Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Paul Kelly' _publ_contact_author_address ; Department of Chemistry Loughborough University Loughborough Leicestershire LE11 3TU ; _publ_contact_author_email P.F.KELLY@LBORO.AC.UK _publ_section_title ; The first examples of metal-mediated addition of a phosphorus imine to nitriles; the preparation and X-ray crystal structures of [PtCl4{NH=C(Et)N=PPh3}2] and [PtCl2(EtCN){NH=C(Et)N=PPh3}] ; loop_ _publ_author_name 'Paul Kelly' 'Nadezhda A. Bokach' 'Matti Haukka' 'Vadim Yu Kukushkin' 'Armando J. L. Pombeiro' data_structure_2b _database_code_depnum_ccdc_archive 'CCDC 264823' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H26 Cl2 N3 P Pt' _chemical_formula_sum 'C24 H26 Cl2 N3 P Pt' _chemical_formula_weight 653.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.0217(3) _cell_length_b 8.7854(5) _cell_length_c 24.7704(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.045(3) _cell_angle_gamma 90.00 _cell_volume 4792.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 6.163 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.20501 _exptl_absorpt_correction_T_max 0.29576 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14991 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 26.35 _reflns_number_total 4744 _reflns_number_gt 3846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.6.14 (Sheldrick, 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The NH hydrogen was located from the difference Fourien map and refined isotropically. Other hydrogens were placed in idealized position and constrained to ride on their parent atom. ; _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^)+(0.0255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4744 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.054561(8) 0.272030(19) 0.047562(8) 0.01892(7) Uani 1 1 d . . . Cl1 Cl 0.10680(5) 0.39232(12) -0.02088(6) 0.0259(3) Uani 1 1 d . . . Cl2 Cl 0.00344(6) 0.15295(14) 0.11659(6) 0.0351(3) Uani 1 1 d . . . P1 P 0.15821(6) 0.59415(13) 0.16425(6) 0.0206(3) Uani 1 1 d . . . N1 N 0.08011(16) 0.0701(4) 0.02011(18) 0.0218(10) Uani 1 1 d . . . N2 N 0.02659(16) 0.4745(4) 0.07333(18) 0.0207(9) Uani 1 1 d . . . H2 H -0.0075 0.5010 0.0611 0.031 Uiso 1 1 d . . . N3 N 0.11037(17) 0.5278(4) 0.12305(18) 0.0222(10) Uani 1 1 d . . . C1 C 0.0928(2) -0.0500(5) 0.0058(2) 0.0246(12) Uani 1 1 d . . . C2 C 0.1081(2) -0.2020(5) -0.0133(3) 0.0396(16) Uani 1 1 d . . . H2A H 0.0849 -0.2217 -0.0468 0.048 Uiso 1 1 calc R . . H2B H 0.0943 -0.2765 0.0141 0.048 Uiso 1 1 calc R . . C3 C 0.1727(2) -0.2304(5) -0.0243(3) 0.0391(16) Uani 1 1 d . . . H3A H 0.1853 -0.1714 -0.0560 0.059 Uiso 1 1 calc R . . H3B H 0.1788 -0.3391 -0.0314 0.059 Uiso 1 1 calc R . . H3C H 0.1970 -0.1998 0.0070 0.059 Uiso 1 1 calc R . . C4 C 0.0557(2) 0.5697(5) 0.1035(2) 0.0201(11) Uani 1 1 d . . . C5 C 0.0276(2) 0.7243(5) 0.1151(2) 0.0230(11) Uani 1 1 d . . . H5A H 0.0596 0.8032 0.1127 0.028 Uiso 1 1 calc R . . H5B H -0.0032 0.7468 0.0872 0.028 Uiso 1 1 calc R . . C6 C -0.0020(2) 0.7331(5) 0.1703(2) 0.0303(13) Uani 1 1 d . . . H6A H -0.0384 0.6692 0.1707 0.045 Uiso 1 1 calc R . . H6B H -0.0132 0.8388 0.1781 0.045 Uiso 1 1 calc R . . H6C H 0.0266 0.6970 0.1978 0.045 Uiso 1 1 calc R . . C7 C 0.2309(2) 0.5219(5) 0.1430(2) 0.0216(11) Uani 1 1 d . . . C8 C 0.2345(2) 0.4236(5) 0.0990(2) 0.0237(12) Uani 1 1 d . . . H8 H 0.1987 0.3971 0.0797 0.028 Uiso 1 1 calc R . . C9 C 0.2894(2) 0.3646(5) 0.0831(2) 0.0290(13) Uani 1 1 d . . . H9 H 0.2913 0.2977 0.0531 0.035 Uiso 1 1 calc R . . C10 C 0.3417(2) 0.4022(5) 0.1107(2) 0.0297(13) Uani 1 1 d . . . H10 H 0.3795 0.3591 0.1003 0.036 Uiso 1 1 calc R . . C11 C 0.3388(2) 0.5018(6) 0.1530(2) 0.0331(14) Uani 1 1 d . . . H11 H 0.3751 0.5291 0.1714 0.040 Uiso 1 1 calc R . . C12 C 0.2844(2) 0.5633(6) 0.1695(2) 0.0303(13) Uani 1 1 d . . . H12 H 0.2832 0.6334 0.1986 0.036 Uiso 1 1 calc R . . C13 C 0.1659(2) 0.7988(5) 0.1681(2) 0.0233(11) Uani 1 1 d . . . C14 C 0.1936(2) 0.8724(6) 0.1253(2) 0.0305(13) Uani 1 1 d . . . H14 H 0.2148 0.8147 0.0989 0.037 Uiso 1 1 calc R . . C15 C 0.1908(2) 1.0281(6) 0.1205(3) 0.0319(14) Uani 1 1 d . . . H15 H 0.2099 1.0775 0.0910 0.038 Uiso 1 1 calc R . . C16 C 0.1603(2) 1.1121(6) 0.1586(3) 0.0329(14) Uani 1 1 d . . . H16 H 0.1579 1.2196 0.1551 0.040 Uiso 1 1 calc R . . C17 C 0.1335(2) 1.0405(6) 0.2016(3) 0.0354(14) Uani 1 1 d . . . H17 H 0.1128 1.0989 0.2280 0.043 Uiso 1 1 calc R . . C18 C 0.1364(2) 0.8846(5) 0.2067(2) 0.0289(13) Uani 1 1 d . . . H18 H 0.1180 0.8360 0.2368 0.035 Uiso 1 1 calc R . . C19 C 0.1421(2) 0.5256(5) 0.2314(2) 0.0231(12) Uani 1 1 d . . . C20 C 0.1744(2) 0.5731(6) 0.2769(2) 0.0282(13) Uani 1 1 d . . . H20 H 0.2064 0.6448 0.2733 0.034 Uiso 1 1 calc R . . C21 C 0.1597(2) 0.5155(6) 0.3268(2) 0.0323(13) Uani 1 1 d . . . H21 H 0.1821 0.5467 0.3576 0.039 Uiso 1 1 calc R . . C22 C 0.1127(2) 0.4127(5) 0.3325(2) 0.0309(13) Uani 1 1 d . . . H22 H 0.1027 0.3745 0.3673 0.037 Uiso 1 1 calc R . . C23 C 0.0801(2) 0.3652(5) 0.2880(2) 0.0309(13) Uani 1 1 d . . . H23 H 0.0480 0.2939 0.2920 0.037 Uiso 1 1 calc R . . C24 C 0.0945(2) 0.4219(5) 0.2376(2) 0.0258(12) Uani 1 1 d . . . H24 H 0.0719 0.3902 0.2069 0.031 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 0.01902(11) 0.01526(10) 0.02247(12) -0.00385(8) -0.00060(8) 0.00259(7) Cl1 0.0271(6) 0.0180(6) 0.0325(8) -0.0013(5) 0.0057(6) 0.0017(5) Cl2 0.0434(8) 0.0255(7) 0.0364(9) 0.0028(6) 0.0138(7) 0.0059(5) P1 0.0240(7) 0.0162(6) 0.0216(8) -0.0010(5) 0.0011(6) 0.0001(5) N1 0.015(2) 0.026(2) 0.025(3) -0.0023(19) 0.0037(19) 0.0000(16) N2 0.014(2) 0.024(2) 0.024(3) -0.0040(18) 0.0004(18) 0.0020(16) N3 0.026(2) 0.016(2) 0.025(3) -0.0066(18) -0.004(2) 0.0030(16) C1 0.018(3) 0.027(3) 0.029(3) -0.002(2) 0.003(2) -0.005(2) C2 0.029(3) 0.019(3) 0.071(5) -0.014(3) 0.018(3) -0.001(2) C3 0.028(3) 0.024(3) 0.065(5) -0.008(3) 0.010(3) 0.003(2) C4 0.024(3) 0.020(2) 0.016(3) 0.001(2) 0.003(2) 0.0034(19) C5 0.026(3) 0.017(2) 0.026(3) -0.001(2) -0.003(2) 0.0051(19) C6 0.028(3) 0.024(3) 0.038(4) -0.007(2) 0.008(3) 0.000(2) C7 0.024(3) 0.019(2) 0.022(3) 0.006(2) 0.001(2) -0.0015(19) C8 0.025(3) 0.021(3) 0.025(3) -0.001(2) 0.001(2) -0.0034(19) C9 0.033(3) 0.022(3) 0.032(4) -0.003(2) 0.008(3) 0.000(2) C10 0.028(3) 0.025(3) 0.037(4) 0.005(2) 0.002(3) 0.008(2) C11 0.022(3) 0.043(3) 0.035(4) -0.002(3) -0.005(3) 0.003(2) C12 0.027(3) 0.033(3) 0.031(4) -0.007(2) 0.004(3) 0.004(2) C13 0.021(2) 0.024(3) 0.025(3) -0.003(2) 0.000(2) -0.0016(19) C14 0.029(3) 0.031(3) 0.031(4) 0.003(2) 0.004(3) 0.002(2) C15 0.031(3) 0.025(3) 0.040(4) 0.015(3) 0.000(3) -0.004(2) C16 0.039(3) 0.017(3) 0.043(4) -0.001(2) -0.006(3) 0.002(2) C17 0.045(3) 0.024(3) 0.038(4) -0.007(3) 0.003(3) 0.004(2) C18 0.031(3) 0.027(3) 0.028(4) -0.004(2) 0.005(3) 0.000(2) C19 0.024(3) 0.019(2) 0.026(3) 0.000(2) 0.002(2) 0.0023(19) C20 0.028(3) 0.030(3) 0.027(4) 0.003(2) 0.000(3) 0.002(2) C21 0.034(3) 0.034(3) 0.030(4) 0.002(3) -0.005(3) 0.007(2) C22 0.041(3) 0.029(3) 0.022(3) 0.008(2) 0.011(3) 0.009(2) C23 0.034(3) 0.019(3) 0.040(4) 0.001(2) 0.009(3) 0.001(2) C24 0.028(3) 0.018(2) 0.032(4) -0.003(2) 0.003(3) 0.0018(19) _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 1.982(4) . ? Pt1 N2 1.988(4) . ? Pt1 Cl2 2.2997(14) . ? Pt1 Cl1 2.3058(13) . ? P1 N3 1.578(4) . ? P1 C7 1.801(5) . ? P1 C19 1.805(6) . ? P1 C13 1.808(5) . ? N1 C1 1.148(6) . ? N2 C4 1.292(6) . ? N2 H2 0.8411 . ? N3 C4 1.348(6) . ? C1 C2 1.455(7) . ? C2 C3 1.470(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.520(6) . ? C5 C6 1.517(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.393(7) . ? C7 C12 1.396(7) . ? C8 C9 1.372(7) . ? C8 H8 0.9500 . ? C9 C10 1.379(7) . ? C9 H9 0.9500 . ? C10 C11 1.367(8) . ? C10 H10 0.9500 . ? C11 C12 1.378(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.380(7) . ? C13 C14 1.385(8) . ? C14 C15 1.374(7) . ? C14 H14 0.9500 . ? C15 C16 1.373(8) . ? C15 H15 0.9500 . ? C16 C17 1.371(8) . ? C16 H16 0.9500 . ? C17 C18 1.377(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.395(7) . ? C19 C24 1.396(6) . ? C20 C21 1.374(8) . ? C20 H20 0.9500 . ? C21 C22 1.382(7) . ? C21 H21 0.9500 . ? C22 C23 1.379(8) . ? C22 H22 0.9500 . ? C23 C24 1.381(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? 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 178.05(16) . . ? N1 Pt1 Cl2 89.27(13) . . ? N2 Pt1 Cl2 90.93(13) . . ? N1 Pt1 Cl1 90.92(12) . . ? N2 Pt1 Cl1 88.90(13) . . ? Cl2 Pt1 Cl1 179.26(5) . . ? N3 P1 C7 105.9(2) . . ? N3 P1 C19 110.0(2) . . ? C7 P1 C19 109.1(2) . . ? N3 P1 C13 117.7(2) . . ? C7 P1 C13 106.4(2) . . ? C19 P1 C13 107.5(2) . . ? C1 N1 Pt1 176.6(4) . . ? C4 N2 Pt1 127.7(3) . . ? C4 N2 H2 118.1 . . ? Pt1 N2 H2 114.1 . . ? C4 N3 P1 136.6(3) . . ? N1 C1 C2 179.0(6) . . ? C1 C2 C3 116.2(4) . . ? C1 C2 H2A 108.2 . . ? C3 C2 H2A 108.2 . . ? C1 C2 H2B 108.2 . . ? C3 C2 H2B 108.2 . . ? H2A C2 H2B 107.4 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 N3 118.2(4) . . ? N2 C4 C5 119.1(4) . . ? N3 C4 C5 122.7(4) . . ? C6 C5 C4 113.0(4) . . ? C6 C5 H5A 109.0 . . ? C4 C5 H5A 109.0 . . ? C6 C5 H5B 109.0 . . ? C4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 118.7(5) . . ? C8 C7 P1 120.0(4) . . ? C12 C7 P1 121.3(4) . . ? C9 C8 C7 120.6(5) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 120.2(5) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.6(5) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 121.3(5) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 119.6(5) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C18 C13 C14 118.9(5) . . ? C18 C13 P1 122.4(4) . . ? C14 C13 P1 117.7(4) . . ? C15 C14 C13 120.7(5) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 119.9(5) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 119.9(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.5(5) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C13 120.1(5) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C20 C19 C24 119.3(5) . . ? C20 C19 P1 122.9(4) . . ? C24 C19 P1 117.8(4) . . ? C21 C20 C19 119.7(5) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 120.7(5) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 120.3(5) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 119.5(5) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C23 C24 C19 120.5(5) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.232 _refine_diff_density_min -1.271 _refine_diff_density_rms 0.159 #===END======================================================================== #CCDC 264824 data_structure_3 _database_code_depnum_ccdc_archive 'CCDC 264824' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 Cl4 N4 P2 Pt' _chemical_formula_sum 'C42 H42 Cl4 N4 P2 Pt' _chemical_formula_weight 1001.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1210(2) _cell_length_b 13.7987(4) _cell_length_c 15.6217(4) _cell_angle_alpha 73.8900(10) _cell_angle_beta 86.897(2) _cell_angle_gamma 89.625(2) _cell_volume 2092.85(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 3.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5721 _exptl_absorpt_correction_T_max 0.8049 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12933 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.06 _reflns_number_total 7363 _reflns_number_gt 5672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.6.14 (Bruker AXS, 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. NH hydrogens were located from the difference Fourien map but were not refined Other hydrogens were placed in idealized position and constrained to ride on their parent atom. ; _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^)+(0.0288P)^2^+0.9156P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7363 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.0000 0.0000 0.5000 0.01282(8) Uani 1 2 d S . . Cl1 Cl -0.21153(11) -0.04882(10) 0.47763(8) 0.0229(3) Uani 1 1 d . . . Cl2 Cl -0.05837(11) 0.16551(9) 0.43063(7) 0.0216(3) Uani 1 1 d . . . P1 P 0.19153(11) 0.06784(10) 0.18823(7) 0.0152(3) Uani 1 1 d . . . N1 N 0.0721(4) -0.0024(3) 0.3770(2) 0.0168(9) Uani 1 1 d . . . H1 H 0.1239 0.0504 0.3564 0.000(10) Uiso 1 1 d R . . N2 N 0.1245(3) -0.0393(3) 0.2408(2) 0.0165(9) Uani 1 1 d . . . C1 C 0.0691(4) -0.0615(4) 0.3243(3) 0.0148(10) Uani 1 1 d . . . C2 C 0.0005(5) -0.1636(4) 0.3567(3) 0.0242(12) Uani 1 1 d . . . H2A H 0.0682 -0.2170 0.3697 0.029 Uiso 1 1 calc R . . H2B H -0.0518 -0.1672 0.4129 0.029 Uiso 1 1 calc R . . C3 C -0.0899(7) -0.1833(6) 0.2896(4) 0.065(2) Uani 1 1 d . . . H3A H -0.1616 -0.1340 0.2801 0.097 Uiso 1 1 calc R . . H3B H -0.1273 -0.2516 0.3121 0.097 Uiso 1 1 calc R . . H3C H -0.0394 -0.1771 0.2330 0.097 Uiso 1 1 calc R . . C4 C 0.0750(4) 0.1692(4) 0.1746(3) 0.0162(10) Uani 1 1 d . . . C5 C 0.1137(4) 0.2699(4) 0.1397(3) 0.0218(11) Uani 1 1 d . . . H5 H 0.2046 0.2869 0.1253 0.026 Uiso 1 1 calc R . . C6 C 0.0193(5) 0.3449(4) 0.1261(3) 0.0256(12) Uani 1 1 d . . . H6 H 0.0461 0.4136 0.1042 0.031 Uiso 1 1 calc R . . C7 C -0.1137(5) 0.3208(4) 0.1442(3) 0.0234(12) Uani 1 1 d . . . H7 H -0.1780 0.3726 0.1339 0.028 Uiso 1 1 calc R . . C8 C -0.1524(5) 0.2207(4) 0.1775(3) 0.0228(11) Uani 1 1 d . . . H8 H -0.2437 0.2040 0.1895 0.027 Uiso 1 1 calc R . . C9 C -0.0594(4) 0.1452(4) 0.1934(3) 0.0190(11) Uani 1 1 d . . . H9 H -0.0867 0.0768 0.2171 0.023 Uiso 1 1 calc R . . C10 C 0.3357(4) 0.1000(4) 0.2378(3) 0.0162(10) Uani 1 1 d . . . C11 C 0.4504(5) 0.0437(4) 0.2340(3) 0.0241(11) Uani 1 1 d . . . H11 H 0.4531 -0.0048 0.2011 0.029 Uiso 1 1 calc R . . C12 C 0.5599(5) 0.0590(4) 0.2783(3) 0.0294(13) Uani 1 1 d . . . H12 H 0.6370 0.0197 0.2767 0.035 Uiso 1 1 calc R . . C13 C 0.5583(5) 0.1306(4) 0.3246(3) 0.0243(12) Uani 1 1 d . . . H13 H 0.6340 0.1405 0.3547 0.029 Uiso 1 1 calc R . . C14 C 0.4481(5) 0.1873(4) 0.3274(3) 0.0228(11) Uani 1 1 d . . . H14 H 0.4478 0.2376 0.3584 0.027 Uiso 1 1 calc R . . C15 C 0.3348(5) 0.1716(4) 0.2844(3) 0.0213(11) Uani 1 1 d . . . H15 H 0.2577 0.2103 0.2875 0.026 Uiso 1 1 calc R . . C16 C 0.2447(4) 0.0594(4) 0.0795(3) 0.0191(11) Uani 1 1 d . . . C17 C 0.1883(5) -0.0124(4) 0.0448(3) 0.0290(12) Uani 1 1 d . . . H17 H 0.1280 -0.0613 0.0808 0.035 Uiso 1 1 calc R . . C18 C 0.2207(5) -0.0122(5) -0.0427(4) 0.0397(15) Uani 1 1 d . . . H18 H 0.1829 -0.0611 -0.0667 0.048 Uiso 1 1 calc R . . C19 C 0.3090(5) 0.0599(5) -0.0951(3) 0.0374(15) Uani 1 1 d . . . H19 H 0.3297 0.0605 -0.1553 0.045 Uiso 1 1 calc R . . C20 C 0.3665(5) 0.1302(5) -0.0614(3) 0.0353(14) Uani 1 1 d . . . H20 H 0.4287 0.1776 -0.0973 0.042 Uiso 1 1 calc R . . C21 C 0.3331(5) 0.1316(4) 0.0263(3) 0.0299(13) Uani 1 1 d . . . H21 H 0.3702 0.1814 0.0496 0.036 Uiso 1 1 calc R . . Pt1B Pt -0.5000 0.5000 0.0000 0.01483(8) Uani 1 2 d S . . Cl1B Cl -0.27710(11) 0.52864(10) 0.01049(8) 0.0230(3) Uani 1 1 d . . . Cl2B Cl -0.49803(11) 0.35221(9) 0.11692(7) 0.0217(3) Uani 1 1 d . . . P1B P -0.55788(11) 0.61065(10) 0.28805(8) 0.0161(3) Uani 1 1 d . . . N1B N -0.5309(4) 0.5688(3) 0.0980(3) 0.0178(9) Uani 1 1 d . . . H1B H -0.484(4) 0.541(3) 0.138(3) 0.000(11) Uiso 1 1 d . . . N2B N -0.6019(4) 0.6696(3) 0.1905(2) 0.0205(9) Uani 1 1 d . . . C1B C -0.6048(4) 0.6394(4) 0.1156(3) 0.0174(10) Uani 1 1 d . . . C2B C -0.7008(5) 0.6964(4) 0.0498(3) 0.0249(12) Uani 1 1 d . . . H2B1 H -0.6966 0.6701 -0.0031 0.030 Uiso 1 1 calc R . . H2B2 H -0.6745 0.7685 0.0298 0.030 Uiso 1 1 calc R . . C3B C -0.8426(5) 0.6872(5) 0.0899(4) 0.0387(15) Uani 1 1 d . . . H3B1 H -0.8690 0.6159 0.1100 0.058 Uiso 1 1 calc R . . H3B2 H -0.9020 0.7239 0.0446 0.058 Uiso 1 1 calc R . . H3B3 H -0.8480 0.7159 0.1407 0.058 Uiso 1 1 calc R . . C4B C -0.5351(4) 0.7026(4) 0.3477(3) 0.0161(10) Uani 1 1 d . . . C5B C -0.6307(5) 0.7771(4) 0.3436(3) 0.0217(11) Uani 1 1 d . . . H5B H -0.7019 0.7824 0.3053 0.026 Uiso 1 1 calc R . . C6B C -0.6211(5) 0.8435(4) 0.3959(3) 0.0239(11) Uani 1 1 d . . . H6B H -0.6869 0.8932 0.3947 0.029 Uiso 1 1 calc R . . C7B C -0.5151(5) 0.8367(4) 0.4495(3) 0.0237(11) Uani 1 1 d . . . H7B H -0.5076 0.8826 0.4845 0.028 Uiso 1 1 calc R . . C8B C -0.4208(5) 0.7642(4) 0.4525(3) 0.0226(11) Uani 1 1 d . . . H8B H -0.3477 0.7607 0.4888 0.027 Uiso 1 1 calc R . . C9B C -0.4319(4) 0.6961(4) 0.4028(3) 0.0205(11) Uani 1 1 d . . . H9B H -0.3680 0.6445 0.4068 0.025 Uiso 1 1 calc R . . C10B C -0.6865(4) 0.5242(4) 0.3492(3) 0.0165(10) Uani 1 1 d . . . C11B C -0.7366(4) 0.5291(4) 0.4329(3) 0.0204(11) Uani 1 1 d . . . H11B H -0.7036 0.5785 0.4583 0.025 Uiso 1 1 calc R . . C12B C -0.8341(4) 0.4623(4) 0.4789(3) 0.0235(12) Uani 1 1 d . . . H12B H -0.8692 0.4667 0.5353 0.028 Uiso 1 1 calc R . . C13B C -0.8808(5) 0.3889(4) 0.4429(3) 0.0258(12) Uani 1 1 d . . . H13B H -0.9464 0.3420 0.4751 0.031 Uiso 1 1 calc R . . C14B C -0.8313(4) 0.3840(4) 0.3593(3) 0.0247(12) Uani 1 1 d . . . H14B H -0.8646 0.3343 0.3344 0.030 Uiso 1 1 calc R . . C15B C -0.7343(5) 0.4508(4) 0.3121(3) 0.0235(12) Uani 1 1 d . . . H15B H -0.7006 0.4468 0.2553 0.028 Uiso 1 1 calc R . . C16B C -0.4074(4) 0.5373(4) 0.2969(3) 0.0194(11) Uani 1 1 d . . . C17B C -0.4011(5) 0.4410(4) 0.3545(3) 0.0234(11) Uani 1 1 d . . . H17B H -0.4774 0.4119 0.3902 0.028 Uiso 1 1 calc R . . C18B C -0.2850(5) 0.3867(4) 0.3605(3) 0.0302(13) Uani 1 1 d . . . H18B H -0.2818 0.3208 0.4001 0.036 Uiso 1 1 calc R . . C19B C -0.1747(5) 0.4282(5) 0.3093(4) 0.0377(15) Uani 1 1 d . . . H19B H -0.0950 0.3908 0.3132 0.045 Uiso 1 1 calc R . . C20B C -0.1790(5) 0.5240(5) 0.2520(4) 0.0367(15) Uani 1 1 d . . . H20B H -0.1018 0.5524 0.2169 0.044 Uiso 1 1 calc R . . C21B C -0.2960(4) 0.5803(5) 0.2448(3) 0.0275(13) Uani 1 1 d . . . H21B H -0.2988 0.6463 0.2052 0.033 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 0.01276(14) 0.01194(16) 0.01234(13) -0.00096(11) -0.00080(9) -0.00124(10) Cl1 0.0146(6) 0.0300(8) 0.0245(6) -0.0075(6) -0.0026(5) -0.0052(5) Cl2 0.0292(6) 0.0140(7) 0.0192(6) -0.0008(5) -0.0029(5) 0.0037(5) P1 0.0164(6) 0.0145(7) 0.0141(6) -0.0034(5) 0.0012(5) -0.0008(5) N1 0.020(2) 0.010(2) 0.018(2) -0.0016(17) 0.0027(16) -0.0057(17) N2 0.017(2) 0.015(2) 0.019(2) -0.0063(17) 0.0013(15) -0.0025(17) C1 0.016(2) 0.013(3) 0.014(2) -0.001(2) -0.0034(18) 0.0024(19) C2 0.026(3) 0.021(3) 0.026(3) -0.009(2) 0.006(2) -0.004(2) C3 0.094(5) 0.059(5) 0.034(4) 0.000(3) -0.009(3) -0.055(5) C4 0.020(2) 0.016(3) 0.011(2) -0.003(2) -0.0026(18) 0.004(2) C5 0.015(2) 0.024(3) 0.024(3) -0.003(2) 0.0028(19) 0.000(2) C6 0.030(3) 0.018(3) 0.024(3) 0.002(2) -0.001(2) 0.001(2) C7 0.025(3) 0.030(3) 0.017(2) -0.008(2) -0.004(2) 0.007(2) C8 0.018(3) 0.030(3) 0.018(2) -0.002(2) -0.0023(19) 0.000(2) C9 0.017(2) 0.020(3) 0.018(2) -0.003(2) -0.0018(19) -0.001(2) C10 0.017(2) 0.016(3) 0.014(2) -0.001(2) 0.0019(18) -0.003(2) C11 0.024(3) 0.023(3) 0.029(3) -0.011(2) -0.003(2) 0.001(2) C12 0.019(3) 0.034(4) 0.035(3) -0.009(3) -0.001(2) 0.004(2) C13 0.018(3) 0.034(3) 0.020(3) -0.006(2) -0.001(2) -0.010(2) C14 0.029(3) 0.025(3) 0.017(2) -0.011(2) -0.005(2) -0.001(2) C15 0.020(3) 0.022(3) 0.020(3) -0.003(2) 0.001(2) 0.002(2) C16 0.020(2) 0.023(3) 0.014(2) -0.005(2) -0.0001(19) 0.002(2) C17 0.032(3) 0.033(4) 0.026(3) -0.014(3) -0.003(2) 0.003(2) C18 0.042(3) 0.055(4) 0.031(3) -0.025(3) -0.005(3) 0.004(3) C19 0.040(3) 0.054(4) 0.019(3) -0.012(3) -0.001(2) 0.017(3) C20 0.039(3) 0.040(4) 0.023(3) -0.003(3) 0.005(2) 0.003(3) C21 0.032(3) 0.033(4) 0.024(3) -0.009(3) 0.006(2) -0.007(3) Pt1B 0.01675(14) 0.01466(16) 0.01117(14) -0.00053(11) -0.00032(10) 0.00243(11) Cl1B 0.0177(6) 0.0241(7) 0.0237(6) -0.0008(5) -0.0021(5) 0.0003(5) Cl2B 0.0262(6) 0.0178(7) 0.0166(6) 0.0025(5) 0.0004(5) 0.0033(5) P1B 0.0161(6) 0.0168(7) 0.0153(6) -0.0040(5) -0.0020(5) 0.0018(5) N1B 0.022(2) 0.017(2) 0.012(2) 0.0003(18) -0.0093(18) 0.0106(18) N2B 0.022(2) 0.022(3) 0.018(2) -0.0073(18) -0.0031(16) 0.0034(18) C1B 0.016(2) 0.017(3) 0.017(2) -0.001(2) -0.0011(18) -0.002(2) C2B 0.030(3) 0.028(3) 0.017(3) -0.006(2) -0.003(2) 0.009(2) C3B 0.031(3) 0.054(4) 0.034(3) -0.016(3) -0.006(2) 0.017(3) C4B 0.019(2) 0.016(3) 0.012(2) -0.001(2) 0.0016(18) -0.003(2) C5B 0.022(3) 0.024(3) 0.021(3) -0.007(2) -0.005(2) 0.002(2) C6B 0.029(3) 0.018(3) 0.026(3) -0.008(2) -0.005(2) 0.009(2) C7B 0.030(3) 0.023(3) 0.021(3) -0.011(2) -0.002(2) -0.002(2) C8B 0.026(3) 0.021(3) 0.019(3) -0.003(2) -0.004(2) -0.001(2) C9B 0.020(3) 0.019(3) 0.021(2) -0.003(2) -0.0016(19) 0.001(2) C10B 0.012(2) 0.019(3) 0.018(2) -0.005(2) -0.0018(18) 0.0017(19) C11B 0.020(3) 0.020(3) 0.021(3) -0.004(2) -0.005(2) 0.000(2) C12B 0.022(3) 0.029(3) 0.019(3) -0.005(2) 0.002(2) 0.002(2) C13B 0.017(3) 0.020(3) 0.037(3) -0.002(2) 0.000(2) 0.001(2) C14B 0.018(3) 0.021(3) 0.039(3) -0.014(2) -0.006(2) 0.001(2) C15B 0.022(3) 0.028(3) 0.021(3) -0.009(2) -0.003(2) 0.000(2) C16B 0.019(2) 0.023(3) 0.019(2) -0.011(2) -0.0053(19) 0.003(2) C17B 0.026(3) 0.019(3) 0.029(3) -0.013(2) -0.008(2) 0.007(2) C18B 0.033(3) 0.030(3) 0.033(3) -0.017(3) -0.015(2) 0.015(3) C19B 0.030(3) 0.058(5) 0.038(3) -0.031(3) -0.018(3) 0.022(3) C20B 0.023(3) 0.057(5) 0.034(3) -0.020(3) -0.002(2) 0.008(3) C21B 0.018(3) 0.042(4) 0.022(3) -0.008(3) -0.003(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.027(3) . ? Pt1 N1 2.027(3) 2_556 ? Pt1 Cl1 2.3216(10) . ? Pt1 Cl1 2.3217(10) 2_556 ? Pt1 Cl2 2.3275(12) . ? Pt1 Cl2 2.3276(12) 2_556 ? P1 N2 1.612(4) . ? P1 C16 1.788(4) . ? P1 C4 1.799(5) . ? P1 C10 1.802(4) . ? N1 C1 1.312(6) . ? N1 H1 0.8747 . ? N2 C1 1.347(5) . ? C1 C2 1.516(6) . ? C2 C3 1.508(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.394(7) . ? C4 C9 1.398(6) . ? C5 C6 1.385(7) . ? C5 H5 0.9500 . ? C6 C7 1.384(7) . ? C6 H6 0.9500 . ? C7 C8 1.384(7) . ? C7 H7 0.9500 . ? C8 C9 1.379(7) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.380(7) . ? C10 C11 1.400(7) . ? C11 C12 1.386(7) . ? C11 H11 0.9500 . ? C12 C13 1.376(7) . ? C12 H12 0.9500 . ? C13 C14 1.364(7) . ? C13 H13 0.9500 . ? C14 C15 1.406(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.394(7) . ? C16 C21 1.399(7) . ? C17 C18 1.387(7) . ? C17 H17 0.9500 . ? C18 C19 1.393(8) . ? C18 H18 0.9500 . ? C19 C20 1.372(8) . ? C19 H19 0.9500 . ? C20 C21 1.398(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? Pt1B N1B 2.024(4) . ? Pt1B N1B 2.024(4) 2_465 ? Pt1B Cl1B 2.3152(11) 2_465 ? Pt1B Cl1B 2.3152(11) . ? Pt1B Cl2B 2.3306(12) . ? Pt1B Cl2B 2.3306(12) 2_465 ? P1B N2B 1.601(4) . ? P1B C4B 1.794(5) . ? P1B C10B 1.812(4) . ? P1B C16B 1.813(5) . ? N1B C1B 1.303(6) . ? N1B H1B 0.81(4) . ? N2B C1B 1.348(6) . ? C1B C2B 1.506(7) . ? C2B C3B 1.526(7) . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? C4B C9B 1.375(6) . ? C4B C5B 1.398(7) . ? C5B C6B 1.394(7) . ? C5B H5B 0.9500 . ? C6B C7B 1.383(7) . ? C6B H6B 0.9500 . ? C7B C8B 1.372(7) . ? C7B H7B 0.9500 . ? C8B C9B 1.384(6) . ? C8B H8B 0.9500 . ? C9B H9B 0.9500 . ? C10B C11B 1.396(6) . ? C10B C15B 1.399(6) . ? C11B C12B 1.381(6) . ? C11B H11B 0.9500 . ? C12B C13B 1.384(7) . ? C12B H12B 0.9500 . ? C13B C14B 1.392(7) . ? C13B H13B 0.9500 . ? C14B C15B 1.383(7) . ? C14B H14B 0.9500 . ? C15B H15B 0.9500 . ? C16B C17B 1.386(7) . ? C16B C21B 1.388(6) . ? C17B C18B 1.382(7) . ? C17B H17B 0.9500 . ? C18B C19B 1.368(7) . ? C18B H18B 0.9500 . ? C19B C20B 1.377(9) . ? C19B H19B 0.9500 . ? C20B C21B 1.404(7) . ? C20B H20B 0.9500 . ? C21B H21B 0.9500 . ? 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 N1 180.000(2) . 2_556 ? N1 Pt1 Cl1 93.67(10) . . ? N1 Pt1 Cl1 86.33(10) 2_556 . ? N1 Pt1 Cl1 86.33(10) . 2_556 ? N1 Pt1 Cl1 93.67(10) 2_556 2_556 ? Cl1 Pt1 Cl1 180.0 . 2_556 ? N1 Pt1 Cl2 85.17(12) . . ? N1 Pt1 Cl2 94.83(12) 2_556 . ? Cl1 Pt1 Cl2 87.95(4) . . ? Cl1 Pt1 Cl2 92.05(4) 2_556 . ? N1 Pt1 Cl2 94.83(12) . 2_556 ? N1 Pt1 Cl2 85.17(12) 2_556 2_556 ? Cl1 Pt1 Cl2 92.05(4) . 2_556 ? Cl1 Pt1 Cl2 87.95(4) 2_556 2_556 ? Cl2 Pt1 Cl2 180.0 . 2_556 ? N2 P1 C16 106.8(2) . . ? N2 P1 C4 111.8(2) . . ? C16 P1 C4 107.8(2) . . ? N2 P1 C10 114.5(2) . . ? C16 P1 C10 106.7(2) . . ? C4 P1 C10 108.8(2) . . ? C1 N1 Pt1 138.6(3) . . ? C1 N1 H1 113.9 . . ? Pt1 N1 H1 107.3 . . ? C1 N2 P1 124.7(3) . . ? N1 C1 N2 124.7(4) . . ? N1 C1 C2 120.0(4) . . ? N2 C1 C2 115.2(4) . . ? C3 C2 C1 112.8(4) . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C9 119.4(4) . . ? C5 C4 P1 121.9(3) . . ? C9 C4 P1 118.5(4) . . ? C6 C5 C4 119.8(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C7 C6 C5 120.6(5) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 119.6(5) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C4 120.0(5) . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? C15 C10 C11 119.1(4) . . ? C15 C10 P1 123.1(4) . . ? C11 C10 P1 117.6(4) . . ? C12 C11 C10 119.8(5) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C11 120.7(5) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 120.1(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.2(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C10 C15 C14 120.1(4) . . ? C10 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C21 120.1(4) . . ? C17 C16 P1 120.0(4) . . ? C21 C16 P1 119.5(4) . . ? C18 C17 C16 119.7(5) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 119.7(5) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 121.1(5) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 119.6(5) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C20 C21 C16 119.7(5) . . ? C20 C21 H21 120.2 . . ? C16 C21 H21 120.2 . . ? N1B Pt1B N1B 180.0 . 2_465 ? N1B Pt1B Cl1B 94.03(12) . 2_465 ? N1B Pt1B Cl1B 85.97(11) 2_465 2_465 ? N1B Pt1B Cl1B 85.97(12) . . ? N1B Pt1B Cl1B 94.03(11) 2_465 . ? Cl1B Pt1B Cl1B 180.0 2_465 . ? N1B Pt1B Cl2B 84.60(12) . . ? N1B Pt1B Cl2B 95.40(12) 2_465 . ? Cl1B Pt1B Cl2B 88.29(4) 2_465 . ? Cl1B Pt1B Cl2B 91.71(4) . . ? N1B Pt1B Cl2B 95.40(12) . 2_465 ? N1B Pt1B Cl2B 84.60(12) 2_465 2_465 ? Cl1B Pt1B Cl2B 91.71(4) 2_465 2_465 ? Cl1B Pt1B Cl2B 88.29(4) . 2_465 ? Cl2B Pt1B Cl2B 179.998(1) . 2_465 ? N2B P1B C4B 107.4(2) . . ? N2B P1B C10B 111.1(2) . . ? C4B P1B C10B 107.2(2) . . ? N2B P1B C16B 118.2(2) . . ? C4B P1B C16B 106.6(2) . . ? C10B P1B C16B 105.7(2) . . ? C1B N1B Pt1B 139.0(3) . . ? C1B N1B H1B 114(3) . . ? Pt1B N1B H1B 107(3) . . ? C1B N2B P1B 130.4(4) . . ? N1B C1B N2B 124.8(4) . . ? N1B C1B C2B 121.0(4) . . ? N2B C1B C2B 114.2(4) . . ? C1B C2B C3B 112.1(4) . . ? C1B C2B H2B1 109.2 . . ? C3B C2B H2B1 109.2 . . ? C1B C2B H2B2 109.2 . . ? C3B C2B H2B2 109.2 . . ? H2B1 C2B H2B2 107.9 . . ? C2B C3B H3B1 109.5 . . ? C2B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C2B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C9B C4B C5B 119.7(4) . . ? C9B C4B P1B 121.2(4) . . ? C5B C4B P1B 118.8(3) . . ? C6B C5B C4B 119.6(4) . . ? C6B C5B H5B 120.2 . . ? C4B C5B H5B 120.2 . . ? C7B C6B C5B 119.6(5) . . ? C7B C6B H6B 120.2 . . ? C5B C6B H6B 120.2 . . ? C8B C7B C6B 120.4(5) . . ? C8B C7B H7B 119.8 . . ? C6B C7B H7B 119.8 . . ? C7B C8B C9B 120.2(4) . . ? C7B C8B H8B 119.9 . . ? C9B C8B H8B 119.9 . . ? C4B C9B C8B 120.3(5) . . ? C4B C9B H9B 119.8 . . ? C8B C9B H9B 119.8 . . ? C11B C10B C15B 119.9(4) . . ? C11B C10B P1B 120.9(4) . . ? C15B C10B P1B 119.2(3) . . ? C12B C11B C10B 120.2(4) . . ? C12B C11B H11B 119.9 . . ? C10B C11B H11B 119.9 . . ? C11B C12B C13B 120.1(4) . . ? C11B C12B H12B 120.0 . . ? C13B C12B H12B 120.0 . . ? C12B C13B C14B 119.9(5) . . ? C12B C13B H13B 120.1 . . ? C14B C13B H13B 120.1 . . ? C15B C14B C13B 120.8(5) . . ? C15B C14B H14B 119.6 . . ? C13B C14B H14B 119.6 . . ? C14B C15B C10B 119.2(4) . . ? C14B C15B H15B 120.4 . . ? C10B C15B H15B 120.4 . . ? C17B C16B C21B 119.8(5) . . ? C17B C16B P1B 121.8(4) . . ? C21B C16B P1B 118.4(4) . . ? C18B C17B C16B 120.8(5) . . ? C18B C17B H17B 119.6 . . ? C16B C17B H17B 119.6 . . ? C19B C18B C17B 119.9(5) . . ? C19B C18B H18B 120.0 . . ? C17B C18B H18B 120.0 . . ? C18B C19B C20B 120.1(5) . . ? C18B C19B H19B 119.9 . . ? C20B C19B H19B 119.9 . . ? C19B C20B C21B 120.8(5) . . ? C19B C20B H20B 119.6 . . ? C21B C20B H20B 119.6 . . ? C16B C21B C20B 118.5(5) . . ? C16B C21B H21B 120.7 . . ? C20B C21B H21B 120.7 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.796 _refine_diff_density_min -1.060 _refine_diff_density_rms 0.160