# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2246 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 Dalton Transactions ; _publ_requested_journal 'NAME OF JOURNAL' # TITLE AND AUTHOR LIST _publ_section_title ; Reactivity of multi-site bound allenylidene towards alkynes and silica gel' ; loop_ _publ_author_name _publ_author_address 'Jonathan P. H. Charmant' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; 'Philip J. King' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; 'Roberto Quesada-Pato' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; 'Enrico Sappa' ; Dipartimento di Chimica Universit\`a di Torino Via P. Giuria Torino I-10125 Italy ; 'Carsten Schaefer' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; ######################################################################### data_5a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H16 O9 Ru3' _chemical_formula_weight 799.62 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2442(12) _cell_length_b 10.6111(13) _cell_length_c 14.171(2) _cell_angle_alpha 82.234(12) _cell_angle_beta 84.141(9) _cell_angle_gamma 78.161(14) _cell_volume 1344.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 203 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.976 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 1.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.723 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details ; G. M. Sheldrick. SADABS: A program for absorption correction with the Siemens SMART system; University of G\"ottingen: Germany, 1996. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 10016 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4668 _reflns_number_gt 3783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0153P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00095(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4668 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0478 _refine_ls_wR_factor_gt 0.0461 _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_restrained_S_all 0.894 _refine_ls_shift/su_max 0.000 _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 0.81506(3) 0.02234(2) 0.35041(2) 0.01723(8) Uani 1 1 d . . . Ru2 Ru 0.77151(3) 0.03714(3) 0.16238(2) 0.01837(8) Uani 1 1 d . . . Ru3 Ru 0.42017(3) 0.31826(3) 0.20243(2) 0.01833(8) Uani 1 1 d . . . C1 C 0.9494(4) -0.1383(3) 0.3910(3) 0.0277(9) Uani 1 1 d . . . C2 C 0.7050(4) 0.0455(3) 0.4683(3) 0.0275(9) Uani 1 1 d . . . C3 C 0.9709(4) 0.1142(3) 0.3677(3) 0.0244(9) Uani 1 1 d . . . C4 C 0.7332(4) -0.0579(4) 0.0653(3) 0.0295(9) Uani 1 1 d . . . C5 C 0.8369(4) 0.1683(4) 0.0695(3) 0.0296(9) Uani 1 1 d . . . C6 C 0.9700(5) -0.0513(4) 0.1789(3) 0.0316(9) Uani 1 1 d . . . C7 C 0.4850(4) 0.3101(4) 0.0726(3) 0.0290(9) Uani 1 1 d . . . C8 C 0.2368(4) 0.2623(3) 0.1856(2) 0.0240(8) Uani 1 1 d . . . C9 C 0.3351(4) 0.5063(4) 0.1844(3) 0.0285(9) Uani 1 1 d . . . C10 C 0.6832(4) -0.2219(3) 0.3114(3) 0.0310(9) Uani 1 1 d . . . H10A H 0.6527 -0.2527 0.2558 0.047 Uiso 1 1 calc R . . H10B H 0.6168 -0.2414 0.3675 0.047 Uiso 1 1 calc R . . H10C H 0.7851 -0.2656 0.3231 0.047 Uiso 1 1 calc R . . C11 C 0.6757(4) -0.0774(3) 0.2925(2) 0.0195(8) Uani 1 1 d . . . C12 C 0.5542(4) -0.0010(3) 0.2453(2) 0.0189(8) Uani 1 1 d . . . C13 C 0.4307(4) -0.0532(3) 0.2098(3) 0.0302(9) Uani 1 1 d . . . H13A H 0.3553 -0.0646 0.2624 0.045 Uiso 1 1 calc R . . H13B H 0.4717 -0.1369 0.1862 0.045 Uiso 1 1 calc R . . H13C H 0.3856 0.0082 0.1579 0.045 Uiso 1 1 calc R . . C14 C 0.5527(4) 0.1352(3) 0.2357(2) 0.0171(8) Uani 1 1 d . . . C15 C 0.6743(4) 0.1703(3) 0.2717(2) 0.0169(8) Uani 1 1 d . . . C16 C 0.6345(4) 0.3178(3) 0.2663(2) 0.0169(8) Uani 1 1 d . . . C17 C 0.5185(4) 0.3672(3) 0.3358(2) 0.0164(7) Uani 1 1 d . . . C18 C 0.4045(4) 0.2959(3) 0.3731(2) 0.0190(8) Uani 1 1 d . . . H18 H 0.4138 0.2085 0.3611 0.023 Uiso 1 1 calc R . . C19 C 0.2784(4) 0.3556(3) 0.4277(2) 0.0226(8) Uani 1 1 d . . . H19 H 0.2040 0.3074 0.4520 0.027 Uiso 1 1 calc R . . C20 C 0.2616(4) 0.4800(3) 0.4459(3) 0.0284(9) Uani 1 1 d . . . H20 H 0.1756 0.5189 0.4819 0.034 Uiso 1 1 calc R . . C21 C 0.3736(4) 0.5515(3) 0.4109(3) 0.0271(9) Uani 1 1 d . . . H21 H 0.3628 0.6382 0.4250 0.033 Uiso 1 1 calc R . . C22 C 0.4954(4) 0.4988(3) 0.3580(3) 0.0237(8) Uani 1 1 d . . . H22 H 0.5677 0.5498 0.3348 0.028 Uiso 1 1 calc R . . C23 C 0.7479(4) 0.4011(3) 0.2296(2) 0.0180(8) Uani 1 1 d . . . C24 C 0.8502(4) 0.4174(3) 0.2903(3) 0.0222(8) Uani 1 1 d . . . H24 H 0.8514 0.3728 0.3531 0.027 Uiso 1 1 calc R . . C25 C 0.9508(4) 0.4983(3) 0.2598(3) 0.0305(10) Uani 1 1 d . . . H25 H 1.0200 0.5088 0.3019 0.037 Uiso 1 1 calc R . . C26 C 0.9505(4) 0.5631(3) 0.1689(3) 0.0356(11) Uani 1 1 d . . . H26 H 1.0198 0.6179 0.1482 0.043 Uiso 1 1 calc R . . C27 C 0.8501(4) 0.5485(3) 0.1083(3) 0.0343(10) Uani 1 1 d . . . H27 H 0.8497 0.5934 0.0455 0.041 Uiso 1 1 calc R . . C28 C 0.7489(4) 0.4680(3) 0.1385(3) 0.0280(9) Uani 1 1 d . . . H28 H 0.6795 0.4587 0.0962 0.034 Uiso 1 1 calc R . . O1 O 1.0293(3) -0.2312(3) 0.4137(2) 0.0487(8) Uani 1 1 d . . . O2 O 0.6363(3) 0.0600(3) 0.53895(19) 0.0460(8) Uani 1 1 d . . . O3 O 1.0712(3) 0.1557(3) 0.37983(19) 0.0394(7) Uani 1 1 d . . . O4 O 0.7095(4) -0.1167(3) 0.0094(2) 0.0552(9) Uani 1 1 d . . . O5 O 0.8828(3) 0.2396(3) 0.0134(2) 0.0456(8) Uani 1 1 d . . . O6 O 1.0913(3) -0.1045(3) 0.1751(2) 0.0495(8) Uani 1 1 d . . . O7 O 0.5193(3) 0.3047(3) -0.0066(2) 0.0459(8) Uani 1 1 d . . . O8 O 0.1343(3) 0.2275(3) 0.17068(19) 0.0374(7) Uani 1 1 d . . . O9 O 0.2915(3) 0.6143(2) 0.1738(2) 0.0443(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02011(17) 0.01445(15) 0.01626(16) 0.00071(12) -0.00279(12) -0.00228(12) Ru2 0.02117(17) 0.01879(15) 0.01563(16) -0.00318(12) -0.00026(12) -0.00477(12) Ru3 0.01653(17) 0.01986(15) 0.01763(17) 0.00305(12) -0.00284(12) -0.00394(12) C1 0.031(2) 0.026(2) 0.026(2) -0.0028(18) -0.0017(18) -0.0041(18) C2 0.027(2) 0.025(2) 0.029(2) -0.0024(18) -0.0069(19) -0.0004(17) C3 0.031(2) 0.0200(19) 0.020(2) 0.0071(16) -0.0071(17) -0.0033(17) C4 0.033(2) 0.032(2) 0.025(2) -0.0057(19) -0.0006(18) -0.0071(18) C5 0.035(2) 0.032(2) 0.021(2) -0.0089(19) 0.0015(18) -0.0031(19) C6 0.033(3) 0.038(2) 0.022(2) -0.0015(19) 0.0010(19) -0.006(2) C7 0.017(2) 0.038(2) 0.031(3) 0.002(2) -0.0060(18) -0.0054(17) C8 0.026(2) 0.025(2) 0.017(2) -0.0040(16) 0.0002(17) 0.0046(17) C9 0.018(2) 0.038(2) 0.027(2) 0.0054(19) -0.0009(17) -0.0079(18) C10 0.035(2) 0.0181(19) 0.040(3) -0.0029(18) -0.0032(19) -0.0058(17) C11 0.023(2) 0.0161(17) 0.022(2) -0.0049(16) 0.0023(16) -0.0084(15) C12 0.020(2) 0.0214(18) 0.0172(19) -0.0051(15) 0.0033(15) -0.0080(15) C13 0.029(2) 0.029(2) 0.038(2) -0.0084(19) -0.0049(19) -0.0140(18) C14 0.0177(19) 0.0206(18) 0.0141(19) -0.0024(15) -0.0023(15) -0.0055(15) C15 0.0188(19) 0.0168(17) 0.0141(19) 0.0023(15) 0.0030(15) -0.0057(15) C16 0.0170(19) 0.0166(17) 0.0177(19) 0.0010(15) -0.0054(15) -0.0049(14) C17 0.0208(19) 0.0138(17) 0.0156(19) 0.0009(15) -0.0034(15) -0.0063(14) C18 0.026(2) 0.0177(18) 0.016(2) -0.0024(15) -0.0037(16) -0.0089(15) C19 0.021(2) 0.029(2) 0.019(2) -0.0014(17) 0.0000(16) -0.0102(16) C20 0.020(2) 0.035(2) 0.030(2) -0.0100(18) 0.0001(17) -0.0014(17) C21 0.029(2) 0.0168(18) 0.037(2) -0.0088(17) -0.0026(18) -0.0031(16) C22 0.025(2) 0.0132(17) 0.033(2) 0.0007(16) -0.0025(17) -0.0052(15) C23 0.0156(19) 0.0111(17) 0.026(2) 0.0013(15) 0.0026(16) -0.0030(14) C24 0.020(2) 0.0140(17) 0.030(2) 0.0032(16) -0.0007(17) -0.0037(15) C25 0.019(2) 0.022(2) 0.051(3) -0.008(2) -0.0027(19) -0.0044(16) C26 0.017(2) 0.021(2) 0.065(3) 0.002(2) 0.009(2) -0.0075(16) C27 0.032(2) 0.027(2) 0.039(3) 0.0110(19) 0.007(2) -0.0091(18) C28 0.025(2) 0.024(2) 0.033(2) 0.0039(18) 0.0005(18) -0.0071(17) O1 0.048(2) 0.0315(16) 0.056(2) 0.0062(15) -0.0094(16) 0.0141(15) O2 0.0463(19) 0.062(2) 0.0236(17) -0.0056(15) 0.0088(15) -0.0027(16) O3 0.0382(18) 0.0438(17) 0.0417(18) 0.0047(14) -0.0183(14) -0.0199(14) O4 0.076(2) 0.067(2) 0.0350(19) -0.0255(17) -0.0064(16) -0.0277(18) O5 0.062(2) 0.0430(17) 0.0312(17) 0.0046(15) 0.0153(15) -0.0229(16) O6 0.0270(18) 0.074(2) 0.0421(19) -0.0175(17) -0.0006(14) 0.0076(16) O7 0.0384(18) 0.078(2) 0.0196(17) 0.0029(16) -0.0006(14) -0.0147(16) O8 0.0249(16) 0.0500(17) 0.0434(18) -0.0182(15) -0.0026(13) -0.0130(13) O9 0.0356(17) 0.0246(16) 0.064(2) 0.0144(15) -0.0054(15) 0.0015(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 C2 1.883(4) . ? Ru1 C1 1.947(4) . ? Ru1 C3 1.949(4) . ? Ru1 C15 2.095(3) . ? Ru1 C11 2.113(3) . ? Ru1 Ru2 2.7140(6) . ? Ru1 C6 2.813(4) . ? Ru2 C6 1.904(4) . ? Ru2 C4 1.912(4) . ? Ru2 C5 1.930(4) . ? Ru2 C15 2.233(3) . ? Ru2 C11 2.273(3) . ? Ru2 C14 2.292(3) . ? Ru2 C12 2.303(3) . ? Ru3 C7 1.884(4) . ? Ru3 C8 1.953(4) . ? Ru3 C9 1.981(4) . ? Ru3 C14 2.095(3) . ? Ru3 C16 2.260(3) . ? Ru3 C17 2.341(3) . ? Ru3 C18 2.390(3) . ? C1 O1 1.134(4) . ? C2 O2 1.141(4) . ? C3 O3 1.142(4) . ? C4 O4 1.135(4) . ? C5 O5 1.133(4) . ? C6 O6 1.147(4) . ? C7 O7 1.141(4) . ? C8 O8 1.134(4) . ? C9 O9 1.129(4) . ? C10 C11 1.509(4) . ? C11 C12 1.414(5) . ? C12 C14 1.430(4) . ? C12 C13 1.522(4) . ? C14 C15 1.415(4) . ? C15 C16 1.526(4) . ? C16 C17 1.445(4) . ? C16 C23 1.515(4) . ? C17 C18 1.439(4) . ? C17 C22 1.441(4) . ? C18 C19 1.415(4) . ? C19 C20 1.354(5) . ? C20 C21 1.418(5) . ? C21 C22 1.351(5) . ? C23 C28 1.387(5) . ? C23 C24 1.391(5) . ? C24 C25 1.390(4) . ? C25 C26 1.376(5) . ? C26 C27 1.372(5) . ? C27 C28 1.391(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 C2 Ru1 C1 98.07(16) . . ? C2 Ru1 C3 97.82(15) . . ? C1 Ru1 C3 87.78(15) . . ? C2 Ru1 C15 94.91(14) . . ? C1 Ru1 C15 163.87(14) . . ? C3 Ru1 C15 99.94(13) . . ? C2 Ru1 C11 98.14(14) . . ? C1 Ru1 C11 92.22(14) . . ? C3 Ru1 C11 163.88(14) . . ? C15 Ru1 C11 76.43(13) . . ? C2 Ru1 Ru2 139.74(11) . . ? C1 Ru1 Ru2 110.56(11) . . ? C3 Ru1 Ru2 110.60(10) . . ? C15 Ru1 Ru2 53.48(9) . . ? C11 Ru1 Ru2 54.48(9) . . ? C2 Ru1 C6 171.11(13) . . ? C1 Ru1 C6 76.42(14) . . ? C3 Ru1 C6 89.01(13) . . ? C15 Ru1 C6 89.47(12) . . ? C11 Ru1 C6 75.34(12) . . ? Ru2 Ru1 C6 40.24(8) . . ? C6 Ru2 C4 97.28(16) . . ? C6 Ru2 C5 91.84(16) . . ? C4 Ru2 C5 92.34(15) . . ? C6 Ru2 C15 114.89(14) . . ? C4 Ru2 C15 146.41(14) . . ? C5 Ru2 C15 95.86(13) . . ? C6 Ru2 C11 93.82(14) . . ? C4 Ru2 C11 99.18(14) . . ? C5 Ru2 C11 166.40(13) . . ? C15 Ru2 C11 70.55(11) . . ? C6 Ru2 C14 145.97(14) . . ? C4 Ru2 C14 110.12(14) . . ? C5 Ru2 C14 106.35(13) . . ? C15 Ru2 C14 36.42(11) . . ? C11 Ru2 C14 62.90(12) . . ? C6 Ru2 C12 129.47(14) . . ? C4 Ru2 C12 88.66(14) . . ? C5 Ru2 C12 138.21(14) . . ? C15 Ru2 C12 63.94(11) . . ? C11 Ru2 C12 35.99(12) . . ? C14 Ru2 C12 36.27(11) . . ? C6 Ru2 Ru1 72.67(11) . . ? C4 Ru2 Ru1 144.18(11) . . ? C5 Ru2 Ru1 121.64(11) . . ? C15 Ru2 Ru1 48.92(8) . . ? C11 Ru2 Ru1 49.15(8) . . ? C14 Ru2 Ru1 73.30(8) . . ? C12 Ru2 Ru1 73.75(8) . . ? C7 Ru3 C8 91.80(15) . . ? C7 Ru3 C9 94.22(16) . . ? C8 Ru3 C9 95.46(14) . . ? C7 Ru3 C14 89.28(14) . . ? C8 Ru3 C14 98.37(13) . . ? C9 Ru3 C14 165.62(14) . . ? C7 Ru3 C16 101.34(13) . . ? C8 Ru3 C16 157.87(13) . . ? C9 Ru3 C16 101.17(13) . . ? C14 Ru3 C16 64.45(12) . . ? C7 Ru3 C17 135.31(13) . . ? C8 Ru3 C17 132.85(13) . . ? C9 Ru3 C17 84.52(13) . . ? C14 Ru3 C17 83.19(12) . . ? C16 Ru3 C17 36.56(11) . . ? C7 Ru3 C18 164.38(14) . . ? C8 Ru3 C18 98.51(13) . . ? C9 Ru3 C18 96.42(14) . . ? C14 Ru3 C18 77.69(12) . . ? C16 Ru3 C18 65.38(11) . . ? C17 Ru3 C18 35.39(10) . . ? O1 C1 Ru1 178.9(4) . . ? O2 C2 Ru1 178.9(3) . . ? O3 C3 Ru1 172.9(3) . . ? O4 C4 Ru2 178.3(3) . . ? O5 C5 Ru2 175.7(3) . . ? O6 C6 Ru2 170.3(3) . . ? O6 C6 Ru1 122.6(3) . . ? Ru2 C6 Ru1 67.09(11) . . ? O7 C7 Ru3 177.5(3) . . ? O8 C8 Ru3 175.8(3) . . ? O9 C9 Ru3 177.6(3) . . ? C12 C11 C10 118.1(3) . . ? C12 C11 Ru1 117.0(2) . . ? C10 C11 Ru1 124.3(3) . . ? C12 C11 Ru2 73.14(19) . . ? C10 C11 Ru2 128.2(2) . . ? Ru1 C11 Ru2 76.37(10) . . ? C11 C12 C14 113.8(3) . . ? C11 C12 C13 125.1(3) . . ? C14 C12 C13 121.1(3) . . ? C11 C12 Ru2 70.87(19) . . ? C14 C12 Ru2 71.48(18) . . ? C13 C12 Ru2 128.0(2) . . ? C15 C14 C12 115.2(3) . . ? C15 C14 Ru3 100.6(2) . . ? C12 C14 Ru3 143.5(2) . . ? C15 C14 Ru2 69.52(18) . . ? C12 C14 Ru2 72.25(19) . . ? Ru3 C14 Ru2 130.43(15) . . ? C14 C15 C16 104.5(3) . . ? C14 C15 Ru1 116.6(2) . . ? C16 C15 Ru1 135.6(2) . . ? C14 C15 Ru2 74.06(19) . . ? C16 C15 Ru2 132.2(2) . . ? Ru1 C15 Ru2 77.60(11) . . ? C17 C16 C23 117.5(3) . . ? C17 C16 C15 114.9(3) . . ? C23 C16 C15 121.3(3) . . ? C17 C16 Ru3 74.77(18) . . ? C23 C16 Ru3 127.1(2) . . ? C15 C16 Ru3 90.44(19) . . ? C18 C17 C22 116.1(3) . . ? C18 C17 C16 121.3(3) . . ? C22 C17 C16 121.7(3) . . ? C18 C17 Ru3 74.19(18) . . ? C22 C17 Ru3 120.9(2) . . ? C16 C17 Ru3 68.67(18) . . ? C19 C18 C17 120.1(3) . . ? C19 C18 Ru3 122.3(2) . . ? C17 C18 Ru3 70.42(18) . . ? C20 C19 C18 121.4(3) . . ? C19 C20 C21 119.4(3) . . ? C22 C21 C20 121.2(3) . . ? C21 C22 C17 121.7(3) . . ? C28 C23 C24 118.2(3) . . ? C28 C23 C16 122.1(3) . . ? C24 C23 C16 119.5(3) . . ? C25 C24 C23 120.6(3) . . ? C26 C25 C24 120.3(4) . . ? C27 C26 C25 119.9(3) . . ? C26 C27 C28 120.1(4) . . ? C23 C28 C27 120.9(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.562 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.087 #===END data_5b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H20 O9 Ru3' _chemical_formula_weight 923.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 13.279(2) _cell_length_b 17.3738(16) _cell_length_c 15.161(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.732(9) _cell_angle_gamma 90.00 _cell_volume 3411.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 355 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 1.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.983 _exptl_absorpt_process_details ; G. M. Sheldrick. SADABS: A program for absorption correction with the Siemens SMART system; University of G\"ottingen: Germany, 1996. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 35148 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7834 _reflns_number_gt 6324 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0276P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7834 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0515 _refine_ls_wR_factor_gt 0.0488 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.003 _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 0.317008(13) 0.607078(10) 0.825728(11) 0.02322(5) Uani 1 1 d . . . Ru2 Ru 0.200242(13) 0.553330(10) 0.667260(11) 0.02123(5) Uani 1 1 d . . . Ru3 Ru 0.005260(13) 0.730438(10) 0.682278(12) 0.02166(5) Uani 1 1 d . . . C1 C 0.45626(19) 0.56121(14) 0.85232(16) 0.0325(5) Uani 1 1 d . . . C2 C 0.29326(19) 0.57322(16) 0.94223(17) 0.0364(6) Uani 1 1 d . . . C3 C 0.35955(19) 0.70699(16) 0.86606(16) 0.0344(6) Uani 1 1 d . . . C4 C 0.23980(18) 0.51309(13) 0.56183(16) 0.0303(5) Uani 1 1 d . . . C5 C 0.06901(19) 0.50152(14) 0.63397(16) 0.0320(5) Uani 1 1 d . . . C6 C 0.25823(18) 0.47466(14) 0.75186(16) 0.0333(5) Uani 1 1 d . . . C7 C 0.02070(17) 0.81449(13) 0.60226(16) 0.0276(5) Uani 1 1 d . . . C8 C -0.05691(19) 0.66087(14) 0.58942(16) 0.0316(5) Uani 1 1 d . . . C9 C -0.12583(19) 0.77431(14) 0.70008(16) 0.0323(5) Uani 1 1 d . . . C11 C 0.32373(16) 0.64223(12) 0.69258(14) 0.0210(4) Uani 1 1 d . . . C12 C 0.23349(16) 0.68162(12) 0.64282(14) 0.0212(4) Uani 1 1 d . . . C14 C 0.14841(16) 0.67961(11) 0.68623(14) 0.0207(4) Uani 1 1 d . . . C15 C 0.16264(16) 0.63634(12) 0.76680(14) 0.0202(4) Uani 1 1 d . . . C16 C 0.06210(16) 0.64381(12) 0.79801(14) 0.0213(4) Uani 1 1 d . . . C17 C 0.04800(16) 0.71609(12) 0.84128(14) 0.0229(5) Uani 1 1 d . . . C18 C 0.09824(17) 0.78447(12) 0.81862(14) 0.0246(5) Uani 1 1 d . . . H18 H 0.1505 0.7810 0.7849 0.029 Uiso 1 1 calc R . . C19 C 0.06838(19) 0.85736(13) 0.84761(16) 0.0328(5) Uani 1 1 d . . . H19 H 0.0999 0.9028 0.8315 0.039 Uiso 1 1 calc R . . C20 C -0.0042(2) 0.86299(14) 0.89775(17) 0.0372(6) Uani 1 1 d . . . H20 H -0.0247 0.9122 0.9149 0.045 Uiso 1 1 calc R . . C21 C -0.04946(19) 0.79570(14) 0.92451(16) 0.0327(5) Uani 1 1 d . . . H21 H -0.0982 0.8000 0.9617 0.039 Uiso 1 1 calc R . . C22 C -0.02437(17) 0.72552(13) 0.89800(15) 0.0267(5) Uani 1 1 d . . . H22 H -0.0554 0.6812 0.9174 0.032 Uiso 1 1 calc R . . C23 C 0.00115(17) 0.57458(12) 0.81525(14) 0.0242(5) Uani 1 1 d . . . C24 C 0.05020(19) 0.50929(14) 0.85717(16) 0.0348(6) Uani 1 1 d . . . H24 H 0.1235 0.5075 0.8730 0.042 Uiso 1 1 calc R . . C25 C -0.0063(2) 0.44661(14) 0.8762(2) 0.0437(7) Uani 1 1 d . . . H25 H 0.0286 0.4025 0.9050 0.052 Uiso 1 1 calc R . . C26 C -0.1116(2) 0.44793(15) 0.8539(2) 0.0462(7) Uani 1 1 d . . . H26 H -0.1498 0.4055 0.8689 0.055 Uiso 1 1 calc R . . C27 C -0.1627(2) 0.51089(15) 0.8095(2) 0.0464(7) Uani 1 1 d . . . H27 H -0.2360 0.5113 0.7921 0.056 Uiso 1 1 calc R . . C28 C -0.10609(19) 0.57368(14) 0.79059(17) 0.0364(6) Uani 1 1 d . . . H28 H -0.1415 0.6169 0.7601 0.044 Uiso 1 1 calc R . . C29 C 0.42485(16) 0.64536(13) 0.66585(14) 0.0225(4) Uani 1 1 d . . . C30 C 0.47546(18) 0.58043(14) 0.64486(16) 0.0314(5) Uani 1 1 d . . . H30 H 0.4428 0.5317 0.6438 0.038 Uiso 1 1 calc R . . C31 C 0.57264(18) 0.58469(15) 0.62542(17) 0.0357(6) Uani 1 1 d . . . H31 H 0.6053 0.5393 0.6108 0.043 Uiso 1 1 calc R . . C32 C 0.62216(19) 0.65507(15) 0.62732(17) 0.0364(6) Uani 1 1 d . . . H32 H 0.6885 0.6584 0.6136 0.044 Uiso 1 1 calc R . . C33 C 0.57378(18) 0.72014(14) 0.64940(16) 0.0331(6) Uani 1 1 d . . . H33 H 0.6072 0.7687 0.6512 0.040 Uiso 1 1 calc R . . C34 C 0.47685(17) 0.71545(13) 0.66899(15) 0.0278(5) Uani 1 1 d . . . H34 H 0.4452 0.7609 0.6849 0.033 Uiso 1 1 calc R . . C35 C 0.22351(16) 0.72298(12) 0.55432(14) 0.0225(4) Uani 1 1 d . . . C36 C 0.26133(17) 0.79771(13) 0.55228(15) 0.0262(5) Uani 1 1 d . . . H36 H 0.2979 0.8208 0.6067 0.031 Uiso 1 1 calc R . . C37 C 0.24643(19) 0.83856(14) 0.47242(16) 0.0325(5) Uani 1 1 d . . . H37 H 0.2725 0.8895 0.4724 0.039 Uiso 1 1 calc R . . C38 C 0.19380(19) 0.80575(15) 0.39252(16) 0.0356(6) Uani 1 1 d . . . H38 H 0.1840 0.8339 0.3376 0.043 Uiso 1 1 calc R . . C39 C 0.1554(2) 0.73180(15) 0.39280(16) 0.0374(6) Uani 1 1 d . . . H39 H 0.1191 0.7090 0.3380 0.045 Uiso 1 1 calc R . . C40 C 0.16994(18) 0.69084(14) 0.47339(15) 0.0310(5) Uani 1 1 d . . . H40 H 0.1429 0.6402 0.4732 0.037 Uiso 1 1 calc R . . O1 O 0.53525(14) 0.53363(11) 0.86745(13) 0.0495(5) Uani 1 1 d . . . O2 O 0.28293(16) 0.55960(14) 1.01244(13) 0.0623(6) Uani 1 1 d . . . O3 O 0.38541(16) 0.76822(11) 0.88569(14) 0.0558(6) Uani 1 1 d . . . O4 O 0.26463(14) 0.49217(11) 0.49922(12) 0.0466(5) Uani 1 1 d . . . O5 O -0.00591(14) 0.46755(11) 0.61572(13) 0.0497(5) Uani 1 1 d . . . O6 O 0.27791(15) 0.41536(10) 0.78491(13) 0.0445(5) Uani 1 1 d . . . O7 O 0.02839(13) 0.86389(10) 0.55468(12) 0.0408(4) Uani 1 1 d . . . O8 O -0.09421(16) 0.62001(11) 0.53321(12) 0.0500(5) Uani 1 1 d . . . O9 O -0.19976(14) 0.80281(12) 0.70825(14) 0.0513(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01951(9) 0.02956(10) 0.02069(9) 0.00288(7) 0.00462(7) 0.00098(7) Ru2 0.02059(9) 0.02133(9) 0.02316(9) -0.00150(7) 0.00783(7) -0.00029(7) Ru3 0.01842(9) 0.02444(9) 0.02224(9) -0.00009(7) 0.00474(7) 0.00109(7) C1 0.0293(14) 0.0382(14) 0.0294(13) 0.0063(11) 0.0054(10) -0.0007(11) C2 0.0260(13) 0.0521(16) 0.0300(13) 0.0082(12) 0.0037(10) 0.0016(11) C3 0.0275(13) 0.0459(15) 0.0278(13) -0.0032(12) 0.0021(10) 0.0010(12) C4 0.0272(13) 0.0301(12) 0.0352(13) -0.0015(10) 0.0100(11) -0.0012(10) C5 0.0328(14) 0.0297(12) 0.0360(13) -0.0090(11) 0.0127(11) -0.0015(11) C6 0.0334(14) 0.0346(13) 0.0372(14) 0.0036(12) 0.0191(11) 0.0043(11) C7 0.0219(12) 0.0319(13) 0.0281(12) -0.0041(10) 0.0036(9) 0.0033(10) C8 0.0296(13) 0.0343(13) 0.0302(13) 0.0042(11) 0.0053(10) -0.0006(10) C9 0.0253(13) 0.0343(13) 0.0365(13) -0.0001(11) 0.0052(10) 0.0005(10) C11 0.0211(11) 0.0215(10) 0.0212(10) -0.0011(9) 0.0064(9) -0.0007(9) C12 0.0231(11) 0.0208(11) 0.0199(10) -0.0025(8) 0.0048(9) -0.0013(9) C14 0.0199(11) 0.0205(11) 0.0214(10) -0.0046(8) 0.0036(8) -0.0004(8) C15 0.0187(11) 0.0204(10) 0.0226(10) -0.0016(9) 0.0068(8) -0.0004(8) C16 0.0201(11) 0.0252(11) 0.0189(10) 0.0012(9) 0.0051(8) 0.0013(9) C17 0.0214(11) 0.0280(12) 0.0195(10) 0.0007(9) 0.0051(9) 0.0008(9) C18 0.0255(12) 0.0273(12) 0.0229(11) -0.0027(9) 0.0096(9) -0.0039(9) C19 0.0417(15) 0.0234(12) 0.0357(13) -0.0038(10) 0.0133(11) -0.0071(10) C20 0.0463(16) 0.0287(13) 0.0409(15) -0.0084(11) 0.0191(12) 0.0027(11) C21 0.0353(14) 0.0376(13) 0.0297(13) -0.0045(11) 0.0167(11) 0.0000(11) C22 0.0262(12) 0.0296(12) 0.0266(12) -0.0015(10) 0.0109(9) -0.0030(10) C23 0.0237(12) 0.0253(11) 0.0266(11) -0.0029(9) 0.0118(9) -0.0019(9) C24 0.0276(13) 0.0350(14) 0.0439(15) 0.0058(11) 0.0124(11) -0.0018(10) C25 0.0420(16) 0.0293(13) 0.0644(19) 0.0104(13) 0.0214(14) 0.0025(12) C26 0.0434(17) 0.0297(14) 0.074(2) -0.0020(13) 0.0304(15) -0.0105(12) C27 0.0264(14) 0.0396(15) 0.075(2) -0.0026(14) 0.0158(14) -0.0065(12) C28 0.0278(13) 0.0339(13) 0.0480(16) 0.0030(12) 0.0094(11) -0.0007(11) C29 0.0203(11) 0.0276(11) 0.0191(10) 0.0011(9) 0.0032(9) 0.0004(9) C30 0.0275(13) 0.0271(12) 0.0422(14) -0.0036(11) 0.0132(11) -0.0033(10) C31 0.0270(13) 0.0367(14) 0.0469(15) -0.0056(12) 0.0155(11) 0.0032(11) C32 0.0222(12) 0.0483(16) 0.0408(15) 0.0010(12) 0.0112(11) -0.0032(11) C33 0.0266(13) 0.0343(14) 0.0375(14) 0.0038(11) 0.0052(10) -0.0083(10) C34 0.0250(12) 0.0259(12) 0.0317(12) -0.0021(10) 0.0047(10) 0.0003(9) C35 0.0202(11) 0.0266(11) 0.0222(11) 0.0022(9) 0.0078(9) 0.0040(9) C36 0.0259(12) 0.0275(11) 0.0260(12) -0.0003(10) 0.0076(9) 0.0019(10) C37 0.0316(13) 0.0298(13) 0.0380(14) 0.0082(11) 0.0115(11) 0.0018(10) C38 0.0366(14) 0.0450(15) 0.0274(13) 0.0145(11) 0.0117(11) 0.0087(12) C39 0.0369(15) 0.0495(16) 0.0241(12) 0.0043(11) 0.0030(11) -0.0030(12) C40 0.0331(13) 0.0339(13) 0.0259(12) 0.0020(10) 0.0062(10) -0.0059(10) O1 0.0283(10) 0.0570(12) 0.0613(13) 0.0115(10) 0.0058(9) 0.0125(9) O2 0.0472(13) 0.1086(19) 0.0321(11) 0.0215(12) 0.0110(9) -0.0022(12) O3 0.0532(14) 0.0447(12) 0.0639(14) -0.0210(10) 0.0010(10) -0.0091(10) O4 0.0488(12) 0.0577(12) 0.0384(10) -0.0155(9) 0.0207(9) 0.0014(9) O5 0.0381(11) 0.0500(12) 0.0629(13) -0.0206(10) 0.0148(10) -0.0192(9) O6 0.0601(13) 0.0307(10) 0.0470(11) 0.0102(9) 0.0213(9) 0.0104(9) O7 0.0397(11) 0.0414(10) 0.0411(10) 0.0140(9) 0.0084(8) 0.0044(8) O8 0.0619(14) 0.0432(11) 0.0379(11) -0.0082(9) -0.0044(9) -0.0121(10) O9 0.0276(10) 0.0586(12) 0.0698(14) -0.0012(11) 0.0152(9) 0.0125(9) _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 1.885(3) . ? Ru1 C2 1.952(2) . ? Ru1 C1 1.972(3) . ? Ru1 C15 2.110(2) . ? Ru1 C11 2.130(2) . ? Ru1 C6 2.602(2) . ? Ru1 Ru2 2.7215(4) . ? Ru2 C6 1.916(2) . ? Ru2 C4 1.921(2) . ? Ru2 C5 1.927(2) . ? Ru2 C15 2.222(2) . ? Ru2 C11 2.224(2) . ? Ru2 C12 2.318(2) . ? Ru2 C14 2.336(2) . ? Ru3 C8 1.901(3) . ? Ru3 C7 1.938(2) . ? Ru3 C9 1.973(2) . ? Ru3 C14 2.085(2) . ? Ru3 C16 2.309(2) . ? Ru3 C18 2.357(2) . ? Ru3 C17 2.365(2) . ? C1 O1 1.130(3) . ? C2 O2 1.128(3) . ? C3 O3 1.137(3) . ? C4 O4 1.131(3) . ? C5 O5 1.137(3) . ? C6 O6 1.150(3) . ? C7 O7 1.140(3) . ? C8 O8 1.136(3) . ? C9 O9 1.130(3) . ? C11 C12 1.440(3) . ? C11 C29 1.487(3) . ? C12 C14 1.428(3) . ? C12 C35 1.502(3) . ? C14 C15 1.411(3) . ? C15 C16 1.517(3) . ? C16 C17 1.448(3) . ? C16 C23 1.504(3) . ? C17 C22 1.433(3) . ? C17 C18 1.441(3) . ? C18 C19 1.425(3) . ? C19 C20 1.357(3) . ? C20 C21 1.414(3) . ? C21 C22 1.348(3) . ? C23 C24 1.390(3) . ? C23 C28 1.390(3) . ? C24 C25 1.388(3) . ? C25 C26 1.364(4) . ? C26 C27 1.382(4) . ? C27 C28 1.390(3) . ? C29 C30 1.386(3) . ? C29 C34 1.395(3) . ? C30 C31 1.388(3) . ? C31 C32 1.386(3) . ? C32 C33 1.378(3) . ? C33 C34 1.386(3) . ? C35 C40 1.392(3) . ? C35 C36 1.395(3) . ? C36 C37 1.380(3) . ? C37 C38 1.381(3) . ? C38 C39 1.383(4) . ? C39 C40 1.390(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 C2 94.62(11) . . ? C3 Ru1 C1 96.05(10) . . ? C2 Ru1 C1 91.40(10) . . ? C3 Ru1 C15 96.27(9) . . ? C2 Ru1 C15 96.90(9) . . ? C1 Ru1 C15 164.53(9) . . ? C3 Ru1 C11 88.35(9) . . ? C2 Ru1 C11 173.19(9) . . ? C1 Ru1 C11 94.38(9) . . ? C15 Ru1 C11 76.66(8) . . ? C3 Ru1 C6 173.57(9) . . ? C2 Ru1 C6 91.72(10) . . ? C1 Ru1 C6 84.81(9) . . ? C15 Ru1 C6 81.92(8) . . ? C11 Ru1 C6 85.23(7) . . ? C3 Ru1 Ru2 132.37(7) . . ? C2 Ru1 Ru2 121.41(8) . . ? C1 Ru1 Ru2 111.59(7) . . ? C15 Ru1 Ru2 52.95(6) . . ? C11 Ru1 Ru2 52.87(6) . . ? C6 Ru1 Ru2 42.11(5) . . ? C6 Ru2 C4 98.87(10) . . ? C6 Ru2 C5 92.81(10) . . ? C4 Ru2 C5 90.54(10) . . ? C6 Ru2 C15 97.21(9) . . ? C4 Ru2 C15 160.88(9) . . ? C5 Ru2 C15 98.94(8) . . ? C6 Ru2 C11 101.99(9) . . ? C4 Ru2 C11 94.01(9) . . ? C5 Ru2 C11 163.64(9) . . ? C15 Ru2 C11 72.51(7) . . ? C6 Ru2 C12 136.92(9) . . ? C4 Ru2 C12 96.91(9) . . ? C5 Ru2 C12 126.90(9) . . ? C15 Ru2 C12 64.13(7) . . ? C11 Ru2 C12 36.91(7) . . ? C6 Ru2 C14 132.33(9) . . ? C4 Ru2 C14 125.90(9) . . ? C5 Ru2 C14 101.36(9) . . ? C15 Ru2 C14 35.96(7) . . ? C11 Ru2 C14 63.41(7) . . ? C12 Ru2 C14 35.73(7) . . ? C6 Ru2 Ru1 65.61(7) . . ? C4 Ru2 Ru1 130.73(7) . . ? C5 Ru2 Ru1 134.25(7) . . ? C15 Ru2 Ru1 49.26(5) . . ? C11 Ru2 Ru1 49.78(5) . . ? C12 Ru2 Ru1 73.72(5) . . ? C14 Ru2 Ru1 72.24(5) . . ? C8 Ru3 C7 95.98(10) . . ? C8 Ru3 C9 95.43(10) . . ? C7 Ru3 C9 90.73(10) . . ? C8 Ru3 C14 89.79(9) . . ? C7 Ru3 C14 96.64(9) . . ? C9 Ru3 C14 170.48(9) . . ? C8 Ru3 C16 99.45(9) . . ? C7 Ru3 C16 154.82(9) . . ? C9 Ru3 C16 107.37(9) . . ? C14 Ru3 C16 63.81(8) . . ? C8 Ru3 C18 163.97(9) . . ? C7 Ru3 C18 98.15(9) . . ? C9 Ru3 C18 91.93(9) . . ? C14 Ru3 C18 81.11(8) . . ? C16 Ru3 C18 64.70(7) . . ? C8 Ru3 C17 130.96(9) . . ? C7 Ru3 C17 133.06(9) . . ? C9 Ru3 C17 85.53(9) . . ? C14 Ru3 C17 85.04(8) . . ? C16 Ru3 C17 36.07(7) . . ? C18 Ru3 C17 35.53(7) . . ? O1 C1 Ru1 178.7(2) . . ? O2 C2 Ru1 174.0(3) . . ? O3 C3 Ru1 176.3(2) . . ? O4 C4 Ru2 177.3(2) . . ? O5 C5 Ru2 176.5(2) . . ? O6 C6 Ru2 161.8(2) . . ? O6 C6 Ru1 125.92(19) . . ? Ru2 C6 Ru1 72.28(8) . . ? O7 C7 Ru3 179.1(2) . . ? O8 C8 Ru3 179.2(2) . . ? O9 C9 Ru3 176.5(2) . . ? C12 C11 C29 122.48(18) . . ? C12 C11 Ru1 115.39(14) . . ? C29 C11 Ru1 119.87(14) . . ? C12 C11 Ru2 75.10(12) . . ? C29 C11 Ru2 130.87(15) . . ? Ru1 C11 Ru2 77.35(7) . . ? C14 C12 C11 113.48(18) . . ? C14 C12 C35 120.04(19) . . ? C11 C12 C35 126.48(19) . . ? C14 C12 Ru2 72.83(12) . . ? C11 C12 Ru2 67.99(11) . . ? C35 C12 Ru2 128.35(14) . . ? C15 C14 C12 116.33(19) . . ? C15 C14 Ru3 101.41(14) . . ? C12 C14 Ru3 141.76(16) . . ? C15 C14 Ru2 67.63(11) . . ? C12 C14 Ru2 71.44(11) . . ? Ru3 C14 Ru2 133.30(10) . . ? C14 C15 C16 105.38(17) . . ? C14 C15 Ru1 115.29(14) . . ? C16 C15 Ru1 136.74(15) . . ? C14 C15 Ru2 76.42(12) . . ? C16 C15 Ru2 127.75(14) . . ? Ru1 C15 Ru2 77.79(7) . . ? C17 C16 C23 119.10(18) . . ? C17 C16 C15 115.22(18) . . ? C23 C16 C15 122.00(18) . . ? C17 C16 Ru3 74.08(12) . . ? C23 C16 Ru3 123.71(15) . . ? C15 C16 Ru3 88.94(12) . . ? C22 C17 C18 117.11(19) . . ? C22 C17 C16 122.81(19) . . ? C18 C17 C16 119.62(18) . . ? C22 C17 Ru3 123.89(16) . . ? C18 C17 Ru3 71.92(12) . . ? C16 C17 Ru3 69.85(11) . . ? C19 C18 C17 119.0(2) . . ? C19 C18 Ru3 119.79(16) . . ? C17 C18 Ru3 72.54(12) . . ? C20 C19 C18 121.2(2) . . ? C19 C20 C21 120.0(2) . . ? C22 C21 C20 120.9(2) . . ? C21 C22 C17 121.6(2) . . ? C24 C23 C28 117.6(2) . . ? C24 C23 C16 121.1(2) . . ? C28 C23 C16 121.4(2) . . ? C25 C24 C23 121.0(2) . . ? C26 C25 C24 120.4(2) . . ? C25 C26 C27 120.1(2) . . ? C26 C27 C28 119.4(2) . . ? C27 C28 C23 121.5(2) . . ? C30 C29 C34 117.2(2) . . ? C30 C29 C11 123.1(2) . . ? C34 C29 C11 119.50(19) . . ? C29 C30 C31 121.8(2) . . ? C32 C31 C30 120.1(2) . . ? C33 C32 C31 119.0(2) . . ? C32 C33 C34 120.6(2) . . ? C33 C34 C29 121.3(2) . . ? C40 C35 C36 118.0(2) . . ? C40 C35 C12 121.52(19) . . ? C36 C35 C12 120.26(19) . . ? C37 C36 C35 121.0(2) . . ? C36 C37 C38 120.3(2) . . ? C37 C38 C39 119.8(2) . . ? C38 C39 C40 119.9(2) . . ? C39 C40 C35 120.9(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.377 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.072 #===END data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H20 O12 Ru4' _chemical_formula_weight 1108.85 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.232(3) _cell_length_b 14.127(5) _cell_length_c 15.478(3) _cell_angle_alpha 83.66(2) _cell_angle_beta 82.26(2) _cell_angle_gamma 74.024(18) _cell_volume 1917.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 355 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 1.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.420 _exptl_absorpt_correction_T_max 0.647 _exptl_absorpt_process_details ; G. M. Sheldrick. SADABS: A program for absorption correction with the Siemens SMART system; University of G\"ottingen: Germany, 1996. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19421 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8649 _reflns_number_gt 6102 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0193P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8649 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0546 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 0.826 _refine_ls_restrained_S_all 0.826 _refine_ls_shift/su_max 0.004 _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 0.40864(3) 0.963427(19) 0.291113(17) 0.02389(7) Uani 1 1 d . . . Ru2 Ru 0.43798(3) 0.764890(19) 0.354167(17) 0.02295(7) Uani 1 1 d . . . Ru3 Ru 0.68276(3) 0.847573(18) 0.345296(17) 0.02194(7) Uani 1 1 d . . . Ru4 Ru 0.70352(3) 0.632061(19) 0.400577(18) 0.02562(7) Uani 1 1 d . . . C1 C 0.2612(4) 1.0038(3) 0.3934(2) 0.0339(8) Uani 1 1 d . . . C2 C 0.4532(4) 1.0876(3) 0.2788(2) 0.0331(8) Uani 1 1 d . . . C3 C 0.2658(4) 1.0137(3) 0.2100(2) 0.0335(8) Uani 1 1 d . . . C4 C 0.2939(4) 0.8201(3) 0.2733(2) 0.0329(8) Uani 1 1 d . . . C5 C 0.3013(4) 0.7911(2) 0.4631(2) 0.0305(8) Uani 1 1 d . . . C6 C 0.4015(4) 0.6383(3) 0.3558(2) 0.0350(8) Uani 1 1 d . . . C7 C 0.7460(4) 0.9661(3) 0.3430(2) 0.0336(8) Uani 1 1 d . . . C8 C 0.5752(4) 0.8690(2) 0.4589(2) 0.0288(8) Uani 1 1 d . . . C9 C 0.8832(4) 0.7829(2) 0.3760(2) 0.0339(8) Uani 1 1 d . . . C10 C 0.6569(4) 0.6591(3) 0.5265(3) 0.0360(9) Uani 1 1 d . . . C11 C 0.9145(4) 0.5737(3) 0.4045(2) 0.0367(9) Uani 1 1 d . . . C12 C 0.6717(4) 0.5059(3) 0.4225(2) 0.0366(9) Uani 1 1 d . . . C13 C 0.6080(3) 0.9051(2) 0.20744(19) 0.0209(7) Uani 1 1 d . . . C14 C 0.6850(3) 0.8036(2) 0.2047(2) 0.0210(7) Uani 1 1 d . . . C15 C 0.6267(3) 0.7308(2) 0.2608(2) 0.0221(7) Uani 1 1 d . . . C16 C 0.7020(3) 0.6273(2) 0.2648(2) 0.0245(7) Uani 1 1 d . . . C17 C 0.7317(3) 0.5581(2) 0.2073(2) 0.0253(7) Uani 1 1 d . . . C18 C 0.6703(3) 0.9759(2) 0.1439(2) 0.0227(7) Uani 1 1 d . . . C19 C 0.5796(4) 1.0325(2) 0.0823(2) 0.0298(8) Uani 1 1 d . . . H19 H 0.4780 1.0287 0.0843 0.036 Uiso 1 1 calc R . . C20 C 0.6341(4) 1.0944(2) 0.0181(2) 0.0366(9) Uani 1 1 d . . . H20 H 0.5707 1.1308 -0.0244 0.044 Uiso 1 1 calc R . . C21 C 0.7785(4) 1.1035(2) 0.0154(2) 0.0362(9) Uani 1 1 d . . . H21 H 0.8158 1.1459 -0.0287 0.043 Uiso 1 1 calc R . . C22 C 0.8693(4) 1.0502(2) 0.0777(2) 0.0345(8) Uani 1 1 d . . . H22 H 0.9688 1.0573 0.0774 0.041 Uiso 1 1 calc R . . C23 C 0.8166(3) 0.9865(2) 0.1405(2) 0.0288(8) Uani 1 1 d . . . H23 H 0.8813 0.9492 0.1820 0.035 Uiso 1 1 calc R . . C24 C 0.8191(3) 0.7677(2) 0.1376(2) 0.0237(7) Uani 1 1 d . . . C25 C 0.7994(4) 0.7841(2) 0.0494(2) 0.0288(8) Uani 1 1 d . . . H25 H 0.7032 0.8197 0.0322 0.035 Uiso 1 1 calc R . . C26 C 0.9189(4) 0.7491(2) -0.0146(2) 0.0343(8) Uani 1 1 d . . . H26 H 0.9042 0.7615 -0.0748 0.041 Uiso 1 1 calc R . . C27 C 1.0567(4) 0.6970(2) 0.0102(3) 0.0384(9) Uani 1 1 d . . . H27 H 1.1379 0.6728 -0.0331 0.046 Uiso 1 1 calc R . . C28 C 1.0795(4) 0.6791(2) 0.0973(3) 0.0352(9) Uani 1 1 d . . . H28 H 1.1759 0.6429 0.1140 0.042 Uiso 1 1 calc R . . C29 C 0.9604(3) 0.7145(2) 0.1607(2) 0.0278(7) Uani 1 1 d . . . H29 H 0.9761 0.7019 0.2208 0.033 Uiso 1 1 calc R . . C30 C 0.6822(3) 0.5796(2) 0.1180(2) 0.0263(7) Uani 1 1 d . . . C31 C 0.5370(4) 0.6350(2) 0.1029(2) 0.0343(8) Uani 1 1 d . . . H31 H 0.4664 0.6606 0.1507 0.041 Uiso 1 1 calc R . . C32 C 0.4937(4) 0.6535(3) 0.0188(3) 0.0423(10) Uani 1 1 d . . . H32 H 0.3933 0.6903 0.0098 0.051 Uiso 1 1 calc R . . C33 C 0.5962(4) 0.6187(3) -0.0522(3) 0.0428(10) Uani 1 1 d . . . H33 H 0.5670 0.6323 -0.1098 0.051 Uiso 1 1 calc R . . C34 C 0.7407(4) 0.5640(3) -0.0381(2) 0.0398(9) Uani 1 1 d . . . H34 H 0.8120 0.5409 -0.0864 0.048 Uiso 1 1 calc R . . C35 C 0.7828(4) 0.5426(2) 0.0459(2) 0.0327(8) Uani 1 1 d . . . H35 H 0.8813 0.5021 0.0548 0.039 Uiso 1 1 calc R . . C36 C 0.8151(4) 0.4529(2) 0.2295(2) 0.0318(8) Uani 1 1 d . . . C37 C 0.9611(4) 0.4269(3) 0.2510(3) 0.0478(10) Uani 1 1 d . . . H37 H 1.0130 0.4764 0.2510 0.057 Uiso 1 1 calc R . . C38 C 1.0342(5) 0.3278(4) 0.2731(3) 0.0655(13) Uani 1 1 d . . . H38 H 1.1350 0.3103 0.2884 0.079 Uiso 1 1 calc R . . C39 C 0.9602(6) 0.2570(3) 0.2726(3) 0.0714(15) Uani 1 1 d . . . H39 H 1.0094 0.1900 0.2884 0.086 Uiso 1 1 calc R . . C40 C 0.8174(6) 0.2807(3) 0.2500(3) 0.0632(13) Uani 1 1 d . . . H40 H 0.7674 0.2304 0.2493 0.076 Uiso 1 1 calc R . . C41 C 0.7439(5) 0.3781(3) 0.2278(3) 0.0471(10) Uani 1 1 d . . . H41 H 0.6441 0.3940 0.2113 0.057 Uiso 1 1 calc R . . O1 O 0.1769(3) 1.0308(2) 0.45117(18) 0.0498(7) Uani 1 1 d . . . O2 O 0.4742(3) 1.16388(18) 0.27086(17) 0.0486(7) Uani 1 1 d . . . O3 O 0.1816(3) 1.0454(2) 0.16011(18) 0.0528(8) Uani 1 1 d . . . O4 O 0.2061(3) 0.82550(19) 0.22565(18) 0.0529(8) Uani 1 1 d . . . O5 O 0.2234(3) 0.80434(19) 0.52637(17) 0.0457(7) Uani 1 1 d . . . O6 O 0.3639(3) 0.56943(18) 0.34999(18) 0.0501(7) Uani 1 1 d . . . O7 O 0.7873(3) 1.03433(18) 0.34537(17) 0.0467(7) Uani 1 1 d . . . O8 O 0.5229(3) 0.88860(17) 0.52767(15) 0.0345(6) Uani 1 1 d . . . O9 O 1.0022(3) 0.75945(19) 0.39763(18) 0.0511(7) Uani 1 1 d . . . O10 O 0.6304(3) 0.6672(2) 0.59878(18) 0.0547(8) Uani 1 1 d . . . O11 O 1.0399(3) 0.5377(2) 0.40824(18) 0.0532(8) Uani 1 1 d . . . O12 O 0.6500(3) 0.43010(19) 0.43680(17) 0.0516(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02581(14) 0.02376(14) 0.02127(16) -0.00271(12) 0.00016(11) -0.00609(11) Ru2 0.02390(14) 0.02503(14) 0.02106(16) -0.00245(12) 0.00302(11) -0.01072(11) Ru3 0.02516(14) 0.02335(14) 0.01885(15) -0.00107(11) -0.00063(11) -0.01006(11) Ru4 0.02992(15) 0.02460(15) 0.02119(16) 0.00187(12) 0.00140(12) -0.00867(11) C1 0.038(2) 0.032(2) 0.031(2) -0.0023(17) -0.0018(17) -0.0098(16) C2 0.037(2) 0.032(2) 0.027(2) -0.0081(17) 0.0022(16) -0.0049(16) C3 0.0313(19) 0.036(2) 0.031(2) -0.0067(17) 0.0020(16) -0.0062(16) C4 0.034(2) 0.036(2) 0.030(2) -0.0042(17) 0.0047(16) -0.0150(16) C5 0.0339(19) 0.033(2) 0.027(2) -0.0037(16) 0.0024(16) -0.0151(16) C6 0.036(2) 0.038(2) 0.032(2) -0.0067(17) 0.0112(16) -0.0170(17) C7 0.047(2) 0.039(2) 0.020(2) -0.0009(16) -0.0035(16) -0.0198(17) C8 0.0304(18) 0.0279(19) 0.028(2) -0.0031(16) 0.0028(15) -0.0100(14) C9 0.036(2) 0.035(2) 0.031(2) -0.0031(17) -0.0015(16) -0.0118(16) C10 0.047(2) 0.029(2) 0.034(2) 0.0013(18) -0.0038(18) -0.0132(16) C11 0.045(2) 0.039(2) 0.025(2) 0.0069(17) -0.0019(17) -0.0144(18) C12 0.043(2) 0.037(2) 0.027(2) -0.0016(18) 0.0078(16) -0.0109(17) C13 0.0243(16) 0.0239(17) 0.0162(17) -0.0025(14) -0.0016(13) -0.0093(13) C14 0.0231(16) 0.0244(17) 0.0168(17) -0.0020(14) -0.0006(13) -0.0092(13) C15 0.0232(16) 0.0296(18) 0.0148(17) -0.0038(14) 0.0036(13) -0.0110(13) C16 0.0233(16) 0.0251(17) 0.0257(19) -0.0006(15) 0.0013(14) -0.0101(13) C17 0.0247(16) 0.0236(17) 0.028(2) -0.0005(15) 0.0046(14) -0.0104(13) C18 0.0269(17) 0.0211(16) 0.0200(18) -0.0034(14) 0.0004(13) -0.0068(13) C19 0.0318(18) 0.0286(19) 0.030(2) 0.0013(16) 0.0005(15) -0.0121(15) C20 0.044(2) 0.033(2) 0.033(2) 0.0087(17) -0.0080(17) -0.0134(17) C21 0.044(2) 0.035(2) 0.033(2) 0.0065(17) 0.0020(17) -0.0227(17) C22 0.036(2) 0.039(2) 0.034(2) -0.0035(18) 0.0020(16) -0.0215(17) C23 0.0332(19) 0.0286(19) 0.026(2) 0.0001(16) -0.0031(15) -0.0112(15) C24 0.0282(17) 0.0216(16) 0.0230(19) -0.0032(14) 0.0065(14) -0.0131(14) C25 0.0356(19) 0.0266(18) 0.025(2) -0.0035(15) 0.0007(15) -0.0112(15) C26 0.050(2) 0.032(2) 0.023(2) -0.0055(16) 0.0092(16) -0.0182(17) C27 0.040(2) 0.033(2) 0.042(3) -0.0112(18) 0.0173(18) -0.0152(17) C28 0.0288(19) 0.031(2) 0.044(3) -0.0059(18) 0.0054(17) -0.0087(15) C29 0.0310(18) 0.0256(18) 0.026(2) -0.0013(15) 0.0035(15) -0.0096(14) C30 0.0321(18) 0.0201(17) 0.027(2) -0.0034(15) 0.0028(15) -0.0102(14) C31 0.0325(19) 0.034(2) 0.037(2) -0.0080(17) 0.0013(16) -0.0104(16) C32 0.039(2) 0.040(2) 0.050(3) -0.003(2) -0.0137(19) -0.0085(17) C33 0.058(3) 0.042(2) 0.031(2) -0.0015(19) -0.011(2) -0.016(2) C34 0.053(2) 0.041(2) 0.024(2) -0.0067(18) 0.0066(17) -0.0128(18) C35 0.0348(19) 0.032(2) 0.029(2) -0.0040(17) 0.0030(16) -0.0074(15) C36 0.045(2) 0.0264(19) 0.0187(19) -0.0030(15) 0.0102(15) -0.0060(16) C37 0.048(2) 0.041(2) 0.045(3) -0.005(2) 0.001(2) 0.0016(19) C38 0.069(3) 0.057(3) 0.048(3) 0.001(3) -0.001(2) 0.017(2) C39 0.118(5) 0.029(3) 0.043(3) 0.001(2) 0.007(3) 0.012(3) C40 0.109(4) 0.027(2) 0.048(3) -0.001(2) 0.010(3) -0.018(2) C41 0.072(3) 0.029(2) 0.039(3) -0.0029(19) 0.005(2) -0.0145(19) O1 0.0502(17) 0.0533(18) 0.0376(18) -0.0094(14) 0.0127(14) -0.0060(13) O2 0.0735(19) 0.0281(15) 0.0463(19) -0.0065(13) 0.0028(14) -0.0199(13) O3 0.0457(16) 0.0598(19) 0.0486(19) -0.0016(15) -0.0185(14) -0.0016(14) O4 0.0569(17) 0.0569(18) 0.056(2) 0.0094(15) -0.0289(15) -0.0282(14) O5 0.0522(17) 0.0514(17) 0.0324(17) -0.0098(13) 0.0194(13) -0.0207(13) O6 0.0554(17) 0.0396(16) 0.064(2) -0.0111(14) 0.0092(14) -0.0312(14) O7 0.0747(19) 0.0419(16) 0.0363(17) -0.0032(13) -0.0045(14) -0.0374(14) O8 0.0462(15) 0.0370(14) 0.0219(14) -0.0092(11) 0.0072(11) -0.0162(11) O9 0.0358(15) 0.0542(18) 0.066(2) 0.0018(15) -0.0142(14) -0.0146(13) O10 0.093(2) 0.0450(18) 0.0251(17) -0.0041(14) -0.0024(15) -0.0180(15) O11 0.0361(15) 0.0614(19) 0.055(2) 0.0111(15) -0.0079(14) -0.0052(13) O12 0.076(2) 0.0326(15) 0.0437(18) 0.0011(13) 0.0167(14) -0.0238(14) _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 1.885(3) . ? Ru1 C2 1.893(4) . ? Ru1 C1 1.969(4) . ? Ru1 C13 2.122(3) . ? Ru1 C4 2.585(3) . ? Ru1 Ru3 2.7883(9) . ? Ru1 Ru2 2.8178(10) . ? Ru2 C4 1.899(4) . ? Ru2 C6 1.905(3) . ? Ru2 C5 1.970(4) . ? Ru2 C15 2.091(3) . ? Ru2 Ru4 2.7733(9) . ? Ru2 Ru3 2.7970(8) . ? Ru3 C8 1.910(4) . ? Ru3 C7 1.914(3) . ? Ru3 C9 1.922(3) . ? Ru3 C13 2.323(3) . ? Ru3 C14 2.324(3) . ? Ru3 C15 2.414(3) . ? Ru3 Ru4 3.0306(11) . ? Ru4 C12 1.872(4) . ? Ru4 C11 1.901(4) . ? Ru4 C10 1.995(4) . ? Ru4 C16 2.113(3) . ? Ru4 C15 2.516(3) . ? C1 O1 1.129(4) . ? C2 O2 1.137(4) . ? C3 O3 1.138(4) . ? C4 O4 1.150(4) . ? C5 O5 1.135(4) . ? C6 O6 1.135(4) . ? C7 O7 1.136(4) . ? C8 O8 1.139(4) . ? C9 O9 1.142(3) . ? C10 O10 1.124(4) . ? C11 O11 1.135(4) . ? C12 O12 1.135(4) . ? C13 C14 1.416(4) . ? C13 C18 1.499(4) . ? C14 C15 1.443(4) . ? C14 C24 1.514(4) . ? C15 C16 1.435(4) . ? C16 C17 1.341(4) . ? C17 C30 1.487(4) . ? C17 C36 1.499(4) . ? C18 C19 1.389(4) . ? C18 C23 1.392(4) . ? C19 C20 1.386(4) . ? C20 C21 1.370(4) . ? C21 C22 1.382(4) . ? C22 C23 1.383(4) . ? C24 C29 1.386(4) . ? C24 C25 1.387(4) . ? C25 C26 1.398(4) . ? C26 C27 1.364(4) . ? C27 C28 1.377(5) . ? C28 C29 1.392(4) . ? C30 C31 1.390(4) . ? C30 C35 1.401(4) . ? C31 C32 1.389(5) . ? C32 C33 1.389(5) . ? C33 C34 1.377(5) . ? C34 C35 1.386(5) . ? C36 C37 1.373(5) . ? C36 C41 1.394(5) . ? C37 C38 1.403(5) . ? C38 C39 1.359(6) . ? C39 C40 1.352(6) . ? C40 C41 1.384(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 C3 Ru1 C2 88.53(14) . . ? C3 Ru1 C1 94.14(14) . . ? C2 Ru1 C1 90.53(14) . . ? C3 Ru1 C13 101.47(13) . . ? C2 Ru1 C13 90.02(13) . . ? C1 Ru1 C13 164.39(12) . . ? C3 Ru1 C4 74.29(13) . . ? C2 Ru1 C4 162.81(13) . . ? C1 Ru1 C4 91.19(12) . . ? C13 Ru1 C4 92.88(11) . . ? C3 Ru1 Ru3 154.60(11) . . ? C2 Ru1 Ru3 98.43(10) . . ? C1 Ru1 Ru3 110.09(10) . . ? C13 Ru1 Ru3 54.43(8) . . ? C4 Ru1 Ru3 97.03(8) . . ? C3 Ru1 Ru2 115.15(10) . . ? C2 Ru1 Ru2 156.30(10) . . ? C1 Ru1 Ru2 88.76(10) . . ? C13 Ru1 Ru2 84.50(8) . . ? C4 Ru1 Ru2 40.87(8) . . ? Ru3 Ru1 Ru2 59.86(2) . . ? C4 Ru2 C6 91.47(15) . . ? C4 Ru2 C5 98.40(14) . . ? C6 Ru2 C5 90.34(14) . . ? C4 Ru2 C15 96.17(13) . . ? C6 Ru2 C15 93.15(13) . . ? C5 Ru2 C15 164.93(12) . . ? C4 Ru2 Ru4 151.55(11) . . ? C6 Ru2 Ru4 75.27(11) . . ? C5 Ru2 Ru4 106.59(10) . . ? C15 Ru2 Ru4 60.39(9) . . ? C4 Ru2 Ru3 116.81(10) . . ? C6 Ru2 Ru3 139.11(10) . . ? C5 Ru2 Ru3 112.13(9) . . ? C15 Ru2 Ru3 57.03(8) . . ? Ru4 Ru2 Ru3 65.92(3) . . ? C4 Ru2 Ru1 62.96(10) . . ? C6 Ru2 Ru1 154.12(11) . . ? C5 Ru2 Ru1 97.04(10) . . ? C15 Ru2 Ru1 86.14(9) . . ? Ru4 Ru2 Ru1 125.33(2) . . ? Ru3 Ru2 Ru1 59.55(2) . . ? C8 Ru3 C7 91.21(14) . . ? C8 Ru3 C9 100.39(14) . . ? C7 Ru3 C9 84.41(14) . . ? C8 Ru3 C13 130.64(12) . . ? C7 Ru3 C13 86.35(12) . . ? C9 Ru3 C13 128.26(13) . . ? C8 Ru3 C14 147.89(11) . . ? C7 Ru3 C14 111.21(13) . . ? C9 Ru3 C14 104.30(13) . . ? C13 Ru3 C14 35.48(10) . . ? C8 Ru3 C15 118.35(12) . . ? C7 Ru3 C15 146.54(13) . . ? C9 Ru3 C15 103.64(12) . . ? C13 Ru3 C15 62.96(10) . . ? C14 Ru3 C15 35.41(10) . . ? C8 Ru3 Ru1 82.67(10) . . ? C7 Ru3 Ru1 88.12(11) . . ? C9 Ru3 Ru1 171.98(10) . . ? C13 Ru3 Ru1 48.00(8) . . ? C14 Ru3 Ru1 75.69(8) . . ? C15 Ru3 Ru1 81.09(7) . . ? C8 Ru3 Ru2 73.85(9) . . ? C7 Ru3 Ru2 146.34(11) . . ? C9 Ru3 Ru2 127.33(10) . . ? C13 Ru3 Ru2 81.50(7) . . ? C14 Ru3 Ru2 74.91(7) . . ? C15 Ru3 Ru2 46.59(7) . . ? Ru1 Ru3 Ru2 60.60(2) . . ? C8 Ru3 Ru4 83.99(10) . . ? C7 Ru3 Ru4 153.25(10) . . ? C9 Ru3 Ru4 70.71(10) . . ? C13 Ru3 Ru4 116.57(7) . . ? C14 Ru3 Ru4 85.10(8) . . ? C15 Ru3 Ru4 53.61(8) . . ? Ru1 Ru3 Ru4 117.14(2) . . ? Ru2 Ru3 Ru4 56.663(19) . . ? C12 Ru4 C11 88.84(15) . . ? C12 Ru4 C10 92.76(15) . . ? C11 Ru4 C10 96.04(15) . . ? C12 Ru4 C16 91.17(14) . . ? C11 Ru4 C16 97.07(14) . . ? C10 Ru4 C16 166.38(13) . . ? C12 Ru4 C15 118.45(13) . . ? C11 Ru4 C15 116.32(12) . . ? C10 Ru4 C15 133.75(12) . . ? C16 Ru4 C15 34.74(10) . . ? C12 Ru4 Ru2 108.97(11) . . ? C11 Ru4 Ru2 159.36(10) . . ? C10 Ru4 Ru2 93.48(10) . . ? C16 Ru4 Ru2 72.92(9) . . ? C15 Ru4 Ru2 46.25(7) . . ? C12 Ru4 Ru3 165.93(11) . . ? C11 Ru4 Ru3 103.93(11) . . ? C10 Ru4 Ru3 91.74(10) . . ? C16 Ru4 Ru3 81.55(9) . . ? C15 Ru4 Ru3 50.57(7) . . ? Ru2 Ru4 Ru3 57.42(2) . . ? O1 C1 Ru1 177.2(3) . . ? O2 C2 Ru1 177.3(3) . . ? O3 C3 Ru1 178.4(3) . . ? O4 C4 Ru2 160.2(3) . . ? O4 C4 Ru1 123.4(3) . . ? Ru2 C4 Ru1 76.17(11) . . ? O5 C5 Ru2 178.7(3) . . ? O6 C6 Ru2 170.5(3) . . ? O7 C7 Ru3 176.4(3) . . ? O8 C8 Ru3 171.6(3) . . ? O9 C9 Ru3 168.7(3) . . ? O10 C10 Ru4 174.8(3) . . ? O11 C11 Ru4 178.7(3) . . ? O12 C12 Ru4 178.7(3) . . ? C14 C13 C18 116.9(3) . . ? C14 C13 Ru1 125.2(2) . . ? C18 C13 Ru1 117.8(2) . . ? C14 C13 Ru3 72.30(17) . . ? C18 C13 Ru3 126.12(18) . . ? Ru1 C13 Ru3 77.57(10) . . ? C13 C14 C15 119.9(3) . . ? C13 C14 C24 121.6(3) . . ? C15 C14 C24 118.2(3) . . ? C13 C14 Ru3 72.21(17) . . ? C15 C14 Ru3 75.72(17) . . ? C24 C14 Ru3 129.03(19) . . ? C16 C15 C14 123.2(3) . . ? C16 C15 Ru2 112.4(2) . . ? C14 C15 Ru2 124.1(2) . . ? C16 C15 Ru3 124.1(2) . . ? C14 C15 Ru3 68.87(16) . . ? Ru2 C15 Ru3 76.38(10) . . ? C16 C15 Ru4 57.06(17) . . ? C14 C15 Ru4 133.14(19) . . ? Ru2 C15 Ru4 73.37(9) . . ? Ru3 C15 Ru4 75.82(9) . . ? C17 C16 C15 133.5(3) . . ? C17 C16 Ru4 137.5(2) . . ? C15 C16 Ru4 88.2(2) . . ? C16 C17 C30 122.7(3) . . ? C16 C17 C36 122.1(3) . . ? C30 C17 C36 115.2(3) . . ? C19 C18 C23 117.3(3) . . ? C19 C18 C13 118.6(3) . . ? C23 C18 C13 124.1(3) . . ? C20 C19 C18 121.4(3) . . ? C21 C20 C19 120.5(3) . . ? C20 C21 C22 119.1(3) . . ? C21 C22 C23 120.5(3) . . ? C22 C23 C18 121.2(3) . . ? C29 C24 C25 118.1(3) . . ? C29 C24 C14 122.5(3) . . ? C25 C24 C14 119.3(3) . . ? C24 C25 C26 121.2(3) . . ? C27 C26 C25 119.4(3) . . ? C26 C27 C28 120.8(3) . . ? C27 C28 C29 119.6(3) . . ? C24 C29 C28 121.0(3) . . ? C31 C30 C35 117.9(3) . . ? C31 C30 C17 122.1(3) . . ? C35 C30 C17 120.0(3) . . ? C32 C31 C30 120.9(3) . . ? C33 C32 C31 120.5(3) . . ? C34 C33 C32 119.2(3) . . ? C33 C34 C35 120.5(3) . . ? C34 C35 C30 121.0(3) . . ? C37 C36 C41 118.2(3) . . ? C37 C36 C17 122.2(3) . . ? C41 C36 C17 119.6(3) . . ? C36 C37 C38 120.5(4) . . ? C39 C38 C37 119.7(4) . . ? C40 C39 C38 120.8(4) . . ? C39 C40 C41 120.2(4) . . ? C40 C41 C36 120.6(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.852 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.100