############################################################################## ### ### ### Electronic paper (Acta Crystallographica Section E) ### ### ### ############################################################################## # # # This CIF contains the data in a paper accepted for publication in Acta # # Crystallographica Section E. It conforms to the requirements of Notes # # for Authors for Section E, and has been peer reviewed under the auspices # # of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.4. # # # # Software is freely available for graphical display of the structure(s) in # # this CIF. For information consult the CIF home page http://www.iucr.org/ # # cif/home.html # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_I _audit_creation_method SHELXL-97 _chemical_name_systematic ; Poly[di-\m~2~-chlorido-dichlorido(\m~3~-dimethyl sulfoxide-\k^3^O:O:S)(\m~2~-dimethyl sulfoxide-\k^2^O:S)ruthenium(III)sodium] ; _chemical_name_common ? _chemical_formula_moiety 'C4 H12 Cl4 Na O2 Ru S2' _chemical_formula_sum 'C4 H12 Cl4 Na O2 Ru S2' _chemical_formula_iupac '[Na Ru Cl4 (C2 H6 O1 S1)2]' _chemical_formula_weight 422.12 _chemical_melting_point ? _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9042(3) _cell_length_b 8.0692(2) _cell_length_c 13.7873(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.470(2) _cell_angle_gamma 90.00 _cell_volume 1309.93(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10079 _cell_measurement_theta_min 2.9267 _cell_measurement_theta_max 31.9755 _cell_measurement_temperature 120(2) _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.140 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 2.336 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; (CrysAlis RED; Oxford Diffraction, 2007) ; _exptl_absorpt_correction_T_min 0.6523 _exptl_absorpt_correction_T_max 0.7207 _exptl_special_details ; ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Enhance (Mo) X-ray Source' _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur2 CCD' _diffrn_measurement_method 'rotation method, \w--scan' _diffrn_detector_area_resol_mean 8.3611 _diffrn_reflns_number 10197 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0160 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _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^ > \s(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. ; _reflns_number_total 2300 _reflns_number_gt 2105 _reflns_threshold_expression I>2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0183 _refine_ls_wR_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.0501 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _refine_ls_number_reflns 2300 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+0.8654P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.706 _refine_diff_density_min -0.361 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2007) ; _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2007) ; _computing_data_reduction ; CrysAlis RED (Oxford Diffraction, 2007) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru1 0.5000 0.5000 0.5000 0.00777(8) Uani d S 1 . . S S1 0.45936(5) 0.30580(7) 0.37416(4) 0.00948(13) Uani d . 1 . . Cl Cl1 0.35603(5) 0.67940(7) 0.42755(4) 0.01284(13) Uani d . 1 . . Na Na1 0.35677(8) 0.00303(10) 0.51520(7) 0.0144(2) Uani d . 1 . . O O1 0.47177(13) 0.12823(19) 0.40510(11) 0.0125(3) Uani d . 1 . . C C1 0.31978(19) 0.3274(3) 0.30958(17) 0.0148(5) Uani d . 1 . . H H1A 0.3050 0.2387 0.2608 0.022 Uiso calc R 1 . . H H1B 0.3125 0.4351 0.2765 0.022 Uiso calc R 1 . . H H1C 0.2648 0.3202 0.3558 0.022 Uiso calc R 1 . . Ru Ru2 0.0000 0.0000 0.5000 0.00862(9) Uani d S 1 . . S S2 0.12479(5) -0.14419(7) 0.61717(4) 0.01206(13) Uani d . 1 . . Cl Cl2 0.63676(5) 0.64639(7) 0.42686(4) 0.01285(13) Uani d . 1 . . O O2 0.24699(13) -0.0998(2) 0.62514(11) 0.0147(4) Uani d . 1 . . C C2 0.5426(2) 0.3346(3) 0.27921(16) 0.0145(5) Uani d . 1 . . H H2A 0.5163 0.2593 0.2249 0.022 Uiso calc R 1 . . H H2B 0.6224 0.3112 0.3042 0.022 Uiso calc R 1 . . H H2C 0.5352 0.4494 0.2559 0.022 Uiso calc R 1 . . Cl Cl3 0.07120(5) 0.23663(7) 0.58529(4) 0.01694(14) Uani d . 1 . . C C3 0.0887(2) -0.1226(4) 0.73698(18) 0.0224(6) Uani d . 1 . . H H3A 0.1455 -0.1794 0.7841 0.034 Uiso calc R 1 . . H H3B 0.0138 -0.1718 0.7390 0.034 Uiso calc R 1 . . H H3C 0.0868 -0.0048 0.7539 0.034 Uiso calc R 1 . . Cl Cl4 -0.14497(5) -0.01787(7) 0.59997(4) 0.01570(14) Uani d . 1 . . C C4 0.1151(2) -0.3619(3) 0.6015(2) 0.0262(6) Uani d . 1 . . H H4A 0.1588 -0.4168 0.6583 0.039 Uiso calc R 1 . . H H4B 0.1458 -0.3934 0.5420 0.039 Uiso calc R 1 . . H H4C 0.0354 -0.3960 0.5956 0.039 Uiso calc R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 0.00907(15) 0.00689(15) 0.00724(14) 0.00048(9) 0.00081(11) 0.00072(9) S1 0.0118(3) 0.0075(3) 0.0088(3) 0.0004(2) 0.0006(2) 0.0000(2) Cl1 0.0137(3) 0.0105(3) 0.0133(3) 0.0032(2) -0.0017(2) 0.0002(2) Na1 0.0131(5) 0.0128(5) 0.0173(5) -0.0001(3) 0.0023(4) 0.0027(4) O1 0.0165(9) 0.0073(8) 0.0136(8) 0.0005(6) 0.0015(7) 0.0005(6) C1 0.0134(12) 0.0148(12) 0.0148(12) 0.0005(10) -0.0027(10) -0.0016(10) Ru2 0.00868(15) 0.00670(15) 0.01060(15) -0.00093(9) 0.00177(11) -0.00048(9) S2 0.0113(3) 0.0106(3) 0.0142(3) -0.0004(2) 0.0014(2) 0.0025(2) Cl2 0.0140(3) 0.0126(3) 0.0126(3) -0.0021(2) 0.0042(2) 0.0007(2) O2 0.0108(8) 0.0183(9) 0.0148(8) 0.0001(7) 0.0013(7) 0.0030(7) C2 0.0195(13) 0.0135(12) 0.0110(11) -0.0006(10) 0.0042(10) -0.0009(9) Cl3 0.0202(3) 0.0107(3) 0.0194(3) -0.0040(2) 0.0013(3) -0.0048(2) C3 0.0176(13) 0.0349(16) 0.0147(12) 0.0010(11) 0.0022(11) 0.0066(11) Cl4 0.0116(3) 0.0220(3) 0.0142(3) -0.0003(2) 0.0040(2) 0.0019(2) C4 0.0267(15) 0.0113(13) 0.0383(16) 0.0002(11) -0.0032(13) 0.0039(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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 S1 . 2.3350(5) y Ru1 S1 3_666 2.3351(5) ? Ru1 Cl1 . 2.3509(5) y Ru1 Cl1 3_666 2.3509(5) ? Ru1 Cl2 3_666 2.3551(5) ? Ru1 Cl2 . 2.3551(5) y S1 O1 . 1.4962(16) ? S1 C2 . 1.770(2) ? S1 C1 . 1.774(2) ? Cl1 Na1 1_565 2.8769(10) y Na1 O2 . 2.2974(18) y Na1 O1 . 2.4105(17) y Na1 O1 3_656 2.4155(18) y Na1 Cl4 3_556 2.7773(11) y Na1 Cl1 1_545 2.8769(10) y Na1 Cl2 3_666 2.9374(10) y Na1 Na1 3_656 3.4968(19) y O1 Na1 3_656 2.4156(18) y C1 H1A . 0.9800 ? C1 H1B . 0.9800 ? C1 H1C . 0.9800 ? Ru2 Cl3 3_556 2.3353(6) ? Ru2 Cl3 . 2.3353(6) y Ru2 S2 3_556 2.3373(6) ? Ru2 S2 . 2.3373(6) y Ru2 Cl4 3_556 2.3663(6) ? Ru2 Cl4 . 2.3663(6) y S2 O2 . 1.4863(16) ? S2 C4 . 1.772(3) ? S2 C3 . 1.776(2) ? Cl2 Na1 3_666 2.9374(10) y C2 H2A . 0.9800 ? C2 H2B . 0.9800 ? C2 H2C . 0.9800 ? C3 H3A . 0.9800 ? C3 H3B . 0.9800 ? C3 H3C . 0.9800 ? Cl4 Na1 3_556 2.7772(11) y C4 H4A . 0.9800 ? C4 H4B . 0.9800 ? C4 H4C . 0.9800 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 Ru1 S1 . 3_666 179.9990(10) ? S1 Ru1 Cl1 . . 92.250(19) ? S1 Ru1 Cl1 3_666 . 87.751(19) ? S1 Ru1 Cl1 . 3_666 87.751(19) ? S1 Ru1 Cl1 3_666 3_666 92.248(19) ? Cl1 Ru1 Cl1 . 3_666 180.0 ? S1 Ru1 Cl2 . 3_666 84.313(19) ? S1 Ru1 Cl2 3_666 3_666 95.687(19) ? Cl1 Ru1 Cl2 . 3_666 89.091(19) ? Cl1 Ru1 Cl2 3_666 3_666 90.909(19) ? S1 Ru1 Cl2 . . 95.686(19) ? S1 Ru1 Cl2 3_666 . 84.314(19) ? Cl1 Ru1 Cl2 . . 90.909(19) ? Cl1 Ru1 Cl2 3_666 . 89.091(19) ? Cl2 Ru1 Cl2 3_666 . 180.0 ? O1 S1 C2 . . 107.12(10) ? O1 S1 C1 . . 106.43(10) ? C2 S1 C1 . . 101.59(11) ? O1 S1 Ru1 . . 115.46(7) ? C2 S1 Ru1 . . 112.59(8) ? C1 S1 Ru1 . . 112.54(8) ? Ru1 Cl1 Na1 . 1_565 115.06(3) ? O2 Na1 O1 . . 176.27(7) ? O2 Na1 O1 . 3_656 93.79(6) ? O1 Na1 O1 . 3_656 87.14(6) ? O2 Na1 Cl4 . 3_556 80.56(5) ? O1 Na1 Cl4 . 3_556 100.01(5) ? O1 Na1 Cl4 3_656 3_556 156.08(5) ? O2 Na1 Cl1 . 1_545 88.98(5) ? O1 Na1 Cl1 . 1_545 94.75(5) ? O1 Na1 Cl1 3_656 1_545 75.12(4) ? Cl4 Na1 Cl1 3_556 1_545 81.52(3) ? O2 Na1 Cl2 . 3_666 99.39(5) ? O1 Na1 Cl2 . 3_666 76.89(4) ? O1 Na1 Cl2 3_656 3_666 108.18(5) ? Cl4 Na1 Cl2 3_556 3_666 95.69(3) ? Cl1 Na1 Cl2 1_545 3_666 170.66(4) ? O2 Na1 Na1 . 3_656 137.18(6) ? O1 Na1 Na1 . 3_656 43.63(4) ? O1 Na1 Na1 3_656 3_656 43.51(4) ? Cl4 Na1 Na1 3_556 3_656 138.71(5) ? Cl1 Na1 Na1 1_545 3_656 83.09(3) ? Cl2 Na1 Na1 3_666 3_656 93.39(4) ? S1 O1 Na1 . . 122.65(9) ? S1 O1 Na1 . 3_656 126.22(9) ? Na1 O1 Na1 . 3_656 92.86(6) ? S1 C1 H1A . . 109.5 ? S1 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? S1 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? Cl3 Ru2 Cl3 3_556 . 179.9990(10) ? Cl3 Ru2 S2 3_556 3_556 84.97(2) ? Cl3 Ru2 S2 . 3_556 95.03(2) ? Cl3 Ru2 S2 3_556 . 95.03(2) ? Cl3 Ru2 S2 . . 84.97(2) ? S2 Ru2 S2 3_556 . 179.9990(10) ? Cl3 Ru2 Cl4 3_556 3_556 89.90(2) ? Cl3 Ru2 Cl4 . 3_556 90.10(2) ? S2 Ru2 Cl4 3_556 3_556 90.63(2) ? S2 Ru2 Cl4 . 3_556 89.37(2) ? Cl3 Ru2 Cl4 3_556 . 90.10(2) ? Cl3 Ru2 Cl4 . . 89.90(2) ? S2 Ru2 Cl4 3_556 . 89.37(2) ? S2 Ru2 Cl4 . . 90.63(2) ? Cl4 Ru2 Cl4 3_556 . 180.0 ? O2 S2 C4 . . 107.04(12) ? O2 S2 C3 . . 106.03(11) ? C4 S2 C3 . . 100.97(14) ? O2 S2 Ru2 . . 116.54(7) ? C4 S2 Ru2 . . 112.72(10) ? C3 S2 Ru2 . . 112.19(9) ? Ru1 Cl2 Na1 . 3_666 111.02(3) ? S2 O2 Na1 . . 133.14(10) ? S1 C2 H2A . . 109.5 ? S1 C2 H2B . . 109.5 ? H2A C2 H2B . . 109.5 ? S1 C2 H2C . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? S2 C3 H3A . . 109.5 ? S2 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? S2 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? Ru2 Cl4 Na1 . 3_556 110.05(3) ? S2 C4 H4A . . 109.5 ? S2 C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? S2 C4 H4C . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? data_global _journal_data_validation_number ? _journal_date_recd_electronic 2010-02-16 _journal_date_accepted 2010-02-24 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2010 _journal_volume 66 _journal_issue 4 _journal_page_first m348 _journal_page_last m349 _journal_paper_category QM _journal_coeditor_code TK2632 _publ_contact_author_name 'Zden\O:O:S)(\m~2~-dimethyl sulfoxide-\k^2^O:S)ruthenium(III)sodium] ; loop_ _publ_author_name _publ_author_address 'Tr\'avn\'i\