# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Alexander J. Blake' _publ_contact_author_address ; School of Chemistry The University of Nottingham University Park NOTTINGHAM NG7 2RD UNITED KINGDOM ; _publ_contact_author_email A.J.BLAKE@NOTTINGHAM.AC.UK _publ_section_title ; High pressure co-ordination chemistry of a palladium thioether complex: pressure versus electrons ; _exptl_special_details ; Sequence of high pressure experiments: Crystal 1, pressure = ambient - successful Crystal 1, pressure = 12.6 kilobars - successful Crystal 1, pressure = 23.5 kilobars - successful Crystal 1, pressure = 36 kilobars - successful Crystal 1, pressure = 48.7 kilobars - unsuccessful Crystal 1, pressure = 60.2 kilobars - unsuccessful Crystal 1, pressure = 73.1 kilobars - successful Crystal 1, pressure = 76.8 kilobars - successful Crystal 1, pressure = 53.5 kilobars - successful Crystal 1, pressure = 90.4 kilobars - unsuccessful Crystal 1, pressure = 0.6 kilobars - unsuccessful Crystal 2, pressure = 46 kilobars - successful Crystal 2, pressure = 42.5 kilobars - successful Crystal 2, pressure = 60.8 kilobars - unsuccessful ; loop_ _publ_author_name 'A. Blake' 'David Allan' 'Deguang Huang' 'Timothy J. Prior' 'M. Schroder' data_s3pdc1 _database_code_depnum_ccdc_archive 'CCDC 607262' # Crystal 1, pressure = ambient _refine_special_details ; The completeness of the data is severely restricted by the geometry of the diamond anvil cell. As a result only Pd, Cl and S atoms were refined anisotropically. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Cl2 Pd S3' _chemical_formula_sum 'C6 H12 Cl2 Pd S3' _chemical_formula_weight 357.64 _cell_measurement_pressure 0 _diffrn_ambient_pressure 0 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.5626(11) _cell_length_b 12.1894(15) _cell_length_c 12.239(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1128.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 692 _cell_measurement_theta_min 3.7 _cell_measurement_theta_max 20.0 _exptl_crystal_description tablet _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 2.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.247 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.8406 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 16.2 SMX' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2458 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_sigmaI/netI 0.057 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 26.72 _reflns_number_total 550 _reflns_number_gt 509 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2004)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON' _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^)+(0.046P)^2^+] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(13) _refine_ls_number_reflns 550 _refine_ls_number_parameters 79 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 1.19285(13) 0.13812(7) 0.3735(2) 0.0271(15) Uani 1 1 d U . . Cl1 Cl 0.0415(5) 0.0080(3) 0.4770(9) 0.053(4) Uani 1 1 d U . . Cl2 Cl 0.4204(5) 0.0182(3) 0.3283(9) 0.059(6) Uani 1 1 d U . . S1 S -0.0186(5) 0.1616(3) 0.1521(9) 0.039(3) Uani 1 1 d DU . . C2 C -0.164(2) 0.2636(10) 0.2108(17) 0.057(6) Uiso 1 1 d DU . . H2A H -0.1161 0.3357 0.1942 0.068 Uiso 1 1 calc R . . H2B H -0.2780 0.2581 0.1752 0.068 Uiso 1 1 calc R . . C3 C -0.1915(18) 0.2558(11) 0.3329(16) 0.037(5) Uiso 1 1 d DU . . H3A H -0.2534 0.1875 0.3463 0.045 Uiso 1 1 calc R . . H3B H -0.2722 0.3144 0.3527 0.045 Uiso 1 1 calc R . . S4 S -0.0101(5) 0.2613(3) 0.4284(8) 0.028(4) Uani 1 1 d DU . . C5 C 0.0943(17) 0.3924(8) 0.4009(19) 0.039(4) Uiso 1 1 d DU . . H5A H 0.0020 0.4469 0.3924 0.047 Uiso 1 1 calc R . . H5B H 0.1632 0.4128 0.4646 0.047 Uiso 1 1 calc R . . C6 C 0.2139(16) 0.3981(7) 0.3017(19) 0.028(4) Uiso 1 1 d DU . . H6A H 0.2923 0.4607 0.3085 0.033 Uiso 1 1 calc R . . H6B H 0.1427 0.4082 0.2366 0.033 Uiso 1 1 calc R . . S7 S 0.3446(5) 0.2732(3) 0.2883(10) 0.038(6) Uani 1 1 d DU . . C8 C 0.3320(17) 0.2445(13) 0.1422(12) 0.047(6) Uiso 1 1 d DU . . H8A H 0.4017 0.2999 0.1051 0.056 Uiso 1 1 calc R . . H8C H 0.3902 0.1747 0.1299 0.056 Uiso 1 1 calc R . . C9 C 0.1522(13) 0.2394(9) 0.0852(16) 0.033(4) Uiso 1 1 d DU . . H9C H 0.1698 0.2088 0.0129 0.040 Uiso 1 1 calc R . . H9A H 0.1098 0.3139 0.0758 0.040 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 Pd 0.0245(7) 0.0242(5) 0.032(5) -0.0012(11) -0.0017(12) 0.0049(4) Cl1 0.066(3) 0.0310(18) 0.063(12) 0.015(4) 0.007(4) -0.0050(19) Cl2 0.046(3) 0.049(2) 0.081(19) -0.010(4) 0.001(4) 0.0245(18) S1 0.041(2) 0.042(2) 0.034(10) -0.005(4) -0.004(4) -0.0126(15) S4 0.031(2) 0.0275(16) 0.027(13) 0.004(3) -0.002(4) -0.0004(15) S7 0.018(2) 0.044(2) 0.051(18) -0.001(4) 0.001(3) -0.0010(16) 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 Pd S4 2.250(4) . ? Pd S7 2.261(6) . ? Pd Cl2 2.325(4) . ? Pd Cl1 2.331(7) . ? Pd S1 3.159(10) . ? Pd S4 3.525(8) 3_556 ? S1 C9 1.800(9) . ? S1 C2 1.807(9) . ? C2 C3 1.512(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 S4 1.804(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? S4 C5 1.813(8) . ? C5 C6 1.516(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 S7 1.823(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? S7 C8 1.824(10) . ? C8 C9 1.529(9) . ? C8 H8A 0.9700 . ? C8 H8C 0.9700 . ? C9 H9C 0.9700 . ? C9 H9A 0.9700 . ? 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 S4 Pd S7 89.89(18) . . ? S4 Pd Cl2 174.7(3) . . ? S7 Pd Cl2 88.4(2) . . ? S4 Pd Cl1 87.52(19) . . ? S7 Pd Cl1 174.5(4) . . ? Cl2 Pd Cl1 93.7(2) . . ? S4 Pd S1 81.4(2) . . ? S7 Pd S1 78.2(3) . . ? Cl2 Pd S1 103.2(3) . . ? Cl1 Pd S1 106.2(2) . . ? S4 Pd S4 89.84(13) . 3_556 ? S7 Pd S4 75.0(3) . 3_556 ? Cl2 Pd S4 84.9(2) . 3_556 ? Cl1 Pd S4 100.1(3) . 3_556 ? S1 Pd S4 151.76(12) . 3_556 ? C9 S1 C2 104.7(7) . . ? C9 S1 Pd 94.3(6) . . ? C2 S1 Pd 91.7(8) . . ? C3 C2 S1 115.7(14) . . ? C3 C2 H2A 108.4 . . ? S1 C2 H2A 108.4 . . ? C3 C2 H2B 108.4 . . ? S1 C2 H2B 108.4 . . ? H2A C2 H2B 107.4 . . ? C2 C3 S4 122.2(14) . . ? C2 C3 H3A 106.8 . . ? S4 C3 H3A 106.8 . . ? C2 C3 H3B 106.8 . . ? S4 C3 H3B 106.8 . . ? H3A C3 H3B 106.6 . . ? C3 S4 C5 104.1(8) . . ? C3 S4 Pd 107.5(6) . . ? C5 S4 Pd 103.6(5) . . ? C6 C5 S4 116.7(11) . . ? C6 C5 H5A 108.1 . . ? S4 C5 H5A 108.1 . . ? C6 C5 H5B 108.1 . . ? S4 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? C5 C6 S7 110.9(10) . . ? C5 C6 H6A 109.5 . . ? S7 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? S7 C6 H6B 109.5 . . ? H6A C6 H6B 108.0 . . ? C6 S7 C8 102.7(10) . . ? C6 S7 Pd 107.0(5) . . ? C8 S7 Pd 106.6(5) . . ? C9 C8 S7 120.1(12) . . ? C9 C8 H8A 107.3 . . ? S7 C8 H8A 107.3 . . ? C9 C8 H8C 107.3 . . ? S7 C8 H8C 107.3 . . ? H8A C8 H8C 106.9 . . ? C8 C9 S1 116.9(11) . . ? C8 C9 H9C 108.1 . . ? S1 C9 H9C 108.1 . . ? C8 C9 H9A 108.1 . . ? S1 C9 H9A 108.1 . . ? H9C C9 H9A 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C2 C3 S4 57.5(17) . . . . ? C2 C3 S4 C5 58.5(14) . . . . ? C3 S4 C5 C6 -78.5(13) . . . . ? S4 C5 C6 S7 -39.6(14) . . . . ? C5 C6 S7 C8 137.0(11) . . . . ? C6 S7 C8 C9 -52.2(13) . . . . ? S7 C8 C9 S1 -46.2(17) . . . . ? C8 C9 S1 C2 104.5(13) . . . . ? C9 S1 C2 C3 -122.8(13) . . . . ? _diffrn_measured_fraction_theta_max 0.397 _diffrn_reflns_theta_full 26.72 _diffrn_measured_fraction_theta_full 0.397 _refine_diff_density_max 0.315 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.085 #===END of CIF data_s3pdc2 _database_code_depnum_ccdc_archive 'CCDC 607263' # Crystal 1, pressure = 12.6 kilobars _refine_special_details ; The completeness of the data is severely restricted by the geometry of the diamond anvil cell. As a result only Pd, Cl and S atoms were refined anisotropically. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Cl2 Pd S3' _chemical_formula_sum 'C6 H12 Cl2 Pd S3' _chemical_formula_weight 357.64 _cell_measurement_pressure 1260000 _diffrn_ambient_pressure 1260000 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.3362(8) _cell_length_b 11.9411(11) _cell_length_c 11.864(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1039.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 814 _cell_measurement_theta_min 3.9 _cell_measurement_theta_max 25.7 _exptl_crystal_description tablet _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 2.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.8406 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 16.2 SMX' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2298 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_av_sigmaI/netI 0.054 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 26.79 _reflns_number_total 531 _reflns_number_gt 493 _reflns_threshold_expression I>2s(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2004)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON' _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^)+(0.055P)^2^+2.042P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(15) _refine_ls_number_reflns 531 _refine_ls_number_parameters 79 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.13 _refine_ls_restrained_S_all 1.11 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.18602(15) 0.13679(8) 0.3737(3) 0.0211(14) Uani 1 1 d U . . Cl1 Cl 0.0369(6) 0.0039(3) 0.4822(9) 0.039(4) Uani 1 1 d U . . Cl2 Cl 0.4226(6) 0.0159(3) 0.3231(9) 0.046(5) Uani 1 1 d U . . S1 S -0.0325(6) 0.1576(3) 0.1507(9) 0.030(3) Uani 1 1 d DU . . C2 C -0.177(2) 0.2655(11) 0.2087(19) 0.033(5) Uiso 1 1 d DU . . H2A H -0.1215 0.3378 0.1945 0.040 Uiso 1 1 calc R . . H2B H -0.2933 0.2641 0.1694 0.040 Uiso 1 1 calc R . . C3 C -0.2124(19) 0.2543(12) 0.3338(17) 0.026(5) Uiso 1 1 d DU . . H3A H -0.2749 0.1837 0.3454 0.032 Uiso 1 1 calc R . . H3B H -0.2970 0.3131 0.3548 0.032 Uiso 1 1 calc R . . S4 S -0.0239(5) 0.2594(3) 0.4327(8) 0.025(4) Uani 1 1 d DU . . C5 C 0.078(2) 0.3954(8) 0.402(2) 0.019(4) Uiso 1 1 d DU . . H5A H -0.0196 0.4498 0.3951 0.023 Uiso 1 1 calc R . . H5B H 0.1512 0.4173 0.4667 0.023 Uiso 1 1 calc R . . C6 C 0.1963(19) 0.4027(8) 0.298(2) 0.015(4) Uiso 1 1 d DU . . H6A H 0.2739 0.4683 0.3019 0.018 Uiso 1 1 calc R . . H6B H 0.1200 0.4095 0.2312 0.018 Uiso 1 1 calc R . . S7 S 0.3362(6) 0.2769(3) 0.2872(9) 0.022(5) Uani 1 1 d DU . . C8 C 0.3282(19) 0.2453(14) 0.1379(13) 0.027(5) Uiso 1 1 d DU . . H8A H 0.3979 0.3027 0.0992 0.032 Uiso 1 1 calc R . . H8C H 0.3919 0.1750 0.1266 0.032 Uiso 1 1 calc R . . C9 C 0.1451(15) 0.2361(12) 0.0790(18) 0.032(5) Uiso 1 1 d DU . . H9C H 0.1650 0.2019 0.0059 0.039 Uiso 1 1 calc R . . H9A H 0.1000 0.3113 0.0658 0.039 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 Pd 0.0136(7) 0.0134(6) 0.036(4) 0.0001(10) 0.0012(12) 0.0026(5) Cl1 0.045(3) 0.0209(19) 0.052(12) 0.010(3) 0.016(4) -0.003(2) Cl2 0.025(3) 0.028(2) 0.083(18) 0.002(4) 0.007(4) 0.0137(17) S1 0.028(3) 0.023(2) 0.038(9) -0.009(3) 0.009(4) -0.0085(16) S4 0.010(2) 0.0186(18) 0.048(11) 0.000(3) 0.000(3) 0.0000(16) S7 0.013(2) 0.020(2) 0.033(15) 0.004(3) 0.004(4) 0.0014(15) 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 Pd S4 2.238(5) . ? Pd S7 2.251(6) . ? Pd Cl1 2.318(7) . ? Pd Cl2 2.336(5) . ? Pd S1 3.104(10) . ? Pd S4 3.367(8) 3_556 ? S1 C2 1.805(9) . ? S1 C9 1.816(9) . ? C2 C3 1.512(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 S4 1.815(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? S4 C5 1.823(8) . ? C5 C6 1.518(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 S7 1.823(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? S7 C8 1.811(10) . ? C8 C9 1.518(10) . ? C8 H8A 0.9700 . ? C8 H8C 0.9700 . ? C9 H9C 0.9700 . ? C9 H9A 0.9700 . ? 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 S4 Pd S7 89.61(19) . . ? S4 Pd Cl1 87.1(2) . . ? S7 Pd Cl1 173.3(4) . . ? S4 Pd Cl2 175.1(3) . . ? S7 Pd Cl2 88.8(2) . . ? Cl1 Pd Cl2 94.0(2) . . ? S4 Pd S1 81.9(2) . . ? S7 Pd S1 78.7(3) . . ? Cl1 Pd S1 106.5(2) . . ? Cl2 Pd S1 102.4(3) . . ? S4 Pd S4 88.90(13) . 3_556 ? S7 Pd S4 74.2(3) . 3_556 ? Cl1 Pd S4 99.9(3) . 3_556 ? Cl2 Pd S4 86.2(2) . 3_556 ? S1 Pd S4 151.45(13) . 3_556 ? C2 S1 C9 103.4(8) . . ? C2 S1 Pd 92.1(8) . . ? C9 S1 Pd 94.0(6) . . ? C3 C2 S1 114.3(14) . . ? C3 C2 H2A 108.7 . . ? S1 C2 H2A 108.7 . . ? C3 C2 H2B 108.7 . . ? S1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C2 C3 S4 120.1(15) . . ? C2 C3 H3A 107.3 . . ? S4 C3 H3A 107.3 . . ? C2 C3 H3B 107.3 . . ? S4 C3 H3B 107.3 . . ? H3A C3 H3B 106.9 . . ? C3 S4 C5 102.4(9) . . ? C3 S4 Pd 107.5(7) . . ? C5 S4 Pd 103.8(6) . . ? C6 C5 S4 116.6(12) . . ? C6 C5 H5A 108.2 . . ? S4 C5 H5A 108.2 . . ? C6 C5 H5B 108.2 . . ? S4 C5 H5B 108.2 . . ? H5A C5 H5B 107.3 . . ? C5 C6 S7 109.3(11) . . ? C5 C6 H6A 109.8 . . ? S7 C6 H6A 109.8 . . ? C5 C6 H6B 109.8 . . ? S7 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? C8 S7 C6 102.7(11) . . ? C8 S7 Pd 106.0(5) . . ? C6 S7 Pd 107.8(6) . . ? C9 C8 S7 119.6(12) . . ? C9 C8 H8A 107.4 . . ? S7 C8 H8A 107.4 . . ? C9 C8 H8C 107.4 . . ? S7 C8 H8C 107.4 . . ? H8A C8 H8C 107.0 . . ? C8 C9 S1 117.2(12) . . ? C8 C9 H9C 108.0 . . ? S1 C9 H9C 108.0 . . ? C8 C9 H9A 108.0 . . ? S1 C9 H9A 108.0 . . ? H9C C9 H9A 107.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 S1 C2 C3 -126.8(13) . . . . ? S1 C2 C3 S4 60.8(16) . . . . ? C2 C3 S4 C5 57.8(14) . . . . ? C3 S4 C5 C6 -77.6(14) . . . . ? S4 C5 C6 S7 -41.0(16) . . . . ? C5 C6 S7 C8 139.2(11) . . . . ? C6 S7 C8 C9 -52.6(14) . . . . ? S7 C8 C9 S1 -44.4(19) . . . . ? C2 S1 C9 C8 102.5(15) . . . . ? _diffrn_measured_fraction_theta_max 0.420 _diffrn_reflns_theta_full 26.79 _diffrn_measured_fraction_theta_full 0.420 _refine_diff_density_max 0.43 _refine_diff_density_min -0.60 _refine_diff_density_rms 0.12 #===END of CIF data_s3pdc3 _database_code_depnum_ccdc_archive 'CCDC 607264' # Crystal 1, pressure = 23.5 kilobars _refine_special_details ; The completeness of the data is severely restricted by the geometry of the diamond anvil cell. As a result only Pd, Cl and S atoms were refined anisotropically. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Cl2 Pd S3' _chemical_formula_sum 'C6 H12 Cl2 Pd S3' _chemical_formula_weight 357.64 _cell_measurement_pressure 2350000 _diffrn_ambient_pressure 2350000 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.2357(9) _cell_length_b 11.8141(12) _cell_length_c 11.692(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 999.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 733 _cell_measurement_theta_min 3.9 _cell_measurement_theta_max 24.4 _exptl_crystal_description tablet _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 2.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.388 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.84060 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 16.2 SMX' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2181 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_av_sigmaI/netI 0.061 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 26.77 _reflns_number_total 543 _reflns_number_gt 507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2004)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON' _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^)+(0.034P)^2^+2.05P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(14) _refine_ls_number_reflns 543 _refine_ls_number_parameters 79 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.14 _refine_ls_restrained_S_all 1.13 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.18257(15) 0.13568(7) 0.3736(2) 0.0178(11) Uani 1 1 d U . . Cl1 Cl 0.0320(6) 0.0031(3) 0.4883(7) 0.032(2) Uani 1 1 d U . . Cl2 Cl 0.4218(5) 0.0142(3) 0.3219(8) 0.032(4) Uani 1 1 d U . . S1 S -0.0372(5) 0.1555(3) 0.1512(9) 0.021(2) Uani 1 1 d U . . C2 C -0.182(2) 0.2634(10) 0.209(3) 0.017(4) Uiso 1 1 d U . . H2A H -0.1246 0.3363 0.1951 0.021 Uiso 1 1 calc R . . H2B H -0.2990 0.2624 0.1687 0.021 Uiso 1 1 calc R . . C3 C -0.2204(19) 0.2522(11) 0.338(4) 0.023(4) Uiso 1 1 d U . . H3A H -0.2817 0.1803 0.3508 0.027 Uiso 1 1 calc R . . H3B H -0.3068 0.3113 0.3596 0.027 Uiso 1 1 calc R . . S4 S -0.0284(5) 0.2598(3) 0.4324(7) 0.014(3) Uani 1 1 d U . . C5 C 0.073(2) 0.3963(10) 0.399(3) 0.019(4) Uiso 1 1 d U . . H5A H -0.0277 0.4499 0.3889 0.023 Uiso 1 1 calc R . . H5B H 0.1431 0.4208 0.4648 0.023 Uiso 1 1 calc R . . C6 C 0.191(2) 0.4049(9) 0.300(3) 0.012(4) Uiso 1 1 d U . . H6A H 0.2702 0.4707 0.3080 0.014 Uiso 1 1 calc R . . H6B H 0.1160 0.4150 0.2322 0.014 Uiso 1 1 calc R . . S7 S 0.3331(6) 0.2784(3) 0.2842(8) 0.025(3) Uani 1 1 d U . . C8 C 0.3274(19) 0.2433(12) 0.139(3) 0.020(4) Uiso 1 1 d U . . H8A H 0.3982 0.3002 0.0979 0.024 Uiso 1 1 calc R . . H8C H 0.3925 0.1720 0.1295 0.024 Uiso 1 1 calc R . . C9 C 0.1393(17) 0.2316(11) 0.078(3) 0.025(5) Uiso 1 1 d U . . H9C H 0.1602 0.1948 0.0045 0.030 Uiso 1 1 calc R . . H9A H 0.0933 0.3071 0.0616 0.030 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 Pd 0.0095(7) 0.0109(5) 0.033(3) 0.0003(9) 0.0008(12) 0.0027(5) Cl1 0.038(3) 0.0181(17) 0.038(8) 0.006(3) 0.008(3) 0.0002(18) Cl2 0.023(2) 0.0194(17) 0.053(12) -0.002(3) 0.009(3) 0.0092(14) S1 0.018(2) 0.0245(19) 0.021(6) -0.003(3) 0.008(4) -0.0062(15) S4 0.012(2) 0.0142(16) 0.018(8) 0.002(3) -0.006(3) 0.0016(14) S7 0.008(2) 0.0148(17) 0.052(11) 0.001(3) 0.001(3) 0.0002(15) 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 Pd S4 2.226(4) . ? Pd S7 2.263(6) . ? Pd Cl2 2.329(4) . ? Pd Cl1 2.333(6) . ? Pd S1 3.058(9) . ? Pd S4 3.323(7) 3_556 ? S1 C2 1.783(18) . ? S1 C9 1.78(2) . ? C2 C3 1.54(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 S4 1.78(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? S4 C5 1.814(14) . ? C5 C6 1.44(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 S7 1.824(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? S7 C8 1.75(4) . ? C8 C9 1.54(3) . ? C8 H8A 0.9700 . ? C8 H8C 0.9700 . ? C9 H9C 0.9700 . ? C9 H9A 0.9700 . ? 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 S4 Pd S7 88.95(17) . . ? S4 Pd Cl2 175.0(2) . . ? S7 Pd Cl2 88.94(18) . . ? S4 Pd Cl1 86.83(18) . . ? S7 Pd Cl1 172.2(3) . . ? Cl2 Pd Cl1 94.73(18) . . ? S4 Pd S1 81.7(2) . . ? S7 Pd S1 78.5(2) . . ? Cl2 Pd S1 102.3(2) . . ? Cl1 Pd S1 107.31(19) . . ? S4 Pd S4 88.63(12) . 3_556 ? S7 Pd S4 74.7(2) . 3_556 ? Cl2 Pd S4 86.47(19) . 3_556 ? Cl1 Pd S4 98.7(2) . 3_556 ? S1 Pd S4 151.58(12) . 3_556 ? C2 S1 C9 104.1(9) . . ? C2 S1 Pd 92.1(10) . . ? C9 S1 Pd 94.4(10) . . ? C3 C2 S1 114.6(14) . . ? C3 C2 H2A 108.6 . . ? S1 C2 H2A 108.6 . . ? C3 C2 H2B 108.6 . . ? S1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C2 C3 S4 117.6(13) . . ? C2 C3 H3A 107.9 . . ? S4 C3 H3A 107.9 . . ? C2 C3 H3B 107.9 . . ? S4 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? C3 S4 C5 103.1(12) . . ? C3 S4 Pd 108.1(9) . . ? C5 S4 Pd 104.0(7) . . ? C6 C5 S4 118.4(16) . . ? C6 C5 H5A 107.7 . . ? S4 C5 H5A 107.7 . . ? C6 C5 H5B 107.7 . . ? S4 C5 H5B 107.7 . . ? H5A C5 H5B 107.1 . . ? C5 C6 S7 111.1(14) . . ? C5 C6 H6A 109.4 . . ? S7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? S7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 S7 C6 106.3(12) . . ? C8 S7 Pd 105.1(6) . . ? C6 S7 Pd 107.0(7) . . ? C9 C8 S7 119.4(19) . . ? C9 C8 H8A 107.5 . . ? S7 C8 H8A 107.5 . . ? C9 C8 H8C 107.5 . . ? S7 C8 H8C 107.5 . . ? H8A C8 H8C 107.0 . . ? C8 C9 S1 117(2) . . ? C8 C9 H9C 108.1 . . ? S1 C9 H9C 108.1 . . ? C8 C9 H9A 108.1 . . ? S1 C9 H9A 108.1 . . ? H9C C9 H9A 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 S1 C2 C3 -128.1(16) . . . . ? S1 C2 C3 S4 61.8(15) . . . . ? C2 C3 S4 C5 57.3(16) . . . . ? C3 S4 C5 C6 -81(2) . . . . ? S4 C5 C6 S7 -38(3) . . . . ? C5 C6 S7 C8 136.2(19) . . . . ? C6 S7 C8 C9 -52.0(14) . . . . ? S7 C8 C9 S1 -44.3(17) . . . . ? C2 S1 C9 C8 101.2(17) . . . . ? _diffrn_measured_fraction_theta_max 0.446 _diffrn_reflns_theta_full 26.77 _diffrn_measured_fraction_theta_full 0.446 _refine_diff_density_max 0.53 _refine_diff_density_min -0.58 _refine_diff_density_rms 0.13 #===END of CIF data_s3pdc4 _database_code_depnum_ccdc_archive 'CCDC 607265' # Crystal 1, pressure = 36 kilobars _refine_special_details ; The completeness of the data is severely restricted by the geometry of the diamond anvil cell. As a result only Pd, Cl and S atoms were refined anisotropically. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Cl2 Pd S3' _chemical_formula_sum 'C6 H12 Cl2 Pd S3' _chemical_formula_weight 357.64 _cell_measurement_pressure 3600000 _diffrn_ambient_pressure 3600000 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.152(2) _cell_length_b 11.695(2) _cell_length_c 11.553(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 966.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 525 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 24.7 _exptl_crystal_description tablet _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 3.058 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.127 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.8406 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 16.2 SMX' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1837 _diffrn_reflns_av_R_equivalents 0.067 _diffrn_reflns_av_sigmaI/netI 0.074 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.95 _diffrn_reflns_theta_max 26.71 _reflns_number_total 521 _reflns_number_gt 459 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2004)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON' _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^)+(0.025P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.0029(9) _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 0.00(13) _refine_ls_number_reflns 521 _refine_ls_number_parameters 80 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.005 _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 Pd Pd 0.17951(17) 0.13469(7) 0.3738(2) 0.0134(11) Uani 1 1 d U . . Cl1 Cl 0.0275(5) 0.0011(2) 0.4897(7) 0.021(3) Uani 1 1 d U . . Cl2 Cl 0.4217(5) 0.0129(3) 0.3204(7) 0.026(4) Uani 1 1 d U . . S1 S -0.0413(5) 0.1549(3) 0.1502(8) 0.019(3) Uani 1 1 d DU . . C2 C -0.191(2) 0.2662(8) 0.2084(17) 0.013(4) Uiso 1 1 d DU . . H2A H -0.1328 0.3400 0.1957 0.015 Uiso 1 1 calc R . . H2B H -0.3094 0.2656 0.1674 0.015 Uiso 1 1 calc R . . C3 C -0.2273(17) 0.2508(10) 0.3365(15) 0.020(4) Uiso 1 1 d DU . . H3A H -0.2856 0.1766 0.3469 0.024 Uiso 1 1 calc R . . H3B H -0.3185 0.3078 0.3594 0.024 Uiso 1 1 calc R . . S4 S -0.0340(5) 0.2595(3) 0.4369(7) 0.012(3) Uani 1 1 d DU . . C5 C 0.0667(19) 0.3977(8) 0.403(2) 0.014(4) Uiso 1 1 d DU . . H5A H -0.0351 0.4520 0.3951 0.017 Uiso 1 1 calc R . . H5B H 0.1410 0.4217 0.4689 0.017 Uiso 1 1 calc R . . C6 C 0.1881(19) 0.4071(8) 0.296(2) 0.014(4) Uiso 1 1 d DU . . H6A H 0.2672 0.4743 0.3009 0.017 Uiso 1 1 calc R . . H6B H 0.1103 0.4141 0.2274 0.017 Uiso 1 1 calc R . . S7 S 0.3318(6) 0.2786(3) 0.2858(8) 0.014(4) Uani 1 1 d DU . . C8 C 0.3318(19) 0.2464(11) 0.1327(11) 0.022(4) Uiso 1 1 d DU . . H8A H 0.3970 0.3076 0.0929 0.027 Uiso 1 1 calc R . . H8C H 0.4038 0.1770 0.1211 0.027 Uiso 1 1 calc R . . C9 C 0.1433(15) 0.2305(10) 0.0751(17) 0.024(5) Uiso 1 1 d DU . . H9C H 0.1647 0.1912 0.0024 0.028 Uiso 1 1 calc R . . H9A H 0.0960 0.3060 0.0562 0.028 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 Pd 0.0085(8) 0.0106(6) 0.021(3) -0.0002(9) 0.0006(12) 0.0022(5) Cl1 0.032(3) 0.017(2) 0.014(10) 0.004(3) 0.008(4) -0.0008(19) Cl2 0.021(2) 0.0156(18) 0.040(13) -0.001(3) 0.012(4) 0.0073(15) S1 0.015(3) 0.0180(18) 0.024(8) 0.000(3) -0.006(4) -0.0062(15) S4 0.009(2) 0.0139(18) 0.014(11) 0.005(3) 0.000(3) 0.0037(16) S7 0.008(3) 0.0178(19) 0.017(13) 0.006(3) 0.005(4) 0.0034(17) 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 Pd S4 2.235(4) . ? Pd S7 2.248(5) . ? Pd Cl1 2.327(6) . ? Pd Cl2 2.326(4) . ? Pd S1 3.038(8) . ? Pd S4 3.242(7) 3_556 ? S1 C9 1.811(9) . ? S1 C2 1.815(8) . ? C2 C3 1.513(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 S4 1.808(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? S4 C5 1.812(8) . ? C5 C6 1.517(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 S7 1.824(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? S7 C8 1.809(10) . ? C8 C9 1.515(10) . ? C8 H8A 0.9700 . ? C8 H8C 0.9700 . ? C9 H9C 0.9700 . ? C9 H9A 0.9700 . ? 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 S4 Pd S7 89.40(16) . . ? S4 Pd Cl1 86.07(16) . . ? S7 Pd Cl1 171.6(3) . . ? S4 Pd Cl2 174.5(2) . . ? S7 Pd Cl2 88.72(17) . . ? Cl1 Pd Cl2 95.13(17) . . ? S4 Pd S1 82.6(2) . . ? S7 Pd S1 79.0(2) . . ? Cl1 Pd S1 107.38(18) . . ? Cl2 Pd S1 102.1(2) . . ? S4 Pd S4 87.85(11) . 3_556 ? S7 Pd S4 73.3(2) . 3_556 ? Cl1 Pd S4 99.4(2) . 3_556 ? Cl2 Pd S4 86.67(18) . 3_556 ? S1 Pd S4 150.77(12) . 3_556 ? C9 S1 C2 104.9(6) . . ? C9 S1 Pd 93.8(6) . . ? C2 S1 Pd 92.7(7) . . ? C3 C2 S1 112.2(11) . . ? C3 C2 H2A 109.2 . . ? S1 C2 H2A 109.2 . . ? C3 C2 H2B 109.2 . . ? S1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C2 C3 S4 119.4(13) . . ? C2 C3 H3A 107.5 . . ? S4 C3 H3A 107.5 . . ? C2 C3 H3B 107.5 . . ? S4 C3 H3B 107.5 . . ? H3A C3 H3B 107.0 . . ? C3 S4 C5 102.4(8) . . ? C3 S4 Pd 106.0(5) . . ? C5 S4 Pd 103.9(5) . . ? C6 C5 S4 118.0(11) . . ? C6 C5 H5A 107.8 . . ? S4 C5 H5A 107.8 . . ? C6 C5 H5B 107.8 . . ? S4 C5 H5B 107.8 . . ? H5A C5 H5B 107.2 . . ? C5 C6 S7 108.3(10) . . ? C5 C6 H6A 110.0 . . ? S7 C6 H6A 110.0 . . ? C5 C6 H6B 110.0 . . ? S7 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C8 S7 C6 103.5(9) . . ? C8 S7 Pd 106.6(5) . . ? C6 S7 Pd 108.4(5) . . ? C9 C8 S7 117.1(12) . . ? C9 C8 H8A 108.0 . . ? S7 C8 H8A 108.0 . . ? C9 C8 H8C 108.0 . . ? S7 C8 H8C 108.0 . . ? H8A C8 H8C 107.3 . . ? C8 C9 S1 119.9(12) . . ? C8 C9 H9C 107.3 . . ? S1 C9 H9C 107.3 . . ? C8 C9 H9A 107.3 . . ? S1 C9 H9A 107.3 . . ? H9C C9 H9A 106.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 S1 C2 C3 -128.2(11) . . . . ? S1 C2 C3 S4 63.6(12) . . . . ? C2 C3 S4 C5 54.7(12) . . . . ? C3 S4 C5 C6 -77.7(14) . . . . ? S4 C5 C6 S7 -39.8(16) . . . . ? C5 C6 S7 C8 140.3(11) . . . . ? C6 S7 C8 C9 -56.4(12) . . . . ? S7 C8 C9 S1 -39.8(16) . . . . ? C2 S1 C9 C8 100.0(13) . . . . ? _diffrn_measured_fraction_theta_max 0.439 _diffrn_reflns_theta_full 26.71 _diffrn_measured_fraction_theta_full 0.439 _refine_diff_density_max 0.53 _refine_diff_density_min -0.46 _refine_diff_density_rms 0.13 #===END of CIF data_s3pdcd _database_code_depnum_ccdc_archive 'CCDC 607266' # Crystal 2, pressure = 42.5 kilobars _refine_special_details ; The completeness of the data is severely restricted by the geometry of the diamond anvil cell. As a result only Cl and S atoms could be refined anisotropically. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Cl2 Pd S3' _chemical_formula_sum 'C6 H12 Cl2 Pd S3' _chemical_formula_weight 357.64 _cell_measurement_pressure 4250000 _diffrn_ambient_pressure 4250000 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.0777(12) _cell_length_b 11.601(8) _cell_length_c 11.4241(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 938.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1215 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.9 _exptl_crystal_description tablet _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 3.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.431 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.8406 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 16.2 SMX' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1999 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_av_sigmaI/netI 0.033 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 26.79 _reflns_number_total 471 _reflns_number_gt 458 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2004)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON' _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^)+(0.040P)^2^] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(11) _refine_ls_number_reflns 471 _refine_ls_number_parameters 74 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.25 _refine_ls_restrained_S_all 1.23 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.1766(3) 0.13402(6) 0.37369(7) 0.0101(3) Uiso 1 1 d U . . Cl1 Cl 0.0227(9) -0.00035(19) 0.4906(2) 0.023(3) Uani 1 1 d U . . Cl2 Cl 0.4219(11) 0.0116(2) 0.3180(3) 0.021(2) Uani 1 1 d U . . S1 S -0.0471(10) 0.1536(2) 0.1506(3) 0.016(3) Uani 1 1 d DU . . C2 C -0.199(3) 0.2666(7) 0.2087(8) 0.021(3) Uiso 1 1 d DU . . H2A H -0.1389 0.3422 0.1938 0.025 Uiso 1 1 calc R . . H2B H -0.3206 0.2652 0.1658 0.025 Uiso 1 1 calc R . . C3 C -0.239(2) 0.2558(8) 0.3384(7) 0.023(3) Uiso 1 1 d DU . . H3A H -0.3069 0.1823 0.3513 0.028 Uiso 1 1 calc R . . H3B H -0.3258 0.3188 0.3608 0.028 Uiso 1 1 calc R . . S4 S -0.0382(11) 0.2594(2) 0.4372(3) 0.012(2) Uani 1 1 d DU . . C5 C 0.059(3) 0.4012(7) 0.4058(8) 0.014(3) Uiso 1 1 d DU . . H5A H -0.0476 0.4557 0.3950 0.016 Uiso 1 1 calc R . . H5B H 0.1316 0.4273 0.4748 0.016 Uiso 1 1 calc R . . C6 C 0.186(2) 0.4079(6) 0.2988(9) 0.011(3) Uiso 1 1 d DU . . H6A H 0.2678 0.4766 0.3048 0.014 Uiso 1 1 calc R . . H6B H 0.1069 0.4162 0.2276 0.014 Uiso 1 1 calc R . . S7 S 0.3316(12) 0.27921(19) 0.2859(2) 0.013(2) Uani 1 1 d DU . . C8 C 0.332(3) 0.2469(8) 0.1318(7) 0.017(3) Uiso 1 1 d DU . . H8A H 0.3952 0.3112 0.0906 0.020 Uiso 1 1 calc R . . H8C H 0.4096 0.1771 0.1196 0.020 Uiso 1 1 calc R . . C9 C 0.142(2) 0.2271(8) 0.0741(10) 0.017(3) Uiso 1 1 d DU . . H9C H 0.1654 0.1837 0.0009 0.021 Uiso 1 1 calc R . . H9A H 0.0925 0.3037 0.0507 0.021 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 Cl1 0.033(9) 0.0163(13) 0.0196(18) 0.0034(11) 0.011(3) 0.001(2) Cl2 0.017(7) 0.0183(13) 0.0278(19) -0.0034(11) 0.003(3) 0.002(2) S1 0.015(8) 0.0185(14) 0.0137(16) -0.0024(10) -0.001(3) -0.005(2) S4 0.010(8) 0.0152(13) 0.0122(16) 0.0007(10) 0.000(3) -0.001(2) S7 0.012(7) 0.0189(13) 0.0074(17) -0.0008(10) 0.001(3) -0.004(3) 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 Pd S4 2.226(6) . ? Pd S7 2.246(5) . ? Pd Cl1 2.324(4) . ? Pd Cl2 2.332(6) . ? Pd S1 3.009(5) . ? Pd S4 3.204(5) 3_556 ? S1 C9 1.810(9) . ? S1 C2 1.821(9) . ? C2 C3 1.514(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 S4 1.815(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? S4 C5 1.818(8) . ? C5 C6 1.520(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 S7 1.821(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? S7 C8 1.800(8) . ? C8 C9 1.516(10) . ? C8 H8A 0.9900 . ? C8 H8C 0.9900 . ? C9 H9C 0.9900 . ? C9 H9A 0.9900 . ? 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 S4 Pd S7 89.38(19) . . ? S4 Pd Cl1 86.02(16) . . ? S7 Pd Cl1 171.28(10) . . ? S4 Pd Cl2 174.7(2) . . ? S7 Pd Cl2 88.4(2) . . ? Cl1 Pd Cl2 95.58(16) . . ? S4 Pd S1 82.38(16) . . ? S7 Pd S1 79.76(18) . . ? Cl1 Pd S1 106.92(17) . . ? Cl2 Pd S1 101.91(15) . . ? S4 Pd S4 87.61(6) . 3_556 ? S7 Pd S4 72.78(16) . 3_556 ? Cl1 Pd S4 99.59(12) . 3_556 ? Cl2 Pd S4 87.15(17) . 3_556 ? S1 Pd S4 150.83(9) . 3_556 ? C9 S1 C2 105.8(6) . . ? C9 S1 Pd 93.2(5) . . ? C2 S1 Pd 93.2(5) . . ? C3 C2 S1 114.0(8) . . ? C3 C2 H2A 108.7 . . ? S1 C2 H2A 108.7 . . ? C3 C2 H2B 108.7 . . ? S1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C2 C3 S4 117.5(11) . . ? C2 C3 H3A 107.9 . . ? S4 C3 H3A 107.9 . . ? C2 C3 H3B 107.9 . . ? S4 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? C3 S4 C5 101.1(6) . . ? C3 S4 Pd 108.4(4) . . ? C5 S4 Pd 105.6(6) . . ? C6 C5 S4 115.4(7) . . ? C6 C5 H5A 108.4 . . ? S4 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? S4 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C5 C6 S7 111.0(7) . . ? C5 C6 H6A 109.4 . . ? S7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? S7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 S7 C6 104.5(5) . . ? C8 S7 Pd 106.3(5) . . ? C6 S7 Pd 107.5(5) . . ? C9 C8 S7 117.2(11) . . ? C9 C8 H8A 108.0 . . ? S7 C8 H8A 108.0 . . ? C9 C8 H8C 108.0 . . ? S7 C8 H8C 108.0 . . ? H8A C8 H8C 107.2 . . ? C8 C9 S1 121.1(9) . . ? C8 C9 H9C 107.1 . . ? S1 C9 H9C 107.1 . . ? C8 C9 H9A 107.1 . . ? S1 C9 H9A 107.1 . . ? H9C C9 H9A 106.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 S1 C2 C3 -127.8(11) . . . . ? S1 C2 C3 S4 59.9(12) . . . . ? C2 C3 S4 C5 60.5(9) . . . . ? C3 S4 C5 C6 -82.3(12) . . . . ? S4 C5 C6 S7 -37.9(14) . . . . ? C5 C6 S7 C8 139.5(11) . . . . ? C6 S7 C8 C9 -57.8(9) . . . . ? S7 C8 C9 S1 -36.8(11) . . . . ? C2 S1 C9 C8 98.1(10) . . . . ? _diffrn_measured_fraction_theta_max 0.411 _diffrn_reflns_theta_full 26.79 _diffrn_measured_fraction_theta_full 0.411 _refine_diff_density_max 0.41 _refine_diff_density_min -0.49 _refine_diff_density_rms 0.10 #===END of CIF data_s3pdcc _database_code_depnum_ccdc_archive 'CCDC 607267' # Crystal 2, pressure = 46 kilobars _refine_special_details ; The completeness of the data is severely restricted by the geometry of the diamond anvil cell. As a result only Pd, Cl1 and Cl2 were refined anisotropically. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Cl2 Pd S3' _chemical_formula_sum 'C6 H12 Cl2 Pd S3' _chemical_formula_weight 357.64 _cell_measurement_pressure 4600000 _diffrn_ambient_pressure 4600000 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.0624(12) _cell_length_b 11.5835(9) _cell_length_c 11.2892(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 923.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1049 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 26.6 _exptl_crystal_description tablet _exptl_crystal_colour 'intensely dark' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 3.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.264 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.8406 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 16.2 SMX' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1969 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.032 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 26.47 _reflns_number_total 451 _reflns_number_gt 441 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2004)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON' _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^)+(0.056P)^2^+9.19P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(18) _refine_ls_number_reflns 449 _refine_ls_number_parameters 64 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.14 _refine_ls_restrained_S_all 1.14 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.2020(4) 0.16928(9) 0.35314(11) 0.0126(14) Uani 1 1 d U . . Cl1 Cl 0.1051(17) 0.0128(3) 0.4680(4) 0.043(4) Uani 1 1 d U . . Cl2 Cl 0.4396(19) 0.0673(4) 0.2623(5) 0.040(3) Uani 1 1 d U . . S1 S -0.0254(14) 0.1860(3) 0.1457(4) 0.0201(12) Uiso 1 1 d DU . . C2 C -0.185(4) 0.2909(14) 0.2107(15) 0.043(6) Uiso 1 1 d DU . . H2A H -0.1305 0.3673 0.2031 0.052 Uiso 1 1 calc R . . H2B H -0.3037 0.2903 0.1670 0.052 Uiso 1 1 calc R . . C3 C -0.226(3) 0.267(2) 0.3406(14) 0.067(8) Uiso 1 1 d DU . . H3A H -0.2822 0.1909 0.3471 0.080 Uiso 1 1 calc R . . H3B H -0.3195 0.3224 0.3679 0.080 Uiso 1 1 calc R . . S4 S -0.0229(15) 0.2737(3) 0.4390(4) 0.0155(12) Uiso 1 1 d DU . . C5 C 0.032(5) 0.4251(10) 0.426(2) 0.054(7) Uiso 1 1 d DU . . H5A H -0.0647 0.4623 0.3782 0.065 Uiso 1 1 calc R . . H5B H 0.0302 0.4600 0.5038 0.065 Uiso 1 1 calc R . . C6 C 0.223(4) 0.4455(15) 0.3698(17) 0.052(7) Uiso 1 1 d DU . . H6A H 0.3088 0.4677 0.4326 0.062 Uiso 1 1 calc R . . H6B H 0.2099 0.5117 0.3178 0.062 Uiso 1 1 calc R . . S7 S 0.3366(15) 0.3326(3) 0.2858(4) 0.0214(12) Uiso 1 1 d DU . . C8 C 0.260(5) 0.3635(15) 0.1362(13) 0.060(7) Uiso 1 1 d DU . . H8A H 0.1769 0.4303 0.1389 0.072 Uiso 1 1 calc R . . H8B H 0.3702 0.3850 0.0902 0.072 Uiso 1 1 calc R . . C9 C 0.157(3) 0.2682(15) 0.0706(16) 0.039(6) Uiso 1 1 d DU . . H9A H 0.2524 0.2138 0.0434 0.047 Uiso 1 1 calc R . . H9B H 0.1007 0.3022 0.0006 0.047 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 Pd 0.010(4) 0.0106(6) 0.0174(9) 0.0011(5) -0.0050(12) 0.0011(9) Cl1 0.076(14) 0.024(2) 0.030(3) 0.0088(17) -0.022(4) -0.033(4) Cl2 0.028(11) 0.032(3) 0.059(4) -0.020(2) -0.008(5) 0.024(4) 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 Pd S4 2.220(8) . ? Pd S7 2.250(6) . ? Pd Cl2 2.294(10) . ? Pd Cl1 2.331(5) . ? Pd S1 2.846(7) . ? Pd S4 3.117(8) 3_556 ? S1 C9 1.815(10) . ? S1 C2 1.815(10) . ? C2 C3 1.520(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 S4 1.816(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? S4 C5 1.802(9) . ? C5 C6 1.505(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 S7 1.805(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? S7 C8 1.810(10) . ? C8 C9 1.513(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? 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 S4 Pd S7 89.5(3) . . ? S4 Pd Cl2 178.0(3) . . ? S7 Pd Cl2 88.5(3) . . ? S4 Pd Cl1 88.3(3) . . ? S7 Pd Cl1 165.0(2) . . ? Cl2 Pd Cl1 93.6(3) . . ? S4 Pd S1 85.3(2) . . ? S7 Pd S1 84.5(2) . . ? Cl2 Pd S1 94.6(3) . . ? Cl1 Pd S1 110.2(3) . . ? S4 Pd S4 90.10(8) . 3_556 ? S7 Pd S4 79.2(2) . 3_556 ? Cl2 Pd S4 89.4(3) . 3_556 ? Cl1 Pd S4 85.9(2) . 3_556 ? S1 Pd S4 163.07(12) . 3_556 ? C9 S1 C2 106.3(9) . . ? C9 S1 Pd 91.1(8) . . ? C2 S1 Pd 93.7(8) . . ? C3 C2 S1 112.7(13) . . ? C3 C2 H2A 109.0 . . ? S1 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? S1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C2 C3 S4 115.7(16) . . ? C2 C3 H3A 108.4 . . ? S4 C3 H3A 108.4 . . ? C2 C3 H3B 108.4 . . ? S4 C3 H3B 108.4 . . ? H3A C3 H3B 107.4 . . ? C5 S4 C3 99.2(13) . . ? C5 S4 Pd 109.8(10) . . ? C3 S4 Pd 106.0(7) . . ? C6 C5 S4 112.4(19) . . ? C6 C5 H5A 109.1 . . ? S4 C5 H5A 109.1 . . ? C6 C5 H5B 109.1 . . ? S4 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C5 C6 S7 120.4(19) . . ? C5 C6 H6A 107.2 . . ? S7 C6 H6A 107.2 . . ? C5 C6 H6B 107.2 . . ? S7 C6 H6B 107.2 . . ? H6A C6 H6B 106.9 . . ? C6 S7 C8 102.3(12) . . ? C6 S7 Pd 104.1(9) . . ? C8 S7 Pd 110.8(7) . . ? C9 C8 S7 117.1(13) . . ? C9 C8 H8A 108.0 . . ? S7 C8 H8A 108.0 . . ? C9 C8 H8B 108.0 . . ? S7 C8 H8B 108.0 . . ? H8A C8 H8B 107.3 . . ? C8 C9 S1 119.6(17) . . ? C8 C9 H9A 107.4 . . ? S1 C9 H9A 107.4 . . ? C8 C9 H9B 107.4 . . ? S1 C9 H9B 107.4 . . ? H9A C9 H9B 106.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C2 C3 S4 63(2) . . . . ? C2 C3 S4 C5 65.6(18) . . . . ? C3 S4 C5 C6 -115.7(19) . . . . ? S4 C5 C6 S7 18(3) . . . . ? C5 C6 S7 C8 93(2) . . . . ? C6 S7 C8 C9 -123(2) . . . . ? S7 C8 C9 S1 45(3) . . . . ? C8 C9 S1 C2 51(2) . . . . ? C9 S1 C2 C3 -130.3(17) . . . . ? _diffrn_measured_fraction_theta_max 0.411 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 0.411 _refine_diff_density_max 0.55 _refine_diff_density_min -0.46 _refine_diff_density_rms 0.12 #===END of CIF data_s3pdc9 _database_code_depnum_ccdc_archive 'CCDC 607268' # Crystal 1, pressure = 53.5 kilobars _refine_special_details ; The completeness of the data is severely restricted by the geometry of the diamond anvil cell. As a result all atoms were refined isotropically. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Cl2 Pd S3' _chemical_formula_sum 'C6 H12 Cl2 Pd S3' _chemical_formula_weight 357.64 _cell_measurement_pressure 5350000 _diffrn_ambient_pressure 5350000 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.0324(8) _cell_length_b 11.5032(11) _cell_length_c 11.223(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 907.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 880 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 26.2 _exptl_crystal_description tablet _exptl_crystal_colour 'intensely dark' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 3.255 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.318 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.8406 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 16.2 SMX' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1979 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_sigmaI/netI 0.046 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 4.02 _diffrn_reflns_theta_max 26.71 _reflns_number_total 467 _reflns_number_gt 448 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2004)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON' _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^)+(0.088P)^2^+40.30P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_number_reflns 466 _refine_ls_number_parameters 49 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1685 _refine_ls_wR_factor_gt 0.1664 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_restrained_S_all 1.08 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.1995(3) 0.16879(16) 0.3533(4) 0.0100(8) Uiso 1 1 d . . . Cl1 Cl 0.1084(14) 0.0112(8) 0.469(2) 0.047(3) Uiso 1 1 d . . . Cl2 Cl 0.4419(11) 0.0661(6) 0.2598(17) 0.030(2) Uiso 1 1 d . . . S1 S -0.0221(10) 0.1864(5) 0.1452(18) 0.019(2) Uiso 1 1 d D . . C2 C -0.189(5) 0.293(3) 0.203(5) 0.046(11) Uiso 1 1 d D . . H2A H -0.1372 0.3706 0.1930 0.055 Uiso 1 1 calc R . . H2B H -0.3075 0.2886 0.1587 0.055 Uiso 1 1 calc R . . C3 C -0.225(5) 0.269(3) 0.333(4) 0.045(11) Uiso 1 1 d D . . H3A H -0.2818 0.1920 0.3389 0.053 Uiso 1 1 calc R . . H3B H -0.3193 0.3238 0.3607 0.053 Uiso 1 1 calc R . . S4 S -0.0287(11) 0.2728(6) 0.4390(16) 0.020(2) Uiso 1 1 d D . . C5 C 0.038(4) 0.4231(17) 0.431(5) 0.037(11) Uiso 1 1 d D . . H5A H -0.0642 0.4659 0.3930 0.044 Uiso 1 1 calc R . . H5B H 0.0518 0.4528 0.5112 0.044 Uiso 1 1 calc R . . C6 C 0.218(4) 0.4467(18) 0.364(4) 0.014(7) Uiso 1 1 d D . . H6A H 0.3087 0.4778 0.4211 0.016 Uiso 1 1 calc R . . H6B H 0.1911 0.5082 0.3077 0.016 Uiso 1 1 calc R . . S7 S 0.3363(9) 0.3324(5) 0.2840(14) 0.0095(18) Uiso 1 1 d D . . C8 C 0.246(5) 0.370(2) 0.138(3) 0.042(11) Uiso 1 1 d D . . H8A H 0.1522 0.4310 0.1475 0.051 Uiso 1 1 calc R . . H8B H 0.3498 0.4014 0.0914 0.051 Uiso 1 1 calc R . . C9 C 0.156(4) 0.273(2) 0.068(3) 0.036(10) Uiso 1 1 d D . . H9A H 0.2566 0.2207 0.0418 0.044 Uiso 1 1 calc R . . H9B H 0.0981 0.3055 -0.0026 0.044 Uiso 1 1 calc R . . 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 Pd S4 2.221(11) . ? Pd S7 2.252(8) . ? Pd Cl1 2.319(15) . ? Pd Cl2 2.324(12) . ? Pd S1 2.815(18) . ? Pd S4 3.088(16) 3_556 ? S1 C2 1.815(18) . ? S1 C9 1.817(19) . ? C2 C3 1.52(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 S4 1.818(19) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? S4 C5 1.794(17) . ? C5 C6 1.49(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 S7 1.798(18) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? S7 C8 1.81(2) . ? C8 C9 1.50(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? 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 S4 Pd S7 90.5(3) . . ? S4 Pd Cl1 88.8(5) . . ? S7 Pd Cl1 164.7(6) . . ? S4 Pd Cl2 177.9(4) . . ? S7 Pd Cl2 87.5(3) . . ? Cl1 Pd Cl2 93.3(4) . . ? S4 Pd S1 85.4(5) . . ? S7 Pd S1 83.7(4) . . ? Cl1 Pd S1 111.5(5) . . ? Cl2 Pd S1 93.9(5) . . ? S4 Pd S4 90.2(2) . 3_556 ? S7 Pd S4 79.3(4) . 3_556 ? Cl1 Pd S4 85.4(5) . 3_556 ? Cl2 Pd S4 89.9(5) . 3_556 ? S1 Pd S4 162.4(2) . 3_556 ? C2 S1 C9 104.3(15) . . ? C2 S1 Pd 96.4(19) . . ? C9 S1 Pd 93.0(14) . . ? C3 C2 S1 109(3) . . ? C3 C2 H2A 109.9 . . ? S1 C2 H2A 109.9 . . ? C3 C2 H2B 109.9 . . ? S1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C2 C3 S4 120(4) . . ? C2 C3 H3A 107.3 . . ? S4 C3 H3A 107.3 . . ? C2 C3 H3B 107.3 . . ? S4 C3 H3B 107.3 . . ? H3A C3 H3B 106.9 . . ? C5 S4 C3 101(2) . . ? C5 S4 Pd 107.9(11) . . ? C3 S4 Pd 104.5(15) . . ? C6 C5 S4 115(2) . . ? C6 C5 H5A 108.5 . . ? S4 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? S4 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C6 S7 120.6(18) . . ? C5 C6 H6A 107.2 . . ? S7 C6 H6A 107.2 . . ? C5 C6 H6B 107.2 . . ? S7 C6 H6B 107.2 . . ? H6A C6 H6B 106.8 . . ? C6 S7 C8 96.7(18) . . ? C6 S7 Pd 103.9(10) . . ? C8 S7 Pd 111.2(10) . . ? C9 C8 S7 116(2) . . ? C9 C8 H8A 108.2 . . ? S7 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? S7 C8 H8B 108.2 . . ? H8A C8 H8B 107.4 . . ? C8 C9 S1 116(2) . . ? C8 C9 H9A 108.2 . . ? S1 C9 H9A 108.2 . . ? C8 C9 H9B 108.2 . . ? S1 C9 H9B 108.2 . . ? H9A C9 H9B 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C2 C3 S4 60(3) . . . . ? C2 C3 S4 C5 64(3) . . . . ? C3 S4 C5 C6 -106(4) . . . . ? S4 C5 C6 S7 8(5) . . . . ? C5 C6 S7 C8 99(3) . . . . ? C6 S7 C8 C9 -129(3) . . . . ? S7 C8 C9 S1 50(4) . . . . ? C8 C9 S1 C2 53(3) . . . . ? C9 S1 C2 C3 -131(3) . . . . ? _diffrn_measured_fraction_theta_max 0.419 _diffrn_reflns_theta_full 26.71 _diffrn_measured_fraction_theta_full 0.419 _refine_diff_density_max 1.31 _refine_diff_density_min -1.13 _refine_diff_density_rms 0.21 #===END of CIF data_s3pdc7 _database_code_depnum_ccdc_archive 'CCDC 607269' # Crystal 1, pressure = 73.1 kilobars _refine_special_details ; The completeness of the data is severely restricted by the geometry of the diamond anvil cell. As a result only Pd, Cl1, Cl2, S1 and S4 were refined anisotropically. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Cl2 Pd S3' _chemical_formula_sum 'C6 H12 Cl2 Pd S3' _chemical_formula_weight 357.64 _cell_measurement_pressure 7310000 _diffrn_ambient_pressure 7310000 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.9416(9) _cell_length_b 11.3535(13) _cell_length_c 11.116(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 876.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 645 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 26.5 _exptl_crystal_description tablet _exptl_crystal_colour 'intensely dark' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 3.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.462 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.8406 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 16.2 SMX' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1909 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_sigmaI/netI 0.048 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 26.78 _reflns_number_total 477 _reflns_number_gt 456 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2004)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON' _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^)+(0.064P)^2^+11.292P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(19) _refine_ls_number_reflns 477 _refine_ls_number_parameters 74 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.08 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.1978(2) 0.16781(11) 0.3532(3) 0.0236(15) Uani 1 1 d U . . Cl1 Cl 0.1052(11) 0.0089(4) 0.4701(13) 0.049(3) Uani 1 1 d U . . Cl2 Cl 0.4393(8) 0.0656(4) 0.2587(12) 0.039(4) Uani 1 1 d U . . S1 S -0.0219(7) 0.1871(4) 0.1450(12) 0.021(3) Uani 1 1 d DU . . C2 C -0.188(3) 0.2965(17) 0.205(3) 0.046(8) Uiso 1 1 d DU . . H2A H -0.1319 0.3745 0.1983 0.056 Uiso 1 1 calc R . . H2B H -0.3072 0.2953 0.1595 0.056 Uiso 1 1 calc R . . C3 C -0.228(4) 0.268(2) 0.336(3) 0.065(9) Uiso 1 1 d DU . . H3A H -0.2817 0.1891 0.3390 0.078 Uiso 1 1 calc R . . H3B H -0.3268 0.3215 0.3638 0.078 Uiso 1 1 calc R . . S4 S -0.0306(8) 0.2738(4) 0.4426(11) 0.018(3) Uani 1 1 d DU . . C5 C 0.034(3) 0.4275(10) 0.438(3) 0.043(8) Uiso 1 1 d DU . . H5A H -0.0709 0.4722 0.4037 0.052 Uiso 1 1 calc R . . H5B H 0.0542 0.4555 0.5200 0.052 Uiso 1 1 calc R . . C6 C 0.213(3) 0.4485(13) 0.367(3) 0.023(5) Uiso 1 1 d DU . . H6A H 0.3069 0.4824 0.4214 0.027 Uiso 1 1 calc R . . H6B H 0.1822 0.5094 0.3085 0.027 Uiso 1 1 calc R . . S7 S 0.3361(7) 0.3343(4) 0.2851(10) 0.0114(13) Uiso 1 1 d DU . . C8 C 0.256(4) 0.3656(18) 0.1327(15) 0.052(9) Uiso 1 1 d DU . . H8A H 0.1676 0.4316 0.1367 0.063 Uiso 1 1 calc R . . H8B H 0.3674 0.3915 0.0871 0.063 Uiso 1 1 calc R . . C9 C 0.159(3) 0.2690(15) 0.061(2) 0.030(6) Uiso 1 1 d DU . . H9A H 0.2565 0.2144 0.0334 0.036 Uiso 1 1 calc R . . H9B H 0.0984 0.3036 -0.0088 0.036 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 Pd 0.0156(10) 0.0059(7) 0.049(5) 0.0034(11) -0.0051(14) 0.0003(6) Cl1 0.103(6) 0.018(2) 0.025(10) 0.000(4) -0.023(6) -0.032(3) Cl2 0.037(4) 0.028(3) 0.050(15) -0.024(4) -0.020(4) 0.022(2) S1 0.022(3) 0.019(2) 0.024(8) 0.003(4) 0.007(5) -0.0029(19) S4 0.015(3) 0.018(2) 0.022(10) 0.004(4) 0.004(4) -0.0092(19) 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 Pd S4 2.225(8) . ? Pd S7 2.251(6) . ? Pd Cl2 2.293(8) . ? Pd Cl1 2.315(9) . ? Pd S1 2.780(12) . ? Pd S4 3.024(10) 3_556 ? S1 C9 1.817(10) . ? S1 C2 1.820(10) . ? C2 C3 1.517(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 S4 1.812(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? S4 C5 1.803(10) . ? C5 C6 1.496(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 S7 1.797(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? S7 C8 1.818(11) . ? C8 C9 1.512(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? 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 S4 Pd S7 90.0(2) . . ? S4 Pd Cl2 177.7(2) . . ? S7 Pd Cl2 87.7(3) . . ? S4 Pd Cl1 88.4(3) . . ? S7 Pd Cl1 164.1(4) . . ? Cl2 Pd Cl1 93.8(3) . . ? S4 Pd S1 86.5(3) . . ? S7 Pd S1 83.6(3) . . ? Cl2 Pd S1 93.4(4) . . ? Cl1 Pd S1 112.1(3) . . ? S4 Pd S4 89.44(17) . 3_556 ? S7 Pd S4 78.6(3) . 3_556 ? Cl2 Pd S4 90.0(3) . 3_556 ? Cl1 Pd S4 85.6(3) . 3_556 ? S1 Pd S4 161.70(16) . 3_556 ? C9 S1 C2 106.0(10) . . ? C9 S1 Pd 95.0(8) . . ? C2 S1 Pd 95.6(13) . . ? C3 C2 S1 109(2) . . ? C3 C2 H2A 110.0 . . ? S1 C2 H2A 110.0 . . ? C3 C2 H2B 110.0 . . ? S1 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? C2 C3 S4 119(2) . . ? C2 C3 H3A 107.6 . . ? S4 C3 H3A 107.6 . . ? C2 C3 H3B 107.6 . . ? S4 C3 H3B 107.6 . . ? H3A C3 H3B 107.0 . . ? C5 S4 C3 102.0(16) . . ? C5 S4 Pd 109.5(7) . . ? C3 S4 Pd 103.0(11) . . ? C6 C5 S4 112.1(14) . . ? C6 C5 H5A 109.2 . . ? S4 C5 H5A 109.2 . . ? C6 C5 H5B 109.2 . . ? S4 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C5 C6 S7 123.2(13) . . ? C5 C6 H6A 106.5 . . ? S7 C6 H6A 106.5 . . ? C5 C6 H6B 106.5 . . ? S7 C6 H6B 106.5 . . ? H6A C6 H6B 106.5 . . ? C6 S7 C8 100.6(12) . . ? C6 S7 Pd 103.5(7) . . ? C8 S7 Pd 110.3(8) . . ? C9 C8 S7 118.9(16) . . ? C9 C8 H8A 107.6 . . ? S7 C8 H8A 107.6 . . ? C9 C8 H8B 107.6 . . ? S7 C8 H8B 107.6 . . ? H8A C8 H8B 107.0 . . ? C8 C9 S1 114.3(16) . . ? C8 C9 H9A 108.7 . . ? S1 C9 H9A 108.7 . . ? C8 C9 H9B 108.7 . . ? S1 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C2 C3 S4 64(2) . . . . ? C2 C3 S4 C5 64(2) . . . . ? C3 S4 C5 C6 -103(2) . . . . ? S4 C5 C6 S7 4(3) . . . . ? C5 C6 S7 C8 102(2) . . . . ? C6 S7 C8 C9 -124.5(19) . . . . ? S7 C8 C9 S1 45(3) . . . . ? C8 C9 S1 C2 54(2) . . . . ? C9 S1 C2 C3 -134.4(18) . . . . ? _diffrn_measured_fraction_theta_max 0.443 _diffrn_reflns_theta_full 26.78 _diffrn_measured_fraction_theta_full 0.443 _refine_diff_density_max 0.55 _refine_diff_density_min -0.61 _refine_diff_density_rms 0.15 #===END of CIF data_s3pdc8 _database_code_depnum_ccdc_archive 'CCDC 607270' # Crystal 1, pressure = 76.8 kilobars _refine_special_details ; The completeness of the data is severely restricted by the geometry of the diamond anvil cell. As a result only Pd, Cl1, Cl2, S1 and S4 were refined anisotropically. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Cl2 Pd S3' _chemical_formula_sum 'C6 H12 Cl2 Pd S3' _chemical_formula_weight 357.64 _cell_measurement_pressure 7680000 _diffrn_ambient_pressure 7680000 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.9234(9) _cell_length_b 11.3268(11) _cell_length_c 11.089(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 869.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 576 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 26.6 _exptl_crystal_description tablet _exptl_crystal_colour 'intensely dark' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 3.399 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.134 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.8406 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 16.2 SMX' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1403 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.049 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 26.85 _reflns_number_total 441 _reflns_number_gt 415 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2004)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON' _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^)+(0.060P)^2^+1.958P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(17) _refine_ls_number_reflns 437 _refine_ls_number_parameters 74 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.12 _refine_ls_restrained_S_all 1.15 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.1973(2) 0.16758(9) 0.3534(3) 0.0190(15) Uani 1 1 d U . . Cl1 Cl 0.1029(11) 0.0089(4) 0.4701(13) 0.047(3) Uani 1 1 d U . . Cl2 Cl 0.4400(7) 0.0654(4) 0.2604(12) 0.044(5) Uani 1 1 d U . . S1 S -0.0233(7) 0.1868(3) 0.1458(13) 0.021(3) Uani 1 1 d DU . . C2 C -0.188(3) 0.2967(16) 0.206(3) 0.048(7) Uiso 1 1 d DU . . H2A H -0.1319 0.3748 0.1990 0.058 Uiso 1 1 calc R . . H2B H -0.3084 0.2958 0.1605 0.058 Uiso 1 1 calc R . . C3 C -0.226(3) 0.267(2) 0.336(3) 0.061(8) Uiso 1 1 d DU . . H3A H -0.2777 0.1875 0.3386 0.073 Uiso 1 1 calc R . . H3B H -0.3269 0.3194 0.3644 0.073 Uiso 1 1 calc R . . S4 S -0.0299(7) 0.2739(4) 0.4444(11) 0.018(3) Uani 1 1 d DU . . C5 C 0.046(3) 0.4227(13) 0.441(4) 0.044(7) Uiso 1 1 d DU . . H5A H -0.0612 0.4710 0.4141 0.053 Uiso 1 1 calc R . . H5B H 0.0774 0.4468 0.5227 0.053 Uiso 1 1 calc R . . C6 C 0.213(3) 0.4474(13) 0.364(3) 0.024(5) Uiso 1 1 d DU . . H6A H 0.3070 0.4881 0.4135 0.029 Uiso 1 1 calc R . . H6B H 0.1701 0.5033 0.3033 0.029 Uiso 1 1 calc R . . S7 S 0.3360(6) 0.3343(3) 0.2881(10) 0.0122(12) Uiso 1 1 d DU . . C8 C 0.265(3) 0.3643(17) 0.133(2) 0.059(8) Uiso 1 1 d DU . . H8A H 0.1844 0.4345 0.1339 0.070 Uiso 1 1 calc R . . H8B H 0.3806 0.3836 0.0883 0.070 Uiso 1 1 calc R . . C9 C 0.158(2) 0.2698(14) 0.064(3) 0.025(5) Uiso 1 1 d DU . . H9A H 0.2522 0.2144 0.0331 0.030 Uiso 1 1 calc R . . H9B H 0.0958 0.3067 -0.0044 0.030 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 Pd 0.0183(9) 0.0060(7) 0.033(5) 0.0024(10) -0.0047(15) 0.0001(5) Cl1 0.106(5) 0.016(2) 0.020(10) 0.002(4) -0.026(5) -0.032(3) Cl2 0.031(3) 0.028(3) 0.071(16) -0.020(4) -0.014(4) 0.022(2) S1 0.022(3) 0.019(2) 0.022(8) 0.003(4) -0.002(5) -0.0039(18) S4 0.015(3) 0.020(2) 0.019(9) 0.006(4) 0.006(4) -0.0077(18) 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 Pd S4 2.223(7) . ? Pd S7 2.239(5) . ? Pd Cl2 2.286(8) . ? Pd Cl1 2.309(9) . ? Pd S1 2.771(13) . ? Pd S4 3.006(10) 3_556 ? S1 C9 1.808(17) . ? S1 C2 1.815(16) . ? C2 C3 1.51(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 S4 1.813(19) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? S4 C5 1.767(14) . ? C5 C6 1.46(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 S7 1.755(17) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? S7 C8 1.82(2) . ? C8 C9 1.510(18) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? 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 S4 Pd S7 89.6(2) . . ? S4 Pd Cl2 177.43(19) . . ? S7 Pd Cl2 88.0(2) . . ? S4 Pd Cl1 88.1(3) . . ? S7 Pd Cl1 163.6(4) . . ? Cl2 Pd Cl1 93.8(3) . . ? S4 Pd S1 86.8(3) . . ? S7 Pd S1 84.3(3) . . ? Cl2 Pd S1 94.0(4) . . ? Cl1 Pd S1 111.8(3) . . ? S4 Pd S4 89.21(16) . 3_556 ? S7 Pd S4 77.6(3) . 3_556 ? Cl2 Pd S4 89.2(3) . 3_556 ? Cl1 Pd S4 86.1(3) . 3_556 ? S1 Pd S4 161.56(15) . 3_556 ? C9 S1 C2 105.2(9) . . ? C9 S1 Pd 94.2(9) . . ? C2 S1 Pd 95.6(13) . . ? C3 C2 S1 108(2) . . ? C3 C2 H2A 110.1 . . ? S1 C2 H2A 110.1 . . ? C3 C2 H2B 110.1 . . ? S1 C2 H2B 110.1 . . ? H2A C2 H2B 108.5 . . ? C2 C3 S4 120(2) . . ? C2 C3 H3A 107.4 . . ? S4 C3 H3A 107.4 . . ? C2 C3 H3B 107.4 . . ? S4 C3 H3B 107.4 . . ? H3A C3 H3B 106.9 . . ? C5 S4 C3 104.5(16) . . ? C5 S4 Pd 107.2(8) . . ? C3 S4 Pd 101.8(10) . . ? C6 C5 S4 115.4(16) . . ? C6 C5 H5A 108.4 . . ? S4 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? S4 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C5 C6 S7 121.6(13) . . ? C5 C6 H6A 106.9 . . ? S7 C6 H6A 106.9 . . ? C5 C6 H6B 106.9 . . ? S7 C6 H6B 106.9 . . ? H6A C6 H6B 106.7 . . ? C6 S7 C8 100.6(12) . . ? C6 S7 Pd 104.6(7) . . ? C8 S7 Pd 110.3(7) . . ? C9 C8 S7 118.6(17) . . ? C9 C8 H8A 107.7 . . ? S7 C8 H8A 107.7 . . ? C9 C8 H8B 107.7 . . ? S7 C8 H8B 107.7 . . ? H8A C8 H8B 107.1 . . ? C8 C9 S1 117.1(19) . . ? C8 C9 H9A 108.0 . . ? S1 C9 H9A 108.0 . . ? C8 C9 H9B 108.0 . . ? S1 C9 H9B 108.0 . . ? H9A C9 H9B 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C2 C3 S4 65(2) . . . . ? C2 C3 S4 C5 61(2) . . . . ? C3 S4 C5 C6 -97(2) . . . . ? S4 C5 C6 S7 -4(3) . . . . ? C5 C6 S7 C8 109(2) . . . . ? C6 S7 C8 C9 -120.2(18) . . . . ? S7 C8 C9 S1 40(2) . . . . ? C8 C9 S1 C2 56(2) . . . . ? C9 S1 C2 C3 -133.6(18) . . . . ? _diffrn_measured_fraction_theta_max 0.402 _diffrn_reflns_theta_full 26.85 _diffrn_measured_fraction_theta_full 0.402 _refine_diff_density_max 0.52 _refine_diff_density_min -0.41 _refine_diff_density_rms 0.12 #===END of CIF