# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2079 data_global _audit_creation_method SHELXL-97 # SUBMISSION DETAILS _publ_contact_author ; Dr Jonathan P. H. Charmant School of Chemistry University of Bristol Bristol BS8 1TS UK ; _publ_contact_author_email jon.charmant@bris.ac.uk _publ_contact_author_fax '+44(0)117 929 0509' _publ_contact_author_phone '+44(0)117 928 9812' _publ_contact_letter ; Please consider this CIF submission for publication in J. Chem. Soc., Dalton Trans. ; _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Reactivity of Dimetallacyclopentenone Complexes [Ru~2~(CO) (\m-CO){\m-C(O)CR^1^CR^2^}(\h-C~5~H~5~)~2~] (R^1^ = Me or Ph; R^2^ = CO~2~Me): X-ray Crystal Structures of [Ru~2~(CO)~2~ {\m-\h^2^,\h^2^-C(O)C~6~H~4~C=C(H)CO~2~Me}(\h-C~5~H~5~)~2~] and [Ru~3~(CO) (\m-CO)~2~{\m~3~-\h^2^-C(Ph)C(CO~2~Me)}(\m~3~-\h^1^,\h^5^-C~5~H~4~) (\h-C~5~H~5~)~2~] ; loop_ _publ_author_name _publ_author_address 'Philip J. King' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; 'Philip J. King' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; 'Selby A. R. Knox' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; 'Gillian J. McCormick' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; 'A. Guy Orpen' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; _publ_section_abstract ; ABSTRACT ; ######################################################################## # data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H18 O5 Ru2' _chemical_formula_weight 576.51 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 14.461(5) _cell_length_b 9.755(4) _cell_length_c 15.217(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.74(3) _cell_angle_gamma 90.00 _cell_volume 2020.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 7.4 _cell_measurement_theta_max 17.0 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 1.528 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.483 _exptl_absorpt_correction_T_max 0.597 _exptl_absorpt_process_details ; Parameters determined using XEMP (Siemens AXS Inc.) software with 420 Psi-scan data and an elipsoidal model of crystal shape. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3/mV' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5029 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.01 _reflns_number_total 4852 _reflns_number_gt 4468 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+1.4140P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4852 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0598 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.777791(13) 0.010956(18) 0.113739(12) 0.02874(6) Uani 1 1 d . . . Ru2 Ru 0.735538(13) 0.253108(17) 0.005785(12) 0.02905(6) Uani 1 1 d . . . O1 O 0.57222(17) 0.0741(3) 0.1061(2) 0.0678(7) Uani 1 1 d . . . O2 O 0.87844(19) 0.4024(3) 0.16794(16) 0.0716(7) Uani 1 1 d . . . O3 O 0.66531(19) -0.2431(2) 0.05965(15) 0.0572(6) Uani 1 1 d . . . O4 O 1.00577(16) 0.1812(4) 0.10385(18) 0.0870(10) Uani 1 1 d . . . O5 O 0.99102(14) 0.2950(2) -0.02559(15) 0.0515(5) Uani 1 1 d . . . C1 C 0.6500(2) 0.0603(3) 0.10348(19) 0.0411(5) Uani 1 1 d . . . C2 C 0.8265(2) 0.3379(3) 0.10832(19) 0.0434(6) Uani 1 1 d . . . C3 C 0.69844(18) -0.1456(2) 0.03079(17) 0.0353(5) Uani 1 1 d . . . C4 C 0.68403(16) -0.1310(2) -0.07065(16) 0.0310(4) Uani 1 1 d . . . C5 C 0.62350(19) -0.2174(3) -0.13890(19) 0.0391(5) Uani 1 1 d . . . H5A H 0.5877 -0.2864 -0.1229 0.045(8) Uiso 1 1 calc R . . C6 C 0.6174(2) -0.1992(3) -0.23087(19) 0.0458(6) Uani 1 1 d . . . H6A H 0.5765 -0.2552 -0.2773 0.073(12) Uiso 1 1 calc R . . C7 C 0.6720(2) -0.0979(3) -0.25353(19) 0.0476(6) Uani 1 1 d . . . H7A H 0.6683 -0.0873 -0.3154 0.062(10) Uiso 1 1 calc R . . C8 C 0.7322(2) -0.0117(3) -0.18605(18) 0.0410(6) Uani 1 1 d . . . H8A H 0.7694 0.0550 -0.2024 0.036(7) Uiso 1 1 calc R . . C9 C 0.73674(16) -0.0253(2) -0.09290(16) 0.0294(4) Uani 1 1 d . . . C10 C 0.79545(15) 0.0613(2) -0.01225(15) 0.0277(4) Uani 1 1 d . . . C11 C 0.85694(16) 0.1648(2) -0.03085(16) 0.0317(4) Uani 1 1 d . . . H11A H 0.8456 0.1731 -0.0979 0.038(7) Uiso 1 1 calc R . . C12 C 0.95687(18) 0.2100(3) 0.02554(18) 0.0390(5) Uani 1 1 d . . . C13 C 1.0881(2) 0.3498(4) 0.0192(3) 0.0639(9) Uani 1 1 d . . . H13A H 1.1050 0.4089 -0.0235 0.110(17) Uiso 1 1 calc R . . H13B H 1.1346 0.2759 0.0374 0.093(15) Uiso 1 1 calc R . . H13C H 1.0894 0.4011 0.0735 0.087(14) Uiso 1 1 calc R . . C14 C 0.9155(3) 0.0722(4) 0.2376(2) 0.0685(11) Uani 1 1 d . . . H14A H 0.9479 0.1619 0.2469 0.059(9) Uiso 1 1 calc R . . C15 C 0.8401(3) 0.0325(4) 0.27078(19) 0.0637(9) Uani 1 1 d . . . H15A H 0.8124 0.0888 0.3091 0.062(10) Uiso 1 1 calc R . . C16 C 0.8164(2) -0.1078(3) 0.24605(19) 0.0517(7) Uani 1 1 d . . . H16A H 0.7720 -0.1658 0.2663 0.062(10) Uiso 1 1 calc R . . C17 C 0.8787(2) -0.1513(3) 0.1970(2) 0.0522(7) Uani 1 1 d . . . H17A H 0.8836 -0.2452 0.1760 0.066(11) Uiso 1 1 calc R . . C18 C 0.9382(2) -0.0401(4) 0.1904(2) 0.0632(9) Uani 1 1 d . . . H18A H 0.9904 -0.0429 0.1628 0.075(12) Uiso 1 1 calc R . . C19 C 0.6707(2) 0.4187(3) -0.0964(2) 0.0505(7) Uani 1 1 d . . . H19A H 0.7072 0.4880 -0.1181 0.066(11) Uiso 1 1 calc R . . C20 C 0.6344(2) 0.4336(3) -0.0227(2) 0.0554(7) Uani 1 1 d . . . H20A H 0.6426 0.5147 0.0172 0.090(14) Uiso 1 1 calc R . . C21 C 0.5793(2) 0.3179(4) -0.0192(3) 0.0659(10) Uani 1 1 d . . . H21A H 0.5423 0.3035 0.0234 0.110(16) Uiso 1 1 calc R . . C22 C 0.5808(2) 0.2292(3) -0.0923(3) 0.0700(12) Uani 1 1 d . . . H22A H 0.5446 0.1429 -0.1100 0.087(13) Uiso 1 1 calc R . . C23 C 0.6370(2) 0.2931(4) -0.1393(2) 0.0572(8) Uani 1 1 d . . . H23B H 0.6468 0.2588 -0.1961 0.087(14) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03142(10) 0.02896(9) 0.02439(9) 0.00308(6) 0.00752(7) 0.00092(7) Ru2 0.03029(10) 0.02515(9) 0.03035(10) 0.00112(6) 0.00845(7) 0.00024(6) O1 0.0522(13) 0.0686(15) 0.0982(19) 0.0210(14) 0.0457(13) 0.0111(11) O2 0.0798(16) 0.0732(16) 0.0540(13) -0.0250(12) 0.0125(12) -0.0291(13) O3 0.0858(16) 0.0405(11) 0.0480(11) 0.0026(8) 0.0262(11) -0.0251(10) O4 0.0437(12) 0.132(3) 0.0647(15) 0.0404(16) -0.0090(11) -0.0329(14) O5 0.0405(10) 0.0574(12) 0.0548(12) 0.0046(10) 0.0136(9) -0.0201(9) C1 0.0457(14) 0.0383(13) 0.0423(13) 0.0051(10) 0.0188(11) 0.0021(11) C2 0.0473(14) 0.0414(13) 0.0411(13) -0.0043(11) 0.0144(11) -0.0057(11) C3 0.0408(12) 0.0296(11) 0.0360(12) 0.0020(9) 0.0137(10) -0.0025(9) C4 0.0337(11) 0.0260(10) 0.0341(11) -0.0018(8) 0.0126(9) 0.0005(8) C5 0.0426(13) 0.0324(11) 0.0453(13) -0.0078(10) 0.0186(11) -0.0074(10) C6 0.0498(15) 0.0458(14) 0.0410(13) -0.0175(12) 0.0142(11) -0.0122(12) C7 0.0572(16) 0.0556(16) 0.0326(12) -0.0101(12) 0.0187(12) -0.0103(13) C8 0.0506(14) 0.0430(13) 0.0336(12) -0.0057(10) 0.0196(11) -0.0110(11) C9 0.0297(10) 0.0282(10) 0.0307(10) -0.0023(8) 0.0107(8) 0.0003(8) C10 0.0285(10) 0.0272(10) 0.0275(10) 0.0011(8) 0.0096(8) 0.0002(8) C11 0.0310(11) 0.0342(11) 0.0306(11) 0.0008(9) 0.0113(9) -0.0028(9) C12 0.0317(11) 0.0430(13) 0.0430(13) 0.0017(11) 0.0137(10) -0.0038(10) C13 0.0425(16) 0.065(2) 0.084(2) -0.0055(19) 0.0211(16) -0.0226(15) C14 0.065(2) 0.061(2) 0.0473(17) 0.0119(15) -0.0229(15) -0.0122(17) C15 0.093(3) 0.064(2) 0.0230(12) -0.0004(12) 0.0048(14) 0.0078(18) C16 0.0643(18) 0.0574(17) 0.0322(13) 0.0150(12) 0.0148(12) 0.0063(14) C17 0.0551(17) 0.0507(16) 0.0445(15) 0.0175(13) 0.0087(13) 0.0154(13) C18 0.0377(15) 0.079(2) 0.062(2) 0.0340(18) 0.0028(14) 0.0116(15) C19 0.0508(16) 0.0416(14) 0.0574(17) 0.0199(13) 0.0158(13) 0.0098(12) C20 0.0637(18) 0.0404(15) 0.0591(18) 0.0045(13) 0.0168(15) 0.0221(14) C21 0.0462(16) 0.070(2) 0.089(3) 0.037(2) 0.0323(17) 0.0265(16) C22 0.0362(15) 0.0412(15) 0.102(3) 0.0162(17) -0.0171(16) 0.0013(12) C23 0.0571(18) 0.0611(18) 0.0393(14) 0.0047(13) -0.0022(13) 0.0253(15) _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 C1 1.865(3) . ? Ru1 C3 2.065(2) . ? Ru1 C10 2.077(2) . ? Ru1 C16 2.224(3) . ? Ru1 C17 2.234(3) . ? Ru1 C15 2.261(3) . ? Ru1 C18 2.272(3) . ? Ru1 C14 2.311(3) . ? Ru1 Ru2 2.8238(9) . ? Ru2 C2 1.861(3) . ? Ru2 C10 2.118(2) . ? Ru2 C11 2.190(2) . ? Ru2 C19 2.218(3) . ? Ru2 C23 2.221(3) . ? Ru2 C20 2.236(3) . ? Ru2 C22 2.244(3) . ? Ru2 C21 2.252(3) . ? O1 C1 1.146(3) . ? O2 C2 1.150(3) . ? O3 C3 1.212(3) . ? O4 C12 1.196(3) . ? O5 C12 1.340(3) . ? O5 C13 1.440(3) . ? C3 C4 1.493(3) . ? C4 C9 1.390(3) . ? C4 C5 1.394(3) . ? C5 C6 1.383(4) . ? C6 C7 1.380(4) . ? C7 C8 1.384(4) . ? C8 C9 1.403(3) . ? C9 C10 1.496(3) . ? C10 C11 1.435(3) . ? C11 C12 1.477(3) . ? C14 C15 1.402(5) . ? C14 C18 1.408(6) . ? C15 C16 1.430(5) . ? C16 C17 1.414(4) . ? C17 C18 1.410(5) . ? C19 C23 1.397(5) . ? C19 C20 1.397(5) . ? C20 C21 1.393(5) . ? C21 C22 1.415(6) . ? C22 C23 1.398(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C3 79.02(11) . . ? C1 Ru1 C10 106.80(10) . . ? C3 Ru1 C10 80.03(9) . . ? C1 Ru1 C16 98.58(12) . . ? C3 Ru1 C16 94.92(11) . . ? C10 Ru1 C16 152.51(10) . . ? C1 Ru1 C17 132.01(12) . . ? C3 Ru1 C17 86.79(12) . . ? C10 Ru1 C17 115.53(10) . . ? C16 Ru1 C17 36.99(11) . . ? C1 Ru1 C15 95.41(14) . . ? C3 Ru1 C15 130.96(12) . . ? C10 Ru1 C15 145.53(12) . . ? C16 Ru1 C15 37.17(12) . . ? C17 Ru1 C15 61.03(13) . . ? C1 Ru1 C18 155.63(13) . . ? C3 Ru1 C18 114.32(13) . . ? C10 Ru1 C18 95.91(11) . . ? C16 Ru1 C18 61.35(12) . . ? C17 Ru1 C18 36.47(12) . . ? C15 Ru1 C18 60.30(15) . . ? C1 Ru1 C14 123.94(15) . . ? C3 Ru1 C14 146.88(12) . . ? C10 Ru1 C14 110.56(12) . . ? C16 Ru1 C14 60.82(13) . . ? C17 Ru1 C14 60.18(13) . . ? C15 Ru1 C14 35.70(14) . . ? C18 Ru1 C14 35.77(14) . . ? C1 Ru1 Ru2 73.84(8) . . ? C3 Ru1 Ru2 107.27(7) . . ? C10 Ru1 Ru2 48.32(6) . . ? C16 Ru1 Ru2 154.30(9) . . ? C17 Ru1 Ru2 153.42(8) . . ? C15 Ru1 Ru2 117.89(9) . . ? C18 Ru1 Ru2 117.69(9) . . ? C14 Ru1 Ru2 102.47(9) . . ? C2 Ru2 C10 107.28(11) . . ? C2 Ru2 C11 89.30(11) . . ? C10 Ru2 C11 38.88(8) . . ? C2 Ru2 C19 105.99(12) . . ? C10 Ru2 C19 130.31(10) . . ? C11 Ru2 C19 107.06(10) . . ? C2 Ru2 C23 142.17(13) . . ? C10 Ru2 C23 100.34(10) . . ? C11 Ru2 C23 96.68(11) . . ? C19 Ru2 C23 36.67(12) . . ? C2 Ru2 C20 92.49(13) . . ? C10 Ru2 C20 160.02(11) . . ? C11 Ru2 C20 142.06(11) . . ? C19 Ru2 C20 36.56(12) . . ? C23 Ru2 C20 60.71(12) . . ? C2 Ru2 C22 150.20(14) . . ? C10 Ru2 C22 100.48(11) . . ? C11 Ru2 C22 119.67(14) . . ? C19 Ru2 C22 61.24(12) . . ? C23 Ru2 C22 36.48(14) . . ? C20 Ru2 C22 60.82(13) . . ? C2 Ru2 C21 113.69(15) . . ? C10 Ru2 C21 131.08(12) . . ? C11 Ru2 C21 155.85(13) . . ? C19 Ru2 C21 60.97(12) . . ? C23 Ru2 C21 60.82(14) . . ? C20 Ru2 C21 36.16(13) . . ? C22 Ru2 C21 36.70(15) . . ? C2 Ru2 Ru1 86.07(9) . . ? C10 Ru2 Ru1 47.07(6) . . ? C11 Ru2 Ru1 77.56(6) . . ? C19 Ru2 Ru1 166.93(8) . . ? C23 Ru2 Ru1 131.72(10) . . ? C20 Ru2 Ru1 140.38(9) . . ? C22 Ru2 Ru1 105.75(9) . . ? C21 Ru2 Ru1 109.92(9) . . ? C12 O5 C13 116.5(2) . . ? O1 C1 Ru1 169.5(2) . . ? O2 C2 Ru2 173.2(3) . . ? O3 C3 C4 121.0(2) . . ? O3 C3 Ru1 124.4(2) . . ? C4 C3 Ru1 114.57(16) . . ? C9 C4 C5 121.7(2) . . ? C9 C4 C3 115.2(2) . . ? C5 C4 C3 123.1(2) . . ? C6 C5 C4 119.1(2) . . ? C7 C6 C5 119.9(2) . . ? C6 C7 C8 121.3(2) . . ? C7 C8 C9 119.7(2) . . ? C4 C9 C8 118.3(2) . . ? C4 C9 C10 115.2(2) . . ? C8 C9 C10 126.5(2) . . ? C11 C10 C9 116.96(19) . . ? C11 C10 Ru1 128.75(16) . . ? C9 C10 Ru1 114.27(15) . . ? C11 C10 Ru2 73.26(13) . . ? C9 C10 Ru2 117.49(15) . . ? Ru1 C10 Ru2 84.61(8) . . ? C10 C11 C12 130.2(2) . . ? C10 C11 Ru2 67.86(12) . . ? C12 C11 Ru2 116.48(17) . . ? O4 C12 O5 120.9(2) . . ? O4 C12 C11 129.9(2) . . ? O5 C12 C11 109.1(2) . . ? C15 C14 C18 108.2(3) . . ? C15 C14 Ru1 70.20(17) . . ? C18 C14 Ru1 70.61(17) . . ? C14 C15 C16 108.4(3) . . ? C14 C15 Ru1 74.10(17) . . ? C16 C15 Ru1 70.02(15) . . ? C17 C16 C15 106.7(3) . . ? C17 C16 Ru1 71.88(15) . . ? C15 C16 Ru1 72.80(16) . . ? C18 C17 C16 108.6(3) . . ? C18 C17 Ru1 73.24(17) . . ? C16 C17 Ru1 71.14(16) . . ? C14 C18 C17 108.0(3) . . ? C14 C18 Ru1 73.62(18) . . ? C17 C18 Ru1 70.29(16) . . ? C23 C19 C20 107.5(3) . . ? C23 C19 Ru2 71.77(16) . . ? C20 C19 Ru2 72.39(16) . . ? C21 C20 C19 108.8(3) . . ? C21 C20 Ru2 72.54(17) . . ? C19 C20 Ru2 71.05(16) . . ? C20 C21 C22 107.7(3) . . ? C20 C21 Ru2 71.29(17) . . ? C22 C21 Ru2 71.36(17) . . ? C23 C22 C21 107.2(3) . . ? C23 C22 Ru2 70.87(17) . . ? C21 C22 Ru2 71.94(18) . . ? C19 C23 C22 108.9(3) . . ? C19 C23 Ru2 71.56(16) . . ? C22 C23 Ru2 72.65(18) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.411 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.068 data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H24 Cl2 O5 Ru3' _chemical_formula_weight 826.59 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2578(19) _cell_length_b 10.657(2) _cell_length_c 15.409(3) _cell_angle_alpha 71.22(3) _cell_angle_beta 81.21(3) _cell_angle_gamma 82.32(3) _cell_volume 1416.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 14.8 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.805 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.609 _exptl_absorpt_correction_T_max 0.686 _exptl_absorpt_process_details ; Parameters determined using XEMP (Siemens AXS Inc.) software with 407 Psi-scan data and an elipsoidal model of crystal shape. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3/mV' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5321 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4984 _reflns_number_gt 4299 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+5.1799P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4984 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru -0.14985(4) -0.21359(4) 0.66194(3) 0.02869(12) Uani 1 1 d . . . Ru2 Ru -0.40279(4) -0.22062(4) 0.78544(3) 0.02928(12) Uani 1 1 d . . . Ru3 Ru -0.18245(5) -0.23674(4) 0.89616(3) 0.03189(13) Uani 1 1 d . . . O1 O -0.2027(6) -0.1062(6) 0.4612(3) 0.0716(15) Uani 1 1 d . . . O2 O -0.3341(6) -0.4378(5) 0.6842(3) 0.0615(13) Uani 1 1 d . . . O3 O -0.2904(5) -0.4962(4) 0.9120(3) 0.0544(11) Uani 1 1 d . . . O4 O -0.4632(5) 0.0730(5) 0.8531(4) 0.0590(12) Uani 1 1 d . . . O5 O -0.2278(5) 0.1134(4) 0.8350(3) 0.0470(10) Uani 1 1 d . . . C1 C -0.1891(7) -0.1461(6) 0.5389(4) 0.0425(14) Uani 1 1 d . . . C2 C -0.2952(7) -0.3440(6) 0.6926(4) 0.0412(13) Uani 1 1 d . . . C3 C -0.2716(7) -0.3829(6) 0.8878(4) 0.0388(13) Uani 1 1 d . . . C4 C -0.2727(5) -0.0599(5) 0.7045(3) 0.0275(10) Uani 1 1 d . . . C5 C -0.3143(6) 0.0702(5) 0.6365(3) 0.0318(11) Uani 1 1 d . . . C6 C -0.4226(6) 0.0867(6) 0.5793(4) 0.0445(14) Uani 1 1 d . . . H6A H -0.4708 0.0138 0.5825 0.053 Uiso 1 1 calc R . . C7 C -0.4594(8) 0.2082(8) 0.5184(4) 0.060(2) Uani 1 1 d . . . H7A H -0.5329 0.2172 0.4813 0.072 Uiso 1 1 calc R . . C8 C -0.3887(10) 0.3175(7) 0.5115(5) 0.068(2) Uani 1 1 d . . . H8A H -0.4154 0.4003 0.4708 0.082 Uiso 1 1 calc R . . C9 C -0.2789(10) 0.3031(7) 0.5651(5) 0.065(2) Uani 1 1 d . . . H9A H -0.2299 0.3762 0.5604 0.078 Uiso 1 1 calc R . . C10 C -0.2405(8) 0.1801(6) 0.6264(4) 0.0499(16) Uani 1 1 d . . . H10A H -0.1641 0.1709 0.6613 0.060 Uiso 1 1 calc R . . C11 C -0.2741(6) -0.0746(5) 0.7992(4) 0.0295(11) Uani 1 1 d . . . C12 C -0.3359(6) 0.0425(6) 0.8320(4) 0.0367(12) Uani 1 1 d . . . C13 C -0.2715(10) 0.2343(7) 0.8587(6) 0.068(2) Uani 1 1 d . . . H13A H -0.1858 0.2761 0.8587 0.081 Uiso 1 1 calc R . . H13B H -0.3263 0.2138 0.9190 0.081 Uiso 1 1 calc R . . H13C H -0.3316 0.2936 0.8143 0.081 Uiso 1 1 calc R . . C14 C -0.0337(6) -0.2560(6) 0.7852(4) 0.0350(12) Uani 1 1 d . . . C15 C 0.0324(6) -0.1493(6) 0.7119(4) 0.0386(13) Uani 1 1 d . . . H15A H 0.0372 -0.0595 0.7150 0.046 Uiso 1 1 calc R . . C16 C 0.0912(6) -0.1944(7) 0.6356(4) 0.0450(15) Uani 1 1 d . . . H16A H 0.1441 -0.1419 0.5781 0.054(19) Uiso 1 1 calc R . . C17 C 0.0713(6) -0.3321(7) 0.6603(4) 0.0464(15) Uani 1 1 d . . . H17A H 0.1069 -0.3913 0.6228 0.056 Uiso 1 1 calc R . . C18 C -0.0018(6) -0.3691(6) 0.7511(4) 0.0438(14) Uani 1 1 d . . . H18A H -0.0270 -0.4595 0.7862 0.053 Uiso 1 1 calc R . . C19 C -0.6021(7) -0.2493(11) 0.7359(6) 0.077(3) Uani 1 1 d . . . H19A H -0.6083 -0.2579 0.6752 0.092 Uiso 1 1 calc R . . C20 C -0.5802(8) -0.3533(8) 0.8155(6) 0.067(2) Uani 1 1 d . . . H20A H -0.5669 -0.4480 0.8204 0.081 Uiso 1 1 calc R . . C21 C -0.5897(7) -0.3022(8) 0.8875(5) 0.062(2) Uani 1 1 d . . . H21A H -0.5828 -0.3549 0.9521 0.074 Uiso 1 1 calc R . . C22 C -0.6164(7) -0.1641(8) 0.8550(5) 0.0576(18) Uani 1 1 d . . . H22A H -0.6343 -0.1033 0.8924 0.069 Uiso 1 1 calc R . . C23 C -0.6257(7) -0.1296(9) 0.7589(6) 0.068(2) Uani 1 1 d . . . H23A H -0.6519 -0.0407 0.7175 0.082 Uiso 1 1 calc R . . C24 C -0.2216(10) -0.1458(9) 1.0125(5) 0.072(3) Uani 1 1 d . . . H24A H -0.2897 -0.0678 1.0147 0.086 Uiso 1 1 calc R . . C25 C -0.2535(10) -0.2763(10) 1.0504(5) 0.072(2) Uani 1 1 d . . . H25A H -0.3478 -0.3067 1.0833 0.086 Uiso 1 1 calc R . . C26 C -0.1246(11) -0.3581(8) 1.0390(5) 0.070(2) Uani 1 1 d . . . H26A H -0.1142 -0.4555 1.0630 0.083 Uiso 1 1 calc R . . C27 C -0.0138(9) -0.2795(9) 0.9931(5) 0.067(2) Uani 1 1 d . . . H27A H 0.0896 -0.3107 0.9810 0.080 Uiso 1 1 calc R . . C28 C -0.0729(11) -0.1428(8) 0.9748(5) 0.071(2) Uani 1 1 d . . . H28A H -0.0177 -0.0641 0.9494 0.085 Uiso 1 1 calc R . . Cl1 Cl 0.3434(5) 0.3926(3) 0.7076(2) 0.1303(12) Uani 1 1 d . . . Cl2 Cl 0.1060(4) 0.2161(7) 0.7488(4) 0.215(3) Uani 1 1 d . . . C29 C 0.2823(12) 0.2454(11) 0.7170(8) 0.104(3) Uani 1 1 d . . . H29A H 0.3092 0.2307 0.6574 0.124 Uiso 1 1 calc R . . H29B H 0.3386 0.1770 0.7603 0.124 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0266(2) 0.0332(2) 0.0272(2) -0.01139(17) -0.00089(16) -0.00339(17) Ru2 0.0249(2) 0.0340(2) 0.0282(2) -0.00754(17) -0.00147(16) -0.00718(17) Ru3 0.0335(2) 0.0365(2) 0.0263(2) -0.01066(18) -0.00855(17) 0.00316(18) O1 0.090(4) 0.091(4) 0.031(3) -0.012(2) -0.007(2) -0.017(3) O2 0.075(3) 0.052(3) 0.068(3) -0.031(2) 0.006(3) -0.030(3) O3 0.074(3) 0.037(2) 0.046(2) -0.002(2) -0.009(2) -0.007(2) O4 0.045(3) 0.059(3) 0.075(3) -0.035(3) 0.005(2) 0.007(2) O5 0.053(3) 0.042(2) 0.056(3) -0.028(2) -0.009(2) -0.003(2) C1 0.040(3) 0.050(3) 0.038(3) -0.015(3) 0.001(3) -0.010(3) C2 0.044(3) 0.041(3) 0.039(3) -0.013(3) -0.004(3) -0.006(3) C3 0.043(3) 0.040(3) 0.029(3) -0.008(2) -0.004(2) 0.000(3) C4 0.025(3) 0.030(3) 0.030(3) -0.010(2) -0.005(2) -0.005(2) C5 0.031(3) 0.036(3) 0.027(3) -0.010(2) 0.000(2) -0.002(2) C6 0.036(3) 0.053(4) 0.037(3) -0.003(3) -0.006(2) -0.002(3) C7 0.047(4) 0.074(5) 0.037(3) 0.007(3) -0.005(3) 0.012(4) C8 0.089(6) 0.044(4) 0.043(4) 0.003(3) 0.017(4) 0.020(4) C9 0.107(7) 0.036(4) 0.045(4) -0.008(3) 0.007(4) -0.018(4) C10 0.069(4) 0.043(3) 0.040(3) -0.013(3) -0.003(3) -0.014(3) C11 0.029(3) 0.030(3) 0.031(3) -0.010(2) -0.007(2) -0.002(2) C12 0.043(3) 0.038(3) 0.029(3) -0.012(2) -0.009(2) 0.004(3) C13 0.094(6) 0.045(4) 0.076(5) -0.035(4) -0.013(4) -0.002(4) C14 0.026(3) 0.043(3) 0.038(3) -0.014(2) -0.010(2) 0.002(2) C15 0.023(3) 0.051(3) 0.046(3) -0.020(3) -0.005(2) -0.004(2) C16 0.022(3) 0.069(4) 0.041(3) -0.018(3) 0.005(2) -0.001(3) C17 0.034(3) 0.056(4) 0.049(4) -0.024(3) -0.002(3) 0.011(3) C18 0.036(3) 0.046(3) 0.046(3) -0.013(3) -0.007(3) 0.011(3) C19 0.023(3) 0.156(9) 0.075(6) -0.063(6) -0.003(3) -0.021(4) C20 0.051(4) 0.063(5) 0.091(6) -0.025(4) 0.010(4) -0.031(4) C21 0.039(4) 0.080(5) 0.055(4) -0.006(4) 0.012(3) -0.020(3) C22 0.032(3) 0.074(5) 0.072(5) -0.036(4) 0.017(3) -0.013(3) C23 0.019(3) 0.080(5) 0.077(5) 0.010(4) -0.001(3) -0.001(3) C24 0.093(6) 0.085(6) 0.045(4) -0.041(4) -0.028(4) 0.038(5) C25 0.076(6) 0.106(7) 0.026(3) -0.011(4) -0.008(3) -0.007(5) C26 0.114(7) 0.062(5) 0.035(4) -0.011(3) -0.034(4) 0.007(5) C27 0.057(5) 0.103(6) 0.053(4) -0.039(4) -0.037(4) 0.022(4) C28 0.105(7) 0.072(5) 0.054(4) -0.024(4) -0.041(5) -0.020(5) Cl1 0.188(4) 0.0882(19) 0.095(2) -0.0103(15) 0.007(2) -0.016(2) Cl2 0.097(3) 0.400(9) 0.243(5) -0.228(6) 0.013(3) -0.064(4) C29 0.104(8) 0.106(8) 0.106(8) -0.041(7) -0.006(6) -0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.873(6) . ? Ru1 C2 1.962(6) . ? Ru1 C4 2.090(5) . ? Ru1 C14 2.215(5) . ? Ru1 C15 2.226(5) . ? Ru1 C16 2.231(6) . ? Ru1 C18 2.239(6) . ? Ru1 C17 2.259(6) . ? Ru1 Ru2 2.7754(11) . ? Ru2 C4 2.158(5) . ? Ru2 C11 2.162(5) . ? Ru2 C19 2.193(6) . ? Ru2 C23 2.199(6) . ? Ru2 C22 2.207(6) . ? Ru2 C20 2.209(7) . ? Ru2 C21 2.216(6) . ? Ru2 C2 2.279(6) . ? Ru2 C3 2.285(6) . ? Ru2 Ru3 2.8076(10) . ? Ru3 C3 1.905(6) . ? Ru3 C11 2.067(5) . ? Ru3 C14 2.072(6) . ? Ru3 C28 2.220(7) . ? Ru3 C27 2.227(6) . ? Ru3 C24 2.261(7) . ? Ru3 C26 2.269(7) . ? Ru3 C25 2.282(7) . ? O1 C1 1.154(7) . ? O2 C2 1.157(7) . ? O3 C3 1.173(7) . ? O4 C12 1.204(7) . ? O5 C12 1.346(7) . ? O5 C13 1.442(7) . ? C4 C11 1.416(7) . ? C4 C5 1.488(7) . ? C5 C10 1.388(8) . ? C5 C6 1.392(8) . ? C6 C7 1.368(9) . ? C7 C8 1.378(12) . ? C8 C9 1.369(12) . ? C9 C10 1.385(10) . ? C11 C12 1.505(7) . ? C14 C18 1.443(8) . ? C14 C15 1.445(8) . ? C15 C16 1.417(8) . ? C16 C17 1.423(9) . ? C17 C18 1.413(9) . ? C19 C20 1.384(12) . ? C19 C23 1.411(12) . ? C20 C21 1.370(11) . ? C21 C22 1.395(11) . ? C22 C23 1.419(11) . ? C24 C25 1.376(12) . ? C24 C28 1.410(12) . ? C25 C26 1.404(12) . ? C26 C27 1.372(12) . ? C27 C28 1.439(11) . ? Cl1 C29 1.694(11) . ? Cl2 C29 1.672(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 92.3(3) . . ? C1 Ru1 C4 95.8(2) . . ? C2 Ru1 C4 101.0(2) . . ? C1 Ru1 C14 159.8(2) . . ? C2 Ru1 C14 107.0(2) . . ? C4 Ru1 C14 86.7(2) . . ? C1 Ru1 C15 122.2(2) . . ? C2 Ru1 C15 144.9(2) . . ? C4 Ru1 C15 83.1(2) . . ? C14 Ru1 C15 38.0(2) . . ? C1 Ru1 C16 97.3(2) . . ? C2 Ru1 C16 142.5(2) . . ? C4 Ru1 C16 113.9(2) . . ? C14 Ru1 C16 63.6(2) . . ? C15 Ru1 C16 37.1(2) . . ? C1 Ru1 C18 140.3(2) . . ? C2 Ru1 C18 88.7(2) . . ? C4 Ru1 C18 123.0(2) . . ? C14 Ru1 C18 37.8(2) . . ? C15 Ru1 C18 61.3(2) . . ? C16 Ru1 C18 61.3(2) . . ? C1 Ru1 C17 106.1(3) . . ? C2 Ru1 C17 105.6(3) . . ? C4 Ru1 C17 144.5(2) . . ? C14 Ru1 C17 63.4(2) . . ? C15 Ru1 C17 61.7(2) . . ? C16 Ru1 C17 36.9(2) . . ? C18 Ru1 C17 36.6(2) . . ? C1 Ru1 Ru2 112.31(19) . . ? C2 Ru1 Ru2 54.28(18) . . ? C4 Ru1 Ru2 50.27(14) . . ? C14 Ru1 Ru2 84.68(14) . . ? C15 Ru1 Ru2 110.37(15) . . ? C16 Ru1 Ru2 146.59(16) . . ? C18 Ru1 Ru2 100.27(16) . . ? C17 Ru1 Ru2 136.43(17) . . ? C4 Ru2 C11 38.28(19) . . ? C4 Ru2 C19 119.8(3) . . ? C11 Ru2 C19 144.7(3) . . ? C4 Ru2 C23 101.3(2) . . ? C11 Ru2 C23 109.6(3) . . ? C19 Ru2 C23 37.5(3) . . ? C4 Ru2 C22 116.4(2) . . ? C11 Ru2 C22 99.6(2) . . ? C19 Ru2 C22 62.3(3) . . ? C23 Ru2 C22 37.6(3) . . ? C4 Ru2 C20 156.2(3) . . ? C11 Ru2 C20 159.1(3) . . ? C19 Ru2 C20 36.6(3) . . ? C23 Ru2 C20 61.8(3) . . ? C22 Ru2 C20 61.5(3) . . ? C4 Ru2 C21 152.3(3) . . ? C11 Ru2 C21 123.2(3) . . ? C19 Ru2 C21 60.9(3) . . ? C23 Ru2 C21 61.6(3) . . ? C22 Ru2 C21 36.8(3) . . ? C20 Ru2 C21 36.1(3) . . ? C4 Ru2 C2 89.6(2) . . ? C11 Ru2 C2 116.5(2) . . ? C19 Ru2 C2 82.1(3) . . ? C23 Ru2 C2 115.3(3) . . ? C22 Ru2 C2 142.7(2) . . ? C20 Ru2 C2 83.8(3) . . ? C21 Ru2 C2 116.9(3) . . ? C4 Ru2 C3 112.0(2) . . ? C11 Ru2 C3 89.2(2) . . ? C19 Ru2 C3 124.7(3) . . ? C23 Ru2 C3 143.7(2) . . ? C22 Ru2 C3 110.5(3) . . ? C20 Ru2 C3 89.5(3) . . ? C21 Ru2 C3 82.1(3) . . ? C2 Ru2 C3 80.2(2) . . ? C4 Ru2 Ru1 48.16(13) . . ? C11 Ru2 Ru1 72.72(14) . . ? C19 Ru2 Ru1 115.0(2) . . ? C23 Ru2 Ru1 129.1(2) . . ? C22 Ru2 Ru1 162.4(2) . . ? C20 Ru2 Ru1 128.0(2) . . ? C21 Ru2 Ru1 159.5(2) . . ? C2 Ru2 Ru1 44.34(15) . . ? C3 Ru2 Ru1 85.55(15) . . ? C4 Ru2 Ru3 76.58(13) . . ? C11 Ru2 Ru3 46.96(14) . . ? C19 Ru2 Ru3 163.3(3) . . ? C23 Ru2 Ru3 142.1(3) . . ? C22 Ru2 Ru3 108.9(2) . . ? C20 Ru2 Ru3 127.2(2) . . ? C21 Ru2 Ru3 103.2(2) . . ? C2 Ru2 Ru3 102.60(16) . . ? C3 Ru2 Ru3 42.40(16) . . ? Ru1 Ru2 Ru3 77.79(2) . . ? C3 Ru3 C11 103.7(2) . . ? C3 Ru3 C14 87.2(2) . . ? C11 Ru3 C14 84.3(2) . . ? C3 Ru3 C28 150.9(3) . . ? C11 Ru3 C28 102.8(3) . . ? C14 Ru3 C28 107.3(3) . . ? C3 Ru3 C27 118.1(3) . . ? C11 Ru3 C27 138.2(3) . . ? C14 Ru3 C27 94.7(3) . . ? C28 Ru3 C27 37.8(3) . . ? C3 Ru3 C24 127.6(3) . . ? C11 Ru3 C24 96.3(2) . . ? C14 Ru3 C24 143.3(3) . . ? C28 Ru3 C24 36.7(3) . . ? C27 Ru3 C24 61.0(3) . . ? C3 Ru3 C26 90.2(3) . . ? C11 Ru3 C26 155.6(3) . . ? C14 Ru3 C26 116.9(3) . . ? C28 Ru3 C26 60.8(3) . . ? C27 Ru3 C26 35.5(3) . . ? C24 Ru3 C26 59.6(3) . . ? C3 Ru3 C25 95.1(3) . . ? C11 Ru3 C25 121.4(3) . . ? C14 Ru3 C25 152.5(3) . . ? C28 Ru3 C25 60.5(3) . . ? C27 Ru3 C25 60.1(3) . . ? C24 Ru3 C25 35.3(3) . . ? C26 Ru3 C25 35.9(3) . . ? C3 Ru3 Ru2 53.97(17) . . ? C11 Ru3 Ru2 49.86(14) . . ? C14 Ru3 Ru2 86.52(14) . . ? C28 Ru3 Ru2 149.0(2) . . ? C27 Ru3 Ru2 171.9(3) . . ? C24 Ru3 Ru2 121.6(2) . . ? C26 Ru3 Ru2 137.5(3) . . ? C25 Ru3 Ru2 116.8(2) . . ? C12 O5 C13 116.9(5) . . ? O1 C1 Ru1 175.1(6) . . ? O2 C2 Ru1 150.0(5) . . ? O2 C2 Ru2 128.6(5) . . ? Ru1 C2 Ru2 81.4(2) . . ? O3 C3 Ru3 151.6(5) . . ? O3 C3 Ru2 124.5(5) . . ? Ru3 C3 Ru2 83.6(2) . . ? C11 C4 C5 121.9(4) . . ? C11 C4 Ru1 114.3(4) . . ? C5 C4 Ru1 121.2(3) . . ? C11 C4 Ru2 71.0(3) . . ? C5 C4 Ru2 130.8(4) . . ? Ru1 C4 Ru2 81.57(17) . . ? C10 C5 C6 117.6(5) . . ? C10 C5 C4 119.8(5) . . ? C6 C5 C4 122.6(5) . . ? C7 C6 C5 121.1(6) . . ? C6 C7 C8 120.7(7) . . ? C9 C8 C7 119.3(6) . . ? C8 C9 C10 120.2(7) . . ? C9 C10 C5 121.1(7) . . ? C4 C11 C12 117.7(4) . . ? C4 C11 Ru3 126.1(4) . . ? C12 C11 Ru3 115.9(4) . . ? C4 C11 Ru2 70.7(3) . . ? C12 C11 Ru2 124.9(4) . . ? Ru3 C11 Ru2 83.18(18) . . ? O4 C12 O5 122.4(5) . . ? O4 C12 C11 126.8(5) . . ? O5 C12 C11 110.7(5) . . ? C18 C14 C15 104.0(5) . . ? C18 C14 Ru3 127.8(4) . . ? C15 C14 Ru3 126.5(4) . . ? C18 C14 Ru1 72.0(3) . . ? C15 C14 Ru1 71.4(3) . . ? Ru3 C14 Ru1 109.7(2) . . ? C16 C15 C14 109.9(5) . . ? C16 C15 Ru1 71.7(3) . . ? C14 C15 Ru1 70.6(3) . . ? C15 C16 C17 108.1(5) . . ? C15 C16 Ru1 71.2(3) . . ? C17 C16 Ru1 72.6(3) . . ? C18 C17 C16 107.1(5) . . ? C18 C17 Ru1 70.9(3) . . ? C16 C17 Ru1 70.5(3) . . ? C17 C18 C14 110.8(6) . . ? C17 C18 Ru1 72.5(3) . . ? C14 C18 Ru1 70.2(3) . . ? C20 C19 C23 108.2(7) . . ? C20 C19 Ru2 72.3(4) . . ? C23 C19 Ru2 71.5(4) . . ? C21 C20 C19 108.6(8) . . ? C21 C20 Ru2 72.3(4) . . ? C19 C20 Ru2 71.1(4) . . ? C20 C21 C22 109.4(7) . . ? C20 C21 Ru2 71.7(4) . . ? C22 C21 Ru2 71.3(4) . . ? C21 C22 C23 106.9(7) . . ? C21 C22 Ru2 72.0(4) . . ? C23 C22 Ru2 70.9(4) . . ? C19 C23 C22 106.9(7) . . ? C19 C23 Ru2 71.0(4) . . ? C22 C23 Ru2 71.5(4) . . ? C25 C24 C28 109.0(7) . . ? C25 C24 Ru3 73.2(4) . . ? C28 C24 Ru3 70.1(4) . . ? C24 C25 C26 108.1(8) . . ? C24 C25 Ru3 71.5(4) . . ? C26 C25 Ru3 71.5(4) . . ? C27 C26 C25 109.0(8) . . ? C27 C26 Ru3 70.6(4) . . ? C25 C26 Ru3 72.5(4) . . ? C26 C27 C28 107.8(7) . . ? C26 C27 Ru3 73.9(4) . . ? C28 C27 Ru3 70.8(4) . . ? C24 C28 C27 106.1(8) . . ? C24 C28 Ru3 73.2(4) . . ? C27 C28 Ru3 71.4(4) . . ? Cl2 C29 Cl1 122.2(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.275 _refine_diff_density_min -1.451 _refine_diff_density_rms 0.115