# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1616 data_global _publ_author_name ; E. Iengo, G. Mestroni, S. Geremia, M. Calligaris and E. Alessio ; _publ_author_address ; Dipartimento di Scienze Chimiche, Universita' di Trieste, Via L. Giorgieri 1, I-34127 Trieste (Italy) ; _publ_section_title ; Synthesis, structural characterization and chemical behavior of new dimeric Ru(III) complexes [Na]2([trans-RuCl4(Me2SO-S)]2(mu-L)) and ([mer,cis-RuCl3(Me2SO)2]2(mu-L)) (L=bridging heterocyclic N-donor ligand) closely related to the antimetastatic complex Na[trans-RuCl4(Me2SO-S)(Him)] ; _publ_contact_author 'Enzo Alessio' _publ_contact_author_email alessi@univ.trieste.it _publ_contact_author_fax '++ 040 6763903' _publ_contact_author_phone '++ 040 6763961' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' data_1a # Compound 1a, [Na]2 [trans-RuCl4(Me2SO)]2(mu-pyrazine), 3(Me2SO), (H2O) _audit_creation_method SHELXL-97 _chemical_formula_moiety '(Na 1+)2, C8 H16 Cl8 N2 O2 Ru S2 2-, 3(C2 H6 O S), H2 O' _chemical_formula_sum 'C14 H36 Cl8 N2 Na2 O6 Ru2 S5' _chemical_formula_weight 1020.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'S' 'S' 0.1246 0.1234 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.419(3) _cell_length_b 11.048(3) _cell_length_c 11.210(7) _cell_angle_alpha 93.33(3) _cell_angle_beta 101.51(3) _cell_angle_gamma 92.61(3) _cell_volume 897.3(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 16 _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 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 1.785 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3689 _diffrn_reflns_av_R_equivalents 0.0936 _diffrn_reflns_av_sigmaI/netI 0.2965 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3502 _reflns_number_gt 1370 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 3502 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2880 _refine_ls_R_factor_gt 0.1129 _refine_ls_wR_factor_ref 0.2786 _refine_ls_wR_factor_gt 0.2194 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.1712(2) 0.34044(17) 0.27211(16) 0.0403(6) Uani 1 d . . . Cl1 Cl 0.0246(10) 0.2731(6) 0.4233(6) 0.078(2) Uani 1 d . . . Cl2 Cl 0.3356(7) 0.4089(6) 0.1288(5) 0.0653(18) Uani 1 d . . . Cl3 Cl -0.0010(8) 0.5112(5) 0.2603(5) 0.0623(17) Uani 1 d . . . Cl4 Cl 0.3485(10) 0.1704(6) 0.2935(5) 0.090(2) Uani 1 d . . . S1 S -0.0457(6) 0.2460(5) 0.1184(5) 0.0437(14) Uani 1 d . . . O1 O -0.024(2) 0.1231(12) 0.0736(13) 0.076(5) Uani 1 d . . . C1 C -0.080(4) 0.332(2) -0.007(2) 0.085(9) Uani 1 d . . . H1A H 0.0306 0.3362 -0.0394 0.128 Uiso 1 calc R . . H1B H -0.1091 0.4123 0.0170 0.128 Uiso 1 calc R . . H1C H -0.1794 0.2949 -0.0680 0.128 Uiso 1 calc R . . C2 C -0.265(3) 0.241(4) 0.155(3) 0.19(2) Uani 1 d . . . H2A H -0.3028 0.3219 0.1661 0.284 Uiso 1 calc R . . H2B H -0.2618 0.1998 0.2281 0.284 Uiso 1 calc R . . H2C H -0.3520 0.1976 0.0890 0.284 Uiso 1 calc R . . N1 N 0.369(2) 0.4366(17) 0.4112(14) 0.055(5) Uani 1 d . . . C3 C 0.551(3) 0.436(2) 0.4115(19) 0.078(9) Uani 1 d . . . H3 H 0.5899 0.3944 0.3471 0.093 Uiso 1 calc R . . C4 C 0.321(3) 0.507(3) 0.497(2) 0.086(10) Uani 1 d . . . H4 H 0.1967 0.5179 0.4953 0.103 Uiso 1 calc R . . Na1 Na 0.185(2) 0.0002(15) 0.0795(15) 0.054(4) Uiso 0.50 d P . . Na2 Na 0.303(2) 0.0104(15) 0.0884(14) 0.051(4) Uiso 0.50 d P . . S1S S 0.7549(16) -0.1344(11) 0.1796(11) 0.062(3) Uiso 0.50 d P . . O1S O 0.614(3) -0.083(2) 0.087(2) 0.045(7) Uiso 0.50 d P . . C1S C 0.650(5) -0.280(4) 0.213(4) 0.054(11) Uiso 0.50 d P . . C2S C 0.757(7) -0.066(5) 0.321(5) 0.084(16) Uiso 0.50 d P . . S2S S 0.4853(15) -0.1511(11) 0.3014(11) 0.059(3) Uiso 0.50 d P . . O2S O 0.400(4) -0.128(3) 0.172(2) 0.057(7) Uiso 0.50 d P . . C3S C 0.567(7) -0.306(5) 0.297(5) 0.090(17) Uiso 0.50 d P . . C4S C 0.300(9) -0.170(6) 0.394(6) 0.102(19) Uiso 0.50 d P . . S3S S 0.1916(17) -0.1652(11) 0.3334(12) 0.060(3) Uiso 0.50 d P . . O3S O 0.281(4) -0.129(3) 0.235(3) 0.066(8) Uiso 0.50 d P . . C5S C 0.287(7) -0.080(5) 0.466(5) 0.081(15) Uiso 0.50 d P . . C6S C -0.023(7) -0.094(5) 0.302(5) 0.090(17) Uiso 0.50 d P . . O4S O 0.658(4) -0.132(3) 0.026(3) 0.069(9) Uiso 0.50 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 0.0306(8) 0.0442(11) 0.0467(10) -0.0071(8) 0.0083(7) 0.0189(7) Cl1 0.112(5) 0.060(4) 0.073(4) 0.000(3) 0.045(4) 0.008(4) Cl2 0.052(3) 0.086(5) 0.061(4) -0.014(3) 0.024(3) -0.007(3) Cl3 0.076(4) 0.041(3) 0.065(4) -0.009(3) -0.001(3) 0.031(3) Cl4 0.119(5) 0.094(5) 0.059(4) -0.004(4) 0.007(4) 0.082(4) S1 0.038(3) 0.035(3) 0.057(3) -0.015(3) 0.012(2) 0.004(2) O1 0.125(14) 0.033(9) 0.061(10) -0.016(8) 0.002(10) 0.016(9) C1 0.12(2) 0.054(16) 0.065(16) 0.009(13) -0.033(15) 0.013(15) C2 0.038(14) 0.31(5) 0.20(3) -0.20(4) 0.069(18) -0.06(2) N1 0.046(10) 0.082(14) 0.038(10) -0.009(10) 0.010(8) 0.015(10) C3 0.034(11) 0.14(2) 0.053(14) -0.057(15) -0.002(10) 0.012(13) C4 0.028(10) 0.16(3) 0.069(16) -0.058(17) 0.014(11) 0.020(14) _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 N1 2.113(16) . ? Ru1 S1 2.275(5) . ? Ru1 Cl3 2.321(5) . ? Ru1 Cl1 2.327(7) . ? Ru1 Cl4 2.339(6) . ? Ru1 Cl2 2.341(6) . ? Cl4 Na2 2.773(17) . ? Cl4 Na1 2.977(17) . ? S1 O1 1.447(14) . ? S1 C1 1.72(2) . ? S1 C2 1.76(2) . ? S1 Na1 3.329(18) . ? O1 Na1 2.10(2) . ? O1 Na1 2.23(2) 2 ? O1 Na2 2.76(2) . ? O1 Na2 2.77(2) 2 ? N1 C4 1.32(2) . ? N1 C3 1.35(2) . ? C3 C4 1.35(3) 2_666 ? C4 C3 1.35(3) 2_666 ? Na1 Na2 0.862(17) . ? Na1 O1 2.23(2) 2 ? Na1 O2S 2.31(3) . ? Na1 O4S 2.34(4) 2_655 ? Na1 O3S 2.34(3) . ? Na1 O1S 2.77(3) 2_655 ? Na1 Na1 2.96(3) 2 ? Na1 Na2 3.73(3) 2 ? Na2 O2S 1.93(3) . ? Na2 O4S 1.96(3) 2_655 ? Na2 O1S 2.34(3) 2_655 ? Na2 O3S 2.34(3) . ? Na2 O1S 2.57(3) . ? Na2 O1 2.77(2) 2 ? Na2 S2S 3.18(2) . ? Na2 S1S 3.33(2) 2_655 ? Na2 Na1 3.73(3) 2 ? S1S O1S 1.48(3) . ? S1S C2S 1.72(5) . ? S1S O4S 1.73(3) . ? S1S C1S 1.85(4) . ? S1S C6S 1.94(5) 1_655 ? S1S Na2 3.33(2) 2_655 ? O1S O4S 0.96(3) . ? O1S Na2 2.34(3) 2_655 ? O1S Na1 2.77(3) 2_655 ? C1S C3S 1.27(6) . ? C1S S2S 2.24(4) . ? C2S C6S 1.73(7) 1_655 ? C2S S2S 2.15(5) . ? S2S O2S 1.51(3) . ? S2S O3S 1.58(3) . ? S2S C3S 1.85(6) . ? S2S C4S 1.89(6) . ? S2S S3S 2.278(17) . ? O2S O3S 1.24(4) . ? C4S S3S 0.95(6) . ? C4S C5S 1.27(7) . ? C4S O3S 1.84(7) . ? S3S O3S 1.46(3) . ? S3S C5S 1.72(5) . ? S3S C6S 1.79(5) . ? C6S C2S 1.73(7) 1_455 ? C6S S1S 1.94(5) 1_455 ? O4S Na2 1.96(3) 2_655 ? O4S Na1 2.34(4) 2_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 N1 Ru1 S1 177.1(6) . . ? N1 Ru1 Cl3 88.5(5) . . ? S1 Ru1 Cl3 88.99(19) . . ? N1 Ru1 Cl1 88.1(5) . . ? S1 Ru1 Cl1 93.3(2) . . ? Cl3 Ru1 Cl1 89.8(2) . . ? N1 Ru1 Cl4 89.5(5) . . ? S1 Ru1 Cl4 93.1(2) . . ? Cl3 Ru1 Cl4 177.4(2) . . ? Cl1 Ru1 Cl4 88.7(3) . . ? N1 Ru1 Cl2 88.8(5) . . ? S1 Ru1 Cl2 89.9(2) . . ? Cl3 Ru1 Cl2 91.8(2) . . ? Cl1 Ru1 Cl2 176.5(2) . . ? Cl4 Ru1 Cl2 89.6(2) . . ? Ru1 Cl4 Na2 115.5(4) . . ? Ru1 Cl4 Na1 105.2(4) . . ? Na2 Cl4 Na1 16.8(4) . . ? O1 S1 C1 106.5(10) . . ? O1 S1 C2 104.3(14) . . ? C1 S1 C2 101.5(18) . . ? O1 S1 Ru1 120.3(7) . . ? C1 S1 Ru1 110.4(8) . . ? C2 S1 Ru1 112.0(9) . . ? O1 S1 Na1 24.7(7) . . ? C1 S1 Na1 113.0(10) . . ? C2 S1 Na1 123.5(15) . . ? Ru1 S1 Na1 96.5(3) . . ? S1 O1 Na1 138.6(11) . . ? S1 O1 Na1 133.4(10) . 2 ? Na1 O1 Na1 86.1(8) . 2 ? S1 O1 Na2 126.4(10) . . ? Na1 O1 Na2 13.3(6) . . ? Na1 O1 Na2 96.0(8) 2 . ? S1 O1 Na2 122.2(9) . 2 ? Na1 O1 Na2 98.9(8) . 2 ? Na1 O1 Na2 15.6(5) 2 2 ? Na2 O1 Na2 110.0(6) . 2 ? C4 N1 C3 116.5(17) . . ? C4 N1 Ru1 121.9(14) . . ? C3 N1 Ru1 121.5(13) . . ? C4 C3 N1 121.8(17) 2_666 . ? N1 C4 C3 121.3(17) . 2_666 ? Na2 Na1 O1 132(2) . . ? Na2 Na1 O1 120.1(19) . 2 ? O1 Na1 O1 93.9(8) . 2 ? Na2 Na1 O2S 53.7(17) . . ? O1 Na1 O2S 155.3(12) . . ? O1 Na1 O2S 101.2(10) 2 . ? Na2 Na1 O4S 54.2(18) . 2_655 ? O1 Na1 O4S 89.6(11) . 2_655 ? O1 Na1 O4S 101.2(10) 2 2_655 ? O2S Na1 O4S 106.3(12) . 2_655 ? Na2 Na1 O3S 79.5(18) . . ? O1 Na1 O3S 126.1(12) . . ? O1 Na1 O3S 104.2(11) 2 . ? O2S Na1 O3S 30.9(9) . . ? O4S Na1 O3S 133.6(13) 2_655 . ? Na2 Na1 O1S 51.8(16) . 2_655 ? O1 Na1 O1S 103.8(10) . 2_655 ? O1 Na1 O1S 86.9(9) 2 2_655 ? O2S Na1 O1S 96.6(11) . 2_655 ? O4S Na1 O1S 19.4(9) 2_655 2_655 ? O3S Na1 O1S 127.2(11) . 2_655 ? Na2 Na1 Na1 149(2) . 2 ? O1 Na1 Na1 48.8(6) . 2 ? O1 Na1 Na1 45.1(6) 2 2 ? O2S Na1 Na1 142.3(12) . 2 ? O4S Na1 Na1 98.2(11) 2_655 2 ? O3S Na1 Na1 127.1(12) . 2 ? O1S Na1 Na1 97.4(9) 2_655 2 ? Na2 Na1 Cl4 68.0(15) . . ? O1 Na1 Cl4 79.5(6) . . ? O1 Na1 Cl4 171.9(9) 2 . ? O2S Na1 Cl4 83.5(8) . . ? O4S Na1 Cl4 83.6(9) 2_655 . ? O3S Na1 Cl4 76.5(8) . . ? O1S Na1 Cl4 99.2(8) 2_655 . ? Na1 Na1 Cl4 128.1(9) 2 . ? Na2 Na1 S1 117.2(18) . . ? O1 Na1 S1 16.7(4) . . ? O1 Na1 S1 110.0(7) 2 . ? O2S Na1 S1 145.6(9) . . ? O4S Na1 S1 82.1(9) 2_655 . ? O3S Na1 S1 122.9(10) . . ? O1S Na1 S1 99.4(7) 2_655 . ? Na1 Na1 S1 65.0(6) 2 . ? Cl4 Na1 S1 63.9(3) . . ? Na2 Na1 Na2 155.9(17) . 2 ? O1 Na1 Na2 47.2(6) . 2 ? O1 Na1 Na2 47.4(5) 2 2 ? O2S Na1 Na2 139.9(10) . 2 ? O4S Na1 Na2 104.4(9) 2_655 2 ? O3S Na1 Na2 121.4(10) . 2 ? O1S Na1 Na2 104.2(7) 2_655 2 ? Na1 Na1 Na2 6.8(5) 2 2 ? Cl4 Na1 Na2 125.2(6) . 2 ? S1 Na1 Na2 63.8(4) . 2 ? Na1 Na2 O2S 105(2) . . ? Na1 Na2 O4S 105(2) . 2_655 ? O2S Na2 O4S 145.7(16) . 2_655 ? Na1 Na2 O1S 111.4(19) . 2_655 ? O2S Na2 O1S 125.8(13) . 2_655 ? O4S Na2 O1S 23.8(10) 2_655 2_655 ? Na1 Na2 O3S 79.3(19) . . ? O2S Na2 O3S 31.9(10) . . ? O4S Na2 O3S 175.1(13) 2_655 . ? O1S Na2 O3S 156.4(13) 2_655 . ? Na1 Na2 O1S 149(2) . . ? O2S Na2 O1S 52.3(11) . . ? O4S Na2 O1S 93.5(12) 2_655 . ? O1S Na2 O1S 76.9(10) 2_655 . ? O3S Na2 O1S 83.6(11) . . ? Na1 Na2 O1 34.2(15) . . ? O2S Na2 O1 132.9(12) . . ? O4S Na2 O1 81.3(11) 2_655 . ? O1S Na2 O1 98.0(9) 2_655 . ? O3S Na2 O1 101.6(10) . . ? O1S Na2 O1 174.8(10) . . ? Na1 Na2 O1 44.3(15) . 2 ? O2S Na2 O1 95.0(10) . 2 ? O4S Na2 O1 95.2(11) 2_655 2 ? O1S Na2 O1 85.0(8) 2_655 2 ? O3S Na2 O1 89.5(9) . 2 ? O1S Na2 O1 110.1(9) . 2 ? O1 Na2 O1 70.0(6) . 2 ? Na1 Na2 Cl4 95.2(17) . . ? O2S Na2 Cl4 96.7(10) . . ? O4S Na2 Cl4 96.5(11) 2_655 . ? O1S Na2 Cl4 117.7(9) 2_655 . ? O3S Na2 Cl4 80.7(8) . . ? O1S Na2 Cl4 107.7(8) . . ? O1 Na2 Cl4 73.7(5) . . ? O1 Na2 Cl4 139.5(7) 2 . ? Na1 Na2 S2S 107.7(19) . . ? O2S Na2 S2S 19.3(8) . . ? O4S Na2 S2S 147.1(12) 2_655 . ? O1S Na2 S2S 135.9(9) 2_655 . ? O3S Na2 S2S 28.4(7) . . ? O1S Na2 S2S 59.1(7) . . ? O1 Na2 S2S 126.0(7) . . ? O1 Na2 S2S 110.5(6) 2 . ? Cl4 Na2 S2S 77.4(5) . . ? Na1 Na2 S1S 89.4(17) . 2_655 ? O2S Na2 S1S 142.7(11) . 2_655 ? O4S Na2 S1S 23.8(9) 2_655 2_655 ? O1S Na2 S1S 22.7(6) 2_655 2_655 ? O3S Na2 S1S 160.6(9) . 2_655 ? O1S Na2 S1S 98.8(8) . 2_655 ? O1 Na2 S1S 76.3(5) . 2_655 ? O1 Na2 S1S 71.6(5) 2 2_655 ? Cl4 Na2 S1S 116.3(6) . 2_655 ? S2S Na2 S1S 157.5(6) . 2_655 ? Na1 Na2 Na1 24.1(17) . 2 ? O2S Na2 Na1 120.6(11) . 2 ? O4S Na2 Na1 84.0(10) 2_655 2 ? O1S Na2 Na1 87.4(7) 2_655 2 ? O3S Na2 Na1 100.7(9) . 2 ? O1S Na2 Na1 142.7(8) . 2 ? O1 Na2 Na1 36.6(4) . 2 ? O1 Na2 Na1 33.9(4) 2 2 ? Cl4 Na2 Na1 109.6(6) . 2 ? S2S Na2 Na1 128.7(6) . 2 ? S1S Na2 Na1 65.9(4) 2_655 2 ? O1S S1S C2S 110(2) . . ? O1S S1S O4S 33.9(12) . . ? C2S S1S O4S 144(2) . . ? O1S S1S C1S 106.0(17) . . ? C2S S1S C1S 94(2) . . ? O4S S1S C1S 100.0(17) . . ? O1S S1S C6S 143(2) . 1_655 ? C2S S1S C6S 56(2) . 1_655 ? O4S S1S C6S 144(2) . 1_655 ? C1S S1S C6S 109(2) . 1_655 ? O1S S1S Na2 37.7(11) . 2_655 ? C2S S1S Na2 128.6(19) . 2_655 ? O4S S1S Na2 27.3(11) . 2_655 ? C1S S1S Na2 127.3(14) . 2_655 ? C6S S1S Na2 120.1(18) 1_655 2_655 ? O4S O1S S1S 87(3) . . ? O4S O1S Na2 55(3) . 2_655 ? S1S O1S Na2 119.6(15) . 2_655 ? O4S O1S Na2 133(3) . . ? S1S O1S Na2 134.6(16) . . ? Na2 O1S Na2 103.1(10) 2_655 . ? O4S O1S Na1 54(3) . 2_655 ? S1S O1S Na1 103.4(13) . 2_655 ? Na2 O1S Na1 16.8(5) 2_655 2_655 ? Na2 O1S Na1 117.2(11) . 2_655 ? C3S C1S S1S 131(4) . . ? C3S C1S S2S 56(3) . . ? S1S C1S S2S 80.0(16) . . ? S1S C2S C6S 68(3) . 1_655 ? S1S C2S S2S 85(2) . . ? C6S C2S S2S 142(4) 1_655 . ? O2S S2S O3S 47.2(14) . . ? O2S S2S C3S 106(2) . . ? O3S S2S C3S 119(2) . . ? O2S S2S C4S 110(2) . . ? O3S S2S C4S 63(2) . . ? C3S S2S C4S 101(3) . . ? O2S S2S C2S 101.8(18) . . ? O3S S2S C2S 138(2) . . ? C3S S2S C2S 94(2) . . ? C4S S2S C2S 139(2) . . ? O2S S2S C1S 83.8(16) . . ? O3S S2S C1S 119.5(16) . . ? C3S S2S C1S 34.5(19) . . ? C4S S2S C1S 134(2) . . ? C2S S2S C1S 73.2(18) . . ? O2S S2S S3S 86.1(12) . . ? O3S S2S S3S 39.5(12) . . ? C3S S2S S3S 107.5(19) . . ? C4S S2S S3S 24.1(18) . . ? C2S S2S S3S 154.3(16) . . ? C1S S2S S3S 132.3(12) . . ? O2S S2S Na2 25.0(11) . . ? O3S S2S Na2 44.8(12) . . ? C3S S2S Na2 131.2(18) . . ? C4S S2S Na2 104(2) . . ? C2S S2S Na2 94.6(15) . . ? C1S S2S Na2 104.7(12) . . ? S3S S2S Na2 82.2(6) . . ? O3S O2S S2S 69.7(19) . . ? O3S O2S Na2 93(2) . . ? S2S O2S Na2 135.7(18) . . ? O3S O2S Na1 76(2) . . ? S2S O2S Na1 135.5(17) . . ? Na2 O2S Na1 21.1(6) . . ? C1S C3S S2S 90(4) . . ? S3S C4S C5S 101(6) . . ? S3S C4S O3S 52(3) . . ? C5S C4S O3S 112(5) . . ? S3S C4S S2S 101(5) . . ? C5S C4S S2S 115(5) . . ? O3S C4S S2S 50.2(19) . . ? C4S S3S O3S 97(4) . . ? C4S S3S C5S 47(4) . . ? O3S S3S C5S 110(2) . . ? C4S S3S C6S 143(5) . . ? O3S S3S C6S 103(2) . . ? C5S S3S C6S 97(3) . . ? C4S S3S S2S 54(4) . . ? O3S S3S S2S 43.7(12) . . ? C5S S3S S2S 83.2(18) . . ? C6S S3S S2S 142(2) . . ? O2S O3S S3S 157(3) . . ? O2S O3S S2S 63.1(18) . . ? S3S O3S S2S 96.8(18) . . ? O2S O3S C4S 129(3) . . ? S3S O3S C4S 31(2) . . ? S2S O3S C4S 67(2) . . ? O2S O3S Na1 73(2) . . ? S3S O3S Na1 130.0(19) . . ? S2S O3S Na1 128.0(18) . . ? C4S O3S Na1 151(3) . . ? O2S O3S Na2 55.3(18) . . ? S3S O3S Na2 147.3(19) . . ? S2S O3S Na2 106.8(16) . . ? C4S O3S Na2 153(3) . . ? Na1 O3S Na2 21.2(5) . . ? C4S C5S S3S 33(3) . . ? C2S C6S S3S 155(4) 1_455 . ? C2S C6S S1S 56(2) 1_455 1_455 ? S3S C6S S1S 131(3) . 1_455 ? O1S O4S S1S 59(2) . . ? O1S O4S Na2 101(3) . 2_655 ? S1S O4S Na2 129.0(18) . 2_655 ? O1S O4S Na1 107(3) . 2_655 ? S1S O4S Na1 114.3(15) . 2_655 ? Na2 O4S Na1 20.8(6) 2_655 2_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 N1 Ru1 S1 O1 151(10) . . . . ? Cl3 Ru1 S1 O1 179.7(9) . . . . ? Cl1 Ru1 S1 O1 -90.6(9) . . . . ? Cl4 Ru1 S1 O1 -1.8(9) . . . . ? Cl2 Ru1 S1 O1 87.9(9) . . . . ? N1 Ru1 S1 C1 27(10) . . . . ? Cl3 Ru1 S1 C1 55.1(10) . . . . ? Cl1 Ru1 S1 C1 144.8(10) . . . . ? Cl4 Ru1 S1 C1 -126.4(10) . . . . ? Cl2 Ru1 S1 C1 -36.8(10) . . . . ? N1 Ru1 S1 C2 -86(10) . . . . ? Cl3 Ru1 S1 C2 -57.3(18) . . . . ? Cl1 Ru1 S1 C2 32.4(18) . . . . ? Cl4 Ru1 S1 C2 121.3(18) . . . . ? Cl2 Ru1 S1 C2 -149.1(17) . . . . ? S1 Ru1 N1 C4 69(11) . . . . ? Cl3 Ru1 N1 C4 41(2) . . . . ? Cl1 Ru1 N1 C4 -49(2) . . . . ? Cl4 Ru1 N1 C4 -138(2) . . . . ? Cl2 Ru1 N1 C4 133(2) . . . . ? S1 Ru1 N1 C3 -106(10) . . . . ? Cl3 Ru1 N1 C3 -134(2) . . . . ? Cl1 Ru1 N1 C3 136(2) . . . . ? Cl4 Ru1 N1 C3 47(2) . . . . ? Cl2 Ru1 N1 C3 -43(2) . . . . ? C4 N1 C3 C4 7(5) . . . 2_666 ? Ru1 N1 C3 C4 -177(2) . . . 2_666 ? C3 N1 C4 C3 -7(5) . . . 2_666 ? Ru1 N1 C4 C3 177(2) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.582 _refine_diff_density_min -1.800 _refine_diff_density_rms 0.235 data_1b # Compound 1b, [Na]2 [trans-RuCl4(Me2SO)]2(mu-pyrimidine), 3(Me2SO), (H2O) _audit_creation_method SHELXL-97 _chemical_formula_moiety '(Na 1+)2, C8 H16 Cl8 N2 O2 Ru S2 2-, 3(C2 H6 O1 S1), H2 O' _chemical_formula_sum 'C14 H36 Cl8 N2 Na2 O6 Ru2 S5' _chemical_formula_weight 1020.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'S' 'S' 0.1246 0.1234 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 11.3710(10) _cell_length_b 14.6130(10) _cell_length_c 22.578(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.415(8) _cell_angle_gamma 90.00 _cell_volume 3728.2(5) _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 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.718 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6529 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.97 _reflns_number_total 6306 _reflns_number_gt 4457 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+3.0890P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 6306 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 1.188 _refine_ls_shift/su_mean 0.033 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.66653(3) 0.28263(2) 0.855910(19) 0.02932(13) Uani 1 d . . . Ru2 Ru 0.34763(3) 0.28268(3) 0.62595(2) 0.03203(14) Uani 1 d . . . S1 S 0.77192(10) 0.20395(8) 0.93137(7) 0.0377(4) Uani 1 d . . . S2 S 0.26276(10) 0.19947(8) 0.54639(7) 0.0375(4) Uani 1 d . . . Cl1 Cl 0.74483(12) 0.19781(9) 0.78040(7) 0.0522(4) Uani 1 d . . . Cl2 Cl 0.58466(12) 0.37022(9) 0.92764(7) 0.0458(4) Uani 1 d . . . Cl3 Cl 0.51367(11) 0.17491(8) 0.85535(7) 0.0466(4) Uani 1 d . . . Cl4 Cl 0.81585(10) 0.39302(9) 0.85161(7) 0.0432(4) Uani 1 d . . . Cl5 Cl 0.16843(10) 0.35495(9) 0.64199(7) 0.0464(4) Uani 1 d . . . Cl6 Cl 0.52902(12) 0.21618(11) 0.61413(8) 0.0611(5) Uani 1 d . . . Cl7 Cl 0.30406(13) 0.16575(9) 0.69101(7) 0.0519(4) Uani 1 d . . . Cl8 Cl 0.39004(13) 0.40518(10) 0.56334(7) 0.0532(4) Uani 1 d . . . O1 O 0.8769(3) 0.2481(2) 0.96422(17) 0.0460(10) Uani 1 d . . . O2 O 0.1335(3) 0.2072(2) 0.53032(17) 0.0449(10) Uani 1 d . . . N1 N 0.5620(3) 0.3575(2) 0.78879(19) 0.0306(10) Uani 1 d . . . N2 N 0.4329(3) 0.3578(2) 0.69921(19) 0.0323(10) Uani 1 d . . . C1 C 0.8220(6) 0.0966(4) 0.9072(3) 0.070(2) Uani 1 d . . . H1A H 0.8730 0.1061 0.8766 0.104 Uiso 1 calc R . . H1B H 0.7552 0.0603 0.8916 0.104 Uiso 1 calc R . . H1C H 0.8648 0.0653 0.9402 0.104 Uiso 1 calc R . . C2 C 0.6814(5) 0.1682(5) 0.9850(3) 0.067(2) Uani 1 d . . . H2A H 0.7274 0.1329 1.0151 0.101 Uiso 1 calc R . . H2B H 0.6179 0.1314 0.9663 0.101 Uiso 1 calc R . . H2C H 0.6494 0.2209 1.0030 0.101 Uiso 1 calc R . . C3 C 0.2924(6) 0.0805(4) 0.5543(3) 0.074(2) Uani 1 d . . . H3A H 0.2493 0.0558 0.5849 0.111 Uiso 1 calc R . . H3B H 0.3756 0.0712 0.5651 0.111 Uiso 1 calc R . . H3C H 0.2682 0.0500 0.5173 0.111 Uiso 1 calc R . . C4 C 0.3317(5) 0.2220(5) 0.4822(3) 0.066(2) Uani 1 d . . . H4A H 0.3022 0.1803 0.4511 0.099 Uiso 1 calc R . . H4B H 0.4157 0.2142 0.4909 0.099 Uiso 1 calc R . . H4C H 0.3149 0.2837 0.4693 0.099 Uiso 1 calc R . . C5 C 0.5052(4) 0.3154(3) 0.7414(2) 0.0323(13) Uani 1 d . . . H5 H 0.5166 0.2527 0.7375 0.039 Uiso 1 calc R . . C6 C 0.5472(4) 0.4486(3) 0.7941(2) 0.0374(14) Uani 1 d . . . H6 H 0.5863 0.4796 0.8265 0.045 Uiso 1 calc R . . C7 C 0.4748(4) 0.4957(3) 0.7522(2) 0.0422(15) Uani 1 d . . . H7 H 0.4648 0.5586 0.7554 0.051 Uiso 1 calc R . . C8 C 0.4179(4) 0.4485(3) 0.7055(3) 0.0441(15) Uani 1 d . . . H8 H 0.3673 0.4797 0.6772 0.053 Uiso 1 calc R . . S1A S -0.1022(2) 0.11598(12) 0.58858(10) 0.0785(6) Uani 1 d . . . O1A O -0.0605(4) 0.0494(3) 0.54465(19) 0.0615(12) Uani 1 d . . . C1A C -0.2422(7) 0.0756(7) 0.6007(4) 0.117(4) Uani 1 d . . . H1A1 H -0.2954 0.0822 0.5648 0.176 Uiso 1 calc R . . H1A2 H -0.2713 0.1103 0.6321 0.176 Uiso 1 calc R . . H1A3 H -0.2367 0.0122 0.6118 0.176 Uiso 1 calc R . . C2A C -0.0264(7) 0.0906(6) 0.6591(3) 0.090(3) Uani 1 d . . . H2A1 H -0.0409 0.0281 0.6691 0.135 Uiso 1 calc R . . H2A2 H -0.0539 0.1302 0.6885 0.135 Uiso 1 calc R . . H2A3 H 0.0570 0.0997 0.6580 0.135 Uiso 1 calc R . . O1B O 1.1165(4) 0.3597(4) 0.8864(2) 0.0720(15) Uani 1 d . . . S1B S 1.1536(7) 0.2780(6) 0.8490(4) 0.095(4) Uani 0.322(8) d P A 1 C1B C 1.252(5) 0.329(3) 0.814(3) 0.15(3) Uani 0.322(8) d P A 1 H1B1 H 1.2138 0.3722 0.7858 0.227 Uiso 0.322(8) calc PR A 1 H1B2 H 1.2943 0.2850 0.7930 0.227 Uiso 0.322(8) calc PR A 1 H1B3 H 1.3071 0.3615 0.8419 0.227 Uiso 0.322(8) calc PR A 1 C2B C 1.0575(19) 0.263(4) 0.7869(17) 0.16(3) Uani 0.322(8) d P A 1 H2B1 H 1.0051 0.2135 0.7929 0.239 Uiso 0.322(8) calc PR A 1 H2B2 H 1.1006 0.2499 0.7537 0.239 Uiso 0.322(8) calc PR A 1 H2B3 H 1.0123 0.3183 0.7789 0.239 Uiso 0.322(8) calc PR A 1 S1C S 1.1142(2) 0.3376(2) 0.82321(16) 0.0643(15) Uani 0.678(8) d P A 2 C1C C 1.2661(13) 0.3223(19) 0.8104(12) 0.119(11) Uani 0.678(8) d P A 2 H1C1 H 1.3079 0.3791 0.8173 0.179 Uiso 0.678(8) calc PR A 2 H1C2 H 1.2697 0.3033 0.7699 0.179 Uiso 0.678(8) calc PR A 2 H1C3 H 1.3019 0.2765 0.8370 0.179 Uiso 0.678(8) calc PR A 2 C2C C 1.086(2) 0.2209(13) 0.8208(13) 0.208(16) Uani 0.678(8) d P A 2 H2C1 H 1.1532 0.1885 0.8397 0.312 Uiso 0.678(8) calc PR A 2 H2C2 H 1.0705 0.2015 0.7800 0.312 Uiso 0.678(8) calc PR A 2 H2C3 H 1.0180 0.2080 0.8412 0.312 Uiso 0.678(8) calc PR A 2 Na1 Na 0.00935(18) 0.32845(15) 0.53969(11) 0.0538(6) Uani 1 d . . . Na2 Na 0.99264(17) 0.38867(14) 0.95573(10) 0.0441(6) Uani 1 d . . . OW O 0.1213(4) 0.4222(3) 0.4868(3) 0.0802(15) Uani 1 d G . . H1W H 0.1883 0.4144 0.5155 0.120 Uiso 1 d G . . H2W H 0.1436 0.4694 0.4621 0.120 Uiso 1 d G . . O1D O -0.1178(3) 0.4235(3) 0.5863(2) 0.0562(12) Uani 1 d . . . S1D S -0.1486(6) 0.3954(7) 0.6508(3) 0.096(3) Uani 0.442(12) d P B 1 C1D C -0.291(2) 0.441(3) 0.6565(17) 0.16(2) Uani 0.442(12) d P B 1 H1D1 H -0.3012 0.4964 0.6335 0.247 Uiso 0.442(12) calc PR B 1 H1D2 H -0.2992 0.4544 0.6975 0.247 Uiso 0.442(12) calc PR B 1 H1D3 H -0.3502 0.3974 0.6416 0.247 Uiso 0.442(12) calc PR B 1 C2D C -0.0819(19) 0.4799(18) 0.6979(9) 0.128(11) Uani 0.442(12) d P B 1 H2D1 H -0.0757 0.5355 0.6758 0.192 Uiso 0.442(12) calc PR B 1 H2D2 H -0.0044 0.4600 0.7139 0.192 Uiso 0.442(12) calc PR B 1 H2D3 H -0.1291 0.4907 0.7299 0.192 Uiso 0.442(12) calc PR B 1 S1E S -0.1438(3) 0.4573(4) 0.6452(2) 0.068(2) Uani 0.558(12) d P B 2 C1E C -0.294(2) 0.493(2) 0.6331(14) 0.147(13) Uani 0.558(12) d P B 2 H1E1 H -0.3050 0.5321 0.5986 0.221 Uiso 0.558(12) calc PR B 2 H1E2 H -0.3140 0.5263 0.6673 0.221 Uiso 0.558(12) calc PR B 2 H1E3 H -0.3445 0.4406 0.6268 0.221 Uiso 0.558(12) calc PR B 2 C2E C -0.165(3) 0.3517(19) 0.6853(11) 0.203(15) Uani 0.558(12) d P B 2 H2E1 H -0.2032 0.3073 0.6583 0.305 Uiso 0.558(12) calc PR B 2 H2E2 H -0.2135 0.3635 0.7166 0.305 Uiso 0.558(12) calc PR B 2 H2E3 H -0.0895 0.3286 0.7021 0.305 Uiso 0.558(12) calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02980(18) 0.02929(17) 0.0263(4) 0.00033(17) -0.00827(16) -0.00368(14) Ru2 0.03103(18) 0.03437(19) 0.0282(4) -0.00183(18) -0.00779(17) 0.00682(15) S1 0.0398(6) 0.0339(6) 0.0351(11) 0.0051(5) -0.0155(6) -0.0055(5) S2 0.0377(6) 0.0399(7) 0.0320(11) -0.0063(6) -0.0089(6) 0.0093(5) Cl1 0.0534(7) 0.0567(8) 0.0445(13) -0.0107(7) -0.0025(7) 0.0109(6) Cl2 0.0553(7) 0.0434(7) 0.0393(12) -0.0054(6) 0.0084(7) -0.0071(6) Cl3 0.0473(7) 0.0399(6) 0.0482(12) 0.0044(6) -0.0141(6) -0.0169(5) Cl4 0.0358(6) 0.0467(7) 0.0451(12) 0.0062(6) -0.0049(6) -0.0113(5) Cl5 0.0380(6) 0.0549(8) 0.0440(12) -0.0100(7) -0.0058(6) 0.0123(5) Cl6 0.0423(7) 0.0838(10) 0.0538(13) -0.0186(9) -0.0092(7) 0.0271(7) Cl7 0.0698(9) 0.0389(7) 0.0434(12) 0.0039(6) -0.0102(7) -0.0035(6) Cl8 0.0595(8) 0.0557(8) 0.0425(13) 0.0098(7) -0.0028(7) -0.0062(6) O1 0.0444(19) 0.0446(18) 0.043(3) 0.0063(17) -0.0208(18) -0.0082(15) O2 0.0391(18) 0.048(2) 0.044(3) -0.0125(18) -0.0105(17) 0.0021(15) N1 0.0325(19) 0.033(2) 0.024(3) -0.0008(18) -0.0061(18) -0.0011(15) N2 0.0345(19) 0.033(2) 0.027(3) -0.0010(18) -0.0080(18) 0.0040(15) C1 0.092(5) 0.039(3) 0.069(6) -0.003(3) -0.033(4) 0.010(3) C2 0.057(4) 0.093(5) 0.048(6) 0.034(4) -0.012(3) -0.014(3) C3 0.101(5) 0.041(3) 0.070(6) -0.019(3) -0.031(4) 0.032(3) C4 0.056(3) 0.104(5) 0.040(6) -0.024(4) 0.011(3) -0.004(3) C5 0.030(2) 0.036(2) 0.029(4) 0.001(2) -0.006(2) 0.0045(19) C6 0.045(3) 0.032(2) 0.033(4) -0.003(2) -0.008(2) -0.003(2) C7 0.056(3) 0.028(2) 0.038(5) 0.000(2) -0.016(3) 0.001(2) C8 0.051(3) 0.034(3) 0.042(5) 0.004(2) -0.020(3) 0.007(2) S1A 0.1186(16) 0.0595(10) 0.0590(17) 0.0001(9) 0.0164(12) 0.0329(10) O1A 0.096(3) 0.050(2) 0.043(4) -0.003(2) 0.025(2) 0.015(2) C1A 0.085(6) 0.159(9) 0.106(8) -0.020(7) 0.007(5) 0.063(6) C2A 0.116(7) 0.096(6) 0.058(7) -0.008(5) 0.007(5) 0.012(5) O1B 0.061(3) 0.115(4) 0.041(5) -0.013(3) 0.012(2) 0.017(3) S1B 0.103(6) 0.082(6) 0.098(8) -0.014(5) 0.009(5) 0.012(4) C1B 0.26(7) 0.06(2) 0.14(6) -0.03(3) 0.07(4) -0.03(3) C2B 0.023(9) 0.38(7) 0.08(3) -0.13(4) 0.013(12) -0.03(2) S1C 0.0582(15) 0.086(2) 0.047(3) -0.0027(16) 0.0002(13) 0.0174(13) C1C 0.042(6) 0.24(3) 0.078(19) -0.079(16) 0.029(7) -0.025(9) C2C 0.27(3) 0.112(14) 0.26(4) -0.107(19) 0.11(2) -0.110(17) Na1 0.0484(12) 0.0570(13) 0.0515(18) -0.0113(12) -0.0139(10) 0.0132(10) Na2 0.0491(11) 0.0480(11) 0.0344(17) -0.0034(10) 0.0010(10) -0.0066(9) OW 0.080(3) 0.070(3) 0.085(5) 0.014(3) -0.016(3) -0.006(2) O1D 0.057(2) 0.071(3) 0.040(4) 0.000(2) 0.005(2) 0.011(2) S1D 0.127(5) 0.090(7) 0.076(7) -0.005(4) 0.029(4) -0.013(4) C1D 0.055(13) 0.34(6) 0.10(3) 0.01(3) 0.027(14) -0.05(2) C2D 0.121(18) 0.21(3) 0.049(18) -0.070(17) 0.006(13) -0.027(17) S1E 0.075(2) 0.069(3) 0.063(4) -0.018(2) 0.020(2) -0.0139(18) C1E 0.133(18) 0.20(3) 0.12(3) -0.001(19) 0.084(16) 0.080(18) C2E 0.28(3) 0.19(3) 0.15(3) 0.13(2) 0.09(2) 0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.122(4) . ? Ru1 S1 2.2814(13) . ? Ru1 Cl2 2.3377(15) . ? Ru1 Cl3 2.3440(12) . ? Ru1 Cl4 2.3519(12) . ? Ru1 Cl1 2.3611(15) . ? Ru2 N2 2.127(4) . ? Ru2 S2 2.2911(14) . ? Ru2 Cl6 2.3223(13) . ? Ru2 Cl7 2.3421(15) . ? Ru2 Cl5 2.3588(12) . ? Ru2 Cl8 2.3639(15) . ? S1 O1 1.482(3) . ? S1 C2 1.754(6) . ? S1 C1 1.776(6) . ? S2 O2 1.479(3) . ? S2 C4 1.754(7) . ? S2 C3 1.777(5) . ? Cl4 Na2 2.918(3) . ? Cl5 Na1 2.797(3) . ? O1 Na1 2.418(4) 4_666 ? O1 Na2 2.458(4) . ? O2 Na1 2.290(4) . ? O2 Na2 2.600(4) 4_465 ? N1 C5 1.337(6) . ? N1 C6 1.350(6) . ? N2 C5 1.339(6) . ? N2 C8 1.345(6) . ? C6 C7 1.369(7) . ? C7 C8 1.361(7) . ? S1A O1A 1.504(4) . ? S1A C1A 1.747(9) . ? S1A C2A 1.763(8) . ? S1A Na2 3.300(3) 4_465 ? O1A Na2 2.342(5) 4_465 ? O1A Na2 2.473(4) 2_646 ? O1B S1C 1.459(6) . ? O1B S1B 1.547(9) . ? O1B Na2 2.260(5) . ? S1B C1B 1.63(5) . ? S1B C2B 1.69(3) . ? S1C C2C 1.736(18) . ? S1C C1C 1.797(15) . ? Na1 OW 2.294(6) . ? Na1 O1D 2.338(5) . ? Na1 O1 2.418(4) 4_465 ? Na1 S1D 3.388(7) . ? Na1 Na2 3.690(3) 4_465 ? Na2 O1A 2.342(5) 4_666 ? Na2 O1A 2.473(4) 2_656 ? Na2 O2 2.600(4) 4_666 ? Na2 S1A 3.300(3) 4_666 ? Na2 Na1 3.690(3) 4_666 ? Na2 Na2 3.813(4) 3_767 ? O1D S1E 1.480(6) . ? O1D S1D 1.590(8) . ? S1D C2D 1.75(2) . ? S1D C1D 1.77(3) . ? S1E C1E 1.78(2) . ? S1E C2E 1.82(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 S1 177.05(12) . . ? N1 Ru1 Cl2 88.74(12) . . ? S1 Ru1 Cl2 88.58(5) . . ? N1 Ru1 Cl3 89.23(10) . . ? S1 Ru1 Cl3 89.59(5) . . ? Cl2 Ru1 Cl3 91.09(5) . . ? N1 Ru1 Cl4 88.07(10) . . ? S1 Ru1 Cl4 93.16(5) . . ? Cl2 Ru1 Cl4 89.90(5) . . ? Cl3 Ru1 Cl4 177.10(5) . . ? N1 Ru1 Cl1 88.92(12) . . ? S1 Ru1 Cl1 93.77(5) . . ? Cl2 Ru1 Cl1 177.65(5) . . ? Cl3 Ru1 Cl1 89.01(5) . . ? Cl4 Ru1 Cl1 89.89(5) . . ? N2 Ru2 S2 177.77(10) . . ? N2 Ru2 Cl6 88.37(11) . . ? S2 Ru2 Cl6 89.40(5) . . ? N2 Ru2 Cl7 89.93(11) . . ? S2 Ru2 Cl7 90.26(5) . . ? Cl6 Ru2 Cl7 91.13(6) . . ? N2 Ru2 Cl5 88.64(10) . . ? S2 Ru2 Cl5 93.59(5) . . ? Cl6 Ru2 Cl5 177.00(5) . . ? Cl7 Ru2 Cl5 89.05(5) . . ? N2 Ru2 Cl8 88.19(11) . . ? S2 Ru2 Cl8 91.68(5) . . ? Cl6 Ru2 Cl8 90.28(6) . . ? Cl7 Ru2 Cl8 177.62(6) . . ? Cl5 Ru2 Cl8 89.44(5) . . ? O1 S1 C2 106.6(3) . . ? O1 S1 C1 105.7(3) . . ? C2 S1 C1 100.5(4) . . ? O1 S1 Ru1 118.75(15) . . ? C2 S1 Ru1 111.5(2) . . ? C1 S1 Ru1 112.0(2) . . ? O2 S2 C4 107.9(3) . . ? O2 S2 C3 105.7(3) . . ? C4 S2 C3 99.8(4) . . ? O2 S2 Ru2 118.16(16) . . ? C4 S2 Ru2 111.1(2) . . ? C3 S2 Ru2 112.5(2) . . ? Ru1 Cl4 Na2 112.79(7) . . ? Ru2 Cl5 Na1 107.54(7) . . ? S1 O1 Na1 123.7(2) . 4_666 ? S1 O1 Na2 137.2(2) . . ? Na1 O1 Na2 98.35(13) 4_666 . ? S2 O2 Na1 130.0(2) . . ? S2 O2 Na2 129.9(2) . 4_465 ? Na1 O2 Na2 97.78(13) . 4_465 ? C5 N1 C6 118.2(4) . . ? C5 N1 Ru1 121.1(3) . . ? C6 N1 Ru1 120.7(3) . . ? C5 N2 C8 117.1(4) . . ? C5 N2 Ru2 120.3(3) . . ? C8 N2 Ru2 122.6(3) . . ? N1 C5 N2 124.0(4) . . ? N1 C6 C7 120.4(5) . . ? C8 C7 C6 118.6(5) . . ? N2 C8 C7 121.8(4) . . ? O1A S1A C1A 104.2(4) . . ? O1A S1A C2A 107.5(3) . . ? C1A S1A C2A 98.6(4) . . ? O1A S1A Na2 39.43(17) . 4_465 ? C1A S1A Na2 122.1(3) . 4_465 ? C2A S1A Na2 129.7(3) . 4_465 ? S1A O1A Na2 116.5(2) . 4_465 ? S1A O1A Na2 137.6(3) . 2_646 ? Na2 O1A Na2 104.69(16) 4_465 2_646 ? S1C O1B S1B 43.3(4) . . ? S1C O1B Na2 140.7(3) . . ? S1B O1B Na2 138.8(4) . . ? O1B S1B C1B 98.9(18) . . ? O1B S1B C2B 111.1(15) . . ? C1B S1B C2B 94(3) . . ? O1B S1C C2C 103.4(10) . . ? O1B S1C C1C 105.8(8) . . ? C2C S1C C1C 93.0(12) . . ? O2 Na1 OW 91.76(18) . . ? O2 Na1 O1D 156.90(19) . . ? OW Na1 O1D 106.6(2) . . ? O2 Na1 O1 85.32(13) . 4_465 ? OW Na1 O1 104.35(19) . 4_465 ? O1D Na1 O1 102.95(15) . 4_465 ? O2 Na1 Cl5 80.50(11) . . ? OW Na1 Cl5 90.09(15) . . ? O1D Na1 Cl5 85.51(13) . . ? O1 Na1 Cl5 160.07(13) 4_465 . ? O2 Na1 S1D 132.4(2) . . ? OW Na1 S1D 125.7(2) . . ? O1D Na1 S1D 24.47(19) . . ? O1 Na1 S1D 108.38(17) 4_465 . ? Cl5 Na1 S1D 72.32(13) . . ? O2 Na1 Na2 44.28(9) . 4_465 ? OW Na1 Na2 104.25(17) . 4_465 ? O1D Na1 Na2 137.97(13) . 4_465 ? O1 Na1 Na2 41.23(9) 4_465 4_465 ? Cl5 Na1 Na2 122.32(8) . 4_465 ? S1D Na1 Na2 128.85(18) . 4_465 ? O1B Na2 O1A 155.06(19) . 4_666 ? O1B Na2 O1 106.12(18) . . ? O1A Na2 O1 93.69(15) 4_666 . ? O1B Na2 O1A 87.54(18) . 2_656 ? O1A Na2 O1A 75.31(16) 4_666 2_656 ? O1 Na2 O1A 164.55(17) . 2_656 ? O1B Na2 O2 87.79(17) . 4_666 ? O1A Na2 O2 81.49(16) 4_666 4_666 ? O1 Na2 O2 78.21(12) . 4_666 ? O1A Na2 O2 110.13(15) 2_656 4_666 ? O1B Na2 Cl4 82.67(14) . . ? O1A Na2 Cl4 117.50(14) 4_666 . ? O1 Na2 Cl4 75.79(10) . . ? O1A Na2 Cl4 99.42(13) 2_656 . ? O2 Na2 Cl4 148.49(11) 4_666 . ? O1B Na2 S1A 156.68(16) . 4_666 ? O1A Na2 S1A 24.07(10) 4_666 4_666 ? O1 Na2 S1A 71.32(11) . 4_666 ? O1A Na2 S1A 99.00(12) 2_656 4_666 ? O2 Na2 S1A 68.92(11) 4_666 4_666 ? Cl4 Na2 S1A 117.84(8) . 4_666 ? O1B Na2 Na1 101.21(15) . 4_666 ? O1A Na2 Na1 83.98(12) 4_666 4_666 ? O1 Na2 Na1 40.43(9) . 4_666 ? O1A Na2 Na1 145.13(14) 2_656 4_666 ? O2 Na2 Na1 37.94(8) 4_666 4_666 ? Cl4 Na2 Na1 115.08(7) . 4_666 ? S1A Na2 Na1 61.22(6) 4_666 4_666 ? O1B Na2 Na2 121.95(17) . 3_767 ? O1A Na2 Na2 38.85(10) 4_666 3_767 ? O1 Na2 Na2 131.66(15) . 3_767 ? O1A Na2 Na2 36.45(10) 2_656 3_767 ? O2 Na2 Na2 97.60(12) 4_666 3_767 ? Cl4 Na2 Na2 112.94(9) . 3_767 ? S1A Na2 Na2 62.65(7) 4_666 3_767 ? Na1 Na2 Na2 117.88(10) 4_666 3_767 ? S1E O1D S1D 34.5(2) . . ? S1E O1D Na1 143.0(3) . . ? S1D O1D Na1 118.0(4) . . ? O1D S1D C2D 104.5(10) . . ? O1D S1D C1D 105.4(12) . . ? C2D S1D C1D 91.6(16) . . ? O1D S1D Na1 37.5(2) . . ? C2D S1D Na1 115.1(8) . . ? C1D S1D Na1 136.7(13) . . ? O1D S1E C1E 104.2(10) . . ? O1D S1E C2E 102.4(9) . . ? C1E S1E C2E 98.5(12) . . ? 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 N1 Ru1 S1 O1 -100.6(19) . . . . ? Cl2 Ru1 S1 O1 -76.0(2) . . . . ? Cl3 Ru1 S1 O1 -167.1(2) . . . . ? Cl4 Ru1 S1 O1 13.8(2) . . . . ? Cl1 Ru1 S1 O1 103.9(2) . . . . ? N1 Ru1 S1 C2 24(2) . . . . ? Cl2 Ru1 S1 C2 48.5(3) . . . . ? Cl3 Ru1 S1 C2 -42.6(3) . . . . ? Cl4 Ru1 S1 C2 138.3(3) . . . . ? Cl1 Ru1 S1 C2 -131.6(3) . . . . ? N1 Ru1 S1 C1 136(2) . . . . ? Cl2 Ru1 S1 C1 160.3(3) . . . . ? Cl3 Ru1 S1 C1 69.2(3) . . . . ? Cl4 Ru1 S1 C1 -109.9(3) . . . . ? Cl1 Ru1 S1 C1 -19.8(3) . . . . ? N2 Ru2 S2 O2 -180(100) . . . . ? Cl6 Ru2 S2 O2 176.78(19) . . . . ? Cl7 Ru2 S2 O2 85.66(19) . . . . ? Cl5 Ru2 S2 O2 -3.41(19) . . . . ? Cl8 Ru2 S2 O2 -92.95(19) . . . . ? N2 Ru2 S2 C4 -54(3) . . . . ? Cl6 Ru2 S2 C4 -57.8(3) . . . . ? Cl7 Ru2 S2 C4 -148.9(3) . . . . ? Cl5 Ru2 S2 C4 122.0(3) . . . . ? Cl8 Ru2 S2 C4 32.5(3) . . . . ? N2 Ru2 S2 C3 57(3) . . . . ? Cl6 Ru2 S2 C3 53.1(3) . . . . ? Cl7 Ru2 S2 C3 -38.0(3) . . . . ? Cl5 Ru2 S2 C3 -127.1(3) . . . . ? Cl8 Ru2 S2 C3 143.4(3) . . . . ? S1 Ru1 N1 C5 -112.1(19) . . . . ? Cl2 Ru1 N1 C5 -136.8(4) . . . . ? Cl3 Ru1 N1 C5 -45.7(4) . . . . ? Cl4 Ru1 N1 C5 133.3(4) . . . . ? Cl1 Ru1 N1 C5 43.4(4) . . . . ? S1 Ru1 N1 C6 65(2) . . . . ? Cl2 Ru1 N1 C6 40.4(4) . . . . ? Cl3 Ru1 N1 C6 131.5(4) . . . . ? Cl4 Ru1 N1 C6 -49.5(4) . . . . ? Cl1 Ru1 N1 C6 -139.5(4) . . . . ? S2 Ru2 N2 C5 -51(3) . . . . ? Cl6 Ru2 N2 C5 -47.8(4) . . . . ? Cl7 Ru2 N2 C5 43.4(4) . . . . ? Cl5 Ru2 N2 C5 132.4(4) . . . . ? Cl8 Ru2 N2 C5 -138.1(4) . . . . ? S2 Ru2 N2 C8 128(3) . . . . ? Cl6 Ru2 N2 C8 132.1(4) . . . . ? Cl7 Ru2 N2 C8 -136.8(4) . . . . ? Cl5 Ru2 N2 C8 -47.8(4) . . . . ? Cl8 Ru2 N2 C8 41.7(4) . . . . ? C6 N1 C5 N2 -1.0(7) . . . . ? Ru1 N1 C5 N2 176.3(4) . . . . ? C8 N2 C5 N1 0.2(7) . . . . ? Ru2 N2 C5 N1 -180.0(4) . . . . ? C5 N1 C6 C7 0.6(8) . . . . ? Ru1 N1 C6 C7 -176.7(4) . . . . ? N1 C6 C7 C8 0.5(8) . . . . ? C5 N2 C8 C7 1.0(8) . . . . ? Ru2 N2 C8 C7 -178.8(4) . . . . ? C6 C7 C8 N2 -1.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.677 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.677 _refine_diff_density_max 0.761 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.094 data_1c # Compound 1c, [Na]2 [trans-RuCl4(Me2SO)]2(mu-4,4' bipyridyl)], 3(Me2SO), (H2O) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '(Na 1+)2, C14 H20 Cl8 N2 O2 Ru S2 2-, 5.6(H2 O)' _chemical_formula_sum 'C14 H31.20 Cl8 N2 Na2 O7.60 Ru2 S2' _chemical_formula_weight 945.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'S' 'S' 0.1246 0.1234 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.363(3) _cell_length_b 7.5610(10) _cell_length_c 16.162(6) _cell_angle_alpha 90.00 _cell_angle_beta 119.00(2) _cell_angle_gamma 90.00 _cell_volume 3245.2(13) _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 1.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 1.783 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4041 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.97 _reflns_number_total 3900 _reflns_number_gt 2802 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+10.4402P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 3900 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.060 _refine_ls_shift/su_mean 0.006 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.645329(14) 0.32564(5) 0.76031(3) 0.02268(11) Uani 1 d . . . Cl1 Cl 0.63999(5) 0.17267(19) 0.62834(8) 0.0369(3) Uani 1 d . . . Cl2 Cl 0.56659(5) 0.19672(17) 0.72536(9) 0.0351(3) Uani 1 d . . . Cl3 Cl 0.72369(5) 0.43936(19) 0.79933(9) 0.0379(3) Uani 1 d . . . Cl4 Cl 0.64575(6) 0.46908(18) 0.88909(9) 0.0399(3) Uani 1 d . . . S1 S 0.60699(5) 0.56163(16) 0.66057(8) 0.0300(3) Uani 1 d . . . O1 O 0.55471(15) 0.5350(5) 0.5832(3) 0.0474(11) Uani 1 d . . . N1 N 0.68320(14) 0.1087(5) 0.8494(3) 0.0252(8) Uani 1 d . . . C1 C 0.6054(3) 0.7539(8) 0.7198(5) 0.0552(17) Uani 1 d . . . H1A H 0.5934 0.8510 0.6761 0.083 Uiso 1 calc R . . H1B H 0.6387 0.7798 0.7698 0.083 Uiso 1 calc R . . H1C H 0.5833 0.7362 0.7459 0.083 Uiso 1 calc R . . C2 C 0.6423(3) 0.6414(10) 0.6070(5) 0.0575(19) Uani 1 d . . . H2A H 0.6441 0.5512 0.5670 0.086 Uiso 1 calc R . . H2B H 0.6757 0.6718 0.6552 0.086 Uiso 1 calc R . . H2C H 0.6261 0.7443 0.5698 0.086 Uiso 1 calc R . . C3 C 0.71938(18) 0.0234(6) 0.8410(3) 0.0269(10) Uani 1 d . . . H3 H 0.7270 0.0605 0.7945 0.032 Uiso 1 calc R . . C4 C 0.74590(19) -0.1170(7) 0.8979(3) 0.0294(10) Uani 1 d . . . H4 H 0.7706 -0.1726 0.8889 0.035 Uiso 1 calc R . . C5 C 0.73590(16) -0.1751(6) 0.9679(3) 0.0231(9) Uani 1 d . . . C6 C 0.69823(18) -0.0861(7) 0.9763(3) 0.0302(11) Uani 1 d . . . H6 H 0.6900 -0.1215 1.0222 0.036 Uiso 1 calc R . . C7 C 0.67313(9) 0.0526(4) 0.91814(18) 0.0302(11) Uani 1 d . . . H7 H 0.6484 0.1103 0.9260 0.036 Uiso 1 calc R . . NaA Na 0.49166(9) 0.3261(4) 0.56385(18) 0.0577(18) Uani 0.566(8) d PR . . NaB Na 0.51726(9) 0.2639(4) 0.52165(18) 0.066(3) Uani 0.434(8) d PR . . O1S O 0.44177(9) 0.1212(4) 0.58269(18) 0.059(3) Uani 0.586(15) d PR . . O2S O 0.48079(9) -0.0290(4) 0.49987(18) 0.086(6) Uani 0.461(15) d PR . . O3S O 0.50000(9) 0.5211(4) 0.75000(18) 0.175(19) Uani 0.66(4) d SPR . . O4S O 0.46524(9) 0.5244(4) 0.64893(18) 0.061(4) Uani 0.461(17) d PR . . O5S O 0.54823(9) 0.2757(4) 0.39954(18) 0.122(7) Uani 0.539(17) d PR . . O6S O 0.53704(9) 0.1029(4) 0.34583(18) 0.139(11) Uani 0.42(2) d PR . . 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 0.02667(19) 0.02291(18) 0.01800(17) 0.00192(15) 0.01047(13) 0.00074(16) Cl1 0.0467(7) 0.0407(7) 0.0262(6) -0.0043(6) 0.0199(5) 0.0007(6) Cl2 0.0341(6) 0.0359(7) 0.0367(6) 0.0038(5) 0.0182(5) -0.0013(5) Cl3 0.0326(6) 0.0415(7) 0.0360(7) 0.0043(6) 0.0137(5) -0.0068(6) Cl4 0.0567(8) 0.0363(7) 0.0274(6) -0.0041(5) 0.0209(6) 0.0038(6) S1 0.0314(6) 0.0267(6) 0.0264(6) 0.0067(5) 0.0098(5) 0.0013(5) O1 0.040(2) 0.044(2) 0.036(2) 0.0110(19) 0.0001(17) -0.0066(19) N1 0.028(2) 0.0243(19) 0.0223(18) 0.0015(16) 0.0114(16) 0.0012(16) C1 0.075(5) 0.029(3) 0.051(4) 0.003(3) 0.023(4) 0.003(3) C2 0.060(4) 0.068(5) 0.058(4) 0.037(4) 0.039(3) 0.014(3) C3 0.031(2) 0.029(2) 0.026(2) 0.007(2) 0.017(2) 0.001(2) C4 0.032(3) 0.034(3) 0.027(2) 0.006(2) 0.019(2) 0.005(2) C5 0.027(2) 0.021(2) 0.0174(19) 0.0029(18) 0.0071(17) 0.0013(19) C6 0.032(3) 0.036(3) 0.027(2) 0.008(2) 0.018(2) 0.007(2) C7 0.033(3) 0.035(3) 0.028(2) 0.005(2) 0.018(2) 0.007(2) NaA 0.039(2) 0.082(4) 0.038(2) 0.023(2) 0.0079(19) -0.004(2) NaB 0.067(5) 0.046(4) 0.050(4) 0.006(3) 0.001(3) -0.002(3) O1S 0.056(5) 0.064(6) 0.055(5) -0.002(4) 0.026(4) -0.005(4) O2S 0.072(9) 0.104(11) 0.052(7) -0.002(7) 0.006(7) -0.025(8) O3S 0.25(3) 0.050(9) 0.38(5) 0.000 0.28(4) 0.000 O4S 0.047(6) 0.088(9) 0.040(6) 0.003(5) 0.014(5) -0.005(6) O5S 0.086(9) 0.115(13) 0.116(11) -0.038(9) 0.012(8) 0.020(8) O6S 0.20(2) 0.096(15) 0.20(2) 0.009(15) 0.17(2) -0.003(14) _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 N1 2.117(4) . ? Ru S1 2.3061(13) . ? Ru Cl3 2.3115(14) . ? Ru Cl4 2.3415(15) . ? Ru Cl1 2.3618(14) . ? Ru Cl2 2.3824(13) . ? Cl1 NaB 3.332(3) . ? Cl2 NaA 2.681(3) . ? Cl2 NaB 2.926(3) . ? S1 O1 1.483(4) . ? S1 C1 1.754(6) . ? S1 C2 1.778(6) . ? O1 NaB 2.321(5) . ? O1 NaA 2.342(4) 5_666 ? O1 NaA 2.383(5) . ? O1 NaB 2.523(5) 5_666 ? N1 C3 1.337(6) . ? N1 C7 1.355(5) . ? C3 C4 1.380(7) . ? C4 C5 1.378(6) . ? C5 C6 1.390(6) . ? C5 C5 1.494(8) 7_647 ? C6 C7 1.367(5) . ? NaA NaB 1.3433 . ? NaA O1S 2.2879 . ? NaA O1 2.342(4) 5_666 ? NaA O4S 2.4191 . ? NaA O2S 2.764(6) 5_656 ? NaA O2S 2.8385 . ? NaA NaB 3.351(5) 5_666 ? NaA NaA 3.527(5) 5_666 ? NaB O2S 1.816(6) 5_656 ? NaB O2S 2.4244 . ? NaB O1 2.523(5) 5_666 ? NaB O5S 2.5664 . ? NaB NaA 3.351(5) 5_666 ? NaB NaB 3.691(5) 5_666 ? NaB NaB 4.100(5) 5_656 ? O2S O2S 1.244(5) 5_656 ? O2S NaB 1.816(6) 5_656 ? O2S NaA 2.764(6) 5_656 ? O3S O4S 1.4530 . ? O3S O4S 1.453(5) 2_656 ? O4S O5S 1.660(5) 5_666 ? O5S O6S 1.5130 . ? O5S O4S 1.660(5) 5_666 ? 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 N1 Ru S1 177.13(11) . . ? N1 Ru Cl3 87.41(11) . . ? S1 Ru Cl3 90.40(5) . . ? N1 Ru Cl4 89.25(11) . . ? S1 Ru Cl4 92.65(5) . . ? Cl3 Ru Cl4 91.37(6) . . ? N1 Ru Cl1 90.69(11) . . ? S1 Ru Cl1 87.55(5) . . ? Cl3 Ru Cl1 92.26(5) . . ? Cl4 Ru Cl1 176.36(5) . . ? N1 Ru Cl2 89.77(11) . . ? S1 Ru Cl2 92.43(5) . . ? Cl3 Ru Cl2 177.17(5) . . ? Cl4 Ru Cl2 88.43(5) . . ? Cl1 Ru Cl2 87.93(5) . . ? Ru Cl1 NaB 86.32(7) . . ? Ru Cl2 NaA 111.21(8) . . ? Ru Cl2 NaB 95.92(7) . . ? NaA Cl2 NaB 27.3 . . ? O1 S1 C1 105.8(3) . . ? O1 S1 C2 106.6(3) . . ? C1 S1 C2 99.6(4) . . ? O1 S1 Ru 117.12(17) . . ? C1 S1 Ru 113.5(2) . . ? C2 S1 Ru 112.6(2) . . ? S1 O1 NaB 125.7(2) . . ? S1 O1 NaA 131.8(2) . 5_666 ? NaB O1 NaA 91.87(16) . 5_666 ? S1 O1 NaA 131.6(2) . . ? NaB O1 NaA 33.16(7) . . ? NaA O1 NaA 96.58(16) 5_666 . ? S1 O1 NaB 135.1(2) . 5_666 ? NaB O1 NaB 99.18(16) . 5_666 ? NaA O1 NaB 31.78(6) 5_666 5_666 ? NaA O1 NaB 86.11(15) . 5_666 ? C3 N1 C7 117.1(4) . . ? C3 N1 Ru 120.4(3) . . ? C7 N1 Ru 122.5(3) . . ? N1 C3 C4 123.1(4) . . ? C5 C4 C3 120.2(4) . . ? C4 C5 C6 116.5(4) . . ? C4 C5 C5 122.2(5) . 7_647 ? C6 C5 C5 121.3(5) . 7_647 ? C7 C6 C5 121.0(4) . . ? N1 C7 C6 122.1(3) . . ? NaB NaA O1S 114.5 . . ? NaB NaA O1 81.55(14) . 5_666 ? O1S NaA O1 109.11(12) . 5_666 ? NaB NaA O1 70.90(13) . . ? O1S NaA O1 166.69(11) . . ? O1 NaA O1 83.42(16) 5_666 . ? NaB NaA O4S 159.8 . . ? O1S NaA O4S 85.4 . . ? O1 NaA O4S 95.56(14) 5_666 . ? O1 NaA O4S 88.93(13) . . ? NaB NaA Cl2 86.55(7) . . ? O1S NaA Cl2 85.83(6) . . ? O1 NaA Cl2 163.78(16) 5_666 . ? O1 NaA Cl2 82.29(12) . . ? O4S NaA Cl2 91.80(7) . . ? NaB NaA O2S 34.14(11) . 5_656 ? O1S NaA O2S 80.72(11) . 5_656 ? O1 NaA O2S 97.35(18) 5_666 5_656 ? O1 NaA O2S 102.63(18) . 5_656 ? O4S NaA O2S 163.54(11) . 5_656 ? Cl2 NaA O2S 78.40(11) . 5_656 ? NaB NaA O2S 58.5 . . ? O1S NaA O2S 56.0 . . ? O1 NaA O2S 98.51(13) 5_666 . ? O1 NaA O2S 128.24(13) . . ? O4S NaA O2S 141.4 . . ? Cl2 NaA O2S 84.46(7) . . ? O2S NaA O2S 25.62(11) 5_656 . ? NaB NaA NaB 93.76(10) . 5_666 ? O1S NaA NaB 139.01(9) . 5_666 ? O1 NaA NaB 43.81(11) 5_666 5_666 ? O1 NaA NaB 48.70(11) . 5_666 ? O4S NaA NaB 71.23(10) . 5_666 ? Cl2 NaA NaB 126.86(13) . 5_666 ? O2S NaA NaB 125.22(18) 5_656 5_666 ? O2S NaA NaB 138.85(10) . 5_666 ? NaB NaA NaA 71.42(10) . 5_666 ? O1S NaA NaA 151.01(8) . 5_666 ? O1 NaA NaA 42.15(11) 5_666 5_666 ? O1 NaA NaA 41.27(10) . 5_666 ? O4S NaA NaA 92.97(10) . 5_666 ? Cl2 NaA NaA 123.16(12) . 5_666 ? O2S NaA NaA 103.45(17) 5_656 5_666 ? O2S NaA NaA 121.08(10) . 5_666 ? NaB NaA NaA 22.3 5_666 5_666 ? NaA NaB O2S 121.34(18) . 5_656 ? NaA NaB O1 75.95(14) . . ? O2S NaB O1 153.0(2) 5_656 . ? NaA NaB O2S 93.3 . . ? O2S NaB O2S 29.98(17) 5_656 . ? O1 NaB O2S 164.46(12) . . ? NaA NaB O1 66.67(12) . 5_666 ? O2S NaB O1 124.0(2) 5_656 5_666 ? O1 NaB O1 80.82(16) . 5_666 ? O2S NaB O1 105.49(11) . 5_666 ? NaA NaB O5S 153.7 . . ? O2S NaB O5S 80.13(17) 5_656 . ? O1 NaB O5S 90.73(13) . . ? O2S NaB O5S 103.4 . . ? O1 NaB O5S 89.07(12) 5_666 . ? NaA NaB Cl2 66.17(7) . . ? O2S NaB Cl2 89.95(16) 5_656 . ? O1 NaB Cl2 78.12(12) . . ? O2S NaB Cl2 87.32(6) . . ? O1 NaB Cl2 131.63(16) 5_666 . ? O5S NaB Cl2 133.86(6) . . ? NaA NaB Cl1 125.94(6) . . ? O2S NaB Cl1 76.38(16) 5_656 . ? O1 NaB Cl1 76.62(12) . . ? O2S NaB Cl1 101.74(5) . . ? O1 NaB Cl1 149.24(14) 5_666 . ? O5S NaB Cl1 70.75(6) . . ? Cl2 NaB Cl1 63.12(6) . . ? NaA NaB NaA 86.24(10) . 5_666 ? O2S NaB NaA 146.0(3) 5_656 5_666 ? O1 NaB NaA 44.32(11) . 5_666 ? O2S NaB NaA 147.70(8) . 5_666 ? O1 NaB NaA 45.19(11) 5_666 5_666 ? O5S NaB NaA 68.74(10) . 5_666 ? Cl2 NaB NaA 121.31(13) . 5_666 ? Cl1 NaB NaA 104.57(11) . 5_666 ? NaA NaB NaB 64.95(9) . 5_666 ? O2S NaB NaB 160.4(2) 5_656 5_666 ? O1 NaB NaB 42.45(11) . 5_666 ? O2S NaB NaB 142.03(8) . 5_666 ? O1 NaB NaB 38.37(10) 5_666 5_666 ? O5S NaB NaB 89.83(9) . 5_666 ? Cl2 NaB NaB 108.95(12) . 5_666 ? Cl1 NaB NaB 116.23(11) . 5_666 ? NaA NaB NaB 21.3 5_666 5_666 ? NaA NaB NaB 105.34(8) . 5_656 ? O2S NaB NaB 17.19(10) 5_656 5_656 ? O1 NaB NaB 164.70(15) . 5_656 ? O2S NaB NaB 12.79(8) . 5_656 ? O1 NaB NaB 113.92(14) 5_666 5_656 ? O5S NaB NaB 93.51(8) . 5_656 ? Cl2 NaB NaB 88.40(9) . 5_656 ? Cl1 NaB NaB 90.92(9) . 5_656 ? NaA NaB NaB 150.15(15) 5_666 5_656 ? NaB NaB NaB 152.09(14) 5_666 5_656 ? O2S O2S NaB 103.2(4) 5_656 5_656 ? O2S O2S NaB 46.8(3) 5_656 . ? NaB O2S NaB 150.02(17) 5_656 . ? O2S O2S NaA 80.5(3) 5_656 5_656 ? NaB O2S NaA 24.52(9) 5_656 5_656 ? NaB O2S NaA 126.67(11) . 5_656 ? O2S O2S NaA 73.9(3) 5_656 . ? NaB O2S NaA 170.39(15) 5_656 . ? NaB O2S NaA 28.2 . . ? NaA O2S NaA 154.38(11) 5_656 . ? O4S O3S O4S 178.0 . 2_656 ? O3S O4S O5S 115.15(18) . 5_666 ? O3S O4S NaA 111.6 . . ? O5S O4S NaA 111.7(2) 5_666 . ? O6S O5S O4S 125.45(19) . 5_666 ? O6S O5S NaB 110.3 . . ? O4S O5S NaB 107.2(2) 5_666 . ? 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 N1 Ru S1 O1 116(2) . . . . ? Cl3 Ru S1 O1 156.6(2) . . . . ? Cl4 Ru S1 O1 -112.1(2) . . . . ? Cl1 Ru S1 O1 64.3(2) . . . . ? Cl2 Ru S1 O1 -23.5(2) . . . . ? N1 Ru S1 C1 -120(2) . . . . ? Cl3 Ru S1 C1 -79.7(3) . . . . ? Cl4 Ru S1 C1 11.7(3) . . . . ? Cl1 Ru S1 C1 -172.0(3) . . . . ? Cl2 Ru S1 C1 100.2(3) . . . . ? N1 Ru S1 C2 -8(2) . . . . ? Cl3 Ru S1 C2 32.4(3) . . . . ? Cl4 Ru S1 C2 123.8(3) . . . . ? Cl1 Ru S1 C2 -59.8(3) . . . . ? Cl2 Ru S1 C2 -147.7(3) . . . . ? S1 Ru N1 C3 -9(3) . . . . ? Cl3 Ru N1 C3 -49.6(4) . . . . ? Cl4 Ru N1 C3 -141.0(4) . . . . ? Cl1 Ru N1 C3 42.6(4) . . . . ? Cl2 Ru N1 C3 130.5(4) . . . . ? S1 Ru N1 C7 169(2) . . . . ? Cl3 Ru N1 C7 128.8(3) . . . . ? Cl4 Ru N1 C7 37.4(3) . . . . ? Cl1 Ru N1 C7 -138.9(3) . . . . ? Cl2 Ru N1 C7 -51.0(3) . . . . ? C7 N1 C3 C4 0.5(7) . . . . ? Ru N1 C3 C4 179.0(4) . . . . ? N1 C3 C4 C5 -0.4(8) . . . . ? C3 C4 C5 C6 0.5(7) . . . . ? C3 C4 C5 C5 -179.1(5) . . . 7_647 ? C4 C5 C6 C7 -0.6(7) . . . . ? C5 C5 C6 C7 179.0(5) 7_647 . . . ? C3 N1 C7 C6 -0.6(6) . . . . ? Ru N1 C7 C6 -179.1(3) . . . . ? C5 C6 C7 N1 0.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.464 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.464 _refine_diff_density_max 1.042 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.135 data_3a # Compound 3a, [mer-RuCl3(Me2SO)2]2(mu-pyrazine), 2(CHCl3) _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C12 H28 Cl6 N2 O4 Ru2 S4, 2(CHCl3)' _chemical_formula_sum 'C14 H30 Cl12 N2 O4 Ru2 S4' _chemical_formula_weight 1046.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'S' 'S' 0.1246 0.1234 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 10.770(3) _cell_length_b 14.526(3) _cell_length_c 11.764(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.070(10) _cell_angle_gamma 90.00 _cell_volume 1812.1(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 ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.975 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71100 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5495 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 29.96 _reflns_number_total 5267 _reflns_number_gt 4043 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+1.6237P] 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 5267 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.171 _refine_ls_shift/su_mean 0.006 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.23645(2) 0.110661(15) 0.193603(19) 0.02861(7) Uani 1 d . . . Cl1 Cl 0.21961(9) -0.00667(6) 0.32465(7) 0.0465(2) Uani 1 d . . . Cl2 Cl 0.23424(9) 0.23147(6) 0.06082(7) 0.0462(2) Uani 1 d . . . Cl3 Cl 0.38772(8) 0.03261(6) 0.11251(8) 0.0470(2) Uani 1 d . . . S1 S 0.39171(8) 0.17763(6) 0.32358(7) 0.03800(18) Uani 1 d . . . S2 S 0.10073(9) 0.28139(6) 0.28942(8) 0.0456(2) Uani 1 d . . . O1 O 0.3500(3) 0.2316(2) 0.4161(2) 0.0551(7) Uani 1 d . . . O2 O 0.0912(2) 0.17785(16) 0.2554(2) 0.0403(5) Uani 1 d . . . N1 N 0.0931(2) 0.04395(16) 0.0776(2) 0.0297(5) Uani 1 d . . . C1 C 0.4919(4) 0.2489(3) 0.2583(4) 0.0624(11) Uani 1 d . . . H1A H 0.4461 0.3023 0.2262 0.094 Uiso 1 calc R . . H1B H 0.5217 0.2155 0.1980 0.094 Uiso 1 calc R . . H1C H 0.5624 0.2678 0.3152 0.094 Uiso 1 calc R . . C2 C 0.5010(4) 0.0952(3) 0.3913(4) 0.0633(12) Uani 1 d . . . H2A H 0.5648 0.1255 0.4457 0.095 Uiso 1 calc R . . H2B H 0.5395 0.0646 0.3340 0.095 Uiso 1 calc R . . H2C H 0.4580 0.0509 0.4309 0.095 Uiso 1 calc R . . C3 C 0.0656(5) 0.2837(3) 0.4319(4) 0.0688(12) Uani 1 d . . . H3A H -0.0106 0.2499 0.4337 0.103 Uiso 1 calc R . . H3B H 0.0547 0.3463 0.4544 0.103 Uiso 1 calc R . . H3C H 0.1338 0.2562 0.4844 0.103 Uiso 1 calc R . . C4 C -0.0425(5) 0.3264(3) 0.2120(5) 0.0796(15) Uani 1 d . . . H4A H -0.0518 0.3893 0.2343 0.119 Uiso 1 calc R . . H4B H -0.1120 0.2908 0.2292 0.119 Uiso 1 calc R . . H4C H -0.0413 0.3236 0.1307 0.119 Uiso 1 calc R . . C5 C -0.0049(3) 0.0900(2) 0.0186(3) 0.0321(6) Uani 1 d . . . H5 H -0.0108 0.1531 0.0301 0.039 Uiso 1 calc R . . C6 C -0.0974(3) 0.0469(2) -0.0586(3) 0.0328(6) Uani 1 d . . . H6 H -0.1639 0.0813 -0.0984 0.039 Uiso 1 calc R . . Cl4A Cl -0.1756(3) 0.10843(18) 0.3840(3) 0.1009(12) Uani 0.607(5) d P A 1 Cl5A Cl -0.2203(5) -0.0038(5) 0.1796(3) 0.132(2) Uani 0.607(5) d P A 1 Cl6A Cl -0.1336(4) -0.0833(2) 0.4007(3) 0.1092(12) Uani 0.607(5) d P A 1 C7A C -0.1250(19) 0.0101(16) 0.3171(13) 0.075(4) Uani 0.607(5) d P A 1 H7A H -0.0373 0.0190 0.3074 0.091 Uiso 0.607(5) calc PR A 1 Cl4B Cl -0.2312(5) 0.1262(4) 0.2235(7) 0.147(3) Uani 0.393(5) d P A 2 Cl5B Cl -0.1684(5) 0.0065(8) 0.4135(4) 0.171(5) Uani 0.393(5) d P A 2 Cl6B Cl -0.1898(9) -0.0559(5) 0.1837(7) 0.109(2) Uani 0.393(5) d P A 2 C7B C -0.143(3) 0.031(2) 0.2772(19) 0.070(6) Uani 0.393(5) d P A 2 H7B H -0.0535 0.0436 0.2792 0.085 Uiso 0.393(5) calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.03094(11) 0.02437(11) 0.02781(11) -0.00037(9) -0.00235(8) -0.00283(9) Cl1 0.0592(5) 0.0399(4) 0.0371(4) 0.0095(3) -0.0006(4) -0.0084(4) Cl2 0.0525(5) 0.0373(4) 0.0451(4) 0.0120(3) -0.0017(4) -0.0075(4) Cl3 0.0410(4) 0.0479(5) 0.0514(5) -0.0093(4) 0.0057(4) 0.0038(4) S1 0.0373(4) 0.0342(4) 0.0377(4) -0.0042(3) -0.0066(3) -0.0071(3) S2 0.0529(5) 0.0346(4) 0.0490(5) -0.0058(4) 0.0083(4) -0.0001(4) O1 0.0550(15) 0.0576(16) 0.0481(14) -0.0201(13) -0.0043(12) -0.0064(13) O2 0.0382(12) 0.0333(11) 0.0489(13) -0.0107(10) 0.0066(10) -0.0027(9) N1 0.0324(12) 0.0255(11) 0.0281(11) -0.0011(9) -0.0032(9) -0.0015(9) C1 0.053(2) 0.066(3) 0.065(3) 0.000(2) -0.0005(19) -0.027(2) C2 0.054(2) 0.057(2) 0.065(3) -0.005(2) -0.0292(19) 0.0029(19) C3 0.095(4) 0.060(3) 0.057(2) -0.011(2) 0.027(2) -0.004(3) C4 0.085(3) 0.060(3) 0.086(3) -0.008(3) -0.009(3) 0.031(3) C5 0.0357(14) 0.0230(13) 0.0344(14) -0.0026(11) -0.0028(12) 0.0001(11) C6 0.0333(14) 0.0255(13) 0.0356(15) -0.0007(11) -0.0046(12) 0.0014(11) Cl4A 0.0811(16) 0.0695(16) 0.163(3) -0.0223(17) 0.0518(18) -0.0066(12) Cl5A 0.107(3) 0.231(7) 0.0582(16) 0.012(3) 0.0108(17) -0.055(4) Cl6A 0.151(3) 0.0844(19) 0.0894(18) 0.0037(14) 0.0127(18) 0.0165(18) C7A 0.053(7) 0.110(12) 0.068(9) -0.006(8) 0.022(7) 0.002(7) Cl4B 0.098(3) 0.102(4) 0.258(9) 0.023(4) 0.074(4) 0.017(3) Cl5B 0.100(3) 0.352(17) 0.061(2) 0.007(5) 0.018(2) 0.026(6) Cl6B 0.117(5) 0.114(4) 0.109(4) -0.008(4) 0.054(4) -0.014(4) C7B 0.051(10) 0.098(17) 0.065(14) -0.009(11) 0.015(10) 0.004(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 O2 2.081(2) . ? Ru N1 2.109(2) . ? Ru S1 2.2774(8) . ? Ru Cl3 2.3223(10) . ? Ru Cl1 2.3264(9) . ? Ru Cl2 2.3467(9) . ? S1 O1 1.474(3) . ? S1 C1 1.766(4) . ? S1 C2 1.767(4) . ? S2 O2 1.555(2) . ? S2 C4 1.774(5) . ? S2 C3 1.782(4) . ? N1 C5 1.337(4) . ? N1 C6 1.340(4) 3 ? C5 C6 1.376(4) . ? C6 N1 1.340(4) 3 ? Cl4A C7A 1.76(2) . ? Cl5A C7A 1.770(17) . ? Cl6A C7A 1.688(18) . ? Cl4B C7B 1.73(3) . ? Cl5B C7B 1.71(2) . ? Cl6B C7B 1.69(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 O2 Ru N1 86.08(9) . . ? O2 Ru S1 94.23(7) . . ? N1 Ru S1 177.70(7) . . ? O2 Ru Cl3 175.72(7) . . ? N1 Ru Cl3 89.80(7) . . ? S1 Ru Cl3 89.93(4) . . ? O2 Ru Cl1 87.79(7) . . ? N1 Ru Cl1 87.66(7) . . ? S1 Ru Cl1 90.07(3) . . ? Cl3 Ru Cl1 93.22(4) . . ? O2 Ru Cl2 87.78(7) . . ? N1 Ru Cl2 89.52(7) . . ? S1 Ru Cl2 92.77(3) . . ? Cl3 Ru Cl2 91.02(4) . . ? Cl1 Ru Cl2 174.90(4) . . ? O1 S1 C1 107.3(2) . . ? O1 S1 C2 107.0(2) . . ? C1 S1 C2 100.6(2) . . ? O1 S1 Ru 116.13(11) . . ? C1 S1 Ru 113.04(14) . . ? C2 S1 Ru 111.48(13) . . ? O2 S2 C4 102.2(2) . . ? O2 S2 C3 104.16(18) . . ? C4 S2 C3 99.6(3) . . ? S2 O2 Ru 121.56(13) . . ? C5 N1 C6 117.0(2) . 3 ? C5 N1 Ru 121.86(19) . . ? C6 N1 Ru 121.15(19) 3 . ? N1 C5 C6 121.9(3) . . ? N1 C6 C5 121.1(3) 3 . ? Cl6A C7A Cl4A 109.8(9) . . ? Cl6A C7A Cl5A 111.0(14) . . ? Cl4A C7A Cl5A 109.0(10) . . ? Cl6B C7B Cl5B 112(2) . . ? Cl6B C7B Cl4B 106.1(12) . . ? Cl5B C7B Cl4B 110.0(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 O2 Ru S1 O1 8.67(15) . . . . ? N1 Ru S1 O1 -89.0(18) . . . . ? Cl3 Ru S1 O1 -172.33(14) . . . . ? Cl1 Ru S1 O1 -79.11(14) . . . . ? Cl2 Ru S1 O1 96.65(14) . . . . ? O2 Ru S1 C1 -116.0(2) . . . . ? N1 Ru S1 C1 146.3(18) . . . . ? Cl3 Ru S1 C1 62.99(19) . . . . ? Cl1 Ru S1 C1 156.21(19) . . . . ? Cl2 Ru S1 C1 -28.03(19) . . . . ? O2 Ru S1 C2 131.5(2) . . . . ? N1 Ru S1 C2 33.9(18) . . . . ? Cl3 Ru S1 C2 -49.46(19) . . . . ? Cl1 Ru S1 C2 43.76(19) . . . . ? Cl2 Ru S1 C2 -140.48(19) . . . . ? C4 S2 O2 Ru 128.9(2) . . . . ? C3 S2 O2 Ru -127.8(2) . . . . ? N1 Ru O2 S2 -140.36(17) . . . . ? S1 Ru O2 S2 41.92(16) . . . . ? Cl3 Ru O2 S2 -124.5(9) . . . . ? Cl1 Ru O2 S2 131.83(15) . . . . ? Cl2 Ru O2 S2 -50.69(15) . . . . ? O2 Ru N1 C5 45.7(2) . . . . ? S1 Ru N1 C5 143.6(17) . . . . ? Cl3 Ru N1 C5 -133.1(2) . . . . ? Cl1 Ru N1 C5 133.7(2) . . . . ? Cl2 Ru N1 C5 -42.1(2) . . . . ? O2 Ru N1 C6 -135.1(2) . . . 3 ? S1 Ru N1 C6 -37.3(19) . . . 3 ? Cl3 Ru N1 C6 46.0(2) . . . 3 ? Cl1 Ru N1 C6 -47.2(2) . . . 3 ? Cl2 Ru N1 C6 137.1(2) . . . 3 ? C6 N1 C5 C6 -0.3(5) 3 . . . ? Ru N1 C5 C6 178.8(2) . . . . ? N1 C5 C6 N1 0.3(5) . . . 3 ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 29.96 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.088 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.092 #===END