Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Belsky, Vitaly K.' 'Kron, Tatyana E.' 'Nadtochenko, Victor A.' 'Smirnov, Vyacheslav A.' 'Strizhakova, Nataly G.' 'Varzataskii, Oleg A.' 'Voloshin, Yan Z.' 'Zavodnik, Valery E.' _publ_contact_author_name 'Prof Yan Z Voloshin' _publ_contact_author_address ; Karpov Institute of Physical Chemistry 10 Vorontsovo Pole Moscow 103064 RUSSIAN FEDERATION ; _publ_contact_author_email 'VOLOSHIN@CC.NIFHI.AC.RU' _publ_section_title ; Encapsulation of ruthenium(II) with macrobicyclic dioxime-functionalized ligands: on the way to the new types of DNA-cleaving agents and probes. ; data_No2 _database_code_CSD 168668 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 B2 Cl6 N6 O6 Ru' _chemical_formula_weight 701.73 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' 'B' 'B' 0.0013 0.0007 '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' '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 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 26.238(5) _cell_length_b 7.999(2) _cell_length_c 13.927(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.76(3) _cell_angle_gamma 90.00 _cell_volume 2609.(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 12.4 _cell_measurement_theta_max 13.8 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 1.258 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5291 _exptl_absorpt_correction_T_max 0.8338 _exptl_absorpt_process_details ? _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 filter _diffrn_measurement_device_type CAD4 _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 100 _diffrn_standards_decay_% .5 _diffrn_reflns_number 1934 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.47 _reflns_number_total 1934 _reflns_number_gt 1840 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef 0.0030 _refine_ls_number_reflns 1840 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.816 _refine_ls_shift/su_mean 0.245 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 0.5000 0.4874(1) 0.2500 0.028(1) Uani 1 2 d S . . Cl1 Cl 0.5478(1) 0.2268(1) 0.5614(1) 0.057(1) Uani 1 1 d . . . Cl2 Cl 0.5910(1) 0.2306(1) 0.0876(1) 0.058(1) Uani 1 1 d . . . Cl3 Cl 0.5697(1) 1.0053(1) 0.3263(1) 0.050(1) Uani 1 1 d . . . O1 O 0.6018(1) 0.3916(3) 0.4475(2) 0.055(1) Uani 1 1 d . . . O2 O 0.6169(1) 0.4026(4) 0.2865(2) 0.062(1) Uani 1 1 d . . . O3 O 0.6095(1) 0.6641(3) 0.3720(2) 0.047(1) Uani 1 1 d . . . N1 N 0.5442(1) 0.3881(3) 0.3937(2) 0.045(1) Uani 1 1 d . . . N2 N 0.5607(1) 0.3948(4) 0.2178(2) 0.048(1) Uani 1 1 d . . . N3 N 0.5522(1) 0.6800(3) 0.3095(2) 0.041(1) Uani 1 1 d . . . C1 C 0.5154(1) 0.3170(3) 0.4376(2) 0.036(1) Uani 1 1 d . . . C2 C 0.5445(1) 0.3191(3) 0.1257(2) 0.038(1) Uani 1 1 d . . . C3 C 0.5301(1) 0.8286(3) 0.2840(2) 0.034(1) Uani 1 1 d . . . C4 C 0.6969(2) 0.4832(5) 0.4652(3) 0.054(1) Uani 1 1 d . . . C5 C 0.7161(2) 0.5632(6) 0.5747(3) 0.061(1) Uani 1 1 d . . . C6 C 0.7792(2) 0.5467(8) 0.6493(5) 0.083(1) Uani 1 1 d . . . C7 C 0.7958(3) 0.6246(15) 0.7566(6) 0.136(1) Uani 1 1 d . . . B B 0.6303(2) 0.4860(4) 0.3912(3) 0.041(1) Uani 1 1 d . . . H41 H 0.7190(2) 0.5380(6) 0.4320(4) 0.0752(7) Uiso 1 1 d . . . H42 H 0.7070(2) 0.3740(7) 0.4780(4) 0.0866(7) Uiso 1 1 d . . . H51 H 0.7074(2) 0.6770(6) 0.5670(3) 0.0742(6) Uiso 1 1 d . . . H52 H 0.6990(2) 0.5260(6) 0.6120(4) 0.0694(8) Uiso 1 1 d . . . H61 H 0.7890(2) 0.4320(7) 0.6650(4) 0.0096(2) Uiso 1 1 d . . . H62 H 0.7970(2) 0.5800(8) 0.6110(4) 0.0973(10) Uiso 1 1 d . . . H71 H 0.7920(4) 0.733(1) 0.7590(8) 0.1894(14) Uiso 1 1 d . . . H72 H 0.8400(4) 0.585(1) 0.8220(7) 0.1907(14) Uiso 1 1 d . . . H73 H 0.7750(3) 0.567(1) 0.8030(6) 0.1383(10) Uiso 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 0.03599(2) 0.01901(0) 0.03000(1) 0.000 0.01499(1) 0.000 Cl1 0.07495(5) 0.05601(2) 0.03899(1) 0.01801(1) 0.02496(2) 0.01298(2) Cl2 0.06605(5) 0.05700(2) 0.06500(2) -0.01499(2) 0.04305(3) 0.00198(2) Cl3 0.05498(5) 0.02301(1) 0.06803(2) -0.00601(1) 0.02499(3) -0.00899(1) O1 0.04005(10) 0.06098(6) 0.04993(5) 0.02294(4) 0.00710(6) -0.00099(6) O2 0.03605(10) 0.08291(8) 0.05899(5) -0.03100(6) 0.01590(6) 0.00502(7) O3 0.03494(9) 0.03004(3) 0.06094(5) -0.00101(4) 0.00907(6) -0.00301(5) N1 0.04292(12) 0.04411(5) 0.03990(4) 0.01299(4) 0.01199(6) -0.00198(6) N2 0.04215(11) 0.05595(7) 0.04796(5) -0.01696(5) 0.02095(6) 0.00104(7) N3 0.03698(11) 0.02398(4) 0.05098(5) 0.00099(3) 0.01186(6) -0.00003(5) C1 0.05601(13) 0.02506(4) 0.02897(4) 0.00396(3) 0.02013(6) 0.00403(5) C2 0.05288(14) 0.02801(4) 0.04298(5) -0.00303(4) 0.02997(7) -0.00204(6) C3 0.04504(13) 0.02199(3) 0.03805(4) -0.00200(3) 0.02094(6) -0.00399(5) C4 0.03809(17) 0.04982(8) 0.06188(9) -0.00303(6) 0.01289(10) 0.00517(9) C5 0.04328(19) 0.06591(11) 0.05912(9) -0.00293(8) 0.00868(10) 0.00096(11) C6 0.0471(2) 0.08699(15) 0.08394(15) -0.00095(12) 0.00131(14) -0.00319(14) C7 0.0900(2) 0.01504(3) 0.08893(11) -0.02188(5) -0.02498(13) -0.00408(7) B 0.0398(2) 0.03615(6) 0.04497(7) -0.00093(5) 0.01726(10) 0.00299(7) _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 1.9726(7) 2_655 ? Ru N1 1.9726(7) . ? Ru N3 1.9782(4) . ? Ru N3 1.9782(4) 2_655 ? Ru N2 1.9824(4) 2_655 ? Ru N2 1.9824(4) . ? Cl1 C1 1.7018(5) . ? Cl2 C2 1.6891(3) . ? Cl3 C3 1.6949(4) . ? O1 N1 1.3517(5) . ? O1 B 1.5070(4) . ? O2 N2 1.3499(6) . ? O2 B 1.4948(4) . ? O3 N3 1.3623(5) . ? O3 B 1.5056(4) . ? N1 C1 1.2977(3) . ? N2 C2 1.3046(3) . ? N3 C3 1.2999(3) . ? C1 C2 1.4144(6) 2_655 ? C2 C1 1.4144(6) 2_655 ? C3 C3 1.4300(6) 2_655 ? C4 C5 1.5157(5) . ? C4 B 1.5802(7) . ? C5 C6 1.5121(7) . ? C6 C7 1.4907(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 132.51(2) 2_655 . ? N1 Ru N3 135.928(14) 2_655 . ? N1 Ru N3 84.76(3) . . ? N1 Ru N3 84.76(3) 2_655 2_655 ? N1 Ru N3 135.928(13) . 2_655 ? N3 Ru N3 77.71(3) . 2_655 ? N1 Ru N2 85.06(2) 2_655 2_655 ? N1 Ru N2 77.60(2) . 2_655 ? N3 Ru N2 132.172(11) . 2_655 ? N3 Ru N2 84.875(16) 2_655 2_655 ? N1 Ru N2 77.60(3) 2_655 . ? N1 Ru N2 85.06(2) . . ? N3 Ru N2 84.875(16) . . ? N3 Ru N2 132.172(10) 2_655 . ? N2 Ru N2 136.114(15) 2_655 . ? N1 O1 B 114.50(2) . . ? N2 O2 B 114.46(3) . . ? N3 O3 B 114.151(13) . . ? C1 N1 O1 119.40(2) . . ? C1 N1 Ru 116.96(2) . . ? O1 N1 Ru 123.64(3) . . ? C2 N2 O2 119.11(3) . . ? C2 N2 Ru 117.17(3) . . ? O2 N2 Ru 123.695(16) . . ? C3 N3 O3 119.199(14) . . ? C3 N3 Ru 117.28(3) . . ? O3 N3 Ru 123.484(17) . . ? N1 C1 C2 114.88(2) . 2_655 ? N1 C1 Cl1 122.13(2) . . ? C2 C1 Cl1 122.99(3) 2_655 . ? N2 C2 C1 113.38(3) . 2_655 ? N2 C2 Cl2 122.81(3) . . ? C1 C2 Cl2 123.805(16) 2_655 . ? N3 C3 C3 113.864(13) . 2_655 ? N3 C3 Cl3 122.65(2) . . ? C3 C3 Cl3 123.476(13) 2_655 . ? C5 C4 B 114.75(4) . . ? C6 C5 C4 114.83(4) . . ? C7 C6 C5 112.88(4) . . ? O2 B O3 109.98(2) . . ? O2 B O1 109.26(2) . . ? O3 B O1 109.99(2) . . ? O2 B C4 109.56(3) . . ? O3 B C4 109.589(15) . . ? O1 B C4 108.43(2) . . ? _diffrn_measured_fraction_theta_max 0.131 _diffrn_reflns_theta_full 25.47 _diffrn_measured_fraction_theta_full 0.131 _refine_diff_density_max 0.468 _refine_diff_density_min -0.996 _refine_diff_density_rms 0.003 data_No6 _database_code_CSD 168669 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H24 B N3 O6 Ru0.50' _chemical_formula_weight 523.82 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' 'B' 'B' 0.0013 0.0007 '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' _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 17.654(2) _cell_length_b 25.336(4) _cell_length_c 13.483(1) _cell_angle_alpha 90.00 _cell_angle_beta 120.99(1) _cell_angle_gamma 90.00 _cell_volume 5169.9(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 11.8 _cell_measurement_theta_max 12.7 _exptl_crystal_description prizm _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.369 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8429 _exptl_absorpt_correction_T_max 0.9038 _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 filter _diffrn_measurement_device_type CAD4 _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 100 _diffrn_standards_decay_% .9 _diffrn_reflns_number 3931 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.97 _reflns_number_total 3757 _reflns_number_gt 3757 _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^)+(0.0561P)^2^+3.1626P] 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 0.00093(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3757 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.624 _refine_ls_shift/su_mean 0.052 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 0.719473(10) 0.2500 0.03445(10) Uani 1 d S . . O1 O 0.42823(13) 0.66405(7) 0.37748(16) 0.0482(4) Uani 1 d . . . O2 O 0.53196(12) 0.73799(7) 0.48489(15) 0.0473(4) Uani 1 d . . . O3 O 0.37922(12) 0.75744(7) 0.32654(15) 0.0459(4) Uani 1 d . . . N1 N 0.45860(14) 0.65867(8) 0.30247(18) 0.0417(4) Uani 1 d . . . N2 N 0.56669(13) 0.74192(8) 0.41459(17) 0.0407(4) Uani 1 d . . . N3 N 0.40029(14) 0.76010(8) 0.24194(17) 0.0399(4) Uani 1 d . . . B1 B 0.4372(2) 0.71982(12) 0.4238(2) 0.0441(6) Uani 1 d . . . C1 C 0.47961(17) 0.61172(9) 0.2846(2) 0.0439(6) Uani 1 d . . . O4 O 0.45932(13) 0.56748(7) 0.32172(18) 0.0533(5) Uani 1 d . . . C2 C 0.5270(2) 0.53162(10) 0.3885(2) 0.0514(7) Uani 1 d . . . C3 C 0.6109(3) 0.54759(18) 0.4637(4) 0.0775(10) Uani 1 d . . . C4 C 0.6724(4) 0.5084(3) 0.5300(5) 0.1124(19) Uani 1 d . . . C5 C 0.6484(5) 0.4570(3) 0.5212(6) 0.120(2) Uani 1 d . . . C6 C 0.5632(5) 0.44263(17) 0.4447(5) 0.1014(18) Uani 1 d . . . C7 C 0.5023(3) 0.47978(12) 0.3782(3) 0.0688(9) Uani 1 d . . . C8 C 0.63261(16) 0.77419(9) 0.4441(2) 0.0422(5) Uani 1 d . . . O5 O 0.67600(13) 0.79953(8) 0.54752(15) 0.0544(5) Uani 1 d . . . C9 C 0.66055(19) 0.85364(12) 0.5431(3) 0.0576(7) Uani 1 d . . . C10 C 0.5819(3) 0.87493(17) 0.4579(5) 0.1171(19) Uani 1 d . . . C11 C 0.5728(4) 0.9299(2) 0.4512(6) 0.155(3) Uani 1 d . . . C12 C 0.6403(5) 0.9595(2) 0.5362(8) 0.174(3) Uani 1 d . . . C13 C 0.7161(4) 0.9375(2) 0.6216(5) 0.124(2) Uani 1 d . . . C14 C 0.7270(2) 0.88416(14) 0.6241(3) 0.0718(9) Uani 1 d . . . C15 C 0.34361(15) 0.78103(9) 0.1426(2) 0.0405(5) Uani 1 d . . . O6 O 0.26558(11) 0.80338(7) 0.11232(16) 0.0494(4) Uani 1 d . . . C16 C 0.26011(17) 0.83765(10) 0.1905(2) 0.0499(6) Uani 1 d . . . C17 C 0.1886(2) 0.83357(14) 0.2015(3) 0.0666(8) Uani 1 d . . . C18 C 0.1788(3) 0.86839(18) 0.2739(4) 0.0828(11) Uani 1 d . . . C19 C 0.2401(3) 0.90598(17) 0.3322(4) 0.0976(14) Uani 1 d . . . C20 C 0.3122(4) 0.9100(2) 0.3194(6) 0.125(2) Uani 1 d . . . C21 C 0.3225(3) 0.87535(16) 0.2477(5) 0.0981(15) Uani 1 d . . . C22 C 0.4059(2) 0.71990(12) 0.5151(3) 0.0539(6) Uani 1 d . . . C23 C 0.3945(3) 0.77447(14) 0.5526(3) 0.0642(8) Uani 1 d . . . C24 C 0.3677(3) 0.7740(2) 0.6431(4) 0.0872(13) Uani 1 d . . . C25 C 0.3556(6) 0.8281(4) 0.6780(9) 0.145(3) Uani 1 d . . . H3 H 0.625(2) 0.5795(16) 0.466(3) 0.075(12) Uiso 1 d . . . H4 H 0.722(3) 0.5245(18) 0.568(4) 0.088(15) Uiso 1 d . . . H5 H 0.687(3) 0.436(2) 0.572(5) 0.130(18) Uiso 1 d . . . H6 H 0.546(3) 0.409(2) 0.434(4) 0.123(18) Uiso 1 d . . . H7 H 0.446(3) 0.4709(16) 0.324(3) 0.087(14) Uiso 1 d . . . H10 H 0.5383 0.8616 0.3815 0.168 Uiso 1 d . . . H11 H 0.5188 0.9370 0.3758 0.120 Uiso 1 d . . . H12 H 0.6489 0.9973 0.5292 0.123 Uiso 1 d . . . H13 H 0.7682 0.9549 0.6798 0.109 Uiso 1 d . . . H14 H 0.7797 0.8659 0.6780 0.065 Uiso 1 d . . . H17 H 0.149(3) 0.8041(17) 0.167(4) 0.095(13) Uiso 1 d . . . H18 H 0.126(3) 0.8597(17) 0.276(3) 0.095(13) Uiso 1 d . . . H19 H 0.239(3) 0.9341(18) 0.389(4) 0.106(13) Uiso 1 d . . . H20 H 0.355(3) 0.942(2) 0.345(4) 0.128(17) Uiso 1 d . . . H21 H 0.376(3) 0.8813(18) 0.236(4) 0.116(15) Uiso 1 d . . . H221 H 0.453(2) 0.7006(13) 0.583(3) 0.058(8) Uiso 1 d . . . H222 H 0.353(2) 0.7019(13) 0.482(3) 0.059(9) Uiso 1 d . . . H231 H 0.446(2) 0.7955(14) 0.585(3) 0.072(10) Uiso 1 d . . . H232 H 0.345(3) 0.7926(15) 0.478(3) 0.081(11) Uiso 1 d . . . H241 H 0.413(3) 0.7519(17) 0.712(4) 0.086(12) Uiso 1 d . . . H242 H 0.317(3) 0.754(2) 0.617(4) 0.100(15) Uiso 1 d . . . H251 H 0.325(4) 0.827(3) 0.719(6) 0.17(2) Uiso 1 d . . . H252 H 0.424(4) 0.847(2) 0.721(5) 0.16(2) Uiso 1 d . . . H253 H 0.327(6) 0.843(3) 0.633(7) 0.17(4) Uiso 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 0.04206(15) 0.02467(15) 0.03579(15) 0.000 0.01946(11) 0.000 O1 0.0670(11) 0.0352(9) 0.0577(10) 0.0033(8) 0.0430(10) 0.0029(8) O2 0.0560(10) 0.0499(10) 0.0387(9) 0.0004(7) 0.0262(8) 0.0024(8) O3 0.0533(10) 0.0436(9) 0.0462(9) 0.0040(8) 0.0294(8) 0.0108(8) N1 0.0504(11) 0.0314(11) 0.0504(11) 0.0010(8) 0.0309(10) 0.0006(8) N2 0.0469(11) 0.0364(10) 0.0368(10) 0.0004(8) 0.0201(9) 0.0017(9) N3 0.0474(11) 0.0313(9) 0.0393(10) 0.0000(8) 0.0212(9) 0.0035(8) B1 0.0546(15) 0.0356(14) 0.0451(14) 0.0035(12) 0.0278(12) 0.0047(12) C1 0.0527(14) 0.0270(12) 0.0576(15) 0.0007(10) 0.0324(12) -0.0014(10) O4 0.0683(12) 0.0300(9) 0.0775(13) 0.0075(8) 0.0489(11) 0.0000(8) C2 0.079(2) 0.0365(14) 0.0586(16) 0.0058(11) 0.0492(16) 0.0085(12) C3 0.091(3) 0.070(2) 0.079(2) 0.0157(19) 0.049(2) 0.011(2) C4 0.092(4) 0.151(6) 0.090(3) 0.038(3) 0.044(3) 0.030(4) C5 0.171(6) 0.115(5) 0.121(4) 0.072(4) 0.108(5) 0.089(5) C6 0.191(6) 0.049(2) 0.114(4) 0.030(2) 0.114(4) 0.041(3) C7 0.121(3) 0.0361(16) 0.078(2) 0.0063(15) 0.072(2) 0.0058(17) C8 0.0477(13) 0.0334(13) 0.0368(11) -0.0013(9) 0.0154(10) 0.0025(10) O5 0.0625(11) 0.0462(10) 0.0397(9) -0.0075(8) 0.0157(9) -0.0015(9) C9 0.0569(16) 0.0480(16) 0.0656(18) -0.0187(13) 0.0299(14) -0.0081(13) C10 0.081(3) 0.060(2) 0.146(4) -0.038(3) 0.013(3) 0.009(2) C11 0.121(4) 0.076(3) 0.196(6) -0.041(4) 0.030(4) 0.024(3) C12 0.170(6) 0.061(3) 0.252(9) -0.064(4) 0.080(6) -0.010(4) C13 0.107(4) 0.076(3) 0.147(5) -0.050(3) 0.035(3) -0.028(3) C14 0.070(2) 0.067(2) 0.072(2) -0.0239(17) 0.0317(17) -0.0212(16) C15 0.0426(12) 0.0282(11) 0.0441(12) 0.0000(10) 0.0176(10) 0.0015(10) O6 0.0439(9) 0.0430(10) 0.0512(10) 0.0003(8) 0.0174(8) 0.0072(8) C16 0.0489(14) 0.0340(13) 0.0594(16) 0.0022(11) 0.0225(12) 0.0092(11) C17 0.0618(19) 0.068(2) 0.070(2) -0.0101(16) 0.0343(16) -0.0062(16) C18 0.080(2) 0.084(3) 0.100(3) -0.009(2) 0.057(2) 0.005(2) C19 0.111(3) 0.071(3) 0.119(3) -0.033(2) 0.065(3) 0.008(2) C20 0.115(4) 0.080(3) 0.204(6) -0.082(4) 0.100(4) -0.035(3) C21 0.085(3) 0.062(2) 0.166(5) -0.050(3) 0.078(3) -0.0207(19) C22 0.0647(17) 0.0508(16) 0.0559(15) 0.0055(14) 0.0381(14) 0.0065(15) C23 0.075(2) 0.066(2) 0.0630(19) -0.0078(16) 0.0438(17) 0.0056(17) C24 0.082(3) 0.126(4) 0.068(2) -0.014(2) 0.050(2) 0.011(3) C25 0.146(6) 0.180(8) 0.129(6) -0.063(6) 0.084(5) 0.026(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 N1 1.985(2) 2_655 ? Ru N1 1.985(2) . ? Ru N2 1.986(2) . ? Ru N2 1.986(2) 2_655 ? Ru N3 1.993(2) 2_655 ? Ru N3 1.993(2) . ? O1 N1 1.374(3) . ? O1 B1 1.520(3) . ? O2 N2 1.372(3) . ? O2 B1 1.506(4) . ? O3 N3 1.372(3) . ? O3 B1 1.514(3) . ? N1 C1 1.305(3) . ? N2 C8 1.305(3) . ? N3 C15 1.302(3) . ? B1 C22 1.588(4) . ? C1 O4 1.349(3) . ? C1 C1 1.441(5) 2_655 ? O4 C2 1.399(3) . ? C2 C3 1.357(5) . ? C2 C7 1.368(4) . ? C3 C4 1.402(7) . ? C4 C5 1.354(9) . ? C5 C6 1.364(9) . ? C6 C7 1.362(6) . ? C8 O5 1.358(3) . ? C8 C15 1.442(3) 2_655 ? O5 C9 1.393(4) . ? C9 C14 1.359(4) . ? C9 C10 1.377(5) . ? C10 C11 1.398(7) . ? C11 C12 1.375(8) . ? C12 C13 1.357(8) . ? C13 C14 1.362(6) . ? C15 O6 1.344(3) . ? C15 C8 1.442(3) 2_655 ? O6 C16 1.407(3) . ? C16 C17 1.349(4) . ? C16 C21 1.359(5) . ? C17 C18 1.391(5) . ? C18 C19 1.349(6) . ? C19 C20 1.375(7) . ? C20 C21 1.385(6) . ? C22 C23 1.521(4) . ? C23 C24 1.520(5) . ? C24 C25 1.499(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 N1 78.20(11) 2_655 . ? N1 Ru N2 120.35(9) 2_655 . ? N1 Ru N2 86.51(9) . . ? N1 Ru N2 86.51(8) 2_655 2_655 ? N1 Ru N2 120.35(9) . 2_655 ? N2 Ru N2 146.72(12) . 2_655 ? N1 Ru N3 86.75(8) 2_655 2_655 ? N1 Ru N3 149.12(9) . 2_655 ? N2 Ru N3 78.02(8) . 2_655 ? N2 Ru N3 84.94(8) 2_655 2_655 ? N1 Ru N3 149.12(9) 2_655 . ? N1 Ru N3 86.75(8) . . ? N2 Ru N3 84.94(8) . . ? N2 Ru N3 78.02(8) 2_655 . ? N3 Ru N3 117.81(12) 2_655 . ? N1 O1 B1 113.38(18) . . ? N2 O2 B1 114.16(18) . . ? N3 O3 B1 113.50(18) . . ? C1 N1 O1 118.85(19) . . ? C1 N1 Ru 116.71(16) . . ? O1 N1 Ru 122.70(14) . . ? C8 N2 O2 118.68(19) . . ? C8 N2 Ru 116.27(16) . . ? O2 N2 Ru 122.18(15) . . ? C15 N3 O3 118.8(2) . . ? C15 N3 Ru 117.12(17) . . ? O3 N3 Ru 122.64(14) . . ? O2 B1 O3 110.3(2) . . ? O2 B1 O1 111.1(2) . . ? O3 B1 O1 110.4(2) . . ? O2 B1 C22 107.9(2) . . ? O3 B1 C22 108.7(2) . . ? O1 B1 C22 108.4(2) . . ? N1 C1 O4 122.2(2) . . ? N1 C1 C1 113.81(14) . 2_655 ? O4 C1 C1 123.82(13) . 2_655 ? C1 O4 C2 118.4(2) . . ? C3 C2 C7 122.1(3) . . ? C3 C2 O4 122.0(3) . . ? C7 C2 O4 115.9(3) . . ? C2 C3 C4 117.0(5) . . ? C5 C4 C3 121.3(6) . . ? C4 C5 C6 119.8(5) . . ? C7 C6 C5 120.2(5) . . ? C6 C7 C2 119.6(5) . . ? N2 C8 O5 123.5(2) . . ? N2 C8 C15 114.5(2) . 2_655 ? O5 C8 C15 122.0(2) . 2_655 ? C8 O5 C9 115.3(2) . . ? C14 C9 C10 122.0(3) . . ? C14 C9 O5 117.2(3) . . ? C10 C9 O5 120.8(3) . . ? C9 C10 C11 118.5(4) . . ? C12 C11 C10 117.9(5) . . ? C13 C12 C11 122.4(5) . . ? C14 C13 C12 119.6(4) . . ? C9 C14 C13 119.4(4) . . ? N3 C15 O6 127.5(2) . . ? N3 C15 C8 113.2(2) . 2_655 ? O6 C15 C8 119.0(2) . 2_655 ? C15 O6 C16 119.17(19) . . ? C17 C16 C21 121.6(3) . . ? C17 C16 O6 117.6(3) . . ? C21 C16 O6 120.7(3) . . ? C16 C17 C18 119.3(3) . . ? C19 C18 C17 120.3(4) . . ? C18 C19 C20 119.7(4) . . ? C19 C20 C21 120.2(4) . . ? C16 C21 C20 118.8(4) . . ? C23 C22 B1 114.7(2) . . ? C24 C23 C22 114.2(3) . . ? C25 C24 C23 113.5(6) . . ? _diffrn_measured_fraction_theta_max 0.362 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.362 _refine_diff_density_max 0.522 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.055 data_No4 _database_code_CSD 168670 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H18 B2 F2 N6 O6 Ru S6' _chemical_formula_weight 695.37 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.518(2) _cell_length_b 12.157(2) _cell_length_c 19.597(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.83(1) _cell_angle_gamma 90.00 _cell_volume 2504.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 12.1 _cell_measurement_theta_max 12.8 _exptl_crystal_description prism _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 1.183 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6619 _exptl_absorpt_correction_T_max 0.7484 _exptl_absorpt_process_details ? _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 filter _diffrn_measurement_device_type CAD4 _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 100 _diffrn_standards_decay_% .4 _diffrn_reflns_number 2927 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.43 _reflns_number_total 2927 _reflns_number_gt 2744 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2744 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0558 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.449 _refine_ls_shift/su_mean 0.269 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 0.033301(2) 0.175182(4) 0.165100(2) 0.02541(3) Uani 1 1 d . . . S1 S 0.023905(10) -0.19030(2) 0.117995(9) 0.05641(15) Uani 1 1 d . . . S2 S -0.024192(8) 0.23153(2) 0.392101(6) 0.04871(10) Uani 1 1 d . . . S3 S 0.428194(5) 0.282908(15) 0.108404(5) 0.05051(8) Uani 1 1 d . . . S4 S -0.178386(7) -0.058782(14) 0.021307(5) 0.04798(8) Uani 1 1 d . . . S5 S -0.215092(7) 0.383672(19) 0.299628(6) 0.04990(9) Uani 1 1 d . . . S6 S 0.207208(7) 0.435982(13) 0.032001(5) 0.04363(8) Uani 1 1 d . . . F1 F 0.323905(13) 0.00109(3) 0.287015(11) 0.04403(15) Uani 1 1 d . . . F2 F -0.258916(13) 0.34860(3) 0.044193(11) 0.04024(13) Uani 1 1 d . . . O1 O 0.180997(16) -0.02480(3) 0.197504(12) 0.03488(19) Uani 1 1 d . . . O2 O 0.134061(14) 0.09228(3) 0.296793(11) 0.03548(15) Uani 1 1 d . . . O3 O 0.298002(14) 0.14943(3) 0.215275(13) 0.03652(15) Uani 1 1 d . . . O4 O -0.19589(2) 0.17555(5) 0.075297(14) 0.0357(3) Uani 1 1 d . . . O5 O -0.172771(16) 0.33796(3) 0.152531(13) 0.03524(17) Uani 1 1 d . . . O6 O -0.042286(15) 0.32276(3) 0.051240(13) 0.0338(2) Uani 1 1 d . . . N1 N 0.086205(17) 0.01895(4) 0.156502(14) 0.02988(17) Uani 1 1 d . . . N2 N 0.039694(17) 0.15362(4) 0.265579(15) 0.0293(2) Uani 1 1 d . . . N3 N 0.217425(17) 0.20986(4) 0.173708(14) 0.0311(2) Uani 1 1 d . . . N4 N -0.10822(2) 0.10987(6) 0.10847(2) 0.0287(3) Uani 1 1 d . . . N5 N -0.087789(16) 0.28671(4) 0.196626(15) 0.02966(18) Uani 1 1 d . . . N6 N 0.059493(15) 0.27525(4) 0.086007(13) 0.02863(18) Uani 1 1 d . . . B1 B 0.23332(3) 0.05473(5) 0.24929(2) 0.0331(3) Uani 1 1 d . . . B2 B -0.16565(3) 0.29544(9) 0.08122(3) 0.0336(6) Uani 1 1 d . . . C1 C 0.01131(2) -0.04782(7) 0.12181(2) 0.0321(4) Uani 1 1 d . . . C2 C -0.09554(3) 0.00783(8) 0.08770(2) 0.0299(4) Uani 1 1 d . . . C3 C 0.267110(19) 0.27072(5) 0.125743(17) 0.0338(2) Uani 1 1 d . . . C4 C 0.17131(2) 0.31962(4) 0.08022(2) 0.0323(3) Uani 1 1 d . . . C5 C -0.02658(2) 0.22108(5) 0.303131(18) 0.0334(3) Uani 1 1 d . . . C6 C -0.10619(2) 0.29551(4) 0.26275(2) 0.0320(3) Uani 1 1 d . . . C7 C 0.18983(5) -0.21682(12) 0.11018(4) 0.0616(5) Uani 1 1 d . . . C8 C -0.00467(5) 0.09266(8) 0.42124(3) 0.0644(4) Uani 1 1 d . . . C9 C 0.50457(3) 0.30624(7) 0.19043(3) 0.0627(4) Uani 1 1 d . . . C10 C -0.33859(3) -0.00953(12) 0.02276(4) 0.0628(5) Uani 1 1 d . . . C11 C -0.18455(9) 0.51153(11) 0.25702(5) 0.0934(5) Uani 1 1 d . . . C12 C 0.13587(4) 0.40699(11) -0.05080(3) 0.0496(4) Uani 1 1 d . . . H71 H 0.1994(6) -0.2909(9) 0.0963(4) 0.103(3) Uiso 1 1 d . . . H72 H 0.2252(4) -0.2009(5) 0.1509(3) 0.0751(18) Uiso 1 1 d . . . H73 H 0.2257(5) -0.1790(7) 0.0761(3) 0.107(3) Uiso 1 1 d . . . H81 H -0.0696(4) 0.0482(5) 0.3958(2) 0.0723(16) Uiso 1 1 d . . . H82 H -0.0279(4) 0.1018(5) 0.4653(3) 0.0961(18) Uiso 1 1 d . . . H83 H 0.0692(4) 0.0668(5) 0.4077(3) 0.0963(19) Uiso 1 1 d . . . H91 H 0.4925(5) 0.2356(8) 0.2186(3) 0.116(3) Uiso 1 1 d . . . H92 H 0.4533(7) 0.3643(9) 0.2157(3) 0.174(3) Uiso 1 1 d . . . H93 H 0.5753(6) 0.3183(5) 0.1806(3) 0.120(2) Uiso 1 1 d . . . H101 H -0.3775(4) -0.0227(5) 0.0705(3) 0.0961(19) Uiso 1 1 d . . . H102 H -0.3851(5) -0.0539(5) -0.0056(3) 0.097(2) Uiso 1 1 d . . . H103 H -0.3430(5) 0.0611(9) 0.0192(4) 0.089(3) Uiso 1 1 d . . . H111 H -0.0941(6) 0.5268(6) 0.2617(3) 0.132(3) Uiso 1 1 d . . . H112 H -0.2133(4) 0.5597(9) 0.2803(3) 0.066(2) Uiso 1 1 d . . . H113 H -0.1982(7) 0.5127(7) 0.2058(4) 0.169(3) Uiso 1 1 d . . . H121 H 0.1640(5) 0.3386(8) -0.0652(3) 0.080(3) Uiso 1 1 d . . . H122 H 0.0398(4) 0.4094(5) -0.0521(2) 0.0772(14) Uiso 1 1 d . . . H123 H 0.1655(4) 0.4587(7) -0.0835(2) 0.0598(17) Uiso 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 0.02301(1) 0.02717(10) 0.02621(3) 0.00099(2) 0.00301(1) -0.00200(1) S1 0.05602(5) 0.0315(5) 0.08164(13) -0.01249(16) 0.00101(6) -0.00106(8) S2 0.05901(4) 0.0593(3) 0.02798(8) -0.00386(12) 0.00395(4) 0.01100(8) S3 0.02797(2) 0.0748(3) 0.04916(7) 0.00627(9) 0.00797(3) -0.00998(4) S4 0.05001(4) 0.0542(3) 0.03944(7) -0.01188(9) -0.00397(4) -0.01196(6) S5 0.04502(3) 0.0643(3) 0.04104(8) -0.00509(11) 0.01099(4) 0.01910(6) S6 0.04609(3) 0.0423(3) 0.04236(7) 0.00983(8) -0.00100(4) -0.01796(5) F1 0.03585(7) 0.0502(5) 0.04574(14) 0.00763(18) -0.00297(8) 0.01008(11) F2 0.03204(6) 0.0459(4) 0.04239(15) 0.00938(15) -0.00514(7) 0.00217(10) O1 0.03418(8) 0.0310(6) 0.03939(17) 0.0003(2) -0.00081(9) 0.00706(13) O2 0.03388(7) 0.0439(5) 0.02859(14) 0.00437(19) -0.00066(7) 0.00495(12) O3 0.02609(6) 0.0425(5) 0.04077(17) 0.00832(18) -0.00279(8) -0.00215(11) O4 0.02902(9) 0.0389(9) 0.0388(2) 0.0056(2) -0.00571(10) -0.00279(14) O5 0.03115(7) 0.0411(6) 0.03355(19) 0.00160(17) 0.00194(9) 0.00779(11) O6 0.03007(7) 0.0389(6) 0.03225(17) 0.00666(16) 0.00030(9) 0.00020(10) N1 0.02902(8) 0.0283(6) 0.03252(18) -0.0005(2) 0.00384(9) 0.00077(14) N2 0.02605(7) 0.0317(6) 0.0304(2) 0.0024(2) 0.00336(9) 0.00086(12) N3 0.02696(7) 0.0358(7) 0.0304(2) 0.0001(2) 0.00007(9) -0.00199(12) N4 0.02496(7) 0.0321(11) 0.0288(2) 0.0017(3) -0.00223(10) -0.00480(18) N5 0.02587(6) 0.0301(6) 0.0331(2) 0.0037(2) 0.00192(9) 0.00213(12) N6 0.02696(6) 0.0319(6) 0.02719(18) 0.0025(2) 0.00375(8) -0.00308(14) B1 0.02903(10) 0.0370(9) 0.0332(3) 0.0022(4) -0.00012(13) 0.00112(17) B2 0.02902(14) 0.037(2) 0.0349(3) 0.0045(4) 0.00272(14) -0.0020(2) C1 0.03502(10) 0.0296(14) 0.0321(3) -0.0037(4) 0.00763(13) -0.0018(2) C2 0.02901(10) 0.0332(14) 0.0278(3) -0.0003(4) 0.00469(12) -0.0078(2) C3 0.02704(8) 0.0384(7) 0.0361(2) -0.0019(3) 0.00428(10) -0.00577(17) C4 0.03205(10) 0.0325(9) 0.0326(2) -0.0036(2) 0.00517(12) -0.00414(14) C5 0.03316(9) 0.0339(9) 0.0334(2) -0.0034(3) 0.00595(11) -0.00125(18) C6 0.02484(7) 0.0382(9) 0.0332(3) -0.0029(3) 0.00330(11) -0.00013(13) C7 0.0690(2) 0.0563(17) 0.0593(4) -0.0102(6) 0.0006(3) 0.0258(4) C8 0.0714(2) 0.0793(13) 0.0438(4) 0.0187(5) 0.0218(2) 0.0237(4) C9 0.03619(13) 0.0853(14) 0.0660(4) -0.0032(4) -0.00687(19) -0.0146(2) C10 0.04620(18) 0.0588(17) 0.0820(5) 0.0025(6) -0.0190(2) -0.0160(3) C11 0.1438(6) 0.0590(15) 0.0793(7) -0.0028(7) 0.0361(5) 0.0429(7) C12 0.0620(2) 0.0488(14) 0.0379(3) 0.0063(5) 0.0028(2) -0.0116(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 N5 1.9729(4) . ? Ru N3 1.9839(4) . ? Ru N2 1.9855(3) . ? Ru N1 1.9878(5) . ? Ru N4 1.9930(4) . ? Ru N6 1.9964(4) . ? S1 C1 1.7389(8) . ? S1 C7 1.7861(6) . ? S2 C5 1.7476(4) . ? S2 C8 1.7920(9) . ? S3 C3 1.7449(4) . ? S3 C9 1.7963(6) . ? S4 C2 1.7423(6) . ? S4 C10 1.7893(7) . ? S5 C6 1.7424(5) . ? S5 C11 1.7982(14) . ? S6 C4 1.7491(5) . ? S6 C12 1.8006(6) . ? F1 B1 1.3545(5) . ? F2 B2 1.3642(7) . ? O1 N1 1.3680(4) . ? O1 B1 1.4939(6) . ? O2 N2 1.3699(4) . ? O2 B1 1.4924(5) . ? O3 N3 1.3702(4) . ? O3 B1 1.5039(6) . ? O4 N4 1.3683(7) . ? O4 B2 1.4956(10) . ? O5 N5 1.3728(4) . ? O5 B2 1.4941(6) . ? O6 N6 1.3774(4) . ? O6 B2 1.4791(5) . ? N1 C1 1.3067(7) . ? N2 C5 1.3164(6) . ? N3 C3 1.3174(6) . ? N4 C2 1.3137(10) . ? N5 C6 1.3207(5) . ? N6 C4 1.3022(4) . ? C1 C2 1.4559(7) . ? C3 C4 1.4516(5) . ? C5 C6 1.4503(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 N5 Ru N3 117.745(18) . . ? N5 Ru N2 77.403(15) . . ? N3 Ru N2 86.656(14) . . ? N5 Ru N1 150.277(13) . . ? N3 Ru N1 86.278(16) . . ? N2 Ru N1 87.549(15) . . ? N5 Ru N4 88.28(2) . . ? N3 Ru N4 147.319(15) . . ? N2 Ru N4 120.044(19) . . ? N1 Ru N4 77.19(2) . . ? N5 Ru N6 86.033(17) . . ? N3 Ru N6 77.174(14) . . ? N2 Ru N6 148.134(17) . . ? N1 Ru N6 118.066(16) . . ? N4 Ru N6 85.96(2) . . ? C1 S1 C7 105.04(5) . . ? C5 S2 C8 104.32(3) . . ? C3 S3 C9 104.38(2) . . ? C2 S4 C10 106.34(4) . . ? C6 S5 C11 102.10(4) . . ? C4 S6 C12 103.75(4) . . ? N1 O1 B1 113.15(4) . . ? N2 O2 B1 113.54(3) . . ? N3 O3 B1 113.20(2) . . ? N4 O4 B2 113.16(4) . . ? N5 O5 B2 112.37(4) . . ? N6 O6 B2 112.77(4) . . ? C1 N1 O1 118.69(5) . . ? C1 N1 Ru 118.16(4) . . ? O1 N1 Ru 121.49(3) . . ? C5 N2 O2 118.59(3) . . ? C5 N2 Ru 118.06(3) . . ? O2 N2 Ru 121.05(2) . . ? C3 N3 O3 118.26(2) . . ? C3 N3 Ru 117.84(2) . . ? O3 N3 Ru 121.35(3) . . ? C2 N4 O4 118.51(4) . . ? C2 N4 Ru 117.86(3) . . ? O4 N4 Ru 120.80(5) . . ? C6 N5 O5 117.91(3) . . ? C6 N5 Ru 118.63(3) . . ? O5 N5 Ru 121.92(2) . . ? C4 N6 O6 118.24(4) . . ? C4 N6 Ru 117.87(3) . . ? O6 N6 Ru 121.013(19) . . ? F1 B1 O2 107.50(3) . . ? F1 B1 O1 107.26(4) . . ? O2 B1 O1 111.83(3) . . ? F1 B1 O3 106.87(3) . . ? O2 B1 O3 112.19(4) . . ? O1 B1 O3 110.88(3) . . ? F2 B2 O6 107.90(5) . . ? F2 B2 O5 106.08(5) . . ? O6 B2 O5 111.39(4) . . ? F2 B2 O4 105.83(4) . . ? O6 B2 O4 112.03(5) . . ? O5 B2 O4 113.14(5) . . ? N1 C1 C2 113.20(7) . . ? N1 C1 S1 126.56(4) . . ? C2 C1 S1 120.12(5) . . ? N4 C2 C1 112.40(5) . . ? N4 C2 S4 128.10(5) . . ? C1 C2 S4 119.16(6) . . ? N3 C3 C4 112.65(2) . . ? N3 C3 S3 126.61(3) . . ? C4 C3 S3 120.32(3) . . ? N6 C4 C3 112.83(4) . . ? N6 C4 S6 126.38(3) . . ? C3 C4 S6 120.38(3) . . ? N2 C5 C6 112.98(3) . . ? N2 C5 S2 127.74(4) . . ? C6 C5 S2 119.25(4) . . ? N5 C6 C5 112.62(4) . . ? N5 C6 S5 125.15(3) . . ? C5 C6 S5 122.22(3) . . ? _diffrn_measured_fraction_theta_max 0.088 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full 0.088 _refine_diff_density_max 0.615 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.003