# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Enzo Alessio' _publ_contact_author_email alessi@units.it _publ_author_name 'Enzo Alessio' data_4 _database_code_depnum_ccdc_archive 'CCDC 872717' #TrackingRef '- CIF Rev1 DT-ART-03-2012-030654.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Cl N2 Ru S3 1+, P F6' _chemical_formula_sum 'C8 H20 Cl F6 N2 P Ru S3' _chemical_formula_weight 521.93 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nma' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 9.1900(18) _cell_length_b 8.244(2) _cell_length_c 23.527(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1782.5(6) _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 block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 1.521 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5153 _exptl_absorpt_correction_T_max 0.7571 _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 'Enraf-Nonius dip1030 image plate diffractometer' _diffrn_measurement_method '\f-scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23344 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 26.37 _reflns_number_total 1931 _reflns_number_gt 1485 _reflns_threshold_expression >2\s(I) _computing_data_collection 'XPRESS (MacScience, 2002)' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.80.05 (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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0697P)^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 1931 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 0.45257(4) 0.2500 -0.586473(19) 0.0499(2) Uani 1 2 d S . . Cl1 Cl 0.55161(17) 0.2500 -0.49094(7) 0.0687(4) Uani 1 2 d S . . S1 S 0.36788(19) 0.2500 -0.67690(7) 0.0743(5) Uani 1 2 d S . . S2 S 0.61798(12) 0.05676(14) -0.61170(6) 0.0703(3) Uani 1 1 d . . . C1 C 0.5693(10) -0.0024(14) -0.6822(4) 0.195(6) Uani 1 1 d . . . H1A H 0.6562 0.0062 -0.7054 0.233 Uiso 1 1 calc R . . H1B H 0.5436 -0.1165 -0.6809 0.233 Uiso 1 1 calc R . . C2 C 0.4578(7) 0.0778(9) -0.7111(3) 0.113(2) Uani 1 1 d . . . H2A H 0.3835 -0.0018 -0.7200 0.135 Uiso 1 1 calc R . . H2B H 0.4972 0.1157 -0.7470 0.135 Uiso 1 1 calc R . . C3 C 0.7825(5) 0.1667(8) -0.6253(4) 0.134(3) Uani 1 1 d . . . H3A H 0.8535 0.1319 -0.5974 0.161 Uiso 1 1 calc R . . H3B H 0.8184 0.1319 -0.6621 0.161 Uiso 1 1 calc R . . N1 N 0.2934(3) 0.0822(4) -0.55490(16) 0.0610(8) Uani 1 1 d . . . H11A H 0.2756 0.0046 -0.5809 0.073 Uiso 0.50 1 calc PR A 1 H12A H 0.3257 0.0345 -0.5229 0.073 Uiso 0.50 1 calc PR A 1 H13B H 0.2460 0.0367 -0.5843 0.073 Uiso 0.50 1 calc PR A 2 H14B H 0.3384 0.0026 -0.5355 0.073 Uiso 0.50 1 calc PR A 2 C4A C 0.1560(16) 0.179(2) -0.5429(8) 0.078(4) Uani 0.50 1 d P . 1 H15A H 0.0839 0.1444 -0.5705 0.093 Uiso 0.50 1 calc PR . 1 H16B H 0.1208 0.1444 -0.5060 0.093 Uiso 0.50 1 calc PR . 1 C4B C 0.1931(16) 0.160(2) -0.5192(8) 0.079(4) Uani 0.50 1 d P . 2 H17A H 0.2108 0.1240 -0.4806 0.094 Uiso 0.50 1 calc PR . 2 H18A H 0.0964 0.1240 -0.5297 0.094 Uiso 0.50 1 calc PR . 2 P1 P 0.9269(2) 0.2500 -0.34566(8) 0.0708(5) Uani 1 2 d S . . F1 F 0.8522(9) 0.2500 -0.2854(3) 0.176(3) Uani 1 2 d S . . F2 F 0.7684(6) 0.2500 -0.3720(3) 0.1239(19) Uani 1 2 d S . . F3 F 0.9207(5) 0.0593(4) -0.3435(2) 0.1451(17) Uani 1 1 d . . . F4 F 1.0760(8) 0.2500 -0.3169(5) 0.219(5) Uani 1 2 d S . . F5 F 0.9861(12) 0.2500 -0.4033(4) 0.258(6) Uani 1 2 d S . . 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 0.0494(3) 0.0434(3) 0.0569(3) 0.000 -0.00101(18) 0.000 Cl1 0.0800(9) 0.0581(9) 0.0681(10) 0.000 -0.0186(7) 0.000 S1 0.0731(9) 0.0916(12) 0.0583(10) 0.000 -0.0071(7) 0.000 S2 0.0638(6) 0.0565(6) 0.0906(9) -0.0066(6) 0.0072(6) 0.0086(5) C1 0.175(8) 0.242(11) 0.167(8) -0.142(8) -0.071(6) 0.116(8) C2 0.150(6) 0.109(5) 0.080(4) -0.034(4) -0.011(4) 0.009(4) C3 0.060(3) 0.093(4) 0.249(9) 0.016(5) 0.037(4) 0.015(3) N1 0.0604(18) 0.0515(19) 0.071(2) 0.0030(16) -0.0009(16) -0.0075(15) C4A 0.052(6) 0.059(7) 0.121(15) 0.007(8) 0.015(7) 0.005(5) C4B 0.063(8) 0.070(6) 0.103(13) 0.032(8) 0.028(7) 0.012(7) P1 0.0717(10) 0.0651(10) 0.0756(12) 0.000 -0.0147(8) 0.000 F1 0.278(9) 0.155(6) 0.096(4) 0.000 0.017(5) 0.000 F2 0.104(3) 0.101(4) 0.167(5) 0.000 -0.053(3) 0.000 F3 0.151(3) 0.069(2) 0.216(5) -0.021(3) -0.054(3) 0.021(2) F4 0.125(5) 0.149(6) 0.382(13) 0.000 -0.141(7) 0.000 F5 0.259(9) 0.367(18) 0.147(8) 0.000 0.115(8) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N1 2.146(3) 8_565 ? Ru N1 2.146(3) . ? Ru S1 2.2653(17) . ? Ru S2 2.2805(12) 8_565 ? Ru S2 2.2805(12) . ? Ru Cl1 2.4249(16) . ? S1 C2 1.829(6) . ? S1 C2 1.829(6) 8_565 ? S2 C1 1.786(7) . ? S2 C3 1.792(5) . ? C1 C2 1.396(10) . ? C3 C3 1.373(13) 8_565 ? N1 C4B 1.40(2) . ? N1 C4A 1.519(17) . ? C4A C4A 1.18(3) 8_565 ? C4B C4B 1.48(4) 8_565 ? P1 F5 1.462(7) . ? P1 F4 1.528(6) . ? P1 F3 1.574(4) . ? P1 F3 1.574(4) 8_565 ? P1 F1 1.575(7) . ? P1 F2 1.582(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru N1 80.30(18) 8_565 . ? N1 Ru S1 95.22(11) 8_565 . ? N1 Ru S1 95.22(11) . . ? N1 Ru S2 95.39(10) 8_565 8_565 ? N1 Ru S2 174.13(10) . 8_565 ? S1 Ru S2 89.12(5) . 8_565 ? N1 Ru S2 174.13(10) 8_565 . ? N1 Ru S2 95.39(10) . . ? S1 Ru S2 89.12(5) . . ? S2 Ru S2 88.62(6) 8_565 . ? N1 Ru Cl1 86.27(11) 8_565 . ? N1 Ru Cl1 86.27(11) . . ? S1 Ru Cl1 178.05(6) . . ? S2 Ru Cl1 89.49(5) 8_565 . ? S2 Ru Cl1 89.49(5) . . ? C2 S1 C2 101.8(5) . 8_565 ? C2 S1 Ru 104.9(2) . . ? C2 S1 Ru 104.9(2) 8_565 . ? C1 S2 C3 100.6(5) . . ? C1 S2 Ru 105.4(2) . . ? C3 S2 Ru 104.8(2) . . ? C2 C1 S2 120.4(5) . . ? C1 C2 S1 119.0(5) . . ? C3 C3 S2 120.39(19) 8_565 . ? C4B N1 C4A 26.2(9) . . ? C4B N1 Ru 111.0(7) . . ? C4A N1 Ru 107.0(6) . . ? C4A C4A N1 121.6(6) 8_565 . ? N1 C4B C4B 117.3(7) . 8_565 ? F5 P1 F4 94.4(6) . . ? F5 P1 F3 92.5(2) . . ? F4 P1 F3 91.03(18) . . ? F5 P1 F3 92.5(2) . 8_565 ? F4 P1 F3 91.03(18) . 8_565 ? F3 P1 F3 174.4(5) . 8_565 ? F5 P1 F1 176.1(6) . . ? F4 P1 F1 89.6(5) . . ? F3 P1 F1 87.4(2) . . ? F3 P1 F1 87.4(2) 8_565 . ? F5 P1 F2 88.8(5) . . ? F4 P1 F2 176.8(6) . . ? F3 P1 F2 88.83(18) . . ? F3 P1 F2 88.83(18) 8_565 . ? F1 P1 F2 87.2(4) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.547 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.085 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 872718' #TrackingRef '- CIF Rev1 DT-ART-03-2012-030654.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H21 N3 Ru S3, 2(Cl)' _chemical_formula_sum 'C6 H21 Cl2 N3 Ru S3' _chemical_formula_weight 403.41 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' 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 orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 27.275(4) _cell_length_b 10.480(3) _cell_length_c 10.403(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2973.6(13) _cell_formula_units_Z 8 _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 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.811 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6709 _exptl_absorpt_correction_T_max 0.6935 _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 'Enraf-Nonius dip1030 image plate diffractometer' _diffrn_measurement_method '\f-scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33087 _diffrn_reflns_av_R_equivalents 0.0950 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3284 _reflns_number_gt 1997 _reflns_threshold_expression >2\s(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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0385P)^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 3284 _refine_ls_number_parameters 139 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 0.398141(10) 0.54384(3) 0.25674(2) 0.04006(9) Uani 1 1 d . . . S1 S 0.37096(4) 0.33827(10) 0.25312(9) 0.0507(2) Uani 1 1 d . . . S2 S 0.38338(4) 0.55412(10) 0.04121(8) 0.0482(2) Uani 1 1 d . . . S3 S 0.31921(4) 0.60782(11) 0.29126(9) 0.0490(3) Uani 1 1 d . . . N1 N 0.42432(11) 0.7404(3) 0.2646(2) 0.0489(8) Uani 1 1 d . . . H1A H 0.4398 0.7535 0.3387 0.073 Uiso 1 1 calc R . . H1B H 0.3990 0.7935 0.2586 0.073 Uiso 1 1 calc R . . H1C H 0.4448 0.7544 0.1996 0.073 Uiso 1 1 calc R . . N2 N 0.41706(12) 0.5258(3) 0.4589(3) 0.0507(8) Uani 1 1 d . . . H2A H 0.4330 0.4528 0.4715 0.076 Uiso 1 1 calc R . . H2B H 0.3898 0.5263 0.5060 0.076 Uiso 1 1 calc R . . H2C H 0.4361 0.5908 0.4821 0.076 Uiso 1 1 calc R . . N3 N 0.47434(12) 0.4907(4) 0.2221(3) 0.0624(10) Uani 1 1 d . . . H3A H 0.4883 0.4679 0.2959 0.094 Uiso 1 1 calc R . . H3B H 0.4904 0.5569 0.1889 0.094 Uiso 1 1 calc R . . H3C H 0.4754 0.4255 0.1672 0.094 Uiso 1 1 calc R . . C1 C 0.37301(17) 0.2931(4) 0.0840(4) 0.0609(11) Uani 1 1 d . . . H1D H 0.4062 0.2687 0.0618 0.073 Uiso 1 1 calc R . . H1E H 0.3521 0.2195 0.0706 0.073 Uiso 1 1 calc R . . C2 C 0.35663(16) 0.3997(4) -0.0033(4) 0.0610(12) Uani 1 1 d . . . H2D H 0.3212 0.4062 -0.0003 0.073 Uiso 1 1 calc R . . H2E H 0.3659 0.3795 -0.0910 0.073 Uiso 1 1 calc R . . C3 C 0.32942(15) 0.6523(4) 0.0293(3) 0.0567(11) Uani 1 1 d . . . H3D H 0.3391 0.7411 0.0349 0.068 Uiso 1 1 calc R . . H3E H 0.3146 0.6392 -0.0545 0.068 Uiso 1 1 calc R . . C4 C 0.29165(14) 0.6257(4) 0.1311(3) 0.0572(11) Uani 1 1 d . . . H4A H 0.2741 0.5482 0.1093 0.069 Uiso 1 1 calc R . . H4B H 0.2682 0.6952 0.1330 0.069 Uiso 1 1 calc R . . C5 C 0.28890(14) 0.4641(4) 0.3470(3) 0.0590(12) Uani 1 1 d . . . H5A H 0.2957 0.4529 0.4378 0.071 Uiso 1 1 calc R . . H5B H 0.2538 0.4744 0.3373 0.071 Uiso 1 1 calc R . . C6 C 0.30468(15) 0.3460(4) 0.2759(4) 0.0596(12) Uani 1 1 d . . . H6A H 0.2887 0.3442 0.1926 0.072 Uiso 1 1 calc R . . H6B H 0.2940 0.2713 0.3235 0.072 Uiso 1 1 calc R . . Cl1 Cl 0.32938(4) 0.96222(11) 0.18323(9) 0.0591(3) Uani 1 1 d . . . Cl2 Cl 0.50450(4) 0.75964(11) 0.02189(9) 0.0611(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 0.04056(16) 0.03929(17) 0.04034(16) 0.00128(13) -0.00040(12) -0.00205(13) S1 0.0551(6) 0.0396(6) 0.0574(6) 0.0061(5) -0.0053(5) -0.0047(4) S2 0.0575(6) 0.0475(7) 0.0396(5) 0.0001(4) 0.0034(4) -0.0050(5) S3 0.0456(6) 0.0547(7) 0.0468(5) -0.0072(4) -0.0004(4) 0.0041(5) N1 0.051(2) 0.043(2) 0.0528(17) -0.0007(15) -0.0005(14) -0.0077(15) N2 0.050(2) 0.056(3) 0.0468(17) 0.0058(15) -0.0024(14) -0.0088(16) N3 0.042(2) 0.065(3) 0.080(2) 0.0042(19) 0.0016(16) 0.0058(17) C1 0.071(3) 0.041(3) 0.070(3) -0.010(2) 0.001(2) 0.001(2) C2 0.089(4) 0.045(3) 0.049(2) -0.0085(19) -0.003(2) -0.003(2) C3 0.072(3) 0.052(3) 0.047(2) 0.0059(18) -0.0138(19) 0.002(2) C4 0.052(3) 0.063(3) 0.057(2) 0.001(2) -0.0094(18) 0.012(2) C5 0.042(2) 0.086(4) 0.048(2) 0.004(2) 0.0025(17) -0.008(2) C6 0.057(3) 0.060(3) 0.062(2) 0.009(2) -0.0044(19) -0.026(2) Cl1 0.0648(7) 0.0598(8) 0.0528(5) 0.0007(5) 0.0057(5) 0.0038(5) Cl2 0.0521(6) 0.0656(8) 0.0655(6) 0.0013(5) 0.0003(4) 0.0014(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.174(3) . ? Ru N1 2.182(3) . ? Ru N3 2.182(3) . ? Ru S1 2.2788(12) . ? Ru S2 2.2806(11) . ? Ru S3 2.2834(11) . ? S1 C1 1.822(4) . ? S1 C6 1.825(4) . ? S2 C3 1.800(4) . ? S2 C2 1.834(4) . ? S3 C5 1.814(4) . ? S3 C4 1.837(4) . ? C1 C2 1.508(5) . ? C3 C4 1.504(5) . ? C5 C6 1.504(6) . ? 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 88.20(11) . . ? N2 Ru N3 84.93(13) . . ? N1 Ru N3 86.31(13) . . ? N2 Ru S1 90.62(9) . . ? N1 Ru S1 178.80(7) . . ? N3 Ru S1 93.77(11) . . ? N2 Ru S2 175.74(9) . . ? N1 Ru S2 92.86(7) . . ? N3 Ru S2 91.01(9) . . ? S1 Ru S2 88.34(4) . . ? N2 Ru S3 95.58(9) . . ? N1 Ru S3 91.46(9) . . ? N3 Ru S3 177.70(11) . . ? S1 Ru S3 88.48(4) . . ? S2 Ru S3 88.53(4) . . ? C1 S1 C6 99.63(19) . . ? C1 S1 Ru 104.57(14) . . ? C6 S1 Ru 106.16(15) . . ? C3 S2 C2 99.3(2) . . ? C3 S2 Ru 103.83(12) . . ? C2 S2 Ru 106.07(13) . . ? C5 S3 C4 100.85(19) . . ? C5 S3 Ru 103.65(15) . . ? C4 S3 Ru 105.85(13) . . ? C2 C1 S1 112.3(3) . . ? C1 C2 S2 112.6(3) . . ? C4 C3 S2 114.0(3) . . ? C3 C4 S3 112.2(3) . . ? C6 C5 S3 113.3(3) . . ? C5 C6 S1 112.5(3) . . ? 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 C1 -158.62(18) . . . . ? N1 Ru S1 C1 -167(15) . . . . ? N3 Ru S1 C1 -73.66(17) . . . . ? S2 Ru S1 C1 17.25(15) . . . . ? S3 Ru S1 C1 105.82(15) . . . . ? N2 Ru S1 C6 96.59(15) . . . . ? N1 Ru S1 C6 88(4) . . . . ? N3 Ru S1 C6 -178.45(15) . . . . ? S2 Ru S1 C6 -87.54(13) . . . . ? S3 Ru S1 C6 1.03(13) . . . . ? N2 Ru S2 C3 -177(15) . . . . ? N1 Ru S2 C3 -73.14(18) . . . . ? N3 Ru S2 C3 -159.49(19) . . . . ? S1 Ru S2 C3 106.77(16) . . . . ? S3 Ru S2 C3 18.25(16) . . . . ? N2 Ru S2 C2 78.5(12) . . . . ? N1 Ru S2 C2 -177.26(18) . . . . ? N3 Ru S2 C2 96.38(19) . . . . ? S1 Ru S2 C2 2.64(16) . . . . ? S3 Ru S2 C2 -85.88(16) . . . . ? N2 Ru S3 C5 -72.16(15) . . . . ? N1 Ru S3 C5 -160.49(14) . . . . ? N3 Ru S3 C5 -175(2) . . . . ? S1 Ru S3 C5 18.31(13) . . . . ? S2 Ru S3 C5 106.69(13) . . . . ? N2 Ru S3 C4 -177.84(18) . . . . ? N1 Ru S3 C4 93.83(17) . . . . ? N3 Ru S3 C4 79(2) . . . . ? S1 Ru S3 C4 -87.37(16) . . . . ? S2 Ru S3 C4 1.01(16) . . . . ? C6 S1 C1 C2 70.0(4) . . . . ? Ru S1 C1 C2 -39.6(3) . . . . ? S1 C1 C2 S2 44.8(4) . . . . ? C3 S2 C2 C1 -135.1(3) . . . . ? Ru S2 C2 C1 -27.7(3) . . . . ? C2 S2 C3 C4 69.0(3) . . . . ? Ru S2 C3 C4 -40.2(3) . . . . ? S2 C3 C4 S3 44.0(4) . . . . ? C5 S3 C4 C3 -133.0(3) . . . . ? Ru S3 C4 C3 -25.3(4) . . . . ? C4 S3 C5 C6 69.3(3) . . . . ? Ru S3 C5 C6 -40.2(3) . . . . ? S3 C5 C6 S1 44.2(4) . . . . ? C1 S1 C6 C5 -134.0(3) . . . . ? Ru S1 C6 C5 -25.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.542 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.099 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 872719' #TrackingRef '- CIF Rev1 DT-ART-03-2012-030654.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H16 Cl N O2 Ru S3' _chemical_formula_sum 'C12 H16 Cl N O2 Ru S3' _chemical_formula_weight 438.96 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 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 17.524(5) _cell_length_b 14.026(3) _cell_length_c 12.357(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3037.2(13) _cell_formula_units_Z 8 _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 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.920 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 1.619 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6397 _exptl_absorpt_correction_T_max 0.8327 _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 'Enraf-Nonius dip1030 image plate diffractometer' _diffrn_measurement_method '\f-scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15177 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.09 _reflns_number_total 3309 _reflns_number_gt 1589 _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^)+(0.0521P)^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 3309 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.898 _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 0.16454(3) 0.41419(3) 0.39001(3) 0.04796(16) Uani 1 1 d . . . S1 S 0.26987(10) 0.51051(12) 0.39833(14) 0.0704(5) Uani 1 1 d . . . S2 S 0.20437(10) 0.34712(10) 0.54525(12) 0.0607(4) Uani 1 1 d . . . S3 S 0.10006(10) 0.52442(11) 0.48931(13) 0.0652(5) Uani 1 1 d . . . Cl1 Cl 0.24211(10) 0.30698(12) 0.27896(13) 0.0751(5) Uani 1 1 d . . . N1 N 0.0742(3) 0.3185(3) 0.3630(4) 0.0527(12) Uani 1 1 d . . . O1 O 0.1161(2) 0.4696(3) 0.2451(3) 0.0630(11) Uani 1 1 d . . . O2 O 0.0275(3) 0.4378(3) 0.1192(3) 0.0800(14) Uani 1 1 d . . . C1 C 0.0571(3) 0.2401(4) 0.4210(5) 0.0585(15) Uani 1 1 d . . . H1 H 0.0819 0.2296 0.4865 0.070 Uiso 1 1 calc R . . C2 C 0.0038(4) 0.1751(4) 0.3857(5) 0.0652(17) Uani 1 1 d . . . H2 H -0.0065 0.1209 0.4265 0.078 Uiso 1 1 calc R . . C3 C -0.0340(3) 0.1905(5) 0.2908(5) 0.0693(18) Uani 1 1 d . . . H3 H -0.0703 0.1470 0.2665 0.083 Uiso 1 1 calc R . . C4 C -0.0179(3) 0.2710(4) 0.2314(5) 0.0604(16) Uani 1 1 d . . . H4 H -0.0436 0.2832 0.1670 0.073 Uiso 1 1 calc R . . C5 C 0.0370(3) 0.3336(4) 0.2691(4) 0.0511(14) Uani 1 1 d . . . C6 C 0.0616(4) 0.4202(4) 0.2044(5) 0.0585(15) Uani 1 1 d . . . C8 C 0.3324(4) 0.4426(6) 0.4919(6) 0.088(2) Uani 1 1 d . . . H8A H 0.3566 0.3912 0.4522 0.105 Uiso 1 1 calc R . . H8B H 0.3723 0.4845 0.5183 0.105 Uiso 1 1 calc R . . C9 C 0.2915(4) 0.4024(5) 0.5846(6) 0.088(2) Uani 1 1 d . . . H9A H 0.2807 0.4527 0.6362 0.105 Uiso 1 1 calc R . . H9B H 0.3237 0.3557 0.6201 0.105 Uiso 1 1 calc R . . C10 C 0.1388(4) 0.3936(5) 0.6463(5) 0.084(2) Uani 1 1 d . . . H10A H 0.0931 0.3546 0.6460 0.100 Uiso 1 1 calc R . . H10B H 0.1623 0.3872 0.7170 0.100 Uiso 1 1 calc R . . C11 C 0.1170(4) 0.4915(5) 0.6310(5) 0.084(2) Uani 1 1 d . . . H11A H 0.1569 0.5321 0.6600 0.100 Uiso 1 1 calc R . . H11B H 0.0709 0.5037 0.6722 0.100 Uiso 1 1 calc R . . C12 C 0.1615(4) 0.6300(4) 0.4796(6) 0.087(2) Uani 1 1 d . . . H12A H 0.1502 0.6628 0.4124 0.105 Uiso 1 1 calc R . . H12B H 0.1490 0.6729 0.5385 0.105 Uiso 1 1 calc R . . C13 C 0.2451(5) 0.6096(4) 0.4833(5) 0.086(2) Uani 1 1 d . . . H13A H 0.2599 0.5958 0.5573 0.103 Uiso 1 1 calc R . . H13B H 0.2730 0.6657 0.4599 0.103 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 0.0557(3) 0.0484(3) 0.0397(3) -0.0011(2) -0.0029(2) -0.0064(2) S1 0.0742(12) 0.0806(11) 0.0566(10) -0.0106(8) 0.0049(9) -0.0284(9) S2 0.0791(12) 0.0558(9) 0.0470(9) -0.0017(7) -0.0120(8) 0.0048(8) S3 0.0674(11) 0.0619(10) 0.0664(11) -0.0055(7) 0.0001(9) 0.0079(8) Cl1 0.0890(13) 0.0773(10) 0.0591(11) -0.0212(8) 0.0108(9) -0.0001(9) N1 0.059(3) 0.053(3) 0.047(3) 0.001(2) -0.004(2) -0.010(2) O1 0.081(3) 0.058(3) 0.051(3) 0.0115(18) -0.016(2) -0.017(2) O2 0.098(4) 0.081(3) 0.061(3) 0.018(2) -0.028(3) -0.015(2) C1 0.070(4) 0.054(3) 0.052(4) 0.007(3) 0.003(3) -0.008(3) C2 0.074(4) 0.060(4) 0.062(4) 0.000(3) 0.006(4) -0.018(3) C3 0.058(4) 0.078(4) 0.072(5) -0.009(4) 0.006(4) -0.024(3) C4 0.053(4) 0.069(4) 0.059(4) -0.005(3) -0.011(3) -0.010(3) C5 0.055(4) 0.054(3) 0.044(3) -0.003(3) 0.000(3) 0.003(3) C6 0.072(4) 0.059(4) 0.044(3) 0.006(3) -0.008(3) -0.001(3) C8 0.048(4) 0.125(6) 0.090(6) -0.017(5) -0.018(4) -0.003(4) C9 0.091(6) 0.075(5) 0.097(6) 0.007(4) -0.023(5) 0.003(4) C10 0.124(6) 0.081(5) 0.046(4) 0.002(3) 0.014(4) 0.009(4) C11 0.096(6) 0.090(5) 0.065(5) -0.002(4) 0.024(4) 0.008(4) C12 0.111(7) 0.046(4) 0.105(6) -0.006(3) -0.032(5) 0.014(4) C13 0.112(7) 0.062(4) 0.083(5) -0.002(3) -0.006(5) -0.023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N1 2.102(4) . ? Ru O1 2.129(4) . ? Ru S2 2.2476(16) . ? Ru S3 2.2743(16) . ? Ru S1 2.2897(17) . ? Ru Cl1 2.4480(16) . ? S1 C13 1.796(7) . ? S1 C8 1.856(7) . ? S2 C9 1.780(7) . ? S2 C10 1.817(7) . ? S3 C12 1.835(7) . ? S3 C11 1.836(7) . ? N1 C1 1.347(6) . ? N1 C5 1.348(6) . ? O1 C6 1.282(6) . ? O2 C6 1.236(6) . ? C1 C2 1.376(7) . ? C2 C3 1.364(8) . ? C3 C4 1.376(8) . ? C4 C5 1.383(7) . ? C5 C6 1.517(7) . ? C8 C9 1.464(9) . ? C10 C11 1.438(8) . ? C12 C13 1.492(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 N1 Ru O1 78.41(16) . . ? N1 Ru S2 95.87(13) . . ? O1 Ru S2 174.04(12) . . ? N1 Ru S3 98.38(13) . . ? O1 Ru S3 90.43(12) . . ? S2 Ru S3 88.76(6) . . ? N1 Ru S1 172.26(13) . . ? O1 Ru S1 98.27(12) . . ? S2 Ru S1 87.61(6) . . ? S3 Ru S1 88.58(6) . . ? N1 Ru Cl1 86.37(13) . . ? O1 Ru Cl1 88.52(12) . . ? S2 Ru Cl1 92.80(6) . . ? S3 Ru Cl1 174.82(6) . . ? S1 Ru Cl1 86.56(6) . . ? C13 S1 C8 100.1(4) . . ? C13 S1 Ru 106.7(3) . . ? C8 S1 Ru 101.6(2) . . ? C9 S2 C10 101.5(4) . . ? C9 S2 Ru 108.5(2) . . ? C10 S2 Ru 103.9(2) . . ? C12 S3 C11 99.8(3) . . ? C12 S3 Ru 102.8(2) . . ? C11 S3 Ru 105.3(2) . . ? C1 N1 C5 118.6(5) . . ? C1 N1 Ru 127.2(4) . . ? C5 N1 Ru 113.7(3) . . ? C6 O1 Ru 115.4(3) . . ? N1 C1 C2 121.5(6) . . ? C3 C2 C1 119.9(6) . . ? C2 C3 C4 119.2(6) . . ? C3 C4 C5 118.9(6) . . ? N1 C5 C4 121.8(5) . . ? N1 C5 C6 116.2(5) . . ? C4 C5 C6 121.9(5) . . ? O2 C6 O1 125.9(5) . . ? O2 C6 C5 118.1(6) . . ? O1 C6 C5 116.0(5) . . ? C9 C8 S1 113.3(5) . . ? C8 C9 S2 112.0(5) . . ? C11 C10 S2 114.9(5) . . ? C10 C11 S3 114.1(5) . . ? C13 C12 S3 114.8(4) . . ? C12 C13 S1 111.6(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.09 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.574 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.100 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 872720' #TrackingRef '- CIF Rev1 DT-ART-03-2012-030654.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H27 Cl N3 O2 Ru S2, Cl, C H4 O' _chemical_formula_sum 'C11 H31 Cl2 N3 O3 Ru S2' _chemical_formula_weight 489.48 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 orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.235(3) _cell_length_b 16.651(4) _cell_length_c 29.040(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3982.0(18) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 1.278 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5627 _exptl_absorpt_correction_T_max 0.8084 _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 27106 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.87 _reflns_number_total 4570 _reflns_number_gt 2585 _reflns_threshold_expression >2\s(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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0315P)^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 4570 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.839 _refine_ls_shift/su_max 0.002 _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 0.28617(3) 0.922718(16) 0.895599(12) 0.03734(9) Uani 1 1 d . . . Cl1 Cl 0.09335(12) 0.85044(6) 0.94324(5) 0.0610(3) Uani 1 1 d . . . S1 S 0.27951(11) 0.81732(5) 0.84713(4) 0.0430(2) Uani 1 1 d . . . S2 S 0.49940(11) 0.87215(6) 0.93539(4) 0.0458(3) Uani 1 1 d . . . O1 O 0.3437(3) 0.73975(13) 0.86461(11) 0.0536(8) Uani 1 1 d . . . O2 O 0.5726(3) 0.93057(14) 0.96799(11) 0.0594(8) Uani 1 1 d . . . N1 N 0.2795(3) 1.02492(16) 0.94017(12) 0.0458(8) Uani 1 1 d . . . H1 H 0.3145 1.0100 0.9686 0.055 Uiso 1 1 calc R . . N2 N 0.0911(3) 0.98815(16) 0.86481(12) 0.0414(8) Uani 1 1 d . . . H2 H 0.0059 0.9541 0.8607 0.050 Uiso 1 1 calc R . . N3 N 0.4219(3) 1.00459(15) 0.85514(11) 0.0384(7) Uani 1 1 d . . . H3 H 0.4978 0.9767 0.8389 0.046 Uiso 1 1 calc R . . C8 C 0.0785(4) 0.7961(2) 0.82746(18) 0.0615(13) Uani 1 1 d . . . H1A H 0.0088 0.7870 0.8535 0.092 Uiso 1 1 calc R . . H1B H 0.0801 0.7490 0.8084 0.092 Uiso 1 1 calc R . . H1C H 0.0385 0.8408 0.8100 0.092 Uiso 1 1 calc R . . C7 C 0.3795(5) 0.8316(2) 0.79347(16) 0.0544(11) Uani 1 1 d . . . H2A H 0.4919 0.8437 0.7988 0.082 Uiso 1 1 calc R . . H2B H 0.3295 0.8754 0.7772 0.082 Uiso 1 1 calc R . . H2C H 0.3709 0.7835 0.7754 0.082 Uiso 1 1 calc R . . C10 C 0.4542(5) 0.7846(2) 0.96843(18) 0.0675(14) Uani 1 1 d . . . H01E H 0.3648 0.7956 0.9887 0.101 Uiso 1 1 calc R . . H01F H 0.5476 0.7697 0.9863 0.101 Uiso 1 1 calc R . . H01G H 0.4258 0.7413 0.9481 0.101 Uiso 1 1 calc R . . C9 C 0.6642(5) 0.8338(2) 0.90210(18) 0.0620(13) Uani 1 1 d . . . H02A H 0.7032 0.8748 0.8817 0.093 Uiso 1 1 calc R . . H02B H 0.6278 0.7885 0.8844 0.093 Uiso 1 1 calc R . . H02C H 0.7503 0.8173 0.9223 0.093 Uiso 1 1 calc R . . C1 C 0.1054(5) 1.0490(2) 0.94314(16) 0.0535(11) Uani 1 1 d . . . H01J H 0.0961 1.1001 0.9590 0.064 Uiso 1 1 calc R . . H01K H 0.0450 1.0091 0.9604 0.064 Uiso 1 1 calc R . . C2 C 0.0371(5) 1.0561(2) 0.89559(17) 0.0522(11) Uani 1 1 d . . . H02D H 0.0714 1.1068 0.8822 0.063 Uiso 1 1 calc R . . H02E H -0.0806 1.0565 0.8973 0.063 Uiso 1 1 calc R . . C3 C 0.1482(4) 1.0158(2) 0.81896(16) 0.0472(10) Uani 1 1 d . . . H00A H 0.0744 1.0563 0.8072 0.057 Uiso 1 1 calc R . . H00B H 0.1479 0.9709 0.7976 0.057 Uiso 1 1 calc R . . C4 C 0.3169(4) 1.0503(2) 0.82202(16) 0.0458(10) Uani 1 1 d . . . H01H H 0.3666 1.0492 0.7917 0.055 Uiso 1 1 calc R . . H01I H 0.3102 1.1059 0.8318 0.055 Uiso 1 1 calc R . . C5 C 0.5067(4) 1.0600(2) 0.88775(15) 0.0471(11) Uani 1 1 d . . . H01A H 0.5538 1.1045 0.8709 0.057 Uiso 1 1 calc R . . H01B H 0.5935 1.0316 0.9034 0.057 Uiso 1 1 calc R . . C6 C 0.3851(4) 1.0912(2) 0.92275(16) 0.0491(11) Uani 1 1 d . . . H01C H 0.4427 1.1154 0.9484 0.059 Uiso 1 1 calc R . . H01D H 0.3181 1.1322 0.9086 0.059 Uiso 1 1 calc R . . Cl2 Cl 0.75317(11) 0.95976(6) 0.80203(4) 0.0572(3) Uani 1 1 d . . . O3 O 0.3375(4) 0.64226(17) 0.72041(15) 0.0791(11) Uani 1 1 d . . . H3A H 0.3155 0.5943 0.7214 0.119 Uiso 1 1 calc R . . C11 C 0.2041(5) 0.6850(2) 0.7032(2) 0.0686(14) Uani 1 1 d . . . H11A H 0.1086 0.6708 0.7203 0.103 Uiso 1 1 calc R . . H11B H 0.1884 0.6717 0.6713 0.103 Uiso 1 1 calc R . . H11C H 0.2238 0.7415 0.7061 0.103 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 0.04197(16) 0.03556(16) 0.03448(19) 0.00294(14) -0.00024(14) 0.00071(12) Cl1 0.0617(6) 0.0623(7) 0.0592(9) 0.0173(6) 0.0109(5) -0.0066(5) S1 0.0506(5) 0.0363(5) 0.0420(7) -0.0005(4) -0.0061(5) -0.0011(4) S2 0.0534(5) 0.0448(6) 0.0391(8) 0.0011(5) -0.0088(5) 0.0060(4) O1 0.0700(18) 0.0335(15) 0.057(2) 0.0055(13) -0.0124(15) 0.0061(11) O2 0.0758(19) 0.0552(17) 0.047(2) -0.0116(14) -0.0255(16) 0.0046(13) N1 0.0628(19) 0.0395(18) 0.035(2) 0.0023(14) 0.0005(16) 0.0031(14) N2 0.0398(16) 0.0396(18) 0.045(3) 0.0073(15) -0.0010(14) -0.0015(12) N3 0.0423(16) 0.0379(17) 0.035(2) -0.0001(14) -0.0002(13) -0.0007(12) C8 0.053(2) 0.053(2) 0.079(4) -0.008(2) -0.015(2) -0.0083(18) C7 0.063(3) 0.055(3) 0.045(3) -0.001(2) 0.001(2) 0.0026(18) C10 0.089(3) 0.053(3) 0.061(4) 0.018(2) -0.014(3) -0.004(2) C9 0.056(2) 0.072(3) 0.058(4) -0.006(2) -0.005(2) 0.0148(19) C1 0.063(3) 0.050(2) 0.048(3) 0.001(2) 0.014(2) 0.0119(17) C2 0.053(2) 0.050(2) 0.054(3) 0.000(2) 0.004(2) 0.0069(16) C3 0.046(2) 0.051(2) 0.044(3) 0.008(2) -0.0036(18) 0.0037(16) C4 0.047(2) 0.048(2) 0.042(3) 0.0059(19) 0.0006(17) -0.0001(15) C5 0.049(2) 0.043(2) 0.050(3) 0.0031(18) -0.0091(18) -0.0060(15) C6 0.058(2) 0.043(2) 0.046(3) -0.0021(19) -0.003(2) -0.0034(16) Cl2 0.0489(5) 0.0693(7) 0.0535(8) -0.0055(6) 0.0033(5) -0.0007(4) O3 0.0677(19) 0.072(2) 0.097(4) 0.005(2) -0.0098(19) 0.0039(15) C11 0.064(3) 0.066(3) 0.076(4) -0.004(3) -0.009(3) 0.001(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N3 2.118(3) . ? Ru N2 2.137(3) . ? Ru N1 2.139(3) . ? Ru S1 2.2504(11) . ? Ru S2 2.2644(11) . ? Ru Cl1 2.4257(11) . ? S1 O1 1.485(2) . ? S1 C7 1.778(5) . ? S1 C8 1.786(4) . ? S2 O2 1.485(3) . ? S2 C9 1.785(4) . ? S2 C10 1.785(4) . ? N1 C1 1.491(4) . ? N1 C6 1.493(4) . ? N1 H1 0.9100 . ? N2 C3 1.485(5) . ? N2 C2 1.510(5) . ? N2 H2 0.9100 . ? N3 C5 1.495(4) . ? N3 C4 1.500(5) . ? N3 H3 0.9100 . ? C8 H1A 0.9600 . ? C8 H1B 0.9600 . ? C8 H1C 0.9600 . ? C7 H2A 0.9600 . ? C7 H2B 0.9600 . ? C7 H2C 0.9600 . ? C10 H01E 0.9600 . ? C10 H01F 0.9600 . ? C10 H01G 0.9600 . ? C9 H02A 0.9600 . ? C9 H02B 0.9600 . ? C9 H02C 0.9600 . ? C1 C2 1.496(6) . ? C1 H01J 0.9700 . ? C1 H01K 0.9700 . ? C2 H02D 0.9700 . ? C2 H02E 0.9700 . ? C3 C4 1.506(5) . ? C3 H00A 0.9700 . ? C3 H00B 0.9700 . ? C4 H01H 0.9700 . ? C4 H01I 0.9700 . ? C5 C6 1.518(5) . ? C5 H01A 0.9700 . ? C5 H01B 0.9700 . ? C6 H01C 0.9700 . ? C6 H01D 0.9700 . ? O3 C11 1.401(5) . ? O3 H3A 0.8200 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ru N2 80.58(12) . . ? N3 Ru N1 80.62(12) . . ? N2 Ru N1 80.11(12) . . ? N3 Ru S1 99.67(9) . . ? N2 Ru S1 96.76(9) . . ? N1 Ru S1 176.78(9) . . ? N3 Ru S2 96.50(9) . . ? N2 Ru S2 170.40(9) . . ? N1 Ru S2 90.40(9) . . ? S1 Ru S2 92.75(4) . . ? N3 Ru Cl1 168.79(8) . . ? N2 Ru Cl1 89.97(9) . . ? N1 Ru Cl1 91.88(9) . . ? S1 Ru Cl1 87.35(4) . . ? S2 Ru Cl1 91.84(5) . . ? O1 S1 C7 104.55(18) . . ? O1 S1 C8 105.48(17) . . ? C7 S1 C8 100.1(2) . . ? O1 S1 Ru 117.13(13) . . ? C7 S1 Ru 115.61(13) . . ? C8 S1 Ru 112.15(15) . . ? O2 S2 C9 105.73(19) . . ? O2 S2 C10 106.1(2) . . ? C9 S2 C10 99.0(2) . . ? O2 S2 Ru 113.35(11) . . ? C9 S2 Ru 116.52(17) . . ? C10 S2 Ru 114.60(14) . . ? C1 N1 C6 112.4(3) . . ? C1 N1 Ru 105.9(2) . . ? C6 N1 Ru 111.6(2) . . ? C1 N1 H1 109.0 . . ? C6 N1 H1 109.0 . . ? Ru N1 H1 109.0 . . ? C3 N2 C2 113.1(3) . . ? C3 N2 Ru 107.2(2) . . ? C2 N2 Ru 110.9(2) . . ? C3 N2 H2 108.5 . . ? C2 N2 H2 108.5 . . ? Ru N2 H2 108.5 . . ? C5 N3 C4 111.3(3) . . ? C5 N3 Ru 107.0(2) . . ? C4 N3 Ru 112.2(2) . . ? C5 N3 H3 108.8 . . ? C4 N3 H3 108.8 . . ? Ru N3 H3 108.8 . . ? S1 C8 H1A 109.5 . . ? S1 C8 H1B 109.5 . . ? H1A C8 H1B 109.5 . . ? S1 C8 H1C 109.5 . . ? H1A C8 H1C 109.5 . . ? H1B C8 H1C 109.5 . . ? S1 C7 H2A 109.5 . . ? S1 C7 H2B 109.5 . . ? H2A C7 H2B 109.5 . . ? S1 C7 H2C 109.5 . . ? H2A C7 H2C 109.5 . . ? H2B C7 H2C 109.5 . . ? S2 C10 H01E 109.5 . . ? S2 C10 H01F 109.5 . . ? H01E C10 H01F 109.5 . . ? S2 C10 H01G 109.5 . . ? H01E C10 H01G 109.5 . . ? H01F C10 H01G 109.5 . . ? S2 C9 H02A 109.5 . . ? S2 C9 H02B 109.5 . . ? H02A C9 H02B 109.5 . . ? S2 C9 H02C 109.5 . . ? H02A C9 H02C 109.5 . . ? H02B C9 H02C 109.5 . . ? N1 C1 C2 109.3(3) . . ? N1 C1 H01J 109.8 . . ? C2 C1 H01J 109.8 . . ? N1 C1 H01K 109.8 . . ? C2 C1 H01K 109.8 . . ? H01J C1 H01K 108.3 . . ? C1 C2 N2 112.1(3) . . ? C1 C2 H02D 109.2 . . ? N2 C2 H02D 109.2 . . ? C1 C2 H02E 109.2 . . ? N2 C2 H02E 109.2 . . ? H02D C2 H02E 107.9 . . ? N2 C3 C4 110.9(3) . . ? N2 C3 H00A 109.5 . . ? C4 C3 H00A 109.5 . . ? N2 C3 H00B 109.5 . . ? C4 C3 H00B 109.5 . . ? H00A C3 H00B 108.0 . . ? N3 C4 C3 112.1(3) . . ? N3 C4 H01H 109.2 . . ? C3 C4 H01H 109.2 . . ? N3 C4 H01I 109.2 . . ? C3 C4 H01I 109.2 . . ? H01H C4 H01I 107.9 . . ? N3 C5 C6 109.1(3) . . ? N3 C5 H01A 109.9 . . ? C6 C5 H01A 109.9 . . ? N3 C5 H01B 109.9 . . ? C6 C5 H01B 109.9 . . ? H01A C5 H01B 108.3 . . ? N1 C6 C5 111.0(3) . . ? N1 C6 H01C 109.4 . . ? C5 C6 H01C 109.4 . . ? N1 C6 H01D 109.4 . . ? C5 C6 H01D 109.4 . . ? H01C C6 H01D 108.0 . . ? C11 O3 H3A 109.5 . . ? O3 C11 H11A 109.5 . . ? O3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? 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 N3 Ru S1 O1 123.55(16) . . . . ? N2 Ru S1 O1 -154.90(16) . . . . ? N1 Ru S1 O1 -141.5(16) . . . . ? S2 Ru S1 O1 26.47(14) . . . . ? Cl1 Ru S1 O1 -65.24(14) . . . . ? N3 Ru S1 C7 -0.41(18) . . . . ? N2 Ru S1 C7 81.14(18) . . . . ? N1 Ru S1 C7 94.5(16) . . . . ? S2 Ru S1 C7 -97.48(16) . . . . ? Cl1 Ru S1 C7 170.80(16) . . . . ? N3 Ru S1 C8 -114.29(19) . . . . ? N2 Ru S1 C8 -32.74(19) . . . . ? N1 Ru S1 C8 -19.4(16) . . . . ? S2 Ru S1 C8 148.63(18) . . . . ? Cl1 Ru S1 C8 56.92(18) . . . . ? N3 Ru S2 O2 68.99(17) . . . . ? N2 Ru S2 O2 -2.8(6) . . . . ? N1 Ru S2 O2 -11.62(17) . . . . ? S1 Ru S2 O2 169.05(15) . . . . ? Cl1 Ru S2 O2 -103.52(15) . . . . ? N3 Ru S2 C9 -54.08(18) . . . . ? N2 Ru S2 C9 -125.8(6) . . . . ? N1 Ru S2 C9 -134.69(18) . . . . ? S1 Ru S2 C9 45.99(16) . . . . ? Cl1 Ru S2 C9 133.42(16) . . . . ? N3 Ru S2 C10 -169.0(2) . . . . ? N2 Ru S2 C10 119.2(6) . . . . ? N1 Ru S2 C10 110.4(2) . . . . ? S1 Ru S2 C10 -68.96(19) . . . . ? Cl1 Ru S2 C10 18.47(19) . . . . ? N3 Ru N1 C1 115.6(3) . . . . ? N2 Ru N1 C1 33.7(2) . . . . ? S1 Ru N1 C1 20.2(18) . . . . ? S2 Ru N1 C1 -147.8(2) . . . . ? Cl1 Ru N1 C1 -56.0(2) . . . . ? N3 Ru N1 C6 -6.9(2) . . . . ? N2 Ru N1 C6 -88.9(2) . . . . ? S1 Ru N1 C6 -102.4(16) . . . . ? S2 Ru N1 C6 89.6(2) . . . . ? Cl1 Ru N1 C6 -178.6(2) . . . . ? N3 Ru N2 C3 30.1(2) . . . . ? N1 Ru N2 C3 112.2(2) . . . . ? S1 Ru N2 C3 -68.6(2) . . . . ? S2 Ru N2 C3 103.2(6) . . . . ? Cl1 Ru N2 C3 -155.9(2) . . . . ? N3 Ru N2 C2 -93.7(2) . . . . ? N1 Ru N2 C2 -11.7(2) . . . . ? S1 Ru N2 C2 167.6(2) . . . . ? S2 Ru N2 C2 -20.7(7) . . . . ? Cl1 Ru N2 C2 80.2(2) . . . . ? N2 Ru N3 C5 111.7(2) . . . . ? N1 Ru N3 C5 30.3(2) . . . . ? S1 Ru N3 C5 -152.9(2) . . . . ? S2 Ru N3 C5 -59.0(2) . . . . ? Cl1 Ru N3 C5 78.8(5) . . . . ? N2 Ru N3 C4 -10.5(2) . . . . ? N1 Ru N3 C4 -92.0(2) . . . . ? S1 Ru N3 C4 84.8(2) . . . . ? S2 Ru N3 C4 178.7(2) . . . . ? Cl1 Ru N3 C4 -43.5(6) . . . . ? C6 N1 C1 C2 71.4(4) . . . . ? Ru N1 C1 C2 -50.6(3) . . . . ? N1 C1 C2 N2 42.7(4) . . . . ? C3 N2 C2 C1 -133.4(4) . . . . ? Ru N2 C2 C1 -13.0(4) . . . . ? C2 N2 C3 C4 77.3(4) . . . . ? Ru N2 C3 C4 -45.2(3) . . . . ? C5 N3 C4 C3 -131.1(3) . . . . ? Ru N3 C4 C3 -11.2(4) . . . . ? N2 C3 C4 N3 37.8(4) . . . . ? C4 N3 C5 C6 74.0(4) . . . . ? Ru N3 C5 C6 -48.9(3) . . . . ? C1 N1 C6 C5 -136.7(4) . . . . ? Ru N1 C6 C5 -17.9(4) . . . . ? N3 C5 C6 N1 44.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.460 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.079 #===END data_9PF6-salt _database_code_depnum_ccdc_archive 'CCDC 872721' #TrackingRef '- CIF Rev1 DT-ART-03-2012-030654.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H27 Cl N3 O2 Ru S2, P F6' _chemical_formula_sum 'C10 H27 Cl F6 N3 O2 P Ru S2' _chemical_formula_weight 566.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.004 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.008 0.004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -0.923 1.037 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.179 0.201 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.014 0.008 '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 7.0860(9) _cell_length_b 10.8960(10) _cell_length_c 13.0630(12) _cell_angle_alpha 92.552(10) _cell_angle_beta 101.365(8) _cell_angle_gamma 93.978(9) _cell_volume 984.67(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(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 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 3.145 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5583 _exptl_absorpt_correction_T_max 0.7371 _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 100(2) _diffrn_radiation_wavelength 0.8000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Elettra Synchrotron, Trieste (Italy)' _diffrn_radiation_monochromator Si111 _diffrn_measurement_device_type 'MarResearch CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6395 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.52 _reflns_number_total 3463 _reflns_number_gt 1918 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.80.05 (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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0538P)^2^+1.0102P] 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 0.0129(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3463 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _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 0.38597(6) 0.29065(3) 0.67795(3) 0.0119(4) Uani 1 1 d . . . Cl1 Cl 0.69818(19) 0.23621(12) 0.65078(9) 0.0185(5) Uani 1 1 d . . . S1 S 0.3036(2) 0.08874(12) 0.68993(10) 0.0162(5) Uani 1 1 d . . . S2 S 0.2749(2) 0.28111(12) 0.50368(10) 0.0141(5) Uani 1 1 d . . . N1 N 0.4726(6) 0.4809(4) 0.6767(3) 0.0093(12) Uani 1 1 d . . . H1 H 0.5124 0.4943 0.6141 0.011 Uiso 1 1 calc R . . N2 N 0.4931(6) 0.3312(4) 0.8406(3) 0.0127(12) Uani 1 1 d . . . H2 H 0.5806 0.2743 0.8652 0.015 Uiso 1 1 calc R . . N3 N 0.1409(7) 0.3649(4) 0.7179(3) 0.0151(12) Uani 1 1 d . . . H3 H 0.0327 0.3110 0.6919 0.018 Uiso 1 1 calc R . . O1 O 0.2892(5) 0.0055(3) 0.5949(2) 0.0209(10) Uani 1 1 d . . . O2 O 0.2895(5) 0.4037(3) 0.4578(2) 0.0177(10) Uani 1 1 d . . . C1 C 0.6420(8) 0.5077(5) 0.7637(4) 0.0173(15) Uani 1 1 d . . . H1A H 0.6756 0.5977 0.7738 0.021 Uiso 1 1 calc R . . H1B H 0.7546 0.4681 0.7467 0.021 Uiso 1 1 calc R . . C2 C 0.5936(8) 0.4587(5) 0.8623(4) 0.0165(15) Uani 1 1 d . . . H2A H 0.7136 0.4564 0.9156 0.020 Uiso 1 1 calc R . . H2B H 0.5089 0.5144 0.8904 0.020 Uiso 1 1 calc R . . C3 C 0.3275(8) 0.3170(5) 0.8936(4) 0.0180(15) Uani 1 1 d . . . H3A H 0.3657 0.3517 0.9667 0.022 Uiso 1 1 calc R . . H3B H 0.2859 0.2286 0.8948 0.022 Uiso 1 1 calc R . . C4 C 0.1618(8) 0.3846(5) 0.8347(4) 0.0179(15) Uani 1 1 d . . . H4A H 0.0399 0.3547 0.8549 0.022 Uiso 1 1 calc R . . H4B H 0.1855 0.4739 0.8547 0.022 Uiso 1 1 calc R . . C5 C 0.1179(8) 0.4846(4) 0.6651(4) 0.0170(15) Uani 1 1 d . . . H5A H 0.0225 0.5314 0.6932 0.020 Uiso 1 1 calc R . . H5B H 0.0695 0.4676 0.5890 0.020 Uiso 1 1 calc R . . C6 C 0.3128(8) 0.5612(5) 0.6841(4) 0.0168(15) Uani 1 1 d . . . H6A H 0.3089 0.6243 0.6317 0.020 Uiso 1 1 calc R . . H6B H 0.3372 0.6043 0.7544 0.020 Uiso 1 1 calc R . . C7 C 0.0811(8) 0.0547(5) 0.7305(4) 0.0197(14) Uani 1 1 d . . . H7A H -0.0242 0.0861 0.6807 0.030 Uiso 1 1 calc R . . H7B H 0.0877 0.0940 0.8002 0.030 Uiso 1 1 calc R . . H7C H 0.0574 -0.0347 0.7328 0.030 Uiso 1 1 calc R . . C8 C 0.4668(9) 0.0233(5) 0.7904(4) 0.0245(16) Uani 1 1 d . . . H8A H 0.5984 0.0360 0.7777 0.037 Uiso 1 1 calc R . . H8B H 0.4310 -0.0652 0.7904 0.037 Uiso 1 1 calc R . . H8C H 0.4609 0.0632 0.8583 0.037 Uiso 1 1 calc R . . C9 C 0.0301(8) 0.2212(5) 0.4630(4) 0.0187(14) Uani 1 1 d . . . H9A H -0.0520 0.2690 0.4991 0.028 Uiso 1 1 calc R . . H9B H 0.0179 0.1347 0.4802 0.028 Uiso 1 1 calc R . . H9C H -0.0103 0.2268 0.3873 0.028 Uiso 1 1 calc R . . C10 C 0.3834(8) 0.1780(5) 0.4272(4) 0.0203(15) Uani 1 1 d . . . H10A H 0.5231 0.1990 0.4405 0.031 Uiso 1 1 calc R . . H10B H 0.3290 0.1849 0.3528 0.031 Uiso 1 1 calc R . . H10C H 0.3576 0.0933 0.4461 0.031 Uiso 1 1 calc R . . P1 P 0.0920(2) 0.76915(13) 0.93205(11) 0.0218(5) Uani 1 1 d . . . F1 F 0.2950(4) 0.7104(3) 0.9346(2) 0.0318(9) Uani 1 1 d . . . F2 F 0.1426(4) 0.7850(3) 1.0582(2) 0.0236(9) Uani 1 1 d . . . F3 F -0.1106(5) 0.8235(3) 0.9301(2) 0.0375(10) Uani 1 1 d . . . F4 F 0.0452(5) 0.7508(3) 0.8067(2) 0.0311(9) Uani 1 1 d . . . F5 F -0.0054(5) 0.6335(3) 0.9393(2) 0.0322(10) Uani 1 1 d . . . F6 F 0.1930(5) 0.9026(3) 0.9265(2) 0.0393(10) 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 0.0118(5) 0.0127(5) 0.0116(5) 0.0016(3) 0.0029(3) 0.0007(3) Cl1 0.0126(11) 0.0216(9) 0.0217(8) 0.0007(6) 0.0042(7) 0.0024(7) S1 0.0181(11) 0.0144(10) 0.0173(9) 0.0023(7) 0.0059(7) 0.0008(7) S2 0.0143(12) 0.0146(10) 0.0139(9) 0.0018(7) 0.0043(7) 0.0000(7) N1 0.008(3) 0.013(3) 0.007(2) 0.0009(19) 0.003(2) -0.002(2) N2 0.007(3) 0.018(3) 0.013(3) 0.001(2) 0.004(2) 0.003(2) N3 0.021(4) 0.015(3) 0.009(3) 0.001(2) 0.003(2) -0.001(2) O1 0.026(3) 0.016(2) 0.022(2) -0.0003(18) 0.0088(18) 0.0022(18) O2 0.018(3) 0.021(2) 0.015(2) 0.0070(17) 0.0028(16) -0.0019(18) C1 0.016(4) 0.012(3) 0.023(3) 0.004(3) 0.003(3) -0.002(3) C2 0.018(4) 0.016(4) 0.013(3) 0.004(3) -0.002(3) -0.004(3) C3 0.023(5) 0.016(3) 0.015(3) 0.002(3) 0.007(3) -0.003(3) C4 0.012(4) 0.020(3) 0.025(4) 0.005(3) 0.012(3) 0.000(3) C5 0.020(5) 0.014(3) 0.020(3) 0.008(3) 0.008(3) 0.008(3) C6 0.016(5) 0.016(3) 0.022(3) 0.010(3) 0.007(3) 0.006(3) C7 0.024(4) 0.015(3) 0.022(3) 0.003(2) 0.008(3) 0.003(3) C8 0.030(5) 0.019(3) 0.026(3) 0.005(3) 0.007(3) 0.002(3) C9 0.014(4) 0.023(3) 0.017(3) 0.005(3) 0.000(2) -0.002(3) C10 0.020(4) 0.021(3) 0.021(3) -0.001(3) 0.006(3) 0.005(3) P1 0.0277(14) 0.0219(11) 0.0161(10) 0.0030(7) 0.0052(8) 0.0006(9) F1 0.022(3) 0.050(2) 0.0263(18) 0.0030(15) 0.0084(16) 0.0132(18) F2 0.029(2) 0.0279(19) 0.0137(18) 0.0035(13) 0.0036(14) -0.0001(15) F3 0.031(3) 0.048(2) 0.0352(19) 0.0023(16) 0.0027(16) 0.0248(19) F4 0.046(3) 0.032(2) 0.0132(18) 0.0032(14) 0.0008(15) 0.0047(17) F5 0.041(3) 0.023(2) 0.0299(18) 0.0025(15) 0.0067(16) -0.0114(17) F6 0.060(3) 0.026(2) 0.0304(18) 0.0077(15) 0.0109(17) -0.0163(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N3 2.111(4) . ? Ru N1 2.123(4) . ? Ru N2 2.126(4) . ? Ru S2 2.2525(13) . ? Ru S1 2.2570(14) . ? Ru Cl1 2.4177(14) . ? S1 O1 1.487(4) . ? S1 C8 1.780(5) . ? S1 C7 1.780(5) . ? S2 O2 1.494(3) . ? S2 C9 1.779(5) . ? S2 C10 1.782(5) . ? N1 C1 1.484(7) . ? N1 C6 1.493(6) . ? N1 H1 0.9300 . ? N2 C3 1.478(6) . ? N2 C2 1.505(6) . ? N2 H2 0.9300 . ? N3 C5 1.507(6) . ? N3 C4 1.507(6) . ? N3 H3 0.9300 . ? C1 C2 1.507(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.526(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.534(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? P1 F6 1.586(3) . ? P1 F3 1.586(4) . ? P1 F5 1.602(3) . ? P1 F4 1.606(3) . ? P1 F1 1.610(4) . ? P1 F2 1.615(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 N3 Ru N1 81.00(16) . . ? N3 Ru N2 80.74(16) . . ? N1 Ru N2 80.20(15) . . ? N3 Ru S2 95.90(11) . . ? N1 Ru S2 90.73(11) . . ? N2 Ru S2 170.69(11) . . ? N3 Ru S1 99.13(12) . . ? N1 Ru S1 176.39(11) . . ? N2 Ru S1 96.25(11) . . ? S2 Ru S1 92.84(5) . . ? N3 Ru Cl1 169.91(12) . . ? N1 Ru Cl1 90.87(12) . . ? N2 Ru Cl1 92.05(12) . . ? S2 Ru Cl1 90.13(5) . . ? S1 Ru Cl1 88.62(5) . . ? O1 S1 C8 105.6(2) . . ? O1 S1 C7 103.9(2) . . ? C8 S1 C7 100.7(3) . . ? O1 S1 Ru 117.57(14) . . ? C8 S1 Ru 111.84(19) . . ? C7 S1 Ru 115.47(19) . . ? O2 S2 C9 106.3(2) . . ? O2 S2 C10 106.3(2) . . ? C9 S2 C10 98.8(3) . . ? O2 S2 Ru 112.79(14) . . ? C9 S2 Ru 114.56(17) . . ? C10 S2 Ru 116.69(19) . . ? C1 N1 C6 112.8(4) . . ? C1 N1 Ru 106.6(3) . . ? C6 N1 Ru 112.6(3) . . ? C1 N1 H1 108.2 . . ? C6 N1 H1 108.2 . . ? Ru N1 H1 108.2 . . ? C3 N2 C2 111.2(4) . . ? C3 N2 Ru 107.5(3) . . ? C2 N2 Ru 111.7(3) . . ? C3 N2 H2 108.8 . . ? C2 N2 H2 108.8 . . ? Ru N2 H2 108.8 . . ? C5 N3 C4 111.2(4) . . ? C5 N3 Ru 106.8(3) . . ? C4 N3 Ru 111.7(3) . . ? C5 N3 H3 109.0 . . ? C4 N3 H3 109.0 . . ? Ru N3 H3 109.0 . . ? N1 C1 C2 109.0(4) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C1 110.5(4) . . ? N2 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N2 C3 C4 109.0(4) . . ? N2 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? N2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N3 C4 C3 111.6(4) . . ? N3 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N3 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? N3 C5 C6 109.8(4) . . ? N3 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? N3 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? N1 C6 C5 110.8(4) . . ? N1 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? S1 C7 H7A 109.5 . . ? S1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S1 C8 H8A 109.5 . . ? S1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? S2 C9 H9A 109.5 . . ? S2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? S2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? S2 C10 H10A 109.5 . . ? S2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? F6 P1 F3 91.4(2) . . ? F6 P1 F5 178.7(2) . . ? F3 P1 F5 89.71(18) . . ? F6 P1 F4 90.78(16) . . ? F3 P1 F4 90.67(17) . . ? F5 P1 F4 89.92(16) . . ? F6 P1 F1 90.10(19) . . ? F3 P1 F1 178.47(19) . . ? F5 P1 F1 88.76(18) . . ? F4 P1 F1 89.52(17) . . ? F6 P1 F2 89.76(16) . . ? F3 P1 F2 90.59(16) . . ? F5 P1 F2 89.51(15) . . ? F4 P1 F2 178.62(18) . . ? F1 P1 F2 89.21(16) . . ? 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 N3 Ru S1 O1 121.3(2) . . . . ? N1 Ru S1 O1 -147.0(18) . . . . ? N2 Ru S1 O1 -157.1(2) . . . . ? S2 Ru S1 O1 24.84(18) . . . . ? Cl1 Ru S1 O1 -65.21(18) . . . . ? N3 Ru S1 C8 -116.4(2) . . . . ? N1 Ru S1 C8 -24.6(18) . . . . ? N2 Ru S1 C8 -34.8(2) . . . . ? S2 Ru S1 C8 147.2(2) . . . . ? Cl1 Ru S1 C8 57.1(2) . . . . ? N3 Ru S1 C7 -2.0(2) . . . . ? N1 Ru S1 C7 89.7(18) . . . . ? N2 Ru S1 C7 79.6(2) . . . . ? S2 Ru S1 C7 -98.5(2) . . . . ? Cl1 Ru S1 C7 171.5(2) . . . . ? N3 Ru S2 O2 77.1(2) . . . . ? N1 Ru S2 O2 -3.9(2) . . . . ? N2 Ru S2 O2 8.8(7) . . . . ? S1 Ru S2 O2 176.63(17) . . . . ? Cl1 Ru S2 O2 -94.75(17) . . . . ? N3 Ru S2 C9 -44.7(2) . . . . ? N1 Ru S2 C9 -125.7(2) . . . . ? N2 Ru S2 C9 -113.0(7) . . . . ? S1 Ru S2 C9 54.8(2) . . . . ? Cl1 Ru S2 C9 143.4(2) . . . . ? N3 Ru S2 C10 -159.4(2) . . . . ? N1 Ru S2 C10 119.6(2) . . . . ? N2 Ru S2 C10 132.3(7) . . . . ? S1 Ru S2 C10 -59.9(2) . . . . ? Cl1 Ru S2 C10 28.7(2) . . . . ? N3 Ru N1 C1 114.1(3) . . . . ? N2 Ru N1 C1 32.0(3) . . . . ? S2 Ru N1 C1 -150.0(3) . . . . ? S1 Ru N1 C1 22(2) . . . . ? Cl1 Ru N1 C1 -59.9(3) . . . . ? N3 Ru N1 C6 -10.1(3) . . . . ? N2 Ru N1 C6 -92.2(3) . . . . ? S2 Ru N1 C6 85.7(3) . . . . ? S1 Ru N1 C6 -102.4(18) . . . . ? Cl1 Ru N1 C6 175.9(3) . . . . ? N3 Ru N2 C3 31.4(3) . . . . ? N1 Ru N2 C3 113.8(3) . . . . ? S2 Ru N2 C3 100.8(7) . . . . ? S1 Ru N2 C3 -66.9(3) . . . . ? Cl1 Ru N2 C3 -155.7(3) . . . . ? N3 Ru N2 C2 -90.9(4) . . . . ? N1 Ru N2 C2 -8.5(3) . . . . ? S2 Ru N2 C2 -21.4(10) . . . . ? S1 Ru N2 C2 170.8(3) . . . . ? Cl1 Ru N2 C2 82.0(3) . . . . ? N1 Ru N3 C5 31.2(3) . . . . ? N2 Ru N3 C5 112.6(3) . . . . ? S2 Ru N3 C5 -58.6(3) . . . . ? S1 Ru N3 C5 -152.5(3) . . . . ? Cl1 Ru N3 C5 67.8(7) . . . . ? N1 Ru N3 C4 -90.6(3) . . . . ? N2 Ru N3 C4 -9.1(3) . . . . ? S2 Ru N3 C4 179.6(3) . . . . ? S1 Ru N3 C4 85.8(3) . . . . ? Cl1 Ru N3 C4 -54.0(8) . . . . ? C6 N1 C1 C2 73.5(5) . . . . ? Ru N1 C1 C2 -50.6(5) . . . . ? C3 N2 C2 C1 -136.8(4) . . . . ? Ru N2 C2 C1 -16.6(5) . . . . ? N1 C1 C2 N2 44.7(6) . . . . ? C2 N2 C3 C4 74.9(5) . . . . ? Ru N2 C3 C4 -47.7(4) . . . . ? C5 N3 C4 C3 -133.6(4) . . . . ? Ru N3 C4 C3 -14.4(5) . . . . ? N2 C3 C4 N3 41.3(5) . . . . ? C4 N3 C5 C6 74.7(5) . . . . ? Ru N3 C5 C6 -47.4(4) . . . . ? C1 N1 C6 C5 -133.9(4) . . . . ? Ru N1 C6 C5 -13.2(5) . . . . ? N3 C5 C6 N1 40.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.52 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.357 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.097 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 872722' #TrackingRef '- CIF Rev1 DT-ART-03-2012-030654.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H29 N5 O Ru S, 2(Cl), H2 O' _chemical_formula_sum 'C10 H31 Cl2 N5 O2 Ru S' _chemical_formula_weight 457.43 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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.027(5) _cell_length_b 8.391(2) _cell_length_c 15.971(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.27(2) _cell_angle_gamma 90.00 _cell_volume 3934.2(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_min 0.31 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_max 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5438 _exptl_absorpt_correction_T_max 0.7838 _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 26525 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 31.09 _reflns_number_total 6044 _reflns_number_gt 4524 _reflns_threshold_expression >2\s(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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Carbon atoms C5-C10 were refined with instruction ISOR 0.02 due to their high thermal motion, likely due to disorder. ; _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^)+(0.0856P)^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 6044 _refine_ls_number_parameters 190 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.997 _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 0.119257(7) 0.45737(2) 0.499048(14) 0.04232(9) Uani 1 1 d . . . O1 O 0.12806(9) 0.0981(3) 0.4515(2) 0.0737(7) Uani 1 1 d . . . N1 N 0.17532(8) 0.6181(3) 0.55725(18) 0.0536(5) Uani 1 1 d . . . H1 H 0.2004 0.5639 0.5987 0.064 Uiso 1 1 calc R . . N2 N 0.10498(9) 0.5986(3) 0.37862(17) 0.0525(5) Uani 1 1 d . . . H2 H 0.0971 0.5332 0.3281 0.063 Uiso 1 1 calc R . . N3 N 0.12574(9) 0.3451(3) 0.62473(19) 0.0580(6) Uani 1 1 d . . . H3C H 0.1546 0.3112 0.6590 0.070 Uiso 1 1 calc R . . H3D H 0.1196 0.4163 0.6595 0.070 Uiso 1 1 calc R . . N4 N 0.05877(8) 0.3156(3) 0.44327(19) 0.0557(6) Uani 1 1 d . . . H4C H 0.0349 0.3753 0.4044 0.067 Uiso 1 1 calc R . . H4D H 0.0617 0.2344 0.4097 0.067 Uiso 1 1 calc R . . N5 N 0.08702(9) 0.6555(3) 0.5285(2) 0.0565(6) Uani 1 1 d . . . H5 H 0.0674 0.6183 0.5495 0.068 Uiso 1 1 calc R . . S1 S 0.15232(2) 0.25373(8) 0.46691(5) 0.04966(16) Uani 1 1 d . . . C1 C 0.16174(14) 0.2675(5) 0.3656(3) 0.0683(9) Uani 1 1 d . . . H1A H 0.1333 0.2878 0.3109 0.103 Uiso 1 1 calc R . . H1B H 0.1744 0.1691 0.3575 0.103 Uiso 1 1 calc R . . H1C H 0.1826 0.3530 0.3740 0.103 Uiso 1 1 calc R . . C2 C 0.20881(12) 0.2166(5) 0.5553(3) 0.0714(9) Uani 1 1 d . . . H2A H 0.2090 0.2063 0.6154 0.107 Uiso 1 1 calc R . . H2B H 0.2281 0.3036 0.5575 0.107 Uiso 1 1 calc R . . H2C H 0.2198 0.1198 0.5409 0.107 Uiso 1 1 calc R . . C3 C 0.09429(15) 0.2085(4) 0.6023(3) 0.0699(9) Uani 1 1 d . . . H3A H 0.0896 0.1824 0.6563 0.084 Uiso 1 1 calc R . . H3B H 0.1072 0.1160 0.5868 0.084 Uiso 1 1 calc R . . C4 C 0.05019(13) 0.2512(5) 0.5209(3) 0.0728(9) Uani 1 1 d . . . H4A H 0.0347 0.3307 0.5399 0.087 Uiso 1 1 calc R . . H4B H 0.0309 0.1577 0.4991 0.087 Uiso 1 1 calc R . . C5 C 0.06069(18) 0.7485(6) 0.4399(4) 0.0980(16) Uani 1 1 d U . . H5A H 0.0287 0.7432 0.4243 0.118 Uiso 1 1 calc R . . H5B H 0.0699 0.8593 0.4526 0.118 Uiso 1 1 calc R . . C6 C 0.06523(17) 0.7011(7) 0.3623(3) 0.0937(15) Uani 1 1 d U . . H6A H 0.0668 0.7961 0.3293 0.112 Uiso 1 1 calc R . . H6B H 0.0378 0.6443 0.3206 0.112 Uiso 1 1 calc R . . C7 C 0.14444(15) 0.6942(5) 0.3908(3) 0.0776(11) Uani 1 1 d U . . H7A H 0.1529 0.6640 0.3423 0.093 Uiso 1 1 calc R . . H7B H 0.1354 0.8053 0.3808 0.093 Uiso 1 1 calc R . . C8 C 0.18417(15) 0.6797(7) 0.4814(3) 0.1028(18) Uani 1 1 d U . . H8A H 0.1983 0.7838 0.4998 0.123 Uiso 1 1 calc R . . H8B H 0.2059 0.6098 0.4746 0.123 Uiso 1 1 calc R . . C9 C 0.16575(15) 0.7479(6) 0.6083(4) 0.1009(17) Uani 1 1 d U . . H9A H 0.1883 0.7431 0.6739 0.121 Uiso 1 1 calc R . . H9B H 0.1697 0.8488 0.5833 0.121 Uiso 1 1 calc R . . C10 C 0.12322(17) 0.7471(7) 0.6043(4) 0.1028(17) Uani 1 1 d U . . H10A H 0.1130 0.8567 0.5991 0.123 Uiso 1 1 calc R . . H10B H 0.1264 0.7065 0.6639 0.123 Uiso 1 1 calc R . . Cl1 Cl 0.04901(3) 0.56944(13) 0.67808(7) 0.0738(3) Uani 1 1 d . . . Cl2 Cl 0.21596(3) 0.93069(12) 0.29260(8) 0.0731(2) Uani 1 1 d . . . O1W O 0.21928(11) 0.5561(4) 0.2980(3) 0.0854(8) Uani 1 1 d . . . H1W H 0.2377 0.5185 0.2703 0.129 Uiso 1 1 d R . . H2W H 0.2183 0.6624 0.2945 0.129 Uiso 1 1 d 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 0.03791(12) 0.04097(13) 0.04602(14) -0.00046(7) 0.01745(9) -0.00128(7) O1 0.0742(16) 0.0449(11) 0.115(2) -0.0107(13) 0.0541(16) -0.0056(11) N1 0.0453(12) 0.0523(13) 0.0562(13) -0.0026(10) 0.0174(10) -0.0070(10) N2 0.0566(14) 0.0504(12) 0.0466(12) 0.0013(9) 0.0203(10) 0.0023(11) N3 0.0586(15) 0.0603(15) 0.0571(14) 0.0055(11) 0.0283(11) -0.0025(12) N4 0.0416(12) 0.0505(13) 0.0679(15) -0.0032(11) 0.0189(10) -0.0060(10) N5 0.0583(14) 0.0465(13) 0.0753(16) -0.0016(11) 0.0397(13) -0.0001(11) S1 0.0460(3) 0.0425(3) 0.0605(4) 0.0012(3) 0.0245(3) 0.0032(3) C1 0.081(2) 0.066(2) 0.067(2) -0.0026(15) 0.0410(17) 0.0119(18) C2 0.0592(19) 0.073(2) 0.074(2) 0.0123(17) 0.0240(16) 0.0198(17) C3 0.083(2) 0.0580(19) 0.073(2) 0.0045(15) 0.0394(18) -0.0125(17) C4 0.064(2) 0.071(2) 0.093(3) -0.0032(18) 0.0445(19) -0.0188(18) C5 0.114(4) 0.095(3) 0.115(3) 0.044(3) 0.078(3) 0.059(3) C6 0.104(3) 0.108(3) 0.061(2) 0.0149(19) 0.0303(19) 0.060(3) C7 0.091(3) 0.080(2) 0.070(2) 0.0017(17) 0.0435(19) -0.028(2) C8 0.065(2) 0.139(4) 0.089(3) 0.039(3) 0.022(2) -0.034(3) C9 0.072(3) 0.083(3) 0.111(3) -0.050(3) 0.010(2) 0.004(2) C10 0.098(3) 0.106(3) 0.135(4) -0.071(3) 0.080(3) -0.041(3) Cl1 0.0519(4) 0.1042(7) 0.0647(5) 0.0184(4) 0.0263(4) 0.0115(4) Cl2 0.0631(5) 0.0689(5) 0.0845(6) 0.0073(4) 0.0314(4) 0.0074(4) O1W 0.0678(17) 0.083(2) 0.104(2) 0.0052(15) 0.0378(16) 0.0007(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.120(2) . ? Ru N1 2.130(2) . ? Ru N4 2.137(2) . ? Ru N3 2.137(3) . ? Ru N5 2.140(3) . ? Ru S1 2.2112(8) . ? O1 S1 1.492(3) . ? N1 C8 1.465(5) . ? N1 C9 1.479(5) . ? N2 C7 1.466(4) . ? N2 C6 1.490(5) . ? N3 C3 1.477(4) . ? N4 C4 1.494(4) . ? N5 C10 1.470(5) . ? N5 C5 1.496(5) . ? S1 C2 1.777(4) . ? S1 C1 1.785(4) . ? C3 C4 1.484(6) . ? C5 C6 1.374(6) . ? C7 C8 1.446(6) . ? C9 C10 1.377(6) . ? 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 80.19(10) . . ? N2 Ru N4 98.97(10) . . ? N1 Ru N4 173.80(10) . . ? N2 Ru N3 169.50(10) . . ? N1 Ru N3 100.15(10) . . ? N4 Ru N3 79.55(11) . . ? N2 Ru N5 80.73(10) . . ? N1 Ru N5 80.36(10) . . ? N4 Ru N5 93.44(10) . . ? N3 Ru N5 88.96(11) . . ? N2 Ru S1 98.60(8) . . ? N1 Ru S1 99.65(8) . . ? N4 Ru S1 86.55(8) . . ? N3 Ru S1 91.70(8) . . ? N5 Ru S1 179.32(8) . . ? C8 N1 C9 111.7(4) . . ? C8 N1 Ru 109.0(2) . . ? C9 N1 Ru 110.1(2) . . ? C7 N2 C6 111.5(4) . . ? C7 N2 Ru 111.8(2) . . ? C6 N2 Ru 107.1(2) . . ? C3 N3 Ru 110.9(2) . . ? C4 N4 Ru 110.6(2) . . ? C10 N5 C5 114.0(4) . . ? C10 N5 Ru 106.8(2) . . ? C5 N5 Ru 109.2(2) . . ? O1 S1 C2 105.45(19) . . ? O1 S1 C1 102.14(18) . . ? C2 S1 C1 100.14(19) . . ? O1 S1 Ru 115.46(11) . . ? C2 S1 Ru 113.66(14) . . ? C1 S1 Ru 118.03(13) . . ? N3 C3 C4 108.9(3) . . ? C3 C4 N4 109.3(3) . . ? C6 C5 N5 116.5(3) . . ? C5 C6 N2 117.5(3) . . ? C8 C7 N2 115.5(3) . . ? C7 C8 N1 115.1(3) . . ? C10 C9 N1 116.3(4) . . ? C9 C10 N5 117.9(3) . . ? 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 C8 -24.7(3) . . . . ? N4 Ru N1 C8 -107.4(10) . . . . ? N3 Ru N1 C8 166.0(3) . . . . ? N5 Ru N1 C8 -106.9(3) . . . . ? S1 Ru N1 C8 72.5(3) . . . . ? N2 Ru N1 C9 98.2(3) . . . . ? N4 Ru N1 C9 15.5(11) . . . . ? N3 Ru N1 C9 -71.1(3) . . . . ? N5 Ru N1 C9 16.1(3) . . . . ? S1 Ru N1 C9 -164.6(3) . . . . ? N1 Ru N2 C7 15.0(3) . . . . ? N4 Ru N2 C7 -171.2(3) . . . . ? N3 Ru N2 C7 107.7(6) . . . . ? N5 Ru N2 C7 96.7(3) . . . . ? S1 Ru N2 C7 -83.4(2) . . . . ? N1 Ru N2 C6 -107.3(3) . . . . ? N4 Ru N2 C6 66.4(3) . . . . ? N3 Ru N2 C6 -14.6(7) . . . . ? N5 Ru N2 C6 -25.6(3) . . . . ? S1 Ru N2 C6 154.3(3) . . . . ? N2 Ru N3 C3 97.7(6) . . . . ? N1 Ru N3 C3 -171.4(2) . . . . ? N4 Ru N3 C3 14.9(2) . . . . ? N5 Ru N3 C3 108.6(3) . . . . ? S1 Ru N3 C3 -71.3(2) . . . . ? N2 Ru N4 C4 -157.2(2) . . . . ? N1 Ru N4 C4 -75.5(10) . . . . ? N3 Ru N4 C4 12.3(2) . . . . ? N5 Ru N4 C4 -76.0(2) . . . . ? S1 Ru N4 C4 104.6(2) . . . . ? N2 Ru N5 C10 -106.0(3) . . . . ? N1 Ru N5 C10 -24.5(3) . . . . ? N4 Ru N5 C10 155.5(3) . . . . ? N3 Ru N5 C10 76.0(3) . . . . ? S1 Ru N5 C10 -116(6) . . . . ? N2 Ru N5 C5 17.8(3) . . . . ? N1 Ru N5 C5 99.3(3) . . . . ? N4 Ru N5 C5 -80.8(3) . . . . ? N3 Ru N5 C5 -160.2(3) . . . . ? S1 Ru N5 C5 8(6) . . . . ? N2 Ru S1 O1 -116.30(16) . . . . ? N1 Ru S1 O1 162.27(16) . . . . ? N4 Ru S1 O1 -17.74(16) . . . . ? N3 Ru S1 O1 61.68(16) . . . . ? N5 Ru S1 O1 -106(6) . . . . ? N2 Ru S1 C2 121.64(17) . . . . ? N1 Ru S1 C2 40.22(17) . . . . ? N4 Ru S1 C2 -139.80(17) . . . . ? N3 Ru S1 C2 -60.38(17) . . . . ? N5 Ru S1 C2 132(6) . . . . ? N2 Ru S1 C1 4.84(17) . . . . ? N1 Ru S1 C1 -76.58(18) . . . . ? N4 Ru S1 C1 103.40(17) . . . . ? N3 Ru S1 C1 -177.18(18) . . . . ? N5 Ru S1 C1 15(6) . . . . ? Ru N3 C3 C4 -39.7(4) . . . . ? N3 C3 C4 N4 50.7(4) . . . . ? Ru N4 C4 C3 -37.4(4) . . . . ? C10 N5 C5 C6 113.7(5) . . . . ? Ru N5 C5 C6 -5.6(6) . . . . ? N5 C5 C6 N2 -17.8(8) . . . . ? C7 N2 C6 C5 -90.8(6) . . . . ? Ru N2 C6 C5 31.7(6) . . . . ? C6 N2 C7 C8 117.6(5) . . . . ? Ru N2 C7 C8 -2.2(5) . . . . ? N2 C7 C8 N1 -19.9(7) . . . . ? C9 N1 C8 C7 -90.5(5) . . . . ? Ru N1 C8 C7 31.4(6) . . . . ? C8 N1 C9 C10 117.6(6) . . . . ? Ru N1 C9 C10 -3.7(6) . . . . ? N1 C9 C10 N5 -19.3(8) . . . . ? C5 N5 C10 C9 -89.2(6) . . . . ? Ru N5 C10 C9 31.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 31.09 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.959 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.114 #===END data_12 _database_code_depnum_ccdc_archive 'CCDC 872723' #TrackingRef '- CIF Rev1 DT-ART-03-2012-030654.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H29 N5 O Ru S, 2(P F6), H2 O' _chemical_formula_sum 'C18 H31 F12 N5 O2 P2 Ru S' _chemical_formula_weight 772.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.863(3) _cell_length_b 11.769(2) _cell_length_c 24.381(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.515(10) _cell_angle_gamma 90.00 _cell_volume 6103.2(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.786 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7367 _exptl_absorpt_correction_T_max 0.8605 _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 'Enraf-Nonius dip1030 image plate diffractometer' _diffrn_measurement_method '\f-scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39597 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_sigmaI/netI 0.1029 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5617 _reflns_number_gt 2914 _reflns_threshold_expression >2\s(I) _computing_data_collection 'XPRESS (MacScience, 2002)' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.80.05 (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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1118P)^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 5617 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1189 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1888 _refine_ls_wR_factor_gt 0.1692 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.883 _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 0.26504(3) 0.10350(5) 0.12580(2) 0.0520(2) Uani 1 1 d . . . N1 N 0.3380(3) 0.0264(5) 0.1931(3) 0.0612(16) Uani 1 1 d . . . N2 N 0.3296(3) 0.2341(5) 0.1549(2) 0.0577(15) Uani 1 1 d . . . C1 C 0.3458(4) -0.0879(7) 0.2039(4) 0.070(2) Uani 1 1 d . . . H1 H 0.3150 -0.1373 0.1804 0.085 Uiso 1 1 calc R . . C2 C 0.3971(5) -0.1322(9) 0.2479(4) 0.090(3) Uani 1 1 d . . . H2 H 0.4022 -0.2103 0.2531 0.108 Uiso 1 1 calc R . . C3 C 0.4405(5) -0.0589(10) 0.2839(4) 0.097(3) Uani 1 1 d . . . H3 H 0.4741 -0.0872 0.3157 0.116 Uiso 1 1 calc R . . C4 C 0.4351(4) 0.0602(9) 0.2736(4) 0.087(3) Uani 1 1 d . . . H4 H 0.4652 0.1104 0.2974 0.105 Uiso 1 1 calc R . . C5 C 0.3834(3) 0.0987(7) 0.2271(3) 0.0627(19) Uani 1 1 d . . . C6 C 0.3771(4) 0.2160(7) 0.2078(3) 0.0615(19) Uani 1 1 d . . . C7 C 0.4157(4) 0.3017(8) 0.2385(4) 0.078(2) Uani 1 1 d . . . H7 H 0.4470 0.2878 0.2751 0.094 Uiso 1 1 calc R . . C8 C 0.4072(4) 0.4097(8) 0.2140(5) 0.090(3) Uani 1 1 d . . . H8 H 0.4324 0.4692 0.2348 0.108 Uiso 1 1 calc R . . C9 C 0.3616(4) 0.4297(7) 0.1592(4) 0.083(3) Uani 1 1 d . . . H9 H 0.3567 0.5016 0.1423 0.099 Uiso 1 1 calc R . . C10 C 0.3235(4) 0.3405(7) 0.1300(4) 0.068(2) Uani 1 1 d . . . H10 H 0.2931 0.3528 0.0927 0.081 Uiso 1 1 calc R . . N3 N 0.1935(3) -0.0208(5) 0.1108(2) 0.0630(16) Uani 1 1 d . . . H3A H 0.2080 -0.0891 0.1038 0.076 Uiso 1 1 calc R . . N4 N 0.1901(3) 0.1919(5) 0.0631(2) 0.0589(15) Uani 1 1 d . . . H4A H 0.2054 0.2365 0.0410 0.071 Uiso 1 1 calc R . . N5 N 0.2198(3) 0.1683(5) 0.1826(2) 0.0576(15) Uani 1 1 d . . . H5 H 0.2494 0.1801 0.2191 0.069 Uiso 1 1 calc R . . C11 C 0.1344(4) 0.0089(8) 0.0598(4) 0.079(2) Uani 1 1 d . . . H11A H 0.1019 0.0319 0.0743 0.094 Uiso 1 1 calc R . . H11B H 0.1194 -0.0571 0.0347 0.094 Uiso 1 1 calc R . . C12 C 0.1479(4) 0.1051(7) 0.0247(3) 0.075(2) Uani 1 1 d . . . H12A H 0.1671 0.0743 -0.0016 0.090 Uiso 1 1 calc R . . H12B H 0.1086 0.1408 0.0007 0.090 Uiso 1 1 calc R . . C13 C 0.1555(4) 0.2657(7) 0.0921(4) 0.077(2) Uani 1 1 d . . . H13A H 0.1480 0.3400 0.0736 0.093 Uiso 1 1 calc R . . H13B H 0.1150 0.2318 0.0866 0.093 Uiso 1 1 calc R . . C14 C 0.1929(4) 0.2787(7) 0.1571(4) 0.071(2) Uani 1 1 d . . . H14A H 0.2264 0.3334 0.1630 0.085 Uiso 1 1 calc R . . H14B H 0.1658 0.3068 0.1768 0.085 Uiso 1 1 calc R . . C15 C 0.1718(4) 0.0879(6) 0.1873(3) 0.066(2) Uani 1 1 d . . . H15A H 0.1301 0.1149 0.1634 0.080 Uiso 1 1 calc R . . H15B H 0.1745 0.0843 0.2279 0.080 Uiso 1 1 calc R . . C16 C 0.1817(4) -0.0273(6) 0.1672(3) 0.071(2) Uani 1 1 d . . . H16A H 0.1448 -0.0737 0.1614 0.085 Uiso 1 1 calc R . . H16B H 0.2173 -0.0631 0.1973 0.085 Uiso 1 1 calc R . . S1 S 0.30243(10) 0.04902(17) 0.05766(8) 0.0642(5) Uani 1 1 d . . . O1 O 0.2835(3) 0.1228(4) 0.0039(2) 0.0750(16) Uani 1 1 d . . . C17 C 0.2846(5) -0.0944(6) 0.0322(4) 0.096(3) Uani 1 1 d . . . H17A H 0.2404 -0.1012 0.0098 0.143 Uiso 1 1 calc R . . H17B H 0.2962 -0.1449 0.0654 0.143 Uiso 1 1 calc R . . H17C H 0.3078 -0.1138 0.0077 0.143 Uiso 1 1 calc R . . C18 C 0.3857(4) 0.0387(9) 0.0836(4) 0.098(3) Uani 1 1 d . . . H18A H 0.3984 0.0154 0.0518 0.147 Uiso 1 1 calc R . . H18B H 0.3999 -0.0162 0.1148 0.147 Uiso 1 1 calc R . . H18C H 0.4039 0.1113 0.0981 0.147 Uiso 1 1 calc R . . P1 P 0.19940(14) 0.63174(19) 0.14119(10) 0.0789(7) Uani 1 1 d . . . F1 F 0.2166(4) 0.5401(5) 0.1921(3) 0.141(3) Uani 1 1 d . . . F2 F 0.2643(5) 0.6863(9) 0.1709(4) 0.243(6) Uani 1 1 d . . . F3 F 0.1834(5) 0.7254(5) 0.0933(3) 0.175(4) Uani 1 1 d . . . F4 F 0.1358(4) 0.5834(10) 0.1176(5) 0.248(6) Uani 1 1 d . . . F5 F 0.2150(6) 0.5485(6) 0.1021(4) 0.195(4) Uani 1 1 d . . . F6 F 0.1825(6) 0.7125(6) 0.1834(4) 0.219(5) Uani 1 1 d . . . P2 P 0.46021(13) 0.6712(3) 0.10192(13) 0.0925(8) Uani 1 1 d . . . F7 F 0.4827(7) 0.5848(14) 0.1455(6) 0.350(11) Uani 1 1 d . . . F8 F 0.5250(4) 0.7211(10) 0.1328(5) 0.230(5) Uani 1 1 d . . . F9 F 0.4325(7) 0.7565(13) 0.0559(8) 0.342(9) Uani 1 1 d . . . F10 F 0.3993(5) 0.6096(10) 0.0740(4) 0.246(6) Uani 1 1 d . . . F11 F 0.4878(4) 0.6264(9) 0.0575(4) 0.199(4) Uani 1 1 d . . . F12 F 0.4335(4) 0.7385(15) 0.1376(6) 0.294(8) Uani 1 1 d . . . O1W O 0.4777(5) 0.2876(9) 0.1164(5) 0.095(5) Uiso 0.579(19) 1 d P . . O2W O 0.5118(9) 0.2868(16) 0.0895(8) 0.124(9) Uiso 0.421(19) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0653(4) 0.0468(3) 0.0457(3) 0.0020(3) 0.0223(3) 0.0014(3) N1 0.077(4) 0.059(4) 0.054(4) 0.012(3) 0.032(3) 0.010(3) N2 0.059(4) 0.063(4) 0.053(3) 0.009(3) 0.023(3) 0.002(3) C1 0.077(5) 0.070(5) 0.070(5) 0.033(5) 0.034(4) 0.018(4) C2 0.093(7) 0.096(7) 0.089(7) 0.043(6) 0.044(6) 0.025(6) C3 0.083(7) 0.120(9) 0.080(6) 0.048(7) 0.021(6) 0.031(6) C4 0.078(6) 0.105(8) 0.069(5) 0.023(6) 0.016(5) 0.011(5) C5 0.060(5) 0.074(5) 0.051(4) 0.019(4) 0.018(4) 0.011(4) C6 0.061(5) 0.073(5) 0.053(4) 0.005(4) 0.025(4) -0.003(4) C7 0.075(6) 0.089(7) 0.064(5) -0.003(5) 0.016(4) -0.013(5) C8 0.081(6) 0.078(7) 0.107(8) -0.030(6) 0.029(6) -0.018(5) C9 0.092(7) 0.056(5) 0.105(7) 0.005(5) 0.042(6) -0.012(5) C10 0.074(5) 0.056(5) 0.080(5) 0.013(4) 0.036(4) -0.005(4) N3 0.074(4) 0.058(4) 0.058(4) -0.005(3) 0.026(3) -0.001(3) N4 0.065(4) 0.055(4) 0.057(3) -0.001(3) 0.022(3) 0.000(3) N5 0.073(4) 0.050(4) 0.051(3) -0.001(3) 0.025(3) -0.004(3) C11 0.076(6) 0.086(6) 0.072(5) -0.017(5) 0.026(5) -0.021(5) C12 0.078(6) 0.076(6) 0.061(5) 0.000(5) 0.013(4) 0.001(5) C13 0.085(6) 0.063(5) 0.087(6) 0.015(5) 0.034(5) 0.015(4) C14 0.082(6) 0.059(5) 0.082(6) -0.004(5) 0.044(5) 0.003(4) C15 0.072(5) 0.072(5) 0.060(4) 0.003(4) 0.030(4) -0.012(4) C16 0.085(6) 0.055(5) 0.070(5) 0.005(4) 0.025(4) -0.012(4) S1 0.0896(14) 0.0549(11) 0.0579(11) 0.0059(10) 0.0386(11) 0.0105(10) O1 0.116(4) 0.062(3) 0.060(3) 0.017(3) 0.048(3) 0.014(3) C17 0.165(10) 0.053(5) 0.095(6) -0.001(5) 0.079(7) 0.008(5) C18 0.096(7) 0.122(8) 0.096(7) 0.011(6) 0.059(6) 0.022(6) P1 0.115(2) 0.0535(13) 0.0707(14) -0.0056(12) 0.0365(14) 0.0012(13) F1 0.243(8) 0.062(3) 0.094(4) 0.005(3) 0.033(5) -0.014(4) F2 0.233(10) 0.226(10) 0.202(9) 0.045(8) -0.002(8) -0.141(9) F3 0.354(11) 0.062(4) 0.086(4) 0.018(3) 0.055(6) 0.025(5) F4 0.104(6) 0.291(13) 0.285(13) 0.022(11) -0.006(7) -0.029(7) F5 0.396(13) 0.091(5) 0.168(7) 0.006(5) 0.186(8) 0.036(7) F6 0.435(15) 0.095(5) 0.216(9) 0.004(6) 0.224(10) 0.064(8) P2 0.0899(19) 0.095(2) 0.0916(18) -0.0254(18) 0.0326(16) -0.0153(16) F7 0.304(16) 0.373(19) 0.288(15) 0.228(15) 0.008(14) -0.074(15) F8 0.109(6) 0.310(13) 0.273(10) -0.176(10) 0.073(6) -0.072(7) F9 0.373(18) 0.289(15) 0.45(2) 0.215(16) 0.251(17) 0.198(15) F10 0.237(10) 0.367(15) 0.159(7) -0.113(9) 0.101(7) -0.218(11) F11 0.172(7) 0.289(12) 0.159(7) -0.101(7) 0.087(6) -0.033(7) F12 0.162(8) 0.447(19) 0.267(12) -0.245(14) 0.073(8) -0.007(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.068(6) . ? Ru N1 2.071(6) . ? Ru N4 2.106(6) . ? Ru N3 2.124(6) . ? Ru N5 2.148(5) . ? Ru S1 2.2235(18) . ? N1 C5 1.363(9) . ? N1 C1 1.369(9) . ? N2 C6 1.364(9) . ? N2 C10 1.377(9) . ? C1 C2 1.370(11) . ? C1 H1 0.9300 . ? C2 C3 1.365(13) . ? C2 H2 0.9300 . ? C3 C4 1.422(13) . ? C3 H3 0.9300 . ? C4 C5 1.381(10) . ? C4 H4 0.9300 . ? C5 C6 1.449(10) . ? C6 C7 1.369(11) . ? C7 C8 1.387(12) . ? C7 H7 0.9300 . ? C8 C9 1.380(12) . ? C8 H8 0.9300 . ? C9 C10 1.383(11) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? N3 C16 1.497(9) . ? N3 C11 1.504(10) . ? N3 H3A 0.9100 . ? N4 C12 1.479(9) . ? N4 C13 1.513(9) . ? N4 H4A 0.9100 . ? N5 C14 1.474(9) . ? N5 C15 1.486(9) . ? N5 H5 0.9100 . ? C11 C12 1.518(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.506(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.487(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? S1 O1 1.498(5) . ? S1 C18 1.777(9) . ? S1 C17 1.793(8) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? P1 F4 1.468(9) . ? P1 F5 1.499(6) . ? P1 F2 1.532(8) . ? P1 F3 1.549(6) . ? P1 F6 1.549(7) . ? P1 F1 1.581(6) . ? P2 F7 1.425(11) . ? P2 F9 1.465(12) . ? P2 F12 1.465(8) . ? P2 F10 1.494(8) . ? P2 F8 1.512(8) . ? P2 F11 1.533(8) . ? O1W O2W 1.187(19) . ? 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 77.8(2) . . ? N2 Ru N4 99.8(2) . . ? N1 Ru N4 174.9(2) . . ? N2 Ru N3 168.2(2) . . ? N1 Ru N3 100.4(2) . . ? N4 Ru N3 81.1(2) . . ? N2 Ru N5 88.1(2) . . ? N1 Ru N5 94.8(2) . . ? N4 Ru N5 80.6(2) . . ? N3 Ru N5 80.4(2) . . ? N2 Ru S1 92.79(16) . . ? N1 Ru S1 92.69(16) . . ? N4 Ru S1 91.93(16) . . ? N3 Ru S1 98.99(16) . . ? N5 Ru S1 172.50(16) . . ? C5 N1 C1 118.7(7) . . ? C5 N1 Ru 114.9(5) . . ? C1 N1 Ru 126.3(6) . . ? C6 N2 C10 118.4(7) . . ? C6 N2 Ru 115.4(5) . . ? C10 N2 Ru 125.5(5) . . ? N1 C1 C2 122.5(9) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 118.4(9) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 120.9(9) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 117.5(9) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? N1 C5 C4 121.8(8) . . ? N1 C5 C6 115.7(6) . . ? C4 C5 C6 122.2(8) . . ? N2 C6 C7 122.2(7) . . ? N2 C6 C5 113.9(7) . . ? C7 C6 C5 123.8(8) . . ? C6 C7 C8 118.6(8) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C9 C8 C7 120.7(8) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 118.6(8) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 121.3(8) . . ? N2 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C16 N3 C11 111.2(6) . . ? C16 N3 Ru 105.3(4) . . ? C11 N3 Ru 112.6(5) . . ? C16 N3 H3A 109.2 . . ? C11 N3 H3A 109.2 . . ? Ru N3 H3A 109.2 . . ? C12 N4 C13 111.2(6) . . ? C12 N4 Ru 106.7(5) . . ? C13 N4 Ru 111.7(4) . . ? C12 N4 H4A 109.1 . . ? C13 N4 H4A 109.1 . . ? Ru N4 H4A 109.1 . . ? C14 N5 C15 112.8(6) . . ? C14 N5 Ru 105.5(4) . . ? C15 N5 Ru 111.6(4) . . ? C14 N5 H5 109.0 . . ? C15 N5 H5 109.0 . . ? Ru N5 H5 109.0 . . ? N3 C11 C12 109.4(6) . . ? N3 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? N3 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? N4 C12 C11 112.2(6) . . ? N4 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? N4 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 N4 111.0(6) . . ? C14 C13 H13A 109.4 . . ? N4 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? N4 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N5 C14 C13 110.0(6) . . ? N5 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? N5 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? N5 C15 C16 110.4(6) . . ? N5 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? N5 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C15 C16 N3 110.9(6) . . ? C15 C16 H16A 109.5 . . ? N3 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? O1 S1 C18 106.2(4) . . ? O1 S1 C17 106.7(4) . . ? C18 S1 C17 97.8(5) . . ? O1 S1 Ru 114.8(2) . . ? C18 S1 Ru 114.2(3) . . ? C17 S1 Ru 115.5(3) . . ? S1 C17 H17A 109.5 . . ? S1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S1 C18 H18A 109.5 . . ? S1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? S1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? F4 P1 F5 86.0(7) . . ? F4 P1 F2 174.4(8) . . ? F5 P1 F2 99.2(7) . . ? F4 P1 F3 93.1(6) . . ? F5 P1 F3 91.8(4) . . ? F2 P1 F3 88.8(5) . . ? F4 P1 F6 92.6(7) . . ? F5 P1 F6 177.0(5) . . ? F2 P1 F6 82.1(6) . . ? F3 P1 F6 90.9(4) . . ? F4 P1 F1 88.2(5) . . ? F5 P1 F1 90.3(4) . . ? F2 P1 F1 89.8(5) . . ? F3 P1 F1 177.6(3) . . ? F6 P1 F1 87.0(4) . . ? F7 P2 F9 175.8(9) . . ? F7 P2 F12 93.3(10) . . ? F9 P2 F12 85.9(9) . . ? F7 P2 F10 90.8(7) . . ? F9 P2 F10 85.2(9) . . ? F12 P2 F10 90.6(6) . . ? F7 P2 F8 83.5(8) . . ? F9 P2 F8 100.6(9) . . ? F12 P2 F8 92.3(5) . . ? F10 P2 F8 173.7(8) . . ? F7 P2 F11 98.8(9) . . ? F9 P2 F11 82.4(7) . . ? F12 P2 F11 167.1(9) . . ? F10 P2 F11 93.8(5) . . ? F8 P2 F11 84.5(5) . . ? 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 C5 10.4(5) . . . . ? N4 Ru N1 C5 -52(3) . . . . ? N3 Ru N1 C5 -157.7(5) . . . . ? N5 Ru N1 C5 -76.7(5) . . . . ? S1 Ru N1 C5 102.6(5) . . . . ? N2 Ru N1 C1 -166.0(6) . . . . ? N4 Ru N1 C1 132(2) . . . . ? N3 Ru N1 C1 26.0(6) . . . . ? N5 Ru N1 C1 107.0(6) . . . . ? S1 Ru N1 C1 -73.7(6) . . . . ? N1 Ru N2 C6 -13.9(5) . . . . ? N4 Ru N2 C6 161.5(5) . . . . ? N3 Ru N2 C6 68.3(13) . . . . ? N5 Ru N2 C6 81.4(5) . . . . ? S1 Ru N2 C6 -106.1(5) . . . . ? N1 Ru N2 C10 175.7(6) . . . . ? N4 Ru N2 C10 -8.9(6) . . . . ? N3 Ru N2 C10 -102.1(12) . . . . ? N5 Ru N2 C10 -89.0(6) . . . . ? S1 Ru N2 C10 83.6(6) . . . . ? C5 N1 C1 C2 0.7(11) . . . . ? Ru N1 C1 C2 176.9(6) . . . . ? N1 C1 C2 C3 3.1(13) . . . . ? C1 C2 C3 C4 -4.4(14) . . . . ? C2 C3 C4 C5 1.9(14) . . . . ? C1 N1 C5 C4 -3.4(10) . . . . ? Ru N1 C5 C4 -180.0(6) . . . . ? C1 N1 C5 C6 171.0(6) . . . . ? Ru N1 C5 C6 -5.7(8) . . . . ? C3 C4 C5 N1 2.1(12) . . . . ? C3 C4 C5 C6 -171.9(8) . . . . ? C10 N2 C6 C7 4.7(10) . . . . ? Ru N2 C6 C7 -166.4(6) . . . . ? C10 N2 C6 C5 -173.8(6) . . . . ? Ru N2 C6 C5 15.1(7) . . . . ? N1 C5 C6 N2 -6.1(9) . . . . ? C4 C5 C6 N2 168.2(7) . . . . ? N1 C5 C6 C7 175.3(7) . . . . ? C4 C5 C6 C7 -10.4(12) . . . . ? N2 C6 C7 C8 -1.9(12) . . . . ? C5 C6 C7 C8 176.5(8) . . . . ? C6 C7 C8 C9 -1.5(14) . . . . ? C7 C8 C9 C10 1.8(13) . . . . ? C6 N2 C10 C9 -4.2(11) . . . . ? Ru N2 C10 C9 165.8(6) . . . . ? C8 C9 C10 N2 1.0(12) . . . . ? N2 Ru N3 C16 -17.0(14) . . . . ? N1 Ru N3 C16 62.8(5) . . . . ? N4 Ru N3 C16 -112.2(5) . . . . ? N5 Ru N3 C16 -30.3(5) . . . . ? S1 Ru N3 C16 157.2(4) . . . . ? N2 Ru N3 C11 104.3(12) . . . . ? N1 Ru N3 C11 -175.8(5) . . . . ? N4 Ru N3 C11 9.2(5) . . . . ? N5 Ru N3 C11 91.0(5) . . . . ? S1 Ru N3 C11 -81.4(5) . . . . ? N2 Ru N4 C12 162.3(4) . . . . ? N1 Ru N4 C12 -137(3) . . . . ? N3 Ru N4 C12 -29.7(5) . . . . ? N5 Ru N4 C12 -111.3(5) . . . . ? S1 Ru N4 C12 69.1(4) . . . . ? N2 Ru N4 C13 -76.1(5) . . . . ? N1 Ru N4 C13 -15(3) . . . . ? N3 Ru N4 C13 92.0(5) . . . . ? N5 Ru N4 C13 10.3(5) . . . . ? S1 Ru N4 C13 -169.2(5) . . . . ? N2 Ru N5 C14 67.7(5) . . . . ? N1 Ru N5 C14 145.2(5) . . . . ? N4 Ru N5 C14 -32.6(5) . . . . ? N3 Ru N5 C14 -115.0(5) . . . . ? S1 Ru N5 C14 -29.3(15) . . . . ? N2 Ru N5 C15 -169.5(5) . . . . ? N1 Ru N5 C15 -92.0(5) . . . . ? N4 Ru N5 C15 90.2(5) . . . . ? N3 Ru N5 C15 7.8(5) . . . . ? S1 Ru N5 C15 93.5(13) . . . . ? C16 N3 C11 C12 131.1(7) . . . . ? Ru N3 C11 C12 13.2(8) . . . . ? C13 N4 C12 C11 -75.1(8) . . . . ? Ru N4 C12 C11 46.9(7) . . . . ? N3 C11 C12 N4 -40.0(9) . . . . ? C12 N4 C13 C14 132.9(7) . . . . ? Ru N4 C13 C14 13.9(8) . . . . ? C15 N5 C14 C13 -72.2(7) . . . . ? Ru N5 C14 C13 49.9(7) . . . . ? N4 C13 C14 N5 -43.1(9) . . . . ? C14 N5 C15 C16 135.9(7) . . . . ? Ru N5 C15 C16 17.3(7) . . . . ? N5 C15 C16 N3 -45.3(9) . . . . ? C11 N3 C16 C15 -72.2(8) . . . . ? Ru N3 C16 C15 50.1(7) . . . . ? N2 Ru S1 O1 -76.6(3) . . . . ? N1 Ru S1 O1 -154.4(3) . . . . ? N4 Ru S1 O1 23.3(3) . . . . ? N3 Ru S1 O1 104.6(3) . . . . ? N5 Ru S1 O1 20.1(13) . . . . ? N2 Ru S1 C18 46.4(4) . . . . ? N1 Ru S1 C18 -31.4(4) . . . . ? N4 Ru S1 C18 146.3(4) . . . . ? N3 Ru S1 C18 -132.4(4) . . . . ? N5 Ru S1 C18 143.1(13) . . . . ? N2 Ru S1 C17 158.7(4) . . . . ? N1 Ru S1 C17 80.8(4) . . . . ? N4 Ru S1 C17 -101.4(4) . . . . ? N3 Ru S1 C17 -20.1(4) . . . . ? N5 Ru S1 C17 -104.6(13) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.926 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.108 #===END data_13 _database_code_depnum_ccdc_archive 'CCDC 872724' #TrackingRef '- CIF Rev1 DT-ART-03-2012-030654.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H23 Cl2 N5 Ru, H2 O' _chemical_formula_sum 'C16 H25 Cl2 N5 O Ru' _chemical_formula_weight 475.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.770(2) _cell_length_b 13.218(3) _cell_length_c 18.553(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.24(2) _cell_angle_gamma 90.00 _cell_volume 1894.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 9.419 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6411 _exptl_absorpt_correction_T_max 0.7140 _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 100(2) _diffrn_radiation_wavelength 0.8000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Elettra Synchrotron, Trieste (Italy)' _diffrn_radiation_monochromator Si111 _diffrn_measurement_device_type 'MarResearch CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9370 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 28.20 _reflns_number_total 3130 _reflns_number_gt 1845 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.80.05 (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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1154P)^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 3130 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1413 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 0.38776(10) 0.38032(6) 0.36358(4) 0.0343(6) Uani 1 1 d . . . Cl1 Cl 0.6370(3) 0.48681(19) 0.40044(14) 0.0372(8) Uani 1 1 d . . . N1 N 0.5287(10) 0.2967(7) 0.2993(5) 0.030(2) Uani 1 1 d . . . N2 N 0.4903(10) 0.2734(6) 0.4347(6) 0.035(2) Uani 1 1 d . . . N3 N 0.2709(9) 0.4861(6) 0.2866(4) 0.033(2) Uani 1 1 d . . . H3 H 0.3484 0.5011 0.2533 0.040 Uiso 1 1 calc R . . N4 N 0.2266(10) 0.4586(6) 0.4293(4) 0.033(2) Uani 1 1 d . . . H4 H 0.2931 0.4766 0.4721 0.039 Uiso 1 1 calc R . . N5 N 0.1581(10) 0.3030(6) 0.3334(5) 0.033(2) Uani 1 1 d . . . H5 H 0.1791 0.2338 0.3366 0.040 Uiso 1 1 calc R . . C1 C 0.5516(13) 0.3190(8) 0.2313(7) 0.036(3) Uani 1 1 d . . . H1 H 0.5026 0.3800 0.2113 0.044 Uiso 1 1 calc R . . C2 C 0.6439(15) 0.2578(10) 0.1875(7) 0.049(3) Uani 1 1 d . . . H2 H 0.6559 0.2763 0.1388 0.059 Uiso 1 1 calc R . . C3 C 0.7177(14) 0.1692(10) 0.2171(8) 0.047(3) Uani 1 1 d . . . H3A H 0.7810 0.1252 0.1892 0.057 Uiso 1 1 calc R . . C4 C 0.6960(14) 0.1473(9) 0.2881(8) 0.047(3) Uani 1 1 d . . . H4A H 0.7485 0.0884 0.3101 0.057 Uiso 1 1 calc R . . C5 C 0.5971(14) 0.2109(9) 0.3286(8) 0.040(3) Uani 1 1 d . . . C6 C 0.5764(13) 0.1981(9) 0.4054(7) 0.035(3) Uani 1 1 d . . . C7 C 0.6444(14) 0.1147(8) 0.4470(9) 0.048(4) Uani 1 1 d . . . H7 H 0.7002 0.0609 0.4248 0.058 Uiso 1 1 calc R . . C8 C 0.6281(16) 0.1130(9) 0.5201(8) 0.048(3) Uani 1 1 d . . . H8 H 0.6716 0.0578 0.5494 0.058 Uiso 1 1 calc R . . C9 C 0.5473(16) 0.1930(11) 0.5497(7) 0.053(3) Uani 1 1 d . . . H9 H 0.5381 0.1949 0.6003 0.064 Uiso 1 1 calc R . . C10 C 0.4797(14) 0.2707(9) 0.5056(8) 0.041(3) Uani 1 1 d . . . H10 H 0.4228 0.3248 0.5270 0.049 Uiso 1 1 calc R . . C11 C 0.2384(12) 0.5794(8) 0.3282(6) 0.031(3) Uani 1 1 d . . . H11A H 0.1637 0.6261 0.2971 0.038 Uiso 1 1 calc R . . H11B H 0.3495 0.6141 0.3430 0.038 Uiso 1 1 calc R . . C12 C 0.1516(13) 0.5530(8) 0.3946(6) 0.043(3) Uani 1 1 d . . . H12A H 0.1667 0.6095 0.4298 0.052 Uiso 1 1 calc R . . H12B H 0.0260 0.5435 0.3807 0.052 Uiso 1 1 calc R . . C13 C 0.0925(14) 0.3851(7) 0.4477(7) 0.040(3) Uani 1 1 d . . . H13A H -0.0014 0.4215 0.4688 0.048 Uiso 1 1 calc R . . H13B H 0.1446 0.3361 0.4840 0.048 Uiso 1 1 calc R . . C14 C 0.0190(14) 0.3296(8) 0.3799(6) 0.047(3) Uani 1 1 d . . . H14A H -0.0391 0.2669 0.3937 0.056 Uiso 1 1 calc R . . H14B H -0.0687 0.3726 0.3519 0.056 Uiso 1 1 calc R . . C15 C 0.1089(14) 0.3304(8) 0.2563(6) 0.039(3) Uani 1 1 d . . . H15A H -0.0084 0.3042 0.2402 0.047 Uiso 1 1 calc R . . H15B H 0.1911 0.2990 0.2257 0.047 Uiso 1 1 calc R . . C16 C 0.1113(13) 0.4424(8) 0.2474(5) 0.034(3) Uani 1 1 d . . . H16A H 0.1059 0.4595 0.1953 0.040 Uiso 1 1 calc R . . H16B H 0.0085 0.4721 0.2666 0.040 Uiso 1 1 calc R . . Cl3 Cl 0.1042(3) 0.0619(2) 0.36630(15) 0.0458(9) Uani 1 1 d . . . O1 O 0.6092(13) 0.3888(7) 0.0409(5) 0.088(3) Uani 1 1 d . . . H1W H 0.5488 0.4375 0.0627 0.132 Uiso 1 1 d R . . H2W H 0.6082 0.4026 -0.0106 0.132 Uiso 1 1 d 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 0.0281(8) 0.0374(8) 0.0391(8) -0.0003(4) 0.0109(5) 0.0012(4) Cl1 0.0291(16) 0.0451(17) 0.0387(19) -0.0008(13) 0.0101(13) -0.0038(13) N1 0.035(6) 0.042(7) 0.018(7) -0.004(5) 0.020(5) 0.004(5) N2 0.031(6) 0.035(6) 0.042(8) 0.003(5) 0.024(5) 0.004(5) N3 0.021(5) 0.042(6) 0.038(6) -0.002(5) 0.005(5) -0.004(4) N4 0.026(5) 0.040(5) 0.035(6) 0.002(5) 0.015(4) 0.000(5) N5 0.023(5) 0.034(5) 0.045(7) -0.002(4) 0.014(5) 0.000(4) C1 0.028(7) 0.035(7) 0.046(10) -0.018(7) 0.004(7) 0.002(6) C2 0.042(8) 0.059(9) 0.048(9) -0.003(8) 0.010(7) -0.015(7) C3 0.038(8) 0.059(10) 0.047(11) -0.019(8) 0.010(7) -0.005(7) C4 0.028(7) 0.041(8) 0.074(12) -0.021(8) 0.007(8) 0.000(6) C5 0.023(7) 0.034(8) 0.061(12) -0.006(8) -0.003(7) 0.000(6) C6 0.025(7) 0.042(9) 0.035(10) -0.001(8) -0.006(7) -0.004(6) C7 0.035(8) 0.045(9) 0.063(12) -0.002(7) 0.003(8) 0.001(6) C8 0.050(9) 0.049(10) 0.043(11) 0.017(7) -0.007(8) 0.002(7) C9 0.057(8) 0.056(9) 0.048(9) 0.000(9) 0.019(8) -0.006(7) C10 0.038(8) 0.040(8) 0.047(10) 0.003(7) 0.015(7) 0.009(6) C11 0.017(6) 0.029(7) 0.048(8) -0.003(6) 0.005(6) -0.001(5) C12 0.036(7) 0.046(8) 0.049(8) -0.001(6) 0.008(7) 0.007(6) C13 0.031(7) 0.041(7) 0.050(9) -0.002(6) 0.007(6) 0.001(6) C14 0.033(7) 0.046(8) 0.063(9) 0.003(7) 0.011(8) 0.002(6) C15 0.034(7) 0.050(8) 0.033(9) -0.003(6) 0.001(6) -0.002(6) C16 0.030(7) 0.048(8) 0.025(7) 0.002(5) 0.013(6) -0.003(6) Cl3 0.0457(18) 0.0484(18) 0.0453(19) 0.0008(14) 0.0128(15) 0.0084(13) O1 0.099(8) 0.100(8) 0.071(7) 0.011(5) 0.031(6) 0.015(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.032(8) . ? Ru1 N2 2.036(9) . ? Ru1 N5 2.080(8) . ? Ru1 N4 2.111(7) . ? Ru1 N3 2.130(8) . ? Ru1 Cl1 2.431(3) . ? N1 C1 1.326(13) . ? N1 C5 1.341(13) . ? N2 C10 1.327(13) . ? N2 C6 1.346(13) . ? N3 C16 1.484(12) . ? N3 C11 1.491(12) . ? N3 H3 0.9300 . ? N4 C13 1.490(12) . ? N4 C12 1.494(12) . ? N4 H4 0.9300 . ? N5 C15 1.485(12) . ? N5 C14 1.496(13) . ? N5 H5 0.9300 . ? C1 C2 1.399(15) . ? C1 H1 0.9500 . ? C2 C3 1.391(16) . ? C2 H2 0.9500 . ? C3 C4 1.376(16) . ? C3 H3A 0.9500 . ? C4 C5 1.410(15) . ? C4 H4A 0.9500 . ? C5 C6 1.462(16) . ? C6 C7 1.415(15) . ? C7 C8 1.376(17) . ? C7 H7 0.9500 . ? C8 C9 1.375(16) . ? C8 H8 0.9500 . ? C9 C10 1.380(15) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.507(14) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.513(15) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.490(15) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O1 H1W 0.9166 . ? O1 H2W 0.9713 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N2 78.7(4) . . ? N1 Ru1 N5 94.4(3) . . ? N2 Ru1 N5 95.6(3) . . ? N1 Ru1 N4 175.6(3) . . ? N2 Ru1 N4 100.4(4) . . ? N5 Ru1 N4 81.4(3) . . ? N1 Ru1 N3 100.4(4) . . ? N2 Ru1 N3 176.9(3) . . ? N5 Ru1 N3 81.4(3) . . ? N4 Ru1 N3 80.2(3) . . ? N1 Ru1 Cl1 90.9(2) . . ? N2 Ru1 Cl1 88.6(2) . . ? N5 Ru1 Cl1 173.8(2) . . ? N4 Ru1 Cl1 93.3(2) . . ? N3 Ru1 Cl1 94.4(2) . . ? C1 N1 C5 119.0(9) . . ? C1 N1 Ru1 125.0(8) . . ? C5 N1 Ru1 116.0(8) . . ? C10 N2 C6 117.8(9) . . ? C10 N2 Ru1 126.8(8) . . ? C6 N2 Ru1 115.4(8) . . ? C16 N3 C11 113.3(7) . . ? C16 N3 Ru1 110.2(6) . . ? C11 N3 Ru1 106.2(6) . . ? C16 N3 H3 109.0 . . ? C11 N3 H3 109.0 . . ? Ru1 N3 H3 109.0 . . ? C13 N4 C12 113.1(7) . . ? C13 N4 Ru1 106.6(6) . . ? C12 N4 Ru1 112.8(6) . . ? C13 N4 H4 108.0 . . ? C12 N4 H4 108.0 . . ? Ru1 N4 H4 108.0 . . ? C15 N5 C14 111.9(8) . . ? C15 N5 Ru1 105.3(6) . . ? C14 N5 Ru1 112.4(6) . . ? C15 N5 H5 109.1 . . ? C14 N5 H5 109.1 . . ? Ru1 N5 H5 109.1 . . ? N1 C1 C2 123.6(10) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 118.3(11) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C4 C3 C2 117.8(11) . . ? C4 C3 H3A 121.1 . . ? C2 C3 H3A 121.1 . . ? C3 C4 C5 121.0(12) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? N1 C5 C4 120.3(12) . . ? N1 C5 C6 114.3(10) . . ? C4 C5 C6 125.1(13) . . ? N2 C6 C7 121.9(11) . . ? N2 C6 C5 114.8(10) . . ? C7 C6 C5 123.2(12) . . ? C8 C7 C6 118.8(11) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 118.4(10) . . ? C9 C8 H8 120.8 . . ? C7 C8 H8 120.8 . . ? C8 C9 C10 119.8(11) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N2 C10 C9 123.1(11) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? N3 C11 C12 110.4(8) . . ? N3 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? N3 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N4 C12 C11 110.9(8) . . ? N4 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? N4 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.0 . . ? N4 C13 C14 109.7(9) . . ? N4 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? N4 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? N5 C14 C13 111.2(8) . . ? N5 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? N5 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? N5 C15 C16 110.0(8) . . ? N5 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? N5 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N3 C16 C15 110.6(8) . . ? N3 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? H1W O1 H2W 110.6 . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.987 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.163