001(6) -0.010(6) C38 0.045(6) 0.044(7) 0.072(9) 0.006(5) 0.015(6) 0.001(4) C39 0.055(7) 0.061(7) 0.060(8) 0.013(6) 0.020(6) -0.008(6) C40 0.053(7) 0.050(8) 0.126(14) 0.044(9) 0.012(8) 0.007(6) C41 0.074(9) 0.036(7) 0.136(16) -0.002(8) 0.044(10) 0.001(6) C42 0.092(10) 0.055(8) 0.084(10) -0.007(7) 0.044(9) -0.010(7) C43 0.045(6) 0.083(9) 0.065(8) 0.018(7) 0.019(6) -0.001(6) C44 0.039(6) 0.096(10) 0.047(7) -0.009(7) 0.011(5) 0.014(6) C45 0.063(7) 0.049(7) 0.067(9) 0.003(6) 0.004(6) 0.012(6) C46 0.051(6) 0.078(9) 0.051(7) 0.026(7) 0.000(5) 0.005(6) C47 0.044(6) 0.066(8) 0.047(6) 0.005(6) 0.004(5) 0.013(5) C48 0.051(6) 0.061(7) 0.043(6) -0.003(5) 0.014(5) -0.005(5) C49 0.067(7) 0.056(7) 0.035(6) -0.001(5) 0.009(5) 0.009(6) C50 0.058(7) 0.085(10) 0.028(5) -0.010(6) 0.000(5) -0.014(6) C51 0.055(6) 0.119(12) 0.010(4) -0.002(6) 0.002(4) 0.020(7) C52 0.050(6) 0.057(7) 0.036(6) 0.002(5) 0.011(5) 0.009(5) C53 0.054(7) 0.080(9) 0.045(7) -0.011(6) 0.004(5) 0.002(6) C54 0.041(5) 0.070(8) 0.041(6) 0.001(6) -0.002(4) 0.009(5) C55 0.077(9) 0.088(10) 0.062(9) -0.007(8) 0.028(7) 0.009(8) C56 0.058(8) 0.074(10) 0.086(12) -0.003(8) 0.018(8) 0.011(6) C57 0.057(7) 0.108(12) 0.039(7) -0.011(7) 0.003(5) 0.016(8) C58 0.065(9) 0.089(11) 0.124(15) 0.053(11) 0.039(9) 0.040(8) C59 0.048(7) 0.043(8) 0.19(2) -0.031(10) 0.022(10) -0.003(6) C60 0.070(8) 0.075(9) 0.051(7) -0.018(7) 0.009(6) 0.001(7) C61 0.090(10) 0.050(8) 0.106(13) 0.026(8) 0.044(10) 0.016(7) C62 0.117(12) 0.078(10) 0.059(8) -0.035(8) 0.056(9) -0.041(9) C63 0.048(6) 0.098(11) 0.051(7) 0.015(7) 0.008(5) -0.009(7) C64 0.066(8) 0.045(7) 0.063(9) -0.006(5) 0.027(7) -0.005(5) C65 0.066(8) 0.100(11) 0.046(8) -0.014(7) 0.016(6) -0.017(8) C66 0.074(9) 0.106(12) 0.053(8) 0.020(8) 0.007(7) 0.013(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 Pt1 N1 2.024(6) . ? Pt1 P2 2.270(2) . ? Pt1 P1 2.284(2) . ? Pt1 Cl1 2.318(2) . ? P1 C13 1.805(9) . ? P1 C7 1.810(9) . ? P1 C1 1.815(9) . ? P2 C24 1.799(8) . ? P2 C31 1.812(9) . ? P2 C25 1.817(8) . ? N1 C18 1.411(11) . ? N1 C19 1.407(11) . ? C1 C6 1.389(12) . ? C1 C2 1.396(13) . ? C2 C3 1.381(14) . ? C3 C4 1.402(14) . ? C4 C5 1.376(13) . ? C5 C6 1.393(12) . ? C7 C12 1.393(13) . ? C7 C8 1.413(12) . ? C8 C9 1.376(14) . ? C9 C10 1.391(15) . ? C10 C11 1.373(15) . ? C11 C12 1.371(14) . ? C13 C14 1.395(12) . ? C13 C18 1.407(12) . ? C14 C15 1.367(12) . ? C15 C16 1.413(12) . ? C16 C17 1.384(12) . ? C17 C18 1.389(12) . ? C19 C24 1.402(11) . ? C19 C20 1.436(12) . ? C20 C21 1.355(13) . ? C21 C22 1.405(12) . ? C22 C23 1.379(12) . ? C23 C24 1.391(12) . ? C25 C30 1.395(12) . ? C25 C26 1.398(12) . ? C26 C27 1.391(13) . ? C27 C28 1.385(14) . ? C28 C29 1.381(14) . ? C29 C30 1.409(12) . ? C31 C32 1.396(12) . ? C31 C36 1.396(13) . ? C32 C33 1.368(13) . ? C33 C34 1.430(14) . ? C34 C35 1.383(14) . ? C35 C36 1.366(13) . ? C37 C38 1.371(19) . ? C37 C42 1.372(19) . ? C38 C39 1.364(18) . ? C39 C40 1.354(19) . ? C40 C41 1.37(2) . ? C41 C42 1.38(2) . ? C43 C48 1.361(17) . ? C43 C44 1.389(19) . ? C44 C45 1.389(18) . ? C45 C46 1.386(18) . ? C46 C47 1.37(2) . ? C47 C48 1.368(16) . ? C49 C50 1.377(17) . ? C49 C54 1.387(17) . ? C50 C51 1.400(19) . ? C51 C52 1.371(18) . ? C52 C53 1.383(17) . ? C53 C54 1.379(17) . ? C55 C56 1.33(2) . ? C55 C60 1.33(2) . ? C56 C57 1.31(2) . ? C57 C58 1.37(2) . ? C58 C59 1.49(3) . ? C59 C60 1.35(2) . ? C61 C66 1.33(2) . ? C61 C62 1.41(2) . ? C62 C63 1.43(2) . ? C63 C64 1.319(18) . ? C64 C65 1.37(2) . ? C65 C66 1.35(2) . ? 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 Pt1 P2 83.72(19) . . ? N1 Pt1 P1 83.60(19) . . ? P2 Pt1 P1 167.30(8) . . ? N1 Pt1 Cl1 177.51(19) . . ? P2 Pt1 Cl1 94.52(8) . . ? P1 Pt1 Cl1 98.18(8) . . ? C13 P1 C7 106.4(4) . . ? C13 P1 C1 110.3(4) . . ? C7 P1 C1 103.3(4) . . ? C13 P1 Pt1 99.6(3) . . ? C7 P1 Pt1 120.1(3) . . ? C1 P1 Pt1 116.6(3) . . ? C24 P2 C31 106.4(4) . . ? C24 P2 C25 108.9(4) . . ? C31 P2 C25 107.2(4) . . ? C24 P2 Pt1 99.9(3) . . ? C31 P2 Pt1 119.6(3) . . ? C25 P2 Pt1 113.9(3) . . ? C18 N1 C19 122.9(6) . . ? C18 N1 Pt1 118.9(5) . . ? C19 N1 Pt1 118.1(5) . . ? C6 C1 C2 120.8(8) . . ? C6 C1 P1 123.1(7) . . ? C2 C1 P1 116.1(6) . . ? C3 C2 C1 119.5(9) . . ? C2 C3 C4 120.1(9) . . ? C5 C4 C3 119.8(9) . . ? C4 C5 C6 120.9(8) . . ? C1 C6 C5 119.0(8) . . ? C12 C7 C8 119.1(8) . . ? C12 C7 P1 120.4(7) . . ? C8 C7 P1 120.5(7) . . ? C9 C8 C7 118.9(9) . . ? C8 C9 C10 121.7(10) . . ? C11 C10 C9 118.5(9) . . ? C12 C11 C10 121.6(9) . . ? C11 C12 C7 120.2(9) . . ? C14 C13 C18 120.3(8) . . ? C14 C13 P1 123.6(6) . . ? C18 C13 P1 115.8(6) . . ? C15 C14 C13 120.9(8) . . ? C14 C15 C16 118.8(8) . . ? C17 C16 C15 120.7(8) . . ? C16 C17 C18 120.4(8) . . ? C17 C18 N1 123.5(7) . . ? C17 C18 C13 118.8(8) . . ? N1 C18 C13 117.7(7) . . ? C24 C19 N1 119.1(7) . . ? C24 C19 C20 116.8(7) . . ? N1 C19 C20 124.0(7) . . ? C21 C20 C19 120.6(8) . . ? C20 C21 C22 122.3(8) . . ? C23 C22 C21 117.7(8) . . ? C22 C23 C24 121.5(8) . . ? C23 C24 C19 121.1(8) . . ? C23 C24 P2 124.0(6) . . ? C19 C24 P2 114.8(6) . . ? C30 C25 C26 120.1(8) . . ? C30 C25 P2 119.0(6) . . ? C26 C25 P2 120.2(6) . . ? C27 C26 C25 120.0(9) . . ? C26 C27 C28 120.0(9) . . ? C29 C28 C27 120.4(9) . . ? C28 C29 C30 120.3(9) . . ? C25 C30 C29 119.1(8) . . ? C32 C31 C36 119.5(8) . . ? C32 C31 P2 122.1(7) . . ? C36 C31 P2 118.2(7) . . ? C33 C32 C31 120.7(8) . . ? C32 C33 C34 120.2(9) . . ? C35 C34 C33 117.5(9) . . ? C36 C35 C34 122.6(9) . . ? C35 C36 C31 119.5(8) . . ? C38 C37 C42 121.2(14) . . ? C37 C38 C39 119.6(12) . . ? C40 C39 C38 119.3(14) . . ? C39 C40 C41 121.7(14) . . ? C40 C41 C42 119.5(13) . . ? C37 C42 C41 118.5(15) . . ? C48 C43 C44 122.1(12) . . ? C45 C44 C43 117.5(11) . . ? C46 C45 C44 120.4(12) . . ? C47 C46 C45 119.9(11) . . ? C46 C47 C48 120.4(11) . . ? C43 C48 C47 119.6(12) . . ? C50 C49 C54 120.4(12) . . ? C49 C50 C51 117.4(12) . . ? C52 C51 C50 122.2(10) . . ? C53 C52 C51 119.9(11) . . ? C52 C53 C54 118.5(12) . . ? C53 C54 C49 121.6(11) . . ? C56 C55 C60 117.7(15) . . ? C57 C56 C55 123.4(16) . . ? C56 C57 C58 123.5(15) . . ? C57 C58 C59 113.7(14) . . ? C60 C59 C58 117.7(12) . . ? C55 C60 C59 123.9(14) . . ? C66 C61 C62 118.1(13) . . ? C61 C62 C63 119.5(12) . . ? C64 C63 C62 119.0(13) . . ? C63 C64 C65 120.6(13) . . ? C66 C65 C64 120.9(14) . . ? C61 C66 C65 121.9(14) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 5.617 _refine_diff_density_min -3.950 _refine_diff_density_rms 0.284