data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'fac-tris(dimethylsulfoxide,S)-chloro-(eta2-malonato,O,O')-ruthenium(II) potassium(I) dihydrated' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H20 Cl O7 Ru S3 1-, K 1+, 2(H2 O)' _chemical_formula_sum 'C9 H24 Cl K O9 Ru S3' _chemical_formula_weight 548.08 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' 'K' 'K' 0.2009 0.2494 '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 n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.930(3) _cell_length_b 8.369(3) _cell_length_c 13.229(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.67(2) _cell_angle_gamma 90.00 _cell_volume 988.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'yellow' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 1.492 _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 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12195 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 30.55 _reflns_number_total 5007 _reflns_number_gt 4777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0623P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0183(16) _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 0.01(3) _refine_ls_number_reflns 5007 _refine_ls_number_parameters 230 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.077 _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 Ru Ru 0.329510(18) 0.42470(3) 0.597682(17) 0.02947(8) Uani 1 1 d . . . Cl1 Cl 0.08917(13) 0.54381(17) 0.63646(11) 0.0515(3) Uani 1 1 d . . . S1 S 0.54770(11) 0.29594(11) 0.57009(8) 0.03527(19) Uani 1 1 d . . . S2 S 0.43354(12) 0.56569(12) 0.72618(8) 0.0356(2) Uani 1 1 d . . . S3 S 0.38460(12) 0.61678(12) 0.48521(8) 0.0360(2) Uani 1 1 d . . . O1 O 0.6759(4) 0.3858(4) 0.5289(3) 0.0470(7) Uani 1 1 d . . . O2 O 0.5979(4) 0.5681(4) 0.7340(3) 0.0467(8) Uani 1 1 d . . . O3 O 0.5093(4) 0.7283(5) 0.5084(3) 0.0537(9) Uani 1 1 d . . . C1 C 0.6122(7) 0.1986(7) 0.6817(5) 0.0568(13) Uani 1 1 d . . . H1A H 0.6314 0.2767 0.7334 0.085 Uiso 1 1 calc R . . H1B H 0.7029 0.1415 0.6676 0.085 Uiso 1 1 calc R . . H1C H 0.5373 0.1250 0.7043 0.085 Uiso 1 1 calc R . . C2 C 0.5255(7) 0.1286(8) 0.4882(6) 0.0631(16) Uani 1 1 d . . . H2A H 0.4897 0.1642 0.4233 0.095 Uiso 1 1 calc R . . H2B H 0.4548 0.0553 0.5166 0.095 Uiso 1 1 calc R . . H2C H 0.6203 0.0759 0.4806 0.095 Uiso 1 1 calc R . . C3 C 0.3673(8) 0.4938(7) 0.8444(4) 0.0552(12) Uani 1 1 d . . . H3A H 0.3916 0.3826 0.8513 0.083 Uiso 1 1 calc R . . H3B H 0.2606 0.5073 0.8472 0.083 Uiso 1 1 calc R . . H3C H 0.4139 0.5530 0.8984 0.083 Uiso 1 1 calc R . . C4 C 0.3722(9) 0.7675(7) 0.7345(5) 0.0627(16) Uani 1 1 d . . . H4A H 0.4009 0.8242 0.6747 0.094 Uiso 1 1 calc R . . H4B H 0.4176 0.8171 0.7927 0.094 Uiso 1 1 calc R . . H4C H 0.2653 0.7700 0.7406 0.094 Uiso 1 1 calc R . . C5 C 0.2297(7) 0.7394(7) 0.4533(5) 0.0560(13) Uani 1 1 d . . . H5A H 0.1970 0.7954 0.5124 0.084 Uiso 1 1 calc R . . H5B H 0.1494 0.6743 0.4276 0.084 Uiso 1 1 calc R . . H5C H 0.2586 0.8151 0.4027 0.084 Uiso 1 1 calc R . . C6 C 0.4175(7) 0.5337(7) 0.3632(4) 0.0517(11) Uani 1 1 d . . . H6A H 0.5009 0.4615 0.3670 0.077 Uiso 1 1 calc R . . H6B H 0.4394 0.6180 0.3164 0.077 Uiso 1 1 calc R . . H6C H 0.3300 0.4769 0.3405 0.077 Uiso 1 1 calc R . . O4 O 0.1149(5) 0.0649(5) 0.7597(3) 0.0550(10) Uani 1 1 d . . . O5 O 0.2730(4) 0.2368(4) 0.6957(2) 0.0410(6) Uani 1 1 d . . . O6 O 0.2302(4) 0.2892(4) 0.4816(2) 0.0407(6) Uani 1 1 d . . . O7 O 0.0991(5) 0.0901(4) 0.4189(3) 0.0478(8) Uani 1 1 d . . . C7 C 0.1546(5) 0.1520(5) 0.6889(4) 0.0381(8) Uani 1 1 d . . . C8 C 0.0595(5) 0.1528(6) 0.5928(4) 0.0447(10) Uani 1 1 d . . . H8A H 0.0070 0.0514 0.5893 0.054 Uiso 1 1 calc R . . H8B H -0.0158 0.2353 0.6002 0.054 Uiso 1 1 calc R . . C9 C 0.1339(5) 0.1785(5) 0.4921(3) 0.0377(8) Uani 1 1 d . . . K1 K 0.78176(11) 0.68783(12) 0.58862(9) 0.0441(2) Uani 1 1 d . . . O1W O 0.8311(6) 0.8906(7) 0.7462(4) 0.0604(10) Uani 1 1 d D . . H10 H 0.809(9) 0.869(11) 0.807(3) 0.086 Uiso 1 1 d D . . H11 H 0.923(4) 0.922(10) 0.743(6) 0.086 Uiso 1 1 d D . . O2W O 0.8412(6) 0.8921(6) 0.4320(4) 0.0576(10) Uani 1 1 d D . . H20 H 0.781(9) 0.913(8) 0.385(6) 0.086 Uiso 1 1 d D . . H21 H 0.908(8) 0.961(8) 0.441(7) 0.086 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.02619(12) 0.03107(12) 0.03106(13) 0.00095(10) -0.00321(9) -0.00125(10) Cl1 0.0336(5) 0.0625(7) 0.0584(7) 0.0017(5) 0.0004(5) 0.0093(4) S1 0.0317(4) 0.0324(4) 0.0417(5) -0.0019(3) -0.0020(4) 0.0014(3) S2 0.0336(5) 0.0402(5) 0.0329(4) -0.0055(3) -0.0041(4) 0.0001(3) S3 0.0338(4) 0.0371(4) 0.0368(5) 0.0064(3) -0.0065(4) -0.0044(3) O1 0.0345(15) 0.0481(16) 0.059(2) 0.0015(15) 0.0056(15) 0.0001(12) O2 0.0308(15) 0.064(2) 0.0454(18) -0.0069(13) -0.0062(14) -0.0082(12) O3 0.052(2) 0.0464(18) 0.062(2) 0.0133(15) -0.0198(18) -0.0200(15) C1 0.046(3) 0.059(3) 0.065(3) 0.018(2) -0.008(2) 0.012(2) C2 0.055(3) 0.050(3) 0.084(4) -0.024(3) -0.007(3) 0.006(2) C3 0.065(3) 0.064(3) 0.036(2) -0.0007(19) 0.000(2) -0.009(2) C4 0.080(4) 0.044(3) 0.063(3) -0.016(2) -0.022(3) 0.013(3) C5 0.053(3) 0.051(3) 0.064(3) 0.016(2) -0.013(3) 0.011(2) C6 0.058(3) 0.063(3) 0.0340(19) 0.0028(19) 0.005(2) -0.006(2) O4 0.056(2) 0.061(2) 0.048(2) 0.0163(15) -0.0019(19) -0.0221(17) O5 0.0377(14) 0.0478(17) 0.0374(15) 0.0084(11) -0.0043(12) -0.0103(12) O6 0.0393(15) 0.0473(17) 0.0355(14) 0.0013(11) -0.0033(12) -0.0122(12) O7 0.055(2) 0.0444(17) 0.0433(17) -0.0027(12) -0.0059(17) -0.0128(13) C7 0.0320(18) 0.043(2) 0.039(2) 0.0030(15) 0.0048(16) -0.0057(15) C8 0.038(2) 0.050(2) 0.046(2) 0.0048(17) -0.006(2) -0.0127(17) C9 0.0356(18) 0.0384(19) 0.0389(19) 0.0009(14) -0.0113(16) -0.0040(14) K1 0.0334(4) 0.0461(5) 0.0526(5) 0.0034(4) -0.0028(4) -0.0034(3) O1W 0.054(2) 0.069(2) 0.058(2) -0.003(2) -0.003(2) -0.011(2) O2W 0.064(3) 0.059(2) 0.050(2) 0.0081(17) -0.005(2) -0.016(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 Ru O6 2.097(3) . ? Ru O5 2.103(3) . ? Ru S3 2.2487(11) . ? Ru S1 2.2599(12) . ? Ru S2 2.2601(11) . ? Ru Cl1 2.4267(14) . ? Cl1 K1 3.0576(17) 1_455 ? S3 O3 1.483(3) . ? S3 C5 1.770(5) . ? S3 C6 1.785(5) . ? S2 O2 1.471(4) . ? S2 C4 1.779(5) . ? S2 C3 1.783(5) . ? S2 K1 3.7626(19) . ? S1 O1 1.479(4) . ? S1 C1 1.776(6) . ? S1 C2 1.780(6) . ? O3 K1 2.665(4) . ? O2 K1 2.734(4) . ? O1 K1 2.809(4) . ? O5 C7 1.276(5) . ? O6 C9 1.273(5) . ? O7 C9 1.255(5) . ? O4 C7 1.242(5) . ? C7 C8 1.520(6) . ? C8 C9 1.510(7) . ? K1 O1W 2.720(5) . ? K1 O2W 2.742(5) . ? K1 Cl1 3.0576(17) 1_655 ? 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 O6 Ru O5 86.82(12) . . ? O6 Ru S3 89.77(9) . . ? O5 Ru S3 176.59(10) . . ? O6 Ru S1 88.96(11) . . ? O5 Ru S1 87.51(11) . . ? S3 Ru S1 92.20(5) . . ? O6 Ru S2 178.29(9) . . ? O5 Ru S2 91.50(9) . . ? S3 Ru S2 91.90(5) . . ? S1 Ru S2 91.31(4) . . ? O6 Ru Cl1 90.54(11) . . ? O5 Ru Cl1 87.58(11) . . ? S3 Ru Cl1 92.70(5) . . ? S1 Ru Cl1 175.08(4) . . ? S2 Ru Cl1 89.05(5) . . ? Ru Cl1 K1 155.83(7) . 1_455 ? O3 S3 C5 105.5(3) . . ? O3 S3 C6 107.5(3) . . ? C5 S3 C6 98.5(3) . . ? O3 S3 Ru 118.88(16) . . ? C5 S3 Ru 113.3(2) . . ? C6 S3 Ru 111.07(19) . . ? O2 S2 C4 106.9(3) . . ? O2 S2 C3 106.5(3) . . ? C4 S2 C3 99.2(3) . . ? O2 S2 Ru 117.49(16) . . ? C4 S2 Ru 114.7(2) . . ? C3 S2 Ru 110.24(19) . . ? O2 S2 K1 36.92(16) . . ? C4 S2 K1 91.6(3) . . ? C3 S2 K1 143.2(2) . . ? Ru S2 K1 96.48(4) . . ? O1 S1 C1 107.1(3) . . ? O1 S1 C2 104.9(3) . . ? C1 S1 C2 100.2(4) . . ? O1 S1 Ru 119.29(15) . . ? C1 S1 Ru 110.9(2) . . ? C2 S1 Ru 112.6(2) . . ? S3 O3 K1 133.0(2) . . ? S2 O2 K1 124.2(2) . . ? S1 O1 K1 127.9(2) . . ? C7 O5 Ru 125.2(3) . . ? C9 O6 Ru 126.5(3) . . ? O4 C7 O5 121.1(4) . . ? O4 C7 C8 118.1(4) . . ? O5 C7 C8 120.7(4) . . ? C9 C8 C7 119.4(4) . . ? O7 C9 O6 120.4(4) . . ? O7 C9 C8 119.3(4) . . ? O6 C9 C8 120.3(4) . . ? O3 K1 O1W 111.41(16) . . ? O3 K1 O2 76.94(12) . . ? O1W K1 O2 77.45(14) . . ? O3 K1 O2W 78.67(14) . . ? O1W K1 O2W 99.14(14) . . ? O2 K1 O2W 152.02(15) . . ? O3 K1 O1 72.52(12) . . ? O1W K1 O1 145.89(14) . . ? O2 K1 O1 70.43(11) . . ? O2W K1 O1 114.59(13) . . ? O3 K1 Cl1 161.08(11) . 1_655 ? O1W K1 Cl1 87.14(12) . 1_655 ? O2 K1 Cl1 104.77(9) . 1_655 ? O2W K1 Cl1 102.77(13) . 1_655 ? O1 K1 Cl1 90.12(9) . 1_655 ? O3 K1 S2 58.08(9) . . ? O1W K1 S2 85.78(12) . . ? O2 K1 S2 18.86(8) . . ? O2W K1 S2 134.66(12) . . ? O1 K1 S2 67.30(8) . . ? Cl1 K1 S2 122.54(5) 1_655 . ? 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 O6 Ru Cl1 K1 -39.06(17) . . . 1_455 ? O5 Ru Cl1 K1 -125.86(17) . . . 1_455 ? S3 Ru Cl1 K1 50.74(15) . . . 1_455 ? S1 Ru Cl1 K1 -123.2(5) . . . 1_455 ? S2 Ru Cl1 K1 142.60(15) . . . 1_455 ? O6 Ru S3 O3 -156.7(2) . . . . ? O5 Ru S3 O3 -152.7(18) . . . . ? S1 Ru S3 O3 -67.7(2) . . . . ? S2 Ru S3 O3 23.7(2) . . . . ? Cl1 Ru S3 O3 112.8(2) . . . . ? O6 Ru S3 C5 78.6(3) . . . . ? O5 Ru S3 C5 82.6(18) . . . . ? S1 Ru S3 C5 167.5(2) . . . . ? S2 Ru S3 C5 -101.1(3) . . . . ? Cl1 Ru S3 C5 -12.0(3) . . . . ? O6 Ru S3 C6 -31.2(2) . . . . ? O5 Ru S3 C6 -27.2(18) . . . . ? S1 Ru S3 C6 57.8(2) . . . . ? S2 Ru S3 C6 149.2(2) . . . . ? Cl1 Ru S3 C6 -121.7(2) . . . . ? O6 Ru S2 O2 115(4) . . . . ? O5 Ru S2 O2 103.1(2) . . . . ? S3 Ru S2 O2 -76.68(18) . . . . ? S1 Ru S2 O2 15.56(18) . . . . ? Cl1 Ru S2 O2 -169.35(19) . . . . ? O6 Ru S2 C4 -119(4) . . . . ? O5 Ru S2 C4 -130.1(3) . . . . ? S3 Ru S2 C4 50.2(3) . . . . ? S1 Ru S2 C4 142.4(3) . . . . ? Cl1 Ru S2 C4 -42.5(3) . . . . ? O6 Ru S2 C3 -8(4) . . . . ? O5 Ru S2 C3 -19.1(3) . . . . ? S3 Ru S2 C3 161.1(2) . . . . ? S1 Ru S2 C3 -106.6(2) . . . . ? Cl1 Ru S2 C3 68.5(2) . . . . ? O6 Ru S2 K1 147(4) . . . . ? O5 Ru S2 K1 135.12(10) . . . . ? S3 Ru S2 K1 -44.66(4) . . . . ? S1 Ru S2 K1 47.58(4) . . . . ? Cl1 Ru S2 K1 -137.33(4) . . . . ? O6 Ru S1 O1 112.7(2) . . . . ? O5 Ru S1 O1 -160.4(2) . . . . ? S3 Ru S1 O1 23.0(2) . . . . ? S2 Ru S1 O1 -69.0(2) . . . . ? Cl1 Ru S1 O1 -163.0(5) . . . . ? O6 Ru S1 C1 -122.2(2) . . . . ? O5 Ru S1 C1 -35.3(2) . . . . ? S3 Ru S1 C1 148.1(2) . . . . ? S2 Ru S1 C1 56.2(2) . . . . ? Cl1 Ru S1 C1 -37.9(6) . . . . ? O6 Ru S1 C2 -10.8(3) . . . . ? O5 Ru S1 C2 76.1(3) . . . . ? S3 Ru S1 C2 -100.5(3) . . . . ? S2 Ru S1 C2 167.5(3) . . . . ? Cl1 Ru S1 C2 73.4(6) . . . . ? C5 S3 O3 K1 170.1(3) . . . . ? C6 S3 O3 K1 -85.5(4) . . . . ? Ru S3 O3 K1 41.7(4) . . . . ? C4 S2 O2 K1 -69.3(3) . . . . ? C3 S2 O2 K1 -174.6(3) . . . . ? Ru S2 O2 K1 61.3(2) . . . . ? C1 S1 O1 K1 -81.9(3) . . . . ? C2 S1 O1 K1 172.2(3) . . . . ? Ru S1 O1 K1 45.0(3) . . . . ? O6 Ru O5 C7 -35.5(4) . . . . ? S3 Ru O5 C7 -40(2) . . . . ? S1 Ru O5 C7 -124.6(4) . . . . ? S2 Ru O5 C7 144.1(4) . . . . ? Cl1 Ru O5 C7 55.2(4) . . . . ? O5 Ru O6 C9 21.8(4) . . . . ? S3 Ru O6 C9 -158.5(4) . . . . ? S1 Ru O6 C9 109.3(4) . . . . ? S2 Ru O6 C9 10(4) . . . . ? Cl1 Ru O6 C9 -65.8(4) . . . . ? Ru O5 C7 O4 -165.9(4) . . . . ? Ru O5 C7 C8 15.1(6) . . . . ? O4 C7 C8 C9 -147.8(5) . . . . ? O5 C7 C8 C9 31.3(7) . . . . ? Ru O6 C9 O7 -169.4(3) . . . . ? Ru O6 C9 C8 11.0(6) . . . . ? C7 C8 C9 O7 134.6(5) . . . . ? C7 C8 C9 O6 -45.8(6) . . . . ? S3 O3 K1 O1W -127.8(3) . . . . ? S3 O3 K1 O2 -57.1(3) . . . . ? S3 O3 K1 O2W 136.7(4) . . . . ? S3 O3 K1 O1 16.2(3) . . . . ? S3 O3 K1 Cl1 40.4(6) . . . 1_655 ? S3 O3 K1 S2 -57.5(3) . . . . ? S2 O2 K1 O3 -1.1(2) . . . . ? S2 O2 K1 O1W 114.7(3) . . . . ? S2 O2 K1 O2W 28.9(4) . . . . ? S2 O2 K1 O1 -76.9(2) . . . . ? S2 O2 K1 Cl1 -161.7(2) . . . 1_655 ? S1 O1 K1 O3 -65.6(3) . . . . ? S1 O1 K1 O1W 37.0(4) . . . . ? S1 O1 K1 O2 16.4(3) . . . . ? S1 O1 K1 O2W -133.8(3) . . . . ? S1 O1 K1 Cl1 122.0(3) . . . 1_655 ? S1 O1 K1 S2 -3.6(2) . . . . ? O2 S2 K1 O3 178.8(3) . . . . ? C4 S2 K1 O3 -64.8(2) . . . . ? C3 S2 K1 O3 -172.6(4) . . . . ? Ru S2 K1 O3 50.29(11) . . . . ? O2 S2 K1 O1W -62.7(3) . . . . ? C4 S2 K1 O1W 53.7(2) . . . . ? C3 S2 K1 O1W -54.1(4) . . . . ? Ru S2 K1 O1W 168.79(12) . . . . ? C4 S2 K1 O2 116.4(3) . . . . ? C3 S2 K1 O2 8.6(4) . . . . ? Ru S2 K1 O2 -128.5(2) . . . . ? O2 S2 K1 O2W -161.4(3) . . . . ? C4 S2 K1 O2W -45.0(3) . . . . ? C3 S2 K1 O2W -152.8(4) . . . . ? Ru S2 K1 O2W 70.10(16) . . . . ? O2 S2 K1 O1 95.8(3) . . . . ? C4 S2 K1 O1 -147.8(2) . . . . ? C3 S2 K1 O1 104.4(4) . . . . ? Ru S2 K1 O1 -32.65(9) . . . . ? O2 S2 K1 Cl1 21.1(2) . . . 1_655 ? C4 S2 K1 Cl1 137.6(2) . . . 1_655 ? C3 S2 K1 Cl1 29.8(4) . . . 1_655 ? Ru S2 K1 Cl1 -107.32(6) . . . 1_655 ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 30.55 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.687 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.095 #===END data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; fac-tris(dimethylsulfoxide,S)-(dimethylsulfoxide,O)- -(eta2-malonate,O,O')-ruthenium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H26 O8 Ru S4' _chemical_formula_sum 'C11 H26 O8 Ru S4' _chemical_formula_weight 515.63 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' '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' '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' 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 8.992(2) _cell_length_b 13.819(4) _cell_length_c 16.524(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.09(3) _cell_angle_gamma 90.00 _cell_volume 1999.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.234 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5129 _exptl_absorpt_correction_T_max 0.8071 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25413 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4235 _reflns_number_gt 3218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+4.2834P] 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 4235 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1391 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Ru Ru 0.60016(5) 0.22589(3) 0.38043(3) 0.03975(15) Uani 1 1 d . . . S1 S 0.80247(18) 0.28731(12) 0.47049(10) 0.0536(4) Uani 1 1 d . . . S2 S 0.70095(17) 0.07602(10) 0.39386(10) 0.0481(3) Uani 1 1 d . . . S3 S 0.69236(18) 0.26228(11) 0.26733(10) 0.0493(4) Uani 1 1 d . . . S4 S 0.24244(17) 0.20220(12) 0.30312(10) 0.0512(4) Uani 1 1 d . . . O1 O 0.8029(6) 0.2745(4) 0.5598(3) 0.0716(14) Uani 1 1 d . . . O2 O 0.8412(5) 0.0545(3) 0.3645(3) 0.0618(11) Uani 1 1 d . . . O3 O 0.8512(6) 0.2965(4) 0.2784(3) 0.0737(14) Uani 1 1 d . . . O4 O 0.4026(4) 0.1745(3) 0.2935(2) 0.0481(9) Uani 1 1 d . . . C1 C 0.9831(8) 0.2485(6) 0.4596(5) 0.076(2) Uani 1 1 d . . . H1A H 1.0611 0.2809 0.4997 0.114 Uiso 1 1 calc R . . H1B H 0.9949 0.2635 0.4046 0.114 Uiso 1 1 calc R . . H1C H 0.9921 0.1799 0.4683 0.114 Uiso 1 1 calc R . . C2 C 0.8193(10) 0.4153(5) 0.4527(6) 0.083(2) Uani 1 1 d . . . H2A H 0.7267 0.4473 0.4571 0.124 Uiso 1 1 calc R . . H2B H 0.8369 0.4254 0.3982 0.124 Uiso 1 1 calc R . . H2C H 0.9033 0.4412 0.4935 0.124 Uiso 1 1 calc R . . C3 C 0.7335(9) 0.0362(5) 0.4983(5) 0.071(2) Uani 1 1 d . . . H3A H 0.7504 -0.0324 0.5005 0.107 Uiso 1 1 calc R . . H3B H 0.6460 0.0510 0.5203 0.107 Uiso 1 1 calc R . . H3C H 0.8216 0.0685 0.5308 0.107 Uiso 1 1 calc R . . C4 C 0.5605(8) -0.0100(5) 0.3470(5) 0.0659(18) Uani 1 1 d . . . H4A H 0.5422 -0.0045 0.2876 0.099 Uiso 1 1 calc R . . H4B H 0.4674 0.0022 0.3644 0.099 Uiso 1 1 calc R . . H4C H 0.5962 -0.0740 0.3636 0.099 Uiso 1 1 calc R . . C5 C 0.6682(8) 0.1658(5) 0.1937(4) 0.0612(17) Uani 1 1 d . . . H5A H 0.6949 0.1879 0.1437 0.092 Uiso 1 1 calc R . . H5B H 0.5637 0.1449 0.1812 0.092 Uiso 1 1 calc R . . H5C H 0.7331 0.1127 0.2165 0.092 Uiso 1 1 calc R . . C6 C 0.5739(9) 0.3499(5) 0.2054(5) 0.0702(19) Uani 1 1 d . . . H6A H 0.5714 0.4076 0.2375 0.105 Uiso 1 1 calc R . . H6B H 0.4724 0.3246 0.1875 0.105 Uiso 1 1 calc R . . H6C H 0.6140 0.3650 0.1577 0.105 Uiso 1 1 calc R . . C7 C 0.1341(9) 0.0983(6) 0.2692(6) 0.090(3) Uani 1 1 d . . . H7A H 0.1505 0.0787 0.2161 0.136 Uiso 1 1 calc R . . H7B H 0.0278 0.1122 0.2641 0.136 Uiso 1 1 calc R . . H7C H 0.1647 0.0470 0.3087 0.136 Uiso 1 1 calc R . . C8 C 0.1708(9) 0.2831(7) 0.2213(5) 0.083(3) Uani 1 1 d . . . H8A H 0.2231 0.3439 0.2322 0.124 Uiso 1 1 calc R . . H8B H 0.0635 0.2927 0.2169 0.124 Uiso 1 1 calc R . . H8C H 0.1867 0.2567 0.1702 0.124 Uiso 1 1 calc R . . O5 O 0.4831(4) 0.1858(3) 0.4707(2) 0.0468(9) Uani 1 1 d . . . O6 O 0.4832(5) 0.3570(3) 0.3672(3) 0.0529(10) Uani 1 1 d . . . O7 O 0.3276(6) 0.2131(3) 0.5540(3) 0.0630(12) Uani 1 1 d . . . O8 O 0.3178(7) 0.4597(4) 0.3984(4) 0.0904(18) Uani 1 1 d . . . C9 C 0.4108(7) 0.2434(4) 0.5105(4) 0.0476(13) Uani 1 1 d . . . C10 C 0.4331(8) 0.3517(4) 0.5052(4) 0.0573(16) Uani 1 1 d . . . H10A H 0.5369 0.3674 0.5338 0.069 Uiso 1 1 calc R . . H10B H 0.3651 0.3839 0.5345 0.069 Uiso 1 1 calc R . . C11 C 0.4044(8) 0.3927(5) 0.4169(4) 0.0564(15) 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 Ru 0.0367(2) 0.0373(2) 0.0463(3) -0.00089(19) 0.01169(18) -0.00006(17) S1 0.0450(8) 0.0611(10) 0.0541(9) -0.0112(7) 0.0097(7) -0.0068(7) S2 0.0477(8) 0.0424(8) 0.0566(9) 0.0014(6) 0.0169(7) 0.0072(6) S3 0.0442(8) 0.0551(9) 0.0508(8) 0.0035(7) 0.0155(6) -0.0045(6) S4 0.0396(8) 0.0609(9) 0.0535(9) -0.0040(7) 0.0115(6) 0.0002(6) O1 0.059(3) 0.098(4) 0.054(3) -0.009(3) 0.006(2) -0.004(3) O2 0.054(3) 0.061(3) 0.077(3) -0.001(2) 0.028(2) 0.015(2) O3 0.060(3) 0.100(4) 0.064(3) 0.004(3) 0.022(2) -0.020(3) O4 0.0333(19) 0.055(2) 0.057(2) -0.0037(19) 0.0122(17) 0.0006(16) C1 0.041(4) 0.105(6) 0.084(5) -0.018(4) 0.017(4) -0.002(3) C2 0.085(5) 0.054(4) 0.112(7) -0.021(4) 0.027(5) -0.021(4) C3 0.085(5) 0.060(4) 0.071(5) 0.019(4) 0.024(4) 0.017(4) C4 0.067(4) 0.043(4) 0.088(5) -0.003(3) 0.018(4) -0.004(3) C5 0.061(4) 0.073(5) 0.054(4) -0.003(3) 0.023(3) 0.003(3) C6 0.083(5) 0.065(5) 0.064(4) 0.022(3) 0.019(4) 0.002(4) C7 0.054(4) 0.089(6) 0.127(8) -0.023(5) 0.019(5) -0.017(4) C8 0.051(4) 0.126(8) 0.073(5) 0.030(5) 0.015(4) 0.025(4) O5 0.044(2) 0.043(2) 0.057(2) 0.0013(18) 0.0191(18) 0.0045(16) O6 0.059(3) 0.043(2) 0.060(3) 0.0054(18) 0.019(2) 0.0094(18) O7 0.067(3) 0.063(3) 0.068(3) 0.011(2) 0.036(2) 0.011(2) O8 0.113(5) 0.067(3) 0.101(4) 0.020(3) 0.045(3) 0.046(3) C9 0.048(3) 0.048(3) 0.049(3) 0.001(2) 0.014(3) 0.007(2) C10 0.069(4) 0.046(3) 0.064(4) -0.009(3) 0.031(3) 0.001(3) C11 0.063(4) 0.045(3) 0.061(4) 0.000(3) 0.014(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 Ru O6 2.081(4) . ? Ru O5 2.087(4) . ? Ru O4 2.138(4) . ? Ru S1 2.2400(17) . ? Ru S2 2.2513(16) . ? Ru S3 2.2662(16) . ? S4 O4 1.533(4) . ? S4 C7 1.755(8) . ? S4 C8 1.760(7) . ? S2 O2 1.480(4) . ? S2 C3 1.772(7) . ? S2 C4 1.779(7) . ? S3 O3 1.476(5) . ? S3 C6 1.776(7) . ? S3 C5 1.785(7) . ? S1 O1 1.486(5) . ? S1 C1 1.759(7) . ? S1 C2 1.805(8) . ? O5 C9 1.296(7) . ? O6 C11 1.298(7) . ? O7 C9 1.223(7) . ? O8 C11 1.205(8) . ? C9 C10 1.516(8) . ? C10 C11 1.531(9) . ? 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 O6 Ru O5 88.95(15) . . ? O6 Ru O4 84.01(16) . . ? O5 Ru O4 85.13(15) . . ? O6 Ru S1 93.15(13) . . ? O5 Ru S1 95.22(12) . . ? O4 Ru S1 177.13(12) . . ? O6 Ru S2 173.54(13) . . ? O5 Ru S2 86.69(11) . . ? O4 Ru S2 90.87(12) . . ? S1 Ru S2 92.00(6) . . ? O6 Ru S3 89.46(12) . . ? O5 Ru S3 170.70(12) . . ? O4 Ru S3 85.60(11) . . ? S1 Ru S3 94.01(6) . . ? S2 Ru S3 94.08(6) . . ? O4 S4 C7 103.2(3) . . ? O4 S4 C8 105.5(3) . . ? C7 S4 C8 101.2(5) . . ? O2 S2 C3 107.0(3) . . ? O2 S2 C4 107.2(3) . . ? C3 S2 C4 99.3(4) . . ? O2 S2 Ru 120.4(2) . . ? C3 S2 Ru 110.8(3) . . ? C4 S2 Ru 110.0(2) . . ? O3 S3 C6 106.9(3) . . ? O3 S3 C5 106.7(3) . . ? C6 S3 C5 98.8(4) . . ? O3 S3 Ru 119.6(2) . . ? C6 S3 Ru 110.0(3) . . ? C5 S3 Ru 112.7(2) . . ? O1 S1 C1 105.7(4) . . ? O1 S1 C2 107.3(4) . . ? C1 S1 C2 99.7(4) . . ? O1 S1 Ru 115.7(2) . . ? C1 S1 Ru 116.5(3) . . ? C2 S1 Ru 110.4(3) . . ? S4 O4 Ru 120.3(2) . . ? C9 O5 Ru 126.2(4) . . ? C11 O6 Ru 126.8(4) . . ? O7 C9 O5 122.1(6) . . ? O7 C9 C10 118.6(5) . . ? O5 C9 C10 119.3(5) . . ? C9 C10 C11 115.1(5) . . ? O8 C11 O6 123.0(6) . . ? O8 C11 C10 119.1(6) . . ? O6 C11 C10 117.7(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 O6 Ru S2 O2 151.0(11) . . . . ? O5 Ru S2 O2 -161.3(3) . . . . ? O4 Ru S2 O2 113.6(3) . . . . ? S1 Ru S2 O2 -66.2(2) . . . . ? S3 Ru S2 O2 28.0(2) . . . . ? O6 Ru S2 C3 -83.1(11) . . . . ? O5 Ru S2 C3 -35.5(3) . . . . ? O4 Ru S2 C3 -120.5(3) . . . . ? S1 Ru S2 C3 59.7(3) . . . . ? S3 Ru S2 C3 153.8(3) . . . . ? O6 Ru S2 C4 25.6(11) . . . . ? O5 Ru S2 C4 73.3(3) . . . . ? O4 Ru S2 C4 -11.8(3) . . . . ? S1 Ru S2 C4 168.4(3) . . . . ? S3 Ru S2 C4 -97.4(3) . . . . ? O6 Ru S3 O3 102.7(3) . . . . ? O5 Ru S3 O3 -177.2(7) . . . . ? O4 Ru S3 O3 -173.3(3) . . . . ? S1 Ru S3 O3 9.6(3) . . . . ? S2 Ru S3 O3 -82.7(3) . . . . ? O6 Ru S3 C6 -21.5(3) . . . . ? O5 Ru S3 C6 58.6(8) . . . . ? O4 Ru S3 C6 62.5(3) . . . . ? S1 Ru S3 C6 -114.7(3) . . . . ? S2 Ru S3 C6 153.0(3) . . . . ? O6 Ru S3 C5 -130.7(3) . . . . ? O5 Ru S3 C5 -50.5(8) . . . . ? O4 Ru S3 C5 -46.7(3) . . . . ? S1 Ru S3 C5 136.2(3) . . . . ? S2 Ru S3 C5 43.9(3) . . . . ? O6 Ru S1 O1 94.6(3) . . . . ? O5 Ru S1 O1 5.3(3) . . . . ? O4 Ru S1 O1 102(2) . . . . ? S2 Ru S1 O1 -81.5(3) . . . . ? S3 Ru S1 O1 -175.8(3) . . . . ? O6 Ru S1 C1 -140.2(4) . . . . ? O5 Ru S1 C1 130.5(4) . . . . ? O4 Ru S1 C1 -133(2) . . . . ? S2 Ru S1 C1 43.7(4) . . . . ? S3 Ru S1 C1 -50.5(4) . . . . ? O6 Ru S1 C2 -27.5(3) . . . . ? O5 Ru S1 C2 -116.7(3) . . . . ? O4 Ru S1 C2 -20(2) . . . . ? S2 Ru S1 C2 156.4(3) . . . . ? S3 Ru S1 C2 62.2(3) . . . . ? C7 S4 O4 Ru -145.0(4) . . . . ? C8 S4 O4 Ru 109.2(4) . . . . ? O6 Ru O4 S4 -43.9(3) . . . . ? O5 Ru O4 S4 45.5(3) . . . . ? S1 Ru O4 S4 -52(2) . . . . ? S2 Ru O4 S4 132.1(3) . . . . ? S3 Ru O4 S4 -133.9(3) . . . . ? O6 Ru O5 C9 -17.4(5) . . . . ? O4 Ru O5 C9 -101.5(5) . . . . ? S1 Ru O5 C9 75.7(5) . . . . ? S2 Ru O5 C9 167.4(5) . . . . ? S3 Ru O5 C9 -97.6(8) . . . . ? O5 Ru O6 C11 13.8(5) . . . . ? O4 Ru O6 C11 99.0(5) . . . . ? S1 Ru O6 C11 -81.4(5) . . . . ? S2 Ru O6 C11 61.4(13) . . . . ? S3 Ru O6 C11 -175.4(5) . . . . ? Ru O5 C9 O7 169.6(5) . . . . ? Ru O5 C9 C10 -12.1(8) . . . . ? O7 C9 C10 C11 -128.0(6) . . . . ? O5 C9 C10 C11 53.7(8) . . . . ? Ru O6 C11 O8 -166.2(6) . . . . ? Ru O6 C11 C10 18.4(8) . . . . ? C9 C10 C11 O8 127.5(7) . . . . ? C9 C10 C11 O6 -56.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.907 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.100 #===END data_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis[aquo-tris(dimethylsulfoxide,S)-(mu-malonate,O,O')- -ruthenium(II)] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H44 O16 Ru2 S6' _chemical_formula_weight 911.03 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' '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.825(2) _cell_length_b 13.695(4) _cell_length_c 14.235(4) _cell_angle_alpha 85.88(2) _cell_angle_beta 88.71(2) _cell_angle_gamma 81.67(3) _cell_volume 1697.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.323 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4776 _exptl_absorpt_correction_T_max 0.7140 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23240 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 29.62 _reflns_number_total 8687 _reflns_number_gt 5850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.01 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8687 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _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 0.30794(2) 0.222863(16) 0.486931(16) 0.03757(7) Uani 1 1 d . . . O1W O 0.2120(3) 0.16202(18) 0.37111(17) 0.0519(6) Uani 1 1 d . . . H2W H 0.303(4) 0.146(3) 0.339(3) 0.062 Uiso 1 1 d . . . H1W H 0.193(4) 0.107(3) 0.396(3) 0.062 Uiso 1 1 d . . . S1 S 0.43484(9) 0.26229(6) 0.61335(5) 0.04228(16) Uani 1 1 d . . . S2 S 0.07111(8) 0.29268(6) 0.52874(6) 0.04737(18) Uani 1 1 d . . . S3 S 0.34448(9) 0.35831(6) 0.39304(6) 0.04425(17) Uani 1 1 d . . . O11 O 0.5273(3) 0.34422(18) 0.60059(17) 0.0653(7) Uani 1 1 d . . . O12 O 0.0526(3) 0.37978(18) 0.58545(19) 0.0633(7) Uani 1 1 d . . . O13 O 0.2675(3) 0.36875(18) 0.30073(17) 0.0641(7) Uani 1 1 d . . . C1 C 0.5608(4) 0.1556(3) 0.6566(3) 0.0594(9) Uani 1 1 d . . . H1A H 0.6323 0.1343 0.6078 0.089 Uiso 1 1 calc R . . H1B H 0.5024 0.1034 0.6756 0.089 Uiso 1 1 calc R . . H1C H 0.6156 0.1715 0.7096 0.089 Uiso 1 1 calc R . . C2 C 0.3209(4) 0.2814(3) 0.7158(2) 0.0661(10) Uani 1 1 d . . . H2A H 0.3857 0.2830 0.7687 0.099 Uiso 1 1 calc R . . H2B H 0.2610 0.2284 0.7269 0.099 Uiso 1 1 calc R . . H2C H 0.2539 0.3431 0.7074 0.099 Uiso 1 1 calc R . . C3 C -0.0366(4) 0.2057(3) 0.5880(3) 0.0648(10) Uani 1 1 d . . . H3A H 0.0144 0.1785 0.6449 0.097 Uiso 1 1 calc R . . H3B H -0.0452 0.1534 0.5478 0.097 Uiso 1 1 calc R . . H3C H -0.1370 0.2383 0.6031 0.097 Uiso 1 1 calc R . . C4 C -0.0443(4) 0.3258(3) 0.4261(3) 0.0705(11) Uani 1 1 d . . . H4A H -0.1479 0.3480 0.4450 0.106 Uiso 1 1 calc R . . H4B H -0.0418 0.2692 0.3898 0.106 Uiso 1 1 calc R . . H4C H -0.0049 0.3779 0.3887 0.106 Uiso 1 1 calc R . . C5 C 0.5410(4) 0.3648(3) 0.3690(3) 0.0609(9) Uani 1 1 d . . . H5A H 0.5824 0.3119 0.3310 0.091 Uiso 1 1 calc R . . H5B H 0.5956 0.3589 0.4271 0.091 Uiso 1 1 calc R . . H5C H 0.5513 0.4271 0.3358 0.091 Uiso 1 1 calc R . . C6 C 0.2933(4) 0.4719(2) 0.4466(3) 0.0582(9) Uani 1 1 d . . . H6A H 0.3240 0.5249 0.4062 0.087 Uiso 1 1 calc R . . H6B H 0.3440 0.4686 0.5060 0.087 Uiso 1 1 calc R . . H6C H 0.1845 0.4834 0.4566 0.087 Uiso 1 1 calc R . . O1 O 0.4887(3) 0.1055(2) 0.30785(18) 0.0724(7) Uani 1 1 d . . . O2 O 0.5286(2) 0.15320(16) 0.45059(16) 0.0507(5) Uani 1 1 d . . . O3 O 0.7159(2) -0.09368(15) 0.42781(16) 0.0496(5) Uani 1 1 d . . . O4 O 0.8212(3) -0.00361(17) 0.52557(18) 0.0607(6) Uani 1 1 d . . . C7 C 0.5704(4) 0.1123(2) 0.3752(2) 0.0493(7) Uani 1 1 d . . . C8 C 0.7387(4) 0.0675(2) 0.3730(3) 0.0551(8) Uani 1 1 d . . . H8A H 0.7656 0.0416 0.3123 0.066 Uiso 1 1 calc R . . H8B H 0.8028 0.1176 0.3833 0.066 Uiso 1 1 calc R . . C9 C 0.7630(3) -0.0149(2) 0.4503(2) 0.0478(7) Uani 1 1 d . . . Ru2 Ru 0.81472(3) 0.222919(16) 0.987638(16) 0.03811(7) Uani 1 1 d . . . O2W O 0.7513(3) 0.17191(17) 0.85656(16) 0.0483(5) Uani 1 1 d . . . H4W H 0.846(4) 0.159(3) 0.834(3) 0.058 Uiso 1 1 d . . . H3W H 0.720(4) 0.121(3) 0.885(3) 0.058 Uiso 1 1 d . . . S4 S 0.90530(9) 0.25149(6) 1.12995(6) 0.04637(18) Uani 1 1 d . . . S5 S 0.56410(9) 0.27527(6) 1.02098(6) 0.04766(18) Uani 1 1 d . . . S6 S 0.84088(10) 0.37098(6) 0.91484(6) 0.04990(19) Uani 1 1 d . . . O14 O 0.7977(3) 0.2811(2) 1.20669(18) 0.0765(8) Uani 1 1 d . . . O15 O 0.4617(3) 0.2897(2) 0.93771(19) 0.0741(8) Uani 1 1 d . . . O16 O 0.8084(3) 0.46074(16) 0.96792(18) 0.0595(6) Uani 1 1 d . . . C11 C 1.0248(4) 0.1430(3) 1.1742(2) 0.0599(9) Uani 1 1 d . . . H11A H 1.0633 0.1539 1.2346 0.090 Uiso 1 1 calc R . . H11B H 1.1089 0.1278 1.1313 0.090 Uiso 1 1 calc R . . H11C H 0.9666 0.0888 1.1807 0.090 Uiso 1 1 calc R . . C12 C 1.0443(5) 0.3337(3) 1.1205(3) 0.0775(12) Uani 1 1 d . . . H12A H 0.9949 0.3996 1.1033 0.116 Uiso 1 1 calc R . . H12B H 1.1190 0.3133 1.0731 0.116 Uiso 1 1 calc R . . H12C H 1.0940 0.3328 1.1799 0.116 Uiso 1 1 calc R . . C13 C 1.0233(5) 0.3739(3) 0.8609(4) 0.0906(15) Uani 1 1 d . . . H13A H 1.0221 0.4343 0.8221 0.136 Uiso 1 1 calc R . . H13B H 1.0471 0.3186 0.8227 0.136 Uiso 1 1 calc R . . H13C H 1.0993 0.3704 0.9086 0.136 Uiso 1 1 calc R . . C14 C 0.7258(6) 0.3937(3) 0.8126(3) 0.0865(15) Uani 1 1 d . . . H14A H 0.6221 0.3857 0.8292 0.130 Uiso 1 1 calc R . . H14B H 0.7643 0.3478 0.7669 0.130 Uiso 1 1 calc R . . H14C H 0.7289 0.4600 0.7865 0.130 Uiso 1 1 calc R . . C15 C 0.4865(4) 0.1926(3) 1.1038(3) 0.0625(9) Uani 1 1 d . . . H15A H 0.3891 0.2234 1.1262 0.094 Uiso 1 1 calc R . . H15B H 0.5550 0.1758 1.1558 0.094 Uiso 1 1 calc R . . H15C H 0.4734 0.1335 1.0742 0.094 Uiso 1 1 calc R . . C16 C 0.5284(4) 0.3844(3) 1.0825(3) 0.0639(9) Uani 1 1 d . . . H16A H 0.5787 0.4350 1.0503 0.096 Uiso 1 1 calc R . . H16B H 0.5671 0.3709 1.1453 0.096 Uiso 1 1 calc R . . H16C H 0.4202 0.4063 1.0852 0.096 Uiso 1 1 calc R . . O5 O 1.0431(3) 0.1224(2) 0.81279(16) 0.0636(6) Uani 1 1 d . . . O6 O 1.0458(2) 0.16431(16) 0.96126(15) 0.0475(5) Uani 1 1 d . . . O7 O 1.2052(2) -0.08276(15) 0.94566(15) 0.0485(5) Uani 1 1 d . . . O8 O 1.3290(3) -0.01528(18) 1.05326(17) 0.0596(6) Uani 1 1 d . . . C17 C 1.1053(4) 0.1234(2) 0.8890(2) 0.0455(7) Uani 1 1 d . . . C18 C 1.2702(3) 0.0737(2) 0.9043(2) 0.0469(7) Uani 1 1 d . . . H18A H 1.3148 0.0515 0.8452 0.056 Uiso 1 1 calc R . . H18B H 1.3311 0.1205 0.9270 0.056 Uiso 1 1 calc R . . C19 C 1.2701(3) -0.0137(2) 0.9756(2) 0.0426(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03857(12) 0.03691(13) 0.03754(12) -0.00100(9) -0.00432(10) -0.00660(9) O1W 0.0550(13) 0.0539(14) 0.0489(13) -0.0062(11) -0.0160(11) -0.0117(11) S1 0.0457(4) 0.0459(4) 0.0372(4) -0.0018(3) -0.0035(3) -0.0133(3) S2 0.0371(4) 0.0512(5) 0.0540(5) -0.0041(3) -0.0016(3) -0.0067(3) S3 0.0459(4) 0.0430(4) 0.0435(4) 0.0047(3) -0.0044(3) -0.0083(3) O11 0.0791(16) 0.0683(16) 0.0571(15) 0.0066(12) -0.0152(13) -0.0427(13) O12 0.0523(13) 0.0555(15) 0.0824(18) -0.0219(13) -0.0004(12) -0.0004(11) O13 0.0814(16) 0.0624(15) 0.0497(13) 0.0138(11) -0.0233(13) -0.0195(13) C1 0.0585(19) 0.063(2) 0.056(2) -0.0013(16) -0.0207(17) -0.0057(16) C2 0.067(2) 0.088(3) 0.0446(19) -0.0133(18) 0.0069(17) -0.011(2) C3 0.0523(18) 0.073(3) 0.073(3) -0.010(2) 0.0155(18) -0.0226(17) C4 0.0440(17) 0.092(3) 0.072(3) 0.008(2) -0.0187(18) -0.0016(18) C5 0.0539(18) 0.065(2) 0.063(2) 0.0072(18) 0.0115(17) -0.0142(16) C6 0.063(2) 0.0408(18) 0.071(2) 0.0009(16) 0.0021(18) -0.0087(15) O1 0.0769(17) 0.096(2) 0.0447(14) -0.0119(13) 0.0023(12) -0.0094(15) O2 0.0526(12) 0.0514(13) 0.0456(12) -0.0088(10) -0.0018(10) 0.0041(10) O3 0.0572(12) 0.0423(12) 0.0504(13) 0.0029(9) -0.0054(10) -0.0130(10) O4 0.0667(15) 0.0519(14) 0.0678(16) -0.0101(12) -0.0061(13) -0.0187(11) C7 0.0593(18) 0.0414(17) 0.0460(17) 0.0030(13) 0.0072(15) -0.0078(14) C8 0.0594(18) 0.0430(17) 0.062(2) 0.0007(15) 0.0225(16) -0.0080(14) C9 0.0402(14) 0.0429(17) 0.061(2) -0.0073(14) 0.0117(14) -0.0084(12) Ru2 0.04235(13) 0.03590(13) 0.03579(12) -0.00001(9) -0.00204(10) -0.00555(9) O2W 0.0554(13) 0.0499(13) 0.0402(12) 0.0001(10) -0.0082(11) -0.0100(11) S4 0.0458(4) 0.0527(5) 0.0412(4) -0.0100(3) -0.0039(3) -0.0053(3) S5 0.0420(4) 0.0529(5) 0.0456(4) 0.0042(3) -0.0038(3) -0.0015(3) S6 0.0626(5) 0.0375(4) 0.0487(4) 0.0021(3) 0.0084(4) -0.0080(3) O14 0.0594(15) 0.118(2) 0.0489(14) -0.0274(15) 0.0038(12) 0.0084(14) O15 0.0580(14) 0.097(2) 0.0624(16) 0.0022(15) -0.0174(13) 0.0049(14) O16 0.0739(15) 0.0376(12) 0.0667(16) -0.0072(11) 0.0103(12) -0.0069(11) C11 0.070(2) 0.062(2) 0.0452(18) -0.0009(16) -0.0150(17) -0.0003(17) C12 0.082(3) 0.066(3) 0.091(3) -0.008(2) -0.027(2) -0.028(2) C13 0.101(3) 0.053(2) 0.114(4) 0.007(2) 0.058(3) -0.014(2) C14 0.144(4) 0.060(2) 0.055(2) 0.0203(19) -0.028(3) -0.024(3) C15 0.0507(18) 0.065(2) 0.070(2) 0.0053(19) 0.0128(17) -0.0113(16) C16 0.057(2) 0.057(2) 0.072(2) -0.0028(18) 0.0055(18) 0.0066(16) O5 0.0677(15) 0.0787(18) 0.0413(13) -0.0057(12) -0.0007(11) 0.0011(13) O6 0.0466(11) 0.0506(13) 0.0445(12) -0.0082(10) -0.0021(9) -0.0023(9) O7 0.0585(13) 0.0393(11) 0.0482(12) 0.0054(9) -0.0096(10) -0.0112(9) O8 0.0717(15) 0.0552(14) 0.0557(14) 0.0022(11) -0.0107(12) -0.0234(12) C17 0.0558(17) 0.0352(15) 0.0448(17) 0.0026(12) 0.0086(14) -0.0083(12) C18 0.0480(15) 0.0419(16) 0.0510(17) -0.0007(13) 0.0092(14) -0.0101(13) C19 0.0398(14) 0.0420(16) 0.0457(16) -0.0004(12) 0.0024(13) -0.0069(11) _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 O3 2.106(2) 2_656 ? Ru1 O2 2.111(2) . ? Ru1 O1W 2.144(2) . ? Ru1 S2 2.2547(11) . ? Ru1 S3 2.2646(10) . ? Ru1 S1 2.2780(9) . ? S1 O11 1.479(2) . ? S1 C2 1.766(4) . ? S1 C1 1.784(3) . ? S2 O12 1.476(3) . ? S2 C3 1.783(4) . ? S2 C4 1.793(3) . ? S3 O13 1.481(2) . ? S3 C5 1.774(3) . ? S3 C6 1.776(4) . ? O1 C7 1.230(4) . ? O2 C7 1.269(4) . ? O3 C9 1.275(4) . ? O3 Ru1 2.106(2) 2_656 ? O4 C9 1.227(4) . ? C7 C8 1.523(4) . ? C8 C9 1.514(4) . ? Ru2 O7 2.108(2) 2_757 ? Ru2 O6 2.116(2) . ? Ru2 O2W 2.152(2) . ? Ru2 S6 2.2498(10) . ? Ru2 S4 2.2745(10) . ? Ru2 S5 2.2745(10) . ? S4 O14 1.471(3) . ? S4 C11 1.777(3) . ? S4 C12 1.778(4) . ? S5 O15 1.491(2) . ? S5 C15 1.771(4) . ? S5 C16 1.771(4) . ? S6 O16 1.478(2) . ? S6 C13 1.772(4) . ? S6 C14 1.777(4) . ? O5 C17 1.229(4) . ? O6 C17 1.273(4) . ? O7 C19 1.277(3) . ? O7 Ru2 2.108(2) 2_757 ? O8 C19 1.229(4) . ? C17 C18 1.528(4) . ? C18 C19 1.514(4) . ? 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 O3 Ru1 O2 87.17(9) 2_656 . ? O3 Ru1 O1W 89.81(9) 2_656 . ? O2 Ru1 O1W 90.47(9) . . ? O3 Ru1 S2 90.92(7) 2_656 . ? O2 Ru1 S2 178.09(7) . . ? O1W Ru1 S2 89.47(8) . . ? O3 Ru1 S3 177.31(7) 2_656 . ? O2 Ru1 S3 90.13(7) . . ? O1W Ru1 S3 90.09(8) . . ? S2 Ru1 S3 91.77(4) . . ? O3 Ru1 S1 83.65(6) 2_656 . ? O2 Ru1 S1 82.18(6) . . ? O1W Ru1 S1 170.38(7) . . ? S2 Ru1 S1 97.66(4) . . ? S3 Ru1 S1 96.11(4) . . ? O11 S1 C2 107.38(18) . . ? O11 S1 C1 106.77(16) . . ? C2 S1 C1 98.54(19) . . ? O11 S1 Ru1 118.46(10) . . ? C2 S1 Ru1 114.81(12) . . ? C1 S1 Ru1 108.77(12) . . ? O12 S2 C3 106.30(18) . . ? O12 S2 C4 106.94(18) . . ? C3 S2 C4 99.47(19) . . ? O12 S2 Ru1 119.63(10) . . ? C3 S2 Ru1 112.41(14) . . ? C4 S2 Ru1 110.09(14) . . ? O13 S3 C5 106.48(17) . . ? O13 S3 C6 107.09(16) . . ? C5 S3 C6 99.53(18) . . ? O13 S3 Ru1 115.59(10) . . ? C5 S3 Ru1 112.59(13) . . ? C6 S3 Ru1 114.10(13) . . ? C7 O2 Ru1 127.8(2) . . ? C9 O3 Ru1 128.8(2) . 2_656 ? O1 C7 O2 126.3(3) . . ? O1 C7 C8 119.7(3) . . ? O2 C7 C8 114.0(3) . . ? C9 C8 C7 107.8(3) . . ? O4 C9 O3 125.7(3) . . ? O4 C9 C8 121.8(3) . . ? O3 C9 C8 112.5(3) . . ? O7 Ru2 O6 85.86(9) 2_757 . ? O7 Ru2 O2W 89.42(9) 2_757 . ? O6 Ru2 O2W 89.68(9) . . ? O7 Ru2 S6 178.69(7) 2_757 . ? O6 Ru2 S6 92.89(7) . . ? O2W Ru2 S6 90.19(7) . . ? O7 Ru2 S4 83.34(6) 2_757 . ? O6 Ru2 S4 83.60(6) . . ? O2W Ru2 S4 170.44(7) . . ? S6 Ru2 S4 96.91(4) . . ? O7 Ru2 S5 90.08(7) 2_757 . ? O6 Ru2 S5 175.94(6) . . ? O2W Ru2 S5 90.20(7) . . ? S6 Ru2 S5 91.17(4) . . ? S4 Ru2 S5 96.02(4) . . ? O14 S4 C11 106.33(18) . . ? O14 S4 C12 108.3(2) . . ? C11 S4 C12 98.69(19) . . ? O14 S4 Ru2 119.99(10) . . ? C11 S4 Ru2 108.57(12) . . ? C12 S4 Ru2 112.70(15) . . ? O15 S5 C15 106.87(17) . . ? O15 S5 C16 107.34(17) . . ? C15 S5 C16 99.3(2) . . ? O15 S5 Ru2 114.65(12) . . ? C15 S5 Ru2 112.00(13) . . ? C16 S5 Ru2 115.28(13) . . ? O16 S6 C13 106.43(19) . . ? O16 S6 C14 106.33(19) . . ? C13 S6 C14 99.0(2) . . ? O16 S6 Ru2 119.33(11) . . ? C13 S6 Ru2 113.14(15) . . ? C14 S6 Ru2 110.48(14) . . ? C17 O6 Ru2 129.20(19) . . ? C19 O7 Ru2 128.53(19) . 2_757 ? O5 C17 O6 126.2(3) . . ? O5 C17 C18 120.7(3) . . ? O6 C17 C18 113.1(3) . . ? C19 C18 C17 108.8(2) . . ? O8 C19 O7 125.6(3) . . ? O8 C19 C18 121.5(3) . . ? O7 C19 C18 112.9(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 O3 Ru1 S1 O11 165.97(15) 2_656 . . . ? O2 Ru1 S1 O11 77.96(15) . . . . ? O1W Ru1 S1 O11 118.5(5) . . . . ? S2 Ru1 S1 O11 -103.96(14) . . . . ? S3 Ru1 S1 O11 -11.33(14) . . . . ? O3 Ru1 S1 C2 -65.36(18) 2_656 . . . ? O2 Ru1 S1 C2 -153.36(17) . . . . ? O1W Ru1 S1 C2 -112.8(5) . . . . ? S2 Ru1 S1 C2 24.72(16) . . . . ? S3 Ru1 S1 C2 117.34(16) . . . . ? O3 Ru1 S1 C1 43.91(15) 2_656 . . . ? O2 Ru1 S1 C1 -44.10(15) . . . . ? O1W Ru1 S1 C1 -3.5(5) . . . . ? S2 Ru1 S1 C1 133.98(14) . . . . ? S3 Ru1 S1 C1 -133.39(14) . . . . ? O3 Ru1 S2 O12 113.41(15) 2_656 . . . ? O2 Ru1 S2 O12 114.8(18) . . . . ? O1W Ru1 S2 O12 -156.79(15) . . . . ? S3 Ru1 S2 O12 -66.71(14) . . . . ? S1 Ru1 S2 O12 29.69(14) . . . . ? O3 Ru1 S2 C3 -12.30(15) 2_656 . . . ? O2 Ru1 S2 C3 -10.9(18) . . . . ? O1W Ru1 S2 C3 77.50(16) . . . . ? S3 Ru1 S2 C3 167.57(15) . . . . ? S1 Ru1 S2 C3 -96.02(15) . . . . ? O3 Ru1 S2 C4 -122.19(17) 2_656 . . . ? O2 Ru1 S2 C4 -120.8(18) . . . . ? O1W Ru1 S2 C4 -32.39(17) . . . . ? S3 Ru1 S2 C4 57.68(16) . . . . ? S1 Ru1 S2 C4 154.09(16) . . . . ? O3 Ru1 S3 O13 99.9(12) 2_656 . . . ? O2 Ru1 S3 O13 102.42(15) . . . . ? O1W Ru1 S3 O13 11.94(15) . . . . ? S2 Ru1 S3 O13 -77.53(14) . . . . ? S1 Ru1 S3 O13 -175.43(13) . . . . ? O3 Ru1 S3 C5 -22.8(13) 2_656 . . . ? O2 Ru1 S3 C5 -20.27(16) . . . . ? O1W Ru1 S3 C5 -110.74(16) . . . . ? S2 Ru1 S3 C5 159.78(15) . . . . ? S1 Ru1 S3 C5 61.89(15) . . . . ? O3 Ru1 S3 C6 -135.3(12) 2_656 . . . ? O2 Ru1 S3 C6 -132.76(14) . . . . ? O1W Ru1 S3 C6 136.77(15) . . . . ? S2 Ru1 S3 C6 47.29(13) . . . . ? S1 Ru1 S3 C6 -50.60(13) . . . . ? O3 Ru1 O2 C7 102.1(3) 2_656 . . . ? O1W Ru1 O2 C7 12.3(3) . . . . ? S2 Ru1 O2 C7 100.8(18) . . . . ? S3 Ru1 O2 C7 -77.7(3) . . . . ? S1 Ru1 O2 C7 -173.9(3) . . . . ? Ru1 O2 C7 O1 0.1(5) . . . . ? Ru1 O2 C7 C8 -179.04(18) . . . . ? O1 C7 C8 C9 -115.4(4) . . . . ? O2 C7 C8 C9 63.8(4) . . . . ? Ru1 O3 C9 O4 9.0(5) 2_656 . . . ? Ru1 O3 C9 C8 -170.55(19) 2_656 . . . ? C7 C8 C9 O4 -101.8(3) . . . . ? C7 C8 C9 O3 77.7(3) . . . . ? O7 Ru2 S4 O14 -82.46(17) 2_757 . . . ? O6 Ru2 S4 O14 -169.02(17) . . . . ? O2W Ru2 S4 O14 -123.5(5) . . . . ? S6 Ru2 S4 O14 98.83(16) . . . . ? S5 Ru2 S4 O14 6.91(16) . . . . ? O7 Ru2 S4 C11 39.98(15) 2_757 . . . ? O6 Ru2 S4 C11 -46.58(16) . . . . ? O2W Ru2 S4 C11 -1.0(5) . . . . ? S6 Ru2 S4 C11 -138.73(14) . . . . ? S5 Ru2 S4 C11 129.35(14) . . . . ? O7 Ru2 S4 C12 148.24(18) 2_757 . . . ? O6 Ru2 S4 C12 61.68(18) . . . . ? O2W Ru2 S4 C12 107.2(5) . . . . ? S6 Ru2 S4 C12 -30.47(17) . . . . ? S5 Ru2 S4 C12 -122.39(17) . . . . ? O7 Ru2 S5 O15 -109.13(15) 2_757 . . . ? O6 Ru2 S5 O15 -108.1(8) . . . . ? O2W Ru2 S5 O15 -19.70(15) . . . . ? S6 Ru2 S5 O15 70.49(14) . . . . ? S4 Ru2 S5 O15 167.56(14) . . . . ? O7 Ru2 S5 C15 12.87(16) 2_757 . . . ? O6 Ru2 S5 C15 13.9(8) . . . . ? O2W Ru2 S5 C15 102.29(16) . . . . ? S6 Ru2 S5 C15 -167.51(15) . . . . ? S4 Ru2 S5 C15 -70.44(15) . . . . ? O7 Ru2 S5 C16 125.46(16) 2_757 . . . ? O6 Ru2 S5 C16 126.5(8) . . . . ? O2W Ru2 S5 C16 -145.12(16) . . . . ? S6 Ru2 S5 C16 -54.92(15) . . . . ? S4 Ru2 S5 C16 42.15(15) . . . . ? O7 Ru2 S6 O16 -138(3) 2_757 . . . ? O6 Ru2 S6 O16 -121.44(14) . . . . ? O2W Ru2 S6 O16 148.87(14) . . . . ? S4 Ru2 S6 O16 -37.55(13) . . . . ? S5 Ru2 S6 O16 58.66(12) . . . . ? O7 Ru2 S6 C13 -12(3) 2_757 . . . ? O6 Ru2 S6 C13 4.9(2) . . . . ? O2W Ru2 S6 C13 -84.8(2) . . . . ? S4 Ru2 S6 C13 88.8(2) . . . . ? S5 Ru2 S6 C13 -175.0(2) . . . . ? O7 Ru2 S6 C14 98(3) 2_757 . . . ? O6 Ru2 S6 C14 114.90(19) . . . . ? O2W Ru2 S6 C14 25.2(2) . . . . ? S4 Ru2 S6 C14 -161.21(19) . . . . ? S5 Ru2 S6 C14 -65.00(19) . . . . ? O7 Ru2 O6 C17 93.6(3) 2_757 . . . ? O2W Ru2 O6 C17 4.1(3) . . . . ? S6 Ru2 O6 C17 -86.1(2) . . . . ? S4 Ru2 O6 C17 177.3(3) . . . . ? S5 Ru2 O6 C17 92.5(8) . . . . ? Ru2 O6 C17 O5 11.4(5) . . . . ? Ru2 O6 C17 C18 -169.24(18) . . . . ? O5 C17 C18 C19 -113.5(3) . . . . ? O6 C17 C18 C19 67.2(3) . . . . ? Ru2 O7 C19 O8 -3.4(5) 2_757 . . . ? Ru2 O7 C19 C18 175.96(19) 2_757 . . . ? C17 C18 C19 O8 -114.2(3) . . . . ? C17 C18 C19 O7 66.4(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2W O1 0.92(4) 1.71(4) 2.613(4) 165(4) . O1W H1W O4 0.84(4) 1.76(4) 2.581(4) 164(4) 2_656 O2W H4W O5 0.89(4) 1.77(4) 2.638(4) 168(4) . O2W H3W O8 0.86(4) 1.74(4) 2.599(3) 175(3) 2_757 _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 29.62 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.608 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.100 #===END data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'fac-tris(dimethylsulfoxide,S)-chloro-(eta2-2-methylmalonato,O,O')- -ruthenium(II) potassium(I) hydrated' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H22 Cl O7 Ru S3 1-, K 1+, 1.5(H2 O)' _chemical_formula_sum 'C10 H25 Cl K O8.50 Ru S3' _chemical_formula_weight 553.10 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' 'Ru' 'Ru' -1.2594 0.8363 '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' 'K' 'K' 0.2009 0.2494 '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' 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 10.423(3) _cell_length_b 13.419(2) _cell_length_c 15.131(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.79(2) _cell_angle_gamma 90.00 _cell_volume 2085.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 1.414 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5776 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24135 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.10 _reflns_number_total 4430 _reflns_number_gt 3464 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1179P)^2^+0.1088P] 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 4430 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1766 _refine_ls_wR_factor_gt 0.1695 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.158 _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 Ru Ru 0.05062(3) 0.38796(3) 0.22174(2) 0.04647(18) Uani 1 1 d . . . Cl1 Cl 0.13165(19) 0.54711(14) 0.17759(14) 0.0897(5) Uani 1 1 d . . . S1 S -0.01351(13) 0.23687(11) 0.26411(10) 0.0592(3) Uani 1 1 d . . . S2 S 0.02614(14) 0.45675(12) 0.35358(10) 0.0648(4) Uani 1 1 d . . . S3 S -0.15290(14) 0.42917(16) 0.15929(10) 0.0743(5) Uani 1 1 d . . . O1 O -0.1449(5) 0.2202(4) 0.2745(5) 0.1071(18) Uani 1 1 d . . . O2 O -0.0569(5) 0.4078(5) 0.4087(3) 0.0955(17) Uani 1 1 d . . . O3 O -0.2554(4) 0.4349(5) 0.2121(4) 0.102(2) Uani 1 1 d . . . C1 C 0.0396(11) 0.1381(7) 0.2034(8) 0.143(5) Uani 1 1 d . . . H1A H -0.0007 0.1430 0.1416 0.215 Uiso 1 1 calc R . . H1B H 0.0160 0.0759 0.2276 0.215 Uiso 1 1 calc R . . H1C H 0.1324 0.1414 0.2078 0.215 Uiso 1 1 calc R . . C2 C 0.0816(8) 0.1996(7) 0.3691(6) 0.108(3) Uani 1 1 d . . . H2A H 0.0691 0.2465 0.4148 0.161 Uiso 1 1 calc R . . H2B H 0.1720 0.1979 0.3637 0.161 Uiso 1 1 calc R . . H2C H 0.0546 0.1346 0.3850 0.161 Uiso 1 1 calc R . . C3 C -0.0433(11) 0.5807(7) 0.3439(7) 0.126(4) Uani 1 1 d . . . H3A H -0.1302 0.5777 0.3105 0.189 Uiso 1 1 calc R . . H3B H 0.0089 0.6232 0.3134 0.189 Uiso 1 1 calc R . . H3C H -0.0456 0.6068 0.4027 0.189 Uiso 1 1 calc R . . C4 C 0.1744(7) 0.4851(8) 0.4164(6) 0.104(3) Uani 1 1 d . . . H4A H 0.2246 0.4253 0.4290 0.157 Uiso 1 1 calc R . . H4B H 0.1617 0.5155 0.4718 0.157 Uiso 1 1 calc R . . H4C H 0.2199 0.5306 0.3837 0.157 Uiso 1 1 calc R . . C5 C -0.2181(10) 0.3346(10) 0.0779(7) 0.138(4) Uani 1 1 d . . . H5A H -0.2196 0.2714 0.1075 0.208 Uiso 1 1 calc R . . H5B H -0.1642 0.3298 0.0325 0.208 Uiso 1 1 calc R . . H5C H -0.3050 0.3525 0.0505 0.208 Uiso 1 1 calc R . . C6 C -0.1654(10) 0.5326(10) 0.0852(8) 0.153(4) Uani 1 1 d . . . H6A H -0.1353 0.5916 0.1183 0.229 Uiso 1 1 calc R . . H6B H -0.2547 0.5413 0.0575 0.229 Uiso 1 1 calc R . . H6C H -0.1132 0.5208 0.0398 0.229 Uiso 1 1 calc R . . O4 O 0.4450(3) 0.3081(5) 0.2692(3) 0.0806(15) Uani 1 1 d . . . O5 O 0.2408(3) 0.3449(3) 0.2742(2) 0.0614(10) Uani 1 1 d . . . O6 O 0.0834(3) 0.3217(3) 0.1016(2) 0.0613(10) Uani 1 1 d . . . O7 O 0.2054(4) 0.2559(4) 0.0135(3) 0.0818(14) Uani 1 1 d . . . C7 C 0.3359(5) 0.3360(5) 0.2302(4) 0.0610(14) Uani 1 1 d . . . C8 C 0.3129(5) 0.3604(5) 0.1299(4) 0.0609(13) Uani 1 1 d . . . H8 H 0.2925 0.4317 0.1253 0.073 Uiso 1 1 calc R . . C9 C 0.1941(5) 0.3071(5) 0.0783(3) 0.0601(13) Uani 1 1 d . . . C10 C 0.4343(6) 0.3467(7) 0.0875(4) 0.0788(19) Uani 1 1 d . . . H10A H 0.5062 0.3810 0.1228 0.118 Uiso 1 1 calc R . . H10B H 0.4190 0.3735 0.0278 0.118 Uiso 1 1 calc R . . H10C H 0.4543 0.2770 0.0852 0.118 Uiso 1 1 calc R . . K1 K 0.69341(11) 0.33689(12) 0.35580(8) 0.0694(4) Uani 1 1 d . . . O1W O 0.4375(7) 0.3216(7) 0.4572(3) 0.134(3) Uani 1 1 d . . . O2W O 0.5633(11) 0.4783(10) 0.4468(9) 0.110(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0410(3) 0.0618(3) 0.0380(2) -0.00191(15) 0.01053(16) 0.00039(14) Cl1 0.1037(12) 0.0758(11) 0.1010(13) 0.0104(9) 0.0505(10) -0.0103(9) S1 0.0614(7) 0.0567(8) 0.0629(8) 0.0008(6) 0.0203(6) 0.0042(6) S2 0.0700(8) 0.0744(9) 0.0563(8) -0.0201(7) 0.0289(6) -0.0167(7) S3 0.0521(7) 0.1215(14) 0.0526(8) 0.0275(8) 0.0187(6) 0.0263(8) O1 0.090(3) 0.084(3) 0.160(5) 0.011(3) 0.056(3) -0.001(3) O2 0.080(3) 0.147(5) 0.069(3) -0.034(3) 0.037(2) -0.032(3) O3 0.054(2) 0.169(6) 0.089(3) 0.059(4) 0.026(2) 0.024(3) C1 0.170(11) 0.078(6) 0.209(13) -0.026(7) 0.106(10) 0.009(6) C2 0.104(6) 0.116(7) 0.107(6) 0.049(5) 0.030(5) 0.033(5) C3 0.166(10) 0.083(6) 0.145(9) -0.024(6) 0.071(8) 0.002(6) C4 0.088(4) 0.146(7) 0.084(4) -0.050(5) 0.029(4) -0.037(4) C5 0.102(6) 0.197(9) 0.109(6) -0.047(6) -0.004(5) 0.020(6) C6 0.112(6) 0.197(9) 0.152(7) 0.091(7) 0.030(5) 0.038(6) O4 0.042(2) 0.141(5) 0.058(2) 0.013(2) 0.0051(17) 0.007(2) O5 0.0429(17) 0.100(3) 0.0414(18) -0.0021(18) 0.0072(14) 0.0000(17) O6 0.0437(17) 0.097(3) 0.0433(18) -0.0139(18) 0.0091(14) -0.0016(16) O7 0.077(3) 0.116(4) 0.055(2) -0.029(2) 0.021(2) 0.004(3) C7 0.044(3) 0.092(4) 0.046(3) -0.004(3) 0.004(2) -0.004(2) C8 0.043(2) 0.092(4) 0.050(3) 0.001(3) 0.016(2) 0.003(2) C9 0.053(3) 0.087(4) 0.040(2) -0.003(2) 0.006(2) 0.005(2) C10 0.051(3) 0.131(6) 0.058(3) 0.007(4) 0.019(3) 0.007(3) K1 0.0483(6) 0.1085(11) 0.0526(7) 0.0162(7) 0.0120(5) -0.0029(6) O1W 0.137(5) 0.207(8) 0.055(3) 0.019(4) 0.014(3) 0.082(5) O2W 0.111(8) 0.098(8) 0.129(10) -0.016(7) 0.046(7) 0.010(6) _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 Ru O5 2.088(3) . ? Ru O6 2.103(3) . ? Ru S3 2.2398(15) . ? Ru S2 2.2516(14) . ? Ru S1 2.2614(15) . ? Ru Cl1 2.4316(18) . ? S1 O1 1.423(5) . ? S1 C1 1.755(9) . ? S1 C2 1.795(8) . ? S2 O2 1.457(5) . ? S2 C4 1.714(7) . ? S2 C3 1.810(9) . ? S3 O3 1.441(5) . ? S3 C6 1.774(10) . ? S3 C5 1.819(11) . ? O1 K1 2.740(6) 1_455 ? O2 K1 2.759(5) 1_455 ? O3 K1 2.672(5) 1_455 ? O4 C7 1.247(6) . ? O4 K1 2.723(4) . ? O5 C7 1.290(6) . ? O6 C9 1.277(6) . ? O7 C9 1.220(7) . ? O7 K1 2.675(4) 4_565 ? C7 C8 1.531(7) . ? C8 C10 1.524(7) . ? C8 C9 1.525(8) . ? K1 O3 2.672(5) 1_655 ? K1 O7 2.675(4) 4_666 ? K1 O1 2.740(6) 1_655 ? K1 O2 2.759(5) 1_655 ? K1 O2W 2.824(11) . ? K1 O1W 3.302(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Ru O6 85.90(14) . . ? O5 Ru S3 177.05(12) . . ? O6 Ru S3 91.21(10) . . ? O5 Ru S2 91.13(11) . . ? O6 Ru S2 177.03(10) . . ? S3 Ru S2 91.76(6) . . ? O5 Ru S1 87.22(13) . . ? O6 Ru S1 88.02(13) . . ? S3 Ru S1 92.10(7) . . ? S2 Ru S1 91.89(6) . . ? O5 Ru Cl1 89.76(13) . . ? O6 Ru Cl1 91.06(13) . . ? S3 Ru Cl1 90.89(7) . . ? S2 Ru Cl1 88.87(7) . . ? S1 Ru Cl1 176.90(6) . . ? O1 S1 C1 109.5(5) . . ? O1 S1 C2 104.8(4) . . ? C1 S1 C2 94.4(5) . . ? O1 S1 Ru 120.6(2) . . ? C1 S1 Ru 113.2(4) . . ? C2 S1 Ru 110.8(3) . . ? O2 S2 C4 110.5(4) . . ? O2 S2 C3 101.1(4) . . ? C4 S2 C3 98.7(5) . . ? O2 S2 Ru 119.4(2) . . ? C4 S2 Ru 110.8(3) . . ? C3 S2 Ru 114.2(3) . . ? O3 S3 C6 109.1(4) . . ? O3 S3 C5 100.7(5) . . ? C6 S3 C5 98.0(6) . . ? O3 S3 Ru 121.2(2) . . ? C6 S3 Ru 115.0(4) . . ? C5 S3 Ru 109.4(3) . . ? S1 O1 K1 129.6(4) . 1_455 ? S2 O2 K1 127.8(3) . 1_455 ? S3 O3 K1 134.0(3) . 1_455 ? C7 O4 K1 154.4(5) . . ? C7 O5 Ru 126.3(3) . . ? C9 O6 Ru 126.2(3) . . ? C9 O7 K1 169.5(4) . 4_565 ? O4 C7 O5 120.1(5) . . ? O4 C7 C8 120.7(5) . . ? O5 C7 C8 119.2(4) . . ? C10 C8 C9 112.9(5) . . ? C10 C8 C7 113.0(5) . . ? C9 C8 C7 112.5(5) . . ? O7 C9 O6 121.6(5) . . ? O7 C9 C8 119.6(5) . . ? O6 C9 C8 118.7(5) . . ? O3 K1 O7 165.81(15) 1_655 4_666 ? O3 K1 O4 89.06(15) 1_655 . ? O7 K1 O4 105.03(14) 4_666 . ? O3 K1 O1 72.12(19) 1_655 1_655 ? O7 K1 O1 101.24(18) 4_666 1_655 ? O4 K1 O1 108.06(18) . 1_655 ? O3 K1 O2 75.96(17) 1_655 1_655 ? O7 K1 O2 90.17(16) 4_666 1_655 ? O4 K1 O2 164.04(18) . 1_655 ? O1 K1 O2 72.87(17) 1_655 1_655 ? O3 K1 O2W 104.2(3) 1_655 . ? O7 K1 O2W 80.3(3) 4_666 . ? O4 K1 O2W 80.4(3) . . ? O1 K1 O2W 170.4(3) 1_655 . ? O2 K1 O2W 97.7(3) 1_655 . ? O3 K1 O1W 134.25(14) 1_655 . ? O7 K1 O1W 58.37(13) 4_666 . ? O4 K1 O1W 55.77(14) . . ? O1 K1 O1W 141.2(2) 1_655 . ? O2 K1 O1W 133.11(17) 1_655 . ? O2W K1 O1W 47.3(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 O5 Ru S1 O1 160.2(4) . . . . ? O6 Ru S1 O1 -113.9(4) . . . . ? S3 Ru S1 O1 -22.7(4) . . . . ? S2 Ru S1 O1 69.1(4) . . . . ? Cl1 Ru S1 O1 173.2(12) . . . . ? O5 Ru S1 C1 -67.3(5) . . . . ? O6 Ru S1 C1 18.7(5) . . . . ? S3 Ru S1 C1 109.8(5) . . . . ? S2 Ru S1 C1 -158.3(5) . . . . ? Cl1 Ru S1 C1 -54.2(13) . . . . ? O5 Ru S1 C2 37.3(3) . . . . ? O6 Ru S1 C2 123.3(3) . . . . ? S3 Ru S1 C2 -145.5(3) . . . . ? S2 Ru S1 C2 -53.7(3) . . . . ? Cl1 Ru S1 C2 50.4(12) . . . . ? O5 Ru S2 O2 -107.8(3) . . . . ? O6 Ru S2 O2 -109(2) . . . . ? S3 Ru S2 O2 71.7(3) . . . . ? S1 Ru S2 O2 -20.5(3) . . . . ? Cl1 Ru S2 O2 162.5(3) . . . . ? O5 Ru S2 C4 22.3(4) . . . . ? O6 Ru S2 C4 21(3) . . . . ? S3 Ru S2 C4 -158.3(4) . . . . ? S1 Ru S2 C4 109.5(4) . . . . ? Cl1 Ru S2 C4 -67.5(4) . . . . ? O5 Ru S2 C3 132.6(4) . . . . ? O6 Ru S2 C3 132(2) . . . . ? S3 Ru S2 C3 -48.0(4) . . . . ? S1 Ru S2 C3 -140.1(4) . . . . ? Cl1 Ru S2 C3 42.9(4) . . . . ? O5 Ru S3 O3 138(2) . . . . ? O6 Ru S3 O3 149.3(4) . . . . ? S2 Ru S3 O3 -30.7(4) . . . . ? S1 Ru S3 O3 61.3(4) . . . . ? Cl1 Ru S3 O3 -119.6(4) . . . . ? O5 Ru S3 C6 -88(3) . . . . ? O6 Ru S3 C6 -76.0(6) . . . . ? S2 Ru S3 C6 104.0(6) . . . . ? S1 Ru S3 C6 -164.1(6) . . . . ? Cl1 Ru S3 C6 15.1(6) . . . . ? O5 Ru S3 C5 22(3) . . . . ? O6 Ru S3 C5 33.0(5) . . . . ? S2 Ru S3 C5 -147.0(5) . . . . ? S1 Ru S3 C5 -55.0(5) . . . . ? Cl1 Ru S3 C5 124.1(5) . . . . ? C1 S1 O1 K1 -178.3(6) . . . 1_455 ? C2 S1 O1 K1 81.4(5) . . . 1_455 ? Ru S1 O1 K1 -44.2(6) . . . 1_455 ? C4 S2 O2 K1 -178.8(4) . . . 1_455 ? C3 S2 O2 K1 77.4(5) . . . 1_455 ? Ru S2 O2 K1 -48.7(5) . . . 1_455 ? C6 S3 O3 K1 -169.6(6) . . . 1_455 ? C5 S3 O3 K1 88.0(6) . . . 1_455 ? Ru S3 O3 K1 -32.6(7) . . . 1_455 ? O6 Ru O5 C7 30.1(5) . . . . ? S3 Ru O5 C7 42(3) . . . . ? S2 Ru O5 C7 -149.8(5) . . . . ? S1 Ru O5 C7 118.3(5) . . . . ? Cl1 Ru O5 C7 -61.0(5) . . . . ? O5 Ru O6 C9 -23.3(5) . . . . ? S3 Ru O6 C9 157.2(5) . . . . ? S2 Ru O6 C9 -22(3) . . . . ? S1 Ru O6 C9 -110.7(5) . . . . ? Cl1 Ru O6 C9 66.3(5) . . . . ? K1 O4 C7 O5 -95.7(9) . . . . ? K1 O4 C7 C8 84.1(10) . . . . ? Ru O5 C7 O4 -178.9(5) . . . . ? Ru O5 C7 C8 1.3(8) . . . . ? O4 C7 C8 C10 0.0(9) . . . . ? O5 C7 C8 C10 179.7(6) . . . . ? O4 C7 C8 C9 129.2(6) . . . . ? O5 C7 C8 C9 -51.0(8) . . . . ? K1 O7 C9 O6 47(3) 4_565 . . . ? K1 O7 C9 C8 -129(2) 4_565 . . . ? Ru O6 C9 O7 169.6(5) . . . . ? Ru O6 C9 C8 -14.2(8) . . . . ? C10 C8 C9 O7 3.7(9) . . . . ? C7 C8 C9 O7 -125.6(6) . . . . ? C10 C8 C9 O6 -172.6(6) . . . . ? C7 C8 C9 O6 58.1(8) . . . . ? C7 O4 K1 O3 -58.4(9) . . . 1_655 ? C7 O4 K1 O7 123.3(9) . . . 4_666 ? C7 O4 K1 O1 -129.3(9) . . . 1_655 ? C7 O4 K1 O2 -38.5(12) . . . 1_655 ? C7 O4 K1 O2W 46.1(9) . . . . ? C7 O4 K1 O1W 90.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.295 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.134 #===END data_10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; fac-tris(dimethylsulfoxide,S)-(dimethylsulfoxide,O)-(eta2-2-methyl- -malonate,O,O')-ruthenium(II) hydrated ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H28 O8 Ru S4, H2 O' _chemical_formula_sum 'C12 H30 O9 Ru S4' _chemical_formula_weight 547.67 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' '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 c' 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' _cell_length_a 13.807(3) _cell_length_b 10.937(2) _cell_length_c 14.872(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.21(2) _cell_angle_gamma 90.00 _cell_volume 2186.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5185 _exptl_absorpt_correction_T_max 0.9029 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16821 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 31.06 _reflns_number_total 6866 _reflns_number_gt 5499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^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 mixed _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 -0.01(3) _refine_ls_number_reflns 6866 _refine_ls_number_parameters 241 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _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 Ru Ru 0.15666(3) 0.75540(2) 0.16257(3) 0.03310(6) Uani 1 1 d . . . S1 S 0.18561(7) 0.94491(8) 0.22234(7) 0.0418(2) Uani 1 1 d . . . S2 S 0.14299(8) 0.82027(10) 0.01658(7) 0.0442(2) Uani 1 1 d . . . S3 S 0.32032(7) 0.70726(10) 0.18390(7) 0.03792(19) Uani 1 1 d . . . S4 S 0.05225(8) 0.49312(8) 0.14410(7) 0.0435(2) Uani 1 1 d . . . O1 O 0.0960(2) 1.0188(3) 0.2249(2) 0.0586(8) Uani 1 1 d . . . O2 O 0.2328(2) 0.8641(3) -0.0110(2) 0.0597(8) Uani 1 1 d . . . O3 O 0.3972(2) 0.8037(3) 0.2075(2) 0.0537(7) Uani 1 1 d . . . O4 O 0.1313(2) 0.5727(2) 0.11364(18) 0.0428(6) Uani 1 1 d . . . C1 C 0.2628(4) 1.0404(4) 0.1727(4) 0.0602(12) Uani 1 1 d . . . H7A H 0.2320 1.0542 0.1088 0.090 Uiso 1 1 calc R . . H7B H 0.3261 1.0016 0.1776 0.090 Uiso 1 1 calc R . . H7C H 0.2720 1.1171 0.2049 0.090 Uiso 1 1 calc R . . C2 C 0.2606(4) 0.9389(4) 0.3359(3) 0.0563(11) Uani 1 1 d . . . H8A H 0.2288 0.8888 0.3737 0.084 Uiso 1 1 calc R . . H8B H 0.2695 1.0200 0.3612 0.084 Uiso 1 1 calc R . . H8C H 0.3243 0.9046 0.3346 0.084 Uiso 1 1 calc R . . C3 C 0.0500(4) 0.9363(5) -0.0122(4) 0.0699(14) Uani 1 1 d . . . H3A H 0.0695 1.0061 0.0270 0.105 Uiso 1 1 calc R . . H3B H -0.0122 0.9053 -0.0033 0.105 Uiso 1 1 calc R . . H3C H 0.0428 0.9598 -0.0755 0.105 Uiso 1 1 calc R . . C4 C 0.0859(4) 0.7092(5) -0.0665(3) 0.0693(14) Uani 1 1 d . . . H4A H 0.1269 0.6375 -0.0605 0.104 Uiso 1 1 calc R . . H4B H 0.0781 0.7424 -0.1275 0.104 Uiso 1 1 calc R . . H4C H 0.0218 0.6879 -0.0563 0.104 Uiso 1 1 calc R . . C5 C 0.3469(3) 0.6222(4) 0.0904(3) 0.0547(10) Uani 1 1 d . . . H5A H 0.3335 0.6718 0.0357 0.082 Uiso 1 1 calc R . . H5B H 0.3058 0.5505 0.0800 0.082 Uiso 1 1 calc R . . H5C H 0.4156 0.5986 0.1050 0.082 Uiso 1 1 calc R . . C6 C 0.3514(3) 0.5934(4) 0.2712(3) 0.0549(10) Uani 1 1 d . . . H6A H 0.3416 0.6255 0.3286 0.082 Uiso 1 1 calc R . . H6B H 0.4198 0.5701 0.2783 0.082 Uiso 1 1 calc R . . H6C H 0.3096 0.5232 0.2538 0.082 Uiso 1 1 calc R . . C7 C -0.0445(3) 0.4819(4) 0.0425(3) 0.0547(10) Uani 1 1 d . . . H1A H -0.0811 0.5572 0.0330 0.082 Uiso 1 1 calc R . . H1B H -0.0885 0.4162 0.0492 0.082 Uiso 1 1 calc R . . H1C H -0.0162 0.4661 -0.0096 0.082 Uiso 1 1 calc R . . C8 C 0.1060(4) 0.3450(4) 0.1454(4) 0.0671(13) Uani 1 1 d . . . H2A H 0.1607 0.3377 0.1981 0.101 Uiso 1 1 calc R . . H2B H 0.1293 0.3332 0.0900 0.101 Uiso 1 1 calc R . . H2C H 0.0568 0.2842 0.1489 0.101 Uiso 1 1 calc R . . O5 O 0.0030(2) 0.7702(3) 0.14217(19) 0.0409(6) Uani 1 1 d . . . O6 O 0.1572(2) 0.6815(2) 0.29110(17) 0.0399(6) Uani 1 1 d . . . O7 O -0.1395(2) 0.7986(3) 0.1804(2) 0.0533(7) Uani 1 1 d . . . O8 O 0.0919(3) 0.6287(4) 0.4059(2) 0.0783(11) Uani 1 1 d . . . C9 C -0.0489(3) 0.7816(3) 0.2036(3) 0.0394(7) Uani 1 1 d . . . C10 C 0.0034(3) 0.7819(4) 0.3061(3) 0.0432(8) Uani 1 1 d . . . H10 H 0.0352 0.8623 0.3169 0.052 Uiso 1 1 calc R . . C11 C 0.0884(3) 0.6897(3) 0.3368(3) 0.0436(8) Uani 1 1 d . . . C12 C -0.0702(3) 0.7788(4) 0.3680(3) 0.0541(10) Uani 1 1 d . . . H12A H -0.1217 0.8379 0.3468 0.081 Uiso 1 1 calc R . . H12B H -0.0362 0.7977 0.4303 0.081 Uiso 1 1 calc R . . H12C H -0.0991 0.6987 0.3661 0.081 Uiso 1 1 calc R . . O1W O -0.1862(3) 0.8170(6) -0.0176(3) 0.1048(15) Uani 1 1 d D . . H1W H -0.175(7) 0.803(8) 0.0428(18) 0.157 Uiso 1 1 d D . . H2W H -0.244(4) 0.855(7) -0.035(6) 0.157 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.03197(10) 0.03667(11) 0.03067(9) 0.00070(11) 0.00720(7) -0.00254(11) S1 0.0411(5) 0.0355(4) 0.0499(5) -0.0040(4) 0.0124(4) -0.0015(4) S2 0.0425(5) 0.0568(5) 0.0329(4) 0.0091(4) 0.0079(4) -0.0054(4) S3 0.0336(5) 0.0400(4) 0.0408(5) -0.0006(4) 0.0098(4) -0.0005(4) S4 0.0436(5) 0.0431(4) 0.0468(5) -0.0054(4) 0.0164(4) -0.0088(4) O1 0.0481(17) 0.0455(15) 0.084(2) -0.0063(14) 0.0187(16) 0.0066(13) O2 0.0517(18) 0.082(2) 0.0494(17) 0.0183(15) 0.0196(14) -0.0093(16) O3 0.0366(15) 0.0512(15) 0.074(2) -0.0076(14) 0.0145(13) -0.0066(12) O4 0.0441(16) 0.0443(13) 0.0441(15) -0.0065(11) 0.0187(13) -0.0099(11) C1 0.062(3) 0.046(2) 0.078(3) -0.002(2) 0.026(2) -0.008(2) C2 0.060(3) 0.054(2) 0.053(3) -0.017(2) 0.011(2) -0.003(2) C3 0.062(3) 0.079(4) 0.059(3) 0.022(3) -0.005(2) 0.012(3) C4 0.083(4) 0.084(3) 0.037(2) 0.001(2) 0.004(2) -0.016(3) C5 0.051(2) 0.060(2) 0.058(2) -0.0089(19) 0.022(2) 0.0011(19) C6 0.049(2) 0.066(2) 0.050(2) 0.0116(19) 0.0100(18) 0.017(2) C7 0.045(2) 0.064(2) 0.057(3) -0.0081(19) 0.0154(19) -0.0116(19) C8 0.056(3) 0.050(2) 0.098(4) 0.006(2) 0.023(3) -0.005(2) O5 0.0348(14) 0.0545(15) 0.0326(13) 0.0015(11) 0.0061(11) -0.0016(12) O6 0.0392(14) 0.0466(13) 0.0354(13) 0.0052(10) 0.0118(11) 0.0022(11) O7 0.0376(15) 0.0656(17) 0.0568(17) 0.0015(14) 0.0107(13) 0.0043(13) O8 0.067(2) 0.115(3) 0.062(2) 0.042(2) 0.0339(18) 0.023(2) C9 0.0312(16) 0.0390(16) 0.050(2) 0.0035(14) 0.0126(15) 0.0000(13) C10 0.043(2) 0.0497(18) 0.0411(19) 0.0018(14) 0.0191(16) -0.0021(15) C11 0.046(2) 0.050(2) 0.0351(18) 0.0038(15) 0.0101(16) -0.0027(17) C12 0.055(3) 0.062(2) 0.051(2) 0.0083(18) 0.0249(19) 0.0070(19) O1W 0.069(3) 0.182(5) 0.057(2) -0.004(3) 0.000(2) 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 Ru O6 2.074(3) . ? Ru O5 2.080(3) . ? Ru O4 2.128(3) . ? Ru S2 2.2507(11) . ? Ru S1 2.2546(10) . ? Ru S3 2.2707(12) . ? S4 O4 1.543(3) . ? S4 C7 1.778(5) . ? S4 C8 1.780(4) . ? S2 O2 1.473(3) . ? S2 C4 1.783(5) . ? S2 C3 1.786(5) . ? S3 O3 1.480(3) . ? S3 C5 1.779(4) . ? S3 C6 1.779(4) . ? S1 O1 1.485(3) . ? S1 C1 1.769(5) . ? S1 C2 1.770(5) . ? O5 C9 1.290(4) . ? O6 C11 1.291(5) . ? O7 C9 1.234(4) . ? O8 C11 1.217(4) . ? C9 C10 1.530(5) . ? C10 C12 1.519(5) . ? C10 C11 1.535(6) . ? 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 O6 Ru O5 87.31(11) . . ? O6 Ru O4 85.11(10) . . ? O5 Ru O4 86.58(11) . . ? O6 Ru S2 173.63(9) . . ? O5 Ru S2 88.67(9) . . ? O4 Ru S2 89.72(8) . . ? O6 Ru S1 91.84(8) . . ? O5 Ru S1 93.96(9) . . ? O4 Ru S1 176.87(9) . . ? S2 Ru S1 93.37(4) . . ? O6 Ru S3 89.27(8) . . ? O5 Ru S3 171.05(10) . . ? O4 Ru S3 84.89(8) . . ? S2 Ru S3 93.97(4) . . ? S1 Ru S3 94.41(4) . . ? O4 S4 C7 103.52(19) . . ? O4 S4 C8 101.3(2) . . ? C7 S4 C8 100.2(2) . . ? O2 S2 C4 107.2(2) . . ? O2 S2 C3 107.9(2) . . ? C4 S2 C3 97.9(3) . . ? O2 S2 Ru 118.74(13) . . ? C4 S2 Ru 112.35(17) . . ? C3 S2 Ru 110.61(18) . . ? O3 S3 C5 107.1(2) . . ? O3 S3 C6 106.6(2) . . ? C5 S3 C6 98.4(2) . . ? O3 S3 Ru 120.30(13) . . ? C5 S3 Ru 112.83(17) . . ? C6 S3 Ru 109.30(15) . . ? O1 S1 C1 105.9(2) . . ? O1 S1 C2 107.8(2) . . ? C1 S1 C2 98.2(3) . . ? O1 S1 Ru 115.90(13) . . ? C1 S1 Ru 116.59(17) . . ? C2 S1 Ru 110.75(15) . . ? S4 O4 Ru 120.11(15) . . ? C9 O5 Ru 128.1(3) . . ? C11 O6 Ru 127.6(2) . . ? O7 C9 O5 120.5(4) . . ? O7 C9 C10 119.8(3) . . ? O5 C9 C10 119.6(3) . . ? C12 C10 C9 112.0(3) . . ? C12 C10 C11 112.1(3) . . ? C9 C10 C11 116.7(3) . . ? O8 C11 O6 120.9(4) . . ? O8 C11 C10 119.5(4) . . ? O6 C11 C10 119.5(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 O6 Ru S2 O2 -145.4(8) . . . . ? O5 Ru S2 O2 163.68(18) . . . . ? O4 Ru S2 O2 -109.74(18) . . . . ? S1 Ru S2 O2 69.78(17) . . . . ? S3 Ru S2 O2 -24.88(17) . . . . ? O6 Ru S2 C4 -19.2(9) . . . . ? O5 Ru S2 C4 -70.1(2) . . . . ? O4 Ru S2 C4 16.5(2) . . . . ? S1 Ru S2 C4 -164.0(2) . . . . ? S3 Ru S2 C4 101.3(2) . . . . ? O6 Ru S2 C3 89.1(8) . . . . ? O5 Ru S2 C3 38.2(2) . . . . ? O4 Ru S2 C3 124.8(2) . . . . ? S1 Ru S2 C3 -55.7(2) . . . . ? S3 Ru S2 C3 -150.4(2) . . . . ? O6 Ru S3 O3 -104.38(18) . . . . ? O5 Ru S3 O3 -171.9(6) . . . . ? O4 Ru S3 O3 170.46(17) . . . . ? S2 Ru S3 O3 81.10(16) . . . . ? S1 Ru S3 O3 -12.60(16) . . . . ? O6 Ru S3 C5 127.71(18) . . . . ? O5 Ru S3 C5 60.2(6) . . . . ? O4 Ru S3 C5 42.55(19) . . . . ? S2 Ru S3 C5 -46.81(18) . . . . ? S1 Ru S3 C5 -140.51(17) . . . . ? O6 Ru S3 C6 19.31(18) . . . . ? O5 Ru S3 C6 -48.2(6) . . . . ? O4 Ru S3 C6 -65.84(18) . . . . ? S2 Ru S3 C6 -155.21(17) . . . . ? S1 Ru S3 C6 111.10(17) . . . . ? O6 Ru S1 O1 -90.14(17) . . . . ? O5 Ru S1 O1 -2.71(17) . . . . ? O4 Ru S1 O1 -102.6(16) . . . . ? S2 Ru S1 O1 86.19(16) . . . . ? S3 Ru S1 O1 -179.55(15) . . . . ? O6 Ru S1 C1 144.2(2) . . . . ? O5 Ru S1 C1 -128.4(2) . . . . ? O4 Ru S1 C1 131.7(16) . . . . ? S2 Ru S1 C1 -39.5(2) . . . . ? S3 Ru S1 C1 54.8(2) . . . . ? O6 Ru S1 C2 33.00(19) . . . . ? O5 Ru S1 C2 120.44(19) . . . . ? O4 Ru S1 C2 20.5(17) . . . . ? S2 Ru S1 C2 -150.66(18) . . . . ? S3 Ru S1 C2 -56.41(18) . . . . ? C7 S4 O4 Ru 108.8(2) . . . . ? C8 S4 O4 Ru -147.7(2) . . . . ? O6 Ru O4 S4 46.4(2) . . . . ? O5 Ru O4 S4 -41.18(19) . . . . ? S2 Ru O4 S4 -129.87(18) . . . . ? S1 Ru O4 S4 58.9(18) . . . . ? S3 Ru O4 S4 136.12(19) . . . . ? O6 Ru O5 C9 26.8(3) . . . . ? O4 Ru O5 C9 112.1(3) . . . . ? S2 Ru O5 C9 -158.1(3) . . . . ? S1 Ru O5 C9 -64.8(3) . . . . ? S3 Ru O5 C9 94.5(6) . . . . ? O5 Ru O6 C11 -18.9(3) . . . . ? O4 Ru O6 C11 -105.7(3) . . . . ? S2 Ru O6 C11 -69.9(9) . . . . ? S1 Ru O6 C11 74.9(3) . . . . ? S3 Ru O6 C11 169.3(3) . . . . ? Ru O5 C9 O7 174.5(3) . . . . ? Ru O5 C9 C10 -1.7(5) . . . . ? O7 C9 C10 C12 11.5(5) . . . . ? O5 C9 C10 C12 -172.3(3) . . . . ? O7 C9 C10 C11 142.6(4) . . . . ? O5 C9 C10 C11 -41.1(5) . . . . ? Ru O6 C11 O8 170.1(3) . . . . ? Ru O6 C11 C10 -12.7(5) . . . . ? C12 C10 C11 O8 -2.6(6) . . . . ? C9 C10 C11 O8 -133.7(4) . . . . ? C12 C10 C11 O6 -179.9(4) . . . . ? C9 C10 C11 O6 49.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 31.06 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.414 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.101 #===END data_11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis[aquo-tris(dimethylsulfoxide,S)-(mu-2,2'-dimethylmalonate,O,O')- -ruthenium(II)] hydrated ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H52 O16 Ru2 S6, H2 O' _chemical_formula_sum 'C22 H54 O17 Ru2 S6' _chemical_formula_weight 985.15 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' '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.553(3) _cell_length_b 11.356(3) _cell_length_c 22.512(4) _cell_angle_alpha 79.08(3) _cell_angle_beta 82.26(2) _cell_angle_gamma 69.96(2) _cell_volume 2011.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 1.125 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5562 _exptl_absorpt_correction_T_max 0.8075 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26261 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8255 _reflns_number_gt 6800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.01 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0925P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8255 _refine_ls_number_parameters 445 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1288 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.13004(3) 0.80952(3) 0.901562(12) 0.04183(10) Uani 1 1 d . . . O1W O -0.1349(3) 0.8435(3) 0.90687(12) 0.0513(6) Uani 1 1 d D . . H11 H -0.171(5) 0.818(4) 0.9462(11) 0.062 Uiso 1 1 d D . . H12 H -0.166(6) 0.9326(19) 0.900(2) 0.062 Uiso 1 1 d D . . S1 S 0.40000(12) 0.78534(10) 0.91110(5) 0.0541(2) Uani 1 1 d . . . S2 S 0.14558(13) 0.82943(10) 0.80015(4) 0.0534(2) Uani 1 1 d . . . S3 S 0.17227(13) 0.59817(9) 0.90836(5) 0.0544(2) Uani 1 1 d . . . O11 O 0.5057(5) 0.6581(4) 0.9356(2) 0.1002(14) Uani 1 1 d . . . O12 O 0.2898(4) 0.7429(4) 0.76885(14) 0.0812(10) Uani 1 1 d . . . O13 O 0.0340(5) 0.5699(3) 0.88718(16) 0.0733(9) Uani 1 1 d . . . C1 C 0.4074(6) 0.8884(6) 0.9593(3) 0.0792(15) Uani 1 1 d . . . H1A H 0.3499 0.8709 0.9979 0.119 Uiso 1 1 calc R . . H1B H 0.3548 0.9747 0.9414 0.119 Uiso 1 1 calc R . . H1C H 0.5216 0.8758 0.9649 0.119 Uiso 1 1 calc R . . C2 C 0.5129(7) 0.8386(9) 0.8462(3) 0.110(3) Uani 1 1 d . . . H2A H 0.5202 0.7904 0.8146 0.165 Uiso 1 1 calc R . . H2B H 0.6232 0.8276 0.8561 0.165 Uiso 1 1 calc R . . H2C H 0.4567 0.9268 0.8325 0.165 Uiso 1 1 calc R . . C3 C 0.1313(7) 0.9849(5) 0.7621(2) 0.0742(13) Uani 1 1 d . . . H3A H 0.2249 1.0061 0.7703 0.111 Uiso 1 1 calc R . . H3B H 0.0297 1.0448 0.7763 0.111 Uiso 1 1 calc R . . H3C H 0.1315 0.9877 0.7192 0.111 Uiso 1 1 calc R . . C4 C -0.0394(7) 0.8186(5) 0.7768(2) 0.0724(13) Uani 1 1 d . . . H4A H -0.0504 0.7375 0.7940 0.109 Uiso 1 1 calc R . . H4B H -0.0329 0.8278 0.7334 0.109 Uiso 1 1 calc R . . H4C H -0.1345 0.8846 0.7905 0.109 Uiso 1 1 calc R . . C5 C 0.2076(7) 0.5157(4) 0.9836(2) 0.0720(13) Uani 1 1 d . . . H5A H 0.1143 0.5524 1.0107 0.108 Uiso 1 1 calc R . . H5B H 0.3071 0.5223 0.9958 0.108 Uiso 1 1 calc R . . H5C H 0.2204 0.4280 0.9846 0.108 Uiso 1 1 calc R . . C6 C 0.3610(7) 0.5096(5) 0.8706(3) 0.0848(16) Uani 1 1 d . . . H6A H 0.3623 0.5428 0.8281 0.127 Uiso 1 1 calc R . . H6B H 0.3675 0.4222 0.8762 0.127 Uiso 1 1 calc R . . H6C H 0.4547 0.5163 0.8873 0.127 Uiso 1 1 calc R . . O1 O -0.1384(4) 0.7781(3) 1.02570(13) 0.0625(7) Uani 1 1 d . . . O2 O 0.1117(3) 0.7985(3) 0.99662(11) 0.0496(6) Uani 1 1 d . . . O3 O -0.0836(3) 0.9947(2) 1.09993(12) 0.0510(6) Uani 1 1 d . . . O4 O 0.1871(4) 0.9142(3) 1.11512(16) 0.0673(8) Uani 1 1 d . . . C7 C -0.0036(5) 0.7843(3) 1.03646(16) 0.0466(8) Uani 1 1 d . . . C8 C 0.0411(5) 0.7733(4) 1.10136(16) 0.0526(9) Uani 1 1 d . . . C9 C 0.0522(5) 0.9040(4) 1.10610(16) 0.0492(8) Uani 1 1 d . . . C20 C -0.0943(7) 0.7454(5) 1.1479(2) 0.0740(13) Uani 1 1 d . . . H20A H -0.1986 0.8119 1.1412 0.111 Uiso 1 1 calc R . . H20B H -0.0641 0.7406 1.1881 0.111 Uiso 1 1 calc R . . H20C H -0.1050 0.6660 1.1437 0.111 Uiso 1 1 calc R . . C21 C 0.2066(6) 0.6679(4) 1.1119(2) 0.0676(12) Uani 1 1 d . . . H21A H 0.2915 0.6857 1.0828 0.101 Uiso 1 1 calc R . . H21B H 0.1960 0.5886 1.1076 0.101 Uiso 1 1 calc R . . H21C H 0.2367 0.6631 1.1521 0.101 Uiso 1 1 calc R . . Ru2 Ru 0.45073(3) 0.74293(3) 0.395704(12) 0.04268(10) Uani 1 1 d . . . O2W O 0.2387(3) 0.6892(3) 0.38731(13) 0.0558(6) Uani 1 1 d D . . H21 H 0.214(6) 0.680(5) 0.4293(9) 0.067 Uiso 1 1 d D . . H22 H 0.292(5) 0.603(2) 0.385(2) 0.067 Uiso 1 1 d D . . S4 S 0.67654(13) 0.78110(11) 0.41855(6) 0.0607(3) Uani 1 1 d . . . S5 S 0.27936(13) 0.94836(9) 0.39043(5) 0.0546(2) Uani 1 1 d . . . S6 S 0.50185(15) 0.77076(11) 0.29440(4) 0.0581(3) Uani 1 1 d . . . O14 O 0.6521(6) 0.9043(4) 0.4355(3) 0.127(2) Uani 1 1 d . . . O15 O 0.1233(4) 0.9763(3) 0.36139(17) 0.0790(10) Uani 1 1 d . . . O16 O 0.5665(5) 0.8742(3) 0.26502(15) 0.0774(9) Uani 1 1 d . . . C11 C 0.7715(6) 0.6641(5) 0.4788(2) 0.0748(13) Uani 1 1 d . . . H11A H 0.6937 0.6679 0.5139 0.112 Uiso 1 1 calc R . . H11B H 0.8684 0.6794 0.4882 0.112 Uiso 1 1 calc R . . H11C H 0.8039 0.5817 0.4669 0.112 Uiso 1 1 calc R . . C12 C 0.8463(7) 0.7530(8) 0.3629(3) 0.123(3) Uani 1 1 d . . . H12A H 0.8141 0.8104 0.3261 0.185 Uiso 1 1 calc R . . H12B H 0.8779 0.6672 0.3553 0.185 Uiso 1 1 calc R . . H12C H 0.9390 0.7662 0.3771 0.185 Uiso 1 1 calc R . . C13 C 0.6376(9) 0.6318(5) 0.2667(2) 0.0914(18) Uani 1 1 d . . . H13A H 0.7445 0.6078 0.2827 0.137 Uiso 1 1 calc R . . H13B H 0.6506 0.6483 0.2232 0.137 Uiso 1 1 calc R . . H13C H 0.5912 0.5643 0.2791 0.137 Uiso 1 1 calc R . . C14 C 0.3182(8) 0.7926(6) 0.2589(2) 0.0905(17) Uani 1 1 d . . . H14A H 0.2308 0.8658 0.2706 0.136 Uiso 1 1 calc R . . H14B H 0.2837 0.7190 0.2713 0.136 Uiso 1 1 calc R . . H14C H 0.3407 0.8050 0.2156 0.136 Uiso 1 1 calc R . . C15 C 0.2231(8) 0.9952(5) 0.4631(2) 0.0884(18) Uani 1 1 d . . . H15A H 0.1722 0.9385 0.4889 0.133 Uiso 1 1 calc R . . H15B H 0.1454 1.0800 0.4595 0.133 Uiso 1 1 calc R . . H15C H 0.3210 0.9925 0.4805 0.133 Uiso 1 1 calc R . . C16 C 0.3657(7) 1.0661(5) 0.3529(3) 0.0890(17) Uani 1 1 d . . . H16A H 0.4032 1.0517 0.3119 0.134 Uiso 1 1 calc R . . H16B H 0.4584 1.0624 0.3738 0.134 Uiso 1 1 calc R . . H16C H 0.2824 1.1483 0.3526 0.134 Uiso 1 1 calc R . . O5 O 0.4346(4) 0.4594(3) 0.37999(17) 0.0731(9) Uani 1 1 d D . . O6 O 0.6028(3) 0.5508(2) 0.40507(12) 0.0515(6) Uani 1 1 d . . . O7 O 0.5926(3) 0.2931(3) 0.50902(11) 0.0498(6) Uani 1 1 d . . . O8 O 0.8574(4) 0.2924(4) 0.49907(15) 0.0712(8) Uani 1 1 d . . . C17 C 0.5681(5) 0.4551(4) 0.39704(16) 0.0504(8) Uani 1 1 d . . . C18 C 0.7098(5) 0.3276(4) 0.40887(18) 0.0560(10) Uani 1 1 d . . . C19 C 0.7255(5) 0.3026(4) 0.47779(18) 0.0520(9) Uani 1 1 d . . . C22 C 0.8717(7) 0.3376(5) 0.3739(2) 0.0811(16) Uani 1 1 d . . . H22A H 0.8658 0.3380 0.3315 0.122 Uiso 1 1 calc R . . H22B H 0.9639 0.2664 0.3889 0.122 Uiso 1 1 calc R . . H22C H 0.8870 0.4148 0.3792 0.122 Uiso 1 1 calc R . . C23 C 0.6650(8) 0.2196(4) 0.3913(2) 0.0772(15) Uani 1 1 d . . . H23A H 0.5632 0.2142 0.4137 0.116 Uiso 1 1 calc R . . H23B H 0.7532 0.1409 0.4006 0.116 Uiso 1 1 calc R . . H23C H 0.6505 0.2361 0.3486 0.116 Uiso 1 1 calc R . . O3W O 0.2155(16) 0.4494(14) 0.2712(6) 0.177(6) Uani 0.50 1 d P . . O4W O 0.5448(14) 0.8043(13) 0.1105(6) 0.141(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.04199(17) 0.04369(16) 0.03988(16) -0.00770(11) -0.00361(11) -0.01316(12) O1W 0.0465(13) 0.0568(15) 0.0528(15) -0.0073(12) -0.0074(11) -0.0187(12) S1 0.0421(5) 0.0609(6) 0.0576(5) -0.0098(4) -0.0050(4) -0.0140(4) S2 0.0576(6) 0.0605(6) 0.0403(4) -0.0100(4) -0.0037(4) -0.0158(4) S3 0.0621(6) 0.0444(5) 0.0562(5) -0.0099(4) -0.0100(4) -0.0136(4) O11 0.071(2) 0.069(2) 0.155(4) 0.001(2) -0.049(2) -0.0093(19) O12 0.082(2) 0.095(2) 0.0501(17) -0.0257(16) 0.0046(15) -0.0043(19) O13 0.088(2) 0.0590(18) 0.086(2) -0.0103(15) -0.0292(18) -0.0320(17) C1 0.059(3) 0.106(4) 0.090(4) -0.040(3) -0.006(2) -0.035(3) C2 0.073(3) 0.206(8) 0.068(3) -0.016(4) 0.008(3) -0.075(5) C3 0.099(4) 0.079(3) 0.050(2) 0.004(2) -0.010(2) -0.043(3) C4 0.088(3) 0.084(3) 0.055(2) -0.009(2) -0.023(2) -0.034(3) C5 0.096(4) 0.048(2) 0.070(3) 0.0007(19) -0.027(2) -0.018(2) C6 0.085(3) 0.060(3) 0.102(4) -0.035(3) 0.006(3) -0.006(2) O1 0.0587(17) 0.076(2) 0.0583(17) -0.0056(14) -0.0027(13) -0.0322(15) O2 0.0514(14) 0.0582(15) 0.0404(13) -0.0085(11) -0.0016(10) -0.0197(12) O3 0.0533(14) 0.0440(13) 0.0557(15) -0.0079(11) -0.0064(11) -0.0148(11) O4 0.0580(17) 0.0536(16) 0.090(2) -0.0079(15) -0.0168(15) -0.0147(14) C7 0.053(2) 0.0382(17) 0.0453(18) -0.0041(13) -0.0002(15) -0.0131(15) C8 0.067(2) 0.0465(19) 0.0417(19) -0.0040(15) 0.0022(16) -0.0192(18) C9 0.057(2) 0.0470(19) 0.0389(17) -0.0039(14) -0.0027(15) -0.0130(17) C20 0.110(4) 0.065(3) 0.054(2) -0.013(2) 0.024(2) -0.045(3) C21 0.087(3) 0.047(2) 0.057(2) -0.0033(17) -0.020(2) -0.003(2) Ru2 0.04233(17) 0.04465(17) 0.04180(16) -0.00311(11) -0.00652(11) -0.01576(12) O2W 0.0507(15) 0.0610(16) 0.0591(16) -0.0021(13) -0.0145(13) -0.0225(13) S4 0.0497(5) 0.0566(6) 0.0807(7) -0.0020(5) -0.0186(5) -0.0229(5) S5 0.0550(5) 0.0470(5) 0.0585(6) -0.0020(4) -0.0140(4) -0.0121(4) S6 0.0724(7) 0.0593(6) 0.0426(5) -0.0009(4) -0.0030(4) -0.0254(5) O14 0.108(3) 0.069(2) 0.227(6) -0.042(3) -0.082(4) -0.021(2) O15 0.075(2) 0.0638(19) 0.093(3) -0.0051(17) -0.0391(19) -0.0086(17) O16 0.101(3) 0.072(2) 0.0628(19) 0.0074(15) 0.0022(17) -0.0451(19) C11 0.064(3) 0.092(4) 0.074(3) 0.007(2) -0.027(2) -0.035(3) C12 0.053(3) 0.196(8) 0.104(5) 0.050(5) -0.012(3) -0.056(4) C13 0.125(5) 0.080(3) 0.057(3) -0.018(2) 0.024(3) -0.025(3) C14 0.115(5) 0.111(4) 0.058(3) 0.001(3) -0.030(3) -0.052(4) C15 0.108(4) 0.059(3) 0.080(3) -0.024(2) -0.018(3) 0.007(3) C16 0.086(4) 0.050(3) 0.118(5) 0.008(3) 0.001(3) -0.020(2) O5 0.074(2) 0.0587(18) 0.095(2) -0.0150(16) -0.0274(18) -0.0225(16) O6 0.0507(14) 0.0471(14) 0.0548(15) -0.0072(11) -0.0063(11) -0.0130(11) O7 0.0489(14) 0.0576(15) 0.0403(13) -0.0036(11) -0.0031(10) -0.0160(12) O8 0.0502(16) 0.097(2) 0.0666(19) -0.0098(17) -0.0023(14) -0.0264(16) C17 0.060(2) 0.050(2) 0.0401(18) -0.0056(14) -0.0020(15) -0.0181(17) C18 0.065(2) 0.046(2) 0.046(2) -0.0071(15) 0.0033(17) -0.0071(17) C19 0.054(2) 0.0469(19) 0.050(2) -0.0068(15) 0.0016(16) -0.0122(16) C22 0.078(3) 0.070(3) 0.066(3) 0.000(2) 0.023(2) -0.003(2) C23 0.128(4) 0.052(2) 0.050(2) -0.0128(18) -0.006(2) -0.025(3) O3W 0.121(9) 0.206(13) 0.178(12) 0.098(10) -0.059(8) -0.068(9) O4W 0.104(7) 0.165(10) 0.147(10) -0.005(8) -0.007(7) -0.047(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O2 2.107(2) . ? Ru1 O3 2.115(3) 2_577 ? Ru1 O1W 2.155(3) . ? Ru1 S2 2.2415(10) . ? Ru1 S1 2.2648(13) . ? Ru1 S3 2.2795(12) . ? S1 O11 1.465(4) . ? S1 C1 1.761(5) . ? S1 C2 1.767(6) . ? S2 O12 1.477(3) . ? S2 C3 1.782(5) . ? S2 C4 1.782(5) . ? S3 O13 1.483(3) . ? S3 C5 1.782(5) . ? S3 C6 1.783(5) . ? O1 C7 1.237(5) . ? O2 C7 1.272(5) . ? O3 C9 1.265(4) . ? O3 Ru1 2.115(3) 2_577 ? O4 C9 1.245(5) . ? C7 C8 1.531(5) . ? C8 C21 1.521(6) . ? C8 C20 1.529(6) . ? C8 C9 1.544(5) . ? Ru2 O6 2.110(3) . ? Ru2 O7 2.112(2) 2_666 ? Ru2 O2W 2.143(3) . ? Ru2 S6 2.2461(11) . ? Ru2 S4 2.2602(12) . ? Ru2 S5 2.2810(12) . ? S4 O14 1.458(4) . ? S4 C12 1.767(6) . ? S4 C11 1.771(5) . ? S5 O15 1.475(3) . ? S5 C16 1.769(5) . ? S5 C15 1.771(5) . ? S6 O16 1.475(3) . ? S6 C13 1.775(5) . ? S6 C14 1.779(5) . ? O5 C17 1.236(5) . ? O6 C17 1.269(5) . ? O8 C19 1.245(5) . ? O7 C19 1.280(5) . ? O7 Ru2 2.112(2) 2_666 ? C17 C18 1.541(5) . ? C18 C22 1.527(7) . ? C18 C23 1.534(7) . ? C18 C19 1.539(6) . ? 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 O2 Ru1 O3 84.89(11) . 2_577 ? O2 Ru1 O1W 88.26(11) . . ? O3 Ru1 O1W 89.68(11) 2_577 . ? O2 Ru1 S2 177.80(8) . . ? O3 Ru1 S2 92.96(8) 2_577 . ? O1W Ru1 S2 91.28(8) . . ? O2 Ru1 S1 82.89(8) . . ? O3 Ru1 S1 86.02(8) 2_577 . ? O1W Ru1 S1 170.46(8) . . ? S2 Ru1 S1 97.43(4) . . ? O2 Ru1 S3 92.26(9) . . ? O3 Ru1 S3 176.82(8) 2_577 . ? O1W Ru1 S3 88.81(8) . . ? S2 Ru1 S3 89.88(5) . . ? S1 Ru1 S3 95.05(5) . . ? O11 S1 C1 106.7(3) . . ? O11 S1 C2 106.6(3) . . ? C1 S1 C2 99.0(3) . . ? O11 S1 Ru1 116.59(18) . . ? C1 S1 Ru1 109.15(17) . . ? C2 S1 Ru1 116.9(2) . . ? O12 S2 C3 105.5(3) . . ? O12 S2 C4 107.8(2) . . ? C3 S2 C4 98.9(2) . . ? O12 S2 Ru1 118.99(14) . . ? C3 S2 Ru1 114.11(18) . . ? C4 S2 Ru1 109.61(17) . . ? O13 S3 C5 108.2(2) . . ? O13 S3 C6 107.1(3) . . ? C5 S3 C6 98.5(3) . . ? O13 S3 Ru1 113.78(14) . . ? C5 S3 Ru1 112.33(17) . . ? C6 S3 Ru1 115.7(2) . . ? C7 O2 Ru1 130.9(3) . . ? C9 O3 Ru1 128.9(3) . 2_577 ? O1 C7 O2 125.2(4) . . ? O1 C7 C8 121.8(4) . . ? O2 C7 C8 113.0(3) . . ? C21 C8 C20 109.5(4) . . ? C21 C8 C7 109.4(3) . . ? C20 C8 C7 111.3(4) . . ? C21 C8 C9 111.7(4) . . ? C20 C8 C9 109.4(3) . . ? C7 C8 C9 105.5(3) . . ? O4 C9 O3 125.1(4) . . ? O4 C9 C8 120.4(3) . . ? O3 C9 C8 114.5(3) . . ? O6 Ru2 O7 84.59(11) . 2_666 ? O6 Ru2 O2W 90.16(11) . . ? O7 Ru2 O2W 88.74(11) 2_666 . ? O6 Ru2 S6 92.66(8) . . ? O7 Ru2 S6 177.15(8) 2_666 . ? O2W Ru2 S6 90.53(9) . . ? O6 Ru2 S4 85.52(8) . . ? O7 Ru2 S4 83.35(8) 2_666 . ? O2W Ru2 S4 171.30(8) . . ? S6 Ru2 S4 97.20(5) . . ? O6 Ru2 S5 176.98(8) . . ? O7 Ru2 S5 92.59(8) 2_666 . ? O2W Ru2 S5 88.72(9) . . ? S6 Ru2 S5 90.15(5) . . ? S4 Ru2 S5 95.22(5) . . ? O14 S4 C12 107.0(4) . . ? O14 S4 C11 107.1(3) . . ? C12 S4 C11 98.9(3) . . ? O14 S4 Ru2 117.99(19) . . ? C12 S4 Ru2 114.7(3) . . ? C11 S4 Ru2 109.28(17) . . ? O15 S5 C16 104.9(3) . . ? O15 S5 C15 107.2(3) . . ? C16 S5 C15 100.4(3) . . ? O15 S5 Ru2 114.61(15) . . ? C16 S5 Ru2 116.62(19) . . ? C15 S5 Ru2 111.75(17) . . ? O16 S6 C13 106.0(3) . . ? O16 S6 C14 106.9(3) . . ? C13 S6 C14 100.1(3) . . ? O16 S6 Ru2 118.90(16) . . ? C13 S6 Ru2 113.25(19) . . ? C14 S6 Ru2 109.9(2) . . ? C17 O6 Ru2 128.7(2) . . ? C19 O7 Ru2 128.5(3) . 2_666 ? O5 C17 O6 124.8(4) . . ? O5 C17 C18 120.5(4) . . ? O6 C17 C18 114.7(4) . . ? C22 C18 C23 110.4(4) . . ? C22 C18 C19 111.2(4) . . ? C23 C18 C19 108.8(3) . . ? C22 C18 C17 110.0(3) . . ? C23 C18 C17 111.2(4) . . ? C19 C18 C17 105.2(3) . . ? O8 C19 O7 125.3(4) . . ? O8 C19 C18 121.4(4) . . ? O7 C19 C18 113.3(4) . . ? 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 O2 Ru1 S1 O11 74.4(2) . . . . ? O3 Ru1 S1 O11 159.7(2) 2_577 . . . ? O1W Ru1 S1 O11 96.3(5) . . . . ? S2 Ru1 S1 O11 -107.8(2) . . . . ? S3 Ru1 S1 O11 -17.3(2) . . . . ? O2 Ru1 S1 C1 -46.6(2) . . . . ? O3 Ru1 S1 C1 38.8(2) 2_577 . . . ? O1W Ru1 S1 C1 -24.6(5) . . . . ? S2 Ru1 S1 C1 131.2(2) . . . . ? S3 Ru1 S1 C1 -138.2(2) . . . . ? O2 Ru1 S1 C2 -157.8(3) . . . . ? O3 Ru1 S1 C2 -72.5(3) 2_577 . . . ? O1W Ru1 S1 C2 -135.8(6) . . . . ? S2 Ru1 S1 C2 20.0(3) . . . . ? S3 Ru1 S1 C2 110.5(3) . . . . ? O2 Ru1 S2 O12 142.0(19) . . . . ? O3 Ru1 S2 O12 130.1(2) 2_577 . . . ? O1W Ru1 S2 O12 -140.2(2) . . . . ? S1 Ru1 S2 O12 43.7(2) . . . . ? S3 Ru1 S2 O12 -51.4(2) . . . . ? O2 Ru1 S2 C3 16(2) . . . . ? O3 Ru1 S2 C3 4.5(2) 2_577 . . . ? O1W Ru1 S2 C3 94.3(2) . . . . ? S1 Ru1 S2 C3 -81.9(2) . . . . ? S3 Ru1 S2 C3 -176.9(2) . . . . ? O2 Ru1 S2 C4 -93.4(19) . . . . ? O3 Ru1 S2 C4 -105.3(2) 2_577 . . . ? O1W Ru1 S2 C4 -15.6(2) . . . . ? S1 Ru1 S2 C4 168.3(2) . . . . ? S3 Ru1 S2 C4 73.2(2) . . . . ? O2 Ru1 S3 O13 113.21(19) . . . . ? O3 Ru1 S3 O13 86.8(14) 2_577 . . . ? O1W Ru1 S3 O13 25.00(19) . . . . ? S2 Ru1 S3 O13 -66.28(18) . . . . ? S1 Ru1 S3 O13 -163.74(18) . . . . ? O2 Ru1 S3 C5 -10.1(2) . . . . ? O3 Ru1 S3 C5 -36.6(14) 2_577 . . . ? O1W Ru1 S3 C5 -98.4(2) . . . . ? S2 Ru1 S3 C5 170.4(2) . . . . ? S1 Ru1 S3 C5 72.9(2) . . . . ? O2 Ru1 S3 C6 -122.2(2) . . . . ? O3 Ru1 S3 C6 -148.6(14) 2_577 . . . ? O1W Ru1 S3 C6 149.6(2) . . . . ? S2 Ru1 S3 C6 58.3(2) . . . . ? S1 Ru1 S3 C6 -39.1(2) . . . . ? O3 Ru1 O2 C7 105.7(3) 2_577 . . . ? O1W Ru1 O2 C7 15.9(3) . . . . ? S2 Ru1 O2 C7 94(2) . . . . ? S1 Ru1 O2 C7 -167.7(3) . . . . ? S3 Ru1 O2 C7 -72.9(3) . . . . ? Ru1 O2 C7 O1 -2.8(6) . . . . ? Ru1 O2 C7 C8 176.5(2) . . . . ? O1 C7 C8 C21 125.2(4) . . . . ? O2 C7 C8 C21 -54.1(5) . . . . ? O1 C7 C8 C20 4.0(5) . . . . ? O2 C7 C8 C20 -175.3(3) . . . . ? O1 C7 C8 C9 -114.5(4) . . . . ? O2 C7 C8 C9 66.2(4) . . . . ? Ru1 O3 C9 O4 3.0(6) 2_577 . . . ? Ru1 O3 C9 C8 -176.7(2) 2_577 . . . ? C21 C8 C9 O4 2.7(5) . . . . ? C20 C8 C9 O4 124.1(4) . . . . ? C7 C8 C9 O4 -116.1(4) . . . . ? C21 C8 C9 O3 -177.5(3) . . . . ? C20 C8 C9 O3 -56.1(5) . . . . ? C7 C8 C9 O3 63.7(4) . . . . ? O6 Ru2 S4 O14 -165.1(3) . . . . ? O7 Ru2 S4 O14 -80.0(3) 2_666 . . . ? O2W Ru2 S4 O14 -104.7(7) . . . . ? S6 Ru2 S4 O14 102.8(3) . . . . ? S5 Ru2 S4 O14 12.0(3) . . . . ? O6 Ru2 S4 C12 67.4(3) . . . . ? O7 Ru2 S4 C12 152.5(3) 2_666 . . . ? O2W Ru2 S4 C12 127.8(6) . . . . ? S6 Ru2 S4 C12 -24.7(3) . . . . ? S5 Ru2 S4 C12 -115.5(3) . . . . ? O6 Ru2 S4 C11 -42.5(2) . . . . ? O7 Ru2 S4 C11 42.5(2) 2_666 . . . ? O2W Ru2 S4 C11 17.9(6) . . . . ? S6 Ru2 S4 C11 -134.6(2) . . . . ? S5 Ru2 S4 C11 134.5(2) . . . . ? O6 Ru2 S5 O15 -90.3(15) . . . . ? O7 Ru2 S5 O15 -110.8(2) 2_666 . . . ? O2W Ru2 S5 O15 -22.1(2) . . . . ? S6 Ru2 S5 O15 68.40(19) . . . . ? S4 Ru2 S5 O15 165.64(19) . . . . ? O6 Ru2 S5 C16 146.6(15) . . . . ? O7 Ru2 S5 C16 126.1(3) 2_666 . . . ? O2W Ru2 S5 C16 -145.2(3) . . . . ? S6 Ru2 S5 C16 -54.7(3) . . . . ? S4 Ru2 S5 C16 42.6(3) . . . . ? O6 Ru2 S5 C15 31.9(15) . . . . ? O7 Ru2 S5 C15 11.4(3) 2_666 . . . ? O2W Ru2 S5 C15 100.1(3) . . . . ? S6 Ru2 S5 C15 -169.4(3) . . . . ? S4 Ru2 S5 C15 -72.1(3) . . . . ? O6 Ru2 S6 O16 -125.61(19) . . . . ? O7 Ru2 S6 O16 -140.7(15) 2_666 . . . ? O2W Ru2 S6 O16 144.2(2) . . . . ? S4 Ru2 S6 O16 -39.79(19) . . . . ? S5 Ru2 S6 O16 55.49(18) . . . . ? O6 Ru2 S6 C13 -0.2(3) . . . . ? O7 Ru2 S6 C13 -15.2(15) 2_666 . . . ? O2W Ru2 S6 C13 -90.3(3) . . . . ? S4 Ru2 S6 C13 85.6(3) . . . . ? S5 Ru2 S6 C13 -179.1(3) . . . . ? O6 Ru2 S6 C14 110.8(2) . . . . ? O7 Ru2 S6 C14 95.8(15) 2_666 . . . ? O2W Ru2 S6 C14 20.6(3) . . . . ? S4 Ru2 S6 C14 -163.4(2) . . . . ? S5 Ru2 S6 C14 -68.1(2) . . . . ? O7 Ru2 O6 C17 98.8(3) 2_666 . . . ? O2W Ru2 O6 C17 10.0(3) . . . . ? S6 Ru2 O6 C17 -80.5(3) . . . . ? S4 Ru2 O6 C17 -177.5(3) . . . . ? S5 Ru2 O6 C17 78.2(16) . . . . ? Ru2 O6 C17 O5 2.1(6) . . . . ? Ru2 O6 C17 C18 -179.2(2) . . . . ? O5 C17 C18 C22 127.7(5) . . . . ? O6 C17 C18 C22 -51.1(5) . . . . ? O5 C17 C18 C23 5.1(5) . . . . ? O6 C17 C18 C23 -173.6(3) . . . . ? O5 C17 C18 C19 -112.6(4) . . . . ? O6 C17 C18 C19 68.7(4) . . . . ? Ru2 O7 C19 O8 -0.4(6) 2_666 . . . ? Ru2 O7 C19 C18 179.1(2) 2_666 . . . ? C22 C18 C19 O8 -0.3(5) . . . . ? C23 C18 C19 O8 121.5(5) . . . . ? C17 C18 C19 O8 -119.3(4) . . . . ? C22 C18 C19 O7 -179.9(4) . . . . ? C23 C18 C19 O7 -58.1(5) . . . . ? C17 C18 C19 O7 61.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 1.376 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.126 #===END data_13 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis[aquo-tris(dimethylsulfoxide,S)-(mu-succinate,O,O')- -ruthenium(II)] ethanol solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H60 O18 Ru2 S6, 2(C2 H6 O)' _chemical_formula_sum 'C24 H60 O18 Ru2 S6' _chemical_formula_weight 1031.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.336(3) _cell_length_b 9.723(3) _cell_length_c 13.185(5) _cell_angle_alpha 102.45(4) _cell_angle_beta 101.29(5) _cell_angle_gamma 95.31(4) _cell_volume 1013.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 9.524 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.0579 _exptl_absorpt_correction_T_max 0.1266 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa-CCD' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14863 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 64.79 _reflns_number_total 3108 _reflns_number_gt 2701 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1053P)^2^+34.5800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3108 _refine_ls_number_parameters 235 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.2396 _refine_ls_wR_factor_gt 0.2314 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.132 _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 Ru Ru 0.12259(14) 0.13503(11) 0.25929(8) 0.0296(4) Uani 1 1 d . . . O1W O -0.0454(14) -0.0237(13) 0.2892(8) 0.040(3) Uani 1 1 d . . . H2W H -0.010(15) -0.096(2) 0.257(13) 0.13(12) Uiso 1 1 d D . . H1W H -0.131(6) -0.014(14) 0.245(11) 0.07(7) Uiso 1 1 d D . . S1 S 0.2833(5) 0.2937(4) 0.2060(3) 0.0346(9) Uani 1 1 d . . . S2 S 0.0463(5) 0.2954(4) 0.3844(3) 0.0351(9) Uani 1 1 d . . . S3 S 0.3309(5) 0.0902(4) 0.3810(3) 0.0362(9) Uani 1 1 d . . . O2 O 0.1828(13) -0.0209(10) 0.1365(7) 0.034(2) Uani 1 1 d . . . O1 O 0.0819(15) -0.2186(11) 0.1787(9) 0.046(3) Uani 1 1 d . . . O3 O -0.0612(13) 0.1713(10) 0.1363(7) 0.034(2) Uani 1 1 d . . . O4 O -0.2796(13) 0.0207(12) 0.1446(8) 0.044(3) Uani 1 1 d . . . C1 C 0.157(2) -0.1569(16) 0.1253(12) 0.039(4) Uani 1 1 d . . . C2 C 0.233(2) -0.2468(16) 0.0436(12) 0.039(4) Uani 1 1 d . . . H2A H 0.3123 -0.2965 0.0804 0.047 Uiso 1 1 calc R . . H2B H 0.1466 -0.3182 -0.0044 0.047 Uiso 1 1 calc R . . C3 C -0.319(2) 0.1684(17) 0.0227(12) 0.041(4) Uani 1 1 d . . . H3A H -0.3863 0.2316 0.0574 0.049 Uiso 1 1 calc R . . H3B H -0.3941 0.0881 -0.0253 0.049 Uiso 1 1 calc R . . C4 C -0.213(2) 0.1143(16) 0.1060(11) 0.038(4) Uani 1 1 d . . . C5 C 0.254(2) 0.2392(19) 0.0644(13) 0.046(4) Uani 1 1 d . . . H5A H 0.2911 0.1484 0.0454 0.070 Uiso 1 1 calc R . . H5B H 0.3166 0.3081 0.0397 0.070 Uiso 1 1 calc R . . H5C H 0.1391 0.2317 0.0319 0.070 Uiso 1 1 calc R . . C6 C 0.209(2) 0.4626(17) 0.2172(17) 0.054(5) Uani 1 1 d . . . H6A H 0.2164 0.5060 0.2909 0.081 Uiso 1 1 calc R . . H6B H 0.0963 0.4490 0.1789 0.081 Uiso 1 1 calc R . . H6C H 0.2754 0.5232 0.1880 0.081 Uiso 1 1 calc R . . C7 C -0.142(2) 0.3530(19) 0.3327(15) 0.052(4) Uani 1 1 d . . . H7A H -0.1277 0.3998 0.2774 0.078 Uiso 1 1 calc R . . H7B H -0.1740 0.4180 0.3887 0.078 Uiso 1 1 calc R . . H7C H -0.2268 0.2723 0.3041 0.078 Uiso 1 1 calc R . . C8 C -0.015(2) 0.215(2) 0.4825(14) 0.052(4) Uani 1 1 d . . . H8A H 0.0777 0.1786 0.5185 0.078 Uiso 1 1 calc R . . H8B H -0.1028 0.1381 0.4487 0.078 Uiso 1 1 calc R . . H8C H -0.0517 0.2842 0.5331 0.078 Uiso 1 1 calc R . . C9 C 0.4808(19) 0.0067(18) 0.3162(14) 0.044(4) Uani 1 1 d . . . H9A H 0.4272 -0.0792 0.2651 0.066 Uiso 1 1 calc R . . H9B H 0.5655 -0.0156 0.3684 0.066 Uiso 1 1 calc R . . H9C H 0.5294 0.0704 0.2806 0.066 Uiso 1 1 calc R . . C10 C 0.465(2) 0.2404(17) 0.4681(13) 0.043(4) Uani 1 1 d . . . H10A H 0.4027 0.2985 0.5097 0.064 Uiso 1 1 calc R . . H10B H 0.5149 0.2950 0.4269 0.064 Uiso 1 1 calc R . . H10C H 0.5497 0.2088 0.5146 0.064 Uiso 1 1 calc R . . O11 O 0.4649(13) 0.3241(14) 0.2494(9) 0.047(3) Uani 1 1 d . . . O12 O 0.1649(13) 0.4239(11) 0.4426(9) 0.043(3) Uani 1 1 d . . . O13 O 0.2796(14) 0.0009(13) 0.4494(9) 0.049(3) Uani 1 1 d . . . O5 O 0.818(2) 0.5555(14) 0.1380(14) 0.073(4) Uani 1 1 d . . . H5 H 0.8803 0.6223 0.1324 0.110 Uiso 1 1 calc R . . C11 C 0.670(3) 0.602(3) 0.1554(17) 0.078(7) Uani 1 1 d . . . H11A H 0.5835 0.5211 0.1261 0.093 Uiso 1 1 calc R . . H11B H 0.6465 0.6715 0.1141 0.093 Uiso 1 1 calc R . . C12 C 0.657(3) 0.6635(17) 0.2640(15) 0.061(5) Uani 1 1 d . . . H12A H 0.5492 0.6918 0.2629 0.091 Uiso 1 1 calc R . . H12B H 0.7396 0.7452 0.2946 0.091 Uiso 1 1 calc R . . H12C H 0.6725 0.5944 0.3058 0.091 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 Ru 0.0309(7) 0.0306(6) 0.0279(6) 0.0085(4) 0.0075(4) 0.0023(4) O1W 0.039(6) 0.053(7) 0.025(5) 0.010(5) 0.009(5) -0.020(5) S1 0.037(2) 0.0309(18) 0.0375(19) 0.0110(14) 0.0087(16) 0.0025(15) S2 0.035(2) 0.0362(19) 0.0318(18) 0.0030(14) 0.0081(15) 0.0025(15) S3 0.040(2) 0.041(2) 0.0296(17) 0.0130(15) 0.0066(15) 0.0081(16) O2 0.041(6) 0.031(5) 0.029(5) 0.004(4) 0.010(4) 0.006(4) O1 0.052(7) 0.039(6) 0.055(7) 0.018(5) 0.026(6) 0.001(5) O3 0.038(6) 0.039(5) 0.024(5) 0.012(4) 0.001(4) 0.003(5) O4 0.036(6) 0.053(7) 0.040(6) 0.013(5) 0.009(5) -0.015(5) C1 0.043(9) 0.032(8) 0.041(8) 0.009(7) -0.002(7) 0.011(7) C2 0.050(10) 0.036(8) 0.029(7) 0.008(6) 0.002(7) 0.009(7) C3 0.043(9) 0.040(8) 0.037(8) 0.003(7) 0.008(7) 0.014(7) C4 0.045(10) 0.039(8) 0.029(7) 0.003(6) 0.012(7) 0.013(7) C5 0.044(10) 0.058(10) 0.043(9) 0.024(8) 0.016(8) -0.005(8) C6 0.048(11) 0.039(9) 0.090(14) 0.035(9) 0.030(10) 0.007(8) C7 0.047(10) 0.045(9) 0.060(11) -0.001(8) 0.013(9) 0.018(8) C8 0.056(11) 0.056(11) 0.045(10) 0.011(8) 0.015(8) 0.010(9) C9 0.023(8) 0.053(10) 0.054(10) 0.014(8) 0.004(7) 0.004(7) C10 0.036(9) 0.047(9) 0.042(9) 0.013(7) 0.006(7) -0.002(7) O11 0.024(6) 0.076(8) 0.048(6) 0.027(6) 0.010(5) 0.006(5) O12 0.030(6) 0.043(6) 0.048(6) -0.004(5) 0.011(5) -0.002(5) O13 0.036(6) 0.066(7) 0.047(6) 0.030(6) 0.002(5) -0.003(5) O5 0.078(11) 0.042(7) 0.098(11) 0.007(7) 0.032(9) -0.001(7) C11 0.048(13) 0.13(2) 0.054(12) 0.018(13) 0.016(10) 0.001(13) C12 0.083(14) 0.022(8) 0.067(12) 0.007(8) -0.004(10) 0.007(8) _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 Ru O3 2.115(9) . ? Ru O2 2.138(9) . ? Ru O1W 2.140(10) . ? Ru S2 2.246(4) . ? Ru S1 2.264(4) . ? Ru S3 2.265(4) . ? S1 O11 1.487(11) . ? S1 C5 1.788(16) . ? S1 C6 1.793(17) . ? S2 O12 1.479(11) . ? S2 C7 1.777(17) . ? S2 C8 1.778(18) . ? S3 O13 1.473(11) . ? S3 C10 1.782(16) . ? S3 C9 1.805(17) . ? O2 C1 1.292(18) . ? O1 C1 1.24(2) . ? O3 C4 1.280(19) . ? O4 C4 1.271(19) . ? C1 C2 1.51(2) . ? C2 C3 1.51(2) 2 ? C3 C4 1.49(2) . ? C3 C2 1.51(2) 2 ? O5 C11 1.39(3) . ? C11 C12 1.46(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ru O2 85.5(4) . . ? O3 Ru O1W 91.4(4) . . ? O2 Ru O1W 90.2(4) . . ? O3 Ru S2 92.4(3) . . ? O2 Ru S2 177.2(3) . . ? O1W Ru S2 88.0(4) . . ? O3 Ru S1 82.6(3) . . ? O2 Ru S1 85.4(3) . . ? O1W Ru S1 172.8(3) . . ? S2 Ru S1 96.12(14) . . ? O3 Ru S3 175.4(3) . . ? O2 Ru S3 90.4(3) . . ? O1W Ru S3 90.7(3) . . ? S2 Ru S3 91.76(14) . . ? S1 Ru S3 95.04(14) . . ? O11 S1 C5 106.3(8) . . ? O11 S1 C6 106.7(8) . . ? C5 S1 C6 99.6(9) . . ? O11 S1 Ru 121.1(5) . . ? C5 S1 Ru 108.2(6) . . ? C6 S1 Ru 112.6(6) . . ? O12 S2 C7 107.4(8) . . ? O12 S2 C8 106.6(8) . . ? C7 S2 C8 100.0(9) . . ? O12 S2 Ru 118.6(5) . . ? C7 S2 Ru 111.5(6) . . ? C8 S2 Ru 111.0(6) . . ? O13 S3 C10 106.2(7) . . ? O13 S3 C9 108.1(8) . . ? C10 S3 C9 98.6(8) . . ? O13 S3 Ru 115.2(5) . . ? C10 S3 Ru 116.8(6) . . ? C9 S3 Ru 110.5(5) . . ? C1 O2 Ru 125.5(10) . . ? C4 O3 Ru 127.9(9) . . ? O1 C1 O2 125.5(15) . . ? O1 C1 C2 117.8(13) . . ? O2 C1 C2 116.6(15) . . ? C3 C2 C1 116.4(13) 2 . ? C4 C3 C2 117.1(14) . 2 ? O4 C4 O3 125.1(14) . . ? O4 C4 C3 118.1(15) . . ? O3 C4 C3 116.7(14) . . ? O5 C11 C12 119.3(19) . . ? 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 O3 Ru S1 O11 -172.5(7) . . . . ? O2 Ru S1 O11 -86.5(7) . . . . ? O1W Ru S1 O11 -139(3) . . . . ? S2 Ru S1 O11 95.8(6) . . . . ? S3 Ru S1 O11 3.5(6) . . . . ? O3 Ru S1 C5 -49.5(7) . . . . ? O2 Ru S1 C5 36.5(7) . . . . ? O1W Ru S1 C5 -16(3) . . . . ? S2 Ru S1 C5 -141.2(7) . . . . ? S3 Ru S1 C5 126.5(7) . . . . ? O3 Ru S1 C6 59.5(8) . . . . ? O2 Ru S1 C6 145.6(8) . . . . ? O1W Ru S1 C6 93(3) . . . . ? S2 Ru S1 C6 -32.1(8) . . . . ? S3 Ru S1 C6 -124.4(8) . . . . ? O3 Ru S2 O12 -115.6(6) . . . . ? O2 Ru S2 O12 -155(6) . . . . ? O1W Ru S2 O12 153.1(6) . . . . ? S1 Ru S2 O12 -32.8(6) . . . . ? S3 Ru S2 O12 62.5(6) . . . . ? O3 Ru S2 C7 9.9(8) . . . . ? O2 Ru S2 C7 -30(6) . . . . ? O1W Ru S2 C7 -81.4(8) . . . . ? S1 Ru S2 C7 92.7(7) . . . . ? S3 Ru S2 C7 -172.0(7) . . . . ? O3 Ru S2 C8 120.4(7) . . . . ? O2 Ru S2 C8 81(6) . . . . ? O1W Ru S2 C8 29.2(8) . . . . ? S1 Ru S2 C8 -156.7(7) . . . . ? S3 Ru S2 C8 -61.5(7) . . . . ? O3 Ru S3 O13 -128(4) . . . . ? O2 Ru S3 O13 -102.1(7) . . . . ? O1W Ru S3 O13 -11.9(7) . . . . ? S2 Ru S3 O13 76.2(6) . . . . ? S1 Ru S3 O13 172.5(6) . . . . ? O3 Ru S3 C10 106(4) . . . . ? O2 Ru S3 C10 132.2(7) . . . . ? O1W Ru S3 C10 -137.6(7) . . . . ? S2 Ru S3 C10 -49.5(7) . . . . ? S1 Ru S3 C10 46.8(7) . . . . ? O3 Ru S3 C9 -6(4) . . . . ? O2 Ru S3 C9 20.7(7) . . . . ? O1W Ru S3 C9 110.9(7) . . . . ? S2 Ru S3 C9 -161.0(6) . . . . ? S1 Ru S3 C9 -64.7(6) . . . . ? O3 Ru O2 C1 -110.1(11) . . . . ? O1W Ru O2 C1 -18.8(12) . . . . ? S2 Ru O2 C1 -70(6) . . . . ? S1 Ru O2 C1 166.9(11) . . . . ? S3 Ru O2 C1 71.9(11) . . . . ? O2 Ru O3 C4 93.1(11) . . . . ? O1W Ru O3 C4 3.0(12) . . . . ? S2 Ru O3 C4 -85.1(11) . . . . ? S1 Ru O3 C4 179.0(11) . . . . ? S3 Ru O3 C4 119(3) . . . . ? Ru O2 C1 O1 6(2) . . . . ? Ru O2 C1 C2 -170.7(9) . . . . ? O1 C1 C2 C3 178.3(14) . . . 2 ? O2 C1 C2 C3 -5(2) . . . 2 ? Ru O3 C4 O4 -2(2) . . . . ? Ru O3 C4 C3 175.1(9) . . . . ? C2 C3 C4 O4 -163.4(13) 2 . . . ? C2 C3 C4 O3 19.6(19) 2 . . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 64.79 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 1.358 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.264 #===END data_15 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (eta4-mu-oxalate,O,O',O'',O''')-bis[fac-tris(dimethylsulfoxide,S)- -chloride-ruthenium(II)] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H36 Cl2 O10 Ru2 S6' _chemical_formula_sum 'C14 H36 Cl2 O10 Ru2 S6' _chemical_formula_weight 829.83 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' 'Ru' 'Ru' -1.2594 0.8363 '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' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.446(2) _cell_length_b 8.548(2) _cell_length_c 10.609(3) _cell_angle_alpha 90.16(3) _cell_angle_beta 74.63(2) _cell_angle_gamma 80.47(2) _cell_volume 727.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 418 _exptl_absorpt_coefficient_mu 1.696 _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 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10817 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 31.06 _reflns_number_total 4191 _reflns_number_gt 3329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.64.05 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^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_number_reflns 4191 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _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 Ru Ru 0.26164(3) 0.21413(3) 0.67267(2) 0.03290(8) Uani 1 1 d . . . Cl1 Cl 0.21501(12) 0.28114(12) 0.46250(9) 0.0518(2) Uani 1 1 d . . . S1 S -0.00706(10) 0.19627(10) 0.76600(8) 0.03919(17) Uani 1 1 d . . . S2 S 0.24529(10) 0.46813(9) 0.73593(9) 0.04051(17) Uani 1 1 d . . . S3 S 0.34567(10) 0.13359(10) 0.85408(8) 0.03919(17) Uani 1 1 d . . . O1 O -0.0323(4) 0.0926(4) 0.8768(3) 0.0724(9) Uani 1 1 d . . . O2 O 0.1591(4) 0.5213(3) 0.8726(3) 0.0585(7) Uani 1 1 d . . . O3 O 0.5108(3) 0.1711(4) 0.8533(3) 0.0592(7) Uani 1 1 d . . . C1 C -0.1502(5) 0.3737(5) 0.8157(5) 0.0668(12) Uani 1 1 d . . . H1A H -0.2608 0.3499 0.8465 0.100 Uiso 1 1 calc R . . H1B H -0.1449 0.4410 0.7429 0.100 Uiso 1 1 calc R . . H1C H -0.1232 0.4271 0.8849 0.100 Uiso 1 1 calc R . . C2 C -0.0949(5) 0.1161(6) 0.6507(4) 0.0628(11) Uani 1 1 d . . . H2A H -0.0324 0.0129 0.6187 0.094 Uiso 1 1 calc R . . H2B H -0.0913 0.1849 0.5790 0.094 Uiso 1 1 calc R . . H2C H -0.2086 0.1072 0.6923 0.094 Uiso 1 1 calc R . . C3 C 0.1664(6) 0.6117(4) 0.6378(5) 0.0614(10) Uani 1 1 d . . . H3A H 0.0487 0.6147 0.6530 0.092 Uiso 1 1 calc R . . H3B H 0.2213 0.5841 0.5472 0.092 Uiso 1 1 calc R . . H3C H 0.1865 0.7142 0.6602 0.092 Uiso 1 1 calc R . . C4 C 0.4531(5) 0.5078(5) 0.7034(5) 0.0619(11) Uani 1 1 d . . . H4A H 0.4498 0.6174 0.7258 0.093 Uiso 1 1 calc R . . H4B H 0.5086 0.4856 0.6122 0.093 Uiso 1 1 calc R . . H4C H 0.5125 0.4416 0.7548 0.093 Uiso 1 1 calc R . . C5 C 0.2101(5) 0.2005(5) 1.0109(4) 0.0559(9) Uani 1 1 d . . . H5A H 0.2627 0.1631 1.0777 0.084 Uiso 1 1 calc R . . H5B H 0.1079 0.1599 1.0231 0.084 Uiso 1 1 calc R . . H5C H 0.1866 0.3145 1.0166 0.084 Uiso 1 1 calc R . . C6 C 0.3603(6) -0.0753(4) 0.8667(4) 0.0550(9) Uani 1 1 d . . . H6A H 0.4459 -0.1283 0.7936 0.083 Uiso 1 1 calc R . . H6B H 0.2556 -0.1050 0.8666 0.083 Uiso 1 1 calc R . . H6C H 0.3873 -0.1054 0.9466 0.083 Uiso 1 1 calc R . . C7 C 0.5619(4) 0.0597(3) 0.4909(3) 0.0338(6) Uani 1 1 d . . . O5 O 0.3043(3) -0.0256(3) 0.5974(2) 0.0387(5) Uani 1 1 d . . . O6 O 0.5186(3) 0.1834(3) 0.5641(2) 0.0375(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.03055(12) 0.03282(12) 0.03290(13) -0.00020(8) -0.00553(9) -0.00357(9) Cl1 0.0540(5) 0.0620(5) 0.0431(4) 0.0109(4) -0.0186(4) -0.0110(4) S1 0.0322(3) 0.0444(4) 0.0386(4) 0.0006(3) -0.0064(3) -0.0050(3) S2 0.0392(4) 0.0337(3) 0.0458(4) -0.0006(3) -0.0082(3) -0.0037(3) S3 0.0377(4) 0.0428(4) 0.0366(4) 0.0026(3) -0.0103(3) -0.0051(3) O1 0.0510(16) 0.098(2) 0.075(2) 0.0464(19) -0.0190(15) -0.0291(17) O2 0.0708(19) 0.0471(14) 0.0488(16) -0.0128(11) -0.0029(13) -0.0068(13) O3 0.0458(14) 0.086(2) 0.0567(17) 0.0160(15) -0.0229(13) -0.0266(15) C1 0.0400(19) 0.061(2) 0.090(3) -0.021(2) -0.009(2) 0.0009(18) C2 0.0460(19) 0.082(3) 0.062(3) -0.020(2) -0.0094(18) -0.027(2) C3 0.067(3) 0.0401(18) 0.079(3) 0.0126(18) -0.025(2) -0.0050(18) C4 0.0392(18) 0.053(2) 0.094(3) -0.005(2) -0.014(2) -0.0141(17) C5 0.062(2) 0.063(2) 0.0382(19) 0.0003(16) -0.0080(17) -0.0066(19) C6 0.067(2) 0.0446(18) 0.054(2) 0.0068(16) -0.0229(19) -0.0006(17) C7 0.0330(13) 0.0339(13) 0.0339(14) 0.0025(11) -0.0082(11) -0.0053(12) O5 0.0372(11) 0.0350(10) 0.0393(12) -0.0026(8) -0.0025(9) -0.0063(9) O6 0.0306(10) 0.0366(10) 0.0410(12) -0.0045(9) -0.0024(8) -0.0062(9) _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 Ru O5 2.136(2) . ? Ru O6 2.142(2) . ? Ru S2 2.2421(10) . ? Ru S1 2.2536(10) . ? Ru S3 2.2916(10) . ? Ru Cl1 2.4192(11) . ? S1 O1 1.466(3) . ? S1 C1 1.758(4) . ? S1 C2 1.778(4) . ? S2 O2 1.472(3) . ? S2 C3 1.771(4) . ? S2 C4 1.786(4) . ? S3 O3 1.480(3) . ? S3 C6 1.777(4) . ? S3 C5 1.782(4) . ? C7 O5 1.252(4) 2_656 ? C7 O6 1.254(4) . ? C7 C7 1.555(6) 2_656 ? O5 C7 1.252(4) 2_656 ? 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 O5 Ru O6 78.53(8) . . ? O5 Ru S2 173.43(6) . . ? O6 Ru S2 95.02(7) . . ? O5 Ru S1 89.45(7) . . ? O6 Ru S1 167.82(6) . . ? S2 Ru S1 96.95(4) . . ? O5 Ru S3 91.27(7) . . ? O6 Ru S3 88.65(7) . . ? S2 Ru S3 89.83(4) . . ? S1 Ru S3 93.63(4) . . ? O5 Ru Cl1 84.55(7) . . ? O6 Ru Cl1 83.09(7) . . ? S2 Ru Cl1 93.48(4) . . ? S1 Ru Cl1 93.91(4) . . ? S3 Ru Cl1 171.34(3) . . ? O1 S1 C1 107.0(2) . . ? O1 S1 C2 105.6(2) . . ? C1 S1 C2 100.0(2) . . ? O1 S1 Ru 114.34(12) . . ? C1 S1 Ru 117.95(16) . . ? C2 S1 Ru 110.40(14) . . ? O2 S2 C3 106.1(2) . . ? O2 S2 C4 107.5(2) . . ? C3 S2 C4 99.0(2) . . ? O2 S2 Ru 118.93(12) . . ? C3 S2 Ru 115.58(15) . . ? C4 S2 Ru 107.60(14) . . ? O3 S3 C6 106.8(2) . . ? O3 S3 C5 106.30(19) . . ? C6 S3 C5 100.3(2) . . ? O3 S3 Ru 113.27(12) . . ? C6 S3 Ru 110.83(14) . . ? C5 S3 Ru 118.10(14) . . ? O5 C7 O6 125.2(3) 2_656 . ? O5 C7 C7 117.3(3) 2_656 2_656 ? O6 C7 C7 117.5(3) . 2_656 ? C7 O5 Ru 112.32(18) 2_656 . ? C7 O6 Ru 112.01(18) . . ? 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 O5 Ru S1 O1 70.12(19) . . . . ? O6 Ru S1 O1 79.4(4) . . . . ? S2 Ru S1 O1 -111.39(18) . . . . ? S3 Ru S1 O1 -21.12(18) . . . . ? Cl1 Ru S1 O1 154.62(18) . . . . ? O5 Ru S1 C1 -162.8(2) . . . . ? O6 Ru S1 C1 -153.5(3) . . . . ? S2 Ru S1 C1 15.7(2) . . . . ? S3 Ru S1 C1 106.0(2) . . . . ? Cl1 Ru S1 C1 -78.3(2) . . . . ? O5 Ru S1 C2 -48.81(19) . . . . ? O6 Ru S1 C2 -39.5(4) . . . . ? S2 Ru S1 C2 129.68(19) . . . . ? S3 Ru S1 C2 -140.04(19) . . . . ? Cl1 Ru S1 C2 35.69(19) . . . . ? O5 Ru S2 O2 -147.2(6) . . . . ? O6 Ru S2 O2 -136.13(16) . . . . ? S1 Ru S2 O2 46.14(15) . . . . ? S3 Ru S2 O2 -47.50(15) . . . . ? Cl1 Ru S2 O2 140.51(15) . . . . ? O5 Ru S2 C3 84.8(6) . . . . ? O6 Ru S2 C3 95.86(19) . . . . ? S1 Ru S2 C3 -81.87(18) . . . . ? S3 Ru S2 C3 -175.51(18) . . . . ? Cl1 Ru S2 C3 12.50(18) . . . . ? O5 Ru S2 C4 -24.7(6) . . . . ? O6 Ru S2 C4 -13.67(18) . . . . ? S1 Ru S2 C4 168.60(17) . . . . ? S3 Ru S2 C4 74.96(18) . . . . ? Cl1 Ru S2 C4 -97.03(18) . . . . ? O5 Ru S3 O3 107.44(16) . . . . ? O6 Ru S3 O3 28.95(16) . . . . ? S2 Ru S3 O3 -66.08(15) . . . . ? S1 Ru S3 O3 -163.03(15) . . . . ? Cl1 Ru S3 O3 46.5(3) . . . . ? O5 Ru S3 C6 -12.51(17) . . . . ? O6 Ru S3 C6 -91.01(17) . . . . ? S2 Ru S3 C6 173.97(16) . . . . ? S1 Ru S3 C6 77.01(17) . . . . ? Cl1 Ru S3 C6 -73.5(3) . . . . ? O5 Ru S3 C5 -127.39(17) . . . . ? O6 Ru S3 C5 154.12(17) . . . . ? S2 Ru S3 C5 59.09(17) . . . . ? S1 Ru S3 C5 -37.86(16) . . . . ? Cl1 Ru S3 C5 171.6(2) . . . . ? O6 Ru O5 C7 -13.3(2) . . . 2_656 ? S2 Ru O5 C7 -2.1(7) . . . 2_656 ? S1 Ru O5 C7 164.7(2) . . . 2_656 ? S3 Ru O5 C7 -101.7(2) . . . 2_656 ? Cl1 Ru O5 C7 70.7(2) . . . 2_656 ? O5 C7 O6 Ru 168.3(2) 2_656 . . . ? C7 C7 O6 Ru -10.5(4) 2_656 . . . ? O5 Ru O6 C7 12.7(2) . . . . ? S2 Ru O6 C7 -166.0(2) . . . . ? S1 Ru O6 C7 3.2(5) . . . . ? S3 Ru O6 C7 104.2(2) . . . . ? Cl1 Ru O6 C7 -73.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 31.06 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 0.513 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.103 #===END data_17 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis[fac-tris(dimethylsulfoxide,S)-(dimethylsulfoxide,O)-(ruthenium(II))]- -(eta4-mu-oxalate,O,O',O'',O''') bis(triflate) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H48 O12 Ru2 S8 2+, 2(S O3 C F3 1-)' _chemical_formula_sum 'C20 H48 F6 O18 Ru2 S10' _chemical_formula_weight 1213.32 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' 'F' 'F' 0.0171 0.0103 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.345(4) _cell_length_b 13.192(3) _cell_length_c 13.618(4) _cell_angle_alpha 109.26(3) _cell_angle_beta 93.02(2) _cell_angle_gamma 92.23(3) _cell_volume 2256.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7085 _exptl_absorpt_correction_T_max 0.8132 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Linear fit to sin(theta)/lambda - 12 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25113 _diffrn_reflns_av_R_equivalents 0.0887 _diffrn_reflns_av_sigmaI/netI 0.1922 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7250 _reflns_number_gt 2880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^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_number_reflns 7250 _refine_ls_number_parameters 505 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1678 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1909 _refine_ls_wR_factor_gt 0.1615 _refine_ls_goodness_of_fit_ref 0.826 _refine_ls_restrained_S_all 0.848 _refine_ls_shift/su_max 0.009 _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 0.40144(7) 0.50661(8) 0.81893(7) 0.0571(3) Uani 1 1 d . . . S1 S 0.2403(2) 0.5231(3) 0.7785(3) 0.0684(9) Uani 1 1 d . . . S2 S 0.4508(2) 0.5080(3) 0.6632(2) 0.0638(9) Uani 1 1 d . . . S3 S 0.3842(3) 0.3250(3) 0.7688(3) 0.0728(10) Uani 1 1 d . . . S4 S 0.4743(3) 0.7426(3) 0.9815(3) 0.0733(10) Uani 1 1 d . . . O1 O 0.2034(6) 0.4852(7) 0.6689(6) 0.087(3) Uani 1 1 d . . . O2 O 0.4478(7) 0.4074(7) 0.5769(6) 0.084(3) Uani 1 1 d . . . O3 O 0.3497(7) 0.2863(7) 0.8518(7) 0.090(3) Uani 1 1 d . . . O4 O 0.4276(6) 0.6769(6) 0.8723(5) 0.061(2) Uani 1 1 d . . . C1 C 0.1604(10) 0.4616(12) 0.8481(10) 0.099(5) Uani 1 1 d . . . H1A H 0.1695 0.3858 0.8263 0.149 Uiso 1 1 calc R . . H1B H 0.0915 0.4733 0.8334 0.149 Uiso 1 1 calc R . . H1C H 0.1777 0.4930 0.9216 0.149 Uiso 1 1 calc R . . C2 C 0.2071(10) 0.6574(10) 0.8335(10) 0.086(4) Uani 1 1 d . . . H2A H 0.2455 0.7027 0.8049 0.129 Uiso 1 1 calc R . . H2B H 0.2210 0.6809 0.9077 0.129 Uiso 1 1 calc R . . H2C H 0.1367 0.6617 0.8178 0.129 Uiso 1 1 calc R . . C3 C 0.3910(10) 0.6041(10) 0.6180(9) 0.080(4) Uani 1 1 d . . . H3A H 0.3207 0.5833 0.6021 0.119 Uiso 1 1 calc R . . H3B H 0.4209 0.6072 0.5564 0.119 Uiso 1 1 calc R . . H3C H 0.3992 0.6735 0.6712 0.119 Uiso 1 1 calc R . . C4 C 0.5764(9) 0.5653(12) 0.6851(10) 0.096(5) Uani 1 1 d . . . H4A H 0.6192 0.5207 0.7096 0.143 Uiso 1 1 calc R . . H4B H 0.5786 0.6359 0.7364 0.143 Uiso 1 1 calc R . . H4C H 0.5992 0.5704 0.6211 0.143 Uiso 1 1 calc R . . C5 C 0.3026(11) 0.2572(11) 0.6551(10) 0.099(5) Uani 1 1 d . . . H5A H 0.2364 0.2832 0.6653 0.148 Uiso 1 1 calc R . . H5B H 0.2995 0.1812 0.6432 0.148 Uiso 1 1 calc R . . H5C H 0.3281 0.2708 0.5957 0.148 Uiso 1 1 calc R . . C6 C 0.4986(10) 0.2663(11) 0.7285(11) 0.099(5) Uani 1 1 d . . . H6A H 0.5504 0.2953 0.7835 0.148 Uiso 1 1 calc R . . H6B H 0.5171 0.2819 0.6676 0.148 Uiso 1 1 calc R . . H6C H 0.4904 0.1898 0.7126 0.148 Uiso 1 1 calc R . . C7 C 0.4107(11) 0.8614(11) 1.0149(11) 0.110(5) Uani 1 1 d . . . H7A H 0.3435 0.8471 1.0309 0.164 Uiso 1 1 calc R . . H7B H 0.4082 0.8883 0.9574 0.164 Uiso 1 1 calc R . . H7C H 0.4454 0.9140 1.0746 0.164 Uiso 1 1 calc R . . C8 C 0.5926(9) 0.7961(11) 0.9583(11) 0.090(4) Uani 1 1 d . . . H8A H 0.6385 0.7397 0.9386 0.136 Uiso 1 1 calc R . . H8B H 0.6195 0.8514 1.0207 0.136 Uiso 1 1 calc R . . H8C H 0.5833 0.8259 0.9032 0.136 Uiso 1 1 calc R . . O6 O 0.5493(5) 0.4964(6) 0.8817(6) 0.066(2) Uani 1 1 d . . . O5 O 0.3729(5) 0.5174(6) 0.9736(5) 0.059(2) Uani 1 1 d . . . C9 C 0.5491(8) 0.4948(8) 0.9755(8) 0.051(3) Uani 1 1 d . . . Ru2 Ru -0.04018(8) 0.00415(8) 0.69788(8) 0.0630(3) Uani 1 1 d . . . S21 S 0.0556(3) 0.0379(3) 0.8455(2) 0.0693(9) Uani 1 1 d . . . S22 S -0.1794(3) -0.0333(3) 0.7677(3) 0.0746(10) Uani 1 1 d . . . S23 S -0.0697(3) 0.1799(3) 0.7327(3) 0.0792(10) Uani 1 1 d . . . S24 S 0.0256(3) -0.2250(3) 0.5477(3) 0.0727(10) Uani 1 1 d . . . O21 O 0.0133(6) 0.0919(7) 0.9448(6) 0.077(2) Uani 1 1 d . . . O22 O -0.2354(7) 0.0575(8) 0.8326(8) 0.110(3) Uani 1 1 d . . . O23 O 0.0071(8) 0.2390(7) 0.6973(7) 0.099(3) Uani 1 1 d . . . O24 O -0.0105(6) -0.1616(6) 0.6551(5) 0.069(2) Uani 1 1 d . . . C11 C 0.1666(10) 0.1145(12) 0.8384(11) 0.108(5) Uani 1 1 d . . . H11A H 0.1486 0.1817 0.8314 0.163 Uiso 1 1 calc R . . H11B H 0.2016 0.0750 0.7792 0.163 Uiso 1 1 calc R . . H11C H 0.2095 0.1281 0.9008 0.163 Uiso 1 1 calc R . . C12 C 0.1110(10) -0.0795(11) 0.8570(9) 0.086(4) Uani 1 1 d . . . H12A H 0.0591 -0.1303 0.8606 0.129 Uiso 1 1 calc R . . H12B H 0.1552 -0.0597 0.9191 0.129 Uiso 1 1 calc R . . H12C H 0.1486 -0.1114 0.7973 0.129 Uiso 1 1 calc R . . C13 C -0.1611(11) -0.1204(12) 0.8397(10) 0.097(5) Uani 1 1 d . . . H13A H -0.1162 -0.0854 0.8999 0.146 Uiso 1 1 calc R . . H13B H -0.1327 -0.1845 0.7970 0.146 Uiso 1 1 calc R . . H13C H -0.2245 -0.1389 0.8615 0.146 Uiso 1 1 calc R . . C14 C -0.2652(10) -0.1101(13) 0.6694(11) 0.109(5) Uani 1 1 d . . . H14A H -0.2812 -0.0713 0.6227 0.164 Uiso 1 1 calc R . . H14B H -0.3252 -0.1253 0.6991 0.164 Uiso 1 1 calc R . . H14C H -0.2368 -0.1763 0.6317 0.164 Uiso 1 1 calc R . . C15 C -0.0884(12) 0.2579(11) 0.8649(9) 0.099(5) Uani 1 1 d . . . H15A H -0.0297 0.2576 0.9086 0.149 Uiso 1 1 calc R . . H15B H -0.1455 0.2275 0.8878 0.149 Uiso 1 1 calc R . . H15C H -0.1002 0.3305 0.8691 0.149 Uiso 1 1 calc R . . C16 C -0.1870(12) 0.1944(13) 0.6722(11) 0.118(6) Uani 1 1 d . . . H16A H -0.1888 0.1551 0.5989 0.177 Uiso 1 1 calc R . . H16B H -0.1951 0.2691 0.6826 0.177 Uiso 1 1 calc R . . H16C H -0.2405 0.1667 0.7024 0.177 Uiso 1 1 calc R . . C17 C 0.1183(11) -0.3043(13) 0.5742(10) 0.112(6) Uani 1 1 d . . . H17A H 0.1771 -0.2593 0.6077 0.168 Uiso 1 1 calc R . . H17B H 0.1353 -0.3563 0.5102 0.168 Uiso 1 1 calc R . . H17C H 0.0935 -0.3407 0.6194 0.168 Uiso 1 1 calc R . . C18 C -0.0665(11) -0.3295(12) 0.4869(11) 0.112(6) Uani 1 1 d . . . H18A H -0.1253 -0.2999 0.4661 0.167 Uiso 1 1 calc R . . H18B H -0.0837 -0.3658 0.5348 0.167 Uiso 1 1 calc R . . H18C H -0.0406 -0.3797 0.4265 0.167 Uiso 1 1 calc R . . O15 O 0.0830(5) 0.0243(6) 0.6116(6) 0.064(2) Uani 1 1 d . . . O16 O -0.1139(6) -0.0283(6) 0.5470(6) 0.066(2) Uani 1 1 d . . . C19 C -0.0540(9) -0.0136(10) 0.4824(9) 0.062(3) Uani 1 1 d . . . S10 S 0.4107(3) 0.9191(3) 0.7317(3) 0.0854(11) Uani 1 1 d . . . O11 O 0.3183(8) 0.8600(9) 0.7280(9) 0.127(4) Uani 1 1 d . . . O12 O 0.4123(10) 1.0297(9) 0.7864(9) 0.148(5) Uani 1 1 d . . . O13 O 0.4955(7) 0.8689(9) 0.7532(8) 0.114(4) Uani 1 1 d . . . C10 C 0.4165(15) 0.9140(16) 0.6042(14) 0.123(7) Uani 1 1 d . . . F11 F 0.4160(13) 0.8190(10) 0.5354(8) 0.210(7) Uani 1 1 d . . . F12 F 0.3481(11) 0.9619(10) 0.5676(9) 0.199(6) Uani 1 1 d . . . F13 F 0.4976(12) 0.9593(13) 0.5884(10) 0.211(7) Uani 1 1 d . . . S19 S 0.8728(4) 0.5563(4) 0.7345(4) 0.1138(15) Uani 1 1 d U . . O19 O 0.8424(15) 0.4476(13) 0.6945(14) 0.250(8) Uani 1 1 d U . . O29 O 0.9721(12) 0.5933(17) 0.7358(15) 0.263(9) Uani 1 1 d U . . O39 O 0.8060(9) 0.6170(10) 0.6974(9) 0.141(4) Uani 1 1 d U . . C30 C 0.8614(16) 0.5799(17) 0.8645(13) 0.138(7) Uani 1 1 d U . . F19 F 0.7734(13) 0.5612(18) 0.8872(14) 0.289(9) Uani 1 1 d U . . F29 F 0.9209(8) 0.5380(9) 0.9160(8) 0.144(4) Uani 1 1 d U . . F39 F 0.8680(15) 0.6764(13) 0.9170(12) 0.254(7) Uani 1 1 d U . . 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 0.0533(6) 0.0663(7) 0.0555(6) 0.0246(5) 0.0069(5) 0.0059(5) S1 0.055(2) 0.085(2) 0.072(2) 0.0349(19) 0.0052(17) 0.0036(18) S2 0.064(2) 0.073(2) 0.0564(19) 0.0236(17) 0.0085(16) 0.0037(17) S3 0.090(3) 0.065(2) 0.067(2) 0.0259(18) 0.0034(19) 0.0106(19) S4 0.068(2) 0.083(2) 0.071(2) 0.0277(19) 0.0073(18) 0.0011(19) O1 0.086(7) 0.105(7) 0.074(6) 0.040(5) -0.013(5) 0.001(5) O2 0.104(7) 0.079(6) 0.071(6) 0.023(5) 0.023(5) 0.017(5) O3 0.109(8) 0.083(6) 0.092(7) 0.048(6) 0.015(6) 0.010(6) O4 0.066(5) 0.060(5) 0.056(5) 0.017(4) 0.005(4) -0.001(4) C1 0.070(10) 0.125(13) 0.102(11) 0.040(10) 0.010(8) -0.022(9) C2 0.071(9) 0.093(10) 0.090(10) 0.026(8) 0.000(8) 0.010(8) C3 0.086(10) 0.091(10) 0.074(9) 0.038(8) 0.032(7) 0.019(8) C4 0.070(10) 0.143(14) 0.072(9) 0.032(9) 0.020(8) -0.004(9) C5 0.111(12) 0.077(10) 0.099(11) 0.025(8) -0.029(9) -0.017(9) C6 0.100(12) 0.081(10) 0.110(11) 0.021(9) 0.009(9) 0.031(9) C7 0.087(11) 0.103(12) 0.109(12) -0.007(10) 0.012(9) 0.018(9) C8 0.073(10) 0.098(11) 0.114(11) 0.056(9) 0.007(8) -0.011(8) O6 0.052(5) 0.089(6) 0.060(5) 0.026(5) 0.016(4) 0.006(4) O5 0.045(5) 0.090(6) 0.052(5) 0.035(4) 0.003(4) 0.007(4) C9 0.070(9) 0.045(6) 0.026(6) -0.005(5) 0.006(6) -0.010(6) Ru2 0.0621(7) 0.0708(7) 0.0621(6) 0.0279(5) 0.0153(5) 0.0068(5) S21 0.075(2) 0.074(2) 0.061(2) 0.0238(18) 0.0096(18) 0.0036(19) S22 0.068(2) 0.088(3) 0.073(2) 0.032(2) 0.0242(19) 0.010(2) S23 0.096(3) 0.068(2) 0.081(2) 0.0313(19) 0.020(2) 0.015(2) S24 0.076(2) 0.076(2) 0.067(2) 0.0235(18) 0.0135(18) 0.0092(19) O21 0.083(6) 0.083(6) 0.063(5) 0.020(5) 0.007(5) 0.003(5) O22 0.101(8) 0.116(8) 0.120(8) 0.039(7) 0.066(7) 0.025(7) O23 0.115(8) 0.078(6) 0.116(8) 0.050(6) 0.019(6) 0.000(6) O24 0.083(6) 0.068(5) 0.059(5) 0.022(4) 0.018(4) 0.016(5) C11 0.077(11) 0.129(14) 0.125(13) 0.058(11) -0.021(9) -0.026(10) C12 0.081(10) 0.119(12) 0.076(9) 0.054(9) 0.020(8) 0.035(9) C13 0.088(11) 0.120(13) 0.102(11) 0.064(10) 0.009(9) -0.012(9) C14 0.072(10) 0.145(15) 0.113(12) 0.056(11) -0.009(9) -0.048(10) C15 0.145(14) 0.081(10) 0.064(9) 0.013(8) 0.008(9) 0.021(10) C16 0.132(14) 0.114(13) 0.115(12) 0.040(10) 0.026(11) 0.069(11) C17 0.102(12) 0.137(14) 0.081(10) 0.015(10) -0.019(9) 0.032(11) C18 0.104(13) 0.111(13) 0.104(12) 0.026(10) -0.033(10) -0.040(10) O15 0.049(5) 0.085(6) 0.065(5) 0.038(5) 0.000(4) -0.003(4) O16 0.057(5) 0.083(6) 0.049(5) 0.011(4) 0.014(4) -0.003(4) C19 0.061(8) 0.069(9) 0.050(8) 0.012(7) -0.008(7) 0.012(7) S10 0.085(3) 0.085(3) 0.086(3) 0.027(2) 0.012(2) 0.008(2) O11 0.079(8) 0.137(10) 0.170(11) 0.051(8) 0.041(7) 0.000(7) O12 0.176(12) 0.097(9) 0.149(10) 0.009(8) 0.013(9) 0.021(8) O13 0.084(7) 0.156(10) 0.128(8) 0.083(8) 0.002(6) 0.010(7) C10 0.114(16) 0.139(19) 0.148(19) 0.085(17) 0.042(14) 0.005(14) F11 0.38(2) 0.138(10) 0.100(8) 0.015(8) 0.048(11) 0.061(13) F12 0.264(17) 0.188(12) 0.157(10) 0.077(9) -0.052(10) 0.071(11) F13 0.259(18) 0.259(18) 0.192(13) 0.165(14) 0.076(12) 0.052(14) S19 0.106(3) 0.122(4) 0.126(4) 0.055(3) 0.026(3) 0.015(3) O19 0.310(12) 0.209(11) 0.227(11) 0.067(9) 0.002(9) 0.017(9) O29 0.238(12) 0.320(13) 0.267(12) 0.147(9) 0.013(9) 0.020(9) O39 0.130(8) 0.163(8) 0.154(8) 0.085(7) -0.008(6) 0.021(7) C30 0.145(11) 0.146(11) 0.139(10) 0.070(9) 0.004(9) 0.012(9) F19 0.258(12) 0.366(13) 0.268(12) 0.138(9) 0.032(9) 0.018(9) F29 0.142(7) 0.168(8) 0.142(7) 0.077(6) 0.004(6) 0.032(6) F39 0.341(12) 0.216(10) 0.210(10) 0.078(8) -0.001(8) 0.042(9) _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 O5 2.119(7) . ? Ru1 O4 2.129(7) . ? Ru1 O6 2.135(7) . ? Ru1 S1 2.228(3) . ? Ru1 S2 2.259(3) . ? Ru1 S3 2.263(4) . ? S1 O1 1.460(8) . ? S1 C2 1.766(13) . ? S1 C1 1.799(13) . ? S2 O2 1.451(8) . ? S2 C3 1.778(12) . ? S2 C4 1.781(13) . ? S3 O3 1.473(9) . ? S3 C6 1.770(13) . ? S3 C5 1.794(12) . ? S4 O4 1.536(7) . ? S4 C7 1.749(14) . ? S4 C8 1.789(13) . ? O6 C9 1.284(12) . ? O5 C9 1.265(12) 2_667 ? C9 O5 1.265(12) 2_667 ? C9 C9 1.49(2) 2_667 ? Ru2 O15 2.128(8) . ? Ru2 O24 2.128(8) . ? Ru2 O16 2.132(7) . ? Ru2 S21 2.229(3) . ? Ru2 S22 2.242(4) . ? Ru2 S23 2.262(4) . ? S21 O21 1.459(8) . ? S21 C11 1.787(14) . ? S21 C12 1.790(12) . ? S22 O22 1.487(10) . ? S22 C14 1.727(12) . ? S22 C13 1.755(13) . ? S23 O23 1.459(10) . ? S23 C16 1.778(14) . ? S23 C15 1.791(12) . ? S24 O24 1.539(8) . ? S24 C17 1.749(13) . ? S24 C18 1.762(13) . ? O15 C19 1.279(12) 2_556 ? O16 C19 1.275(14) . ? C19 O15 1.279(12) 2_556 ? C19 C19 1.49(2) 2_556 ? S10 O13 1.399(9) . ? S10 O12 1.401(11) . ? S10 O11 1.423(10) . ? S10 C10 1.721(17) . ? C10 F13 1.278(17) . ? C10 F11 1.294(18) . ? C10 F12 1.298(17) . ? S19 O19 1.390(15) . ? S19 O29 1.391(15) . ? S19 O39 1.403(10) . ? S19 C30 1.709(17) . ? C30 F39 1.234(18) . ? C30 F19 1.266(19) . ? C30 F29 1.288(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Ru1 O4 88.4(3) . . ? O5 Ru1 O6 78.9(3) . . ? O4 Ru1 O6 88.2(3) . . ? O5 Ru1 S1 92.4(2) . . ? O4 Ru1 S1 90.4(2) . . ? O6 Ru1 S1 171.2(2) . . ? O5 Ru1 S2 172.5(2) . . ? O4 Ru1 S2 87.0(2) . . ? O6 Ru1 S2 95.0(2) . . ? S1 Ru1 S2 93.55(12) . . ? O5 Ru1 S3 90.2(2) . . ? O4 Ru1 S3 175.8(2) . . ? O6 Ru1 S3 87.7(2) . . ? S1 Ru1 S3 93.63(14) . . ? S2 Ru1 S3 94.06(13) . . ? O1 S1 C2 107.6(6) . . ? O1 S1 C1 108.2(6) . . ? C2 S1 C1 98.8(7) . . ? O1 S1 Ru1 118.8(4) . . ? C2 S1 Ru1 111.1(4) . . ? C1 S1 Ru1 110.4(5) . . ? O2 S2 C3 107.9(5) . . ? O2 S2 C4 108.1(6) . . ? C3 S2 C4 99.6(7) . . ? O2 S2 Ru1 119.0(4) . . ? C3 S2 Ru1 113.4(4) . . ? C4 S2 Ru1 106.9(4) . . ? O3 S3 C6 108.3(6) . . ? O3 S3 C5 106.1(6) . . ? C6 S3 C5 100.2(7) . . ? O3 S3 Ru1 112.7(4) . . ? C6 S3 Ru1 111.3(5) . . ? C5 S3 Ru1 117.2(5) . . ? O4 S4 C7 104.0(6) . . ? O4 S4 C8 104.5(6) . . ? C7 S4 C8 98.2(7) . . ? S4 O4 Ru1 123.8(4) . . ? C9 O6 Ru1 111.9(7) . . ? C9 O5 Ru1 112.2(7) 2_667 . ? O5 C9 O6 123.3(10) 2_667 . ? O5 C9 C9 119.2(12) 2_667 2_667 ? O6 C9 C9 117.5(13) . 2_667 ? O15 Ru2 O24 87.9(3) . . ? O15 Ru2 O16 79.2(3) . . ? O24 Ru2 O16 88.6(3) . . ? O15 Ru2 S21 93.4(2) . . ? O24 Ru2 S21 90.0(2) . . ? O16 Ru2 S21 172.5(2) . . ? O15 Ru2 S22 172.0(2) . . ? O24 Ru2 S22 88.2(2) . . ? O16 Ru2 S22 93.8(2) . . ? S21 Ru2 S22 93.48(13) . . ? O15 Ru2 S23 89.3(2) . . ? O24 Ru2 S23 176.3(2) . . ? O16 Ru2 S23 88.6(2) . . ? S21 Ru2 S23 92.53(14) . . ? S22 Ru2 S23 94.36(15) . . ? O21 S21 C11 107.9(7) . . ? O21 S21 C12 106.9(5) . . ? C11 S21 C12 99.6(7) . . ? O21 S21 Ru2 119.2(4) . . ? C11 S21 Ru2 108.5(5) . . ? C12 S21 Ru2 112.9(4) . . ? O22 S22 C14 105.6(7) . . ? O22 S22 C13 107.0(7) . . ? C14 S22 C13 100.9(7) . . ? O22 S22 Ru2 118.7(5) . . ? C14 S22 Ru2 109.4(5) . . ? C13 S22 Ru2 113.6(5) . . ? O23 S23 C16 107.3(7) . . ? O23 S23 C15 106.8(7) . . ? C16 S23 C15 99.5(7) . . ? O23 S23 Ru2 113.3(4) . . ? C16 S23 Ru2 110.9(6) . . ? C15 S23 Ru2 117.7(5) . . ? O24 S24 C17 104.7(6) . . ? O24 S24 C18 107.0(6) . . ? C17 S24 C18 97.6(8) . . ? S24 O24 Ru2 122.4(4) . . ? C19 O15 Ru2 111.3(7) 2_556 . ? C19 O16 Ru2 111.7(7) . . ? O16 C19 O15 122.4(10) . 2_556 ? O16 C19 C19 118.4(13) . 2_556 ? O15 C19 C19 119.2(16) 2_556 2_556 ? O13 S10 O12 114.5(8) . . ? O13 S10 O11 113.9(7) . . ? O12 S10 O11 115.7(8) . . ? O13 S10 C10 105.4(8) . . ? O12 S10 C10 103.0(9) . . ? O11 S10 C10 102.2(8) . . ? F13 C10 F11 102.3(17) . . ? F13 C10 F12 102.1(16) . . ? F11 C10 F12 104.5(17) . . ? F13 C10 S10 112.9(14) . . ? F11 C10 S10 116.0(14) . . ? F12 C10 S10 117.1(14) . . ? O19 S19 O29 122.2(13) . . ? O19 S19 O39 110.4(10) . . ? O29 S19 O39 111.4(10) . . ? O19 S19 C30 100.3(11) . . ? O29 S19 C30 100.7(11) . . ? O39 S19 C30 110.3(9) . . ? F39 C30 F19 96.1(19) . . ? F39 C30 F29 103.4(17) . . ? F19 C30 F29 106.1(18) . . ? F39 C30 S19 113.4(16) . . ? F19 C30 S19 114.1(16) . . ? F29 C30 S19 120.5(15) . . ? 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 O5 Ru1 S1 O1 -159.0(5) . . . . ? O4 Ru1 S1 O1 112.6(5) . . . . ? O6 Ru1 S1 O1 -167.0(15) . . . . ? S2 Ru1 S1 O1 25.7(5) . . . . ? S3 Ru1 S1 O1 -68.6(5) . . . . ? O5 Ru1 S1 C2 75.4(5) . . . . ? O4 Ru1 S1 C2 -13.0(5) . . . . ? O6 Ru1 S1 C2 67.3(16) . . . . ? S2 Ru1 S1 C2 -100.0(5) . . . . ? S3 Ru1 S1 C2 165.7(5) . . . . ? O5 Ru1 S1 C1 -33.2(6) . . . . ? O4 Ru1 S1 C1 -121.5(6) . . . . ? O6 Ru1 S1 C1 -41.2(17) . . . . ? S2 Ru1 S1 C1 151.5(5) . . . . ? S3 Ru1 S1 C1 57.2(5) . . . . ? O5 Ru1 S2 O2 131.2(17) . . . . ? O4 Ru1 S2 O2 -177.3(5) . . . . ? O6 Ru1 S2 O2 94.8(5) . . . . ? S1 Ru1 S2 O2 -87.2(4) . . . . ? S3 Ru1 S2 O2 6.7(4) . . . . ? O5 Ru1 S2 C3 -100.2(18) . . . . ? O4 Ru1 S2 C3 -48.8(5) . . . . ? O6 Ru1 S2 C3 -136.7(5) . . . . ? S1 Ru1 S2 C3 41.4(5) . . . . ? S3 Ru1 S2 C3 135.3(5) . . . . ? O5 Ru1 S2 C4 8.5(19) . . . . ? O4 Ru1 S2 C4 60.0(6) . . . . ? O6 Ru1 S2 C4 -27.9(6) . . . . ? S1 Ru1 S2 C4 150.1(5) . . . . ? S3 Ru1 S2 C4 -116.0(5) . . . . ? O5 Ru1 S3 O3 6.9(5) . . . . ? O4 Ru1 S3 O3 77(3) . . . . ? O6 Ru1 S3 O3 85.8(5) . . . . ? S1 Ru1 S3 O3 -85.5(4) . . . . ? S2 Ru1 S3 O3 -179.3(4) . . . . ? O5 Ru1 S3 C6 -115.0(5) . . . . ? O4 Ru1 S3 C6 -45(3) . . . . ? O6 Ru1 S3 C6 -36.1(5) . . . . ? S1 Ru1 S3 C6 152.6(5) . . . . ? S2 Ru1 S3 C6 58.8(5) . . . . ? O5 Ru1 S3 C5 130.4(6) . . . . ? O4 Ru1 S3 C5 -160(3) . . . . ? O6 Ru1 S3 C5 -150.6(6) . . . . ? S1 Ru1 S3 C5 38.1(6) . . . . ? S2 Ru1 S3 C5 -55.8(6) . . . . ? C7 S4 O4 Ru1 -143.6(7) . . . . ? C8 S4 O4 Ru1 113.9(6) . . . . ? O5 Ru1 O4 S4 33.2(5) . . . . ? O6 Ru1 O4 S4 -45.8(5) . . . . ? S1 Ru1 O4 S4 125.5(5) . . . . ? S2 Ru1 O4 S4 -140.9(5) . . . . ? S3 Ru1 O4 S4 -37(3) . . . . ? O5 Ru1 O6 C9 4.0(7) . . . . ? O4 Ru1 O6 C9 92.7(7) . . . . ? S1 Ru1 O6 C9 12(2) . . . . ? S2 Ru1 O6 C9 179.4(7) . . . . ? S3 Ru1 O6 C9 -86.7(7) . . . . ? O4 Ru1 O5 C9 -93.2(7) . . . 2_667 ? O6 Ru1 O5 C9 -4.8(7) . . . 2_667 ? S1 Ru1 O5 C9 176.5(7) . . . 2_667 ? S2 Ru1 O5 C9 -42(2) . . . 2_667 ? S3 Ru1 O5 C9 82.8(7) . . . 2_667 ? Ru1 O6 C9 O5 175.6(8) . . . 2_667 ? Ru1 O6 C9 C9 -2.8(14) . . . 2_667 ? O15 Ru2 S21 O21 147.0(5) . . . . ? O24 Ru2 S21 O21 -125.1(5) . . . . ? O16 Ru2 S21 O21 155.8(19) . . . . ? S22 Ru2 S21 O21 -37.0(4) . . . . ? S23 Ru2 S21 O21 57.6(5) . . . . ? O15 Ru2 S21 C11 23.0(6) . . . . ? O24 Ru2 S21 C11 110.9(6) . . . . ? O16 Ru2 S21 C11 32(2) . . . . ? S22 Ru2 S21 C11 -161.0(6) . . . . ? S23 Ru2 S21 C11 -66.4(6) . . . . ? O15 Ru2 S21 C12 -86.4(5) . . . . ? O24 Ru2 S21 C12 1.5(5) . . . . ? O16 Ru2 S21 C12 -78(2) . . . . ? S22 Ru2 S21 C12 89.6(5) . . . . ? S23 Ru2 S21 C12 -175.8(5) . . . . ? O15 Ru2 S22 O22 -129.8(17) . . . . ? O24 Ru2 S22 O22 170.0(6) . . . . ? O16 Ru2 S22 O22 -101.6(6) . . . . ? S21 Ru2 S22 O22 80.1(5) . . . . ? S23 Ru2 S22 O22 -12.7(5) . . . . ? O15 Ru2 S22 C14 -8.6(18) . . . . ? O24 Ru2 S22 C14 -68.8(6) . . . . ? O16 Ru2 S22 C14 19.6(6) . . . . ? S21 Ru2 S22 C14 -158.7(6) . . . . ? S23 Ru2 S22 C14 108.5(6) . . . . ? O15 Ru2 S22 C13 103.2(17) . . . . ? O24 Ru2 S22 C13 43.0(6) . . . . ? O16 Ru2 S22 C13 131.4(6) . . . . ? S21 Ru2 S22 C13 -46.9(6) . . . . ? S23 Ru2 S22 C13 -139.7(6) . . . . ? O15 Ru2 S23 O23 -6.6(5) . . . . ? O24 Ru2 S23 O23 -47(4) . . . . ? O16 Ru2 S23 O23 -85.8(5) . . . . ? S21 Ru2 S23 O23 86.9(5) . . . . ? S22 Ru2 S23 O23 -179.5(5) . . . . ? O15 Ru2 S23 C16 114.2(6) . . . . ? O24 Ru2 S23 C16 74(4) . . . . ? O16 Ru2 S23 C16 34.9(6) . . . . ? S21 Ru2 S23 C16 -152.4(6) . . . . ? S22 Ru2 S23 C16 -58.7(6) . . . . ? O15 Ru2 S23 C15 -132.2(6) . . . . ? O24 Ru2 S23 C15 -172(4) . . . . ? O16 Ru2 S23 C15 148.6(6) . . . . ? S21 Ru2 S23 C15 -38.8(6) . . . . ? S22 Ru2 S23 C15 54.9(6) . . . . ? C17 S24 O24 Ru2 138.4(7) . . . . ? C18 S24 O24 Ru2 -118.8(7) . . . . ? O15 Ru2 O24 S24 -36.2(5) . . . . ? O16 Ru2 O24 S24 43.1(6) . . . . ? S21 Ru2 O24 S24 -129.6(5) . . . . ? S22 Ru2 O24 S24 136.9(5) . . . . ? S23 Ru2 O24 S24 4(4) . . . . ? O24 Ru2 O15 C19 92.3(8) . . . 2_556 ? O16 Ru2 O15 C19 3.4(7) . . . 2_556 ? S21 Ru2 O15 C19 -177.8(7) . . . 2_556 ? S22 Ru2 O15 C19 32(2) . . . 2_556 ? S23 Ru2 O15 C19 -85.3(7) . . . 2_556 ? O15 Ru2 O16 C19 -4.4(8) . . . . ? O24 Ru2 O16 C19 -92.5(8) . . . . ? S21 Ru2 O16 C19 -13(2) . . . . ? S22 Ru2 O16 C19 179.5(8) . . . . ? S23 Ru2 O16 C19 85.2(8) . . . . ? Ru2 O16 C19 O15 -177.2(9) . . . 2_556 ? Ru2 O16 C19 C19 4.7(17) . . . 2_556 ? O13 S10 C10 F13 -57.8(17) . . . . ? O12 S10 C10 F13 62.5(17) . . . . ? O11 S10 C10 F13 -177.1(15) . . . . ? O13 S10 C10 F11 59.8(18) . . . . ? O12 S10 C10 F11 -179.9(16) . . . . ? O11 S10 C10 F11 -59.5(17) . . . . ? O13 S10 C10 F12 -176.0(15) . . . . ? O12 S10 C10 F12 -55.7(18) . . . . ? O11 S10 C10 F12 64.7(17) . . . . ? O19 S19 C30 F39 -168.4(19) . . . . ? O29 S19 C30 F39 66(2) . . . . ? O39 S19 C30 F39 -52(2) . . . . ? O19 S19 C30 F19 -60(2) . . . . ? O29 S19 C30 F19 174.4(19) . . . . ? O39 S19 C30 F19 57(2) . . . . ? O19 S19 C30 F29 68(2) . . . . ? O29 S19 C30 F29 -57(2) . . . . ? O39 S19 C30 F29 -175.2(16) . . . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 1.275 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.117 #===END data_18 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra[fac-tris(dimethylsulfoxide,S)-(eta3-mu-oxalate,O,O',O'')- -ruthenium(II)] hydrated ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C32 H72 O23 Ru4 S12) 5(H2 O)' _chemical_formula_sum 'C32 H82 O33 Ru4 S12' _chemical_formula_weight 1783.98 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' '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 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 14.192(3) _cell_length_b 14.192(3) _cell_length_c 33.548(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6757(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3624 _exptl_absorpt_coefficient_mu 1.328 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.2411 _exptl_absorpt_correction_T_max 1.0977 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36607 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.72 _reflns_number_total 3589 _reflns_number_gt 2182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Scala (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0888P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3588 _refine_ls_number_parameters 192 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0993 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1507 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.021 _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 Ru Ru 0.68416(4) 0.55490(4) 0.101641(17) 0.0528(2) Uani 1 1 d . . . S1 S 0.72522(14) 0.58266(14) 0.03764(6) 0.0605(5) Uani 1 1 d . . . S2 S 0.66594(13) 0.39815(13) 0.09326(5) 0.0568(5) Uani 1 1 d . . . S3 S 0.83256(14) 0.53968(14) 0.12488(6) 0.0599(5) Uani 1 1 d . . . O1 O 0.7787(4) 0.5108(4) 0.01505(16) 0.0789(16) Uani 1 1 d . . . O2 O 0.7500(4) 0.3380(3) 0.08972(17) 0.0682(14) Uani 1 1 d . . . O3 O 0.8730(4) 0.6279(4) 0.14110(16) 0.0735(15) Uani 1 1 d . . . C1 C 0.6272(6) 0.6132(7) 0.0077(2) 0.086(3) Uani 1 1 d . . . H1A H 0.5851 0.5604 0.0059 0.128 Uiso 1 1 calc R . . H1B H 0.6485 0.6301 -0.0185 0.128 Uiso 1 1 calc R . . H1C H 0.5948 0.6657 0.0195 0.128 Uiso 1 1 calc R . . C2 C 0.7873(7) 0.6907(6) 0.0350(3) 0.082(3) Uani 1 1 d . . . H2A H 0.8442 0.6862 0.0504 0.123 Uiso 1 1 calc R . . H2B H 0.7487 0.7404 0.0455 0.123 Uiso 1 1 calc R . . H2C H 0.8028 0.7042 0.0077 0.123 Uiso 1 1 calc R . . C3 C 0.5982(6) 0.3562(6) 0.1337(2) 0.066(2) Uani 1 1 d . . . H3A H 0.6314 0.3675 0.1582 0.099 Uiso 1 1 calc R . . H3B H 0.5876 0.2898 0.1306 0.099 Uiso 1 1 calc R . . H3C H 0.5388 0.3885 0.1343 0.099 Uiso 1 1 calc R . . C4 C 0.5894(6) 0.3687(6) 0.0532(2) 0.078(2) Uani 1 1 d . . . H4A H 0.6175 0.3877 0.0285 0.117 Uiso 1 1 calc R . . H4B H 0.5303 0.4006 0.0566 0.117 Uiso 1 1 calc R . . H4C H 0.5789 0.3019 0.0530 0.117 Uiso 1 1 calc R . . C5 C 0.9154(5) 0.4937(7) 0.0921(2) 0.075(2) Uani 1 1 d . . . H5A H 0.9200 0.5337 0.0691 0.112 Uiso 1 1 calc R . . H5B H 0.8965 0.4317 0.0840 0.112 Uiso 1 1 calc R . . H5C H 0.9756 0.4905 0.1050 0.112 Uiso 1 1 calc R . . C6 C 0.8388(6) 0.4561(6) 0.1641(2) 0.072(2) Uani 1 1 d . . . H6A H 0.7955 0.4734 0.1848 0.108 Uiso 1 1 calc R . . H6B H 0.9017 0.4547 0.1746 0.108 Uiso 1 1 calc R . . H6C H 0.8226 0.3949 0.1540 0.108 Uiso 1 1 calc R . . C7 C 0.6659(5) 0.7154(5) 0.1511(2) 0.0528(16) Uani 1 1 d . . . C8 C 0.6371(5) 0.6323(5) 0.1780(2) 0.0593(18) Uani 1 1 d . . . O4 O 0.6690(4) 0.7949(4) 0.16718(14) 0.0638(13) Uani 1 1 d . . . O5 O 0.6869(4) 0.6982(3) 0.11538(14) 0.0589(12) Uani 1 1 d . . . O6 O 0.6453(3) 0.5507(3) 0.16162(14) 0.0560(11) Uani 1 1 d . . . O7 O 0.6075(5) 0.6471(4) 0.21172(15) 0.0799(17) Uani 1 1 d . . . O1W O 0.9449(8) 0.4200(9) -0.0119(4) 0.162(4) Uani 1 1 d D . . H1W H 0.932(12) 0.481(3) -0.015(6) 0.242 Uiso 1 1 d D . . H2W H 0.888(6) 0.398(11) -0.007(6) 0.242 Uiso 1 1 d D . . O2W O 1.0000 0.2500 0.0313(8) 0.148(9) Uani 0.50 2 d SPU . . 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 Ru 0.0550(4) 0.0547(4) 0.0485(3) -0.0017(2) 0.0017(2) 0.0002(3) S1 0.0611(11) 0.0672(11) 0.0531(10) -0.0017(9) 0.0040(8) 0.0018(9) S2 0.0593(10) 0.0542(10) 0.0568(10) -0.0035(8) 0.0005(8) -0.0002(8) S3 0.0582(10) 0.0606(11) 0.0610(11) -0.0041(9) -0.0028(8) -0.0036(9) O1 0.088(4) 0.089(4) 0.060(3) -0.009(3) 0.009(3) 0.016(3) O2 0.060(3) 0.058(3) 0.087(4) -0.008(3) 0.008(3) 0.009(3) O3 0.074(3) 0.061(3) 0.085(4) -0.007(3) -0.013(3) -0.013(3) C1 0.071(5) 0.127(8) 0.059(5) 0.013(5) 0.003(4) 0.001(5) C2 0.096(7) 0.078(6) 0.073(5) 0.000(4) 0.025(5) -0.011(5) C3 0.065(5) 0.063(5) 0.070(5) 0.002(4) 0.009(4) 0.005(4) C4 0.086(6) 0.079(6) 0.069(5) -0.015(4) -0.019(4) -0.007(5) C5 0.057(5) 0.097(6) 0.069(5) -0.009(5) 0.004(4) 0.010(5) C6 0.075(5) 0.079(5) 0.062(5) 0.000(4) -0.013(4) 0.010(4) C7 0.056(4) 0.041(3) 0.062(4) -0.002(3) -0.003(3) 0.004(3) C8 0.062(4) 0.059(4) 0.057(4) 0.001(3) -0.005(3) 0.001(4) O4 0.075(3) 0.061(3) 0.055(3) -0.001(2) 0.007(3) -0.006(3) O5 0.068(3) 0.058(3) 0.051(3) 0.000(2) 0.005(2) 0.003(2) O6 0.057(3) 0.061(3) 0.050(3) 0.001(2) 0.003(2) 0.002(2) O7 0.114(5) 0.074(4) 0.052(3) -0.008(3) 0.017(3) -0.006(3) O1W 0.157(9) 0.181(10) 0.146(8) -0.033(9) 0.044(7) 0.024(8) O2W 0.145(12) 0.126(12) 0.173(12) 0.000 0.000 0.005(9) _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 Ru O5 2.085(5) . ? Ru O6 2.087(5) . ? Ru O4 2.108(5) 15_565 ? Ru S3 2.256(2) . ? Ru S2 2.257(2) . ? Ru S1 2.259(2) . ? S1 O1 1.480(6) . ? S1 C1 1.769(8) . ? S1 C2 1.771(9) . ? S2 O2 1.472(5) . ? S2 C3 1.766(7) . ? S2 C4 1.777(8) . ? S3 O3 1.481(5) . ? S3 C5 1.738(8) . ? S3 C6 1.773(8) . ? C7 O4 1.252(8) . ? C7 O5 1.258(8) . ? C7 C8 1.539(10) . ? C8 O7 1.225(8) . ? C8 O6 1.287(8) . ? O4 Ru 2.108(5) 12_766 ? 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 O5 Ru O6 79.62(19) . . ? O5 Ru O4 85.0(2) . 15_565 ? O6 Ru O4 92.63(19) . 15_565 ? O5 Ru S3 89.98(15) . . ? O6 Ru S3 84.89(14) . . ? O4 Ru S3 174.70(16) 15_565 . ? O5 Ru S2 172.17(14) . . ? O6 Ru S2 93.53(14) . . ? O4 Ru S2 91.64(15) 15_565 . ? S3 Ru S2 93.19(7) . . ? O5 Ru S1 92.02(14) . . ? O6 Ru S1 171.60(15) . . ? O4 Ru S1 85.79(14) 15_565 . ? S3 Ru S1 95.99(7) . . ? S2 Ru S1 94.76(7) . . ? O1 S1 C1 106.4(4) . . ? O1 S1 C2 108.4(4) . . ? C1 S1 C2 98.7(5) . . ? O1 S1 Ru 119.9(3) . . ? C1 S1 Ru 112.3(3) . . ? C2 S1 Ru 109.1(3) . . ? O2 S2 C3 107.9(4) . . ? O2 S2 C4 107.4(4) . . ? C3 S2 C4 99.7(4) . . ? O2 S2 Ru 119.3(2) . . ? C3 S2 Ru 107.4(3) . . ? C4 S2 Ru 113.3(3) . . ? O3 S3 C5 106.7(4) . . ? O3 S3 C6 105.9(4) . . ? C5 S3 C6 100.6(4) . . ? O3 S3 Ru 114.1(2) . . ? C5 S3 Ru 116.7(3) . . ? C6 S3 Ru 111.5(3) . . ? O4 C7 O5 125.2(6) . . ? O4 C7 C8 116.5(6) . . ? O5 C7 C8 118.2(6) . . ? O7 C8 O6 125.4(7) . . ? O7 C8 C7 120.1(7) . . ? O6 C8 C7 114.5(6) . . ? C8 O6 Ru 114.1(4) . . ? C7 O5 Ru 113.3(4) . . ? C7 O4 Ru 136.3(5) . 12_766 ? 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 O5 Ru S1 O1 151.0(3) . . . . ? O6 Ru S1 O1 156.4(10) . . . . ? O4 Ru S1 O1 -124.2(3) 15_565 . . . ? S3 Ru S1 O1 60.8(3) . . . . ? S2 Ru S1 O1 -32.9(3) . . . . ? O5 Ru S1 C1 -83.0(4) . . . . ? O6 Ru S1 C1 -77.6(10) . . . . ? O4 Ru S1 C1 1.8(4) 15_565 . . . ? S3 Ru S1 C1 -173.2(4) . . . . ? S2 Ru S1 C1 93.1(4) . . . . ? O5 Ru S1 C2 25.3(4) . . . . ? O6 Ru S1 C2 30.7(11) . . . . ? O4 Ru S1 C2 110.1(4) 15_565 . . . ? S3 Ru S1 C2 -64.9(4) . . . . ? S2 Ru S1 C2 -158.6(4) . . . . ? O5 Ru S2 O2 -135.1(11) . . . . ? O6 Ru S2 O2 -106.4(3) . . . . ? O4 Ru S2 O2 160.9(3) 15_565 . . . ? S3 Ru S2 O2 -21.3(3) . . . . ? S1 Ru S2 O2 75.0(3) . . . . ? O5 Ru S2 C3 -12.0(11) . . . . ? O6 Ru S2 C3 16.6(3) . . . . ? O4 Ru S2 C3 -76.1(3) 15_565 . . . ? S3 Ru S2 C3 101.7(3) . . . . ? S1 Ru S2 C3 -162.0(3) . . . . ? O5 Ru S2 C4 97.0(11) . . . . ? O6 Ru S2 C4 125.7(4) . . . . ? O4 Ru S2 C4 33.0(4) 15_565 . . . ? S3 Ru S2 C4 -149.2(3) . . . . ? S1 Ru S2 C4 -52.9(3) . . . . ? O5 Ru S3 O3 1.7(3) . . . . ? O6 Ru S3 O3 -77.9(3) . . . . ? O4 Ru S3 O3 -15.6(16) 15_565 . . . ? S2 Ru S3 O3 -171.1(3) . . . . ? S1 Ru S3 O3 93.7(3) . . . . ? O5 Ru S3 C5 -123.5(4) . . . . ? O6 Ru S3 C5 156.9(4) . . . . ? O4 Ru S3 C5 -140.8(16) 15_565 . . . ? S2 Ru S3 C5 63.6(4) . . . . ? S1 Ru S3 C5 -31.5(4) . . . . ? O5 Ru S3 C6 121.6(3) . . . . ? O6 Ru S3 C6 42.0(3) . . . . ? O4 Ru S3 C6 104.3(16) 15_565 . . . ? S2 Ru S3 C6 -51.2(3) . . . . ? S1 Ru S3 C6 -146.3(3) . . . . ? O4 C7 C8 O7 9.1(11) . . . . ? O5 C7 C8 O7 -173.0(7) . . . . ? O4 C7 C8 O6 -172.4(6) . . . . ? O5 C7 C8 O6 5.6(10) . . . . ? O7 C8 O6 Ru 173.5(6) . . . . ? C7 C8 O6 Ru -4.9(8) . . . . ? O5 Ru O6 C8 2.8(5) . . . . ? O4 Ru O6 C8 -81.6(5) 15_565 . . . ? S3 Ru O6 C8 93.7(5) . . . . ? S2 Ru O6 C8 -173.4(5) . . . . ? S1 Ru O6 C8 -2.7(13) . . . . ? O4 C7 O5 Ru 174.7(6) . . . . ? C8 C7 O5 Ru -3.1(8) . . . . ? O6 Ru O5 C7 0.4(5) . . . . ? O4 Ru O5 C7 94.0(5) 15_565 . . . ? S3 Ru O5 C7 -84.4(5) . . . . ? S2 Ru O5 C7 29.5(14) . . . . ? S1 Ru O5 C7 179.6(5) . . . . ? O5 C7 O4 Ru 5.8(12) . . . 12_766 ? C8 C7 O4 Ru -176.4(5) . . . 12_766 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.72 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.316 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.139