# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _publ_contact_author 'Dr José M. Vila' _publ_contact_author_email QIDEPORT@USC.ES _publ_contact_author_address ; Química Inorgánica University of Santiago Av. de las Ciencias s/n. Facultad d Santiago de Compostela la Coruña 15782 SPAIN ; _publ_section_title ; Cyclopalladated Compounds Derived From a [C,N,S] Terdentate Ligand: Synthesis, Characterization and Reactivity. Crystal and Molecular Structures of [Pd{2-ClC6H3C(H)==NCH2CH2SMe}(Cl)] and [{Pd[2-ClC6H3C(H)==NCH2CH2SMe]}2{m-Ph2P(CH2)4PPh2}][CF3SO3]2 ; _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Castro-Juiz, Samuel' 'Fernandez, Alberto' 'Fernandez, Jesus J.' 'Lopez-Torres, Margarita' 'Ortigueira, Juan M.' 'Suarez, Antonio' 'Vazquez-Garcia, Digna' 'Vila, José M.' data_3 _database_code_CSD 157897 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H11 Cl2 N Pd S' _chemical_formula_weight 354.56 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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.24110(10) _cell_length_b 15.2287(2) _cell_length_c 19.36720(10) _cell_angle_alpha 90.000 _cell_angle_beta 90.2070(10) _cell_angle_gamma 90.000 _cell_volume 2430.59(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 180 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 28.27 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 2.103 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.4867 _exptl_absorpt_correction_T_max 0.6784 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 16370 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.27 _reflns_number_total 5963 _reflns_number_gt 4356 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.3126P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5963 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.70793(3) 0.113288(18) 0.803703(15) 0.03838(9) Uani 1 1 d . . . Pd2 Pd 1.16214(4) 0.075190(18) 0.798874(14) 0.03773(9) Uani 1 1 d . . . Cl1 Cl 0.78294(12) 0.25730(6) 0.82477(6) 0.0571(3) Uani 1 1 d . . . Cl2 Cl 0.39100(17) -0.03830(9) 0.58211(6) 0.0724(3) Uani 1 1 d . . . Cl3 Cl 1.17687(17) -0.06709(7) 0.84038(6) 0.0666(3) Uani 1 1 d . . . Cl4 Cl 0.97381(17) 0.20425(9) 0.54489(6) 0.0794(4) Uani 1 1 d . . . S1 S 0.80565(14) 0.04999(8) 0.91024(6) 0.0579(3) Uani 1 1 d . . . S2 S 1.29046(13) 0.14672(7) 0.89649(5) 0.0498(3) Uani 1 1 d . . . N1 N 0.6328(4) -0.00805(19) 0.78305(16) 0.0438(8) Uani 1 1 d . . . N2 N 1.1633(4) 0.19426(19) 0.75718(16) 0.0381(7) Uani 1 1 d . . . C1 C 0.6008(5) 0.1350(2) 0.71250(19) 0.0400(9) Uani 1 1 d . . . C2 C 0.5736(5) 0.2134(3) 0.6773(2) 0.0535(11) Uani 1 1 d . . . H2 H 0.6106 0.2660 0.6960 0.064 Uiso 1 1 calc R . . C3 C 0.4922(6) 0.2138(3) 0.6148(2) 0.0619(13) Uani 1 1 d . . . H3 H 0.4731 0.2669 0.5925 0.074 Uiso 1 1 calc R . . C4 C 0.4381(6) 0.1361(3) 0.5848(2) 0.0588(12) Uani 1 1 d . . . H4 H 0.3858 0.1366 0.5422 0.071 Uiso 1 1 calc R . . C5 C 0.4635(5) 0.0590(3) 0.6191(2) 0.0487(10) Uani 1 1 d . . . C6 C 0.5399(5) 0.0565(2) 0.6826(2) 0.0409(9) Uani 1 1 d . . . C7 C 0.5623(5) -0.0207(3) 0.7251(2) 0.0486(10) Uani 1 1 d . . . H7 H 0.5276 -0.0760 0.7111 0.058 Uiso 1 1 calc R . . C8 C 0.6647(8) -0.0776(3) 0.8333(3) 0.0757(15) Uani 1 1 d . . . H8A H 0.5698 -0.1151 0.8360 0.091 Uiso 1 1 calc R . . H8B H 0.7541 -0.1132 0.8168 0.091 Uiso 1 1 calc R . . C9 C 0.7000(14) -0.0494(5) 0.8955(4) 0.235(7) Uani 1 1 d . . . H9A H 0.7624 -0.0955 0.9178 0.282 Uiso 1 1 calc R . . H9B H 0.5983 -0.0451 0.9203 0.282 Uiso 1 1 calc R . . C10 C 0.6941(7) 0.0998(5) 0.9796(3) 0.125(3) Uani 1 1 d . . . H10A H 0.5805 0.0997 0.9685 0.187 Uiso 1 1 calc R . . H10B H 0.7304 0.1592 0.9860 0.187 Uiso 1 1 calc R . . H10C H 0.7119 0.0671 1.0213 0.187 Uiso 1 1 calc R . . C11 C 1.0564(4) 0.0458(2) 0.70841(18) 0.0372(8) Uani 1 1 d . . . C12 C 0.9881(5) -0.0319(3) 0.6856(2) 0.0449(9) Uani 1 1 d . . . H12 H 0.9912 -0.0813 0.7137 0.054 Uiso 1 1 calc R . . C13 C 0.9151(5) -0.0368(3) 0.6213(2) 0.0549(11) Uani 1 1 d . . . H13 H 0.8688 -0.0894 0.6068 0.066 Uiso 1 1 calc R . . C14 C 0.9102(5) 0.0362(3) 0.5780(2) 0.0552(11) Uani 1 1 d . . . H14 H 0.8611 0.0326 0.5348 0.066 Uiso 1 1 calc R . . C15 C 0.9784(5) 0.1133(3) 0.5998(2) 0.0489(10) Uani 1 1 d . . . C16 C 1.0509(4) 0.1204(2) 0.66433(19) 0.0394(8) Uani 1 1 d . . . C17 C 1.1143(4) 0.2005(2) 0.6946(2) 0.0418(9) Uani 1 1 d . . . H17 H 1.1190 0.2530 0.6702 0.050 Uiso 1 1 calc R . . C18 C 1.2133(5) 0.2711(2) 0.79749(19) 0.0451(9) Uani 1 1 d . . . H18A H 1.1203 0.2951 0.8216 0.054 Uiso 1 1 calc R . . H18B H 1.2549 0.3161 0.7668 0.054 Uiso 1 1 calc R . . C19 C 1.3432(5) 0.2456(3) 0.8492(2) 0.0492(10) Uani 1 1 d . . . H19A H 1.3591 0.2935 0.8816 0.059 Uiso 1 1 calc R . . H19B H 1.4447 0.2362 0.8251 0.059 Uiso 1 1 calc R . . C20 C 1.1275(5) 0.1872(3) 0.9495(2) 0.0589(11) Uani 1 1 d . . . H20A H 1.1684 0.2316 0.9802 0.088 Uiso 1 1 calc R . . H20B H 1.0832 0.1397 0.9760 0.088 Uiso 1 1 calc R . . H20C H 1.0443 0.2118 0.9206 0.088 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 Pd1 0.03941(17) 0.03095(15) 0.04483(19) -0.00347(12) 0.00634(12) -0.00144(12) Pd2 0.04860(18) 0.03195(16) 0.03264(16) 0.00057(11) 0.00006(12) 0.00671(12) Cl1 0.0465(6) 0.0354(5) 0.0893(8) -0.0098(5) -0.0038(5) -0.0046(4) Cl2 0.0912(9) 0.0699(8) 0.0559(7) -0.0096(6) -0.0151(6) -0.0130(7) Cl3 0.1166(10) 0.0355(5) 0.0476(7) 0.0054(4) -0.0057(6) 0.0124(6) Cl4 0.0987(10) 0.0850(9) 0.0543(8) 0.0272(6) -0.0200(7) 0.0013(8) S1 0.0544(7) 0.0554(7) 0.0638(8) -0.0011(5) -0.0162(5) -0.0021(5) S2 0.0509(6) 0.0508(6) 0.0477(6) -0.0008(5) -0.0131(5) 0.0082(5) N1 0.060(2) 0.0286(16) 0.043(2) -0.0017(13) 0.0007(16) 0.0004(15) N2 0.0394(17) 0.0345(16) 0.0402(19) 0.0017(13) -0.0015(13) 0.0009(13) C1 0.044(2) 0.035(2) 0.040(2) 0.0009(16) 0.0122(16) -0.0019(16) C2 0.068(3) 0.036(2) 0.056(3) 0.0081(19) 0.016(2) 0.001(2) C3 0.079(3) 0.053(3) 0.054(3) 0.023(2) 0.014(2) 0.008(2) C4 0.064(3) 0.071(3) 0.042(3) 0.007(2) 0.004(2) 0.008(2) C5 0.048(2) 0.054(3) 0.044(2) 0.0003(19) 0.0074(19) -0.0030(19) C6 0.043(2) 0.037(2) 0.043(2) -0.0023(16) 0.0085(17) 0.0023(16) C7 0.057(3) 0.032(2) 0.056(3) -0.0042(18) 0.003(2) -0.0060(18) C8 0.128(5) 0.034(2) 0.065(3) 0.010(2) -0.014(3) 0.000(3) C9 0.453(17) 0.103(6) 0.147(7) 0.086(5) -0.206(9) -0.158(8) C10 0.069(4) 0.249(10) 0.055(4) 0.019(4) 0.002(3) 0.042(5) C11 0.038(2) 0.037(2) 0.037(2) -0.0019(15) 0.0070(16) 0.0041(15) C12 0.047(2) 0.042(2) 0.046(2) -0.0029(17) 0.0046(18) 0.0006(18) C13 0.057(3) 0.055(3) 0.053(3) -0.015(2) -0.001(2) -0.005(2) C14 0.049(3) 0.074(3) 0.043(3) -0.002(2) -0.0070(19) 0.005(2) C15 0.048(2) 0.057(3) 0.042(2) 0.0041(19) -0.0020(18) 0.006(2) C16 0.036(2) 0.047(2) 0.036(2) 0.0012(17) 0.0036(15) 0.0048(17) C17 0.041(2) 0.039(2) 0.046(2) 0.0124(17) 0.0022(17) 0.0017(17) C18 0.052(2) 0.032(2) 0.051(3) 0.0022(16) 0.0026(19) -0.0032(17) C19 0.041(2) 0.051(2) 0.056(3) -0.0085(19) 0.0010(19) -0.0016(18) C20 0.060(3) 0.073(3) 0.044(3) -0.009(2) 0.000(2) -0.010(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 Pd1 N1 1.989(3) . ? Pd1 C1 1.999(4) . ? Pd1 Cl1 2.3144(10) . ? Pd1 S1 2.4132(12) . ? Pd2 N2 1.985(3) . ? Pd2 C11 2.005(4) . ? Pd2 Cl3 2.3141(10) . ? Pd2 S2 2.4216(11) . ? Cl2 C5 1.750(4) . ? Cl4 C15 1.747(4) . ? S1 C9 1.769(6) . ? S1 C10 1.798(6) . ? S2 C20 1.802(4) . ? S2 C19 1.816(4) . ? N1 C7 1.276(5) . ? N1 C8 1.462(5) . ? N2 C17 1.279(4) . ? N2 C18 1.466(5) . ? C1 C2 1.394(5) . ? C1 C6 1.420(5) . ? C2 C3 1.381(6) . ? C3 C4 1.391(7) . ? C4 C5 1.364(6) . ? C5 C6 1.380(6) . ? C6 C7 1.447(5) . ? C8 C9 1.310(8) . ? C11 C12 1.381(5) . ? C11 C16 1.423(5) . ? C12 C13 1.383(5) . ? C13 C14 1.393(6) . ? C14 C15 1.368(6) . ? C15 C16 1.387(5) . ? C16 C17 1.450(5) . ? C18 C19 1.514(5) . ? 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 Pd1 C1 80.78(14) . . ? N1 Pd1 Cl1 176.92(10) . . ? C1 Pd1 Cl1 96.66(11) . . ? N1 Pd1 S1 84.46(10) . . ? C1 Pd1 S1 165.10(11) . . ? Cl1 Pd1 S1 98.03(4) . . ? N2 Pd2 C11 81.45(14) . . ? N2 Pd2 Cl3 175.09(9) . . ? C11 Pd2 Cl3 96.69(11) . . ? N2 Pd2 S2 84.49(9) . . ? C11 Pd2 S2 165.94(11) . . ? Cl3 Pd2 S2 97.34(4) . . ? C9 S1 C10 103.2(5) . . ? C9 S1 Pd1 92.4(2) . . ? C10 S1 Pd1 107.5(2) . . ? C20 S2 C19 100.6(2) . . ? C20 S2 Pd2 105.95(14) . . ? C19 S2 Pd2 94.82(14) . . ? C7 N1 C8 123.8(4) . . ? C7 N1 Pd1 117.2(3) . . ? C8 N1 Pd1 118.9(3) . . ? C17 N2 C18 122.2(3) . . ? C17 N2 Pd2 116.8(3) . . ? C18 N2 Pd2 121.0(2) . . ? C2 C1 C6 117.7(4) . . ? C2 C1 Pd1 130.1(3) . . ? C6 C1 Pd1 112.1(3) . . ? C3 C2 C1 120.6(4) . . ? C2 C3 C4 121.1(4) . . ? C5 C4 C3 118.7(4) . . ? C4 C5 C6 121.8(4) . . ? C4 C5 Cl2 118.5(4) . . ? C6 C5 Cl2 119.7(3) . . ? C5 C6 C1 120.0(4) . . ? C5 C6 C7 126.0(4) . . ? C1 C6 C7 114.0(4) . . ? N1 C7 C6 115.8(4) . . ? C9 C8 N1 114.5(5) . . ? C8 C9 S1 122.4(5) . . ? C12 C11 C16 118.7(4) . . ? C12 C11 Pd2 130.3(3) . . ? C16 C11 Pd2 111.0(3) . . ? C11 C12 C13 120.7(4) . . ? C12 C13 C14 120.7(4) . . ? C15 C14 C13 119.2(4) . . ? C14 C15 C16 121.4(4) . . ? C14 C15 Cl4 119.0(3) . . ? C16 C15 Cl4 119.7(3) . . ? C15 C16 C11 119.4(4) . . ? C15 C16 C17 125.7(4) . . ? C11 C16 C17 114.7(3) . . ? N2 C17 C16 115.7(3) . . ? N2 C18 C19 110.1(3) . . ? C18 C19 S2 112.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 S1 C9 -11.0(4) . . . . ? C1 Pd1 S1 C9 -3.1(6) . . . . ? Cl1 Pd1 S1 C9 167.1(4) . . . . ? N1 Pd1 S1 C10 -115.7(3) . . . . ? C1 Pd1 S1 C10 -107.8(5) . . . . ? Cl1 Pd1 S1 C10 62.5(3) . . . . ? N2 Pd2 S2 C20 87.02(18) . . . . ? C11 Pd2 S2 C20 86.5(4) . . . . ? Cl3 Pd2 S2 C20 -97.57(17) . . . . ? N2 Pd2 S2 C19 -15.44(15) . . . . ? C11 Pd2 S2 C19 -16.0(4) . . . . ? Cl3 Pd2 S2 C19 159.98(13) . . . . ? C1 Pd1 N1 C7 2.9(3) . . . . ? Cl1 Pd1 N1 C7 36.9(19) . . . . ? S1 Pd1 N1 C7 -179.1(3) . . . . ? C1 Pd1 N1 C8 -178.7(4) . . . . ? Cl1 Pd1 N1 C8 -144.8(16) . . . . ? S1 Pd1 N1 C8 -0.8(3) . . . . ? C11 Pd2 N2 C17 -5.3(3) . . . . ? Cl3 Pd2 N2 C17 62.7(12) . . . . ? S2 Pd2 N2 C17 174.9(3) . . . . ? C11 Pd2 N2 C18 172.9(3) . . . . ? Cl3 Pd2 N2 C18 -119.2(11) . . . . ? S2 Pd2 N2 C18 -7.0(3) . . . . ? N1 Pd1 C1 C2 174.6(4) . . . . ? Cl1 Pd1 C1 C2 -3.7(4) . . . . ? S1 Pd1 C1 C2 166.6(3) . . . . ? N1 Pd1 C1 C6 -2.7(3) . . . . ? Cl1 Pd1 C1 C6 179.0(2) . . . . ? S1 Pd1 C1 C6 -10.7(6) . . . . ? C6 C1 C2 C3 -1.0(6) . . . . ? Pd1 C1 C2 C3 -178.2(3) . . . . ? C1 C2 C3 C4 -1.3(7) . . . . ? C2 C3 C4 C5 1.6(7) . . . . ? C3 C4 C5 C6 0.5(6) . . . . ? C3 C4 C5 Cl2 178.5(3) . . . . ? C4 C5 C6 C1 -2.8(6) . . . . ? Cl2 C5 C6 C1 179.2(3) . . . . ? C4 C5 C6 C7 175.4(4) . . . . ? Cl2 C5 C6 C7 -2.6(6) . . . . ? C2 C1 C6 C5 3.0(5) . . . . ? Pd1 C1 C6 C5 -179.3(3) . . . . ? C2 C1 C6 C7 -175.4(3) . . . . ? Pd1 C1 C6 C7 2.3(4) . . . . ? C8 N1 C7 C6 179.3(4) . . . . ? Pd1 N1 C7 C6 -2.4(5) . . . . ? C5 C6 C7 N1 -178.2(4) . . . . ? C1 C6 C7 N1 0.0(5) . . . . ? C7 N1 C8 C9 -163.7(7) . . . . ? Pd1 N1 C8 C9 18.0(9) . . . . ? N1 C8 C9 S1 -32.6(12) . . . . ? C10 S1 C9 C8 135.8(9) . . . . ? Pd1 S1 C9 C8 27.3(10) . . . . ? N2 Pd2 C11 C12 -173.8(4) . . . . ? Cl3 Pd2 C11 C12 10.7(3) . . . . ? S2 Pd2 C11 C12 -173.3(3) . . . . ? N2 Pd2 C11 C16 4.0(2) . . . . ? Cl3 Pd2 C11 C16 -171.4(2) . . . . ? S2 Pd2 C11 C16 4.5(6) . . . . ? C16 C11 C12 C13 -0.3(5) . . . . ? Pd2 C11 C12 C13 177.4(3) . . . . ? C11 C12 C13 C14 0.5(6) . . . . ? C12 C13 C14 C15 -0.1(6) . . . . ? C13 C14 C15 C16 -0.7(6) . . . . ? C13 C14 C15 Cl4 179.3(3) . . . . ? C14 C15 C16 C11 0.9(6) . . . . ? Cl4 C15 C16 C11 -179.1(3) . . . . ? C14 C15 C16 C17 -174.5(4) . . . . ? Cl4 C15 C16 C17 5.5(5) . . . . ? C12 C11 C16 C15 -0.4(5) . . . . ? Pd2 C11 C16 C15 -178.5(3) . . . . ? C12 C11 C16 C17 175.5(3) . . . . ? Pd2 C11 C16 C17 -2.7(4) . . . . ? C18 N2 C17 C16 -173.0(3) . . . . ? Pd2 N2 C17 C16 5.2(4) . . . . ? C15 C16 C17 N2 174.1(4) . . . . ? C11 C16 C17 N2 -1.5(5) . . . . ? C17 N2 C18 C19 -149.2(3) . . . . ? Pd2 N2 C18 C19 32.8(4) . . . . ? N2 C18 C19 S2 -47.2(4) . . . . ? C20 S2 C19 C18 -70.3(3) . . . . ? Pd2 S2 C19 C18 36.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.946 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.116 #======END data_11 _database_code_CSD 157898 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H50 Cl2 F6 N2 O6 P2 Pd2 S4' _chemical_formula_weight 1362.80 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 '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' 'F' 'F' 0.0171 0.0103 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3501(15) _cell_length_b 11.1288(16) _cell_length_c 12.7800(19) _cell_angle_alpha 74.691(3) _cell_angle_beta 82.642(3) _cell_angle_gamma 82.434(3) _cell_volume 1400.7(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 190 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 28.30 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 686 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.6588 _exptl_absorpt_correction_T_max 0.7860 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1% _diffrn_reflns_number 9629 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0993 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.30 _reflns_number_total 6726 _reflns_number_gt 4357 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0808P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6726 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.30823(4) 0.32326(4) 0.78085(3) 0.02010(13) Uani 1 1 d . . . P1 P 0.48300(14) 0.19158(12) 0.73790(10) 0.0195(3) Uani 1 1 d . . . S1 S 0.13348(15) 0.21325(15) 0.75939(12) 0.0308(3) Uani 1 1 d . . . Cl1 Cl 0.26964(16) 0.73045(14) 0.95849(13) 0.0384(4) Uani 1 1 d . . . N1 N 0.1552(4) 0.4408(4) 0.8264(4) 0.0220(10) Uani 1 1 d . . . C1 C 0.4112(6) 0.4474(5) 0.8175(4) 0.0243(12) Uani 1 1 d . . . C2 C 0.5467(6) 0.4569(5) 0.8091(5) 0.0291(13) Uani 1 1 d . . . H2 H 0.6052 0.4008 0.7795 0.035 Uiso 1 1 calc R . . C3 C 0.5939(6) 0.5492(6) 0.8444(5) 0.0340(14) Uani 1 1 d . . . H3 H 0.6835 0.5551 0.8369 0.041 Uiso 1 1 calc R . . C4 C 0.5079(6) 0.6338(5) 0.8913(5) 0.0311(13) Uani 1 1 d . . . H4 H 0.5400 0.6949 0.9154 0.037 Uiso 1 1 calc R . . C5 C 0.3757(6) 0.6245(5) 0.9010(5) 0.0287(13) Uani 1 1 d . . . C6 C 0.3251(5) 0.5337(5) 0.8649(4) 0.0234(12) Uani 1 1 d . . . C7 C 0.1857(6) 0.5248(5) 0.8683(4) 0.0258(12) Uani 1 1 d . . . H7 H 0.1228 0.5766 0.8990 0.031 Uiso 1 1 calc R . . C8 C 0.0179(6) 0.4215(6) 0.8228(5) 0.0331(14) Uani 1 1 d . . . H8A H -0.0100 0.4620 0.7512 0.040 Uiso 1 1 calc R . . H8B H -0.0386 0.4569 0.8762 0.040 Uiso 1 1 calc R . . C9 C 0.0102(6) 0.2806(6) 0.8484(5) 0.0350(14) Uani 1 1 d . . . H9A H -0.0762 0.2644 0.8373 0.042 Uiso 1 1 calc R . . H9B H 0.0251 0.2424 0.9239 0.042 Uiso 1 1 calc R . . C10 C 0.1424(7) 0.0519(6) 0.8384(6) 0.0437(17) Uani 1 1 d . . . H10A H 0.2055 0.0018 0.8016 0.065 Uiso 1 1 calc R . . H10B H 0.0581 0.0217 0.8464 0.065 Uiso 1 1 calc R . . H10C H 0.1685 0.0466 0.9090 0.065 Uiso 1 1 calc R . . C11 C 0.5590(6) 0.1001(5) 0.8577(4) 0.0228(11) Uani 1 1 d . . . H11A H 0.6224 0.0360 0.8370 0.027 Uiso 1 1 calc R . . H11B H 0.6066 0.1544 0.8835 0.027 Uiso 1 1 calc R . . C12 C 0.4644(5) 0.0371(5) 0.9513(4) 0.0210(11) Uani 1 1 d . . . H12A H 0.4008 0.1004 0.9731 0.025 Uiso 1 1 calc R . . H12B H 0.4173 -0.0186 0.9268 0.025 Uiso 1 1 calc R . . C13 C 0.4311(5) 0.0826(5) 0.6715(4) 0.0237(12) Uani 1 1 d . . . C14 C 0.4639(6) -0.0450(5) 0.7029(5) 0.0291(13) Uani 1 1 d . . . H14 H 0.5189 -0.0787 0.7578 0.035 Uiso 1 1 calc R . . C15 C 0.4142(7) -0.1238(6) 0.6521(5) 0.0396(16) Uani 1 1 d . . . H15 H 0.4337 -0.2101 0.6755 0.048 Uiso 1 1 calc R . . C16 C 0.3381(7) -0.0755(8) 0.5690(5) 0.0471(19) Uani 1 1 d . . . H16 H 0.3073 -0.1287 0.5348 0.056 Uiso 1 1 calc R . . C17 C 0.3057(7) 0.0533(7) 0.5348(5) 0.0442(17) Uani 1 1 d . . . H17 H 0.2531 0.0863 0.4780 0.053 Uiso 1 1 calc R . . C18 C 0.3527(6) 0.1329(6) 0.5864(5) 0.0345(14) Uani 1 1 d . . . H18 H 0.3318 0.2190 0.5638 0.041 Uiso 1 1 calc R . . C19 C 0.6187(6) 0.2580(5) 0.6435(4) 0.0250(12) Uani 1 1 d . . . C20 C 0.7469(6) 0.2119(6) 0.6546(5) 0.0291(13) Uani 1 1 d . . . H20 H 0.7676 0.1457 0.7136 0.035 Uiso 1 1 calc R . . C21 C 0.8462(6) 0.2630(7) 0.5787(5) 0.0418(16) Uani 1 1 d . . . H21 H 0.9329 0.2321 0.5888 0.050 Uiso 1 1 calc R . . C22 C 0.8194(7) 0.3557(7) 0.4913(6) 0.0480(18) Uani 1 1 d . . . H22 H 0.8872 0.3911 0.4427 0.058 Uiso 1 1 calc R . . C23 C 0.6884(8) 0.4000(7) 0.4728(6) 0.065(3) Uani 1 1 d . . . H23 H 0.6688 0.4601 0.4094 0.078 Uiso 1 1 calc R . . C24 C 0.5882(7) 0.3524(7) 0.5508(6) 0.052(2) Uani 1 1 d . . . H24 H 0.5015 0.3835 0.5412 0.062 Uiso 1 1 calc R . . S1S S 0.14699(14) 0.19913(14) 0.14507(13) 0.0314(3) Uani 1 1 d . . . O1 O 0.2779(4) 0.1781(4) 0.1766(5) 0.0532(14) Uani 1 1 d . . . O2 O 0.1133(5) 0.1027(5) 0.1002(4) 0.0537(14) Uani 1 1 d . . . O3 O 0.1068(5) 0.3257(4) 0.0886(4) 0.0479(12) Uani 1 1 d . . . C1S C 0.0453(7) 0.1793(6) 0.2745(5) 0.0404(16) Uani 1 1 d . . . F1 F 0.0673(5) 0.0630(4) 0.3381(3) 0.0673(14) Uani 1 1 d . . . F2 F 0.0717(5) 0.2582(4) 0.3295(4) 0.0684(14) Uani 1 1 d . . . F3 F -0.0811(4) 0.1993(4) 0.2621(3) 0.0602(12) Uani 1 1 d . . . 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 Pd1 0.0178(2) 0.0190(2) 0.0226(2) -0.00660(15) 0.00246(15) -0.00037(15) P1 0.0212(7) 0.0169(7) 0.0179(6) -0.0037(5) 0.0019(5) 0.0014(6) S1 0.0240(8) 0.0368(9) 0.0369(8) -0.0189(7) 0.0000(6) -0.0061(6) Cl1 0.0374(9) 0.0274(8) 0.0549(10) -0.0221(7) -0.0007(7) 0.0009(7) N1 0.014(2) 0.024(2) 0.028(2) -0.0083(19) 0.0004(18) -0.0009(19) C1 0.025(3) 0.022(3) 0.023(3) -0.003(2) 0.002(2) -0.002(2) C2 0.023(3) 0.020(3) 0.042(3) -0.005(2) 0.003(3) -0.003(2) C3 0.026(3) 0.031(3) 0.045(4) -0.007(3) 0.003(3) -0.013(3) C4 0.032(3) 0.020(3) 0.042(3) -0.009(2) -0.003(3) -0.003(3) C5 0.028(3) 0.021(3) 0.034(3) -0.006(2) 0.001(3) -0.001(2) C6 0.023(3) 0.016(3) 0.029(3) -0.003(2) 0.001(2) -0.001(2) C7 0.023(3) 0.023(3) 0.029(3) -0.007(2) 0.002(2) 0.004(2) C8 0.019(3) 0.037(3) 0.047(4) -0.021(3) 0.001(3) 0.000(3) C9 0.021(3) 0.041(4) 0.048(4) -0.020(3) 0.004(3) -0.009(3) C10 0.038(4) 0.033(4) 0.066(5) -0.022(3) 0.008(3) -0.016(3) C11 0.031(3) 0.018(3) 0.021(3) -0.007(2) 0.000(2) -0.003(2) C12 0.023(3) 0.020(3) 0.020(2) -0.005(2) 0.000(2) -0.002(2) C13 0.018(3) 0.035(3) 0.017(2) -0.008(2) 0.002(2) 0.002(2) C14 0.030(3) 0.030(3) 0.029(3) -0.016(2) 0.003(2) 0.000(3) C15 0.044(4) 0.044(4) 0.037(3) -0.025(3) 0.007(3) -0.007(3) C16 0.045(4) 0.072(5) 0.038(4) -0.038(4) 0.011(3) -0.021(4) C17 0.036(4) 0.071(5) 0.032(3) -0.026(3) -0.004(3) 0.000(4) C18 0.035(4) 0.042(4) 0.029(3) -0.017(3) -0.001(3) 0.000(3) C19 0.026(3) 0.020(3) 0.026(3) -0.006(2) 0.008(2) -0.002(2) C20 0.023(3) 0.034(3) 0.026(3) -0.001(2) 0.000(2) -0.004(3) C21 0.023(3) 0.057(4) 0.041(4) -0.005(3) 0.004(3) -0.010(3) C22 0.045(4) 0.042(4) 0.048(4) -0.007(3) 0.023(3) -0.007(3) C23 0.066(6) 0.050(5) 0.049(4) 0.015(4) 0.030(4) 0.010(4) C24 0.041(4) 0.043(4) 0.051(4) 0.009(3) 0.013(3) 0.008(3) S1S 0.0189(7) 0.0300(8) 0.0488(9) -0.0181(7) 0.0019(6) -0.0036(6) O1 0.018(2) 0.041(3) 0.105(4) -0.026(3) -0.009(3) 0.003(2) O2 0.055(3) 0.062(3) 0.060(3) -0.038(3) 0.013(3) -0.031(3) O3 0.041(3) 0.040(3) 0.052(3) -0.005(2) 0.008(2) 0.010(2) C1S 0.043(4) 0.040(4) 0.040(4) -0.018(3) -0.003(3) 0.002(3) F1 0.087(4) 0.048(3) 0.052(3) 0.002(2) -0.002(2) 0.011(2) F2 0.089(4) 0.067(3) 0.058(3) -0.039(2) -0.011(3) 0.009(3) F3 0.028(2) 0.082(3) 0.059(3) -0.010(2) 0.012(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 Pd1 C1 2.030(6) . ? Pd1 N1 2.044(4) . ? Pd1 P1 2.2788(14) . ? Pd1 S1 2.3944(16) . ? P1 C11 1.810(5) . ? P1 C13 1.819(6) . ? P1 C19 1.828(5) . ? S1 C10 1.810(7) . ? S1 C9 1.819(6) . ? Cl1 C5 1.745(6) . ? N1 C7 1.283(7) . ? N1 C8 1.473(7) . ? C1 C2 1.408(8) . ? C1 C6 1.424(7) . ? C2 C3 1.389(8) . ? C3 C4 1.407(8) . ? C4 C5 1.373(8) . ? C5 C6 1.399(8) . ? C6 C7 1.453(8) . ? C8 C9 1.526(8) . ? C11 C12 1.523(7) . ? C12 C12 1.519(10) 2_657 ? C13 C14 1.378(8) . ? C13 C18 1.393(8) . ? C14 C15 1.400(8) . ? C15 C16 1.356(10) . ? C16 C17 1.392(10) . ? C17 C18 1.400(9) . ? C19 C20 1.368(8) . ? C19 C24 1.400(8) . ? C20 C21 1.389(8) . ? C21 C22 1.336(9) . ? C22 C23 1.408(11) . ? C23 C24 1.396(9) . ? S1S O1 1.435(5) . ? S1S O3 1.437(5) . ? S1S O2 1.442(5) . ? S1S C1S 1.820(7) . ? C1S F3 1.321(8) . ? C1S F2 1.333(7) . ? C1S F1 1.343(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N1 81.1(2) . . ? C1 Pd1 P1 97.17(16) . . ? N1 Pd1 P1 177.17(13) . . ? C1 Pd1 S1 162.90(16) . . ? N1 Pd1 S1 81.95(13) . . ? P1 Pd1 S1 99.73(5) . . ? C11 P1 C13 107.6(2) . . ? C11 P1 C19 104.5(3) . . ? C13 P1 C19 103.1(2) . . ? C11 P1 Pd1 111.86(17) . . ? C13 P1 Pd1 110.18(18) . . ? C19 P1 Pd1 118.78(18) . . ? C10 S1 C9 98.7(3) . . ? C10 S1 Pd1 113.6(2) . . ? C9 S1 Pd1 96.1(2) . . ? C7 N1 C8 121.9(5) . . ? C7 N1 Pd1 115.7(4) . . ? C8 N1 Pd1 122.1(3) . . ? C2 C1 C6 117.9(5) . . ? C2 C1 Pd1 131.7(4) . . ? C6 C1 Pd1 110.3(4) . . ? C3 C2 C1 120.7(5) . . ? C2 C3 C4 120.9(6) . . ? C5 C4 C3 118.8(5) . . ? C4 C5 C6 121.6(5) . . ? C4 C5 Cl1 118.6(5) . . ? C6 C5 Cl1 119.8(5) . . ? C5 C6 C1 120.0(5) . . ? C5 C6 C7 123.3(5) . . ? C1 C6 C7 116.6(5) . . ? N1 C7 C6 115.6(5) . . ? N1 C8 C9 107.4(5) . . ? C8 C9 S1 109.3(4) . . ? C12 C11 P1 114.8(4) . . ? C12 C12 C11 111.5(6) 2_657 . ? C14 C13 C18 119.7(5) . . ? C14 C13 P1 123.1(4) . . ? C18 C13 P1 117.2(4) . . ? C13 C14 C15 120.0(6) . . ? C16 C15 C14 120.6(6) . . ? C15 C16 C17 120.3(6) . . ? C16 C17 C18 119.6(6) . . ? C13 C18 C17 119.8(6) . . ? C20 C19 C24 119.0(5) . . ? C20 C19 P1 122.9(4) . . ? C24 C19 P1 117.9(5) . . ? C19 C20 C21 120.8(5) . . ? C22 C21 C20 121.1(6) . . ? C21 C22 C23 120.0(6) . . ? C24 C23 C22 119.2(7) . . ? C23 C24 C19 119.8(7) . . ? O1 S1S O3 115.0(3) . . ? O1 S1S O2 113.6(3) . . ? O3 S1S O2 115.9(3) . . ? O1 S1S C1S 103.5(3) . . ? O3 S1S C1S 102.9(3) . . ? O2 S1S C1S 103.6(3) . . ? F3 C1S F2 107.7(6) . . ? F3 C1S F1 107.2(6) . . ? F2 C1S F1 107.1(5) . . ? F3 C1S S1S 112.6(5) . . ? F2 C1S S1S 110.7(5) . . ? F1 C1S S1S 111.3(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pd1 P1 C11 72.6(2) . . . . ? N1 Pd1 P1 C11 21(3) . . . . ? S1 Pd1 P1 C11 -104.8(2) . . . . ? C1 Pd1 P1 C13 -167.8(2) . . . . ? N1 Pd1 P1 C13 141(3) . . . . ? S1 Pd1 P1 C13 14.81(19) . . . . ? C1 Pd1 P1 C19 -49.3(3) . . . . ? N1 Pd1 P1 C19 -100(3) . . . . ? S1 Pd1 P1 C19 133.3(2) . . . . ? C1 Pd1 S1 C10 -117.0(6) . . . . ? N1 Pd1 S1 C10 -123.4(3) . . . . ? P1 Pd1 S1 C10 54.3(2) . . . . ? C1 Pd1 S1 C9 -14.8(6) . . . . ? N1 Pd1 S1 C9 -21.2(3) . . . . ? P1 Pd1 S1 C9 156.5(2) . . . . ? C1 Pd1 N1 C7 -8.1(4) . . . . ? P1 Pd1 N1 C7 43(3) . . . . ? S1 Pd1 N1 C7 170.0(4) . . . . ? C1 Pd1 N1 C8 178.5(5) . . . . ? P1 Pd1 N1 C8 -130(3) . . . . ? S1 Pd1 N1 C8 -3.5(4) . . . . ? N1 Pd1 C1 C2 -176.7(5) . . . . ? P1 Pd1 C1 C2 5.6(5) . . . . ? S1 Pd1 C1 C2 176.9(3) . . . . ? N1 Pd1 C1 C6 6.9(4) . . . . ? P1 Pd1 C1 C6 -170.9(3) . . . . ? S1 Pd1 C1 C6 0.4(8) . . . . ? C6 C1 C2 C3 -1.0(8) . . . . ? Pd1 C1 C2 C3 -177.3(4) . . . . ? C1 C2 C3 C4 1.2(9) . . . . ? C2 C3 C4 C5 -0.6(9) . . . . ? C3 C4 C5 C6 -0.3(9) . . . . ? C3 C4 C5 Cl1 -179.6(4) . . . . ? C4 C5 C6 C1 0.5(8) . . . . ? Cl1 C5 C6 C1 179.8(4) . . . . ? C4 C5 C6 C7 -176.7(5) . . . . ? Cl1 C5 C6 C7 2.6(8) . . . . ? C2 C1 C6 C5 0.2(8) . . . . ? Pd1 C1 C6 C5 177.2(4) . . . . ? C2 C1 C6 C7 177.5(5) . . . . ? Pd1 C1 C6 C7 -5.4(6) . . . . ? C8 N1 C7 C6 -179.3(5) . . . . ? Pd1 N1 C7 C6 7.3(6) . . . . ? C5 C6 C7 N1 176.2(5) . . . . ? C1 C6 C7 N1 -1.1(7) . . . . ? C7 N1 C8 C9 -140.0(5) . . . . ? Pd1 N1 C8 C9 33.0(6) . . . . ? N1 C8 C9 S1 -51.9(6) . . . . ? C10 S1 C9 C8 160.0(5) . . . . ? Pd1 S1 C9 C8 45.0(4) . . . . ? C13 P1 C11 C12 -72.6(4) . . . . ? C19 P1 C11 C12 178.3(4) . . . . ? Pd1 P1 C11 C12 48.5(4) . . . . ? P1 C11 C12 C12 -179.7(4) . . . 2_657 ? C11 P1 C13 C14 -8.2(5) . . . . ? C19 P1 C13 C14 101.9(5) . . . . ? Pd1 P1 C13 C14 -130.3(4) . . . . ? C11 P1 C13 C18 170.7(4) . . . . ? C19 P1 C13 C18 -79.2(5) . . . . ? Pd1 P1 C13 C18 48.6(5) . . . . ? C18 C13 C14 C15 -2.5(8) . . . . ? P1 C13 C14 C15 176.4(5) . . . . ? C13 C14 C15 C16 2.6(9) . . . . ? C14 C15 C16 C17 -1.5(10) . . . . ? C15 C16 C17 C18 0.3(10) . . . . ? C14 C13 C18 C17 1.3(8) . . . . ? P1 C13 C18 C17 -177.6(5) . . . . ? C16 C17 C18 C13 -0.2(9) . . . . ? C11 P1 C19 C20 17.7(6) . . . . ? C13 P1 C19 C20 -94.6(5) . . . . ? Pd1 P1 C19 C20 143.2(4) . . . . ? C11 P1 C19 C24 -168.3(5) . . . . ? C13 P1 C19 C24 79.3(5) . . . . ? Pd1 P1 C19 C24 -42.8(6) . . . . ? C24 C19 C20 C21 3.9(9) . . . . ? P1 C19 C20 C21 177.8(5) . . . . ? C19 C20 C21 C22 -2.0(10) . . . . ? C20 C21 C22 C23 -2.4(12) . . . . ? C21 C22 C23 C24 4.8(13) . . . . ? C22 C23 C24 C19 -2.8(13) . . . . ? C20 C19 C24 C23 -1.5(11) . . . . ? P1 C19 C24 C23 -175.7(6) . . . . ? O1 S1S C1S F3 178.0(5) . . . . ? O3 S1S C1S F3 57.9(6) . . . . ? O2 S1S C1S F3 -63.2(6) . . . . ? O1 S1S C1S F2 57.4(5) . . . . ? O3 S1S C1S F2 -62.7(5) . . . . ? O2 S1S C1S F2 176.2(5) . . . . ? O1 S1S C1S F1 -61.6(5) . . . . ? O3 S1S C1S F1 178.3(5) . . . . ? O2 S1S C1S F1 57.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.832 _refine_diff_density_min -1.403 _refine_diff_density_rms 0.209