Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Cassoux, P.' 'Doublet, M.-L.' 'Faulmann, Christophe' 'Garreau de Bonneval, B.' 'Granier, F.' 'Legros, J. P.' 'Malfant, I.' 'Togonidze, T.' _publ_contact_author_name 'Dr Christophe Faulmann' _publ_contact_author_address ; Dr Christophe Faulmann Laboratoire de Chimie de Coordination CNRS 205 route de Narbonne Toulouse 321077 Cedex FRANCE ; _publ_contact_author_email 'FAULMANN@LCC-TOULOUSE.FR' data_pd36_ta _database_code_CSD 162839 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H13 S, 2(C6 Pd S10)' _chemical_formula_sum 'C17 H13 Pd2 S21' _chemical_formula_weight 1103.58 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' '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 7.804(4) _cell_length_b 36.171(18) _cell_length_c 6.284(2) _cell_angle_alpha 91.68(4) _cell_angle_beta 112.08(4) _cell_angle_gamma 88.79(5) _cell_volume 1642.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 6.0 _cell_measurement_theta_max 11.5 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1086 _exptl_absorpt_coefficient_mu 2.446 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.5116 _exptl_absorpt_correction_T_max 0.9902 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 4 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _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 'CAD4 Enraf-Nonius' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 3 _diffrn_reflns_number 4698 _diffrn_reflns_av_R_equivalents 0.2488 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 22.5 _reflns_number_total 4305 _reflns_number_gt 3071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'Sir92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Cameron (Watkin, 1996)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0791P)^2^+30.8852P] 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 4305 _refine_ls_number_parameters 394 _refine_ls_number_restraints 71 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1987 _refine_ls_wR_factor_gt 0.1708 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.164 _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 S1 S 0.4510(11) 0.2526(2) 0.7682(12) 0.106(2) Uani 1 1 d DU . . C1A C 0.336(5) 0.2331(11) 0.506(3) 0.078(8) Uani 0.50 1 d PDU A 1 H1A1 H 0.3891 0.2411 0.4002 0.118 Uiso 0.50 1 calc PR A 1 H1A2 H 0.2082 0.2404 0.4532 0.118 Uiso 0.50 1 calc PR A 1 H1A3 H 0.3459 0.2066 0.5168 0.118 Uiso 0.50 1 calc PR A 1 C1B C 0.441(5) 0.2081(7) 0.637(5) 0.068(8) Uani 0.50 1 d PDU A 2 H1B1 H 0.3151 0.2023 0.5449 0.103 Uiso 0.50 1 calc PR A 2 H1B2 H 0.4911 0.1900 0.7535 0.103 Uiso 0.50 1 calc PR A 2 H1B3 H 0.5126 0.2080 0.5411 0.103 Uiso 0.50 1 calc PR A 2 C2 C 0.483(4) 0.2838(9) 0.567(5) 0.130(9) Uani 1 1 d DU A . H2A H 0.3778 0.2818 0.4224 0.156 Uiso 1 1 calc R B 1 H2B H 0.4854 0.3090 0.6256 0.156 Uiso 1 1 calc R B 1 C3A C 0.659(9) 0.276(2) 0.525(17) 0.13(2) Uani 0.50 1 d PDU A 1 H3A1 H 0.7624 0.2854 0.6519 0.190 Uiso 0.50 1 calc PR A 1 H3A2 H 0.6513 0.2877 0.3865 0.190 Uiso 0.50 1 calc PR A 1 H3A3 H 0.6737 0.2497 0.5087 0.190 Uiso 0.50 1 calc PR A 1 C3B C 0.611(12) 0.262(2) 0.48(2) 0.16(2) Uani 0.50 1 d PDU A 2 H3B1 H 0.6244 0.2370 0.5351 0.236 Uiso 0.50 1 calc PR A 2 H3B2 H 0.7300 0.2733 0.5330 0.236 Uiso 0.50 1 calc PR A 2 H3B3 H 0.5604 0.2611 0.3145 0.236 Uiso 0.50 1 calc PR A 2 C4 C 0.211(4) 0.2618(8) 0.727(4) 0.112(8) Uani 1 1 d DU A . H4A H 0.1851 0.2881 0.7321 0.135 Uiso 1 1 calc R C 1 H4B H 0.1265 0.2511 0.5835 0.135 Uiso 1 1 calc R C 1 C5A C 0.202(11) 0.2427(19) 0.930(9) 0.121(18) Uani 0.50 1 d PDU A 1 H5A1 H 0.1138 0.2230 0.8789 0.182 Uiso 0.50 1 calc PR A 1 H5A2 H 0.1637 0.2601 1.0230 0.182 Uiso 0.50 1 calc PR A 1 H5A3 H 0.3213 0.2328 1.0198 0.182 Uiso 0.50 1 calc PR A 1 C5B C 0.135(9) 0.2319(18) 0.825(9) 0.107(17) Uani 0.50 1 d PDU A 2 H5B1 H 0.2352 0.2186 0.9357 0.160 Uiso 0.50 1 calc PR A 2 H5B2 H 0.0635 0.2152 0.7041 0.160 Uiso 0.50 1 calc PR A 2 H5B3 H 0.0575 0.2427 0.8988 0.160 Uiso 0.50 1 calc PR A 2 Pd1 Pd 0.18800(15) 0.48157(3) 1.01782(18) 0.0310(3) Uani 1 1 d . . . S11 S 0.0370(6) 0.43437(10) 0.7701(6) 0.0368(9) Uani 1 1 d . . . S12 S 0.1981(6) 0.44737(10) 1.3228(6) 0.0372(9) Uani 1 1 d . . . S13 S -0.0659(6) 0.35916(11) 0.8588(7) 0.0451(10) Uani 1 1 d . . . S14 S 0.0787(6) 0.37004(11) 1.3484(7) 0.0447(10) Uani 1 1 d . . . S15 S -0.0893(8) 0.29828(13) 1.1517(9) 0.0688(14) Uani 1 1 d . . . S16 S 0.3559(6) 0.52614(10) 1.2691(6) 0.0384(9) Uani 1 1 d . . . S17 S 0.1974(6) 0.51506(10) 0.7178(6) 0.0379(9) Uani 1 1 d . . . S18 S 0.5042(6) 0.59777(11) 1.1968(7) 0.0425(10) Uani 1 1 d . . . S19 S 0.3638(6) 0.58794(11) 0.7048(7) 0.0422(10) Uani 1 1 d . . . S20 S 0.5617(7) 0.65656(12) 0.9137(9) 0.0595(12) Uani 1 1 d . . . C11 C 0.0279(18) 0.4024(4) 0.957(3) 0.033(3) Uani 1 1 d . . . C12 C 0.100(2) 0.4075(4) 1.194(2) 0.033(3) Uani 1 1 d . . . C13 C -0.030(3) 0.3396(4) 1.123(3) 0.050(4) Uani 1 1 d . . . C14 C 0.3823(19) 0.5565(4) 1.092(3) 0.035(4) Uani 1 1 d . . . C15 C 0.316(2) 0.5530(4) 0.858(2) 0.035(4) Uani 1 1 d . . . C16 C 0.481(2) 0.6171(4) 0.940(3) 0.038(4) Uani 1 1 d . . . Pd2 Pd 0.18507(15) 0.01893(3) 1.02142(18) 0.0309(3) Uani 1 1 d . . . S21 S 0.1970(5) -0.01440(10) 0.7116(6) 0.0370(9) Uani 1 1 d . . . S22 S 0.3587(5) -0.02574(10) 1.2604(6) 0.0382(9) Uani 1 1 d . . . S23 S 0.3729(6) -0.08723(11) 0.6780(7) 0.0419(10) Uani 1 1 d . . . S24 S 0.5151(6) -0.09717(11) 1.1667(7) 0.0409(10) Uani 1 1 d . . . S25 S 0.5770(7) -0.15608(12) 0.8651(9) 0.0592(13) Uani 1 1 d . . . S26 S 0.1909(5) 0.05337(10) 1.3351(6) 0.0369(9) Uani 1 1 d . . . S27 S 0.0295(6) 0.06601(10) 0.7861(6) 0.0384(9) Uani 1 1 d . . . S28 S 0.0602(6) 0.13061(11) 1.3803(7) 0.0472(11) Uani 1 1 d . . . S29 S -0.0848(6) 0.14117(11) 0.8923(7) 0.0488(11) Uani 1 1 d . . . S30 S -0.1167(8) 0.20230(13) 1.2012(10) 0.0767(16) Uani 1 1 d . . . C21 C 0.325(2) -0.0517(4) 0.844(2) 0.033(3) Uani 1 1 d . . . C22 C 0.3879(17) -0.0567(4) 1.071(2) 0.031(3) Uani 1 1 d . . . C23 C 0.489(2) -0.1159(4) 0.902(3) 0.042(4) Uani 1 1 d . . . C24 C 0.0813(18) 0.0929(4) 1.212(2) 0.032(3) Uani 1 1 d . . . C25 C 0.0169(19) 0.0981(4) 0.983(2) 0.035(4) Uani 1 1 d . . . C26 C -0.055(2) 0.1602(4) 1.158(3) 0.048(4) 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 S1 0.100(5) 0.132(6) 0.079(4) 0.002(4) 0.027(4) -0.001(4) C1A 0.04(2) 0.18(3) 0.018(11) 0.060(11) 0.012(12) -0.009(16) C1B 0.028(18) 0.161(15) 0.012(15) -0.033(16) 0.004(15) -0.053(16) C2 0.12(2) 0.17(2) 0.097(19) 0.017(15) 0.034(17) -0.027(18) C3A 0.10(3) 0.15(5) 0.12(4) 0.05(4) 0.03(3) -0.01(3) C3B 0.15(5) 0.23(6) 0.11(4) 0.03(4) 0.06(3) -0.01(4) C4 0.098(12) 0.15(2) 0.086(17) 0.000(15) 0.030(14) -0.002(15) C5A 0.11(4) 0.16(4) 0.10(4) 0.02(3) 0.05(3) 0.04(3) C5B 0.07(3) 0.15(4) 0.07(3) 0.03(3) 0.00(3) 0.01(3) Pd1 0.0319(7) 0.0317(6) 0.0294(6) 0.0018(5) 0.0112(5) -0.0026(5) S11 0.040(2) 0.038(2) 0.032(2) 0.0004(15) 0.0121(18) -0.0076(17) S12 0.045(2) 0.035(2) 0.031(2) 0.0006(15) 0.0123(19) -0.0093(17) S13 0.050(3) 0.036(2) 0.046(2) -0.0005(17) 0.014(2) -0.0059(19) S14 0.058(3) 0.037(2) 0.043(2) 0.0067(17) 0.023(2) -0.0047(19) S15 0.086(4) 0.040(2) 0.078(3) 0.009(2) 0.026(3) -0.018(2) S16 0.039(2) 0.041(2) 0.033(2) 0.0028(16) 0.0090(18) -0.0077(17) S17 0.047(3) 0.035(2) 0.032(2) 0.0007(15) 0.0153(19) -0.0098(17) S18 0.041(2) 0.040(2) 0.040(2) -0.0025(17) 0.009(2) -0.0079(18) S19 0.047(3) 0.042(2) 0.039(2) 0.0041(17) 0.018(2) -0.0079(19) S20 0.062(3) 0.040(2) 0.079(3) 0.004(2) 0.028(3) -0.014(2) C11 0.011(7) 0.040(8) 0.048(10) -0.011(7) 0.012(7) -0.008(6) C12 0.035(9) 0.034(8) 0.036(9) 0.015(6) 0.021(7) 0.010(7) C13 0.068(12) 0.036(9) 0.053(10) 0.002(7) 0.032(10) 0.007(8) C14 0.016(8) 0.043(9) 0.049(10) 0.008(7) 0.015(7) 0.002(6) C15 0.037(9) 0.037(8) 0.040(9) 0.006(7) 0.024(8) 0.002(7) C16 0.027(9) 0.037(8) 0.048(9) 0.008(7) 0.010(8) -0.009(7) Pd2 0.0287(7) 0.0329(6) 0.0306(6) 0.0005(5) 0.0108(5) 0.0047(5) S21 0.040(2) 0.038(2) 0.032(2) 0.0029(16) 0.0128(18) 0.0111(17) S22 0.039(2) 0.042(2) 0.031(2) -0.0018(16) 0.0100(18) 0.0059(18) S23 0.046(3) 0.042(2) 0.042(2) -0.0014(17) 0.021(2) 0.0110(19) S24 0.038(2) 0.042(2) 0.038(2) 0.0033(17) 0.0093(19) 0.0083(18) S25 0.063(3) 0.042(2) 0.074(3) -0.003(2) 0.029(3) 0.016(2) S26 0.034(2) 0.040(2) 0.034(2) 0.0007(16) 0.0104(18) 0.0057(17) S27 0.041(2) 0.039(2) 0.034(2) 0.0013(16) 0.0135(19) 0.0064(18) S28 0.055(3) 0.037(2) 0.056(3) -0.0089(18) 0.028(2) 0.0017(19) S29 0.048(3) 0.037(2) 0.055(3) 0.0036(18) 0.013(2) 0.0077(19) S30 0.087(4) 0.041(3) 0.101(4) -0.009(3) 0.037(3) 0.014(3) C21 0.034(9) 0.032(8) 0.034(9) -0.004(6) 0.014(7) 0.013(7) C22 0.008(7) 0.051(9) 0.032(8) 0.004(6) 0.005(6) 0.000(6) C23 0.045(10) 0.036(9) 0.042(9) 0.001(7) 0.014(8) 0.003(7) C24 0.016(7) 0.038(8) 0.043(9) 0.000(6) 0.015(7) 0.007(6) C25 0.016(8) 0.044(9) 0.038(9) 0.010(7) 0.004(7) 0.012(7) C26 0.031(9) 0.043(9) 0.073(12) 0.000(8) 0.021(9) -0.002(7) _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 S1 C1A 1.692(19) . ? S1 C1B 1.777(18) . ? S1 C2 1.81(3) . ? S1 C4 1.82(3) . ? C2 C3B 1.52(2) . ? C2 C3A 1.51(2) . ? C4 C5A 1.50(2) . ? C4 C5B 1.50(2) . ? Pd1 S16 2.279(4) . ? Pd1 S12 2.287(4) . ? Pd1 S17 2.295(4) . ? Pd1 S11 2.297(4) . ? Pd1 Pd1 3.130(3) 2_567 ? S11 C11 1.694(15) . ? S12 C12 1.681(15) . ? S13 C11 1.736(14) . ? S13 C13 1.747(16) . ? S14 C13 1.724(17) . ? S14 C12 1.736(13) . ? S15 C13 1.610(17) . ? S16 C14 1.659(15) . ? S17 C15 1.697(16) . ? S18 C16 1.724(15) . ? S18 C14 1.760(15) . ? S19 C15 1.738(14) . ? S19 C16 1.751(16) . ? S20 C16 1.609(15) . ? C11 C12 1.39(2) . ? C14 C15 1.37(2) . ? Pd2 S22 2.285(4) . ? Pd2 S26 2.287(4) . ? Pd2 S21 2.290(4) . ? Pd2 S27 2.296(4) . ? Pd2 Pd2 3.139(3) 2_557 ? S21 C21 1.701(13) . ? S22 C22 1.684(14) . ? S23 C23 1.722(15) . ? S23 C21 1.754(12) . ? S24 C23 1.721(15) . ? S24 C22 1.740(14) . ? S25 C23 1.640(15) . ? S26 C24 1.701(14) . ? S27 C25 1.700(15) . ? S28 C26 1.733(17) . ? S28 C24 1.742(14) . ? S29 C26 1.723(18) . ? S29 C25 1.743(14) . ? S30 C26 1.633(16) . ? C21 C22 1.340(19) . ? C24 C25 1.35(2) . ? 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 C1A S1 C1B 43.6(17) . . ? C1A S1 C2 75.0(15) . . ? C1B S1 C2 104.3(15) . . ? C1A S1 C4 77.7(16) . . ? C1B S1 C4 102.7(15) . . ? C2 S1 C4 101.4(13) . . ? C3B C2 C3A 24(6) . . ? C3B C2 S1 102(5) . . ? C3A C2 S1 113(4) . . ? C5A C4 C5B 30(3) . . ? C5A C4 S1 100(4) . . ? C5B C4 S1 111(3) . . ? S16 Pd1 S12 89.12(14) . . ? S16 Pd1 S17 89.73(14) . . ? S12 Pd1 S17 176.37(16) . . ? S16 Pd1 S11 176.11(15) . . ? S12 Pd1 S11 90.01(14) . . ? S17 Pd1 S11 90.91(14) . . ? S16 Pd1 Pd1 92.50(12) . 2_567 ? S12 Pd1 Pd1 91.55(12) . 2_567 ? S17 Pd1 Pd1 91.94(12) . 2_567 ? S11 Pd1 Pd1 91.31(12) . 2_567 ? C11 S11 Pd1 101.0(5) . . ? C12 S12 Pd1 102.3(5) . . ? C11 S13 C13 98.7(8) . . ? C13 S14 C12 99.4(8) . . ? C14 S16 Pd1 101.4(6) . . ? C15 S17 Pd1 101.5(5) . . ? C16 S18 C14 99.3(7) . . ? C15 S19 C16 97.3(7) . . ? C12 C11 S11 124.0(11) . . ? C12 C11 S13 115.4(11) . . ? S11 C11 S13 120.5(9) . . ? C11 C12 S12 122.5(10) . . ? C11 C12 S14 115.0(11) . . ? S12 C12 S14 122.5(8) . . ? S15 C13 S14 124.6(10) . . ? S15 C13 S13 123.9(10) . . ? S14 C13 S13 111.5(9) . . ? C15 C14 S16 125.6(12) . . ? C15 C14 S18 113.4(11) . . ? S16 C14 S18 121.0(9) . . ? C14 C15 S17 121.8(11) . . ? C14 C15 S19 117.9(12) . . ? S17 C15 S19 120.3(8) . . ? S20 C16 S18 125.1(10) . . ? S20 C16 S19 122.9(9) . . ? S18 C16 S19 111.9(8) . . ? S22 Pd2 S26 89.42(14) . . ? S22 Pd2 S21 89.87(14) . . ? S26 Pd2 S21 176.55(15) . . ? S22 Pd2 S27 175.97(16) . . ? S26 Pd2 S27 89.98(14) . . ? S21 Pd2 S27 90.49(13) . . ? S22 Pd2 Pd2 91.84(12) . 2_557 ? S26 Pd2 Pd2 91.68(12) . 2_557 ? S21 Pd2 Pd2 91.71(12) . 2_557 ? S27 Pd2 Pd2 92.16(12) . 2_557 ? C21 S21 Pd2 100.7(5) . . ? C22 S22 Pd2 101.4(5) . . ? C23 S23 C21 96.7(7) . . ? C23 S24 C22 97.5(7) . . ? C24 S26 Pd2 101.8(5) . . ? C25 S27 Pd2 100.9(5) . . ? C26 S28 C24 97.5(7) . . ? C26 S29 C25 98.0(7) . . ? C22 C21 S21 124.0(10) . . ? C22 C21 S23 116.5(10) . . ? S21 C21 S23 119.4(8) . . ? C21 C22 S22 123.9(11) . . ? C21 C22 S24 115.7(10) . . ? S22 C22 S24 120.4(8) . . ? S25 C23 S24 123.6(9) . . ? S25 C23 S23 122.9(9) . . ? S24 C23 S23 113.4(8) . . ? C25 C24 S26 122.8(11) . . ? C25 C24 S28 116.1(11) . . ? S26 C24 S28 120.9(9) . . ? C24 C25 S27 124.5(11) . . ? C24 C25 S29 115.7(11) . . ? S27 C25 S29 119.8(8) . . ? S30 C26 S29 124.3(11) . . ? S30 C26 S28 123.0(11) . . ? S29 C26 S28 112.6(9) . . ? _diffrn_measured_fraction_theta_max 0.215 _diffrn_reflns_theta_full 22.5 _diffrn_measured_fraction_theta_full 0.215 _refine_diff_density_max 1.701 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.236 #===END data_pd36_bt _database_code_CSD 162840 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H13 S, 2(C6 Pd S10)' _chemical_formula_sum 'C17 H13 Pd2 S21' _chemical_formula_weight 1103.58 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' '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 7.7888(9) _cell_length_b 36.181(3) _cell_length_c 6.2573(6) _cell_angle_alpha 92.112(11) _cell_angle_beta 112.169(12) _cell_angle_gamma 88.740(12) _cell_volume 1631.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 21.0 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1086 _exptl_absorpt_coefficient_mu 2.463 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.2078 _exptl_absorpt_correction_T_max 0.5464 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS).The crystal-to-detector distance was 100 mm. 250 exposures (5 min per exposure) were obtained with 0 < \f < 250\% and with the crystals rotated through 1.0\% in \f. Crystal decay was monitored by measuring 200 reflexions per image. ; _diffrn_ambient_temperature 160(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 'STOE Imaging Plate Diffraction System' _diffrn_measurement_method '\f scan ' _diffrn_standards_decay_% 'negligible' _diffrn_reflns_number 9065 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 21.03 _reflns_number_total 3336 _reflns_number_gt 2890 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS software (Stoe, 1996)' _computing_cell_refinement 'IPDS software (Stoe, 1996)' _computing_data_reduction 'IPDS software (Stoe, 1996)' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, 1996)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0262P)^2^+81.7913P] 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 3336 _refine_ls_number_parameters 364 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.2292 _refine_ls_wR_factor_gt 0.2233 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.007 _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 S1 S 0.4437(12) 0.2531(3) 0.7689(15) 0.091(2) Uani 1 1 d U . . C1 C 0.433(6) 0.2097(11) 0.633(7) 0.132(14) Uani 1 1 d U . . H1A H 0.3994 0.1911 0.7204 0.197 Uiso 1 1 calc R . . H1B H 0.5542 0.2034 0.6275 0.197 Uiso 1 1 calc R . . H1C H 0.3394 0.2102 0.4760 0.197 Uiso 1 1 calc R . . C2 C 0.472(5) 0.2843(12) 0.558(6) 0.114(10) Uani 1 1 d U . . H2A H 0.3594 0.2838 0.4141 0.137 Uiso 1 1 calc R . . H2B H 0.4896 0.3100 0.6218 0.137 Uiso 1 1 calc R . . C3 C 0.639(5) 0.2717(12) 0.505(6) 0.123(13) Uani 1 1 d U . . H3A H 0.7371 0.2634 0.6473 0.184 Uiso 1 1 calc R . . H3B H 0.6846 0.2924 0.4449 0.184 Uiso 1 1 calc R . . H3C H 0.6039 0.2513 0.3903 0.184 Uiso 1 1 calc R . . C4 C 0.208(4) 0.2623(10) 0.728(6) 0.096(8) Uani 1 1 d U . . H4A H 0.1940 0.2883 0.7749 0.115 Uiso 1 1 calc R . . H4B H 0.1282 0.2587 0.5625 0.115 Uiso 1 1 calc R . . C5 C 0.150(5) 0.2360(11) 0.873(6) 0.110(11) Uani 1 1 d U . . H5A H 0.2535 0.2191 0.9507 0.165 Uiso 1 1 calc R . . H5B H 0.0429 0.2217 0.7729 0.165 Uiso 1 1 calc R . . H5C H 0.1180 0.2502 0.9888 0.165 Uiso 1 1 calc R . . Pd1 Pd 0.1882(2) 0.48155(5) 1.0166(3) 0.0474(6) Uani 1 1 d . . . S11 S 0.0361(8) 0.43429(17) 0.7638(10) 0.0492(15) Uani 1 1 d . . . S12 S 0.1991(8) 0.44738(17) 1.3227(10) 0.0493(15) Uani 1 1 d . . . S13 S -0.0697(9) 0.35876(18) 0.8493(11) 0.0556(16) Uani 1 1 d . . . S14 S 0.0774(9) 0.36966(18) 1.3461(11) 0.0575(17) Uani 1 1 d . . . S15 S -0.0942(10) 0.2980(2) 1.1453(12) 0.070(2) Uani 1 1 d . . . S16 S 0.3583(9) 0.52657(18) 1.2734(10) 0.0515(15) Uani 1 1 d . . . S17 S 0.1977(8) 0.51461(17) 0.7164(10) 0.0488(15) Uani 1 1 d . . . S18 S 0.5077(9) 0.59822(18) 1.2049(10) 0.0543(16) Uani 1 1 d . . . S19 S 0.3661(9) 0.58830(18) 0.7070(11) 0.0539(16) Uani 1 1 d . . . S20 S 0.5637(10) 0.65747(19) 0.9209(12) 0.0649(18) Uani 1 1 d . . . C11 C 0.030(3) 0.4007(6) 0.955(4) 0.038(5) Uani 1 1 d . . . C12 C 0.096(3) 0.4074(6) 1.183(4) 0.049(6) Uani 1 1 d . . . C13 C -0.030(3) 0.3398(6) 1.118(4) 0.049(6) Uani 1 1 d . . . C14 C 0.386(3) 0.5581(6) 1.081(5) 0.053(7) Uani 1 1 d . . . C15 C 0.315(3) 0.5535(6) 0.858(4) 0.037(5) Uani 1 1 d . . . C16 C 0.479(3) 0.6174(7) 0.941(4) 0.053(6) Uani 1 1 d . . . Pd2 Pd 0.1850(2) 0.01911(5) 1.0218(3) 0.0477(6) Uani 1 1 d . . . S21 S 0.1973(8) -0.01421(17) 0.7086(10) 0.0502(15) Uani 1 1 d . . . S22 S 0.3596(9) -0.02569(18) 1.2625(10) 0.0510(15) Uani 1 1 d . . . S23 S 0.3748(9) -0.08752(18) 0.6712(10) 0.0528(16) Uani 1 1 d . . . S24 S 0.5180(9) -0.09763(18) 1.1650(10) 0.0543(16) Uani 1 1 d . . . S25 S 0.5795(10) -0.1564(2) 0.8587(12) 0.0657(18) Uani 1 1 d . . . S26 S 0.1911(8) 0.05370(17) 1.3405(10) 0.0512(15) Uani 1 1 d . . . S27 S 0.0286(8) 0.06611(17) 0.7857(10) 0.0501(15) Uani 1 1 d . . . S28 S 0.0567(9) 0.13113(18) 1.3876(11) 0.0574(17) Uani 1 1 d . . . S29 S -0.0903(9) 0.14154(18) 0.8924(11) 0.0588(17) Uani 1 1 d . . . S30 S -0.1233(11) 0.2026(2) 1.2088(14) 0.072(2) Uani 1 1 d . . . C21 C 0.321(3) -0.0528(6) 0.839(4) 0.043(6) Uani 1 1 d . . . C22 C 0.391(3) -0.0578(7) 1.059(5) 0.055(6) Uani 1 1 d . . . C23 C 0.492(3) -0.1168(7) 0.892(4) 0.058(7) Uani 1 1 d . . . C24 C 0.083(3) 0.0937(6) 1.213(5) 0.055(7) Uani 1 1 d . . . C25 C 0.016(3) 0.0990(6) 0.983(4) 0.043(6) Uani 1 1 d . . . C26 C -0.054(3) 0.1613(7) 1.171(4) 0.056(6) 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 S1 0.084(5) 0.097(7) 0.085(5) 0.000(4) 0.023(4) -0.003(5) C1 0.14(3) 0.143(18) 0.16(4) -0.07(2) 0.12(3) -0.04(2) C2 0.09(2) 0.17(3) 0.08(2) 0.026(18) 0.027(17) 0.00(2) C3 0.12(3) 0.17(4) 0.08(2) 0.05(2) 0.043(19) 0.03(2) C4 0.086(13) 0.10(2) 0.10(2) -0.011(17) 0.038(17) -0.010(16) C5 0.086(19) 0.13(3) 0.11(3) 0.03(2) 0.033(19) 0.01(2) Pd1 0.0461(11) 0.0507(13) 0.0451(11) 0.0025(8) 0.0165(9) -0.0033(9) S11 0.050(4) 0.050(4) 0.046(3) -0.001(3) 0.017(3) -0.005(3) S12 0.046(4) 0.052(4) 0.047(3) -0.002(3) 0.015(3) -0.005(3) S13 0.054(4) 0.052(4) 0.056(4) 0.003(3) 0.015(3) -0.005(3) S14 0.065(4) 0.053(4) 0.055(4) 0.008(3) 0.023(3) -0.001(3) S15 0.077(5) 0.056(5) 0.073(5) 0.007(3) 0.025(4) -0.010(4) S16 0.056(4) 0.053(4) 0.041(3) 0.004(3) 0.013(3) -0.003(3) S17 0.050(4) 0.049(4) 0.046(3) 0.000(3) 0.016(3) -0.005(3) S18 0.050(4) 0.053(4) 0.055(4) -0.001(3) 0.014(3) -0.007(3) S19 0.054(4) 0.048(4) 0.061(4) 0.006(3) 0.023(3) -0.004(3) S20 0.066(4) 0.054(5) 0.075(4) 0.004(3) 0.026(4) -0.009(3) C11 0.035(12) 0.039(14) 0.042(13) -0.006(10) 0.018(10) 0.002(10) C12 0.033(13) 0.040(15) 0.080(19) 0.008(12) 0.029(13) 0.016(10) C13 0.049(14) 0.039(15) 0.047(13) 0.000(10) 0.005(11) 0.007(11) C14 0.041(14) 0.025(14) 0.10(2) 0.020(12) 0.029(14) 0.014(10) C15 0.045(13) 0.033(14) 0.040(13) 0.007(10) 0.025(11) 0.002(10) C16 0.042(14) 0.063(17) 0.056(15) -0.002(12) 0.020(12) -0.007(12) Pd2 0.0459(11) 0.0490(13) 0.0477(11) 0.0006(8) 0.0175(9) 0.0021(9) S21 0.053(4) 0.046(4) 0.050(3) 0.004(3) 0.018(3) 0.006(3) S22 0.054(4) 0.055(4) 0.040(3) 0.002(3) 0.014(3) 0.004(3) S23 0.054(4) 0.050(4) 0.057(4) -0.001(3) 0.025(3) 0.010(3) S24 0.052(4) 0.058(4) 0.052(4) 0.006(3) 0.018(3) 0.009(3) S25 0.066(4) 0.059(5) 0.075(4) 0.001(3) 0.030(4) 0.009(3) S26 0.048(4) 0.053(4) 0.051(4) 0.004(3) 0.017(3) 0.004(3) S27 0.049(4) 0.052(4) 0.050(3) 0.005(3) 0.020(3) 0.002(3) S28 0.060(4) 0.053(4) 0.061(4) -0.005(3) 0.025(3) -0.001(3) S29 0.053(4) 0.053(4) 0.066(4) 0.002(3) 0.019(3) 0.006(3) S30 0.076(5) 0.051(5) 0.094(5) -0.001(4) 0.037(4) 0.009(4) C21 0.054(15) 0.033(14) 0.049(15) -0.016(10) 0.030(12) 0.001(10) C22 0.040(14) 0.061(18) 0.072(19) -0.002(13) 0.031(13) 0.004(12) C23 0.048(15) 0.066(18) 0.061(16) -0.012(13) 0.023(13) -0.008(13) C24 0.033(13) 0.037(15) 0.11(2) -0.011(13) 0.045(14) -0.011(11) C25 0.044(14) 0.038(15) 0.048(14) 0.019(11) 0.016(11) -0.008(10) C26 0.048(15) 0.058(17) 0.065(16) 0.002(12) 0.023(13) -0.003(12) _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 S1 C1 1.74(3) . ? S1 C4 1.78(3) . ? S1 C2 1.85(4) . ? C2 C3 1.52(5) . ? C4 C5 1.53(4) . ? Pd1 S17 2.289(6) . ? Pd1 S12 2.291(6) . ? Pd1 S16 2.299(6) . ? Pd1 S11 2.303(6) . ? Pd1 Pd1 3.132(4) 2_567 ? S11 C11 1.75(2) . ? S12 C12 1.71(2) . ? S13 C11 1.71(2) . ? S13 C13 1.75(2) . ? S14 C13 1.71(2) . ? S14 C12 1.77(2) . ? S15 C13 1.64(2) . ? S16 C14 1.76(2) . ? S17 C15 1.72(2) . ? S18 C14 1.74(2) . ? S18 C16 1.75(2) . ? S19 C16 1.72(2) . ? S19 C15 1.74(2) . ? S20 C16 1.63(3) . ? C11 C12 1.34(3) . ? C14 C15 1.30(3) . ? Pd2 S21 2.295(6) . ? Pd2 S22 2.299(6) . ? Pd2 S26 2.300(6) . ? Pd2 S27 2.301(6) . ? Pd2 Pd2 3.138(4) 2_557 ? S21 C21 1.72(2) . ? S22 C22 1.77(3) . ? S23 C23 1.73(3) . ? S23 C21 1.75(2) . ? S24 C22 1.73(3) . ? S24 C23 1.76(2) . ? S25 C23 1.61(3) . ? S26 C24 1.72(3) . ? S27 C25 1.71(2) . ? S28 C26 1.72(3) . ? S28 C24 1.76(2) . ? S29 C25 1.74(2) . ? S29 C26 1.78(2) . ? S30 C26 1.62(3) . ? C21 C22 1.30(3) . ? C24 C25 1.35(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C4 102.9(17) . . ? C1 S1 C2 102(2) . . ? C4 S1 C2 100.4(17) . . ? C3 C2 S1 109(3) . . ? C5 C4 S1 109(2) . . ? S17 Pd1 S12 176.1(2) . . ? S17 Pd1 S16 90.0(2) . . ? S12 Pd1 S16 89.0(2) . . ? S17 Pd1 S11 90.4(2) . . ? S12 Pd1 S11 90.4(2) . . ? S16 Pd1 S11 176.1(2) . . ? S17 Pd1 Pd1 92.19(18) . 2_567 ? S12 Pd1 Pd1 91.57(17) . 2_567 ? S16 Pd1 Pd1 92.35(18) . 2_567 ? S11 Pd1 Pd1 91.47(17) . 2_567 ? C11 S11 Pd1 101.3(7) . . ? C12 S12 Pd1 100.9(9) . . ? C11 S13 C13 96.5(11) . . ? C13 S14 C12 97.2(12) . . ? C14 S16 Pd1 100.4(9) . . ? C15 S17 Pd1 101.7(7) . . ? C14 S18 C16 94.6(12) . . ? C16 S19 C15 97.5(11) . . ? C12 C11 S13 118.6(17) . . ? C12 C11 S11 121.5(17) . . ? S13 C11 S11 119.9(12) . . ? C11 C12 S12 125.9(18) . . ? C11 C12 S14 114.4(17) . . ? S12 C12 S14 119.7(15) . . ? S15 C13 S14 123.8(14) . . ? S15 C13 S13 122.9(13) . . ? S14 C13 S13 113.3(13) . . ? C15 C14 S18 120.1(18) . . ? C15 C14 S16 123.6(18) . . ? S18 C14 S16 116.2(16) . . ? C14 C15 S17 124.2(17) . . ? C14 C15 S19 114.5(17) . . ? S17 C15 S19 121.0(12) . . ? S20 C16 S19 123.9(15) . . ? S20 C16 S18 123.0(14) . . ? S19 C16 S18 113.0(14) . . ? S21 Pd2 S22 90.1(2) . . ? S21 Pd2 S26 176.4(2) . . ? S22 Pd2 S26 89.2(2) . . ? S21 Pd2 S27 90.3(2) . . ? S22 Pd2 S27 176.1(2) . . ? S26 Pd2 S27 90.2(2) . . ? S21 Pd2 Pd2 91.87(18) . 2_557 ? S22 Pd2 Pd2 91.50(18) . 2_557 ? S26 Pd2 Pd2 91.63(17) . 2_557 ? S27 Pd2 Pd2 92.38(17) . 2_557 ? C21 S21 Pd2 101.2(7) . . ? C22 S22 Pd2 100.7(9) . . ? C23 S23 C21 97.6(12) . . ? C22 S24 C23 95.2(13) . . ? C24 S26 Pd2 100.8(9) . . ? C25 S27 Pd2 101.5(8) . . ? C26 S28 C24 98.0(13) . . ? C25 S29 C26 97.2(12) . . ? C22 C21 S21 125.3(17) . . ? C22 C21 S23 114.7(19) . . ? S21 C21 S23 119.8(13) . . ? C21 C22 S24 119.9(19) . . ? C21 C22 S22 123(2) . . ? S24 C22 S22 117.4(15) . . ? S25 C23 S23 124.9(15) . . ? S25 C23 S24 122.8(16) . . ? S23 C23 S24 112.3(14) . . ? C25 C24 S26 124.3(18) . . ? C25 C24 S28 116.1(19) . . ? S26 C24 S28 119.6(17) . . ? C24 C25 S27 123.2(18) . . ? C24 C25 S29 116.6(18) . . ? S27 C25 S29 120.3(13) . . ? S30 C26 S28 125.2(15) . . ? S30 C26 S29 122.6(15) . . ? S28 C26 S29 112.1(14) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 21.03 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.757 _refine_diff_density_min -0.984 _refine_diff_density_rms 0.207 #===END data_pd18_bt _database_code_CSD 162841 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H13 S, 2(C6 Pd S10)' _chemical_formula_sum 'C17 H13 Pd2 S21' _chemical_formula_weight 1103.58 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.7877(12) _cell_length_b 18.323(3) _cell_length_c 6.2846(10) _cell_angle_alpha 96.80(2) _cell_angle_beta 112.257(18) _cell_angle_gamma 84.17(2) _cell_volume 822.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 24.0 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 543 _exptl_absorpt_coefficient_mu 2.443 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5385 _exptl_absorpt_correction_T_max 1.1389 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS).The crystal-to-detector distance was 80 mm. 209 exposures (3 min per exposure) were obtained with 0 < \f < 250\% and with the crystals rotated through 1.2\% in \f. Crystal decay was monitored by measuring 200 reflexions per image. ; _diffrn_ambient_temperature 160(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 'STOE Imaging Plate Diffraction System' _diffrn_measurement_method '\f scan ' _diffrn_standards_decay_% 'negligible' _diffrn_reflns_number 6587 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 24.08 _reflns_number_total 2415 _reflns_number_gt 2250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS software (Stoe, 1996)' _computing_cell_refinement 'IPDS software (Stoe, 1996)' _computing_data_reduction 'IPDS software (Stoe, 1996)' _computing_structure_solution 'Sir92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Cameron (Watkin, 1993)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0509P)^2^+1.9613P] 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 2415 _refine_ls_number_parameters 208 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.013 _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 0.19262(5) 0.462940(16) 0.50681(5) 0.02012(16) Uani 1 1 d . . . S11 S 0.19349(18) 0.52913(6) 0.21893(19) 0.0250(3) Uani 1 1 d . . . S12 S 0.35108(18) 0.55246(6) 0.77802(19) 0.0258(3) Uani 1 1 d . . . S13 S 0.34154(18) 0.67499(6) 0.2332(2) 0.0288(3) Uani 1 1 d . . . S14 S 0.47885(19) 0.69603(7) 0.7314(2) 0.0301(3) Uani 1 1 d . . . S15 S 0.5167(2) 0.81320(8) 0.4658(3) 0.0451(4) Uani 1 1 d . . . S16 S 0.21039(17) 0.39408(6) 0.79868(19) 0.0237(3) Uani 1 1 d . . . S17 S 0.05396(17) 0.36899(6) 0.23657(19) 0.0249(3) Uani 1 1 d . . . S18 S 0.10733(19) 0.23983(6) 0.7874(2) 0.0313(3) Uani 1 1 d . . . S19 S -0.03019(19) 0.21809(6) 0.2906(2) 0.0327(3) Uani 1 1 d . . . S20 S -0.0342(3) 0.09522(8) 0.5572(3) 0.0557(5) Uani 1 1 d . . . C11 C 0.3036(7) 0.6044(2) 0.3713(8) 0.0216(9) Uani 1 1 d . . . C12 C 0.3694(6) 0.6144(2) 0.6090(8) 0.0222(10) Uani 1 1 d . . . C13 C 0.4474(7) 0.7324(3) 0.4763(9) 0.0300(11) Uani 1 1 d . . . C14 C 0.1186(7) 0.3148(2) 0.6461(8) 0.0244(10) Uani 1 1 d . . . C15 C 0.0538(7) 0.3044(2) 0.4101(8) 0.0229(10) Uani 1 1 d . . . C16 C 0.0126(8) 0.1799(3) 0.5449(10) 0.0356(12) Uani 1 1 d . . . S1 S 0.5569(7) -0.0003(3) 0.1224(6) 0.0813(13) Uani 0.50 1 d PDU A -1 C1 C 0.506(3) -0.0920(9) -0.005(3) 0.076(4) Uani 0.50 1 d PU A -1 H1A H 0.6223 -0.1225 0.0242 0.091 Uiso 0.50 1 calc PR A -1 H1B H 0.4388 -0.0911 -0.1721 0.091 Uiso 0.50 1 calc PR A -1 H1C H 0.4290 -0.1128 0.0621 0.091 Uiso 0.50 1 calc PR A -1 C2 C 0.655(5) 0.0320(9) -0.069(4) 0.129(8) Uani 0.50 1 d PDU A -1 H2A H 0.5622 0.0680 -0.1635 0.154 Uiso 0.50 1 calc PR A -1 H2B H 0.7645 0.0598 0.0297 0.154 Uiso 0.50 1 calc PR A -1 C3 C 0.717(5) -0.0210(13) -0.234(5) 0.179(15) Uani 0.50 1 d PDU A -1 H3A H 0.7760 0.0059 -0.3105 0.215 Uiso 0.50 1 calc PR A -1 H3B H 0.6084 -0.0444 -0.3494 0.215 Uiso 0.50 1 calc PR A -1 H3C H 0.8056 -0.0588 -0.1474 0.215 Uiso 0.50 1 calc PR A -1 C4 C 0.369(4) 0.0521(16) 0.061(5) 0.150(9) Uani 0.50 1 d PU A -1 H4A H 0.3881 0.0989 0.1604 0.180 Uiso 0.50 1 calc PR A -1 H4B H 0.3190 0.0628 -0.1031 0.180 Uiso 0.50 1 calc PR A -1 C5 C 0.241(4) 0.005(3) 0.111(5) 0.227(19) Uani 0.50 1 d PU A -1 H5A H 0.1156 0.0284 0.0635 0.272 Uiso 0.50 1 calc PR A -1 H5B H 0.2883 -0.0015 0.2763 0.272 Uiso 0.50 1 calc PR A -1 H5C H 0.2376 -0.0438 0.0244 0.272 Uiso 0.50 1 calc PR A -1 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 0.0217(3) 0.0195(2) 0.0177(2) 0.00124(14) 0.00538(17) -0.00281(14) S11 0.0325(7) 0.0227(6) 0.0181(6) 0.0006(4) 0.0067(5) -0.0066(5) S12 0.0301(8) 0.0253(6) 0.0187(6) 0.0012(4) 0.0042(5) -0.0071(5) S13 0.0330(8) 0.0266(6) 0.0285(6) 0.0051(5) 0.0112(6) -0.0067(5) S14 0.0306(8) 0.0266(6) 0.0288(6) -0.0011(5) 0.0052(6) -0.0098(5) S15 0.0459(10) 0.0293(7) 0.0602(9) 0.0065(6) 0.0164(8) -0.0123(6) S16 0.0283(7) 0.0225(6) 0.0195(6) 0.0020(4) 0.0070(5) -0.0043(5) S17 0.0296(7) 0.0232(6) 0.0201(6) 0.0003(4) 0.0066(5) -0.0056(5) S18 0.0396(8) 0.0238(6) 0.0338(7) 0.0069(5) 0.0159(6) -0.0026(5) S19 0.0361(8) 0.0227(6) 0.0343(7) -0.0005(5) 0.0070(6) -0.0073(5) S20 0.0713(12) 0.0282(8) 0.0644(10) 0.0080(7) 0.0173(9) -0.0157(7) C11 0.019(3) 0.019(2) 0.027(2) 0.0051(18) 0.008(2) -0.0015(17) C12 0.015(3) 0.021(2) 0.027(2) -0.0015(18) 0.004(2) -0.0017(17) C13 0.022(3) 0.029(3) 0.035(3) 0.003(2) 0.007(2) 0.001(2) C14 0.022(3) 0.024(2) 0.029(2) 0.0081(19) 0.010(2) 0.0017(19) C15 0.020(3) 0.018(2) 0.030(2) -0.0011(18) 0.008(2) -0.0025(18) C16 0.033(3) 0.027(3) 0.043(3) 0.006(2) 0.009(3) -0.003(2) S1 0.080(3) 0.104(3) 0.0338(18) 0.0002(18) -0.0025(19) 0.010(2) C1 0.088(13) 0.091(8) 0.068(9) 0.032(7) 0.042(9) -0.014(8) C2 0.25(3) 0.057(10) 0.094(15) 0.016(9) 0.066(17) -0.034(12) C3 0.34(4) 0.148(18) 0.13(2) -0.083(16) 0.16(2) -0.19(2) C4 0.140(17) 0.140(16) 0.112(16) -0.006(15) 0.001(14) 0.047(13) C5 0.066(14) 0.49(6) 0.077(19) 0.02(3) -0.032(16) -0.06(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S11 2.2966(12) . ? Pd1 S12 2.2966(14) . ? Pd1 S16 2.3012(12) . ? Pd1 S17 2.3043(13) . ? Pd1 Pd1 3.1397(9) 2_566 ? S11 C11 1.692(5) . ? S12 C12 1.693(5) . ? S13 C13 1.721(5) . ? S13 C11 1.746(4) . ? S14 C13 1.732(5) . ? S14 C12 1.745(5) . ? S15 C13 1.643(5) . ? S16 C14 1.704(5) . ? S17 C15 1.702(5) . ? S18 C16 1.729(6) . ? S18 C14 1.748(4) . ? S19 C16 1.723(5) . ? S19 C15 1.746(4) . ? S20 C16 1.646(5) . ? C11 C12 1.379(7) . ? C14 C15 1.370(7) . ? S1 C4 1.61(3) . ? S1 C1 1.789(18) . ? S1 C2 1.831(15) . ? C2 C3 1.509(18) . ? C4 C5 1.52(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 S11 Pd1 S12 89.84(4) . . ? S11 Pd1 S16 176.46(4) . . ? S12 Pd1 S16 89.52(4) . . ? S11 Pd1 S17 90.18(4) . . ? S12 Pd1 S17 175.89(4) . . ? S16 Pd1 S17 90.21(4) . . ? S11 Pd1 Pd1 92.70(4) . 2_566 ? S12 Pd1 Pd1 91.83(4) . 2_566 ? S16 Pd1 Pd1 90.80(4) . 2_566 ? S17 Pd1 Pd1 92.27(4) . 2_566 ? C11 S11 Pd1 101.82(16) . . ? C12 S12 Pd1 101.48(16) . . ? C13 S13 C11 97.5(2) . . ? C13 S14 C12 97.4(2) . . ? C14 S16 Pd1 101.26(16) . . ? C15 S17 Pd1 100.97(16) . . ? C16 S18 C14 97.5(2) . . ? C16 S19 C15 97.8(2) . . ? C12 C11 S11 123.1(3) . . ? C12 C11 S13 115.7(3) . . ? S11 C11 S13 121.2(3) . . ? C11 C12 S12 123.7(3) . . ? C11 C12 S14 115.6(3) . . ? S12 C12 S14 120.7(3) . . ? S15 C13 S13 122.8(3) . . ? S15 C13 S14 123.4(3) . . ? S13 C13 S14 113.7(3) . . ? C15 C14 S16 123.4(3) . . ? C15 C14 S18 115.8(4) . . ? S16 C14 S18 120.8(3) . . ? C14 C15 S17 124.1(4) . . ? C14 C15 S19 115.6(3) . . ? S17 C15 S19 120.3(3) . . ? S20 C16 S19 123.6(3) . . ? S20 C16 S18 123.1(3) . . ? S19 C16 S18 113.3(3) . . ? C4 S1 C1 110.3(13) . . ? C4 S1 C2 99.7(15) . . ? C1 S1 C2 100.9(7) . . ? C3 C2 S1 121.4(13) . . ? C5 C4 S1 101(3) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 24.08 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.901 _refine_diff_density_min -1.198 _refine_diff_density_rms 0.121 #===END data_pd18ta _database_code_CSD 162842 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H13 S, 2(C6 Pd S10)' _chemical_formula_sum 'C17 H13 Pd2 S21' _chemical_formula_weight 1103.58 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' '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 7.844(5) _cell_length_b 18.397(5) _cell_length_c 6.320(5) _cell_angle_alpha 97.654(5) _cell_angle_beta 112.076(5) _cell_angle_gamma 83.572(5) _cell_volume 835.7(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 16.5 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 543 _exptl_absorpt_coefficient_mu 2.405 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.5886 _exptl_absorpt_correction_T_max 0.8863 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 7 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 Enraf-Nonius' _diffrn_measurement_method 'omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1 _diffrn_reflns_number 4847 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 29.96 _reflns_number_total 4847 _reflns_number_gt 3616 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Cameron (Watkin, 1998)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0443P)^2^+0.3621P] 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 4847 _refine_ls_number_parameters 208 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _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 0.19289(3) 0.463118(11) 0.50583(4) 0.02881(7) Uani 1 1 d . . . S11 S 0.19283(11) 0.52939(4) 0.22268(12) 0.03559(15) Uani 1 1 d . . . S12 S 0.34886(11) 0.55239(4) 0.77844(12) 0.03733(16) Uani 1 1 d . . . S13 S 0.33840(12) 0.67470(4) 0.24293(14) 0.04119(17) Uani 1 1 d . . . S14 S 0.47500(11) 0.69543(4) 0.73809(14) 0.04289(18) Uani 1 1 d . . . S15 S 0.51224(16) 0.81245(5) 0.4796(2) 0.0629(3) Uani 1 1 d . . . S16 S 0.21108(10) 0.39451(4) 0.79312(12) 0.03459(15) Uani 1 1 d . . . S17 S 0.05638(11) 0.36938(4) 0.23423(12) 0.03594(15) Uani 1 1 d . . . S18 S 0.11200(13) 0.24051(4) 0.77640(15) 0.04447(18) Uani 1 1 d . . . S19 S -0.02455(13) 0.21860(4) 0.28222(15) 0.04668(19) Uani 1 1 d . . . S20 S -0.0275(2) 0.09625(6) 0.5429(2) 0.0780(4) Uani 1 1 d . . . C11 C 0.3019(4) 0.60421(15) 0.3765(5) 0.0309(5) Uani 1 1 d . . . C12 C 0.3673(4) 0.61424(14) 0.6134(5) 0.0302(5) Uani 1 1 d . . . C13 C 0.4440(4) 0.73167(17) 0.4868(6) 0.0401(7) Uani 1 1 d . . . C14 C 0.1221(4) 0.31506(15) 0.6391(5) 0.0321(5) Uani 1 1 d . . . C15 C 0.0564(4) 0.30511(15) 0.4036(5) 0.0331(6) Uani 1 1 d . . . C16 C 0.0186(5) 0.18099(18) 0.5344(6) 0.0468(8) Uani 1 1 d . . . S1 S 0.5557(5) 0.0055(2) 0.1207(5) 0.1013(10) Uani 0.50 1 d PU A -1 C1 C 0.515(2) -0.0941(8) 0.011(3) 0.122(5) Uani 0.50 1 d PU A -1 H1A H 0.4086 -0.0969 -0.1289 0.183 Uiso 0.50 1 calc PR A -1 H1B H 0.4938 -0.1184 0.1237 0.183 Uiso 0.50 1 calc PR A -1 H1C H 0.6207 -0.1176 -0.0172 0.183 Uiso 0.50 1 calc PR A -1 C2 C 0.596(4) 0.0449(12) -0.063(4) 0.183(7) Uani 0.50 1 d PDU A -1 H2A H 0.4893 0.0426 -0.2050 0.220 Uiso 0.50 1 calc PR A -1 H2B H 0.6137 0.0963 -0.0076 0.220 Uiso 0.50 1 calc PR A -1 C3 C 0.759(3) 0.0113(18) -0.109(4) 0.227(14) Uani 0.50 1 d PDU A -1 H3A H 0.8328 -0.0181 0.0127 0.340 Uiso 0.50 1 calc PR A -1 H3B H 0.8307 0.0492 -0.1165 0.340 Uiso 0.50 1 calc PR A -1 H3C H 0.7210 -0.0192 -0.2518 0.340 Uiso 0.50 1 calc PR A -1 C4 C 0.327(2) 0.0385(10) 0.058(3) 0.151(6) Uani 0.50 1 d PDU A -1 H4A H 0.3127 0.0918 0.0703 0.182 Uiso 0.50 1 calc PR A -1 H4B H 0.2463 0.0187 -0.0918 0.182 Uiso 0.50 1 calc PR A -1 C5 C 0.296(4) 0.0091(15) 0.242(4) 0.220(12) Uani 0.50 1 d PDU A -1 H5A H 0.2577 -0.0401 0.1931 0.330 Uiso 0.50 1 calc PR A -1 H5B H 0.2020 0.0393 0.2810 0.330 Uiso 0.50 1 calc PR A -1 H5C H 0.4085 0.0085 0.3745 0.330 Uiso 0.50 1 calc PR A -1 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 0.02763(11) 0.02997(10) 0.02894(10) 0.00299(7) 0.01075(8) -0.00093(7) S11 0.0431(4) 0.0346(3) 0.0297(3) 0.0014(3) 0.0134(3) -0.0071(3) S12 0.0412(4) 0.0385(4) 0.0297(3) 0.0029(3) 0.0090(3) -0.0070(3) S13 0.0442(4) 0.0399(4) 0.0437(4) 0.0079(3) 0.0188(3) -0.0062(3) S14 0.0408(4) 0.0397(4) 0.0438(4) -0.0020(3) 0.0105(3) -0.0108(3) S15 0.0645(6) 0.0419(5) 0.0878(8) 0.0073(5) 0.0304(6) -0.0160(4) S16 0.0385(4) 0.0343(3) 0.0310(3) 0.0045(3) 0.0122(3) -0.0030(3) S17 0.0407(4) 0.0354(3) 0.0313(3) 0.0016(3) 0.0126(3) -0.0051(3) S18 0.0536(5) 0.0357(4) 0.0499(4) 0.0104(3) 0.0241(4) -0.0009(3) S19 0.0494(5) 0.0347(4) 0.0501(5) -0.0002(3) 0.0117(4) -0.0077(3) S20 0.0991(9) 0.0406(5) 0.0911(8) 0.0131(5) 0.0244(7) -0.0212(5) C11 0.0264(13) 0.0310(12) 0.0361(14) 0.0043(10) 0.0122(11) -0.0007(10) C12 0.0253(12) 0.0286(12) 0.0360(14) 0.0006(10) 0.0121(11) 0.0012(10) C13 0.0290(14) 0.0377(15) 0.0552(19) 0.0049(13) 0.0170(13) -0.0026(12) C14 0.0295(13) 0.0307(12) 0.0401(15) 0.0086(11) 0.0171(11) 0.0034(10) C15 0.0292(13) 0.0273(12) 0.0421(15) 0.0012(10) 0.0138(12) 0.0013(10) C16 0.0420(18) 0.0355(15) 0.063(2) 0.0079(14) 0.0180(16) -0.0019(13) S1 0.096(2) 0.128(3) 0.0549(14) 0.0029(15) 0.0042(14) 0.0042(19) C1 0.152(14) 0.099(7) 0.128(12) 0.034(8) 0.070(11) 0.035(8) C2 0.247(19) 0.167(16) 0.144(14) 0.041(13) 0.061(15) -0.061(16) C3 0.147(16) 0.44(4) 0.097(14) 0.05(2) 0.016(10) -0.118(19) C4 0.155(11) 0.153(15) 0.103(11) 0.005(10) 0.022(10) 0.065(12) C5 0.26(3) 0.28(3) 0.175(19) -0.095(18) 0.14(2) -0.14(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S11 2.2954(14) . ? Pd1 S12 2.2965(11) . ? Pd1 S16 2.2990(14) . ? Pd1 S17 2.3044(11) . ? Pd1 Pd1 3.1534(18) 2_566 ? S11 C11 1.689(3) . ? S12 C12 1.694(3) . ? S13 C13 1.722(3) . ? S13 C11 1.741(3) . ? S14 C13 1.726(4) . ? S14 C12 1.742(3) . ? S15 C13 1.647(3) . ? S16 C14 1.706(3) . ? S17 C15 1.698(3) . ? S18 C16 1.722(4) . ? S18 C14 1.742(3) . ? S19 C16 1.723(4) . ? S19 C15 1.749(3) . ? S20 C16 1.652(3) . ? C11 C12 1.382(4) . ? C14 C15 1.373(4) . ? S1 C2 1.587(19) . ? S1 C4 1.745(17) . ? S1 C1 1.888(15) . ? C2 C3 1.472(18) . ? C4 C5 1.452(17) . ? 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 S11 Pd1 S12 89.78(5) . . ? S11 Pd1 S16 176.57(3) . . ? S12 Pd1 S16 89.47(5) . . ? S11 Pd1 S17 90.32(5) . . ? S12 Pd1 S17 175.93(3) . . ? S16 Pd1 S17 90.19(5) . . ? S11 Pd1 Pd1 92.58(3) . 2_566 ? S12 Pd1 Pd1 92.16(4) . 2_566 ? S16 Pd1 Pd1 90.80(3) . 2_566 ? S17 Pd1 Pd1 91.90(4) . 2_566 ? C11 S11 Pd1 101.92(11) . . ? C12 S12 Pd1 101.63(11) . . ? C13 S13 C11 97.62(15) . . ? C13 S14 C12 97.32(15) . . ? C14 S16 Pd1 101.34(11) . . ? C15 S17 Pd1 101.05(11) . . ? C16 S18 C14 97.57(16) . . ? C16 S19 C15 97.57(16) . . ? C12 C11 S11 123.2(2) . . ? C12 C11 S13 115.4(2) . . ? S11 C11 S13 121.37(17) . . ? C11 C12 S12 123.5(2) . . ? C11 C12 S14 115.8(2) . . ? S12 C12 S14 120.74(17) . . ? S15 C13 S13 122.8(2) . . ? S15 C13 S14 123.4(2) . . ? S13 C13 S14 113.75(18) . . ? C15 C14 S16 123.2(2) . . ? C15 C14 S18 115.9(2) . . ? S16 C14 S18 120.89(18) . . ? C14 C15 S17 124.2(2) . . ? C14 C15 S19 115.3(2) . . ? S17 C15 S19 120.47(18) . . ? S20 C16 S18 123.2(2) . . ? S20 C16 S19 123.2(2) . . ? S18 C16 S19 113.60(18) . . ? C2 S1 C4 98.2(11) . . ? C2 S1 C1 109.3(9) . . ? C4 S1 C1 98.2(8) . . ? C3 C2 S1 112.6(17) . . ? C5 C4 S1 98.2(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.96 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.556 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.100 #===END