#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/27/2012717.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2012717 loop_ _publ_author_name 'Bruno, Giuseppe' 'Lanza, Santo' 'Nicol\'o, Francesco' 'Tresoldi, Giuseppe' 'Rosace, Giuseppe' _publ_section_title ;(\h^3^-Allyl-2\k^3^C)(chloro-1\kCl)(\m-N,N'-diethyldithioxamidato-1:2\k^4^S,S':N,N')[diphenyl(2-pyridyl)phosphine-1\kP]palladium(II)platinum(II) chloroform solvate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m316 _journal_page_last m318 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Pd Pt (C3 H5) (C6 H10 N2 S2) (C17 H14 N P) Cl] C H Cl3' _chemical_formula_moiety 'C26 H29 Cl N3 P Pd Pt S2 , C H Cl3' _chemical_formula_sum 'C27 H30 Cl4 N3 P Pd Pt S2' _chemical_formula_weight 934.92 _chemical_name_systematic ;(\h^3^-Allyl-2\k^3^C)(chloro-1\kCl)(\m-N,N'-diethyldithioxamidato- 1:2\k^4^S,S':N,N')[diphenyl(2-pyridyl)phosphine-1\kP]palladium(II)platinum(II) chloroform solvate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 106.83(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.423(3) _cell_length_b 13.561(3) _cell_length_c 19.156(4) _cell_measurement_reflns_used 50 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 15.0 _cell_measurement_theta_min 6.3 _cell_volume 3337.6(14) _computing_cell_refinement P3/V _computing_data_collection 'P3/V (Siemens, 1989)' _computing_data_reduction 'SHELXTL-Plus (Siemens, 1990)' _computing_molecular_graphics 'XPW in SHELXTL (Siemens, 1996)' _computing_publication_material 'PARST95 (Nardelli, 1995, locally modified) and SHELXL97' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.100 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 7636 _diffrn_reflns_theta_full 27.07 _diffrn_reflns_theta_max 27.07 _diffrn_reflns_theta_min 1.87 _diffrn_standards_decay_% 10 _diffrn_standards_interval_count 197 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.241 _exptl_absorpt_correction_T_max 0.456 _exptl_absorpt_correction_T_min 0.249 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(Kopfmann & Huber, 1968)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.861 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 1808 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.20 _refine_diff_density_min -0.82 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.801 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 361 _refine_ls_number_reflns 7328 _refine_ls_number_restraints 36 _refine_ls_restrained_S_all 0.835 _refine_ls_R_factor_all 0.088 _refine_ls_R_factor_gt 0.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0424P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.082 _refine_ls_wR_factor_ref 0.089 _reflns_number_gt 3944 _reflns_number_total 7328 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file na1566.cif _[local]_cod_data_source_block IV _[local]_cod_cif_authors_sg_H-M 'P 21/c' _[local]_cod_cif_authors_sg_Hall 'P 2ybc' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 3337.0(10) _cod_database_code 2012717 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Pt 0.31771(2) 0.27755(2) 0.507707(15) 0.04267(10) Uani d . 1 . . Pt Pd 0.42874(6) -0.13022(5) 0.59334(4) 0.0664(2) Uani d . 1 . . Pd Cl1 0.32558(18) 0.42133(16) 0.57598(11) 0.0672(6) Uani d . 1 . . Cl S1 0.31647(18) 0.13494(15) 0.44664(10) 0.0572(6) Uani d . 1 B . S S2 0.42803(17) 0.20524(14) 0.61092(10) 0.0593(6) Uani d . 1 . . S P 0.20184(15) 0.34915(14) 0.41166(10) 0.0412(5) Uani d . 1 . . P N1 0.3727(5) -0.0435(4) 0.5013(3) 0.0513(16) Uani d . 1 B . N N2 0.4487(6) 0.0114(5) 0.6368(4) 0.091(3) Uani d . 1 B . N C1 0.3712(6) 0.0487(5) 0.5126(4) 0.0438(18) Uani d . 1 . . C C2 0.4185(6) 0.0819(6) 0.5901(4) 0.062(2) Uani d . 1 B . C C3 0.3263(9) -0.0840(6) 0.4284(5) 0.087(3) Uani d . 1 . . C H3A 0.3661 -0.1408 0.4212 0.104 Uiso calc R 1 B . H H3B 0.3285 -0.0348 0.3921 0.104 Uiso calc R 1 . . H C4 0.2134(9) -0.1146(8) 0.4187(6) 0.116(4) Uani d U 1 B . C H4A 0.1842 -0.1410 0.3706 0.174 Uiso calc R 1 . . H H4B 0.1739 -0.0581 0.4252 0.174 Uiso calc R 1 . . H H4C 0.2114 -0.1638 0.4543 0.174 Uiso calc R 1 . . H C5 0.4750(10) 0.0290(9) 0.7255(7) 0.123(5) Uani d U 1 . . C H5A 0.4451 0.0895 0.7374 0.148 Uiso calc R 1 B . H H5B 0.4545 -0.0265 0.7502 0.148 Uiso calc R 1 . . H C6 0.5862(14) 0.0354(9) 0.7387(7) 0.166(7) Uani d . 1 B . C H6A 0.6189 0.0471 0.7896 0.249 Uiso calc R 1 . . H H6B 0.6021 0.0886 0.7107 0.249 Uiso calc R 1 . . H H6C 0.6117 -0.0254 0.7246 0.249 Uiso calc R 1 . . H C7 0.4105(10) -0.2773(7) 0.5586(7) 0.094(3) Uani d . 1 B . C H7A 0.3461 -0.3096 0.5588 0.113 Uiso calc R 1 A 1 H H7B 0.4344 -0.2942 0.5169 0.113 Uiso calc R 1 A 1 H C8A 0.488(3) -0.2676(19) 0.627(2) 0.102(10) Uani d P 0.50 B 1 C H8A 0.5600 -0.2801 0.6274 0.123 Uiso calc PR 0.50 B 1 H C8B 0.411(3) -0.2761(19) 0.6245(17) 0.093(8) Uani d P 0.50 B 2 C H8B 0.3421 -0.2888 0.6308 0.111 Uiso calc PR 0.50 B 2 H C9 0.4745(14) -0.2261(8) 0.6811(7) 0.137(6) Uani d . 1 B . C H9A 0.5368 -0.2083 0.7194 0.164 Uiso calc R 1 C 1 H H9B 0.4196 -0.2524 0.6994 0.164 Uiso calc R 1 C 1 H C10 0.1780(6) 0.2810(5) 0.3266(4) 0.0470(18) Uani d . 1 . . C C11 0.1068(7) 0.2018(6) 0.3116(4) 0.063(2) Uani d . 1 . . C H11 0.0652 0.1895 0.3420 0.076 Uiso calc R 1 . . H C12 0.0994(8) 0.1431(7) 0.2522(5) 0.088(3) Uani d . 1 . . C H12 0.0527 0.0908 0.2423 0.105 Uiso calc R 1 . . H C13 0.1605(9) 0.1611(7) 0.2069(5) 0.084(3) Uani d . 1 . . C H13 0.1563 0.1209 0.1669 0.101 Uiso calc R 1 . . H C14 0.2271(8) 0.2389(7) 0.2219(5) 0.083(3) Uani d . 1 . . C H14 0.2674 0.2528 0.1909 0.100 Uiso calc R 1 . . H C15 0.2361(6) 0.2967(6) 0.2814(4) 0.058(2) Uani d . 1 . . C H15 0.2837 0.3484 0.2910 0.070 Uiso calc R 1 . . H C16 0.2430(6) 0.4702(5) 0.3891(4) 0.0440(18) Uani d . 1 . . C C17 0.3480(7) 0.4905(6) 0.4034(5) 0.064(2) Uani d . 1 . . C H17 0.3972 0.4442 0.4274 0.077 Uiso calc R 1 . . H C18 0.3798(8) 0.5804(7) 0.3820(5) 0.080(3) Uani d . 1 . . C H18 0.4502 0.5949 0.3912 0.096 Uiso calc R 1 . . H C19 0.3069(10) 0.6457(7) 0.3476(5) 0.085(3) Uani d . 1 . . C H19 0.3267 0.7062 0.3330 0.102 Uiso calc R 1 . . H C20 0.2051(9) 0.6240(7) 0.3342(6) 0.093(3) Uani d . 1 . . C H20 0.1562 0.6705 0.3100 0.111 Uiso calc R 1 . . H N3 0.1702(6) 0.5361(6) 0.3547(4) 0.086(2) Uani d . 1 . . N C21 0.0750(6) 0.3634(5) 0.4253(5) 0.055(2) Uani d . 1 . . C C22 -0.0092(7) 0.3918(6) 0.3682(6) 0.078(3) Uani d . 1 . . C H22 -0.0013 0.4018 0.3221 0.094 Uiso calc R 1 . . H C23 -0.1061(8) 0.4053(8) 0.3799(8) 0.100(4) Uani d . 1 . . C H23 -0.1635 0.4234 0.3415 0.121 Uiso calc R 1 . . H C24 -0.1159(9) 0.3915(8) 0.4487(8) 0.099(4) Uani d . 1 . . C H24 -0.1797 0.4031 0.4572 0.119 Uiso calc R 1 . . H C25 -0.0344(10) 0.3613(8) 0.5040(7) 0.102(4) Uani d . 1 . . C H25 -0.0428 0.3496 0.5498 0.123 Uiso calc R 1 . . H C26 0.0605(7) 0.3480(7) 0.4927(5) 0.067(2) Uani d . 1 . . C H26 0.1165 0.3280 0.5313 0.081 Uiso calc R 1 . . H C27 -0.1648(14) 0.0094(14) 0.3448(10) 0.191(7) Uani d U 1 . . C H27 -0.2284 0.0038 0.3040 0.229 Uiso calc R 1 . . H Cl2 -0.0424(5) -0.0341(4) 0.3355(3) 0.231(2) Uani d U 1 . . Cl Cl3 -0.1473(5) -0.0720(4) 0.4356(3) 0.253(3) Uani d U 1 . . Cl Cl4 -0.1332(6) 0.1202(5) 0.3909(5) 0.318(4) Uani d U 1 . . Cl loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt 0.04411(17) 0.03947(16) 0.04363(15) 0.00331(17) 0.01144(12) 0.00032(16) Pd 0.0730(5) 0.0442(4) 0.0755(5) 0.0028(4) 0.0112(4) 0.0154(3) Cl1 0.0750(16) 0.0555(13) 0.0631(13) 0.0071(12) 0.0076(12) -0.0171(11) S1 0.0844(17) 0.0434(11) 0.0417(11) 0.0111(12) 0.0152(11) 0.0007(9) S2 0.0701(15) 0.0436(13) 0.0515(11) 0.0008(11) -0.0026(10) 0.0010(9) P 0.0396(11) 0.0381(11) 0.0455(11) 0.0010(9) 0.0116(9) -0.0008(9) N1 0.062(4) 0.039(4) 0.052(4) 0.006(3) 0.014(3) -0.001(3) N2 0.116(7) 0.047(5) 0.076(5) -0.007(5) -0.024(5) 0.011(4) C1 0.039(4) 0.042(5) 0.049(4) 0.003(4) 0.012(4) 0.007(4) C2 0.059(6) 0.052(5) 0.062(5) -0.005(5) -0.004(4) 0.015(4) C3 0.151(11) 0.046(5) 0.076(7) 0.030(6) 0.050(7) -0.005(5) C4 0.104(7) 0.106(7) 0.114(7) 0.011(6) -0.006(6) -0.032(6) C5 0.120(8) 0.089(7) 0.130(8) 0.016(7) -0.013(7) -0.023(6) C6 0.28(2) 0.097(10) 0.143(12) 0.008(13) 0.098(14) 0.027(9) C7 0.122(11) 0.044(6) 0.124(9) -0.014(7) 0.050(9) -0.008(7) C8A 0.12(2) 0.035(14) 0.15(3) 0.034(17) 0.03(3) -0.003(15) C8B 0.12(2) 0.049(13) 0.10(2) -0.022(18) 0.015(19) 0.022(16) C9 0.205(16) 0.053(7) 0.117(10) -0.018(10) -0.010(12) 0.051(7) C10 0.055(5) 0.037(4) 0.044(4) 0.004(4) 0.007(4) -0.003(4) C11 0.072(6) 0.063(6) 0.054(5) -0.009(5) 0.018(4) -0.012(4) C12 0.110(9) 0.077(7) 0.063(6) -0.030(6) 0.004(6) -0.022(6) C13 0.129(10) 0.064(7) 0.054(6) 0.003(7) 0.020(6) -0.018(5) C14 0.105(8) 0.082(8) 0.073(6) 0.005(6) 0.045(6) -0.001(6) C15 0.072(6) 0.051(6) 0.055(5) -0.007(4) 0.025(5) -0.010(4) C16 0.045(5) 0.042(4) 0.044(4) -0.004(4) 0.011(4) -0.001(3) C17 0.052(6) 0.046(5) 0.096(7) -0.007(4) 0.025(5) 0.003(5) C18 0.085(8) 0.070(7) 0.090(7) -0.024(6) 0.034(6) -0.011(6) C19 0.118(10) 0.048(6) 0.096(8) -0.019(7) 0.040(7) 0.000(5) C20 0.086(8) 0.046(6) 0.147(10) 0.006(6) 0.035(8) 0.025(6) N3 0.082(6) 0.064(5) 0.101(6) 0.003(5) 0.009(5) 0.010(5) C21 0.041(5) 0.040(4) 0.081(6) -0.003(4) 0.015(5) 0.005(4) C22 0.050(6) 0.060(6) 0.119(8) 0.012(5) 0.017(6) 0.035(6) C23 0.056(7) 0.074(7) 0.165(12) 0.010(6) 0.022(8) 0.032(8) C24 0.062(8) 0.062(7) 0.190(14) -0.004(6) 0.064(9) -0.022(8) C25 0.092(9) 0.100(9) 0.134(10) -0.005(8) 0.063(8) -0.032(8) C26 0.055(6) 0.079(7) 0.074(6) -0.010(5) 0.028(5) -0.010(5) C27 0.182(10) 0.184(10) 0.220(11) -0.030(9) 0.079(9) -0.020(9) Cl2 0.226(5) 0.263(6) 0.218(5) -0.022(4) 0.085(4) 0.009(4) Cl3 0.310(6) 0.215(5) 0.297(6) -0.037(5) 0.191(5) 0.004(5) Cl4 0.333(7) 0.250(6) 0.437(8) 0.000(5) 0.215(6) -0.007(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt P . 2.256(2) yes Pt S1 . 2.258(2) yes Pt S2 . 2.317(2) yes Pt Cl1 . 2.333(2) yes Pd N1 . 2.071(6) yes Pd N2 . 2.079(7) yes Pd C7 . 2.094(10) yes Pd C8A . 2.05(2) ? Pd C8B . 2.10(2) ? Pd C9 . 2.073(10) yes S1 C1 . 1.722(7) yes S2 C2 . 1.716(9) yes P C21 . 1.805(8) ? P C10 . 1.819(7) ? P C16 . 1.824(7) ? N1 C1 . 1.270(8) yes N1 C3 . 1.461(10) yes N2 C2 . 1.291(9) yes N2 C5 . 1.650(13) yes C1 C2 . 1.505(10) yes C3 C4 . 1.529(13) ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 H4A . 0.9600 ? C4 H4B . 0.9600 ? C4 H4C . 0.9600 ? C5 C6 . 1.443(17) ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? C6 H6A . 0.9600 ? C6 H6B . 0.9600 ? C6 H6C . 0.9600 ? C7 C8B . 1.26(3) ? C7 C8A . 1.42(4) ? C7 H7A . 0.9700 ? C7 H7B . 0.9700 ? C8A C9 . 1.24(3) ? C8A H8A . 0.9800 ? C8B C9 . 1.35(3) ? C8B H8B . 0.9800 ? C9 H9A . 0.9700 ? C9 H9B . 0.9700 ? C10 C15 . 1.340(10) ? C10 C11 . 1.410(10) ? C11 C12 . 1.369(11) ? C11 H11 . 0.9300 ? C12 C13 . 1.378(12) ? C12 H12 . 0.9300 ? C13 C14 . 1.358(12) ? C13 H13 . 0.9300 ? C14 C15 . 1.360(11) ? C14 H14 . 0.9300 ? C15 H15 . 0.9300 ? C16 N3 . 1.347(9) ? C16 C17 . 1.383(10) ? C17 C18 . 1.393(11) ? C17 H17 . 0.9300 ? C18 C19 . 1.343(12) ? C18 H18 . 0.9300 ? C19 C20 . 1.347(13) ? C19 H19 . 0.9300 ? C20 N3 . 1.380(11) ? C20 H20 . 0.9300 ? C21 C26 . 1.377(10) ? C21 C22 . 1.380(11) ? C22 C23 . 1.394(13) ? C22 H22 . 0.9300 ? C23 C24 . 1.376(14) ? C23 H23 . 0.9300 ? C24 C25 . 1.346(15) ? C24 H24 . 0.9300 ? C25 C26 . 1.365(12) ? C25 H25 . 0.9300 ? C26 H26 . 0.9300 ? C27 Cl4 . 1.731(17) ? C27 Cl2 . 1.803(17) ? C27 Cl3 . 2.015(17) ? C27 H27 . 0.9800 ? 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' S S 0.1246 0.1234 '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' Pd Pd -0.9988 1.0072 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag P Pt S1 92.65(7) yes P Pt S2 175.90(8) ? S1 Pt S2 89.23(7) yes P Pt Cl1 90.35(7) yes S1 Pt Cl1 177.00(8) ? S2 Pt Cl1 87.78(7) yes C8A Pd N1 142.5(10) ? C8A Pd C9 34.9(10) ? N1 Pd C9 174.8(4) ? C8A Pd N2 136.0(11) ? N1 Pd N2 77.8(3) yes C9 Pd N2 106.3(4) yes C8A Pd C7 40.1(10) ? N1 Pd C7 106.8(4) yes C9 Pd C7 68.9(4) ? N2 Pd C7 175.2(4) ? C8A Pd C8B 28.6(9) ? N1 Pd C8B 137.2(9) ? C9 Pd C8B 37.8(9) ? N2 Pd C8B 140.2(9) ? C7 Pd C8B 35.0(9) ? C1 S1 Pt 105.3(3) ? C2 S2 Pt 103.2(3) ? C21 P C10 104.8(4) ? C21 P C16 107.5(4) ? C10 P C16 103.4(3) ? C21 P Pt 112.6(3) ? C10 P Pt 114.4(2) ? C16 P Pt 113.3(2) ? C1 N1 C3 120.6(6) ? C1 N1 Pd 115.7(5) ? C3 N1 Pd 123.4(5) ? C2 N2 C5 122.5(8) ? C2 N2 Pd 115.4(6) ? C5 N2 Pd 120.6(6) ? N1 C1 C2 116.1(7) yes N1 C1 S1 124.6(6) yes C2 C1 S1 119.3(6) yes N2 C2 C1 114.8(7) yes N2 C2 S2 125.0(7) yes C1 C2 S2 120.2(6) yes N1 C3 C4 110.5(8) ? N1 C3 H3A 109.5 ? C4 C3 H3A 109.5 ? N1 C3 H3B 109.5 ? C4 C3 H3B 109.5 ? H3A C3 H3B 108.1 ? C3 C4 H4A 109.5 ? C3 C4 H4B 109.5 ? H4A C4 H4B 109.5 ? C3 C4 H4C 109.5 ? H4A C4 H4C 109.5 ? H4B C4 H4C 109.5 ? C6 C5 N2 95.2(11) ? C6 C5 H5A 112.7 ? N2 C5 H5A 112.7 ? C6 C5 H5B 112.7 ? N2 C5 H5B 112.7 ? H5A C5 H5B 110.2 ? 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 ? C8B C7 Pd 72.8(13) ? C8A C7 Pd 68.4(11) ? C8B C7 H7A 75.3 ? C8A C7 H7A 116.8 ? Pd C7 H7A 116.8 ? C8B C7 H7B 156.9 ? C8A C7 H7B 116.8 ? Pd C7 H7B 116.8 ? H7A C7 H7B 113.8 ? C9 C8A C7 125(3) ? C9 C8A Pd 73.4(12) ? C7 C8A Pd 71.5(12) ? C9 C8A H8A 116.8 ? C7 C8A H8A 116.8 ? Pd C8A H8A 116.8 ? C7 C8B C9 129(3) ? C7 C8B Pd 72.2(12) ? C9 C8B Pd 70.0(11) ? C7 C8B H8B 112.9 ? C9 C8B H8B 112.9 ? Pd C8B H8B 112.9 ? C8A C9 Pd 71.7(13) ? C8B C9 Pd 72.2(12) ? C8A C9 H9A 116.4 ? C8B C9 H9A 159.6 ? Pd C9 H9A 116.4 ? C8A C9 H9B 116.4 ? C8B C9 H9B 74.7 ? Pd C9 H9B 116.4 ? H9A C9 H9B 113.4 ? C15 C10 C11 118.5(7) ? C15 C10 P 120.9(6) ? C11 C10 P 120.1(6) ? C12 C11 C10 119.6(8) ? C12 C11 H11 120.2 ? C10 C11 H11 120.2 ? C11 C12 C13 120.5(9) ? C11 C12 H12 119.8 ? C13 C12 H12 119.8 ? C14 C13 C12 118.7(9) ? C14 C13 H13 120.7 ? C12 C13 H13 120.7 ? C13 C14 C15 121.2(9) ? C13 C14 H14 119.4 ? C15 C14 H14 119.4 ? C10 C15 C14 121.5(8) ? C10 C15 H15 119.2 ? C14 C15 H15 119.2 ? N3 C16 C17 121.2(8) ? N3 C16 P 119.1(6) ? C17 C16 P 119.5(6) ? C16 C17 C18 119.8(9) ? C16 C17 H17 120.1 ? C18 C17 H17 120.1 ? C19 C18 C17 118.6(10) ? C19 C18 H18 120.7 ? C17 C18 H18 120.7 ? C18 C19 C20 120.4(10) ? C18 C19 H19 119.8 ? C20 C19 H19 119.8 ? C19 C20 N3 122.9(10) ? C19 C20 H20 118.5 ? N3 C20 H20 118.5 ? C16 N3 C20 117.0(8) ? C26 C21 C22 118.6(8) ? C26 C21 P 121.0(7) ? C22 C21 P 120.4(7) ? C21 C22 C23 119.9(10) ? C21 C22 H22 120.0 ? C23 C22 H22 120.0 ? C24 C23 C22 119.2(11) ? C24 C23 H23 120.4 ? C22 C23 H23 120.4 ? C25 C24 C23 120.9(11) ? C25 C24 H24 119.6 ? C23 C24 H24 119.6 ? C24 C25 C26 119.9(11) ? C24 C25 H25 120.0 ? C26 C25 H25 120.0 ? C25 C26 C21 121.4(9) ? C25 C26 H26 119.3 ? C21 C26 H26 119.3 ? Cl4 C27 Cl2 103.8(10) ? Cl4 C27 Cl3 94.9(9) ? Cl2 C27 Cl3 91.4(9) ? Cl4 C27 H27 120.2 ? Cl2 C27 H27 120.2 ? Cl3 C27 H27 120.2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C4 H4B Cl2 . 0.96 2.93 3.515(12) 120 C18 H18 Cl1 3_666 0.93 2.90 3.800(11) 163 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag P Pt S1 C1 -163.8(3) ? S2 Pt S1 C1 12.6(3) ? S1 Pt S2 C2 -14.8(3) ? Cl1 Pt S2 C2 165.5(3) ? S1 Pt P C21 107.9(3) ? Cl1 Pt P C21 -72.3(3) ? S1 Pt P C10 -11.6(3) ? Cl1 Pt P C10 168.3(3) ? S1 Pt P C16 -129.8(3) ? Cl1 Pt P C16 50.0(3) ? C8A Pd N1 C1 -161.3(18) ? N2 Pd N1 C1 -3.1(6) ? C7 Pd N1 C1 175.5(7) ? C8B Pd N1 C1 154.4(15) ? C8A Pd N1 C3 25(2) ? N2 Pd N1 C3 -176.3(7) ? C7 Pd N1 C3 2.3(8) ? C8B Pd N1 C3 -18.8(17) ? C8A Pd N2 C2 161.5(16) ? N1 Pd N2 C2 0.5(7) ? C9 Pd N2 C2 -176.3(9) ? C8B Pd N2 C2 -155.5(15) ? C8A Pd N2 C5 -32.1(18) ? N1 Pd N2 C5 166.9(8) ? C9 Pd N2 C5 -10.0(10) ? C8B Pd N2 C5 10.8(17) ? C3 N1 C1 C2 178.4(8) ? Pd N1 C1 C2 5.0(9) ? C3 N1 C1 S1 .0(10) yes Pd N1 C1 S1 -173.2(4) ? Pt S1 C1 N1 170.7(6) ? Pt S1 C1 C2 -7.4(7) ? C5 N2 C2 C1 -164.3(8) ? Pd N2 C2 C1 1.7(11) ? C5 N2 C2 S2 15.0(10) yes Pd N2 C2 S2 -178.9(5) ? N1 C1 C2 N2 -4.5(12) ? S1 C1 C2 N2 173.8(7) yes N1 C1 C2 S2 176.0(6) yes S1 C1 C2 S2 -5.7(9) ? Pt S2 C2 N2 -164.4(8) ? Pt S2 C2 C1 15.0(7) ? C1 N1 C3 C4 -93.2(10) ? Pd N1 C3 C4 79.6(9) ? C2 N2 C5 C6 -98.9(12) ? Pd N2 C5 C6 95.8(10) ? C8A Pd C7 C8B 47.1(16) ? N1 Pd C7 C8B -154.7(18) ? C9 Pd C7 C8B 22(2) ? N1 Pd C7 C8A 158.2(18) ? C9 Pd C7 C8A -25(2) ? C8B Pd C7 C8A -47.1(16) ? C8B C7 C8A C9 -34(3) ? Pd C7 C8A C9 53(3) ? C8B C7 C8A Pd -87(2) ? N1 Pd C8A C9 -172.4(10) ? N2 Pd C8A C9 39(3) ? C7 Pd C8A C9 -137(3) ? C8B Pd C8A C9 -75(3) ? N1 Pd C8A C7 -36(3) ? C9 Pd C8A C7 137(3) ? N2 Pd C8A C7 175.8(7) ? C8B Pd C8A C7 62(3) ? C8A C7 C8B C9 33(2) ? Pd C7 C8B C9 -44(3) ? C8A C7 C8B Pd 76(2) ? C8A Pd C8B C7 -80(4) ? N1 Pd C8B C7 37(3) ? C9 Pd C8B C7 -145(3) ? N2 Pd C8B C7 -178.7(8) ? C8A Pd C8B C9 65(3) ? N1 Pd C8B C9 -178.1(10) ? N2 Pd C8B C9 -34(3) ? C7 Pd C8B C9 145(3) ? C7 C8A C9 C8B 30(2) ? Pd C8A C9 C8B 83(2) ? C7 C8A C9 Pd -52(3) ? C7 C8B C9 C8A -37(3) ? Pd C8B C9 C8A -81(2) ? C7 C8B C9 Pd 45(3) ? N2 Pd C9 C8A -153(2) ? C7 Pd C9 C8A 28(2) ? C8B Pd C9 C8A 49.0(16) ? C8A Pd C9 C8B -49.0(16) ? N2 Pd C9 C8B 158.2(19) ? C7 Pd C9 C8B -21(2) ? C21 P C10 C15 146.9(6) ? C16 P C10 C15 34.5(7) ? Pt P C10 C15 -89.3(7) ? C21 P C10 C11 -41.3(7) ? C16 P C10 C11 -153.8(6) ? Pt P C10 C11 82.5(6) ? C15 C10 C11 C12 0.4(12) ? P C10 C11 C12 -171.6(7) ? C10 C11 C12 C13 -0.2(14) ? C11 C12 C13 C14 -0.9(15) ? C12 C13 C14 C15 1.8(15) ? C11 C10 C15 C14 0.5(12) ? P C10 C15 C14 172.5(7) ? C13 C14 C15 C10 -1.7(14) ? C21 P C16 N3 -29.2(7) ? C10 P C16 N3 81.2(7) ? Pt P C16 N3 -154.3(6) ? C21 P C16 C17 154.8(6) ? C10 P C16 C17 -94.7(7) ? Pt P C16 C17 29.7(7) ? N3 C16 C17 C18 -0.1(12) ? P C16 C17 C18 175.7(6) ? C16 C17 C18 C19 0.1(14) ? C17 C18 C19 C20 -0.2(15) ? C18 C19 C20 N3 0.4(17) ? C17 C16 N3 C20 0.3(13) ? P C16 N3 C20 -175.5(7) ? C19 C20 N3 C16 -0.4(16) ? C10 P C21 C26 135.9(7) ? C16 P C21 C26 -114.5(7) ? Pt P C21 C26 11.0(8) ? C10 P C21 C22 -45.2(8) ? C16 P C21 C22 64.4(7) ? Pt P C21 C22 -170.1(6) ? C26 C21 C22 C23 0.8(13) ? P C21 C22 C23 -178.2(7) ? C21 C22 C23 C24 1.0(15) ? C22 C23 C24 C25 -2.8(17) ? C23 C24 C25 C26 2.7(17) ? C24 C25 C26 C21 -0.9(16) ? C22 C21 C26 C25 -0.9(14) ? P C21 C26 C25 178.1(8) ?