Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Carty, A. J.' 'Enright, Gary D.' 'Goeta, Andres E.' 'Hayes, Tim M.' 'Howard, Judith A. K.' 'Low, Paul J.' 'Udachin, Kostantin A.' _publ_contact_author_name 'Dr Paul J Low' _publ_contact_author_address ; Dr Paul J Low Department of Chemistry University of Durham South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email 'P.J.Low@durham.ac.uk' _publ_section_title ; Acetylide generation and coupling on electron-rich Ru3 clusters ; data_pjl54 _database_code_CSD 153694 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H38 O6 P2 Ru3' _chemical_formula_weight 1003.87 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.4209(14) _cell_length_b 9.4333(7) _cell_length_c 44.914(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.4240(10) _cell_angle_gamma 90.00 _cell_volume 8117.3(10) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4000 _exptl_absorpt_coefficient_mu 1.226 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _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 36640 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.73 _reflns_number_total 10344 _reflns_number_gt 9490 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+76.0943P] 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 10344 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.1017 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.132110(17) 0.04806(4) 0.082400(8) 0.02587(8) Uani 1 d . . . Ru2 Ru 0.168666(17) 0.29424(4) 0.132024(8) 0.02585(8) Uani 1 d . . . Ru3 Ru 0.150410(16) 0.00195(4) 0.149507(8) 0.02476(8) Uani 1 d . . . P1 P 0.11680(5) 0.28901(12) 0.08154(3) 0.0255(2) Uani 1 d . . . P2 P 0.22013(6) 0.17946(13) 0.17658(3) 0.0308(2) Uani 1 d . . . O7 O 0.28308(19) 0.0885(5) 0.07725(11) 0.0554(11) Uani 1 d . . . O8 O 0.0989(3) 0.0120(6) 0.01475(9) 0.0716(15) Uani 1 d . . . O9 O 0.30844(19) 0.3863(5) 0.11538(10) 0.0565(11) Uani 1 d . . . O10 O 0.1317(3) 0.5896(4) 0.14827(12) 0.0665(13) Uani 1 d . . . O11 O 0.2611(2) -0.1958(4) 0.13428(10) 0.0522(10) Uani 1 d . . . O12 O 0.1363(2) -0.1880(4) 0.20267(9) 0.0496(10) Uani 1 d . . . C1 C 0.0851(2) 0.2089(5) 0.14806(10) 0.0263(8) Uani 1 d . . . C2 C 0.0461(2) 0.1369(5) 0.16069(10) 0.0292(9) Uani 1 d . . . C3 C -0.0150(2) 0.0890(5) 0.17437(11) 0.0323(9) Uani 1 d . . . C4 C 0.0828(2) -0.0711(4) 0.11392(9) 0.0242(8) Uani 1 d . . . C5 C 0.0476(2) -0.1013(5) 0.08879(10) 0.0276(8) Uani 1 d . . . C6 C -0.0140(2) -0.1760(5) 0.07090(11) 0.0321(9) Uani 1 d . . . C7 C 0.2257(3) 0.0809(5) 0.07977(12) 0.0368(11) Uani 1 d . . . C8 C 0.1090(3) 0.0229(6) 0.04059(12) 0.0421(12) Uani 1 d . . . C9 C 0.2566(2) 0.3510(6) 0.12113(12) 0.0370(10) Uani 1 d . . . C10 C 0.1476(3) 0.4781(5) 0.14227(12) 0.0370(11) Uani 1 d . . . C11 C 0.2204(2) -0.1177(5) 0.14039(12) 0.0347(10) Uani 1 d . . . C12 C 0.1402(2) -0.1133(5) 0.18296(11) 0.0348(10) Uani 1 d . . . C20 C 0.1620(2) 0.3980(5) 0.05706(11) 0.0314(9) Uani 1 d . . . C21 C 0.1759(3) 0.5398(6) 0.06537(12) 0.0405(11) Uani 1 d . . . H21 H 0.1586 0.5779 0.0823 0.049 Uiso 1 calc R . . C22 C 0.2145(3) 0.6247(6) 0.04910(13) 0.0474(13) Uani 1 d . . . H22 H 0.2231 0.7209 0.0548 0.057 Uiso 1 calc R . . C23 C 0.2406(3) 0.5706(7) 0.02482(14) 0.0487(14) Uani 1 d . . . H23 H 0.2691 0.6280 0.0144 0.058 Uiso 1 calc R . . C24 C 0.2255(3) 0.4342(7) 0.01558(14) 0.0521(15) Uani 1 d . . . H24 H 0.2417 0.3985 -0.0018 0.063 Uiso 1 calc R . . C25 C 0.1865(3) 0.3474(6) 0.03166(13) 0.0429(12) Uani 1 d . . . H25 H 0.1764 0.2526 0.0252 0.051 Uiso 1 calc R . . C31 C -0.0726(3) 0.1989(8) 0.16570(17) 0.0638(19) Uani 1 d . . . H31A H -0.0678 0.2744 0.1809 0.077 Uiso 1 calc R . . H31B H -0.1183 0.1533 0.1647 0.077 Uiso 1 calc R . . H31C H -0.0687 0.2395 0.1460 0.077 Uiso 1 calc R . . C32 C -0.0412(3) -0.0535(7) 0.16137(13) 0.0477(13) Uani 1 d . . . H32A H -0.0493 -0.0484 0.1393 0.057 Uiso 1 calc R . . H32B H -0.0850 -0.0773 0.1684 0.057 Uiso 1 calc R . . H32C H -0.0063 -0.1267 0.1681 0.057 Uiso 1 calc R . . C33 C 0.0045(3) 0.0786(7) 0.20868(12) 0.0485(14) Uani 1 d . . . H33A H 0.0477 0.0237 0.2138 0.058 Uiso 1 calc R . . H33B H -0.0332 0.0314 0.2169 0.058 Uiso 1 calc R . . H33C H 0.0116 0.1740 0.2173 0.058 Uiso 1 calc R . . C40 C 0.0247(2) 0.3220(4) 0.06736(10) 0.0269(8) Uani 1 d . . . C41 C 0.0012(2) 0.3513(6) 0.03698(12) 0.0370(11) Uani 1 d . . . H41 H 0.0338 0.3584 0.0234 0.044 Uiso 1 calc R . . C42 C -0.0695(3) 0.3700(6) 0.02638(12) 0.0400(11) Uani 1 d . . . H42 H -0.0853 0.3900 0.0056 0.048 Uiso 1 calc R . . C43 C -0.1168(2) 0.3594(5) 0.04614(12) 0.0376(11) Uani 1 d . . . H43 H -0.1652 0.3722 0.0389 0.045 Uiso 1 calc R . . C44 C -0.0943(2) 0.3303(6) 0.07615(12) 0.0395(11) Uani 1 d . . . H44 H -0.1272 0.3226 0.0896 0.047 Uiso 1 calc R . . C45 C -0.0236(2) 0.3123(5) 0.08696(11) 0.0341(10) Uani 1 d . . . H45 H -0.0082 0.2933 0.1078 0.041 Uiso 1 calc R . . C50 C 0.3146(2) 0.1663(6) 0.18570(13) 0.0408(12) Uani 1 d . . . C51 C 0.3516(3) 0.1034(6) 0.16540(16) 0.0501(15) Uani 1 d . . . H51 H 0.3276 0.0701 0.1466 0.060 Uiso 1 calc R . . C52 C 0.4241(3) 0.0883(7) 0.1724(2) 0.069(2) Uani 1 d . . . H52 H 0.4495 0.0451 0.1584 0.083 Uiso 1 calc R . . C53 C 0.4585(3) 0.1376(9) 0.2000(2) 0.088(3) Uani 1 d . . . H53 H 0.5074 0.1241 0.2054 0.105 Uiso 1 calc R . . C54 C 0.4224(4) 0.2051(11) 0.21945(19) 0.087(3) Uani 1 d . . . H54 H 0.4470 0.2418 0.2379 0.104 Uiso 1 calc R . . C55 C 0.3509(3) 0.2214(8) 0.21287(14) 0.0585(18) Uani 1 d . . . H55 H 0.3266 0.2693 0.2266 0.070 Uiso 1 calc R . . C61 C 0.0022(3) -0.2438(7) 0.04177(13) 0.0482(13) Uani 1 d . . . H61A H 0.0241 -0.1733 0.0303 0.058 Uiso 1 calc R . . H61B H -0.0412 -0.2775 0.0296 0.058 Uiso 1 calc R . . H61C H 0.0341 -0.3239 0.0468 0.058 Uiso 1 calc R . . C62 C -0.0735(3) -0.0672(6) 0.06274(13) 0.0462(13) Uani 1 d . . . H62A H -0.0875 -0.0306 0.0813 0.055 Uiso 1 calc R . . H62B H -0.1135 -0.1132 0.0504 0.055 Uiso 1 calc R . . H62C H -0.0572 0.0113 0.0514 0.055 Uiso 1 calc R . . C63 C -0.0366(3) -0.2909(6) 0.09126(13) 0.0473(13) Uani 1 d . . . H63A H 0.0045 -0.3432 0.1011 0.057 Uiso 1 calc R . . H63B H -0.0689 -0.3564 0.0791 0.057 Uiso 1 calc R . . H63C H -0.0600 -0.2469 0.1067 0.057 Uiso 1 calc R . . C70 C 0.1942(3) 0.2300(6) 0.21228(12) 0.0403(11) Uani 1 d . . . C71 C 0.2061(3) 0.1366(7) 0.23699(12) 0.0479(13) Uani 1 d . . . H71 H 0.2270 0.0469 0.2349 0.057 Uiso 1 calc R . . C72 C 0.1873(4) 0.1751(9) 0.26436(14) 0.066(2) Uani 1 d . . . H72 H 0.1959 0.1118 0.2810 0.080 Uiso 1 calc R . . C73 C 0.1566(4) 0.3035(9) 0.26764(16) 0.074(2) Uani 1 d . . . H73 H 0.1443 0.3296 0.2865 0.089 Uiso 1 calc R . . C74 C 0.1439(5) 0.3930(8) 0.24388(17) 0.073(2) Uani 1 d . . . H74 H 0.1217 0.4812 0.2461 0.088 Uiso 1 calc R . . C75 C 0.1627(4) 0.3587(7) 0.21623(14) 0.0540(15) Uani 1 d . . . H75 H 0.1538 0.4240 0.1999 0.065 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02519(15) 0.02380(16) 0.02885(17) -0.00033(13) 0.00508(12) -0.00048(13) Ru2 0.02333(15) 0.02244(16) 0.03086(17) 0.00043(13) 0.00169(12) -0.00347(12) Ru3 0.02193(14) 0.02294(16) 0.02815(17) 0.00032(13) 0.00033(12) -0.00147(12) P1 0.0219(5) 0.0233(5) 0.0313(6) 0.0015(4) 0.0046(4) -0.0002(4) P2 0.0287(5) 0.0280(6) 0.0332(6) 0.0006(5) -0.0023(4) -0.0067(4) O7 0.0324(19) 0.060(3) 0.077(3) 0.002(2) 0.0191(19) 0.0069(18) O8 0.107(4) 0.075(3) 0.034(2) -0.006(2) 0.014(2) -0.029(3) O9 0.0305(18) 0.073(3) 0.065(3) 0.014(2) 0.0055(18) -0.0155(19) O10 0.100(4) 0.027(2) 0.074(3) -0.005(2) 0.021(3) 0.001(2) O11 0.0384(19) 0.045(2) 0.073(3) -0.004(2) 0.0082(19) 0.0123(17) O12 0.054(2) 0.047(2) 0.047(2) 0.0167(19) 0.0063(18) -0.0015(18) C1 0.0264(19) 0.0215(19) 0.030(2) -0.0062(16) 0.0013(16) -0.0040(15) C2 0.030(2) 0.024(2) 0.033(2) -0.0024(17) 0.0023(17) 0.0019(16) C3 0.030(2) 0.029(2) 0.039(3) 0.0017(19) 0.0095(18) -0.0017(17) C4 0.0245(18) 0.0194(19) 0.028(2) 0.0024(15) 0.0029(15) 0.0002(15) C5 0.0279(19) 0.022(2) 0.033(2) -0.0020(17) 0.0036(17) 0.0012(16) C6 0.027(2) 0.029(2) 0.038(2) -0.0017(19) 0.0005(18) -0.0027(17) C7 0.035(2) 0.032(3) 0.046(3) 0.001(2) 0.013(2) 0.0029(19) C8 0.050(3) 0.039(3) 0.039(3) 0.001(2) 0.010(2) -0.009(2) C9 0.031(2) 0.037(3) 0.041(3) 0.007(2) -0.0017(19) -0.0038(19) C10 0.048(3) 0.020(2) 0.044(3) 0.0029(19) 0.010(2) -0.0025(19) C11 0.027(2) 0.033(2) 0.043(3) 0.003(2) -0.0006(18) -0.0007(18) C12 0.029(2) 0.037(3) 0.036(2) 0.003(2) -0.0013(18) -0.0021(19) C20 0.0203(18) 0.039(3) 0.033(2) 0.0078(19) 0.0003(16) 0.0014(17) C21 0.043(3) 0.038(3) 0.039(3) 0.006(2) 0.001(2) -0.010(2) C22 0.051(3) 0.038(3) 0.050(3) 0.013(2) 0.000(3) -0.013(2) C23 0.036(3) 0.054(4) 0.057(3) 0.023(3) 0.008(2) -0.004(2) C24 0.053(3) 0.055(4) 0.055(4) 0.015(3) 0.029(3) 0.006(3) C25 0.047(3) 0.033(3) 0.053(3) 0.009(2) 0.021(2) 0.004(2) C31 0.047(3) 0.070(4) 0.082(5) 0.029(4) 0.033(3) 0.019(3) C32 0.038(3) 0.055(3) 0.052(3) -0.005(3) 0.014(2) -0.016(2) C33 0.048(3) 0.067(4) 0.032(3) -0.007(3) 0.011(2) -0.017(3) C40 0.0225(18) 0.022(2) 0.035(2) -0.0011(17) 0.0014(16) 0.0004(15) C41 0.028(2) 0.046(3) 0.037(3) 0.001(2) 0.0041(18) 0.001(2) C42 0.033(2) 0.051(3) 0.032(2) 0.000(2) -0.0032(19) 0.000(2) C43 0.024(2) 0.037(3) 0.048(3) -0.002(2) -0.0015(19) 0.0030(19) C44 0.025(2) 0.046(3) 0.048(3) 0.008(2) 0.010(2) 0.006(2) C45 0.029(2) 0.038(3) 0.036(2) 0.010(2) 0.0048(18) 0.0061(18) C50 0.030(2) 0.037(3) 0.051(3) 0.015(2) -0.009(2) -0.010(2) C51 0.030(2) 0.032(3) 0.086(5) 0.014(3) 0.002(3) -0.001(2) C52 0.033(3) 0.042(3) 0.132(7) 0.036(4) 0.012(4) 0.004(2) C53 0.026(3) 0.088(6) 0.136(8) 0.066(6) -0.024(4) -0.016(3) C54 0.041(4) 0.127(8) 0.079(5) 0.052(5) -0.026(3) -0.038(4) C55 0.044(3) 0.076(5) 0.048(3) 0.022(3) -0.013(2) -0.031(3) C61 0.048(3) 0.051(3) 0.046(3) -0.017(3) 0.007(2) -0.009(3) C62 0.035(2) 0.049(3) 0.051(3) -0.001(3) -0.006(2) 0.002(2) C63 0.050(3) 0.040(3) 0.050(3) -0.003(2) 0.003(2) -0.021(2) C70 0.043(3) 0.036(3) 0.042(3) -0.009(2) 0.007(2) -0.014(2) C71 0.059(3) 0.047(3) 0.035(3) -0.001(2) 0.001(2) -0.016(3) C72 0.083(5) 0.081(5) 0.037(3) -0.003(3) 0.014(3) -0.029(4) C73 0.097(6) 0.082(6) 0.048(4) -0.022(4) 0.024(4) -0.023(5) C74 0.104(6) 0.055(4) 0.065(5) -0.024(4) 0.027(4) -0.013(4) C75 0.077(4) 0.042(3) 0.042(3) -0.010(2) 0.007(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C7 1.867(5) . ? Ru1 C8 1.873(5) . ? Ru1 C4 2.152(4) . ? Ru1 C5 2.217(4) . ? Ru1 P1 2.2918(12) . ? Ru1 Ru3 3.0081(5) . ? Ru2 C10 1.858(5) . ? Ru2 C9 1.929(5) . ? Ru2 C1 2.045(4) . ? Ru2 P1 2.3260(12) . ? Ru2 P2 2.3497(13) . ? Ru2 Ru3 2.9044(5) . ? Ru3 C11 1.864(5) . ? Ru3 C12 1.892(5) . ? Ru3 C4 2.017(4) . ? Ru3 C1 2.323(4) . ? Ru3 P2 2.3616(12) . ? Ru3 C2 2.512(4) . ? P1 C40 1.824(4) . ? P1 C20 1.831(5) . ? P2 C50 1.818(5) . ? P2 C70 1.821(5) . ? O7 C7 1.140(6) . ? O8 C8 1.150(6) . ? O9 C9 1.129(6) . ? O10 C10 1.140(6) . ? O11 C11 1.145(6) . ? O12 C12 1.143(6) . ? C1 C2 1.224(6) . ? C2 C3 1.492(6) . ? C3 C32 1.520(7) . ? C3 C33 1.529(7) . ? C3 C31 1.529(7) . ? C4 C5 1.253(6) . ? C5 C6 1.503(6) . ? C6 C63 1.528(7) . ? C6 C61 1.534(7) . ? C6 C62 1.543(7) . ? C20 C25 1.390(7) . ? C20 C21 1.403(7) . ? C21 C22 1.385(7) . ? C22 C23 1.374(9) . ? C23 C24 1.369(9) . ? C24 C25 1.396(7) . ? C40 C45 1.390(6) . ? C40 C41 1.394(7) . ? C41 C42 1.389(6) . ? C42 C43 1.382(7) . ? C43 C44 1.375(7) . ? C44 C45 1.391(6) . ? C50 C51 1.384(8) . ? C50 C55 1.405(8) . ? C51 C52 1.399(7) . ? C52 C53 1.391(12) . ? C53 C54 1.363(13) . ? C54 C55 1.380(9) . ? C70 C75 1.384(8) . ? C70 C71 1.406(8) . ? C71 C72 1.387(8) . ? C72 C73 1.368(11) . ? C73 C74 1.351(11) . ? C74 C75 1.388(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Ru1 C8 91.9(2) . . ? C7 Ru1 C4 132.17(19) . . ? C8 Ru1 C4 122.26(19) . . ? C7 Ru1 C5 149.65(19) . . ? C8 Ru1 C5 89.3(2) . . ? C4 Ru1 C5 33.28(16) . . ? C7 Ru1 P1 87.67(16) . . ? C8 Ru1 P1 95.73(17) . . ? C4 Ru1 P1 117.32(11) . . ? C5 Ru1 P1 122.38(11) . . ? C7 Ru1 Ru3 97.52(17) . . ? C8 Ru1 Ru3 162.89(16) . . ? C4 Ru1 Ru3 42.06(11) . . ? C5 Ru1 Ru3 75.34(12) . . ? P1 Ru1 Ru3 98.86(3) . . ? C10 Ru2 C9 92.5(2) . . ? C10 Ru2 C1 93.47(19) . . ? C9 Ru2 C1 170.3(2) . . ? C10 Ru2 P1 100.56(17) . . ? C9 Ru2 P1 91.07(15) . . ? C1 Ru2 P1 95.34(12) . . ? C10 Ru2 P2 107.44(17) . . ? C9 Ru2 P2 94.19(15) . . ? C1 Ru2 P2 76.71(13) . . ? P1 Ru2 P2 151.21(4) . . ? C10 Ru2 Ru3 141.07(15) . . ? C9 Ru2 Ru3 118.99(16) . . ? C1 Ru2 Ru3 52.56(12) . . ? P1 Ru2 Ru3 101.00(3) . . ? P2 Ru2 Ru3 52.13(3) . . ? C11 Ru3 C12 90.1(2) . . ? C11 Ru3 C4 91.30(19) . . ? C12 Ru3 C4 107.07(19) . . ? C11 Ru3 C1 156.54(18) . . ? C12 Ru3 C1 112.18(18) . . ? C4 Ru3 C1 89.06(15) . . ? C11 Ru3 P2 99.49(15) . . ? C12 Ru3 P2 97.16(15) . . ? C4 Ru3 P2 153.45(12) . . ? C1 Ru3 P2 71.51(10) . . ? C11 Ru3 C2 172.85(18) . . ? C12 Ru3 C2 86.52(18) . . ? C4 Ru3 C2 83.68(15) . . ? C1 Ru3 C2 29.00(14) . . ? P2 Ru3 C2 87.19(11) . . ? C11 Ru3 Ru2 112.93(15) . . ? C12 Ru3 Ru2 142.55(16) . . ? C4 Ru3 Ru2 101.70(12) . . ? C1 Ru3 Ru2 44.35(10) . . ? P2 Ru3 Ru2 51.76(3) . . ? C2 Ru3 Ru2 73.21(10) . . ? C11 Ru3 Ru1 80.69(16) . . ? C12 Ru3 Ru1 150.29(15) . . ? C4 Ru3 Ru1 45.61(11) . . ? C1 Ru3 Ru1 82.88(11) . . ? P2 Ru3 Ru1 112.15(3) . . ? C2 Ru3 Ru1 99.22(11) . . ? Ru2 Ru3 Ru1 65.888(12) . . ? C40 P1 C20 103.5(2) . . ? C40 P1 Ru1 106.98(14) . . ? C20 P1 Ru1 119.55(16) . . ? C40 P1 Ru2 125.45(15) . . ? C20 P1 Ru2 113.56(15) . . ? Ru1 P1 Ru2 88.30(4) . . ? C50 P2 C70 103.5(3) . . ? C50 P2 Ru2 119.75(17) . . ? C70 P2 Ru2 119.27(19) . . ? C50 P2 Ru3 122.70(19) . . ? C70 P2 Ru3 114.91(16) . . ? Ru2 P2 Ru3 76.12(4) . . ? C2 C1 Ru2 165.7(4) . . ? C2 C1 Ru3 84.1(3) . . ? Ru2 C1 Ru3 83.10(15) . . ? C1 C2 C3 162.4(5) . . ? C1 C2 Ru3 66.9(3) . . ? C3 C2 Ru3 130.6(3) . . ? C2 C3 C32 110.4(4) . . ? C2 C3 C33 110.6(4) . . ? C32 C3 C33 110.0(4) . . ? C2 C3 C31 106.7(4) . . ? C32 C3 C31 108.5(5) . . ? C33 C3 C31 110.5(5) . . ? C5 C4 Ru3 168.6(4) . . ? C5 C4 Ru1 76.2(3) . . ? Ru3 C4 Ru1 92.33(16) . . ? C4 C5 C6 149.0(4) . . ? C4 C5 Ru1 70.5(3) . . ? C6 C5 Ru1 140.4(3) . . ? C5 C6 C63 107.1(4) . . ? C5 C6 C61 113.2(4) . . ? C63 C6 C61 109.5(4) . . ? C5 C6 C62 108.3(4) . . ? C63 C6 C62 109.7(4) . . ? C61 C6 C62 109.0(4) . . ? O7 C7 Ru1 173.7(5) . . ? O8 C8 Ru1 175.4(5) . . ? O9 C9 Ru2 178.3(5) . . ? O10 C10 Ru2 177.1(5) . . ? O11 C11 Ru3 176.8(5) . . ? O12 C12 Ru3 176.4(5) . . ? C25 C20 C21 118.0(5) . . ? C25 C20 P1 124.2(4) . . ? C21 C20 P1 117.7(4) . . ? C22 C21 C20 120.5(5) . . ? C23 C22 C21 120.4(6) . . ? C24 C23 C22 120.1(5) . . ? C23 C24 C25 120.1(6) . . ? C20 C25 C24 120.7(5) . . ? C45 C40 C41 119.1(4) . . ? C45 C40 P1 119.5(3) . . ? C41 C40 P1 121.4(3) . . ? C42 C41 C40 120.5(4) . . ? C43 C42 C41 119.6(5) . . ? C44 C43 C42 120.4(4) . . ? C43 C44 C45 120.2(4) . . ? C44 C45 C40 120.1(4) . . ? C51 C50 C55 119.3(5) . . ? C51 C50 P2 119.7(4) . . ? C55 C50 P2 121.0(5) . . ? C50 C51 C52 120.6(7) . . ? C53 C52 C51 119.0(8) . . ? C54 C53 C52 120.4(6) . . ? C53 C54 C55 121.3(8) . . ? C54 C55 C50 119.3(8) . . ? C75 C70 C71 117.8(5) . . ? C75 C70 P2 122.3(5) . . ? C71 C70 P2 119.8(4) . . ? C72 C71 C70 120.2(6) . . ? C73 C72 C71 120.6(7) . . ? C74 C73 C72 119.6(7) . . ? C73 C74 C75 121.4(7) . . ? C70 C75 C74 120.3(7) . . ? _diffrn_measured_fraction_theta_max 0.464 _diffrn_reflns_theta_full 28.73 _diffrn_measured_fraction_theta_full 0.464 _refine_diff_density_max 1.068 _refine_diff_density_min -1.284 _refine_diff_density_rms 0.116 #===END data_pjl56 _database_code_CSD 153695 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H34 O7 P2 Ru3' _chemical_formula_weight 1051.87 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7431(6) _cell_length_b 12.7649(6) _cell_length_c 16.5142(7) _cell_angle_alpha 68.4710(10) _cell_angle_beta 75.5390(10) _cell_angle_gamma 61.1850(10) _cell_volume 2180.69(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _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 26030 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.75 _reflns_number_total 11214 _reflns_number_gt 8937 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.3424P] 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 11214 _refine_ls_number_parameters 532 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.780 _refine_ls_shift/su_mean 0.083 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.433190(18) 0.384394(19) 0.198923(13) 0.02763(5) Uani 1 d . . . Ru2 Ru 0.305239(15) 0.238945(17) 0.339512(12) 0.02168(5) Uani 1 d . . . Ru3 Ru 0.193364(17) 0.386488(18) 0.171492(13) 0.02674(5) Uani 1 d . . . P1 P 0.36483(5) 0.38119(6) 0.34674(4) 0.02463(12) Uani 1 d . . . P2 P 0.23190(5) 0.18191(6) 0.25370(4) 0.02494(12) Uani 1 d . . . O7 O 0.5185(2) 0.3508(2) 0.01476(14) 0.0591(6) Uani 1 d . . . O8 O 0.66990(18) 0.1552(2) 0.25528(16) 0.0526(6) Uani 1 d . . . O9 O 0.54084(17) 0.00226(19) 0.36284(15) 0.0493(5) Uani 1 d . . . O10 O 0.22436(18) 0.1385(2) 0.52698(12) 0.0461(5) Uani 1 d . . . O11 O 0.2963(2) 0.3333(2) -0.00087(14) 0.0539(6) Uani 1 d . . . O12 O -0.0404(2) 0.4469(3) 0.11419(17) 0.0691(7) Uani 1 d . . . O13 O 0.5440(2) 0.5585(2) 0.17323(15) 0.0564(6) Uani 1 d . . . C1 C 0.1400(2) 0.3872(2) 0.31642(15) 0.0260(5) Uani 1 d . . . C2 C 0.0379(2) 0.4668(2) 0.30218(16) 0.0292(5) Uani 1 d . . . C4 C 0.2716(2) 0.5216(2) 0.15359(16) 0.0326(5) Uani 1 d . . . C5 C 0.1795(3) 0.5966(3) 0.11656(17) 0.0388(6) Uani 1 d D . . C6 C 0.0917(7) 0.7152(7) 0.0609(6) 0.0447(14) Uani 0.69 d PD A 1 C61 C 0.1518(9) 0.7361(11) -0.0324(6) 0.096(3) Uani 0.69 d PD A 1 H61A H 0.2261 0.7417 -0.0330 0.145 Uiso 0.69 calc PR A 1 H61B H 0.0971 0.8140 -0.0704 0.145 Uiso 0.69 calc PR A 1 H61C H 0.1708 0.6661 -0.0537 0.145 Uiso 0.69 calc PR A 1 C62 C -0.0313(4) 0.7233(5) 0.0587(3) 0.0601(14) Uani 0.69 d PD A 1 H62A H -0.0215 0.6639 0.0299 0.090 Uiso 0.69 calc PR A 1 H62B H -0.0832 0.8083 0.0262 0.090 Uiso 0.69 calc PR A 1 H62C H -0.0679 0.7030 0.1185 0.090 Uiso 0.69 calc PR A 1 C63 C 0.0680(7) 0.8198(5) 0.1005(4) 0.085(2) Uani 0.69 d PD A 1 H63A H 0.0393 0.7981 0.1625 0.128 Uiso 0.69 calc PR A 1 H63B H 0.0072 0.8997 0.0692 0.128 Uiso 0.69 calc PR A 1 H63C H 0.1429 0.8271 0.0947 0.128 Uiso 0.69 calc PR A 1 C6A C 0.1090(17) 0.7271(16) 0.0619(14) 0.0447(14) Uani 0.31 d PD A 2 C61A C -0.0201(12) 0.7607(16) 0.0953(9) 0.096(3) Uani 0.31 d PD A 2 H61D H -0.0389 0.6916 0.1025 0.145 Uiso 0.31 calc PR A 2 H61E H -0.0714 0.8361 0.0536 0.145 Uiso 0.31 calc PR A 2 H61F H -0.0347 0.7763 0.1519 0.145 Uiso 0.31 calc PR A 2 C62A C 0.1303(18) 0.721(2) -0.0307(11) 0.0601(14) Uani 0.31 d PD A 2 H62D H 0.2170 0.6830 -0.0473 0.090 Uiso 0.31 calc PR A 2 H62E H 0.0935 0.8057 -0.0703 0.090 Uiso 0.31 calc PR A 2 H62F H 0.0944 0.6706 -0.0347 0.090 Uiso 0.31 calc PR A 2 C63A C 0.1610(14) 0.8152(11) 0.0546(10) 0.085(2) Uani 0.31 d PD A 2 H63D H 0.1526 0.8256 0.1122 0.128 Uiso 0.31 calc PR A 2 H63E H 0.1177 0.8966 0.0135 0.128 Uiso 0.31 calc PR A 2 H63F H 0.2463 0.7804 0.0334 0.128 Uiso 0.31 calc PR A 2 C7 C 0.4823(3) 0.3617(3) 0.08240(18) 0.0366(6) Uani 1 d . . . C8 C 0.5802(2) 0.2381(3) 0.23809(18) 0.0350(6) Uani 1 d . . . C9 C 0.4549(2) 0.0935(2) 0.35249(17) 0.0303(5) Uani 1 d . . . C10 C 0.2547(2) 0.1768(2) 0.45581(17) 0.0301(5) Uani 1 d . . . C11 C 0.2618(2) 0.3524(3) 0.06528(18) 0.0350(6) Uani 1 d . . . C12 C 0.0476(3) 0.4266(3) 0.13607(19) 0.0433(7) Uani 1 d . . . C13 C 0.5017(3) 0.4945(3) 0.18196(18) 0.0397(6) Uani 1 d . . . C20 C 0.4812(2) 0.3327(2) 0.41657(16) 0.0282(5) Uani 1 d . . . C21 C 0.5218(2) 0.2158(3) 0.47833(18) 0.0394(6) Uani 1 d . . . H21 H 0.4902 0.1593 0.4838 0.047 Uiso 1 calc R . . C22 C 0.6082(3) 0.1813(3) 0.5320(2) 0.0492(8) Uani 1 d . . . H22 H 0.6357 0.1013 0.5739 0.059 Uiso 1 calc R . . C23 C 0.6545(2) 0.2627(3) 0.52468(19) 0.0439(7) Uani 1 d . . . H23 H 0.7124 0.2395 0.5624 0.053 Uiso 1 calc R . . C24 C 0.6167(3) 0.3771(3) 0.4628(2) 0.0490(8) Uani 1 d . . . H24 H 0.6502 0.4322 0.4566 0.059 Uiso 1 calc R . . C25 C 0.5298(3) 0.4127(3) 0.4095(2) 0.0420(7) Uani 1 d . . . H25 H 0.5032 0.4927 0.3675 0.050 Uiso 1 calc R . . C30 C -0.0854(2) 0.5596(2) 0.30122(16) 0.0294(5) Uani 1 d . . . C31 C -0.1140(2) 0.6737(3) 0.31193(19) 0.0373(6) Uani 1 d . . . H31 H -0.0519 0.6905 0.3181 0.045 Uiso 1 calc R . . C32 C -0.2316(3) 0.7628(3) 0.3137(2) 0.0473(7) Uani 1 d . . . H32 H -0.2505 0.8404 0.3213 0.057 Uiso 1 calc R . . C33 C -0.3217(3) 0.7387(3) 0.3044(2) 0.0493(8) Uani 1 d . . . H33 H -0.4028 0.8001 0.3053 0.059 Uiso 1 calc R . . C34 C -0.2946(3) 0.6255(3) 0.2939(2) 0.0491(8) Uani 1 d . . . H34 H -0.3572 0.6097 0.2874 0.059 Uiso 1 calc R . . C35 C -0.1771(2) 0.5353(3) 0.29263(19) 0.0396(6) Uani 1 d . . . H35 H -0.1589 0.4572 0.2860 0.048 Uiso 1 calc R . . C40 C 0.2522(2) 0.5265(2) 0.37001(16) 0.0271(5) Uani 1 d . . . C41 C 0.1873(2) 0.5219(3) 0.45164(17) 0.0355(6) Uani 1 d . . . H41 H 0.2032 0.4435 0.4946 0.043 Uiso 1 calc R . . C42 C 0.0996(3) 0.6308(3) 0.47111(18) 0.0397(6) Uani 1 d . . . H42 H 0.0560 0.6263 0.5271 0.048 Uiso 1 calc R . . C43 C 0.0758(2) 0.7455(2) 0.40904(18) 0.0347(6) Uani 1 d . . . H43 H 0.0157 0.8198 0.4223 0.042 Uiso 1 calc R . . C44 C 0.1391(2) 0.7519(2) 0.32809(18) 0.0323(5) Uani 1 d . . . H44 H 0.1230 0.8307 0.2855 0.039 Uiso 1 calc R . . C45 C 0.2271(2) 0.6424(2) 0.30841(17) 0.0303(5) Uani 1 d . . . H45 H 0.2702 0.6474 0.2522 0.036 Uiso 1 calc R . . C50 C 0.3331(2) 0.0558(2) 0.20591(16) 0.0291(5) Uani 1 d . . . C51 C 0.4351(2) 0.0617(3) 0.15209(18) 0.0377(6) Uani 1 d . . . H51 H 0.4502 0.1321 0.1404 0.045 Uiso 1 calc R . . C52 C 0.5146(3) -0.0339(3) 0.1155(2) 0.0461(7) Uani 1 d . . . H52 H 0.5827 -0.0277 0.0781 0.055 Uiso 1 calc R . . C53 C 0.4953(3) -0.1376(3) 0.1330(2) 0.0529(8) Uani 1 d . . . H53 H 0.5485 -0.2021 0.1068 0.063 Uiso 1 calc R . . C54 C 0.3991(3) -0.1468(3) 0.1885(3) 0.0641(10) Uani 1 d . . . H54 H 0.3874 -0.2198 0.2026 0.077 Uiso 1 calc R . . C55 C 0.3182(3) -0.0520(3) 0.2247(2) 0.0497(8) Uani 1 d . . . H55 H 0.2515 -0.0605 0.2630 0.060 Uiso 1 calc R . . C70 C 0.0972(2) 0.1549(2) 0.29290(17) 0.0302(5) Uani 1 d . . . C71 C 0.0388(3) 0.1474(4) 0.23557(19) 0.0523(9) Uani 1 d . . . H71 H 0.0706 0.1538 0.1764 0.063 Uiso 1 calc R . . C72 C -0.0653(3) 0.1306(4) 0.2646(2) 0.0643(11) Uani 1 d . . . H72 H -0.1041 0.1252 0.2251 0.077 Uiso 1 calc R . . C73 C -0.1132(3) 0.1217(3) 0.3501(2) 0.0505(8) Uani 1 d . . . H73 H -0.1849 0.1107 0.3697 0.061 Uiso 1 calc R . . C74 C -0.0564(3) 0.1289(3) 0.4063(2) 0.0472(8) Uani 1 d . . . H74 H -0.0893 0.1236 0.4652 0.057 Uiso 1 calc R . . C75 C 0.0489(2) 0.1440(3) 0.37841(18) 0.0386(6) Uani 1 d . . . H75 H 0.0882 0.1468 0.4189 0.046 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03283(10) 0.02788(10) 0.02520(10) -0.01000(8) 0.00302(8) -0.01645(9) Ru2 0.02017(9) 0.02102(9) 0.02372(10) -0.00854(7) -0.00098(7) -0.00782(7) Ru3 0.02908(10) 0.02583(10) 0.02302(10) -0.00911(8) -0.00289(7) -0.00845(8) P1 0.0266(3) 0.0243(3) 0.0250(3) -0.0091(2) -0.0005(2) -0.0121(2) P2 0.0245(3) 0.0274(3) 0.0258(3) -0.0114(3) 0.0005(2) -0.0121(2) O7 0.0729(16) 0.0814(18) 0.0387(12) -0.0310(12) 0.0185(11) -0.0466(14) O8 0.0303(10) 0.0551(14) 0.0640(15) -0.0157(12) -0.0037(10) -0.0134(10) O9 0.0298(10) 0.0336(11) 0.0676(15) -0.0119(10) -0.0026(10) -0.0037(9) O10 0.0468(12) 0.0642(14) 0.0274(10) -0.0074(10) 0.0004(9) -0.0301(11) O11 0.0596(14) 0.0672(16) 0.0349(11) -0.0279(11) 0.0045(10) -0.0222(12) O12 0.0411(12) 0.092(2) 0.0721(17) -0.0435(15) -0.0208(12) -0.0062(13) O13 0.0786(16) 0.0617(15) 0.0550(14) -0.0220(12) 0.0080(12) -0.0531(14) C1 0.0282(11) 0.0283(12) 0.0229(11) -0.0126(10) 0.0022(9) -0.0119(10) C2 0.0311(12) 0.0284(13) 0.0284(13) -0.0090(10) -0.0017(10) -0.0129(11) C4 0.0455(15) 0.0271(13) 0.0243(12) -0.0063(10) 0.0000(11) -0.0176(12) C5 0.0551(17) 0.0298(14) 0.0264(13) -0.0079(11) -0.0018(12) -0.0154(13) C6 0.060(3) 0.029(2) 0.0369(17) 0.0015(15) -0.017(2) -0.0146(18) C61 0.086(6) 0.112(7) 0.047(3) 0.017(4) -0.009(3) -0.037(4) C62 0.056(3) 0.051(3) 0.046(3) 0.001(2) -0.026(2) -0.003(2) C63 0.132(6) 0.025(2) 0.078(5) -0.004(3) -0.059(4) -0.003(3) C6A 0.060(3) 0.029(2) 0.0369(17) 0.0015(15) -0.017(2) -0.0146(18) C61A 0.086(6) 0.112(7) 0.047(3) 0.017(4) -0.009(3) -0.037(4) C62A 0.056(3) 0.051(3) 0.046(3) 0.001(2) -0.026(2) -0.003(2) C63A 0.132(6) 0.025(2) 0.078(5) -0.004(3) -0.059(4) -0.003(3) C7 0.0421(15) 0.0403(16) 0.0320(14) -0.0131(12) 0.0043(12) -0.0229(13) C8 0.0314(13) 0.0444(16) 0.0355(14) -0.0164(12) 0.0074(11) -0.0228(13) C9 0.0259(11) 0.0283(13) 0.0357(14) -0.0102(11) 0.0003(10) -0.0119(10) C10 0.0281(12) 0.0334(14) 0.0309(13) -0.0107(11) -0.0029(10) -0.0139(11) C11 0.0363(14) 0.0337(14) 0.0330(14) -0.0113(12) -0.0003(11) -0.0137(12) C12 0.0376(14) 0.0473(18) 0.0365(16) -0.0197(14) -0.0073(12) -0.0047(13) C13 0.0518(17) 0.0419(16) 0.0326(14) -0.0139(12) 0.0043(12) -0.0272(14) C20 0.0268(11) 0.0339(13) 0.0293(12) -0.0131(11) 0.0001(10) -0.0158(10) C21 0.0439(15) 0.0414(16) 0.0395(15) -0.0039(13) -0.0131(12) -0.0246(13) C22 0.0494(17) 0.056(2) 0.0429(17) -0.0014(15) -0.0186(14) -0.0260(16) C23 0.0338(14) 0.065(2) 0.0425(17) -0.0207(15) -0.0062(12) -0.0238(14) C24 0.0499(18) 0.061(2) 0.058(2) -0.0212(17) -0.0069(15) -0.0365(16) C25 0.0484(16) 0.0393(16) 0.0486(17) -0.0118(13) -0.0096(13) -0.0250(14) C30 0.0243(11) 0.0291(13) 0.0281(13) -0.0059(10) -0.0037(9) -0.0076(10) C31 0.0306(13) 0.0360(15) 0.0469(16) -0.0175(13) -0.0089(12) -0.0091(11) C32 0.0399(15) 0.0394(16) 0.058(2) -0.0269(15) -0.0127(14) -0.0010(13) C33 0.0302(14) 0.0482(18) 0.0550(19) -0.0200(16) -0.0092(13) 0.0000(13) C34 0.0287(14) 0.0543(19) 0.063(2) -0.0162(16) -0.0092(13) -0.0156(14) C35 0.0334(14) 0.0343(15) 0.0507(17) -0.0128(13) -0.0079(12) -0.0121(12) C40 0.0302(12) 0.0257(12) 0.0298(12) -0.0125(10) -0.0024(10) -0.0123(10) C41 0.0398(14) 0.0306(14) 0.0315(14) -0.0102(11) 0.0017(11) -0.0132(12) C42 0.0411(15) 0.0399(16) 0.0323(14) -0.0170(12) 0.0044(12) -0.0121(13) C43 0.0328(13) 0.0317(14) 0.0417(15) -0.0188(12) -0.0035(11) -0.0098(11) C44 0.0380(14) 0.0241(12) 0.0375(14) -0.0082(11) -0.0061(11) -0.0147(11) C45 0.0329(13) 0.0291(13) 0.0321(13) -0.0120(11) 0.0012(10) -0.0156(11) C50 0.0347(13) 0.0298(13) 0.0265(12) -0.0111(10) -0.0014(10) -0.0153(11) C51 0.0378(14) 0.0304(14) 0.0404(15) -0.0131(12) 0.0049(12) -0.0132(12) C52 0.0446(16) 0.0411(17) 0.0419(17) -0.0188(14) 0.0106(13) -0.0124(14) C53 0.062(2) 0.0428(18) 0.053(2) -0.0302(16) 0.0026(16) -0.0135(16) C54 0.070(2) 0.046(2) 0.091(3) -0.042(2) 0.018(2) -0.0319(18) C55 0.0548(18) 0.0453(18) 0.063(2) -0.0313(16) 0.0161(16) -0.0317(16) C70 0.0283(12) 0.0332(14) 0.0320(13) -0.0100(11) -0.0028(10) -0.0152(11) C71 0.0489(17) 0.098(3) 0.0311(15) -0.0210(17) 0.0047(13) -0.0499(19) C72 0.061(2) 0.121(3) 0.0398(18) -0.020(2) -0.0046(15) -0.064(2) C73 0.0384(15) 0.082(2) 0.0421(17) -0.0153(16) 0.0015(13) -0.0386(17) C74 0.0387(15) 0.078(2) 0.0361(16) -0.0208(16) 0.0082(12) -0.0357(16) C75 0.0360(14) 0.0593(19) 0.0322(14) -0.0182(13) -0.0013(11) -0.0268(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C13 1.894(3) . ? Ru1 C8 1.940(3) . ? Ru1 C7 1.952(3) . ? Ru1 C4 2.050(3) . ? Ru1 P1 2.3704(6) . ? Ru1 Ru2 3.0594(3) . ? Ru2 C10 1.868(3) . ? Ru2 C9 1.905(2) . ? Ru2 C1 2.047(2) . ? Ru2 P1 2.3283(6) . ? Ru2 P2 2.3422(6) . ? Ru2 Ru3 2.9716(3) . ? Ru3 C12 1.860(3) . ? Ru3 C11 1.860(3) . ? Ru3 C4 2.279(2) . ? Ru3 C1 2.321(2) . ? Ru3 P2 2.3235(7) . ? Ru3 C5 2.426(3) . ? P1 C40 1.825(2) . ? P1 C20 1.832(2) . ? P2 C50 1.816(2) . ? P2 C70 1.827(2) . ? O7 C7 1.129(3) . ? O8 C8 1.132(3) . ? O9 C9 1.141(3) . ? O10 C10 1.142(3) . ? O11 C11 1.139(3) . ? O12 C12 1.144(3) . ? O13 C13 1.130(3) . ? C1 C2 1.218(3) . ? C2 C30 1.441(3) . ? C4 C5 1.230(4) . ? C5 C6 1.500(8) . ? C5 C6A 1.503(17) . ? C6 C62 1.529(8) . ? C6 C61 1.529(9) . ? C6 C63 1.568(9) . ? C6A C61A 1.495(17) . ? C6A C62A 1.509(17) . ? C6A C63A 1.516(16) . ? C20 C25 1.387(3) . ? C20 C21 1.392(4) . ? C21 C22 1.387(4) . ? C22 C23 1.380(4) . ? C23 C24 1.371(4) . ? C24 C25 1.385(4) . ? C30 C31 1.389(4) . ? C30 C35 1.396(3) . ? C31 C32 1.378(4) . ? C32 C33 1.378(4) . ? C33 C34 1.382(4) . ? C34 C35 1.382(4) . ? C40 C45 1.388(3) . ? C40 C41 1.391(3) . ? C41 C42 1.391(4) . ? C42 C43 1.383(4) . ? C43 C44 1.375(4) . ? C44 C45 1.399(3) . ? C50 C55 1.391(4) . ? C50 C51 1.398(4) . ? C51 C52 1.388(4) . ? C52 C53 1.376(4) . ? C53 C54 1.362(5) . ? C54 C55 1.381(4) . ? C70 C75 1.377(4) . ? C70 C71 1.395(4) . ? C71 C72 1.383(4) . ? C72 C73 1.379(4) . ? C73 C74 1.362(4) . ? C74 C75 1.387(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Ru1 C8 92.34(12) . . ? C13 Ru1 C7 96.92(11) . . ? C8 Ru1 C7 88.58(12) . . ? C13 Ru1 C4 95.47(12) . . ? C8 Ru1 C4 171.62(10) . . ? C7 Ru1 C4 87.48(11) . . ? C13 Ru1 P1 93.23(8) . . ? C8 Ru1 P1 88.89(8) . . ? C7 Ru1 P1 169.63(8) . . ? C4 Ru1 P1 93.68(7) . . ? C13 Ru1 Ru2 141.91(8) . . ? C8 Ru1 Ru2 85.21(7) . . ? C7 Ru1 Ru2 120.95(8) . . ? C4 Ru1 Ru2 90.48(7) . . ? P1 Ru1 Ru2 48.780(15) . . ? C10 Ru2 C9 89.80(11) . . ? C10 Ru2 C1 92.46(10) . . ? C9 Ru2 C1 173.29(10) . . ? C10 Ru2 P1 102.79(8) . . ? C9 Ru2 P1 99.70(7) . . ? C1 Ru2 P1 85.97(7) . . ? C10 Ru2 P2 107.03(7) . . ? C9 Ru2 P2 94.95(8) . . ? C1 Ru2 P2 78.34(7) . . ? P1 Ru2 P2 146.70(2) . . ? C10 Ru2 Ru3 136.82(7) . . ? C9 Ru2 Ru3 123.97(8) . . ? C1 Ru2 Ru3 51.14(6) . . ? P1 Ru2 Ru3 97.370(17) . . ? P2 Ru2 Ru3 50.161(16) . . ? C10 Ru2 Ru1 151.90(7) . . ? C9 Ru2 Ru1 88.79(7) . . ? C1 Ru2 Ru1 92.18(7) . . ? P1 Ru2 Ru1 49.975(16) . . ? P2 Ru2 Ru1 101.057(17) . . ? Ru3 Ru2 Ru1 63.755(7) . . ? C12 Ru3 C11 86.06(12) . . ? C12 Ru3 C4 126.60(12) . . ? C11 Ru3 C4 95.57(10) . . ? C12 Ru3 C1 101.64(10) . . ? C11 Ru3 C1 167.74(10) . . ? C4 Ru3 C1 87.52(8) . . ? C12 Ru3 P2 96.25(10) . . ? C11 Ru3 P2 96.27(8) . . ? C4 Ru3 P2 136.16(7) . . ? C1 Ru3 P2 73.59(6) . . ? C12 Ru3 C5 96.53(12) . . ? C11 Ru3 C5 93.41(10) . . ? C4 Ru3 C5 30.09(9) . . ? C1 Ru3 C5 95.15(9) . . ? P2 Ru3 C5 164.46(7) . . ? C12 Ru3 Ru2 132.96(10) . . ? C11 Ru3 Ru2 124.70(8) . . ? C4 Ru3 Ru2 88.49(7) . . ? C1 Ru3 Ru2 43.37(6) . . ? P2 Ru3 Ru2 50.717(15) . . ? C5 Ru3 Ru2 113.75(7) . . ? C40 P1 C20 101.26(11) . . ? C40 P1 Ru2 119.83(8) . . ? C20 P1 Ru2 121.28(8) . . ? C40 P1 Ru1 118.43(8) . . ? C20 P1 Ru1 115.37(8) . . ? Ru2 P1 Ru1 81.24(2) . . ? C50 P2 C70 103.74(11) . . ? C50 P2 Ru3 119.15(8) . . ? C70 P2 Ru3 113.91(8) . . ? C50 P2 Ru2 120.10(8) . . ? C70 P2 Ru2 120.29(8) . . ? Ru3 P2 Ru2 79.12(2) . . ? C2 C1 Ru2 173.2(2) . . ? C2 C1 Ru3 92.96(17) . . ? Ru2 C1 Ru3 85.49(8) . . ? C1 C2 C30 170.0(3) . . ? C5 C4 Ru1 170.7(2) . . ? C5 C4 Ru3 81.61(18) . . ? Ru1 C4 Ru3 94.65(10) . . ? C4 C5 C6 159.7(4) . . ? C4 C5 C6A 147.4(7) . . ? C6 C5 C6A 12.6(9) . . ? C4 C5 Ru3 68.30(17) . . ? C6 C5 Ru3 131.3(3) . . ? C6A C5 Ru3 143.8(7) . . ? C5 C6 C62 117.6(5) . . ? C5 C6 C61 107.4(7) . . ? C62 C6 C61 108.6(6) . . ? C5 C6 C63 105.2(5) . . ? C62 C6 C63 106.6(6) . . ? C61 C6 C63 111.5(7) . . ? C61A C6A C5 106.3(13) . . ? C61A C6A C62A 110.7(15) . . ? C5 C6A C62A 106.2(14) . . ? C61A C6A C63A 118.4(15) . . ? C5 C6A C63A 112.2(12) . . ? C62A C6A C63A 102.4(15) . . ? O7 C7 Ru1 174.2(2) . . ? O8 C8 Ru1 175.2(2) . . ? O9 C9 Ru2 175.9(2) . . ? O10 C10 Ru2 179.7(2) . . ? O11 C11 Ru3 175.4(2) . . ? O12 C12 Ru3 177.5(3) . . ? O13 C13 Ru1 178.6(3) . . ? C25 C20 C21 118.6(2) . . ? C25 C20 P1 120.5(2) . . ? C21 C20 P1 120.90(18) . . ? C22 C21 C20 120.2(3) . . ? C23 C22 C21 120.3(3) . . ? C24 C23 C22 119.8(3) . . ? C23 C24 C25 120.3(3) . . ? C24 C25 C20 120.7(3) . . ? C31 C30 C35 119.4(2) . . ? C31 C30 C2 119.5(2) . . ? C35 C30 C2 121.0(2) . . ? C32 C31 C30 120.6(2) . . ? C33 C32 C31 119.7(3) . . ? C32 C33 C34 120.3(3) . . ? C33 C34 C35 120.5(3) . . ? C34 C35 C30 119.5(3) . . ? C45 C40 C41 118.4(2) . . ? C45 C40 P1 122.27(19) . . ? C41 C40 P1 119.36(19) . . ? C42 C41 C40 120.9(2) . . ? C43 C42 C41 120.1(3) . . ? C44 C43 C42 119.9(2) . . ? C43 C44 C45 120.0(2) . . ? C40 C45 C44 120.8(2) . . ? C55 C50 C51 117.4(2) . . ? C55 C50 P2 122.8(2) . . ? C51 C50 P2 119.63(19) . . ? C52 C51 C50 120.8(3) . . ? C53 C52 C51 120.3(3) . . ? C54 C53 C52 119.3(3) . . ? C53 C54 C55 121.2(3) . . ? C54 C55 C50 120.8(3) . . ? C75 C70 C71 118.1(2) . . ? C75 C70 P2 121.66(19) . . ? C71 C70 P2 120.2(2) . . ? C72 C71 C70 120.3(3) . . ? C73 C72 C71 120.7(3) . . ? C74 C73 C72 119.1(3) . . ? C73 C74 C75 120.7(3) . . ? C70 C75 C74 121.0(2) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.633 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.091 #===END data_pjl57 _database_code_CSD 153696 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H34 O7 P2 Ru3' _chemical_formula_weight 1051.87 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.8147(8) _cell_length_b 15.4012(9) _cell_length_c 19.3937(11) _cell_angle_alpha 90.6950(10) _cell_angle_beta 104.5970(10) _cell_angle_gamma 91.5470(10) _cell_volume 4279.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 1.169 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _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 51171 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.1109 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 28.75 _reflns_number_total 22012 _reflns_number_gt 13119 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22012 _refine_ls_number_parameters 1046 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.884 _refine_ls_shift/su_max 0.239 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.30618(2) 0.19577(2) 0.262730(17) 0.02222(8) Uani 1 d . . . Ru2 Ru 0.35469(2) 0.15315(2) 0.131466(17) 0.02247(8) Uani 1 d . . . Ru3 Ru 0.48176(2) 0.14267(2) 0.267956(17) 0.02228(8) Uani 1 d . . . P1 P 0.24061(8) 0.24666(7) 0.14653(6) 0.0242(2) Uani 1 d . . . P2 P 0.48344(8) 0.06675(7) 0.16679(6) 0.0234(2) Uani 1 d . . . O7 O 0.1653(2) 0.0413(2) 0.23471(17) 0.0403(8) Uani 1 d . . . O8 O 0.2055(3) 0.3314(2) 0.32877(19) 0.0523(10) Uani 1 d . . . O9 O 0.2096(2) 0.0052(2) 0.07669(18) 0.0466(9) Uani 1 d . . . O10 O 0.3837(2) 0.2114(2) -0.01026(16) 0.0448(9) Uani 1 d . . . O11 O 0.5289(2) -0.0154(2) 0.35960(17) 0.0407(8) Uani 1 d . . . O12 O 0.6806(2) 0.2103(2) 0.32216(19) 0.0480(9) Uani 1 d . . . O13 O 0.3848(2) 0.1172(2) 0.40957(16) 0.0393(8) Uani 1 d . . . C1 C 0.4454(3) 0.2544(3) 0.1892(2) 0.0234(9) Uani 1 d . . . C2 C 0.4210(3) 0.2782(3) 0.2511(2) 0.0253(9) Uani 1 d . . . C4 C 0.5183(3) 0.2941(3) 0.1624(2) 0.0233(9) Uani 1 d . . . C5 C 0.5770(3) 0.3217(3) 0.1359(2) 0.0271(10) Uani 1 d . . . C6 C 0.6504(3) 0.3537(3) 0.1027(3) 0.0390(12) Uani 1 d . . . C7 C 0.2137(3) 0.1008(3) 0.2473(2) 0.0283(10) Uani 1 d . . . C8 C 0.2438(3) 0.2815(3) 0.3048(2) 0.0315(10) Uani 1 d . . . C9 C 0.2643(3) 0.0602(3) 0.0956(2) 0.0310(10) Uani 1 d . . . C10 C 0.3716(3) 0.1877(3) 0.0418(2) 0.0309(10) Uani 1 d . . . C11 C 0.5084(3) 0.0429(3) 0.3236(2) 0.0281(10) Uani 1 d . . . C12 C 0.6062(3) 0.1827(3) 0.3033(2) 0.0302(10) Uani 1 d . . . C13 C 0.3677(3) 0.1441(3) 0.3529(2) 0.0299(10) Uani 1 d . . . C20 C 0.1170(3) 0.2237(3) 0.1074(2) 0.0293(10) Uani 1 d . . . C21 C 0.0508(3) 0.2210(3) 0.1463(3) 0.0351(11) Uani 1 d . . . H21 H 0.0701 0.2270 0.1968 0.042 Uiso 1 calc R . . C22 C -0.0420(3) 0.2097(3) 0.1135(3) 0.0469(14) Uani 1 d . . . H22 H -0.0861 0.2059 0.1415 0.056 Uiso 1 calc R . . C23 C -0.0717(4) 0.2039(4) 0.0414(3) 0.0596(17) Uani 1 d . . . H23 H -0.1366 0.1999 0.0190 0.072 Uiso 1 calc R . . C24 C -0.0076(4) 0.2040(5) 0.0009(3) 0.074(2) Uani 1 d . . . H24 H -0.0277 0.1974 -0.0494 0.089 Uiso 1 calc R . . C25 C 0.0863(4) 0.2138(4) 0.0341(3) 0.0552(16) Uani 1 d . . . H25 H 0.1306 0.2138 0.0062 0.066 Uiso 1 calc R . . C30 C 0.4588(3) 0.3554(3) 0.2964(2) 0.0242(9) Uani 1 d . . . C31 C 0.4688(3) 0.4352(3) 0.2638(2) 0.0321(11) Uani 1 d . . . H31 H 0.4537 0.4387 0.2134 0.039 Uiso 1 calc R . . C32 C 0.5009(3) 0.5088(3) 0.3059(3) 0.0387(12) Uani 1 d . . . H32 H 0.5069 0.5626 0.2838 0.046 Uiso 1 calc R . . C33 C 0.5242(3) 0.5052(3) 0.3791(3) 0.0405(12) Uani 1 d . . . H33 H 0.5473 0.5557 0.4074 0.049 Uiso 1 calc R . . C34 C 0.5136(4) 0.4273(3) 0.4106(3) 0.0445(13) Uani 1 d . . . H34 H 0.5289 0.4242 0.4611 0.053 Uiso 1 calc R . . C35 C 0.4813(3) 0.3540(3) 0.3701(2) 0.0375(12) Uani 1 d . . . H35 H 0.4742 0.3011 0.3931 0.045 Uiso 1 calc R . . C40 C 0.2477(3) 0.3627(3) 0.1301(2) 0.0284(10) Uani 1 d . . . C41 C 0.1887(4) 0.4183(3) 0.1530(3) 0.0419(13) Uani 1 d . . . H41 H 0.1461 0.3956 0.1780 0.050 Uiso 1 calc R . . C42 C 0.1910(4) 0.5071(3) 0.1399(3) 0.0507(14) Uani 1 d . . . H42 H 0.1506 0.5447 0.1561 0.061 Uiso 1 calc R . . C43 C 0.2525(4) 0.5399(3) 0.1032(3) 0.0485(14) Uani 1 d . . . H43 H 0.2538 0.6001 0.0934 0.058 Uiso 1 calc R . . C44 C 0.3117(4) 0.4860(3) 0.0808(3) 0.0446(13) Uani 1 d . . . H44 H 0.3549 0.5092 0.0565 0.054 Uiso 1 calc R . . C45 C 0.3090(3) 0.3972(3) 0.0935(2) 0.0370(12) Uani 1 d . . . H45 H 0.3496 0.3601 0.0769 0.044 Uiso 1 calc R . . C50 C 0.4650(3) -0.0506(3) 0.1684(2) 0.0256(9) Uani 1 d . . . C51 C 0.3939(3) -0.0828(3) 0.1979(2) 0.0331(11) Uani 1 d . . . H51 H 0.3585 -0.0438 0.2181 0.040 Uiso 1 calc R . . C52 C 0.3751(3) -0.1718(3) 0.1976(3) 0.0407(12) Uani 1 d . . . H52 H 0.3279 -0.1932 0.2188 0.049 Uiso 1 calc R . . C53 C 0.4232(3) -0.2289(3) 0.1672(2) 0.0389(12) Uani 1 d . . . H53 H 0.4090 -0.2895 0.1667 0.047 Uiso 1 calc R . . C54 C 0.4928(3) -0.1980(3) 0.1374(2) 0.0339(11) Uani 1 d . . . H54 H 0.5265 -0.2374 0.1161 0.041 Uiso 1 calc R . . C55 C 0.5135(3) -0.1099(3) 0.1383(2) 0.0249(9) Uani 1 d . . . H55 H 0.5620 -0.0895 0.1180 0.030 Uiso 1 calc R . . C61 C 0.6609(4) 0.4522(3) 0.1106(3) 0.0491(14) Uani 1 d . . . H61C H 0.6783 0.4686 0.1614 0.059 Uiso 1 calc R . . H61B H 0.6016 0.4783 0.0875 0.059 Uiso 1 calc R . . H61A H 0.7096 0.4731 0.0883 0.059 Uiso 1 calc R . . C62 C 0.7434(4) 0.3132(4) 0.1424(4) 0.0713(19) Uani 1 d . . . H62C H 0.7354 0.2498 0.1414 0.086 Uiso 1 calc R . . H62B H 0.7610 0.3345 0.1919 0.086 Uiso 1 calc R . . H62A H 0.7924 0.3296 0.1189 0.086 Uiso 1 calc R . . C63 C 0.6268(5) 0.3248(4) 0.0244(3) 0.0638(18) Uani 1 d . . . H63C H 0.5746 0.3581 -0.0027 0.077 Uiso 1 calc R . . H63B H 0.6092 0.2628 0.0204 0.077 Uiso 1 calc R . . H63A H 0.6813 0.3348 0.0053 0.077 Uiso 1 calc R . . C70 C 0.5858(3) 0.0757(3) 0.1313(2) 0.0231(9) Uani 1 d . . . C71 C 0.5757(3) 0.0785(3) 0.0583(2) 0.0284(10) Uani 1 d . . . H71 H 0.5155 0.0845 0.0272 0.034 Uiso 1 calc R . . C72 C 0.6538(3) 0.0725(3) 0.0305(2) 0.0326(11) Uani 1 d . . . H72 H 0.6464 0.0734 -0.0196 0.039 Uiso 1 calc R . . C73 C 0.7414(3) 0.0653(3) 0.0756(2) 0.0321(11) Uani 1 d . . . H73 H 0.7943 0.0605 0.0566 0.039 Uiso 1 calc R . . C74 C 0.7523(3) 0.0649(3) 0.1479(2) 0.0344(11) Uani 1 d . . . H74 H 0.8129 0.0609 0.1788 0.041 Uiso 1 calc R . . C75 C 0.6751(3) 0.0702(3) 0.1766(2) 0.0262(10) Uani 1 d . . . H75 H 0.6833 0.0701 0.2267 0.031 Uiso 1 calc R . . Ru1A Ru 0.80367(2) 0.76956(2) 0.236192(17) 0.02212(8) Uani 1 d . . . Ru2A Ru 0.93485(2) 0.79835(2) 0.372417(17) 0.02220(8) Uani 1 d . . . Ru3A Ru 0.98191(2) 0.82771(2) 0.242759(17) 0.02267(8) Uani 1 d . . . P1A P 0.80760(8) 0.70187(7) 0.34627(6) 0.0236(2) Uani 1 d . . . P2A P 1.04705(8) 0.89477(7) 0.34961(6) 0.0239(2) Uani 1 d . . . O7A O 0.6885(2) 0.9145(2) 0.27912(16) 0.0379(8) Uani 1 d . . . O8A O 0.7995(2) 0.8609(2) 0.09611(16) 0.0389(8) Uani 1 d . . . O9A O 0.8321(3) 0.9349(2) 0.43828(18) 0.0526(10) Uani 1 d . . . O10A O 1.0525(3) 0.7278(2) 0.50943(16) 0.0483(9) Uani 1 d . . . O11A O 0.9696(2) 0.9941(2) 0.15998(17) 0.0440(9) Uani 1 d . . . O12A O 1.1431(2) 0.7725(3) 0.18541(18) 0.0531(10) Uani 1 d . . . O13A O 0.6545(3) 0.6431(2) 0.1507(2) 0.0567(11) Uani 1 d . . . C1A C 0.9855(3) 0.7055(3) 0.3095(2) 0.0240(9) Uani 1 d . . . C2A C 0.9223(3) 0.6895(3) 0.2441(2) 0.0246(9) Uani 1 d . . . C4A C 1.0712(3) 0.6618(3) 0.3361(2) 0.0275(10) Uani 1 d . . . C5A C 1.1434(3) 0.6294(3) 0.3638(2) 0.0346(11) Uani 1 d D . . C6A C 1.2283(10) 0.5940(11) 0.4103(7) 0.035(2) Uani 0.439(8) d PD A 1 C61A C 1.2775(10) 0.6568(9) 0.4692(9) 0.078(4) Uani 0.439(8) d PD A 1 H61D H 1.2918 0.7116 0.4485 0.117 Uiso 0.439(8) calc PR A 1 H61E H 1.3356 0.6318 0.4963 0.117 Uiso 0.439(8) calc PR A 1 H61F H 1.2371 0.6678 0.5011 0.117 Uiso 0.439(8) calc PR A 1 C62A C 1.203(2) 0.5083(18) 0.4420(18) 0.057(5) Uani 0.439(8) d PD A 1 H62D H 1.1688 0.5207 0.4778 0.086 Uiso 0.439(8) calc PR A 1 H62E H 1.2604 0.4784 0.4643 0.086 Uiso 0.439(8) calc PR A 1 H62F H 1.1642 0.4712 0.4039 0.086 Uiso 0.439(8) calc PR A 1 C63A C 1.2906(12) 0.5746(14) 0.3592(8) 0.082(4) Uani 0.439(8) d PD A 1 H63D H 1.2574 0.5338 0.3216 0.122 Uiso 0.439(8) calc PR A 1 H63E H 1.3486 0.5490 0.3859 0.122 Uiso 0.439(8) calc PR A 1 H63F H 1.3053 0.6287 0.3377 0.122 Uiso 0.439(8) calc PR A 1 C6B C 1.2345(8) 0.5862(8) 0.3851(6) 0.035(2) Uani 0.561(8) d PD A 2 C61B C 1.3112(7) 0.6538(7) 0.4162(8) 0.078(4) Uani 0.561(8) d PD A 2 H61G H 1.3180 0.6940 0.3789 0.117 Uiso 0.561(8) calc PR A 2 H61H H 1.3702 0.6247 0.4348 0.117 Uiso 0.561(8) calc PR A 2 H61I H 1.2948 0.6862 0.4549 0.117 Uiso 0.561(8) calc PR A 2 C62B C 1.2308(17) 0.5190(14) 0.4417(13) 0.057(5) Uani 0.561(8) d PD A 2 H62G H 1.2198 0.5482 0.4839 0.086 Uiso 0.561(8) calc PR A 2 H62H H 1.2903 0.4893 0.4550 0.086 Uiso 0.561(8) calc PR A 2 H62I H 1.1801 0.4764 0.4227 0.086 Uiso 0.561(8) calc PR A 2 C63B C 1.2553(9) 0.5385(11) 0.3210(7) 0.082(4) Uani 0.561(8) d PD A 2 H63G H 1.1987 0.5072 0.2939 0.122 Uiso 0.561(8) calc PR A 2 H63H H 1.3048 0.4971 0.3380 0.122 Uiso 0.561(8) calc PR A 2 H63I H 1.2757 0.5807 0.2902 0.122 Uiso 0.561(8) calc PR A 2 C7A C 0.7263(3) 0.8597(3) 0.2607(2) 0.0271(10) Uani 1 d . . . C8A C 0.8132(3) 0.8298(3) 0.1507(2) 0.0283(10) Uani 1 d . . . C9A C 0.8708(3) 0.8850(3) 0.4147(2) 0.0298(10) Uani 1 d . . . C10A C 1.0077(3) 0.7557(3) 0.4592(2) 0.0316(11) Uani 1 d . . . C11A C 0.9744(3) 0.9327(3) 0.1929(2) 0.0301(10) Uani 1 d . . . C12A C 1.0831(3) 0.7957(3) 0.2075(2) 0.0343(11) Uani 1 d . . . C13A C 0.7103(3) 0.6891(3) 0.1824(2) 0.0328(11) Uani 1 d . . . C20A C 0.7080(3) 0.7162(3) 0.3851(2) 0.0246(9) Uani 1 d . . . C21A C 0.7221(3) 0.7035(3) 0.4581(2) 0.0326(11) Uani 1 d . . . H21A H 0.7815 0.6875 0.4858 0.039 Uiso 1 calc R . . C22A C 0.6491(3) 0.7142(3) 0.4900(2) 0.0402(12) Uani 1 d . . . H22A H 0.6592 0.7061 0.5398 0.048 Uiso 1 calc R . . C23A C 0.5626(3) 0.7365(3) 0.4505(3) 0.0380(12) Uani 1 d . . . H23A H 0.5131 0.7437 0.4729 0.046 Uiso 1 calc R . . C24A C 0.5476(3) 0.7481(3) 0.3785(2) 0.0337(11) Uani 1 d . . . H24A H 0.4878 0.7640 0.3514 0.040 Uiso 1 calc R . . C25A C 0.6197(3) 0.7367(3) 0.3449(2) 0.0303(10) Uani 1 d . . . H25A H 0.6083 0.7429 0.2948 0.036 Uiso 1 calc R . . C30A C 0.9289(3) 0.6180(3) 0.1926(2) 0.0278(10) Uani 1 d . . . C31A C 0.9087(3) 0.6320(3) 0.1196(2) 0.0375(12) Uani 1 d . . . H31A H 0.8917 0.6881 0.1020 0.045 Uiso 1 calc R . . C32A C 0.9132(3) 0.5651(4) 0.0724(3) 0.0443(13) Uani 1 d . . . H32A H 0.9008 0.5758 0.0228 0.053 Uiso 1 calc R . . C33A C 0.9355(3) 0.4828(3) 0.0972(3) 0.0427(13) Uani 1 d . . . H33A H 0.9386 0.4367 0.0649 0.051 Uiso 1 calc R . . C34A C 0.9532(3) 0.4682(3) 0.1685(3) 0.0412(12) Uani 1 d . . . H34A H 0.9677 0.4114 0.1856 0.049 Uiso 1 calc R . . C35A C 0.9504(3) 0.5349(3) 0.2165(2) 0.0310(10) Uani 1 d . . . H35A H 0.9633 0.5235 0.2660 0.037 Uiso 1 calc R . . C40A C 0.8205(3) 0.5839(3) 0.3535(2) 0.0243(9) Uani 1 d . . . C41A C 0.7453(3) 0.5298(3) 0.3219(2) 0.0346(11) Uani 1 d . . . H41A H 0.6896 0.5543 0.2949 0.042 Uiso 1 calc R . . C42A C 0.7495(4) 0.4406(3) 0.3288(3) 0.0411(12) Uani 1 d . . . H42A H 0.6967 0.4043 0.3075 0.049 Uiso 1 calc R . . C43A C 0.8313(4) 0.4045(3) 0.3670(2) 0.0396(12) Uani 1 d . . . H43A H 0.8354 0.3433 0.3715 0.047 Uiso 1 calc R . . C44A C 0.9071(3) 0.4587(3) 0.3984(2) 0.0377(12) Uani 1 d . . . H44A H 0.9634 0.4345 0.4248 0.045 Uiso 1 calc R . . C45A C 0.9013(3) 0.5470(3) 0.3917(2) 0.0296(10) Uani 1 d . . . H45A H 0.9537 0.5834 0.4137 0.035 Uiso 1 calc R . . C50A C 1.0316(3) 1.0117(3) 0.3534(2) 0.0268(10) Uani 1 d . . . C51A C 0.9435(3) 1.0444(3) 0.3253(2) 0.0369(11) Uani 1 d . . . H51A H 0.8925 1.0054 0.3057 0.044 Uiso 1 calc R . . C52A C 0.9290(4) 1.1331(3) 0.3255(3) 0.0441(13) Uani 1 d . . . H52A H 0.8684 1.1541 0.3058 0.053 Uiso 1 calc R . . C53A C 1.0015(4) 1.1906(3) 0.3540(3) 0.0470(14) Uani 1 d . . . H53A H 0.9916 1.2513 0.3532 0.056 Uiso 1 calc R . . C54A C 1.0882(4) 1.1596(3) 0.3835(3) 0.0423(13) Uani 1 d . . . H54A H 1.1381 1.1994 0.4042 0.051 Uiso 1 calc R . . C55A C 1.1050(3) 1.0705(3) 0.3839(2) 0.0354(11) Uani 1 d . . . H55A H 1.1656 1.0501 0.4047 0.043 Uiso 1 calc R . . C70A C 1.1705(3) 0.8868(3) 0.3943(2) 0.0282(10) Uani 1 d . . . C71A C 1.1985(3) 0.8915(3) 0.4677(2) 0.0391(12) Uani 1 d . . . H71A H 1.1533 0.8913 0.4948 0.047 Uiso 1 calc R . . C72A C 1.2931(4) 0.8965(4) 0.5020(3) 0.0498(14) Uani 1 d . . . H72A H 1.3120 0.9002 0.5525 0.060 Uiso 1 calc R . . C73A C 1.3586(4) 0.8961(3) 0.4643(3) 0.0458(13) Uani 1 d . . . H73A H 1.4229 0.8999 0.4885 0.055 Uiso 1 calc R . . C74A C 1.3324(3) 0.8903(3) 0.3908(3) 0.0412(12) Uani 1 d . . . H74A H 1.3787 0.8895 0.3647 0.049 Uiso 1 calc R . . C75A C 1.2389(3) 0.8855(3) 0.3551(2) 0.0323(11) Uani 1 d . . . H75A H 1.2208 0.8814 0.3045 0.039 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02146(19) 0.02336(19) 0.02312(17) -0.00008(14) 0.00822(14) -0.00113(15) Ru2 0.01843(18) 0.0281(2) 0.02124(17) -0.00146(14) 0.00578(13) 0.00031(15) Ru3 0.02053(19) 0.02418(19) 0.02176(17) 0.00017(13) 0.00474(13) -0.00024(15) P1 0.0197(6) 0.0281(6) 0.0258(6) 0.0025(5) 0.0073(4) -0.0001(5) P2 0.0204(6) 0.0260(6) 0.0243(6) -0.0015(4) 0.0069(4) -0.0006(5) O7 0.041(2) 0.036(2) 0.043(2) -0.0004(16) 0.0100(16) -0.0131(17) O8 0.065(3) 0.039(2) 0.061(2) -0.0071(18) 0.030(2) 0.0132(19) O9 0.034(2) 0.053(2) 0.051(2) -0.0185(18) 0.0118(17) -0.0129(18) O10 0.041(2) 0.067(3) 0.0278(18) 0.0053(17) 0.0110(16) 0.0008(18) O11 0.040(2) 0.039(2) 0.0411(19) 0.0147(16) 0.0068(16) 0.0039(17) O12 0.027(2) 0.048(2) 0.063(2) -0.0023(18) 0.0009(17) -0.0096(18) O13 0.050(2) 0.045(2) 0.0261(17) 0.0068(15) 0.0143(15) 0.0070(17) C1 0.020(2) 0.024(2) 0.026(2) 0.0048(17) 0.0050(17) 0.0022(18) C2 0.020(2) 0.023(2) 0.032(2) 0.0016(18) 0.0035(18) -0.0037(18) C4 0.020(2) 0.025(2) 0.023(2) 0.0009(17) 0.0014(17) 0.0011(19) C5 0.032(3) 0.022(2) 0.030(2) 0.0020(18) 0.012(2) -0.001(2) C6 0.042(3) 0.034(3) 0.049(3) 0.000(2) 0.027(2) -0.009(2) C7 0.025(3) 0.033(3) 0.026(2) 0.0021(19) 0.0064(18) 0.000(2) C8 0.034(3) 0.030(3) 0.032(2) 0.002(2) 0.011(2) -0.001(2) C9 0.026(3) 0.038(3) 0.031(2) -0.005(2) 0.011(2) 0.002(2) C10 0.018(2) 0.045(3) 0.028(2) -0.003(2) 0.0018(18) 0.001(2) C11 0.021(2) 0.033(3) 0.031(2) -0.003(2) 0.0100(19) -0.001(2) C12 0.034(3) 0.027(3) 0.027(2) -0.0008(19) 0.004(2) 0.004(2) C13 0.030(3) 0.031(3) 0.030(2) -0.005(2) 0.0107(19) -0.003(2) C20 0.021(2) 0.029(3) 0.036(2) 0.006(2) 0.0032(19) 0.001(2) C21 0.022(3) 0.039(3) 0.048(3) -0.004(2) 0.016(2) -0.002(2) C22 0.025(3) 0.052(4) 0.064(4) 0.008(3) 0.012(3) -0.001(3) C23 0.025(3) 0.069(4) 0.079(4) 0.027(3) 0.000(3) -0.006(3) C24 0.046(4) 0.120(6) 0.042(3) 0.025(4) -0.013(3) -0.019(4) C25 0.032(3) 0.098(5) 0.034(3) 0.012(3) 0.005(2) -0.010(3) C30 0.016(2) 0.026(2) 0.030(2) -0.0049(18) 0.0069(17) -0.0012(18) C31 0.033(3) 0.029(3) 0.037(3) 0.000(2) 0.013(2) -0.001(2) C32 0.037(3) 0.023(3) 0.060(3) 0.000(2) 0.018(2) -0.002(2) C33 0.031(3) 0.037(3) 0.051(3) -0.015(2) 0.006(2) -0.004(2) C34 0.049(3) 0.042(3) 0.038(3) -0.012(2) 0.003(2) -0.008(3) C35 0.050(3) 0.031(3) 0.032(3) 0.001(2) 0.011(2) -0.002(2) C40 0.027(3) 0.025(2) 0.032(2) 0.0049(19) 0.0058(19) 0.001(2) C41 0.043(3) 0.032(3) 0.057(3) 0.005(2) 0.026(3) 0.000(2) C42 0.059(4) 0.025(3) 0.072(4) 0.006(3) 0.024(3) 0.004(3) C43 0.052(4) 0.036(3) 0.054(3) 0.015(3) 0.008(3) -0.005(3) C44 0.041(3) 0.049(3) 0.045(3) 0.018(3) 0.013(2) -0.004(3) C45 0.029(3) 0.043(3) 0.040(3) 0.015(2) 0.009(2) 0.005(2) C50 0.020(2) 0.029(2) 0.026(2) -0.0019(18) 0.0025(17) -0.0016(19) C51 0.031(3) 0.035(3) 0.034(3) -0.003(2) 0.011(2) -0.001(2) C52 0.036(3) 0.042(3) 0.044(3) -0.002(2) 0.013(2) -0.009(2) C53 0.038(3) 0.027(3) 0.046(3) 0.000(2) 0.000(2) 0.000(2) C54 0.032(3) 0.031(3) 0.037(3) -0.002(2) 0.004(2) 0.008(2) C55 0.025(2) 0.026(2) 0.024(2) -0.0007(18) 0.0071(18) 0.0018(19) C61 0.062(4) 0.033(3) 0.065(4) -0.003(3) 0.039(3) -0.007(3) C62 0.048(4) 0.057(4) 0.122(6) 0.007(4) 0.044(4) 0.003(3) C63 0.104(5) 0.047(4) 0.058(4) -0.010(3) 0.057(4) -0.021(3) C70 0.023(2) 0.019(2) 0.029(2) 0.0004(17) 0.0112(18) 0.0012(18) C71 0.022(2) 0.033(3) 0.030(2) -0.0031(19) 0.0063(18) 0.000(2) C72 0.035(3) 0.037(3) 0.028(2) 0.004(2) 0.012(2) 0.003(2) C73 0.022(2) 0.036(3) 0.041(3) -0.002(2) 0.014(2) 0.001(2) C74 0.021(2) 0.040(3) 0.040(3) 0.005(2) 0.003(2) 0.007(2) C75 0.025(2) 0.027(2) 0.025(2) 0.0024(18) 0.0044(18) 0.0049(19) Ru1A 0.01960(19) 0.02207(18) 0.02369(17) 0.00129(13) 0.00348(13) 0.00138(14) Ru2A 0.02149(19) 0.02368(19) 0.02127(17) 0.00100(13) 0.00501(14) 0.00140(15) Ru3A 0.02058(19) 0.02557(19) 0.02148(17) 0.00100(14) 0.00470(13) -0.00047(15) P1A 0.0204(6) 0.0239(6) 0.0271(6) 0.0027(4) 0.0067(4) 0.0022(5) P2A 0.0222(6) 0.0255(6) 0.0233(5) 0.0004(4) 0.0047(4) 0.0000(5) O7A 0.037(2) 0.037(2) 0.0415(19) 0.0070(15) 0.0122(15) 0.0127(16) O8A 0.039(2) 0.045(2) 0.0298(18) 0.0101(15) 0.0032(15) -0.0027(16) O9A 0.061(3) 0.054(2) 0.046(2) -0.0101(18) 0.0179(19) 0.019(2) O10A 0.060(3) 0.051(2) 0.0282(18) 0.0097(16) 0.0008(17) 0.0089(19) O11A 0.038(2) 0.043(2) 0.045(2) 0.0210(17) 0.0014(16) -0.0052(17) O12A 0.036(2) 0.080(3) 0.047(2) -0.012(2) 0.0203(18) 0.002(2) O13A 0.039(2) 0.034(2) 0.082(3) -0.0140(19) -0.0120(19) -0.0042(18) C1A 0.021(2) 0.024(2) 0.028(2) 0.0043(18) 0.0088(18) 0.0011(18) C2A 0.021(2) 0.024(2) 0.029(2) 0.0014(18) 0.0072(18) 0.0022(19) C4A 0.025(3) 0.027(2) 0.030(2) 0.0001(19) 0.0052(19) 0.000(2) C5A 0.029(3) 0.031(3) 0.041(3) -0.001(2) 0.004(2) 0.001(2) C6A 0.023(3) 0.049(4) 0.038(7) 0.004(5) 0.014(5) 0.017(3) C61A 0.024(6) 0.049(5) 0.142(12) 0.011(7) -0.016(5) 0.001(4) C62A 0.048(14) 0.047(6) 0.067(4) 0.009(4) -0.006(7) 0.013(7) C63A 0.060(8) 0.128(13) 0.059(8) 0.008(7) 0.016(6) 0.046(8) C6B 0.023(3) 0.049(4) 0.038(7) 0.004(5) 0.014(5) 0.017(3) C61B 0.024(6) 0.049(5) 0.142(12) 0.011(7) -0.016(5) 0.001(4) C62B 0.048(14) 0.047(6) 0.067(4) 0.009(4) -0.006(7) 0.013(7) C63B 0.060(8) 0.128(13) 0.059(8) 0.008(7) 0.016(6) 0.046(8) C7A 0.026(3) 0.026(3) 0.028(2) 0.0091(19) 0.0031(19) 0.005(2) C8A 0.025(3) 0.027(3) 0.031(2) 0.0000(19) 0.0042(19) 0.001(2) C9A 0.038(3) 0.029(3) 0.021(2) -0.0030(18) 0.0054(19) 0.002(2) C10A 0.035(3) 0.033(3) 0.027(2) -0.004(2) 0.008(2) -0.005(2) C11A 0.018(2) 0.040(3) 0.032(2) 0.003(2) 0.0065(18) -0.003(2) C12A 0.029(3) 0.043(3) 0.032(3) -0.004(2) 0.011(2) -0.004(2) C13A 0.028(3) 0.024(3) 0.043(3) 0.004(2) 0.002(2) 0.007(2) C20A 0.020(2) 0.021(2) 0.035(2) -0.0037(18) 0.0101(18) -0.0020(18) C21A 0.025(3) 0.037(3) 0.035(3) 0.002(2) 0.008(2) 0.002(2) C22A 0.041(3) 0.049(3) 0.032(3) -0.009(2) 0.014(2) -0.004(3) C23A 0.035(3) 0.037(3) 0.049(3) -0.006(2) 0.024(2) 0.000(2) C24A 0.023(3) 0.039(3) 0.041(3) 0.000(2) 0.011(2) 0.007(2) C25A 0.028(3) 0.034(3) 0.030(2) 0.006(2) 0.0100(19) 0.002(2) C30A 0.017(2) 0.027(3) 0.038(3) -0.0070(19) 0.0061(19) -0.0018(19) C31A 0.040(3) 0.037(3) 0.033(3) -0.002(2) 0.005(2) 0.003(2) C32A 0.043(3) 0.060(4) 0.030(3) -0.013(2) 0.010(2) 0.002(3) C33A 0.037(3) 0.038(3) 0.055(3) -0.020(3) 0.018(2) -0.004(2) C34A 0.039(3) 0.027(3) 0.063(3) -0.005(2) 0.021(3) 0.001(2) C35A 0.023(2) 0.033(3) 0.038(3) -0.001(2) 0.010(2) 0.000(2) C40A 0.026(2) 0.022(2) 0.027(2) 0.0026(17) 0.0096(18) 0.0010(19) C41A 0.027(3) 0.027(3) 0.046(3) 0.003(2) 0.003(2) 0.006(2) C42A 0.038(3) 0.024(3) 0.056(3) 0.003(2) 0.004(2) -0.011(2) C43A 0.052(3) 0.022(3) 0.045(3) 0.009(2) 0.012(2) 0.005(2) C44A 0.037(3) 0.034(3) 0.042(3) 0.011(2) 0.008(2) 0.010(2) C45A 0.027(3) 0.029(3) 0.033(2) 0.0014(19) 0.0087(19) -0.001(2) C50A 0.032(3) 0.026(2) 0.024(2) -0.0010(18) 0.0096(19) 0.000(2) C51A 0.037(3) 0.030(3) 0.043(3) 0.003(2) 0.008(2) 0.001(2) C52A 0.047(3) 0.035(3) 0.052(3) 0.008(2) 0.014(3) 0.012(3) C53A 0.075(4) 0.025(3) 0.044(3) 0.002(2) 0.022(3) 0.007(3) C54A 0.065(4) 0.024(3) 0.042(3) -0.009(2) 0.022(3) -0.014(3) C55A 0.042(3) 0.037(3) 0.029(2) -0.008(2) 0.014(2) -0.009(2) C70A 0.026(3) 0.025(2) 0.031(2) 0.0015(18) 0.0032(19) -0.002(2) C71A 0.037(3) 0.045(3) 0.030(3) -0.001(2) 0.000(2) -0.004(2) C72A 0.040(3) 0.060(4) 0.039(3) 0.004(3) -0.010(2) -0.003(3) C73A 0.023(3) 0.039(3) 0.064(4) 0.005(3) -0.010(2) -0.005(2) C74A 0.021(3) 0.042(3) 0.059(3) 0.003(2) 0.007(2) -0.001(2) C75A 0.030(3) 0.034(3) 0.034(2) -0.002(2) 0.009(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C8 1.919(5) . ? Ru1 C7 1.945(5) . ? Ru1 C13 1.947(5) . ? Ru1 C2 2.154(4) . ? Ru1 P1 2.3701(11) . ? Ru1 Ru3 2.7256(5) . ? Ru1 Ru2 2.8870(5) . ? Ru2 C10 1.898(5) . ? Ru2 C9 1.931(5) . ? Ru2 C1 2.139(4) . ? Ru2 P2 2.3191(11) . ? Ru2 P1 2.3208(12) . ? Ru2 Ru3 2.8446(5) . ? Ru3 C12 1.881(5) . ? Ru3 C11 1.881(5) . ? Ru3 P2 2.2777(11) . ? Ru3 C2 2.291(4) . ? Ru3 C1 2.298(4) . ? P1 C20 1.820(4) . ? P1 C40 1.825(4) . ? P2 C70 1.820(4) . ? P2 C50 1.823(4) . ? O7 C7 1.133(5) . ? O8 C8 1.130(5) . ? O9 C9 1.146(5) . ? O10 C10 1.133(5) . ? O11 C11 1.144(5) . ? O12 C12 1.140(5) . ? O13 C13 1.149(5) . ? C1 C2 1.386(6) . ? C1 C4 1.439(5) . ? C2 C30 1.479(6) . ? C4 C5 1.188(5) . ? C5 C6 1.474(6) . ? C6 C61 1.522(6) . ? C6 C63 1.528(7) . ? C6 C62 1.550(7) . ? C20 C21 1.381(6) . ? C20 C25 1.383(6) . ? C21 C22 1.367(6) . ? C22 C23 1.357(7) . ? C23 C24 1.377(8) . ? C24 C25 1.381(7) . ? C30 C35 1.384(6) . ? C30 C31 1.411(6) . ? C31 C32 1.389(6) . ? C32 C33 1.375(6) . ? C33 C34 1.377(7) . ? C34 C35 1.372(6) . ? C40 C45 1.385(6) . ? C40 C41 1.386(6) . ? C41 C42 1.395(6) . ? C42 C43 1.380(7) . ? C43 C44 1.367(7) . ? C44 C45 1.393(6) . ? C50 C55 1.386(5) . ? C50 C51 1.402(6) . ? C51 C52 1.392(6) . ? C52 C53 1.364(7) . ? C53 C54 1.381(6) . ? C54 C55 1.382(6) . ? C70 C71 1.386(5) . ? C70 C75 1.397(6) . ? C71 C72 1.400(6) . ? C72 C73 1.378(6) . ? C73 C74 1.370(6) . ? C74 C75 1.395(6) . ? Ru1A C13A 1.919(5) . ? Ru1A C8A 1.943(4) . ? Ru1A C7A 1.952(5) . ? Ru1A C2A 2.149(4) . ? Ru1A P1A 2.3754(11) . ? Ru1A Ru3A 2.7370(5) . ? Ru1A Ru2A 2.8793(5) . ? Ru2A C10A 1.891(5) . ? Ru2A C9A 1.946(5) . ? Ru2A C1A 2.138(4) . ? Ru2A P1A 2.3169(12) . ? Ru2A P2A 2.3274(12) . ? Ru2A Ru3A 2.8121(5) . ? Ru3A C12A 1.872(5) . ? Ru3A C11A 1.885(5) . ? Ru3A P2A 2.2755(11) . ? Ru3A C2A 2.285(4) . ? Ru3A C1A 2.292(4) . ? P1A C20A 1.835(4) . ? P1A C40A 1.835(4) . ? P2A C70A 1.823(4) . ? P2A C50A 1.824(4) . ? O7A C7A 1.129(5) . ? O8A C8A 1.141(5) . ? O9A C9A 1.129(5) . ? O10A C10A 1.129(5) . ? O11A C11A 1.141(5) . ? O12A C12A 1.144(5) . ? O13A C13A 1.125(5) . ? C1A C2A 1.388(6) . ? C1A C4A 1.435(6) . ? C2A C30A 1.500(6) . ? C4A C5A 1.194(6) . ? C5A C6A 1.473(14) . ? C5A C6B 1.487(11) . ? C6A C61A 1.513(15) . ? C6A C62A 1.538(16) . ? C6A C63A 1.548(13) . ? C6B C61B 1.520(13) . ? C6B C62B 1.529(13) . ? C6B C63B 1.537(12) . ? C20A C25A 1.391(6) . ? C20A C21A 1.394(6) . ? C21A C22A 1.387(6) . ? C22A C23A 1.373(7) . ? C23A C24A 1.371(6) . ? C24A C25A 1.398(6) . ? C30A C35A 1.384(6) . ? C30A C31A 1.392(6) . ? C31A C32A 1.385(6) . ? C32A C33A 1.380(7) . ? C33A C34A 1.365(7) . ? C34A C35A 1.386(6) . ? C40A C41A 1.379(6) . ? C40A C45A 1.380(6) . ? C41A C42A 1.384(6) . ? C42A C43A 1.385(7) . ? C43A C44A 1.387(7) . ? C44A C45A 1.371(6) . ? C50A C51A 1.391(6) . ? C50A C55A 1.401(6) . ? C51A C52A 1.389(6) . ? C52A C53A 1.371(7) . ? C53A C54A 1.369(7) . ? C54A C55A 1.402(6) . ? C70A C71A 1.380(6) . ? C70A C75A 1.412(6) . ? C71A C72A 1.391(7) . ? C72A C73A 1.354(7) . ? C73A C74A 1.380(7) . ? C74A C75A 1.383(6) . ? 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 C8 Ru1 C7 100.25(19) . . ? C8 Ru1 C13 94.87(18) . . ? C7 Ru1 C13 88.48(18) . . ? C8 Ru1 C2 97.23(18) . . ? C7 Ru1 C2 160.80(17) . . ? C13 Ru1 C2 97.92(17) . . ? C8 Ru1 P1 91.87(13) . . ? C7 Ru1 P1 90.49(12) . . ? C13 Ru1 P1 173.26(13) . . ? C2 Ru1 P1 81.02(11) . . ? C8 Ru1 Ru3 140.22(14) . . ? C7 Ru1 Ru3 113.29(13) . . ? C13 Ru1 Ru3 66.45(13) . . ? C2 Ru1 Ru3 54.48(11) . . ? P1 Ru1 Ru3 107.98(3) . . ? C8 Ru1 Ru2 141.63(13) . . ? C7 Ru1 Ru2 91.35(12) . . ? C13 Ru1 Ru2 122.11(13) . . ? C2 Ru1 Ru2 69.89(11) . . ? P1 Ru1 Ru2 51.25(3) . . ? Ru3 Ru1 Ru2 60.824(12) . . ? C10 Ru2 C9 96.69(18) . . ? C10 Ru2 C1 93.79(17) . . ? C9 Ru2 C1 169.03(16) . . ? C10 Ru2 P2 98.86(13) . . ? C9 Ru2 P2 96.86(14) . . ? C1 Ru2 P2 84.70(11) . . ? C10 Ru2 P1 101.56(14) . . ? C9 Ru2 P1 92.49(13) . . ? C1 Ru2 P1 82.20(11) . . ? P2 Ru2 P1 156.36(4) . . ? C10 Ru2 Ru3 131.87(13) . . ? C9 Ru2 Ru3 120.62(13) . . ? C1 Ru2 Ru3 52.62(10) . . ? P2 Ru2 Ru3 51.12(3) . . ? P1 Ru2 Ru3 105.62(3) . . ? C10 Ru2 Ru1 149.66(14) . . ? C9 Ru2 Ru1 100.02(12) . . ? C1 Ru2 Ru1 69.13(10) . . ? P2 Ru2 Ru1 104.04(3) . . ? P1 Ru2 Ru1 52.79(3) . . ? Ru3 Ru2 Ru1 56.782(12) . . ? C12 Ru3 C11 89.59(18) . . ? C12 Ru3 P2 103.94(13) . . ? C11 Ru3 P2 91.74(13) . . ? C12 Ru3 C2 95.23(17) . . ? C11 Ru3 C2 150.00(16) . . ? P2 Ru3 C2 115.55(11) . . ? C12 Ru3 C1 93.42(16) . . ? C11 Ru3 C1 173.68(17) . . ? P2 Ru3 C1 82.15(11) . . ? C2 Ru3 C1 35.16(14) . . ? C12 Ru3 Ru1 138.93(13) . . ? C11 Ru3 Ru1 110.60(13) . . ? P2 Ru3 Ru1 110.48(3) . . ? C2 Ru3 Ru1 49.93(10) . . ? C1 Ru3 Ru1 70.41(10) . . ? C12 Ru3 Ru2 132.12(13) . . ? C11 Ru3 Ru2 126.77(13) . . ? P2 Ru3 Ru2 52.43(3) . . ? C2 Ru3 Ru2 69.14(10) . . ? C1 Ru3 Ru2 47.70(10) . . ? Ru1 Ru3 Ru2 62.394(12) . . ? C20 P1 C40 100.5(2) . . ? C20 P1 Ru2 122.12(15) . . ? C40 P1 Ru2 121.88(15) . . ? C20 P1 Ru1 117.85(14) . . ? C40 P1 Ru1 119.01(14) . . ? Ru2 P1 Ru1 75.96(3) . . ? C70 P2 C50 101.87(19) . . ? C70 P2 Ru3 119.23(14) . . ? C50 P2 Ru3 116.64(13) . . ? C70 P2 Ru2 123.73(13) . . ? C50 P2 Ru2 118.81(14) . . ? Ru3 P2 Ru2 76.45(4) . . ? C2 C1 C4 126.1(4) . . ? C2 C1 Ru2 111.8(3) . . ? C4 C1 Ru2 122.0(3) . . ? C2 C1 Ru3 72.1(2) . . ? C4 C1 Ru3 118.8(3) . . ? Ru2 C1 Ru3 79.67(13) . . ? C1 C2 C30 125.3(4) . . ? C1 C2 Ru1 109.1(3) . . ? C30 C2 Ru1 125.2(3) . . ? C1 C2 Ru3 72.7(2) . . ? C30 C2 Ru3 124.4(3) . . ? Ru1 C2 Ru3 75.58(13) . . ? C5 C4 C1 174.4(4) . . ? C4 C5 C6 178.7(5) . . ? C5 C6 C61 109.9(4) . . ? C5 C6 C63 109.7(4) . . ? C61 C6 C63 111.4(4) . . ? C5 C6 C62 107.7(4) . . ? C61 C6 C62 108.9(4) . . ? C63 C6 C62 109.1(5) . . ? O7 C7 Ru1 173.1(4) . . ? O8 C8 Ru1 178.7(5) . . ? O9 C9 Ru2 177.4(4) . . ? O10 C10 Ru2 177.1(4) . . ? O11 C11 Ru3 176.3(4) . . ? O12 C12 Ru3 176.4(4) . . ? O13 C13 Ru1 164.3(4) . . ? C21 C20 C25 117.8(4) . . ? C21 C20 P1 123.5(3) . . ? C25 C20 P1 118.5(3) . . ? C22 C21 C20 121.1(5) . . ? C23 C22 C21 120.7(5) . . ? C22 C23 C24 119.8(5) . . ? C23 C24 C25 119.4(5) . . ? C24 C25 C20 121.1(5) . . ? C35 C30 C31 117.8(4) . . ? C35 C30 C2 122.9(4) . . ? C31 C30 C2 119.3(4) . . ? C32 C31 C30 119.7(4) . . ? C33 C32 C31 121.2(4) . . ? C32 C33 C34 118.9(5) . . ? C35 C34 C33 120.8(5) . . ? C34 C35 C30 121.5(4) . . ? C45 C40 C41 118.5(4) . . ? C45 C40 P1 121.9(3) . . ? C41 C40 P1 119.5(3) . . ? C40 C41 C42 120.9(4) . . ? C43 C42 C41 119.4(5) . . ? C44 C43 C42 120.3(5) . . ? C43 C44 C45 120.3(5) . . ? C40 C45 C44 120.5(5) . . ? C55 C50 C51 117.9(4) . . ? C55 C50 P2 123.8(3) . . ? C51 C50 P2 118.1(3) . . ? C52 C51 C50 119.9(4) . . ? C53 C52 C51 121.1(5) . . ? C52 C53 C54 119.5(4) . . ? C53 C54 C55 120.2(4) . . ? C54 C55 C50 121.3(4) . . ? C71 C70 C75 119.2(4) . . ? C71 C70 P2 120.2(3) . . ? C75 C70 P2 120.3(3) . . ? C70 C71 C72 120.1(4) . . ? C73 C72 C71 120.1(4) . . ? C74 C73 C72 120.0(4) . . ? C73 C74 C75 120.7(4) . . ? C74 C75 C70 119.8(4) . . ? C13A Ru1A C8A 92.00(18) . . ? C13A Ru1A C7A 101.23(19) . . ? C8A Ru1A C7A 91.64(17) . . ? C13A Ru1A C2A 97.64(17) . . ? C8A Ru1A C2A 96.71(16) . . ? C7A Ru1A C2A 159.06(17) . . ? C13A Ru1A P1A 93.44(14) . . ? C8A Ru1A P1A 174.13(13) . . ? C7A Ru1A P1A 89.45(12) . . ? C2A Ru1A P1A 80.39(11) . . ? C13A Ru1A Ru3A 139.93(14) . . ? C8A Ru1A Ru3A 67.48(13) . . ? C7A Ru1A Ru3A 112.90(13) . . ? C2A Ru1A Ru3A 54.15(11) . . ? P1A Ru1A Ru3A 106.80(3) . . ? C13A Ru1A Ru2A 143.33(13) . . ? C8A Ru1A Ru2A 123.00(13) . . ? C7A Ru1A Ru2A 89.31(12) . . ? C2A Ru1A Ru2A 70.04(11) . . ? P1A Ru1A Ru2A 51.23(3) . . ? Ru3A Ru1A Ru2A 60.028(12) . . ? C10A Ru2A C9A 96.52(18) . . ? C10A Ru2A C1A 93.04(17) . . ? C9A Ru2A C1A 169.89(17) . . ? C10A Ru2A P1A 102.36(14) . . ? C9A Ru2A P1A 93.68(14) . . ? C1A Ru2A P1A 81.03(11) . . ? C10A Ru2A P2A 97.28(14) . . ? C9A Ru2A P2A 95.53(14) . . ? C1A Ru2A P2A 86.48(11) . . ? P1A Ru2A P2A 157.18(4) . . ? C10A Ru2A Ru3A 129.98(14) . . ? C9A Ru2A Ru3A 121.30(12) . . ? C1A Ru2A Ru3A 53.06(10) . . ? P1A Ru2A Ru3A 106.12(3) . . ? P2A Ru2A Ru3A 51.51(3) . . ? C10A Ru2A Ru1A 150.55(14) . . ? C9A Ru2A Ru1A 100.69(13) . . ? C1A Ru2A Ru1A 69.24(11) . . ? P1A Ru2A Ru1A 53.07(3) . . ? P2A Ru2A Ru1A 104.58(3) . . ? Ru3A Ru2A Ru1A 57.475(12) . . ? C12A Ru3A C11A 90.24(19) . . ? C12A Ru3A P2A 105.02(14) . . ? C11A Ru3A P2A 92.89(14) . . ? C12A Ru3A C2A 95.34(18) . . ? C11A Ru3A C2A 146.10(17) . . ? P2A Ru3A C2A 117.58(10) . . ? C12A Ru3A C1A 93.89(18) . . ? C11A Ru3A C1A 175.45(17) . . ? P2A Ru3A C1A 84.20(11) . . ? C2A Ru3A C1A 35.31(14) . . ? C12A Ru3A Ru1A 138.59(14) . . ? C11A Ru3A Ru1A 107.75(13) . . ? P2A Ru3A Ru1A 110.74(3) . . ? C2A Ru3A Ru1A 49.68(10) . . ? C1A Ru3A Ru1A 70.21(10) . . ? C12A Ru3A Ru2A 133.02(14) . . ? C11A Ru3A Ru2A 127.26(13) . . ? P2A Ru3A Ru2A 53.18(3) . . ? C2A Ru3A Ru2A 69.77(10) . . ? C1A Ru3A Ru2A 48.21(10) . . ? Ru1A Ru3A Ru2A 62.497(12) . . ? C20A P1A C40A 100.58(18) . . ? C20A P1A Ru2A 121.27(14) . . ? C40A P1A Ru2A 122.21(14) . . ? C20A P1A Ru1A 117.87(14) . . ? C40A P1A Ru1A 119.66(13) . . ? Ru2A P1A Ru1A 75.69(3) . . ? C70A P2A C50A 101.6(2) . . ? C70A P2A Ru3A 122.21(15) . . ? C50A P2A Ru3A 115.80(14) . . ? C70A P2A Ru2A 121.72(14) . . ? C50A P2A Ru2A 120.27(15) . . ? Ru3A P2A Ru2A 75.30(4) . . ? C2A C1A C4A 125.9(4) . . ? C2A C1A Ru2A 111.6(3) . . ? C4A C1A Ru2A 122.4(3) . . ? C2A C1A Ru3A 72.1(2) . . ? C4A C1A Ru3A 120.5(3) . . ? Ru2A C1A Ru3A 78.73(13) . . ? C1A C2A C30A 125.1(4) . . ? C1A C2A Ru1A 109.1(3) . . ? C30A C2A Ru1A 125.2(3) . . ? C1A C2A Ru3A 72.6(2) . . ? C30A C2A Ru3A 125.0(3) . . ? Ru1A C2A Ru3A 76.17(13) . . ? C5A C4A C1A 174.2(5) . . ? C4A C5A C6A 169.5(7) . . ? C4A C5A C6B 169.8(6) . . ? C6A C5A C6B 20.8(6) . . ? C5A C6A C61A 112.9(11) . . ? C5A C6A C62A 109.4(16) . . ? C61A C6A C62A 110.3(16) . . ? C5A C6A C63A 104.1(10) . . ? C61A C6A C63A 110.9(13) . . ? C62A C6A C63A 109.1(17) . . ? C5A C6B C61B 109.4(9) . . ? C5A C6B C62B 109.2(12) . . ? C61B C6B C62B 109.0(12) . . ? C5A C6B C63B 110.7(8) . . ? C61B C6B C63B 110.6(10) . . ? C62B C6B C63B 107.9(13) . . ? O7A C7A Ru1A 173.9(4) . . ? O8A C8A Ru1A 165.8(4) . . ? O9A C9A Ru2A 178.7(4) . . ? O10A C10A Ru2A 177.3(4) . . ? O11A C11A Ru3A 176.9(4) . . ? O12A C12A Ru3A 176.9(4) . . ? O13A C13A Ru1A 178.8(4) . . ? C25A C20A C21A 119.2(4) . . ? C25A C20A P1A 123.0(3) . . ? C21A C20A P1A 117.8(3) . . ? C22A C21A C20A 119.9(4) . . ? C23A C22A C21A 120.7(4) . . ? C24A C23A C22A 119.9(4) . . ? C23A C24A C25A 120.5(4) . . ? C20A C25A C24A 119.7(4) . . ? C35A C30A C31A 118.3(4) . . ? C35A C30A C2A 120.4(4) . . ? C31A C30A C2A 121.1(4) . . ? C32A C31A C30A 120.7(5) . . ? C33A C32A C31A 120.2(5) . . ? C34A C33A C32A 119.3(4) . . ? C33A C34A C35A 121.1(5) . . ? C30A C35A C34A 120.4(4) . . ? C41A C40A C45A 118.4(4) . . ? C41A C40A P1A 118.9(3) . . ? C45A C40A P1A 122.6(3) . . ? C40A C41A C42A 121.4(4) . . ? C41A C42A C43A 119.5(5) . . ? C42A C43A C44A 119.3(4) . . ? C45A C44A C43A 120.4(4) . . ? C44A C45A C40A 121.1(4) . . ? C51A C50A C55A 118.2(4) . . ? C51A C50A P2A 119.2(3) . . ? C55A C50A P2A 122.6(4) . . ? C52A C51A C50A 121.1(5) . . ? C53A C52A C51A 120.5(5) . . ? C54A C53A C52A 119.3(5) . . ? C53A C54A C55A 121.4(5) . . ? C50A C55A C54A 119.4(5) . . ? C71A C70A C75A 119.1(4) . . ? C71A C70A P2A 119.4(3) . . ? C75A C70A P2A 121.1(3) . . ? C70A C71A C72A 119.9(5) . . ? C73A C72A C71A 120.9(5) . . ? C72A C73A C74A 120.3(5) . . ? C73A C74A C75A 120.2(5) . . ? C74A C75A C70A 119.6(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.734 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.133 #===END data_pjl60 _database_code_CSD 153697 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H30 O7 P2 Ru3' _chemical_formula_weight 1071.86 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1720(5) _cell_length_b 13.2256(6) _cell_length_c 15.5535(7) _cell_angle_alpha 80.4040(10) _cell_angle_beta 70.1680(10) _cell_angle_gamma 89.3950(10) _cell_volume 2128.96(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 1.177 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _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 25414 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 28.74 _reflns_number_total 10924 _reflns_number_gt 8974 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10924 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.544843(19) 0.299377(15) 0.662046(15) 0.02279(6) Uani 1 d . . . Ru2 Ru 0.643755(19) 0.156675(14) 0.816233(14) 0.02071(6) Uani 1 d . . . Ru3 Ru 0.822060(19) 0.290675(14) 0.653934(14) 0.02048(6) Uani 1 d . . . P1 P 0.73113(6) 0.26493(5) 0.54448(5) 0.02226(13) Uani 1 d . . . P2 P 0.80931(6) 0.26658(5) 0.80983(5) 0.02226(13) Uani 1 d . . . O7 O 0.5911(2) 0.52650(16) 0.56695(19) 0.0498(6) Uani 1 d . . . O8 O 0.3457(2) 0.3663(2) 0.83311(16) 0.0529(7) Uani 1 d . . . O9 O 0.4399(2) 0.23899(16) 0.96610(15) 0.0397(5) Uani 1 d . . . O10 O 0.6660(2) -0.00706(15) 0.96934(15) 0.0376(5) Uani 1 d . . . O11 O 0.8193(2) 0.52423(15) 0.63597(17) 0.0412(5) Uani 1 d . . . O12 O 1.0992(2) 0.29836(18) 0.53356(16) 0.0450(6) Uani 1 d . . . O13 O 0.3600(2) 0.26474(18) 0.56519(18) 0.0494(6) Uani 1 d . . . C1 C 0.8149(2) 0.13356(19) 0.68852(18) 0.0230(5) Uani 1 d . . . C2 C 0.8074(2) 0.0431(2) 0.72099(18) 0.0255(5) Uani 1 d . . . C4 C 0.5184(2) 0.1500(2) 0.72784(19) 0.0256(5) Uani 1 d . . . C5 C 0.4983(3) 0.0619(2) 0.77137(19) 0.0275(5) Uani 1 d . . . C7 C 0.5779(3) 0.4432(2) 0.6025(2) 0.0327(6) Uani 1 d . . . C8 C 0.4212(3) 0.3395(2) 0.7729(2) 0.0336(6) Uani 1 d . . . C9 C 0.5166(3) 0.2101(2) 0.90704(19) 0.0279(6) Uani 1 d . . . C10 C 0.6568(3) 0.0542(2) 0.91077(19) 0.0268(5) Uani 1 d . . . C11 C 0.8176(3) 0.4370(2) 0.64105(19) 0.0273(5) Uani 1 d . . . C12 C 0.9949(3) 0.2964(2) 0.5804(2) 0.0292(6) Uani 1 d . . . C13 C 0.4290(3) 0.2790(2) 0.6012(2) 0.0306(6) Uani 1 d . . . C20 C 0.7697(2) 0.3542(2) 0.43396(18) 0.0251(5) Uani 1 d . . . C21 C 0.8698(3) 0.4263(2) 0.4052(2) 0.0365(7) Uani 1 d . . . H21 H 0.9215 0.4289 0.4423 0.044 Uiso 1 calc R . . C22 C 0.8958(3) 0.4952(3) 0.3222(2) 0.0432(8) Uani 1 d . . . H22 H 0.9644 0.5451 0.3035 0.052 Uiso 1 calc R . . C23 C 0.8227(3) 0.4913(2) 0.2676(2) 0.0376(7) Uani 1 d . . . H23 H 0.8414 0.5375 0.2105 0.045 Uiso 1 calc R . . C24 C 0.7218(3) 0.4199(2) 0.2959(2) 0.0406(7) Uani 1 d . . . H24 H 0.6699 0.4181 0.2587 0.049 Uiso 1 calc R . . C25 C 0.6957(3) 0.3507(2) 0.3785(2) 0.0357(7) Uani 1 d . . . H25 H 0.6271 0.3009 0.3971 0.043 Uiso 1 calc R . . C30 C 0.8215(3) -0.0666(2) 0.74106(19) 0.0296(6) Uani 1 d . . . C31 C 0.7774(3) -0.1326(2) 0.6968(2) 0.0414(7) Uani 1 d . . . H31 H 0.7300 -0.1068 0.6581 0.050 Uiso 1 calc R . . C32 C 0.8019(4) -0.2362(2) 0.7087(3) 0.0561(10) Uani 1 d . . . H32 H 0.7727 -0.2808 0.6772 0.067 Uiso 1 calc R . . C33 C 0.8686(4) -0.2743(3) 0.7659(3) 0.0642(13) Uani 1 d . . . H33 H 0.8859 -0.3450 0.7734 0.077 Uiso 1 calc R . . C34 C 0.9105(4) -0.2099(3) 0.8125(3) 0.0635(12) Uani 1 d . . . H34 H 0.9550 -0.2368 0.8529 0.076 Uiso 1 calc R . . C35 C 0.8874(3) -0.1059(2) 0.8002(3) 0.0462(8) Uani 1 d . . . H35 H 0.9165 -0.0616 0.8320 0.055 Uiso 1 calc R . . C40 C 0.7454(3) 0.14054(19) 0.50716(18) 0.0253(5) Uani 1 d . . . C41 C 0.8653(3) 0.1114(2) 0.4575(2) 0.0409(7) Uani 1 d . . . H41 H 0.9373 0.1576 0.4407 0.049 Uiso 1 calc R . . C42 C 0.8802(3) 0.0149(3) 0.4325(3) 0.0480(9) Uani 1 d . . . H42 H 0.9629 -0.0054 0.4003 0.058 Uiso 1 calc R . . C43 C 0.7769(3) -0.0515(2) 0.4537(2) 0.0389(7) Uani 1 d . . . H43 H 0.7877 -0.1162 0.4339 0.047 Uiso 1 calc R . . C44 C 0.6583(3) -0.0245(2) 0.5033(2) 0.0379(7) Uani 1 d . . . H44 H 0.5869 -0.0712 0.5196 0.045 Uiso 1 calc R . . C45 C 0.6421(3) 0.0721(2) 0.5300(2) 0.0317(6) Uani 1 d . . . H45 H 0.5595 0.0908 0.5642 0.038 Uiso 1 calc R . . C50 C 0.9352(3) 0.20620(19) 0.84683(19) 0.0266(5) Uani 1 d . . . C51 C 1.0576(3) 0.2036(2) 0.7843(2) 0.0356(7) Uani 1 d . . . H51 H 1.0760 0.2300 0.7203 0.043 Uiso 1 calc R . . C52 C 1.1535(3) 0.1620(3) 0.8158(3) 0.0484(9) Uani 1 d . . . H52 H 1.2371 0.1599 0.7727 0.058 Uiso 1 calc R . . C53 C 1.1287(4) 0.1240(3) 0.9079(3) 0.0537(10) Uani 1 d . . . H53 H 1.1951 0.0965 0.9285 0.064 Uiso 1 calc R . . C54 C 1.0075(3) 0.1259(2) 0.9707(3) 0.0468(8) Uani 1 d . . . H54 H 0.9901 0.0998 1.0346 0.056 Uiso 1 calc R . . C55 C 0.9108(3) 0.1661(2) 0.9402(2) 0.0346(6) Uani 1 d . . . H55 H 0.8270 0.1662 0.9835 0.042 Uiso 1 calc R . . C60 C 0.4404(3) -0.0417(2) 0.79673(19) 0.0281(6) Uani 1 d . . . C61 C 0.3499(3) -0.0637(2) 0.7574(2) 0.0416(7) Uani 1 d . . . H61 H 0.3300 -0.0118 0.7148 0.050 Uiso 1 calc R . . C62 C 0.2892(4) -0.1601(3) 0.7799(3) 0.0538(9) Uani 1 d . . . H62 H 0.2272 -0.1739 0.7535 0.065 Uiso 1 calc R . . C63 C 0.3189(4) -0.2362(3) 0.8410(3) 0.0522(9) Uani 1 d . . . H63 H 0.2763 -0.3020 0.8573 0.063 Uiso 1 calc R . . C64 C 0.4094(3) -0.2168(2) 0.8779(2) 0.0425(8) Uani 1 d . . . H64 H 0.4304 -0.2698 0.9189 0.051 Uiso 1 calc R . . C65 C 0.4714(3) -0.1201(2) 0.8561(2) 0.0329(6) Uani 1 d . . . H65 H 0.5348 -0.1077 0.8818 0.040 Uiso 1 calc R . . C70 C 0.7731(3) 0.37476(19) 0.87289(19) 0.0272(5) Uani 1 d . . . C71 C 0.6702(3) 0.4340(2) 0.8670(2) 0.0370(7) Uani 1 d . . . H71 H 0.6192 0.4156 0.8335 0.044 Uiso 1 calc R . . C72 C 0.6433(3) 0.5191(2) 0.9099(2) 0.0441(8) Uani 1 d . . . H72 H 0.5740 0.5592 0.9051 0.053 Uiso 1 calc R . . C73 C 0.7154(4) 0.5467(3) 0.9597(2) 0.0517(9) Uani 1 d . . . H73 H 0.6953 0.6047 0.9898 0.062 Uiso 1 calc R . . C74 C 0.8160(4) 0.4897(3) 0.9653(3) 0.0521(9) Uani 1 d . . . H74 H 0.8661 0.5086 0.9994 0.063 Uiso 1 calc R . . C75 C 0.8463(3) 0.4042(2) 0.9219(2) 0.0391(7) Uani 1 d . . . H75 H 0.9173 0.3659 0.9258 0.047 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02045(10) 0.02122(10) 0.02644(11) -0.00150(8) -0.00896(8) 0.00268(8) Ru2 0.01998(10) 0.01935(10) 0.02157(11) -0.00137(7) -0.00655(8) 0.00128(7) Ru3 0.01968(10) 0.01873(10) 0.02222(11) -0.00092(7) -0.00736(8) 0.00105(7) P1 0.0216(3) 0.0211(3) 0.0233(3) -0.0016(2) -0.0078(3) 0.0006(2) P2 0.0225(3) 0.0212(3) 0.0232(3) -0.0027(2) -0.0087(3) 0.0016(2) O7 0.0469(14) 0.0261(11) 0.0697(17) 0.0065(11) -0.0184(13) 0.0037(10) O8 0.0516(15) 0.0703(17) 0.0368(13) -0.0148(12) -0.0136(11) 0.0342(13) O9 0.0393(12) 0.0415(12) 0.0315(11) -0.0047(9) -0.0043(9) 0.0153(10) O10 0.0456(12) 0.0312(10) 0.0346(12) 0.0044(8) -0.0166(10) 0.0034(9) O11 0.0449(13) 0.0231(10) 0.0575(15) -0.0021(9) -0.0222(11) 0.0000(9) O12 0.0269(11) 0.0547(14) 0.0414(13) 0.0032(10) -0.0019(10) 0.0064(10) O13 0.0465(14) 0.0466(13) 0.0651(17) 0.0022(12) -0.0371(13) -0.0064(11) C1 0.0197(12) 0.0252(12) 0.0253(13) -0.0083(10) -0.0076(10) 0.0044(10) C2 0.0243(13) 0.0273(13) 0.0245(13) -0.0051(10) -0.0076(10) 0.0039(10) C4 0.0220(12) 0.0277(13) 0.0265(13) -0.0035(10) -0.0083(11) 0.0018(10) C5 0.0236(13) 0.0299(13) 0.0294(14) -0.0056(11) -0.0093(11) 0.0033(11) C7 0.0244(14) 0.0303(14) 0.0422(17) -0.0039(12) -0.0111(12) 0.0053(11) C8 0.0355(16) 0.0350(15) 0.0336(16) -0.0042(12) -0.0171(13) 0.0126(13) C9 0.0303(14) 0.0240(12) 0.0291(14) -0.0004(10) -0.0118(12) 0.0051(11) C10 0.0248(13) 0.0262(13) 0.0258(13) -0.0038(10) -0.0046(11) 0.0015(10) C11 0.0238(13) 0.0277(13) 0.0306(14) -0.0008(10) -0.0113(11) -0.0007(10) C12 0.0289(14) 0.0280(13) 0.0288(14) 0.0025(10) -0.0110(12) 0.0007(11) C13 0.0273(14) 0.0279(13) 0.0369(16) 0.0034(11) -0.0153(12) -0.0004(11) C20 0.0236(13) 0.0262(12) 0.0240(13) -0.0018(10) -0.0077(10) 0.0026(10) C21 0.0363(16) 0.0403(16) 0.0331(16) 0.0061(12) -0.0177(13) -0.0082(13) C22 0.0398(18) 0.0460(18) 0.0359(18) 0.0155(14) -0.0128(14) -0.0135(14) C23 0.0405(17) 0.0389(16) 0.0303(16) 0.0062(12) -0.0138(13) 0.0017(13) C24 0.0468(19) 0.0474(18) 0.0335(17) -0.0009(13) -0.0243(15) 0.0020(15) C25 0.0403(17) 0.0354(15) 0.0343(16) -0.0004(12) -0.0186(14) -0.0069(13) C30 0.0296(14) 0.0223(12) 0.0290(14) 0.0006(10) -0.0024(11) 0.0028(11) C31 0.0475(19) 0.0281(14) 0.0443(19) -0.0089(13) -0.0088(15) 0.0009(13) C32 0.067(3) 0.0273(16) 0.060(2) -0.0125(15) -0.002(2) -0.0029(16) C33 0.077(3) 0.0253(16) 0.060(3) 0.0051(16) 0.009(2) 0.0111(17) C34 0.075(3) 0.041(2) 0.066(3) 0.0095(18) -0.023(2) 0.023(2) C35 0.056(2) 0.0320(16) 0.053(2) -0.0014(14) -0.0251(18) 0.0107(15) C40 0.0269(13) 0.0234(12) 0.0254(13) -0.0034(10) -0.0090(11) 0.0009(10) C41 0.0282(15) 0.0365(16) 0.0475(19) -0.0105(14) 0.0021(14) -0.0078(13) C42 0.0345(17) 0.0405(18) 0.059(2) -0.0202(16) 0.0023(16) 0.0052(14) C43 0.0399(17) 0.0296(14) 0.0509(19) -0.0154(13) -0.0165(15) 0.0072(13) C44 0.0346(16) 0.0327(15) 0.054(2) -0.0153(14) -0.0216(15) 0.0000(12) C45 0.0268(14) 0.0320(14) 0.0413(17) -0.0148(12) -0.0142(12) 0.0050(11) C50 0.0277(13) 0.0259(13) 0.0286(14) -0.0050(10) -0.0124(11) 0.0005(10) C51 0.0280(15) 0.0397(16) 0.0376(17) 0.0022(13) -0.0133(13) 0.0022(12) C52 0.0255(15) 0.054(2) 0.060(2) 0.0095(17) -0.0157(15) 0.0052(14) C53 0.042(2) 0.056(2) 0.068(3) 0.0103(18) -0.0341(19) 0.0037(17) C54 0.056(2) 0.0428(18) 0.048(2) 0.0081(15) -0.0333(18) 0.0007(16) C55 0.0372(16) 0.0363(15) 0.0324(16) -0.0026(12) -0.0162(13) 0.0033(13) C60 0.0262(13) 0.0269(13) 0.0269(14) -0.0038(10) -0.0038(11) -0.0014(11) C61 0.0425(18) 0.0391(17) 0.048(2) -0.0047(14) -0.0221(16) -0.0065(14) C62 0.055(2) 0.051(2) 0.061(2) -0.0108(18) -0.0244(19) -0.0181(17) C63 0.067(2) 0.0357(17) 0.046(2) -0.0077(15) -0.0077(18) -0.0218(16) C64 0.060(2) 0.0262(14) 0.0332(17) -0.0012(12) -0.0075(15) -0.0058(14) C65 0.0379(16) 0.0277(14) 0.0316(15) -0.0035(11) -0.0105(13) -0.0022(12) C70 0.0300(14) 0.0236(12) 0.0252(13) -0.0039(10) -0.0058(11) -0.0012(10) C71 0.0370(16) 0.0280(14) 0.0422(17) -0.0094(12) -0.0073(14) 0.0061(12) C72 0.0433(19) 0.0309(15) 0.049(2) -0.0122(14) -0.0023(15) 0.0076(14) C73 0.070(3) 0.0326(16) 0.044(2) -0.0176(14) -0.0036(18) 0.0030(16) C74 0.080(3) 0.0380(18) 0.046(2) -0.0164(15) -0.026(2) -0.0039(18) C75 0.0489(19) 0.0330(15) 0.0388(17) -0.0111(13) -0.0173(15) 0.0006(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C13 1.888(3) . ? Ru1 C7 1.951(3) . ? Ru1 C8 1.959(3) . ? Ru1 C4 2.042(3) . ? Ru1 P1 2.3576(7) . ? Ru1 Ru3 3.0583(3) . ? Ru2 C9 1.860(3) . ? Ru2 C10 1.870(3) . ? Ru2 C4 2.282(3) . ? Ru2 C1 2.304(2) . ? Ru2 P2 2.3296(7) . ? Ru2 C5 2.409(3) . ? Ru2 C2 2.576(2) . ? Ru2 Ru3 2.9415(3) . ? Ru3 C12 1.876(3) . ? Ru3 C11 1.913(3) . ? Ru3 C1 2.053(3) . ? Ru3 P1 2.3281(7) . ? Ru3 P2 2.3473(7) . ? P1 C40 1.822(3) . ? P1 C20 1.834(3) . ? P2 C50 1.822(3) . ? P2 C70 1.833(3) . ? O7 C7 1.134(3) . ? O8 C8 1.132(4) . ? O9 C9 1.141(3) . ? O10 C10 1.146(3) . ? O11 C11 1.144(3) . ? O12 C12 1.143(3) . ? O13 C13 1.130(3) . ? C1 C2 1.210(4) . ? C2 C30 1.451(3) . ? C4 C5 1.228(4) . ? C5 C60 1.454(4) . ? C20 C21 1.378(4) . ? C20 C25 1.388(4) . ? C21 C22 1.393(4) . ? C22 C23 1.371(4) . ? C23 C24 1.379(5) . ? C24 C25 1.391(4) . ? C30 C31 1.385(4) . ? C30 C35 1.397(4) . ? C31 C32 1.389(4) . ? C32 C33 1.375(6) . ? C33 C34 1.384(6) . ? C34 C35 1.391(4) . ? C40 C45 1.383(4) . ? C40 C41 1.388(4) . ? C41 C42 1.388(4) . ? C42 C43 1.371(5) . ? C43 C44 1.366(4) . ? C44 C45 1.399(4) . ? C50 C51 1.388(4) . ? C50 C55 1.394(4) . ? C51 C52 1.394(4) . ? C52 C53 1.370(5) . ? C53 C54 1.378(5) . ? C54 C55 1.387(4) . ? C60 C65 1.393(4) . ? C60 C61 1.403(4) . ? C61 C62 1.384(4) . ? C62 C63 1.384(5) . ? C63 C64 1.365(5) . ? C64 C65 1.395(4) . ? C70 C75 1.389(4) . ? C70 C71 1.404(4) . ? C71 C72 1.381(4) . ? C72 C73 1.382(5) . ? C73 C74 1.366(5) . ? C74 C75 1.393(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Ru1 C7 91.74(12) . . ? C13 Ru1 C8 97.23(13) . . ? C7 Ru1 C8 90.14(12) . . ? C13 Ru1 C4 91.70(11) . . ? C7 Ru1 C4 176.56(12) . . ? C8 Ru1 C4 89.68(11) . . ? C13 Ru1 P1 97.11(9) . . ? C7 Ru1 P1 86.96(9) . . ? C8 Ru1 P1 165.45(9) . . ? C4 Ru1 P1 92.36(7) . . ? C13 Ru1 Ru3 145.85(9) . . ? C7 Ru1 Ru3 89.12(8) . . ? C8 Ru1 Ru3 116.91(9) . . ? C4 Ru1 Ru3 87.89(7) . . ? P1 Ru1 Ru3 48.839(17) . . ? C9 Ru2 C10 87.54(11) . . ? C9 Ru2 C4 92.91(11) . . ? C10 Ru2 C4 126.92(11) . . ? C9 Ru2 C1 165.56(10) . . ? C10 Ru2 C1 103.78(10) . . ? C4 Ru2 C1 87.45(9) . . ? C9 Ru2 P2 96.41(9) . . ? C10 Ru2 P2 97.59(9) . . ? C4 Ru2 P2 134.87(7) . . ? C1 Ru2 P2 73.48(7) . . ? C9 Ru2 C5 94.82(11) . . ? C10 Ru2 C5 96.83(11) . . ? C4 Ru2 C5 30.20(9) . . ? C1 Ru2 C5 92.73(9) . . ? P2 Ru2 C5 162.05(7) . . ? C9 Ru2 C2 166.03(10) . . ? C10 Ru2 C2 79.23(10) . . ? C4 Ru2 C2 91.49(9) . . ? C1 Ru2 C2 28.01(9) . . ? P2 Ru2 C2 89.82(6) . . ? C5 Ru2 C2 82.44(9) . . ? C9 Ru2 Ru3 121.55(8) . . ? C10 Ru2 Ru3 136.29(8) . . ? C4 Ru2 Ru3 86.60(7) . . ? C1 Ru2 Ru3 44.03(6) . . ? P2 Ru2 Ru3 51.298(17) . . ? C5 Ru2 Ru3 110.77(7) . . ? C2 Ru2 Ru3 71.94(6) . . ? C12 Ru3 C11 92.62(12) . . ? C12 Ru3 C1 92.72(11) . . ? C11 Ru3 C1 171.50(11) . . ? C12 Ru3 P1 99.55(9) . . ? C11 Ru3 P1 99.41(8) . . ? C1 Ru3 P1 86.22(7) . . ? C12 Ru3 P2 107.79(9) . . ? C11 Ru3 P2 94.30(9) . . ? C1 Ru3 P2 77.77(7) . . ? P1 Ru3 P2 148.74(3) . . ? C12 Ru3 Ru2 138.15(8) . . ? C11 Ru3 Ru2 121.13(8) . . ? C1 Ru3 Ru2 51.25(7) . . ? P1 Ru3 Ru2 98.431(18) . . ? P2 Ru3 Ru2 50.761(17) . . ? C12 Ru3 Ru1 147.74(9) . . ? C11 Ru3 Ru1 84.78(8) . . ? C1 Ru3 Ru1 94.18(7) . . ? P1 Ru3 Ru1 49.675(17) . . ? P2 Ru3 Ru1 104.466(18) . . ? Ru2 Ru3 Ru1 66.320(7) . . ? C40 P1 C20 102.12(12) . . ? C40 P1 Ru3 118.32(9) . . ? C20 P1 Ru3 120.68(9) . . ? C40 P1 Ru1 119.91(9) . . ? C20 P1 Ru1 114.82(8) . . ? Ru3 P1 Ru1 81.49(2) . . ? C50 P2 C70 102.57(12) . . ? C50 P2 Ru2 115.92(9) . . ? C70 P2 Ru2 119.44(9) . . ? C50 P2 Ru3 121.30(9) . . ? C70 P2 Ru3 119.60(9) . . ? Ru2 P2 Ru3 77.94(2) . . ? C2 C1 Ru3 171.2(2) . . ? C2 C1 Ru2 88.61(19) . . ? Ru3 C1 Ru2 84.71(8) . . ? C1 C2 C30 167.3(3) . . ? C1 C2 Ru2 63.39(16) . . ? C30 C2 Ru2 129.34(19) . . ? C5 C4 Ru1 176.7(2) . . ? C5 C4 Ru2 80.65(19) . . ? Ru1 C4 Ru2 98.66(11) . . ? C4 C5 C60 154.4(3) . . ? C4 C5 Ru2 69.15(18) . . ? C60 C5 Ru2 136.40(19) . . ? O7 C7 Ru1 176.3(3) . . ? O8 C8 Ru1 175.3(2) . . ? O9 C9 Ru2 176.4(2) . . ? O10 C10 Ru2 178.5(2) . . ? O11 C11 Ru3 176.4(2) . . ? O12 C12 Ru3 177.8(3) . . ? O13 C13 Ru1 178.7(2) . . ? C21 C20 C25 118.9(3) . . ? C21 C20 P1 121.4(2) . . ? C25 C20 P1 119.7(2) . . ? C20 C21 C22 120.7(3) . . ? C23 C22 C21 120.1(3) . . ? C22 C23 C24 119.8(3) . . ? C23 C24 C25 120.2(3) . . ? C20 C25 C24 120.2(3) . . ? C31 C30 C35 119.3(3) . . ? C31 C30 C2 120.2(3) . . ? C35 C30 C2 120.3(3) . . ? C30 C31 C32 120.4(3) . . ? C33 C32 C31 120.1(4) . . ? C32 C33 C34 120.3(3) . . ? C33 C34 C35 119.9(4) . . ? C34 C35 C30 120.0(4) . . ? C45 C40 C41 118.7(3) . . ? C45 C40 P1 122.5(2) . . ? C41 C40 P1 118.7(2) . . ? C42 C41 C40 120.1(3) . . ? C43 C42 C41 120.7(3) . . ? C44 C43 C42 119.9(3) . . ? C43 C44 C45 119.9(3) . . ? C40 C45 C44 120.6(3) . . ? C51 C50 C55 118.8(3) . . ? C51 C50 P2 121.2(2) . . ? C55 C50 P2 119.9(2) . . ? C50 C51 C52 119.7(3) . . ? C53 C52 C51 120.9(3) . . ? C52 C53 C54 119.9(3) . . ? C53 C54 C55 119.8(3) . . ? C54 C55 C50 120.8(3) . . ? C65 C60 C61 118.5(3) . . ? C65 C60 C5 123.8(3) . . ? C61 C60 C5 117.6(3) . . ? C62 C61 C60 120.7(3) . . ? C63 C62 C61 119.9(3) . . ? C64 C63 C62 120.1(3) . . ? C63 C64 C65 120.9(3) . . ? C60 C65 C64 119.9(3) . . ? C75 C70 C71 118.5(3) . . ? C75 C70 P2 123.3(2) . . ? C71 C70 P2 118.1(2) . . ? C72 C71 C70 120.0(3) . . ? C71 C72 C73 121.0(3) . . ? C74 C73 C72 119.3(3) . . ? C73 C74 C75 120.9(3) . . ? C70 C75 C74 120.2(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.74 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.168 _refine_diff_density_min -1.446 _refine_diff_density_rms 0.132 #===END data_wb46 _database_code_CSD 153698 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H38 O7 P2 Ru3' _chemical_formula_weight 1031.88 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 20.2682(10) _cell_length_b 11.0110(5) _cell_length_c 20.1026(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.1240(10) _cell_angle_gamma 90.00 _cell_volume 4369.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 1.143 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71070 _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 49056 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.75 _reflns_number_total 11306 _reflns_number_gt 8836 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+8.3056P] 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 11306 _refine_ls_number_parameters 502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.160800(16) 0.91486(3) 0.115795(16) 0.04659(9) Uani 1 d . . . Ru2 Ru 0.285641(16) 1.05986(3) 0.200029(18) 0.05045(10) Uani 1 d . . . Ru3 Ru 0.283472(16) 0.79829(3) 0.220797(15) 0.04652(9) Uani 1 d . . . P1 P 0.16869(5) 1.09472(10) 0.18286(5) 0.0468(2) Uani 1 d . . . P2 P 0.37233(5) 0.91647(11) 0.20367(6) 0.0533(3) Uani 1 d . . . O7 O 0.1692(3) 0.6962(4) 0.0231(2) 0.0963(13) Uani 1 d . . . O8 O 0.1633(2) 1.0726(3) -0.00961(18) 0.0812(11) Uani 1 d . . . O9 O 0.3060(2) 1.1583(4) 0.06707(19) 0.0867(11) Uani 1 d . . . O10 O 0.3474(2) 1.2930(4) 0.2629(2) 0.0943(12) Uani 1 d . . . O11 O 0.2963(2) 0.5939(4) 0.1238(2) 0.0961(13) Uani 1 d . . . O12 O 0.3664(2) 0.6485(5) 0.3339(2) 0.1044(15) Uani 1 d . . . O13 O 0.00808(19) 0.9145(4) 0.0820(3) 0.1050(15) Uani 1 d . . . C1 C 0.2823(2) 0.9403(4) 0.2906(2) 0.0564(10) Uani 1 d . . . C2 C 0.2918(2) 1.0078(5) 0.3372(2) 0.0611(11) Uani 1 d . . . C3 C 0.3053(4) 1.0755(7) 0.4035(3) 0.103(2) Uani 1 d . . . C4 C 0.1681(2) 0.7980(4) 0.1967(2) 0.0495(9) Uani 1 d . . . C5 C 0.1775(2) 0.7235(4) 0.2431(2) 0.0554(10) Uani 1 d . . . C6 C 0.1651(3) 0.6381(5) 0.2963(3) 0.0717(13) Uani 1 d . . . C7 C 0.1706(3) 0.7743(4) 0.0596(2) 0.0626(11) Uani 1 d . . . C8 C 0.1648(2) 1.0181(4) 0.0383(2) 0.0549(10) Uani 1 d . . . C9 C 0.2957(2) 1.1191(5) 0.1164(2) 0.0613(11) Uani 1 d . . . C10 C 0.3252(2) 1.2033(5) 0.2408(2) 0.0620(11) Uani 1 d . . . C11 C 0.2900(2) 0.6731(5) 0.1584(2) 0.0633(11) Uani 1 d . . . C12 C 0.3343(2) 0.7042(5) 0.2908(2) 0.0658(12) Uani 1 d . . . C13 C 0.0653(3) 0.9148(5) 0.0943(3) 0.0682(13) Uani 1 d . . . C20 C 0.1333(2) 1.2259(4) 0.1312(2) 0.0499(9) Uani 1 d . . . C21 C 0.1736(3) 1.3195(4) 0.1184(3) 0.0694(13) Uani 1 d . . . H21 H 0.2200 1.3168 0.1368 0.083 Uiso 1 calc R . . C22 C 0.1463(3) 1.4176(5) 0.0786(3) 0.0897(18) Uani 1 d . . . H22 H 0.1743 1.4801 0.0705 0.108 Uiso 1 calc R . . C23 C 0.0792(4) 1.4228(5) 0.0516(4) 0.096(2) Uani 1 d . . . H23 H 0.0610 1.4888 0.0247 0.115 Uiso 1 calc R . . C24 C 0.0374(3) 1.3313(6) 0.0635(3) 0.0925(19) Uani 1 d . . . H24 H -0.0089 1.3354 0.0450 0.111 Uiso 1 calc R . . C25 C 0.0643(3) 1.2334(5) 0.1029(3) 0.0716(13) Uani 1 d . . . H25 H 0.0358 1.1715 0.1107 0.086 Uiso 1 calc R . . C31 C 0.2771(4) 1.0034(8) 0.4530(3) 0.117(3) Uani 1 d . . . H31A H 0.2987 0.9254 0.4593 0.175 Uiso 1 calc R . . H31B H 0.2293 0.9929 0.4358 0.175 Uiso 1 calc R . . H31C H 0.2851 1.0454 0.4960 0.175 Uiso 1 calc R . . C32 C 0.2646(6) 1.2046(8) 0.3927(4) 0.161(4) Uani 1 d . . . H32A H 0.2723 1.2473 0.4354 0.241 Uiso 1 calc R . . H32B H 0.2170 1.1895 0.3767 0.241 Uiso 1 calc R . . H32C H 0.2805 1.2528 0.3598 0.241 Uiso 1 calc R . . C33 C 0.3756(5) 1.1115(10) 0.4252(4) 0.158(4) Uani 1 d . . . H33A H 0.3807 1.1668 0.4629 0.237 Uiso 1 calc R . . H33B H 0.3897 1.1506 0.3880 0.237 Uiso 1 calc R . . H33C H 0.4032 1.0409 0.4390 0.237 Uiso 1 calc R . . C40 C 0.1240(2) 1.1057(5) 0.2524(2) 0.0624(11) Uani 1 d . . . C41 C 0.1067(4) 1.2193(7) 0.2732(3) 0.106(2) Uani 1 d . . . H41 H 0.1159 1.2884 0.2502 0.127 Uiso 1 calc R . . C42 C 0.0758(5) 1.2307(9) 0.3282(4) 0.135(3) Uani 1 d . . . H42 H 0.0652 1.3072 0.3424 0.162 Uiso 1 calc R . . C43 C 0.0611(4) 1.1303(9) 0.3607(4) 0.121(3) Uani 1 d . . . H43 H 0.0422 1.1375 0.3985 0.145 Uiso 1 calc R . . C44 C 0.0738(4) 1.0214(8) 0.3384(5) 0.135(4) Uani 1 d . . . H44 H 0.0616 0.9525 0.3595 0.162 Uiso 1 calc R . . C45 C 0.1053(4) 1.0083(6) 0.2838(4) 0.104(2) Uani 1 d . . . H45 H 0.1134 0.9309 0.2689 0.125 Uiso 1 calc R . . C50 C 0.4077(2) 0.8890(5) 0.1293(2) 0.0626(11) Uani 1 d . . . C51 C 0.3649(3) 0.8616(6) 0.0674(3) 0.0830(16) Uani 1 d . . . H51 H 0.3185 0.8559 0.0643 0.100 Uiso 1 calc R . . C52 C 0.3899(4) 0.8424(8) 0.0102(3) 0.112(3) Uani 1 d . . . H52 H 0.3604 0.8231 -0.0310 0.134 Uiso 1 calc R . . C53 C 0.4572(4) 0.8514(8) 0.0133(4) 0.115(3) Uani 1 d . . . H53 H 0.4738 0.8384 -0.0257 0.138 Uiso 1 calc R . . C54 C 0.5002(3) 0.8791(8) 0.0731(4) 0.103(2) Uani 1 d . . . H54 H 0.5465 0.8849 0.0752 0.124 Uiso 1 calc R . . C55 C 0.4759(3) 0.8991(6) 0.1313(3) 0.0788(15) Uani 1 d . . . H55 H 0.5059 0.9195 0.1720 0.095 Uiso 1 calc R . . C61 C 0.1987(4) 0.5155(5) 0.2915(3) 0.102(2) Uani 1 d . . . H61A H 0.1830 0.4831 0.2463 0.153 Uiso 1 calc R . . H61B H 0.1872 0.4606 0.3241 0.153 Uiso 1 calc R . . H61C H 0.2469 0.5257 0.3009 0.153 Uiso 1 calc R . . C62 C 0.1933(4) 0.6922(6) 0.3671(3) 0.099(2) Uani 1 d . . . H62A H 0.2414 0.7020 0.3741 0.149 Uiso 1 calc R . . H62B H 0.1834 0.6388 0.4013 0.149 Uiso 1 calc R . . H62C H 0.1726 0.7699 0.3702 0.149 Uiso 1 calc R . . C63 C 0.0892(4) 0.6219(9) 0.2850(5) 0.144(4) Uani 1 d . . . H63A H 0.0690 0.6971 0.2940 0.217 Uiso 1 calc R . . H63B H 0.0796 0.5602 0.3152 0.217 Uiso 1 calc R . . H63C H 0.0710 0.5980 0.2385 0.217 Uiso 1 calc R . . C70 C 0.4484(2) 0.9204(5) 0.2725(2) 0.0610(11) Uani 1 d . . . C71 C 0.4753(3) 1.0273(6) 0.3017(3) 0.0777(14) Uani 1 d . . . H71 H 0.4536 1.1004 0.2876 0.093 Uiso 1 calc R . . C72 C 0.5352(3) 1.0267(8) 0.3527(3) 0.102(2) Uani 1 d . . . H72 H 0.5533 1.0993 0.3724 0.123 Uiso 1 calc R . . C73 C 0.5668(3) 0.9202(8) 0.3732(3) 0.103(2) Uani 1 d . . . H73 H 0.6069 0.9204 0.4066 0.123 Uiso 1 calc R . . C74 C 0.5407(3) 0.8138(7) 0.3457(3) 0.096(2) Uani 1 d . . . H74 H 0.5624 0.7412 0.3609 0.115 Uiso 1 calc R . . C75 C 0.4817(2) 0.8124(6) 0.2948(3) 0.0771(15) Uani 1 d . . . H75 H 0.4643 0.7391 0.2755 0.093 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.04444(16) 0.04691(18) 0.04513(17) 0.00716(13) 0.00328(12) -0.00301(12) Ru2 0.04123(16) 0.05078(19) 0.05642(19) 0.00836(14) 0.00496(13) -0.00295(13) Ru3 0.04795(17) 0.05043(18) 0.03896(15) 0.00263(13) 0.00526(12) 0.00335(13) P1 0.0452(5) 0.0480(5) 0.0465(5) 0.0089(4) 0.0087(4) 0.0003(4) P2 0.0407(5) 0.0636(7) 0.0517(6) 0.0038(5) 0.0025(4) 0.0015(4) O7 0.156(4) 0.062(2) 0.063(2) -0.0057(18) 0.010(2) 0.004(2) O8 0.105(3) 0.080(2) 0.056(2) 0.0186(17) 0.0113(18) -0.009(2) O9 0.084(2) 0.110(3) 0.064(2) 0.016(2) 0.0121(18) -0.013(2) O10 0.115(3) 0.073(3) 0.091(3) -0.016(2) 0.016(2) -0.027(2) O11 0.093(3) 0.098(3) 0.094(3) -0.039(2) 0.013(2) 0.014(2) O12 0.096(3) 0.135(4) 0.077(3) 0.050(3) 0.008(2) 0.032(3) O13 0.049(2) 0.121(4) 0.136(4) 0.019(3) 0.004(2) -0.015(2) C1 0.051(2) 0.074(3) 0.042(2) -0.0013(19) 0.0041(17) 0.007(2) C2 0.068(3) 0.072(3) 0.045(2) -0.005(2) 0.0151(19) -0.016(2) C3 0.105(5) 0.150(7) 0.058(3) -0.042(4) 0.028(3) -0.048(4) C4 0.049(2) 0.051(2) 0.047(2) 0.0032(17) 0.0076(16) -0.0046(17) C5 0.058(2) 0.055(2) 0.053(2) 0.0064(19) 0.0112(18) -0.0018(19) C6 0.084(3) 0.065(3) 0.068(3) 0.024(2) 0.021(3) -0.002(3) C7 0.079(3) 0.057(3) 0.046(2) 0.009(2) 0.002(2) 0.001(2) C8 0.056(2) 0.058(2) 0.047(2) 0.0026(19) 0.0042(17) -0.0039(19) C9 0.051(2) 0.070(3) 0.059(3) 0.009(2) 0.0026(19) -0.006(2) C10 0.065(3) 0.064(3) 0.057(2) 0.006(2) 0.013(2) -0.009(2) C11 0.057(2) 0.074(3) 0.057(3) -0.008(2) 0.0081(19) 0.005(2) C12 0.067(3) 0.077(3) 0.053(2) 0.012(2) 0.012(2) 0.015(2) C13 0.056(3) 0.073(3) 0.070(3) 0.013(2) 0.004(2) -0.013(2) C20 0.054(2) 0.049(2) 0.047(2) 0.0076(17) 0.0107(16) 0.0084(17) C21 0.065(3) 0.060(3) 0.081(3) 0.021(2) 0.011(2) 0.001(2) C22 0.089(4) 0.064(3) 0.110(5) 0.036(3) 0.011(3) 0.003(3) C23 0.103(5) 0.066(4) 0.108(5) 0.031(3) 0.001(4) 0.016(3) C24 0.076(4) 0.085(4) 0.102(4) 0.014(3) -0.009(3) 0.024(3) C25 0.062(3) 0.063(3) 0.085(3) 0.010(3) 0.007(2) 0.008(2) C31 0.151(7) 0.154(7) 0.049(3) -0.013(4) 0.030(4) -0.041(6) C32 0.260(13) 0.118(7) 0.102(6) -0.046(5) 0.033(7) 0.018(7) C33 0.150(8) 0.249(12) 0.073(4) -0.052(6) 0.020(5) -0.104(8) C40 0.060(3) 0.078(3) 0.053(2) 0.007(2) 0.020(2) 0.002(2) C41 0.151(6) 0.095(5) 0.089(4) -0.026(4) 0.064(4) -0.037(4) C42 0.191(9) 0.137(7) 0.104(6) -0.037(5) 0.089(6) -0.017(6) C43 0.140(7) 0.152(8) 0.090(5) 0.026(5) 0.069(5) 0.029(6) C44 0.166(8) 0.122(6) 0.157(7) 0.073(6) 0.119(7) 0.059(6) C45 0.127(5) 0.082(4) 0.133(6) 0.041(4) 0.092(5) 0.034(4) C50 0.057(3) 0.072(3) 0.059(3) 0.009(2) 0.014(2) 0.002(2) C51 0.070(3) 0.122(5) 0.057(3) 0.007(3) 0.015(2) -0.003(3) C52 0.110(5) 0.175(8) 0.056(3) -0.004(4) 0.029(3) -0.019(5) C53 0.118(6) 0.166(8) 0.076(4) 0.007(5) 0.051(4) 0.001(5) C54 0.081(4) 0.139(6) 0.101(5) 0.021(5) 0.044(4) 0.012(4) C55 0.061(3) 0.097(4) 0.081(4) 0.009(3) 0.021(3) 0.002(3) C61 0.161(7) 0.053(3) 0.094(4) 0.018(3) 0.033(4) 0.001(4) C62 0.149(6) 0.097(5) 0.060(3) 0.012(3) 0.040(4) -0.007(4) C63 0.095(5) 0.166(8) 0.175(9) 0.086(7) 0.036(5) -0.023(5) C70 0.042(2) 0.082(3) 0.055(2) 0.003(2) 0.0014(17) 0.002(2) C71 0.055(3) 0.090(4) 0.080(3) -0.004(3) -0.001(2) -0.008(3) C72 0.067(4) 0.137(6) 0.088(4) -0.019(4) -0.011(3) -0.025(4) C73 0.058(3) 0.164(8) 0.073(4) 0.015(4) -0.013(3) -0.008(4) C74 0.056(3) 0.137(6) 0.084(4) 0.030(4) -0.004(3) 0.017(3) C75 0.050(2) 0.092(4) 0.082(3) 0.002(3) -0.001(2) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C13 1.885(5) . ? Ru1 C8 1.945(4) . ? Ru1 C7 1.953(5) . ? Ru1 C4 2.052(4) . ? Ru1 P1 2.3806(12) . ? Ru1 Ru2 3.1422(5) . ? Ru1 Ru3 3.1467(4) . ? Ru2 C9 1.858(5) . ? Ru2 C10 1.874(5) . ? Ru2 C1 2.261(4) . ? Ru2 P1 2.3480(11) . ? Ru2 P2 2.3510(12) . ? Ru2 Ru3 2.9120(5) . ? Ru3 C12 1.859(5) . ? Ru3 C11 1.889(5) . ? Ru3 C1 2.105(5) . ? Ru3 C4 2.278(4) . ? Ru3 P2 2.3103(12) . ? Ru3 C5 2.436(4) . ? P1 C20 1.828(4) . ? P1 C40 1.834(4) . ? P2 C70 1.824(4) . ? P2 C50 1.825(5) . ? O7 C7 1.126(6) . ? O8 C8 1.129(5) . ? O9 C9 1.142(6) . ? O10 C10 1.133(6) . ? O11 C11 1.140(6) . ? O12 C12 1.138(5) . ? O13 C13 1.129(6) . ? C1 C2 1.177(6) . ? C2 C3 1.496(7) . ? C3 C33 1.448(10) . ? C3 C31 1.486(9) . ? C3 C32 1.633(12) . ? C4 C5 1.226(6) . ? C5 C6 1.487(6) . ? C6 C63 1.514(9) . ? C6 C61 1.524(8) . ? C6 C62 1.528(8) . ? C20 C21 1.376(6) . ? C20 C25 1.388(6) . ? C21 C22 1.382(7) . ? C22 C23 1.347(9) . ? C23 C24 1.371(9) . ? C24 C25 1.374(7) . ? C40 C45 1.342(7) . ? C40 C41 1.388(8) . ? C41 C42 1.396(9) . ? C42 C43 1.351(11) . ? C43 C44 1.326(12) . ? C44 C45 1.397(8) . ? C50 C55 1.379(7) . ? C50 C51 1.379(7) . ? C51 C52 1.374(8) . ? C52 C53 1.355(10) . ? C53 C54 1.349(10) . ? C54 C55 1.386(8) . ? C70 C71 1.372(7) . ? C70 C75 1.389(7) . ? C71 C72 1.399(7) . ? C72 C73 1.354(10) . ? C73 C74 1.351(10) . ? C74 C75 1.387(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 C13 Ru1 C8 92.51(19) . . ? C13 Ru1 C7 95.8(2) . . ? C8 Ru1 C7 88.39(18) . . ? C13 Ru1 C4 93.83(18) . . ? C8 Ru1 C4 172.93(17) . . ? C7 Ru1 C4 87.86(17) . . ? C13 Ru1 P1 93.66(17) . . ? C8 Ru1 P1 87.58(13) . . ? C7 Ru1 P1 169.88(15) . . ? C4 Ru1 P1 95.13(12) . . ? C13 Ru1 Ru2 141.56(17) . . ? C8 Ru1 Ru2 87.70(12) . . ? C7 Ru1 Ru2 122.63(15) . . ? C4 Ru1 Ru2 89.28(11) . . ? P1 Ru1 Ru2 47.91(3) . . ? C13 Ru1 Ru3 140.12(15) . . ? C8 Ru1 Ru3 127.26(13) . . ? C7 Ru1 Ru3 84.03(13) . . ? C4 Ru1 Ru3 46.30(11) . . ? P1 Ru1 Ru3 91.04(3) . . ? Ru2 Ru1 Ru3 55.167(10) . . ? C9 Ru2 C10 88.6(2) . . ? C9 Ru2 C1 164.4(2) . . ? C10 Ru2 C1 103.13(18) . . ? C9 Ru2 P1 97.14(14) . . ? C10 Ru2 P1 104.10(15) . . ? C1 Ru2 P1 89.97(11) . . ? C9 Ru2 P2 91.66(16) . . ? C10 Ru2 P2 108.07(15) . . ? C1 Ru2 P2 75.11(11) . . ? P1 Ru2 P2 146.80(4) . . ? C9 Ru2 Ru3 119.03(16) . . ? C10 Ru2 Ru3 142.20(14) . . ? C1 Ru2 Ru3 45.92(12) . . ? P1 Ru2 Ru3 97.77(3) . . ? P2 Ru2 Ru3 50.72(3) . . ? C9 Ru2 Ru1 86.04(14) . . ? C10 Ru2 Ru1 151.17(15) . . ? C1 Ru2 Ru1 88.30(11) . . ? P1 Ru2 Ru1 48.80(3) . . ? P2 Ru2 Ru1 100.38(3) . . ? Ru3 Ru2 Ru1 62.495(11) . . ? C12 Ru3 C11 89.2(2) . . ? C12 Ru3 C1 89.9(2) . . ? C11 Ru3 C1 176.60(19) . . ? C12 Ru3 C4 121.77(18) . . ? C11 Ru3 C4 94.65(18) . . ? C1 Ru3 C4 88.63(16) . . ? C12 Ru3 P2 96.29(16) . . ? C11 Ru3 P2 97.91(16) . . ? C1 Ru3 P2 78.97(13) . . ? C4 Ru3 P2 140.03(10) . . ? C12 Ru3 C5 91.88(19) . . ? C11 Ru3 C5 94.21(18) . . ? C1 Ru3 C5 89.08(16) . . ? C4 Ru3 C5 29.90(14) . . ? P2 Ru3 C5 165.46(11) . . ? C12 Ru3 Ru2 129.48(17) . . ? C11 Ru3 Ru2 128.41(16) . . ? C1 Ru3 Ru2 50.50(12) . . ? C4 Ru3 Ru2 91.09(10) . . ? P2 Ru3 Ru2 51.97(3) . . ? C5 Ru3 Ru2 113.80(11) . . ? C12 Ru3 Ru1 162.33(16) . . ? C11 Ru3 Ru1 90.93(14) . . ? C1 Ru3 Ru1 91.00(11) . . ? C4 Ru3 Ru1 40.63(10) . . ? P2 Ru3 Ru1 101.20(3) . . ? C5 Ru3 Ru1 70.49(10) . . ? Ru2 Ru3 Ru1 62.338(10) . . ? C20 P1 C40 100.5(2) . . ? C20 P1 Ru2 117.77(14) . . ? C40 P1 Ru2 123.73(16) . . ? C20 P1 Ru1 111.62(14) . . ? C40 P1 Ru1 120.35(18) . . ? Ru2 P1 Ru1 83.28(4) . . ? C70 P2 C50 101.7(2) . . ? C70 P2 Ru3 116.99(16) . . ? C50 P2 Ru3 119.58(17) . . ? C70 P2 Ru2 120.33(17) . . ? C50 P2 Ru2 121.06(16) . . ? Ru3 P2 Ru2 77.32(4) . . ? C2 C1 Ru3 167.2(4) . . ? C2 C1 Ru2 104.1(4) . . ? Ru3 C1 Ru2 83.58(15) . . ? C1 C2 C3 170.7(6) . . ? C33 C3 C31 116.5(7) . . ? C33 C3 C2 111.9(6) . . ? C31 C3 C2 108.1(5) . . ? C33 C3 C32 103.6(8) . . ? C31 C3 C32 107.1(7) . . ? C2 C3 C32 109.3(6) . . ? C5 C4 Ru1 174.0(4) . . ? C5 C4 Ru3 82.2(3) . . ? Ru1 C4 Ru3 93.07(15) . . ? C4 C5 C6 161.7(5) . . ? C4 C5 Ru3 67.9(3) . . ? C6 C5 Ru3 130.2(3) . . ? C5 C6 C63 107.3(5) . . ? C5 C6 C61 111.3(5) . . ? C63 C6 C61 109.8(6) . . ? C5 C6 C62 109.5(4) . . ? C63 C6 C62 109.8(6) . . ? C61 C6 C62 109.1(5) . . ? O7 C7 Ru1 172.3(5) . . ? O8 C8 Ru1 174.7(4) . . ? O9 C9 Ru2 175.5(4) . . ? O10 C10 Ru2 176.9(5) . . ? O11 C11 Ru3 176.0(4) . . ? O12 C12 Ru3 178.6(5) . . ? O13 C13 Ru1 179.4(5) . . ? C21 C20 C25 117.7(4) . . ? C21 C20 P1 121.7(3) . . ? C25 C20 P1 120.6(3) . . ? C20 C21 C22 121.2(5) . . ? C23 C22 C21 120.1(6) . . ? C22 C23 C24 120.3(5) . . ? C23 C24 C25 119.9(5) . . ? C24 C25 C20 120.9(5) . . ? C45 C40 C41 117.5(5) . . ? C45 C40 P1 123.1(4) . . ? C41 C40 P1 119.4(4) . . ? C40 C41 C42 120.6(7) . . ? C43 C42 C41 119.9(8) . . ? C44 C43 C42 119.7(7) . . ? C43 C44 C45 121.2(7) . . ? C40 C45 C44 121.0(7) . . ? C55 C50 C51 117.7(5) . . ? C55 C50 P2 122.8(4) . . ? C51 C50 P2 119.4(4) . . ? C52 C51 C50 120.8(6) . . ? C53 C52 C51 120.7(6) . . ? C54 C53 C52 119.8(6) . . ? C53 C54 C55 120.4(6) . . ? C50 C55 C54 120.6(6) . . ? C71 C70 C75 118.7(4) . . ? C71 C70 P2 122.0(4) . . ? C75 C70 P2 119.3(4) . . ? C70 C71 C72 120.2(6) . . ? C73 C72 C71 119.9(7) . . ? C74 C73 C72 120.9(6) . . ? C73 C74 C75 120.2(6) . . ? C74 C75 C70 120.2(6) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.869 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.081 #===END data_B108626J _journal_coden_Cambridge 186 #======================================================================== # 1. SUBMISSION DETAILS _publ_contact_author 'Dr Paul J Low' _publ_contact_author_address ; Dr Paul J Low Department of Chemistry University of Durham South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email 'P.J.LOW@DURHAM.AC.UK' _publ_requested_journal 'Dalton Transactions' #====================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Acetylide generation and coupling on electron-rich Ru3 clusters ; loop_ _publ_author_name 'Low, P.J.' 'Hayes, T.M.' 'Udachin, K.A.' 'Goeta, A.E.' 'Howard, J.A.K.' 'Enright, J.D.' 'Carty, A.J.' _publ_section_references ; Bruker (1998a). SMART-NT V5.0. Data Collection Software. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Bruker (1998b). SAINT-NT V5.0. Data Reduction Software. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Bruker (1998c). SHELXTL-NT. Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1990) Acta Cryst. A46, 467-473 Sheldrick, G.M. (1998). SADABS. Empirical Absorption Correction Program. University of G\"ottingen, Germany. Sheldrick, G.M. (1997) SHELXL-97. Program for the Refinement of Crystal Structures. University of G\"ottingen, Germany. ; _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998a)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998a)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1 (Bruker, 1998c)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; #================================================================= data_8 _database_code_CSD 172817 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H31 Cl3 O8 P2 Ru3' _chemical_formula_weight 1219.24 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.574(3) _cell_length_b 12.941(3) _cell_length_c 15.380(3) _cell_angle_alpha 88.280(10) _cell_angle_beta 87.370(10) _cell_angle_gamma 71.980(10) _cell_volume 2377.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 870 _cell_measurement_theta_min 12.03 _cell_measurement_theta_max 22.90 _exptl_crystal_description prism _exptl_crystal_colour 'intense yellow' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 1.230 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.636 _exptl_absorpt_correction_T_max 0.855 _exptl_absorpt_process_details 'XPREP in SHELXTL (Bruker, 1998c)' _exptl_special_details ; The data collection nominally covered a full sphere of reciprocal space, by a combination of 4 sets of \w scans each set at different \f angles and each scan (16s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _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 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% 0 _diffrn_reflns_number 31655 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.28 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.991 _reflns_number_total 11684 _reflns_number_gt 10237 _reflns_threshold_expression >2sigma(I) _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^)+(0.0151P)^2^+3.6695P] 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 11684 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.726 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.083 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.003503(13) 0.399094(13) 0.247335(11) 0.01308(4) Uani 1 1 d . . . Ru2 Ru 0.210162(13) 0.287774(13) 0.310836(10) 0.01159(4) Uani 1 1 d . . . Ru3 Ru 0.407940(13) 0.248882(13) 0.124147(10) 0.01240(4) Uani 1 1 d . . . P1 P 0.36336(4) 0.43031(4) 0.18019(3) 0.01263(10) Uani 1 1 d . . . P2 P 0.39346(4) 0.17662(4) 0.27272(3) 0.01257(10) Uani 1 1 d . . . C1 C 0.23231(17) 0.41309(16) 0.22000(13) 0.0125(4) Uani 1 1 d . . . C2 C 0.13162(17) 0.46329(17) 0.27031(13) 0.0143(4) Uani 1 1 d . . . C4 C 0.23408(17) 0.32083(16) 0.16681(13) 0.0127(4) Uani 1 1 d . . . C5 C 0.13615(17) 0.29058(16) 0.17432(13) 0.0133(4) Uani 1 1 d . . . C7 C -0.09125(19) 0.30437(19) 0.24310(15) 0.0212(5) Uani 1 1 d . . . O7 O -0.14848(16) 0.25124(15) 0.23966(14) 0.0340(4) Uani 1 1 d . . . C8 C -0.0562(2) 0.49353(18) 0.15418(16) 0.0214(5) Uani 1 1 d . . . O8 O -0.08807(19) 0.55253(16) 0.09737(14) 0.0403(5) Uani 1 1 d . . . C9 C -0.09174(19) 0.4907(2) 0.33547(16) 0.0240(5) Uani 1 1 d . . . O9 O -0.14784(16) 0.54809(19) 0.38566(13) 0.0420(5) Uani 1 1 d . . . C10 C 0.25828(18) 0.31929(17) 0.41833(14) 0.0170(4) Uani 1 1 d . . . O10 O 0.29247(14) 0.33699(14) 0.48210(11) 0.0262(4) Uani 1 1 d . . . C11 C 0.13778(19) 0.19268(18) 0.36493(14) 0.0188(4) Uani 1 1 d . . . O11 O 0.09305(16) 0.13525(15) 0.39710(12) 0.0292(4) Uani 1 1 d . . . C12 C 0.39455(18) 0.11188(18) 0.08325(14) 0.0180(4) Uani 1 1 d . . . O12 O 0.39006(14) 0.03292(13) 0.05684(11) 0.0240(4) Uani 1 1 d . . . C13 C 0.57149(19) 0.19237(19) 0.12049(14) 0.0205(4) Uani 1 1 d . . . O13 O 0.66551(14) 0.15498(17) 0.12306(12) 0.0326(4) Uani 1 1 d . . . C14 C 0.39318(18) 0.30857(18) 0.00545(14) 0.0184(4) Uani 1 1 d . . . O14 O 0.38642(15) 0.33876(15) -0.06493(11) 0.0283(4) Uani 1 1 d . . . C20 C 0.31249(17) 0.54520(17) 0.10417(13) 0.0152(4) Uani 1 1 d . . . C21 C 0.22486(19) 0.54640(18) 0.05054(14) 0.0188(4) Uani 1 1 d . . . H21 H 0.2020 0.4832 0.0470 0.023 Uiso 1 1 calc R . . C22 C 0.1711(2) 0.63899(19) 0.00262(16) 0.0237(5) Uani 1 1 d . . . H22 H 0.1119 0.6389 -0.0336 0.028 Uiso 1 1 calc R . . C23 C 0.2038(2) 0.7316(2) 0.00751(16) 0.0269(5) Uani 1 1 d . . . H23 H 0.1660 0.7953 -0.0245 0.032 Uiso 1 1 calc R . . C24 C 0.2918(2) 0.7313(2) 0.05914(16) 0.0253(5) Uani 1 1 d . . . H24 H 0.3149 0.7944 0.0617 0.030 Uiso 1 1 calc R . . C25 C 0.34607(19) 0.63853(18) 0.10712(15) 0.0196(4) Uani 1 1 d . . . H25 H 0.4064 0.6386 0.1421 0.024 Uiso 1 1 calc R . . C30 C 0.11995(17) 0.56454(17) 0.31918(15) 0.0165(4) Uani 1 1 d . . . C31 C 0.1038(2) 0.5691(2) 0.41010(15) 0.0234(5) Uani 1 1 d . . . H31 H 0.0975 0.5072 0.4421 0.028 Uiso 1 1 calc R . . C32 C 0.0968(2) 0.6645(2) 0.45374(18) 0.0322(6) Uani 1 1 d . . . H32 H 0.0877 0.6664 0.5154 0.039 Uiso 1 1 calc R . . C33 C 0.1032(2) 0.7558(2) 0.4076(2) 0.0345(6) Uani 1 1 d . . . H33 H 0.1002 0.8198 0.4376 0.041 Uiso 1 1 calc R . . C34 C 0.1140(2) 0.7539(2) 0.3174(2) 0.0298(6) Uani 1 1 d . . . H34 H 0.1151 0.8176 0.2856 0.036 Uiso 1 1 calc R . . C35 C 0.12310(18) 0.65860(18) 0.27308(17) 0.0218(5) Uani 1 1 d . . . H35 H 0.1315 0.6576 0.2114 0.026 Uiso 1 1 calc R . . C40 C 0.44777(18) 0.47543(16) 0.25351(14) 0.0155(4) Uani 1 1 d . . . C41 C 0.40781(19) 0.51613(18) 0.33632(14) 0.0187(4) Uani 1 1 d . . . H41 H 0.3338 0.5209 0.3561 0.022 Uiso 1 1 calc R . . C42 C 0.4773(2) 0.54945(18) 0.38924(16) 0.0228(5) Uani 1 1 d . . . H42 H 0.4508 0.5764 0.4456 0.027 Uiso 1 1 calc R . . C43 C 0.5857(2) 0.54365(19) 0.36025(16) 0.0246(5) Uani 1 1 d . . . H43 H 0.6326 0.5669 0.3967 0.029 Uiso 1 1 calc R . . C44 C 0.62538(19) 0.50378(19) 0.27791(16) 0.0223(5) Uani 1 1 d . . . H44 H 0.6992 0.4999 0.2582 0.027 Uiso 1 1 calc R . . C45 C 0.55649(18) 0.46962(17) 0.22453(15) 0.0184(4) Uani 1 1 d . . . H45 H 0.5834 0.4424 0.1684 0.022 Uiso 1 1 calc R . . C50 C 0.49665(17) 0.18065(16) 0.35259(14) 0.0148(4) Uani 1 1 d . . . C51 C 0.48743(19) 0.13323(17) 0.43518(14) 0.0181(4) Uani 1 1 d . . . H51 H 0.4341 0.0954 0.4454 0.022 Uiso 1 1 calc R . . C52 C 0.5551(2) 0.14108(18) 0.50167(15) 0.0209(4) Uani 1 1 d . . . H52 H 0.5479 0.1088 0.5570 0.025 Uiso 1 1 calc R . . C53 C 0.6339(2) 0.19629(19) 0.48745(15) 0.0223(5) Uani 1 1 d . . . H53 H 0.6796 0.2027 0.5333 0.027 Uiso 1 1 calc R . . C54 C 0.64530(19) 0.24187(18) 0.40586(16) 0.0219(5) Uani 1 1 d . . . H54 H 0.6993 0.2789 0.3958 0.026 Uiso 1 1 calc R . . C55 C 0.57747(18) 0.23337(17) 0.33857(14) 0.0174(4) Uani 1 1 d . . . H55 H 0.5865 0.2638 0.2828 0.021 Uiso 1 1 calc R . . C60 C 0.12680(17) 0.20329(16) 0.11723(13) 0.0140(4) Uani 1 1 d . . . C61 C 0.14152(19) 0.21765(18) 0.02703(14) 0.0187(4) Uani 1 1 d . . . H61 H 0.1549 0.2822 0.0054 0.022 Uiso 1 1 calc R . . C62 C 0.1368(2) 0.1391(2) -0.03105(15) 0.0244(5) Uani 1 1 d . . . H62 H 0.1461 0.1505 -0.0919 0.029 Uiso 1 1 calc R . . C63 C 0.1186(2) 0.0442(2) -0.00008(17) 0.0261(5) Uani 1 1 d . . . H63 H 0.1181 -0.0109 -0.0394 0.031 Uiso 1 1 calc R . . C64 C 0.1009(2) 0.02953(19) 0.08877(17) 0.0238(5) Uani 1 1 d . . . H64 H 0.0869 -0.0350 0.1098 0.029 Uiso 1 1 calc R . . C65 C 0.10364(18) 0.10908(18) 0.14732(15) 0.0186(4) Uani 1 1 d . . . H65 H 0.0897 0.0992 0.2077 0.022 Uiso 1 1 calc R . . C70 C 0.42364(18) 0.02841(16) 0.26693(13) 0.0146(4) Uani 1 1 d . . . C71 C 0.5350(2) -0.03597(19) 0.25166(16) 0.0225(5) Uani 1 1 d . . . H71 H 0.5927 -0.0028 0.2474 0.027 Uiso 1 1 calc R . . C72 C 0.5618(2) -0.1478(2) 0.24275(17) 0.0278(5) Uani 1 1 d . . . H72 H 0.6374 -0.1906 0.2325 0.033 Uiso 1 1 calc R . . C73 C 0.4779(2) -0.19658(19) 0.24881(16) 0.0267(5) Uani 1 1 d . . . H73 H 0.4962 -0.2730 0.2429 0.032 Uiso 1 1 calc R . . C74 C 0.3677(2) -0.13423(19) 0.26347(16) 0.0254(5) Uani 1 1 d . . . H74 H 0.3103 -0.1679 0.2672 0.030 Uiso 1 1 calc R . . C75 C 0.34051(19) -0.02186(18) 0.27277(15) 0.0199(4) Uani 1 1 d . . . H75 H 0.2647 0.0205 0.2831 0.024 Uiso 1 1 calc R . . C100 C -0.1960(2) -0.0238(2) 0.35977(16) 0.0259(5) Uani 1 1 d . . . H100 H -0.2707 0.0328 0.3670 0.031 Uiso 1 1 calc R . . Cl1 Cl -0.09776(6) 0.01993(5) 0.41425(5) 0.03340(14) Uani 1 1 d . . . Cl2 Cl -0.20814(7) -0.14700(6) 0.40305(5) 0.04343(17) Uani 1 1 d . . . Cl3 Cl -0.15949(6) -0.03520(6) 0.24773(4) 0.03937(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01080(7) 0.01539(8) 0.01256(8) -0.00118(6) -0.00024(6) -0.00326(6) Ru2 0.01177(7) 0.01317(7) 0.00961(7) -0.00072(5) -0.00021(5) -0.00349(6) Ru3 0.01205(8) 0.01427(8) 0.01039(8) -0.00131(6) 0.00043(6) -0.00335(6) P1 0.0124(2) 0.0142(2) 0.0120(2) -0.00013(18) -0.00125(18) -0.00509(19) P2 0.0128(2) 0.0123(2) 0.0121(2) -0.00067(18) -0.00095(18) -0.00298(18) C1 0.0123(9) 0.0117(9) 0.0139(9) -0.0003(7) -0.0021(7) -0.0041(7) C2 0.0137(9) 0.0150(9) 0.0135(9) -0.0008(7) -0.0019(7) -0.0030(7) C4 0.0125(9) 0.0159(9) 0.0086(9) 0.0013(7) -0.0015(7) -0.0031(7) C5 0.0135(9) 0.0134(9) 0.0128(9) -0.0014(7) -0.0016(7) -0.0035(7) C7 0.0165(10) 0.0213(11) 0.0237(12) -0.0003(9) 0.0011(9) -0.0031(8) O7 0.0259(9) 0.0306(10) 0.0510(12) -0.0031(9) 0.0032(8) -0.0170(8) C8 0.0221(11) 0.0195(11) 0.0240(12) -0.0008(9) -0.0060(9) -0.0078(9) O8 0.0535(13) 0.0333(10) 0.0376(11) 0.0154(9) -0.0238(10) -0.0166(9) C9 0.0170(11) 0.0334(13) 0.0220(12) -0.0056(10) -0.0019(9) -0.0075(9) O9 0.0242(10) 0.0619(14) 0.0364(11) -0.0267(10) 0.0080(8) -0.0070(9) C10 0.0145(10) 0.0177(10) 0.0152(10) -0.0022(8) 0.0036(8) -0.0001(8) O10 0.0255(9) 0.0302(9) 0.0172(8) -0.0093(7) -0.0061(7) 0.0012(7) C11 0.0194(10) 0.0223(11) 0.0146(10) 0.0000(8) -0.0012(8) -0.0064(8) O11 0.0330(10) 0.0338(10) 0.0264(9) 0.0062(7) 0.0007(7) -0.0194(8) C12 0.0164(10) 0.0208(11) 0.0144(10) -0.0027(8) 0.0014(8) -0.0026(8) O12 0.0267(9) 0.0203(8) 0.0241(9) -0.0072(7) -0.0009(7) -0.0052(7) C13 0.0211(11) 0.0245(11) 0.0145(10) 0.0000(8) 0.0021(8) -0.0053(9) O13 0.0163(8) 0.0472(11) 0.0278(10) 0.0069(8) 0.0010(7) -0.0015(8) C14 0.0177(10) 0.0195(10) 0.0178(11) -0.0030(8) 0.0000(8) -0.0053(8) O14 0.0324(10) 0.0351(10) 0.0154(8) 0.0030(7) 0.0002(7) -0.0079(8) C20 0.0161(10) 0.0167(10) 0.0127(9) 0.0006(7) 0.0000(8) -0.0048(8) C21 0.0211(11) 0.0182(10) 0.0179(10) 0.0007(8) -0.0039(8) -0.0071(8) C22 0.0259(12) 0.0247(12) 0.0202(11) 0.0037(9) -0.0092(9) -0.0067(9) C23 0.0341(14) 0.0205(11) 0.0255(12) 0.0065(9) -0.0084(10) -0.0070(10) C24 0.0339(13) 0.0211(11) 0.0252(12) 0.0033(9) -0.0034(10) -0.0147(10) C25 0.0213(11) 0.0212(11) 0.0185(11) 0.0018(8) -0.0023(8) -0.0098(9) C30 0.0103(9) 0.0157(10) 0.0225(11) -0.0057(8) -0.0020(8) -0.0018(7) C31 0.0214(11) 0.0228(11) 0.0211(11) -0.0062(9) -0.0051(9) 0.0014(9) C32 0.0297(13) 0.0304(13) 0.0287(13) -0.0165(11) -0.0074(10) 0.0045(10) C33 0.0263(13) 0.0239(13) 0.0502(17) -0.0209(12) -0.0099(12) -0.0001(10) C34 0.0209(12) 0.0173(11) 0.0508(17) -0.0062(11) -0.0011(11) -0.0048(9) C35 0.0147(10) 0.0195(11) 0.0303(12) -0.0030(9) 0.0003(9) -0.0039(8) C40 0.0164(10) 0.0135(9) 0.0177(10) 0.0007(8) -0.0050(8) -0.0057(8) C41 0.0187(10) 0.0186(10) 0.0181(11) -0.0009(8) -0.0037(8) -0.0043(8) C42 0.0270(12) 0.0192(11) 0.0205(11) -0.0041(9) -0.0065(9) -0.0037(9) C43 0.0265(12) 0.0208(11) 0.0271(12) -0.0008(9) -0.0120(10) -0.0069(9) C44 0.0161(10) 0.0207(11) 0.0310(13) 0.0011(9) -0.0055(9) -0.0066(8) C45 0.0178(10) 0.0173(10) 0.0200(11) 0.0000(8) -0.0025(8) -0.0051(8) C50 0.0144(9) 0.0126(9) 0.0151(10) -0.0020(7) -0.0025(7) -0.0007(7) C51 0.0195(10) 0.0169(10) 0.0178(10) 0.0002(8) -0.0015(8) -0.0052(8) C52 0.0251(11) 0.0213(11) 0.0139(10) 0.0000(8) -0.0038(8) -0.0034(9) C53 0.0223(11) 0.0219(11) 0.0212(11) -0.0049(9) -0.0090(9) -0.0033(9) C54 0.0180(11) 0.0197(11) 0.0284(12) -0.0013(9) -0.0038(9) -0.0058(8) C55 0.0165(10) 0.0172(10) 0.0172(10) -0.0004(8) -0.0021(8) -0.0028(8) C60 0.0116(9) 0.0152(9) 0.0152(10) -0.0011(7) -0.0033(7) -0.0038(7) C61 0.0195(10) 0.0205(10) 0.0169(10) -0.0012(8) -0.0021(8) -0.0070(8) C62 0.0277(12) 0.0313(13) 0.0148(11) -0.0066(9) -0.0017(9) -0.0092(10) C63 0.0256(12) 0.0245(12) 0.0292(13) -0.0116(10) -0.0054(10) -0.0074(9) C64 0.0250(12) 0.0160(10) 0.0325(13) -0.0026(9) -0.0077(10) -0.0086(9) C65 0.0181(10) 0.0185(10) 0.0203(11) -0.0002(8) -0.0039(8) -0.0070(8) C70 0.0190(10) 0.0124(9) 0.0124(9) -0.0003(7) -0.0032(8) -0.0042(8) C71 0.0212(11) 0.0193(11) 0.0266(12) -0.0030(9) -0.0019(9) -0.0054(9) C72 0.0260(12) 0.0199(11) 0.0326(14) -0.0067(10) -0.0052(10) 0.0014(9) C73 0.0398(14) 0.0132(10) 0.0262(12) -0.0021(9) -0.0096(10) -0.0058(9) C74 0.0310(13) 0.0211(11) 0.0273(12) -0.0009(9) -0.0065(10) -0.0119(10) C75 0.0216(11) 0.0200(11) 0.0196(11) -0.0005(8) -0.0051(9) -0.0079(9) C100 0.0259(12) 0.0275(12) 0.0232(12) -0.0036(9) -0.0053(9) -0.0057(10) Cl1 0.0305(3) 0.0287(3) 0.0404(4) -0.0071(3) -0.0119(3) -0.0063(2) Cl2 0.0501(4) 0.0449(4) 0.0437(4) 0.0139(3) -0.0161(3) -0.0263(3) Cl3 0.0423(4) 0.0506(4) 0.0231(3) -0.0017(3) -0.0017(3) -0.0111(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C8 1.880(2) . ? Ru1 C9 1.936(2) . ? Ru1 C7 1.960(2) . ? Ru1 C2 2.076(2) . ? Ru1 C5 2.119(2) . ? Ru1 Ru2 2.7593(6) . ? Ru2 C10 1.884(2) . ? Ru2 C11 1.897(2) . ? Ru2 C1 2.183(2) . ? Ru2 C2 2.260(2) . ? Ru2 C4 2.268(2) . ? Ru2 C5 2.330(2) . ? Ru2 P2 2.3665(7) . ? Ru3 C14 1.955(2) . ? Ru3 C13 1.957(2) . ? Ru3 C12 1.957(2) . ? Ru3 C4 2.173(2) . ? Ru3 P1 2.4150(8) . ? Ru3 P2 2.4633(7) . ? P1 C1 1.807(2) . ? P1 C40 1.809(2) . ? P1 C20 1.834(2) . ? P2 C50 1.840(2) . ? P2 C70 1.841(2) . ? C1 C2 1.433(3) . ? C1 C4 1.461(3) . ? C2 C30 1.494(3) . ? C4 C5 1.402(3) . ? C5 C60 1.487(3) . ? C7 O7 1.142(3) . ? C8 O8 1.145(3) . ? C9 O9 1.143(3) . ? C10 O10 1.146(3) . ? C11 O11 1.151(3) . ? C12 O12 1.129(3) . ? C13 O13 1.132(3) . ? C14 O14 1.138(3) . ? C20 C25 1.400(3) . ? C20 C21 1.402(3) . ? C21 C22 1.388(3) . ? C21 H21 0.9500 . ? C22 C23 1.387(3) . ? C22 H22 0.9500 . ? C23 C24 1.390(4) . ? C23 H23 0.9500 . ? C24 C25 1.392(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C30 C35 1.400(3) . ? C30 C31 1.404(3) . ? C31 C32 1.399(3) . ? C31 H31 0.9500 . ? C32 C33 1.382(4) . ? C32 H32 0.9500 . ? C33 C34 1.387(4) . ? C33 H33 0.9500 . ? C34 C35 1.398(3) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C40 C45 1.399(3) . ? C40 C41 1.404(3) . ? C41 C42 1.390(3) . ? C41 H41 0.9500 . ? C42 C43 1.395(4) . ? C42 H42 0.9500 . ? C43 C44 1.393(3) . ? C43 H43 0.9500 . ? C44 C45 1.394(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C50 C55 1.395(3) . ? C50 C51 1.410(3) . ? C51 C52 1.386(3) . ? C51 H51 0.9500 . ? C52 C53 1.396(3) . ? C52 H52 0.9500 . ? C53 C54 1.391(3) . ? C53 H53 0.9500 . ? C54 C55 1.399(3) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C60 C65 1.400(3) . ? C60 C61 1.406(3) . ? C61 C62 1.389(3) . ? C61 H61 0.9500 . ? C62 C63 1.385(4) . ? C62 H62 0.9500 . ? C63 C64 1.391(4) . ? C63 H63 0.9500 . ? C64 C65 1.397(3) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C70 C75 1.390(3) . ? C70 C71 1.404(3) . ? C71 C72 1.390(3) . ? C71 H71 0.9500 . ? C72 C73 1.385(4) . ? C72 H72 0.9500 . ? C73 C74 1.383(4) . ? C73 H73 0.9500 . ? C74 C75 1.397(3) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C100 Cl2 1.757(3) . ? C100 Cl3 1.762(3) . ? C100 Cl1 1.762(3) . ? C100 H100 1.0000 . ? 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 C8 Ru1 C9 94.60(11) . . ? C8 Ru1 C7 98.52(10) . . ? C9 Ru1 C7 93.33(10) . . ? C8 Ru1 C2 96.23(9) . . ? C9 Ru1 C2 90.79(9) . . ? C7 Ru1 C2 164.30(9) . . ? C8 Ru1 C5 96.54(9) . . ? C9 Ru1 C5 166.31(9) . . ? C7 Ru1 C5 92.86(9) . . ? C2 Ru1 C5 80.13(8) . . ? C8 Ru1 Ru2 138.72(7) . . ? C9 Ru1 Ru2 111.13(7) . . ? C7 Ru1 Ru2 111.05(7) . . ? C2 Ru1 Ru2 53.49(6) . . ? C5 Ru1 Ru2 55.20(6) . . ? C10 Ru2 C11 91.91(10) . . ? C10 Ru2 C1 105.44(9) . . ? C11 Ru2 C1 157.04(9) . . ? C10 Ru2 C2 95.23(8) . . ? C11 Ru2 C2 127.52(9) . . ? C1 Ru2 C2 37.59(7) . . ? C10 Ru2 C4 139.16(9) . . ? C11 Ru2 C4 128.57(9) . . ? C1 Ru2 C4 38.28(7) . . ? C2 Ru2 C4 66.19(7) . . ? C10 Ru2 C5 167.27(8) . . ? C11 Ru2 C5 96.10(9) . . ? C1 Ru2 C5 64.40(7) . . ? C2 Ru2 C5 72.04(7) . . ? C4 Ru2 C5 35.47(7) . . ? C10 Ru2 P2 90.77(6) . . ? C11 Ru2 P2 105.37(7) . . ? C1 Ru2 P2 89.59(6) . . ? C2 Ru2 P2 126.37(6) . . ? C4 Ru2 P2 74.95(5) . . ? C5 Ru2 P2 96.59(5) . . ? C10 Ru2 Ru1 122.88(6) . . ? C11 Ru2 Ru1 85.87(7) . . ? C1 Ru2 Ru1 72.18(5) . . ? C2 Ru2 Ru1 47.58(5) . . ? C4 Ru2 Ru1 72.03(5) . . ? C5 Ru2 Ru1 48.30(5) . . ? P2 Ru2 Ru1 144.587(18) . . ? C14 Ru3 C13 96.66(9) . . ? C14 Ru3 C12 90.40(9) . . ? C13 Ru3 C12 92.19(9) . . ? C14 Ru3 C4 96.86(8) . . ? C13 Ru3 C4 163.41(8) . . ? C12 Ru3 C4 97.29(8) . . ? C14 Ru3 P1 89.92(7) . . ? C13 Ru3 P1 105.19(7) . . ? C12 Ru3 P1 162.46(6) . . ? C4 Ru3 P1 65.28(6) . . ? C14 Ru3 P2 170.53(7) . . ? C13 Ru3 P2 92.44(7) . . ? C12 Ru3 P2 86.63(7) . . ? C4 Ru3 P2 74.65(5) . . ? P1 Ru3 P2 90.22(2) . . ? C1 P1 C40 119.54(10) . . ? C1 P1 C20 100.45(10) . . ? C40 P1 C20 104.26(10) . . ? C1 P1 Ru3 86.41(7) . . ? C40 P1 Ru3 125.31(7) . . ? C20 P1 Ru3 118.01(7) . . ? C50 P2 C70 99.10(9) . . ? C50 P2 Ru2 112.92(7) . . ? C70 P2 Ru2 119.84(7) . . ? C50 P2 Ru3 119.59(7) . . ? C70 P2 Ru3 108.40(7) . . ? Ru2 P2 Ru3 98.24(2) . . ? C2 C1 C4 117.28(18) . . ? C2 C1 P1 143.55(16) . . ? C4 C1 P1 98.31(13) . . ? C2 C1 Ru2 74.10(12) . . ? C4 C1 Ru2 73.98(11) . . ? P1 C1 Ru2 126.89(10) . . ? C1 C2 C30 120.04(18) . . ? C1 C2 Ru1 113.05(14) . . ? C30 C2 Ru1 125.89(14) . . ? C1 C2 Ru2 68.31(11) . . ? C30 C2 Ru2 129.45(15) . . ? Ru1 C2 Ru2 78.93(7) . . ? C5 C4 C1 114.49(17) . . ? C5 C4 Ru3 137.89(15) . . ? C1 C4 Ru3 105.47(13) . . ? C5 C4 Ru2 74.70(12) . . ? C1 C4 Ru2 67.74(11) . . ? Ru3 C4 Ru2 110.65(8) . . ? C4 C5 C60 118.21(18) . . ? C4 C5 Ru1 114.26(14) . . ? C60 C5 Ru1 126.14(14) . . ? C4 C5 Ru2 69.82(11) . . ? C60 C5 Ru2 132.81(14) . . ? Ru1 C5 Ru2 76.50(7) . . ? O7 C7 Ru1 178.3(2) . . ? O8 C8 Ru1 176.8(2) . . ? O9 C9 Ru1 177.4(3) . . ? O10 C10 Ru2 176.85(19) . . ? O11 C11 Ru2 179.3(2) . . ? O12 C12 Ru3 177.0(2) . . ? O13 C13 Ru3 175.2(2) . . ? O14 C14 Ru3 177.0(2) . . ? C25 C20 C21 118.7(2) . . ? C25 C20 P1 122.08(17) . . ? C21 C20 P1 118.54(16) . . ? C22 C21 C20 120.6(2) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.1(2) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 120.1(2) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C20 120.5(2) . . ? C24 C25 H25 119.8 . . ? C20 C25 H25 119.8 . . ? C35 C30 C31 118.7(2) . . ? C35 C30 C2 119.2(2) . . ? C31 C30 C2 122.1(2) . . ? C32 C31 C30 120.3(2) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C33 C32 C31 120.3(2) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 120.0(2) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C35 120.3(3) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C30 120.3(2) . . ? C34 C35 H35 119.8 . . ? C30 C35 H35 119.8 . . ? C45 C40 C41 119.9(2) . . ? C45 C40 P1 117.43(16) . . ? C41 C40 P1 122.63(17) . . ? C42 C41 C40 119.5(2) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C41 C42 C43 120.5(2) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 120.1(2) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 119.9(2) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C44 C45 C40 120.1(2) . . ? C44 C45 H45 119.9 . . ? C40 C45 H45 119.9 . . ? C55 C50 C51 118.5(2) . . ? C55 C50 P2 124.37(17) . . ? C51 C50 P2 117.01(16) . . ? C52 C51 C50 120.9(2) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C51 C52 C53 120.1(2) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C54 C53 C52 119.7(2) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C53 C54 C55 120.2(2) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? C50 C55 C54 120.6(2) . . ? C50 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? C65 C60 C61 118.31(19) . . ? C65 C60 C5 124.43(19) . . ? C61 C60 C5 117.26(19) . . ? C62 C61 C60 121.2(2) . . ? C62 C61 H61 119.4 . . ? C60 C61 H61 119.4 . . ? C63 C62 C61 119.8(2) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 119.9(2) . . ? C62 C63 H63 120.1 . . ? C64 C63 H63 120.1 . . ? C63 C64 C65 120.5(2) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? C64 C65 C60 120.2(2) . . ? C64 C65 H65 119.9 . . ? C60 C65 H65 119.9 . . ? C75 C70 C71 118.7(2) . . ? C75 C70 P2 122.89(16) . . ? C71 C70 P2 118.37(17) . . ? C72 C71 C70 120.7(2) . . ? C72 C71 H71 119.6 . . ? C70 C71 H71 119.6 . . ? C73 C72 C71 119.9(2) . . ? C73 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C74 C73 C72 120.1(2) . . ? C74 C73 H73 119.9 . . ? C72 C73 H73 119.9 . . ? C73 C74 C75 120.2(2) . . ? C73 C74 H74 119.9 . . ? C75 C74 H74 119.9 . . ? C70 C75 C74 120.4(2) . . ? C70 C75 H75 119.8 . . ? C74 C75 H75 119.8 . . ? Cl2 C100 Cl3 110.74(14) . . ? Cl2 C100 Cl1 112.12(14) . . ? Cl3 C100 Cl1 109.75(15) . . ? Cl2 C100 H100 108.0 . . ? Cl3 C100 H100 108.0 . . ? Cl1 C100 H100 108.0 . . ? 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 C8 Ru1 Ru2 C10 114.00(13) . . . . ? C9 Ru1 Ru2 C10 -10.80(12) . . . . ? C7 Ru1 Ru2 C10 -113.24(11) . . . . ? C2 Ru1 Ru2 C10 63.68(11) . . . . ? C5 Ru1 Ru2 C10 168.44(11) . . . . ? C8 Ru1 Ru2 C11 -156.40(12) . . . . ? C9 Ru1 Ru2 C11 78.81(11) . . . . ? C7 Ru1 Ru2 C11 -23.63(10) . . . . ? C2 Ru1 Ru2 C11 153.28(10) . . . . ? C5 Ru1 Ru2 C11 -101.95(10) . . . . ? C8 Ru1 Ru2 C1 16.80(12) . . . . ? C9 Ru1 Ru2 C1 -107.99(10) . . . . ? C7 Ru1 Ru2 C1 149.57(9) . . . . ? C2 Ru1 Ru2 C1 -33.52(9) . . . . ? C5 Ru1 Ru2 C1 71.24(9) . . . . ? C8 Ru1 Ru2 C2 50.32(13) . . . . ? C9 Ru1 Ru2 C2 -74.47(11) . . . . ? C7 Ru1 Ru2 C2 -176.91(10) . . . . ? C5 Ru1 Ru2 C2 104.77(10) . . . . ? C8 Ru1 Ru2 C4 -23.50(12) . . . . ? C9 Ru1 Ru2 C4 -148.30(10) . . . . ? C7 Ru1 Ru2 C4 109.26(9) . . . . ? C2 Ru1 Ru2 C4 -73.82(9) . . . . ? C5 Ru1 Ru2 C4 30.94(9) . . . . ? C8 Ru1 Ru2 C5 -54.45(13) . . . . ? C9 Ru1 Ru2 C5 -179.24(11) . . . . ? C7 Ru1 Ru2 C5 78.32(10) . . . . ? C2 Ru1 Ru2 C5 -104.77(10) . . . . ? C8 Ru1 Ru2 P2 -45.48(11) . . . . ? C9 Ru1 Ru2 P2 -170.27(9) . . . . ? C7 Ru1 Ru2 P2 87.29(8) . . . . ? C2 Ru1 Ru2 P2 -95.80(8) . . . . ? C5 Ru1 Ru2 P2 8.96(7) . . . . ? C14 Ru3 P1 C1 109.99(9) . . . . ? C13 Ru3 P1 C1 -153.13(9) . . . . ? C12 Ru3 P1 C1 18.9(2) . . . . ? C4 Ru3 P1 C1 12.40(9) . . . . ? P2 Ru3 P1 C1 -60.54(7) . . . . ? C14 Ru3 P1 C40 -125.89(11) . . . . ? C13 Ru3 P1 C40 -29.01(11) . . . . ? C12 Ru3 P1 C40 143.0(2) . . . . ? C4 Ru3 P1 C40 136.52(11) . . . . ? P2 Ru3 P1 C40 63.58(9) . . . . ? C14 Ru3 P1 C20 10.06(10) . . . . ? C13 Ru3 P1 C20 106.94(10) . . . . ? C12 Ru3 P1 C20 -81.0(2) . . . . ? C4 Ru3 P1 C20 -87.53(10) . . . . ? P2 Ru3 P1 C20 -160.48(8) . . . . ? C10 Ru2 P2 C50 -5.54(10) . . . . ? C11 Ru2 P2 C50 -97.74(10) . . . . ? C1 Ru2 P2 C50 99.90(9) . . . . ? C2 Ru2 P2 C50 91.53(10) . . . . ? C4 Ru2 P2 C50 135.70(9) . . . . ? C5 Ru2 P2 C50 164.06(9) . . . . ? Ru1 Ru2 P2 C50 157.33(7) . . . . ? C10 Ru2 P2 C70 110.59(10) . . . . ? C11 Ru2 P2 C70 18.39(11) . . . . ? C1 Ru2 P2 C70 -143.97(9) . . . . ? C2 Ru2 P2 C70 -152.34(10) . . . . ? C4 Ru2 P2 C70 -108.17(10) . . . . ? C5 Ru2 P2 C70 -79.81(9) . . . . ? Ru1 Ru2 P2 C70 -86.54(8) . . . . ? C10 Ru2 P2 Ru3 -132.63(7) . . . . ? C11 Ru2 P2 Ru3 135.18(7) . . . . ? C1 Ru2 P2 Ru3 -27.19(5) . . . . ? C2 Ru2 P2 Ru3 -35.55(7) . . . . ? C4 Ru2 P2 Ru3 8.62(5) . . . . ? C5 Ru2 P2 Ru3 36.97(5) . . . . ? Ru1 Ru2 P2 Ru3 30.25(3) . . . . ? C14 Ru3 P2 C50 -158.0(4) . . . . ? C13 Ru3 P2 C50 38.10(10) . . . . ? C12 Ru3 P2 C50 130.15(10) . . . . ? C4 Ru3 P2 C50 -131.34(9) . . . . ? P1 Ru3 P2 C50 -67.11(8) . . . . ? C14 Ru3 P2 C70 89.7(4) . . . . ? C13 Ru3 P2 C70 -74.26(10) . . . . ? C12 Ru3 P2 C70 17.79(10) . . . . ? C4 Ru3 P2 C70 116.30(9) . . . . ? P1 Ru3 P2 C70 -179.47(7) . . . . ? C14 Ru3 P2 Ru2 -35.6(4) . . . . ? C13 Ru3 P2 Ru2 160.43(7) . . . . ? C12 Ru3 P2 Ru2 -107.52(7) . . . . ? C4 Ru3 P2 Ru2 -9.01(6) . . . . ? P1 Ru3 P2 Ru2 55.22(2) . . . . ? C40 P1 C1 C2 46.1(3) . . . . ? C20 P1 C1 C2 -67.0(3) . . . . ? Ru3 P1 C1 C2 175.2(3) . . . . ? C40 P1 C1 C4 -146.11(13) . . . . ? C20 P1 C1 C4 100.79(14) . . . . ? Ru3 P1 C1 C4 -17.05(12) . . . . ? C40 P1 C1 Ru2 -69.95(15) . . . . ? C20 P1 C1 Ru2 176.95(12) . . . . ? Ru3 P1 C1 Ru2 59.11(11) . . . . ? C10 Ru2 C1 C2 -78.25(13) . . . . ? C11 Ru2 C1 C2 59.6(3) . . . . ? C4 Ru2 C1 C2 125.28(17) . . . . ? C5 Ru2 C1 C2 93.56(13) . . . . ? P2 Ru2 C1 C2 -168.93(11) . . . . ? Ru1 Ru2 C1 C2 41.93(10) . . . . ? C10 Ru2 C1 C4 156.47(12) . . . . ? C11 Ru2 C1 C4 -65.7(2) . . . . ? C2 Ru2 C1 C4 -125.28(17) . . . . ? C5 Ru2 C1 C4 -31.73(11) . . . . ? P2 Ru2 C1 C4 65.79(11) . . . . ? Ru1 Ru2 C1 C4 -83.35(11) . . . . ? C10 Ru2 C1 P1 68.05(14) . . . . ? C11 Ru2 C1 P1 -154.13(18) . . . . ? C2 Ru2 C1 P1 146.3(2) . . . . ? C4 Ru2 C1 P1 -88.42(16) . . . . ? C5 Ru2 C1 P1 -120.14(14) . . . . ? P2 Ru2 C1 P1 -22.63(12) . . . . ? Ru1 Ru2 C1 P1 -171.77(13) . . . . ? C4 C1 C2 C30 -173.97(18) . . . . ? P1 C1 C2 C30 -7.6(4) . . . . ? Ru2 C1 C2 C30 124.05(19) . . . . ? C4 C1 C2 Ru1 -4.8(2) . . . . ? P1 C1 C2 Ru1 161.52(19) . . . . ? Ru2 C1 C2 Ru1 -66.81(11) . . . . ? C4 C1 C2 Ru2 61.98(16) . . . . ? P1 C1 C2 Ru2 -131.7(3) . . . . ? C8 Ru1 C2 C1 -88.79(16) . . . . ? C9 Ru1 C2 C1 176.49(16) . . . . ? C7 Ru1 C2 C1 71.2(4) . . . . ? C5 Ru1 C2 C1 6.79(15) . . . . ? Ru2 Ru1 C2 C1 60.49(13) . . . . ? C8 Ru1 C2 C30 79.59(19) . . . . ? C9 Ru1 C2 C30 -15.12(19) . . . . ? C7 Ru1 C2 C30 -120.4(3) . . . . ? C5 Ru1 C2 C30 175.18(19) . . . . ? Ru2 Ru1 C2 C30 -131.1(2) . . . . ? C8 Ru1 C2 Ru2 -149.29(8) . . . . ? C9 Ru1 C2 Ru2 116.00(9) . . . . ? C7 Ru1 C2 Ru2 10.7(3) . . . . ? C5 Ru1 C2 Ru2 -53.70(7) . . . . ? C10 Ru2 C2 C1 108.62(13) . . . . ? C11 Ru2 C2 C1 -154.91(13) . . . . ? C4 Ru2 C2 C1 -33.55(11) . . . . ? C5 Ru2 C2 C1 -71.11(12) . . . . ? P2 Ru2 C2 C1 13.80(14) . . . . ? Ru1 Ru2 C2 C1 -120.48(13) . . . . ? C10 Ru2 C2 C30 -3.11(19) . . . . ? C11 Ru2 C2 C30 93.4(2) . . . . ? C1 Ru2 C2 C30 -111.7(2) . . . . ? C4 Ru2 C2 C30 -145.3(2) . . . . ? C5 Ru2 C2 C30 177.2(2) . . . . ? P2 Ru2 C2 C30 -97.94(18) . . . . ? Ru1 Ru2 C2 C30 127.8(2) . . . . ? C10 Ru2 C2 Ru1 -130.89(8) . . . . ? C11 Ru2 C2 Ru1 -34.43(12) . . . . ? C1 Ru2 C2 Ru1 120.48(13) . . . . ? C4 Ru2 C2 Ru1 86.93(8) . . . . ? C5 Ru2 C2 Ru1 49.37(7) . . . . ? P2 Ru2 C2 Ru1 134.28(4) . . . . ? C2 C1 C4 C5 -2.0(3) . . . . ? P1 C1 C4 C5 -173.87(15) . . . . ? Ru2 C1 C4 C5 60.02(16) . . . . ? C2 C1 C4 Ru3 -168.43(15) . . . . ? P1 C1 C4 Ru3 19.72(13) . . . . ? Ru2 C1 C4 Ru3 -106.39(9) . . . . ? C2 C1 C4 Ru2 -62.04(16) . . . . ? P1 C1 C4 Ru2 126.11(10) . . . . ? C14 Ru3 C4 C5 95.9(2) . . . . ? C13 Ru3 C4 C5 -119.7(3) . . . . ? C12 Ru3 C4 C5 4.6(2) . . . . ? P1 Ru3 C4 C5 -177.4(2) . . . . ? P2 Ru3 C4 C5 -79.8(2) . . . . ? C14 Ru3 C4 C1 -102.71(14) . . . . ? C13 Ru3 C4 C1 41.7(4) . . . . ? C12 Ru3 C4 C1 166.01(14) . . . . ? P1 Ru3 C4 C1 -15.97(11) . . . . ? P2 Ru3 C4 C1 81.55(13) . . . . ? C14 Ru3 C4 Ru2 -174.31(9) . . . . ? C13 Ru3 C4 Ru2 -29.9(3) . . . . ? C12 Ru3 C4 Ru2 94.41(10) . . . . ? P1 Ru3 C4 Ru2 -87.57(8) . . . . ? P2 Ru3 C4 Ru2 9.95(6) . . . . ? C10 Ru2 C4 C5 -161.24(13) . . . . ? C11 Ru2 C4 C5 27.76(16) . . . . ? C1 Ru2 C4 C5 -125.20(17) . . . . ? C2 Ru2 C4 C5 -92.22(13) . . . . ? P2 Ru2 C4 C5 125.61(12) . . . . ? Ru1 Ru2 C4 C5 -41.41(10) . . . . ? C10 Ru2 C4 C1 -36.04(17) . . . . ? C11 Ru2 C4 C1 152.95(13) . . . . ? C2 Ru2 C4 C1 32.98(11) . . . . ? C5 Ru2 C4 C1 125.20(17) . . . . ? P2 Ru2 C4 C1 -109.19(11) . . . . ? Ru1 Ru2 C4 C1 83.78(11) . . . . ? C10 Ru2 C4 Ru3 62.80(15) . . . . ? C11 Ru2 C4 Ru3 -108.20(12) . . . . ? C1 Ru2 C4 Ru3 98.84(14) . . . . ? C2 Ru2 C4 Ru3 131.82(11) . . . . ? C5 Ru2 C4 Ru3 -135.96(16) . . . . ? P2 Ru2 C4 Ru3 -10.35(6) . . . . ? Ru1 Ru2 C4 Ru3 -177.37(9) . . . . ? C1 C4 C5 C60 175.15(17) . . . . ? Ru3 C4 C5 C60 -24.6(3) . . . . ? Ru2 C4 C5 C60 -128.64(18) . . . . ? C1 C4 C5 Ru1 7.8(2) . . . . ? Ru3 C4 C5 Ru1 168.04(13) . . . . ? Ru2 C4 C5 Ru1 64.01(11) . . . . ? C1 C4 C5 Ru2 -56.21(15) . . . . ? Ru3 C4 C5 Ru2 104.0(2) . . . . ? C8 Ru1 C5 C4 87.12(16) . . . . ? C9 Ru1 C5 C4 -57.2(5) . . . . ? C7 Ru1 C5 C4 -173.96(16) . . . . ? C2 Ru1 C5 C4 -8.11(15) . . . . ? Ru2 Ru1 C5 C4 -60.19(14) . . . . ? C8 Ru1 C5 C60 -79.07(19) . . . . ? C9 Ru1 C5 C60 136.6(4) . . . . ? C7 Ru1 C5 C60 19.86(19) . . . . ? C2 Ru1 C5 C60 -174.29(19) . . . . ? Ru2 Ru1 C5 C60 133.63(19) . . . . ? C8 Ru1 C5 Ru2 147.30(8) . . . . ? C9 Ru1 C5 Ru2 3.0(4) . . . . ? C7 Ru1 C5 Ru2 -113.78(8) . . . . ? C2 Ru1 C5 Ru2 52.08(7) . . . . ? C10 Ru2 C5 C4 72.8(4) . . . . ? C11 Ru2 C5 C4 -158.52(13) . . . . ? C1 Ru2 C5 C4 34.15(12) . . . . ? C2 Ru2 C5 C4 73.94(12) . . . . ? P2 Ru2 C5 C4 -52.22(11) . . . . ? Ru1 Ru2 C5 C4 122.57(13) . . . . ? C10 Ru2 C5 C60 -177.0(3) . . . . ? C11 Ru2 C5 C60 -48.3(2) . . . . ? C1 Ru2 C5 C60 144.4(2) . . . . ? C2 Ru2 C5 C60 -175.8(2) . . . . ? C4 Ru2 C5 C60 110.2(2) . . . . ? P2 Ru2 C5 C60 58.03(19) . . . . ? Ru1 Ru2 C5 C60 -127.2(2) . . . . ? C10 Ru2 C5 Ru1 -49.8(4) . . . . ? C11 Ru2 C5 Ru1 78.91(8) . . . . ? C1 Ru2 C5 Ru1 -88.42(8) . . . . ? C2 Ru2 C5 Ru1 -48.63(7) . . . . ? C4 Ru2 C5 Ru1 -122.57(13) . . . . ? P2 Ru2 C5 Ru1 -174.79(4) . . . . ? C8 Ru1 C7 O7 -25(8) . . . . ? C9 Ru1 C7 O7 70(8) . . . . ? C2 Ru1 C7 O7 175(100) . . . . ? C5 Ru1 C7 O7 -122(8) . . . . ? Ru2 Ru1 C7 O7 -176(100) . . . . ? C9 Ru1 C8 O8 103(4) . . . . ? C7 Ru1 C8 O8 -163(4) . . . . ? C2 Ru1 C8 O8 12(4) . . . . ? C5 Ru1 C8 O8 -69(4) . . . . ? Ru2 Ru1 C8 O8 -27(4) . . . . ? C8 Ru1 C9 O9 -33(5) . . . . ? C7 Ru1 C9 O9 -132(5) . . . . ? C2 Ru1 C9 O9 63(5) . . . . ? C5 Ru1 C9 O9 111(5) . . . . ? Ru2 Ru1 C9 O9 114(5) . . . . ? C11 Ru2 C10 O10 125(4) . . . . ? C1 Ru2 C10 O10 -70(4) . . . . ? C2 Ru2 C10 O10 -107(4) . . . . ? C4 Ru2 C10 O10 -48(4) . . . . ? C5 Ru2 C10 O10 -106(4) . . . . ? P2 Ru2 C10 O10 19(4) . . . . ? Ru1 Ru2 C10 O10 -149(4) . . . . ? C10 Ru2 C11 O11 149(19) . . . . ? C1 Ru2 C11 O11 9(19) . . . . ? C2 Ru2 C11 O11 51(19) . . . . ? C4 Ru2 C11 O11 -37(19) . . . . ? C5 Ru2 C11 O11 -21(19) . . . . ? P2 Ru2 C11 O11 -120(19) . . . . ? Ru1 Ru2 C11 O11 26(19) . . . . ? C14 Ru3 C12 O12 47(4) . . . . ? C13 Ru3 C12 O12 -50(4) . . . . ? C4 Ru3 C12 O12 144(4) . . . . ? P1 Ru3 C12 O12 138(4) . . . . ? P2 Ru3 C12 O12 -142(4) . . . . ? C14 Ru3 C13 O13 -159(3) . . . . ? C12 Ru3 C13 O13 -68(3) . . . . ? C4 Ru3 C13 O13 57(3) . . . . ? P1 Ru3 C13 O13 109(3) . . . . ? P2 Ru3 C13 O13 18(3) . . . . ? C13 Ru3 C14 O14 66(4) . . . . ? C12 Ru3 C14 O14 -26(4) . . . . ? C4 Ru3 C14 O14 -123(4) . . . . ? P1 Ru3 C14 O14 172(4) . . . . ? P2 Ru3 C14 O14 -98(4) . . . . ? C1 P1 C20 C25 128.34(18) . . . . ? C40 P1 C20 C25 4.0(2) . . . . ? Ru3 P1 C20 C25 -140.17(16) . . . . ? C1 P1 C20 C21 -41.81(18) . . . . ? C40 P1 C20 C21 -166.15(17) . . . . ? Ru3 P1 C20 C21 49.68(19) . . . . ? C25 C20 C21 C22 -1.2(3) . . . . ? P1 C20 C21 C22 169.30(18) . . . . ? C20 C21 C22 C23 -0.1(4) . . . . ? C21 C22 C23 C24 1.2(4) . . . . ? C22 C23 C24 C25 -1.0(4) . . . . ? C23 C24 C25 C20 -0.3(4) . . . . ? C21 C20 C25 C24 1.4(3) . . . . ? P1 C20 C25 C24 -168.78(18) . . . . ? C1 C2 C30 C35 62.1(3) . . . . ? Ru1 C2 C30 C35 -105.6(2) . . . . ? Ru2 C2 C30 C35 147.63(17) . . . . ? C1 C2 C30 C31 -119.1(2) . . . . ? Ru1 C2 C30 C31 73.2(3) . . . . ? Ru2 C2 C30 C31 -33.6(3) . . . . ? C35 C30 C31 C32 -3.3(3) . . . . ? C2 C30 C31 C32 177.9(2) . . . . ? C30 C31 C32 C33 1.5(4) . . . . ? C31 C32 C33 C34 1.5(4) . . . . ? C32 C33 C34 C35 -2.7(4) . . . . ? C33 C34 C35 C30 0.9(4) . . . . ? C31 C30 C35 C34 2.1(3) . . . . ? C2 C30 C35 C34 -179.1(2) . . . . ? C1 P1 C40 C45 169.19(16) . . . . ? C20 P1 C40 C45 -79.76(18) . . . . ? Ru3 P1 C40 C45 60.94(19) . . . . ? C1 P1 C40 C41 -11.5(2) . . . . ? C20 P1 C40 C41 99.60(19) . . . . ? Ru3 P1 C40 C41 -119.70(17) . . . . ? C45 C40 C41 C42 -0.6(3) . . . . ? P1 C40 C41 C42 -179.95(17) . . . . ? C40 C41 C42 C43 0.6(3) . . . . ? C41 C42 C43 C44 -0.3(4) . . . . ? C42 C43 C44 C45 0.0(4) . . . . ? C43 C44 C45 C40 0.1(3) . . . . ? C41 C40 C45 C44 0.3(3) . . . . ? P1 C40 C45 C44 179.64(17) . . . . ? C70 P2 C50 C55 124.83(18) . . . . ? Ru2 P2 C50 C55 -107.23(17) . . . . ? Ru3 P2 C50 C55 7.5(2) . . . . ? C70 P2 C50 C51 -59.62(17) . . . . ? Ru2 P2 C50 C51 68.31(17) . . . . ? Ru3 P2 C50 C51 -176.91(13) . . . . ? C55 C50 C51 C52 1.6(3) . . . . ? P2 C50 C51 C52 -174.20(17) . . . . ? C50 C51 C52 C53 -0.1(3) . . . . ? C51 C52 C53 C54 -1.0(3) . . . . ? C52 C53 C54 C55 0.6(3) . . . . ? C51 C50 C55 C54 -2.0(3) . . . . ? P2 C50 C55 C54 173.48(16) . . . . ? C53 C54 C55 C50 0.9(3) . . . . ? C4 C5 C60 C65 125.5(2) . . . . ? Ru1 C5 C60 C65 -68.8(3) . . . . ? Ru2 C5 C60 C65 37.6(3) . . . . ? C4 C5 C60 C61 -55.1(3) . . . . ? Ru1 C5 C60 C61 110.6(2) . . . . ? Ru2 C5 C60 C61 -142.96(17) . . . . ? C65 C60 C61 C62 -2.0(3) . . . . ? C5 C60 C61 C62 178.5(2) . . . . ? C60 C61 C62 C63 -0.7(4) . . . . ? C61 C62 C63 C64 2.4(4) . . . . ? C62 C63 C64 C65 -1.3(4) . . . . ? C63 C64 C65 C60 -1.5(3) . . . . ? C61 C60 C65 C64 3.1(3) . . . . ? C5 C60 C65 C64 -177.4(2) . . . . ? C50 P2 C70 C75 131.87(19) . . . . ? Ru2 P2 C70 C75 8.7(2) . . . . ? Ru3 P2 C70 C75 -102.67(18) . . . . ? C50 P2 C70 C71 -51.38(19) . . . . ? Ru2 P2 C70 C71 -174.51(15) . . . . ? Ru3 P2 C70 C71 74.09(18) . . . . ? C75 C70 C71 C72 -0.2(3) . . . . ? P2 C70 C71 C72 -177.06(19) . . . . ? C70 C71 C72 C73 0.1(4) . . . . ? C71 C72 C73 C74 0.2(4) . . . . ? C72 C73 C74 C75 -0.4(4) . . . . ? C71 C70 C75 C74 -0.1(3) . . . . ? P2 C70 C75 C74 176.69(18) . . . . ? C73 C74 C75 C70 0.3(4) . . . . ? data_p22 _database_code_CSD 172818 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61 H53 Cl2 O6 P3 Ru3' _chemical_formula_sum ' C122 H106 Cl4 O12 P6 Ru6' _chemical_formula_weight 1349.05 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 triclinil _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0485(10) _cell_length_b 12.9634(10) _cell_length_c 20.482(2) _cell_angle_alpha 72.421(10) _cell_angle_beta 87.320(10) _cell_angle_gamma 89.122(10) _cell_volume 3046.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS (Sheldrick, 1998) _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _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 24040 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10601 _reflns_number_gt 8500 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0951P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10601 _refine_ls_number_parameters 811 _refine_ls_number_restraints 243 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.458244(4) 0.601303(4) 0.259732(3) 0.02365(1) Uani 1 1 d . A . Ru2 Ru 0.283114(5) 0.783688(4) 0.245248(3) 0.02947(2) Uani 1 1 d . . . Ru3 Ru 0.294273(4) 0.625530(4) 0.381065(3) 0.02556(2) Uani 1 1 d . A . P1 P 0.320473(15) 0.670555(14) 0.175763(9) 0.02906(5) Uani 1 1 d . A . P2 P 0.287832(15) 0.811956(14) 0.352632(9) 0.02861(5) Uani 1 1 d . A . P3 P 0.543420(14) 0.453442(14) 0.233865(8) 0.02556(5) Uani 1 1 d . . . O7 O 0.62652(4) 0.59058(4) 0.36801(3) 0.04338(17) Uani 1 1 d . A . O8 O 0.61442(5) 0.77232(4) 0.16632(3) 0.04957(19) Uani 1 1 d . A . O9 O 0.46491(5) 0.94275(4) 0.18253(3) 0.05049(19) Uani 1 1 d . . . O10 O 0.12791(5) 0.95704(6) 0.17011(4) 0.0760(3) Uani 1 1 d . . . O11 O 0.47645(4) 0.61395(4) 0.48111(2) 0.04402(17) Uani 1 1 d . A . O12 O 0.13770(6) 0.56452(5) 0.50472(3) 0.0672(2) Uani 1 1 d . A . C4 C 0.35317(5) 0.49786(5) 0.32894(3) 0.02406(18) Uani 1 1 d . . . C5 C 0.29086(5) 0.44038(5) 0.37630(3) 0.0291(2) Uani 1 1 d . A . C6 C 0.22600(6) 0.34382(6) 0.41711(4) 0.0341(2) Uani 1 1 d . . . C7 C 0.56261(5) 0.59386(5) 0.32784(3) 0.0279(2) Uani 1 1 d . . . C8 C 0.55314(6) 0.71130(5) 0.19953(4) 0.0344(2) Uani 1 1 d . . . C9 C 0.39867(6) 0.87903(5) 0.20648(3) 0.0343(2) Uani 1 1 d . A . C10 C 0.18537(7) 0.88856(6) 0.19886(4) 0.0435(3) Uani 1 1 d . A . C11 C 0.40939(6) 0.61381(5) 0.44456(3) 0.0332(2) Uani 1 1 d . . . C12 C 0.19656(7) 0.58704(6) 0.45792(4) 0.0412(2) Uani 1 1 d . . . C20 C 0.37922(6) 0.73984(6) 0.08856(3) 0.0356(2) Uani 1 1 d . . . C21 C 0.45228(6) 0.68405(6) 0.05677(4) 0.0384(2) Uani 1 1 d . A . H21 H 0.4699 0.6106 0.0794 0.046 Uiso 1 1 calc R . . C22 C 0.49944(7) 0.73492(7) -0.00771(4) 0.0489(3) Uani 1 1 d . . . H22 H 0.5502 0.6963 -0.0286 0.059 Uiso 1 1 calc R A . C23 C 0.47384(9) 0.84024(8) -0.04178(4) 0.0632(4) Uani 1 1 d . A . H23 H 0.5052 0.8743 -0.0864 0.076 Uiso 1 1 calc R . . C24 C 0.40311(9) 0.89510(8) -0.01088(5) 0.0764(4) Uani 1 1 d . . . H24 H 0.3856 0.9683 -0.0342 0.092 Uiso 1 1 calc R A . C25 C 0.35556(9) 0.84675(7) 0.05432(4) 0.0576(3) Uani 1 1 d . A . H25 H 0.3070 0.8871 0.0752 0.069 Uiso 1 1 calc R . . C1 C 0.16349(9) 0.66714(8) 0.31569(6) 0.0336(2) Uani 0.63 1 d PD A -1 C2 C 0.07815(8) 0.69430(9) 0.28793(5) 0.0327(2) Uani 0.63 1 d PD A -1 C3 C -0.03692(9) 0.71589(10) 0.26573(6) 0.0492(3) Uani 0.63 1 d PD A -1 C31 C -0.08238(12) 0.81489(11) 0.28497(7) 0.0680(4) Uani 0.63 1 d PD A -1 H31A H -0.0750 0.8031 0.3341 0.082 Uiso 0.63 1 calc PR A -1 H31B H -0.1609 0.8253 0.2741 0.082 Uiso 0.63 1 calc PR A -1 H31C H -0.0402 0.8794 0.2589 0.082 Uiso 0.63 1 calc PR A -1 C32 C -0.10279(11) 0.61133(12) 0.30379(7) 0.0636(5) Uani 0.63 1 d PD A -1 H32A H -0.0655 0.5489 0.2949 0.076 Uiso 0.63 1 calc PR A -1 H32B H -0.1784 0.6174 0.2873 0.076 Uiso 0.63 1 calc PR A -1 H32C H -0.1060 0.6018 0.3532 0.076 Uiso 0.63 1 calc PR A -1 C33 C -0.04383(11) 0.73830(12) 0.18646(6) 0.0522(3) Uani 0.63 1 d PD A -1 H33A H -0.0120 0.8095 0.1625 0.063 Uiso 0.63 1 calc PR A -1 H33B H -0.1217 0.7368 0.1750 0.063 Uiso 0.63 1 calc PR A -1 H33C H -0.0021 0.6825 0.1724 0.063 Uiso 0.63 1 calc PR A -1 C1A C 0.15879(13) 0.65011(14) 0.31580(10) 0.0336(2) Uani 0.37 1 d PD A -2 C2A C 0.06761(11) 0.67483(15) 0.29636(9) 0.0327(2) Uani 0.37 1 d PD A -2 C3A C -0.05137(13) 0.68747(14) 0.28081(9) 0.0492(3) Uani 0.37 1 d PD A -2 C31A C -0.10400(19) 0.76792(16) 0.31482(11) 0.0680(4) Uani 0.37 1 d PD A -2 H31D H -0.1025 0.7373 0.3648 0.082 Uiso 0.37 1 calc PR A -2 H31E H -0.1811 0.7820 0.3014 0.082 Uiso 0.37 1 calc PR A -2 H31F H -0.0620 0.8358 0.3001 0.082 Uiso 0.37 1 calc PR A -2 C32A C -0.10255(18) 0.57303(16) 0.30898(13) 0.0636(5) Uani 0.37 1 d PD A -2 H32D H -0.0744 0.5280 0.2811 0.076 Uiso 0.37 1 calc PR A -2 H32E H -0.1836 0.5783 0.3072 0.076 Uiso 0.37 1 calc PR A -2 H32F H -0.0820 0.5403 0.3566 0.076 Uiso 0.37 1 calc PR A -2 C33A C -0.06576(18) 0.73240(19) 0.20152(9) 0.0522(3) Uani 0.37 1 d PD A -2 H33D H -0.0104 0.7889 0.1812 0.063 Uiso 0.37 1 calc PR A -2 H33E H -0.1405 0.7629 0.1928 0.063 Uiso 0.37 1 calc PR A -2 H33F H -0.0554 0.6735 0.1811 0.063 Uiso 0.37 1 calc PR A -2 C40 C 0.20605(6) 0.59370(6) 0.15766(3) 0.0325(2) Uani 1 1 d . A -2 C41 C 0.16314(6) 0.61842(6) 0.09238(4) 0.0430(2) Uani 1 1 d . A -2 H41 H 0.1939 0.6765 0.0560 0.052 Uiso 1 1 calc R A -2 C42 C 0.07747(7) 0.55970(7) 0.08068(4) 0.0544(3) Uani 1 1 d . A -2 H42 H 0.0484 0.5787 0.0363 0.065 Uiso 1 1 calc R A -2 C43 C 0.03197(7) 0.47350(7) 0.13169(4) 0.0554(3) Uani 1 1 d . A -2 H43 H -0.0263 0.4322 0.1223 0.067 Uiso 1 1 calc R A -2 C44 C 0.07253(7) 0.44822(7) 0.19675(4) 0.0495(3) Uani 1 1 d . A -2 H44 H 0.0415 0.3895 0.2325 0.059 Uiso 1 1 calc R A -2 C45 C 0.15864(6) 0.50835(6) 0.21016(4) 0.0396(2) Uani 1 1 d . A -2 H45 H 0.1852 0.4912 0.2551 0.048 Uiso 1 1 calc R A -2 C50 C 0.40490(6) 0.88385(5) 0.37332(3) 0.0308(2) Uani 1 1 d . A -2 C51 C 0.51156(6) 0.85914(6) 0.35340(3) 0.0355(2) Uani 1 1 d . A -2 H51 H 0.5220 0.8044 0.3316 0.043 Uiso 1 1 calc R A -2 C52 C 0.60282(7) 0.91406(7) 0.36520(4) 0.0475(3) Uani 1 1 d . A -2 H52 H 0.6753 0.8964 0.3515 0.057 Uiso 1 1 calc R A -2 C53 C 0.58935(7) 0.99379(6) 0.39649(4) 0.0482(3) Uani 1 1 d . A -2 H53 H 0.6520 1.0314 0.4043 0.058 Uiso 1 1 calc R A -2 C54 C 0.48371(7) 1.01847(6) 0.41638(4) 0.0466(3) Uani 1 1 d . A -2 H54 H 0.4736 1.0730 0.4384 0.056 Uiso 1 1 calc R A -2 C55 C 0.39269(7) 0.96426(6) 0.40450(4) 0.0358(2) Uani 1 1 d . A -2 H55 H 0.3204 0.9826 0.4180 0.043 Uiso 1 1 calc R A -2 C61 C 0.25714(7) 0.30985(7) 0.49178(4) 0.0504(3) Uani 1 1 d . A -2 H61A H 0.3359 0.2897 0.4948 0.060 Uiso 1 1 calc R A -2 H61B H 0.2118 0.2477 0.5180 0.060 Uiso 1 1 calc R A -2 H61C H 0.2438 0.3702 0.5106 0.060 Uiso 1 1 calc R A -2 C62 C 0.10162(6) 0.36816(7) 0.41174(5) 0.0473(3) Uani 1 1 d . A -2 H62A H 0.0835 0.4289 0.4296 0.057 Uiso 1 1 calc R A -2 H62B H 0.0595 0.3041 0.4386 0.057 Uiso 1 1 calc R A -2 H62C H 0.0821 0.3871 0.3636 0.057 Uiso 1 1 calc R A -2 C63 C 0.25415(8) 0.25224(6) 0.38502(5) 0.0545(3) Uani 1 1 d . A -2 H63A H 0.2287 0.2728 0.3381 0.065 Uiso 1 1 calc R A -2 H63B H 0.2169 0.1854 0.4124 0.065 Uiso 1 1 calc R A -2 H63C H 0.3347 0.2405 0.3843 0.065 Uiso 1 1 calc R A -2 C70 C 0.16706(6) 0.88480(6) 0.37420(4) 0.0332(2) Uani 1 1 d . A -2 C71 C 0.14544(7) 0.98787(6) 0.33073(4) 0.0478(3) Uani 1 1 d . A -2 H71 H 0.1931 1.0177 0.2915 0.057 Uiso 1 1 calc R A -2 C72 C 0.05528(8) 1.04784(7) 0.34384(5) 0.0559(3) Uani 1 1 d . A -2 H72 H 0.0425 1.1186 0.3142 0.067 Uiso 1 1 calc R A -2 C73 C -0.01495(7) 1.00493(7) 0.39939(4) 0.0502(3) Uani 1 1 d . A -2 H73 H -0.0771 1.0457 0.4080 0.060 Uiso 1 1 calc R A -2 C74 C 0.00354(7) 0.90434(7) 0.44233(4) 0.0516(3) Uani 1 1 d . A -2 H74 H -0.0456 0.8753 0.4810 0.062 Uiso 1 1 calc R A -2 C75 C 0.09477(7) 0.84251(6) 0.43023(4) 0.0400(2) Uani 1 1 d . A -2 H75 H 0.1067 0.7719 0.4604 0.048 Uiso 1 1 calc R A -2 C80 C 0.63507(6) 0.48629(5) 0.15613(3) 0.0290(2) Uani 1 1 d . A -2 C81 C 0.62121(6) 0.44180(6) 0.10278(4) 0.0396(2) Uani 1 1 d . A -2 H81 H 0.5658 0.3885 0.1071 0.048 Uiso 1 1 calc R A -2 C82 C 0.68960(7) 0.47628(7) 0.04263(4) 0.0500(3) Uani 1 1 d . A -2 H82 H 0.6798 0.4463 0.0063 0.060 Uiso 1 1 calc R A -2 C83 C 0.76949(6) 0.55207(7) 0.03608(4) 0.0414(3) Uani 1 1 d . A -2 H83 H 0.8144 0.5756 -0.0050 0.050 Uiso 1 1 calc R A -2 C84 C 0.78573(6) 0.59526(6) 0.08939(4) 0.0380(2) Uani 1 1 d . A -2 H84 H 0.8411 0.6486 0.0850 0.046 Uiso 1 1 calc R A -2 C85 C 0.72039(6) 0.55950(6) 0.14840(3) 0.0337(2) Uani 1 1 d . A -2 H85 H 0.7344 0.5863 0.1856 0.040 Uiso 1 1 calc R A -2 C90 C 0.63527(6) 0.37481(6) 0.29956(3) 0.0322(2) Uani 1 1 d . A -2 C91 C 0.59428(7) 0.33638(5) 0.36788(3) 0.0378(2) Uani 1 1 d . A -2 H91 H 0.5211 0.3555 0.3794 0.045 Uiso 1 1 calc R A -2 C92 C 0.65774(8) 0.27158(6) 0.41857(4) 0.0474(3) Uani 1 1 d . A -2 H92 H 0.6288 0.2470 0.4646 0.057 Uiso 1 1 calc R A -2 C93 C 0.76339(7) 0.24262(7) 0.40212(4) 0.0511(3) Uani 1 1 d . A -2 H93 H 0.8072 0.1973 0.4368 0.061 Uiso 1 1 calc R A -2 C94 C 0.80580(7) 0.27902(8) 0.33551(5) 0.0602(3) Uani 1 1 d . A -2 H94 H 0.8789 0.2592 0.3245 0.072 Uiso 1 1 calc R A -2 C95 C 0.74201(7) 0.34451(7) 0.28463(4) 0.0463(3) Uani 1 1 d . A -2 H95 H 0.7718 0.3690 0.2388 0.056 Uiso 1 1 calc R A -2 C100 C 0.45686(6) 0.34576(5) 0.22218(3) 0.0285(2) Uani 1 1 d . A -2 C101 C 0.47930(7) 0.23828(6) 0.25102(4) 0.0385(2) Uani 1 1 d . A -2 H101 H 0.5369 0.2173 0.2825 0.046 Uiso 1 1 calc R A -2 C102 C 0.41917(8) 0.15935(6) 0.23501(4) 0.0479(3) Uani 1 1 d . A -2 H102 H 0.4366 0.0851 0.2550 0.057 Uiso 1 1 calc R A -2 C103 C 0.33423(7) 0.18855(6) 0.19015(4) 0.0418(2) Uani 1 1 d D A -2 H103 H 0.2932 0.1346 0.1791 0.050 Uiso 1 1 calc R A -2 C104 C 0.30921(6) 0.29632(7) 0.16144(4) 0.0425(3) Uani 1 1 d . A -2 H104 H 0.2500 0.3168 0.1311 0.051 Uiso 1 1 calc R A -2 C105 C 0.37094(6) 0.37529(6) 0.17693(4) 0.0350(2) Uani 1 1 d . A -2 H105 H 0.3543 0.4496 0.1565 0.042 Uiso 1 1 calc R A -2 Cl1L Cl 0.2257(3) 0.1325(2) 0.02236(12) 0.1033(6) Uani 0.10 1 d PDU B -1 Cl2L Cl 0.0623(2) 0.00360(18) -0.00177(14) 0.0806(4) Uani 0.10 1 d PDU B -1 C1L C 0.17490(13) 0.0863(2) -0.04392(14) 0.0294(5) Uani 0.10 1 d PDU B -1 H1L1 H 0.1499 0.1474 -0.0825 0.035 Uiso 0.10 1 calc PR B -1 H1L2 H 0.2321 0.0443 -0.0613 0.035 Uiso 0.10 1 calc PR B -1 Cl1M Cl 0.01095(16) 0.15600(13) -0.00531(9) 0.1033(6) Uani 0.18 1 d PDU C -2 Cl2M Cl 0.23833(14) 0.13334(11) 0.02132(8) 0.0806(4) Uani 0.18 1 d PDU C -2 C1M C 0.12995(18) 0.0799(2) -0.01114(15) 0.0294(5) Uani 0.18 1 d PDU C -2 H1M1 H 0.1178 0.0031 0.0157 0.035 Uiso 0.18 1 calc PR C -2 H1M2 H 0.1476 0.0838 -0.0595 0.035 Uiso 0.18 1 calc PR C -2 Cl1N Cl 0.0932(5) 0.2012(2) 0.06614(15) 0.1033(6) Uani 0.07 1 d PDU D -3 Cl2N Cl 0.0125(3) 0.1479(3) -0.03972(15) 0.0806(4) Uani 0.07 1 d PDU D -3 C1N C 0.1212(3) 0.1084(3) 0.01747(15) 0.0294(5) Uani 0.07 1 d PDU D -3 H1N1 H 0.1953 0.1205 -0.0066 0.035 Uiso 0.07 1 calc PR D -3 H1N2 H 0.1143 0.0320 0.0462 0.035 Uiso 0.07 1 calc PR D -3 Cl1O Cl 0.1802(6) 0.1052(2) -0.00954(15) 0.1033(6) Uani 0.05 1 d PDU E -4 Cl2O Cl 0.0406(3) 0.2243(3) 0.0793(2) 0.0806(4) Uani 0.05 1 d PDU E -4 C1O C 0.1614 0.1810 0.0455 0.037(3) Uiso 0.05 1 d PD E -4 H1O1 H 0.2037 0.2482 0.0232 0.044 Uiso 0.05 1 calc PR E -4 H1O2 H 0.2032 0.1418 0.0861 0.044 Uiso 0.05 1 calc PR E -4 Cl1P Cl -0.0660(3) 0.2086(4) 0.13316(19) 0.1033(6) Uani 0.05 1 d PDU F -5 Cl2P Cl 0.0646(5) 0.1248(2) 0.02804(15) 0.0806(4) Uani 0.05 1 d PDU F -5 C1P C 0.0581(3) 0.2145(3) 0.08000(15) 0.0294(5) Uani 0.05 1 d PDU F -5 H1P1 H 0.0669 0.2895 0.0493 0.035 Uiso 0.05 1 calc PR F -5 H1P2 H 0.1223 0.1986 0.1099 0.035 Uiso 0.05 1 calc PR F -5 Cl1Q Cl 0.72174(16) 0.07197(14) 0.20442(9) 0.0811(4) Uani 0.16 1 d PDU G -6 Cl2Q Cl 0.88683(17) 0.22434(17) 0.15358(11) 0.1063(6) Uani 0.16 1 d PDU G -6 C1Q C 0.7502(2) 0.1926(3) 0.13709(18) 0.0434(4) Uani 0.16 1 d PDU G -6 H1Q1 H 0.6972 0.2507 0.1392 0.052 Uiso 0.16 1 calc PR G -6 H1Q2 H 0.7476 0.1805 0.0917 0.052 Uiso 0.16 1 calc PR G -6 Cl1R Cl 0.9092(2) 0.1950(2) 0.17219(14) 0.0811(4) Uani 0.10 1 d PDU H -7 Cl2R Cl 0.7323(3) 0.0373(2) 0.18296(13) 0.1063(6) Uani 0.10 1 d PDU H -7 C1R C 0.8204(3) 0.0952(3) 0.23012(17) 0.0434(4) Uani 0.10 1 d PDU H -7 H1R1 H 0.8662 0.0378 0.2602 0.052 Uiso 0.10 1 calc PR H -7 H1R2 H 0.7746 0.1293 0.2594 0.052 Uiso 0.10 1 calc PR H -7 Cl1S Cl 0.7478(2) 0.00375(15) 0.17411(12) 0.0811(4) Uani 0.12 1 d PDU I -8 Cl2S Cl 0.8158(3) 0.2274(2) 0.11302(12) 0.1063(6) Uani 0.12 1 d PDU I -8 C1S C 0.7351(4) 0.1368(2) 0.18028(19) 0.0434(4) Uani 0.12 1 d PDU I -8 H1S1 H 0.7609 0.1386 0.2251 0.052 Uiso 0.12 1 calc PR I -8 H1S2 H 0.6562 0.1595 0.1772 0.052 Uiso 0.12 1 calc PR I -8 Cl1T Cl 0.7971(3) 0.00578(18) 0.14046(16) 0.0811(4) Uani 0.08 1 d PDU J -9 Cl2T Cl 0.7791(4) 0.1198(3) 0.23130(12) 0.1063(6) Uani 0.08 1 d PDU J -9 C1T C 0.7767(8) 0.1439(2) 0.14099(14) 0.0434(4) Uani 0.08 1 d PDU J -9 H1T1 H 0.8379 0.1919 0.1159 0.052 Uiso 0.08 1 calc PR J -9 H1T2 H 0.7046 0.1737 0.1225 0.052 Uiso 0.08 1 calc PR J -9 Cl1U Cl 0.7576(2) 0.0713(3) 0.2260(2) 0.0811(4) Uani 0.07 1 d PDU K -10 Cl2U Cl 0.8755(5) 0.2439(3) 0.12682(16) 0.1063(6) Uani 0.07 1 d PDU K -10 C1U C 0.8879(3) 0.1418(3) 0.2068(2) 0.0434(4) Uani 0.07 1 d PDU K -10 H1U1 H 0.9038 0.1747 0.2431 0.052 Uiso 0.07 1 calc PR K -10 H1U2 H 0.9490 0.0913 0.2037 0.052 Uiso 0.07 1 calc PR K -10 Cl1W Cl 0.9414(3) 0.1965(3) 0.1718(4) 0.0811(4) Uani 0.03 1 d PDU L -11 Cl2W Cl 0.7267(3) 0.1023(7) 0.1689(2) 0.1063(6) Uani 0.03 1 d PDU L -11 C1W C 0.8506(2) 0.0862(4) 0.2159(3) 0.0434(4) Uani 0.03 1 d PDU L -11 H1W1 H 0.8867 0.0162 0.2180 0.052 Uiso 0.03 1 calc PR L -11 H1W2 H 0.8328 0.0876 0.2633 0.052 Uiso 0.03 1 calc PR L -11 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02026(2) 0.02232(2) 0.03024(2) -0.01164(2) 0.00398(2) 0.00264(2) Ru2 0.03324(3) 0.02335(2) 0.03315(3) -0.01091(2) -0.00046(2) 0.00508(2) Ru3 0.02005(2) 0.02267(2) 0.03539(2) -0.01200(2) 0.00493(2) 0.00384(2) P1 0.03068(9) 0.02717(8) 0.03163(8) -0.01265(6) -0.00085(7) 0.00512(7) P2 0.02810(9) 0.02428(8) 0.03583(8) -0.01339(6) 0.00169(7) 0.00630(7) P3 0.02402(8) 0.02504(8) 0.03015(7) -0.01308(6) 0.00350(7) 0.00485(7) O7 0.0253(2) 0.0649(3) 0.0519(2) -0.0358(2) -0.0019(2) 0.0058(2) O8 0.0377(3) 0.0384(3) 0.0671(3) -0.0106(3) 0.0187(3) -0.0044(2) O9 0.0527(3) 0.0340(3) 0.0676(3) -0.0220(2) 0.0140(3) -0.0008(2) O10 0.0548(4) 0.0790(4) 0.0836(4) -0.0077(4) -0.0182(3) 0.0315(3) O11 0.0430(3) 0.0531(3) 0.0424(2) -0.0235(2) -0.0100(2) 0.0132(2) O12 0.0694(4) 0.0519(3) 0.0791(3) -0.0256(3) 0.0511(3) -0.0095(3) C4 0.0213(3) 0.0207(3) 0.0370(3) -0.0197(2) 0.0014(3) 0.0059(2) C5 0.0192(3) 0.0281(3) 0.0425(3) -0.0153(3) 0.0009(3) 0.0068(3) C6 0.0290(4) 0.0285(3) 0.0427(4) -0.0081(3) 0.0045(3) -0.0017(3) C7 0.0276(3) 0.0254(3) 0.0342(3) -0.0157(2) 0.0062(3) 0.0060(3) C8 0.0289(4) 0.0301(3) 0.0456(4) -0.0151(3) 0.0048(3) 0.0079(3) C9 0.0391(4) 0.0252(3) 0.0394(3) -0.0125(3) 0.0084(3) 0.0025(3) C10 0.0403(4) 0.0403(4) 0.0492(4) -0.0120(3) -0.0059(3) 0.0051(3) C11 0.0375(4) 0.0273(3) 0.0376(3) -0.0153(3) 0.0084(3) 0.0020(3) C12 0.0381(4) 0.0275(3) 0.0595(4) -0.0178(3) 0.0133(4) -0.0013(3) C20 0.0345(4) 0.0398(4) 0.0332(3) -0.0119(3) -0.0036(3) 0.0017(3) C21 0.0397(4) 0.0417(4) 0.0372(3) -0.0174(3) -0.0008(3) 0.0050(3) C22 0.0564(5) 0.0530(5) 0.0372(4) -0.0148(3) 0.0084(4) -0.0032(4) C23 0.0812(7) 0.0667(6) 0.0363(4) -0.0090(4) 0.0124(4) -0.0109(5) C24 0.1263(9) 0.0393(5) 0.0547(5) -0.0038(4) 0.0114(6) 0.0113(6) C25 0.0929(7) 0.0356(4) 0.0373(4) -0.0025(3) 0.0040(4) 0.0172(4) C1 0.0307(4) 0.0248(3) 0.0558(4) -0.0279(3) -0.0003(3) -0.0032(3) C2 0.0272(4) 0.0368(4) 0.0368(3) -0.0158(3) 0.0007(3) 0.0061(3) C3 0.0280(4) 0.0632(5) 0.0684(5) -0.0384(4) -0.0037(4) 0.0159(4) C31 0.0410(5) 0.0917(7) 0.0922(7) -0.0593(4) -0.0114(5) 0.0284(5) C32 0.0243(4) 0.0992(10) 0.0713(6) -0.0324(6) 0.0028(4) 0.0032(6) C33 0.0336(5) 0.0649(5) 0.0667(5) -0.0314(4) -0.0134(4) 0.0099(4) C1A 0.0307(4) 0.0248(3) 0.0558(4) -0.0279(3) -0.0003(3) -0.0032(3) C2A 0.0272(4) 0.0368(4) 0.0368(3) -0.0158(3) 0.0007(3) 0.0061(3) C3A 0.0280(4) 0.0632(5) 0.0684(5) -0.0384(4) -0.0037(4) 0.0159(4) C31A 0.0410(5) 0.0917(7) 0.0922(7) -0.0593(4) -0.0114(5) 0.0284(5) C32A 0.0243(4) 0.0992(10) 0.0713(6) -0.0324(6) 0.0028(4) 0.0032(6) C33A 0.0336(5) 0.0649(5) 0.0667(5) -0.0314(4) -0.0134(4) 0.0099(4) C40 0.0261(3) 0.0357(3) 0.0435(3) -0.0239(2) -0.0035(3) 0.0096(3) C41 0.0316(4) 0.0566(4) 0.0503(4) -0.0304(3) -0.0050(3) 0.0156(3) C42 0.0335(4) 0.0817(5) 0.0643(4) -0.0459(3) -0.0110(3) 0.0184(4) C43 0.0256(4) 0.0747(4) 0.0906(5) -0.0610(3) -0.0117(4) 0.0100(3) C44 0.0316(4) 0.0480(4) 0.0786(5) -0.0344(3) 0.0005(4) 0.0049(3) C45 0.0319(4) 0.0424(4) 0.0501(4) -0.0226(3) -0.0015(3) 0.0046(3) C50 0.0357(4) 0.0224(3) 0.0331(3) -0.0070(3) 0.0001(3) 0.0019(3) C51 0.0361(4) 0.0290(3) 0.0431(4) -0.0137(3) -0.0013(3) 0.0041(3) C52 0.0364(4) 0.0423(4) 0.0641(5) -0.0168(4) 0.0009(4) -0.0048(4) C53 0.0489(4) 0.0355(4) 0.0618(4) -0.0151(3) -0.0150(4) -0.0053(3) C54 0.0696(5) 0.0307(4) 0.0443(4) -0.0168(3) -0.0121(4) -0.0046(4) C55 0.0424(4) 0.0286(3) 0.0389(3) -0.0141(3) -0.0015(3) 0.0037(3) C61 0.0434(4) 0.0462(5) 0.0532(5) -0.0022(4) 0.0002(4) -0.0136(4) C62 0.0293(4) 0.0427(4) 0.0647(5) -0.0098(4) 0.0075(4) -0.0043(3) C63 0.0507(5) 0.0346(4) 0.0790(5) -0.0211(4) 0.0176(4) -0.0064(4) C70 0.0355(4) 0.0283(3) 0.0412(3) -0.0193(3) 0.0009(3) 0.0039(3) C71 0.0527(5) 0.0333(4) 0.0509(4) -0.0058(3) 0.0139(4) 0.0122(4) C72 0.0593(5) 0.0366(4) 0.0641(5) -0.0058(4) 0.0039(4) 0.0255(4) C73 0.0414(4) 0.0462(4) 0.0682(5) -0.0275(3) 0.0089(4) 0.0156(3) C74 0.0470(5) 0.0439(4) 0.0649(5) -0.0211(3) 0.0183(4) 0.0084(4) C75 0.0415(4) 0.0306(3) 0.0515(4) -0.0198(3) 0.0100(3) 0.0091(3) C80 0.0236(3) 0.0343(3) 0.0322(3) -0.0159(2) 0.0056(3) 0.0067(3) C81 0.0348(4) 0.0465(4) 0.0447(4) -0.0259(3) 0.0095(3) -0.0050(3) C82 0.0524(5) 0.0690(5) 0.0384(3) -0.0321(3) 0.0051(3) 0.0004(4) C83 0.0350(4) 0.0504(4) 0.0363(3) -0.0115(3) 0.0129(3) 0.0023(3) C84 0.0234(3) 0.0400(4) 0.0504(4) -0.0142(3) 0.0024(3) 0.0036(3) C85 0.0254(3) 0.0418(4) 0.0372(3) -0.0177(3) 0.0035(3) 0.0052(3) C90 0.0303(4) 0.0307(3) 0.0398(3) -0.0168(3) -0.0042(3) 0.0078(3) C91 0.0433(4) 0.0385(4) 0.0331(3) -0.0139(3) -0.0020(3) 0.0146(3) C92 0.0705(5) 0.0373(4) 0.0399(4) -0.0189(3) -0.0152(4) 0.0146(4) C93 0.0558(5) 0.0472(4) 0.0573(4) -0.0246(3) -0.0240(4) 0.0240(4) C94 0.0379(4) 0.0607(5) 0.0738(6) -0.0084(5) -0.0072(4) 0.0260(4) C95 0.0402(4) 0.0425(4) 0.0510(4) -0.0084(4) 0.0076(4) 0.0125(4) C100 0.0316(4) 0.0241(3) 0.0346(3) -0.0173(2) 0.0068(3) -0.0001(3) C101 0.0516(4) 0.0277(3) 0.0379(3) -0.0124(3) -0.0038(3) 0.0024(3) C102 0.0745(6) 0.0281(4) 0.0408(4) -0.0098(3) -0.0020(4) -0.0055(4) C103 0.0561(5) 0.0294(3) 0.0448(4) -0.0192(3) 0.0057(4) -0.0107(3) C104 0.0317(4) 0.0531(4) 0.0478(4) -0.0225(3) -0.0026(3) -0.0013(3) C105 0.0303(4) 0.0288(3) 0.0482(4) -0.0157(3) 0.0016(3) 0.0030(3) Cl1L 0.1470(12) 0.0530(7) 0.0893(8) 0.0055(7) 0.0266(8) -0.0122(8) Cl2L 0.1179(9) 0.0367(5) 0.0774(7) 0.0004(5) -0.0227(6) -0.0016(6) C1L 0.0316(8) 0.0230(8) 0.0286(8) 0.0000(6) -0.0017(6) -0.0007(7) Cl1M 0.1470(12) 0.0530(7) 0.0893(8) 0.0055(7) 0.0266(8) -0.0122(8) Cl2M 0.1179(9) 0.0367(5) 0.0774(7) 0.0004(5) -0.0227(6) -0.0016(6) C1M 0.0316(8) 0.0230(8) 0.0286(8) 0.0000(6) -0.0017(6) -0.0007(7) Cl1N 0.1470(12) 0.0530(7) 0.0893(8) 0.0055(7) 0.0266(8) -0.0122(8) Cl2N 0.1179(9) 0.0367(5) 0.0774(7) 0.0004(5) -0.0227(6) -0.0016(6) C1N 0.0316(8) 0.0230(8) 0.0286(8) 0.0000(6) -0.0017(6) -0.0007(7) Cl1O 0.1470(12) 0.0530(7) 0.0893(8) 0.0055(7) 0.0266(8) -0.0122(8) Cl2O 0.1179(9) 0.0367(5) 0.0774(7) 0.0004(5) -0.0227(6) -0.0016(6) Cl1P 0.1470(12) 0.0530(7) 0.0893(8) 0.0055(7) 0.0266(8) -0.0122(8) Cl2P 0.1179(9) 0.0367(5) 0.0774(7) 0.0004(5) -0.0227(6) -0.0016(6) C1P 0.0316(8) 0.0230(8) 0.0286(8) 0.0000(6) -0.0017(6) -0.0007(7) Cl1Q 0.0850(8) 0.0748(6) 0.0763(7) -0.0124(5) 0.0016(6) -0.0054(6) Cl2Q 0.1440(12) 0.0893(7) 0.0981(8) -0.0483(5) -0.0043(8) 0.0226(7) C1Q 0.0424(7) 0.0447(7) 0.0444(7) -0.0155(5) -0.0010(6) 0.0015(6) Cl1R 0.0850(8) 0.0748(6) 0.0763(7) -0.0124(5) 0.0016(6) -0.0054(6) Cl2R 0.1440(12) 0.0893(7) 0.0981(8) -0.0483(5) -0.0043(8) 0.0226(7) C1R 0.0424(7) 0.0447(7) 0.0444(7) -0.0155(5) -0.0010(6) 0.0015(6) Cl1S 0.0850(8) 0.0748(6) 0.0763(7) -0.0124(5) 0.0016(6) -0.0054(6) Cl2S 0.1440(12) 0.0893(7) 0.0981(8) -0.0483(5) -0.0043(8) 0.0226(7) C1S 0.0424(7) 0.0447(7) 0.0444(7) -0.0155(5) -0.0010(6) 0.0015(6) Cl1T 0.0850(8) 0.0748(6) 0.0763(7) -0.0124(5) 0.0016(6) -0.0054(6) Cl2T 0.1440(12) 0.0893(7) 0.0981(8) -0.0483(5) -0.0043(8) 0.0226(7) C1T 0.0424(7) 0.0447(7) 0.0444(7) -0.0155(5) -0.0010(6) 0.0015(6) Cl1U 0.0850(8) 0.0748(6) 0.0763(7) -0.0124(5) 0.0016(6) -0.0054(6) Cl2U 0.1440(12) 0.0893(7) 0.0981(8) -0.0483(5) -0.0043(8) 0.0226(7) C1U 0.0424(7) 0.0447(7) 0.0444(7) -0.0155(5) -0.0010(6) 0.0015(6) Cl1W 0.0850(8) 0.0748(6) 0.0763(7) -0.0124(5) 0.0016(6) -0.0054(6) Cl2W 0.1440(12) 0.0893(7) 0.0981(8) -0.0483(5) -0.0043(8) 0.0226(7) C1W 0.0424(7) 0.0447(7) 0.0444(7) -0.0155(5) -0.0010(6) 0.0015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C7 1.9014(7) . ? Ru1 C8 1.9280(7) . ? Ru1 C4 2.0363(6) . ? Ru1 P3 2.3474(3) . ? Ru1 P1 2.4100(3) . ? Ru1 Ru2 3.1004(4) . ? Ru2 C10 1.8475(8) . ? Ru2 C9 1.8583(7) . ? Ru2 C1 2.2355(10) . ? Ru2 P2 2.3397(3) . ? Ru2 P1 2.3579(3) . ? Ru2 C1A 2.3866(16) . ? Ru2 Ru3 2.9226(4) . ? Ru3 C12 1.8664(8) . ? Ru3 C11 1.9186(7) . ? Ru3 C1 2.0742(11) . ? Ru3 C1A 2.1176(18) . ? Ru3 P2 2.3096(3) . ? Ru3 C4 2.3114(7) . ? Ru3 C5 2.4325(8) . ? P1 C40 1.8286(8) . ? P1 C20 1.8520(7) . ? P2 C70 1.8314(8) . ? P2 C50 1.8364(8) . ? P3 C90 1.8304(7) . ? P3 C100 1.8339(8) . ? P3 C80 1.8374(7) . ? O7 C7 1.1440(9) . ? O8 C8 1.1311(8) . ? O9 C9 1.1396(9) . ? O10 C10 1.1479(10) . ? O11 C11 1.1273(9) . ? O12 C12 1.1316(10) . ? C4 C5 1.2539(8) . ? C5 C6 1.4878(9) . ? C6 C61 1.5217(11) . ? C6 C62 1.5289(11) . ? C6 C63 1.5475(13) . ? C20 C25 1.3833(11) . ? C20 C21 1.3904(12) . ? C21 C22 1.3846(10) . ? C22 C23 1.3704(13) . ? C23 C24 1.3548(16) . ? C24 C25 1.3922(12) . ? C1 C2 1.1946(15) . ? C2 C3 1.4756(15) . ? C3 C31 1.538(2) . ? C3 C32 1.5529(17) . ? C3 C33 1.5666(17) . ? C1A C2A 1.192(2) . ? C2A C3A 1.479(2) . ? C3A C31A 1.534(3) . ? C3A C32A 1.547(3) . ? C3A C33A 1.568(2) . ? C40 C45 1.3965(9) . ? C40 C41 1.3994(11) . ? C41 C42 1.3637(13) . ? C42 C43 1.3786(11) . ? C43 C44 1.3836(12) . ? C44 C45 1.3929(12) . ? C50 C55 1.3802(11) . ? C50 C51 1.3921(10) . ? C51 C52 1.3882(12) . ? C52 C53 1.3750(14) . ? C53 C54 1.3806(12) . ? C54 C55 1.3812(12) . ? C70 C75 1.3846(10) . ? C70 C71 1.3923(10) . ? C71 C72 1.3890(13) . ? C72 C73 1.3645(12) . ? C73 C74 1.3565(11) . ? C74 C75 1.4071(12) . ? C80 C85 1.3808(10) . ? C80 C81 1.3983(12) . ? C81 C82 1.4073(11) . ? C82 C83 1.3592(13) . ? C83 C84 1.3916(13) . ? C84 C85 1.3708(10) . ? C90 C95 1.3863(11) . ? C90 C91 1.4044(10) . ? C91 C92 1.3769(11) . ? C92 C93 1.3771(13) . ? C93 C94 1.3778(12) . ? C94 C95 1.3849(12) . ? C100 C101 1.3673(9) . ? C100 C105 1.3929(10) . ? C101 C102 1.3881(13) . ? C102 C103 1.3788(12) . ? C103 C104 1.3769(11) . ? C104 C105 1.3942(12) . ? Cl1L C1L 1.777(4) . ? Cl2L C1L 1.764(3) . ? Cl1M C1M 1.748(3) . ? Cl2M C1M 1.736(3) . ? Cl1N C1N 1.798(5) . ? Cl2N C1N 1.763(4) . ? Cl1O C1O 1.711(4) . ? Cl2O C1O 1.740(4) . ? Cl1P C1P 1.797(5) . ? Cl2P C1P 1.796(5) . ? Cl1Q C1Q 1.771(3) . ? Cl2Q C1Q 1.774(4) . ? Cl1R C1R 1.794(4) . ? Cl2R C1R 1.784(5) . ? Cl1S C1S 1.771(4) . ? Cl2S C1S 1.776(4) . ? Cl1T C1T 1.806(4) . ? Cl2T C1T 1.782(4) . ? Cl1U C1U 1.796(5) . ? Cl2U C1U 1.779(5) . ? Cl1W C1W 1.799(5) . ? Cl2W C1W 1.790(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Ru1 C8 86.17(3) . . ? C7 Ru1 C4 91.70(3) . . ? C8 Ru1 C4 173.43(3) . . ? C7 Ru1 P3 90.75(2) . . ? C8 Ru1 P3 96.59(2) . . ? C4 Ru1 P3 89.65(2) . . ? C7 Ru1 P1 161.06(2) . . ? C8 Ru1 P1 84.92(2) . . ? C4 Ru1 P1 95.27(2) . . ? P3 Ru1 P1 106.847(11) . . ? C7 Ru1 Ru2 113.99(2) . . ? C8 Ru1 Ru2 86.00(2) . . ? C4 Ru1 Ru2 89.20(2) . . ? P3 Ru1 Ru2 155.255(6) . . ? P1 Ru1 Ru2 48.711(9) . . ? C10 Ru2 C9 88.28(3) . . ? C10 Ru2 C1 100.03(4) . . ? C9 Ru2 C1 166.01(4) . . ? C10 Ru2 P2 103.24(3) . . ? C9 Ru2 P2 94.37(3) . . ? C1 Ru2 P2 72.88(3) . . ? C10 Ru2 P1 106.55(3) . . ? C9 Ru2 P1 94.81(3) . . ? C1 Ru2 P1 93.56(3) . . ? P2 Ru2 P1 149.026(9) . . ? C10 Ru2 C1A 101.59(5) . . ? C9 Ru2 C1A 167.76(5) . . ? C1 Ru2 C1A 4.24(6) . . ? P2 Ru2 C1A 76.45(5) . . ? P1 Ru2 C1A 89.34(5) . . ? C10 Ru2 Ru3 137.45(3) . . ? C9 Ru2 Ru3 122.16(2) . . ? C1 Ru2 Ru3 45.02(3) . . ? P2 Ru2 Ru3 50.593(7) . . ? P1 Ru2 Ru3 100.115(9) . . ? C1A Ru2 Ru3 45.64(4) . . ? C10 Ru2 Ru1 155.31(3) . . ? C9 Ru2 Ru1 86.14(2) . . ? C1 Ru2 Ru1 90.67(3) . . ? P2 Ru2 Ru1 101.161(11) . . ? P1 Ru2 Ru1 50.174(8) . . ? C1A Ru2 Ru1 87.71(4) . . ? Ru3 Ru2 Ru1 63.864(10) . . ? C12 Ru3 C11 86.09(3) . . ? C12 Ru3 C1 91.53(4) . . ? C11 Ru3 C1 168.77(4) . . ? C12 Ru3 C1A 90.41(5) . . ? C11 Ru3 C1A 173.93(6) . . ? C1 Ru3 C1A 6.13(6) . . ? C12 Ru3 P2 100.85(3) . . ? C11 Ru3 P2 93.20(2) . . ? C1 Ru3 P2 76.45(3) . . ? C1A Ru3 P2 82.58(5) . . ? C12 Ru3 C4 120.37(3) . . ? C11 Ru3 C4 100.61(3) . . ? C1 Ru3 C4 90.07(4) . . ? C1A Ru3 C4 85.44(6) . . ? P2 Ru3 C4 137.064(16) . . ? C12 Ru3 C5 89.85(3) . . ? C11 Ru3 C5 100.08(3) . . ? C1 Ru3 C5 90.87(4) . . ? C1A Ru3 C5 84.85(5) . . ? P2 Ru3 C5 163.507(17) . . ? C4 Ru3 C5 30.52(2) . . ? C12 Ru3 Ru2 133.32(2) . . ? C11 Ru3 Ru2 126.40(2) . . ? C1 Ru3 Ru2 49.67(3) . . ? C1A Ru3 Ru2 53.69(4) . . ? P2 Ru3 Ru2 51.514(9) . . ? C4 Ru3 Ru2 88.720(16) . . ? C5 Ru3 Ru2 112.131(18) . . ? C40 P1 C20 101.90(4) . . ? C40 P1 Ru2 118.67(3) . . ? C20 P1 Ru2 115.12(3) . . ? C40 P1 Ru1 126.07(2) . . ? C20 P1 Ru1 114.08(3) . . ? Ru2 P1 Ru1 81.115(11) . . ? C70 P2 C50 102.71(4) . . ? C70 P2 Ru3 122.57(2) . . ? C50 P2 Ru3 118.94(2) . . ? C70 P2 Ru2 114.19(3) . . ? C50 P2 Ru2 120.40(2) . . ? Ru3 P2 Ru2 77.893(12) . . ? C90 P3 C100 100.86(3) . . ? C90 P3 C80 102.26(3) . . ? C100 P3 C80 101.81(3) . . ? C90 P3 Ru1 114.03(3) . . ? C100 P3 Ru1 119.46(2) . . ? C80 P3 Ru1 115.91(2) . . ? C5 C4 Ru1 173.25(6) . . ? C5 C4 Ru3 80.09(5) . . ? Ru1 C4 Ru3 94.15(3) . . ? C4 C5 C6 158.37(8) . . ? C4 C5 Ru3 69.40(4) . . ? C6 C5 Ru3 131.91(5) . . ? C5 C6 C61 110.80(7) . . ? C5 C6 C62 109.94(6) . . ? C61 C6 C62 110.28(7) . . ? C5 C6 C63 106.80(6) . . ? C61 C6 C63 110.19(6) . . ? C62 C6 C63 108.75(7) . . ? O7 C7 Ru1 178.85(5) . . ? O8 C8 Ru1 175.62(6) . . ? O9 C9 Ru2 175.64(7) . . ? O10 C10 Ru2 177.04(8) . . ? O11 C11 Ru3 175.53(6) . . ? O12 C12 Ru3 179.32(8) . . ? C25 C20 C21 118.38(7) . . ? C25 C20 P1 122.32(7) . . ? C21 C20 P1 119.28(5) . . ? C22 C21 C20 120.36(7) . . ? C23 C22 C21 120.83(9) . . ? C24 C23 C22 119.03(8) . . ? C23 C24 C25 121.53(9) . . ? C20 C25 C24 119.86(9) . . ? C2 C1 Ru3 168.24(11) . . ? C2 C1 Ru2 101.39(7) . . ? Ru3 C1 Ru2 85.31(4) . . ? C1 C2 C3 169.45(10) . . ? C2 C3 C31 109.37(11) . . ? C2 C3 C32 105.44(9) . . ? C31 C3 C32 112.02(10) . . ? C2 C3 C33 111.79(10) . . ? C31 C3 C33 108.89(10) . . ? C32 C3 C33 109.32(11) . . ? C2A C1A Ru3 158.30(18) . . ? C2A C1A Ru2 107.15(12) . . ? Ru3 C1A Ru2 80.67(6) . . ? C1A C2A C3A 170.11(17) . . ? C2A C3A C31A 108.78(17) . . ? C2A C3A C32A 105.99(14) . . ? C31A C3A C32A 112.75(15) . . ? C2A C3A C33A 110.80(14) . . ? C31A C3A C33A 108.64(15) . . ? C32A C3A C33A 109.88(18) . . ? C45 C40 C41 118.43(7) . . ? C45 C40 P1 119.67(6) . . ? C41 C40 P1 121.89(5) . . ? C42 C41 C40 120.40(7) . . ? C41 C42 C43 121.66(8) . . ? C42 C43 C44 118.89(8) . . ? C43 C44 C45 120.42(7) . . ? C44 C45 C40 120.18(7) . . ? C55 C50 C51 118.32(7) . . ? C55 C50 P2 123.73(6) . . ? C51 C50 P2 117.88(6) . . ? C52 C51 C50 120.39(8) . . ? C53 C52 C51 120.62(8) . . ? C52 C53 C54 119.17(8) . . ? C53 C54 C55 120.36(8) . . ? C50 C55 C54 121.14(8) . . ? C75 C70 C71 118.18(7) . . ? C75 C70 P2 123.90(5) . . ? C71 C70 P2 117.91(6) . . ? C72 C71 C70 121.09(7) . . ? C73 C72 C71 119.91(7) . . ? C74 C73 C72 120.30(8) . . ? C73 C74 C75 120.70(8) . . ? C70 C75 C74 119.81(6) . . ? C85 C80 C81 117.59(6) . . ? C85 C80 P3 119.59(6) . . ? C81 C80 P3 122.80(5) . . ? C80 C81 C82 119.78(7) . . ? C83 C82 C81 120.54(9) . . ? C82 C83 C84 120.24(7) . . ? C85 C84 C83 118.84(7) . . ? C84 C85 C80 122.86(8) . . ? C95 C90 C91 117.63(6) . . ? C95 C90 P3 123.08(6) . . ? C91 C90 P3 119.14(5) . . ? C92 C91 C90 121.46(7) . . ? C91 C92 C93 119.57(7) . . ? C92 C93 C94 120.28(7) . . ? C93 C94 C95 120.08(8) . . ? C94 C95 C90 120.99(7) . . ? C101 C100 C105 118.85(7) . . ? C101 C100 P3 122.79(6) . . ? C105 C100 P3 118.09(5) . . ? C100 C101 C102 121.04(7) . . ? C103 C102 C101 120.12(7) . . ? C104 C103 C102 119.69(8) . . ? C103 C104 C105 119.93(7) . . ? C100 C105 C104 120.36(6) . . ? Cl2L C1L Cl1L 102.31(19) . . ? Cl2M C1M Cl1M 107.61(19) . . ? Cl2N C1N Cl1N 98.2(3) . . ? Cl1O C1O Cl2O 131.0(3) . . ? Cl2P C1P Cl1P 116.5(3) . . ? Cl1Q C1Q Cl2Q 102.35(18) . . ? Cl2R C1R Cl1R 109.9(2) . . ? Cl1S C1S Cl2S 109.9(2) . . ? Cl2T C1T Cl1T 97.7(2) . . ? Cl2U C1U Cl1U 106.8(3) . . ? Cl2W C1W Cl1W 107.2(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.555 _refine_diff_density_min -1.233 _refine_diff_density_rms 0.149