#------------------------------------------------------------------------------ #$Date: 2019-12-09 10:44:34 +0200 (Mon, 09 Dec 2019) $ #$Revision: 244951 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556465.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1556465 loop_ _publ_author_name 'Delgado-Martinez, P.' 'Elvira-Bravo, A.' 'Gonzalez-Prieto, R.' 'Priego, J.L.' 'Jimenez-Aparicio, R.' 'Torres, M.R.' _publ_section_title ; Synthesis of Ru2Br(mu-O2CC6H4-R)4 (R = o-Me, m-Me, p-Me) Using Microwave Activation: Structural and Magnetic Properties ; _journal_name_full Inorganics _journal_page_first 524 _journal_page_last 536 _journal_paper_doi 10.3390/inorganics2030524 _journal_volume 2 _journal_year 2014 _chemical_formula_sum 'C32 H28 Br O8 Ru2' _chemical_formula_weight 822.59 _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 98.071(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.0936(4) _cell_length_b 11.1271(4) _cell_length_c 21.8306(7) _cell_measurement_reflns_used 4459 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.3664 _cell_measurement_theta_min 3.3687 _cell_volume 3149.08(18) _computing_cell_refinement ; 'Mon Mar 03 15:59:24 2014' ; _computing_data_collection ; 'Mon Mar 03 15:59:24 2014' ; _computing_data_reduction ; 'Mon Mar 03 15:59:24 2014' ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10.3317 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Xcalibur, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 15156 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 3.37 _exptl_absorpt_coefficient_mu 2.277 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.97089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; 'Mon Mar 03 15:59:24 2014' ; _exptl_crystal_colour 'clear dark brown' _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1628 _exptl_crystal_size_max 0.3800 _exptl_crystal_size_mid 0.1600 _exptl_crystal_size_min 0.0700 _refine_diff_density_max 0.954 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.106 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 364 _refine_ls_number_reflns 6181 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.993 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0445 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+3.4578P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1015 _refine_ls_wR_factor_ref 0.1206 _reflns_number_gt 4452 _reflns_number_total 6181 _reflns_threshold_expression >2sigma(I) _cod_data_source_file cif-compound_2.cif _cod_data_source_block aeb11 _cod_original_cell_volume 3149.07(18) _cod_database_code 1556465 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' 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 Br1 Br 0.74330(4) 1.16755(5) 0.46780(3) 0.04728(18) Uani 1 1 d . . . C1 C 0.9032(4) 0.8020(5) 0.4611(2) 0.0359(12) Uani 1 1 d . . . C2 C 0.8483(5) 0.6903(5) 0.4422(3) 0.0463(14) Uani 1 1 d . . . C3 C 0.7448(5) 0.6922(5) 0.4170(3) 0.0473(14) Uani 1 1 d . . . H3 H 0.7101 0.7653 0.4125 0.057 Uiso 1 1 calc R . . C4 C 0.6932(6) 0.5889(7) 0.3987(4) 0.0811(17) Uani 1 1 d . . . C5 C 0.7441(6) 0.4820(6) 0.4070(4) 0.083(3) Uani 1 1 d . . . H5 H 0.7092 0.4112 0.3949 0.099 Uiso 1 1 calc R . . C6 C 0.8459(7) 0.4769(7) 0.4327(6) 0.130(5) Uani 1 1 d . . . H6 H 0.8790 0.4031 0.4393 0.155 Uiso 1 1 calc R . . C7 C 0.8992(6) 0.5832(6) 0.4488(5) 0.096(3) Uani 1 1 d . . . H7 H 0.9691 0.5812 0.4641 0.115 Uiso 1 1 calc R . . C8 C 0.5835(5) 0.5883(7) 0.3709(4) 0.0811(17) Uani 1 1 d . . . H8A H 0.5421 0.6215 0.3997 0.122 Uiso 1 1 calc R . . H8B H 0.5620 0.5072 0.3611 0.122 Uiso 1 1 calc R . . H8C H 0.5751 0.6357 0.3338 0.122 Uiso 1 1 calc R . . C9 C 1.0510(4) 1.0469(5) 0.3907(2) 0.0371(12) Uani 1 1 d . . . C10 C 1.0853(5) 1.0784(6) 0.3318(3) 0.0483(15) Uani 1 1 d . . . C11 C 1.0271(6) 1.1522(6) 0.2905(3) 0.068(2) Uani 1 1 d . . . H11 H 0.9624 1.1773 0.2983 0.082 Uiso 1 1 calc R . . C12 C 1.0637(9) 1.1899(10) 0.2369(4) 0.129(3) Uani 1 1 d . . . C13 C 1.1574(8) 1.1491(10) 0.2260(4) 0.141(5) Uani 1 1 d . . . H13 H 1.1812 1.1712 0.1894 0.169 Uiso 1 1 calc R . . C14 C 1.2181(7) 1.0766(9) 0.2669(4) 0.115(4) Uani 1 1 d . . . H14 H 1.2829 1.0527 0.2589 0.138 Uiso 1 1 calc R . . C15 C 1.1819(5) 1.0399(6) 0.3201(3) 0.066(2) Uani 1 1 d . . . H15 H 1.2216 0.9897 0.3480 0.079 Uiso 1 1 calc R . . C16 C 1.0000(8) 1.2723(9) 0.1916(4) 0.129(3) Uani 1 1 d . . . H16A H 0.9374 1.2323 0.1747 0.194 Uiso 1 1 calc R . . H16B H 1.0385 1.2928 0.1588 0.194 Uiso 1 1 calc R . . H16C H 0.9836 1.3441 0.2125 0.194 Uiso 1 1 calc R . . C17 C 0.4808(5) 0.9148(5) 0.3866(3) 0.0428(13) Uani 1 1 d . . . C18 C 0.4690(5) 0.8659(5) 0.3233(2) 0.0473(15) Uani 1 1 d . . . C19 C 0.3839(5) 0.7989(6) 0.3006(3) 0.0573(17) Uani 1 1 d . . . H19 H 0.3322 0.7865 0.3251 0.069 Uiso 1 1 calc R . . C20 C 0.3738(7) 0.7493(8) 0.2414(4) 0.0916(19) Uani 1 1 d . . . C21 C 0.4530(7) 0.7659(8) 0.2076(3) 0.084(2) Uani 1 1 d . . . H21 H 0.4476 0.7328 0.1681 0.101 Uiso 1 1 calc R . . C22 C 0.5391(7) 0.8288(8) 0.2294(3) 0.092(3) Uani 1 1 d . . . H22 H 0.5921 0.8370 0.2055 0.110 Uiso 1 1 calc R . . C23 C 0.5477(6) 0.8815(7) 0.2883(3) 0.073(2) Uani 1 1 d . . . H23 H 0.6058 0.9263 0.3035 0.088 Uiso 1 1 calc R . . C24 C 0.2796(6) 0.6783(8) 0.2167(4) 0.0916(19) Uani 1 1 d . . . H24A H 0.2792 0.6638 0.1733 0.137 Uiso 1 1 calc R . . H24B H 0.2189 0.7226 0.2228 0.137 Uiso 1 1 calc R . . H24C H 0.2803 0.6029 0.2382 0.137 Uiso 1 1 calc R . . C25 C 0.5990(4) 0.8051(6) 0.5406(3) 0.0434(14) Uani 1 1 d . . . C26 C 0.6519(5) 0.6917(6) 0.5617(3) 0.0521(16) Uani 1 1 d . . . C27 C 0.7517(6) 0.6866(7) 0.5844(4) 0.078(2) Uani 1 1 d . . . H27 H 0.7898 0.7574 0.5881 0.094 Uiso 1 1 calc R . . C28 C 0.8012(9) 0.5786(11) 0.6026(7) 0.149(4) Uani 1 1 d . . . C29 C 0.7478(9) 0.4725(10) 0.5936(6) 0.121(4) Uani 1 1 d . . . H29 H 0.7808 0.3999 0.6042 0.145 Uiso 1 1 calc R . . C30 C 0.6466(9) 0.4741(9) 0.5689(7) 0.141(5) Uani 1 1 d . . . H30 H 0.6105 0.4024 0.5614 0.169 Uiso 1 1 calc R . . C31 C 0.5966(7) 0.5845(8) 0.5549(5) 0.107(3) Uani 1 1 d . . . H31 H 0.5262 0.5859 0.5409 0.128 Uiso 1 1 calc R . . C32 C 0.9165(7) 0.5778(9) 0.6257(6) 0.149(4) Uani 1 1 d . . . H32A H 0.9379 0.4978 0.6379 0.224 Uiso 1 1 calc R . . H32B H 0.9309 0.6308 0.6606 0.224 Uiso 1 1 calc R . . H32C H 0.9535 0.6045 0.5933 0.224 Uiso 1 1 calc R . . O1 O 0.8545(3) 0.8996(3) 0.45586(16) 0.0395(9) Uani 1 1 d . . . O2 O 0.9991(3) 0.7951(3) 0.48246(17) 0.0403(9) Uani 1 1 d . . . O3 O 0.9645(3) 1.0859(3) 0.40250(15) 0.0381(9) Uani 1 1 d . . . O4 O 1.1097(3) 0.9812(3) 0.42779(16) 0.0403(9) Uani 1 1 d . . . O5 O 0.5597(3) 0.9757(3) 0.40644(16) 0.0453(10) Uani 1 1 d . . . O6 O 0.4088(3) 0.8934(3) 0.41947(16) 0.0429(9) Uani 1 1 d . . . O7 O 0.5016(3) 0.8071(3) 0.53731(18) 0.0454(9) Uani 1 1 d . . . O8 O 0.6513(3) 0.8918(3) 0.52608(17) 0.0433(9) Uani 1 1 d . . . Ru1 Ru 0.92511(3) 1.05291(4) 0.487187(18) 0.03032(13) Uani 1 1 d . . . Ru2 Ru 0.57700(3) 1.04327(4) 0.49336(2) 0.03527(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0341(3) 0.0435(3) 0.0649(4) 0.0142(3) 0.0096(3) 0.0016(3) C1 0.040(3) 0.029(3) 0.040(3) 0.004(2) 0.009(2) -0.003(3) C2 0.053(4) 0.036(3) 0.048(3) -0.002(3) 0.000(3) -0.010(3) C3 0.049(3) 0.036(3) 0.057(4) -0.002(3) 0.007(3) -0.005(3) C4 0.066(3) 0.061(3) 0.110(5) 0.001(3) -0.010(3) -0.012(3) C5 0.073(5) 0.043(4) 0.123(7) -0.005(4) -0.018(5) -0.014(4) C6 0.089(7) 0.036(4) 0.240(13) -0.007(6) -0.063(8) -0.003(4) C7 0.067(5) 0.039(4) 0.167(9) -0.013(5) -0.033(5) 0.000(4) C8 0.066(3) 0.061(3) 0.110(5) 0.001(3) -0.010(3) -0.012(3) C9 0.038(3) 0.038(3) 0.036(3) -0.004(3) 0.006(2) 0.002(3) C10 0.058(4) 0.052(4) 0.037(3) 0.009(3) 0.014(3) 0.009(3) C11 0.091(5) 0.073(5) 0.045(4) 0.017(4) 0.025(4) 0.034(4) C12 0.174(7) 0.152(6) 0.073(4) 0.066(4) 0.057(5) 0.092(6) C13 0.169(10) 0.182(11) 0.091(7) 0.079(7) 0.091(7) 0.098(9) C14 0.123(7) 0.155(9) 0.082(6) 0.057(6) 0.066(6) 0.073(7) C15 0.072(5) 0.079(5) 0.054(4) 0.022(4) 0.032(4) 0.023(4) C16 0.174(7) 0.152(6) 0.073(4) 0.066(4) 0.057(5) 0.092(6) C17 0.049(3) 0.042(3) 0.037(3) 0.001(3) 0.006(3) 0.007(3) C18 0.055(4) 0.053(4) 0.033(3) -0.005(3) 0.005(3) 0.011(3) C19 0.056(4) 0.067(4) 0.045(4) -0.012(3) -0.005(3) 0.011(4) C20 0.086(4) 0.116(5) 0.065(4) -0.033(3) -0.016(3) 0.010(4) C21 0.105(7) 0.099(6) 0.045(4) -0.021(4) 0.002(4) 0.015(6) C22 0.106(7) 0.124(8) 0.050(4) -0.013(5) 0.025(4) 0.008(6) C23 0.084(5) 0.086(5) 0.054(4) -0.019(4) 0.023(4) -0.003(5) C24 0.086(4) 0.116(5) 0.065(4) -0.033(3) -0.016(3) 0.010(4) C25 0.040(3) 0.050(4) 0.041(3) -0.002(3) 0.009(3) 0.009(3) C26 0.051(4) 0.051(4) 0.056(4) 0.013(3) 0.019(3) 0.011(3) C27 0.054(4) 0.071(5) 0.108(6) -0.005(5) 0.001(4) 0.011(4) C28 0.093(5) 0.110(6) 0.231(10) -0.019(6) -0.026(6) 0.051(5) C29 0.099(8) 0.096(8) 0.166(11) 0.024(7) 0.015(8) 0.028(7) C30 0.112(9) 0.065(6) 0.241(15) 0.040(8) 0.007(9) 0.007(6) C31 0.078(6) 0.066(5) 0.172(10) 0.042(6) 0.004(6) 0.003(5) C32 0.093(5) 0.110(6) 0.231(10) -0.019(6) -0.026(6) 0.051(5) O1 0.037(2) 0.036(2) 0.044(2) 0.0002(18) 0.0007(17) -0.0056(17) O2 0.041(2) 0.032(2) 0.047(2) -0.0026(17) 0.0035(17) -0.0022(17) O3 0.043(2) 0.041(2) 0.0309(19) 0.0079(17) 0.0053(16) 0.0025(18) O4 0.040(2) 0.048(2) 0.035(2) 0.0069(18) 0.0113(17) 0.0068(19) O5 0.048(2) 0.053(2) 0.036(2) -0.0004(18) 0.0086(18) -0.007(2) O6 0.040(2) 0.051(2) 0.037(2) -0.0067(19) 0.0053(17) -0.0065(19) O7 0.040(2) 0.044(2) 0.054(2) 0.0093(19) 0.0132(18) -0.0001(18) O8 0.035(2) 0.045(2) 0.051(2) 0.002(2) 0.0067(18) 0.0024(18) Ru1 0.0300(2) 0.0308(2) 0.0305(2) 0.00165(18) 0.00559(17) -0.00126(18) Ru2 0.0317(2) 0.0401(3) 0.0347(2) 0.0009(2) 0.00701(18) -0.0018(2) 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' Br Br -0.2901 2.4595 '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' 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 Ru1 Br1 Ru2 116.56(2) . . O1 C1 O2 123.0(5) . . O1 C1 C2 119.1(5) . . O2 C1 C2 117.9(5) . . C7 C2 C3 119.4(6) . . C7 C2 C1 120.0(5) . . C3 C2 C1 120.7(5) . . C4 C3 C2 121.2(6) . . C3 C4 C5 118.9(7) . . C3 C4 C8 122.5(7) . . C5 C4 C8 118.6(7) . . C6 C5 C4 121.3(7) . . C5 C6 C7 119.4(7) . . C2 C7 C6 119.7(7) . . O4 C9 O3 122.9(5) . . O4 C9 C10 117.8(5) . . O3 C9 C10 119.2(5) . . C11 C10 C15 120.0(6) . . C11 C10 C9 120.7(5) . . C15 C10 C9 119.1(5) . . C10 C11 C12 120.6(7) . . C11 C12 C13 118.3(8) . . C11 C12 C16 120.6(8) . . C13 C12 C16 121.1(8) . . C14 C13 C12 122.4(7) . . C13 C14 C15 119.2(7) . . C14 C15 C10 119.5(7) . . O5 C17 O6 122.6(5) . . O5 C17 C18 119.5(5) . . O6 C17 C18 117.9(5) . . C19 C18 C23 120.1(6) . . C19 C18 C17 120.7(5) . . C23 C18 C17 119.1(6) . . C18 C19 C20 121.0(7) . . C21 C20 C19 117.8(8) . . C21 C20 C24 121.6(7) . . C19 C20 C24 120.6(8) . . C22 C21 C20 122.4(7) . . C21 C22 C23 119.6(8) . . C18 C23 C22 119.0(7) . . O8 C25 O7 123.7(5) . . O8 C25 C26 119.2(5) . . O7 C25 C26 117.2(6) . . C27 C26 C31 118.1(7) . . C27 C26 C25 122.9(6) . . C31 C26 C25 118.9(6) . . C26 C27 C28 122.3(9) . . C29 C28 C27 119.5(9) . . C29 C28 C32 120.3(10) . . C27 C28 C32 119.8(11) . . C30 C29 C28 119.6(10) . . C29 C30 C31 119.8(10) . . C26 C31 C30 120.4(8) . . C1 O1 Ru1 119.9(3) . . C1 O2 Ru1 118.7(3) . 3_776 C9 O3 Ru1 118.2(3) . . C9 O4 Ru1 120.3(3) . 3_776 C17 O5 Ru2 120.0(3) . . C17 O6 Ru2 119.0(3) . 3_676 C25 O7 Ru2 119.7(4) . 3_676 C25 O8 Ru2 118.6(3) . . O4 Ru1 O1 90.04(15) 3_776 . O4 Ru1 O3 178.31(14) 3_776 . O1 Ru1 O3 90.41(14) . . O4 Ru1 O2 91.14(15) 3_776 3_776 O1 Ru1 O2 177.87(14) . 3_776 O3 Ru1 O2 88.36(14) . 3_776 O4 Ru1 Ru1 88.54(10) 3_776 3_776 O1 Ru1 Ru1 89.08(10) . 3_776 O3 Ru1 Ru1 89.84(10) . 3_776 O2 Ru1 Ru1 89.19(10) 3_776 3_776 O4 Ru1 Br1 85.66(10) 3_776 . O1 Ru1 Br1 89.67(10) . . O3 Ru1 Br1 95.97(10) . . O2 Ru1 Br1 92.18(10) 3_776 . Ru1 Ru1 Br1 174.07(3) 3_776 . O6 Ru2 O7 90.00(16) 3_676 3_676 O6 Ru2 O5 178.23(15) 3_676 . O7 Ru2 O5 90.60(16) 3_676 . O6 Ru2 O8 88.96(15) 3_676 . O7 Ru2 O8 177.77(14) 3_676 . O5 Ru2 O8 90.37(15) . . O6 Ru2 Ru2 89.64(10) 3_676 3_676 O7 Ru2 Ru2 88.40(10) 3_676 3_676 O5 Ru2 Ru2 88.72(11) . 3_676 O8 Ru2 Ru2 89.62(11) . 3_676 O6 Ru2 Br1 92.63(10) 3_676 . O7 Ru2 Br1 84.12(10) 3_676 . O5 Ru2 Br1 89.08(11) . . O8 Ru2 Br1 97.90(11) . . Ru2 Ru2 Br1 172.18(3) 3_676 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Br1 Ru1 2.6815(7) . Br1 Ru2 2.7030(7) . C1 O1 1.256(6) . C1 O2 1.279(6) . C1 C2 1.465(7) . C2 C7 1.362(9) . C2 C3 1.390(8) . C3 C4 1.364(9) . C4 C5 1.363(10) . C4 C8 1.479(9) . C5 C6 1.374(10) . C6 C7 1.394(10) . C9 O4 1.267(6) . C9 O3 1.273(6) . C9 C10 1.463(8) . C10 C11 1.369(8) . C10 C15 1.392(8) . C11 C12 1.390(10) . C12 C13 1.360(12) . C12 C16 1.511(11) . C13 C14 1.372(11) . C14 C15 1.376(9) . C17 O5 1.260(7) . C17 O6 1.284(6) . C17 C18 1.474(8) . C18 C19 1.374(8) . C18 C23 1.377(8) . C19 C20 1.393(9) . C20 C21 1.368(11) . C20 C24 1.501(11) . C21 C22 1.355(11) . C22 C23 1.403(10) . C25 O8 1.250(7) . C25 O7 1.268(6) . C25 C26 1.481(8) . C26 C27 1.332(9) . C26 C31 1.393(10) . C27 C28 1.397(12) . C28 C29 1.371(14) . C28 C32 1.524(13) . C29 C30 1.359(13) . C30 C31 1.404(12) . O1 Ru1 2.013(3) . O2 Ru1 2.025(3) 3_776 O3 Ru1 2.021(3) . O4 Ru1 2.009(3) 3_776 O5 Ru2 2.024(4) . O6 Ru2 2.013(3) 3_676 O7 Ru2 2.021(4) 3_676 O8 Ru2 2.026(4) . Ru1 O4 2.008(3) 3_776 Ru1 O2 2.025(4) 3_776 Ru1 Ru1 2.2885(8) 3_776 Ru2 O6 2.013(3) 3_676 Ru2 O7 2.021(4) 3_676 Ru2 Ru2 2.2893(8) 3_676 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 O1 C1 C2 C7 -178.5(7) . . . . O2 C1 C2 C7 1.2(9) . . . . O1 C1 C2 C3 2.1(8) . . . . O2 C1 C2 C3 -178.2(5) . . . . C7 C2 C3 C4 0.0(11) . . . . C1 C2 C3 C4 179.4(6) . . . . C2 C3 C4 C5 1.6(12) . . . . C2 C3 C4 C8 -179.1(7) . . . . C3 C4 C5 C6 -0.5(15) . . . . C8 C4 C5 C6 -179.9(9) . . . . C4 C5 C6 C7 -2.1(17) . . . . C3 C2 C7 C6 -2.7(13) . . . . C1 C2 C7 C6 178.0(9) . . . . C5 C6 C7 C2 3.7(17) . . . . O4 C9 C10 C11 -177.9(6) . . . . O3 C9 C10 C11 2.1(9) . . . . O4 C9 C10 C15 -2.8(9) . . . . O3 C9 C10 C15 177.3(6) . . . . C15 C10 C11 C12 -0.4(13) . . . . C9 C10 C11 C12 174.7(8) . . . . C10 C11 C12 C13 1.7(17) . . . . C10 C11 C12 C16 -179.4(9) . . . . C11 C12 C13 C14 -3(2) . . . . C16 C12 C13 C14 178.4(11) . . . . C12 C13 C14 C15 2(2) . . . . C13 C14 C15 C10 -1.0(15) . . . . C11 C10 C15 C14 0.1(12) . . . . C9 C10 C15 C14 -175.1(8) . . . . O5 C17 C18 C19 179.8(5) . . . . O6 C17 C18 C19 -0.5(9) . . . . O5 C17 C18 C23 4.0(9) . . . . O6 C17 C18 C23 -176.2(6) . . . . C23 C18 C19 C20 -2.3(10) . . . . C17 C18 C19 C20 -178.0(6) . . . . C18 C19 C20 C21 2.3(12) . . . . C18 C19 C20 C24 -178.8(7) . . . . C19 C20 C21 C22 -0.5(14) . . . . C24 C20 C21 C22 -179.3(8) . . . . C20 C21 C22 C23 -1.3(14) . . . . C19 C18 C23 C22 0.4(11) . . . . C17 C18 C23 C22 176.2(7) . . . . C21 C22 C23 C18 1.3(13) . . . . O8 C25 C26 C27 21.4(9) . . . . O7 C25 C26 C27 -159.8(6) . . . . O8 C25 C26 C31 -155.2(7) . . . . O7 C25 C26 C31 23.6(9) . . . . C31 C26 C27 C28 -1.7(14) . . . . C25 C26 C27 C28 -178.3(9) . . . . C26 C27 C28 C29 4.3(19) . . . . C26 C27 C28 C32 177.5(10) . . . . C27 C28 C29 C30 -2(2) . . . . C32 C28 C29 C30 -175.5(12) . . . . C28 C29 C30 C31 -2(2) . . . . C27 C26 C31 C30 -2.8(14) . . . . C25 C26 C31 C30 174.0(9) . . . . C29 C30 C31 C26 4.7(18) . . . . O2 C1 O1 Ru1 -4.2(7) . . . . C2 C1 O1 Ru1 175.5(4) . . . . O1 C1 O2 Ru1 2.7(7) . . . 3_776 C2 C1 O2 Ru1 -177.0(4) . . . 3_776 O4 C9 O3 Ru1 5.3(7) . . . . C10 C9 O3 Ru1 -174.7(4) . . . . O3 C9 O4 Ru1 -6.0(7) . . . 3_776 C10 C9 O4 Ru1 174.1(4) . . . 3_776 O6 C17 O5 Ru2 0.3(7) . . . . C18 C17 O5 Ru2 -179.9(4) . . . . O5 C17 O6 Ru2 -1.1(7) . . . 3_676 C18 C17 O6 Ru2 179.2(4) . . . 3_676 O8 C25 O7 Ru2 0.4(7) . . . 3_676 C26 C25 O7 Ru2 -178.3(4) . . . 3_676 O7 C25 O8 Ru2 -1.6(7) . . . . C26 C25 O8 Ru2 177.1(4) . . . . C1 O1 Ru1 O4 -85.4(4) . . . 3_776 C1 O1 Ru1 O3 93.0(4) . . . . C1 O1 Ru1 O2 38(4) . . . 3_776 C1 O1 Ru1 Ru1 3.1(4) . . . 3_776 C1 O1 Ru1 Br1 -171.1(4) . . . . C9 O3 Ru1 O4 14(5) . . . 3_776 C9 O3 Ru1 O1 -91.2(4) . . . . C9 O3 Ru1 O2 87.1(4) . . . 3_776 C9 O3 Ru1 Ru1 -2.1(4) . . . 3_776 C9 O3 Ru1 Br1 179.1(4) . . . . Ru2 Br1 Ru1 O4 -52.13(11) . . . 3_776 Ru2 Br1 Ru1 O1 37.93(11) . . . . Ru2 Br1 Ru1 O3 128.31(11) . . . . Ru2 Br1 Ru1 O2 -143.12(10) . . . 3_776 Ru2 Br1 Ru1 Ru1 -39.9(3) . . . 3_776 C17 O5 Ru2 O6 22(5) . . . 3_676 C17 O5 Ru2 O7 -87.9(4) . . . 3_676 C17 O5 Ru2 O8 90.0(4) . . . . C17 O5 Ru2 Ru2 0.4(4) . . . 3_676 C17 O5 Ru2 Br1 -172.1(4) . . . . C25 O8 Ru2 O6 91.3(4) . . . 3_676 C25 O8 Ru2 O7 29(4) . . . 3_676 C25 O8 Ru2 O5 -87.0(4) . . . . C25 O8 Ru2 Ru2 1.7(4) . . . 3_676 C25 O8 Ru2 Br1 -176.1(4) . . . . Ru1 Br1 Ru2 O6 92.22(11) . . . 3_676 Ru1 Br1 Ru2 O7 -178.04(11) . . . 3_676 Ru1 Br1 Ru2 O5 -87.34(11) . . . . Ru1 Br1 Ru2 O8 2.91(11) . . . . Ru1 Br1 Ru2 Ru2 -161.0(2) . . . 3_676