Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bin, Zhang' 'Dao-Ben, Zhu' 'Mak, Thomas C. W.' 'Min-Hua, Jiang' 'Qi, Fang' 'Qing-Chuan, Yang' 'Zhi, Liu' 'Zhong-Yuan, Zhou' _publ_contact_author_name 'Prof Fang Qi' _publ_contact_author_address ; State Key Laboratory Of Crystal Materials Shandong University Jinan Shandong 250100 CHINA ; _publ_contact_author_email 'FANGQI@ICM.SDU.EDU.CN' _publ_section_title ; Syntheses and Crystal Structrues of Molecular Conductors Z[Pd(dmit)2}2 (Z = (Me3NEt)+, (MeNEt3)+, (NEt4)+) and Their Precursors Z2[Pd(dmit)2] ; data_fa1 _database_code_CSD 168855 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Me3NEt)2[Pd(dmit)2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H28 N2 Pd S10' _chemical_formula_weight 675.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.471(3) _cell_length_b 10.522(3) _cell_length_c 12.358(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.760(15) _cell_angle_gamma 90.00 _cell_volume 1385.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 1.432 _exptl_absorpt_correction_type 'abscor' _exptl_absorpt_correction_T_min 0.6571 _exptl_absorpt_correction_T_max 0.9583 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IP Rigaku' _diffrn_measurement_method 'IP' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2047 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0931 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2047 _reflns_number_gt 1741 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAXIS Rigaku' _computing_cell_refinement 'BIOTEX Rigaku' _computing_data_reduction 'BIOTEX Rigaku' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0941P)^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 SHELXL _refine_ls_extinction_coef 0.0066(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2047 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.2004 _refine_ls_wR_factor_gt 0.1856 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.002 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 Pd1 Pd 0.0000 0.0000 0.5000 0.06213(11) Uani 1 2 d S . . N1 N 0.2698(2) 0.7857(3) 0.4122(2) 0.0796(10) Uani 1 1 d . . . C1 C 0.2128(3) 0.1906(3) 0.6463(3) 0.0629(10) Uani 1 1 d . . . C2 C 0.1922(3) 0.2255(3) 0.5337(2) 0.0629(10) Uani 1 1 d . . . C3 C 0.3602(3) 0.3891(3) 0.6618(2) 0.0631(10) Uani 1 1 d . . . C4 C 0.1961(3) 0.7306(4) 0.4798(3) 0.1070(16) Uani 1 1 d . . . H4A H 0.2539 0.6844 0.5459 0.128 Uiso 1 1 calc R . . H4B H 0.1625 0.8004 0.5105 0.128 Uiso 1 1 calc R . . C5 C 0.1884(3) 0.8467(4) 0.3018(3) 0.0953(15) Uani 1 1 d . . . H5A H 0.1366 0.9098 0.3181 0.143 Uiso 1 1 calc R . . H5B H 0.1361 0.7835 0.2505 0.143 Uiso 1 1 calc R . . H5C H 0.2398 0.8864 0.2653 0.143 Uiso 1 1 calc R . . C6 C 0.3498(3) 0.6852(4) 0.3875(3) 0.0945(14) Uani 1 1 d . . . H6A H 0.3953 0.7217 0.3438 0.142 Uiso 1 1 calc R . . H6B H 0.2971 0.6178 0.3432 0.142 Uiso 1 1 calc R . . H6C H 0.4079 0.6519 0.4597 0.142 Uiso 1 1 calc R . . C7 C 0.3574(4) 0.8883(4) 0.4873(4) 0.137(2) Uani 1 1 d . . . H7A H 0.3086 0.9528 0.5059 0.206 Uiso 1 1 calc R . . H7B H 0.4042 0.9257 0.4452 0.206 Uiso 1 1 calc R . . H7C H 0.4143 0.8508 0.5579 0.206 Uiso 1 1 calc R . . C8 C 0.0922(4) 0.6454(4) 0.4164(3) 0.1094(17) Uani 1 1 d . . . H8A H 0.0491 0.6205 0.4664 0.164 Uiso 1 1 calc R . . H8B H 0.1245 0.5713 0.3918 0.164 Uiso 1 1 calc R . . H8C H 0.0349 0.6886 0.3493 0.164 Uiso 1 1 calc R . . S1 S 0.13545(8) 0.06594(9) 0.68191(7) 0.0735(3) Uani 1 1 d . . . S2 S 0.08296(8) 0.15118(8) 0.41217(7) 0.0727(3) Uani 1 1 d . . . S3 S 0.32099(8) 0.28566(9) 0.75126(7) 0.0756(3) Uani 1 1 d . . . S4 S 0.28139(9) 0.35390(9) 0.51720(7) 0.0754(3) Uani 1 1 d . . . S5 S 0.46101(10) 0.51038(8) 0.70904(9) 0.0816(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.06007(17) 0.05047(18) 0.07465(18) 0.00231(15) 0.02358(15) 0.00467(15) N1 0.0726(15) 0.0809(18) 0.0868(14) -0.0176(14) 0.0311(12) 0.0059(15) C1 0.0504(15) 0.0601(18) 0.0774(15) 0.0096(14) 0.0227(12) 0.0074(14) C2 0.0606(16) 0.0557(17) 0.0686(15) -0.0001(14) 0.0195(13) -0.0021(15) C3 0.0530(15) 0.0610(19) 0.0734(16) 0.0004(14) 0.0213(13) 0.0075(14) C4 0.101(2) 0.108(3) 0.119(2) 0.013(2) 0.048(2) 0.040(2) C5 0.085(2) 0.106(3) 0.0765(19) 0.003(2) 0.0095(18) -0.003(2) C6 0.074(2) 0.096(3) 0.123(2) -0.022(2) 0.0475(17) 0.006(2) C7 0.119(3) 0.121(4) 0.126(3) -0.045(3) -0.007(3) 0.003(3) C8 0.109(3) 0.093(3) 0.137(3) 0.016(3) 0.057(2) 0.015(3) S1 0.0751(5) 0.0651(5) 0.0753(4) 0.0056(4) 0.0219(4) -0.0088(4) S2 0.0776(5) 0.0650(5) 0.0716(4) 0.0024(4) 0.0231(4) -0.0089(4) S3 0.0749(5) 0.0696(5) 0.0754(4) -0.0006(4) 0.0198(4) -0.0077(4) S4 0.0854(5) 0.0639(5) 0.0771(4) 0.0005(4) 0.0306(4) -0.0095(5) S5 0.0794(5) 0.0648(5) 0.0969(6) -0.0064(4) 0.0284(5) -0.0083(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S1 2.3151(9) . ? Pd1 S1 2.3151(9) 3_556 ? Pd1 S2 2.3195(10) 3_556 ? Pd1 S2 2.3195(10) . ? N1 C5 1.484(4) . ? N1 C6 1.504(5) . ? N1 C4 1.508(5) . ? N1 C7 1.531(5) . ? C1 C2 1.372(4) . ? C1 S1 1.730(3) . ? C1 S3 1.740(3) . ? C2 S2 1.744(3) . ? C2 S4 1.751(3) . ? C3 S5 1.675(3) . ? C3 S4 1.717(3) . ? C3 S3 1.726(3) . ? C4 C8 1.465(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Pd1 S1 180.0 . 3_556 ? S1 Pd1 S2 89.73(3) . 3_556 ? S1 Pd1 S2 90.27(3) 3_556 3_556 ? S1 Pd1 S2 90.27(3) . . ? S1 Pd1 S2 89.73(3) 3_556 . ? S2 Pd1 S2 180.0 3_556 . ? C5 N1 C6 109.9(3) . . ? C5 N1 C4 112.6(3) . . ? C6 N1 C4 110.6(3) . . ? C5 N1 C7 107.5(3) . . ? C6 N1 C7 107.8(3) . . ? C4 N1 C7 108.2(3) . . ? C2 C1 S1 123.3(2) . . ? C2 C1 S3 114.2(2) . . ? S1 C1 S3 122.50(18) . . ? C1 C2 S2 123.5(2) . . ? C1 C2 S4 115.8(2) . . ? S2 C2 S4 120.66(17) . . ? S5 C3 S4 123.8(2) . . ? S5 C3 S3 124.55(17) . . ? S4 C3 S3 111.66(16) . . ? C8 C4 N1 116.8(3) . . ? C1 S1 Pd1 101.72(10) . . ? C2 S2 Pd1 101.14(11) . . ? C3 S3 C1 99.65(15) . . ? C3 S4 C2 98.63(15) . . ? _diffrn_measured_fraction_theta_max 0.837 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.837 _refine_diff_density_max 0.565 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.110 #===END data_m3epd2 #(CIF file of (Me3NEt)[Pd(dmit)2]2) _database_code_CSD 168856 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Me3NEt)[Pd(dmit)2]2)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 N Pd2 S20' _chemical_formula_weight 1086.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 6.2647(5) _cell_length_b 36.486(3) _cell_length_c 7.7255(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.976(2) _cell_angle_gamma 90.00 _cell_volume 1669.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description PLATE _exptl_crystal_colour BLACK _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1070 _exptl_absorpt_coefficient_mu 2.346 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8346 _exptl_absorpt_correction_T_max 0.9546 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER CCD AREA DETECTOR' _diffrn_measurement_method 'PHI AND OMEGA SCAN' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3861 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3861 _reflns_number_gt 3398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction SHELXTL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+3.9088P] 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 3861 _refine_ls_number_parameters 184 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 Pd1 Pd 0.479850(19) 0.518823(3) 0.811790(16) 0.02462(3) Uani 1 1 d . . . S1 S 0.78680(7) 0.484696(12) 0.80655(6) 0.03075(11) Uani 1 1 d . . . S2 S 0.24254(7) 0.474720(12) 0.64013(6) 0.03266(12) Uani 1 1 d . . . S3 S 0.81719(8) 0.411042(13) 0.64295(7) 0.03542(12) Uani 1 1 d . . . S4 S 0.33174(8) 0.403038(13) 0.49301(6) 0.03541(12) Uani 1 1 d . . . S5 S 0.62416(11) 0.342832(15) 0.44267(8) 0.05375(16) Uani 1 1 d . . . S6 S 0.71233(7) 0.565888(12) 0.96448(6) 0.02916(11) Uani 1 1 d . . . S7 S 0.16693(7) 0.553127(12) 0.79787(6) 0.02986(11) Uani 1 1 d . . . S8 S 0.60127(8) 0.641150(13) 1.06732(7) 0.03950(14) Uani 1 1 d . . . S9 S 0.12011(8) 0.630321(13) 0.91395(7) 0.03627(12) Uani 1 1 d . . . S10 S 0.29316(12) 0.702430(16) 1.07970(10) 0.0651(2) Uani 1 1 d . . . C1 C 0.6594(3) 0.44721(4) 0.6857(2) 0.0260(4) Uani 1 1 d . . . C2 C 0.4288(3) 0.44334(4) 0.6153(2) 0.0259(4) Uani 1 1 d . . . C3 C 0.5928(3) 0.38344(5) 0.5234(2) 0.0335(5) Uani 1 1 d . . . C4 C 0.5167(3) 0.59796(4) 0.9706(2) 0.0266(4) Uani 1 1 d . . . C5 C 0.2872(3) 0.59281(4) 0.8988(2) 0.0266(4) Uani 1 1 d . . . C6 C 0.3372(3) 0.65987(5) 1.0232(3) 0.0382(5) Uani 1 1 d . . . N1 N 0.0785(3) 0.2500 0.5133(3) 0.0661(11) Uani 1 2 d SD . . C7 C -0.1771(6) 0.2500 0.4223(11) 0.071(2) Uiso 0.50 2 d SPD A 1 C8 C 0.111(2) 0.2500 0.7178(5) 0.154(6) Uiso 0.50 2 d SPD A 1 C9 C 0.1531(10) 0.20960(9) 0.5225(10) 0.092(2) Uiso 0.50 1 d PD . . C10 C 0.2259(6) 0.27428(13) 0.4391(5) 0.093(2) Uiso 0.50 1 d PD . . C11 C 0.2444(9) 0.25840(17) 0.2603(5) 0.091(2) Uiso 0.50 1 d PD . . C7' C -0.1587(10) 0.2500 0.3714(9) 0.0474(15) Uiso 0.50 2 d SPD A 2 C8' C 0.110(3) 0.2500 0.7143(13) 0.142(6) Uiso 0.50 2 d SPD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02525(5) 0.01899(5) 0.02956(5) -0.00352(5) 0.00881(4) 0.00008(4) S1 0.02565(16) 0.02180(18) 0.0442(2) -0.00794(17) 0.01058(15) -0.00088(15) S2 0.02623(17) 0.02533(19) 0.0433(2) -0.00988(17) 0.00698(15) -0.00008(15) S3 0.03674(19) 0.0271(2) 0.0438(2) -0.00554(18) 0.01491(16) 0.00519(17) S4 0.0398(2) 0.0256(2) 0.0373(2) -0.00967(17) 0.00773(17) -0.00398(17) S5 0.0816(3) 0.0253(2) 0.0617(3) -0.0117(2) 0.0335(2) 0.0032(2) S6 0.02702(16) 0.02270(18) 0.03696(19) -0.00487(16) 0.00930(14) -0.00085(15) S7 0.02675(16) 0.02178(18) 0.03910(19) -0.00681(16) 0.00804(14) 0.00067(15) S8 0.0430(2) 0.02229(19) 0.0451(2) -0.00813(19) 0.0032(2) -0.00175(18) S9 0.03908(19) 0.0235(2) 0.0463(2) -0.00225(18) 0.01397(17) 0.00659(17) S10 0.0771(4) 0.0275(2) 0.0777(4) -0.0158(3) 0.0070(3) 0.0133(3) C1 0.0361(7) 0.0157(7) 0.0282(7) 0.0016(6) 0.0130(5) 0.0055(6) C2 0.0379(7) 0.0150(7) 0.0255(6) -0.0011(6) 0.0114(5) -0.0008(6) C3 0.0496(9) 0.0251(8) 0.0283(7) 0.0039(6) 0.0161(6) 0.0021(7) C4 0.0374(7) 0.0169(7) 0.0240(7) 0.0002(6) 0.0078(6) 0.0018(6) C5 0.0379(7) 0.0161(7) 0.0275(7) -0.0013(6) 0.0128(5) 0.0020(6) C6 0.0497(10) 0.0284(9) 0.0332(8) -0.0012(7) 0.0088(7) 0.0068(8) N1 0.0440(13) 0.073(2) 0.0765(19) 0.000 0.0131(13) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S2 2.2970(4) . ? Pd1 S7 2.2986(5) . ? Pd1 S1 2.3023(5) . ? Pd1 S6 2.3117(4) . ? Pd1 Pd1 3.1511(3) 3_667 ? S1 C1 1.7013(16) . ? S2 C2 1.6896(18) . ? S3 C3 1.7317(18) . ? S3 C1 1.7437(18) . ? S4 C3 1.730(2) . ? S4 C2 1.7468(16) . ? S5 C3 1.6439(19) . ? S6 C4 1.7064(18) . ? S7 C5 1.7002(16) . ? S8 C6 1.718(2) . ? S8 C4 1.7504(16) . ? S9 C6 1.726(2) . ? S9 C5 1.7499(18) . ? S10 C6 1.660(2) . ? C1 C2 1.375(2) . ? C4 C5 1.375(2) . ? N1 C8' 1.500(11) . ? N1 C10 1.520(4) 4_565 ? N1 C10 1.520(4) . ? N1 C7 1.525(4) . ? N1 C8 1.526(5) . ? N1 C9 1.541(4) 4_565 ? N1 C9 1.541(4) . ? N1 C7' 1.533(6) . ? C9 C10 1.077(8) 4_565 ? C10 C9 1.077(8) 4_565 ? C10 C11 1.537(5) . ? C10 C10 1.772(9) 4_565 ? C10 C11 1.857(7) 4_565 ? C11 C11 0.613(13) 4_565 ? C11 C10 1.857(7) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Pd1 S7 88.419(17) . . ? S2 Pd1 S1 89.911(17) . . ? S7 Pd1 S1 176.500(17) . . ? S2 Pd1 S6 175.623(17) . . ? S7 Pd1 S6 90.321(16) . . ? S1 Pd1 S6 91.117(17) . . ? S2 Pd1 Pd1 94.017(15) . 3_667 ? S7 Pd1 Pd1 95.262(14) . 3_667 ? S1 Pd1 Pd1 87.922(13) . 3_667 ? S6 Pd1 Pd1 90.272(13) . 3_667 ? C1 S1 Pd1 101.47(6) . . ? C2 S2 Pd1 101.48(6) . . ? C3 S3 C1 97.43(9) . . ? C3 S4 C2 97.30(8) . . ? C4 S6 Pd1 100.64(6) . . ? C5 S7 Pd1 101.43(6) . . ? C6 S8 C4 97.75(9) . . ? C6 S9 C5 97.33(9) . . ? C2 C1 S1 123.00(13) . . ? C2 C1 S3 115.76(12) . . ? S1 C1 S3 121.24(9) . . ? C1 C2 S2 124.12(12) . . ? C1 C2 S4 115.88(13) . . ? S2 C2 S4 120.00(10) . . ? S5 C3 S4 123.06(11) . . ? S5 C3 S3 123.37(12) . . ? S4 C3 S3 113.56(10) . . ? C5 C4 S6 124.13(13) . . ? C5 C4 S8 115.27(13) . . ? S6 C4 S8 120.58(10) . . ? C4 C5 S7 123.42(13) . . ? C4 C5 S9 115.84(12) . . ? S7 C5 S9 120.74(10) . . ? S10 C6 S8 123.46(12) . . ? S10 C6 S9 122.74(12) . . ? S8 C6 S9 113.80(11) . . ? C8' N1 C10 120.0(5) . 4_565 ? C8' N1 C10 120.0(5) . . ? C10 N1 C10 71.3(4) 4_565 . ? C8' N1 C7 104.0(7) . . ? C10 N1 C7 120.1(3) 4_565 . ? C10 N1 C7 120.1(3) . . ? C8' N1 C8 0.1(8) . . ? C10 N1 C8 119.9(4) 4_565 . ? C10 N1 C8 119.9(4) . . ? C7 N1 C8 104.1(6) . . ? C8' N1 C9 91.0(3) . 4_565 ? C10 N1 C9 111.3(4) 4_565 4_565 ? C10 N1 C9 41.2(3) . 4_565 ? C7 N1 C9 106.2(2) . 4_565 ? C8 N1 C9 90.9(3) . 4_565 ? C8' N1 C9 91.0(3) . . ? C10 N1 C9 41.2(3) 4_565 . ? C10 N1 C9 111.3(4) . . ? C7 N1 C9 106.2(2) . . ? C8 N1 C9 90.9(3) . . ? C9 N1 C9 146.1(5) 4_565 . ? C8' N1 C7' 120.7(7) . . ? C10 N1 C7' 107.2(3) 4_565 . ? C10 N1 C7' 107.2(3) . . ? C7 N1 C7' 16.7(4) . . ? C8 N1 C7' 120.8(6) . . ? C9 N1 C7' 104.0(2) 4_565 . ? C9 N1 C7' 104.0(2) . . ? C10 C9 N1 68.4(3) 4_565 . ? C9 C10 N1 70.4(3) 4_565 . ? C9 C10 C11 156.1(5) 4_565 . ? N1 C10 C11 110.6(4) . . ? C9 C10 C10 123.1(3) 4_565 4_565 ? N1 C10 C10 54.35(18) . 4_565 ? C11 C10 C10 67.8(3) . 4_565 ? C9 C10 C11 159.5(5) 4_565 4_565 ? N1 C10 C11 95.7(3) . 4_565 ? C11 C10 C11 17.8(4) . 4_565 ? C10 C10 C11 50.1(2) 4_565 4_565 ? C11 C11 C10 112.2(3) 4_565 . ? C11 C11 C10 50.1(2) 4_565 4_565 ? C10 C11 C10 62.1(3) . 4_565 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.874 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.129 #===END data_me32.pd #(CIF file of (MeNEt3)2[Pd(dmit)2]) _database_code_CSD 168857 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(MeNEt3)2[Pd(dmit)2]' _chemical_melting_point ? _chemical_formula_moiety 'Pd C6 S10 (N C7 H18 )2' _chemical_formula_sum 'C20 H36 N2 Pd S10' _chemical_formula_weight 731.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.410(2) _cell_length_b 12.937(3) _cell_length_c 23.445(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3157.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type 'abscor' _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 1.153 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IP Rigaku' _diffrn_measurement_method 'IP' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8289 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.46 _reflns_number_total 2746 _reflns_number_gt 2416 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAXIS Rigaku' _computing_cell_refinement 'BIOTEX Rigaku' _computing_data_reduction 'BIOTEX Rigaku' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+1.6674P] 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 SHELXL _refine_ls_extinction_coef 0.0016(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2746 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.0000 0.0000 0.0000 0.0670(2) Uani 1 2 d S . . S1 S 0.03102(13) -0.11908(11) 0.07237(6) 0.0807(4) Uani 1 1 d . . . S2 S 0.17204(13) 0.09659(11) 0.03261(6) 0.0786(4) Uani 1 1 d . . . S3 S 0.22083(14) -0.12010(11) 0.17001(6) 0.0818(4) Uani 1 1 d . . . S4 S 0.34164(14) 0.06800(11) 0.13591(6) 0.0831(4) Uani 1 1 d . . . S5 S 0.43994(18) -0.04116(13) 0.23961(7) 0.0973(5) Uani 1 1 d . . . C1 C 0.1580(4) -0.0628(4) 0.1085(2) 0.0688(12) Uani 1 1 d . . . C2 C 0.2161(5) 0.0261(4) 0.0921(2) 0.0693(12) Uani 1 1 d . . . C3 C 0.3385(5) -0.0318(4) 0.1851(2) 0.0772(13) Uani 1 1 d . . . N1 N 0.8425(4) 0.2359(3) 0.13088(16) 0.0767(11) Uani 1 1 d . . . C4 C 0.9642(6) 0.2087(5) 0.1635(3) 0.106(2) Uani 1 1 d . . . H4A H 1.0314 0.1919 0.1371 0.160 Uiso 1 1 calc R . . H4B H 0.9480 0.1504 0.1878 0.160 Uiso 1 1 calc R . . H4C H 0.9900 0.2667 0.1864 0.160 Uiso 1 1 calc R . . C5 C 0.8645(6) 0.3373(5) 0.0993(3) 0.1017(18) Uani 1 1 d . . . H5A H 0.7853 0.3561 0.0801 0.122 Uiso 1 1 calc R . . H5B H 0.8824 0.3906 0.1272 0.122 Uiso 1 1 calc R . . C6 C 0.9689(6) 0.3376(6) 0.0568(3) 0.111(2) Uani 1 1 d . . . H6A H 0.9742 0.4045 0.0393 0.167 Uiso 1 1 calc R . . H6B H 0.9515 0.2865 0.0281 0.167 Uiso 1 1 calc R . . H6C H 1.0488 0.3218 0.0753 0.167 Uiso 1 1 calc R . . C7 C 0.7362(6) 0.2611(5) 0.1721(2) 0.0981(18) Uani 1 1 d . . . H7A H 0.7646 0.3177 0.1962 0.118 Uiso 1 1 calc R . . H7B H 0.6628 0.2855 0.1505 0.118 Uiso 1 1 calc R . . C8 C 0.6929(7) 0.1754(7) 0.2096(3) 0.138(3) Uani 1 1 d . . . H8A H 0.6267 0.2000 0.2347 0.207 Uiso 1 1 calc R . . H8B H 0.7641 0.1506 0.2317 0.207 Uiso 1 1 calc R . . H8C H 0.6596 0.1201 0.1865 0.207 Uiso 1 1 calc R . . C9 C 0.8122(6) 0.1448(5) 0.0949(3) 0.1022(19) Uani 1 1 d . . . H9A H 0.8848 0.1321 0.0700 0.123 Uiso 1 1 calc R . . H9B H 0.8034 0.0851 0.1196 0.123 Uiso 1 1 calc R . . C10 C 0.6953(6) 0.1524(6) 0.0593(3) 0.121(2) Uani 1 1 d . . . H10A H 0.6857 0.0903 0.0373 0.182 Uiso 1 1 calc R . . H10B H 0.7027 0.2105 0.0341 0.182 Uiso 1 1 calc R . . H10C H 0.6216 0.1613 0.0835 0.182 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0640(4) 0.0708(4) 0.0663(4) -0.0001(2) 0.0091(2) 0.0010(2) S1 0.0772(8) 0.0834(9) 0.0814(9) 0.0129(7) -0.0060(7) -0.0162(7) S2 0.0756(8) 0.0775(8) 0.0829(9) 0.0111(7) -0.0003(6) -0.0084(6) S3 0.0810(9) 0.0846(9) 0.0800(8) 0.0114(7) -0.0046(7) -0.0067(7) S4 0.0788(9) 0.0774(8) 0.0931(10) 0.0008(7) -0.0087(7) -0.0086(7) S5 0.1002(11) 0.0956(10) 0.0961(11) -0.0019(9) -0.0239(9) -0.0019(9) C1 0.062(3) 0.071(3) 0.074(3) 0.002(2) 0.001(2) -0.003(2) C2 0.063(3) 0.074(3) 0.071(3) -0.004(2) 0.003(2) 0.002(2) C3 0.075(3) 0.079(3) 0.078(3) -0.009(3) -0.001(3) 0.002(3) N1 0.076(3) 0.080(3) 0.073(2) 0.006(2) 0.000(2) 0.004(2) C4 0.087(4) 0.121(5) 0.112(5) 0.031(4) -0.015(4) 0.006(4) C5 0.104(4) 0.107(4) 0.094(4) 0.018(4) -0.010(4) 0.010(4) C6 0.100(4) 0.123(5) 0.111(5) 0.035(4) 0.008(4) 0.001(4) C7 0.101(4) 0.107(4) 0.087(4) -0.012(3) 0.010(3) 0.019(4) C8 0.126(6) 0.175(8) 0.113(5) 0.022(5) 0.040(5) 0.003(5) C9 0.097(4) 0.115(5) 0.094(4) -0.023(4) 0.003(3) 0.016(4) C10 0.108(5) 0.132(5) 0.123(5) -0.021(5) -0.022(4) 0.022(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S2 2.3138(14) . ? Pd1 S2 2.3138(14) 5 ? Pd1 S1 2.3143(14) . ? Pd1 S1 2.3143(14) 5 ? S1 C1 1.731(5) . ? S2 C2 1.728(5) . ? S3 C3 1.712(5) . ? S3 C1 1.748(5) . ? S4 C3 1.730(6) . ? S4 C2 1.749(5) . ? S5 C3 1.663(5) . ? C1 C2 1.355(7) . ? N1 C9 1.482(7) . ? N1 C7 1.506(6) . ? N1 C4 1.521(7) . ? N1 C5 1.524(7) . ? C5 C6 1.474(8) . ? C7 C8 1.484(8) . ? C9 C10 1.479(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Pd1 S2 180.00(10) . 5 ? S2 Pd1 S1 90.53(5) . . ? S2 Pd1 S1 89.47(5) 5 . ? S2 Pd1 S1 89.47(5) . 5 ? S2 Pd1 S1 90.53(5) 5 5 ? S1 Pd1 S1 180.00(7) . 5 ? C1 S1 Pd1 100.70(17) . . ? C2 S2 Pd1 100.77(17) . . ? C3 S3 C1 98.9(2) . . ? C3 S4 C2 98.4(2) . . ? C2 C1 S1 123.9(4) . . ? C2 C1 S3 115.3(4) . . ? S1 C1 S3 120.8(3) . . ? C1 C2 S2 124.0(4) . . ? C1 C2 S4 115.4(4) . . ? S2 C2 S4 120.6(3) . . ? S5 C3 S3 124.3(3) . . ? S5 C3 S4 123.7(3) . . ? S3 C3 S4 112.0(3) . . ? C9 N1 C7 112.4(4) . . ? C9 N1 C4 106.3(5) . . ? C7 N1 C4 109.8(4) . . ? C9 N1 C5 116.1(4) . . ? C7 N1 C5 103.7(4) . . ? C4 N1 C5 108.6(4) . . ? C6 C5 N1 116.2(5) . . ? C8 C7 N1 116.2(5) . . ? C10 C9 N1 116.3(5) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 25.46 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.442 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.065 #===END data_me3pd2 #(CIF file of (MeNEt3)[Pd(dmit)2]2) _database_code_CSD 168858 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(MeNEt3)[Pd(dmit)2]2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H18 N Pd2 S20' _chemical_formula_weight 1114.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 6.222(3) _cell_length_b 7.838(3) _cell_length_c 18.622(9) _cell_angle_alpha 84.981(13) _cell_angle_beta 83.699(13) _cell_angle_gamma 73.128(12) _cell_volume 862.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description PLATE _exptl_crystal_colour BLACK _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 551 _exptl_absorpt_coefficient_mu 2.274 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.843 _exptl_absorpt_correction_T_max 0.852 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER CCD AREA DETECTOR' _diffrn_measurement_method 'PHI AND OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4543 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1055 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.67 _reflns_number_total 4471 _reflns_number_gt 2826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction SHELXTL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 SHELXL _refine_ls_extinction_coef 0.00000(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.31(16) _refine_ls_number_reflns 4471 _refine_ls_number_parameters 380 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1465 _refine_ls_R_factor_gt 0.0945 _refine_ls_wR_factor_ref 0.2426 _refine_ls_wR_factor_gt 0.2229 _refine_ls_goodness_of_fit_ref 1.334 _refine_ls_restrained_S_all 1.339 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.007 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 Pd1 Pd 0.19436(3) 0.26793(3) 0.357836(16) 0.02459(7) Uani 1 1 d . . . Pd2 Pd 0.21059(3) -0.11072(3) 0.432454(16) 0.02964(8) Uani 1 1 d . . . S1 S -0.09729(16) 0.28723(12) 0.28837(5) 0.0302(3) Uani 1 1 d . . . S2 S 0.44768(15) 0.12252(11) 0.26676(5) 0.0288(3) Uani 1 1 d . . . S3 S -0.09866(17) 0.16959(13) 0.13811(6) 0.0390(3) Uani 1 1 d . . . S4 S 0.37434(19) 0.01873(13) 0.12099(5) 0.0364(3) Uani 1 1 d . . . S5 S 0.1149(3) -0.00264(18) 0.00097(7) 0.0700(5) Uani 1 1 d . . . S6 S -0.06162(17) 0.43264(13) 0.44074(6) 0.0360(3) Uani 1 1 d . . . S7 S 0.47810(15) 0.26994(11) 0.42527(5) 0.0291(3) Uani 1 1 d . . . S8 S -0.0157(2) 0.56716(14) 0.57756(7) 0.0458(4) Uani 1 1 d . . . S9 S 0.4753(2) 0.41115(16) 0.56843(7) 0.0516(4) Uani 1 1 d . . . S10 S 0.2811(3) 0.5922(2) 0.69925(9) 0.0930(7) Uani 1 1 d . . . S11 S -0.08073(16) -0.10312(11) 0.36479(5) 0.0287(3) Uani 1 1 d . . . S12 S 0.46628(17) -0.27356(12) 0.34675(7) 0.0360(3) Uani 1 1 d . . . S13 S -0.07403(17) -0.26214(11) 0.22183(6) 0.0313(3) Uani 1 1 d . . . S14 S 0.3990(2) -0.41382(12) 0.20795(6) 0.0394(3) Uani 1 1 d . . . S15 S 0.1612(2) -0.46441(13) 0.09311(6) 0.0474(4) Uani 1 1 d . . . S16 S -0.04182(17) 0.03104(12) 0.52247(6) 0.0343(3) Uani 1 1 d . . . S17 S 0.50519(18) -0.13228(14) 0.49807(7) 0.0423(3) Uani 1 1 d . . . S18 S 0.0330(2) 0.10409(16) 0.66939(7) 0.0526(4) Uani 1 1 d . . . S19 S 0.5260(2) -0.04337(18) 0.64906(7) 0.0581(4) Uani 1 1 d . . . S20 S 0.3251(3) 0.1032(2) 0.78872(7) 0.0709(5) Uani 1 1 d . . . C1 C 0.0366(6) 0.2040(4) 0.21522(19) 0.0219(10) Uani 1 1 d . . . C2 C 0.2409(9) 0.1250(5) 0.2055(2) 0.0460(16) Uani 1 1 d . . . C3 C 0.1689(12) 0.0797(8) 0.0775(4) 0.111(3) Uani 1 1 d . . . C4 C 0.1077(6) 0.4523(4) 0.5050(2) 0.0281(11) Uani 1 1 d . . . C5 C 0.3499(7) 0.3711(4) 0.4972(2) 0.0306(12) Uani 1 1 d . . . C6 C 0.2542(8) 0.5334(4) 0.6251(2) 0.0387(13) Uani 1 1 d . . . C7 C 0.0741(6) -0.2282(4) 0.29561(18) 0.0202(9) Uani 1 1 d . . . C8 C 0.2857(7) -0.2867(4) 0.2879(2) 0.0308(11) Uani 1 1 d . . . C9 C 0.1730(8) -0.3798(5) 0.1742(3) 0.0467(14) Uani 1 1 d . . . C10 C 0.1145(7) 0.0344(5) 0.5874(2) 0.0301(11) Uani 1 1 d . . . C11 C 0.3567(8) -0.0244(5) 0.5780(2) 0.0424(14) Uani 1 1 d . . . C12 C 0.2945(7) 0.0814(4) 0.7089(2) 0.0291(11) Uani 1 1 d . . . N1 N 0.6730(5) 0.5894(4) 0.90246(16) 0.0680(16) Uani 1 1 d D . . C13 C 0.8442(10) 0.4686(7) 0.8537(3) 0.102(3) Uani 1 1 d D . . C14 C 0.6237(7) 0.7390(5) 0.8451(2) 0.135(3) Uani 1 1 d D . . C15 C 0.8249(9) 0.8167(7) 0.8435(5) 0.160(4) Uani 1 1 d D . . C16 C 0.5297(10) 0.7262(6) 0.9561(2) 0.258(10) Uani 1 1 d D . . C17 C 0.7002(9) 0.6537(9) 1.0060(3) 0.132(3) Uani 1 1 d D . . C18 C 0.4722(5) 0.5142(4) 0.9038(3) 0.074(2) Uani 1 1 d D . . C19 C 0.4893(9) 0.3231(5) 0.9379(3) 0.072(2) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01693(11) 0.02479(9) 0.03432(13) -0.00054(10) -0.00468(10) -0.00893(8) Pd2 0.01834(12) 0.03109(11) 0.04279(16) 0.00059(12) -0.00539(12) -0.01201(9) S1 0.0198(4) 0.0354(4) 0.0346(5) -0.0014(4) -0.0123(4) -0.0031(3) S2 0.0200(4) 0.0375(4) 0.0302(5) -0.0013(4) -0.0041(4) -0.0097(3) S3 0.0309(5) 0.0492(4) 0.0435(6) 0.0088(5) -0.0151(4) -0.0209(4) S4 0.0432(6) 0.0426(4) 0.0254(5) -0.0056(4) -0.0040(4) -0.0137(4) S5 0.0960(10) 0.0691(7) 0.0519(7) -0.0143(6) -0.0250(6) -0.0246(6) S6 0.0198(5) 0.0416(4) 0.0472(6) -0.0005(5) -0.0076(4) -0.0084(4) S7 0.0138(4) 0.0375(4) 0.0391(5) -0.0059(4) -0.0035(4) -0.0105(3) S8 0.0367(6) 0.0472(5) 0.0536(7) -0.0129(5) 0.0093(5) -0.0139(4) S9 0.0426(6) 0.0720(6) 0.0512(6) -0.0184(5) -0.0053(5) -0.0289(4) S10 0.0968(13) 0.1255(11) 0.0623(9) -0.0306(9) 0.0105(9) -0.0394(10) S11 0.0211(4) 0.0320(4) 0.0355(5) -0.0013(4) -0.0047(4) -0.0112(3) S12 0.0172(5) 0.0330(4) 0.0574(6) -0.0020(5) -0.0025(4) -0.0069(3) S13 0.0301(5) 0.0325(4) 0.0364(5) -0.0042(4) -0.0051(4) -0.0155(3) S14 0.0413(6) 0.0290(4) 0.0414(6) -0.0028(4) 0.0002(5) -0.0013(4) S15 0.0781(8) 0.0375(4) 0.0306(5) -0.0111(4) -0.0022(5) -0.0211(4) S16 0.0268(5) 0.0433(4) 0.0370(5) -0.0027(4) -0.0065(4) -0.0151(4) S17 0.0230(5) 0.0482(5) 0.0602(7) -0.0017(5) -0.0103(5) -0.0149(4) S18 0.0382(6) 0.0652(6) 0.0574(7) -0.0019(6) -0.0045(5) -0.0199(5) S19 0.0467(7) 0.0807(7) 0.0543(7) 0.0013(6) -0.0154(6) -0.0272(5) S20 0.0885(10) 0.0853(8) 0.0439(7) 0.0010(7) -0.0270(6) -0.0260(7) C1 0.0235(17) 0.0226(13) 0.0224(16) 0.0112(13) -0.0129(13) -0.0105(12) C2 0.052(3) 0.046(2) 0.041(2) -0.006(2) -0.008(2) -0.0144(19) C3 0.110(4) 0.135(4) 0.116(4) -0.058(3) -0.044(3) -0.051(3) C4 0.0211(18) 0.0167(13) 0.043(2) -0.0018(15) 0.0033(16) -0.0027(12) C5 0.0233(19) 0.0345(16) 0.036(2) -0.0022(17) -0.0020(16) -0.0116(14) C6 0.037(2) 0.0246(15) 0.052(2) 0.0104(18) -0.0059(19) -0.0076(15) C7 0.0217(16) 0.0236(13) 0.0216(16) 0.0059(13) -0.0131(13) -0.0144(11) C8 0.046(2) 0.0344(14) 0.0210(18) -0.0093(14) -0.0005(15) -0.0245(13) C9 0.044(2) 0.0564(18) 0.051(3) -0.0191(19) 0.006(2) -0.0308(15) C10 0.0264(19) 0.0318(15) 0.036(2) -0.0036(16) -0.0021(16) -0.0148(13) C11 0.041(2) 0.0457(18) 0.047(3) -0.002(2) -0.003(2) -0.0218(16) C12 0.041(2) 0.0226(13) 0.0273(18) 0.0230(14) -0.0145(15) -0.0174(12) N1 0.050(3) 0.089(2) 0.054(2) -0.020(2) 0.009(2) -0.003(2) C13 0.092(6) 0.097(4) 0.099(5) -0.018(4) 0.006(4) 0.002(4) C14 0.041(4) 0.134(4) 0.189(6) 0.103(4) 0.005(4) 0.002(4) C15 0.186(7) 0.084(4) 0.169(6) 0.044(4) 0.095(5) -0.028(4) C16 0.188(15) 0.154(9) 0.38(2) -0.036(11) 0.038(14) 0.009(10) C17 0.114(4) 0.176(5) 0.134(4) 0.114(3) -0.092(3) -0.093(4) C18 0.030(3) 0.091(3) 0.093(4) -0.005(3) 0.019(3) -0.013(3) C19 0.053(3) 0.0511(19) 0.120(5) 0.017(3) 0.005(3) -0.0380(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S6 2.2807(12) . ? Pd1 S7 2.2803(13) . ? Pd1 S1 2.3045(13) . ? Pd1 S2 2.3169(12) . ? Pd1 Pd2 3.1438(10) . ? Pd2 S17 2.2709(15) . ? Pd2 S16 2.2904(12) . ? Pd2 S11 2.3025(13) . ? Pd2 S12 2.3081(13) . ? S1 C1 1.602(3) . ? S2 C2 1.805(6) . ? S3 C1 1.818(4) . ? S3 C3 1.894(7) . ? S4 C3 1.524(8) . ? S4 C2 1.845(5) . ? S5 C3 1.718(8) . ? S6 C4 1.723(4) . ? S7 C5 1.626(4) . ? S8 C4 1.676(4) . ? S8 C6 1.924(5) . ? S9 C5 1.705(5) . ? S9 C6 1.737(4) . ? S10 C6 1.534(5) . ? S11 C7 1.717(3) . ? S12 C8 1.683(5) . ? S13 C9 1.738(4) . ? S13 C7 1.814(4) . ? S14 C9 1.546(5) . ? S14 C8 1.824(4) . ? S15 C9 1.719(5) . ? S16 C10 1.639(5) . ? S17 C11 1.803(5) . ? S18 C10 1.644(4) . ? S18 C12 1.814(5) . ? S19 C11 1.749(5) . ? S19 C12 1.814(4) . ? S20 C12 1.550(4) . ? C1 C2 1.242(6) . ? C4 C5 1.452(5) . ? C7 C8 1.259(5) . ? C10 C11 1.438(6) . ? N1 C13 1.486(5) . ? N1 C14 1.501(5) . ? N1 C18 1.525(5) . ? N1 C16 1.542(5) . ? C14 C15 1.539(8) . ? C16 C17 1.444(7) . ? C18 C19 1.553(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S6 Pd1 S7 89.72(5) . . ? S6 Pd1 S1 88.57(5) . . ? S7 Pd1 S1 175.99(3) . . ? S6 Pd1 S2 175.01(3) . . ? S7 Pd1 S2 91.97(5) . . ? S1 Pd1 S2 89.45(5) . . ? S6 Pd1 Pd2 97.27(4) . . ? S7 Pd1 Pd2 87.48(3) . . ? S1 Pd1 Pd2 96.33(3) . . ? S2 Pd1 Pd2 87.50(3) . . ? S17 Pd2 S16 91.42(5) . . ? S17 Pd2 S11 177.25(3) . . ? S16 Pd2 S11 90.45(5) . . ? S17 Pd2 S12 87.77(5) . . ? S16 Pd2 S12 175.69(4) . . ? S11 Pd2 S12 90.21(5) . . ? S17 Pd2 Pd1 96.08(3) . . ? S16 Pd2 Pd1 87.91(4) . . ? S11 Pd2 Pd1 86.01(3) . . ? S12 Pd2 Pd1 96.39(4) . . ? C1 S1 Pd1 101.58(15) . . ? C2 S2 Pd1 96.46(15) . . ? C1 S3 C3 96.8(3) . . ? C3 S4 C2 97.8(3) . . ? C4 S6 Pd1 102.00(13) . . ? C5 S7 Pd1 104.49(16) . . ? C4 S8 C6 96.78(19) . . ? C5 S9 C6 104.7(2) . . ? C7 S11 Pd2 98.38(13) . . ? C8 S12 Pd2 98.96(13) . . ? C9 S13 C7 93.0(2) . . ? C9 S14 C8 96.9(2) . . ? C10 S16 Pd2 104.20(14) . . ? C11 S17 Pd2 100.17(17) . . ? C10 S18 C12 104.1(2) . . ? C11 S19 C12 93.4(2) . . ? C2 C1 S1 126.9(4) . . ? C2 C1 S3 107.9(3) . . ? S1 C1 S3 124.1(2) . . ? C1 C2 S2 124.7(4) . . ? C1 C2 S4 123.4(4) . . ? S2 C2 S4 111.6(3) . . ? S4 C3 S5 130.0(4) . . ? S4 C3 S3 111.2(4) . . ? S5 C3 S3 111.5(4) . . ? C5 C4 S8 120.6(3) . . ? C5 C4 S6 121.4(3) . . ? S8 C4 S6 118.0(2) . . ? C4 C5 S7 122.2(3) . . ? C4 C5 S9 111.5(3) . . ? S7 C5 S9 126.2(2) . . ? S10 C6 S9 124.3(3) . . ? S10 C6 S8 129.3(3) . . ? S9 C6 S8 106.4(2) . . ? C8 C7 S11 125.8(3) . . ? C8 C7 S13 115.9(3) . . ? S11 C7 S13 118.03(19) . . ? C7 C8 S12 126.5(3) . . ? C7 C8 S14 115.0(3) . . ? S12 C8 S14 118.3(2) . . ? S14 C9 S15 121.3(3) . . ? S14 C9 S13 118.8(3) . . ? S15 C9 S13 119.9(3) . . ? C11 C10 S16 122.3(3) . . ? C11 C10 S18 109.3(3) . . ? S16 C10 S18 128.4(2) . . ? C10 C11 S19 122.9(3) . . ? C10 C11 S17 121.5(4) . . ? S19 C11 S17 114.1(2) . . ? S20 C12 S19 121.4(2) . . ? S20 C12 S18 127.5(2) . . ? S19 C12 S18 108.3(2) . . ? C13 N1 C14 93.1(3) . . ? C13 N1 C18 101.8(4) . . ? C14 N1 C18 102.8(3) . . ? C13 N1 C16 170.0(4) . . ? C14 N1 C16 86.6(3) . . ? C18 N1 C16 88.0(3) . . ? N1 C14 C15 103.2(4) . . ? C17 C16 N1 87.8(4) . . ? N1 C18 C19 119.6(3) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 1.401 _refine_diff_density_min -1.134 _refine_diff_density_rms 0.306 #===END data_e42pd #(CIF file of (NEt4)2[Pd(dmit)2]) _database_code_CSD 168859 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(NEt4)2[Pd(dmit)2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H40 N2 Pd S10' _chemical_formula_weight 759.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 11.805(2) _cell_length_b 13.477(3) _cell_length_c 21.458(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3414.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6175 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22434 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4216 _reflns_number_gt 2128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1089P)^2^+0.8320P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4216 _refine_ls_number_parameters 161 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1247 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1994 _refine_ls_wR_factor_gt 0.1614 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.0000 0.0000 0.0000 0.0606(2) Uani 1 2 d S . . S1 S 0.13854(14) -0.11957(12) 0.01374(7) 0.0720(4) Uani 1 1 d . . . S2 S 0.07236(15) 0.09146(13) 0.08265(8) 0.0788(5) Uani 1 1 d . . . S3 S 0.34260(14) -0.12090(12) 0.09838(7) 0.0704(4) Uani 1 1 d . . . S4 S 0.28553(15) 0.06135(13) 0.15866(8) 0.0789(5) Uani 1 1 d . . . S5 S 0.49500(15) -0.04492(17) 0.19891(9) 0.0867(5) Uani 1 1 d . . . C1 C 0.2186(5) -0.0644(4) 0.0734(2) 0.0621(14) Uani 1 1 d . . . C2 C 0.1905(5) 0.0218(5) 0.1010(3) 0.0664(15) Uani 1 1 d . . . C3 C 0.3812(5) -0.0346(5) 0.1542(3) 0.0713(16) Uani 1 1 d . . . N1 N 0.2500 0.2500 -0.0850(3) 0.0698(18) Uani 1 2 d SD . . C4 C 0.2694(13) 0.1849(11) -0.0304(6) 0.123(7) Uiso 0.539(16) 1 d PD . 2 H4A H 0.2698 0.2272 0.0062 0.148 Uiso 0.539(16) 1 calc PR . 2 H4B H 0.2037 0.1420 -0.0267 0.148 Uiso 0.539(16) 1 calc PR . 2 C5 C 0.3699(8) 0.1212(8) -0.0266(5) 0.145(4) Uani 1 1 d D . . H5A H 0.3199 0.1332 0.0079 0.217 Uiso 0.461(16) 1 calc PR . 1 H5B H 0.4462 0.1147 -0.0115 0.217 Uiso 0.461(16) 1 calc PR . 1 H5C H 0.3479 0.0612 -0.0474 0.217 Uiso 0.461(16) 1 calc PR . 1 H5D H 0.3690 0.0854 0.0121 0.217 Uiso 0.539(16) 1 calc PR . 2 H5E H 0.4369 0.1615 -0.0286 0.217 Uiso 0.539(16) 1 calc PR . 2 H5F H 0.3697 0.0752 -0.0607 0.217 Uiso 0.539(16) 1 calc PR . 2 C4' C 0.3634(9) 0.2073(10) -0.0718(7) 0.100(6) Uiso 0.461(16) 1 d PD . 1 H4C H 0.4111 0.2601 -0.0559 0.120 Uiso 0.461(16) 1 calc PR . 1 H4D H 0.3959 0.1857 -0.1111 0.120 Uiso 0.461(16) 1 calc PR . 1 C6 C 0.1544(9) 0.1867(9) -0.0995(6) 0.106(6) Uiso 0.572(15) 1 d PD . 1 H6A H 0.0935 0.2298 -0.1132 0.127 Uiso 0.572(15) 1 calc PR . 1 H6B H 0.1299 0.1572 -0.0605 0.127 Uiso 0.572(15) 1 calc PR . 1 C6' C 0.2350(15) 0.1922(10) -0.1430(5) 0.099(7) Uiso 0.428(15) 1 d PD . 2 H6C H 0.3100 0.1721 -0.1564 0.118 Uiso 0.428(15) 1 calc PR . 2 H6D H 0.2070 0.2382 -0.1742 0.118 Uiso 0.428(15) 1 calc PR . 2 C7 C 0.1625(8) 0.1031(7) -0.1466(4) 0.132(3) Uani 1 1 d D . . H7A H 0.0887 0.0752 -0.1533 0.198 Uiso 0.572(15) 1 calc PR . 1 H7B H 0.2126 0.0526 -0.1311 0.198 Uiso 0.572(15) 1 calc PR . 1 H7C H 0.1915 0.1285 -0.1852 0.198 Uiso 0.572(15) 1 calc PR . 1 H7D H 0.0849 0.1216 -0.1401 0.198 Uiso 0.428(15) 1 calc PR . 2 H7E H 0.1852 0.0566 -0.1151 0.198 Uiso 0.428(15) 1 calc PR . 2 H7F H 0.1704 0.0731 -0.1869 0.198 Uiso 0.428(15) 1 calc PR . 2 N2 N 0.2500 -0.2500 -0.1859(2) 0.0524(14) Uani 1 2 d SD . . C8 C 0.1493(7) -0.2249(5) -0.1471(4) 0.111(3) Uani 1 1 d D . . H8A H 0.0875 -0.2060 -0.1745 0.133 Uiso 1 1 calc R . . H8B H 0.1674 -0.1679 -0.1214 0.133 Uiso 1 1 calc R . . C9 C 0.1091(6) -0.3104(5) -0.1047(3) 0.088(2) Uani 1 1 d D . . H9A H 0.0438 -0.2895 -0.0815 0.131 Uiso 1 1 calc R . . H9B H 0.1687 -0.3281 -0.0763 0.131 Uiso 1 1 calc R . . H9C H 0.0898 -0.3669 -0.1298 0.131 Uiso 1 1 calc R . . C10 C 0.2757(6) -0.1608(5) -0.2271(3) 0.097(2) Uani 1 1 d D . . H10A H 0.2901 -0.1038 -0.2007 0.117 Uiso 1 1 calc R . . H10B H 0.2091 -0.1461 -0.2520 0.117 Uiso 1 1 calc R . . C11 C 0.3771(6) -0.1751(6) -0.2710(3) 0.100(2) Uani 1 1 d D . . H11A H 0.3879 -0.1160 -0.2953 0.150 Uiso 1 1 calc R . . H11B H 0.3628 -0.2301 -0.2982 0.150 Uiso 1 1 calc R . . H11C H 0.4440 -0.1879 -0.2468 0.150 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0614(4) 0.0636(4) 0.0569(4) -0.0046(3) 0.0072(3) 0.0013(3) S1 0.0731(10) 0.0694(9) 0.0735(9) -0.0168(8) -0.0057(7) 0.0081(8) S2 0.0824(12) 0.0765(10) 0.0775(10) -0.0197(8) -0.0030(8) 0.0138(9) S3 0.0688(10) 0.0682(9) 0.0744(10) -0.0029(7) -0.0028(7) -0.0002(8) S4 0.0882(12) 0.0724(10) 0.0761(10) -0.0148(8) -0.0083(8) -0.0034(9) S5 0.0772(12) 0.0932(13) 0.0896(12) 0.0015(10) -0.0131(9) -0.0168(10) C1 0.068(4) 0.062(3) 0.056(3) 0.000(3) -0.001(3) -0.005(3) C2 0.071(4) 0.070(4) 0.059(3) -0.005(3) 0.001(3) 0.000(3) C3 0.070(4) 0.067(4) 0.077(4) 0.007(3) 0.011(3) -0.012(3) N1 0.051(4) 0.097(5) 0.061(4) 0.000 0.000 0.002(4) C5 0.101(7) 0.180(11) 0.153(8) 0.081(8) 0.002(6) 0.015(7) C7 0.148(9) 0.133(8) 0.114(7) -0.021(6) 0.004(6) 0.021(6) N2 0.060(4) 0.041(3) 0.057(3) 0.000 0.000 0.008(3) C8 0.122(7) 0.091(6) 0.120(7) -0.010(5) 0.012(5) 0.005(5) C9 0.093(5) 0.094(5) 0.076(4) -0.015(4) 0.030(3) -0.015(4) C10 0.115(6) 0.080(5) 0.096(5) 0.008(4) -0.008(5) -0.006(4) C11 0.112(6) 0.108(6) 0.079(4) -0.001(4) 0.015(4) -0.038(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S1 2.3149(16) 5 ? Pd1 S1 2.3149(16) . ? Pd1 S2 2.3226(16) 5 ? Pd1 S2 2.3226(16) . ? S1 C1 1.757(6) . ? S2 C2 1.726(6) . ? S3 C3 1.731(7) . ? S3 C1 1.735(6) . ? S4 C3 1.720(7) . ? S4 C2 1.754(6) . ? S5 C3 1.656(7) . ? C1 C2 1.345(8) . ? N1 C6 1.449(8) . ? N1 C6 1.449(8) 2 ? N1 C6' 1.479(8) . ? N1 C6' 1.479(8) 2 ? N1 C4 1.482(9) 2 ? N1 C4 1.482(9) . ? N1 C4' 1.484(9) . ? N1 C4' 1.484(9) 2 ? C4 C5 1.467(9) . ? C4 C4 1.81(3) 2 ? C5 C4' 1.514(9) . ? C6 C7 1.517(9) . ? C6' C7 1.477(8) . ? N2 C8 1.490(6) 2_545 ? N2 C8 1.490(6) . ? N2 C10 1.523(6) 2_545 ? N2 C10 1.523(6) . ? C8 C9 1.545(7) . ? C10 C11 1.535(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Pd1 S1 180.00(12) 5 . ? S1 Pd1 S2 90.71(6) 5 5 ? S1 Pd1 S2 89.29(6) . 5 ? S1 Pd1 S2 89.29(6) 5 . ? S1 Pd1 S2 90.71(6) . . ? S2 Pd1 S2 180.00(8) 5 . ? C1 S1 Pd1 100.3(2) . . ? C2 S2 Pd1 100.5(2) . . ? C3 S3 C1 98.1(3) . . ? C3 S4 C2 98.8(3) . . ? C2 C1 S3 116.8(4) . . ? C2 C1 S1 123.6(5) . . ? S3 C1 S1 119.5(3) . . ? C1 C2 S2 124.7(5) . . ? C1 C2 S4 114.5(5) . . ? S2 C2 S4 120.8(4) . . ? S5 C3 S4 124.3(4) . . ? S5 C3 S3 123.9(4) . . ? S4 C3 S3 111.8(4) . . ? C6 N1 C6 155.3(12) . 2 ? C6 N1 C6' 54.3(8) . . ? C6 N1 C6' 102.9(9) 2 . ? C6 N1 C6' 102.9(9) . 2 ? C6 N1 C6' 54.3(8) 2 2 ? C6' N1 C6' 65.3(11) . 2 ? C6 N1 C4 113.4(8) . 2 ? C6 N1 C4 86.6(10) 2 2 ? C6' N1 C4 163.5(9) . 2 ? C6' N1 C4 111.9(9) 2 2 ? C6 N1 C4 86.6(10) . . ? C6 N1 C4 113.4(9) 2 . ? C6' N1 C4 111.9(9) . . ? C6' N1 C4 163.5(9) 2 . ? C4 N1 C4 75.4(13) 2 . ? C6 N1 C4' 121.0(8) . . ? C6 N1 C4' 64.3(7) 2 . ? C6' N1 C4' 93.7(10) . . ? C6' N1 C4' 104.9(9) 2 . ? C4 N1 C4' 102.6(9) 2 . ? C4 N1 C4' 58.7(8) . . ? C6 N1 C4' 64.3(7) . 2 ? C6 N1 C4' 121.0(8) 2 2 ? C6' N1 C4' 104.9(9) . 2 ? C6' N1 C4' 93.7(10) 2 2 ? C4 N1 C4' 58.7(8) 2 2 ? C4 N1 C4' 102.6(9) . 2 ? C4' N1 C4' 158.0(13) . 2 ? C5 C4 N1 121.0(9) . . ? C5 C4 C4 140.4(18) . 2 ? N1 C4 C4 52.3(6) . 2 ? C4 C5 C4' 58.3(8) . . ? N1 C4' C5 117.8(9) . . ? N1 C6 C7 122.1(9) . . ? N1 C6' C7 122.8(9) . . ? C6' C7 C6 53.0(8) . . ? C8 N2 C8 112.2(8) 2_545 . ? C8 N2 C10 107.7(4) 2_545 2_545 ? C8 N2 C10 110.2(5) . 2_545 ? C8 N2 C10 110.2(5) 2_545 . ? C8 N2 C10 107.7(4) . . ? C10 N2 C10 109.0(7) 2_545 . ? N2 C8 C9 113.9(5) . . ? N2 C10 C11 114.4(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.336 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.100 #===END data_e4pd2 #(CIF file of (NEt4)[Pd(dmit)2]2) _database_code_CSD 168860 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(NEt4)[Pd(dmit)2]2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 N Pd2 S20' _chemical_formula_weight 1128.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.297(1) _cell_length_b 7.875(1) _cell_length_c 18.885(3) _cell_angle_alpha 83.947(4) _cell_angle_beta 83.301(4) _cell_angle_gamma 72.741(4) _cell_volume 885.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 559 _exptl_absorpt_coefficient_mu 2.215 _exptl_absorpt_correction_type 'abscor' _exptl_absorpt_correction_T_min 0.3959 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4364 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0873 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.38 _reflns_number_total 4364 _reflns_number_gt 2865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+0.8260P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4364 _refine_ls_number_parameters 214 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1239 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.2144 _refine_ls_wR_factor_gt 0.1844 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 Pd1 Pd 0.51275(4) -0.18986(3) 0.536828(13) 0.02833(6) Uani 1 1 d . . . S1 S 0.22781(13) -0.19009(13) 0.47054(5) 0.0343(2) Uani 1 1 d . . . S2 S 0.76930(14) -0.34651(13) 0.45321(5) 0.0372(2) Uani 1 1 d . . . S3 S 0.23918(16) -0.33916(13) 0.32990(5) 0.0422(3) Uani 1 1 d . . . S4 S 0.71981(17) -0.48370(13) 0.31796(5) 0.0420(3) Uani 1 1 d . . . S5 S 0.4681(2) -0.53336(16) 0.20274(6) 0.0628(4) Uani 1 1 d . . . S6 S 0.26101(13) -0.05416(12) 0.62714(4) 0.0318(2) Uani 1 1 d . . . S7 S 0.80409(14) -0.20920(12) 0.60298(5) 0.0349(2) Uani 1 1 d . . . S8 S 0.33281(16) 0.03162(13) 0.77108(5) 0.0419(3) Uani 1 1 d . . . S9 S 0.81102(15) -0.11083(13) 0.75140(5) 0.0402(3) Uani 1 1 d . . . S10 S 0.6053(2) 0.03941(19) 0.88897(6) 0.0663(4) Uani 1 1 d . . . N1 N 0.0000 0.5000 1.0000 0.0478(15) Uani 1 2 d SD . . C1 C 0.3736(5) -0.3017(4) 0.39926(16) 0.0307(8) Uani 1 1 d . . . C2 C 0.6021(6) -0.3686(4) 0.39396(17) 0.0307(9) Uani 1 1 d . . . C3 C 0.4771(6) -0.4546(4) 0.27909(18) 0.0369(10) Uani 1 1 d . . . C4 C 0.4386(6) -0.0556(4) 0.68910(17) 0.0332(9) Uani 1 1 d . . . C5 C 0.6674(5) -0.1242(4) 0.67957(18) 0.0312(9) Uani 1 1 d . . . C6 C 0.5870(7) -0.0109(5) 0.8077(2) 0.0427(11) Uani 1 1 d . . . C7 C 0.1549(9) 0.3812(10) 0.9513(2) 0.055(3) Uani 0.50 1 d PD A 1 H7A H 0.1952 0.2613 0.9741 0.066 Uiso 0.50 1 calc PR A 1 H7B H 0.2900 0.4181 0.9411 0.066 Uiso 0.50 1 calc PR A 1 C8 C 0.0557(8) 0.3800(6) 0.88014(18) 0.088(2) Uani 0.50 1 d PD A 1 H8A H 0.1623 0.2977 0.8501 0.132 Uiso 0.50 1 calc PR A 1 H8B H 0.0217 0.4974 0.8563 0.132 Uiso 0.50 1 calc PR A 1 H8C H -0.0783 0.3439 0.8899 0.132 Uiso 0.50 1 calc PR A 1 C7' C -0.1007(11) 0.5180(8) 0.9271(3) 0.054(3) Uani 0.50 1 d PD . 2 H7'A H -0.2469 0.4984 0.9346 0.065 Uiso 0.50 1 calc PR . 2 H7'B H -0.1168 0.6367 0.9042 0.065 Uiso 0.50 1 calc PR . 2 C8' C 0.0557(8) 0.3800(6) 0.88014(18) 0.088(2) Uani 0.50 1 d P B 2 H8'A H -0.0051 0.3874 0.8352 0.132 Uiso 0.50 1 calc PR B 2 H8'B H 0.0725 0.2630 0.9035 0.132 Uiso 0.50 1 calc PR B 2 H8'C H 0.1988 0.4021 0.8720 0.132 Uiso 0.50 1 calc PR B 2 C9 C -0.0450(6) 0.6952(6) 0.9732(4) 0.050(3) Uani 0.50 1 d PD A 1 H9A H -0.1408 0.7693 1.0090 0.060 Uiso 0.50 1 calc PR A 1 H9B H -0.1218 0.7171 0.9301 0.060 Uiso 0.50 1 calc PR A 1 C10 C 0.1744(6) 0.7450(4) 0.9575(4) 0.099(2) Uani 0.50 1 d PD A 1 H10A H 0.1428 0.8690 0.9413 0.148 Uiso 0.50 1 calc PR A 1 H10B H 0.2673 0.6741 0.9211 0.148 Uiso 0.50 1 calc PR A 1 H10C H 0.2502 0.7233 1.0002 0.148 Uiso 0.50 1 calc PR A 1 C9' C 0.2158(9) 0.5450(5) 0.9797(4) 0.044(2) Uani 0.50 1 d PD . 2 H9'A H 0.2978 0.4762 0.9404 0.053 Uiso 0.50 1 calc PR . 2 H9'B H 0.3061 0.5128 1.0200 0.053 Uiso 0.50 1 calc PR . 2 C10' C 0.1744(6) 0.7450(4) 0.9575(4) 0.099(2) Uani 0.50 1 d P C 2 H10D H 0.3148 0.7698 0.9445 0.148 Uiso 0.50 1 calc PR C 2 H10E H 0.0964 0.8132 0.9968 0.148 Uiso 0.50 1 calc PR C 2 H10F H 0.0861 0.7769 0.9174 0.148 Uiso 0.50 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02795(10) 0.03443(11) 0.02433(10) -0.00576(9) -0.00301(9) -0.01011(9) S1 0.0279(3) 0.0471(4) 0.0296(4) -0.0085(4) 0.0003(3) -0.0121(3) S2 0.0297(4) 0.0484(5) 0.0326(4) -0.0115(4) -0.0042(3) -0.0066(3) S3 0.0446(4) 0.0509(5) 0.0376(4) -0.0110(4) -0.0086(4) -0.0193(4) S4 0.0470(5) 0.0416(5) 0.0351(4) -0.0098(4) -0.0008(4) -0.0081(4) S5 0.1004(7) 0.0634(6) 0.0364(5) -0.0173(4) -0.0044(5) -0.0374(5) S6 0.0284(3) 0.0401(4) 0.0288(4) -0.0067(3) -0.0026(3) -0.0112(3) S7 0.0303(4) 0.0436(4) 0.0309(4) -0.0067(4) -0.0040(3) -0.0088(3) S8 0.0451(5) 0.0478(5) 0.0315(4) -0.0140(4) -0.0041(4) -0.0071(4) S9 0.0429(4) 0.0491(5) 0.0324(4) -0.0047(4) -0.0113(3) -0.0157(4) S10 0.0785(7) 0.0816(8) 0.0394(5) -0.0206(5) -0.0215(5) -0.0124(6) N1 0.036(2) 0.045(3) 0.056(3) 0.005(2) -0.009(2) -0.001(2) C1 0.0358(14) 0.0434(16) 0.0204(13) -0.0080(13) -0.0050(12) -0.0200(12) C2 0.0423(16) 0.0263(14) 0.0221(14) -0.0019(13) -0.0019(13) -0.0079(13) C3 0.0559(18) 0.0303(15) 0.0294(16) 0.0014(14) -0.0073(15) -0.0197(13) C4 0.0473(16) 0.0326(15) 0.0250(14) 0.0016(13) -0.0090(13) -0.0186(12) C5 0.0314(14) 0.0331(16) 0.0290(15) 0.0032(14) -0.0048(13) -0.0105(12) C6 0.060(2) 0.0354(17) 0.0354(17) -0.0004(16) -0.0109(16) -0.0161(15) C7 0.037(3) 0.083(5) 0.052(5) -0.005(4) 0.004(4) -0.028(3) C8 0.090(4) 0.099(4) 0.071(3) -0.034(3) 0.022(3) -0.022(3) C7' 0.049(4) 0.077(6) 0.033(4) -0.016(4) -0.010(3) -0.009(4) C8' 0.090(4) 0.099(4) 0.071(3) -0.034(3) 0.022(3) -0.022(3) C9 0.059(5) 0.038(4) 0.045(4) 0.005(4) -0.005(4) -0.004(4) C10 0.108(4) 0.101(4) 0.105(5) -0.008(4) -0.007(4) -0.060(3) C9' 0.022(3) 0.057(4) 0.050(4) -0.006(4) 0.001(3) -0.008(3) C10' 0.108(4) 0.101(4) 0.105(5) -0.008(4) -0.007(4) -0.060(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S2 2.2931(9) . ? Pd1 S7 2.2975(10) . ? Pd1 S6 2.3048(9) . ? Pd1 S1 2.3051(10) . ? Pd1 Pd1 3.1295(7) 2_656 ? S1 C1 1.706(3) . ? S2 C2 1.678(4) . ? S3 C1 1.734(4) . ? S3 C3 1.741(3) . ? S4 C3 1.716(4) . ? S4 C2 1.749(3) . ? S5 C3 1.642(4) . ? S6 C4 1.708(4) . ? S7 C5 1.689(3) . ? S8 C4 1.739(3) . ? S8 C6 1.744(4) . ? S9 C6 1.705(4) . ? S9 C5 1.744(4) . ? S10 C6 1.651(4) . ? N1 C7 1.451(5) 2_567 ? N1 C7 1.451(5) . ? N1 C9' 1.501(6) 2_567 ? N1 C9' 1.501(6) . ? N1 C9 1.520(5) . ? N1 C9 1.520(5) 2_567 ? N1 C7' 1.558(5) . ? N1 C7' 1.558(5) 2_567 ? C1 C2 1.373(5) . ? C4 C5 1.378(5) . ? C7 C8 1.548(6) . ? C7' C9' 1.897(9) 2_567 ? C9 C10 1.533(5) . ? C9' C7' 1.897(9) 2_567 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Pd1 S7 87.88(3) . . ? S2 Pd1 S6 175.17(3) . . ? S7 Pd1 S6 90.43(3) . . ? S2 Pd1 S1 90.06(4) . . ? S7 Pd1 S1 176.33(4) . . ? S6 Pd1 S1 91.38(3) . . ? S2 Pd1 Pd1 96.48(3) . 2_656 ? S7 Pd1 Pd1 96.05(3) . 2_656 ? S6 Pd1 Pd1 88.19(3) . 2_656 ? S1 Pd1 Pd1 87.20(3) . 2_656 ? C1 S1 Pd1 101.30(12) . . ? C2 S2 Pd1 101.09(11) . . ? C1 S3 C3 97.14(17) . . ? C3 S4 C2 97.71(17) . . ? C4 S6 Pd1 100.35(11) . . ? C5 S7 Pd1 101.57(12) . . ? C4 S8 C6 97.50(18) . . ? C6 S9 C5 98.28(18) . . ? C7 N1 C7 180.0(3) 2_567 . ? C7 N1 C9' 66.0(4) 2_567 2_567 ? C7 N1 C9' 114.0(4) . 2_567 ? C7 N1 C9' 114.0(4) 2_567 . ? C7 N1 C9' 66.0(4) . . ? C9' N1 C9' 180.0(6) 2_567 . ? C7 N1 C9 67.3(4) 2_567 . ? C7 N1 C9 112.7(4) . . ? C9' N1 C9 110.4(2) 2_567 . ? C9' N1 C9 69.6(2) . . ? C7 N1 C9 112.7(4) 2_567 2_567 ? C7 N1 C9 67.3(4) . 2_567 ? C9' N1 C9 69.6(2) 2_567 2_567 ? C9' N1 C9 110.4(2) . 2_567 ? C9 N1 C9 180.000(2) . 2_567 ? C7 N1 C7' 109.8(3) 2_567 . ? C7 N1 C7' 70.2(3) . . ? C9' N1 C7' 76.6(4) 2_567 . ? C9' N1 C7' 103.4(4) . . ? C9 N1 C7' 74.2(4) . . ? C9 N1 C7' 105.8(4) 2_567 . ? C7 N1 C7' 70.2(3) 2_567 2_567 ? C7 N1 C7' 109.8(3) . 2_567 ? C9' N1 C7' 103.4(4) 2_567 2_567 ? C9' N1 C7' 76.6(4) . 2_567 ? C9 N1 C7' 105.8(4) . 2_567 ? C9 N1 C7' 74.2(4) 2_567 2_567 ? C7' N1 C7' 180.000(3) . 2_567 ? C2 C1 S1 122.2(3) . . ? C2 C1 S3 116.4(2) . . ? S1 C1 S3 121.40(18) . . ? C1 C2 S2 125.3(3) . . ? C1 C2 S4 115.2(3) . . ? S2 C2 S4 119.4(2) . . ? S5 C3 S4 123.5(2) . . ? S5 C3 S3 123.0(2) . . ? S4 C3 S3 113.5(2) . . ? C5 C4 S6 124.4(3) . . ? C5 C4 S8 115.6(3) . . ? S6 C4 S8 119.96(19) . . ? C4 C5 S7 123.1(3) . . ? C4 C5 S9 115.4(3) . . ? S7 C5 S9 121.41(19) . . ? S10 C6 S9 124.0(3) . . ? S10 C6 S8 122.8(2) . . ? S9 C6 S8 113.2(2) . . ? N1 C7 C8 112.4(4) . . ? N1 C7' C9' 50.3(2) . 2_567 ? N1 C9 C10 110.6(3) . . ? N1 C9' C7' 53.0(3) . 2_567 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.368 _refine_diff_density_min -1.521 _refine_diff_density_rms 0.221