# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_2 _database_code_depnum_ccdc_archive 'CCDC 908513' #TrackingRef '2_3_5a.cif' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H50 Cl2 O10 P2 Ru2, 2(F6 Sb)' _chemical_formula_sum 'C52 H50 Cl2 F12 O10 P2 Ru2 Sb2' _chemical_formula_weight 1641.40 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9387(3) _cell_length_b 11.8480(4) _cell_length_c 24.2871(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.775(2) _cell_angle_gamma 90.00 _cell_volume 2856.54(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4911 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.350 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 1.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.734 _exptl_absorpt_correction_T_max 0.890 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95 mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18346 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_unetI/netI 0.0650 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.36 _reflns_number_total 5227 _reflns_number_gt 3718 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker, 2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowki & Minor 1997)' _computing_data_reduction 'HKL Denzo and scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0865P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5227 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1459 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2930(6) 0.1538(6) 0.4248(2) 0.0356(15) Uani 1 1 d . . . H1 H 0.2869 0.2267 0.4096 0.043 Uiso 1 1 calc R . . C2 C 0.2853(6) 0.0569(6) 0.3904(2) 0.0342(15) Uani 1 1 d . . . H2 H 0.2714 0.0665 0.3522 0.041 Uiso 1 1 calc R . . C3 C 0.2978(6) -0.0524(5) 0.4117(2) 0.0319(14) Uani 1 1 d . . . H3 H 0.2854 -0.1155 0.3886 0.038 Uiso 1 1 calc R . . C4 C 0.3300(6) -0.0665(5) 0.4698(3) 0.0332(14) Uani 1 1 d . . . C5 C 0.3296(5) 0.0294(6) 0.5050(2) 0.0335(14) Uani 1 1 d . . . H5 H 0.3423 0.0207 0.5434 0.040 Uiso 1 1 calc R . . C6 C 0.3097(6) 0.1386(5) 0.4816(3) 0.0331(14) Uani 1 1 d . . . H6 H 0.3078 0.2018 0.5050 0.040 Uiso 1 1 calc R . . C7 C 0.3370(8) -0.2681(6) 0.4616(3) 0.0520(19) Uani 1 1 d . . . H7A H 0.4042 -0.2691 0.4334 0.062 Uiso 1 1 calc R . . H7B H 0.2471 -0.2729 0.4433 0.062 Uiso 1 1 calc R . . C8 C 0.3597(9) -0.3653(7) 0.5010(4) 0.063(2) Uani 1 1 d . . . H8A H 0.3755 -0.4352 0.4808 0.075 Uiso 1 1 calc R . . H8B H 0.4379 -0.3507 0.5261 0.075 Uiso 1 1 calc R . . C9 C 0.0436(6) 0.2941(6) 0.3680(3) 0.0423(16) Uani 1 1 d . . . C10 C 0.1184(7) 0.3014(7) 0.3219(3) 0.0501(18) Uani 1 1 d . . . H10 H 0.1048 0.2508 0.2923 0.060 Uiso 1 1 calc R . . C11 C 0.2147(8) 0.3866(8) 0.3205(4) 0.062(2) Uani 1 1 d . . . H11 H 0.2677 0.3948 0.2898 0.074 Uiso 1 1 calc R . . C12 C 0.2315(10) 0.4597(7) 0.3655(5) 0.076(3) Uani 1 1 d . . . H12 H 0.2985 0.5157 0.3652 0.091 Uiso 1 1 calc R . . C13 C 0.1530(10) 0.4517(8) 0.4098(5) 0.086(3) Uani 1 1 d . . . H13 H 0.1645 0.5034 0.4390 0.103 Uiso 1 1 calc R . . C14 C 0.0580(8) 0.3691(7) 0.4120(4) 0.063(2) Uani 1 1 d . . . H14 H 0.0035 0.3629 0.4424 0.076 Uiso 1 1 calc R . . C15 C 0.0538(6) -0.0650(6) 0.3089(2) 0.0356(15) Uani 1 1 d . . . C16 C 0.0172(7) -0.1625(6) 0.3340(2) 0.0404(16) Uani 1 1 d . . . H16 H -0.0473 -0.1615 0.3611 0.048 Uiso 1 1 calc R . . C17 C 0.0769(8) -0.2640(7) 0.3189(3) 0.0511(18) Uani 1 1 d . . . H17 H 0.0537 -0.3320 0.3359 0.061 Uiso 1 1 calc R . . C18 C 0.1718(8) -0.2633(7) 0.2780(3) 0.057(2) Uani 1 1 d . . . H18 H 0.2141 -0.3307 0.2679 0.068 Uiso 1 1 calc R . . C19 C 0.2025(8) -0.1640(8) 0.2530(3) 0.056(2) Uani 1 1 d . . . H19 H 0.2653 -0.1642 0.2253 0.067 Uiso 1 1 calc R . . C20 C 0.1445(7) -0.0645(7) 0.2672(3) 0.0454(17) Uani 1 1 d . . . H20 H 0.1654 0.0029 0.2491 0.054 Uiso 1 1 calc R . . C21 C -0.2895(6) 0.0746(6) 0.3601(2) 0.0390(16) Uani 1 1 d . . . C22 C -0.3386(7) -0.0024(8) 0.3211(3) 0.053(2) Uani 1 1 d . . . H22 H -0.2984 -0.0735 0.3170 0.064 Uiso 1 1 calc R . . C23 C -0.4508(9) 0.0310(10) 0.2881(3) 0.074(3) Uani 1 1 d . . . H23 H -0.4876 -0.0179 0.2609 0.089 Uiso 1 1 calc R . . C24 C -0.5072(8) 0.1357(10) 0.2956(4) 0.072(3) Uani 1 1 d . . . H24 H -0.5819 0.1578 0.2729 0.087 Uiso 1 1 calc R . . C25 C -0.4573(8) 0.2082(8) 0.3352(3) 0.062(2) Uani 1 1 d . . . H25 H -0.4986 0.2786 0.3402 0.074 Uiso 1 1 calc R . . C26 C -0.3454(7) 0.1776(7) 0.3680(3) 0.0503(19) Uani 1 1 d . . . H26 H -0.3090 0.2269 0.3952 0.060 Uiso 1 1 calc R . . O1 O 0.3495(4) -0.1656(4) 0.49419(18) 0.0427(11) Uani 1 1 d . . . O2 O 0.2408(7) -0.3744(5) 0.5309(3) 0.0769(19) Uani 1 1 d . . . H2A H 0.2494 -0.4269 0.5535 0.115 Uiso 1 1 calc R . . O3 O -0.0564(4) 0.2096(4) 0.37209(18) 0.0405(11) Uani 1 1 d . . . O4 O -0.0002(4) 0.0411(4) 0.32248(16) 0.0372(10) Uani 1 1 d . . . O5 O -0.1760(4) 0.0405(4) 0.39464(16) 0.0344(10) Uani 1 1 d . . . F1 F -0.2999(9) 0.7779(5) 0.3985(2) 0.124(3) Uani 1 1 d . . . F2 F -0.2608(5) 0.6843(4) 0.30260(16) 0.0660(13) Uani 1 1 d . . . F3 F -0.3894(6) 0.5923(5) 0.4378(2) 0.0894(18) Uani 1 1 d . . . F4 F -0.4993(6) 0.6777(8) 0.3466(2) 0.122(3) Uani 1 1 d . . . F5 F -0.1605(8) 0.5872(11) 0.3930(3) 0.194(5) Uani 1 1 d . . . F6 F -0.3641(13) 0.4977(6) 0.3386(4) 0.196(5) Uani 1 1 d . . . P1 P -0.02742(15) 0.07999(14) 0.38383(6) 0.0280(3) Uani 1 1 d . . . Cl1 Cl -0.00794(14) 0.12640(12) 0.51786(5) 0.0281(3) Uani 1 1 d . . . Ru1 Ru 0.13251(4) 0.03709(4) 0.451299(17) 0.02499(16) Uani 1 1 d . . . Sb1 Sb -0.32710(6) 0.63777(5) 0.36944(2) 0.0531(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 C1 0.019(3) 0.051(4) 0.037(3) 0.008(3) 0.002(2) -0.005(3) C2 0.020(3) 0.054(4) 0.029(3) -0.001(3) 0.010(2) -0.007(3) C3 0.020(3) 0.044(4) 0.032(3) -0.008(3) 0.011(2) 0.001(3) C4 0.014(3) 0.040(4) 0.047(4) 0.009(3) 0.009(3) 0.003(3) C5 0.014(3) 0.057(4) 0.029(3) -0.001(3) -0.001(2) -0.001(3) C6 0.020(3) 0.040(4) 0.040(3) -0.001(3) 0.001(3) -0.010(3) C7 0.052(5) 0.039(4) 0.066(5) 0.000(4) 0.018(4) 0.011(3) C8 0.055(5) 0.060(5) 0.075(6) 0.010(4) 0.025(4) 0.011(4) C9 0.027(3) 0.038(4) 0.062(4) 0.019(3) 0.002(3) -0.002(3) C10 0.043(4) 0.058(5) 0.048(4) 0.021(4) -0.002(3) 0.005(4) C11 0.041(4) 0.071(6) 0.075(6) 0.041(5) 0.007(4) 0.001(4) C12 0.073(6) 0.040(5) 0.115(8) 0.016(5) 0.009(6) -0.012(4) C13 0.078(7) 0.051(5) 0.131(9) -0.017(6) 0.028(7) -0.011(5) C14 0.055(5) 0.049(5) 0.087(6) -0.014(4) 0.022(5) 0.004(4) C15 0.031(3) 0.048(4) 0.027(3) -0.009(3) -0.008(3) 0.002(3) C16 0.034(4) 0.061(4) 0.026(3) -0.012(3) 0.007(3) -0.004(3) C17 0.054(5) 0.056(5) 0.043(4) -0.002(4) -0.003(3) 0.001(4) C18 0.050(5) 0.066(5) 0.054(4) -0.026(4) 0.004(4) 0.009(4) C19 0.039(4) 0.089(6) 0.041(4) -0.024(4) 0.011(3) -0.005(4) C20 0.044(4) 0.064(5) 0.028(3) -0.004(3) 0.007(3) -0.002(4) C21 0.025(3) 0.067(5) 0.025(3) 0.018(3) 0.003(3) 0.002(3) C22 0.035(4) 0.087(6) 0.038(4) 0.001(4) -0.002(3) -0.006(4) C23 0.047(5) 0.136(10) 0.038(4) 0.012(5) -0.006(4) -0.019(6) C24 0.031(4) 0.137(9) 0.049(5) 0.048(6) 0.006(4) 0.002(5) C25 0.034(4) 0.096(7) 0.055(5) 0.037(5) 0.009(4) 0.010(4) C26 0.032(4) 0.077(5) 0.042(4) 0.022(4) 0.008(3) 0.005(4) O1 0.031(3) 0.048(3) 0.049(3) 0.004(2) 0.006(2) 0.008(2) O2 0.079(4) 0.064(4) 0.090(4) 0.022(3) 0.035(4) 0.016(3) O3 0.035(3) 0.039(3) 0.047(3) 0.010(2) 0.005(2) -0.001(2) O4 0.037(2) 0.051(3) 0.025(2) 0.0014(19) 0.0051(18) 0.003(2) O5 0.022(2) 0.054(3) 0.027(2) 0.0115(19) 0.0007(16) -0.0028(19) F1 0.238(9) 0.091(4) 0.046(3) -0.025(3) 0.021(4) -0.060(5) F2 0.059(3) 0.100(4) 0.040(2) -0.010(2) 0.007(2) -0.022(3) F3 0.097(4) 0.100(4) 0.075(3) 0.044(3) 0.043(3) 0.027(3) F4 0.059(4) 0.245(9) 0.062(3) 0.006(4) 0.012(3) 0.011(5) F5 0.100(6) 0.379(14) 0.107(5) 0.118(7) 0.042(4) 0.119(8) F6 0.342(15) 0.069(4) 0.191(8) -0.030(5) 0.153(10) -0.028(6) P1 0.0240(8) 0.0377(9) 0.0224(7) 0.0028(6) 0.0028(6) 0.0003(7) Cl1 0.0272(7) 0.0316(7) 0.0260(7) -0.0010(6) 0.0075(6) -0.0018(6) Ru1 0.0210(3) 0.0331(3) 0.0212(2) -0.00022(19) 0.00417(17) -0.0015(2) Sb1 0.0570(4) 0.0574(4) 0.0461(3) -0.0007(2) 0.0154(2) -0.0020(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.394(8) . ? C1 C2 1.420(9) . ? C1 Ru1 2.229(6) . ? C1 H1 0.9400 . ? C2 C3 1.397(9) . ? C2 Ru1 2.183(5) . ? C2 H2 0.9400 . ? C3 C4 1.440(8) . ? C3 Ru1 2.214(5) . ? C3 H3 0.9400 . ? C4 O1 1.327(7) . ? C4 C5 1.423(9) . ? C4 Ru1 2.340(6) . ? C5 C6 1.423(9) . ? C5 Ru1 2.302(6) . ? C5 H5 0.9400 . ? C6 Ru1 2.228(6) . ? C6 H6 0.9400 . ? C7 O1 1.451(8) . ? C7 C8 1.508(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 O2 1.421(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.378(9) . ? C9 C14 1.391(11) . ? C9 O3 1.417(8) . ? C10 C11 1.392(11) . ? C10 H10 0.9400 . ? C11 C12 1.399(13) . ? C11 H11 0.9400 . ? C12 C13 1.362(13) . ? C12 H12 0.9400 . ? C13 C14 1.363(12) . ? C13 H13 0.9400 . ? C14 H14 0.9400 . ? C15 C16 1.364(9) . ? C15 C20 1.389(9) . ? C15 O4 1.412(8) . ? C16 C17 1.398(10) . ? C16 H16 0.9400 . ? C17 C18 1.402(10) . ? C17 H17 0.9400 . ? C18 C19 1.366(12) . ? C18 H18 0.9400 . ? C19 C20 1.363(11) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 C26 1.359(10) . ? C21 C22 1.386(10) . ? C21 O5 1.431(7) . ? C22 C23 1.398(11) . ? C22 H22 0.9400 . ? C23 C24 1.377(14) . ? C23 H23 0.9400 . ? C24 C25 1.365(13) . ? C24 H24 0.9400 . ? C25 C26 1.384(10) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? O2 H2A 0.8300 . ? O3 P1 1.586(5) . ? O4 P1 1.595(4) . ? O5 P1 1.583(4) . ? F1 Sb1 1.819(5) . ? F2 Sb1 1.864(4) . ? F3 Sb1 1.879(4) . ? F4 Sb1 1.835(6) . ? F5 Sb1 1.827(7) . ? F6 Sb1 1.850(8) . ? P1 Ru1 2.2842(16) . ? Cl1 Ru1 2.4290(13) . ? Cl1 Ru1 2.4363(14) 3_556 ? Ru1 Cl1 2.4363(14) 3_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.6(6) . . ? C6 C1 Ru1 71.7(3) . . ? C2 C1 Ru1 69.5(3) . . ? C6 C1 H1 120.7 . . ? C2 C1 H1 120.7 . . ? Ru1 C1 H1 130.5 . . ? C3 C2 C1 122.0(6) . . ? C3 C2 Ru1 72.7(3) . . ? C1 C2 Ru1 73.0(3) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? Ru1 C2 H2 127.5 . . ? C2 C3 C4 118.7(6) . . ? C2 C3 Ru1 70.3(3) . . ? C4 C3 Ru1 76.4(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? Ru1 C3 H3 124.2 . . ? O1 C4 C5 116.3(6) . . ? O1 C4 C3 124.1(6) . . ? C5 C4 C3 119.4(6) . . ? O1 C4 Ru1 130.8(4) . . ? C5 C4 Ru1 70.7(3) . . ? C3 C4 Ru1 66.9(3) . . ? C6 C5 C4 119.3(5) . . ? C6 C5 Ru1 68.9(3) . . ? C4 C5 Ru1 73.6(3) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? Ru1 C5 H5 129.5 . . ? C1 C6 C5 121.4(6) . . ? C1 C6 Ru1 71.8(3) . . ? C5 C6 Ru1 74.6(3) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? Ru1 C6 H6 126.2 . . ? O1 C7 C8 106.6(6) . . ? O1 C7 H7A 110.4 . . ? C8 C7 H7A 110.4 . . ? O1 C7 H7B 110.4 . . ? C8 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? O2 C8 C7 106.3(6) . . ? O2 C8 H8A 110.5 . . ? C7 C8 H8A 110.5 . . ? O2 C8 H8B 110.5 . . ? C7 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? C10 C9 C14 123.0(7) . . ? C10 C9 O3 120.6(7) . . ? C14 C9 O3 116.4(6) . . ? C9 C10 C11 117.6(8) . . ? C9 C10 H10 121.2 . . ? C11 C10 H10 121.2 . . ? C10 C11 C12 119.1(8) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 121.5(9) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 120.3(10) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C9 118.3(8) . . ? C13 C14 H14 120.8 . . ? C9 C14 H14 120.8 . . ? C16 C15 C20 121.8(6) . . ? C16 C15 O4 122.5(5) . . ? C20 C15 O4 115.7(6) . . ? C15 C16 C17 119.0(6) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C18 119.4(7) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 119.5(7) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C20 C19 C18 121.7(7) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C19 C20 C15 118.6(7) . . ? C19 C20 H20 120.7 . . ? C15 C20 H20 120.7 . . ? C26 C21 C22 123.7(7) . . ? C26 C21 O5 119.1(6) . . ? C22 C21 O5 117.2(6) . . ? C21 C22 C23 116.7(9) . . ? C21 C22 H22 121.6 . . ? C23 C22 H22 121.6 . . ? C24 C23 C22 119.8(9) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 121.6(8) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C24 C25 C26 119.7(9) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C21 C26 C25 118.4(8) . . ? C21 C26 H26 120.8 . . ? C25 C26 H26 120.8 . . ? C4 O1 C7 119.3(5) . . ? C8 O2 H2A 109.5 . . ? C9 O3 P1 125.0(4) . . ? C15 O4 P1 123.9(4) . . ? C21 O5 P1 122.3(4) . . ? O5 P1 O3 98.8(2) . . ? O5 P1 O4 105.7(2) . . ? O3 P1 O4 98.6(2) . . ? O5 P1 Ru1 115.95(16) . . ? O3 P1 Ru1 117.30(18) . . ? O4 P1 Ru1 117.52(17) . . ? Ru1 Cl1 Ru1 100.09(5) . 3_556 ? C2 Ru1 C3 37.1(2) . . ? C2 Ru1 C6 66.5(2) . . ? C3 Ru1 C6 79.1(2) . . ? C2 Ru1 C1 37.5(2) . . ? C3 Ru1 C1 67.4(2) . . ? C6 Ru1 C1 36.4(2) . . ? C2 Ru1 P1 88.45(17) . . ? C3 Ru1 P1 107.47(16) . . ? C6 Ru1 P1 128.94(17) . . ? C1 Ru1 P1 97.91(16) . . ? C2 Ru1 C5 77.7(2) . . ? C3 Ru1 C5 66.3(2) . . ? C6 Ru1 C5 36.6(2) . . ? C1 Ru1 C5 65.6(2) . . ? P1 Ru1 C5 163.50(16) . . ? C2 Ru1 C4 65.2(2) . . ? C3 Ru1 C4 36.8(2) . . ? C6 Ru1 C4 65.0(2) . . ? C1 Ru1 C4 77.0(2) . . ? P1 Ru1 C4 143.35(17) . . ? C5 Ru1 C4 35.7(2) . . ? C2 Ru1 Cl1 147.68(18) . . ? C3 Ru1 Cl1 163.79(17) . . ? C6 Ru1 Cl1 90.88(16) . . ? C1 Ru1 Cl1 111.36(17) . . ? P1 Ru1 Cl1 88.75(5) . . ? C5 Ru1 Cl1 98.07(15) . . ? C4 Ru1 Cl1 127.21(16) . . ? C2 Ru1 Cl1 132.39(17) . 3_556 ? C3 Ru1 Cl1 98.72(16) . 3_556 ? C6 Ru1 Cl1 137.12(16) . 3_556 ? C1 Ru1 Cl1 164.42(17) . 3_556 ? P1 Ru1 Cl1 92.93(5) . 3_556 ? C5 Ru1 Cl1 103.02(16) . 3_556 ? C4 Ru1 Cl1 87.61(15) . 3_556 ? Cl1 Ru1 Cl1 79.91(5) . 3_556 ? F1 Sb1 F5 93.6(5) . . ? F1 Sb1 F4 90.1(4) . . ? F5 Sb1 F4 175.7(5) . . ? F1 Sb1 F6 176.9(5) . . ? F5 Sb1 F6 89.6(6) . . ? F4 Sb1 F6 86.8(5) . . ? F1 Sb1 F2 90.9(2) . . ? F5 Sb1 F2 91.0(3) . . ? F4 Sb1 F2 91.4(2) . . ? F6 Sb1 F2 89.1(3) . . ? F1 Sb1 F3 88.2(3) . . ? F5 Sb1 F3 87.8(3) . . ? F4 Sb1 F3 89.9(3) . . ? F6 Sb1 F3 91.9(3) . . ? F2 Sb1 F3 178.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.8(8) . . . . ? Ru1 C1 C2 C3 -56.0(5) . . . . ? C6 C1 C2 Ru1 54.2(5) . . . . ? C1 C2 C3 C4 -5.0(8) . . . . ? Ru1 C2 C3 C4 -61.2(5) . . . . ? C1 C2 C3 Ru1 56.2(5) . . . . ? C2 C3 C4 O1 -177.3(5) . . . . ? Ru1 C3 C4 O1 124.7(5) . . . . ? C2 C3 C4 C5 8.8(8) . . . . ? Ru1 C3 C4 C5 -49.3(5) . . . . ? C2 C3 C4 Ru1 58.1(5) . . . . ? O1 C4 C5 C6 179.8(5) . . . . ? C3 C4 C5 C6 -5.8(8) . . . . ? Ru1 C4 C5 C6 -53.4(5) . . . . ? O1 C4 C5 Ru1 -126.8(5) . . . . ? C3 C4 C5 Ru1 47.6(5) . . . . ? C2 C1 C6 C5 5.0(8) . . . . ? Ru1 C1 C6 C5 58.1(5) . . . . ? C2 C1 C6 Ru1 -53.1(5) . . . . ? C4 C5 C6 C1 -1.1(8) . . . . ? Ru1 C5 C6 C1 -56.8(5) . . . . ? C4 C5 C6 Ru1 55.7(5) . . . . ? O1 C7 C8 O2 74.6(8) . . . . ? C14 C9 C10 C11 1.7(11) . . . . ? O3 C9 C10 C11 179.8(6) . . . . ? C9 C10 C11 C12 0.2(11) . . . . ? C10 C11 C12 C13 -2.0(14) . . . . ? C11 C12 C13 C14 2.0(16) . . . . ? C12 C13 C14 C9 0.0(15) . . . . ? C10 C9 C14 C13 -1.9(13) . . . . ? O3 C9 C14 C13 180.0(8) . . . . ? C20 C15 C16 C17 2.8(10) . . . . ? O4 C15 C16 C17 -179.0(6) . . . . ? C15 C16 C17 C18 -0.6(10) . . . . ? C16 C17 C18 C19 -1.2(11) . . . . ? C17 C18 C19 C20 0.9(12) . . . . ? C18 C19 C20 C15 1.2(11) . . . . ? C16 C15 C20 C19 -3.1(10) . . . . ? O4 C15 C20 C19 178.6(6) . . . . ? C26 C21 C22 C23 1.1(10) . . . . ? O5 C21 C22 C23 179.0(6) . . . . ? C21 C22 C23 C24 -0.4(11) . . . . ? C22 C23 C24 C25 -0.8(12) . . . . ? C23 C24 C25 C26 1.5(11) . . . . ? C22 C21 C26 C25 -0.4(10) . . . . ? O5 C21 C26 C25 -178.4(5) . . . . ? C24 C25 C26 C21 -0.8(10) . . . . ? C5 C4 O1 C7 173.5(5) . . . . ? C3 C4 O1 C7 -0.6(8) . . . . ? Ru1 C4 O1 C7 87.0(7) . . . . ? C8 C7 O1 C4 -178.0(6) . . . . ? C10 C9 O3 P1 74.8(7) . . . . ? C14 C9 O3 P1 -107.0(7) . . . . ? C16 C15 O4 P1 40.3(8) . . . . ? C20 C15 O4 P1 -141.4(5) . . . . ? C26 C21 O5 P1 -81.4(6) . . . . ? C22 C21 O5 P1 100.5(6) . . . . ? C21 O5 P1 O3 44.9(5) . . . . ? C21 O5 P1 O4 -56.7(5) . . . . ? C21 O5 P1 Ru1 171.1(4) . . . . ? C9 O3 P1 O5 169.4(5) . . . . ? C9 O3 P1 O4 -83.0(5) . . . . ? C9 O3 P1 Ru1 44.1(5) . . . . ? C15 O4 P1 O5 -89.4(5) . . . . ? C15 O4 P1 O3 168.8(5) . . . . ? C15 O4 P1 Ru1 41.8(5) . . . . ? C1 C2 Ru1 C3 -132.6(5) . . . . ? C3 C2 Ru1 C6 103.5(4) . . . . ? C1 C2 Ru1 C6 -29.1(4) . . . . ? C3 C2 Ru1 C1 132.6(5) . . . . ? C3 C2 Ru1 P1 -122.3(3) . . . . ? C1 C2 Ru1 P1 105.1(3) . . . . ? C3 C2 Ru1 C5 66.8(4) . . . . ? C1 C2 Ru1 C5 -65.8(4) . . . . ? C3 C2 Ru1 C4 31.4(4) . . . . ? C1 C2 Ru1 C4 -101.2(4) . . . . ? C3 C2 Ru1 Cl1 152.5(3) . . . . ? C1 C2 Ru1 Cl1 19.9(6) . . . . ? C3 C2 Ru1 Cl1 -29.7(4) . . . 3_556 ? C1 C2 Ru1 Cl1 -162.3(3) . . . 3_556 ? C4 C3 Ru1 C2 127.8(5) . . . . ? C2 C3 Ru1 C6 -65.2(4) . . . . ? C4 C3 Ru1 C6 62.5(4) . . . . ? C2 C3 Ru1 C1 -29.1(4) . . . . ? C4 C3 Ru1 C1 98.7(4) . . . . ? C2 C3 Ru1 P1 62.4(4) . . . . ? C4 C3 Ru1 P1 -169.9(3) . . . . ? C2 C3 Ru1 C5 -101.3(4) . . . . ? C4 C3 Ru1 C5 26.5(3) . . . . ? C2 C3 Ru1 C4 -127.8(5) . . . . ? C2 C3 Ru1 Cl1 -117.9(6) . . . . ? C4 C3 Ru1 Cl1 9.8(8) . . . . ? C2 C3 Ru1 Cl1 158.3(3) . . . 3_556 ? C4 C3 Ru1 Cl1 -74.0(3) . . . 3_556 ? C1 C6 Ru1 C2 29.9(4) . . . . ? C5 C6 Ru1 C2 -101.4(4) . . . . ? C1 C6 Ru1 C3 66.5(4) . . . . ? C5 C6 Ru1 C3 -64.8(4) . . . . ? C5 C6 Ru1 C1 -131.3(5) . . . . ? C1 C6 Ru1 P1 -37.2(4) . . . . ? C5 C6 Ru1 P1 -168.5(3) . . . . ? C1 C6 Ru1 C5 131.3(5) . . . . ? C1 C6 Ru1 C4 102.4(4) . . . . ? C5 C6 Ru1 C4 -28.9(3) . . . . ? C1 C6 Ru1 Cl1 -126.3(4) . . . . ? C5 C6 Ru1 Cl1 102.4(3) . . . . ? C1 C6 Ru1 Cl1 157.6(3) . . . 3_556 ? C5 C6 Ru1 Cl1 26.4(5) . . . 3_556 ? C6 C1 Ru1 C2 -131.4(6) . . . . ? C6 C1 Ru1 C3 -102.7(4) . . . . ? C2 C1 Ru1 C3 28.7(4) . . . . ? C2 C1 Ru1 C6 131.4(6) . . . . ? C6 C1 Ru1 P1 151.6(3) . . . . ? C2 C1 Ru1 P1 -77.0(4) . . . . ? C6 C1 Ru1 C5 -29.5(4) . . . . ? C2 C1 Ru1 C5 102.0(4) . . . . ? C6 C1 Ru1 C4 -65.3(4) . . . . ? C2 C1 Ru1 C4 66.1(4) . . . . ? C6 C1 Ru1 Cl1 59.9(4) . . . . ? C2 C1 Ru1 Cl1 -168.7(3) . . . . ? C6 C1 Ru1 Cl1 -74.7(7) . . . 3_556 ? C2 C1 Ru1 Cl1 56.7(7) . . . 3_556 ? O5 P1 Ru1 C2 159.3(3) . . . . ? O3 P1 Ru1 C2 -84.4(3) . . . . ? O4 P1 Ru1 C2 32.9(3) . . . . ? O5 P1 Ru1 C3 127.1(3) . . . . ? O3 P1 Ru1 C3 -116.7(3) . . . . ? O4 P1 Ru1 C3 0.6(3) . . . . ? O5 P1 Ru1 C6 -143.0(3) . . . . ? O3 P1 Ru1 C6 -26.7(3) . . . . ? O4 P1 Ru1 C6 90.6(3) . . . . ? O5 P1 Ru1 C1 -164.3(3) . . . . ? O3 P1 Ru1 C1 -48.0(3) . . . . ? O4 P1 Ru1 C1 69.3(3) . . . . ? O5 P1 Ru1 C5 -167.7(6) . . . . ? O3 P1 Ru1 C5 -51.5(6) . . . . ? O4 P1 Ru1 C5 65.8(6) . . . . ? O5 P1 Ru1 C4 116.9(3) . . . . ? O3 P1 Ru1 C4 -126.8(3) . . . . ? O4 P1 Ru1 C4 -9.5(3) . . . . ? O5 P1 Ru1 Cl1 -52.9(2) . . . . ? O3 P1 Ru1 Cl1 63.42(19) . . . . ? O4 P1 Ru1 Cl1 -179.3(2) . . . . ? O5 P1 Ru1 Cl1 27.0(2) . . . 3_556 ? O3 P1 Ru1 Cl1 143.24(19) . . . 3_556 ? O4 P1 Ru1 Cl1 -99.5(2) . . . 3_556 ? C6 C5 Ru1 C2 66.9(4) . . . . ? C4 C5 Ru1 C2 -64.4(4) . . . . ? C6 C5 Ru1 C3 104.1(4) . . . . ? C4 C5 Ru1 C3 -27.2(3) . . . . ? C4 C5 Ru1 C6 -131.3(5) . . . . ? C6 C5 Ru1 C1 29.4(3) . . . . ? C4 C5 Ru1 C1 -102.0(4) . . . . ? C6 C5 Ru1 P1 33.2(8) . . . . ? C4 C5 Ru1 P1 -98.2(6) . . . . ? C6 C5 Ru1 C4 131.3(5) . . . . ? C6 C5 Ru1 Cl1 -80.5(3) . . . . ? C4 C5 Ru1 Cl1 148.2(3) . . . . ? C6 C5 Ru1 Cl1 -161.9(3) . . . 3_556 ? C4 C5 Ru1 Cl1 66.7(3) . . . 3_556 ? O1 C4 Ru1 C2 -147.6(7) . . . . ? C5 C4 Ru1 C2 103.9(4) . . . . ? C3 C4 Ru1 C2 -31.6(4) . . . . ? O1 C4 Ru1 C3 -115.9(7) . . . . ? C5 C4 Ru1 C3 135.6(5) . . . . ? O1 C4 Ru1 C6 138.1(7) . . . . ? C5 C4 Ru1 C6 29.6(3) . . . . ? C3 C4 Ru1 C6 -106.0(4) . . . . ? O1 C4 Ru1 C1 174.6(6) . . . . ? C5 C4 Ru1 C1 66.1(4) . . . . ? C3 C4 Ru1 C1 -69.5(4) . . . . ? O1 C4 Ru1 P1 -99.6(6) . . . . ? C5 C4 Ru1 P1 151.9(3) . . . . ? C3 C4 Ru1 P1 16.3(5) . . . . ? O1 C4 Ru1 C5 108.5(7) . . . . ? C3 C4 Ru1 C5 -135.6(5) . . . . ? O1 C4 Ru1 Cl1 67.5(6) . . . . ? C5 C4 Ru1 Cl1 -41.0(4) . . . . ? C3 C4 Ru1 Cl1 -176.6(3) . . . . ? O1 C4 Ru1 Cl1 -7.9(6) . . . 3_556 ? C5 C4 Ru1 Cl1 -116.4(3) . . . 3_556 ? C3 C4 Ru1 Cl1 108.0(3) . . . 3_556 ? Ru1 Cl1 Ru1 C2 178.3(3) 3_556 . . . ? Ru1 Cl1 Ru1 C3 -86.5(6) 3_556 . . . ? Ru1 Cl1 Ru1 C6 -137.87(17) 3_556 . . . ? Ru1 Cl1 Ru1 C1 -168.79(17) 3_556 . . . ? Ru1 Cl1 Ru1 P1 93.20(6) 3_556 . . . ? Ru1 Cl1 Ru1 C5 -101.88(17) 3_556 . . . ? Ru1 Cl1 Ru1 C4 -79.1(2) 3_556 . . . ? Ru1 Cl1 Ru1 Cl1 0.0 3_556 . . 3_556 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.695 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.227 data_3 _database_code_depnum_ccdc_archive 'CCDC 908514' #TrackingRef '2_3_5a.cif' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H50 Cl3 O4 P2 Ru2, F6 Sb, 2(C4 H10 O)' _chemical_formula_sum 'C60 H70 Cl3 F6 O6 P2 Ru2 Sb' _chemical_formula_weight 1493.34 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.3423(11) _cell_length_b 14.4711(7) _cell_length_c 15.0960(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.850(4) _cell_angle_gamma 90.00 _cell_volume 6213.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6905 _cell_measurement_theta_min 3.1060 _cell_measurement_theta_max 66.6755 _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.316 _exptl_crystal_size_mid 0.085 _exptl_crystal_size_min 0.037 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 9.543 _exptl_absorpt_correction_T_min 0.32744 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur Nova ; _diffrn_measurement_device ; 165 mm Onyx CCD detector in \k-geometry diffractometer ; _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 16.0827 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17101 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_unetI/netI 0.0427 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 66.98 _reflns_number_total 5479 _reflns_number_gt 4378 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5479 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1206 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.10690(17) 0.0229(4) 0.7168(4) 0.0373(11) Uani 1 1 d . . . H1 H 0.1174 -0.0252 0.6903 0.045 Uiso 1 1 calc R . . C25 C 0.2133(2) -0.2183(5) 0.8423(4) 0.0570(17) Uani 1 1 d . . . H25 H 0.2458 -0.2250 0.8733 0.068 Uiso 1 1 calc R . . C6 C 0.06129(16) 0.0570(4) 0.6693(3) 0.0335(11) Uani 1 1 d . . . H6 H 0.0402 0.0270 0.6136 0.040 Uiso 1 1 calc R . . C5 C 0.04602(16) 0.1365(4) 0.7036(3) 0.0343(11) Uani 1 1 d . . . H5 H 0.0157 0.1592 0.6694 0.041 Uiso 1 1 calc R . . C4 C 0.07675(17) 0.1795(4) 0.7883(4) 0.0362(11) Uani 1 1 d . . . C3 C 0.12167(16) 0.1391(4) 0.8459(4) 0.0395(12) Uani 1 1 d . . . H3 H 0.1404 0.1620 0.9077 0.047 Uiso 1 1 calc R . . C2 C 0.13696(16) 0.0642(4) 0.8075(4) 0.0408(13) Uani 1 1 d . . . H2 H 0.1672 0.0412 0.8417 0.049 Uiso 1 1 calc R . . C7 C 0.0874(3) 0.3017(5) 0.9027(6) 0.0690(8) Uani 1 1 d . . . H7A H 0.1168 0.3216 0.9019 0.083 Uiso 1 1 calc R . . H7B H 0.0943 0.2622 0.9590 0.083 Uiso 1 1 calc R . . C8 C 0.0585(3) 0.3836(5) 0.9059(6) 0.0690(8) Uani 1 1 d . . . H8A H 0.0301 0.3621 0.9102 0.083 Uiso 1 1 calc R . . H8B H 0.0763 0.4199 0.9638 0.083 Uiso 1 1 calc R . . C26 C 0.18942(19) -0.1786(4) 0.8923(4) 0.0460(14) Uani 1 1 d . . . H26 H 0.2060 -0.1582 0.9562 0.055 Uiso 1 1 calc R . . C12 C 0.21920(18) -0.0740(5) 1.2197(4) 0.0513(17) Uani 1 1 d . . . H12 H 0.2423 -0.0671 1.2830 0.062 Uiso 1 1 calc R . . C19 C 0.0055(2) -0.2371(4) 0.9601(4) 0.0440(13) Uani 1 1 d . . . H19 H -0.0147 -0.2199 0.9880 0.053 Uiso 1 1 calc R . . C16 C 0.0664(2) -0.2885(4) 0.8796(5) 0.0514(14) Uani 1 1 d . . . H16 H 0.0870 -0.3066 0.8530 0.062 Uiso 1 1 calc R . . C18 C 0.0041(2) -0.3267(4) 0.9252(4) 0.0543(15) Uani 1 1 d . . . H18 H -0.0172 -0.3694 0.9291 0.065 Uiso 1 1 calc R . . C10 C 0.17446(17) -0.0129(5) 1.0601(4) 0.0435(13) Uani 1 1 d . . . H10 H 0.1674 0.0357 1.0160 0.052 Uiso 1 1 calc R . . C21 C 0.14117(18) -0.1693(4) 0.8473(4) 0.0401(12) Uani 1 1 d . . . C23 C 0.1406(3) -0.2384(5) 0.7019(4) 0.0620(19) Uani 1 1 d . . . H23 H 0.1241 -0.2588 0.6380 0.074 Uiso 1 1 calc R . . C17 C 0.0343(3) -0.3514(5) 0.8853(5) 0.0639(18) Uani 1 1 d . . . H17 H 0.0333 -0.4111 0.8617 0.077 Uiso 1 1 calc R . . C20 C 0.03683(18) -0.1738(4) 0.9531(3) 0.0358(11) Uani 1 1 d . . . H20 H 0.0371 -0.1137 0.9753 0.043 Uiso 1 1 calc R . . C11 C 0.20935(18) -0.0017(5) 1.1555(4) 0.0514(16) Uani 1 1 d . . . H11 H 0.2255 0.0539 1.1747 0.062 Uiso 1 1 calc R . . C9 C 0.15082(15) -0.0943(4) 1.0318(3) 0.0381(12) Uani 1 1 d . . . C15 C 0.06807(16) -0.1988(4) 0.9133(3) 0.0356(11) Uani 1 1 d . . . C14 C 0.16103(17) -0.1673(5) 1.0975(4) 0.0436(13) Uani 1 1 d . . . H14 H 0.1449 -0.2229 1.0782 0.052 Uiso 1 1 calc R . . C22 C 0.1166(2) -0.1991(5) 0.7508(4) 0.0521(15) Uani 1 1 d . . . H22 H 0.0841 -0.1923 0.7197 0.063 Uiso 1 1 calc R . . C24 C 0.1890(2) -0.2479(5) 0.7468(5) 0.0624(19) Uani 1 1 d . . . H24 H 0.2051 -0.2737 0.7132 0.075 Uiso 1 1 calc R . . C13 C 0.19547(18) -0.1567(5) 1.1921(4) 0.0487(15) Uani 1 1 d . . . H13 H 0.2025 -0.2051 1.2364 0.058 Uiso 1 1 calc R . . C27 C 0.6736(4) 0.9651(8) 0.4967(10) 0.128(5) Uani 1 1 d . . . H27A H 0.6758 1.0270 0.5211 0.191 Uiso 1 1 calc R . . H27B H 0.6989 0.9286 0.5421 0.191 Uiso 1 1 calc R . . H27C H 0.6441 0.9385 0.4885 0.191 Uiso 1 1 calc R . . C28 C 0.6768(4) 0.9670(9) 0.3965(9) 0.118(4) Uani 1 1 d . . . H28A H 0.7049 0.9999 0.4033 0.141 Uiso 1 1 calc R . . H28B H 0.6790 0.9042 0.3763 0.141 Uiso 1 1 calc R . . C29 C 0.6370(4) 1.0242(9) 0.2245(9) 0.118(2) Uani 1 1 d . . . H29A H 0.6673 1.0480 0.2322 0.142 Uiso 1 1 calc R . . H29B H 0.6321 0.9652 0.1911 0.142 Uiso 1 1 calc R . . C30 C 0.6007(4) 1.0874(11) 0.1667(8) 0.145(6) Uani 1 1 d . . . H30A H 0.5708 1.0644 0.1600 0.218 Uiso 1 1 calc R . . H30B H 0.6006 1.0936 0.1033 0.218 Uiso 1 1 calc R . . H30C H 0.6064 1.1467 0.1983 0.218 Uiso 1 1 calc R . . Cl2 Cl 0.05940(3) 0.06622(8) 0.95995(7) 0.0284(2) Uani 1 1 d . . . Cl1 Cl 0.0000 -0.06236(11) 0.7500 0.0259(3) Uani 1 2 d S . . F1 F 0.29544(12) 0.2054(3) 0.1187(2) 0.0627(10) Uani 1 1 d . . . F2 F 0.23851(12) 0.1290(3) -0.0493(2) 0.0597(9) Uani 1 1 d . . . F3 F 0.20349(12) 0.2351(3) 0.0454(3) 0.0677(12) Uani 1 1 d . . . O1 O 0.0592(2) 0.2537(3) 0.8147(4) 0.0690(8) Uani 1 1 d . . . O2 O 0.0462(2) 0.4399(3) 0.8222(4) 0.0690(8) Uani 1 1 d . . . H2A H 0.0700 0.4540 0.8155 0.103 Uiso 1 1 calc R . . O3 O 0.6372(3) 1.0103(6) 0.3247(7) 0.118(2) Uani 1 1 d . . . P1 P 0.10791(4) -0.11005(10) 0.90485(8) 0.0328(3) Uani 1 1 d . . . Ru1 Ru 0.072937(10) 0.02453(3) 0.81905(2) 0.02570(12) Uani 1 1 d . . . Sb1 Sb 0.2500 0.2500 0.0000 0.04463(17) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(2) 0.059(3) 0.033(2) 0.000(2) 0.018(2) -0.003(2) C25 0.043(3) 0.090(5) 0.044(3) 0.017(3) 0.025(3) 0.030(3) C6 0.028(2) 0.050(3) 0.025(2) 0.003(2) 0.0132(18) -0.007(2) C5 0.028(2) 0.044(3) 0.031(2) 0.006(2) 0.0116(19) -0.007(2) C4 0.036(2) 0.044(3) 0.032(2) 0.003(2) 0.017(2) -0.006(2) C3 0.028(2) 0.061(4) 0.029(2) -0.001(2) 0.0115(19) -0.014(2) C2 0.020(2) 0.067(4) 0.036(3) 0.008(3) 0.0123(19) -0.009(2) C7 0.091(2) 0.0539(16) 0.0669(17) -0.0093(13) 0.0377(16) -0.0120(15) C8 0.091(2) 0.0539(16) 0.0669(17) -0.0093(13) 0.0377(16) -0.0120(15) C26 0.039(3) 0.067(4) 0.038(3) 0.012(3) 0.022(2) 0.026(3) C12 0.026(2) 0.103(5) 0.024(2) 0.005(3) 0.010(2) 0.019(3) C19 0.059(3) 0.041(3) 0.039(3) -0.001(2) 0.027(3) -0.007(3) C16 0.060(4) 0.043(3) 0.059(4) -0.001(3) 0.033(3) 0.013(3) C18 0.077(4) 0.042(3) 0.048(3) 0.001(3) 0.030(3) -0.008(3) C10 0.024(2) 0.075(4) 0.030(3) 0.007(3) 0.010(2) 0.008(2) C21 0.036(3) 0.055(3) 0.032(2) 0.005(2) 0.017(2) 0.018(2) C23 0.072(4) 0.080(5) 0.031(3) 0.006(3) 0.017(3) 0.035(4) C17 0.091(5) 0.034(3) 0.072(4) -0.005(3) 0.039(4) 0.007(3) C20 0.042(3) 0.036(3) 0.031(2) 0.001(2) 0.017(2) 0.001(2) C11 0.026(3) 0.092(5) 0.031(3) -0.003(3) 0.007(2) 0.003(3) C9 0.022(2) 0.069(4) 0.024(2) 0.005(2) 0.0105(18) 0.012(2) C15 0.034(2) 0.039(3) 0.029(2) 0.002(2) 0.0085(19) 0.011(2) C14 0.030(2) 0.069(4) 0.036(3) 0.008(3) 0.018(2) 0.020(2) C22 0.046(3) 0.072(4) 0.036(3) 0.002(3) 0.015(2) 0.030(3) C24 0.065(4) 0.080(5) 0.057(4) 0.019(3) 0.040(3) 0.043(4) C13 0.033(3) 0.084(5) 0.031(3) 0.015(3) 0.016(2) 0.026(3) C27 0.099(8) 0.114(10) 0.148(12) 0.021(8) 0.031(8) -0.033(7) C28 0.115(9) 0.120(10) 0.123(9) 0.022(8) 0.055(8) 0.027(7) C29 0.117(5) 0.129(6) 0.128(5) 0.002(4) 0.070(5) 0.019(4) C30 0.119(9) 0.239(18) 0.072(6) 0.031(9) 0.035(6) 0.065(11) Cl2 0.0224(5) 0.0379(6) 0.0246(5) -0.0012(4) 0.0096(4) -0.0011(4) Cl1 0.0178(6) 0.0322(8) 0.0261(7) 0.000 0.0076(5) 0.000 F1 0.0489(19) 0.091(3) 0.0336(16) -0.0130(18) 0.0027(13) -0.0138(19) F2 0.0508(19) 0.070(2) 0.0469(18) -0.0186(17) 0.0097(15) -0.0185(17) F3 0.0437(18) 0.122(4) 0.0466(19) -0.022(2) 0.0279(16) -0.029(2) O1 0.091(2) 0.0539(16) 0.0669(17) -0.0093(13) 0.0377(16) -0.0120(15) O2 0.091(2) 0.0539(16) 0.0669(17) -0.0093(13) 0.0377(16) -0.0120(15) O3 0.117(5) 0.129(6) 0.128(5) 0.002(4) 0.070(5) 0.019(4) P1 0.0232(5) 0.0491(8) 0.0263(5) 0.0035(5) 0.0104(4) 0.0105(5) Ru1 0.01489(18) 0.0391(2) 0.02241(18) 0.00074(13) 0.00713(13) -0.00080(13) Sb1 0.0295(2) 0.0758(4) 0.0278(2) -0.0146(2) 0.01124(18) -0.0212(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.393(7) . ? C1 C2 1.426(8) . ? C1 Ru1 2.212(5) . ? C1 H1 0.9300 . ? C25 C24 1.386(10) . ? C25 C26 1.390(8) . ? C25 H25 0.9300 . ? C6 C5 1.424(8) . ? C6 Ru1 2.184(4) . ? C6 H6 0.9300 . ? C5 C4 1.384(7) . ? C5 Ru1 2.267(5) . ? C5 H5 0.9300 . ? C4 O1 1.341(8) . ? C4 C3 1.432(7) . ? C4 Ru1 2.304(5) . ? C3 C2 1.405(8) . ? C3 Ru1 2.174(5) . ? C3 H3 0.9300 . ? C2 Ru1 2.164(4) . ? C2 H2 0.9300 . ? C7 O1 1.429(9) . ? C7 C8 1.504(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O2 1.414(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C26 C21 1.379(7) . ? C26 H26 0.9300 . ? C12 C11 1.371(10) . ? C12 C13 1.378(10) . ? C12 H12 0.9300 . ? C19 C20 1.378(8) . ? C19 C18 1.394(8) . ? C19 H19 0.9300 . ? C16 C17 1.387(10) . ? C16 C15 1.388(8) . ? C16 H16 0.9300 . ? C18 C17 1.364(10) . ? C18 H18 0.9300 . ? C10 C9 1.362(9) . ? C10 C11 1.403(8) . ? C10 H10 0.9300 . ? C21 C22 1.400(8) . ? C21 P1 1.827(5) . ? C23 C22 1.380(8) . ? C23 C24 1.385(10) . ? C23 H23 0.9300 . ? C17 H17 0.9300 . ? C20 C15 1.395(7) . ? C20 H20 0.9300 . ? C11 H11 0.9300 . ? C9 C14 1.391(8) . ? C9 P1 1.835(5) . ? C15 P1 1.832(6) . ? C14 C13 1.390(8) . ? C14 H14 0.9300 . ? C22 H22 0.9300 . ? C24 H24 0.9300 . ? C13 H13 0.9300 . ? C27 C28 1.556(15) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 O3 1.406(13) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.436(16) . ? C29 O3 1.524(13) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? Cl2 Ru1 2.4139(10) . ? Cl1 Ru1 2.4271(8) . ? Cl1 Ru1 2.4271(8) 2_556 ? F1 Sb1 1.874(3) . ? F2 Sb1 1.878(4) . ? F3 Sb1 1.866(3) . ? O2 H2A 0.8200 . ? P1 Ru1 2.3407(13) . ? Sb1 F3 1.866(3) 7 ? Sb1 F1 1.874(3) 7 ? Sb1 F2 1.878(4) 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 C6 C1 C2 117.8(5) . . ? C6 C1 Ru1 70.4(3) . . ? C2 C1 Ru1 69.1(3) . . ? C6 C1 H1 121.1 . . ? C2 C1 H1 121.1 . . ? Ru1 C1 H1 132.0 . . ? C24 C25 C26 120.6(6) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C1 C6 C5 121.9(5) . . ? C1 C6 Ru1 72.7(3) . . ? C5 C6 Ru1 74.5(3) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? Ru1 C6 H6 125.6 . . ? C4 C5 C6 119.3(5) . . ? C4 C5 Ru1 73.8(3) . . ? C6 C5 Ru1 68.2(3) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? Ru1 C5 H5 130.0 . . ? O1 C4 C5 114.9(5) . . ? O1 C4 C3 124.7(5) . . ? C5 C4 C3 120.1(5) . . ? O1 C4 Ru1 131.1(4) . . ? C5 C4 Ru1 70.9(3) . . ? C3 C4 Ru1 66.5(3) . . ? C2 C3 C4 118.9(5) . . ? C2 C3 Ru1 70.7(3) . . ? C4 C3 Ru1 76.4(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? Ru1 C3 H3 123.9 . . ? C3 C2 C1 121.1(5) . . ? C3 C2 Ru1 71.5(3) . . ? C1 C2 Ru1 72.8(3) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? Ru1 C2 H2 128.5 . . ? O1 C7 C8 105.5(7) . . ? O1 C7 H7A 110.6 . . ? C8 C7 H7A 110.6 . . ? O1 C7 H7B 110.6 . . ? C8 C7 H7B 110.6 . . ? H7A C7 H7B 108.8 . . ? O2 C8 C7 111.5(6) . . ? O2 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? O2 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C21 C26 C25 120.1(6) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C11 C12 C13 121.1(5) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C20 C19 C18 120.0(5) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C17 C16 C15 120.4(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C17 C18 C19 119.5(6) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C9 C10 C11 120.6(6) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C26 C21 C22 119.5(5) . . ? C26 C21 P1 122.6(4) . . ? C22 C21 P1 117.7(4) . . ? C22 C23 C24 120.7(6) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C18 C17 C16 120.8(6) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C20 C15 120.8(5) . . ? C19 C20 H20 119.6 . . ? C15 C20 H20 119.6 . . ? C12 C11 C10 118.9(7) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C10 C9 C14 120.1(5) . . ? C10 C9 P1 119.9(4) . . ? C14 C9 P1 119.9(5) . . ? C16 C15 C20 118.4(5) . . ? C16 C15 P1 123.4(4) . . ? C20 C15 P1 118.1(4) . . ? C13 C14 C9 119.7(6) . . ? C13 C14 H14 120.1 . . ? C9 C14 H14 120.1 . . ? C23 C22 C21 120.0(5) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C23 C24 C25 119.1(5) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C12 C13 C14 119.6(6) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O3 C28 C27 111.2(10) . . ? O3 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? O3 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C30 C29 O3 110.9(9) . . ? C30 C29 H29A 109.5 . . ? O3 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? O3 C29 H29B 109.5 . . ? H29A C29 H29B 108.0 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Ru1 Cl1 Ru1 117.59(6) . 2_556 ? C4 O1 C7 119.6(6) . . ? C8 O2 H2A 109.5 . . ? C28 O3 C29 117.2(9) . . ? C21 P1 C15 104.3(3) . . ? C21 P1 C9 103.9(2) . . ? C15 P1 C9 103.6(2) . . ? C21 P1 Ru1 110.84(18) . . ? C15 P1 Ru1 116.56(15) . . ? C9 P1 Ru1 116.2(2) . . ? C2 Ru1 C3 37.8(2) . . ? C2 Ru1 C6 67.46(18) . . ? C3 Ru1 C6 80.09(19) . . ? C2 Ru1 C1 38.0(2) . . ? C3 Ru1 C1 68.41(19) . . ? C6 Ru1 C1 36.93(19) . . ? C2 Ru1 C5 78.84(19) . . ? C3 Ru1 C5 66.65(18) . . ? C6 Ru1 C5 37.3(2) . . ? C1 Ru1 C5 66.68(19) . . ? C2 Ru1 C4 66.2(2) . . ? C3 Ru1 C4 37.16(19) . . ? C6 Ru1 C4 65.33(19) . . ? C1 Ru1 C4 77.8(2) . . ? C5 Ru1 C4 35.25(18) . . ? C2 Ru1 P1 91.77(16) . . ? C3 Ru1 P1 113.73(15) . . ? C6 Ru1 P1 125.97(15) . . ? C1 Ru1 P1 97.26(15) . . ? C5 Ru1 P1 163.06(13) . . ? C4 Ru1 P1 150.42(13) . . ? C2 Ru1 Cl2 121.15(15) . . ? C3 Ru1 Cl2 90.85(13) . . ? C6 Ru1 Cl2 147.51(14) . . ? C1 Ru1 Cl2 158.66(14) . . ? C5 Ru1 Cl2 110.63(13) . . ? C4 Ru1 Cl2 88.69(13) . . ? P1 Ru1 Cl2 86.28(4) . . ? C2 Ru1 Cl1 147.23(15) . . ? C3 Ru1 Cl1 159.45(15) . . ? C6 Ru1 Cl1 87.09(12) . . ? C1 Ru1 Cl1 109.71(14) . . ? C5 Ru1 Cl1 93.50(12) . . ? C4 Ru1 Cl1 122.49(13) . . ? P1 Ru1 Cl1 86.80(4) . . ? Cl2 Ru1 Cl1 91.45(3) . . ? F3 Sb1 F3 180.0(3) . 7 ? F3 Sb1 F1 90.36(17) . . ? F3 Sb1 F1 89.64(17) 7 . ? F3 Sb1 F1 89.64(17) . 7 ? F3 Sb1 F1 90.36(17) 7 7 ? F1 Sb1 F1 180.0(4) . 7 ? F3 Sb1 F2 89.36(18) . . ? F3 Sb1 F2 90.64(18) 7 . ? F1 Sb1 F2 89.99(17) . . ? F1 Sb1 F2 90.01(17) 7 . ? F3 Sb1 F2 90.64(18) . 7 ? F3 Sb1 F2 89.36(18) 7 7 ? F1 Sb1 F2 90.01(17) . 7 ? F1 Sb1 F2 89.99(17) 7 7 ? F2 Sb1 F2 180.0(2) . 7 ? 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 C2 C1 C6 C5 6.4(7) . . . . ? Ru1 C1 C6 C5 58.4(4) . . . . ? C2 C1 C6 Ru1 -52.0(4) . . . . ? C1 C6 C5 C4 -2.2(7) . . . . ? Ru1 C6 C5 C4 55.4(4) . . . . ? C1 C6 C5 Ru1 -57.6(4) . . . . ? C6 C5 C4 O1 180.0(4) . . . . ? Ru1 C5 C4 O1 -127.3(4) . . . . ? C6 C5 C4 C3 -6.2(7) . . . . ? Ru1 C5 C4 C3 46.5(4) . . . . ? C6 C5 C4 Ru1 -52.7(4) . . . . ? O1 C4 C3 C2 -176.7(5) . . . . ? C5 C4 C3 C2 10.2(7) . . . . ? Ru1 C4 C3 C2 58.5(4) . . . . ? O1 C4 C3 Ru1 124.8(5) . . . . ? C5 C4 C3 Ru1 -48.3(4) . . . . ? C4 C3 C2 C1 -5.8(7) . . . . ? Ru1 C3 C2 C1 55.6(4) . . . . ? C4 C3 C2 Ru1 -61.4(4) . . . . ? C6 C1 C2 C3 -2.3(7) . . . . ? Ru1 C1 C2 C3 -54.9(4) . . . . ? C6 C1 C2 Ru1 52.6(4) . . . . ? O1 C7 C8 O2 -57.7(8) . . . . ? C24 C25 C26 C21 0.8(11) . . . . ? C20 C19 C18 C17 0.7(10) . . . . ? C25 C26 C21 C22 -0.8(10) . . . . ? C25 C26 C21 P1 -175.2(5) . . . . ? C19 C18 C17 C16 0.3(11) . . . . ? C15 C16 C17 C18 -0.8(11) . . . . ? C18 C19 C20 C15 -1.3(8) . . . . ? C13 C12 C11 C10 -0.1(8) . . . . ? C9 C10 C11 C12 -0.1(8) . . . . ? C11 C10 C9 C14 0.2(8) . . . . ? C11 C10 C9 P1 -176.3(4) . . . . ? C17 C16 C15 C20 0.2(9) . . . . ? C17 C16 C15 P1 -177.8(5) . . . . ? C19 C20 C15 C16 0.9(8) . . . . ? C19 C20 C15 P1 179.0(4) . . . . ? C10 C9 C14 C13 -0.1(7) . . . . ? P1 C9 C14 C13 176.4(4) . . . . ? C24 C23 C22 C21 -0.8(12) . . . . ? C26 C21 C22 C23 0.8(10) . . . . ? P1 C21 C22 C23 175.5(6) . . . . ? C22 C23 C24 C25 0.8(12) . . . . ? C26 C25 C24 C23 -0.7(12) . . . . ? C11 C12 C13 C14 0.2(8) . . . . ? C9 C14 C13 C12 -0.1(7) . . . . ? C5 C4 O1 C7 178.0(5) . . . . ? C3 C4 O1 C7 4.6(9) . . . . ? Ru1 C4 O1 C7 92.2(7) . . . . ? C8 C7 O1 C4 176.1(5) . . . . ? C27 C28 O3 C29 175.3(10) . . . . ? C30 C29 O3 C28 -166.3(12) . . . . ? C26 C21 P1 C15 -119.6(5) . . . . ? C22 C21 P1 C15 65.9(5) . . . . ? C26 C21 P1 C9 -11.3(6) . . . . ? C22 C21 P1 C9 174.2(5) . . . . ? C26 C21 P1 Ru1 114.2(5) . . . . ? C22 C21 P1 Ru1 -60.3(6) . . . . ? C16 C15 P1 C21 -0.7(5) . . . . ? C20 C15 P1 C21 -178.8(4) . . . . ? C16 C15 P1 C9 -109.2(5) . . . . ? C20 C15 P1 C9 72.8(4) . . . . ? C16 C15 P1 Ru1 121.7(4) . . . . ? C20 C15 P1 Ru1 -56.3(4) . . . . ? C10 C9 P1 C21 96.3(4) . . . . ? C14 C9 P1 C21 -80.2(4) . . . . ? C10 C9 P1 C15 -155.0(4) . . . . ? C14 C9 P1 C15 28.5(4) . . . . ? C10 C9 P1 Ru1 -25.8(4) . . . . ? C14 C9 P1 Ru1 157.8(3) . . . . ? C1 C2 Ru1 C3 -132.4(5) . . . . ? C3 C2 Ru1 C6 103.3(3) . . . . ? C1 C2 Ru1 C6 -29.0(3) . . . . ? C3 C2 Ru1 C1 132.4(5) . . . . ? C3 C2 Ru1 C5 66.1(3) . . . . ? C1 C2 Ru1 C5 -66.2(3) . . . . ? C3 C2 Ru1 C4 31.5(3) . . . . ? C1 C2 Ru1 C4 -100.9(4) . . . . ? C3 C2 Ru1 P1 -128.1(3) . . . . ? C1 C2 Ru1 P1 99.5(3) . . . . ? C3 C2 Ru1 Cl2 -41.4(3) . . . . ? C1 C2 Ru1 Cl2 -173.7(3) . . . . ? C3 C2 Ru1 Cl1 145.1(3) . . . . ? C1 C2 Ru1 Cl1 12.7(5) . . . . ? C4 C3 Ru1 C2 127.7(4) . . . . ? C2 C3 Ru1 C6 -65.8(3) . . . . ? C4 C3 Ru1 C6 61.9(3) . . . . ? C2 C3 Ru1 C1 -29.3(3) . . . . ? C4 C3 Ru1 C1 98.4(3) . . . . ? C2 C3 Ru1 C5 -102.3(3) . . . . ? C4 C3 Ru1 C5 25.5(3) . . . . ? C2 C3 Ru1 C4 -127.7(4) . . . . ? C2 C3 Ru1 P1 59.2(3) . . . . ? C4 C3 Ru1 P1 -173.0(2) . . . . ? C2 C3 Ru1 Cl2 145.6(3) . . . . ? C4 C3 Ru1 Cl2 -86.7(3) . . . . ? C2 C3 Ru1 Cl1 -118.0(4) . . . . ? C4 C3 Ru1 Cl1 9.7(6) . . . . ? C1 C6 Ru1 C2 29.8(3) . . . . ? C5 C6 Ru1 C2 -101.5(3) . . . . ? C1 C6 Ru1 C3 67.1(3) . . . . ? C5 C6 Ru1 C3 -64.2(3) . . . . ? C5 C6 Ru1 C1 -131.3(4) . . . . ? C1 C6 Ru1 C5 131.3(4) . . . . ? C1 C6 Ru1 C4 103.0(3) . . . . ? C5 C6 Ru1 C4 -28.3(3) . . . . ? C1 C6 Ru1 P1 -45.1(4) . . . . ? C5 C6 Ru1 P1 -176.4(2) . . . . ? C1 C6 Ru1 Cl2 142.8(3) . . . . ? C5 C6 Ru1 Cl2 11.5(4) . . . . ? C1 C6 Ru1 Cl1 -129.0(3) . . . . ? C5 C6 Ru1 Cl1 99.6(2) . . . . ? C6 C1 Ru1 C2 -131.8(5) . . . . ? C6 C1 Ru1 C3 -102.6(4) . . . . ? C2 C1 Ru1 C3 29.2(3) . . . . ? C2 C1 Ru1 C6 131.8(5) . . . . ? C6 C1 Ru1 C5 -29.7(3) . . . . ? C2 C1 Ru1 C5 102.1(4) . . . . ? C6 C1 Ru1 C4 -64.9(3) . . . . ? C2 C1 Ru1 C4 66.8(4) . . . . ? C6 C1 Ru1 P1 144.7(3) . . . . ? C2 C1 Ru1 P1 -83.6(3) . . . . ? C6 C1 Ru1 Cl2 -116.9(4) . . . . ? C2 C1 Ru1 Cl2 14.9(6) . . . . ? C6 C1 Ru1 Cl1 55.5(3) . . . . ? C2 C1 Ru1 Cl1 -172.7(3) . . . . ? C4 C5 Ru1 C2 -64.4(3) . . . . ? C6 C5 Ru1 C2 67.3(3) . . . . ? C4 C5 Ru1 C3 -26.7(3) . . . . ? C6 C5 Ru1 C3 104.9(3) . . . . ? C4 C5 Ru1 C6 -131.7(4) . . . . ? C4 C5 Ru1 C1 -102.2(3) . . . . ? C6 C5 Ru1 C1 29.4(3) . . . . ? C6 C5 Ru1 C4 131.7(4) . . . . ? C4 C5 Ru1 P1 -121.7(4) . . . . ? C6 C5 Ru1 P1 9.9(6) . . . . ? C4 C5 Ru1 Cl2 54.9(3) . . . . ? C6 C5 Ru1 Cl2 -173.4(2) . . . . ? C4 C5 Ru1 Cl1 147.8(3) . . . . ? C6 C5 Ru1 Cl1 -80.6(3) . . . . ? O1 C4 Ru1 C2 -148.3(6) . . . . ? C5 C4 Ru1 C2 104.9(3) . . . . ? C3 C4 Ru1 C2 -32.0(3) . . . . ? O1 C4 Ru1 C3 -116.3(6) . . . . ? C5 C4 Ru1 C3 136.9(4) . . . . ? O1 C4 Ru1 C6 136.7(6) . . . . ? C5 C4 Ru1 C6 29.9(3) . . . . ? C3 C4 Ru1 C6 -107.0(3) . . . . ? O1 C4 Ru1 C1 173.5(5) . . . . ? C5 C4 Ru1 C1 66.6(3) . . . . ? C3 C4 Ru1 C1 -70.2(3) . . . . ? O1 C4 Ru1 C5 106.8(6) . . . . ? C3 C4 Ru1 C5 -136.9(4) . . . . ? O1 C4 Ru1 P1 -103.3(5) . . . . ? C5 C4 Ru1 P1 149.9(2) . . . . ? C3 C4 Ru1 P1 13.0(4) . . . . ? O1 C4 Ru1 Cl2 -23.2(5) . . . . ? C5 C4 Ru1 Cl2 -130.0(3) . . . . ? C3 C4 Ru1 Cl2 93.1(3) . . . . ? O1 C4 Ru1 Cl1 67.7(5) . . . . ? C5 C4 Ru1 Cl1 -39.1(3) . . . . ? C3 C4 Ru1 Cl1 -176.0(2) . . . . ? C21 P1 Ru1 C2 -45.2(3) . . . . ? C15 P1 Ru1 C2 -164.1(2) . . . . ? C9 P1 Ru1 C2 73.1(2) . . . . ? C21 P1 Ru1 C3 -77.0(2) . . . . ? C15 P1 Ru1 C3 164.0(2) . . . . ? C9 P1 Ru1 C3 41.3(2) . . . . ? C21 P1 Ru1 C6 18.0(3) . . . . ? C15 P1 Ru1 C6 -101.0(2) . . . . ? C9 P1 Ru1 C6 136.3(2) . . . . ? C21 P1 Ru1 C1 -7.4(2) . . . . ? C15 P1 Ru1 C1 -126.4(2) . . . . ? C9 P1 Ru1 C1 110.9(2) . . . . ? C21 P1 Ru1 C5 10.6(5) . . . . ? C15 P1 Ru1 C5 -108.4(4) . . . . ? C9 P1 Ru1 C5 128.9(4) . . . . ? C21 P1 Ru1 C4 -85.5(3) . . . . ? C15 P1 Ru1 C4 155.5(3) . . . . ? C9 P1 Ru1 C4 32.8(3) . . . . ? C21 P1 Ru1 Cl2 -166.3(2) . . . . ? C15 P1 Ru1 Cl2 74.75(18) . . . . ? C9 P1 Ru1 Cl2 -47.96(17) . . . . ? C21 P1 Ru1 Cl1 102.1(2) . . . . ? C15 P1 Ru1 Cl1 -16.92(18) . . . . ? C9 P1 Ru1 Cl1 -139.62(17) . . . . ? Ru1 Cl1 Ru1 C2 -111.6(3) 2_556 . . . ? Ru1 Cl1 Ru1 C3 -22.4(4) 2_556 . . . ? Ru1 Cl1 Ru1 C6 -73.59(14) 2_556 . . . ? Ru1 Cl1 Ru1 C1 -103.31(16) 2_556 . . . ? Ru1 Cl1 Ru1 C5 -36.85(13) 2_556 . . . ? Ru1 Cl1 Ru1 C4 -15.45(14) 2_556 . . . ? Ru1 Cl1 Ru1 P1 160.12(3) 2_556 . . . ? Ru1 Cl1 Ru1 Cl2 73.92(3) 2_556 . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 66.98 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.885 _refine_diff_density_min -2.202 _refine_diff_density_rms 0.114 data_5a _database_code_depnum_ccdc_archive 'CCDC 908515' #TrackingRef '2_3_5a.cif' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H27 Cl O4 P Ru, F6 Sb, C3 H6 O' _chemical_formula_sum 'C30 H33 Cl F6 O5 P Ru Sb' _chemical_formula_weight 876.80 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 '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' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 11.7393(1) _cell_length_b 19.5779(2) _cell_length_c 15.0206(1) _cell_angle_alpha 90.00 _cell_angle_beta 99.505(1) _cell_angle_gamma 90.00 _cell_volume 3404.80(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17555 _cell_measurement_theta_min 2.9749 _cell_measurement_theta_max 73.8714 _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1671 _exptl_crystal_size_mid 0.1267 _exptl_crystal_size_min 0.0871 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 11.671 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.73079 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur Nova ; _diffrn_measurement_device ; 165 mm Onyx CCD detector in \k-geometry diffractometer ; _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.2640 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23902 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 73.98 _reflns_number_total 6878 _reflns_number_gt 6432 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1015P)^2^+7.6131P] 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 6878 _refine_ls_number_parameters 392 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1700 _refine_ls_wR_factor_gt 0.1672 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.149 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1727(8) 0.0099(5) 0.2594(7) 0.090(3) Uani 1 1 d . . . H1 H 0.2494 -0.0015 0.2588 0.107 Uiso 1 1 calc R . . C2 C 0.1116(7) -0.0237(4) 0.3156(6) 0.081(2) Uani 1 1 d . . . H2 H 0.1468 -0.0574 0.3543 0.097 Uiso 1 1 calc R . . C3 C -0.0100(7) -0.0061(3) 0.3145(6) 0.075(2) Uani 1 1 d . . . H3 H -0.0524 -0.0293 0.3521 0.090 Uiso 1 1 calc R . . C4 C -0.0602(7) 0.0426(4) 0.2604(5) 0.0728(19) Uani 1 1 d . . . C5 C 0.0028(9) 0.0778(5) 0.2021(5) 0.083(2) Uani 1 1 d . . . H5 H -0.0329 0.1115 0.1636 0.100 Uiso 1 1 calc R . . C6 C 0.1200(9) 0.0616(5) 0.2024(5) 0.084(3) Uani 1 1 d . . . H6 H 0.1622 0.0852 0.1651 0.101 Uiso 1 1 calc R . . C7 C -0.1824(7) 0.0644(5) 0.2641(6) 0.0848(10) Uani 1 1 d . . . H7A H -0.2304 0.0239 0.2589 0.102 Uiso 1 1 calc R . . H7B H -0.2088 0.0926 0.2116 0.102 Uiso 1 1 calc R . . C8 C -0.2034(7) 0.1035(5) 0.3470(6) 0.0848(10) Uani 1 1 d . . . H8A H -0.2817 0.1212 0.3361 0.102 Uiso 1 1 calc R . . H8B H -0.1974 0.0720 0.3974 0.102 Uiso 1 1 calc R . . C9 C -0.1239(6) 0.1603(5) 0.3724(5) 0.0848(10) Uani 1 1 d D . . H9A H -0.1297 0.1897 0.3199 0.102 Uiso 1 1 calc R . . H9B H -0.1548 0.1860 0.4182 0.102 Uiso 1 1 calc R . . C10 C 0.1391(5) 0.2519(3) 0.2008(3) 0.0456(11) Uani 1 1 d . . . C11 C 0.1570(6) 0.2672(4) 0.1157(4) 0.0601(15) Uani 1 1 d . . . H11 H 0.2254 0.2554 0.0961 0.072 Uiso 1 1 calc R . . C12 C 0.0688(8) 0.3014(4) 0.0588(4) 0.075(2) Uani 1 1 d . . . H12 H 0.0788 0.3126 0.0004 0.090 Uiso 1 1 calc R . . C13 C -0.0311(7) 0.3185(4) 0.0876(4) 0.0695(19) Uani 1 1 d . . . H13 H -0.0892 0.3408 0.0487 0.083 Uiso 1 1 calc R . . C14 C -0.0464(6) 0.3032(4) 0.1733(5) 0.0667(17) Uani 1 1 d . . . H14 H -0.1151 0.3150 0.1925 0.080 Uiso 1 1 calc R . . C15 C 0.0401(5) 0.2700(3) 0.2326(4) 0.0562(13) Uani 1 1 d . . . H15 H 0.0310 0.2604 0.2916 0.067 Uiso 1 1 calc R . . C16 C 0.4151(5) 0.1039(3) 0.3271(4) 0.0485(11) Uani 1 1 d . . . C17 C 0.4225(6) 0.1050(4) 0.2362(4) 0.0575(14) Uani 1 1 d . . . H17 H 0.3925 0.1414 0.2000 0.069 Uiso 1 1 calc R . . C18 C 0.4757(6) 0.0504(4) 0.2001(5) 0.0687(17) Uani 1 1 d . . . H18 H 0.4796 0.0496 0.1388 0.082 Uiso 1 1 calc R . . C19 C 0.5226(8) -0.0023(4) 0.2548(6) 0.083(2) Uani 1 1 d . . . H19 H 0.5577 -0.0389 0.2306 0.099 Uiso 1 1 calc R . . C20 C 0.5172(10) -0.0007(5) 0.3430(6) 0.094(3) Uani 1 1 d . . . H20 H 0.5509 -0.0360 0.3796 0.113 Uiso 1 1 calc R . . C21 C 0.4630(8) 0.0521(4) 0.3817(5) 0.074(2) Uani 1 1 d . . . H21 H 0.4595 0.0521 0.4431 0.089 Uiso 1 1 calc R . . C22 C 0.2530(5) 0.2963(3) 0.4312(4) 0.0494(12) Uani 1 1 d . . . C23 C 0.3666(6) 0.3131(3) 0.4322(5) 0.0603(14) Uani 1 1 d . . . H23 H 0.4198 0.2799 0.4224 0.072 Uiso 1 1 calc R . . C24 C 0.4012(9) 0.3802(4) 0.4479(6) 0.078(2) Uani 1 1 d . . . H24 H 0.4776 0.3923 0.4472 0.094 Uiso 1 1 calc R . . C25 C 0.3237(9) 0.4288(4) 0.4645(6) 0.084(2) Uani 1 1 d . . . H25 H 0.3471 0.4739 0.4756 0.101 Uiso 1 1 calc R . . C26 C 0.2085(10) 0.4099(4) 0.4646(7) 0.093(3) Uani 1 1 d . . . H26 H 0.1555 0.4427 0.4762 0.112 Uiso 1 1 calc R . . C27 C 0.1732(7) 0.3441(4) 0.4478(6) 0.075(2) Uani 1 1 d . . . H27 H 0.0966 0.3319 0.4476 0.090 Uiso 1 1 calc R . . C28 C 0.0503(8) 0.2106(4) 0.6563(5) 0.150(7) Uani 1 1 d D . . C29 C -0.0214(6) 0.1660(3) 0.5839(3) 0.0662(17) Uani 1 1 d D . . H29A H 0.0120 0.1672 0.5297 0.099 Uiso 1 1 calc R . . H29B H -0.0991 0.1831 0.5714 0.099 Uiso 1 1 calc R . . H29C H -0.0222 0.1198 0.6052 0.099 Uiso 1 1 calc R . . C30 C -0.0196(8) 0.1969(5) 0.7296(6) 0.087(2) Uani 1 1 d . . . H30A H 0.0130 0.2215 0.7831 0.130 Uiso 1 1 calc R . . H30B H -0.0188 0.1489 0.7425 0.130 Uiso 1 1 calc R . . H30C H -0.0977 0.2117 0.7101 0.130 Uiso 1 1 calc R . . Cl1 Cl 0.19376(16) 0.06628(9) 0.49181(10) 0.0671(4) Uani 1 1 d . . . F1 F 0.3094(8) 0.5798(4) 0.6452(7) 0.183(5) Uani 1 1 d . . . F2 F 0.2827(7) 0.6017(4) 0.4707(5) 0.131(3) Uani 1 1 d . . . F3 F 0.1099(6) 0.5576(3) 0.5477(5) 0.116(2) Uani 1 1 d . . . F4 F 0.1152(6) 0.6839(4) 0.4783(5) 0.126(2) Uani 1 1 d . . . F5 F 0.1344(9) 0.6642(5) 0.6517(6) 0.167(4) Uani 1 1 d . . . F6 F 0.3152(5) 0.7045(3) 0.5854(4) 0.0943(15) Uani 1 1 d . . . O1 O -0.0095(5) 0.1519(3) 0.4035(4) 0.0848(10) Uani 1 1 d D . . O2 O 0.2139(4) 0.22803(19) 0.4209(3) 0.0499(8) Uani 1 1 d . . . O3 O 0.2325(3) 0.2191(2) 0.2556(3) 0.0512(9) Uani 1 1 d . . . O4 O 0.3618(3) 0.1582(2) 0.3668(2) 0.0480(8) Uani 1 1 d . . . O5 O 0.1369(16) 0.2340(11) 0.6358(11) 0.254(9) Uani 1 1 d . . . P1 P 0.22783(12) 0.17499(6) 0.34427(8) 0.0420(3) Uani 1 1 d . . . Ru1 Ru 0.09982(4) 0.08592(2) 0.34080(3) 0.04765(16) Uani 1 1 d D . . Sb1 Sb 0.21325(4) 0.63117(2) 0.56599(3) 0.05988(17) Uani 1 1 d . . . H1O H -0.0258(9) 0.0944(7) 0.4329(9) 0.38(16) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.085(5) 0.082(5) 0.108(7) -0.055(5) 0.038(5) -0.018(4) C2 0.103(6) 0.049(4) 0.090(5) -0.021(4) 0.013(5) 0.001(4) C3 0.088(5) 0.058(4) 0.082(5) -0.021(4) 0.024(4) -0.027(4) C4 0.078(4) 0.074(4) 0.063(4) -0.029(4) 0.001(3) -0.014(4) C5 0.111(7) 0.088(5) 0.043(3) -0.016(3) -0.009(4) -0.022(5) C6 0.114(7) 0.095(6) 0.050(4) -0.034(4) 0.033(4) -0.038(5) C7 0.0704(19) 0.095(3) 0.089(2) -0.031(2) 0.0102(17) 0.0000(19) C8 0.0704(19) 0.095(3) 0.089(2) -0.031(2) 0.0102(17) 0.0000(19) C9 0.0704(19) 0.095(3) 0.089(2) -0.031(2) 0.0102(17) 0.0000(19) C10 0.056(3) 0.041(2) 0.039(2) 0.004(2) 0.006(2) 0.007(2) C11 0.071(4) 0.069(4) 0.041(3) 0.002(3) 0.013(3) 0.014(3) C12 0.101(5) 0.087(5) 0.035(3) 0.011(3) 0.010(3) 0.022(4) C13 0.088(5) 0.067(4) 0.047(3) 0.001(3) -0.010(3) 0.023(4) C14 0.065(4) 0.076(4) 0.057(3) -0.002(3) 0.006(3) 0.019(3) C15 0.059(3) 0.066(4) 0.044(3) 0.006(2) 0.011(2) 0.010(3) C16 0.054(3) 0.048(3) 0.042(3) -0.005(2) 0.003(2) 0.009(2) C17 0.063(3) 0.061(3) 0.049(3) 0.001(3) 0.012(3) 0.011(3) C18 0.069(4) 0.080(5) 0.060(4) -0.012(3) 0.018(3) 0.009(3) C19 0.092(5) 0.073(5) 0.083(5) -0.018(4) 0.018(4) 0.028(4) C20 0.135(8) 0.070(5) 0.078(5) 0.007(4) 0.021(5) 0.048(5) C21 0.103(6) 0.062(4) 0.057(4) 0.007(3) 0.013(4) 0.032(4) C22 0.062(3) 0.043(3) 0.044(3) -0.005(2) 0.009(2) 0.003(2) C23 0.068(4) 0.053(3) 0.062(4) -0.007(3) 0.019(3) 0.002(3) C24 0.101(6) 0.063(4) 0.073(5) -0.009(3) 0.021(4) -0.020(4) C25 0.122(7) 0.046(4) 0.086(5) -0.005(3) 0.019(5) -0.007(4) C26 0.116(7) 0.057(4) 0.103(7) -0.021(4) 0.003(5) 0.029(5) C27 0.070(4) 0.060(4) 0.095(5) -0.017(4) 0.013(4) 0.014(3) C28 0.186(13) 0.189(13) 0.095(7) 0.081(9) 0.080(8) 0.141(12) C29 0.092(5) 0.073(4) 0.038(3) -0.001(3) 0.024(3) 0.004(4) C30 0.104(6) 0.089(6) 0.069(5) -0.012(4) 0.023(4) 0.019(5) Cl1 0.0854(10) 0.0672(9) 0.0466(7) 0.0125(6) 0.0046(7) -0.0007(8) F1 0.161(7) 0.141(6) 0.210(9) 0.116(7) -0.076(6) -0.021(5) F2 0.168(7) 0.123(5) 0.123(5) -0.029(4) 0.089(5) 0.000(5) F3 0.119(4) 0.091(4) 0.144(5) -0.024(4) 0.042(4) -0.043(3) F4 0.114(5) 0.113(5) 0.141(6) 0.032(4) -0.012(4) 0.014(4) F5 0.211(9) 0.167(7) 0.159(7) -0.069(6) 0.134(7) -0.043(7) F6 0.107(4) 0.082(3) 0.092(3) 0.003(3) 0.010(3) -0.031(3) O1 0.0704(19) 0.095(3) 0.089(2) -0.031(2) 0.0102(17) 0.0000(19) O2 0.062(2) 0.0413(18) 0.049(2) -0.0060(15) 0.0165(17) -0.0007(16) O3 0.054(2) 0.055(2) 0.0453(19) 0.0126(16) 0.0108(16) 0.0075(17) O4 0.054(2) 0.0458(19) 0.0426(18) -0.0055(15) 0.0027(15) 0.0069(16) O5 0.257(16) 0.33(2) 0.210(15) -0.003(15) 0.138(14) -0.018(17) P1 0.0524(7) 0.0388(6) 0.0347(6) -0.0004(5) 0.0069(5) 0.0025(5) Ru1 0.0609(3) 0.0448(2) 0.0380(2) -0.00476(15) 0.01005(18) -0.00569(16) Sb1 0.0685(3) 0.0577(3) 0.0593(3) -0.00526(16) 0.0279(2) -0.00241(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.364(12) . ? C1 C6 1.401(15) . ? C1 Ru1 2.188(7) . ? C1 H1 0.9300 . ? C2 C3 1.466(11) . ? C2 Ru1 2.187(7) . ? C2 H2 0.9300 . ? C3 C4 1.325(11) . ? C3 Ru1 2.213(7) . ? C3 H3 0.9300 . ? C4 C5 1.416(12) . ? C4 C7 1.507(12) . ? C4 Ru1 2.227(7) . ? C5 C6 1.410(14) . ? C5 Ru1 2.209(7) . ? C5 H5 0.9300 . ? C6 Ru1 2.182(7) . ? C6 H6 0.9300 . ? C7 C8 1.515(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.460(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O1 1.357(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.363(8) . ? C10 C15 1.373(8) . ? C10 O3 1.411(6) . ? C11 C12 1.400(9) . ? C11 H11 0.9300 . ? C12 C13 1.357(11) . ? C12 H12 0.9300 . ? C13 C14 1.362(10) . ? C13 H13 0.9300 . ? C14 C15 1.396(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.366(9) . ? C16 C17 1.382(8) . ? C16 O4 1.414(7) . ? C17 C18 1.393(9) . ? C17 H17 0.9300 . ? C18 C19 1.376(12) . ? C18 H18 0.9300 . ? C19 C20 1.336(13) . ? C19 H19 0.9300 . ? C20 C21 1.390(11) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.373(9) . ? C22 C27 1.376(9) . ? C22 O2 1.413(7) . ? C23 C24 1.382(10) . ? C23 H23 0.9300 . ? C24 C25 1.368(13) . ? C24 H24 0.9300 . ? C25 C26 1.402(15) . ? C25 H25 0.9300 . ? C26 C27 1.363(12) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 O5 1.200(18) . ? C28 C30 1.502(13) . ? C28 C29 1.534(2) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? Cl1 Ru1 2.3840(15) . ? F1 Sb1 1.805(6) . ? F2 Sb1 1.852(5) . ? F3 Sb1 1.874(5) . ? F4 Sb1 1.904(6) . ? F5 Sb1 1.824(6) . ? F6 Sb1 1.861(5) . ? O1 Ru1 2.145(5) . ? O1 H1O 1.236(15) . ? O2 P1 1.579(4) . ? O3 P1 1.595(4) . ? O4 P1 1.588(4) . ? P1 Ru1 2.2970(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.2(9) . . ? C2 C1 Ru1 71.8(4) . . ? C6 C1 Ru1 71.1(4) . . ? C2 C1 H1 119.9 . . ? C6 C1 H1 119.9 . . ? Ru1 C1 H1 129.6 . . ? C1 C2 C3 119.3(9) . . ? C1 C2 Ru1 71.9(4) . . ? C3 C2 Ru1 71.5(4) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? Ru1 C2 H2 128.5 . . ? C4 C3 C2 120.6(8) . . ? C4 C3 Ru1 73.2(4) . . ? C2 C3 Ru1 69.6(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? Ru1 C3 H3 130.1 . . ? C3 C4 C5 120.3(8) . . ? C3 C4 C7 120.7(9) . . ? C5 C4 C7 118.9(9) . . ? C3 C4 Ru1 72.0(4) . . ? C5 C4 Ru1 70.7(4) . . ? C7 C4 Ru1 126.5(5) . . ? C6 C5 C4 119.8(9) . . ? C6 C5 Ru1 70.2(4) . . ? C4 C5 Ru1 72.1(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? Ru1 C5 H5 130.1 . . ? C1 C6 C5 119.7(8) . . ? C1 C6 Ru1 71.5(4) . . ? C5 C6 Ru1 72.3(4) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? Ru1 C6 H6 128.2 . . ? C4 C7 C8 117.3(7) . . ? C4 C7 H7A 108.0 . . ? C8 C7 H7A 108.0 . . ? C4 C7 H7B 108.0 . . ? C8 C7 H7B 108.0 . . ? H7A C7 H7B 107.2 . . ? C9 C8 C7 114.6(8) . . ? C9 C8 H8A 108.6 . . ? C7 C8 H8A 108.6 . . ? C9 C8 H8B 108.6 . . ? C7 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? O1 C9 C8 123.4(8) . . ? O1 C9 H9A 106.5 . . ? C8 C9 H9A 106.5 . . ? O1 C9 H9B 106.5 . . ? C8 C9 H9B 106.5 . . ? H9A C9 H9B 106.5 . . ? C11 C10 C15 122.6(5) . . ? C11 C10 O3 115.0(5) . . ? C15 C10 O3 122.4(5) . . ? C10 C11 C12 117.8(6) . . ? C10 C11 H11 121.1 . . ? C12 C11 H11 121.1 . . ? C13 C12 C11 120.9(6) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 120.2(6) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 120.6(7) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C10 C15 C14 117.9(6) . . ? C10 C15 H15 121.1 . . ? C14 C15 H15 121.1 . . ? C21 C16 C17 121.2(6) . . ? C21 C16 O4 118.2(5) . . ? C17 C16 O4 120.6(5) . . ? C16 C17 C18 118.6(6) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? C19 C18 C17 120.3(7) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 119.6(7) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 122.2(8) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C16 C21 C20 118.1(7) . . ? C16 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? C23 C22 C27 121.6(6) . . ? C23 C22 O2 121.8(5) . . ? C27 C22 O2 116.4(6) . . ? C22 C23 C24 119.2(7) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 120.5(8) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.1(7) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C27 C26 C25 120.9(8) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C22 118.8(8) . . ? C26 C27 H27 120.6 . . ? C22 C27 H27 120.6 . . ? O5 C28 C30 147.6(11) . . ? O5 C28 C29 115.1(11) . . ? C30 C28 C29 96.7(7) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C9 O1 Ru1 123.5(4) . . ? C9 O1 H1O 91.8(7) . . ? Ru1 O1 H1O 75.4(5) . . ? C22 O2 P1 129.1(4) . . ? C10 O3 P1 127.1(4) . . ? C16 O4 P1 123.9(3) . . ? O2 P1 O4 101.5(2) . . ? O2 P1 O3 105.9(2) . . ? O4 P1 O3 97.0(2) . . ? O2 P1 Ru1 111.69(16) . . ? O4 P1 Ru1 117.95(16) . . ? O3 P1 Ru1 120.27(17) . . ? O1 Ru1 C6 135.7(4) . . ? O1 Ru1 C2 136.6(3) . . ? C6 Ru1 C2 66.5(4) . . ? O1 Ru1 C1 166.5(3) . . ? C6 Ru1 C1 37.4(4) . . ? C2 Ru1 C1 36.3(3) . . ? O1 Ru1 C5 101.8(3) . . ? C6 Ru1 C5 37.5(4) . . ? C2 Ru1 C5 78.7(3) . . ? C1 Ru1 C5 67.2(4) . . ? O1 Ru1 C3 101.3(3) . . ? C6 Ru1 C3 78.7(3) . . ? C2 Ru1 C3 38.9(3) . . ? C1 Ru1 C3 67.5(3) . . ? C5 Ru1 C3 65.1(3) . . ? O1 Ru1 C4 87.4(2) . . ? C6 Ru1 C4 67.4(3) . . ? C2 Ru1 C4 66.7(3) . . ? C1 Ru1 C4 79.1(3) . . ? C5 Ru1 C4 37.2(3) . . ? C3 Ru1 C4 34.7(3) . . ? O1 Ru1 P1 88.25(17) . . ? C6 Ru1 P1 90.8(2) . . ? C2 Ru1 P1 133.5(2) . . ? C1 Ru1 P1 102.4(2) . . ? C5 Ru1 P1 108.0(2) . . ? C3 Ru1 P1 169.1(2) . . ? C4 Ru1 P1 142.4(2) . . ? O1 Ru1 Cl1 84.02(16) . . ? C6 Ru1 Cl1 139.9(3) . . ? C2 Ru1 Cl1 88.5(3) . . ? C1 Ru1 Cl1 105.1(3) . . ? C5 Ru1 Cl1 166.2(2) . . ? C3 Ru1 Cl1 101.7(2) . . ? C4 Ru1 Cl1 132.1(2) . . ? P1 Ru1 Cl1 84.41(5) . . ? F1 Sb1 F5 93.8(6) . . ? F1 Sb1 F2 91.6(5) . . ? F5 Sb1 F2 174.5(5) . . ? F1 Sb1 F6 90.6(3) . . ? F5 Sb1 F6 90.3(3) . . ? F2 Sb1 F6 90.4(3) . . ? F1 Sb1 F3 89.3(4) . . ? F5 Sb1 F3 89.1(3) . . ? F2 Sb1 F3 90.3(3) . . ? F6 Sb1 F3 179.3(3) . . ? F1 Sb1 F4 177.5(5) . . ? F5 Sb1 F4 88.7(5) . . ? F2 Sb1 F4 85.8(4) . . ? F6 Sb1 F4 89.4(3) . . ? F3 Sb1 F4 90.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.3(11) . . . . ? Ru1 C1 C2 C3 55.4(6) . . . . ? C6 C1 C2 Ru1 -54.2(6) . . . . ? C1 C2 C3 C4 -0.9(11) . . . . ? Ru1 C2 C3 C4 54.7(6) . . . . ? C1 C2 C3 Ru1 -55.6(6) . . . . ? C2 C3 C4 C5 0.7(10) . . . . ? Ru1 C3 C4 C5 53.7(6) . . . . ? C2 C3 C4 C7 -175.3(6) . . . . ? Ru1 C3 C4 C7 -122.3(6) . . . . ? C2 C3 C4 Ru1 -53.0(6) . . . . ? C3 C4 C5 C6 -0.9(10) . . . . ? C7 C4 C5 C6 175.2(6) . . . . ? Ru1 C4 C5 C6 53.5(6) . . . . ? C3 C4 C5 Ru1 -54.3(6) . . . . ? C7 C4 C5 Ru1 121.8(6) . . . . ? C2 C1 C6 C5 -1.4(11) . . . . ? Ru1 C1 C6 C5 -55.9(6) . . . . ? C2 C1 C6 Ru1 54.5(7) . . . . ? C4 C5 C6 C1 1.2(10) . . . . ? Ru1 C5 C6 C1 55.5(6) . . . . ? C4 C5 C6 Ru1 -54.3(6) . . . . ? C3 C4 C7 C8 70.2(11) . . . . ? C5 C4 C7 C8 -105.9(10) . . . . ? Ru1 C4 C7 C8 -19.4(14) . . . . ? C4 C7 C8 C9 48.5(13) . . . . ? C7 C8 C9 O1 -67.2(11) . . . . ? C15 C10 C11 C12 -1.5(10) . . . . ? O3 C10 C11 C12 -178.3(6) . . . . ? C10 C11 C12 C13 -0.2(12) . . . . ? C11 C12 C13 C14 0.8(13) . . . . ? C12 C13 C14 C15 0.1(12) . . . . ? C11 C10 C15 C14 2.4(10) . . . . ? O3 C10 C15 C14 179.0(6) . . . . ? C13 C14 C15 C10 -1.7(11) . . . . ? C21 C16 C17 C18 2.7(11) . . . . ? O4 C16 C17 C18 -180.0(6) . . . . ? C16 C17 C18 C19 -1.8(12) . . . . ? C17 C18 C19 C20 -0.4(14) . . . . ? C18 C19 C20 C21 1.7(17) . . . . ? C17 C16 C21 C20 -1.5(13) . . . . ? O4 C16 C21 C20 -178.9(8) . . . . ? C19 C20 C21 C16 -0.7(17) . . . . ? C27 C22 C23 C24 -1.7(11) . . . . ? O2 C22 C23 C24 -176.1(6) . . . . ? C22 C23 C24 C25 1.6(12) . . . . ? C23 C24 C25 C26 -0.5(14) . . . . ? C24 C25 C26 C27 -0.5(15) . . . . ? C25 C26 C27 C22 0.4(15) . . . . ? C23 C22 C27 C26 0.7(12) . . . . ? O2 C22 C27 C26 175.4(8) . . . . ? C8 C9 O1 Ru1 47.0(11) . . . . ? C23 C22 O2 P1 -54.4(8) . . . . ? C27 C22 O2 P1 130.9(6) . . . . ? C11 C10 O3 P1 -159.9(5) . . . . ? C15 C10 O3 P1 23.2(8) . . . . ? C21 C16 O4 P1 -115.4(6) . . . . ? C17 C16 O4 P1 67.2(7) . . . . ? C22 O2 P1 O4 71.2(5) . . . . ? C22 O2 P1 O3 -29.6(5) . . . . ? C22 O2 P1 Ru1 -162.3(4) . . . . ? C16 O4 P1 O2 168.5(4) . . . . ? C16 O4 P1 O3 -83.7(5) . . . . ? C16 O4 P1 Ru1 46.1(5) . . . . ? C10 O3 P1 O2 -74.6(5) . . . . ? C10 O3 P1 O4 -178.7(4) . . . . ? C10 O3 P1 Ru1 53.1(5) . . . . ? C9 O1 Ru1 C6 41.0(8) . . . . ? C9 O1 Ru1 C2 -63.7(8) . . . . ? C9 O1 Ru1 C1 -11.9(19) . . . . ? C9 O1 Ru1 C5 22.3(7) . . . . ? C9 O1 Ru1 C3 -44.3(7) . . . . ? C9 O1 Ru1 C4 -12.2(7) . . . . ? C9 O1 Ru1 P1 130.4(7) . . . . ? C9 O1 Ru1 Cl1 -145.1(7) . . . . ? C1 C6 Ru1 O1 -162.1(5) . . . . ? C5 C6 Ru1 O1 -31.1(7) . . . . ? C1 C6 Ru1 C2 -28.6(5) . . . . ? C5 C6 Ru1 C2 102.4(6) . . . . ? C5 C6 Ru1 C1 131.0(8) . . . . ? C1 C6 Ru1 C5 -131.0(8) . . . . ? C1 C6 Ru1 C3 -67.5(5) . . . . ? C5 C6 Ru1 C3 63.5(5) . . . . ? C1 C6 Ru1 C4 -101.9(6) . . . . ? C5 C6 Ru1 C4 29.1(5) . . . . ? C1 C6 Ru1 P1 109.6(5) . . . . ? C5 C6 Ru1 P1 -119.4(5) . . . . ? C1 C6 Ru1 Cl1 27.4(7) . . . . ? C5 C6 Ru1 Cl1 158.3(4) . . . . ? C1 C2 Ru1 O1 162.0(5) . . . . ? C3 C2 Ru1 O1 31.2(7) . . . . ? C1 C2 Ru1 C6 29.4(6) . . . . ? C3 C2 Ru1 C6 -101.4(6) . . . . ? C3 C2 Ru1 C1 -130.8(8) . . . . ? C1 C2 Ru1 C5 66.7(6) . . . . ? C3 C2 Ru1 C5 -64.1(5) . . . . ? C1 C2 Ru1 C3 130.8(8) . . . . ? C1 C2 Ru1 C4 103.7(7) . . . . ? C3 C2 Ru1 C4 -27.1(5) . . . . ? C1 C2 Ru1 P1 -37.5(7) . . . . ? C3 C2 Ru1 P1 -168.3(4) . . . . ? C1 C2 Ru1 Cl1 -118.4(6) . . . . ? C3 C2 Ru1 Cl1 110.8(5) . . . . ? C2 C1 Ru1 O1 -65.6(18) . . . . ? C6 C1 Ru1 O1 66.6(17) . . . . ? C2 C1 Ru1 C6 -132.2(8) . . . . ? C6 C1 Ru1 C2 132.2(8) . . . . ? C2 C1 Ru1 C5 -102.3(6) . . . . ? C6 C1 Ru1 C5 29.9(5) . . . . ? C2 C1 Ru1 C3 -31.0(5) . . . . ? C6 C1 Ru1 C3 101.2(6) . . . . ? C2 C1 Ru1 C4 -65.3(6) . . . . ? C6 C1 Ru1 C4 66.9(5) . . . . ? C2 C1 Ru1 P1 153.1(5) . . . . ? C6 C1 Ru1 P1 -74.7(5) . . . . ? C2 C1 Ru1 Cl1 65.6(6) . . . . ? C6 C1 Ru1 Cl1 -162.2(5) . . . . ? C6 C5 Ru1 O1 158.4(5) . . . . ? C4 C5 Ru1 O1 -69.4(5) . . . . ? C4 C5 Ru1 C6 132.2(8) . . . . ? C6 C5 Ru1 C2 -66.0(6) . . . . ? C4 C5 Ru1 C2 66.2(5) . . . . ? C6 C5 Ru1 C1 -29.8(5) . . . . ? C4 C5 Ru1 C1 102.4(6) . . . . ? C6 C5 Ru1 C3 -104.6(6) . . . . ? C4 C5 Ru1 C3 27.6(5) . . . . ? C6 C5 Ru1 C4 -132.2(8) . . . . ? C6 C5 Ru1 P1 66.3(6) . . . . ? C4 C5 Ru1 P1 -161.5(4) . . . . ? C6 C5 Ru1 Cl1 -87.6(13) . . . . ? C4 C5 Ru1 Cl1 44.6(15) . . . . ? C4 C3 Ru1 O1 68.5(5) . . . . ? C2 C3 Ru1 O1 -158.7(5) . . . . ? C4 C3 Ru1 C6 -66.4(6) . . . . ? C2 C3 Ru1 C6 66.5(6) . . . . ? C4 C3 Ru1 C2 -132.8(8) . . . . ? C4 C3 Ru1 C1 -103.8(6) . . . . ? C2 C3 Ru1 C1 29.1(5) . . . . ? C4 C3 Ru1 C5 -29.5(5) . . . . ? C2 C3 Ru1 C5 103.4(6) . . . . ? C2 C3 Ru1 C4 132.8(8) . . . . ? C4 C3 Ru1 P1 -81.9(12) . . . . ? C2 C3 Ru1 P1 50.9(13) . . . . ? C4 C3 Ru1 Cl1 154.6(5) . . . . ? C2 C3 Ru1 Cl1 -72.6(5) . . . . ? C3 C4 Ru1 O1 -114.1(5) . . . . ? C5 C4 Ru1 O1 113.5(6) . . . . ? C7 C4 Ru1 O1 1.3(8) . . . . ? C3 C4 Ru1 C6 103.3(6) . . . . ? C5 C4 Ru1 C6 -29.2(6) . . . . ? C7 C4 Ru1 C6 -141.4(9) . . . . ? C3 C4 Ru1 C2 30.1(5) . . . . ? C5 C4 Ru1 C2 -102.4(6) . . . . ? C7 C4 Ru1 C2 145.5(9) . . . . ? C3 C4 Ru1 C1 66.0(6) . . . . ? C5 C4 Ru1 C1 -66.5(6) . . . . ? C7 C4 Ru1 C1 -178.6(9) . . . . ? C3 C4 Ru1 C5 132.5(8) . . . . ? C7 C4 Ru1 C5 -112.2(11) . . . . ? C5 C4 Ru1 C3 -132.5(8) . . . . ? C7 C4 Ru1 C3 115.4(10) . . . . ? C3 C4 Ru1 P1 162.2(4) . . . . ? C5 C4 Ru1 P1 29.7(7) . . . . ? C7 C4 Ru1 P1 -82.5(9) . . . . ? C3 C4 Ru1 Cl1 -34.5(6) . . . . ? C5 C4 Ru1 Cl1 -167.0(5) . . . . ? C7 C4 Ru1 Cl1 80.9(9) . . . . ? O2 P1 Ru1 O1 24.3(2) . . . . ? O4 P1 Ru1 O1 141.3(2) . . . . ? O3 P1 Ru1 O1 -100.8(2) . . . . ? O2 P1 Ru1 C6 160.0(4) . . . . ? O4 P1 Ru1 C6 -83.0(4) . . . . ? O3 P1 Ru1 C6 35.0(4) . . . . ? O2 P1 Ru1 C2 -142.4(4) . . . . ? O4 P1 Ru1 C2 -25.4(4) . . . . ? O3 P1 Ru1 C2 92.5(4) . . . . ? O2 P1 Ru1 C1 -164.1(4) . . . . ? O4 P1 Ru1 C1 -47.1(4) . . . . ? O3 P1 Ru1 C1 70.8(4) . . . . ? O2 P1 Ru1 C5 126.2(3) . . . . ? O4 P1 Ru1 C5 -116.8(3) . . . . ? O3 P1 Ru1 C5 1.1(3) . . . . ? O2 P1 Ru1 C3 175.3(11) . . . . ? O4 P1 Ru1 C3 -67.7(11) . . . . ? O3 P1 Ru1 C3 50.2(11) . . . . ? O2 P1 Ru1 C4 107.8(4) . . . . ? O4 P1 Ru1 C4 -135.2(4) . . . . ? O3 P1 Ru1 C4 -17.2(4) . . . . ? O2 P1 Ru1 Cl1 -59.87(18) . . . . ? O4 P1 Ru1 Cl1 57.15(17) . . . . ? O3 P1 Ru1 Cl1 175.08(19) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 73.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.422 _refine_diff_density_min -1.823 _refine_diff_density_rms 0.128 #===END