# 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 'Takaki Kanbara' _publ_contact_author_email KANBARA@IMS.TSUKUBA.AC.JP _publ_section_title ; Palladium(II) and platinum(II) complexes bearing kappa3SCS pincer ligand with azulene unit ; loop_ _publ_author_name 'Takaki Kanbara' 'Junpei Kuwabara' 'Goro Munezawa' 'Ken Okamoto' # Attachment '1CIF.cif' data_Azligand2 _database_code_depnum_ccdc_archive 'CCDC 750102' #TrackingRef '1CIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C23 H28 Cl2 N2 S2 ' _chemical_formula_moiety 'C23 H28 Cl2 N2 S2 ' _chemical_formula_weight 467.51 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2+Z 3 +X,1/2-Y,+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,1/2-Z 7 -X,1/2+Y,-Z 8 1/2+X,+Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 16.1348(6) _cell_length_b 16.0405(7) _cell_length_c 8.8982(3) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2302.95(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 12287 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 88.1 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984.00 _exptl_absorpt_coefficient_mu 0.476 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 20625 _diffrn_reflns_av_R_equivalents 0.092 _diffrn_reflns_theta_max 27.44 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_ambient_temperature 88.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2713 _reflns_number_gt 1856 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1578 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2713 _refine_ls_number_parameters 144 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0661P)^2^+2.0386P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.54 _refine_diff_density_min -0.67 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl(1) Cl 0.70727(8) 0.2500 1.06745(15) 0.0378(3) Uani 1.00 2 d S . . Cl(2) Cl 0.52962(8) 0.2500 1.00072(13) 0.0329(3) Uani 1.00 2 d S . . S(1) S 0.62849(5) 0.05635(5) 0.34597(8) 0.0214(2) Uani 1.00 1 d . . . N(1) N 0.64754(16) 0.04400(16) 0.6444(2) 0.0201(5) Uani 1.00 1 d . . . C(1) C 0.6481(3) 0.2500 0.5125(5) 0.0203(8) Uani 1.00 2 d S . . C(2) C 0.60261(18) 0.17854(19) 0.5518(3) 0.0183(6) Uani 1.00 1 d . . . C(3) C 0.52567(17) 0.20365(18) 0.6105(3) 0.0169(6) Uani 1.00 1 d . . . C(4) C 0.46209(18) 0.15114(19) 0.6564(3) 0.0194(6) Uani 1.00 1 d . . . C(5) C 0.38437(18) 0.1714(2) 0.7158(3) 0.0217(6) Uani 1.00 1 d . . . C(6) C 0.3506(3) 0.2500 0.7438(5) 0.0219(9) Uani 1.00 2 d S . . C(7) C 0.62810(17) 0.09074(19) 0.5243(3) 0.0184(6) Uani 1.00 1 d . . . C(8) C 0.6696(2) -0.04525(19) 0.6322(3) 0.0224(6) Uani 1.00 1 d . . . C(9) C 0.6156(2) -0.0972(2) 0.7362(3) 0.0256(7) Uani 1.00 1 d . . . C(10) C 0.6210(2) -0.0664(2) 0.8990(3) 0.0269(7) Uani 1.00 1 d . . . C(12) C 0.5998(2) 0.0262(2) 0.9058(3) 0.0256(7) Uani 1.00 1 d . . . C(13) C 0.65457(19) 0.0763(2) 0.7991(3) 0.0216(6) Uani 1.00 1 d . . . C(14) C 0.6055(3) 0.2500 1.1442(5) 0.0280(10) Uani 1.00 2 d S . . H(1) H 0.7013 0.2500 0.4667 0.024 Uiso 1.00 2 c R . . H(2) H 0.4729 0.0932 0.6459 0.023 Uiso 1.00 1 c R . . H(3) H 0.3499 0.1254 0.7406 0.026 Uiso 1.00 1 c R . . H(4) H 0.2970 0.2500 0.7881 0.026 Uiso 1.00 2 c R . . H(5) H 0.7286 -0.0530 0.6593 0.027 Uiso 1.00 1 c R . . H(6) H 0.6620 -0.0641 0.5272 0.027 Uiso 1.00 1 c R . . H(7) H 0.6334 -0.1562 0.7315 0.031 Uiso 1.00 1 c R . . H(8) H 0.5573 -0.0943 0.7018 0.031 Uiso 1.00 1 c R . . H(9) H 0.5819 -0.0983 0.9626 0.032 Uiso 1.00 1 c R . . H(10) H 0.6777 -0.0756 0.9381 0.032 Uiso 1.00 1 c R . . H(11) H 0.5409 0.0343 0.8782 0.031 Uiso 1.00 1 c R . . H(12) H 0.6076 0.0468 1.0097 0.031 Uiso 1.00 1 c R . . H(13) H 0.6377 0.1356 0.8012 0.026 Uiso 1.00 1 c R . . H(14) H 0.7130 0.0728 0.8326 0.026 Uiso 1.00 1 c R . . H(15) H 0.6001(19) 0.299(2) 1.200(3) 0.022(8) Uiso 1.00 1 c . . . 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 Cl(1) 0.0360(6) 0.0367(7) 0.0407(7) 0.0000 -0.0049(5) 0.0000 Cl(2) 0.0395(6) 0.0332(6) 0.0259(5) 0.0000 -0.0074(5) 0.0000 S(1) 0.0284(4) 0.0186(4) 0.0173(3) 0.0015(3) 0.0011(3) -0.0006(3) N(1) 0.0226(12) 0.0174(13) 0.0204(12) 0.0023(9) -0.0024(10) 0.0003(10) C(1) 0.023(2) 0.021(2) 0.0168(19) 0.0000 -0.0032(17) 0.0000 C(2) 0.0231(14) 0.0192(15) 0.0126(12) 0.0019(11) -0.0014(11) 0.0006(11) C(3) 0.0190(13) 0.0166(15) 0.0151(13) 0.0007(11) -0.0020(11) -0.0012(10) C(4) 0.0246(14) 0.0176(15) 0.0160(13) 0.0011(11) -0.0009(12) -0.0016(11) C(5) 0.0218(15) 0.0211(16) 0.0222(15) -0.0038(12) 0.0002(12) -0.0005(12) C(6) 0.019(2) 0.026(2) 0.021(2) 0.0000 0.0007(17) 0.0000 C(7) 0.0153(13) 0.0197(15) 0.0202(14) -0.0015(11) 0.0003(11) 0.0011(12) C(8) 0.0277(16) 0.0177(16) 0.0218(15) 0.0062(12) 0.0011(12) -0.0001(12) C(9) 0.0288(16) 0.0210(16) 0.0272(16) 0.0010(13) -0.0003(13) 0.0012(13) C(10) 0.0291(16) 0.0297(18) 0.0219(15) 0.0037(13) -0.0003(13) 0.0080(13) C(12) 0.0278(15) 0.0282(17) 0.0209(14) 0.0031(13) 0.0009(13) -0.0021(13) C(13) 0.0254(15) 0.0240(17) 0.0153(13) 0.0027(12) -0.0012(12) -0.0009(12) C(14) 0.040(2) 0.022(2) 0.022(2) 0.0000 -0.002(2) 0.0000 #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cl(1) C(14) 1.778(4) yes . . Cl(2) C(14) 1.769(4) yes . . S(1) C(7) 1.680(2) yes . . N(1) C(7) 1.343(3) yes . . N(1) C(8) 1.479(3) yes . . N(1) C(13) 1.475(3) yes . . C(1) C(2) 1.405(4) yes . . C(1) C(2) 1.405(4) yes . 3_555 C(2) C(3) 1.406(3) yes . . C(2) C(7) 1.487(4) yes . . C(3) C(3) 1.487(4) yes . 3_555 C(3) C(4) 1.389(4) yes . . C(4) C(5) 1.399(4) yes . . C(5) C(6) 1.396(3) yes . . C(8) C(9) 1.520(4) yes . . C(9) C(10) 1.533(4) yes . . C(10) C(12) 1.526(4) yes . . C(12) C(13) 1.525(4) yes . . C(1) H(1) 0.950 no . . C(4) H(2) 0.950 no . . C(5) H(3) 0.950 no . . C(6) H(4) 0.950 no . . C(8) H(5) 0.990 no . . C(8) H(6) 0.990 no . . C(9) H(7) 0.990 no . . C(9) H(8) 0.990 no . . C(10) H(9) 0.990 no . . C(10) H(10) 0.990 no . . C(12) H(11) 0.990 no . . C(12) H(12) 0.990 no . . C(13) H(13) 0.990 no . . C(13) H(14) 0.990 no . . C(14) H(15) 0.93(3) no . . C(14) H(15) 0.93(3) no . 3_555 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(7) N(1) C(8) 122.6(2) yes . . . C(7) N(1) C(13) 124.4(2) yes . . . C(8) N(1) C(13) 112.9(2) yes . . . C(2) C(1) C(2) 109.3(3) yes . . 3_555 C(1) C(2) C(3) 108.7(2) yes . . . C(1) C(2) C(7) 125.9(2) yes . . . C(3) C(2) C(7) 125.2(2) yes . . . C(2) C(3) C(3) 106.6(2) yes . . 3_555 C(2) C(3) C(4) 126.0(2) yes . . . C(3) C(3) C(4) 127.3(2) yes 3_555 . . C(3) C(4) C(5) 129.2(2) yes . . . C(4) C(5) C(6) 128.8(3) yes . . . C(5) C(6) C(5) 129.2(3) yes . . 3_555 S(1) C(7) N(1) 124.6(2) yes . . . S(1) C(7) C(2) 117.9(2) yes . . . N(1) C(7) C(2) 117.5(2) yes . . . N(1) C(8) C(9) 110.4(2) yes . . . C(8) C(9) C(10) 111.5(2) yes . . . C(9) C(10) C(12) 109.7(2) yes . . . C(10) C(12) C(13) 111.0(2) yes . . . N(1) C(13) C(12) 110.6(2) yes . . . Cl(1) C(14) Cl(2) 111.2(2) yes . . . C(2) C(1) H(1) 125.3 no . . . C(2) C(1) H(1) 125.3 no 3_555 . . C(3) C(4) H(2) 115.4 no . . . C(5) C(4) H(2) 115.4 no . . . C(4) C(5) H(3) 115.6 no . . . C(6) C(5) H(3) 115.6 no . . . C(5) C(6) H(4) 115.4 no . . . C(5) C(6) H(4) 115.4 no 3_555 . . N(1) C(8) H(5) 109.6 no . . . N(1) C(8) H(6) 109.6 no . . . C(9) C(8) H(5) 109.6 no . . . C(9) C(8) H(6) 109.6 no . . . H(5) C(8) H(6) 108.1 no . . . C(8) C(9) H(7) 109.3 no . . . C(8) C(9) H(8) 109.3 no . . . C(10) C(9) H(7) 109.3 no . . . C(10) C(9) H(8) 109.3 no . . . H(7) C(9) H(8) 108.0 no . . . C(9) C(10) H(9) 109.7 no . . . C(9) C(10) H(10) 109.7 no . . . C(12) C(10) H(9) 109.7 no . . . C(12) C(10) H(10) 109.7 no . . . H(9) C(10) H(10) 108.2 no . . . C(10) C(12) H(11) 109.4 no . . . C(10) C(12) H(12) 109.4 no . . . C(13) C(12) H(11) 109.4 no . . . C(13) C(12) H(12) 109.4 no . . . H(11) C(12) H(12) 108.0 no . . . N(1) C(13) H(13) 109.5 no . . . N(1) C(13) H(14) 109.5 no . . . C(12) C(13) H(13) 109.5 no . . . C(12) C(13) H(14) 109.5 no . . . H(13) C(13) H(14) 108.1 no . . . Cl(1) C(14) H(15) 106.9(19) no . . . Cl(1) C(14) H(15) 107(2) no . . 3_555 Cl(2) C(14) H(15) 108.6(19) no . . . Cl(2) C(14) H(15) 108.6(19) no . . 3_555 H(15) C(14) H(15) 115(2) no . . 3_555 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(7) N(1) C(8) C(9) -126.4(2) ? . . . . C(8) N(1) C(7) S(1) -1.8(4) ? . . . . C(8) N(1) C(7) C(2) 176.8(2) ? . . . . C(7) N(1) C(13) C(12) 126.1(3) ? . . . . C(13) N(1) C(7) S(1) 174.1(2) ? . . . . C(13) N(1) C(7) C(2) -7.3(4) ? . . . . C(8) N(1) C(13) C(12) -57.6(3) ? . . . . C(13) N(1) C(8) C(9) 57.3(3) ? . . . . C(2) C(1) C(2) C(3) -2.7(4) ? . . 3_555 3_555 C(2) C(1) C(2) C(7) -177.9(2) ? . . 3_555 3_555 C(2) C(1) C(2) C(3) 2.7(4) ? 3_555 . . . C(2) C(1) C(2) C(7) 177.9(2) ? 3_555 . . . C(1) C(2) C(3) C(4) 177.3(3) ? . . . . C(1) C(2) C(3) C(3) -1.6(3) ? . . . 3_555 C(1) C(2) C(7) S(1) -70.1(3) ? . . . . C(1) C(2) C(7) N(1) 111.2(3) ? . . . . C(3) C(2) C(7) S(1) 104.3(2) ? . . . . C(3) C(2) C(7) N(1) -74.3(3) ? . . . . C(7) C(2) C(3) C(4) 2.0(4) ? . . . . C(7) C(2) C(3) C(3) -176.9(2) ? . . . 3_555 C(2) C(3) C(3) C(4) 178.9(2) ? . . 3_555 3_555 C(2) C(3) C(4) C(5) 179.9(2) ? . . . . C(3) C(3) C(4) C(5) -1.5(4) ? 3_555 . . . C(4) C(3) C(3) C(2) -178.9(2) ? . . 3_555 3_555 C(3) C(4) C(5) C(6) 0.3(5) ? . . . . C(4) C(5) C(6) C(5) 2.1(6) ? . . . 3_555 N(1) C(8) C(9) C(10) -55.5(3) ? . . . . C(8) C(9) C(10) C(12) 54.8(3) ? . . . . C(9) C(10) C(12) C(13) -54.8(3) ? . . . . C(10) C(12) C(13) N(1) 56.1(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(2) C(3) 3.551(2) ? . . Cl(2) C(3) 3.551(2) ? . 3_555 C(1) C(14) 3.349(6) ? . 1_554 C(3) Cl(2) 3.551(2) ? . . C(14) C(1) 3.349(6) ? . 1_556 Cl(1) H(1) 3.554 ? . 1_556 Cl(1) H(4) 3.479 ? . 6_556 Cl(1) H(5) 3.424 ? . 2_655 Cl(1) H(5) 3.424 ? . 4_655 Cl(1) H(7) 3.316 ? . 2_655 Cl(1) H(7) 3.316 ? . 4_655 Cl(1) H(13) 3.200 ? . . Cl(1) H(13) 3.200 ? . 3_555 Cl(1) H(14) 3.530 ? . . Cl(1) H(14) 3.530 ? . 3_555 Cl(2) H(9) 3.043 ? . 5_657 Cl(2) H(9) 3.043 ? . 7_657 Cl(2) H(12) 3.495 ? . . Cl(2) H(12) 3.495 ? . 3_555 Cl(2) H(13) 3.092 ? . . Cl(2) H(13) 3.092 ? . 3_555 S(1) H(2) 2.905 ? . 5_656 S(1) H(3) 3.035 ? . 5_656 S(1) H(5) 2.842 ? . 4_654 S(1) H(8) 3.088 ? . 5_656 S(1) H(10) 3.247 ? . 4_654 S(1) H(12) 3.015 ? . 1_554 S(1) H(14) 3.294 ? . 4_654 S(1) H(15) 2.70(3) ? . 3_554 N(1) H(10) 3.402 ? . 4_654 C(1) H(4) 2.987 ? . 6_556 C(1) H(15) 2.99(3) ? . 1_554 C(1) H(15) 2.99(3) ? . 3_554 C(2) H(15) 3.15(3) ? . 3_554 C(3) H(8) 3.549 ? . 5_656 C(4) H(6) 2.936 ? . 5_656 C(4) H(8) 3.330 ? . 5_656 C(4) H(9) 3.566 ? . 5_657 C(5) H(6) 2.863 ? . 5_656 C(5) H(9) 3.140 ? . 5_657 C(5) H(10) 3.584 ? . 5_657 C(5) H(14) 3.215 ? . 8_456 C(6) H(1) 3.528 ? . 6_456 C(7) H(10) 3.234 ? . 4_654 C(7) H(15) 3.42(3) ? . 3_554 C(8) H(2) 3.464 ? . 5_656 C(8) H(3) 3.571 ? . 5_656 C(8) H(10) 3.579 ? . 4_654 C(8) H(14) 3.301 ? . 4_654 C(10) H(3) 3.376 ? . 5_657 C(10) H(11) 3.320 ? . 5_657 C(12) H(5) 3.597 ? . 4_655 C(12) H(9) 3.362 ? . 5_657 C(12) H(11) 3.130 ? . 5_657 C(13) H(3) 3.268 ? . 8_556 C(13) H(6) 3.595 ? . 4_655 C(14) H(1) 3.259 ? . 1_556 C(14) H(12) 3.473 ? . . C(14) H(12) 3.473 ? . 3_555 C(14) H(13) 3.599 ? . . C(14) H(13) 3.599 ? . 3_555 H(1) Cl(1) 3.554 ? . 1_554 H(1) C(6) 3.528 ? . 6_556 H(1) C(14) 3.259 ? . 1_554 H(1) H(4) 2.674 ? . 6_556 H(1) H(10) 3.421 ? . 2_654 H(1) H(10) 3.421 ? . 4_654 H(1) H(15) 2.986 ? . 1_554 H(1) H(15) 2.986 ? . 3_554 H(2) S(1) 2.905 ? . 5_656 H(2) C(8) 3.464 ? . 5_656 H(2) H(6) 2.706 ? . 5_656 H(2) H(8) 3.132 ? . 5_656 H(2) H(9) 3.595 ? . 5_657 H(3) S(1) 3.035 ? . 5_656 H(3) C(8) 3.571 ? . 5_656 H(3) C(10) 3.376 ? . 5_657 H(3) C(13) 3.268 ? . 8_456 H(3) H(5) 3.579 ? . 8_456 H(3) H(6) 2.584 ? . 5_656 H(3) H(9) 2.894 ? . 5_657 H(3) H(10) 3.002 ? . 5_657 H(3) H(13) 3.448 ? . 8_456 H(3) H(14) 2.453 ? . 8_456 H(4) Cl(1) 3.479 ? . 6_456 H(4) C(1) 2.987 ? . 6_456 H(4) H(1) 2.674 ? . 6_456 H(4) H(13) 3.257 ? . 6_456 H(4) H(13) 3.257 ? . 8_456 H(4) H(14) 3.327 ? . 6_456 H(4) H(14) 3.327 ? . 8_456 H(5) Cl(1) 3.424 ? . 2_644 H(5) S(1) 2.842 ? . 4_655 H(5) C(12) 3.597 ? . 4_654 H(5) H(3) 3.579 ? . 8_556 H(5) H(10) 3.226 ? . 4_654 H(5) H(12) 2.960 ? . 4_654 H(5) H(14) 3.073 ? . 4_654 H(6) C(4) 2.936 ? . 5_656 H(6) C(5) 2.863 ? . 5_656 H(6) C(13) 3.595 ? . 4_654 H(6) H(2) 2.706 ? . 5_656 H(6) H(3) 2.584 ? . 5_656 H(6) H(10) 3.513 ? . 4_654 H(6) H(14) 2.663 ? . 4_654 H(7) Cl(1) 3.316 ? . 2_644 H(7) H(7) 3.010 ? . 3_545 H(8) S(1) 3.088 ? . 5_656 H(8) C(3) 3.549 ? . 5_656 H(8) C(4) 3.330 ? . 5_656 H(8) H(2) 3.132 ? . 5_656 H(8) H(15) 3.185 ? . 7_647 H(9) Cl(2) 3.043 ? . 5_657 H(9) C(4) 3.566 ? . 5_657 H(9) C(5) 3.140 ? . 5_657 H(9) C(12) 3.362 ? . 5_657 H(9) H(2) 3.595 ? . 5_657 H(9) H(3) 2.894 ? . 5_657 H(9) H(11) 2.643 ? . 5_657 H(9) H(12) 3.177 ? . 5_657 H(10) S(1) 3.247 ? . 4_655 H(10) N(1) 3.402 ? . 4_655 H(10) C(5) 3.584 ? . 5_657 H(10) C(7) 3.234 ? . 4_655 H(10) C(8) 3.579 ? . 4_655 H(10) H(1) 3.421 ? . 2_645 H(10) H(3) 3.002 ? . 5_657 H(10) H(5) 3.226 ? . 4_655 H(10) H(6) 3.513 ? . 4_655 H(11) C(10) 3.320 ? . 5_657 H(11) C(12) 3.130 ? . 5_657 H(11) H(9) 2.643 ? . 5_657 H(11) H(11) 2.767 ? . 5_657 H(11) H(12) 2.903 ? . 5_657 H(12) Cl(2) 3.495 ? . . H(12) S(1) 3.015 ? . 1_556 H(12) C(14) 3.473 ? . . H(12) H(5) 2.960 ? . 4_655 H(12) H(9) 3.177 ? . 5_657 H(12) H(11) 2.903 ? . 5_657 H(12) H(15) 3.002 ? . 3_555 H(13) Cl(1) 3.200 ? . . H(13) Cl(2) 3.092 ? . . H(13) C(14) 3.599 ? . . H(13) H(3) 3.448 ? . 8_556 H(13) H(4) 3.257 ? . 6_556 H(14) Cl(1) 3.530 ? . . H(14) S(1) 3.294 ? . 4_655 H(14) C(5) 3.215 ? . 8_556 H(14) C(8) 3.301 ? . 4_655 H(14) H(3) 2.453 ? . 8_556 H(14) H(4) 3.327 ? . 6_556 H(14) H(5) 3.073 ? . 4_655 H(14) H(6) 2.663 ? . 4_655 H(15) S(1) 2.70(3) ? . 3_556 H(15) C(1) 2.99(3) ? . 1_556 H(15) C(2) 3.15(3) ? . 3_556 H(15) C(7) 3.42(3) ? . 3_556 H(15) H(1) 2.986 ? . 1_556 H(15) H(8) 3.185 ? . 7_657 H(15) H(12) 3.002 ? . 3_555 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '2CIF.cif' data_azulenepdmune3 _database_code_depnum_ccdc_archive 'CCDC 750103' #TrackingRef '2CIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C25 H32 Cl N3 O Pd S2 ' _chemical_formula_moiety 'C25 H32 Cl N3 O Pd S2 ' _chemical_formula_weight 596.52 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 12.7161(6) _cell_length_b 14.7195(5) _cell_length_c 13.6311(6) _cell_angle_alpha 90.0000 _cell_angle_beta 91.4037(14) _cell_angle_gamma 90.0000 _cell_volume 2550.64(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15780 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 93.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224.00 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.700 _exptl_absorpt_correction_T_max 0.903 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 23767 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_theta_max 27.44 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5793 _reflns_number_gt 4834 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0705 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5793 _refine_ls_number_parameters 299 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0302P)^2^+1.4779P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.67 _refine_diff_density_min -0.46 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.999 1.007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Pd(1) Pd 0.215260(14) 0.313846(12) 0.340899(13) 0.01433(5) Uani 1.00 1 d . . . Cl(1) Cl 0.16421(5) 0.22198(4) 0.20269(5) 0.02271(14) Uani 1.00 1 d . . . S(1) S 0.14329(5) 0.44848(4) 0.28315(4) 0.01922(13) Uani 1.00 1 d . . . S(2) S 0.30970(5) 0.20140(4) 0.42614(4) 0.01840(13) Uani 1.00 1 d . . . O(1) O 0.1817(2) 0.33660(15) 0.9240(2) 0.0510(6) Uani 1.00 1 d . . . N(1) N 0.12624(16) 0.60193(14) 0.38497(14) 0.0166(4) Uani 1.00 1 d . . . N(2) N 0.39115(16) 0.22112(13) 0.60752(15) 0.0166(4) Uani 1.00 1 d . . . N(3) N 0.31269(19) 0.41910(16) 0.99618(18) 0.0289(5) Uani 1.00 1 d . . . C(1) C 0.25758(18) 0.38875(16) 0.45004(17) 0.0152(4) Uani 1.00 1 d . . . C(2) C 0.24549(18) 0.48418(16) 0.45450(17) 0.0141(4) Uani 1.00 1 d . . . C(3) C 0.32243(18) 0.51807(16) 0.52425(17) 0.0146(4) Uani 1.00 1 d . . . C(4) C 0.37248(18) 0.43725(16) 0.57072(16) 0.0138(4) Uani 1.00 1 d . . . C(5) C 0.35643(18) 0.60791(16) 0.53468(17) 0.0155(4) Uani 1.00 1 d . . . C(6) C 0.32462(18) 0.35903(16) 0.52662(17) 0.0147(4) Uani 1.00 1 d . . . C(7) C 0.17357(18) 0.52221(16) 0.38067(17) 0.0149(4) Uani 1.00 1 d . . . C(8) C 0.43508(19) 0.64426(17) 0.59630(18) 0.0179(5) Uani 1.00 1 d . . . C(9) C 0.50595(19) 0.60055(17) 0.65912(18) 0.0192(5) Uani 1.00 1 d . . . C(10) C 0.5202(2) 0.50788(17) 0.67290(18) 0.0188(5) Uani 1.00 1 d . . . C(11) C 0.46233(19) 0.43590(16) 0.63244(17) 0.0165(4) Uani 1.00 1 d . . . C(12) C 0.12294(19) 0.65809(17) 0.47380(18) 0.0185(5) Uani 1.00 1 d . . . C(13) C 0.34714(18) 0.26263(16) 0.53003(17) 0.0151(4) Uani 1.00 1 d . . . C(14) C 0.0094(2) 0.67942(18) 0.49925(19) 0.0229(5) Uani 1.00 1 d . . . C(15) C -0.0510(2) 0.72340(19) 0.4133(2) 0.0248(5) Uani 1.00 1 d . . . C(16) C -0.0458(2) 0.66136(18) 0.3240(2) 0.0242(5) Uani 1.00 1 d . . . C(17) C 0.0683(2) 0.64186(18) 0.30009(18) 0.0213(5) Uani 1.00 1 d . . . C(18) C 0.3722(2) 0.25074(17) 0.70882(17) 0.0185(5) Uani 1.00 1 d . . . C(19) C 0.2966(2) 0.18453(17) 0.75638(19) 0.0221(5) Uani 1.00 1 d . . . C(20) C 0.3381(2) 0.08695(18) 0.7543(2) 0.0264(5) Uani 1.00 1 d . . . C(21) C 0.3620(2) 0.05969(17) 0.6493(2) 0.0262(5) Uani 1.00 1 d . . . C(22) C 0.4350(2) 0.12833(17) 0.60227(19) 0.0208(5) Uani 1.00 1 d . . . C(23) C 0.2212(2) 0.3749(2) 0.9954(2) 0.0342(6) Uani 1.00 1 d . . . C(24) C 0.3525(2) 0.4649(2) 1.0836(2) 0.0429(8) Uani 1.00 1 d . . . C(25) C 0.3741(2) 0.4267(2) 0.9085(2) 0.0457(8) Uani 1.00 1 d . . . H(1) H 0.3207 0.6507 0.4937 0.019 Uiso 1.00 1 c R . . H(2) H 0.4409 0.7086 0.5949 0.022 Uiso 1.00 1 c R . . H(3) H 0.5505 0.6390 0.6977 0.023 Uiso 1.00 1 c R . . H(4) H 0.5771 0.4912 0.7157 0.023 Uiso 1.00 1 c R . . H(5) H 0.4876 0.3771 0.6493 0.020 Uiso 1.00 1 c R . . H(6) H 0.1616 0.7155 0.4631 0.022 Uiso 1.00 1 c R . . H(7) H 0.1578 0.6255 0.5292 0.022 Uiso 1.00 1 c R . . H(8) H 0.0089 0.7209 0.5564 0.027 Uiso 1.00 1 c R . . H(9) H -0.0266 0.6225 0.5179 0.027 Uiso 1.00 1 c R . . H(10) H -0.1252 0.7332 0.4308 0.030 Uiso 1.00 1 c R . . H(11) H -0.0196 0.7831 0.3980 0.030 Uiso 1.00 1 c R . . H(12) H -0.0827 0.6036 0.3376 0.029 Uiso 1.00 1 c R . . H(13) H -0.0816 0.6908 0.2671 0.029 Uiso 1.00 1 c R . . H(14) H 0.0706 0.5994 0.2439 0.026 Uiso 1.00 1 c R . . H(15) H 0.1031 0.6991 0.2806 0.026 Uiso 1.00 1 c R . . H(16) H 0.3417 0.3126 0.7084 0.022 Uiso 1.00 1 c R . . H(17) H 0.4395 0.2524 0.7469 0.022 Uiso 1.00 1 c R . . H(18) H 0.2276 0.1872 0.7212 0.026 Uiso 1.00 1 c R . . H(19) H 0.2859 0.2030 0.8253 0.026 Uiso 1.00 1 c R . . H(20) H 0.4029 0.0823 0.7959 0.032 Uiso 1.00 1 c R . . H(21) H 0.2850 0.0452 0.7812 0.032 Uiso 1.00 1 c R . . H(22) H 0.3954 -0.0011 0.6493 0.031 Uiso 1.00 1 c R . . H(23) H 0.2955 0.0559 0.6102 0.031 Uiso 1.00 1 c R . . H(24) H 0.5046 0.1268 0.6365 0.025 Uiso 1.00 1 c R . . H(25) H 0.4451 0.1117 0.5328 0.025 Uiso 1.00 1 c R . . H(26) H 0.1838 0.3730 1.0548 0.041 Uiso 1.00 1 c R . . H(27) H 0.3272 0.5278 1.0838 0.052 Uiso 1.00 1 c R . . H(28) H 0.4296 0.4646 1.0841 0.052 Uiso 1.00 1 c R . . H(29) H 0.3277 0.4334 1.1419 0.052 Uiso 1.00 1 c R . . H(30) H 0.4225 0.3751 0.9049 0.055 Uiso 1.00 1 c R . . H(31) H 0.4144 0.4834 0.9107 0.055 Uiso 1.00 1 c R . . H(32) H 0.3269 0.4268 0.8506 0.055 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.01499(9) 0.01645(10) 0.01147(9) -0.00129(7) -0.00159(7) -0.00262(7) Cl(1) 0.0217(3) 0.0265(3) 0.0197(3) 0.0011(2) -0.0052(2) -0.0102(2) S(1) 0.0223(3) 0.0203(3) 0.0147(2) 0.0019(2) -0.0059(2) -0.0025(2) S(2) 0.0244(3) 0.0161(2) 0.0146(2) 0.0002(2) -0.0027(2) -0.0029(2) O(1) 0.0592(15) 0.0277(11) 0.0649(17) -0.0101(10) -0.0212(13) -0.0026(11) N(1) 0.0188(10) 0.0191(10) 0.0118(9) 0.0012(8) -0.0010(8) 0.0016(7) N(2) 0.0203(10) 0.0158(10) 0.0138(9) 0.0025(8) 0.0001(8) 0.0001(7) N(3) 0.0306(13) 0.0294(12) 0.0266(12) 0.0006(10) 0.0003(10) -0.0029(9) C(1) 0.0134(11) 0.0200(12) 0.0122(11) -0.0018(9) 0.0024(9) -0.0021(8) C(2) 0.0144(10) 0.0162(11) 0.0118(10) 0.0003(8) 0.0004(9) -0.0004(8) C(3) 0.0132(10) 0.0186(12) 0.0121(11) 0.0009(8) 0.0023(9) -0.0009(8) C(4) 0.0152(11) 0.0174(11) 0.0091(10) -0.0008(8) 0.0031(8) -0.0004(8) C(5) 0.0150(11) 0.0192(12) 0.0123(11) 0.0010(9) 0.0014(9) -0.0004(8) C(6) 0.0150(11) 0.0174(11) 0.0117(10) -0.0004(9) 0.0016(9) 0.0001(8) C(7) 0.0121(10) 0.0196(12) 0.0129(11) -0.0015(9) 0.0011(9) -0.0006(8) C(8) 0.0186(11) 0.0162(12) 0.0192(12) -0.0018(9) 0.0029(10) -0.0027(9) C(9) 0.0176(11) 0.0223(12) 0.0178(12) -0.0049(9) 0.0017(9) -0.0050(9) C(10) 0.0193(12) 0.0235(13) 0.0134(11) 0.0001(9) -0.0024(9) -0.0005(9) C(11) 0.0186(11) 0.0191(12) 0.0119(10) 0.0009(9) 0.0014(9) 0.0018(8) C(12) 0.0192(12) 0.0194(12) 0.0168(11) 0.0007(9) -0.0026(10) -0.0031(9) C(13) 0.0147(11) 0.0172(12) 0.0134(11) -0.0010(9) 0.0017(9) -0.0007(8) C(14) 0.0214(12) 0.0293(14) 0.0179(12) 0.0040(10) 0.0005(10) -0.0011(10) C(15) 0.0169(12) 0.0322(15) 0.0254(14) 0.0057(10) 0.0023(11) 0.0045(11) C(16) 0.0210(12) 0.0268(14) 0.0245(13) 0.0010(10) -0.0050(11) 0.0052(10) C(17) 0.0258(13) 0.0236(13) 0.0144(12) 0.0056(10) -0.0040(10) 0.0033(9) C(18) 0.0229(12) 0.0209(12) 0.0115(11) 0.0011(9) -0.0009(9) -0.0009(9) C(19) 0.0244(13) 0.0240(13) 0.0180(12) 0.0014(10) 0.0029(10) 0.0040(10) C(20) 0.0307(14) 0.0221(13) 0.0265(14) -0.0017(11) 0.0031(12) 0.0067(10) C(21) 0.0357(15) 0.0166(12) 0.0261(14) 0.0005(11) -0.0034(12) 0.0016(10) C(22) 0.0243(13) 0.0211(13) 0.0169(12) 0.0080(10) -0.0005(10) 0.0009(9) C(23) 0.0336(16) 0.0260(15) 0.0427(18) -0.0036(12) -0.0049(14) 0.0113(13) C(24) 0.0338(17) 0.063(2) 0.0320(17) -0.0013(15) -0.0052(14) -0.0106(15) C(25) 0.0437(19) 0.053(2) 0.0411(19) -0.0017(16) 0.0143(16) -0.0093(16) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Pd(1) Cl(1) 2.3957(6) yes . . Pd(1) S(1) 2.3128(6) yes . . Pd(1) S(2) 2.3374(6) yes . . Pd(1) C(1) 1.918(2) yes . . S(1) C(7) 1.752(2) yes . . S(2) C(13) 1.735(2) yes . . O(1) C(23) 1.221(4) yes . . N(1) C(7) 1.321(3) yes . . N(1) C(12) 1.468(3) yes . . N(1) C(17) 1.478(3) yes . . N(2) C(13) 1.332(3) yes . . N(2) C(18) 1.473(3) yes . . N(2) C(22) 1.478(3) yes . . N(3) C(23) 1.334(3) yes . . N(3) C(24) 1.450(4) yes . . N(3) C(25) 1.448(4) yes . . C(1) C(2) 1.415(3) yes . . C(1) C(6) 1.401(3) yes . . C(2) C(3) 1.437(3) yes . . C(2) C(7) 1.455(3) yes . . C(3) C(4) 1.484(3) yes . . C(3) C(5) 1.397(3) yes . . C(4) C(6) 1.428(3) yes . . C(4) C(11) 1.402(3) yes . . C(5) C(8) 1.397(3) yes . . C(6) C(13) 1.448(3) yes . . C(8) C(9) 1.386(3) yes . . C(9) C(10) 1.388(3) yes . . C(10) C(11) 1.396(3) yes . . C(12) C(14) 1.526(3) yes . . C(14) C(15) 1.529(3) yes . . C(15) C(16) 1.524(3) yes . . C(16) C(17) 1.523(3) yes . . C(18) C(19) 1.525(3) yes . . C(19) C(20) 1.531(3) yes . . C(20) C(21) 1.525(3) yes . . C(21) C(22) 1.524(3) yes . . C(5) H(1) 0.950 no . . C(8) H(2) 0.950 no . . C(9) H(3) 0.950 no . . C(10) H(4) 0.950 no . . C(11) H(5) 0.950 no . . C(12) H(6) 0.990 no . . C(12) H(7) 0.990 no . . C(14) H(8) 0.990 no . . C(14) H(9) 0.990 no . . C(15) H(10) 0.990 no . . C(15) H(11) 0.990 no . . C(16) H(12) 0.990 no . . C(16) H(13) 0.990 no . . C(17) H(14) 0.990 no . . C(17) H(15) 0.990 no . . C(18) H(16) 0.990 no . . C(18) H(17) 0.990 no . . C(19) H(18) 0.990 no . . C(19) H(19) 0.990 no . . C(20) H(20) 0.990 no . . C(20) H(21) 0.990 no . . C(21) H(22) 0.990 no . . C(21) H(23) 0.990 no . . C(22) H(24) 0.990 no . . C(22) H(25) 0.990 no . . C(23) H(26) 0.950 no . . C(24) H(27) 0.980 no . . C(24) H(28) 0.980 no . . C(24) H(29) 0.980 no . . C(25) H(30) 0.980 no . . C(25) H(31) 0.980 no . . C(25) H(32) 0.980 no . . 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Pd(1) S(1) 96.81(2) yes . . . Cl(1) Pd(1) S(2) 96.73(2) yes . . . Cl(1) Pd(1) C(1) 178.97(7) yes . . . S(1) Pd(1) S(2) 165.96(2) yes . . . S(1) Pd(1) C(1) 82.68(7) yes . . . S(2) Pd(1) C(1) 83.71(7) yes . . . Pd(1) S(1) C(7) 101.23(8) yes . . . Pd(1) S(2) C(13) 99.51(8) yes . . . C(7) N(1) C(12) 124.01(19) yes . . . C(7) N(1) C(17) 122.51(19) yes . . . C(12) N(1) C(17) 113.46(19) yes . . . C(13) N(2) C(18) 122.17(19) yes . . . C(13) N(2) C(22) 122.5(2) yes . . . C(18) N(2) C(22) 112.92(18) yes . . . C(23) N(3) C(24) 121.4(2) yes . . . C(23) N(3) C(25) 121.3(2) yes . . . C(24) N(3) C(25) 117.2(2) yes . . . Pd(1) C(1) C(2) 125.13(17) yes . . . Pd(1) C(1) C(6) 123.52(17) yes . . . C(2) C(1) C(6) 110.0(2) yes . . . C(1) C(2) C(3) 107.47(19) yes . . . C(1) C(2) C(7) 114.8(2) yes . . . C(3) C(2) C(7) 136.9(2) yes . . . C(2) C(3) C(4) 106.39(19) yes . . . C(2) C(3) C(5) 126.9(2) yes . . . C(4) C(3) C(5) 125.9(2) yes . . . C(3) C(4) C(6) 107.02(18) yes . . . C(3) C(4) C(11) 127.0(2) yes . . . C(6) C(4) C(11) 125.0(2) yes . . . C(3) C(5) C(8) 129.7(2) yes . . . C(1) C(6) C(4) 107.9(2) yes . . . C(1) C(6) C(13) 116.5(2) yes . . . C(4) C(6) C(13) 134.0(2) yes . . . S(1) C(7) N(1) 119.49(17) yes . . . S(1) C(7) C(2) 114.16(17) yes . . . N(1) C(7) C(2) 126.2(2) yes . . . C(5) C(8) C(9) 129.7(2) yes . . . C(8) C(9) C(10) 128.3(2) yes . . . C(9) C(10) C(11) 128.8(2) yes . . . C(4) C(11) C(10) 129.8(2) yes . . . N(1) C(12) C(14) 110.47(19) yes . . . S(2) C(13) N(2) 120.70(17) yes . . . S(2) C(13) C(6) 115.64(16) yes . . . N(2) C(13) C(6) 123.6(2) yes . . . C(12) C(14) C(15) 111.9(2) yes . . . C(14) C(15) C(16) 109.1(2) yes . . . C(15) C(16) C(17) 110.1(2) yes . . . N(1) C(17) C(16) 111.5(2) yes . . . N(2) C(18) C(19) 109.18(19) yes . . . C(18) C(19) C(20) 111.7(2) yes . . . C(19) C(20) C(21) 109.9(2) yes . . . C(20) C(21) C(22) 111.0(2) yes . . . N(2) C(22) C(21) 111.0(2) yes . . . O(1) C(23) N(3) 124.9(3) yes . . . C(3) C(5) H(1) 115.1 no . . . C(8) C(5) H(1) 115.2 no . . . C(5) C(8) H(2) 115.1 no . . . C(9) C(8) H(2) 115.2 no . . . C(8) C(9) H(3) 115.8 no . . . C(10) C(9) H(3) 115.8 no . . . C(9) C(10) H(4) 115.6 no . . . C(11) C(10) H(4) 115.6 no . . . C(4) C(11) H(5) 115.1 no . . . C(10) C(11) H(5) 115.1 no . . . N(1) C(12) H(6) 109.6 no . . . N(1) C(12) H(7) 109.6 no . . . C(14) C(12) H(6) 109.6 no . . . C(14) C(12) H(7) 109.6 no . . . H(6) C(12) H(7) 108.1 no . . . C(12) C(14) H(8) 109.2 no . . . C(12) C(14) H(9) 109.2 no . . . C(15) C(14) H(8) 109.2 no . . . C(15) C(14) H(9) 109.2 no . . . H(8) C(14) H(9) 107.9 no . . . C(14) C(15) H(10) 109.9 no . . . C(14) C(15) H(11) 109.9 no . . . C(16) C(15) H(10) 109.9 no . . . C(16) C(15) H(11) 109.8 no . . . H(10) C(15) H(11) 108.3 no . . . C(15) C(16) H(12) 109.6 no . . . C(15) C(16) H(13) 109.6 no . . . C(17) C(16) H(12) 109.6 no . . . C(17) C(16) H(13) 109.6 no . . . H(12) C(16) H(13) 108.1 no . . . N(1) C(17) H(14) 109.3 no . . . N(1) C(17) H(15) 109.3 no . . . C(16) C(17) H(14) 109.3 no . . . C(16) C(17) H(15) 109.3 no . . . H(14) C(17) H(15) 108.0 no . . . N(2) C(18) H(16) 109.8 no . . . N(2) C(18) H(17) 109.8 no . . . C(19) C(18) H(16) 109.8 no . . . C(19) C(18) H(17) 109.8 no . . . H(16) C(18) H(17) 108.3 no . . . C(18) C(19) H(18) 109.3 no . . . C(18) C(19) H(19) 109.3 no . . . C(20) C(19) H(18) 109.3 no . . . C(20) C(19) H(19) 109.3 no . . . H(18) C(19) H(19) 107.9 no . . . C(19) C(20) H(20) 109.7 no . . . C(19) C(20) H(21) 109.7 no . . . C(21) C(20) H(20) 109.7 no . . . C(21) C(20) H(21) 109.7 no . . . H(20) C(20) H(21) 108.2 no . . . C(20) C(21) H(22) 109.4 no . . . C(20) C(21) H(23) 109.4 no . . . C(22) C(21) H(22) 109.5 no . . . C(22) C(21) H(23) 109.5 no . . . H(22) C(21) H(23) 108.0 no . . . N(2) C(22) H(24) 109.4 no . . . N(2) C(22) H(25) 109.4 no . . . C(21) C(22) H(24) 109.4 no . . . C(21) C(22) H(25) 109.5 no . . . H(24) C(22) H(25) 108.0 no . . . O(1) C(23) H(26) 117.5 no . . . N(3) C(23) H(26) 117.5 no . . . N(3) C(24) H(27) 109.5 no . . . N(3) C(24) H(28) 109.5 no . . . N(3) C(24) H(29) 109.5 no . . . H(27) C(24) H(28) 109.5 no . . . H(27) C(24) H(29) 109.5 no . . . H(28) C(24) H(29) 109.5 no . . . N(3) C(25) H(30) 109.5 no . . . N(3) C(25) H(31) 109.5 no . . . N(3) C(25) H(32) 109.5 no . . . H(30) C(25) H(31) 109.5 no . . . H(30) C(25) H(32) 109.5 no . . . H(31) C(25) H(32) 109.5 no . . . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Pd(1) S(1) C(7) 178.84(8) ? . . . . Cl(1) Pd(1) S(2) C(13) -178.62(8) ? . . . . Cl(1) Pd(1) C(1) C(2) 54(3) ? . . . . Cl(1) Pd(1) C(1) C(6) -112(3) ? . . . . S(1) Pd(1) S(2) C(13) 16.64(13) ? . . . . S(2) Pd(1) S(1) C(7) -16.42(13) ? . . . . S(1) Pd(1) C(1) C(2) -6.82(19) ? . . . . S(1) Pd(1) C(1) C(6) -172.4(2) ? . . . . C(1) Pd(1) S(1) C(7) -2.06(10) ? . . . . S(2) Pd(1) C(1) C(2) 169.7(2) ? . . . . S(2) Pd(1) C(1) C(6) 4.09(19) ? . . . . C(1) Pd(1) S(2) C(13) 2.31(10) ? . . . . Pd(1) S(1) C(7) N(1) -165.67(17) ? . . . . Pd(1) S(1) C(7) C(2) 9.95(18) ? . . . . Pd(1) S(2) C(13) N(2) 170.21(18) ? . . . . Pd(1) S(2) C(13) C(6) -8.19(18) ? . . . . C(7) N(1) C(12) C(14) -123.8(2) ? . . . . C(12) N(1) C(7) S(1) 162.89(18) ? . . . . C(12) N(1) C(7) C(2) -12.2(3) ? . . . . C(7) N(1) C(17) C(16) 122.2(2) ? . . . . C(17) N(1) C(7) S(1) -15.2(3) ? . . . . C(17) N(1) C(7) C(2) 169.7(2) ? . . . . C(12) N(1) C(17) C(16) -56.1(2) ? . . . . C(17) N(1) C(12) C(14) 54.5(2) ? . . . . C(13) N(2) C(18) C(19) 104.4(2) ? . . . . C(18) N(2) C(13) S(2) -145.35(18) ? . . . . C(18) N(2) C(13) C(6) 32.9(3) ? . . . . C(13) N(2) C(22) C(21) -104.5(2) ? . . . . C(22) N(2) C(13) S(2) 15.8(3) ? . . . . C(22) N(2) C(13) C(6) -165.9(2) ? . . . . C(18) N(2) C(22) C(21) 58.3(2) ? . . . . C(22) N(2) C(18) C(19) -58.4(2) ? . . . . C(24) N(3) C(23) O(1) 178.3(2) ? . . . . C(25) N(3) C(23) O(1) 1.1(4) ? . . . . Pd(1) C(1) C(2) C(3) -156.16(17) ? . . . . Pd(1) C(1) C(2) C(7) 15.3(3) ? . . . . Pd(1) C(1) C(6) C(4) 156.74(17) ? . . . . Pd(1) C(1) C(6) C(13) -10.7(3) ? . . . . C(2) C(1) C(6) C(4) -10.8(2) ? . . . . C(2) C(1) C(6) C(13) -178.3(2) ? . . . . C(6) C(1) C(2) C(3) 11.1(2) ? . . . . C(6) C(1) C(2) C(7) -177.5(2) ? . . . . C(1) C(2) C(3) C(4) -6.9(2) ? . . . . C(1) C(2) C(3) C(5) 163.1(2) ? . . . . C(1) C(2) C(7) S(1) -15.7(2) ? . . . . C(1) C(2) C(7) N(1) 159.6(2) ? . . . . C(3) C(2) C(7) S(1) 152.3(2) ? . . . . C(3) C(2) C(7) N(1) -32.4(4) ? . . . . C(7) C(2) C(3) C(4) -175.5(2) ? . . . . C(7) C(2) C(3) C(5) -5.5(4) ? . . . . C(2) C(3) C(4) C(6) 0.5(2) ? . . . . C(2) C(3) C(4) C(11) 169.8(2) ? . . . . C(2) C(3) C(5) C(8) -175.5(2) ? . . . . C(4) C(3) C(5) C(8) -7.3(4) ? . . . . C(5) C(3) C(4) C(6) -169.6(2) ? . . . . C(5) C(3) C(4) C(11) -0.4(3) ? . . . . C(3) C(4) C(6) C(1) 6.1(2) ? . . . . C(3) C(4) C(6) C(13) 170.5(2) ? . . . . C(3) C(4) C(11) C(10) 6.9(4) ? . . . . C(6) C(4) C(11) C(10) 174.3(2) ? . . . . C(11) C(4) C(6) C(1) -163.4(2) ? . . . . C(11) C(4) C(6) C(13) 1.0(4) ? . . . . C(3) C(5) C(8) C(9) 5.0(4) ? . . . . C(1) C(6) C(13) S(2) 12.3(2) ? . . . . C(1) C(6) C(13) N(2) -166.0(2) ? . . . . C(4) C(6) C(13) S(2) -151.0(2) ? . . . . C(4) C(6) C(13) N(2) 30.6(4) ? . . . . C(5) C(8) C(9) C(10) 3.7(4) ? . . . . C(8) C(9) C(10) C(11) -5.0(4) ? . . . . C(9) C(10) C(11) C(4) -2.9(4) ? . . . . N(1) C(12) C(14) C(15) -54.9(2) ? . . . . C(12) C(14) C(15) C(16) 56.3(2) ? . . . . C(14) C(15) C(16) C(17) -56.4(2) ? . . . . C(15) C(16) C(17) N(1) 56.5(2) ? . . . . N(2) C(18) C(19) C(20) 56.8(2) ? . . . . C(18) C(19) C(20) C(21) -55.1(2) ? . . . . C(19) C(20) C(21) C(22) 53.5(2) ? . . . . C(20) C(21) C(22) N(2) -55.0(2) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) N(1) 3.436(2) ? . 2_545 Cl(1) C(11) 3.576(2) ? . 4_454 S(2) C(17) 3.594(2) ? . 2_545 O(1) C(5) 3.449(3) ? . 2_546 O(1) C(8) 3.206(3) ? . 2_546 O(1) C(19) 3.539(3) ? . . O(1) C(21) 3.473(3) ? . 2_556 N(1) Cl(1) 3.436(2) ? . 2_555 N(3) C(21) 3.596(3) ? . 2_556 C(1) C(9) 3.391(3) ? . 3_666 C(2) C(10) 3.487(3) ? . 3_666 C(3) C(10) 3.411(3) ? . 3_666 C(3) C(11) 3.578(3) ? . 3_666 C(4) C(8) 3.589(3) ? . 3_666 C(4) C(9) 3.571(3) ? . 3_666 C(5) O(1) 3.449(3) ? . 2_556 C(5) C(11) 3.343(3) ? . 3_666 C(6) C(8) 3.521(3) ? . 3_666 C(6) C(9) 3.417(3) ? . 3_666 C(8) O(1) 3.206(3) ? . 2_556 C(8) C(4) 3.589(3) ? . 3_666 C(8) C(6) 3.521(3) ? . 3_666 C(8) C(13) 3.570(3) ? . 3_666 C(9) C(1) 3.391(3) ? . 3_666 C(9) C(4) 3.571(3) ? . 3_666 C(9) C(6) 3.417(3) ? . 3_666 C(10) C(2) 3.487(3) ? . 3_666 C(10) C(3) 3.411(3) ? . 3_666 C(11) Cl(1) 3.576(2) ? . 4_555 C(11) C(3) 3.578(3) ? . 3_666 C(11) C(5) 3.343(3) ? . 3_666 C(13) C(8) 3.570(3) ? . 3_666 C(17) S(2) 3.594(2) ? . 2_555 C(19) O(1) 3.539(3) ? . . C(21) O(1) 3.473(3) ? . 2_546 C(21) N(3) 3.596(3) ? . 2_546 C(21) C(23) 3.508(4) ? . 2_546 C(23) C(21) 3.508(4) ? . 2_556 Pd(1) H(3) 3.116 ? . 3_666 Pd(1) H(8) 3.247 ? . 3_566 Pd(1) H(9) 3.250 ? . 3_566 Pd(1) H(10) 3.413 ? . 3_566 Pd(1) H(15) 3.335 ? . 2_545 Pd(1) H(29) 3.562 ? . 1_554 Cl(1) H(1) 2.886 ? . 2_545 Cl(1) H(4) 3.334 ? . 4_454 Cl(1) H(5) 2.760 ? . 4_454 Cl(1) H(6) 3.204 ? . 2_545 Cl(1) H(15) 2.982 ? . 2_545 Cl(1) H(17) 2.959 ? . 4_454 Cl(1) H(24) 3.131 ? . 4_454 Cl(1) H(26) 3.015 ? . 1_554 S(1) H(9) 3.293 ? . 3_566 S(1) H(20) 3.099 ? . 4_454 S(1) H(24) 2.857 ? . 4_454 S(1) H(26) 3.356 ? . 1_554 S(1) H(29) 3.078 ? . 1_554 S(2) H(2) 3.456 ? . 3_666 S(2) H(3) 3.418 ? . 3_666 S(2) H(10) 3.234 ? . 3_566 S(2) H(14) 3.181 ? . 2_545 S(2) H(15) 3.054 ? . 2_545 S(2) H(27) 3.093 ? . 2_546 O(1) H(1) 2.958 ? . 2_546 O(1) H(2) 2.455 ? . 2_546 O(1) H(6) 3.060 ? . 2_546 O(1) H(13) 2.899 ? . 3_566 O(1) H(18) 3.591 ? . . O(1) H(19) 2.742 ? . . O(1) H(22) 2.761 ? . 2_556 O(1) H(23) 3.275 ? . 2_556 O(1) H(25) 3.471 ? . 4_455 N(2) H(10) 3.475 ? . 3_566 N(3) H(6) 3.065 ? . 2_546 N(3) H(11) 3.580 ? . 2_546 N(3) H(22) 3.472 ? . 2_556 N(3) H(23) 2.820 ? . 2_556 C(1) H(3) 3.228 ? . 3_666 C(1) H(4) 3.589 ? . 3_666 C(1) H(9) 2.985 ? . 3_566 C(1) H(10) 2.971 ? . 3_566 C(2) H(4) 3.295 ? . 3_666 C(2) H(9) 3.227 ? . 3_566 C(3) H(4) 3.543 ? . 3_666 C(3) H(21) 3.040 ? . 2_556 C(4) H(21) 3.288 ? . 2_556 C(5) H(5) 3.242 ? . 3_666 C(5) H(19) 3.008 ? . 2_556 C(5) H(21) 3.257 ? . 2_556 C(6) H(2) 3.588 ? . 3_666 C(6) H(3) 3.480 ? . 3_666 C(6) H(10) 2.946 ? . 3_566 C(7) H(4) 3.467 ? . 3_666 C(7) H(9) 3.174 ? . 3_566 C(8) H(5) 3.526 ? . 3_666 C(8) H(13) 3.374 ? . 4_565 C(8) H(18) 3.334 ? . 2_556 C(8) H(19) 3.152 ? . 2_556 C(9) H(13) 3.594 ? . 4_565 C(9) H(15) 3.587 ? . 4_565 C(9) H(29) 3.435 ? . 3_667 C(10) H(28) 3.382 ? . 3_667 C(10) H(29) 3.259 ? . 3_667 C(10) H(31) 3.558 ? . . C(11) H(1) 3.525 ? . 3_666 C(11) H(32) 3.475 ? . . C(12) H(19) 3.021 ? . 2_556 C(12) H(20) 3.356 ? . 2_556 C(13) H(2) 3.252 ? . 3_666 C(13) H(10) 2.886 ? . 3_566 C(14) H(19) 3.509 ? . 2_556 C(14) H(20) 3.307 ? . 2_556 C(14) H(30) 3.271 ? . 2_556 C(15) H(18) 3.152 ? . 3_566 C(16) H(18) 3.259 ? . 3_566 C(16) H(22) 3.422 ? . 4_454 C(17) H(3) 3.520 ? . 4_464 C(18) H(8) 3.533 ? . 2_546 C(18) H(30) 3.289 ? . . C(18) H(32) 3.292 ? . . C(19) H(7) 3.091 ? . 2_546 C(19) H(8) 3.551 ? . 2_546 C(19) H(10) 3.529 ? . 3_566 C(19) H(13) 3.302 ? . 3_566 C(20) H(7) 3.004 ? . 2_546 C(20) H(12) 3.180 ? . 4_555 C(20) H(32) 3.444 ? . 2_546 C(21) H(12) 3.574 ? . 4_555 C(21) H(32) 3.098 ? . 2_546 C(22) H(26) 3.244 ? . 4_554 C(23) H(1) 3.346 ? . 2_546 C(23) H(2) 3.410 ? . 2_546 C(23) H(6) 2.829 ? . 2_546 C(23) H(19) 3.542 ? . . C(23) H(22) 3.046 ? . 2_556 C(23) H(23) 3.033 ? . 2_556 C(23) H(24) 3.398 ? . 4_455 C(23) H(25) 3.565 ? . 4_455 C(24) H(3) 3.545 ? . 3_667 C(24) H(4) 2.930 ? . 3_667 C(24) H(11) 3.422 ? . 2_546 C(24) H(23) 3.474 ? . 2_556 C(24) H(31) 3.059 ? . 3_667 C(25) H(8) 3.404 ? . 2_546 C(25) H(16) 3.221 ? . . C(25) H(17) 3.495 ? . . C(25) H(23) 2.881 ? . 2_556 C(25) H(28) 2.965 ? . 3_667 H(1) Cl(1) 2.886 ? . 2_555 H(1) O(1) 2.958 ? . 2_556 H(1) C(11) 3.525 ? . 3_666 H(1) C(23) 3.346 ? . 2_556 H(1) H(5) 3.184 ? . 3_666 H(1) H(19) 2.947 ? . 2_556 H(1) H(26) 3.338 ? . 2_556 H(2) S(2) 3.456 ? . 3_666 H(2) O(1) 2.455 ? . 2_556 H(2) C(6) 3.588 ? . 3_666 H(2) C(13) 3.252 ? . 3_666 H(2) C(23) 3.410 ? . 2_556 H(2) H(13) 2.795 ? . 4_565 H(2) H(15) 3.500 ? . 4_565 H(2) H(18) 3.351 ? . 2_556 H(2) H(19) 3.108 ? . 2_556 H(2) H(25) 3.500 ? . 3_666 H(2) H(26) 3.518 ? . 2_556 H(3) Pd(1) 3.116 ? . 3_666 H(3) S(2) 3.418 ? . 3_666 H(3) C(1) 3.228 ? . 3_666 H(3) C(6) 3.480 ? . 3_666 H(3) C(17) 3.520 ? . 4_565 H(3) C(24) 3.545 ? . 3_667 H(3) H(11) 3.112 ? . 4_565 H(3) H(13) 3.174 ? . 4_565 H(3) H(15) 2.715 ? . 4_565 H(3) H(28) 3.345 ? . 3_667 H(3) H(29) 2.854 ? . 3_667 H(4) Cl(1) 3.334 ? . 4_555 H(4) C(1) 3.589 ? . 3_666 H(4) C(2) 3.295 ? . 3_666 H(4) C(3) 3.543 ? . 3_666 H(4) C(7) 3.467 ? . 3_666 H(4) C(24) 2.930 ? . 3_667 H(4) H(27) 2.979 ? . 3_667 H(4) H(28) 2.808 ? . 3_667 H(4) H(29) 2.521 ? . 3_667 H(4) H(31) 3.409 ? . . H(5) Cl(1) 2.760 ? . 4_555 H(5) C(5) 3.242 ? . 3_666 H(5) C(8) 3.526 ? . 3_666 H(5) H(1) 3.184 ? . 3_666 H(5) H(32) 3.538 ? . . H(6) Cl(1) 3.204 ? . 2_555 H(6) O(1) 3.060 ? . 2_556 H(6) N(3) 3.065 ? . 2_556 H(6) C(23) 2.829 ? . 2_556 H(6) H(19) 2.950 ? . 2_556 H(6) H(26) 3.053 ? . 2_556 H(6) H(29) 3.517 ? . 2_556 H(6) H(30) 3.162 ? . 2_556 H(7) C(19) 3.091 ? . 2_556 H(7) C(20) 3.004 ? . 2_556 H(7) H(19) 2.384 ? . 2_556 H(7) H(20) 2.603 ? . 2_556 H(7) H(21) 2.919 ? . 2_556 H(8) Pd(1) 3.247 ? . 3_566 H(8) C(18) 3.533 ? . 2_556 H(8) C(19) 3.551 ? . 2_556 H(8) C(25) 3.404 ? . 2_556 H(8) H(17) 2.784 ? . 2_556 H(8) H(19) 3.045 ? . 2_556 H(8) H(20) 3.060 ? . 2_556 H(8) H(30) 2.483 ? . 2_556 H(9) Pd(1) 3.250 ? . 3_566 H(9) S(1) 3.293 ? . 3_566 H(9) C(1) 2.985 ? . 3_566 H(9) C(2) 3.227 ? . 3_566 H(9) C(7) 3.174 ? . 3_566 H(9) H(20) 3.012 ? . 2_556 H(10) Pd(1) 3.413 ? . 3_566 H(10) S(2) 3.234 ? . 3_566 H(10) N(2) 3.475 ? . 3_566 H(10) C(1) 2.971 ? . 3_566 H(10) C(6) 2.946 ? . 3_566 H(10) C(13) 2.886 ? . 3_566 H(10) C(19) 3.529 ? . 3_566 H(10) H(16) 3.373 ? . 3_566 H(10) H(18) 2.689 ? . 3_566 H(11) N(3) 3.580 ? . 2_556 H(11) C(24) 3.422 ? . 2_556 H(11) H(3) 3.112 ? . 4_464 H(11) H(18) 3.102 ? . 3_566 H(11) H(28) 2.913 ? . 2_556 H(11) H(29) 3.347 ? . 2_556 H(11) H(30) 3.227 ? . 2_556 H(11) H(31) 3.542 ? . 4_464 H(12) C(20) 3.180 ? . 4_454 H(12) C(21) 3.574 ? . 4_454 H(12) H(16) 3.558 ? . 3_566 H(12) H(20) 2.800 ? . 4_454 H(12) H(21) 2.856 ? . 4_454 H(12) H(22) 2.985 ? . 4_454 H(13) O(1) 2.899 ? . 3_566 H(13) C(8) 3.374 ? . 4_464 H(13) C(9) 3.594 ? . 4_464 H(13) C(19) 3.302 ? . 3_566 H(13) H(2) 2.795 ? . 4_464 H(13) H(3) 3.174 ? . 4_464 H(13) H(16) 3.333 ? . 3_566 H(13) H(18) 2.591 ? . 3_566 H(13) H(19) 3.259 ? . 3_566 H(13) H(22) 3.231 ? . 4_454 H(14) S(2) 3.181 ? . 2_555 H(14) H(20) 3.504 ? . 4_454 H(14) H(22) 2.929 ? . 4_454 H(15) Pd(1) 3.335 ? . 2_555 H(15) Cl(1) 2.982 ? . 2_555 H(15) S(2) 3.054 ? . 2_555 H(15) C(9) 3.587 ? . 4_464 H(15) H(2) 3.500 ? . 4_464 H(15) H(3) 2.715 ? . 4_464 H(16) C(25) 3.221 ? . . H(16) H(10) 3.373 ? . 3_566 H(16) H(12) 3.558 ? . 3_566 H(16) H(13) 3.333 ? . 3_566 H(16) H(30) 2.990 ? . . H(16) H(32) 2.576 ? . . H(17) Cl(1) 2.959 ? . 4_555 H(17) C(25) 3.495 ? . . H(17) H(8) 2.784 ? . 2_546 H(17) H(30) 2.823 ? . . H(17) H(32) 3.276 ? . . H(18) O(1) 3.591 ? . . H(18) C(8) 3.334 ? . 2_546 H(18) C(15) 3.152 ? . 3_566 H(18) C(16) 3.259 ? . 3_566 H(18) H(2) 3.351 ? . 2_546 H(18) H(10) 2.689 ? . 3_566 H(18) H(11) 3.102 ? . 3_566 H(18) H(13) 2.591 ? . 3_566 H(19) O(1) 2.742 ? . . H(19) C(5) 3.008 ? . 2_546 H(19) C(8) 3.152 ? . 2_546 H(19) C(12) 3.021 ? . 2_546 H(19) C(14) 3.509 ? . 2_546 H(19) C(23) 3.542 ? . . H(19) H(1) 2.947 ? . 2_546 H(19) H(2) 3.108 ? . 2_546 H(19) H(6) 2.950 ? . 2_546 H(19) H(7) 2.384 ? . 2_546 H(19) H(8) 3.045 ? . 2_546 H(19) H(13) 3.259 ? . 3_566 H(19) H(30) 3.243 ? . . H(19) H(32) 3.352 ? . . H(20) S(1) 3.099 ? . 4_555 H(20) C(12) 3.356 ? . 2_546 H(20) C(14) 3.307 ? . 2_546 H(20) H(7) 2.603 ? . 2_546 H(20) H(8) 3.060 ? . 2_546 H(20) H(9) 3.012 ? . 2_546 H(20) H(12) 2.800 ? . 4_555 H(20) H(14) 3.504 ? . 4_555 H(21) C(3) 3.040 ? . 2_546 H(21) C(4) 3.288 ? . 2_546 H(21) C(5) 3.257 ? . 2_546 H(21) H(7) 2.919 ? . 2_546 H(21) H(12) 2.856 ? . 4_555 H(21) H(32) 2.856 ? . 2_546 H(22) O(1) 2.761 ? . 2_546 H(22) N(3) 3.472 ? . 2_546 H(22) C(16) 3.422 ? . 4_555 H(22) C(23) 3.046 ? . 2_546 H(22) H(12) 2.985 ? . 4_555 H(22) H(13) 3.231 ? . 4_555 H(22) H(14) 2.929 ? . 4_555 H(22) H(26) 3.472 ? . 2_546 H(22) H(32) 3.020 ? . 2_546 H(23) O(1) 3.275 ? . 2_546 H(23) N(3) 2.820 ? . 2_546 H(23) C(23) 3.033 ? . 2_546 H(23) C(24) 3.474 ? . 2_546 H(23) C(25) 2.881 ? . 2_546 H(23) H(26) 3.522 ? . 2_546 H(23) H(27) 3.065 ? . 2_546 H(23) H(31) 2.882 ? . 2_546 H(23) H(32) 2.521 ? . 2_546 H(24) Cl(1) 3.131 ? . 4_555 H(24) S(1) 2.857 ? . 4_555 H(24) C(23) 3.398 ? . 4_554 H(24) H(26) 2.560 ? . 4_554 H(25) O(1) 3.471 ? . 4_554 H(25) C(23) 3.565 ? . 4_554 H(25) H(2) 3.500 ? . 3_666 H(25) H(26) 3.050 ? . 4_554 H(26) Cl(1) 3.015 ? . 1_556 H(26) S(1) 3.356 ? . 1_556 H(26) C(22) 3.244 ? . 4_455 H(26) H(1) 3.338 ? . 2_546 H(26) H(2) 3.518 ? . 2_546 H(26) H(6) 3.053 ? . 2_546 H(26) H(22) 3.472 ? . 2_556 H(26) H(23) 3.522 ? . 2_556 H(26) H(24) 2.560 ? . 4_455 H(26) H(25) 3.050 ? . 4_455 H(27) S(2) 3.093 ? . 2_556 H(27) H(4) 2.979 ? . 3_667 H(27) H(23) 3.065 ? . 2_556 H(27) H(30) 3.489 ? . 3_667 H(27) H(31) 3.289 ? . 3_667 H(28) C(10) 3.382 ? . 3_667 H(28) C(25) 2.965 ? . 3_667 H(28) H(3) 3.345 ? . 3_667 H(28) H(4) 2.808 ? . 3_667 H(28) H(11) 2.913 ? . 2_546 H(28) H(28) 3.124 ? . 3_667 H(28) H(30) 3.019 ? . 3_667 H(28) H(31) 2.125 ? . 3_667 H(28) H(32) 3.578 ? . 3_667 H(29) Pd(1) 3.562 ? . 1_556 H(29) S(1) 3.078 ? . 1_556 H(29) C(9) 3.435 ? . 3_667 H(29) C(10) 3.259 ? . 3_667 H(29) H(3) 2.854 ? . 3_667 H(29) H(4) 2.521 ? . 3_667 H(29) H(6) 3.517 ? . 2_546 H(29) H(11) 3.347 ? . 2_546 H(29) H(31) 3.589 ? . 3_667 H(30) C(14) 3.271 ? . 2_546 H(30) C(18) 3.289 ? . . H(30) H(6) 3.162 ? . 2_546 H(30) H(8) 2.483 ? . 2_546 H(30) H(11) 3.227 ? . 2_546 H(30) H(16) 2.990 ? . . H(30) H(17) 2.823 ? . . H(30) H(19) 3.243 ? . . H(30) H(27) 3.489 ? . 3_667 H(30) H(28) 3.019 ? . 3_667 H(31) C(10) 3.558 ? . . H(31) C(24) 3.059 ? . 3_667 H(31) H(4) 3.409 ? . . H(31) H(11) 3.542 ? . 4_565 H(31) H(23) 2.882 ? . 2_556 H(31) H(27) 3.289 ? . 3_667 H(31) H(28) 2.125 ? . 3_667 H(31) H(29) 3.589 ? . 3_667 H(31) H(31) 3.262 ? . 3_667 H(32) C(11) 3.475 ? . . H(32) C(18) 3.292 ? . . H(32) C(20) 3.444 ? . 2_556 H(32) C(21) 3.098 ? . 2_556 H(32) H(5) 3.538 ? . . H(32) H(16) 2.576 ? . . H(32) H(17) 3.276 ? . . H(32) H(19) 3.352 ? . . H(32) H(21) 2.856 ? . 2_556 H(32) H(22) 3.020 ? . 2_556 H(32) H(23) 2.521 ? . 2_556 H(32) H(28) 3.578 ? . 3_667 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '3CIF.cif' data_AzPt _database_code_depnum_ccdc_archive 'CCDC 750104' #TrackingRef '3CIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C25 H32 Cl N3 O Pt S2 ' _chemical_formula_moiety 'C25 H32 Cl N3 O Pt S2 ' _chemical_formula_weight 685.21 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 11.6349(3) _cell_length_b 15.3558(4) _cell_length_c 13.7152(3) _cell_angle_alpha 90.0000 _cell_angle_beta 96.3359(8) _cell_angle_gamma 90.0000 _cell_volume 2435.44(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 19001 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 93.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352.00 _exptl_absorpt_coefficient_mu 6.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.231 _exptl_absorpt_correction_T_max 0.299 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 23350 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_theta_max 27.42 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5525 _reflns_number_gt 4944 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0631 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5525 _refine_ls_number_parameters 282 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0179P)^2^+10.4900P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 1.57 _refine_diff_density_min -1.10 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pt Pt -1.703 8.390 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Pt(1) Pt 0.328013(12) 0.104647(9) 0.807917(10) 0.01306(4) Uani 1.00 1 d . . . Cl(1) Cl 0.41094(9) 0.11638(7) 0.65520(7) 0.0200(2) Uani 1.00 1 d . . . S(1) S 0.37024(9) -0.04035(6) 0.83710(7) 0.01667(18) Uani 1.00 1 d . . . S(2) S 0.26770(9) 0.24782(7) 0.81218(7) 0.0173(2) Uani 1.00 1 d . . . O(1) O 0.3661(5) 0.0164(4) 0.2955(4) 0.0292(14) Uiso 0.50 1 d P . . O(2) O 0.4723(8) 0.2727(6) 0.3318(7) 0.063(2) Uiso 0.50 1 d P . . N(1) N 0.3415(2) -0.1283(2) 0.9999(2) 0.0159(6) Uani 1.00 1 d . . . N(2) N 0.2062(2) 0.3252(2) 0.9726(2) 0.0154(6) Uani 1.00 1 d . . . N(3) N 0.4150(5) 0.1410(4) 0.3160(5) 0.0700(17) Uiso 1.00 1 d . . . C(1) C 0.2656(3) 0.0965(2) 0.9306(2) 0.0127(7) Uani 1.00 1 d . . . C(2) C 0.2542(3) 0.0189(2) 0.9838(2) 0.0137(7) Uani 1.00 1 d . . . C(3) C 0.1692(3) 0.0332(2) 1.0494(2) 0.0136(7) Uani 1.00 1 d . . . C(4) C 0.1393(3) 0.1280(2) 1.0438(2) 0.0128(7) Uani 1.00 1 d . . . C(5) C 0.0509(3) 0.1693(2) 1.0864(2) 0.0157(7) Uani 1.00 1 d . . . C(6) C 0.2079(3) 0.1650(2) 0.9734(2) 0.0130(7) Uani 1.00 1 d . . . C(7) C 0.3169(3) -0.0547(2) 0.9499(2) 0.0141(7) Uani 1.00 1 d . . . C(8) C -0.0253(3) 0.1361(2) 1.1486(2) 0.0181(8) Uani 1.00 1 d . . . C(9) C -0.0373(3) 0.0513(2) 1.1813(2) 0.0183(8) Uani 1.00 1 d . . . C(10) C 0.0211(3) -0.0229(2) 1.1566(2) 0.0174(8) Uani 1.00 1 d . . . C(11) C 0.1120(3) -0.0309(2) 1.0985(2) 0.0152(7) Uani 1.00 1 d . . . C(12) C 0.3995(3) -0.2011(2) 0.9552(3) 0.0211(8) Uani 1.00 1 d . . . C(13) C 0.2204(3) 0.2498(2) 0.9293(2) 0.0155(7) Uani 1.00 1 d . . . C(14) C 0.3655(3) -0.2877(2) 0.9976(3) 0.0223(8) Uani 1.00 1 d . . . C(15) C 0.3913(3) -0.2888(2) 1.1098(3) 0.0218(8) Uani 1.00 1 d . . . C(16) C 0.3299(3) -0.2127(2) 1.1534(3) 0.0224(8) Uani 1.00 1 d . . . C(17) C 0.3632(3) -0.1272(2) 1.1087(2) 0.0158(7) Uani 1.00 1 d . . . C(18) C 0.2143(3) 0.4091(2) 0.9211(3) 0.0207(8) Uani 1.00 1 d . . . C(19) C 0.3320(3) 0.4516(2) 0.9499(3) 0.0231(9) Uani 1.00 1 d . . . C(20) C 0.3508(4) 0.4641(3) 1.0612(3) 0.0291(10) Uani 1.00 1 d . . . C(21) C 0.3341(3) 0.3786(2) 1.1143(3) 0.0239(9) Uani 1.00 1 d . . . C(22) C 0.2178(3) 0.3359(2) 1.0807(2) 0.0171(7) Uani 1.00 1 d . . . C(23) C 0.3567(6) 0.0871(5) 0.2504(5) 0.0618(18) Uiso 1.00 1 d . . . C(24) C 0.448(3) 0.205(2) 0.402(3) 0.101(12) Uiso 0.25 1 d P . . C(25) C 0.4141(12) 0.1160(9) 0.4216(10) 0.095(3) Uiso 0.75 1 d P . . C(26) C 0.4395(10) 0.2036(8) 0.2788(9) 0.116(3) Uiso 1.00 1 d . . . H(1) H 0.1392 -0.0886 1.0911 0.018 Uiso 1.00 1 c R . . H(2) H -0.0043 -0.0758 1.1830 0.021 Uiso 1.00 1 c R . . H(3) H -0.0928 0.0430 1.2263 0.022 Uiso 1.00 1 c R . . H(4) H -0.0765 0.1775 1.1721 0.022 Uiso 1.00 1 c R . . H(5) H 0.0410 0.2293 1.0707 0.019 Uiso 1.00 1 c R . . H(6) H 0.3183 -0.0793 1.1345 0.019 Uiso 1.00 1 c R . . H(7) H 0.4462 -0.1157 1.1284 0.019 Uiso 1.00 1 c R . . H(8) H 0.2451 -0.2210 1.1408 0.027 Uiso 1.00 1 c R . . H(9) H 0.3510 -0.2111 1.2253 0.027 Uiso 1.00 1 c R . . H(10) H 0.3644 -0.3444 1.1359 0.026 Uiso 1.00 1 c R . . H(11) H 0.4757 -0.2841 1.1285 0.026 Uiso 1.00 1 c R . . H(12) H 0.4087 -0.3353 0.9695 0.027 Uiso 1.00 1 c R . . H(13) H 0.2820 -0.2980 0.9792 0.027 Uiso 1.00 1 c R . . H(14) H 0.4844 -0.1935 0.9675 0.025 Uiso 1.00 1 c R . . H(15) H 0.3778 -0.2010 0.8833 0.025 Uiso 1.00 1 c R . . H(16) H 0.2132 0.2783 1.1125 0.021 Uiso 1.00 1 c R . . H(17) H 0.1541 0.3726 1.0998 0.021 Uiso 1.00 1 c R . . H(18) H 0.3393 0.3897 1.1857 0.029 Uiso 1.00 1 c R . . H(19) H 0.3972 0.3380 1.1023 0.029 Uiso 1.00 1 c R . . H(20) H 0.4301 0.4862 1.0802 0.035 Uiso 1.00 1 c R . . H(21) H 0.2955 0.5079 1.0810 0.035 Uiso 1.00 1 c R . . H(22) H 0.3352 0.5087 0.9168 0.028 Uiso 1.00 1 c R . . H(23) H 0.3939 0.4143 0.9286 0.028 Uiso 1.00 1 c R . . H(24) H 0.1522 0.4486 0.9381 0.025 Uiso 1.00 1 c R . . H(25) H 0.2034 0.3993 0.8493 0.025 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.01433(8) 0.01456(8) 0.01060(7) -0.00308(6) 0.00274(5) -0.00015(6) Cl(1) 0.0252(4) 0.0220(4) 0.0141(4) -0.0047(3) 0.0075(3) 0.0005(3) S(1) 0.0203(4) 0.0164(4) 0.0142(4) -0.0008(3) 0.0060(3) -0.0004(3) S(2) 0.0229(4) 0.0158(4) 0.0139(4) -0.0021(3) 0.0047(3) 0.0024(3) N(1) 0.0173(15) 0.0170(16) 0.0136(15) 0.0027(13) 0.0020(13) -0.0024(13) N(2) 0.0163(15) 0.0134(15) 0.0166(15) -0.0014(13) 0.0015(12) 0.0001(13) C(1) 0.0094(15) 0.0159(18) 0.0128(16) -0.0019(14) 0.0009(13) -0.0016(14) C(2) 0.0132(16) 0.0153(18) 0.0123(17) -0.0008(14) 0.0005(14) -0.0018(14) C(3) 0.0130(16) 0.0171(18) 0.0102(16) -0.0021(14) -0.0009(13) -0.0010(14) C(4) 0.0135(16) 0.0137(17) 0.0102(16) -0.0035(14) -0.0036(14) -0.0010(14) C(5) 0.0158(17) 0.0171(19) 0.0139(17) -0.0003(15) -0.0003(14) -0.0025(15) C(6) 0.0129(16) 0.0147(18) 0.0111(16) -0.0007(14) -0.0006(13) 0.0005(14) C(7) 0.0109(16) 0.0187(19) 0.0126(17) -0.0023(14) 0.0006(14) -0.0031(15) C(8) 0.0166(18) 0.023(2) 0.0152(18) 0.0002(16) 0.0035(15) -0.0037(16) C(9) 0.0127(17) 0.028(2) 0.0143(18) -0.0041(16) 0.0035(14) -0.0008(16) C(10) 0.0159(18) 0.022(2) 0.0131(17) -0.0061(16) -0.0014(14) 0.0018(15) C(11) 0.0145(17) 0.0180(19) 0.0125(17) 0.0008(15) -0.0010(14) 0.0030(15) C(12) 0.025(2) 0.019(2) 0.0197(19) 0.0075(17) 0.0063(17) 0.0007(16) C(13) 0.0145(17) 0.0165(18) 0.0152(18) -0.0029(15) 0.0000(14) -0.0004(15) C(14) 0.024(2) 0.0163(19) 0.026(2) 0.0026(16) 0.0020(17) -0.0023(17) C(15) 0.025(2) 0.0160(19) 0.025(2) 0.0018(16) 0.0057(17) 0.0050(16) C(16) 0.024(2) 0.019(2) 0.025(2) 0.0006(17) 0.0073(17) 0.0050(17) C(17) 0.0157(17) 0.0169(18) 0.0148(18) -0.0010(15) 0.0015(15) 0.0016(15) C(18) 0.022(2) 0.0143(19) 0.026(2) -0.0003(16) 0.0040(17) 0.0035(16) C(19) 0.021(2) 0.0157(19) 0.034(2) -0.0059(16) 0.0088(18) 0.0013(18) C(20) 0.028(2) 0.023(2) 0.037(2) -0.0113(19) 0.006(2) -0.006(2) C(21) 0.023(2) 0.026(2) 0.022(2) -0.0066(17) 0.0000(17) -0.0063(17) C(22) 0.0195(18) 0.0142(18) 0.0181(19) -0.0028(15) 0.0041(15) -0.0049(15) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Pt(1) Cl(1) 2.4076(10) yes . . Pt(1) S(1) 2.3056(9) yes . . Pt(1) S(2) 2.3105(10) yes . . Pt(1) C(1) 1.910(3) yes . . S(1) C(7) 1.743(3) yes . . S(2) C(13) 1.755(4) yes . . O(1) C(23) 1.249(10) yes . . O(2) C(24) 1.46(4) yes . . O(2) C(26) 1.319(16) yes . . N(1) C(7) 1.336(5) yes . . N(1) C(12) 1.475(5) yes . . N(1) C(17) 1.486(4) yes . . N(2) C(13) 1.320(5) yes . . N(2) C(18) 1.478(5) yes . . N(2) C(22) 1.483(5) yes . . N(3) C(23) 1.349(9) yes . . N(3) C(24) 1.55(4) yes . . N(3) C(25) 1.500(15) yes . . N(3) C(26) 1.138(14) yes . . C(1) C(2) 1.410(5) yes . . C(1) C(6) 1.410(5) yes . . C(2) C(3) 1.426(5) yes . . C(2) C(7) 1.449(5) yes . . C(3) C(4) 1.496(5) yes . . C(3) C(11) 1.401(5) yes . . C(4) C(5) 1.391(5) yes . . C(4) C(6) 1.437(5) yes . . C(5) C(8) 1.393(5) yes . . C(6) C(13) 1.450(5) yes . . C(8) C(9) 1.390(6) yes . . C(9) C(10) 1.388(5) yes . . C(10) C(11) 1.398(5) yes . . C(12) C(14) 1.521(6) yes . . C(14) C(15) 1.535(6) yes . . C(15) C(16) 1.525(6) yes . . C(16) C(17) 1.518(5) yes . . C(18) C(19) 1.529(5) yes . . C(19) C(20) 1.531(6) yes . . C(20) C(21) 1.524(6) yes . . C(21) C(22) 1.529(5) yes . . C(24) C(25) 1.46(4) yes . . C(24) C(26) 1.68(4) yes . . C(5) H(5) 0.950 no . . C(8) H(4) 0.950 no . . C(9) H(3) 0.950 no . . C(10) H(2) 0.950 no . . C(11) H(1) 0.950 no . . C(12) H(14) 0.990 no . . C(12) H(15) 0.990 no . . C(14) H(12) 0.990 no . . C(14) H(13) 0.990 no . . C(15) H(10) 0.990 no . . C(15) H(11) 0.990 no . . C(16) H(8) 0.990 no . . C(16) H(9) 0.990 no . . C(17) H(6) 0.990 no . . C(17) H(7) 0.990 no . . C(18) H(24) 0.990 no . . C(18) H(25) 0.990 no . . C(19) H(22) 0.990 no . . C(19) H(23) 0.990 no . . C(20) H(20) 0.990 no . . C(20) H(21) 0.990 no . . C(21) H(18) 0.990 no . . C(21) H(19) 0.990 no . . C(22) H(16) 0.990 no . . C(22) H(17) 0.990 no . . 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Pt(1) S(1) 97.19(3) yes . . . Cl(1) Pt(1) S(2) 95.90(3) yes . . . Cl(1) Pt(1) C(1) 178.63(11) yes . . . S(1) Pt(1) S(2) 166.91(3) yes . . . S(1) Pt(1) C(1) 82.99(11) yes . . . S(2) Pt(1) C(1) 83.93(11) yes . . . Pt(1) S(1) C(7) 100.72(13) yes . . . Pt(1) S(2) C(13) 99.56(13) yes . . . C(24) O(2) C(26) 74.0(18) yes . . . C(7) N(1) C(12) 120.7(3) yes . . . C(7) N(1) C(17) 120.6(3) yes . . . C(12) N(1) C(17) 113.0(3) yes . . . C(13) N(2) C(18) 122.2(3) yes . . . C(13) N(2) C(22) 123.0(3) yes . . . C(18) N(2) C(22) 112.2(3) yes . . . C(23) N(3) C(24) 163.9(17) yes . . . C(23) N(3) C(25) 115.4(7) yes . . . C(23) N(3) C(26) 110.6(8) yes . . . C(24) N(3) C(25) 57.2(17) yes . . . C(24) N(3) C(26) 75.5(17) yes . . . C(25) N(3) C(26) 132.7(9) yes . . . Pt(1) C(1) C(2) 125.3(2) yes . . . Pt(1) C(1) C(6) 124.2(2) yes . . . C(2) C(1) C(6) 109.8(3) yes . . . C(1) C(2) C(3) 107.8(3) yes . . . C(1) C(2) C(7) 114.4(3) yes . . . C(3) C(2) C(7) 137.1(3) yes . . . C(2) C(3) C(4) 107.0(3) yes . . . C(2) C(3) C(11) 126.4(3) yes . . . C(4) C(3) C(11) 126.0(3) yes . . . C(3) C(4) C(5) 127.0(3) yes . . . C(3) C(4) C(6) 106.0(3) yes . . . C(5) C(4) C(6) 126.4(3) yes . . . C(4) C(5) C(8) 129.8(3) yes . . . C(1) C(6) C(4) 108.0(3) yes . . . C(1) C(6) C(13) 115.0(3) yes . . . C(4) C(6) C(13) 136.4(3) yes . . . S(1) C(7) N(1) 119.0(2) yes . . . S(1) C(7) C(2) 115.3(2) yes . . . N(1) C(7) C(2) 125.5(3) yes . . . C(5) C(8) C(9) 129.3(3) yes . . . C(8) C(9) C(10) 128.5(3) yes . . . C(9) C(10) C(11) 129.2(3) yes . . . C(3) C(11) C(10) 129.9(3) yes . . . N(1) C(12) C(14) 110.7(3) yes . . . S(2) C(13) N(2) 119.6(3) yes . . . S(2) C(13) C(6) 115.0(2) yes . . . N(2) C(13) C(6) 125.2(3) yes . . . C(12) C(14) C(15) 111.3(3) yes . . . C(14) C(15) C(16) 109.7(3) yes . . . C(15) C(16) C(17) 110.6(3) yes . . . N(1) C(17) C(16) 111.9(3) yes . . . N(2) C(18) C(19) 110.5(3) yes . . . C(18) C(19) C(20) 109.7(3) yes . . . C(19) C(20) C(21) 110.9(3) yes . . . C(20) C(21) C(22) 112.4(3) yes . . . N(2) C(22) C(21) 109.2(3) yes . . . O(1) C(23) N(3) 101.2(6) yes . . . O(2) C(24) N(3) 90(2) yes . . . O(2) C(24) C(25) 150(3) yes . . . O(2) C(24) C(26) 49.1(14) yes . . . N(3) C(24) C(25) 59.7(17) yes . . . N(3) C(24) C(26) 41.0(11) yes . . . C(25) C(24) C(26) 101(2) yes . . . N(3) C(25) C(24) 63.1(18) yes . . . O(2) C(26) N(3) 120.3(11) yes . . . O(2) C(26) C(24) 56.9(16) yes . . . N(3) C(26) C(24) 63.4(16) yes . . . C(4) C(5) H(5) 115.1 no . . . C(8) C(5) H(5) 115.1 no . . . C(5) C(8) H(4) 115.3 no . . . C(9) C(8) H(4) 115.3 no . . . C(8) C(9) H(3) 115.8 no . . . C(10) C(9) H(3) 115.8 no . . . C(9) C(10) H(2) 115.4 no . . . C(11) C(10) H(2) 115.4 no . . . C(3) C(11) H(1) 115.0 no . . . C(10) C(11) H(1) 115.0 no . . . N(1) C(12) H(14) 109.5 no . . . N(1) C(12) H(15) 109.5 no . . . C(14) C(12) H(14) 109.5 no . . . C(14) C(12) H(15) 109.5 no . . . H(14) C(12) H(15) 108.1 no . . . C(12) C(14) H(12) 109.4 no . . . C(12) C(14) H(13) 109.4 no . . . C(15) C(14) H(12) 109.4 no . . . C(15) C(14) H(13) 109.4 no . . . H(12) C(14) H(13) 108.0 no . . . C(14) C(15) H(10) 109.7 no . . . C(14) C(15) H(11) 109.7 no . . . C(16) C(15) H(10) 109.7 no . . . C(16) C(15) H(11) 109.7 no . . . H(10) C(15) H(11) 108.2 no . . . C(15) C(16) H(8) 109.5 no . . . C(15) C(16) H(9) 109.5 no . . . C(17) C(16) H(8) 109.5 no . . . C(17) C(16) H(9) 109.5 no . . . H(8) C(16) H(9) 108.1 no . . . N(1) C(17) H(6) 109.2 no . . . N(1) C(17) H(7) 109.2 no . . . C(16) C(17) H(6) 109.2 no . . . C(16) C(17) H(7) 109.2 no . . . H(6) C(17) H(7) 107.9 no . . . N(2) C(18) H(24) 109.6 no . . . N(2) C(18) H(25) 109.5 no . . . C(19) C(18) H(24) 109.5 no . . . C(19) C(18) H(25) 109.5 no . . . H(24) C(18) H(25) 108.1 no . . . C(18) C(19) H(22) 109.7 no . . . C(18) C(19) H(23) 109.7 no . . . C(20) C(19) H(22) 109.7 no . . . C(20) C(19) H(23) 109.7 no . . . H(22) C(19) H(23) 108.2 no . . . C(19) C(20) H(20) 109.5 no . . . C(19) C(20) H(21) 109.5 no . . . C(21) C(20) H(20) 109.5 no . . . C(21) C(20) H(21) 109.5 no . . . H(20) C(20) H(21) 108.1 no . . . C(20) C(21) H(18) 109.1 no . . . C(20) C(21) H(19) 109.1 no . . . C(22) C(21) H(18) 109.1 no . . . C(22) C(21) H(19) 109.1 no . . . H(18) C(21) H(19) 107.9 no . . . N(2) C(22) H(16) 109.8 no . . . N(2) C(22) H(17) 109.8 no . . . C(21) C(22) H(16) 109.8 no . . . C(21) C(22) H(17) 109.8 no . . . H(16) C(22) H(17) 108.3 no . . . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Pt(1) S(1) C(7) 178.18(12) ? . . . . Cl(1) Pt(1) S(2) C(13) -173.36(12) ? . . . . Cl(1) Pt(1) C(1) C(2) -104(4) ? . . . . Cl(1) Pt(1) C(1) C(6) 86(4) ? . . . . S(1) Pt(1) S(2) C(13) 6.2(2) ? . . . . S(2) Pt(1) S(1) C(7) -1.4(2) ? . . . . S(1) Pt(1) C(1) C(2) -6.8(2) ? . . . . S(1) Pt(1) C(1) C(6) -176.4(3) ? . . . . C(1) Pt(1) S(1) C(7) -0.45(16) ? . . . . S(2) Pt(1) C(1) C(2) 173.0(3) ? . . . . S(2) Pt(1) C(1) C(6) 3.4(2) ? . . . . C(1) Pt(1) S(2) C(13) 5.27(16) ? . . . . Pt(1) S(1) C(7) N(1) -169.6(2) ? . . . . Pt(1) S(1) C(7) C(2) 6.8(2) ? . . . . Pt(1) S(2) C(13) N(2) 162.5(2) ? . . . . Pt(1) S(2) C(13) C(6) -13.4(2) ? . . . . C(24) O(2) C(26) N(3) 0.3(19) ? . . . . C(26) O(2) C(24) N(3) -0.2(12) ? . . . . C(26) O(2) C(24) C(25) 2(3) ? . . . . C(7) N(1) C(12) C(14) -151.2(3) ? . . . . C(12) N(1) C(7) S(1) -7.9(4) ? . . . . C(12) N(1) C(7) C(2) 176.1(3) ? . . . . C(7) N(1) C(17) C(16) 151.1(3) ? . . . . C(17) N(1) C(7) S(1) 143.5(3) ? . . . . C(17) N(1) C(7) C(2) -32.5(5) ? . . . . C(12) N(1) C(17) C(16) -55.4(4) ? . . . . C(17) N(1) C(12) C(14) 55.3(4) ? . . . . C(13) N(2) C(18) C(19) -100.9(4) ? . . . . C(18) N(2) C(13) S(2) 8.0(4) ? . . . . C(18) N(2) C(13) C(6) -176.6(3) ? . . . . C(13) N(2) C(22) C(21) 103.3(4) ? . . . . C(22) N(2) C(13) S(2) -152.2(2) ? . . . . C(22) N(2) C(13) C(6) 23.2(5) ? . . . . C(18) N(2) C(22) C(21) -58.6(4) ? . . . . C(22) N(2) C(18) C(19) 61.2(4) ? . . . . C(23) N(3) C(24) O(2) -114(5) ? . . . . C(23) N(3) C(24) C(25) 67(6) ? . . . . C(23) N(3) C(24) C(26) -115(5) ? . . . . C(24) N(3) C(23) O(1) -88(6) ? . . . . C(23) N(3) C(25) C(24) -164(2) ? . . . . C(25) N(3) C(23) O(1) -29.0(10) ? . . . . C(23) N(3) C(26) O(2) 164.1(10) ? . . . . C(23) N(3) C(26) C(24) 164.4(17) ? . . . . C(26) N(3) C(23) O(1) 162.4(9) ? . . . . C(25) N(3) C(24) O(2) 178.9(12) ? . . . . C(25) N(3) C(24) C(26) 178.6(17) ? . . . . C(24) N(3) C(26) O(2) -0.3(18) ? . . . . C(26) N(3) C(24) O(2) 0.2(14) ? . . . . C(26) N(3) C(24) C(25) -178.6(17) ? . . . . C(25) N(3) C(26) O(2) -1.9(19) ? . . . . C(25) N(3) C(26) C(24) -2(2) ? . . . . C(26) N(3) C(25) C(24) 2(2) ? . . . . Pt(1) C(1) C(2) C(3) -159.3(2) ? . . . . Pt(1) C(1) C(2) C(7) 13.0(4) ? . . . . Pt(1) C(1) C(6) C(4) 159.9(2) ? . . . . Pt(1) C(1) C(6) C(13) -13.2(4) ? . . . . C(2) C(1) C(6) C(4) -11.1(4) ? . . . . C(2) C(1) C(6) C(13) 175.8(3) ? . . . . C(6) C(1) C(2) C(3) 11.6(4) ? . . . . C(6) C(1) C(2) C(7) -176.1(3) ? . . . . C(1) C(2) C(3) C(4) -7.4(3) ? . . . . C(1) C(2) C(3) C(11) 164.0(3) ? . . . . C(1) C(2) C(7) S(1) -12.1(4) ? . . . . C(1) C(2) C(7) N(1) 164.0(3) ? . . . . C(3) C(2) C(7) S(1) 157.0(3) ? . . . . C(3) C(2) C(7) N(1) -26.8(6) ? . . . . C(7) C(2) C(3) C(4) -177.0(3) ? . . . . C(7) C(2) C(3) C(11) -5.6(6) ? . . . . C(2) C(3) C(4) C(5) 171.9(3) ? . . . . C(2) C(3) C(4) C(6) 0.8(3) ? . . . . C(2) C(3) C(11) C(10) -173.7(3) ? . . . . C(4) C(3) C(11) C(10) -3.8(6) ? . . . . C(11) C(3) C(4) C(5) 0.5(5) ? . . . . C(11) C(3) C(4) C(6) -170.7(3) ? . . . . C(3) C(4) C(5) C(8) 4.7(6) ? . . . . C(3) C(4) C(6) C(1) 6.2(3) ? . . . . C(3) C(4) C(6) C(13) 177.1(3) ? . . . . C(5) C(4) C(6) C(1) -165.1(3) ? . . . . C(5) C(4) C(6) C(13) 5.8(6) ? . . . . C(6) C(4) C(5) C(8) 174.2(3) ? . . . . C(4) C(5) C(8) C(9) -3.5(6) ? . . . . C(1) C(6) C(13) S(2) 17.5(4) ? . . . . C(1) C(6) C(13) N(2) -158.1(3) ? . . . . C(4) C(6) C(13) S(2) -153.0(3) ? . . . . C(4) C(6) C(13) N(2) 31.5(6) ? . . . . C(5) C(8) C(9) C(10) -2.9(6) ? . . . . C(8) C(9) C(10) C(11) 4.9(6) ? . . . . C(9) C(10) C(11) C(3) 0.1(5) ? . . . . N(1) C(12) C(14) C(15) -55.9(4) ? . . . . C(12) C(14) C(15) C(16) 56.2(4) ? . . . . C(14) C(15) C(16) C(17) -55.2(4) ? . . . . C(15) C(16) C(17) N(1) 55.0(4) ? . . . . N(2) C(18) C(19) C(20) -57.3(4) ? . . . . C(18) C(19) C(20) C(21) 53.6(4) ? . . . . C(19) C(20) C(21) C(22) -53.4(4) ? . . . . C(20) C(21) C(22) N(2) 54.6(4) ? . . . . O(2) C(24) C(25) N(3) -2(2) ? . . . . O(2) C(24) C(26) N(3) -179.7(18) ? . . . . N(3) C(24) C(26) O(2) 179.7(18) ? . . . . C(25) C(24) C(26) O(2) -179.1(16) ? . . . . C(25) C(24) C(26) N(3) 1.2(15) ? . . . . C(26) C(24) C(25) N(3) -0.9(11) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) O(1) 3.310(6) ? . 3_656 Cl(1) C(25) 3.208(14) ? . . S(1) C(23) 3.591(7) ? . 3_656 S(2) O(2) 3.492(9) ? . 4_455 O(1) Cl(1) 3.310(6) ? . 3_656 O(1) C(17) 3.377(7) ? . 1_554 O(1) C(20) 3.460(8) ? . 2_546 O(1) C(21) 3.474(8) ? . 2_546 O(1) C(22) 3.447(7) ? . 2_546 O(2) S(2) 3.492(9) ? . 4_554 O(2) N(2) 3.499(9) ? . 4_554 O(2) C(6) 3.321(10) ? . 4_554 O(2) C(10) 3.142(11) ? . 2_556 O(2) C(11) 3.343(10) ? . 2_556 O(2) C(13) 3.065(10) ? . 4_554 O(2) C(16) 3.550(10) ? . 2_556 N(2) O(2) 3.499(9) ? . 4_455 N(2) C(24) 3.08(4) ? . 4_455 N(2) C(25) 3.512(14) ? . 4_455 C(1) C(10) 3.599(5) ? . 3_557 C(2) C(9) 3.375(5) ? . 3_557 C(2) C(10) 3.551(5) ? . 3_557 C(3) C(10) 3.395(5) ? . 3_557 C(3) C(23) 3.424(8) ? . 1_556 C(4) C(10) 3.537(5) ? . 3_557 C(5) C(24) 3.30(4) ? . 4_455 C(6) O(2) 3.321(10) ? . 4_455 C(7) C(9) 3.540(5) ? . 3_557 C(9) C(2) 3.375(5) ? . 3_557 C(9) C(7) 3.540(5) ? . 3_557 C(10) O(2) 3.142(11) ? . 2_546 C(10) C(1) 3.599(5) ? . 3_557 C(10) C(2) 3.551(5) ? . 3_557 C(10) C(3) 3.395(5) ? . 3_557 C(10) C(4) 3.537(5) ? . 3_557 C(11) O(2) 3.343(10) ? . 2_546 C(13) O(2) 3.065(10) ? . 4_455 C(13) C(24) 3.22(4) ? . 4_455 C(16) O(2) 3.550(10) ? . 2_546 C(16) C(24) 3.48(4) ? . 2_546 C(17) O(1) 3.377(7) ? . 1_556 C(18) C(24) 3.54(4) ? . 4_455 C(18) C(25) 3.515(14) ? . 4_455 C(20) O(1) 3.460(8) ? . 2_556 C(21) O(1) 3.474(8) ? . 2_556 C(22) O(1) 3.447(7) ? . 2_556 C(23) S(1) 3.591(7) ? . 3_656 C(23) C(3) 3.424(8) ? . 1_554 C(24) N(2) 3.08(4) ? . 4_554 C(24) C(5) 3.30(4) ? . 4_554 C(24) C(13) 3.22(4) ? . 4_554 C(24) C(16) 3.48(4) ? . 2_556 C(24) C(18) 3.54(4) ? . 4_554 C(25) Cl(1) 3.208(14) ? . . C(25) N(2) 3.512(14) ? . 4_554 C(25) C(18) 3.515(14) ? . 4_554 Pt(1) H(3) 3.545 ? . 3_557 Pt(1) H(7) 2.680 ? . 3_657 Cl(1) H(4) 3.176 ? . 4_554 Cl(1) H(5) 3.104 ? . 4_554 Cl(1) H(7) 3.238 ? . 3_657 Cl(1) H(9) 3.387 ? . 3_657 Cl(1) H(13) 3.042 ? . 2_556 Cl(1) H(17) 3.014 ? . 4_554 Cl(1) H(22) 3.359 ? . 2_546 Cl(1) H(24) 2.934 ? . 2_546 Cl(1) H(25) 3.587 ? . 2_546 S(1) H(3) 3.249 ? . 3_557 S(1) H(7) 3.209 ? . 3_657 S(1) H(25) 2.765 ? . 2_546 S(2) H(4) 3.010 ? . 4_554 S(2) H(11) 3.057 ? . 3_657 S(2) H(15) 3.110 ? . 2_556 O(1) H(6) 2.660 ? . 1_554 O(1) H(7) 3.272 ? . 1_554 O(1) H(17) 2.658 ? . 2_546 O(1) H(18) 3.114 ? . 2_546 O(1) H(21) 2.668 ? . 2_546 O(2) H(1) 2.763 ? . 2_556 O(2) H(2) 2.367 ? . 2_556 O(2) H(5) 3.287 ? . 4_554 O(2) H(8) 2.600 ? . 2_556 O(2) H(18) 2.991 ? . 1_554 O(2) H(19) 3.326 ? . 1_554 N(3) H(8) 2.925 ? . 2_556 N(3) H(10) 3.396 ? . 2_556 N(3) H(21) 3.596 ? . 2_546 N(3) H(24) 3.360 ? . 4_554 N(3) H(25) 3.392 ? . 4_554 C(1) H(2) 3.275 ? . 3_557 C(1) H(3) 3.508 ? . 3_557 C(1) H(7) 3.548 ? . 3_657 C(1) H(14) 3.426 ? . 3_657 C(2) H(3) 3.397 ? . 3_557 C(3) H(2) 3.594 ? . 3_557 C(4) H(2) 3.422 ? . 3_557 C(5) H(1) 3.342 ? . 3_557 C(5) H(9) 3.269 ? . 2_557 C(6) H(2) 3.311 ? . 3_557 C(7) H(3) 3.359 ? . 3_557 C(8) H(1) 3.484 ? . 3_557 C(8) H(9) 3.439 ? . 2_557 C(8) H(10) 3.332 ? . 2_557 C(8) H(11) 3.284 ? . 2_557 C(9) H(10) 3.433 ? . 2_557 C(9) H(20) 3.515 ? . 2_547 C(10) H(18) 2.888 ? . 2_547 C(10) H(20) 3.594 ? . 2_547 C(11) H(18) 3.194 ? . 2_547 C(12) H(19) 3.324 ? . 3_657 C(14) H(19) 3.307 ? . 3_657 C(14) H(21) 3.468 ? . 1_545 C(14) H(22) 3.323 ? . 1_545 C(14) H(23) 3.465 ? . 3_657 C(15) H(4) 3.526 ? . 2_547 C(15) H(20) 3.514 ? . 1_545 C(15) H(21) 3.324 ? . 1_545 C(15) H(23) 3.244 ? . 3_657 C(16) H(16) 3.306 ? . 2_547 C(16) H(18) 3.490 ? . 2_547 C(19) H(3) 3.281 ? . 4_554 C(19) H(12) 3.395 ? . 1_565 C(19) H(12) 3.575 ? . 3_657 C(19) H(20) 3.000 ? . 3_667 C(20) H(10) 3.113 ? . 1_565 C(20) H(12) 3.422 ? . 1_565 C(20) H(12) 3.489 ? . 3_657 C(20) H(20) 3.455 ? . 3_667 C(20) H(23) 3.498 ? . 3_667 C(21) H(2) 3.305 ? . 2_557 C(21) H(9) 3.525 ? . 2_557 C(21) H(12) 3.387 ? . 3_657 C(22) H(9) 2.952 ? . 2_557 C(23) H(6) 3.017 ? . 1_554 C(23) H(8) 3.564 ? . 2_556 C(23) H(10) 3.323 ? . 2_556 C(23) H(21) 3.295 ? . 2_546 C(24) H(1) 3.332 ? . 2_556 C(24) H(5) 2.645 ? . 4_554 C(24) H(8) 2.531 ? . 2_556 C(24) H(13) 3.289 ? . 2_556 C(24) H(24) 3.344 ? . 4_554 C(24) H(25) 3.516 ? . 4_554 C(25) H(5) 3.368 ? . 4_554 C(25) H(8) 3.175 ? . 2_556 C(25) H(10) 3.306 ? . 2_556 C(25) H(13) 3.079 ? . 2_556 C(25) H(17) 3.506 ? . 4_554 C(25) H(21) 2.946 ? . 2_546 C(25) H(24) 3.351 ? . 2_546 C(25) H(24) 2.928 ? . 4_554 C(26) H(2) 3.497 ? . 2_556 C(26) H(8) 2.774 ? . 2_556 C(26) H(14) 3.590 ? . 3_656 C(26) H(15) 3.242 ? . 3_656 C(26) H(16) 3.482 ? . 1_554 C(26) H(18) 3.291 ? . 1_554 C(26) H(19) 3.179 ? . 1_554 C(26) H(25) 3.493 ? . 4_554 H(1) O(2) 2.763 ? . 2_546 H(1) C(5) 3.342 ? . 3_557 H(1) C(8) 3.484 ? . 3_557 H(1) C(24) 3.332 ? . 2_546 H(1) H(18) 3.061 ? . 2_547 H(2) O(2) 2.367 ? . 2_546 H(2) C(1) 3.275 ? . 3_557 H(2) C(3) 3.594 ? . 3_557 H(2) C(4) 3.422 ? . 3_557 H(2) C(6) 3.311 ? . 3_557 H(2) C(21) 3.305 ? . 2_547 H(2) C(26) 3.497 ? . 2_546 H(2) H(18) 2.538 ? . 2_547 H(2) H(19) 3.341 ? . 2_547 H(2) H(20) 3.403 ? . 2_547 H(3) Pt(1) 3.545 ? . 3_557 H(3) S(1) 3.249 ? . 3_557 H(3) C(1) 3.508 ? . 3_557 H(3) C(2) 3.397 ? . 3_557 H(3) C(7) 3.359 ? . 3_557 H(3) C(19) 3.281 ? . 4_455 H(3) H(10) 3.537 ? . 2_557 H(3) H(11) 3.503 ? . 2_557 H(3) H(20) 3.206 ? . 2_547 H(3) H(22) 2.939 ? . 4_455 H(3) H(23) 2.872 ? . 4_455 H(3) H(25) 3.184 ? . 4_455 H(4) Cl(1) 3.176 ? . 4_455 H(4) S(2) 3.010 ? . 4_455 H(4) C(15) 3.526 ? . 2_557 H(4) H(9) 3.312 ? . 2_557 H(4) H(10) 3.420 ? . 2_557 H(4) H(11) 2.914 ? . 2_557 H(4) H(13) 3.515 ? . 3_557 H(4) H(15) 3.523 ? . 3_557 H(5) Cl(1) 3.104 ? . 4_455 H(5) O(2) 3.287 ? . 4_455 H(5) C(24) 2.645 ? . 4_455 H(5) C(25) 3.368 ? . 4_455 H(5) H(9) 3.076 ? . 2_557 H(6) O(1) 2.660 ? . 1_556 H(6) C(23) 3.017 ? . 1_556 H(6) H(18) 3.266 ? . 2_547 H(7) Pt(1) 2.680 ? . 3_657 H(7) Cl(1) 3.238 ? . 3_657 H(7) S(1) 3.209 ? . 3_657 H(7) O(1) 3.272 ? . 1_556 H(7) C(1) 3.548 ? . 3_657 H(8) O(2) 2.600 ? . 2_546 H(8) N(3) 2.925 ? . 2_546 H(8) C(23) 3.564 ? . 2_546 H(8) C(24) 2.531 ? . 2_546 H(8) C(25) 3.175 ? . 2_546 H(8) C(26) 2.774 ? . 2_546 H(8) H(16) 3.364 ? . 2_547 H(8) H(18) 3.168 ? . 2_547 H(9) Cl(1) 3.387 ? . 3_657 H(9) C(5) 3.269 ? . 2_547 H(9) C(8) 3.439 ? . 2_547 H(9) C(21) 3.525 ? . 2_547 H(9) C(22) 2.952 ? . 2_547 H(9) H(4) 3.312 ? . 2_547 H(9) H(5) 3.076 ? . 2_547 H(9) H(16) 2.429 ? . 2_547 H(9) H(17) 2.728 ? . 2_547 H(9) H(18) 3.064 ? . 2_547 H(10) N(3) 3.396 ? . 2_546 H(10) C(8) 3.332 ? . 2_547 H(10) C(9) 3.433 ? . 2_547 H(10) C(20) 3.113 ? . 1_545 H(10) C(23) 3.323 ? . 2_546 H(10) C(25) 3.306 ? . 2_546 H(10) H(3) 3.537 ? . 2_547 H(10) H(4) 3.420 ? . 2_547 H(10) H(20) 2.840 ? . 1_545 H(10) H(21) 2.494 ? . 1_545 H(10) H(23) 3.223 ? . 3_657 H(11) S(2) 3.057 ? . 3_657 H(11) C(8) 3.284 ? . 2_547 H(11) H(3) 3.503 ? . 2_547 H(11) H(4) 2.914 ? . 2_547 H(11) H(23) 2.678 ? . 3_657 H(12) C(19) 3.395 ? . 1_545 H(12) C(19) 3.575 ? . 3_657 H(12) C(20) 3.422 ? . 1_545 H(12) C(20) 3.489 ? . 3_657 H(12) C(21) 3.387 ? . 3_657 H(12) H(19) 2.561 ? . 3_657 H(12) H(20) 3.130 ? . 1_545 H(12) H(20) 3.104 ? . 3_657 H(12) H(21) 3.212 ? . 1_545 H(12) H(22) 2.618 ? . 1_545 H(12) H(23) 2.826 ? . 3_657 H(13) Cl(1) 3.042 ? . 2_546 H(13) C(24) 3.289 ? . 2_546 H(13) C(25) 3.079 ? . 2_546 H(13) H(4) 3.515 ? . 3_557 H(13) H(21) 3.287 ? . 1_545 H(13) H(22) 3.170 ? . 1_545 H(14) C(1) 3.426 ? . 3_657 H(14) C(26) 3.590 ? . 3_656 H(14) H(19) 2.834 ? . 3_657 H(15) S(2) 3.110 ? . 2_546 H(15) C(26) 3.242 ? . 3_656 H(15) H(4) 3.523 ? . 3_557 H(15) H(19) 3.348 ? . 3_657 H(15) H(25) 3.575 ? . 2_546 H(16) C(16) 3.306 ? . 2_557 H(16) C(26) 3.482 ? . 1_556 H(16) H(8) 3.364 ? . 2_557 H(16) H(9) 2.429 ? . 2_557 H(17) Cl(1) 3.014 ? . 4_455 H(17) O(1) 2.658 ? . 2_556 H(17) C(25) 3.506 ? . 4_455 H(17) H(9) 2.728 ? . 2_557 H(18) O(1) 3.114 ? . 2_556 H(18) O(2) 2.991 ? . 1_556 H(18) C(10) 2.888 ? . 2_557 H(18) C(11) 3.194 ? . 2_557 H(18) C(16) 3.490 ? . 2_557 H(18) C(26) 3.291 ? . 1_556 H(18) H(1) 3.061 ? . 2_557 H(18) H(2) 2.538 ? . 2_557 H(18) H(6) 3.266 ? . 2_557 H(18) H(8) 3.168 ? . 2_557 H(18) H(9) 3.064 ? . 2_557 H(19) O(2) 3.326 ? . 1_556 H(19) C(12) 3.324 ? . 3_657 H(19) C(14) 3.307 ? . 3_657 H(19) C(26) 3.179 ? . 1_556 H(19) H(2) 3.341 ? . 2_557 H(19) H(12) 2.561 ? . 3_657 H(19) H(14) 2.834 ? . 3_657 H(19) H(15) 3.348 ? . 3_657 H(20) C(9) 3.515 ? . 2_557 H(20) C(10) 3.594 ? . 2_557 H(20) C(15) 3.514 ? . 1_565 H(20) C(19) 3.000 ? . 3_667 H(20) C(20) 3.455 ? . 3_667 H(20) H(2) 3.403 ? . 2_557 H(20) H(3) 3.206 ? . 2_557 H(20) H(10) 2.840 ? . 1_565 H(20) H(12) 3.130 ? . 1_565 H(20) H(12) 3.104 ? . 3_657 H(20) H(20) 2.909 ? . 3_667 H(20) H(22) 2.728 ? . 3_667 H(20) H(23) 2.569 ? . 3_667 H(21) O(1) 2.668 ? . 2_556 H(21) N(3) 3.596 ? . 2_556 H(21) C(14) 3.468 ? . 1_565 H(21) C(15) 3.324 ? . 1_565 H(21) C(23) 3.295 ? . 2_556 H(21) C(25) 2.946 ? . 2_556 H(21) H(10) 2.494 ? . 1_565 H(21) H(12) 3.212 ? . 1_565 H(21) H(13) 3.287 ? . 1_565 H(22) Cl(1) 3.359 ? . 2_556 H(22) C(14) 3.323 ? . 1_565 H(22) H(3) 2.939 ? . 4_554 H(22) H(12) 2.618 ? . 1_565 H(22) H(13) 3.170 ? . 1_565 H(22) H(20) 2.728 ? . 3_667 H(23) C(14) 3.465 ? . 3_657 H(23) C(15) 3.244 ? . 3_657 H(23) C(20) 3.498 ? . 3_667 H(23) H(3) 2.872 ? . 4_554 H(23) H(10) 3.223 ? . 3_657 H(23) H(11) 2.678 ? . 3_657 H(23) H(12) 2.826 ? . 3_657 H(23) H(20) 2.569 ? . 3_667 H(24) Cl(1) 2.934 ? . 2_556 H(24) N(3) 3.360 ? . 4_455 H(24) C(24) 3.344 ? . 4_455 H(24) C(25) 3.351 ? . 2_556 H(24) C(25) 2.928 ? . 4_455 H(25) Cl(1) 3.587 ? . 2_556 H(25) S(1) 2.765 ? . 2_556 H(25) N(3) 3.392 ? . 4_455 H(25) C(24) 3.516 ? . 4_455 H(25) C(26) 3.493 ? . 4_455 H(25) H(3) 3.184 ? . 4_554 H(25) H(15) 3.575 ? . 2_556 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '5CIF.cif' data_SNSPdmune2 _database_code_depnum_ccdc_archive 'CCDC 750105' #TrackingRef '5CIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C16 H22 Cl N3 Pd S2 ' _chemical_formula_moiety 'C16 H22 Cl N3 Pd S2 ' _chemical_formula_weight 462.34 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 9.4925(5) _cell_length_b 10.1758(4) _cell_length_c 10.9510(4) _cell_angle_alpha 61.6480(10) _cell_angle_beta 73.5321(17) _cell_angle_gamma 85.2855(17) _cell_volume 891.00(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7754 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 93.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468.00 _exptl_absorpt_coefficient_mu 1.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.752 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 8856 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4033 _reflns_number_gt 3602 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0548 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 4033 _refine_ls_number_parameters 207 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0135P)^2^+1.0507P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.60 _refine_diff_density_min -0.55 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.999 1.007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Pd(1) Pd 0.80930(2) 1.146995(19) 0.112012(19) 0.01199(5) Uani 1.00 1 d . . . Cl(1) Cl 0.66083(7) 1.34612(6) 0.03876(6) 0.01881(12) Uani 1.00 1 d . . . S(1) S 0.6805(2) 0.9926(2) 0.0775(2) 0.0125(6) Uiso 0.50 1 d P . . S(2) S 0.9629(2) 1.2560(2) 0.1774(2) 0.0119(6) Uiso 0.50 1 d P . . S(3) S 0.6704(2) 0.9823(2) 0.0972(2) 0.0142(7) Uiso 0.50 1 d P . . S(4) S 0.9706(2) 1.2630(2) 0.1547(2) 0.0122(6) Uiso 0.50 1 d P . . N(1) N 0.7380(2) 0.7105(2) 0.1417(2) 0.0153(4) Uani 1.00 1 d . . . N(2) N 1.2105(2) 1.1436(2) 0.2354(2) 0.0138(3) Uani 1.00 1 d . . . N(3) N 0.9322(2) 0.9793(2) 0.1740(2) 0.0126(3) Uani 1.00 1 d . . . C(1) C 0.9993(2) 0.7437(2) 0.2674(2) 0.0184(4) Uani 1.00 1 d . . . C(2) C 0.9012(2) 0.8405(2) 0.1948(2) 0.0143(4) Uani 1.00 1 d . . . C(3) C 1.0899(2) 0.8272(2) 0.2869(2) 0.0179(4) Uani 1.00 1 d . . . C(4) C 0.8074(2) 0.5670(2) 0.1961(2) 0.0183(4) Uani 1.00 1 d . . . C(5) C 0.7151(3) 0.4643(2) 0.3495(2) 0.0211(5) Uani 1.00 1 d . . . C(6) C 1.0476(2) 0.9764(2) 0.2253(2) 0.0134(4) Uani 1.00 1 d . . . C(7) C 0.7771(2) 0.8304(2) 0.1452(2) 0.0134(4) Uani 1.00 1 d . . . C(8) C 0.5582(3) 0.4434(2) 0.3476(2) 0.0233(5) Uani 1.00 1 d . . . C(9) C 0.4915(2) 0.5925(2) 0.2700(2) 0.0213(5) Uani 1.00 1 d . . . C(10) C 0.5958(2) 0.6918(2) 0.1210(2) 0.0177(4) Uani 1.00 1 d . . . C(11) C 1.3258(2) 1.0374(2) 0.2674(2) 0.0197(5) Uani 1.00 1 d . . . C(12) C 1.3153(3) 0.9681(2) 0.4267(3) 0.0286(6) Uani 1.00 1 d . . . C(13) C 1.0878(2) 1.1180(2) 0.2133(2) 0.0130(4) Uani 1.00 1 d . . . C(14) C 1.3345(3) 1.0916(3) 0.4633(3) 0.0318(6) Uani 1.00 1 d . . . C(15) C 1.2278(3) 1.2129(3) 0.4144(2) 0.0272(6) Uani 1.00 1 d . . . C(16) C 1.2374(2) 1.2722(2) 0.2549(2) 0.0183(4) Uani 1.00 1 d . . . H(1) H 1.0023 0.6395 0.2975 0.022 Uiso 1.00 1 c R . . H(2) H 1.1663 0.7912 0.3329 0.021 Uiso 1.00 1 c R . . H(3) H 0.9088 0.5830 0.1963 0.022 Uiso 1.00 1 c R . . H(4) H 0.8125 0.5209 0.1333 0.022 Uiso 1.00 1 c R . . H(5) H 0.7136 0.5089 0.4129 0.025 Uiso 1.00 1 c R . . H(6) H 0.7589 0.3661 0.3881 0.025 Uiso 1.00 1 c R . . H(7) H 0.4956 0.3877 0.4483 0.028 Uiso 1.00 1 c R . . H(8) H 0.5588 0.3826 0.2988 0.028 Uiso 1.00 1 c R . . H(9) H 0.3965 0.5733 0.2589 0.026 Uiso 1.00 1 c R . . H(10) H 0.4721 0.6450 0.3290 0.026 Uiso 1.00 1 c R . . H(11) H 0.6088 0.6445 0.0581 0.021 Uiso 1.00 1 c R . . H(12) H 0.5547 0.7904 0.0747 0.021 Uiso 1.00 1 c R . . H(13) H 1.4238 1.0900 0.2089 0.024 Uiso 1.00 1 c R . . H(14) H 1.3134 0.9583 0.2424 0.024 Uiso 1.00 1 c R . . H(15) H 1.3928 0.8962 0.4495 0.034 Uiso 1.00 1 c R . . H(16) H 1.2183 0.9132 0.4851 0.034 Uiso 1.00 1 c R . . H(17) H 1.3176 1.0481 0.5690 0.038 Uiso 1.00 1 c R . . H(18) H 1.4367 1.1363 0.4155 0.038 Uiso 1.00 1 c R . . H(19) H 1.2501 1.2964 0.4297 0.033 Uiso 1.00 1 c R . . H(20) H 1.1262 1.1718 0.4738 0.033 Uiso 1.00 1 c R . . H(21) H 1.1628 1.3464 0.2271 0.022 Uiso 1.00 1 c R . . H(22) H 1.3361 1.3215 0.1935 0.022 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.01134(9) 0.01022(8) 0.01473(9) 0.00225(6) -0.00423(6) -0.00605(7) Cl(1) 0.0200(2) 0.0131(2) 0.0263(3) 0.0060(2) -0.0126(2) -0.0091(2) N(1) 0.0171(10) 0.0131(9) 0.0156(9) 0.0003(7) -0.0039(7) -0.0070(8) N(2) 0.0150(9) 0.0124(8) 0.0147(9) 0.0012(7) -0.0050(7) -0.0064(7) N(3) 0.0130(9) 0.0129(8) 0.0130(9) 0.0018(7) -0.0031(7) -0.0073(7) C(1) 0.0186(12) 0.0118(10) 0.0218(12) 0.0034(9) -0.0046(9) -0.0065(9) C(2) 0.0135(11) 0.0114(10) 0.0170(11) 0.0020(8) -0.0019(8) -0.0072(9) C(3) 0.0164(11) 0.0147(11) 0.0214(12) 0.0040(9) -0.0063(9) -0.0076(10) C(4) 0.0233(13) 0.0127(10) 0.0207(12) 0.0022(9) -0.0056(9) -0.0097(9) C(5) 0.0308(14) 0.0154(11) 0.0179(12) -0.0015(10) -0.0078(10) -0.0077(10) C(6) 0.0109(10) 0.0133(10) 0.0162(11) 0.0027(8) -0.0022(8) -0.0082(9) C(7) 0.0151(11) 0.0149(10) 0.0094(10) 0.0006(8) -0.0023(8) -0.0057(9) C(8) 0.0318(15) 0.0227(12) 0.0137(11) -0.0088(11) -0.0041(10) -0.0069(10) C(9) 0.0207(12) 0.0275(13) 0.0169(12) -0.0062(10) -0.0043(9) -0.0109(10) C(10) 0.0224(12) 0.0190(11) 0.0156(11) -0.0023(9) -0.0076(9) -0.0095(9) C(11) 0.0128(11) 0.0178(11) 0.0280(13) 0.0026(9) -0.0070(9) -0.0100(10) C(12) 0.0328(15) 0.0179(12) 0.0318(15) -0.0040(11) -0.0167(12) -0.0041(11) C(13) 0.0137(11) 0.0136(10) 0.0105(10) 0.0006(8) -0.0023(8) -0.0052(8) C(14) 0.0425(17) 0.0263(14) 0.0202(13) -0.0105(12) -0.0120(12) -0.0022(11) C(15) 0.0286(14) 0.0354(15) 0.0214(13) -0.0115(11) 0.0026(10) -0.0195(12) C(16) 0.0185(12) 0.0154(11) 0.0237(12) 0.0004(9) -0.0093(9) -0.0095(10) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Pd(1) Cl(1) 2.3159(6) yes . . Pd(1) S(1) 2.290(3) yes . . Pd(1) S(2) 2.342(2) yes . . Pd(1) S(3) 2.306(3) yes . . Pd(1) S(4) 2.277(2) yes . . Pd(1) N(3) 1.9383(19) yes . . S(1) S(3) 0.187(2) yes . . S(1) C(7) 1.758(3) yes . . S(2) S(4) 0.215(3) yes . . S(2) C(13) 1.732(3) yes . . S(3) C(7) 1.722(3) yes . . S(4) C(13) 1.750(3) yes . . N(1) C(4) 1.470(3) yes . . N(1) C(7) 1.325(3) yes . . N(1) C(10) 1.472(3) yes . . N(2) C(11) 1.467(3) yes . . N(2) C(13) 1.323(3) yes . . N(2) C(16) 1.475(4) yes . . N(3) C(2) 1.363(3) yes . . N(3) C(6) 1.357(3) yes . . C(1) C(2) 1.411(3) yes . . C(1) C(3) 1.379(4) yes . . C(2) C(7) 1.460(4) yes . . C(3) C(6) 1.415(3) yes . . C(4) C(5) 1.526(2) yes . . C(5) C(8) 1.529(4) yes . . C(6) C(13) 1.457(4) yes . . C(8) C(9) 1.533(3) yes . . C(9) C(10) 1.532(2) yes . . C(11) C(12) 1.515(4) yes . . C(12) C(14) 1.527(5) yes . . C(14) C(15) 1.520(4) yes . . C(15) C(16) 1.531(4) yes . . C(1) H(1) 0.950 no . . C(3) H(2) 0.950 no . . C(4) H(3) 0.990 no . . C(4) H(4) 0.990 no . . C(5) H(5) 0.990 no . . C(5) H(6) 0.990 no . . C(8) H(7) 0.990 no . . C(8) H(8) 0.990 no . . C(9) H(9) 0.990 no . . C(9) H(10) 0.990 no . . C(10) H(11) 0.990 no . . C(10) H(12) 0.990 no . . C(11) H(13) 0.990 no . . C(11) H(14) 0.990 no . . C(12) H(15) 0.990 no . . C(12) H(16) 0.990 no . . C(14) H(17) 0.990 no . . C(14) H(18) 0.990 no . . C(15) H(19) 0.990 no . . C(15) H(20) 0.990 no . . C(16) H(21) 0.990 no . . C(16) H(22) 0.990 no . . 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Pd(1) S(1) 95.56(6) yes . . . Cl(1) Pd(1) S(2) 96.55(5) yes . . . Cl(1) Pd(1) S(3) 96.30(6) yes . . . Cl(1) Pd(1) S(4) 96.08(5) yes . . . Cl(1) Pd(1) N(3) 179.56(5) yes . . . S(1) Pd(1) S(2) 167.38(7) yes . . . S(1) Pd(1) S(3) 4.66(7) yes . . . S(1) Pd(1) S(4) 168.25(8) yes . . . S(1) Pd(1) N(3) 84.08(9) yes . . . S(2) Pd(1) S(3) 164.77(7) yes . . . S(2) Pd(1) S(4) 5.08(6) yes . . . S(2) Pd(1) N(3) 83.79(9) yes . . . S(3) Pd(1) S(4) 167.23(7) yes . . . S(3) Pd(1) N(3) 83.32(9) yes . . . S(4) Pd(1) N(3) 84.28(9) yes . . . Pd(1) S(1) S(3) 92.4(14) yes . . . Pd(1) S(1) C(7) 98.97(15) yes . . . S(3) S(1) C(7) 75.8(10) yes . . . Pd(1) S(2) S(4) 69.9(9) yes . . . Pd(1) S(2) C(13) 97.44(15) yes . . . S(4) S(2) C(13) 91.2(8) yes . . . Pd(1) S(3) S(1) 82.9(13) yes . . . Pd(1) S(3) C(7) 99.51(16) yes . . . S(1) S(3) C(7) 98.1(10) yes . . . Pd(1) S(4) S(2) 105.1(9) yes . . . Pd(1) S(4) C(13) 99.30(15) yes . . . S(2) S(4) C(13) 81.7(7) yes . . . C(4) N(1) C(7) 124.5(2) yes . . . C(4) N(1) C(10) 110.7(2) yes . . . C(7) N(1) C(10) 122.8(2) yes . . . C(11) N(2) C(13) 124.8(2) yes . . . C(11) N(2) C(16) 110.7(2) yes . . . C(13) N(2) C(16) 123.8(2) yes . . . Pd(1) N(3) C(2) 124.76(17) yes . . . Pd(1) N(3) C(6) 124.34(19) yes . . . C(2) N(3) C(6) 110.08(19) yes . . . C(2) C(1) C(3) 108.0(2) yes . . . N(3) C(2) C(1) 107.2(2) yes . . . N(3) C(2) C(7) 114.7(2) yes . . . C(1) C(2) C(7) 138.1(2) yes . . . C(1) C(3) C(6) 107.0(2) yes . . . N(1) C(4) C(5) 108.26(19) yes . . . C(4) C(5) C(8) 109.3(2) yes . . . N(3) C(6) C(3) 107.7(2) yes . . . N(3) C(6) C(13) 115.1(2) yes . . . C(3) C(6) C(13) 137.0(2) yes . . . S(1) C(7) S(3) 6.06(10) yes . . . S(1) C(7) N(1) 118.6(2) yes . . . S(1) C(7) C(2) 116.9(2) yes . . . S(3) C(7) N(1) 118.6(2) yes . . . S(3) C(7) C(2) 116.9(2) yes . . . N(1) C(7) C(2) 124.4(2) yes . . . C(5) C(8) C(9) 112.5(2) yes . . . C(8) C(9) C(10) 110.8(2) yes . . . N(1) C(10) C(9) 107.7(2) yes . . . N(2) C(11) C(12) 109.2(2) yes . . . C(11) C(12) C(14) 109.2(2) yes . . . S(2) C(13) S(4) 7.04(10) yes . . . S(2) C(13) N(2) 118.7(2) yes . . . S(2) C(13) C(6) 117.6(2) yes . . . S(4) C(13) N(2) 119.7(2) yes . . . S(4) C(13) C(6) 116.6(2) yes . . . N(2) C(13) C(6) 123.6(2) yes . . . C(12) C(14) C(15) 111.1(3) yes . . . C(14) C(15) C(16) 111.6(2) yes . . . N(2) C(16) C(15) 107.59(19) yes . . . C(2) C(1) H(1) 126.0 no . . . C(3) C(1) H(1) 126.0 no . . . C(1) C(3) H(2) 126.5 no . . . C(6) C(3) H(2) 126.5 no . . . N(1) C(4) H(3) 110.0 no . . . N(1) C(4) H(4) 110.0 no . . . C(5) C(4) H(3) 110.0 no . . . C(5) C(4) H(4) 110.0 no . . . H(3) C(4) H(4) 108.4 no . . . C(4) C(5) H(5) 109.8 no . . . C(4) C(5) H(6) 109.8 no . . . C(8) C(5) H(5) 109.8 no . . . C(8) C(5) H(6) 109.8 no . . . H(5) C(5) H(6) 108.2 no . . . C(5) C(8) H(7) 109.1 no . . . C(5) C(8) H(8) 109.1 no . . . C(9) C(8) H(7) 109.1 no . . . C(9) C(8) H(8) 109.1 no . . . H(7) C(8) H(8) 107.8 no . . . C(8) C(9) H(9) 109.5 no . . . C(8) C(9) H(10) 109.5 no . . . C(10) C(9) H(9) 109.5 no . . . C(10) C(9) H(10) 109.5 no . . . H(9) C(9) H(10) 108.0 no . . . N(1) C(10) H(11) 110.2 no . . . N(1) C(10) H(12) 110.2 no . . . C(9) C(10) H(11) 110.2 no . . . C(9) C(10) H(12) 110.2 no . . . H(11) C(10) H(12) 108.5 no . . . N(2) C(11) H(13) 109.9 no . . . N(2) C(11) H(14) 109.8 no . . . C(12) C(11) H(13) 109.8 no . . . C(12) C(11) H(14) 109.9 no . . . H(13) C(11) H(14) 108.3 no . . . C(11) C(12) H(15) 109.8 no . . . C(11) C(12) H(16) 109.8 no . . . C(14) C(12) H(15) 109.8 no . . . C(14) C(12) H(16) 109.8 no . . . H(15) C(12) H(16) 108.3 no . . . C(12) C(14) H(17) 109.4 no . . . C(12) C(14) H(18) 109.4 no . . . C(15) C(14) H(17) 109.4 no . . . C(15) C(14) H(18) 109.4 no . . . H(17) C(14) H(18) 108.0 no . . . C(14) C(15) H(19) 109.3 no . . . C(14) C(15) H(20) 109.3 no . . . C(16) C(15) H(19) 109.3 no . . . C(16) C(15) H(20) 109.3 no . . . H(19) C(15) H(20) 108.0 no . . . N(2) C(16) H(21) 110.2 no . . . N(2) C(16) H(22) 110.2 no . . . C(15) C(16) H(21) 110.2 no . . . C(15) C(16) H(22) 110.2 no . . . H(21) C(16) H(22) 108.5 no . . . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Pd(1) S(1) S(3) -99.4(10) ? . . . . Cl(1) Pd(1) S(1) C(7) -175.36(10) ? . . . . Cl(1) Pd(1) S(2) S(4) -85.0(8) ? . . . . Cl(1) Pd(1) S(2) C(13) -173.60(9) ? . . . . Cl(1) Pd(1) S(3) S(1) 81.1(10) ? . . . . Cl(1) Pd(1) S(3) C(7) 178.24(10) ? . . . . Cl(1) Pd(1) S(4) S(2) 95.5(8) ? . . . . Cl(1) Pd(1) S(4) C(13) 179.40(9) ? . . . . Cl(1) Pd(1) N(3) C(2) 28(10) ? . . . . Cl(1) Pd(1) N(3) C(6) -141(9) ? . . . . S(1) Pd(1) S(2) S(4) 111.4(8) ? . . . . S(1) Pd(1) S(2) C(13) 22.8(3) ? . . . . S(2) Pd(1) S(1) S(3) 64.3(11) ? . . . . S(2) Pd(1) S(1) C(7) -11.8(4) ? . . . . S(1) Pd(1) S(3) C(7) 97.1(10) ? . . . . S(3) Pd(1) S(1) C(7) -76.0(10) ? . . . . S(1) Pd(1) S(4) S(2) -91.9(9) ? . . . . S(1) Pd(1) S(4) C(13) -8.1(4) ? . . . . S(4) Pd(1) S(1) S(3) 88.1(11) ? . . . . S(4) Pd(1) S(1) C(7) 12.1(4) ? . . . . S(1) Pd(1) N(3) C(2) -8.30(18) ? . . . . S(1) Pd(1) N(3) C(6) -176.90(17) ? . . . . N(3) Pd(1) S(1) S(3) 80.4(10) ? . . . . N(3) Pd(1) S(1) C(7) 4.38(11) ? . . . . S(2) Pd(1) S(3) S(1) -131.5(9) ? . . . . S(2) Pd(1) S(3) C(7) -34.3(3) ? . . . . S(3) Pd(1) S(2) S(4) 127.6(7) ? . . . . S(3) Pd(1) S(2) C(13) 39.0(3) ? . . . . S(2) Pd(1) S(4) C(13) 83.9(8) ? . . . . S(4) Pd(1) S(2) C(13) -88.6(8) ? . . . . S(2) Pd(1) N(3) C(2) 168.19(19) ? . . . . S(2) Pd(1) N(3) C(6) -0.40(16) ? . . . . N(3) Pd(1) S(2) S(4) 95.3(8) ? . . . . N(3) Pd(1) S(2) C(13) 6.69(10) ? . . . . S(3) Pd(1) S(4) S(2) -70.4(9) ? . . . . S(3) Pd(1) S(4) C(13) 13.5(4) ? . . . . S(4) Pd(1) S(3) S(1) -113.0(10) ? . . . . S(4) Pd(1) S(3) C(7) -15.8(4) ? . . . . S(3) Pd(1) N(3) C(2) -3.68(18) ? . . . . S(3) Pd(1) N(3) C(6) -172.27(17) ? . . . . N(3) Pd(1) S(3) S(1) -99.1(10) ? . . . . N(3) Pd(1) S(3) C(7) -2.00(12) ? . . . . S(4) Pd(1) N(3) C(2) 173.27(19) ? . . . . S(4) Pd(1) N(3) C(6) 4.68(16) ? . . . . N(3) Pd(1) S(4) S(2) -84.2(8) ? . . . . N(3) Pd(1) S(4) C(13) -0.34(11) ? . . . . Pd(1) S(1) S(3) C(7) -98.7(3) ? . . . . Pd(1) S(1) C(7) S(3) 90.2(14) ? . . . . Pd(1) S(1) C(7) N(1) -178.38(15) ? . . . . Pd(1) S(1) C(7) C(2) -1.59(19) ? . . . . S(3) S(1) C(7) N(1) 91.4(14) ? . . . . S(3) S(1) C(7) C(2) -91.8(13) ? . . . . C(7) S(1) S(3) Pd(1) 98.7(3) ? . . . . Pd(1) S(2) S(4) C(13) -97.5(2) ? . . . . Pd(1) S(2) C(13) S(4) 69.8(9) ? . . . . Pd(1) S(2) C(13) N(2) 170.24(16) ? . . . . Pd(1) S(2) C(13) C(6) -13.04(19) ? . . . . S(4) S(2) C(13) N(2) 100.4(9) ? . . . . S(4) S(2) C(13) C(6) -82.9(9) ? . . . . C(13) S(2) S(4) Pd(1) 97.5(2) ? . . . . Pd(1) S(3) C(7) S(1) -84.2(13) ? . . . . Pd(1) S(3) C(7) N(1) -176.06(15) ? . . . . Pd(1) S(3) C(7) C(2) 7.12(19) ? . . . . S(1) S(3) C(7) N(1) -91.9(13) ? . . . . S(1) S(3) C(7) C(2) 91.3(14) ? . . . . Pd(1) S(4) C(13) S(2) -104.0(9) ? . . . . Pd(1) S(4) C(13) N(2) 172.47(17) ? . . . . Pd(1) S(4) C(13) C(6) -3.34(19) ? . . . . S(2) S(4) C(13) N(2) -83.5(9) ? . . . . S(2) S(4) C(13) C(6) 100.7(9) ? . . . . C(4) N(1) C(7) S(1) -179.14(17) ? . . . . C(4) N(1) C(7) S(3) -172.23(18) ? . . . . C(4) N(1) C(7) C(2) 4.3(3) ? . . . . C(7) N(1) C(4) C(5) 96.3(2) ? . . . . C(4) N(1) C(10) C(9) 65.8(2) ? . . . . C(10) N(1) C(4) C(5) -67.8(3) ? . . . . C(7) N(1) C(10) C(9) -98.7(2) ? . . . . C(10) N(1) C(7) S(1) -16.9(2) ? . . . . C(10) N(1) C(7) S(3) -10.0(2) ? . . . . C(10) N(1) C(7) C(2) 166.61(19) ? . . . . C(11) N(2) C(13) S(2) 179.74(18) ? . . . . C(11) N(2) C(13) S(4) -172.28(18) ? . . . . C(11) N(2) C(13) C(6) 3.2(3) ? . . . . C(13) N(2) C(11) C(12) -104.1(3) ? . . . . C(11) N(2) C(16) C(15) -63.4(2) ? . . . . C(16) N(2) C(11) C(12) 66.4(2) ? . . . . C(13) N(2) C(16) C(15) 107.2(2) ? . . . . C(16) N(2) C(13) S(2) 10.4(2) ? . . . . C(16) N(2) C(13) S(4) 18.4(2) ? . . . . C(16) N(2) C(13) C(6) -166.1(2) ? . . . . Pd(1) N(3) C(2) C(1) -168.04(15) ? . . . . Pd(1) N(3) C(2) C(7) 9.2(2) ? . . . . Pd(1) N(3) C(6) C(3) 167.93(15) ? . . . . Pd(1) N(3) C(6) C(13) -8.0(2) ? . . . . C(2) N(3) C(6) C(3) -2.1(2) ? . . . . C(2) N(3) C(6) C(13) -178.03(18) ? . . . . C(6) N(3) C(2) C(1) 1.9(2) ? . . . . C(6) N(3) C(2) C(7) 179.16(18) ? . . . . C(2) C(1) C(3) C(6) -0.2(2) ? . . . . C(3) C(1) C(2) N(3) -1.0(2) ? . . . . C(3) C(1) C(2) C(7) -177.2(2) ? . . . . N(3) C(2) C(7) S(1) -3.8(2) ? . . . . N(3) C(2) C(7) S(3) -10.6(2) ? . . . . N(3) C(2) C(7) N(1) 172.82(19) ? . . . . C(1) C(2) C(7) S(1) 172.3(2) ? . . . . C(1) C(2) C(7) S(3) 165.5(2) ? . . . . C(1) C(2) C(7) N(1) -11.2(4) ? . . . . C(1) C(3) C(6) N(3) 1.4(2) ? . . . . C(1) C(3) C(6) C(13) 176.0(2) ? . . . . N(1) C(4) C(5) C(8) 58.6(3) ? . . . . C(4) C(5) C(8) C(9) -51.6(3) ? . . . . N(3) C(6) C(13) S(2) 14.8(2) ? . . . . N(3) C(6) C(13) S(4) 7.0(2) ? . . . . N(3) C(6) C(13) N(2) -168.6(2) ? . . . . C(3) C(6) C(13) S(2) -159.5(2) ? . . . . C(3) C(6) C(13) S(4) -167.3(2) ? . . . . C(3) C(6) C(13) N(2) 17.1(4) ? . . . . C(5) C(8) C(9) C(10) 50.8(3) ? . . . . C(8) C(9) C(10) N(1) -55.9(3) ? . . . . N(2) C(11) C(12) C(14) -59.4(3) ? . . . . C(11) C(12) C(14) C(15) 53.3(2) ? . . . . C(12) C(14) C(15) C(16) -52.8(2) ? . . . . C(14) C(15) C(16) N(2) 56.3(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) C(10) 3.515(3) ? . 2_675 S(1) C(3) 3.580(3) ? . 2_775 S(1) C(6) 3.471(3) ? . 2_775 S(1) C(11) 3.542(3) ? . 1_455 S(2) C(4) 3.451(3) ? . 1_565 S(3) C(11) 3.424(3) ? . 1_455 S(4) N(1) 3.530(2) ? . 2_775 S(4) C(4) 3.510(3) ? . 1_565 S(4) C(4) 3.448(2) ? . 2_775 N(1) S(4) 3.530(2) ? . 2_775 N(1) N(2) 3.556(2) ? . 2_775 N(1) C(13) 3.358(2) ? . 2_775 N(2) N(1) 3.556(2) ? . 2_775 N(2) C(10) 3.413(2) ? . 2_775 N(3) N(3) 3.484(3) ? . 2_775 N(3) C(2) 3.464(2) ? . 2_775 N(3) C(7) 3.545(2) ? . 2_775 C(2) N(3) 3.464(2) ? . 2_775 C(3) S(1) 3.580(3) ? . 2_775 C(4) S(2) 3.451(3) ? . 1_545 C(4) S(4) 3.510(3) ? . 1_545 C(4) S(4) 3.448(2) ? . 2_775 C(6) S(1) 3.471(3) ? . 2_775 C(6) C(7) 3.498(2) ? . 2_775 C(7) N(3) 3.545(2) ? . 2_775 C(7) C(6) 3.498(2) ? . 2_775 C(7) C(13) 3.555(3) ? . 2_775 C(10) Cl(1) 3.515(3) ? . 2_675 C(10) N(2) 3.413(2) ? . 2_775 C(11) S(1) 3.542(3) ? . 1_655 C(11) S(3) 3.424(3) ? . 1_655 C(13) N(1) 3.358(2) ? . 2_775 C(13) C(7) 3.555(3) ? . 2_775 Pd(1) H(13) 3.524 ? . 1_455 Pd(1) H(17) 3.003 ? . 2_776 Cl(1) H(4) 3.053 ? . 1_565 Cl(1) H(8) 2.927 ? . 1_565 Cl(1) H(9) 3.160 ? . 2_675 Cl(1) H(11) 3.132 ? . 1_565 Cl(1) H(11) 3.014 ? . 2_675 Cl(1) H(12) 3.348 ? . 2_675 Cl(1) H(13) 3.050 ? . 1_455 Cl(1) H(21) 3.243 ? . 2_785 Cl(1) H(22) 3.033 ? . 1_455 Cl(1) H(22) 3.117 ? . 2_785 S(1) H(12) 3.231 ? . 2_675 S(1) H(13) 2.821 ? . 1_455 S(1) H(14) 3.400 ? . 1_455 S(1) H(14) 3.280 ? . 2_775 S(2) H(3) 3.419 ? . 1_565 S(2) H(3) 3.471 ? . 2_775 S(2) H(4) 2.839 ? . 1_565 S(2) H(4) 3.259 ? . 2_775 S(2) H(6) 3.146 ? . 1_565 S(2) H(16) 3.228 ? . 2_776 S(3) H(12) 3.285 ? . 2_675 S(3) H(13) 2.721 ? . 1_455 S(3) H(14) 3.284 ? . 1_455 S(3) H(14) 3.432 ? . 2_775 S(3) H(17) 3.554 ? . 2_776 S(4) H(3) 3.478 ? . 1_565 S(4) H(3) 3.259 ? . 2_775 S(4) H(4) 2.857 ? . 1_565 S(4) H(4) 3.082 ? . 2_775 S(4) H(6) 3.311 ? . 1_565 S(4) H(16) 3.434 ? . 2_776 N(2) H(11) 2.970 ? . 2_775 N(2) H(12) 3.277 ? . 2_775 N(3) H(17) 3.034 ? . 2_776 N(3) H(20) 3.292 ? . 2_776 C(1) H(19) 3.346 ? . 2_776 C(1) H(20) 3.228 ? . 2_776 C(2) H(17) 3.412 ? . 2_776 C(2) H(19) 3.529 ? . 2_776 C(2) H(20) 3.505 ? . 2_776 C(3) H(19) 3.593 ? . 2_776 C(3) H(20) 2.837 ? . 2_776 C(5) H(7) 3.366 ? . 2_666 C(5) H(10) 3.138 ? . 2_666 C(5) H(15) 3.321 ? . 2_766 C(5) H(16) 3.476 ? . 2_766 C(6) H(17) 3.512 ? . 2_776 C(6) H(20) 2.908 ? . 2_776 C(8) H(5) 3.307 ? . 2_666 C(8) H(7) 3.327 ? . 2_666 C(8) H(10) 3.142 ? . 2_666 C(8) H(15) 3.182 ? . 2_766 C(8) H(18) 3.090 ? . 1_445 C(8) H(19) 3.090 ? . 1_445 C(9) H(5) 3.163 ? . 2_666 C(9) H(7) 3.222 ? . 2_666 C(9) H(19) 3.354 ? . 1_445 C(10) H(13) 3.273 ? . 2_775 C(10) H(22) 3.386 ? . 2_775 C(11) H(11) 3.418 ? . 2_775 C(11) H(12) 3.174 ? . 2_775 C(12) H(6) 3.035 ? . 2_766 C(12) H(17) 3.488 ? . 2_876 C(12) H(18) 3.132 ? . 2_876 C(13) H(11) 3.527 ? . 2_775 C(13) H(20) 3.465 ? . 2_776 C(14) H(7) 3.403 ? . 1_665 C(14) H(8) 3.216 ? . 1_665 C(14) H(15) 3.032 ? . 2_876 C(14) H(17) 3.478 ? . 2_876 C(14) H(18) 3.121 ? . 2_876 C(15) H(7) 3.416 ? . 1_665 C(15) H(8) 3.320 ? . 1_665 C(15) H(9) 3.522 ? . 1_665 C(16) H(8) 3.565 ? . 1_665 C(16) H(9) 3.549 ? . 1_665 C(16) H(11) 3.034 ? . 2_775 H(1) H(19) 3.553 ? . 2_776 H(1) H(21) 3.548 ? . 1_545 H(2) H(5) 3.395 ? . 2_766 H(2) H(6) 2.966 ? . 2_766 H(2) H(9) 3.203 ? . 1_655 H(2) H(10) 3.150 ? . 1_655 H(2) H(20) 3.095 ? . 2_776 H(3) S(2) 3.419 ? . 1_545 H(3) S(2) 3.471 ? . 2_775 H(3) S(4) 3.478 ? . 1_545 H(3) S(4) 3.259 ? . 2_775 H(3) H(21) 3.234 ? . 1_545 H(4) Cl(1) 3.053 ? . 1_545 H(4) S(2) 2.839 ? . 1_545 H(4) S(2) 3.259 ? . 2_775 H(4) S(4) 2.857 ? . 1_545 H(4) S(4) 3.082 ? . 2_775 H(4) H(21) 3.452 ? . 2_775 H(5) C(8) 3.307 ? . 2_666 H(5) C(9) 3.163 ? . 2_666 H(5) H(2) 3.395 ? . 2_766 H(5) H(7) 2.613 ? . 2_666 H(5) H(9) 3.142 ? . 2_666 H(5) H(10) 2.641 ? . 2_666 H(5) H(19) 3.272 ? . 2_776 H(6) S(2) 3.146 ? . 1_545 H(6) S(4) 3.311 ? . 1_545 H(6) C(12) 3.035 ? . 2_766 H(6) H(2) 2.966 ? . 2_766 H(6) H(10) 3.205 ? . 2_666 H(6) H(15) 2.652 ? . 2_766 H(6) H(16) 2.525 ? . 2_766 H(7) C(5) 3.366 ? . 2_666 H(7) C(8) 3.327 ? . 2_666 H(7) C(9) 3.222 ? . 2_666 H(7) C(14) 3.403 ? . 1_445 H(7) C(15) 3.416 ? . 1_445 H(7) H(5) 2.613 ? . 2_666 H(7) H(7) 3.010 ? . 2_666 H(7) H(10) 2.406 ? . 2_666 H(7) H(15) 2.797 ? . 2_766 H(7) H(17) 3.450 ? . 1_445 H(7) H(18) 2.864 ? . 1_445 H(7) H(19) 2.672 ? . 1_445 H(8) Cl(1) 2.927 ? . 1_545 H(8) C(14) 3.216 ? . 1_445 H(8) C(15) 3.320 ? . 1_445 H(8) C(16) 3.565 ? . 1_445 H(8) H(15) 2.989 ? . 2_766 H(8) H(18) 2.419 ? . 1_445 H(8) H(19) 2.874 ? . 1_445 H(8) H(22) 2.910 ? . 1_445 H(9) Cl(1) 3.160 ? . 2_675 H(9) C(15) 3.522 ? . 1_445 H(9) C(16) 3.549 ? . 1_445 H(9) H(2) 3.203 ? . 1_455 H(9) H(5) 3.142 ? . 2_666 H(9) H(19) 2.745 ? . 1_445 H(9) H(21) 3.524 ? . 1_445 H(9) H(22) 3.103 ? . 1_445 H(10) C(5) 3.138 ? . 2_666 H(10) C(8) 3.142 ? . 2_666 H(10) H(2) 3.150 ? . 1_455 H(10) H(5) 2.641 ? . 2_666 H(10) H(6) 3.205 ? . 2_666 H(10) H(7) 2.406 ? . 2_666 H(10) H(14) 3.238 ? . 1_455 H(10) H(15) 3.342 ? . 1_455 H(11) Cl(1) 3.132 ? . 1_545 H(11) Cl(1) 3.014 ? . 2_675 H(11) N(2) 2.970 ? . 2_775 H(11) C(11) 3.418 ? . 2_775 H(11) C(13) 3.527 ? . 2_775 H(11) C(16) 3.034 ? . 2_775 H(11) H(13) 2.970 ? . 2_775 H(11) H(21) 3.222 ? . 2_775 H(11) H(22) 2.508 ? . 2_775 H(12) Cl(1) 3.348 ? . 2_675 H(12) S(1) 3.231 ? . 2_675 H(12) S(3) 3.285 ? . 2_675 H(12) N(2) 3.277 ? . 2_775 H(12) C(11) 3.174 ? . 2_775 H(12) H(13) 2.695 ? . 2_775 H(12) H(14) 3.390 ? . 1_455 H(12) H(14) 3.129 ? . 2_775 H(12) H(22) 3.500 ? . 2_775 H(13) Pd(1) 3.524 ? . 1_655 H(13) Cl(1) 3.050 ? . 1_655 H(13) S(1) 2.821 ? . 1_655 H(13) S(3) 2.721 ? . 1_655 H(13) C(10) 3.273 ? . 2_775 H(13) H(11) 2.970 ? . 2_775 H(13) H(12) 2.695 ? . 2_775 H(14) S(1) 3.400 ? . 1_655 H(14) S(1) 3.280 ? . 2_775 H(14) S(3) 3.284 ? . 1_655 H(14) S(3) 3.432 ? . 2_775 H(14) H(10) 3.238 ? . 1_655 H(14) H(12) 3.390 ? . 1_655 H(14) H(12) 3.129 ? . 2_775 H(15) C(5) 3.321 ? . 2_766 H(15) C(8) 3.182 ? . 2_766 H(15) C(14) 3.032 ? . 2_876 H(15) H(6) 2.652 ? . 2_766 H(15) H(7) 2.797 ? . 2_766 H(15) H(8) 2.989 ? . 2_766 H(15) H(10) 3.342 ? . 1_655 H(15) H(17) 2.785 ? . 2_876 H(15) H(18) 2.392 ? . 2_876 H(16) S(2) 3.228 ? . 2_776 H(16) S(4) 3.434 ? . 2_776 H(16) C(5) 3.476 ? . 2_766 H(16) H(6) 2.525 ? . 2_766 H(16) H(20) 3.303 ? . 2_776 H(17) Pd(1) 3.003 ? . 2_776 H(17) S(3) 3.554 ? . 2_776 H(17) N(3) 3.034 ? . 2_776 H(17) C(2) 3.412 ? . 2_776 H(17) C(6) 3.512 ? . 2_776 H(17) C(12) 3.488 ? . 2_876 H(17) C(14) 3.478 ? . 2_876 H(17) H(7) 3.450 ? . 1_665 H(17) H(15) 2.785 ? . 2_876 H(17) H(18) 2.863 ? . 2_876 H(18) C(8) 3.090 ? . 1_665 H(18) C(12) 3.132 ? . 2_876 H(18) C(14) 3.121 ? . 2_876 H(18) H(7) 2.864 ? . 1_665 H(18) H(8) 2.419 ? . 1_665 H(18) H(15) 2.392 ? . 2_876 H(18) H(17) 2.863 ? . 2_876 H(18) H(18) 2.899 ? . 2_876 H(19) C(1) 3.346 ? . 2_776 H(19) C(2) 3.529 ? . 2_776 H(19) C(3) 3.593 ? . 2_776 H(19) C(8) 3.090 ? . 1_665 H(19) C(9) 3.354 ? . 1_665 H(19) H(1) 3.553 ? . 2_776 H(19) H(5) 3.272 ? . 2_776 H(19) H(7) 2.672 ? . 1_665 H(19) H(8) 2.874 ? . 1_665 H(19) H(9) 2.745 ? . 1_665 H(20) N(3) 3.292 ? . 2_776 H(20) C(1) 3.228 ? . 2_776 H(20) C(2) 3.505 ? . 2_776 H(20) C(3) 2.837 ? . 2_776 H(20) C(6) 2.908 ? . 2_776 H(20) C(13) 3.465 ? . 2_776 H(20) H(2) 3.095 ? . 2_776 H(20) H(16) 3.303 ? . 2_776 H(21) Cl(1) 3.243 ? . 2_785 H(21) H(1) 3.548 ? . 1_565 H(21) H(3) 3.234 ? . 1_565 H(21) H(4) 3.452 ? . 2_775 H(21) H(9) 3.524 ? . 1_665 H(21) H(11) 3.222 ? . 2_775 H(22) Cl(1) 3.033 ? . 1_655 H(22) Cl(1) 3.117 ? . 2_785 H(22) C(10) 3.386 ? . 2_775 H(22) H(8) 2.910 ? . 1_665 H(22) H(9) 3.103 ? . 1_665 H(22) H(11) 2.508 ? . 2_775 H(22) H(12) 3.500 ? . 2_775 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================