# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Martin Smith' 'Mark Elsegood' 'Andrew J. Lake' _publ_contact_author_name 'Martin Smith' _publ_contact_author_email M.B.SMITH@LBORO.AC.UK _publ_section_title ; A novel fluorene-containing ?4-P2N2-tetradentate platinum(II) complex ; # Attachment 'Dalton_Trans_Comm_CIF_data__MBSmith_.cif' # Manuscript submitted to: Dalton Trans. # Authors: Mark R. J. Elsegood, Andrew J. Lake and Martin B. Smith # Title: A novel fluorene containing kappa4-P2N2-tetradentate platinum(II) complex # Corresponding author for crystallography: # m.r.j.elsegood@lboro.ac.uk data_2 _database_code_depnum_ccdc_archive 'CCDC 702768' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H21 N2 O P' _chemical_formula_sum 'C26 H21 N2 O P' _chemical_formula_weight 408.42 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' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6349(7) _cell_length_b 13.7094(8) _cell_length_c 13.7679(8) _cell_angle_alpha 71.744(2) _cell_angle_beta 84.887(2) _cell_angle_gamma 71.011(2) _cell_volume 2141.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6841 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 28.21 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.923 _exptl_absorpt_correction_T_max 0.9882 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18991 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 29.01 _reflns_number_total 9889 _reflns_number_gt 7137 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0496P)^2^+1.0055P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'Geom except both NH coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9889 _refine_ls_number_parameters 547 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 P1 P -0.18585(4) 0.35456(4) 0.10532(3) 0.02595(11) Uani 1 1 d . . . O1 O -0.15790(11) 0.24000(10) 0.17209(9) 0.0326(3) Uani 1 1 d . . . C1 C -0.10216(14) 0.42808(15) 0.13644(14) 0.0272(4) Uani 1 1 d . . . H1A H -0.1122 0.4973 0.0813 0.033 Uiso 1 1 calc R . . H1B H -0.1298 0.4452 0.2006 0.033 Uiso 1 1 calc R . . N1 N 0.01565(12) 0.36731(13) 0.14850(12) 0.0282(3) Uani 1 1 d . . . H1 H 0.0430(18) 0.3379(18) 0.2106(17) 0.042 Uiso 1 1 d . . . N2 N 0.06595(12) 0.34258(12) 0.06602(11) 0.0261(3) Uani 1 1 d . . . C2 C 0.16998(14) 0.28393(14) 0.06755(13) 0.0259(4) Uani 1 1 d . . . C3 C 0.21659(15) 0.25621(14) -0.02576(14) 0.0293(4) Uani 1 1 d . . . C4 C 0.16517(17) 0.28349(16) -0.11952(15) 0.0347(4) Uani 1 1 d . . . H4 H 0.0900 0.3296 -0.1325 0.042 Uiso 1 1 calc R . . C5 C 0.22686(19) 0.24134(18) -0.19418(17) 0.0434(5) Uani 1 1 d . . . H5 H 0.1936 0.2591 -0.2592 0.052 Uiso 1 1 calc R . . C6 C 0.33641(19) 0.1737(2) -0.17472(18) 0.0479(6) Uani 1 1 d . . . H6 H 0.3766 0.1449 -0.2265 0.057 Uiso 1 1 calc R . . C7 C 0.38830(18) 0.14718(18) -0.08173(18) 0.0430(5) Uani 1 1 d . . . H7 H 0.4636 0.1013 -0.0694 0.052 Uiso 1 1 calc R . . C8 C 0.32773(16) 0.18926(15) -0.00628(16) 0.0332(4) Uani 1 1 d . . . C9 C 0.35666(15) 0.17544(15) 0.09877(16) 0.0324(4) Uani 1 1 d . . . C10 C 0.45650(17) 0.12017(18) 0.15358(18) 0.0447(5) Uani 1 1 d . . . H10 H 0.5207 0.0831 0.1227 0.054 Uiso 1 1 calc R . . C11 C 0.46147(18) 0.11972(19) 0.25363(19) 0.0503(6) Uani 1 1 d . . . H11 H 0.5297 0.0822 0.2914 0.060 Uiso 1 1 calc R . . C12 C 0.36833(17) 0.17326(19) 0.29970(17) 0.0451(5) Uani 1 1 d . . . H12 H 0.3735 0.1716 0.3686 0.054 Uiso 1 1 calc R . . C13 C 0.26737(16) 0.22935(16) 0.24621(15) 0.0350(4) Uani 1 1 d . . . H13 H 0.2037 0.2658 0.2781 0.042 Uiso 1 1 calc R . . C14 C 0.26102(14) 0.23123(14) 0.14543(14) 0.0276(4) Uani 1 1 d . . . C15 C -0.32896(15) 0.43059(16) 0.12002(14) 0.0310(4) Uani 1 1 d . . . C16 C -0.40144(19) 0.3748(2) 0.1705(2) 0.0538(6) Uani 1 1 d . . . H16 H -0.3752 0.2981 0.1960 0.065 Uiso 1 1 calc R . . C17 C -0.5125(2) 0.4307(2) 0.1839(2) 0.0678(8) Uani 1 1 d . . . H17 H -0.5619 0.3921 0.2186 0.081 Uiso 1 1 calc R . . C18 C -0.55101(19) 0.5418(2) 0.1471(2) 0.0546(6) Uani 1 1 d . . . H18 H -0.6264 0.5799 0.1578 0.065 Uiso 1 1 calc R . . C19 C -0.4808(2) 0.5973(2) 0.0950(2) 0.0636(8) Uani 1 1 d . . . H19 H -0.5079 0.6740 0.0684 0.076 Uiso 1 1 calc R . . C20 C -0.36994(19) 0.54187(18) 0.0809(2) 0.0566(7) Uani 1 1 d . . . H20 H -0.3218 0.5809 0.0439 0.068 Uiso 1 1 calc R . . C21 C -0.16413(14) 0.36170(15) -0.02768(13) 0.0264(4) Uani 1 1 d . . . C22 C -0.14597(16) 0.26730(16) -0.05325(15) 0.0331(4) Uani 1 1 d . . . H22 H -0.1475 0.2028 -0.0016 0.040 Uiso 1 1 calc R . . C23 C -0.12551(18) 0.26647(17) -0.15408(15) 0.0373(5) Uani 1 1 d . . . H23 H -0.1135 0.2017 -0.1711 0.045 Uiso 1 1 calc R . . C24 C -0.12271(17) 0.35980(17) -0.22929(15) 0.0372(5) Uani 1 1 d . . . H24 H -0.1076 0.3590 -0.2979 0.045 Uiso 1 1 calc R . . C25 C -0.14184(17) 0.45460(16) -0.20484(14) 0.0360(4) Uani 1 1 d . . . H25 H -0.1404 0.5188 -0.2569 0.043 Uiso 1 1 calc R . . C26 C -0.16311(16) 0.45629(15) -0.10473(14) 0.0317(4) Uani 1 1 d . . . H26 H -0.1770 0.5218 -0.0885 0.038 Uiso 1 1 calc R . . P2 P -0.02391(4) 0.27346(4) 0.44411(3) 0.02633(11) Uani 1 1 d . . . O2 O 0.03539(11) 0.33256(11) 0.35946(9) 0.0336(3) Uani 1 1 d . . . C27 C -0.08254(16) 0.18417(15) 0.40667(14) 0.0299(4) Uani 1 1 d . . . H27A H -0.0949 0.1286 0.4687 0.036 Uiso 1 1 calc R . . H27B H -0.1559 0.2271 0.3722 0.036 Uiso 1 1 calc R . . N3 N -0.00923(14) 0.13171(13) 0.33896(13) 0.0349(4) Uani 1 1 d . . . H3 H -0.031(2) 0.1514(19) 0.2768(19) 0.052 Uiso 1 1 d . . . N4 N 0.08944(13) 0.06266(12) 0.37778(12) 0.0319(4) Uani 1 1 d . . . C28 C 0.16265(16) 0.01186(14) 0.32291(15) 0.0316(4) Uani 1 1 d . . . C29 C 0.16492(16) 0.00847(14) 0.21622(15) 0.0312(4) Uani 1 1 d . . . C30 C 0.09110(17) 0.06527(15) 0.13319(15) 0.0332(4) Uani 1 1 d . . . H30 H 0.0227 0.1182 0.1399 0.040 Uiso 1 1 calc R . . C31 C 0.11885(18) 0.04356(16) 0.04001(16) 0.0387(5) Uani 1 1 d . . . H31 H 0.0687 0.0823 -0.0167 0.046 Uiso 1 1 calc R . . C32 C 0.21778(19) -0.03304(17) 0.02869(17) 0.0431(5) Uani 1 1 d . . . H32 H 0.2351 -0.0464 -0.0355 0.052 Uiso 1 1 calc R . . C33 C 0.29193(18) -0.09048(17) 0.11029(18) 0.0439(5) Uani 1 1 d . . . H33 H 0.3597 -0.1437 0.1026 0.053 Uiso 1 1 calc R . . C34 C 0.26668(17) -0.06976(16) 0.20351(17) 0.0371(5) Uani 1 1 d . . . C35 C 0.33052(17) -0.11514(16) 0.29984(18) 0.0408(5) Uani 1 1 d . . . C36 C 0.43428(19) -0.1936(2) 0.3268(2) 0.0554(6) Uani 1 1 d . . . H36 H 0.4757 -0.2289 0.2795 0.067 Uiso 1 1 calc R . . C37 C 0.4754(2) -0.2189(2) 0.4244(2) 0.0656(8) Uani 1 1 d . . . H37 H 0.5465 -0.2719 0.4438 0.079 Uiso 1 1 calc R . . C38 C 0.4157(2) -0.1692(2) 0.4948(2) 0.0607(7) Uani 1 1 d . . . H38 H 0.4466 -0.1882 0.5612 0.073 Uiso 1 1 calc R . . C39 C 0.31041(19) -0.09128(18) 0.46906(19) 0.0458(5) Uani 1 1 d . . . H39 H 0.2686 -0.0575 0.5172 0.055 Uiso 1 1 calc R . . C40 C 0.26922(17) -0.06503(16) 0.37105(17) 0.0372(5) Uani 1 1 d . . . C41 C -0.13974(16) 0.36545(14) 0.48938(13) 0.0292(4) Uani 1 1 d . . . C42 C -0.23185(17) 0.33819(17) 0.53837(16) 0.0389(5) Uani 1 1 d . . . H42 H -0.2368 0.2681 0.5482 0.047 Uiso 1 1 calc R . . C43 C -0.31660(19) 0.41315(19) 0.57301(18) 0.0503(6) Uani 1 1 d . . . H43 H -0.3795 0.3943 0.6063 0.060 Uiso 1 1 calc R . . C44 C -0.3096(2) 0.51480(19) 0.55921(19) 0.0575(7) Uani 1 1 d . . . H44 H -0.3668 0.5654 0.5842 0.069 Uiso 1 1 calc R . . C45 C -0.2199(2) 0.54297(19) 0.5094(2) 0.0607(7) Uani 1 1 d . . . H45 H -0.2160 0.6136 0.4990 0.073 Uiso 1 1 calc R . . C46 C -0.1348(2) 0.46905(16) 0.47401(17) 0.0438(5) Uani 1 1 d . . . H46 H -0.0732 0.4892 0.4393 0.053 Uiso 1 1 calc R . . C47 C 0.06943(15) 0.18870(14) 0.55116(13) 0.0267(4) Uani 1 1 d . . . C48 C 0.18319(16) 0.17361(16) 0.53711(14) 0.0333(4) Uani 1 1 d . . . H48 H 0.2089 0.2127 0.4749 0.040 Uiso 1 1 calc R . . C49 C 0.25949(17) 0.10169(17) 0.61368(15) 0.0375(5) Uani 1 1 d . . . H49 H 0.3372 0.0921 0.6042 0.045 Uiso 1 1 calc R . . C50 C 0.22234(18) 0.04401(17) 0.70374(15) 0.0380(5) Uani 1 1 d . . . H50 H 0.2748 -0.0066 0.7554 0.046 Uiso 1 1 calc R . . C51 C 0.10948(18) 0.05946(16) 0.71910(15) 0.0376(5) Uani 1 1 d . . . H51 H 0.0844 0.0207 0.7818 0.045 Uiso 1 1 calc R . . C52 C 0.03259(16) 0.13146(16) 0.64317(14) 0.0325(4) Uani 1 1 d . . . H52 H -0.0451 0.1418 0.6538 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0222(2) 0.0298(2) 0.0235(2) -0.00786(18) 0.00023(17) -0.00525(18) O1 0.0325(7) 0.0332(7) 0.0278(7) -0.0044(5) -0.0001(5) -0.0089(6) C1 0.0239(9) 0.0310(9) 0.0253(9) -0.0121(7) 0.0009(7) -0.0036(7) N1 0.0229(8) 0.0359(9) 0.0225(7) -0.0093(7) -0.0003(6) -0.0044(6) N2 0.0270(8) 0.0264(7) 0.0260(8) -0.0095(6) 0.0024(6) -0.0088(6) C2 0.0244(9) 0.0250(9) 0.0295(9) -0.0082(7) 0.0025(7) -0.0098(7) C3 0.0287(10) 0.0275(9) 0.0353(10) -0.0130(8) 0.0081(8) -0.0124(8) C4 0.0344(11) 0.0369(11) 0.0359(11) -0.0152(9) 0.0060(8) -0.0125(9) C5 0.0505(13) 0.0499(13) 0.0391(12) -0.0224(10) 0.0095(10) -0.0220(11) C6 0.0448(13) 0.0595(15) 0.0541(14) -0.0361(12) 0.0222(11) -0.0232(11) C7 0.0305(11) 0.0470(12) 0.0603(14) -0.0306(11) 0.0156(10) -0.0138(9) C8 0.0271(10) 0.0315(10) 0.0455(11) -0.0163(9) 0.0101(8) -0.0132(8) C9 0.0247(9) 0.0286(9) 0.0451(11) -0.0123(8) 0.0061(8) -0.0102(8) C10 0.0255(10) 0.0422(12) 0.0609(15) -0.0179(11) 0.0011(10) -0.0012(9) C11 0.0273(11) 0.0536(14) 0.0552(14) -0.0072(11) -0.0100(10) 0.0007(10) C12 0.0309(11) 0.0571(14) 0.0379(12) -0.0069(10) -0.0059(9) -0.0069(10) C13 0.0256(10) 0.0394(11) 0.0350(10) -0.0074(9) 0.0002(8) -0.0074(8) C14 0.0215(9) 0.0242(9) 0.0349(10) -0.0057(7) 0.0023(7) -0.0075(7) C15 0.0235(9) 0.0393(10) 0.0294(9) -0.0126(8) -0.0008(7) -0.0063(8) C16 0.0360(12) 0.0492(14) 0.0688(17) -0.0099(12) 0.0101(11) -0.0138(11) C17 0.0342(13) 0.0736(19) 0.090(2) -0.0182(16) 0.0190(13) -0.0200(13) C18 0.0248(11) 0.0706(17) 0.0662(16) -0.0307(14) 0.0035(10) -0.0033(11) C19 0.0331(13) 0.0447(14) 0.106(2) -0.0261(15) 0.0058(13) -0.0016(11) C20 0.0321(12) 0.0352(12) 0.097(2) -0.0175(13) 0.0170(12) -0.0100(10) C21 0.0232(9) 0.0326(9) 0.0246(9) -0.0098(7) 0.0001(7) -0.0089(7) C22 0.0368(11) 0.0326(10) 0.0311(10) -0.0093(8) 0.0008(8) -0.0130(8) C23 0.0443(12) 0.0373(11) 0.0357(11) -0.0178(9) 0.0021(9) -0.0137(9) C24 0.0425(12) 0.0478(12) 0.0261(10) -0.0155(9) 0.0024(8) -0.0167(10) C25 0.0444(12) 0.0385(11) 0.0259(10) -0.0062(8) -0.0016(8) -0.0169(9) C26 0.0367(11) 0.0303(10) 0.0295(10) -0.0102(8) -0.0012(8) -0.0108(8) P2 0.0290(2) 0.0273(2) 0.0213(2) -0.00772(18) 0.00025(18) -0.00665(19) O2 0.0384(8) 0.0355(7) 0.0242(6) -0.0059(6) 0.0027(5) -0.0116(6) C27 0.0314(10) 0.0306(9) 0.0274(9) -0.0109(8) -0.0038(7) -0.0061(8) N3 0.0371(9) 0.0339(9) 0.0295(9) -0.0145(7) -0.0074(7) 0.0009(7) N4 0.0348(9) 0.0262(8) 0.0344(9) -0.0090(7) -0.0061(7) -0.0077(7) C28 0.0316(10) 0.0225(9) 0.0414(11) -0.0089(8) -0.0013(8) -0.0096(8) C29 0.0317(10) 0.0247(9) 0.0411(11) -0.0127(8) 0.0085(8) -0.0134(8) C30 0.0368(11) 0.0284(9) 0.0371(10) -0.0133(8) 0.0067(8) -0.0122(8) C31 0.0478(13) 0.0351(11) 0.0390(11) -0.0144(9) 0.0089(9) -0.0198(10) C32 0.0529(14) 0.0400(12) 0.0449(12) -0.0201(10) 0.0197(10) -0.0236(10) C33 0.0383(12) 0.0359(11) 0.0616(15) -0.0224(11) 0.0226(11) -0.0153(9) C34 0.0327(11) 0.0281(10) 0.0506(12) -0.0109(9) 0.0093(9) -0.0130(8) C35 0.0295(10) 0.0316(10) 0.0575(14) -0.0097(10) 0.0088(9) -0.0102(8) C36 0.0333(12) 0.0458(13) 0.0713(17) -0.0058(12) 0.0062(12) -0.0045(10) C37 0.0313(13) 0.0572(16) 0.087(2) -0.0032(15) -0.0034(13) -0.0029(11) C38 0.0446(14) 0.0583(16) 0.0687(18) -0.0006(13) -0.0195(13) -0.0150(12) C39 0.0401(12) 0.0397(12) 0.0557(14) -0.0069(10) -0.0086(10) -0.0149(10) C40 0.0321(11) 0.0295(10) 0.0495(12) -0.0070(9) -0.0042(9) -0.0126(8) C41 0.0330(10) 0.0269(9) 0.0238(9) -0.0068(7) -0.0016(7) -0.0046(8) C42 0.0363(11) 0.0358(11) 0.0450(12) -0.0157(9) 0.0041(9) -0.0094(9) C43 0.0375(12) 0.0515(14) 0.0541(14) -0.0170(11) 0.0093(10) -0.0051(10) C44 0.0584(16) 0.0411(13) 0.0546(15) -0.0153(11) 0.0093(12) 0.0067(11) C45 0.0777(19) 0.0284(11) 0.0658(17) -0.0144(11) 0.0160(14) -0.0073(12) C46 0.0524(14) 0.0297(10) 0.0449(12) -0.0097(9) 0.0102(10) -0.0111(10) C47 0.0308(9) 0.0258(9) 0.0238(9) -0.0091(7) -0.0014(7) -0.0075(7) C48 0.0352(11) 0.0393(11) 0.0252(9) -0.0091(8) 0.0015(8) -0.0124(9) C49 0.0300(10) 0.0471(12) 0.0348(11) -0.0146(9) -0.0018(8) -0.0085(9) C50 0.0399(12) 0.0377(11) 0.0316(10) -0.0078(9) -0.0093(9) -0.0058(9) C51 0.0465(12) 0.0395(11) 0.0265(10) -0.0027(8) -0.0027(8) -0.0190(10) C52 0.0321(10) 0.0379(10) 0.0286(10) -0.0085(8) -0.0004(8) -0.0137(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 P1 O1 1.4929(13) . ? P1 C15 1.7993(19) . ? P1 C21 1.8037(18) . ? P1 C1 1.8336(19) . ? C1 N1 1.445(2) . ? N1 N2 1.334(2) . ? N2 C2 1.297(2) . ? C2 C3 1.472(2) . ? C2 C14 1.479(2) . ? C3 C4 1.385(3) . ? C3 C8 1.400(3) . ? C4 C5 1.391(3) . ? C5 C6 1.387(3) . ? C6 C7 1.380(3) . ? C7 C8 1.394(3) . ? C8 C9 1.463(3) . ? C9 C10 1.387(3) . ? C9 C14 1.423(2) . ? C10 C11 1.383(3) . ? C11 C12 1.387(3) . ? C12 C13 1.391(3) . ? C13 C14 1.389(3) . ? C15 C20 1.381(3) . ? C15 C16 1.384(3) . ? C16 C17 1.390(3) . ? C17 C18 1.375(4) . ? C18 C19 1.365(4) . ? C19 C20 1.389(3) . ? C21 C22 1.389(3) . ? C21 C26 1.398(3) . ? C22 C23 1.392(3) . ? C23 C24 1.380(3) . ? C24 C25 1.384(3) . ? C25 C26 1.387(3) . ? P2 O2 1.4914(13) . ? P2 C41 1.8026(18) . ? P2 C47 1.8051(18) . ? P2 C27 1.8347(19) . ? C27 N3 1.441(2) . ? N3 N4 1.330(2) . ? N4 C28 1.303(2) . ? C28 C40 1.470(3) . ? C28 C29 1.482(3) . ? C29 C30 1.394(3) . ? C29 C34 1.419(3) . ? C30 C31 1.396(3) . ? C31 C32 1.380(3) . ? C32 C33 1.383(3) . ? C33 C34 1.388(3) . ? C34 C35 1.464(3) . ? C35 C36 1.390(3) . ? C35 C40 1.405(3) . ? C36 C37 1.383(4) . ? C37 C38 1.386(4) . ? C38 C39 1.400(3) . ? C39 C40 1.386(3) . ? C41 C46 1.390(3) . ? C41 C42 1.391(3) . ? C42 C43 1.389(3) . ? C43 C44 1.378(3) . ? C44 C45 1.373(4) . ? C45 C46 1.388(3) . ? C47 C48 1.389(3) . ? C47 C52 1.395(3) . ? C48 C49 1.387(3) . ? C49 C50 1.381(3) . ? C50 C51 1.379(3) . ? C51 C52 1.386(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 O1 P1 C15 111.55(8) . . ? O1 P1 C21 111.23(8) . . ? C15 P1 C21 108.34(8) . . ? O1 P1 C1 112.79(8) . . ? C15 P1 C1 105.02(8) . . ? C21 P1 C1 107.58(8) . . ? N1 C1 P1 112.64(12) . . ? N2 N1 C1 115.86(14) . . ? C2 N2 N1 122.30(15) . . ? N2 C2 C3 118.39(16) . . ? N2 C2 C14 135.09(17) . . ? C3 C2 C14 106.50(15) . . ? C4 C3 C8 121.44(17) . . ? C4 C3 C2 129.47(17) . . ? C8 C3 C2 109.04(17) . . ? C3 C4 C5 118.02(19) . . ? C6 C5 C4 120.7(2) . . ? C7 C6 C5 121.4(2) . . ? C6 C7 C8 118.5(2) . . ? C7 C8 C3 119.9(2) . . ? C7 C8 C9 131.98(19) . . ? C3 C8 C9 108.13(16) . . ? C10 C9 C14 120.03(19) . . ? C10 C9 C8 130.86(18) . . ? C14 C9 C8 109.11(16) . . ? C11 C10 C9 119.21(19) . . ? C10 C11 C12 121.0(2) . . ? C11 C12 C13 120.8(2) . . ? C14 C13 C12 118.99(19) . . ? C13 C14 C9 119.96(17) . . ? C13 C14 C2 132.86(17) . . ? C9 C14 C2 107.17(16) . . ? C20 C15 C16 118.77(19) . . ? C20 C15 P1 122.70(16) . . ? C16 C15 P1 118.51(16) . . ? C15 C16 C17 120.2(2) . . ? C18 C17 C16 120.2(2) . . ? C19 C18 C17 120.0(2) . . ? C18 C19 C20 120.1(2) . . ? C15 C20 C19 120.7(2) . . ? C22 C21 C26 119.14(17) . . ? C22 C21 P1 117.54(14) . . ? C26 C21 P1 123.31(14) . . ? C21 C22 C23 120.48(18) . . ? C24 C23 C22 119.93(18) . . ? C23 C24 C25 120.08(18) . . ? C24 C25 C26 120.33(18) . . ? C25 C26 C21 120.02(17) . . ? O2 P2 C41 111.56(8) . . ? O2 P2 C47 111.20(8) . . ? C41 P2 C47 108.02(8) . . ? O2 P2 C27 113.28(8) . . ? C41 P2 C27 106.13(9) . . ? C47 P2 C27 106.31(8) . . ? N3 C27 P2 111.56(13) . . ? N4 N3 C27 116.55(15) . . ? C28 N4 N3 121.62(16) . . ? N4 C28 C40 118.89(18) . . ? N4 C28 C29 134.65(18) . . ? C40 C28 C29 106.41(16) . . ? C30 C29 C34 118.97(18) . . ? C30 C29 C28 133.26(17) . . ? C34 C29 C28 107.77(17) . . ? C29 C30 C31 119.28(19) . . ? C32 C31 C30 121.2(2) . . ? C31 C32 C33 120.3(2) . . ? C32 C33 C34 119.53(19) . . ? C33 C34 C29 120.6(2) . . ? C33 C34 C35 130.87(19) . . ? C29 C34 C35 108.47(18) . . ? C36 C35 C40 120.4(2) . . ? C36 C35 C34 130.9(2) . . ? C40 C35 C34 108.68(17) . . ? C37 C36 C35 118.0(2) . . ? C36 C37 C38 121.9(2) . . ? C37 C38 C39 120.6(3) . . ? C40 C39 C38 117.8(2) . . ? C39 C40 C35 121.3(2) . . ? C39 C40 C28 130.0(2) . . ? C35 C40 C28 108.63(19) . . ? C46 C41 C42 119.13(18) . . ? C46 C41 P2 117.11(15) . . ? C42 C41 P2 123.76(15) . . ? C43 C42 C41 120.2(2) . . ? C44 C43 C42 120.1(2) . . ? C45 C44 C43 120.1(2) . . ? C44 C45 C46 120.5(2) . . ? C45 C46 C41 120.0(2) . . ? C48 C47 C52 119.42(17) . . ? C48 C47 P2 117.85(14) . . ? C52 C47 P2 122.50(14) . . ? C49 C48 C47 120.22(18) . . ? C50 C49 C48 119.91(19) . . ? C51 C50 C49 120.36(19) . . ? C50 C51 C52 120.12(19) . . ? C51 C52 C47 119.96(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 C1 N1 46.75(15) . . . . ? C15 P1 C1 N1 168.44(13) . . . . ? C21 P1 C1 N1 -76.30(14) . . . . ? P1 C1 N1 N2 61.75(18) . . . . ? C1 N1 N2 C2 -176.59(16) . . . . ? N1 N2 C2 C3 176.89(15) . . . . ? N1 N2 C2 C14 -1.4(3) . . . . ? N2 C2 C3 C4 -0.2(3) . . . . ? C14 C2 C3 C4 178.52(18) . . . . ? N2 C2 C3 C8 -177.53(16) . . . . ? C14 C2 C3 C8 1.2(2) . . . . ? C8 C3 C4 C5 0.7(3) . . . . ? C2 C3 C4 C5 -176.34(19) . . . . ? C3 C4 C5 C6 0.3(3) . . . . ? C4 C5 C6 C7 -0.9(3) . . . . ? C5 C6 C7 C8 0.6(3) . . . . ? C6 C7 C8 C3 0.4(3) . . . . ? C6 C7 C8 C9 178.6(2) . . . . ? C4 C3 C8 C7 -1.1(3) . . . . ? C2 C3 C8 C7 176.54(17) . . . . ? C4 C3 C8 C9 -179.62(17) . . . . ? C2 C3 C8 C9 -2.0(2) . . . . ? C7 C8 C9 C10 4.0(4) . . . . ? C3 C8 C9 C10 -177.6(2) . . . . ? C7 C8 C9 C14 -176.2(2) . . . . ? C3 C8 C9 C14 2.2(2) . . . . ? C14 C9 C10 C11 0.3(3) . . . . ? C8 C9 C10 C11 -179.9(2) . . . . ? C9 C10 C11 C12 0.2(4) . . . . ? C10 C11 C12 C13 -0.3(4) . . . . ? C11 C12 C13 C14 -0.1(3) . . . . ? C12 C13 C14 C9 0.6(3) . . . . ? C12 C13 C14 C2 -178.3(2) . . . . ? C10 C9 C14 C13 -0.7(3) . . . . ? C8 C9 C14 C13 179.50(17) . . . . ? C10 C9 C14 C2 178.44(18) . . . . ? C8 C9 C14 C2 -1.4(2) . . . . ? N2 C2 C14 C13 -2.5(4) . . . . ? C3 C2 C14 C13 179.11(19) . . . . ? N2 C2 C14 C9 178.6(2) . . . . ? C3 C2 C14 C9 0.15(19) . . . . ? O1 P1 C15 C20 168.37(19) . . . . ? C21 P1 C15 C20 -68.9(2) . . . . ? C1 P1 C15 C20 45.9(2) . . . . ? O1 P1 C15 C16 -13.3(2) . . . . ? C21 P1 C15 C16 109.48(18) . . . . ? C1 P1 C15 C16 -135.78(18) . . . . ? C20 C15 C16 C17 -2.0(4) . . . . ? P1 C15 C16 C17 179.6(2) . . . . ? C15 C16 C17 C18 0.1(4) . . . . ? C16 C17 C18 C19 1.6(4) . . . . ? C17 C18 C19 C20 -1.2(4) . . . . ? C16 C15 C20 C19 2.3(4) . . . . ? P1 C15 C20 C19 -179.3(2) . . . . ? C18 C19 C20 C15 -0.7(4) . . . . ? O1 P1 C21 C22 11.53(17) . . . . ? C15 P1 C21 C22 -111.42(15) . . . . ? C1 P1 C21 C22 135.53(15) . . . . ? O1 P1 C21 C26 -167.48(15) . . . . ? C15 P1 C21 C26 69.56(17) . . . . ? C1 P1 C21 C26 -43.49(17) . . . . ? C26 C21 C22 C23 0.9(3) . . . . ? P1 C21 C22 C23 -178.19(15) . . . . ? C21 C22 C23 C24 0.3(3) . . . . ? C22 C23 C24 C25 -0.9(3) . . . . ? C23 C24 C25 C26 0.5(3) . . . . ? C24 C25 C26 C21 0.7(3) . . . . ? C22 C21 C26 C25 -1.3(3) . . . . ? P1 C21 C26 C25 177.66(15) . . . . ? O2 P2 C27 N3 38.03(16) . . . . ? C41 P2 C27 N3 160.77(13) . . . . ? C47 P2 C27 N3 -84.38(14) . . . . ? P2 C27 N3 N4 65.1(2) . . . . ? C27 N3 N4 C28 -179.11(17) . . . . ? N3 N4 C28 C40 -178.78(17) . . . . ? N3 N4 C28 C29 -1.5(3) . . . . ? N4 C28 C29 C30 5.4(4) . . . . ? C40 C28 C29 C30 -177.1(2) . . . . ? N4 C28 C29 C34 -175.6(2) . . . . ? C40 C28 C29 C34 1.9(2) . . . . ? C34 C29 C30 C31 0.2(3) . . . . ? C28 C29 C30 C31 179.19(19) . . . . ? C29 C30 C31 C32 0.1(3) . . . . ? C30 C31 C32 C33 0.2(3) . . . . ? C31 C32 C33 C34 -0.7(3) . . . . ? C32 C33 C34 C29 1.0(3) . . . . ? C32 C33 C34 C35 -177.7(2) . . . . ? C30 C29 C34 C33 -0.8(3) . . . . ? C28 C29 C34 C33 -179.95(17) . . . . ? C30 C29 C34 C35 178.20(17) . . . . ? C28 C29 C34 C35 -1.0(2) . . . . ? C33 C34 C35 C36 -1.3(4) . . . . ? C29 C34 C35 C36 179.9(2) . . . . ? C33 C34 C35 C40 178.4(2) . . . . ? C29 C34 C35 C40 -0.4(2) . . . . ? C40 C35 C36 C37 -1.1(3) . . . . ? C34 C35 C36 C37 178.6(2) . . . . ? C35 C36 C37 C38 0.6(4) . . . . ? C36 C37 C38 C39 0.4(4) . . . . ? C37 C38 C39 C40 -0.8(4) . . . . ? C38 C39 C40 C35 0.3(3) . . . . ? C38 C39 C40 C28 179.5(2) . . . . ? C36 C35 C40 C39 0.6(3) . . . . ? C34 C35 C40 C39 -179.12(18) . . . . ? C36 C35 C40 C28 -178.65(19) . . . . ? C34 C35 C40 C28 1.6(2) . . . . ? N4 C28 C40 C39 -3.4(3) . . . . ? C29 C28 C40 C39 178.6(2) . . . . ? N4 C28 C40 C35 175.79(17) . . . . ? C29 C28 C40 C35 -2.2(2) . . . . ? O2 P2 C41 C46 -24.54(18) . . . . ? C47 P2 C41 C46 97.96(17) . . . . ? C27 P2 C41 C46 -148.37(16) . . . . ? O2 P2 C41 C42 155.72(16) . . . . ? C47 P2 C41 C42 -81.78(18) . . . . ? C27 P2 C41 C42 31.89(19) . . . . ? C46 C41 C42 C43 -1.2(3) . . . . ? P2 C41 C42 C43 178.57(17) . . . . ? C41 C42 C43 C44 -0.2(4) . . . . ? C42 C43 C44 C45 1.3(4) . . . . ? C43 C44 C45 C46 -1.1(4) . . . . ? C44 C45 C46 C41 -0.3(4) . . . . ? C42 C41 C46 C45 1.4(3) . . . . ? P2 C41 C46 C45 -178.36(19) . . . . ? O2 P2 C47 C48 -10.68(17) . . . . ? C41 P2 C47 C48 -133.41(15) . . . . ? C27 P2 C47 C48 113.04(15) . . . . ? O2 P2 C47 C52 174.87(15) . . . . ? C41 P2 C47 C52 52.14(17) . . . . ? C27 P2 C47 C52 -61.41(17) . . . . ? C52 C47 C48 C49 0.4(3) . . . . ? P2 C47 C48 C49 -174.18(15) . . . . ? C47 C48 C49 C50 0.7(3) . . . . ? C48 C49 C50 C51 -1.6(3) . . . . ? C49 C50 C51 C52 1.4(3) . . . . ? C50 C51 C52 C47 -0.2(3) . . . . ? C48 C47 C52 C51 -0.7(3) . . . . ? P2 C47 C52 C51 173.68(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O2 0.87(2) 2.02(2) 2.813(2) 150(2) . N3 H3 O1 0.86(2) 2.04(2) 2.798(2) 147(2) . _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.473 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.048 #===End data_3 _database_code_depnum_ccdc_archive 'CCDC 702769' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H42 Cl2 N4 P2 Pt, C4 H10 O' _chemical_formula_sum 'C28 H26 Cl N2 O0.50 P Pt0.50' _chemical_formula_weight 562.47 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2/a _symmetry_space_group_name_Hall '-I 2ya' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 20.0646(8) _cell_length_b 10.7880(4) _cell_length_c 23.7050(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.046(2) _cell_angle_gamma 90.00 _cell_volume 4788.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10767 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.97 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 3.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.405 _exptl_absorpt_correction_T_max 0.685 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20850 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 29.08 _reflns_number_total 5835 _reflns_number_gt 4567 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0154P)^2^+6.4730P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 5835 _refine_ls_number_parameters 313 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0471 _refine_ls_wR_factor_gt 0.0414 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.2500 0.246212(12) 0.0000 0.02410(4) Uani 1 2 d S . . Cl1 Cl 0.32506(4) 0.08876(5) 0.05837(3) 0.03518(15) Uani 1 1 d . . . P1 P 0.32458(3) 0.37755(5) 0.06628(3) 0.02659(14) Uani 1 1 d . . . C1 C 0.33837(16) 0.3198(2) 0.14409(12) 0.0404(6) Uani 1 1 d . . . H1A H 0.3784 0.2599 0.1568 0.049 Uiso 1 1 calc R . . H1B H 0.3512 0.3902 0.1728 0.049 Uiso 1 1 calc R . . N1 N 0.27435(15) 0.2602(2) 0.14589(11) 0.0462(6) Uani 1 1 d . . . H1 H 0.2654(18) 0.191(3) 0.1289(16) 0.069 Uiso 1 1 d . . . N2 N 0.23605(15) 0.3163(2) 0.17411(10) 0.0444(6) Uani 1 1 d . . . C2 C 0.17542(17) 0.2675(2) 0.17125(12) 0.0417(6) Uani 1 1 d . . . C3 C 0.13257(16) 0.1618(2) 0.13828(12) 0.0391(6) Uani 1 1 d . . . C4 C 0.14219(16) 0.0739(2) 0.09860(12) 0.0400(6) Uani 1 1 d . . . H4 H 0.1846 0.0737 0.0895 0.048 Uiso 1 1 calc R . . C5 C 0.08892(17) -0.0133(3) 0.07255(13) 0.0453(7) Uani 1 1 d . . . H5 H 0.0954 -0.0735 0.0457 0.054 Uiso 1 1 calc R . . C6 C 0.02644(18) -0.0142(3) 0.08504(14) 0.0492(7) Uani 1 1 d . . . H6 H -0.0092 -0.0749 0.0670 0.059 Uiso 1 1 calc R . . C7 C 0.01591(17) 0.0736(3) 0.12392(13) 0.0473(7) Uani 1 1 d . . . H7 H -0.0270 0.0739 0.1322 0.057 Uiso 1 1 calc R . . C8 C 0.06828(17) 0.1603(3) 0.15033(12) 0.0427(7) Uani 1 1 d . . . C9 C 0.06992(19) 0.2637(3) 0.19162(12) 0.0494(8) Uani 1 1 d . . . C10 C 0.0208(2) 0.3021(3) 0.21688(14) 0.0625(10) Uani 1 1 d . . . H10 H -0.0230 0.2590 0.2086 0.075 Uiso 1 1 calc R . . C11 C 0.0371(3) 0.4052(4) 0.25451(16) 0.0775(13) Uani 1 1 d . . . H11 H 0.0037 0.4336 0.2715 0.093 Uiso 1 1 calc R . . C12 C 0.1007(3) 0.4666(4) 0.26749(15) 0.0766(13) Uani 1 1 d . . . H12 H 0.1110 0.5355 0.2942 0.092 Uiso 1 1 calc R . . C13 C 0.1504(2) 0.4301(3) 0.24239(14) 0.0637(10) Uani 1 1 d . . . H13 H 0.1940 0.4739 0.2510 0.076 Uiso 1 1 calc R . . C14 C 0.13417(19) 0.3270(3) 0.20407(13) 0.0504(8) Uani 1 1 d . . . C15 C 0.41161(13) 0.3763(2) 0.05968(12) 0.0305(5) Uani 1 1 d . . . C16 C 0.47253(15) 0.4167(3) 0.10674(13) 0.0420(7) Uani 1 1 d . . . H16 H 0.4688 0.4481 0.1429 0.050 Uiso 1 1 calc R . . C17 C 0.53824(15) 0.4106(3) 0.10033(15) 0.0488(8) Uani 1 1 d . . . H17 H 0.5797 0.4381 0.1323 0.059 Uiso 1 1 calc R . . C18 C 0.54415(15) 0.3653(3) 0.04814(14) 0.0452(7) Uani 1 1 d . . . H18 H 0.5897 0.3612 0.0444 0.054 Uiso 1 1 calc R . . C19 C 0.48437(15) 0.3256(2) 0.00114(14) 0.0407(6) Uani 1 1 d . . . H19 H 0.4886 0.2946 -0.0350 0.049 Uiso 1 1 calc R . . C20 C 0.41809(14) 0.3314(2) 0.00699(12) 0.0335(6) Uani 1 1 d . . . H20 H 0.3768 0.3044 -0.0253 0.040 Uiso 1 1 calc R . . C21 C 0.30257(12) 0.53922(19) 0.07177(11) 0.0264(5) Uani 1 1 d . . . C22 C 0.24877(13) 0.5691(2) 0.09370(11) 0.0313(5) Uani 1 1 d . . . H22 H 0.2214 0.5051 0.1024 0.038 Uiso 1 1 calc R . . C23 C 0.23512(14) 0.6921(2) 0.10286(12) 0.0359(6) Uani 1 1 d . . . H23 H 0.1993 0.7118 0.1188 0.043 Uiso 1 1 calc R . . C24 C 0.27341(15) 0.7861(2) 0.08888(13) 0.0376(6) Uani 1 1 d . . . H24 H 0.2637 0.8702 0.0949 0.045 Uiso 1 1 calc R . . C25 C 0.32582(14) 0.7573(2) 0.06610(12) 0.0378(6) Uani 1 1 d . . . H25 H 0.3515 0.8218 0.0557 0.045 Uiso 1 1 calc R . . C26 C 0.34126(13) 0.6343(2) 0.05822(12) 0.0321(5) Uani 1 1 d . . . H26 H 0.3783 0.6150 0.0435 0.039 Uiso 1 1 calc R . . O1 O 0.2500 0.7500 0.2500 0.0810(13) Uani 1 2 d SDU . . C27 C 0.3124(4) 0.7446(7) 0.2557(3) 0.063(2) Uani 0.514(8) 1 d PDU A 1 H27A H 0.3377 0.7981 0.2909 0.076 Uiso 0.514(8) 1 calc PR A 1 H27B H 0.3156 0.7879 0.2199 0.076 Uiso 0.514(8) 1 calc PR A 1 C28 C 0.3557(3) 0.6383(5) 0.2631(2) 0.129(2) Uani 1 1 d DU . . H28A H 0.4041 0.6633 0.2669 0.194 Uiso 0.514(8) 1 calc PR A 1 H28B H 0.3357 0.5840 0.2279 0.194 Uiso 0.514(8) 1 calc PR A 1 H28C H 0.3575 0.5937 0.2996 0.194 Uiso 0.514(8) 1 calc PR A 1 H28D H 0.3730 0.5529 0.2722 0.194 Uiso 0.486(8) 1 calc PR A 2 H28E H 0.3863 0.6939 0.2944 0.194 Uiso 0.486(8) 1 calc PR A 2 H28F H 0.3572 0.6626 0.2237 0.194 Uiso 0.486(8) 1 calc PR A 2 C27X C 0.2935(5) 0.6450(6) 0.2617(4) 0.070(3) Uani 0.486(8) 1 d PDU A 2 H27C H 0.2952 0.6141 0.3015 0.084 Uiso 0.486(8) 1 calc PR A 2 H27D H 0.2664 0.5824 0.2317 0.084 Uiso 0.486(8) 1 calc PR A 2 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 0.02823(6) 0.01393(5) 0.02893(7) 0.000 0.00879(5) 0.000 Cl1 0.0408(4) 0.0194(3) 0.0413(4) 0.0054(2) 0.0099(3) 0.0055(2) P1 0.0296(3) 0.0177(3) 0.0295(3) -0.0010(2) 0.0069(3) 0.0012(2) C1 0.0559(18) 0.0267(13) 0.0316(14) 0.0008(11) 0.0071(13) -0.0006(12) N1 0.0773(18) 0.0267(11) 0.0407(13) -0.0034(11) 0.0284(12) -0.0051(13) N2 0.0743(18) 0.0287(11) 0.0277(12) 0.0041(9) 0.0152(12) 0.0113(12) C2 0.0624(18) 0.0309(14) 0.0302(13) 0.0072(11) 0.0148(12) 0.0091(13) C3 0.0595(18) 0.0285(13) 0.0314(14) 0.0084(11) 0.0189(13) 0.0083(12) C4 0.0588(18) 0.0288(13) 0.0386(15) 0.0042(11) 0.0250(14) 0.0037(12) C5 0.066(2) 0.0337(14) 0.0395(16) 0.0013(12) 0.0232(15) 0.0025(14) C6 0.061(2) 0.0416(16) 0.0456(18) 0.0053(13) 0.0203(16) -0.0030(14) C7 0.0537(19) 0.0506(17) 0.0436(17) 0.0157(14) 0.0248(15) 0.0114(15) C8 0.0616(19) 0.0391(15) 0.0311(15) 0.0112(12) 0.0212(14) 0.0154(14) C9 0.072(2) 0.0472(17) 0.0301(13) 0.0108(13) 0.0196(14) 0.0248(17) C10 0.084(3) 0.070(2) 0.0400(18) 0.0116(16) 0.0303(18) 0.036(2) C11 0.100(3) 0.090(3) 0.045(2) 0.003(2) 0.028(2) 0.052(3) C12 0.113(4) 0.071(3) 0.0364(19) -0.0068(17) 0.016(2) 0.050(3) C13 0.090(3) 0.0519(19) 0.0376(17) -0.0041(15) 0.0090(18) 0.0270(19) C14 0.079(2) 0.0410(16) 0.0280(15) 0.0056(12) 0.0157(15) 0.0248(16) C15 0.0281(13) 0.0185(10) 0.0396(14) -0.0024(10) 0.0057(11) 0.0028(9) C16 0.0367(15) 0.0388(15) 0.0425(16) -0.0087(12) 0.0045(13) 0.0001(12) C17 0.0295(15) 0.0467(17) 0.058(2) -0.0047(15) 0.0009(14) -0.0051(13) C18 0.0300(15) 0.0397(15) 0.065(2) 0.0017(14) 0.0156(14) 0.0005(12) C19 0.0405(16) 0.0330(14) 0.0521(18) -0.0048(12) 0.0207(14) -0.0004(12) C20 0.0313(13) 0.0253(12) 0.0406(15) -0.0048(10) 0.0088(12) -0.0030(10) C21 0.0301(13) 0.0179(10) 0.0287(12) -0.0033(9) 0.0077(10) -0.0002(9) C22 0.0336(14) 0.0236(11) 0.0383(14) 0.0005(10) 0.0146(11) -0.0010(10) C23 0.0385(15) 0.0321(13) 0.0407(15) 0.0000(11) 0.0185(12) 0.0064(11) C24 0.0447(16) 0.0200(11) 0.0471(16) -0.0057(10) 0.0153(13) 0.0033(10) C25 0.0416(14) 0.0208(11) 0.0526(15) -0.0008(12) 0.0191(12) -0.0047(12) C26 0.0341(14) 0.0230(11) 0.0426(15) -0.0016(10) 0.0178(12) -0.0010(10) O1 0.141(4) 0.056(2) 0.0469(19) 0.0119(18) 0.035(3) 0.042(3) C27 0.095(5) 0.051(4) 0.044(3) 0.000(3) 0.025(4) -0.012(4) C28 0.151(5) 0.130(5) 0.080(3) 0.018(3) 0.008(4) 0.080(4) C27X 0.121(7) 0.033(4) 0.053(4) 0.010(3) 0.026(5) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2420(6) . ? Pt1 P1 2.2420(6) 2 ? Pt1 Cl1 2.3603(6) 2 ? Pt1 Cl1 2.3603(6) . ? P1 C15 1.808(3) . ? P1 C21 1.815(2) . ? P1 C1 1.871(3) . ? C1 N1 1.451(4) . ? N1 N2 1.332(3) . ? N2 C2 1.305(4) . ? C2 C14 1.471(4) . ? C2 C3 1.473(4) . ? C3 C4 1.397(4) . ? C3 C8 1.418(4) . ? C4 C5 1.391(4) . ? C5 C6 1.388(4) . ? C6 C7 1.390(4) . ? C7 C8 1.377(4) . ? C8 C9 1.477(4) . ? C9 C10 1.388(4) . ? C9 C14 1.394(5) . ? C10 C11 1.389(5) . ? C11 C12 1.371(6) . ? C12 C13 1.388(5) . ? C13 C14 1.399(4) . ? C15 C20 1.388(4) . ? C15 C16 1.396(3) . ? C16 C17 1.382(4) . ? C17 C18 1.374(4) . ? C18 C19 1.380(4) . ? C19 C20 1.387(4) . ? C21 C26 1.391(3) . ? C21 C22 1.394(3) . ? C22 C23 1.387(3) . ? C23 C24 1.382(4) . ? C24 C25 1.379(4) . ? C25 C26 1.391(3) . ? O1 C27 1.211(8) 7_565 ? O1 C27 1.211(8) . ? O1 C27X 1.396(7) 7_565 ? O1 C27X 1.396(7) . ? C27 C28 1.412(8) . ? C28 C27X 1.239(8) . ? 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 P1 Pt1 P1 101.61(3) . 2 ? P1 Pt1 Cl1 172.04(2) . 2 ? P1 Pt1 Cl1 85.36(2) 2 2 ? P1 Pt1 Cl1 85.36(2) . . ? P1 Pt1 Cl1 172.04(2) 2 . ? Cl1 Pt1 Cl1 87.95(3) 2 . ? C15 P1 C21 106.31(11) . . ? C15 P1 C1 106.09(13) . . ? C21 P1 C1 101.71(12) . . ? C15 P1 Pt1 110.90(8) . . ? C21 P1 Pt1 122.62(8) . . ? C1 P1 Pt1 107.80(9) . . ? N1 C1 P1 110.94(19) . . ? N2 N1 C1 119.4(2) . . ? C2 N2 N1 119.1(2) . . ? N2 C2 C14 119.2(3) . . ? N2 C2 C3 134.1(3) . . ? C14 C2 C3 106.6(3) . . ? C4 C3 C8 118.9(3) . . ? C4 C3 C2 133.5(3) . . ? C8 C3 C2 107.6(2) . . ? C5 C4 C3 119.2(3) . . ? C6 C5 C4 121.3(3) . . ? C5 C6 C7 120.1(3) . . ? C8 C7 C6 119.4(3) . . ? C7 C8 C3 121.1(3) . . ? C7 C8 C9 130.2(3) . . ? C3 C8 C9 108.6(3) . . ? C10 C9 C14 120.5(3) . . ? C10 C9 C8 131.4(3) . . ? C14 C9 C8 108.0(3) . . ? C9 C10 C11 118.5(4) . . ? C12 C11 C10 121.1(4) . . ? C11 C12 C13 121.4(4) . . ? C12 C13 C14 117.9(4) . . ? C9 C14 C13 120.6(3) . . ? C9 C14 C2 109.1(3) . . ? C13 C14 C2 130.3(4) . . ? C20 C15 C16 119.3(2) . . ? C20 C15 P1 119.07(19) . . ? C16 C15 P1 121.6(2) . . ? C17 C16 C15 119.6(3) . . ? C18 C17 C16 120.7(3) . . ? C17 C18 C19 120.4(3) . . ? C18 C19 C20 119.5(3) . . ? C19 C20 C15 120.6(2) . . ? C26 C21 C22 119.1(2) . . ? C26 C21 P1 121.42(18) . . ? C22 C21 P1 119.34(17) . . ? C23 C22 C21 120.2(2) . . ? C24 C23 C22 120.4(2) . . ? C25 C24 C23 119.8(2) . . ? C24 C25 C26 120.4(2) . . ? C25 C26 C21 120.2(2) . . ? C27 O1 C27 180.0(7) 7_565 . ? C27 O1 C27X 52.5(5) 7_565 7_565 ? C27 O1 C27X 127.5(5) . 7_565 ? C27 O1 C27X 127.5(5) 7_565 . ? C27 O1 C27X 52.5(5) . . ? C27X O1 C27X 180.000(2) 7_565 . ? O1 C27 C28 128.2(6) . . ? C27X C28 C27 51.6(5) . . ? C28 C27X O1 127.2(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pt1 P1 C15 -108.78(9) 2 . . . ? Cl1 Pt1 P1 C15 67.35(9) . . . . ? P1 Pt1 P1 C21 18.18(9) 2 . . . ? Cl1 Pt1 P1 C21 -165.69(10) . . . . ? P1 Pt1 P1 C1 135.48(10) 2 . . . ? Cl1 Pt1 P1 C1 -48.39(10) . . . . ? C15 P1 C1 N1 -152.07(18) . . . . ? C21 P1 C1 N1 96.93(19) . . . . ? Pt1 P1 C1 N1 -33.2(2) . . . . ? P1 C1 N1 N2 -108.7(2) . . . . ? C1 N1 N2 C2 174.3(2) . . . . ? N1 N2 C2 C14 178.0(2) . . . . ? N1 N2 C2 C3 -5.7(4) . . . . ? N2 C2 C3 C4 1.2(5) . . . . ? C14 C2 C3 C4 177.8(3) . . . . ? N2 C2 C3 C8 -175.7(3) . . . . ? C14 C2 C3 C8 0.9(3) . . . . ? C8 C3 C4 C5 -0.7(4) . . . . ? C2 C3 C4 C5 -177.3(3) . . . . ? C3 C4 C5 C6 0.3(4) . . . . ? C4 C5 C6 C7 0.4(4) . . . . ? C5 C6 C7 C8 -0.7(4) . . . . ? C6 C7 C8 C3 0.3(4) . . . . ? C6 C7 C8 C9 178.5(3) . . . . ? C4 C3 C8 C7 0.4(4) . . . . ? C2 C3 C8 C7 177.8(2) . . . . ? C4 C3 C8 C9 -178.2(2) . . . . ? C2 C3 C8 C9 -0.7(3) . . . . ? C7 C8 C9 C10 1.7(5) . . . . ? C3 C8 C9 C10 -179.9(3) . . . . ? C7 C8 C9 C14 -178.1(3) . . . . ? C3 C8 C9 C14 0.3(3) . . . . ? C14 C9 C10 C11 0.2(4) . . . . ? C8 C9 C10 C11 -179.6(3) . . . . ? C9 C10 C11 C12 -1.2(5) . . . . ? C10 C11 C12 C13 1.6(6) . . . . ? C11 C12 C13 C14 -1.1(5) . . . . ? C10 C9 C14 C13 0.2(4) . . . . ? C8 C9 C14 C13 -179.9(3) . . . . ? C10 C9 C14 C2 -179.5(3) . . . . ? C8 C9 C14 C2 0.3(3) . . . . ? C12 C13 C14 C9 0.2(4) . . . . ? C12 C13 C14 C2 179.9(3) . . . . ? N2 C2 C14 C9 176.5(2) . . . . ? C3 C2 C14 C9 -0.8(3) . . . . ? N2 C2 C14 C13 -3.2(5) . . . . ? C3 C2 C14 C13 179.5(3) . . . . ? C21 P1 C15 C20 -115.9(2) . . . . ? C1 P1 C15 C20 136.4(2) . . . . ? Pt1 P1 C15 C20 19.6(2) . . . . ? C21 P1 C15 C16 65.5(2) . . . . ? C1 P1 C15 C16 -42.2(2) . . . . ? Pt1 P1 C15 C16 -158.99(19) . . . . ? C20 C15 C16 C17 -0.4(4) . . . . ? P1 C15 C16 C17 178.1(2) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? C16 C17 C18 C19 0.3(5) . . . . ? C17 C18 C19 C20 -0.2(4) . . . . ? C18 C19 C20 C15 -0.2(4) . . . . ? C16 C15 C20 C19 0.5(4) . . . . ? P1 C15 C20 C19 -178.1(2) . . . . ? C15 P1 C21 C26 13.4(2) . . . . ? C1 P1 C21 C26 124.2(2) . . . . ? Pt1 P1 C21 C26 -115.6(2) . . . . ? C15 P1 C21 C22 -162.5(2) . . . . ? C1 P1 C21 C22 -51.6(2) . . . . ? Pt1 P1 C21 C22 68.6(2) . . . . ? C26 C21 C22 C23 -1.2(4) . . . . ? P1 C21 C22 C23 174.8(2) . . . . ? C21 C22 C23 C24 1.7(4) . . . . ? C22 C23 C24 C25 -0.5(4) . . . . ? C23 C24 C25 C26 -1.2(4) . . . . ? C24 C25 C26 C21 1.7(4) . . . . ? C22 C21 C26 C25 -0.5(4) . . . . ? P1 C21 C26 C25 -176.3(2) . . . . ? C27X O1 C27 C28 -174.8(6) 7_565 . . . ? C27X O1 C27 C28 5.2(6) . . . . ? O1 C27 C28 C27X -5.9(7) . . . . ? C27 C28 C27X O1 5.1(6) . . . . ? C27 O1 C27X C28 174.2(7) 7_565 . . . ? C27 O1 C27X C28 -5.8(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl1 0.84(3) 2.62(3) 3.206(2) 128(3) . _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.662 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.073 #===End data_4 _database_code_depnum_ccdc_archive 'CCDC 702770' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H38 N4 P2 Pt, C7 H8' _chemical_formula_sum 'C59 H46 N4 P2 Pt' _chemical_formula_weight 1068.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 12.0681(6) _cell_length_b 15.7231(8) _cell_length_c 25.0731(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.648(2) _cell_angle_gamma 90.00 _cell_volume 4703.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10074 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 28.23 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 3.096 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.457 _exptl_absorpt_correction_T_max 0.671 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 40505 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10772 _reflns_number_gt 7718 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0175P)^2^+7.9269P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 10772 _refine_ls_number_parameters 596 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Pt1 Pt 0.517270(14) 0.838240(11) 0.788503(6) 0.02052(5) Uani 1 1 d . . . P1 P 0.48425(9) 0.84645(8) 0.87367(4) 0.0236(2) Uani 1 1 d . . . P2 P 0.69831(9) 0.81274(7) 0.78343(5) 0.0236(3) Uani 1 1 d . . . N2 N 0.3516(3) 0.8587(2) 0.77090(13) 0.0214(8) Uani 1 1 d . . . N4 N 0.5068(3) 0.8491(2) 0.70815(13) 0.0230(8) Uani 1 1 d . . . C1 C 0.3356(4) 0.8714(3) 0.85884(18) 0.0267(10) Uani 1 1 d . . . H1 H 0.2924 0.8781 0.8873 0.032 Uiso 1 1 calc R . . N1 N 0.2890(3) 0.8799(2) 0.80894(15) 0.0268(8) Uani 1 1 d . . . C2 C 0.3179(3) 0.8958(3) 0.71680(16) 0.0227(9) Uani 1 1 d . . . C3 C 0.3383(4) 0.9921(3) 0.71555(16) 0.0236(10) Uani 1 1 d . . . C4 C 0.4340(4) 1.0385(3) 0.73393(17) 0.0280(10) Uani 1 1 d . . . H4 H 0.4988 1.0113 0.7526 0.034 Uiso 1 1 calc R . . C5 C 0.4333(4) 1.1255(3) 0.72454(19) 0.0361(12) Uani 1 1 d . . . H5 H 0.4984 1.1580 0.7369 0.043 Uiso 1 1 calc R . . C6 C 0.3395(4) 1.1658(3) 0.69747(19) 0.0375(11) Uani 1 1 d . . . H6 H 0.3416 1.2252 0.6907 0.045 Uiso 1 1 calc R . . C7 C 0.2421(4) 1.1203(3) 0.68005(18) 0.0344(11) Uani 1 1 d . . . H7 H 0.1774 1.1480 0.6618 0.041 Uiso 1 1 calc R . . C8 C 0.2415(4) 1.0332(3) 0.68993(18) 0.0297(11) Uani 1 1 d . . . C9 C 0.1503(4) 0.9701(3) 0.67892(17) 0.0279(10) Uani 1 1 d . . . C10 C 0.0380(4) 0.9811(3) 0.6580(2) 0.0398(12) Uani 1 1 d . . . H10 H 0.0095 1.0358 0.6473 0.048 Uiso 1 1 calc R . . C11 C -0.0315(4) 0.9104(3) 0.6532(2) 0.0400(13) Uani 1 1 d . . . H11 H -0.1084 0.9165 0.6386 0.048 Uiso 1 1 calc R . . C12 C 0.0096(4) 0.8320(3) 0.66925(18) 0.0343(11) Uani 1 1 d . . . H12 H -0.0393 0.7843 0.6655 0.041 Uiso 1 1 calc R . . C13 C 0.1219(4) 0.8206(3) 0.69095(17) 0.0295(11) Uani 1 1 d . . . H13 H 0.1493 0.7659 0.7024 0.035 Uiso 1 1 calc R . . C14 C 0.1923(4) 0.8899(3) 0.69544(16) 0.0237(10) Uani 1 1 d . . . C15 C 0.5037(4) 0.7600(3) 0.92199(17) 0.0287(10) Uani 1 1 d . . . C16 C 0.5558(4) 0.6859(3) 0.91053(19) 0.0345(12) Uani 1 1 d . . . H16 H 0.5820 0.6794 0.8769 0.041 Uiso 1 1 calc R . . C17 C 0.5703(5) 0.6200(3) 0.9484(2) 0.0454(14) Uani 1 1 d . . . H17 H 0.6069 0.5690 0.9406 0.054 Uiso 1 1 calc R . . C18 C 0.5315(5) 0.6289(4) 0.9972(2) 0.0528(16) Uani 1 1 d . . . H18 H 0.5396 0.5835 1.0225 0.063 Uiso 1 1 calc R . . C19 C 0.4818(6) 0.7027(4) 1.0089(2) 0.0627(18) Uani 1 1 d . . . H19 H 0.4569 0.7093 1.0429 0.075 Uiso 1 1 calc R . . C20 C 0.4672(5) 0.7682(4) 0.9719(2) 0.0538(16) Uani 1 1 d . . . H20 H 0.4319 0.8193 0.9805 0.065 Uiso 1 1 calc R . . C21 C 0.5521(4) 0.9376(3) 0.91039(18) 0.0282(10) Uani 1 1 d . . . C22 C 0.6444(5) 0.9270(3) 0.9502(2) 0.0462(14) Uani 1 1 d . . . H22 H 0.6670 0.8715 0.9623 0.055 Uiso 1 1 calc R . . C23 C 0.7035(5) 0.9977(4) 0.9721(2) 0.0529(15) Uani 1 1 d . . . H23 H 0.7658 0.9904 0.9997 0.063 Uiso 1 1 calc R . . C24 C 0.6732(5) 1.0773(4) 0.9543(2) 0.0499(15) Uani 1 1 d . . . H24 H 0.7151 1.1251 0.9692 0.060 Uiso 1 1 calc R . . C25 C 0.5816(5) 1.0891(3) 0.9148(2) 0.0484(15) Uani 1 1 d . . . H25 H 0.5598 1.1449 0.9029 0.058 Uiso 1 1 calc R . . C26 C 0.5215(4) 1.0191(3) 0.8923(2) 0.0359(12) Uani 1 1 d . . . H26 H 0.4595 1.0270 0.8645 0.043 Uiso 1 1 calc R . . C27 C 0.6869(4) 0.8113(3) 0.71021(18) 0.0305(11) Uani 1 1 d . . . H27 H 0.7503 0.7987 0.6933 0.037 Uiso 1 1 calc R . . N3 N 0.5898(3) 0.8280(2) 0.68120(14) 0.0272(8) Uani 1 1 d . . . C28 C 0.3918(3) 0.8475(3) 0.67853(16) 0.0228(9) Uani 1 1 d . . . C29 C 0.3808(3) 0.8867(3) 0.62208(17) 0.0233(10) Uani 1 1 d . . . C30 C 0.4122(4) 0.9664(3) 0.60629(18) 0.0287(10) Uani 1 1 d . . . H30 H 0.4455 1.0062 0.6324 0.034 Uiso 1 1 calc R . . C31 C 0.3946(4) 0.9875(3) 0.55195(18) 0.0356(12) Uani 1 1 d . . . H31 H 0.4150 1.0424 0.5410 0.043 Uiso 1 1 calc R . . C32 C 0.3480(4) 0.9297(3) 0.51366(19) 0.0433(13) Uani 1 1 d . . . H32 H 0.3369 0.9450 0.4766 0.052 Uiso 1 1 calc R . . C33 C 0.3173(4) 0.8496(3) 0.52889(19) 0.0409(13) Uani 1 1 d . . . H33 H 0.2856 0.8096 0.5025 0.049 Uiso 1 1 calc R . . C34 C 0.3333(4) 0.8284(3) 0.58338(18) 0.0302(10) Uani 1 1 d . . . C35 C 0.3120(4) 0.7486(3) 0.61022(18) 0.0268(10) Uani 1 1 d . . . C36 C 0.2650(4) 0.6731(3) 0.5894(2) 0.0372(12) Uani 1 1 d . . . H36 H 0.2390 0.6678 0.5519 0.045 Uiso 1 1 calc R . . C37 C 0.2561(4) 0.6054(3) 0.6237(2) 0.0371(12) Uani 1 1 d . . . H37 H 0.2240 0.5533 0.6098 0.044 Uiso 1 1 calc R . . C38 C 0.2942(4) 0.6136(3) 0.6785(2) 0.0328(11) Uani 1 1 d . . . H38 H 0.2869 0.5669 0.7018 0.039 Uiso 1 1 calc R . . C39 C 0.3428(4) 0.6886(3) 0.69987(18) 0.0270(10) Uani 1 1 d . . . H39 H 0.3710 0.6931 0.7372 0.032 Uiso 1 1 calc R . . C40 C 0.3491(3) 0.7566(3) 0.66568(18) 0.0254(10) Uani 1 1 d . . . C41 C 0.8041(4) 0.8908(3) 0.80763(17) 0.0251(10) Uani 1 1 d . . . C42 C 0.9151(4) 0.8823(3) 0.79851(19) 0.0334(11) Uani 1 1 d . . . H42 H 0.9380 0.8323 0.7819 0.040 Uiso 1 1 calc R . . C43 C 0.9916(4) 0.9466(3) 0.8137(2) 0.0385(13) Uani 1 1 d . . . H43 H 1.0665 0.9411 0.8068 0.046 Uiso 1 1 calc R . . C44 C 0.9597(4) 1.0188(3) 0.8390(2) 0.0420(13) Uani 1 1 d . . . H44 H 1.0129 1.0624 0.8496 0.050 Uiso 1 1 calc R . . C45 C 0.8510(4) 1.0277(3) 0.8488(2) 0.0389(12) Uani 1 1 d . . . H45 H 0.8296 1.0771 0.8666 0.047 Uiso 1 1 calc R . . C46 C 0.7725(4) 0.9642(3) 0.83277(19) 0.0325(11) Uani 1 1 d . . . H46 H 0.6972 0.9708 0.8390 0.039 Uiso 1 1 calc R . . C47 C 0.7539(4) 0.7107(3) 0.80734(18) 0.0254(10) Uani 1 1 d . . . C48 C 0.7084(4) 0.6371(3) 0.7817(2) 0.0359(12) Uani 1 1 d . . . H48 H 0.6544 0.6419 0.7501 0.043 Uiso 1 1 calc R . . C49 C 0.7407(4) 0.5576(3) 0.8014(2) 0.0422(13) Uani 1 1 d . . . H49 H 0.7091 0.5080 0.7835 0.051 Uiso 1 1 calc R . . C50 C 0.8192(4) 0.5507(3) 0.8472(2) 0.0409(13) Uani 1 1 d . . . H50 H 0.8414 0.4961 0.8611 0.049 Uiso 1 1 calc R . . C51 C 0.8657(4) 0.6224(3) 0.8729(2) 0.0394(13) Uani 1 1 d . . . H51 H 0.9210 0.6170 0.9039 0.047 Uiso 1 1 calc R . . C52 C 0.8323(4) 0.7024(3) 0.85377(19) 0.0320(11) Uani 1 1 d . . . H52 H 0.8629 0.7517 0.8724 0.038 Uiso 1 1 calc R . . C53 C 0.6265(5) 0.7690(4) 0.5204(3) 0.0587(17) Uani 1 1 d . . . C54 C 0.5653(5) 0.7120(4) 0.5431(3) 0.0630(18) Uani 1 1 d . . . H54 H 0.5600 0.7170 0.5804 0.076 Uiso 1 1 calc R . . C55 C 0.5095(6) 0.6461(5) 0.5138(3) 0.079(2) Uani 1 1 d . . . H55 H 0.4633 0.6091 0.5308 0.095 Uiso 1 1 calc R . . C56 C 0.5198(6) 0.6334(5) 0.4615(3) 0.075(2) Uani 1 1 d . . . H56 H 0.4843 0.5867 0.4418 0.090 Uiso 1 1 calc R . . C57 C 0.5841(6) 0.6911(5) 0.4374(3) 0.073(2) Uani 1 1 d . . . H57 H 0.5911 0.6843 0.4004 0.087 Uiso 1 1 calc R . . C58 C 0.6391(6) 0.7593(5) 0.4664(3) 0.0667(19) Uani 1 1 d . . . H58 H 0.6838 0.7978 0.4497 0.080 Uiso 1 1 calc R . . C59 C 0.6870(6) 0.8389(4) 0.5527(2) 0.0707(18) Uani 1 1 d . . . H59A H 0.6329 0.8814 0.5613 0.106 Uiso 1 1 calc R . . H59B H 0.7400 0.8658 0.5319 0.106 Uiso 1 1 calc R . . H59C H 0.7279 0.8156 0.5863 0.106 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01974(8) 0.02354(8) 0.01822(8) -0.00021(8) 0.00267(6) 0.00055(8) P1 0.0254(6) 0.0263(6) 0.0190(5) 0.0000(5) 0.0034(5) -0.0002(5) P2 0.0210(6) 0.0278(6) 0.0213(6) 0.0000(5) 0.0015(5) 0.0010(5) N2 0.0178(17) 0.027(2) 0.0202(18) -0.0014(15) 0.0045(15) 0.0024(15) N4 0.0188(19) 0.032(2) 0.0184(17) 0.0010(17) 0.0018(15) 0.0015(16) C1 0.029(2) 0.029(2) 0.023(2) -0.0035(19) 0.006(2) -0.002(2) N1 0.024(2) 0.030(2) 0.028(2) 0.0007(17) 0.0067(17) 0.0004(17) C2 0.021(2) 0.026(2) 0.021(2) -0.0020(18) 0.0038(18) 0.0054(19) C3 0.030(2) 0.023(2) 0.019(2) -0.0036(18) 0.0076(19) 0.0009(19) C4 0.029(3) 0.031(3) 0.024(2) -0.002(2) 0.006(2) 0.000(2) C5 0.042(3) 0.033(3) 0.035(3) -0.004(2) 0.010(2) -0.005(2) C6 0.053(3) 0.024(2) 0.038(3) -0.001(2) 0.014(2) 0.004(3) C7 0.040(3) 0.035(3) 0.028(3) 0.004(2) 0.005(2) 0.007(2) C8 0.035(3) 0.028(3) 0.026(2) 0.001(2) 0.006(2) 0.003(2) C9 0.028(2) 0.032(3) 0.023(2) 0.001(2) 0.001(2) 0.003(2) C10 0.032(3) 0.042(3) 0.042(3) 0.003(3) -0.005(2) 0.012(2) C11 0.024(3) 0.054(4) 0.040(3) -0.009(3) -0.003(2) 0.004(2) C12 0.025(2) 0.046(3) 0.033(3) -0.011(3) 0.006(2) -0.002(2) C13 0.025(2) 0.038(3) 0.026(2) -0.003(2) 0.0037(19) 0.000(2) C14 0.024(2) 0.032(3) 0.016(2) -0.0035(19) 0.0041(18) 0.004(2) C15 0.033(3) 0.031(3) 0.021(2) 0.001(2) -0.001(2) 0.000(2) C16 0.041(3) 0.037(3) 0.024(2) 0.002(2) -0.001(2) -0.003(2) C17 0.055(4) 0.036(3) 0.042(3) 0.004(3) -0.003(3) 0.007(3) C18 0.069(4) 0.045(3) 0.041(3) 0.018(3) -0.002(3) -0.012(3) C19 0.095(5) 0.060(4) 0.038(3) 0.018(3) 0.028(3) 0.005(4) C20 0.079(4) 0.048(4) 0.040(3) 0.006(3) 0.026(3) 0.012(3) C21 0.035(3) 0.027(3) 0.023(2) -0.004(2) 0.006(2) -0.004(2) C22 0.060(4) 0.039(3) 0.036(3) 0.001(2) -0.007(3) -0.012(3) C23 0.056(4) 0.059(4) 0.039(3) -0.013(3) -0.006(3) -0.015(3) C24 0.050(4) 0.047(4) 0.055(4) -0.027(3) 0.018(3) -0.020(3) C25 0.053(4) 0.030(3) 0.067(4) -0.011(3) 0.022(3) -0.002(3) C26 0.031(3) 0.036(3) 0.041(3) -0.004(2) 0.007(2) 0.002(2) C27 0.027(2) 0.037(3) 0.028(3) 0.000(2) 0.007(2) 0.004(2) N3 0.026(2) 0.034(2) 0.0218(18) 0.0013(17) 0.0036(16) -0.0003(18) C28 0.019(2) 0.030(2) 0.018(2) -0.0024(19) -0.0019(17) 0.0006(19) C29 0.017(2) 0.033(3) 0.021(2) -0.0005(19) 0.0051(18) 0.0080(19) C30 0.025(2) 0.037(3) 0.024(2) 0.002(2) 0.004(2) -0.003(2) C31 0.041(3) 0.041(3) 0.027(3) 0.009(2) 0.011(2) 0.000(2) C32 0.058(4) 0.051(4) 0.019(3) 0.008(2) -0.001(2) 0.001(3) C33 0.053(3) 0.042(3) 0.025(2) -0.005(2) -0.004(2) 0.005(3) C34 0.028(2) 0.034(3) 0.027(2) 0.000(2) -0.0011(19) 0.004(2) C35 0.023(2) 0.030(3) 0.027(2) -0.004(2) 0.005(2) 0.001(2) C36 0.038(3) 0.038(3) 0.033(3) -0.010(2) -0.001(2) -0.007(2) C37 0.035(3) 0.034(3) 0.042(3) -0.013(2) 0.006(2) -0.009(2) C38 0.027(3) 0.029(3) 0.045(3) 0.002(2) 0.014(2) -0.002(2) C39 0.023(2) 0.031(3) 0.027(2) -0.003(2) 0.005(2) 0.0024(19) C40 0.020(2) 0.028(2) 0.030(3) -0.006(2) 0.0062(19) -0.0007(19) C41 0.024(2) 0.029(2) 0.022(2) 0.0055(19) 0.0015(19) 0.0010(19) C42 0.029(3) 0.037(3) 0.035(3) 0.004(2) 0.008(2) 0.003(2) C43 0.020(2) 0.050(3) 0.045(3) 0.006(3) 0.003(2) -0.008(2) C44 0.035(3) 0.048(3) 0.043(3) -0.005(3) 0.006(2) -0.019(3) C45 0.041(3) 0.038(3) 0.039(3) -0.004(2) 0.013(2) -0.006(2) C46 0.028(3) 0.035(3) 0.035(3) -0.001(2) 0.007(2) -0.002(2) C47 0.023(2) 0.026(2) 0.028(2) -0.003(2) 0.008(2) 0.0019(19) C48 0.035(3) 0.038(3) 0.034(3) -0.003(2) 0.003(2) 0.002(2) C49 0.052(3) 0.031(3) 0.044(3) -0.003(2) 0.010(3) -0.001(3) C50 0.040(3) 0.031(3) 0.054(3) 0.011(3) 0.015(3) 0.011(2) C51 0.032(3) 0.046(3) 0.039(3) 0.011(3) 0.003(2) 0.004(2) C52 0.031(3) 0.033(3) 0.032(3) -0.001(2) 0.003(2) 0.000(2) C53 0.048(4) 0.072(5) 0.052(4) 0.017(3) -0.005(3) 0.016(3) C54 0.056(4) 0.071(5) 0.061(4) 0.011(4) 0.004(3) 0.018(4) C55 0.062(5) 0.096(6) 0.081(5) -0.012(5) 0.017(4) 0.006(4) C56 0.065(5) 0.087(6) 0.069(5) -0.011(4) -0.001(4) 0.004(4) C57 0.062(4) 0.096(6) 0.057(4) -0.007(4) -0.001(4) 0.019(4) C58 0.069(4) 0.080(5) 0.047(4) -0.004(4) -0.003(3) 0.018(4) C59 0.091(5) 0.069(4) 0.052(4) -0.007(4) 0.010(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N4 2.007(3) . ? Pt1 N2 2.007(3) . ? Pt1 P1 2.2341(11) . ? Pt1 P2 2.2436(11) . ? P1 C15 1.812(5) . ? P1 C1 1.820(5) . ? P1 C21 1.829(5) . ? P2 C47 1.806(4) . ? P2 C41 1.809(5) . ? P2 C27 1.820(5) . ? N2 N1 1.345(5) . ? N2 C2 1.477(5) . ? N4 N3 1.332(4) . ? N4 C28 1.473(5) . ? C1 N1 1.299(5) . ? C2 C14 1.532(6) . ? C2 C3 1.535(6) . ? C2 C28 1.597(6) . ? C3 C4 1.385(6) . ? C3 C8 1.404(6) . ? C4 C5 1.389(6) . ? C5 C6 1.383(7) . ? C6 C7 1.388(7) . ? C7 C8 1.391(6) . ? C8 C9 1.477(6) . ? C9 C10 1.388(6) . ? C9 C14 1.398(6) . ? C10 C11 1.387(7) . ? C11 C12 1.366(7) . ? C12 C13 1.393(6) . ? C13 C14 1.376(6) . ? C15 C16 1.375(6) . ? C15 C20 1.393(6) . ? C16 C17 1.399(6) . ? C17 C18 1.380(7) . ? C18 C19 1.359(8) . ? C19 C20 1.379(7) . ? C21 C22 1.389(7) . ? C21 C26 1.391(6) . ? C22 C23 1.389(7) . ? C23 C24 1.361(8) . ? C24 C25 1.382(8) . ? C25 C26 1.390(7) . ? C27 N3 1.309(5) . ? C28 C29 1.531(6) . ? C28 C40 1.536(6) . ? C29 C30 1.384(6) . ? C29 C34 1.394(6) . ? C30 C31 1.387(6) . ? C31 C32 1.379(7) . ? C32 C33 1.382(7) . ? C33 C34 1.391(6) . ? C34 C35 1.465(6) . ? C35 C36 1.384(6) . ? C35 C40 1.401(6) . ? C36 C37 1.383(7) . ? C37 C38 1.387(6) . ? C38 C39 1.389(6) . ? C39 C40 1.380(6) . ? C41 C46 1.395(6) . ? C41 C42 1.399(6) . ? C42 C43 1.383(6) . ? C43 C44 1.382(7) . ? C44 C45 1.378(7) . ? C45 C46 1.394(6) . ? C47 C52 1.391(6) . ? C47 C48 1.395(6) . ? C48 C49 1.379(7) . ? C49 C50 1.379(7) . ? C50 C51 1.375(7) . ? C51 C52 1.384(6) . ? C53 C54 1.342(8) . ? C53 C58 1.393(8) . ? C53 C59 1.490(8) . ? C54 C55 1.384(9) . ? C55 C56 1.352(9) . ? C56 C57 1.389(9) . ? C57 C58 1.405(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Pt1 N2 81.68(13) . . ? N4 Pt1 P1 164.00(10) . . ? N2 Pt1 P1 83.46(10) . . ? N4 Pt1 P2 82.71(10) . . ? N2 Pt1 P2 164.20(10) . . ? P1 Pt1 P2 112.31(4) . . ? C15 P1 C1 108.8(2) . . ? C15 P1 C21 104.4(2) . . ? C1 P1 C21 106.7(2) . . ? C15 P1 Pt1 124.88(16) . . ? C1 P1 Pt1 97.43(15) . . ? C21 P1 Pt1 113.31(15) . . ? C47 P2 C41 106.5(2) . . ? C47 P2 C27 107.0(2) . . ? C41 P2 C27 106.8(2) . . ? C47 P2 Pt1 117.13(15) . . ? C41 P2 Pt1 120.27(15) . . ? C27 P2 Pt1 97.61(15) . . ? N1 N2 C2 116.5(3) . . ? N1 N2 Pt1 122.1(3) . . ? C2 N2 Pt1 113.2(2) . . ? N3 N4 C28 117.6(3) . . ? N3 N4 Pt1 123.3(3) . . ? C28 N4 Pt1 114.7(2) . . ? N1 C1 P1 119.3(3) . . ? C1 N1 N2 116.7(4) . . ? N2 C2 C14 114.8(3) . . ? N2 C2 C3 112.7(3) . . ? C14 C2 C3 101.9(3) . . ? N2 C2 C28 105.2(3) . . ? C14 C2 C28 111.9(3) . . ? C3 C2 C28 110.5(3) . . ? C4 C3 C8 120.3(4) . . ? C4 C3 C2 129.9(4) . . ? C8 C3 C2 109.8(4) . . ? C3 C4 C5 118.6(4) . . ? C6 C5 C4 121.2(5) . . ? C5 C6 C7 120.6(5) . . ? C6 C7 C8 118.6(5) . . ? C7 C8 C3 120.6(4) . . ? C7 C8 C9 130.7(4) . . ? C3 C8 C9 108.7(4) . . ? C10 C9 C14 120.9(4) . . ? C10 C9 C8 130.1(4) . . ? C14 C9 C8 108.9(4) . . ? C11 C10 C9 118.5(5) . . ? C12 C11 C10 120.6(5) . . ? C11 C12 C13 121.3(5) . . ? C14 C13 C12 118.8(4) . . ? C13 C14 C9 119.9(4) . . ? C13 C14 C2 130.0(4) . . ? C9 C14 C2 110.1(4) . . ? C16 C15 C20 118.8(4) . . ? C16 C15 P1 120.9(4) . . ? C20 C15 P1 120.3(4) . . ? C15 C16 C17 120.0(5) . . ? C18 C17 C16 120.2(5) . . ? C19 C18 C17 119.8(5) . . ? C18 C19 C20 120.5(5) . . ? C19 C20 C15 120.7(5) . . ? C22 C21 C26 119.3(4) . . ? C22 C21 P1 121.1(4) . . ? C26 C21 P1 118.7(4) . . ? C21 C22 C23 119.8(5) . . ? C24 C23 C22 120.7(5) . . ? C23 C24 C25 120.3(5) . . ? C24 C25 C26 119.8(5) . . ? C25 C26 C21 120.0(5) . . ? N3 C27 P2 118.9(3) . . ? C27 N3 N4 116.5(4) . . ? N4 C28 C29 113.8(3) . . ? N4 C28 C40 112.5(3) . . ? C29 C28 C40 101.6(3) . . ? N4 C28 C2 104.9(3) . . ? C29 C28 C2 112.6(3) . . ? C40 C28 C2 111.6(3) . . ? C30 C29 C34 119.9(4) . . ? C30 C29 C28 129.8(4) . . ? C34 C29 C28 110.3(4) . . ? C29 C30 C31 119.3(4) . . ? C32 C31 C30 120.9(5) . . ? C31 C32 C33 120.4(5) . . ? C32 C33 C34 119.1(5) . . ? C33 C34 C29 120.5(4) . . ? C33 C34 C35 130.4(4) . . ? C29 C34 C35 109.0(4) . . ? C36 C35 C40 120.3(4) . . ? C36 C35 C34 130.7(4) . . ? C40 C35 C34 109.1(4) . . ? C37 C36 C35 119.4(4) . . ? C36 C37 C38 120.0(4) . . ? C37 C38 C39 121.2(5) . . ? C40 C39 C38 118.6(4) . . ? C39 C40 C35 120.5(4) . . ? C39 C40 C28 129.7(4) . . ? C35 C40 C28 109.8(4) . . ? C46 C41 C42 119.1(4) . . ? C46 C41 P2 119.0(3) . . ? C42 C41 P2 121.7(4) . . ? C43 C42 C41 120.0(5) . . ? C44 C43 C42 120.4(5) . . ? C45 C44 C43 120.3(5) . . ? C44 C45 C46 119.9(5) . . ? C45 C46 C41 120.2(4) . . ? C52 C47 C48 118.6(4) . . ? C52 C47 P2 122.2(3) . . ? C48 C47 P2 118.9(3) . . ? C49 C48 C47 121.1(5) . . ? C48 C49 C50 119.4(5) . . ? C51 C50 C49 120.4(5) . . ? C50 C51 C52 120.4(5) . . ? C51 C52 C47 120.0(4) . . ? C54 C53 C58 119.1(7) . . ? C54 C53 C59 121.3(6) . . ? C58 C53 C59 119.5(6) . . ? C53 C54 C55 122.0(7) . . ? C56 C55 C54 121.1(8) . . ? C55 C56 C57 117.7(7) . . ? C56 C57 C58 121.6(7) . . ? C53 C58 C57 118.4(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Pt1 P1 C15 137.8(4) . . . . ? N2 Pt1 P1 C15 115.9(2) . . . . ? P2 Pt1 P1 C15 -63.18(19) . . . . ? N4 Pt1 P1 C1 18.6(4) . . . . ? N2 Pt1 P1 C1 -3.23(17) . . . . ? P2 Pt1 P1 C1 177.64(14) . . . . ? N4 Pt1 P1 C21 -93.2(4) . . . . ? N2 Pt1 P1 C21 -115.05(19) . . . . ? P2 Pt1 P1 C21 65.83(17) . . . . ? N4 Pt1 P2 C47 -119.20(19) . . . . ? N2 Pt1 P2 C47 -110.3(4) . . . . ? P1 Pt1 P2 C47 66.49(17) . . . . ? N4 Pt1 P2 C41 108.92(19) . . . . ? N2 Pt1 P2 C41 117.8(4) . . . . ? P1 Pt1 P2 C41 -65.38(17) . . . . ? N4 Pt1 P2 C27 -5.66(18) . . . . ? N2 Pt1 P2 C27 3.2(4) . . . . ? P1 Pt1 P2 C27 -179.97(15) . . . . ? N4 Pt1 N2 N1 -165.1(3) . . . . ? P1 Pt1 N2 N1 9.0(3) . . . . ? P2 Pt1 N2 N1 -174.0(2) . . . . ? N4 Pt1 N2 C2 -17.9(3) . . . . ? P1 Pt1 N2 C2 156.2(3) . . . . ? P2 Pt1 N2 C2 -26.8(5) . . . . ? N2 Pt1 N4 N3 -167.8(3) . . . . ? P1 Pt1 N4 N3 170.3(2) . . . . ? P2 Pt1 N4 N3 9.7(3) . . . . ? N2 Pt1 N4 C28 -11.9(3) . . . . ? P1 Pt1 N4 C28 -33.8(6) . . . . ? P2 Pt1 N4 C28 165.6(3) . . . . ? C15 P1 C1 N1 -132.5(4) . . . . ? C21 P1 C1 N1 115.5(4) . . . . ? Pt1 P1 C1 N1 -1.6(4) . . . . ? P1 C1 N1 N2 8.5(5) . . . . ? C2 N2 N1 C1 -158.7(4) . . . . ? Pt1 N2 N1 C1 -12.5(5) . . . . ? N1 N2 C2 C14 -46.9(5) . . . . ? Pt1 N2 C2 C14 163.9(3) . . . . ? N1 N2 C2 C3 69.2(4) . . . . ? Pt1 N2 C2 C3 -80.0(4) . . . . ? N1 N2 C2 C28 -170.4(3) . . . . ? Pt1 N2 C2 C28 40.5(4) . . . . ? N2 C2 C3 C4 51.0(6) . . . . ? C14 C2 C3 C4 174.5(4) . . . . ? C28 C2 C3 C4 -66.4(6) . . . . ? N2 C2 C3 C8 -130.8(4) . . . . ? C14 C2 C3 C8 -7.3(4) . . . . ? C28 C2 C3 C8 111.8(4) . . . . ? C8 C3 C4 C5 -2.5(6) . . . . ? C2 C3 C4 C5 175.5(4) . . . . ? C3 C4 C5 C6 0.0(7) . . . . ? C4 C5 C6 C7 1.6(7) . . . . ? C5 C6 C7 C8 -0.6(7) . . . . ? C6 C7 C8 C3 -1.9(7) . . . . ? C6 C7 C8 C9 176.5(4) . . . . ? C4 C3 C8 C7 3.5(7) . . . . ? C2 C3 C8 C7 -174.9(4) . . . . ? C4 C3 C8 C9 -175.2(4) . . . . ? C2 C3 C8 C9 6.4(5) . . . . ? C7 C8 C9 C10 -3.7(8) . . . . ? C3 C8 C9 C10 174.7(5) . . . . ? C7 C8 C9 C14 178.8(5) . . . . ? C3 C8 C9 C14 -2.7(5) . . . . ? C14 C9 C10 C11 -0.9(7) . . . . ? C8 C9 C10 C11 -178.1(5) . . . . ? C9 C10 C11 C12 0.8(7) . . . . ? C10 C11 C12 C13 0.1(7) . . . . ? C11 C12 C13 C14 -0.9(7) . . . . ? C12 C13 C14 C9 0.8(6) . . . . ? C12 C13 C14 C2 -179.2(4) . . . . ? C10 C9 C14 C13 0.1(7) . . . . ? C8 C9 C14 C13 177.8(4) . . . . ? C10 C9 C14 C2 -179.9(4) . . . . ? C8 C9 C14 C2 -2.2(5) . . . . ? N2 C2 C14 C13 -52.3(6) . . . . ? C3 C2 C14 C13 -174.4(4) . . . . ? C28 C2 C14 C13 67.5(6) . . . . ? N2 C2 C14 C9 127.8(4) . . . . ? C3 C2 C14 C9 5.7(4) . . . . ? C28 C2 C14 C9 -112.5(4) . . . . ? C1 P1 C15 C16 123.0(4) . . . . ? C21 P1 C15 C16 -123.4(4) . . . . ? Pt1 P1 C15 C16 9.2(5) . . . . ? C1 P1 C15 C20 -57.9(5) . . . . ? C21 P1 C15 C20 55.7(5) . . . . ? Pt1 P1 C15 C20 -171.7(4) . . . . ? C20 C15 C16 C17 0.7(7) . . . . ? P1 C15 C16 C17 179.8(4) . . . . ? C15 C16 C17 C18 0.6(8) . . . . ? C16 C17 C18 C19 -1.7(9) . . . . ? C17 C18 C19 C20 1.6(10) . . . . ? C18 C19 C20 C15 -0.4(10) . . . . ? C16 C15 C20 C19 -0.8(9) . . . . ? P1 C15 C20 C19 -179.9(5) . . . . ? C15 P1 C21 C22 31.4(5) . . . . ? C1 P1 C21 C22 146.5(4) . . . . ? Pt1 P1 C21 C22 -107.5(4) . . . . ? C15 P1 C21 C26 -158.7(4) . . . . ? C1 P1 C21 C26 -43.6(4) . . . . ? Pt1 P1 C21 C26 62.5(4) . . . . ? C26 C21 C22 C23 1.2(8) . . . . ? P1 C21 C22 C23 171.1(4) . . . . ? C21 C22 C23 C24 -1.1(9) . . . . ? C22 C23 C24 C25 1.1(9) . . . . ? C23 C24 C25 C26 -1.2(8) . . . . ? C24 C25 C26 C21 1.3(8) . . . . ? C22 C21 C26 C25 -1.4(7) . . . . ? P1 C21 C26 C25 -171.5(4) . . . . ? C47 P2 C27 N3 124.8(4) . . . . ? C41 P2 C27 N3 -121.5(4) . . . . ? Pt1 P2 C27 N3 3.4(4) . . . . ? P2 C27 N3 N4 3.1(6) . . . . ? C28 N4 N3 C27 -165.2(4) . . . . ? Pt1 N4 N3 C27 -10.0(5) . . . . ? N3 N4 C28 C29 -43.5(5) . . . . ? Pt1 N4 C28 C29 159.2(3) . . . . ? N3 N4 C28 C40 71.4(5) . . . . ? Pt1 N4 C28 C40 -85.9(4) . . . . ? N3 N4 C28 C2 -167.0(3) . . . . ? Pt1 N4 C28 C2 35.6(4) . . . . ? N2 C2 C28 N4 -47.2(4) . . . . ? C14 C2 C28 N4 -172.5(3) . . . . ? C3 C2 C28 N4 74.7(4) . . . . ? N2 C2 C28 C29 -171.5(3) . . . . ? C14 C2 C28 C29 63.2(5) . . . . ? C3 C2 C28 C29 -49.6(4) . . . . ? N2 C2 C28 C40 74.9(4) . . . . ? C14 C2 C28 C40 -50.4(5) . . . . ? C3 C2 C28 C40 -163.2(3) . . . . ? N4 C28 C29 C30 -54.6(6) . . . . ? C40 C28 C29 C30 -175.8(4) . . . . ? C2 C28 C29 C30 64.7(6) . . . . ? N4 C28 C29 C34 124.0(4) . . . . ? C40 C28 C29 C34 2.8(4) . . . . ? C2 C28 C29 C34 -116.7(4) . . . . ? C34 C29 C30 C31 0.8(6) . . . . ? C28 C29 C30 C31 179.3(4) . . . . ? C29 C30 C31 C32 -1.0(7) . . . . ? C30 C31 C32 C33 0.4(8) . . . . ? C31 C32 C33 C34 0.5(8) . . . . ? C32 C33 C34 C29 -0.7(7) . . . . ? C32 C33 C34 C35 -177.8(5) . . . . ? C30 C29 C34 C33 0.0(7) . . . . ? C28 C29 C34 C33 -178.7(4) . . . . ? C30 C29 C34 C35 177.8(4) . . . . ? C28 C29 C34 C35 -1.0(5) . . . . ? C33 C34 C35 C36 -3.5(8) . . . . ? C29 C34 C35 C36 179.0(5) . . . . ? C33 C34 C35 C40 175.9(5) . . . . ? C29 C34 C35 C40 -1.5(5) . . . . ? C40 C35 C36 C37 -0.7(7) . . . . ? C34 C35 C36 C37 178.7(5) . . . . ? C35 C36 C37 C38 0.0(7) . . . . ? C36 C37 C38 C39 -0.8(7) . . . . ? C37 C38 C39 C40 2.2(7) . . . . ? C38 C39 C40 C35 -2.9(6) . . . . ? C38 C39 C40 C28 176.2(4) . . . . ? C36 C35 C40 C39 2.2(7) . . . . ? C34 C35 C40 C39 -177.3(4) . . . . ? C36 C35 C40 C28 -177.1(4) . . . . ? C34 C35 C40 C28 3.4(5) . . . . ? N4 C28 C40 C39 54.9(6) . . . . ? C29 C28 C40 C39 177.0(4) . . . . ? C2 C28 C40 C39 -62.7(6) . . . . ? N4 C28 C40 C35 -125.8(4) . . . . ? C29 C28 C40 C35 -3.8(4) . . . . ? C2 C28 C40 C35 116.5(4) . . . . ? C47 P2 C41 C46 -131.9(4) . . . . ? C27 P2 C41 C46 114.0(4) . . . . ? Pt1 P2 C41 C46 4.4(4) . . . . ? C47 P2 C41 C42 52.5(4) . . . . ? C27 P2 C41 C42 -61.5(4) . . . . ? Pt1 P2 C41 C42 -171.2(3) . . . . ? C46 C41 C42 C43 -0.8(7) . . . . ? P2 C41 C42 C43 174.7(4) . . . . ? C41 C42 C43 C44 1.3(7) . . . . ? C42 C43 C44 C45 -0.6(8) . . . . ? C43 C44 C45 C46 -0.7(8) . . . . ? C44 C45 C46 C41 1.2(7) . . . . ? C42 C41 C46 C45 -0.4(7) . . . . ? P2 C41 C46 C45 -176.1(4) . . . . ? C41 P2 C47 C52 26.7(4) . . . . ? C27 P2 C47 C52 140.7(4) . . . . ? Pt1 P2 C47 C52 -111.2(4) . . . . ? C41 P2 C47 C48 -160.0(4) . . . . ? C27 P2 C47 C48 -46.1(4) . . . . ? Pt1 P2 C47 C48 62.1(4) . . . . ? C52 C47 C48 C49 -0.5(7) . . . . ? P2 C47 C48 C49 -174.0(4) . . . . ? C47 C48 C49 C50 0.0(8) . . . . ? C48 C49 C50 C51 -0.4(8) . . . . ? C49 C50 C51 C52 1.5(8) . . . . ? C50 C51 C52 C47 -2.1(7) . . . . ? C48 C47 C52 C51 1.6(7) . . . . ? P2 C47 C52 C51 174.9(4) . . . . ? C58 C53 C54 C55 -3.3(10) . . . . ? C59 C53 C54 C55 -179.3(6) . . . . ? C53 C54 C55 C56 3.9(11) . . . . ? C54 C55 C56 C57 -2.9(11) . . . . ? C55 C56 C57 C58 1.5(10) . . . . ? C54 C53 C58 C57 1.8(9) . . . . ? C59 C53 C58 C57 177.9(6) . . . . ? C56 C57 C58 C53 -1.0(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.956 _refine_diff_density_min -1.232 _refine_diff_density_rms 0.131 #===End