Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Nobuhiko Iki' 'Chizuko Kabuto' 'Hiroshi Katagiri' 'Sotaro Miyano' 'Naoya Morohashi' _publ_contact_author_address ; Biomolecular Engineering Tohoku University Aramaki-Aoba 07 Aoba-ku Sendai 980-8579 JAPAN ; _publ_contact_author_email IKI@ORGSYNTH.CHE.TOHOKU.AC.JP _publ_contact_author_name 'Dr Nobuhiko Iki' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_page_first ? _journal_year ? _publ_section_title ; Pd(II) Complexes with Thiacalix[4]arene and Thiacalix[4]aniline; Subtle, but Distinct Influences of the Phenol and Aniline Units on the Three-Dimensional Structure ; data_Pd-TCA-complex-miyano _database_code_CSD 192371 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C92 H124 Cl4 N4 O14 Pd2 S8 ' _chemical_formula_moiety '?' _chemical_formula_weight 2121.10 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 13.0224(7) _cell_length_b 31.4980(2) _cell_length_c 13.5987(7) _cell_angle_alpha 90 _cell_angle_beta 107.0044(4) _cell_angle_gamma 90 _cell_volume 5334.1(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 33249 _cell_measurement_theta_min ? _cell_measurement_theta_max 27.5 _cell_measurement_temperature 223.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.678 _exptl_absorpt_correction_T_max 0.878 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 65670 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 26.00 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All oxygen atoms are refined anisotropically to give smaller R values. Although O(17) has very large thermal ellipsoids, the residual peak indicates the presence of water molecule and also indicates the hydrogen bonding with O(18) water molecule. The occupancies of the water molecules seem to decrease in the further refinement, but the water molecules are not so important for the global complex structure. Therefore we terminated the refinement in the data represented herein. Similarly, in the included MeCN, if the atoms are allowed to refine freely, Me-C-N bond significantly bends due to the disorder of N atom. Hence, N(202) and C(204) were fixed. Because one of the water oxygen is disordered into two sites, O(12) and O(13), the number of oxygen in the chemical formula sum is given by subtracting one from the number of total oxygen sites, 8, followed by multiplying by 2 due to symmetry to give O14. ; _refine_ls_structure_factor_coef Fsqd _reflns_number_total 10266 _reflns_number_gt 7595 _reflns_threshold_expression >2sigma(I) _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10266 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.605 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.081 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) ; 'O' 'O' 0.011 0.006 ;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) ; 'N' 'N' 0.006 0.003 ;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) ; '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 DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd 0.16277(2) -0.04694(1) -0.01164(2) 0.02303(8) Uani 1.00 d . . . Cl(1) Cl -0.3720(7) -0.2949(3) -0.5422(7) 0.156(4) Uani 0.30 d P . . Cl(2) Cl -0.4339(8) -0.2191(3) -0.383(1) 0.182(5) Uani 0.30 d P . . S(1) S -0.23302(8) 0.01096(3) -0.35558(7) 0.0364(2) Uani 1.00 d . . . S(2) S 0.12972(7) -0.08679(3) -0.15795(6) 0.0270(2) Uani 1.00 d . . . S(3) S -0.07326(7) -0.14151(3) 0.11934(7) 0.0334(2) Uani 1.00 d . . . S(4) S -0.31079(6) 0.00884(3) 0.01725(6) 0.0248(2) Uani 1.00 d . . . O(1) O -0.1906(2) 0.02513(7) -0.1316(2) 0.0270(5) Uani 1.00 d . . . O(2) O -0.0452(2) -0.02444(9) -0.1640(2) 0.0407(6) Uani 1.00 d . . . O(3) O 0.0526(2) -0.08266(7) 0.0254(2) 0.0272(5) Uani 1.00 d . . . O(4) O -0.1219(2) -0.04630(8) 0.0337(2) 0.0391(6) Uani 1.00 d . . . O(12) O -0.827(1) -0.1873(6) -0.367(1) 0.084(4) Uani 0.50 d P . . O(13) O -0.786(2) -0.1909(6) -0.338(2) 0.161(10) Uani 0.50 d P . . O(17) O -0.683(4) -0.2047(6) -1.087(5) 0.66(6) Uani 0.50 d P . . O(18) O -0.780(1) -0.2106(3) -0.941(1) 0.151(6) Uani 0.50 d P . . N(201) N -0.672(1) -0.1800(4) -0.643(1) 0.267(8) Uani 1.00 d . . . N(202) N -0.3126 -0.1234 -0.4311 0.45(2) Uani 1.00 d . . . C(1) C -0.2825(3) 0.0051(1) -0.1728(2) 0.0250(7) Uani 1.00 d . . . C(2) C -0.3126(3) -0.0070(1) -0.2775(3) 0.0303(7) Uani 1.00 d . . . C(3) C -0.4089(3) -0.0281(1) -0.3201(3) 0.0355(8) Uani 1.00 d . . . C(4) C -0.4782(3) -0.0393(1) -0.2624(3) 0.0340(8) Uani 1.00 d . . . C(5) C -0.4474(3) -0.0272(1) -0.1591(3) 0.0323(8) Uani 1.00 d . . . C(6) C -0.3517(3) -0.0056(1) -0.1160(2) 0.0262(7) Uani 1.00 d . . . C(7) C -0.0498(3) -0.0381(1) -0.2582(3) 0.0294(7) Uani 1.00 d . . . C(8) C 0.0312(3) -0.0658(1) -0.2673(2) 0.0274(7) Uani 1.00 d . . . C(9) C 0.0349(3) -0.0807(1) -0.3624(3) 0.0311(7) Uani 1.00 d . . . C(10) C -0.0437(3) -0.0698(1) -0.4525(3) 0.0340(8) Uani 1.00 d . . . C(11) C -0.1264(3) -0.0434(1) -0.4423(3) 0.0343(8) Uani 1.00 d . . . C(12) C -0.1312(3) -0.0274(1) -0.3485(3) 0.0307(7) Uani 1.00 d . . . C(13) C 0.0211(3) -0.1177(1) -0.0298(3) 0.0266(7) Uani 1.00 d . . . C(14) C -0.0443(3) -0.1479(1) -0.0002(3) 0.0305(7) Uani 1.00 d . . . C(15) C -0.0726(3) -0.1850(1) -0.0562(3) 0.0366(8) Uani 1.00 d . . . C(16) C -0.0404(3) -0.1938(1) -0.1437(3) 0.0416(9) Uani 1.00 d . . . C(17) C 0.0223(3) -0.1633(1) -0.1739(3) 0.0374(8) Uani 1.00 d . . . C(18) C 0.0508(3) -0.1263(1) -0.1182(3) 0.0304(7) Uani 1.00 d . . . C(19) C -0.1945(3) -0.0663(1) 0.0689(2) 0.0260(7) Uani 1.00 d . . . C(20) C -0.2850(3) -0.0429(1) 0.0725(2) 0.0262(7) Uani 1.00 d . . . C(21) C -0.3648(3) -0.0600(1) 0.1095(3) 0.0323(8) Uani 1.00 d . . . C(22) C -0.3591(3) -0.1021(1) 0.1425(3) 0.0394(9) Uani 1.00 d . . . C(23) C -0.2715(3) -0.1256(1) 0.1355(3) 0.0342(8) Uani 1.00 d . . . C(24) C -0.1884(3) -0.1088(1) 0.1010(3) 0.0279(7) Uani 1.00 d . . . C(101) C -0.5852(3) -0.0622(2) -0.3097(3) 0.048(1) Uani 1.00 d . . . C(102) C -0.6763(4) -0.0299(2) -0.3240(5) 0.076(2) Uani 1.00 d . . . C(103) C -0.5932(4) -0.0818(2) -0.4138(4) 0.074(2) Uani 1.00 d . . . C(104) C -0.6007(5) -0.0976(2) -0.2379(5) 0.082(2) Uani 1.00 d . . . C(105) C -0.0445(3) -0.0874(1) -0.5580(3) 0.0428(10) Uani 1.00 d . . . C(106) C -0.0866(6) -0.0540(2) -0.6423(3) 0.071(2) Uani 1.00 d . . . C(107) C -0.1161(6) -0.1258(2) -0.5819(4) 0.081(2) Uani 1.00 d . . . C(108) C 0.0669(5) -0.0998(3) -0.5596(4) 0.118(3) Uani 1.00 d . . . C(109) C -0.0693(4) -0.2359(1) -0.2034(4) 0.056(1) Uani 1.00 d . . . C(110) C -0.4503(4) -0.1199(1) 0.1814(4) 0.053(1) Uani 1.00 d . . . C(111) C -0.5542(4) -0.1190(2) 0.0926(5) 0.079(2) Uani 1.00 d . . . C(112) C -0.4638(5) -0.0926(2) 0.2696(5) 0.080(2) Uani 1.00 d . . . C(113) C -0.4257(5) -0.1655(2) 0.2202(5) 0.081(2) Uani 1.00 d . . . C(114) C -0.1592(7) -0.2588(2) -0.1779(6) 0.107(3) Uani 1.00 d . . . C(115) C -0.1005(7) -0.2279(2) -0.3186(5) 0.107(3) Uani 1.00 d . . . C(116) C 0.0298(6) -0.2639(2) -0.1754(7) 0.116(3) Uani 1.00 d . . . C(201) C -0.7794(5) -0.1215(2) -0.7551(6) 0.091(2) Uani 1.00 d . . . C(202) C -0.7259(7) -0.1537(3) -0.6980(9) 0.134(3) Uani 1.00 d . . . C(203) C -0.2645(9) -0.1187(3) -0.217(1) 0.170(5) Uani 1.00 d . . . C(204) C -0.2855 -0.1227 -0.3452 0.25(1) Uani 1.00 d . . . C(205) C -0.416(3) -0.2163(8) -0.516(2) 0.11(1) Uani 0.30 d P . . C(206) C -0.430(4) -0.248(2) -0.567(3) 0.18(2) Uani 0.30 d P . . H(1) H -0.0562 -0.0628 0.0409 0.0416 Uiso 1.00 calc . . . H(2) H -0.0973 -0.0042 -0.1491 0.0416 Uiso 1.00 calc . . . H(3) H -0.4286 -0.0353 -0.3912 0.0422 Uiso 1.00 calc . . . H(4) H -0.4927 -0.0338 -0.1172 0.0390 Uiso 1.00 calc . . . H(5) H 0.0917 -0.0988 -0.3656 0.0371 Uiso 1.00 calc . . . H(6) H -0.1824 -0.0362 -0.5024 0.0412 Uiso 1.00 calc . . . H(7) H -0.1151 -0.2054 -0.0339 0.0436 Uiso 1.00 calc . . . H(8) H 0.0453 -0.1680 -0.2333 0.0446 Uiso 1.00 calc . . . H(9) H -0.4242 -0.0428 0.1120 0.0391 Uiso 1.00 calc . . . H(10) H -0.2674 -0.1547 0.1555 0.0412 Uiso 1.00 calc . . . H(11) H -0.6730 -0.0174 -0.2596 0.0902 Uiso 1.00 calc . . . H(12) H -0.6691 -0.0085 -0.3707 0.0902 Uiso 1.00 calc . . . H(13) H -0.7433 -0.0439 -0.3508 0.0902 Uiso 1.00 calc . . . H(14) H -0.6623 -0.0940 -0.4414 0.0869 Uiso 1.00 calc . . . H(15) H -0.5830 -0.0602 -0.4593 0.0869 Uiso 1.00 calc . . . H(16) H -0.5398 -0.1029 -0.4063 0.0869 Uiso 1.00 calc . . . H(17) H -0.5975 -0.0860 -0.1735 0.0946 Uiso 1.00 calc . . . H(18) H -0.6702 -0.1100 -0.2679 0.0946 Uiso 1.00 calc . . . H(19) H -0.5475 -0.1185 -0.2320 0.0946 Uiso 1.00 calc . . . H(20) H -0.0415 -0.0298 -0.6279 0.0845 Uiso 1.00 calc . . . H(21) H -0.0874 -0.0657 -0.7068 0.0845 Uiso 1.00 calc . . . H(22) H -0.1576 -0.0462 -0.6437 0.0845 Uiso 1.00 calc . . . H(23) H -0.1859 -0.1176 -0.5807 0.0980 Uiso 1.00 calc . . . H(24) H -0.1185 -0.1359 -0.6478 0.0980 Uiso 1.00 calc . . . H(25) H -0.0884 -0.1468 -0.5316 0.0980 Uiso 1.00 calc . . . H(26) H 0.0943 -0.1215 -0.5092 0.1433 Uiso 1.00 calc . . . H(27) H 0.0641 -0.1109 -0.6256 0.1433 Uiso 1.00 calc . . . H(28) H 0.1132 -0.0761 -0.5448 0.1433 Uiso 1.00 calc . . . H(29) H -0.5691 -0.0906 0.0699 0.0908 Uiso 1.00 calc . . . H(30) H -0.5459 -0.1362 0.0386 0.0908 Uiso 1.00 calc . . . H(31) H -0.6111 -0.1296 0.1163 0.0908 Uiso 1.00 calc . . . H(32) H -0.3998 -0.0935 0.3230 0.0945 Uiso 1.00 calc . . . H(33) H -0.4799 -0.0647 0.2442 0.0945 Uiso 1.00 calc . . . H(34) H -0.5216 -0.1039 0.2900 0.0945 Uiso 1.00 calc . . . H(35) H -0.4837 -0.1761 0.2423 0.0962 Uiso 1.00 calc . . . H(36) H -0.4164 -0.1828 0.1665 0.0962 Uiso 1.00 calc . . . H(37) H -0.3619 -0.1657 0.2764 0.0962 Uiso 1.00 calc . . . H(38) H -0.2212 -0.2417 -0.1975 0.1205 Uiso 1.00 calc . . . H(39) H -0.1723 -0.2846 -0.2170 0.1205 Uiso 1.00 calc . . . H(40) H -0.1391 -0.2649 -0.1077 0.1205 Uiso 1.00 calc . . . H(41) H -0.1638 -0.2118 -0.3385 0.1218 Uiso 1.00 calc . . . H(42) H -0.0437 -0.2139 -0.3350 0.1218 Uiso 1.00 calc . . . H(43) H -0.1125 -0.2549 -0.3530 0.1218 Uiso 1.00 calc . . . H(44) H 0.0476 -0.2700 -0.1029 0.1330 Uiso 1.00 calc . . . H(45) H 0.0134 -0.2897 -0.2123 0.1330 Uiso 1.00 calc . . . H(46) H 0.0864 -0.2498 -0.1898 0.1330 Uiso 1.00 calc . . . H(47) H -0.1873 -0.1172 -0.1841 0.0542 Uiso 1.00 calc . . . H(48) H -0.2952 -0.0933 -0.2012 0.0542 Uiso 1.00 calc . . . H(49) H -0.2917 -0.1424 -0.1917 0.0542 Uiso 1.00 calc . . . H(50) H -0.7293 -0.1022 -0.7675 0.1183 Uiso 1.00 calc . . . H(51) H -0.8226 -0.1076 -0.7191 0.1183 Uiso 1.00 calc . . . H(52) H -0.8253 -0.1317 -0.8194 0.1183 Uiso 1.00 calc . . . H(53) H -0.4555 -0.1936 -0.5539 0.1321 Uiso 0.30 calc P . . H(54) H -0.3395 -0.2106 -0.5084 0.1321 Uiso 0.30 calc P . . H(55) H -0.4311 -0.2387 -0.6335 0.2146 Uiso 0.30 calc P . . H(56) H -0.5087 -0.2522 -0.5716 0.2146 Uiso 0.30 calc P . . 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) 0.0249(1) 0.0224(1) 0.0214(1) 0.0002(1) 0.00623(9) -0.0010(1) Cl(1) 0.150(7) 0.180(8) 0.165(7) 0.061(6) 0.087(6) 0.111(7) Cl(2) 0.127(7) 0.110(6) 0.27(1) -0.020(5) 0.002(7) 0.038(7) S(1) 0.0416(5) 0.0431(5) 0.0246(4) 0.0078(4) 0.0098(4) 0.0066(4) S(2) 0.0293(4) 0.0276(4) 0.0248(4) -0.0004(3) 0.0092(3) -0.0035(3) S(3) 0.0379(5) 0.0299(5) 0.0356(5) 0.0075(4) 0.0158(4) 0.0105(4) S(4) 0.0260(4) 0.0240(4) 0.0247(4) 0.0009(3) 0.0077(3) 0.0005(3) O(1) 0.029(1) 0.031(1) 0.022(1) -0.001(1) 0.0091(9) -0.0024(10) O(2) 0.042(2) 0.058(2) 0.020(1) 0.017(1) 0.006(1) -0.007(1) O(3) 0.032(1) 0.024(1) 0.028(1) -0.0037(10) 0.013(1) -0.0030(9) O(4) 0.039(1) 0.027(1) 0.061(2) 0.004(1) 0.030(1) 0.010(1) O(12) 0.071(8) 0.086(8) 0.088(6) 0.016(7) 0.016(6) 0.003(5) O(13) 0.12(2) 0.08(1) 0.31(3) -0.06(1) 0.10(2) -0.02(1) O(17) 0.53(6) 0.09(1) 0.92(10) -0.08(2) -0.45(7) -0.01(3) O(18) 0.140(10) 0.061(6) 0.17(1) 0.013(6) -0.085(8) -0.030(6) N(201) 0.21(1) 0.21(1) 0.38(2) 0.079(10) 0.08(1) 0.17(1) N(202) 0.37(3) 0.67(4) 0.41(3) 0.31(3) 0.25(2) 0.26(3) C(1) 0.026(2) 0.023(2) 0.025(2) 0.002(1) 0.005(1) 0.001(1) C(2) 0.031(2) 0.034(2) 0.024(2) 0.006(1) 0.006(1) -0.002(1) C(3) 0.037(2) 0.039(2) 0.024(2) 0.004(2) -0.001(1) -0.005(2) C(4) 0.028(2) 0.036(2) 0.034(2) 0.001(1) 0.001(1) -0.003(2) C(5) 0.024(2) 0.033(2) 0.037(2) 0.000(1) 0.005(1) 0.000(2) C(6) 0.027(2) 0.026(2) 0.023(2) 0.003(1) 0.004(1) 0.000(1) C(7) 0.032(2) 0.033(2) 0.023(2) -0.004(1) 0.008(1) -0.002(1) C(8) 0.029(2) 0.030(2) 0.024(2) -0.004(1) 0.008(1) -0.002(1) C(9) 0.035(2) 0.033(2) 0.028(2) -0.005(2) 0.013(2) -0.004(1) C(10) 0.039(2) 0.041(2) 0.026(2) -0.010(2) 0.014(2) -0.006(2) C(11) 0.035(2) 0.043(2) 0.023(2) -0.004(2) 0.005(1) 0.001(2) C(12) 0.030(2) 0.035(2) 0.027(2) -0.001(2) 0.010(1) 0.000(1) C(13) 0.029(2) 0.020(2) 0.029(2) 0.001(1) 0.006(1) 0.000(1) C(14) 0.036(2) 0.024(2) 0.032(2) -0.001(1) 0.011(2) 0.000(1) C(15) 0.043(2) 0.022(2) 0.045(2) -0.004(2) 0.015(2) 0.001(2) C(16) 0.049(2) 0.028(2) 0.048(2) -0.005(2) 0.014(2) -0.007(2) C(17) 0.048(2) 0.030(2) 0.036(2) -0.001(2) 0.015(2) -0.005(2) C(18) 0.035(2) 0.024(2) 0.034(2) 0.001(1) 0.013(2) -0.001(1) C(19) 0.028(2) 0.026(2) 0.024(2) 0.000(1) 0.008(1) 0.002(1) C(20) 0.031(2) 0.023(2) 0.024(2) 0.000(1) 0.008(1) 0.003(1) C(21) 0.031(2) 0.032(2) 0.036(2) 0.002(1) 0.014(2) 0.003(1) C(22) 0.033(2) 0.040(2) 0.048(2) -0.001(2) 0.018(2) 0.013(2) C(23) 0.037(2) 0.028(2) 0.038(2) -0.002(2) 0.012(2) 0.006(2) C(24) 0.031(2) 0.026(2) 0.027(2) 0.000(1) 0.009(1) 0.002(1) C(101) 0.035(2) 0.055(3) 0.047(2) -0.009(2) 0.003(2) -0.015(2) C(102) 0.030(2) 0.089(4) 0.094(4) 0.003(2) -0.004(2) -0.029(3) C(103) 0.046(3) 0.100(4) 0.069(3) -0.025(3) 0.007(2) -0.043(3) C(104) 0.071(4) 0.076(4) 0.085(4) -0.042(3) 0.000(3) -0.003(3) C(105) 0.046(2) 0.060(3) 0.023(2) -0.001(2) 0.012(2) -0.011(2) C(106) 0.125(5) 0.067(3) 0.027(2) -0.012(3) 0.029(3) -0.006(2) C(107) 0.137(6) 0.059(3) 0.047(3) -0.025(3) 0.027(3) -0.021(2) C(108) 0.071(4) 0.248(10) 0.038(3) 0.037(5) 0.021(3) -0.046(4) C(109) 0.075(3) 0.030(2) 0.064(3) -0.010(2) 0.021(3) -0.014(2) C(110) 0.044(2) 0.042(2) 0.083(3) 0.003(2) 0.034(2) 0.025(2) C(111) 0.042(3) 0.083(4) 0.113(5) -0.015(3) 0.026(3) 0.029(4) C(112) 0.074(4) 0.089(4) 0.102(4) 0.007(3) 0.064(4) 0.027(3) C(113) 0.069(3) 0.058(3) 0.136(5) 0.007(3) 0.062(4) 0.041(3) C(114) 0.131(6) 0.063(4) 0.142(6) -0.057(4) 0.062(5) -0.056(4) C(115) 0.182(8) 0.061(4) 0.070(4) -0.040(4) 0.026(4) -0.038(3) C(116) 0.105(5) 0.049(4) 0.176(8) 0.012(3) 0.014(5) -0.050(4) C(201) 0.070(4) 0.104(5) 0.106(5) 0.028(4) 0.036(4) 0.026(4) C(202) 0.096(6) 0.125(7) 0.180(9) -0.001(5) 0.038(6) 0.055(7) C(203) 0.125(8) 0.103(7) 0.22(1) 0.059(6) -0.040(8) 0.029(7) C(204) 0.13(1) 0.088(8) 0.57(4) -0.005(7) 0.14(2) 0.07(1) C(205) 0.14(2) 0.08(2) 0.06(1) -0.02(2) -0.06(1) 0.02(1) C(206) 0.21(4) 0.24(5) 0.11(3) 0.05(4) 0.09(3) 0.11(3) #------------------------------------------------------------------------------ _computing_data_collection 'P' _computing_cell_refinement 'P' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) S(2) 2.2844(9) . . yes Pd(1) S(4) 2.2908(9) . 3_555 yes Pd(1) O(1) 1.996(2) . 3_555 yes Pd(1) O(3) 2.000(3) . . yes Cl(1) C(206) 1.66(5) . . yes Cl(2) C(205) 1.89(3) . . yes S(1) C(2) 1.780(4) . . yes S(1) C(12) 1.776(4) . . yes S(2) C(8) 1.783(3) . . yes S(2) C(18) 1.796(4) . . yes S(3) C(14) 1.784(4) . . yes S(3) C(24) 1.775(4) . . yes S(4) C(6) 1.792(3) . . yes S(4) C(20) 1.785(3) . . yes O(1) C(1) 1.324(4) . . yes O(2) C(7) 1.336(4) . . yes O(3) C(13) 1.330(4) . . yes O(4) C(19) 1.336(5) . . yes N(201) C(202) 1.19(2) . . yes N(202) C(204) 1.117 . . yes C(1) C(2) 1.413(4) . . yes C(1) C(6) 1.388(5) . . yes C(2) C(3) 1.388(5) . . yes C(3) C(4) 1.403(6) . . yes C(4) C(5) 1.396(5) . . yes C(4) C(101) 1.533(5) . . yes C(5) C(6) 1.390(5) . . yes C(7) C(8) 1.402(5) . . yes C(7) C(12) 1.408(4) . . yes C(8) C(9) 1.390(5) . . yes C(9) C(10) 1.389(4) . . yes C(10) C(11) 1.399(6) . . yes C(10) C(105) 1.535(5) . . yes C(11) C(12) 1.391(5) . . yes C(13) C(14) 1.411(5) . . yes C(13) C(18) 1.393(6) . . yes C(14) C(15) 1.387(5) . . yes C(15) C(16) 1.400(7) . . yes C(16) C(17) 1.399(6) . . yes C(16) C(109) 1.543(6) . . yes C(17) C(18) 1.379(5) . . yes C(19) C(20) 1.403(5) . . yes C(19) C(24) 1.404(5) . . yes C(20) C(21) 1.388(6) . . yes C(21) C(22) 1.396(5) . . yes C(22) C(23) 1.387(6) . . yes C(22) C(110) 1.540(7) . . yes C(23) C(24) 1.403(6) . . yes C(101) C(102) 1.532(7) . . yes C(101) C(103) 1.518(7) . . yes C(101) C(104) 1.532(8) . . yes C(105) C(106) 1.535(6) . . yes C(105) C(107) 1.503(7) . . yes C(105) C(108) 1.509(8) . . yes C(109) C(114) 1.50(1) . . yes C(109) C(115) 1.519(8) . . yes C(109) C(116) 1.515(9) . . yes C(110) C(111) 1.528(7) . . yes C(110) C(112) 1.528(9) . . yes C(110) C(113) 1.531(7) . . yes C(201) C(202) 1.34(1) . . yes C(203) C(204) 1.69(1) . . yes C(205) C(206) 1.19(5) . . yes O(2) H(2) 0.995 . . no O(4) H(1) 0.982 . . no C(3) H(3) 0.952 . . no C(5) H(4) 0.956 . . no C(9) H(5) 0.946 . . no C(11) H(6) 0.950 . . no C(15) H(7) 0.953 . . no C(17) H(8) 0.952 . . no C(21) H(9) 0.952 . . no C(23) H(10) 0.952 . . no C(102) H(11) 0.950 . . no C(102) H(12) 0.950 . . no C(102) H(13) 0.950 . . no C(103) H(14) 0.951 . . no C(103) H(15) 0.953 . . no C(103) H(16) 0.947 . . no C(104) H(17) 0.939 . . no C(104) H(18) 0.961 . . no C(104) H(19) 0.942 . . no C(106) H(20) 0.946 . . no C(106) H(21) 0.948 . . no C(106) H(22) 0.951 . . no C(107) H(23) 0.950 . . no C(107) H(24) 0.943 . . no C(107) H(25) 0.943 . . no C(108) H(26) 0.959 . . no C(108) H(27) 0.954 . . no C(108) H(28) 0.943 . . no C(111) H(29) 0.947 . . no C(111) H(30) 0.945 . . no C(111) H(31) 0.951 . . no C(112) H(32) 0.931 . . no C(112) H(33) 0.946 . . no C(112) H(34) 0.945 . . no C(113) H(35) 0.951 . . no C(113) H(36) 0.947 . . no C(113) H(37) 0.951 . . no C(114) H(38) 0.943 . . no C(114) H(39) 0.960 . . no C(114) H(40) 0.934 . . no C(115) H(41) 0.938 . . no C(115) H(42) 0.943 . . no C(115) H(43) 0.961 . . no C(116) H(44) 0.963 . . no C(116) H(45) 0.946 . . no C(116) H(46) 0.930 . . no C(201) H(50) 0.943 . . no C(201) H(51) 0.954 . . no C(201) H(52) 0.958 . . no C(203) H(47) 0.975 . . no C(203) H(48) 0.949 . . no C(203) H(49) 0.934 . . no C(205) H(53) 0.941 . . no C(205) H(54) 0.990 . . no C(206) H(55) 0.951 . . no C(206) H(56) 1.014 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(2) Pd(1) S(4) 101.82(3) . . 3_555 yes S(2) Pd(1) O(1) 166.71(7) . . 3_555 yes S(2) Pd(1) O(3) 86.79(7) . . . yes S(4) Pd(1) O(1) 86.42(7) 3_555 . 3_555 yes S(4) Pd(1) O(3) 167.31(6) 3_555 . . yes O(1) Pd(1) O(3) 83.51(9) 3_555 . . yes C(2) S(1) C(12) 107.9(2) . . . yes Pd(1) S(2) C(8) 115.4(1) . . . yes Pd(1) S(2) C(18) 95.6(1) . . . yes C(8) S(2) C(18) 100.0(2) . . . yes C(14) S(3) C(24) 109.4(2) . . . yes Pd(1) S(4) C(6) 95.9(1) 3_555 . . yes Pd(1) S(4) C(20) 115.8(1) 3_555 . . yes C(6) S(4) C(20) 99.1(1) . . . yes Pd(1) O(1) C(1) 117.5(2) 3_555 . . yes Pd(1) O(3) C(13) 116.8(2) . . . yes O(1) C(1) C(2) 120.3(3) . . . yes O(1) C(1) C(6) 122.3(3) . . . yes C(2) C(1) C(6) 117.4(3) . . . yes S(1) C(2) C(1) 118.5(3) . . . yes S(1) C(2) C(3) 121.0(3) . . . yes C(1) C(2) C(3) 120.0(4) . . . yes C(2) C(3) C(4) 122.5(3) . . . yes C(3) C(4) C(5) 116.8(3) . . . yes C(3) C(4) C(101) 122.6(3) . . . yes C(5) C(4) C(101) 120.6(4) . . . yes C(4) C(5) C(6) 121.0(4) . . . yes S(4) C(6) C(1) 116.8(2) . . . yes S(4) C(6) C(5) 121.0(3) . . . yes C(1) C(6) C(5) 122.2(3) . . . yes O(2) C(7) C(8) 117.4(3) . . . yes O(2) C(7) C(12) 124.8(3) . . . yes C(8) C(7) C(12) 117.8(3) . . . yes S(2) C(8) C(7) 122.3(3) . . . yes S(2) C(8) C(9) 116.0(3) . . . yes C(7) C(8) C(9) 121.5(3) . . . yes C(8) C(9) C(10) 121.4(3) . . . yes C(9) C(10) C(11) 116.7(3) . . . yes C(9) C(10) C(105) 122.5(4) . . . yes C(11) C(10) C(105) 120.8(3) . . . yes C(10) C(11) C(12) 123.3(3) . . . yes S(1) C(12) C(7) 124.7(3) . . . yes S(1) C(12) C(11) 115.5(2) . . . yes C(7) C(12) C(11) 119.3(3) . . . yes O(3) C(13) C(14) 120.7(3) . . . yes O(3) C(13) C(18) 122.1(3) . . . yes C(14) C(13) C(18) 117.3(3) . . . yes S(3) C(14) C(13) 119.4(3) . . . yes S(3) C(14) C(15) 120.1(3) . . . yes C(13) C(14) C(15) 119.8(4) . . . yes C(14) C(15) C(16) 122.4(4) . . . yes C(15) C(16) C(17) 117.4(3) . . . yes C(15) C(16) C(109) 122.0(4) . . . yes C(17) C(16) C(109) 120.6(4) . . . yes C(16) C(17) C(18) 120.3(4) . . . yes S(2) C(18) C(13) 116.9(3) . . . yes S(2) C(18) C(17) 120.4(3) . . . yes C(13) C(18) C(17) 122.7(4) . . . yes O(4) C(19) C(20) 117.1(3) . . . yes O(4) C(19) C(24) 125.4(3) . . . yes C(20) C(19) C(24) 117.6(3) . . . yes S(4) C(20) C(19) 121.4(3) . . . yes S(4) C(20) C(21) 116.0(3) . . . yes C(19) C(20) C(21) 122.3(3) . . . yes C(20) C(21) C(22) 120.7(4) . . . yes C(21) C(22) C(23) 116.9(4) . . . yes C(21) C(22) C(110) 118.9(4) . . . yes C(23) C(22) C(110) 124.1(4) . . . yes C(22) C(23) C(24) 123.5(3) . . . yes S(3) C(24) C(19) 124.5(3) . . . yes S(3) C(24) C(23) 115.9(3) . . . yes C(19) C(24) C(23) 119.0(3) . . . yes C(4) C(101) C(102) 108.4(4) . . . yes C(4) C(101) C(103) 112.8(4) . . . yes C(4) C(101) C(104) 110.4(3) . . . yes C(102) C(101) C(103) 108.1(4) . . . yes C(102) C(101) C(104) 108.8(5) . . . yes C(103) C(101) C(104) 108.2(4) . . . yes C(10) C(105) C(106) 110.7(4) . . . yes C(10) C(105) C(107) 109.1(4) . . . yes C(10) C(105) C(108) 111.3(3) . . . yes C(106) C(105) C(107) 109.0(4) . . . yes C(106) C(105) C(108) 107.5(5) . . . yes C(107) C(105) C(108) 109.1(5) . . . yes C(16) C(109) C(114) 112.2(5) . . . yes C(16) C(109) C(115) 110.6(4) . . . yes C(16) C(109) C(116) 108.0(4) . . . yes C(114) C(109) C(115) 109.0(5) . . . yes C(114) C(109) C(116) 109.1(5) . . . yes C(115) C(109) C(116) 107.9(6) . . . yes C(22) C(110) C(111) 108.4(4) . . . yes C(22) C(110) C(112) 109.9(4) . . . yes C(22) C(110) C(113) 110.9(4) . . . yes C(111) C(110) C(112) 109.3(4) . . . yes C(111) C(110) C(113) 109.8(4) . . . yes C(112) C(110) C(113) 108.6(5) . . . yes N(201) C(202) C(201) 174(1) . . . yes N(202) C(204) C(203) 170.8(4) . . . yes Cl(2) C(205) C(206) 118(2) . . . yes Cl(1) C(206) C(205) 130(2) . . . yes C(7) O(2) H(2) 124.1 . . . no C(19) O(4) H(1) 113.7 . . . no C(2) C(3) H(3) 118.7 . . . no C(4) C(3) H(3) 118.8 . . . no C(4) C(5) H(4) 119.7 . . . no C(6) C(5) H(4) 119.3 . . . no C(8) C(9) H(5) 119.1 . . . no C(10) C(9) H(5) 119.5 . . . no C(10) C(11) H(6) 118.6 . . . no C(12) C(11) H(6) 118.2 . . . no C(14) C(15) H(7) 118.7 . . . no C(16) C(15) H(7) 118.9 . . . no C(16) C(17) H(8) 119.8 . . . no C(18) C(17) H(8) 119.8 . . . no C(20) C(21) H(9) 119.7 . . . no C(22) C(21) H(9) 119.6 . . . no C(22) C(23) H(10) 118.2 . . . no C(24) C(23) H(10) 118.3 . . . no C(101) C(102) H(11) 109.5 . . . no C(101) C(102) H(12) 109.5 . . . no C(101) C(102) H(13) 109.4 . . . no H(11) C(102) H(12) 109.5 . . . no H(11) C(102) H(13) 109.5 . . . no H(12) C(102) H(13) 109.5 . . . no C(101) C(103) H(14) 109.4 . . . no C(101) C(103) H(15) 109.4 . . . no C(101) C(103) H(16) 109.7 . . . no H(14) C(103) H(15) 109.2 . . . no H(14) C(103) H(16) 109.7 . . . no H(15) C(103) H(16) 109.5 . . . no C(101) C(104) H(17) 109.6 . . . no C(101) C(104) H(18) 108.1 . . . no C(101) C(104) H(19) 109.4 . . . no H(17) C(104) H(18) 109.4 . . . no H(17) C(104) H(19) 111.1 . . . no H(18) C(104) H(19) 109.2 . . . no C(105) C(106) H(20) 109.4 . . . no C(105) C(106) H(21) 109.2 . . . no C(105) C(106) H(22) 108.9 . . . no H(20) C(106) H(21) 110.0 . . . no H(20) C(106) H(22) 109.7 . . . no H(21) C(106) H(22) 109.5 . . . no C(105) C(107) H(23) 108.2 . . . no C(105) C(107) H(24) 108.8 . . . no C(105) C(107) H(25) 108.9 . . . no H(23) C(107) H(24) 110.1 . . . no H(23) C(107) H(25) 110.1 . . . no H(24) C(107) H(25) 110.7 . . . no C(105) C(108) H(26) 109.4 . . . no C(105) C(108) H(27) 109.7 . . . no C(105) C(108) H(28) 110.4 . . . no H(26) C(108) H(27) 108.4 . . . no H(26) C(108) H(28) 109.2 . . . no H(27) C(108) H(28) 109.7 . . . no C(110) C(111) H(29) 109.1 . . . no C(110) C(111) H(30) 109.1 . . . no C(110) C(111) H(31) 108.9 . . . no H(29) C(111) H(30) 110.2 . . . no H(29) C(111) H(31) 109.6 . . . no H(30) C(111) H(31) 109.9 . . . no C(110) C(112) H(32) 108.2 . . . no C(110) C(112) H(33) 107.5 . . . no C(110) C(112) H(34) 107.6 . . . no H(32) C(112) H(33) 111.5 . . . no H(32) C(112) H(34) 111.5 . . . no H(33) C(112) H(34) 110.3 . . . no C(110) C(113) H(35) 109.4 . . . no C(110) C(113) H(36) 109.5 . . . no C(110) C(113) H(37) 109.2 . . . no H(35) C(113) H(36) 109.7 . . . no H(35) C(113) H(37) 109.3 . . . no H(36) C(113) H(37) 109.7 . . . no C(109) C(114) H(38) 108.8 . . . no C(109) C(114) H(39) 107.8 . . . no C(109) C(114) H(40) 109.4 . . . no H(38) C(114) H(39) 109.2 . . . no H(38) C(114) H(40) 111.5 . . . no H(39) C(114) H(40) 110.0 . . . no C(109) C(115) H(41) 109.6 . . . no C(109) C(115) H(42) 109.2 . . . no C(109) C(115) H(43) 108.2 . . . no H(41) C(115) H(42) 111.2 . . . no H(41) C(115) H(43) 109.6 . . . no H(42) C(115) H(43) 109.1 . . . no C(109) C(116) H(44) 107.9 . . . no C(109) C(116) H(45) 108.8 . . . no C(109) C(116) H(46) 109.7 . . . no H(44) C(116) H(45) 108.7 . . . no H(44) C(116) H(46) 110.1 . . . no H(45) C(116) H(46) 111.6 . . . no C(202) C(201) H(50) 108.9 . . . no C(202) C(201) H(51) 109.5 . . . no C(202) C(201) H(52) 110.9 . . . no H(50) C(201) H(51) 109.7 . . . no H(50) C(201) H(52) 109.4 . . . no H(51) C(201) H(52) 108.5 . . . no C(204) C(203) H(47) 108.3 . . . no C(204) C(203) H(48) 110.3 . . . no C(204) C(203) H(49) 111.0 . . . no H(47) C(203) H(48) 107.5 . . . no H(47) C(203) H(49) 108.7 . . . no H(48) C(203) H(49) 110.9 . . . no Cl(2) C(205) H(53) 110.9 . . . no Cl(2) C(205) H(54) 108.0 . . . no C(206) C(205) H(53) 110.6 . . . no C(206) C(205) H(54) 101.2 . . . no H(53) C(205) H(54) 106.9 . . . no Cl(1) C(206) H(55) 109.7 . . . no Cl(1) C(206) H(56) 106.4 . . . no C(205) C(206) H(55) 105.1 . . . no C(205) C(206) H(56) 97.9 . . . no H(55) C(206) H(56) 104.3 . . . no #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_kata-10-Pd-complex-230k _database_code_CSD 192372 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C83.50 H103.50 Cl10.50 N8 Pd2 S8 ' _chemical_formula_moiety 'C83.50 H103.50 Cl10.50 N8 Pd2 S8 ' _chemical_formula_weight 2060.83 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 16.0963(4) _cell_length_b 35.1851(4) _cell_length_c 17.7567(9) _cell_angle_alpha 90 _cell_angle_beta 104.0085(4) _cell_angle_gamma 90 _cell_volume 9757.4(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 16008 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 230.2 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.872 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.840 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 64044 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.00 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _reflns_number_total 17047 _reflns_number_gt 11045 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0894P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17047 _refine_ls_number_parameters 1027 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1501 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.384 _refine_diff_density_min -0.875 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) ; Pd Pd -0.999 1.007 ;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 DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd 0.65160(2) 0.72936(1) 0.83670(2) 0.0308(1) Uani 1.00 d . . . Pd(2) Pd 0.71341(2) 0.74836(1) 0.53811(2) 0.0289(1) Uani 1.00 d . . . Cl(1) Cl 0.8663(2) 0.5415(1) 1.1157(2) 0.186(2) Uani 1.00 d . . . Cl(2) Cl 0.7385(2) 0.4892(1) 1.0622(3) 0.230(2) Uani 1.00 d . . . Cl(3) Cl 0.8575(3) 0.50345(8) 0.9745(2) 0.184(2) Uani 1.00 d . . . Cl(4) Cl 0.1009(3) 0.7582(1) 0.3485(3) 0.194(2) Uani 1.00 d . . . Cl(5) Cl 0.0830(3) 0.7408(1) 0.4988(2) 0.175(1) Uani 1.00 d . . . Cl(6) Cl 0.2467(3) 0.7314(1) 0.4672(5) 0.339(4) Uani 1.00 d . . . Cl(7) Cl 0.9017(2) 0.97646(9) 0.9474(2) 0.1274(9) Uani 1.00 d . . . Cl(8) Cl 0.7900(2) 0.9715(1) 0.7967(2) 0.179(1) Uani 1.00 d . . . Cl(9) Cl 0.7368(3) 1.0094(2) 0.9151(2) 0.234(2) Uani 1.00 d . . . Cl(10) Cl 0.5789(6) 0.9981(4) 1.0860(5) 0.149(3) Uani 0.50 d P . . Cl(11) Cl 0.5684(4) 0.9585(2) 0.9550(3) 0.127(2) Uani 0.50 d P . . Cl(12) Cl 0.4430(8) 1.0040(5) 0.9489(9) 0.27(1) Uani 0.50 d P . . S(1) S 0.67630(8) 0.89221(3) 0.55693(7) 0.0419(3) Uani 1.00 d . . . S(2) S 0.60612(9) 0.87215(3) 0.84578(7) 0.0446(3) Uani 1.00 d . . . S(3) S 0.50835(7) 0.72455(3) 0.77905(6) 0.0341(2) Uani 1.00 d . . . S(4) S 0.56938(7) 0.74585(3) 0.48346(6) 0.0288(2) Uani 1.00 d . . . S(5) S 0.69426(8) 0.58626(3) 0.83068(7) 0.0437(3) Uani 1.00 d . . . S(6) S 0.74472(9) 0.60424(3) 0.53383(7) 0.0446(3) Uani 1.00 d . . . S(7) S 0.85787(7) 0.75053(3) 0.59388(6) 0.0315(2) Uani 1.00 d . . . S(8) S 0.79545(7) 0.73396(3) 0.89152(6) 0.0310(2) Uani 1.00 d . . . N(1) N 0.6779(3) 0.8497(1) 0.7077(2) 0.048(1) Uani 1.00 d . . . N(2) N 0.6320(2) 0.7850(1) 0.8311(2) 0.0343(8) Uani 1.00 d . . . N(3) N 0.5874(3) 0.7666(1) 0.6566(2) 0.0382(9) Uani 1.00 d . . . N(4) N 0.6947(2) 0.8040(1) 0.5472(2) 0.0345(8) Uani 1.00 d . . . N(5) N 0.6857(3) 0.6281(1) 0.6770(2) 0.051(1) Uani 1.00 d . . . N(6) N 0.7309(2) 0.6925(1) 0.5358(2) 0.0396(9) Uani 1.00 d . . . N(7) N 0.7823(2) 0.7091(1) 0.7195(2) 0.0347(8) Uani 1.00 d . . . N(8) N 0.6730(2) 0.6733(1) 0.8341(2) 0.0357(9) Uani 1.00 d . . . C(1) C 0.6384(3) 0.8845(1) 0.7007(3) 0.039(1) Uani 1.00 d . . . C(2) C 0.6313(3) 0.9074(1) 0.6349(3) 0.038(1) Uani 1.00 d . . . C(3) C 0.5871(3) 0.9417(1) 0.6279(3) 0.044(1) Uani 1.00 d . . . C(4) C 0.5487(3) 0.9556(1) 0.6836(3) 0.045(1) Uani 1.00 d . . . C(5) C 0.5585(3) 0.9330(1) 0.7494(3) 0.045(1) Uani 1.00 d . . . C(6) C 0.6007(3) 0.8985(1) 0.7588(3) 0.039(1) Uani 1.00 d . . . C(7) C 0.4956(4) 0.9919(2) 0.6752(3) 0.056(1) Uani 1.00 d . . . C(8) C 0.5322(7) 1.0194(2) 0.7405(5) 0.126(4) Uani 1.00 d . . . C(9) C 0.4041(6) 0.9811(2) 0.6793(6) 0.116(3) Uani 1.00 d . . . C(10) C 0.4907(6) 1.0118(2) 0.5992(4) 0.098(3) Uani 1.00 d . . . C(11) C 0.6166(3) 0.8193(1) 0.5144(2) 0.0304(9) Uani 1.00 d . . . C(12) C 0.5462(3) 0.7954(1) 0.4843(2) 0.0293(9) Uani 1.00 d . . . C(13) C 0.4647(3) 0.8084(1) 0.4517(2) 0.036(1) Uani 1.00 d . . . C(14) C 0.4467(3) 0.8470(1) 0.4446(3) 0.041(1) Uani 1.00 d . . . C(15) C 0.5154(3) 0.8714(1) 0.4752(3) 0.041(1) Uani 1.00 d . . . C(16) C 0.5967(3) 0.8587(1) 0.5107(3) 0.036(1) Uani 1.00 d . . . C(17) C 0.3593(3) 0.8632(2) 0.4026(3) 0.052(1) Uani 1.00 d . . . C(18) C 0.3321(4) 0.8940(2) 0.4506(5) 0.093(2) Uani 1.00 d . . . C(19) C 0.3668(5) 0.8797(3) 0.3254(4) 0.098(3) Uani 1.00 d . . . C(20) C 0.2891(4) 0.8332(2) 0.3897(5) 0.087(2) Uani 1.00 d . . . C(21) C 0.5393(3) 0.7357(1) 0.6307(2) 0.0316(10) Uani 1.00 d . . . C(22) C 0.5006(3) 0.7131(1) 0.6794(2) 0.0342(10) Uani 1.00 d . . . C(23) C 0.4572(3) 0.6800(1) 0.6534(3) 0.040(1) Uani 1.00 d . . . C(24) C 0.4472(3) 0.6667(1) 0.5779(3) 0.042(1) Uani 1.00 d . . . C(25) C 0.4796(3) 0.6896(1) 0.5281(3) 0.038(1) Uani 1.00 d . . . C(26) C 0.5238(3) 0.7231(1) 0.5533(2) 0.0317(10) Uani 1.00 d . . . C(27) C 0.4037(4) 0.6286(2) 0.5513(3) 0.056(1) Uani 1.00 d . . . C(28) C 0.4194(9) 0.6157(3) 0.4782(6) 0.182(6) Uani 1.00 d . . . C(29) C 0.3122(7) 0.6320(3) 0.543(1) 0.27(1) Uani 1.00 d . . . C(30) C 0.435(1) 0.5985(2) 0.6116(6) 0.207(8) Uani 1.00 d . . . C(31) C 0.8271(3) 0.7411(1) 0.7429(2) 0.0313(10) Uani 1.00 d . . . C(32) C 0.8392(3) 0.7554(1) 0.8186(2) 0.0312(10) Uani 1.00 d . . . C(33) C 0.8786(3) 0.7902(1) 0.8406(2) 0.037(1) Uani 1.00 d . . . C(34) C 0.9100(3) 0.8128(1) 0.7894(3) 0.039(1) Uani 1.00 d . . . C(35) C 0.9050(3) 0.7972(1) 0.7158(3) 0.038(1) Uani 1.00 d . . . C(36) C 0.8657(3) 0.7625(1) 0.6931(2) 0.0310(9) Uani 1.00 d . . . C(37) C 0.9483(4) 0.8521(2) 0.8119(3) 0.054(1) Uani 1.00 d . . . C(38) C 0.9151(9) 0.8693(2) 0.8742(6) 0.171(6) Uani 1.00 d . . . C(39) C 0.924(1) 0.8793(2) 0.7470(5) 0.185(6) Uani 1.00 d . . . C(40) C 1.0416(6) 0.8487(3) 0.838(1) 0.26(1) Uani 1.00 d . . . C(41) C 0.8109(3) 0.6773(1) 0.5602(2) 0.033(1) Uani 1.00 d . . . C(42) C 0.8808(3) 0.7013(1) 0.5917(2) 0.035(1) Uani 1.00 d . . . C(43) C 0.9642(3) 0.6877(2) 0.6191(3) 0.042(1) Uani 1.00 d . . . C(44) C 0.9827(3) 0.6495(2) 0.6189(3) 0.048(1) Uani 1.00 d . . . C(45) C 0.9135(3) 0.6252(2) 0.5909(3) 0.047(1) Uani 1.00 d . . . C(46) C 0.8298(3) 0.6379(1) 0.5626(2) 0.040(1) Uani 1.00 d . . . C(47) C 1.0721(4) 0.6327(2) 0.6497(4) 0.069(2) Uani 1.00 d . . . C(48) C 1.0963(5) 0.6086(3) 0.5888(6) 0.128(4) Uani 1.00 d . . . C(49) C 1.1392(4) 0.6641(3) 0.6715(5) 0.104(3) Uani 1.00 d . . . C(50) C 1.0732(5) 0.6097(3) 0.7215(6) 0.136(4) Uani 1.00 d . . . C(51) C 0.7234(3) 0.5929(1) 0.6830(3) 0.039(1) Uani 1.00 d . . . C(52) C 0.7333(3) 0.5709(1) 0.7501(3) 0.039(1) Uani 1.00 d . . . C(53) C 0.7748(3) 0.5356(1) 0.7552(3) 0.044(1) Uani 1.00 d . . . C(54) C 0.8061(3) 0.5208(1) 0.6960(3) 0.049(1) Uani 1.00 d . . . C(55) C 0.7951(3) 0.5432(1) 0.6285(3) 0.046(1) Uani 1.00 d . . . C(56) C 0.7553(3) 0.5784(1) 0.6219(3) 0.040(1) Uani 1.00 d . . . C(57) C 0.8531(4) 0.4825(2) 0.7011(4) 0.065(2) Uani 1.00 d . . . C(58) C 0.7999(7) 0.4555(2) 0.6395(5) 0.130(4) Uani 1.00 d . . . C(59) C 0.9391(6) 0.4888(3) 0.6848(6) 0.137(4) Uani 1.00 d . . . C(60) C 0.8641(5) 0.4642(2) 0.7787(4) 0.089(2) Uani 1.00 d . . . C(61) C 0.7524(3) 0.6595(1) 0.8677(2) 0.0325(10) Uani 1.00 d . . . C(62) C 0.7741(3) 0.6206(1) 0.8723(3) 0.037(1) Uani 1.00 d . . . C(63) C 0.8563(3) 0.6090(1) 0.9040(3) 0.043(1) Uani 1.00 d . . . C(64) C 0.9243(3) 0.6344(1) 0.9320(3) 0.045(1) Uani 1.00 d . . . C(65) C 0.9045(3) 0.6726(1) 0.9260(3) 0.040(1) Uani 1.00 d . . . C(66) C 0.8214(3) 0.6846(1) 0.8944(2) 0.0320(10) Uani 1.00 d . . . C(67) C 1.0155(4) 0.6199(2) 0.9698(4) 0.063(2) Uani 1.00 d . . . C(68) C 1.0223(5) 0.6154(4) 1.0553(5) 0.142(4) Uani 1.00 d . . . C(69) C 1.0819(4) 0.6481(2) 0.9581(5) 0.093(2) Uani 1.00 d . . . C(70) C 1.0324(5) 0.5830(3) 0.9330(7) 0.149(5) Uani 1.00 d . . . C(71) C 0.5487(3) 0.7987(1) 0.8102(2) 0.033(1) Uani 1.00 d . . . C(72) C 0.5255(3) 0.8374(1) 0.8112(3) 0.040(1) Uani 1.00 d . . . C(73) C 0.4413(3) 0.8486(2) 0.7810(3) 0.049(1) Uani 1.00 d . . . C(74) C 0.3757(3) 0.8231(2) 0.7485(3) 0.049(1) Uani 1.00 d . . . C(75) C 0.3986(3) 0.7854(2) 0.7498(3) 0.043(1) Uani 1.00 d . . . C(76) C 0.4823(3) 0.7736(1) 0.7793(2) 0.036(1) Uani 1.00 d . . . C(77) C 0.2854(4) 0.8375(2) 0.7129(4) 0.080(2) Uani 1.00 d . . . C(78) C 0.2272(6) 0.8086(3) 0.680(1) 0.244(10) Uani 1.00 d . . . C(79) C 0.2906(6) 0.8655(5) 0.6497(8) 0.220(8) Uani 1.00 d . . . C(80) C 0.2517(6) 0.8608(4) 0.7675(8) 0.195(7) Uani 1.00 d . . . C(101) C 0.8007(5) 0.5213(2) 1.0357(6) 0.111(3) Uani 1.00 d . . . C(102) C 0.1566(8) 0.7555(3) 0.4471(9) 0.159(5) Uani 1.00 d . . . C(103) C 0.7956(6) 0.9724(3) 0.8932(5) 0.106(3) Uani 1.00 d . . . C(104) C 0.538(1) 0.9971(5) 0.985(1) 0.096(5) Uani 0.50 d P . . H(1) H 0.6741 0.8342 0.7539 0.0544 Uiso 1.00 calc . . . H(2) H 0.6997 0.8415 0.6675 0.0544 Uiso 1.00 calc . . . H(3) H 0.5985 0.7869 0.6297 0.0544 Uiso 1.00 calc . . . H(4) H 0.6054 0.7725 0.7128 0.0544 Uiso 1.00 calc . . . H(5) H 0.7398 0.8209 0.5605 0.0544 Uiso 1.00 calc . . . H(6) H 0.6736 0.8059 0.8524 0.0544 Uiso 1.00 calc . . . H(7) H 0.7603 0.6990 0.6651 0.0544 Uiso 1.00 calc . . . H(8) H 0.7464 0.6967 0.7484 0.0544 Uiso 1.00 calc . . . H(9) H 0.6618 0.6369 0.7068 0.0544 Uiso 1.00 calc . . . H(10) H 0.6813 0.6388 0.6272 0.0544 Uiso 1.00 calc . . . H(11) H 0.6166 0.6577 0.8156 0.0544 Uiso 1.00 calc . . . H(12) H 0.6821 0.6762 0.5160 0.0544 Uiso 1.00 calc . . . H(13) H 0.5833 0.9564 0.5821 0.0522 Uiso 1.00 calc . . . H(14) H 0.5357 0.9421 0.7907 0.0543 Uiso 1.00 calc . . . H(15) H 0.4195 0.7906 0.4335 0.0437 Uiso 1.00 calc . . . H(16) H 0.5058 0.8979 0.4711 0.0488 Uiso 1.00 calc . . . H(17) H 0.4336 0.6657 0.6887 0.0483 Uiso 1.00 calc . . . H(18) H 0.4716 0.6822 0.4754 0.0455 Uiso 1.00 calc . . . H(19) H 0.4278 0.8750 0.7826 0.0580 Uiso 1.00 calc . . . H(20) H 0.3556 0.7669 0.7299 0.0511 Uiso 1.00 calc . . . H(21) H 0.8841 0.7988 0.8923 0.0448 Uiso 1.00 calc . . . H(22) H 0.9293 0.8109 0.6802 0.0457 Uiso 1.00 calc . . . H(23) H 1.0094 0.7052 0.6387 0.0512 Uiso 1.00 calc . . . H(24) H 0.9240 0.5986 0.5915 0.0566 Uiso 1.00 calc . . . H(25) H 0.7819 0.5214 0.8017 0.0535 Uiso 1.00 calc . . . H(26) H 0.8149 0.5339 0.5857 0.0548 Uiso 1.00 calc . . . H(27) H 0.8680 0.5825 0.9070 0.0524 Uiso 1.00 calc . . . H(28) H 0.9482 0.6909 0.9437 0.0482 Uiso 1.00 calc . . . H(29) H 0.5347 1.0070 0.7880 0.1582 Uiso 1.00 calc . . . H(30) H 0.5867 1.0270 0.7364 0.1582 Uiso 1.00 calc . . . H(31) H 0.4948 1.0407 0.7352 0.1582 Uiso 1.00 calc . . . H(32) H 0.3710 1.0036 0.6756 0.1376 Uiso 1.00 calc . . . H(33) H 0.3808 0.9648 0.6370 0.1376 Uiso 1.00 calc . . . H(34) H 0.4066 0.9687 0.7267 0.1376 Uiso 1.00 calc . . . H(35) H 0.5459 1.0196 0.5968 0.1195 Uiso 1.00 calc . . . H(36) H 0.4679 0.9946 0.5582 0.1195 Uiso 1.00 calc . . . H(37) H 0.4539 1.0332 0.5956 0.1195 Uiso 1.00 calc . . . H(38) H 0.3739 0.9135 0.4600 0.1113 Uiso 1.00 calc . . . H(39) H 0.2787 0.9040 0.4228 0.1113 Uiso 1.00 calc . . . H(40) H 0.3265 0.8835 0.4981 0.1113 Uiso 1.00 calc . . . H(41) H 0.4078 0.8996 0.3349 0.1156 Uiso 1.00 calc . . . H(42) H 0.3838 0.8604 0.2956 0.1156 Uiso 1.00 calc . . . H(43) H 0.3126 0.8896 0.2991 0.1156 Uiso 1.00 calc . . . H(44) H 0.2365 0.8443 0.3632 0.1061 Uiso 1.00 calc . . . H(45) H 0.3034 0.8131 0.3598 0.1061 Uiso 1.00 calc . . . H(46) H 0.2842 0.8238 0.4386 0.1061 Uiso 1.00 calc . . . H(47) H 0.3890 0.5923 0.4642 0.2313 Uiso 1.00 calc . . . H(48) H 0.4006 0.6340 0.4401 0.2313 Uiso 1.00 calc . . . H(49) H 0.4790 0.6110 0.4857 0.2313 Uiso 1.00 calc . . . H(50) H 0.2984 0.6417 0.5889 0.2937 Uiso 1.00 calc . . . H(51) H 0.2875 0.6507 0.5015 0.2937 Uiso 1.00 calc . . . H(52) H 0.2820 0.6090 0.5285 0.2937 Uiso 1.00 calc . . . H(53) H 0.4226 0.6072 0.6589 0.2601 Uiso 1.00 calc . . . H(54) H 0.4024 0.5760 0.5952 0.2601 Uiso 1.00 calc . . . H(55) H 0.4924 0.5946 0.6173 0.2601 Uiso 1.00 calc . . . H(56) H 0.1740 0.8207 0.6557 0.3014 Uiso 1.00 calc . . . H(57) H 0.2492 0.7980 0.6370 0.3014 Uiso 1.00 calc . . . H(58) H 0.2230 0.7909 0.7143 0.3014 Uiso 1.00 calc . . . H(59) H 0.3251 0.8861 0.6731 0.2585 Uiso 1.00 calc . . . H(60) H 0.3120 0.8535 0.6126 0.2585 Uiso 1.00 calc . . . H(61) H 0.2334 0.8746 0.6285 0.2585 Uiso 1.00 calc . . . H(62) H 0.2882 0.8806 0.7851 0.2366 Uiso 1.00 calc . . . H(63) H 0.1962 0.8694 0.7405 0.2366 Uiso 1.00 calc . . . H(64) H 0.2455 0.8445 0.8088 0.2366 Uiso 1.00 calc . . . H(65) H 0.9422 0.8931 0.8877 0.2103 Uiso 1.00 calc . . . H(66) H 0.8559 0.8719 0.8584 0.2103 Uiso 1.00 calc . . . H(67) H 0.9300 0.8529 0.9189 0.2103 Uiso 1.00 calc . . . H(68) H 0.9483 0.9034 0.7629 0.2213 Uiso 1.00 calc . . . H(69) H 0.9421 0.8704 0.7038 0.2213 Uiso 1.00 calc . . . H(70) H 0.8625 0.8819 0.7334 0.2213 Uiso 1.00 calc . . . H(71) H 1.0540 0.8330 0.8829 0.3265 Uiso 1.00 calc . . . H(72) H 1.0625 0.8381 0.7983 0.3265 Uiso 1.00 calc . . . H(73) H 1.0643 0.8733 0.8511 0.3265 Uiso 1.00 calc . . . H(74) H 1.0557 0.5887 0.5749 0.1543 Uiso 1.00 calc . . . H(75) H 1.0974 0.6237 0.5456 0.1543 Uiso 1.00 calc . . . H(76) H 1.1515 0.5979 0.6101 0.1543 Uiso 1.00 calc . . . H(77) H 1.1941 0.6527 0.6916 0.1247 Uiso 1.00 calc . . . H(78) H 1.1403 0.6786 0.6274 0.1247 Uiso 1.00 calc . . . H(79) H 1.1256 0.6796 0.7106 0.1247 Uiso 1.00 calc . . . H(80) H 1.0605 0.6261 0.7603 0.1592 Uiso 1.00 calc . . . H(81) H 1.0315 0.5902 0.7098 0.1592 Uiso 1.00 calc . . . H(82) H 1.1283 0.5989 0.7407 0.1592 Uiso 1.00 calc . . . H(83) H 0.7463 0.4516 0.6499 0.1570 Uiso 1.00 calc . . . H(84) H 0.7942 0.4668 0.5900 0.1570 Uiso 1.00 calc . . . H(85) H 0.8302 0.4321 0.6416 0.1570 Uiso 1.00 calc . . . H(86) H 0.9649 0.4641 0.6831 0.1614 Uiso 1.00 calc . . . H(87) H 0.9307 0.5001 0.6350 0.1614 Uiso 1.00 calc . . . H(88) H 0.9726 0.5036 0.7230 0.1614 Uiso 1.00 calc . . . H(89) H 0.8098 0.4606 0.7892 0.1079 Uiso 1.00 calc . . . H(90) H 0.8910 0.4400 0.7775 0.1079 Uiso 1.00 calc . . . H(91) H 0.8989 0.4796 0.8169 0.1079 Uiso 1.00 calc . . . H(92) H 0.9809 0.5979 1.0633 0.1653 Uiso 1.00 calc . . . H(93) H 1.0782 0.6066 1.0800 0.1653 Uiso 1.00 calc . . . H(94) H 1.0131 0.6395 1.0764 0.1653 Uiso 1.00 calc . . . H(95) H 1.1375 0.6387 0.9825 0.1114 Uiso 1.00 calc . . . H(96) H 1.0772 0.6515 0.9046 0.1114 Uiso 1.00 calc . . . H(97) H 1.0731 0.6716 0.9813 0.1114 Uiso 1.00 calc . . . H(98) H 0.9907 0.5648 0.9399 0.1784 Uiso 1.00 calc . . . H(99) H 1.0283 0.5869 0.8802 0.1784 Uiso 1.00 calc . . . H(100) H 1.0877 0.5742 0.9585 0.1784 Uiso 1.00 calc . . . H(101) H 0.7617 0.5408 1.0074 0.1243 Uiso 1.00 calc . . . H(102) H 0.1716 0.7799 0.4650 0.1844 Uiso 1.00 calc . . . H(103) H 0.7707 0.9493 0.9066 0.1224 Uiso 1.00 calc . . . H(104) H 0.5777 1.0195 0.9804 0.1122 Uiso 0.50 calc P . . 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) 0.0369(2) 0.0336(2) 0.0248(2) 0.0050(2) 0.0131(1) 0.0034(1) Pd(2) 0.0350(2) 0.0306(2) 0.0233(2) 0.0016(1) 0.0114(1) 0.0006(1) Cl(1) 0.201(3) 0.200(3) 0.139(3) -0.083(3) 0.007(2) -0.030(2) Cl(2) 0.131(2) 0.139(3) 0.436(7) -0.043(2) 0.100(3) -0.042(4) Cl(3) 0.320(5) 0.119(2) 0.136(2) 0.100(3) 0.098(3) 0.038(2) Cl(4) 0.289(5) 0.136(3) 0.184(4) -0.060(3) 0.107(3) -0.019(2) Cl(5) 0.197(3) 0.147(3) 0.179(3) -0.031(2) 0.039(3) 0.044(2) Cl(6) 0.196(4) 0.151(4) 0.67(1) 0.070(3) 0.107(6) 0.085(5) Cl(7) 0.100(2) 0.170(3) 0.114(2) -0.014(2) 0.030(1) -0.017(2) Cl(8) 0.161(3) 0.250(4) 0.115(2) 0.037(3) 0.014(2) -0.055(2) Cl(9) 0.216(4) 0.336(6) 0.141(3) 0.165(4) 0.027(2) -0.044(3) Cl(10) 0.120(6) 0.184(7) 0.128(6) 0.028(6) 0.001(5) 0.016(5) Cl(11) 0.157(4) 0.132(4) 0.097(3) 0.017(3) 0.039(3) -0.006(3) Cl(12) 0.159(9) 0.26(1) 0.31(2) -0.069(8) -0.11(1) 0.14(1) S(1) 0.0516(7) 0.0321(6) 0.0471(7) -0.0036(5) 0.0217(6) -0.0040(5) S(2) 0.0628(8) 0.0393(7) 0.0291(6) 0.0096(6) 0.0062(6) -0.0022(5) S(3) 0.0379(6) 0.0425(6) 0.0254(5) 0.0014(5) 0.0145(5) 0.0039(5) S(4) 0.0363(6) 0.0316(6) 0.0200(5) -0.0004(5) 0.0097(4) -0.0002(4) S(5) 0.0515(7) 0.0326(6) 0.0506(7) -0.0041(5) 0.0193(6) 0.0009(5) S(6) 0.0624(8) 0.0324(6) 0.0344(6) 0.0049(6) 0.0030(6) -0.0010(5) S(7) 0.0362(6) 0.0365(6) 0.0251(5) -0.0010(5) 0.0136(5) 0.0000(4) S(8) 0.0400(6) 0.0329(6) 0.0216(5) 0.0018(5) 0.0100(4) 0.0007(4) N(1) 0.067(3) 0.037(2) 0.044(2) 0.013(2) 0.022(2) 0.001(2) N(2) 0.038(2) 0.045(2) 0.022(2) -0.005(2) 0.012(2) 0.001(2) N(3) 0.052(2) 0.037(2) 0.029(2) -0.007(2) 0.015(2) 0.004(2) N(4) 0.034(2) 0.037(2) 0.032(2) -0.004(2) 0.006(2) -0.002(2) N(5) 0.072(3) 0.040(2) 0.044(2) 0.018(2) 0.020(2) 0.007(2) N(6) 0.035(2) 0.041(2) 0.039(2) -0.002(2) 0.002(2) -0.001(2) N(7) 0.039(2) 0.038(2) 0.029(2) -0.014(2) 0.011(2) -0.003(2) N(8) 0.032(2) 0.034(2) 0.042(2) 0.005(2) 0.009(2) 0.001(2) C(1) 0.040(3) 0.034(2) 0.040(3) 0.001(2) 0.004(2) -0.003(2) C(2) 0.038(3) 0.036(3) 0.041(3) -0.003(2) 0.010(2) -0.007(2) C(3) 0.059(3) 0.032(3) 0.040(3) -0.001(2) 0.012(2) 0.001(2) C(4) 0.061(3) 0.029(2) 0.046(3) 0.009(2) 0.014(2) -0.001(2) C(5) 0.054(3) 0.042(3) 0.042(3) 0.009(2) 0.015(2) -0.008(2) C(6) 0.050(3) 0.031(2) 0.034(2) 0.003(2) 0.006(2) -0.003(2) C(7) 0.079(4) 0.043(3) 0.050(3) 0.021(3) 0.024(3) 0.005(2) C(8) 0.21(1) 0.065(5) 0.084(6) 0.064(6) 0.006(6) -0.010(4) C(9) 0.114(7) 0.075(5) 0.174(9) 0.049(5) 0.063(6) 0.030(5) C(10) 0.142(7) 0.074(5) 0.089(5) 0.057(5) 0.052(5) 0.023(4) C(11) 0.037(2) 0.033(2) 0.022(2) 0.002(2) 0.010(2) 0.000(2) C(12) 0.042(3) 0.029(2) 0.018(2) 0.004(2) 0.010(2) 0.000(2) C(13) 0.039(3) 0.045(3) 0.025(2) -0.001(2) 0.009(2) 0.000(2) C(14) 0.046(3) 0.046(3) 0.032(2) 0.011(2) 0.009(2) 0.006(2) C(15) 0.046(3) 0.039(3) 0.038(3) 0.012(2) 0.013(2) 0.008(2) C(16) 0.045(3) 0.034(2) 0.032(2) -0.003(2) 0.017(2) -0.001(2) C(17) 0.042(3) 0.055(3) 0.055(3) 0.019(3) 0.006(2) 0.007(3) C(18) 0.058(4) 0.099(6) 0.122(6) 0.037(4) 0.019(4) -0.017(5) C(19) 0.075(5) 0.142(7) 0.072(5) 0.028(5) 0.006(4) 0.052(5) C(20) 0.038(3) 0.080(5) 0.128(6) 0.011(3) -0.011(4) 0.011(4) C(21) 0.033(2) 0.034(2) 0.030(2) 0.000(2) 0.011(2) 0.002(2) C(22) 0.044(3) 0.039(2) 0.024(2) 0.000(2) 0.015(2) 0.000(2) C(23) 0.044(3) 0.038(3) 0.042(3) -0.006(2) 0.018(2) 0.005(2) C(24) 0.048(3) 0.037(3) 0.043(3) -0.008(2) 0.014(2) -0.002(2) C(25) 0.045(3) 0.037(2) 0.032(2) -0.006(2) 0.010(2) -0.004(2) C(26) 0.036(2) 0.035(2) 0.027(2) -0.002(2) 0.014(2) 0.002(2) C(27) 0.071(4) 0.040(3) 0.059(3) -0.025(3) 0.021(3) -0.011(3) C(28) 0.34(2) 0.108(7) 0.138(8) -0.154(9) 0.146(10) -0.080(6) C(29) 0.093(7) 0.099(8) 0.60(3) -0.065(6) 0.07(1) -0.15(1) C(30) 0.43(2) 0.056(5) 0.095(7) -0.095(9) -0.015(9) 0.008(5) C(31) 0.037(2) 0.032(2) 0.024(2) 0.004(2) 0.007(2) 0.000(2) C(32) 0.039(2) 0.031(2) 0.025(2) -0.002(2) 0.010(2) 0.001(2) C(33) 0.046(3) 0.040(3) 0.026(2) -0.004(2) 0.010(2) -0.006(2) C(34) 0.047(3) 0.032(2) 0.039(3) -0.005(2) 0.010(2) -0.002(2) C(35) 0.042(3) 0.046(3) 0.029(2) -0.007(2) 0.015(2) 0.003(2) C(36) 0.035(2) 0.037(2) 0.023(2) -0.001(2) 0.011(2) -0.001(2) C(37) 0.069(4) 0.041(3) 0.051(3) -0.012(3) 0.012(3) -0.007(2) C(38) 0.31(1) 0.077(6) 0.179(9) -0.110(8) 0.17(1) -0.087(6) C(39) 0.40(2) 0.060(5) 0.079(6) -0.092(8) 0.017(8) 0.002(4) C(40) 0.077(6) 0.084(7) 0.59(3) -0.029(5) 0.00(1) -0.12(1) C(41) 0.039(3) 0.037(2) 0.024(2) 0.011(2) 0.010(2) 0.001(2) C(42) 0.042(3) 0.041(3) 0.026(2) 0.003(2) 0.014(2) 0.002(2) C(43) 0.039(3) 0.060(3) 0.029(2) 0.004(2) 0.010(2) 0.001(2) C(44) 0.047(3) 0.061(3) 0.036(3) 0.015(3) 0.010(2) 0.003(2) C(45) 0.054(3) 0.049(3) 0.037(3) 0.022(3) 0.011(2) 0.004(2) C(46) 0.056(3) 0.037(3) 0.027(2) 0.006(2) 0.012(2) 0.000(2) C(47) 0.050(4) 0.081(4) 0.068(4) 0.024(3) -0.002(3) 0.008(3) C(48) 0.067(5) 0.147(8) 0.160(9) 0.063(5) 0.004(5) -0.043(7) C(49) 0.042(4) 0.117(7) 0.138(7) 0.027(4) -0.010(4) 0.011(5) C(50) 0.085(6) 0.18(1) 0.128(8) 0.030(6) -0.001(5) 0.085(7) C(51) 0.039(3) 0.030(2) 0.044(3) 0.001(2) 0.003(2) -0.003(2) C(52) 0.041(3) 0.035(3) 0.044(3) -0.003(2) 0.012(2) -0.001(2) C(53) 0.052(3) 0.032(2) 0.050(3) 0.001(2) 0.014(2) 0.008(2) C(54) 0.056(3) 0.033(3) 0.055(3) 0.010(2) 0.009(3) 0.002(2) C(55) 0.062(3) 0.033(3) 0.044(3) 0.004(2) 0.018(2) -0.002(2) C(56) 0.047(3) 0.034(2) 0.036(3) 0.004(2) 0.007(2) 0.002(2) C(57) 0.092(5) 0.039(3) 0.067(4) 0.028(3) 0.029(3) 0.015(3) C(58) 0.23(1) 0.039(4) 0.107(6) 0.036(5) 0.010(7) -0.014(4) C(59) 0.133(7) 0.112(7) 0.198(10) 0.091(6) 0.104(7) 0.094(7) C(60) 0.138(7) 0.061(4) 0.078(5) 0.043(4) 0.042(4) 0.024(3) C(61) 0.039(3) 0.035(2) 0.027(2) 0.003(2) 0.013(2) 0.003(2) C(62) 0.045(3) 0.031(2) 0.035(2) -0.001(2) 0.012(2) 0.008(2) C(63) 0.049(3) 0.036(3) 0.045(3) 0.013(2) 0.011(2) 0.010(2) C(64) 0.046(3) 0.045(3) 0.041(3) 0.008(2) 0.007(2) 0.009(2) C(65) 0.045(3) 0.038(3) 0.034(2) 0.001(2) 0.003(2) 0.001(2) C(66) 0.034(2) 0.034(2) 0.028(2) 0.006(2) 0.008(2) 0.006(2) C(67) 0.047(3) 0.059(4) 0.076(4) 0.011(3) -0.002(3) 0.020(3) C(68) 0.063(5) 0.26(1) 0.091(6) 0.010(6) -0.013(4) 0.096(7) C(69) 0.045(4) 0.105(6) 0.127(6) 0.021(4) 0.014(4) 0.032(5) C(70) 0.078(6) 0.087(6) 0.26(1) 0.048(5) -0.013(7) -0.030(7) C(71) 0.039(3) 0.044(3) 0.018(2) 0.011(2) 0.012(2) 0.004(2) C(72) 0.051(3) 0.045(3) 0.025(2) 0.012(2) 0.012(2) 0.004(2) C(73) 0.055(3) 0.054(3) 0.036(3) 0.024(3) 0.011(2) 0.004(2) C(74) 0.045(3) 0.063(3) 0.037(3) 0.018(3) 0.006(2) 0.000(2) C(75) 0.033(3) 0.063(3) 0.036(3) 0.006(2) 0.012(2) 0.002(2) C(76) 0.049(3) 0.042(3) 0.017(2) 0.005(2) 0.011(2) 0.002(2) C(77) 0.056(4) 0.094(5) 0.076(5) 0.037(4) -0.012(3) 0.000(4) C(78) 0.078(6) 0.110(8) 0.45(2) 0.034(6) -0.12(1) -0.07(1) C(79) 0.081(7) 0.33(2) 0.22(1) 0.049(9) -0.028(8) 0.17(1) C(80) 0.074(6) 0.26(2) 0.23(1) 0.090(8) 0.009(7) -0.06(1) C(101) 0.099(6) 0.071(5) 0.165(9) 0.026(4) 0.037(6) -0.008(5) C(102) 0.15(1) 0.140(10) 0.20(1) 0.007(8) 0.056(10) 0.021(9) C(103) 0.110(6) 0.114(7) 0.102(6) -0.006(5) 0.045(5) 0.000(5) C(104) 0.09(1) 0.09(1) 0.12(1) -0.01(1) 0.05(1) 0.00(1) #------------------------------------------------------------------------------ _computing_data_collection P _computing_cell_refinement P _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) S(3) 2.291(1) . . yes Pd(1) S(8) 2.290(1) . . yes Pd(1) N(2) 1.982(4) . . yes Pd(1) N(8) 2.004(4) . . yes Pd(2) S(4) 2.288(1) . . yes Pd(2) S(7) 2.297(1) . . yes Pd(2) N(4) 1.994(4) . . yes Pd(2) N(6) 1.988(4) . . yes Cl(1) C(101) 1.706(9) . . yes Cl(2) C(101) 1.65(1) . . yes Cl(3) C(101) 1.70(1) . . yes Cl(4) C(102) 1.77(1) . . yes Cl(5) C(102) 1.74(2) . . yes Cl(6) C(102) 1.64(1) . . yes Cl(7) C(103) 1.752(8) . . yes Cl(8) C(103) 1.695(10) . . yes Cl(9) C(103) 1.71(1) . . yes Cl(10) C(104) 1.75(2) . . yes Cl(11) C(104) 1.58(2) . . yes Cl(12) C(104) 1.53(2) . . yes S(1) C(2) 1.793(5) . . yes S(1) C(16) 1.787(4) . . yes S(2) C(6) 1.784(5) . . yes S(2) C(72) 1.781(5) . . yes S(3) C(22) 1.790(4) . . yes S(3) C(76) 1.776(5) . . yes S(4) C(12) 1.782(4) . . yes S(4) C(26) 1.777(5) . . yes S(5) C(52) 1.781(5) . . yes S(5) C(62) 1.787(4) . . yes S(6) C(46) 1.789(5) . . yes S(6) C(56) 1.781(5) . . yes S(7) C(36) 1.787(4) . . yes S(7) C(42) 1.773(5) . . yes S(8) C(32) 1.784(5) . . yes S(8) C(66) 1.785(4) . . yes N(1) C(1) 1.374(6) . . yes N(2) C(71) 1.387(6) . . yes N(3) C(21) 1.348(6) . . yes N(4) C(11) 1.361(5) . . yes N(5) C(51) 1.373(6) . . yes N(6) C(41) 1.365(6) . . yes N(7) C(31) 1.347(5) . . yes N(8) C(61) 1.363(5) . . yes C(1) C(2) 1.399(7) . . yes C(1) C(6) 1.406(7) . . yes C(2) C(3) 1.392(7) . . yes C(3) C(4) 1.376(8) . . yes C(4) C(5) 1.389(7) . . yes C(4) C(7) 1.526(7) . . yes C(5) C(6) 1.384(7) . . yes C(7) C(8) 1.515(9) . . yes C(7) C(9) 1.54(1) . . yes C(7) C(10) 1.506(10) . . yes C(11) C(12) 1.410(6) . . yes C(11) C(16) 1.421(6) . . yes C(12) C(13) 1.379(6) . . yes C(13) C(14) 1.388(7) . . yes C(14) C(15) 1.401(7) . . yes C(14) C(17) 1.533(7) . . yes C(15) C(16) 1.382(6) . . yes C(17) C(18) 1.508(10) . . yes C(17) C(19) 1.520(10) . . yes C(17) C(20) 1.523(8) . . yes C(21) C(22) 1.426(7) . . yes C(21) C(26) 1.407(6) . . yes C(22) C(23) 1.379(6) . . yes C(23) C(24) 1.391(7) . . yes C(24) C(25) 1.388(7) . . yes C(24) C(27) 1.534(7) . . yes C(25) C(26) 1.395(6) . . yes C(27) C(28) 1.45(1) . . yes C(27) C(29) 1.45(1) . . yes C(27) C(30) 1.50(1) . . yes C(31) C(32) 1.404(6) . . yes C(31) C(36) 1.416(7) . . yes C(32) C(33) 1.391(6) . . yes C(33) C(34) 1.392(7) . . yes C(34) C(35) 1.401(7) . . yes C(34) C(37) 1.527(7) . . yes C(35) C(36) 1.390(6) . . yes C(37) C(38) 1.47(1) . . yes C(37) C(39) 1.47(1) . . yes C(37) C(40) 1.46(1) . . yes C(41) C(42) 1.410(6) . . yes C(41) C(46) 1.417(6) . . yes C(42) C(43) 1.398(6) . . yes C(43) C(44) 1.376(8) . . yes C(44) C(45) 1.397(7) . . yes C(44) C(47) 1.529(8) . . yes C(45) C(46) 1.394(7) . . yes C(47) C(48) 1.50(1) . . yes C(47) C(49) 1.528(10) . . yes C(47) C(50) 1.51(1) . . yes C(51) C(52) 1.398(7) . . yes C(51) C(56) 1.404(7) . . yes C(52) C(53) 1.402(7) . . yes C(53) C(54) 1.374(8) . . yes C(54) C(55) 1.412(7) . . yes C(54) C(57) 1.537(8) . . yes C(55) C(56) 1.385(7) . . yes C(57) C(58) 1.541(10) . . yes C(57) C(59) 1.50(1) . . yes C(57) C(60) 1.492(9) . . yes C(61) C(62) 1.411(6) . . yes C(61) C(66) 1.408(6) . . yes C(62) C(63) 1.368(6) . . yes C(63) C(64) 1.407(7) . . yes C(64) C(65) 1.382(7) . . yes C(64) C(67) 1.545(7) . . yes C(65) C(66) 1.385(6) . . yes C(67) C(68) 1.50(1) . . yes C(67) C(69) 1.509(10) . . yes C(67) C(70) 1.51(1) . . yes C(71) C(72) 1.413(7) . . yes C(71) C(76) 1.393(6) . . yes C(72) C(73) 1.388(7) . . yes C(73) C(74) 1.401(7) . . yes C(74) C(75) 1.373(8) . . yes C(74) C(77) 1.525(8) . . yes C(75) C(76) 1.386(6) . . yes C(77) C(78) 1.41(1) . . yes C(77) C(79) 1.51(2) . . yes C(77) C(80) 1.47(2) . . yes N(1) H(1) 1.000 . . no N(1) H(2) 0.914 . . no N(2) H(6) 1.006 . . no N(3) H(3) 0.902 . . no N(3) H(4) 0.991 . . no N(4) H(5) 0.924 . . no N(5) H(9) 0.788 . . no N(5) H(10) 0.948 . . no N(6) H(12) 0.966 . . no N(7) H(7) 1.011 . . no N(7) H(8) 0.966 . . no N(8) H(11) 1.044 . . no C(3) H(13) 0.952 . . no C(5) H(14) 0.950 . . no C(8) H(29) 0.943 . . no C(8) H(30) 0.937 . . no C(8) H(31) 0.951 . . no C(9) H(32) 0.945 . . no C(9) H(33) 0.948 . . no C(9) H(34) 0.941 . . no C(10) H(35) 0.941 . . no C(10) H(36) 0.950 . . no C(10) H(37) 0.950 . . no C(13) H(15) 0.955 . . no C(15) H(16) 0.945 . . no C(18) H(38) 0.947 . . no C(18) H(39) 0.951 . . no C(18) H(40) 0.945 . . no C(19) H(41) 0.948 . . no C(19) H(42) 0.941 . . no C(19) H(43) 0.951 . . no C(20) H(44) 0.948 . . no C(20) H(45) 0.947 . . no C(20) H(46) 0.950 . . no C(23) H(17) 0.951 . . no C(25) H(18) 0.949 . . no C(28) H(47) 0.957 . . no C(28) H(48) 0.930 . . no C(28) H(49) 0.951 . . no C(29) H(50) 0.953 . . no C(29) H(51) 0.999 . . no C(29) H(52) 0.948 . . no C(30) H(53) 0.955 . . no C(30) H(54) 0.950 . . no C(30) H(55) 0.923 . . no C(33) H(21) 0.951 . . no C(35) H(22) 0.950 . . no C(38) H(65) 0.949 . . no C(38) H(66) 0.931 . . no C(38) H(67) 0.964 . . no C(39) H(68) 0.948 . . no C(39) H(69) 0.938 . . no C(39) H(70) 0.964 . . no C(40) H(71) 0.953 . . no C(40) H(72) 0.929 . . no C(40) H(73) 0.947 . . no C(43) H(23) 0.952 . . no C(45) H(24) 0.949 . . no C(48) H(74) 0.948 . . no C(48) H(75) 0.937 . . no C(48) H(76) 0.954 . . no C(49) H(77) 0.957 . . no C(49) H(78) 0.939 . . no C(49) H(79) 0.948 . . no C(50) H(80) 0.956 . . no C(50) H(81) 0.947 . . no C(50) H(82) 0.949 . . no C(53) H(25) 0.950 . . no C(55) H(26) 0.950 . . no C(58) H(83) 0.934 . . no C(58) H(84) 0.949 . . no C(58) H(85) 0.953 . . no C(59) H(86) 0.965 . . no C(59) H(87) 0.950 . . no C(59) H(88) 0.920 . . no C(60) H(89) 0.946 . . no C(60) H(90) 0.956 . . no C(60) H(91) 0.942 . . no C(63) H(27) 0.950 . . no C(65) H(28) 0.948 . . no C(68) H(92) 0.942 . . no C(68) H(93) 0.951 . . no C(68) H(94) 0.955 . . no C(69) H(95) 0.953 . . no C(69) H(96) 0.942 . . no C(69) H(97) 0.951 . . no C(70) H(98) 0.957 . . no C(70) H(99) 0.934 . . no C(70) H(100) 0.948 . . no C(73) H(19) 0.955 . . no C(75) H(20) 0.954 . . no C(78) H(56) 0.958 . . no C(78) H(57) 0.983 . . no C(78) H(58) 0.891 . . no C(79) H(59) 0.946 . . no C(79) H(60) 0.918 . . no C(79) H(61) 0.961 . . no C(80) H(62) 0.915 . . no C(80) H(63) 0.956 . . no C(80) H(64) 0.956 . . no C(101) H(101) 0.982 . . no C(102) H(102) 0.928 . . no C(103) H(103) 0.961 . . no C(104) H(104) 1.028 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(3) Pd(1) S(8) 178.65(4) . . . yes S(3) Pd(1) N(2) 85.4(1) . . . yes S(3) Pd(1) N(8) 94.40(10) . . . yes S(8) Pd(1) N(2) 94.8(1) . . . yes S(8) Pd(1) N(8) 85.29(10) . . . yes N(2) Pd(1) N(8) 175.6(2) . . . yes S(4) Pd(2) S(7) 179.48(4) . . . yes S(4) Pd(2) N(4) 85.10(10) . . . yes S(4) Pd(2) N(6) 95.0(1) . . . yes S(7) Pd(2) N(4) 95.14(10) . . . yes S(7) Pd(2) N(6) 84.8(1) . . . yes N(4) Pd(2) N(6) 176.4(2) . . . yes C(2) S(1) C(16) 100.0(2) . . . yes C(6) S(2) C(72) 100.3(2) . . . yes Pd(1) S(3) C(22) 106.2(2) . . . yes Pd(1) S(3) C(76) 98.0(1) . . . yes C(22) S(3) C(76) 105.2(2) . . . yes Pd(2) S(4) C(12) 98.7(1) . . . yes Pd(2) S(4) C(26) 105.6(1) . . . yes C(12) S(4) C(26) 108.1(2) . . . yes C(52) S(5) C(62) 100.3(2) . . . yes C(46) S(6) C(56) 100.6(2) . . . yes Pd(2) S(7) C(36) 104.8(1) . . . yes Pd(2) S(7) C(42) 98.8(1) . . . yes C(36) S(7) C(42) 106.7(2) . . . yes Pd(1) S(8) C(32) 104.9(1) . . . yes Pd(1) S(8) C(66) 98.5(1) . . . yes C(32) S(8) C(66) 107.5(2) . . . yes Pd(1) N(2) C(71) 119.2(3) . . . yes Pd(2) N(4) C(11) 119.7(3) . . . yes Pd(2) N(6) C(41) 120.5(3) . . . yes Pd(1) N(8) C(61) 119.3(3) . . . yes N(1) C(1) C(2) 122.1(5) . . . yes N(1) C(1) C(6) 121.1(4) . . . yes C(2) C(1) C(6) 116.7(4) . . . yes S(1) C(2) C(1) 120.4(4) . . . yes S(1) C(2) C(3) 118.9(4) . . . yes C(1) C(2) C(3) 120.7(5) . . . yes C(2) C(3) C(4) 123.5(4) . . . yes C(3) C(4) C(5) 115.0(4) . . . yes C(3) C(4) C(7) 124.4(4) . . . yes C(5) C(4) C(7) 120.5(5) . . . yes C(4) C(5) C(6) 123.8(5) . . . yes S(2) C(6) C(1) 121.0(3) . . . yes S(2) C(6) C(5) 118.7(4) . . . yes C(1) C(6) C(5) 120.3(4) . . . yes C(4) C(7) C(8) 110.8(5) . . . yes C(4) C(7) C(9) 108.0(5) . . . yes C(4) C(7) C(10) 112.5(6) . . . yes C(8) C(7) C(9) 108.7(7) . . . yes C(8) C(7) C(10) 108.4(5) . . . yes C(9) C(7) C(10) 108.3(6) . . . yes N(4) C(11) C(12) 120.0(4) . . . yes N(4) C(11) C(16) 125.4(4) . . . yes C(12) C(11) C(16) 114.5(4) . . . yes S(4) C(12) C(11) 115.9(3) . . . yes S(4) C(12) C(13) 120.1(3) . . . yes C(11) C(12) C(13) 123.8(4) . . . yes C(12) C(13) C(14) 121.3(4) . . . yes C(13) C(14) C(15) 115.9(4) . . . yes C(13) C(14) C(17) 123.6(4) . . . yes C(15) C(14) C(17) 120.4(4) . . . yes C(14) C(15) C(16) 123.5(4) . . . yes S(1) C(16) C(11) 119.6(3) . . . yes S(1) C(16) C(15) 119.5(3) . . . yes C(11) C(16) C(15) 120.9(4) . . . yes C(14) C(17) C(18) 110.4(4) . . . yes C(14) C(17) C(19) 108.5(5) . . . yes C(14) C(17) C(20) 112.1(4) . . . yes C(18) C(17) C(19) 109.4(6) . . . yes C(18) C(17) C(20) 106.0(5) . . . yes C(19) C(17) C(20) 110.4(5) . . . yes N(3) C(21) C(22) 122.8(4) . . . yes N(3) C(21) C(26) 122.7(4) . . . yes C(22) C(21) C(26) 114.5(4) . . . yes S(3) C(22) C(21) 122.5(3) . . . yes S(3) C(22) C(23) 115.4(4) . . . yes C(21) C(22) C(23) 122.0(4) . . . yes C(22) C(23) C(24) 122.4(5) . . . yes C(23) C(24) C(25) 116.6(4) . . . yes C(23) C(24) C(27) 121.8(5) . . . yes C(25) C(24) C(27) 121.6(4) . . . yes C(24) C(25) C(26) 121.7(4) . . . yes S(4) C(26) C(21) 122.2(3) . . . yes S(4) C(26) C(25) 114.9(3) . . . yes C(21) C(26) C(25) 122.5(4) . . . yes C(24) C(27) C(28) 112.6(6) . . . yes C(24) C(27) C(29) 109.5(6) . . . yes C(24) C(27) C(30) 110.5(5) . . . yes C(28) C(27) C(29) 109(1) . . . yes C(28) C(27) C(30) 108.5(7) . . . yes C(29) C(27) C(30) 106(1) . . . yes N(7) C(31) C(32) 122.4(4) . . . yes N(7) C(31) C(36) 122.4(4) . . . yes C(32) C(31) C(36) 115.2(4) . . . yes S(8) C(32) C(31) 123.7(3) . . . yes S(8) C(32) C(33) 113.7(3) . . . yes C(31) C(32) C(33) 122.2(4) . . . yes C(32) C(33) C(34) 122.2(4) . . . yes C(33) C(34) C(35) 115.9(4) . . . yes C(33) C(34) C(37) 122.3(4) . . . yes C(35) C(34) C(37) 121.8(5) . . . yes C(34) C(35) C(36) 122.2(4) . . . yes S(7) C(36) C(31) 123.6(3) . . . yes S(7) C(36) C(35) 114.3(3) . . . yes C(31) C(36) C(35) 121.7(4) . . . yes C(34) C(37) C(38) 111.8(6) . . . yes C(34) C(37) C(39) 111.6(5) . . . yes C(34) C(37) C(40) 109.1(6) . . . yes C(38) C(37) C(39) 104.2(7) . . . yes C(38) C(37) C(40) 109.1(10) . . . yes C(39) C(37) C(40) 110(1) . . . yes N(6) C(41) C(42) 119.5(4) . . . yes N(6) C(41) C(46) 124.9(4) . . . yes C(42) C(41) C(46) 115.4(4) . . . yes S(7) C(42) C(41) 116.4(3) . . . yes S(7) C(42) C(43) 120.9(4) . . . yes C(41) C(42) C(43) 122.7(4) . . . yes C(42) C(43) C(44) 121.6(4) . . . yes C(43) C(44) C(45) 116.5(5) . . . yes C(43) C(44) C(47) 124.2(5) . . . yes C(45) C(44) C(47) 119.4(5) . . . yes C(44) C(45) C(46) 123.3(5) . . . yes S(6) C(46) C(41) 119.7(3) . . . yes S(6) C(46) C(45) 119.8(4) . . . yes C(41) C(46) C(45) 120.5(4) . . . yes C(44) C(47) C(48) 110.3(5) . . . yes C(44) C(47) C(49) 111.0(5) . . . yes C(44) C(47) C(50) 109.1(6) . . . yes C(48) C(47) C(49) 107.6(6) . . . yes C(48) C(47) C(50) 110.7(7) . . . yes C(49) C(47) C(50) 108.1(6) . . . yes N(5) C(51) C(52) 121.6(5) . . . yes N(5) C(51) C(56) 120.4(4) . . . yes C(52) C(51) C(56) 118.0(4) . . . yes S(5) C(52) C(51) 121.8(4) . . . yes S(5) C(52) C(53) 118.2(4) . . . yes C(51) C(52) C(53) 120.0(5) . . . yes C(52) C(53) C(54) 123.0(5) . . . yes C(53) C(54) C(55) 116.3(5) . . . yes C(53) C(54) C(57) 123.7(5) . . . yes C(55) C(54) C(57) 119.9(5) . . . yes C(54) C(55) C(56) 122.2(5) . . . yes S(6) C(56) C(51) 121.2(3) . . . yes S(6) C(56) C(55) 118.3(4) . . . yes C(51) C(56) C(55) 120.5(4) . . . yes C(54) C(57) C(58) 108.4(5) . . . yes C(54) C(57) C(59) 108.9(5) . . . yes C(54) C(57) C(60) 112.3(6) . . . yes C(58) C(57) C(59) 109.6(7) . . . yes C(58) C(57) C(60) 108.1(5) . . . yes C(59) C(57) C(60) 109.5(6) . . . yes N(8) C(61) C(62) 124.4(4) . . . yes N(8) C(61) C(66) 120.2(4) . . . yes C(62) C(61) C(66) 115.2(4) . . . yes S(5) C(62) C(61) 119.3(3) . . . yes S(5) C(62) C(63) 119.8(3) . . . yes C(61) C(62) C(63) 120.9(4) . . . yes C(62) C(63) C(64) 123.3(4) . . . yes C(63) C(64) C(65) 116.5(4) . . . yes C(63) C(64) C(67) 121.4(4) . . . yes C(65) C(64) C(67) 122.1(4) . . . yes C(64) C(65) C(66) 120.6(4) . . . yes S(8) C(66) C(61) 116.2(3) . . . yes S(8) C(66) C(65) 120.2(3) . . . yes C(61) C(66) C(65) 123.5(4) . . . yes C(64) C(67) C(68) 107.7(5) . . . yes C(64) C(67) C(69) 110.7(5) . . . yes C(64) C(67) C(70) 110.3(5) . . . yes C(68) C(67) C(69) 109.2(6) . . . yes C(68) C(67) C(70) 111.7(7) . . . yes C(69) C(67) C(70) 107.3(6) . . . yes N(2) C(71) C(72) 124.9(4) . . . yes N(2) C(71) C(76) 119.0(4) . . . yes C(72) C(71) C(76) 115.9(4) . . . yes S(2) C(72) C(71) 119.6(3) . . . yes S(2) C(72) C(73) 119.9(4) . . . yes C(71) C(72) C(73) 120.4(4) . . . yes C(72) C(73) C(74) 123.0(5) . . . yes C(73) C(74) C(75) 116.0(4) . . . yes C(73) C(74) C(77) 120.3(5) . . . yes C(75) C(74) C(77) 123.7(5) . . . yes C(74) C(75) C(76) 122.0(4) . . . yes S(3) C(76) C(71) 117.3(3) . . . yes S(3) C(76) C(75) 120.0(4) . . . yes C(71) C(76) C(75) 122.7(4) . . . yes C(74) C(77) C(78) 113.6(7) . . . yes C(74) C(77) C(79) 107.9(6) . . . yes C(74) C(77) C(80) 112.3(6) . . . yes C(78) C(77) C(79) 108.0(9) . . . yes C(78) C(77) C(80) 111.4(9) . . . yes C(79) C(77) C(80) 102.9(9) . . . yes Cl(1) C(101) Cl(2) 110.1(6) . . . yes Cl(1) C(101) Cl(3) 111.4(5) . . . yes Cl(2) C(101) Cl(3) 112.7(5) . . . yes Cl(4) C(102) Cl(5) 106.9(7) . . . yes Cl(4) C(102) Cl(6) 117.0(10) . . . yes Cl(5) C(102) Cl(6) 114.2(8) . . . yes Cl(7) C(103) Cl(8) 111.2(6) . . . yes Cl(7) C(103) Cl(9) 109.5(5) . . . yes Cl(8) C(103) Cl(9) 110.4(5) . . . yes Cl(10) C(104) Cl(11) 107(1) . . . yes Cl(10) C(104) Cl(12) 121(1) . . . yes Cl(11) C(104) Cl(12) 110(1) . . . yes C(1) N(1) H(1) 116.2 . . . no C(1) N(1) H(2) 117.9 . . . no H(1) N(1) H(2) 125.5 . . . no Pd(1) N(2) H(6) 128.4 . . . no C(71) N(2) H(6) 111.0 . . . no C(21) N(3) H(3) 128.9 . . . no C(21) N(3) H(4) 121.1 . . . no H(3) N(3) H(4) 108.7 . . . no Pd(2) N(4) H(5) 121.8 . . . no C(11) N(4) H(5) 116.2 . . . no C(51) N(5) H(9) 125.5 . . . no C(51) N(5) H(10) 111.2 . . . no H(9) N(5) H(10) 122.1 . . . no Pd(2) N(6) H(12) 119.2 . . . no C(41) N(6) H(12) 120.3 . . . no C(31) N(7) H(7) 128.9 . . . no C(31) N(7) H(8) 123.9 . . . no H(7) N(7) H(8) 103.4 . . . no Pd(1) N(8) H(11) 112.7 . . . no C(61) N(8) H(11) 126.9 . . . no C(2) C(3) H(13) 118.2 . . . no C(4) C(3) H(13) 118.3 . . . no C(4) C(5) H(14) 118.2 . . . no C(6) C(5) H(14) 118.1 . . . no C(7) C(8) H(29) 108.3 . . . no C(7) C(8) H(30) 108.7 . . . no C(7) C(8) H(31) 107.9 . . . no H(29) C(8) H(30) 111.3 . . . no H(29) C(8) H(31) 110.1 . . . no H(30) C(8) H(31) 110.5 . . . no C(7) C(9) H(32) 108.6 . . . no C(7) C(9) H(33) 108.1 . . . no C(7) C(9) H(34) 108.8 . . . no H(32) C(9) H(33) 110.1 . . . no H(32) C(9) H(34) 110.7 . . . no H(33) C(9) H(34) 110.4 . . . no C(7) C(10) H(35) 109.4 . . . no C(7) C(10) H(36) 108.5 . . . no C(7) C(10) H(37) 108.9 . . . no H(35) C(10) H(36) 110.3 . . . no H(35) C(10) H(37) 110.2 . . . no H(36) C(10) H(37) 109.5 . . . no C(12) C(13) H(15) 119.6 . . . no C(14) C(13) H(15) 119.1 . . . no C(14) C(15) H(16) 118.3 . . . no C(16) C(15) H(16) 118.2 . . . no C(17) C(18) H(38) 109.2 . . . no C(17) C(18) H(39) 108.9 . . . no C(17) C(18) H(40) 109.1 . . . no H(38) C(18) H(39) 109.6 . . . no H(38) C(18) H(40) 110.1 . . . no H(39) C(18) H(40) 109.8 . . . no C(17) C(19) H(41) 109.0 . . . no C(17) C(19) H(42) 109.1 . . . no C(17) C(19) H(43) 108.6 . . . no H(41) C(19) H(42) 110.5 . . . no H(41) C(19) H(43) 109.6 . . . no H(42) C(19) H(43) 110.2 . . . no C(17) C(20) H(44) 109.3 . . . no C(17) C(20) H(45) 109.2 . . . no C(17) C(20) H(46) 109.1 . . . no H(44) C(20) H(45) 109.9 . . . no H(44) C(20) H(46) 109.6 . . . no H(45) C(20) H(46) 109.8 . . . no C(22) C(23) H(17) 118.5 . . . no C(24) C(23) H(17) 119.1 . . . no C(24) C(25) H(18) 119.3 . . . no C(26) C(25) H(18) 119.0 . . . no C(27) C(28) H(47) 108.2 . . . no C(27) C(28) H(48) 109.7 . . . no C(27) C(28) H(49) 108.5 . . . no H(47) C(28) H(48) 110.5 . . . no H(47) C(28) H(49) 108.8 . . . no H(48) C(28) H(49) 111.1 . . . no C(27) C(29) H(50) 112.8 . . . no C(27) C(29) H(51) 109.9 . . . no C(27) C(29) H(52) 113.4 . . . no H(50) C(29) H(51) 105.2 . . . no H(50) C(29) H(52) 109.3 . . . no H(51) C(29) H(52) 105.7 . . . no C(27) C(30) H(53) 107.3 . . . no C(27) C(30) H(54) 107.8 . . . no C(27) C(30) H(55) 109.4 . . . no H(53) C(30) H(54) 109.0 . . . no H(53) C(30) H(55) 111.4 . . . no H(54) C(30) H(55) 111.8 . . . no C(32) C(33) H(21) 118.7 . . . no C(34) C(33) H(21) 119.0 . . . no C(34) C(35) H(22) 118.9 . . . no C(36) C(35) H(22) 118.9 . . . no C(37) C(38) H(65) 109.0 . . . no C(37) C(38) H(66) 110.2 . . . no C(37) C(38) H(67) 108.1 . . . no H(65) C(38) H(66) 111.2 . . . no H(65) C(38) H(67) 108.4 . . . no H(66) C(38) H(67) 109.9 . . . no C(37) C(39) H(68) 109.6 . . . no C(37) C(39) H(69) 110.2 . . . no C(37) C(39) H(70) 108.7 . . . no H(68) C(39) H(69) 110.6 . . . no H(68) C(39) H(70) 108.4 . . . no H(69) C(39) H(70) 109.2 . . . no C(37) C(40) H(71) 107.6 . . . no C(37) C(40) H(72) 109.0 . . . no C(37) C(40) H(73) 108.0 . . . no H(71) C(40) H(72) 111.0 . . . no H(71) C(40) H(73) 109.5 . . . no H(72) C(40) H(73) 111.6 . . . no C(42) C(43) H(23) 119.3 . . . no C(44) C(43) H(23) 119.1 . . . no C(44) C(45) H(24) 118.4 . . . no C(46) C(45) H(24) 118.3 . . . no C(47) C(48) H(74) 108.8 . . . no C(47) C(48) H(75) 109.1 . . . no C(47) C(48) H(76) 108.4 . . . no H(74) C(48) H(75) 110.8 . . . no H(74) C(48) H(76) 109.3 . . . no H(75) C(48) H(76) 110.3 . . . no C(47) C(49) H(77) 108.8 . . . no C(47) C(49) H(78) 109.6 . . . no C(47) C(49) H(79) 109.1 . . . no H(77) C(49) H(78) 109.8 . . . no H(77) C(49) H(79) 109.0 . . . no H(78) C(49) H(79) 110.5 . . . no C(47) C(50) H(80) 109.0 . . . no C(47) C(50) H(81) 109.9 . . . no C(47) C(50) H(82) 109.8 . . . no H(80) C(50) H(81) 109.2 . . . no H(80) C(50) H(82) 109.1 . . . no H(81) C(50) H(82) 109.9 . . . no C(52) C(53) H(25) 118.6 . . . no C(54) C(53) H(25) 118.4 . . . no C(54) C(55) H(26) 119.2 . . . no C(56) C(55) H(26) 118.6 . . . no C(57) C(58) H(83) 109.5 . . . no C(57) C(58) H(84) 108.3 . . . no C(57) C(58) H(85) 108.2 . . . no H(83) C(58) H(84) 110.9 . . . no H(83) C(58) H(85) 110.6 . . . no H(84) C(58) H(85) 109.3 . . . no C(57) C(59) H(86) 107.3 . . . no C(57) C(59) H(87) 108.1 . . . no C(57) C(59) H(88) 110.2 . . . no H(86) C(59) H(87) 108.2 . . . no H(86) C(59) H(88) 110.7 . . . no H(87) C(59) H(88) 112.1 . . . no C(57) C(60) H(89) 109.3 . . . no C(57) C(60) H(90) 108.5 . . . no C(57) C(60) H(91) 109.5 . . . no H(89) C(60) H(90) 109.3 . . . no H(89) C(60) H(91) 110.5 . . . no H(90) C(60) H(91) 109.7 . . . no C(62) C(63) H(27) 118.2 . . . no C(64) C(63) H(27) 118.4 . . . no C(64) C(65) H(28) 119.8 . . . no C(66) C(65) H(28) 119.6 . . . no C(67) C(68) H(92) 109.9 . . . no C(67) C(68) H(93) 109.2 . . . no C(67) C(68) H(94) 108.7 . . . no H(92) C(68) H(93) 110.1 . . . no H(92) C(68) H(94) 109.8 . . . no H(93) C(68) H(94) 109.0 . . . no C(67) C(69) H(95) 109.2 . . . no C(67) C(69) H(96) 109.6 . . . no C(67) C(69) H(97) 109.0 . . . no H(95) C(69) H(96) 109.8 . . . no H(95) C(69) H(97) 109.1 . . . no H(96) C(69) H(97) 110.1 . . . no C(67) C(70) H(98) 108.3 . . . no C(67) C(70) H(99) 109.4 . . . no C(67) C(70) H(100) 108.7 . . . no H(98) C(70) H(99) 110.2 . . . no H(98) C(70) H(100) 109.1 . . . no H(99) C(70) H(100) 111.1 . . . no C(72) C(73) H(19) 118.3 . . . no C(74) C(73) H(19) 118.7 . . . no C(74) C(75) H(20) 119.0 . . . no C(76) C(75) H(20) 119.1 . . . no C(77) C(78) H(56) 107.2 . . . no C(77) C(78) H(57) 105.7 . . . no C(77) C(78) H(58) 111.6 . . . no H(56) C(78) H(57) 106.1 . . . no H(56) C(78) H(58) 114.0 . . . no H(57) C(78) H(58) 111.7 . . . no C(77) C(79) H(59) 107.8 . . . no C(77) C(79) H(60) 109.4 . . . no C(77) C(79) H(61) 106.7 . . . no H(59) C(79) H(60) 112.6 . . . no H(59) C(79) H(61) 108.8 . . . no H(60) C(79) H(61) 111.3 . . . no C(77) C(80) H(62) 109.8 . . . no C(77) C(80) H(63) 107.1 . . . no C(77) C(80) H(64) 107.2 . . . no H(62) C(80) H(63) 112.0 . . . no H(62) C(80) H(64) 112.0 . . . no H(63) C(80) H(64) 108.5 . . . no Cl(1) C(101) H(101) 108.9 . . . no Cl(2) C(101) H(101) 105.5 . . . no Cl(3) C(101) H(101) 107.9 . . . no Cl(4) C(102) H(102) 108.5 . . . no Cl(5) C(102) H(102) 104.3 . . . no Cl(6) C(102) H(102) 105.1 . . . no Cl(7) C(103) H(103) 110.0 . . . no Cl(8) C(103) H(103) 108.1 . . . no Cl(9) C(103) H(103) 107.5 . . . no Cl(10) C(104) H(104) 89.3 . . . no Cl(11) C(104) H(104) 112.5 . . . no Cl(12) C(104) H(104) 114.6 . . . no #------------------------------------------------------------------------------