# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Puddephatt, R.' _publ_contact_author_email PUDD@UWO.CA _publ_section_title ; Organoplatinum(II) Complexes with Bridging bis(Diphenylphosphino) ethane or Monodentate Benzo[h]quinolyl Ligands ; loop_ _publ_author_name 'M.Golbon Haghighi' M.Rashidi S.M.Nabavizadeh S.Jamali ; Puddephatt ; # Attachment '- 1b.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 784480' #TrackingRef '- 1b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H21 N Pt S' _chemical_formula_sum 'C20 H21 N Pt S' _chemical_formula_weight 502.53 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' S S 0.1246 0.1234 '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 9.9851(6) _cell_length_b 9.4255(5) _cell_length_c 18.8056(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.461(3) _cell_angle_gamma 90.00 _cell_volume 1754.90(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9023 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 29.72 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.902 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 8.113 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5927 _exptl_absorpt_correction_T_max 0.7929 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 55061 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 29.57 _reflns_number_total 4908 _reflns_number_gt 4240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0129P)^2^+1.5439P] 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 4908 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0386 _refine_ls_wR_factor_gt 0.0368 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.145424(10) 0.097940(10) 0.106774(5) 0.02082(3) Uani 1 1 d . . . S1 S 0.22690(7) 0.27940(7) 0.03756(4) 0.02661(14) Uani 1 1 d . . . N1 N 0.3251(2) -0.0238(2) 0.11661(11) 0.0234(5) Uani 1 1 d . . . C1 C 0.2304(3) 0.4393(3) 0.09028(17) 0.0356(7) Uani 1 1 d . . . H1A H 0.2639 0.5180 0.0635 0.053 Uiso 1 1 calc R . . H1B H 0.2901 0.4257 0.1354 0.053 Uiso 1 1 calc R . . H1C H 0.1389 0.4611 0.1007 0.053 Uiso 1 1 calc R . . C2 C 0.0979(3) 0.3269(4) -0.03487(16) 0.0429(8) Uani 1 1 d . . . H2A H 0.0134 0.3471 -0.0156 0.064 Uiso 1 1 calc R . . H2B H 0.0839 0.2480 -0.0690 0.064 Uiso 1 1 calc R . . H2C H 0.1265 0.4112 -0.0594 0.064 Uiso 1 1 calc R . . C3 C 0.0889(3) -0.0641(3) 0.16525(13) 0.0225(5) Uani 1 1 d . . . C4 C 0.1870(3) -0.1724(3) 0.17964(13) 0.0241(5) Uani 1 1 d . . . C5 C 0.1604(3) -0.2951(3) 0.21733(14) 0.0301(6) Uani 1 1 d . . . H5 H 0.2279 -0.3660 0.2269 0.036 Uiso 1 1 calc R . . C6 C 0.0360(3) -0.3131(3) 0.24055(15) 0.0348(7) Uani 1 1 d . . . H6 H 0.0171 -0.3973 0.2652 0.042 Uiso 1 1 calc R . . C7 C -0.0614(3) -0.2079(3) 0.22787(15) 0.0335(6) Uani 1 1 d . . . H7 H -0.1468 -0.2201 0.2442 0.040 Uiso 1 1 calc R . . C8 C -0.0348(3) -0.0845(3) 0.19135(15) 0.0295(6) Uani 1 1 d . . . H8 H -0.1019 -0.0127 0.1840 0.035 Uiso 1 1 calc R . . C9 C 0.3176(3) -0.1477(3) 0.15364(13) 0.0236(5) Uani 1 1 d . . . C10 C 0.4420(3) 0.0104(3) 0.09227(14) 0.0282(6) Uani 1 1 d . . . H10 H 0.4458 0.0962 0.0661 0.034 Uiso 1 1 calc R . . C11 C 0.5564(3) -0.0729(3) 0.10351(15) 0.0308(6) Uani 1 1 d . . . H11 H 0.6374 -0.0447 0.0861 0.037 Uiso 1 1 calc R . . C12 C 0.5499(3) -0.1988(3) 0.14094(15) 0.0328(6) Uani 1 1 d . . . H12 H 0.6268 -0.2587 0.1494 0.039 Uiso 1 1 calc R . . C13 C 0.4307(3) -0.2363(3) 0.16579(15) 0.0303(6) Uani 1 1 d . . . H13 H 0.4253 -0.3228 0.1913 0.036 Uiso 1 1 calc R . . C14 C -0.0325(2) 0.1970(3) 0.10319(13) 0.0220(5) Uani 1 1 d . . . C15 C -0.0565(3) 0.3033(3) 0.15252(13) 0.0237(5) Uani 1 1 d . . . H15 H 0.0138 0.3276 0.1895 0.028 Uiso 1 1 calc R . . C16 C -0.1790(3) 0.3739(3) 0.14910(15) 0.0261(6) Uani 1 1 d . . . H16 H -0.1907 0.4440 0.1840 0.031 Uiso 1 1 calc R . . C17 C -0.2848(3) 0.3443(3) 0.09581(14) 0.0250(5) Uani 1 1 d . . . C18 C -0.2639(3) 0.2397(3) 0.04632(15) 0.0266(6) Uani 1 1 d . . . H18 H -0.3345 0.2174 0.0091 0.032 Uiso 1 1 calc R . . C19 C -0.1414(3) 0.1666(3) 0.05004(14) 0.0259(6) Uani 1 1 d . . . H19 H -0.1314 0.0946 0.0158 0.031 Uiso 1 1 calc R . . C20 C -0.4155(3) 0.4256(3) 0.09019(17) 0.0368(7) Uani 1 1 d . . . H20A H -0.4425 0.4376 0.1381 0.055 Uiso 1 1 calc R . . H20B H -0.4858 0.3732 0.0598 0.055 Uiso 1 1 calc R . . H20C H -0.4032 0.5190 0.0691 0.055 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 0.01956(5) 0.02105(5) 0.02179(5) -0.00072(4) 0.00249(4) 0.00148(4) S1 0.0250(4) 0.0247(3) 0.0308(4) 0.0012(3) 0.0064(3) 0.0008(3) N1 0.0211(12) 0.0263(11) 0.0223(11) -0.0045(8) 0.0008(9) 0.0029(9) C1 0.0318(17) 0.0250(14) 0.0510(19) -0.0056(12) 0.0090(14) -0.0045(12) C2 0.046(2) 0.0474(19) 0.0334(17) 0.0142(14) -0.0019(14) -0.0104(16) C3 0.0259(14) 0.0229(12) 0.0182(12) -0.0022(9) 0.0007(10) -0.0009(10) C4 0.0271(14) 0.0253(13) 0.0188(12) -0.0027(10) -0.0007(10) 0.0008(11) C5 0.0356(17) 0.0280(14) 0.0255(14) 0.0020(11) -0.0005(12) 0.0020(12) C6 0.0430(18) 0.0340(15) 0.0271(15) 0.0070(12) 0.0034(13) -0.0038(13) C7 0.0324(16) 0.0414(16) 0.0280(15) 0.0024(12) 0.0091(12) -0.0049(13) C8 0.0281(15) 0.0312(14) 0.0300(15) 0.0019(11) 0.0065(12) 0.0021(12) C9 0.0269(14) 0.0241(12) 0.0182(12) -0.0053(9) -0.0029(10) 0.0019(11) C10 0.0264(15) 0.0319(14) 0.0266(14) -0.0043(11) 0.0044(11) 0.0003(12) C11 0.0227(15) 0.0362(16) 0.0339(16) -0.0063(12) 0.0048(12) 0.0036(12) C12 0.0269(16) 0.0333(15) 0.0359(16) -0.0060(12) -0.0043(12) 0.0099(13) C13 0.0315(16) 0.0276(14) 0.0296(15) -0.0028(11) -0.0040(12) 0.0065(12) C14 0.0184(13) 0.0233(12) 0.0246(13) 0.0021(10) 0.0040(10) -0.0005(10) C15 0.0212(13) 0.0269(13) 0.0226(13) -0.0002(10) 0.0015(10) -0.0008(11) C16 0.0257(14) 0.0247(13) 0.0287(14) -0.0005(10) 0.0071(11) 0.0009(11) C17 0.0218(14) 0.0236(12) 0.0303(14) 0.0057(10) 0.0063(11) 0.0003(11) C18 0.0210(14) 0.0280(13) 0.0301(14) 0.0036(11) 0.0004(11) -0.0025(11) C19 0.0247(14) 0.0261(13) 0.0273(14) -0.0036(10) 0.0043(11) 0.0005(11) C20 0.0263(16) 0.0371(17) 0.0466(19) 0.0014(13) 0.0035(14) 0.0066(13) _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 C14 2.000(2) . ? Pt1 C3 2.006(2) . ? Pt1 N1 2.118(2) . ? Pt1 S1 2.3572(7) . ? S1 C1 1.802(3) . ? S1 C2 1.805(3) . ? N1 C10 1.347(3) . ? N1 C9 1.366(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C8 1.400(4) . ? C3 C4 1.415(4) . ? C4 C5 1.400(4) . ? C4 C9 1.470(4) . ? C5 C6 1.379(4) . ? C5 H5 0.9500 . ? C6 C7 1.387(4) . ? C6 H6 0.9500 . ? C7 C8 1.394(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C13 1.399(4) . ? C10 C11 1.379(4) . ? C10 H10 0.9500 . ? C11 C12 1.386(4) . ? C11 H11 0.9500 . ? C12 C13 1.381(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.407(3) . ? C14 C19 1.407(4) . ? C15 C16 1.387(4) . ? C15 H15 0.9500 . ? C16 C17 1.387(4) . ? C16 H16 0.9500 . ? C17 C18 1.390(4) . ? C17 C20 1.505(4) . ? C18 C19 1.398(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? 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 C14 Pt1 C3 93.56(10) . . ? C14 Pt1 N1 174.04(9) . . ? C3 Pt1 N1 80.48(9) . . ? C14 Pt1 S1 90.66(7) . . ? C3 Pt1 S1 175.76(8) . . ? N1 Pt1 S1 95.30(6) . . ? C1 S1 C2 99.72(15) . . ? C1 S1 Pt1 106.63(10) . . ? C2 S1 Pt1 109.44(10) . . ? C10 N1 C9 119.0(2) . . ? C10 N1 Pt1 127.00(18) . . ? C9 N1 Pt1 113.95(17) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C8 C3 C4 117.0(2) . . ? C8 C3 Pt1 128.3(2) . . ? C4 C3 Pt1 114.65(19) . . ? C5 C4 C3 121.4(2) . . ? C5 C4 C9 122.3(2) . . ? C3 C4 C9 116.4(2) . . ? C6 C5 C4 120.0(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 119.9(3) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C8 120.4(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C3 121.4(3) . . ? C7 C8 H8 119.3 . . ? C3 C8 H8 119.3 . . ? N1 C9 C13 119.8(2) . . ? N1 C9 C4 114.5(2) . . ? C13 C9 C4 125.7(2) . . ? N1 C10 C11 123.2(3) . . ? N1 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C10 C11 C12 118.3(3) . . ? C10 C11 H11 120.9 . . ? C12 C11 H11 120.9 . . ? C13 C12 C11 119.4(3) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C9 120.3(3) . . ? C12 C13 H13 119.9 . . ? C9 C13 H13 119.9 . . ? C15 C14 C19 115.5(2) . . ? C15 C14 Pt1 122.44(19) . . ? C19 C14 Pt1 122.00(19) . . ? C16 C15 C14 122.4(2) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C17 C16 C15 121.4(2) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 117.4(2) . . ? C16 C17 C20 121.4(2) . . ? C18 C17 C20 121.2(3) . . ? C17 C18 C19 121.5(3) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C19 C14 121.7(2) . . ? C18 C19 H19 119.1 . . ? C14 C19 H19 119.1 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.536 _refine_diff_density_min -0.930 _refine_diff_density_rms 0.104 # Attachment '- 5b.cif' data_5b _database_code_depnum_ccdc_archive 'CCDC 784481' #TrackingRef '- 5b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C62 H54 N2 P2 Pt2), 2(C H2 Cl2)' _chemical_formula_sum 'C62.67 H55.33 Cl1.33 N2 P2 Pt2' _chemical_formula_weight 1335.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 14.4438(5) _cell_length_b 33.6884(12) _cell_length_c 17.0228(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.626(2) _cell_angle_gamma 90.00 _cell_volume 7977.0(5) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9710 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.23 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3924 _exptl_absorpt_coefficient_mu 5.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7367 _exptl_absorpt_correction_T_max 0.8763 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 432171 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 29.57 _reflns_number_total 22381 _reflns_number_gt 18106 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0126P)^2^+10.2314P] 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 22381 _refine_ls_number_parameters 949 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0484 _refine_ls_wR_factor_gt 0.0438 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.009 _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 0.636402(7) 0.241367(3) 0.821168(6) 0.01785(2) Uani 1 1 d . . . Pt2 Pt 0.399649(7) 0.095841(3) 1.117066(6) 0.01929(3) Uani 1 1 d . . . Pt3 Pt 0.584375(7) 0.592115(3) 0.867198(6) 0.01804(2) Uani 1 1 d . . . Cl1 Cl 0.72262(11) 0.54143(4) 0.64961(10) 0.0901(4) Uani 1 1 d . . . Cl2 Cl 0.84006(11) 0.56266(6) 0.81110(9) 0.1018(5) Uani 1 1 d . . . P1 P 0.62755(5) 0.21241(2) 0.94263(4) 0.01852(14) Uani 1 1 d . . . P2 P 0.41971(5) 0.12240(2) 0.99704(4) 0.02017(14) Uani 1 1 d . . . P3 P 0.57816(5) 0.55601(2) 0.98107(4) 0.01883(14) Uani 1 1 d . . . N1 N 0.26226(17) 0.06929(7) 1.07242(15) 0.0231(5) Uani 1 1 d . . . N2 N 0.75148(17) 0.28071(7) 0.86882(14) 0.0216(5) Uani 1 1 d . . . N3 N 0.69328(17) 0.63340(7) 0.92329(14) 0.0223(5) Uani 1 1 d . . . C1 C 0.5267(2) 0.20738(9) 0.75855(17) 0.0233(6) Uani 1 1 d . . . C2 C 0.5423(2) 0.17229(9) 0.72014(18) 0.0293(7) Uani 1 1 d . . . H2 H 0.6065 0.1640 0.7250 0.035 Uiso 1 1 calc R . . C3 C 0.4667(3) 0.14913(11) 0.6749(2) 0.0429(9) Uani 1 1 d . . . H3 H 0.4805 0.1257 0.6492 0.051 Uiso 1 1 calc R . . C4 C 0.3724(3) 0.15942(13) 0.6666(2) 0.0508(11) Uani 1 1 d . . . C5 C 0.3550(2) 0.19423(13) 0.7036(2) 0.0492(11) Uani 1 1 d . . . H5 H 0.2905 0.2022 0.6984 0.059 Uiso 1 1 calc R . . C6 C 0.4304(2) 0.21794(11) 0.7486(2) 0.0356(8) Uani 1 1 d . . . H6 H 0.4160 0.2417 0.7729 0.043 Uiso 1 1 calc R . . C7 C 0.2897(4) 0.13401(17) 0.6183(3) 0.0855(19) Uani 1 1 d . . . H7A H 0.2326 0.1506 0.5980 0.128 Uiso 1 1 calc R . . H7B H 0.2758 0.1131 0.6536 0.128 Uiso 1 1 calc R . . H7C H 0.3074 0.1218 0.5721 0.128 Uiso 1 1 calc R . . C8 C 0.5307(2) 0.17585(9) 0.93115(16) 0.0226(6) Uani 1 1 d . . . H8A H 0.4688 0.1892 0.9057 0.027 Uiso 1 1 calc R . . H8B H 0.5398 0.1549 0.8931 0.027 Uiso 1 1 calc R . . C9 C 0.5232(2) 0.15593(9) 1.00987(17) 0.0243(6) Uani 1 1 d . . . H9A H 0.5190 0.1768 1.0497 0.029 Uiso 1 1 calc R . . H9B H 0.5828 0.1406 1.0332 0.029 Uiso 1 1 calc R . . C10 C 0.3214(2) 0.15444(9) 0.94356(18) 0.0240(6) Uani 1 1 d . . . C11 C 0.2478(2) 0.14335(10) 0.8755(2) 0.0315(7) Uani 1 1 d . . . H11 H 0.2489 0.1178 0.8522 0.038 Uiso 1 1 calc R . . C12 C 0.1730(2) 0.16933(12) 0.8412(2) 0.0430(9) Uani 1 1 d . . . H12 H 0.1231 0.1614 0.7951 0.052 Uiso 1 1 calc R . . C13 C 0.1714(3) 0.20660(12) 0.8745(2) 0.0477(10) Uani 1 1 d . . . H13 H 0.1203 0.2244 0.8512 0.057 Uiso 1 1 calc R . . C14 C 0.2436(3) 0.21805(12) 0.9413(2) 0.0484(10) Uani 1 1 d . . . H14 H 0.2426 0.2439 0.9636 0.058 Uiso 1 1 calc R . . C15 C 0.3175(3) 0.19233(10) 0.9763(2) 0.0353(8) Uani 1 1 d . . . H15 H 0.3662 0.2004 1.0230 0.042 Uiso 1 1 calc R . . C16 C 0.4450(2) 0.08666(8) 0.92538(18) 0.0237(6) Uani 1 1 d . . . C17 C 0.4273(2) 0.09217(9) 0.84111(17) 0.0258(6) Uani 1 1 d . . . H17 H 0.3935 0.1151 0.8161 0.031 Uiso 1 1 calc R . . C18 C 0.4589(2) 0.06439(10) 0.7937(2) 0.0333(7) Uani 1 1 d . . . H18 H 0.4447 0.0682 0.7364 0.040 Uiso 1 1 calc R . . C19 C 0.5106(3) 0.03143(10) 0.8287(2) 0.0408(9) Uani 1 1 d . . . H19 H 0.5315 0.0125 0.7957 0.049 Uiso 1 1 calc R . . C20 C 0.5315(3) 0.02621(11) 0.9124(2) 0.0446(9) Uani 1 1 d . . . H20 H 0.5687 0.0040 0.9371 0.054 Uiso 1 1 calc R . . C21 C 0.4985(3) 0.05319(10) 0.9603(2) 0.0368(8) Uani 1 1 d . . . H21 H 0.5123 0.0490 1.0174 0.044 Uiso 1 1 calc R . . C22 C 0.3773(2) 0.07578(8) 1.22314(17) 0.0238(6) Uani 1 1 d . . . C23 C 0.2809(2) 0.06439(9) 1.21600(19) 0.0281(7) Uani 1 1 d . . . C24 C 0.2501(3) 0.05436(10) 1.2843(2) 0.0373(8) Uani 1 1 d . . . H24 H 0.1845 0.0480 1.2782 0.045 Uiso 1 1 calc R . . C25 C 0.3143(3) 0.05366(10) 1.3604(2) 0.0401(8) Uani 1 1 d . . . H25 H 0.2931 0.0472 1.4070 0.048 Uiso 1 1 calc R . . C26 C 0.4105(3) 0.06252(10) 1.3688(2) 0.0361(8) Uani 1 1 d . . . H26 H 0.4555 0.0609 1.4209 0.043 Uiso 1 1 calc R . . C27 C 0.4416(2) 0.07379(9) 1.30111(18) 0.0292(7) Uani 1 1 d . . . H27 H 0.5073 0.0802 1.3081 0.035 Uiso 1 1 calc R . . C28 C 0.2178(2) 0.06208(9) 1.13261(19) 0.0273(6) Uani 1 1 d . . . C29 C 0.1205(2) 0.05222(11) 1.1119(2) 0.0391(8) Uani 1 1 d . . . H29 H 0.0891 0.0483 1.1537 0.047 Uiso 1 1 calc R . . C30 C 0.0697(2) 0.04811(11) 1.0315(2) 0.0428(9) Uani 1 1 d . . . H30 H 0.0030 0.0420 1.0175 0.051 Uiso 1 1 calc R . . C31 C 0.1163(2) 0.05296(10) 0.9713(2) 0.0357(8) Uani 1 1 d . . . H31 H 0.0835 0.0490 0.9155 0.043 Uiso 1 1 calc R . . C32 C 0.2124(2) 0.06382(9) 0.99438(19) 0.0285(7) Uani 1 1 d . . . H32 H 0.2445 0.0676 0.9530 0.034 Uiso 1 1 calc R . . C33 C 0.5201(2) 0.12400(9) 1.17835(17) 0.0229(6) Uani 1 1 d . . . C34 C 0.5127(2) 0.16078(9) 1.21482(18) 0.0260(6) Uani 1 1 d . . . H34 H 0.4508 0.1712 1.2120 0.031 Uiso 1 1 calc R . . C35 C 0.5935(2) 0.18252(9) 1.25498(18) 0.0286(7) Uani 1 1 d . . . H35 H 0.5853 0.2072 1.2794 0.034 Uiso 1 1 calc R . . C36 C 0.6857(2) 0.16906(9) 1.26015(18) 0.0288(7) Uani 1 1 d . . . C37 C 0.6942(2) 0.13244(10) 1.22490(18) 0.0296(7) Uani 1 1 d . . . H37 H 0.7563 0.1223 1.2274 0.035 Uiso 1 1 calc R . . C38 C 0.6132(2) 0.11035(9) 1.18603(18) 0.0276(6) Uani 1 1 d . . . H38 H 0.6217 0.0851 1.1640 0.033 Uiso 1 1 calc R . . C39 C 0.7729(2) 0.19365(11) 1.3010(2) 0.0407(8) Uani 1 1 d . . . H39A H 0.8011 0.1837 1.3563 0.061 Uiso 1 1 calc R . . H39B H 0.7537 0.2214 1.3036 0.061 Uiso 1 1 calc R . . H39C H 0.8204 0.1918 1.2695 0.061 Uiso 1 1 calc R . . C40 C 0.5957(2) 0.24940(8) 1.00892(17) 0.0215(6) Uani 1 1 d . . . C41 C 0.6058(2) 0.24406(9) 1.09263(18) 0.0269(6) Uani 1 1 d . . . H41 H 0.6357 0.2208 1.1192 0.032 Uiso 1 1 calc R . . C42 C 0.5720(3) 0.27285(10) 1.1367(2) 0.0362(8) Uani 1 1 d . . . H42 H 0.5798 0.2692 1.1935 0.043 Uiso 1 1 calc R . . C43 C 0.5274(3) 0.30665(10) 1.0987(2) 0.0405(8) Uani 1 1 d . . . H43 H 0.5043 0.3261 1.1292 0.049 Uiso 1 1 calc R . . C44 C 0.5163(3) 0.31211(10) 1.0164(2) 0.0390(8) Uani 1 1 d . . . H44 H 0.4850 0.3352 0.9901 0.047 Uiso 1 1 calc R . . C45 C 0.5506(2) 0.28394(9) 0.9719(2) 0.0319(7) Uani 1 1 d . . . H45 H 0.5434 0.2882 0.9154 0.038 Uiso 1 1 calc R . . C46 C 0.7306(2) 0.18457(8) 1.00462(17) 0.0224(6) Uani 1 1 d . . . C47 C 0.7449(3) 0.14641(10) 0.9785(2) 0.0352(8) Uani 1 1 d . . . H47 H 0.7010 0.1358 0.9312 0.042 Uiso 1 1 calc R . . C48 C 0.8229(3) 0.12367(12) 1.0208(2) 0.0482(10) Uani 1 1 d . . . H48 H 0.8313 0.0976 1.0028 0.058 Uiso 1 1 calc R . . C49 C 0.8875(3) 0.13874(13) 1.0883(2) 0.0487(10) Uani 1 1 d . . . H49 H 0.9410 0.1232 1.1166 0.058 Uiso 1 1 calc R . . C50 C 0.8752(2) 0.17645(11) 1.1155(2) 0.0385(8) Uani 1 1 d . . . H50 H 0.9201 0.1868 1.1625 0.046 Uiso 1 1 calc R . . C51 C 0.7971(2) 0.19930(10) 1.07399(19) 0.0289(7) Uani 1 1 d . . . H51 H 0.7889 0.2252 1.0931 0.035 Uiso 1 1 calc R . . C52 C 0.7676(2) 0.30778(8) 0.81471(17) 0.0209(6) Uani 1 1 d . . . C53 C 0.8394(2) 0.33614(9) 0.83911(19) 0.0305(7) Uani 1 1 d . . . H53 H 0.8485 0.3555 0.8013 0.037 Uiso 1 1 calc R . . C54 C 0.8977(2) 0.33631(9) 0.9182(2) 0.0326(7) Uani 1 1 d . . . H54 H 0.9472 0.3555 0.9349 0.039 Uiso 1 1 calc R . . C55 C 0.8829(2) 0.30817(10) 0.97239(19) 0.0324(7) Uani 1 1 d . . . H55 H 0.9227 0.3073 1.0268 0.039 Uiso 1 1 calc R . . C56 C 0.8088(2) 0.28130(10) 0.94566(19) 0.0305(7) Uani 1 1 d . . . H56 H 0.7977 0.2623 0.9834 0.037 Uiso 1 1 calc R . . C57 C 0.7042(2) 0.30372(8) 0.73114(17) 0.0222(6) Uani 1 1 d . . . C58 C 0.7112(2) 0.32902(9) 0.66777(18) 0.0276(6) Uani 1 1 d . . . H58 H 0.7572 0.3499 0.6782 0.033 Uiso 1 1 calc R . . C59 C 0.6512(2) 0.32374(9) 0.58998(19) 0.0304(7) Uani 1 1 d . . . H59 H 0.6560 0.3408 0.5468 0.036 Uiso 1 1 calc R . . C60 C 0.5844(2) 0.29336(9) 0.57565(19) 0.0289(7) Uani 1 1 d . . . H60 H 0.5432 0.2896 0.5224 0.035 Uiso 1 1 calc R . . C61 C 0.5770(2) 0.26820(8) 0.63879(17) 0.0233(6) Uani 1 1 d . . . H61 H 0.5304 0.2476 0.6276 0.028 Uiso 1 1 calc R . . C62 C 0.63665(19) 0.27252(8) 0.71842(17) 0.0197(5) Uani 1 1 d . . . C63 C 0.69543(19) 0.53647(8) 1.03766(17) 0.0206(6) Uani 1 1 d . . . C64 C 0.7624(2) 0.53140(9) 0.99253(18) 0.0268(6) Uani 1 1 d . . . H64 H 0.7460 0.5391 0.9368 0.032 Uiso 1 1 calc R . . C65 C 0.8521(2) 0.51530(10) 1.0277(2) 0.0332(7) Uani 1 1 d . . . H65 H 0.8966 0.5119 0.9961 0.040 Uiso 1 1 calc R . . C66 C 0.8768(2) 0.50422(10) 1.1089(2) 0.0337(7) Uani 1 1 d . . . H66 H 0.9387 0.4935 1.1336 0.040 Uiso 1 1 calc R . . C67 C 0.8112(2) 0.50877(10) 1.1539(2) 0.0336(7) Uani 1 1 d . . . H67 H 0.8281 0.5010 1.2096 0.040 Uiso 1 1 calc R . . C68 C 0.7208(2) 0.52454(9) 1.11889(18) 0.0277(6) Uani 1 1 d . . . H68 H 0.6761 0.5272 1.1505 0.033 Uiso 1 1 calc R . . C69 C 0.5039(2) 0.51090(8) 0.96180(17) 0.0230(6) Uani 1 1 d . . . H69A H 0.4383 0.5182 0.9293 0.028 Uiso 1 1 calc R . . H69B H 0.5310 0.4925 0.9285 0.028 Uiso 1 1 calc R . . C70 C 0.4835(2) 0.55622(8) 0.79756(16) 0.0207(6) Uani 1 1 d . . . C71 C 0.5076(2) 0.51972(9) 0.76850(18) 0.0254(6) Uani 1 1 d . . . H71 H 0.5732 0.5118 0.7820 0.031 Uiso 1 1 calc R . . C72 C 0.4383(2) 0.49474(9) 0.72051(19) 0.0309(7) Uani 1 1 d . . . H72 H 0.4577 0.4701 0.7030 0.037 Uiso 1 1 calc R . . C73 C 0.3415(2) 0.50485(10) 0.69760(19) 0.0303(7) Uani 1 1 d . . . C74 C 0.2670(3) 0.47788(12) 0.6437(2) 0.0480(10) Uani 1 1 d . . . H74A H 0.2780 0.4764 0.5894 0.072 Uiso 1 1 calc R . . H74B H 0.2026 0.4885 0.6390 0.072 Uiso 1 1 calc R . . H74C H 0.2722 0.4513 0.6678 0.072 Uiso 1 1 calc R . . C75 C 0.3167(2) 0.54100(9) 0.72554(18) 0.0287(7) Uani 1 1 d . . . H75 H 0.2512 0.5490 0.7110 0.034 Uiso 1 1 calc R . . C76 C 0.3862(2) 0.56583(9) 0.77468(18) 0.0251(6) Uani 1 1 d . . . H76 H 0.3662 0.5902 0.7931 0.030 Uiso 1 1 calc R . . C77 C 0.7468(2) 0.63336(9) 1.00141(18) 0.0282(7) Uani 1 1 d . . . H77 H 0.7326 0.6143 1.0376 0.034 Uiso 1 1 calc R . . C78 C 0.8215(2) 0.65968(10) 1.0316(2) 0.0321(7) Uani 1 1 d . . . H78 H 0.8588 0.6582 1.0868 0.039 Uiso 1 1 calc R . . C79 C 0.8405(2) 0.68816(9) 0.9794(2) 0.0319(7) Uani 1 1 d . . . H79 H 0.8912 0.7067 0.9983 0.038 Uiso 1 1 calc R . . C80 C 0.7850(2) 0.68926(9) 0.8999(2) 0.0302(7) Uani 1 1 d . . . H80 H 0.7960 0.7092 0.8640 0.036 Uiso 1 1 calc R . . C81 C 0.7125(2) 0.66122(8) 0.87195(18) 0.0234(6) Uani 1 1 d . . . C82 C 0.6544(2) 0.65803(8) 0.78661(18) 0.0236(6) Uani 1 1 d . . . C83 C 0.5904(2) 0.62564(8) 0.76853(17) 0.0221(6) Uani 1 1 d . . . C84 C 0.5396(2) 0.62056(10) 0.68684(18) 0.0288(7) Uani 1 1 d . . . H84 H 0.4963 0.5989 0.6722 0.035 Uiso 1 1 calc R . . C85 C 0.5509(2) 0.64653(11) 0.6261(2) 0.0349(8) Uani 1 1 d . . . H85 H 0.5157 0.6422 0.5710 0.042 Uiso 1 1 calc R . . C86 C 0.6128(2) 0.67829(11) 0.6458(2) 0.0375(8) Uani 1 1 d . . . H86 H 0.6194 0.6962 0.6045 0.045 Uiso 1 1 calc R . . C87 C 0.6653(2) 0.68418(10) 0.7259(2) 0.0328(7) Uani 1 1 d . . . H87 H 0.7086 0.7059 0.7395 0.039 Uiso 1 1 calc R . . C88 C 0.5257(2) 0.58214(8) 1.05289(17) 0.0211(6) Uani 1 1 d . . . C89 C 0.5787(2) 0.59870(9) 1.12618(18) 0.0280(6) Uani 1 1 d . . . H89 H 0.6468 0.5964 1.1416 0.034 Uiso 1 1 calc R . . C90 C 0.5331(2) 0.61852(11) 1.1770(2) 0.0361(8) Uani 1 1 d . . . H90 H 0.5703 0.6292 1.2273 0.043 Uiso 1 1 calc R . . C91 C 0.4347(3) 0.62287(11) 1.1552(2) 0.0381(8) Uani 1 1 d . . . H91 H 0.4039 0.6364 1.1901 0.046 Uiso 1 1 calc R . . C92 C 0.3813(2) 0.60735(11) 1.0817(2) 0.0365(8) Uani 1 1 d . . . H92 H 0.3134 0.6104 1.0659 0.044 Uiso 1 1 calc R . . C93 C 0.4261(2) 0.58739(9) 1.0311(2) 0.0307(7) Uani 1 1 d . . . H93 H 0.3884 0.5771 0.9807 0.037 Uiso 1 1 calc R . . C94 C 0.7856(3) 0.57878(13) 0.7123(3) 0.0671(13) Uani 1 1 d . . . H94A H 0.7408 0.6007 0.7146 0.080 Uiso 1 1 calc R . . H94B H 0.8356 0.5894 0.6880 0.080 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 0.02027(5) 0.01728(5) 0.01716(5) 0.00099(4) 0.00706(4) -0.00178(4) Pt2 0.02100(5) 0.01879(5) 0.02006(5) 0.00291(4) 0.00894(4) -0.00005(4) Pt3 0.02017(5) 0.01675(5) 0.01800(5) 0.00274(4) 0.00654(4) -0.00182(4) Cl1 0.0955(10) 0.0543(8) 0.1196(12) -0.0036(8) 0.0277(9) 0.0061(7) Cl2 0.0911(10) 0.1509(15) 0.0815(10) 0.0313(10) 0.0544(9) 0.0056(10) P1 0.0212(3) 0.0176(3) 0.0178(3) 0.0012(3) 0.0072(3) -0.0022(3) P2 0.0219(3) 0.0206(3) 0.0194(3) 0.0022(3) 0.0079(3) -0.0033(3) P3 0.0206(3) 0.0178(3) 0.0184(3) 0.0032(3) 0.0057(3) -0.0030(3) N1 0.0236(12) 0.0182(11) 0.0291(13) 0.0023(10) 0.0098(10) -0.0009(9) N2 0.0255(12) 0.0198(12) 0.0203(12) -0.0004(9) 0.0075(10) -0.0059(10) N3 0.0246(12) 0.0198(12) 0.0243(13) 0.0023(10) 0.0094(10) -0.0025(10) C1 0.0242(14) 0.0289(15) 0.0164(13) 0.0060(11) 0.0047(11) -0.0052(12) C2 0.0355(17) 0.0284(16) 0.0233(15) 0.0002(13) 0.0065(13) -0.0084(13) C3 0.058(2) 0.043(2) 0.0254(17) -0.0036(15) 0.0063(16) -0.0254(18) C4 0.046(2) 0.069(3) 0.0280(19) 0.0106(19) -0.0067(16) -0.035(2) C5 0.0221(17) 0.076(3) 0.044(2) 0.023(2) -0.0008(15) -0.0118(18) C6 0.0277(16) 0.045(2) 0.0332(18) 0.0130(15) 0.0061(14) -0.0002(15) C7 0.074(3) 0.118(5) 0.047(3) 0.006(3) -0.013(2) -0.070(3) C8 0.0265(15) 0.0255(15) 0.0163(13) 0.0018(11) 0.0065(11) -0.0099(12) C9 0.0260(15) 0.0262(15) 0.0213(14) 0.0028(12) 0.0074(12) -0.0087(12) C10 0.0260(15) 0.0255(15) 0.0235(15) 0.0070(12) 0.0115(12) 0.0001(12) C11 0.0259(16) 0.0322(17) 0.0360(18) 0.0078(14) 0.0073(13) -0.0032(13) C12 0.0298(18) 0.054(2) 0.044(2) 0.0181(18) 0.0072(16) 0.0035(16) C13 0.041(2) 0.055(2) 0.053(2) 0.028(2) 0.0235(19) 0.0231(18) C14 0.063(3) 0.040(2) 0.051(2) 0.0090(18) 0.029(2) 0.0222(19) C15 0.044(2) 0.0313(17) 0.0331(18) 0.0002(14) 0.0153(15) 0.0069(15) C16 0.0257(14) 0.0219(14) 0.0256(15) -0.0008(12) 0.0104(12) -0.0047(11) C17 0.0289(15) 0.0258(15) 0.0231(14) -0.0030(12) 0.0079(12) -0.0054(12) C18 0.0395(18) 0.0342(18) 0.0301(17) -0.0086(14) 0.0161(14) -0.0110(14) C19 0.049(2) 0.0295(18) 0.054(2) -0.0079(16) 0.0318(19) -0.0038(16) C20 0.055(2) 0.0287(18) 0.058(2) 0.0039(17) 0.028(2) 0.0088(16) C21 0.047(2) 0.0320(18) 0.0365(19) 0.0096(15) 0.0193(16) 0.0077(15) C22 0.0322(16) 0.0196(14) 0.0232(15) 0.0030(11) 0.0139(12) 0.0034(12) C23 0.0349(17) 0.0224(15) 0.0329(17) 0.0040(13) 0.0192(14) 0.0014(12) C24 0.044(2) 0.0358(18) 0.040(2) 0.0059(15) 0.0257(16) -0.0041(15) C25 0.059(2) 0.0387(19) 0.0327(19) 0.0098(15) 0.0293(17) 0.0063(17) C26 0.052(2) 0.0326(18) 0.0259(16) 0.0104(14) 0.0143(15) 0.0163(16) C27 0.0371(17) 0.0280(16) 0.0269(16) 0.0085(13) 0.0163(14) 0.0117(13) C28 0.0289(16) 0.0199(14) 0.0375(18) 0.0023(12) 0.0167(13) -0.0010(12) C29 0.0306(17) 0.042(2) 0.051(2) -0.0024(17) 0.0231(16) -0.0086(15) C30 0.0271(17) 0.043(2) 0.059(2) -0.0063(18) 0.0122(17) -0.0095(15) C31 0.0312(17) 0.0319(17) 0.0409(19) 0.0006(15) 0.0041(15) -0.0028(14) C32 0.0315(16) 0.0239(15) 0.0313(17) 0.0012(13) 0.0105(13) -0.0052(12) C33 0.0256(14) 0.0264(15) 0.0178(14) 0.0045(11) 0.0079(11) 0.0028(12) C34 0.0252(15) 0.0289(16) 0.0245(15) 0.0025(12) 0.0077(12) 0.0053(12) C35 0.0355(17) 0.0292(16) 0.0214(15) -0.0002(12) 0.0082(13) -0.0022(13) C36 0.0313(16) 0.0324(17) 0.0209(15) 0.0024(13) 0.0040(12) -0.0055(13) C37 0.0226(15) 0.0358(17) 0.0287(16) 0.0029(14) 0.0043(12) 0.0028(13) C38 0.0279(15) 0.0271(15) 0.0270(16) -0.0001(13) 0.0058(13) 0.0038(12) C39 0.0355(19) 0.047(2) 0.038(2) -0.0048(17) 0.0078(15) -0.0124(16) C40 0.0223(14) 0.0193(13) 0.0240(14) -0.0007(11) 0.0083(11) -0.0009(11) C41 0.0353(17) 0.0206(14) 0.0256(15) 0.0019(12) 0.0096(13) 0.0020(12) C42 0.054(2) 0.0311(17) 0.0270(17) -0.0032(14) 0.0164(16) 0.0048(15) C43 0.054(2) 0.0311(18) 0.041(2) -0.0040(15) 0.0204(17) 0.0103(16) C44 0.049(2) 0.0255(17) 0.045(2) 0.0052(15) 0.0186(17) 0.0128(15) C45 0.0440(19) 0.0259(16) 0.0282(17) 0.0062(13) 0.0137(15) 0.0087(14) C46 0.0228(14) 0.0228(14) 0.0236(15) 0.0067(12) 0.0098(12) 0.0011(11) C47 0.045(2) 0.0306(17) 0.0345(18) 0.0009(14) 0.0173(16) 0.0063(15) C48 0.058(3) 0.041(2) 0.053(2) 0.0113(18) 0.028(2) 0.0224(19) C49 0.039(2) 0.061(3) 0.052(2) 0.029(2) 0.0229(19) 0.0246(19) C50 0.0235(16) 0.053(2) 0.0381(19) 0.0183(17) 0.0067(14) -0.0012(15) C51 0.0261(15) 0.0315(16) 0.0304(17) 0.0078(13) 0.0100(13) -0.0032(13) C52 0.0245(14) 0.0171(13) 0.0235(14) 0.0017(11) 0.0107(11) -0.0003(11) C53 0.0340(17) 0.0275(16) 0.0319(17) 0.0043(13) 0.0121(14) -0.0079(13) C54 0.0316(17) 0.0286(16) 0.0360(18) -0.0021(14) 0.0065(14) -0.0131(13) C55 0.0344(17) 0.0338(18) 0.0256(16) -0.0025(13) 0.0020(13) -0.0096(14) C56 0.0356(17) 0.0314(17) 0.0233(16) 0.0008(13) 0.0059(13) -0.0119(14) C57 0.0277(15) 0.0194(14) 0.0219(14) 0.0021(11) 0.0110(12) 0.0035(11) C58 0.0339(17) 0.0226(15) 0.0283(16) 0.0070(12) 0.0118(13) -0.0025(12) C59 0.0382(18) 0.0305(17) 0.0248(16) 0.0107(13) 0.0125(14) 0.0033(14) C60 0.0319(16) 0.0317(17) 0.0232(15) 0.0068(13) 0.0074(13) 0.0070(13) C61 0.0257(14) 0.0212(14) 0.0238(15) -0.0002(11) 0.0078(12) 0.0028(11) C62 0.0218(13) 0.0184(13) 0.0212(14) 0.0018(11) 0.0098(11) 0.0060(10) C63 0.0215(13) 0.0176(13) 0.0213(14) 0.0018(11) 0.0036(11) -0.0028(11) C64 0.0257(15) 0.0317(16) 0.0234(15) -0.0030(13) 0.0072(12) -0.0005(12) C65 0.0249(16) 0.0373(18) 0.0387(19) -0.0065(15) 0.0108(14) 0.0004(13) C66 0.0227(15) 0.0357(18) 0.0397(19) 0.0060(15) 0.0035(14) 0.0042(13) C67 0.0274(16) 0.0377(18) 0.0325(18) 0.0139(15) 0.0023(14) 0.0017(14) C68 0.0252(15) 0.0309(16) 0.0273(16) 0.0081(13) 0.0075(12) 0.0005(12) C69 0.0290(15) 0.0185(14) 0.0214(14) 0.0023(11) 0.0065(12) -0.0070(11) C70 0.0239(14) 0.0230(14) 0.0168(13) 0.0051(11) 0.0081(11) 0.0004(11) C71 0.0227(14) 0.0260(15) 0.0300(16) -0.0022(12) 0.0113(12) 0.0009(12) C72 0.0372(18) 0.0273(16) 0.0320(17) -0.0080(13) 0.0160(14) -0.0051(13) C73 0.0313(16) 0.0348(18) 0.0248(16) -0.0007(13) 0.0076(13) -0.0096(14) C74 0.040(2) 0.053(2) 0.047(2) -0.0104(19) 0.0055(17) -0.0187(18) C75 0.0194(14) 0.0360(17) 0.0287(16) 0.0094(13) 0.0034(12) -0.0007(12) C76 0.0266(15) 0.0226(14) 0.0267(15) 0.0033(12) 0.0082(12) 0.0017(12) C77 0.0355(17) 0.0277(16) 0.0229(15) -0.0021(12) 0.0105(13) -0.0073(13) C78 0.0349(17) 0.0344(18) 0.0265(16) -0.0070(14) 0.0073(14) -0.0074(14) C79 0.0301(16) 0.0296(17) 0.0379(18) -0.0072(14) 0.0123(14) -0.0121(13) C80 0.0304(16) 0.0244(15) 0.0387(18) 0.0021(13) 0.0145(14) -0.0069(13) C81 0.0256(14) 0.0195(14) 0.0282(15) 0.0031(12) 0.0125(12) 0.0004(11) C82 0.0234(14) 0.0224(14) 0.0274(15) 0.0055(12) 0.0111(12) 0.0016(11) C83 0.0213(14) 0.0225(14) 0.0253(15) 0.0073(12) 0.0112(12) 0.0030(11) C84 0.0261(15) 0.0335(17) 0.0277(16) 0.0085(13) 0.0090(13) -0.0012(13) C85 0.0288(17) 0.048(2) 0.0263(17) 0.0135(15) 0.0057(13) 0.0008(15) C86 0.0359(18) 0.045(2) 0.0332(18) 0.0212(16) 0.0128(15) 0.0020(15) C87 0.0317(17) 0.0322(17) 0.0356(18) 0.0134(14) 0.0109(14) -0.0050(14) C88 0.0216(13) 0.0199(13) 0.0226(14) 0.0044(11) 0.0076(11) -0.0011(11) C89 0.0236(14) 0.0335(17) 0.0272(16) -0.0023(13) 0.0071(12) -0.0003(13) C90 0.0346(18) 0.044(2) 0.0307(18) -0.0083(15) 0.0106(14) 0.0014(15) C91 0.041(2) 0.041(2) 0.0373(19) 0.0008(16) 0.0202(16) 0.0080(16) C92 0.0251(16) 0.045(2) 0.0404(19) 0.0039(16) 0.0109(14) 0.0061(14) C93 0.0270(15) 0.0343(18) 0.0295(16) 0.0002(14) 0.0055(13) 0.0014(13) C94 0.067(3) 0.052(3) 0.094(4) 0.012(3) 0.042(3) 0.018(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 C1 2.012(3) . ? Pt1 C62 2.041(3) . ? Pt1 N2 2.110(2) . ? Pt1 P1 2.3206(7) . ? Pt2 C33 2.009(3) . ? Pt2 C22 2.033(3) . ? Pt2 N1 2.122(2) . ? Pt2 P2 2.3190(7) . ? Pt3 C70 2.015(3) . ? Pt3 C83 2.045(3) . ? Pt3 N3 2.124(2) . ? Pt3 P3 2.3106(7) . ? Cl1 C94 1.740(5) . ? Cl2 C94 1.741(5) . ? P1 C40 1.822(3) . ? P1 C46 1.834(3) . ? P1 C8 1.835(3) . ? P2 C16 1.820(3) . ? P2 C10 1.820(3) . ? P2 C9 1.839(3) . ? P3 C88 1.829(3) . ? P3 C63 1.831(3) . ? P3 C69 1.838(3) . ? N1 C32 1.342(4) . ? N1 C28 1.369(4) . ? N2 C56 1.346(4) . ? N2 C52 1.360(3) . ? N3 C77 1.346(4) . ? N3 C81 1.360(3) . ? C1 C2 1.398(4) . ? C1 C6 1.401(4) . ? C2 C3 1.394(4) . ? C2 H2 0.9500 . ? C3 C4 1.374(6) . ? C3 H3 0.9500 . ? C4 C5 1.386(6) . ? C4 C7 1.519(5) . ? C5 C6 1.400(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.528(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.396(4) . ? C10 C15 1.400(4) . ? C11 C12 1.391(5) . ? C11 H11 0.9500 . ? C12 C13 1.380(6) . ? C12 H12 0.9500 . ? C13 C14 1.375(6) . ? C13 H13 0.9500 . ? C14 C15 1.379(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.400(4) . ? C16 C21 1.405(4) . ? C17 C18 1.390(4) . ? C17 H17 0.9500 . ? C18 C19 1.380(5) . ? C18 H18 0.9500 . ? C19 C20 1.386(5) . ? C19 H19 0.9500 . ? C20 C21 1.388(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.401(4) . ? C22 C23 1.418(4) . ? C23 C24 1.393(4) . ? C23 C28 1.468(4) . ? C24 C25 1.376(5) . ? C24 H24 0.9500 . ? C25 C26 1.391(5) . ? C25 H25 0.9500 . ? C26 C27 1.396(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.394(4) . ? C29 C30 1.376(5) . ? C29 H29 0.9500 . ? C30 C31 1.379(5) . ? C30 H30 0.9500 . ? C31 C32 1.385(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.394(4) . ? C33 C34 1.403(4) . ? C34 C35 1.391(4) . ? C34 H34 0.9500 . ? C35 C36 1.387(4) . ? C35 H35 0.9500 . ? C36 C37 1.392(4) . ? C36 C39 1.511(4) . ? C37 C38 1.394(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C45 1.398(4) . ? C40 C41 1.404(4) . ? C41 C42 1.393(4) . ? C41 H41 0.9500 . ? C42 C43 1.380(5) . ? C42 H42 0.9500 . ? C43 C44 1.379(5) . ? C43 H43 0.9500 . ? C44 C45 1.386(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.394(4) . ? C46 C51 1.397(4) . ? C47 C48 1.392(5) . ? C47 H47 0.9500 . ? C48 C49 1.368(6) . ? C48 H48 0.9500 . ? C49 C50 1.380(5) . ? C49 H49 0.9500 . ? C50 C51 1.391(4) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.389(4) . ? C52 C57 1.476(4) . ? C53 C54 1.382(4) . ? C53 H53 0.9500 . ? C54 C55 1.379(4) . ? C54 H54 0.9500 . ? C55 C56 1.382(4) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.400(4) . ? C57 C62 1.410(4) . ? C58 C59 1.385(4) . ? C58 H58 0.9500 . ? C59 C60 1.382(4) . ? C59 H59 0.9500 . ? C60 C61 1.396(4) . ? C60 H60 0.9500 . ? C61 C62 1.404(4) . ? C61 H61 0.9500 . ? C63 C68 1.391(4) . ? C63 C64 1.399(4) . ? C64 C65 1.383(4) . ? C64 H64 0.9500 . ? C65 C66 1.383(5) . ? C65 H65 0.9500 . ? C66 C67 1.378(4) . ? C66 H66 0.9500 . ? C67 C68 1.387(4) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C69 1.524(5) 3_667 ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C76 1.393(4) . ? C70 C71 1.404(4) . ? C71 C72 1.392(4) . ? C71 H71 0.9500 . ? C72 C73 1.389(4) . ? C72 H72 0.9500 . ? C73 C75 1.389(5) . ? C73 C74 1.514(4) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.398(4) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C78 1.384(4) . ? C77 H77 0.9500 . ? C78 C79 1.384(4) . ? C78 H78 0.9500 . ? C79 C80 1.375(4) . ? C79 H79 0.9500 . ? C80 C81 1.396(4) . ? C80 H80 0.9500 . ? C81 C82 1.473(4) . ? C82 C87 1.399(4) . ? C82 C83 1.409(4) . ? C83 C84 1.397(4) . ? C84 C85 1.397(4) . ? C84 H84 0.9500 . ? C85 C86 1.376(5) . ? C85 H85 0.9500 . ? C86 C87 1.384(5) . ? C86 H86 0.9500 . ? C87 H87 0.9500 . ? C88 C89 1.393(4) . ? C88 C93 1.397(4) . ? C89 C90 1.391(4) . ? C89 H89 0.9500 . ? C90 C91 1.377(5) . ? C90 H90 0.9500 . ? C91 C92 1.383(5) . ? C91 H91 0.9500 . ? C92 C93 1.382(4) . ? C92 H92 0.9500 . ? C93 H93 0.9500 . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? 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 C1 Pt1 C62 91.24(11) . . ? C1 Pt1 N2 171.00(10) . . ? C62 Pt1 N2 79.83(10) . . ? C1 Pt1 P1 90.47(8) . . ? C62 Pt1 P1 173.27(7) . . ? N2 Pt1 P1 98.53(6) . . ? C33 Pt2 C22 91.03(12) . . ? C33 Pt2 N1 168.61(10) . . ? C22 Pt2 N1 79.70(11) . . ? C33 Pt2 P2 88.81(8) . . ? C22 Pt2 P2 176.30(8) . . ? N1 Pt2 P2 100.01(7) . . ? C70 Pt3 C83 91.85(11) . . ? C70 Pt3 N3 171.14(10) . . ? C83 Pt3 N3 79.47(10) . . ? C70 Pt3 P3 89.56(8) . . ? C83 Pt3 P3 178.23(8) . . ? N3 Pt3 P3 99.15(7) . . ? C40 P1 C46 107.15(13) . . ? C40 P1 C8 102.25(13) . . ? C46 P1 C8 101.27(13) . . ? C40 P1 Pt1 110.38(9) . . ? C46 P1 Pt1 119.79(9) . . ? C8 P1 Pt1 114.26(9) . . ? C16 P2 C10 109.11(14) . . ? C16 P2 C9 100.51(13) . . ? C10 P2 C9 101.23(14) . . ? C16 P2 Pt2 115.51(10) . . ? C10 P2 Pt2 113.81(9) . . ? C9 P2 Pt2 115.01(9) . . ? C88 P3 C63 108.22(13) . . ? C88 P3 C69 100.95(13) . . ? C63 P3 C69 102.11(13) . . ? C88 P3 Pt3 115.11(9) . . ? C63 P3 Pt3 113.03(9) . . ? C69 P3 Pt3 115.99(9) . . ? C32 N1 C28 118.8(3) . . ? C32 N1 Pt2 127.8(2) . . ? C28 N1 Pt2 112.9(2) . . ? C56 N2 C52 118.4(2) . . ? C56 N2 Pt1 126.67(19) . . ? C52 N2 Pt1 114.92(18) . . ? C77 N3 C81 118.2(3) . . ? C77 N3 Pt3 127.04(19) . . ? C81 N3 Pt3 114.64(19) . . ? C2 C1 C6 116.0(3) . . ? C2 C1 Pt1 121.7(2) . . ? C6 C1 Pt1 122.3(2) . . ? C3 C2 C1 122.0(3) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C4 C3 C2 121.5(4) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 117.6(3) . . ? C3 C4 C7 121.7(5) . . ? C5 C4 C7 120.7(4) . . ? C4 C5 C6 121.4(4) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 121.5(4) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 P1 115.69(19) . . ? C9 C8 H8A 108.4 . . ? P1 C8 H8A 108.4 . . ? C9 C8 H8B 108.4 . . ? P1 C8 H8B 108.4 . . ? H8A C8 H8B 107.4 . . ? C8 C9 P2 114.4(2) . . ? C8 C9 H9A 108.7 . . ? P2 C9 H9A 108.7 . . ? C8 C9 H9B 108.7 . . ? P2 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C11 C10 C15 118.1(3) . . ? C11 C10 P2 125.0(2) . . ? C15 C10 P2 116.8(2) . . ? C12 C11 C10 120.8(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C13 C12 C11 119.8(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.5(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C10 120.7(3) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? C17 C16 C21 117.9(3) . . ? C17 C16 P2 125.8(2) . . ? C21 C16 P2 115.7(2) . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 121.0(3) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 119.2(3) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C19 C20 C21 120.4(3) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C16 120.9(3) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? C27 C22 C23 116.9(3) . . ? C27 C22 Pt2 129.3(2) . . ? C23 C22 Pt2 113.6(2) . . ? C24 C23 C22 121.4(3) . . ? C24 C23 C28 122.7(3) . . ? C22 C23 C28 115.9(3) . . ? C25 C24 C23 120.2(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 120.5(3) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 121.1(3) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? N1 C28 C29 119.8(3) . . ? N1 C28 C23 114.9(3) . . ? C29 C28 C23 125.3(3) . . ? C30 C29 C28 120.5(3) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 119.4(3) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C30 C31 C32 118.3(3) . . ? C30 C31 H31 120.9 . . ? C32 C31 H31 120.9 . . ? N1 C32 C31 123.1(3) . . ? N1 C32 H32 118.5 . . ? C31 C32 H32 118.5 . . ? C38 C33 C34 115.8(3) . . ? C38 C33 Pt2 124.9(2) . . ? C34 C33 Pt2 119.3(2) . . ? C35 C34 C33 122.0(3) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? C36 C35 C34 121.5(3) . . ? C36 C35 H35 119.2 . . ? C34 C35 H35 119.2 . . ? C35 C36 C37 117.2(3) . . ? C35 C36 C39 121.1(3) . . ? C37 C36 C39 121.7(3) . . ? C36 C37 C38 121.2(3) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C33 C38 C37 122.3(3) . . ? C33 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C41 118.2(3) . . ? C45 C40 P1 117.1(2) . . ? C41 C40 P1 124.5(2) . . ? C42 C41 C40 120.1(3) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C43 C42 C41 120.6(3) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C44 C43 C42 119.9(3) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.2(3) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C40 121.0(3) . . ? C44 C45 H45 119.5 . . ? C40 C45 H45 119.5 . . ? C47 C46 C51 118.0(3) . . ? C47 C46 P1 117.1(2) . . ? C51 C46 P1 124.8(2) . . ? C48 C47 C46 120.8(3) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C49 C48 C47 120.3(4) . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C48 C49 C50 120.2(3) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C49 C50 C51 120.0(3) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C50 C51 C46 120.8(3) . . ? C50 C51 H51 119.6 . . ? C46 C51 H51 119.6 . . ? N2 C52 C53 120.6(3) . . ? N2 C52 C57 114.6(2) . . ? C53 C52 C57 124.8(3) . . ? C54 C53 C52 120.3(3) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C55 C54 C53 119.0(3) . . ? C55 C54 H54 120.5 . . ? C53 C54 H54 120.5 . . ? C54 C55 C56 118.4(3) . . ? C54 C55 H55 120.8 . . ? C56 C55 H55 120.8 . . ? N2 C56 C55 123.3(3) . . ? N2 C56 H56 118.4 . . ? C55 C56 H56 118.4 . . ? C58 C57 C62 121.7(3) . . ? C58 C57 C52 122.1(3) . . ? C62 C57 C52 116.2(2) . . ? C59 C58 C57 120.1(3) . . ? C59 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? C60 C59 C58 119.4(3) . . ? C60 C59 H59 120.3 . . ? C58 C59 H59 120.3 . . ? C59 C60 C61 120.6(3) . . ? C59 C60 H60 119.7 . . ? C61 C60 H60 119.7 . . ? C60 C61 C62 121.7(3) . . ? C60 C61 H61 119.1 . . ? C62 C61 H61 119.1 . . ? C61 C62 C57 116.4(3) . . ? C61 C62 Pt1 129.2(2) . . ? C57 C62 Pt1 114.4(2) . . ? C68 C63 C64 118.3(3) . . ? C68 C63 P3 125.9(2) . . ? C64 C63 P3 115.7(2) . . ? C65 C64 C63 121.1(3) . . ? C65 C64 H64 119.5 . . ? C63 C64 H64 119.5 . . ? C64 C65 C66 119.9(3) . . ? C64 C65 H65 120.1 . . ? C66 C65 H65 120.1 . . ? C67 C66 C65 119.6(3) . . ? C67 C66 H66 120.2 . . ? C65 C66 H66 120.2 . . ? C66 C67 C68 120.8(3) . . ? C66 C67 H67 119.6 . . ? C68 C67 H67 119.6 . . ? C67 C68 C63 120.3(3) . . ? C67 C68 H68 119.9 . . ? C63 C68 H68 119.9 . . ? C69 C69 P3 114.8(3) 3_667 . ? C69 C69 H69A 108.6 3_667 . ? P3 C69 H69A 108.6 . . ? C69 C69 H69B 108.6 3_667 . ? P3 C69 H69B 108.6 . . ? H69A C69 H69B 107.5 . . ? C76 C70 C71 115.6(3) . . ? C76 C70 Pt3 122.7(2) . . ? C71 C70 Pt3 121.6(2) . . ? C72 C71 C70 121.9(3) . . ? C72 C71 H71 119.0 . . ? C70 C71 H71 119.0 . . ? C73 C72 C71 121.8(3) . . ? C73 C72 H72 119.1 . . ? C71 C72 H72 119.1 . . ? C72 C73 C75 116.9(3) . . ? C72 C73 C74 121.3(3) . . ? C75 C73 C74 121.8(3) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 C76 121.3(3) . . ? C73 C75 H75 119.3 . . ? C76 C75 H75 119.3 . . ? C70 C76 C75 122.4(3) . . ? C70 C76 H76 118.8 . . ? C75 C76 H76 118.8 . . ? N3 C77 C78 123.3(3) . . ? N3 C77 H77 118.3 . . ? C78 C77 H77 118.3 . . ? C77 C78 C79 118.4(3) . . ? C77 C78 H78 120.8 . . ? C79 C78 H78 120.8 . . ? C80 C79 C78 119.1(3) . . ? C80 C79 H79 120.5 . . ? C78 C79 H79 120.5 . . ? C79 C80 C81 120.2(3) . . ? C79 C80 H80 119.9 . . ? C81 C80 H80 119.9 . . ? N3 C81 C80 120.7(3) . . ? N3 C81 C82 115.0(2) . . ? C80 C81 C82 124.2(3) . . ? C87 C82 C83 121.6(3) . . ? C87 C82 C81 122.3(3) . . ? C83 C82 C81 116.0(2) . . ? C84 C83 C82 116.7(3) . . ? C84 C83 Pt3 128.5(2) . . ? C82 C83 Pt3 114.8(2) . . ? C85 C84 C83 121.7(3) . . ? C85 C84 H84 119.1 . . ? C83 C84 H84 119.1 . . ? C86 C85 C84 120.2(3) . . ? C86 C85 H85 119.9 . . ? C84 C85 H85 119.9 . . ? C85 C86 C87 120.0(3) . . ? C85 C86 H86 120.0 . . ? C87 C86 H86 120.0 . . ? C86 C87 C82 119.7(3) . . ? C86 C87 H87 120.1 . . ? C82 C87 H87 120.1 . . ? C89 C88 C93 117.7(3) . . ? C89 C88 P3 124.4(2) . . ? C93 C88 P3 117.8(2) . . ? C90 C89 C88 120.8(3) . . ? C90 C89 H89 119.6 . . ? C88 C89 H89 119.6 . . ? C91 C90 C89 120.7(3) . . ? C91 C90 H90 119.7 . . ? C89 C90 H90 119.7 . . ? C90 C91 C92 119.2(3) . . ? C90 C91 H91 120.4 . . ? C92 C91 H91 120.4 . . ? C93 C92 C91 120.4(3) . . ? C93 C92 H92 119.8 . . ? C91 C92 H92 119.8 . . ? C92 C93 C88 121.2(3) . . ? C92 C93 H93 119.4 . . ? C88 C93 H93 119.4 . . ? Cl1 C94 Cl2 113.1(3) . . ? Cl1 C94 H94A 109.0 . . ? Cl2 C94 H94A 109.0 . . ? Cl1 C94 H94B 109.0 . . ? Cl2 C94 H94B 109.0 . . ? H94A C94 H94B 107.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.055 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.112 # Attachment '- 6b.cif' data_6b _database_code_depnum_ccdc_archive 'CCDC 784482' #TrackingRef '- 6b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H54 N2 P2 Pt2, 2(C H2 Cl2)' _chemical_formula_sum 'C68 H58 Cl4 N2 P2 Pt2' _chemical_formula_weight 1497.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _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 13.5252(9) _cell_length_b 14.6944(10) _cell_length_c 15.0201(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.079(3) _cell_angle_gamma 90.00 _cell_volume 2939.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 49129 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 27.52 _exptl_crystal_description block _exptl_crystal_colour yellow-green _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 5.035 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8407 _exptl_absorpt_correction_T_max 0.9181 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49129 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6751 _reflns_number_gt 6297 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0093P)^2^+4.4085P] 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 6751 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0184 _refine_ls_R_factor_gt 0.0161 _refine_ls_wR_factor_ref 0.0359 _refine_ls_wR_factor_gt 0.0352 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.418244(6) 0.774029(5) 0.960407(5) 0.01199(3) Uani 1 1 d . . . P1 P 0.52400(4) 0.64970(3) 0.96819(3) 0.01254(10) Uani 1 1 d . . . Cl1 Cl 0.43189(6) 0.65109(5) 1.45182(5) 0.04429(17) Uani 1 1 d . . . N1 N 0.51251(13) 0.87289(11) 0.91358(11) 0.0142(3) Uani 1 1 d . . . C1 C 0.31221(16) 0.70068(13) 1.00633(15) 0.0168(4) Uani 1 1 d . . . Cl2 Cl 0.38013(7) 0.80857(6) 1.33846(6) 0.0564(2) Uani 1 1 d . . . C2 C 0.24050(17) 0.64816(15) 0.94997(16) 0.0240(5) Uani 1 1 d . . . H2A H 0.2460 0.6408 0.8882 0.029 Uiso 1 1 calc R . . C3 C 0.16098(18) 0.60620(17) 0.98266(19) 0.0313(6) Uani 1 1 d . . . H3A H 0.1143 0.5704 0.9428 0.038 Uiso 1 1 calc R . . C4 C 0.14898(18) 0.61595(17) 1.07226(19) 0.0298(6) Uani 1 1 d . . . C5 C 0.0620(2) 0.5714(2) 1.1075(2) 0.0478(8) Uani 1 1 d . . . H5A H 0.0780 0.5074 1.1215 0.072 Uiso 1 1 calc R . . H5B H 0.0012 0.5752 1.0613 0.072 Uiso 1 1 calc R . . H5C H 0.0507 0.6029 1.1624 0.072 Uiso 1 1 calc R . . C6 C 0.21982(18) 0.66687(16) 1.12850(17) 0.0274(5) Uani 1 1 d . . . H6A H 0.2138 0.6743 1.1902 0.033 Uiso 1 1 calc R . . C7 C 0.30000(18) 0.70763(15) 1.09652(16) 0.0227(5) Uani 1 1 d . . . H7A H 0.3479 0.7412 1.1375 0.027 Uiso 1 1 calc R . . C8 C 0.32176(15) 0.88240(13) 0.94434(13) 0.0143(4) Uani 1 1 d . . . C9 C 0.22314(16) 0.89140(14) 0.95887(14) 0.0179(4) Uani 1 1 d . . . H9A H 0.1926 0.8422 0.9849 0.021 Uiso 1 1 calc R . . C10 C 0.16773(17) 0.97191(15) 0.93571(15) 0.0213(5) Uani 1 1 d . . . H10A H 0.1005 0.9754 0.9461 0.026 Uiso 1 1 calc R . . C11 C 0.20850(17) 1.04534(15) 0.89859(15) 0.0222(5) Uani 1 1 d . . . H11A H 0.1695 1.0986 0.8829 0.027 Uiso 1 1 calc R . . C12 C 0.30858(16) 1.04111(14) 0.88398(14) 0.0175(4) Uani 1 1 d . . . C13 C 0.36273(15) 0.95970(13) 0.90719(13) 0.0140(4) Uani 1 1 d . . . C14 C 0.46461(16) 0.95453(13) 0.89263(13) 0.0144(4) Uani 1 1 d . . . C15 C 0.51244(16) 1.02922(14) 0.85980(13) 0.0168(4) Uani 1 1 d . . . C16 C 0.45494(18) 1.11083(14) 0.83782(15) 0.0218(5) Uani 1 1 d . . . H16A H 0.4858 1.1623 0.8159 0.026 Uiso 1 1 calc R . . C17 C 0.35747(18) 1.11584(15) 0.84778(15) 0.0226(5) Uani 1 1 d . . . H17A H 0.3206 1.1699 0.8305 0.027 Uiso 1 1 calc R . . C18 C 0.61390(17) 1.01991(14) 0.85220(14) 0.0194(4) Uani 1 1 d . . . H18A H 0.6491 1.0695 0.8318 0.023 Uiso 1 1 calc R . . C19 C 0.66194(16) 0.93857(15) 0.87456(14) 0.0196(4) Uani 1 1 d . . . H19A H 0.7306 0.9313 0.8696 0.024 Uiso 1 1 calc R . . C20 C 0.60873(16) 0.86667(14) 0.90462(14) 0.0181(4) Uani 1 1 d . . . H20A H 0.6427 0.8106 0.9194 0.022 Uiso 1 1 calc R . . C21 C 0.57119(15) 0.62542(14) 0.86374(13) 0.0151(4) Uani 1 1 d . . . C22 C 0.64942(16) 0.56420(14) 0.85805(14) 0.0191(4) Uani 1 1 d . . . H22A H 0.6837 0.5354 0.9112 0.023 Uiso 1 1 calc R . . C23 C 0.67695(18) 0.54546(16) 0.77517(16) 0.0244(5) Uani 1 1 d . . . H23A H 0.7294 0.5033 0.7717 0.029 Uiso 1 1 calc R . . C24 C 0.62808(19) 0.58818(17) 0.69714(16) 0.0285(5) Uani 1 1 d . . . H24A H 0.6471 0.5752 0.6405 0.034 Uiso 1 1 calc R . . C25 C 0.55167(19) 0.64959(17) 0.70211(15) 0.0283(5) Uani 1 1 d . . . H25A H 0.5190 0.6796 0.6490 0.034 Uiso 1 1 calc R . . C26 C 0.52273(17) 0.66731(15) 0.78454(14) 0.0217(5) Uani 1 1 d . . . H26A H 0.4692 0.7085 0.7872 0.026 Uiso 1 1 calc R . . C27 C 0.63507(16) 0.65388(13) 1.05728(13) 0.0154(4) Uani 1 1 d . . . C28 C 0.62153(18) 0.63757(15) 1.14602(14) 0.0225(5) Uani 1 1 d . . . H28A H 0.5564 0.6238 1.1577 0.027 Uiso 1 1 calc R . . C29 C 0.7017(2) 0.64122(16) 1.21706(16) 0.0309(6) Uani 1 1 d . . . H29A H 0.6917 0.6287 1.2769 0.037 Uiso 1 1 calc R . . C30 C 0.7969(2) 0.66325(16) 1.20090(17) 0.0326(6) Uani 1 1 d . . . H30A H 0.8521 0.6659 1.2496 0.039 Uiso 1 1 calc R . . C31 C 0.81099(18) 0.68114(16) 1.11413(17) 0.0289(5) Uani 1 1 d . . . H31A H 0.8759 0.6970 1.1033 0.035 Uiso 1 1 calc R . . C32 C 0.73068(16) 0.67619(14) 1.04180(15) 0.0201(4) Uani 1 1 d . . . H32A H 0.7413 0.6881 0.9820 0.024 Uiso 1 1 calc R . . C33 C 0.46579(15) 0.54157(13) 0.99335(14) 0.0157(4) Uani 1 1 d . . . H33A H 0.4367 0.5500 1.0489 0.019 Uiso 1 1 calc R . . H33B H 0.4095 0.5285 0.9433 0.019 Uiso 1 1 calc R . . C34 C 0.4711(2) 0.7248(2) 1.3728(2) 0.0506(8) Uani 1 1 d . . . H34A H 0.5351 0.7542 1.4001 0.061 Uiso 1 1 calc R . . H34B H 0.4829 0.6896 1.3195 0.061 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 0.01177(4) 0.01062(4) 0.01400(4) 0.00085(3) 0.00338(3) 0.00001(3) P1 0.0128(2) 0.0112(2) 0.0139(2) 0.00079(18) 0.00317(19) -0.00006(19) Cl1 0.0452(4) 0.0441(4) 0.0459(4) 0.0146(3) 0.0145(3) 0.0072(3) N1 0.0153(9) 0.0138(8) 0.0136(8) -0.0010(6) 0.0028(7) -0.0005(7) C1 0.0137(10) 0.0113(9) 0.0261(11) 0.0036(8) 0.0055(8) 0.0018(8) Cl2 0.0759(6) 0.0510(5) 0.0478(4) 0.0205(4) 0.0259(4) 0.0248(4) C2 0.0191(11) 0.0228(11) 0.0302(12) 0.0018(9) 0.0043(9) -0.0013(9) C3 0.0177(12) 0.0284(13) 0.0462(15) 0.0062(11) 0.0012(11) -0.0064(10) C4 0.0177(12) 0.0255(12) 0.0488(15) 0.0146(11) 0.0134(11) 0.0029(10) C5 0.0251(14) 0.0511(18) 0.071(2) 0.0227(16) 0.0204(14) -0.0028(13) C6 0.0286(13) 0.0258(12) 0.0323(13) 0.0093(10) 0.0174(10) 0.0056(10) C7 0.0250(12) 0.0174(10) 0.0274(12) 0.0026(9) 0.0089(9) -0.0008(9) C8 0.0149(10) 0.0137(9) 0.0138(9) -0.0014(7) 0.0012(8) 0.0003(8) C9 0.0171(11) 0.0172(10) 0.0198(10) -0.0009(8) 0.0043(8) -0.0005(8) C10 0.0154(11) 0.0215(11) 0.0274(11) -0.0029(9) 0.0053(9) 0.0034(9) C11 0.0204(11) 0.0174(10) 0.0286(12) 0.0002(9) 0.0038(9) 0.0071(9) C12 0.0197(11) 0.0148(10) 0.0175(10) 0.0000(8) 0.0019(8) 0.0021(8) C13 0.0163(10) 0.0134(9) 0.0120(9) -0.0017(7) 0.0017(8) 0.0003(8) C14 0.0176(10) 0.0136(9) 0.0117(9) -0.0011(7) 0.0015(8) -0.0008(8) C15 0.0216(11) 0.0143(9) 0.0148(9) -0.0004(7) 0.0039(8) -0.0020(8) C16 0.0286(12) 0.0139(10) 0.0237(11) 0.0034(8) 0.0072(9) -0.0008(9) C17 0.0285(13) 0.0140(10) 0.0251(11) 0.0023(8) 0.0040(9) 0.0038(9) C18 0.0219(11) 0.0178(10) 0.0200(10) 0.0016(8) 0.0076(9) -0.0054(9) C19 0.0151(10) 0.0234(11) 0.0213(10) 0.0013(8) 0.0061(8) -0.0025(8) C20 0.0172(11) 0.0179(10) 0.0197(10) 0.0025(8) 0.0047(8) 0.0018(8) C21 0.0153(10) 0.0156(9) 0.0154(9) -0.0019(7) 0.0054(8) -0.0017(8) C22 0.0198(11) 0.0178(10) 0.0203(10) 0.0017(8) 0.0053(8) 0.0016(8) C23 0.0249(12) 0.0244(11) 0.0268(12) -0.0014(9) 0.0126(10) 0.0046(10) C24 0.0331(14) 0.0360(13) 0.0189(11) -0.0029(10) 0.0114(10) 0.0010(11) C25 0.0319(14) 0.0363(14) 0.0162(11) 0.0033(9) 0.0029(10) 0.0055(11) C26 0.0207(11) 0.0251(11) 0.0190(10) 0.0012(9) 0.0025(9) 0.0060(9) C27 0.0180(11) 0.0119(9) 0.0155(9) 0.0007(7) 0.0008(8) 0.0010(8) C28 0.0275(12) 0.0202(11) 0.0194(10) 0.0019(8) 0.0030(9) -0.0050(9) C29 0.0433(16) 0.0263(12) 0.0194(11) 0.0057(9) -0.0045(10) -0.0084(11) C30 0.0332(14) 0.0244(12) 0.0325(13) 0.0076(10) -0.0153(11) -0.0053(10) C31 0.0186(12) 0.0236(12) 0.0412(14) 0.0025(10) -0.0038(10) -0.0028(10) C32 0.0182(11) 0.0172(10) 0.0243(11) 0.0012(8) 0.0019(9) 0.0001(9) C33 0.0148(10) 0.0111(9) 0.0217(10) 0.0006(8) 0.0045(8) -0.0006(8) C34 0.0418(18) 0.0533(19) 0.062(2) 0.0218(16) 0.0253(16) 0.0107(15) _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 C1 2.010(2) . ? Pt1 C8 2.046(2) . ? Pt1 N1 2.1318(17) . ? Pt1 P1 2.3106(5) . ? P1 C21 1.829(2) . ? P1 C27 1.830(2) . ? P1 C33 1.842(2) . ? Cl1 C34 1.756(3) . ? N1 C20 1.335(3) . ? N1 C14 1.373(3) . ? C1 C7 1.397(3) . ? C1 C2 1.402(3) . ? Cl2 C34 1.752(3) . ? C2 C3 1.401(3) . ? C2 H2A 0.9500 . ? C3 C4 1.391(4) . ? C3 H3A 0.9500 . ? C4 C6 1.381(4) . ? C4 C5 1.520(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.396(3) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.395(3) . ? C8 C13 1.420(3) . ? C9 C10 1.411(3) . ? C9 H9A 0.9500 . ? C10 C11 1.374(3) . ? C10 H10A 0.9500 . ? C11 C12 1.410(3) . ? C11 H11A 0.9500 . ? C12 C13 1.414(3) . ? C12 C17 1.437(3) . ? C13 C14 1.434(3) . ? C14 C15 1.406(3) . ? C15 C18 1.404(3) . ? C15 C16 1.436(3) . ? C16 C17 1.355(3) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.374(3) . ? C18 H18A 0.9500 . ? C19 C20 1.397(3) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C26 1.397(3) . ? C21 C22 1.403(3) . ? C22 C23 1.388(3) . ? C22 H22A 0.9500 . ? C23 C24 1.391(3) . ? C23 H23A 0.9500 . ? C24 C25 1.384(3) . ? C24 H24A 0.9500 . ? C25 C26 1.387(3) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C32 1.393(3) . ? C27 C28 1.397(3) . ? C28 C29 1.383(3) . ? C28 H28A 0.9500 . ? C29 C30 1.390(4) . ? C29 H29A 0.9500 . ? C30 C31 1.375(4) . ? C30 H30A 0.9500 . ? C31 C32 1.397(3) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C33 1.525(4) 3_667 ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? 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 C1 Pt1 C8 88.81(8) . . ? C1 Pt1 N1 169.25(7) . . ? C8 Pt1 N1 80.60(7) . . ? C1 Pt1 P1 91.79(6) . . ? C8 Pt1 P1 176.11(6) . . ? N1 Pt1 P1 98.91(5) . . ? C21 P1 C27 105.59(10) . . ? C21 P1 C33 103.51(9) . . ? C27 P1 C33 101.81(9) . . ? C21 P1 Pt1 114.62(7) . . ? C27 P1 Pt1 115.61(7) . . ? C33 P1 Pt1 114.17(7) . . ? C20 N1 C14 117.77(18) . . ? C20 N1 Pt1 129.54(14) . . ? C14 N1 Pt1 112.67(13) . . ? C7 C1 C2 116.0(2) . . ? C7 C1 Pt1 120.41(16) . . ? C2 C1 Pt1 123.21(17) . . ? C3 C2 C1 121.5(2) . . ? C3 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C4 C3 C2 121.4(2) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C6 C4 C3 117.5(2) . . ? C6 C4 C5 121.1(3) . . ? C3 C4 C5 121.4(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 C7 121.3(2) . . ? C4 C6 H6A 119.3 . . ? C7 C6 H6A 119.3 . . ? C6 C7 C1 122.2(2) . . ? C6 C7 H7A 118.9 . . ? C1 C7 H7A 118.9 . . ? C9 C8 C13 115.79(18) . . ? C9 C8 Pt1 131.52(15) . . ? C13 C8 Pt1 112.59(14) . . ? C8 C9 C10 121.5(2) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C11 C10 C9 121.7(2) . . ? C11 C10 H10A 119.2 . . ? C9 C10 H10A 119.2 . . ? C10 C11 C12 119.5(2) . . ? C10 C11 H11A 120.2 . . ? C12 C11 H11A 120.2 . . ? C11 C12 C13 117.96(19) . . ? C11 C12 C17 122.9(2) . . ? C13 C12 C17 119.1(2) . . ? C12 C13 C8 123.55(19) . . ? C12 C13 C14 118.50(18) . . ? C8 C13 C14 117.95(18) . . ? N1 C14 C15 122.31(19) . . ? N1 C14 C13 116.01(18) . . ? C15 C14 C13 121.68(18) . . ? C18 C15 C14 117.95(19) . . ? C18 C15 C16 124.1(2) . . ? C14 C15 C16 117.9(2) . . ? C17 C16 C15 121.2(2) . . ? C17 C16 H16A 119.4 . . ? C15 C16 H16A 119.4 . . ? C16 C17 C12 121.4(2) . . ? C16 C17 H17A 119.3 . . ? C12 C17 H17A 119.3 . . ? C19 C18 C15 119.5(2) . . ? C19 C18 H18A 120.3 . . ? C15 C18 H18A 120.3 . . ? C18 C19 C20 119.3(2) . . ? C18 C19 H19A 120.4 . . ? C20 C19 H19A 120.4 . . ? N1 C20 C19 123.2(2) . . ? N1 C20 H20A 118.4 . . ? C19 C20 H20A 118.4 . . ? C26 C21 C22 118.51(19) . . ? C26 C21 P1 117.54(16) . . ? C22 C21 P1 123.88(16) . . ? C23 C22 C21 120.4(2) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C24 120.3(2) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C25 C24 C23 119.9(2) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C24 C25 C26 120.1(2) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 C21 120.9(2) . . ? C25 C26 H26A 119.5 . . ? C21 C26 H26A 119.5 . . ? C32 C27 C28 118.70(19) . . ? C32 C27 P1 123.60(16) . . ? C28 C27 P1 117.64(17) . . ? C29 C28 C27 120.9(2) . . ? C29 C28 H28A 119.6 . . ? C27 C28 H28A 119.6 . . ? C28 C29 C30 120.0(2) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 119.7(2) . . ? C31 C30 H30A 120.1 . . ? C29 C30 H30A 120.1 . . ? C30 C31 C32 120.6(2) . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C27 C32 C31 120.0(2) . . ? C27 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C33 C33 P1 116.54(19) 3_667 . ? C33 C33 H33A 108.2 3_667 . ? P1 C33 H33A 108.2 . . ? C33 C33 H33B 108.2 3_667 . ? P1 C33 H33B 108.2 . . ? H33A C33 H33B 107.3 . . ? Cl2 C34 Cl1 110.65(17) . . ? Cl2 C34 H34A 109.5 . . ? Cl1 C34 H34A 109.5 . . ? Cl2 C34 H34B 109.5 . . ? Cl1 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.710 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.082