# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year 2010 _journal_volume 39 _journal_page_first 0 #TrackingRef 'dalton.cif' # start Validation Reply Form _vrf_PLAT432_FO3742 ; PROBLEM: Short Inter X...Y Contact C16 .. C16 .. 2.69 Ang. RESPONSE: Part of a disorderd propyle group! ; # end Validation Reply Form #Added by publCIF (CCDC output) (Mo 22. Feb 14:09:27 2010) _audit_update_record ; 2010-02-22 # Formatted by publCIF ; # 1. SUBMISSION DETAILS _publ_contact_author ; Wolfgang Imhof Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 07743 Jena Germany ; _publ_contact_author_phone '03641 948 185' _publ_contact_author_fax '03641 948 102' _publ_contact_author_email w.imhof@uni-jena.de # 3. TITLE AND AUTHOR LIST _publ_section_title ; A straightforward and generalizable synthetic methodology for the synthesis of ruthenium(II) complexes with thioether ligands from either Ru(III) or Ru(0) precursors; Synthesis of the first structurally characterized dinuclear ruthenium complex with bridging tetrahydrothiophene ; loop_ _publ_author_name _publ_author_address 'Wolfgang Imhof' ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; 'Biplab Maiti ' ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; 'Olaf Klobes ' ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; H.Gorls ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena Lessing-Str. 8 D-07743 Jena Germany ; _publ_contact_author_name 'Wolfgang Imhof' # data_FO3795 _database_code_depnum_ccdc_archive 'CCDC 767201' #TrackingRef 'dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H8 Cl2 O4 Ru S' _chemical_formula_sum 'C7 H8 Cl2 O4 Ru S' _chemical_formula_weight 360.16 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' O O 0.0106 0.0060 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.0582(3) _cell_length_b 8.8920(4) _cell_length_c 22.1496(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.771(3) _cell_angle_gamma 90.00 _cell_volume 1187.14(9) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 7482 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.015 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.935 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7482 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2686 _reflns_number_gt 1995 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0321P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2686 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _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 Ru1 Ru 0.80823(4) 0.33856(3) 0.862887(12) 0.02143(10) Uani 1 1 d . . . Cl1 Cl 1.15899(14) 0.36813(10) 0.92400(4) 0.0307(2) Uani 1 1 d . . . Cl2 Cl 0.94374(14) 0.48572(10) 0.78345(4) 0.0275(2) Uani 1 1 d . . . S1 S 0.67151(15) 0.56675(10) 0.90752(4) 0.0242(2) Uani 1 1 d . . . O1 O 0.6802(4) 0.9114(3) 0.88038(11) 0.0330(6) Uani 1 1 d . . . O2 O 1.0342(4) 0.0644(3) 0.81287(12) 0.0365(7) Uani 1 1 d . . . O3 O 0.6494(5) 0.1719(3) 0.96983(12) 0.0380(7) Uani 1 1 d . . . O4 O 0.3894(4) 0.2932(3) 0.77744(12) 0.0370(7) Uani 1 1 d . . . C1 C 0.9036(6) 0.6957(4) 0.91675(17) 0.0273(9) Uani 1 1 d . . . H1A H 1.0113 0.6619 0.9506 0.033 Uiso 1 1 calc R . . H1B H 0.9798 0.6976 0.8793 0.033 Uiso 1 1 calc R . . C2 C 0.8207(6) 0.8513(4) 0.92993(17) 0.0319(9) Uani 1 1 d . . . H2A H 0.7379 0.8471 0.9662 0.038 Uiso 1 1 calc R . . H2B H 0.9492 0.9191 0.9392 0.038 Uiso 1 1 calc R . . C3 C 0.4776(6) 0.8315(4) 0.86851(17) 0.0296(9) Uani 1 1 d . . . H3A H 0.3812 0.8853 0.8368 0.036 Uiso 1 1 calc R . . H3B H 0.4004 0.8294 0.9058 0.036 Uiso 1 1 calc R . . C4 C 0.5120(6) 0.6713(4) 0.84767(16) 0.0276(8) Uani 1 1 d . . . H4A H 0.5918 0.6720 0.8108 0.033 Uiso 1 1 calc R . . H4B H 0.3664 0.6221 0.8374 0.033 Uiso 1 1 calc R . . C5 C 0.9425(6) 0.1624(4) 0.83061(16) 0.0253(8) Uani 1 1 d . . . C6 C 0.7045(6) 0.2305(4) 0.92863(17) 0.0265(8) Uani 1 1 d . . . C7 C 0.5411(6) 0.3107(4) 0.81037(16) 0.0242(8) 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 Ru1 0.01868(16) 0.02080(17) 0.02460(17) 0.00061(12) 0.00116(12) 0.00060(12) Cl1 0.0222(5) 0.0377(6) 0.0310(5) 0.0016(4) -0.0039(4) 0.0017(4) Cl2 0.0250(5) 0.0314(5) 0.0267(5) 0.0044(4) 0.0057(4) 0.0016(4) S1 0.0235(5) 0.0229(5) 0.0261(5) -0.0008(4) 0.0024(4) -0.0001(4) O1 0.0388(15) 0.0253(14) 0.0337(15) 0.0054(11) -0.0022(13) 0.0000(12) O2 0.0317(15) 0.0313(16) 0.0469(17) -0.0053(13) 0.0059(13) 0.0044(13) O3 0.0472(18) 0.0332(16) 0.0360(16) 0.0051(13) 0.0161(14) 0.0038(13) O4 0.0241(14) 0.0405(17) 0.0445(16) -0.0120(13) -0.0058(13) 0.0022(12) C1 0.0232(19) 0.030(2) 0.0282(19) -0.0051(16) -0.0017(16) -0.0034(15) C2 0.034(2) 0.028(2) 0.033(2) -0.0043(17) -0.0014(18) -0.0001(17) C3 0.0272(19) 0.031(2) 0.031(2) -0.0022(17) 0.0021(16) 0.0070(17) C4 0.0233(19) 0.031(2) 0.0271(19) 0.0007(16) -0.0021(16) 0.0012(16) C5 0.0208(18) 0.028(2) 0.0267(19) 0.0023(17) -0.0011(16) -0.0026(16) C6 0.0228(19) 0.025(2) 0.031(2) -0.0041(17) 0.0010(17) 0.0043(16) C7 0.0239(19) 0.023(2) 0.0267(19) -0.0059(15) 0.0097(17) 0.0015(15) _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 Ru1 C6 1.903(4) . ? Ru1 C7 1.912(4) . ? Ru1 C5 1.935(4) . ? Ru1 Cl2 2.4026(9) . ? Ru1 Cl1 2.4163(8) . ? Ru1 S1 2.4383(9) . ? S1 C1 1.810(3) . ? S1 C4 1.816(3) . ? O1 C2 1.423(4) . ? O1 C3 1.420(4) . ? O2 C5 1.126(4) . ? O3 C6 1.130(4) . ? O4 C7 1.125(4) . ? C1 C2 1.510(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.519(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 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 C6 Ru1 C7 94.35(15) . . ? C6 Ru1 C5 93.28(15) . . ? C7 Ru1 C5 91.82(14) . . ? C6 Ru1 Cl2 177.02(11) . . ? C7 Ru1 Cl2 87.45(11) . . ? C5 Ru1 Cl2 89.03(11) . . ? C6 Ru1 Cl1 88.03(10) . . ? C7 Ru1 Cl1 176.29(11) . . ? C5 Ru1 Cl1 85.20(10) . . ? Cl2 Ru1 Cl1 90.29(3) . . ? C6 Ru1 S1 87.61(11) . . ? C7 Ru1 S1 93.06(10) . . ? C5 Ru1 S1 174.96(10) . . ? Cl2 Ru1 S1 89.93(3) . . ? Cl1 Ru1 S1 89.87(3) . . ? C1 S1 C4 96.23(16) . . ? C1 S1 Ru1 106.34(12) . . ? C4 S1 Ru1 107.90(12) . . ? C2 O1 C3 113.2(3) . . ? C2 C1 S1 109.4(3) . . ? C2 C1 H1A 109.8 . . ? S1 C1 H1A 109.8 . . ? C2 C1 H1B 109.8 . . ? S1 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? O1 C2 C1 112.3(3) . . ? O1 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? O1 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? O1 C3 C4 112.6(3) . . ? O1 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? O1 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C3 C4 S1 109.7(2) . . ? C3 C4 H4A 109.7 . . ? S1 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? S1 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? O2 C5 Ru1 175.3(3) . . ? O3 C6 Ru1 176.1(3) . . ? O4 C7 Ru1 177.0(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.495 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.125 #=== END data_FO3950 _database_code_depnum_ccdc_archive 'CCDC 767202' #TrackingRef 'dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H18 Cl2 O2 Ru S2' _chemical_formula_sum 'C10 H18 Cl2 O2 Ru S2' _chemical_formula_weight 406.33 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' O O 0.0106 0.0060 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6574(6) _cell_length_b 10.9318(4) _cell_length_c 13.3984(8) _cell_angle_alpha 90.00 _cell_angle_beta 114.560(2) _cell_angle_gamma 90.00 _cell_volume 1552.96(13) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 14317 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 27.44 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.610 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14317 _diffrn_reflns_av_R_equivalents 0.1774 _diffrn_reflns_av_sigmaI/netI 0.1125 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3536 _reflns_number_gt 2562 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0280P)^2^+9.7514P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3536 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1087 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.82481(5) 0.15703(5) 0.59069(4) 0.01726(14) Uani 1 1 d . . . Cl1 Cl 0.77713(16) 0.22597(16) 0.40613(13) 0.0278(4) Uani 1 1 d . . . Cl2 Cl 0.61026(14) 0.19302(15) 0.57009(12) 0.0255(4) Uani 1 1 d . . . S1 S 0.86518(14) 0.36778(14) 0.65105(12) 0.0193(3) Uani 1 1 d . . . S2 S 0.85105(14) 0.10807(15) 0.77033(12) 0.0203(3) Uani 1 1 d . . . O1 O 1.0914(5) 0.1107(5) 0.6209(4) 0.0392(13) Uani 1 1 d . . . O2 O 0.7448(5) -0.1000(5) 0.5064(4) 0.0390(12) Uani 1 1 d . . . C5 C 0.9595(6) 0.6464(7) 0.6505(6) 0.0334(16) Uani 1 1 d . . . H5A H 0.9940 0.7228 0.6898 0.050 Uiso 1 1 calc R . . H5B H 0.8817 0.6257 0.6579 0.050 Uiso 1 1 calc R . . H5C H 0.9412 0.6567 0.5726 0.050 Uiso 1 1 calc R . . C4 C 1.0547(6) 0.5448(7) 0.6984(6) 0.0324(16) Uani 1 1 d . . . H4A H 1.0755 0.5378 0.7777 0.039 Uiso 1 1 calc R . . H4B H 1.1331 0.5670 0.6909 0.039 Uiso 1 1 calc R . . C3 C 1.0102(6) 0.4214(6) 0.6451(5) 0.0244(14) Uani 1 1 d . . . H3A H 1.0775 0.3604 0.6815 0.029 Uiso 1 1 calc R . . H3B H 0.9967 0.4264 0.5672 0.029 Uiso 1 1 calc R . . C1 C 0.9188(6) 0.3552(6) 0.7993(5) 0.0214(13) Uani 1 1 d . . . H1A H 1.0093 0.3330 0.8335 0.026 Uiso 1 1 calc R . . H1B H 0.9085 0.4348 0.8299 0.026 Uiso 1 1 calc R . . C2 C 0.8428(6) 0.2589(6) 0.8248(5) 0.0231(14) Uani 1 1 d . . . H2A H 0.7535 0.2853 0.7944 0.028 Uiso 1 1 calc R . . H2B H 0.8728 0.2526 0.9054 0.028 Uiso 1 1 calc R . . C6 C 1.0132(6) 0.0648(6) 0.8547(5) 0.0254(14) Uani 1 1 d . . . H6A H 1.0712 0.1240 0.8436 0.030 Uiso 1 1 calc R . . H6B H 1.0285 0.0668 0.9331 0.030 Uiso 1 1 calc R . . C7 C 1.0395(6) -0.0641(6) 0.8240(6) 0.0292(15) Uani 1 1 d . . . H7A H 0.9807 -0.1230 0.8343 0.035 Uiso 1 1 calc R . . H7B H 1.0248 -0.0657 0.7458 0.035 Uiso 1 1 calc R . . C8 C 1.1747(7) -0.1019(7) 0.8949(7) 0.0407(19) Uani 1 1 d . . . H8A H 1.1906 -0.1831 0.8723 0.061 Uiso 1 1 calc R . . H8B H 1.1880 -0.1044 0.9720 0.061 Uiso 1 1 calc R . . H8C H 1.2328 -0.0425 0.8860 0.061 Uiso 1 1 calc R . . C9 C 0.9923(7) 0.1287(6) 0.6100(5) 0.0251(14) Uani 1 1 d . . . C10 C 0.7745(5) -0.0079(7) 0.5375(5) 0.0204(13) 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 Ru1 0.0180(2) 0.0178(2) 0.0165(2) 0.0010(2) 0.00763(18) 0.0004(2) Cl1 0.0289(8) 0.0321(9) 0.0237(8) 0.0030(7) 0.0122(7) -0.0009(7) Cl2 0.0193(7) 0.0333(9) 0.0219(7) -0.0006(6) 0.0065(6) 0.0013(6) S1 0.0216(7) 0.0165(8) 0.0200(7) -0.0001(6) 0.0088(6) -0.0001(6) S2 0.0205(7) 0.0225(8) 0.0173(7) 0.0017(6) 0.0073(6) -0.0030(6) O1 0.022(3) 0.046(3) 0.059(3) 0.004(3) 0.025(2) 0.009(2) O2 0.049(3) 0.035(3) 0.041(3) -0.008(3) 0.028(3) -0.008(3) C5 0.027(4) 0.028(4) 0.053(4) -0.013(3) 0.024(3) -0.009(3) C4 0.028(4) 0.031(4) 0.036(4) -0.002(3) 0.012(3) -0.010(3) C3 0.026(3) 0.021(3) 0.033(4) 0.001(3) 0.020(3) -0.003(3) C1 0.022(3) 0.023(3) 0.018(3) -0.005(3) 0.008(2) -0.003(3) C2 0.022(3) 0.027(4) 0.021(3) -0.003(3) 0.010(3) -0.003(3) C6 0.023(3) 0.027(4) 0.019(3) 0.004(3) 0.002(3) -0.001(3) C7 0.028(4) 0.023(4) 0.033(4) 0.004(3) 0.009(3) -0.001(3) C8 0.034(4) 0.028(4) 0.050(5) 0.011(4) 0.009(4) 0.012(3) C9 0.035(4) 0.021(4) 0.022(3) 0.002(3) 0.014(3) 0.004(3) C10 0.017(3) 0.033(4) 0.014(3) -0.002(3) 0.010(2) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C9 1.886(7) . ? Ru1 C10 1.938(7) . ? Ru1 S2 2.3581(15) . ? Ru1 Cl1 2.4186(16) . ? Ru1 S1 2.4222(16) . ? Ru1 Cl2 2.4315(16) . ? S1 C3 1.822(6) . ? S1 C1 1.824(6) . ? S2 C6 1.816(6) . ? S2 C2 1.822(7) . ? O1 C9 1.120(8) . ? O2 C10 1.090(8) . ? C5 C4 1.512(10) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C4 C3 1.514(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C1 C2 1.503(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C6 C7 1.533(10) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.521(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 C9 Ru1 C10 92.0(3) . . ? C9 Ru1 S2 97.77(19) . . ? C10 Ru1 S2 93.18(18) . . ? C9 Ru1 Cl1 88.63(19) . . ? C10 Ru1 Cl1 90.44(18) . . ? S2 Ru1 Cl1 172.52(6) . . ? C9 Ru1 S1 93.7(2) . . ? C10 Ru1 S1 174.18(18) . . ? S2 Ru1 S1 87.16(5) . . ? Cl1 Ru1 S1 88.58(6) . . ? C9 Ru1 Cl2 178.76(19) . . ? C10 Ru1 Cl2 88.22(18) . . ? S2 Ru1 Cl2 81.00(5) . . ? Cl1 Ru1 Cl2 92.58(6) . . ? S1 Ru1 Cl2 86.10(6) . . ? C3 S1 C1 99.7(3) . . ? C3 S1 Ru1 110.3(2) . . ? C1 S1 Ru1 102.9(2) . . ? C6 S2 C2 101.6(3) . . ? C6 S2 Ru1 110.7(2) . . ? C2 S2 Ru1 101.4(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C5 C4 C3 114.0(6) . . ? C5 C4 H4A 108.7 . . ? C3 C4 H4A 108.7 . . ? C5 C4 H4B 108.7 . . ? C3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C4 C3 S1 114.1(5) . . ? C4 C3 H3A 108.7 . . ? S1 C3 H3A 108.7 . . ? C4 C3 H3B 108.7 . . ? S1 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C2 C1 S1 109.4(4) . . ? C2 C1 H1A 109.8 . . ? S1 C1 H1A 109.8 . . ? C2 C1 H1B 109.8 . . ? S1 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? C1 C2 S2 114.1(5) . . ? C1 C2 H2A 108.7 . . ? S2 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? S2 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C7 C6 S2 110.2(4) . . ? C7 C6 H6A 109.6 . . ? S2 C6 H6A 109.6 . . ? C7 C6 H6B 109.6 . . ? S2 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C6 110.7(6) . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 Ru1 179.2(7) . . ? O2 C10 Ru1 179.0(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.930 _refine_diff_density_min -1.568 _refine_diff_density_rms 0.178 #=== END data_FO3743 _database_code_depnum_ccdc_archive 'CCDC 767203' #TrackingRef 'dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H32 Cl2 O4 Ru S4, 2(C H Cl3)' _chemical_formula_sum 'C18 H34 Cl8 O4 Ru S4' _chemical_formula_weight 827.36 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' O O 0.0106 0.0060 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9993(4) _cell_length_b 9.6273(3) _cell_length_c 12.9450(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.500(2) _cell_angle_gamma 90.00 _cell_volume 1619.98(9) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 11159 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 1.426 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11159 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3695 _reflns_number_gt 3068 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0534P)^2^+1.4611P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3695 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.5000 0.0000 0.5000 0.01642(11) Uani 1 2 d S . . Cl1 Cl 0.56346(6) 0.05358(8) 0.67214(5) 0.02418(17) Uani 1 1 d . . . S1 S 0.62079(5) -0.17920(7) 0.48228(5) 0.02025(16) Uani 1 1 d . . . S2 S 0.61873(5) 0.15896(7) 0.43174(6) 0.02189(17) Uani 1 1 d . . . O1 O 0.6711(2) -0.4930(2) 0.52589(18) 0.0315(5) Uani 1 1 d . . . O2 O 0.84189(17) 0.1728(2) 0.33976(18) 0.0322(5) Uani 1 1 d . . . C1 C 0.6493(2) -0.2641(3) 0.6039(2) 0.0261(7) Uani 1 1 d . . . H1A H 0.6830 -0.1978 0.6518 0.031 Uiso 1 1 calc R . . H1B H 0.5848 -0.2967 0.6359 0.031 Uiso 1 1 calc R . . C2 C 0.7199(3) -0.3865(3) 0.5843(2) 0.0305(7) Uani 1 1 d . . . H2A H 0.7814 -0.3538 0.5468 0.037 Uiso 1 1 calc R . . H2B H 0.7434 -0.4252 0.6514 0.037 Uiso 1 1 calc R . . C3 C 0.6469(3) -0.4505(3) 0.4234(2) 0.0299(7) Uani 1 1 d . . . H3A H 0.6189 -0.5309 0.3847 0.036 Uiso 1 1 calc R . . H3B H 0.7110 -0.4209 0.3889 0.036 Uiso 1 1 calc R . . C4 C 0.5695(2) -0.3321(3) 0.4183(2) 0.0264(7) Uani 1 1 d . . . H4A H 0.5049 -0.3609 0.4520 0.032 Uiso 1 1 calc R . . H4B H 0.5536 -0.3100 0.3452 0.032 Uiso 1 1 calc R . . C5 C 0.6637(2) 0.1048(3) 0.3057(2) 0.0269(6) Uani 1 1 d . . . H5A H 0.6841 0.0057 0.3082 0.032 Uiso 1 1 calc R . . H5B H 0.6074 0.1147 0.2542 0.032 Uiso 1 1 calc R . . C6 C 0.7546(2) 0.1921(3) 0.2734(3) 0.0298(7) Uani 1 1 d . . . H6A H 0.7737 0.1676 0.2018 0.036 Uiso 1 1 calc R . . H6B H 0.7346 0.2913 0.2741 0.036 Uiso 1 1 calc R . . C7 C 0.8244(3) 0.2239(4) 0.4416(3) 0.0347(8) Uani 1 1 d . . . H7A H 0.8033 0.3226 0.4376 0.042 Uiso 1 1 calc R . . H7B H 0.8893 0.2191 0.4820 0.042 Uiso 1 1 calc R . . C8 C 0.7420(2) 0.1418(4) 0.4968(2) 0.0313(7) Uani 1 1 d . . . H8A H 0.7362 0.1756 0.5687 0.038 Uiso 1 1 calc R . . H8B H 0.7619 0.0426 0.4992 0.038 Uiso 1 1 calc R . . Cl3A Cl 0.99814(11) -0.45311(16) 0.37703(10) 0.0738(4) Uani 1 1 d . . . Cl2A Cl 0.88727(11) -0.20287(14) 0.32405(11) 0.0711(4) Uani 1 1 d . . . Cl1A Cl 0.87571(12) -0.4441(2) 0.19270(13) 0.1017(6) Uani 1 1 d . . . C1CL C 0.9550(3) -0.3463(5) 0.2756(3) 0.0488(10) Uani 1 1 d . . . H1CA H 1.0158 -0.3123 0.2361 0.059 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 Ru1 0.01723(17) 0.01565(17) 0.01639(17) -0.00071(12) 0.00055(12) -0.00024(12) Cl1 0.0287(4) 0.0254(4) 0.0184(3) -0.0022(3) -0.0029(3) -0.0014(3) S1 0.0203(4) 0.0172(3) 0.0233(4) 0.0000(3) 0.0016(3) 0.0014(3) S2 0.0196(4) 0.0187(3) 0.0274(4) 0.0001(3) 0.0054(3) -0.0009(3) O1 0.0446(14) 0.0196(11) 0.0301(12) 0.0021(9) 0.0003(10) 0.0036(9) O2 0.0236(11) 0.0363(13) 0.0367(13) 0.0019(10) 0.0078(10) 0.0025(10) C1 0.0305(16) 0.0253(15) 0.0225(15) -0.0008(12) -0.0028(12) 0.0056(13) C2 0.0357(18) 0.0263(16) 0.0294(17) 0.0038(13) -0.0031(14) 0.0087(14) C3 0.0407(19) 0.0230(15) 0.0258(16) -0.0024(13) 0.0012(14) 0.0063(14) C4 0.0315(17) 0.0216(15) 0.0260(15) -0.0063(12) -0.0012(13) 0.0004(12) C5 0.0278(16) 0.0311(16) 0.0217(14) 0.0013(13) 0.0023(12) -0.0028(13) C6 0.0294(17) 0.0329(17) 0.0272(16) 0.0065(13) 0.0085(13) -0.0020(14) C7 0.0253(17) 0.0401(19) 0.0389(19) -0.0046(16) 0.0033(14) -0.0083(14) C8 0.0267(16) 0.0419(19) 0.0252(16) -0.0032(14) -0.0013(13) -0.0074(14) Cl3A 0.0814(9) 0.0875(9) 0.0524(7) 0.0108(6) -0.0056(6) 0.0149(7) Cl2A 0.0719(8) 0.0642(7) 0.0772(9) 0.0030(6) 0.0071(7) 0.0027(6) Cl1A 0.0707(9) 0.1341(14) 0.0996(12) -0.0523(11) -0.0445(9) 0.0357(9) C1CL 0.0254(18) 0.084(3) 0.037(2) 0.007(2) 0.0058(16) -0.0028(19) _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 Ru1 S1 2.3453(7) 3_656 ? Ru1 S1 2.3453(7) . ? Ru1 S2 2.3513(7) . ? Ru1 S2 2.3513(7) 3_656 ? Ru1 Cl1 2.4249(7) 3_656 ? Ru1 Cl1 2.4249(7) . ? S1 C4 1.814(3) . ? S1 C1 1.809(3) . ? S2 C8 1.811(3) . ? S2 C5 1.815(3) . ? O1 C3 1.422(4) . ? O1 C2 1.421(4) . ? O2 C7 1.428(4) . ? O2 C6 1.429(4) . ? C1 C2 1.517(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.521(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.513(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.515(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? Cl3A C1CL 1.756(4) . ? Cl2A C1CL 1.757(5) . ? Cl1A C1CL 1.755(4) . ? C1CL H1CA 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ru1 S1 180.0 3_656 . ? S1 Ru1 S2 90.01(3) 3_656 . ? S1 Ru1 S2 89.99(3) . . ? S1 Ru1 S2 89.99(3) 3_656 3_656 ? S1 Ru1 S2 90.01(3) . 3_656 ? S2 Ru1 S2 180.0 . 3_656 ? S1 Ru1 Cl1 91.36(2) 3_656 3_656 ? S1 Ru1 Cl1 88.64(2) . 3_656 ? S2 Ru1 Cl1 90.70(3) . 3_656 ? S2 Ru1 Cl1 89.30(3) 3_656 3_656 ? S1 Ru1 Cl1 88.64(2) 3_656 . ? S1 Ru1 Cl1 91.36(2) . . ? S2 Ru1 Cl1 89.30(3) . . ? S2 Ru1 Cl1 90.70(3) 3_656 . ? Cl1 Ru1 Cl1 180.0 3_656 . ? C4 S1 C1 95.88(15) . . ? C4 S1 Ru1 113.47(10) . . ? C1 S1 Ru1 112.29(10) . . ? C8 S2 C5 95.80(15) . . ? C8 S2 Ru1 110.31(11) . . ? C5 S2 Ru1 111.62(10) . . ? C3 O1 C2 112.5(2) . . ? C7 O2 C6 112.2(2) . . ? C2 C1 S1 109.0(2) . . ? C2 C1 H1A 109.9 . . ? S1 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? S1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? O1 C2 C1 112.4(3) . . ? O1 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? O1 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? O1 C3 C4 113.4(3) . . ? O1 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? O1 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C3 C4 S1 110.4(2) . . ? C3 C4 H4A 109.6 . . ? S1 C4 H4A 109.6 . . ? C3 C4 H4B 109.6 . . ? S1 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C6 C5 S2 110.3(2) . . ? C6 C5 H5A 109.6 . . ? S2 C5 H5A 109.6 . . ? C6 C5 H5B 109.6 . . ? S2 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? O2 C6 C5 112.3(3) . . ? O2 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? O2 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? O2 C7 C8 112.0(3) . . ? O2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? O2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 S2 111.1(2) . . ? C7 C8 H8A 109.4 . . ? S2 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? S2 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? Cl3A C1CL Cl2A 110.6(2) . . ? Cl3A C1CL Cl1A 109.0(3) . . ? Cl2A C1CL Cl1A 110.3(2) . . ? Cl3A C1CL H1CA 109.0 . . ? Cl2A C1CL H1CA 109.0 . . ? Cl1A C1CL H1CA 109.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.053 _refine_diff_density_min -1.471 _refine_diff_density_rms 0.108 #=== END data_FO3742 _database_code_depnum_ccdc_archive 'CCDC 767204' #TrackingRef 'dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 Cl2 Ru S4' _chemical_formula_sum 'C16 H36 Cl2 Ru S4' _chemical_formula_weight 528.66 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall 'C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.6376(9) _cell_length_b 20.1958(9) _cell_length_c 11.2202(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.911(3) _cell_angle_gamma 90.00 _cell_volume 4620.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 16068 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 1.269 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16068 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5292 _reflns_number_gt 3472 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5292 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 Ru1 Ru 0.710033(15) 0.129831(14) 0.73554(2) 0.02247(11) Uani 1 1 d . . . Cl1 Cl 0.69173(5) 0.12767(5) 0.51667(7) 0.0322(2) Uani 1 1 d . . . Cl2 Cl 0.72726(5) 0.13020(5) 0.95404(7) 0.0315(2) Uani 1 1 d . . . S1 S 0.60994(5) 0.07908(5) 0.75147(8) 0.0281(2) Uani 1 1 d . . . S2 S 0.75507(5) 0.02342(5) 0.72282(8) 0.0321(2) Uani 1 1 d . . . S3 S 0.81278(5) 0.18101(5) 0.75479(8) 0.0297(2) Uani 1 1 d . C . S4 S 0.66388(5) 0.23575(5) 0.72044(7) 0.0263(2) Uani 1 1 d . . . C1 C 0.6827(2) -0.0293(2) 0.7015(4) 0.0392(10) Uani 1 1 d . . . H1A H 0.6627 -0.0286 0.6154 0.047 Uiso 1 1 calc R . . H1B H 0.6959 -0.0755 0.7228 0.047 Uiso 1 1 calc R . . C2 C 0.6329(2) -0.0075(2) 0.7769(3) 0.0376(10) Uani 1 1 d . . . H2A H 0.6508 -0.0139 0.8632 0.045 Uiso 1 1 calc R . . H2B H 0.5932 -0.0355 0.7580 0.045 Uiso 1 1 calc R . . C3 C 0.5553(2) 0.0711(2) 0.6089(3) 0.0358(10) Uani 1 1 d . . . H3A H 0.5802 0.0544 0.5465 0.043 Uiso 1 1 calc R . . H3B H 0.5204 0.0387 0.6176 0.043 Uiso 1 1 calc R . . C4 C 0.5245(2) 0.1376(2) 0.5693(3) 0.0389(10) Uani 1 1 d . . . H4A H 0.5591 0.1688 0.5531 0.047 Uiso 1 1 calc R . . H4B H 0.5033 0.1564 0.6351 0.047 Uiso 1 1 calc R . . C5 C 0.4735(3) 0.1300(3) 0.4557(4) 0.0607(15) Uani 1 1 d . . . H5A H 0.4563 0.1736 0.4291 0.091 Uiso 1 1 calc R . . H5B H 0.4375 0.1019 0.4736 0.091 Uiso 1 1 calc R . . H5C H 0.4941 0.1095 0.3917 0.091 Uiso 1 1 calc R . . C6 C 0.7937(2) -0.0088(2) 0.8681(4) 0.0451(12) Uani 1 1 d . A . H6A H 0.7663 0.0025 0.9303 0.054 Uiso 1 1 calc R . . H6B H 0.7964 -0.0576 0.8635 0.054 Uiso 1 1 calc R . . C7 C 0.8616(3) 0.0193(3) 0.9046(5) 0.0688(17) Uani 1 1 d . . . H7A H 0.8590 0.0681 0.8956 0.083 Uiso 0.714(9) 1 calc PR A 1 H7B H 0.8758 0.0097 0.9912 0.083 Uiso 0.714(9) 1 calc PR A 1 H7C H 0.8829 0.0226 0.8316 0.083 Uiso 0.286(9) 1 calc PR A 2 H7D H 0.8573 0.0649 0.9350 0.083 Uiso 0.286(9) 1 calc PR A 2 C8 C 0.9117(5) -0.0047(5) 0.8382(8) 0.095(3) Uiso 0.714(9) 1 d P A 1 H8A H 0.9536 0.0168 0.8686 0.142 Uiso 0.714(9) 1 calc PR A 1 H8B H 0.8991 0.0056 0.7523 0.142 Uiso 0.714(9) 1 calc PR A 1 H8C H 0.9163 -0.0527 0.8486 0.142 Uiso 0.714(9) 1 calc PR A 1 C8A C 0.9019(11) -0.0154(10) 0.9900(17) 0.073(7) Uiso 0.286(9) 1 d P A 2 H8AA H 0.9446 0.0068 1.0069 0.109 Uiso 0.286(9) 1 calc PR A 2 H8AB H 0.9079 -0.0603 0.9603 0.109 Uiso 0.286(9) 1 calc PR A 2 H8AC H 0.8823 -0.0177 1.0640 0.109 Uiso 0.286(9) 1 calc PR A 2 C9 C 0.7948(2) 0.2649(2) 0.7993(3) 0.0345(10) Uani 1 1 d . . . H9A H 0.7904 0.2651 0.8859 0.041 Uiso 1 1 calc R . . H9B H 0.8320 0.2941 0.7887 0.041 Uiso 1 1 calc R . . C10 C 0.7330(2) 0.29225(19) 0.7273(3) 0.0314(9) Uani 1 1 d . . . H10A H 0.7409 0.3019 0.6443 0.038 Uiso 1 1 calc R . . H10B H 0.7218 0.3345 0.7640 0.038 Uiso 1 1 calc R . . C11 C 0.6319(2) 0.2589(2) 0.8565(3) 0.0327(9) Uani 1 1 d . B . H11A H 0.6044 0.2223 0.8794 0.039 Uiso 1 1 calc R . . H11B H 0.6690 0.2649 0.9229 0.039 Uiso 1 1 calc R . . C12 C 0.5918(3) 0.3212(3) 0.8428(4) 0.0581(15) Uani 1 1 d . . . H12A H 0.6215 0.3594 0.8393 0.070 Uiso 0.806(9) 1 calc PR B 1 H12B H 0.5615 0.3195 0.7653 0.070 Uiso 0.806(9) 1 calc PR B 1 H12C H 0.5473 0.3035 0.8157 0.070 Uiso 0.194(9) 1 calc PR B 2 H12D H 0.5919 0.3338 0.9281 0.070 Uiso 0.194(9) 1 calc PR B 2 C13 C 0.5531(3) 0.3322(3) 0.9421(4) 0.0433(16) Uiso 0.806(9) 1 d P B 1 H13A H 0.5280 0.3733 0.9275 0.065 Uiso 0.806(9) 1 calc PR B 1 H13B H 0.5828 0.3354 1.0189 0.065 Uiso 0.806(9) 1 calc PR B 1 H13C H 0.5228 0.2950 0.9452 0.065 Uiso 0.806(9) 1 calc PR B 1 C13A C 0.5885(12) 0.3722(12) 0.796(2) 0.045(7) Uiso 0.194(9) 1 d P B 2 H13D H 0.6125 0.3710 0.7276 0.068 Uiso 0.194(9) 1 calc PR B 2 H13E H 0.6079 0.4059 0.8541 0.068 Uiso 0.194(9) 1 calc PR B 2 H13F H 0.5424 0.3831 0.7683 0.068 Uiso 0.194(9) 1 calc PR B 2 C14 C 0.8398(2) 0.1965(2) 0.6103(3) 0.0429(11) Uani 1 1 d . . . H14A H 0.8214 0.1614 0.5533 0.051 Uiso 0.535(7) 1 calc PR C 1 H14B H 0.8209 0.2392 0.5784 0.051 Uiso 0.535(7) 1 calc PR C 1 H14C H 0.8009 0.2050 0.5485 0.051 Uiso 0.465(7) 1 calc PR C 2 H14D H 0.8676 0.2366 0.6170 0.051 Uiso 0.465(7) 1 calc PR C 2 C15 C 0.9108(4) 0.1988(4) 0.6120(7) 0.039(2) Uiso 0.535(7) 1 d P C 1 H15A H 0.9300 0.1559 0.6421 0.047 Uiso 0.535(7) 1 calc PR C 1 H15B H 0.9197 0.2047 0.5284 0.047 Uiso 0.535(7) 1 calc PR C 1 C16 C 0.9404(7) 0.2478(7) 0.6812(10) 0.103(5) Uiso 0.535(7) 1 d P C 1 H16A H 0.9877 0.2465 0.6794 0.154 Uiso 0.535(7) 1 calc PR C 1 H16B H 0.9323 0.2419 0.7644 0.154 Uiso 0.535(7) 1 calc PR C 1 H16C H 0.9226 0.2905 0.6504 0.154 Uiso 0.535(7) 1 calc PR C 1 C15A C 0.8750(7) 0.1436(7) 0.5732(12) 0.082(4) Uiso 0.465(7) 1 d P C 2 H15C H 0.8800 0.1512 0.4879 0.098 Uiso 0.465(7) 1 calc PR C 2 H15D H 0.8482 0.1031 0.5753 0.098 Uiso 0.465(7) 1 calc PR C 2 C16A C 0.9402(6) 0.1303(7) 0.6414(10) 0.075(4) Uiso 0.465(7) 1 d P C 2 H16D H 0.9596 0.0920 0.6065 0.112 Uiso 0.465(7) 1 calc PR C 2 H16E H 0.9363 0.1209 0.7257 0.112 Uiso 0.465(7) 1 calc PR C 2 H16F H 0.9684 0.1691 0.6377 0.112 Uiso 0.465(7) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0315(2) 0.01819(17) 0.01821(16) -0.00089(11) 0.00528(11) -0.00017(13) Cl1 0.0469(6) 0.0314(6) 0.0188(4) -0.0030(4) 0.0072(4) -0.0042(5) Cl2 0.0472(6) 0.0287(5) 0.0183(4) 0.0006(3) 0.0043(4) 0.0022(5) S1 0.0337(6) 0.0250(5) 0.0263(5) -0.0020(4) 0.0068(4) -0.0026(4) S2 0.0402(6) 0.0227(5) 0.0351(5) -0.0015(4) 0.0110(4) 0.0040(5) S3 0.0320(6) 0.0284(6) 0.0290(5) 0.0028(4) 0.0058(4) -0.0015(5) S4 0.0340(6) 0.0210(5) 0.0228(4) -0.0016(3) 0.0008(4) -0.0004(4) C1 0.049(3) 0.021(2) 0.047(2) -0.0031(18) 0.004(2) 0.003(2) C2 0.046(3) 0.025(2) 0.042(2) 0.0053(17) 0.007(2) -0.008(2) C3 0.037(3) 0.030(2) 0.038(2) -0.0069(17) -0.0005(18) -0.004(2) C4 0.040(3) 0.035(3) 0.038(2) -0.0051(18) -0.0048(18) -0.003(2) C5 0.060(4) 0.055(4) 0.058(3) -0.003(2) -0.017(3) -0.002(3) C6 0.051(3) 0.032(3) 0.050(3) 0.009(2) 0.002(2) 0.005(2) C7 0.075(4) 0.042(3) 0.081(4) 0.004(3) -0.017(3) 0.002(3) C9 0.040(3) 0.028(2) 0.036(2) -0.0079(17) 0.0059(18) -0.008(2) C10 0.044(3) 0.021(2) 0.032(2) -0.0004(15) 0.0125(17) -0.0038(19) C11 0.036(2) 0.031(2) 0.033(2) 0.0003(17) 0.0114(17) 0.0019(19) C12 0.061(4) 0.066(4) 0.045(3) -0.011(2) 0.001(2) 0.028(3) C14 0.047(3) 0.047(3) 0.039(2) 0.001(2) 0.021(2) -0.002(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 Ru1 S4 2.3371(10) . ? Ru1 S1 2.3375(10) . ? Ru1 S3 2.3387(11) . ? Ru1 S2 2.3545(10) . ? Ru1 Cl2 2.4221(8) . ? Ru1 Cl1 2.4266(8) . ? S1 C3 1.816(4) . ? S1 C2 1.822(4) . ? S2 C1 1.820(4) . ? S2 C6 1.820(4) . ? S3 C9 1.820(4) . ? S3 C14 1.820(4) . ? S4 C11 1.816(4) . ? S4 C10 1.818(4) . ? C1 C2 1.495(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.523(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.530(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.509(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8A 1.363(19) . ? C7 C8 1.448(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 H7C 0.9900 . ? C7 H7D 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C8A H8AA 0.9800 . ? C8A H8AB 0.9800 . ? C8A H8AC 0.9800 . ? C9 C10 1.506(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.501(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13A 1.15(2) . ? C12 C13 1.485(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 H12C 0.9900 . ? C12 H12D 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C14 C15A 1.392(14) . ? C14 C15 1.464(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 H14C 0.9900 . ? C14 H14D 0.9900 . ? C15 C16 1.344(14) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C15A C16A 1.467(16) . ? C15A H15C 0.9900 . ? C15A H15D 0.9900 . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? 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 Ru1 S1 92.97(4) . . ? S4 Ru1 S3 87.46(4) . . ? S1 Ru1 S3 170.43(3) . . ? S4 Ru1 S2 172.44(3) . . ? S1 Ru1 S2 88.07(4) . . ? S3 Ru1 S2 92.76(4) . . ? S4 Ru1 Cl2 93.72(3) . . ? S1 Ru1 Cl2 85.23(3) . . ? S3 Ru1 Cl2 85.20(3) . . ? S2 Ru1 Cl2 93.83(3) . . ? S4 Ru1 Cl1 86.86(3) . . ? S1 Ru1 Cl1 93.93(3) . . ? S3 Ru1 Cl1 95.63(3) . . ? S2 Ru1 Cl1 85.60(3) . . ? Cl2 Ru1 Cl1 179.01(4) . . ? C3 S1 C2 99.40(19) . . ? C3 S1 Ru1 114.00(15) . . ? C2 S1 Ru1 102.80(15) . . ? C1 S2 C6 98.3(2) . . ? C1 S2 Ru1 102.62(14) . . ? C6 S2 Ru1 113.20(16) . . ? C9 S3 C14 100.8(2) . . ? C9 S3 Ru1 102.49(14) . . ? C14 S3 Ru1 113.05(16) . . ? C11 S4 C10 100.81(18) . . ? C11 S4 Ru1 111.84(13) . . ? C10 S4 Ru1 105.26(14) . . ? C2 C1 S2 112.0(3) . . ? C2 C1 H1A 109.2 . . ? S2 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? S2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 C2 S1 112.3(3) . . ? C1 C2 H2A 109.1 . . ? S1 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? S1 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C4 C3 S1 110.6(3) . . ? C4 C3 H3A 109.5 . . ? S1 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? S1 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C3 C4 C5 110.8(3) . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 S2 111.6(3) . . ? C7 C6 H6A 109.3 . . ? S2 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? S2 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C8A C7 C8 77.4(10) . . ? C8A C7 C6 115.9(10) . . ? C8 C7 C6 116.2(6) . . ? C8A C7 H7A 127.0 . . ? C8 C7 H7A 108.2 . . ? C6 C7 H7A 108.2 . . ? C8A C7 H7B 32.1 . . ? C8 C7 H7B 108.2 . . ? C6 C7 H7B 108.2 . . ? H7A C7 H7B 107.4 . . ? C8A C7 H7C 108.3 . . ? C8 C7 H7C 32.0 . . ? C6 C7 H7C 108.3 . . ? H7A C7 H7C 82.8 . . ? H7B C7 H7C 136.3 . . ? C8A C7 H7D 108.3 . . ? C8 C7 H7D 126.7 . . ? C6 C7 H7D 108.3 . . ? H7A C7 H7D 26.5 . . ? H7B C7 H7D 82.7 . . ? H7C C7 H7D 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C8A H8AA 109.5 . . ? C7 C8A H8AB 109.5 . . ? H8AA C8A H8AB 109.5 . . ? C7 C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? C10 C9 S3 112.7(3) . . ? C10 C9 H9A 109.0 . . ? S3 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? S3 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 S4 112.7(3) . . ? C9 C10 H10A 109.0 . . ? S4 C10 H10A 109.0 . . ? C9 C10 H10B 109.0 . . ? S4 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C12 C11 S4 113.3(3) . . ? C12 C11 H11A 108.9 . . ? S4 C11 H11A 108.9 . . ? C12 C11 H11B 108.9 . . ? S4 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C13A C12 C13 101.8(13) . . ? C13A C12 C11 142.2(14) . . ? C13 C12 C11 113.6(4) . . ? C13A C12 H12A 43.8 . . ? C13 C12 H12A 108.9 . . ? C11 C12 H12A 108.9 . . ? C13A C12 H12B 69.5 . . ? C13 C12 H12B 108.9 . . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C13A C12 H12C 101.4 . . ? C13 C12 H12C 72.6 . . ? C11 C12 H12C 101.4 . . ? H12A C12 H12C 145.2 . . ? H12B C12 H12C 44.5 . . ? C13A C12 H12D 101.4 . . ? C13 C12 H12D 32.6 . . ? C11 C12 H12D 101.4 . . ? H12A C12 H12D 86.0 . . ? H12B C12 H12D 139.8 . . ? H12C C12 H12D 104.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C13A H13D 109.5 . . ? C12 C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? C12 C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C15A C14 C15 57.3(7) . . ? C15A C14 S3 112.4(7) . . ? C15 C14 S3 116.0(4) . . ? C15A C14 H14A 54.8 . . ? C15 C14 H14A 108.3 . . ? S3 C14 H14A 108.3 . . ? C15A C14 H14B 139.0 . . ? C15 C14 H14B 108.3 . . ? S3 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C15A C14 H14C 109.1 . . ? C15 C14 H14C 134.7 . . ? S3 C14 H14C 109.1 . . ? H14A C14 H14C 59.0 . . ? H14B C14 H14C 50.5 . . ? C15A C14 H14D 109.1 . . ? C15 C14 H14D 53.5 . . ? S3 C14 H14D 109.1 . . ? H14A C14 H14D 142.6 . . ? H14B C14 H14D 60.3 . . ? H14C C14 H14D 107.9 . . ? C16 C15 C14 113.2(9) . . ? C16 C15 H15A 108.9 . . ? C14 C15 H15A 108.9 . . ? C16 C15 H15B 108.9 . . ? C14 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C15A C16A 117.6(11) . . ? C14 C15A H15C 107.9 . . ? C16A C15A H15C 107.9 . . ? C14 C15A H15D 107.9 . . ? C16A C15A H15D 107.9 . . ? H15C C15A H15D 107.2 . . ? C15A C16A H16D 109.5 . . ? C15A C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? C15A C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.549 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.142 #=== END data_FO3728 _database_code_depnum_ccdc_archive 'CCDC 767205' #TrackingRef 'dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H32 Cl2 Ru S4' _chemical_formula_sum 'C16 H32 Cl2 Ru S4' _chemical_formula_weight 524.63 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 4/m' _symmetry_space_group_name_Hall '-I 4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 9.9415(5) _cell_length_b 9.9415(5) _cell_length_c 10.8281(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1070.18(9) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 5222 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 1.369 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5228 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.45 _reflns_number_total 654 _reflns_number_gt 606 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0089(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 654 _refine_ls_number_parameters 41 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0616 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 2.376 _refine_ls_restrained_S_all 2.376 _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 Ru1 Ru 0.0000 0.0000 0.0000 0.0151(2) Uani 1 8 d S . . Cl1 Cl 0.0000 0.0000 0.22270(9) 0.0228(3) Uani 1 4 d S . . S1 S -0.01120(7) 0.23674(7) 0.0000 0.0233(2) Uani 1 2 d S . . C1 C -0.1185(3) 0.3037(3) -0.1230(2) 0.0385(7) Uani 1 1 d . . . H1A H -0.0629 0.3396 -0.1913 0.046 Uiso 0.54(2) 1 calc PR A 1 H1B H -0.1776 0.2321 -0.1562 0.046 Uiso 0.54(2) 1 calc PR A 1 H1C H -0.0717 0.3762 -0.1686 0.046 Uiso 0.46(2) 1 calc PR A 2 H1D H -0.1437 0.2318 -0.1819 0.046 Uiso 0.46(2) 1 calc PR A 2 C2 C -0.1997(13) 0.4120(12) -0.0669(6) 0.038(2) Uani 0.54(2) 1 d P . 1 H2A H -0.2936 0.4034 -0.0962 0.045 Uiso 0.54(2) 1 calc PR A 1 H2B H -0.1650 0.4998 -0.0962 0.045 Uiso 0.54(2) 1 calc PR A 1 C2A C -0.2430(10) 0.3585(15) -0.0568(8) 0.038(2) Uani 0.46(2) 1 d P . 2 H2AA H -0.2570 0.4523 -0.0848 0.045 Uiso 0.46(2) 1 calc PR A 2 H2AB H -0.3217 0.3057 -0.0848 0.045 Uiso 0.46(2) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0149(2) 0.0149(2) 0.0155(3) 0.000 0.000 0.000 Cl1 0.0258(4) 0.0258(4) 0.0166(6) 0.000 0.000 0.000 S1 0.0188(4) 0.0164(4) 0.0346(5) 0.000 0.000 0.0009(3) C1 0.0595(18) 0.0293(14) 0.0268(14) 0.0073(10) -0.0018(11) 0.0165(12) C2 0.041(5) 0.028(4) 0.044(3) 0.001(3) -0.006(3) 0.019(3) C2A 0.027(4) 0.031(6) 0.055(4) 0.004(3) -0.017(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 S1 2.3562(7) . ? Ru1 S1 2.3562(7) 10 ? Ru1 S1 2.3562(7) 9 ? Ru1 S1 2.3562(7) 2 ? Ru1 Cl1 2.4114(10) 9 ? Ru1 Cl1 2.4114(10) . ? S1 C1 1.831(2) . ? S1 C1 1.831(2) 11 ? C1 C2 1.477(7) . ? C1 C2A 1.531(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 C2 1.450(12) 11 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2A C2A 1.231(18) 11 ? C2A H2AA 0.9900 . ? C2A H2AB 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 S1 Ru1 S1 90.0 . 10 ? S1 Ru1 S1 180.0 . 9 ? S1 Ru1 S1 90.0 10 9 ? S1 Ru1 S1 90.0 . 2 ? S1 Ru1 S1 180.0 10 2 ? S1 Ru1 S1 90.0 9 2 ? S1 Ru1 Cl1 90.0 . 9 ? S1 Ru1 Cl1 90.0 10 9 ? S1 Ru1 Cl1 90.0 9 9 ? S1 Ru1 Cl1 90.0 2 9 ? S1 Ru1 Cl1 90.0 . . ? S1 Ru1 Cl1 90.0 10 . ? S1 Ru1 Cl1 90.0 9 . ? S1 Ru1 Cl1 90.0 2 . ? Cl1 Ru1 Cl1 180.0 9 . ? C1 S1 C1 93.30(16) . 11 ? C1 S1 Ru1 112.98(9) . . ? C1 S1 Ru1 112.98(9) 11 . ? C2 C1 C2A 26.6(3) . . ? C2 C1 S1 106.5(3) . . ? C2A C1 S1 105.1(4) . . ? C2 C1 H1A 110.4 . . ? C2A C1 H1A 132.3 . . ? S1 C1 H1A 110.4 . . ? C2 C1 H1B 110.4 . . ? C2A C1 H1B 86.9 . . ? S1 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? C2 C1 H1C 86.0 . . ? C2A C1 H1C 110.7 . . ? S1 C1 H1C 110.7 . . ? H1A C1 H1C 26.1 . . ? H1B C1 H1C 128.3 . . ? C2 C1 H1D 130.7 . . ? C2A C1 H1D 110.7 . . ? S1 C1 H1D 110.7 . . ? H1A C1 H1D 85.5 . . ? H1B C1 H1D 25.5 . . ? H1C C1 H1D 108.8 . . ? C1 C2 C2 114.3(3) . 11 ? C1 C2 H2A 108.7 . . ? C2 C2 H2A 108.7 11 . ? C1 C2 H2B 108.7 . . ? C2 C2 H2B 108.7 11 . ? H2A C2 H2B 107.6 . . ? C2A C2A C1 117.9(3) 11 . ? C2A C2A H2AA 107.8 11 . ? C1 C2A H2AA 107.8 . . ? C2A C2A H2AB 107.8 11 . ? C1 C2A H2AB 107.8 . . ? H2AA C2A H2AB 107.2 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.566 _refine_diff_density_min -1.283 _refine_diff_density_rms 0.244 #=== END data_FO3973 _database_code_depnum_ccdc_archive 'CCDC 767206' #TrackingRef 'dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H32 Cl4 O2 Ru2 S4, 2(C H Cl3)' _chemical_formula_sum 'C20 H34 Cl10 O2 Ru2 S4' _chemical_formula_weight 991.35 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' O O 0.0106 0.0060 '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' Ru Ru -1.2594 0.8363 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8206(6) _cell_length_b 9.4353(7) _cell_length_c 11.1979(7) _cell_angle_alpha 75.907(4) _cell_angle_beta 85.203(4) _cell_angle_gamma 73.196(4) _cell_volume 865.21(10) _cell_formula_units_Z 1 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 6032 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 27.46 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.903 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 1.908 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6032 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3902 _reflns_number_gt 3179 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0383P)^2^+0.4187P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3902 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Ru1 Ru 0.57200(3) 0.56813(3) 0.61401(2) 0.01366(9) Uani 1 1 d . . . Cl1 Cl 0.34661(10) 0.53017(10) 0.74614(7) 0.02252(19) Uani 1 1 d . . . Cl2 Cl 0.51689(10) 0.81984(9) 0.64609(7) 0.02012(18) Uani 1 1 d . . . S1 S 0.59689(9) 0.33807(9) 0.55891(7) 0.01427(17) Uani 1 1 d . . . S2 S 0.72312(10) 0.44099(9) 0.79431(7) 0.01870(18) Uani 1 1 d . . . O1 O 0.8484(3) 0.6353(3) 0.4647(2) 0.0291(6) Uani 1 1 d . . . C1 C 0.5527(4) 0.1841(4) 0.6779(3) 0.0196(7) Uani 1 1 d . . . H1A H 0.4988 0.2227 0.7495 0.024 Uiso 1 1 calc R . . H1B H 0.4837 0.1365 0.6453 0.024 Uiso 1 1 calc R . . C2 C 0.7120(4) 0.0708(4) 0.7142(3) 0.0222(7) Uani 1 1 d . . . H2A H 0.6987 -0.0303 0.7558 0.027 Uiso 1 1 calc R . . H2B H 0.7666 0.1054 0.7707 0.027 Uiso 1 1 calc R . . C3 C 0.8063(4) 0.0630(4) 0.5949(3) 0.0240(8) Uani 1 1 d . . . H3A H 0.7601 0.0145 0.5436 0.029 Uiso 1 1 calc R . . H3B H 0.9176 0.0030 0.6123 0.029 Uiso 1 1 calc R . . C4 C 0.7980(4) 0.2263(4) 0.5288(3) 0.0198(7) Uani 1 1 d . . . H4A H 0.8172 0.2348 0.4392 0.024 Uiso 1 1 calc R . . H4B H 0.8778 0.2619 0.5614 0.024 Uiso 1 1 calc R . . C5 C 0.6638(4) 0.5582(4) 0.9082(3) 0.0218(7) Uani 1 1 d . . . H5A H 0.5646 0.6393 0.8829 0.026 Uiso 1 1 calc R . . H5B H 0.6454 0.4948 0.9896 0.026 Uiso 1 1 calc R . . C6 C 0.7984(4) 0.6285(4) 0.9158(3) 0.0245(8) Uani 1 1 d . . . H6A H 0.7541 0.7352 0.9232 0.029 Uiso 1 1 calc R . . H6B H 0.8636 0.5708 0.9890 0.029 Uiso 1 1 calc R . . C7 C 0.9002(4) 0.6231(4) 0.7988(3) 0.0252(8) Uani 1 1 d . . . H7A H 0.8471 0.7039 0.7287 0.030 Uiso 1 1 calc R . . H7B H 1.0045 0.6371 0.8106 0.030 Uiso 1 1 calc R . . C8 C 0.9199(4) 0.4692(4) 0.7754(3) 0.0226(7) Uani 1 1 d . . . H8A H 0.9939 0.3898 0.8350 0.027 Uiso 1 1 calc R . . H8B H 0.9615 0.4654 0.6910 0.027 Uiso 1 1 calc R . . C9 C 0.7460(4) 0.6065(3) 0.5163(3) 0.0197(7) Uani 1 1 d . . . Cl1C Cl 0.84220(12) -0.08345(11) 1.24630(10) 0.0400(3) Uani 1 1 d . . . Cl2C Cl 0.63782(12) 0.08012(13) 1.03975(9) 0.0388(2) Uani 1 1 d . . . Cl3C Cl 0.92402(11) 0.16066(11) 1.06596(9) 0.0344(2) Uani 1 1 d . . . C1C C 0.7681(4) 0.0946(4) 1.1444(3) 0.0250(8) Uani 1 1 d . . . H1CA H 0.7079 0.1690 1.1935 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 Ru1 0.01460(14) 0.01493(14) 0.01218(14) -0.00335(10) -0.00101(10) -0.00481(10) Cl1 0.0217(4) 0.0258(4) 0.0198(4) -0.0047(3) 0.0009(3) -0.0071(4) Cl2 0.0242(4) 0.0168(4) 0.0213(4) -0.0079(3) -0.0005(3) -0.0058(3) S1 0.0153(4) 0.0142(4) 0.0134(4) -0.0031(3) -0.0009(3) -0.0042(3) S2 0.0211(4) 0.0198(4) 0.0152(4) -0.0024(3) -0.0048(3) -0.0058(3) O1 0.0295(14) 0.0300(14) 0.0231(13) -0.0029(11) 0.0000(11) -0.0038(12) C1 0.0232(17) 0.0148(16) 0.0196(16) -0.0006(13) 0.0021(14) -0.0067(14) C2 0.0276(19) 0.0168(17) 0.0212(17) -0.0016(14) -0.0070(15) -0.0050(15) C3 0.0228(18) 0.0178(17) 0.0286(19) -0.0049(15) -0.0059(15) 0.0002(15) C4 0.0147(16) 0.0202(17) 0.0217(17) -0.0070(14) -0.0030(13) 0.0021(14) C5 0.0211(17) 0.0285(19) 0.0161(16) -0.0078(14) 0.0010(13) -0.0055(15) C6 0.0254(19) 0.030(2) 0.0222(17) -0.0124(15) -0.0030(15) -0.0077(16) C7 0.0182(17) 0.0295(19) 0.0288(19) -0.0055(16) -0.0036(15) -0.0081(15) C8 0.0166(16) 0.033(2) 0.0177(16) -0.0074(15) -0.0017(13) -0.0039(15) C9 0.0202(17) 0.0097(15) 0.0280(18) -0.0006(14) -0.0163(15) -0.0008(14) Cl1C 0.0342(5) 0.0309(5) 0.0440(6) 0.0076(4) -0.0024(4) -0.0053(4) Cl2C 0.0344(5) 0.0546(7) 0.0333(5) -0.0144(5) -0.0036(4) -0.0173(5) Cl3C 0.0335(5) 0.0333(5) 0.0386(5) -0.0064(4) 0.0045(4) -0.0157(4) C1C 0.0249(18) 0.0256(19) 0.0233(18) -0.0053(15) -0.0016(15) -0.0049(16) _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 Ru1 C9 1.879(4) . ? Ru1 S1 2.3441(8) . ? Ru1 S2 2.3745(8) . ? Ru1 S1 2.3744(8) 2_666 ? Ru1 Cl2 2.3926(8) . ? Ru1 Cl1 2.4355(8) . ? S1 C1 1.826(3) . ? S1 C4 1.834(3) . ? S1 Ru1 2.3744(8) 2_666 ? S2 C8 1.818(3) . ? S2 C5 1.834(3) . ? O1 C9 1.097(4) . ? C1 C2 1.516(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.519(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.522(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.536(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.528(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.496(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? Cl1C C1C 1.763(4) . ? Cl2C C1C 1.763(4) . ? Cl3C C1C 1.754(3) . ? C1C H1CA 1.0000 . ? 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 C9 Ru1 S1 93.77(10) . . ? C9 Ru1 S2 94.56(10) . . ? S1 Ru1 S2 91.85(3) . . ? C9 Ru1 S1 91.67(10) . 2_666 ? S1 Ru1 S1 81.01(3) . 2_666 ? S2 Ru1 S1 170.83(3) . 2_666 ? C9 Ru1 Cl2 87.28(10) . . ? S1 Ru1 Cl2 171.23(3) . . ? S2 Ru1 Cl2 96.75(3) . . ? S1 Ru1 Cl2 90.25(3) 2_666 . ? C9 Ru1 Cl1 176.71(10) . . ? S1 Ru1 Cl1 89.45(3) . . ? S2 Ru1 Cl1 84.65(3) . . ? S1 Ru1 Cl1 89.50(3) 2_666 . ? Cl2 Ru1 Cl1 89.64(3) . . ? C1 S1 C4 94.28(15) . . ? C1 S1 Ru1 117.20(12) . . ? C4 S1 Ru1 116.91(11) . . ? C1 S1 Ru1 115.83(11) . 2_666 ? C4 S1 Ru1 114.91(11) . 2_666 ? Ru1 S1 Ru1 98.99(3) . 2_666 ? C8 S2 C5 92.58(15) . . ? C8 S2 Ru1 110.75(11) . . ? C5 S2 Ru1 108.52(12) . . ? C2 C1 S1 105.3(2) . . ? C2 C1 H1A 110.7 . . ? S1 C1 H1A 110.7 . . ? C2 C1 H1B 110.7 . . ? S1 C1 H1B 110.7 . . ? H1A C1 H1B 108.8 . . ? C1 C2 C3 105.8(3) . . ? C1 C2 H2A 110.6 . . ? C3 C2 H2A 110.6 . . ? C1 C2 H2B 110.6 . . ? C3 C2 H2B 110.6 . . ? H2A C2 H2B 108.7 . . ? C2 C3 C4 106.5(3) . . ? C2 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? C2 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? C3 C4 S1 105.3(2) . . ? C3 C4 H4A 110.7 . . ? S1 C4 H4A 110.7 . . ? C3 C4 H4B 110.7 . . ? S1 C4 H4B 110.7 . . ? H4A C4 H4B 108.8 . . ? C6 C5 S2 107.6(2) . . ? C6 C5 H5A 110.2 . . ? S2 C5 H5A 110.2 . . ? C6 C5 H5B 110.2 . . ? S2 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? C7 C6 C5 108.4(3) . . ? C7 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? C7 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C8 C7 C6 105.8(3) . . ? C8 C7 H7A 110.6 . . ? C6 C7 H7A 110.6 . . ? C8 C7 H7B 110.6 . . ? C6 C7 H7B 110.6 . . ? H7A C7 H7B 108.7 . . ? C7 C8 S2 105.5(2) . . ? C7 C8 H8A 110.6 . . ? S2 C8 H8A 110.6 . . ? C7 C8 H8B 110.6 . . ? S2 C8 H8B 110.6 . . ? H8A C8 H8B 108.8 . . ? O1 C9 Ru1 174.9(3) . . ? Cl3C C1C Cl2C 110.75(19) . . ? Cl3C C1C Cl1C 110.55(19) . . ? Cl2C C1C Cl1C 109.91(19) . . ? Cl3C C1C H1CA 108.5 . . ? Cl2C C1C H1CA 108.5 . . ? Cl1C C1C H1CA 108.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.668 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.121