# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Roddick, Dean' _publ_contact_author_email dmr@uwyo.edu loop_ _publ_author_name 'Adams, Jeramie' 'Donohoue, Rose' 'Gruver, Brian' 'Parson, Thomas' 'Arulsamy, Navamoney' 'Dean Roddick' data_jja13n _database_code_depnum_ccdc_archive 'CCDC 886418' #TrackingRef '- Combined.cif' #Compound 1: (CF3PCP)Ru(CO)Cl2-Et3NH+ #----------------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H7 Cl2 F12 O P2 Ru, C6 H16 N' _chemical_formula_sum 'C19 H23 Cl2 F12 N O P2 Ru' _chemical_formula_weight 743.29 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5313(9) _cell_length_b 10.8851(10) _cell_length_c 13.0549(11) _cell_angle_alpha 87.389(5) _cell_angle_beta 85.182(4) _cell_angle_gamma 67.290(4) _cell_volume 1375.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9873 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description rectangular_prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7743 _exptl_absorpt_correction_T_max 0.8851 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28588 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 31.50 _reflns_number_total 9091 _reflns_number_gt 8222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2004)' _computing_cell_refinement 'Bruker SMART (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V. 6.14 (Bruker, 2004)' _computing_publication_material 'Bruker SHELXTL V. 6.14 (Bruker, 2004)' _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^)+(0.0256P)^2^+0.4333P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9091 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Ru1 Ru 0.803747(10) 0.184242(9) 0.219864(7) 0.01613(3) Uani 1 1 d . . . Cl1 Cl 0.91412(4) 0.10000(3) 0.38485(2) 0.03043(8) Uani 1 1 d . . . Cl2 Cl 0.62638(3) 0.37032(3) 0.31141(2) 0.02451(6) Uani 1 1 d . . . P1 P 0.63982(4) 0.09492(3) 0.22678(3) 0.02195(7) Uani 1 1 d . . . P2 P 0.92472(3) 0.30912(3) 0.16236(2) 0.01914(6) Uani 1 1 d . . . C1 C 0.70693(13) 0.26457(12) 0.08467(9) 0.0186(2) Uani 1 1 d . . . C13 C 0.93752(15) 0.03577(15) 0.15228(11) 0.0256(3) Uani 1 1 d . . . O1 O 1.01645(14) -0.05359(13) 0.11546(10) 0.0416(3) Uani 1 1 d . . . C2 C 0.76643(14) 0.32710(13) 0.00936(9) 0.0215(2) Uani 1 1 d . . . C3 C 0.69897(17) 0.38468(15) -0.07862(10) 0.0271(3) Uani 1 1 d . . . H3 H 0.742(2) 0.4271(19) -0.1277(16) 0.037(5) Uiso 1 1 d . . . C4 C 0.57312(17) 0.37874(16) -0.09592(11) 0.0303(3) Uani 1 1 d . . . H4 H 0.531(2) 0.4167(19) -0.1532(15) 0.034(5) Uiso 1 1 d . . . C5 C 0.51372(16) 0.31656(15) -0.02383(11) 0.0280(3) Uani 1 1 d . . . H5 H 0.428(2) 0.3168(19) -0.0316(15) 0.037(5) Uiso 1 1 d . . . C6 C 0.57762(14) 0.26235(13) 0.06638(10) 0.0223(2) Uani 1 1 d . . . C7 C 0.50562(15) 0.20388(16) 0.14748(11) 0.0265(3) Uani 1 1 d . . . H7A H 0.459(2) 0.153(2) 0.1206(16) 0.046(6) Uiso 1 1 d . . . H7B H 0.4453(19) 0.2722(19) 0.1887(14) 0.029(5) Uiso 1 1 d . . . C8 C 0.68600(19) -0.07141(16) 0.16567(14) 0.0379(4) Uani 1 1 d . . . F8A F 0.58105(14) -0.11131(12) 0.16708(11) 0.0582(3) Uani 1 1 d . . . F8B F 0.78924(13) -0.16759(10) 0.21077(10) 0.0538(3) Uani 1 1 d . . . F8C F 0.72952(14) -0.06471(12) 0.06754(9) 0.0522(3) Uani 1 1 d . . . C9 C 0.54081(18) 0.06328(17) 0.34555(13) 0.0336(3) Uani 1 1 d . . . F9A F 0.61204(14) -0.05222(13) 0.38950(10) 0.0627(4) Uani 1 1 d . . . F9B F 0.51167(14) 0.15757(13) 0.41347(9) 0.0551(3) Uani 1 1 d . . . F9C F 0.42023(13) 0.05941(15) 0.32500(10) 0.0590(3) Uani 1 1 d . . . C10 C 0.90542(16) 0.33148(16) 0.02512(10) 0.0254(3) Uani 1 1 d . . . H10A H 0.911(2) 0.416(2) -0.0008(15) 0.039(5) Uiso 1 1 d . . . H10B H 0.9775(19) 0.2598(19) -0.0062(14) 0.028(4) Uiso 1 1 d . . . C11 C 1.11751(16) 0.25218(17) 0.16988(12) 0.0311(3) Uani 1 1 d . . . F11A F 1.14928(11) 0.27784(12) 0.26101(8) 0.0448(3) Uani 1 1 d . . . F11B F 1.17619(11) 0.30973(13) 0.09818(9) 0.0484(3) Uani 1 1 d . . . F11C F 1.17824(10) 0.12173(11) 0.15593(9) 0.0434(2) Uani 1 1 d . . . C12 C 0.87567(16) 0.48552(14) 0.20585(10) 0.0251(3) Uani 1 1 d . . . F12A F 0.96380(11) 0.54018(10) 0.16464(8) 0.0390(2) Uani 1 1 d . . . F12B F 0.75073(10) 0.56241(9) 0.17761(8) 0.0354(2) Uani 1 1 d . . . F12C F 0.87578(11) 0.49309(9) 0.30718(7) 0.0339(2) Uani 1 1 d . . . N1 N 0.84700(19) 0.27577(16) 0.57785(11) 0.0432(4) Uani 1 1 d . . . H1 H 0.860(2) 0.230(2) 0.5234(18) 0.053(6) Uiso 1 1 d . . . C14 C 0.7678(2) 0.4188(2) 0.54652(14) 0.0459(5) Uani 1 1 d . . . H14A H 0.686(3) 0.428(3) 0.524(2) 0.066(7) Uiso 1 1 d . . . H14B H 0.815(2) 0.436(2) 0.4915(19) 0.054(7) Uiso 1 1 d . . . C15 C 0.7426(2) 0.51580(19) 0.63103(17) 0.0435(4) Uani 1 1 d . . . H15A H 0.683(3) 0.496(2) 0.6891(19) 0.060(7) Uiso 1 1 d . . . H15B H 0.840(3) 0.510(2) 0.6517(18) 0.056(7) Uiso 1 1 d . . . H15C H 0.699(3) 0.597(3) 0.602(2) 0.077(9) Uiso 1 1 d . . . C16 C 0.9888(2) 0.25087(18) 0.61107(16) 0.0442(4) Uani 1 1 d . . . H16A H 0.972(2) 0.302(2) 0.6702(17) 0.042(5) Uiso 1 1 d . . . H16B H 1.027(3) 0.158(3) 0.6305(18) 0.059(7) Uiso 1 1 d . . . C17 C 1.0798(3) 0.2847(3) 0.5301(2) 0.0551(5) Uani 1 1 d . . . H17C H 1.174(3) 0.255(3) 0.557(2) 0.071(8) Uiso 1 1 d . . . H17B H 1.048(3) 0.379(3) 0.512(2) 0.063(7) Uiso 1 1 d . . . H17A H 1.088(3) 0.235(3) 0.472(2) 0.082(9) Uiso 1 1 d . . . C18 C 0.7707(3) 0.2218(2) 0.65847(18) 0.0549(6) Uani 1 1 d . . . H18A H 0.767(2) 0.269(2) 0.7207(18) 0.049(6) Uiso 1 1 d . . . H18B H 0.832(3) 0.125(3) 0.667(2) 0.066(7) Uiso 1 1 d . . . C19 C 0.6262(4) 0.2431(4) 0.6302(3) 0.0861(12) Uani 1 1 d . . . H19A H 0.596(4) 0.194(3) 0.679(3) 0.096(11) Uiso 1 1 d . . . H19B H 0.631(4) 0.203(4) 0.576(3) 0.103(12) Uiso 1 1 d . . . H19C H 0.564(5) 0.333(5) 0.632(3) 0.143(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01790(5) 0.01582(5) 0.01434(5) -0.00086(3) -0.00266(3) -0.00575(4) Cl1 0.0408(2) 0.02387(15) 0.01893(14) -0.00133(11) -0.01101(13) -0.00205(14) Cl2 0.02413(15) 0.02303(15) 0.02389(14) -0.00356(11) 0.00109(12) -0.00652(12) P1 0.02461(17) 0.02042(15) 0.02343(16) -0.00079(12) -0.00250(13) -0.01131(13) P2 0.01886(15) 0.02312(16) 0.01698(14) -0.00119(11) -0.00111(11) -0.00967(12) C1 0.0197(6) 0.0186(5) 0.0160(5) -0.0021(4) -0.0032(4) -0.0050(5) C13 0.0252(7) 0.0303(7) 0.0228(6) 0.0045(5) -0.0073(5) -0.0117(6) O1 0.0420(7) 0.0349(6) 0.0432(7) -0.0112(5) 0.0015(6) -0.0094(6) C2 0.0254(6) 0.0222(6) 0.0159(5) -0.0026(4) -0.0018(5) -0.0076(5) C3 0.0349(8) 0.0274(7) 0.0157(5) 0.0005(5) -0.0024(5) -0.0083(6) C4 0.0351(8) 0.0312(7) 0.0189(6) -0.0012(5) -0.0099(6) -0.0049(6) C5 0.0249(7) 0.0310(7) 0.0252(6) -0.0044(5) -0.0099(5) -0.0056(6) C6 0.0219(6) 0.0228(6) 0.0213(6) -0.0028(4) -0.0052(5) -0.0066(5) C7 0.0213(6) 0.0316(7) 0.0287(7) -0.0010(5) -0.0047(5) -0.0119(6) C8 0.0429(9) 0.0282(8) 0.0470(9) -0.0096(7) -0.0039(7) -0.0175(7) F8A 0.0613(8) 0.0471(7) 0.0837(9) -0.0193(6) -0.0047(7) -0.0381(6) F8B 0.0609(8) 0.0223(5) 0.0741(8) -0.0050(5) -0.0141(6) -0.0090(5) F8C 0.0697(8) 0.0464(6) 0.0431(6) -0.0217(5) 0.0033(6) -0.0243(6) C9 0.0352(8) 0.0339(8) 0.0358(8) 0.0056(6) 0.0009(6) -0.0190(7) F9A 0.0601(8) 0.0530(7) 0.0623(8) 0.0316(6) 0.0060(6) -0.0134(6) F9B 0.0780(9) 0.0587(7) 0.0382(6) -0.0096(5) 0.0222(6) -0.0412(7) F9C 0.0468(7) 0.0876(10) 0.0593(7) 0.0089(7) 0.0009(6) -0.0461(7) C10 0.0280(7) 0.0333(7) 0.0179(6) -0.0010(5) 0.0007(5) -0.0156(6) C11 0.0218(7) 0.0397(8) 0.0332(7) -0.0028(6) -0.0015(6) -0.0133(6) F11A 0.0321(5) 0.0624(7) 0.0431(6) -0.0092(5) -0.0146(4) -0.0181(5) F11B 0.0278(5) 0.0658(7) 0.0555(7) 0.0067(5) 0.0050(5) -0.0248(5) F11C 0.0238(5) 0.0404(6) 0.0594(7) -0.0102(5) -0.0013(4) -0.0044(4) C12 0.0310(7) 0.0268(7) 0.0215(6) -0.0007(5) 0.0003(5) -0.0158(6) F12A 0.0496(6) 0.0372(5) 0.0410(5) -0.0029(4) 0.0091(4) -0.0310(5) F12B 0.0365(5) 0.0241(4) 0.0428(5) 0.0016(4) -0.0085(4) -0.0077(4) F12C 0.0492(6) 0.0362(5) 0.0223(4) -0.0064(3) -0.0012(4) -0.0226(4) N1 0.0657(11) 0.0471(9) 0.0302(7) -0.0201(6) 0.0165(7) -0.0382(8) C14 0.0476(11) 0.0739(14) 0.0269(8) 0.0130(8) -0.0121(8) -0.0349(10) C15 0.0357(9) 0.0309(9) 0.0579(12) 0.0041(8) -0.0004(8) -0.0072(7) C16 0.0514(11) 0.0242(8) 0.0499(11) -0.0016(7) 0.0029(9) -0.0078(8) C17 0.0560(14) 0.0542(13) 0.0622(14) -0.0104(11) 0.0075(11) -0.0300(11) C18 0.0763(16) 0.0381(11) 0.0556(12) -0.0149(9) 0.0295(11) -0.0333(11) C19 0.104(3) 0.114(3) 0.078(2) -0.0437(19) 0.0387(18) -0.087(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C13 1.8810(15) . ? Ru1 C1 2.0959(12) . ? Ru1 P2 2.2623(4) . ? Ru1 P1 2.2794(4) . ? Ru1 Cl2 2.4381(4) . ? Ru1 Cl1 2.4997(4) . ? P1 C7 1.8209(15) . ? P1 C8 1.8809(16) . ? P1 C9 1.8886(17) . ? P2 C10 1.8150(14) . ? P2 C12 1.8868(14) . ? P2 C11 1.8900(15) . ? C1 C2 1.4098(19) . ? C1 C6 1.4116(18) . ? C13 O1 1.1042(19) . ? C2 C3 1.3945(18) . ? C2 C10 1.514(2) . ? C3 C4 1.389(2) . ? C3 H3 0.95(2) . ? C4 C5 1.380(2) . ? C4 H4 0.903(19) . ? C5 C6 1.3969(18) . ? C5 H5 0.92(2) . ? C6 C7 1.509(2) . ? C7 H7A 0.96(2) . ? C7 H7B 0.927(19) . ? C8 F8C 1.332(2) . ? C8 F8A 1.333(2) . ? C8 F8B 1.341(2) . ? C9 F9B 1.314(2) . ? C9 F9A 1.3232(19) . ? C9 F9C 1.336(2) . ? C10 H10A 0.99(2) . ? C10 H10B 0.934(19) . ? C11 F11C 1.3271(19) . ? C11 F11A 1.3322(18) . ? C11 F11B 1.3411(19) . ? C12 F12C 1.3294(16) . ? C12 F12B 1.3307(18) . ? C12 F12A 1.3484(16) . ? N1 C18 1.505(2) . ? N1 C16 1.509(3) . ? N1 C14 1.511(3) . ? N1 H1 0.86(2) . ? C14 C15 1.498(3) . ? C14 H14A 0.90(3) . ? C14 H14B 0.90(2) . ? C15 H15A 1.01(3) . ? C15 H15B 1.06(2) . ? C15 H15C 0.90(3) . ? C16 C17 1.496(3) . ? C16 H16A 0.94(2) . ? C16 H16B 0.96(2) . ? C17 H17C 1.01(3) . ? C17 H17B 0.98(3) . ? C17 H17A 0.93(3) . ? C18 C19 1.523(5) . ? C18 H18A 0.97(2) . ? C18 H18B 1.01(3) . ? C19 H19A 0.93(4) . ? C19 H19B 0.83(4) . ? C19 H19C 0.95(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Ru1 C1 93.18(5) . . ? C13 Ru1 P2 89.70(5) . . ? C1 Ru1 P2 79.73(4) . . ? C13 Ru1 P1 92.96(4) . . ? C1 Ru1 P1 79.38(4) . . ? P2 Ru1 P1 159.049(13) . . ? C13 Ru1 Cl2 177.56(4) . . ? C1 Ru1 Cl2 87.78(4) . . ? P2 Ru1 Cl2 92.673(14) . . ? P1 Ru1 Cl2 85.020(14) . . ? C13 Ru1 Cl1 89.49(4) . . ? C1 Ru1 Cl1 177.10(3) . . ? P2 Ru1 Cl1 99.172(14) . . ? P1 Ru1 Cl1 101.628(15) . . ? Cl2 Ru1 Cl1 89.593(13) . . ? C7 P1 C8 101.85(8) . . ? C7 P1 C9 103.84(7) . . ? C8 P1 C9 97.09(8) . . ? C7 P1 Ru1 105.70(5) . . ? C8 P1 Ru1 118.11(6) . . ? C9 P1 Ru1 127.04(5) . . ? C10 P2 C12 102.25(7) . . ? C10 P2 C11 102.72(7) . . ? C12 P2 C11 97.56(7) . . ? C10 P2 Ru1 106.00(5) . . ? C12 P2 Ru1 122.00(5) . . ? C11 P2 Ru1 123.20(5) . . ? C2 C1 C6 117.06(11) . . ? C2 C1 Ru1 121.24(9) . . ? C6 C1 Ru1 121.67(10) . . ? O1 C13 Ru1 177.77(13) . . ? C3 C2 C1 120.92(13) . . ? C3 C2 C10 119.98(13) . . ? C1 C2 C10 119.10(11) . . ? C4 C3 C2 120.94(14) . . ? C4 C3 H3 120.2(12) . . ? C2 C3 H3 118.8(12) . . ? C5 C4 C3 119.14(13) . . ? C5 C4 H4 121.1(12) . . ? C3 C4 H4 119.8(12) . . ? C4 C5 C6 120.66(14) . . ? C4 C5 H5 120.5(12) . . ? C6 C5 H5 118.7(13) . . ? C5 C6 C1 121.24(13) . . ? C5 C6 C7 119.62(13) . . ? C1 C6 C7 119.12(11) . . ? C6 C7 P1 105.88(9) . . ? C6 C7 H7A 114.3(13) . . ? P1 C7 H7A 109.1(13) . . ? C6 C7 H7B 108.6(12) . . ? P1 C7 H7B 107.6(11) . . ? H7A C7 H7B 111.1(17) . . ? F8C C8 F8A 107.18(14) . . ? F8C C8 F8B 106.86(15) . . ? F8A C8 F8B 107.50(15) . . ? F8C C8 P1 109.25(12) . . ? F8A C8 P1 113.86(13) . . ? F8B C8 P1 111.86(11) . . ? F9B C9 F9A 108.38(15) . . ? F9B C9 F9C 106.25(15) . . ? F9A C9 F9C 106.87(14) . . ? F9B C9 P1 111.50(11) . . ? F9A C9 P1 111.02(12) . . ? F9C C9 P1 112.55(12) . . ? C2 C10 P2 105.75(9) . . ? C2 C10 H10A 111.7(12) . . ? P2 C10 H10A 111.8(12) . . ? C2 C10 H10B 111.5(11) . . ? P2 C10 H10B 106.2(11) . . ? H10A C10 H10B 109.7(16) . . ? F11C C11 F11A 107.58(13) . . ? F11C C11 F11B 106.73(13) . . ? F11A C11 F11B 107.15(13) . . ? F11C C11 P2 110.24(10) . . ? F11A C11 P2 111.80(11) . . ? F11B C11 P2 113.05(11) . . ? F12C C12 F12B 108.42(12) . . ? F12C C12 F12A 106.02(11) . . ? F12B C12 F12A 107.08(12) . . ? F12C C12 P2 112.35(10) . . ? F12B C12 P2 110.47(9) . . ? F12A C12 P2 112.24(10) . . ? C18 N1 C16 109.56(18) . . ? C18 N1 C14 114.13(17) . . ? C16 N1 C14 113.42(14) . . ? C18 N1 H1 107.6(16) . . ? C16 N1 H1 105.9(16) . . ? C14 N1 H1 105.6(16) . . ? C15 C14 N1 113.57(14) . . ? C15 C14 H14A 108.7(17) . . ? N1 C14 H14A 110.5(17) . . ? C15 C14 H14B 112.1(15) . . ? N1 C14 H14B 106.7(15) . . ? H14A C14 H14B 105(2) . . ? C14 C15 H15A 108.9(14) . . ? C14 C15 H15B 107.8(13) . . ? H15A C15 H15B 114.8(19) . . ? C14 C15 H15C 105.2(18) . . ? H15A C15 H15C 111(2) . . ? H15B C15 H15C 108(2) . . ? C17 C16 N1 113.71(18) . . ? C17 C16 H16A 112.5(13) . . ? N1 C16 H16A 104.2(13) . . ? C17 C16 H16B 111.8(15) . . ? N1 C16 H16B 105.2(15) . . ? H16A C16 H16B 108.8(19) . . ? C16 C17 H17C 106.8(16) . . ? C16 C17 H17B 114.0(16) . . ? H17C C17 H17B 109(2) . . ? C16 C17 H17A 109.0(19) . . ? H17C C17 H17A 108(2) . . ? H17B C17 H17A 110(2) . . ? N1 C18 C19 112.6(2) . . ? N1 C18 H18A 105.1(14) . . ? C19 C18 H18A 110.9(14) . . ? N1 C18 H18B 105.5(15) . . ? C19 C18 H18B 112.9(15) . . ? H18A C18 H18B 109(2) . . ? C18 C19 H19A 104(2) . . ? C18 C19 H19B 110(3) . . ? H19A C19 H19B 103(3) . . ? C18 C19 H19C 114(3) . . ? H19A C19 H19C 109(3) . . ? H19B C19 H19C 115(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.500 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------- data_jja56 _database_code_depnum_ccdc_archive 'CCDC 886419' #TrackingRef '- Combined.cif' #Compound 2: [(CF3PCP)Ru(CO)Cl]2(\^I -CF3PCPH) #----------------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H22 Cl2 F36 O2 P6 Ru2' _chemical_formula_sum 'C38 H22 Cl2 F36 O2 P6 Ru2' _chemical_formula_weight 1653.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 38.3484(16) _cell_length_b 15.6169(5) _cell_length_c 9.1059(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.456(3) _cell_angle_gamma 90.00 _cell_volume 5303.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9620 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 33.80 _exptl_crystal_description rectangular_prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7818 _exptl_absorpt_correction_T_max 0.8878 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67258 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -60 _diffrn_reflns_limit_h_max 59 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 34.01 _reflns_number_total 10627 _reflns_number_gt 9435 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V. 6.10 (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL V. 6.10 (Bruker, 2001)' _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^)+(0.0417P)^2^+687.1965P] 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 10627 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1455 _refine_ls_R_factor_gt 0.1387 _refine_ls_wR_factor_ref 0.3659 _refine_ls_wR_factor_gt 0.3635 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.13054(2) 0.25679(5) 0.06222(9) 0.01402(16) Uani 1 1 d . . . Cl1 Cl 0.12022(7) 0.35013(18) 0.2624(3) 0.0233(5) Uani 1 1 d . . . P1 P 0.17887(7) 0.21838(18) 0.2525(3) 0.0195(5) Uani 1 1 d . . . P2 P 0.09927(8) 0.34089(19) -0.1331(3) 0.0212(5) Uani 1 1 d . . . P3 P 0.08652(7) 0.15626(17) 0.1087(3) 0.0182(5) Uani 1 1 d . . . C1 C 0.1701(4) 0.3479(8) 0.0379(15) 0.029(2) Uani 1 1 d . . . C13 C 0.1442(3) 0.1857(8) -0.0826(13) 0.024(2) Uani 1 1 d . . . O1 O 0.1537(3) 0.1495(7) -0.1743(13) 0.037(2) Uani 1 1 d . . . C2 C 0.1662(3) 0.3986(7) -0.0939(14) 0.025(2) Uani 1 1 d . . . C3 C 0.1923(4) 0.4572(8) -0.1126(15) 0.030(2) Uani 1 1 d . . . H3A H 0.1884 0.4908 -0.2019 0.036 Uiso 1 1 calc R . . C4 C 0.2234(4) 0.4671(9) -0.0050(18) 0.035(3) Uani 1 1 d . . . H4A H 0.2413 0.5060 -0.0197 0.042 Uiso 1 1 calc R . . C5 C 0.2286(3) 0.4168(8) 0.1329(17) 0.030(2) Uani 1 1 d . . . H5A H 0.2499 0.4221 0.2101 0.035 Uiso 1 1 calc R . . C6 C 0.2018(3) 0.3612(7) 0.1484(14) 0.024(2) Uani 1 1 d . . . C7 C 0.2062(3) 0.3146(7) 0.2970(13) 0.024(2) Uani 1 1 d . . . H7A H 0.1978 0.3504 0.3715 0.029 Uiso 1 1 calc R . . H7B H 0.2317 0.2995 0.3387 0.029 Uiso 1 1 calc R . . C8 C 0.1794(3) 0.1724(10) 0.4466(15) 0.033(3) Uani 1 1 d . . . F8A F 0.1895(3) 0.0941(8) 0.4681(13) 0.057(3) Uani 1 1 d . . . F8B F 0.1467(2) 0.1792(8) 0.4761(11) 0.050(3) Uani 1 1 d . . . F8C F 0.2011(3) 0.2189(8) 0.5557(11) 0.056(3) Uani 1 1 d . . . C9 C 0.2135(3) 0.1470(9) 0.2034(18) 0.035(3) Uani 1 1 d . . . F9A F 0.2425(2) 0.1372(6) 0.3137(12) 0.044(2) Uani 1 1 d . . . F9B F 0.2012(2) 0.0665(6) 0.1643(14) 0.048(3) Uani 1 1 d . . . F9C F 0.2234(3) 0.1764(7) 0.0861(12) 0.047(2) Uani 1 1 d . . . C10 C 0.1325(3) 0.3918(8) -0.2169(14) 0.027(2) Uani 1 1 d . . . H10A H 0.1368 0.3570 -0.3017 0.033 Uiso 1 1 calc R . . H10B H 0.1242 0.4494 -0.2555 0.033 Uiso 1 1 calc R . . C11 C 0.0680(5) 0.3032(12) -0.3138(17) 0.048(4) Uani 1 1 d . . . F11A F 0.0341(3) 0.2946(8) -0.2992(12) 0.066(4) Uani 1 1 d . . . F11B F 0.0796(4) 0.2260(7) -0.3508(12) 0.059(3) Uani 1 1 d . . . F11C F 0.0673(3) 0.3544(7) -0.4255(10) 0.053(3) Uani 1 1 d . . . C12 C 0.0726(4) 0.4346(10) -0.0913(18) 0.037(3) Uani 1 1 d . . . F12A F 0.0472(3) 0.4105(8) -0.0176(12) 0.053(3) Uani 1 1 d . . . F12B F 0.0550(3) 0.4734(7) -0.2176(13) 0.055(3) Uani 1 1 d . . . F12C F 0.0943(3) 0.4900(6) -0.0070(11) 0.049(3) Uani 1 1 d . . . C14 C 0.0000 0.1613(11) 0.2500 0.024(3) Uani 1 2 d S . . H14 H 0.0000 0.1005 0.2500 0.029 Uiso 1 2 calc SR . . C15 C 0.0318(3) 0.2061(8) 0.2580(12) 0.0227(19) Uani 1 1 d . . . C16 C 0.0320(3) 0.2949(8) 0.2591(14) 0.027(2) Uani 1 1 d . . . H16A H 0.0538 0.3253 0.2661 0.032 Uiso 1 1 calc R . . C17 C 0.0000 0.3396(13) 0.2500 0.032(3) Uani 1 2 d S . . H17 H 0.0000 0.4004 0.2500 0.038 Uiso 1 2 calc SR . . C18 C 0.0669(3) 0.1566(10) 0.2766(14) 0.029(2) Uani 1 1 d . . . H18A H 0.0626 0.0965 0.3027 0.035 Uiso 1 1 calc R . . H18B H 0.0846 0.1813 0.3627 0.035 Uiso 1 1 calc R . . C19 C 0.1066(4) 0.0439(7) 0.1210(16) 0.030(2) Uani 1 1 d . . . F19A F 0.0833(3) -0.0179(5) 0.1370(13) 0.044(2) Uani 1 1 d . . . F19B F 0.1187(3) 0.0245(5) 0.0023(11) 0.040(2) Uani 1 1 d . . . F19C F 0.1333(2) 0.0409(5) 0.2418(10) 0.0382(19) Uani 1 1 d . . . C20 C 0.0455(3) 0.1315(8) -0.0402(15) 0.029(2) Uani 1 1 d . . . F20A F 0.0545(3) 0.1066(7) -0.1712(9) 0.045(2) Uani 1 1 d . . . F20B F 0.0254(3) 0.0685(7) -0.0084(12) 0.046(2) Uani 1 1 d . . . F20C F 0.0256(2) 0.1998(6) -0.0755(10) 0.0376(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0126(3) 0.0126(3) 0.0169(3) 0.0003(2) 0.0035(2) 0.0002(2) Cl1 0.0188(10) 0.0268(12) 0.0249(11) -0.0066(9) 0.0064(8) -0.0001(9) P1 0.0133(10) 0.0203(11) 0.0241(12) 0.0021(9) 0.0029(9) 0.0028(8) P2 0.0225(12) 0.0197(11) 0.0193(11) 0.0020(9) 0.0008(9) -0.0025(9) P3 0.0166(10) 0.0177(11) 0.0215(11) 0.0005(9) 0.0070(9) -0.0006(8) C1 0.041(7) 0.021(5) 0.033(6) -0.001(4) 0.024(5) -0.001(4) C13 0.020(4) 0.031(5) 0.023(5) -0.003(4) 0.008(4) -0.001(4) O1 0.043(5) 0.031(5) 0.048(6) -0.006(4) 0.031(5) 0.001(4) C2 0.026(5) 0.018(4) 0.035(6) 0.004(4) 0.018(4) -0.002(4) C3 0.034(6) 0.025(5) 0.032(6) 0.005(4) 0.011(5) -0.002(5) C4 0.028(6) 0.029(6) 0.055(8) -0.009(6) 0.025(6) -0.012(5) C5 0.017(4) 0.024(5) 0.049(7) -0.009(5) 0.011(5) -0.004(4) C6 0.021(5) 0.021(4) 0.030(5) -0.008(4) 0.008(4) -0.009(4) C7 0.014(4) 0.025(5) 0.030(5) -0.005(4) -0.002(4) -0.003(3) C8 0.025(5) 0.039(7) 0.030(6) 0.013(5) -0.001(4) -0.005(5) F8A 0.057(6) 0.059(7) 0.055(6) 0.035(5) 0.013(5) 0.024(5) F8B 0.029(4) 0.088(8) 0.035(4) 0.024(5) 0.009(3) 0.002(5) F8C 0.048(6) 0.080(8) 0.033(5) 0.009(5) -0.007(4) -0.018(5) C9 0.022(5) 0.034(6) 0.051(8) 0.006(6) 0.009(5) 0.013(5) F9A 0.021(4) 0.042(5) 0.065(6) 0.007(4) 0.003(4) 0.013(3) F9B 0.030(4) 0.024(4) 0.094(8) -0.008(4) 0.022(5) 0.004(3) F9C 0.042(5) 0.046(5) 0.059(6) 0.010(5) 0.026(5) 0.020(4) C10 0.026(5) 0.027(5) 0.030(5) 0.010(4) 0.008(4) 0.000(4) C11 0.052(9) 0.060(10) 0.028(6) 0.007(6) -0.002(6) -0.034(8) F11A 0.047(6) 0.086(8) 0.049(6) 0.031(6) -0.023(5) -0.042(6) F11B 0.092(9) 0.046(6) 0.034(5) -0.011(4) 0.001(5) -0.018(6) F11C 0.064(7) 0.056(6) 0.029(4) 0.012(4) -0.011(4) -0.021(5) C12 0.028(6) 0.039(7) 0.044(7) 0.012(6) 0.009(5) 0.011(5) F12A 0.042(5) 0.069(7) 0.057(6) 0.027(5) 0.028(5) 0.024(5) F12B 0.054(6) 0.052(6) 0.053(6) 0.023(5) 0.004(5) 0.026(5) F12C 0.073(7) 0.022(4) 0.044(5) -0.008(3) -0.001(5) 0.006(4) C14 0.020(6) 0.026(7) 0.027(7) 0.000 0.008(5) 0.000 C15 0.019(4) 0.029(5) 0.018(4) 0.000(4) 0.002(3) -0.003(4) C16 0.025(5) 0.027(5) 0.028(5) -0.003(4) 0.006(4) -0.001(4) C17 0.027(8) 0.030(8) 0.039(9) 0.000 0.009(7) 0.000 C18 0.021(5) 0.047(7) 0.024(5) 0.002(5) 0.013(4) 0.004(5) C19 0.041(7) 0.014(4) 0.038(6) 0.005(4) 0.017(5) -0.004(4) F19A 0.046(5) 0.018(3) 0.074(7) 0.009(4) 0.025(5) -0.006(3) F19B 0.056(5) 0.024(4) 0.049(5) 0.001(3) 0.032(4) 0.010(4) F19C 0.043(5) 0.030(4) 0.042(5) 0.011(3) 0.011(4) 0.013(3) C20 0.027(5) 0.028(5) 0.031(6) -0.008(4) 0.006(4) -0.015(4) F20A 0.045(5) 0.068(7) 0.024(4) -0.010(4) 0.013(3) -0.013(5) F20B 0.039(5) 0.048(5) 0.054(6) -0.004(4) 0.014(4) -0.027(4) F20C 0.021(3) 0.049(5) 0.037(4) 0.002(4) -0.005(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C13 1.888(11) . ? Ru1 C1 2.130(12) . ? Ru1 P1 2.303(3) . ? Ru1 P2 2.309(3) . ? Ru1 P3 2.414(3) . ? Ru1 Cl1 2.437(3) . ? P1 C7 1.823(11) . ? P1 C9 1.865(13) . ? P1 C8 1.903(13) . ? P2 C10 1.814(12) . ? P2 C12 1.875(15) . ? P2 C11 1.890(15) . ? P3 C18 1.855(11) . ? P3 C20 1.864(12) . ? P3 C19 1.909(12) . ? C1 C6 1.400(18) . ? C1 C2 1.416(17) . ? C13 O1 1.136(14) . ? C2 C3 1.398(16) . ? C2 C10 1.503(18) . ? C3 C4 1.36(2) . ? C3 H3A 0.9500 . ? C4 C5 1.45(2) . ? C4 H4A 0.9500 . ? C5 C6 1.378(15) . ? C5 H5A 0.9500 . ? C6 C7 1.511(17) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 F8A 1.282(18) . ? C8 F8B 1.349(16) . ? C8 F8C 1.350(17) . ? C9 F9C 1.298(18) . ? C9 F9A 1.322(16) . ? C9 F9B 1.360(18) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 F11C 1.289(17) . ? C11 F11A 1.34(2) . ? C11 F11B 1.35(2) . ? C12 F12C 1.317(19) . ? C12 F12B 1.336(17) . ? C12 F12A 1.357(17) . ? C14 C15 1.393(14) . ? C14 C15 1.393(14) 2 ? C14 H14 0.9500 . ? C15 C16 1.388(17) . ? C15 C18 1.525(17) . ? C16 C17 1.398(16) . ? C16 H16A 0.9500 . ? C17 C16 1.398(16) 2 ? C17 H17 0.9500 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 F19B 1.308(15) . ? C19 F19C 1.318(17) . ? C19 F19A 1.347(14) . ? C20 F20C 1.307(16) . ? C20 F20B 1.323(14) . ? C20 F20A 1.374(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Ru1 C1 90.0(5) . . ? C13 Ru1 P1 93.8(4) . . ? C1 Ru1 P1 77.5(4) . . ? C13 Ru1 P2 88.6(4) . . ? C1 Ru1 P2 78.2(4) . . ? P1 Ru1 P2 155.57(11) . . ? C13 Ru1 P3 93.4(4) . . ? C1 Ru1 P3 175.9(4) . . ? P1 Ru1 P3 99.89(10) . . ? P2 Ru1 P3 104.24(10) . . ? C13 Ru1 Cl1 173.4(4) . . ? C1 Ru1 Cl1 85.5(3) . . ? P1 Ru1 Cl1 80.52(10) . . ? P2 Ru1 Cl1 95.18(10) . . ? P3 Ru1 Cl1 90.91(10) . . ? C7 P1 C9 98.1(6) . . ? C7 P1 C8 102.9(6) . . ? C9 P1 C8 98.2(7) . . ? C7 P1 Ru1 105.9(4) . . ? C9 P1 Ru1 117.9(5) . . ? C8 P1 Ru1 129.1(4) . . ? C10 P2 C12 102.3(7) . . ? C10 P2 C11 97.8(6) . . ? C12 P2 C11 98.9(9) . . ? C10 P2 Ru1 106.5(4) . . ? C12 P2 Ru1 119.8(5) . . ? C11 P2 Ru1 127.2(6) . . ? C18 P3 C20 99.4(6) . . ? C18 P3 C19 100.9(6) . . ? C20 P3 C19 96.5(6) . . ? C18 P3 Ru1 125.3(5) . . ? C20 P3 Ru1 120.9(4) . . ? C19 P3 Ru1 108.6(4) . . ? C6 C1 C2 115.5(11) . . ? C6 C1 Ru1 123.0(9) . . ? C2 C1 Ru1 121.5(10) . . ? O1 C13 Ru1 173.8(11) . . ? C3 C2 C1 122.0(12) . . ? C3 C2 C10 118.2(11) . . ? C1 C2 C10 119.7(10) . . ? C4 C3 C2 121.2(12) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 118.7(11) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? C6 C5 C4 118.3(12) . . ? C6 C5 H5A 120.9 . . ? C4 C5 H5A 120.9 . . ? C5 C6 C1 124.2(12) . . ? C5 C6 C7 117.6(11) . . ? C1 C6 C7 118.1(9) . . ? C6 C7 P1 105.0(7) . . ? C6 C7 H7A 110.8 . . ? P1 C7 H7A 110.8 . . ? C6 C7 H7B 110.8 . . ? P1 C7 H7B 110.8 . . ? H7A C7 H7B 108.8 . . ? F8A C8 F8B 107.8(12) . . ? F8A C8 F8C 106.8(12) . . ? F8B C8 F8C 104.6(13) . . ? F8A C8 P1 116.1(12) . . ? F8B C8 P1 110.2(8) . . ? F8C C8 P1 110.6(9) . . ? F9C C9 F9A 108.1(12) . . ? F9C C9 F9B 105.2(13) . . ? F9A C9 F9B 105.8(11) . . ? F9C C9 P1 110.3(9) . . ? F9A C9 P1 114.0(11) . . ? F9B C9 P1 113.1(9) . . ? C2 C10 P2 106.5(8) . . ? C2 C10 H10A 110.4 . . ? P2 C10 H10A 110.4 . . ? C2 C10 H10B 110.4 . . ? P2 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? F11C C11 F11A 107.3(15) . . ? F11C C11 F11B 107.7(15) . . ? F11A C11 F11B 108.4(14) . . ? F11C C11 P2 112.7(10) . . ? F11A C11 P2 112.2(12) . . ? F11B C11 P2 108.4(12) . . ? F12C C12 F12B 109.2(13) . . ? F12C C12 F12A 108.9(14) . . ? F12B C12 F12A 106.0(12) . . ? F12C C12 P2 109.3(10) . . ? F12B C12 P2 111.7(11) . . ? F12A C12 P2 111.8(11) . . ? C15 C14 C15 119.8(16) . 2 ? C15 C14 H14 120.1 . . ? C15 C14 H14 120.1 2 . ? C16 C15 C14 120.4(12) . . ? C16 C15 C18 120.2(11) . . ? C14 C15 C18 119.3(12) . . ? C15 C16 C17 119.6(13) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C16 C17 C16 120.2(18) . 2 ? C16 C17 H17 119.9 . . ? C16 C17 H17 119.9 2 . ? C15 C18 P3 115.2(9) . . ? C15 C18 H18A 108.5 . . ? P3 C18 H18A 108.5 . . ? C15 C18 H18B 108.5 . . ? P3 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? F19B C19 F19C 109.0(12) . . ? F19B C19 F19A 107.2(11) . . ? F19C C19 F19A 106.9(10) . . ? F19B C19 P3 112.4(8) . . ? F19C C19 P3 107.8(9) . . ? F19A C19 P3 113.3(9) . . ? F20C C20 F20B 109.0(11) . . ? F20C C20 F20A 105.6(11) . . ? F20B C20 F20A 104.9(10) . . ? F20C C20 P3 110.8(8) . . ? F20B C20 P3 115.5(10) . . ? F20A C20 P3 110.4(9) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 34.01 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 6.918 _refine_diff_density_min -6.093 _refine_diff_density_rms 0.423 #----------------------------------------------------------------------------- data_jja17 _database_code_depnum_ccdc_archive 'CCDC 886420' #TrackingRef '- Combined.cif' #Compound 3: cis-(CF3PCP)Ru(CO)2Cl #----------------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H7 Cl F12 O2 P2 Ru' _chemical_formula_sum 'C14 H7 Cl F12 O2 P2 Ru' _chemical_formula_weight 633.66 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 7.8669(3) _cell_length_b 18.9807(6) _cell_length_c 26.8450(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4008.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9955 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 33.24 _exptl_crystal_description rectangular_prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.100 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 1.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6042 _exptl_absorpt_correction_T_max 0.8602 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27654 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 32.03 _reflns_number_total 6976 _reflns_number_gt 5939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2004)' _computing_cell_refinement 'Bruker SMART (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V. 6.10 (Bruker, 2004)' _computing_publication_material 'Bruker SHELXTL V. 6.10 (Bruker, 2004)' _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^)+(0.0198P)^2^+3.9589P] 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 6976 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.160735(18) 0.052842(7) 0.110749(5) 0.01507(4) Uani 1 1 d . . . Cl1 Cl 0.36542(6) 0.03994(2) 0.177836(16) 0.02195(9) Uani 1 1 d . . . P1 P 0.30520(6) 0.15473(2) 0.092832(16) 0.01685(9) Uani 1 1 d . . . P2 P -0.02809(6) -0.02011(2) 0.150212(17) 0.01793(9) Uani 1 1 d . . . C1 C 0.0084(3) 0.06781(10) 0.05758(7) 0.0221(4) Uani 1 1 d . . . C2 C 0.2983(3) -0.01774(11) 0.07355(8) 0.0285(4) Uani 1 1 d . . . C3 C 0.0345(2) 0.12582(8) 0.15869(6) 0.0156(3) Uani 1 1 d . . . O1 O -0.0775(2) 0.07765(9) 0.02441(5) 0.0319(3) Uani 1 1 d . . . O2 O 0.3817(3) -0.05772(10) 0.05466(8) 0.0546(6) Uani 1 1 d . . . C4 C -0.1143(2) 0.10791(9) 0.18468(6) 0.0171(3) Uani 1 1 d . . . C5 C -0.2003(2) 0.15753(10) 0.21374(7) 0.0223(4) Uani 1 1 d . . . H5A H -0.3002 0.1443 0.2313 0.027 Uiso 1 1 calc R . . C6 C -0.1399(3) 0.22594(10) 0.21702(7) 0.0243(4) Uani 1 1 d . . . H6A H -0.2021 0.2604 0.2351 0.029 Uiso 1 1 calc R . . C7 C 0.0113(3) 0.24391(9) 0.19389(6) 0.0219(4) Uani 1 1 d . . . H7A H 0.0547 0.2904 0.1970 0.026 Uiso 1 1 calc R . . C8 C 0.0999(2) 0.19404(9) 0.16616(6) 0.0181(3) Uani 1 1 d . . . C9 C 0.2751(3) 0.21193(9) 0.14613(6) 0.0208(3) Uani 1 1 d . . . H9A H 0.3633 0.2030 0.1717 0.025 Uiso 1 1 calc R . . H9B H 0.2808 0.2620 0.1360 0.025 Uiso 1 1 calc R . . C10 C 0.5387(3) 0.15688(10) 0.07690(7) 0.0245(4) Uani 1 1 d . . . F10A F 0.6167(2) 0.21275(9) 0.09518(8) 0.0678(6) Uani 1 1 d . . . F10B F 0.61811(18) 0.10102(8) 0.09393(6) 0.0486(4) Uani 1 1 d . . . F10C F 0.5618(2) 0.15776(10) 0.02815(5) 0.0539(4) Uani 1 1 d . . . C11 C 0.2248(3) 0.21224(11) 0.04106(7) 0.0266(4) Uani 1 1 d . . . F11A F 0.06392(17) 0.22974(7) 0.05079(5) 0.0391(3) Uani 1 1 d . . . F11B F 0.31379(18) 0.27182(6) 0.03688(5) 0.0364(3) Uani 1 1 d . . . F11C F 0.2284(2) 0.17999(7) -0.00290(4) 0.0406(3) Uani 1 1 d . . . C12 C -0.1815(2) 0.03340(9) 0.18365(7) 0.0215(3) Uani 1 1 d . . . H12A H -0.2931 0.0319 0.1666 0.026 Uiso 1 1 calc R . . H12B H -0.1961 0.0155 0.2180 0.026 Uiso 1 1 calc R . . C13 C -0.1597(3) -0.08250(11) 0.11181(8) 0.0303(4) Uani 1 1 d . . . F13A F -0.29304(19) -0.10883(8) 0.13570(6) 0.0468(4) Uani 1 1 d . . . F13B F -0.2192(2) -0.04893(7) 0.07169(5) 0.0410(3) Uani 1 1 d . . . F13C F -0.0645(2) -0.13595(7) 0.09591(6) 0.0473(4) Uani 1 1 d . . . C14 C 0.0504(3) -0.08594(10) 0.19749(8) 0.0265(4) Uani 1 1 d . . . F14A F 0.18588(19) -0.12060(7) 0.18056(5) 0.0398(3) Uani 1 1 d . . . F14B F 0.09380(18) -0.05409(6) 0.23959(4) 0.0315(3) Uani 1 1 d . . . F14C F -0.0675(2) -0.13400(7) 0.20920(6) 0.0462(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01429(6) 0.01617(6) 0.01474(6) -0.00267(4) -0.00088(5) 0.00116(5) Cl1 0.01749(19) 0.0279(2) 0.02042(18) 0.00129(15) -0.00375(16) 0.00057(16) P1 0.0170(2) 0.01892(19) 0.01457(17) 0.00067(15) 0.00066(16) -0.00005(17) P2 0.0172(2) 0.01502(18) 0.0216(2) -0.00073(15) -0.00260(17) -0.00139(17) C1 0.0210(9) 0.0244(8) 0.0210(8) -0.0037(6) 0.0018(7) 0.0005(7) C2 0.0243(10) 0.0324(10) 0.0287(9) -0.0117(8) -0.0043(8) 0.0046(8) C3 0.0161(7) 0.0171(7) 0.0137(6) -0.0005(5) -0.0014(6) 0.0036(6) O1 0.0271(8) 0.0442(9) 0.0245(7) 0.0016(6) -0.0082(6) -0.0006(7) O2 0.0405(10) 0.0604(12) 0.0630(12) -0.0370(10) -0.0049(10) 0.0216(9) C4 0.0168(7) 0.0184(7) 0.0160(7) 0.0011(6) 0.0005(6) 0.0015(6) C5 0.0203(8) 0.0263(8) 0.0202(8) 0.0011(7) 0.0060(7) 0.0041(7) C6 0.0264(10) 0.0238(8) 0.0227(8) -0.0032(7) 0.0048(8) 0.0070(8) C7 0.0276(9) 0.0177(7) 0.0203(8) -0.0026(6) 0.0021(7) 0.0023(7) C8 0.0198(8) 0.0192(7) 0.0151(7) -0.0005(6) 0.0011(6) 0.0003(7) C9 0.0226(9) 0.0204(8) 0.0196(7) -0.0036(6) 0.0016(7) -0.0042(7) C10 0.0203(9) 0.0271(9) 0.0260(9) 0.0024(7) 0.0040(8) -0.0005(8) F10A 0.0306(8) 0.0586(10) 0.1144(16) -0.0362(10) 0.0169(10) -0.0183(8) F10B 0.0258(7) 0.0554(9) 0.0647(10) 0.0314(8) 0.0139(7) 0.0130(7) F10C 0.0380(8) 0.0960(13) 0.0277(7) 0.0170(7) 0.0149(6) 0.0173(9) C11 0.0296(10) 0.0275(9) 0.0227(8) 0.0048(7) -0.0041(8) 0.0014(8) F11A 0.0293(7) 0.0445(8) 0.0436(8) 0.0158(6) -0.0041(6) 0.0100(6) F11B 0.0431(8) 0.0286(6) 0.0374(7) 0.0133(5) -0.0043(6) -0.0058(6) F11C 0.0566(9) 0.0470(8) 0.0182(5) 0.0032(5) -0.0082(6) -0.0020(7) C12 0.0175(8) 0.0201(7) 0.0268(8) 0.0016(6) 0.0033(7) 0.0006(7) C13 0.0305(10) 0.0256(9) 0.0346(10) -0.0022(8) -0.0064(9) -0.0073(9) F13A 0.0394(8) 0.0505(8) 0.0505(8) 0.0027(7) -0.0077(7) -0.0273(7) F13B 0.0424(8) 0.0422(7) 0.0384(7) 0.0030(6) -0.0219(7) -0.0132(6) F13C 0.0549(10) 0.0304(7) 0.0566(9) -0.0217(6) -0.0137(8) 0.0015(7) C14 0.0277(10) 0.0180(8) 0.0338(10) 0.0032(7) -0.0053(9) -0.0020(8) F14A 0.0434(8) 0.0263(6) 0.0496(8) -0.0018(6) -0.0061(7) 0.0173(6) F14B 0.0359(7) 0.0329(6) 0.0258(6) 0.0022(5) -0.0072(5) -0.0022(6) F14C 0.0475(9) 0.0324(7) 0.0587(9) 0.0222(6) -0.0160(8) -0.0188(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.8850(19) . ? Ru1 C2 1.991(2) . ? Ru1 C3 2.1358(16) . ? Ru1 P2 2.2905(5) . ? Ru1 P1 2.2941(5) . ? Ru1 Cl1 2.4282(5) . ? P1 C9 1.8115(17) . ? P1 C11 1.8769(19) . ? P1 C10 1.886(2) . ? P2 C12 1.8150(19) . ? P2 C13 1.880(2) . ? P2 C14 1.885(2) . ? C1 O1 1.134(2) . ? C2 O2 1.124(2) . ? C3 C4 1.404(2) . ? C3 C8 1.408(2) . ? C4 C5 1.398(2) . ? C4 C12 1.510(2) . ? C5 C6 1.385(3) . ? C5 H5A 0.9500 . ? C6 C7 1.385(3) . ? C6 H6A 0.9500 . ? C7 C8 1.391(2) . ? C7 H7A 0.9500 . ? C8 C9 1.518(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 F10B 1.313(2) . ? C10 F10A 1.320(2) . ? C10 F10C 1.321(2) . ? C11 F11C 1.330(2) . ? C11 F11A 1.335(3) . ? C11 F11B 1.335(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 F13A 1.328(3) . ? C13 F13C 1.331(3) . ? C13 F13B 1.336(2) . ? C14 F14B 1.326(2) . ? C14 F14A 1.332(2) . ? C14 F14C 1.339(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 93.85(8) . . ? C1 Ru1 C3 93.60(7) . . ? C2 Ru1 C3 172.54(7) . . ? C1 Ru1 P2 91.67(6) . . ? C2 Ru1 P2 100.24(7) . . ? C3 Ru1 P2 79.15(5) . . ? C1 Ru1 P1 91.67(6) . . ? C2 Ru1 P1 101.12(7) . . ? C3 Ru1 P1 79.04(5) . . ? P2 Ru1 P1 158.107(17) . . ? C1 Ru1 Cl1 176.62(6) . . ? C2 Ru1 Cl1 86.77(6) . . ? C3 Ru1 Cl1 85.81(5) . . ? P2 Ru1 Cl1 91.495(16) . . ? P1 Ru1 Cl1 84.951(16) . . ? C9 P1 C11 101.08(9) . . ? C9 P1 C10 107.06(9) . . ? C11 P1 C10 98.49(9) . . ? C9 P1 Ru1 105.95(6) . . ? C11 P1 Ru1 118.60(7) . . ? C10 P1 Ru1 123.24(6) . . ? C12 P2 C13 104.92(10) . . ? C12 P2 C14 104.82(9) . . ? C13 P2 C14 97.60(9) . . ? C12 P2 Ru1 108.76(6) . . ? C13 P2 Ru1 118.95(7) . . ? C14 P2 Ru1 119.97(7) . . ? O1 C1 Ru1 177.12(18) . . ? O2 C2 Ru1 176.30(19) . . ? C4 C3 C8 117.17(15) . . ? C4 C3 Ru1 122.00(12) . . ? C8 C3 Ru1 120.82(12) . . ? C5 C4 C3 121.18(16) . . ? C5 C4 C12 118.14(16) . . ? C3 C4 C12 120.64(15) . . ? C6 C5 C4 120.07(17) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C7 C6 C5 119.79(17) . . ? C7 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C6 C7 C8 120.17(17) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C7 C8 C3 121.26(17) . . ? C7 C8 C9 119.47(16) . . ? C3 C8 C9 119.16(15) . . ? C8 C9 P1 105.33(12) . . ? C8 C9 H9A 110.7 . . ? P1 C9 H9A 110.7 . . ? C8 C9 H9B 110.7 . . ? P1 C9 H9B 110.7 . . ? H9A C9 H9B 108.8 . . ? F10B C10 F10A 107.34(19) . . ? F10B C10 F10C 106.83(17) . . ? F10A C10 F10C 107.10(18) . . ? F10B C10 P1 111.54(13) . . ? F10A C10 P1 112.70(14) . . ? F10C C10 P1 111.02(14) . . ? F11C C11 F11A 107.95(18) . . ? F11C C11 F11B 107.72(17) . . ? F11A C11 F11B 107.64(17) . . ? F11C C11 P1 112.48(14) . . ? F11A C11 P1 108.62(13) . . ? F11B C11 P1 112.24(14) . . ? C4 C12 P2 107.46(12) . . ? C4 C12 H12A 110.2 . . ? P2 C12 H12A 110.2 . . ? C4 C12 H12B 110.2 . . ? P2 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? F13A C13 F13C 108.20(18) . . ? F13A C13 F13B 106.96(18) . . ? F13C C13 F13B 107.59(18) . . ? F13A C13 P2 114.03(15) . . ? F13C C13 P2 110.27(15) . . ? F13B C13 P2 109.55(14) . . ? F14B C14 F14A 108.07(17) . . ? F14B C14 F14C 106.79(17) . . ? F14A C14 F14C 107.34(16) . . ? F14B C14 P2 110.85(12) . . ? F14A C14 P2 111.08(14) . . ? F14C C14 P2 112.49(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 32.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.755 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.084 #----------------------------------------------------------------------------- data_jja46 _database_code_depnum_ccdc_archive 'CCDC 886421' #TrackingRef '- Combined.cif' #Compound 6: cis-(CF3PCP)Ru(CO)2(H) #----------------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H8 F12 O2 P2 Ru' _chemical_formula_sum 'C14 H8 F12 O2 P2 Ru' _chemical_formula_weight 599.21 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' 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 P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 7.3937(2) _cell_length_b 19.1595(6) _cell_length_c 13.8088(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.646(2) _cell_angle_gamma 90.00 _cell_volume 1943.0(1) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9185 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 33.59 _exptl_crystal_description rectangular_prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8030 _exptl_absorpt_correction_T_max 0.8782 _exptl_absorpt_process_details 'SADABS, (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17658 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 33.14 _reflns_number_total 7374 _reflns_number_gt 5738 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V. 6.10 (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL V. 6.10 (Bruker, 2001)' _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^)+(0.0250P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7374 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0713 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.538730(18) 0.358267(7) 0.212719(10) 0.01856(4) Uani 1 1 d . . . H1 H 0.377(3) 0.4106(13) 0.1785(18) 0.049(7) Uiso 1 1 d . . . P1 P 0.68187(6) 0.45982(3) 0.25264(4) 0.02179(10) Uani 1 1 d . . . P2 P 0.40573(6) 0.27886(3) 0.10670(3) 0.02159(10) Uani 1 1 d . . . C1 C 0.6432(2) 0.38553(10) 0.07858(13) 0.0211(3) Uani 1 1 d . . . C13 C 0.7445(3) 0.29602(10) 0.25337(14) 0.0265(4) Uani 1 1 d . . . C14 C 0.4054(3) 0.34474(10) 0.32460(15) 0.0261(4) Uani 1 1 d . . . O1 O 0.8640(2) 0.26026(9) 0.27574(12) 0.0436(4) Uani 1 1 d . . . O2 O 0.3207(2) 0.33957(9) 0.38774(12) 0.0427(4) Uani 1 1 d . . . C2 C 0.6396(2) 0.33683(10) 0.00134(14) 0.0236(4) Uani 1 1 d . . . C3 C 0.7049(3) 0.35443(12) -0.08608(15) 0.0284(4) Uani 1 1 d . . . H3 H 0.704(3) 0.3203(11) -0.1380(16) 0.027(5) Uiso 1 1 d . . . C4 C 0.7739(3) 0.42012(12) -0.09897(15) 0.0309(4) Uani 1 1 d . . . H4 H 0.819(3) 0.4316(13) -0.1568(18) 0.043(7) Uiso 1 1 d . . . C5 C 0.7756(3) 0.46936(11) -0.02553(15) 0.0281(4) Uani 1 1 d . . . H5 H 0.825(3) 0.5150(12) -0.0325(15) 0.027(6) Uiso 1 1 d . . . C6 C 0.7104(2) 0.45254(10) 0.06255(14) 0.0237(4) Uani 1 1 d . . . C7 C 0.7045(3) 0.50711(10) 0.14092(15) 0.0259(4) Uani 1 1 d . . . H7A H 0.602(3) 0.5339(11) 0.1278(14) 0.018(5) Uiso 1 1 d . . . H7B H 0.808(3) 0.5364(11) 0.1475(15) 0.032(6) Uiso 1 1 d . . . C8 C 0.9239(3) 0.45516(11) 0.31134(16) 0.0304(4) Uani 1 1 d . . . F8A F 0.93923(17) 0.41642(8) 0.39172(9) 0.0438(3) Uani 1 1 d . . . F8B F 1.02458(16) 0.42495(8) 0.24882(10) 0.0433(3) Uani 1 1 d . . . F8C F 0.99797(17) 0.51716(7) 0.33431(12) 0.0494(4) Uani 1 1 d . . . C9 C 0.5945(3) 0.52560(12) 0.33670(17) 0.0339(5) Uani 1 1 d . . . F9A F 0.6419(2) 0.50811(9) 0.42979(11) 0.0574(4) Uani 1 1 d . . . F9C F 0.41483(17) 0.52864(7) 0.32273(11) 0.0478(4) Uani 1 1 d . . . F9B F 0.6573(2) 0.58966(7) 0.32419(13) 0.0577(4) Uani 1 1 d . . . C10 C 0.5613(3) 0.26548(11) 0.01558(15) 0.0269(4) Uani 1 1 d . . . H10A H 0.499(3) 0.2497(12) -0.0383(19) 0.036(6) Uiso 1 1 d . . . H10B H 0.651(3) 0.2305(13) 0.0432(17) 0.042(7) Uiso 1 1 d . . . C11 C 0.3473(3) 0.18791(11) 0.14252(16) 0.0349(5) Uani 1 1 d . . . F11A F 0.3340(2) 0.14286(7) 0.06865(11) 0.0550(4) Uani 1 1 d . . . F11B F 0.4760(2) 0.16461(7) 0.21062(11) 0.0521(4) Uani 1 1 d . . . F11C F 0.18913(19) 0.18659(7) 0.18078(10) 0.0478(4) Uani 1 1 d . . . C12 C 0.1845(3) 0.30103(11) 0.03253(16) 0.0307(4) Uani 1 1 d . . . F12A F 0.20675(19) 0.35464(7) -0.02500(11) 0.0462(3) Uani 1 1 d . . . F12B F 0.05823(17) 0.31719(9) 0.08910(11) 0.0539(4) Uani 1 1 d . . . F12C F 0.12007(19) 0.24857(8) -0.02485(11) 0.0514(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01797(7) 0.02024(7) 0.01767(7) 0.00185(5) 0.00290(5) 0.00192(5) P1 0.0192(2) 0.0227(2) 0.0235(2) -0.00050(18) 0.00249(17) 0.00086(17) P2 0.0237(2) 0.0209(2) 0.0205(2) 0.00045(18) 0.00428(18) -0.00107(18) C1 0.0154(7) 0.0267(9) 0.0211(8) 0.0044(7) 0.0026(6) 0.0029(6) C13 0.0285(9) 0.0298(10) 0.0211(9) 0.0007(8) 0.0024(7) 0.0044(8) C14 0.0251(9) 0.0298(10) 0.0238(9) 0.0041(8) 0.0040(7) 0.0046(7) O1 0.0409(9) 0.0489(10) 0.0397(9) 0.0039(8) -0.0009(7) 0.0206(8) O2 0.0395(9) 0.0542(10) 0.0379(9) 0.0157(8) 0.0190(7) 0.0120(7) C2 0.0198(8) 0.0306(10) 0.0208(9) 0.0017(7) 0.0041(7) 0.0019(7) C3 0.0246(9) 0.0421(12) 0.0191(9) 0.0000(9) 0.0047(7) 0.0025(8) C4 0.0255(9) 0.0450(13) 0.0234(10) 0.0088(9) 0.0073(8) 0.0011(9) C5 0.0213(9) 0.0334(11) 0.0299(10) 0.0127(9) 0.0045(8) -0.0004(8) C6 0.0174(8) 0.0276(9) 0.0256(9) 0.0049(8) 0.0011(7) 0.0023(7) C7 0.0224(9) 0.0246(9) 0.0305(10) 0.0052(8) 0.0024(8) 0.0009(8) C8 0.0264(9) 0.0339(11) 0.0300(10) -0.0001(9) 0.0001(8) -0.0029(8) F8A 0.0374(7) 0.0571(9) 0.0344(7) 0.0122(6) -0.0058(6) 0.0003(6) F8B 0.0244(6) 0.0615(9) 0.0442(8) -0.0023(7) 0.0048(5) 0.0098(6) F8C 0.0346(7) 0.0415(8) 0.0687(10) -0.0047(7) -0.0088(7) -0.0115(6) C9 0.0328(10) 0.0328(11) 0.0371(12) -0.0060(9) 0.0082(9) 0.0024(9) F9A 0.0691(10) 0.0702(11) 0.0333(8) -0.0131(7) 0.0076(7) 0.0165(8) F9C 0.0341(7) 0.0493(8) 0.0616(9) -0.0155(7) 0.0131(7) 0.0091(6) F9B 0.0645(9) 0.0293(7) 0.0842(12) -0.0181(7) 0.0288(9) -0.0071(7) C10 0.0294(10) 0.0304(10) 0.0217(9) -0.0044(8) 0.0059(8) 0.0002(8) C11 0.0506(13) 0.0253(10) 0.0298(11) -0.0012(9) 0.0083(10) -0.0042(9) F11A 0.0985(12) 0.0270(7) 0.0417(8) -0.0095(6) 0.0172(8) -0.0096(7) F11B 0.0752(10) 0.0295(7) 0.0493(9) 0.0132(6) -0.0030(8) 0.0056(7) F11C 0.0607(9) 0.0408(8) 0.0457(8) 0.0026(6) 0.0224(7) -0.0192(6) C12 0.0265(9) 0.0341(11) 0.0310(10) -0.0038(9) 0.0005(8) -0.0040(8) F12A 0.0415(7) 0.0453(8) 0.0480(8) 0.0175(7) -0.0101(6) -0.0008(6) F12B 0.0269(6) 0.0864(12) 0.0484(9) -0.0066(8) 0.0047(6) 0.0080(7) F12C 0.0490(8) 0.0485(9) 0.0516(9) -0.0153(7) -0.0168(7) -0.0090(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C14 1.944(2) . ? Ru1 C13 1.9634(19) . ? Ru1 C1 2.1520(18) . ? Ru1 P1 2.2527(5) . ? Ru1 P2 2.2565(5) . ? Ru1 H1 1.59(2) . ? P1 C7 1.813(2) . ? P1 C9 1.878(2) . ? P1 C8 1.879(2) . ? P2 C10 1.8186(19) . ? P2 C12 1.875(2) . ? P2 C11 1.876(2) . ? C1 C6 1.404(3) . ? C1 C2 1.415(3) . ? C13 O1 1.132(2) . ? C14 O2 1.135(2) . ? C2 C3 1.392(3) . ? C2 C10 1.506(3) . ? C3 C4 1.377(3) . ? C3 H3 0.97(2) . ? C4 C5 1.384(3) . ? C4 H4 0.93(2) . ? C5 C6 1.397(3) . ? C5 H5 0.96(2) . ? C6 C7 1.509(3) . ? C7 H7A 0.91(2) . ? C7 H7B 0.95(2) . ? C8 F8A 1.329(2) . ? C8 F8C 1.331(2) . ? C8 F8B 1.336(2) . ? C9 F9C 1.321(2) . ? C9 F9B 1.331(3) . ? C9 F9A 1.335(3) . ? C10 H10A 0.88(2) . ? C10 H10B 0.99(2) . ? C11 F11A 1.331(2) . ? C11 F11B 1.335(3) . ? C11 F11C 1.338(3) . ? C12 F12A 1.320(2) . ? C12 F12B 1.322(2) . ? C12 F12C 1.333(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Ru1 C13 98.01(8) . . ? C14 Ru1 C1 169.10(7) . . ? C13 Ru1 C1 92.88(7) . . ? C14 Ru1 P1 100.83(6) . . ? C13 Ru1 P1 97.36(6) . . ? C1 Ru1 P1 78.22(5) . . ? C14 Ru1 P2 101.70(6) . . ? C13 Ru1 P2 92.35(6) . . ? C1 Ru1 P2 77.17(5) . . ? P1 Ru1 P2 153.924(19) . . ? C14 Ru1 H1 83.5(9) . . ? C13 Ru1 H1 177.9(9) . . ? C1 Ru1 H1 85.6(9) . . ? P1 Ru1 H1 81.0(9) . . ? P2 Ru1 H1 88.7(9) . . ? C7 P1 C9 105.23(10) . . ? C7 P1 C8 102.35(9) . . ? C9 P1 C8 98.27(10) . . ? C7 P1 Ru1 108.08(7) . . ? C9 P1 Ru1 123.05(7) . . ? C8 P1 Ru1 117.48(7) . . ? C10 P2 C12 103.63(10) . . ? C10 P2 C11 103.59(10) . . ? C12 P2 C11 98.13(10) . . ? C10 P2 Ru1 106.31(7) . . ? C12 P2 Ru1 119.26(7) . . ? C11 P2 Ru1 123.48(7) . . ? C6 C1 C2 117.41(17) . . ? C6 C1 Ru1 121.77(14) . . ? C2 C1 Ru1 120.77(13) . . ? O1 C13 Ru1 179.16(18) . . ? O2 C14 Ru1 176.14(17) . . ? C3 C2 C1 121.05(18) . . ? C3 C2 C10 120.66(18) . . ? C1 C2 C10 118.29(16) . . ? C4 C3 C2 120.3(2) . . ? C4 C3 H3 119.4(13) . . ? C2 C3 H3 120.3(13) . . ? C3 C4 C5 120.01(19) . . ? C3 C4 H4 120.2(16) . . ? C5 C4 H4 119.8(16) . . ? C4 C5 C6 120.40(19) . . ? C4 C5 H5 121.3(13) . . ? C6 C5 H5 118.2(13) . . ? C5 C6 C1 120.82(18) . . ? C5 C6 C7 120.41(18) . . ? C1 C6 C7 118.73(17) . . ? C6 C7 P1 106.08(13) . . ? C6 C7 H7A 109.8(12) . . ? P1 C7 H7A 107.2(12) . . ? C6 C7 H7B 112.9(13) . . ? P1 C7 H7B 111.6(13) . . ? H7A C7 H7B 109.1(18) . . ? F8A C8 F8C 107.84(17) . . ? F8A C8 F8B 107.31(17) . . ? F8C C8 F8B 107.20(17) . . ? F8A C8 P1 111.84(14) . . ? F8C C8 P1 113.93(14) . . ? F8B C8 P1 108.42(14) . . ? F9C C9 F9B 107.51(18) . . ? F9C C9 F9A 107.41(18) . . ? F9B C9 F9A 107.44(19) . . ? F9C C9 P1 110.57(15) . . ? F9B C9 P1 112.85(15) . . ? F9A C9 P1 110.84(15) . . ? C2 C10 P2 104.23(13) . . ? C2 C10 H10A 111.8(15) . . ? P2 C10 H10A 108.9(15) . . ? C2 C10 H10B 114.4(14) . . ? P2 C10 H10B 106.3(14) . . ? H10A C10 H10B 111(2) . . ? F11A C11 F11B 107.82(18) . . ? F11A C11 F11C 107.48(19) . . ? F11B C11 F11C 107.46(18) . . ? F11A C11 P2 113.51(15) . . ? F11B C11 P2 109.21(15) . . ? F11C C11 P2 111.13(15) . . ? F12A C12 F12B 108.59(18) . . ? F12A C12 F12C 106.84(17) . . ? F12B C12 F12C 107.42(16) . . ? F12A C12 P2 110.09(14) . . ? F12B C12 P2 111.19(14) . . ? F12C C12 P2 112.53(14) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.547 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.096 #----------------------------------------------------------------------------- data_cl01 _database_code_depnum_ccdc_archive 'CCDC 886422' #TrackingRef '- Combined.cif' #Compound 8: (CF3PCP)Ru(CO)(PPh3)(H) #----------------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H23 F12 O P3 Ru' _chemical_formula_sum 'C31 H23 F12 O P3 Ru' _chemical_formula_weight 833.47 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5524(5) _cell_length_b 11.1009(7) _cell_length_c 16.8061(9) _cell_angle_alpha 82.842(4) _cell_angle_beta 75.036(4) _cell_angle_gamma 68.235(4) _cell_volume 1598.13(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4950 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 29.96 _exptl_crystal_description rectangular_prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8423 _exptl_absorpt_correction_T_max 0.9128 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11206 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5478 _reflns_number_gt 4552 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V. 6.14 (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL V. 6.14 (Bruker, 2001)' _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^)+(0.1136P)^2^+10.9524P] 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 5478 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.2010 _refine_ls_wR_factor_gt 0.1910 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.50715(6) 0.60961(5) 0.72321(3) 0.0155(2) Uani 1 1 d . . . H1 H 0.3851(18) 0.6642(17) 0.6683(14) 0.018(6) Uiso 1 1 d . . . P1 P 0.6515(2) 0.67063(18) 0.60818(11) 0.0182(4) Uani 1 1 d . . . P2 P 0.3713(2) 0.48464(18) 0.79229(12) 0.0210(4) Uani 1 1 d . . . P3 P 0.3745(2) 0.81157(17) 0.79271(11) 0.0171(4) Uani 1 1 d . . . C1 C 0.5936(8) 0.4415(7) 0.6475(4) 0.0189(14) Uani 1 1 d . . . C13 C 0.6642(9) 0.5378(8) 0.7870(5) 0.0280(17) Uani 1 1 d . . . O1 O 0.7598(8) 0.4975(7) 0.8223(5) 0.0497(18) Uani 1 1 d . . . C2 C 0.5784(9) 0.3219(7) 0.6788(5) 0.0255(16) Uani 1 1 d . . . C3 C 0.6362(9) 0.2129(8) 0.6305(6) 0.0324(19) Uani 1 1 d . . . H3A H 0.6252 0.1335 0.6538 0.039 Uiso 1 1 calc R . . C4 C 0.7100(9) 0.2210(8) 0.5483(6) 0.0332(19) Uani 1 1 d . . . H4A H 0.7533 0.1462 0.5157 0.040 Uiso 1 1 calc R . . C5 C 0.7202(8) 0.3375(7) 0.5142(5) 0.0248(16) Uani 1 1 d . . . H5A H 0.7673 0.3437 0.4575 0.030 Uiso 1 1 calc R . . C6 C 0.6618(8) 0.4471(7) 0.5625(5) 0.0240(16) Uani 1 1 d . . . C7 C 0.6642(8) 0.5771(7) 0.5231(4) 0.0220(15) Uani 1 1 d . . . H7A H 0.5751 0.6203 0.4972 0.026 Uiso 1 1 calc R . . H7B H 0.7613 0.5663 0.4807 0.026 Uiso 1 1 calc R . . C8 C 0.6037(9) 0.8405(8) 0.5619(5) 0.0269(17) Uani 1 1 d . . . F8A F 0.6942(7) 0.8473(6) 0.4886(3) 0.0607(18) Uani 1 1 d . . . F8B F 0.6081(8) 0.9230(5) 0.6104(4) 0.0532(15) Uani 1 1 d . . . F8C F 0.4598(6) 0.8830(5) 0.5512(3) 0.0421(13) Uani 1 1 d . . . C9 C 0.8644(9) 0.6361(8) 0.5986(5) 0.0287(18) Uani 1 1 d . . . F9A F 0.8927(6) 0.7184(6) 0.6374(4) 0.0530(16) Uani 1 1 d . . . F9B F 0.9284(5) 0.5174(6) 0.6301(4) 0.0492(15) Uani 1 1 d . . . F9C F 0.9440(5) 0.6364(5) 0.5204(3) 0.0363(11) Uani 1 1 d . . . C10 C 0.4935(9) 0.3174(7) 0.7666(5) 0.0293(18) Uani 1 1 d . . . H10A H 0.5673 0.2812 0.8029 0.035 Uiso 1 1 calc R . . H10B H 0.4294 0.2626 0.7734 0.035 Uiso 1 1 calc R . . C11 C 0.1875(9) 0.5010(8) 0.7630(5) 0.0294(18) Uani 1 1 d . . . F11A F 0.1238(6) 0.4155(5) 0.8023(4) 0.0467(14) Uani 1 1 d . . . F11B F 0.2168(6) 0.4808(5) 0.6824(3) 0.0425(13) Uani 1 1 d . . . F11C F 0.0807(5) 0.6175(5) 0.7771(4) 0.0403(12) Uani 1 1 d . . . C12 C 0.3013(10) 0.4607(8) 0.9072(5) 0.0329(19) Uani 1 1 d . . . F12A F 0.4079(6) 0.4619(5) 0.9451(3) 0.0408(12) Uani 1 1 d . . . F12B F 0.2828(7) 0.3463(5) 0.9268(3) 0.0455(14) Uani 1 1 d . . . F12C F 0.1666(6) 0.5509(5) 0.9389(3) 0.0361(11) Uani 1 1 d . . . C14 C 0.4933(8) 0.8890(7) 0.8220(4) 0.0207(15) Uani 1 1 d . . . C15 C 0.4282(9) 0.9899(7) 0.8775(4) 0.0222(15) Uani 1 1 d . . . H15A H 0.3194 1.0215 0.8996 0.027 Uiso 1 1 calc R . . C16 C 0.5198(9) 1.0440(7) 0.9006(5) 0.0259(17) Uani 1 1 d . . . H16A H 0.4740 1.1120 0.9387 0.031 Uiso 1 1 calc R . . C17 C 0.6788(10) 0.9996(8) 0.8685(5) 0.0312(18) Uani 1 1 d . . . H17A H 0.7416 1.0383 0.8834 0.037 Uiso 1 1 calc R . . C18 C 0.7447(10) 0.8990(9) 0.8147(6) 0.037(2) Uani 1 1 d . . . H18A H 0.8535 0.8676 0.7928 0.044 Uiso 1 1 calc R . . C19 C 0.6515(9) 0.8427(8) 0.7920(5) 0.0255(16) Uani 1 1 d . . . H19A H 0.6980 0.7722 0.7557 0.031 Uiso 1 1 calc R . . C20 C 0.2440(9) 0.8081(7) 0.8945(4) 0.0206(15) Uani 1 1 d . . . C21 C 0.0851(9) 0.8502(8) 0.9072(5) 0.0274(17) Uani 1 1 d . . . H21A H 0.0382 0.8857 0.8621 0.033 Uiso 1 1 calc R . . C22 C -0.0075(10) 0.8419(9) 0.9847(6) 0.037(2) Uani 1 1 d . . . H22A H -0.1166 0.8693 0.9921 0.045 Uiso 1 1 calc R . . C23 C 0.0590(11) 0.7940(9) 1.0507(5) 0.037(2) Uani 1 1 d . . . H23A H -0.0044 0.7897 1.1040 0.044 Uiso 1 1 calc R . . C24 C 0.2175(11) 0.7522(9) 1.0398(5) 0.036(2) Uani 1 1 d . . . H24A H 0.2632 0.7200 1.0857 0.044 Uiso 1 1 calc R . . C25 C 0.3110(9) 0.7570(8) 0.9613(5) 0.0262(16) Uani 1 1 d . . . H25A H 0.4205 0.7254 0.9536 0.031 Uiso 1 1 calc R . . C26 C 0.2438(8) 0.9416(7) 0.7376(5) 0.0206(15) Uani 1 1 d . . . C27 C 0.1477(8) 0.9100(7) 0.7010(5) 0.0247(16) Uani 1 1 d . . . H27A H 0.1552 0.8221 0.7015 0.030 Uiso 1 1 calc R . . C28 C 0.0409(9) 1.0058(8) 0.6640(5) 0.0311(18) Uani 1 1 d . . . H28A H -0.0255 0.9833 0.6400 0.037 Uiso 1 1 calc R . . C29 C 0.0298(10) 1.1353(8) 0.6614(5) 0.0324(18) Uani 1 1 d . . . H29A H -0.0449 1.2011 0.6370 0.039 Uiso 1 1 calc R . . C30 C 0.1291(10) 1.1656(8) 0.6949(5) 0.0329(19) Uani 1 1 d . . . H30A H 0.1256 1.2527 0.6916 0.039 Uiso 1 1 calc R . . C31 C 0.2353(10) 1.0696(8) 0.7339(5) 0.0277(17) Uani 1 1 d . . . H31A H 0.3017 1.0922 0.7579 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0144(3) 0.0165(3) 0.0165(3) -0.0005(2) -0.0042(2) -0.0060(2) P1 0.0157(9) 0.0209(9) 0.0181(9) -0.0008(7) -0.0032(7) -0.0071(7) P2 0.0198(9) 0.0200(9) 0.0238(10) 0.0001(8) -0.0048(8) -0.0080(8) P3 0.0157(9) 0.0191(9) 0.0154(9) -0.0008(7) -0.0026(7) -0.0057(7) C1 0.013(3) 0.023(4) 0.019(4) -0.004(3) -0.005(3) -0.004(3) C13 0.025(4) 0.031(4) 0.027(4) 0.002(3) -0.001(3) -0.013(3) O1 0.041(4) 0.066(5) 0.056(4) 0.022(4) -0.034(3) -0.026(3) C2 0.020(4) 0.023(4) 0.033(4) -0.004(3) -0.008(3) -0.004(3) C3 0.025(4) 0.020(4) 0.055(6) -0.006(4) -0.013(4) -0.007(3) C4 0.021(4) 0.031(4) 0.046(5) -0.018(4) -0.008(4) -0.002(3) C5 0.019(4) 0.031(4) 0.027(4) -0.011(3) -0.008(3) -0.006(3) C6 0.014(3) 0.026(4) 0.034(4) -0.009(3) -0.007(3) -0.005(3) C7 0.020(4) 0.027(4) 0.016(3) -0.003(3) -0.004(3) -0.005(3) C8 0.031(4) 0.030(4) 0.019(4) -0.003(3) -0.001(3) -0.012(3) F8A 0.065(4) 0.044(3) 0.037(3) 0.017(3) 0.019(3) -0.005(3) F8B 0.088(5) 0.031(3) 0.060(4) 0.008(3) -0.040(3) -0.032(3) F8C 0.038(3) 0.032(3) 0.055(3) 0.010(2) -0.018(2) -0.010(2) C9 0.022(4) 0.042(5) 0.023(4) -0.007(4) -0.001(3) -0.014(4) F9A 0.026(3) 0.085(4) 0.057(4) -0.041(3) 0.006(2) -0.028(3) F9B 0.020(2) 0.060(4) 0.055(3) 0.017(3) -0.013(2) -0.004(2) F9C 0.022(2) 0.055(3) 0.031(3) -0.011(2) 0.0042(19) -0.017(2) C10 0.025(4) 0.021(4) 0.042(5) 0.000(3) -0.006(3) -0.009(3) C11 0.031(4) 0.033(4) 0.033(4) 0.001(3) -0.009(3) -0.020(4) F11A 0.036(3) 0.051(3) 0.065(4) 0.008(3) -0.013(3) -0.032(3) F11B 0.040(3) 0.059(3) 0.041(3) -0.010(3) -0.016(2) -0.024(3) F11C 0.025(2) 0.032(3) 0.062(3) -0.001(2) -0.017(2) -0.004(2) C12 0.037(5) 0.029(4) 0.030(4) 0.000(3) -0.003(4) -0.012(4) F12A 0.049(3) 0.045(3) 0.028(3) 0.007(2) -0.015(2) -0.014(2) F12B 0.064(4) 0.030(3) 0.036(3) 0.004(2) 0.006(3) -0.022(3) F12C 0.037(3) 0.034(3) 0.031(3) -0.003(2) 0.005(2) -0.014(2) C14 0.019(4) 0.023(4) 0.020(4) -0.001(3) -0.005(3) -0.008(3) C15 0.026(4) 0.021(4) 0.018(4) 0.003(3) -0.005(3) -0.008(3) C16 0.039(5) 0.018(4) 0.023(4) 0.000(3) -0.009(3) -0.011(3) C17 0.037(5) 0.028(4) 0.039(5) 0.002(4) -0.017(4) -0.018(4) C18 0.023(4) 0.040(5) 0.050(6) -0.008(4) -0.005(4) -0.015(4) C19 0.022(4) 0.031(4) 0.027(4) -0.008(3) -0.004(3) -0.012(3) C20 0.027(4) 0.021(4) 0.014(3) 0.000(3) -0.002(3) -0.010(3) C21 0.026(4) 0.035(4) 0.016(4) 0.002(3) 0.000(3) -0.008(3) C22 0.027(4) 0.040(5) 0.036(5) 0.002(4) 0.003(4) -0.010(4) C23 0.047(5) 0.037(5) 0.022(4) -0.002(4) 0.004(4) -0.018(4) C24 0.055(6) 0.041(5) 0.020(4) 0.005(4) -0.008(4) -0.027(4) C25 0.029(4) 0.030(4) 0.021(4) 0.006(3) -0.009(3) -0.012(3) C26 0.013(3) 0.024(4) 0.023(4) -0.004(3) -0.001(3) -0.005(3) C27 0.020(4) 0.023(4) 0.030(4) 0.002(3) -0.005(3) -0.009(3) C28 0.023(4) 0.039(5) 0.038(5) 0.002(4) -0.012(4) -0.016(4) C29 0.028(4) 0.029(4) 0.035(5) 0.008(4) -0.011(4) -0.006(3) C30 0.047(5) 0.025(4) 0.028(4) 0.003(3) -0.013(4) -0.011(4) C31 0.034(4) 0.029(4) 0.022(4) -0.002(3) -0.008(3) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C13 1.941(9) . ? Ru1 C1 2.166(7) . ? Ru1 P1 2.2553(18) . ? Ru1 P2 2.2609(19) . ? Ru1 P3 2.4037(18) . ? Ru1 H1 1.57(7) . ? P1 C7 1.823(7) . ? P1 C8 1.884(8) . ? P1 C9 1.892(8) . ? P2 C10 1.824(8) . ? P2 C11 1.884(8) . ? P2 C12 1.893(9) . ? P3 C14 1.840(7) . ? P3 C20 1.844(7) . ? P3 C26 1.852(8) . ? C1 C2 1.411(11) . ? C1 C6 1.412(11) . ? C13 O1 1.138(10) . ? C2 C3 1.395(11) . ? C2 C10 1.494(12) . ? C3 C4 1.388(13) . ? C3 H3A 0.9500 . ? C4 C5 1.375(12) . ? C4 H4A 0.9500 . ? C5 C6 1.399(10) . ? C5 H5A 0.9500 . ? C6 C7 1.518(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 F8B 1.319(9) . ? C8 F8A 1.321(9) . ? C8 F8C 1.330(10) . ? C9 F9A 1.325(9) . ? C9 F9B 1.337(10) . ? C9 F9C 1.339(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 F11C 1.320(10) . ? C11 F11A 1.331(9) . ? C11 F11B 1.341(10) . ? C12 F12C 1.329(10) . ? C12 F12B 1.336(10) . ? C12 F12A 1.338(10) . ? C14 C19 1.377(10) . ? C14 C15 1.399(10) . ? C15 C16 1.379(11) . ? C15 H15A 0.9500 . ? C16 C17 1.389(12) . ? C16 H16A 0.9500 . ? C17 C18 1.377(12) . ? C17 H17A 0.9500 . ? C18 C19 1.406(11) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.378(11) . ? C20 C25 1.391(11) . ? C21 C22 1.386(11) . ? C21 H21A 0.9500 . ? C22 C23 1.373(13) . ? C22 H22A 0.9500 . ? C23 C24 1.377(13) . ? C23 H23A 0.9500 . ? C24 C25 1.397(11) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C31 1.387(11) . ? C26 C27 1.389(11) . ? C27 C28 1.385(11) . ? C27 H27A 0.9500 . ? C28 C29 1.398(12) . ? C28 H28A 0.9500 . ? C29 C30 1.374(13) . ? C29 H29A 0.9500 . ? C30 C31 1.400(12) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Ru1 C1 94.2(3) . . ? C13 Ru1 P1 98.7(2) . . ? C1 Ru1 P1 77.41(19) . . ? C13 Ru1 P2 92.5(2) . . ? C1 Ru1 P2 76.57(19) . . ? P1 Ru1 P2 152.30(7) . . ? C13 Ru1 P3 96.5(2) . . ? C1 Ru1 P3 169.29(19) . . ? P1 Ru1 P3 101.18(7) . . ? P2 Ru1 P3 102.61(7) . . ? C13 Ru1 H1 177(2) . . ? C1 Ru1 H1 83(2) . . ? P1 Ru1 H1 80(2) . . ? P2 Ru1 H1 88(2) . . ? P3 Ru1 H1 86(2) . . ? C7 P1 C8 102.3(3) . . ? C7 P1 C9 99.9(3) . . ? C8 P1 C9 96.9(4) . . ? C7 P1 Ru1 108.3(2) . . ? C8 P1 Ru1 124.9(2) . . ? C9 P1 Ru1 120.7(3) . . ? C10 P2 C11 102.3(4) . . ? C10 P2 C12 99.2(4) . . ? C11 P2 C12 96.9(4) . . ? C10 P2 Ru1 106.3(3) . . ? C11 P2 Ru1 118.3(3) . . ? C12 P2 Ru1 129.7(3) . . ? C14 P3 C20 98.4(3) . . ? C14 P3 C26 104.7(3) . . ? C20 P3 C26 101.4(3) . . ? C14 P3 Ru1 117.6(2) . . ? C20 P3 Ru1 116.9(2) . . ? C26 P3 Ru1 115.2(2) . . ? C2 C1 C6 115.9(7) . . ? C2 C1 Ru1 122.2(5) . . ? C6 C1 Ru1 121.8(5) . . ? O1 C13 Ru1 177.5(7) . . ? C3 C2 C1 122.3(7) . . ? C3 C2 C10 120.9(7) . . ? C1 C2 C10 116.8(7) . . ? C4 C3 C2 119.7(8) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C5 C4 C3 119.8(7) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 C6 120.5(8) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C5 C6 C1 121.6(7) . . ? C5 C6 C7 120.0(7) . . ? C1 C6 C7 118.4(6) . . ? C6 C7 P1 104.5(5) . . ? C6 C7 H7A 110.9 . . ? P1 C7 H7A 110.9 . . ? C6 C7 H7B 110.9 . . ? P1 C7 H7B 110.9 . . ? H7A C7 H7B 108.9 . . ? F8B C8 F8A 109.0(7) . . ? F8B C8 F8C 106.4(7) . . ? F8A C8 F8C 106.4(7) . . ? F8B C8 P1 112.4(6) . . ? F8A C8 P1 113.0(5) . . ? F8C C8 P1 109.2(5) . . ? F9A C9 F9B 107.3(7) . . ? F9A C9 F9C 106.5(6) . . ? F9B C9 F9C 106.0(6) . . ? F9A C9 P1 114.2(5) . . ? F9B C9 P1 109.3(5) . . ? F9C C9 P1 113.1(5) . . ? C2 C10 P2 106.1(5) . . ? C2 C10 H10A 110.5 . . ? P2 C10 H10A 110.5 . . ? C2 C10 H10B 110.5 . . ? P2 C10 H10B 110.5 . . ? H10A C10 H10B 108.7 . . ? F11C C11 F11A 107.1(7) . . ? F11C C11 F11B 107.4(7) . . ? F11A C11 F11B 106.2(6) . . ? F11C C11 P2 112.4(5) . . ? F11A C11 P2 113.5(6) . . ? F11B C11 P2 109.9(5) . . ? F12C C12 F12B 106.5(7) . . ? F12C C12 F12A 108.9(7) . . ? F12B C12 F12A 106.5(7) . . ? F12C C12 P2 113.3(6) . . ? F12B C12 P2 112.4(6) . . ? F12A C12 P2 108.9(6) . . ? C19 C14 C15 118.7(7) . . ? C19 C14 P3 119.5(6) . . ? C15 C14 P3 121.7(5) . . ? C16 C15 C14 120.8(7) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 120.4(7) . . ? C15 C16 H16A 119.8 . . ? C17 C16 H16A 119.8 . . ? C18 C17 C16 119.4(7) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 120.2(8) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C14 C19 C18 120.4(8) . . ? C14 C19 H19A 119.8 . . ? C18 C19 H19A 119.8 . . ? C21 C20 C25 118.7(7) . . ? C21 C20 P3 123.6(6) . . ? C25 C20 P3 117.7(6) . . ? C20 C21 C22 121.2(8) . . ? C20 C21 H21A 119.4 . . ? C22 C21 H21A 119.4 . . ? C23 C22 C21 119.8(8) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C22 C23 C24 120.1(8) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C23 C24 C25 120.0(8) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C20 C25 C24 120.1(8) . . ? C20 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C31 C26 C27 119.1(7) . . ? C31 C26 P3 122.3(6) . . ? C27 C26 P3 118.5(6) . . ? C28 C27 C26 120.3(7) . . ? C28 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? C27 C28 C29 120.8(8) . . ? C27 C28 H28A 119.6 . . ? C29 C28 H28A 119.6 . . ? C30 C29 C28 118.8(8) . . ? C30 C29 H29A 120.6 . . ? C28 C29 H29A 120.6 . . ? C29 C30 C31 120.7(8) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C26 C31 C30 120.2(8) . . ? C26 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 3.182 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.190 #----------------------------------------------------------------------------- data_jja95m _database_code_depnum_ccdc_archive 'CCDC 886423' #TrackingRef '- Combined.cif' #Compound 9: (CF3PCP)Ru(CO)3+B(C6F5)4- #----------------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C24 B F20), 2(C15 H7 F12 O3 P2 Ru), C H2 Cl2' _chemical_formula_sum 'C79 H16 B2 Cl2 F64 O6 P4 Ru2' _chemical_formula_weight 2695.46 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 18.6632(4) _cell_length_b 20.1318(5) _cell_length_c 23.9866(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9012.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7686 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 29.59 _exptl_crystal_description rectangular_plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.987 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5224 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7887 _exptl_absorpt_correction_T_max 0.9484 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 66906 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 30.51 _reflns_number_total 13752 _reflns_number_gt 8458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 V. 2.2 (Bruker AXS Inc, 2007)' _computing_cell_refinement 'Bruker APEX2 V. 2.2 (Bruker AXS Inc, 2007)' _computing_data_reduction 'Bruker SAINT V. 7.34a (Bruker AXS Inc, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL V. 6.14 (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL V. 6.14 (Bruker, 2001)' _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^)+(0.0537P)^2^+12.7418P] 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 13752 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.7500 0.7500 0.192117(12) 0.02397(8) Uani 1 2 d S . . P1 P 0.65351(5) 0.68114(4) 0.17393(3) 0.02780(17) Uani 1 1 d . . . C1 C 0.7500 0.7500 0.10233(15) 0.0247(8) Uani 1 2 d S . . C8 C 0.7500 0.7500 0.27569(18) 0.0315(9) Uani 1 2 d S . . C9 C 0.81559(19) 0.67333(16) 0.19005(12) 0.0317(7) Uani 1 1 d . . . O1 O 0.7500 0.7500 0.32258(13) 0.0463(9) Uani 1 2 d S . . O2 O 0.85280(15) 0.62989(13) 0.19008(10) 0.0450(6) Uani 1 1 d . . . C2 C 0.69395(19) 0.72087(15) 0.07204(12) 0.0311(7) Uani 1 1 d . . . C3 C 0.6950(2) 0.72014(16) 0.01391(12) 0.0343(7) Uani 1 1 d . . . H3A H 0.6574 0.6988 -0.0060 0.041 Uiso 1 1 calc R . . C4 C 0.7500 0.7500 -0.01491(17) 0.0317(9) Uani 1 2 d S . . H4A H 0.7500 0.7500 -0.0545 0.038 Uiso 1 2 calc SR . . C5 C 0.6289(2) 0.69384(19) 0.10173(13) 0.0403(8) Uani 1 1 d . . . H5A H 0.6138 0.6513 0.0847 0.048 Uiso 1 1 calc R . . H5B H 0.5887 0.7257 0.0991 0.048 Uiso 1 1 calc R . . C6 C 0.6680(2) 0.58932(18) 0.18272(15) 0.0447(9) Uani 1 1 d . . . F6A F 0.69494(15) 0.57670(11) 0.23191(9) 0.0585(7) Uani 1 1 d . . . F6B F 0.60972(14) 0.55407(11) 0.17586(12) 0.0620(7) Uani 1 1 d . . . F6C F 0.71693(16) 0.57074(12) 0.14494(11) 0.0667(7) Uani 1 1 d . . . C7 C 0.5670(2) 0.6904(2) 0.21301(16) 0.0477(9) Uani 1 1 d . . . F7A F 0.57307(16) 0.66692(16) 0.26410(10) 0.0765(9) Uani 1 1 d . . . F7B F 0.51324(13) 0.65948(13) 0.18624(12) 0.0671(7) Uani 1 1 d . . . F7C F 0.54925(11) 0.75330(11) 0.21594(10) 0.0494(5) Uani 1 1 d . . . Ru2 Ru 0.7500 0.2500 0.146617(13) 0.02900(9) Uani 1 2 d S . . C10 C 0.7500 0.2500 0.23629(16) 0.0262(8) Uani 1 2 d S . . C17 C 0.82763(19) 0.18348(18) 0.14983(12) 0.0352(7) Uani 1 1 d . . . C18 C 0.7500 0.2500 0.0632(2) 0.0433(12) Uani 1 2 d S . . O3 O 0.87209(16) 0.14652(14) 0.15134(11) 0.0510(7) Uani 1 1 d . . . O4 O 0.7500 0.2500 0.01619(14) 0.0590(12) Uani 1 2 d S . . P2 P 0.66448(5) 0.16976(5) 0.16425(4) 0.0371(2) Uani 1 1 d . . . C11 C 0.69789(18) 0.21503(15) 0.26626(12) 0.0317(7) Uani 1 1 d . . . C12 C 0.6987(2) 0.21497(16) 0.32442(13) 0.0372(8) Uani 1 1 d . . . H12A H 0.6636 0.1905 0.3443 0.045 Uiso 1 1 calc R . . C13 C 0.7500 0.2500 0.35323(17) 0.0371(11) Uani 1 2 d S . . H13A H 0.7500 0.2500 0.3928 0.045 Uiso 1 2 calc SR . . C14 C 0.6388(2) 0.1790(2) 0.23656(15) 0.0491(10) Uani 1 1 d . . . H14A H 0.5936 0.2046 0.2393 0.059 Uiso 1 1 calc R . . H14B H 0.6312 0.1349 0.2537 0.059 Uiso 1 1 calc R . . C15 C 0.6897(3) 0.0809(2) 0.15346(19) 0.0608(12) Uani 1 1 d . . . F15A F 0.6408(2) 0.03877(15) 0.1702(2) 0.1175(15) Uani 1 1 d . . . F15B F 0.7041(3) 0.07090(18) 0.10236(13) 0.164(3) Uani 1 1 d . . . F15C F 0.74766(16) 0.06803(13) 0.18306(14) 0.0753(8) Uani 1 1 d . . . C16 C 0.5772(2) 0.1715(2) 0.1254(2) 0.0555(11) Uani 1 1 d . . . F16A F 0.58696(17) 0.16328(17) 0.07209(12) 0.0838(9) Uani 1 1 d . . . F16B F 0.53311(15) 0.12423(15) 0.14431(13) 0.0770(8) Uani 1 1 d . . . F16C F 0.54715(15) 0.23020(14) 0.13245(16) 0.0843(10) Uani 1 1 d . . . B1 B 0.28458(19) 0.49816(17) 0.08002(13) 0.0263(7) Uani 1 1 d . . . C19 C 0.33958(17) 0.52994(15) 0.03318(11) 0.0279(6) Uani 1 1 d . . . F20 F 0.32292(11) 0.64432(9) 0.05511(8) 0.0381(5) Uani 1 1 d . . . C20 C 0.35547(18) 0.59620(16) 0.02504(12) 0.0314(7) Uani 1 1 d . . . F21 F 0.41623(13) 0.68466(11) -0.01964(10) 0.0534(6) Uani 1 1 d . . . C21 C 0.4049(2) 0.61931(17) -0.01333(14) 0.0384(8) Uani 1 1 d . . . F22 F 0.49106(12) 0.59629(12) -0.08252(9) 0.0509(6) Uani 1 1 d . . . C22 C 0.44245(18) 0.57475(19) -0.04565(13) 0.0372(8) Uani 1 1 d . . . F23 F 0.46647(11) 0.46341(11) -0.06973(8) 0.0450(5) Uani 1 1 d . . . C23 C 0.43014(18) 0.50806(18) -0.03884(12) 0.0340(7) Uani 1 1 d . . . F24 F 0.37248(11) 0.42125(9) 0.00507(8) 0.0371(4) Uani 1 1 d . . . C24 C 0.38055(18) 0.48752(16) 0.00005(12) 0.0300(6) Uani 1 1 d . . . C25 C 0.22807(17) 0.55354(15) 0.10660(12) 0.0272(6) Uani 1 1 d . . . F26 F 0.24754(11) 0.52933(10) 0.20257(7) 0.0362(4) Uani 1 1 d . . . C26 C 0.21129(17) 0.56193(15) 0.16251(12) 0.0289(6) Uani 1 1 d . . . F27 F 0.14516(12) 0.60932(11) 0.23650(8) 0.0486(6) Uani 1 1 d . . . C27 C 0.15738(18) 0.60347(17) 0.18149(14) 0.0357(7) Uani 1 1 d . . . F28 F 0.06598(12) 0.68065(12) 0.16223(10) 0.0573(6) Uani 1 1 d . . . C28 C 0.11756(19) 0.63933(18) 0.14430(16) 0.0403(8) Uani 1 1 d . . . F29 F 0.09457(13) 0.66940(12) 0.05125(10) 0.0566(6) Uani 1 1 d . . . C29 C 0.1322(2) 0.63375(18) 0.08822(15) 0.0399(8) Uani 1 1 d . . . F30 F 0.19594(11) 0.58708(10) 0.01543(7) 0.0397(5) Uani 1 1 d . . . C30 C 0.18599(18) 0.59142(16) 0.07134(13) 0.0321(7) Uani 1 1 d . . . C31 C 0.34000(16) 0.46562(15) 0.12619(11) 0.0257(6) Uani 1 1 d . . . F32 F 0.37639(11) 0.57351(9) 0.15299(8) 0.0377(4) Uani 1 1 d . . . C32 C 0.38281(17) 0.50663(15) 0.15847(12) 0.0296(6) Uani 1 1 d . . . F33 F 0.46868(12) 0.52910(11) 0.22856(9) 0.0482(5) Uani 1 1 d . . . C33 C 0.43127(17) 0.48542(17) 0.19762(13) 0.0333(7) Uani 1 1 d . . . F34 F 0.48927(11) 0.39560(12) 0.24240(9) 0.0484(5) Uani 1 1 d . . . C34 C 0.44160(17) 0.41824(18) 0.20493(13) 0.0338(7) Uani 1 1 d . . . F35 F 0.41245(12) 0.30899(10) 0.17910(9) 0.0461(5) Uani 1 1 d . . . C35 C 0.40272(18) 0.37504(16) 0.17327(13) 0.0313(7) Uani 1 1 d . . . F36 F 0.32033(11) 0.35136(9) 0.10451(7) 0.0333(4) Uani 1 1 d . . . C36 C 0.35404(16) 0.39873(15) 0.13454(11) 0.0261(6) Uani 1 1 d . . . C37 C 0.22726(17) 0.44316(15) 0.05439(12) 0.0284(6) Uani 1 1 d . . . F38 F 0.19630(11) 0.41023(10) 0.14579(7) 0.0380(4) Uani 1 1 d . . . C38 C 0.18514(18) 0.40570(16) 0.09043(14) 0.0330(7) Uani 1 1 d . . . F39 F 0.09661(13) 0.32566(12) 0.11155(11) 0.0589(6) Uani 1 1 d . . . C39 C 0.1316(2) 0.36257(18) 0.07392(17) 0.0423(8) Uani 1 1 d . . . F40 F 0.06357(13) 0.31572(13) 0.00130(12) 0.0676(8) Uani 1 1 d . . . C40 C 0.1157(2) 0.35703(19) 0.01820(18) 0.0463(9) Uani 1 1 d . . . F41 F 0.14078(14) 0.38713(12) -0.07422(9) 0.0610(7) Uani 1 1 d . . . C41 C 0.1540(2) 0.39294(18) -0.01900(15) 0.0422(9) Uani 1 1 d . . . F42 F 0.24398(12) 0.46774(10) -0.04177(7) 0.0427(5) Uani 1 1 d . . . C42 C 0.20826(18) 0.43455(16) -0.00120(13) 0.0341(7) Uani 1 1 d . . . Cl1 Cl 0.49247(14) -0.00871(11) 0.06145(17) 0.1828(13) Uani 1 1 d . . . C43 C 0.4696(5) -0.0291(4) -0.0040(4) 0.0515(19) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03073(18) 0.02619(15) 0.01499(14) 0.000 0.000 0.00484(14) P1 0.0345(4) 0.0297(4) 0.0191(3) 0.0003(3) 0.0015(3) 0.0014(3) C1 0.037(2) 0.0223(17) 0.0150(16) 0.000 0.000 0.0069(18) C8 0.032(2) 0.036(2) 0.026(2) 0.000 0.000 0.008(2) C9 0.0417(19) 0.0329(16) 0.0206(14) -0.0003(11) -0.0033(12) 0.0060(15) O1 0.057(2) 0.063(2) 0.0192(15) 0.000 0.000 0.013(2) O2 0.0537(17) 0.0398(13) 0.0415(14) -0.0012(11) -0.0073(12) 0.0177(13) C2 0.0432(19) 0.0303(15) 0.0198(13) 0.0017(11) -0.0009(12) -0.0033(14) C3 0.049(2) 0.0337(16) 0.0208(14) -0.0015(12) -0.0051(13) -0.0027(15) C4 0.051(3) 0.0267(19) 0.0174(18) 0.000 0.000 0.003(2) C5 0.050(2) 0.0441(19) 0.0265(16) -0.0004(14) -0.0049(14) -0.0041(17) C6 0.063(3) 0.0383(18) 0.0328(18) 0.0028(14) 0.0004(17) -0.0004(18) F6A 0.093(2) 0.0426(12) 0.0400(12) 0.0116(10) -0.0109(12) 0.0115(13) F6B 0.0646(17) 0.0368(12) 0.0846(18) 0.0048(12) -0.0069(14) -0.0147(12) F6C 0.091(2) 0.0433(13) 0.0660(16) -0.0072(11) 0.0270(14) 0.0105(13) C7 0.046(2) 0.057(2) 0.040(2) -0.0007(17) 0.0057(16) 0.0012(19) F7A 0.0773(19) 0.112(2) 0.0401(13) 0.0204(14) 0.0232(12) 0.0132(17) F7B 0.0448(14) 0.0687(16) 0.0879(19) -0.0252(14) 0.0121(13) -0.0176(13) F7C 0.0369(12) 0.0541(13) 0.0573(13) -0.0146(11) -0.0001(10) 0.0123(10) Ru2 0.03261(19) 0.03764(19) 0.01676(15) 0.000 0.000 0.01263(16) C10 0.034(2) 0.0271(18) 0.0180(17) 0.000 0.000 0.0084(19) C17 0.0402(19) 0.0452(18) 0.0202(14) 0.0022(13) 0.0077(12) 0.0131(16) C18 0.051(3) 0.053(3) 0.027(2) 0.000 0.000 0.020(3) O3 0.0529(17) 0.0587(17) 0.0413(14) 0.0143(12) 0.0154(12) 0.0297(14) O4 0.082(3) 0.075(3) 0.0202(17) 0.000 0.000 0.031(2) P2 0.0411(5) 0.0425(5) 0.0275(4) -0.0068(3) -0.0063(3) 0.0045(4) C11 0.0399(18) 0.0328(16) 0.0224(14) -0.0024(11) 0.0031(12) 0.0047(14) C12 0.057(2) 0.0298(15) 0.0254(15) -0.0002(12) 0.0086(14) 0.0014(15) C13 0.063(3) 0.029(2) 0.019(2) 0.000 0.000 0.006(2) C14 0.050(2) 0.063(2) 0.0353(19) -0.0085(17) 0.0075(16) -0.017(2) C15 0.081(3) 0.047(2) 0.054(3) -0.0059(19) -0.019(2) 0.014(2) F15A 0.089(3) 0.0456(16) 0.218(5) -0.010(2) -0.034(3) -0.0129(17) F15B 0.357(8) 0.088(2) 0.0472(18) -0.0263(17) -0.020(3) 0.116(4) F15C 0.076(2) 0.0494(14) 0.101(2) 0.0194(14) -0.0232(17) 0.0108(14) C16 0.048(2) 0.054(2) 0.065(3) -0.013(2) -0.019(2) 0.003(2) F16A 0.083(2) 0.115(2) 0.0534(16) -0.0067(16) -0.0364(14) 0.0016(19) F16B 0.0533(17) 0.0743(18) 0.103(2) -0.0003(16) -0.0185(15) -0.0095(15) F16C 0.0510(16) 0.0650(17) 0.137(3) -0.0204(18) -0.0371(17) 0.0155(14) B1 0.0333(18) 0.0280(15) 0.0175(14) -0.0011(11) 0.0023(12) 0.0045(15) C19 0.0326(16) 0.0338(15) 0.0175(12) 0.0039(11) 0.0013(11) 0.0052(13) F20 0.0494(12) 0.0284(9) 0.0366(10) 0.0038(8) 0.0156(9) 0.0049(9) C20 0.0364(18) 0.0335(15) 0.0244(14) 0.0046(12) 0.0062(12) 0.0063(14) F21 0.0596(15) 0.0410(11) 0.0595(14) 0.0177(10) 0.0222(11) 0.0005(11) C21 0.042(2) 0.0393(18) 0.0340(17) 0.0141(14) 0.0063(14) 0.0042(15) F22 0.0395(12) 0.0757(15) 0.0374(11) 0.0171(11) 0.0167(9) 0.0064(11) C22 0.0310(17) 0.058(2) 0.0225(14) 0.0100(14) 0.0066(12) 0.0060(16) F23 0.0412(12) 0.0650(14) 0.0290(10) -0.0064(9) 0.0093(8) 0.0172(11) C23 0.0321(17) 0.0500(19) 0.0199(14) 0.0002(13) 0.0034(11) 0.0141(15) F24 0.0451(12) 0.0345(10) 0.0318(10) -0.0046(8) 0.0041(8) 0.0104(9) C24 0.0331(17) 0.0367(16) 0.0202(13) 0.0030(11) 0.0003(11) 0.0087(14) C25 0.0300(16) 0.0282(14) 0.0233(14) -0.0036(11) 0.0032(11) -0.0003(12) F26 0.0447(11) 0.0438(10) 0.0201(8) 0.0004(7) 0.0064(8) 0.0009(9) C26 0.0319(17) 0.0319(15) 0.0230(14) -0.0031(11) 0.0054(11) -0.0044(13) F27 0.0489(13) 0.0641(14) 0.0329(11) -0.0163(10) 0.0195(9) -0.0049(11) C27 0.0335(18) 0.0440(18) 0.0296(16) -0.0107(14) 0.0125(13) -0.0053(15) F28 0.0444(13) 0.0610(14) 0.0666(15) -0.0198(12) 0.0145(11) 0.0175(11) C28 0.0309(18) 0.0400(18) 0.050(2) -0.0148(15) 0.0112(15) 0.0043(15) F29 0.0533(14) 0.0592(14) 0.0571(14) -0.0017(11) -0.0059(11) 0.0305(12) C29 0.0360(19) 0.0402(18) 0.0437(19) -0.0060(15) -0.0010(15) 0.0086(16) F30 0.0474(12) 0.0471(11) 0.0247(9) -0.0014(8) -0.0014(8) 0.0163(10) C30 0.0370(18) 0.0355(16) 0.0238(14) -0.0045(12) 0.0030(12) 0.0052(14) C31 0.0283(15) 0.0317(14) 0.0172(12) 0.0008(11) 0.0031(10) -0.0017(12) F32 0.0458(12) 0.0292(9) 0.0380(10) 0.0001(8) -0.0046(8) -0.0065(9) C32 0.0316(17) 0.0319(15) 0.0254(14) 0.0044(12) 0.0026(12) -0.0022(13) F33 0.0453(13) 0.0549(13) 0.0443(12) -0.0004(10) -0.0139(9) -0.0177(11) C33 0.0287(17) 0.0448(18) 0.0264(15) 0.0020(13) -0.0003(12) -0.0085(14) F34 0.0382(12) 0.0666(14) 0.0406(11) 0.0172(10) -0.0149(9) -0.0010(11) C34 0.0269(16) 0.0495(19) 0.0251(14) 0.0087(13) -0.0020(11) -0.0011(15) F35 0.0534(13) 0.0385(11) 0.0463(12) 0.0113(9) -0.0103(10) 0.0094(10) C35 0.0328(17) 0.0355(16) 0.0255(14) 0.0083(12) 0.0017(12) 0.0033(14) F36 0.0428(11) 0.0288(9) 0.0284(9) -0.0026(7) -0.0052(8) 0.0016(8) C36 0.0293(16) 0.0307(14) 0.0182(12) 0.0014(11) 0.0022(11) -0.0003(12) C37 0.0287(15) 0.0305(15) 0.0259(14) -0.0046(11) -0.0027(11) 0.0085(13) F38 0.0416(12) 0.0443(11) 0.0281(9) -0.0015(8) 0.0070(8) -0.0084(9) C38 0.0313(17) 0.0354(16) 0.0323(16) -0.0058(13) 0.0001(13) 0.0029(14) F39 0.0446(14) 0.0521(13) 0.0799(17) -0.0070(12) 0.0131(12) -0.0159(11) C39 0.0309(19) 0.0397(19) 0.056(2) -0.0106(16) 0.0036(16) 0.0000(15) F40 0.0386(13) 0.0643(15) 0.100(2) -0.0346(14) -0.0192(13) -0.0031(12) C40 0.0275(18) 0.044(2) 0.068(3) -0.0219(19) -0.0129(17) 0.0063(16) F41 0.0661(16) 0.0704(15) 0.0466(13) -0.0271(12) -0.0318(11) 0.0220(13) C41 0.042(2) 0.0445(19) 0.0407(19) -0.0197(15) -0.0202(16) 0.0167(17) F42 0.0597(14) 0.0474(11) 0.0209(8) -0.0011(8) -0.0059(9) 0.0121(10) C42 0.0363(19) 0.0371(17) 0.0289(16) -0.0053(13) -0.0057(13) 0.0136(14) Cl1 0.1079(18) 0.0933(14) 0.347(4) -0.010(2) 0.025(2) 0.0146(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C9 1.971(3) 2_665 ? Ru1 C9 1.971(3) . ? Ru1 C8 2.005(4) . ? Ru1 C1 2.154(4) . ? Ru1 P1 2.3140(8) . ? Ru1 P1 2.3140(8) 2_665 ? P1 C5 1.810(3) . ? P1 C7 1.876(4) . ? P1 C6 1.880(4) . ? C1 C2 1.402(4) . ? C1 C2 1.402(4) 2_665 ? C8 O1 1.125(5) . ? C9 O2 1.117(4) . ? C2 C3 1.395(4) . ? C2 C5 1.509(5) . ? C3 C4 1.376(4) . ? C3 H3A 0.9500 . ? C4 C3 1.376(4) 2_665 ? C4 H4A 0.9500 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 F6A 1.307(4) . ? C6 F6B 1.310(5) . ? C6 F6C 1.339(5) . ? C7 F7C 1.311(5) . ? C7 F7A 1.318(5) . ? C7 F7B 1.344(5) . ? Ru2 C17 1.974(3) . ? Ru2 C17 1.974(3) 2_655 ? Ru2 C18 2.002(5) . ? Ru2 C10 2.151(4) . ? Ru2 P2 2.3099(10) . ? Ru2 P2 2.3099(10) 2_655 ? C10 C11 1.399(4) . ? C10 C11 1.400(4) 2_655 ? C17 O3 1.115(4) . ? C18 O4 1.127(6) . ? P2 C14 1.809(4) . ? P2 C15 1.868(4) . ? P2 C16 1.877(4) . ? C11 C12 1.395(4) . ? C11 C14 1.499(5) . ? C12 C13 1.375(4) . ? C12 H12A 0.9500 . ? C13 C12 1.375(4) 2_655 ? C13 H13A 0.9500 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 F15B 1.271(6) . ? C15 F15A 1.308(6) . ? C15 F15C 1.320(5) . ? C16 F16A 1.303(5) . ? C16 F16C 1.319(5) . ? C16 F16B 1.336(5) . ? B1 C31 1.651(4) . ? B1 C19 1.651(4) . ? B1 C37 1.658(5) . ? B1 C25 1.662(4) . ? C19 C20 1.381(4) . ? C19 C24 1.395(4) . ? F20 C20 1.352(4) . ? C20 C21 1.384(4) . ? F21 C21 1.341(4) . ? C21 C22 1.377(5) . ? F22 C22 1.339(4) . ? C22 C23 1.372(5) . ? F23 C23 1.348(4) . ? C23 C24 1.377(4) . ? F24 C24 1.348(4) . ? C25 C30 1.383(4) . ? C25 C26 1.387(4) . ? F26 C26 1.346(4) . ? C26 C27 1.385(4) . ? F27 C27 1.344(4) . ? C27 C28 1.367(5) . ? F28 C28 1.343(4) . ? C28 C29 1.377(5) . ? F29 C29 1.340(4) . ? C29 C30 1.377(5) . ? F30 C30 1.357(3) . ? C31 C32 1.385(4) . ? C31 C36 1.386(4) . ? F32 C32 1.358(4) . ? C32 C33 1.372(4) . ? F33 C33 1.346(4) . ? C33 C34 1.377(5) . ? F34 C34 1.344(4) . ? C34 C35 1.364(5) . ? F35 C35 1.349(4) . ? C35 C36 1.384(4) . ? F36 C36 1.351(3) . ? C37 C42 1.391(4) . ? C37 C38 1.391(5) . ? F38 C38 1.347(4) . ? C38 C39 1.382(5) . ? F39 C39 1.339(4) . ? C39 C40 1.374(6) . ? F40 C40 1.342(4) . ? C40 C41 1.353(6) . ? F41 C41 1.352(4) . ? C41 C42 1.382(5) . ? F42 C42 1.356(4) . ? Cl1 C43 1.679(9) . ? Cl1 C43 1.726(9) 5_655 ? C43 C43 1.643(18) 5_655 ? C43 Cl1 1.726(9) 5_655 ? 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 C9 Ru1 C9 177.12(17) 2_665 . ? C9 Ru1 C8 91.44(8) 2_665 . ? C9 Ru1 C8 91.44(8) . . ? C9 Ru1 C1 88.56(8) 2_665 . ? C9 Ru1 C1 88.56(8) . . ? C8 Ru1 C1 180.000(1) . . ? C9 Ru1 P1 88.92(10) 2_665 . ? C9 Ru1 P1 90.54(10) . . ? C8 Ru1 P1 100.87(2) . . ? C1 Ru1 P1 79.13(2) . . ? C9 Ru1 P1 90.54(10) 2_665 2_665 ? C9 Ru1 P1 88.92(10) . 2_665 ? C8 Ru1 P1 100.87(2) . 2_665 ? C1 Ru1 P1 79.13(2) . 2_665 ? P1 Ru1 P1 158.26(4) . 2_665 ? C5 P1 C7 104.23(18) . . ? C5 P1 C6 106.43(17) . . ? C7 P1 C6 99.53(19) . . ? C5 P1 Ru1 107.06(12) . . ? C7 P1 Ru1 121.05(13) . . ? C6 P1 Ru1 117.11(14) . . ? C2 C1 C2 117.6(4) . 2_665 ? C2 C1 Ru1 121.20(18) . . ? C2 C1 Ru1 121.20(18) 2_665 . ? O1 C8 Ru1 180.000(1) . . ? O2 C9 Ru1 178.5(3) . . ? C3 C2 C1 120.8(3) . . ? C3 C2 C5 118.7(3) . . ? C1 C2 C5 120.4(3) . . ? C4 C3 C2 120.6(3) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C3 119.7(4) . 2_665 ? C3 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 2_665 . ? C2 C5 P1 107.4(2) . . ? C2 C5 H5A 110.2 . . ? P1 C5 H5A 110.2 . . ? C2 C5 H5B 110.2 . . ? P1 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? F6A C6 F6B 109.1(3) . . ? F6A C6 F6C 107.1(3) . . ? F6B C6 F6C 109.3(3) . . ? F6A C6 P1 110.3(3) . . ? F6B C6 P1 113.5(3) . . ? F6C C6 P1 107.3(2) . . ? F7C C7 F7A 108.6(3) . . ? F7C C7 F7B 106.5(3) . . ? F7A C7 F7B 110.0(4) . . ? F7C C7 P1 109.9(3) . . ? F7A C7 P1 110.8(3) . . ? F7B C7 P1 111.0(3) . . ? C17 Ru2 C17 175.53(17) . 2_655 ? C17 Ru2 C18 92.23(9) . . ? C17 Ru2 C18 92.24(9) 2_655 . ? C17 Ru2 C10 87.77(9) . . ? C17 Ru2 C10 87.76(9) 2_655 . ? C18 Ru2 C10 180.0 . . ? C17 Ru2 P2 91.47(11) . . ? C17 Ru2 P2 87.71(11) 2_655 . ? C18 Ru2 P2 100.55(2) . . ? C10 Ru2 P2 79.45(2) . . ? C17 Ru2 P2 87.71(11) . 2_655 ? C17 Ru2 P2 91.47(11) 2_655 2_655 ? C18 Ru2 P2 100.55(2) . 2_655 ? C10 Ru2 P2 79.45(2) . 2_655 ? P2 Ru2 P2 158.90(4) . 2_655 ? C11 C10 C11 118.2(4) . 2_655 ? C11 C10 Ru2 120.91(18) . . ? C11 C10 Ru2 120.91(18) 2_655 . ? O3 C17 Ru2 179.1(3) . . ? O4 C18 Ru2 180.0 . . ? C14 P2 C15 107.4(2) . . ? C14 P2 C16 104.1(2) . . ? C15 P2 C16 99.6(2) . . ? C14 P2 Ru2 106.64(13) . . ? C15 P2 Ru2 118.06(18) . . ? C16 P2 Ru2 119.76(16) . . ? C12 C11 C10 120.4(3) . . ? C12 C11 C14 118.9(3) . . ? C10 C11 C14 120.7(3) . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C12 C13 C12 119.6(4) . 2_655 ? C12 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 2_655 . ? C11 C14 P2 108.1(2) . . ? C11 C14 H14A 110.1 . . ? P2 C14 H14A 110.1 . . ? C11 C14 H14B 110.1 . . ? P2 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? F15B C15 F15A 109.9(5) . . ? F15B C15 F15C 108.3(5) . . ? F15A C15 F15C 106.2(4) . . ? F15B C15 P2 109.8(3) . . ? F15A C15 P2 113.7(4) . . ? F15C C15 P2 108.7(3) . . ? F16A C16 F16C 107.3(4) . . ? F16A C16 F16B 109.2(4) . . ? F16C C16 F16B 109.5(4) . . ? F16A C16 P2 111.3(3) . . ? F16C C16 P2 108.8(3) . . ? F16B C16 P2 110.7(3) . . ? C31 B1 C19 102.8(2) . . ? C31 B1 C37 112.8(2) . . ? C19 B1 C37 114.1(2) . . ? C31 B1 C25 114.0(2) . . ? C19 B1 C25 113.3(2) . . ? C37 B1 C25 100.4(2) . . ? C20 C19 C24 113.2(3) . . ? C20 C19 B1 127.2(3) . . ? C24 C19 B1 119.4(3) . . ? F20 C20 C19 121.4(3) . . ? F20 C20 C21 114.4(3) . . ? C19 C20 C21 124.2(3) . . ? F21 C21 C22 119.7(3) . . ? F21 C21 C20 120.7(3) . . ? C22 C21 C20 119.6(3) . . ? F22 C22 C23 120.6(3) . . ? F22 C22 C21 120.4(3) . . ? C23 C22 C21 119.0(3) . . ? F23 C23 C22 120.2(3) . . ? F23 C23 C24 120.7(3) . . ? C22 C23 C24 119.1(3) . . ? F24 C24 C23 115.6(3) . . ? F24 C24 C19 119.6(3) . . ? C23 C24 C19 124.8(3) . . ? C30 C25 C26 113.3(3) . . ? C30 C25 B1 119.7(2) . . ? C26 C25 B1 126.6(3) . . ? F26 C26 C27 115.1(3) . . ? F26 C26 C25 121.1(3) . . ? C27 C26 C25 123.7(3) . . ? F27 C27 C28 120.1(3) . . ? F27 C27 C26 119.9(3) . . ? C28 C27 C26 119.9(3) . . ? F28 C28 C27 120.5(3) . . ? F28 C28 C29 120.4(3) . . ? C27 C28 C29 119.1(3) . . ? F29 C29 C28 119.9(3) . . ? F29 C29 C30 121.3(3) . . ? C28 C29 C30 118.8(3) . . ? F30 C30 C29 115.5(3) . . ? F30 C30 C25 119.4(3) . . ? C29 C30 C25 125.1(3) . . ? C32 C31 C36 112.9(3) . . ? C32 C31 B1 120.0(3) . . ? C36 C31 B1 126.9(3) . . ? F32 C32 C33 115.7(3) . . ? F32 C32 C31 119.1(3) . . ? C33 C32 C31 125.3(3) . . ? F33 C33 C32 121.1(3) . . ? F33 C33 C34 119.9(3) . . ? C32 C33 C34 119.0(3) . . ? F34 C34 C35 120.5(3) . . ? F34 C34 C33 120.7(3) . . ? C35 C34 C33 118.7(3) . . ? F35 C35 C34 119.9(3) . . ? F35 C35 C36 119.8(3) . . ? C34 C35 C36 120.2(3) . . ? F36 C36 C35 114.9(3) . . ? F36 C36 C31 121.4(3) . . ? C35 C36 C31 123.8(3) . . ? C42 C37 C38 112.6(3) . . ? C42 C37 B1 127.1(3) . . ? C38 C37 B1 119.8(3) . . ? F38 C38 C39 115.9(3) . . ? F38 C38 C37 119.3(3) . . ? C39 C38 C37 124.8(3) . . ? F39 C39 C40 120.4(3) . . ? F39 C39 C38 120.5(3) . . ? C40 C39 C38 119.1(4) . . ? F40 C40 C41 121.0(4) . . ? F40 C40 C39 120.1(4) . . ? C41 C40 C39 118.9(3) . . ? F41 C41 C40 120.2(3) . . ? F41 C41 C42 119.3(4) . . ? C40 C41 C42 120.5(3) . . ? F42 C42 C41 115.9(3) . . ? F42 C42 C37 120.1(3) . . ? C41 C42 C37 124.0(3) . . ? C43 Cl1 C43 57.7(6) . 5_655 ? C43 C43 Cl1 62.6(5) 5_655 . ? C43 C43 Cl1 59.7(5) 5_655 5_655 ? Cl1 C43 Cl1 122.3(6) . 5_655 ? 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 C1 C2 C5 P1 -19.2(4) . . . . ? C10 C11 C14 P2 16.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.301 _refine_diff_density_min -0.914 _refine_diff_density_rms 0.095 #----------------------------------------------------------------------------- data_jja42 _database_code_depnum_ccdc_archive 'CCDC 886424' #TrackingRef '- Combined.cif' #Compound 11: cis (CF3PCP)Ru(CO)2(\^I -Cl)(\^I -Ag)CO(CH3)2+SbF6- #----------------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H13 Ag Cl F18 O3 P2 Ru Sb' _chemical_formula_sum 'C17 H13 Ag Cl F18 O3 P2 Ru Sb' _chemical_formula_weight 1035.35 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' Ag Ag -0.8971 1.1015 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9732(5) _cell_length_b 11.1878(9) _cell_length_c 18.8885(14) _cell_angle_alpha 91.529(4) _cell_angle_beta 97.851(4) _cell_angle_gamma 104.386(4) _cell_volume 1411.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9902 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 33.90 _exptl_crystal_description rectangular_plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 2.515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4343 _exptl_absorpt_correction_T_max 0.8516 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30112 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 32.58 _reflns_number_total 10170 _reflns_number_gt 8942 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V. 6.10 (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL V. 6.10 (Bruker, 2001)' _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^)+(0.0285P)^2^+2.5553P] 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 10170 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Ru1 Ru 0.30337(2) 0.154947(16) 0.147392(9) 0.01591(4) Uani 1 1 d . . . P1 P 0.33111(9) 0.36414(5) 0.14527(3) 0.01982(10) Uani 1 1 d . . . P2 P 0.25152(9) -0.04121(5) 0.18802(3) 0.01984(11) Uani 1 1 d . . . C1 C 0.2126(3) 0.1879(2) 0.24761(12) 0.0188(4) Uani 1 1 d . . . C13 C 0.0355(4) 0.1157(2) 0.10305(13) 0.0238(4) Uani 1 1 d . . . C14 C 0.4042(3) 0.1333(2) 0.05522(13) 0.0222(4) Uani 1 1 d . . . Cl1 Cl 0.65427(8) 0.20654(6) 0.20384(3) 0.02357(10) Uani 1 1 d . . . Ag1 Ag 0.73897(4) 0.23211(2) 0.333991(12) 0.04123(6) Uani 1 1 d . . . O3 O 0.6359(4) 0.1601(2) 0.43516(13) 0.0464(6) Uani 1 1 d . . . O1 O -0.1256(3) 0.0897(2) 0.07527(12) 0.0364(4) Uani 1 1 d . . . O2 O 0.4597(3) 0.1269(2) 0.00265(11) 0.0355(4) Uani 1 1 d . . . C2 C 0.2275(3) 0.3093(2) 0.27495(12) 0.0221(4) Uani 1 1 d . . . C3 C 0.1722(4) 0.3303(3) 0.34174(14) 0.0269(5) Uani 1 1 d . . . H3 H 0.194(6) 0.412(4) 0.360(2) 0.036(9) Uiso 1 1 d . . . C4 C 0.1034(4) 0.2314(3) 0.38269(14) 0.0296(5) Uani 1 1 d . . . H4 H 0.071(6) 0.242(4) 0.428(2) 0.037(10) Uiso 1 1 d . . . C5 C 0.0852(4) 0.1110(3) 0.35645(14) 0.0278(5) Uani 1 1 d . . . H5 H 0.033(6) 0.046(4) 0.379(2) 0.048(11) Uiso 1 1 d . . . C6 C 0.1386(3) 0.0891(2) 0.28969(13) 0.0214(4) Uani 1 1 d . . . C7 C 0.1102(4) -0.0434(2) 0.26219(15) 0.0258(5) Uani 1 1 d . . . H7A H -0.027(6) -0.077(3) 0.243(2) 0.034(9) Uiso 1 1 d . . . H7B H 0.141(5) -0.097(4) 0.295(2) 0.034(9) Uiso 1 1 d . . . C8 C 0.4670(4) -0.1075(3) 0.22344(17) 0.0319(6) Uani 1 1 d . . . F8A F 0.5981(3) -0.09764(19) 0.17784(12) 0.0448(5) Uani 1 1 d . . . F8B F 0.4039(3) -0.22598(18) 0.23594(15) 0.0524(6) Uani 1 1 d . . . F8C F 0.5615(3) -0.0472(2) 0.28521(11) 0.0452(5) Uani 1 1 d . . . C9 C 0.1032(4) -0.1770(2) 0.12592(16) 0.0293(5) Uani 1 1 d . . . F9A F -0.0536(3) -0.14801(19) 0.08842(14) 0.0531(6) Uani 1 1 d . . . F9B F 0.0329(3) -0.27734(16) 0.15900(11) 0.0425(4) Uani 1 1 d . . . F9C F 0.2146(3) -0.20525(18) 0.07957(11) 0.0436(5) Uani 1 1 d . . . C10 C 0.3055(5) 0.4199(3) 0.23354(15) 0.0313(5) Uani 1 1 d . . . H10A H 0.215(7) 0.473(4) 0.230(2) 0.056(12) Uiso 1 1 d . . . H10B H 0.439(7) 0.470(4) 0.254(3) 0.059(13) Uiso 1 1 d . . . C11 C 0.5601(4) 0.4724(2) 0.11850(15) 0.0282(5) Uani 1 1 d . . . F11A F 0.7203(3) 0.47909(17) 0.16632(10) 0.0363(4) Uani 1 1 d . . . F11B F 0.5934(3) 0.42851(19) 0.05611(10) 0.0376(4) Uani 1 1 d . . . F11C F 0.5383(3) 0.58614(17) 0.11023(13) 0.0484(5) Uani 1 1 d . . . C12 C 0.1346(4) 0.4102(2) 0.08123(16) 0.0288(5) Uani 1 1 d . . . F12A F -0.0455(3) 0.3496(2) 0.09415(13) 0.0468(5) Uani 1 1 d . . . F12B F 0.1498(3) 0.3786(2) 0.01447(10) 0.0415(4) Uani 1 1 d . . . F12C F 0.1430(4) 0.52945(18) 0.08549(14) 0.0564(6) Uani 1 1 d . . . C15 C 0.5900(5) 0.2183(3) 0.48314(16) 0.0353(6) Uani 1 1 d . . . C16 C 0.5911(6) 0.3498(3) 0.4793(2) 0.0422(7) Uani 1 1 d . . . H16A H 0.712(8) 0.394(5) 0.509(3) 0.074(16) Uiso 1 1 d . . . H16B H 0.474(8) 0.367(5) 0.495(3) 0.065(14) Uiso 1 1 d . . . H16C H 0.581(8) 0.365(5) 0.432(3) 0.072(15) Uiso 1 1 d . . . C17 C 0.5310(9) 0.1560(4) 0.5485(2) 0.0631(13) Uani 1 1 d . . . H17A H 0.3848 0.1278 0.5434 0.095 Uiso 1 1 calc R . . H17B H 0.5807 0.2144 0.5904 0.095 Uiso 1 1 calc R . . H17C H 0.5888 0.0849 0.5546 0.095 Uiso 1 1 calc R . . Sb1 Sb 0.14839(3) 0.357833(18) 0.640117(10) 0.03236(5) Uani 1 1 d . . . F1 F 0.0946(5) 0.1919(2) 0.60789(15) 0.0701(8) Uani 1 1 d . . . F2 F -0.1092(4) 0.3348(3) 0.6626(2) 0.0847(10) Uani 1 1 d . . . F3 F 0.2033(4) 0.52563(19) 0.67179(13) 0.0514(5) Uani 1 1 d . . . F4 F 0.4135(3) 0.3898(2) 0.62291(13) 0.0536(6) Uani 1 1 d . . . F5 F 0.0703(5) 0.3949(3) 0.54706(14) 0.0836(10) Uani 1 1 d . . . F6 F 0.2321(4) 0.3156(2) 0.73174(11) 0.0502(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01586(7) 0.01615(8) 0.01697(7) 0.00166(5) 0.00364(5) 0.00569(5) P1 0.0231(3) 0.0171(3) 0.0211(3) 0.00303(19) 0.0045(2) 0.0077(2) P2 0.0191(2) 0.0167(2) 0.0254(3) 0.0034(2) 0.0071(2) 0.00545(19) C1 0.0166(8) 0.0222(10) 0.0180(9) 0.0010(7) 0.0027(7) 0.0060(7) C13 0.0245(10) 0.0239(11) 0.0249(11) -0.0005(8) 0.0037(8) 0.0099(8) C14 0.0200(9) 0.0222(11) 0.0255(10) 0.0003(8) 0.0046(8) 0.0070(8) Cl1 0.0177(2) 0.0292(3) 0.0234(2) 0.0043(2) 0.00308(18) 0.00494(19) Ag1 0.06171(16) 0.04102(13) 0.02387(10) 0.00394(8) 0.01060(10) 0.01600(11) O3 0.0659(16) 0.0420(13) 0.0331(11) 0.0057(9) 0.0207(11) 0.0096(11) O1 0.0235(9) 0.0399(12) 0.0431(12) -0.0034(9) -0.0048(8) 0.0091(8) O2 0.0354(10) 0.0453(12) 0.0280(9) -0.0025(8) 0.0123(8) 0.0105(9) C2 0.0226(10) 0.0239(11) 0.0205(10) -0.0006(8) 0.0045(8) 0.0070(8) C3 0.0285(11) 0.0295(13) 0.0229(11) -0.0056(9) 0.0046(9) 0.0080(9) C4 0.0278(11) 0.0407(15) 0.0207(11) -0.0019(10) 0.0080(9) 0.0072(10) C5 0.0279(11) 0.0330(13) 0.0228(11) 0.0038(9) 0.0094(9) 0.0050(10) C6 0.0188(9) 0.0242(11) 0.0220(10) 0.0021(8) 0.0056(8) 0.0053(8) C7 0.0275(11) 0.0215(11) 0.0295(12) 0.0037(9) 0.0134(9) 0.0032(9) C8 0.0248(11) 0.0280(13) 0.0465(16) 0.0137(11) 0.0078(11) 0.0107(9) F8A 0.0306(8) 0.0478(11) 0.0667(13) 0.0158(10) 0.0208(9) 0.0216(8) F8B 0.0416(10) 0.0284(9) 0.0934(17) 0.0277(10) 0.0142(11) 0.0156(8) F8C 0.0391(10) 0.0489(11) 0.0462(11) 0.0184(9) -0.0049(8) 0.0129(8) C9 0.0326(12) 0.0203(11) 0.0351(13) -0.0014(9) 0.0106(10) 0.0043(9) F9A 0.0422(10) 0.0344(10) 0.0726(15) -0.0153(10) -0.0191(10) 0.0074(8) F9B 0.0537(11) 0.0217(8) 0.0480(11) -0.0001(7) 0.0237(9) -0.0064(7) F9C 0.0536(11) 0.0352(10) 0.0416(10) -0.0083(8) 0.0263(9) 0.0016(8) C10 0.0468(15) 0.0210(12) 0.0270(12) -0.0007(9) 0.0109(11) 0.0076(11) C11 0.0278(11) 0.0229(11) 0.0349(13) 0.0084(9) 0.0061(10) 0.0068(9) F11A 0.0287(8) 0.0318(9) 0.0424(10) 0.0031(7) -0.0009(7) 0.0001(6) F11B 0.0340(8) 0.0481(11) 0.0328(9) 0.0089(8) 0.0135(7) 0.0086(7) F11C 0.0476(11) 0.0234(9) 0.0789(15) 0.0203(9) 0.0198(10) 0.0106(8) C12 0.0273(11) 0.0211(11) 0.0395(14) 0.0063(10) 0.0016(10) 0.0102(9) F12A 0.0255(8) 0.0507(12) 0.0734(14) 0.0230(10) 0.0145(8) 0.0208(8) F12B 0.0401(9) 0.0532(12) 0.0295(9) 0.0077(8) -0.0039(7) 0.0129(8) F12C 0.0592(13) 0.0238(9) 0.0839(17) 0.0021(9) -0.0197(11) 0.0226(9) C15 0.0393(14) 0.0367(15) 0.0269(12) 0.0033(11) 0.0081(11) 0.0024(12) C16 0.0488(18) 0.0390(17) 0.0396(17) 0.0088(13) 0.0122(14) 0.0089(14) C17 0.114(4) 0.0364(18) 0.0416(19) 0.0086(15) 0.040(2) 0.009(2) Sb1 0.03216(9) 0.02985(10) 0.03192(9) 0.00725(7) 0.00596(7) 0.00082(7) F1 0.098(2) 0.0321(11) 0.0659(16) -0.0057(10) 0.0229(14) -0.0153(12) F2 0.0334(11) 0.097(2) 0.129(3) 0.038(2) 0.0259(14) 0.0156(13) F3 0.0689(14) 0.0325(10) 0.0582(13) 0.0067(9) 0.0155(11) 0.0195(10) F4 0.0460(11) 0.0503(13) 0.0657(14) -0.0026(10) 0.0287(10) 0.0038(9) F5 0.098(2) 0.0746(19) 0.0486(14) 0.0234(13) -0.0268(14) -0.0155(16) F6 0.0671(14) 0.0517(12) 0.0380(10) 0.0169(9) 0.0099(9) 0.0243(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C13 1.878(2) . ? Ru1 C14 1.995(2) . ? Ru1 C1 2.127(2) . ? Ru1 P1 2.3019(6) . ? Ru1 P2 2.3037(6) . ? Ru1 Cl1 2.4515(6) . ? P1 C10 1.812(3) . ? P1 C12 1.881(3) . ? P1 C11 1.888(3) . ? P2 C7 1.817(2) . ? P2 C9 1.883(3) . ? P2 C8 1.887(3) . ? C1 C6 1.413(3) . ? C1 C2 1.415(3) . ? C13 O1 1.136(3) . ? C14 O2 1.121(3) . ? Cl1 Ag1 2.4406(6) . ? Ag1 O3 2.233(2) . ? Ag1 C4 2.584(3) 1_655 ? O3 C15 1.224(4) . ? C2 C3 1.399(3) . ? C2 C10 1.507(4) . ? C3 C4 1.391(4) . ? C3 H3 0.93(4) . ? C4 C5 1.392(4) . ? C4 Ag1 2.584(3) 1_455 ? C4 H4 0.93(4) . ? C5 C6 1.395(3) . ? C5 H5 0.88(4) . ? C6 C7 1.514(4) . ? C7 H7A 0.95(4) . ? C7 H7B 0.91(4) . ? C8 F8A 1.326(3) . ? C8 F8B 1.327(3) . ? C8 F8C 1.333(4) . ? C9 F9B 1.319(3) . ? C9 F9C 1.328(3) . ? C9 F9A 1.334(4) . ? C10 H10A 0.97(5) . ? C10 H10B 0.98(5) . ? C11 F11A 1.322(3) . ? C11 F11C 1.330(3) . ? C11 F11B 1.336(3) . ? C12 F12C 1.321(3) . ? C12 F12B 1.326(4) . ? C12 F12A 1.329(3) . ? C15 C16 1.473(5) . ? C15 C17 1.490(4) . ? C16 H16A 0.96(6) . ? C16 H16B 0.97(5) . ? C16 H16C 0.92(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? Sb1 F5 1.857(2) . ? Sb1 F2 1.859(2) . ? Sb1 F6 1.861(2) . ? Sb1 F1 1.868(2) . ? Sb1 F4 1.869(2) . ? Sb1 F3 1.884(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Ru1 C14 92.65(10) . . ? C13 Ru1 C1 90.32(9) . . ? C14 Ru1 C1 176.25(9) . . ? C13 Ru1 P1 92.45(8) . . ? C14 Ru1 P1 97.51(7) . . ? C1 Ru1 P1 80.07(6) . . ? C13 Ru1 P2 89.30(8) . . ? C14 Ru1 P2 101.97(7) . . ? C1 Ru1 P2 80.33(6) . . ? P1 Ru1 P2 160.34(2) . . ? C13 Ru1 Cl1 179.30(8) . . ? C14 Ru1 Cl1 86.68(7) . . ? C1 Ru1 Cl1 90.34(6) . . ? P1 Ru1 Cl1 87.46(2) . . ? P2 Ru1 Cl1 91.02(2) . . ? C10 P1 C12 105.94(14) . . ? C10 P1 C11 106.80(14) . . ? C12 P1 C11 98.58(12) . . ? C10 P1 Ru1 107.92(9) . . ? C12 P1 Ru1 115.47(9) . . ? C11 P1 Ru1 120.90(9) . . ? C7 P2 C9 104.70(12) . . ? C7 P2 C8 104.64(13) . . ? C9 P2 C8 98.02(13) . . ? C7 P2 Ru1 106.68(9) . . ? C9 P2 Ru1 119.26(9) . . ? C8 P2 Ru1 121.64(9) . . ? C6 C1 C2 117.8(2) . . ? C6 C1 Ru1 120.97(17) . . ? C2 C1 Ru1 121.26(16) . . ? O1 C13 Ru1 178.4(2) . . ? O2 C14 Ru1 176.5(2) . . ? Ag1 Cl1 Ru1 120.30(2) . . ? O3 Ag1 Cl1 142.74(7) . . ? O3 Ag1 C4 91.07(10) . 1_655 ? Cl1 Ag1 C4 114.81(6) . 1_655 ? C15 O3 Ag1 127.1(2) . . ? C3 C2 C1 120.8(2) . . ? C3 C2 C10 118.1(2) . . ? C1 C2 C10 121.1(2) . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3 121(2) . . ? C2 C3 H3 119(2) . . ? C3 C4 C5 119.9(2) . . ? C3 C4 Ag1 89.71(17) . 1_455 ? C5 C4 Ag1 94.83(17) . 1_455 ? C3 C4 H4 122(2) . . ? C5 C4 H4 118(2) . . ? Ag1 C4 H4 87(2) 1_455 . ? C4 C5 C6 120.3(2) . . ? C4 C5 H5 123(3) . . ? C6 C5 H5 117(3) . . ? C5 C6 C1 120.9(2) . . ? C5 C6 C7 118.6(2) . . ? C1 C6 C7 120.5(2) . . ? C6 C7 P2 107.72(16) . . ? C6 C7 H7A 109(2) . . ? P2 C7 H7A 107(2) . . ? C6 C7 H7B 117(2) . . ? P2 C7 H7B 111(2) . . ? H7A C7 H7B 105(3) . . ? F8A C8 F8B 108.3(2) . . ? F8A C8 F8C 108.3(2) . . ? F8B C8 F8C 107.5(2) . . ? F8A C8 P2 111.5(2) . . ? F8B C8 P2 111.41(19) . . ? F8C C8 P2 109.8(2) . . ? F9B C9 F9C 108.0(2) . . ? F9B C9 F9A 107.1(2) . . ? F9C C9 F9A 107.6(3) . . ? F9B C9 P2 113.9(2) . . ? F9C C9 P2 110.37(19) . . ? F9A C9 P2 109.67(18) . . ? C2 C10 P1 108.03(18) . . ? C2 C10 H10A 111(3) . . ? P1 C10 H10A 110(3) . . ? C2 C10 H10B 114(3) . . ? P1 C10 H10B 106(3) . . ? H10A C10 H10B 108(4) . . ? F11A C11 F11C 108.4(2) . . ? F11A C11 F11B 108.0(2) . . ? F11C C11 F11B 108.0(2) . . ? F11A C11 P1 111.23(18) . . ? F11C C11 P1 112.58(18) . . ? F11B C11 P1 108.55(19) . . ? F12C C12 F12B 108.0(2) . . ? F12C C12 F12A 107.5(2) . . ? F12B C12 F12A 107.6(2) . . ? F12C C12 P1 114.3(2) . . ? F12B C12 P1 109.96(18) . . ? F12A C12 P1 109.12(18) . . ? O3 C15 C16 122.4(3) . . ? O3 C15 C17 119.8(3) . . ? C16 C15 C17 117.8(3) . . ? C15 C16 H16A 105(3) . . ? C15 C16 H16B 112(3) . . ? H16A C16 H16B 111(4) . . ? C15 C16 H16C 106(3) . . ? H16A C16 H16C 116(5) . . ? H16B C16 H16C 105(4) . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? F5 Sb1 F2 92.38(16) . . ? F5 Sb1 F6 177.43(14) . . ? F2 Sb1 F6 89.27(13) . . ? F5 Sb1 F1 88.73(14) . . ? F2 Sb1 F1 91.13(15) . . ? F6 Sb1 F1 89.27(12) . . ? F5 Sb1 F4 89.81(14) . . ? F2 Sb1 F4 175.87(14) . . ? F6 Sb1 F4 88.66(11) . . ? F1 Sb1 F4 92.40(12) . . ? F5 Sb1 F3 90.81(13) . . ? F2 Sb1 F3 89.15(14) . . ? F6 Sb1 F3 91.18(10) . . ? F1 Sb1 F3 179.47(11) . . ? F4 Sb1 F3 87.33(10) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 32.58 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 3.436 _refine_diff_density_min -2.882 _refine_diff_density_rms 0.114 #----------------------------------------------------------------------------- data_jja22 _database_code_depnum_ccdc_archive 'CCDC 886425' #TrackingRef '- Combined.cif' #Compound 12: cis (CF3PCP)Ru(CO)2(OH2)+SbF6- #----------------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H9 F12 O3 P2 Ru, F6 Sb' _chemical_formula_sum 'C14 H9 F18 O3 P2 Ru Sb' _chemical_formula_weight 851.97 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' 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 P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 9.9476(3) _cell_length_b 18.9614(5) _cell_length_c 13.3993(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.113(1) _cell_angle_gamma 90.00 _cell_volume 2502.09(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9700 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 36.46 _exptl_crystal_description rectangular_prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.962 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4763 _exptl_absorpt_correction_T_max 0.5981 _exptl_absorpt_process_details 'SADABS, (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73168 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 35.63 _reflns_number_total 11515 _reflns_number_gt 10236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V. 6.10 (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL V. 6.10 (Bruker, 2001)' _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^)+(0.0227P)^2^+3.1968P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11515 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.724419(13) 0.403372(7) 0.791783(10) 0.02100(3) Uani 1 1 d . . . C1 C 0.66909(17) 0.42266(9) 0.63495(13) 0.0227(3) Uani 1 1 d . . . P1 P 0.54875(5) 0.32501(3) 0.75392(4) 0.02881(9) Uani 1 1 d . . . P2 P 0.88406(5) 0.48799(2) 0.76605(3) 0.02250(8) Uani 1 1 d . . . C13 C 0.7789(2) 0.37943(11) 0.93807(15) 0.0292(3) Uani 1 1 d . . . C14 C 0.6016(2) 0.47140(12) 0.82250(16) 0.0316(4) Uani 1 1 d . . . O1W O 0.86423(16) 0.32666(9) 0.74879(12) 0.0313(3) Uani 1 1 d . . . H1A H 0.916(5) 0.298(2) 0.786(4) 0.088(15) Uiso 1 1 d . . . H1B H 0.870(3) 0.3172(18) 0.700(3) 0.041(9) Uiso 1 1 d . . . O1 O 0.8012(2) 0.36765(11) 1.02057(13) 0.0458(4) Uani 1 1 d . . . O2 O 0.5255(2) 0.51257(10) 0.84035(16) 0.0476(4) Uani 1 1 d . . . C2 C 0.75496(17) 0.46081(9) 0.57964(13) 0.0223(3) Uani 1 1 d . . . C3 C 0.7229(2) 0.46894(10) 0.47565(14) 0.0271(3) Uani 1 1 d . . . H3 H 0.783(3) 0.4934(15) 0.442(2) 0.034(7) Uiso 1 1 d . . . C4 C 0.6058(2) 0.43896(11) 0.42468(15) 0.0306(4) Uani 1 1 d . . . H4 H 0.586(3) 0.4416(16) 0.358(2) 0.037(7) Uiso 1 1 d . . . C5 C 0.5190(2) 0.40173(11) 0.47750(16) 0.0307(4) Uani 1 1 d . . . H5 H 0.440(3) 0.3816(17) 0.443(2) 0.043(8) Uiso 1 1 d . . . C6 C 0.54894(18) 0.39412(10) 0.58148(14) 0.0261(3) Uani 1 1 d . . . C7 C 0.4505(2) 0.35499(13) 0.63768(18) 0.0345(4) Uani 1 1 d . . . H7A H 0.386(3) 0.3861(15) 0.661(2) 0.031(7) Uiso 1 1 d . . . H7B H 0.406(3) 0.3165(18) 0.604(3) 0.048(9) Uiso 1 1 d . . . C8 C 0.4233(2) 0.30969(16) 0.8445(2) 0.0434(5) Uani 1 1 d . . . F8A F 0.39181(18) 0.37175(11) 0.88158(16) 0.0610(5) Uani 1 1 d . . . F8B F 0.30972(17) 0.28029(13) 0.80224(16) 0.0650(6) Uani 1 1 d . . . F8C F 0.47859(19) 0.26998(12) 0.92164(14) 0.0608(5) Uani 1 1 d . . . C9 C 0.5958(3) 0.23157(13) 0.7279(2) 0.0437(5) Uani 1 1 d . . . F9A F 0.65288(19) 0.23047(9) 0.64354(14) 0.0527(4) Uani 1 1 d . . . F9B F 0.6826(2) 0.20528(9) 0.80284(16) 0.0584(5) Uani 1 1 d . . . F9C F 0.4874(2) 0.18956(10) 0.7137(2) 0.0725(6) Uani 1 1 d . . . C10 C 0.88654(19) 0.49204(11) 0.63131(14) 0.0266(3) Uani 1 1 d . . . H10A H 0.902(3) 0.5401(16) 0.617(2) 0.033(7) Uiso 1 1 d . . . H10B H 0.960(3) 0.4652(15) 0.617(2) 0.032(7) Uiso 1 1 d . . . C11 C 1.0681(2) 0.47830(12) 0.82116(16) 0.0329(4) Uani 1 1 d . . . F11A F 1.10746(16) 0.41254(9) 0.81129(16) 0.0555(5) Uani 1 1 d . . . F11B F 1.14934(15) 0.51971(11) 0.77712(14) 0.0543(4) Uani 1 1 d . . . F11C F 1.08593(17) 0.49394(11) 0.91852(12) 0.0554(4) Uani 1 1 d . . . C12 C 0.8526(3) 0.58092(11) 0.80527(17) 0.0349(4) Uani 1 1 d . . . F12A F 0.8386(2) 0.58294(9) 0.90269(12) 0.0569(5) Uani 1 1 d . . . F12B F 0.94986(18) 0.62513(8) 0.78951(13) 0.0481(4) Uani 1 1 d . . . F12C F 0.73697(17) 0.60314(8) 0.75298(13) 0.0455(3) Uani 1 1 d . . . Sb1 Sb 0.064269(13) 0.300188(7) 0.502009(10) 0.02612(3) Uani 1 1 d . . . F1 F -0.04931(18) 0.36038(11) 0.41932(17) 0.0633(5) Uani 1 1 d . . . F2 F -0.08194(19) 0.27799(11) 0.57102(13) 0.0581(5) Uani 1 1 d . . . F3 F 0.1782(2) 0.24060(9) 0.58352(15) 0.0632(5) Uani 1 1 d . . . F4 F 0.20734(15) 0.32522(10) 0.43318(13) 0.0484(4) Uani 1 1 d . . . F5 F 0.01346(16) 0.22504(9) 0.41263(12) 0.0481(4) Uani 1 1 d . . . F6 F 0.11169(17) 0.37478(9) 0.59219(14) 0.0516(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02004(5) 0.02116(6) 0.02140(6) 0.00359(4) 0.00152(4) 0.00217(4) C1 0.0224(6) 0.0214(6) 0.0234(7) 0.0023(5) -0.0003(5) 0.0026(5) P1 0.02296(19) 0.0291(2) 0.0337(2) 0.00753(18) 0.00200(17) -0.00306(17) P2 0.02373(18) 0.02114(18) 0.02203(18) 0.00049(14) 0.00109(14) 0.00021(14) C13 0.0325(8) 0.0287(8) 0.0259(8) 0.0023(6) 0.0021(6) 0.0024(7) C14 0.0294(8) 0.0330(9) 0.0328(9) 0.0054(7) 0.0059(7) 0.0055(7) O1W 0.0327(7) 0.0337(7) 0.0265(6) -0.0013(6) 0.0001(5) 0.0119(6) O1 0.0626(12) 0.0467(10) 0.0265(7) 0.0057(7) 0.0008(7) 0.0043(9) O2 0.0447(9) 0.0433(9) 0.0580(11) 0.0050(8) 0.0184(8) 0.0177(8) C2 0.0234(7) 0.0204(6) 0.0224(7) 0.0015(5) 0.0011(5) 0.0031(5) C3 0.0329(8) 0.0253(7) 0.0225(7) 0.0027(6) 0.0016(6) 0.0042(6) C4 0.0369(9) 0.0311(9) 0.0217(7) 0.0006(6) -0.0038(6) 0.0048(7) C5 0.0301(8) 0.0290(8) 0.0298(8) -0.0015(7) -0.0067(7) 0.0013(7) C6 0.0234(7) 0.0251(7) 0.0278(8) 0.0022(6) -0.0031(6) -0.0002(6) C7 0.0241(8) 0.0392(10) 0.0377(10) 0.0065(8) -0.0046(7) -0.0060(7) C8 0.0302(9) 0.0554(15) 0.0453(12) 0.0153(11) 0.0077(9) -0.0054(9) F8A 0.0434(9) 0.0716(12) 0.0742(12) 0.0040(10) 0.0300(9) 0.0041(8) F8B 0.0350(8) 0.0949(15) 0.0650(11) 0.0169(11) 0.0067(7) -0.0281(9) F8C 0.0527(9) 0.0789(13) 0.0524(10) 0.0329(9) 0.0130(8) 0.0009(9) C9 0.0376(11) 0.0285(10) 0.0641(16) 0.0041(10) 0.0037(10) -0.0076(8) F9A 0.0583(10) 0.0398(8) 0.0610(10) -0.0130(7) 0.0113(8) -0.0037(7) F9B 0.0593(10) 0.0370(8) 0.0772(13) 0.0229(8) 0.0036(9) 0.0069(7) F9C 0.0527(10) 0.0383(9) 0.125(2) -0.0013(10) 0.0079(11) -0.0218(8) C10 0.0269(7) 0.0287(8) 0.0241(7) 0.0012(6) 0.0038(6) -0.0036(6) C11 0.0264(8) 0.0388(10) 0.0314(9) 0.0018(8) -0.0031(7) -0.0041(7) F11A 0.0308(7) 0.0461(9) 0.0845(13) -0.0025(8) -0.0096(7) 0.0100(6) F11B 0.0294(6) 0.0741(12) 0.0577(10) 0.0183(9) 0.0006(6) -0.0152(7) F11C 0.0460(8) 0.0852(13) 0.0304(7) -0.0013(8) -0.0105(6) -0.0083(8) C12 0.0522(12) 0.0228(8) 0.0307(9) -0.0006(7) 0.0095(8) 0.0017(8) F12A 0.1064(15) 0.0354(7) 0.0323(7) -0.0050(6) 0.0217(8) 0.0059(9) F12B 0.0606(10) 0.0276(6) 0.0565(9) -0.0059(6) 0.0098(8) -0.0128(6) F12C 0.0506(8) 0.0308(6) 0.0560(9) 0.0058(6) 0.0109(7) 0.0144(6) Sb1 0.02649(5) 0.02483(5) 0.02783(6) -0.00438(4) 0.00653(4) -0.00457(4) F1 0.0399(8) 0.0592(11) 0.0871(14) 0.0254(10) -0.0040(9) 0.0052(8) F2 0.0600(10) 0.0700(11) 0.0518(9) -0.0212(8) 0.0337(8) -0.0337(9) F3 0.0766(12) 0.0390(8) 0.0638(11) 0.0122(8) -0.0258(9) -0.0063(8) F4 0.0342(7) 0.0667(10) 0.0476(8) -0.0073(8) 0.0179(6) -0.0119(7) F5 0.0455(8) 0.0537(9) 0.0444(8) -0.0250(7) 0.0040(6) -0.0130(7) F6 0.0486(8) 0.0413(8) 0.0673(10) -0.0308(8) 0.0167(8) -0.0116(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C14 1.862(2) . ? Ru1 C13 2.0106(19) . ? Ru1 C1 2.1275(17) . ? Ru1 O1W 2.1467(15) . ? Ru1 P1 2.2953(5) . ? Ru1 P2 2.3172(5) . ? C1 C2 1.408(2) . ? C1 C6 1.412(2) . ? P1 C7 1.810(2) . ? P1 C9 1.878(3) . ? P1 C8 1.882(2) . ? P2 C10 1.8107(19) . ? P2 C12 1.878(2) . ? P2 C11 1.884(2) . ? C13 O1 1.119(2) . ? C14 O2 1.136(3) . ? O1W H1A 0.86(5) . ? O1W H1B 0.69(4) . ? C2 C3 1.393(2) . ? C2 C10 1.512(3) . ? C3 C4 1.386(3) . ? C3 H3 0.92(3) . ? C4 C5 1.385(3) . ? C4 H4 0.89(3) . ? C5 C6 1.391(3) . ? C5 H5 0.94(3) . ? C6 C7 1.512(3) . ? C7 H7A 0.95(3) . ? C7 H7B 0.93(3) . ? C8 F8B 1.314(3) . ? C8 F8A 1.332(4) . ? C8 F8C 1.334(3) . ? C9 F9B 1.326(3) . ? C9 F9C 1.332(3) . ? C9 F9A 1.335(3) . ? C10 H10A 0.95(3) . ? C10 H10B 0.93(3) . ? C11 F11A 1.319(3) . ? C11 F11B 1.323(3) . ? C11 F11C 1.325(3) . ? C12 F12B 1.320(3) . ? C12 F12C 1.328(3) . ? C12 F12A 1.333(3) . ? Sb1 F3 1.8452(17) . ? Sb1 F1 1.8583(17) . ? Sb1 F4 1.8633(14) . ? Sb1 F6 1.8768(14) . ? Sb1 F2 1.8780(15) . ? Sb1 F5 1.8839(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 C14 Ru1 C13 92.07(9) . . ? C14 Ru1 C1 90.74(8) . . ? C13 Ru1 C1 176.74(7) . . ? C14 Ru1 O1W 177.18(8) . . ? C13 Ru1 O1W 90.74(7) . . ? C1 Ru1 O1W 86.47(6) . . ? C14 Ru1 P1 89.67(7) . . ? C13 Ru1 P1 99.29(6) . . ? C1 Ru1 P1 79.06(5) . . ? O1W Ru1 P1 90.22(5) . . ? C14 Ru1 P2 92.19(7) . . ? C13 Ru1 P2 101.84(6) . . ? C1 Ru1 P2 79.70(5) . . ? O1W Ru1 P2 86.89(5) . . ? P1 Ru1 P2 158.699(19) . . ? C2 C1 C6 117.58(16) . . ? C2 C1 Ru1 121.12(12) . . ? C6 C1 Ru1 121.19(13) . . ? C7 P1 C9 104.77(13) . . ? C7 P1 C8 106.05(11) . . ? C9 P1 C8 100.34(13) . . ? C7 P1 Ru1 106.79(7) . . ? C9 P1 Ru1 116.75(8) . . ? C8 P1 Ru1 120.72(10) . . ? C10 P2 C12 105.40(9) . . ? C10 P2 C11 104.22(9) . . ? C12 P2 C11 99.97(11) . . ? C10 P2 Ru1 106.49(6) . . ? C12 P2 Ru1 117.59(8) . . ? C11 P2 Ru1 121.52(7) . . ? O1 C13 Ru1 175.5(2) . . ? O2 C14 Ru1 179.2(2) . . ? Ru1 O1W H1A 129(3) . . ? Ru1 O1W H1B 125(3) . . ? H1A O1W H1B 105(4) . . ? C3 C2 C1 120.87(17) . . ? C3 C2 C10 118.40(16) . . ? C1 C2 C10 120.70(15) . . ? C4 C3 C2 120.35(18) . . ? C4 C3 H3 121.5(18) . . ? C2 C3 H3 118.1(19) . . ? C5 C4 C3 119.90(18) . . ? C5 C4 H4 118.3(19) . . ? C3 C4 H4 121.8(19) . . ? C4 C5 C6 120.27(18) . . ? C4 C5 H5 120(2) . . ? C6 C5 H5 120(2) . . ? C5 C6 C1 121.01(18) . . ? C5 C6 C7 119.19(17) . . ? C1 C6 C7 119.80(17) . . ? C6 C7 P1 105.87(13) . . ? C6 C7 H7A 111.5(17) . . ? P1 C7 H7A 102.7(17) . . ? C6 C7 H7B 116(2) . . ? P1 C7 H7B 109(2) . . ? H7A C7 H7B 111(3) . . ? F8B C8 F8A 107.6(2) . . ? F8B C8 F8C 109.3(2) . . ? F8A C8 F8C 107.6(2) . . ? F8B C8 P1 113.3(2) . . ? F8A C8 P1 108.46(17) . . ? F8C C8 P1 110.39(17) . . ? F9B C9 F9C 108.1(2) . . ? F9B C9 F9A 109.0(2) . . ? F9C C9 F9A 107.6(2) . . ? F9B C9 P1 111.5(2) . . ? F9C C9 P1 111.90(19) . . ? F9A C9 P1 108.61(17) . . ? C2 C10 P2 107.89(12) . . ? C2 C10 H10A 116.0(17) . . ? P2 C10 H10A 105.5(17) . . ? C2 C10 H10B 110.5(18) . . ? P2 C10 H10B 107.3(18) . . ? H10A C10 H10B 109(2) . . ? F11A C11 F11B 107.9(2) . . ? F11A C11 F11C 108.1(2) . . ? F11B C11 F11C 107.53(19) . . ? F11A C11 P2 109.77(14) . . ? F11B C11 P2 112.83(15) . . ? F11C C11 P2 110.57(16) . . ? F12B C12 F12C 108.30(18) . . ? F12B C12 F12A 108.6(2) . . ? F12C C12 F12A 107.8(2) . . ? F12B C12 P2 113.34(16) . . ? F12C C12 P2 108.44(16) . . ? F12A C12 P2 110.22(15) . . ? F3 Sb1 F1 179.52(10) . . ? F3 Sb1 F4 90.04(10) . . ? F1 Sb1 F4 89.49(9) . . ? F3 Sb1 F6 90.16(9) . . ? F1 Sb1 F6 89.86(10) . . ? F4 Sb1 F6 89.23(7) . . ? F3 Sb1 F2 91.44(10) . . ? F1 Sb1 F2 89.04(10) . . ? F4 Sb1 F2 178.14(9) . . ? F6 Sb1 F2 89.64(7) . . ? F3 Sb1 F5 90.02(8) . . ? F1 Sb1 F5 89.97(9) . . ? F4 Sb1 F5 91.90(7) . . ? F6 Sb1 F5 178.86(7) . . ? F2 Sb1 F5 89.23(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 35.63 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.066 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.100 #----------------------------------------------------------------------------- data_bcg02 _database_code_depnum_ccdc_archive 'CCDC 886426' #TrackingRef '- Combined.cif' #Compound 13: [(O-(CF3)2PCH2C6H3CH2P(CF3)O)-Ru(CO)2]2 #----------------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H14 F18 O6 P4 Ru2' _chemical_formula_sum 'C26 H14 F18 O6 P4 Ru2' _chemical_formula_weight 1090.39 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4378(6) _cell_length_b 10.7359(6) _cell_length_c 17.9606(10) _cell_angle_alpha 87.327(3) _cell_angle_beta 80.705(3) _cell_angle_gamma 64.441(3) _cell_volume 1791.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9949 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 35.21 _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.156 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7364 _exptl_absorpt_correction_T_max 0.8709 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45442 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 33.73 _reflns_number_total 14207 _reflns_number_gt 12296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0299P)^2^+0.8503P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14207 _refine_ls_number_parameters 561 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Ru1 Ru 0.762682(13) 0.624248(11) 0.535820(7) 0.02412(3) Uani 1 1 d . . . P1 P 0.67059(4) 0.78977(4) 0.63376(2) 0.02648(7) Uani 1 1 d . . . P2 P 0.89095(4) 0.52147(4) 0.42184(2) 0.02551(7) Uani 1 1 d . . . C1 C 0.81174(14) 0.78273(13) 0.48395(8) 0.0210(2) Uani 1 1 d . . . C12 C 0.7359(3) 0.4628(2) 0.58062(12) 0.0462(5) Uani 1 1 d . . . C13 C 0.59338(19) 0.69041(19) 0.49481(11) 0.0357(3) Uani 1 1 d . . . O1 O 1.05116(13) 0.42770(12) 0.41326(7) 0.0358(3) Uani 1 1 d . . . C2 C 0.85796(16) 0.77823(14) 0.40555(8) 0.0243(3) Uani 1 1 d . . . O2 O 0.7210(3) 0.3693(2) 0.60257(12) 0.0756(6) Uani 1 1 d . . . O3 O 0.49029(16) 0.73387(18) 0.46909(11) 0.0569(4) Uani 1 1 d . . . C3 C 0.90176(18) 0.87589(16) 0.37197(9) 0.0307(3) Uani 1 1 d . . . H3 H 0.942(2) 0.865(2) 0.3187(13) 0.034(5) Uiso 1 1 d . . . C4 C 0.8926(2) 0.98398(18) 0.41529(11) 0.0345(3) Uani 1 1 d . . . H4 H 0.918(3) 1.051(3) 0.3918(14) 0.049(7) Uiso 1 1 d . . . C5 C 0.84401(17) 0.99287(16) 0.49207(10) 0.0299(3) Uani 1 1 d . . . H5 H 0.838(3) 1.068(2) 0.5228(13) 0.042(6) Uiso 1 1 d . . . C6 C 0.80678(15) 0.89195(14) 0.52668(8) 0.0231(2) Uani 1 1 d . . . C7 C 0.76477(18) 0.89821(17) 0.61160(9) 0.0285(3) Uani 1 1 d . . . H7A H 0.855(3) 0.853(2) 0.6364(13) 0.043(6) Uiso 1 1 d . . . H7B H 0.707(3) 0.985(3) 0.6347(15) 0.050(7) Uiso 1 1 d . . . C8 C 0.47637(18) 0.91554(19) 0.64301(10) 0.0341(3) Uani 1 1 d . . . F8A F 0.39137(13) 0.85235(14) 0.66302(8) 0.0508(3) Uani 1 1 d . . . F8B F 0.45152(12) 0.97088(12) 0.57618(6) 0.0436(3) Uani 1 1 d . . . F8C F 0.43634(13) 1.01888(13) 0.69294(7) 0.0496(3) Uani 1 1 d . . . C9 C 0.6817(2) 0.7498(2) 0.73637(10) 0.0438(4) Uani 1 1 d . . . F9A F 0.6004(3) 0.6898(3) 0.76324(10) 0.1146(9) Uani 1 1 d . . . F9B F 0.81321(17) 0.6703(2) 0.74613(8) 0.0807(6) Uani 1 1 d . . . F9C F 0.6431(3) 0.86021(19) 0.78008(8) 0.1037(8) Uani 1 1 d . . . C10 C 0.8589(2) 0.66436(15) 0.35852(9) 0.0303(3) Uani 1 1 d . . . H10A H 0.933(3) 0.638(2) 0.3138(14) 0.042(6) Uiso 1 1 d . . . H10B H 0.764(2) 0.693(2) 0.3445(12) 0.032(5) Uiso 1 1 d . . . C11 C 0.8227(3) 0.4144(2) 0.37563(14) 0.0491(5) Uani 1 1 d . . . F11A F 0.68368(16) 0.48331(16) 0.36900(11) 0.0711(5) Uani 1 1 d . . . F11B F 0.89465(18) 0.36870(18) 0.30733(10) 0.0748(5) Uani 1 1 d . . . F11C F 0.8358(2) 0.30316(16) 0.41565(13) 0.0890(6) Uani 1 1 d . . . Ru2 Ru 0.882850(11) 1.023226(10) -0.097975(6) 0.01852(3) Uani 1 1 d . . . P3 P 0.66132(4) 1.20908(4) -0.10622(2) 0.02607(7) Uani 1 1 d . . . P4 P 1.12426(4) 0.91618(4) -0.090650(19) 0.02008(6) Uani 1 1 d . . . C14 C 0.94360(16) 1.18810(15) -0.12034(8) 0.0237(2) Uani 1 1 d . . . C25 C 0.83701(17) 0.86453(16) -0.06921(9) 0.0282(3) Uani 1 1 d . . . C26 C 0.92200(17) 0.97251(16) -0.19922(8) 0.0268(3) Uani 1 1 d . . . O4 O 1.17777(11) 0.90202(11) -0.01550(6) 0.02492(19) Uani 1 1 d . . . O5 O 0.81635(17) 0.77086(15) -0.05533(10) 0.0491(4) Uani 1 1 d . . . O6 O 0.94367(16) 0.94242(15) -0.26162(7) 0.0403(3) Uani 1 1 d . . . C15 C 1.08882(17) 1.16113(17) -0.14280(8) 0.0273(3) Uani 1 1 d . . . C16 C 1.1299(2) 1.2696(2) -0.15172(10) 0.0382(4) Uani 1 1 d . . . H16 H 1.230(3) 1.247(2) -0.1667(13) 0.041(6) Uiso 1 1 d . . . C17 C 1.0274(3) 1.4048(2) -0.13929(12) 0.0457(5) Uani 1 1 d . . . H17 H 1.054(3) 1.473(3) -0.1452(16) 0.064(8) Uiso 1 1 d . . . C18 C 0.8841(2) 1.43396(19) -0.11759(11) 0.0401(4) Uani 1 1 d . . . H18 H 0.820(3) 1.523(3) -0.1087(13) 0.043(6) Uiso 1 1 d . . . C19 C 0.84123(19) 1.32663(16) -0.10793(9) 0.0293(3) Uani 1 1 d . . . C20 C 0.6845(2) 1.36035(17) -0.08187(11) 0.0326(3) Uani 1 1 d . . . H20A H 0.666(3) 1.369(2) -0.0308(14) 0.041(6) Uiso 1 1 d . . . H20B H 0.623(3) 1.441(3) -0.1044(14) 0.050(7) Uiso 1 1 d . . . C21 C 0.6008(2) 1.2522(2) -0.20087(12) 0.0451(5) Uani 1 1 d . . . F21A F 0.4867(2) 1.37186(17) -0.20150(10) 0.0870(6) Uani 1 1 d . . . F21B F 0.5686(2) 1.15671(17) -0.22552(9) 0.0702(4) Uani 1 1 d . . . F21C F 0.7065(2) 1.2564(2) -0.25001(8) 0.0788(5) Uani 1 1 d . . . C22 C 0.48628(18) 1.2302(2) -0.04742(12) 0.0378(4) Uani 1 1 d . . . F22A F 0.50078(14) 1.2088(2) 0.02387(8) 0.0663(4) Uani 1 1 d . . . F22B F 0.44427(15) 1.13945(16) -0.06967(9) 0.0616(4) Uani 1 1 d . . . F22C F 0.37916(14) 1.35358(15) -0.05124(12) 0.0768(5) Uani 1 1 d . . . C23 C 1.19859(17) 1.01224(18) -0.15513(9) 0.0295(3) Uani 1 1 d . . . H23A H 1.207(2) 0.982(2) -0.2051(13) 0.037(6) Uiso 1 1 d . . . H23B H 1.292(2) 0.996(2) -0.1459(13) 0.036(6) Uiso 1 1 d . . . C24 C 1.22506(18) 0.73483(18) -0.13065(10) 0.0340(3) Uani 1 1 d . . . F24A F 1.36524(12) 0.68219(13) -0.12658(7) 0.0475(3) Uani 1 1 d . . . F24B F 1.17595(15) 0.65040(12) -0.09239(9) 0.0575(4) Uani 1 1 d . . . F24C F 1.21371(16) 0.72633(15) -0.20270(8) 0.0614(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02680(6) 0.01815(5) 0.02608(6) 0.00185(4) -0.00732(4) -0.00745(4) P1 0.02508(17) 0.02650(17) 0.02098(16) 0.00073(13) -0.00401(13) -0.00455(14) P2 0.02932(18) 0.01593(14) 0.02758(17) -0.00214(12) -0.01288(14) -0.00312(13) C1 0.0198(6) 0.0171(5) 0.0233(6) 0.0000(4) -0.0066(4) -0.0043(4) C12 0.0624(13) 0.0380(9) 0.0445(10) 0.0093(8) -0.0112(9) -0.0273(10) C13 0.0303(8) 0.0349(8) 0.0415(9) -0.0065(7) -0.0069(7) -0.0127(7) O1 0.0329(6) 0.0292(5) 0.0303(6) -0.0054(4) -0.0156(5) 0.0048(5) C2 0.0258(6) 0.0189(5) 0.0227(6) 0.0002(4) -0.0070(5) -0.0034(5) O2 0.1167(18) 0.0593(11) 0.0739(13) 0.0262(9) -0.0194(12) -0.0601(12) O3 0.0336(7) 0.0613(10) 0.0704(11) -0.0196(8) -0.0202(7) -0.0093(7) C3 0.0314(7) 0.0269(7) 0.0285(7) 0.0028(6) -0.0026(6) -0.0085(6) C4 0.0358(8) 0.0279(7) 0.0405(9) 0.0040(6) -0.0024(7) -0.0159(7) C5 0.0280(7) 0.0233(6) 0.0390(8) -0.0042(6) -0.0061(6) -0.0109(6) C6 0.0209(6) 0.0204(5) 0.0254(6) -0.0036(5) -0.0055(5) -0.0055(5) C7 0.0294(7) 0.0266(7) 0.0262(7) -0.0072(5) -0.0059(5) -0.0078(6) C8 0.0273(7) 0.0368(8) 0.0285(7) -0.0009(6) -0.0015(6) -0.0057(6) F8A 0.0315(6) 0.0564(7) 0.0603(8) 0.0052(6) -0.0009(5) -0.0176(5) F8B 0.0306(5) 0.0478(6) 0.0326(5) 0.0068(5) -0.0061(4) 0.0013(5) F8C 0.0374(6) 0.0467(7) 0.0450(6) -0.0179(5) -0.0011(5) 0.0002(5) C9 0.0442(10) 0.0503(11) 0.0254(8) 0.0068(7) -0.0069(7) -0.0099(9) F9A 0.1352(18) 0.211(3) 0.0555(10) 0.0705(14) -0.0379(11) -0.127(2) F9B 0.0599(9) 0.1058(13) 0.0363(7) 0.0190(8) -0.0189(6) 0.0040(9) F9C 0.161(2) 0.0706(11) 0.0296(7) -0.0092(7) -0.0261(9) 0.0016(12) C10 0.0392(8) 0.0215(6) 0.0239(6) -0.0010(5) -0.0132(6) -0.0043(6) C11 0.0530(12) 0.0307(8) 0.0645(13) -0.0144(8) -0.0231(10) -0.0127(8) F11A 0.0483(8) 0.0611(9) 0.1084(13) -0.0346(9) -0.0296(8) -0.0182(7) F11B 0.0676(10) 0.0761(10) 0.0758(10) -0.0499(8) -0.0177(8) -0.0190(8) F11C 0.1307(17) 0.0416(8) 0.1217(16) 0.0055(9) -0.0467(13) -0.0533(10) Ru2 0.01970(5) 0.01960(5) 0.01754(5) -0.00064(3) -0.00312(3) -0.00946(4) P3 0.02446(17) 0.02454(16) 0.02794(18) 0.00106(13) -0.00944(14) -0.00757(14) P4 0.01908(15) 0.02295(15) 0.01700(14) -0.00303(11) -0.00084(11) -0.00824(12) C14 0.0303(7) 0.0250(6) 0.0204(6) 0.0032(5) -0.0063(5) -0.0158(5) C25 0.0267(7) 0.0275(7) 0.0319(7) -0.0016(5) -0.0006(6) -0.0141(6) C26 0.0288(7) 0.0307(7) 0.0249(6) -0.0012(5) -0.0058(5) -0.0159(6) O4 0.0220(5) 0.0290(5) 0.0179(4) -0.0025(4) -0.0025(3) -0.0054(4) O5 0.0522(9) 0.0362(7) 0.0657(10) 0.0006(6) 0.0026(7) -0.0292(7) O6 0.0472(8) 0.0536(8) 0.0242(5) -0.0075(5) -0.0055(5) -0.0248(6) C15 0.0329(7) 0.0362(7) 0.0215(6) 0.0065(5) -0.0070(5) -0.0227(6) C16 0.0474(10) 0.0496(10) 0.0353(8) 0.0126(7) -0.0131(7) -0.0361(9) C17 0.0672(14) 0.0438(10) 0.0482(11) 0.0138(8) -0.0198(10) -0.0421(11) C18 0.0580(12) 0.0276(8) 0.0436(10) 0.0071(7) -0.0157(9) -0.0246(8) C19 0.0385(8) 0.0255(6) 0.0284(7) 0.0042(5) -0.0111(6) -0.0163(6) C20 0.0354(8) 0.0220(6) 0.0376(8) 0.0000(6) -0.0093(7) -0.0084(6) C21 0.0500(11) 0.0423(10) 0.0383(9) 0.0053(8) -0.0234(8) -0.0101(9) F21A 0.0961(13) 0.0569(9) 0.0712(10) -0.0004(8) -0.0575(10) 0.0169(8) F21B 0.0947(12) 0.0728(10) 0.0569(8) -0.0017(7) -0.0442(8) -0.0376(9) F21C 0.0885(12) 0.1130(14) 0.0399(7) 0.0341(8) -0.0239(8) -0.0464(11) C22 0.0225(7) 0.0373(9) 0.0493(10) -0.0042(7) -0.0069(7) -0.0080(6) F22A 0.0364(7) 0.1215(14) 0.0399(7) -0.0038(8) 0.0014(5) -0.0349(8) F22B 0.0474(7) 0.0714(9) 0.0780(10) -0.0172(8) 0.0018(7) -0.0387(7) F22C 0.0295(6) 0.0469(8) 0.1264(15) 0.0085(8) 0.0031(8) 0.0036(6) C23 0.0260(7) 0.0425(8) 0.0223(6) 0.0028(6) -0.0007(5) -0.0183(6) C24 0.0263(7) 0.0321(8) 0.0371(8) -0.0138(6) -0.0038(6) -0.0055(6) F24A 0.0247(5) 0.0446(6) 0.0587(7) -0.0220(5) -0.0035(5) -0.0003(4) F24B 0.0492(7) 0.0264(5) 0.0918(11) -0.0101(6) 0.0020(7) -0.0149(5) F24C 0.0632(8) 0.0565(8) 0.0468(7) -0.0317(6) -0.0178(6) -0.0029(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C13 1.8597(18) . ? Ru1 C12 1.9864(19) . ? Ru1 C1 2.1154(14) . ? Ru1 O1 2.1247(12) 2_766 ? Ru1 P2 2.2916(4) . ? Ru1 P1 2.3339(4) . ? Ru1 Ru1 4.4914(4) 2_766 ? P1 C7 1.8161(17) . ? P1 C8 1.8736(17) . ? P1 C9 1.8834(18) . ? P2 O1 1.5206(13) . ? P2 C10 1.8100(16) . ? P2 C11 1.8718(19) . ? C1 C2 1.409(2) . ? C1 C6 1.4090(19) . ? C12 O2 1.125(2) . ? C13 O3 1.138(2) . ? O1 Ru1 2.1247(12) 2_766 ? C2 C3 1.392(2) . ? C2 C10 1.514(2) . ? C3 C4 1.388(2) . ? C3 H3 0.97(2) . ? C4 C5 1.383(3) . ? C4 H4 0.93(3) . ? C5 C6 1.391(2) . ? C5 H5 0.98(2) . ? C6 C7 1.514(2) . ? C7 H7A 1.02(2) . ? C7 H7B 0.94(3) . ? C8 F8B 1.327(2) . ? C8 F8A 1.330(2) . ? C8 F8C 1.335(2) . ? C9 F9A 1.296(3) . ? C9 F9B 1.302(3) . ? C9 F9C 1.325(3) . ? C10 H10A 0.98(2) . ? C10 H10B 0.98(2) . ? C11 F11B 1.323(3) . ? C11 F11C 1.331(3) . ? C11 F11A 1.338(3) . ? Ru2 C26 1.8522(15) . ? Ru2 C25 1.9850(15) . ? Ru2 O4 2.1203(10) 2_775 ? Ru2 C14 2.1252(14) . ? Ru2 P4 2.2982(4) . ? Ru2 P3 2.3350(4) . ? Ru2 Ru2 4.4922(3) 2_775 ? P3 C20 1.8238(17) . ? P3 C21 1.8772(19) . ? P3 C22 1.8832(19) . ? P4 O4 1.5192(11) . ? P4 C23 1.8153(15) . ? P4 C24 1.8795(17) . ? C14 C15 1.407(2) . ? C14 C19 1.409(2) . ? C25 O5 1.1253(19) . ? C26 O6 1.1403(19) . ? O4 Ru2 2.1203(10) 2_775 ? C15 C16 1.399(2) . ? C15 C23 1.512(2) . ? C16 C17 1.384(3) . ? C16 H16 0.96(2) . ? C17 C18 1.381(3) . ? C17 H17 0.89(3) . ? C18 C19 1.400(2) . ? C18 H18 0.90(2) . ? C19 C20 1.511(3) . ? C20 H20A 0.91(2) . ? C20 H20B 0.95(3) . ? C21 F21C 1.313(3) . ? C21 F21B 1.322(3) . ? C21 F21A 1.324(2) . ? C22 F22A 1.312(2) . ? C22 F22C 1.322(2) . ? C22 F22B 1.328(2) . ? C23 H23A 0.95(2) . ? C23 H23B 0.96(2) . ? C24 F24C 1.329(2) . ? C24 F24A 1.335(2) . ? C24 F24B 1.336(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Ru1 C12 93.16(9) . . ? C13 Ru1 C1 90.51(7) . . ? C12 Ru1 C1 174.49(8) . . ? C13 Ru1 O1 173.46(6) . 2_766 ? C12 Ru1 O1 91.50(8) . 2_766 ? C1 Ru1 O1 85.19(5) . 2_766 ? C13 Ru1 P2 89.93(6) . . ? C12 Ru1 P2 97.41(7) . . ? C1 Ru1 P2 78.47(4) . . ? O1 Ru1 P2 94.02(3) 2_766 . ? C13 Ru1 P1 94.95(6) . . ? C12 Ru1 P1 104.63(7) . . ? C1 Ru1 P1 79.12(4) . . ? O1 Ru1 P1 79.42(3) 2_766 . ? P2 Ru1 P1 157.091(16) . . ? C13 Ru1 Ru1 139.20(6) . 2_766 ? C12 Ru1 Ru1 93.05(7) . 2_766 ? C1 Ru1 Ru1 81.49(4) . 2_766 ? O1 Ru1 Ru1 44.93(3) 2_766 2_766 ? P2 Ru1 Ru1 49.271(10) . 2_766 ? P1 Ru1 Ru1 122.161(12) . 2_766 ? C7 P1 C8 103.46(8) . . ? C7 P1 C9 104.37(9) . . ? C8 P1 C9 99.03(8) . . ? C7 P1 Ru1 105.02(5) . . ? C8 P1 Ru1 117.94(6) . . ? C9 P1 Ru1 124.65(7) . . ? O1 P2 C10 109.81(8) . . ? O1 P2 C11 101.85(9) . . ? C10 P2 C11 102.10(9) . . ? O1 P2 Ru1 121.21(5) . . ? C10 P2 Ru1 104.09(5) . . ? C11 P2 Ru1 116.26(8) . . ? C2 C1 C6 117.75(13) . . ? C2 C1 Ru1 120.70(10) . . ? C6 C1 Ru1 121.47(10) . . ? O2 C12 Ru1 176.7(2) . . ? O3 C13 Ru1 178.21(19) . . ? P2 O1 Ru1 143.09(7) . 2_766 ? C3 C2 C1 120.98(14) . . ? C3 C2 C10 120.66(14) . . ? C1 C2 C10 118.36(13) . . ? C4 C3 C2 119.86(15) . . ? C4 C3 H3 120.6(13) . . ? C2 C3 H3 119.5(13) . . ? C5 C4 C3 120.27(15) . . ? C5 C4 H4 120.6(16) . . ? C3 C4 H4 119.1(16) . . ? C4 C5 C6 120.21(14) . . ? C4 C5 H5 120.4(14) . . ? C6 C5 H5 119.4(14) . . ? C5 C6 C1 120.82(14) . . ? C5 C6 C7 119.13(13) . . ? C1 C6 C7 120.03(13) . . ? C6 C7 P1 106.91(10) . . ? C6 C7 H7A 109.7(14) . . ? P1 C7 H7A 105.5(13) . . ? C6 C7 H7B 117.5(16) . . ? P1 C7 H7B 108.4(16) . . ? H7A C7 H7B 108(2) . . ? F8B C8 F8A 108.18(15) . . ? F8B C8 F8C 107.54(15) . . ? F8A C8 F8C 107.18(14) . . ? F8B C8 P1 108.11(11) . . ? F8A C8 P1 111.03(13) . . ? F8C C8 P1 114.59(13) . . ? F9A C9 F9B 108.7(2) . . ? F9A C9 F9C 107.0(2) . . ? F9B C9 F9C 104.6(2) . . ? F9A C9 P1 111.22(16) . . ? F9B C9 P1 111.21(14) . . ? F9C C9 P1 113.77(15) . . ? C2 C10 P2 104.52(10) . . ? C2 C10 H10A 112.6(14) . . ? P2 C10 H10A 111.2(14) . . ? C2 C10 H10B 109.4(12) . . ? P2 C10 H10B 108.0(12) . . ? H10A C10 H10B 110.8(19) . . ? F11B C11 F11C 106.40(18) . . ? F11B C11 F11A 107.29(19) . . ? F11C C11 F11A 106.8(2) . . ? F11B C11 P2 112.59(17) . . ? F11C C11 P2 110.80(16) . . ? F11A C11 P2 112.55(13) . . ? C26 Ru2 C25 91.39(7) . . ? C26 Ru2 O4 174.78(6) . 2_775 ? C25 Ru2 O4 90.89(6) . 2_775 ? C26 Ru2 C14 92.39(6) . . ? C25 Ru2 C14 174.59(6) . . ? O4 Ru2 C14 85.67(5) 2_775 . ? C26 Ru2 P4 90.21(5) . . ? C25 Ru2 P4 97.97(5) . . ? O4 Ru2 P4 94.13(3) 2_775 . ? C14 Ru2 P4 78.15(4) . . ? C26 Ru2 P3 94.81(5) . . ? C25 Ru2 P3 105.05(5) . . ? O4 Ru2 P3 80.05(3) 2_775 . ? C14 Ru2 P3 78.49(4) . . ? P4 Ru2 P3 156.276(14) . . ? C26 Ru2 Ru2 139.48(5) . 2_775 ? C25 Ru2 Ru2 93.58(5) . 2_775 ? O4 Ru2 Ru2 44.98(3) 2_775 2_775 ? C14 Ru2 Ru2 81.04(4) . 2_775 ? P4 Ru2 Ru2 49.269(9) . 2_775 ? P3 Ru2 Ru2 122.337(11) . 2_775 ? C20 P3 C21 102.98(9) . . ? C20 P3 C22 104.69(9) . . ? C21 P3 C22 99.19(10) . . ? C20 P3 Ru2 104.48(6) . . ? C21 P3 Ru2 118.91(7) . . ? C22 P3 Ru2 124.14(6) . . ? O4 P4 C23 110.18(7) . . ? O4 P4 C24 101.66(7) . . ? C23 P4 C24 102.86(8) . . ? O4 P4 Ru2 121.13(4) . . ? C23 P4 Ru2 103.41(6) . . ? C24 P4 Ru2 116.28(6) . . ? C15 C14 C19 118.34(13) . . ? C15 C14 Ru2 120.59(11) . . ? C19 C14 Ru2 120.92(11) . . ? O5 C25 Ru2 176.76(15) . . ? O6 C26 Ru2 178.84(16) . . ? P4 O4 Ru2 143.59(7) . 2_775 ? C16 C15 C14 120.49(16) . . ? C16 C15 C23 121.31(15) . . ? C14 C15 C23 118.18(13) . . ? C17 C16 C15 120.12(18) . . ? C17 C16 H16 121.9(14) . . ? C15 C16 H16 118.0(14) . . ? C18 C17 C16 120.44(16) . . ? C18 C17 H17 119.6(19) . . ? C16 C17 H17 119.9(19) . . ? C17 C18 C19 120.18(18) . . ? C17 C18 H18 118.7(15) . . ? C19 C18 H18 121.1(16) . . ? C18 C19 C14 120.42(17) . . ? C18 C19 C20 119.38(16) . . ? C14 C19 C20 120.18(13) . . ? C19 C20 P3 106.14(11) . . ? C19 C20 H20A 108.7(15) . . ? P3 C20 H20A 106.9(15) . . ? C19 C20 H20B 112.1(15) . . ? P3 C20 H20B 111.6(15) . . ? H20A C20 H20B 111(2) . . ? F21C C21 F21B 107.1(2) . . ? F21C C21 F21A 108.2(2) . . ? F21B C21 F21A 106.97(19) . . ? F21C C21 P3 108.87(14) . . ? F21B C21 P3 111.56(15) . . ? F21A C21 P3 113.84(15) . . ? F22A C22 F22C 107.35(18) . . ? F22A C22 F22B 107.67(18) . . ? F22C C22 F22B 106.49(16) . . ? F22A C22 P3 110.62(12) . . ? F22C C22 P3 113.96(15) . . ? F22B C22 P3 110.46(13) . . ? C15 C23 P4 104.66(10) . . ? C15 C23 H23A 110.5(14) . . ? P4 C23 H23A 108.7(14) . . ? C15 C23 H23B 113.8(13) . . ? P4 C23 H23B 111.0(13) . . ? H23A C23 H23B 108.2(19) . . ? F24C C24 F24A 106.98(14) . . ? F24C C24 F24B 107.48(16) . . ? F24A C24 F24B 106.27(16) . . ? F24C C24 P4 112.48(13) . . ? F24A C24 P4 112.41(12) . . ? F24B C24 P4 110.88(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C6 C7 P1 -19.52(17) . . . . ? C1 C2 C10 P2 -29.79(17) . . . . ? C14 C19 C20 P3 -20.40(18) . . . . ? C14 C15 C23 P4 -29.82(16) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 33.73 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.797 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.075 #----------------------------------------------------------------------------- data_jja07 _database_code_depnum_ccdc_archive 'CCDC 886427' #TrackingRef '- Combined.cif' #Compound 14: (CF3PCP)Ru(PPh3)(\^I.2-O2CMe) #----------------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H25 F12 O2 P3 Ru' _chemical_formula_sum 'C32 H25 F12 O2 P3 Ru' _chemical_formula_weight 863.50 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' 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 P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 9.6943(3) _cell_length_b 22.1871(7) _cell_length_c 16.0255(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.631(2) _cell_angle_gamma 90.00 _cell_volume 3302.71(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9826 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 40.10 _exptl_crystal_description rectangular_prism _exptl_crystal_colour brown-yellow _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7388 _exptl_absorpt_correction_T_max 0.8334 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56633 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 34.97 _reflns_number_total 14492 _reflns_number_gt 12428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V.6.14 (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL V.6.14 (Bruker, 2001)' _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^)+(0.0251P)^2^+2.1379P] 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 14492 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.746577(10) 0.622773(4) 0.790609(6) 0.01362(2) Uani 1 1 d . . . P1 P 0.66376(4) 0.604943(15) 0.90900(2) 0.01786(6) Uani 1 1 d . . . P2 P 0.81483(4) 0.590235(15) 0.67532(2) 0.01901(6) Uani 1 1 d . . . P3 P 0.57515(3) 0.689773(14) 0.713508(19) 0.01489(5) Uani 1 1 d . . . O1 O 0.93292(10) 0.68180(4) 0.85728(6) 0.02055(17) Uani 1 1 d . . . O2 O 0.94531(10) 0.58397(4) 0.87275(6) 0.02173(17) Uani 1 1 d . . . C13 C 1.00409(14) 0.63558(6) 0.89049(8) 0.0207(2) Uani 1 1 d . . . C14 C 1.15462(16) 0.64035(8) 0.94895(10) 0.0321(3) Uani 1 1 d . . . H14A H 1.1802 0.6821 0.9592 0.048 Uiso 1 1 calc R . . H14B H 1.2195 0.6212 0.9218 0.048 Uiso 1 1 calc R . . H14C H 1.1608 0.6209 1.0034 0.048 Uiso 1 1 calc R . . C1 C 0.59670(13) 0.55264(5) 0.74638(8) 0.0176(2) Uani 1 1 d . . . C2 C 0.58918(15) 0.51930(6) 0.67012(8) 0.0214(2) Uani 1 1 d . . . C3 C 0.49437(16) 0.47109(6) 0.64327(10) 0.0268(3) Uani 1 1 d . . . H3A H 0.4950 0.4494 0.5937 0.032 Uiso 1 1 calc R . . C4 C 0.39942(17) 0.45515(7) 0.68966(11) 0.0296(3) Uani 1 1 d . . . H4A H 0.3366 0.4229 0.6717 0.035 Uiso 1 1 calc R . . C5 C 0.39927(15) 0.48797(6) 0.76323(10) 0.0257(3) Uani 1 1 d . . . H5A H 0.3351 0.4780 0.7945 0.031 Uiso 1 1 calc R . . C6 C 0.49490(14) 0.53592(6) 0.79071(8) 0.0199(2) Uani 1 1 d . . . C7 C 0.48595(15) 0.57291(6) 0.86818(9) 0.0226(2) Uani 1 1 d . . . H7A H 0.4629 0.5477 0.9118 0.027 Uiso 1 1 calc R . . H7B H 0.4137 0.6043 0.8507 0.027 Uiso 1 1 calc R . . C8 C 0.65109(17) 0.65225(7) 1.00626(9) 0.0283(3) Uani 1 1 d . . . F8A F 0.73029(14) 0.70199(5) 1.01349(8) 0.0473(3) Uani 1 1 d . . . F8B F 0.51569(13) 0.66963(6) 0.99610(8) 0.0477(3) Uani 1 1 d . . . F8C F 0.69451(17) 0.62442(6) 1.08289(7) 0.0554(4) Uani 1 1 d . . . C9 C 0.76377(16) 0.53909(7) 0.97507(9) 0.0253(3) Uani 1 1 d . . . F9A F 0.88807(11) 0.55577(5) 1.03081(6) 0.0331(2) Uani 1 1 d . . . F9B F 0.68530(12) 0.51291(5) 1.02240(7) 0.0402(2) Uani 1 1 d . . . F9C F 0.79046(11) 0.49629(4) 0.92380(6) 0.03084(19) Uani 1 1 d . . . C10 C 0.67744(18) 0.53954(7) 0.61156(9) 0.0280(3) Uani 1 1 d . . . H10A H 0.6170 0.5602 0.5609 0.034 Uiso 1 1 calc R . . H10B H 0.7217 0.5051 0.5921 0.034 Uiso 1 1 calc R . . C11 C 0.9797(2) 0.54009(8) 0.70353(11) 0.0341(3) Uani 1 1 d . . . F11A F 0.96150(15) 0.49419(5) 0.75262(8) 0.0474(3) Uani 1 1 d . . . F11B F 1.00569(15) 0.51586(6) 0.63245(8) 0.0548(3) Uani 1 1 d . . . F11C F 1.09875(11) 0.56988(6) 0.74614(7) 0.0430(3) Uani 1 1 d . . . C12 C 0.86554(17) 0.63247(7) 0.58565(9) 0.0258(3) Uani 1 1 d . . . F12A F 0.86527(15) 0.59816(5) 0.51708(7) 0.0466(3) Uani 1 1 d . . . F12B F 0.99494(11) 0.65750(6) 0.61353(7) 0.0408(2) Uani 1 1 d . . . F12C F 0.77166(12) 0.67677(5) 0.55527(6) 0.0374(2) Uani 1 1 d . . . C15 C 0.44785(14) 0.71944(6) 0.76870(8) 0.0189(2) Uani 1 1 d . . . C16 C 0.50659(16) 0.75475(7) 0.84222(10) 0.0281(3) Uani 1 1 d . . . H16A H 0.6059 0.7592 0.8632 0.034 Uiso 1 1 calc R . . C17 C 0.4181(2) 0.78345(9) 0.88445(11) 0.0364(4) Uani 1 1 d . . . H17A H 0.4583 0.8075 0.9328 0.044 Uiso 1 1 calc R . . C18 C 0.27071(19) 0.77635(8) 0.85485(12) 0.0352(3) Uani 1 1 d . . . H18A H 0.2114 0.7957 0.8829 0.042 Uiso 1 1 calc R . . C19 C 0.21217(17) 0.74034(8) 0.78351(12) 0.0335(3) Uani 1 1 d . . . H19A H 0.1131 0.7345 0.7645 0.040 Uiso 1 1 calc R . . C20 C 0.29955(15) 0.71245(7) 0.73939(10) 0.0263(3) Uani 1 1 d . . . H20A H 0.2585 0.6892 0.6903 0.032 Uiso 1 1 calc R . . C21 C 0.65582(14) 0.76175(5) 0.69581(8) 0.0181(2) Uani 1 1 d . . . C22 C 0.57154(16) 0.81406(6) 0.67717(9) 0.0243(2) Uani 1 1 d . . . H22A H 0.4726 0.8115 0.6681 0.029 Uiso 1 1 calc R . . C23 C 0.63445(19) 0.86970(6) 0.67205(10) 0.0302(3) Uani 1 1 d . . . H23A H 0.5776 0.9042 0.6599 0.036 Uiso 1 1 calc R . . C24 C 0.78167(19) 0.87399(7) 0.68495(10) 0.0328(3) Uani 1 1 d . . . H24A H 0.8239 0.9114 0.6827 0.039 Uiso 1 1 calc R . . C25 C 0.86561(17) 0.82254(7) 0.70118(11) 0.0309(3) Uani 1 1 d . . . H25A H 0.9641 0.8252 0.7084 0.037 Uiso 1 1 calc R . . C26 C 0.80288(15) 0.76664(6) 0.70676(9) 0.0225(2) Uani 1 1 d . . . H26A H 0.8601 0.7323 0.7179 0.027 Uiso 1 1 calc R . . C27 C 0.45832(14) 0.66866(6) 0.60565(8) 0.0185(2) Uani 1 1 d . . . C28 C 0.46592(15) 0.69912(6) 0.53065(8) 0.0226(2) Uani 1 1 d . . . H28A H 0.5290 0.7314 0.5354 0.027 Uiso 1 1 calc R . . C29 C 0.37969(18) 0.68144(7) 0.44893(9) 0.0298(3) Uani 1 1 d . . . H29A H 0.3871 0.7013 0.3993 0.036 Uiso 1 1 calc R . . C30 C 0.28323(19) 0.63452(7) 0.44126(10) 0.0324(3) Uani 1 1 d . . . H30A H 0.2257 0.6230 0.3866 0.039 Uiso 1 1 calc R . . C31 C 0.27224(16) 0.60465(7) 0.51517(10) 0.0277(3) Uani 1 1 d . . . H31A H 0.2060 0.5735 0.5101 0.033 Uiso 1 1 calc R . . C32 C 0.36016(15) 0.62117(6) 0.59703(9) 0.0220(2) Uani 1 1 d . . . H32A H 0.3536 0.6005 0.6462 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01385(4) 0.01373(4) 0.01402(4) 0.00124(3) 0.00518(3) 0.00031(3) P1 0.01912(14) 0.01980(14) 0.01619(12) 0.00068(10) 0.00751(11) -0.00349(11) P2 0.02124(15) 0.02000(14) 0.01821(13) 0.00045(10) 0.00954(11) 0.00345(11) P3 0.01375(13) 0.01524(12) 0.01542(11) -0.00044(9) 0.00374(10) 0.00072(9) O1 0.0178(4) 0.0198(4) 0.0225(4) 0.0033(3) 0.0033(3) -0.0017(3) O2 0.0192(4) 0.0217(4) 0.0239(4) 0.0070(3) 0.0056(3) 0.0031(3) C13 0.0163(5) 0.0273(6) 0.0186(5) 0.0052(4) 0.0052(4) 0.0005(4) C14 0.0185(6) 0.0431(9) 0.0299(7) 0.0083(6) -0.0007(5) -0.0006(6) C1 0.0170(5) 0.0159(5) 0.0191(5) 0.0003(4) 0.0040(4) -0.0008(4) C2 0.0239(6) 0.0181(5) 0.0216(5) -0.0024(4) 0.0053(4) 0.0000(4) C3 0.0280(7) 0.0203(6) 0.0282(6) -0.0062(5) 0.0017(5) -0.0008(5) C4 0.0253(7) 0.0212(6) 0.0371(7) -0.0032(5) 0.0007(6) -0.0062(5) C5 0.0204(6) 0.0235(6) 0.0314(6) 0.0019(5) 0.0048(5) -0.0055(5) C6 0.0177(5) 0.0198(5) 0.0210(5) 0.0019(4) 0.0039(4) -0.0025(4) C7 0.0197(6) 0.0272(6) 0.0228(5) 0.0008(4) 0.0092(4) -0.0054(5) C8 0.0326(8) 0.0321(7) 0.0236(6) -0.0042(5) 0.0135(5) -0.0052(6) F8A 0.0570(7) 0.0468(6) 0.0437(6) -0.0228(5) 0.0233(5) -0.0262(5) F8B 0.0369(6) 0.0593(7) 0.0530(7) -0.0230(6) 0.0228(5) 0.0007(5) F8C 0.0923(11) 0.0565(8) 0.0220(5) 0.0018(4) 0.0241(6) 0.0097(7) C9 0.0285(7) 0.0255(6) 0.0220(5) 0.0069(5) 0.0073(5) -0.0041(5) F9A 0.0314(5) 0.0398(5) 0.0224(4) 0.0056(4) -0.0015(3) -0.0026(4) F9B 0.0442(6) 0.0422(6) 0.0388(5) 0.0202(4) 0.0192(5) -0.0054(5) F9C 0.0382(5) 0.0200(4) 0.0325(4) 0.0037(3) 0.0073(4) 0.0006(3) C10 0.0357(8) 0.0276(7) 0.0233(6) -0.0082(5) 0.0127(5) -0.0033(6) C11 0.0387(9) 0.0364(8) 0.0321(7) 0.0034(6) 0.0178(7) 0.0181(7) F11A 0.0650(8) 0.0294(5) 0.0516(6) 0.0130(5) 0.0229(6) 0.0215(5) F11B 0.0646(8) 0.0624(8) 0.0460(6) -0.0029(6) 0.0297(6) 0.0352(7) F11C 0.0245(5) 0.0628(7) 0.0429(6) 0.0100(5) 0.0113(4) 0.0161(5) C12 0.0280(7) 0.0315(7) 0.0214(5) 0.0015(5) 0.0124(5) 0.0015(5) F12A 0.0753(9) 0.0457(6) 0.0306(5) -0.0054(4) 0.0342(5) -0.0029(6) F12B 0.0285(5) 0.0563(7) 0.0401(5) 0.0111(5) 0.0138(4) -0.0080(5) F12C 0.0382(5) 0.0461(6) 0.0314(5) 0.0177(4) 0.0156(4) 0.0134(4) C15 0.0162(5) 0.0205(5) 0.0202(5) -0.0020(4) 0.0057(4) 0.0015(4) C16 0.0220(6) 0.0363(8) 0.0262(6) -0.0110(5) 0.0072(5) 0.0000(5) C17 0.0363(9) 0.0434(9) 0.0317(7) -0.0147(7) 0.0133(6) 0.0043(7) C18 0.0336(8) 0.0384(8) 0.0398(8) -0.0047(7) 0.0206(7) 0.0089(7) C19 0.0199(6) 0.0419(9) 0.0416(8) -0.0055(7) 0.0132(6) 0.0048(6) C20 0.0176(6) 0.0296(7) 0.0312(6) -0.0066(5) 0.0064(5) 0.0005(5) C21 0.0187(5) 0.0157(5) 0.0183(5) 0.0013(4) 0.0029(4) 0.0003(4) C22 0.0245(6) 0.0190(5) 0.0271(6) 0.0022(4) 0.0038(5) 0.0041(5) C23 0.0405(9) 0.0166(6) 0.0285(6) 0.0026(5) 0.0017(6) 0.0028(5) C24 0.0400(9) 0.0200(6) 0.0301(7) 0.0063(5) -0.0032(6) -0.0084(6) C25 0.0256(7) 0.0272(7) 0.0345(7) 0.0107(5) -0.0002(6) -0.0079(5) C26 0.0193(6) 0.0205(6) 0.0257(6) 0.0061(4) 0.0036(4) -0.0012(4) C27 0.0172(5) 0.0194(5) 0.0172(5) -0.0013(4) 0.0022(4) 0.0033(4) C28 0.0250(6) 0.0228(6) 0.0189(5) 0.0010(4) 0.0044(4) 0.0053(5) C29 0.0365(8) 0.0319(7) 0.0174(5) 0.0004(5) 0.0019(5) 0.0096(6) C30 0.0352(8) 0.0326(7) 0.0218(6) -0.0076(5) -0.0040(5) 0.0085(6) C31 0.0246(7) 0.0251(6) 0.0281(6) -0.0079(5) -0.0007(5) 0.0018(5) C32 0.0203(6) 0.0206(5) 0.0227(5) -0.0034(4) 0.0022(4) 0.0012(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 Ru1 C1 2.1084(12) . ? Ru1 O2 2.1757(9) . ? Ru1 O1 2.2394(10) . ? Ru1 P2 2.2522(3) . ? Ru1 P1 2.2963(3) . ? Ru1 P3 2.3071(3) . ? Ru1 C13 2.5666(13) . ? P1 C7 1.8052(14) . ? P1 C9 1.8996(15) . ? P1 C8 1.9119(15) . ? P2 C10 1.8176(15) . ? P2 C11 1.8928(16) . ? P2 C12 1.8945(14) . ? P3 C15 1.8339(13) . ? P3 C27 1.8355(12) . ? P3 C21 1.8355(13) . ? O1 C13 1.2651(16) . ? O2 C13 1.2743(17) . ? C13 C14 1.495(2) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C1 C2 1.4124(17) . ? C1 C6 1.4204(18) . ? C2 C3 1.3956(19) . ? C2 C10 1.508(2) . ? C3 C4 1.384(2) . ? C3 H3A 0.9300 . ? C4 C5 1.386(2) . ? C4 H4A 0.9300 . ? C5 C6 1.3970(19) . ? C5 H5A 0.9300 . ? C6 C7 1.5114(19) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 F8A 1.3303(18) . ? C8 F8C 1.3306(19) . ? C8 F8B 1.333(2) . ? C9 F9C 1.3288(18) . ? C9 F9A 1.3307(17) . ? C9 F9B 1.3496(16) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 F11A 1.329(2) . ? C11 F11C 1.336(2) . ? C11 F11B 1.3470(18) . ? C12 F12B 1.3270(19) . ? C12 F12C 1.3332(18) . ? C12 F12A 1.3362(17) . ? C15 C20 1.3874(19) . ? C15 C16 1.3936(19) . ? C16 C17 1.390(2) . ? C16 H16A 0.9300 . ? C17 C18 1.379(3) . ? C17 H17A 0.9300 . ? C18 C19 1.377(2) . ? C18 H18A 0.9300 . ? C19 C20 1.394(2) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C26 1.3900(19) . ? C21 C22 1.4015(18) . ? C22 C23 1.390(2) . ? C22 H22A 0.9300 . ? C23 C24 1.386(3) . ? C23 H23A 0.9300 . ? C24 C25 1.383(2) . ? C24 H24A 0.9300 . ? C25 C26 1.3954(19) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C28 1.3992(18) . ? C27 C32 1.3998(19) . ? C28 C29 1.3933(19) . ? C28 H28A 0.9300 . ? C29 C30 1.381(3) . ? C29 H29A 0.9300 . ? C30 C31 1.388(2) . ? C30 H30A 0.9300 . ? C31 C32 1.3935(19) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 O2 108.48(4) . . ? C1 Ru1 O1 167.46(4) . . ? O2 Ru1 O1 59.27(4) . . ? C1 Ru1 P2 79.84(3) . . ? O2 Ru1 P2 87.27(3) . . ? O1 Ru1 P2 101.10(3) . . ? C1 Ru1 P1 77.31(3) . . ? O2 Ru1 P1 83.71(3) . . ? O1 Ru1 P1 97.56(3) . . ? P2 Ru1 P1 151.269(13) . . ? C1 Ru1 P3 88.51(3) . . ? O2 Ru1 P3 163.00(3) . . ? O1 Ru1 P3 103.76(3) . . ? P2 Ru1 P3 95.908(12) . . ? P1 Ru1 P3 100.655(12) . . ? C1 Ru1 C13 138.16(4) . . ? O2 Ru1 C13 29.74(4) . . ? O1 Ru1 C13 29.53(4) . . ? P2 Ru1 C13 94.90(3) . . ? P1 Ru1 C13 90.66(3) . . ? P3 Ru1 C13 133.28(3) . . ? C7 P1 C9 100.44(7) . . ? C7 P1 C8 103.54(7) . . ? C9 P1 C8 96.29(7) . . ? C7 P1 Ru1 106.97(4) . . ? C9 P1 Ru1 110.47(5) . . ? C8 P1 Ru1 134.28(5) . . ? C10 P2 C11 101.73(8) . . ? C10 P2 C12 100.79(7) . . ? C11 P2 C12 95.01(7) . . ? C10 P2 Ru1 108.63(5) . . ? C11 P2 Ru1 114.75(5) . . ? C12 P2 Ru1 131.65(5) . . ? C15 P3 C27 103.11(6) . . ? C15 P3 C21 97.91(6) . . ? C27 P3 C21 104.59(6) . . ? C15 P3 Ru1 117.00(4) . . ? C27 P3 Ru1 119.71(4) . . ? C21 P3 Ru1 111.71(4) . . ? C13 O1 Ru1 89.72(8) . . ? C13 O2 Ru1 92.38(8) . . ? O1 C13 O2 118.63(12) . . ? O1 C13 C14 121.55(13) . . ? O2 C13 C14 119.82(13) . . ? O1 C13 Ru1 60.75(7) . . ? O2 C13 Ru1 57.88(7) . . ? C14 C13 Ru1 177.70(11) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2 C1 C6 115.14(11) . . ? C2 C1 Ru1 122.50(9) . . ? C6 C1 Ru1 122.36(9) . . ? C3 C2 C1 122.31(13) . . ? C3 C2 C10 118.51(12) . . ? C1 C2 C10 118.98(12) . . ? C4 C3 C2 120.71(13) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 119.04(13) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? C4 C5 C6 120.40(13) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 122.32(12) . . ? C5 C6 C7 118.92(12) . . ? C1 C6 C7 118.72(11) . . ? C6 C7 P1 103.78(9) . . ? C6 C7 H7A 111.0 . . ? P1 C7 H7A 111.0 . . ? C6 C7 H7B 111.0 . . ? P1 C7 H7B 111.0 . . ? H7A C7 H7B 109.0 . . ? F8A C8 F8C 106.39(14) . . ? F8A C8 F8B 107.12(14) . . ? F8C C8 F8B 106.70(13) . . ? F8A C8 P1 110.87(10) . . ? F8C C8 P1 114.86(12) . . ? F8B C8 P1 110.50(11) . . ? F9C C9 F9A 108.34(13) . . ? F9C C9 F9B 106.31(12) . . ? F9A C9 F9B 106.87(11) . . ? F9C C9 P1 111.33(9) . . ? F9A C9 P1 112.33(10) . . ? F9B C9 P1 111.38(11) . . ? C2 C10 P2 106.83(9) . . ? C2 C10 H10A 110.4 . . ? P2 C10 H10A 110.4 . . ? C2 C10 H10B 110.4 . . ? P2 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? F11A C11 F11C 108.55(14) . . ? F11A C11 F11B 106.46(14) . . ? F11C C11 F11B 106.64(14) . . ? F11A C11 P2 110.23(12) . . ? F11C C11 P2 112.23(12) . . ? F11B C11 P2 112.47(12) . . ? F12B C12 F12C 107.17(13) . . ? F12B C12 F12A 107.12(12) . . ? F12C C12 F12A 106.21(12) . . ? F12B C12 P2 112.16(10) . . ? F12C C12 P2 110.09(9) . . ? F12A C12 P2 113.71(11) . . ? C20 C15 C16 118.83(12) . . ? C20 C15 P3 124.86(10) . . ? C16 C15 P3 116.17(10) . . ? C17 C16 C15 120.62(14) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C18 C17 C16 120.21(15) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C19 C18 C17 119.47(14) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? C18 C19 C20 120.85(15) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C15 C20 C19 119.99(14) . . ? C15 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C26 C21 C22 118.46(12) . . ? C26 C21 P3 121.02(9) . . ? C22 C21 P3 120.35(10) . . ? C23 C22 C21 120.62(14) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C24 C23 C22 120.19(14) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C25 C24 C23 119.80(14) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C24 C25 C26 120.14(15) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C21 C26 C25 120.75(13) . . ? C21 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C28 C27 C32 118.70(12) . . ? C28 C27 P3 121.04(10) . . ? C32 C27 P3 120.26(10) . . ? C29 C28 C27 120.43(14) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C30 C29 C28 120.31(14) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 119.97(13) . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C30 C31 C32 120.14(15) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C31 C32 C27 120.42(13) . . ? C31 C32 H32A 119.8 . . ? C27 C32 H32A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 34.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.939 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.076 #END