####################################################################### # # 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_Ruh3po2 _database_code_depnum_ccdc_archive 'CCDC 278841' #============================================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H38 O2 P3 Ru +, C F3 O3 S -' _chemical_formula_sum 'C42 H38 F3 O5 P3 Ru S' _chemical_formula_weight 905.76 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' F F 0.0171 0.0103 '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' 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 'P 21 21 21' 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 12.243(1) _cell_length_b 15.030(1) _cell_length_c 21.803(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4012.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9320 _cell_measurement_theta_min 4.10 _cell_measurement_theta_max 28.0 _exptl_crystal_description 'elongated prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.621 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_process_details 'CrysAlisRED (Oxford Diffraction, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3 CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44421 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.05 _diffrn_reflns_theta_max 34.65 _diffrn_reflns_theta_full 34.65 _diffrn_measured_fraction_theta_max 0.913 _diffrn_measured_fraction_theta_full 0.913 _reflns_number_total 15460 _reflns_number_gt 8918 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrysAlisCCD (Oxford Diffraction, 2001)' _computing_cell_refinement 'CrysAlisCCD (Oxford Diffraction, 2001)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2001)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (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^)+(0.0555P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(2) _refine_ls_number_reflns 15460 _refine_ls_number_parameters 507 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0879 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.902 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.229 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.070 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 Ru Ru -0.169724(16) 0.001630(17) -0.178684(8) 0.03750(6) Uani 1 1 d . . . P1 P -0.07442(8) 0.04114(6) -0.09578(4) 0.04781(19) Uani 1 1 d . . . H3 H 0.016(2) 0.0987(15) -0.1004(15) 0.057 Uiso 1 1 d D . . O1 O -0.1402(2) 0.10362(18) -0.05082(13) 0.0711(8) Uani 1 1 d D . . H1 H -0.112(4) 0.134(3) -0.011(2) 0.107 Uiso 1 1 d D . . O2 O -0.0167(3) -0.03396(17) -0.05888(13) 0.0710(8) Uani 1 1 d D . . H2 H 0.021(4) -0.021(3) -0.0172(19) 0.107 Uiso 1 1 d D . . P3 P -0.29749(6) -0.07247(5) -0.11633(3) 0.03755(16) Uani 1 1 d . . . P2 P -0.05095(6) -0.11544(5) -0.20220(3) 0.03941(17) Uani 1 1 d . . . C11 C -0.0496(2) -0.2213(2) -0.15925(13) 0.0434(7) Uani 1 1 d . . . C12 C 0.0150(3) -0.2299(2) -0.10774(15) 0.0542(8) Uani 1 1 d . . . H12 H 0.0593 -0.1827 -0.0959 0.065 Uiso 1 1 calc R . . C13 C 0.0156(4) -0.3071(3) -0.07336(19) 0.0729(12) Uani 1 1 d . . . H13 H 0.0598 -0.3114 -0.0388 0.087 Uiso 1 1 calc R . . C14 C -0.0492(4) -0.3775(3) -0.0903(2) 0.0739(12) Uani 1 1 d . . . H14 H -0.0490 -0.4295 -0.0673 0.089 Uiso 1 1 calc R . . C15 C -0.1138(4) -0.3708(3) -0.14091(19) 0.0668(10) Uani 1 1 d . . . H15 H -0.1569 -0.4189 -0.1525 0.080 Uiso 1 1 calc R . . C16 C -0.1164(3) -0.2920(2) -0.17614(17) 0.0550(8) Uani 1 1 d . . . H16 H -0.1620 -0.2875 -0.2101 0.066 Uiso 1 1 calc R . . C21 C -0.0677(3) -0.1517(2) -0.28316(13) 0.0481(7) Uani 1 1 d . . . C22 C 0.0158(3) -0.1465(3) -0.32567(15) 0.0632(9) Uani 1 1 d . . . H22 H 0.0848 -0.1276 -0.3135 0.076 Uiso 1 1 calc R . . C23 C -0.0028(4) -0.1693(4) -0.38663(19) 0.0896(15) Uani 1 1 d . . . H23 H 0.0539 -0.1652 -0.4148 0.108 Uiso 1 1 calc R . . C24 C -0.1028(5) -0.1976(4) -0.40565(19) 0.0911(15) Uani 1 1 d . . . H24 H -0.1144 -0.2127 -0.4465 0.109 Uiso 1 1 calc R . . C25 C -0.1869(4) -0.2037(3) -0.36366(19) 0.0849(13) Uani 1 1 d . . . H25 H -0.2555 -0.2236 -0.3759 0.102 Uiso 1 1 calc R . . C26 C -0.1684(3) -0.1800(3) -0.30311(17) 0.0654(10) Uani 1 1 d . . . H26 H -0.2257 -0.1833 -0.2752 0.079 Uiso 1 1 calc R . . C31 C 0.0953(2) -0.0877(2) -0.20288(13) 0.0445(7) Uani 1 1 d . . . C32 C 0.1286(2) 0.0002(3) -0.20878(13) 0.0545(7) Uani 1 1 d . . . H32 H 0.0772 0.0458 -0.2074 0.065 Uiso 1 1 calc R . . C33 C 0.2385(3) 0.0202(3) -0.21672(19) 0.0732(12) Uani 1 1 d . . . H33 H 0.2604 0.0792 -0.2205 0.088 Uiso 1 1 calc R . . C34 C 0.3150(3) -0.0468(3) -0.21903(19) 0.0782(12) Uani 1 1 d . . . H34 H 0.3884 -0.0328 -0.2247 0.094 Uiso 1 1 calc R . . C35 C 0.2839(3) -0.1335(3) -0.2131(2) 0.0747(12) Uani 1 1 d . . . H35 H 0.3357 -0.1787 -0.2146 0.090 Uiso 1 1 calc R . . C36 C 0.1749(3) -0.1535(2) -0.20484(17) 0.0566(8) Uani 1 1 d . . . H36 H 0.1542 -0.2127 -0.2005 0.068 Uiso 1 1 calc R . . C41 C -0.2589(3) -0.1046(2) -0.03800(13) 0.0465(7) Uani 1 1 d . . . C42 C -0.2016(3) -0.1816(3) -0.02533(15) 0.0586(9) Uani 1 1 d . . . H42 H -0.1849 -0.2211 -0.0568 0.070 Uiso 1 1 calc R . . C43 C -0.1690(4) -0.1999(3) 0.03391(18) 0.0774(12) Uani 1 1 d . . . H43 H -0.1307 -0.2521 0.0419 0.093 Uiso 1 1 calc R . . C44 C -0.1918(4) -0.1430(4) 0.08115(16) 0.0793(13) Uani 1 1 d . . . H44 H -0.1690 -0.1561 0.1208 0.095 Uiso 1 1 calc R . . C45 C -0.2487(3) -0.0664(3) 0.06920(14) 0.0690(11) Uani 1 1 d . . . H45 H -0.2649 -0.0269 0.1008 0.083 Uiso 1 1 calc R . . C46 C -0.2818(3) -0.0481(3) 0.01017(14) 0.0573(9) Uani 1 1 d . . . H46 H -0.3207 0.0038 0.0026 0.069 Uiso 1 1 calc R . . C51 C -0.4218(2) -0.0079(2) -0.09883(12) 0.0441(6) Uani 1 1 d . . . C52 C -0.4170(4) 0.0839(3) -0.08847(17) 0.0635(10) Uani 1 1 d . . . H52 H -0.3512 0.1141 -0.0928 0.076 Uiso 1 1 calc R . . C53 C -0.5108(4) 0.1300(3) -0.0716(2) 0.0792(13) Uani 1 1 d . . . H53 H -0.5078 0.1914 -0.0667 0.095 Uiso 1 1 calc R . . C54 C -0.6062(4) 0.0872(3) -0.06235(19) 0.0773(12) Uani 1 1 d . . . H54 H -0.6677 0.1189 -0.0500 0.093 Uiso 1 1 calc R . . C55 C -0.6127(3) -0.0023(4) -0.07096(18) 0.0812(12) Uani 1 1 d . . . H55 H -0.6785 -0.0318 -0.0645 0.097 Uiso 1 1 calc R . . C56 C -0.5209(3) -0.0496(3) -0.08948(17) 0.0645(9) Uani 1 1 d . . . H56 H -0.5263 -0.1106 -0.0957 0.077 Uiso 1 1 calc R . . C61 C -0.3607(2) -0.1726(2) -0.15011(14) 0.0431(7) Uani 1 1 d . . . C62 C -0.3961(3) -0.1656(3) -0.21054(16) 0.0567(9) Uani 1 1 d . . . H62 H -0.3892 -0.1120 -0.2315 0.068 Uiso 1 1 calc R . . C63 C -0.4422(3) -0.2396(4) -0.2398(2) 0.0784(13) Uani 1 1 d . . . H63 H -0.4655 -0.2354 -0.2803 0.094 Uiso 1 1 calc R . . C64 C -0.4526(4) -0.3174(4) -0.2090(3) 0.0968(18) Uani 1 1 d . . . H64 H -0.4799 -0.3670 -0.2293 0.116 Uiso 1 1 calc R . . C65 C -0.4239(4) -0.3245(3) -0.1488(3) 0.0876(15) Uani 1 1 d . . . H65 H -0.4355 -0.3776 -0.1279 0.105 Uiso 1 1 calc R . . C66 C -0.3774(3) -0.2522(3) -0.1186(2) 0.0655(10) Uani 1 1 d . . . H66 H -0.3576 -0.2569 -0.0776 0.079 Uiso 1 1 calc R . . C71 C -0.2485(3) 0.0287(3) -0.27058(15) 0.0643(11) Uani 1 1 d . . . H71 H -0.2798 -0.0156 -0.2946 0.077 Uiso 1 1 calc R . . C72 C -0.1381(3) 0.0582(2) -0.27235(15) 0.0595(9) Uani 1 1 d . . . H72 H -0.0835 0.0361 -0.2978 0.071 Uiso 1 1 calc R . . C73 C -0.1263(4) 0.1254(3) -0.22959(18) 0.0666(10) Uani 1 1 d . . . H73 H -0.0618 0.1561 -0.2218 0.080 Uiso 1 1 calc R . . C74 C -0.2250(4) 0.1403(3) -0.1999(2) 0.0757(12) Uani 1 1 d . . . H74 H -0.2385 0.1820 -0.1693 0.091 Uiso 1 1 calc R . . C75 C -0.3010(3) 0.0798(3) -0.2253(2) 0.0795(14) Uani 1 1 d . . . H75 H -0.3739 0.0746 -0.2138 0.095 Uiso 1 1 calc R . . S S 0.02179(10) 0.07784(8) 0.08914(5) 0.0782(3) Uani 1 1 d . . . O4 O 0.0495(4) 0.0018(2) 0.05273(14) 0.1153(13) Uani 1 1 d . . . O5 O -0.0384(3) 0.1437(2) 0.05612(17) 0.0988(11) Uani 1 1 d . . . O6 O -0.0090(4) 0.0573(3) 0.15114(16) 0.1187(13) Uani 1 1 d . . . C8 C 0.1538(5) 0.1298(4) 0.0982(3) 0.1045(17) Uani 1 1 d . . . F1 F 0.1447(4) 0.1984(2) 0.13567(19) 0.1424(15) Uani 1 1 d . . . F2 F 0.2236(3) 0.0748(3) 0.1243(2) 0.1400(13) Uani 1 1 d . . . F3 F 0.1907(4) 0.1588(4) 0.0475(2) 0.183(2) 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 Ru 0.03918(10) 0.04024(12) 0.03307(9) 0.00522(11) 0.00114(8) 0.00186(13) P1 0.0506(5) 0.0450(5) 0.0478(4) -0.0074(4) -0.0046(4) -0.0023(4) O1 0.0819(19) 0.0625(17) 0.0690(17) -0.0202(13) -0.0090(14) 0.0085(14) O2 0.0842(19) 0.0656(16) 0.0633(15) -0.0080(12) -0.0278(14) 0.0048(13) P3 0.0385(4) 0.0422(4) 0.0319(3) 0.0037(3) 0.0017(3) 0.0026(3) P2 0.0367(4) 0.0478(5) 0.0337(3) -0.0019(3) 0.0019(3) 0.0013(3) C11 0.0419(16) 0.0462(18) 0.0423(15) -0.0028(12) 0.0060(12) 0.0087(14) C12 0.0520(19) 0.056(2) 0.0542(19) 0.0035(15) 0.0003(15) 0.0139(16) C13 0.078(3) 0.079(3) 0.062(2) 0.016(2) 0.002(2) 0.036(2) C14 0.086(3) 0.058(3) 0.077(3) 0.021(2) 0.017(2) 0.015(2) C15 0.078(3) 0.048(2) 0.075(3) -0.0003(18) 0.011(2) -0.0002(19) C16 0.057(2) 0.053(2) 0.0541(18) -0.0020(17) 0.0071(16) 0.0003(16) C21 0.0470(17) 0.059(2) 0.0384(15) -0.0038(13) 0.0032(13) -0.0017(15) C22 0.054(2) 0.093(3) 0.0421(16) -0.0078(18) 0.0072(15) -0.0091(19) C23 0.087(3) 0.134(4) 0.048(2) -0.020(2) 0.021(2) -0.005(3) C24 0.104(4) 0.123(4) 0.046(2) -0.026(2) 0.001(2) -0.010(3) C25 0.073(3) 0.120(4) 0.062(2) -0.025(2) -0.012(2) -0.018(3) C26 0.055(2) 0.090(3) 0.0516(18) -0.0106(18) 0.0024(17) -0.005(2) C31 0.0374(15) 0.058(2) 0.0383(14) -0.0010(14) 0.0033(12) 0.0025(14) C32 0.0457(14) 0.067(2) 0.0508(15) 0.000(2) -0.0008(12) 0.000(2) C33 0.053(2) 0.083(3) 0.084(3) 0.018(2) -0.0029(18) -0.018(2) C34 0.042(2) 0.114(4) 0.079(3) 0.013(2) 0.0056(18) -0.004(2) C35 0.0416(19) 0.102(4) 0.081(3) -0.005(2) 0.0077(18) 0.010(2) C36 0.0422(17) 0.063(2) 0.064(2) -0.0100(16) 0.0035(16) 0.0020(17) C41 0.0471(17) 0.059(2) 0.0332(13) 0.0075(13) 0.0040(12) -0.0030(15) C42 0.058(2) 0.072(2) 0.0459(17) 0.0126(16) 0.0026(15) 0.0163(18) C43 0.063(2) 0.108(3) 0.062(2) 0.029(2) -0.007(2) 0.023(2) C44 0.067(3) 0.134(4) 0.0370(17) 0.019(2) -0.0070(16) -0.007(3) C45 0.078(3) 0.095(3) 0.0335(15) 0.0015(18) 0.0019(16) -0.011(2) C46 0.060(2) 0.071(2) 0.0408(16) 0.0030(15) 0.0013(14) -0.0123(18) C51 0.0429(13) 0.0502(19) 0.0391(12) 0.0083(15) 0.0018(10) 0.0042(16) C52 0.068(2) 0.058(2) 0.065(2) 0.0026(18) 0.0157(18) 0.0127(19) C53 0.088(3) 0.061(3) 0.089(3) 0.001(2) 0.021(2) 0.027(2) C54 0.064(3) 0.092(3) 0.076(3) -0.009(2) 0.013(2) 0.035(2) C55 0.0492(19) 0.107(4) 0.087(3) -0.010(3) 0.0118(17) 0.014(3) C56 0.055(2) 0.078(3) 0.061(2) -0.0075(19) 0.0128(17) 0.0062(19) C61 0.0349(15) 0.0464(18) 0.0479(16) -0.0047(14) 0.0042(12) 0.0008(12) C62 0.0424(17) 0.077(2) 0.0512(18) -0.0068(17) 0.0001(14) -0.0097(17) C63 0.042(2) 0.111(4) 0.082(3) -0.036(3) -0.0053(19) -0.004(2) C64 0.055(3) 0.079(4) 0.156(5) -0.049(4) -0.006(3) -0.023(2) C65 0.066(3) 0.051(3) 0.146(5) -0.001(3) 0.003(3) -0.011(2) C66 0.057(2) 0.056(2) 0.084(3) 0.010(2) 0.0005(19) -0.0050(18) C71 0.070(2) 0.080(3) 0.0427(16) 0.0228(16) -0.0109(16) -0.0033(19) C72 0.075(2) 0.059(2) 0.0446(17) 0.0206(16) 0.0129(15) 0.0041(18) C73 0.071(2) 0.056(2) 0.073(3) 0.027(2) 0.004(2) 0.0032(19) C74 0.091(3) 0.054(2) 0.082(3) 0.025(2) 0.015(2) 0.028(2) C75 0.051(2) 0.099(3) 0.088(3) 0.066(3) 0.002(2) 0.023(2) S 0.0867(8) 0.0799(7) 0.0679(6) -0.0153(6) -0.0193(6) -0.0088(6) O4 0.197(4) 0.0680(18) 0.0812(19) -0.0245(18) -0.067(2) 0.026(3) O5 0.115(3) 0.0693(19) 0.112(3) -0.0302(17) -0.055(2) 0.0140(18) O6 0.131(3) 0.154(3) 0.071(2) -0.004(2) 0.011(2) -0.037(3) C8 0.099(4) 0.100(4) 0.114(5) 0.005(4) -0.008(4) 0.008(3) F1 0.156(4) 0.102(2) 0.169(4) -0.045(2) -0.049(3) -0.027(2) F2 0.105(3) 0.142(3) 0.173(3) -0.005(3) -0.049(2) 0.028(2) F3 0.137(4) 0.269(6) 0.142(3) 0.071(4) 0.034(3) -0.016(4) _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 Ru C73 2.230(4) . ? Ru P1 2.2319(9) . ? Ru C75 2.235(3) . ? Ru C74 2.239(4) . ? Ru C72 2.246(3) . ? Ru C71 2.261(3) . ? Ru P2 2.3396(8) . ? Ru P3 2.3527(8) . ? P1 O2 1.556(3) . ? P1 O1 1.579(3) . ? P1 H3 1.40(3) . ? O1 H1 1.04(4) . ? O2 H2 1.03(4) . ? P3 C41 1.837(3) . ? P3 C51 1.845(3) . ? P3 C61 1.845(3) . ? P2 C31 1.839(3) . ? P2 C11 1.846(3) . ? P2 C21 1.859(3) . ? C11 C12 1.380(5) . ? C11 C16 1.391(5) . ? C12 C13 1.381(5) . ? C12 H12 0.9300 . ? C13 C14 1.373(6) . ? C13 H13 0.9300 . ? C14 C15 1.361(6) . ? C14 H14 0.9300 . ? C15 C16 1.412(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C26 1.374(5) . ? C21 C22 1.383(4) . ? C22 C23 1.392(5) . ? C22 H22 0.9300 . ? C23 C24 1.360(7) . ? C23 H23 0.9300 . ? C24 C25 1.381(6) . ? C24 H24 0.9300 . ? C25 C26 1.386(5) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C32 1.389(5) . ? C31 C36 1.389(4) . ? C32 C33 1.390(5) . ? C32 H32 0.9300 . ? C33 C34 1.376(6) . ? C33 H33 0.9300 . ? C34 C35 1.364(6) . ? C34 H34 0.9300 . ? C35 C36 1.380(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C46 1.379(5) . ? C41 C42 1.381(5) . ? C42 C43 1.380(5) . ? C42 H42 0.9300 . ? C43 C44 1.368(6) . ? C43 H43 0.9300 . ? C44 C45 1.371(6) . ? C44 H44 0.9300 . ? C45 C46 1.376(5) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C56 1.380(5) . ? C51 C52 1.399(5) . ? C52 C53 1.391(6) . ? C52 H52 0.9300 . ? C53 C54 1.348(7) . ? C53 H53 0.9300 . ? C54 C55 1.361(7) . ? C54 H54 0.9300 . ? C55 C56 1.390(5) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C61 C62 1.391(5) . ? C61 C66 1.394(5) . ? C62 C63 1.400(6) . ? C62 H62 0.9300 . ? C63 C64 1.354(7) . ? C63 H63 0.9300 . ? C64 C65 1.362(8) . ? C64 H64 0.9300 . ? C65 C66 1.392(6) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C71 C75 1.406(6) . ? C71 C72 1.423(6) . ? C71 H71 0.9300 . ? C72 C73 1.382(5) . ? C72 H72 0.9300 . ? C73 C74 1.389(6) . ? C73 H73 0.9300 . ? C74 C75 1.413(6) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? S O5 1.428(3) . ? S O4 1.432(3) . ? S O6 1.437(4) . ? S C8 1.806(6) . ? C8 F3 1.272(7) . ? C8 F2 1.318(6) . ? C8 F1 1.320(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C73 Ru P1 93.24(12) . . ? C73 Ru C75 60.45(16) . . ? P1 Ru C75 127.17(15) . . ? C73 Ru C74 36.21(15) . . ? P1 Ru C74 94.46(14) . . ? C75 Ru C74 36.83(17) . . ? C73 Ru C72 35.97(14) . . ? P1 Ru C72 123.07(11) . . ? C75 Ru C72 60.77(14) . . ? C74 Ru C72 60.79(15) . . ? C73 Ru C71 60.70(15) . . ? P1 Ru C71 153.25(11) . . ? C75 Ru C71 36.46(15) . . ? C74 Ru C71 61.34(17) . . ? C72 Ru C71 36.82(14) . . ? C73 Ru P2 111.71(11) . . ? P1 Ru P2 93.02(3) . . ? C75 Ru P2 137.96(14) . . ? C74 Ru P2 147.40(12) . . ? C72 Ru P2 88.75(10) . . ? C71 Ru P2 101.91(11) . . ? C73 Ru P3 147.23(11) . . ? P1 Ru P3 90.32(3) . . ? C75 Ru P3 91.92(10) . . ? C74 Ru P3 111.04(12) . . ? C72 Ru P3 145.02(11) . . ? C71 Ru P3 108.28(10) . . ? P2 Ru P3 100.59(3) . . ? O2 P1 O1 110.01(16) . . ? O2 P1 Ru 117.59(10) . . ? O1 P1 Ru 113.23(12) . . ? O2 P1 H3 97.3(9) . . ? O1 P1 H3 94.5(9) . . ? Ru P1 H3 121.1(13) . . ? P1 O1 H1 128(3) . . ? P1 O2 H2 121(3) . . ? C41 P3 C51 99.11(13) . . ? C41 P3 C61 105.35(15) . . ? C51 P3 C61 99.52(14) . . ? C41 P3 Ru 119.38(10) . . ? C51 P3 Ru 114.77(10) . . ? C61 P3 Ru 115.74(10) . . ? C31 P2 C11 101.00(14) . . ? C31 P2 C21 99.58(14) . . ? C11 P2 C21 103.31(14) . . ? C31 P2 Ru 115.89(11) . . ? C11 P2 Ru 122.84(9) . . ? C21 P2 Ru 111.10(11) . . ? C12 C11 C16 118.7(3) . . ? C12 C11 P2 120.0(3) . . ? C16 C11 P2 121.3(2) . . ? C11 C12 C13 121.6(4) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C14 C13 C12 119.9(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 119.9(4) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 121.0(4) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C11 C16 C15 119.0(3) . . ? C11 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C26 C21 C22 118.0(3) . . ? C26 C21 P2 119.4(2) . . ? C22 C21 P2 122.6(3) . . ? C21 C22 C23 120.3(4) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 121.1(4) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 119.3(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C26 119.5(4) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C21 C26 C25 121.9(4) . . ? C21 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C32 C31 C36 118.0(3) . . ? C32 C31 P2 120.1(2) . . ? C36 C31 P2 121.5(3) . . ? C31 C32 C33 120.1(4) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 120.4(4) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 120.3(4) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 119.4(4) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C35 C36 C31 121.8(4) . . ? C35 C36 H36 119.1 . . ? C31 C36 H36 119.1 . . ? C46 C41 C42 117.8(3) . . ? C46 C41 P3 119.6(3) . . ? C42 C41 P3 122.5(3) . . ? C43 C42 C41 120.1(4) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 C42 121.4(4) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C43 C44 C45 119.1(3) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C44 C45 C46 119.6(4) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C45 C46 C41 122.0(4) . . ? C45 C46 H46 119.0 . . ? C41 C46 H46 119.0 . . ? C56 C51 C52 117.4(3) . . ? C56 C51 P3 121.1(3) . . ? C52 C51 P3 121.2(3) . . ? C53 C52 C51 119.9(4) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C54 C53 C52 121.2(4) . . ? C54 C53 H53 119.4 . . ? C52 C53 H53 119.4 . . ? C53 C54 C55 120.1(4) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C54 C55 C56 119.9(4) . . ? C54 C55 H55 120.1 . . ? C56 C55 H55 120.1 . . ? C51 C56 C55 121.5(4) . . ? C51 C56 H56 119.3 . . ? C55 C56 H56 119.3 . . ? C62 C61 C66 119.0(3) . . ? C62 C61 P3 116.6(3) . . ? C66 C61 P3 124.4(3) . . ? C61 C62 C63 119.8(4) . . ? C61 C62 H62 120.1 . . ? C63 C62 H62 120.1 . . ? C64 C63 C62 119.8(4) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C63 C64 C65 121.4(4) . . ? C63 C64 H64 119.3 . . ? C65 C64 H64 119.3 . . ? C64 C65 C66 120.0(4) . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C65 C66 C61 119.8(4) . . ? C65 C66 H66 120.1 . . ? C61 C66 H66 120.1 . . ? C75 C71 C72 106.4(4) . . ? C75 C71 Ru 70.77(19) . . ? C72 C71 Ru 71.02(19) . . ? C75 C71 H71 126.8 . . ? C72 C71 H71 126.8 . . ? Ru C71 H71 123.1 . . ? C73 C72 C71 108.0(4) . . ? C73 C72 Ru 71.4(2) . . ? C71 C72 Ru 72.16(18) . . ? C73 C72 H72 126.0 . . ? C71 C72 H72 126.0 . . ? Ru C72 H72 122.1 . . ? C72 C73 C74 110.0(4) . . ? C72 C73 Ru 72.6(2) . . ? C74 C73 Ru 72.3(2) . . ? C72 C73 H73 125.0 . . ? C74 C73 H73 125.0 . . ? Ru C73 H73 121.7 . . ? C73 C74 C75 106.6(4) . . ? C73 C74 Ru 71.5(2) . . ? C75 C74 Ru 71.4(2) . . ? C73 C74 H74 126.7 . . ? C75 C74 H74 126.7 . . ? Ru C74 H74 122.2 . . ? C71 C75 C74 109.0(4) . . ? C71 C75 Ru 72.8(2) . . ? C74 C75 Ru 71.8(2) . . ? C71 C75 H75 125.5 . . ? C74 C75 H75 125.5 . . ? Ru C75 H75 121.6 . . ? O5 S O4 113.29(18) . . ? O5 S O6 119.2(3) . . ? O4 S O6 114.3(2) . . ? O5 S C8 102.5(2) . . ? O4 S C8 101.2(3) . . ? O6 S C8 103.0(3) . . ? F3 C8 F2 111.1(6) . . ? F3 C8 F1 107.5(6) . . ? F2 C8 F1 106.2(5) . . ? F3 C8 S 111.7(5) . . ? F2 C8 S 110.9(4) . . ? F1 C8 S 109.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C73 Ru P1 O2 -145.36(19) . . . . ? C75 Ru P1 O2 159.88(19) . . . . ? C74 Ru P1 O2 178.36(19) . . . . ? C72 Ru P1 O2 -123.86(19) . . . . ? C71 Ru P1 O2 -157.7(3) . . . . ? P2 Ru P1 O2 -33.39(15) . . . . ? P3 Ru P1 O2 67.23(15) . . . . ? C73 Ru P1 O1 84.52(17) . . . . ? C75 Ru P1 O1 29.75(18) . . . . ? C74 Ru P1 O1 48.24(18) . . . . ? C72 Ru P1 O1 106.01(18) . . . . ? C71 Ru P1 O1 72.2(3) . . . . ? P2 Ru P1 O1 -163.52(13) . . . . ? P3 Ru P1 O1 -62.89(13) . . . . ? C73 Ru P3 C41 -116.2(2) . . . . ? P1 Ru P3 C41 -19.69(13) . . . . ? C75 Ru P3 C41 -146.9(2) . . . . ? C74 Ru P3 C41 -114.6(2) . . . . ? C72 Ru P3 C41 176.7(2) . . . . ? C71 Ru P3 C41 179.87(17) . . . . ? P2 Ru P3 C41 73.44(13) . . . . ? C73 Ru P3 C51 1.2(2) . . . . ? P1 Ru P3 C51 97.69(11) . . . . ? C75 Ru P3 C51 -29.52(18) . . . . ? C74 Ru P3 C51 2.79(18) . . . . ? C72 Ru P3 C51 -66.0(2) . . . . ? C71 Ru P3 C51 -62.75(16) . . . . ? P2 Ru P3 C51 -169.18(10) . . . . ? C73 Ru P3 C61 116.3(2) . . . . ? P1 Ru P3 C61 -147.18(11) . . . . ? C75 Ru P3 C61 85.61(18) . . . . ? C74 Ru P3 C61 117.92(18) . . . . ? C72 Ru P3 C61 49.2(2) . . . . ? C71 Ru P3 C61 52.38(16) . . . . ? P2 Ru P3 C61 -54.05(11) . . . . ? C73 Ru P2 C31 45.41(17) . . . . ? P1 Ru P2 C31 -49.29(11) . . . . ? C75 Ru P2 C31 114.9(2) . . . . ? C74 Ru P2 C31 53.8(3) . . . . ? C72 Ru P2 C31 73.76(15) . . . . ? C71 Ru P2 C31 108.38(15) . . . . ? P3 Ru P2 C31 -140.18(11) . . . . ? C73 Ru P2 C11 169.86(17) . . . . ? P1 Ru P2 C11 75.17(13) . . . . ? C75 Ru P2 C11 -120.7(2) . . . . ? C74 Ru P2 C11 178.3(3) . . . . ? C72 Ru P2 C11 -161.78(16) . . . . ? C71 Ru P2 C11 -127.16(16) . . . . ? P3 Ru P2 C11 -15.72(13) . . . . ? C73 Ru P2 C21 -67.27(17) . . . . ? P1 Ru P2 C21 -161.97(11) . . . . ? C75 Ru P2 C21 2.2(2) . . . . ? C74 Ru P2 C21 -58.9(3) . . . . ? C72 Ru P2 C21 -38.92(15) . . . . ? C71 Ru P2 C21 -4.30(15) . . . . ? P3 Ru P2 C21 107.14(11) . . . . ? C31 P2 C11 C12 42.6(3) . . . . ? C21 P2 C11 C12 145.3(3) . . . . ? Ru P2 C11 C12 -88.3(3) . . . . ? C31 P2 C11 C16 -140.2(3) . . . . ? C21 P2 C11 C16 -37.5(3) . . . . ? Ru P2 C11 C16 88.9(3) . . . . ? C16 C11 C12 C13 0.7(5) . . . . ? P2 C11 C12 C13 178.0(3) . . . . ? C11 C12 C13 C14 0.1(6) . . . . ? C12 C13 C14 C15 -0.1(6) . . . . ? C13 C14 C15 C16 -0.7(6) . . . . ? C12 C11 C16 C15 -1.5(5) . . . . ? P2 C11 C16 C15 -178.7(3) . . . . ? C14 C15 C16 C11 1.5(6) . . . . ? C31 P2 C21 C26 179.4(3) . . . . ? C11 P2 C21 C26 75.6(3) . . . . ? Ru P2 C21 C26 -57.9(3) . . . . ? C31 P2 C21 C22 -4.6(3) . . . . ? C11 P2 C21 C22 -108.4(3) . . . . ? Ru P2 C21 C22 118.1(3) . . . . ? C26 C21 C22 C23 0.0(6) . . . . ? P2 C21 C22 C23 -176.0(4) . . . . ? C21 C22 C23 C24 -0.4(8) . . . . ? C22 C23 C24 C25 0.0(9) . . . . ? C23 C24 C25 C26 0.7(8) . . . . ? C22 C21 C26 C25 0.7(6) . . . . ? P2 C21 C26 C25 176.9(3) . . . . ? C24 C25 C26 C21 -1.1(7) . . . . ? C11 P2 C31 C32 -154.9(2) . . . . ? C21 P2 C31 C32 99.4(3) . . . . ? Ru P2 C31 C32 -19.7(3) . . . . ? C11 P2 C31 C36 32.8(3) . . . . ? C21 P2 C31 C36 -72.9(3) . . . . ? Ru P2 C31 C36 167.9(2) . . . . ? C36 C31 C32 C33 0.4(5) . . . . ? P2 C31 C32 C33 -172.2(3) . . . . ? C31 C32 C33 C34 0.2(5) . . . . ? C32 C33 C34 C35 -0.5(6) . . . . ? C33 C34 C35 C36 0.1(6) . . . . ? C34 C35 C36 C31 0.6(6) . . . . ? C32 C31 C36 C35 -0.8(5) . . . . ? P2 C31 C36 C35 171.7(3) . . . . ? C51 P3 C41 C46 -32.1(3) . . . . ? C61 P3 C41 C46 -134.7(3) . . . . ? Ru P3 C41 C46 93.1(3) . . . . ? C51 P3 C41 C42 151.7(3) . . . . ? C61 P3 C41 C42 49.2(3) . . . . ? Ru P3 C41 C42 -83.0(3) . . . . ? C46 C41 C42 C43 -0.1(5) . . . . ? P3 C41 C42 C43 176.1(3) . . . . ? C41 C42 C43 C44 -0.3(6) . . . . ? C42 C43 C44 C45 0.3(7) . . . . ? C43 C44 C45 C46 0.0(6) . . . . ? C44 C45 C46 C41 -0.4(6) . . . . ? C42 C41 C46 C45 0.4(5) . . . . ? P3 C41 C46 C45 -175.9(3) . . . . ? C41 P3 C51 C56 -82.4(3) . . . . ? C61 P3 C51 C56 25.0(3) . . . . ? Ru P3 C51 C56 149.2(2) . . . . ? C41 P3 C51 C52 91.1(3) . . . . ? C61 P3 C51 C52 -161.5(3) . . . . ? Ru P3 C51 C52 -37.3(3) . . . . ? C56 C51 C52 C53 -2.3(5) . . . . ? P3 C51 C52 C53 -176.0(3) . . . . ? C51 C52 C53 C54 3.0(6) . . . . ? C52 C53 C54 C55 -1.8(7) . . . . ? C53 C54 C55 C56 -0.1(7) . . . . ? C52 C51 C56 C55 0.5(5) . . . . ? P3 C51 C56 C55 174.2(3) . . . . ? C54 C55 C56 C51 0.7(6) . . . . ? C41 P3 C61 C62 -179.2(2) . . . . ? C51 P3 C61 C62 78.6(3) . . . . ? Ru P3 C61 C62 -45.0(3) . . . . ? C41 P3 C61 C66 2.7(3) . . . . ? C51 P3 C61 C66 -99.6(3) . . . . ? Ru P3 C61 C66 136.9(3) . . . . ? C66 C61 C62 C63 -3.5(5) . . . . ? P3 C61 C62 C63 178.2(3) . . . . ? C61 C62 C63 C64 0.4(6) . . . . ? C62 C63 C64 C65 3.2(7) . . . . ? C63 C64 C65 C66 -3.5(8) . . . . ? C64 C65 C66 C61 0.3(7) . . . . ? C62 C61 C66 C65 3.2(5) . . . . ? P3 C61 C66 C65 -178.7(3) . . . . ? C73 Ru C71 C75 -78.9(3) . . . . ? P1 Ru C71 C75 -64.8(4) . . . . ? C74 Ru C71 C75 -37.3(2) . . . . ? C72 Ru C71 C75 -115.9(3) . . . . ? P2 Ru C71 C75 172.7(2) . . . . ? P3 Ru C71 C75 67.2(3) . . . . ? C73 Ru C71 C72 37.0(2) . . . . ? P1 Ru C71 C72 51.1(4) . . . . ? C75 Ru C71 C72 115.9(3) . . . . ? C74 Ru C71 C72 78.6(3) . . . . ? P2 Ru C71 C72 -71.4(2) . . . . ? P3 Ru C71 C72 -176.9(2) . . . . ? C75 C71 C72 C73 -0.5(4) . . . . ? Ru C71 C72 C73 -62.8(2) . . . . ? C75 C71 C72 Ru 62.3(2) . . . . ? P1 Ru C72 C73 -38.5(3) . . . . ? C75 Ru C72 C73 79.0(3) . . . . ? C74 Ru C72 C73 36.5(3) . . . . ? C71 Ru C72 C73 116.8(3) . . . . ? P2 Ru C72 C73 -131.3(2) . . . . ? P3 Ru C72 C73 121.9(2) . . . . ? C73 Ru C72 C71 -116.8(3) . . . . ? P1 Ru C72 C71 -155.3(2) . . . . ? C75 Ru C72 C71 -37.8(2) . . . . ? C74 Ru C72 C71 -80.2(3) . . . . ? P2 Ru C72 C71 111.9(2) . . . . ? P3 Ru C72 C71 5.1(3) . . . . ? C71 C72 C73 C74 0.3(4) . . . . ? Ru C72 C73 C74 -63.1(3) . . . . ? C71 C72 C73 Ru 63.3(2) . . . . ? P1 Ru C73 C72 148.5(2) . . . . ? C75 Ru C73 C72 -80.0(3) . . . . ? C74 Ru C73 C72 -118.4(4) . . . . ? C71 Ru C73 C72 -37.9(2) . . . . ? P2 Ru C73 C72 53.9(3) . . . . ? P3 Ru C73 C72 -115.9(2) . . . . ? P1 Ru C73 C74 -93.1(3) . . . . ? C75 Ru C73 C74 38.4(3) . . . . ? C72 Ru C73 C74 118.4(4) . . . . ? C71 Ru C73 C74 80.5(3) . . . . ? P2 Ru C73 C74 172.3(3) . . . . ? P3 Ru C73 C74 2.5(4) . . . . ? C72 C73 C74 C75 0.1(4) . . . . ? Ru C73 C74 C75 -63.2(2) . . . . ? C72 C73 C74 Ru 63.3(3) . . . . ? P1 Ru C74 C73 89.4(3) . . . . ? C75 Ru C74 C73 -115.5(4) . . . . ? C72 Ru C74 C73 -36.3(3) . . . . ? C71 Ru C74 C73 -78.6(3) . . . . ? P2 Ru C74 C73 -13.3(5) . . . . ? P3 Ru C74 C73 -178.5(2) . . . . ? C73 Ru C74 C75 115.5(4) . . . . ? P1 Ru C74 C75 -155.1(2) . . . . ? C72 Ru C74 C75 79.2(3) . . . . ? C71 Ru C74 C75 36.9(2) . . . . ? P2 Ru C74 C75 102.2(3) . . . . ? P3 Ru C74 C75 -63.0(3) . . . . ? C72 C71 C75 C74 0.6(4) . . . . ? Ru C71 C75 C74 63.1(2) . . . . ? C72 C71 C75 Ru -62.5(2) . . . . ? C73 C74 C75 C71 -0.4(4) . . . . ? Ru C74 C75 C71 -63.7(2) . . . . ? C73 C74 C75 Ru 63.3(3) . . . . ? C73 Ru C75 C71 79.7(3) . . . . ? P1 Ru C75 C71 149.3(2) . . . . ? C74 Ru C75 C71 117.5(3) . . . . ? C72 Ru C75 C71 38.2(2) . . . . ? P2 Ru C75 C71 -10.7(3) . . . . ? P3 Ru C75 C71 -118.9(2) . . . . ? C73 Ru C75 C74 -37.8(2) . . . . ? P1 Ru C75 C74 31.8(3) . . . . ? C72 Ru C75 C74 -79.3(3) . . . . ? C71 Ru C75 C74 -117.5(3) . . . . ? P2 Ru C75 C74 -128.2(3) . . . . ? P3 Ru C75 C74 123.7(2) . . . . ? O5 S C8 F3 -50.8(5) . . . . ? O4 S C8 F3 66.4(5) . . . . ? O6 S C8 F3 -175.1(5) . . . . ? O5 S C8 F2 -175.3(4) . . . . ? O4 S C8 F2 -58.1(5) . . . . ? O6 S C8 F2 60.4(5) . . . . ? O5 S C8 F1 68.0(5) . . . . ? O4 S C8 F1 -174.8(4) . . . . ? O6 S C8 F1 -56.3(5) . . . . ? data_Ruh3po3 _database_code_depnum_ccdc_archive 'CCDC 278842' #============================================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H38 O3 P3 Ru +, C F3 O3 S -, C H2 Cl2' _chemical_formula_sum 'C43 H40 Cl2 F3 O6 P3 Ru S' _chemical_formula_weight 1006.69 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 2 n n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' 'x+1/2, -y+1/2, z+1/2' 'x+1/2, y+1/2, -z+1/2' _cell_length_a 14.100(2) _cell_length_b 14.337(2) _cell_length_c 22.247(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4497.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2470 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 16.0 _exptl_crystal_description 'flat prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _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 2048 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details 'CrysAlisRED (Oxford Diffraction, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3 CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34879 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.19 _diffrn_reflns_theta_max 33.20 _diffrn_reflns_theta_full 33.20 _diffrn_measured_fraction_theta_max 0.901 _diffrn_measured_fraction_theta_full 0.901 _reflns_number_total 12107 _reflns_number_gt 6859 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrysAlisCCD (Oxford Diffraction, 2001)' _computing_cell_refinement 'CrysAlisCCD (Oxford Diffraction, 2001)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2001)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (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^)+(0.0680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(3) _refine_ls_number_reflns 12107 _refine_ls_number_parameters 486 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.727 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.065 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 Ru Ru 0.27723(3) 0.053489(18) -0.286722(11) 0.04479(9) Uani 1 1 d . . . P1 P 0.31358(9) -0.04064(7) -0.20292(4) 0.0468(2) Uani 1 1 d . . . P2 P 0.12680(8) -0.00464(7) -0.31282(4) 0.0461(2) Uani 1 1 d . . . P3 P 0.35406(9) -0.03057(8) -0.35788(5) 0.0522(3) Uani 1 1 d . . . O1 O 0.2919(3) -0.0538(2) -0.41474(12) 0.0669(9) Uani 1 1 d D . . H1O H 0.314(4) -0.084(4) -0.4433(16) 0.100 Uiso 1 1 d D . . O2 O 0.4448(3) 0.0208(2) -0.38712(16) 0.0770(10) Uani 1 1 d . . . H2O H 0.4335 0.0334 -0.4224 0.115 Uiso 1 1 calc R . . O3 O 0.4031(2) -0.1261(2) -0.33891(13) 0.0613(8) Uani 1 1 d D . . H3O H 0.420(4) -0.159(3) -0.3678(14) 0.092 Uiso 1 1 d D . . C11 C 0.44080(17) -0.0641(2) -0.18990(13) 0.0530(10) Uani 1 1 d G . . C12 C 0.4676(2) -0.12255(19) -0.14301(12) 0.0652(12) Uani 1 1 d G . . H12 H 0.4217 -0.1540 -0.1209 0.078 Uiso 1 1 calc R . . C13 C 0.5630(2) -0.1340(2) -0.12919(13) 0.0783(15) Uani 1 1 d G . . H13 H 0.5810 -0.1730 -0.0978 0.094 Uiso 1 1 calc R . . C14 C 0.63168(17) -0.0870(2) -0.16227(17) 0.0826(16) Uani 1 1 d G . . H14 H 0.6955 -0.0946 -0.1530 0.099 Uiso 1 1 calc R . . C15 C 0.6049(2) -0.0286(2) -0.20916(15) 0.0737(14) Uani 1 1 d G . . H15 H 0.6508 0.0029 -0.2313 0.088 Uiso 1 1 calc R . . C16 C 0.5094(2) -0.0172(2) -0.22297(12) 0.0653(12) Uani 1 1 d G . . H16 H 0.4915 0.0219 -0.2543 0.078 Uiso 1 1 calc R . . C21 C 0.2650(2) -0.15899(12) -0.18866(11) 0.0472(9) Uani 1 1 d G . . C22 C 0.30665(19) -0.23305(16) -0.21912(11) 0.0555(11) Uani 1 1 d G . . H22 H 0.3581 -0.2225 -0.2444 0.067 Uiso 1 1 calc R . . C23 C 0.2714(2) -0.32290(13) -0.21182(12) 0.0634(10) Uani 1 1 d G . . H23 H 0.2993 -0.3725 -0.2322 0.076 Uiso 1 1 calc R . . C24 C 0.1946(3) -0.33868(15) -0.17406(14) 0.0738(14) Uani 1 1 d G . . H24 H 0.1710 -0.3988 -0.1692 0.089 Uiso 1 1 calc R . . C25 C 0.1529(2) -0.2646(2) -0.14360(14) 0.0788(15) Uani 1 1 d G . . H25 H 0.1014 -0.2752 -0.1183 0.095 Uiso 1 1 calc R . . C26 C 0.1881(2) -0.17477(17) -0.15090(12) 0.0637(12) Uani 1 1 d G . . H26 H 0.1602 -0.1252 -0.1305 0.076 Uiso 1 1 calc R . . C31 C 0.2811(2) 0.02481(18) -0.13274(9) 0.0527(9) Uani 1 1 d G . . C32 C 0.3496(2) 0.0515(2) -0.09123(12) 0.0641(13) Uani 1 1 d G . . H32 H 0.4130 0.0364 -0.0977 0.077 Uiso 1 1 calc R . . C33 C 0.3235(3) 0.1006(2) -0.03999(11) 0.0775(16) Uani 1 1 d G . . H33 H 0.3693 0.1185 -0.0122 0.093 Uiso 1 1 calc R . . C34 C 0.2288(3) 0.1232(2) -0.03027(11) 0.0894(19) Uani 1 1 d G . . H34 H 0.2114 0.1561 0.0040 0.107 Uiso 1 1 calc R . . C35 C 0.1603(2) 0.0965(3) -0.07178(15) 0.0913(19) Uani 1 1 d G . . H35 H 0.0970 0.1116 -0.0653 0.110 Uiso 1 1 calc R . . C36 C 0.1865(2) 0.0473(2) -0.12302(12) 0.0699(14) Uani 1 1 d G . . H36 H 0.1406 0.0295 -0.1508 0.084 Uiso 1 1 calc R . . C41 C 0.1041(2) -0.12422(14) -0.33939(12) 0.0504(10) Uani 1 1 d G . . C42 C 0.01650(18) -0.14720(18) -0.36391(13) 0.0614(11) Uani 1 1 d G . . H42 H -0.0300 -0.1016 -0.3682 0.074 Uiso 1 1 calc R . . C43 C -0.0017(2) -0.2383(2) -0.38196(13) 0.0689(14) Uani 1 1 d G . . H43 H -0.0603 -0.2537 -0.3984 0.083 Uiso 1 1 calc R . . C44 C 0.0678(3) -0.30637(15) -0.37550(14) 0.0750(15) Uani 1 1 d G . . H44 H 0.0556 -0.3673 -0.3876 0.090 Uiso 1 1 calc R . . C45 C 0.1554(2) -0.28339(16) -0.35097(15) 0.0763(14) Uani 1 1 d G . . H45 H 0.2018 -0.3289 -0.3466 0.092 Uiso 1 1 calc R . . C46 C 0.17354(17) -0.19231(18) -0.33292(13) 0.0593(11) Uani 1 1 d G . . H46 H 0.2322 -0.1769 -0.3165 0.071 Uiso 1 1 calc R . . C51 C 0.0671(2) 0.06305(19) -0.37363(10) 0.0515(10) Uani 1 1 d G . . C52 C -0.02820(19) 0.0871(2) -0.37010(11) 0.0658(12) Uani 1 1 d G . . H52 H -0.0632 0.0718 -0.3361 0.079 Uiso 1 1 calc R . . C53 C -0.07127(18) 0.1341(3) -0.41744(14) 0.0803(16) Uani 1 1 d G . . H53 H -0.1351 0.1502 -0.4151 0.096 Uiso 1 1 calc R . . C54 C -0.0190(2) 0.1570(3) -0.46832(11) 0.0863(17) Uani 1 1 d G . . H54 H -0.0478 0.1885 -0.5000 0.104 Uiso 1 1 calc R . . C55 C 0.0763(2) 0.1330(2) -0.47185(11) 0.0804(16) Uani 1 1 d G . . H55 H 0.1113 0.1483 -0.5059 0.096 Uiso 1 1 calc R . . C56 C 0.11939(17) 0.0860(2) -0.42451(12) 0.0602(11) Uani 1 1 d G . . H56 H 0.1832 0.0699 -0.4269 0.072 Uiso 1 1 calc R . . C61 C 0.0389(2) 0.00256(19) -0.25072(12) 0.0514(10) Uani 1 1 d G . . C62 C 0.0029(3) -0.07775(16) -0.22420(14) 0.0695(14) Uani 1 1 d G . . H62 H 0.0202 -0.1361 -0.2388 0.083 Uiso 1 1 calc R . . C63 C -0.0590(3) -0.0709(2) -0.17580(15) 0.096(2) Uani 1 1 d G . . H63 H -0.0832 -0.1246 -0.1581 0.115 Uiso 1 1 calc R . . C64 C -0.0849(3) 0.0163(3) -0.15391(14) 0.0908(18) Uani 1 1 d G . . H64 H -0.1264 0.0209 -0.1215 0.109 Uiso 1 1 calc R . . C65 C -0.0489(3) 0.0966(2) -0.18043(14) 0.0732(14) Uani 1 1 d G . . H65 H -0.0662 0.1549 -0.1658 0.088 Uiso 1 1 calc R . . C66 C 0.0130(2) 0.08972(16) -0.22884(13) 0.0605(11) Uani 1 1 d G . . H66 H 0.0372 0.1435 -0.2466 0.073 Uiso 1 1 calc R . . C71 C 0.2452(3) 0.1869(2) -0.23698(13) 0.0692(15) Uani 1 1 d G . . H71 H 0.2064 0.1898 -0.2032 0.083 Uiso 1 1 calc R . . C72 C 0.2153(2) 0.1961(2) -0.29763(16) 0.0674(14) Uani 1 1 d G . . H72 H 0.1534 0.2062 -0.3106 0.081 Uiso 1 1 calc R . . C73 C 0.2964(3) 0.1873(2) -0.33503(10) 0.0710(15) Uani 1 1 d G . . H73 H 0.2970 0.1906 -0.3768 0.085 Uiso 1 1 calc R . . C74 C 0.3765(2) 0.1726(2) -0.29750(18) 0.0721(15) Uani 1 1 d G . . H74 H 0.4387 0.1646 -0.3103 0.086 Uiso 1 1 calc R . . C75 C 0.3448(3) 0.1723(2) -0.23690(14) 0.0721(15) Uani 1 1 d G . . H75 H 0.3827 0.1641 -0.2031 0.087 Uiso 1 1 calc R . . S S 0.42588(13) -0.22628(11) -0.49841(6) 0.0861(4) Uani 1 1 d . . . O4 O 0.4634(3) -0.2250(3) -0.43748(17) 0.1051(14) Uani 1 1 d D . . O5 O 0.3660(5) -0.1517(3) -0.50953(18) 0.159(3) Uani 1 1 d D . . O6 O 0.4926(6) -0.2489(9) -0.5434(3) 0.280(6) Uani 1 1 d . . . C1 C 0.3528(9) -0.3235(6) -0.5029(3) 0.138(4) Uani 1 1 d . . . F1 F 0.3128(4) -0.3369(3) -0.55555(17) 0.156(2) Uani 1 1 d . . . F2 F 0.2866(9) -0.3179(8) -0.4607(3) 0.279(5) Uani 1 1 d . . . F3 F 0.3907(9) -0.3976(4) -0.4886(4) 0.280(6) Uani 1 1 d . . . C2 C -0.3319(15) -0.123(3) -0.4246(9) 0.137(12) Uani 0.302(10) 1 d PDU A 1 H76 H -0.3763 -0.0801 -0.4428 0.165 Uiso 0.302(10) 1 calc PR A 1 H77 H -0.3439 -0.1853 -0.4404 0.165 Uiso 0.302(10) 1 calc PR A 1 Cl1 Cl -0.2173(11) -0.0900(18) -0.4387(11) 0.285(12) Uani 0.302(10) 1 d PDU A 1 Cl2 Cl -0.3426(10) -0.1223(7) -0.3480(4) 0.161(6) Uani 0.302(10) 1 d PDU A 1 C3 C -0.3289(18) -0.093(3) -0.4114(9) 0.332(19) Uani 0.698(10) 1 d PDU A 2 H78 H -0.3832 -0.1330 -0.4051 0.399 Uiso 0.698(10) 1 calc PR A 2 H79 H -0.3517 -0.0287 -0.4130 0.399 Uiso 0.698(10) 1 calc PR A 2 Cl3 Cl -0.2500(7) -0.1047(4) -0.3508(4) 0.269(4) Uani 0.698(10) 1 d PDU A 2 Cl4 Cl -0.2786(14) -0.1189(7) -0.4757(5) 0.398(9) Uani 0.698(10) 1 d PDU A 2 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 Ru 0.05582(17) 0.03912(13) 0.03944(13) 0.00126(11) 0.00128(17) 0.00045(18) P1 0.0546(6) 0.0432(5) 0.0425(5) -0.0004(4) -0.0016(4) 0.0025(4) P2 0.0533(6) 0.0471(5) 0.0379(5) 0.0010(4) 0.0009(5) 0.0038(5) P3 0.0603(7) 0.0528(5) 0.0436(5) 0.0032(5) 0.0110(5) 0.0039(5) O1 0.079(3) 0.0763(18) 0.0454(14) -0.0067(13) 0.0025(18) 0.0159(18) O2 0.077(2) 0.083(2) 0.071(2) 0.0080(18) 0.0234(19) -0.0053(19) O3 0.068(2) 0.065(2) 0.0501(16) 0.0056(14) 0.0078(15) 0.0113(16) C11 0.057(3) 0.048(2) 0.055(2) -0.0055(18) -0.004(2) -0.0021(19) C12 0.064(3) 0.063(3) 0.069(3) 0.012(2) -0.010(2) 0.007(2) C13 0.083(4) 0.062(3) 0.090(4) 0.016(3) -0.025(3) 0.006(3) C14 0.065(3) 0.074(3) 0.109(4) -0.016(3) -0.018(3) -0.002(3) C15 0.058(3) 0.065(3) 0.098(4) 0.000(3) 0.003(3) 0.001(3) C16 0.061(3) 0.059(3) 0.077(3) 0.000(2) 0.004(2) -0.002(2) C21 0.055(3) 0.0474(18) 0.0390(15) 0.0039(14) 0.0031(19) -0.0003(19) C22 0.062(3) 0.050(2) 0.055(2) 0.0042(18) 0.006(2) 0.0023(18) C23 0.068(3) 0.0495(19) 0.073(2) 0.0035(19) 0.002(3) 0.004(3) C24 0.083(4) 0.062(3) 0.076(3) 0.011(2) 0.002(3) -0.016(3) C25 0.086(4) 0.076(3) 0.074(3) 0.012(3) 0.025(3) -0.011(3) C26 0.069(3) 0.067(3) 0.055(2) 0.003(2) 0.010(2) 0.004(2) C31 0.064(3) 0.063(2) 0.0303(15) -0.0098(14) 0.005(2) -0.004(3) C32 0.083(4) 0.055(2) 0.054(2) 0.000(2) -0.006(3) -0.014(2) C33 0.121(5) 0.068(3) 0.044(2) -0.005(2) 0.000(3) -0.016(3) C34 0.148(6) 0.068(3) 0.052(3) -0.008(2) 0.022(3) 0.005(4) C35 0.118(5) 0.102(4) 0.055(3) -0.012(3) 0.007(3) 0.036(4) C36 0.076(4) 0.082(3) 0.051(2) -0.010(2) 0.003(2) 0.020(3) C41 0.063(3) 0.049(2) 0.040(2) 0.0067(17) 0.0059(19) -0.006(2) C42 0.064(3) 0.063(3) 0.057(2) 0.007(2) -0.008(2) -0.007(2) C43 0.080(4) 0.079(3) 0.047(2) -0.001(2) -0.011(2) -0.025(3) C44 0.101(4) 0.061(3) 0.063(3) -0.004(2) -0.006(3) -0.019(3) C45 0.078(4) 0.050(2) 0.101(4) -0.009(3) -0.011(3) 0.003(2) C46 0.064(3) 0.052(2) 0.062(2) 0.001(2) 0.003(2) 0.001(2) C51 0.064(3) 0.047(2) 0.043(2) -0.0030(17) -0.0033(19) 0.0099(19) C52 0.064(3) 0.084(3) 0.050(2) 0.013(2) 0.003(2) 0.007(3) C53 0.069(3) 0.113(4) 0.059(3) 0.013(3) -0.002(2) 0.027(3) C54 0.096(4) 0.110(4) 0.053(3) 0.021(3) -0.008(3) 0.022(4) C55 0.095(4) 0.091(4) 0.055(3) 0.020(3) 0.007(3) 0.016(3) C56 0.065(3) 0.066(3) 0.050(2) 0.003(2) 0.002(2) 0.004(2) C61 0.051(3) 0.054(2) 0.049(2) -0.002(2) -0.0014(19) 0.005(2) C62 0.086(4) 0.073(3) 0.049(2) -0.001(2) 0.018(2) 0.001(3) C63 0.111(5) 0.098(4) 0.079(4) -0.015(3) 0.027(4) -0.024(4) C64 0.092(4) 0.112(5) 0.068(3) -0.013(3) 0.022(3) -0.011(4) C65 0.079(4) 0.072(3) 0.069(3) -0.013(3) 0.004(3) 0.013(3) C66 0.072(3) 0.054(2) 0.055(2) 0.002(2) 0.001(2) 0.011(2) C71 0.113(5) 0.036(2) 0.058(3) -0.0067(19) 0.000(3) 0.002(2) C72 0.089(4) 0.036(2) 0.076(3) 0.006(2) -0.011(3) 0.009(2) C73 0.112(5) 0.0393(19) 0.062(2) 0.0042(18) 0.008(3) -0.008(2) C74 0.082(4) 0.049(3) 0.085(4) 0.000(2) 0.005(3) -0.017(3) C75 0.101(4) 0.044(2) 0.071(3) -0.009(2) -0.022(3) -0.013(3) S 0.1091(12) 0.0964(10) 0.0527(6) -0.0060(7) 0.0130(7) 0.0194(9) O4 0.119(4) 0.118(3) 0.079(2) -0.020(2) -0.014(2) 0.043(3) O5 0.290(8) 0.100(3) 0.088(3) -0.022(3) -0.066(4) 0.099(4) O6 0.181(7) 0.529(17) 0.129(5) -0.137(7) 0.090(5) -0.077(9) C1 0.247(11) 0.105(5) 0.061(4) 0.015(4) -0.013(5) -0.036(7) F1 0.245(7) 0.133(3) 0.092(2) 0.018(2) -0.051(3) -0.037(4) F2 0.339(11) 0.356(12) 0.144(5) -0.015(6) 0.059(7) -0.214(10) F3 0.541(17) 0.090(3) 0.209(7) 0.027(4) -0.190(9) 0.021(6) C2 0.074(17) 0.26(3) 0.079(14) -0.067(19) -0.009(13) 0.030(19) Cl1 0.104(8) 0.35(2) 0.40(3) 0.04(2) -0.017(12) -0.059(12) Cl2 0.194(13) 0.152(7) 0.137(7) 0.021(5) -0.001(7) 0.063(7) C3 0.20(3) 0.49(4) 0.31(3) -0.20(3) 0.07(2) 0.02(3) Cl3 0.205(8) 0.176(4) 0.428(12) 0.103(6) 0.063(7) 0.046(5) Cl4 0.62(2) 0.268(9) 0.306(11) 0.039(8) 0.234(14) 0.004(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 Ru C73 2.216(3) . ? Ru C74 2.221(3) . ? Ru C72 2.237(3) . ? Ru C75 2.245(3) . ? Ru C71 2.255(3) . ? Ru P3 2.2654(11) . ? Ru P2 2.3517(13) . ? Ru P1 2.3578(11) . ? P1 C11 1.848(3) . ? P1 C21 1.857(2) . ? P1 C31 1.878(2) . ? P2 C41 1.841(2) . ? P2 C61 1.858(2) . ? P2 C51 1.866(2) . ? P3 O1 1.575(3) . ? P3 O3 1.590(3) . ? P3 O2 1.613(4) . ? O1 H1O 0.830(8) . ? O2 H2O 0.8200 . ? O3 H3O 0.834(8) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C32 H32 0.9300 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 C35 1.3900 . ? C34 H34 0.9300 . ? C35 C36 1.3900 . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C42 H42 0.9300 . ? C43 C44 1.3900 . ? C43 H43 0.9300 . ? C44 C45 1.3900 . ? C44 H44 0.9300 . ? C45 C46 1.3900 . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C52 H52 0.9300 . ? C53 C54 1.3900 . ? C53 H53 0.9300 . ? C54 C55 1.3900 . ? C54 H54 0.9300 . ? C55 C56 1.3900 . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C62 H62 0.9300 . ? C63 C64 1.3900 . ? C63 H63 0.9300 . ? C64 C65 1.3900 . ? C64 H64 0.9300 . ? C65 C66 1.3900 . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C71 C72 1.4200 . ? C71 C75 1.4200 . ? C71 H71 0.9300 . ? C72 C73 1.4200 . ? C72 H72 0.9300 . ? C73 C74 1.4200 . ? C73 H73 0.9300 . ? C74 C75 1.4200 . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? S O5 1.385(5) . ? S O6 1.410(6) . ? S O4 1.455(4) . ? S C1 1.736(9) . ? C1 F3 1.231(11) . ? C1 F1 1.314(8) . ? C1 F2 1.326(13) . ? C2 Cl2 1.710(18) . ? C2 Cl1 1.713(19) . ? C2 H76 0.9700 . ? C2 H77 0.9700 . ? C3 Cl4 1.640(18) . ? C3 Cl3 1.757(19) . ? C3 H78 0.9700 . ? C3 H79 0.9700 . ? 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 C73 Ru C74 37.3 . . ? C73 Ru C72 37.2 . . ? C74 Ru C72 62.05(5) . . ? C73 Ru C75 62.00(6) . . ? C74 Ru C75 37.1 . . ? C72 Ru C75 61.68(5) . . ? C73 Ru C71 61.85(5) . . ? C74 Ru C71 61.77(5) . . ? C72 Ru C71 36.9 . . ? C75 Ru C71 36.8 . . ? C73 Ru P3 93.64(9) . . ? C74 Ru P3 91.86(9) . . ? C72 Ru P3 126.68(10) . . ? C75 Ru P3 123.07(12) . . ? C71 Ru P3 152.85(8) . . ? C73 Ru P2 107.29(11) . . ? C74 Ru P2 144.50(10) . . ? C72 Ru P2 86.84(8) . . ? C75 Ru P2 140.70(11) . . ? C71 Ru P2 103.95(11) . . ? P3 Ru P2 94.03(4) . . ? C73 Ru P1 148.50(9) . . ? C74 Ru P1 112.87(11) . . ? C72 Ru P1 133.94(10) . . ? C75 Ru P1 87.23(8) . . ? C71 Ru P1 98.09(9) . . ? P3 Ru P1 98.28(4) . . ? P2 Ru P1 100.86(4) . . ? C11 P1 C21 99.49(14) . . ? C11 P1 C31 101.37(14) . . ? C21 P1 C31 102.97(12) . . ? C11 P1 Ru 116.06(10) . . ? C21 P1 Ru 125.29(10) . . ? C31 P1 Ru 108.57(10) . . ? C41 P2 C61 100.05(13) . . ? C41 P2 C51 99.97(13) . . ? C61 P2 C51 102.10(14) . . ? C41 P2 Ru 124.47(10) . . ? C61 P2 Ru 113.45(11) . . ? C51 P2 Ru 113.67(10) . . ? O1 P3 O3 105.83(17) . . ? O1 P3 O2 102.35(19) . . ? O3 P3 O2 98.95(19) . . ? O1 P3 Ru 114.07(14) . . ? O3 P3 Ru 118.71(11) . . ? O2 P3 Ru 114.72(14) . . ? P3 O1 H1O 121(4) . . ? P3 O2 H2O 109.5 . . ? P3 O3 H3O 114(4) . . ? C12 C11 C16 120.0 . . ? C12 C11 P1 119.43(17) . . ? C16 C11 P1 120.30(17) . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C22 C21 C26 120.0 . . ? C22 C21 P1 117.29(15) . . ? C26 C21 P1 122.67(15) . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 P1 121.36(17) . . ? C36 C31 P1 118.64(17) . . ? C31 C32 C33 120.0 . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 P2 120.08(15) . . ? C46 C41 P2 119.88(15) . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 P2 121.62(16) . . ? C56 C51 P2 118.32(16) . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C56 C55 C54 120.0 . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 P2 120.88(16) . . ? C66 C61 P2 119.04(16) . . ? C63 C62 C61 120.0 . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? C72 C71 C75 108.0 . . ? C72 C71 Ru 70.88(11) . . ? C75 C71 Ru 71.24(13) . . ? C72 C71 H71 126.0 . . ? C75 C71 H71 126.0 . . ? Ru C71 H71 123.5 . . ? C73 C72 C71 108.0 . . ? C73 C72 Ru 70.60(12) . . ? C71 C72 Ru 72.26(10) . . ? C73 C72 H72 126.0 . . ? C71 C72 H72 126.0 . . ? Ru C72 H72 122.8 . . ? C74 C73 C72 108.0 . . ? C74 C73 Ru 71.54(13) . . ? C72 C73 Ru 72.21(13) . . ? C74 C73 H73 126.0 . . ? C72 C73 H73 126.0 . . ? Ru C73 H73 122.0 . . ? C73 C74 C75 108.0 . . ? C73 C74 Ru 71.13(12) . . ? C75 C74 Ru 72.39(11) . . ? C73 C74 H74 126.0 . . ? C75 C74 H74 126.0 . . ? Ru C74 H74 122.2 . . ? C74 C75 C71 108.0 . . ? C74 C75 Ru 70.54(11) . . ? C71 C75 Ru 71.97(13) . . ? C74 C75 H75 126.0 . . ? C71 C75 H75 126.0 . . ? Ru C75 H75 123.1 . . ? O5 S O6 117.2(6) . . ? O5 S O4 112.2(2) . . ? O6 S O4 114.9(4) . . ? O5 S C1 104.3(5) . . ? O6 S C1 99.8(6) . . ? O4 S C1 106.2(3) . . ? F3 C1 F1 106.8(7) . . ? F3 C1 F2 100.0(9) . . ? F1 C1 F2 109.8(11) . . ? F3 C1 S 114.8(10) . . ? F1 C1 S 115.1(5) . . ? F2 C1 S 109.2(6) . . ? Cl2 C2 Cl1 105.3(13) . . ? Cl2 C2 H76 110.7 . . ? Cl1 C2 H76 110.7 . . ? Cl2 C2 H77 110.7 . . ? Cl1 C2 H77 110.7 . . ? H76 C2 H77 108.8 . . ? Cl4 C3 Cl3 111.9(14) . . ? Cl4 C3 H78 109.2 . . ? Cl3 C3 H78 109.2 . . ? Cl4 C3 H79 109.2 . . ? Cl3 C3 H79 109.2 . . ? H78 C3 H79 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C73 Ru P1 C11 -56.5(2) . . . . ? C74 Ru P1 C11 -40.96(15) . . . . ? C72 Ru P1 C11 -113.50(17) . . . . ? C75 Ru P1 C11 -68.43(16) . . . . ? C71 Ru P1 C11 -103.67(15) . . . . ? P3 Ru P1 C11 54.60(12) . . . . ? P2 Ru P1 C11 150.35(12) . . . . ? C73 Ru P1 C21 178.7(2) . . . . ? C74 Ru P1 C21 -165.78(14) . . . . ? C72 Ru P1 C21 121.68(16) . . . . ? C75 Ru P1 C21 166.75(16) . . . . ? C71 Ru P1 C21 131.51(15) . . . . ? P3 Ru P1 C21 -70.22(12) . . . . ? P2 Ru P1 C21 25.53(12) . . . . ? C73 Ru P1 C31 56.8(2) . . . . ? C74 Ru P1 C31 72.36(15) . . . . ? C72 Ru P1 C31 -0.18(18) . . . . ? C75 Ru P1 C31 44.89(16) . . . . ? C71 Ru P1 C31 9.65(15) . . . . ? P3 Ru P1 C31 167.92(11) . . . . ? P2 Ru P1 C31 -96.33(12) . . . . ? C73 Ru P2 C41 129.76(14) . . . . ? C74 Ru P2 C41 133.59(19) . . . . ? C72 Ru P2 C41 161.25(15) . . . . ? C75 Ru P2 C41 -163.57(16) . . . . ? C71 Ru P2 C41 -165.82(14) . . . . ? P3 Ru P2 C41 34.68(12) . . . . ? P1 Ru P2 C41 -64.55(12) . . . . ? C73 Ru P2 C61 -108.33(13) . . . . ? C74 Ru P2 C61 -104.51(18) . . . . ? C72 Ru P2 C61 -76.84(14) . . . . ? C75 Ru P2 C61 -41.67(17) . . . . ? C71 Ru P2 C61 -43.92(13) . . . . ? P3 Ru P2 C61 156.59(11) . . . . ? P1 Ru P2 C61 57.35(11) . . . . ? C73 Ru P2 C51 7.75(13) . . . . ? C74 Ru P2 C51 11.57(19) . . . . ? C72 Ru P2 C51 39.24(14) . . . . ? C75 Ru P2 C51 74.41(17) . . . . ? C71 Ru P2 C51 72.16(13) . . . . ? P3 Ru P2 C51 -87.33(11) . . . . ? P1 Ru P2 C51 173.43(10) . . . . ? C73 Ru P3 O1 -79.60(17) . . . . ? C74 Ru P3 O1 -116.93(17) . . . . ? C72 Ru P3 O1 -61.03(18) . . . . ? C75 Ru P3 O1 -138.27(16) . . . . ? C71 Ru P3 O1 -103.8(3) . . . . ? P2 Ru P3 O1 28.03(14) . . . . ? P1 Ru P3 O1 129.64(14) . . . . ? C73 Ru P3 O3 154.58(19) . . . . ? C74 Ru P3 O3 117.25(19) . . . . ? C72 Ru P3 O3 173.15(18) . . . . ? C75 Ru P3 O3 95.92(18) . . . . ? C71 Ru P3 O3 130.4(3) . . . . ? P2 Ru P3 O3 -97.78(16) . . . . ? P1 Ru P3 O3 3.82(17) . . . . ? C73 Ru P3 O2 38.01(19) . . . . ? C74 Ru P3 O2 0.67(19) . . . . ? C72 Ru P3 O2 56.6(2) . . . . ? C75 Ru P3 O2 -20.66(19) . . . . ? C71 Ru P3 O2 13.8(3) . . . . ? P2 Ru P3 O2 145.64(16) . . . . ? P1 Ru P3 O2 -112.75(16) . . . . ? C21 P1 C11 C12 -39.88(19) . . . . ? C31 P1 C11 C12 65.54(19) . . . . ? Ru P1 C11 C12 -177.08(13) . . . . ? C21 P1 C11 C16 146.12(17) . . . . ? C31 P1 C11 C16 -108.46(18) . . . . ? Ru P1 C11 C16 8.9(2) . . . . ? C16 C11 C12 C13 0.0 . . . . ? P1 C11 C12 C13 -174.0(2) . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C11 0.0 . . . . ? C12 C11 C16 C15 0.0 . . . . ? P1 C11 C16 C15 174.0(2) . . . . ? C11 P1 C21 C22 -51.22(19) . . . . ? C31 P1 C21 C22 -155.33(17) . . . . ? Ru P1 C21 C22 80.38(18) . . . . ? C11 P1 C21 C26 130.90(18) . . . . ? C31 P1 C21 C26 26.8(2) . . . . ? Ru P1 C21 C26 -97.49(17) . . . . ? C26 C21 C22 C23 0.0 . . . . ? P1 C21 C22 C23 -177.9(2) . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C21 0.0 . . . . ? C22 C21 C26 C25 0.0 . . . . ? P1 C21 C26 C25 177.8(2) . . . . ? C11 P1 C31 C32 6.8(2) . . . . ? C21 P1 C31 C32 109.46(19) . . . . ? Ru P1 C31 C32 -115.89(16) . . . . ? C11 P1 C31 C36 -173.80(17) . . . . ? C21 P1 C31 C36 -71.15(19) . . . . ? Ru P1 C31 C36 63.50(17) . . . . ? C36 C31 C32 C33 0.0 . . . . ? P1 C31 C32 C33 179.4(2) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? P1 C31 C36 C35 -179.4(2) . . . . ? C61 P2 C41 C42 63.90(18) . . . . ? C51 P2 C41 C42 -40.42(18) . . . . ? Ru P2 C41 C42 -168.37(12) . . . . ? C61 P2 C41 C46 -113.81(18) . . . . ? C51 P2 C41 C46 141.88(17) . . . . ? Ru P2 C41 C46 13.9(2) . . . . ? C46 C41 C42 C43 0.0 . . . . ? P2 C41 C42 C43 -177.7(2) . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C41 0.0 . . . . ? C42 C41 C46 C45 0.0 . . . . ? P2 C41 C46 C45 177.7(2) . . . . ? C41 P2 C51 C52 89.4(2) . . . . ? C61 P2 C51 C52 -13.3(2) . . . . ? Ru P2 C51 C52 -135.87(16) . . . . ? C41 P2 C51 C56 -87.9(2) . . . . ? C61 P2 C51 C56 169.43(18) . . . . ? Ru P2 C51 C56 46.86(19) . . . . ? C56 C51 C52 C53 0.0 . . . . ? P2 C51 C52 C53 -177.2(2) . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C51 0.0 . . . . ? C52 C51 C56 C55 0.0 . . . . ? P2 C51 C56 C55 177.3(2) . . . . ? C41 P2 C61 C62 21.2(2) . . . . ? C51 P2 C61 C62 123.8(2) . . . . ? Ru P2 C61 C62 -113.53(18) . . . . ? C41 P2 C61 C66 -162.08(18) . . . . ? C51 P2 C61 C66 -59.5(2) . . . . ? Ru P2 C61 C66 63.22(19) . . . . ? C66 C61 C62 C63 0.0 . . . . ? P2 C61 C62 C63 176.7(2) . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C66 0.0 . . . . ? C64 C65 C66 C61 0.0 . . . . ? C62 C61 C66 C65 0.0 . . . . ? P2 C61 C66 C65 -176.8(2) . . . . ? C73 Ru C71 C72 37.6 . . . . ? C74 Ru C71 C72 80.17(6) . . . . ? C75 Ru C71 C72 117.59(6) . . . . ? P3 Ru C71 C72 65.2(3) . . . . ? P2 Ru C71 C72 -64.79(13) . . . . ? P1 Ru C71 C72 -168.17(14) . . . . ? C73 Ru C71 C75 -80.01(8) . . . . ? C74 Ru C71 C75 -37.42(5) . . . . ? C72 Ru C71 C75 -117.59(6) . . . . ? P3 Ru C71 C75 -52.4(3) . . . . ? P2 Ru C71 C75 177.62(14) . . . . ? P1 Ru C71 C75 74.24(14) . . . . ? C75 C71 C72 C73 0.0 . . . . ? Ru C71 C72 C73 -61.93(13) . . . . ? C75 C71 C72 Ru 61.93(13) . . . . ? C74 Ru C72 C73 37.8 . . . . ? C75 Ru C72 C73 80.09(8) . . . . ? C71 Ru C72 C73 117.17(7) . . . . ? P3 Ru C72 C73 -31.72(16) . . . . ? P2 Ru C72 C73 -124.40(15) . . . . ? P1 Ru C72 C73 133.54(19) . . . . ? C73 Ru C72 C71 -117.17(7) . . . . ? C74 Ru C72 C71 -79.34(7) . . . . ? C75 Ru C72 C71 -37.1 . . . . ? P3 Ru C72 C71 -148.89(16) . . . . ? P2 Ru C72 C71 118.43(15) . . . . ? P1 Ru C72 C71 16.37(18) . . . . ? C71 C72 C73 C74 0.0 . . . . ? Ru C72 C73 C74 -63.00(11) . . . . ? C71 C72 C73 Ru 63.00(11) . . . . ? C72 Ru C73 C74 116.70(5) . . . . ? C75 Ru C73 C74 37.54(5) . . . . ? C71 Ru C73 C74 79.45(7) . . . . ? P3 Ru C73 C74 -88.30(14) . . . . ? P2 Ru C73 C74 176.34(14) . . . . ? P1 Ru C73 C74 24.0(3) . . . . ? C74 Ru C73 C72 -116.70(5) . . . . ? C75 Ru C73 C72 -79.16(7) . . . . ? C71 Ru C73 C72 -37.25(5) . . . . ? P3 Ru C73 C72 155.00(14) . . . . ? P2 Ru C73 C72 59.64(14) . . . . ? P1 Ru C73 C72 -92.7(3) . . . . ? C72 C73 C74 C75 0.0 . . . . ? Ru C73 C74 C75 -63.43(11) . . . . ? C72 C73 C74 Ru 63.43(11) . . . . ? C72 Ru C74 C73 -37.7 . . . . ? C75 Ru C74 C73 -116.82(7) . . . . ? C71 Ru C74 C73 -79.68(7) . . . . ? P3 Ru C74 C73 93.56(14) . . . . ? P2 Ru C74 C73 -6.0(2) . . . . ? P1 Ru C74 C73 -166.65(13) . . . . ? C73 Ru C74 C75 116.82(7) . . . . ? C72 Ru C74 C75 79.13(7) . . . . ? C71 Ru C74 C75 37.1 . . . . ? P3 Ru C74 C75 -149.62(14) . . . . ? P2 Ru C74 C75 110.8(2) . . . . ? P1 Ru C74 C75 -49.83(13) . . . . ? C73 C74 C75 C71 0.0 . . . . ? Ru C74 C75 C71 -62.62(13) . . . . ? C73 C74 C75 Ru 62.62(13) . . . . ? C72 C71 C75 C74 0.0 . . . . ? Ru C71 C75 C74 61.70(10) . . . . ? C72 C71 C75 Ru -61.70(10) . . . . ? C73 Ru C75 C74 -37.8 . . . . ? C72 Ru C75 C74 -80.21(6) . . . . ? C71 Ru C75 C74 -117.36(6) . . . . ? P3 Ru C75 C74 37.09(14) . . . . ? P2 Ru C75 C74 -121.0(2) . . . . ? P1 Ru C75 C74 135.18(14) . . . . ? C73 Ru C75 C71 79.56(8) . . . . ? C74 Ru C75 C71 117.36(6) . . . . ? C72 Ru C75 C71 37.15(5) . . . . ? P3 Ru C75 C71 154.46(14) . . . . ? P2 Ru C75 C71 -3.6(2) . . . . ? P1 Ru C75 C71 -107.46(14) . . . . ? O5 S C1 F3 -173.3(8) . . . . ? O6 S C1 F3 65.1(9) . . . . ? O4 S C1 F3 -54.6(9) . . . . ? O5 S C1 F1 62.0(9) . . . . ? O6 S C1 F1 -59.5(10) . . . . ? O4 S C1 F1 -179.2(8) . . . . ? O5 S C1 F2 -62.0(9) . . . . ? O6 S C1 F2 176.5(9) . . . . ? O4 S C1 F2 56.7(10) . . . . ? data_RuPFO2 _database_code_depnum_ccdc_archive 'CCDC 278843' #============================================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H37 F O2 P3 Ru +, F2 O2 P -, C6 H14 ' _chemical_formula_sum 'C47 H51 F3 O4 P4 Ru' _chemical_formula_weight 961.83 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 13.666(3) _cell_length_b 22.517(4) _cell_length_c 14.244(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.91(2) _cell_angle_gamma 90.00 _cell_volume 4380.7(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3540 _cell_measurement_theta_min 4.3 _cell_measurement_theta_max 18.0 _exptl_crystal_description 'flat prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 0.560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.678 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1986)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3 CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37004 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.25 _diffrn_reflns_theta_max 34.43 _diffrn_reflns_theta_full 34.43 _diffrn_measured_fraction_theta_max 0.734 _diffrn_measured_fraction_theta_full 0.734 _reflns_number_total 13561 _reflns_number_gt 6467 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrysAlisCCD (Oxford Diffraction, 2001)' _computing_cell_refinement 'CrysAlisCCD (Oxford Diffraction, 2001)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2001)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (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^)+(0.1440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13561 _refine_ls_number_parameters 643 _refine_ls_number_restraints 146 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.2331 _refine_ls_wR_factor_gt 0.2060 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.227 _refine_diff_density_min -1.189 _refine_diff_density_rms 0.114 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 Ru Ru 0.37167(2) 0.283283(14) 0.80062(2) 0.04451(11) Uani 1 1 d . . . P1 P 0.39790(8) 0.19823(5) 0.70847(7) 0.0457(2) Uani 1 1 d . . . P2 P 0.21646(8) 0.31533(5) 0.74457(7) 0.0461(2) Uani 1 1 d . . . P3 P 0.45282(9) 0.34651(6) 0.70975(8) 0.0586(3) Uani 1 1 d . . . O1 O 0.4891(3) 0.32472(18) 0.6124(2) 0.0865(10) Uani 0.50 1 d PD . . H1O H 0.503(9) 0.356(3) 0.583(8) 0.130 Uiso 0.50 1 d PD . . F1 F 0.4891(3) 0.32472(18) 0.6124(2) 0.0865(10) Uani 0.50 1 d P . . O2 O 0.3987(3) 0.40587(15) 0.6842(3) 0.0901(11) Uani 0.50 1 d PD . . H2O H 0.407(9) 0.427(4) 0.635(5) 0.135 Uiso 0.50 1 d PD . . F2 F 0.3987(3) 0.40587(15) 0.6842(3) 0.0901(11) Uani 0.50 1 d P . . O3 O 0.5546(3) 0.36809(18) 0.7526(3) 0.0868(11) Uani 1 1 d D . . H3O H 0.541(4) 0.3978(9) 0.7892(17) 0.130 Uiso 1 1 d D . . C11 C 0.5274(3) 0.1835(2) 0.6853(3) 0.0502(9) Uani 1 1 d . . . C12 C 0.6027(3) 0.2154(2) 0.7284(3) 0.0581(11) Uani 1 1 d . . . H12 H 0.5880 0.2467 0.7681 0.070 Uiso 1 1 calc R . . C13 C 0.6999(4) 0.2014(3) 0.7133(4) 0.0722(14) Uani 1 1 d . . . H13 H 0.7492 0.2241 0.7418 0.087 Uiso 1 1 calc R . . C14 C 0.7243(4) 0.1548(3) 0.6573(3) 0.0728(14) Uani 1 1 d . . . H14 H 0.7896 0.1449 0.6493 0.087 Uiso 1 1 calc R . . C15 C 0.6503(4) 0.1225(3) 0.6127(4) 0.0812(16) Uani 1 1 d . . . H15 H 0.6660 0.0912 0.5734 0.097 Uiso 1 1 calc R . . C16 C 0.5532(3) 0.1363(2) 0.6259(3) 0.0649(12) Uani 1 1 d . . . H16 H 0.5043 0.1143 0.5952 0.078 Uiso 1 1 calc R . . C21 C 0.3630(3) 0.1310(2) 0.7735(3) 0.0511(9) Uani 1 1 d . . . C22 C 0.4253(3) 0.0840(2) 0.7943(3) 0.0601(11) Uani 1 1 d . . . H22 H 0.4900 0.0861 0.7764 0.072 Uiso 1 1 calc R . . C23 C 0.3943(4) 0.0351(2) 0.8403(4) 0.0729(13) Uani 1 1 d . . . H23 H 0.4380 0.0042 0.8528 0.087 Uiso 1 1 calc R . . C24 C 0.2989(4) 0.0302(2) 0.8691(4) 0.0729(14) Uani 1 1 d . . . H24 H 0.2785 -0.0032 0.9016 0.087 Uiso 1 1 calc R . . C25 C 0.2350(4) 0.0758(2) 0.8483(4) 0.0749(14) Uani 1 1 d . . . H25 H 0.1703 0.0732 0.8661 0.090 Uiso 1 1 calc R . . C26 C 0.2664(4) 0.1253(2) 0.8013(3) 0.0633(12) Uani 1 1 d . . . H26 H 0.2221 0.1557 0.7878 0.076 Uiso 1 1 calc R . . C31 C 0.3432(3) 0.1839(2) 0.5910(3) 0.0526(10) Uani 1 1 d . . . C32 C 0.3862(4) 0.2082(2) 0.5122(3) 0.0704(14) Uani 1 1 d . . . H32 H 0.4419 0.2317 0.5203 0.085 Uiso 1 1 calc R . . C33 C 0.3476(4) 0.1982(3) 0.4216(3) 0.0787(16) Uani 1 1 d . . . H33 H 0.3762 0.2157 0.3701 0.094 Uiso 1 1 calc R . . C34 C 0.2665(4) 0.1620(3) 0.4091(4) 0.0820(16) Uani 1 1 d . . . H34 H 0.2416 0.1537 0.3490 0.098 Uiso 1 1 calc R . . C35 C 0.2228(4) 0.1382(3) 0.4866(4) 0.0752(14) Uani 1 1 d . . . H35 H 0.1674 0.1146 0.4779 0.090 Uiso 1 1 calc R . . C36 C 0.2593(3) 0.1487(2) 0.5768(3) 0.0598(11) Uani 1 1 d . . . H36 H 0.2283 0.1325 0.6280 0.072 Uiso 1 1 calc R . . C41 C 0.1915(3) 0.34164(18) 0.6238(3) 0.0498(9) Uani 1 1 d . . . C42 C 0.1072(4) 0.3744(2) 0.6018(3) 0.0652(12) Uani 1 1 d . . . H42 H 0.0630 0.3830 0.6483 0.078 Uiso 1 1 calc R . . C43 C 0.0892(4) 0.3944(2) 0.5100(4) 0.0760(15) Uani 1 1 d . . . H43 H 0.0333 0.4166 0.4957 0.091 Uiso 1 1 calc R . . C44 C 0.1529(5) 0.3817(3) 0.4415(3) 0.0810(16) Uani 1 1 d . . . H44 H 0.1408 0.3950 0.3804 0.097 Uiso 1 1 calc R . . C45 C 0.2363(5) 0.3485(3) 0.4637(4) 0.097(2) Uani 1 1 d . . . H45 H 0.2805 0.3397 0.4174 0.117 Uiso 1 1 calc R . . C46 C 0.2536(4) 0.3288(3) 0.5540(3) 0.0779(15) Uani 1 1 d . . . H46 H 0.3091 0.3061 0.5678 0.093 Uiso 1 1 calc R . . C51 C 0.1205(3) 0.2587(2) 0.7584(3) 0.0520(9) Uani 1 1 d . . . C52 C 0.0758(3) 0.2320(2) 0.6816(3) 0.0616(11) Uani 1 1 d . . . H52 H 0.0907 0.2444 0.6214 0.074 Uiso 1 1 calc R . . C53 C 0.0076(4) 0.1860(3) 0.6933(5) 0.0884(17) Uani 1 1 d . . . H53 H -0.0234 0.1686 0.6412 0.106 Uiso 1 1 calc R . . C54 C -0.0130(4) 0.1671(3) 0.7818(5) 0.0870(17) Uani 1 1 d . . . H54 H -0.0563 0.1357 0.7897 0.104 Uiso 1 1 calc R . . C55 C 0.0302(4) 0.1942(3) 0.8592(4) 0.0728(14) Uani 1 1 d . . . H55 H 0.0143 0.1824 0.9193 0.087 Uiso 1 1 calc R . . C56 C 0.0971(4) 0.2391(2) 0.8471(3) 0.0636(12) Uani 1 1 d . . . H56 H 0.1273 0.2566 0.8996 0.076 Uiso 1 1 calc R . . C61 C 0.1696(3) 0.3791(2) 0.8117(3) 0.0557(10) Uani 1 1 d . . . C62 C 0.0713(4) 0.3826(2) 0.8353(3) 0.0695(13) Uani 1 1 d . . . H62 H 0.0285 0.3518 0.8196 0.083 Uiso 1 1 calc R . . C63 C 0.0377(5) 0.4325(3) 0.8826(4) 0.0856(17) Uani 1 1 d . . . H63 H -0.0275 0.4346 0.8992 0.103 Uiso 1 1 calc R . . C64 C 0.1001(6) 0.4784(3) 0.9047(4) 0.0888(18) Uani 1 1 d . . . H64 H 0.0772 0.5119 0.9353 0.107 Uiso 1 1 calc R . . C65 C 0.1959(5) 0.4748(2) 0.8818(4) 0.0848(17) Uani 1 1 d . . . H65 H 0.2383 0.5057 0.8978 0.102 Uiso 1 1 calc R . . C66 C 0.2309(4) 0.4259(2) 0.8352(3) 0.0670(12) Uani 1 1 d . . . H66 H 0.2964 0.4244 0.8194 0.080 Uiso 1 1 calc R . . C71 C 0.4403(4) 0.2322(2) 0.9210(3) 0.0611(11) Uani 1 1 d . . . H71 H 0.4721 0.1961 0.9131 0.073 Uiso 1 1 calc R . . C72 C 0.4835(4) 0.2886(2) 0.9179(3) 0.0629(12) Uani 1 1 d . . . H72 H 0.5491 0.2965 0.9080 0.075 Uiso 1 1 calc R . . C73 C 0.3225(4) 0.3020(2) 0.9452(3) 0.0646(12) Uani 1 1 d . . . H73 H 0.2625 0.3197 0.9564 0.077 Uiso 1 1 calc R . . C74 C 0.4096(4) 0.3317(2) 0.9326(3) 0.0661(13) Uani 1 1 d . . . H74 H 0.4182 0.3727 0.9335 0.079 Uiso 1 1 calc R . . C75 C 0.3395(4) 0.2400(2) 0.9384(3) 0.0624(12) Uani 1 1 d . . . H75 H 0.2932 0.2101 0.9442 0.075 Uiso 1 1 calc R . . P4 P 0.5000 0.5000 0.5000 0.1372(13) Uani 1 2 d SD . . O4 O 0.5128(8) 0.5069(4) 0.3976(5) 0.136(4) Uani 0.25 1 d PD . . F4 F 0.5128(8) 0.5069(4) 0.3976(5) 0.136(4) Uani 0.25 1 d P . . O5 O 0.5412(7) 0.4332(4) 0.5191(7) 0.149(4) Uani 0.25 1 d PDU . . F5 F 0.5412(7) 0.4332(4) 0.5191(7) 0.149(4) Uani 0.25 1 d P . . O6 O 0.3943(6) 0.4909(5) 0.5175(9) 0.183(6) Uani 0.25 1 d PD . . F6 F 0.3943(6) 0.4909(5) 0.5175(9) 0.183(6) Uani 0.25 1 d P . . O7 O 0.5541(12) 0.5378(6) 0.5609(11) 0.380(17) Uani 0.25 1 d PDU . . F7 F 0.5541(12) 0.5378(6) 0.5609(11) 0.380(17) Uani 0.25 1 d PU . . P5 P 0.5415(4) 0.50963(17) 0.8628(4) 0.152(2) Uani 0.50 1 d PD . . O8 O 0.6144(7) 0.5402(4) 0.9162(8) 0.191(6) Uani 0.25 1 d PD . . F8 F 0.6144(7) 0.5402(4) 0.9162(8) 0.191(6) Uani 0.25 1 d P . . O9 O 0.4441(6) 0.5326(5) 0.8826(12) 0.241(10) Uani 0.25 1 d PD . . F9 F 0.4441(6) 0.5326(5) 0.8826(12) 0.241(10) Uani 0.25 1 d P . . O10 O 0.5452(8) 0.4489(3) 0.8680(8) 0.171(5) Uani 0.25 1 d PD . . F10 F 0.5452(8) 0.4489(3) 0.8680(8) 0.171(5) Uani 0.25 1 d P . . O11 O 0.5555(15) 0.5281(6) 0.7647(7) 0.389(17) Uani 0.25 1 d PDU . . F11 F 0.5555(15) 0.5281(6) 0.7647(7) 0.389(17) Uani 0.25 1 d PU . . C101 C 0.8278(13) 0.3486(7) 0.6710(10) 0.063(4) Uani 0.336(8) 1 d PDU A 1 H101 H 0.8343 0.3093 0.6457 0.094 Uiso 0.336(8) 1 calc PR A 1 H102 H 0.7635 0.3533 0.6951 0.094 Uiso 0.336(8) 1 calc PR A 1 H103 H 0.8759 0.3545 0.7207 0.094 Uiso 0.336(8) 1 calc PR A 1 C102 C 0.8370(13) 0.3761(5) 0.6244(11) 0.076(4) Uani 0.336(8) 1 d PDU A 1 H104 H 0.7822 0.3650 0.5831 0.091 Uiso 0.336(8) 1 calc PR A 1 H105 H 0.8928 0.3577 0.5958 0.091 Uiso 0.336(8) 1 calc PR A 1 C103 C 0.8461(17) 0.4153(5) 0.6021(10) 0.112(4) Uani 0.336(8) 1 d PDU A 1 H106 H 0.7850 0.4228 0.5675 0.134 Uiso 0.336(8) 1 calc PR A 1 H107 H 0.8940 0.4096 0.5541 0.134 Uiso 0.336(8) 1 calc PR A 1 C104 C 0.8635(13) 0.4556(6) 0.6267(11) 0.093(4) Uani 0.336(8) 1 d PDU A 1 H108 H 0.9329 0.4598 0.6158 0.111 Uiso 0.336(8) 1 calc PR A 1 H109 H 0.8306 0.4830 0.5836 0.111 Uiso 0.336(8) 1 calc PR A 1 C105 C 0.8548(11) 0.4729(8) 0.6894(11) 0.068(4) Uani 0.336(8) 1 d PDU A 1 H110 H 0.8951 0.4485 0.7313 0.081 Uiso 0.336(8) 1 calc PR A 1 H111 H 0.8875 0.5111 0.6872 0.081 Uiso 0.336(8) 1 calc PR A 1 C106 C 0.7955(11) 0.4806(8) 0.7244(11) 0.070(4) Uani 0.336(8) 1 d PDU A 1 H112 H 0.7457 0.4526 0.7057 0.105 Uiso 0.336(8) 1 calc PR A 1 H113 H 0.7727 0.5202 0.7112 0.105 Uiso 0.336(8) 1 calc PR A 1 H114 H 0.8102 0.4767 0.7905 0.105 Uiso 0.336(8) 1 calc PR A 1 C111 C 0.8496(7) 0.3358(5) 0.6495(7) 0.081(3) Uani 0.664(8) 1 d PDU A 2 H115 H 0.8594 0.3050 0.6043 0.122 Uiso 0.664(8) 1 calc PR A 2 H116 H 0.8441 0.3186 0.7107 0.122 Uiso 0.664(8) 1 calc PR A 2 H117 H 0.9042 0.3626 0.6499 0.122 Uiso 0.664(8) 1 calc PR A 2 C112 C 0.7915(9) 0.3568(4) 0.6333(9) 0.113(4) Uani 0.664(8) 1 d PDU A 2 H118 H 0.7463 0.3425 0.6792 0.136 Uiso 0.664(8) 1 calc PR A 2 H119 H 0.7704 0.3382 0.5747 0.136 Uiso 0.664(8) 1 calc PR A 2 C113 C 0.7712(11) 0.3969(4) 0.6244(13) 0.189(6) Uani 0.664(8) 1 d PDU A 2 H120 H 0.7008 0.3923 0.6272 0.227 Uiso 0.664(8) 1 calc PR A 2 H121 H 0.7828 0.4016 0.5580 0.227 Uiso 0.664(8) 1 calc PR A 2 C114 C 0.7781(11) 0.4375(5) 0.6450(12) 0.206(6) Uani 0.664(8) 1 d PDU A 2 H122 H 0.7287 0.4414 0.6919 0.248 Uiso 0.664(8) 1 calc PR A 2 H123 H 0.7534 0.4602 0.5914 0.248 Uiso 0.664(8) 1 calc PR A 2 C115 C 0.8340(12) 0.4629(7) 0.6710(11) 0.168(6) Uani 0.664(8) 1 d PDU A 2 H124 H 0.8913 0.4377 0.6675 0.202 Uiso 0.664(8) 1 calc PR A 2 H125 H 0.8421 0.4936 0.6241 0.202 Uiso 0.664(8) 1 calc PR A 2 C116 C 0.8422(11) 0.4828(7) 0.7291(8) 0.126(5) Uani 0.664(8) 1 d PDU A 2 H126 H 0.9095 0.4802 0.7505 0.189 Uiso 0.664(8) 1 calc PR A 2 H127 H 0.8012 0.4648 0.7745 0.189 Uiso 0.664(8) 1 calc PR A 2 H128 H 0.8244 0.5238 0.7212 0.189 Uiso 0.664(8) 1 calc PR A 2 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 Ru 0.0490(2) 0.0474(2) 0.03709(16) 0.00192(12) -0.00021(13) -0.00258(13) P1 0.0445(5) 0.0528(6) 0.0397(5) -0.0011(4) 0.0015(4) -0.0033(4) P2 0.0497(5) 0.0492(6) 0.0395(5) 0.0017(4) 0.0014(4) 0.0023(4) P3 0.0609(7) 0.0594(7) 0.0557(6) 0.0087(5) 0.0040(5) -0.0118(5) O1 0.088(2) 0.106(3) 0.0667(19) 0.0158(18) 0.0275(17) -0.016(2) F1 0.088(2) 0.106(3) 0.0667(19) 0.0158(18) 0.0275(17) -0.016(2) O2 0.087(2) 0.076(2) 0.108(3) 0.0420(19) 0.012(2) -0.0006(18) F2 0.087(2) 0.076(2) 0.108(3) 0.0420(19) 0.012(2) -0.0006(18) O3 0.071(2) 0.084(3) 0.105(3) 0.017(2) -0.007(2) -0.027(2) C11 0.046(2) 0.064(3) 0.0402(18) 0.0010(18) 0.0008(16) -0.0022(19) C12 0.051(2) 0.068(3) 0.055(2) -0.001(2) 0.001(2) 0.000(2) C13 0.049(3) 0.101(4) 0.066(3) -0.006(3) -0.003(2) -0.009(3) C14 0.053(3) 0.105(4) 0.060(3) 0.004(3) 0.003(2) 0.001(3) C15 0.073(3) 0.109(4) 0.062(3) -0.019(3) 0.010(3) 0.013(3) C16 0.057(3) 0.072(3) 0.066(3) -0.019(2) 0.010(2) -0.003(2) C21 0.0376(19) 0.059(2) 0.056(2) 0.0098(19) 0.0041(16) -0.0001(17) C22 0.061(3) 0.061(3) 0.058(2) 0.001(2) -0.004(2) -0.009(2) C23 0.086(3) 0.058(3) 0.074(3) 0.008(2) -0.006(3) 0.007(3) C24 0.088(4) 0.056(3) 0.074(3) 0.012(2) 0.010(3) -0.010(3) C25 0.070(3) 0.070(3) 0.086(3) 0.015(3) 0.017(3) -0.007(3) C26 0.067(3) 0.054(3) 0.070(3) 0.010(2) 0.014(2) 0.004(2) C31 0.045(2) 0.062(3) 0.050(2) -0.0081(19) -0.0011(17) -0.0024(19) C32 0.058(3) 0.105(4) 0.048(2) 0.003(2) -0.003(2) -0.016(3) C33 0.068(3) 0.122(5) 0.045(2) -0.002(3) -0.001(2) -0.001(3) C34 0.075(3) 0.112(5) 0.058(3) -0.017(3) -0.018(3) 0.000(3) C35 0.061(3) 0.083(4) 0.080(3) -0.006(3) -0.018(3) -0.016(3) C36 0.052(2) 0.063(3) 0.064(3) -0.004(2) -0.002(2) -0.008(2) C41 0.054(2) 0.052(2) 0.0426(19) 0.0031(17) -0.0038(17) -0.0056(18) C42 0.079(3) 0.060(3) 0.056(2) -0.001(2) -0.006(2) 0.009(2) C43 0.100(4) 0.061(3) 0.064(3) -0.001(2) -0.031(3) 0.019(3) C44 0.106(4) 0.084(4) 0.051(2) 0.016(2) -0.024(3) -0.010(3) C45 0.082(4) 0.157(6) 0.053(3) 0.027(3) 0.001(3) 0.009(4) C46 0.060(3) 0.123(5) 0.049(2) 0.010(3) -0.003(2) 0.015(3) C51 0.041(2) 0.056(2) 0.059(2) 0.0034(19) 0.0062(17) 0.0041(18) C52 0.057(3) 0.064(3) 0.065(3) -0.003(2) 0.003(2) -0.007(2) C53 0.081(4) 0.092(4) 0.092(4) -0.001(3) -0.003(3) -0.025(3) C54 0.067(3) 0.087(4) 0.108(5) 0.005(3) 0.024(3) -0.019(3) C55 0.057(3) 0.085(3) 0.078(3) 0.014(3) 0.023(3) -0.001(3) C56 0.065(3) 0.068(3) 0.058(3) -0.001(2) 0.009(2) -0.001(2) C61 0.070(3) 0.052(2) 0.045(2) 0.0030(18) -0.0003(19) 0.009(2) C62 0.074(3) 0.075(3) 0.060(3) -0.008(2) -0.001(2) 0.020(3) C63 0.105(4) 0.089(4) 0.063(3) 0.001(3) 0.013(3) 0.039(4) C64 0.136(5) 0.063(3) 0.069(3) 0.000(3) 0.016(3) 0.040(4) C65 0.128(5) 0.049(3) 0.076(3) -0.001(2) -0.003(3) 0.004(3) C66 0.089(3) 0.055(3) 0.056(2) 0.001(2) -0.002(2) 0.010(2) C71 0.081(3) 0.061(3) 0.041(2) 0.0013(19) -0.015(2) 0.010(2) C72 0.056(3) 0.090(4) 0.041(2) 0.000(2) -0.0118(19) -0.006(2) C73 0.079(3) 0.079(3) 0.0357(19) 0.000(2) 0.000(2) 0.021(3) C74 0.100(4) 0.052(2) 0.044(2) -0.0098(18) -0.014(2) 0.003(3) C75 0.075(3) 0.074(3) 0.038(2) 0.008(2) 0.005(2) -0.006(3) P4 0.115(2) 0.178(3) 0.122(2) 0.073(2) 0.0496(19) 0.021(2) O4 0.176(10) 0.111(7) 0.125(7) 0.050(6) 0.052(7) 0.017(7) F4 0.176(10) 0.111(7) 0.125(7) 0.050(6) 0.052(7) 0.017(7) O5 0.191(10) 0.124(8) 0.133(8) 0.062(6) 0.038(7) 0.046(7) F5 0.191(10) 0.124(8) 0.133(8) 0.062(6) 0.038(7) 0.046(7) O6 0.130(9) 0.188(12) 0.236(15) -0.054(11) 0.087(10) -0.012(8) F6 0.130(9) 0.188(12) 0.236(15) -0.054(11) 0.087(10) -0.012(8) O7 0.49(4) 0.31(3) 0.34(3) -0.18(2) -0.09(3) -0.06(3) F7 0.49(4) 0.31(3) 0.34(3) -0.18(2) -0.09(3) -0.06(3) P5 0.211(6) 0.057(2) 0.184(5) 0.002(3) -0.054(4) -0.021(3) O8 0.233(12) 0.135(9) 0.201(12) -0.024(8) -0.037(10) -0.123(9) F8 0.233(12) 0.135(9) 0.201(12) -0.024(8) -0.037(10) -0.123(9) O9 0.083(7) 0.138(11) 0.50(3) -0.046(14) -0.017(11) 0.026(7) F9 0.083(7) 0.138(11) 0.50(3) -0.046(14) -0.017(11) 0.026(7) O10 0.212(10) 0.066(5) 0.226(12) 0.006(6) -0.119(9) -0.001(6) F10 0.212(10) 0.066(5) 0.226(12) 0.006(6) -0.119(9) -0.001(6) O11 0.70(5) 0.23(2) 0.24(2) -0.098(18) 0.08(3) -0.05(3) F11 0.70(5) 0.23(2) 0.24(2) -0.098(18) 0.08(3) -0.05(3) C101 0.060(7) 0.087(9) 0.043(7) -0.001(6) 0.027(6) 0.026(7) C102 0.052(6) 0.089(9) 0.089(7) -0.006(7) 0.035(6) 0.003(7) C103 0.082(7) 0.126(9) 0.129(8) -0.022(8) 0.016(7) 0.000(8) C104 0.073(7) 0.091(8) 0.114(8) -0.019(7) 0.001(7) -0.025(7) C105 0.064(6) 0.064(6) 0.073(6) -0.029(5) -0.024(5) -0.029(5) C106 0.083(7) 0.068(6) 0.058(6) -0.014(5) -0.019(6) -0.033(6) C111 0.088(7) 0.109(8) 0.049(4) -0.033(5) 0.040(5) -0.015(6) C112 0.169(11) 0.102(8) 0.072(6) -0.025(6) 0.056(7) 0.009(8) C113 0.190(11) 0.229(15) 0.151(11) -0.028(12) 0.037(10) -0.103(12) C114 0.185(12) 0.267(15) 0.168(11) -0.099(11) 0.021(10) -0.080(12) C115 0.160(11) 0.162(11) 0.182(12) -0.087(9) -0.011(10) -0.084(9) C116 0.134(9) 0.137(10) 0.102(8) 0.022(7) -0.073(7) -0.078(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 Ru C74 2.220(4) . ? Ru C73 2.228(4) . ? Ru C72 2.230(4) . ? Ru P3 2.2422(12) . ? Ru C71 2.245(4) . ? Ru C75 2.248(4) . ? Ru P2 2.3547(12) . ? Ru P1 2.3560(11) . ? P1 C31 1.838(4) . ? P1 C11 1.842(4) . ? P1 C21 1.846(4) . ? P2 C41 1.841(4) . ? P2 C51 1.844(4) . ? P2 C61 1.851(4) . ? P3 O2 1.564(4) . ? P3 O1 1.567(4) . ? P3 O3 1.576(4) . ? O1 H1O 0.85(2) . ? O2 H2O 0.86(2) . ? O3 H3O 0.871(15) . ? C11 C12 1.382(6) . ? C11 C16 1.409(6) . ? C12 C13 1.389(7) . ? C12 H12 0.9300 . ? C13 C14 1.366(8) . ? C13 H13 0.9300 . ? C14 C15 1.382(7) . ? C14 H14 0.9300 . ? C15 C16 1.382(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C22 1.384(6) . ? C21 C26 1.397(6) . ? C22 C23 1.358(7) . ? C22 H22 0.9300 . ? C23 C24 1.384(7) . ? C23 H23 0.9300 . ? C24 C25 1.373(7) . ? C24 H24 0.9300 . ? C25 C26 1.375(7) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C32 1.396(6) . ? C31 C36 1.402(6) . ? C32 C33 1.396(7) . ? C32 H32 0.9300 . ? C33 C34 1.383(8) . ? C33 H33 0.9300 . ? C34 C35 1.380(8) . ? C34 H34 0.9300 . ? C35 C36 1.384(7) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C46 1.359(6) . ? C41 C42 1.395(6) . ? C42 C43 1.397(6) . ? C42 H42 0.9300 . ? C43 C44 1.360(8) . ? C43 H43 0.9300 . ? C44 C45 1.390(8) . ? C44 H44 0.9300 . ? C45 C46 1.374(7) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C52 1.375(6) . ? C51 C56 1.385(6) . ? C52 C53 1.406(7) . ? C52 H52 0.9300 . ? C53 C54 1.369(8) . ? C53 H53 0.9300 . ? C54 C55 1.376(8) . ? C54 H54 0.9300 . ? C55 C56 1.378(7) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C61 C66 1.381(7) . ? C61 C62 1.397(7) . ? C62 C63 1.396(7) . ? C62 H62 0.9300 . ? C63 C64 1.370(9) . ? C63 H63 0.9300 . ? C64 C65 1.363(9) . ? C64 H64 0.9300 . ? C65 C66 1.380(7) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C71 C72 1.403(6) . ? C71 C75 1.419(7) . ? C71 H71 0.9300 . ? C72 C74 1.421(7) . ? C72 H72 0.9300 . ? C73 C74 1.383(7) . ? C73 C75 1.418(7) . ? C73 H73 0.9300 . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? P4 O7 1.407(8) . ? P4 O4 1.483(7) . ? P4 O6 1.489(7) . ? P4 O5 1.626(7) . ? P5 O10 1.371(7) . ? P5 O8 1.412(8) . ? P5 O9 1.464(8) . ? P5 O11 1.476(9) . ? C101 C102 0.919(9) . ? C101 C103 1.817(10) . ? C101 H101 0.9600 . ? C101 H102 0.9600 . ? C101 H103 0.9600 . ? C102 C103 0.949(8) . ? C102 C104 1.827(10) . ? C102 H104 0.9700 . ? C102 H105 0.9700 . ? C103 C104 0.999(9) . ? C103 C105 1.798(10) . ? C103 H106 0.9700 . ? C103 H107 0.9700 . ? C104 C105 0.985(9) . ? C104 C106 1.789(10) . ? C104 H108 0.9700 . ? C104 H109 0.9700 . ? C105 C106 0.980(10) . ? C105 H110 0.9700 . ? C105 H111 0.9700 . ? C106 H112 0.9600 . ? C106 H113 0.9600 . ? C106 H114 0.9600 . ? C111 C112 0.945(9) . ? C111 C113 1.772(10) . ? C111 H115 0.9600 . ? C111 H116 0.9600 . ? C111 H117 0.9600 . ? C112 C113 0.952(8) . ? C112 C114 1.834(10) . ? C112 H118 0.9700 . ? C112 H119 0.9700 . ? C113 C114 0.963(8) . ? C113 C115 1.828(10) . ? C113 H120 0.9700 . ? C113 H121 0.9700 . ? C114 C115 1.013(9) . ? C114 C116 1.781(10) . ? C114 H122 0.9700 . ? C114 H123 0.9700 . ? C115 C116 0.944(9) . ? C115 H124 0.9700 . ? C115 H125 0.9700 . ? C116 H126 0.9600 . ? C116 H127 0.9600 . ? C116 H128 0.9600 . ? 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 C74 Ru C73 36.23(19) . . ? C74 Ru C72 37.26(18) . . ? C73 Ru C72 61.13(19) . . ? C74 Ru P3 94.06(14) . . ? C73 Ru P3 125.73(15) . . ? C72 Ru P3 93.36(13) . . ? C74 Ru C71 61.66(18) . . ? C73 Ru C71 61.43(18) . . ? C72 Ru C71 36.53(17) . . ? P3 Ru C71 124.36(14) . . ? C74 Ru C75 61.36(19) . . ? C73 Ru C75 36.95(18) . . ? C72 Ru C75 61.19(18) . . ? P3 Ru C75 153.40(14) . . ? C71 Ru C75 36.83(18) . . ? C74 Ru P2 108.58(14) . . ? C73 Ru P2 87.68(14) . . ? C72 Ru P2 145.55(13) . . ? P3 Ru P2 93.84(4) . . ? C71 Ru P2 139.91(14) . . ? C75 Ru P2 103.22(14) . . ? C74 Ru P1 146.70(13) . . ? C73 Ru P1 136.46(14) . . ? C72 Ru P1 110.38(13) . . ? P3 Ru P1 96.15(4) . . ? C71 Ru P1 86.64(12) . . ? C75 Ru P1 99.89(14) . . ? P2 Ru P1 102.26(4) . . ? C31 P1 C11 99.73(18) . . ? C31 P1 C21 102.0(2) . . ? C11 P1 C21 102.02(19) . . ? C31 P1 Ru 125.82(15) . . ? C11 P1 Ru 114.31(14) . . ? C21 P1 Ru 109.91(14) . . ? C41 P2 C51 102.26(19) . . ? C41 P2 C61 100.18(19) . . ? C51 P2 C61 102.8(2) . . ? C41 P2 Ru 123.54(14) . . ? C51 P2 Ru 112.77(14) . . ? C61 P2 Ru 112.71(15) . . ? O2 P3 O1 102.8(2) . . ? O2 P3 O3 103.3(2) . . ? O1 P3 O3 97.9(2) . . ? O2 P3 Ru 115.97(14) . . ? O1 P3 Ru 119.29(15) . . ? O3 P3 Ru 114.79(16) . . ? P3 O1 H1O 105(8) . . ? P3 O2 H2O 126(7) . . ? P3 O3 H3O 106(4) . . ? C12 C11 C16 117.5(4) . . ? C12 C11 P1 122.1(3) . . ? C16 C11 P1 120.3(3) . . ? C11 C12 C13 120.9(4) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 121.2(5) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 118.8(5) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 120.7(5) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C11 120.7(5) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C22 C21 C26 116.7(4) . . ? C22 C21 P1 124.5(3) . . ? C26 C21 P1 118.7(3) . . ? C23 C22 C21 121.6(4) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 121.3(5) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C25 C24 C23 118.3(5) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? C24 C25 C26 120.3(5) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 121.7(5) . . ? C25 C26 H26 119.1 . . ? C21 C26 H26 119.1 . . ? C32 C31 C36 118.0(4) . . ? C32 C31 P1 119.6(3) . . ? C36 C31 P1 122.4(3) . . ? C31 C32 C33 121.6(5) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C34 C33 C32 119.4(5) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 119.5(5) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 121.6(5) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C35 C36 C31 119.9(4) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C46 C41 C42 118.7(4) . . ? C46 C41 P2 120.9(3) . . ? C42 C41 P2 120.4(3) . . ? C41 C42 C43 119.9(5) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C44 C43 C42 120.5(5) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 119.3(5) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? C46 C45 C44 120.1(5) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C41 C46 C45 121.6(5) . . ? C41 C46 H46 119.2 . . ? C45 C46 H46 119.2 . . ? C52 C51 C56 118.5(4) . . ? C52 C51 P2 121.1(3) . . ? C56 C51 P2 120.3(4) . . ? C51 C52 C53 120.4(5) . . ? C51 C52 H52 119.8 . . ? C53 C52 H52 119.8 . . ? C54 C53 C52 119.8(6) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C53 C54 C55 120.2(5) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? C54 C55 C56 119.6(5) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C55 C56 C51 121.5(5) . . ? C55 C56 H56 119.2 . . ? C51 C56 H56 119.2 . . ? C66 C61 C62 118.6(4) . . ? C66 C61 P2 119.9(4) . . ? C62 C61 P2 121.4(4) . . ? C63 C62 C61 119.8(5) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C64 C63 C62 120.4(6) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C65 C64 C63 119.7(5) . . ? C65 C64 H64 120.1 . . ? C63 C64 H64 120.1 . . ? C64 C65 C66 121.0(6) . . ? C64 C65 H65 119.5 . . ? C66 C65 H65 119.5 . . ? C65 C66 C61 120.5(5) . . ? C65 C66 H66 119.7 . . ? C61 C66 H66 119.7 . . ? C72 C71 C75 107.7(4) . . ? C72 C71 Ru 71.1(3) . . ? C75 C71 Ru 71.7(3) . . ? C72 C71 H71 126.1 . . ? C75 C71 H71 126.1 . . ? Ru C71 H71 122.7 . . ? C71 C72 C74 108.2(4) . . ? C71 C72 Ru 72.3(3) . . ? C74 C72 Ru 71.0(2) . . ? C71 C72 H72 125.9 . . ? C74 C72 H72 125.9 . . ? Ru C72 H72 122.5 . . ? C74 C73 C75 108.9(4) . . ? C74 C73 Ru 71.6(3) . . ? C75 C73 Ru 72.3(2) . . ? C74 C73 H73 125.5 . . ? C75 C73 H73 125.5 . . ? Ru C73 H73 122.3 . . ? C73 C74 C72 107.9(4) . . ? C73 C74 Ru 72.2(3) . . ? C72 C74 Ru 71.8(2) . . ? C73 C74 H74 126.1 . . ? C72 C74 H74 126.1 . . ? Ru C74 H74 121.7 . . ? C73 C75 C71 107.2(5) . . ? C73 C75 Ru 70.8(2) . . ? C71 C75 Ru 71.5(2) . . ? C73 C75 H75 126.4 . . ? C71 C75 H75 126.4 . . ? Ru C75 H75 123.1 . . ? O7 P4 O4 117.8(6) . . ? O7 P4 O6 118.2(6) . . ? O4 P4 O6 109.0(5) . . ? O7 P4 O5 106.5(6) . . ? O4 P4 O5 102.1(4) . . ? O6 P4 O5 100.2(5) . . ? O10 P5 O8 115.6(6) . . ? O10 P5 O9 112.0(6) . . ? O8 P5 O9 110.8(6) . . ? O10 P5 O11 109.0(6) . . ? O8 P5 O11 105.1(7) . . ? O9 P5 O11 103.3(7) . . ? C102 C101 C103 13.6(11) . . ? C102 C101 H101 109.5 . . ? C103 C101 H101 122.9 . . ? C102 C101 H102 109.5 . . ? C103 C101 H102 104.3 . . ? H101 C101 H102 109.5 . . ? C102 C101 H103 109.5 . . ? C103 C101 H103 100.5 . . ? H101 C101 H103 109.5 . . ? H102 C101 H103 109.5 . . ? C101 C102 C103 153(2) . . ? C101 C102 C104 132.8(18) . . ? C103 C102 C104 20.8(9) . . ? C101 C102 H104 98.2 . . ? C103 C102 H104 98.2 . . ? C104 C102 H104 114.3 . . ? C101 C102 H105 98.2 . . ? C103 C102 H105 98.2 . . ? C104 C102 H105 105.6 . . ? H104 C102 H105 103.8 . . ? C102 C103 C104 139.5(17) . . ? C102 C103 C105 116.5(15) . . ? C104 C103 C105 24.8(8) . . ? C102 C103 C101 13.2(11) . . ? C104 C103 C101 126.6(14) . . ? C105 C103 C101 103.3(11) . . ? C102 C103 H106 102.2 . . ? C104 C103 H106 102.2 . . ? C105 C103 H106 105.1 . . ? C101 C103 H106 106.6 . . ? C102 C103 H107 102.2 . . ? C104 C103 H107 102.2 . . ? C105 C103 H107 123.6 . . ? C101 C103 H107 112.2 . . ? H106 C103 H107 104.8 . . ? C105 C104 C103 130.0(15) . . ? C105 C104 C106 24.3(9) . . ? C103 C104 C106 115.8(15) . . ? C105 C104 C102 111.9(14) . . ? C103 C104 C102 19.7(8) . . ? C106 C104 C102 102.4(10) . . ? C105 C104 H108 104.8 . . ? C103 C104 H108 104.8 . . ? C106 C104 H108 129.0 . . ? C102 C104 H108 106.7 . . ? C105 C104 H109 104.8 . . ? C103 C104 H109 104.8 . . ? C106 C104 H109 92.9 . . ? C102 C104 H109 121.6 . . ? H108 C104 H109 105.8 . . ? C106 C105 C104 131.2(17) . . ? C106 C105 C103 116.3(16) . . ? C104 C105 C103 25.2(8) . . ? C106 C105 H110 104.5 . . ? C104 C105 H110 104.5 . . ? C103 C105 H110 92.3 . . ? C106 C105 H111 104.5 . . ? C104 C105 H111 104.5 . . ? C103 C105 H111 129.5 . . ? H110 C105 H111 105.6 . . ? C105 C106 C104 24.5(8) . . ? C105 C106 H112 109.5 . . ? C104 C106 H112 87.7 . . ? C105 C106 H113 109.5 . . ? C104 C106 H113 108.3 . . ? H112 C106 H113 109.5 . . ? C105 C106 H114 109.5 . . ? C104 C106 H114 129.5 . . ? H112 C106 H114 109.5 . . ? H113 C106 H114 109.5 . . ? C112 C111 C113 21.0(9) . . ? C112 C111 H115 109.5 . . ? C113 C111 H115 121.6 . . ? C112 C111 H116 109.5 . . ? C113 C111 H116 115.6 . . ? H115 C111 H116 109.5 . . ? C112 C111 H117 109.5 . . ? C113 C111 H117 88.7 . . ? H115 C111 H117 109.5 . . ? H116 C111 H117 109.5 . . ? C111 C112 C113 138.2(17) . . ? C111 C112 C114 124.0(14) . . ? C113 C112 C114 16.8(9) . . ? C111 C112 H118 102.6 . . ? C113 C112 H118 102.6 . . ? C114 C112 H118 101.6 . . ? C111 C112 H119 102.6 . . ? C113 C112 H119 102.6 . . ? C114 C112 H119 118.5 . . ? H118 C112 H119 104.9 . . ? C112 C113 C114 146.5(18) . . ? C112 C113 C111 20.8(9) . . ? C114 C113 C111 128.5(13) . . ? C112 C113 C115 126.2(15) . . ? C114 C113 C115 23.0(9) . . ? C111 C113 C115 106.5(11) . . ? C112 C113 H120 100.2 . . ? C114 C113 H120 100.2 . . ? C111 C113 H120 120.1 . . ? C115 C113 H120 121.8 . . ? C112 C113 H121 100.2 . . ? C114 C113 H121 100.2 . . ? C111 C113 H121 99.4 . . ? C115 C113 H121 100.2 . . ? H120 C113 H121 104.2 . . ? C113 C114 C115 135.3(17) . . ? C113 C114 C116 142.1(16) . . ? C115 C114 C116 23.6(9) . . ? C113 C114 C112 16.6(9) . . ? C115 C114 C112 121.0(15) . . ? C116 C114 C112 125.4(12) . . ? C113 C114 H122 103.4 . . ? C115 C114 H122 103.4 . . ? C116 C114 H122 79.9 . . ? C112 C114 H122 103.0 . . ? C113 C114 H123 103.4 . . ? C115 C114 H123 103.4 . . ? C116 C114 H123 112.3 . . ? C112 C114 H123 118.9 . . ? H122 C114 H123 105.2 . . ? C116 C115 C114 131.0(18) . . ? C116 C115 C113 138.2(17) . . ? C114 C115 C113 21.8(8) . . ? C116 C115 H124 104.5 . . ? C114 C115 H124 104.5 . . ? C113 C115 H124 82.8 . . ? C116 C115 H125 104.5 . . ? C114 C115 H125 104.5 . . ? C113 C115 H125 113.0 . . ? H124 C115 H125 105.7 . . ? C115 C116 C114 25.4(10) . . ? C115 C116 H126 109.5 . . ? C114 C116 H126 128.4 . . ? C115 C116 H127 109.5 . . ? C114 C116 H127 85.8 . . ? H126 C116 H127 109.5 . . ? C115 C116 H128 109.5 . . ? C114 C116 H128 110.8 . . ? H126 C116 H128 109.5 . . ? H127 C116 H128 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C74 Ru P1 C31 -176.6(3) . . . . ? C73 Ru P1 C31 125.5(3) . . . . ? C72 Ru P1 C31 -165.4(2) . . . . ? P3 Ru P1 C31 -69.48(17) . . . . ? C71 Ru P1 C31 166.3(2) . . . . ? C75 Ru P1 C31 131.8(2) . . . . ? P2 Ru P1 C31 25.82(17) . . . . ? C74 Ru P1 C11 -52.9(3) . . . . ? C73 Ru P1 C11 -110.8(2) . . . . ? C72 Ru P1 C11 -41.7(2) . . . . ? P3 Ru P1 C11 54.21(15) . . . . ? C71 Ru P1 C11 -70.0(2) . . . . ? C75 Ru P1 C11 -104.5(2) . . . . ? P2 Ru P1 C11 149.51(14) . . . . ? C74 Ru P1 C21 61.1(3) . . . . ? C73 Ru P1 C21 3.2(3) . . . . ? C72 Ru P1 C21 72.30(19) . . . . ? P3 Ru P1 C21 168.20(14) . . . . ? C71 Ru P1 C21 43.99(19) . . . . ? C75 Ru P1 C21 9.50(19) . . . . ? P2 Ru P1 C21 -96.50(14) . . . . ? C74 Ru P2 C41 128.2(2) . . . . ? C73 Ru P2 C41 158.2(2) . . . . ? C72 Ru P2 C41 134.2(3) . . . . ? P3 Ru P2 C41 32.56(17) . . . . ? C71 Ru P2 C41 -164.1(2) . . . . ? C75 Ru P2 C41 -168.0(2) . . . . ? P1 Ru P2 C41 -64.59(17) . . . . ? C74 Ru P2 C51 -108.2(2) . . . . ? C73 Ru P2 C51 -78.1(2) . . . . ? C72 Ru P2 C51 -102.1(3) . . . . ? P3 Ru P2 C51 156.24(15) . . . . ? C71 Ru P2 C51 -40.4(2) . . . . ? C75 Ru P2 C51 -44.3(2) . . . . ? P1 Ru P2 C51 59.09(16) . . . . ? C74 Ru P2 C61 7.7(2) . . . . ? C73 Ru P2 C61 37.7(2) . . . . ? C72 Ru P2 C61 13.7(3) . . . . ? P3 Ru P2 C61 -87.92(16) . . . . ? C71 Ru P2 C61 75.4(2) . . . . ? C75 Ru P2 C61 71.5(2) . . . . ? P1 Ru P2 C61 174.93(15) . . . . ? C74 Ru P3 O2 -79.8(2) . . . . ? C73 Ru P3 O2 -60.8(2) . . . . ? C72 Ru P3 O2 -117.1(2) . . . . ? C71 Ru P3 O2 -137.9(2) . . . . ? C75 Ru P3 O2 -101.1(4) . . . . ? P2 Ru P3 O2 29.15(19) . . . . ? P1 Ru P3 O2 131.94(19) . . . . ? C74 Ru P3 O1 156.4(2) . . . . ? C73 Ru P3 O1 175.4(2) . . . . ? C72 Ru P3 O1 119.0(2) . . . . ? C71 Ru P3 O1 98.2(2) . . . . ? C75 Ru P3 O1 135.1(3) . . . . ? P2 Ru P3 O1 -94.67(18) . . . . ? P1 Ru P3 O1 8.12(18) . . . . ? C74 Ru P3 O3 40.7(2) . . . . ? C73 Ru P3 O3 59.7(3) . . . . ? C72 Ru P3 O3 3.3(2) . . . . ? C71 Ru P3 O3 -17.5(2) . . . . ? C75 Ru P3 O3 19.4(4) . . . . ? P2 Ru P3 O3 149.64(19) . . . . ? P1 Ru P3 O3 -107.58(19) . . . . ? C31 P1 C11 C12 144.6(4) . . . . ? C21 P1 C11 C12 -110.8(4) . . . . ? Ru P1 C11 C12 7.8(4) . . . . ? C31 P1 C11 C16 -38.9(4) . . . . ? C21 P1 C11 C16 65.7(4) . . . . ? Ru P1 C11 C16 -175.7(3) . . . . ? C16 C11 C12 C13 0.1(7) . . . . ? P1 C11 C12 C13 176.7(4) . . . . ? C11 C12 C13 C14 -1.6(8) . . . . ? C12 C13 C14 C15 2.2(8) . . . . ? C13 C14 C15 C16 -1.3(9) . . . . ? C14 C15 C16 C11 -0.2(9) . . . . ? C12 C11 C16 C15 0.8(7) . . . . ? P1 C11 C16 C15 -175.9(4) . . . . ? C31 P1 C21 C22 102.3(4) . . . . ? C11 P1 C21 C22 -0.5(4) . . . . ? Ru P1 C21 C22 -122.2(4) . . . . ? C31 P1 C21 C26 -75.3(4) . . . . ? C11 P1 C21 C26 -178.2(4) . . . . ? Ru P1 C21 C26 60.2(4) . . . . ? C26 C21 C22 C23 -0.6(7) . . . . ? P1 C21 C22 C23 -178.3(4) . . . . ? C21 C22 C23 C24 -0.5(8) . . . . ? C22 C23 C24 C25 1.3(8) . . . . ? C23 C24 C25 C26 -1.0(8) . . . . ? C24 C25 C26 C21 -0.1(8) . . . . ? C22 C21 C26 C25 0.9(7) . . . . ? P1 C21 C26 C25 178.7(4) . . . . ? C11 P1 C31 C32 -46.6(4) . . . . ? C21 P1 C31 C32 -151.2(4) . . . . ? Ru P1 C31 C32 83.1(4) . . . . ? C11 P1 C31 C36 133.0(4) . . . . ? C21 P1 C31 C36 28.4(4) . . . . ? Ru P1 C31 C36 -97.3(4) . . . . ? C36 C31 C32 C33 0.0(8) . . . . ? P1 C31 C32 C33 179.6(4) . . . . ? C31 C32 C33 C34 -1.8(9) . . . . ? C32 C33 C34 C35 2.5(9) . . . . ? C33 C34 C35 C36 -1.4(9) . . . . ? C34 C35 C36 C31 -0.5(8) . . . . ? C32 C31 C36 C35 1.2(7) . . . . ? P1 C31 C36 C35 -178.4(4) . . . . ? C51 P2 C41 C46 -109.9(4) . . . . ? C61 P2 C41 C46 144.5(4) . . . . ? Ru P2 C41 C46 18.3(5) . . . . ? C51 P2 C41 C42 69.0(4) . . . . ? C61 P2 C41 C42 -36.6(4) . . . . ? Ru P2 C41 C42 -162.7(3) . . . . ? C46 C41 C42 C43 -1.4(7) . . . . ? P2 C41 C42 C43 179.7(4) . . . . ? C41 C42 C43 C44 0.6(8) . . . . ? C42 C43 C44 C45 0.0(9) . . . . ? C43 C44 C45 C46 0.2(10) . . . . ? C42 C41 C46 C45 1.6(8) . . . . ? P2 C41 C46 C45 -179.5(5) . . . . ? C44 C45 C46 C41 -1.0(10) . . . . ? C41 P2 C51 C52 21.8(4) . . . . ? C61 P2 C51 C52 125.4(4) . . . . ? Ru P2 C51 C52 -113.0(4) . . . . ? C41 P2 C51 C56 -162.9(4) . . . . ? C61 P2 C51 C56 -59.3(4) . . . . ? Ru P2 C51 C56 62.4(4) . . . . ? C56 C51 C52 C53 0.3(7) . . . . ? P2 C51 C52 C53 175.7(4) . . . . ? C51 C52 C53 C54 -1.2(9) . . . . ? C52 C53 C54 C55 2.3(9) . . . . ? C53 C54 C55 C56 -2.5(9) . . . . ? C54 C55 C56 C51 1.6(8) . . . . ? C52 C51 C56 C55 -0.5(7) . . . . ? P2 C51 C56 C55 -175.9(4) . . . . ? C41 P2 C61 C66 -89.0(4) . . . . ? C51 P2 C61 C66 165.8(4) . . . . ? Ru P2 C61 C66 44.2(4) . . . . ? C41 P2 C61 C62 87.6(4) . . . . ? C51 P2 C61 C62 -17.6(4) . . . . ? Ru P2 C61 C62 -139.3(3) . . . . ? C66 C61 C62 C63 -0.7(7) . . . . ? P2 C61 C62 C63 -177.3(4) . . . . ? C61 C62 C63 C64 1.0(8) . . . . ? C62 C63 C64 C65 -1.1(8) . . . . ? C63 C64 C65 C66 1.0(9) . . . . ? C64 C65 C66 C61 -0.8(8) . . . . ? C62 C61 C66 C65 0.6(7) . . . . ? P2 C61 C66 C65 177.3(4) . . . . ? C74 Ru C71 C72 -37.7(3) . . . . ? C73 Ru C71 C72 -79.1(3) . . . . ? P3 Ru C71 C72 36.5(3) . . . . ? C75 Ru C71 C72 -116.9(4) . . . . ? P2 Ru C71 C72 -123.2(3) . . . . ? P1 Ru C71 C72 131.7(3) . . . . ? C74 Ru C71 C75 79.1(3) . . . . ? C73 Ru C71 C75 37.7(3) . . . . ? C72 Ru C71 C75 116.9(4) . . . . ? P3 Ru C71 C75 153.4(2) . . . . ? P2 Ru C71 C75 -6.3(4) . . . . ? P1 Ru C71 C75 -111.4(3) . . . . ? C75 C71 C72 C74 -0.5(5) . . . . ? Ru C71 C72 C74 62.3(3) . . . . ? C75 C71 C72 Ru -62.8(3) . . . . ? C74 Ru C72 C71 117.2(4) . . . . ? C73 Ru C72 C71 80.0(3) . . . . ? P3 Ru C72 C71 -150.5(3) . . . . ? C75 Ru C72 C71 37.6(3) . . . . ? P2 Ru C72 C71 107.7(3) . . . . ? P1 Ru C72 C71 -52.7(3) . . . . ? C73 Ru C72 C74 -37.2(3) . . . . ? P3 Ru C72 C74 92.3(3) . . . . ? C71 Ru C72 C74 -117.2(4) . . . . ? C75 Ru C72 C74 -79.6(3) . . . . ? P2 Ru C72 C74 -9.5(4) . . . . ? P1 Ru C72 C74 -169.9(3) . . . . ? C72 Ru C73 C74 38.2(3) . . . . ? P3 Ru C73 C74 -33.4(3) . . . . ? C71 Ru C73 C74 80.1(3) . . . . ? C75 Ru C73 C74 117.7(4) . . . . ? P2 Ru C73 C74 -126.5(3) . . . . ? P1 Ru C73 C74 128.1(3) . . . . ? C74 Ru C73 C75 -117.7(4) . . . . ? C72 Ru C73 C75 -79.5(3) . . . . ? P3 Ru C73 C75 -151.2(3) . . . . ? C71 Ru C73 C75 -37.6(3) . . . . ? P2 Ru C73 C75 115.8(3) . . . . ? P1 Ru C73 C75 10.3(4) . . . . ? C75 C73 C74 C72 -0.3(5) . . . . ? Ru C73 C74 C72 -63.3(3) . . . . ? C75 C73 C74 Ru 63.0(3) . . . . ? C71 C72 C74 C73 0.5(5) . . . . ? Ru C72 C74 C73 63.6(3) . . . . ? C71 C72 C74 Ru -63.2(3) . . . . ? C72 Ru C74 C73 -116.4(4) . . . . ? P3 Ru C74 C73 153.4(3) . . . . ? C71 Ru C74 C73 -79.5(3) . . . . ? C75 Ru C74 C73 -37.3(3) . . . . ? P2 Ru C74 C73 57.9(3) . . . . ? P1 Ru C74 C73 -99.0(4) . . . . ? C73 Ru C74 C72 116.4(4) . . . . ? P3 Ru C74 C72 -90.2(3) . . . . ? C71 Ru C74 C72 37.0(3) . . . . ? C75 Ru C74 C72 79.1(3) . . . . ? P2 Ru C74 C72 174.4(3) . . . . ? P1 Ru C74 C72 17.5(5) . . . . ? C74 C73 C75 C71 0.0(5) . . . . ? Ru C73 C75 C71 62.6(3) . . . . ? C74 C73 C75 Ru -62.6(3) . . . . ? C72 C71 C75 C73 0.3(5) . . . . ? Ru C71 C75 C73 -62.1(3) . . . . ? C72 C71 C75 Ru 62.4(3) . . . . ? C74 Ru C75 C73 36.6(3) . . . . ? C72 Ru C75 C73 79.3(3) . . . . ? P3 Ru C75 C73 61.0(5) . . . . ? C71 Ru C75 C73 116.6(4) . . . . ? P2 Ru C75 C73 -67.6(3) . . . . ? P1 Ru C75 C73 -172.8(3) . . . . ? C74 Ru C75 C71 -80.0(3) . . . . ? C73 Ru C75 C71 -116.6(4) . . . . ? C72 Ru C75 C71 -37.3(3) . . . . ? P3 Ru C75 C71 -55.7(4) . . . . ? P2 Ru C75 C71 175.8(3) . . . . ? P1 Ru C75 C71 70.6(3) . . . . ? C103 C101 C102 C104 7(5) . . . . ? C101 C102 C103 C104 15(10) . . . . ? C101 C102 C103 C105 3(8) . . . . ? C104 C102 C103 C105 -12(3) . . . . ? C104 C102 C103 C101 -15(10) . . . . ? C102 C101 C103 C104 -168(8) . . . . ? C102 C101 C103 C105 -177(7) . . . . ? C102 C103 C104 C105 -26(6) . . . . ? C101 C103 C104 C105 -22(5) . . . . ? C102 C103 C104 C106 -50(5) . . . . ? C105 C103 C104 C106 -23.8(18) . . . . ? C101 C103 C104 C106 -46(3) . . . . ? C105 C103 C104 C102 26(6) . . . . ? C101 C103 C104 C102 4(3) . . . . ? C101 C102 C104 C105 -12(4) . . . . ? C103 C102 C104 C105 159(5) . . . . ? C101 C102 C104 C103 -171(6) . . . . ? C101 C102 C104 C106 -36(3) . . . . ? C103 C102 C104 C106 135(5) . . . . ? C103 C104 C105 C106 -62(5) . . . . ? C102 C104 C105 C106 -71(3) . . . . ? C106 C104 C105 C103 62(5) . . . . ? C102 C104 C105 C103 -9(2) . . . . ? C102 C103 C105 C106 -66(3) . . . . ? C104 C103 C105 C106 132(4) . . . . ? C101 C103 C105 C106 -66(2) . . . . ? C102 C103 C105 C104 161(5) . . . . ? C101 C103 C105 C104 162(4) . . . . ? C103 C105 C106 C104 -24.7(17) . . . . ? C103 C104 C106 C105 132(4) . . . . ? C102 C104 C106 C105 116(3) . . . . ? C113 C111 C112 C114 -12(2) . . . . ? C111 C112 C113 C114 -37(7) . . . . ? C114 C112 C113 C111 37(7) . . . . ? C111 C112 C113 C115 -21(4) . . . . ? C114 C112 C113 C115 16(3) . . . . ? C112 C111 C113 C114 155(5) . . . . ? C112 C111 C113 C115 162(4) . . . . ? C112 C113 C114 C115 35(7) . . . . ? C111 C113 C114 C115 19(5) . . . . ? C112 C113 C114 C116 0(7) . . . . ? C111 C113 C114 C116 -16(5) . . . . ? C115 C113 C114 C116 -34.6(17) . . . . ? C111 C113 C114 C112 -16(3) . . . . ? C115 C113 C114 C112 -35(7) . . . . ? C111 C112 C114 C113 151(5) . . . . ? C111 C112 C114 C115 -1(3) . . . . ? C113 C112 C114 C115 -152(6) . . . . ? C111 C112 C114 C116 -29(3) . . . . ? C113 C112 C114 C116 180(6) . . . . ? C113 C114 C115 C116 -119(4) . . . . ? C112 C114 C115 C116 -108(3) . . . . ? C116 C114 C115 C113 119(4) . . . . ? C112 C114 C115 C113 11(2) . . . . ? C112 C113 C115 C116 -76(4) . . . . ? C114 C113 C115 C116 81(4) . . . . ? C111 C113 C115 C116 -83(3) . . . . ? C112 C113 C115 C114 -157(5) . . . . ? C111 C113 C115 C114 -165(4) . . . . ? C113 C115 C116 C114 -29.0(14) . . . . ? C113 C114 C116 C115 87(4) . . . . ? C112 C114 C116 C115 87(3) . . . . ? #============================================================================= # END of CIF #=============================================================================