# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 1999 # CCDC Number: 440/135 data_S1 #*complex 1* _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H22 Cl F6 O P Ru S5' _chemical_formula_weight 600.07 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' 'O' 'O' 0.0106 0.0060 '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' '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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x, -y+1/2, z' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z-1/2' '-x, y-1/2, -z' 'x-1/2, y, -z-1/2' _cell_length_a 9.210(10) _cell_length_b 9.779(11) _cell_length_c 22.60(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2035(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.958 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 1.544 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5300 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.89 _reflns_number_total 1885 _reflns_number_gt 1763 _reflns_threshold_expression 2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+5.3533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0070(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1885 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 0.721 _refine_ls_restrained_S_all 0.721 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.10796(3) 0.7500 0.886281(11) 0.02012(16) Uani 1 d S . . S1 S -0.14096(11) 0.7500 0.86302(4) 0.0317(3) Uani 1 d S . . C2 C -0.2010(4) 0.8993(4) 0.90431(15) 0.0457(8) Uani 1 d . . . H2A H -0.3041 0.9141 0.8984 0.055 Uiso 1 calc R . . H2B H -0.1833 0.8865 0.9463 0.055 Uiso 1 calc R . . C3 C -0.1156(4) 1.0194(5) 0.88153(17) 0.0511(10) Uani 1 d . . . H3A H -0.1350 1.0978 0.9066 0.061 Uiso 1 calc R . . H3B H -0.1493 1.0414 0.8420 0.061 Uiso 1 calc R . . S4 S 0.08337(9) 0.99036(9) 0.87894(3) 0.0358(2) Uani 1 d . . . C5 C 0.1200(5) 1.0177(4) 0.79945(15) 0.0497(9) Uani 1 d . . . H5A H 0.0679 1.0986 0.7865 0.060 Uiso 1 calc R . . H5B H 0.2229 1.0351 0.7942 0.060 Uiso 1 calc R . . C6 C 0.0764(4) 0.8979(4) 0.76024(13) 0.0439(8) Uani 1 d . . . H6A H 0.1041 0.9150 0.7195 0.053 Uiso 1 calc R . . H6B H -0.0277 0.8835 0.7619 0.053 Uiso 1 calc R . . S7 S 0.17187(11) 0.7500 0.78888(4) 0.0307(3) Uani 1 d S . . Cl Cl 0.04844(12) 0.7500 0.99156(4) 0.0414(3) Uani 1 d S . . S8 S 0.34785(10) 0.7500 0.91309(4) 0.0247(2) Uani 1 d S . . O81 O 0.4616(3) 0.7500 0.86669(13) 0.0390(7) Uani 1 d S . . C92 C 0.3864(4) 0.6109(4) 0.96169(14) 0.0399(8) Uani 1 d . . . H92A H 0.3169 0.6099 0.9933 0.048 Uiso 1 calc R . . H92B H 0.4823 0.6214 0.9777 0.048 Uiso 1 calc R . . H92C H 0.3808 0.5264 0.9401 0.048 Uiso 1 calc R . . P P 0.50680(13) 1.2500 0.85022(5) 0.0358(3) Uani 1 d S . . F11 F 0.3666(5) 1.2500 0.8891(3) 0.111(2) Uani 1 d S . . F12 F 0.4159(5) 1.2500 0.7912(2) 0.1102(18) Uani 1 d S . . F13 F 0.5054(4) 1.4108(3) 0.84941(16) 0.1089(13) Uani 1 d . . . F14 F 0.6487(4) 1.2500 0.81045(16) 0.0793(12) Uani 1 d S . . F15 F 0.6049(6) 1.2500 0.90647(18) 0.124(2) Uani 1 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 0.0182(2) 0.0255(2) 0.01659(19) 0.000 -0.00080(9) 0.000 S1 0.0206(5) 0.0432(6) 0.0311(5) 0.000 -0.0033(4) 0.000 C2 0.0289(16) 0.062(2) 0.0458(17) -0.0094(16) 0.0008(13) 0.0161(16) C3 0.048(2) 0.042(2) 0.063(2) -0.0127(17) -0.0122(16) 0.0215(17) S4 0.0397(5) 0.0285(5) 0.0392(4) -0.0027(3) -0.0092(3) 0.0018(3) C5 0.063(2) 0.037(2) 0.0489(19) 0.0149(16) -0.0069(16) -0.0087(17) C6 0.055(2) 0.051(2) 0.0261(14) 0.0141(14) -0.0075(13) -0.0023(17) S7 0.0293(6) 0.0438(6) 0.0189(4) 0.000 0.0009(3) 0.000 Cl 0.0361(6) 0.0690(8) 0.0191(4) 0.000 0.0028(4) 0.000 S8 0.0201(5) 0.0323(6) 0.0216(4) 0.000 -0.0022(3) 0.000 O81 0.0255(16) 0.059(2) 0.0320(14) 0.000 0.0060(12) 0.000 C92 0.0395(18) 0.044(2) 0.0360(16) 0.0083(14) -0.0075(12) 0.0076(15) P 0.0375(7) 0.0302(6) 0.0397(6) 0.000 0.0021(5) 0.000 F11 0.084(3) 0.089(4) 0.161(5) 0.000 0.079(3) 0.000 F12 0.078(3) 0.153(5) 0.100(3) 0.000 -0.048(3) 0.000 F13 0.162(4) 0.0367(15) 0.128(3) -0.0029(16) 0.046(3) -0.0079(18) F14 0.055(2) 0.127(4) 0.056(2) 0.000 0.0159(17) 0.000 F15 0.122(4) 0.212(7) 0.0374(19) 0.000 -0.021(2) 0.000 _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 S7 2.278(2) . ? Ru S8 2.291(3) . ? Ru S1 2.352(3) . ? Ru S4 2.367(3) 3_565 ? Ru S4 2.367(3) . ? Ru Cl 2.441(3) . ? S1 C2 1.818(4) . ? S1 C2 1.818(4) 3_565 ? C2 C3 1.504(6) . ? C3 S4 1.855(4) . ? S4 C5 1.847(4) . ? C5 C6 1.523(5) . ? C6 S7 1.812(4) . ? S7 C6 1.812(4) 3_565 ? S8 O81 1.482(3) . ? S8 C92 1.784(3) . ? S8 C92 1.784(3) 3_565 ? P F15 1.560(4) . ? P F11 1.561(4) . ? P F13 1.572(3) 3_575 ? P F13 1.572(3) . ? P F12 1.574(4) . ? P F14 1.586(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S7 Ru S8 90.36(6) . . ? S7 Ru S1 92.06(5) . . ? S8 Ru S1 177.58(3) . . ? S7 Ru S4 87.54(2) . 3_565 ? S8 Ru S4 96.36(2) . 3_565 ? S1 Ru S4 83.75(2) . 3_565 ? S7 Ru S4 87.54(2) . . ? S8 Ru S4 96.36(2) . . ? S1 Ru S4 83.75(2) . . ? S4 Ru S4 166.38(5) 3_565 . ? S7 Ru Cl 178.00(4) . . ? S8 Ru Cl 87.64(5) . . ? S1 Ru Cl 89.94(5) . . ? S4 Ru Cl 92.68(2) 3_565 . ? S4 Ru Cl 92.68(2) . . ? C2 S1 C2 106.8(3) . 3_565 ? C2 S1 Ru 100.46(12) . . ? C2 S1 Ru 100.46(12) 3_565 . ? C3 C2 S1 107.0(2) . . ? C2 C3 S4 114.1(3) . . ? C5 S4 C3 100.88(18) . . ? C5 S4 Ru 101.22(12) . . ? C3 S4 Ru 104.13(15) . . ? C6 C5 S4 114.0(2) . . ? C5 C6 S7 106.2(2) . . ? C6 S7 C6 105.9(2) 3_565 . ? C6 S7 Ru 102.70(11) 3_565 . ? C6 S7 Ru 102.70(11) . . ? O81 S8 C92 107.14(15) . . ? O81 S8 C92 107.14(15) . 3_565 ? C92 S8 C92 99.4(2) . 3_565 ? O81 S8 Ru 119.65(15) . . ? C92 S8 Ru 110.78(12) . . ? C92 S8 Ru 110.78(12) 3_565 . ? F15 P F11 91.2(3) . . ? F15 P F13 90.82(16) . 3_575 ? F11 P F13 89.97(13) . 3_575 ? F15 P F13 90.82(16) . . ? F11 P F13 89.97(13) . . ? F13 P F13 178.4(3) 3_575 . ? F15 P F12 176.7(3) . . ? F11 P F12 92.1(3) . . ? F13 P F12 89.18(15) 3_575 . ? F13 P F12 89.18(15) . . ? F15 P F14 89.1(3) . . ? F11 P F14 179.7(3) . . ? F13 P F14 90.02(13) 3_575 . ? F13 P F14 90.02(13) . . ? F12 P F14 87.6(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 S1 C2 C3 S4 -50.3(3) . . . . ? C2 C3 S4 C5 121.2(3) . . . . ? C3 S4 C5 C6 -77.1(3) . . . . ? S4 C5 C6 S7 -56.2(3) . . . . ? C5 C6 S7 C6 161.01(17) . . . 3_565 ? C6 S7 C6 C5 -161.01(17) . . 3_565 3_565 ? S7 C6 C5 S4 56.2(3) . 3_565 3_565 3_565 ? C6 C5 S4 C3 77.1(3) 3_565 3_565 3_565 3_565 ? C5 S4 C3 C2 -121.2(3) 3_565 3_565 3_565 3_565 ? S4 C3 C2 S1 50.3(3) 3_565 3_565 3_565 . ? C3 C2 S1 C2 -163.27(16) 3_565 3_565 . . ? C2 S1 C2 C3 163.27(16) 3_565 . . . ? _diffrn_measured_fraction_theta_max 0.874 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full 0.874 _refine_diff_density_max 0.520 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.088 #=END data_S2 #*Complex 2* _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 F12 N2 P2 Ru S4' _chemical_formula_weight 713.57 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' '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.391(11) _cell_length_b 20.94(2) _cell_length_c 11.488(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.380(10) _cell_angle_gamma 90.00 _cell_volume 2499(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 1.184 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4582 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.93 _reflns_number_total 4582 _reflns_number_gt 3723 _reflns_threshold_expression 2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+12.3182P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4582 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1713 _refine_ls_wR_factor_gt 0.1613 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.75330(5) 0.86025(2) 0.28323(4) 0.0404(2) Uani 1 d . . . S10 S 0.75279(18) 0.74830(8) 0.30947(15) 0.0500(4) Uani 1 d . . . C9A C 0.8889(8) 0.7228(4) 0.2197(7) 0.0623(19) Uani 0.591(2) d P A 1 H9A1 H 0.9651 0.7205 0.2688 0.075 Uiso 0.591(2) calc PR A 1 H9A2 H 0.8715 0.6801 0.1910 0.075 Uiso 0.591(2) calc PR A 1 C8A C 0.9180(11) 0.7654(5) 0.1171(10) 0.0461(5) Uiso 0.591(2) d P A 1 H8A1 H 0.8466 0.7650 0.0623 0.055 Uiso 0.591(2) calc PR A 1 H8A2 H 0.9945 0.7506 0.0775 0.055 Uiso 0.591(2) calc PR A 1 S7A S 0.9433(3) 0.84631(13) 0.1742(3) 0.0461(5) Uiso 0.591(2) d P A 1 C6A C 0.9159(11) 0.9009(5) 0.0536(10) 0.0461(5) Uiso 0.591(2) d P A 1 H6A1 H 0.9915 0.9035 0.0047 0.055 Uiso 0.591(2) calc PR A 1 H6A2 H 0.8434 0.8869 0.0065 0.055 Uiso 0.591(2) calc PR A 1 C5A C 0.8873(8) 0.9667(4) 0.1114(7) 0.0595(19) Uani 0.591(2) d P A 1 H5A1 H 0.8693 0.9976 0.0505 0.071 Uiso 0.591(2) calc PR A 1 H5A2 H 0.9640 0.9808 0.1525 0.071 Uiso 0.591(2) calc PR A 1 C9B C 0.8889(8) 0.7228(4) 0.2197(7) 0.0623(19) Uani 0.409(2) d P A 2 H9B1 H 0.9407 0.6924 0.2631 0.075 Uiso 0.409(2) calc PR A 2 H9B2 H 0.8565 0.7015 0.1505 0.075 Uiso 0.409(2) calc PR A 2 C8B C 0.9669(16) 0.7750(8) 0.1865(15) 0.0461(5) Uiso 0.409(2) d P A 2 H8B1 H 1.0285 0.7610 0.1288 0.055 Uiso 0.409(2) calc PR A 2 H8B2 H 1.0145 0.7905 0.2537 0.055 Uiso 0.409(2) calc PR A 2 S7B S 0.8705(4) 0.8392(2) 0.1270(4) 0.0461(5) Uiso 0.409(2) d P A 2 C6B C 0.9718(16) 0.9100(7) 0.1264(15) 0.0461(5) Uiso 0.409(2) d P A 2 H6B1 H 1.0193 0.9132 0.1992 0.055 Uiso 0.409(2) calc PR A 2 H6B2 H 1.0330 0.9076 0.0632 0.055 Uiso 0.409(2) calc PR A 2 C5B C 0.8873(8) 0.9667(4) 0.1114(7) 0.0595(19) Uani 0.409(2) d P A 2 H5B1 H 0.8539 0.9674 0.0323 0.071 Uiso 0.409(2) calc PR A 2 H5B2 H 0.9378 1.0052 0.1231 0.071 Uiso 0.409(2) calc PR A 2 S4 S 0.75215(18) 0.96639(8) 0.21369(15) 0.0496(4) Uani 1 d . . . C3A C 0.6154(7) 0.9668(4) 0.1123(7) 0.0571(18) Uani 0.591(2) d P A 1 H3A1 H 0.5654 1.0052 0.1249 0.068 Uiso 0.591(2) calc PR A 1 H3A2 H 0.6479 0.9682 0.0333 0.068 Uiso 0.591(2) calc PR A 1 C2A C 0.5284(10) 0.9098(5) 0.1241(10) 0.0437(5) Uiso 0.591(2) d P A 1 H2A1 H 0.4690 0.9077 0.0588 0.052 Uiso 0.591(2) calc PR A 1 H2A2 H 0.4791 0.9128 0.1953 0.052 Uiso 0.591(2) calc PR A 1 S1A S 0.6300(3) 0.83936(13) 0.1273(2) 0.0437(5) Uiso 0.591(2) d P A 1 C12A C 0.5305(11) 0.7756(5) 0.1854(10) 0.0437(5) Uiso 0.591(2) d P A 1 H12A H 0.4824 0.7905 0.2521 0.052 Uiso 0.591(2) calc PR A 1 H12B H 0.4702 0.7605 0.1267 0.052 Uiso 0.591(2) calc PR A 1 C11A C 0.624(7) 0.722(4) 0.221(6) 0.058(7) Uani 0.591(2) d P A 1 H11A H 0.6580 0.7020 0.1518 0.069 Uiso 0.591(2) calc PR A 1 H11B H 0.5761 0.6893 0.2634 0.069 Uiso 0.591(2) calc PR A 1 C3B C 0.6154(7) 0.9668(4) 0.1123(7) 0.0571(18) Uani 0.409(2) d P A 2 H3B1 H 0.5400 0.9814 0.1538 0.068 Uiso 0.409(2) calc PR A 2 H3B2 H 0.6328 0.9976 0.0513 0.068 Uiso 0.409(2) calc PR A 2 C2B C 0.5828(16) 0.9008(7) 0.0535(14) 0.0437(5) Uiso 0.409(2) d P A 2 H2B1 H 0.6533 0.8866 0.0051 0.052 Uiso 0.409(2) calc PR A 2 H2B2 H 0.5056 0.9041 0.0059 0.052 Uiso 0.409(2) calc PR A 2 S1B S 0.5583(4) 0.84643(19) 0.1728(4) 0.0437(5) Uiso 0.409(2) d P A 2 C12B C 0.5782(16) 0.7660(7) 0.1171(14) 0.0437(5) Uiso 0.409(2) d P A 2 H12C H 0.5007 0.7522 0.0770 0.052 Uiso 0.409(2) calc PR A 2 H12D H 0.6494 0.7643 0.0629 0.052 Uiso 0.409(2) calc PR A 2 C11B C 0.605(11) 0.724(5) 0.218(9) 0.058(7) Uani 0.409(2) d P A 2 H11C H 0.6162 0.6810 0.1910 0.069 Uiso 0.409(2) calc PR A 2 H11D H 0.5297 0.7247 0.2685 0.069 Uiso 0.409(2) calc PR A 2 P1 P 1.2517(2) 0.81598(14) -0.1126(2) 0.0745(7) Uani 1 d . . . F11 F 1.2506(8) 0.7935(4) -0.2408(6) 0.127(3) Uani 1 d . . . F12 F 1.3656(9) 0.7708(6) -0.0842(8) 0.181(4) Uani 1 d . . . F13 F 1.2533(8) 0.8383(7) 0.0134(8) 0.220(6) Uani 1 d . . . F14 F 1.3610(9) 0.8647(5) -0.1456(12) 0.197(5) Uani 1 d . . . F15 F 1.1432(10) 0.8638(5) -0.1442(10) 0.186(5) Uani 1 d . . . F16 F 1.1424(9) 0.7701(6) -0.0817(8) 0.190(5) Uani 1 d . . . P2 P 0.7491(2) 0.52490(11) 0.23633(19) 0.0627(5) Uani 1 d . . . F21 F 0.6435(7) 0.5642(4) 0.3044(7) 0.129(3) Uani 1 d . . . F22 F 0.8598(7) 0.5630(4) 0.3002(7) 0.129(3) Uani 1 d . . . F23 F 0.7469(7) 0.5782(4) 0.1398(6) 0.128(3) Uani 1 d . . . F24 F 0.7515(8) 0.4771(3) 0.3420(6) 0.122(2) Uani 1 d . . . F25 F 0.6363(9) 0.4886(4) 0.1771(7) 0.159(4) Uani 1 d . . . F26 F 0.8572(9) 0.4877(4) 0.1733(7) 0.159(3) Uani 1 d . . . N100 N 0.8929(6) 0.8780(3) 0.4105(5) 0.0533(14) Uani 1 d . . . C101 C 0.9693(7) 0.8886(4) 0.4747(7) 0.0590(19) Uani 1 d . . . C102 C 1.0735(8) 0.9028(6) 0.5592(9) 0.093(3) Uani 1 d . . . H10A H 1.1214 0.8646 0.5751 0.112 Uiso 1 calc R . . H10B H 1.0369 0.9186 0.6302 0.112 Uiso 1 calc R . . H10C H 1.1299 0.9345 0.5273 0.112 Uiso 1 calc R . . N200 N 0.6118(5) 0.8763(3) 0.4039(6) 0.0520(14) Uani 1 d . . . C201 C 0.5322(7) 0.8868(4) 0.4682(7) 0.0602(19) Uani 1 d . . . C202 C 0.4291(9) 0.9012(6) 0.5521(9) 0.095(3) Uani 1 d . . . H20A H 0.4658 0.9065 0.6284 0.114 Uiso 1 calc R . . H20B H 0.3684 0.8667 0.5531 0.114 Uiso 1 calc R . . H20C H 0.3861 0.9398 0.5293 0.114 Uiso 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 0.0502(3) 0.0419(3) 0.0292(3) 0.0004(2) -0.0010(2) -0.0005(2) S10 0.0564(10) 0.0456(9) 0.0479(9) 0.0107(7) -0.0011(8) -0.0008(7) C9A 0.061(5) 0.054(4) 0.072(5) -0.001(4) 0.001(4) 0.017(4) C5A 0.061(4) 0.058(4) 0.060(4) 0.013(4) 0.009(4) -0.010(4) C9B 0.061(5) 0.054(4) 0.072(5) -0.001(4) 0.001(4) 0.017(4) C5B 0.061(4) 0.058(4) 0.060(4) 0.013(4) 0.009(4) -0.010(4) S4 0.0623(10) 0.0407(8) 0.0458(9) 0.0001(7) -0.0009(8) 0.0000(8) C3A 0.054(4) 0.057(4) 0.060(4) 0.016(3) -0.004(3) 0.007(3) C11A 0.05(2) 0.047(7) 0.072(6) 0.002(4) -0.005(10) -0.012(11) C3B 0.054(4) 0.057(4) 0.060(4) 0.016(3) -0.004(3) 0.007(3) C11B 0.05(2) 0.047(7) 0.072(6) 0.002(4) -0.005(10) -0.012(11) P1 0.0465(11) 0.1108(19) 0.0662(14) -0.0266(13) -0.0020(10) -0.0012(12) F11 0.150(6) 0.167(7) 0.065(3) -0.032(4) -0.002(4) 0.010(5) F12 0.147(7) 0.258(12) 0.139(7) 0.017(7) -0.009(6) 0.111(8) F13 0.112(6) 0.427(17) 0.123(6) -0.160(9) -0.001(5) -0.005(8) F14 0.122(7) 0.217(11) 0.252(13) -0.040(9) 0.024(8) -0.080(7) F15 0.153(8) 0.210(11) 0.194(10) -0.033(8) -0.016(7) 0.093(7) F16 0.153(8) 0.269(12) 0.147(7) 0.020(8) 0.016(6) -0.116(8) P2 0.0721(14) 0.0624(12) 0.0536(11) 0.0081(9) 0.0002(10) -0.0007(10) F21 0.115(5) 0.136(6) 0.136(6) 0.006(5) 0.042(5) 0.041(5) F22 0.120(5) 0.131(6) 0.135(6) 0.003(5) -0.043(5) -0.031(5) F23 0.128(5) 0.153(6) 0.105(5) 0.074(5) -0.002(4) -0.002(5) F24 0.162(6) 0.108(5) 0.094(4) 0.049(4) 0.000(4) -0.001(4) F25 0.189(8) 0.167(7) 0.121(6) -0.010(5) -0.055(6) -0.082(6) F26 0.196(8) 0.145(7) 0.137(6) -0.021(5) 0.062(6) 0.070(6) N100 0.043(3) 0.062(4) 0.055(4) 0.008(3) -0.003(3) -0.004(3) C101 0.042(4) 0.081(5) 0.054(4) 0.016(4) -0.007(3) -0.013(4) C102 0.055(5) 0.144(10) 0.080(6) 0.015(6) -0.026(5) -0.026(6) N200 0.033(3) 0.066(4) 0.057(4) 0.011(3) -0.002(3) -0.004(3) C201 0.045(4) 0.077(5) 0.059(5) 0.020(4) 0.001(4) 0.003(4) C202 0.058(5) 0.138(10) 0.089(7) 0.021(7) 0.027(5) 0.038(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N200 2.055(7) . ? Ru N100 2.086(6) . ? Ru S7B 2.220(5) . ? Ru S1A 2.239(3) . ? Ru S4 2.362(3) . ? Ru S10 2.363(3) . ? Ru S7A 2.364(4) . ? Ru S1B 2.401(5) . ? S10 C11A 1.77(8) . ? S10 C9B 1.835(8) . ? S10 C9A 1.835(8) . ? S10 C11B 1.92(12) . ? C9A C8A 1.510(14) . ? C9A H9A1 0.9700 . ? C9A H9A2 0.9700 . ? C8A S7A 1.835(12) . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? S7A C6A 1.817(11) . ? C6A C5A 1.560(13) . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C5A S4 1.838(8) . ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C9B C8B 1.415(18) . ? C9B H9B1 0.9700 . ? C9B H9B2 0.9700 . ? C8B S7B 1.806(16) . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? S7B C6B 1.819(16) . ? C6B C5B 1.485(17) . ? C6B H6B1 0.9700 . ? C6B H6B2 0.9700 . ? C5B S4 1.838(8) . ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? S4 C3B 1.831(7) . ? S4 C3A 1.831(7) . ? C3A C2A 1.504(13) . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C2A S1A 1.813(11) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? S1A C12A 1.819(11) . ? C12A C11A 1.54(7) . ? C12A H12A 0.9700 . ? C12A H12B 0.9700 . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C3B C2B 1.574(17) . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C2B S1B 1.800(16) . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? S1B C12B 1.814(16) . ? C12B C11B 1.48(11) . ? C12B H12C 0.9700 . ? C12B H12D 0.9700 . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? P1 F13 1.521(8) . ? P1 F16 1.531(8) . ? P1 F11 1.547(7) . ? P1 F15 1.549(9) . ? P1 F12 1.548(8) . ? P1 F14 1.575(9) . ? P2 F26 1.551(7) . ? P2 F25 1.551(7) . ? P2 F24 1.573(6) . ? P2 F23 1.573(6) . ? P2 F22 1.576(7) . ? P2 F21 1.582(7) . ? N100 C101 1.103(9) . ? C101 C102 1.480(10) . ? C102 H10A 0.9600 . ? C102 H10B 0.9600 . ? C102 H10C 0.9600 . ? N200 C201 1.134(10) . ? C201 C202 1.477(11) . ? C202 H20A 0.9600 . ? C202 H20B 0.9600 . ? C202 H20C 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 N200 Ru N100 89.7(2) . . ? N200 Ru S7B 167.62(19) . . ? N100 Ru S7B 102.7(2) . . ? N200 Ru S1A 99.4(2) . . ? N100 Ru S1A 170.85(18) . . ? S7B Ru S1A 68.21(16) . . ? N200 Ru S4 94.13(18) . . ? N100 Ru S4 94.07(18) . . ? S7B Ru S4 85.15(12) . . ? S1A Ru S4 84.93(9) . . ? N200 Ru S10 94.26(18) . . ? N100 Ru S10 95.15(18) . . ? S7B Ru S10 84.69(12) . . ? S1A Ru S10 84.64(9) . . ? S4 Ru S10 167.55(7) . . ? N200 Ru S7A 168.99(18) . . ? N100 Ru S7A 79.3(2) . . ? S7B Ru S7A 23.39(12) . . ? S1A Ru S7A 91.60(13) . . ? S4 Ru S7A 86.52(9) . . ? S10 Ru S7A 87.01(8) . . ? N200 Ru S1B 76.8(2) . . ? N100 Ru S1B 166.5(2) . . ? S7B Ru S1B 90.82(17) . . ? S1A Ru S1B 22.62(11) . . ? S4 Ru S1B 86.11(11) . . ? S10 Ru S1B 86.87(11) . . ? S7A Ru S1B 114.21(15) . . ? C11A S10 C9B 100(2) . . ? C11A S10 C9A 100(2) . . ? C9B S10 C9A 0.0(8) . . ? C11A S10 C11B 4(5) . . ? C9B S10 C11B 104(3) . . ? C9A S10 C11B 104(3) . . ? C11A S10 Ru 104(2) . . ? C9B S10 Ru 102.4(3) . . ? C9A S10 Ru 102.4(3) . . ? C11B S10 Ru 101(3) . . ? C8A C9A S10 115.2(6) . . ? C8A C9A H9A1 108.5 . . ? S10 C9A H9A1 108.5 . . ? C8A C9A H9A2 108.5 . . ? S10 C9A H9A2 108.5 . . ? H9A1 C9A H9A2 107.5 . . ? C9A C8A S7A 107.2(7) . . ? C9A C8A H8A1 110.3 . . ? S7A C8A H8A1 110.3 . . ? C9A C8A H8A2 110.3 . . ? S7A C8A H8A2 110.3 . . ? H8A1 C8A H8A2 108.5 . . ? C6A S7A C8A 106.7(5) . . ? C6A S7A Ru 101.5(4) . . ? C8A S7A Ru 100.6(4) . . ? C5A C6A S7A 105.1(7) . . ? C5A C6A H6A1 110.7 . . ? S7A C6A H6A1 110.7 . . ? C5A C6A H6A2 110.7 . . ? S7A C6A H6A2 110.7 . . ? H6A1 C6A H6A2 108.8 . . ? C6A C5A S4 114.7(6) . . ? C6A C5A H5A1 108.6 . . ? S4 C5A H5A1 108.6 . . ? C6A C5A H5A2 108.6 . . ? S4 C5A H5A2 108.6 . . ? H5A1 C5A H5A2 107.6 . . ? C8B C9B S10 111.8(8) . . ? C8B C9B H9B1 109.3 . . ? S10 C9B H9B1 109.3 . . ? C8B C9B H9B2 109.3 . . ? S10 C9B H9B2 109.3 . . ? H9B1 C9B H9B2 107.9 . . ? C9B C8B S7B 111.1(10) . . ? C9B C8B H8B1 109.4 . . ? S7B C8B H8B1 109.4 . . ? C9B C8B H8B2 109.4 . . ? S7B C8B H8B2 109.4 . . ? H8B1 C8B H8B2 108.0 . . ? C8B S7B C6B 106.8(8) . . ? C8B S7B Ru 98.5(6) . . ? C6B S7B Ru 99.3(6) . . ? C5B C6B S7B 108.1(10) . . ? C5B C6B H6B1 110.1 . . ? S7B C6B H6B1 110.1 . . ? C5B C6B H6B2 110.1 . . ? S7B C6B H6B2 110.1 . . ? H6B1 C6B H6B2 108.4 . . ? C6B C5B S4 112.1(8) . . ? C6B C5B H5B1 109.2 . . ? S4 C5B H5B1 109.2 . . ? C6B C5B H5B2 109.2 . . ? S4 C5B H5B2 109.2 . . ? H5B1 C5B H5B2 107.9 . . ? C3B S4 C3A 0.0(7) . . ? C3B S4 C5A 100.7(4) . . ? C3A S4 C5A 100.7(4) . . ? C3B S4 C5B 100.7(4) . . ? C3A S4 C5B 100.7(4) . . ? C5A S4 C5B 0.0(7) . . ? C3B S4 Ru 102.8(2) . . ? C3A S4 Ru 102.8(2) . . ? C5A S4 Ru 102.6(2) . . ? C5B S4 Ru 102.6(2) . . ? C2A C3A S4 113.8(6) . . ? C2A C3A H3A1 108.8 . . ? S4 C3A H3A1 108.8 . . ? C2A C3A H3A2 108.8 . . ? S4 C3A H3A2 108.8 . . ? H3A1 C3A H3A2 107.7 . . ? C3A C2A S1A 107.3(7) . . ? C3A C2A H2A1 110.3 . . ? S1A C2A H2A1 110.3 . . ? C3A C2A H2A2 110.3 . . ? S1A C2A H2A2 110.3 . . ? H2A1 C2A H2A2 108.5 . . ? C2A S1A C12A 105.8(5) . . ? C2A S1A Ru 100.8(4) . . ? C12A S1A Ru 100.0(4) . . ? C11A C12A S1A 106(3) . . ? C11A C12A H12A 110.5 . . ? S1A C12A H12A 110.5 . . ? C11A C12A H12B 110.5 . . ? S1A C12A H12B 110.5 . . ? H12A C12A H12B 108.7 . . ? C12A C11A S10 113(5) . . ? C12A C11A H11A 108.9 . . ? S10 C11A H11A 108.9 . . ? C12A C11A H11B 108.9 . . ? S10 C11A H11B 108.9 . . ? H11A C11A H11B 107.7 . . ? C2B C3B S4 115.7(7) . . ? C2B C3B H3B1 108.4 . . ? S4 C3B H3B1 108.4 . . ? C2B C3B H3B2 108.4 . . ? S4 C3B H3B2 108.4 . . ? H3B1 C3B H3B2 107.4 . . ? C3B C2B S1B 105.1(9) . . ? C3B C2B H2B1 110.7 . . ? S1B C2B H2B1 110.7 . . ? C3B C2B H2B2 110.7 . . ? S1B C2B H2B2 110.7 . . ? H2B1 C2B H2B2 108.8 . . ? C2B S1B C12B 107.6(8) . . ? C2B S1B Ru 101.7(5) . . ? C12B S1B Ru 101.5(5) . . ? C11B C12B S1B 107(5) . . ? C11B C12B H12C 110.3 . . ? S1B C12B H12C 110.3 . . ? C11B C12B H12D 110.3 . . ? S1B C12B H12D 110.3 . . ? H12C C12B H12D 108.6 . . ? C12B C11B S10 115(7) . . ? C12B C11B H11C 108.6 . . ? S10 C11B H11C 108.6 . . ? C12B C11B H11D 108.6 . . ? S10 C11B H11D 108.6 . . ? H11C C11B H11D 107.6 . . ? F13 P1 F16 88.6(6) . . ? F13 P1 F11 179.8(6) . . ? F16 P1 F11 91.6(5) . . ? F13 P1 F15 91.6(6) . . ? F16 P1 F15 85.4(7) . . ? F11 P1 F15 88.4(5) . . ? F13 P1 F12 89.1(6) . . ? F16 P1 F12 97.8(7) . . ? F11 P1 F12 90.9(5) . . ? F15 P1 F12 176.7(7) . . ? F13 P1 F14 91.6(7) . . ? F16 P1 F14 178.3(7) . . ? F11 P1 F14 88.2(6) . . ? F15 P1 F14 92.9(7) . . ? F12 P1 F14 83.9(6) . . ? F26 P2 F25 95.5(6) . . ? F26 P2 F24 91.8(5) . . ? F25 P2 F24 92.0(4) . . ? F26 P2 F23 92.0(5) . . ? F25 P2 F23 91.8(5) . . ? F24 P2 F23 174.3(5) . . ? F26 P2 F22 86.7(5) . . ? F25 P2 F22 177.7(5) . . ? F24 P2 F22 87.4(4) . . ? F23 P2 F22 88.7(4) . . ? F26 P2 F21 177.4(5) . . ? F25 P2 F21 87.0(5) . . ? F24 P2 F21 87.5(4) . . ? F23 P2 F21 88.4(4) . . ? F22 P2 F21 90.8(5) . . ? C101 N100 Ru 177.4(6) . . ? N100 C101 C102 179.0(9) . . ? C101 C102 H10A 109.5 . . ? C101 C102 H10B 109.5 . . ? H10A C102 H10B 109.5 . . ? C101 C102 H10C 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? C201 N200 Ru 177.7(6) . . ? N200 C201 C202 179.3(9) . . ? C201 C202 H20A 109.5 . . ? C201 C202 H20B 109.5 . . ? H20A C202 H20B 109.5 . . ? C201 C202 H20C 109.5 . . ? H20A C202 H20C 109.5 . . ? H20B C202 H20C 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 S1A C2A C3A S4 -48.0(8) . . . . ? C2A C3A S4 C5A 119.9(7) . . . . ? C3A S4 C5A C6A -77.3(7) . . . . ? S4 C5A C6A S7A -56.7(8) . . . . ? C5A C6A S7A C8A 159.5(7) . . . . ? C6A S7A C8A C9A -158.3(7) . . . . ? S7A C8A C9A S10 55.8(8) . . . . ? C8A C9A S10 C11A 78(2) . . . . ? C9A S10 C11A C12A -122(4) . . . . ? S10 C11A C12A S1A 50(4) . . . . ? C11A C12A S1A C2A -164(3) . . . . ? C12A S1A C2A C3A 163.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.945 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.118 #=END data_S3 #*Complex 3* _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H19 Cl F6 N P Ru S4' _chemical_formula_weight 562.99 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' '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' 'Cl' 'Cl' 0.1484 0.1585 '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 Cm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' _cell_length_a 12.264(15) _cell_length_b 9.189(11) _cell_length_c 8.822(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.020(10) _cell_angle_gamma 90.00 _cell_volume 989(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 1.479 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1642 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 25.82 _reflns_number_total 1021 _reflns_number_gt 1017 _reflns_threshold_expression 2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+3.8761P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.027(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(10) _refine_ls_number_reflns 1021 _refine_ls_number_parameters 126 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.0000 0.0000 0.0000 0.0241(4) Uani 1 d S . . Cl Cl 0.1591(3) 0.0000 -0.1486(5) 0.0414(10) Uani 1 d S . . S1 S -0.1215(3) 0.0000 -0.2147(5) 0.0360(9) Uani 1 d S . . C2 C -0.0751(11) -0.1551(14) -0.3141(13) 0.051(3) Uani 1 d . . . H2A H -0.1200 -0.1685 -0.4103 0.061 Uiso 1 calc R . . H2B H 0.0004 -0.1416 -0.3347 0.061 Uiso 1 calc R . . C3 C -0.0847(13) -0.2876(16) -0.2109(17) 0.064(4) Uani 1 d . . . H3A H -0.0501 -0.3707 -0.2538 0.077 Uiso 1 calc R . . H3B H -0.1616 -0.3106 -0.2072 0.077 Uiso 1 calc R . . S4 S -0.0196(2) -0.2548(2) -0.0148(4) 0.0407(7) Uani 1 d . . . C5 C -0.1372(10) -0.2845(12) 0.0964(14) 0.049(3) Uani 1 d . . . H5A H -0.1769 -0.3702 0.0572 0.058 Uiso 1 calc R . . H5B H -0.1095 -0.3041 0.2015 0.058 Uiso 1 calc R . . C6 C -0.2163(10) -0.1576(16) 0.0931(15) 0.055(3) Uani 1 d . . . H6A H -0.2724 -0.1758 0.1605 0.066 Uiso 1 calc R . . H6B H -0.2516 -0.1428 -0.0094 0.066 Uiso 1 calc R . . S7 S -0.1363(3) 0.0000 0.1558(5) 0.0361(10) Uani 1 d S . . N100 N 0.1087(13) 0.0000 0.1961(19) 0.040(3) Uani 1 d S . . C101 C 0.15944(4) 0.0000 0.30775(5) 0.042(3) Uani 1 d SD . . C102 C 0.21829(2) 0.0000 0.46313(5) 0.091(9) Uani 1 d SD . . H10C H 0.19853(3) 0.085319(1) 0.51680(5) 0.109 Uiso 1 d D . . H10D H 0.29591(2) 0.0000 0.45638(8) 0.109 Uiso 1 d SD . . P P -0.4031(4) 0.0000 0.4555(5) 0.0565(11) Uani 0.50 d SPD . 1 F11 F -0.421(2) 0.0000 0.275(2) 0.110(3) Uiso 0.50 d SPD . 1 F12 F -0.386(2) 0.0000 0.635(2) 0.110(3) Uiso 0.50 d SPD . 1 F13 F -0.4951(16) 0.1200(13) 0.459(2) 0.110(3) Uiso 0.50 d PD . 1 F14 F -0.3134(15) -0.1223(13) 0.451(2) 0.110(3) Uiso 0.50 d PD . 1 P P -0.4031(4) 0.0000 0.4555(5) 0.0565(11) Uani 0.50 d SPD . 2 F111 F -0.2759(15) 0.0000 0.431(3) 0.110(3) Uiso 0.50 d SPD . 2 F121 F -0.5254(15) 0.0000 0.480(3) 0.110(3) Uiso 0.50 d SPD . 2 F131 F -0.3778(17) 0.1195(13) 0.583(2) 0.110(3) Uiso 0.50 d PD . 2 F141 F -0.4216(17) -0.1223(13) 0.331(2) 0.110(3) Uiso 0.50 d PD . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0175(5) 0.0249(5) 0.0293(5) 0.000 0.0000(3) 0.000 Cl 0.0242(17) 0.061(3) 0.040(2) 0.000 0.0069(13) 0.000 S1 0.0268(18) 0.046(2) 0.0331(18) 0.000 -0.0060(15) 0.000 C2 0.052(6) 0.059(6) 0.039(5) -0.015(5) -0.003(4) -0.005(6) C3 0.068(9) 0.050(6) 0.077(9) -0.031(6) 0.022(7) -0.022(7) S4 0.0399(18) 0.0272(9) 0.0557(16) 0.0026(12) 0.0084(14) 0.0014(10) C5 0.054(7) 0.039(5) 0.054(6) 0.000(5) 0.010(5) -0.014(5) C6 0.035(6) 0.072(7) 0.060(7) 0.007(6) 0.015(5) -0.013(5) S7 0.027(2) 0.041(2) 0.041(2) 0.000 0.0091(15) 0.000 N100 0.028(7) 0.044(8) 0.047(8) 0.000 -0.004(6) 0.000 C101 0.024(6) 0.079(11) 0.024(6) 0.000 0.005(5) 0.000 C102 0.069(14) 0.17(3) 0.027(8) 0.000 -0.025(8) 0.000 P 0.035(2) 0.090(3) 0.045(2) 0.000 0.0076(16) 0.000 P 0.035(2) 0.090(3) 0.045(2) 0.000 0.0076(16) 0.000 _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 N100 2.070(16) . ? Ru S7 2.272(4) . ? Ru S1 2.284(4) . ? Ru S4 2.356(4) . ? Ru S4 2.356(4) 2 ? Ru Cl 2.462(5) . ? S1 C2 1.797(12) . ? S1 C2 1.797(12) 2 ? C2 C3 1.53(2) . ? C3 S4 1.852(15) . ? S4 C5 1.848(12) . ? C5 C6 1.516(19) . ? C6 S7 1.803(14) . ? S7 C6 1.803(14) 2 ? N100 C101 1.108(16) . ? C101 C102 1.4807(14) . ? P F14 1.575(16) 2 ? P F14 1.575(16) . ? P F12 1.579(18) . ? P F13 1.581(17) 2 ? P F13 1.581(17) . ? P F11 1.585(18) . ? P F121 1.538(18) . ? P F141 1.570(16) . ? P F141 1.570(16) 2 ? P F131 1.579(16) . ? P F131 1.579(16) 2 ? P F111 1.597(18) . ? 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 N100 Ru S7 86.8(5) . . ? N100 Ru S1 179.3(5) . . ? S7 Ru S1 92.53(18) . . ? N100 Ru S4 95.71(8) . . ? S7 Ru S4 87.50(8) . . ? S1 Ru S4 84.26(7) . . ? N100 Ru S4 95.71(8) . 2 ? S7 Ru S4 87.50(8) . 2 ? S1 Ru S4 84.26(7) . 2 ? S4 Ru S4 167.25(13) . 2 ? N100 Ru Cl 88.2(5) . . ? S7 Ru Cl 175.00(18) . . ? S1 Ru Cl 92.47(18) . . ? S4 Ru Cl 93.01(8) . . ? S4 Ru Cl 93.01(8) 2 . ? C2 S1 C2 104.9(9) . 2 ? C2 S1 Ru 101.1(4) . . ? C2 S1 Ru 101.1(4) 2 . ? C3 C2 S1 107.0(8) . . ? C2 C3 S4 111.9(8) . . ? C5 S4 C3 100.8(6) . . ? C5 S4 Ru 101.4(4) . . ? C3 S4 Ru 104.2(5) . . ? C6 C5 S4 114.2(8) . . ? C5 C6 S7 106.6(8) . . ? C6 S7 C6 106.8(9) . 2 ? C6 S7 Ru 103.0(4) . . ? C6 S7 Ru 103.0(4) 2 . ? C101 N100 Ru 174.2(13) . . ? N100 C101 C102 175.0(9) . . ? F14 P F14 91.0(11) 2 . ? F14 P F12 90.1(8) 2 . ? F14 P F12 90.1(8) . . ? F14 P F13 178.7(10) 2 2 ? F14 P F13 90.2(5) . 2 ? F12 P F13 90.1(7) . 2 ? F14 P F13 90.2(5) 2 . ? F14 P F13 178.7(10) . . ? F12 P F13 90.1(7) . . ? F13 P F13 88.5(11) 2 . ? F14 P F11 90.0(8) 2 . ? F14 P F11 90.0(8) . . ? F12 P F11 179.9(14) . . ? F13 P F11 89.8(8) 2 . ? F13 P F11 89.8(8) . . ? F121 P F141 91.5(8) . . ? F121 P F141 91.5(8) . 2 ? F141 P F141 91.4(10) . 2 ? F121 P F131 91.2(8) . . ? F141 P F131 176.8(10) . . ? F141 P F131 90.2(5) 2 . ? F121 P F131 91.2(8) . 2 ? F141 P F131 90.2(5) . 2 ? F141 P F131 176.8(10) 2 2 ? F131 P F131 88.1(10) . 2 ? F121 P F111 179.5(13) . . ? F141 P F111 88.8(8) . . ? F141 P F111 88.8(8) 2 . ? F131 P F111 88.4(8) . . ? F131 P F111 88.4(8) 2 . ? 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 S1 C2 C3 S4 -50.4(12) . . . . ? C2 C3 S4 C5 121.5(10) . . . . ? C3 S4 C5 C6 -78.2(11) . . . . ? S4 C5 C6 S7 -54.9(11) . . . . ? C5 C6 S7 C6 161.1(5) . . . 2 ? C6 S7 C6 C5 -161.1(5) . . 2 2 ? S7 C6 C5 S4 54.9(11) . 2 2 2 ? C6 C5 S4 C3 78.2(11) 2 2 2 2 ? C5 S4 C3 C2 -121.5(10) 2 2 2 2 ? S4 C3 C2 S1 50.4(12) 2 2 2 . ? C3 C2 S1 C2 -165.1(7) 2 2 . . ? C2 S1 C2 C3 165.1(7) 2 . . . ? _diffrn_measured_fraction_theta_max 0.485 _diffrn_reflns_theta_full 25.82 _diffrn_measured_fraction_theta_full 0.485 _refine_diff_density_max 1.976 _refine_diff_density_min -1.180 _refine_diff_density_rms 0.160 #=END data_S4 #*Complex 4* _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H25 Cl F6 N3 P Ru S4' _chemical_formula_weight 681.13 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' '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' '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 Pc21b loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, z+1/2' _cell_length_a 7.655(9) _cell_length_b 15.928(17) _cell_length_c 21.47(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2618(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.136 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7339 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.96 _reflns_number_total 4295 _reflns_number_gt 3527 _reflns_threshold_expression 2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1553P)^2^+2.7144P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0028(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(5) _refine_ls_number_reflns 4295 _refine_ls_number_parameters 288 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.2202 _refine_ls_wR_factor_gt 0.1946 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.227 _refine_ls_shift/su_mean 0.016 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.04052(9) 0.20817(4) 0.15144(3) 0.0382(3) Uani 1 d . . . S1 S -0.1123(4) 0.08290(17) 0.15659(14) 0.0545(7) Uani 1 d . . . C2 C 0.0654(17) 0.0086(6) 0.1688(7) 0.064(3) Uani 1 d . . . H2A H 0.0193 -0.0479 0.1719 0.077 Uiso 1 calc R . . H2B H 0.1458 0.0106 0.1339 0.077 Uiso 1 calc R . . C3 C 0.158(2) 0.0314(7) 0.2272(6) 0.071(4) Uani 1 d . . . H3A H 0.2637 -0.0017 0.2307 0.086 Uiso 1 calc R . . H3B H 0.0840 0.0181 0.2626 0.086 Uiso 1 calc R . . S4 S 0.2159(4) 0.14653(19) 0.22958(13) 0.0548(7) Uani 1 d . . . C5 C 0.1057(18) 0.1778(10) 0.3011(5) 0.072(4) Uani 1 d . . . H5A H 0.1234 0.1347 0.3323 0.086 Uiso 1 calc R . . H5B H 0.1584 0.2292 0.3164 0.086 Uiso 1 calc R . . C6 C -0.0934(19) 0.1922(9) 0.2924(6) 0.075(4) Uani 1 d . . . H6A H -0.1446 0.2141 0.3304 0.090 Uiso 1 calc R . . H6B H -0.1512 0.1399 0.2820 0.090 Uiso 1 calc R . . S7 S -0.1178(4) 0.26764(19) 0.22917(12) 0.0554(7) Uani 1 d . . . C8 C -0.3439(15) 0.2537(11) 0.2017(6) 0.081(4) Uani 1 d . . . H8A H -0.3748 0.1947 0.2000 0.097 Uiso 1 calc R . . H8B H -0.4257 0.2826 0.2288 0.097 Uiso 1 calc R . . C9 C -0.3430(18) 0.2924(10) 0.1370(7) 0.078(4) Uani 1 d . . . H9A H -0.3220 0.3522 0.1412 0.094 Uiso 1 calc R . . H9B H -0.4583 0.2854 0.1190 0.094 Uiso 1 calc R . . S10 S -0.1833(4) 0.2497(2) 0.08299(13) 0.0577(7) Uani 1 d . . . C11 C -0.2923(17) 0.1478(9) 0.0613(5) 0.069(4) Uani 1 d . . . H11A H -0.4028 0.1435 0.0831 0.083 Uiso 1 calc R . . H11B H -0.3165 0.1478 0.0169 0.083 Uiso 1 calc R . . C12 C -0.1823(17) 0.0739(9) 0.0768(5) 0.064(3) Uani 1 d . . . H12A H -0.0815 0.0718 0.0495 0.077 Uiso 1 calc R . . H12B H -0.2490 0.0226 0.0712 0.077 Uiso 1 calc R . . Cl Cl 0.2248(4) 0.15776(17) 0.06613(12) 0.0505(6) Uani 1 d . . . N21 N 0.1800(10) 0.3216(4) 0.1463(4) 0.0382(16) Uani 1 d . . . C22 C 0.2386(14) 0.3745(7) 0.1888(4) 0.048(2) Uani 1 d . . . H22 H 0.2256 0.3670 0.2315 0.057 Uiso 1 calc R . . C23 C 0.3227(12) 0.4435(6) 0.1616(5) 0.045(2) Uani 1 d . . . C24 C 0.4014(15) 0.5179(6) 0.1863(5) 0.052(3) Uani 1 d . . . H24 H 0.4087 0.5278 0.2289 0.062 Uiso 1 calc R . . C25 C 0.4634(17) 0.5721(7) 0.1446(6) 0.064(3) Uani 1 d . . . H25 H 0.5206 0.6194 0.1597 0.077 Uiso 1 calc R . . C26 C 0.4496(18) 0.5637(7) 0.0785(6) 0.061(3) Uani 1 d . . . H26 H 0.4860 0.6067 0.0523 0.073 Uiso 1 calc R . . C27 C 0.3782(16) 0.4873(7) 0.0536(6) 0.056(3) Uani 1 d . . . H27 H 0.3774 0.4759 0.0111 0.068 Uiso 1 calc R . . C28 C 0.3097(13) 0.4311(5) 0.0977(4) 0.040(2) Uani 1 d . . . N29 N 0.2252(12) 0.3586(5) 0.0897(4) 0.0449(19) Uani 1 d . . . H29 H 0.2016 0.3372 0.0539 0.054 Uiso 1 calc R . . P P 0.4841(4) 0.35826(17) 0.37741(13) 0.0696(10) Uani 1 d D . . F11 F 0.4898(13) 0.4288(4) 0.3264(3) 0.140(3) Uiso 0.527(8) d PD A 1 F12 F 0.4784(12) 0.2877(4) 0.4284(3) 0.140(3) Uiso 0.527(8) d PD A 1 F13 F 0.2805(5) 0.3682(6) 0.3821(5) 0.140(3) Uiso 0.527(8) d PD A 1 F14 F 0.6876(5) 0.3483(6) 0.3727(5) 0.140(3) Uiso 0.527(8) d PD A 1 F15 F 0.5079(15) 0.4263(4) 0.4296(3) 0.140(3) Uiso 0.527(8) d PD A 1 F16 F 0.4603(15) 0.2902(4) 0.3253(3) 0.140(3) Uiso 0.527(8) d PD A 1 F11 F 0.6016(10) 0.3730(7) 0.3185(3) 0.140(3) Uiso 0.473(8) d PD A 2 F12 F 0.3666(10) 0.3435(6) 0.4363(3) 0.140(3) Uiso 0.473(8) d PD A 2 F13 F 0.3211(8) 0.3917(6) 0.3407(4) 0.140(3) Uiso 0.473(8) d PD A 2 F14 F 0.6471(8) 0.3248(6) 0.4141(4) 0.140(3) Uiso 0.473(8) d PD A 2 F15 F 0.5247(14) 0.4497(3) 0.4003(5) 0.140(3) Uiso 0.473(8) d PD A 2 F16 F 0.4435(14) 0.2668(3) 0.3545(5) 0.140(3) Uiso 0.473(8) d PD A 2 N100 N -0.099(3) 0.4974(14) 0.0891(11) 0.154(9) Uani 1 d . . . C101 C -0.064(3) 0.5556(16) 0.0563(10) 0.108(7) Uani 1 d . . . C102 C -0.009(4) 0.6224(17) 0.0168(15) 0.184(13) Uani 1 d . . . H10A H -0.0349 0.6752 0.0364 0.221 Uiso 1 calc R . . H10B H -0.0695 0.6188 -0.0222 0.221 Uiso 1 calc R . . H10C H 0.1145 0.6182 0.0098 0.221 Uiso 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 0.0294(4) 0.0454(4) 0.0398(4) -0.0001(3) 0.0028(3) 0.0001(3) S1 0.0514(15) 0.0578(15) 0.0543(15) 0.0021(13) 0.0022(12) -0.0151(12) C2 0.061(8) 0.033(5) 0.098(10) 0.008(5) 0.005(6) 0.008(5) C3 0.092(11) 0.049(6) 0.073(8) 0.023(5) -0.016(7) 0.011(6) S4 0.0450(16) 0.0628(17) 0.0567(16) 0.0124(13) -0.0069(11) -0.0022(12) C5 0.063(8) 0.108(11) 0.045(6) 0.012(6) 0.000(5) -0.013(7) C6 0.083(10) 0.095(10) 0.046(6) -0.009(6) 0.021(6) -0.018(7) S7 0.0456(15) 0.0732(19) 0.0473(14) -0.0104(12) 0.0115(11) 0.0050(13) C8 0.035(7) 0.148(13) 0.060(7) -0.018(8) 0.016(5) 0.008(7) C9 0.040(8) 0.100(10) 0.096(10) -0.006(8) -0.007(6) 0.007(6) S10 0.0431(15) 0.0788(19) 0.0512(14) -0.0016(13) -0.0082(11) 0.0082(14) C11 0.041(7) 0.122(12) 0.043(6) 0.000(6) -0.009(4) -0.023(7) C12 0.056(8) 0.091(9) 0.046(6) -0.009(6) 0.004(5) -0.033(7) Cl 0.0457(16) 0.0529(14) 0.0530(14) -0.0063(11) 0.0144(10) -0.0011(11) N21 0.039(4) 0.034(4) 0.041(4) 0.004(3) 0.004(3) 0.004(3) C22 0.053(6) 0.057(6) 0.033(5) -0.008(4) -0.005(4) -0.008(5) C23 0.036(5) 0.046(5) 0.053(6) -0.003(4) -0.007(4) -0.001(4) C24 0.055(7) 0.039(5) 0.061(7) -0.016(5) -0.002(5) 0.001(4) C25 0.058(7) 0.042(5) 0.094(9) -0.002(6) -0.011(7) -0.014(5) C26 0.055(7) 0.051(6) 0.078(8) 0.003(5) 0.002(6) -0.017(6) C27 0.052(6) 0.056(6) 0.061(7) 0.004(5) -0.005(5) -0.010(5) C28 0.037(5) 0.030(4) 0.054(6) -0.002(4) 0.001(4) -0.006(4) N29 0.052(5) 0.044(5) 0.039(4) -0.006(3) 0.003(3) -0.012(4) P 0.078(3) 0.071(2) 0.0596(18) -0.0184(15) -0.0026(15) 0.0135(18) N100 0.16(2) 0.149(18) 0.149(19) -0.015(15) -0.022(16) 0.066(17) C101 0.117(16) 0.112(15) 0.094(14) -0.032(11) -0.035(12) 0.034(14) C102 0.19(3) 0.18(3) 0.18(3) 0.01(2) -0.01(2) 0.06(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N21 2.101(7) . ? Ru S7 2.270(3) . ? Ru S1 2.316(3) . ? Ru S10 2.352(3) . ? Ru S4 2.363(3) . ? Ru Cl 2.448(3) . ? S1 C12 1.801(11) . ? S1 C2 1.821(12) . ? C2 C3 1.486(19) . ? C3 S4 1.887(12) . ? S4 C5 1.822(13) . ? C5 C6 1.55(2) . ? C6 S7 1.823(14) . ? S7 C8 1.842(13) . ? C8 C9 1.519(18) . ? C9 S10 1.818(14) . ? S10 C11 1.883(13) . ? C11 C12 1.486(19) . ? N21 C22 1.322(12) . ? N21 N29 1.394(11) . ? C22 C23 1.400(14) . ? C23 C28 1.389(14) . ? C23 C24 1.432(14) . ? C24 C25 1.332(16) . ? C25 C26 1.428(17) . ? C26 C27 1.437(16) . ? C27 C28 1.406(14) . ? C28 N29 1.335(12) . ? P F12 1.569(2) . ? P F15 1.569(2) . ? P F11 1.569(2) . ? P F13 1.569(3) . ? P F15 1.569(2) . ? P F14 1.569(2) . ? P F14 1.569(3) . ? P F12 1.569(2) . ? P F16 1.569(2) . ? P F13 1.569(2) . ? P F11 1.569(2) . ? P F16 1.569(2) . ? N100 C101 1.19(3) . ? C101 C102 1.42(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 N21 Ru S7 87.2(2) . . ? N21 Ru S1 179.6(2) . . ? S7 Ru S1 93.14(12) . . ? N21 Ru S10 95.5(2) . . ? S7 Ru S10 87.33(13) . . ? S1 Ru S10 84.51(13) . . ? N21 Ru S4 96.1(2) . . ? S7 Ru S4 87.40(14) . . ? S1 Ru S4 83.98(12) . . ? S10 Ru S4 167.05(11) . . ? N21 Ru Cl 87.1(2) . . ? S7 Ru Cl 174.29(11) . . ? S1 Ru Cl 92.53(11) . . ? S10 Ru Cl 92.53(13) . . ? S4 Ru Cl 93.88(13) . . ? C12 S1 C2 107.9(7) . . ? C12 S1 Ru 100.0(4) . . ? C2 S1 Ru 100.9(4) . . ? C3 C2 S1 108.5(9) . . ? C2 C3 S4 111.9(7) . . ? C5 S4 C3 100.3(7) . . ? C5 S4 Ru 102.8(5) . . ? C3 S4 Ru 104.5(4) . . ? C6 C5 S4 113.2(9) . . ? C5 C6 S7 106.7(9) . . ? C6 S7 C8 104.8(7) . . ? C6 S7 Ru 102.6(4) . . ? C8 S7 Ru 102.5(4) . . ? C9 C8 S7 103.9(9) . . ? C8 C9 S10 115.8(10) . . ? C9 S10 C11 100.5(7) . . ? C9 S10 Ru 101.3(5) . . ? C11 S10 Ru 103.6(4) . . ? C12 C11 S10 112.1(8) . . ? C11 C12 S1 108.6(9) . . ? C22 N21 N29 104.4(7) . . ? C22 N21 Ru 133.2(7) . . ? N29 N21 Ru 122.4(6) . . ? N21 C22 C23 111.6(8) . . ? C28 C23 C22 105.5(8) . . ? C28 C23 C24 120.9(9) . . ? C22 C23 C24 133.4(10) . . ? C25 C24 C23 115.8(10) . . ? C24 C25 C26 125.6(10) . . ? C25 C26 C27 118.5(10) . . ? C28 C27 C26 115.5(11) . . ? N29 C28 C23 106.6(8) . . ? N29 C28 C27 130.1(9) . . ? C23 C28 C27 123.3(9) . . ? C28 N29 N21 111.9(7) . . ? F12 P F15 66.1(5) . . ? F12 P F11 133.3(4) . . ? F15 P F11 90.01(9) . . ? F12 P F13 52.7(4) . . ? F15 P F13 90.00(4) . . ? F11 P F13 90.00(3) . . ? F12 P F15 90.00(5) . . ? F15 P F15 27.3(4) . . ? F11 P F15 63.2(4) . . ? F13 P F15 94.8(6) . . ? F12 P F14 90.00(8) . . ? F15 P F14 77.5(5) . . ? F11 P F14 124.9(4) . . ? F13 P F14 142.3(4) . . ? F15 P F14 90.00(6) . . ? F12 P F14 127.3(4) . . ? F15 P F14 90.01(4) . . ? F11 P F14 90.00(3) . . ? F13 P F14 180.0(5) . . ? F15 P F14 85.2(6) . . ? F14 P F14 37.7(4) . . ? F12 P F12 46.7(4) . . ? F15 P F12 90.00(9) . . ? F11 P F12 180.0(5) . . ? F13 P F12 90.00(3) . . ? F15 P F12 116.8(4) . . ? F14 P F12 55.1(4) . . ? F14 P F12 90.00(3) . . ? F12 P F16 90.01(5) . . ? F15 P F16 152.7(4) . . ? F11 P F16 116.8(4) . . ? F13 P F16 85.2(6) . . ? F15 P F16 180.0(5) . . ? F14 P F16 90.00(6) . . ? F14 P F16 94.8(6) . . ? F12 P F16 63.2(4) . . ? F12 P F13 90.00(8) . . ? F15 P F13 102.5(5) . . ? F11 P F13 55.1(4) . . ? F13 P F13 37.7(4) . . ? F15 P F13 90.00(6) . . ? F14 P F13 180.0(5) . . ? F14 P F13 142.3(4) . . ? F12 P F13 124.9(4) . . ? F16 P F13 90.00(6) . . ? F12 P F11 180.0(5) . . ? F15 P F11 113.9(5) . . ? F11 P F11 46.7(4) . . ? F13 P F11 127.3(4) . . ? F15 P F11 89.99(5) . . ? F14 P F11 90.00(8) . . ? F14 P F11 52.7(4) . . ? F12 P F11 133.3(4) . . ? F16 P F11 90.00(5) . . ? F13 P F11 90.00(8) . . ? F12 P F16 113.9(5) . . ? F15 P F16 180.0(5) . . ? F11 P F16 90.00(9) . . ? F13 P F16 89.99(4) . . ? F15 P F16 152.7(4) . . ? F14 P F16 102.5(5) . . ? F14 P F16 90.00(4) . . ? F12 P F16 89.99(9) . . ? F16 P F16 27.3(4) . . ? F13 P F16 77.5(5) . . ? F11 P F16 66.1(5) . . ? N100 C101 C102 175(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 S1 C2 C3 S4 -49.7(12) . . . . ? C2 C3 S4 C5 122.6(11) . . . . ? C3 S4 C5 C6 -79.7(11) . . . . ? S4 C5 C6 S7 -54.3(12) . . . . ? C5 C6 S7 C8 159.9(9) . . . . ? C6 S7 C8 C9 -160.8(10) . . . . ? S7 C8 C9 S10 56.1(13) . . . . ? C8 C9 S10 C11 76.7(12) . . . . ? C9 S10 C11 C12 -120.7(9) . . . . ? S10 C11 C12 S1 50.7(10) . . . . ? C11 C12 S1 C2 -165.2(8) . . . . ? C12 S1 C2 C3 164.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.875 _refine_diff_density_max 1.460 _refine_diff_density_min -1.193 _refine_diff_density_rms 0.147 #=END data_S5 #*Complex 5* _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H28 F12 N2 P2 Ru S4' _chemical_formula_weight 887.75 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' '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 Pcab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y, -z+1/2' '-x, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y, z-1/2' 'x, y-1/2, -z-1/2' _cell_length_a 19.95(2) _cell_length_b 14.860(16) _cell_length_c 21.52(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6382(12) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17142 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.91 _reflns_number_total 5856 _reflns_number_gt 4306 _reflns_threshold_expression 2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+12.8685P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5856 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1306 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.153662(17) 0.79543(3) 0.341272(17) 0.03003(14) Uani 1 d . . . S1 S 0.19377(7) 0.90517(9) 0.27565(7) 0.0469(3) Uani 1 d . . . C2 C 0.1272(3) 0.9181(4) 0.2188(3) 0.0572(16) Uani 1 d . . . H2A H 0.0876 0.9439 0.2379 0.069 Uiso 1 calc R . . H2B H 0.1414 0.9569 0.1851 0.069 Uiso 1 calc R . . C3 C 0.1126(3) 0.8243(5) 0.1950(2) 0.0561(16) Uani 1 d . . . H3A H 0.1518 0.8026 0.1729 0.067 Uiso 1 calc R . . H3B H 0.0760 0.8277 0.1654 0.067 Uiso 1 calc R . . S4 S 0.09035(6) 0.74106(9) 0.25583(6) 0.0416(3) Uani 1 d . . . C5 C 0.0033(2) 0.7754(4) 0.2735(2) 0.0453(13) Uani 1 d . . . H5A H -0.0091 0.8243 0.2459 0.054 Uiso 1 calc R . . H5B H -0.0263 0.7253 0.2648 0.054 Uiso 1 calc R . . C6 C -0.0076(3) 0.8053(4) 0.3397(2) 0.0441(13) Uani 1 d . . . H62A H -0.0065 0.7541 0.3676 0.053 Uiso 1 calc R . . H62B H -0.0507 0.8350 0.3440 0.053 Uiso 1 calc R . . S7 S 0.06001(6) 0.88293(9) 0.35759(6) 0.0409(3) Uani 1 d . . . C8 C 0.0590(3) 0.9119(5) 0.4397(3) 0.0579(16) Uani 1 d . . . H8A H 0.0366 0.9692 0.4450 0.070 Uiso 1 calc R . . H8B H 0.0337 0.8667 0.4622 0.070 Uiso 1 calc R . . C9 C 0.1275(3) 0.9177(5) 0.4663(3) 0.0668(18) Uani 1 d . . . H9A H 0.1270 0.8846 0.5051 0.080 Uiso 1 calc R . . H9B H 0.1353 0.9804 0.4767 0.080 Uiso 1 calc R . . S10 S 0.20046(7) 0.87936(10) 0.42274(7) 0.0499(4) Uani 1 d . . . C11 C 0.2297(4) 0.9821(5) 0.3834(4) 0.081(2) Uani 1 d . . . H11A H 0.2259 1.0321 0.4121 0.098 Uiso 1 calc R . . H11B H 0.2768 0.9749 0.3733 0.098 Uiso 1 calc R . . C12 C 0.1918(4) 1.0058(4) 0.3239(3) 0.0675(19) Uani 1 d . . . H12A H 0.2133 1.0557 0.3028 0.081 Uiso 1 calc R . . H12B H 0.1459 1.0225 0.3334 0.081 Uiso 1 calc R . . N21 N 0.13401(19) 0.6857(3) 0.40238(18) 0.0346(9) Uani 1 d . . . C22 C 0.1798(2) 0.6176(3) 0.3976(2) 0.0310(10) Uani 1 d . . . C23 C 0.1778(2) 0.5384(3) 0.4336(2) 0.0351(11) Uani 1 d . . . C24 C 0.1252(3) 0.5303(4) 0.4769(2) 0.0429(12) Uani 1 d . . . H24 H 0.1211 0.4791 0.5015 0.051 Uiso 1 calc R . . C25 C 0.0803(3) 0.5990(4) 0.4820(2) 0.0460(13) Uani 1 d . . . H25 H 0.0460 0.5954 0.5111 0.055 Uiso 1 calc R . . C26 C 0.0852(2) 0.6747(4) 0.4440(2) 0.0431(12) Uani 1 d . . . H26 H 0.0529 0.7195 0.4478 0.052 Uiso 1 calc R . . N31 N 0.23460(18) 0.7084(3) 0.32139(18) 0.0334(9) Uani 1 d . . . C32 C 0.2823(2) 0.7188(4) 0.2781(2) 0.0435(12) Uani 1 d . . . H32 H 0.2855 0.7737 0.2577 0.052 Uiso 1 calc R . . C33 C 0.3272(2) 0.6510(4) 0.2624(2) 0.0443(13) Uani 1 d . . . H33 H 0.3579 0.6599 0.2305 0.053 Uiso 1 calc R . . C34 C 0.3262(2) 0.5699(4) 0.2945(2) 0.0400(12) Uani 1 d . . . H34 H 0.3556 0.5239 0.2838 0.048 Uiso 1 calc R . . C35 C 0.2804(2) 0.5582(3) 0.3433(2) 0.0336(10) Uani 1 d . . . C36 C 0.2332(2) 0.6285(3) 0.3535(2) 0.0303(10) Uani 1 d . . . C41 C 0.2775(2) 0.4793(3) 0.3823(2) 0.0381(11) Uani 1 d . . . C42 C 0.2275(2) 0.4716(3) 0.4254(2) 0.0390(11) Uani 1 d . . . H42 H 0.2262 0.4205 0.4503 0.047 Uiso 1 calc R . . C51 C 0.3306(3) 0.4079(3) 0.3785(2) 0.0409(12) Uani 1 d . . . C52 C 0.3989(3) 0.4264(4) 0.3745(3) 0.0530(14) Uani 1 d . . . H52 H 0.4132 0.4855 0.3693 0.064 Uiso 1 calc R . . C53 C 0.4457(3) 0.3584(6) 0.3781(3) 0.069(2) Uani 1 d . . . H53 H 0.4911 0.3720 0.3753 0.082 Uiso 1 calc R . . C54 C 0.4258(4) 0.2706(5) 0.3858(3) 0.0691(19) Uani 1 d . . . H54 H 0.4578 0.2253 0.3884 0.083 Uiso 1 calc R . . C55 C 0.3587(4) 0.2493(4) 0.3895(3) 0.0642(18) Uani 1 d . . . H55 H 0.3456 0.1897 0.3947 0.077 Uiso 1 calc R . . C56 C 0.3105(3) 0.3166(4) 0.3857(3) 0.0532(14) Uani 1 d . . . H56 H 0.2653 0.3020 0.3878 0.064 Uiso 1 calc R . . P1 P -0.04853(7) 0.52580(10) 0.34041(7) 0.0424(3) Uani 1 d . . . F11 F -0.09329(19) 0.5985(3) 0.3061(2) 0.0807(12) Uani 1 d . . . F12 F -0.00393(19) 0.4516(3) 0.3741(2) 0.0799(12) Uani 1 d . . . F13 F -0.11415(18) 0.4678(3) 0.3537(2) 0.0848(13) Uani 1 d . . . F14 F 0.01747(17) 0.5819(2) 0.32672(18) 0.0672(10) Uani 1 d . . . F15 F -0.0573(2) 0.5768(3) 0.40441(19) 0.0881(13) Uani 1 d . . . F16 F -0.03847(19) 0.4734(3) 0.27607(19) 0.0837(13) Uani 1 d . . . P2 P -0.13026(8) 0.79753(11) 0.50561(8) 0.0530(4) Uani 1 d . . . F21 F -0.1525(3) 0.7125(4) 0.5403(4) 0.153(3) Uani 1 d . . . F22 F -0.1484(3) 0.7521(5) 0.4430(3) 0.152(3) Uani 1 d . . . F23 F -0.1112(3) 0.8470(4) 0.5673(3) 0.138(2) Uani 1 d . . . F24 F -0.2004(2) 0.8427(5) 0.5082(3) 0.136(2) Uani 1 d . . . F25 F -0.0577(2) 0.7578(4) 0.4997(3) 0.126(2) Uani 1 d . . . F26 F -0.1060(4) 0.8840(4) 0.4678(3) 0.149(3) Uani 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 0.0261(2) 0.0318(3) 0.0322(2) 0.00200(15) 0.00085(14) 0.00229(15) S1 0.0399(7) 0.0450(8) 0.0557(8) 0.0119(6) 0.0118(6) 0.0011(6) C2 0.051(3) 0.064(4) 0.056(3) 0.033(3) 0.010(3) 0.008(3) C3 0.057(3) 0.079(5) 0.032(3) 0.013(3) 0.000(2) -0.001(3) S4 0.0421(7) 0.0480(8) 0.0347(6) -0.0015(6) -0.0019(5) 0.0032(6) C5 0.033(3) 0.054(4) 0.049(3) 0.009(3) -0.007(2) -0.001(2) C6 0.034(3) 0.047(3) 0.051(3) 0.003(3) 0.001(2) 0.000(2) S7 0.0331(6) 0.0401(8) 0.0495(7) -0.0013(6) 0.0018(5) 0.0050(5) C8 0.051(3) 0.069(4) 0.054(3) -0.020(3) 0.011(3) 0.008(3) C9 0.061(4) 0.087(5) 0.053(4) -0.026(3) 0.004(3) -0.004(3) S10 0.0387(7) 0.0567(9) 0.0541(8) -0.0142(7) -0.0080(6) -0.0027(6) C11 0.070(4) 0.077(5) 0.097(6) -0.015(4) 0.015(4) -0.044(4) C12 0.077(4) 0.035(3) 0.090(5) 0.001(3) 0.029(4) -0.018(3) N21 0.033(2) 0.040(2) 0.031(2) 0.0021(17) 0.0009(16) 0.0032(18) C22 0.025(2) 0.041(3) 0.028(2) -0.003(2) -0.0016(17) -0.001(2) C23 0.041(3) 0.037(3) 0.027(2) 0.002(2) -0.0063(19) -0.001(2) C24 0.048(3) 0.045(3) 0.037(3) 0.007(2) 0.003(2) -0.002(3) C25 0.038(3) 0.063(4) 0.037(3) 0.005(3) 0.012(2) -0.001(3) C26 0.033(2) 0.054(3) 0.042(3) 0.003(2) 0.003(2) 0.008(2) N31 0.0255(19) 0.042(2) 0.033(2) 0.0025(17) 0.0022(16) -0.0001(17) C32 0.038(3) 0.047(3) 0.045(3) 0.010(2) 0.011(2) 0.004(2) C33 0.033(2) 0.050(3) 0.049(3) 0.009(3) 0.010(2) 0.007(2) C34 0.033(2) 0.047(3) 0.040(3) -0.001(2) 0.003(2) 0.009(2) C35 0.034(2) 0.034(3) 0.033(2) -0.003(2) -0.0034(19) 0.006(2) C36 0.030(2) 0.032(3) 0.029(2) -0.0009(19) -0.0028(17) -0.0006(19) C41 0.039(3) 0.037(3) 0.038(3) 0.001(2) -0.007(2) 0.002(2) C42 0.044(3) 0.033(3) 0.040(3) 0.007(2) -0.003(2) 0.002(2) C51 0.047(3) 0.038(3) 0.037(3) -0.003(2) -0.006(2) 0.008(2) C52 0.045(3) 0.064(4) 0.050(3) 0.003(3) -0.001(3) 0.010(3) C53 0.049(4) 0.099(6) 0.057(4) 0.008(4) 0.001(3) 0.025(4) C54 0.079(5) 0.068(5) 0.060(4) -0.003(3) -0.002(4) 0.035(4) C55 0.097(5) 0.037(4) 0.059(4) -0.007(3) -0.002(4) 0.017(3) C56 0.064(4) 0.042(3) 0.054(3) 0.000(3) -0.006(3) 0.004(3) P1 0.0392(7) 0.0384(8) 0.0495(8) -0.0054(6) 0.0037(6) -0.0051(6) F11 0.066(2) 0.066(3) 0.110(3) 0.019(2) -0.003(2) 0.016(2) F12 0.071(2) 0.069(3) 0.099(3) 0.024(2) -0.002(2) 0.004(2) F13 0.053(2) 0.073(3) 0.128(4) -0.005(3) 0.017(2) -0.025(2) F14 0.053(2) 0.065(2) 0.084(3) 0.0056(19) 0.0046(18) -0.0210(18) F15 0.091(3) 0.104(3) 0.069(3) -0.036(2) 0.015(2) -0.005(2) F16 0.063(2) 0.113(3) 0.075(3) -0.045(2) -0.0076(19) 0.002(2) P2 0.0465(8) 0.0481(9) 0.0645(10) -0.0018(7) 0.0061(7) -0.0025(7) F21 0.162(6) 0.096(4) 0.202(7) 0.049(4) 0.061(5) -0.040(4) F22 0.162(6) 0.165(6) 0.128(5) -0.071(5) -0.037(4) 0.029(5) F23 0.156(5) 0.148(5) 0.109(4) -0.051(4) -0.052(4) 0.034(4) F24 0.077(3) 0.187(6) 0.146(5) -0.039(5) -0.011(3) 0.056(4) F25 0.061(3) 0.141(5) 0.174(6) -0.022(4) 0.008(3) 0.019(3) F26 0.177(6) 0.091(4) 0.180(6) 0.043(4) 0.055(5) -0.003(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 N31 2.113(4) . ? Ru N21 2.131(4) . ? Ru S1 2.301(2) . ? Ru S7 2.303(2) . ? Ru S10 2.346(2) . ? Ru S4 2.373(2) . ? S1 C2 1.817(6) . ? S1 C12 1.821(7) . ? C2 C3 1.513(9) . ? C3 S4 1.855(6) . ? S4 C5 1.850(5) . ? C5 C6 1.510(7) . ? C6 S7 1.816(6) . ? S7 C8 1.818(6) . ? C8 C9 1.485(9) . ? C9 S10 1.822(6) . ? S10 C11 1.841(7) . ? C11 C12 1.527(10) . ? N21 C26 1.333(6) . ? N21 C22 1.368(6) . ? C22 C23 1.410(7) . ? C22 C36 1.437(6) . ? C23 C24 1.410(7) . ? C23 C42 1.414(7) . ? C24 C25 1.362(7) . ? C25 C26 1.394(7) . ? N31 C32 1.340(6) . ? N31 C36 1.374(6) . ? C32 C33 1.390(7) . ? C33 C34 1.388(7) . ? C34 C35 1.404(7) . ? C35 C36 1.422(7) . ? C35 C41 1.444(7) . ? C41 C42 1.367(7) . ? C41 C51 1.500(7) . ? C51 C52 1.394(8) . ? C51 C56 1.423(8) . ? C52 C53 1.377(8) . ? C53 C54 1.373(10) . ? C54 C55 1.379(10) . ? C55 C56 1.389(9) . ? P1 F15 1.582(4) . ? P1 F11 1.584(4) . ? P1 F14 1.586(4) . ? P1 F12 1.592(4) . ? P1 F13 1.593(4) . ? P1 F16 1.601(4) . ? P2 F21 1.532(5) . ? P2 F22 1.551(6) . ? P2 F24 1.552(5) . ? P2 F23 1.565(5) . ? P2 F25 1.568(5) . ? P2 F26 1.596(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 N31 Ru N21 78.32(16) . . ? N31 Ru S1 92.50(13) . . ? N21 Ru S1 170.07(11) . . ? N31 Ru S7 175.22(11) . . ? N21 Ru S7 100.86(12) . . ? S1 Ru S7 88.61(8) . . ? N31 Ru S10 99.94(13) . . ? N21 Ru S10 91.06(14) . . ? S1 Ru S10 86.77(9) . . ? S7 Ru S10 84.77(8) . . ? N31 Ru S4 92.38(13) . . ? N21 Ru S4 96.89(13) . . ? S1 Ru S4 87.18(9) . . ? S7 Ru S4 83.02(8) . . ? S10 Ru S4 166.49(5) . . ? C2 S1 C12 106.4(3) . . ? C2 S1 Ru 103.5(2) . . ? C12 S1 Ru 102.9(2) . . ? C3 C2 S1 105.7(4) . . ? C2 C3 S4 114.9(4) . . ? C5 S4 C3 100.7(3) . . ? C5 S4 Ru 104.28(19) . . ? C3 S4 Ru 101.1(2) . . ? C6 C5 S4 114.3(4) . . ? C5 C6 S7 106.2(4) . . ? C6 S7 C8 110.3(3) . . ? C6 S7 Ru 102.2(2) . . ? C8 S7 Ru 106.9(2) . . ? C9 C8 S7 112.2(4) . . ? C8 C9 S10 121.2(4) . . ? C9 S10 C11 103.3(4) . . ? C9 S10 Ru 103.5(2) . . ? C11 S10 Ru 102.9(3) . . ? C12 C11 S10 114.8(4) . . ? C11 C12 S1 106.2(5) . . ? C26 N21 C22 116.6(4) . . ? C26 N21 Ru 130.0(4) . . ? C22 N21 Ru 113.4(3) . . ? N21 C22 C23 123.9(4) . . ? N21 C22 C36 117.5(4) . . ? C23 C22 C36 118.6(4) . . ? C24 C23 C22 117.1(4) . . ? C24 C23 C42 123.0(5) . . ? C22 C23 C42 119.9(4) . . ? C25 C24 C23 118.6(5) . . ? C24 C25 C26 120.8(5) . . ? N21 C26 C25 123.0(5) . . ? C32 N31 C36 117.6(4) . . ? C32 N31 Ru 127.8(3) . . ? C36 N31 Ru 114.3(3) . . ? N31 C32 C33 122.9(5) . . ? C34 C33 C32 120.0(5) . . ? C33 C34 C35 119.2(5) . . ? C34 C35 C36 117.1(4) . . ? C34 C35 C41 124.1(4) . . ? C36 C35 C41 118.7(4) . . ? N31 C36 C35 122.9(4) . . ? N31 C36 C22 116.4(4) . . ? C35 C36 C22 120.7(4) . . ? C42 C41 C35 119.4(4) . . ? C42 C41 C51 119.5(5) . . ? C35 C41 C51 121.0(4) . . ? C41 C42 C23 122.5(5) . . ? C52 C51 C56 118.0(5) . . ? C52 C51 C41 123.7(5) . . ? C56 C51 C41 118.0(5) . . ? C53 C52 C51 121.0(6) . . ? C54 C53 C52 120.6(6) . . ? C53 C54 C55 120.4(6) . . ? C54 C55 C56 120.2(6) . . ? C55 C56 C51 120.0(6) . . ? F15 P1 F11 91.0(3) . . ? F15 P1 F14 90.1(2) . . ? F11 P1 F14 91.3(2) . . ? F15 P1 F12 89.8(3) . . ? F11 P1 F12 179.1(2) . . ? F14 P1 F12 89.1(2) . . ? F15 P1 F13 90.6(2) . . ? F11 P1 F13 89.4(2) . . ? F14 P1 F13 179.0(2) . . ? F12 P1 F13 90.2(2) . . ? F15 P1 F16 179.0(2) . . ? F11 P1 F16 89.9(3) . . ? F14 P1 F16 89.5(2) . . ? F12 P1 F16 89.3(3) . . ? F13 P1 F16 89.8(2) . . ? F21 P2 F22 89.9(5) . . ? F21 P2 F24 94.5(4) . . ? F22 P2 F24 90.5(3) . . ? F21 P2 F23 92.5(4) . . ? F22 P2 F23 177.6(4) . . ? F24 P2 F23 89.2(3) . . ? F21 P2 F25 89.8(4) . . ? F22 P2 F25 88.9(4) . . ? F24 P2 F25 175.7(4) . . ? F23 P2 F25 91.2(3) . . ? F21 P2 F26 178.1(4) . . ? F22 P2 F26 88.7(4) . . ? F24 P2 F26 86.8(4) . . ? F23 P2 F26 88.9(4) . . ? F25 P2 F26 88.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C2 C3 S4 56.3(5) . . . . ? C2 C3 S4 C5 75.6(5) . . . . ? C3 S4 C5 C6 -118.6(4) . . . . ? S4 C5 C6 S7 47.3(5) . . . . ? C5 C6 S7 C8 -172.2(4) . . . . ? C6 S7 C8 C9 140.7(5) . . . . ? S7 C8 C9 S10 -10.3(8) . . . . ? C8 C9 S10 C11 93.0(7) . . . . ? C9 S10 C11 C12 -81.3(6) . . . . ? S10 C11 C12 S1 -52.7(6) . . . . ? C11 C12 S1 C2 161.2(4) . . . . ? C12 S1 C2 C3 -160.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 25.91 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 1.259 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.104 #=END data_S10 #*Complex 10* _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 F12 N4 O2 P2 Ru S4' _chemical_formula_weight 923.75 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' '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 Monoclinic _symmetry_space_group_name_H-M C2/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 18.89(2) _cell_length_b 11.713(13) _cell_length_c 15.908(18) _cell_angle_alpha 90.00 _cell_angle_beta 104.060(10) _cell_angle_gamma 90.00 _cell_volume 3415(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.895 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4329 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.92 _reflns_number_total 2433 _reflns_number_gt 2127 _reflns_threshold_expression 2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1378P)^2^+33.7552P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2433 _refine_ls_number_parameters 219 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1644 _refine_ls_wR_factor_gt 0.1551 _refine_ls_goodness_of_fit_ref 0.829 _refine_ls_restrained_S_all 0.828 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.5000 0.41615(5) 0.2500 0.0250(3) Uani 1 d S . . S1 S 0.54496(7) 0.53698(13) 0.16193(9) 0.0314(4) Uani 1 d . . . C2 C 0.4710(3) 0.6294(6) 0.1072(4) 0.0416(15) Uani 1 d . . . H2A H 0.4580 0.6828 0.1476 0.050 Uiso 1 calc R . . H2B H 0.4845 0.6719 0.0611 0.050 Uiso 1 calc R . . C3 C 0.4078(3) 0.5478(6) 0.0705(4) 0.0426(15) Uani 1 d . . . H3A H 0.4197 0.5039 0.0241 0.051 Uiso 1 calc R . . H3B H 0.3647 0.5926 0.0455 0.051 Uiso 1 calc R . . S4 S 0.38587(7) 0.44829(14) 0.14949(9) 0.0332(4) Uani 1 d . . . C5 C 0.3370(3) 0.5444(6) 0.2077(4) 0.0463(16) Uani 1 d . . . H5A H 0.3022 0.5887 0.1653 0.056 Uiso 1 calc R . . H5B H 0.3095 0.4981 0.2392 0.056 Uiso 1 calc R . . C6 C 0.3847(3) 0.6263(6) 0.2711(4) 0.0421(15) Uani 1 d . . . H6A H 0.3565 0.6646 0.3062 0.050 Uiso 1 calc R . . H6B H 0.4061 0.6833 0.2406 0.050 Uiso 1 calc R . . N21 N 0.5381(2) 0.2732(4) 0.1886(3) 0.0319(12) Uani 1 d . . . C22 C 0.5770(3) 0.2759(7) 0.1284(4) 0.0490(17) Uani 1 d . . . H22 H 0.5913 0.3467 0.1116 0.059 Uiso 1 calc R . . C23 C 0.5972(4) 0.1788(8) 0.0898(5) 0.063(2) Uani 1 d . . . H23 H 0.6237 0.1840 0.0478 0.076 Uiso 1 calc R . . C24 C 0.5769(4) 0.0763(8) 0.1155(6) 0.066(3) Uani 1 d . . . H24 H 0.5890 0.0099 0.0902 0.079 Uiso 1 calc R . . C25 C 0.5377(3) 0.0688(6) 0.1799(5) 0.0480(19) Uani 1 d . . . C26 C 0.5198(3) 0.1702(6) 0.2158(4) 0.0333(14) Uani 1 d . . . C27 C 0.5184(4) -0.0412(8) 0.2119(6) 0.069(3) Uani 1 d . . . O28 O 0.5307(3) -0.1317(6) 0.1799(5) 0.092(2) Uani 1 d . . . P P 0.20671(9) 0.56965(17) -0.11350(12) 0.0493(5) Uani 1 d D . . F11 F 0.2284(6) 0.5843(12) -0.0106(6) 0.076(3) Uiso 0.546(16) d PD A 1 F12 F 0.1859(6) 0.5467(14) -0.2165(6) 0.093(4) Uiso 0.546(16) d PD A 1 F13 F 0.1617(7) 0.6877(11) -0.1128(7) 0.085(4) Uiso 0.546(16) d PD A 1 F14 F 0.2539(7) 0.4535(12) -0.1043(8) 0.100(4) Uiso 0.546(16) d PD A 1 F15 F 0.1337(7) 0.5042(13) -0.1154(9) 0.106(4) Uiso 0.546(16) d PD A 1 F16 F 0.2799(7) 0.6318(15) -0.1134(10) 0.124(5) Uiso 0.546(16) d PD A 1 F11 F 0.2137(7) 0.5374(14) -0.0133(7) 0.076(4) Uiso 0.454(16) d PD A 2 F12 F 0.1974(7) 0.6041(16) -0.2136(8) 0.086(4) Uiso 0.454(16) d PD A 2 F13 F 0.1363(8) 0.6446(14) -0.1195(9) 0.088(4) Uiso 0.454(16) d PD A 2 F14 F 0.2806(7) 0.5023(13) -0.1107(8) 0.083(4) Uiso 0.454(16) d PD A 2 F15 F 0.1582(11) 0.4572(16) -0.1302(14) 0.134(7) Uiso 0.454(16) d PD A 2 F16 F 0.2600(10) 0.6796(15) -0.0909(13) 0.129(7) Uiso 0.454(16) d PD A 2 N100 N 0.4105(4) 0.2634(8) 0.0035(5) 0.087(2) Uani 1 d . . . C101 C 0.3578(4) 0.2296(7) -0.0355(5) 0.061(2) Uani 1 d . . . C102 C 0.2902(5) 0.1846(9) -0.0890(6) 0.086(3) Uani 1 d . . . H10A H 0.2995 0.1498 -0.1399 0.104 Uiso 1 calc R . . H10B H 0.2557 0.2456 -0.1057 0.104 Uiso 1 calc R . . H10C H 0.2706 0.1286 -0.0568 0.104 Uiso 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 0.0305(3) 0.0216(6) 0.0225(4) 0.000 0.0056(2) 0.000 S1 0.0345(7) 0.0301(11) 0.0293(8) 0.0065(6) 0.0068(5) -0.0012(5) C2 0.042(3) 0.036(4) 0.042(4) 0.016(3) 0.001(2) -0.002(3) C3 0.045(3) 0.048(5) 0.030(3) 0.007(3) -0.002(2) -0.004(3) S4 0.0319(7) 0.0368(11) 0.0282(8) -0.0039(6) 0.0020(5) -0.0054(5) C5 0.029(3) 0.059(5) 0.049(4) -0.008(3) 0.004(2) 0.009(3) C6 0.045(3) 0.029(4) 0.049(4) -0.009(3) 0.004(2) 0.011(3) N21 0.036(2) 0.026(4) 0.031(3) -0.008(2) 0.0030(16) 0.0021(19) C22 0.054(3) 0.055(5) 0.044(4) -0.010(3) 0.021(3) 0.012(3) C23 0.078(5) 0.057(7) 0.061(5) -0.014(4) 0.028(4) 0.012(4) C24 0.063(4) 0.065(7) 0.064(6) -0.031(4) 0.007(4) 0.024(4) C25 0.045(3) 0.026(6) 0.061(5) -0.006(3) -0.009(3) 0.007(3) C26 0.037(3) 0.019(5) 0.038(4) -0.006(3) -0.001(2) 0.006(2) C27 0.049(4) 0.030(7) 0.111(8) -0.021(5) -0.012(4) 0.007(3) O28 0.086(4) 0.031(5) 0.144(6) -0.023(4) 0.000(4) 0.012(3) P 0.0409(8) 0.0640(15) 0.0413(11) 0.0036(8) 0.0064(6) 0.0067(7) N100 0.066(4) 0.121(7) 0.073(5) -0.022(4) 0.019(3) -0.024(4) C101 0.066(5) 0.060(6) 0.062(5) 0.000(4) 0.025(4) -0.012(4) C102 0.073(5) 0.091(8) 0.086(7) 0.017(5) 0.003(4) -0.027(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N21 2.149(5) . ? Ru N21 2.149(5) 2_655 ? Ru S1 2.295(2) 2_655 ? Ru S1 2.295(2) . ? Ru S4 2.382(2) 2_655 ? Ru S4 2.382(2) . ? S1 C2 1.814(6) . ? S1 C6 1.819(6) 2_655 ? C2 C3 1.530(8) . ? C3 S4 1.833(6) . ? S4 C5 1.842(6) . ? C5 C6 1.520(9) . ? C6 S1 1.819(6) 2_655 ? N21 C22 1.343(7) . ? N21 C26 1.355(8) . ? C22 C23 1.389(10) . ? C23 C24 1.354(12) . ? C24 C25 1.403(12) . ? C25 C26 1.395(10) . ? C25 C27 1.464(13) . ? C26 C26 1.462(12) 2_655 ? C27 O28 1.223(10) . ? C27 C27 1.54(2) 2_655 ? P F16 1.562(12) . ? P F15 1.571(11) . ? P F13 1.577(11) . ? P F15 1.590(15) . ? P F14 1.594(11) . ? P F11 1.598(10) . ? P F12 1.610(12) . ? P F12 1.612(10) . ? P F11 1.612(11) . ? P F14 1.613(11) . ? P F16 1.620(14) . ? P F13 1.625(10) . ? N100 C101 1.110(10) . ? C101 C102 1.451(11) . ? 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 N21 Ru N21 77.6(3) . 2_655 ? N21 Ru S1 166.56(14) . 2_655 ? N21 Ru S1 89.35(16) 2_655 2_655 ? N21 Ru S1 89.35(16) . . ? N21 Ru S1 166.56(14) 2_655 . ? S1 Ru S1 103.84(11) 2_655 . ? N21 Ru S4 94.57(13) . 2_655 ? N21 Ru S4 99.60(13) 2_655 2_655 ? S1 Ru S4 84.36(8) 2_655 2_655 ? S1 Ru S4 84.45(8) . 2_655 ? N21 Ru S4 99.60(13) . . ? N21 Ru S4 94.57(13) 2_655 . ? S1 Ru S4 84.45(8) 2_655 . ? S1 Ru S4 84.36(8) . . ? S4 Ru S4 161.81(9) 2_655 . ? C2 S1 C6 107.8(3) . 2_655 ? C2 S1 Ru 107.7(2) . . ? C6 S1 Ru 108.9(2) 2_655 . ? C3 C2 S1 104.4(5) . . ? C2 C3 S4 114.9(4) . . ? C3 S4 C5 100.4(3) . . ? C3 S4 Ru 103.99(19) . . ? C5 S4 Ru 104.0(2) . . ? C6 C5 S4 115.5(4) . . ? C5 C6 S1 104.9(5) . 2_655 ? C22 N21 C26 118.4(5) . . ? C22 N21 Ru 127.4(5) . . ? C26 N21 Ru 114.2(4) . . ? N21 C22 C23 123.5(7) . . ? C24 C23 C22 117.7(7) . . ? C23 C24 C25 120.9(7) . . ? C26 C25 C24 118.0(7) . . ? C26 C25 C27 120.0(7) . . ? C24 C25 C27 121.9(7) . . ? N21 C26 C25 121.4(6) . . ? N21 C26 C26 117.0(3) . 2_655 ? C25 C26 C26 121.6(4) . 2_655 ? O28 C27 C25 121.9(9) . . ? O28 C27 C27 119.8(6) . 2_655 ? C25 C27 C27 118.3(5) . 2_655 ? F16 P F15 178.2(8) . . ? F16 P F13 118.3(9) . . ? F15 P F13 63.1(8) . . ? F16 P F15 149.3(10) . . ? F15 P F15 29.0(8) . . ? F13 P F15 90.5(9) . . ? F16 P F14 57.4(8) . . ? F15 P F14 121.1(8) . . ? F13 P F14 175.4(7) . . ? F15 P F14 93.4(9) . . ? F16 P F11 86.7(7) . . ? F15 P F11 94.5(6) . . ? F13 P F11 90.3(6) . . ? F15 P F11 104.8(9) . . ? F14 P F11 91.1(6) . . ? F16 P F12 76.6(8) . . ? F15 P F12 102.6(7) . . ? F13 P F12 84.9(7) . . ? F15 P F12 97.0(10) . . ? F14 P F12 92.1(7) . . ? F11 P F12 157.8(7) . . ? F16 P F12 94.4(7) . . ? F15 P F12 84.4(7) . . ? F13 P F12 92.1(7) . . ? F15 P F12 72.8(9) . . ? F14 P F12 86.6(6) . . ? F11 P F12 176.5(6) . . ? F12 P F12 25.3(6) . . ? F16 P F11 104.3(8) . . ? F15 P F11 76.5(7) . . ? F13 P F11 93.2(6) . . ? F15 P F11 82.9(9) . . ? F14 P F11 89.7(6) . . ? F11 P F11 22.0(5) . . ? F12 P F11 178.2(7) . . ? F12 P F11 155.1(7) . . ? F16 P F14 85.6(8) . . ? F15 P F14 93.0(7) . . ? F13 P F14 156.1(7) . . ? F15 P F14 66.4(9) . . ? F14 P F14 28.3(5) . . ? F11 P F14 89.9(6) . . ? F12 P F14 103.1(7) . . ? F12 P F14 86.8(7) . . ? F11 P F14 78.6(6) . . ? F16 P F16 29.2(7) . . ? F15 P F16 152.5(9) . . ? F13 P F16 92.3(9) . . ? F15 P F16 176.0(10) . . ? F14 P F16 83.9(8) . . ? F11 P F16 72.3(8) . . ? F12 P F16 86.1(9) . . ? F12 P F16 110.0(9) . . ? F11 P F16 94.0(9) . . ? F14 P F16 110.5(8) . . ? F16 P F13 93.9(8) . . ? F15 P F13 87.6(7) . . ? F13 P F13 24.7(5) . . ? F15 P F13 115.2(9) . . ? F14 P F13 151.3(7) . . ? F11 P F13 84.6(6) . . ? F12 P F13 82.0(7) . . ? F12 P F13 98.6(7) . . ? F11 P F13 96.3(6) . . ? F14 P F13 174.5(6) . . ? F16 P F13 67.7(8) . . ? N100 C101 C102 177.9(9) . . ? 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 S1 C2 C3 S4 52.3(5) . . . . ? C2 C3 S4 C5 76.4(5) . . . . ? C3 S4 C5 C6 -75.6(6) . . . . ? S4 C5 C6 S1 -50.7(6) . . . 2_655 ? C5 C6 S1 C2 163.1(4) . . 2_655 2_655 ? C6 S1 C2 C3 -166.9(4) . 2_655 2_655 2_655 ? S1 C2 C3 S4 52.3(5) 2_655 2_655 2_655 2_655 ? C2 C3 S4 C5 76.4(5) 2_655 2_655 2_655 2_655 ? C3 S4 C5 C6 -75.6(6) 2_655 2_655 2_655 2_655 ? S4 C5 C6 S1 -50.7(6) 2_655 2_655 2_655 . ? C5 C6 S1 C2 163.1(4) 2_655 2_655 . . ? C6 S1 C2 C3 -166.9(4) 2_655 . . . ? _diffrn_measured_fraction_theta_max 0.346 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.346 _refine_diff_density_max 0.746 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.115