# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Eszter Nagy' _publ_contact_author_email neszma@hotmail.com _publ_section_title ; Promising Anticancer Mono- and Dinuclear Ruthenium(III) Dithiocarbamato Complexes: Systematic Solution Studies ; _publ_author_name E.Nagy # Attachment '- RuDTC.cif' #BEGIN data_fb10 _database_code_depnum_ccdc_archive 'CCDC 824317' #TrackingRef '- RuDTC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H18 N3 Ru S6' _chemical_formula_sum 'C9 H18 N3 Ru S6' _chemical_formula_weight 461.69 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' N N 0.0061 0.0033 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.255(1) _cell_length_b 17.542(2) _cell_length_c 20.379(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3666.0(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14994 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.51 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _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 'Bruker Smart 1000 CCD' _diffrn_measurement_method 'theta & omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 40740 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4215 _reflns_number_gt 2917 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Sir97 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4215 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0523 _refine_ls_wR_factor_gt 0.0486 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.003 _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 0.843299(19) 0.062394(11) 0.623578(10) 0.03900(7) Uani 1 1 d . . . S11 S 0.68599(6) 0.15754(4) 0.65303(3) 0.04586(17) Uani 1 1 d . . . S21 S 0.81523(7) 0.14295(4) 0.53035(3) 0.04809(17) Uani 1 1 d . . . S23 S 1.01829(6) 0.12871(4) 0.67471(3) 0.04595(17) Uani 1 1 d . . . S22 S 0.69229(7) -0.03050(4) 0.58412(4) 0.05390(19) Uani 1 1 d . . . S13 S 1.04015(6) 0.00509(4) 0.58544(4) 0.04911(17) Uani 1 1 d . . . S12 S 0.79641(8) -0.02152(4) 0.71283(4) 0.0613(2) Uani 1 1 d . . . N11 N 0.65108(19) 0.25937(12) 0.55603(10) 0.0455(5) Uani 1 1 d . . . C13 C 1.1231(2) 0.07017(13) 0.63276(11) 0.0379(6) Uani 1 1 d . . . C23 C 1.3137(3) 0.13661(18) 0.67285(14) 0.0670(9) Uani 1 1 d . . . H23A H 1.3423 0.1764 0.6439 0.101 Uiso 1 1 calc R . . H23B H 1.3874 0.1159 0.6958 0.101 Uiso 1 1 calc R . . H23C H 1.2526 0.1570 0.7039 0.101 Uiso 1 1 calc R . . N12 N 0.6157(3) -0.12697(14) 0.67927(15) 0.0745(8) Uani 1 1 d . . . C11 C 0.7088(2) 0.19612(13) 0.57629(11) 0.0392(6) Uani 1 1 d . . . C12 C 0.6911(2) -0.06774(14) 0.66125(15) 0.0549(7) Uani 1 1 d . . . C21 C 0.5628(3) 0.30223(15) 0.59815(14) 0.0572(7) Uani 1 1 d . . . H21A H 0.4747 0.2862 0.5901 0.086 Uiso 1 1 calc R . . H21B H 0.5709 0.3557 0.5888 0.086 Uiso 1 1 calc R . . H21C H 0.5846 0.2931 0.6433 0.086 Uiso 1 1 calc R . . C31 C 0.6760(3) 0.29011(17) 0.49056(13) 0.0661(8) Uani 1 1 d . . . H31A H 0.7628 0.2768 0.4771 0.099 Uiso 1 1 calc R . . H31B H 0.6674 0.3446 0.4915 0.099 Uiso 1 1 calc R . . H31C H 0.6142 0.2691 0.4601 0.099 Uiso 1 1 calc R . . N13 N 1.2510(2) 0.07656(13) 0.63481(9) 0.0472(6) Uani 1 1 d . . . C32 C 0.5290(3) -0.16485(19) 0.6323(2) 0.1013(13) Uani 1 1 d . . . H32A H 0.5314 -0.1382 0.5912 0.152 Uiso 1 1 calc R . . H32B H 0.4415 -0.1647 0.6491 0.152 Uiso 1 1 calc R . . H32C H 0.5574 -0.2165 0.6259 0.152 Uiso 1 1 calc R . . C22 C 0.6183(4) -0.1558(2) 0.74612(18) 0.1128(15) Uani 1 1 d . . . H22A H 0.6893 -0.1327 0.7695 0.169 Uiso 1 1 calc R . . H22B H 0.6296 -0.2101 0.7454 0.169 Uiso 1 1 calc R . . H22C H 0.5376 -0.1435 0.7676 0.169 Uiso 1 1 calc R . . C33 C 1.3366(3) 0.0237(2) 0.60003(16) 0.0771(10) Uani 1 1 d . . . H33A H 1.3896 -0.0033 0.6311 0.116 Uiso 1 1 calc R . . H33B H 1.3917 0.0516 0.5705 0.116 Uiso 1 1 calc R . . H33C H 1.2848 -0.0120 0.5756 0.116 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 0.03594(11) 0.03735(11) 0.04371(12) 0.00169(9) 0.00283(10) 0.00178(10) S11 0.0428(4) 0.0504(4) 0.0444(4) 0.0068(3) 0.0087(3) 0.0085(3) S21 0.0504(4) 0.0498(4) 0.0441(4) 0.0054(3) 0.0102(3) 0.0062(3) S23 0.0430(4) 0.0427(4) 0.0521(4) -0.0089(3) 0.0017(3) -0.0002(3) S22 0.0461(4) 0.0490(4) 0.0666(5) 0.0005(4) -0.0026(4) -0.0074(3) S13 0.0421(4) 0.0444(4) 0.0608(4) -0.0137(3) 0.0018(3) 0.0036(3) S12 0.0819(6) 0.0501(4) 0.0518(4) 0.0089(4) 0.0059(4) -0.0013(4) N11 0.0459(13) 0.0430(12) 0.0476(13) 0.0072(10) -0.0016(11) 0.0055(10) C13 0.0381(13) 0.0388(13) 0.0369(14) 0.0068(11) 0.0012(10) 0.0018(11) C23 0.0493(18) 0.091(2) 0.0608(19) 0.0052(17) -0.0113(15) -0.0201(17) N12 0.0751(19) 0.0474(16) 0.101(2) 0.0104(15) 0.0295(17) -0.0051(14) C11 0.0335(13) 0.0405(14) 0.0435(15) 0.0015(11) -0.0014(11) -0.0029(11) C12 0.0462(16) 0.0387(15) 0.080(2) 0.0034(14) 0.0172(14) 0.0041(13) C21 0.0514(17) 0.0477(16) 0.0724(19) -0.0021(15) -0.0041(15) 0.0137(14) C31 0.080(2) 0.063(2) 0.0555(18) 0.0178(15) -0.0045(16) 0.0086(17) N13 0.0356(11) 0.0614(16) 0.0447(13) 0.0032(11) -0.0021(10) 0.0017(10) C32 0.073(2) 0.055(2) 0.177(4) 0.000(2) 0.015(3) -0.0224(19) C22 0.140(4) 0.076(3) 0.122(3) 0.037(2) 0.052(3) -0.010(2) C33 0.0462(18) 0.105(3) 0.080(2) -0.006(2) 0.0057(16) 0.0234(18) _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 S23 2.3789(7) . ? Ru S13 2.3852(7) . ? Ru S21 2.3852(7) . ? Ru S22 2.3876(7) . ? Ru S12 2.3888(8) . ? Ru S11 2.3976(7) . ? S11 C11 1.720(2) . ? S21 C11 1.714(2) . ? S23 C13 1.714(2) . ? S22 C12 1.702(3) . ? S13 C13 1.719(2) . ? S12 C12 1.711(3) . ? N11 C11 1.324(3) . ? N11 C21 1.457(3) . ? N11 C31 1.462(3) . ? C13 N13 1.318(3) . ? C23 N13 1.457(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? N12 C12 1.346(3) . ? N12 C22 1.453(4) . ? N12 C32 1.465(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N13 C33 1.460(3) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? 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 S23 Ru S13 73.16(2) . . ? S23 Ru S21 98.64(3) . . ? S13 Ru S21 95.30(3) . . ? S23 Ru S22 166.06(3) . . ? S13 Ru S22 98.72(3) . . ? S21 Ru S22 93.31(3) . . ? S23 Ru S12 96.87(3) . . ? S13 Ru S12 99.14(3) . . ? S21 Ru S12 161.31(3) . . ? S22 Ru S12 72.86(3) . . ? S23 Ru S11 93.30(3) . . ? S13 Ru S11 160.80(2) . . ? S21 Ru S11 72.89(2) . . ? S22 Ru S11 97.07(3) . . ? S12 Ru S11 95.91(3) . . ? C11 S11 Ru 87.41(8) . . ? C11 S21 Ru 87.95(8) . . ? C13 S23 Ru 87.79(8) . . ? C12 S22 Ru 87.45(10) . . ? C13 S13 Ru 87.48(8) . . ? C12 S12 Ru 87.20(10) . . ? C11 N11 C21 121.8(2) . . ? C11 N11 C31 121.1(2) . . ? C21 N11 C31 117.1(2) . . ? N13 C13 S23 123.87(19) . . ? N13 C13 S13 124.53(19) . . ? S23 C13 S13 111.55(13) . . ? N13 C23 H23A 109.5 . . ? N13 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N13 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C12 N12 C22 120.9(3) . . ? C12 N12 C32 121.3(3) . . ? C22 N12 C32 117.8(3) . . ? N11 C11 S21 124.78(19) . . ? N11 C11 S11 123.56(19) . . ? S21 C11 S11 111.66(13) . . ? N12 C12 S22 123.5(2) . . ? N12 C12 S12 124.1(2) . . ? S22 C12 S12 112.39(15) . . ? N11 C21 H21A 109.5 . . ? N11 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N11 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N11 C31 H31A 109.5 . . ? N11 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N11 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C13 N13 C23 121.2(2) . . ? C13 N13 C33 121.9(2) . . ? C23 N13 C33 116.9(2) . . ? N12 C32 H32A 109.5 . . ? N12 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N12 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N12 C22 H22A 109.5 . . ? N12 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N12 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N13 C33 H33A 109.5 . . ? N13 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N13 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.310 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.060 #END #BEGIN data_fb23 _database_code_depnum_ccdc_archive 'CCDC 824318' #TrackingRef '- RuDTC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H24 N3 Ru S6, C H Cl3' _chemical_formula_sum 'C16 H25 Cl3 N3 Ru S6' _chemical_formula_weight 659.17 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' N N 0.0061 0.0033 '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 8.942(2) _cell_length_b 11.338(2) _cell_length_c 13.568(3) _cell_angle_alpha 85.612(3) _cell_angle_beta 83.206(3) _cell_angle_gamma 71.499(3) _cell_volume 1294.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9285 _cell_measurement_theta_min 1.51 _cell_measurement_theta_max 25.66 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 1.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _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 'Bruker Smart APEXII' _diffrn_measurement_method 'Theta & omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 14980 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.66 _reflns_number_total 4903 _reflns_number_gt 3600 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Sir97 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+0.0277P] 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 4903 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 0.34891(4) 0.32643(3) 0.22715(2) 0.04655(12) Uani 1 1 d . . . S21 S 0.52781(12) 0.13406(9) 0.16791(8) 0.0524(3) Uani 1 1 d . . . S13 S 0.40627(12) 0.29826(10) 0.39807(8) 0.0505(3) Uani 1 1 d . . . S11 S 0.20277(12) 0.18105(9) 0.24026(8) 0.0501(3) Uani 1 1 d . . . S12 S 0.12070(12) 0.50821(9) 0.23963(7) 0.0491(3) Uani 1 1 d . . . S22 S 0.30914(14) 0.40926(10) 0.06290(8) 0.0601(3) Uani 1 1 d . . . S23 S 0.55155(13) 0.41669(10) 0.23997(8) 0.0579(3) Uani 1 1 d . . . Cl3 Cl 0.73016(17) -0.02857(13) 0.52614(9) 0.0822(4) Uani 1 1 d . . . Cl2 Cl 0.86891(17) 0.05042(15) 0.34150(11) 0.0931(4) Uani 1 1 d . . . Cl1 Cl 0.7537(2) -0.16062(14) 0.35264(11) 0.1097(6) Uani 1 1 d . . . N12 N 0.0844(4) 0.6316(3) 0.0623(2) 0.0503(8) Uani 1 1 d . . . N11 N 0.3849(4) -0.0417(3) 0.1743(2) 0.0524(8) Uani 1 1 d . . . N13 N 0.6580(4) 0.3712(3) 0.4195(3) 0.0560(9) Uani 1 1 d . . . C1S C 0.7246(5) -0.0145(4) 0.3975(3) 0.0609(11) Uani 1 1 d . . . H1S H 0.6200 0.0404 0.3825 0.073 Uiso 1 1 calc R . . C23 C 0.6669(5) 0.3240(4) 0.5222(3) 0.0635(12) Uani 1 1 d . . . H23A H 0.6403 0.2471 0.5314 0.076 Uiso 1 1 calc R . . H23B H 0.5953 0.3844 0.5670 0.076 Uiso 1 1 calc R . . C12 C 0.1589(4) 0.5306(4) 0.1132(3) 0.0454(9) Uani 1 1 d . . . C11 C 0.3734(4) 0.0741(4) 0.1913(3) 0.0459(9) Uani 1 1 d . . . C13 C 0.5533(5) 0.3647(3) 0.3613(3) 0.0488(10) Uani 1 1 d . . . C52 C 0.1305(6) 0.6581(4) -0.0427(3) 0.0682(13) Uani 1 1 d . . . H52A H 0.0786 0.6232 -0.0864 0.082 Uiso 1 1 calc R . . H52B H 0.2443 0.6255 -0.0585 0.082 Uiso 1 1 calc R . . C32 C -0.0775(6) 0.8327(4) 0.0199(4) 0.0748(14) Uani 1 1 d . . . H32A H -0.1015 0.9163 0.0429 0.090 Uiso 1 1 calc R . . H32B H -0.1666 0.8275 -0.0119 0.090 Uiso 1 1 calc R . . C42 C 0.0740(6) 0.7983(4) -0.0507(3) 0.0704(13) Uani 1 1 d . . . H42A H 0.0525 0.8281 -0.1181 0.084 Uiso 1 1 calc R . . H42B H 0.1516 0.8324 -0.0302 0.084 Uiso 1 1 calc R . . C53 C 0.7946(6) 0.4151(5) 0.3827(4) 0.0783(15) Uani 1 1 d . . . H53A H 0.7602 0.5035 0.3653 0.094 Uiso 1 1 calc R . . H53B H 0.8537 0.3703 0.3250 0.094 Uiso 1 1 calc R . . C51 C 0.5331(5) -0.1345(4) 0.1361(3) 0.0589(11) Uani 1 1 d . . . H51A H 0.6241 -0.1219 0.1609 0.071 Uiso 1 1 calc R . . H51B H 0.5466 -0.1305 0.0641 0.071 Uiso 1 1 calc R . . C22 C -0.0402(5) 0.7367(4) 0.1053(3) 0.0593(11) Uani 1 1 d . . . H22A H -0.0039 0.7689 0.1589 0.071 Uiso 1 1 calc R . . H22B H -0.1330 0.7128 0.1308 0.071 Uiso 1 1 calc R . . C41 C 0.5124(6) -0.2566(4) 0.1750(4) 0.0858(16) Uani 1 1 d . . . H41A H 0.5723 -0.3233 0.1317 0.103 Uiso 1 1 calc R . . H41B H 0.5458 -0.2775 0.2413 0.103 Uiso 1 1 calc R . . C21 C 0.2587(5) -0.0987(4) 0.2035(4) 0.0651(12) Uani 1 1 d . . . H21A H 0.1677 -0.0606 0.1665 0.078 Uiso 1 1 calc R . . H21B H 0.2252 -0.0925 0.2740 0.078 Uiso 1 1 calc R . . C31 C 0.3420(6) -0.2344(4) 0.1759(5) 0.0914(18) Uani 1 1 d . . . H31A H 0.3077 -0.2905 0.2242 0.110 Uiso 1 1 calc R . . H31B H 0.3169 -0.2482 0.1110 0.110 Uiso 1 1 calc R . . C33 C 0.8367(7) 0.3023(6) 0.5403(5) 0.0983(19) Uani 1 1 d . . . H33A H 0.8436 0.3208 0.6079 0.118 Uiso 1 1 calc R . . H33B H 0.8995 0.2165 0.5289 0.118 Uiso 1 1 calc R . . C43 C 0.8923(7) 0.3873(6) 0.4690(5) 0.104(2) Uani 1 1 d . . . H43A H 1.0032 0.3491 0.4463 0.124 Uiso 1 1 calc R . . H43B H 0.8818 0.4638 0.5006 0.124 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 0.0486(2) 0.03853(19) 0.0500(2) -0.00039(14) 0.00026(15) -0.01211(15) S21 0.0481(6) 0.0410(6) 0.0663(7) -0.0041(5) 0.0019(5) -0.0134(5) S13 0.0510(6) 0.0508(6) 0.0526(6) 0.0034(5) -0.0027(5) -0.0220(5) S11 0.0435(6) 0.0454(6) 0.0608(7) -0.0032(5) -0.0051(5) -0.0128(5) S12 0.0529(6) 0.0442(6) 0.0446(6) -0.0001(4) 0.0025(5) -0.0104(5) S22 0.0702(7) 0.0518(7) 0.0461(6) -0.0053(5) 0.0040(5) -0.0048(5) S23 0.0615(7) 0.0536(6) 0.0624(7) 0.0050(5) 0.0017(5) -0.0276(5) Cl3 0.1106(11) 0.0859(9) 0.0568(7) -0.0045(6) -0.0074(7) -0.0402(8) Cl2 0.0777(9) 0.1061(11) 0.0934(10) 0.0140(8) 0.0063(7) -0.0350(8) Cl1 0.1784(17) 0.0867(10) 0.0745(10) -0.0147(8) -0.0216(10) -0.0504(11) N12 0.050(2) 0.050(2) 0.0441(19) 0.0029(15) 0.0007(15) -0.0081(16) N11 0.052(2) 0.042(2) 0.064(2) -0.0073(16) -0.0044(17) -0.0154(16) N13 0.052(2) 0.054(2) 0.068(2) -0.0040(18) -0.0075(18) -0.0242(17) C1S 0.060(3) 0.065(3) 0.057(3) 0.000(2) -0.006(2) -0.017(2) C23 0.064(3) 0.060(3) 0.066(3) -0.012(2) -0.008(2) -0.017(2) C12 0.045(2) 0.047(2) 0.044(2) -0.0061(18) -0.0020(18) -0.0151(18) C11 0.049(2) 0.043(2) 0.045(2) 0.0024(17) -0.0117(18) -0.0122(18) C13 0.047(2) 0.037(2) 0.060(3) -0.0044(18) 0.000(2) -0.0097(18) C52 0.066(3) 0.077(3) 0.052(3) 0.008(2) -0.003(2) -0.013(2) C32 0.076(3) 0.063(3) 0.077(3) 0.013(3) -0.013(3) -0.011(3) C42 0.070(3) 0.079(3) 0.065(3) 0.025(3) -0.020(3) -0.030(3) C53 0.065(3) 0.081(4) 0.103(4) -0.005(3) -0.007(3) -0.042(3) C51 0.062(3) 0.046(2) 0.065(3) -0.013(2) 0.007(2) -0.014(2) C22 0.051(3) 0.055(3) 0.064(3) 0.003(2) -0.005(2) -0.007(2) C41 0.090(4) 0.047(3) 0.114(5) -0.014(3) 0.014(3) -0.020(3) C21 0.053(3) 0.053(3) 0.095(4) -0.008(2) -0.011(2) -0.024(2) C31 0.085(4) 0.052(3) 0.151(6) 0.000(3) -0.035(4) -0.033(3) C33 0.077(4) 0.126(5) 0.099(4) -0.016(4) -0.025(3) -0.033(4) C43 0.079(4) 0.132(6) 0.120(5) -0.016(4) -0.023(4) -0.054(4) _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 S22 2.3729(12) . ? Ru S23 2.3748(12) . ? Ru S21 2.3900(11) . ? Ru S11 2.3924(11) . ? Ru S12 2.3964(11) . ? Ru S13 2.4098(12) . ? S21 C11 1.711(4) . ? S13 C13 1.722(4) . ? S11 C11 1.717(4) . ? S12 C12 1.724(4) . ? S22 C12 1.708(4) . ? S23 C13 1.705(4) . ? Cl3 C1S 1.746(4) . ? Cl2 C1S 1.752(4) . ? Cl1 C1S 1.740(5) . ? N12 C12 1.318(5) . ? N12 C22 1.453(5) . ? N12 C52 1.471(5) . ? N11 C11 1.321(5) . ? N11 C21 1.471(5) . ? N11 C51 1.473(5) . ? N13 C13 1.316(5) . ? N13 C23 1.457(5) . ? N13 C53 1.481(5) . ? C1S H1S 0.9800 . ? C23 C33 1.506(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C52 C42 1.506(6) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C32 C22 1.518(6) . ? C32 C42 1.523(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C53 C43 1.498(7) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C51 C41 1.502(6) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C41 C31 1.462(7) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C21 C31 1.536(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C33 C43 1.470(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S22 Ru S23 92.98(4) . . ? S22 Ru S21 91.78(4) . . ? S23 Ru S21 94.44(4) . . ? S22 Ru S11 100.68(4) . . ? S23 Ru S11 161.66(4) . . ? S21 Ru S11 73.13(4) . . ? S22 Ru S12 73.29(4) . . ? S23 Ru S12 100.14(4) . . ? S21 Ru S12 159.54(4) . . ? S11 Ru S12 95.51(4) . . ? S22 Ru S13 163.18(4) . . ? S23 Ru S13 73.00(4) . . ? S21 Ru S13 98.40(4) . . ? S11 Ru S13 95.09(4) . . ? S12 Ru S13 99.55(4) . . ? C11 S21 Ru 87.32(13) . . ? C13 S13 Ru 86.43(14) . . ? C11 S11 Ru 87.11(14) . . ? C12 S12 Ru 86.51(13) . . ? C12 S22 Ru 87.62(13) . . ? C13 S23 Ru 87.92(14) . . ? C12 N12 C22 124.3(3) . . ? C12 N12 C52 123.8(3) . . ? C22 N12 C52 111.5(3) . . ? C11 N11 C21 124.4(3) . . ? C11 N11 C51 123.7(3) . . ? C21 N11 C51 111.4(3) . . ? C13 N13 C23 125.6(3) . . ? C13 N13 C53 122.5(4) . . ? C23 N13 C53 111.5(4) . . ? Cl1 C1S Cl3 109.0(2) . . ? Cl1 C1S Cl2 111.0(2) . . ? Cl3 C1S Cl2 110.4(2) . . ? Cl1 C1S H1S 108.8 . . ? Cl3 C1S H1S 108.8 . . ? Cl2 C1S H1S 108.8 . . ? N13 C23 C33 104.4(4) . . ? N13 C23 H23A 110.9 . . ? C33 C23 H23A 110.9 . . ? N13 C23 H23B 110.9 . . ? C33 C23 H23B 110.9 . . ? H23A C23 H23B 108.9 . . ? N12 C12 S22 124.1(3) . . ? N12 C12 S12 123.8(3) . . ? S22 C12 S12 112.1(2) . . ? N11 C11 S21 123.7(3) . . ? N11 C11 S11 123.9(3) . . ? S21 C11 S11 112.4(2) . . ? N13 C13 S23 124.0(3) . . ? N13 C13 S13 123.7(3) . . ? S23 C13 S13 112.3(2) . . ? N12 C52 C42 102.7(4) . . ? N12 C52 H52A 111.2 . . ? C42 C52 H52A 111.2 . . ? N12 C52 H52B 111.2 . . ? C42 C52 H52B 111.2 . . ? H52A C52 H52B 109.1 . . ? C22 C32 C42 103.8(4) . . ? C22 C32 H32A 111.0 . . ? C42 C32 H32A 111.0 . . ? C22 C32 H32B 111.0 . . ? C42 C32 H32B 111.0 . . ? H32A C32 H32B 109.0 . . ? C52 C42 C32 103.3(4) . . ? C52 C42 H42A 111.1 . . ? C32 C42 H42A 111.1 . . ? C52 C42 H42B 111.1 . . ? C32 C42 H42B 111.1 . . ? H42A C42 H42B 109.1 . . ? N13 C53 C43 103.4(4) . . ? N13 C53 H53A 111.1 . . ? C43 C53 H53A 111.1 . . ? N13 C53 H53B 111.1 . . ? C43 C53 H53B 111.1 . . ? H53A C53 H53B 109.0 . . ? N11 C51 C41 103.7(3) . . ? N11 C51 H51A 111.0 . . ? C41 C51 H51A 111.0 . . ? N11 C51 H51B 111.0 . . ? C41 C51 H51B 111.0 . . ? H51A C51 H51B 109.0 . . ? N12 C22 C32 104.5(3) . . ? N12 C22 H22A 110.8 . . ? C32 C22 H22A 110.8 . . ? N12 C22 H22B 110.8 . . ? C32 C22 H22B 110.8 . . ? H22A C22 H22B 108.9 . . ? C31 C41 C51 103.4(4) . . ? C31 C41 H41A 111.1 . . ? C51 C41 H41A 111.1 . . ? C31 C41 H41B 111.1 . . ? C51 C41 H41B 111.1 . . ? H41A C41 H41B 109.1 . . ? N11 C21 C31 101.8(4) . . ? N11 C21 H21A 111.4 . . ? C31 C21 H21A 111.4 . . ? N11 C21 H21B 111.4 . . ? C31 C21 H21B 111.4 . . ? H21A C21 H21B 109.3 . . ? C41 C31 C21 107.2(4) . . ? C41 C31 H31A 110.3 . . ? C21 C31 H31A 110.3 . . ? C41 C31 H31B 110.3 . . ? C21 C31 H31B 110.3 . . ? H31A C31 H31B 108.5 . . ? C43 C33 C23 105.3(5) . . ? C43 C33 H33A 110.7 . . ? C23 C33 H33A 110.7 . . ? C43 C33 H33B 110.7 . . ? C23 C33 H33B 110.7 . . ? H33A C33 H33B 108.8 . . ? C33 C43 C53 108.7(4) . . ? C33 C43 H43A 110.0 . . ? C53 C43 H43A 110.0 . . ? C33 C43 H43B 110.0 . . ? C53 C43 H43B 110.0 . . ? H43A C43 H43B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.563 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.074 #END #BEGIN data_rul55as1 _database_code_depnum_ccdc_archive 'CCDC 824319' #TrackingRef '- RuDTC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 N3 O6 Ru S6' _chemical_formula_sum 'C18 H30 N3 O6 Ru S6' _chemical_formula_weight 677.88 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' N N 0.0061 0.0033 '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 Orthorhombic _symmetry_space_group_name_H-M Pcan loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 10.077(8) _cell_length_b 16.701(9) _cell_length_c 18.769(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3159(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 8.11 _cell_measurement_theta_max 12.83 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 0.926 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.940 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'local program based on Walker & Stuart' _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 'Philips PW 1100' _diffrn_measurement_method Theta-2-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3440 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0928 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.04 _reflns_number_total 3440 _reflns_number_gt 1576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'local program' _computing_cell_refinement 'local program' _computing_data_reduction 'local program' _computing_structure_solution Sir97 _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. The peripheral ethyl group of one dithiocarbamate moiety was found disordered in two positions that were refined with 0.6/0.4 site occupancy factors. The second dithiocarbamate moiety was found disodered in two positions that were refined with site occupancy factors of 0.5 each. Due to the poor quality of the crystals, the peripheral parts of the molecule were refined with isotropic thermal parameters. ; _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^)+(0.1161P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3440 _refine_ls_number_parameters 149 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1599 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.2330 _refine_ls_wR_factor_gt 0.1928 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.018 _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 0.17866(8) 0.0000 0.2500 0.0542(3) Uani 1 2 d S . . S1 S 0.3287(2) 0.07534(14) 0.18004(13) 0.0713(7) Uani 1 1 d . . . S2 S 0.2166(2) 0.12237(13) 0.31046(13) 0.0678(7) Uani 1 1 d . . . N11 N 0.3923(8) 0.2153(4) 0.2405(5) 0.080(2) Uani 1 1 d . . . C11 C 0.3232(7) 0.1475(5) 0.2421(5) 0.064(2) Uani 1 1 d . . . C21 C 0.3784(18) 0.2737(8) 0.2941(11) 0.185(8) Uani 1 1 d . . . H21A H 0.4361 0.3180 0.2841 0.277 Uiso 1 1 calc R . . H21B H 0.4015 0.2508 0.3394 0.277 Uiso 1 1 calc R . . H21C H 0.2882 0.2920 0.2955 0.277 Uiso 1 1 calc R . . C31 C 0.4769(10) 0.2342(6) 0.1843(7) 0.094(3) Uani 1 1 d . . . H31A H 0.5170 0.1858 0.1656 0.113 Uiso 1 1 calc R . . H31B H 0.5473 0.2691 0.2010 0.113 Uiso 1 1 calc R . . O11 O 0.2822(9) 0.2942(6) 0.1229(6) 0.138(4) Uani 1 1 d . . . C41 C 0.3979(17) 0.2765(9) 0.1251(8) 0.125(5) Uani 1 1 d . A . O21 O 0.4787(15) 0.2930(10) 0.0725(8) 0.212(6) Uiso 1 1 d D . . C51 C 0.428(2) 0.3394(18) 0.0066(12) 0.149(9) Uiso 0.60 1 d PD A 1 H51A H 0.3954 0.3028 -0.0294 0.179 Uiso 0.60 1 calc PR A 1 H51B H 0.3578 0.3760 0.0197 0.179 Uiso 0.60 1 calc PR A 1 C71 C 0.550(3) 0.3853(19) -0.0209(14) 0.228(16) Uiso 0.60 1 d PD A 1 H71A H 0.5256 0.4151 -0.0627 0.343 Uiso 0.60 1 calc PR A 1 H71B H 0.6190 0.3481 -0.0325 0.343 Uiso 0.60 1 calc PR A 1 H71C H 0.5803 0.4215 0.0152 0.343 Uiso 0.60 1 calc PR A 1 C61 C 0.406(6) 0.277(4) 0.005(2) 0.25(3) Uiso 0.40 1 d PD A 2 H61A H 0.3939 0.3271 -0.0204 0.296 Uiso 0.40 1 calc PR A 2 H61B H 0.3182 0.2565 0.0165 0.296 Uiso 0.40 1 calc PR A 2 C81 C 0.474(11) 0.218(7) -0.044(4) 0.51(8) Uiso 0.40 1 d PD A 2 H81A H 0.4292 0.2166 -0.0891 0.759 Uiso 0.40 1 calc PR A 2 H81B H 0.4722 0.1656 -0.0229 0.759 Uiso 0.40 1 calc PR A 2 H81C H 0.5647 0.2341 -0.0511 0.759 Uiso 0.40 1 calc PR A 2 S3 S -0.0109(2) 0.03268(15) 0.18107(15) 0.0758(7) Uani 1 1 d . B . C12 C -0.1034(9) 0.0000 0.2500 0.072(4) Uani 1 2 d S . . N12 N -0.2353(12) 0.0029(18) 0.2312(8) 0.071(6) Uani 0.50 1 d PD B -1 C22 C -0.302(3) 0.0239(17) 0.1628(12) 0.114(9) Uiso 0.50 1 d PD B -1 H22A H -0.3961 0.0199 0.1684 0.171 Uiso 0.50 1 calc PR B -1 H22B H -0.2730 -0.0123 0.1262 0.171 Uiso 0.50 1 calc PR B -1 H22C H -0.2786 0.0777 0.1496 0.171 Uiso 0.50 1 calc PR B -1 C32 C -0.317(2) -0.0250(13) 0.2978(13) 0.085(6) Uiso 0.50 1 d PD B -1 H32A H -0.2651 -0.0637 0.3246 0.102 Uiso 0.50 1 calc PR B -1 H32B H -0.3976 -0.0509 0.2821 0.102 Uiso 0.50 1 calc PR B -1 O12 O -0.354(4) 0.122(2) 0.3323(17) 0.265(15) Uiso 0.50 1 d PD B -1 O22 O -0.397(3) 0.0173(14) 0.4104(15) 0.203(10) Uiso 0.50 1 d PD B -1 C42 C -0.353(4) 0.0491(17) 0.3481(17) 0.169(13) Uiso 0.50 1 d PD B -1 C52 C -0.433(4) 0.078(3) 0.464(2) 0.34(3) Uiso 0.50 1 d PD B -1 H52A H -0.4189 0.1309 0.4442 0.410 Uiso 0.50 1 calc PR B -1 H52B H -0.3737 0.0725 0.5048 0.410 Uiso 0.50 1 calc PR B -1 C62 C -0.574(4) 0.072(3) 0.490(2) 0.26(2) Uiso 0.50 1 d PD B -1 H62A H -0.5908 0.1145 0.5238 0.385 Uiso 0.50 1 calc PR B -1 H62B H -0.5873 0.0215 0.5129 0.385 Uiso 0.50 1 calc PR B -1 H62C H -0.6333 0.0774 0.4505 0.385 Uiso 0.50 1 calc PR B -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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0358(4) 0.0491(5) 0.0778(7) 0.0004(5) 0.000 0.000 S1 0.0549(13) 0.0683(14) 0.0908(16) 0.0059(13) 0.0142(13) -0.0031(11) S2 0.0556(13) 0.0561(12) 0.0918(16) -0.0067(12) 0.0085(12) -0.0059(10) N11 0.069(5) 0.055(4) 0.115(7) 0.014(5) 0.013(5) -0.015(4) C11 0.040(4) 0.061(5) 0.091(6) 0.002(5) 0.010(5) 0.000(4) C21 0.173(13) 0.097(10) 0.284(19) -0.091(12) 0.128(15) -0.085(10) C31 0.065(6) 0.067(6) 0.150(10) 0.022(7) 0.008(8) -0.011(5) O11 0.083(6) 0.146(8) 0.186(10) 0.026(7) 0.002(7) 0.006(6) C41 0.113(11) 0.125(11) 0.136(12) -0.006(9) 0.065(11) -0.011(9) S3 0.0498(12) 0.0714(14) 0.1062(19) -0.0009(14) -0.0166(13) 0.0135(11) C12 0.024(5) 0.047(6) 0.146(11) -0.007(8) 0.000 0.000 N12 0.036(5) 0.096(10) 0.080(18) 0.052(16) -0.014(7) -0.022(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 S1 2.365(2) . ? Ru S1 2.365(2) 3 ? Ru S2 2.369(2) . ? Ru S2 2.369(2) 3 ? Ru S3 2.371(3) 3 ? Ru S3 2.371(3) . ? S1 C11 1.677(9) . ? S2 C11 1.726(8) . ? N11 C11 1.329(11) . ? N11 C31 1.393(12) . ? N11 C21 1.409(15) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C31 C41 1.54(2) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? O11 C41 1.203(16) . ? C41 O21 1.309(15) . ? O21 C61 1.490(19) . ? O21 C51 1.543(16) . ? C51 C71 1.533(18) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C61 C81 1.51(2) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? S3 C12 1.685(6) . ? C12 N12 1.376(15) 3 ? C12 N12 1.376(15) . ? C12 S3 1.685(6) 3 ? N12 C22 1.490(17) . ? N12 C32 1.56(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C32 C42 1.599(18) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? O12 C42 1.262(18) . ? O22 C42 1.36(3) . ? O22 C52 1.478(19) . ? C52 C62 1.50(2) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ru S1 100.51(13) . 3 ? S1 Ru S2 72.78(9) . . ? S1 Ru S2 95.16(9) 3 . ? S1 Ru S2 95.16(9) . 3 ? S1 Ru S2 72.78(9) 3 3 ? S2 Ru S2 161.44(12) . 3 ? S1 Ru S3 160.15(9) . 3 ? S1 Ru S3 95.15(10) 3 3 ? S2 Ru S3 93.85(9) . 3 ? S2 Ru S3 101.11(9) 3 3 ? S1 Ru S3 95.15(10) . . ? S1 Ru S3 160.15(9) 3 . ? S2 Ru S3 101.11(9) . . ? S2 Ru S3 93.85(9) 3 . ? S3 Ru S3 72.63(15) 3 . ? C11 S1 Ru 88.6(3) . . ? C11 S2 Ru 87.4(3) . . ? C11 N11 C31 122.1(9) . . ? C11 N11 C21 121.4(9) . . ? C31 N11 C21 116.4(8) . . ? N11 C11 S1 125.3(7) . . ? N11 C11 S2 123.4(7) . . ? S1 C11 S2 111.2(5) . . ? N11 C21 H21A 109.5 . . ? N11 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N11 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N11 C31 C41 109.5(9) . . ? N11 C31 H31A 109.8 . . ? C41 C31 H31A 109.8 . . ? N11 C31 H31B 109.8 . . ? C41 C31 H31B 109.8 . . ? H31A C31 H31B 108.2 . . ? O11 C41 O21 121.6(18) . . ? O11 C41 C31 129.7(13) . . ? O21 C41 C31 108.6(14) . . ? C41 O21 C61 107(3) . . ? C41 O21 C51 120.4(17) . . ? C61 O21 C51 41(2) . . ? C71 C51 O21 105.0(14) . . ? C71 C51 H51A 110.7 . . ? O21 C51 H51A 110.7 . . ? C71 C51 H51B 110.7 . . ? O21 C51 H51B 110.7 . . ? H51A C51 H51B 108.8 . . ? C51 C71 H71A 109.5 . . ? C51 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C51 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? O21 C61 C81 114(2) . . ? O21 C61 H61A 108.7 . . ? C81 C61 H61A 108.7 . . ? O21 C61 H61B 108.7 . . ? C81 C61 H61B 108.7 . . ? H61A C61 H61B 107.6 . . ? C61 C81 H81A 109.5 . . ? C61 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C61 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C12 S3 Ru 87.3(3) . . ? N12 C12 N12 30.0(12) 3 . ? N12 C12 S3 137.9(6) 3 . ? N12 C12 S3 109.0(5) . . ? N12 C12 S3 109.0(5) 3 3 ? N12 C12 S3 137.9(6) . 3 ? S3 C12 S3 112.9(6) . 3 ? C12 N12 C22 131.5(14) . . ? C12 N12 C32 106.9(12) . . ? C22 N12 C32 121.5(16) . . ? N12 C22 H22A 109.5 . . ? N12 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N12 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N12 C32 C42 111(2) . . ? N12 C32 H32A 109.4 . . ? C42 C32 H32A 109.4 . . ? N12 C32 H32B 109.4 . . ? C42 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C42 O22 C52 114(2) . . ? O12 C42 O22 125(2) . . ? O12 C42 C32 128(3) . . ? O22 C42 C32 106(3) . . ? O22 C52 C62 114(2) . . ? O22 C52 H52A 108.8 . . ? C62 C52 H52A 108.8 . . ? O22 C52 H52B 108.8 . . ? C62 C52 H52B 108.8 . . ? H52A C52 H52B 107.7 . . ? C52 C62 H62A 109.5 . . ? C52 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C52 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.04 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.741 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.104 #END