# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Brian James' _publ_contact_author_email brj@chem.ubc.ca loop_ _publ_author_name 'Brian James' 'Brian Patrick' 'Adam Wu' 'Enoch Chung' data_bj473 _database_code_depnum_ccdc_archive 'CCDC 883563' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H38 Cl2 O4 P2 Ru' _chemical_formula_weight 900.68 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.689(2) _cell_length_b 14.871(3) _cell_length_c 14.223(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.352(3) _cell_angle_gamma 90.00 _cell_volume 2022.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 90.0(1) _cell_measurement_reflns_used 9968 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 30.17 _exptl_crystal_description irregular _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(1) _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 'Bruker APEX DUO' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6130 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 30.08 _reflns_number_total 6130 _reflns_number_gt 5511 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0377P)^2^+2.3503P] 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 6130 _refine_ls_number_parameters 284 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 C1 C 0.45521(18) 0.02826(11) 0.19246(12) 0.0160(3) Uani 1 1 d . . . C2 C 0.59205(19) 0.02584(12) 0.17415(13) 0.0198(3) Uani 1 1 d . . . H2 H 0.6541 0.0741 0.1944 0.024 Uiso 1 1 calc R . . C3 C 0.6383(2) -0.04715(13) 0.12619(14) 0.0240(4) Uani 1 1 d . . . H3 H 0.7319 -0.0488 0.1143 0.029 Uiso 1 1 calc R . . C4 C 0.5477(2) -0.11729(13) 0.09593(14) 0.0243(4) Uani 1 1 d . . . H4 H 0.5786 -0.1662 0.0617 0.029 Uiso 1 1 calc R . . C5 C 0.4123(2) -0.11610(13) 0.11548(14) 0.0242(4) Uani 1 1 d . . . H5 H 0.3512 -0.1650 0.0959 0.029 Uiso 1 1 calc R . . C6 C 0.3656(2) -0.04403(13) 0.16338(13) 0.0213(3) Uani 1 1 d . . . H6 H 0.2726 -0.0436 0.1766 0.026 Uiso 1 1 calc R . . C7 C 0.21001(17) 0.13111(12) 0.18680(12) 0.0166(3) Uani 1 1 d . . . C8 C 0.1820(2) 0.12713(18) 0.08726(14) 0.0325(5) Uani 1 1 d . . . H8 H 0.2574 0.1268 0.0521 0.039 Uiso 1 1 calc R . . C9 C 0.0458(2) 0.12370(19) 0.03948(15) 0.0349(5) Uani 1 1 d . . . H9 H 0.0283 0.1201 -0.0281 0.042 Uiso 1 1 calc R . . C10 C -0.0647(2) 0.12554(15) 0.08953(15) 0.0282(4) Uani 1 1 d . . . H10 H -0.1581 0.1225 0.0568 0.034 Uiso 1 1 calc R . . C11 C -0.0384(2) 0.1319(2) 0.18754(16) 0.0376(6) Uani 1 1 d . . . H11 H -0.1143 0.1345 0.2222 0.045 Uiso 1 1 calc R . . C12 C 0.0989(2) 0.13453(17) 0.23634(14) 0.0292(5) Uani 1 1 d . . . H12 H 0.1159 0.1387 0.3039 0.035 Uiso 1 1 calc R . . C13 C 0.42005(17) 0.17070(12) 0.43650(12) 0.0153(3) Uani 1 1 d . . . C14 C 0.38079(17) 0.10347(12) 0.37002(12) 0.0157(3) Uani 1 1 d . . . C15 C 0.33193(19) 0.02302(12) 0.40414(13) 0.0201(3) Uani 1 1 d . . . H15 H 0.3042 -0.0252 0.3615 0.024 Uiso 1 1 calc R . . C16 C 0.32408(19) 0.01387(14) 0.50029(14) 0.0235(4) Uani 1 1 d . . . H16 H 0.2944 -0.0416 0.5234 0.028 Uiso 1 1 calc R . . C17 C 0.35916(19) 0.08518(14) 0.56350(13) 0.0227(4) Uani 1 1 d . . . H17 H 0.3502 0.0781 0.6286 0.027 Uiso 1 1 calc R . . C18 C 0.40724(18) 0.16677(13) 0.53252(12) 0.0186(3) Uani 1 1 d . . . C19 C 0.4485(3) 0.2500 0.59381(17) 0.0219(5) Uani 1 2 d S . . C20 C 0.6094(3) 0.2500 0.6244(2) 0.0294(6) Uani 1 2 d S . . C21 C 0.3768(3) 0.2500 0.68229(19) 0.0330(7) Uani 1 2 d S . . H21A H 0.4047 0.3038 0.7204 0.049 Uiso 0.50 1 calc PR . . H21B H 0.4048 0.1962 0.7205 0.049 Uiso 0.50 1 calc PR . . H21C H 0.2751 0.2500 0.6625 0.049 Uiso 1 2 calc SR . . C22 C 0.5811(2) 0.2500 0.14611(17) 0.0152(4) Uani 1 2 d S . . C23 C 0.79855(17) 0.29762(12) 0.38147(11) 0.0163(3) Uani 1 1 d . . . C24 C 0.91281(18) 0.34380(14) 0.43140(13) 0.0213(3) Uani 1 1 d . . . H24 H 0.9137 0.4077 0.4311 0.026 Uiso 1 1 calc R . . C25 C 1.02612(19) 0.29658(15) 0.48193(14) 0.0266(4) Uani 1 1 d . . . H25 H 1.1032 0.3285 0.5163 0.032 Uiso 1 1 calc R . . C26 C 0.0254(6) 0.7843(5) 0.2858(4) 0.0570(17) Uani 0.50 1 d PD A -1 H26A H 0.0914 0.7732 0.3454 0.068 Uiso 0.50 1 calc PR A -1 H26B H -0.0664 0.7584 0.2929 0.068 Uiso 0.50 1 calc PR A -1 O1 O 0.47641(18) 0.2500 0.40494(11) 0.0141(3) Uani 1 2 d S . . O2 O 0.6067(2) 0.2500 0.06953(13) 0.0226(4) Uani 1 2 d S . . O3 O 0.68952(12) 0.34107(8) 0.33062(8) 0.0158(2) Uani 1 1 d . . . P1 P 0.39156(4) 0.12911(3) 0.24549(3) 0.01316(9) Uani 1 1 d . . . Cl1 Cl 0.0866(2) 0.7338(5) 0.19125(11) 0.114(2) Uani 0.50 1 d PD A -1 Cl2 Cl 0.00850(17) 0.89950(14) 0.26499(12) 0.0616(4) Uani 0.50 1 d P A -1 Ru1 Ru 0.541692(18) 0.2500 0.266417(12) 0.01125(5) Uani 1 2 d S . . H20A H 0.659(4) 0.2500 0.566(3) 0.034(10) Uiso 1 2 d S . . H20B H 0.635(3) 0.1979(18) 0.6638(18) 0.032(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0180(7) 0.0154(7) 0.0145(7) -0.0016(6) 0.0025(6) 0.0007(6) C2 0.0190(8) 0.0192(8) 0.0216(8) -0.0040(6) 0.0043(6) -0.0011(6) C3 0.0241(9) 0.0233(9) 0.0264(9) -0.0049(7) 0.0096(7) 0.0016(7) C4 0.0324(10) 0.0198(8) 0.0220(8) -0.0057(7) 0.0087(7) 0.0007(7) C5 0.0305(10) 0.0189(8) 0.0232(9) -0.0048(7) 0.0038(7) -0.0051(7) C6 0.0219(8) 0.0200(8) 0.0219(8) -0.0022(7) 0.0033(7) -0.0040(7) C7 0.0141(7) 0.0168(7) 0.0179(7) -0.0002(6) -0.0005(6) -0.0009(6) C8 0.0191(9) 0.0605(15) 0.0175(9) 0.0078(9) 0.0017(7) -0.0029(9) C9 0.0243(10) 0.0582(15) 0.0193(9) 0.0041(9) -0.0045(7) -0.0010(10) C10 0.0157(8) 0.0352(11) 0.0307(10) -0.0047(8) -0.0053(7) -0.0001(7) C11 0.0139(8) 0.0693(17) 0.0291(10) -0.0169(11) 0.0019(7) 0.0004(9) C12 0.0154(8) 0.0512(13) 0.0205(9) -0.0122(9) 0.0017(7) -0.0002(8) C13 0.0132(7) 0.0183(7) 0.0141(7) 0.0040(6) 0.0013(5) 0.0010(6) C14 0.0135(7) 0.0180(8) 0.0156(7) 0.0027(6) 0.0022(6) 0.0018(6) C15 0.0191(8) 0.0177(8) 0.0238(8) 0.0042(7) 0.0042(6) 0.0009(6) C16 0.0197(8) 0.0242(9) 0.0279(9) 0.0114(7) 0.0077(7) 0.0026(7) C17 0.0196(8) 0.0315(10) 0.0173(8) 0.0110(7) 0.0038(6) 0.0047(7) C18 0.0149(7) 0.0281(9) 0.0123(7) 0.0035(6) 0.0004(6) 0.0028(6) C19 0.0204(12) 0.0330(14) 0.0112(10) 0.000 -0.0009(9) 0.000 C20 0.0238(13) 0.0392(17) 0.0217(13) 0.000 -0.0070(10) 0.000 C21 0.0346(16) 0.0512(19) 0.0130(12) 0.000 0.0035(11) 0.000 C22 0.0120(10) 0.0162(10) 0.0169(10) 0.000 0.0007(8) 0.000 C23 0.0136(7) 0.0220(8) 0.0133(7) -0.0005(6) 0.0022(5) -0.0001(6) C24 0.0165(8) 0.0266(9) 0.0202(8) -0.0036(7) 0.0012(6) -0.0037(7) C25 0.0151(8) 0.0401(11) 0.0229(9) -0.0027(8) -0.0019(6) -0.0035(8) C26 0.043(3) 0.080(5) 0.053(3) 0.001(3) 0.021(2) -0.003(3) O1 0.0159(8) 0.0154(8) 0.0111(7) 0.000 0.0024(6) 0.000 O2 0.0261(10) 0.0272(10) 0.0156(8) 0.000 0.0070(7) 0.000 O3 0.0127(5) 0.0169(6) 0.0169(5) -0.0006(4) -0.0006(4) -0.0018(4) P1 0.01205(18) 0.01459(19) 0.01265(18) -0.00047(14) 0.00143(14) -0.00035(14) Cl1 0.0713(10) 0.222(6) 0.0442(7) -0.049(2) -0.0074(7) 0.044(2) Cl2 0.0494(8) 0.0757(11) 0.0569(9) 0.0049(8) 0.0002(7) -0.0020(8) Ru1 0.01022(8) 0.01340(9) 0.00991(8) 0.000 0.00099(6) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.392(2) . ? C1 C6 1.401(2) . ? C1 P1 1.8301(17) . ? C2 C3 1.394(3) . ? C2 H2 0.9500 . ? C3 C4 1.386(3) . ? C3 H3 0.9500 . ? C4 C5 1.385(3) . ? C4 H4 0.9500 . ? C5 C6 1.385(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.380(3) . ? C7 C8 1.399(3) . ? C7 P1 1.8206(17) . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 C10 1.378(3) . ? C9 H9 0.9500 . ? C10 C11 1.379(3) . ? C10 H10 0.9500 . ? C11 C12 1.398(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.386(2) . ? C13 C18 1.392(2) . ? C13 O1 1.4035(19) . ? C14 C15 1.402(2) . ? C14 P1 1.8312(17) . ? C15 C16 1.389(3) . ? C15 H15 0.9500 . ? C16 C17 1.396(3) . ? C16 H16 0.9500 . ? C17 C18 1.397(3) . ? C17 H17 0.9500 . ? C18 C19 1.529(2) . ? C19 C18 1.529(2) 4_565 ? C19 C21 1.533(4) . ? C19 C20 1.549(4) . ? C20 H20A 1.02(4) . ? C20 H20B 0.96(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 O2 1.156(3) . ? C22 Ru1 1.813(2) . ? C23 O3 1.345(2) . ? C23 C24 1.395(2) . ? C23 C23 1.416(4) 4_565 ? C24 C25 1.399(3) . ? C24 H24 0.9500 . ? C25 C25 1.385(5) 4_565 ? C25 H25 0.9500 . ? C26 Cl1 1.727(6) . ? C26 Cl2 1.741(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O1 C13 1.4035(19) 4_565 ? O1 Ru1 2.1649(17) . ? O3 Ru1 2.0723(12) . ? P1 Ru1 2.3013(5) . ? Ru1 O3 2.0723(12) 4_565 ? Ru1 P1 2.3013(5) 4_565 ? 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 C1 C6 119.21(16) . . ? C2 C1 P1 119.55(13) . . ? C6 C1 P1 121.07(13) . . ? C1 C2 C3 120.20(17) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 120.04(18) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.04(17) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.32(18) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.16(17) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C12 C7 C8 118.65(17) . . ? C12 C7 P1 122.83(14) . . ? C8 C7 P1 118.51(14) . . ? C9 C8 C7 120.73(19) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 120.28(19) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.48(18) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C10 C11 C12 120.55(19) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C7 C12 C11 120.26(18) . . ? C7 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 C18 125.48(16) . . ? C14 C13 O1 117.76(15) . . ? C18 C13 O1 116.76(16) . . ? C13 C14 C15 116.74(16) . . ? C13 C14 P1 117.20(13) . . ? C15 C14 P1 126.02(14) . . ? C16 C15 C14 120.01(18) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.88(17) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C18 121.03(17) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C13 C18 C17 115.69(17) . . ? C13 C18 C19 117.93(17) . . ? C17 C18 C19 126.37(17) . . ? C18 C19 C18 108.1(2) . 4_565 ? C18 C19 C21 110.89(15) . . ? C18 C19 C21 110.89(15) 4_565 . ? C18 C19 C20 108.56(15) . . ? C18 C19 C20 108.56(15) 4_565 . ? C21 C19 C20 109.8(2) . . ? C19 C20 H20A 111(2) . . ? C19 C20 H20B 108.4(16) . . ? H20A C20 H20B 111.0(19) . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O2 C22 Ru1 179.8(2) . . ? O3 C23 C24 121.75(16) . . ? O3 C23 C23 118.72(9) . 4_565 ? C24 C23 C23 119.49(11) . 4_565 ? C23 C24 C25 120.39(18) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C25 C25 C24 120.12(12) 4_565 . ? C25 C25 H25 119.9 4_565 . ? C24 C25 H25 119.9 . . ? Cl1 C26 Cl2 109.3(4) . . ? Cl1 C26 H26A 109.8 . . ? Cl2 C26 H26A 109.8 . . ? Cl1 C26 H26B 109.8 . . ? Cl2 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? C13 O1 C13 114.32(18) 4_565 . ? C13 O1 Ru1 118.52(9) 4_565 . ? C13 O1 Ru1 118.52(9) . . ? C23 O3 Ru1 110.44(10) . . ? C7 P1 C1 100.93(8) . . ? C7 P1 C14 104.13(8) . . ? C1 P1 C14 107.69(8) . . ? C7 P1 Ru1 126.15(6) . . ? C1 P1 Ru1 116.44(6) . . ? C14 P1 Ru1 99.89(6) . . ? C22 Ru1 O3 100.33(6) . . ? C22 Ru1 O3 100.33(6) . 4_565 ? O3 Ru1 O3 81.62(7) . 4_565 ? C22 Ru1 O1 175.24(8) . . ? O3 Ru1 O1 83.24(5) . . ? O3 Ru1 O1 83.24(5) 4_565 . ? C22 Ru1 P1 95.95(5) . . ? O3 Ru1 P1 160.85(4) . . ? O3 Ru1 P1 85.61(4) 4_565 . ? O1 Ru1 P1 81.12(3) . . ? C22 Ru1 P1 95.95(5) . 4_565 ? O3 Ru1 P1 85.61(4) . 4_565 ? O3 Ru1 P1 160.85(4) 4_565 4_565 ? O1 Ru1 P1 81.12(3) . 4_565 ? P1 Ru1 P1 102.74(3) . 4_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.9(3) . . . . ? P1 C1 C2 C3 -174.34(15) . . . . ? C1 C2 C3 C4 0.5(3) . . . . ? C2 C3 C4 C5 -1.7(3) . . . . ? C3 C4 C5 C6 1.5(3) . . . . ? C4 C5 C6 C1 0.0(3) . . . . ? C2 C1 C6 C5 -1.2(3) . . . . ? P1 C1 C6 C5 174.03(14) . . . . ? C12 C7 C8 C9 -2.1(4) . . . . ? P1 C7 C8 C9 176.6(2) . . . . ? C7 C8 C9 C10 1.0(4) . . . . ? C8 C9 C10 C11 0.8(4) . . . . ? C9 C10 C11 C12 -1.3(4) . . . . ? C8 C7 C12 C11 1.5(3) . . . . ? P1 C7 C12 C11 -177.14(19) . . . . ? C10 C11 C12 C7 0.2(4) . . . . ? C18 C13 C14 C15 -4.0(3) . . . . ? O1 C13 C14 C15 176.62(15) . . . . ? C18 C13 C14 P1 173.92(14) . . . . ? O1 C13 C14 P1 -5.5(2) . . . . ? C13 C14 C15 C16 0.3(2) . . . . ? P1 C14 C15 C16 -177.37(14) . . . . ? C14 C15 C16 C17 2.5(3) . . . . ? C15 C16 C17 C18 -2.0(3) . . . . ? C14 C13 C18 C17 4.5(3) . . . . ? O1 C13 C18 C17 -176.14(15) . . . . ? C14 C13 C18 C19 -176.50(18) . . . . ? O1 C13 C18 C19 2.9(2) . . . . ? C16 C17 C18 C13 -1.3(3) . . . . ? C16 C17 C18 C19 179.73(19) . . . . ? C13 C18 C19 C18 35.7(3) . . . 4_565 ? C17 C18 C19 C18 -145.32(15) . . . 4_565 ? C13 C18 C19 C21 157.48(18) . . . . ? C17 C18 C19 C21 -23.6(3) . . . . ? C13 C18 C19 C20 -81.8(2) . . . . ? C17 C18 C19 C20 97.1(2) . . . . ? O3 C23 C24 C25 -178.55(16) . . . . ? C23 C23 C24 C25 -0.6(2) 4_565 . . . ? C23 C24 C25 C25 0.6(2) . . . 4_565 ? C14 C13 O1 C13 133.44(14) . . . 4_565 ? C18 C13 O1 C13 -46.0(2) . . . 4_565 ? C14 C13 O1 Ru1 -13.9(2) . . . . ? C18 C13 O1 Ru1 166.65(12) . . . . ? C24 C23 O3 Ru1 179.72(13) . . . . ? C23 C23 O3 Ru1 1.77(11) 4_565 . . . ? C12 C7 P1 C1 125.65(18) . . . . ? C8 C7 P1 C1 -52.98(18) . . . . ? C12 C7 P1 C14 14.07(19) . . . . ? C8 C7 P1 C14 -164.57(17) . . . . ? C12 C7 P1 Ru1 -99.71(17) . . . . ? C8 C7 P1 Ru1 81.65(18) . . . . ? C2 C1 P1 C7 144.98(14) . . . . ? C6 C1 P1 C7 -30.21(16) . . . . ? C2 C1 P1 C14 -106.20(15) . . . . ? C6 C1 P1 C14 78.61(16) . . . . ? C2 C1 P1 Ru1 4.90(16) . . . . ? C6 C1 P1 Ru1 -170.29(12) . . . . ? C13 C14 P1 C7 -112.27(14) . . . . ? C15 C14 P1 C7 65.41(17) . . . . ? C13 C14 P1 C1 141.13(13) . . . . ? C15 C14 P1 C1 -41.18(17) . . . . ? C13 C14 P1 Ru1 19.13(14) . . . . ? C15 C14 P1 Ru1 -163.19(14) . . . . ? O2 C22 Ru1 O3 41.63(8) . . . . ? O2 C22 Ru1 O3 -41.63(10) . . . 4_565 ? O2 C22 Ru1 O1 180.00(8) . . . . ? O2 C22 Ru1 P1 -128.24(9) . . . . ? O2 C22 Ru1 P1 128.24(8) . . . 4_565 ? C23 O3 Ru1 C22 -101.10(11) . . . . ? C23 O3 Ru1 O3 -2.05(12) . . . 4_565 ? C23 O3 Ru1 O1 82.08(10) . . . . ? C23 O3 Ru1 P1 46.67(17) . . . . ? C23 O3 Ru1 P1 163.64(10) . . . 4_565 ? C13 O1 Ru1 C22 -72.98(12) 4_565 . . . ? C13 O1 Ru1 C22 72.98(12) . . . . ? C13 O1 Ru1 O3 65.86(12) 4_565 . . . ? C13 O1 Ru1 O3 -148.17(13) . . . . ? C13 O1 Ru1 O3 148.17(13) 4_565 . . 4_565 ? C13 O1 Ru1 O3 -65.86(12) . . . 4_565 ? C13 O1 Ru1 P1 -125.23(13) 4_565 . . . ? C13 O1 Ru1 P1 20.73(12) . . . . ? C13 O1 Ru1 P1 -20.73(12) 4_565 . . 4_565 ? C13 O1 Ru1 P1 125.23(13) . . . 4_565 ? C7 P1 Ru1 C22 -78.67(9) . . . . ? C1 P1 Ru1 C22 50.05(8) . . . . ? C14 P1 Ru1 C22 165.59(8) . . . . ? C7 P1 Ru1 O3 133.17(13) . . . . ? C1 P1 Ru1 O3 -98.12(13) . . . . ? C14 P1 Ru1 O3 17.43(13) . . . . ? C7 P1 Ru1 O3 -178.62(8) . . . 4_565 ? C1 P1 Ru1 O3 -49.91(7) . . . 4_565 ? C14 P1 Ru1 O3 65.64(6) . . . 4_565 ? C7 P1 Ru1 O1 97.55(8) . . . . ? C1 P1 Ru1 O1 -133.74(7) . . . . ? C14 P1 Ru1 O1 -18.19(6) . . . . ? C7 P1 Ru1 P1 18.82(8) . . . 4_565 ? C1 P1 Ru1 P1 147.54(6) . . . 4_565 ? C14 P1 Ru1 P1 -96.92(6) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.034 _refine_diff_density_min -1.261 _refine_diff_density_rms 0.081 data_bj477_a _database_code_depnum_ccdc_archive 'CCDC 883564' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H44 O6 P2 Ru' _chemical_formula_weight 975.92 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' P P 0.1023 0.0942 '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3989(6) _cell_length_b 35.6883(19) _cell_length_c 12.4658(7) _cell_angle_alpha 90.00 _cell_angle_beta 116.6450(10) _cell_angle_gamma 90.00 _cell_volume 4532.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(2) _cell_measurement_reflns_used 9966 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.82 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.794 _exptl_absorpt_correction_T_max 0.963 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59917 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.91 _reflns_number_total 10803 _reflns_number_gt 8410 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0413P)^2^+5.9489P] 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 10803 _refine_ls_number_parameters 589 _refine_ls_number_restraints 199 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.002 _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 C1 C 0.8168(3) 0.87778(8) 0.6032(3) 0.0161(6) Uani 1 1 d U . . C2 C 0.7786(3) 0.91517(9) 0.5996(3) 0.0217(7) Uani 1 1 d U . . H2 H 0.6889 0.9220 0.5553 0.026 Uiso 1 1 calc R . . C3 C 0.8716(4) 0.94216(10) 0.6608(3) 0.0320(8) Uani 1 1 d U . . H3 H 0.8460 0.9677 0.6565 0.038 Uiso 1 1 calc R . . C4 C 1.0023(4) 0.93225(11) 0.7285(3) 0.0355(9) Uani 1 1 d U . . H4 H 1.0657 0.9509 0.7708 0.043 Uiso 1 1 calc R . . C5 C 1.0395(4) 0.89565(11) 0.7341(3) 0.0319(8) Uani 1 1 d U . . H5 H 1.1287 0.8889 0.7815 0.038 Uiso 1 1 calc R . . C6 C 0.9477(3) 0.86808(10) 0.6709(3) 0.0243(7) Uani 1 1 d U . . H6 H 0.9746 0.8427 0.6741 0.029 Uiso 1 1 calc R . . C7 C 0.7753(3) 0.79848(8) 0.5555(3) 0.0158(6) Uani 1 1 d U . . C8 C 0.8561(3) 0.78837(8) 0.5029(3) 0.0202(6) Uani 1 1 d U . . H8 H 0.8682 0.8052 0.4497 0.024 Uiso 1 1 calc R . . C9 C 0.9187(3) 0.75385(9) 0.5281(3) 0.0253(7) Uani 1 1 d U . . H9 H 0.9756 0.7472 0.4941 0.030 Uiso 1 1 calc R . . C10 C 0.8977(3) 0.72910(9) 0.6034(3) 0.0268(7) Uani 1 1 d U . . H10 H 0.9389 0.7052 0.6193 0.032 Uiso 1 1 calc R . . C11 C 0.8167(3) 0.73879(9) 0.6560(3) 0.0256(7) Uani 1 1 d U . . H11 H 0.8034 0.7217 0.7079 0.031 Uiso 1 1 calc R . . C12 C 0.7556(3) 0.77367(8) 0.6319(3) 0.0198(6) Uani 1 1 d U . . H12 H 0.7005 0.7805 0.6677 0.024 Uiso 1 1 calc R . . C13 C 0.4351(3) 0.84702(8) 0.4817(3) 0.0137(6) Uani 1 1 d U . . C14 C 0.5687(3) 0.84664(8) 0.5622(3) 0.0152(6) Uani 1 1 d U . . C15 C 0.6045(3) 0.84935(9) 0.6844(3) 0.0184(6) Uani 1 1 d U . . H15 H 0.6947 0.8501 0.7406 0.022 Uiso 1 1 calc R . . C16 C 0.5093(3) 0.85102(9) 0.7243(3) 0.0230(7) Uani 1 1 d U . . H16 H 0.5340 0.8525 0.8077 0.028 Uiso 1 1 calc R . . C17 C 0.3778(3) 0.85051(9) 0.6422(3) 0.0199(6) Uani 1 1 d U . . H17 H 0.3134 0.8515 0.6709 0.024 Uiso 1 1 calc R . . C18 C 0.3368(3) 0.84863(8) 0.5191(3) 0.0152(6) Uani 1 1 d U . . C19 C 0.1922(3) 0.84546(8) 0.4313(3) 0.0163(6) Uani 1 1 d U . . C20 C 0.1724(3) 0.85330(8) 0.3040(3) 0.0145(6) Uani 1 1 d U . . C21 C 0.0468(3) 0.86059(8) 0.2127(3) 0.0160(6) Uani 1 1 d U . . H21 H -0.0255 0.8611 0.2311 0.019 Uiso 1 1 calc R . . C22 C 0.0253(3) 0.86713(8) 0.0953(3) 0.0171(6) Uani 1 1 d U . . H22 H -0.0609 0.8719 0.0345 0.021 Uiso 1 1 calc R . . C23 C 0.1294(3) 0.86666(8) 0.0672(3) 0.0163(6) Uani 1 1 d U . . H23 H 0.1145 0.8721 -0.0125 0.020 Uiso 1 1 calc R . . C24 C 0.2563(3) 0.85838(8) 0.1543(3) 0.0147(6) Uani 1 1 d U . . C25 C 0.2747(3) 0.85226(8) 0.2727(3) 0.0124(5) Uani 1 1 d U . . C26 C 0.1082(3) 0.87319(11) 0.4624(3) 0.0278(8) Uani 1 1 d U . . H26A H 0.1276 0.8989 0.4474 0.042 Uiso 1 1 calc R . . H26B H 0.1286 0.8705 0.5472 0.042 Uiso 1 1 calc R . . H26C H 0.0149 0.8678 0.4123 0.042 Uiso 1 1 calc R . . C27 C 0.1474(4) 0.80517(10) 0.4373(3) 0.0287(8) Uani 1 1 d U . . H27A H 0.0561 0.8019 0.3768 0.043 Uiso 1 1 calc R . . H27B H 0.1541 0.8005 0.5173 0.043 Uiso 1 1 calc R . . H27C H 0.2035 0.7874 0.4216 0.043 Uiso 1 1 calc R . . C28 C 0.3644(3) 0.82162(8) 0.0047(3) 0.0176(6) Uani 1 1 d U . . C29 C 0.2412(3) 0.80877(9) -0.0763(3) 0.0238(7) Uani 1 1 d U . . H29 H 0.1651 0.8174 -0.0709 0.029 Uiso 1 1 calc R . . C30 C 0.2291(4) 0.78334(10) -0.1653(3) 0.0310(8) Uani 1 1 d U . . H30 H 0.1447 0.7747 -0.2207 0.037 Uiso 1 1 calc R . . C31 C 0.3401(4) 0.77056(9) -0.1732(3) 0.0318(8) Uani 1 1 d U . . H31 H 0.3313 0.7533 -0.2344 0.038 Uiso 1 1 calc R . . C32 C 0.4629(4) 0.78286(10) -0.0927(3) 0.0295(8) Uani 1 1 d U . . H32 H 0.5387 0.7740 -0.0979 0.035 Uiso 1 1 calc R . . C33 C 0.4754(3) 0.80830(9) -0.0041(3) 0.0219(7) Uani 1 1 d U . . H33 H 0.5601 0.8168 0.0513 0.026 Uiso 1 1 calc R . . C34 C 0.3725(3) 0.90123(8) 0.0340(3) 0.0151(6) Uani 1 1 d U . . C35 C 0.3813(3) 0.90235(10) -0.0737(3) 0.0230(7) Uani 1 1 d U . . H35 H 0.3929 0.8798 -0.1083 0.028 Uiso 1 1 calc R . . C36 C 0.3729(4) 0.93642(11) -0.1307(3) 0.0327(8) Uani 1 1 d U . . H36 H 0.3770 0.9370 -0.2052 0.039 Uiso 1 1 calc R . . C37 C 0.3588(3) 0.96941(10) -0.0801(3) 0.0323(8) Uani 1 1 d U . . H37 H 0.3555 0.9927 -0.1185 0.039 Uiso 1 1 calc R . . C38 C 0.3496(3) 0.96857(9) 0.0259(3) 0.0289(8) Uani 1 1 d U . . H38 H 0.3383 0.9913 0.0600 0.035 Uiso 1 1 calc R . . C39 C 0.3567(3) 0.93479(9) 0.0836(3) 0.0217(7) Uani 1 1 d U . . H39 H 0.3508 0.9345 0.1572 0.026 Uiso 1 1 calc R . . C40 C 0.6526(3) 0.92716(8) 0.3208(3) 0.0151(6) Uani 1 1 d U . . C41 C 0.7317(3) 0.90807(8) 0.2830(3) 0.0140(6) Uani 1 1 d U . . C42 C 0.7150(3) 0.86730(8) 0.2657(2) 0.0130(5) Uani 1 1 d U . . C43 C 0.6615(3) 0.96763(8) 0.3531(3) 0.0188(6) Uani 1 1 d U . . C44 C 0.5540(3) 0.98421(9) 0.3590(3) 0.0241(7) Uani 1 1 d U . . H44 H 0.4764 0.9700 0.3382 0.029 Uiso 1 1 calc R . . C45 C 0.5583(4) 1.02132(9) 0.3948(3) 0.0290(8) Uani 1 1 d U . . H45 H 0.4837 1.0323 0.3972 0.035 Uiso 1 1 calc R . . C46 C 0.6710(4) 1.04207(9) 0.4267(3) 0.0286(8) Uani 1 1 d U . . H46 H 0.6743 1.0674 0.4515 0.034 Uiso 1 1 calc R . . C47 C 0.7793(4) 1.02608(9) 0.4225(3) 0.0283(8) Uani 1 1 d U . . H47 H 0.8572 1.0404 0.4455 0.034 Uiso 1 1 calc R . . C48 C 0.7748(3) 0.98916(9) 0.3848(3) 0.0230(7) Uani 1 1 d U . . H48 H 0.8491 0.9785 0.3806 0.028 Uiso 1 1 calc R . . C49 C 0.8221(3) 0.93208(8) 0.1559(3) 0.0206(6) Uani 1 1 d U . . C50 C 0.7103(3) 0.92354(9) 0.0523(3) 0.0243(7) Uani 1 1 d U . . H50 H 0.6359 0.9134 0.0574 0.029 Uiso 1 1 calc R . . C51 C 0.7066(4) 0.92979(10) -0.0599(3) 0.0308(8) Uani 1 1 d U . . H51 H 0.6299 0.9234 -0.1306 0.037 Uiso 1 1 calc R . . C52 C 0.8091(4) 0.94465(10) -0.0694(3) 0.0303(8) Uani 1 1 d U . . H52 H 0.8058 0.9485 -0.1461 0.036 Uiso 1 1 calc R . . C53 C 0.9238(3) 0.95464(9) 0.0369(3) 0.0249(7) Uani 1 1 d U . . H53 H 0.9973 0.9651 0.0308 0.030 Uiso 1 1 calc R . . C54 C 0.9286(3) 0.94929(9) 0.1477(3) 0.0225(7) Uani 1 1 d U . . C55 C 1.1594(3) 0.95963(10) 0.2495(3) 0.0305(8) Uani 1 1 d U . . H55A H 1.1747 0.9376 0.2107 0.046 Uiso 1 1 calc R . . H55B H 1.2308 0.9621 0.3309 0.046 Uiso 1 1 calc R . . H55C H 1.1561 0.9821 0.2030 0.046 Uiso 1 1 calc R . . C56 C 0.5849(3) 0.80081(8) 0.2763(3) 0.0146(6) Uani 1 1 d U . . O1 O 0.40354(19) 0.84482(5) 0.35934(18) 0.0140(4) Uani 1 1 d U . . O2 O 0.5617(2) 0.90837(5) 0.33554(18) 0.0143(4) Uani 1 1 d U . . O3 O 0.7843(2) 0.84822(6) 0.23459(19) 0.0177(4) Uani 1 1 d U . . O4 O 0.8368(2) 0.92549(6) 0.2705(2) 0.0210(5) Uani 1 1 d U . . O5 O 1.0378(2) 0.95550(7) 0.2551(2) 0.0277(5) Uani 1 1 d U . . O6 O 0.5949(2) 0.76962(6) 0.2590(2) 0.0218(5) Uani 1 1 d U . . P1 P 0.69418(7) 0.84374(2) 0.50943(7) 0.01236(15) Uani 1 1 d U . . P2 P 0.39375(7) 0.85780(2) 0.11743(7) 0.01268(15) Uani 1 1 d U . . Ru1 Ru 0.57005(2) 0.851195(6) 0.30440(2) 0.01090(7) Uani 1 1 d U . . 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 C1 0.0169(15) 0.0189(14) 0.0135(14) -0.0010(11) 0.0075(12) -0.0035(11) C2 0.0274(18) 0.0207(15) 0.0163(15) -0.0007(12) 0.0093(14) -0.0012(13) C3 0.053(2) 0.0210(17) 0.0269(19) -0.0047(14) 0.0222(18) -0.0102(16) C4 0.044(2) 0.042(2) 0.0242(19) -0.0129(16) 0.0181(17) -0.0256(18) C5 0.0216(18) 0.050(2) 0.0237(18) -0.0059(16) 0.0097(15) -0.0109(16) C6 0.0195(17) 0.0315(18) 0.0230(17) -0.0036(14) 0.0106(13) -0.0029(13) C7 0.0141(15) 0.0143(13) 0.0174(15) 0.0025(11) 0.0055(12) 0.0008(11) C8 0.0211(17) 0.0167(15) 0.0258(17) 0.0066(12) 0.0131(14) 0.0049(12) C9 0.0235(18) 0.0227(16) 0.0332(19) 0.0040(14) 0.0158(15) 0.0088(13) C10 0.0260(19) 0.0152(15) 0.036(2) 0.0055(14) 0.0114(16) 0.0068(13) C11 0.0255(18) 0.0177(15) 0.0329(19) 0.0109(14) 0.0123(15) 0.0009(13) C12 0.0171(16) 0.0179(15) 0.0258(17) 0.0048(12) 0.0109(13) 0.0004(12) C13 0.0174(14) 0.0116(13) 0.0158(13) 0.0005(11) 0.0108(12) -0.0002(11) C14 0.0166(14) 0.0131(14) 0.0191(14) 0.0002(11) 0.0110(12) -0.0006(11) C15 0.0170(15) 0.0232(15) 0.0169(14) 0.0015(12) 0.0091(12) 0.0007(12) C16 0.0251(17) 0.0305(17) 0.0206(15) 0.0012(14) 0.0167(14) 0.0023(14) C17 0.0202(15) 0.0234(15) 0.0246(16) -0.0009(13) 0.0177(13) -0.0015(13) C18 0.0163(14) 0.0130(13) 0.0207(14) 0.0008(12) 0.0121(12) 0.0004(11) C19 0.0136(14) 0.0164(14) 0.0234(15) -0.0023(12) 0.0123(12) -0.0029(11) C20 0.0132(14) 0.0096(13) 0.0228(15) -0.0029(11) 0.0098(12) -0.0024(11) C21 0.0117(14) 0.0137(14) 0.0266(16) -0.0008(12) 0.0123(13) -0.0007(10) C22 0.0095(14) 0.0157(14) 0.0248(16) -0.0009(12) 0.0066(12) -0.0017(11) C23 0.0147(15) 0.0146(14) 0.0185(15) 0.0009(11) 0.0065(12) -0.0009(11) C24 0.0140(14) 0.0116(13) 0.0191(14) -0.0023(11) 0.0081(12) -0.0025(10) C25 0.0069(12) 0.0104(12) 0.0191(14) -0.0018(11) 0.0051(11) -0.0004(10) C26 0.0196(17) 0.043(2) 0.0247(18) -0.0072(15) 0.0133(15) 0.0054(15) C27 0.033(2) 0.0267(17) 0.0286(19) 0.0014(14) 0.0152(16) -0.0145(15) C28 0.0211(16) 0.0158(14) 0.0155(15) 0.0008(11) 0.0079(12) 0.0009(12) C29 0.0244(17) 0.0185(16) 0.0266(18) -0.0017(13) 0.0099(14) -0.0004(13) C30 0.037(2) 0.0236(17) 0.0267(19) -0.0059(14) 0.0089(16) -0.0075(15) C31 0.055(2) 0.0203(17) 0.0227(18) -0.0046(14) 0.0192(17) 0.0016(16) C32 0.040(2) 0.0281(18) 0.0265(18) 0.0002(14) 0.0203(17) 0.0081(15) C33 0.0241(17) 0.0232(16) 0.0206(16) -0.0005(13) 0.0120(14) 0.0025(13) C34 0.0095(14) 0.0173(14) 0.0160(14) 0.0029(11) 0.0037(11) -0.0021(11) C35 0.0227(17) 0.0295(17) 0.0194(16) 0.0042(13) 0.0118(14) -0.0009(13) C36 0.0262(19) 0.045(2) 0.0262(19) 0.0123(16) 0.0112(16) -0.0038(16) C37 0.0225(18) 0.0308(18) 0.037(2) 0.0178(16) 0.0080(16) -0.0025(15) C38 0.0258(19) 0.0188(16) 0.039(2) 0.0052(14) 0.0115(16) 0.0015(14) C39 0.0206(17) 0.0195(15) 0.0257(17) 0.0019(13) 0.0110(14) 0.0012(12) C40 0.0159(15) 0.0129(13) 0.0157(14) 0.0002(11) 0.0063(12) 0.0001(11) C41 0.0141(14) 0.0131(13) 0.0167(14) 0.0000(11) 0.0086(12) -0.0045(11) C42 0.0099(14) 0.0147(13) 0.0124(14) 0.0016(11) 0.0034(11) -0.0007(11) C43 0.0256(17) 0.0157(14) 0.0166(15) 0.0011(12) 0.0108(13) 0.0015(12) C44 0.0284(18) 0.0188(15) 0.0277(18) -0.0005(13) 0.0151(15) 0.0020(13) C45 0.040(2) 0.0200(16) 0.033(2) -0.0002(14) 0.0219(17) 0.0082(15) C46 0.051(2) 0.0128(15) 0.0268(18) -0.0022(13) 0.0212(17) 0.0008(14) C47 0.041(2) 0.0185(16) 0.0277(18) -0.0017(14) 0.0174(17) -0.0058(15) C48 0.0301(19) 0.0173(15) 0.0231(17) 0.0018(12) 0.0133(15) 0.0011(13) C49 0.0275(18) 0.0139(14) 0.0249(16) 0.0013(12) 0.0157(14) 0.0001(12) C50 0.0232(17) 0.0246(17) 0.0257(17) 0.0003(13) 0.0115(14) -0.0009(13) C51 0.029(2) 0.0264(18) 0.0295(19) 0.0018(15) 0.0067(16) -0.0018(15) C52 0.047(2) 0.0281(18) 0.0266(18) 0.0096(15) 0.0259(17) 0.0126(16) C53 0.0276(18) 0.0222(16) 0.0286(18) 0.0027(14) 0.0160(15) -0.0023(14) C54 0.0218(17) 0.0306(18) 0.0194(16) -0.0047(13) 0.0131(14) -0.0109(13) C55 0.0259(19) 0.0295(19) 0.041(2) -0.0043(16) 0.0200(17) -0.0068(15) C56 0.0119(14) 0.0198(15) 0.0164(14) 0.0015(11) 0.0101(12) -0.0015(11) O1 0.0110(10) 0.0189(10) 0.0146(10) -0.0001(8) 0.0080(8) 0.0004(8) O2 0.0154(10) 0.0131(9) 0.0175(10) 0.0001(8) 0.0101(9) 0.0017(8) O3 0.0168(11) 0.0150(10) 0.0281(12) -0.0038(9) 0.0160(9) -0.0012(8) O4 0.0205(12) 0.0227(11) 0.0239(12) -0.0009(9) 0.0137(10) -0.0044(9) O5 0.0249(13) 0.0299(13) 0.0326(13) -0.0027(11) 0.0167(11) -0.0062(10) O6 0.0291(13) 0.0136(11) 0.0259(12) -0.0015(9) 0.0152(10) -0.0006(9) P1 0.0117(4) 0.0121(3) 0.0147(4) 0.0018(3) 0.0072(3) 0.0008(3) P2 0.0118(4) 0.0136(4) 0.0140(4) -0.0004(3) 0.0070(3) -0.0003(3) Ru1 0.01101(11) 0.01025(11) 0.01399(11) 0.00041(9) 0.00788(9) 0.00064(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C6 1.389(4) . ? C1 C2 1.398(4) . ? C1 P1 1.825(3) . ? C2 C3 1.381(5) . ? C2 H2 0.9500 . ? C3 C4 1.389(6) . ? C3 H3 0.9500 . ? C4 C5 1.365(6) . ? C4 H4 0.9500 . ? C5 C6 1.395(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.391(4) . ? C7 C8 1.396(4) . ? C7 P1 1.821(3) . ? C8 C9 1.387(4) . ? C8 H8 0.9500 . ? C9 C10 1.385(5) . ? C9 H9 0.9500 . ? C10 C11 1.395(5) . ? C10 H10 0.9500 . ? C11 C12 1.392(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.395(4) . ? C13 C14 1.399(4) . ? C13 O1 1.403(3) . ? C14 C15 1.392(4) . ? C14 P1 1.825(3) . ? C15 C16 1.383(4) . ? C15 H15 0.9500 . ? C16 C17 1.386(5) . ? C16 H16 0.9500 . ? C17 C18 1.390(4) . ? C17 H17 0.9500 . ? C18 C19 1.520(4) . ? C19 C20 1.525(4) . ? C19 C27 1.539(4) . ? C19 C26 1.542(4) . ? C20 C25 1.388(4) . ? C20 C21 1.397(4) . ? C21 C22 1.391(4) . ? C21 H21 0.9500 . ? C22 C23 1.379(4) . ? C22 H22 0.9500 . ? C23 C24 1.397(4) . ? C23 H23 0.9500 . ? C24 C25 1.412(4) . ? C24 P2 1.819(3) . ? C25 O1 1.404(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.389(4) . ? C28 C33 1.401(4) . ? C28 P2 1.826(3) . ? C29 C30 1.391(5) . ? C29 H29 0.9500 . ? C30 C31 1.390(5) . ? C30 H30 0.9500 . ? C31 C32 1.378(5) . ? C31 H31 0.9500 . ? C32 C33 1.387(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.390(4) . ? C34 C39 1.396(4) . ? C34 P2 1.821(3) . ? C35 C36 1.390(5) . ? C35 H35 0.9500 . ? C36 C37 1.379(6) . ? C36 H36 0.9500 . ? C37 C38 1.372(5) . ? C37 H37 0.9500 . ? C38 C39 1.388(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 O2 1.314(3) . ? C40 C41 1.371(4) . ? C40 C43 1.491(4) . ? C41 O4 1.419(3) . ? C41 C42 1.471(4) . ? C42 O3 1.229(3) . ? C42 Ru1 2.003(3) . ? C43 C44 1.393(4) . ? C43 C48 1.399(5) . ? C44 C45 1.391(4) . ? C44 H44 0.9500 . ? C45 C46 1.378(5) . ? C45 H45 0.9500 . ? C46 C47 1.382(5) . ? C46 H46 0.9500 . ? C47 C48 1.392(4) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.381(5) . ? C49 O4 1.383(4) . ? C49 C54 1.405(4) . ? C50 C51 1.398(5) . ? C50 H50 0.9500 . ? C51 C52 1.336(5) . ? C51 H51 0.9500 . ? C52 C53 1.428(5) . ? C52 H52 0.9500 . ? C53 C54 1.370(4) . ? C53 H53 0.9500 . ? C54 O5 1.377(4) . ? C55 O5 1.426(4) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 O6 1.149(4) . ? C56 Ru1 1.854(3) . ? O1 Ru1 2.2999(19) . ? O2 Ru1 2.0871(19) . ? P1 Ru1 2.3156(8) . ? P2 Ru1 2.3076(8) . ? 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 C6 C1 C2 119.5(3) . . ? C6 C1 P1 121.9(2) . . ? C2 C1 P1 118.5(2) . . ? C3 C2 C1 119.8(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 120.4(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.6(4) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 119.8(3) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C12 C7 C8 120.0(3) . . ? C12 C7 P1 124.4(2) . . ? C8 C7 P1 115.5(2) . . ? C9 C8 C7 120.3(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 119.5(3) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.8(3) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 119.6(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C7 C12 C11 119.9(3) . . ? C7 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C18 C13 C14 122.7(3) . . ? C18 C13 O1 120.9(3) . . ? C14 C13 O1 116.4(2) . . ? C15 C14 C13 118.3(3) . . ? C15 C14 P1 120.4(2) . . ? C13 C14 P1 121.3(2) . . ? C16 C15 C14 120.3(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.9(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 122.1(3) . . ? C16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C17 C18 C13 116.7(3) . . ? C17 C18 C19 121.1(3) . . ? C13 C18 C19 122.0(3) . . ? C18 C19 C20 110.0(2) . . ? C18 C19 C27 108.1(3) . . ? C20 C19 C27 108.9(2) . . ? C18 C19 C26 111.5(3) . . ? C20 C19 C26 108.9(3) . . ? C27 C19 C26 109.3(3) . . ? C25 C20 C21 117.3(3) . . ? C25 C20 C19 122.5(3) . . ? C21 C20 C19 120.1(3) . . ? C22 C21 C20 121.4(3) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 121.0(3) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C25 117.5(3) . . ? C23 C24 P2 121.1(2) . . ? C25 C24 P2 121.4(2) . . ? C20 C25 O1 120.6(3) . . ? C20 C25 C24 122.8(3) . . ? O1 C25 C24 116.6(2) . . ? C19 C26 H26A 109.5 . . ? C19 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C19 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C19 C27 H27A 109.5 . . ? C19 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C19 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 119.1(3) . . ? C29 C28 P2 124.7(2) . . ? C33 C28 P2 116.1(2) . . ? C28 C29 C30 120.1(3) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.2(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C30 120.2(3) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 119.8(3) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C28 120.7(3) . . ? C32 C33 H33 119.7 . . ? C28 C33 H33 119.7 . . ? C35 C34 C39 118.9(3) . . ? C35 C34 P2 121.8(2) . . ? C39 C34 P2 119.1(2) . . ? C36 C35 C34 120.1(3) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C37 C36 C35 120.5(3) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C38 C37 C36 119.8(3) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C39 120.4(3) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C34 120.3(3) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? O2 C40 C41 118.4(3) . . ? O2 C40 C43 114.8(3) . . ? C41 C40 C43 126.8(3) . . ? C40 C41 O4 122.5(3) . . ? C40 C41 C42 118.7(3) . . ? O4 C41 C42 118.5(2) . . ? O3 C42 C41 122.4(3) . . ? O3 C42 Ru1 129.3(2) . . ? C41 C42 Ru1 108.35(19) . . ? C44 C43 C48 118.4(3) . . ? C44 C43 C40 118.1(3) . . ? C48 C43 C40 123.4(3) . . ? C45 C44 C43 121.0(3) . . ? C45 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? C46 C45 C44 119.9(3) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.0(3) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C48 120.4(3) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C47 C48 C43 120.3(3) . . ? C47 C48 H48 119.9 . . ? C43 C48 H48 119.9 . . ? C50 C49 O4 124.2(3) . . ? C50 C49 C54 119.6(3) . . ? O4 C49 C54 116.2(3) . . ? C49 C50 C51 120.1(3) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C52 C51 C50 121.1(3) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C51 C52 C53 119.3(3) . . ? C51 C52 H52 120.3 . . ? C53 C52 H52 120.3 . . ? C54 C53 C52 120.5(3) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C53 C54 O5 124.6(3) . . ? C53 C54 C49 119.3(3) . . ? O5 C54 C49 115.7(3) . . ? O5 C55 H55A 109.5 . . ? O5 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O5 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O6 C56 Ru1 179.6(2) . . ? C13 O1 C25 119.7(2) . . ? C13 O1 Ru1 118.34(16) . . ? C25 O1 Ru1 118.03(16) . . ? C40 O2 Ru1 111.63(17) . . ? C49 O4 C41 118.1(2) . . ? C54 O5 C55 116.3(3) . . ? C7 P1 C1 104.71(14) . . ? C7 P1 C14 107.79(14) . . ? C1 P1 C14 103.31(14) . . ? C7 P1 Ru1 114.98(10) . . ? C1 P1 Ru1 122.94(10) . . ? C14 P1 Ru1 101.64(10) . . ? C24 P2 C34 103.04(13) . . ? C24 P2 C28 108.72(14) . . ? C34 P2 C28 103.33(14) . . ? C24 P2 Ru1 101.81(10) . . ? C34 P2 Ru1 119.76(10) . . ? C28 P2 Ru1 118.77(10) . . ? C56 Ru1 C42 94.43(12) . . ? C56 Ru1 O2 177.23(10) . . ? C42 Ru1 O2 82.85(10) . . ? C56 Ru1 O1 96.79(10) . . ? C42 Ru1 O1 168.73(9) . . ? O2 Ru1 O1 85.93(7) . . ? C56 Ru1 P2 91.16(9) . . ? C42 Ru1 P2 99.57(8) . . ? O2 Ru1 P2 89.79(6) . . ? O1 Ru1 P2 81.36(5) . . ? C56 Ru1 P1 92.00(9) . . ? C42 Ru1 P1 97.89(8) . . ? O2 Ru1 P1 87.89(6) . . ? O1 Ru1 P1 80.64(5) . . ? P2 Ru1 P1 161.96(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.7(5) . . . . ? P1 C1 C2 C3 -174.0(2) . . . . ? C1 C2 C3 C4 -1.8(5) . . . . ? C2 C3 C4 C5 0.5(5) . . . . ? C3 C4 C5 C6 1.0(5) . . . . ? C2 C1 C6 C5 -0.2(5) . . . . ? P1 C1 C6 C5 175.3(3) . . . . ? C4 C5 C6 C1 -1.1(5) . . . . ? C12 C7 C8 C9 -1.1(5) . . . . ? P1 C7 C8 C9 -177.6(3) . . . . ? C7 C8 C9 C10 1.7(5) . . . . ? C8 C9 C10 C11 -1.4(5) . . . . ? C9 C10 C11 C12 0.4(5) . . . . ? C8 C7 C12 C11 0.1(5) . . . . ? P1 C7 C12 C11 176.3(3) . . . . ? C10 C11 C12 C7 0.2(5) . . . . ? C18 C13 C14 C15 -2.4(4) . . . . ? O1 C13 C14 C15 179.0(2) . . . . ? C18 C13 C14 P1 179.0(2) . . . . ? O1 C13 C14 P1 0.4(3) . . . . ? C13 C14 C15 C16 2.3(4) . . . . ? P1 C14 C15 C16 -179.1(2) . . . . ? C14 C15 C16 C17 -0.9(5) . . . . ? C15 C16 C17 C18 -0.5(5) . . . . ? C16 C17 C18 C13 0.4(4) . . . . ? C16 C17 C18 C19 175.8(3) . . . . ? C14 C13 C18 C17 1.1(4) . . . . ? O1 C13 C18 C17 179.6(2) . . . . ? C14 C13 C18 C19 -174.3(3) . . . . ? O1 C13 C18 C19 4.2(4) . . . . ? C17 C18 C19 C20 166.5(3) . . . . ? C13 C18 C19 C20 -18.4(4) . . . . ? C17 C18 C19 C27 -74.7(3) . . . . ? C13 C18 C19 C27 100.5(3) . . . . ? C17 C18 C19 C26 45.5(4) . . . . ? C13 C18 C19 C26 -139.3(3) . . . . ? C18 C19 C20 C25 17.2(4) . . . . ? C27 C19 C20 C25 -101.1(3) . . . . ? C26 C19 C20 C25 139.8(3) . . . . ? C18 C19 C20 C21 -165.1(3) . . . . ? C27 C19 C20 C21 76.6(3) . . . . ? C26 C19 C20 C21 -42.6(4) . . . . ? C25 C20 C21 C22 -1.0(4) . . . . ? C19 C20 C21 C22 -178.8(3) . . . . ? C20 C21 C22 C23 -0.3(4) . . . . ? C21 C22 C23 C24 2.3(4) . . . . ? C22 C23 C24 C25 -2.9(4) . . . . ? C22 C23 C24 P2 -179.9(2) . . . . ? C21 C20 C25 O1 -179.5(2) . . . . ? C19 C20 C25 O1 -1.8(4) . . . . ? C21 C20 C25 C24 0.3(4) . . . . ? C19 C20 C25 C24 178.0(3) . . . . ? C23 C24 C25 C20 1.6(4) . . . . ? P2 C24 C25 C20 178.6(2) . . . . ? C23 C24 C25 O1 -178.6(2) . . . . ? P2 C24 C25 O1 -1.5(3) . . . . ? C33 C28 C29 C30 -0.7(5) . . . . ? P2 C28 C29 C30 174.6(3) . . . . ? C28 C29 C30 C31 0.3(5) . . . . ? C29 C30 C31 C32 0.3(5) . . . . ? C30 C31 C32 C33 -0.5(5) . . . . ? C31 C32 C33 C28 0.1(5) . . . . ? C29 C28 C33 C32 0.5(5) . . . . ? P2 C28 C33 C32 -175.2(3) . . . . ? C39 C34 C35 C36 -0.6(5) . . . . ? P2 C34 C35 C36 -175.8(3) . . . . ? C34 C35 C36 C37 1.4(5) . . . . ? C35 C36 C37 C38 -1.7(5) . . . . ? C36 C37 C38 C39 1.1(5) . . . . ? C37 C38 C39 C34 -0.4(5) . . . . ? C35 C34 C39 C38 0.1(5) . . . . ? P2 C34 C39 C38 175.5(3) . . . . ? O2 C40 C41 O4 -176.6(2) . . . . ? C43 C40 C41 O4 0.4(5) . . . . ? O2 C40 C41 C42 -2.5(4) . . . . ? C43 C40 C41 C42 174.6(3) . . . . ? C40 C41 C42 O3 -178.3(3) . . . . ? O4 C41 C42 O3 -4.0(4) . . . . ? C40 C41 C42 Ru1 0.4(3) . . . . ? O4 C41 C42 Ru1 174.8(2) . . . . ? O2 C40 C43 C44 -19.3(4) . . . . ? C41 C40 C43 C44 163.5(3) . . . . ? O2 C40 C43 C48 156.6(3) . . . . ? C41 C40 C43 C48 -20.5(5) . . . . ? C48 C43 C44 C45 0.4(5) . . . . ? C40 C43 C44 C45 176.5(3) . . . . ? C43 C44 C45 C46 -0.9(5) . . . . ? C44 C45 C46 C47 0.3(5) . . . . ? C45 C46 C47 C48 0.8(5) . . . . ? C46 C47 C48 C43 -1.3(5) . . . . ? C44 C43 C48 C47 0.7(5) . . . . ? C40 C43 C48 C47 -175.2(3) . . . . ? O4 C49 C50 C51 -177.3(3) . . . . ? C54 C49 C50 C51 4.1(5) . . . . ? C49 C50 C51 C52 -1.2(5) . . . . ? C50 C51 C52 C53 -0.7(5) . . . . ? C51 C52 C53 C54 -0.4(5) . . . . ? C52 C53 C54 O5 175.1(3) . . . . ? C52 C53 C54 C49 3.2(5) . . . . ? C50 C49 C54 C53 -5.1(5) . . . . ? O4 C49 C54 C53 176.2(3) . . . . ? C50 C49 C54 O5 -177.6(3) . . . . ? O4 C49 C54 O5 3.7(4) . . . . ? C18 C13 O1 C25 13.7(4) . . . . ? C14 C13 O1 C25 -167.7(2) . . . . ? C18 C13 O1 Ru1 171.0(2) . . . . ? C14 C13 O1 Ru1 -10.4(3) . . . . ? C20 C25 O1 C13 -14.8(4) . . . . ? C24 C25 O1 C13 165.3(2) . . . . ? C20 C25 O1 Ru1 -172.2(2) . . . . ? C24 C25 O1 Ru1 7.9(3) . . . . ? C41 C40 O2 Ru1 3.1(3) . . . . ? C43 C40 O2 Ru1 -174.27(19) . . . . ? C50 C49 O4 C41 1.5(4) . . . . ? C54 C49 O4 C41 -179.9(3) . . . . ? C40 C41 O4 C49 -107.5(3) . . . . ? C42 C41 O4 C49 78.4(3) . . . . ? C53 C54 O5 C55 -14.4(5) . . . . ? C49 C54 O5 C55 157.7(3) . . . . ? C12 C7 P1 C1 101.1(3) . . . . ? C8 C7 P1 C1 -82.5(3) . . . . ? C12 C7 P1 C14 -8.4(3) . . . . ? C8 C7 P1 C14 167.9(2) . . . . ? C12 C7 P1 Ru1 -120.9(3) . . . . ? C8 C7 P1 Ru1 55.4(3) . . . . ? C6 C1 P1 C7 12.4(3) . . . . ? C2 C1 P1 C7 -172.1(2) . . . . ? C6 C1 P1 C14 125.1(3) . . . . ? C2 C1 P1 C14 -59.4(3) . . . . ? C6 C1 P1 Ru1 -121.3(2) . . . . ? C2 C1 P1 Ru1 54.2(3) . . . . ? C15 C14 P1 C7 68.9(3) . . . . ? C13 C14 P1 C7 -112.5(2) . . . . ? C15 C14 P1 C1 -41.6(3) . . . . ? C13 C14 P1 C1 137.0(2) . . . . ? C15 C14 P1 Ru1 -169.9(2) . . . . ? C13 C14 P1 Ru1 8.7(2) . . . . ? C23 C24 P2 C34 47.3(3) . . . . ? C25 C24 P2 C34 -129.7(2) . . . . ? C23 C24 P2 C28 -61.9(3) . . . . ? C25 C24 P2 C28 121.2(2) . . . . ? C23 C24 P2 Ru1 171.9(2) . . . . ? C25 C24 P2 Ru1 -5.0(2) . . . . ? C35 C34 P2 C24 -133.2(3) . . . . ? C39 C34 P2 C24 51.6(3) . . . . ? C35 C34 P2 C28 -20.0(3) . . . . ? C39 C34 P2 C28 164.8(2) . . . . ? C35 C34 P2 Ru1 114.8(2) . . . . ? C39 C34 P2 Ru1 -60.4(3) . . . . ? C29 C28 P2 C24 26.0(3) . . . . ? C33 C28 P2 C24 -158.7(2) . . . . ? C29 C28 P2 C34 -83.0(3) . . . . ? C33 C28 P2 C34 92.4(3) . . . . ? C29 C28 P2 Ru1 141.6(2) . . . . ? C33 C28 P2 Ru1 -43.0(3) . . . . ? O6 C56 Ru1 C42 31(38) . . . . ? O6 C56 Ru1 O2 21(40) . . . . ? O6 C56 Ru1 O1 -147(38) . . . . ? O6 C56 Ru1 P2 131(38) . . . . ? O6 C56 Ru1 P1 -67(38) . . . . ? O3 C42 Ru1 C56 0.1(3) . . . . ? C41 C42 Ru1 C56 -178.6(2) . . . . ? O3 C42 Ru1 O2 179.6(3) . . . . ? C41 C42 Ru1 O2 0.92(19) . . . . ? O3 C42 Ru1 O1 174.4(3) . . . . ? C41 C42 Ru1 O1 -4.3(6) . . . . ? O3 C42 Ru1 P2 -91.8(3) . . . . ? C41 C42 Ru1 P2 89.49(19) . . . . ? O3 C42 Ru1 P1 92.7(3) . . . . ? C41 C42 Ru1 P1 -85.94(19) . . . . ? C40 O2 Ru1 C56 8(2) . . . . ? C40 O2 Ru1 C42 -2.23(19) . . . . ? C40 O2 Ru1 O1 176.75(19) . . . . ? C40 O2 Ru1 P2 -101.90(18) . . . . ? C40 O2 Ru1 P1 95.99(18) . . . . ? C13 O1 Ru1 C56 103.45(19) . . . . ? C25 O1 Ru1 C56 -98.87(19) . . . . ? C13 O1 Ru1 C42 -70.8(5) . . . . ? C25 O1 Ru1 C42 86.9(5) . . . . ? C13 O1 Ru1 O2 -76.00(18) . . . . ? C25 O1 Ru1 O2 81.68(18) . . . . ? C13 O1 Ru1 P2 -166.41(18) . . . . ? C25 O1 Ru1 P2 -8.73(17) . . . . ? C13 O1 Ru1 P1 12.53(17) . . . . ? C25 O1 Ru1 P1 170.21(18) . . . . ? C24 P2 Ru1 C56 102.80(12) . . . . ? C34 P2 Ru1 C56 -144.55(14) . . . . ? C28 P2 Ru1 C56 -16.46(14) . . . . ? C24 P2 Ru1 C42 -162.52(12) . . . . ? C34 P2 Ru1 C42 -49.86(14) . . . . ? C28 P2 Ru1 C42 78.22(14) . . . . ? C24 P2 Ru1 O2 -79.81(11) . . . . ? C34 P2 Ru1 O2 32.85(13) . . . . ? C28 P2 Ru1 O2 160.93(13) . . . . ? C24 P2 Ru1 O1 6.11(10) . . . . ? C34 P2 Ru1 O1 118.76(13) . . . . ? C28 P2 Ru1 O1 -113.15(13) . . . . ? C24 P2 Ru1 P1 2.72(14) . . . . ? C34 P2 Ru1 P1 115.38(14) . . . . ? C28 P2 Ru1 P1 -116.54(14) . . . . ? C7 P1 Ru1 C56 10.16(14) . . . . ? C1 P1 Ru1 C56 139.62(15) . . . . ? C14 P1 Ru1 C56 -105.95(13) . . . . ? C7 P1 Ru1 C42 -84.59(14) . . . . ? C1 P1 Ru1 C42 44.87(15) . . . . ? C14 P1 Ru1 C42 159.30(12) . . . . ? C7 P1 Ru1 O2 -167.07(12) . . . . ? C1 P1 Ru1 O2 -37.61(13) . . . . ? C14 P1 Ru1 O2 76.82(11) . . . . ? C7 P1 Ru1 O1 106.71(12) . . . . ? C1 P1 Ru1 O1 -123.83(13) . . . . ? C14 P1 Ru1 O1 -9.40(10) . . . . ? C7 P1 Ru1 P2 110.10(13) . . . . ? C1 P1 Ru1 P2 -120.44(14) . . . . ? C14 P1 Ru1 P2 -6.01(14) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.032 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.100 data_bj479 _database_code_depnum_ccdc_archive 'CCDC 883565' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H18 O5' _chemical_formula_weight 302.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.4510(3) _cell_length_b 15.0943(9) _cell_length_c 18.1232(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.661(2) _cell_angle_gamma 90.00 _cell_volume 1488.12(15) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(1) _cell_measurement_reflns_used 9894 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 67.63 _exptl_crystal_description blade _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details 'SADABS, Sheldrick (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX DUO' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27645 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 67.96 _reflns_number_total 5231 _reflns_number_gt 5181 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0696P)^2^+0.2186P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.15(11) _refine_ls_number_reflns 5231 _refine_ls_number_parameters 409 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 C1 C 0.6887(3) 1.13343(10) 0.29844(8) 0.0151(3) Uani 1 1 d . . . C2 C 0.5233(3) 1.17433(10) 0.34292(9) 0.0169(3) Uani 1 1 d . . . H2 H 0.3897 1.2075 0.3209 0.020 Uiso 1 1 calc R . . C3 C 0.5526(3) 1.16695(11) 0.41923(9) 0.0191(3) Uani 1 1 d . . . H3 H 0.4401 1.1957 0.4492 0.023 Uiso 1 1 calc R . . C4 C 0.7448(3) 1.11796(11) 0.45198(9) 0.0196(3) Uani 1 1 d . . . H4 H 0.7629 1.1123 0.5042 0.024 Uiso 1 1 calc R . . C5 C 0.9112(3) 1.07714(11) 0.40782(9) 0.0190(3) Uani 1 1 d . . . H5 H 1.0443 1.0439 0.4300 0.023 Uiso 1 1 calc R . . C6 C 0.8831(3) 1.08485(10) 0.33136(9) 0.0174(3) Uani 1 1 d . . . H6 H 0.9971 1.0568 0.3014 0.021 Uiso 1 1 calc R . . C7 C 0.6475(3) 1.13879(10) 0.21519(8) 0.0156(3) Uani 1 1 d . . . H7 H 0.8000 1.1200 0.1916 0.019 Uiso 1 1 calc R . . C8 C 0.4339(3) 1.07823(10) 0.18952(8) 0.0145(3) Uani 1 1 d . . . H8 H 0.2873 1.0919 0.2180 0.017 Uiso 1 1 calc R . . C9 C 0.3700(3) 1.09166(10) 0.10711(8) 0.0160(3) Uani 1 1 d . . . C10 C 0.0717(3) 1.15106(13) 0.02117(9) 0.0264(4) Uani 1 1 d . . . H10A H 0.1859 1.1930 0.0003 0.040 Uiso 1 1 calc R . . H10B H -0.0934 1.1770 0.0193 0.040 Uiso 1 1 calc R . . H10C H 0.0682 1.0961 -0.0076 0.040 Uiso 1 1 calc R . . C11 C 0.3470(3) 0.93863(10) 0.24147(8) 0.0154(3) Uani 1 1 d . . . C12 C 0.1432(3) 0.90178(10) 0.20173(8) 0.0164(3) Uani 1 1 d . . . C13 C -0.0207(3) 0.85013(10) 0.23878(9) 0.0187(3) Uani 1 1 d . . . H13 H -0.1587 0.8241 0.2124 0.022 Uiso 1 1 calc R . . C14 C 0.0183(3) 0.83672(11) 0.31466(9) 0.0198(3) Uani 1 1 d . . . H14 H -0.0945 0.8018 0.3400 0.024 Uiso 1 1 calc R . . C15 C 0.2193(3) 0.87368(11) 0.35355(9) 0.0190(3) Uani 1 1 d . . . H15 H 0.2443 0.8642 0.4053 0.023 Uiso 1 1 calc R . . C16 C 0.3853(3) 0.92492(11) 0.31663(9) 0.0175(3) Uani 1 1 d . . . H16 H 0.5241 0.9503 0.3431 0.021 Uiso 1 1 calc R . . C17 C -0.0954(3) 0.89262(12) 0.08684(9) 0.0236(3) Uani 1 1 d . . . H17A H -0.0999 0.8277 0.0855 0.035 Uiso 1 1 calc R . . H17B H -0.0960 0.9157 0.0363 0.035 Uiso 1 1 calc R . . H17C H -0.2398 0.9148 0.1105 0.035 Uiso 1 1 calc R . . O1 O 0.5774(2) 1.22558(7) 0.19018(6) 0.0189(2) Uani 1 1 d . . . O2 O 0.51286(18) 0.98938(7) 0.20436(6) 0.0158(2) Uani 1 1 d . . . O3 O 0.50020(19) 1.07189(8) 0.05867(6) 0.0210(2) Uani 1 1 d . . . O4 O 0.15204(19) 1.13208(7) 0.09708(6) 0.0193(2) Uani 1 1 d . . . O5 O 0.12360(19) 0.92129(8) 0.12813(6) 0.0210(2) Uani 1 1 d . . . H1O H 0.701(5) 1.2546(17) 0.1901(14) 0.036(6) Uiso 1 1 d . . . C18 C 0.2024(3) 0.38030(10) 0.32696(8) 0.0158(3) Uani 1 1 d . . . C19 C 0.0356(3) 0.33496(11) 0.36868(9) 0.0185(3) Uani 1 1 d . . . H19 H -0.0978 0.3037 0.3445 0.022 Uiso 1 1 calc R . . C20 C 0.0640(3) 0.33543(11) 0.44525(9) 0.0200(3) Uani 1 1 d . . . H20 H -0.0499 0.3043 0.4732 0.024 Uiso 1 1 calc R . . C21 C 0.2573(3) 0.38093(11) 0.48143(9) 0.0209(3) Uani 1 1 d . . . H21 H 0.2756 0.3813 0.5339 0.025 Uiso 1 1 calc R . . C22 C 0.4241(3) 0.42603(11) 0.44022(9) 0.0201(3) Uani 1 1 d . . . H22 H 0.5578 0.4570 0.4645 0.024 Uiso 1 1 calc R . . C23 C 0.3954(3) 0.42581(11) 0.36357(9) 0.0181(3) Uani 1 1 d . . . H23 H 0.5091 0.4572 0.3358 0.022 Uiso 1 1 calc R . . C24 C 0.1624(3) 0.38400(10) 0.24372(8) 0.0159(3) Uani 1 1 d . . . H24 H 0.3162 0.4052 0.2221 0.019 Uiso 1 1 calc R . . C25 C -0.0488(3) 0.44772(10) 0.22163(8) 0.0147(3) Uani 1 1 d . . . H25 H -0.1961 0.4321 0.2492 0.018 Uiso 1 1 calc R . . C26 C -0.1133(3) 0.44175(10) 0.13889(9) 0.0164(3) Uani 1 1 d . . . C27 C -0.4104(3) 0.38644(12) 0.04984(9) 0.0253(4) Uani 1 1 d . . . H27A H -0.4272 0.4437 0.0245 0.038 Uiso 1 1 calc R . . H27B H -0.5695 0.3560 0.0470 0.038 Uiso 1 1 calc R . . H27C H -0.2891 0.3500 0.0261 0.038 Uiso 1 1 calc R . . C28 C -0.1323(3) 0.58227(10) 0.28211(8) 0.0157(3) Uani 1 1 d . . . C29 C -0.3366(3) 0.62298(10) 0.24533(9) 0.0170(3) Uani 1 1 d . . . C30 C -0.4991(3) 0.66997(10) 0.28656(9) 0.0185(3) Uani 1 1 d . . . H30 H -0.6381 0.6983 0.2626 0.022 Uiso 1 1 calc R . . C31 C -0.4577(3) 0.67548(10) 0.36296(9) 0.0183(3) Uani 1 1 d . . . H31 H -0.5709 0.7070 0.3909 0.022 Uiso 1 1 calc R . . C32 C -0.2545(3) 0.63585(10) 0.39900(9) 0.0189(3) Uani 1 1 d . . . H32 H -0.2270 0.6408 0.4511 0.023 Uiso 1 1 calc R . . C33 C -0.0908(3) 0.58867(10) 0.35784(9) 0.0168(3) Uani 1 1 d . . . H33 H 0.0489 0.5610 0.3819 0.020 Uiso 1 1 calc R . . C34 C -0.5708(3) 0.64681(13) 0.13136(9) 0.0244(3) Uani 1 1 d . . . H34A H -0.7184 0.6211 0.1510 0.037 Uiso 1 1 calc R . . H34B H -0.5668 0.6322 0.0788 0.037 Uiso 1 1 calc R . . H34C H -0.5736 0.7113 0.1374 0.037 Uiso 1 1 calc R . . O6 O 0.0925(2) 0.30016(7) 0.21163(6) 0.0192(2) Uani 1 1 d . . . O7 O 0.03301(19) 0.53491(7) 0.24187(6) 0.0160(2) Uani 1 1 d . . . O8 O 0.0155(2) 0.46755(8) 0.09178(6) 0.0216(2) Uani 1 1 d . . . O9 O -0.32966(19) 0.40073(7) 0.12662(6) 0.0182(2) Uani 1 1 d . . . O10 O -0.3567(2) 0.61137(8) 0.17076(6) 0.0224(3) Uani 1 1 d . . . H6O H 0.232(4) 0.2776(16) 0.1984(12) 0.032(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0136(7) 0.0150(7) 0.0167(7) -0.0008(6) 0.0006(5) -0.0037(6) C2 0.0135(7) 0.0164(8) 0.0208(8) 0.0009(6) 0.0008(6) 0.0007(5) C3 0.0196(7) 0.0202(8) 0.0181(7) -0.0018(6) 0.0048(6) -0.0013(6) C4 0.0221(8) 0.0215(8) 0.0152(7) -0.0003(6) 0.0000(6) -0.0033(6) C5 0.0149(7) 0.0207(8) 0.0210(8) 0.0005(6) -0.0025(6) 0.0002(6) C6 0.0131(7) 0.0179(8) 0.0211(7) -0.0014(6) 0.0014(5) -0.0019(6) C7 0.0147(7) 0.0159(7) 0.0163(7) 0.0002(6) 0.0023(5) 0.0000(6) C8 0.0129(7) 0.0145(7) 0.0162(7) -0.0008(6) 0.0024(5) 0.0010(6) C9 0.0156(7) 0.0142(7) 0.0182(7) 0.0007(6) 0.0009(6) -0.0032(5) C10 0.0270(8) 0.0325(9) 0.0188(8) 0.0038(7) -0.0060(6) 0.0042(7) C11 0.0139(7) 0.0132(7) 0.0193(7) 0.0006(6) 0.0035(5) 0.0014(6) C12 0.0169(7) 0.0158(8) 0.0167(7) -0.0009(6) 0.0019(6) 0.0020(6) C13 0.0154(7) 0.0169(7) 0.0238(8) -0.0010(6) 0.0002(6) -0.0003(6) C14 0.0169(7) 0.0159(8) 0.0271(8) 0.0028(6) 0.0055(6) 0.0009(6) C15 0.0212(7) 0.0182(7) 0.0177(7) 0.0032(6) 0.0032(6) 0.0044(6) C16 0.0153(7) 0.0167(7) 0.0204(7) -0.0001(6) -0.0001(6) 0.0016(6) C17 0.0186(8) 0.0319(9) 0.0197(7) -0.0045(7) -0.0026(6) -0.0007(7) O1 0.0208(6) 0.0158(5) 0.0200(5) 0.0034(4) 0.0001(4) -0.0030(5) O2 0.0142(5) 0.0149(5) 0.0186(5) 0.0020(4) 0.0035(4) 0.0001(4) O3 0.0209(5) 0.0262(6) 0.0162(5) 0.0000(5) 0.0029(4) 0.0010(5) O4 0.0166(5) 0.0236(6) 0.0173(5) 0.0018(4) -0.0015(4) 0.0028(4) O5 0.0194(5) 0.0273(6) 0.0158(5) 0.0007(4) -0.0023(4) -0.0043(4) C18 0.0148(7) 0.0140(7) 0.0185(7) -0.0014(6) 0.0017(5) 0.0043(5) C19 0.0168(7) 0.0174(8) 0.0211(8) -0.0005(6) 0.0005(6) -0.0004(6) C20 0.0204(7) 0.0183(8) 0.0220(8) 0.0014(6) 0.0057(6) 0.0004(6) C21 0.0232(8) 0.0219(8) 0.0175(7) -0.0005(6) 0.0012(6) 0.0053(6) C22 0.0158(7) 0.0212(8) 0.0228(8) -0.0018(6) -0.0034(6) 0.0015(6) C23 0.0135(7) 0.0182(8) 0.0229(8) 0.0012(6) 0.0026(6) 0.0011(6) C24 0.0144(7) 0.0155(8) 0.0180(7) -0.0018(6) 0.0016(5) -0.0007(6) C25 0.0127(7) 0.0157(7) 0.0158(7) -0.0009(6) 0.0019(5) -0.0020(6) C26 0.0149(7) 0.0150(7) 0.0192(7) 0.0001(6) 0.0014(6) 0.0020(6) C27 0.0255(9) 0.0311(9) 0.0182(8) 0.0006(7) -0.0069(6) -0.0052(7) C28 0.0133(7) 0.0144(7) 0.0197(7) -0.0002(6) 0.0037(5) -0.0022(6) C29 0.0174(7) 0.0167(7) 0.0171(7) 0.0015(6) 0.0016(6) -0.0038(6) C30 0.0154(7) 0.0165(8) 0.0233(8) 0.0034(6) 0.0004(6) 0.0001(6) C31 0.0168(7) 0.0166(8) 0.0221(8) -0.0012(6) 0.0058(6) -0.0001(6) C32 0.0200(7) 0.0193(8) 0.0176(7) -0.0006(6) 0.0028(6) -0.0019(6) C33 0.0150(7) 0.0161(7) 0.0192(7) -0.0010(6) -0.0009(6) -0.0008(6) C34 0.0193(7) 0.0331(9) 0.0201(8) 0.0034(7) -0.0033(6) 0.0007(7) O6 0.0194(5) 0.0175(6) 0.0206(5) -0.0052(5) 0.0000(4) 0.0019(4) O7 0.0134(5) 0.0147(5) 0.0199(5) -0.0031(4) 0.0025(4) -0.0013(4) O8 0.0204(5) 0.0284(6) 0.0162(5) 0.0009(5) 0.0026(4) -0.0028(5) O9 0.0169(5) 0.0220(6) 0.0154(5) 0.0004(4) -0.0020(4) -0.0032(4) O10 0.0203(6) 0.0286(6) 0.0179(5) 0.0002(5) -0.0015(4) 0.0041(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.391(2) . ? C1 C6 1.391(2) . ? C1 C7 1.513(2) . ? C2 C3 1.387(2) . ? C2 H2 0.9500 . ? C3 C4 1.385(2) . ? C3 H3 0.9500 . ? C4 C5 1.391(2) . ? C4 H4 0.9500 . ? C5 C6 1.389(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O1 1.4303(19) . ? C7 C8 1.529(2) . ? C7 H7 1.0000 . ? C8 O2 1.4288(18) . ? C8 C9 1.525(2) . ? C8 H8 1.0000 . ? C9 O3 1.2011(19) . ? C9 O4 1.3377(19) . ? C10 O4 1.4455(18) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.380(2) . ? C11 O2 1.3906(18) . ? C11 C12 1.400(2) . ? C12 O5 1.3634(19) . ? C12 C13 1.391(2) . ? C13 C14 1.393(2) . ? C13 H13 0.9500 . ? C14 C15 1.382(2) . ? C14 H14 0.9500 . ? C15 C16 1.393(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 O5 1.4345(19) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O1 H1O 0.80(3) . ? C18 C23 1.389(2) . ? C18 C19 1.398(2) . ? C18 C24 1.511(2) . ? C19 C20 1.386(2) . ? C19 H19 0.9500 . ? C20 C21 1.387(2) . ? C20 H20 0.9500 . ? C21 C22 1.391(2) . ? C21 H21 0.9500 . ? C22 C23 1.388(2) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 O6 1.4341(18) . ? C24 C25 1.5337(19) . ? C24 H24 1.0000 . ? C25 O7 1.4299(18) . ? C25 C26 1.521(2) . ? C25 H25 1.0000 . ? C26 O8 1.204(2) . ? C26 O9 1.3380(18) . ? C27 O9 1.4486(18) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.380(2) . ? C28 O7 1.3926(18) . ? C28 C29 1.402(2) . ? C29 O10 1.3603(19) . ? C29 C30 1.389(2) . ? C30 C31 1.391(2) . ? C30 H30 0.9500 . ? C31 C32 1.385(2) . ? C31 H31 0.9500 . ? C32 C33 1.395(2) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 O10 1.4322(18) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O6 H6O 0.88(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.30(14) . . ? C2 C1 C7 119.58(13) . . ? C6 C1 C7 121.06(13) . . ? C3 C2 C1 120.31(14) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 120.40(14) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.56(14) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.15(14) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 120.28(14) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? O1 C7 C1 112.61(12) . . ? O1 C7 C8 105.55(11) . . ? C1 C7 C8 109.44(12) . . ? O1 C7 H7 109.7 . . ? C1 C7 H7 109.7 . . ? C8 C7 H7 109.7 . . ? O2 C8 C9 110.87(12) . . ? O2 C8 C7 106.83(11) . . ? C9 C8 C7 109.90(12) . . ? O2 C8 H8 109.7 . . ? C9 C8 H8 109.7 . . ? C7 C8 H8 109.7 . . ? O3 C9 O4 125.11(14) . . ? O3 C9 C8 125.02(14) . . ? O4 C9 C8 109.82(12) . . ? O4 C10 H10A 109.5 . . ? O4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 O2 119.87(13) . . ? C16 C11 C12 120.86(13) . . ? O2 C11 C12 119.27(13) . . ? O5 C12 C13 125.51(14) . . ? O5 C12 C11 115.32(13) . . ? C13 C12 C11 119.17(14) . . ? C12 C13 C14 119.74(14) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 120.72(14) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.81(15) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 119.70(14) . . ? C11 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? O5 C17 H17A 109.5 . . ? O5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C7 O1 H1O 106.9(18) . . ? C11 O2 C8 114.26(11) . . ? C9 O4 C10 115.60(12) . . ? C12 O5 C17 117.12(12) . . ? C23 C18 C19 118.85(14) . . ? C23 C18 C24 121.01(14) . . ? C19 C18 C24 120.02(13) . . ? C20 C19 C18 120.24(14) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.59(15) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C22 119.43(15) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 120.03(14) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C18 120.86(15) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? O6 C24 C18 112.94(12) . . ? O6 C24 C25 105.78(11) . . ? C18 C24 C25 109.99(12) . . ? O6 C24 H24 109.3 . . ? C18 C24 H24 109.3 . . ? C25 C24 H24 109.3 . . ? O7 C25 C26 110.87(12) . . ? O7 C25 C24 107.06(11) . . ? C26 C25 C24 110.03(12) . . ? O7 C25 H25 109.6 . . ? C26 C25 H25 109.6 . . ? C24 C25 H25 109.6 . . ? O8 C26 O9 125.42(14) . . ? O8 C26 C25 124.85(14) . . ? O9 C26 C25 109.70(12) . . ? O9 C27 H27A 109.5 . . ? O9 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O9 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 O7 119.10(13) . . ? C33 C28 C29 121.12(14) . . ? O7 C28 C29 119.79(13) . . ? O10 C29 C30 125.89(14) . . ? O10 C29 C28 115.28(13) . . ? C30 C29 C28 118.83(14) . . ? C29 C30 C31 119.83(14) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 121.15(14) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C33 119.21(14) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C28 C33 C32 119.86(14) . . ? C28 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? O10 C34 H34A 109.5 . . ? O10 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O10 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C24 O6 H6O 103.9(15) . . ? C28 O7 C25 113.89(11) . . ? C26 O9 C27 116.04(12) . . ? C29 O10 C34 117.31(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.2(2) . . . . ? C7 C1 C2 C3 177.31(14) . . . . ? C1 C2 C3 C4 -0.8(2) . . . . ? C2 C3 C4 C5 1.0(2) . . . . ? C3 C4 C5 C6 -0.6(2) . . . . ? C4 C5 C6 C1 0.0(2) . . . . ? C2 C1 C6 C5 0.2(2) . . . . ? C7 C1 C6 C5 -176.90(14) . . . . ? C2 C1 C7 O1 43.48(18) . . . . ? C6 C1 C7 O1 -139.48(14) . . . . ? C2 C1 C7 C8 -73.59(17) . . . . ? C6 C1 C7 C8 103.46(15) . . . . ? O1 C7 C8 O2 171.93(11) . . . . ? C1 C7 C8 O2 -66.64(15) . . . . ? O1 C7 C8 C9 51.57(15) . . . . ? C1 C7 C8 C9 173.01(12) . . . . ? O2 C8 C9 O3 -50.68(19) . . . . ? C7 C8 C9 O3 67.20(18) . . . . ? O2 C8 C9 O4 131.90(12) . . . . ? C7 C8 C9 O4 -110.22(13) . . . . ? C16 C11 C12 O5 178.96(14) . . . . ? O2 C11 C12 O5 -1.27(19) . . . . ? C16 C11 C12 C13 -0.6(2) . . . . ? O2 C11 C12 C13 179.19(13) . . . . ? O5 C12 C13 C14 -178.72(15) . . . . ? C11 C12 C13 C14 0.8(2) . . . . ? C12 C13 C14 C15 -0.5(2) . . . . ? C13 C14 C15 C16 0.0(2) . . . . ? O2 C11 C16 C15 -179.69(13) . . . . ? C12 C11 C16 C15 0.1(2) . . . . ? C14 C15 C16 C11 0.2(2) . . . . ? C16 C11 O2 C8 -100.68(16) . . . . ? C12 C11 O2 C8 79.55(16) . . . . ? C9 C8 O2 C11 -109.58(14) . . . . ? C7 C8 O2 C11 130.69(12) . . . . ? O3 C9 O4 C10 1.0(2) . . . . ? C8 C9 O4 C10 178.43(12) . . . . ? C13 C12 O5 C17 5.8(2) . . . . ? C11 C12 O5 C17 -173.72(14) . . . . ? C23 C18 C19 C20 -0.3(2) . . . . ? C24 C18 C19 C20 -176.47(13) . . . . ? C18 C19 C20 C21 0.2(2) . . . . ? C19 C20 C21 C22 -0.3(2) . . . . ? C20 C21 C22 C23 0.5(2) . . . . ? C21 C22 C23 C18 -0.6(2) . . . . ? C19 C18 C23 C22 0.5(2) . . . . ? C24 C18 C23 C22 176.62(14) . . . . ? C23 C18 C24 O6 139.81(14) . . . . ? C19 C18 C24 O6 -44.08(18) . . . . ? C23 C18 C24 C25 -102.28(15) . . . . ? C19 C18 C24 C25 73.84(17) . . . . ? O6 C24 C25 O7 -170.33(11) . . . . ? C18 C24 C25 O7 67.41(15) . . . . ? O6 C24 C25 C26 -49.77(15) . . . . ? C18 C24 C25 C26 -172.03(12) . . . . ? O7 C25 C26 O8 48.73(19) . . . . ? C24 C25 C26 O8 -69.51(18) . . . . ? O7 C25 C26 O9 -133.52(12) . . . . ? C24 C25 C26 O9 108.24(13) . . . . ? C33 C28 C29 O10 -179.79(13) . . . . ? O7 C28 C29 O10 0.6(2) . . . . ? C33 C28 C29 C30 -0.3(2) . . . . ? O7 C28 C29 C30 -179.94(13) . . . . ? O10 C29 C30 C31 179.08(14) . . . . ? C28 C29 C30 C31 -0.3(2) . . . . ? C29 C30 C31 C32 0.9(2) . . . . ? C30 C31 C32 C33 -0.9(2) . . . . ? O7 C28 C33 C32 179.99(13) . . . . ? C29 C28 C33 C32 0.4(2) . . . . ? C31 C32 C33 C28 0.2(2) . . . . ? C33 C28 O7 C25 100.92(15) . . . . ? C29 C28 O7 C25 -79.47(17) . . . . ? C26 C25 O7 C28 109.56(13) . . . . ? C24 C25 O7 C28 -130.41(13) . . . . ? O8 C26 O9 C27 0.5(2) . . . . ? C25 C26 O9 C27 -177.26(12) . . . . ? C30 C29 O10 C34 -3.4(2) . . . . ? C28 C29 O10 C34 176.03(14) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 67.96 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.156 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.043 data_bj481 _database_code_depnum_ccdc_archive 'CCDC 883566' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H38 O4 P2 Ru' _chemical_formula_weight 853.80 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' P P 0.1023 0.0942 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.647(4) _cell_length_b 38.343(8) _cell_length_c 11.412(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.182(4) _cell_angle_gamma 90.00 _cell_volume 7720(3) _cell_formula_units_Z 8 _cell_measurement_temperature 90.0(1) _cell_measurement_reflns_used 9687 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.37 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 0.536 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.690 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details 'TWINABS, Sheldrick (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(1) _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 'Bruker APEX DUO' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15985 _diffrn_reflns_av_R_equivalents 0.108 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 25.45 _reflns_number_total 15985 _reflns_number_gt 12980 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0001P)^2^+101.5698P] 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 15985 _refine_ls_number_parameters 891 _refine_ls_number_restraints 1320 _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_gt 0.1021 _refine_ls_wR_factor_ref 0.2425 _refine_ls_wR_factor_gt 0.2310 _refine_ls_goodness_of_fit_ref 1.264 _refine_ls_restrained_S_all 1.217 _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 C1 C 0.4607(3) 0.0761(2) 0.9616(6) 0.028(2) Uani 1 1 d GU . . C2 C 0.4711(4) 0.0850(2) 0.8449(5) 0.033(3) Uani 1 1 d GU . . H2 H 0.4296 0.0840 0.7906 0.040 Uiso 1 1 calc . . . C3 C 0.5422(4) 0.0953(2) 0.8077(5) 0.038(3) Uani 1 1 d GU . . H3 H 0.5493 0.1013 0.7280 0.046 Uiso 1 1 calc . . . C4 C 0.6029(3) 0.0967(2) 0.8872(7) 0.036(3) Uani 1 1 d GU . . H4 H 0.6515 0.1037 0.8618 0.044 Uiso 1 1 calc . . . C5 C 0.5924(4) 0.0878(2) 1.0039(6) 0.045(3) Uani 1 1 d GU . . H5 H 0.6339 0.0888 1.0582 0.054 Uiso 1 1 calc . . . C6 C 0.5213(4) 0.0775(2) 1.0411(5) 0.039(3) Uani 1 1 d GU . . H6 H 0.5142 0.0715 1.1208 0.046 Uiso 1 1 calc . . . C7 C 0.3342(4) 0.03144(15) 0.9035(6) 0.026(2) Uani 1 1 d GU . . C8 C 0.3849(3) 0.00682(19) 0.8621(6) 0.036(3) Uani 1 1 d GU . . H8 H 0.4367 0.0076 0.8866 0.043 Uiso 1 1 calc . . . C9 C 0.3599(4) -0.01891(16) 0.7847(6) 0.033(3) Uani 1 1 d GU . . H9 H 0.3945 -0.0357 0.7564 0.040 Uiso 1 1 calc . . . C10 C 0.2842(4) -0.02004(17) 0.7488(6) 0.041(3) Uani 1 1 d GU . . H10 H 0.2671 -0.0376 0.6959 0.050 Uiso 1 1 calc . . . C11 C 0.2335(3) 0.0046(2) 0.7903(7) 0.047(3) Uani 1 1 d GU . . H11 H 0.1817 0.0038 0.7658 0.056 Uiso 1 1 calc . . . C12 C 0.2585(4) 0.03031(17) 0.8676(7) 0.040(3) Uani 1 1 d GU . . H12 H 0.2239 0.0471 0.8960 0.048 Uiso 1 1 calc . . . C13 C 0.3691(6) 0.0618(3) 1.2547(9) 0.025(2) Uani 1 1 d U . . C14 C 0.3807(7) 0.0436(2) 1.1498(9) 0.028(2) Uani 1 1 d U . . C15 C 0.4074(7) 0.0094(3) 1.1546(10) 0.036(3) Uani 1 1 d U . . H15 H 0.4149 -0.0036 1.0849 0.044 Uiso 1 1 calc . . . C16 C 0.4226(9) -0.0052(4) 1.2636(12) 0.051(3) Uani 1 1 d U . . H16 H 0.4399 -0.0286 1.2681 0.061 Uiso 1 1 calc . . . C17 C 0.4133(8) 0.0133(3) 1.3652(11) 0.044(3) Uani 1 1 d U . . H17 H 0.4254 0.0027 1.4385 0.053 Uiso 1 1 calc . . . C18 C 0.3863(7) 0.0477(3) 1.3618(10) 0.035(3) Uani 1 1 d U . . C19 C 0.3783(8) 0.0683(3) 1.4737(10) 0.039(3) Uani 1 1 d U . . C20 C 0.3279(7) 0.0998(3) 1.4516(9) 0.035(3) Uani 1 1 d U . . C21 C 0.2980(8) 0.1187(3) 1.5464(11) 0.042(3) Uani 1 1 d U . . H21 H 0.3076 0.1107 1.6242 0.051 Uiso 1 1 calc . . . C22 C 0.2562(7) 0.1477(3) 1.5292(10) 0.039(3) Uani 1 1 d U . . H22 H 0.2397 0.1605 1.5951 0.047 Uiso 1 1 calc . . . C23 C 0.2366(7) 0.1592(3) 1.4165(10) 0.039(3) Uani 1 1 d U . . H23 H 0.2042 0.1787 1.4045 0.047 Uiso 1 1 calc . . . C24 C 0.2667(8) 0.1408(3) 1.3214(9) 0.036(3) Uani 1 1 d U . . C25 C 0.3102(7) 0.1112(3) 1.3423(10) 0.033(3) Uani 1 1 d U . . C26 C 0.4574(9) 0.0804(4) 1.5136(12) 0.054(4) Uani 1 1 d U . . H26A H 0.4536 0.0938 1.5864 0.080 Uiso 1 1 calc R . . H26B H 0.4792 0.0952 1.4528 0.080 Uiso 1 1 calc R . . H26C H 0.4900 0.0601 1.5271 0.080 Uiso 1 1 calc R . . C27 C 0.3454(8) 0.0451(3) 1.5702(11) 0.046(3) Uani 1 1 d U . . H27A H 0.3406 0.0588 1.6422 0.069 Uiso 1 1 calc R . . H27B H 0.3792 0.0253 1.5849 0.069 Uiso 1 1 calc R . . H27C H 0.2953 0.0366 1.5448 0.069 Uiso 1 1 calc R . . C28 C 0.1385(4) 0.1626(2) 1.1786(9) 0.046(3) Uani 1 1 d GU . . C29 C 0.0960(5) 0.13619(19) 1.2286(8) 0.055(4) Uani 1 1 d GU . . H29 H 0.1204 0.1160 1.2592 0.066 Uiso 1 1 calc . . . C30 C 0.0176(5) 0.1394(3) 1.2339(10) 0.066(4) Uani 1 1 d GU . . H30 H -0.0115 0.1213 1.2681 0.079 Uiso 1 1 calc . . . C31 C -0.0181(4) 0.1690(3) 1.1891(13) 0.098(6) Uani 1 1 d GU . . H31 H -0.0716 0.1711 1.1926 0.117 Uiso 1 1 calc . . . C32 C 0.0245(6) 0.1953(3) 1.1390(13) 0.102(7) Uani 1 1 d GU . . H32 H 0.0000 0.2156 1.1084 0.122 Uiso 1 1 calc . . . C33 C 0.1028(6) 0.1922(2) 1.1338(11) 0.081(5) Uani 1 1 d GU . . H33 H 0.1319 0.2102 1.0995 0.097 Uiso 1 1 calc . . . C34 C 0.2803(5) 0.19984(15) 1.1581(7) 0.036(3) Uani 1 1 d GU . . C35 C 0.3210(6) 0.2162(2) 1.2481(6) 0.064(4) Uani 1 1 d GU . . H35 H 0.3293 0.2045 1.3207 0.077 Uiso 1 1 calc . . . C36 C 0.3496(6) 0.2496(2) 1.2318(8) 0.064(4) Uani 1 1 d GU . . H36 H 0.3774 0.2607 1.2933 0.076 Uiso 1 1 calc . . . C37 C 0.3375(6) 0.26663(17) 1.1256(9) 0.058(4) Uani 1 1 d GU . . H37 H 0.3570 0.2895 1.1145 0.070 Uiso 1 1 calc . . . C38 C 0.2968(6) 0.25029(19) 1.0357(7) 0.060(4) Uani 1 1 d GU . . H38 H 0.2885 0.2620 0.9631 0.072 Uiso 1 1 calc . . . C39 C 0.2682(6) 0.21690(19) 1.0519(6) 0.049(3) Uani 1 1 d GU . . H39 H 0.2404 0.2057 0.9904 0.059 Uiso 1 1 calc . . . C40 C 0.3986(7) 0.1587(2) 0.9596(10) 0.029(2) Uani 1 1 d U . . C41 C 0.3455(8) 0.1540(3) 0.8698(10) 0.036(3) Uani 1 1 d U . . H41 H 0.3514 0.1648 0.7956 0.044 Uiso 1 1 calc . . . C42 C 0.2808(6) 0.1321(3) 0.8932(8) 0.026(2) Uani 1 1 d U . . C43 C 0.4644(5) 0.1826(2) 0.9451(8) 0.040(3) Uani 1 1 d GU . . C44 C 0.4870(6) 0.2043(2) 1.0368(6) 0.062(4) Uani 1 1 d GU . . H44 H 0.4627 0.2029 1.1101 0.074 Uiso 1 1 calc . . . C45 C 0.5453(7) 0.2282(2) 1.0213(8) 0.065(4) Uani 1 1 d GU . . H45 H 0.5607 0.2431 1.0840 0.078 Uiso 1 1 calc . . . C46 C 0.5809(6) 0.2303(2) 0.9141(9) 0.073(5) Uani 1 1 d GU . . H46 H 0.6207 0.2466 0.9035 0.088 Uiso 1 1 calc . . . C47 C 0.5583(6) 0.2086(3) 0.8223(7) 0.058(4) Uani 1 1 d GU . . H47 H 0.5827 0.2101 0.7490 0.069 Uiso 1 1 calc . . . C48 C 0.5001(5) 0.1847(2) 0.8378(6) 0.047(3) Uani 1 1 d GU . . H48 H 0.4846 0.1699 0.7751 0.057 Uiso 1 1 calc . . . C49 C 0.2006(6) 0.0890(3) 1.0470(10) 0.029(2) Uani 1 1 d U . . O1 O 0.3379(5) 0.09515(18) 1.2408(6) 0.0283(17) Uani 1 1 d U . . O2 O 0.3899(4) 0.14378(18) 1.0596(6) 0.0265(16) Uani 1 1 d U . . O3 O 0.2300(5) 0.1269(2) 0.8206(7) 0.041(2) Uani 1 1 d U . . O4 O 0.1424(6) 0.0778(2) 1.0338(8) 0.049(2) Uani 1 1 d U . . P1 P 0.36530(17) 0.06549(7) 1.0063(2) 0.0254(6) Uani 1 1 d U . . P2 P 0.24020(18) 0.15592(7) 1.1706(3) 0.0288(6) Uani 1 1 d U . . P3 P 0.72159(19) 0.15637(7) 0.3716(2) 0.0302(7) Uani 1 1 d U . . P4 P 0.87323(18) 0.06679(7) 0.4942(2) 0.0266(6) Uani 1 1 d U . . Ru1 Ru 0.29267(6) 0.11296(2) 1.05759(7) 0.0260(2) Uani 1 1 d U . . C50 C 0.6192(3) 0.1594(2) 0.3866(7) 0.035(3) Uani 1 1 d GU . . C51 C 0.5666(5) 0.1541(2) 0.2960(5) 0.045(3) Uani 1 1 d GU . . H51 H 0.5833 0.1478 0.2203 0.054 Uiso 1 1 calc . . . C52 C 0.4897(4) 0.1580(3) 0.3163(7) 0.052(4) Uani 1 1 d GU . . H52 H 0.4538 0.1543 0.2544 0.063 Uiso 1 1 calc . . . C53 C 0.4654(4) 0.1672(3) 0.4271(9) 0.054(4) Uani 1 1 d GU . . H53 H 0.4128 0.1699 0.4409 0.064 Uiso 1 1 calc . . . C54 C 0.5180(5) 0.1726(3) 0.5177(7) 0.072(5) Uani 1 1 d GU . . H54 H 0.5013 0.1789 0.5934 0.086 Uiso 1 1 calc . . . C55 C 0.5949(5) 0.1687(3) 0.4974(6) 0.072(5) Uani 1 1 d GU . . H55 H 0.6308 0.1723 0.5593 0.087 Uiso 1 1 calc . . . C56 C 0.7608(6) 0.20033(19) 0.3897(9) 0.043(3) Uani 1 1 d GU . . C57 C 0.8051(8) 0.2157(2) 0.3047(8) 0.086(6) Uani 1 1 d GU . . H57 H 0.8118 0.2044 0.2317 0.103 Uiso 1 1 calc . . . C58 C 0.8396(8) 0.2477(2) 0.3266(11) 0.092(6) Uani 1 1 d GU . . H58 H 0.8699 0.2582 0.2685 0.110 Uiso 1 1 calc . . . C59 C 0.8299(7) 0.2643(2) 0.4335(12) 0.076(5) Uani 1 1 d GU . . H59 H 0.8535 0.2862 0.4484 0.092 Uiso 1 1 calc . . . C60 C 0.7856(8) 0.2489(3) 0.5185(9) 0.097(6) Uani 1 1 d GU . . H60 H 0.7789 0.2603 0.5915 0.116 Uiso 1 1 calc . . . C61 C 0.7510(7) 0.2169(3) 0.4966(8) 0.074(5) Uani 1 1 d GU . . H61 H 0.7207 0.2064 0.5547 0.089 Uiso 1 1 calc . . . C62 C 0.7846(7) 0.1205(2) 0.1816(9) 0.031(3) Uani 1 1 d U . . C63 C 0.7372(7) 0.1468(3) 0.2163(9) 0.029(3) Uani 1 1 d U . . C64 C 0.7048(9) 0.1683(3) 0.1310(11) 0.048(3) Uani 1 1 d U . . H64 H 0.6716 0.1866 0.1524 0.058 Uiso 1 1 calc . . . C65 C 0.7218(9) 0.1627(3) 0.0133(10) 0.046(3) Uani 1 1 d U . . H65 H 0.7000 0.1775 -0.0451 0.055 Uiso 1 1 calc . . . C66 C 0.7682(7) 0.1368(3) -0.0186(9) 0.034(3) Uani 1 1 d U . . H66 H 0.7775 0.1328 -0.0992 0.041 Uiso 1 1 calc . . . C67 C 0.8029(7) 0.1158(3) 0.0665(9) 0.032(2) Uani 1 1 d U . . C68 C 0.8550(8) 0.0871(3) 0.0276(10) 0.044(3) Uani 1 1 d U . . C69 C 0.8957(8) 0.0709(3) 0.1341(11) 0.039(3) Uani 1 1 d U . . C70 C 0.9565(9) 0.0481(3) 0.1177(11) 0.046(3) Uani 1 1 d U . . H70 H 0.9724 0.0431 0.0405 0.055 Uiso 1 1 calc . . . C71 C 0.9937(8) 0.0329(3) 0.2116(12) 0.045(3) Uani 1 1 d U . . H71 H 1.0379 0.0193 0.1996 0.054 Uiso 1 1 calc . . . C72 C 0.9669(8) 0.0374(3) 0.3235(11) 0.039(3) Uani 1 1 d U . . H72 H 0.9906 0.0256 0.3876 0.046 Uiso 1 1 calc . . . C73 C 0.9059(6) 0.0589(3) 0.3429(10) 0.027(2) Uani 1 1 d U . . C74 C 0.8726(7) 0.0760(3) 0.2472(9) 0.028(2) Uani 1 1 d U . . C75 C 0.9167(11) 0.1035(6) -0.0522(15) 0.096(7) Uani 1 1 d U . . H75A H 0.9512 0.0852 -0.0784 0.145 Uiso 1 1 calc R . . H75B H 0.9454 0.1211 -0.0076 0.145 Uiso 1 1 calc R . . H75C H 0.8920 0.1145 -0.1205 0.145 Uiso 1 1 calc R . . C76 C 0.8098(12) 0.0586(4) -0.0390(14) 0.088(7) Uani 1 1 d U . . H76A H 0.8445 0.0401 -0.0638 0.132 Uiso 1 1 calc R . . H76B H 0.7845 0.0688 -0.1080 0.132 Uiso 1 1 calc R . . H76C H 0.7717 0.0486 0.0127 0.132 Uiso 1 1 calc R . . C77 C 0.8380(4) 0.02557(14) 0.5500(5) 0.027(2) Uani 1 1 d GU . . C78 C 0.8608(4) -0.00717(18) 0.5120(6) 0.034(3) Uani 1 1 d GU . . H78 H 0.8889 -0.0093 0.4423 0.041 Uiso 1 1 calc . . . C79 C 0.8424(5) -0.03671(13) 0.5760(7) 0.042(3) Uani 1 1 d GU . . H79 H 0.8579 -0.0591 0.5500 0.051 Uiso 1 1 calc . . . C80 C 0.8012(5) -0.03352(15) 0.6780(7) 0.045(3) Uani 1 1 d GU . . H80 H 0.7886 -0.0537 0.7217 0.054 Uiso 1 1 calc . . . C81 C 0.7785(5) -0.00079(19) 0.7160(5) 0.042(3) Uani 1 1 d GU . . H81 H 0.7503 0.0014 0.7857 0.051 Uiso 1 1 calc . . . C82 C 0.7969(4) 0.02876(14) 0.6520(6) 0.027(2) Uani 1 1 d GU . . H82 H 0.7813 0.0511 0.6780 0.033 Uiso 1 1 calc . . . C83 C 0.9626(4) 0.07279(18) 0.5754(6) 0.024(2) Uani 1 1 d GU . . C84 C 0.9778(4) 0.05369(17) 0.6767(6) 0.036(3) Uani 1 1 d GU . . H84 H 0.9435 0.0361 0.7008 0.043 Uiso 1 1 calc . . . C85 C 1.0433(5) 0.0603(2) 0.7428(6) 0.044(3) Uani 1 1 d GU . . H85 H 1.0538 0.0473 0.8120 0.053 Uiso 1 1 calc . . . C86 C 1.0935(4) 0.0860(2) 0.7075(8) 0.048(3) Uani 1 1 d GU . . H86 H 1.1383 0.0905 0.7527 0.058 Uiso 1 1 calc . . . C87 C 1.0782(4) 0.10510(19) 0.6063(8) 0.053(4) Uani 1 1 d GU . . H87 H 1.1125 0.1227 0.5822 0.064 Uiso 1 1 calc . . . C88 C 1.0128(5) 0.09849(19) 0.5402(6) 0.047(3) Uani 1 1 d GU . . H88 H 1.0023 0.1115 0.4710 0.056 Uiso 1 1 calc . . . C89 C 0.8958(7) 0.1592(3) 0.5727(11) 0.034(3) Uani 1 1 d U . . C90 C 0.8450(7) 0.1520(3) 0.6579(10) 0.033(3) Uani 1 1 d U . . H90 H 0.8504 0.1626 0.7329 0.040 Uiso 1 1 calc . . . C91 C 0.7814(6) 0.1277(3) 0.6334(8) 0.022(2) Uani 1 1 d U . . C92 C 0.9645(5) 0.1806(2) 0.5928(9) 0.046(3) Uani 1 1 d GU . . C93 C 0.9986(7) 0.1971(3) 0.4991(8) 0.070(5) Uani 1 1 d GU . . H93 H 0.9753 0.1963 0.4233 0.084 Uiso 1 1 calc . . . C94 C 1.0668(7) 0.2147(3) 0.5161(11) 0.089(6) Uani 1 1 d GU . . H94 H 1.0900 0.2260 0.4521 0.107 Uiso 1 1 calc . . . C95 C 1.1009(5) 0.2158(3) 0.6269(13) 0.090(6) Uani 1 1 d GU . . H95 H 1.1475 0.2279 0.6386 0.108 Uiso 1 1 calc . . . C96 C 1.0668(6) 0.1994(3) 0.7207(10) 0.087(6) Uani 1 1 d GU . . H96 H 1.0901 0.2001 0.7964 0.104 Uiso 1 1 calc . . . C97 C 0.9986(6) 0.1818(3) 0.7036(8) 0.067(5) Uani 1 1 d GU . . H97 H 0.9753 0.1705 0.7677 0.081 Uiso 1 1 calc . . . C98 C 0.7018(7) 0.0850(3) 0.4803(9) 0.029(2) Uani 1 1 d U . . O5 O 0.8153(5) 0.09984(19) 0.2719(6) 0.0333(19) Uani 1 1 d U . . O6 O 0.8828(4) 0.14549(19) 0.4672(6) 0.0268(16) Uani 1 1 d U . . O7 O 0.7364(5) 0.1205(2) 0.7054(7) 0.042(2) Uani 1 1 d U . . O8 O 0.6502(5) 0.0696(2) 0.4956(8) 0.044(2) Uani 1 1 d U . . Ru2 Ru 0.78918(6) 0.11260(2) 0.46520(7) 0.0261(2) Uani 1 1 d U . . 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 C1 0.034(6) 0.025(5) 0.027(6) -0.002(5) 0.003(5) -0.004(5) C2 0.025(6) 0.049(7) 0.027(6) -0.004(5) -0.002(5) -0.007(5) C3 0.059(8) 0.038(6) 0.018(5) 0.002(5) 0.003(5) -0.004(6) C4 0.049(7) 0.031(6) 0.030(6) 0.003(5) 0.010(5) -0.008(6) C5 0.035(7) 0.060(8) 0.040(7) -0.002(6) -0.002(6) -0.007(6) C6 0.043(7) 0.050(7) 0.022(6) -0.006(5) 0.000(5) 0.006(6) C7 0.036(6) 0.018(5) 0.023(5) -0.004(4) -0.001(5) -0.004(5) C8 0.043(7) 0.036(6) 0.029(6) 0.001(5) 0.004(5) 0.001(6) C9 0.044(7) 0.024(5) 0.031(6) -0.003(5) -0.003(5) 0.004(5) C10 0.055(8) 0.036(6) 0.034(6) -0.010(5) 0.002(6) -0.004(6) C11 0.054(8) 0.044(7) 0.042(7) -0.016(6) 0.000(6) -0.009(7) C12 0.042(7) 0.039(6) 0.039(7) -0.007(5) -0.003(6) 0.003(6) C13 0.029(6) 0.030(5) 0.017(5) 0.009(4) -0.002(4) 0.000(5) C14 0.040(6) 0.015(5) 0.029(6) 0.012(4) -0.007(5) -0.005(5) C15 0.048(7) 0.039(6) 0.023(6) -0.001(5) -0.002(5) 0.000(6) C16 0.063(9) 0.047(7) 0.043(8) 0.016(6) 0.000(7) 0.013(7) C17 0.046(7) 0.050(7) 0.036(7) 0.028(6) 0.003(6) 0.001(6) C18 0.033(6) 0.045(7) 0.028(6) 0.009(5) -0.011(5) -0.012(6) C19 0.056(8) 0.036(6) 0.027(6) 0.001(5) -0.007(6) -0.015(6) C20 0.053(7) 0.038(6) 0.012(5) -0.003(4) -0.002(5) -0.032(6) C21 0.049(8) 0.038(6) 0.039(6) 0.002(5) -0.011(6) -0.019(6) C22 0.036(7) 0.053(7) 0.029(6) -0.015(5) 0.002(5) -0.024(6) C23 0.036(7) 0.046(7) 0.034(6) -0.016(5) 0.001(5) -0.021(6) C24 0.063(8) 0.029(5) 0.015(5) -0.003(4) 0.003(5) -0.008(6) C25 0.045(7) 0.025(5) 0.030(6) -0.013(5) 0.001(5) -0.002(5) C26 0.067(10) 0.049(8) 0.043(8) 0.010(6) -0.029(7) -0.019(8) C27 0.060(9) 0.051(7) 0.027(6) 0.013(6) -0.004(6) -0.008(7) C28 0.080(10) 0.020(5) 0.037(7) -0.007(5) 0.006(7) -0.008(6) C29 0.052(8) 0.067(9) 0.047(8) -0.008(7) 0.008(7) -0.028(7) C30 0.040(8) 0.072(10) 0.087(12) 0.004(9) 0.015(8) -0.016(8) C31 0.042(9) 0.096(13) 0.156(17) 0.020(13) 0.028(11) -0.018(10) C32 0.052(10) 0.102(13) 0.153(17) 0.038(13) 0.030(11) 0.004(10) C33 0.062(10) 0.067(10) 0.114(14) 0.014(10) 0.025(10) -0.006(9) C34 0.051(7) 0.013(4) 0.044(7) -0.003(4) -0.005(6) -0.004(5) C35 0.074(11) 0.045(8) 0.073(10) 0.001(7) -0.010(9) -0.024(8) C36 0.082(11) 0.035(7) 0.074(10) -0.004(7) -0.015(9) -0.029(8) C37 0.076(10) 0.022(6) 0.077(10) -0.003(7) 0.012(8) -0.014(7) C38 0.080(10) 0.026(6) 0.073(9) 0.012(6) 0.017(9) -0.002(7) C39 0.053(8) 0.033(6) 0.060(8) 0.013(6) -0.009(7) 0.008(6) C40 0.040(6) 0.012(4) 0.034(6) 0.008(4) 0.012(5) -0.006(5) C41 0.058(8) 0.028(6) 0.024(6) 0.001(5) 0.011(5) -0.009(6) C42 0.029(6) 0.034(6) 0.014(5) 0.001(4) -0.001(4) -0.008(5) C43 0.042(7) 0.033(6) 0.046(7) 0.014(6) -0.004(6) -0.002(6) C44 0.095(12) 0.044(7) 0.047(8) 0.001(7) 0.002(8) -0.023(8) C45 0.085(11) 0.042(7) 0.069(10) -0.004(7) -0.005(9) -0.031(8) C46 0.098(13) 0.057(9) 0.065(10) 0.004(8) -0.006(10) -0.022(9) C47 0.067(10) 0.054(8) 0.053(8) 0.022(7) 0.002(8) -0.014(8) C48 0.041(7) 0.049(7) 0.052(8) 0.006(6) -0.001(6) -0.001(6) C49 0.011(5) 0.035(6) 0.041(6) -0.012(5) 0.001(5) 0.004(5) O1 0.052(5) 0.020(3) 0.013(3) -0.002(3) 0.001(3) -0.005(4) O2 0.024(4) 0.026(4) 0.029(4) -0.003(3) -0.007(3) -0.006(3) O3 0.037(5) 0.057(5) 0.028(4) 0.010(4) -0.010(4) -0.009(4) O4 0.047(6) 0.054(6) 0.046(5) -0.007(4) 0.000(5) -0.021(5) P1 0.0355(16) 0.0235(13) 0.0170(13) 0.0029(11) -0.0047(12) -0.0055(12) P2 0.0389(17) 0.0224(13) 0.0255(15) -0.0009(11) 0.0068(12) -0.0072(13) P3 0.0434(18) 0.0259(13) 0.0210(13) -0.0025(11) -0.0051(13) 0.0033(14) P4 0.0364(16) 0.0230(13) 0.0203(14) 0.0036(11) -0.0025(12) -0.0031(13) Ru1 0.0408(5) 0.0213(4) 0.0158(4) -0.0001(3) -0.0015(4) -0.0057(4) C50 0.037(7) 0.038(6) 0.030(6) 0.008(5) -0.013(5) -0.001(5) C51 0.055(8) 0.048(7) 0.030(7) 0.003(6) -0.004(6) -0.008(7) C52 0.038(7) 0.067(9) 0.051(8) 0.021(7) -0.015(6) -0.018(7) C53 0.029(7) 0.065(9) 0.067(9) -0.005(8) -0.001(7) -0.006(7) C54 0.060(10) 0.093(11) 0.063(10) -0.032(9) 0.017(8) -0.041(9) C55 0.060(10) 0.100(12) 0.056(9) -0.018(9) -0.003(8) -0.040(9) C56 0.037(7) 0.033(6) 0.057(8) -0.004(6) 0.005(6) 0.001(6) C57 0.132(15) 0.027(7) 0.099(12) -0.014(7) 0.037(12) -0.021(9) C58 0.118(14) 0.053(9) 0.105(13) -0.011(9) 0.042(12) -0.047(10) C59 0.077(11) 0.029(7) 0.123(15) -0.020(8) -0.008(11) -0.008(8) C60 0.112(15) 0.048(9) 0.130(15) -0.043(10) -0.007(14) 0.002(11) C61 0.068(10) 0.054(8) 0.101(12) -0.036(9) -0.009(9) 0.000(8) C62 0.051(7) 0.012(4) 0.030(5) 0.001(4) -0.009(5) -0.002(5) C63 0.046(7) 0.025(5) 0.017(5) -0.001(4) 0.001(5) -0.011(5) C64 0.067(9) 0.034(6) 0.043(7) 0.011(5) -0.018(7) -0.005(7) C65 0.069(9) 0.038(6) 0.031(6) 0.007(5) -0.008(7) -0.016(7) C66 0.035(6) 0.043(6) 0.024(6) 0.003(5) -0.001(5) -0.019(6) C67 0.044(7) 0.032(5) 0.020(5) 0.008(5) 0.001(5) -0.014(6) C68 0.059(8) 0.051(7) 0.023(6) 0.006(5) -0.002(6) 0.005(7) C69 0.051(7) 0.033(6) 0.035(6) 0.001(5) 0.005(6) 0.010(6) C70 0.064(9) 0.048(7) 0.026(6) -0.001(6) 0.005(6) 0.007(7) C71 0.045(8) 0.049(7) 0.041(7) -0.005(6) 0.004(6) 0.006(6) C72 0.046(7) 0.041(6) 0.029(6) 0.002(5) 0.001(5) -0.009(6) C73 0.027(6) 0.020(5) 0.032(6) 0.000(4) 0.004(5) 0.006(4) C74 0.037(6) 0.032(6) 0.016(5) 0.004(4) 0.002(5) 0.010(5) C75 0.081(13) 0.155(18) 0.055(11) 0.048(12) 0.038(10) 0.024(13) C76 0.146(18) 0.065(9) 0.050(9) -0.042(8) -0.046(11) 0.040(11) C77 0.020(5) 0.031(5) 0.030(6) -0.001(5) -0.014(5) -0.003(4) C78 0.021(6) 0.037(6) 0.044(7) -0.009(5) -0.002(5) -0.010(5) C79 0.040(7) 0.030(6) 0.057(8) 0.003(6) -0.005(6) 0.001(6) C80 0.037(7) 0.040(6) 0.058(8) 0.019(6) -0.008(6) -0.006(6) C81 0.050(8) 0.044(7) 0.032(6) 0.007(5) -0.003(6) -0.011(6) C82 0.026(6) 0.030(5) 0.027(5) 0.006(4) 0.003(5) -0.004(5) C83 0.028(6) 0.020(5) 0.025(5) -0.008(4) 0.002(4) -0.003(4) C84 0.043(7) 0.029(6) 0.035(6) -0.003(5) 0.004(5) 0.003(5) C85 0.043(7) 0.054(7) 0.035(7) -0.010(6) -0.009(6) 0.008(7) C86 0.041(7) 0.037(7) 0.066(9) -0.017(6) -0.020(7) 0.012(6) C87 0.042(8) 0.039(7) 0.079(10) 0.005(7) -0.002(7) 0.002(6) C88 0.033(7) 0.040(7) 0.067(9) 0.001(6) -0.007(6) -0.006(6) C89 0.028(6) 0.024(5) 0.051(7) 0.000(5) -0.011(5) 0.002(5) C90 0.049(7) 0.029(6) 0.022(6) 0.000(5) -0.013(5) 0.002(6) C91 0.012(5) 0.040(6) 0.013(5) -0.009(4) -0.010(4) 0.003(5) C92 0.046(8) 0.026(6) 0.067(9) -0.006(6) -0.001(7) 0.000(6) C93 0.084(11) 0.038(7) 0.089(12) -0.002(8) 0.013(10) -0.016(8) C94 0.097(14) 0.045(8) 0.126(15) -0.003(10) 0.026(12) -0.031(9) C95 0.066(11) 0.054(9) 0.151(17) -0.014(11) 0.000(12) -0.038(9) C96 0.070(11) 0.084(12) 0.106(14) -0.025(11) -0.008(11) -0.023(10) C97 0.050(9) 0.057(9) 0.093(12) 0.001(8) -0.027(9) -0.021(8) C98 0.028(6) 0.032(6) 0.026(6) 0.006(4) 0.009(5) 0.004(5) O5 0.055(5) 0.029(4) 0.016(4) 0.000(3) -0.006(3) 0.015(4) O6 0.017(4) 0.031(4) 0.032(4) -0.002(3) -0.004(3) -0.004(3) O7 0.050(5) 0.055(5) 0.021(4) -0.005(4) 0.010(4) -0.003(4) O8 0.036(5) 0.043(5) 0.052(6) -0.002(4) 0.008(4) -0.003(4) Ru2 0.0387(5) 0.0255(4) 0.0140(4) 0.0004(3) -0.0017(4) -0.0005(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 P1 1.815(6) . ? C2 C3 1.3900 . ? C2 H2 0.9500 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C7 P1 1.832(5) . ? C8 C9 1.3900 . ? C8 H8 0.9500 . ? C9 C10 1.3900 . ? C9 H9 0.9500 . ? C10 C11 1.3900 . ? C10 H10 0.9500 . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.366(15) . ? C13 O1 1.400(12) . ? C13 C14 1.404(15) . ? C14 C15 1.394(15) . ? C14 P1 1.855(10) . ? C15 C16 1.385(17) . ? C15 H15 0.9500 . ? C16 C17 1.372(19) . ? C16 H16 0.9500 . ? C17 C18 1.401(18) . ? C17 H17 0.9500 . ? C18 C19 1.510(17) . ? C19 C20 1.518(18) . ? C19 C26 1.531(18) . ? C19 C27 1.537(16) . ? C20 C25 1.353(16) . ? C20 C21 1.413(17) . ? C21 C22 1.347(18) . ? C21 H21 0.9500 . ? C22 C23 1.397(18) . ? C22 H22 0.9500 . ? C23 C24 1.407(16) . ? C23 H23 0.9500 . ? C24 C25 1.388(16) . ? C24 P2 1.866(11) . ? C25 O1 1.409(13) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.3900 . ? C28 C33 1.3900 . ? C28 P2 1.816(8) . ? C29 C30 1.3900 . ? C29 H29 0.9500 . ? C30 C31 1.3900 . ? C30 H30 0.9500 . ? C31 C32 1.3900 . ? C31 H31 0.9500 . ? C32 C33 1.3900 . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C34 P2 1.834(6) . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 C37 1.3900 . ? C36 H36 0.9500 . ? C37 C38 1.3900 . ? C37 H37 0.9500 . ? C38 C39 1.3900 . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 O2 1.288(13) . ? C40 C41 1.386(17) . ? C40 C43 1.491(12) . ? C41 C42 1.447(16) . ? C41 H41 0.9500 . ? C42 O3 1.224(13) . ? C42 Ru1 2.021(10) . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 C46 1.3900 . ? C45 H45 0.9500 . ? C46 C47 1.3900 . ? C46 H46 0.9500 . ? C47 C48 1.3900 . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O4 1.123(13) . ? C49 Ru1 1.867(11) . ? O1 Ru1 2.325(7) . ? O2 Ru1 2.084(7) . ? P1 Ru1 2.308(3) . ? P2 Ru1 2.299(3) . ? P3 C50 1.821(7) . ? P3 C56 1.832(7) . ? P3 C63 1.836(11) . ? P3 Ru2 2.308(3) . ? P4 C77 1.818(6) . ? P4 C83 1.826(6) . ? P4 C73 1.857(11) . ? P4 Ru2 2.318(3) . ? C50 C51 1.3900 . ? C50 C55 1.3900 . ? C51 C52 1.3900 . ? C51 H51 0.9500 . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 C55 1.3900 . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C57 1.3900 . ? C56 C61 1.3900 . ? C57 C58 1.3900 . ? C57 H57 0.9500 . ? C58 C59 1.3900 . ? C58 H58 0.9500 . ? C59 C60 1.3900 . ? C59 H59 0.9500 . ? C60 C61 1.3900 . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C67 1.371(15) . ? C62 C63 1.373(16) . ? C62 O5 1.401(12) . ? C63 C64 1.391(16) . ? C64 C65 1.399(19) . ? C64 H64 0.9500 . ? C65 C66 1.342(19) . ? C65 H65 0.9500 . ? C66 C67 1.393(16) . ? C66 H66 0.9500 . ? C67 C68 1.508(18) . ? C68 C69 1.531(17) . ? C68 C76 1.54(2) . ? C68 C75 1.57(2) . ? C69 C74 1.376(16) . ? C69 C70 1.399(18) . ? C70 C71 1.375(18) . ? C70 H70 0.9500 . ? C71 C72 1.382(18) . ? C71 H71 0.9500 . ? C72 C73 1.376(16) . ? C72 H72 0.9500 . ? C73 C74 1.394(15) . ? C74 O5 1.395(13) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.3900 . ? C77 C82 1.3900 . ? C78 C79 1.3900 . ? C78 H78 0.9500 . ? C79 C80 1.3900 . ? C79 H79 0.9500 . ? C80 C81 1.3900 . ? C80 H80 0.9500 . ? C81 C82 1.3900 . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.3900 . ? C83 C88 1.3900 . ? C84 C85 1.3900 . ? C84 H84 0.9500 . ? C85 C86 1.3900 . ? C85 H85 0.9500 . ? C86 C87 1.3900 . ? C86 H86 0.9500 . ? C87 C88 1.3900 . ? C87 H87 0.9500 . ? C88 H88 0.9500 . ? C89 O6 1.330(14) . ? C89 C90 1.364(18) . ? C89 C92 1.478(13) . ? C90 C91 1.482(15) . ? C90 H90 0.9500 . ? C91 O7 1.186(13) . ? C91 Ru2 2.012(9) . ? C92 C93 1.3900 . ? C92 C97 1.3900 . ? C93 C94 1.3900 . ? C93 H93 0.9500 . ? C94 C95 1.3900 . ? C94 H94 0.9500 . ? C95 C96 1.3900 . ? C95 H95 0.9500 . ? C96 C97 1.3900 . ? C96 H96 0.9500 . ? C97 H97 0.9500 . ? C98 O8 1.103(13) . ? C98 Ru2 1.881(12) . ? O5 Ru2 2.315(7) . ? O6 Ru2 2.079(7) . ? 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 C1 C6 120.0 . . ? C2 C1 P1 117.8(4) . . ? C6 C1 P1 122.1(4) . . ? C1 C2 C3 120.0 . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 P1 121.0(4) . . ? C12 C7 P1 119.0(4) . . ? C7 C8 C9 120.0 . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C18 C13 O1 122.9(10) . . ? C18 C13 C14 122.1(10) . . ? O1 C13 C14 114.9(8) . . ? C15 C14 C13 119.3(9) . . ? C15 C14 P1 120.2(9) . . ? C13 C14 P1 120.4(7) . . ? C16 C15 C14 118.3(11) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C17 C16 C15 121.7(12) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 120.6(11) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C13 C18 C17 117.8(12) . . ? C13 C18 C19 121.7(11) . . ? C17 C18 C19 120.4(11) . . ? C18 C19 C20 109.9(10) . . ? C18 C19 C26 108.1(12) . . ? C20 C19 C26 109.5(10) . . ? C18 C19 C27 110.2(10) . . ? C20 C19 C27 110.4(11) . . ? C26 C19 C27 108.5(10) . . ? C25 C20 C21 117.2(12) . . ? C25 C20 C19 122.3(11) . . ? C21 C20 C19 120.5(10) . . ? C22 C21 C20 121.5(11) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C21 C22 C23 121.3(12) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C24 117.5(12) . . ? C22 C23 H23 121.3 . . ? C24 C23 H23 121.3 . . ? C25 C24 C23 119.5(10) . . ? C25 C24 P2 122.7(8) . . ? C23 C24 P2 117.7(9) . . ? C20 C25 C24 122.7(11) . . ? C20 C25 O1 122.6(11) . . ? C24 C25 O1 114.6(10) . . ? C19 C26 H26A 109.5 . . ? C19 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C19 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C19 C27 H27A 109.5 . . ? C19 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C19 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 120.0 . . ? C29 C28 P2 117.4(5) . . ? C33 C28 P2 122.5(5) . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C28 120.0 . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? C35 C34 C39 120.0 . . ? C35 C34 P2 123.4(5) . . ? C39 C34 P2 116.6(4) . . ? C36 C35 C34 120.0 . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C34 120.0 . . ? C38 C39 H39 120.0 . . ? C34 C39 H39 120.0 . . ? O2 C40 C41 120.4(10) . . ? O2 C40 C43 118.6(10) . . ? C41 C40 C43 120.9(9) . . ? C40 C41 C42 117.6(10) . . ? C40 C41 H41 121.2 . . ? C42 C41 H41 121.2 . . ? O3 C42 C41 122.6(10) . . ? O3 C42 Ru1 129.0(8) . . ? C41 C42 Ru1 108.4(7) . . ? C44 C43 C48 120.0 . . ? C44 C43 C40 119.8(7) . . ? C48 C43 C40 120.1(7) . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 120.0 . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C47 C46 C45 120.0 . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? O4 C49 Ru1 172.3(11) . . ? C13 O1 C25 116.6(8) . . ? C13 O1 Ru1 119.8(6) . . ? C25 O1 Ru1 119.5(7) . . ? C40 O2 Ru1 110.8(7) . . ? C1 P1 C7 104.3(4) . . ? C1 P1 C14 103.3(5) . . ? C7 P1 C14 106.2(4) . . ? C1 P1 Ru1 114.7(3) . . ? C7 P1 Ru1 124.3(3) . . ? C14 P1 Ru1 101.8(4) . . ? C28 P2 C34 105.0(4) . . ? C28 P2 C24 103.1(6) . . ? C34 P2 C24 105.5(4) . . ? C28 P2 Ru1 122.6(3) . . ? C34 P2 Ru1 117.0(3) . . ? C24 P2 Ru1 101.5(4) . . ? C50 P3 C56 107.6(5) . . ? C50 P3 C63 105.8(5) . . ? C56 P3 C63 103.3(5) . . ? C50 P3 Ru2 120.5(3) . . ? C56 P3 Ru2 115.3(4) . . ? C63 P3 Ru2 102.4(4) . . ? C77 P4 C83 103.3(3) . . ? C77 P4 C73 107.4(4) . . ? C83 P4 C73 102.2(4) . . ? C77 P4 Ru2 119.1(3) . . ? C83 P4 Ru2 121.3(3) . . ? C73 P4 Ru2 101.6(3) . . ? C49 Ru1 C42 92.6(5) . . ? C49 Ru1 O2 174.1(4) . . ? C42 Ru1 O2 82.7(4) . . ? C49 Ru1 P2 91.6(3) . . ? C42 Ru1 P2 103.0(3) . . ? O2 Ru1 P2 85.9(2) . . ? C49 Ru1 P1 94.8(3) . . ? C42 Ru1 P1 95.7(3) . . ? O2 Ru1 P1 89.3(2) . . ? P2 Ru1 P1 159.94(11) . . ? C49 Ru1 O1 101.3(4) . . ? C42 Ru1 O1 165.5(4) . . ? O2 Ru1 O1 83.6(3) . . ? P2 Ru1 O1 80.8(2) . . ? P1 Ru1 O1 79.29(19) . . ? C51 C50 C55 120.0 . . ? C51 C50 P3 124.7(5) . . ? C55 C50 P3 115.3(5) . . ? C50 C51 C52 120.0 . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C54 C55 C50 120.0 . . ? C54 C55 H55 120.0 . . ? C50 C55 H55 120.0 . . ? C57 C56 C61 120.0 . . ? C57 C56 P3 121.9(6) . . ? C61 C56 P3 117.9(6) . . ? C58 C57 C56 120.0 . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C59 120.0 . . ? C57 C58 H58 120.0 . . ? C59 C58 H58 120.0 . . ? C60 C59 C58 120.0 . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C61 120.0 . . ? C59 C60 H60 120.0 . . ? C61 C60 H60 120.0 . . ? C60 C61 C56 120.0 . . ? C60 C61 H61 120.0 . . ? C56 C61 H61 120.0 . . ? C67 C62 C63 122.0(10) . . ? C67 C62 O5 122.4(10) . . ? C63 C62 O5 115.6(9) . . ? C62 C63 C64 118.5(11) . . ? C62 C63 P3 122.0(8) . . ? C64 C63 P3 119.3(9) . . ? C63 C64 C65 119.2(13) . . ? C63 C64 H64 120.4 . . ? C65 C64 H64 120.4 . . ? C66 C65 C64 121.2(12) . . ? C66 C65 H65 119.4 . . ? C64 C65 H65 119.4 . . ? C65 C66 C67 120.0(11) . . ? C65 C66 H66 120.0 . . ? C67 C66 H66 120.0 . . ? C62 C67 C66 119.0(11) . . ? C62 C67 C68 122.3(10) . . ? C66 C67 C68 118.6(10) . . ? C67 C68 C69 110.0(10) . . ? C67 C68 C76 110.5(12) . . ? C69 C68 C76 109.4(11) . . ? C67 C68 C75 108.2(12) . . ? C69 C68 C75 107.7(12) . . ? C76 C68 C75 110.9(14) . . ? C74 C69 C70 117.2(11) . . ? C74 C69 C68 122.9(11) . . ? C70 C69 C68 119.8(11) . . ? C71 C70 C69 121.1(12) . . ? C71 C70 H70 119.5 . . ? C69 C70 H70 119.5 . . ? C70 C71 C72 120.0(13) . . ? C70 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C73 C72 C71 120.5(12) . . ? C73 C72 H72 119.8 . . ? C71 C72 H72 119.8 . . ? C72 C73 C74 118.4(10) . . ? C72 C73 P4 120.4(9) . . ? C74 C73 P4 121.2(8) . . ? C69 C74 C73 122.6(11) . . ? C69 C74 O5 120.9(10) . . ? C73 C74 O5 116.5(9) . . ? C68 C75 H75A 109.5 . . ? C68 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C68 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C68 C76 H76A 109.5 . . ? C68 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C68 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 C82 120.0 . . ? C78 C77 P4 124.9(4) . . ? C82 C77 P4 113.9(4) . . ? C79 C78 C77 120.0 . . ? C79 C78 H78 120.0 . . ? C77 C78 H78 120.0 . . ? C78 C79 C80 120.0 . . ? C78 C79 H79 120.0 . . ? C80 C79 H79 120.0 . . ? C81 C80 C79 120.0 . . ? C81 C80 H80 120.0 . . ? C79 C80 H80 120.0 . . ? C80 C81 C82 120.0 . . ? C80 C81 H81 120.0 . . ? C82 C81 H81 120.0 . . ? C81 C82 C77 120.0 . . ? C81 C82 H82 120.0 . . ? C77 C82 H82 120.0 . . ? C84 C83 C88 120.0 . . ? C84 C83 P4 120.4(4) . . ? C88 C83 P4 119.4(4) . . ? C83 C84 C85 120.0 . . ? C83 C84 H84 120.0 . . ? C85 C84 H84 120.0 . . ? C86 C85 C84 120.0 . . ? C86 C85 H85 120.0 . . ? C84 C85 H85 120.0 . . ? C85 C86 C87 120.0 . . ? C85 C86 H86 120.0 . . ? C87 C86 H86 120.0 . . ? C86 C87 C88 120.0 . . ? C86 C87 H87 120.0 . . ? C88 C87 H87 120.0 . . ? C87 C88 C83 120.0 . . ? C87 C88 H88 120.0 . . ? C83 C88 H88 120.0 . . ? O6 C89 C90 117.5(10) . . ? O6 C89 C92 119.1(11) . . ? C90 C89 C92 123.4(11) . . ? C89 C90 C91 120.0(10) . . ? C89 C90 H90 120.0 . . ? C91 C90 H90 120.0 . . ? O7 C91 C90 121.9(9) . . ? O7 C91 Ru2 131.0(8) . . ? C90 C91 Ru2 107.1(7) . . ? C93 C92 C97 120.0 . . ? C93 C92 C89 120.0(8) . . ? C97 C92 C89 119.8(8) . . ? C94 C93 C92 120.0 . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C95 C94 C93 120.0 . . ? C95 C94 H94 120.0 . . ? C93 C94 H94 120.0 . . ? C94 C95 C96 120.0 . . ? C94 C95 H95 120.0 . . ? C96 C95 H95 120.0 . . ? C95 C96 C97 120.0 . . ? C95 C96 H96 120.0 . . ? C97 C96 H96 120.0 . . ? C96 C97 C92 120.0 . . ? C96 C97 H97 120.0 . . ? C92 C97 H97 120.0 . . ? O8 C98 Ru2 175.9(10) . . ? C74 O5 C62 119.5(8) . . ? C74 O5 Ru2 119.4(6) . . ? C62 O5 Ru2 120.0(6) . . ? C89 O6 Ru2 111.8(7) . . ? C98 Ru2 C91 90.1(4) . . ? C98 Ru2 O6 173.4(4) . . ? C91 Ru2 O6 83.4(4) . . ? C98 Ru2 P3 92.0(3) . . ? C91 Ru2 P3 100.8(3) . . ? O6 Ru2 P3 88.1(2) . . ? C98 Ru2 O5 98.5(4) . . ? C91 Ru2 O5 171.3(4) . . ? O6 Ru2 O5 88.0(3) . . ? P3 Ru2 O5 79.86(19) . . ? C98 Ru2 P4 94.8(3) . . ? C91 Ru2 P4 97.9(3) . . ? O6 Ru2 P4 87.3(2) . . ? P3 Ru2 P4 160.05(11) . . ? O5 Ru2 P4 80.59(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.0 . . . . ? P1 C1 C2 C3 176.3(6) . . . . ? C1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C1 0.0 . . . . ? C2 C1 C6 C5 0.0 . . . . ? P1 C1 C6 C5 -176.1(6) . . . . ? C12 C7 C8 C9 0.0 . . . . ? P1 C7 C8 C9 179.6(6) . . . . ? C7 C8 C9 C10 0.0 . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C7 0.0 . . . . ? C8 C7 C12 C11 0.0 . . . . ? P1 C7 C12 C11 -179.6(5) . . . . ? C18 C13 C14 C15 3.0(18) . . . . ? O1 C13 C14 C15 -176.3(10) . . . . ? C18 C13 C14 P1 -174.0(9) . . . . ? O1 C13 C14 P1 6.7(14) . . . . ? C13 C14 C15 C16 -1.1(19) . . . . ? P1 C14 C15 C16 176.0(11) . . . . ? C14 C15 C16 C17 -1(2) . . . . ? C15 C16 C17 C18 1(2) . . . . ? O1 C13 C18 C17 176.5(11) . . . . ? C14 C13 C18 C17 -2.7(18) . . . . ? O1 C13 C18 C19 -4.8(18) . . . . ? C14 C13 C18 C19 176.0(11) . . . . ? C16 C17 C18 C13 0(2) . . . . ? C16 C17 C18 C19 -178.2(13) . . . . ? C13 C18 C19 C20 17.7(16) . . . . ? C17 C18 C19 C20 -163.7(11) . . . . ? C13 C18 C19 C26 -101.9(13) . . . . ? C17 C18 C19 C26 76.8(14) . . . . ? C13 C18 C19 C27 139.7(12) . . . . ? C17 C18 C19 C27 -41.7(17) . . . . ? C18 C19 C20 C25 -14.9(16) . . . . ? C26 C19 C20 C25 103.7(13) . . . . ? C27 C19 C20 C25 -136.8(12) . . . . ? C18 C19 C20 C21 165.7(11) . . . . ? C26 C19 C20 C21 -75.7(14) . . . . ? C27 C19 C20 C21 43.8(14) . . . . ? C25 C20 C21 C22 -2.7(17) . . . . ? C19 C20 C21 C22 176.7(11) . . . . ? C20 C21 C22 C23 4.0(19) . . . . ? C21 C22 C23 C24 -4.5(18) . . . . ? C22 C23 C24 C25 3.8(17) . . . . ? C22 C23 C24 P2 179.6(9) . . . . ? C21 C20 C25 C24 2.2(18) . . . . ? C19 C20 C25 C24 -177.3(11) . . . . ? C21 C20 C25 O1 178.5(10) . . . . ? C19 C20 C25 O1 -1.0(18) . . . . ? C23 C24 C25 C20 -2.8(19) . . . . ? P2 C24 C25 C20 -178.4(9) . . . . ? C23 C24 C25 O1 -179.4(10) . . . . ? P2 C24 C25 O1 5.1(15) . . . . ? C33 C28 C29 C30 0.0 . . . . ? P2 C28 C29 C30 -178.1(8) . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C28 0.0 . . . . ? C29 C28 C33 C32 0.0 . . . . ? P2 C28 C33 C32 178.0(8) . . . . ? C39 C34 C35 C36 0.0 . . . . ? P2 C34 C35 C36 -179.9(8) . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C34 0.0 . . . . ? C35 C34 C39 C38 0.0 . . . . ? P2 C34 C39 C38 179.9(7) . . . . ? O2 C40 C41 C42 0.3(17) . . . . ? C43 C40 C41 C42 -176.2(10) . . . . ? C40 C41 C42 O3 178.4(11) . . . . ? C40 C41 C42 Ru1 -2.4(13) . . . . ? O2 C40 C43 C44 -38.0(12) . . . . ? C41 C40 C43 C44 138.6(10) . . . . ? O2 C40 C43 C48 146.0(8) . . . . ? C41 C40 C43 C48 -37.4(13) . . . . ? C48 C43 C44 C45 0.0 . . . . ? C40 C43 C44 C45 -176.0(9) . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C48 0.0 . . . . ? C46 C47 C48 C43 0.0 . . . . ? C44 C43 C48 C47 0.0 . . . . ? C40 C43 C48 C47 176.0(9) . . . . ? C18 C13 O1 C25 -12.6(15) . . . . ? C14 C13 O1 C25 166.6(10) . . . . ? C18 C13 O1 Ru1 -169.9(9) . . . . ? C14 C13 O1 Ru1 9.4(12) . . . . ? C20 C25 O1 C13 15.6(16) . . . . ? C24 C25 O1 C13 -167.8(10) . . . . ? C20 C25 O1 Ru1 172.9(9) . . . . ? C24 C25 O1 Ru1 -10.5(13) . . . . ? C41 C40 O2 Ru1 1.9(13) . . . . ? C43 C40 O2 Ru1 178.5(7) . . . . ? C2 C1 P1 C7 53.5(5) . . . . ? C6 C1 P1 C7 -130.3(5) . . . . ? C2 C1 P1 C14 164.4(5) . . . . ? C6 C1 P1 C14 -19.4(6) . . . . ? C2 C1 P1 Ru1 -85.7(4) . . . . ? C6 C1 P1 Ru1 90.5(5) . . . . ? C8 C7 P1 C1 35.3(5) . . . . ? C12 C7 P1 C1 -145.1(5) . . . . ? C8 C7 P1 C14 -73.4(6) . . . . ? C12 C7 P1 C14 106.1(6) . . . . ? C8 C7 P1 Ru1 169.3(3) . . . . ? C12 C7 P1 Ru1 -11.1(5) . . . . ? C15 C14 P1 C1 -75.7(10) . . . . ? C13 C14 P1 C1 101.3(10) . . . . ? C15 C14 P1 C7 33.7(11) . . . . ? C13 C14 P1 C7 -149.2(9) . . . . ? C15 C14 P1 Ru1 165.1(9) . . . . ? C13 C14 P1 Ru1 -17.9(10) . . . . ? C29 C28 P2 C34 -157.9(6) . . . . ? C33 C28 P2 C34 24.1(7) . . . . ? C29 C28 P2 C24 -47.7(7) . . . . ? C33 C28 P2 C24 134.3(7) . . . . ? C29 C28 P2 Ru1 65.4(7) . . . . ? C33 C28 P2 Ru1 -112.6(6) . . . . ? C35 C34 P2 C28 108.3(6) . . . . ? C39 C34 P2 C28 -71.6(7) . . . . ? C35 C34 P2 C24 -0.2(8) . . . . ? C39 C34 P2 C24 179.9(6) . . . . ? C35 C34 P2 Ru1 -112.1(5) . . . . ? C39 C34 P2 Ru1 68.0(6) . . . . ? C25 C24 P2 C28 130.0(11) . . . . ? C23 C24 P2 C28 -45.6(10) . . . . ? C25 C24 P2 C34 -120.2(11) . . . . ? C23 C24 P2 C34 64.2(11) . . . . ? C25 C24 P2 Ru1 2.3(11) . . . . ? C23 C24 P2 Ru1 -173.3(9) . . . . ? O4 C49 Ru1 C42 -37(8) . . . . ? O4 C49 Ru1 O2 0(11) . . . . ? O4 C49 Ru1 P2 66(8) . . . . ? O4 C49 Ru1 P1 -133(8) . . . . ? O4 C49 Ru1 O1 147(8) . . . . ? O3 C42 Ru1 C49 -2.0(11) . . . . ? C41 C42 Ru1 C49 178.9(8) . . . . ? O3 C42 Ru1 O2 -178.3(11) . . . . ? C41 C42 Ru1 O2 2.5(7) . . . . ? O3 C42 Ru1 P2 -94.3(11) . . . . ? C41 C42 Ru1 P2 86.6(8) . . . . ? O3 C42 Ru1 P1 93.1(11) . . . . ? C41 C42 Ru1 P1 -86.1(8) . . . . ? O3 C42 Ru1 O1 161.8(10) . . . . ? C41 C42 Ru1 O1 -17.4(19) . . . . ? C40 O2 Ru1 C49 -41(4) . . . . ? C40 O2 Ru1 C42 -2.5(7) . . . . ? C40 O2 Ru1 P2 -106.2(7) . . . . ? C40 O2 Ru1 P1 93.3(7) . . . . ? C40 O2 Ru1 O1 172.6(7) . . . . ? C28 P2 Ru1 C49 -17.8(5) . . . . ? C34 P2 Ru1 C49 -149.8(5) . . . . ? C24 P2 Ru1 C49 96.0(5) . . . . ? C28 P2 Ru1 C42 75.2(5) . . . . ? C34 P2 Ru1 C42 -56.8(5) . . . . ? C24 P2 Ru1 C42 -170.9(5) . . . . ? C28 P2 Ru1 O2 156.8(4) . . . . ? C34 P2 Ru1 O2 24.8(4) . . . . ? C24 P2 Ru1 O2 -89.4(5) . . . . ? C28 P2 Ru1 P1 -126.5(5) . . . . ? C34 P2 Ru1 P1 101.5(4) . . . . ? C24 P2 Ru1 P1 -12.7(6) . . . . ? C28 P2 Ru1 O1 -119.0(4) . . . . ? C34 P2 Ru1 O1 109.0(4) . . . . ? C24 P2 Ru1 O1 -5.2(5) . . . . ? C1 P1 Ru1 C49 163.4(4) . . . . ? C7 P1 Ru1 C49 33.4(5) . . . . ? C14 P1 Ru1 C49 -85.9(5) . . . . ? C1 P1 Ru1 C42 70.3(4) . . . . ? C7 P1 Ru1 C42 -59.7(4) . . . . ? C14 P1 Ru1 C42 -178.9(5) . . . . ? C1 P1 Ru1 O2 -12.3(3) . . . . ? C7 P1 Ru1 O2 -142.3(4) . . . . ? C14 P1 Ru1 O2 98.4(4) . . . . ? C1 P1 Ru1 P2 -88.5(4) . . . . ? C7 P1 Ru1 P2 141.6(4) . . . . ? C14 P1 Ru1 P2 22.3(5) . . . . ? C1 P1 Ru1 O1 -96.0(3) . . . . ? C7 P1 Ru1 O1 134.1(4) . . . . ? C14 P1 Ru1 O1 14.8(4) . . . . ? C13 O1 Ru1 C49 76.4(8) . . . . ? C25 O1 Ru1 C49 -80.2(8) . . . . ? C13 O1 Ru1 C42 -87.0(15) . . . . ? C25 O1 Ru1 C42 116.3(15) . . . . ? C13 O1 Ru1 O2 -106.9(7) . . . . ? C25 O1 Ru1 O2 96.5(8) . . . . ? C13 O1 Ru1 P2 166.3(7) . . . . ? C25 O1 Ru1 P2 9.6(7) . . . . ? C13 O1 Ru1 P1 -16.4(7) . . . . ? C25 O1 Ru1 P1 -173.0(8) . . . . ? C56 P3 C50 C51 111.9(6) . . . . ? C63 P3 C50 C51 2.0(7) . . . . ? Ru2 P3 C50 C51 -113.2(5) . . . . ? C56 P3 C50 C55 -66.5(6) . . . . ? C63 P3 C50 C55 -176.4(5) . . . . ? Ru2 P3 C50 C55 68.4(5) . . . . ? C55 C50 C51 C52 0.0 . . . . ? P3 C50 C51 C52 -178.3(7) . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C50 0.0 . . . . ? C51 C50 C55 C54 0.0 . . . . ? P3 C50 C55 C54 178.5(7) . . . . ? C50 P3 C56 C57 -123.9(7) . . . . ? C63 P3 C56 C57 -12.3(8) . . . . ? Ru2 P3 C56 C57 98.5(7) . . . . ? C50 P3 C56 C61 62.1(7) . . . . ? C63 P3 C56 C61 173.7(7) . . . . ? Ru2 P3 C56 C61 -75.5(7) . . . . ? C61 C56 C57 C58 0.0 . . . . ? P3 C56 C57 C58 -173.9(8) . . . . ? C56 C57 C58 C59 0.0 . . . . ? C57 C58 C59 C60 0.0 . . . . ? C58 C59 C60 C61 0.0 . . . . ? C59 C60 C61 C56 0.0 . . . . ? C57 C56 C61 C60 0.0 . . . . ? P3 C56 C61 C60 174.1(8) . . . . ? C67 C62 C63 C64 2.3(18) . . . . ? O5 C62 C63 C64 180.0(11) . . . . ? C67 C62 C63 P3 -172.6(9) . . . . ? O5 C62 C63 P3 5.0(15) . . . . ? C50 P3 C63 C62 -131.6(10) . . . . ? C56 P3 C63 C62 115.4(10) . . . . ? Ru2 P3 C63 C62 -4.6(10) . . . . ? C50 P3 C63 C64 53.5(11) . . . . ? C56 P3 C63 C64 -59.5(11) . . . . ? Ru2 P3 C63 C64 -179.5(10) . . . . ? C62 C63 C64 C65 -0.2(19) . . . . ? P3 C63 C64 C65 174.8(10) . . . . ? C63 C64 C65 C66 0(2) . . . . ? C64 C65 C66 C67 -3(2) . . . . ? C63 C62 C67 C66 -4.4(18) . . . . ? O5 C62 C67 C66 178.1(10) . . . . ? C63 C62 C67 C68 180.0(11) . . . . ? O5 C62 C67 C68 2.5(18) . . . . ? C65 C66 C67 C62 4.5(17) . . . . ? C65 C66 C67 C68 -179.8(12) . . . . ? C62 C67 C68 C69 -12.7(17) . . . . ? C66 C67 C68 C69 171.7(11) . . . . ? C62 C67 C68 C76 108.3(14) . . . . ? C66 C67 C68 C76 -67.3(15) . . . . ? C62 C67 C68 C75 -130.1(13) . . . . ? C66 C67 C68 C75 54.3(16) . . . . ? C67 C68 C69 C74 15.3(18) . . . . ? C76 C68 C69 C74 -106.3(16) . . . . ? C75 C68 C69 C74 133.0(15) . . . . ? C67 C68 C69 C70 -168.6(12) . . . . ? C76 C68 C69 C70 69.7(17) . . . . ? C75 C68 C69 C70 -50.9(18) . . . . ? C74 C69 C70 C71 -3(2) . . . . ? C68 C69 C70 C71 -179.3(13) . . . . ? C69 C70 C71 C72 6(2) . . . . ? C70 C71 C72 C73 -4(2) . . . . ? C71 C72 C73 C74 -0.5(18) . . . . ? C71 C72 C73 P4 -176.6(10) . . . . ? C77 P4 C73 C72 -65.5(10) . . . . ? C83 P4 C73 C72 42.7(10) . . . . ? Ru2 P4 C73 C72 168.7(9) . . . . ? C77 P4 C73 C74 118.4(9) . . . . ? C83 P4 C73 C74 -133.3(9) . . . . ? Ru2 P4 C73 C74 -7.3(10) . . . . ? C70 C69 C74 C73 -1.8(19) . . . . ? C68 C69 C74 C73 174.4(12) . . . . ? C70 C69 C74 O5 176.3(11) . . . . ? C68 C69 C74 O5 -7.6(19) . . . . ? C72 C73 C74 C69 3.5(18) . . . . ? P4 C73 C74 C69 179.6(10) . . . . ? C72 C73 C74 O5 -174.6(10) . . . . ? P4 C73 C74 O5 1.5(15) . . . . ? C83 P4 C77 C78 -82.0(5) . . . . ? C73 P4 C77 C78 25.5(6) . . . . ? Ru2 P4 C77 C78 140.1(4) . . . . ? C83 P4 C77 C82 85.6(5) . . . . ? C73 P4 C77 C82 -166.9(5) . . . . ? Ru2 P4 C77 C82 -52.4(4) . . . . ? C82 C77 C78 C79 0.0 . . . . ? P4 C77 C78 C79 166.9(6) . . . . ? C77 C78 C79 C80 0.0 . . . . ? C78 C79 C80 C81 0.0 . . . . ? C79 C80 C81 C82 0.0 . . . . ? C80 C81 C82 C77 0.0 . . . . ? C78 C77 C82 C81 0.0 . . . . ? P4 C77 C82 C81 -168.3(5) . . . . ? C77 P4 C83 C84 -16.9(6) . . . . ? C73 P4 C83 C84 -128.2(5) . . . . ? Ru2 P4 C83 C84 119.9(4) . . . . ? C77 P4 C83 C88 168.0(4) . . . . ? C73 P4 C83 C88 56.6(5) . . . . ? Ru2 P4 C83 C88 -55.3(5) . . . . ? C88 C83 C84 C85 0.0 . . . . ? P4 C83 C84 C85 -175.1(6) . . . . ? C83 C84 C85 C86 0.0 . . . . ? C84 C85 C86 C87 0.0 . . . . ? C85 C86 C87 C88 0.0 . . . . ? C86 C87 C88 C83 0.0 . . . . ? C84 C83 C88 C87 0.0 . . . . ? P4 C83 C88 C87 175.2(6) . . . . ? O6 C89 C90 C91 4.3(16) . . . . ? C92 C89 C90 C91 -174.4(9) . . . . ? C89 C90 C91 O7 179.3(11) . . . . ? C89 C90 C91 Ru2 -1.7(13) . . . . ? O6 C89 C92 C93 24.1(13) . . . . ? C90 C89 C92 C93 -157.1(10) . . . . ? O6 C89 C92 C97 -150.3(9) . . . . ? C90 C89 C92 C97 28.5(14) . . . . ? C97 C92 C93 C94 0.0 . . . . ? C89 C92 C93 C94 -174.3(9) . . . . ? C92 C93 C94 C95 0.0 . . . . ? C93 C94 C95 C96 0.0 . . . . ? C94 C95 C96 C97 0.0 . . . . ? C95 C96 C97 C92 0.0 . . . . ? C93 C92 C97 C96 0.0 . . . . ? C89 C92 C97 C96 174.3(9) . . . . ? C69 C74 O5 C62 -4.5(16) . . . . ? C73 C74 O5 C62 173.7(10) . . . . ? C69 C74 O5 Ru2 -172.3(9) . . . . ? C73 C74 O5 Ru2 5.9(13) . . . . ? C67 C62 O5 C74 7.2(16) . . . . ? C63 C62 O5 C74 -170.5(10) . . . . ? C67 C62 O5 Ru2 174.9(9) . . . . ? C63 C62 O5 Ru2 -2.8(13) . . . . ? C90 C89 O6 Ru2 -4.5(12) . . . . ? C92 C89 O6 Ru2 174.4(7) . . . . ? O8 C98 Ru2 C91 5(14) . . . . ? O8 C98 Ru2 O6 -5(17) . . . . ? O8 C98 Ru2 P3 -95(14) . . . . ? O8 C98 Ru2 O5 -176(100) . . . . ? O8 C98 Ru2 P4 103(14) . . . . ? O7 C91 Ru2 C98 -0.6(11) . . . . ? C90 C91 Ru2 C98 -179.4(7) . . . . ? O7 C91 Ru2 O6 178.2(11) . . . . ? C90 C91 Ru2 O6 -0.5(7) . . . . ? O7 C91 Ru2 P3 91.4(11) . . . . ? C90 C91 Ru2 P3 -87.3(7) . . . . ? O7 C91 Ru2 O5 -174.8(17) . . . . ? C90 C91 Ru2 O5 6(3) . . . . ? O7 C91 Ru2 P4 -95.5(11) . . . . ? C90 C91 Ru2 P4 85.7(7) . . . . ? C89 O6 Ru2 C98 13(4) . . . . ? C89 O6 Ru2 C91 2.7(7) . . . . ? C89 O6 Ru2 P3 103.9(7) . . . . ? C89 O6 Ru2 O5 -176.2(7) . . . . ? C89 O6 Ru2 P4 -95.5(7) . . . . ? C50 P3 Ru2 C98 20.6(5) . . . . ? C56 P3 Ru2 C98 152.3(5) . . . . ? C63 P3 Ru2 C98 -96.4(5) . . . . ? C50 P3 Ru2 C91 -69.9(5) . . . . ? C56 P3 Ru2 C91 61.9(5) . . . . ? C63 P3 Ru2 C91 173.2(5) . . . . ? C50 P3 Ru2 O6 -152.9(4) . . . . ? C56 P3 Ru2 O6 -21.1(4) . . . . ? C63 P3 Ru2 O6 90.2(4) . . . . ? C50 P3 Ru2 O5 118.9(4) . . . . ? C56 P3 Ru2 O5 -109.3(4) . . . . ? C63 P3 Ru2 O5 2.0(4) . . . . ? C50 P3 Ru2 P4 130.6(4) . . . . ? C56 P3 Ru2 P4 -97.7(5) . . . . ? C63 P3 Ru2 P4 13.6(5) . . . . ? C74 O5 Ru2 C98 -101.8(8) . . . . ? C62 O5 Ru2 C98 90.5(8) . . . . ? C74 O5 Ru2 C91 72(2) . . . . ? C62 O5 Ru2 C91 -95(2) . . . . ? C74 O5 Ru2 O6 79.2(8) . . . . ? C62 O5 Ru2 O6 -88.5(8) . . . . ? C74 O5 Ru2 P3 167.7(8) . . . . ? C62 O5 Ru2 P3 0.0(8) . . . . ? C74 O5 Ru2 P4 -8.3(7) . . . . ? C62 O5 Ru2 P4 -176.0(8) . . . . ? C77 P4 Ru2 C98 -12.9(4) . . . . ? C83 P4 Ru2 C98 -143.1(4) . . . . ? C73 P4 Ru2 C98 104.7(5) . . . . ? C77 P4 Ru2 C91 77.8(4) . . . . ? C83 P4 Ru2 C91 -52.4(4) . . . . ? C73 P4 Ru2 C91 -164.6(5) . . . . ? C77 P4 Ru2 O6 160.8(3) . . . . ? C83 P4 Ru2 O6 30.6(4) . . . . ? C73 P4 Ru2 O6 -81.6(4) . . . . ? C77 P4 Ru2 P3 -122.4(4) . . . . ? C83 P4 Ru2 P3 107.3(4) . . . . ? C73 P4 Ru2 P3 -4.9(5) . . . . ? C77 P4 Ru2 O5 -110.8(4) . . . . ? C83 P4 Ru2 O5 119.0(4) . . . . ? C73 P4 Ru2 O5 6.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.906 _refine_diff_density_min -1.594 _refine_diff_density_rms 0.167