# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Iztok Turel' _publ_contact_author_name 'Iztok Turel' _publ_contact_author_email iztok.turel@fkkt.uni-lj.si data_1 _database_code_depnum_ccdc_archive 'CCDC 805600' #TrackingRef '- data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H24 Cl2 N4 O2 Ru S2' _chemical_formula_sum 'C18 H24 Cl2 N4 O2 Ru S2' _chemical_formula_weight 564.50 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.411(3) _cell_length_b 10.009(4) _cell_length_c 13.997(4) _cell_angle_alpha 104.37(3) _cell_angle_beta 96.23(2) _cell_angle_gamma 94.18(2) _cell_volume 1128.6(7) _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 needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7565 _exptl_absorpt_correction_T_max 0.8255 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Quadratic fit to sin(theta)/lambda - 18 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13115 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.08 _reflns_number_total 4678 _reflns_number_gt 2373 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^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 4678 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.839 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.34273(5) 0.31858(4) 0.20544(3) 0.05167(15) Uani 1 1 d . . . Cl2 Cl 0.21352(17) 0.39224(15) 0.35130(11) 0.0670(4) Uani 1 1 d . . . Cl1 Cl 0.47402(16) 0.24177(14) 0.05802(11) 0.0629(4) Uani 1 1 d . . . S1 S 0.54170(16) 0.49599(14) 0.26383(11) 0.0606(4) Uani 1 1 d . . . S2 S 0.19410(16) 0.44525(14) 0.12158(12) 0.0599(4) Uani 1 1 d . . . O1 O 0.5358(5) 0.6223(4) 0.2270(3) 0.0795(12) Uani 1 1 d . . . O2 O 0.0387(4) 0.3729(4) 0.0660(3) 0.0799(12) Uani 1 1 d . . . N1 N 0.1560(5) 0.1453(4) 0.1631(3) 0.0536(11) Uani 1 1 d . . . N2 N 0.4672(5) 0.1827(4) 0.2721(3) 0.0524(11) Uani 1 1 d . . . N3 N 0.4497(5) 0.0435(4) 0.2309(3) 0.0565(11) Uani 1 1 d . . . N4 N 0.5610(5) 0.2091(4) 0.3564(3) 0.0585(11) Uani 1 1 d . . . C1 C 0.0014(6) 0.1706(6) 0.1696(4) 0.0642(15) Uani 1 1 d . . . H1 H -0.0202 0.2614 0.1956 0.077 Uiso 1 1 calc R . . C2 C -0.1266(7) 0.0676(7) 0.1393(5) 0.0735(17) Uani 1 1 d . . . H2 H -0.2317 0.0887 0.1444 0.088 Uiso 1 1 calc R . . C3 C -0.0942(8) -0.0658(7) 0.1018(5) 0.0786(19) Uani 1 1 d . . . H3 H -0.1777 -0.1366 0.0784 0.094 Uiso 1 1 calc R . . C4 C 0.0633(7) -0.0945(6) 0.0991(4) 0.0692(16) Uani 1 1 d . . . H4 H 0.0870 -0.1850 0.0750 0.083 Uiso 1 1 calc R . . C5 C 0.1845(6) 0.0115(5) 0.1320(4) 0.0561(13) Uani 1 1 d . . . C6 C 0.3575(6) -0.0202(5) 0.1344(4) 0.0606(14) Uani 1 1 d . . . H6A H 0.3611 -0.1198 0.1190 0.073 Uiso 1 1 calc R . . H6B H 0.4056 0.0137 0.0838 0.073 Uiso 1 1 calc R . . C7 C 0.5383(6) -0.0171(6) 0.2922(4) 0.0632(15) Uani 1 1 d . . . H7 H 0.5496 -0.1111 0.2824 0.076 Uiso 1 1 calc R . . C8 C 0.6063(6) 0.0867(6) 0.3700(4) 0.0595(14) Uani 1 1 d . . . C9 C 0.7138(7) 0.0818(6) 0.4594(4) 0.0641(15) Uani 1 1 d . . . C10 C 0.7059(7) -0.0352(7) 0.4944(5) 0.0797(19) Uani 1 1 d . . . H10 H 0.6296 -0.1091 0.4621 0.096 Uiso 1 1 calc R . . C11 C 0.8080(9) -0.0464(9) 0.5763(6) 0.100(2) Uani 1 1 d . . . H11 H 0.7997 -0.1253 0.6000 0.120 Uiso 1 1 calc R . . C12 C 0.9200(10) 0.0614(11) 0.6203(6) 0.102(3) Uani 1 1 d . . . H12 H 0.9918 0.0541 0.6737 0.122 Uiso 1 1 calc R . . C13 C 0.9320(8) 0.1798(9) 0.5898(5) 0.097(2) Uani 1 1 d . . . H13 H 1.0091 0.2526 0.6230 0.117 Uiso 1 1 calc R . . C14 C 0.8278(7) 0.1916(7) 0.5083(5) 0.0836(19) Uani 1 1 d . . . H14 H 0.8348 0.2724 0.4869 0.100 Uiso 1 1 calc R . . C15 C 0.7337(6) 0.4394(6) 0.2475(5) 0.0783(18) Uani 1 1 d . . . H15A H 0.7419 0.4084 0.1778 0.117 Uiso 1 1 calc R . . H15B H 0.7484 0.3643 0.2779 0.117 Uiso 1 1 calc R . . H15C H 0.8152 0.5147 0.2780 0.117 Uiso 1 1 calc R . . C16 C 0.5687(8) 0.5564(6) 0.3955(4) 0.0840(19) Uani 1 1 d . . . H16A H 0.6659 0.6183 0.4169 0.126 Uiso 1 1 calc R . . H16B H 0.5760 0.4791 0.4242 0.126 Uiso 1 1 calc R . . H16C H 0.4789 0.6047 0.4165 0.126 Uiso 1 1 calc R . . C17 C 0.1499(8) 0.6020(6) 0.2000(5) 0.0812(18) Uani 1 1 d . . . H17A H 0.0727 0.6436 0.1639 0.122 Uiso 1 1 calc R . . H17B H 0.2465 0.6644 0.2221 0.122 Uiso 1 1 calc R . . H17C H 0.1064 0.5833 0.2565 0.122 Uiso 1 1 calc R . . C18 C 0.2898(7) 0.5120(6) 0.0345(5) 0.0749(17) Uani 1 1 d . . . H18A H 0.3186 0.4367 -0.0158 0.112 Uiso 1 1 calc R . . H18B H 0.3851 0.5711 0.0678 0.112 Uiso 1 1 calc R . . H18C H 0.2179 0.5643 0.0041 0.112 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 0.0573(3) 0.0445(3) 0.0559(3) 0.0163(2) 0.00863(19) 0.00967(18) Cl2 0.0805(9) 0.0630(9) 0.0611(10) 0.0154(7) 0.0223(7) 0.0128(7) Cl1 0.0704(8) 0.0613(9) 0.0617(9) 0.0180(7) 0.0190(7) 0.0161(7) S1 0.0658(8) 0.0509(8) 0.0656(10) 0.0181(7) 0.0063(7) 0.0026(6) S2 0.0617(8) 0.0518(8) 0.0723(10) 0.0261(7) 0.0078(7) 0.0129(6) O1 0.094(3) 0.056(2) 0.093(3) 0.037(2) 0.004(2) -0.007(2) O2 0.066(2) 0.075(3) 0.099(3) 0.037(2) -0.018(2) -0.001(2) N1 0.055(3) 0.052(3) 0.055(3) 0.016(2) 0.008(2) 0.010(2) N2 0.064(3) 0.044(3) 0.052(3) 0.016(2) 0.006(2) 0.013(2) N3 0.063(3) 0.046(3) 0.062(3) 0.016(2) 0.008(2) 0.011(2) N4 0.057(3) 0.060(3) 0.061(3) 0.019(2) 0.005(2) 0.013(2) C1 0.070(4) 0.064(4) 0.064(4) 0.021(3) 0.011(3) 0.014(3) C2 0.074(4) 0.075(4) 0.074(5) 0.032(4) 0.003(3) -0.007(3) C3 0.077(4) 0.081(5) 0.077(5) 0.033(4) -0.008(3) -0.014(4) C4 0.090(4) 0.052(4) 0.062(4) 0.020(3) -0.008(3) -0.005(3) C5 0.068(3) 0.047(3) 0.055(4) 0.017(3) 0.006(3) 0.007(3) C6 0.081(4) 0.041(3) 0.056(4) 0.006(3) 0.009(3) 0.006(3) C7 0.074(4) 0.048(3) 0.075(4) 0.025(3) 0.014(3) 0.018(3) C8 0.066(3) 0.054(3) 0.064(4) 0.022(3) 0.011(3) 0.017(3) C9 0.064(3) 0.074(4) 0.062(4) 0.026(3) 0.010(3) 0.021(3) C10 0.069(4) 0.098(5) 0.087(5) 0.045(4) 0.016(3) 0.023(3) C11 0.110(6) 0.131(7) 0.090(6) 0.064(5) 0.031(5) 0.061(5) C12 0.100(6) 0.151(8) 0.063(5) 0.025(6) 0.017(4) 0.062(6) C13 0.098(5) 0.108(6) 0.072(5) -0.001(5) -0.007(4) 0.027(4) C14 0.083(5) 0.083(5) 0.080(5) 0.010(4) 0.003(4) 0.023(4) C15 0.063(4) 0.080(4) 0.090(5) 0.019(4) 0.008(3) 0.005(3) C16 0.108(5) 0.067(4) 0.066(4) 0.006(3) 0.005(4) -0.013(3) C17 0.108(5) 0.060(4) 0.088(5) 0.028(3) 0.030(4) 0.036(3) C18 0.086(4) 0.077(4) 0.079(5) 0.045(4) 0.018(3) 0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N2 2.107(4) . ? Ru N1 2.172(4) . ? Ru S1 2.2740(16) . ? Ru S2 2.2802(15) . ? Ru Cl2 2.3967(16) . ? Ru Cl1 2.4289(16) . ? S1 O1 1.481(4) . ? S1 C15 1.770(6) . ? S1 C16 1.774(6) . ? S2 O2 1.483(4) . ? S2 C18 1.766(5) . ? S2 C17 1.768(6) . ? N1 C5 1.349(6) . ? N1 C1 1.351(6) . ? N2 N4 1.303(5) . ? N2 N3 1.360(5) . ? N3 C7 1.359(6) . ? N3 C6 1.451(6) . ? N4 C8 1.360(6) . ? C1 C2 1.387(7) . ? C2 C3 1.367(8) . ? C3 C4 1.378(8) . ? C4 C5 1.369(7) . ? C5 C6 1.510(7) . ? C7 C8 1.345(7) . ? C8 C9 1.476(7) . ? C9 C10 1.376(8) . ? C9 C14 1.388(8) . ? C10 C11 1.389(9) . ? C11 C12 1.352(10) . ? C12 C13 1.356(10) . ? C13 C14 1.396(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru N1 82.89(16) . . ? N2 Ru S1 93.20(12) . . ? N1 Ru S1 174.72(12) . . ? N2 Ru S2 173.94(13) . . ? N1 Ru S2 91.76(11) . . ? S1 Ru S2 92.31(6) . . ? N2 Ru Cl2 90.05(12) . . ? N1 Ru Cl2 85.26(12) . . ? S1 Ru Cl2 91.20(6) . . ? S2 Ru Cl2 92.35(6) . . ? N2 Ru Cl1 89.44(12) . . ? N1 Ru Cl1 94.43(12) . . ? S1 Ru Cl1 89.07(6) . . ? S2 Ru Cl1 88.13(6) . . ? Cl2 Ru Cl1 179.43(5) . . ? O1 S1 C15 106.4(3) . . ? O1 S1 C16 105.3(3) . . ? C15 S1 C16 98.8(3) . . ? O1 S1 Ru 119.57(17) . . ? C15 S1 Ru 111.6(2) . . ? C16 S1 Ru 112.9(2) . . ? O2 S2 C18 105.0(3) . . ? O2 S2 C17 106.6(3) . . ? C18 S2 C17 99.5(3) . . ? O2 S2 Ru 115.30(16) . . ? C18 S2 Ru 116.1(2) . . ? C17 S2 Ru 112.7(2) . . ? C5 N1 C1 117.0(4) . . ? C5 N1 Ru 124.0(3) . . ? C1 N1 Ru 119.0(4) . . ? N4 N2 N3 108.7(4) . . ? N4 N2 Ru 129.5(3) . . ? N3 N2 Ru 121.6(3) . . ? C7 N3 N2 108.3(4) . . ? C7 N3 C6 128.9(5) . . ? N2 N3 C6 122.7(4) . . ? N2 N4 C8 107.9(4) . . ? N1 C1 C2 123.1(6) . . ? C3 C2 C1 118.3(6) . . ? C2 C3 C4 119.4(6) . . ? C5 C4 C3 119.5(6) . . ? N1 C5 C4 122.5(5) . . ? N1 C5 C6 117.8(4) . . ? C4 C5 C6 119.7(5) . . ? N3 C6 C5 111.6(4) . . ? C8 C7 N3 105.9(5) . . ? C7 C8 N4 109.2(5) . . ? C7 C8 C9 129.7(5) . . ? N4 C8 C9 121.1(5) . . ? C10 C9 C14 118.4(6) . . ? C10 C9 C8 120.1(6) . . ? C14 C9 C8 121.4(6) . . ? C9 C10 C11 122.2(7) . . ? C12 C11 C10 117.6(7) . . ? C11 C12 C13 122.8(8) . . ? C12 C13 C14 119.5(7) . . ? C9 C14 C13 119.5(7) . . ? 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 N2 Ru S1 O1 170.2(2) . . . . ? N1 Ru S1 O1 -147.6(13) . . . . ? S2 Ru S1 O1 -7.3(2) . . . . ? Cl2 Ru S1 O1 -99.7(2) . . . . ? Cl1 Ru S1 O1 80.8(2) . . . . ? N2 Ru S1 C15 45.0(3) . . . . ? N1 Ru S1 C15 87.2(13) . . . . ? S2 Ru S1 C15 -132.4(2) . . . . ? Cl2 Ru S1 C15 135.2(2) . . . . ? Cl1 Ru S1 C15 -44.3(2) . . . . ? N2 Ru S1 C16 -65.3(3) . . . . ? N1 Ru S1 C16 -23.0(13) . . . . ? S2 Ru S1 C16 117.3(3) . . . . ? Cl2 Ru S1 C16 24.9(3) . . . . ? Cl1 Ru S1 C16 -154.6(3) . . . . ? N2 Ru S2 O2 24.7(12) . . . . ? N1 Ru S2 O2 -3.2(2) . . . . ? S1 Ru S2 O2 -179.9(2) . . . . ? Cl2 Ru S2 O2 -88.6(2) . . . . ? Cl1 Ru S2 O2 91.1(2) . . . . ? N2 Ru S2 C18 -98.7(11) . . . . ? N1 Ru S2 C18 -126.6(3) . . . . ? S1 Ru S2 C18 56.8(3) . . . . ? Cl2 Ru S2 C18 148.1(3) . . . . ? Cl1 Ru S2 C18 -32.2(3) . . . . ? N2 Ru S2 C17 147.5(11) . . . . ? N1 Ru S2 C17 119.5(3) . . . . ? S1 Ru S2 C17 -57.1(2) . . . . ? Cl2 Ru S2 C17 34.2(2) . . . . ? Cl1 Ru S2 C17 -146.1(2) . . . . ? N2 Ru N1 C5 -40.3(4) . . . . ? S1 Ru N1 C5 -82.8(14) . . . . ? S2 Ru N1 C5 136.9(4) . . . . ? Cl2 Ru N1 C5 -130.9(4) . . . . ? Cl1 Ru N1 C5 48.6(4) . . . . ? N2 Ru N1 C1 138.3(4) . . . . ? S1 Ru N1 C1 95.8(13) . . . . ? S2 Ru N1 C1 -44.5(4) . . . . ? Cl2 Ru N1 C1 47.7(4) . . . . ? Cl1 Ru N1 C1 -132.8(4) . . . . ? N1 Ru N2 N4 -141.3(4) . . . . ? S1 Ru N2 N4 35.1(4) . . . . ? S2 Ru N2 N4 -169.5(8) . . . . ? Cl2 Ru N2 N4 -56.1(4) . . . . ? Cl1 Ru N2 N4 124.1(4) . . . . ? N1 Ru N2 N3 34.4(4) . . . . ? S1 Ru N2 N3 -149.2(3) . . . . ? S2 Ru N2 N3 6.2(14) . . . . ? Cl2 Ru N2 N3 119.6(3) . . . . ? Cl1 Ru N2 N3 -60.2(3) . . . . ? N4 N2 N3 C7 -0.8(6) . . . . ? Ru N2 N3 C7 -177.3(3) . . . . ? N4 N2 N3 C6 -177.5(4) . . . . ? Ru N2 N3 C6 6.0(6) . . . . ? N3 N2 N4 C8 0.6(5) . . . . ? Ru N2 N4 C8 176.7(3) . . . . ? C5 N1 C1 C2 -4.8(8) . . . . ? Ru N1 C1 C2 176.5(4) . . . . ? N1 C1 C2 C3 0.5(9) . . . . ? C1 C2 C3 C4 2.6(9) . . . . ? C2 C3 C4 C5 -1.3(9) . . . . ? C1 N1 C5 C4 6.2(7) . . . . ? Ru N1 C5 C4 -175.2(4) . . . . ? C1 N1 C5 C6 -173.8(5) . . . . ? Ru N1 C5 C6 4.8(7) . . . . ? C3 C4 C5 N1 -3.3(8) . . . . ? C3 C4 C5 C6 176.7(5) . . . . ? C7 N3 C6 C5 124.7(5) . . . . ? N2 N3 C6 C5 -59.3(6) . . . . ? N1 C5 C6 N3 51.3(6) . . . . ? C4 C5 C6 N3 -128.7(5) . . . . ? N2 N3 C7 C8 0.7(6) . . . . ? C6 N3 C7 C8 177.1(5) . . . . ? N3 C7 C8 N4 -0.3(6) . . . . ? N3 C7 C8 C9 179.6(5) . . . . ? N2 N4 C8 C7 -0.2(6) . . . . ? N2 N4 C8 C9 180.0(5) . . . . ? C7 C8 C9 C10 -27.5(10) . . . . ? N4 C8 C9 C10 152.3(5) . . . . ? C7 C8 C9 C14 150.4(6) . . . . ? N4 C8 C9 C14 -29.7(8) . . . . ? C14 C9 C10 C11 -0.1(9) . . . . ? C8 C9 C10 C11 177.9(6) . . . . ? C9 C10 C11 C12 -1.5(10) . . . . ? C10 C11 C12 C13 2.3(12) . . . . ? C11 C12 C13 C14 -1.5(12) . . . . ? C10 C9 C14 C13 1.0(9) . . . . ? C8 C9 C14 C13 -177.0(6) . . . . ? C12 C13 C14 C9 -0.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.503 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.077 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 805601' #TrackingRef '- data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H24 Cl2 N4 O2 Ru S2' _chemical_formula_sum 'C18 H24 Cl2 N4 O2 Ru S2' _chemical_formula_weight 564.50 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 10.796(3) _cell_length_b 12.813(3) _cell_length_c 16.220(4) _cell_angle_alpha 90.00(2) _cell_angle_beta 91.19(2) _cell_angle_gamma 90.00(2) _cell_volume 2243.2(10) _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 prims _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.146 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6735 _exptl_absorpt_correction_T_max 0.8337 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14079 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.1041 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 28.73 _reflns_number_total 5423 _reflns_number_gt 2541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.01 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^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 SHELXL _refine_ls_extinction_coef 0.0027(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5423 _refine_ls_number_parameters 267 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 0.838 _refine_ls_restrained_S_all 0.881 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.71314(4) 0.11546(3) 0.18290(3) 0.04486(17) Uani 1 1 d . . . Cl1 Cl 0.68365(15) 0.09633(12) 0.33071(10) 0.0647(4) Uani 1 1 d . . . Cl2 Cl 0.76505(14) 0.29639(10) 0.20951(12) 0.0742(5) Uani 1 1 d . . . N1 N 0.5195(4) 0.1564(3) 0.1705(3) 0.0454(11) Uani 1 1 d . . . N2 N 0.6611(4) -0.0370(3) 0.1625(3) 0.0486(11) Uani 1 1 d . . . N3 N 0.5488(4) -0.0754(3) 0.1781(3) 0.0467(11) Uani 1 1 d . . . N4 N 0.7272(4) -0.1110(3) 0.1260(3) 0.0538(12) Uani 1 1 d . . . C1 C 0.4871(6) 0.2503(4) 0.1437(4) 0.0574(16) Uani 1 1 d . . . H1 H 0.5494 0.2962 0.1286 0.069 Uiso 1 1 calc R . . C2 C 0.3654(6) 0.2838(5) 0.1369(4) 0.0643(17) Uani 1 1 d . . . H2 H 0.3467 0.3514 0.1199 0.077 Uiso 1 1 calc R . . C3 C 0.2737(6) 0.2156(5) 0.1558(4) 0.0654(17) Uani 1 1 d . . . H3 H 0.1910 0.2356 0.1509 0.078 Uiso 1 1 calc R . . C4 C 0.3044(5) 0.1178(4) 0.1819(4) 0.0610(16) Uani 1 1 d . . . H4 H 0.2423 0.0703 0.1940 0.073 Uiso 1 1 calc R . . C5 C 0.4281(5) 0.0885(4) 0.1906(4) 0.0516(14) Uani 1 1 d . . . C6 C 0.4592(5) -0.0155(4) 0.2248(4) 0.0577(16) Uani 1 1 d . . . H6A H 0.4917 -0.0064 0.2806 0.069 Uiso 1 1 calc R . . H6B H 0.3835 -0.0559 0.2282 0.069 Uiso 1 1 calc R . . C7 C 0.5424(5) -0.1749(4) 0.1509(3) 0.0499(14) Uani 1 1 d . . . H7 H 0.4749 -0.2198 0.1537 0.060 Uiso 1 1 calc R . . C8 C 0.6544(5) -0.1960(4) 0.1189(3) 0.0469(13) Uani 1 1 d . . . C9 C 0.7032(5) -0.2917(4) 0.0809(3) 0.0513(14) Uani 1 1 d . . . C10 C 0.6303(6) -0.3831(4) 0.0769(4) 0.0700(18) Uani 1 1 d . . . H10 H 0.5508 -0.3837 0.0979 0.084 Uiso 1 1 calc R . . C11 C 0.6791(8) -0.4716(4) 0.0413(4) 0.080(2) Uani 1 1 d . . . H11 H 0.6314 -0.5320 0.0387 0.096 Uiso 1 1 calc R . . C12 C 0.7955(7) -0.4726(5) 0.0098(4) 0.076(2) Uani 1 1 d . . . H12 H 0.8268 -0.5334 -0.0130 0.091 Uiso 1 1 calc R . . C13 C 0.8655(6) -0.3843(5) 0.0121(4) 0.0723(19) Uani 1 1 d . . . H13 H 0.9445 -0.3849 -0.0098 0.087 Uiso 1 1 calc R . . C14 C 0.8203(6) -0.2940(4) 0.0465(4) 0.0640(17) Uani 1 1 d . . . H14 H 0.8686 -0.2339 0.0468 0.077 Uiso 1 1 calc R . . S1 S 0.91533(14) 0.07328(11) 0.20738(10) 0.0590(4) Uani 1 1 d . . . S2 S 0.73214(17) 0.14049(15) 0.04577(11) 0.0759(5) Uani 1 1 d . . . O1 O 1.0031(4) 0.0733(4) 0.1388(3) 0.0918(15) Uani 1 1 d . . . O2 O 0.6195(7) 0.1763(8) 0.0053(4) 0.191(3) Uani 1 1 d U . . C15 C 0.9313(6) -0.0498(5) 0.2568(5) 0.093(3) Uani 1 1 d . . . H15A H 0.8980 -0.1033 0.2214 0.139 Uiso 1 1 calc R . . H15B H 0.8871 -0.0490 0.3076 0.139 Uiso 1 1 calc R . . H15C H 1.0173 -0.0634 0.2682 0.139 Uiso 1 1 calc R . . C16 C 0.9830(6) 0.1521(5) 0.2860(4) 0.079(2) Uani 1 1 d . . . H16A H 1.0610 0.1227 0.3034 0.119 Uiso 1 1 calc R . . H16B H 0.9286 0.1551 0.3321 0.119 Uiso 1 1 calc R . . H16C H 0.9959 0.2213 0.2652 0.119 Uiso 1 1 calc R . . C17 C 0.8438(11) 0.2340(6) 0.0200(6) 0.161(5) Uani 1 1 d . . . H17A H 0.8396 0.2469 -0.0383 0.242 Uiso 1 1 calc R . . H17B H 0.9248 0.2085 0.0351 0.242 Uiso 1 1 calc R . . H17C H 0.8280 0.2977 0.0491 0.242 Uiso 1 1 calc R . . C18 C 0.7964(11) 0.0387(6) -0.0106(5) 0.141(4) Uani 1 1 d . . . H18A H 0.7455 -0.0224 -0.0060 0.211 Uiso 1 1 calc R . . H18B H 0.8782 0.0237 0.0106 0.211 Uiso 1 1 calc R . . H18C H 0.8009 0.0586 -0.0675 0.211 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 0.0380(3) 0.0423(2) 0.0544(3) -0.0020(2) 0.00232(19) -0.00087(18) Cl1 0.0602(10) 0.0842(10) 0.0497(10) -0.0035(8) 0.0004(8) 0.0071(8) Cl2 0.0542(10) 0.0462(8) 0.1221(15) -0.0116(8) 0.0001(10) -0.0032(6) N1 0.036(3) 0.045(2) 0.055(3) 0.001(2) 0.001(2) 0.0033(18) N2 0.038(3) 0.046(2) 0.062(3) -0.004(2) 0.007(2) 0.0016(19) N3 0.041(3) 0.042(2) 0.058(3) -0.003(2) 0.006(2) -0.0012(18) N4 0.048(3) 0.055(3) 0.059(3) -0.005(2) 0.003(2) 0.002(2) C1 0.055(4) 0.055(3) 0.062(4) 0.009(3) -0.005(3) 0.005(3) C2 0.064(4) 0.064(3) 0.064(4) 0.011(3) -0.007(4) 0.017(3) C3 0.044(4) 0.073(4) 0.079(5) 0.001(3) -0.004(3) 0.011(3) C4 0.039(3) 0.071(4) 0.073(4) -0.011(3) 0.007(3) -0.005(3) C5 0.044(4) 0.060(3) 0.050(4) -0.004(3) 0.001(3) -0.002(2) C6 0.044(4) 0.054(3) 0.075(5) 0.008(3) 0.016(3) -0.002(2) C7 0.053(4) 0.042(3) 0.055(4) -0.002(2) -0.002(3) -0.008(2) C8 0.049(4) 0.045(3) 0.047(4) -0.001(2) -0.006(3) -0.002(2) C9 0.056(4) 0.048(3) 0.049(4) -0.002(3) -0.008(3) 0.006(2) C10 0.087(5) 0.048(3) 0.076(5) -0.009(3) 0.017(4) -0.001(3) C11 0.111(7) 0.045(3) 0.085(5) -0.005(3) 0.011(5) -0.007(3) C12 0.087(6) 0.057(4) 0.083(5) -0.011(3) -0.011(4) 0.020(4) C13 0.064(4) 0.078(4) 0.075(5) -0.022(4) -0.004(4) 0.021(4) C14 0.059(4) 0.060(3) 0.073(5) -0.011(3) -0.006(4) 0.002(3) S1 0.0397(9) 0.0631(8) 0.0741(12) -0.0130(8) -0.0048(8) 0.0053(6) S2 0.0653(12) 0.1070(13) 0.0557(11) 0.0192(9) 0.0113(9) 0.0043(9) O1 0.037(3) 0.152(4) 0.087(4) -0.024(3) 0.016(3) 0.006(3) O2 0.121(5) 0.363(8) 0.088(4) 0.053(5) -0.012(4) 0.068(6) C15 0.070(5) 0.068(4) 0.138(7) 0.003(4) -0.033(5) 0.016(3) C16 0.056(4) 0.087(4) 0.093(6) -0.021(4) -0.020(4) 0.000(3) C17 0.261(13) 0.088(6) 0.140(9) 0.012(5) 0.110(9) -0.045(7) C18 0.267(13) 0.080(6) 0.077(6) -0.015(4) 0.042(7) -0.013(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N2 2.058(4) . ? Ru N1 2.161(4) . ? Ru S2 2.2607(19) . ? Ru S1 2.2756(17) . ? Ru Cl2 2.4217(15) . ? Ru Cl1 2.4374(17) . ? N1 C1 1.324(6) . ? N1 C5 1.360(6) . ? N2 N4 1.333(5) . ? N2 N3 1.337(5) . ? N3 C7 1.350(6) . ? N3 C6 1.460(6) . ? N4 C8 1.347(6) . ? C1 C2 1.385(8) . ? C2 C3 1.359(8) . ? C3 C4 1.362(7) . ? C4 C5 1.391(7) . ? C5 C6 1.480(7) . ? C7 C8 1.353(7) . ? C8 C9 1.474(7) . ? C9 C14 1.393(8) . ? C9 C10 1.411(7) . ? C10 C11 1.382(8) . ? C11 C12 1.367(9) . ? C12 C13 1.360(9) . ? C13 C14 1.378(7) . ? S1 O1 1.476(5) . ? S1 C16 1.773(6) . ? S1 C15 1.775(6) . ? S2 O2 1.444(6) . ? S2 C18 1.746(8) . ? S2 C17 1.756(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 N2 Ru N1 87.44(16) . . ? N2 Ru S2 90.36(14) . . ? N1 Ru S2 88.95(13) . . ? N2 Ru S1 93.45(13) . . ? N1 Ru S1 175.28(12) . . ? S2 Ru S1 95.68(7) . . ? N2 Ru Cl2 177.36(13) . . ? N1 Ru Cl2 90.22(11) . . ? S2 Ru Cl2 90.81(7) . . ? S1 Ru Cl2 88.78(6) . . ? N2 Ru Cl1 91.26(14) . . ? N1 Ru Cl1 88.27(12) . . ? S2 Ru Cl1 176.71(6) . . ? S1 Ru Cl1 87.07(6) . . ? Cl2 Ru Cl1 87.44(6) . . ? C1 N1 C5 118.2(5) . . ? C1 N1 Ru 120.0(4) . . ? C5 N1 Ru 121.8(3) . . ? N4 N2 N3 108.6(4) . . ? N4 N2 Ru 126.9(3) . . ? N3 N2 Ru 124.4(3) . . ? N2 N3 C7 109.1(4) . . ? N2 N3 C6 121.2(4) . . ? C7 N3 C6 129.5(4) . . ? N2 N4 C8 107.2(4) . . ? N1 C1 C2 123.4(5) . . ? C3 C2 C1 118.6(5) . . ? C2 C3 C4 119.1(6) . . ? C3 C4 C5 120.5(5) . . ? N1 C5 C4 120.2(5) . . ? N1 C5 C6 120.4(5) . . ? C4 C5 C6 119.4(5) . . ? N3 C6 C5 115.2(5) . . ? N3 C7 C8 105.9(4) . . ? N4 C8 C7 109.3(4) . . ? N4 C8 C9 119.7(5) . . ? C7 C8 C9 131.0(5) . . ? C14 C9 C10 118.2(5) . . ? C14 C9 C8 121.4(5) . . ? C10 C9 C8 120.4(5) . . ? C11 C10 C9 118.9(6) . . ? C12 C11 C10 121.6(6) . . ? C13 C12 C11 119.8(6) . . ? C12 C13 C14 120.5(7) . . ? C13 C14 C9 120.8(6) . . ? O1 S1 C16 106.3(3) . . ? O1 S1 C15 106.4(3) . . ? C16 S1 C15 98.4(4) . . ? O1 S1 Ru 119.8(2) . . ? C16 S1 Ru 111.7(2) . . ? C15 S1 Ru 111.9(2) . . ? O2 S2 C18 109.8(5) . . ? O2 S2 C17 104.5(6) . . ? C18 S2 C17 95.9(5) . . ? O2 S2 Ru 113.5(3) . . ? C18 S2 Ru 117.1(3) . . ? C17 S2 Ru 114.1(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru N1 C1 -151.8(4) . . . . ? S2 Ru N1 C1 -61.4(4) . . . . ? S1 Ru N1 C1 107.1(13) . . . . ? Cl2 Ru N1 C1 29.4(4) . . . . ? Cl1 Ru N1 C1 116.8(4) . . . . ? N2 Ru N1 C5 29.0(4) . . . . ? S2 Ru N1 C5 119.4(4) . . . . ? S1 Ru N1 C5 -72.1(15) . . . . ? Cl2 Ru N1 C5 -149.8(4) . . . . ? Cl1 Ru N1 C5 -62.4(4) . . . . ? N1 Ru N2 N4 148.9(4) . . . . ? S2 Ru N2 N4 60.0(4) . . . . ? S1 Ru N2 N4 -35.7(4) . . . . ? Cl2 Ru N2 N4 176(43) . . . . ? Cl1 Ru N2 N4 -122.9(4) . . . . ? N1 Ru N2 N3 -25.1(4) . . . . ? S2 Ru N2 N3 -114.0(4) . . . . ? S1 Ru N2 N3 150.3(4) . . . . ? Cl2 Ru N2 N3 3(3) . . . . ? Cl1 Ru N2 N3 63.1(4) . . . . ? N4 N2 N3 C7 -0.3(6) . . . . ? Ru N2 N3 C7 174.6(3) . . . . ? N4 N2 N3 C6 174.2(5) . . . . ? Ru N2 N3 C6 -10.9(7) . . . . ? N3 N2 N4 C8 0.1(6) . . . . ? Ru N2 N4 C8 -174.6(4) . . . . ? C5 N1 C1 C2 1.7(9) . . . . ? Ru N1 C1 C2 -177.6(5) . . . . ? N1 C1 C2 C3 -2.6(10) . . . . ? C1 C2 C3 C4 1.1(10) . . . . ? C2 C3 C4 C5 1.1(10) . . . . ? C1 N1 C5 C4 0.6(8) . . . . ? Ru N1 C5 C4 179.9(4) . . . . ? C1 N1 C5 C6 -176.9(5) . . . . ? Ru N1 C5 C6 2.3(7) . . . . ? C3 C4 C5 N1 -2.0(9) . . . . ? C3 C4 C5 C6 175.5(6) . . . . ? N2 N3 C6 C5 56.8(7) . . . . ? C7 N3 C6 C5 -129.9(6) . . . . ? N1 C5 C6 N3 -50.6(7) . . . . ? C4 C5 C6 N3 131.8(6) . . . . ? N2 N3 C7 C8 0.4(6) . . . . ? C6 N3 C7 C8 -173.5(5) . . . . ? N2 N4 C8 C7 0.2(6) . . . . ? N2 N4 C8 C9 -179.6(5) . . . . ? N3 C7 C8 N4 -0.3(6) . . . . ? N3 C7 C8 C9 179.4(5) . . . . ? N4 C8 C9 C14 -4.8(8) . . . . ? C7 C8 C9 C14 175.5(6) . . . . ? N4 C8 C9 C10 176.7(5) . . . . ? C7 C8 C9 C10 -3.0(9) . . . . ? C14 C9 C10 C11 1.8(9) . . . . ? C8 C9 C10 C11 -179.7(6) . . . . ? C9 C10 C11 C12 -0.2(11) . . . . ? C10 C11 C12 C13 -1.0(11) . . . . ? C11 C12 C13 C14 0.6(11) . . . . ? C12 C13 C14 C9 1.1(10) . . . . ? C10 C9 C14 C13 -2.2(9) . . . . ? C8 C9 C14 C13 179.2(6) . . . . ? N2 Ru S1 O1 91.7(3) . . . . ? N1 Ru S1 O1 -167.4(13) . . . . ? S2 Ru S1 O1 1.0(2) . . . . ? Cl2 Ru S1 O1 -89.7(2) . . . . ? Cl1 Ru S1 O1 -177.2(2) . . . . ? N2 Ru S1 C16 -143.1(3) . . . . ? N1 Ru S1 C16 -42.3(14) . . . . ? S2 Ru S1 C16 126.2(3) . . . . ? Cl2 Ru S1 C16 35.5(3) . . . . ? Cl1 Ru S1 C16 -52.0(3) . . . . ? N2 Ru S1 C15 -33.8(3) . . . . ? N1 Ru S1 C15 67.0(14) . . . . ? S2 Ru S1 C15 -124.6(3) . . . . ? Cl2 Ru S1 C15 144.8(3) . . . . ? Cl1 Ru S1 C15 57.2(3) . . . . ? N2 Ru S2 O2 90.1(5) . . . . ? N1 Ru S2 O2 2.7(5) . . . . ? S1 Ru S2 O2 -176.4(5) . . . . ? Cl2 Ru S2 O2 -87.5(5) . . . . ? Cl1 Ru S2 O2 -29.5(13) . . . . ? N2 Ru S2 C18 -39.6(4) . . . . ? N1 Ru S2 C18 -127.0(4) . . . . ? S1 Ru S2 C18 54.0(4) . . . . ? Cl2 Ru S2 C18 142.8(4) . . . . ? Cl1 Ru S2 C18 -159.2(11) . . . . ? N2 Ru S2 C17 -150.3(4) . . . . ? N1 Ru S2 C17 122.2(4) . . . . ? S1 Ru S2 C17 -56.8(4) . . . . ? Cl2 Ru S2 C17 32.0(4) . . . . ? Cl1 Ru S2 C17 90.1(12) . . . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 28.73 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.813 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.093 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 805602' #TrackingRef '- data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H30 N4 O Ru S4 2+, 2(C F3 S O3 1-)' _chemical_formula_sum 'C24 H30 F6 N4 O7 Ru S6' _chemical_formula_weight 893.95 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.590(3) _cell_length_b 12.611(3) _cell_length_c 12.511(5) _cell_angle_alpha 64.09(2) _cell_angle_beta 71.65(3) _cell_angle_gamma 85.07(3) _cell_volume 1692.7(9) _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 block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.915 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6566 _exptl_absorpt_correction_T_max 0.8210 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Linear fit to sin(theta)/lambda - 12 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15655 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6379 _reflns_number_gt 3177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1282P)^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 6379 _refine_ls_number_parameters 398 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1198 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2254 _refine_ls_wR_factor_gt 0.1980 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.928 _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 0.70966(6) 0.29402(6) 0.65491(6) 0.0587(3) Uani 1 1 d . . . S4 S 0.5723(2) 0.1738(2) 0.8310(2) 0.0684(6) Uani 1 1 d . . . O1 O 0.5867(6) 0.0469(5) 0.8636(7) 0.093(2) Uani 1 1 d . . . S1 S 0.5904(2) 0.3534(2) 0.5345(2) 0.0711(6) Uani 1 1 d . . . S2 S 0.7511(2) 0.1362(2) 0.6024(2) 0.0715(6) Uani 1 1 d . . . S3 S 0.85577(19) 0.4041(2) 0.4694(2) 0.0705(6) Uani 1 1 d . . . N1 N 0.8220(6) 0.2490(7) 0.7671(7) 0.0670(18) Uani 1 1 d . . . N2 N 0.6668(6) 0.4347(6) 0.7055(6) 0.0582(16) Uani 1 1 d . . . N3 N 0.7371(5) 0.4879(6) 0.7297(7) 0.0627(18) Uani 1 1 d . . . N4 N 0.5665(6) 0.4744(6) 0.7317(7) 0.0637(18) Uani 1 1 d . . . C1 C 0.8365(9) 0.1349(9) 0.8331(10) 0.081(3) Uani 1 1 d . . . H1 H 0.8079 0.0777 0.8198 0.097 Uiso 1 1 calc R . . C2 C 0.8930(11) 0.1005(11) 0.9204(12) 0.105(4) Uani 1 1 d . . . H2 H 0.8997 0.0205 0.9667 0.126 Uiso 1 1 calc R . . C3 C 0.9387(9) 0.1816(10) 0.9396(12) 0.092(3) Uani 1 1 d . . . H3 H 0.9777 0.1597 0.9973 0.111 Uiso 1 1 calc R . . C4 C 0.9246(8) 0.2953(10) 0.8707(10) 0.079(3) Uani 1 1 d . . . H4 H 0.9553 0.3531 0.8814 0.095 Uiso 1 1 calc R . . C5 C 0.8673(7) 0.3300(9) 0.7860(8) 0.065(2) Uani 1 1 d . . . C6 C 0.8539(7) 0.4588(8) 0.7105(9) 0.069(2) Uani 1 1 d . . . H6A H 0.8917 0.5060 0.7332 0.083 Uiso 1 1 calc R . . H6B H 0.8900 0.4792 0.6226 0.083 Uiso 1 1 calc R . . C7 C 0.6840(8) 0.5626(8) 0.7728(8) 0.068(2) Uani 1 1 d . . . H7 H 0.7136 0.6095 0.7981 0.081 Uiso 1 1 calc R . . C8 C 0.5743(7) 0.5567(8) 0.7726(8) 0.062(2) Uani 1 1 d . . . C9 C 0.4799(8) 0.6265(8) 0.7999(8) 0.066(2) Uani 1 1 d . . . C10 C 0.4964(8) 0.7467(8) 0.7613(8) 0.067(2) Uani 1 1 d . . . H10 H 0.5691 0.7809 0.7246 0.081 Uiso 1 1 calc R . . C11 C 0.4097(10) 0.8154(10) 0.7755(10) 0.085(3) Uani 1 1 d . . . H11 H 0.4223 0.8961 0.7476 0.102 Uiso 1 1 calc R . . C12 C 0.3019(10) 0.7639(11) 0.8322(10) 0.086(3) Uani 1 1 d . . . H12 H 0.2418 0.8109 0.8414 0.103 Uiso 1 1 calc R . . C13 C 0.2820(9) 0.6461(11) 0.8748(10) 0.085(3) Uani 1 1 d . . . H13 H 0.2091 0.6123 0.9138 0.102 Uiso 1 1 calc R . . C14 C 0.3732(8) 0.5761(9) 0.8591(8) 0.071(2) Uani 1 1 d . . . H14 H 0.3609 0.4951 0.8891 0.085 Uiso 1 1 calc R . . C15 C 0.5990(9) 0.2425(10) 0.4735(9) 0.084(3) Uani 1 1 d . . . H15A H 0.5270 0.2328 0.4648 0.101 Uiso 1 1 calc R . . H15B H 0.6541 0.2710 0.3912 0.101 Uiso 1 1 calc R . . C16 C 0.6298(9) 0.1274(9) 0.5551(10) 0.082(3) Uani 1 1 d . . . H16A H 0.6460 0.0772 0.5119 0.098 Uiso 1 1 calc R . . H16B H 0.5662 0.0903 0.6295 0.098 Uiso 1 1 calc R . . C17 C 0.8617(9) 0.1913(11) 0.4516(10) 0.094(3) Uani 1 1 d . . . H17A H 0.9078 0.1272 0.4455 0.113 Uiso 1 1 calc R . . H17B H 0.8281 0.2206 0.3847 0.113 Uiso 1 1 calc R . . C18 C 0.9339(8) 0.2891(10) 0.4370(10) 0.084(3) Uani 1 1 d . . . H18A H 0.9846 0.3240 0.3522 0.101 Uiso 1 1 calc R . . H18B H 0.9791 0.2554 0.4928 0.101 Uiso 1 1 calc R . . C19 C 0.7909(9) 0.4672(10) 0.3458(9) 0.084(3) Uani 1 1 d . . . H19A H 0.8283 0.5434 0.2843 0.101 Uiso 1 1 calc R . . H19B H 0.7996 0.4160 0.3044 0.101 Uiso 1 1 calc R . . C20 C 0.6668(10) 0.4823(9) 0.3976(9) 0.085(3) Uani 1 1 d . . . H20A H 0.6323 0.5019 0.3325 0.102 Uiso 1 1 calc R . . H20B H 0.6594 0.5485 0.4188 0.102 Uiso 1 1 calc R . . C21 C 0.5624(9) 0.1947(9) 0.9639(9) 0.085(3) Uani 1 1 d . . . H21A H 0.5072 0.1385 1.0352 0.127 Uiso 1 1 calc R . . H21B H 0.5407 0.2733 0.9504 0.127 Uiso 1 1 calc R . . H21C H 0.6338 0.1837 0.9787 0.127 Uiso 1 1 calc R . . C22 C 0.4340(9) 0.2028(11) 0.8292(11) 0.100(4) Uani 1 1 d . . . H22A H 0.4188 0.1792 0.7720 0.150 Uiso 1 1 calc R . . H22B H 0.4242 0.2858 0.8032 0.150 Uiso 1 1 calc R . . H22C H 0.3833 0.1594 0.9115 0.150 Uiso 1 1 calc R . . S5 S 0.9119(2) 0.6646(2) 0.9148(2) 0.0772(7) Uani 1 1 d . . . O2 O 0.8881(6) 0.5931(6) 0.8623(7) 0.088(2) Uani 1 1 d . . . O3 O 1.0243(6) 0.7171(8) 0.8606(8) 0.104(2) Uani 1 1 d . . . O4 O 0.8706(8) 0.6178(8) 1.0460(7) 0.115(3) Uani 1 1 d . . . C25 C 0.8290(11) 0.7895(12) 0.8637(15) 0.103(4) Uani 1 1 d . . . F1 F 0.7203(7) 0.7521(9) 0.8992(11) 0.160(4) Uani 1 1 d . . . F2 F 0.8596(9) 0.8440(8) 0.7399(9) 0.162(4) Uani 1 1 d . . . F3 F 0.8319(8) 0.8635(7) 0.9075(10) 0.156(4) Uani 1 1 d . . . S6 S 0.7833(5) 0.7682(5) 0.4016(7) 0.195(3) Uani 1 1 d D . . O5 O 0.6752(10) 0.7122(12) 0.4707(13) 0.186(5) Uiso 1 1 d D . . O6 O 0.8040(15) 0.8308(15) 0.2495(14) 0.230(7) Uiso 1 1 d D . . O7 O 0.8846(13) 0.6992(14) 0.4230(15) 0.211(6) Uiso 1 1 d D . . C26 C 0.8188(19) 0.9096(16) 0.401(2) 0.200 Uiso 1 1 d D . . F4 F 0.7251(17) 0.9524(17) 0.3684(18) 0.300 Uiso 1 1 d D . . F5 F 0.7846(17) 0.8513(19) 0.525(2) 0.303(8) Uiso 1 1 d D . . F6 F 0.906(2) 0.9529(19) 0.297(2) 0.324(9) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0623(4) 0.0587(4) 0.0543(4) -0.0241(3) -0.0149(3) -0.0058(3) S4 0.0770(14) 0.0643(14) 0.0584(13) -0.0260(11) -0.0098(11) -0.0155(11) O1 0.126(6) 0.053(4) 0.076(4) -0.024(3) 0.000(4) -0.022(4) S1 0.0728(14) 0.0796(16) 0.0686(14) -0.0313(12) -0.0312(12) -0.0030(12) S2 0.0813(15) 0.0666(14) 0.0714(15) -0.0362(12) -0.0194(12) -0.0002(12) S3 0.0677(13) 0.0763(16) 0.0606(13) -0.0300(12) -0.0059(11) -0.0132(11) N1 0.069(4) 0.066(5) 0.072(5) -0.034(4) -0.025(4) 0.000(4) N2 0.058(4) 0.052(4) 0.064(4) -0.026(3) -0.016(3) -0.003(3) N3 0.051(4) 0.066(4) 0.080(5) -0.035(4) -0.025(4) 0.000(3) N4 0.069(4) 0.058(4) 0.070(5) -0.028(4) -0.027(4) 0.002(3) C1 0.096(7) 0.072(7) 0.093(7) -0.040(6) -0.050(6) 0.011(5) C2 0.150(11) 0.080(8) 0.112(9) -0.046(7) -0.077(9) 0.039(8) C3 0.101(8) 0.089(8) 0.126(10) -0.063(7) -0.069(8) 0.031(6) C4 0.075(6) 0.096(8) 0.091(7) -0.057(6) -0.035(6) 0.014(5) C5 0.055(4) 0.088(6) 0.068(5) -0.045(5) -0.023(4) 0.009(4) C6 0.070(5) 0.064(6) 0.082(6) -0.040(5) -0.021(5) 0.001(4) C7 0.078(6) 0.070(6) 0.070(6) -0.037(5) -0.032(5) 0.006(5) C8 0.066(5) 0.058(5) 0.059(5) -0.024(4) -0.016(4) -0.003(4) C9 0.073(6) 0.067(6) 0.062(5) -0.033(5) -0.019(5) 0.005(5) C10 0.074(6) 0.071(6) 0.071(6) -0.040(5) -0.029(5) 0.007(5) C11 0.098(8) 0.076(7) 0.092(8) -0.048(6) -0.025(6) 0.006(6) C12 0.093(8) 0.096(8) 0.074(6) -0.046(6) -0.025(6) 0.029(6) C13 0.082(7) 0.086(8) 0.078(7) -0.034(6) -0.012(6) -0.002(6) C14 0.074(6) 0.068(6) 0.062(5) -0.025(5) -0.013(5) 0.004(5) C15 0.099(7) 0.101(8) 0.068(6) -0.040(6) -0.037(6) -0.009(6) C16 0.096(7) 0.072(6) 0.084(7) -0.044(6) -0.018(6) -0.013(5) C17 0.091(7) 0.124(9) 0.083(7) -0.069(7) -0.012(6) 0.005(7) C18 0.069(6) 0.106(8) 0.084(7) -0.053(6) -0.007(5) -0.014(6) C19 0.099(8) 0.086(7) 0.051(5) -0.017(5) -0.012(5) -0.026(6) C20 0.118(9) 0.073(6) 0.066(6) -0.014(5) -0.051(6) -0.003(6) C21 0.101(7) 0.082(7) 0.064(6) -0.030(5) -0.014(5) -0.015(6) C22 0.080(7) 0.121(10) 0.084(8) -0.043(7) 0.002(6) -0.031(6) S5 0.0892(17) 0.0761(16) 0.0743(16) -0.0361(13) -0.0285(14) -0.0016(13) O2 0.107(5) 0.086(5) 0.096(5) -0.057(4) -0.039(4) 0.002(4) O3 0.075(4) 0.125(6) 0.124(6) -0.057(5) -0.041(5) -0.001(4) O4 0.160(8) 0.119(6) 0.067(5) -0.038(4) -0.030(5) -0.028(6) C25 0.100(9) 0.099(9) 0.125(11) -0.061(9) -0.034(8) 0.004(7) F1 0.105(6) 0.209(9) 0.236(11) -0.143(9) -0.087(7) 0.063(6) F2 0.201(10) 0.133(7) 0.121(7) -0.018(6) -0.075(7) 0.050(6) F3 0.186(9) 0.106(6) 0.233(11) -0.108(7) -0.095(8) 0.039(6) S6 0.143(4) 0.151(4) 0.247(7) -0.035(4) -0.062(4) -0.055(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N2 2.108(7) . ? Ru N1 2.170(7) . ? Ru S4 2.297(3) . ? Ru S1 2.308(2) . ? Ru S2 2.326(3) . ? Ru S3 2.374(3) . ? S4 O1 1.478(7) . ? S4 C22 1.753(11) . ? S4 C21 1.761(10) . ? S1 C20 1.816(10) . ? S1 C15 1.845(10) . ? S2 C16 1.830(10) . ? S2 C17 1.830(11) . ? S3 C18 1.804(11) . ? S3 C19 1.816(10) . ? N1 C1 1.340(12) . ? N1 C5 1.349(11) . ? N2 N4 1.314(9) . ? N2 N3 1.331(9) . ? N3 C7 1.318(11) . ? N3 C6 1.455(11) . ? N4 C8 1.365(10) . ? C1 C2 1.382(14) . ? C2 C3 1.356(15) . ? C3 C4 1.342(14) . ? C4 C5 1.363(12) . ? C5 C6 1.507(12) . ? C7 C8 1.390(12) . ? C8 C9 1.460(12) . ? C9 C14 1.366(13) . ? C9 C10 1.388(12) . ? C10 C11 1.350(13) . ? C11 C12 1.381(15) . ? C12 C13 1.357(15) . ? C13 C14 1.404(13) . ? C15 C16 1.470(14) . ? C17 C18 1.508(14) . ? C19 C20 1.522(15) . ? S5 O4 1.408(8) . ? S5 O2 1.421(6) . ? S5 O3 1.438(8) . ? S5 C25 1.799(14) . ? C25 F3 1.280(14) . ? C25 F2 1.326(15) . ? C25 F1 1.356(15) . ? S6 O5 1.411(12) . ? S6 O7 1.509(12) . ? S6 O6 1.650(13) . ? S6 C26 1.872(16) . ? C26 F6 1.330(16) . ? C26 F5 1.333(16) . ? C26 F4 1.359(16) . ? 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 N2 Ru N1 85.8(3) . . ? N2 Ru S4 89.8(2) . . ? N1 Ru S4 88.3(2) . . ? N2 Ru S1 90.97(19) . . ? N1 Ru S1 176.5(2) . . ? S4 Ru S1 92.96(9) . . ? N2 Ru S2 178.17(19) . . ? N1 Ru S2 95.0(2) . . ? S4 Ru S2 88.54(9) . . ? S1 Ru S2 88.27(9) . . ? N2 Ru S3 95.0(2) . . ? N1 Ru S3 91.8(2) . . ? S4 Ru S3 175.13(9) . . ? S1 Ru S3 87.24(9) . . ? S2 Ru S3 86.60(9) . . ? O1 S4 C22 108.2(5) . . ? O1 S4 C21 107.5(5) . . ? C22 S4 C21 97.7(6) . . ? O1 S4 Ru 112.9(3) . . ? C22 S4 Ru 115.8(4) . . ? C21 S4 Ru 113.6(4) . . ? C20 S1 C15 102.9(5) . . ? C20 S1 Ru 102.8(3) . . ? C15 S1 Ru 105.1(3) . . ? C16 S2 C17 100.8(5) . . ? C16 S2 Ru 101.3(3) . . ? C17 S2 Ru 106.7(4) . . ? C18 S3 C19 102.3(5) . . ? C18 S3 Ru 102.1(4) . . ? C19 S3 Ru 105.8(3) . . ? C1 N1 C5 117.8(8) . . ? C1 N1 Ru 119.0(6) . . ? C5 N1 Ru 122.7(6) . . ? N4 N2 N3 109.5(6) . . ? N4 N2 Ru 126.5(5) . . ? N3 N2 Ru 123.6(5) . . ? C7 N3 N2 110.2(7) . . ? C7 N3 C6 128.9(7) . . ? N2 N3 C6 120.9(7) . . ? N2 N4 C8 106.9(6) . . ? N1 C1 C2 121.4(9) . . ? C3 C2 C1 120.9(10) . . ? C4 C3 C2 116.4(10) . . ? C3 C4 C5 123.1(10) . . ? N1 C5 C4 120.4(9) . . ? N1 C5 C6 118.5(7) . . ? C4 C5 C6 121.2(8) . . ? N3 C6 C5 112.8(7) . . ? N3 C7 C8 105.6(8) . . ? N4 C8 C7 107.7(8) . . ? N4 C8 C9 121.6(8) . . ? C7 C8 C9 130.5(8) . . ? C14 C9 C10 118.7(9) . . ? C14 C9 C8 120.8(9) . . ? C10 C9 C8 120.4(9) . . ? C11 C10 C9 121.7(10) . . ? C10 C11 C12 119.0(10) . . ? C13 C12 C11 121.3(10) . . ? C12 C13 C14 118.9(10) . . ? C9 C14 C13 120.4(10) . . ? C16 C15 S1 112.4(6) . . ? C15 C16 S2 113.8(7) . . ? C18 C17 S2 110.7(7) . . ? C17 C18 S3 114.0(7) . . ? C20 C19 S3 111.1(6) . . ? C19 C20 S1 114.6(7) . . ? O4 S5 O2 115.4(5) . . ? O4 S5 O3 114.8(5) . . ? O2 S5 O3 114.7(5) . . ? O4 S5 C25 103.6(7) . . ? O2 S5 C25 102.9(5) . . ? O3 S5 C25 103.0(6) . . ? F3 C25 F2 110.0(12) . . ? F3 C25 F1 107.4(12) . . ? F2 C25 F1 104.9(12) . . ? F3 C25 S5 113.9(10) . . ? F2 C25 S5 110.5(9) . . ? F1 C25 S5 109.8(10) . . ? O5 S6 O7 119.4(9) . . ? O5 S6 O6 112.6(10) . . ? O7 S6 O6 106.9(10) . . ? O5 S6 C26 119.7(10) . . ? O7 S6 C26 101.8(10) . . ? O6 S6 C26 92.7(10) . . ? F6 C26 F5 147(2) . . ? F6 C26 F4 107(2) . . ? F5 C26 F4 106(2) . . ? F6 C26 S6 100.7(16) . . ? F5 C26 S6 86.0(14) . . ? F4 C26 S6 87.8(13) . . ? 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 N2 Ru S4 O1 -162.5(4) . . . . ? N1 Ru S4 O1 -76.7(4) . . . . ? S1 Ru S4 O1 106.5(4) . . . . ? S2 Ru S4 O1 18.3(4) . . . . ? S3 Ru S4 O1 14.2(11) . . . . ? N2 Ru S4 C22 72.0(5) . . . . ? N1 Ru S4 C22 157.8(5) . . . . ? S1 Ru S4 C22 -19.0(5) . . . . ? S2 Ru S4 C22 -107.2(5) . . . . ? S3 Ru S4 C22 -111.2(11) . . . . ? N2 Ru S4 C21 -39.9(5) . . . . ? N1 Ru S4 C21 45.9(5) . . . . ? S1 Ru S4 C21 -130.9(4) . . . . ? S2 Ru S4 C21 141.0(4) . . . . ? S3 Ru S4 C21 136.9(10) . . . . ? N2 Ru S1 C20 75.0(4) . . . . ? N1 Ru S1 C20 53(4) . . . . ? S4 Ru S1 C20 164.8(4) . . . . ? S2 Ru S1 C20 -106.7(4) . . . . ? S3 Ru S1 C20 -20.0(4) . . . . ? N2 Ru S1 C15 -177.7(4) . . . . ? N1 Ru S1 C15 161(3) . . . . ? S4 Ru S1 C15 -87.9(4) . . . . ? S2 Ru S1 C15 0.6(4) . . . . ? S3 Ru S1 C15 87.3(4) . . . . ? N2 Ru S2 C16 45(6) . . . . ? N1 Ru S2 C16 160.5(4) . . . . ? S4 Ru S2 C16 72.4(4) . . . . ? S1 Ru S2 C16 -20.6(4) . . . . ? S3 Ru S2 C16 -108.0(4) . . . . ? N2 Ru S2 C17 150(6) . . . . ? N1 Ru S2 C17 -94.4(4) . . . . ? S4 Ru S2 C17 177.4(4) . . . . ? S1 Ru S2 C17 84.4(4) . . . . ? S3 Ru S2 C17 -2.9(4) . . . . ? N2 Ru S3 C18 162.1(4) . . . . ? N1 Ru S3 C18 76.2(4) . . . . ? S4 Ru S3 C18 -14.6(11) . . . . ? S1 Ru S3 C18 -107.2(4) . . . . ? S2 Ru S3 C18 -18.7(4) . . . . ? N2 Ru S3 C19 -91.2(4) . . . . ? N1 Ru S3 C19 -177.1(4) . . . . ? S4 Ru S3 C19 92.0(11) . . . . ? S1 Ru S3 C19 -0.5(4) . . . . ? S2 Ru S3 C19 88.0(4) . . . . ? N2 Ru N1 C1 144.1(7) . . . . ? S4 Ru N1 C1 54.1(7) . . . . ? S1 Ru N1 C1 166(3) . . . . ? S2 Ru N1 C1 -34.2(7) . . . . ? S3 Ru N1 C1 -121.0(7) . . . . ? N2 Ru N1 C5 -27.4(7) . . . . ? S4 Ru N1 C5 -117.3(7) . . . . ? S1 Ru N1 C5 -6(4) . . . . ? S2 Ru N1 C5 154.3(7) . . . . ? S3 Ru N1 C5 67.5(7) . . . . ? N1 Ru N2 N4 -141.9(7) . . . . ? S4 Ru N2 N4 -53.6(6) . . . . ? S1 Ru N2 N4 39.4(6) . . . . ? S2 Ru N2 N4 -26(6) . . . . ? S3 Ru N2 N4 126.7(6) . . . . ? N1 Ru N2 N3 30.0(6) . . . . ? S4 Ru N2 N3 118.3(6) . . . . ? S1 Ru N2 N3 -148.7(6) . . . . ? S2 Ru N2 N3 146(6) . . . . ? S3 Ru N2 N3 -61.4(6) . . . . ? N4 N2 N3 C7 0.4(9) . . . . ? Ru N2 N3 C7 -172.6(6) . . . . ? N4 N2 N3 C6 179.1(8) . . . . ? Ru N2 N3 C6 6.1(10) . . . . ? N3 N2 N4 C8 0.7(9) . . . . ? Ru N2 N4 C8 173.5(5) . . . . ? C5 N1 C1 C2 1.9(15) . . . . ? Ru N1 C1 C2 -170.0(9) . . . . ? N1 C1 C2 C3 -2.0(19) . . . . ? C1 C2 C3 C4 0.8(19) . . . . ? C2 C3 C4 C5 0.4(17) . . . . ? C1 N1 C5 C4 -0.7(13) . . . . ? Ru N1 C5 C4 170.8(7) . . . . ? C1 N1 C5 C6 178.7(9) . . . . ? Ru N1 C5 C6 -9.7(11) . . . . ? C3 C4 C5 N1 -0.4(15) . . . . ? C3 C4 C5 C6 -179.8(10) . . . . ? C7 N3 C6 C5 119.8(10) . . . . ? N2 N3 C6 C5 -58.6(10) . . . . ? N1 C5 C6 N3 59.7(11) . . . . ? C4 C5 C6 N3 -120.9(9) . . . . ? N2 N3 C7 C8 -1.3(10) . . . . ? C6 N3 C7 C8 -179.9(8) . . . . ? N2 N4 C8 C7 -1.5(9) . . . . ? N2 N4 C8 C9 174.7(8) . . . . ? N3 C7 C8 N4 1.7(10) . . . . ? N3 C7 C8 C9 -174.0(9) . . . . ? N4 C8 C9 C14 40.4(13) . . . . ? C7 C8 C9 C14 -144.4(10) . . . . ? N4 C8 C9 C10 -136.8(9) . . . . ? C7 C8 C9 C10 38.4(14) . . . . ? C14 C9 C10 C11 -3.1(14) . . . . ? C8 C9 C10 C11 174.1(9) . . . . ? C9 C10 C11 C12 1.2(15) . . . . ? C10 C11 C12 C13 0.8(16) . . . . ? C11 C12 C13 C14 -0.8(17) . . . . ? C10 C9 C14 C13 3.0(14) . . . . ? C8 C9 C14 C13 -174.2(8) . . . . ? C12 C13 C14 C9 -1.1(15) . . . . ? C20 S1 C15 C16 133.7(8) . . . . ? Ru S1 C15 C16 26.5(8) . . . . ? S1 C15 C16 S2 -48.5(10) . . . . ? C17 S2 C16 C15 -64.9(9) . . . . ? Ru S2 C16 C15 44.7(8) . . . . ? C16 S2 C17 C18 135.1(8) . . . . ? Ru S2 C17 C18 29.7(9) . . . . ? S2 C17 C18 S3 -50.4(10) . . . . ? C19 S3 C18 C17 -65.0(9) . . . . ? Ru S3 C18 C17 44.4(8) . . . . ? C18 S3 C19 C20 132.8(8) . . . . ? Ru S3 C19 C20 26.2(8) . . . . ? S3 C19 C20 S1 -47.8(9) . . . . ? C15 S1 C20 C19 -64.7(8) . . . . ? Ru S1 C20 C19 44.2(8) . . . . ? O4 S5 C25 F3 55.1(12) . . . . ? O2 S5 C25 F3 175.7(10) . . . . ? O3 S5 C25 F3 -64.8(12) . . . . ? O4 S5 C25 F2 179.5(9) . . . . ? O2 S5 C25 F2 -60.0(11) . . . . ? O3 S5 C25 F2 59.6(10) . . . . ? O4 S5 C25 F1 -65.4(11) . . . . ? O2 S5 C25 F1 55.2(11) . . . . ? O3 S5 C25 F1 174.8(9) . . . . ? O5 S6 C26 F6 -158.9(15) . . . . ? O7 S6 C26 F6 67.0(17) . . . . ? O6 S6 C26 F6 -40.9(17) . . . . ? O5 S6 C26 F5 54.1(17) . . . . ? O7 S6 C26 F5 -80.0(16) . . . . ? O6 S6 C26 F5 172.1(15) . . . . ? O5 S6 C26 F4 -51.9(17) . . . . ? O7 S6 C26 F4 174.0(14) . . . . ? O6 S6 C26 F4 66.1(15) . . . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 1.097 _refine_diff_density_min -0.897 _refine_diff_density_rms 0.132 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 805603' #TrackingRef '- data.cif' _vrf_PLAT306_4 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W RESPONSE: Residual interpreted as lattice water (O1w) with H atoms not located ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Cl N4 Ru S3 1+, C F3 O3 S 1-, H2 O' _chemical_formula_sum 'C21 H26 Cl F3 N4 O4 Ru S4' _chemical_formula_weight 720.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' F F 0.0171 0.0103 '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 8.276(3) _cell_length_b 13.690(4) _cell_length_c 14.262(4) _cell_angle_alpha 86.21(3) _cell_angle_beta 73.46(2) _cell_angle_gamma 71.34(2) _cell_volume 1467.0(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 needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.8028 _exptl_absorpt_correction_T_max 0.8536 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Linear fit to sin(theta)/lambda - 12 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21726 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.08 _reflns_number_total 5825 _reflns_number_gt 2755 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1153P)^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 5825 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1840 _refine_ls_wR_factor_gt 0.1655 _refine_ls_goodness_of_fit_ref 0.860 _refine_ls_restrained_S_all 0.860 _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 0.37636(7) 0.33501(4) 0.74834(4) 0.0799(2) Uani 1 1 d . . . S1 S 0.5024(3) 0.18854(14) 0.65184(13) 0.0920(5) Uani 1 1 d . . . S2 S 0.3985(3) 0.42898(14) 0.60914(13) 0.0905(5) Uani 1 1 d . . . S3 S 0.1052(2) 0.33357(14) 0.74147(13) 0.0864(5) Uani 1 1 d . . . Cl1 Cl 0.6736(2) 0.33779(15) 0.73982(15) 0.0998(5) Uani 1 1 d . . . N1 N 0.2685(7) 0.4675(4) 0.8464(4) 0.0811(13) Uani 1 1 d . . . N2 N 0.3534(7) 0.2459(4) 0.8751(4) 0.0786(13) Uani 1 1 d . . . N3 N 0.3672(7) 0.2726(4) 0.9594(4) 0.0840(14) Uani 1 1 d . . . N4 N 0.3164(7) 0.1595(4) 0.8842(4) 0.0832(14) Uani 1 1 d . . . C1 C 0.1730(9) 0.5590(5) 0.8209(5) 0.0899(18) Uani 1 1 d . . . H1 H 0.1654 0.5657 0.7569 0.108 Uiso 1 1 calc R . . C2 C 0.0852(10) 0.6439(5) 0.8836(6) 0.096(2) Uani 1 1 d . . . H2 H 0.0193 0.7054 0.8622 0.115 Uiso 1 1 calc R . . C3 C 0.0970(10) 0.6360(6) 0.9779(6) 0.101(2) Uani 1 1 d . . . H3 H 0.0363 0.6910 1.0227 0.121 Uiso 1 1 calc R . . C4 C 0.2031(10) 0.5426(5) 1.0048(5) 0.0943(19) Uani 1 1 d . . . H4 H 0.2168 0.5357 1.0676 0.113 Uiso 1 1 calc R . . C5 C 0.2871(9) 0.4610(5) 0.9387(5) 0.0854(17) Uani 1 1 d . . . C6 C 0.4136(10) 0.3657(5) 0.9671(5) 0.0915(19) Uani 1 1 d . . . H6A H 0.5326 0.3571 0.9251 0.110 Uiso 1 1 calc R . . H6B H 0.4142 0.3746 1.0339 0.110 Uiso 1 1 calc R . . C7 C 0.3392(9) 0.2010(5) 1.0249(5) 0.0854(17) Uani 1 1 d . . . H7 H 0.3425 0.2002 1.0896 0.103 Uiso 1 1 calc R . . C8 C 0.3054(8) 0.1305(5) 0.9785(5) 0.0814(16) Uani 1 1 d . . . C9 C 0.2664(9) 0.0337(5) 1.0124(5) 0.0841(17) Uani 1 1 d . . . C10 C 0.2378(11) 0.0125(6) 1.1126(5) 0.101(2) Uani 1 1 d . . . H10 H 0.2416 0.0588 1.1562 0.122 Uiso 1 1 calc R . . C11 C 0.2038(12) -0.0789(6) 1.1452(6) 0.111(2) Uani 1 1 d . . . H11 H 0.1940 -0.0961 1.2103 0.134 Uiso 1 1 calc R . . C12 C 0.1846(10) -0.1432(6) 1.0841(6) 0.099(2) Uani 1 1 d . . . H12 H 0.1542 -0.2018 1.1075 0.119 Uiso 1 1 calc R . . C13 C 0.2109(11) -0.1201(6) 0.9858(6) 0.111(2) Uani 1 1 d . . . H13 H 0.2021 -0.1651 0.9429 0.134 Uiso 1 1 calc R . . C14 C 0.2498(9) -0.0319(5) 0.9507(5) 0.0934(19) Uani 1 1 d . . . H14 H 0.2648 -0.0170 0.8848 0.112 Uiso 1 1 calc R . . C15 C 0.5424(12) 0.2306(6) 0.5247(5) 0.114(3) Uani 1 1 d . . . H15A H 0.6491 0.1818 0.4845 0.137 Uiso 1 1 calc R . . H15B H 0.4438 0.2315 0.5004 0.137 Uiso 1 1 calc R . . C16 C 0.5633(11) 0.3367(6) 0.5163(5) 0.108(2) Uani 1 1 d . . . H16A H 0.5555 0.3627 0.4522 0.129 Uiso 1 1 calc R . . H16B H 0.6806 0.3311 0.5209 0.129 Uiso 1 1 calc R . . C17 C 0.1942(10) 0.4444(6) 0.5731(5) 0.098(2) Uani 1 1 d . . . H17A H 0.1583 0.5118 0.5453 0.118 Uiso 1 1 calc R . . H17B H 0.2203 0.3929 0.5227 0.118 Uiso 1 1 calc R . . C18 C 0.0435(10) 0.4340(6) 0.6560(6) 0.102(2) Uani 1 1 d . . . H18A H -0.0425 0.4198 0.6294 0.123 Uiso 1 1 calc R . . H18B H -0.0143 0.4994 0.6919 0.123 Uiso 1 1 calc R . . C19 C 0.1478(11) 0.2202(6) 0.6662(6) 0.105(2) Uani 1 1 d . . . H19A H 0.0531 0.1903 0.6927 0.126 Uiso 1 1 calc R . . H19B H 0.1437 0.2423 0.6007 0.126 Uiso 1 1 calc R . . C20 C 0.3198(12) 0.1393(6) 0.6597(6) 0.110(2) Uani 1 1 d . . . H20A H 0.3499 0.0955 0.6026 0.132 Uiso 1 1 calc R . . H20B H 0.3062 0.0969 0.7168 0.132 Uiso 1 1 calc R . . S4 S 0.1294(5) 0.2433(2) 0.3573(2) 0.1441(10) Uani 1 1 d . . . O1 O 0.2136(18) 0.2222(11) 0.2635(6) 0.285(7) Uani 1 1 d . . . O2 O -0.053(2) 0.2788(11) 0.3524(11) 0.315(8) Uani 1 1 d . . . O3 O 0.150(2) 0.2913(7) 0.4213(7) 0.321(9) Uani 1 1 d . . . C21 C 0.121(3) 0.1161(11) 0.4062(12) 0.212(8) Uani 1 1 d . . . F1 F 0.109(2) 0.0568(8) 0.3614(7) 0.291(7) Uani 1 1 d . . . F2 F 0.2717(15) 0.0779(7) 0.4362(8) 0.261(5) Uani 1 1 d . . . F3 F 0.0106(15) 0.1319(7) 0.4986(7) 0.241(5) Uani 1 1 d . . . O1W O 0.3886(10) 0.4257(6) 1.1954(5) 0.166(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0886(4) 0.0741(3) 0.0845(4) 0.0108(2) -0.0307(3) -0.0317(3) S1 0.1059(13) 0.0815(11) 0.0895(11) 0.0062(9) -0.0283(10) -0.0306(9) S2 0.1047(12) 0.0846(11) 0.0906(11) 0.0180(9) -0.0326(10) -0.0395(9) S3 0.0933(11) 0.0893(11) 0.0881(11) 0.0114(9) -0.0348(9) -0.0377(9) Cl1 0.0876(11) 0.1037(12) 0.1181(13) 0.0163(10) -0.0362(10) -0.0394(9) N1 0.087(3) 0.074(3) 0.088(4) 0.008(3) -0.030(3) -0.030(3) N2 0.090(3) 0.072(3) 0.081(3) 0.010(3) -0.030(3) -0.032(3) N3 0.102(4) 0.078(3) 0.083(3) 0.010(3) -0.041(3) -0.032(3) N4 0.094(4) 0.074(3) 0.089(4) 0.013(3) -0.032(3) -0.033(3) C1 0.094(5) 0.082(4) 0.099(5) 0.019(4) -0.035(4) -0.030(4) C2 0.106(5) 0.074(4) 0.106(5) 0.003(4) -0.036(4) -0.022(4) C3 0.108(5) 0.082(5) 0.112(6) -0.003(4) -0.022(4) -0.035(4) C4 0.105(5) 0.089(5) 0.101(5) -0.002(4) -0.037(4) -0.038(4) C5 0.094(4) 0.080(4) 0.096(5) 0.007(4) -0.033(4) -0.040(4) C6 0.109(5) 0.083(4) 0.099(5) 0.010(4) -0.047(4) -0.038(4) C7 0.100(5) 0.084(4) 0.080(4) 0.014(3) -0.034(4) -0.033(4) C8 0.089(4) 0.076(4) 0.082(4) 0.014(3) -0.028(3) -0.027(3) C9 0.092(4) 0.074(4) 0.091(4) 0.014(3) -0.033(4) -0.029(3) C10 0.136(6) 0.097(5) 0.084(5) 0.014(4) -0.032(4) -0.054(5) C11 0.148(7) 0.104(6) 0.102(5) 0.029(5) -0.050(5) -0.058(5) C12 0.118(6) 0.088(5) 0.102(5) 0.026(4) -0.038(4) -0.043(4) C13 0.145(7) 0.085(5) 0.126(6) 0.006(5) -0.059(5) -0.047(5) C14 0.118(5) 0.078(4) 0.096(5) 0.013(4) -0.040(4) -0.040(4) C15 0.126(6) 0.107(6) 0.091(5) 0.003(4) -0.001(4) -0.039(5) C16 0.110(6) 0.111(6) 0.084(5) 0.009(4) 0.000(4) -0.036(4) C17 0.110(5) 0.106(5) 0.090(5) 0.020(4) -0.042(4) -0.040(4) C18 0.103(5) 0.103(5) 0.118(6) 0.027(4) -0.055(5) -0.041(4) C19 0.133(6) 0.101(5) 0.106(5) 0.004(4) -0.050(5) -0.053(5) C20 0.153(7) 0.085(5) 0.115(6) -0.001(4) -0.056(5) -0.051(5) S4 0.182(3) 0.1248(19) 0.1060(18) 0.0074(14) -0.0476(18) -0.0163(18) O1 0.377(17) 0.443(18) 0.112(6) -0.015(8) -0.003(8) -0.288(16) O2 0.323(18) 0.275(15) 0.286(15) 0.110(12) -0.110(13) -0.012(12) O3 0.72(3) 0.162(7) 0.202(9) 0.017(7) -0.290(14) -0.155(12) C21 0.36(2) 0.127(10) 0.137(12) -0.007(8) -0.122(14) -0.015(12) F1 0.58(2) 0.188(8) 0.170(7) 0.007(6) -0.167(10) -0.153(10) F2 0.292(12) 0.178(7) 0.249(9) 0.011(7) -0.116(9) 0.047(7) F3 0.357(15) 0.221(9) 0.148(6) 0.026(6) -0.065(7) -0.105(9) O1W 0.170(6) 0.185(7) 0.147(5) -0.031(5) -0.034(5) -0.063(5) _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 N2 2.110(5) . ? Ru N1 2.152(5) . ? Ru S3 2.2801(19) . ? Ru S1 2.283(2) . ? Ru S2 2.2883(19) . ? Ru Cl1 2.441(2) . ? S1 C20 1.815(8) . ? S1 C15 1.836(7) . ? S2 C16 1.817(8) . ? S2 C17 1.849(7) . ? S3 C18 1.822(7) . ? S3 C19 1.827(7) . ? N1 C1 1.340(8) . ? N1 C5 1.362(8) . ? N2 N4 1.303(6) . ? N2 N3 1.325(7) . ? N3 C7 1.337(7) . ? N3 C6 1.462(8) . ? N4 C8 1.364(8) . ? C1 C2 1.381(10) . ? C2 C3 1.371(10) . ? C3 C4 1.401(10) . ? C4 C5 1.374(9) . ? C5 C6 1.503(9) . ? C7 C8 1.346(9) . ? C8 C9 1.481(8) . ? C9 C14 1.361(9) . ? C9 C10 1.406(9) . ? C10 C11 1.391(10) . ? C11 C12 1.353(10) . ? C12 C13 1.386(10) . ? C13 C14 1.374(9) . ? C15 C16 1.510(10) . ? C17 C18 1.492(10) . ? C19 C20 1.480(11) . ? S4 O3 1.240(7) . ? S4 O1 1.323(9) . ? S4 O2 1.455(15) . ? S4 C21 1.848(16) . ? C21 F1 1.108(15) . ? C21 F3 1.358(19) . ? C21 F2 1.37(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 N2 Ru N1 86.3(2) . . ? N2 Ru S3 89.93(14) . . ? N1 Ru S3 94.07(14) . . ? N2 Ru S1 90.51(15) . . ? N1 Ru S1 175.87(15) . . ? S3 Ru S1 88.54(7) . . ? N2 Ru S2 178.53(15) . . ? N1 Ru S2 94.78(15) . . ? S3 Ru S2 89.00(7) . . ? S1 Ru S2 88.46(7) . . ? N2 Ru Cl1 94.55(14) . . ? N1 Ru Cl1 88.70(14) . . ? S3 Ru Cl1 174.88(6) . . ? S1 Ru Cl1 88.94(7) . . ? S2 Ru Cl1 86.48(7) . . ? C20 S1 C15 99.8(4) . . ? C20 S1 Ru 104.5(3) . . ? C15 S1 Ru 106.4(3) . . ? C16 S2 C17 101.2(4) . . ? C16 S2 Ru 103.3(3) . . ? C17 S2 Ru 105.9(2) . . ? C18 S3 C19 99.3(4) . . ? C18 S3 Ru 104.5(2) . . ? C19 S3 Ru 105.9(3) . . ? C1 N1 C5 117.0(6) . . ? C1 N1 Ru 121.4(5) . . ? C5 N1 Ru 121.5(4) . . ? N4 N2 N3 109.7(5) . . ? N4 N2 Ru 125.8(4) . . ? N3 N2 Ru 124.4(4) . . ? N2 N3 C7 108.8(5) . . ? N2 N3 C6 120.1(5) . . ? C7 N3 C6 131.1(6) . . ? N2 N4 C8 106.9(5) . . ? N1 C1 C2 124.2(7) . . ? C3 C2 C1 118.8(7) . . ? C2 C3 C4 117.9(7) . . ? C5 C4 C3 120.3(7) . . ? N1 C5 C4 121.6(6) . . ? N1 C5 C6 119.6(6) . . ? C4 C5 C6 118.7(6) . . ? N3 C6 C5 112.7(5) . . ? N3 C7 C8 106.3(6) . . ? C7 C8 N4 108.3(6) . . ? C7 C8 C9 131.4(6) . . ? N4 C8 C9 120.3(6) . . ? C14 C9 C10 119.7(6) . . ? C14 C9 C8 122.1(6) . . ? C10 C9 C8 118.2(6) . . ? C11 C10 C9 118.8(7) . . ? C12 C11 C10 121.3(7) . . ? C11 C12 C13 118.8(7) . . ? C14 C13 C12 121.3(7) . . ? C9 C14 C13 120.0(7) . . ? C16 C15 S1 111.6(6) . . ? C15 C16 S2 113.7(5) . . ? C18 C17 S2 113.5(5) . . ? C17 C18 S3 114.9(5) . . ? C20 C19 S3 114.8(5) . . ? C19 C20 S1 114.3(5) . . ? O3 S4 O1 133.2(9) . . ? O3 S4 O2 111.7(10) . . ? O1 S4 O2 99.9(8) . . ? O3 S4 C21 107.5(7) . . ? O1 S4 C21 103.1(8) . . ? O2 S4 C21 94.8(10) . . ? F1 C21 F3 116(2) . . ? F1 C21 F2 109.9(16) . . ? F3 C21 F2 94.1(11) . . ? F1 C21 S4 121.7(12) . . ? F3 C21 S4 107.6(10) . . ? F2 C21 S4 103.9(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru S1 C20 73.1(3) . . . . ? N1 Ru S1 C20 112.5(19) . . . . ? S3 Ru S1 C20 -16.8(3) . . . . ? S2 Ru S1 C20 -105.9(3) . . . . ? Cl1 Ru S1 C20 167.6(3) . . . . ? N2 Ru S1 C15 178.2(3) . . . . ? N1 Ru S1 C15 -142.4(19) . . . . ? S3 Ru S1 C15 88.2(3) . . . . ? S2 Ru S1 C15 -0.8(3) . . . . ? Cl1 Ru S1 C15 -87.3(3) . . . . ? N2 Ru S2 C16 -64(6) . . . . ? N1 Ru S2 C16 158.6(3) . . . . ? S3 Ru S2 C16 -107.4(3) . . . . ? S1 Ru S2 C16 -18.9(3) . . . . ? Cl1 Ru S2 C16 70.2(3) . . . . ? N2 Ru S2 C17 42(6) . . . . ? N1 Ru S2 C17 -95.5(3) . . . . ? S3 Ru S2 C17 -1.5(3) . . . . ? S1 Ru S2 C17 87.1(3) . . . . ? Cl1 Ru S2 C17 176.1(3) . . . . ? N2 Ru S3 C18 165.4(3) . . . . ? N1 Ru S3 C18 79.2(3) . . . . ? S1 Ru S3 C18 -104.0(3) . . . . ? S2 Ru S3 C18 -15.6(3) . . . . ? Cl1 Ru S3 C18 -43.5(8) . . . . ? N2 Ru S3 C19 -90.3(3) . . . . ? N1 Ru S3 C19 -176.6(3) . . . . ? S1 Ru S3 C19 0.2(3) . . . . ? S2 Ru S3 C19 88.7(3) . . . . ? Cl1 Ru S3 C19 60.8(8) . . . . ? N2 Ru N1 C1 -151.0(5) . . . . ? S3 Ru N1 C1 -61.3(5) . . . . ? S1 Ru N1 C1 169.5(16) . . . . ? S2 Ru N1 C1 28.0(5) . . . . ? Cl1 Ru N1 C1 114.4(5) . . . . ? N2 Ru N1 C5 25.9(5) . . . . ? S3 Ru N1 C5 115.6(5) . . . . ? S1 Ru N1 C5 -14(2) . . . . ? S2 Ru N1 C5 -155.1(4) . . . . ? Cl1 Ru N1 C5 -68.7(5) . . . . ? N1 Ru N2 N4 146.2(5) . . . . ? S3 Ru N2 N4 52.1(5) . . . . ? S1 Ru N2 N4 -36.5(5) . . . . ? S2 Ru N2 N4 9(6) . . . . ? Cl1 Ru N2 N4 -125.4(5) . . . . ? N1 Ru N2 N3 -30.7(5) . . . . ? S3 Ru N2 N3 -124.8(5) . . . . ? S1 Ru N2 N3 146.7(5) . . . . ? S2 Ru N2 N3 -168(5) . . . . ? Cl1 Ru N2 N3 57.7(5) . . . . ? N4 N2 N3 C7 0.4(7) . . . . ? Ru N2 N3 C7 177.6(4) . . . . ? N4 N2 N3 C6 178.1(5) . . . . ? Ru N2 N3 C6 -4.6(8) . . . . ? N3 N2 N4 C8 0.3(7) . . . . ? Ru N2 N4 C8 -176.9(4) . . . . ? C5 N1 C1 C2 -3.9(10) . . . . ? Ru N1 C1 C2 173.1(5) . . . . ? N1 C1 C2 C3 0.9(11) . . . . ? C1 C2 C3 C4 2.1(11) . . . . ? C2 C3 C4 C5 -2.2(11) . . . . ? C1 N1 C5 C4 3.8(9) . . . . ? Ru N1 C5 C4 -173.2(5) . . . . ? C1 N1 C5 C6 -171.2(6) . . . . ? Ru N1 C5 C6 11.8(8) . . . . ? C3 C4 C5 N1 -0.9(10) . . . . ? C3 C4 C5 C6 174.2(6) . . . . ? N2 N3 C6 C5 57.0(8) . . . . ? C7 N3 C6 C5 -125.8(7) . . . . ? N1 C5 C6 N3 -60.8(8) . . . . ? C4 C5 C6 N3 124.0(7) . . . . ? N2 N3 C7 C8 -0.9(7) . . . . ? C6 N3 C7 C8 -178.3(6) . . . . ? N3 C7 C8 N4 1.0(7) . . . . ? N3 C7 C8 C9 179.3(7) . . . . ? N2 N4 C8 C7 -0.8(7) . . . . ? N2 N4 C8 C9 -179.3(5) . . . . ? C7 C8 C9 C14 -174.5(7) . . . . ? N4 C8 C9 C14 3.6(10) . . . . ? C7 C8 C9 C10 8.5(11) . . . . ? N4 C8 C9 C10 -173.4(6) . . . . ? C14 C9 C10 C11 3.9(11) . . . . ? C8 C9 C10 C11 -179.0(7) . . . . ? C9 C10 C11 C12 -5.1(13) . . . . ? C10 C11 C12 C13 4.2(13) . . . . ? C11 C12 C13 C14 -2.3(12) . . . . ? C10 C9 C14 C13 -2.1(11) . . . . ? C8 C9 C14 C13 -179.0(7) . . . . ? C12 C13 C14 C9 1.2(12) . . . . ? C20 S1 C15 C16 134.1(6) . . . . ? Ru S1 C15 C16 25.7(7) . . . . ? S1 C15 C16 S2 -45.0(8) . . . . ? C17 S2 C16 C15 -68.1(7) . . . . ? Ru S2 C16 C15 41.4(7) . . . . ? C16 S2 C17 C18 130.8(6) . . . . ? Ru S2 C17 C18 23.3(6) . . . . ? S2 C17 C18 S3 -39.4(8) . . . . ? C19 S3 C18 C17 -73.8(6) . . . . ? Ru S3 C18 C17 35.4(6) . . . . ? C18 S3 C19 C20 129.8(6) . . . . ? Ru S3 C19 C20 21.7(7) . . . . ? S3 C19 C20 S1 -38.5(8) . . . . ? C15 S1 C20 C19 -74.4(7) . . . . ? Ru S1 C20 C19 35.6(6) . . . . ? O3 S4 C21 F1 -177(2) . . . . ? O1 S4 C21 F1 -33(3) . . . . ? O2 S4 C21 F1 68(2) . . . . ? O3 S4 C21 F3 46.2(18) . . . . ? O1 S4 C21 F3 -169.7(14) . . . . ? O2 S4 C21 F3 -68.4(16) . . . . ? O3 S4 C21 F2 -52.8(15) . . . . ? O1 S4 C21 F2 91.3(12) . . . . ? O2 S4 C21 F2 -167.3(12) . . . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.760 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.090 #===END