# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2236 #Manuscript No. data_global _publ_section_title ; Novel coordination modes of partially hydrogenated diyne ligands on metal carbonyl clusters ; _publ_contact_author 'Dr. P. R. Raithby' _publ_contact_author_email 'prr1@cam.ac.uk' _publ_requested_journal 'J.Chem.Soc.,Dalton Trans.' loop_ _publ_author_name 'Clarke,L.P.' 'Davies,J.E.' 'Raithby,P.R.' 'Shields,G.P.' _journal_name_full '?' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '?' data_lpc107b _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H8 O12 Ru4' _chemical_formula_weight 820.52 _chemical_melting_point ? _chemical_compound_source ? 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.020(4) _cell_length_b 21.034(7) _cell_length_c 10.018(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2322.1(30) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 30 _cell_measurement_theta_max 40 _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.347 _exptl_crystal_density_method ? _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 2.612 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 0.997 _exptl_special_details ; Half-sphere of data measured; crystal weakly diffracting, collected as triclinic. ; _diffrn_ambient_temperature 150(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 'Rigaku AFC7r' _diffrn_measurement_method 'Omega Scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 500 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.41 _diffrn_reflns_number 4093 _diffrn_reflns_av_R_equivalents 0.1176 _diffrn_reflns_av_sigmaI/netI 0.1511 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 2 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 22.58 _reflns_number_total 3050 _reflns_number_observed 2189 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0290P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(16) _refine_ls_number_reflns 3050 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_obs 0.0631 _refine_ls_wR_factor_all 0.1285 _refine_ls_wR_factor_obs 0.1122 _refine_ls_goodness_of_fit_all 1.010 _refine_ls_goodness_of_fit_obs 1.054 _refine_ls_restrained_S_all 1.010 _refine_ls_restrained_S_obs 1.054 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.0848(2) 0.95487(8) 0.5645(2) 0.0166(4) Uani 1 d . . Ru2 Ru 0.0763(2) 0.89214(7) 0.8066(2) 0.0147(4) Uani 1 d . . Ru3 Ru -0.1167(2) 0.79893(8) 0.8247(2) 0.0152(4) Uani 1 d . . Ru4 Ru 0.0067(2) 0.82374(8) 0.5897(2) 0.0135(4) Uani 1 d . . O1 O 0.1410(14) 1.0971(6) 0.5854(16) 0.032(4) Uani 1 d . . O2 O 0.3080(14) 0.9288(7) 0.3840(15) 0.031(5) Uani 1 d . . O3 O -0.0859(14) 0.9723(8) 0.3371(15) 0.040(4) Uani 1 d . . O4 O 0.3277(13) 0.9461(7) 0.7580(15) 0.031(4) Uani 1 d . . O5 O 0.0534(17) 0.9516(9) 1.0818(18) 0.063(6) Uani 1 d . . O6 O 0.2297(15) 0.7788(8) 0.8861(15) 0.036(5) Uani 1 d . . O7 O -0.2541(14) 0.8726(8) 1.0318(17) 0.044(5) Uani 1 d . . O8 O 0.0124(13) 0.7148(7) 1.0313(15) 0.033(4) Uani 1 d . . O9 O -0.3148(14) 0.7011(7) 0.7831(13) 0.029(4) Uani 1 d . . O10 O 0.0105(15) 0.6818(7) 0.6526(13) 0.033(4) Uani 1 d . . O11 O 0.2754(12) 0.8031(7) 0.5364(15) 0.025(4) Uani 1 d . . O12 O -0.0880(14) 0.8049(8) 0.3055(14) 0.038(4) Uani 1 d . . C1 C 0.1213(20) 1.0430(11) 0.5809(23) 0.031(6) Uiso 1 d . . C2 C 0.2264(20) 0.9365(10) 0.4514(22) 0.021(6) Uiso 1 d . . C3 C -0.0208(22) 0.9662(10) 0.4195(25) 0.031(6) Uiso 1 d . . C4 C 0.2292(21) 0.9323(10) 0.7521(21) 0.019(5) Uiso 1 d . . C5 C 0.0622(23) 0.9286(12) 0.9794(26) 0.037(7) Uiso 1 d . . C6 C 0.1676(18) 0.8190(10) 0.8612(19) 0.013(5) Uiso 1 d . . C7 C -0.1993(20) 0.8432(10) 0.9585(23) 0.022(6) Uiso 1 d . . C8 C -0.0335(17) 0.7457(9) 0.9566(21) 0.014(5) Uiso 1 d . . C9 C -0.2416(18) 0.7389(9) 0.7969(21) 0.014(5) Uiso 1 d . . C10 C -0.0058(22) 0.7375(11) 0.6460(21) 0.025(6) Uiso 1 d . . C11 C 0.1775(21) 0.8135(11) 0.5545(23) 0.024(6) Uiso 1 d . . C12 C -0.0554(17) 0.8128(9) 0.4130(22) 0.019(5) Uiso 1 d . . C13 C -0.1097(19) 1.0181(9) 0.7751(19) 0.019(5) Uiso 1 d . . H13A H -0.0538(19) 1.0543(9) 0.7790(19) 0.029 Uiso 1 calc R . H13B H -0.1349(19) 1.0066(9) 0.8657(19) 0.029 Uiso 1 calc R . H13C H -0.1812(19) 1.0297(9) 0.7223(19) 0.029 Uiso 1 calc R . C14 C -0.0469(17) 0.9624(9) 0.7109(20) 0.014(5) Uiso 1 d . . C15 C -0.1018(16) 0.9031(8) 0.6903(19) 0.012(4) Uiso 1 d . . C16 C -0.1697(18) 0.8556(10) 0.6657(22) 0.017(5) Uiso 1 d . . C17 C -0.2927(16) 0.8570(9) 0.5848(20) 0.014(5) Uiso 1 d . . H17A H -0.2814(16) 0.8830(9) 0.5033(20) 0.017 Uiso 1 calc R . H17B H -0.3130(16) 0.8132(9) 0.5563(20) 0.017 Uiso 1 calc R . C18 C -0.3957(20) 0.8832(10) 0.6627(22) 0.035(6) Uiso 1 d . . H18A H -0.4692(20) 0.8829(10) 0.6076(22) 0.052 Uiso 1 calc R . H18B H -0.3772(20) 0.9270(10) 0.6895(22) 0.052 Uiso 1 calc R . H18C H -0.4088(20) 0.8571(10) 0.7425(22) 0.052 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 Ru1 0.0162(10) 0.0156(9) 0.0180(11) 0.0014(8) 0.0002(9) -0.0014(9) Ru2 0.0132(9) 0.0156(9) 0.0152(9) -0.0007(9) 0.0009(10) -0.0005(8) Ru3 0.0154(10) 0.0152(9) 0.0152(10) -0.0005(9) 0.0019(9) -0.0018(8) Ru4 0.0115(9) 0.0142(9) 0.0147(10) -0.0002(8) 0.0013(9) -0.0009(8) O1 0.046(11) 0.010(8) 0.039(10) -0.003(8) -0.007(9) -0.008(8) O2 0.028(10) 0.019(9) 0.046(11) 0.022(8) 0.032(9) 0.008(8) O3 0.021(9) 0.075(12) 0.024(9) 0.018(9) -0.013(9) -0.001(10) O4 0.014(9) 0.033(10) 0.045(11) 0.005(8) -0.005(8) -0.016(8) O5 0.076(15) 0.085(15) 0.027(11) -0.022(11) 0.024(11) -0.022(12) O6 0.042(11) 0.039(11) 0.027(10) 0.007(8) 0.001(9) -0.002(9) O7 0.033(11) 0.052(12) 0.048(12) -0.015(10) 0.014(9) 0.003(10) O8 0.007(8) 0.047(11) 0.043(11) 0.022(9) -0.008(8) -0.009(8) O9 0.034(9) 0.040(10) 0.012(9) -0.010(8) -0.008(8) -0.005(9) O10 0.036(9) 0.035(9) 0.027(9) 0.003(8) 0.014(8) 0.011(9) O11 0.019(9) 0.018(8) 0.038(10) 0.004(8) 0.002(8) -0.006(7) O12 0.031(9) 0.071(11) 0.012(8) -0.008(9) 0.002(9) -0.005(10) _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 Ru1 C3 1.88(3) . ? Ru1 C1 1.90(2) . ? Ru1 C2 1.97(2) . ? Ru1 C14 2.07(2) . ? Ru1 C4 2.51(2) . ? Ru1 C15 2.65(2) . ? Ru1 Ru2 2.763(3) . ? Ru1 Ru4 2.900(2) . ? Ru2 C5 1.90(3) . ? Ru2 C6 1.92(2) . ? Ru2 C4 1.96(2) . ? Ru2 C14 2.22(2) . ? Ru2 C15 2.29(2) . ? Ru2 Ru4 2.717(3) . ? Ru2 Ru3 2.898(2) . ? Ru3 C7 1.87(2) . ? Ru3 C9 1.89(2) . ? Ru3 C8 1.96(2) . ? Ru3 C16 2.07(2) . ? Ru3 C10 2.52(2) . ? Ru3 C15 2.58(2) . ? Ru3 Ru4 2.768(3) . ? Ru4 C10 1.91(2) . ? Ru4 C12 1.91(2) . ? Ru4 C11 1.93(2) . ? Ru4 C16 2.19(2) . ? Ru4 C15 2.29(2) . ? O1 C1 1.16(2) . ? O2 C2 1.14(2) . ? O3 C3 1.10(3) . ? O4 C4 1.13(2) . ? O5 C5 1.14(3) . ? O6 C6 1.12(2) . ? O7 C7 1.13(2) . ? O8 C8 1.11(2) . ? O9 C9 1.14(2) . ? O10 C10 1.19(2) . ? O11 C11 1.12(2) . ? O12 C12 1.15(2) . ? C13 C14 1.51(2) . ? C14 C15 1.40(3) . ? C15 C16 1.27(3) . ? C16 C17 1.58(3) . ? C17 C18 1.48(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 C3 Ru1 C1 94.2(10) . . ? C3 Ru1 C2 94.1(9) . . ? C1 Ru1 C2 94.3(9) . . ? C3 Ru1 C14 96.0(9) . . ? C1 Ru1 C14 90.7(9) . . ? C2 Ru1 C14 168.4(8) . . ? C3 Ru1 C4 176.1(8) . . ? C1 Ru1 C4 89.2(8) . . ? C2 Ru1 C4 83.8(7) . . ? C14 Ru1 C4 85.9(7) . . ? C3 Ru1 C15 86.5(8) . . ? C1 Ru1 C15 121.6(8) . . ? C2 Ru1 C15 144.1(7) . . ? C14 Ru1 C15 31.7(7) . . ? C4 Ru1 C15 93.3(7) . . ? C3 Ru1 Ru2 136.0(7) . . ? C1 Ru1 Ru2 113.3(7) . . ? C2 Ru1 Ru2 116.0(6) . . ? C14 Ru1 Ru2 52.4(5) . . ? C4 Ru1 Ru2 43.4(5) . . ? C15 Ru1 Ru2 50.1(4) . . ? C3 Ru1 Ru4 90.3(7) . . ? C1 Ru1 Ru4 168.8(7) . . ? C2 Ru1 Ru4 95.6(6) . . ? C14 Ru1 Ru4 78.6(5) . . ? C4 Ru1 Ru4 86.8(5) . . ? C15 Ru1 Ru4 48.4(4) . . ? Ru2 Ru1 Ru4 57.27(6) . . ? C5 Ru2 C6 96.2(9) . . ? C5 Ru2 C4 98.6(10) . . ? C6 Ru2 C4 88.6(9) . . ? C5 Ru2 C14 94.2(9) . . ? C6 Ru2 C14 167.5(8) . . ? C4 Ru2 C14 96.8(8) . . ? C5 Ru2 C15 110.6(9) . . ? C6 Ru2 C15 132.4(7) . . ? C4 Ru2 C15 123.4(8) . . ? C14 Ru2 C15 36.1(6) . . ? C5 Ru2 Ru4 156.9(8) . . ? C6 Ru2 Ru4 87.2(6) . . ? C4 Ru2 Ru4 104.4(6) . . ? C14 Ru2 Ru4 80.5(5) . . ? C15 Ru2 Ru4 53.5(5) . . ? C5 Ru2 Ru1 127.6(7) . . ? C6 Ru2 Ru1 128.0(6) . . ? C4 Ru2 Ru1 61.4(6) . . ? C14 Ru2 Ru1 47.6(5) . . ? C15 Ru2 Ru1 62.3(5) . . ? Ru4 Ru2 Ru1 63.91(9) . . ? C5 Ru2 Ru3 99.0(8) . . ? C6 Ru2 Ru3 79.9(6) . . ? C4 Ru2 Ru3 159.9(6) . . ? C14 Ru2 Ru3 91.6(5) . . ? C15 Ru2 Ru3 58.1(4) . . ? Ru4 Ru2 Ru3 58.97(7) . . ? Ru1 Ru2 Ru3 113.76(8) . . ? C7 Ru3 C9 94.8(9) . . ? C7 Ru3 C8 91.7(9) . . ? C9 Ru3 C8 93.3(8) . . ? C7 Ru3 C16 97.3(8) . . ? C9 Ru3 C16 93.8(8) . . ? C8 Ru3 C16 168.1(8) . . ? C7 Ru3 C10 179.1(8) . . ? C9 Ru3 C10 84.6(8) . . ? C8 Ru3 C10 87.6(7) . . ? C16 Ru3 C10 83.5(8) . . ? C7 Ru3 C15 89.0(8) . . ? C9 Ru3 C15 122.5(8) . . ? C8 Ru3 C15 144.0(7) . . ? C16 Ru3 C15 29.3(7) . . ? C10 Ru3 C15 92.0(6) . . ? C7 Ru3 Ru4 139.0(6) . . ? C9 Ru3 Ru4 111.0(6) . . ? C8 Ru3 Ru4 116.8(6) . . ? C16 Ru3 Ru4 51.5(6) . . ? C10 Ru3 Ru4 41.9(5) . . ? C15 Ru3 Ru4 50.5(4) . . ? C7 Ru3 Ru2 93.7(7) . . ? C9 Ru3 Ru2 167.9(6) . . ? C8 Ru3 Ru2 94.9(6) . . ? C16 Ru3 Ru2 76.7(6) . . ? C10 Ru3 Ru2 87.0(5) . . ? C15 Ru3 Ru2 49.1(4) . . ? Ru4 Ru3 Ru2 57.24(6) . . ? C10 Ru4 C12 97.7(8) . . ? C10 Ru4 C11 91.0(10) . . ? C12 Ru4 C11 99.6(9) . . ? C10 Ru4 C16 97.2(9) . . ? C12 Ru4 C16 92.3(8) . . ? C11 Ru4 C16 164.5(9) . . ? C10 Ru4 C15 121.8(8) . . ? C12 Ru4 C15 108.0(7) . . ? C11 Ru4 C15 132.3(8) . . ? C16 Ru4 C15 32.9(7) . . ? C10 Ru4 Ru2 106.7(6) . . ? C12 Ru4 Ru2 154.9(6) . . ? C11 Ru4 Ru2 86.0(7) . . ? C16 Ru4 Ru2 79.1(6) . . ? C15 Ru4 Ru2 53.8(5) . . ? C10 Ru4 Ru3 62.2(7) . . ? C12 Ru4 Ru3 126.1(6) . . ? C11 Ru4 Ru3 127.9(7) . . ? C16 Ru4 Ru3 47.7(6) . . ? C15 Ru4 Ru3 60.4(5) . . ? Ru2 Ru4 Ru3 63.79(9) . . ? C10 Ru4 Ru1 162.3(7) . . ? C12 Ru4 Ru1 98.1(6) . . ? C11 Ru4 Ru1 78.5(7) . . ? C16 Ru4 Ru1 90.1(5) . . ? C15 Ru4 Ru1 60.0(5) . . ? Ru2 Ru4 Ru1 58.82(7) . . ? Ru3 Ru4 Ru1 113.52(7) . . ? O1 C1 Ru1 176.9(21) . . ? O2 C2 Ru1 176.7(19) . . ? O3 C3 Ru1 177.6(21) . . ? O4 C4 Ru2 157.6(19) . . ? O4 C4 Ru1 127.0(17) . . ? Ru2 C4 Ru1 75.2(7) . . ? O5 C5 Ru2 178.7(23) . . ? O6 C6 Ru2 173.3(18) . . ? O7 C7 Ru3 174.5(20) . . ? O8 C8 Ru3 179.0(18) . . ? O9 C9 Ru3 177.5(18) . . ? O10 C10 Ru4 161.0(19) . . ? O10 C10 Ru3 122.6(16) . . ? Ru4 C10 Ru3 75.9(7) . . ? O11 C11 Ru4 175.0(20) . . ? O12 C12 Ru4 177.0(18) . . ? C15 C14 C13 123.9(17) . . ? C15 C14 Ru1 97.5(13) . . ? C13 C14 Ru1 133.2(14) . . ? C15 C14 Ru2 74.7(11) . . ? C13 C14 Ru2 127.9(14) . . ? Ru1 C14 Ru2 80.0(6) . . ? C16 C15 C14 168.8(20) . . ? C16 C15 Ru4 69.5(12) . . ? C14 C15 Ru4 119.3(13) . . ? C16 C15 Ru2 121.5(14) . . ? C14 C15 Ru2 69.2(11) . . ? Ru4 C15 Ru2 72.7(5) . . ? C16 C15 Ru3 52.9(12) . . ? C14 C15 Ru3 135.0(14) . . ? Ru4 C15 Ru3 69.1(5) . . ? Ru2 C15 Ru3 72.8(5) . . ? C16 C15 Ru1 133.5(15) . . ? C14 C15 Ru1 50.9(10) . . ? Ru4 C15 Ru1 71.6(5) . . ? Ru2 C15 Ru1 67.6(5) . . ? Ru3 C15 Ru1 130.4(7) . . ? C15 C16 C17 126.2(19) . . ? C15 C16 Ru3 97.9(15) . . ? C17 C16 Ru3 130.3(14) . . ? C15 C16 Ru4 77.6(12) . . ? C17 C16 Ru4 126.0(14) . . ? Ru3 C16 Ru4 80.8(7) . . ? C18 C17 C16 113.2(17) . . ? _refine_diff_density_max 0.950 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.217 data_pr9608 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H8 O12 Ru4' _chemical_formula_weight 820.52 _chemical_melting_point ? _chemical_compound_source ? 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' _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 13.257(3) _cell_length_b 9.861(2) _cell_length_c 19.176(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.640(10) _cell_angle_gamma 90.00 _cell_volume 2330.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Maroon _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.339 _exptl_crystal_density_method ? _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 2.603 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.960 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7R four-circle diffractometer' _diffrn_measurement_method 'Omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.7 _diffrn_reflns_number 2788 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2675 _reflns_number_observed 2141 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Rigaku AFC7R diffractometer control software' _computing_cell_refinement 'Rigaku AFC7R diffractometer control software' _computing_data_reduction 'Rigaku AFC7R diffractometer control software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL PLUS (Sheldrick, 1991)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 13 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0558P)^2^+3.3881P] 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 'riding atoms/rigid methyl groups' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2662 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_obs 0.0356 _refine_ls_wR_factor_all 0.1709 _refine_ls_wR_factor_obs 0.0946 _refine_ls_goodness_of_fit_all 1.035 _refine_ls_goodness_of_fit_obs 1.046 _refine_ls_restrained_S_all 1.691 _refine_ls_restrained_S_obs 1.046 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru -0.12241(4) 0.49971(4) 0.12525(2) 0.04395(14) Uani 1 d . . Ru2 Ru -0.09005(3) 0.57260(4) 0.27195(2) 0.03914(13) Uani 1 d . . C1 C -0.2709(6) 0.4554(7) 0.0657(4) 0.064(2) Uani 1 d . . O1 O -0.3585(5) 0.4318(7) 0.0307(3) 0.098(2) Uani 1 d . . C2 C -0.1238(5) 0.6763(6) 0.0829(3) 0.0575(15) Uani 1 d . . O2 O -0.1308(5) 0.7784(6) 0.0547(3) 0.093(2) Uani 1 d . . C3 C -0.0720(6) 0.4122(7) 0.0579(4) 0.061(2) Uani 1 d . . O3 O -0.0410(5) 0.3567(6) 0.0180(3) 0.089(2) Uani 1 d . . C4 C -0.2303(5) 0.6126(6) 0.2007(3) 0.0519(13) Uani 1 d . . O4 O -0.3181(4) 0.6475(6) 0.1720(3) 0.0766(14) Uani 1 d . . C5 C -0.1502(5) 0.5034(6) 0.3404(4) 0.0569(15) Uani 1 d . . O5 O -0.1906(5) 0.4593(7) 0.3780(3) 0.091(2) Uani 1 d . . C6 C -0.0752(5) 0.7639(6) 0.3003(4) 0.0565(14) Uani 1 d . . O6 O -0.0704(5) 0.8762(5) 0.3117(4) 0.094(2) Uani 1 d . . C7 C -0.0909(5) 0.1674(6) 0.1587(4) 0.060(2) Uani 1 d . . H7A H -0.1391(22) 0.1476(26) 0.1084(10) 0.089 Uiso 1 calc R . H7B H -0.0913(36) 0.0933(11) 0.1910(15) 0.089 Uiso 1 calc R . H7C H -0.0187(15) 0.1803(17) 0.1595(25) 0.089 Uiso 1 calc R . C8 C -0.1277(4) 0.2942(5) 0.1854(3) 0.0452(11) Uani 1 d . . H8 H -0.2017(4) 0.3129(5) 0.1674(3) 0.054 Uiso 1 calc R . C9 C -0.0579(4) 0.3859(5) 0.2356(3) 0.0381(10) 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 Ru1 0.0491(3) 0.0435(2) 0.0391(2) 0.0015(2) 0.0160(2) -0.0041(2) Ru2 0.0419(2) 0.0347(2) 0.0459(2) -0.0010(2) 0.0221(2) 0.0026(2) C1 0.072(4) 0.062(4) 0.051(3) -0.004(3) 0.015(3) -0.013(3) O1 0.065(3) 0.127(5) 0.080(4) -0.014(4) -0.001(3) -0.033(3) C2 0.062(4) 0.053(3) 0.052(3) 0.010(3) 0.015(3) 0.002(3) O2 0.102(4) 0.072(3) 0.096(4) 0.042(3) 0.024(3) 0.005(3) C3 0.084(5) 0.054(3) 0.058(4) -0.004(3) 0.041(4) -0.008(3) O3 0.127(5) 0.076(3) 0.088(4) -0.017(3) 0.069(4) -0.017(3) C4 0.047(3) 0.051(3) 0.057(3) 0.001(3) 0.018(3) 0.006(3) O4 0.048(2) 0.092(4) 0.084(3) -0.001(3) 0.018(2) 0.017(3) C5 0.061(4) 0.062(4) 0.057(3) 0.002(3) 0.032(3) 0.007(3) O5 0.098(4) 0.111(4) 0.093(4) 0.029(4) 0.069(4) 0.013(4) C6 0.054(3) 0.047(3) 0.073(4) -0.006(3) 0.029(3) 0.000(3) O6 0.103(4) 0.039(2) 0.140(5) -0.019(3) 0.046(4) 0.001(3) C7 0.069(4) 0.047(3) 0.068(4) -0.014(3) 0.031(3) -0.011(3) C8 0.047(3) 0.040(3) 0.050(3) 0.000(2) 0.021(2) -0.003(2) C9 0.050(3) 0.028(2) 0.044(3) 0.001(2) 0.026(2) -0.004(2) _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 Ru1 C3 1.869(6) . ? Ru1 C2 1.918(6) . ? Ru1 C1 1.927(7) . ? Ru1 C9 2.266(5) . ? Ru1 C8 2.346(5) . ? Ru1 Ru2 2.7793(7) . ? Ru1 Ru2 2.8706(8) 2 ? Ru2 C5 1.896(6) . ? Ru2 C4 1.899(6) . ? Ru2 C6 1.953(6) . ? Ru2 C9 2.068(5) . ? Ru2 Ru2 2.8092(9) 2 ? Ru2 Ru1 2.8706(8) 2 ? C1 O1 1.130(8) . ? C2 O2 1.131(7) . ? C3 O3 1.135(7) . ? C4 O4 1.141(7) . ? C5 O5 1.131(7) . ? C6 O6 1.126(7) . ? C7 C8 1.500(8) . ? C8 C9 1.394(7) . ? C9 C9 1.427(10) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Ru1 C2 94.4(3) . . ? C3 Ru1 C1 91.9(3) . . ? C2 Ru1 C1 96.1(3) . . ? C3 Ru1 C9 107.9(2) . . ? C2 Ru1 C9 141.8(2) . . ? C1 Ru1 C9 113.1(2) . . ? C3 Ru1 C8 91.4(2) . . ? C2 Ru1 C8 174.2(2) . . ? C1 Ru1 C8 83.5(2) . . ? C9 Ru1 C8 35.1(2) . . ? C3 Ru1 Ru2 149.0(2) . . ? C2 Ru1 Ru2 99.6(2) . . ? C1 Ru1 Ru2 113.7(2) . . ? C9 Ru1 Ru2 47.05(12) . . ? C8 Ru1 Ru2 75.34(13) . . ? C3 Ru1 Ru2 94.6(2) . 2 ? C2 Ru1 Ru2 85.2(2) . 2 ? C1 Ru1 Ru2 173.3(2) . 2 ? C9 Ru1 Ru2 62.99(12) . 2 ? C8 Ru1 Ru2 94.50(14) . 2 ? Ru2 Ru1 Ru2 59.60(2) . 2 ? C5 Ru2 C4 91.3(3) . . ? C5 Ru2 C6 100.3(3) . . ? C4 Ru2 C6 88.3(3) . . ? C5 Ru2 C9 96.0(2) . . ? C4 Ru2 C9 102.2(2) . . ? C6 Ru2 C9 160.4(2) . . ? C5 Ru2 Ru1 131.3(2) . . ? C4 Ru2 Ru1 65.2(2) . . ? C6 Ru2 Ru1 119.6(2) . . ? C9 Ru2 Ru1 53.33(14) . . ? C5 Ru2 Ru2 145.9(2) . 2 ? C4 Ru2 Ru2 120.0(2) . 2 ? C6 Ru2 Ru2 94.3(2) . 2 ? C9 Ru2 Ru2 66.14(13) . 2 ? Ru1 Ru2 Ru2 61.82(2) . 2 ? C5 Ru2 Ru1 89.5(2) . 2 ? C4 Ru2 Ru1 176.9(2) . 2 ? C6 Ru2 Ru1 94.5(2) . 2 ? C9 Ru2 Ru1 74.72(15) . 2 ? Ru1 Ru2 Ru1 112.11(2) . 2 ? Ru2 Ru2 Ru1 58.58(2) 2 2 ? O1 C1 Ru1 178.7(7) . . ? O2 C2 Ru1 175.7(6) . . ? O3 C3 Ru1 178.6(6) . . ? O4 C4 Ru2 164.4(6) . . ? O5 C5 Ru2 176.2(7) . . ? O6 C6 Ru2 175.3(7) . . ? C9 C8 C7 124.0(5) . . ? C9 C8 Ru1 69.3(3) . . ? C7 C8 Ru1 118.6(4) . . ? C8 C9 C9 127.8(4) . 2 ? C8 C9 Ru2 130.0(4) . . ? C9 C9 Ru2 101.3(2) 2 . ? C8 C9 Ru1 75.5(3) . . ? C9 C9 Ru1 110.0(4) 2 . ? Ru2 C9 Ru1 79.6(2) . . ? _refine_diff_density_max 0.833 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.120 data_lpc108c _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H12 O12 Ru4' _chemical_formula_weight 944.66 _chemical_melting_point ? _chemical_compound_source 'dichloromethane/hexane at -30 deg. C.' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 19.012(4) _cell_length_b 9.359(2) _cell_length_c 34.315(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6105.8(22) _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 'Dark Purple' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.055 _exptl_crystal_density_method ? _exptl_crystal_F_000 3616 _exptl_absorpt_coefficient_mu 2.002 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 1.00 _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4062 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0775 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4062 _reflns_number_observed 2877 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 14 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0646P)^2^+103.1155P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(15) _refine_ls_number_reflns 4048 _refine_ls_number_parameters 345 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_obs 0.0602 _refine_ls_wR_factor_all 0.2325 _refine_ls_wR_factor_obs 0.1438 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.020 _refine_ls_restrained_S_all 1.366 _refine_ls_restrained_S_obs 1.020 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.2289(2) 0.0306(3) -0.00002(7) 0.0528(7) Uani 1 d . . Ru2 Ru 0.11245(15) 0.0439(2) -0.04885(7) 0.0505(7) Uani 1 d . . Ru3 Ru 0.0607(2) 0.3314(3) -0.06486(7) 0.0524(7) Uani 1 d . . Ru4 Ru 0.20061(14) 0.2772(3) -0.04882(7) 0.0487(7) Uani 1 d . . O11 O 0.3063(15) 0.2174(30) 0.0588(9) 0.090(8) Uiso 1 d . . C11 C 0.2766(19) 0.1414(38) 0.0368(10) 0.065(10) Uiso 1 d . . O12 O 0.2393(13) -0.2468(27) 0.0468(8) 0.080(8) Uiso 1 d . . C12 C 0.2317(17) -0.1390(35) 0.0299(9) 0.054(9) Uiso 1 d . . O13 O 0.3645(14) -0.0741(27) -0.0438(8) 0.083(7) Uiso 1 d . . C13 C 0.3120(19) -0.0346(37) -0.0274(10) 0.061(9) Uiso 1 d . . O21 O 0.1264(14) 0.0184(29) -0.1362(8) 0.089(8) Uiso 1 d . . C21 C 0.1178(17) 0.0354(35) -0.1021(10) 0.057(9) Uiso 1 d . . O22 O 0.1764(11) -0.2556(24) -0.0509(8) 0.068(6) Uiso 1 d . . C22 C 0.1573(16) -0.1379(32) -0.0442(9) 0.049(8) Uiso 1 d . . O23 O -0.0376(15) -0.0693(27) -0.0435(8) 0.082(7) Uiso 1 d . . C23 C 0.0157(21) -0.0289(39) -0.0458(12) 0.071(10) Uiso 1 d . . O31 O -0.0850(17) 0.2719(33) -0.0354(9) 0.105(10) Uiso 1 d . . C31 C -0.0313(22) 0.2946(41) -0.0479(12) 0.077(11) Uiso 1 d . . O32 O 0.0243(17) 0.2776(35) -0.1498(11) 0.111(10) Uiso 1 d . . C32 C 0.0415(20) 0.2925(43) -0.1173(13) 0.077(11) Uiso 1 d . . O33 O 0.0269(11) 0.6490(24) -0.0731(6) 0.062(6) Uiso 1 d . . C33 C 0.0428(16) 0.5292(31) -0.0698(9) 0.044(7) Uiso 1 d . . O41 O 0.3047(18) 0.4810(37) -0.0089(10) 0.117(11) Uiso 1 d . . C41 C 0.2668(23) 0.3992(48) -0.0242(12) 0.086(12) Uiso 1 d . . O42 O 0.3012(16) 0.1299(33) -0.1062(9) 0.106(9) Uiso 1 d . . C42 C 0.2593(19) 0.1767(37) -0.0830(10) 0.065(9) Uiso 1 d . . O43 O 0.1900(15) 0.4799(31) -0.1171(8) 0.091(9) Uiso 1 d . . C43 C 0.1814(21) 0.4075(43) -0.0887(12) 0.076(11) Uiso 1 d . . C51 C 0.0484(10) 0.5209(23) 0.0366(6) 0.060(9) Uiso 1 d G . C52 C 0.0205(13) 0.4372(21) 0.0663(6) 0.062(9) Uiso 1 d G . H52A H 0.0446(17) 0.3565(27) 0.0748(9) 0.075 Uiso 1 calc R . C53 C -0.0434(13) 0.4741(26) 0.0832(6) 0.089(13) Uiso 1 d G . H53A H -0.0620(18) 0.4180(35) 0.1031(8) 0.107 Uiso 1 calc R . C54 C -0.0793(11) 0.5947(28) 0.0705(7) 0.087(12) Uiso 1 d G . H54A H -0.1221(13) 0.6193(39) 0.0819(10) 0.105 Uiso 1 calc R . C55 C -0.0514(12) 0.6784(22) 0.0408(7) 0.079(11) Uiso 1 d G . H55A H -0.0755(16) 0.7591(28) 0.0323(10) 0.095 Uiso 1 calc R . C56 C 0.0124(12) 0.6415(22) 0.0239(6) 0.063(9) Uiso 1 d G . H56A H 0.0311(17) 0.6975(30) 0.0040(8) 0.076 Uiso 1 calc R . C57 C 0.1195(16) 0.4764(34) 0.0185(9) 0.052(9) Uiso 1 d . . H57A H 0.1513(16) 0.4478(34) 0.0392(9) 0.062 Uiso 1 calc R . H57B H 0.1400(16) 0.5582(34) 0.0054(9) 0.062 Uiso 1 calc R . C58 C 0.1125(15) 0.3511(32) -0.0113(9) 0.045(8) Uiso 1 d . . C59 C 0.1228(15) 0.2143(33) -0.0033(9) 0.045(7) Uiso 1 d . . C60 C 0.1245(18) 0.0854(39) 0.0158(10) 0.063(10) Uiso 1 d . . C61 C 0.0764(11) 0.0422(25) 0.0493(6) 0.059(9) Uiso 1 d G . C62 C 0.0055(12) 0.0774(24) 0.0474(6) 0.073(11) Uiso 1 d G . H62A H -0.0122(16) 0.1248(35) 0.0257(7) 0.088 Uiso 1 calc R . C63 C -0.0391(9) 0.0418(26) 0.0780(7) 0.062(9) Uiso 1 d G . H63A H -0.0866(10) 0.0653(37) 0.0768(10) 0.075 Uiso 1 calc R . C64 C -0.0127(11) -0.0291(27) 0.1105(6) 0.084(12) Uiso 1 d G . H64A H -0.0426(15) -0.0529(39) 0.1310(8) 0.101 Uiso 1 calc R . C65 C 0.0582(12) -0.0643(26) 0.1124(5) 0.074(11) Uiso 1 d G . H65A H 0.0758(17) -0.1117(36) 0.1341(7) 0.089 Uiso 1 calc R . C66 C 0.1028(9) -0.0286(25) 0.0818(6) 0.062(9) Uiso 1 d G . H66A H 0.1503(10) -0.0522(36) 0.0830(9) 0.074 Uiso 1 calc R . Ru1' Ru 0.4979(2) 0.9643(3) -0.26550(7) 0.0537(7) Uani 1 d . . Ru2' Ru 0.38233(14) 0.9549(2) -0.21675(7) 0.0480(7) Uani 1 d . . Ru3' Ru 0.32630(15) 0.6725(3) -0.20029(7) 0.0524(7) Uani 1 d . . Ru4' Ru 0.46789(15) 0.7177(3) -0.21567(7) 0.0488(7) Uani 1 d . . O11' O 0.5744(16) 0.7796(34) -0.3227(10) 0.102(9) Uiso 1 d . . C11' C 0.5459(19) 0.8555(39) -0.3004(11) 0.067(10) Uiso 1 d . . O12' O 0.5107(14) 1.2404(30) -0.3117(8) 0.086(8) Uiso 1 d . . C12' C 0.5038(18) 1.1333(37) -0.2933(10) 0.062(9) Uiso 1 d . . O13' O 0.6262(15) 1.0784(32) -0.2206(9) 0.100(9) Uiso 1 d . . C13' C 0.5782(17) 1.0228(33) -0.2356(9) 0.051(8) Uiso 1 d . . O21' O 0.4149(12) 0.9563(25) -0.1296(7) 0.065(6) Uiso 1 d . . C21' C 0.4003(20) 0.9517(40) -0.1615(12) 0.068(10) Uiso 1 d . . O22' O 0.4391(11) 1.2593(23) -0.2196(7) 0.067(6) Uiso 1 d . . C22' C 0.4184(20) 1.1400(42) -0.2228(11) 0.075(11) Uiso 1 d . . O23' O 0.2297(14) 1.0686(28) -0.2137(8) 0.087(8) Uiso 1 d . . C23' C 0.2860(18) 1.0247(34) -0.2160(10) 0.057(8) Uiso 1 d . . O31' O 0.1853(16) 0.7278(32) -0.2380(9) 0.097(9) Uiso 1 d . . C31' C 0.2389(18) 0.7069(34) -0.2218(10) 0.057(8) Uiso 1 d . . O32' O 0.2830(16) 0.7624(33) -0.1140(10) 0.107(10) Uiso 1 d . . C32' C 0.2953(21) 0.7351(43) -0.1471(13) 0.081(12) Uiso 1 d . . O33' O 0.2933(14) 0.3597(29) -0.1838(7) 0.083(8) Uiso 1 d . . C33' C 0.3077(17) 0.4807(34) -0.1917(9) 0.054(9) Uiso 1 d . . O41' O 0.5655(17) 0.5056(35) -0.2527(9) 0.108(10) Uiso 1 d . . C41' C 0.5267(18) 0.5832(37) -0.2391(9) 0.058(9) Uiso 1 d . . O42' O 0.5782(14) 0.8455(28) -0.1632(8) 0.086(8) Uiso 1 d . . C42' C 0.5374(18) 0.7969(34) -0.1848(9) 0.057(9) Uiso 1 d . . O43' O 0.4489(14) 0.5372(30) -0.1420(9) 0.092(8) Uiso 1 d . . C43' C 0.4443(18) 0.6032(37) -0.1710(10) 0.059(9) Uiso 1 d . . C51' C 0.3124(10) 0.4809(23) -0.3000(6) 0.044(8) Uiso 1 d G . C52' C 0.2844(12) 0.5649(21) -0.3296(6) 0.071(10) Uiso 1 d G . H52B H 0.3084(16) 0.6458(26) -0.3380(9) 0.086 Uiso 1 calc R . C53' C 0.2206(13) 0.5279(25) -0.3466(6) 0.085(12) Uiso 1 d G . H53B H 0.2019(18) 0.5841(34) -0.3664(8) 0.102 Uiso 1 calc R . C54' C 0.1848(10) 0.4068(27) -0.3340(7) 0.086(12) Uiso 1 d G . H54B H 0.1422(12) 0.3821(37) -0.3454(10) 0.103 Uiso 1 calc R . C55' C 0.2128(12) 0.3228(22) -0.3044(7) 0.077(11) Uiso 1 d G . H55B H 0.1889(16) 0.2419(28) -0.2960(10) 0.092 Uiso 1 calc R . C56' C 0.2766(12) 0.3599(22) -0.2874(6) 0.082(12) Uiso 1 d G . H56B H 0.2954(17) 0.3037(30) -0.2676(8) 0.098 Uiso 1 calc R . C57' C 0.3839(17) 0.5230(34) -0.2816(9) 0.052(9) Uiso 1 d . . H57C H 0.4040(17) 0.4401(34) -0.2689(9) 0.063 Uiso 1 calc R . H57D H 0.4159(17) 0.5521(34) -0.3022(9) 0.063 Uiso 1 calc R . C58' C 0.3774(15) 0.6412(32) -0.2528(8) 0.043(8) Uiso 1 d . . C59' C 0.3888(15) 0.7852(33) -0.2622(9) 0.046(7) Uiso 1 d . . C60' C 0.3960(15) 0.9089(30) -0.2813(8) 0.038(7) Uiso 1 d . . C61' C 0.3455(12) 0.9562(27) -0.3136(6) 0.062(9) Uiso 1 d G . C62' C 0.2743(13) 0.9243(26) -0.3109(6) 0.076(11) Uiso 1 d G . H62B H 0.2570(17) 0.8774(38) -0.2890(8) 0.091 Uiso 1 calc R . C63' C 0.2289(10) 0.9624(27) -0.3409(7) 0.085(12) Uiso 1 d G . H63B H 0.1812(10) 0.9411(39) -0.3391(10) 0.101 Uiso 1 calc R . C64' C 0.2547(12) 1.0325(27) -0.3736(6) 0.078(11) Uiso 1 d G . H64B H 0.2243(16) 1.0580(40) -0.3937(8) 0.094 Uiso 1 calc R . C65' C 0.3259(13) 1.0644(27) -0.3764(6) 0.092(13) Uiso 1 d G . H65B H 0.3432(18) 1.1113(38) -0.3983(7) 0.111 Uiso 1 calc R . C66' C 0.3713(10) 1.0263(27) -0.3464(7) 0.073(11) Uiso 1 d G . H66B H 0.4190(10) 1.0476(39) -0.3482(10) 0.087 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 Ru1 0.080(2) 0.0377(13) 0.0410(14) 0.0101(12) -0.0017(14) 0.0005(14) Ru2 0.084(2) 0.0325(13) 0.0353(13) 0.0011(12) -0.0016(14) 0.0000(12) Ru3 0.079(2) 0.0334(13) 0.0449(14) 0.0017(11) -0.0030(14) 0.0016(13) Ru4 0.075(2) 0.0325(12) 0.0387(13) 0.0052(13) 0.0024(14) 0.0003(13) Ru1' 0.078(2) 0.0410(14) 0.0417(14) 0.0073(12) 0.0039(14) -0.0012(14) Ru2' 0.076(2) 0.0307(12) 0.0376(13) 0.0019(12) 0.0018(14) 0.0042(12) Ru3' 0.077(2) 0.0380(14) 0.0421(14) 0.0029(11) 0.0056(14) -0.0046(14) Ru4' 0.075(2) 0.0330(11) 0.0387(14) 0.0024(13) -0.0027(14) 0.0040(13) _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 Ru1 C11 1.87(4) . ? Ru1 C12 1.89(3) . ? Ru1 C13 1.94(4) . ? Ru1 C60 2.12(3) . ? Ru1 C22 2.58(3) . ? Ru1 Ru2 2.779(4) . ? Ru1 Ru4 2.902(3) . ? Ru2 C21 1.83(3) . ? Ru2 C22 1.91(3) . ? Ru2 C23 1.96(4) . ? Ru2 C59 2.24(3) . ? Ru2 C60 2.26(3) . ? Ru2 Ru4 2.753(4) . ? Ru2 Ru3 2.916(3) . ? Ru3 C32 1.87(4) . ? Ru3 C31 1.88(4) . ? Ru3 C33 1.89(3) . ? Ru3 C58 2.09(3) . ? Ru3 C43 2.54(4) . ? Ru3 Ru4 2.763(4) . ? Ru4 C43 1.87(4) . ? Ru4 C42 1.87(4) . ? Ru4 C41 1.90(5) . ? Ru4 C58 2.22(3) . ? Ru4 C59 2.23(3) . ? O11 C11 1.18(4) . ? O12 C12 1.17(4) . ? O13 C13 1.20(4) . ? O21 C21 1.19(4) . ? O22 C22 1.18(3) . ? O23 C23 1.09(4) . ? O31 C31 1.13(4) . ? O32 C32 1.17(5) . ? O33 C33 1.17(3) . ? O41 C41 1.17(5) . ? O42 C42 1.21(4) . ? O43 C43 1.20(4) . ? C51 C52 1.39 . ? C51 C56 1.39 . ? C51 C57 1.54(3) . ? C52 C53 1.39 . ? C53 C54 1.39 . ? C54 C55 1.39 . ? C55 C56 1.39 . ? C57 C58 1.56(4) . ? C58 C59 1.32(4) . ? C59 C60 1.37(4) . ? C60 C61 1.52(4) . ? C61 C62 1.39 . ? C61 C66 1.39 . ? C62 C63 1.39 . ? C63 C64 1.39 . ? C64 C65 1.39 . ? C65 C66 1.39 . ? Ru1' C11' 1.82(4) . ? Ru1' C12' 1.85(4) . ? Ru1' C13' 1.92(3) . ? Ru1' C60' 2.08(3) . ? Ru1' Ru2' 2.763(4) . ? Ru1' Ru4' 2.929(3) . ? Ru2' C22' 1.87(4) . ? Ru2' C21' 1.93(4) . ? Ru2' C23' 1.94(3) . ? Ru2' C59' 2.23(3) . ? Ru2' C60' 2.27(3) . ? Ru2' Ru4' 2.752(3) . ? Ru2' Ru3' 2.905(3) . ? Ru3' C31' 1.85(3) . ? Ru3' C33' 1.85(3) . ? Ru3' C32' 2.01(4) . ? Ru3' C58' 2.07(3) . ? Ru3' C43' 2.54(3) . ? Ru3' Ru4' 2.776(4) . ? Ru4' C42' 1.85(3) . ? Ru4' C41' 1.87(4) . ? Ru4' C43' 1.92(4) . ? Ru4' C58' 2.26(3) . ? Ru4' C59' 2.28(3) . ? O11' C11' 1.17(4) . ? O12' C12' 1.19(4) . ? O13' C13' 1.17(4) . ? O21' C21' 1.13(4) . ? O22' C22' 1.19(4) . ? O23' C23' 1.15(3) . ? O31' C31' 1.18(4) . ? O32' C32' 1.19(5) . ? O33' C33' 1.20(4) . ? O41' C41' 1.14(4) . ? O42' C42' 1.16(4) . ? O43' C43' 1.18(4) . ? C51' C52' 1.39 . ? C51' C56' 1.39 . ? C51' C57' 1.55(3) . ? C52' C53' 1.39 . ? C53' C54' 1.39 . ? C54' C55' 1.39 . ? C55' C56' 1.39 . ? C57' C58' 1.49(4) . ? C58' C59' 1.40(4) . ? C59' C60' 1.34(4) . ? C60' C61' 1.53(3) . ? C61' C62' 1.39 . ? C61' C66' 1.39 . ? C62' C63' 1.39 . ? C63' C64' 1.39 . ? C64' C65' 1.39 . ? C65' C66' 1.39 . ? 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 C11 Ru1 C12 94.9(14) . . ? C11 Ru1 C13 96.1(15) . . ? C12 Ru1 C13 88.6(14) . . ? C11 Ru1 C60 98.5(14) . . ? C12 Ru1 C60 95.2(14) . . ? C13 Ru1 C60 164.5(14) . . ? C11 Ru1 C22 173.5(13) . . ? C12 Ru1 C22 79.7(12) . . ? C13 Ru1 C22 87.3(12) . . ? C60 Ru1 C22 78.7(12) . . ? C11 Ru1 Ru2 140.3(11) . . ? C12 Ru1 Ru2 112.8(10) . . ? C13 Ru1 Ru2 111.8(11) . . ? C60 Ru1 Ru2 52.9(9) . . ? C22 Ru1 Ru2 41.6(7) . . ? C11 Ru1 Ru4 92.2(11) . . ? C12 Ru1 Ru4 170.5(10) . . ? C13 Ru1 Ru4 97.0(10) . . ? C60 Ru1 Ru4 77.4(10) . . ? C22 Ru1 Ru4 92.8(7) . . ? Ru2 Ru1 Ru4 57.91(8) . . ? C21 Ru2 C22 91.1(14) . . ? C21 Ru2 C23 95.2(16) . . ? C22 Ru2 C23 96.0(14) . . ? C21 Ru2 C59 136.2(13) . . ? C22 Ru2 C59 122.5(12) . . ? C23 Ru2 C59 107.0(14) . . ? C21 Ru2 C60 168.3(13) . . ? C22 Ru2 C60 91.5(13) . . ? C23 Ru2 C60 95.8(14) . . ? C59 Ru2 C60 35.5(11) . . ? C21 Ru2 Ru4 90.1(10) . . ? C22 Ru2 Ru4 115.8(9) . . ? C23 Ru2 Ru4 147.7(11) . . ? C59 Ru2 Ru4 51.8(7) . . ? C60 Ru2 Ru4 78.6(9) . . ? C21 Ru2 Ru1 123.7(10) . . ? C22 Ru2 Ru1 63.5(9) . . ? C23 Ru2 Ru1 134.2(12) . . ? C59 Ru2 Ru1 62.7(7) . . ? C60 Ru2 Ru1 48.4(9) . . ? Ru4 Ru2 Ru1 63.28(9) . . ? C21 Ru2 Ru3 82.6(10) . . ? C22 Ru2 Ru3 171.1(9) . . ? C23 Ru2 Ru3 90.8(11) . . ? C59 Ru2 Ru3 60.3(8) . . ? C60 Ru2 Ru3 93.5(9) . . ? Ru4 Ru2 Ru3 58.25(9) . . ? Ru1 Ru2 Ru3 115.07(11) . . ? C32 Ru3 C31 94.6(17) . . ? C32 Ru3 C33 94.0(15) . . ? C31 Ru3 C33 92.2(15) . . ? C32 Ru3 C58 162.4(15) . . ? C31 Ru3 C58 100.5(15) . . ? C33 Ru3 C58 94.4(12) . . ? C32 Ru3 C43 85.5(15) . . ? C31 Ru3 C43 174.2(15) . . ? C33 Ru3 C43 81.9(13) . . ? C58 Ru3 C43 80.4(12) . . ? C32 Ru3 Ru4 110.1(12) . . ? C31 Ru3 Ru4 143.4(12) . . ? C33 Ru3 Ru4 111.8(9) . . ? C58 Ru3 Ru4 52.3(8) . . ? C43 Ru3 Ru4 41.0(9) . . ? C32 Ru3 Ru2 93.9(12) . . ? C31 Ru3 Ru2 95.0(12) . . ? C33 Ru3 Ru2 168.8(9) . . ? C58 Ru3 Ru2 76.0(8) . . ? C43 Ru3 Ru2 90.8(9) . . ? Ru4 Ru3 Ru2 57.90(9) . . ? C43 Ru4 C42 89.1(16) . . ? C43 Ru4 C41 93.6(17) . . ? C42 Ru4 C41 100.7(17) . . ? C43 Ru4 C58 94.3(14) . . ? C42 Ru4 C58 165.5(13) . . ? C41 Ru4 C58 93.2(15) . . ? C43 Ru4 C59 123.8(14) . . ? C42 Ru4 C59 134.5(13) . . ? C41 Ru4 C59 106.7(15) . . ? C58 Ru4 C59 34.6(10) . . ? C43 Ru4 Ru2 113.5(12) . . ? C42 Ru4 Ru2 88.0(11) . . ? C41 Ru4 Ru2 151.8(12) . . ? C58 Ru4 Ru2 77.8(8) . . ? C59 Ru4 Ru2 52.2(8) . . ? C43 Ru4 Ru3 63.0(12) . . ? C42 Ru4 Ru3 122.8(11) . . ? C41 Ru4 Ru3 128.1(13) . . ? C58 Ru4 Ru3 48.2(8) . . ? C59 Ru4 Ru3 63.2(8) . . ? Ru2 Ru4 Ru3 63.84(10) . . ? C43 Ru4 Ru1 167.8(12) . . ? C42 Ru4 Ru1 81.4(10) . . ? C41 Ru4 Ru1 95.7(13) . . ? C58 Ru4 Ru1 93.0(8) . . ? C59 Ru4 Ru1 60.6(8) . . ? Ru2 Ru4 Ru1 58.81(9) . . ? Ru3 Ru4 Ru1 116.05(12) . . ? O11 C11 Ru1 176.6(32) . . ? O12 C12 Ru1 173.9(29) . . ? O13 C13 Ru1 178.7(29) . . ? O21 C21 Ru2 173.0(30) . . ? O22 C22 Ru2 162.1(28) . . ? O22 C22 Ru1 121.4(23) . . ? Ru2 C22 Ru1 74.9(10) . . ? O23 C23 Ru2 178.9(37) . . ? O31 C31 Ru3 175.7(38) . . ? O32 C32 Ru3 173.5(38) . . ? O33 C33 Ru3 175.3(27) . . ? O41 C41 Ru4 175.9(40) . . ? O42 C42 Ru4 171.0(32) . . ? O43 C43 Ru4 159.8(35) . . ? O43 C43 Ru3 123.0(30) . . ? Ru4 C43 Ru3 75.9(14) . . ? C52 C51 C56 120.0 . . ? C52 C51 C57 118.5(18) . . ? C56 C51 C57 121.5(18) . . ? C53 C52 C51 120.0 . . ? C54 C53 C52 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C51 C57 C58 113.1(24) . . ? C59 C58 C57 125.4(28) . . ? C59 C58 Ru3 99.5(21) . . ? C57 C58 Ru3 133.0(21) . . ? C59 C58 Ru4 72.9(19) . . ? C57 C58 Ru4 123.3(20) . . ? Ru3 C58 Ru4 79.5(10) . . ? C58 C59 C60 162.1(33) . . ? C58 C59 Ru4 72.5(19) . . ? C60 C59 Ru4 123.4(23) . . ? C58 C59 Ru2 122.1(23) . . ? C60 C59 Ru2 73.1(19) . . ? Ru4 C59 Ru2 76.0(10) . . ? C59 C60 C61 125.4(30) . . ? C59 C60 Ru1 96.5(22) . . ? C61 C60 Ru1 133.6(23) . . ? C59 C60 Ru2 71.4(19) . . ? C61 C60 Ru2 129.4(21) . . ? Ru1 C60 Ru2 78.6(12) . . ? C62 C61 C66 120.0 . . ? C62 C61 C60 118.9(19) . . ? C66 C61 C60 121.0(19) . . ? C63 C62 C61 120.0 . . ? C62 C63 C64 120.0 . . ? C63 C64 C65 120.0 . . ? C66 C65 C64 120.0 . . ? C65 C66 C61 120.0 . . ? C11' Ru1' C12' 96.2(15) . . ? C11' Ru1' C13' 96.5(15) . . ? C12' Ru1' C13' 89.1(14) . . ? C11' Ru1' C60' 99.0(14) . . ? C12' Ru1' C60' 97.8(13) . . ? C13' Ru1' C60' 162.3(12) . . ? C11' Ru1' Ru2' 141.3(11) . . ? C12' Ru1' Ru2' 112.8(11) . . ? C13' Ru1' Ru2' 108.6(9) . . ? C60' Ru1' Ru2' 53.7(8) . . ? C11' Ru1' Ru4' 92.4(11) . . ? C12' Ru1' Ru4' 170.5(11) . . ? C13' Ru1' Ru4' 93.9(9) . . ? C60' Ru1' Ru4' 76.9(8) . . ? Ru2' Ru1' Ru4' 57.75(8) . . ? C22' Ru2' C21' 93.4(17) . . ? C22' Ru2' C23' 92.0(14) . . ? C21' Ru2' C23' 99.2(16) . . ? C22' Ru2' C59' 124.1(14) . . ? C21' Ru2' C59' 131.8(14) . . ? C23' Ru2' C59' 107.5(13) . . ? C22' Ru2' C60' 91.5(14) . . ? C21' Ru2' C60' 159.4(13) . . ? C23' Ru2' C60' 100.7(13) . . ? C59' Ru2' C60' 34.6(10) . . ? C22' Ru2' Ru4' 122.1(12) . . ? C21' Ru2' Ru4' 82.5(11) . . ? C23' Ru2' Ru4' 145.8(9) . . ? C59' Ru2' Ru4' 53.3(8) . . ? C60' Ru2' Ru4' 78.0(7) . . ? C22' Ru2' Ru1' 67.2(12) . . ? C21' Ru2' Ru1' 117.1(12) . . ? C23' Ru2' Ru1' 138.3(10) . . ? C59' Ru2' Ru1' 63.6(8) . . ? C60' Ru2' Ru1' 47.5(7) . . ? Ru4' Ru2' Ru1' 64.14(9) . . ? C22' Ru2' Ru3' 175.1(12) . . ? C21' Ru2' Ru3' 81.9(11) . . ? C23' Ru2' Ru3' 87.6(9) . . ? C59' Ru2' Ru3' 60.5(8) . . ? C60' Ru2' Ru3' 93.4(7) . . ? Ru4' Ru2' Ru3' 58.68(9) . . ? Ru1' Ru2' Ru3' 116.00(11) . . ? C31' Ru3' C33' 93.5(14) . . ? C31' Ru3' C32' 92.8(15) . . ? C33' Ru3' C32' 94.7(15) . . ? C31' Ru3' C58' 95.7(13) . . ? C33' Ru3' C58' 95.3(13) . . ? C32' Ru3' C58' 166.5(14) . . ? C31' Ru3' C43' 175.3(13) . . ? C33' Ru3' C43' 81.9(13) . . ? C32' Ru3' C43' 88.5(14) . . ? C58' Ru3' C43' 83.9(11) . . ? C31' Ru3' Ru4' 140.4(10) . . ? C33' Ru3' Ru4' 111.3(10) . . ? C32' Ru3' Ru4' 114.4(11) . . ? C58' Ru3' Ru4' 53.2(8) . . ? C43' Ru3' Ru4' 42.1(8) . . ? C31' Ru3' Ru2' 95.4(10) . . ? C33' Ru3' Ru2' 169.2(10) . . ? C32' Ru3' Ru2' 91.1(12) . . ? C58' Ru3' Ru2' 77.7(8) . . ? C43' Ru3' Ru2' 89.2(8) . . ? Ru4' Ru3' Ru2' 57.90(9) . . ? C42' Ru4' C41' 95.1(14) . . ? C42' Ru4' C43' 86.2(14) . . ? C41' Ru4' C43' 96.1(14) . . ? C42' Ru4' C58' 174.5(12) . . ? C41' Ru4' C58' 90.0(13) . . ? C43' Ru4' C58' 95.5(12) . . ? C42' Ru4' C59' 139.6(13) . . ? C41' Ru4' C59' 106.3(13) . . ? C43' Ru4' C59' 123.9(13) . . ? C58' Ru4' C59' 36.0(10) . . ? C42' Ru4' Ru2' 96.2(10) . . ? C41' Ru4' Ru2' 153.2(10) . . ? C43' Ru4' Ru2' 108.8(10) . . ? C58' Ru4' Ru2' 78.3(8) . . ? C59' Ru4' Ru2' 51.5(8) . . ? C42' Ru4' Ru3' 130.2(10) . . ? C41' Ru4' Ru3' 124.1(11) . . ? C43' Ru4' Ru3' 62.4(10) . . ? C58' Ru4' Ru3' 47.1(7) . . ? C59' Ru4' Ru3' 62.3(7) . . ? Ru2' Ru4' Ru3' 63.42(10) . . ? C42' Ru4' Ru1' 83.1(10) . . ? C41' Ru4' Ru1' 99.4(10) . . ? C43' Ru4' Ru1' 161.8(10) . . ? C58' Ru4' Ru1' 94.0(8) . . ? C59' Ru4' Ru1' 60.1(8) . . ? Ru2' Ru4' Ru1' 58.11(9) . . ? Ru3' Ru4' Ru1' 114.86(11) . . ? O11' C11' Ru1' 176.4(34) . . ? O12' C12' Ru1' 176.9(32) . . ? O13' C13' Ru1' 169.4(28) . . ? O21' C21' Ru2' 175.0(34) . . ? O22' C22' Ru2' 168.1(34) . . ? O23' C23' Ru2' 176.7(31) . . ? O31' C31' Ru3' 175.3(30) . . ? O32' C32' Ru3' 172.5(35) . . ? O33' C33' Ru3' 175.5(28) . . ? O41' C41' Ru4' 176.4(34) . . ? O42' C42' Ru4' 175.3(30) . . ? O43' C43' Ru4' 162.0(31) . . ? O43' C43' Ru3' 122.3(27) . . ? Ru4' C43' Ru3' 75.4(11) . . ? C52' C51' C56' 120.0 . . ? C52' C51' C57' 119.3(18) . . ? C56' C51' C57' 120.7(18) . . ? C51' C52' C53' 120.0 . . ? C54' C53' C52' 120.0 . . ? C55' C54' C53' 120.0 . . ? C54' C55' C56' 120.0 . . ? C55' C56' C51' 120.0 . . ? C58' C57' C51' 112.8(25) . . ? C59' C58' C57' 123.3(27) . . ? C59' C58' Ru3' 97.8(20) . . ? C57' C58' Ru3' 136.3(22) . . ? C59' C58' Ru4' 73.0(18) . . ? C57' C58' Ru4' 123.2(21) . . ? Ru3' C58' Ru4' 79.7(10) . . ? C60' C59' C58' 163.7(31) . . ? C60' C59' Ru2' 74.5(18) . . ? C58' C59' Ru2' 121.1(21) . . ? C60' C59' Ru4' 121.0(22) . . ? C58' C59' Ru4' 71.1(17) . . ? Ru2' C59' Ru4' 75.2(10) . . ? C59' C60' C61' 122.7(25) . . ? C59' C60' Ru1' 100.6(20) . . ? C61' C60' Ru1' 134.5(19) . . ? C59' C60' Ru2' 70.9(17) . . ? C61' C60' Ru2' 125.4(18) . . ? Ru1' C60' Ru2' 78.7(9) . . ? C62' C61' C66' 120.0 . . ? C62' C61' C60' 120.0(19) . . ? C66' C61' C60' 120.0(19) . . ? C63' C62' C61' 120.0 . . ? C62' C63' C64' 120.0 . . ? C63' C64' C65' 120.0 . . ? C64' C65' C66' 120.0 . . ? C65' C66' C61' 120.0 . . ? _refine_diff_density_max 1.576 _refine_diff_density_min -1.136 _refine_diff_density_rms 0.195 data_pr9609 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H12 O12 Ru4' _chemical_formula_weight 944.66 _chemical_melting_point ? _chemical_compound_source ? 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' _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 10.748(3) _cell_length_b 18.891(4) _cell_length_c 15.778(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.870(10) _cell_angle_gamma 90.00 _cell_volume 3049.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.058 _exptl_crystal_density_method ? _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 2.005 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.889 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5R four-circle diffractometer' _diffrn_measurement_method 'Omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.4 _diffrn_reflns_number 5672 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.1077 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5370 _reflns_number_observed 3298 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Rigaku AFC5R data collection software' _computing_cell_refinement 'Rigaku AFC5R data collection software' _computing_data_reduction 'Riagku AFC5R data collection software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1991)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 12 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5358 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1233 _refine_ls_R_factor_obs 0.0443 _refine_ls_wR_factor_all 0.2145 _refine_ls_wR_factor_obs 0.0927 _refine_ls_goodness_of_fit_all 1.001 _refine_ls_goodness_of_fit_obs 1.052 _refine_ls_restrained_S_all 1.868 _refine_ls_restrained_S_obs 1.052 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru -0.03051(7) 0.19811(4) 0.25734(5) 0.0409(2) Uani 1 d . . Ru2 Ru 0.18597(7) 0.24912(4) 0.21469(4) 0.0335(2) Uani 1 d . . Ru3 Ru 0.25563(7) 0.17088(4) 0.07874(5) 0.0385(2) Uani 1 d . . Ru4 Ru 0.00209(7) 0.16484(4) 0.08628(5) 0.0376(2) Uani 1 d . . O11 O -0.2347(8) 0.0925(5) 0.2652(7) 0.105(3) Uani 1 d . . C11 C -0.1595(10) 0.1322(6) 0.2607(7) 0.061(3) Uani 1 d . . O12 O -0.0222(9) 0.2450(6) 0.4419(6) 0.120(4) Uani 1 d . . C12 C -0.0257(11) 0.2282(7) 0.3725(8) 0.074(4) Uani 1 d . . O13 O -0.2282(8) 0.3087(4) 0.1562(7) 0.095(3) Uani 1 d . . C13 C -0.1518(10) 0.2673(6) 0.1919(8) 0.062(3) Uani 1 d . . O21 O 0.1321(8) 0.3909(4) 0.1115(5) 0.073(2) Uani 1 d . . C21 C 0.1520(9) 0.3389(5) 0.1475(7) 0.047(2) Uani 1 d . . O22 O 0.1826(7) 0.3280(4) 0.3803(4) 0.065(2) Uani 1 d . . C22 C 0.1703(9) 0.2946(5) 0.3178(6) 0.045(2) Uani 1 d . . O23 O 0.4793(7) 0.2642(4) 0.2980(6) 0.082(3) Uani 1 d . . C23 C 0.3714(10) 0.2578(5) 0.2621(7) 0.052(3) Uani 1 d . . O31 O 0.5477(7) 0.1896(5) 0.1472(6) 0.095(3) Uani 1 d . . C31 C 0.4369(10) 0.1825(5) 0.1211(6) 0.054(3) Uani 1 d . . O32 O 0.2055(8) 0.3053(4) -0.0350(5) 0.072(2) Uani 1 d . . C32 C 0.2247(9) 0.2577(6) 0.0106(6) 0.045(2) Uani 1 d . . O33 O 0.2915(11) 0.0852(5) -0.0740(6) 0.118(4) Uani 1 d . . C33 C 0.2762(13) 0.1167(6) -0.0171(7) 0.072(4) Uani 1 d . . O41 O -0.2506(8) 0.0848(5) 0.0650(6) 0.101(3) Uani 1 d . . C41 C -0.1553(10) 0.1159(7) 0.0773(7) 0.063(3) Uani 1 d . . O42 O -0.1226(8) 0.2992(4) -0.0145(6) 0.097(3) Uani 1 d . . C42 C -0.0782(10) 0.2501(6) 0.0234(6) 0.060(3) Uani 1 d . . O43 O -0.0096(9) 0.0803(5) -0.0790(5) 0.096(3) Uani 1 d . . C43 C 0.0056(11) 0.1145(6) -0.0172(6) 0.063(3) Uani 1 d . . C51 C 0.3712(9) 0.0359(5) 0.2154(6) 0.040(2) Uani 1 d . . C52 C 0.4254(9) 0.0603(5) 0.3030(6) 0.045(2) Uani 1 d . . H52 H 0.3850(9) 0.0963(5) 0.3249(6) 0.054 Uiso 1 calc R . C53 C 0.5413(9) 0.0294(6) 0.3569(7) 0.055(3) Uani 1 d . . H53 H 0.5767(9) 0.0448(6) 0.4154(7) 0.067 Uiso 1 calc R . C54 C 0.6033(10) -0.0227(5) 0.3253(8) 0.058(3) Uani 1 d . . H54 H 0.6796(10) -0.0429(5) 0.3624(8) 0.069 Uiso 1 calc R . C55 C 0.5529(11) -0.0454(6) 0.2387(8) 0.065(3) Uani 1 d . . H55 H 0.5960(11) -0.0798(6) 0.2161(8) 0.079 Uiso 1 calc R . C56 C 0.4378(9) -0.0164(5) 0.1858(6) 0.049(2) Uani 1 d . . H56 H 0.4033(9) -0.0328(5) 0.1276(6) 0.058 Uiso 1 calc R . C57 C 0.2496(8) 0.0638(4) 0.1522(5) 0.038(2) Uani 1 d . . H57 H 0.2054(8) 0.0271(4) 0.1097(5) 0.046 Uiso 1 calc R . C58 C 0.1589(8) 0.1091(4) 0.1703(5) 0.034(2) Uani 1 d . . C59 C 0.1638(7) 0.1460(4) 0.2511(5) 0.031(2) Uani 1 d . . C60 C 0.1359(8) 0.1205(5) 0.3276(5) 0.036(2) Uani 1 d . . H60 H 0.1948(8) 0.1418(5) 0.3817(5) 0.043 Uiso 1 calc R . C61 C 0.1041(8) 0.0467(5) 0.3444(5) 0.034(2) Uani 1 d . . C62 C 0.1367(9) 0.0229(6) 0.4319(6) 0.053(3) Uani 1 d . . H62 H 0.1806(9) 0.0530(6) 0.4780(6) 0.064 Uiso 1 calc R . C63 C 0.1052(11) -0.0443(6) 0.4513(7) 0.061(3) Uani 1 d . . H63 H 0.1274(11) -0.0587(6) 0.5104(7) 0.074 Uiso 1 calc R . C64 C 0.0423(11) -0.0902(6) 0.3858(8) 0.065(3) Uani 1 d . . H64 H 0.0225(11) -0.1357(6) 0.4002(8) 0.078 Uiso 1 calc R . C65 C 0.0081(10) -0.0691(5) 0.2982(7) 0.054(3) Uani 1 d . . H65 H -0.0364(10) -0.0997(5) 0.2528(7) 0.065 Uiso 1 calc R . C66 C 0.0416(10) -0.0008(5) 0.2788(6) 0.051(3) Uani 1 d . . H66 H 0.0209(10) 0.0132(5) 0.2196(6) 0.061 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 Ru1 0.0356(4) 0.0401(4) 0.0497(4) -0.0044(4) 0.0169(3) -0.0015(4) Ru2 0.0337(4) 0.0292(4) 0.0350(4) -0.0016(3) 0.0069(3) -0.0022(3) Ru3 0.0446(4) 0.0391(4) 0.0345(4) 0.0044(4) 0.0160(3) 0.0018(4) Ru4 0.0368(4) 0.0374(4) 0.0320(4) 0.0001(3) 0.0010(3) -0.0026(3) O11 0.062(5) 0.112(8) 0.141(8) 0.038(6) 0.030(6) -0.036(5) C11 0.045(6) 0.061(7) 0.080(8) 0.007(6) 0.025(6) -0.010(6) O12 0.112(8) 0.171(10) 0.104(7) -0.064(7) 0.074(6) -0.009(7) C12 0.060(7) 0.095(10) 0.079(8) -0.031(7) 0.040(7) -0.004(7) O13 0.056(5) 0.064(5) 0.146(8) 0.008(6) 0.005(5) 0.023(5) C13 0.041(6) 0.055(7) 0.088(8) -0.006(6) 0.018(6) -0.007(5) O21 0.090(6) 0.051(5) 0.089(6) 0.018(4) 0.044(5) 0.011(4) C21 0.046(6) 0.041(6) 0.057(6) 0.002(5) 0.020(5) 0.000(5) O22 0.079(5) 0.063(5) 0.044(4) -0.022(4) 0.007(4) 0.008(4) C22 0.049(6) 0.044(6) 0.040(5) -0.008(5) 0.010(4) 0.011(5) O23 0.038(4) 0.083(6) 0.108(6) -0.012(5) -0.001(4) -0.013(4) C23 0.045(6) 0.047(6) 0.061(6) -0.005(5) 0.011(5) -0.007(5) O31 0.040(5) 0.126(8) 0.108(7) 0.020(6) 0.009(4) 0.000(5) C31 0.054(7) 0.054(7) 0.050(6) 0.022(5) 0.010(5) 0.000(5) O32 0.100(6) 0.052(5) 0.065(5) 0.025(4) 0.026(4) 0.000(4) C32 0.040(5) 0.056(7) 0.043(5) -0.001(5) 0.019(4) -0.003(5) O33 0.187(11) 0.101(8) 0.089(7) -0.040(6) 0.078(7) -0.012(7) C33 0.117(11) 0.052(7) 0.059(7) -0.010(6) 0.042(7) -0.013(7) O41 0.071(6) 0.133(8) 0.087(6) 0.006(6) 0.006(5) -0.051(6) C41 0.043(6) 0.084(9) 0.054(6) 0.005(6) 0.003(5) -0.012(6) O42 0.090(6) 0.060(5) 0.098(6) 0.028(5) -0.034(5) 0.011(5) C42 0.067(7) 0.048(6) 0.052(6) 0.015(6) -0.001(5) -0.008(6) O43 0.114(7) 0.117(8) 0.056(5) -0.038(5) 0.024(5) -0.012(6) C43 0.074(8) 0.072(8) 0.035(6) -0.002(6) 0.002(5) 0.015(6) C51 0.043(5) 0.035(5) 0.043(5) 0.002(4) 0.012(4) 0.003(4) C52 0.051(6) 0.040(5) 0.041(5) -0.009(4) 0.007(5) 0.008(5) C53 0.037(6) 0.064(7) 0.058(6) 0.005(6) 0.003(5) 0.005(5) C54 0.040(6) 0.048(6) 0.084(8) 0.016(6) 0.019(6) 0.006(5) C55 0.070(8) 0.055(7) 0.074(8) 0.008(6) 0.027(7) 0.012(6) C56 0.057(6) 0.047(6) 0.042(5) -0.002(5) 0.016(5) 0.008(5) C57 0.047(6) 0.031(5) 0.036(5) 0.000(4) 0.013(4) -0.003(4) C58 0.035(5) 0.030(5) 0.036(5) -0.001(4) 0.007(4) -0.016(4) C59 0.023(4) 0.033(5) 0.031(4) 0.005(4) 0.000(3) -0.004(4) C60 0.027(4) 0.047(5) 0.027(4) -0.004(4) 0.001(4) -0.003(4) C61 0.032(5) 0.039(5) 0.028(4) 0.001(4) 0.007(4) 0.001(4) C62 0.054(6) 0.060(7) 0.040(5) 0.010(5) 0.005(5) 0.004(5) C63 0.076(8) 0.061(7) 0.050(6) 0.018(6) 0.024(6) 0.007(6) C64 0.070(8) 0.039(6) 0.087(9) 0.018(6) 0.024(7) 0.000(6) C65 0.060(7) 0.027(5) 0.074(7) 0.007(5) 0.020(6) -0.007(5) C66 0.064(7) 0.042(6) 0.039(5) 0.009(5) 0.006(5) 0.000(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 Ru1 C11 1.876(10) . ? Ru1 C12 1.889(11) . ? Ru1 C13 1.909(11) . ? Ru1 C60 2.316(8) . ? Ru1 C59 2.337(8) . ? Ru1 Ru2 2.7848(12) . ? Ru1 Ru4 2.8952(11) . ? Ru2 C22 1.892(9) . ? Ru2 C23 1.909(10) . ? Ru2 C21 1.973(10) . ? Ru2 C59 2.065(8) . ? Ru2 Ru4 2.8440(11) . ? Ru2 Ru3 2.8865(10) . ? Ru3 C31 1.869(11) . ? Ru3 C33 1.894(11) . ? Ru3 C32 1.933(11) . ? Ru3 C58 2.335(8) . ? Ru3 C57 2.343(8) . ? Ru3 Ru4 2.7662(13) . ? Ru4 C41 1.894(11) . ? Ru4 C43 1.899(11) . ? Ru4 C42 1.950(11) . ? Ru4 C58 2.083(9) . ? O11 C11 1.121(11) . ? O12 C12 1.131(12) . ? O13 C13 1.150(12) . ? O21 C21 1.123(11) . ? O22 C22 1.143(10) . ? O23 C23 1.130(11) . ? O31 C31 1.142(11) . ? O32 C32 1.130(11) . ? O33 C33 1.131(12) . ? O41 C41 1.145(11) . ? O42 C42 1.126(11) . ? O43 C43 1.139(11) . ? C51 C56 1.383(12) . ? C51 C52 1.403(11) . ? C51 C57 1.476(11) . ? C52 C53 1.401(12) . ? C53 C54 1.367(13) . ? C54 C55 1.376(14) . ? C55 C56 1.375(13) . ? C57 C58 1.391(11) . ? C58 C59 1.441(11) . ? C59 C60 1.414(11) . ? C60 C61 1.478(12) . ? C61 C66 1.379(12) . ? C61 C62 1.391(11) . ? C62 C63 1.371(14) . ? C63 C64 1.360(14) . ? C64 C65 1.376(14) . ? C65 C66 1.399(12) . ? 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 C11 Ru1 C12 88.6(5) . . ? C11 Ru1 C13 94.7(4) . . ? C12 Ru1 C13 97.3(5) . . ? C11 Ru1 C60 92.0(4) . . ? C12 Ru1 C60 86.6(4) . . ? C13 Ru1 C60 172.3(4) . . ? C11 Ru1 C59 113.5(4) . . ? C12 Ru1 C59 113.9(4) . . ? C13 Ru1 C59 137.4(4) . . ? C60 Ru1 C59 35.4(3) . . ? C11 Ru1 Ru2 156.3(3) . . ? C12 Ru1 Ru2 110.5(3) . . ? C13 Ru1 Ru2 96.6(3) . . ? C60 Ru1 Ru2 75.8(2) . . ? C59 Ru1 Ru2 46.5(2) . . ? C11 Ru1 Ru4 100.6(3) . . ? C12 Ru1 Ru4 170.5(3) . . ? C13 Ru1 Ru4 84.4(3) . . ? C60 Ru1 Ru4 90.7(2) . . ? C59 Ru1 Ru4 60.3(2) . . ? Ru2 Ru1 Ru4 60.05(3) . . ? C22 Ru2 C23 89.0(4) . . ? C22 Ru2 C21 91.2(4) . . ? C23 Ru2 C21 97.8(4) . . ? C22 Ru2 C59 98.1(4) . . ? C23 Ru2 C59 99.7(4) . . ? C21 Ru2 C59 160.3(3) . . ? C22 Ru2 Ru1 69.4(3) . . ? C23 Ru2 Ru1 141.7(3) . . ? C21 Ru2 Ru1 113.4(3) . . ? C59 Ru2 Ru1 55.2(2) . . ? C22 Ru2 Ru4 129.9(3) . . ? C23 Ru2 Ru4 137.8(3) . . ? C21 Ru2 Ru4 97.1(3) . . ? C59 Ru2 Ru4 63.6(2) . . ? Ru1 Ru2 Ru4 61.90(3) . . ? C22 Ru2 Ru3 169.5(3) . . ? C23 Ru2 Ru3 81.8(3) . . ? C21 Ru2 Ru3 95.0(3) . . ? C59 Ru2 Ru3 78.6(2) . . ? Ru1 Ru2 Ru3 115.39(3) . . ? Ru4 Ru2 Ru3 57.72(3) . . ? C31 Ru3 C33 89.1(5) . . ? C31 Ru3 C32 94.7(4) . . ? C33 Ru3 C32 93.3(4) . . ? C31 Ru3 C58 116.8(3) . . ? C33 Ru3 C58 114.0(4) . . ? C32 Ru3 C58 137.3(3) . . ? C31 Ru3 C57 96.3(4) . . ? C33 Ru3 C57 87.5(4) . . ? C32 Ru3 C57 169.1(3) . . ? C58 Ru3 C57 34.6(3) . . ? C31 Ru3 Ru4 157.3(3) . . ? C33 Ru3 Ru4 111.7(4) . . ? C32 Ru3 Ru4 93.2(3) . . ? C58 Ru3 Ru4 47.3(2) . . ? C57 Ru3 Ru4 76.5(2) . . ? C31 Ru3 Ru2 98.9(3) . . ? C33 Ru3 Ru2 172.0(4) . . ? C32 Ru3 Ru2 86.5(3) . . ? C58 Ru3 Ru2 62.0(2) . . ? C57 Ru3 Ru2 91.2(2) . . ? Ru4 Ru3 Ru2 60.37(3) . . ? C41 Ru4 C43 86.8(5) . . ? C41 Ru4 C42 96.9(5) . . ? C43 Ru4 C42 95.7(4) . . ? C41 Ru4 C58 109.3(4) . . ? C43 Ru4 C58 93.9(4) . . ? C42 Ru4 C58 152.6(4) . . ? C41 Ru4 Ru3 152.4(4) . . ? C43 Ru4 Ru3 72.8(3) . . ? C42 Ru4 Ru3 103.4(3) . . ? C58 Ru4 Ru3 55.4(2) . . ? C41 Ru4 Ru2 137.4(3) . . ? C43 Ru4 Ru2 134.4(4) . . ? C42 Ru4 Ru2 90.1(3) . . ? C58 Ru4 Ru2 65.2(2) . . ? Ru3 Ru4 Ru2 61.91(3) . . ? C41 Ru4 Ru1 79.3(3) . . ? C43 Ru4 Ru1 161.8(4) . . ? C42 Ru4 Ru1 97.7(3) . . ? C58 Ru4 Ru1 79.8(2) . . ? Ru3 Ru4 Ru1 115.71(3) . . ? Ru2 Ru4 Ru1 58.05(3) . . ? O11 C11 Ru1 178.0(11) . . ? O12 C12 Ru1 178.7(13) . . ? O13 C13 Ru1 176.1(11) . . ? O21 C21 Ru2 177.8(9) . . ? O22 C22 Ru2 167.0(9) . . ? O23 C23 Ru2 173.2(9) . . ? O31 C31 Ru3 179.8(8) . . ? O32 C32 Ru3 174.5(9) . . ? O33 C33 Ru3 178.2(12) . . ? O41 C41 Ru4 174.4(10) . . ? O42 C42 Ru4 178.2(11) . . ? O43 C43 Ru4 169.8(11) . . ? C56 C51 C52 117.8(8) . . ? C56 C51 C57 118.0(8) . . ? C52 C51 C57 124.2(8) . . ? C53 C52 C51 119.0(9) . . ? C54 C53 C52 121.4(10) . . ? C53 C54 C55 119.9(10) . . ? C56 C55 C54 119.1(10) . . ? C55 C56 C51 122.8(9) . . ? C58 C57 C51 127.7(8) . . ? C58 C57 Ru3 72.4(5) . . ? C51 C57 Ru3 119.3(6) . . ? C57 C58 C59 130.0(8) . . ? C57 C58 Ru4 131.4(6) . . ? C59 C58 Ru4 96.9(6) . . ? C57 C58 Ru3 73.0(5) . . ? C59 C58 Ru3 113.8(5) . . ? Ru4 C58 Ru3 77.3(3) . . ? C60 C59 C58 129.0(7) . . ? C60 C59 Ru2 129.2(6) . . ? C58 C59 Ru2 100.8(5) . . ? C60 C59 Ru1 71.5(5) . . ? C58 C59 Ru1 116.8(5) . . ? Ru2 C59 Ru1 78.2(3) . . ? C59 C60 C61 126.7(7) . . ? C59 C60 Ru1 73.1(5) . . ? C61 C60 Ru1 119.7(5) . . ? C66 C61 C62 116.8(8) . . ? C66 C61 C60 124.3(7) . . ? C62 C61 C60 118.9(8) . . ? C63 C62 C61 121.1(10) . . ? C64 C63 C62 121.3(10) . . ? C63 C64 C65 119.7(10) . . ? C64 C65 C66 118.6(10) . . ? C61 C66 C65 122.3(9) . . ? _refine_diff_density_max 0.717 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.142 data_lpc108a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C25 H14 O9 Ru3' _chemical_formula_weight 761.57 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.457(3) _cell_length_b 13.594(5) _cell_length_c 9.919(2) _cell_angle_alpha 100.90(2) _cell_angle_beta 105.55(2) _cell_angle_gamma 78.18(3) _cell_volume 1316.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour Orange-yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method ? _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.749 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6375 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6039 _reflns_number_observed 5196 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0909P)^2^+0.2882P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6039 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_obs 0.0441 _refine_ls_wR_factor_all 0.1442 _refine_ls_wR_factor_obs 0.1291 _refine_ls_goodness_of_fit_all 1.226 _refine_ls_goodness_of_fit_obs 1.188 _refine_ls_restrained_S_all 1.226 _refine_ls_restrained_S_obs 1.188 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.28518(3) 0.39114(3) 0.40848(4) 0.03263(12) Uani 1 d . . Ru2 Ru 0.37370(4) 0.36319(3) 0.13815(4) 0.03327(12) Uani 1 d . . Ru3 Ru 0.13319(3) 0.31206(3) 0.15391(4) 0.03201(12) Uani 1 d . . O1 O 0.5112(5) 0.3659(4) 0.6718(5) 0.0696(13) Uani 1 d . . C1 C 0.4287(5) 0.3782(4) 0.5723(6) 0.0444(11) Uani 1 d . . O2 O 0.2299(6) 0.6278(3) 0.4488(7) 0.079(2) Uani 1 d . . C2 C 0.2474(6) 0.5422(4) 0.4324(6) 0.0475(12) Uani 1 d . . O3 O 0.0668(5) 0.3815(4) 0.5514(5) 0.0757(14) Uani 1 d . . C3 C 0.1494(5) 0.3862(4) 0.4987(6) 0.0464(12) Uani 1 d . . O4 O 0.6621(5) 0.4006(5) 0.1723(7) 0.094(2) Uani 1 d . . C4 C 0.5574(6) 0.3839(5) 0.1591(7) 0.0543(14) Uani 1 d . . O5 O 0.2377(4) 0.5815(3) 0.1076(5) 0.0579(11) Uani 1 d . . C5 C 0.2867(5) 0.5009(4) 0.1221(6) 0.0422(11) Uani 1 d . . O6 O 0.3068(5) 0.3149(4) -0.1852(5) 0.0719(14) Uani 1 d . . C6 C 0.3316(6) 0.3311(4) -0.0656(6) 0.0464(12) Uani 1 d . . O7 O -0.0881(5) 0.2359(4) 0.2326(7) 0.085(2) Uani 1 d . . C7 C -0.0068(5) 0.2627(4) 0.2010(7) 0.0501(13) Uani 1 d . . O8 O 0.0429(6) 0.2402(4) -0.1646(5) 0.0715(13) Uani 1 d . . C8 C 0.0772(6) 0.2652(4) -0.0459(6) 0.0451(11) Uani 1 d . . O9 O -0.0334(4) 0.5241(3) 0.1573(4) 0.0578(11) Uani 1 d . . C9 C 0.0302(5) 0.4459(4) 0.1564(5) 0.0396(10) Uani 1 d . . C10 C 0.6207(6) 0.1621(4) 0.3520(6) 0.0505(12) Uani 1 d . . H10 H 0.5730(6) 0.2139(4) 0.4038(6) 0.061 Uiso 1 calc R . C11 C 0.7445(6) 0.1097(6) 0.4193(8) 0.067(2) Uani 1 d . . H11 H 0.7795(6) 0.1265(6) 0.5157(8) 0.080 Uiso 1 calc R . C12 C 0.8133(7) 0.0334(6) 0.3416(10) 0.079(2) Uani 1 d . . H12 H 0.8946(7) -0.0023(6) 0.3862(10) 0.095 Uiso 1 calc R . C13 C 0.7639(7) 0.0091(5) 0.1989(9) 0.076(2) Uani 1 d . . H13 H 0.8121(7) -0.0426(5) 0.1475(9) 0.091 Uiso 1 calc R . C14 C 0.6416(6) 0.0615(4) 0.1303(7) 0.0514(13) Uani 1 d . . H14 H 0.6091(6) 0.0460(4) 0.0332(7) 0.062 Uiso 1 calc R . C15 C 0.5695(5) 0.1366(4) 0.2080(6) 0.0405(10) Uani 1 d . . C16 C 0.4335(5) 0.1854(3) 0.1320(5) 0.0344(9) Uani 1 d . . H16 H 0.4030(5) 0.1487(3) 0.0373(5) 0.041 Uiso 1 calc R . C17 C 0.3284(5) 0.2239(3) 0.1985(5) 0.0338(9) Uani 1 d . . C18 C 0.2938(4) 0.2392(3) 0.3251(5) 0.0339(9) Uani 1 d . . C19 C 0.2849(6) 0.1531(4) 0.3992(6) 0.0457(11) Uani 1 d . . H19B H 0.3603(6) 0.1485(4) 0.4811(6) 0.055 Uiso 1 calc R . H19A H 0.2033(6) 0.1709(4) 0.4333(6) 0.055 Uiso 1 calc R . C20 C 0.2848(6) 0.0483(4) 0.3103(6) 0.0459(12) Uani 1 d . . C21 C 0.1648(7) 0.0170(5) 0.2308(9) 0.068(2) Uani 1 d . . H21 H 0.0842(7) 0.0615(5) 0.2293(9) 0.082 Uiso 1 calc R . C22 C 0.1635(10) -0.0780(6) 0.1551(11) 0.093(3) Uani 1 d . . H22 H 0.0826(10) -0.0970(6) 0.1010(11) 0.112 Uiso 1 calc R . C23 C 0.2819(11) -0.1461(5) 0.1585(9) 0.087(3) Uani 1 d . . H23 H 0.2806(11) -0.2115(5) 0.1096(9) 0.104 Uiso 1 calc R . C24 C 0.3997(9) -0.1167(5) 0.2336(8) 0.072(2) Uani 1 d . . H24 H 0.4796(9) -0.1620(5) 0.2338(8) 0.086 Uiso 1 calc R . C25 C 0.4037(7) -0.0190(4) 0.3113(6) 0.0531(13) Uani 1 d . . H25 H 0.4853(7) 0.0001(4) 0.3629(6) 0.064 Uiso 1 calc R . H012 H 0.4235 0.4021 0.3315 0.080 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 Ru1 0.0318(2) 0.0285(2) 0.0343(2) 0.00232(14) 0.00649(14) -0.00132(14) Ru2 0.0328(2) 0.0285(2) 0.0380(2) 0.00973(14) 0.00927(15) 0.00175(14) Ru3 0.0286(2) 0.0254(2) 0.0371(2) 0.00665(14) 0.00206(14) 0.00083(13) O1 0.062(3) 0.084(3) 0.055(3) 0.017(2) -0.015(2) -0.026(2) C1 0.044(3) 0.041(3) 0.046(3) 0.003(2) 0.005(2) -0.011(2) O2 0.092(4) 0.031(2) 0.116(4) 0.000(2) 0.040(3) -0.005(2) C2 0.046(3) 0.038(3) 0.056(3) 0.000(2) 0.016(2) -0.003(2) O3 0.063(3) 0.100(4) 0.073(3) 0.005(3) 0.038(3) -0.012(3) C3 0.041(3) 0.051(3) 0.045(3) 0.001(2) 0.014(2) -0.003(2) O4 0.046(3) 0.119(5) 0.126(5) 0.029(4) 0.029(3) -0.017(3) C4 0.043(3) 0.054(3) 0.072(4) 0.017(3) 0.023(3) 0.000(2) O5 0.056(2) 0.032(2) 0.077(3) 0.018(2) 0.001(2) 0.004(2) C5 0.041(2) 0.037(2) 0.048(3) 0.011(2) 0.004(2) -0.008(2) O6 0.081(3) 0.088(4) 0.043(2) 0.019(2) 0.021(2) 0.010(3) C6 0.051(3) 0.045(3) 0.044(3) 0.011(2) 0.018(2) 0.005(2) O7 0.057(3) 0.080(4) 0.134(5) 0.032(3) 0.034(3) -0.016(3) C7 0.036(3) 0.046(3) 0.065(3) 0.010(3) 0.004(2) -0.006(2) O8 0.091(4) 0.063(3) 0.047(2) -0.009(2) -0.001(2) -0.018(3) C8 0.046(3) 0.033(2) 0.048(3) 0.001(2) 0.004(2) -0.002(2) O9 0.063(3) 0.037(2) 0.059(2) 0.007(2) 0.008(2) 0.017(2) C9 0.036(2) 0.033(2) 0.040(2) 0.004(2) -0.001(2) 0.000(2) C10 0.042(3) 0.049(3) 0.054(3) 0.011(2) 0.007(2) 0.005(2) C11 0.049(3) 0.075(4) 0.065(4) 0.024(3) -0.007(3) 0.001(3) C12 0.040(3) 0.075(5) 0.114(7) 0.042(5) 0.003(4) 0.015(3) C13 0.051(4) 0.055(4) 0.107(6) 0.009(4) 0.021(4) 0.022(3) C14 0.046(3) 0.040(3) 0.062(3) 0.003(2) 0.014(3) 0.003(2) C15 0.037(2) 0.030(2) 0.052(3) 0.012(2) 0.008(2) 0.003(2) C16 0.038(2) 0.025(2) 0.035(2) 0.006(2) 0.007(2) 0.005(2) C17 0.034(2) 0.022(2) 0.041(2) 0.006(2) 0.003(2) 0.001(2) C18 0.031(2) 0.024(2) 0.042(2) 0.008(2) 0.002(2) 0.001(2) C19 0.060(3) 0.033(2) 0.045(3) 0.013(2) 0.013(2) -0.002(2) C20 0.057(3) 0.030(2) 0.053(3) 0.018(2) 0.012(2) -0.004(2) C21 0.054(3) 0.044(3) 0.100(5) 0.011(3) 0.002(3) -0.014(3) C22 0.103(7) 0.054(4) 0.116(7) 0.014(4) -0.003(5) -0.038(4) C23 0.134(8) 0.038(3) 0.086(6) 0.002(3) 0.023(5) -0.018(4) C24 0.098(6) 0.040(3) 0.077(5) 0.011(3) 0.031(4) 0.010(3) C25 0.060(3) 0.042(3) 0.056(3) 0.015(2) 0.014(3) 0.003(2) _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 Ru1 C3 1.888(5) . ? Ru1 C1 1.902(5) . ? Ru1 C2 1.991(5) . ? Ru1 C18 2.068(4) . ? Ru1 Ru3 2.7531(9) . ? Ru1 Ru2 2.9988(8) . ? Ru2 C5 1.922(5) . ? Ru2 C6 1.933(5) . ? Ru2 C4 1.949(6) . ? Ru2 C17 2.263(4) . ? Ru2 C16 2.363(4) . ? Ru2 Ru3 2.7930(9) . ? Ru3 C9 1.914(5) . ? Ru3 C7 1.924(6) . ? Ru3 C8 1.931(5) . ? Ru3 C17 2.124(4) . ? Ru3 C18 2.260(4) . ? O1 C1 1.137(7) . ? O2 C2 1.127(7) . ? O3 C3 1.141(7) . ? O4 C4 1.131(8) . ? O5 C5 1.128(6) . ? O6 C6 1.132(7) . ? O7 C7 1.125(7) . ? O8 C8 1.141(7) . ? O9 C9 1.133(6) . ? C10 C15 1.388(8) . ? C10 C11 1.403(8) . ? C11 C12 1.370(11) . ? C12 C13 1.372(12) . ? C13 C14 1.396(9) . ? C14 C15 1.380(7) . ? C15 C16 1.502(6) . ? C16 C17 1.393(6) . ? C17 C18 1.365(7) . ? C18 C19 1.524(6) . ? C19 C20 1.527(7) . ? C20 C25 1.383(8) . ? C20 C21 1.393(9) . ? C21 C22 1.366(10) . ? C22 C23 1.382(13) . ? C23 C24 1.352(12) . ? C24 C25 1.406(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 C3 Ru1 C1 95.2(2) . . ? C3 Ru1 C2 91.8(2) . . ? C1 Ru1 C2 97.1(2) . . ? C3 Ru1 C18 91.9(2) . . ? C1 Ru1 C18 98.6(2) . . ? C2 Ru1 C18 163.5(2) . . ? C3 Ru1 Ru3 90.3(2) . . ? C1 Ru1 Ru3 151.9(2) . . ? C2 Ru1 Ru3 110.3(2) . . ? C18 Ru1 Ru3 53.66(12) . . ? C3 Ru1 Ru2 148.0(2) . . ? C1 Ru1 Ru2 114.3(2) . . ? C2 Ru1 Ru2 96.2(2) . . ? C18 Ru1 Ru2 72.63(14) . . ? Ru3 Ru1 Ru2 57.91(2) . . ? C5 Ru2 C6 89.9(2) . . ? C5 Ru2 C4 97.7(2) . . ? C6 Ru2 C4 96.0(3) . . ? C5 Ru2 C17 137.0(2) . . ? C6 Ru2 C17 100.9(2) . . ? C4 Ru2 C17 121.9(2) . . ? C5 Ru2 C16 167.5(2) . . ? C6 Ru2 C16 84.1(2) . . ? C4 Ru2 C16 93.9(2) . . ? C17 Ru2 C16 35.0(2) . . ? C5 Ru2 Ru3 90.2(2) . . ? C6 Ru2 Ru3 92.3(2) . . ? C4 Ru2 Ru3 168.5(2) . . ? C17 Ru2 Ru3 48.30(11) . . ? C16 Ru2 Ru3 79.08(12) . . ? C5 Ru2 Ru1 86.3(2) . . ? C6 Ru2 Ru1 148.6(2) . . ? C4 Ru2 Ru1 115.4(2) . . ? C17 Ru2 Ru1 63.26(12) . . ? C16 Ru2 Ru1 93.15(11) . . ? Ru3 Ru2 Ru1 56.63(2) . . ? C9 Ru3 C7 90.7(2) . . ? C9 Ru3 C8 98.4(2) . . ? C7 Ru3 C8 94.2(3) . . ? C9 Ru3 C17 146.1(2) . . ? C7 Ru3 C17 116.4(2) . . ? C8 Ru3 C17 99.4(2) . . ? C9 Ru3 C18 130.8(2) . . ? C7 Ru3 C18 92.3(2) . . ? C8 Ru3 C18 130.3(2) . . ? C17 Ru3 C18 36.1(2) . . ? C9 Ru3 Ru1 84.49(14) . . ? C7 Ru3 Ru1 105.2(2) . . ? C8 Ru3 Ru1 160.4(2) . . ? C17 Ru3 Ru1 69.55(12) . . ? C18 Ru3 Ru1 47.48(11) . . ? C9 Ru3 Ru2 97.3(2) . . ? C7 Ru3 Ru2 166.9(2) . . ? C8 Ru3 Ru2 94.9(2) . . ? C17 Ru3 Ru2 52.68(12) . . ? C18 Ru3 Ru2 74.65(12) . . ? Ru1 Ru3 Ru2 65.46(2) . . ? O1 C1 Ru1 175.9(5) . . ? O2 C2 Ru1 177.8(6) . . ? O3 C3 Ru1 178.7(6) . . ? O4 C4 Ru2 176.9(6) . . ? O5 C5 Ru2 177.0(5) . . ? O6 C6 Ru2 178.3(5) . . ? O7 C7 Ru3 177.7(6) . . ? O8 C8 Ru3 178.2(5) . . ? O9 C9 Ru3 178.4(5) . . ? C15 C10 C11 119.9(6) . . ? C12 C11 C10 119.3(7) . . ? C11 C12 C13 120.8(6) . . ? C12 C13 C14 120.4(6) . . ? C15 C14 C13 119.3(6) . . ? C14 C15 C10 120.1(5) . . ? C14 C15 C16 117.6(5) . . ? C10 C15 C16 122.3(5) . . ? C17 C16 C15 122.8(4) . . ? C17 C16 Ru2 68.6(2) . . ? C15 C16 Ru2 122.2(3) . . ? C18 C17 C16 143.7(4) . . ? C18 C17 Ru3 77.4(3) . . ? C16 C17 Ru3 138.5(3) . . ? C18 C17 Ru2 114.7(3) . . ? C16 C17 Ru2 76.4(3) . . ? Ru3 C17 Ru2 79.02(14) . . ? C17 C18 C19 123.4(4) . . ? C17 C18 Ru1 109.3(3) . . ? C19 C18 Ru1 126.7(3) . . ? C17 C18 Ru3 66.5(3) . . ? C19 C18 Ru3 127.4(3) . . ? Ru1 C18 Ru3 78.86(14) . . ? C20 C19 C18 116.2(4) . . ? C25 C20 C21 118.5(5) . . ? C25 C20 C19 120.6(5) . . ? C21 C20 C19 120.8(5) . . ? C22 C21 C20 121.1(7) . . ? C21 C22 C23 120.3(8) . . ? C24 C23 C22 119.4(7) . . ? C23 C24 C25 121.2(7) . . ? C20 C25 C24 119.3(6) . . ? _refine_diff_density_max 1.267 _refine_diff_density_min -2.226 _refine_diff_density_rms 0.370