Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_c:\word_f~1\papers\inorga~1\mkw\august~1\k03mkw~4\k03mkw5 _database_code_depnum_ccdc_archive 'CCDC 250924' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H42 Cl4 O2 P2 Ru' _chemical_formula_weight 631.36 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbn21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.4470(1) _cell_length_b 16.1500(1) _cell_length_c 18.4840(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2820.09(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Tabloid _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 1.064 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69600 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 33.14 _reflns_number_total 10642 _reflns_number_gt 9715 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+1.9535*P+(0.0330P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_number_reflns 10642 _refine_ls_number_parameters 283 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.705889(13) 0.217994(7) 0.116591(11) 0.01862(3) Uani 1 1 d . . . Cl1 Cl 0.59194(8) 0.29812(4) 0.02046(4) 0.03638(13) Uani 1 1 d . . . Cl2 Cl 0.61845(7) 0.32007(3) 0.20436(3) 0.03248(12) Uani 1 1 d . . . Cl3 Cl 1.23775(13) -0.06516(9) 0.19544(10) 0.0976(5) Uani 1 1 d . . . Cl4 Cl 1.24523(13) -0.07086(11) 0.03862(10) 0.1059(6) Uani 1 1 d . . . P1 P 0.80492(6) 0.12271(4) 0.03272(3) 0.01992(11) Uani 1 1 d . . . P2 P 0.80426(6) 0.13312(4) 0.20876(3) 0.01905(10) Uani 1 1 d . . . O1 O 0.39974(19) 0.15929(12) 0.13368(12) 0.0440(5) Uani 1 1 d . . . O2 O 0.9272(2) 0.35122(12) 0.09544(11) 0.0416(4) Uani 1 1 d . . . C1 C 0.5155(2) 0.17176(13) 0.12678(14) 0.0302(5) Uani 1 1 d . . . C2 C 0.8588(2) 0.29787(15) 0.10428(12) 0.0297(5) Uani 1 1 d . . . C3 C 0.8686(2) 0.03416(12) 0.08690(11) 0.0225(4) Uani 1 1 d . . . H3A H 0.7911 -0.0067 0.0914 0.027 Uiso 1 1 calc R . . H3B H 0.9474 0.0071 0.0607 0.027 Uiso 1 1 calc R . . C4 C 0.9195(2) 0.05741(12) 0.16257(10) 0.0220(4) Uani 1 1 d . . . H4A H 1.0161 0.0807 0.1590 0.026 Uiso 1 1 calc R . . H4B H 0.9250 0.0066 0.1924 0.026 Uiso 1 1 calc R . . C5 C 0.9698(3) 0.16030(15) -0.01661(12) 0.0300(4) Uani 1 1 d . . . C6 C 0.9388(3) 0.24251(17) -0.05694(15) 0.0398(6) Uani 1 1 d . . . H6A H 0.8732 0.2761 -0.0282 0.060 Uiso 1 1 calc R . . H6B H 0.8962 0.2303 -0.1041 0.060 Uiso 1 1 calc R . . H6C H 1.0274 0.2730 -0.0640 0.060 Uiso 1 1 calc R . . C7 C 1.0288(4) 0.09756(18) -0.07205(15) 0.0418(7) Uani 1 1 d . . . H7A H 1.1165 0.1193 -0.0930 0.063 Uiso 1 1 calc R . . H7B H 0.9590 0.0888 -0.1105 0.063 Uiso 1 1 calc R . . H7C H 1.0483 0.0448 -0.0477 0.063 Uiso 1 1 calc R . . C8 C 1.0893(2) 0.17264(16) 0.03876(14) 0.0341(5) Uani 1 1 d . . . H8A H 1.1182 0.1188 0.0581 0.051 Uiso 1 1 calc R . . H8B H 1.0555 0.2079 0.0783 0.051 Uiso 1 1 calc R . . H8C H 1.1703 0.1992 0.0151 0.051 Uiso 1 1 calc R . . C9 C 0.6840(3) 0.07185(16) -0.03627(14) 0.0293(5) Uani 1 1 d . . . C10 C 0.6674(4) 0.12758(18) -0.10373(14) 0.0410(6) Uani 1 1 d . . . H10A H 0.5946 0.1043 -0.1356 0.062 Uiso 1 1 calc R . . H10B H 0.7577 0.1304 -0.1297 0.062 Uiso 1 1 calc R . . H10C H 0.6392 0.1834 -0.0886 0.062 Uiso 1 1 calc R . . C11 C 0.7363(3) -0.01410(17) -0.05909(15) 0.0408(6) Uani 1 1 d . . . H11A H 0.7364 -0.0510 -0.0170 0.061 Uiso 1 1 calc R . . H11B H 0.8326 -0.0097 -0.0784 0.061 Uiso 1 1 calc R . . H11C H 0.6734 -0.0366 -0.0964 0.061 Uiso 1 1 calc R . . C12 C 0.5363(3) 0.06207(18) -0.00464(14) 0.0395(6) Uani 1 1 d . . . H12A H 0.4812 0.0240 -0.0348 0.059 Uiso 1 1 calc R . . H12B H 0.4893 0.1161 -0.0033 0.059 Uiso 1 1 calc R . . H12C H 0.5432 0.0398 0.0445 0.059 Uiso 1 1 calc R . . C13 C 0.6726(3) 0.06656(15) 0.26018(13) 0.0269(5) Uani 1 1 d . . . C14 C 0.6103(3) 0.00284(14) 0.20666(13) 0.0309(4) Uani 1 1 d . . . H14A H 0.5329 -0.0274 0.2301 0.046 Uiso 1 1 calc R . . H14B H 0.6844 -0.0362 0.1921 0.046 Uiso 1 1 calc R . . H14C H 0.5742 0.0317 0.1638 0.046 Uiso 1 1 calc R . . C15 C 0.7409(3) 0.01336(18) 0.32013(14) 0.0378(5) Uani 1 1 d . . . H15A H 0.6709 -0.0258 0.3391 0.057 Uiso 1 1 calc R . . H15B H 0.7738 0.0494 0.3593 0.057 Uiso 1 1 calc R . . H15C H 0.8214 -0.0172 0.3000 0.057 Uiso 1 1 calc R . . C16 C 0.5534(3) 0.11884(16) 0.29331(14) 0.0358(5) Uani 1 1 d . . . H16A H 0.5284 0.1637 0.2600 0.054 Uiso 1 1 calc R . . H16B H 0.5855 0.1424 0.3394 0.054 Uiso 1 1 calc R . . H16C H 0.4703 0.0838 0.3017 0.054 Uiso 1 1 calc R . . C17 C 0.9270(3) 0.18253(14) 0.27858(13) 0.0293(4) Uani 1 1 d . . . C18 C 1.0105(3) 0.25265(17) 0.24255(15) 0.0387(5) Uani 1 1 d . . . H18A H 1.0811 0.2742 0.2766 0.058 Uiso 1 1 calc R . . H18B H 0.9455 0.2972 0.2287 0.058 Uiso 1 1 calc R . . H18C H 1.0584 0.2314 0.1993 0.058 Uiso 1 1 calc R . . C19 C 0.8412(3) 0.22206(17) 0.34062(15) 0.0412(6) Uani 1 1 d . . . H19A H 0.9031 0.2580 0.3693 0.062 Uiso 1 1 calc R . . H19B H 0.8024 0.1784 0.3716 0.062 Uiso 1 1 calc R . . H19C H 0.7635 0.2549 0.3203 0.062 Uiso 1 1 calc R . . C20 C 1.0355(4) 0.12052(19) 0.30861(16) 0.0423(7) Uani 1 1 d . . . H20A H 1.1021 0.1050 0.2703 0.064 Uiso 1 1 calc R . . H20B H 0.9861 0.0710 0.3260 0.064 Uiso 1 1 calc R . . H20C H 1.0874 0.1460 0.3488 0.064 Uiso 1 1 calc R . . C21 C 1.1979(3) -0.12333(17) 0.1175(3) 0.0520(7) Uani 1 1 d . . . H21A H 1.2490 -0.1768 0.1195 0.062 Uiso 1 1 calc R . . H21B H 1.0951 -0.1353 0.1165 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02038(5) 0.01403(5) 0.02143(6) 0.00005(6) -0.00094(7) 0.00129(4) Cl1 0.0438(3) 0.0308(2) 0.0345(3) 0.0090(2) -0.0042(2) 0.0107(2) Cl2 0.0369(3) 0.0244(2) 0.0360(3) -0.0062(2) 0.0027(2) 0.0067(2) Cl3 0.0445(5) 0.0894(8) 0.1588(14) -0.0473(9) -0.0407(7) 0.0114(5) Cl4 0.0414(5) 0.1298(12) 0.1465(13) 0.0933(11) 0.0111(7) 0.0001(6) P1 0.0254(3) 0.0166(2) 0.0177(2) -0.00022(18) -0.00125(19) 0.00139(18) P2 0.0223(3) 0.0168(2) 0.0180(2) -0.00045(18) -0.00262(19) 0.00073(17) O1 0.0274(8) 0.0429(10) 0.0617(15) 0.0010(9) -0.0035(7) -0.0006(7) O2 0.0454(10) 0.0334(9) 0.0459(11) -0.0022(7) 0.0052(8) -0.0010(8) C1 0.0326(9) 0.0218(8) 0.0362(14) 0.0017(8) -0.0031(9) 0.0019(7) C2 0.0287(9) 0.0342(11) 0.0263(13) -0.0018(8) 0.0014(7) 0.0042(8) C3 0.0279(9) 0.0177(8) 0.0220(8) 0.0001(7) -0.0018(7) 0.0042(7) C4 0.0241(9) 0.0220(9) 0.0201(8) 0.0008(7) -0.0044(7) 0.0027(7) C5 0.0351(11) 0.0287(10) 0.0262(10) 0.0017(8) 0.0084(9) 0.0021(9) C6 0.0526(15) 0.0335(12) 0.0334(12) 0.0085(10) 0.0125(11) -0.0026(11) C7 0.0493(16) 0.0441(15) 0.0319(12) -0.0063(11) 0.0170(12) 0.0075(13) C8 0.0269(10) 0.0332(11) 0.0422(13) -0.0016(9) 0.0085(9) -0.0023(8) C9 0.0402(13) 0.0263(11) 0.0215(10) -0.0012(8) -0.0086(9) -0.0005(10) C10 0.0607(17) 0.0367(13) 0.0258(11) 0.0025(9) -0.0159(11) 0.0043(12) C11 0.0596(17) 0.0283(11) 0.0344(13) -0.0100(10) -0.0130(12) 0.0026(11) C12 0.0390(13) 0.0427(13) 0.0367(13) -0.0043(11) -0.0143(10) -0.0088(11) C13 0.0350(12) 0.0230(10) 0.0226(10) 0.0028(8) 0.0038(9) -0.0002(9) C14 0.0334(11) 0.0251(9) 0.0342(11) 0.0040(8) -0.0005(9) -0.0068(8) C15 0.0520(15) 0.0364(13) 0.0251(11) 0.0076(9) -0.0008(10) 0.0006(11) C16 0.0395(13) 0.0342(12) 0.0339(12) -0.0014(9) 0.0137(10) -0.0011(10) C17 0.0342(11) 0.0279(10) 0.0257(10) -0.0048(8) -0.0102(8) -0.0001(9) C18 0.0424(13) 0.0353(13) 0.0384(13) -0.0037(10) -0.0128(11) -0.0112(11) C19 0.0500(15) 0.0436(15) 0.0300(12) -0.0165(10) -0.0044(11) -0.0039(12) C20 0.0457(16) 0.0425(15) 0.0388(14) -0.0016(11) -0.0221(12) 0.0020(12) C21 0.0404(12) 0.0394(12) 0.0763(19) 0.013(2) -0.002(2) -0.0054(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 1.950(2) . ? Ru1 C1 1.956(2) . ? Ru1 P2 2.3759(6) . ? Ru1 P1 2.3763(6) . ? Ru1 Cl1 2.4475(6) . ? Ru1 Cl2 2.4560(6) . ? Cl3 C21 1.760(5) . ? Cl4 C21 1.745(4) . ? P1 C3 1.847(2) . ? P1 C9 1.899(3) . ? P1 C5 1.904(2) . ? P2 C4 1.846(2) . ? P2 C13 1.899(3) . ? P2 C17 1.910(2) . ? O1 C1 1.120(3) . ? O2 C2 1.090(3) . ? C3 C4 1.526(3) . ? C5 C8 1.537(4) . ? C5 C7 1.545(3) . ? C5 C6 1.550(3) . ? C9 C12 1.522(4) . ? C9 C11 1.533(4) . ? C9 C10 1.546(4) . ? C13 C16 1.534(4) . ? C13 C14 1.544(3) . ? C13 C15 1.544(4) . ? C17 C18 1.532(4) . ? C17 C20 1.536(4) . ? C17 C19 1.543(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 C2 Ru1 C1 160.86(9) . . ? C2 Ru1 P2 100.11(7) . . ? C1 Ru1 P2 94.03(7) . . ? C2 Ru1 P1 93.48(7) . . ? C1 Ru1 P1 100.23(7) . . ? P2 Ru1 P1 86.570(18) . . ? C2 Ru1 Cl1 83.76(7) . . ? C1 Ru1 Cl1 82.38(7) . . ? P2 Ru1 Cl1 176.04(2) . . ? P1 Ru1 Cl1 92.40(2) . . ? C2 Ru1 Cl2 83.23(7) . . ? C1 Ru1 Cl2 83.31(7) . . ? P2 Ru1 Cl2 92.59(2) . . ? P1 Ru1 Cl2 176.41(2) . . ? Cl1 Ru1 Cl2 88.67(2) . . ? C3 P1 C9 103.01(11) . . ? C3 P1 C5 103.90(11) . . ? C9 P1 C5 107.96(12) . . ? C3 P1 Ru1 106.02(7) . . ? C9 P1 Ru1 118.78(9) . . ? C5 P1 Ru1 115.34(8) . . ? C4 P2 C13 104.05(10) . . ? C4 P2 C17 103.36(10) . . ? C13 P2 C17 107.23(11) . . ? C4 P2 Ru1 106.33(6) . . ? C13 P2 Ru1 115.41(9) . . ? C17 P2 Ru1 118.75(8) . . ? O1 C1 Ru1 167.9(2) . . ? O2 C2 Ru1 168.6(2) . . ? C4 C3 P1 114.16(14) . . ? C3 C4 P2 113.65(14) . . ? C8 C5 C7 105.2(2) . . ? C8 C5 C6 110.4(2) . . ? C7 C5 C6 108.1(2) . . ? C8 C5 P1 108.86(15) . . ? C7 C5 P1 113.80(18) . . ? C6 C5 P1 110.42(17) . . ? C12 C9 C11 107.9(2) . . ? C12 C9 C10 106.1(2) . . ? C11 C9 C10 109.8(2) . . ? C12 C9 P1 109.80(17) . . ? C11 C9 P1 112.51(19) . . ? C10 C9 P1 110.55(19) . . ? C16 C13 C14 110.1(2) . . ? C16 C13 C15 109.1(2) . . ? C14 C13 C15 104.4(2) . . ? C16 C13 P2 111.63(17) . . ? C14 C13 P2 107.82(16) . . ? C15 C13 P2 113.6(2) . . ? C18 C17 C20 107.2(2) . . ? C18 C17 C19 106.7(2) . . ? C20 C17 C19 110.6(2) . . ? C18 C17 P2 109.13(16) . . ? C20 C17 P2 112.13(17) . . ? C19 C17 P2 110.84(17) . . ? Cl4 C21 Cl3 111.71(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.418 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.071 data_c:\word_f~1\papers\inorga~1\mkw\august~1\k03mkw2\k03mkw2 _database_code_depnum_ccdc_archive 'CCDC 250925' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H83 Cl11 F6 O8 P4 Ru2 S2' _chemical_formula_weight 1622.18 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 '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 Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.8689(1) _cell_length_b 20.1360(2) _cell_length_c 31.2785(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6845.49(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description tabloid _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3304 _exptl_absorpt_coefficient_mu 1.084 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.681 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details ? _exptl_special_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 102369 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 30.00 _reflns_number_total 19835 _reflns_number_gt 16545 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+8.3294*P+(0.0453P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(2) _refine_ls_number_reflns 19835 _refine_ls_number_parameters 818 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.30330(2) -0.027181(13) 0.351432(8) 0.02039(6) Uani 1 1 d . . . Ru2 Ru 0.18121(2) 0.026328(14) 0.246967(8) 0.02136(6) Uani 1 1 d . . . Cl1 Cl 0.12871(8) 0.03969(4) 0.32379(3) 0.02558(17) Uani 1 1 d . . . Cl2 Cl 0.33312(9) -0.05414(4) 0.27503(3) 0.02667(18) Uani 1 1 d . . . Cl3 Cl 0.21692(13) 0.19446(8) 0.04240(6) 0.0746(5) Uani 1 1 d . . . Cl4 Cl 0.00160(19) 0.25671(9) 0.00700(4) 0.0780(5) Uani 1 1 d . . . Cl5 Cl 0.03835(14) 0.25636(6) 0.09737(4) 0.0518(3) Uani 1 1 d . . . Cl6 Cl -0.2081(2) 0.15624(12) 0.39329(9) 0.1171(9) Uani 1 1 d . . . Cl7 Cl -0.06707(19) 0.23861(11) 0.44872(12) 0.1378(12) Uani 1 1 d . . . Cl8 Cl -0.33024(16) 0.25108(8) 0.44539(9) 0.0969(7) Uani 1 1 d . . . Cl9 Cl 0.5775(3) -0.13191(17) 0.05083(12) 0.1098(9) Uani 0.75 1 d PD A 1 Cl10 Cl 0.8341(4) -0.1552(3) 0.04525(13) 0.177(2) Uani 0.75 1 d PD A 1 Cl11 Cl 0.7193(4) -0.16502(17) 0.12577(13) 0.1220(16) Uani 0.75 1 d PD A 1 Cl9A Cl 0.5660(8) -0.1630(4) 0.1030(4) 0.115(4) Uani 0.25 1 d PD B 2 Cl9B Cl 0.7242(7) -0.1319(4) 0.1741(4) 0.098(3) Uani 0.25 1 d PD B 2 Cl9C Cl 0.8202(8) -0.1910(5) 0.0973(7) 0.215(10) Uani 0.25 1 d PD B 2 S1 S 0.43238(9) 0.09276(5) 0.29239(3) 0.02675(18) Uani 1 1 d . . . S1A S 0.8543(2) 0.03238(11) 0.04679(7) 0.0384(4) Uani 0.50 1 d P C 1 S1B S 0.8332(2) 0.07460(12) 0.07240(8) 0.0458(5) Uani 0.50 1 d P D 3 P1 P 0.27307(10) 0.00173(5) 0.42416(3) 0.0266(2) Uani 1 1 d . . . P2 P 0.46453(9) -0.09730(5) 0.37624(3) 0.0267(2) Uani 1 1 d . . . P3 P 0.03350(9) 0.10451(5) 0.22287(3) 0.02568(19) Uani 1 1 d . . . P4 P 0.23107(10) 0.01044(5) 0.17331(3) 0.0307(2) Uani 1 1 d . . . F1 F 0.5640(3) 0.18205(15) 0.33117(10) 0.0572(8) Uani 1 1 d . . . F2 F 0.3749(3) 0.21034(12) 0.32298(9) 0.0497(7) Uani 1 1 d . . . F3 F 0.4975(3) 0.21119(14) 0.26900(10) 0.0612(9) Uani 1 1 d . . . F1A F 0.7798(8) 0.1502(4) 0.0665(3) 0.085(3) Uani 0.50 1 d P C 1 F2A F 0.6302(14) 0.0906(11) 0.0366(4) 0.076(6) Uani 0.50 1 d P C 1 F3A F 0.7747(14) 0.1315(6) -0.0045(3) 0.048(2) Uani 0.50 1 d P C 1 F1B F 0.7842(18) 0.1262(10) 0.0054(5) 0.115(7) Uani 0.50 1 d P D 3 F2B F 0.7357(10) 0.0232(5) 0.0035(3) 0.105(3) Uani 0.50 1 d P D 3 F3B F 0.635(2) 0.0994(11) 0.0402(7) 0.101(7) Uani 0.50 1 d P D 3 O1 O 0.3241(2) 0.09986(12) 0.26505(8) 0.0266(5) Uani 1 1 d . . . O2 O 0.4066(2) 0.06447(12) 0.33438(8) 0.0256(5) Uani 1 1 d . . . O3 O 0.5402(3) 0.06837(15) 0.27163(9) 0.0365(6) Uani 1 1 d . . . O4 O 0.1188(3) -0.13377(14) 0.34459(9) 0.0374(7) Uani 1 1 d . . . O5 O 0.0204(3) -0.09140(14) 0.25185(10) 0.0429(7) Uani 1 1 d . . . O1A O 0.8261(9) -0.0107(4) 0.0120(3) 0.067(2) Uani 0.50 1 d P C 1 O2A O 0.9779(18) 0.0594(13) 0.0452(6) 0.047(3) Uani 0.50 1 d P C 1 O3A O 0.8153(16) 0.0076(7) 0.0873(4) 0.061(3) Uani 0.50 1 d P C 1 O1B O 0.8251(9) 0.1400(4) 0.0903(2) 0.056(2) Uani 0.50 1 d P D 3 O2B O 0.9510(17) 0.0570(13) 0.0554(6) 0.057(4) Uani 0.50 1 d P D 3 O3B O 0.7788(16) 0.0236(7) 0.0979(4) 0.059(4) Uani 0.50 1 d P D 3 C1 C 0.4696(4) 0.1794(2) 0.30503(14) 0.0393(10) Uani 1 1 d . . . C2 C 0.1934(4) -0.09450(18) 0.35125(11) 0.0290(7) Uani 1 1 d . . . C3 C 0.0763(4) -0.04337(19) 0.24642(13) 0.0313(8) Uani 1 1 d . . . C4 C 0.3638(4) -0.0586(2) 0.45588(12) 0.0350(9) Uani 1 1 d . . . H4A H 0.3857 -0.0378 0.4836 0.042 Uiso 1 1 calc R . . H4B H 0.3115 -0.0976 0.4621 0.042 Uiso 1 1 calc R . . C5 C 0.4811(4) -0.0822(2) 0.43417(12) 0.0332(9) Uani 1 1 d . . . H5A H 0.5085 -0.1239 0.4481 0.040 Uiso 1 1 calc R . . H5B H 0.5462 -0.0485 0.4386 0.040 Uiso 1 1 calc R . . C6 C 0.3359(5) 0.0867(2) 0.43947(12) 0.0402(10) Uani 1 1 d . . . C7 C 0.3169(7) 0.1044(3) 0.48690(14) 0.0598(15) Uani 1 1 d . . . H7A H 0.3574 0.1467 0.4932 0.090 Uiso 1 1 calc R . . H7B H 0.3525 0.0694 0.5049 0.090 Uiso 1 1 calc R . . H7C H 0.2287 0.1082 0.4929 0.090 Uiso 1 1 calc R . . C8 C 0.2753(5) 0.1408(2) 0.41176(16) 0.0468(12) Uani 1 1 d . . . H8A H 0.1920 0.1496 0.4223 0.070 Uiso 1 1 calc R . . H8B H 0.2712 0.1256 0.3820 0.070 Uiso 1 1 calc R . . H8C H 0.3242 0.1816 0.4133 0.070 Uiso 1 1 calc R . . C9 C 0.4739(5) 0.0855(2) 0.43174(15) 0.0463(11) Uani 1 1 d . . . H9A H 0.4905 0.0683 0.4030 0.069 Uiso 1 1 calc R . . H9B H 0.5134 0.0569 0.4530 0.069 Uiso 1 1 calc R . . H9C H 0.5068 0.1307 0.4342 0.069 Uiso 1 1 calc R . . C10 C 0.1136(4) -0.0072(2) 0.44847(13) 0.0361(9) Uani 1 1 d . . . C11 C 0.0333(5) 0.0530(3) 0.43894(16) 0.0519(13) Uani 1 1 d . . . H11A H -0.0508 0.0445 0.4488 0.078 Uiso 1 1 calc R . . H11B H 0.0326 0.0614 0.4081 0.078 Uiso 1 1 calc R . . H11C H 0.0664 0.0920 0.4538 0.078 Uiso 1 1 calc R . . C12 C 0.1215(5) -0.0178(3) 0.49741(13) 0.0492(12) Uani 1 1 d . . . H12A H 0.1694 0.0183 0.5103 0.074 Uiso 1 1 calc R . . H12B H 0.1617 -0.0604 0.5034 0.074 Uiso 1 1 calc R . . H12C H 0.0384 -0.0180 0.5096 0.074 Uiso 1 1 calc R . . C13 C 0.0477(5) -0.0682(2) 0.42990(15) 0.0459(11) Uani 1 1 d . . . H13A H -0.0303 -0.0750 0.4450 0.069 Uiso 1 1 calc R . . H13B H 0.0999 -0.1075 0.4334 0.069 Uiso 1 1 calc R . . H13C H 0.0316 -0.0610 0.3994 0.069 Uiso 1 1 calc R . . C14 C 0.4268(4) -0.19012(19) 0.37265(14) 0.0363(9) Uani 1 1 d . . . C15 C 0.3240(5) -0.2048(2) 0.40487(15) 0.0417(10) Uani 1 1 d . . . H15A H 0.2601 -0.1707 0.4026 0.063 Uiso 1 1 calc R . . H15B H 0.3581 -0.2047 0.4339 0.063 Uiso 1 1 calc R . . H15C H 0.2883 -0.2484 0.3988 0.063 Uiso 1 1 calc R . . C16 C 0.5348(5) -0.2351(2) 0.38512(18) 0.0513(13) Uani 1 1 d . . . H16A H 0.5039 -0.2796 0.3919 0.077 Uiso 1 1 calc R . . H16B H 0.5765 -0.2166 0.4102 0.077 Uiso 1 1 calc R . . H16C H 0.5929 -0.2379 0.3612 0.077 Uiso 1 1 calc R . . C17 C 0.3881(5) -0.2091(2) 0.32720(16) 0.0448(11) Uani 1 1 d . . . H17A H 0.3731 -0.2570 0.3258 0.067 Uiso 1 1 calc R . . H17B H 0.4539 -0.1972 0.3072 0.067 Uiso 1 1 calc R . . H17C H 0.3128 -0.1851 0.3196 0.067 Uiso 1 1 calc R . . C18 C 0.6276(4) -0.0832(2) 0.35588(14) 0.0361(9) Uani 1 1 d . . . C19 C 0.6594(4) -0.0096(2) 0.35911(16) 0.0423(10) Uani 1 1 d . . . H19A H 0.7434 -0.0024 0.3487 0.063 Uiso 1 1 calc R . . H19B H 0.6538 0.0046 0.3890 0.063 Uiso 1 1 calc R . . H19C H 0.6017 0.0162 0.3417 0.063 Uiso 1 1 calc R . . C20 C 0.6369(5) -0.1046(3) 0.30862(15) 0.0491(12) Uani 1 1 d . . . H20A H 0.5758 -0.0803 0.2917 0.074 Uiso 1 1 calc R . . H20B H 0.6214 -0.1524 0.3063 0.074 Uiso 1 1 calc R . . H20C H 0.7195 -0.0946 0.2978 0.074 Uiso 1 1 calc R . . C21 C 0.7264(5) -0.1199(3) 0.38180(19) 0.0554(14) Uani 1 1 d . . . H21A H 0.7238 -0.1673 0.3749 0.083 Uiso 1 1 calc R . . H21B H 0.7108 -0.1136 0.4124 0.083 Uiso 1 1 calc R . . H21C H 0.8077 -0.1020 0.3746 0.083 Uiso 1 1 calc R . . C22 C 0.0228(4) 0.0938(2) 0.16447(12) 0.0343(9) Uani 1 1 d . . . H22A H -0.0409 0.0600 0.1583 0.041 Uiso 1 1 calc R . . H22B H -0.0048 0.1363 0.1517 0.041 Uiso 1 1 calc R . . C23 C 0.1427(4) 0.0728(2) 0.14282(12) 0.0374(9) Uani 1 1 d . . . H23A H 0.1947 0.1126 0.1386 0.045 Uiso 1 1 calc R . . H23B H 0.1233 0.0544 0.1143 0.045 Uiso 1 1 calc R . . C24 C 0.0784(4) 0.19448(19) 0.23216(14) 0.0351(9) Uani 1 1 d . . . C25 C -0.0185(5) 0.2447(2) 0.21622(17) 0.0456(11) Uani 1 1 d . . . H25A H -0.0923 0.2416 0.2341 0.068 Uiso 1 1 calc R . . H25B H -0.0400 0.2345 0.1865 0.068 Uiso 1 1 calc R . . H25C H 0.0153 0.2897 0.2179 0.068 Uiso 1 1 calc R . . C26 C 0.1949(5) 0.2077(2) 0.20611(15) 0.0425(10) Uani 1 1 d . . . H26A H 0.1766 0.2029 0.1756 0.064 Uiso 1 1 calc R . . H26B H 0.2588 0.1758 0.2143 0.064 Uiso 1 1 calc R . . H26C H 0.2241 0.2529 0.2118 0.064 Uiso 1 1 calc R . . C27 C 0.1051(5) 0.2070(2) 0.27962(15) 0.0408(10) Uani 1 1 d . . . H27A H 0.1467 0.2499 0.2829 0.061 Uiso 1 1 calc R . . H27B H 0.1581 0.1716 0.2907 0.061 Uiso 1 1 calc R . . H27C H 0.0276 0.2076 0.2956 0.061 Uiso 1 1 calc R . . C28 C -0.1327(4) 0.0946(2) 0.23968(14) 0.0356(9) Uani 1 1 d . . . C29 C -0.1557(4) 0.1234(3) 0.28460(14) 0.0461(11) Uani 1 1 d . . . H29A H -0.2383 0.1108 0.2943 0.069 Uiso 1 1 calc R . . H29B H -0.1493 0.1719 0.2836 0.069 Uiso 1 1 calc R . . H29C H -0.0943 0.1057 0.3045 0.069 Uiso 1 1 calc R . . C30 C -0.2214(4) 0.1274(3) 0.20753(17) 0.0496(12) Uani 1 1 d . . . H30A H -0.2210 0.1023 0.1807 0.074 Uiso 1 1 calc R . . H30B H -0.1947 0.1731 0.2020 0.074 Uiso 1 1 calc R . . H30C H -0.3048 0.1278 0.2194 0.074 Uiso 1 1 calc R . . C31 C -0.1679(4) 0.0210(2) 0.24190(16) 0.0464(11) Uani 1 1 d . . . H31A H -0.2568 0.0169 0.2464 0.070 Uiso 1 1 calc R . . H31B H -0.1241 -0.0002 0.2657 0.070 Uiso 1 1 calc R . . H31C H -0.1454 -0.0009 0.2150 0.070 Uiso 1 1 calc R . . C32 C 0.1812(5) -0.0728(2) 0.15044(13) 0.0412(10) Uani 1 1 d . . . C33 C 0.0400(5) -0.0731(2) 0.14837(15) 0.0455(11) Uani 1 1 d . . . H33A H 0.0108 -0.1188 0.1445 0.068 Uiso 1 1 calc R . . H33B H 0.0127 -0.0458 0.1242 0.068 Uiso 1 1 calc R . . H33C H 0.0065 -0.0550 0.1750 0.068 Uiso 1 1 calc R . . C34 C 0.2295(6) -0.1301(2) 0.17728(17) 0.0536(13) Uani 1 1 d . . . H34A H 0.2051 -0.1238 0.2072 0.080 Uiso 1 1 calc R . . H34B H 0.3195 -0.1316 0.1753 0.080 Uiso 1 1 calc R . . H34C H 0.1951 -0.1720 0.1666 0.080 Uiso 1 1 calc R . . C35 C 0.2245(6) -0.0836(3) 0.10402(16) 0.0619(15) Uani 1 1 d . . . H35A H 0.3130 -0.0929 0.1038 0.093 Uiso 1 1 calc R . . H35B H 0.2080 -0.0436 0.0872 0.093 Uiso 1 1 calc R . . H35C H 0.1801 -0.1213 0.0916 0.093 Uiso 1 1 calc R . . C36 C 0.3945(4) 0.0287(3) 0.15499(12) 0.0398(9) Uani 1 1 d . . . C37 C 0.4847(5) -0.0227(3) 0.17219(16) 0.0557(13) Uani 1 1 d . . . H37A H 0.5686 -0.0103 0.1640 0.084 Uiso 1 1 calc R . . H37B H 0.4649 -0.0664 0.1602 0.084 Uiso 1 1 calc R . . H37C H 0.4785 -0.0245 0.2034 0.084 Uiso 1 1 calc R . . C38 C 0.4082(5) 0.0341(3) 0.10582(14) 0.0558(14) Uani 1 1 d . . . H38A H 0.4905 0.0507 0.0988 0.084 Uiso 1 1 calc R . . H38B H 0.3461 0.0649 0.0946 0.084 Uiso 1 1 calc R . . H38C H 0.3965 -0.0098 0.0929 0.084 Uiso 1 1 calc R . . C39 C 0.4342(5) 0.0977(3) 0.17172(14) 0.0492(12) Uani 1 1 d . . . H39A H 0.4344 0.0975 0.2031 0.074 Uiso 1 1 calc R . . H39B H 0.3764 0.1315 0.1614 0.074 Uiso 1 1 calc R . . H39C H 0.5171 0.1080 0.1613 0.074 Uiso 1 1 calc R . . C40 C 0.0606(4) 0.2117(2) 0.05018(15) 0.0361(8) Uani 1 1 d . . . H40 H 0.0150 0.1687 0.0524 0.043 Uiso 1 1 calc R . . C41 C -0.2049(6) 0.1960(3) 0.4401(2) 0.0681(17) Uani 1 1 d . . . H41 H -0.2127 0.1618 0.4631 0.082 Uiso 1 1 calc R . . C42 C 0.7178(7) -0.1249(4) 0.0771(2) 0.063(2) Uani 0.75 1 d PD A 1 H42 H 0.7340 -0.0767 0.0823 0.075 Uiso 0.75 1 calc PR A 1 C1A C 0.7607(12) 0.1049(8) 0.0388(4) 0.051(3) Uani 0.50 1 d P C 1 C42A C 0.7127(11) -0.1364(11) 0.1191(6) 0.102(19) Uani 0.25 1 d PD B 2 H42A H 0.7276 -0.0911 0.1070 0.122 Uiso 0.25 1 calc PR B 2 C1B C 0.7352(13) 0.0837(10) 0.0260(4) 0.059(4) Uani 0.50 1 d P D 3 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 0.02531(13) 0.01920(11) 0.01664(11) 0.00055(10) -0.00187(10) 0.00124(11) Ru2 0.02247(12) 0.02330(12) 0.01831(11) 0.00309(10) -0.00111(10) 0.00115(11) Cl1 0.0261(4) 0.0294(4) 0.0212(4) 0.0047(3) 0.0033(3) 0.0055(3) Cl2 0.0319(5) 0.0292(4) 0.0190(3) -0.0015(3) -0.0029(3) 0.0088(3) Cl3 0.0421(7) 0.0743(9) 0.1075(13) -0.0325(9) 0.0022(8) 0.0043(6) Cl4 0.1125(14) 0.0845(11) 0.0370(7) -0.0019(7) -0.0181(8) 0.0272(10) Cl5 0.0714(9) 0.0517(7) 0.0322(5) -0.0008(5) 0.0021(5) 0.0041(6) Cl6 0.0985(16) 0.1173(17) 0.1355(19) -0.0480(15) -0.0475(15) 0.0357(14) Cl7 0.0635(12) 0.0864(13) 0.263(3) -0.0794(19) -0.0258(17) 0.0054(10) Cl8 0.0580(9) 0.0498(8) 0.183(2) -0.0196(11) -0.0043(12) 0.0058(7) Cl9 0.0687(16) 0.128(2) 0.132(2) -0.028(2) -0.0139(17) -0.0004(15) Cl10 0.099(3) 0.324(7) 0.108(3) -0.076(3) -0.012(2) 0.095(3) Cl11 0.171(4) 0.080(2) 0.115(3) 0.041(2) -0.007(2) -0.017(2) Cl9A 0.071(5) 0.075(5) 0.200(11) -0.048(6) -0.013(6) -0.001(4) Cl9B 0.069(5) 0.058(4) 0.167(9) 0.018(5) -0.034(5) -0.004(3) Cl9C 0.056(5) 0.087(6) 0.50(3) -0.160(12) 0.024(10) -0.028(4) S1 0.0238(4) 0.0306(4) 0.0259(4) 0.0043(3) -0.0006(3) -0.0026(3) S1A 0.0379(11) 0.0445(11) 0.0328(9) -0.0058(10) 0.0035(9) -0.0039(9) S1B 0.0482(14) 0.0465(12) 0.0426(12) 0.0067(10) -0.0122(11) -0.0074(11) P1 0.0377(5) 0.0247(4) 0.0175(4) -0.0007(3) -0.0004(4) 0.0000(4) P2 0.0300(5) 0.0248(4) 0.0253(4) 0.0018(4) -0.0059(4) 0.0053(4) P3 0.0238(5) 0.0273(4) 0.0259(4) 0.0077(4) -0.0012(4) 0.0019(4) P4 0.0333(5) 0.0401(6) 0.0187(4) 0.0006(4) -0.0022(4) 0.0040(4) F1 0.0516(18) 0.0506(16) 0.070(2) 0.0010(14) -0.0227(15) -0.0177(14) F2 0.0548(17) 0.0303(12) 0.0639(18) -0.0041(12) -0.0021(14) -0.0023(12) F3 0.083(2) 0.0461(16) 0.0541(17) 0.0174(13) 0.0036(16) -0.0257(16) F1A 0.081(6) 0.079(5) 0.095(6) -0.042(5) 0.003(5) 0.018(4) F2A 0.024(6) 0.161(16) 0.044(4) 0.014(6) -0.002(4) -0.027(7) F3A 0.055(5) 0.066(5) 0.024(4) 0.028(4) 0.001(3) 0.011(4) F1B 0.062(7) 0.201(14) 0.081(10) 0.111(8) -0.005(6) 0.005(7) F2B 0.130(8) 0.109(7) 0.077(5) -0.036(5) -0.038(5) -0.029(7) F3B 0.061(11) 0.075(7) 0.167(15) -0.002(9) 0.010(9) -0.019(7) O1 0.0269(13) 0.0285(12) 0.0244(12) 0.0048(9) -0.0002(10) -0.0039(11) O2 0.0255(13) 0.0270(12) 0.0244(12) 0.0036(10) -0.0006(10) 0.0024(10) O3 0.0262(14) 0.0498(17) 0.0334(14) 0.0039(13) 0.0038(12) -0.0005(12) O4 0.0431(17) 0.0339(14) 0.0353(15) 0.0016(12) -0.0080(13) -0.0123(13) O5 0.0479(18) 0.0319(14) 0.0490(17) 0.0118(14) -0.0134(15) -0.0122(13) O1A 0.069(6) 0.065(5) 0.068(5) -0.025(4) 0.000(5) -0.005(4) O2A 0.030(7) 0.064(6) 0.048(7) 0.001(5) 0.016(4) -0.004(5) O3A 0.090(9) 0.054(8) 0.040(7) 0.007(5) 0.002(5) -0.012(6) O1B 0.080(6) 0.047(4) 0.040(4) -0.007(3) -0.019(4) 0.002(4) O2B 0.033(9) 0.071(7) 0.065(11) 0.007(8) -0.009(6) 0.007(7) O3B 0.104(11) 0.034(5) 0.040(6) -0.007(4) -0.010(6) -0.014(6) C1 0.041(3) 0.036(2) 0.041(2) 0.0077(18) -0.0064(19) -0.0063(18) C2 0.036(2) 0.0313(17) 0.0194(15) 0.0015(14) -0.0026(16) 0.0018(16) C3 0.034(2) 0.0320(19) 0.0276(18) 0.0043(15) -0.0076(16) 0.0011(15) C4 0.049(2) 0.040(2) 0.0165(17) 0.0039(15) -0.0070(16) 0.0004(18) C5 0.039(2) 0.035(2) 0.0257(17) 0.0064(15) -0.0096(16) 0.0022(17) C6 0.065(3) 0.0278(18) 0.0273(19) -0.0100(14) 0.0013(19) -0.008(2) C7 0.102(5) 0.045(3) 0.033(2) -0.0212(19) 0.007(3) -0.018(3) C8 0.066(3) 0.026(2) 0.048(3) -0.0036(18) 0.015(2) 0.002(2) C9 0.062(3) 0.041(2) 0.037(2) -0.0048(19) -0.010(2) -0.015(2) C10 0.047(2) 0.038(2) 0.0236(17) 0.0020(16) 0.0115(18) -0.0002(17) C11 0.053(3) 0.058(3) 0.045(3) 0.010(2) 0.019(2) 0.015(2) C12 0.059(3) 0.063(3) 0.0254(19) 0.003(2) 0.0086(19) -0.007(3) C13 0.039(2) 0.059(3) 0.040(2) -0.004(2) 0.009(2) -0.004(2) C14 0.049(3) 0.0231(18) 0.037(2) -0.0006(15) -0.0066(19) 0.0068(17) C15 0.050(3) 0.0284(19) 0.047(2) 0.0087(17) -0.005(2) -0.0003(19) C16 0.063(3) 0.030(2) 0.061(3) 0.006(2) -0.005(3) 0.015(2) C17 0.057(3) 0.029(2) 0.049(3) -0.0083(19) -0.011(2) -0.0003(19) C18 0.033(2) 0.039(2) 0.037(2) 0.0082(18) -0.0059(18) 0.0042(17) C19 0.027(2) 0.042(2) 0.058(3) 0.005(2) -0.0053(19) 0.0029(17) C20 0.043(3) 0.063(3) 0.041(2) -0.004(2) 0.005(2) 0.009(2) C21 0.040(3) 0.060(3) 0.066(3) 0.017(3) -0.011(2) 0.009(2) C22 0.039(2) 0.035(2) 0.0279(19) 0.0106(16) -0.0074(17) -0.0001(17) C23 0.041(2) 0.050(2) 0.0213(18) 0.0068(17) -0.0024(16) 0.0026(19) C24 0.039(2) 0.0259(18) 0.040(2) 0.0069(16) -0.0029(18) 0.0023(16) C25 0.051(3) 0.031(2) 0.055(3) 0.007(2) -0.004(2) 0.013(2) C26 0.046(3) 0.0296(19) 0.052(3) 0.0110(18) -0.002(2) -0.0075(19) C27 0.046(3) 0.032(2) 0.044(2) -0.0021(18) -0.006(2) 0.0041(19) C28 0.0206(18) 0.043(2) 0.043(2) 0.0142(18) 0.0012(16) 0.0033(16) C29 0.029(2) 0.072(3) 0.037(2) 0.010(2) 0.0061(18) 0.009(2) C30 0.026(2) 0.068(3) 0.055(3) 0.021(2) -0.005(2) 0.008(2) C31 0.027(2) 0.052(3) 0.060(3) 0.011(2) 0.0069(19) -0.006(2) C32 0.051(3) 0.045(2) 0.0285(19) -0.0067(17) -0.006(2) -0.002(2) C33 0.054(3) 0.041(2) 0.042(2) -0.005(2) -0.014(2) -0.005(2) C34 0.076(4) 0.037(2) 0.047(3) -0.010(2) -0.014(3) 0.008(2) C35 0.082(4) 0.070(4) 0.034(2) -0.016(2) -0.004(3) 0.007(3) C36 0.036(2) 0.062(3) 0.0219(17) 0.0047(19) 0.0034(15) 0.005(2) C37 0.044(3) 0.081(4) 0.043(3) 0.012(3) 0.007(2) 0.010(3) C38 0.046(3) 0.092(4) 0.029(2) 0.004(3) 0.0088(19) 0.002(3) C39 0.044(3) 0.071(3) 0.033(2) 0.004(2) 0.009(2) -0.014(2) C40 0.033(2) 0.038(2) 0.037(2) -0.0049(19) -0.0023(19) -0.0072(16) C41 0.061(4) 0.045(3) 0.098(5) -0.004(3) -0.013(3) 0.010(3) C42 0.065(5) 0.048(4) 0.075(5) 0.004(4) 0.008(4) -0.001(4) C1A 0.027(6) 0.082(9) 0.043(8) -0.006(6) -0.001(5) -0.003(5) C42A 0.018(11) 0.042(15) 0.25(6) -0.03(2) 0.021(19) -0.019(10) C1B 0.035(7) 0.114(14) 0.029(6) 0.008(7) -0.014(5) -0.009(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 1.806(4) . ? Ru1 O2 2.225(3) . ? Ru1 P1 2.3711(9) . ? Ru1 P2 2.3803(10) . ? Ru1 Cl2 2.4721(8) . ? Ru1 Cl1 2.4823(9) . ? Ru2 C3 1.808(4) . ? Ru2 O1 2.219(3) . ? Ru2 P3 2.3714(10) . ? Ru2 P4 2.3883(10) . ? Ru2 Cl2 2.4742(9) . ? Ru2 Cl1 2.4842(8) . ? Cl3 C40 1.751(4) . ? Cl4 C40 1.749(5) . ? Cl5 C40 1.746(5) . ? Cl6 C41 1.669(7) . ? Cl7 C41 1.748(6) . ? Cl8 C41 1.765(6) . ? Cl9 C42 1.738(8) . ? Cl10 C42 1.721(8) . ? Cl11 C42 1.724(7) . ? Cl9A C42A 1.755(13) . ? Cl9B C42A 1.725(15) . ? Cl9C C42A 1.744(14) . ? S1 O3 1.427(3) . ? S1 O2 1.459(3) . ? S1 O1 1.462(3) . ? S1 C1 1.834(4) . ? S1A O3A 1.427(14) . ? S1A O1A 1.425(8) . ? S1A O2A 1.45(2) . ? S1A C1A 1.797(16) . ? S1B O3B 1.429(16) . ? S1B O1B 1.434(8) . ? S1B O2B 1.432(16) . ? S1B C1B 1.809(12) . ? P1 C4 1.852(4) . ? P1 C10 1.902(4) . ? P1 C6 1.903(4) . ? P2 C5 1.846(4) . ? P2 C18 1.904(4) . ? P2 C14 1.917(4) . ? P3 C22 1.843(4) . ? P3 C28 1.892(4) . ? P3 C24 1.899(4) . ? P4 C23 1.846(4) . ? P4 C32 1.901(4) . ? P4 C36 1.903(4) . ? F1 C1 1.313(5) . ? F2 C1 1.327(6) . ? F3 C1 1.331(5) . ? F1A C1A 1.276(15) . ? F2A C1A 1.45(2) . ? F3A C1A 1.465(18) . ? F1B C1B 1.20(2) . ? F2B C1B 1.41(2) . ? F3B C1B 1.22(3) . ? O4 C2 1.152(5) . ? O5 C3 1.155(5) . ? C4 C5 1.522(6) . ? C6 C9 1.519(7) . ? C6 C7 1.540(6) . ? C6 C8 1.540(6) . ? C10 C11 1.524(6) . ? C10 C13 1.535(6) . ? C10 C12 1.548(6) . ? C14 C17 1.530(6) . ? C14 C16 1.533(6) . ? C14 C15 1.533(7) . ? C18 C19 1.525(6) . ? C18 C21 1.535(6) . ? C18 C20 1.543(6) . ? C22 C23 1.528(6) . ? C24 C26 1.530(6) . ? C24 C27 1.534(6) . ? C24 C25 1.542(6) . ? C28 C31 1.534(6) . ? C28 C29 1.540(6) . ? C28 C30 1.542(6) . ? C32 C34 1.521(7) . ? C32 C33 1.536(7) . ? C32 C35 1.542(6) . ? C36 C37 1.524(7) . ? C36 C39 1.547(7) . ? C36 C38 1.549(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 C2 Ru1 O2 162.78(13) . . ? C2 Ru1 P1 95.48(12) . . ? O2 Ru1 P1 95.53(7) . . ? C2 Ru1 P2 92.44(12) . . ? O2 Ru1 P2 101.45(7) . . ? P1 Ru1 P2 86.27(4) . . ? C2 Ru1 Cl2 85.35(11) . . ? O2 Ru1 Cl2 83.35(7) . . ? P1 Ru1 Cl2 178.40(3) . . ? P2 Ru1 Cl2 95.07(3) . . ? C2 Ru1 Cl1 84.29(12) . . ? O2 Ru1 Cl1 81.52(7) . . ? P1 Ru1 Cl1 95.46(3) . . ? P2 Ru1 Cl1 176.43(3) . . ? Cl2 Ru1 Cl1 83.26(3) . . ? C3 Ru2 O1 164.06(13) . . ? C3 Ru2 P3 94.89(12) . . ? O1 Ru2 P3 96.42(7) . . ? C3 Ru2 P4 91.72(13) . . ? O1 Ru2 P4 100.16(7) . . ? P3 Ru2 P4 86.33(3) . . ? C3 Ru2 Cl2 85.18(12) . . ? O1 Ru2 Cl2 83.08(7) . . ? P3 Ru2 Cl2 177.75(3) . . ? P4 Ru2 Cl2 95.91(3) . . ? C3 Ru2 Cl1 87.04(13) . . ? O1 Ru2 Cl1 80.91(7) . . ? P3 Ru2 Cl1 94.59(3) . . ? P4 Ru2 Cl1 178.51(3) . . ? Cl2 Ru2 Cl1 83.17(3) . . ? Ru1 Cl1 Ru2 95.89(3) . . ? Ru1 Cl2 Ru2 96.41(3) . . ? O3 S1 O2 115.65(16) . . ? O3 S1 O1 115.38(16) . . ? O2 S1 O1 114.23(15) . . ? O3 S1 C1 104.2(2) . . ? O2 S1 C1 102.69(18) . . ? O1 S1 C1 102.16(18) . . ? O3A S1A O1A 113.6(7) . . ? O3A S1A O2A 115.9(11) . . ? O1A S1A O2A 113.7(9) . . ? O3A S1A C1A 103.8(7) . . ? O1A S1A C1A 105.5(6) . . ? O2A S1A C1A 102.5(12) . . ? O3B S1B O1B 114.7(5) . . ? O3B S1B O2B 113.6(12) . . ? O1B S1B O2B 115.3(12) . . ? O3B S1B C1B 106.1(9) . . ? O1B S1B C1B 100.6(7) . . ? O2B S1B C1B 104.7(10) . . ? C4 P1 C10 102.06(19) . . ? C4 P1 C6 105.3(2) . . ? C10 P1 C6 108.2(2) . . ? C4 P1 Ru1 106.21(13) . . ? C10 P1 Ru1 119.12(14) . . ? C6 P1 Ru1 114.35(13) . . ? C5 P2 C18 102.28(19) . . ? C5 P2 C14 103.81(19) . . ? C18 P2 C14 109.0(2) . . ? C5 P2 Ru1 107.12(13) . . ? C18 P2 Ru1 119.20(13) . . ? C14 P2 Ru1 113.68(14) . . ? C22 P3 C28 101.7(2) . . ? C22 P3 C24 106.22(19) . . ? C28 P3 C24 107.6(2) . . ? C22 P3 Ru2 106.27(14) . . ? C28 P3 Ru2 119.22(13) . . ? C24 P3 Ru2 114.27(14) . . ? C23 P4 C32 104.9(2) . . ? C23 P4 C36 101.5(2) . . ? C32 P4 C36 108.9(2) . . ? C23 P4 Ru2 106.81(14) . . ? C32 P4 Ru2 114.60(14) . . ? C36 P4 Ru2 118.46(13) . . ? S1 O1 Ru2 130.34(15) . . ? S1 O2 Ru1 129.54(15) . . ? F1 C1 F2 108.9(4) . . ? F1 C1 F3 109.2(4) . . ? F2 C1 F3 108.0(4) . . ? F1 C1 S1 110.2(3) . . ? F2 C1 S1 111.5(3) . . ? F3 C1 S1 109.0(3) . . ? O4 C2 Ru1 168.9(3) . . ? O5 C3 Ru2 168.6(3) . . ? C5 C4 P1 114.4(3) . . ? C4 C5 P2 114.1(3) . . ? C9 C6 C7 106.8(4) . . ? C9 C6 C8 110.1(4) . . ? C7 C6 C8 108.7(4) . . ? C9 C6 P1 107.5(3) . . ? C7 C6 P1 113.7(3) . . ? C8 C6 P1 109.9(3) . . ? C11 C10 C13 107.2(4) . . ? C11 C10 C12 109.6(4) . . ? C13 C10 C12 106.9(4) . . ? C11 C10 P1 111.6(3) . . ? C13 C10 P1 110.5(3) . . ? C12 C10 P1 111.0(3) . . ? C17 C14 C16 107.4(4) . . ? C17 C14 C15 111.3(4) . . ? C16 C14 C15 106.1(4) . . ? C17 C14 P2 110.9(3) . . ? C16 C14 P2 113.4(3) . . ? C15 C14 P2 107.8(3) . . ? C19 C18 C21 105.9(4) . . ? C19 C18 C20 108.6(4) . . ? C21 C18 C20 109.0(4) . . ? C19 C18 P2 109.5(3) . . ? C21 C18 P2 113.8(3) . . ? C20 C18 P2 109.9(3) . . ? C23 C22 P3 114.7(3) . . ? C22 C23 P4 113.8(3) . . ? C26 C24 C27 109.3(4) . . ? C26 C24 C25 106.2(3) . . ? C27 C24 C25 109.6(4) . . ? C26 C24 P3 107.3(3) . . ? C27 C24 P3 110.7(3) . . ? C25 C24 P3 113.6(3) . . ? C31 C28 C29 106.4(4) . . ? C31 C28 C30 106.7(4) . . ? C29 C28 C30 109.4(4) . . ? C31 C28 P3 110.7(3) . . ? C29 C28 P3 111.7(3) . . ? C30 C28 P3 111.7(3) . . ? C34 C32 C33 111.4(4) . . ? C34 C32 C35 107.8(4) . . ? C33 C32 C35 105.3(4) . . ? C34 C32 P4 111.3(3) . . ? C33 C32 P4 107.7(3) . . ? C35 C32 P4 113.1(4) . . ? C37 C36 C39 108.2(4) . . ? C37 C36 C38 109.7(4) . . ? C39 C36 C38 104.2(4) . . ? C37 C36 P4 111.3(3) . . ? C39 C36 P4 109.4(3) . . ? C38 C36 P4 113.7(3) . . ? Cl5 C40 Cl4 109.6(2) . . ? Cl5 C40 Cl3 110.7(2) . . ? Cl4 C40 Cl3 110.6(3) . . ? Cl6 C41 Cl7 112.9(4) . . ? Cl6 C41 Cl8 111.6(4) . . ? Cl7 C41 Cl8 109.8(3) . . ? Cl10 C42 Cl11 109.8(5) . . ? Cl10 C42 Cl9 110.0(5) . . ? Cl11 C42 Cl9 112.8(5) . . ? F1A C1A F2A 109.5(13) . . ? F1A C1A F3A 110.4(13) . . ? F2A C1A F3A 97.5(11) . . ? F1A C1A S1A 113.3(10) . . ? F2A C1A S1A 113.6(13) . . ? F3A C1A S1A 111.5(9) . . ? Cl9B C42A Cl9C 111.9(14) . . ? Cl9B C42A Cl9A 111.6(11) . . ? Cl9C C42A Cl9A 107.6(10) . . ? F1B C1B F3B 114(2) . . ? F1B C1B F2B 110.3(15) . . ? F3B C1B F2B 114.3(16) . . ? F1B C1B S1B 104.0(12) . . ? F3B C1B S1B 105.1(14) . . ? F2B C1B S1B 108.2(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.232 _refine_diff_density_min -0.934 _refine_diff_density_rms 0.088 data_k03mkw6 _database_code_depnum_ccdc_archive 'CCDC 250926' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H40 Cl2 O P2 Ru' _chemical_formula_weight 518.42 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 11.0660(1) _cell_length_b 15.7550(2) _cell_length_c 14.3190(1) _cell_angle_alpha 90.00 _cell_angle_beta 109.178(1) _cell_angle_gamma 90.00 _cell_volume 2357.90(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.7468 _exptl_absorpt_correction_T_max 0.8200 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature ? _diffrn_radiation_wavelength ? _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50276 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 30.05 _reflns_number_total 6879 _reflns_number_gt 6074 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+1.4821*P+(0.0190P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _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 6879 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0565 _refine_ls_wR_factor_gt 0.0533 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.020878(11) 0.200641(7) 0.714901(8) 0.01501(4) Uani 1 1 d . . . Cl1 Cl -0.12123(4) 0.30503(2) 0.61263(3) 0.02640(9) Uani 1 1 d . . . Cl2 Cl 0.18536(4) 0.30534(2) 0.73473(3) 0.02933(9) Uani 1 1 d . . . P1 P -0.14341(3) 0.11283(2) 0.72503(3) 0.01545(7) Uani 1 1 d . . . P2 P 0.16198(3) 0.10999(2) 0.83287(3) 0.01558(7) Uani 1 1 d . . . O1 O 0.03484(12) 0.11971(7) 0.53426(8) 0.0267(2) Uani 1 1 d . . . C1 C 0.03156(14) 0.14692(9) 0.60823(11) 0.0194(3) Uani 1 1 d . . . C2 C -0.06992(14) 0.02211(9) 0.80482(11) 0.0188(3) Uani 1 1 d . . . H2A H -0.1293 0.0020 0.8388 0.023 Uiso 1 1 calc R . . H2B H -0.0576 -0.0249 0.7629 0.023 Uiso 1 1 calc R . . C3 C 0.05890(14) 0.04349(9) 0.88242(11) 0.0183(3) Uani 1 1 d . . . H3A H 0.1045 -0.0100 0.9087 0.022 Uiso 1 1 calc R . . H3B H 0.0436 0.0738 0.9381 0.022 Uiso 1 1 calc R . . C4 C -0.25998(14) 0.05965(10) 0.61359(11) 0.0211(3) Uani 1 1 d . . . C5 C -0.19135(17) -0.00921(11) 0.57340(12) 0.0272(3) Uani 1 1 d . . . H5A H -0.2512 -0.0335 0.5128 0.041 Uiso 1 1 calc R . . H5B H -0.1605 -0.0540 0.6230 0.041 Uiso 1 1 calc R . . H5C H -0.1187 0.0161 0.5588 0.041 Uiso 1 1 calc R . . C6 C -0.36746(16) 0.01496(12) 0.64116(13) 0.0306(4) Uani 1 1 d . . . H6A H -0.4211 -0.0175 0.5843 0.046 Uiso 1 1 calc R . . H6B H -0.4199 0.0575 0.6598 0.046 Uiso 1 1 calc R . . H6C H -0.3297 -0.0235 0.6969 0.046 Uiso 1 1 calc R . . C7 C -0.31598(17) 0.12457(12) 0.53006(12) 0.0294(4) Uani 1 1 d . . . H7A H -0.2461 0.1530 0.5145 0.044 Uiso 1 1 calc R . . H7B H -0.3664 0.1668 0.5515 0.044 Uiso 1 1 calc R . . H7C H -0.3710 0.0952 0.4711 0.044 Uiso 1 1 calc R . . C8 C -0.23188(15) 0.17577(10) 0.79517(11) 0.0211(3) Uani 1 1 d . . . C9 C -0.28064(16) 0.12101(11) 0.86413(12) 0.0278(3) Uani 1 1 d . . . H9A H -0.2081 0.0930 0.9130 0.042 Uiso 1 1 calc R . . H9B H -0.3400 0.0780 0.8252 0.042 Uiso 1 1 calc R . . H9C H -0.3250 0.1571 0.8982 0.042 Uiso 1 1 calc R . . C10 C -0.34313(17) 0.22823(12) 0.72700(13) 0.0308(4) Uani 1 1 d . . . H10A H -0.4123 0.1901 0.6902 0.046 Uiso 1 1 calc R . . H10B H -0.3132 0.2607 0.6805 0.046 Uiso 1 1 calc R . . H10C H -0.3748 0.2673 0.7669 0.046 Uiso 1 1 calc R . . C11 C -0.13132(17) 0.23763(11) 0.85932(12) 0.0250(3) Uani 1 1 d . . . C12 C 0.25747(14) 0.03401(10) 0.78262(11) 0.0209(3) Uani 1 1 d . . . C13 C 0.16566(16) -0.02972(10) 0.71283(12) 0.0234(3) Uani 1 1 d . . . H13A H 0.2126 -0.0635 0.6787 0.035 Uiso 1 1 calc R . . H13B H 0.0964 0.0012 0.6641 0.035 Uiso 1 1 calc R . . H13C H 0.1295 -0.0674 0.7513 0.035 Uiso 1 1 calc R . . C14 C 0.32875(16) 0.08392(11) 0.72404(13) 0.0282(3) Uani 1 1 d . . . H14A H 0.3925 0.1212 0.7691 0.042 Uiso 1 1 calc R . . H14B H 0.2674 0.1182 0.6730 0.042 Uiso 1 1 calc R . . H14C H 0.3717 0.0441 0.6928 0.042 Uiso 1 1 calc R . . C15 C 0.35465(16) -0.01940(11) 0.86279(13) 0.0294(4) Uani 1 1 d . . . H15A H 0.3948 -0.0609 0.8313 0.044 Uiso 1 1 calc R . . H15B H 0.3105 -0.0492 0.9023 0.044 Uiso 1 1 calc R . . H15C H 0.4205 0.0179 0.9058 0.044 Uiso 1 1 calc R . . C16 C 0.27332(15) 0.16190(10) 0.95004(11) 0.0220(3) Uani 1 1 d . . . C17 C 0.39696(17) 0.19557(12) 0.93608(14) 0.0318(4) Uani 1 1 d . . . H17A H 0.3751 0.2326 0.8779 0.048 Uiso 1 1 calc R . . H17B H 0.4483 0.1477 0.9266 0.048 Uiso 1 1 calc R . . H17C H 0.4461 0.2278 0.9948 0.048 Uiso 1 1 calc R . . C18 C 0.30871(16) 0.10083(11) 1.03921(12) 0.0280(3) Uani 1 1 d . . . H18A H 0.3690 0.1289 1.0969 0.042 Uiso 1 1 calc R . . H18B H 0.3484 0.0496 1.0234 0.042 Uiso 1 1 calc R . . H18C H 0.2312 0.0852 1.0540 0.042 Uiso 1 1 calc R . . C19 C 0.20292(18) 0.23715(11) 0.97676(13) 0.0276(3) Uani 1 1 d . . . H11A H -0.0958(19) 0.2746(13) 0.8190(15) 0.031(5) Uiso 1 1 d . . . H19A H 0.130(2) 0.2172(13) 0.9970(15) 0.032(5) Uiso 1 1 d . . . H11B H -0.060(2) 0.2093(14) 0.9095(17) 0.044(6) Uiso 1 1 d . . . H19B H 0.171(2) 0.2776(14) 0.9215(16) 0.034(5) Uiso 1 1 d . . . H11C H -0.172(2) 0.2721(14) 0.8911(16) 0.039(6) Uiso 1 1 d . . . H19C H 0.263(2) 0.2652(14) 1.0347(16) 0.036(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02074(6) 0.01095(6) 0.01489(6) 0.00045(4) 0.00795(4) 0.00059(4) Cl1 0.0385(2) 0.01882(17) 0.02087(18) 0.00494(13) 0.00837(16) 0.00855(15) Cl2 0.0363(2) 0.01916(18) 0.0343(2) 0.00082(15) 0.01406(18) -0.00920(15) P1 0.01608(16) 0.01589(17) 0.01456(16) 0.00019(13) 0.00528(13) 0.00091(13) P2 0.01581(16) 0.01370(16) 0.01750(17) -0.00022(13) 0.00584(13) 0.00007(13) O1 0.0389(7) 0.0241(6) 0.0220(5) -0.0012(4) 0.0167(5) 0.0009(5) C1 0.0237(7) 0.0148(6) 0.0220(7) 0.0029(5) 0.0104(6) 0.0002(5) C2 0.0196(7) 0.0155(6) 0.0212(7) 0.0024(5) 0.0067(6) -0.0017(5) C3 0.0190(7) 0.0170(7) 0.0187(7) 0.0033(5) 0.0059(6) 0.0002(5) C4 0.0191(7) 0.0249(7) 0.0181(7) -0.0028(6) 0.0043(6) -0.0032(6) C5 0.0297(8) 0.0257(8) 0.0254(8) -0.0092(6) 0.0080(7) -0.0041(6) C6 0.0223(8) 0.0405(10) 0.0279(8) -0.0035(7) 0.0066(7) -0.0108(7) C7 0.0301(9) 0.0349(9) 0.0185(7) 0.0012(7) 0.0017(6) 0.0020(7) C8 0.0212(7) 0.0249(7) 0.0195(7) -0.0001(6) 0.0099(6) 0.0045(6) C9 0.0279(8) 0.0357(9) 0.0240(8) -0.0006(7) 0.0144(7) -0.0008(7) C10 0.0291(9) 0.0357(9) 0.0296(9) 0.0021(7) 0.0124(7) 0.0135(7) C11 0.0313(9) 0.0229(8) 0.0229(8) -0.0046(6) 0.0116(7) 0.0015(7) C12 0.0191(7) 0.0206(7) 0.0239(7) -0.0024(6) 0.0082(6) 0.0032(5) C13 0.0274(8) 0.0177(7) 0.0261(8) -0.0026(6) 0.0102(6) 0.0030(6) C14 0.0241(8) 0.0325(9) 0.0328(9) -0.0039(7) 0.0160(7) -0.0017(7) C15 0.0252(8) 0.0283(8) 0.0319(9) -0.0007(7) 0.0057(7) 0.0108(7) C16 0.0208(7) 0.0219(7) 0.0212(7) -0.0041(6) 0.0039(6) -0.0015(6) C17 0.0238(8) 0.0356(10) 0.0340(9) -0.0075(7) 0.0069(7) -0.0094(7) C18 0.0249(8) 0.0332(9) 0.0213(8) 0.0001(7) 0.0013(6) 0.0035(7) C19 0.0323(9) 0.0247(8) 0.0247(8) -0.0072(7) 0.0078(7) 0.0003(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.7838(15) . ? Ru1 P1 2.3267(4) . ? Ru1 P2 2.3660(4) . ? Ru1 Cl2 2.4031(4) . ? Ru1 Cl1 2.4103(4) . ? Ru1 H11A 2.55(2) . ? Ru1 H19B 3.12(2) . ? Ru1 H11B 3.20(2) . ? Ru1 H19A 3.83(2) . ? P1 C2 1.8437(15) . ? P1 C4 1.8868(15) . ? P1 C8 1.8964(15) . ? P2 C3 1.8531(15) . ? P2 C12 1.8887(15) . ? P2 C16 1.9088(15) . ? O1 C1 1.1542(18) . ? C2 C3 1.530(2) . ? C4 C5 1.540(2) . ? C4 C7 1.541(2) . ? C4 C6 1.541(2) . ? C8 C11 1.536(2) . ? C8 C9 1.536(2) . ? C8 C10 1.537(2) . ? C11 H11C 0.92(2) . ? C11 H11B 0.99(2) . ? C11 H11A 0.99(2) . ? C12 C15 1.540(2) . ? C12 C13 1.540(2) . ? C12 C14 1.542(2) . ? C16 C19 1.535(2) . ? C16 C17 1.541(2) . ? C16 C18 1.543(2) . ? C19 H19C 0.98(2) . ? C19 H19B 0.99(2) . ? C19 H19A 0.99(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 P1 92.53(5) . . ? C1 Ru1 P2 96.38(5) . . ? P1 Ru1 P2 86.702(13) . . ? C1 Ru1 Cl2 99.57(5) . . ? P1 Ru1 Cl2 167.902(15) . . ? P2 Ru1 Cl2 91.915(14) . . ? C1 Ru1 Cl1 90.98(5) . . ? P1 Ru1 Cl1 94.384(14) . . ? P2 Ru1 Cl1 172.512(14) . . ? Cl2 Ru1 Cl1 85.471(15) . . ? C1 Ru1 H11A 154.9(5) . . ? P1 Ru1 H11A 71.3(5) . . ? P2 Ru1 H11A 101.6(5) . . ? Cl2 Ru1 H11A 97.3(5) . . ? Cl1 Ru1 H11A 71.9(5) . . ? C1 Ru1 H19B 146.2(4) . . ? P1 Ru1 H19B 110.8(4) . . ? P2 Ru1 H19B 62.4(4) . . ? Cl2 Ru1 H19B 58.4(4) . . ? Cl1 Ru1 H19B 110.4(4) . . ? H11A Ru1 H19B 58.8(6) . . ? C1 Ru1 H11B 152.0(4) . . ? P1 Ru1 H11B 61.5(4) . . ? P2 Ru1 H11B 73.2(4) . . ? Cl2 Ru1 H11B 106.6(4) . . ? Cl1 Ru1 H11B 100.8(4) . . ? H11A Ru1 H11B 29.7(6) . . ? H19B Ru1 H11B 51.0(6) . . ? C1 Ru1 H19A 148.2(3) . . ? P1 Ru1 H19A 87.5(3) . . ? P2 Ru1 H19A 51.8(3) . . ? Cl2 Ru1 H19A 82.2(3) . . ? Cl1 Ru1 H19A 120.8(3) . . ? H11A Ru1 H19A 52.9(5) . . ? H19B Ru1 H19A 24.2(5) . . ? H11B Ru1 H19A 32.7(5) . . ? C2 P1 C4 102.69(7) . . ? C2 P1 C8 106.06(7) . . ? C4 P1 C8 110.59(7) . . ? C2 P1 Ru1 107.76(5) . . ? C4 P1 Ru1 122.85(5) . . ? C8 P1 Ru1 105.78(5) . . ? C3 P2 C12 106.22(7) . . ? C3 P2 C16 101.92(7) . . ? C12 P2 C16 109.03(7) . . ? C3 P2 Ru1 105.65(5) . . ? C12 P2 Ru1 115.54(5) . . ? C16 P2 Ru1 116.94(5) . . ? O1 C1 Ru1 173.16(13) . . ? C3 C2 P1 113.30(10) . . ? C2 C3 P2 112.98(10) . . ? C5 C4 C7 107.43(13) . . ? C5 C4 C6 106.89(13) . . ? C7 C4 C6 110.78(14) . . ? C5 C4 P1 110.17(11) . . ? C7 C4 P1 110.53(11) . . ? C6 C4 P1 110.92(11) . . ? C11 C8 C9 108.07(13) . . ? C11 C8 C10 108.08(14) . . ? C9 C8 C10 109.45(13) . . ? C11 C8 P1 104.47(10) . . ? C9 C8 P1 113.46(11) . . ? C10 C8 P1 112.96(11) . . ? H11C C11 H11B 108.4(18) . . ? H11C C11 H11A 107.2(18) . . ? H11B C11 H11A 108.3(17) . . ? H11C C11 C8 107.1(14) . . ? H11B C11 C8 113.6(13) . . ? H11A C11 C8 112.0(12) . . ? C15 C12 C13 106.12(13) . . ? C15 C12 C14 109.11(13) . . ? C13 C12 C14 109.01(13) . . ? C15 C12 P2 113.80(11) . . ? C13 C12 P2 109.15(10) . . ? C14 C12 P2 109.52(11) . . ? C19 C16 C17 108.15(14) . . ? C19 C16 C18 106.68(14) . . ? C17 C16 C18 109.10(13) . . ? C19 C16 P2 108.43(11) . . ? C17 C16 P2 112.20(11) . . ? C18 C16 P2 112.04(11) . . ? H19C C19 H19B 110.5(17) . . ? H19C C19 H19A 106.7(17) . . ? H19B C19 H19A 109.0(17) . . ? H19C C19 C16 107.5(12) . . ? H19B C19 C16 112.2(12) . . ? H19A C19 C16 110.8(12) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.605 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.068 data_c:\word_f~1\papers\inorga~1\mkw\august~1\h03mkw1\maxus\h03mkw1 _database_code_depnum_ccdc_archive 'CCDC 250927' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H124 Cl10 O3 P6 Ru3' _chemical_formula_weight 1725.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 11.2930(3) _cell_length_b 16.9890(5) _cell_length_c 40.7010(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.158(1) _cell_angle_gamma 90.00 _cell_volume 7763.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Irregular _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3576 _exptl_absorpt_coefficient_mu 1.083 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22539 _diffrn_reflns_av_R_equivalents 0.1169 _diffrn_reflns_av_sigmaI/netI 0.1963 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 27.37 _reflns_number_total 7143 _reflns_number_gt 3783 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.1222P)^2^+152.7364P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7143 _refine_ls_number_parameters 731 _refine_ls_number_restraints 336 _refine_ls_R_factor_all 0.2107 _refine_ls_R_factor_gt 0.1092 _refine_ls_wR_factor_ref 0.2929 _refine_ls_wR_factor_gt 0.2611 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.26355(17) 0.97487(9) 0.07635(5) 0.0354(6) Uani 1 1 d . . . Ru2 Ru 0.26099(18) 0.77592(10) 0.06977(5) 0.0436(7) Uani 1 1 d . . . Ru3 Ru 0.35642(15) 0.35143(9) 0.19331(5) 0.0327(6) Uani 1 1 d . . . Cl1 Cl 0.2941(6) 0.8664(3) 0.11967(15) 0.0541(19) Uani 1 1 d . . . Cl2 Cl 0.3960(5) 0.8792(3) 0.05241(15) 0.0443(17) Uani 1 1 d . . . Cl3 Cl 0.1062(5) 0.8781(3) 0.05790(16) 0.0493(18) Uani 1 1 d . . . Cl4 Cl 0.3624(7) 0.4779(3) 0.16341(17) 0.083(3) Uani 1 1 d . . . Cl5 Cl 0.1757(5) 0.3278(4) 0.15557(16) 0.0555(19) Uani 1 1 d . . . Cl6 Cl 0.4845(5) 0.3108(4) 0.15053(15) 0.0523(18) Uani 1 1 d . . . Cl7 Cl 0.8679(8) 0.3678(7) 0.1307(3) 0.154(5) Uani 1 1 d . . . Cl8 Cl 0.7421(8) 0.3835(5) 0.0667(2) 0.101(3) Uani 1 1 d . . . Cl9 Cl 0.3863(11) 0.3816(5) 0.0592(3) 0.154(5) Uani 1 1 d . . . Cl10 Cl 0.1340(9) 0.3836(4) 0.0664(2) 0.127(4) Uani 1 1 d . . . P1 P 0.1327(5) 1.0672(3) 0.09755(16) 0.0403(18) Uani 1 1 d . . . P2 P 0.4183(5) 1.0669(3) 0.09228(16) 0.0372(18) Uani 1 1 d . . . P3 P 0.1252(6) 0.6761(3) 0.08420(17) 0.049(2) Uani 1 1 d . . . P4 P 0.4120(6) 0.6796(3) 0.08047(17) 0.051(2) Uani 1 1 d . . . P5 P 0.2423(6) 0.3843(4) 0.23692(17) 0.0497(19) Uani 1 1 d . . . P6 P 0.5279(5) 0.3740(3) 0.23098(16) 0.0414(18) Uani 1 1 d . . . O1 O 0.2191(13) 1.0277(8) 0.0064(4) 0.046(4) Uani 1 1 d . . . O2 O 0.2148(16) 0.7538(8) -0.0019(4) 0.071(6) Uani 1 1 d . . . O3 O 0.3354(18) 0.1805(9) 0.2011(4) 0.084(7) Uani 1 1 d . . . C1 C 0.2361(18) 1.0138(11) 0.0342(6) 0.028(6) Uani 1 1 d U . . C2 C 0.2361(19) 0.7554(12) 0.0272(7) 0.040(6) Uani 1 1 d U . . C3 C 0.336(2) 0.2436(16) 0.2012(6) 0.053(7) Uani 1 1 d U . . C4 C 0.3442(19) 1.1517(13) 0.1053(6) 0.053(7) Uani 1 1 d U . . H4A H 0.3944 1.1729 0.1247 0.064 Uiso 1 1 calc R . . H4B H 0.3459 1.1911 0.0874 0.064 Uiso 1 1 calc R . . C5 C 0.227(2) 1.1504(14) 0.1137(7) 0.069(8) Uani 1 1 d U . . H5A H 0.1878 1.2000 0.1058 0.083 Uiso 1 1 calc R . . H5B H 0.2307 1.1501 0.1381 0.083 Uiso 1 1 calc R . . C6 C 0.020(2) 1.1144(16) 0.0685(7) 0.072(8) Uani 1 1 d U . . C7 C 0.114(3) 1.1720(19) 0.0454(8) 0.118(12) Uani 1 1 d U . . H7A H 0.1728 1.1376 0.0365 0.177 Uiso 1 1 calc R . . H7B H 0.1556 1.2116 0.0599 0.177 Uiso 1 1 calc R . . H7C H 0.0661 1.1983 0.0272 0.177 Uiso 1 1 calc R . . C8 C -0.0514(19) 1.1779(12) 0.0804(6) 0.051(7) Uani 1 1 d U . . H8A H -0.1003 1.2018 0.0617 0.077 Uiso 1 1 calc R . . H8B H 0.0016 1.2178 0.0914 0.077 Uiso 1 1 calc R . . H8C H -0.1032 1.1567 0.0961 0.077 Uiso 1 1 calc R . . C9 C -0.019(3) 1.068(2) 0.0409(8) 0.117(12) Uani 1 1 d U . . H9A H -0.0899 1.0385 0.0453 0.176 Uiso 1 1 calc R . . H9B H 0.0443 1.0318 0.0364 0.176 Uiso 1 1 calc R . . H9C H -0.0386 1.1025 0.0217 0.176 Uiso 1 1 calc R . . C10 C 0.0554(17) 1.0405(11) 0.1356(5) 0.034(6) Uani 1 1 d U . . C11 C -0.006(2) 1.1083(13) 0.1511(6) 0.063(8) Uani 1 1 d U . . H11A H -0.0914 1.1069 0.1437 0.095 Uiso 1 1 calc R . . H11B H 0.0276 1.1582 0.1443 0.095 Uiso 1 1 calc R . . H11C H 0.0065 1.1037 0.1752 0.095 Uiso 1 1 calc R . . C12 C -0.038(2) 0.9751(16) 0.1275(7) 0.095(10) Uani 1 1 d U . . H12A H -0.0037 0.9342 0.1143 0.143 Uiso 1 1 calc R . . H12B H -0.1085 0.9974 0.1149 0.143 Uiso 1 1 calc R . . H12C H -0.0595 0.9521 0.1480 0.143 Uiso 1 1 calc R . . C13 C 0.150(3) 1.0076(18) 0.1614(7) 0.105(11) Uani 1 1 d U . . H13A H 0.1217 1.0101 0.1832 0.157 Uiso 1 1 calc R . . H13B H 0.2233 1.0388 0.1614 0.157 Uiso 1 1 calc R . . H13C H 0.1670 0.9528 0.1560 0.157 Uiso 1 1 calc R . . C14 C 0.511(3) 1.1071(17) 0.0601(8) 0.086(9) Uani 1 1 d U . . C15 C 0.5739(18) 1.1811(11) 0.0692(6) 0.043(6) Uani 1 1 d U . . H15A H 0.6018 1.2048 0.0495 0.064 Uiso 1 1 calc R . . H15B H 0.6422 1.1702 0.0855 0.064 Uiso 1 1 calc R . . H15C H 0.5195 1.2176 0.0787 0.064 Uiso 1 1 calc R . . C16 C 0.463(3) 1.095(2) 0.0277(9) 0.130(13) Uani 1 1 d U . . H16A H 0.3765 1.1014 0.0259 0.195 Uiso 1 1 calc R . . H16B H 0.4819 1.0411 0.0209 0.195 Uiso 1 1 calc R . . H16C H 0.4972 1.1326 0.0132 0.195 Uiso 1 1 calc R . . C17 C 0.617(3) 1.042(2) 0.0553(9) 0.148(15) Uani 1 1 d U . . H17A H 0.5815 0.9902 0.0502 0.221 Uiso 1 1 calc R . . H17B H 0.6717 1.0385 0.0757 0.221 Uiso 1 1 calc R . . H17C H 0.6619 1.0585 0.0371 0.221 Uiso 1 1 calc R . . C18 C 0.5292(19) 1.0403(12) 0.1286(6) 0.044(6) Uani 1 1 d U . . C19 C 0.457(2) 1.0287(16) 0.1584(7) 0.086(9) Uani 1 1 d U . . H19A H 0.4197 0.9764 0.1572 0.129 Uiso 1 1 calc R . . H19B H 0.3943 1.0690 0.1579 0.129 Uiso 1 1 calc R . . H19C H 0.5096 1.0333 0.1790 0.129 Uiso 1 1 calc R . . C20 C 0.589(2) 0.9660(15) 0.1215(7) 0.086(9) Uani 1 1 d U . . H20A H 0.6261 0.9432 0.1421 0.129 Uiso 1 1 calc R . . H20B H 0.6497 0.9764 0.1066 0.129 Uiso 1 1 calc R . . H20C H 0.5298 0.9291 0.1109 0.129 Uiso 1 1 calc R . . C21 C 0.618(2) 1.1047(14) 0.1401(7) 0.070(8) Uani 1 1 d U . . H21A H 0.6530 1.0936 0.1627 0.105 Uiso 1 1 calc R . . H21B H 0.5774 1.1557 0.1395 0.105 Uiso 1 1 calc R . . H21C H 0.6815 1.1064 0.1254 0.105 Uiso 1 1 calc R . . C22 C 0.212(2) 0.5881(15) 0.0952(7) 0.074(8) Uani 1 1 d U . . H22A H 0.2083 0.5778 0.1190 0.089 Uiso 1 1 calc R . . H22B H 0.1727 0.5433 0.0829 0.089 Uiso 1 1 calc R . . C23 C 0.333(2) 0.5880(14) 0.0895(7) 0.067(8) Uani 1 1 d U . . H23A H 0.3404 0.5517 0.0708 0.080 Uiso 1 1 calc R . . H23B H 0.3781 0.5640 0.1091 0.080 Uiso 1 1 calc R . . C24 C 0.044(2) 0.6912(16) 0.1209(8) 0.080(9) Uani 1 1 d U . . C25 C -0.061(3) 0.7529(19) 0.1133(8) 0.125(13) Uani 1 1 d U . . H25A H -0.1063 0.7567 0.1324 0.187 Uiso 1 1 calc R . . H25B H -0.1131 0.7357 0.0939 0.187 Uiso 1 1 calc R . . H25C H -0.0268 0.8045 0.1089 0.187 Uiso 1 1 calc R . . C26 C 0.125(3) 0.721(2) 0.1496(8) 0.126(13) Uani 1 1 d U . . H26A H 0.1464 0.7760 0.1454 0.190 Uiso 1 1 calc R . . H26B H 0.1969 0.6889 0.1525 0.190 Uiso 1 1 calc R . . H26C H 0.0841 0.7188 0.1697 0.190 Uiso 1 1 calc R . . C27 C -0.0155(19) 0.6233(12) 0.1352(6) 0.054(7) Uani 1 1 d U . . H27A H 0.0438 0.5826 0.1418 0.081 Uiso 1 1 calc R . . H27B H -0.0766 0.6018 0.1187 0.081 Uiso 1 1 calc R . . H27C H -0.0528 0.6406 0.1547 0.081 Uiso 1 1 calc R . . C28 C 0.015(2) 0.6393(14) 0.0490(7) 0.062(8) Uani 1 1 d U . . C29 C -0.064(3) 0.7045(19) 0.0350(9) 0.126(13) Uani 1 1 d U . . H29A H -0.1038 0.7286 0.0528 0.189 Uiso 1 1 calc R . . H29B H -0.1240 0.6833 0.0182 0.189 Uiso 1 1 calc R . . H29C H -0.0162 0.7442 0.0251 0.189 Uiso 1 1 calc R . . C30 C -0.069(2) 0.5768(13) 0.0589(6) 0.060(7) Uani 1 1 d U . . H30A H -0.1159 0.5980 0.0759 0.091 Uiso 1 1 calc R . . H30B H -0.0234 0.5311 0.0678 0.091 Uiso 1 1 calc R . . H30C H -0.1229 0.5608 0.0396 0.091 Uiso 1 1 calc R . . C31 C 0.078(3) 0.600(2) 0.0228(9) 0.143(14) Uani 1 1 d U . . H31A H 0.1289 0.5580 0.0327 0.215 Uiso 1 1 calc R . . H31B H 0.1278 0.6393 0.0128 0.215 Uiso 1 1 calc R . . H31C H 0.0196 0.5787 0.0057 0.215 Uiso 1 1 calc R . . C32 C 0.500(2) 0.6464(14) 0.0450(7) 0.058(7) Uani 1 1 d U . . C33 C 0.596(3) 0.712(2) 0.0438(10) 0.159(16) Uani 1 1 d U . . H33A H 0.6168 0.7175 0.0211 0.239 Uiso 1 1 calc R . . H33B H 0.6672 0.6981 0.0585 0.239 Uiso 1 1 calc R . . H33C H 0.5641 0.7623 0.0509 0.239 Uiso 1 1 calc R . . C34 C 0.567(2) 0.5757(16) 0.0485(7) 0.091(10) Uani 1 1 d U . . H34A H 0.5133 0.5309 0.0498 0.137 Uiso 1 1 calc R . . H34B H 0.6226 0.5783 0.0687 0.137 Uiso 1 1 calc R . . H34C H 0.6121 0.5692 0.0294 0.137 Uiso 1 1 calc R . . C35 C 0.428(4) 0.656(3) 0.0155(11) 0.183(18) Uani 1 1 d U . . H35A H 0.4683 0.6903 0.0008 0.275 Uiso 1 1 calc R . . H35B H 0.3524 0.6798 0.0198 0.275 Uiso 1 1 calc R . . H35C H 0.4132 0.6045 0.0049 0.275 Uiso 1 1 calc R . . C36 C 0.521(3) 0.6958(19) 0.1194(9) 0.096(10) Uani 1 1 d U . . C37 C 0.576(4) 0.765(3) 0.1164(11) 0.20(2) Uani 1 1 d U . . H37A H 0.5183 0.8044 0.1078 0.295 Uiso 1 1 calc R . . H37B H 0.6372 0.7587 0.1011 0.295 Uiso 1 1 calc R . . H37C H 0.6142 0.7812 0.1381 0.295 Uiso 1 1 calc R . . C38 C 0.450(3) 0.697(2) 0.1479(9) 0.144(15) Uani 1 1 d U . . H38A H 0.4838 0.7352 0.1642 0.217 Uiso 1 1 calc R . . H38B H 0.4506 0.6444 0.1579 0.217 Uiso 1 1 calc R . . H38C H 0.3674 0.7118 0.1403 0.217 Uiso 1 1 calc R . . C39 C 0.611(2) 0.6248(13) 0.1256(6) 0.071(9) Uani 1 1 d . . . H39A H 0.6500 0.6150 0.1056 0.107 Uiso 1 1 calc R . . H39B H 0.5679 0.5775 0.1312 0.107 Uiso 1 1 calc R . . H39C H 0.6717 0.6379 0.1439 0.107 Uiso 1 1 calc R . . C40 C 0.352(3) 0.4125(17) 0.2729(7) 0.104(12) Uani 1 1 d . . . H40A H 0.3549 0.4707 0.2745 0.124 Uiso 1 1 calc R . . H40B H 0.3233 0.3923 0.2934 0.124 Uiso 1 1 calc R . . C41 C 0.470(2) 0.3840(16) 0.2710(7) 0.081(9) Uani 1 1 d U . . H41A H 0.4755 0.3316 0.2817 0.098 Uiso 1 1 calc R . . H41B H 0.5250 0.4192 0.2848 0.098 Uiso 1 1 calc R . . C42 C 0.140(2) 0.4720(13) 0.2342(6) 0.054(7) Uani 1 1 d U . . C43 C 0.202(2) 0.5413(16) 0.2198(7) 0.091(10) Uani 1 1 d U . . H43A H 0.2205 0.5282 0.1975 0.137 Uiso 1 1 calc R . . H43B H 0.2762 0.5530 0.2338 0.137 Uiso 1 1 calc R . . H43C H 0.1499 0.5875 0.2189 0.137 Uiso 1 1 calc R . . C44 C 0.0315(19) 0.4566(14) 0.2107(6) 0.061(7) Uani 1 1 d U . . H44A H -0.0174 0.4164 0.2200 0.091 Uiso 1 1 calc R . . H44B H 0.0554 0.4381 0.1896 0.091 Uiso 1 1 calc R . . H44C H -0.0145 0.5053 0.2071 0.091 Uiso 1 1 calc R . . C45 C 0.105(2) 0.5018(16) 0.2666(7) 0.085(9) Uani 1 1 d U . . H45A H 0.0798 0.5569 0.2642 0.128 Uiso 1 1 calc R . . H45B H 0.1737 0.4981 0.2835 0.128 Uiso 1 1 calc R . . H45C H 0.0396 0.4699 0.2733 0.128 Uiso 1 1 calc R . . C46 C 0.162(2) 0.2971(13) 0.2548(6) 0.053(7) Uani 1 1 d U . . C47 C 0.088(3) 0.2576(19) 0.2285(8) 0.114(12) Uani 1 1 d U . . H47A H 0.0904 0.2007 0.2325 0.170 Uiso 1 1 calc R . . H47B H 0.1177 0.2691 0.2073 0.170 Uiso 1 1 calc R . . H47C H 0.0058 0.2764 0.2281 0.170 Uiso 1 1 calc R . . C48 C 0.083(3) 0.3222(18) 0.2808(8) 0.108(11) Uani 1 1 d U . . H48A H 0.0406 0.2761 0.2882 0.162 Uiso 1 1 calc R . . H48B H 0.0247 0.3610 0.2713 0.162 Uiso 1 1 calc R . . H48C H 0.1316 0.3455 0.2997 0.162 Uiso 1 1 calc R . . C49 C 0.252(3) 0.2446(19) 0.2726(8) 0.119(12) Uani 1 1 d U . . H49A H 0.2218 0.2249 0.2928 0.179 Uiso 1 1 calc R . . H49B H 0.3260 0.2739 0.2785 0.179 Uiso 1 1 calc R . . H49C H 0.2678 0.2001 0.2584 0.179 Uiso 1 1 calc R . . C50 C 0.639(2) 0.2879(15) 0.2385(7) 0.069(8) Uani 1 1 d U . . C51 C 0.733(2) 0.2860(15) 0.2126(7) 0.075(9) Uani 1 1 d U . . H51A H 0.8084 0.2646 0.2231 0.113 Uiso 1 1 calc R . . H51B H 0.7460 0.3396 0.2048 0.113 Uiso 1 1 calc R . . H51C H 0.7032 0.2527 0.1939 0.113 Uiso 1 1 calc R . . C52 C 0.713(3) 0.2917(17) 0.2723(8) 0.101(11) Uani 1 1 d U . . H52A H 0.6627 0.2772 0.2895 0.151 Uiso 1 1 calc R . . H52B H 0.7433 0.3453 0.2762 0.151 Uiso 1 1 calc R . . H52C H 0.7799 0.2549 0.2727 0.151 Uiso 1 1 calc R . . C53 C 0.584(3) 0.2087(17) 0.2327(8) 0.105(11) Uani 1 1 d U . . H53A H 0.6469 0.1692 0.2317 0.157 Uiso 1 1 calc R . . H53B H 0.5324 0.2090 0.2118 0.157 Uiso 1 1 calc R . . H53C H 0.5370 0.1958 0.2508 0.157 Uiso 1 1 calc R . . C54 C 0.6172(18) 0.4644(12) 0.2257(6) 0.042(6) Uani 1 1 d U . . C55 C 0.669(2) 0.4679(13) 0.1933(6) 0.056(7) Uani 1 1 d U . . H55A H 0.7134 0.5171 0.1919 0.084 Uiso 1 1 calc R . . H55B H 0.6046 0.4656 0.1751 0.084 Uiso 1 1 calc R . . H55C H 0.7228 0.4231 0.1916 0.084 Uiso 1 1 calc R . . C56 C 0.539(2) 0.5366(15) 0.2312(7) 0.082(9) Uani 1 1 d U . . H56A H 0.5887 0.5838 0.2337 0.123 Uiso 1 1 calc R . . H56B H 0.4988 0.5287 0.2511 0.123 Uiso 1 1 calc R . . H56C H 0.4788 0.5430 0.2121 0.123 Uiso 1 1 calc R . . C57 C 0.725(2) 0.4760(16) 0.2535(7) 0.089(10) Uani 1 1 d U . . H57A H 0.7667 0.4258 0.2577 0.133 Uiso 1 1 calc R . . H57B H 0.6948 0.4943 0.2739 0.133 Uiso 1 1 calc R . . H57C H 0.7802 0.5152 0.2462 0.133 Uiso 1 1 calc R . . C58 C 0.736(3) 0.381(2) 0.1079(9) 0.120(12) Uani 1 1 d U . . H58A H 0.7007 0.4303 0.1148 0.143 Uiso 1 1 calc R . . H58B H 0.6826 0.3372 0.1129 0.143 Uiso 1 1 calc R . . C59 C 0.2750(17) 0.3742(12) 0.0867(6) 0.052(8) Uani 1 1 d . . . H59A H 0.2820 0.3226 0.0981 0.062 Uiso 1 1 calc R . . H59B H 0.2879 0.4159 0.1038 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0606(14) 0.0183(11) 0.0270(13) -0.0005(9) 0.0035(11) -0.0036(9) Ru2 0.0812(16) 0.0188(11) 0.0305(14) -0.0018(9) 0.0036(12) -0.0026(10) Ru3 0.0428(12) 0.0203(11) 0.0341(13) -0.0028(9) -0.0001(10) -0.0015(9) Cl1 0.111(5) 0.023(3) 0.028(4) -0.001(3) 0.007(4) 0.005(3) Cl2 0.073(4) 0.018(3) 0.042(4) 0.001(3) 0.007(4) 0.003(3) Cl3 0.076(4) 0.017(3) 0.056(5) -0.001(3) 0.011(4) -0.007(3) Cl4 0.162(7) 0.031(4) 0.050(5) 0.006(3) -0.012(5) 0.006(4) Cl5 0.045(4) 0.077(5) 0.044(5) -0.020(4) 0.000(3) 0.002(3) Cl6 0.041(4) 0.075(5) 0.040(4) -0.014(3) 0.004(3) 0.001(3) Cl7 0.103(7) 0.266(14) 0.089(9) -0.045(8) -0.013(6) 0.043(8) Cl8 0.135(7) 0.096(6) 0.071(7) 0.005(5) 0.007(6) -0.004(5) Cl9 0.280(13) 0.060(6) 0.148(10) 0.027(5) 0.144(10) 0.048(7) Cl10 0.189(10) 0.057(5) 0.115(8) 0.018(5) -0.079(7) -0.021(5) P1 0.058(4) 0.021(3) 0.045(5) -0.003(3) 0.018(4) -0.011(3) P2 0.050(4) 0.018(3) 0.042(5) -0.002(3) -0.001(4) -0.001(3) P3 0.080(5) 0.022(4) 0.043(5) -0.002(3) 0.003(4) 0.001(3) P4 0.082(5) 0.029(4) 0.039(5) 0.004(3) -0.005(4) 0.001(3) P5 0.050(4) 0.064(5) 0.035(5) -0.012(4) 0.005(4) 0.008(3) P6 0.056(4) 0.045(4) 0.022(4) -0.004(3) -0.004(4) -0.003(3) O1 0.069(11) 0.033(9) 0.032(11) 0.001(8) -0.013(9) 0.003(8) O2 0.149(17) 0.027(9) 0.033(12) -0.006(8) -0.004(12) 0.011(10) O3 0.165(19) 0.029(11) 0.055(15) 0.011(9) -0.008(13) -0.020(11) C1 0.028(6) 0.028(6) 0.029(6) -0.001(3) 0.003(3) 0.000(3) C2 0.041(7) 0.038(7) 0.040(7) 0.000(3) 0.004(3) 0.002(3) C3 0.054(8) 0.054(8) 0.053(8) 0.000(3) 0.005(3) 0.001(3) C4 0.053(7) 0.052(7) 0.054(7) -0.001(3) 0.004(3) 0.001(3) C5 0.070(8) 0.068(8) 0.070(9) -0.001(3) 0.010(3) -0.001(3) C6 0.073(9) 0.072(9) 0.072(9) 0.000(3) 0.008(3) 0.001(3) C7 0.118(12) 0.118(12) 0.118(12) 0.000(3) 0.013(3) 0.000(3) C8 0.051(7) 0.051(7) 0.052(7) -0.001(3) 0.006(3) 0.000(3) C9 0.117(12) 0.118(12) 0.117(12) -0.001(3) 0.011(3) 0.001(3) C10 0.034(6) 0.034(6) 0.033(6) 0.000(3) 0.003(3) -0.001(3) C11 0.064(8) 0.063(8) 0.063(8) 0.000(3) 0.008(3) 0.000(3) C12 0.096(10) 0.095(10) 0.095(10) -0.001(3) 0.012(3) -0.001(3) C13 0.104(11) 0.106(11) 0.104(11) 0.000(3) 0.012(3) 0.002(3) C14 0.086(10) 0.086(10) 0.085(10) 0.000(3) 0.009(3) -0.002(3) C15 0.043(7) 0.042(7) 0.043(7) 0.000(3) 0.006(3) -0.001(3) C16 0.130(13) 0.130(13) 0.130(13) 0.000(3) 0.014(3) -0.002(3) C17 0.147(15) 0.148(15) 0.148(15) 0.000(3) 0.016(3) 0.000(3) C18 0.045(7) 0.043(7) 0.044(7) -0.001(3) 0.005(3) 0.001(3) C19 0.085(10) 0.087(10) 0.086(10) 0.001(3) 0.008(3) -0.001(3) C20 0.086(10) 0.086(10) 0.086(10) -0.002(3) 0.008(3) 0.002(3) C21 0.070(9) 0.070(9) 0.070(9) 0.000(3) 0.006(3) -0.001(3) C22 0.074(9) 0.073(9) 0.074(9) 0.001(3) 0.006(3) 0.000(3) C23 0.067(8) 0.066(8) 0.066(8) 0.001(3) 0.009(3) 0.001(3) C24 0.081(9) 0.079(9) 0.080(9) 0.000(3) 0.009(3) -0.001(3) C25 0.125(13) 0.124(13) 0.125(13) 0.001(3) 0.014(3) 0.000(3) C26 0.126(13) 0.127(13) 0.126(13) 0.000(3) 0.014(3) -0.002(3) C27 0.054(7) 0.053(7) 0.054(7) 0.000(3) 0.006(3) -0.001(3) C28 0.061(8) 0.061(8) 0.062(8) 0.000(3) 0.006(3) 0.000(3) C29 0.126(13) 0.125(13) 0.127(13) 0.000(3) 0.012(3) -0.001(3) C30 0.060(8) 0.060(8) 0.061(8) 0.000(3) 0.007(3) 0.000(3) C31 0.144(15) 0.144(15) 0.143(15) -0.001(3) 0.016(3) -0.001(3) C32 0.058(8) 0.058(8) 0.059(8) 0.001(3) 0.006(3) 0.002(3) C33 0.159(16) 0.159(16) 0.160(16) 0.000(3) 0.018(3) 0.001(3) C34 0.092(10) 0.090(10) 0.091(10) 0.000(3) 0.010(3) 0.001(3) C35 0.183(19) 0.184(19) 0.183(19) -0.001(3) 0.020(4) 0.001(3) C36 0.096(11) 0.095(11) 0.096(11) 0.001(3) 0.010(3) -0.001(3) C37 0.20(2) 0.20(2) 0.20(2) 0.000(3) 0.019(4) 0.000(3) C38 0.145(15) 0.144(15) 0.144(15) 0.000(3) 0.015(3) 0.002(3) C39 0.12(2) 0.052(17) 0.032(18) 0.003(13) -0.033(17) -0.005(16) C40 0.11(3) 0.10(2) 0.09(3) -0.042(19) -0.06(2) 0.06(2) C41 0.081(9) 0.081(9) 0.081(9) 0.000(3) 0.008(3) -0.002(3) C42 0.055(8) 0.054(7) 0.055(8) 0.000(3) 0.007(3) 0.000(3) C43 0.091(10) 0.090(10) 0.093(10) 0.000(3) 0.011(3) 0.000(3) C44 0.061(8) 0.060(8) 0.061(8) 0.000(3) 0.006(3) 0.001(3) C45 0.086(10) 0.085(10) 0.085(10) 0.000(3) 0.009(3) 0.002(3) C46 0.053(7) 0.053(7) 0.053(7) 0.000(3) 0.006(3) 0.000(3) C47 0.114(12) 0.114(12) 0.113(12) 0.001(3) 0.012(3) -0.001(3) C48 0.109(11) 0.108(11) 0.108(12) 0.000(3) 0.012(3) -0.001(3) C49 0.119(12) 0.119(12) 0.119(12) 0.001(3) 0.013(3) -0.001(3) C50 0.069(8) 0.069(8) 0.070(9) 0.001(3) 0.006(3) -0.001(3) C51 0.076(9) 0.075(9) 0.075(9) -0.001(3) 0.008(3) 0.002(3) C52 0.101(11) 0.101(11) 0.100(11) 0.000(3) 0.010(3) 0.001(3) C53 0.105(11) 0.104(11) 0.105(11) 0.000(3) 0.010(3) 0.001(3) C54 0.042(7) 0.042(7) 0.042(7) -0.001(3) 0.004(3) 0.000(3) C55 0.056(7) 0.056(7) 0.056(8) 0.000(3) 0.006(3) -0.001(3) C56 0.081(9) 0.081(9) 0.083(9) -0.001(3) 0.009(3) 0.000(3) C57 0.089(10) 0.089(10) 0.089(10) 0.000(3) 0.008(3) -0.001(3) C58 0.119(12) 0.120(12) 0.119(12) 0.000(3) 0.013(3) 0.000(3) C59 0.041(15) 0.030(14) 0.08(2) -0.027(13) -0.001(16) 0.023(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.83(2) . ? Ru1 P1 2.379(6) . ? Ru1 P2 2.382(6) . ? Ru1 Cl3 2.477(6) . ? Ru1 Cl2 2.479(6) . ? Ru1 Cl1 2.548(6) . ? Ru2 C2 1.76(3) . ? Ru2 P4 2.369(6) . ? Ru2 P3 2.401(7) . ? Ru2 Cl3 2.475(6) . ? Ru2 Cl2 2.476(6) . ? Ru2 Cl1 2.543(6) . ? Ru3 C3 1.88(3) . ? Ru3 P6 2.368(6) . ? Ru3 P5 2.369(7) . ? Ru3 Cl5 2.452(6) . ? Ru3 Cl4 2.473(6) . ? Ru3 Cl6 2.478(6) . ? Cl7 C58 1.68(3) . ? Cl8 C58 1.69(3) . ? Cl9 C59 1.78(2) . ? Cl10 C59 1.72(2) . ? P1 C6 1.83(3) . ? P1 C5 1.85(2) . ? P1 C10 1.91(2) . ? P2 C4 1.78(2) . ? P2 C18 1.89(2) . ? P2 C14 1.89(3) . ? P3 C22 1.82(2) . ? P3 C24 1.86(3) . ? P3 C28 1.90(3) . ? P4 C23 1.85(2) . ? P4 C36 1.92(3) . ? P4 C32 1.92(3) . ? P5 C40 1.88(2) . ? P5 C42 1.88(2) . ? P5 C46 1.92(2) . ? P6 C41 1.83(3) . ? P6 C54 1.86(2) . ? P6 C50 1.93(3) . ? O1 C1 1.15(2) . ? O2 C2 1.19(2) . ? O3 C3 1.07(2) . ? C4 C5 1.40(3) . ? C6 C9 1.40(4) . ? C6 C8 1.46(3) . ? C6 C7 1.79(4) . ? C10 C11 1.52(3) . ? C10 C13 1.52(3) . ? C10 C12 1.54(3) . ? C14 C16 1.39(4) . ? C14 C15 1.47(3) . ? C14 C17 1.66(4) . ? C18 C20 1.47(3) . ? C18 C21 1.53(3) . ? C18 C19 1.55(3) . ? C22 C23 1.41(3) . ? C24 C27 1.48(3) . ? C24 C26 1.50(4) . ? C24 C25 1.58(4) . ? C28 C29 1.50(4) . ? C28 C31 1.50(4) . ? C28 C30 1.51(3) . ? C32 C35 1.38(4) . ? C32 C34 1.42(3) . ? C32 C33 1.56(4) . ? C36 C37 1.34(4) . ? C36 C38 1.48(4) . ? C36 C39 1.58(4) . ? C40 C41 1.43(3) . ? C42 C44 1.49(3) . ? C42 C45 1.50(3) . ? C42 C43 1.52(3) . ? C46 C47 1.45(3) . ? C46 C49 1.48(3) . ? C46 C48 1.52(3) . ? C50 C53 1.49(3) . ? C50 C52 1.53(3) . ? C50 C51 1.57(3) . ? C54 C55 1.50(3) . ? C54 C56 1.54(3) . ? C54 C57 1.58(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 P1 93.0(7) . . ? C1 Ru1 P2 93.6(6) . . ? P1 Ru1 P2 86.3(2) . . ? C1 Ru1 Cl3 85.0(6) . . ? P1 Ru1 Cl3 95.4(2) . . ? P2 Ru1 Cl3 177.9(2) . . ? C1 Ru1 Cl2 85.3(7) . . ? P1 Ru1 Cl2 178.1(2) . . ? P2 Ru1 Cl2 94.7(2) . . ? Cl3 Ru1 Cl2 83.64(19) . . ? C1 Ru1 Cl1 154.8(6) . . ? P1 Ru1 Cl1 105.6(2) . . ? P2 Ru1 Cl1 104.2(2) . . ? Cl3 Ru1 Cl1 76.7(2) . . ? Cl2 Ru1 Cl1 75.8(2) . . ? C2 Ru2 P4 94.6(7) . . ? C2 Ru2 P3 93.6(7) . . ? P4 Ru2 P3 86.2(2) . . ? C2 Ru2 Cl3 84.9(7) . . ? P4 Ru2 Cl3 178.8(2) . . ? P3 Ru2 Cl3 95.0(2) . . ? C2 Ru2 Cl2 84.1(7) . . ? P4 Ru2 Cl2 95.1(2) . . ? P3 Ru2 Cl2 177.5(2) . . ? Cl3 Ru2 Cl2 83.75(19) . . ? C2 Ru2 Cl1 154.2(7) . . ? P4 Ru2 Cl1 103.3(2) . . ? P3 Ru2 Cl1 105.9(2) . . ? Cl3 Ru2 Cl1 76.8(2) . . ? Cl2 Ru2 Cl1 76.0(2) . . ? C3 Ru3 P6 98.9(7) . . ? C3 Ru3 P5 90.9(8) . . ? P6 Ru3 P5 87.1(2) . . ? C3 Ru3 Cl5 80.7(7) . . ? P6 Ru3 Cl5 178.4(2) . . ? P5 Ru3 Cl5 91.4(2) . . ? C3 Ru3 Cl4 160.3(8) . . ? P6 Ru3 Cl4 96.6(2) . . ? P5 Ru3 Cl4 102.1(3) . . ? Cl5 Ru3 Cl4 84.2(2) . . ? C3 Ru3 Cl6 86.5(8) . . ? P6 Ru3 Cl6 90.1(2) . . ? P5 Ru3 Cl6 175.9(2) . . ? Cl5 Ru3 Cl6 91.4(2) . . ? Cl4 Ru3 Cl6 81.2(2) . . ? Ru2 Cl1 Ru1 83.52(18) . . ? Ru2 Cl2 Ru1 86.4(2) . . ? Ru2 Cl3 Ru1 86.4(2) . . ? C6 P1 C5 103.4(12) . . ? C6 P1 C10 106.2(11) . . ? C5 P1 C10 100.9(11) . . ? C6 P1 Ru1 118.1(10) . . ? C5 P1 Ru1 106.0(8) . . ? C10 P1 Ru1 119.5(6) . . ? C4 P2 C18 104.8(11) . . ? C4 P2 C14 103.1(12) . . ? C18 P2 C14 105.0(12) . . ? C4 P2 Ru1 104.9(8) . . ? C18 P2 Ru1 117.5(7) . . ? C14 P2 Ru1 119.6(10) . . ? C22 P3 C24 102.6(13) . . ? C22 P3 C28 102.0(12) . . ? C24 P3 C28 108.2(13) . . ? C22 P3 Ru2 107.4(9) . . ? C24 P3 Ru2 119.0(9) . . ? C28 P3 Ru2 115.5(9) . . ? C23 P4 C36 103.7(13) . . ? C23 P4 C32 101.5(11) . . ? C36 P4 C32 109.0(13) . . ? C23 P4 Ru2 105.4(8) . . ? C36 P4 Ru2 116.0(10) . . ? C32 P4 Ru2 118.9(8) . . ? C40 P5 C42 101.2(11) . . ? C40 P5 C46 101.5(14) . . ? C42 P5 C46 108.8(11) . . ? C40 P5 Ru3 106.1(10) . . ? C42 P5 Ru3 121.5(8) . . ? C46 P5 Ru3 114.7(8) . . ? C41 P6 C54 106.0(12) . . ? C41 P6 C50 102.6(13) . . ? C54 P6 C50 106.9(10) . . ? C41 P6 Ru3 104.3(9) . . ? C54 P6 Ru3 118.3(7) . . ? C50 P6 Ru3 117.0(8) . . ? O1 C1 Ru1 170.6(18) . . ? O2 C2 Ru2 169.7(18) . . ? O3 C3 Ru3 167(2) . . ? C5 C4 P2 123.2(18) . . ? C4 C5 P1 116.6(19) . . ? C9 C6 C8 123(3) . . ? C9 C6 C7 92(2) . . ? C8 C6 C7 99(2) . . ? C9 C6 P1 114(2) . . ? C8 C6 P1 119(2) . . ? C7 C6 P1 99.4(16) . . ? C11 C10 C13 108(2) . . ? C11 C10 C12 107.9(18) . . ? C13 C10 C12 107(2) . . ? C11 C10 P1 115.1(15) . . ? C13 C10 P1 107.2(16) . . ? C12 C10 P1 110.9(16) . . ? C16 C14 C15 120(3) . . ? C16 C14 C17 90(3) . . ? C15 C14 C17 105(2) . . ? C16 C14 P2 115(2) . . ? C15 C14 P2 115(2) . . ? C17 C14 P2 108(2) . . ? C20 C18 C21 112(2) . . ? C20 C18 C19 110(2) . . ? C21 C18 C19 104(2) . . ? C20 C18 P2 109.2(17) . . ? C21 C18 P2 115.4(16) . . ? C19 C18 P2 106.4(16) . . ? C23 C22 P3 118(2) . . ? C22 C23 P4 121.9(19) . . ? C27 C24 C26 103(3) . . ? C27 C24 C25 104(2) . . ? C26 C24 C25 108(3) . . ? C27 C24 P3 119(2) . . ? C26 C24 P3 111(2) . . ? C25 C24 P3 111(2) . . ? C29 C28 C31 112(3) . . ? C29 C28 C30 105(2) . . ? C31 C28 C30 104(2) . . ? C29 C28 P3 111(2) . . ? C31 C28 P3 111(2) . . ? C30 C28 P3 114.1(19) . . ? C35 C32 C34 116(3) . . ? C35 C32 C33 103(3) . . ? C34 C32 C33 104(2) . . ? C35 C32 P4 109(2) . . ? C34 C32 P4 119(2) . . ? C33 C32 P4 103(2) . . ? C37 C36 C38 111(3) . . ? C37 C36 C39 112(3) . . ? C38 C36 C39 106(3) . . ? C37 C36 P4 108(3) . . ? C38 C36 P4 107(2) . . ? C39 C36 P4 112(2) . . ? C41 C40 P5 114(2) . . ? C40 C41 P6 120(2) . . ? C44 C42 C45 110(2) . . ? C44 C42 C43 106(2) . . ? C45 C42 C43 105(2) . . ? C44 C42 P5 110.8(16) . . ? C45 C42 P5 115.5(18) . . ? C43 C42 P5 109.3(17) . . ? C47 C46 C49 113(2) . . ? C47 C46 C48 108(2) . . ? C49 C46 C48 105(2) . . ? C47 C46 P5 110(2) . . ? C49 C46 P5 109.0(18) . . ? C48 C46 P5 112.7(18) . . ? C53 C50 C52 111(2) . . ? C53 C50 C51 100(2) . . ? C52 C50 C51 105(2) . . ? C53 C50 P6 113.9(19) . . ? C52 C50 P6 113.1(19) . . ? C51 C50 P6 112.6(18) . . ? C55 C54 C56 112.3(19) . . ? C55 C54 C57 106.3(19) . . ? C56 C54 C57 102.0(19) . . ? C55 C54 P6 113.6(15) . . ? C56 C54 P6 108.2(15) . . ? C57 C54 P6 114.0(16) . . ? Cl7 C58 Cl8 115(2) . . ? Cl10 C59 Cl9 111.7(15) . . ? _diffrn_measured_fraction_theta_max 0.405 _diffrn_reflns_theta_full 27.37 _diffrn_measured_fraction_theta_full 0.405 _refine_diff_density_max 1.422 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.155 data_c:\backup\kappa\k03mkw8\maxus\k03mkw8 _database_code_depnum_ccdc_archive 'CCDC 250928' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H95 Cl4 N5 O2 P4 Ru2' _chemical_formula_weight 1242.1 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.6490(1) _cell_length_b 21.6770(2) _cell_length_c 35.1500(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11923.70(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Tabloid _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5200 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 125399 _diffrn_reflns_av_R_equivalents 0.1132 _diffrn_reflns_av_sigmaI/netI 0.1198 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 30.03 _reflns_number_total 17213 _reflns_number_gt 9708 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0384P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _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 17213 _refine_ls_number_parameters 615 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.244629(14) 0.221265(11) 0.027214(8) 0.01759(7) Uani 1 1 d . . . Ru2 Ru 0.032442(14) 0.100633(10) 0.276650(7) 0.01539(7) Uani 1 1 d . . . Cl1 Cl 0.15297(5) 0.13287(4) 0.01014(3) 0.0296(2) Uani 1 1 d . . . Cl2 Cl 0.13389(4) 0.26205(4) 0.07100(2) 0.0265(2) Uani 1 1 d . . . Cl3 Cl -0.07471(4) 0.02161(3) 0.29302(2) 0.02365(19) Uani 1 1 d . . . Cl4 Cl -0.06250(4) 0.18281(3) 0.30036(2) 0.02388(19) Uani 1 1 d . . . P1 P 0.35185(5) 0.18682(3) -0.01560(2) 0.01843(19) Uani 1 1 d . . . P2 P 0.33948(5) 0.30314(4) 0.04338(2) 0.01806(19) Uani 1 1 d . . . P3 P 0.12881(5) 0.02307(3) 0.25614(3) 0.01850(19) Uani 1 1 d . . . P4 P 0.13646(5) 0.17369(3) 0.25667(3) 0.01877(19) Uani 1 1 d . . . O1 O 0.14186(13) 0.28159(10) -0.03310(7) 0.0323(6) Uani 1 1 d . . . O2 O -0.07191(13) 0.11595(9) 0.20680(7) 0.0286(6) Uani 1 1 d . . . N1 N 0.27783(14) 0.16733(11) 0.07558(8) 0.0191(6) Uani 1 1 d . . . N2 N 0.06607(15) 0.09211(11) 0.33493(8) 0.0196(6) Uani 1 1 d . . . N3 N 0.1985(2) -0.06364(17) -0.08675(11) 0.0714(12) Uani 1 1 d . . . N4 N 0.1180(2) 0.03280(16) 0.11083(11) 0.0628(11) Uani 1 1 d . . . N5 N 0.03991(17) 0.47906(13) 0.10160(9) 0.0372(8) Uani 1 1 d . . . C1 C 0.18779(18) 0.26148(14) -0.01074(10) 0.0222(8) Uani 1 1 d . . . C2 C 0.28890(17) 0.13565(14) 0.10051(10) 0.0199(7) Uani 1 1 d . . . C3 C 0.3118(2) 0.09378(14) 0.13138(9) 0.0290(8) Uani 1 1 d . . . H3A H 0.3556 0.0649 0.1225 0.043 Uiso 1 1 calc R . . H3B H 0.2610 0.0707 0.1395 0.043 Uiso 1 1 calc R . . H3C H 0.3341 0.1176 0.1529 0.043 Uiso 1 1 calc R . . C4 C 0.44721(16) 0.23339(13) -0.00450(9) 0.0197(7) Uani 1 1 d . . . H4A H 0.4801 0.2124 0.0158 0.024 Uiso 1 1 calc R . . H4B H 0.4839 0.2354 -0.0274 0.024 Uiso 1 1 calc R . . C5 C 0.42689(17) 0.29906(13) 0.00844(9) 0.0210(7) Uani 1 1 d . . . H5A H 0.4113 0.3241 -0.0141 0.025 Uiso 1 1 calc R . . H5B H 0.4789 0.3174 0.0198 0.025 Uiso 1 1 calc R . . C6 C 0.39418(18) 0.10415(13) -0.01188(10) 0.0218(7) Uani 1 1 d . . . C7 C 0.3848(2) 0.08144(13) 0.02899(9) 0.0282(8) Uani 1 1 d . . . H7A H 0.3240 0.0785 0.0355 0.042 Uiso 1 1 calc R . . H7B H 0.4130 0.1105 0.0463 0.042 Uiso 1 1 calc R . . H7C H 0.4114 0.0407 0.0315 0.042 Uiso 1 1 calc R . . C8 C 0.3430(2) 0.05857(14) -0.03641(10) 0.0324(9) Uani 1 1 d . . . H8A H 0.3619 0.0164 -0.0310 0.049 Uiso 1 1 calc R . . H8B H 0.3523 0.0678 -0.0634 0.049 Uiso 1 1 calc R . . H8C H 0.2820 0.0625 -0.0305 0.049 Uiso 1 1 calc R . . C9 C 0.48981(19) 0.10053(14) -0.02176(10) 0.0303(8) Uani 1 1 d . . . H9A H 0.5069 0.0572 -0.0242 0.045 Uiso 1 1 calc R . . H9B H 0.5232 0.1201 -0.0015 0.045 Uiso 1 1 calc R . . H9C H 0.5003 0.1219 -0.0459 0.045 Uiso 1 1 calc R . . C10 C 0.33353(18) 0.20204(14) -0.06834(9) 0.0233(7) Uani 1 1 d . . . C11 C 0.33195(19) 0.27223(13) -0.07537(10) 0.0291(8) Uani 1 1 d . . . H11A H 0.3146 0.2804 -0.1017 0.044 Uiso 1 1 calc R . . H11B H 0.3891 0.2893 -0.0710 0.044 Uiso 1 1 calc R . . H11C H 0.2912 0.2916 -0.0579 0.044 Uiso 1 1 calc R . . C12 C 0.40623(19) 0.17807(15) -0.09404(9) 0.0308(8) Uani 1 1 d . . . H12A H 0.4094 0.1330 -0.0921 0.046 Uiso 1 1 calc R . . H12B H 0.4606 0.1961 -0.0858 0.046 Uiso 1 1 calc R . . H12C H 0.3948 0.1898 -0.1205 0.046 Uiso 1 1 calc R . . C13 C 0.24842(18) 0.17309(15) -0.08191(10) 0.0311(8) Uani 1 1 d . . . H13A H 0.2348 0.1883 -0.1075 0.047 Uiso 1 1 calc R . . H13B H 0.2025 0.1846 -0.0643 0.047 Uiso 1 1 calc R . . H13C H 0.2541 0.1281 -0.0825 0.047 Uiso 1 1 calc R . . C14 C 0.30197(19) 0.38670(13) 0.03865(10) 0.0254(8) Uani 1 1 d . . . C15 C 0.2380(2) 0.39101(14) 0.00611(11) 0.0381(10) Uani 1 1 d . . . H15A H 0.1870 0.3668 0.0124 0.057 Uiso 1 1 calc R . . H15B H 0.2640 0.3747 -0.0172 0.057 Uiso 1 1 calc R . . H15C H 0.2219 0.4342 0.0022 0.057 Uiso 1 1 calc R . . C16 C 0.3754(2) 0.43086(14) 0.02916(11) 0.0368(9) Uani 1 1 d . . . H16A H 0.3543 0.4734 0.0294 0.055 Uiso 1 1 calc R . . H16B H 0.3981 0.4211 0.0039 0.055 Uiso 1 1 calc R . . H16C H 0.4209 0.4263 0.0481 0.055 Uiso 1 1 calc R . . C17 C 0.2555(2) 0.40887(14) 0.07458(11) 0.0351(9) Uani 1 1 d . . . H17A H 0.2273 0.4483 0.0694 0.053 Uiso 1 1 calc R . . H17B H 0.2970 0.4142 0.0952 0.053 Uiso 1 1 calc R . . H17C H 0.2127 0.3782 0.0821 0.053 Uiso 1 1 calc R . . C18 C 0.39624(17) 0.29579(13) 0.09117(9) 0.0194(7) Uani 1 1 d . . . C19 C 0.45605(18) 0.35018(14) 0.10064(10) 0.0311(9) Uani 1 1 d . . . H19A H 0.4874 0.3412 0.1241 0.047 Uiso 1 1 calc R . . H19B H 0.4221 0.3878 0.1041 0.047 Uiso 1 1 calc R . . H19C H 0.4966 0.3562 0.0797 0.047 Uiso 1 1 calc R . . C20 C 0.33126(19) 0.28904(14) 0.12393(9) 0.0264(8) Uani 1 1 d . . . H20A H 0.2867 0.2596 0.1165 0.040 Uiso 1 1 calc R . . H20B H 0.3053 0.3292 0.1293 0.040 Uiso 1 1 calc R . . H20C H 0.3606 0.2739 0.1467 0.040 Uiso 1 1 calc R . . C21 C 0.45441(17) 0.23865(13) 0.09009(9) 0.0237(8) Uani 1 1 d . . . H21A H 0.5042 0.2472 0.0740 0.036 Uiso 1 1 calc R . . H21B H 0.4226 0.2036 0.0796 0.036 Uiso 1 1 calc R . . H21C H 0.4735 0.2288 0.1159 0.036 Uiso 1 1 calc R . . C22 C -0.02561(17) 0.10902(13) 0.23172(9) 0.0188(7) Uani 1 1 d . . . C23 C 0.07448(18) 0.09088(14) 0.36701(11) 0.0221(8) Uani 1 1 d . . . C24 C 0.0901(2) 0.09330(15) 0.40802(9) 0.0305(8) Uani 1 1 d . . . H24A H 0.1493 0.0811 0.4133 0.046 Uiso 1 1 calc R . . H24B H 0.0510 0.0650 0.4210 0.046 Uiso 1 1 calc R . . H24C H 0.0805 0.1354 0.4172 0.046 Uiso 1 1 calc R . . C25 C 0.21113(17) 0.06412(13) 0.22881(10) 0.0242(8) Uani 1 1 d . . . H25A H 0.2641 0.0391 0.2287 0.029 Uiso 1 1 calc R . . H25B H 0.1916 0.0683 0.2021 0.029 Uiso 1 1 calc R . . C26 C 0.23169(17) 0.12818(13) 0.24449(10) 0.0251(8) Uani 1 1 d . . . H26A H 0.2655 0.1511 0.2253 0.030 Uiso 1 1 calc R . . H26B H 0.2675 0.1236 0.2675 0.030 Uiso 1 1 calc R . . C27 C 0.09086(19) -0.03874(13) 0.22159(10) 0.0265(8) Uani 1 1 d . . . C28 C 0.0208(2) -0.01152(15) 0.19566(10) 0.0381(9) Uani 1 1 d . . . H28A H 0.0049 -0.0420 0.1763 0.057 Uiso 1 1 calc R . . H28B H 0.0425 0.0258 0.1832 0.057 Uiso 1 1 calc R . . H28C H -0.0294 -0.0011 0.2110 0.057 Uiso 1 1 calc R . . C29 C 0.1640(2) -0.06082(15) 0.19464(10) 0.0385(10) Uani 1 1 d . . . H29A H 0.2122 -0.0757 0.2099 0.058 Uiso 1 1 calc R . . H29B H 0.1828 -0.0263 0.1787 0.058 Uiso 1 1 calc R . . H29C H 0.1430 -0.0943 0.1784 0.058 Uiso 1 1 calc R . . C30 C 0.0519(2) -0.09440(13) 0.24190(11) 0.0381(10) Uani 1 1 d . . . H30A H 0.0082 -0.0803 0.2599 0.057 Uiso 1 1 calc R . . H30B H 0.0968 -0.1166 0.2557 0.057 Uiso 1 1 calc R . . H30C H 0.0259 -0.1220 0.2231 0.057 Uiso 1 1 calc R . . C31 C 0.19176(18) -0.01863(13) 0.29486(10) 0.0229(8) Uani 1 1 d . . . C32 C 0.24853(17) 0.02890(13) 0.31550(10) 0.0293(8) Uani 1 1 d . . . H32A H 0.2148 0.0658 0.3213 0.044 Uiso 1 1 calc R . . H32B H 0.2968 0.0401 0.2991 0.044 Uiso 1 1 calc R . . H32C H 0.2701 0.0109 0.3392 0.044 Uiso 1 1 calc R . . C33 C 0.13121(19) -0.04979(14) 0.32366(10) 0.0282(8) Uani 1 1 d . . . H33A H 0.1094 -0.0884 0.3129 0.042 Uiso 1 1 calc R . . H33B H 0.0833 -0.0221 0.3292 0.042 Uiso 1 1 calc R . . H33C H 0.1625 -0.0586 0.3472 0.042 Uiso 1 1 calc R . . C34 C 0.25472(19) -0.06748(14) 0.27932(10) 0.0328(9) Uani 1 1 d . . . H34A H 0.2886 -0.0843 0.3003 0.049 Uiso 1 1 calc R . . H34B H 0.2929 -0.0482 0.2607 0.049 Uiso 1 1 calc R . . H34C H 0.2226 -0.1009 0.2671 0.049 Uiso 1 1 calc R . . C35 C 0.11348(18) 0.21766(13) 0.21085(10) 0.0250(8) Uani 1 1 d . . . C36 C 0.02660(18) 0.25110(13) 0.21265(10) 0.0276(8) Uani 1 1 d . . . H36A H 0.0092 0.2633 0.1869 0.041 Uiso 1 1 calc R . . H36B H 0.0318 0.2879 0.2287 0.041 Uiso 1 1 calc R . . H36C H -0.0164 0.2234 0.2235 0.041 Uiso 1 1 calc R . . C37 C 0.18291(19) 0.26525(14) 0.20059(11) 0.0356(9) Uani 1 1 d . . . H37A H 0.2392 0.2455 0.2015 0.053 Uiso 1 1 calc R . . H37B H 0.1812 0.2994 0.2188 0.053 Uiso 1 1 calc R . . H37C H 0.1725 0.2811 0.1749 0.053 Uiso 1 1 calc R . . C38 C 0.11323(19) 0.17221(14) 0.17736(10) 0.0313(9) Uani 1 1 d . . . H38A H 0.0945 0.1936 0.1542 0.047 Uiso 1 1 calc R . . H38B H 0.0740 0.1381 0.1829 0.047 Uiso 1 1 calc R . . H38C H 0.1710 0.1559 0.1736 0.047 Uiso 1 1 calc R . . C39 C 0.17869(19) 0.23307(13) 0.29207(11) 0.0286(9) Uani 1 1 d . . . C40 C 0.12045(19) 0.28989(13) 0.29412(10) 0.0317(9) Uani 1 1 d . . . H40A H 0.0609 0.2766 0.2968 0.048 Uiso 1 1 calc R . . H40B H 0.1267 0.3142 0.2708 0.048 Uiso 1 1 calc R . . H40C H 0.1365 0.3151 0.3161 0.048 Uiso 1 1 calc R . . C41 C 0.1772(2) 0.20493(14) 0.33212(10) 0.0396(10) Uani 1 1 d . . . H41A H 0.2004 0.2347 0.3504 0.059 Uiso 1 1 calc R . . H41B H 0.2121 0.1674 0.3325 0.059 Uiso 1 1 calc R . . H41C H 0.1183 0.1947 0.3391 0.059 Uiso 1 1 calc R . . C42 C 0.27205(19) 0.25301(15) 0.28399(11) 0.0410(11) Uani 1 1 d . . . H42A H 0.2765 0.2682 0.2578 0.062 Uiso 1 1 calc R . . H42B H 0.3102 0.2176 0.2874 0.062 Uiso 1 1 calc R . . H42C H 0.2884 0.2859 0.3017 0.062 Uiso 1 1 calc R . . C43 C 0.1564(2) -0.0232(2) -0.08047(14) 0.0564(13) Uani 1 1 d . . . C44 C 0.0993(3) 0.0292(2) -0.07186(18) 0.105(2) Uani 1 1 d . . . H44A H 0.0400 0.0148 -0.0709 0.158 Uiso 1 1 calc R . . H44B H 0.1051 0.0607 -0.0917 0.158 Uiso 1 1 calc R . . H44C H 0.1150 0.0470 -0.0472 0.158 Uiso 1 1 calc R . . C45 C 0.0757(2) 0.07187(18) 0.09967(12) 0.0424(10) Uani 1 1 d . . . C46 C 0.0197(2) 0.11955(17) 0.08737(12) 0.0532(12) Uani 1 1 d . . . H46A H -0.0271 0.1241 0.1057 0.080 Uiso 1 1 calc R . . H46B H -0.0038 0.1090 0.0624 0.080 Uiso 1 1 calc R . . H46C H 0.0513 0.1585 0.0856 0.080 Uiso 1 1 calc R . . C47 C 0.0631(2) 0.44162(16) 0.12152(10) 0.0273(8) Uani 1 1 d . . . C48 C 0.0931(2) 0.39278(15) 0.14699(11) 0.0398(10) Uani 1 1 d . . . H48A H 0.0516 0.3868 0.1675 0.060 Uiso 1 1 calc R . . H48B H 0.1485 0.4045 0.1578 0.060 Uiso 1 1 calc R . . H48C H 0.0993 0.3543 0.1327 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01384(12) 0.02136(13) 0.01759(15) 0.00258(11) -0.00069(11) 0.00039(10) Ru2 0.01276(12) 0.01721(12) 0.01621(14) -0.00106(11) 0.00136(11) 0.00009(9) Cl1 0.0247(4) 0.0320(5) 0.0322(6) 0.0005(4) -0.0026(4) -0.0095(3) Cl2 0.0177(4) 0.0338(5) 0.0282(5) 0.0006(4) 0.0031(4) 0.0035(3) Cl3 0.0180(4) 0.0264(4) 0.0265(5) 0.0022(4) 0.0025(4) -0.0041(3) Cl4 0.0195(4) 0.0255(4) 0.0267(5) -0.0043(4) 0.0037(4) 0.0054(3) P1 0.0174(4) 0.0207(4) 0.0171(5) 0.0003(4) -0.0012(4) -0.0008(3) P2 0.0170(4) 0.0198(4) 0.0174(5) 0.0000(4) 0.0006(4) 0.0010(3) P3 0.0178(4) 0.0155(4) 0.0221(5) 0.0009(4) 0.0053(4) 0.0005(3) P4 0.0154(4) 0.0155(4) 0.0254(5) 0.0010(4) 0.0013(4) 0.0001(3) O1 0.0231(12) 0.0401(14) 0.0338(17) 0.0082(12) -0.0055(11) 0.0040(10) O2 0.0249(12) 0.0354(13) 0.0256(16) 0.0005(11) -0.0031(11) 0.0007(10) N1 0.0170(13) 0.0217(14) 0.0187(17) -0.0003(13) 0.0015(12) 0.0018(11) N2 0.0175(13) 0.0209(14) 0.0202(17) -0.0040(13) -0.0024(13) 0.0002(10) N3 0.067(3) 0.074(3) 0.073(3) 0.008(2) 0.010(2) 0.023(2) N4 0.071(2) 0.059(2) 0.058(3) -0.001(2) -0.001(2) 0.008(2) N5 0.0490(19) 0.0360(18) 0.027(2) -0.0054(15) -0.0012(16) 0.0055(15) C1 0.0152(16) 0.0268(18) 0.025(2) 0.0020(16) 0.0021(15) -0.0014(13) C2 0.0159(16) 0.0220(17) 0.022(2) -0.0028(16) 0.0027(15) 0.0003(13) C3 0.0346(19) 0.0332(19) 0.019(2) 0.0057(16) 0.0004(16) 0.0052(15) C4 0.0156(15) 0.0274(17) 0.0162(19) -0.0030(14) 0.0001(14) -0.0029(13) C5 0.0167(15) 0.0258(17) 0.020(2) -0.0026(15) -0.0002(14) -0.0043(13) C6 0.0276(17) 0.0198(16) 0.0181(19) -0.0039(15) 0.0016(15) 0.0033(13) C7 0.0379(19) 0.0225(17) 0.024(2) -0.0005(16) 0.0010(17) 0.0113(14) C8 0.042(2) 0.0254(18) 0.029(2) -0.0005(17) 0.0038(18) -0.0036(16) C9 0.0314(18) 0.0278(18) 0.032(2) -0.0067(17) 0.0016(16) 0.0122(15) C10 0.0279(17) 0.0277(18) 0.0142(19) 0.0005(15) -0.0021(15) -0.0044(14) C11 0.0317(18) 0.033(2) 0.022(2) 0.0089(16) -0.0070(16) -0.0046(15) C12 0.039(2) 0.037(2) 0.016(2) -0.0034(16) -0.0004(16) -0.0071(16) C13 0.0327(18) 0.038(2) 0.022(2) 0.0061(17) -0.0106(16) -0.0068(16) C14 0.0319(18) 0.0198(17) 0.025(2) -0.0012(15) -0.0012(16) 0.0024(14) C15 0.044(2) 0.0234(18) 0.047(3) 0.0071(18) -0.007(2) 0.0097(16) C16 0.048(2) 0.0239(18) 0.038(3) -0.0011(18) 0.0065(19) -0.0010(16) C17 0.0356(19) 0.0248(18) 0.045(3) -0.0030(18) 0.0074(19) 0.0068(15) C18 0.0186(15) 0.0235(17) 0.0160(19) -0.0032(14) -0.0018(14) -0.0027(13) C19 0.0291(18) 0.035(2) 0.029(2) -0.0078(17) -0.0019(17) -0.0048(15) C20 0.0329(18) 0.0322(19) 0.0141(19) -0.0029(15) 0.0026(16) 0.0020(15) C21 0.0191(16) 0.0325(18) 0.020(2) 0.0023(15) -0.0018(14) 0.0023(14) C22 0.0149(16) 0.0200(16) 0.021(2) 0.0021(14) 0.0037(14) 0.0022(12) C23 0.0167(16) 0.0228(17) 0.027(2) -0.0013(17) 0.0013(16) 0.0018(13) C24 0.0339(19) 0.042(2) 0.015(2) -0.0015(17) -0.0026(16) -0.0010(16) C25 0.0214(16) 0.0196(16) 0.032(2) 0.0052(16) 0.0112(15) 0.0053(13) C26 0.0161(16) 0.0205(16) 0.039(2) 0.0066(16) 0.0056(15) -0.0011(13) C27 0.0311(18) 0.0223(17) 0.026(2) -0.0085(16) 0.0057(17) 0.0008(14) C28 0.043(2) 0.038(2) 0.033(3) -0.0152(19) -0.0057(19) -0.0004(17) C29 0.049(2) 0.029(2) 0.038(3) -0.0126(18) 0.0114(19) 0.0051(17) C30 0.042(2) 0.0240(18) 0.049(3) -0.0102(18) 0.0049(19) -0.0120(16) C31 0.0196(16) 0.0199(17) 0.029(2) 0.0034(15) 0.0002(15) 0.0046(13) C32 0.0203(16) 0.0263(18) 0.041(2) 0.0050(17) -0.0036(17) 0.0017(14) C33 0.0318(18) 0.0262(18) 0.027(2) 0.0097(16) 0.0020(16) 0.0011(15) C34 0.0306(18) 0.0244(18) 0.043(3) 0.0056(17) 0.0025(18) 0.0074(15) C35 0.0227(17) 0.0225(17) 0.030(2) 0.0055(16) 0.0050(15) -0.0001(13) C36 0.0268(18) 0.0254(18) 0.031(2) 0.0062(16) -0.0015(16) 0.0044(14) C37 0.0321(19) 0.030(2) 0.044(3) 0.0140(18) 0.0115(18) 0.0027(15) C38 0.0345(19) 0.033(2) 0.026(2) 0.0088(17) 0.0082(17) 0.0050(16) C39 0.0250(17) 0.0173(17) 0.043(3) -0.0018(16) -0.0094(17) -0.0026(13) C40 0.0322(19) 0.0198(17) 0.043(3) -0.0046(17) 0.0016(18) -0.0026(14) C41 0.056(2) 0.0255(19) 0.037(3) -0.0049(18) -0.022(2) -0.0079(17) C42 0.0261(19) 0.0255(19) 0.072(3) -0.003(2) -0.0121(19) -0.0019(15) C43 0.039(2) 0.063(3) 0.068(4) 0.003(3) -0.004(2) 0.000(2) C44 0.058(3) 0.073(4) 0.184(7) -0.049(4) -0.035(4) 0.019(3) C45 0.046(2) 0.040(2) 0.041(3) -0.001(2) -0.005(2) 0.0046(19) C46 0.045(2) 0.058(3) 0.057(3) 0.010(2) -0.007(2) 0.003(2) C47 0.0286(18) 0.032(2) 0.022(2) -0.0075(17) 0.0072(16) -0.0012(15) C48 0.049(2) 0.036(2) 0.034(3) 0.0014(19) 0.008(2) 0.0083(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.825(3) . ? Ru1 N1 2.128(3) . ? Ru1 P1 2.3744(8) . ? Ru1 P2 2.3824(8) . ? Ru1 Cl1 2.4675(8) . ? Ru1 Cl2 2.4807(8) . ? Ru2 C22 1.831(3) . ? Ru2 N2 2.123(3) . ? Ru2 P3 2.3708(8) . ? Ru2 P4 2.3773(8) . ? Ru2 Cl3 2.4651(7) . ? Ru2 Cl4 2.4648(7) . ? P1 C4 1.843(3) . ? P1 C10 1.905(3) . ? P1 C6 1.915(3) . ? P2 C5 1.841(3) . ? P2 C18 1.907(3) . ? P2 C14 1.911(3) . ? P3 C25 1.837(3) . ? P3 C27 1.903(3) . ? P3 C31 1.908(3) . ? P4 C26 1.838(3) . ? P4 C35 1.905(3) . ? P4 C39 1.908(3) . ? O1 C1 1.151(3) . ? O2 C22 1.147(3) . ? N1 C2 1.127(4) . ? N2 C23 1.135(4) . ? N3 C43 1.119(5) . ? N4 C45 1.145(4) . ? N5 C47 1.132(4) . ? C2 C3 1.459(4) . ? C4 C5 1.528(4) . ? C6 C7 1.526(4) . ? C6 C8 1.537(4) . ? C6 C9 1.538(4) . ? C10 C11 1.541(4) . ? C10 C12 1.543(4) . ? C10 C13 1.548(4) . ? C14 C15 1.523(4) . ? C14 C17 1.534(4) . ? C14 C16 1.533(4) . ? C18 C20 1.543(4) . ? C18 C21 1.538(4) . ? C18 C19 1.542(4) . ? C23 C24 1.463(4) . ? C25 C26 1.528(4) . ? C27 C30 1.529(4) . ? C27 C28 1.543(4) . ? C27 C29 1.561(4) . ? C31 C32 1.542(4) . ? C31 C33 1.542(4) . ? C31 C34 1.546(4) . ? C35 C38 1.535(4) . ? C35 C37 1.541(4) . ? C35 C36 1.542(4) . ? C39 C40 1.534(4) . ? C39 C41 1.534(5) . ? C39 C42 1.550(4) . ? C43 C44 1.476(5) . ? C45 C46 1.422(5) . ? C47 C48 1.464(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 N1 164.91(11) . . ? C1 Ru1 P1 91.79(10) . . ? N1 Ru1 P1 99.27(6) . . ? C1 Ru1 P2 97.02(9) . . ? N1 Ru1 P2 93.82(7) . . ? P1 Ru1 P2 86.86(3) . . ? C1 Ru1 Cl1 84.82(9) . . ? N1 Ru1 Cl1 84.81(7) . . ? P1 Ru1 Cl1 90.71(3) . . ? P2 Ru1 Cl1 176.99(3) . . ? C1 Ru1 Cl2 86.72(10) . . ? N1 Ru1 Cl2 82.57(7) . . ? P1 Ru1 Cl2 177.43(3) . . ? P2 Ru1 Cl2 91.24(3) . . ? Cl1 Ru1 Cl2 91.24(3) . . ? C22 Ru2 N2 164.55(11) . . ? C22 Ru2 P3 97.11(9) . . ? N2 Ru2 P3 94.24(7) . . ? C22 Ru2 P4 91.08(9) . . ? N2 Ru2 P4 99.98(7) . . ? P3 Ru2 P4 86.97(3) . . ? C22 Ru2 Cl3 86.14(9) . . ? N2 Ru2 Cl3 83.28(7) . . ? P3 Ru2 Cl3 90.62(3) . . ? P4 Ru2 Cl3 176.07(3) . . ? C22 Ru2 Cl4 85.46(9) . . ? N2 Ru2 Cl4 83.45(7) . . ? P3 Ru2 Cl4 177.16(3) . . ? P4 Ru2 Cl4 91.79(3) . . ? Cl3 Ru2 Cl4 90.76(3) . . ? C4 P1 C10 103.48(14) . . ? C4 P1 C6 102.58(13) . . ? C10 P1 C6 106.31(14) . . ? C4 P1 Ru1 105.41(10) . . ? C10 P1 Ru1 117.14(10) . . ? C6 P1 Ru1 119.69(10) . . ? C5 P2 C18 103.74(13) . . ? C5 P2 C14 102.45(14) . . ? C18 P2 C14 107.39(14) . . ? C5 P2 Ru1 105.55(9) . . ? C18 P2 Ru1 115.98(9) . . ? C14 P2 Ru1 119.60(10) . . ? C25 P3 C27 103.06(15) . . ? C25 P3 C31 103.91(14) . . ? C27 P3 C31 106.42(14) . . ? C25 P3 Ru2 105.16(9) . . ? C27 P3 Ru2 119.66(10) . . ? C31 P3 Ru2 116.59(10) . . ? C26 P4 C35 103.00(15) . . ? C26 P4 C39 103.48(14) . . ? C35 P4 C39 106.20(14) . . ? C26 P4 Ru2 105.45(10) . . ? C35 P4 Ru2 116.98(10) . . ? C39 P4 Ru2 119.59(11) . . ? C2 N1 Ru1 173.7(2) . . ? C23 N2 Ru2 171.4(2) . . ? O1 C1 Ru1 169.9(3) . . ? N1 C2 C3 174.3(3) . . ? C5 C4 P1 113.88(19) . . ? C4 C5 P2 113.5(2) . . ? C7 C6 C8 105.7(3) . . ? C7 C6 C9 106.8(3) . . ? C8 C6 C9 110.4(3) . . ? C7 C6 P1 109.5(2) . . ? C8 C6 P1 112.5(2) . . ? C9 C6 P1 111.6(2) . . ? C11 C10 C12 104.5(2) . . ? C11 C10 C13 109.7(2) . . ? C12 C10 C13 108.5(3) . . ? C11 C10 P1 109.2(2) . . ? C12 C10 P1 113.6(2) . . ? C13 C10 P1 111.0(2) . . ? C15 C14 C17 106.7(3) . . ? C15 C14 C16 106.9(3) . . ? C17 C14 C16 109.8(3) . . ? C15 C14 P2 109.0(2) . . ? C17 C14 P2 111.8(2) . . ? C16 C14 P2 112.4(2) . . ? C20 C18 C21 109.4(2) . . ? C20 C18 C19 108.1(2) . . ? C21 C18 C19 105.2(2) . . ? C20 C18 P2 110.99(19) . . ? C21 C18 P2 108.7(2) . . ? C19 C18 P2 114.2(2) . . ? O2 C22 Ru2 170.2(3) . . ? N2 C23 C24 175.5(3) . . ? C26 C25 P3 113.5(2) . . ? C25 C26 P4 113.65(19) . . ? C30 C27 C28 107.1(3) . . ? C30 C27 C29 109.5(3) . . ? C28 C27 C29 106.3(3) . . ? C30 C27 P3 112.4(2) . . ? C28 C27 P3 109.2(2) . . ? C29 C27 P3 112.0(2) . . ? C32 C31 C33 109.7(3) . . ? C32 C31 C34 104.9(2) . . ? C33 C31 C34 108.9(2) . . ? C32 C31 P3 108.5(2) . . ? C33 C31 P3 111.01(19) . . ? C34 C31 P3 113.7(2) . . ? C38 C35 C37 104.6(3) . . ? C38 C35 C36 109.3(3) . . ? C37 C35 C36 108.5(2) . . ? C38 C35 P4 109.1(2) . . ? C37 C35 P4 113.6(2) . . ? C36 C35 P4 111.5(2) . . ? C40 C39 C41 105.5(3) . . ? C40 C39 C42 110.2(2) . . ? C41 C39 C42 107.0(3) . . ? C40 C39 P4 111.5(2) . . ? C41 C39 P4 109.0(2) . . ? C42 C39 P4 113.3(2) . . ? N3 C43 C44 178.7(5) . . ? N4 C45 C46 176.8(5) . . ? N5 C47 C48 179.5(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.818 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.126 data_c:\word_f~1\papers\inorga~1\mkw\august~1\jose3\jose3 _database_code_depnum_ccdc_archive 'CCDC 250929' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H50.33 F6 O10.67 P2 Ru S2' _chemical_formula_weight 814.76 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 28.2140(10) _cell_length_b 16.2490(4) _cell_length_c 22.7860(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.872(1) _cell_angle_gamma 90.00 _cell_volume 10048.0(6) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5060 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16717 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 22.80 _reflns_number_total 5303 _reflns_number_gt 5017 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.1260P)^2^+474.3392P] 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 5303 _refine_ls_number_parameters 781 _refine_ls_number_restraints 383 _refine_ls_R_factor_all 0.1244 _refine_ls_R_factor_gt 0.1203 _refine_ls_wR_factor_ref 0.2889 _refine_ls_wR_factor_gt 0.2853 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 3.133 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.83344(13) 0.0170(2) 0.72566(16) 0.0459(14) Uani 1 1 d . . . Ru2 Ru 1.0000 0.5053(3) 0.7500 0.0508(18) Uani 1 2 d S . . S101 S 0.9867(5) -0.0486(7) 0.6540(4) 0.070(4) Uani 1 1 d DU . . S201 S 0.8682(10) 0.2921(18) 0.6018(15) 0.069(11) Uani 0.40 1 d PDU A 6 S301 S 0.8705(10) 0.3019(14) 0.6255(13) 0.097(10) Uani 0.60 1 d PDU B 5 S401 S 0.9015(16) 0.297(3) 0.8330(17) 0.083(15) Uani 0.40 1 d PDU C 7 S501 S 0.8991(7) 0.2967(11) 0.8634(11) 0.060(6) Uani 0.60 1 d PDU D 8 P1 P 0.7878(4) -0.0289(6) 0.7925(5) 0.040(3) Uani 1 1 d . H . P2 P 0.7675(4) -0.0326(7) 0.6458(5) 0.045(3) Uani 1 1 d . H . P3 P 0.9929(4) 0.6116(6) 0.6770(6) 0.044(3) Uani 1 1 d . E . F101 F 1.0173(10) 0.0087(16) 0.5643(9) 0.113(10) Uani 1 1 d DU . . F102 F 0.9382(9) 0.0082(17) 0.5479(8) 0.116(10) Uani 1 1 d DU . . F103 F 0.9769(11) -0.1054(12) 0.5447(7) 0.092(9) Uani 1 1 d DU . . F201 F 0.881(3) 0.286(4) 0.493(2) 0.13(2) Uani 0.40 1 d PDU A 6 F202 F 0.870(3) 0.168(3) 0.531(3) 0.13(3) Uani 0.40 1 d PDU A 6 F203 F 0.9395(18) 0.231(5) 0.563(3) 0.13(3) Uani 0.40 1 d PDU A 6 F301 F 0.9133(19) 0.332(3) 0.5402(19) 0.133(19) Uani 0.60 1 d PDU B 5 F302 F 0.8427(17) 0.272(4) 0.5089(15) 0.148(19) Uani 0.60 1 d PDU B 5 F303 F 0.906(2) 0.203(3) 0.559(2) 0.14(2) Uani 0.60 1 d PDU B 5 F401 F 0.960(3) 0.344(5) 0.937(3) 0.15(4) Uani 0.40 1 d PDU C 7 F402 F 0.932(3) 0.221(4) 0.937(3) 0.12(3) Uani 0.40 1 d PDU C 7 F403 F 0.885(3) 0.325(7) 0.938(3) 0.24(9) Uani 0.40 1 d PDU C 7 F501 F 0.9814(15) 0.295(4) 0.950(2) 0.21(3) Uani 0.60 1 d PDU D 8 F502 F 0.9812(16) 0.219(4) 0.872(2) 0.20(3) Uani 0.60 1 d PDU D 8 F503 F 0.942(2) 0.179(3) 0.936(3) 0.21(3) Uani 0.60 1 d PDU D 8 O1 O 0.8954(12) 0.063(2) 0.7999(14) 0.070(10) Uani 1 1 d . H . O2 O 0.8761(12) 0.058(2) 0.6634(14) 0.069(10) Uani 1 1 d . H . O4 O 1.0077(13) 0.4079(18) 0.8175(19) 0.079(11) Uani 1 1 d . E . O5 O 1.073(3) 0.470(5) 0.766(3) 0.05(2) Uani 0.50 1 d PU E 2 O12 O 1.054(3) 0.142(5) 0.766(4) 0.09(2) Uani 0.50 1 d P . . O14 O 0.969(3) 0.249(6) 0.743(4) 0.12(3) Uani 0.50 1 d P . . O101 O 0.9898(11) 0.0296(9) 0.6807(9) 0.101(9) Uani 1 1 d DU . . O102 O 0.9452(7) -0.0924(15) 0.6594(9) 0.071(7) Uani 1 1 d DU . . O103 O 1.0303(7) -0.0941(15) 0.6764(9) 0.080(8) Uani 1 1 d DU . . O201 O 0.8175(11) 0.305(3) 0.577(2) 0.072(14) Uani 0.40 1 d PDU A 6 O202 O 0.8776(19) 0.239(3) 0.6523(18) 0.071(14) Uani 0.40 1 d PDU A 6 O203 O 0.8941(18) 0.367(2) 0.616(2) 0.074(14) Uani 0.40 1 d PDU A 6 O301 O 0.8480(17) 0.3797(17) 0.618(2) 0.106(13) Uani 0.60 1 d PDU B 5 O302 O 0.8388(15) 0.241(2) 0.637(2) 0.097(13) Uani 0.60 1 d PDU B 5 O303 O 0.9157(12) 0.303(3) 0.6708(14) 0.105(13) Uani 0.60 1 d PDU B 5 O401 O 0.882(4) 0.375(4) 0.815(3) 0.15(5) Uani 0.40 1 d PDU C 7 O402 O 0.944(2) 0.282(6) 0.814(3) 0.13(4) Uani 0.40 1 d PDU C 7 O403 O 0.866(3) 0.234(6) 0.814(3) 0.39(18) Uani 0.40 1 d PDU C 7 O501 O 0.8757(12) 0.330(2) 0.9050(16) 0.075(10) Uani 0.60 1 d PDU D 8 O502 O 0.9146(14) 0.358(2) 0.8294(18) 0.078(10) Uani 0.60 1 d PDU D 8 O503 O 0.8696(12) 0.2376(18) 0.8254(18) 0.076(11) Uani 0.60 1 d PDU D 8 C1 C 0.7312(16) -0.075(4) 0.745(2) 0.068(15) Uani 1 1 d . . . H1A H 0.7348 -0.1355 0.7496 0.082 Uiso 1 1 calc R F 1 H1B H 0.7041 -0.0587 0.7624 0.082 Uiso 1 1 calc R F 1 C3 C 0.7658(19) 0.054(3) 0.837(2) 0.064(13) Uani 1 1 d . . . C4 C 0.807(3) 0.096(6) 0.879(5) 0.17(5) Uani 1 1 d . H . H4A H 0.8305 0.1139 0.8559 0.261 Uiso 1 1 calc R . . H4B H 0.8243 0.0586 0.9114 0.261 Uiso 1 1 calc R . . H4C H 0.7955 0.1442 0.8962 0.261 Uiso 1 1 calc R . . C5 C 0.738(5) 0.119(6) 0.792(5) 0.22(7) Uani 1 1 d . H . H5A H 0.7099 0.0931 0.7628 0.334 Uiso 1 1 calc R . . H5B H 0.7605 0.1416 0.7696 0.334 Uiso 1 1 calc R . . H5C H 0.7268 0.1628 0.8138 0.334 Uiso 1 1 calc R . . C6 C 0.730(2) 0.026(4) 0.871(3) 0.079(17) Uani 1 1 d . H . H6A H 0.7016 -0.0007 0.8423 0.118 Uiso 1 1 calc R . . H6B H 0.7183 0.0735 0.8896 0.118 Uiso 1 1 calc R . . H6C H 0.7458 -0.0135 0.9028 0.118 Uiso 1 1 calc R . . C7 C 0.8170(19) -0.115(3) 0.848(2) 0.064(13) Uani 1 1 d . . . C8 C 0.784(2) -0.147(4) 0.885(3) 0.09(2) Uani 1 1 d . H . H8A H 0.7520 -0.1625 0.8581 0.140 Uiso 1 1 calc R . . H8B H 0.7793 -0.1032 0.9130 0.140 Uiso 1 1 calc R . . H8C H 0.7994 -0.1945 0.9092 0.140 Uiso 1 1 calc R . . C9 C 0.824(4) -0.189(4) 0.812(4) 0.17(5) Uani 1 1 d . H . H9A H 0.7918 -0.2069 0.7863 0.259 Uiso 1 1 calc R . . H9B H 0.8389 -0.2331 0.8401 0.259 Uiso 1 1 calc R . . H9C H 0.8453 -0.1745 0.7863 0.259 Uiso 1 1 calc R . . C10 C 0.866(2) -0.088(5) 0.887(4) 0.15(4) Uani 1 1 d . H . H10A H 0.8625 -0.0403 0.9109 0.227 Uiso 1 1 calc R . . H10B H 0.8875 -0.0736 0.8603 0.227 Uiso 1 1 calc R . . H10C H 0.8817 -0.1333 0.9138 0.227 Uiso 1 1 calc R . . C11 C 0.7330(16) 0.045(3) 0.589(2) 0.057(12) Uani 1 1 d . . . C12 C 0.765(3) 0.084(6) 0.554(5) 0.19(6) Uani 1 1 d . H . H12A H 0.7775 0.0421 0.5321 0.280 Uiso 1 1 calc R . . H12B H 0.7922 0.1125 0.5830 0.280 Uiso 1 1 calc R . . H12C H 0.7452 0.1243 0.5255 0.280 Uiso 1 1 calc R . . C13 C 0.715(4) 0.110(7) 0.621(5) 0.27(9) Uani 1 1 d . H . H13A H 0.6940 0.0863 0.6453 0.404 Uiso 1 1 calc R . . H13B H 0.6950 0.1495 0.5917 0.404 Uiso 1 1 calc R . . H13C H 0.7425 0.1393 0.6488 0.404 Uiso 1 1 calc R . . C14 C 0.685(2) 0.014(4) 0.546(3) 0.10(2) Uani 1 1 d . H . H14A H 0.6922 -0.0329 0.5224 0.152 Uiso 1 1 calc R . . H14B H 0.6701 0.0584 0.5176 0.152 Uiso 1 1 calc R . . H14C H 0.6625 -0.0030 0.5692 0.152 Uiso 1 1 calc R . . C15 C 0.782(2) -0.122(3) 0.601(2) 0.070(15) Uani 1 1 d . . . C16 C 0.737(2) -0.157(5) 0.555(3) 0.12(3) Uani 1 1 d . H . H16A H 0.7117 -0.1709 0.5751 0.181 Uiso 1 1 calc R . . H16B H 0.7462 -0.2074 0.5362 0.181 Uiso 1 1 calc R . . H16C H 0.7239 -0.1166 0.5225 0.181 Uiso 1 1 calc R . . C17 C 0.797(7) -0.192(5) 0.645(5) 0.29(10) Uani 1 1 d . H . H17A H 0.7699 -0.2037 0.6635 0.434 Uiso 1 1 calc R . . H17B H 0.8263 -0.1761 0.6775 0.434 Uiso 1 1 calc R . . H17C H 0.8039 -0.2407 0.6242 0.434 Uiso 1 1 calc R . . C18 C 0.821(2) -0.101(5) 0.570(4) 0.14(4) Uani 1 1 d . H . H18A H 0.8508 -0.0850 0.6013 0.207 Uiso 1 1 calc R . . H18B H 0.8093 -0.0558 0.5419 0.207 Uiso 1 1 calc R . . H18C H 0.8275 -0.1495 0.5481 0.207 Uiso 1 1 calc R . . C19 C 0.994(2) 0.709(3) 0.717(2) 0.067(14) Uani 1 1 d . . . H19A H 1.0187 0.7450 0.7056 0.081 Uiso 1 1 calc R E . H19B H 0.9617 0.7355 0.7011 0.081 Uiso 1 1 calc R . . C20 C 1.045(2) 0.621(3) 0.641(3) 0.084(19) Uani 1 1 d . . . C21 C 1.092(3) 0.648(5) 0.703(4) 0.13(3) Uani 1 1 d U E . H21A H 1.0840 0.6990 0.7206 0.198 Uiso 1 1 calc R . . H21B H 1.1223 0.6571 0.6892 0.198 Uiso 1 1 calc R . . H21C H 1.0985 0.6041 0.7331 0.198 Uiso 1 1 calc R . . C22 C 1.063(4) 0.548(7) 0.620(5) 0.19(5) Uani 1 1 d U E . H22A H 1.0633 0.5032 0.6493 0.287 Uiso 1 1 calc R . . H22B H 1.0963 0.5575 0.6170 0.287 Uiso 1 1 calc R . . H22C H 1.0413 0.5328 0.5802 0.287 Uiso 1 1 calc R . . C23 C 1.043(2) 0.696(3) 0.600(2) 0.067(14) Uani 1 1 d U E . H23A H 1.0388 0.7459 0.6225 0.101 Uiso 1 1 calc R . . H23B H 1.0145 0.6907 0.5639 0.101 Uiso 1 1 calc R . . H23C H 1.0731 0.6995 0.5875 0.101 Uiso 1 1 calc R . . C24 C 0.933(2) 0.621(3) 0.616(3) 0.09(2) Uani 1 1 d . . . C25 C 0.894(3) 0.581(5) 0.622(4) 0.13(3) Uani 1 1 d U E . H25A H 0.9045 0.5306 0.6461 0.196 Uiso 1 1 calc R . . H25B H 0.8725 0.5665 0.5821 0.196 Uiso 1 1 calc R . . H25C H 0.8761 0.6163 0.6437 0.196 Uiso 1 1 calc R . . C26 C 0.944(4) 0.550(6) 0.558(5) 0.16(4) Uani 1 1 d U E . H26A H 0.9730 0.5668 0.5462 0.239 Uiso 1 1 calc R . . H26B H 0.9149 0.5514 0.5220 0.239 Uiso 1 1 calc R . . H26C H 0.9480 0.4941 0.5745 0.239 Uiso 1 1 calc R . . C27 C 0.926(2) 0.698(3) 0.579(2) 0.068(14) Uani 1 1 d U E . H27A H 0.9558 0.7099 0.5658 0.101 Uiso 1 1 calc R . . H27B H 0.9195 0.7439 0.6032 0.101 Uiso 1 1 calc R . . H27C H 0.8980 0.6911 0.5425 0.101 Uiso 1 1 calc R . . C101 C 0.9796(7) -0.0341(10) 0.5768(5) 0.104(9) Uani 1 1 d DU . . C201 C 0.8899(17) 0.244(3) 0.547(2) 0.13(2) Uani 0.40 1 d PDU A 6 C301 C 0.8833(13) 0.277(2) 0.5576(13) 0.142(18) Uani 0.60 1 d PDU B 5 C401 C 0.920(2) 0.297(4) 0.9118(17) 0.31(19) Uani 0.40 1 d PDU C 7 C501 C 0.9514(11) 0.247(2) 0.9057(15) 0.21(3) Uani 0.60 1 d PDU D 8 O1A O 0.791(2) 0.195(4) 0.716(3) 0.054(15) Uani 0.50 1 d PU G 2 O2A O 1.111(3) 0.486(4) 0.768(3) 0.062(17) Uani 0.50 1 d PU E 1 O3A O 0.823(3) 0.134(4) 0.721(3) 0.047(16) Uani 0.50 1 d PU H 1 C1A C 0.798(3) 0.125(5) 0.721(3) 0.03(2) Uani 0.50 1 d PU G 2 C2A C 1.069(4) 0.501(7) 0.757(5) 0.05(3) Uani 0.50 1 d PU E 1 O1B O 0.884(3) -0.157(6) 0.734(4) 0.10(3) Uani 0.50 1 d PU H 1 O3B O 0.887(3) -0.071(4) 0.737(3) 0.043(16) Uani 0.50 1 d P H 2 C1B C 0.866(4) -0.092(6) 0.728(4) 0.04(3) Uani 0.50 1 d PU H 1 C2A2 C 0.733(4) -0.094(7) 0.684(4) 0.04(2) Uani 0.40 1 d PU H 2 H2A1 H 0.6983 -0.0942 0.6584 0.043 Uiso 0.40 1 calc PR H 2 H2A2 H 0.7451 -0.1511 0.6848 0.043 Uiso 0.40 1 calc PR H 2 C2A1 C 0.715(3) -0.057(5) 0.679(3) 0.044(18) Uani 0.60 1 d PU H 1 H2A3 H 0.6919 -0.0099 0.6715 0.053 Uiso 0.60 1 calc PR H 1 H2A4 H 0.6969 -0.1054 0.6570 0.053 Uiso 0.60 1 calc PR H 1 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 0.034(2) 0.059(3) 0.045(2) 0.0032(17) 0.0123(16) -0.0126(16) Ru2 0.048(4) 0.020(3) 0.084(4) 0.000 0.018(3) 0.000 S101 0.109(11) 0.053(7) 0.050(7) -0.002(6) 0.024(7) -0.003(6) S201 0.048(18) 0.041(18) 0.10(2) 0.029(16) -0.008(16) -0.010(13) S301 0.09(2) 0.042(13) 0.17(3) 0.010(16) 0.060(18) -0.017(13) S401 0.081(16) 0.080(16) 0.087(17) -0.004(9) 0.021(9) 0.003(9) S501 0.060(13) 0.038(10) 0.092(17) -0.006(10) 0.038(11) -0.010(8) P1 0.032(7) 0.042(6) 0.047(7) -0.003(5) 0.015(5) -0.005(5) P2 0.048(8) 0.045(7) 0.045(7) -0.010(5) 0.018(5) -0.013(5) P3 0.036(7) 0.027(6) 0.069(8) -0.006(5) 0.015(6) -0.003(4) F101 0.17(3) 0.101(19) 0.060(16) 0.009(15) 0.024(17) -0.047(18) F102 0.18(3) 0.10(2) 0.060(16) 0.007(15) 0.022(17) 0.016(18) F103 0.15(2) 0.080(17) 0.052(15) -0.010(13) 0.041(15) -0.026(16) F201 0.13(5) 0.13(5) 0.17(6) 0.04(5) 0.09(5) 0.03(4) F202 0.13(5) 0.12(5) 0.17(6) 0.04(5) 0.09(5) 0.03(4) F203 0.12(5) 0.12(5) 0.17(6) 0.04(5) 0.09(5) 0.03(4) F301 0.17(5) 0.09(3) 0.11(3) -0.01(3) 0.00(3) 0.01(3) F302 0.18(5) 0.10(3) 0.12(3) 0.00(3) -0.02(3) 0.00(3) F303 0.18(5) 0.10(3) 0.13(3) -0.01(3) -0.01(3) 0.01(3) F401 0.15(4) 0.15(4) 0.15(4) 0.000(10) 0.039(15) 0.000(10) F402 0.12(4) 0.12(4) 0.12(4) -0.001(9) 0.033(13) 0.001(9) F403 0.24(9) 0.24(9) 0.24(9) 0.000(10) 0.07(2) 0.001(10) F501 0.15(5) 0.30(8) 0.17(5) -0.07(5) 0.02(4) 0.12(5) F502 0.14(5) 0.29(8) 0.17(5) -0.07(5) 0.02(4) 0.12(5) F503 0.15(5) 0.30(8) 0.17(5) -0.05(5) 0.02(4) 0.12(5) O1 0.05(2) 0.10(3) 0.052(19) 0.018(18) 0.001(15) -0.033(18) O2 0.06(2) 0.10(3) 0.06(2) 0.022(19) 0.019(16) -0.022(18) O4 0.07(2) 0.031(17) 0.14(3) 0.034(19) 0.04(2) 0.007(15) O5 0.05(2) 0.05(2) 0.05(2) 0.001(9) 0.015(10) 0.001(9) O12 0.07(5) 0.07(5) 0.14(7) 0.03(5) 0.06(5) 0.02(4) O14 0.11(7) 0.10(7) 0.13(8) -0.02(6) 0.01(6) 0.04(5) O101 0.16(2) 0.068(15) 0.066(16) -0.009(14) 0.014(16) -0.001(16) O102 0.092(18) 0.075(16) 0.054(14) 0.000(13) 0.031(13) 0.003(14) O103 0.099(18) 0.078(16) 0.060(15) 0.005(14) 0.020(14) -0.011(14) O201 0.05(2) 0.05(2) 0.10(3) 0.03(2) -0.01(2) -0.01(2) O202 0.05(2) 0.05(2) 0.10(3) 0.03(2) 0.00(2) -0.01(2) O203 0.05(2) 0.04(2) 0.11(3) 0.02(2) -0.01(2) -0.01(2) O301 0.10(2) 0.050(19) 0.18(3) 0.01(2) 0.06(2) -0.008(19) O302 0.09(2) 0.043(19) 0.17(3) 0.01(2) 0.05(2) -0.027(18) O303 0.10(3) 0.057(19) 0.17(3) 0.01(2) 0.05(2) -0.03(2) O401 0.15(5) 0.15(5) 0.15(5) 0.001(10) 0.040(17) 0.000(10) O402 0.13(4) 0.13(4) 0.13(4) 0.000(10) 0.035(15) 0.000(10) O403 0.39(18) 0.39(18) 0.39(18) 0.000(10) 0.11(5) 0.000(10) O501 0.07(2) 0.063(19) 0.10(2) -0.013(18) 0.031(18) 0.014(17) O502 0.08(2) 0.058(18) 0.11(2) 0.010(18) 0.041(18) -0.015(17) O503 0.07(2) 0.046(18) 0.10(2) -0.021(18) 0.020(19) -0.013(17) C1 0.03(3) 0.11(4) 0.07(3) 0.00(3) 0.01(2) -0.02(3) C3 0.06(3) 0.06(3) 0.07(3) -0.01(3) 0.03(3) 0.00(3) C4 0.13(7) 0.18(8) 0.25(11) -0.17(9) 0.10(7) -0.09(6) C5 0.33(15) 0.18(9) 0.24(11) 0.13(9) 0.22(12) 0.21(10) C6 0.07(4) 0.10(4) 0.09(4) -0.02(3) 0.05(3) 0.00(3) C7 0.07(4) 0.05(3) 0.07(3) 0.01(3) 0.02(3) -0.01(2) C8 0.09(4) 0.10(5) 0.11(5) 0.06(4) 0.07(4) 0.02(3) C9 0.31(14) 0.07(5) 0.20(9) 0.03(5) 0.18(10) 0.08(7) C10 0.07(5) 0.15(7) 0.18(8) 0.12(6) -0.06(5) -0.04(4) C11 0.03(3) 0.06(3) 0.07(3) -0.01(2) -0.01(2) 0.00(2) C12 0.06(5) 0.21(10) 0.27(11) 0.19(9) 0.01(6) -0.01(5) C13 0.25(13) 0.28(14) 0.18(9) -0.12(10) -0.11(9) 0.23(12) C14 0.09(5) 0.11(5) 0.07(4) 0.02(4) -0.02(3) -0.03(4) C15 0.10(4) 0.05(3) 0.06(3) -0.02(3) 0.02(3) 0.00(3) C16 0.08(5) 0.15(6) 0.15(6) -0.12(6) 0.06(4) -0.06(4) C17 0.6(3) 0.05(5) 0.14(8) -0.01(5) 0.00(12) 0.11(10) C18 0.08(5) 0.16(7) 0.21(8) -0.12(7) 0.09(5) -0.01(4) C19 0.11(5) 0.03(2) 0.06(3) 0.01(2) 0.03(3) 0.00(2) C20 0.13(5) 0.03(2) 0.13(5) -0.01(3) 0.08(4) -0.01(3) C21 0.13(3) 0.13(3) 0.13(3) 0.001(9) 0.035(12) -0.001(9) C22 0.19(5) 0.19(5) 0.19(5) 0.000(10) 0.053(15) 0.000(10) C23 0.068(16) 0.068(16) 0.067(16) -0.001(9) 0.020(9) -0.002(9) C24 0.05(3) 0.07(3) 0.12(5) 0.02(3) -0.03(3) -0.04(3) C25 0.13(3) 0.13(3) 0.13(3) 0.003(9) 0.035(12) -0.002(9) C26 0.16(4) 0.16(4) 0.16(4) -0.001(10) 0.042(13) 0.000(10) C27 0.068(16) 0.068(16) 0.067(16) 0.000(9) 0.018(9) 0.002(9) C101 0.17(2) 0.092(18) 0.054(15) 0.003(13) 0.030(15) -0.020(16) C201 0.13(5) 0.13(5) 0.17(6) 0.04(4) 0.09(5) 0.03(4) C301 0.18(5) 0.10(3) 0.12(3) -0.01(3) -0.01(3) 0.01(3) C401 0.31(19) 0.31(19) 0.31(19) 0.000(10) 0.08(5) 0.000(10) C501 0.15(5) 0.29(8) 0.17(5) -0.06(5) 0.02(4) 0.12(5) O1A 0.054(17) 0.053(17) 0.055(17) -0.001(9) 0.012(10) 0.002(9) O2A 0.062(19) 0.062(19) 0.064(19) 0.000(9) 0.018(10) 0.000(9) O3A 0.048(18) 0.045(18) 0.048(18) 0.000(9) 0.012(10) 0.002(9) C1A 0.03(2) 0.03(2) 0.03(2) 0.000(9) 0.009(10) 0.000(9) C2A 0.05(3) 0.05(3) 0.05(3) 0.000(9) 0.014(12) -0.001(9) O1B 0.10(3) 0.10(3) 0.11(3) 0.000(9) 0.030(12) 0.001(9) O3B 0.03(4) 0.03(3) 0.07(4) 0.00(3) 0.02(3) 0.00(3) C1B 0.04(3) 0.04(3) 0.04(3) 0.000(9) 0.010(12) 0.001(9) C2A2 0.04(3) 0.04(3) 0.04(3) 0.000(9) 0.010(11) 0.000(9) C2A1 0.04(2) 0.04(2) 0.04(2) 0.000(9) 0.012(10) -0.001(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O3A 1.92(6) . ? Ru1 C1B 1.98(10) . ? Ru1 C1A 2.01(8) . ? Ru1 O3B 2.05(6) . ? Ru1 O2 2.20(3) . ? Ru1 O1 2.20(3) . ? Ru1 P2 2.360(12) . ? Ru1 P1 2.368(11) . ? Ru2 C2A 1.92(11) . ? Ru2 C2A 1.92(11) 2_756 ? Ru2 O5 2.07(7) 2_756 ? Ru2 O5 2.07(7) . ? Ru2 O4 2.18(3) 2_756 ? Ru2 O4 2.18(3) . ? Ru2 P3 2.369(12) 2_756 ? Ru2 P3 2.369(12) . ? S101 O101 1.401(8) . ? S101 O102 1.403(8) . ? S101 O103 1.406(8) . ? S101 C101 1.732(7) . ? S201 O203 1.404(8) . ? S201 O201 1.404(8) . ? S201 O202 1.405(8) . ? S201 C201 1.729(8) . ? S301 O302 1.404(8) . ? S301 O301 1.404(8) . ? S301 O303 1.405(8) . ? S301 C301 1.729(8) . ? S401 O403 1.404(8) . ? S401 O402 1.405(8) . ? S401 O401 1.405(8) . ? S401 C401 1.728(8) . ? S501 O503 1.403(8) . ? S501 O501 1.405(8) . ? S501 O502 1.405(8) . ? S501 C501 1.727(8) . ? P1 C1 1.83(4) . ? P1 C3 1.89(5) . ? P1 C7 1.91(5) . ? P2 C2A2 1.79(10) . ? P2 C11 1.88(5) . ? P2 C2A1 1.88(7) . ? P2 C15 1.89(5) . ? P3 C19 1.82(4) . ? P3 C20 1.87(5) . ? P3 C24 1.87(5) . ? F101 C101 1.362(8) . ? F102 C101 1.360(8) . ? F103 C101 1.362(8) . ? F201 C201 1.362(9) . ? F202 C201 1.364(9) . ? F203 C201 1.363(9) . ? F301 C301 1.364(9) . ? F302 C301 1.362(9) . ? F303 C301 1.363(9) . ? F401 C401 1.364(9) . ? F402 C401 1.363(9) . ? F403 C401 1.363(9) . ? F501 C501 1.364(9) . ? F502 C501 1.363(9) . ? F503 C501 1.363(9) . ? O14 O14 1.68(19) 2_756 ? C1 C2A2 1.43(11) . ? C1 C2A1 1.48(9) . ? C3 C4 1.46(8) . ? C3 C6 1.50(7) . ? C3 C5 1.54(9) . ? C7 C9 1.49(8) . ? C7 C10 1.50(8) . ? C7 C8 1.51(7) . ? C11 C13 1.47(9) . ? C11 C12 1.49(8) . ? C11 C14 1.52(7) . ? C15 C18 1.48(8) . ? C15 C17 1.50(10) . ? C15 C16 1.52(7) . ? C19 C19 1.45(9) 2_756 ? C20 C22 1.42(12) . ? C20 C23 1.53(7) . ? C20 C21 1.71(10) . ? C24 C25 1.33(9) . ? C24 C27 1.50(7) . ? C24 C26 1.83(11) . ? O1A C1A 1.15(9) . ? O2A C2A 1.15(12) . ? O1B C1B 1.17(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3A Ru1 C1B 161(4) . . ? O3A Ru1 C1A 21(2) . . ? C1B Ru1 C1A 178(4) . . ? O3A Ru1 O3B 143(3) . . ? C1B Ru1 O3B 19(3) . . ? C1A Ru1 O3B 163(3) . . ? O3A Ru1 O2 77(2) . . ? C1B Ru1 O2 87(3) . . ? C1A Ru1 O2 93(3) . . ? O3B Ru1 O2 77(2) . . ? O3A Ru1 O1 78(2) . . ? C1B Ru1 O1 91(3) . . ? C1A Ru1 O1 91(3) . . ? O3B Ru1 O1 75(2) . . ? O2 Ru1 O1 86.2(12) . . ? O3A Ru1 P2 102.5(19) . . ? C1B Ru1 P2 88(3) . . ? C1A Ru1 P2 89(2) . . ? O3B Ru1 P2 105(2) . . ? O2 Ru1 P2 93.5(9) . . ? O1 Ru1 P2 179.6(11) . . ? O3A Ru1 P1 104(2) . . ? C1B Ru1 P1 92(3) . . ? C1A Ru1 P1 88(3) . . ? O3B Ru1 P1 102.6(18) . . ? O2 Ru1 P1 179.1(11) . . ? O1 Ru1 P1 94.0(9) . . ? P2 Ru1 P1 86.3(4) . . ? C2A Ru2 C2A 175(7) . 2_756 ? C2A Ru2 O5 161(4) . 2_756 ? C2A Ru2 O5 15(4) 2_756 2_756 ? C2A Ru2 O5 15(4) . . ? C2A Ru2 O5 161(4) 2_756 . ? O5 Ru2 O5 148(4) 2_756 . ? C2A Ru2 O4 86(3) . 2_756 ? C2A Ru2 O4 91(4) 2_756 2_756 ? O5 Ru2 O4 77(2) 2_756 2_756 ? O5 Ru2 O4 80(2) . 2_756 ? C2A Ru2 O4 91(4) . . ? C2A Ru2 O4 86(3) 2_756 . ? O5 Ru2 O4 80(2) 2_756 . ? O5 Ru2 O4 77(2) . . ? O4 Ru2 O4 87(2) 2_756 . ? C2A Ru2 P3 95(3) . 2_756 ? C2A Ru2 P3 88(4) 2_756 2_756 ? O5 Ru2 P3 102(2) 2_756 2_756 ? O5 Ru2 P3 101(2) . 2_756 ? O4 Ru2 P3 179.1(9) 2_756 2_756 ? O4 Ru2 P3 93.5(11) . 2_756 ? C2A Ru2 P3 88(4) . . ? C2A Ru2 P3 95(3) 2_756 . ? O5 Ru2 P3 101(2) 2_756 . ? O5 Ru2 P3 102(2) . . ? O4 Ru2 P3 93.5(11) 2_756 . ? O4 Ru2 P3 179.1(9) . . ? P3 Ru2 P3 86.3(6) 2_756 . ? O101 S101 O102 112.2(8) . . ? O101 S101 O103 112.0(8) . . ? O102 S101 O103 111.7(8) . . ? O101 S101 C101 107.0(7) . . ? O102 S101 C101 106.9(7) . . ? O103 S101 C101 106.6(7) . . ? O203 S201 O201 111.8(8) . . ? O203 S201 O202 111.8(8) . . ? O201 S201 O202 111.8(8) . . ? O203 S201 C201 107.1(7) . . ? O201 S201 C201 107.0(7) . . ? O202 S201 C201 106.9(7) . . ? O302 S301 O301 111.9(8) . . ? O302 S301 O303 111.8(8) . . ? O301 S301 O303 111.7(8) . . ? O302 S301 C301 107.1(7) . . ? O301 S301 C301 107.0(7) . . ? O303 S301 C301 106.9(7) . . ? O403 S401 O402 111.8(8) . . ? O403 S401 O401 111.8(8) . . ? O402 S401 O401 111.6(8) . . ? O403 S401 C401 107.2(7) . . ? O402 S401 C401 107.1(7) . . ? O401 S401 C401 107.1(7) . . ? O503 S501 O501 111.8(8) . . ? O503 S501 O502 111.7(8) . . ? O501 S501 O502 111.6(8) . . ? O503 S501 C501 107.2(7) . . ? O501 S501 C501 107.0(7) . . ? O502 S501 C501 107.1(7) . . ? C1 P1 C3 104(2) . . ? C1 P1 C7 104(2) . . ? C3 P1 C7 108(2) . . ? C1 P1 Ru1 106.8(16) . . ? C3 P1 Ru1 116.2(16) . . ? C7 P1 Ru1 116.2(16) . . ? C2A2 P2 C11 117(4) . . ? C2A2 P2 C2A1 24(3) . . ? C11 P2 C2A1 96(3) . . ? C2A2 P2 C15 94(4) . . ? C11 P2 C15 107(2) . . ? C2A1 P2 C15 111(3) . . ? C2A2 P2 Ru1 104(3) . . ? C11 P2 Ru1 117.0(14) . . ? C2A1 P2 Ru1 108(2) . . ? C15 P2 Ru1 116.0(18) . . ? C19 P3 C20 104(2) . . ? C19 P3 C24 101(3) . . ? C20 P3 C24 109(3) . . ? C19 P3 Ru2 107.2(15) . . ? C20 P3 Ru2 116.1(19) . . ? C24 P3 Ru2 117.9(17) . . ? C2A2 C1 C2A1 31(4) . . ? C2A2 C1 P1 114(5) . . ? C2A1 C1 P1 120(4) . . ? C4 C3 C6 111(5) . . ? C4 C3 C5 106(8) . . ? C6 C3 C5 105(5) . . ? C4 C3 P1 111(4) . . ? C6 C3 P1 116(4) . . ? C5 C3 P1 107(4) . . ? C9 C7 C10 108(7) . . ? C9 C7 C8 103(5) . . ? C10 C7 C8 112(5) . . ? C9 C7 P1 109(5) . . ? C10 C7 P1 110(3) . . ? C8 C7 P1 114(4) . . ? C13 C11 C12 107(8) . . ? C13 C11 C14 101(6) . . ? C12 C11 C14 111(6) . . ? C13 C11 P2 109(5) . . ? C12 C11 P2 112(4) . . ? C14 C11 P2 115(4) . . ? C18 C15 C17 113(9) . . ? C18 C15 C16 110(5) . . ? C17 C15 C16 102(7) . . ? C18 C15 P2 112(4) . . ? C17 C15 P2 106(5) . . ? C16 C15 P2 113(4) . . ? C19 C19 P3 119.2(16) 2_756 . ? C22 C20 C23 115(6) . . ? C22 C20 C21 102(7) . . ? C23 C20 C21 101(5) . . ? C22 C20 P3 118(6) . . ? C23 C20 P3 115(4) . . ? C21 C20 P3 101(4) . . ? C25 C24 C27 119(6) . . ? C25 C24 C26 94(6) . . ? C27 C24 C26 98(5) . . ? C25 C24 P3 119(5) . . ? C27 C24 P3 116(3) . . ? C26 C24 P3 102(5) . . ? F102 C101 F101 104.9(8) . . ? F102 C101 F103 104.8(8) . . ? F101 C101 F103 104.8(8) . . ? F102 C101 S101 113.9(7) . . ? F101 C101 S101 113.7(7) . . ? F103 C101 S101 113.8(7) . . ? F201 C201 F203 104.7(8) . . ? F201 C201 F202 104.6(8) . . ? F203 C201 F202 104.5(8) . . ? F201 C201 S201 114.1(8) . . ? F203 C201 S201 114.0(8) . . ? F202 C201 S201 113.9(8) . . ? F302 C301 F303 104.7(8) . . ? F302 C301 F301 104.6(8) . . ? F303 C301 F301 104.6(8) . . ? F302 C301 S301 114.0(8) . . ? F303 C301 S301 114.0(8) . . ? F301 C301 S301 113.9(8) . . ? F403 C401 F402 104.6(8) . . ? F403 C401 F401 104.5(8) . . ? F402 C401 F401 104.5(8) . . ? F403 C401 S401 114.1(8) . . ? F402 C401 S401 114.1(8) . . ? F401 C401 S401 114.0(8) . . ? F502 C501 F503 104.6(8) . . ? F502 C501 F501 104.5(8) . . ? F503 C501 F501 104.5(8) . . ? F502 C501 S501 114.1(8) . . ? F503 C501 S501 114.1(8) . . ? F501 C501 S501 114.0(8) . . ? O1A C1A Ru1 160(8) . . ? O2A C2A Ru2 167(10) . . ? O1B C1B Ru1 174(9) . . ? C1 C2A2 P2 121(7) . . ? C1 C2A1 P2 113(5) . . ? _diffrn_measured_fraction_theta_max 0.778 _diffrn_reflns_theta_full 22.80 _diffrn_measured_fraction_theta_full 0.778 _refine_diff_density_max 1.678 _refine_diff_density_min -2.268 _refine_diff_density_rms 0.160 data_c:\word_f~1\papers\inorga~1\mkw\august~1\k03mkw12\k03mkw12 _database_code_depnum_ccdc_archive 'CCDC 250930' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H43.25 Cl2 F6 O9.63 P2 Ru S2' _chemical_formula_weight 873.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.9480(2) _cell_length_b 21.0360(3) _cell_length_c 22.6090(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.180(1) _cell_angle_gamma 90.00 _cell_volume 7440.98(17) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3570 _exptl_absorpt_coefficient_mu 0.837 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details ? _exptl_special_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61559 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.49 _reflns_number_total 16851 _reflns_number_gt 12168 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0764P)^2^+24.7646P] 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 SHELXL _refine_ls_extinction_coef 0.00076(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16851 _refine_ls_number_parameters 1012 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1713 _refine_ls_wR_factor_gt 0.1496 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru -0.08618(2) 0.811174(17) 0.259936(15) 0.02679(11) Uani 1 1 d . C . Ru2 Ru 0.09120(2) 1.131204(17) 0.247871(15) 0.02594(11) Uani 1 1 d . . . Cl1 Cl 0.0259 0.5864 0.5398 0.1126(18) Uiso 0.45 1 d P A 4 Cl2 Cl -0.0067 0.5836 0.5588 0.117(2) Uiso 0.40 1 d P A 4 Cl3 Cl -0.0649 0.5317 0.6129 0.093(4) Uiso 0.15 1 d P A 4 Cl4 Cl -0.0307 0.5110 0.6472 0.153(4) Uiso 0.35 1 d P A 4 Cl5 Cl 0.0252(19) 0.5195(18) 0.7003(14) 0.500(16) Uiso 0.55 1 d P A 4 Cl6 Cl -0.0222 0.4065 0.0077 0.1011(18) Uiso 0.40 1 d P B 5 Cl7 Cl -0.0622 0.4281(5) 0.0370(4) 0.111(2) Uiso 0.35 1 d P B 5 Cl9 Cl 0.0204 0.4630 0.1863 0.092(3) Uiso 0.20 1 d P B 5 Cl10 Cl 0.0001 0.4475 0.1846 0.268(7) Uiso 0.50 1 d P B 5 Cl11 Cl -0.0378 0.4954 0.0945 0.318(14) Uiso 0.30 1 d P B 5 S1 S 0.03961(8) 0.88041(5) 0.17579(5) 0.0321(3) Uani 1 1 d . C . S2 S -0.03784(7) 1.06256(5) 0.32860(5) 0.0268(2) Uani 1 1 d . . . S3 S -0.21410(9) 1.03795(7) 0.12584(6) 0.0424(3) Uani 1 1 d . . . S4 S 0.21039(7) 0.90470(6) 0.37181(5) 0.0331(3) Uani 1 1 d . . . P1 P -0.17974(8) 0.73999(6) 0.19850(5) 0.0324(3) Uani 1 1 d . . . P2 P -0.15006(8) 0.77776(6) 0.33993(5) 0.0306(3) Uani 1 1 d . . . P3 P 0.19143(8) 1.19473(6) 0.31293(6) 0.0348(3) Uani 1 1 d . . . P4 P 0.14836(8) 1.17554(6) 0.16884(5) 0.0348(3) Uani 1 1 d . . . F1 F 0.0344(3) 0.8273(2) 0.07142(16) 0.0741(12) Uani 1 1 d . C . F2 F -0.0444(3) 0.9082(2) 0.06802(16) 0.0729(11) Uani 1 1 d . C . F3 F 0.0907(3) 0.9189(3) 0.08019(18) 0.0936(16) Uani 1 1 d . C . F4 F -0.0123(3) 1.10979(19) 0.43709(14) 0.0633(10) Uani 1 1 d . . . F5 F 0.0293(2) 1.0132(2) 0.43314(15) 0.0685(11) Uani 1 1 d . . . F6 F -0.1039(2) 1.03445(17) 0.42124(14) 0.0531(8) Uani 1 1 d . . . F7 F -0.1412(4) 1.0318(3) 0.0324(2) 0.1094(19) Uani 1 1 d . . . F8 F -0.2589(5) 1.0829(3) 0.0173(2) 0.141(3) Uani 1 1 d . . . F9 F -0.2594(5) 0.9827(3) 0.0224(3) 0.141(3) Uani 1 1 d . . . F10 F 0.2753(4) 0.9667(3) 0.4692(2) 0.123(2) Uani 1 1 d . . . F11 F 0.2909(4) 0.8671(3) 0.47665(18) 0.107(2) Uani 1 1 d . . . F12 F 0.1680(4) 0.9097(3) 0.47709(19) 0.108(2) Uani 1 1 d . . . O1 O 0.0598(3) 0.7233(2) 0.2862(3) 0.0667(13) Uani 1 1 d . C . O2 O -0.0017(2) 0.87579(17) 0.31872(15) 0.0350(7) Uani 1 1 d D . . O3 O -0.1548(3) 0.90020(18) 0.23846(18) 0.0463(9) Uani 1 1 d D . . O4 O -0.0346(3) 0.8424(2) 0.18079(17) 0.0703(15) Uani 1 1 d . . . O5 O 0.1202(3) 0.8512(2) 0.19560(19) 0.0693(14) Uani 1 1 d . . . O6 O 0.0341(3) 0.94433(18) 0.19533(17) 0.0473(9) Uani 1 1 d . . . O7 O -0.0498(2) 1.22455(18) 0.23380(19) 0.0469(9) Uani 1 1 d . . . O8 O 0.0003(2) 1.07092(17) 0.18997(15) 0.0364(8) Uani 1 1 d D . . O9 O 0.1553(2) 1.04076(16) 0.25848(15) 0.0342(7) Uani 1 1 d D . . O10 O 0.04750(19) 1.08598(16) 0.32504(13) 0.0317(7) Uani 1 1 d . . . O11 O -0.1052(2) 1.10705(18) 0.31010(16) 0.0417(8) Uani 1 1 d . . . O12 O -0.0540(2) 0.99905(17) 0.30606(16) 0.0397(8) Uani 1 1 d . . . O13 O -0.1673(3) 1.0952(2) 0.1431(2) 0.0592(11) Uani 1 1 d . . . O14 O -0.2989(3) 1.0418(4) 0.1332(3) 0.100(2) Uani 1 1 d . . . O15 O -0.1643(3) 0.9822(2) 0.1469(2) 0.0679(13) Uani 1 1 d . . . O16 O 0.1579(2) 0.95946(18) 0.35364(16) 0.0409(8) Uani 1 1 d . . . O17 O 0.2916(2) 0.9041(2) 0.3535(2) 0.0559(11) Uani 1 1 d . . . O18 O 0.1645(2) 0.84527(18) 0.36320(18) 0.0455(9) Uani 1 1 d . . . O19 O 0.2560(4) 0.9511(3) 0.2267(3) 0.0944(18) Uani 1 1 d . . . O21 O -0.2522(15) 0.9997(13) 0.2635(13) 0.097(7) Uani 0.25 1 d P . . C1 C -0.0022(3) 0.7524(2) 0.2765(2) 0.0390(11) Uani 1 1 d . . . C2A C -0.2682(19) 0.7853(12) 0.1403(12) 0.028(5) Uani 0.45 1 d P C 1 C3 C -0.3307(19) 0.729(2) 0.1090(18) 0.048(7) Uani 0.55 1 d P C 2 H3A H -0.3615 0.7483 0.0716 0.071 Uiso 0.55 1 calc PR C 2 H3B H -0.3686 0.7261 0.1382 0.071 Uiso 0.55 1 calc PR C 2 H3C H -0.3118 0.6862 0.1003 0.071 Uiso 0.55 1 calc PR C 2 C4A C -0.2262(9) 0.8301(7) 0.1045(5) 0.043(3) Uani 0.45 1 d P C 1 H4A H -0.2686 0.8603 0.0836 0.064 Uiso 0.45 1 calc PR C 1 H4B H -0.2013 0.8063 0.0749 0.064 Uiso 0.45 1 calc PR C 1 H4C H -0.1810 0.8533 0.1315 0.064 Uiso 0.45 1 calc PR C 1 C5A C -0.3188(7) 0.8190(6) 0.1829(5) 0.036(3) Uani 0.45 1 d P C 1 H5A H -0.2810 0.8483 0.2093 0.054 Uiso 0.45 1 calc PR C 1 H5B H -0.3413 0.7873 0.2075 0.054 Uiso 0.45 1 calc PR C 1 H5C H -0.3664 0.8429 0.1590 0.054 Uiso 0.45 1 calc PR C 1 C6 C -0.1287(14) 0.6770(9) 0.1538(7) 0.048(4) Uani 0.55 1 d P C 3 C7 C -0.0470(7) 0.6512(7) 0.1906(6) 0.064(3) Uani 0.55 1 d P C 3 H7A H -0.0320 0.6114 0.1726 0.096 Uiso 0.55 1 calc PR C 3 H7B H -0.0547 0.6432 0.2319 0.096 Uiso 0.55 1 calc PR C 3 H7C H -0.0010 0.6823 0.1912 0.096 Uiso 0.55 1 calc PR C 3 C8 C -0.1084(9) 0.7035(7) 0.0952(5) 0.065(4) Uani 0.55 1 d P C 3 H8A H -0.0771 0.7436 0.1035 0.097 Uiso 0.55 1 calc PR C 3 H8B H -0.1618 0.7109 0.0663 0.097 Uiso 0.55 1 calc PR C 3 H8C H -0.0733 0.6728 0.0782 0.097 Uiso 0.55 1 calc PR C 3 C9 C -0.1903(18) 0.6213(13) 0.1391(11) 0.043(6) Uani 0.55 1 d P C 3 H9A H -0.1674 0.5908 0.1136 0.065 Uiso 0.55 1 calc PR C 3 H9B H -0.2459 0.6369 0.1177 0.065 Uiso 0.55 1 calc PR C 3 H9C H -0.1974 0.6004 0.1766 0.065 Uiso 0.55 1 calc PR C 3 C10 C -0.2560(8) 0.7081(8) 0.2459(7) 0.034(3) Uani 0.55 1 d P C 3 H10C H -0.3094 0.7334 0.2374 0.041 Uiso 0.55 1 calc PR C 3 H10D H -0.2707 0.6636 0.2339 0.041 Uiso 0.55 1 calc PR C 3 C11 C -0.2201(10) 0.7100(7) 0.3136(6) 0.035(3) Uani 0.55 1 d P C 3 H11C H -0.1876 0.6703 0.3250 0.042 Uiso 0.55 1 calc PR C 3 H11D H -0.2685 0.7105 0.3351 0.042 Uiso 0.55 1 calc PR C 3 C12A C -0.1953(9) 0.8426(8) 0.3834(6) 0.033(3) Uani 0.45 1 d P C 1 C13A C -0.270(3) 0.8177(18) 0.4099(18) 0.050(9) Uani 0.45 1 d P C 1 H13D H -0.2507 0.7816 0.4366 0.074 Uiso 0.45 1 calc PR C 1 H13E H -0.3160 0.8039 0.3772 0.074 Uiso 0.45 1 calc PR C 1 H13F H -0.2909 0.8515 0.4331 0.074 Uiso 0.45 1 calc PR C 1 C14A C -0.2327(9) 0.8959(7) 0.3394(6) 0.050(3) Uani 0.45 1 d P C 1 H14D H -0.2687 0.9237 0.3587 0.075 Uiso 0.45 1 calc PR C 1 H14E H -0.2672 0.8772 0.3029 0.075 Uiso 0.45 1 calc PR C 1 H14F H -0.1861 0.9208 0.3284 0.075 Uiso 0.45 1 calc PR C 1 C15A C -0.1303(8) 0.8715(7) 0.4337(5) 0.046(3) Uani 0.45 1 d P C 1 H15D H -0.0820 0.8880 0.4174 0.068 Uiso 0.45 1 calc PR C 1 H15E H -0.1098 0.8390 0.4641 0.068 Uiso 0.45 1 calc PR C 1 H15F H -0.1568 0.9063 0.4523 0.068 Uiso 0.45 1 calc PR C 1 C16 C -0.082(2) 0.7240(12) 0.3981(11) 0.051(5) Uani 0.55 1 d P C 3 C17 C -0.124(2) 0.7072(19) 0.4505(15) 0.086(12) Uani 0.55 1 d P C 3 H17A H -0.0938 0.6715 0.4728 0.129 Uiso 0.55 1 calc PR C 3 H17B H -0.1839 0.6952 0.4353 0.129 Uiso 0.55 1 calc PR C 3 H17C H -0.1221 0.7440 0.4773 0.129 Uiso 0.55 1 calc PR C 3 C18 C -0.0702(8) 0.6595(5) 0.3680(5) 0.053(3) Uani 0.55 1 d P C 3 H18A H -0.0580 0.6670 0.3277 0.080 Uiso 0.55 1 calc PR C 3 H18B H -0.1224 0.6342 0.3647 0.080 Uiso 0.55 1 calc PR C 3 H18C H -0.0223 0.6366 0.3926 0.080 Uiso 0.55 1 calc PR C 3 C19 C 0.0073(7) 0.7548(7) 0.4250(5) 0.053(3) Uani 0.55 1 d P C 3 H19A H 0.0518 0.7221 0.4292 0.080 Uiso 0.55 1 calc PR C 3 H19B H 0.0059 0.7732 0.4647 0.080 Uiso 0.55 1 calc PR C 3 H19C H 0.0199 0.7883 0.3979 0.080 Uiso 0.55 1 calc PR C 3 C21 C 0.0096(3) 1.1928(2) 0.2397(2) 0.0339(10) Uani 1 1 d . . . C22 C 0.2704(3) 1.1533(3) 0.3752(2) 0.0470(13) Uani 1 1 d . . . C23 C 0.3462(4) 1.1965(4) 0.4031(3) 0.067(2) Uani 1 1 d . . . H23A H 0.3281 1.2258 0.4319 0.100 Uiso 1 1 calc R . . H23B H 0.3652 1.2208 0.3711 0.100 Uiso 1 1 calc R . . H23C H 0.3935 1.1702 0.4241 0.100 Uiso 1 1 calc R . . C24 C 0.2238(4) 1.1296(4) 0.4242(3) 0.0611(18) Uani 1 1 d . . . H24A H 0.1764 1.1019 0.4061 0.092 Uiso 1 1 calc R . . H24B H 0.2015 1.1660 0.4433 0.092 Uiso 1 1 calc R . . H24C H 0.2638 1.1058 0.4546 0.092 Uiso 1 1 calc R . . C25 C 0.3107(4) 1.0953(4) 0.3496(3) 0.0578(16) Uani 1 1 d . . . H25A H 0.3487 1.0731 0.3825 0.087 Uiso 1 1 calc R . . H25B H 0.3437 1.1096 0.3198 0.087 Uiso 1 1 calc R . . H25C H 0.2655 1.0663 0.3304 0.087 Uiso 1 1 calc R . . C26 C 0.1428(4) 1.2646(3) 0.3475(3) 0.0480(14) Uani 1 1 d . . . C27 C 0.0659(4) 1.2430(3) 0.3748(3) 0.0498(14) Uani 1 1 d . . . H27A H 0.0864 1.2176 0.4111 0.075 Uiso 1 1 calc R . . H27B H 0.0273 1.2172 0.3452 0.075 Uiso 1 1 calc R . . H27C H 0.0352 1.2803 0.3854 0.075 Uiso 1 1 calc R . . C28 C 0.2067(4) 1.3001(4) 0.3972(3) 0.065(2) Uani 1 1 d . . . H28A H 0.2570 1.3129 0.3811 0.098 Uiso 1 1 calc R . . H28B H 0.2243 1.2719 0.4319 0.098 Uiso 1 1 calc R . . H28C H 0.1790 1.3380 0.4099 0.098 Uiso 1 1 calc R . . C29 C 0.1140(5) 1.3137(3) 0.2968(3) 0.0586(17) Uani 1 1 d . . . H29A H 0.0850 1.3492 0.3126 0.088 Uiso 1 1 calc R . . H29B H 0.0746 1.2934 0.2635 0.088 Uiso 1 1 calc R . . H29C H 0.1641 1.3297 0.2823 0.088 Uiso 1 1 calc R . . C30 C 0.2637(3) 1.2294(3) 0.2670(2) 0.0451(13) Uani 1 1 d . . . H30A H 0.2857 1.2705 0.2850 0.054 Uiso 1 1 calc R . . H30B H 0.3132 1.2007 0.2682 0.054 Uiso 1 1 calc R . . C31 C 0.2207(3) 1.2403(3) 0.2014(2) 0.0431(12) Uani 1 1 d . . . H31A H 0.2655 1.2454 0.1770 0.052 Uiso 1 1 calc R . . H31B H 0.1877 1.2804 0.1987 0.052 Uiso 1 1 calc R . . C32 C 0.0689(4) 1.2151(3) 0.1057(2) 0.0472(13) Uani 1 1 d . . . C33 C 0.0424(5) 1.2810(3) 0.1260(3) 0.0642(17) Uani 1 1 d . . . H33A H 0.0917 1.3096 0.1319 0.096 Uiso 1 1 calc R . . H33B H 0.0218 1.2766 0.1639 0.096 Uiso 1 1 calc R . . H33C H -0.0033 1.2985 0.0950 0.096 Uiso 1 1 calc R . . C34 C -0.0102(4) 1.1735(4) 0.0882(3) 0.0611(17) Uani 1 1 d . . . H34A H -0.0474 1.1912 0.0524 0.092 Uiso 1 1 calc R . . H34B H -0.0412 1.1722 0.1216 0.092 Uiso 1 1 calc R . . H34C H 0.0071 1.1304 0.0795 0.092 Uiso 1 1 calc R . . C35 C 0.1063(5) 1.2280(4) 0.0494(3) 0.069(2) Uani 1 1 d . . . H35A H 0.1091 1.1882 0.0274 0.104 Uiso 1 1 calc R . . H35B H 0.1639 1.2458 0.0614 0.104 Uiso 1 1 calc R . . H35C H 0.0698 1.2584 0.0234 0.104 Uiso 1 1 calc R . . C36 C 0.2195(4) 1.1184(3) 0.1364(2) 0.0461(13) Uani 1 1 d . . . C37 C 0.2907(4) 1.0969(3) 0.1885(3) 0.0542(15) Uani 1 1 d . . . H37A H 0.2666 1.0899 0.2247 0.081 Uiso 1 1 calc R . . H37B H 0.3348 1.1299 0.1967 0.081 Uiso 1 1 calc R . . H37C H 0.3160 1.0573 0.1775 0.081 Uiso 1 1 calc R . . C38 C 0.1667(4) 1.0612(3) 0.1092(3) 0.0542(15) Uani 1 1 d . . . H38A H 0.2047 1.0291 0.0970 0.081 Uiso 1 1 calc R . . H38B H 0.1248 1.0748 0.0738 0.081 Uiso 1 1 calc R . . H38C H 0.1369 1.0429 0.1392 0.081 Uiso 1 1 calc R . . C39 C 0.2668(5) 1.1462(4) 0.0886(3) 0.0653(18) Uani 1 1 d . . . H39A H 0.3129 1.1174 0.0831 0.098 Uiso 1 1 calc R . . H39B H 0.2909 1.1878 0.1022 0.098 Uiso 1 1 calc R . . H39C H 0.2265 1.1512 0.0502 0.098 Uiso 1 1 calc R . . C40 C -0.0300(3) 1.0541(3) 0.4097(2) 0.0375(11) Uani 1 1 d . . . C41 C -0.2196(6) 1.0343(4) 0.0451(3) 0.074(2) Uani 1 1 d . . . C42 C 0.0286(4) 0.8847(3) 0.0940(2) 0.0423(12) Uani 1 1 d . . . C43 C 0.2371(5) 0.9122(3) 0.4534(3) 0.069(2) Uani 1 1 d . . . C91 C 0.0287 0.5204 0.5912 0.120(6) Uiso 0.65 1 d P A 4 C92 C -0.0679(15) 0.5174 0.5931 0.081(6) Uiso 0.35 1 d P A 4 C93 C 0.0105 0.4646 0.1191 0.146(9) Uiso 0.55 1 d P B 5 C94 C 0.0234 0.4542 0.0746 0.083(5) Uiso 0.45 1 d P B 5 H201 H 0.047(2) 0.856(3) 0.331(3) 0.048(17) Uiso 1 1 d D . . H202 H -0.006(3) 0.9166(11) 0.309(2) 0.038(14) Uiso 1 1 d D . . H301 H -0.130(5) 0.933(3) 0.260(3) 0.10(3) Uiso 1 1 d D . . H302 H -0.142(5) 0.905(4) 0.2025(18) 0.09(3) Uiso 1 1 d D . . H801 H -0.002(4) 1.0296(11) 0.197(3) 0.057(18) Uiso 1 1 d D . . H802 H -0.054(2) 1.083(4) 0.179(3) 0.07(2) Uiso 1 1 d D . . H901 H 0.133(5) 1.024(3) 0.288(3) 0.09(3) Uiso 1 1 d D . . H902 H 0.180(6) 1.011(3) 0.241(4) 0.14(4) Uiso 1 1 d D . . C2 C -0.2545(18) 0.7687(13) 0.1346(14) 0.046(6) Uani 0.55 1 d P C 2 C3A C -0.334(3) 0.741(2) 0.101(2) 0.054(10) Uani 0.45 1 d P C 1 H3A1 H -0.3542 0.7088 0.1271 0.080 Uiso 0.45 1 calc PR C 1 H3A2 H -0.3074 0.7189 0.0713 0.080 Uiso 0.45 1 calc PR C 1 H3A3 H -0.3831 0.7656 0.0805 0.080 Uiso 0.45 1 calc PR C 1 C4 C -0.2115(10) 0.7828(12) 0.0780(6) 0.100(7) Uani 0.55 1 d P C 2 H4A1 H -0.2033 0.7427 0.0578 0.149 Uiso 0.55 1 calc PR C 2 H4A2 H -0.1560 0.8034 0.0916 0.149 Uiso 0.55 1 calc PR C 2 H4A3 H -0.2487 0.8109 0.0498 0.149 Uiso 0.55 1 calc PR C 2 C5 C -0.2946(16) 0.8360(9) 0.1463(9) 0.127(10) Uani 0.55 1 d P C 2 H5A1 H -0.3337 0.8499 0.1097 0.190 Uiso 0.55 1 calc PR C 2 H5A2 H -0.2487 0.8673 0.1572 0.190 Uiso 0.55 1 calc PR C 2 H5A3 H -0.3261 0.8321 0.1793 0.190 Uiso 0.55 1 calc PR C 2 C6A C -0.1329(14) 0.6639(9) 0.1755(8) 0.036(4) Uani 0.45 1 d P C 1 C7A C -0.1045(8) 0.6226(6) 0.2317(6) 0.047(3) Uani 0.45 1 d P C 1 H7A1 H -0.1548 0.6084 0.2469 0.070 Uiso 0.45 1 calc PR C 1 H7A2 H -0.0673 0.6475 0.2628 0.070 Uiso 0.45 1 calc PR C 1 H7A3 H -0.0731 0.5855 0.2212 0.070 Uiso 0.45 1 calc PR C 1 C8A C -0.0591(9) 0.6806(8) 0.1434(6) 0.052(3) Uani 0.45 1 d P C 1 H8A1 H -0.0210 0.7113 0.1678 0.079 Uiso 0.45 1 calc PR C 1 H8A2 H -0.0823 0.6992 0.1039 0.079 Uiso 0.45 1 calc PR C 1 H8A3 H -0.0270 0.6420 0.1381 0.079 Uiso 0.45 1 calc PR C 1 C9A C -0.195(3) 0.619(2) 0.1315(19) 0.081(14) Uani 0.45 1 d P C 1 H9A1 H -0.1684 0.5779 0.1293 0.122 Uiso 0.45 1 calc PR C 1 H9A2 H -0.2078 0.6387 0.0913 0.122 Uiso 0.45 1 calc PR C 1 H9A3 H -0.2486 0.6142 0.1464 0.122 Uiso 0.45 1 calc PR C 1 C10A C -0.2236(10) 0.6929(10) 0.2497(9) 0.035(4) Uani 0.45 1 d P C 1 H10A H -0.2773 0.6731 0.2283 0.042 Uiso 0.45 1 calc PR C 1 H10B H -0.1831 0.6583 0.2651 0.042 Uiso 0.45 1 calc PR C 1 C11A C -0.2422(11) 0.7318(8) 0.3032(8) 0.032(4) Uani 0.45 1 d P C 1 H11A H -0.2597 0.7027 0.3330 0.038 Uiso 0.45 1 calc PR C 1 H11B H -0.2904 0.7611 0.2887 0.038 Uiso 0.45 1 calc PR C 1 C12 C -0.2287(9) 0.8367(7) 0.3641(6) 0.047(3) Uani 0.55 1 d P C 3 C13 C -0.276(2) 0.810(2) 0.4131(14) 0.067(10) Uani 0.55 1 d P C 3 H13A H -0.2336 0.7967 0.4485 0.101 Uiso 0.55 1 calc PR C 3 H13B H -0.3102 0.7728 0.3968 0.101 Uiso 0.55 1 calc PR C 3 H13C H -0.3131 0.8425 0.4246 0.101 Uiso 0.55 1 calc PR C 3 C14 C -0.1863(10) 0.9010(7) 0.3816(8) 0.079(5) Uani 0.55 1 d P C 3 H14A H -0.1464 0.9108 0.3549 0.118 Uiso 0.55 1 calc PR C 3 H14B H -0.1551 0.8993 0.4234 0.118 Uiso 0.55 1 calc PR C 3 H14C H -0.2302 0.9341 0.3777 0.118 Uiso 0.55 1 calc PR C 3 C15 C -0.3027(7) 0.8478(6) 0.3100(6) 0.057(3) Uani 0.55 1 d P C 3 H15A H -0.3391 0.8824 0.3195 0.086 Uiso 0.55 1 calc PR C 3 H15B H -0.3366 0.8089 0.3017 0.086 Uiso 0.55 1 calc PR C 3 H15C H -0.2793 0.8593 0.2744 0.086 Uiso 0.55 1 calc PR C 3 C16A C -0.078(3) 0.7461(15) 0.4104(13) 0.052(7) Uani 0.45 1 d P C 2 C17A C -0.131(3) 0.7039(13) 0.4473(11) 0.054(10) Uani 0.45 1 d P C 2 H17D H -0.1602 0.6699 0.4214 0.081 Uiso 0.45 1 calc PR C 2 H17E H -0.1742 0.7303 0.4614 0.081 Uiso 0.45 1 calc PR C 2 H17F H -0.0929 0.6852 0.4820 0.081 Uiso 0.45 1 calc PR C 2 C18A C -0.0463(11) 0.8052(8) 0.4535(6) 0.066(4) Uani 0.45 1 d P C 2 H18D H -0.0028 0.7909 0.4876 0.099 Uiso 0.45 1 calc PR C 2 H18E H -0.0948 0.8234 0.4685 0.099 Uiso 0.45 1 calc PR C 2 H18F H -0.0218 0.8376 0.4307 0.099 Uiso 0.45 1 calc PR C 2 C19A C -0.0038(11) 0.7133(9) 0.3960(7) 0.064(4) Uani 0.45 1 d P C 2 H19D H 0.0334 0.7442 0.3813 0.097 Uiso 0.45 1 calc PR C 2 H19E H -0.0228 0.6813 0.3647 0.097 Uiso 0.45 1 calc PR C 2 H19F H 0.0279 0.6924 0.4323 0.097 Uiso 0.45 1 calc PR C 2 Cl8 Cl -0.0767(5) 0.4543(5) 0.0684(4) 0.112(2) Uiso 0.35 1 d P . . 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 0.0297(2) 0.0254(2) 0.02627(18) -0.00053(13) 0.00803(13) -0.00648(14) Ru2 0.02588(19) 0.02436(19) 0.02866(18) -0.00262(13) 0.00797(13) -0.00457(14) S1 0.0413(6) 0.0244(6) 0.0333(5) 0.0006(4) 0.0138(5) -0.0010(5) S2 0.0265(5) 0.0253(5) 0.0297(5) -0.0007(4) 0.0080(4) -0.0025(4) S3 0.0429(7) 0.0356(7) 0.0462(7) -0.0025(5) 0.0020(5) 0.0033(6) S4 0.0293(6) 0.0347(6) 0.0340(6) 0.0017(5) 0.0026(4) 0.0021(5) P1 0.0374(6) 0.0348(7) 0.0255(5) -0.0038(5) 0.0074(5) -0.0110(5) P2 0.0325(6) 0.0348(7) 0.0248(5) -0.0003(4) 0.0065(4) -0.0099(5) P3 0.0316(6) 0.0407(7) 0.0350(6) -0.0115(5) 0.0140(5) -0.0137(5) P4 0.0395(7) 0.0354(7) 0.0324(6) -0.0015(5) 0.0144(5) -0.0095(5) F1 0.116(3) 0.065(3) 0.0446(19) -0.0153(17) 0.023(2) 0.012(2) F2 0.077(3) 0.088(3) 0.049(2) 0.0071(19) 0.0027(18) 0.029(2) F3 0.100(3) 0.135(4) 0.056(2) 0.005(2) 0.039(2) -0.057(3) F4 0.093(3) 0.061(2) 0.0382(17) -0.0150(15) 0.0185(17) -0.024(2) F5 0.068(2) 0.095(3) 0.0450(18) 0.0284(19) 0.0163(16) 0.027(2) F6 0.0562(19) 0.062(2) 0.0500(18) -0.0031(15) 0.0313(15) -0.0138(17) F7 0.158(5) 0.100(4) 0.087(3) 0.006(3) 0.066(3) 0.036(4) F8 0.220(7) 0.130(5) 0.064(3) 0.022(3) 0.000(4) 0.095(5) F9 0.189(7) 0.129(5) 0.084(4) -0.052(4) -0.025(4) -0.023(5) F10 0.149(5) 0.096(4) 0.093(4) -0.044(3) -0.051(3) 0.006(4) F11 0.145(5) 0.112(4) 0.049(2) 0.008(2) -0.018(2) 0.073(4) F12 0.160(5) 0.123(5) 0.052(2) 0.013(2) 0.051(3) 0.057(4) O1 0.039(2) 0.044(2) 0.124(4) 0.002(2) 0.033(2) 0.007(2) O2 0.0333(18) 0.0291(18) 0.0407(18) -0.0005(14) 0.0026(14) -0.0050(15) O3 0.054(2) 0.029(2) 0.050(2) 0.0051(17) -0.0043(18) -0.0051(17) O4 0.105(4) 0.079(3) 0.034(2) -0.0133(19) 0.031(2) -0.059(3) O5 0.082(3) 0.072(3) 0.051(2) -0.002(2) 0.004(2) 0.044(3) O6 0.055(2) 0.0301(19) 0.057(2) -0.0093(16) 0.0091(18) 0.0056(17) O7 0.037(2) 0.035(2) 0.072(3) 0.0100(18) 0.0175(18) 0.0080(17) O8 0.040(2) 0.0265(18) 0.0386(18) 0.0009(14) -0.0030(14) -0.0084(15) O9 0.0353(18) 0.0331(18) 0.0359(17) 0.0015(14) 0.0113(14) 0.0025(15) O10 0.0273(16) 0.0360(18) 0.0321(16) 0.0021(13) 0.0066(12) -0.0071(14) O11 0.0361(19) 0.044(2) 0.047(2) 0.0059(16) 0.0129(15) 0.0107(16) O12 0.047(2) 0.0306(18) 0.0442(19) -0.0063(14) 0.0141(15) -0.0076(15) O13 0.055(3) 0.047(2) 0.074(3) -0.016(2) 0.009(2) -0.002(2) O14 0.061(3) 0.145(6) 0.100(4) -0.026(4) 0.031(3) -0.035(4) O15 0.104(4) 0.042(2) 0.060(3) 0.009(2) 0.020(2) 0.016(2) O16 0.0389(19) 0.038(2) 0.0443(19) 0.0069(15) 0.0050(15) 0.0059(16) O17 0.0317(19) 0.063(3) 0.074(3) 0.009(2) 0.0132(18) 0.0033(19) O18 0.040(2) 0.036(2) 0.061(2) -0.0042(17) 0.0085(17) 0.0008(16) O19 0.113(5) 0.079(4) 0.097(4) -0.003(3) 0.037(4) 0.031(4) O21 0.072(14) 0.089(18) 0.13(2) 0.003(15) 0.029(14) -0.005(13) C1 0.033(3) 0.031(3) 0.057(3) -0.005(2) 0.019(2) -0.007(2) C2A 0.021(9) 0.022(13) 0.038(8) 0.013(7) -0.001(6) 0.006(7) C3 0.039(10) 0.057(17) 0.037(12) 0.005(11) -0.016(7) -0.003(9) C4A 0.056(8) 0.055(8) 0.014(5) 0.010(5) 0.000(5) -0.023(6) C5A 0.032(5) 0.047(7) 0.024(5) 0.010(5) -0.007(4) -0.001(5) C6 0.056(9) 0.042(9) 0.047(10) -0.011(7) 0.010(8) -0.010(6) C7 0.052(7) 0.068(8) 0.078(9) -0.036(7) 0.025(6) -0.012(6) C8 0.080(8) 0.071(8) 0.051(6) -0.028(6) 0.033(6) -0.045(7) C9 0.051(12) 0.042(12) 0.042(7) -0.013(7) 0.021(7) 0.001(10) C10 0.032(8) 0.041(8) 0.030(5) -0.003(5) 0.011(6) -0.013(6) C11 0.044(8) 0.043(9) 0.019(6) 0.002(5) 0.005(5) -0.018(6) C12A 0.029(7) 0.046(8) 0.025(7) -0.012(6) 0.007(5) -0.015(6) C13A 0.048(14) 0.048(10) 0.067(17) -0.033(11) 0.046(12) -0.025(9) C14A 0.050(8) 0.053(8) 0.047(7) -0.004(6) 0.012(6) 0.002(6) C15A 0.046(7) 0.054(8) 0.042(6) -0.020(5) 0.023(5) -0.022(6) C16 0.050(9) 0.061(15) 0.039(12) 0.020(8) -0.002(8) -0.026(11) C17 0.053(13) 0.13(3) 0.07(2) 0.046(16) 0.015(12) -0.014(15) C18 0.059(7) 0.037(6) 0.060(6) 0.019(5) 0.002(5) -0.007(5) C19 0.038(5) 0.083(9) 0.033(5) 0.007(5) -0.007(4) -0.001(6) C21 0.038(3) 0.028(2) 0.039(2) 0.0007(19) 0.012(2) -0.009(2) C22 0.033(3) 0.067(4) 0.039(3) -0.008(2) 0.003(2) -0.016(3) C23 0.041(3) 0.096(6) 0.059(4) -0.023(4) 0.002(3) -0.026(3) C24 0.048(3) 0.095(6) 0.039(3) 0.001(3) 0.005(2) -0.012(3) C25 0.043(3) 0.074(5) 0.052(3) -0.002(3) -0.002(3) 0.004(3) C26 0.053(3) 0.043(3) 0.054(3) -0.021(3) 0.026(3) -0.017(3) C27 0.052(3) 0.050(3) 0.053(3) -0.020(3) 0.024(3) -0.011(3) C28 0.065(4) 0.069(4) 0.068(4) -0.040(3) 0.029(3) -0.032(3) C29 0.075(4) 0.033(3) 0.075(4) -0.016(3) 0.033(3) -0.013(3) C30 0.041(3) 0.054(3) 0.045(3) -0.013(2) 0.019(2) -0.024(3) C31 0.046(3) 0.042(3) 0.047(3) -0.005(2) 0.023(2) -0.017(2) C32 0.051(3) 0.053(3) 0.037(3) 0.011(2) 0.008(2) -0.012(3) C33 0.066(4) 0.053(4) 0.073(4) 0.015(3) 0.013(3) -0.005(3) C34 0.058(4) 0.069(4) 0.050(3) 0.018(3) -0.006(3) -0.015(3) C35 0.077(5) 0.086(5) 0.048(3) 0.025(3) 0.018(3) -0.013(4) C36 0.052(3) 0.053(3) 0.040(3) -0.006(2) 0.025(2) -0.007(3) C37 0.048(3) 0.066(4) 0.054(3) -0.007(3) 0.025(3) 0.003(3) C38 0.065(4) 0.054(4) 0.049(3) -0.017(3) 0.025(3) -0.008(3) C39 0.077(5) 0.074(5) 0.056(4) -0.002(3) 0.041(3) -0.005(4) C40 0.039(3) 0.041(3) 0.035(2) -0.001(2) 0.013(2) -0.004(2) C41 0.094(6) 0.072(5) 0.052(4) -0.001(3) 0.002(4) 0.031(4) C42 0.052(3) 0.043(3) 0.036(3) 0.004(2) 0.019(2) -0.003(2) C43 0.098(6) 0.056(4) 0.043(3) -0.004(3) -0.009(3) 0.027(4) C2 0.029(10) 0.033(13) 0.077(11) 0.013(9) 0.014(7) 0.003(8) C3A 0.09(2) 0.040(14) 0.029(12) 0.008(10) 0.002(13) -0.017(12) C4 0.061(8) 0.19(2) 0.044(7) 0.038(10) 0.000(6) -0.047(11) C5 0.18(2) 0.061(11) 0.092(14) -0.010(9) -0.090(15) 0.014(12) C6A 0.038(7) 0.030(9) 0.043(10) -0.016(7) 0.015(8) -0.010(6) C7A 0.038(6) 0.032(6) 0.070(8) -0.008(6) 0.008(5) 0.004(5) C8A 0.048(8) 0.067(9) 0.049(8) -0.028(7) 0.026(6) -0.006(7) C9A 0.068(19) 0.07(2) 0.11(2) -0.054(18) 0.011(17) -0.048(17) C10A 0.025(9) 0.050(12) 0.029(6) -0.003(6) 0.003(7) -0.021(7) C11A 0.032(8) 0.039(10) 0.022(7) 0.015(6) -0.001(5) -0.010(6) C12 0.048(8) 0.052(7) 0.045(8) -0.024(6) 0.019(6) -0.017(7) C13 0.045(12) 0.12(2) 0.040(10) 0.000(10) 0.014(9) -0.031(11) C14 0.080(10) 0.069(10) 0.102(12) -0.042(9) 0.054(9) -0.025(8) C15 0.053(7) 0.051(7) 0.073(7) -0.015(6) 0.023(6) -0.004(5) C16A 0.056(11) 0.07(2) 0.027(10) 0.013(10) -0.005(8) -0.027(14) C17A 0.10(2) 0.042(12) 0.017(9) 0.018(8) -0.009(10) -0.029(13) C18A 0.095(12) 0.063(10) 0.032(6) 0.002(6) -0.008(6) -0.033(9) C19A 0.070(11) 0.078(12) 0.040(7) 0.019(7) -0.004(7) 0.010(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.808(5) . ? Ru1 O3 2.176(4) . ? Ru1 O2 2.176(3) . ? Ru1 O4 2.209(4) . ? Ru1 P2 2.3490(11) . ? Ru1 P1 2.3652(12) . ? Ru2 C21 1.820(5) . ? Ru2 O9 2.151(3) . ? Ru2 O8 2.165(3) . ? Ru2 O10 2.215(3) . ? Ru2 P4 2.3505(12) . ? Ru2 P3 2.3649(12) . ? Cl1 Cl2 0.7389 . ? Cl1 C91 1.8063 . ? Cl2 C91 1.5699 . ? Cl2 C92 1.947(14) . ? Cl2 Cl3 1.9971 . ? Cl3 C92 0.5338(18) . ? Cl3 Cl4 0.9618 . ? Cl3 C91 1.6755 . ? Cl3 Cl5 2.22(3) . ? Cl4 C92 1.259(7) . ? Cl4 Cl5 1.36(3) . ? Cl4 C91 1.7336 . ? Cl6 Cl7 1.103(8) . ? Cl6 C94 1.8430 . ? Cl6 Cl8 2.027(10) . ? Cl7 Cl8 0.960(10) . ? Cl7 C94 1.561(5) . ? Cl7 Cl11 1.910(10) . ? Cl7 C93 2.132(8) . ? Cl9 C93 1.4971 . ? Cl9 Cl11 2.2102 . ? Cl10 C93 1.5619 . ? Cl10 Cl11 2.2460 . ? Cl11 C93 1.0750 . ? Cl11 Cl8 1.157(9) . ? Cl11 C94 1.4413 . ? S1 O5 1.416(4) . ? S1 O6 1.423(4) . ? S1 O4 1.451(4) . ? S1 C42 1.824(5) . ? S2 O11 1.425(4) . ? S2 O12 1.435(4) . ? S2 O10 1.464(3) . ? S2 C40 1.822(5) . ? S3 O14 1.397(5) . ? S3 O13 1.431(5) . ? S3 O15 1.444(5) . ? S3 C41 1.813(7) . ? S4 O17 1.434(4) . ? S4 O16 1.436(4) . ? S4 O18 1.443(4) . ? S4 C43 1.817(6) . ? P1 C10A 1.77(2) . ? P1 C2 1.79(3) . ? P1 C6A 1.88(2) . ? P1 C10 1.893(15) . ? P1 C6 1.94(2) . ? P1 C2A 1.98(2) . ? P2 C11A 1.819(18) . ? P2 C11 1.838(15) . ? P2 C16A 1.89(4) . ? P2 C16 1.90(3) . ? P2 C12A 1.902(16) . ? P2 C12 1.916(14) . ? P3 C30 1.844(5) . ? P3 C26 1.901(6) . ? P3 C22 1.908(6) . ? P4 C31 1.843(5) . ? P4 C36 1.896(6) . ? P4 C32 1.907(6) . ? F1 C42 1.322(7) . ? F2 C42 1.296(7) . ? F3 C42 1.310(6) . ? F4 C40 1.330(6) . ? F5 C40 1.310(6) . ? F6 C40 1.322(6) . ? F7 C41 1.337(10) . ? F8 C41 1.296(9) . ? F9 C41 1.310(11) . ? F10 C43 1.316(10) . ? F11 C43 1.318(8) . ? F12 C43 1.316(10) . ? O1 C1 1.147(6) . ? O7 C21 1.145(6) . ? C2A C4A 1.48(3) . ? C2A C5A 1.54(3) . ? C2A C3A 1.56(6) . ? C3 C2 1.50(5) . ? C6 C7 1.50(2) . ? C6 C9 1.53(4) . ? C6 C8 1.528(18) . ? C10 C11 1.53(2) . ? C12A C15A 1.511(17) . ? C12A C13A 1.53(4) . ? C12A C14A 1.54(2) . ? C16 C17 1.51(4) . ? C16 C18 1.55(3) . ? C16 C19 1.58(3) . ? C22 C24 1.533(8) . ? C22 C25 1.543(9) . ? C22 C23 1.546(8) . ? C26 C29 1.545(9) . ? C26 C27 1.544(7) . ? C26 C28 1.554(8) . ? C30 C31 1.526(8) . ? C32 C34 1.523(8) . ? C32 C35 1.531(8) . ? C32 C33 1.544(10) . ? C36 C38 1.528(8) . ? C36 C37 1.537(9) . ? C36 C39 1.548(7) . ? C91 C92 1.55(2) . ? C93 C94 1.0886 . ? C93 Cl8 1.637(9) . ? C94 Cl8 1.575(9) . ? C2 C4 1.59(3) . ? C2 C5 1.60(2) . ? C6A C7A 1.53(2) . ? C6A C8A 1.54(2) . ? C6A C9A 1.57(4) . ? C10A C11A 1.54(3) . ? C12 C14 1.530(18) . ? C12 C15 1.544(19) . ? C12 C13 1.56(4) . ? C16A C19A 1.46(5) . ? C16A C17A 1.57(5) . ? C16A C18A 1.60(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 O3 162.77(19) . . ? C1 Ru1 O2 87.40(19) . . ? O3 Ru1 O2 79.86(14) . . ? C1 Ru1 O4 89.6(2) . . ? O3 Ru1 O4 79.23(19) . . ? O2 Ru1 O4 91.43(14) . . ? C1 Ru1 P2 92.92(16) . . ? O3 Ru1 P2 98.91(12) . . ? O2 Ru1 P2 91.52(10) . . ? O4 Ru1 P2 176.18(14) . . ? C1 Ru1 P1 92.65(16) . . ? O3 Ru1 P1 100.43(11) . . ? O2 Ru1 P1 178.32(10) . . ? O4 Ru1 P1 90.25(11) . . ? P2 Ru1 P1 86.81(4) . . ? C21 Ru2 O9 162.92(17) . . ? C21 Ru2 O8 88.49(18) . . ? O9 Ru2 O8 78.32(14) . . ? C21 Ru2 O10 93.31(17) . . ? O9 Ru2 O10 75.39(12) . . ? O8 Ru2 O10 87.06(12) . . ? C21 Ru2 P4 90.88(15) . . ? O9 Ru2 P4 100.93(9) . . ? O8 Ru2 P4 94.91(10) . . ? O10 Ru2 P4 175.42(9) . . ? C21 Ru2 P3 92.57(15) . . ? O9 Ru2 P3 100.43(10) . . ? O8 Ru2 P3 178.46(10) . . ? O10 Ru2 P3 91.76(9) . . ? P4 Ru2 P3 86.20(4) . . ? Cl2 Cl1 C91 59.769(1) . . ? Cl1 Cl2 C91 96.237(1) . . ? Cl1 Cl2 C92 138.8(4) . . ? C91 Cl2 C92 50.9(6) . . ? Cl1 Cl2 Cl3 149.651(1) . . ? C91 Cl2 Cl3 54.452(1) . . ? C92 Cl2 Cl3 15.49(7) . . ? C92 Cl3 Cl4 111.4(12) . . ? C92 Cl3 C91 67(3) . . ? Cl4 Cl3 C91 76.962(1) . . ? C92 Cl3 Cl2 76.9(15) . . ? Cl4 Cl3 Cl2 118.947(1) . . ? C91 Cl3 Cl2 49.672(1) . . ? C92 Cl3 Cl5 128(2) . . ? Cl4 Cl3 Cl5 20.4(10) . . ? C91 Cl3 Cl5 77.6(8) . . ? Cl2 Cl3 Cl5 108.1(8) . . ? Cl3 Cl4 C92 23.3(4) . . ? Cl3 Cl4 Cl5 145.4(16) . . ? C92 Cl4 Cl5 161.3(17) . . ? Cl3 Cl4 C91 70.320(1) . . ? C92 Cl4 C91 59.9(11) . . ? Cl5 Cl4 C91 105.8(13) . . ? Cl4 Cl5 Cl3 14.2(7) . . ? Cl7 Cl6 C94 57.6(3) . . ? Cl7 Cl6 Cl8 10.1(4) . . ? C94 Cl6 Cl8 47.7(2) . . ? Cl8 Cl7 Cl6 158.4(7) . . ? Cl8 Cl7 C94 73.0(7) . . ? Cl6 Cl7 C94 85.70(6) . . ? Cl8 Cl7 Cl11 28.3(6) . . ? Cl6 Cl7 Cl11 130.5(3) . . ? C94 Cl7 Cl11 47.8(2) . . ? Cl8 Cl7 C93 47.1(6) . . ? Cl6 Cl7 C93 113.04(15) . . ? C94 Cl7 C93 29.44(17) . . ? Cl11 Cl7 C93 30.22(12) . . ? C93 Cl9 Cl11 25.548(1) . . ? C93 Cl10 Cl11 25.6 . . ? C93 Cl11 Cl8 94.2(4) . . ? C93 Cl11 C94 48.634(1) . . ? Cl8 Cl11 C94 73.7(5) . . ? C93 Cl11 Cl7 86.37(19) . . ? Cl8 Cl11 Cl7 23.1(4) . . ? C94 Cl11 Cl7 53.33(6) . . ? C93 Cl11 Cl9 36.913(1) . . ? Cl8 Cl11 Cl9 109.6(4) . . ? C94 Cl11 Cl9 85.539(1) . . ? Cl7 Cl11 Cl9 113.8(2) . . ? C93 Cl11 Cl10 38.852(1) . . ? Cl8 Cl11 Cl10 98.8(4) . . ? C94 Cl11 Cl10 86.262(1) . . ? Cl7 Cl11 Cl10 105.6(3) . . ? Cl9 Cl11 Cl10 11.7 . . ? O5 S1 O6 114.7(3) . . ? O5 S1 O4 116.1(3) . . ? O6 S1 O4 113.3(3) . . ? O5 S1 C42 104.2(3) . . ? O6 S1 C42 105.5(2) . . ? O4 S1 C42 100.8(2) . . ? O11 S2 O12 115.7(2) . . ? O11 S2 O10 114.8(2) . . ? O12 S2 O10 113.5(2) . . ? O11 S2 C40 105.1(2) . . ? O12 S2 C40 103.8(2) . . ? O10 S2 C40 101.8(2) . . ? O14 S3 O13 112.7(4) . . ? O14 S3 O15 119.4(4) . . ? O13 S3 O15 111.7(3) . . ? O14 S3 C41 105.3(4) . . ? O13 S3 C41 103.3(4) . . ? O15 S3 C41 102.3(3) . . ? O17 S4 O16 115.6(2) . . ? O17 S4 O18 114.7(3) . . ? O16 S4 O18 113.8(2) . . ? O17 S4 C43 104.3(3) . . ? O16 S4 C43 103.3(3) . . ? O18 S4 C43 103.0(3) . . ? C10A P1 C2 115.6(12) . . ? C10A P1 C6A 86.1(8) . . ? C2 P1 C6A 107.6(10) . . ? C10A P1 C10 18.5(6) . . ? C2 P1 C10 100.1(11) . . ? C6A P1 C10 100.8(7) . . ? C10A P1 C6 102.6(8) . . ? C2 P1 C6 95.3(9) . . ? C6A P1 C6 17.4(5) . . ? C10 P1 C6 115.7(7) . . ? C10A P1 C2A 112.6(11) . . ? C2 P1 C2A 12.3(12) . . ? C6A P1 C2A 119.8(9) . . ? C10 P1 C2A 95.4(10) . . ? C6 P1 C2A 107.5(9) . . ? C10A P1 Ru1 104.8(6) . . ? C2 P1 Ru1 120.4(10) . . ? C6A P1 Ru1 117.5(7) . . ? C10 P1 Ru1 107.0(5) . . ? C6 P1 Ru1 117.2(6) . . ? C2A P1 Ru1 111.9(9) . . ? C11A P2 C11 18.9(5) . . ? C11A P2 C16A 120.0(10) . . ? C11 P2 C16A 103.3(9) . . ? C11A P2 C16 107.4(8) . . ? C11 P2 C16 89.5(7) . . ? C16A P2 C16 16.3(10) . . ? C11A P2 C12A 105.2(7) . . ? C11 P2 C12A 117.1(7) . . ? C16A P2 C12A 92.6(11) . . ? C16 P2 C12A 106.8(9) . . ? C11A P2 C12 87.6(7) . . ? C11 P2 C12 101.8(7) . . ? C16A P2 C12 108.1(12) . . ? C16 P2 C12 120.1(10) . . ? C12A P2 C12 19.0(4) . . ? C11A P2 Ru1 103.9(6) . . ? C11 P2 Ru1 108.0(4) . . ? C16A P2 Ru1 118.1(12) . . ? C16 P2 Ru1 116.0(10) . . ? C12A P2 Ru1 116.6(5) . . ? C12 P2 Ru1 115.5(5) . . ? C30 P3 C26 106.0(3) . . ? C30 P3 C22 101.6(3) . . ? C26 P3 C22 108.3(3) . . ? C30 P3 Ru2 107.10(17) . . ? C26 P3 Ru2 114.35(19) . . ? C22 P3 Ru2 118.06(19) . . ? C31 P4 C36 104.4(3) . . ? C31 P4 C32 104.5(3) . . ? C36 P4 C32 110.4(3) . . ? C31 P4 Ru2 107.13(16) . . ? C36 P4 Ru2 113.07(18) . . ? C32 P4 Ru2 116.30(17) . . ? S1 O4 Ru1 131.7(2) . . ? S2 O10 Ru2 128.73(18) . . ? O1 C1 Ru1 168.8(5) . . ? C4A C2A C5A 113.2(18) . . ? C4A C2A C3A 114(3) . . ? C5A C2A C3A 105(3) . . ? C4A C2A P1 109.2(18) . . ? C5A C2A P1 101.5(14) . . ? C3A C2A P1 114(2) . . ? C7 C6 C9 107.2(16) . . ? C7 C6 C8 107.7(14) . . ? C9 C6 C8 109.1(15) . . ? C7 C6 P1 111.4(11) . . ? C9 C6 P1 108.7(14) . . ? C8 C6 P1 112.6(12) . . ? C11 C10 P1 113.6(10) . . ? C10 C11 P2 115.6(10) . . ? C15A C12A C13A 108.4(16) . . ? C15A C12A C14A 108.4(13) . . ? C13A C12A C14A 106(2) . . ? C15A C12A P2 113.8(10) . . ? C13A C12A P2 111.1(14) . . ? C14A C12A P2 109.1(9) . . ? C17 C16 C18 105(2) . . ? C17 C16 C19 107(2) . . ? C18 C16 C19 110(2) . . ? C17 C16 P2 114(2) . . ? C18 C16 P2 108.7(13) . . ? C19 C16 P2 111.8(14) . . ? O7 C21 Ru2 170.3(4) . . ? C24 C22 C25 108.0(6) . . ? C24 C22 C23 110.2(5) . . ? C25 C22 C23 105.5(5) . . ? C24 C22 P3 109.8(4) . . ? C25 C22 P3 110.4(4) . . ? C23 C22 P3 112.6(5) . . ? C29 C26 C27 110.4(5) . . ? C29 C26 C28 105.9(5) . . ? C27 C26 C28 108.3(4) . . ? C29 C26 P3 107.4(4) . . ? C27 C26 P3 110.8(4) . . ? C28 C26 P3 114.0(4) . . ? C31 C30 P3 113.2(3) . . ? C30 C31 P4 114.0(4) . . ? C34 C32 C35 108.9(5) . . ? C34 C32 C33 109.4(6) . . ? C35 C32 C33 105.1(5) . . ? C34 C32 P4 109.8(4) . . ? C35 C32 P4 113.0(4) . . ? C33 C32 P4 110.5(4) . . ? C38 C36 C37 110.2(5) . . ? C38 C36 C39 108.8(5) . . ? C37 C36 C39 105.0(5) . . ? C38 C36 P4 109.4(4) . . ? C37 C36 P4 107.3(4) . . ? C39 C36 P4 116.0(5) . . ? F5 C40 F6 108.5(4) . . ? F5 C40 F4 108.6(5) . . ? F6 C40 F4 107.4(4) . . ? F5 C40 S2 112.0(3) . . ? F6 C40 S2 109.8(3) . . ? F4 C40 S2 110.4(4) . . ? F8 C41 F9 108.1(7) . . ? F8 C41 F7 108.2(8) . . ? F9 C41 F7 106.7(7) . . ? F8 C41 S3 112.3(6) . . ? F9 C41 S3 110.7(7) . . ? F7 C41 S3 110.7(5) . . ? F2 C42 F3 109.7(5) . . ? F2 C42 F1 107.3(5) . . ? F3 C42 F1 107.2(5) . . ? F2 C42 S1 112.4(4) . . ? F3 C42 S1 109.9(4) . . ? F1 C42 S1 110.2(4) . . ? F12 C43 F10 107.7(6) . . ? F12 C43 F11 110.0(7) . . ? F10 C43 F11 106.7(6) . . ? F12 C43 S4 111.1(5) . . ? F10 C43 S4 110.8(6) . . ? F11 C43 S4 110.4(5) . . ? C92 C91 Cl2 77.21(5) . . ? C92 C91 Cl3 18.526(2) . . ? Cl2 C91 Cl3 75.875(1) . . ? C92 C91 Cl4 44.64(3) . . ? Cl2 C91 Cl4 103.845(1) . . ? Cl3 C91 Cl4 32.718(1) . . ? C92 C91 Cl1 98.58(5) . . ? Cl2 C91 Cl1 24.0 . . ? Cl3 C91 Cl1 99.614(1) . . ? Cl4 C91 Cl1 127.519(1) . . ? Cl3 C92 Cl4 45.4(8) . . ? Cl3 C92 C91 94(3) . . ? Cl4 C92 C91 75.4(11) . . ? Cl3 C92 Cl2 87.6(15) . . ? Cl4 C92 Cl2 106.6(11) . . ? C91 C92 Cl2 51.9(5) . . ? Cl11 C93 C94 83.541(1) . . ? Cl11 C93 Cl9 117.538(1) . . ? C94 C93 Cl9 158.9 . . ? Cl11 C93 Cl10 115.571(1) . . ? C94 C93 Cl10 154.7 . . ? Cl9 C93 Cl10 16.9 . . ? Cl11 C93 Cl8 44.9(3) . . ? C94 C93 Cl8 67.2(3) . . ? Cl9 C93 Cl8 128.1(3) . . ? Cl10 C93 Cl8 113.8(3) . . ? Cl11 C93 Cl7 63.4(2) . . ? C94 C93 Cl7 44.83(14) . . ? Cl9 C93 Cl7 144.0(2) . . ? Cl10 C93 Cl7 127.1(2) . . ? Cl8 C93 Cl7 25.4(3) . . ? C93 C94 Cl11 47.825(1) . . ? C93 C94 Cl7 105.7(3) . . ? Cl11 C94 Cl7 78.9(3) . . ? C93 C94 Cl8 73.3(3) . . ? Cl11 C94 Cl8 44.8(4) . . ? Cl7 C94 Cl8 35.7(4) . . ? C93 C94 Cl6 138.825(1) . . ? Cl11 C94 Cl6 113.620(1) . . ? Cl7 C94 Cl6 36.7(3) . . ? Cl8 C94 Cl6 72.3(4) . . ? C3 C2 C4 104(2) . . ? C3 C2 C5 104(2) . . ? C4 C2 C5 103(2) . . ? C3 C2 P1 119(2) . . ? C4 C2 P1 112.8(16) . . ? C5 C2 P1 113.0(18) . . ? C7A C6A C8A 112.9(16) . . ? C7A C6A C9A 104(2) . . ? C8A C6A C9A 106.5(19) . . ? C7A C6A P1 108.9(11) . . ? C8A C6A P1 108.4(12) . . ? C9A C6A P1 116(2) . . ? C11A C10A P1 112.2(14) . . ? C10A C11A P2 112.4(13) . . ? C14 C12 C15 107.6(13) . . ? C14 C12 C13 112.8(16) . . ? C15 C12 C13 102.6(15) . . ? C14 C12 P2 111.4(10) . . ? C15 C12 P2 108.3(8) . . ? C13 C12 P2 113.4(17) . . ? C19A C16A C17A 113(3) . . ? C19A C16A C18A 109(2) . . ? C17A C16A C18A 105(2) . . ? C19A C16A P2 111.2(19) . . ? C17A C16A P2 110(2) . . ? C18A C16A P2 108(2) . . ? Cl7 Cl8 Cl11 128.6(9) . . ? Cl7 Cl8 C94 71.4(6) . . ? Cl11 Cl8 C94 61.4(4) . . ? Cl7 Cl8 C93 107.5(7) . . ? Cl11 Cl8 C93 40.9(3) . . ? C94 Cl8 C93 39.6(2) . . ? Cl7 Cl8 Cl6 11.6(4) . . ? Cl11 Cl8 Cl6 117.3(6) . . ? C94 Cl8 Cl6 60.0(3) . . ? C93 Cl8 Cl6 97.1(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.895 _refine_diff_density_min -1.223 _refine_diff_density_rms 0.113 data_c:\word_f~1\papers\inorga~1\mkw\august~1\k03mkw13\k03mkw13 _database_code_depnum_ccdc_archive 'CCDC 250931' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H58 F6 O10 P2 Ru S5' _chemical_formula_weight 980.04 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' P P 0.1023 0.0942 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 13.5939(1) _cell_length_b 18.9779(2) _cell_length_c 16.2799(1) _cell_angle_alpha 90.00 _cell_angle_beta 94.311(1) _cell_angle_gamma 90.00 _cell_volume 4188.07(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.774 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 98870 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 33.16 _reflns_number_total 15909 _reflns_number_gt 12818 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0362P)^2^+2.5804P] 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 15909 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.730342(8) 0.129643(6) 0.289414(7) 0.01435(3) Uani 1 1 d . . . S1 S 0.50492(3) 0.15407(2) 0.33407(2) 0.01995(7) Uani 1 1 d . . . S2 S 0.66814(3) 0.29766(2) 0.23747(2) 0.02094(7) Uani 1 1 d . . . S3 S 0.59179(3) 0.10386(2) 0.12115(2) 0.02021(7) Uani 1 1 d . . . S4 S 0.76327(3) 0.49375(2) 0.24820(3) 0.02741(8) Uani 1 1 d . . . S5 S 0.62481(4) 0.70024(3) 0.52717(4) 0.03880(11) Uani 1 1 d . . . P1 P 0.79291(3) 0.02233(2) 0.34866(2) 0.01744(7) Uani 1 1 d . . . P2 P 0.89771(3) 0.15428(2) 0.26244(2) 0.01788(7) Uani 1 1 d . . . F1 F 0.77174(10) 0.40749(6) 0.37510(7) 0.0388(3) Uani 1 1 d . . . F2 F 0.75601(17) 0.51653(8) 0.40524(9) 0.0737(5) Uani 1 1 d . . . F3 F 0.89482(12) 0.47588(11) 0.37149(11) 0.0814(6) Uani 1 1 d . . . F4 F 0.80529(10) 0.65304(9) 0.53033(9) 0.0509(3) Uani 1 1 d . . . F5 F 0.79042(14) 0.76155(9) 0.49773(11) 0.0718(5) Uani 1 1 d . . . F6 F 0.74350(12) 0.68171(10) 0.40985(8) 0.0622(4) Uani 1 1 d . . . O1 O 0.57776(8) 0.09875(6) 0.30406(7) 0.0198(2) Uani 1 1 d . . . O2 O 0.65310(8) 0.21779(6) 0.23041(7) 0.0214(2) Uani 1 1 d . . . O3 O 0.68994(8) 0.08689(6) 0.17068(7) 0.0203(2) Uani 1 1 d . . . O4 O 0.72707(9) 0.21009(7) 0.44467(7) 0.0272(2) Uani 1 1 d . . . O5 O 0.81565(17) 0.44303(10) 0.20348(10) 0.0621(6) Uani 1 1 d . . . O6 O 0.79230(10) 0.56566(8) 0.23976(10) 0.0365(3) Uani 1 1 d . . . O7 O 0.65771(12) 0.48239(9) 0.24299(12) 0.0502(4) Uani 1 1 d . . . O8 O 0.57057(16) 0.74764(13) 0.47167(13) 0.0743(7) Uani 1 1 d . . . O9 O 0.59624(15) 0.62706(11) 0.51979(16) 0.0693(6) Uani 1 1 d . . . O10 O 0.64189(14) 0.72468(10) 0.61047(10) 0.0525(4) Uani 1 1 d . . . C1 C 0.73833(10) 0.17619(8) 0.38726(9) 0.0188(3) Uani 1 1 d . . . C2 C 0.43318(13) 0.10469(11) 0.40103(12) 0.0300(4) Uani 1 1 d . . . H2A H 0.4110 0.0609 0.3737 0.045 Uiso 1 1 calc R . . H2B H 0.3757 0.1325 0.4143 0.045 Uiso 1 1 calc R . . H2C H 0.4734 0.0936 0.4519 0.045 Uiso 1 1 calc R . . C3 C 0.41310(12) 0.16564(10) 0.25044(11) 0.0270(3) Uani 1 1 d . . . H3A H 0.4425 0.1893 0.2047 0.041 Uiso 1 1 calc R . . H3B H 0.3590 0.1944 0.2687 0.041 Uiso 1 1 calc R . . H3C H 0.3876 0.1195 0.2321 0.041 Uiso 1 1 calc R . . C4 C 0.61650(17) 0.32791(10) 0.14016(11) 0.0350(4) Uani 1 1 d . . . H4A H 0.6607 0.3158 0.0975 0.053 Uiso 1 1 calc R . . H4B H 0.6081 0.3792 0.1419 0.053 Uiso 1 1 calc R . . H4C H 0.5522 0.3055 0.1275 0.053 Uiso 1 1 calc R . . C5 C 0.57534(14) 0.32843(10) 0.30090(12) 0.0306(4) Uani 1 1 d . . . H5A H 0.5108 0.3106 0.2795 0.046 Uiso 1 1 calc R . . H5B H 0.5744 0.3801 0.3006 0.046 Uiso 1 1 calc R . . H5C H 0.5899 0.3115 0.3574 0.046 Uiso 1 1 calc R . . C6 C 0.52060(14) 0.02492(10) 0.11976(13) 0.0327(4) Uani 1 1 d . . . H6A H 0.5597 -0.0142 0.1002 0.049 Uiso 1 1 calc R . . H6B H 0.4609 0.0310 0.0828 0.049 Uiso 1 1 calc R . . H6C H 0.5021 0.0146 0.1755 0.049 Uiso 1 1 calc R . . C7 C 0.62805(14) 0.10033(15) 0.01827(11) 0.0409(5) Uani 1 1 d . . . H7A H 0.6674 0.1421 0.0074 0.061 Uiso 1 1 calc R . . H7B H 0.5692 0.0991 -0.0203 0.061 Uiso 1 1 calc R . . H7C H 0.6675 0.0578 0.0112 0.061 Uiso 1 1 calc R . . C8 C 0.74225(13) -0.06486(9) 0.30575(11) 0.0260(3) Uani 1 1 d . . . C9 C 0.74352(18) -0.06444(10) 0.21137(12) 0.0378(4) Uani 1 1 d . . . H9A H 0.8119 -0.0627 0.1962 0.057 Uiso 1 1 calc R . . H9B H 0.7077 -0.0230 0.1890 0.057 Uiso 1 1 calc R . . H9C H 0.7118 -0.1073 0.1888 0.057 Uiso 1 1 calc R . . C10 C 0.63601(15) -0.07507(11) 0.32875(16) 0.0404(5) Uani 1 1 d . . . H10A H 0.6065 -0.1154 0.2984 0.061 Uiso 1 1 calc R . . H10B H 0.5976 -0.0325 0.3145 0.061 Uiso 1 1 calc R . . H10C H 0.6359 -0.0839 0.3881 0.061 Uiso 1 1 calc R . . C11 C 0.80468(16) -0.12943(10) 0.33402(13) 0.0350(4) Uani 1 1 d . . . H11A H 0.7830 -0.1706 0.3011 0.053 Uiso 1 1 calc R . . H11B H 0.7964 -0.1388 0.3923 0.053 Uiso 1 1 calc R . . H11C H 0.8743 -0.1200 0.3267 0.053 Uiso 1 1 calc R . . C12 C 0.79270(11) 0.01971(9) 0.46534(9) 0.0216(3) Uani 1 1 d . . . C13 C 0.87004(12) 0.07262(10) 0.50184(10) 0.0267(3) Uani 1 1 d . . . H13A H 0.8628 0.0782 0.5609 0.040 Uiso 1 1 calc R . . H13B H 0.8601 0.1183 0.4743 0.040 Uiso 1 1 calc R . . H13C H 0.9364 0.0551 0.4935 0.040 Uiso 1 1 calc R . . C14 C 0.69005(12) 0.03946(9) 0.49225(10) 0.0248(3) Uani 1 1 d . . . H14A H 0.6415 0.0048 0.4703 0.037 Uiso 1 1 calc R . . H14B H 0.6717 0.0863 0.4710 0.037 Uiso 1 1 calc R . . H14C H 0.6917 0.0398 0.5525 0.037 Uiso 1 1 calc R . . C15 C 0.82039(14) -0.05194(10) 0.50465(11) 0.0300(4) Uani 1 1 d . . . H15A H 0.8822 -0.0686 0.4842 0.045 Uiso 1 1 calc R . . H15B H 0.7678 -0.0861 0.4902 0.045 Uiso 1 1 calc R . . H15C H 0.8287 -0.0468 0.5647 0.045 Uiso 1 1 calc R . . C16 C 0.92376(11) 0.01577(9) 0.32750(10) 0.0236(3) Uani 1 1 d . . . H16A H 0.9596 -0.0106 0.3729 0.028 Uiso 1 1 calc R . . H16B H 0.9288 -0.0116 0.2762 0.028 Uiso 1 1 calc R . . C17 C 0.97389(11) 0.08680(9) 0.31838(10) 0.0231(3) Uani 1 1 d . . . H17A H 1.0345 0.0795 0.2893 0.028 Uiso 1 1 calc R . . H17B H 0.9943 0.1051 0.3740 0.028 Uiso 1 1 calc R . . C18 C 0.92089(12) 0.14473(10) 0.14972(10) 0.0250(3) Uani 1 1 d . . . C19 C 0.84959(12) 0.19262(11) 0.09774(11) 0.0295(4) Uani 1 1 d . . . H19A H 0.8714 0.2417 0.1038 0.044 Uiso 1 1 calc R . . H19B H 0.7831 0.1879 0.1165 0.044 Uiso 1 1 calc R . . H19C H 0.8488 0.1788 0.0397 0.044 Uiso 1 1 calc R . . C20 C 1.02733(13) 0.16090(12) 0.12894(11) 0.0323(4) Uani 1 1 d . . . H20A H 1.0348 0.1493 0.0711 0.048 Uiso 1 1 calc R . . H20B H 1.0736 0.1326 0.1643 0.048 Uiso 1 1 calc R . . H20C H 1.0413 0.2111 0.1382 0.048 Uiso 1 1 calc R . . C21 C 0.90168(13) 0.06718(10) 0.12555(11) 0.0290(3) Uani 1 1 d . . . H21A H 0.8354 0.0536 0.1395 0.043 Uiso 1 1 calc R . . H21B H 0.9507 0.0371 0.1556 0.043 Uiso 1 1 calc R . . H21C H 0.9067 0.0615 0.0662 0.043 Uiso 1 1 calc R . . C22 C 0.96457(11) 0.23765(10) 0.30186(11) 0.0262(3) Uani 1 1 d . . . C23 C 0.93043(15) 0.25806(11) 0.38643(13) 0.0357(4) Uani 1 1 d . . . H23A H 0.9352 0.2170 0.4230 0.054 Uiso 1 1 calc R . . H23B H 0.8618 0.2743 0.3800 0.054 Uiso 1 1 calc R . . H23C H 0.9725 0.2960 0.4102 0.054 Uiso 1 1 calc R . . C24 C 1.07751(12) 0.22622(11) 0.31322(12) 0.0323(4) Uani 1 1 d . . . H24A H 1.1102 0.2714 0.3259 0.048 Uiso 1 1 calc R . . H24B H 1.1009 0.2069 0.2624 0.048 Uiso 1 1 calc R . . H24C H 1.0929 0.1932 0.3586 0.048 Uiso 1 1 calc R . . C25 C 0.94272(13) 0.30079(10) 0.24450(14) 0.0340(4) Uani 1 1 d . . . H25A H 0.9692 0.3438 0.2711 0.051 Uiso 1 1 calc R . . H25B H 0.8712 0.3056 0.2329 0.051 Uiso 1 1 calc R . . H25C H 0.9738 0.2933 0.1928 0.051 Uiso 1 1 calc R . . C26 C 0.79869(15) 0.47292(11) 0.35540(12) 0.0346(4) Uani 1 1 d . . . C27 C 0.74688(15) 0.69878(12) 0.48912(12) 0.0358(4) 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 0.01380(5) 0.01760(5) 0.01179(5) 0.00041(4) 0.00180(3) 0.00040(4) S1 0.01636(15) 0.02297(17) 0.02115(17) -0.00036(14) 0.00565(12) -0.00074(12) S2 0.02014(16) 0.02034(17) 0.02237(17) -0.00042(14) 0.00180(13) -0.00218(13) S3 0.01823(15) 0.02709(18) 0.01517(15) -0.00236(14) 0.00023(12) 0.00001(13) S4 0.0316(2) 0.02495(19) 0.0261(2) 0.00072(16) 0.00484(16) 0.00188(15) S5 0.0296(2) 0.0445(3) 0.0423(3) -0.0067(2) 0.00234(19) 0.0068(2) P1 0.01758(16) 0.01960(17) 0.01534(16) 0.00205(13) 0.00259(12) 0.00195(13) P2 0.01429(15) 0.02380(18) 0.01580(16) 0.00307(14) 0.00281(12) 0.00008(13) F1 0.0522(7) 0.0357(6) 0.0288(6) 0.0048(5) 0.0060(5) -0.0081(5) F2 0.1417(17) 0.0455(9) 0.0376(8) -0.0132(7) 0.0326(9) -0.0084(10) F3 0.0489(8) 0.1149(16) 0.0753(11) 0.0505(11) -0.0284(8) -0.0406(9) F4 0.0359(6) 0.0677(9) 0.0490(8) 0.0073(7) 0.0034(6) 0.0157(6) F5 0.0833(12) 0.0690(11) 0.0609(10) 0.0218(8) -0.0085(8) -0.0455(9) F6 0.0582(9) 0.1015(13) 0.0275(6) -0.0085(8) 0.0079(6) 0.0049(9) O1 0.0164(4) 0.0218(5) 0.0219(5) -0.0010(4) 0.0047(4) -0.0002(4) O2 0.0229(5) 0.0192(5) 0.0220(5) 0.0017(4) 0.0001(4) 0.0016(4) O3 0.0181(5) 0.0267(5) 0.0161(5) -0.0032(4) 0.0005(4) 0.0017(4) O4 0.0305(6) 0.0308(6) 0.0208(5) -0.0068(5) 0.0046(5) -0.0024(5) O5 0.1080(16) 0.0503(10) 0.0315(8) 0.0084(7) 0.0274(9) 0.0391(10) O6 0.0325(7) 0.0325(7) 0.0450(8) 0.0073(6) 0.0059(6) -0.0060(5) O7 0.0375(8) 0.0418(9) 0.0690(12) 0.0151(8) -0.0105(7) -0.0127(7) O8 0.0670(12) 0.0892(16) 0.0630(13) -0.0052(11) -0.0197(10) 0.0429(12) O9 0.0513(11) 0.0613(12) 0.0968(17) -0.0162(11) 0.0167(11) -0.0277(9) O10 0.0643(11) 0.0575(11) 0.0371(8) -0.0076(8) 0.0127(8) 0.0186(9) C1 0.0178(6) 0.0221(7) 0.0165(6) 0.0011(5) 0.0020(5) -0.0012(5) C2 0.0250(8) 0.0364(9) 0.0302(9) 0.0058(7) 0.0120(6) -0.0024(7) C3 0.0203(7) 0.0321(9) 0.0284(8) 0.0023(7) 0.0002(6) 0.0027(6) C4 0.0532(12) 0.0276(9) 0.0240(8) 0.0082(7) 0.0012(8) 0.0024(8) C5 0.0337(9) 0.0254(8) 0.0338(9) -0.0017(7) 0.0108(7) 0.0023(7) C6 0.0291(8) 0.0335(9) 0.0348(10) -0.0040(8) -0.0031(7) -0.0085(7) C7 0.0298(9) 0.0783(16) 0.0148(7) -0.0030(9) 0.0021(6) -0.0102(9) C8 0.0307(8) 0.0195(7) 0.0278(8) -0.0009(6) 0.0026(6) 0.0009(6) C9 0.0594(13) 0.0238(8) 0.0291(9) -0.0059(7) -0.0054(9) 0.0009(8) C10 0.0317(9) 0.0305(10) 0.0596(14) -0.0108(9) 0.0066(9) -0.0085(7) C11 0.0472(11) 0.0218(8) 0.0367(10) 0.0020(7) 0.0073(8) 0.0081(7) C12 0.0228(7) 0.0268(8) 0.0155(6) 0.0044(6) 0.0029(5) 0.0019(6) C13 0.0258(7) 0.0364(9) 0.0176(7) 0.0033(6) -0.0008(6) -0.0006(6) C14 0.0246(7) 0.0300(8) 0.0206(7) 0.0033(6) 0.0070(6) 0.0005(6) C15 0.0335(9) 0.0330(9) 0.0239(8) 0.0111(7) 0.0044(7) 0.0054(7) C16 0.0208(7) 0.0277(8) 0.0228(7) 0.0064(6) 0.0055(5) 0.0065(6) C17 0.0163(6) 0.0319(8) 0.0211(7) 0.0057(6) 0.0022(5) 0.0029(6) C18 0.0199(7) 0.0388(9) 0.0169(7) 0.0056(6) 0.0053(5) 0.0016(6) C19 0.0233(7) 0.0426(10) 0.0226(8) 0.0109(7) 0.0017(6) 0.0002(7) C20 0.0213(7) 0.0520(12) 0.0248(8) 0.0071(8) 0.0094(6) -0.0001(7) C21 0.0265(8) 0.0395(10) 0.0219(8) -0.0015(7) 0.0082(6) 0.0044(7) C22 0.0179(6) 0.0294(8) 0.0316(8) 0.0004(7) 0.0037(6) -0.0054(6) C23 0.0343(9) 0.0364(10) 0.0374(10) -0.0104(8) 0.0085(8) -0.0124(8) C24 0.0189(7) 0.0416(10) 0.0358(10) 0.0026(8) -0.0015(6) -0.0066(7) C25 0.0238(8) 0.0290(9) 0.0495(11) 0.0086(8) 0.0058(7) -0.0039(7) C26 0.0391(10) 0.0380(10) 0.0271(9) 0.0000(8) 0.0047(7) -0.0134(8) C27 0.0352(9) 0.0454(11) 0.0267(9) 0.0030(8) 0.0017(7) -0.0061(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.8176(15) . ? Ru1 O3 2.1300(11) . ? Ru1 O2 2.1615(11) . ? Ru1 O1 2.1857(10) . ? Ru1 P1 2.3828(4) . ? Ru1 P2 2.3955(4) . ? S1 O1 1.5474(11) . ? S1 C2 1.7824(17) . ? S1 C3 1.7901(17) . ? S2 O2 1.5325(12) . ? S2 C4 1.7791(19) . ? S2 C5 1.7873(18) . ? S3 O3 1.5402(11) . ? S3 C7 1.7824(18) . ? S3 C6 1.7826(18) . ? S4 O5 1.4289(16) . ? S4 O6 1.4300(14) . ? S4 O7 1.4473(16) . ? S4 C26 1.819(2) . ? S5 O10 1.4355(17) . ? S5 O8 1.4384(19) . ? S5 O9 1.445(2) . ? S5 C27 1.815(2) . ? P1 C16 1.8412(16) . ? P1 C12 1.9003(16) . ? P1 C8 1.9048(17) . ? P2 C17 1.8438(16) . ? P2 C18 1.8939(16) . ? P2 C22 1.9115(18) . ? F1 C26 1.340(2) . ? F2 C26 1.323(3) . ? F3 C26 1.315(2) . ? F4 C27 1.324(2) . ? F5 C27 1.333(3) . ? F6 C27 1.328(2) . ? O4 C1 1.1542(19) . ? C8 C10 1.531(3) . ? C8 C9 1.538(3) . ? C8 C11 1.541(2) . ? C12 C15 1.537(2) . ? C12 C14 1.540(2) . ? C12 C13 1.540(2) . ? C16 C17 1.523(2) . ? C18 C19 1.536(2) . ? C18 C21 1.541(3) . ? C18 C20 1.541(2) . ? C22 C25 1.534(3) . ? C22 C23 1.535(3) . ? C22 C24 1.548(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 O3 167.12(5) . . ? C1 Ru1 O2 90.48(6) . . ? O3 Ru1 O2 78.93(4) . . ? C1 Ru1 O1 91.69(5) . . ? O3 Ru1 O1 79.32(4) . . ? O2 Ru1 O1 79.79(4) . . ? C1 Ru1 P1 93.71(5) . . ? O3 Ru1 P1 95.83(3) . . ? O2 Ru1 P1 171.13(3) . . ? O1 Ru1 P1 92.26(3) . . ? C1 Ru1 P2 94.06(5) . . ? O3 Ru1 P2 95.26(3) . . ? O2 Ru1 P2 101.76(3) . . ? O1 Ru1 P2 174.03(3) . . ? P1 Ru1 P2 85.752(14) . . ? O1 S1 C2 103.23(8) . . ? O1 S1 C3 105.61(7) . . ? C2 S1 C3 98.47(9) . . ? O2 S2 C4 102.17(8) . . ? O2 S2 C5 105.69(8) . . ? C4 S2 C5 99.24(10) . . ? O3 S3 C7 101.20(8) . . ? O3 S3 C6 106.21(8) . . ? C7 S3 C6 98.32(11) . . ? O5 S4 O6 116.25(11) . . ? O5 S4 O7 113.55(13) . . ? O6 S4 O7 114.59(9) . . ? O5 S4 C26 103.67(10) . . ? O6 S4 C26 104.16(9) . . ? O7 S4 C26 102.34(10) . . ? O10 S5 O8 115.49(12) . . ? O10 S5 O9 114.36(13) . . ? O8 S5 O9 115.28(15) . . ? O10 S5 C27 103.91(10) . . ? O8 S5 C27 103.53(12) . . ? O9 S5 C27 101.76(11) . . ? C16 P1 C12 105.03(7) . . ? C16 P1 C8 101.55(8) . . ? C12 P1 C8 108.43(8) . . ? C16 P1 Ru1 107.61(5) . . ? C12 P1 Ru1 113.56(5) . . ? C8 P1 Ru1 119.07(6) . . ? C17 P2 C18 106.50(8) . . ? C17 P2 C22 100.02(8) . . ? C18 P2 C22 107.16(8) . . ? C17 P2 Ru1 106.25(5) . . ? C18 P2 Ru1 112.86(5) . . ? C22 P2 Ru1 122.29(5) . . ? S1 O1 Ru1 119.17(6) . . ? S2 O2 Ru1 132.41(7) . . ? S3 O3 Ru1 123.34(6) . . ? O4 C1 Ru1 167.88(13) . . ? C10 C8 C9 109.05(17) . . ? C10 C8 C11 109.56(16) . . ? C9 C8 C11 104.79(15) . . ? C10 C8 P1 109.99(12) . . ? C9 C8 P1 109.33(12) . . ? C11 C8 P1 113.92(13) . . ? C15 C12 C14 107.19(13) . . ? C15 C12 C13 106.10(14) . . ? C14 C12 C13 109.77(14) . . ? C15 C12 P1 114.87(12) . . ? C14 C12 P1 110.33(11) . . ? C13 C12 P1 108.44(11) . . ? C17 C16 P1 113.83(11) . . ? C16 C17 P2 115.10(11) . . ? C19 C18 C21 109.68(14) . . ? C19 C18 C20 108.98(14) . . ? C21 C18 C20 106.14(15) . . ? C19 C18 P2 109.47(12) . . ? C21 C18 P2 107.54(11) . . ? C20 C18 P2 114.89(12) . . ? C25 C22 C23 106.92(16) . . ? C25 C22 C24 109.09(14) . . ? C23 C22 C24 106.99(15) . . ? C25 C22 P2 112.13(13) . . ? C23 C22 P2 109.98(11) . . ? C24 C22 P2 111.50(13) . . ? F3 C26 F2 109.0(2) . . ? F3 C26 F1 106.11(19) . . ? F2 C26 F1 107.01(16) . . ? F3 C26 S4 111.68(14) . . ? F2 C26 S4 110.83(16) . . ? F1 C26 S4 111.94(13) . . ? F4 C27 F6 107.94(19) . . ? F4 C27 F5 106.73(17) . . ? F6 C27 F5 107.63(18) . . ? F4 C27 S5 111.47(14) . . ? F6 C27 S5 111.70(14) . . ? F5 C27 S5 111.14(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 33.16 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.801 _refine_diff_density_min -1.014 _refine_diff_density_rms 0.097 data_c:\word_f~1\papers\inorga~1\mkw\august~1\h03mkw~2\h03mkw4 _database_code_depnum_ccdc_archive 'CCDC 250932' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H43 F3 O7 P2 Ru S' _chemical_formula_weight 671.63 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.8970(2) _cell_length_b 10.4600(1) _cell_length_c 18.5370(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.029(1) _cell_angle_gamma 90.00 _cell_volume 2990.44(7) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8950 _exptl_absorpt_correction_T_max 0.8950 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46121 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6839 _reflns_number_gt 5322 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+1.7093*P+(0.0345P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6839 _refine_ls_number_parameters 350 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.621568(12) 0.233759(18) 0.962927(10) 0.02460(8) Uani 1 1 d D . . S1 S 0.99555(5) 0.65656(7) 1.14117(4) 0.04393(19) Uani 1 1 d . . . P2 P 0.68235(4) 0.39992(5) 0.89774(3) 0.02340(14) Uani 1 1 d . . . P3 P 0.76939(4) 0.21045(6) 1.03978(3) 0.02377(14) Uani 1 1 d . . . F1 F 0.90134(14) 0.80827(18) 1.20229(12) 0.0708(6) Uani 1 1 d . . . F2 F 0.85049(16) 0.6235(3) 1.17936(18) 0.1174(11) Uani 1 1 d . . . F3 F 0.95674(18) 0.6552(3) 1.26936(12) 0.1077(10) Uani 1 1 d . . . O1 O 0.43650(13) 0.3043(2) 0.88118(12) 0.0572(6) Uani 1 1 d . . . O2 O 0.61283(13) -0.00649(18) 0.86156(11) 0.0448(5) Uani 1 1 d . . . O3 O 0.55036(14) 0.0752(2) 1.07269(11) 0.0543(6) Uani 1 1 d . . . O4 O 0.9438(2) 0.6897(4) 1.07025(14) 0.1264(14) Uani 1 1 d . . . O5 O 1.01684(16) 0.5251(2) 1.15232(15) 0.0699(7) Uani 1 1 d . . . O6 O 1.06513(18) 0.7417(2) 1.1687(2) 0.0891(10) Uani 1 1 d . . . O7 O 0.92499(17) 0.6941(2) 0.91612(13) 0.0579(6) Uani 1 1 d D . . C1 C 0.50590(18) 0.2796(3) 0.91005(15) 0.0363(6) Uani 1 1 d . . . C2 C 0.62140(16) 0.0834(2) 0.89633(14) 0.0315(6) Uani 1 1 d . . . C3 C 0.57845(17) 0.1322(3) 1.03223(15) 0.0355(6) Uani 1 1 d . . . C4 C 0.83159(15) 0.3435(2) 1.01333(13) 0.0268(5) Uani 1 1 d . . . H4A H 0.8286 0.4174 1.0460 0.032 Uiso 1 1 calc R . . H4B H 0.8932 0.3175 1.0224 0.032 Uiso 1 1 calc R . . C5 C 0.80041(15) 0.3862(2) 0.93230(13) 0.0270(5) Uani 1 1 d . . . H5A H 0.8221 0.3245 0.9005 0.032 Uiso 1 1 calc R . . H5B H 0.8268 0.4703 0.9268 0.032 Uiso 1 1 calc R . . C6 C 0.82724(16) 0.0593(2) 1.02248(14) 0.0283(5) Uani 1 1 d . . . C7 C 0.83869(17) 0.0648(2) 0.94283(14) 0.0345(6) Uani 1 1 d . . . H7D H 0.8603 -0.0178 0.9299 0.052 Uiso 1 1 calc R . . H7E H 0.8803 0.1321 0.9392 0.052 Uiso 1 1 calc R . . H7C H 0.7828 0.0834 0.9084 0.052 Uiso 1 1 calc R . . C8 C 0.77359(18) -0.0597(2) 1.03108(15) 0.0363(6) Uani 1 1 d . . . H8A H 0.7150 -0.0513 0.9990 0.054 Uiso 1 1 calc R . . H8B H 0.7703 -0.0677 1.0830 0.054 Uiso 1 1 calc R . . H8C H 0.8014 -0.1361 1.0167 0.054 Uiso 1 1 calc R . . C9 C 0.91848(17) 0.0446(3) 1.07410(15) 0.0374(6) Uani 1 1 d . . . H9A H 0.9467 -0.0309 1.0594 0.056 Uiso 1 1 calc R . . H9B H 0.9138 0.0347 1.1255 0.056 Uiso 1 1 calc R . . H9C H 0.9530 0.1209 1.0702 0.056 Uiso 1 1 calc R . . C10 C 0.78503(17) 0.2345(2) 1.14388(13) 0.0332(6) Uani 1 1 d . . . C11 C 0.72183(19) 0.3368(3) 1.15897(15) 0.0428(7) Uani 1 1 d . . . H11A H 0.7339 0.3537 1.2125 0.064 Uiso 1 1 calc R . . H11B H 0.6621 0.3060 1.1413 0.064 Uiso 1 1 calc R . . H11C H 0.7292 0.4157 1.1327 0.064 Uiso 1 1 calc R . . C12 C 0.87732(19) 0.2817(3) 1.17981(15) 0.0418(7) Uani 1 1 d . . . H12A H 0.8867 0.3649 1.1587 0.063 Uiso 1 1 calc R . . H12B H 0.9196 0.2200 1.1700 0.063 Uiso 1 1 calc R . . H12C H 0.8845 0.2903 1.2336 0.063 Uiso 1 1 calc R . . C13 C 0.7684(2) 0.1105(3) 1.18331(15) 0.0444(7) Uani 1 1 d . . . H13A H 0.7707 0.1290 1.2356 0.067 Uiso 1 1 calc R . . H13B H 0.8129 0.0472 1.1804 0.067 Uiso 1 1 calc R . . H13C H 0.7111 0.0766 1.1590 0.067 Uiso 1 1 calc R . . C14 C 0.65431(17) 0.5691(2) 0.92053(14) 0.0320(6) Uani 1 1 d . . . C15 C 0.6874(2) 0.6703(2) 0.87398(16) 0.0426(7) Uani 1 1 d . . . H15A H 0.6560 0.6620 0.8217 0.064 Uiso 1 1 calc R . . H15B H 0.7495 0.6576 0.8785 0.064 Uiso 1 1 calc R . . H15C H 0.6777 0.7558 0.8920 0.064 Uiso 1 1 calc R . . C16 C 0.55610(19) 0.5846(3) 0.91017(18) 0.0454(7) Uani 1 1 d . . . H16A H 0.5428 0.6739 0.9191 0.068 Uiso 1 1 calc R . . H16B H 0.5365 0.5293 0.9455 0.068 Uiso 1 1 calc R . . H16C H 0.5263 0.5606 0.8593 0.068 Uiso 1 1 calc R . . C17 C 0.69803(19) 0.5971(2) 1.00226(15) 0.0398(7) Uani 1 1 d . . . H17A H 0.7611 0.5959 1.0093 0.060 Uiso 1 1 calc R . . H17B H 0.6810 0.5319 1.0339 0.060 Uiso 1 1 calc R . . H17C H 0.6799 0.6815 1.0158 0.060 Uiso 1 1 calc R . . C18 C 0.66567(17) 0.3845(2) 0.79333(13) 0.0300(5) Uani 1 1 d . . . C19 C 0.57721(18) 0.4372(3) 0.75132(15) 0.0442(7) Uani 1 1 d . . . H19A H 0.5666 0.4145 0.6986 0.066 Uiso 1 1 calc R . . H19B H 0.5770 0.5305 0.7564 0.066 Uiso 1 1 calc R . . H19C H 0.5316 0.4004 0.7722 0.066 Uiso 1 1 calc R . . C20 C 0.73804(19) 0.4503(3) 0.76542(15) 0.0451(7) Uani 1 1 d . . . H20A H 0.7263 0.4420 0.7112 0.068 Uiso 1 1 calc R . . H20B H 0.7938 0.4100 0.7883 0.068 Uiso 1 1 calc R . . H20C H 0.7403 0.5411 0.7789 0.068 Uiso 1 1 calc R . . C21 C 0.6673(2) 0.2434(3) 0.77325(15) 0.0475(8) Uani 1 1 d . . . H21A H 0.6155 0.2012 0.7815 0.071 Uiso 1 1 calc R . . H21B H 0.7192 0.2032 0.8045 0.071 Uiso 1 1 calc R . . H21C H 0.6684 0.2352 0.7208 0.071 Uiso 1 1 calc R . . C22 C 0.9239(2) 0.6872(3) 1.20174(17) 0.0434(7) Uani 1 1 d . . . H7A H 0.945(2) 0.622(2) 0.9062(19) 0.064(11) Uiso 1 1 d D . . H1 H 0.6192(19) 0.350(2) 1.0219(14) 0.057(9) Uiso 1 1 d D . . H7B H 0.932(2) 0.684(3) 0.9627(11) 0.069(12) Uiso 1 1 d 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 0.02333(11) 0.02562(12) 0.02642(11) -0.00070(8) 0.00907(8) -0.00276(8) S1 0.0509(5) 0.0439(4) 0.0440(4) -0.0010(3) 0.0251(4) 0.0033(3) P2 0.0253(3) 0.0220(3) 0.0239(3) 0.0007(2) 0.0080(3) 0.0009(2) P3 0.0268(3) 0.0230(3) 0.0221(3) 0.0006(2) 0.0072(3) -0.0026(2) F1 0.0932(15) 0.0555(11) 0.0778(14) 0.0079(10) 0.0484(12) 0.0270(11) F2 0.0731(16) 0.114(2) 0.188(3) -0.070(2) 0.0775(18) -0.0423(15) F3 0.139(2) 0.146(2) 0.0523(13) 0.0437(14) 0.0515(15) 0.0781(19) O1 0.0290(12) 0.0849(16) 0.0548(14) -0.0033(12) 0.0043(10) 0.0056(11) O2 0.0544(13) 0.0340(11) 0.0442(12) -0.0092(9) 0.0084(10) -0.0058(9) O3 0.0581(14) 0.0647(14) 0.0448(12) 0.0041(10) 0.0214(11) -0.0266(11) O4 0.150(3) 0.197(3) 0.0333(14) 0.0074(18) 0.0253(17) 0.091(3) O5 0.0835(18) 0.0371(12) 0.107(2) -0.0059(12) 0.0585(16) 0.0025(11) O6 0.0731(18) 0.0599(15) 0.159(3) -0.0300(16) 0.075(2) -0.0253(13) O7 0.0741(17) 0.0557(15) 0.0434(14) 0.0006(11) 0.0132(13) 0.0132(12) C1 0.0305(15) 0.0442(16) 0.0365(15) -0.0032(12) 0.0125(12) -0.0022(12) C2 0.0305(14) 0.0326(14) 0.0310(14) 0.0017(11) 0.0065(11) -0.0044(11) C3 0.0363(15) 0.0382(15) 0.0339(14) -0.0033(12) 0.0122(12) -0.0115(12) C4 0.0258(13) 0.0264(13) 0.0280(13) 0.0020(10) 0.0061(10) -0.0029(10) C5 0.0260(13) 0.0276(12) 0.0290(13) 0.0045(10) 0.0095(10) -0.0022(10) C6 0.0298(13) 0.0235(12) 0.0305(13) 0.0012(10) 0.0049(11) 0.0022(10) C7 0.0371(15) 0.0333(14) 0.0344(14) -0.0015(11) 0.0115(12) 0.0076(11) C8 0.0409(15) 0.0240(13) 0.0410(16) 0.0016(11) 0.0042(12) -0.0018(11) C9 0.0325(15) 0.0345(14) 0.0417(16) 0.0057(12) 0.0020(12) 0.0025(11) C10 0.0411(15) 0.0365(14) 0.0223(12) 0.0018(10) 0.0082(11) -0.0027(11) C11 0.0522(18) 0.0496(17) 0.0282(14) -0.0074(12) 0.0128(13) 0.0003(14) C12 0.0481(17) 0.0453(16) 0.0275(14) -0.0005(12) 0.0004(12) -0.0052(13) C13 0.0597(19) 0.0457(17) 0.0294(15) 0.0081(12) 0.0137(14) -0.0051(14) C14 0.0366(15) 0.0235(12) 0.0371(15) -0.0005(10) 0.0115(12) 0.0050(10) C15 0.0578(19) 0.0244(14) 0.0455(17) 0.0045(12) 0.0121(14) 0.0008(12) C16 0.0455(17) 0.0353(15) 0.0579(19) -0.0019(13) 0.0177(15) 0.0129(13) C17 0.0568(18) 0.0250(13) 0.0389(15) -0.0046(11) 0.0140(14) 0.0017(12) C18 0.0360(14) 0.0312(13) 0.0227(12) 0.0036(10) 0.0069(11) 0.0043(11) C19 0.0412(16) 0.0556(18) 0.0314(15) 0.0032(13) 0.0000(12) 0.0034(14) C20 0.0489(18) 0.0592(19) 0.0303(15) 0.0098(13) 0.0159(13) -0.0014(14) C21 0.076(2) 0.0426(16) 0.0249(13) -0.0036(12) 0.0136(14) 0.0081(15) C22 0.0458(18) 0.0421(16) 0.0467(18) 0.0001(13) 0.0200(14) -0.0018(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 H1 1.639(17) . ? Ru1 C3 1.917(3) . ? Ru1 C1 1.923(3) . ? Ru1 C2 1.999(3) . ? Ru1 P2 2.4456(6) . ? Ru1 P3 2.4470(7) . ? S1 O6 1.416(3) . ? S1 O4 1.415(3) . ? S1 O5 1.419(2) . ? S1 C22 1.811(3) . ? P2 C5 1.836(2) . ? P2 C18 1.896(2) . ? P2 C14 1.898(2) . ? P3 C4 1.841(2) . ? P3 C6 1.895(2) . ? P3 C10 1.902(2) . ? F1 C22 1.317(3) . ? F2 C22 1.321(4) . ? F3 C22 1.280(3) . ? O1 C1 1.133(3) . ? O2 C2 1.129(3) . ? O3 C3 1.131(3) . ? O7 H7B 0.848(18) . ? O7 H7A 0.859(18) . ? C4 C5 1.530(3) . ? C6 C7 1.532(3) . ? C6 C9 1.539(4) . ? C6 C8 1.539(3) . ? C10 C12 1.538(4) . ? C10 C11 1.539(4) . ? C10 C13 1.542(4) . ? C14 C16 1.535(4) . ? C14 C17 1.534(4) . ? C14 C15 1.536(4) . ? C18 C21 1.523(3) . ? C18 C20 1.534(4) . ? C18 C19 1.535(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 H1 Ru1 C3 83.8(10) . . ? H1 Ru1 C1 89.0(11) . . ? C3 Ru1 C1 91.53(11) . . ? H1 Ru1 C2 175.6(10) . . ? C3 Ru1 C2 91.76(10) . . ? C1 Ru1 C2 91.35(11) . . ? H1 Ru1 P2 83.1(10) . . ? C3 Ru1 P2 166.69(8) . . ? C1 Ru1 P2 90.83(8) . . ? C2 Ru1 P2 101.28(7) . . ? H1 Ru1 P3 81.9(11) . . ? C3 Ru1 P3 90.20(8) . . ? C1 Ru1 P3 170.48(8) . . ? C2 Ru1 P3 97.96(7) . . ? P2 Ru1 P3 85.40(2) . . ? O6 S1 O4 114.1(2) . . ? O6 S1 O5 114.78(17) . . ? O4 S1 O5 116.0(2) . . ? O6 S1 C22 102.63(15) . . ? O4 S1 C22 102.77(17) . . ? O5 S1 C22 104.17(14) . . ? C5 P2 C18 103.16(11) . . ? C5 P2 C14 105.71(11) . . ? C18 P2 C14 108.94(11) . . ? C5 P2 Ru1 105.37(7) . . ? C18 P2 Ru1 118.01(8) . . ? C14 P2 Ru1 114.24(8) . . ? C4 P3 C6 105.75(11) . . ? C4 P3 C10 102.93(11) . . ? C6 P3 C10 109.43(11) . . ? C4 P3 Ru1 105.76(8) . . ? C6 P3 Ru1 114.93(8) . . ? C10 P3 Ru1 116.65(9) . . ? H7B O7 H7A 98(3) . . ? O1 C1 Ru1 177.1(2) . . ? O2 C2 Ru1 171.6(2) . . ? O3 C3 Ru1 177.4(3) . . ? C5 C4 P3 114.53(16) . . ? C4 C5 P2 115.21(16) . . ? C7 C6 C9 106.8(2) . . ? C7 C6 C8 109.2(2) . . ? C9 C6 C8 108.5(2) . . ? C7 C6 P3 107.94(16) . . ? C9 C6 P3 113.62(17) . . ? C8 C6 P3 110.71(17) . . ? C12 C10 C11 107.1(2) . . ? C12 C10 C13 108.6(2) . . ? C11 C10 C13 107.7(2) . . ? C12 C10 P3 110.99(17) . . ? C11 C10 P3 110.23(17) . . ? C13 C10 P3 111.98(18) . . ? C16 C14 C17 107.9(2) . . ? C16 C14 C15 109.5(2) . . ? C17 C14 C15 106.8(2) . . ? C16 C14 P2 110.94(18) . . ? C17 C14 P2 108.86(17) . . ? C15 C14 P2 112.73(18) . . ? C21 C18 C20 107.1(2) . . ? C21 C18 C19 107.0(2) . . ? C20 C18 C19 109.7(2) . . ? C21 C18 P2 109.00(17) . . ? C20 C18 P2 112.03(18) . . ? C19 C18 P2 111.80(17) . . ? F3 C22 F1 106.9(3) . . ? F3 C22 F2 107.2(3) . . ? F1 C22 F2 105.4(3) . . ? F3 C22 S1 113.1(2) . . ? F1 C22 S1 112.9(2) . . ? F2 C22 S1 110.9(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.841 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.117