Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global loop_ _publ_author_name 'Clegg, W.' 'Elsegood, Mark' 'Gummerson, Sarah L.' 'Houlton, Andrew' 'Price, Clayton' 'Shipman, Michelle A.' _journal_coden_Cambridge 186 _publ_contact_author_name W.Clegg _publ_contact_author_email W.Clegg@ncl.ac.uk data_ah20 _database_code_CSD 154228 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H25 Cl2 N7 O4 Ru S' _chemical_formula_weight 523.41 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.4932(10) _cell_length_b 11.5769(8) _cell_length_c 19.8969(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3799.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 13990 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 28.41 _exptl_crystal_description 'long block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 1.250 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.679 _exptl_absorpt_correction_T_max 0.831 _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22124 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.58 _reflns_number_total 4535 _reflns_number_gt 3951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0277P)^2^+7.3347P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and some NH2 and H2O H-coords refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00063(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4535 _refine_ls_number_parameters 256 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.087034(14) 0.151962(19) 0.130027(11) 0.01701(8) Uani 1 d . . . Cl1 Cl 0.22369(5) 0.18697(7) 0.16786(4) 0.03012(18) Uani 1 d . . . Cl2 Cl -0.04392(4) 0.09819(6) 0.08263(4) 0.02244(16) Uani 1 d . . . N1 N 0.09666(16) 0.6496(2) -0.01921(14) 0.0246(6) Uani 1 d . . . H1 H 0.0892 0.7236 -0.0274 0.030 Uiso 1 calc R . . C2 C 0.13409(18) 0.5863(3) -0.06798(15) 0.0224(6) Uani 1 d . . . N2 N 0.1597(2) 0.6438(3) -0.12242(16) 0.0337(7) Uani 1 d . . . H2A H 0.179(3) 0.605(4) -0.152(2) 0.040 Uiso 1 d . . . H2B H 0.163(3) 0.716(4) -0.120(2) 0.040 Uiso 1 d . . . N3 N 0.14675(15) 0.4736(2) -0.06305(12) 0.0206(5) Uani 1 d . . . C4 C 0.12083(17) 0.4301(2) -0.00344(14) 0.0175(6) Uani 1 d . . . C5 C 0.08822(18) 0.4886(2) 0.04942(14) 0.0188(6) Uani 1 d . . . C6 C 0.06892(18) 0.6075(3) 0.04285(16) 0.0228(6) Uani 1 d . . . O6 O 0.03257(15) 0.67042(18) 0.08229(12) 0.0309(5) Uani 1 d . . . N7 N 0.07125(15) 0.40769(19) 0.09901(12) 0.0183(5) Uani 1 d . . . H7 H 0.0498 0.4244 0.1383 0.022 Uiso 1 calc R . . C8 C 0.09194(17) 0.3002(2) 0.07914(14) 0.0172(5) Uani 1 d . . . N9 N 0.12311(15) 0.31478(19) 0.01480(12) 0.0182(5) Uani 1 d . . . C10 C 0.1431(2) 0.2217(3) -0.03196(15) 0.0253(7) Uani 1 d . . . H10A H 0.1770 0.2535 -0.0686 0.030 Uiso 1 calc R . . H10B H 0.0924 0.1923 -0.0523 0.030 Uiso 1 calc R . . C11 C 0.1873(2) 0.1227(3) -0.00011(16) 0.0257(7) Uani 1 d . . . H11A H 0.2071 0.0698 -0.0356 0.031 Uiso 1 calc R . . H11B H 0.2351 0.1524 0.0246 0.031 Uiso 1 calc R . . N12 N 0.13517(15) 0.0590(2) 0.04610(12) 0.0200(5) Uani 1 d . . . H12 H 0.0905 0.0361 0.0209 0.024 Uiso 1 calc R . . C13 C 0.1722(2) -0.0488(3) 0.07165(17) 0.0280(7) Uani 1 d . . . H13A H 0.2245 -0.0314 0.0939 0.034 Uiso 1 calc R . . H13B H 0.1829 -0.1024 0.0339 0.034 Uiso 1 calc R . . C14 C 0.1152(2) -0.1038(3) 0.12078(18) 0.0310(7) Uani 1 d . . . H14A H 0.0648 -0.1272 0.0976 0.037 Uiso 1 calc R . . H14B H 0.1405 -0.1737 0.1403 0.037 Uiso 1 calc R . . N15 N 0.09625(18) -0.0204(2) 0.17470(15) 0.0260(6) Uani 1 d . . . H15A H 0.055(2) -0.045(3) 0.1958(19) 0.031 Uiso 1 d . . . H15B H 0.138(2) -0.018(3) 0.2043(18) 0.031 Uiso 1 d . . . S1 S 0.03572(5) 0.23042(7) 0.22216(4) 0.02392(17) Uani 1 d . . . O1 O 0.02233(19) 0.3583(2) 0.22779(12) 0.0445(7) Uani 1 d . . . C16 C 0.0934(2) 0.1937(5) 0.29512(17) 0.0512(12) Uani 1 d . . . H16A H 0.1480 0.2266 0.2913 0.077 Uiso 1 calc R . . H16B H 0.0973 0.1095 0.2989 0.077 Uiso 1 calc R . . H16C H 0.0667 0.2249 0.3352 0.077 Uiso 1 calc R . . C17 C -0.0582(2) 0.1657(3) 0.24733(16) 0.0265(7) Uani 1 d . . . H17A H -0.0706 0.1881 0.2937 0.040 Uiso 1 calc R . . H17B H -0.0536 0.0815 0.2445 0.040 Uiso 1 calc R . . H17C H -0.1017 0.1923 0.2176 0.040 Uiso 1 calc R . . O1W O 0.2786(2) 0.3807(4) -0.1409(2) 0.0840(12) Uani 1 d . . . O2W O 0.2491(2) 0.5734(3) -0.24388(18) 0.0581(9) Uani 1 d D . . H2WB H 0.273(4) 0.527(5) -0.231(3) 0.087 Uiso 1 d D . . H2WA H 0.268(4) 0.619(4) -0.262(3) 0.087 Uiso 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02072(13) 0.01369(12) 0.01661(12) 0.00276(8) 0.00056(9) -0.00195(9) Cl1 0.0252(4) 0.0345(4) 0.0306(4) 0.0034(3) -0.0035(3) -0.0099(3) Cl2 0.0226(4) 0.0201(3) 0.0246(3) 0.0015(3) -0.0014(3) -0.0001(3) N1 0.0307(14) 0.0123(11) 0.0309(14) 0.0048(10) -0.0080(11) -0.0022(10) C2 0.0236(15) 0.0213(14) 0.0223(14) 0.0056(12) -0.0074(12) -0.0073(12) N2 0.0428(18) 0.0272(15) 0.0313(16) 0.0163(13) -0.0052(14) -0.0080(14) N3 0.0241(13) 0.0192(12) 0.0184(12) 0.0051(10) 0.0001(10) -0.0014(10) C4 0.0188(14) 0.0137(13) 0.0200(14) 0.0030(10) -0.0010(11) -0.0017(11) C5 0.0218(14) 0.0141(13) 0.0204(14) 0.0005(10) -0.0002(11) -0.0001(11) C6 0.0224(15) 0.0161(13) 0.0300(16) -0.0020(12) -0.0067(13) -0.0027(11) O6 0.0386(13) 0.0187(11) 0.0354(13) -0.0066(9) -0.0012(11) 0.0048(9) N7 0.0245(13) 0.0135(11) 0.0168(11) -0.0017(9) 0.0025(10) -0.0006(9) C8 0.0197(14) 0.0173(13) 0.0146(12) -0.0016(10) 0.0021(11) -0.0010(11) N9 0.0256(13) 0.0127(11) 0.0162(11) 0.0016(9) 0.0045(10) 0.0009(10) C10 0.0368(18) 0.0194(14) 0.0197(14) 0.0004(12) 0.0061(13) 0.0038(13) C11 0.0282(17) 0.0179(14) 0.0308(17) 0.0005(12) 0.0113(14) 0.0010(12) N12 0.0239(13) 0.0133(11) 0.0228(12) 0.0014(9) 0.0017(10) 0.0030(9) C13 0.0285(17) 0.0167(14) 0.0388(18) 0.0029(13) 0.0038(14) 0.0042(12) C14 0.0341(18) 0.0186(15) 0.0403(19) 0.0081(14) -0.0015(15) 0.0014(13) N15 0.0235(14) 0.0214(13) 0.0332(15) 0.0105(11) 0.0008(12) -0.0001(11) S1 0.0318(4) 0.0248(4) 0.0151(3) 0.0000(3) 0.0034(3) -0.0063(3) O1 0.081(2) 0.0242(12) 0.0285(13) -0.0073(10) 0.0248(14) -0.0118(13) C16 0.037(2) 0.102(4) 0.0153(16) 0.0045(19) -0.0011(15) -0.015(2) C17 0.0270(16) 0.0305(16) 0.0221(15) 0.0021(13) 0.0062(13) -0.0017(13) O1W 0.069(3) 0.084(3) 0.099(3) -0.008(2) 0.013(2) 0.002(2) O2W 0.068(2) 0.059(2) 0.0470(19) 0.0105(16) -0.0097(17) -0.0190(17) _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 C8 1.994(3) . ? Ru1 N12 2.139(2) . ? Ru1 N15 2.189(3) . ? Ru1 S1 2.2139(8) . ? Ru1 Cl1 2.4105(8) . ? Ru1 Cl2 2.4375(8) . ? N1 C2 1.364(4) . ? N1 C6 1.404(4) . ? C2 N3 1.325(4) . ? C2 N2 1.340(4) . ? N3 C4 1.358(4) . ? C4 C5 1.362(4) . ? C4 N9 1.384(3) . ? C5 N7 1.389(4) . ? C5 C6 1.419(4) . ? C6 O6 1.227(4) . ? N7 C8 1.349(4) . ? C8 N9 1.390(3) . ? N9 C10 1.462(4) . ? C10 C11 1.499(4) . ? C11 N12 1.459(4) . ? N12 C13 1.481(4) . ? C13 C14 1.498(5) . ? C14 N15 1.477(4) . ? S1 O1 1.501(3) . ? S1 C16 1.787(4) . ? S1 C17 1.792(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 Ru1 N12 91.23(10) . . ? C8 Ru1 N15 170.93(11) . . ? N12 Ru1 N15 80.38(10) . . ? C8 Ru1 S1 94.75(8) . . ? N12 Ru1 S1 174.00(7) . . ? N15 Ru1 S1 93.68(8) . . ? C8 Ru1 Cl1 88.62(8) . . ? N12 Ru1 Cl1 88.92(7) . . ? N15 Ru1 Cl1 87.79(8) . . ? S1 Ru1 Cl1 91.71(3) . . ? C8 Ru1 Cl2 93.40(8) . . ? N12 Ru1 Cl2 84.17(7) . . ? N15 Ru1 Cl2 89.19(8) . . ? S1 Ru1 Cl2 94.96(3) . . ? Cl1 Ru1 Cl2 172.84(3) . . ? C2 N1 C6 125.9(3) . . ? N3 C2 N2 120.0(3) . . ? N3 C2 N1 123.2(3) . . ? N2 C2 N1 116.8(3) . . ? C2 N3 C4 112.3(3) . . ? N3 C4 C5 127.9(3) . . ? N3 C4 N9 125.3(3) . . ? C5 C4 N9 106.8(2) . . ? C4 C5 N7 107.0(2) . . ? C4 C5 C6 120.0(3) . . ? N7 C5 C6 132.4(3) . . ? O6 C6 N1 121.0(3) . . ? O6 C6 C5 128.8(3) . . ? N1 C6 C5 110.2(3) . . ? C8 N7 C5 111.3(2) . . ? N7 C8 N9 104.6(2) . . ? N7 C8 Ru1 129.4(2) . . ? N9 C8 Ru1 125.9(2) . . ? C4 N9 C8 110.4(2) . . ? C4 N9 C10 123.4(2) . . ? C8 N9 C10 125.5(2) . . ? N9 C10 C11 113.9(3) . . ? N12 C11 C10 111.5(3) . . ? C11 N12 C13 113.5(2) . . ? C11 N12 Ru1 117.19(18) . . ? C13 N12 Ru1 108.03(18) . . ? N12 C13 C14 108.9(3) . . ? N15 C14 C13 109.2(3) . . ? C14 N15 Ru1 108.41(19) . . ? O1 S1 C16 104.6(2) . . ? O1 S1 C17 105.32(16) . . ? C16 S1 C17 97.68(17) . . ? O1 S1 Ru1 121.52(10) . . ? C16 S1 Ru1 111.81(15) . . ? C17 S1 Ru1 112.98(11) . . ? _diffrn_measured_fraction_theta_max 0.845 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 0.597 _refine_diff_density_min -0.842 _refine_diff_density_rms 0.092 data_ah40 _database_code_CSD 154229 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H17 Cl3 N5 O3 Ru S' _chemical_formula_weight 482.76 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 8.5032(7) _cell_length_b 24.3211(19) _cell_length_c 8.1957(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.942(2) _cell_angle_gamma 90.00 _cell_volume 1694.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 7355 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.51 _exptl_crystal_description lath _exptl_crystal_colour orange _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 1.539 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.474 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14609 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.64 _reflns_number_total 4060 _reflns_number_gt 2940 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0683P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except N&O-H coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4060 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.38362(4) 0.116706(14) 0.46421(4) 0.01694(13) Uani 1 1 d . . . Cl1 Cl 0.40435(16) 0.21169(5) 0.45749(16) 0.0384(3) Uani 1 1 d . . . Cl2 Cl 0.59104(17) 0.10727(9) 0.65149(16) 0.0631(5) Uani 1 1 d . . . Cl3 Cl 0.16115(13) 0.11854(5) 0.28491(14) 0.0310(3) Uani 1 1 d . . . O1 O 0.3678(5) 0.03300(15) 0.4534(5) 0.0508(13) Uani 1 1 d . . . H1A H 0.303(8) 0.015(2) 0.515(8) 0.061 Uiso 1 1 d . . . H1B H 0.424(8) 0.016(3) 0.414(8) 0.061 Uiso 1 1 d . . . S1 S 0.54086(12) 0.11033(4) 0.24865(13) 0.0195(2) Uani 1 1 d . . . O2 O 0.5378(4) 0.05441(13) 0.1775(4) 0.0279(7) Uani 1 1 d . . . C12 C 0.4916(7) 0.1567(2) 0.0871(6) 0.0404(14) Uani 1 1 d . . . H12A H 0.5545 0.1481 -0.0076 0.061 Uiso 1 1 calc R . . H12B H 0.5137 0.1944 0.1229 0.061 Uiso 1 1 calc R . . H12C H 0.3796 0.1531 0.0570 0.061 Uiso 1 1 calc R . . C13 C 0.7398(5) 0.12831(19) 0.2909(6) 0.0289(11) Uani 1 1 d . . . H13A H 0.7811 0.1066 0.3835 0.043 Uiso 1 1 calc R . . H13B H 0.7466 0.1675 0.3177 0.043 Uiso 1 1 calc R . . H13C H 0.8018 0.1207 0.1948 0.043 Uiso 1 1 calc R . . N1 N -0.0447(4) 0.00791(15) 0.7694(4) 0.0213(8) Uani 1 1 d . . . H1 H -0.069(5) -0.0246(19) 0.756(6) 0.026 Uiso 1 1 d . . . C2 C -0.1288(5) 0.03636(18) 0.8813(5) 0.0188(9) Uani 1 1 d . . . N2 N -0.2450(5) 0.00948(17) 0.9515(5) 0.0250(9) Uani 1 1 d . . . H2A H -0.291(6) 0.027(2) 1.017(6) 0.030 Uiso 1 1 d . . . H2B H -0.277(6) -0.015(2) 0.906(6) 0.030 Uiso 1 1 d . . . N3 N -0.0945(4) 0.08766(15) 0.9219(4) 0.0204(8) Uani 1 1 d . . . C4 C 0.0254(5) 0.10787(16) 0.8369(5) 0.0179(9) Uani 1 1 d . . . C5 C 0.1144(5) 0.08266(17) 0.7198(5) 0.0179(9) Uani 1 1 d . . . C6 C 0.0821(5) 0.02709(17) 0.6851(5) 0.0191(9) Uani 1 1 d . . . O6 O 0.1492(4) -0.00593(13) 0.5946(4) 0.0276(7) Uani 1 1 d . . . N7 N 0.2250(4) 0.11991(14) 0.6624(4) 0.0204(8) Uani 1 1 d . . . C8 C 0.2023(5) 0.16528(18) 0.7468(5) 0.0229(9) Uani 1 1 d . . . H8 H 0.2615 0.1980 0.7337 0.028 Uiso 1 1 calc R . . N9 N 0.0852(4) 0.16019(14) 0.8543(4) 0.0216(8) Uani 1 1 d . . . C10 C 0.0225(6) 0.20365(19) 0.9585(6) 0.0289(11) Uani 1 1 d . . . H10A H 0.1029 0.2327 0.9750 0.035 Uiso 1 1 calc R . . H10B H -0.0005 0.1880 1.0667 0.035 Uiso 1 1 calc R . . C11 C -0.1253(9) 0.2285(3) 0.8835(8) 0.066(2) Uani 1 1 d . . . H11A H -0.1004 0.2474 0.7820 0.100 Uiso 1 1 calc R . . H11B H -0.1692 0.2549 0.9600 0.100 Uiso 1 1 calc R . . H11C H -0.2023 0.1994 0.8599 0.100 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01190(19) 0.0228(2) 0.01614(19) 0.00200(14) 0.00086(12) 0.00440(14) Cl1 0.0470(8) 0.0240(6) 0.0456(8) -0.0093(5) 0.0229(6) -0.0115(5) Cl2 0.0265(7) 0.1406(17) 0.0217(7) -0.0019(8) -0.0072(5) 0.0320(9) Cl3 0.0185(6) 0.0442(7) 0.0297(6) -0.0005(5) -0.0065(5) -0.0015(5) O1 0.069(3) 0.0208(19) 0.066(3) 0.0115(18) 0.051(2) 0.0141(18) S1 0.0160(5) 0.0232(6) 0.0195(5) 0.0002(4) 0.0034(4) -0.0004(4) O2 0.0237(17) 0.0296(18) 0.0308(18) -0.0089(14) 0.0069(14) -0.0085(14) C12 0.043(3) 0.049(3) 0.030(3) 0.018(2) 0.006(2) 0.011(3) C13 0.014(2) 0.033(3) 0.040(3) -0.010(2) 0.005(2) -0.0053(18) N1 0.0170(19) 0.0233(19) 0.023(2) -0.0034(16) -0.0014(15) -0.0001(15) C2 0.015(2) 0.026(2) 0.015(2) -0.0009(17) -0.0045(16) 0.0029(17) N2 0.024(2) 0.026(2) 0.025(2) -0.0057(17) 0.0042(17) -0.0048(17) N3 0.0151(18) 0.027(2) 0.0193(19) 0.0017(15) 0.0007(15) 0.0006(15) C4 0.018(2) 0.022(2) 0.0135(19) 0.0009(16) -0.0012(16) 0.0028(17) C5 0.013(2) 0.027(2) 0.014(2) 0.0000(17) -0.0019(16) 0.0042(17) C6 0.014(2) 0.026(2) 0.017(2) -0.0016(17) -0.0043(17) 0.0055(17) O6 0.0186(17) 0.0313(18) 0.0331(18) -0.0102(15) 0.0065(14) 0.0024(13) N7 0.0188(19) 0.0249(19) 0.0177(18) 0.0034(15) 0.0038(14) 0.0050(15) C8 0.018(2) 0.027(2) 0.024(2) 0.0006(18) 0.0030(18) 0.0023(18) N9 0.025(2) 0.0214(19) 0.0191(19) -0.0018(14) 0.0062(15) 0.0016(15) C10 0.030(3) 0.026(2) 0.031(3) -0.008(2) 0.011(2) -0.003(2) C11 0.098(6) 0.056(4) 0.047(4) 0.009(3) 0.023(4) 0.055(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 Ru1 O1 2.042(4) . ? Ru1 N7 2.148(3) . ? Ru1 S1 2.2567(11) . ? Ru1 Cl2 2.3100(14) . ? Ru1 Cl1 2.3175(12) . ? Ru1 Cl3 2.3562(12) . ? S1 O2 1.480(3) . ? S1 C13 1.770(4) . ? S1 C12 1.778(5) . ? N1 C2 1.369(5) . ? N1 C6 1.381(5) . ? C2 N3 1.321(5) . ? C2 N2 1.332(6) . ? N3 C4 1.347(5) . ? C4 N9 1.376(5) . ? C4 C5 1.385(6) . ? C5 N7 1.399(5) . ? C5 C6 1.406(6) . ? C6 O6 1.245(5) . ? N7 C8 1.320(5) . ? C8 N9 1.357(5) . ? N9 C10 1.470(5) . ? C10 C11 1.507(8) . ? 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 O1 Ru1 N7 91.54(14) . . ? O1 Ru1 S1 86.41(10) . . ? N7 Ru1 S1 176.89(10) . . ? O1 Ru1 Cl2 88.70(15) . . ? N7 Ru1 Cl2 89.19(10) . . ? S1 Ru1 Cl2 93.10(5) . . ? O1 Ru1 Cl1 176.09(12) . . ? N7 Ru1 Cl1 91.83(10) . . ? S1 Ru1 Cl1 90.13(4) . . ? Cl2 Ru1 Cl1 93.31(7) . . ? O1 Ru1 Cl3 86.66(15) . . ? N7 Ru1 Cl3 87.69(10) . . ? S1 Ru1 Cl3 89.86(4) . . ? Cl2 Ru1 Cl3 174.33(6) . . ? Cl1 Ru1 Cl3 91.51(5) . . ? O2 S1 C13 107.9(2) . . ? O2 S1 C12 106.8(2) . . ? C13 S1 C12 100.9(3) . . ? O2 S1 Ru1 111.63(13) . . ? C13 S1 Ru1 114.68(17) . . ? C12 S1 Ru1 114.11(18) . . ? C2 N1 C6 126.8(4) . . ? N3 C2 N2 121.0(4) . . ? N3 C2 N1 122.0(4) . . ? N2 C2 N1 117.0(4) . . ? C2 N3 C4 112.3(4) . . ? N3 C4 N9 124.6(4) . . ? N3 C4 C5 129.6(4) . . ? N9 C4 C5 105.8(4) . . ? C4 C5 N7 109.6(4) . . ? C4 C5 C6 117.3(4) . . ? N7 C5 C6 133.1(4) . . ? O6 C6 N1 117.5(4) . . ? O6 C6 C5 130.6(4) . . ? N1 C6 C5 111.9(4) . . ? C8 N7 C5 104.7(3) . . ? C8 N7 Ru1 122.2(3) . . ? C5 N7 Ru1 132.6(3) . . ? N7 C8 N9 112.8(4) . . ? C8 N9 C4 107.1(4) . . ? C8 N9 C10 126.9(4) . . ? C4 N9 C10 125.8(4) . . ? N9 C10 C11 111.4(4) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.360 _refine_diff_density_min -1.428 _refine_diff_density_rms 0.161