# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_B _database_code_depnum_ccdc_archive 'CCDC 891251' #TrackingRef 'Gomez.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H25 N O4' _chemical_formula_sum 'C28 H25 N O4' _chemical_formula_weight 439.49 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6933(10) _cell_length_b 10.0519(9) _cell_length_c 19.3915(16) _cell_angle_alpha 90 _cell_angle_beta 101.035(3) _cell_angle_gamma 90 _cell_volume 2237.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 3059 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 24.55 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_absorpt_correction_T_min 0.9828 _exptl_absorpt_correction_T_max 0.9965 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'Bruker Kappa APEX II Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_unetI/netI 0.0553 _diffrn_reflns_number 13083 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.34 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.954 _diffrn_measured_fraction_theta_max 0.954 _reflns_number_total 3902 _reflns_number_gt 2662 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0562P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0154(15) _refine_ls_number_reflns 3902 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1111 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.272 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.071 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.14088(16) 0.9290(2) 0.32398(11) 0.0381(5) Uani 1 1 d . . . H1 H -0.1163 0.9836 0.3641 0.046 Uiso 1 1 calc R . . C2 C -0.24396(17) 0.8562(2) 0.31669(12) 0.0481(6) Uani 1 1 d . . . H2 H -0.2891 0.8601 0.3525 0.058 Uiso 1 1 calc R . . C3 C -0.28092(17) 0.7788(2) 0.25807(12) 0.0506(6) Uani 1 1 d . . . H3 H -0.3514 0.7297 0.2538 0.061 Uiso 1 1 calc R . . C4 C -0.21657(15) 0.7717(2) 0.20529(11) 0.0406(5) Uani 1 1 d . . . H4 H -0.2431 0.7193 0.1646 0.049 Uiso 1 1 calc R . . C5 C -0.04898(15) 1.0571(2) 0.07634(10) 0.0326(5) Uani 1 1 d . . . H5 H -0.0813 1.0063 0.036 0.039 Uiso 1 1 calc R . . C6 C -0.02405(15) 1.1918(2) 0.07004(10) 0.0352(5) Uani 1 1 d . . . H6 H -0.0415 1.2336 0.0253 0.042 Uiso 1 1 calc R . . C7 C 0.02573(14) 1.26427(19) 0.12839(9) 0.0319(5) Uani 1 1 d . . . H7 H 0.0452 1.355 0.1233 0.038 Uiso 1 1 calc R . . C8 C 0.04766(14) 1.20604(18) 0.19451(9) 0.0280(4) Uani 1 1 d . . . H8 H 0.0823 1.2563 0.2346 0.034 Uiso 1 1 calc R . . C9 C 0.03739(14) 0.99733(18) 0.26991(9) 0.0275(4) Uani 1 1 d . . . C10 C -0.03694(14) 0.85162(19) 0.15754(9) 0.0283(4) Uani 1 1 d . . . C11 C -0.11287(14) 0.84207(19) 0.21253(10) 0.0309(5) Uani 1 1 d . . . C12 C -0.02617(13) 0.99870(18) 0.14187(9) 0.0260(4) Uani 1 1 d . . . C13 C 0.01851(13) 1.07402(17) 0.20150(9) 0.0245(4) Uani 1 1 d . . . C14 C -0.07472(14) 0.92058(18) 0.27188(10) 0.0299(5) Uani 1 1 d . . . C15 C 0.13160(14) 0.88827(18) 0.26184(9) 0.0261(4) Uani 1 1 d . . . H15 H 0.1467 0.8283 0.3037 0.031 Uiso 1 1 calc R . . C16 C 0.08986(13) 0.80783(18) 0.19402(9) 0.0270(4) Uani 1 1 d . . . H16 H 0.0916 0.7105 0.2047 0.032 Uiso 1 1 calc R . . C17 C 0.17611(14) 0.84031(19) 0.14763(10) 0.0290(4) Uani 1 1 d . . . C18 C 0.24290(14) 0.95478(18) 0.25116(10) 0.0274(4) Uani 1 1 d . . . C19 C 0.34380(15) 0.99657(19) 0.15045(10) 0.0323(5) Uani 1 1 d . . . C20 C 0.30625(18) 1.0642(2) 0.08833(11) 0.0480(6) Uani 1 1 d . . . H20 H 0.2255 1.0688 0.0684 0.058 Uiso 1 1 calc R . . C21 C 0.3872(2) 1.1253(3) 0.05534(12) 0.0603(7) Uani 1 1 d . . . H21 H 0.3619 1.171 0.0122 0.072 Uiso 1 1 calc R . . C22 C 0.5040(2) 1.1204(2) 0.08440(13) 0.0573(7) Uani 1 1 d . . . H22 H 0.5594 1.1613 0.0612 0.069 Uiso 1 1 calc R . . C23 C 0.53986(18) 1.0559(2) 0.14716(13) 0.0558(7) Uani 1 1 d . . . H23 H 0.6203 1.0545 0.1679 0.067 Uiso 1 1 calc R . . C24 C 0.46025(16) 0.9927(2) 0.18072(11) 0.0431(5) Uani 1 1 d . . . H24 H 0.4857 0.9474 0.2239 0.052 Uiso 1 1 calc R . . C25 C 0.11720(16) 1.0341(2) 0.39435(9) 0.0370(5) Uani 1 1 d . . . H25A H 0.2024 1.0218 0.3995 0.044 Uiso 1 1 calc R . . H25B H 0.0814 0.9469 0.4009 0.044 Uiso 1 1 calc R . . C26 C 0.09108(17) 1.1321(2) 0.44783(10) 0.0457(6) Uani 1 1 d . . . H26A H 0.1266 1.2181 0.4407 0.069 Uiso 1 1 calc R . . H26B H 0.1231 1.0992 0.4952 0.069 Uiso 1 1 calc R . . H26C H 0.0065 1.143 0.4425 0.069 Uiso 1 1 calc R . . C27 C -0.06546(16) 0.64016(19) 0.09581(10) 0.0359(5) Uani 1 1 d . . . H27A H -0.0786 0.6027 0.1408 0.043 Uiso 1 1 calc R . . H27B H 0.015 0.6183 0.0905 0.043 Uiso 1 1 calc R . . C28 C -0.15150(17) 0.5837(2) 0.03584(11) 0.0457(6) Uani 1 1 d . . . H28A H -0.2308 0.6001 0.0435 0.069 Uiso 1 1 calc R . . H28B H -0.1388 0.4876 0.0328 0.069 Uiso 1 1 calc R . . H28C H -0.1413 0.6262 -0.008 0.069 Uiso 1 1 calc R . . N1 N 0.25780(11) 0.93119(15) 0.18304(7) 0.0282(4) Uani 1 1 d . . . O1 O 0.06938(10) 1.08705(12) 0.32590(6) 0.0316(3) Uani 1 1 d . . . O2 O -0.08190(10) 0.78224(12) 0.09484(6) 0.0331(3) Uani 1 1 d . . . O3 O 0.30897(10) 1.02000(13) 0.29409(7) 0.0361(4) Uani 1 1 d . . . O4 O 0.17674(10) 0.79807(14) 0.08933(7) 0.0394(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 C1 0.0368(11) 0.0341(12) 0.0479(13) 0.0032(10) 0.0191(9) 0.0046(9) C2 0.0404(12) 0.0439(14) 0.0683(15) 0.0050(13) 0.0311(11) 0.0010(11) C3 0.0316(11) 0.0399(14) 0.0859(17) 0.0010(14) 0.0256(11) -0.0041(10) C4 0.0290(10) 0.0323(12) 0.0624(13) -0.0026(11) 0.0132(9) -0.0025(9) C5 0.0299(9) 0.0339(12) 0.0331(11) -0.0029(10) 0.0037(8) 0.0027(9) C6 0.0375(10) 0.0332(12) 0.0337(11) 0.0068(10) 0.0043(8) 0.0045(9) C7 0.0337(10) 0.0232(11) 0.0401(11) 0.0030(10) 0.0103(9) 0.0006(8) C8 0.0245(9) 0.0277(11) 0.0325(10) -0.0036(9) 0.0069(8) 0.0019(8) C9 0.0274(9) 0.0256(11) 0.0303(10) -0.0024(9) 0.0077(8) 0.0002(8) C10 0.0247(9) 0.0256(11) 0.0337(10) -0.0043(9) 0.0037(8) -0.0015(8) C11 0.0242(9) 0.0278(11) 0.0414(11) 0.0034(10) 0.0080(8) 0.0028(8) C12 0.0201(8) 0.0255(11) 0.0329(11) 0.0002(9) 0.0064(8) 0.0018(8) C13 0.0200(8) 0.0229(11) 0.0319(10) 0.0007(9) 0.0082(7) 0.0023(8) C14 0.0262(9) 0.0256(11) 0.0402(11) 0.0059(10) 0.0123(8) 0.0029(8) C15 0.0256(9) 0.0225(11) 0.0306(10) 0.0041(9) 0.0062(7) 0.0028(8) C16 0.0255(9) 0.0231(10) 0.0329(10) -0.0001(9) 0.0068(8) 0.0008(8) C17 0.0252(9) 0.0274(11) 0.0334(11) -0.0002(10) 0.0034(8) 0.0050(8) C18 0.0243(9) 0.0238(11) 0.0336(11) 0.0010(9) 0.0043(8) 0.0031(8) C19 0.0308(10) 0.0317(12) 0.0365(11) 0.0022(10) 0.0120(9) -0.0013(8) C20 0.0403(11) 0.0578(16) 0.0456(13) 0.0098(12) 0.0075(10) -0.0012(11) C21 0.0685(16) 0.0647(18) 0.0511(14) 0.0205(14) 0.0201(12) -0.0061(13) C22 0.0587(15) 0.0543(16) 0.0660(16) 0.0112(14) 0.0296(12) -0.0111(12) C23 0.0348(11) 0.0567(16) 0.0794(17) 0.0150(15) 0.0197(11) -0.0077(11) C24 0.0318(11) 0.0425(13) 0.0552(13) 0.0144(11) 0.0085(10) -0.0024(9) C25 0.0428(11) 0.0401(13) 0.0279(11) 0.0051(10) 0.0061(9) 0.0026(10) C26 0.0525(13) 0.0521(15) 0.0345(11) -0.0030(11) 0.0133(10) 0.0005(11) C27 0.0380(10) 0.0228(11) 0.0458(12) -0.0036(10) 0.0054(9) -0.0014(9) C28 0.0483(12) 0.0347(13) 0.0510(13) -0.0066(11) 0.0017(10) -0.0086(10) N1 0.0229(7) 0.0311(9) 0.0314(9) 0.0000(8) 0.0070(7) -0.0021(7) O1 0.0384(7) 0.0288(8) 0.0277(7) -0.0023(6) 0.0068(6) 0.0005(6) O2 0.0314(7) 0.0263(8) 0.0391(8) -0.0036(7) 0.0008(6) -0.0026(6) O3 0.0332(7) 0.0351(8) 0.0394(8) -0.0052(7) 0.0052(6) -0.0052(6) O4 0.0340(7) 0.0488(9) 0.0363(8) -0.0073(8) 0.0087(6) 0.0000(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C14 1.388(3) . ? C1 C2 1.394(3) . ? C1 H1 0.95 . ? C2 C3 1.377(3) . ? C2 H2 0.95 . ? C3 C4 1.383(3) . ? C3 H3 0.95 . ? C4 C11 1.387(3) . ? C4 H4 0.95 . ? C5 C12 1.379(2) . ? C5 C6 1.395(3) . ? C5 H5 0.95 . ? C6 C7 1.378(2) . ? C6 H6 0.95 . ? C7 C8 1.388(2) . ? C7 H7 0.95 . ? C8 C13 1.383(2) . ? C8 H8 0.95 . ? C9 O1 1.406(2) . ? C9 C13 1.513(2) . ? C9 C14 1.528(2) . ? C9 C15 1.583(2) . ? C10 O2 1.413(2) . ? C10 C11 1.516(2) . ? C10 C12 1.519(3) . ? C10 C16 1.578(2) . ? C11 C14 1.396(3) . ? C12 C13 1.397(2) . ? C15 C18 1.512(2) . ? C15 C16 1.541(2) . ? C15 H15 1 . ? C16 C17 1.510(2) . ? C16 H16 1 . ? C17 O4 1.209(2) . ? C17 N1 1.403(2) . ? C18 O3 1.214(2) . ? C18 N1 1.386(2) . ? C19 C24 1.376(3) . ? C19 C20 1.380(3) . ? C19 N1 1.444(2) . ? C20 C21 1.384(3) . ? C20 H20 0.95 . ? C21 C22 1.375(3) . ? C21 H21 0.95 . ? C22 C23 1.372(3) . ? C22 H22 0.95 . ? C23 C24 1.388(3) . ? C23 H23 0.95 . ? C24 H24 0.95 . ? C25 O1 1.440(2) . ? C25 C26 1.503(3) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 O2 1.441(2) . ? C27 C28 1.496(3) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? 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 C1 C2 119.1(2) . . ? C14 C1 H1 120.5 . . ? C2 C1 H1 120.5 . . ? C3 C2 C1 120.59(18) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 120.69(18) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C11 119.2(2) . . ? C3 C4 H4 120.4 . . ? C11 C4 H4 120.4 . . ? C12 C5 C6 119.17(18) . . ? C12 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C7 C6 C5 120.26(17) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.65(17) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C13 C8 C7 119.32(17) . . ? C13 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? O1 C9 C13 108.83(14) . . ? O1 C9 C14 114.04(13) . . ? C13 C9 C14 107.29(14) . . ? O1 C9 C15 115.68(13) . . ? C13 C9 C15 104.69(13) . . ? C14 C9 C15 105.63(14) . . ? O2 C10 C11 113.74(14) . . ? O2 C10 C12 109.85(14) . . ? C11 C10 C12 106.53(15) . . ? O2 C10 C16 114.26(14) . . ? C11 C10 C16 107.07(14) . . ? C12 C10 C16 104.73(13) . . ? C4 C11 C14 120.45(17) . . ? C4 C11 C10 125.40(17) . . ? C14 C11 C10 113.97(15) . . ? C5 C12 C13 120.51(17) . . ? C5 C12 C10 126.16(17) . . ? C13 C12 C10 113.20(15) . . ? C8 C13 C12 119.92(16) . . ? C8 C13 C9 125.26(16) . . ? C12 C13 C9 114.72(15) . . ? C1 C14 C11 119.98(16) . . ? C1 C14 C9 126.02(17) . . ? C11 C14 C9 113.90(15) . . ? C18 C15 C16 104.80(13) . . ? C18 C15 C9 109.93(15) . . ? C16 C15 C9 109.57(13) . . ? C18 C15 H15 110.8 . . ? C16 C15 H15 110.8 . . ? C9 C15 H15 110.8 . . ? C17 C16 C15 104.85(14) . . ? C17 C16 C10 110.49(14) . . ? C15 C16 C10 110.67(13) . . ? C17 C16 H16 110.2 . . ? C15 C16 H16 110.2 . . ? C10 C16 H16 110.2 . . ? O4 C17 N1 124.12(16) . . ? O4 C17 C16 127.26(17) . . ? N1 C17 C16 108.61(15) . . ? O3 C18 N1 124.52(16) . . ? O3 C18 C15 126.60(16) . . ? N1 C18 C15 108.87(15) . . ? C24 C19 C20 120.65(17) . . ? C24 C19 N1 121.04(17) . . ? C20 C19 N1 118.32(15) . . ? C19 C20 C21 119.39(19) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C22 C21 C20 120.6(2) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C23 C22 C21 119.4(2) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 120.9(2) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C19 C24 C23 119.01(19) . . ? C19 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? O1 C25 C26 107.44(15) . . ? O1 C25 H25A 110.2 . . ? C26 C25 H25A 110.2 . . ? O1 C25 H25B 110.2 . . ? C26 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C27 C28 107.34(16) . . ? O2 C27 H27A 110.2 . . ? C28 C27 H27A 110.2 . . ? O2 C27 H27B 110.2 . . ? C28 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C18 N1 C17 112.33(14) . . ? C18 N1 C19 124.36(15) . . ? C17 N1 C19 123.25(14) . . ? C9 O1 C25 118.29(14) . . ? C10 O2 C27 116.83(14) . . ? data_C _database_code_depnum_ccdc_archive 'CCDC 901523' #TrackingRef 'Gomez.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H21 N' _chemical_formula_weight 323.42 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.4935(10) _cell_length_b 9.1390(16) _cell_length_c 14.860(3) _cell_angle_alpha 90.294(7) _cell_angle_beta 97.462(6) _cell_angle_gamma 105.779(6) _cell_volume 840.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4141 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 29.44 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9504 _exptl_absorpt_correction_T_max 0.9985 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 kappa APEX-II CCD Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15378 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4138 _reflns_number_gt 2949 _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^)+(0.0462P)^2^+0.2667P] 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 4138 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1220 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 N1 N 0.5486(2) 0.44658(16) 0.27303(9) 0.0374(3) Uani 1 1 d . . . C1 C 0.5984(2) 0.83999(17) -0.04264(10) 0.0323(3) Uani 1 1 d . . . H1 H 0.4716 0.8738 -0.0462 0.039 Uiso 1 1 calc R . . C2 C 0.7103(3) 0.84933(19) -0.11711(11) 0.0407(4) Uani 1 1 d . . . H2 H 0.6595 0.8898 -0.1717 0.049 Uiso 1 1 calc R . . C3 C 0.8939(3) 0.8004(2) -0.11241(11) 0.0423(4) Uani 1 1 d . . . H3 H 0.9699 0.8083 -0.1635 0.051 Uiso 1 1 calc R . . C4 C 0.9686(2) 0.73963(18) -0.03343(11) 0.0352(4) Uani 1 1 d . . . H4 H 1.0944 0.7048 -0.0306 0.042 Uiso 1 1 calc R . . C5 C 1.1074(2) 0.84481(17) 0.27068(10) 0.0297(3) Uani 1 1 d . . . H5 H 1.2311 0.8075 0.2744 0.036 Uiso 1 1 calc R . . C6 C 1.1007(2) 0.95811(18) 0.33173(10) 0.0335(3) Uani 1 1 d . . . H6 H 1.2212 1.0000 0.3766 0.040 Uiso 1 1 calc R . . C7 C 0.9193(2) 1.01009(17) 0.32745(10) 0.0322(3) Uani 1 1 d . . . H7 H 0.9154 1.0874 0.3697 0.039 Uiso 1 1 calc R . . C8 C 0.7422(2) 0.95053(16) 0.26195(10) 0.0282(3) Uani 1 1 d . . . H8 H 0.6171 0.9859 0.2597 0.034 Uiso 1 1 calc R . . C9 C 0.5738(2) 0.76175(16) 0.12431(9) 0.0244(3) Uani 1 1 d . . . H9 H 0.4457 0.8033 0.1210 0.029 Uiso 1 1 calc R . . C10 C 0.9158(2) 0.66616(16) 0.13167(10) 0.0261(3) Uani 1 1 d . . . H10 H 1.0517 0.6339 0.1340 0.031 Uiso 1 1 calc R . . C11 C 0.8587(2) 0.72999(16) 0.04131(10) 0.0272(3) Uani 1 1 d . . . C12 C 0.9335(2) 0.78647(16) 0.20443(10) 0.0252(3) Uani 1 1 d . . . C13 C 0.7495(2) 0.83940(15) 0.20004(9) 0.0240(3) Uani 1 1 d . . . C14 C 0.6732(2) 0.78104(16) 0.03674(10) 0.0263(3) Uani 1 1 d . . . C15 C 0.5133(2) 0.58809(16) 0.14150(10) 0.0249(3) Uani 1 1 d . . . H15 H 0.4027 0.5328 0.0907 0.030 Uiso 1 1 calc R . . C16 C 0.7186(2) 0.53056(16) 0.14396(10) 0.0262(3) Uani 1 1 d . . . H16 H 0.6954 0.4538 0.0928 0.031 Uiso 1 1 calc R . . C17 C 0.7415(2) 0.45247(17) 0.23366(11) 0.0311(3) Uani 1 1 d . . . H17A H 0.7547 0.3486 0.2231 0.037 Uiso 1 1 calc R . . H17B H 0.8709 0.5113 0.2743 0.037 Uiso 1 1 calc R . . C18 C 0.4281(2) 0.54550(17) 0.23183(10) 0.0277(3) Uani 1 1 d . . . H18A H 0.4509 0.6377 0.2713 0.033 Uiso 1 1 calc R . . H18B H 0.2717 0.4925 0.2214 0.033 Uiso 1 1 calc R . . C19 C 0.5098(2) 0.37938(17) 0.35419(10) 0.0317(3) Uani 1 1 d . . . C20 C 0.6499(3) 0.3012(2) 0.39758(11) 0.0407(4) Uani 1 1 d . . . H20 H 0.7750 0.2974 0.3718 0.049 Uiso 1 1 calc R . . C21 C 0.6081(3) 0.2296(2) 0.47740(12) 0.0500(5) Uani 1 1 d . . . H21 H 0.7042 0.1762 0.5056 0.060 Uiso 1 1 calc R . . C22 C 0.4300(3) 0.2344(2) 0.51672(12) 0.0498(5) Uani 1 1 d . . . H22 H 0.4018 0.1839 0.5714 0.060 Uiso 1 1 calc R . . C23 C 0.2926(3) 0.3135(2) 0.47577(11) 0.0439(4) Uani 1 1 d . . . H23 H 0.1704 0.3189 0.5032 0.053 Uiso 1 1 calc R . . C24 C 0.3300(2) 0.38525(19) 0.39531(11) 0.0358(4) Uani 1 1 d . . . H24 H 0.2332 0.4387 0.3679 0.043 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 N1 0.0372(7) 0.0483(9) 0.0366(8) 0.0176(6) 0.0138(6) 0.0241(6) C1 0.0333(7) 0.0260(8) 0.0329(8) 0.0042(6) 0.0013(6) 0.0018(6) C2 0.0483(9) 0.0351(9) 0.0316(9) 0.0087(7) 0.0043(7) -0.0002(7) C3 0.0481(9) 0.0399(10) 0.0335(9) 0.0035(7) 0.0171(7) -0.0027(7) C4 0.0312(7) 0.0343(9) 0.0378(9) -0.0013(7) 0.0121(6) 0.0017(6) C5 0.0241(6) 0.0305(8) 0.0338(8) 0.0038(6) 0.0016(6) 0.0073(6) C6 0.0318(7) 0.0326(9) 0.0303(8) 0.0003(7) -0.0035(6) 0.0026(6) C7 0.0396(8) 0.0263(8) 0.0289(8) -0.0012(6) 0.0046(6) 0.0062(6) C8 0.0290(7) 0.0253(8) 0.0319(8) 0.0049(6) 0.0078(6) 0.0085(6) C9 0.0208(6) 0.0244(7) 0.0287(8) 0.0033(6) 0.0034(5) 0.0072(5) C10 0.0212(6) 0.0278(8) 0.0314(8) 0.0014(6) 0.0063(5) 0.0089(5) C11 0.0245(6) 0.0247(7) 0.0294(8) -0.0011(6) 0.0055(5) 0.0008(5) C12 0.0235(6) 0.0246(7) 0.0275(7) 0.0051(6) 0.0052(5) 0.0056(5) C13 0.0228(6) 0.0224(7) 0.0268(7) 0.0052(6) 0.0052(5) 0.0053(5) C14 0.0252(6) 0.0218(7) 0.0281(8) 0.0003(6) 0.0025(5) 0.0006(5) C15 0.0206(6) 0.0254(7) 0.0279(7) 0.0020(6) 0.0029(5) 0.0053(5) C16 0.0254(6) 0.0226(7) 0.0317(8) 0.0000(6) 0.0061(6) 0.0077(5) C17 0.0291(7) 0.0290(8) 0.0399(9) 0.0078(7) 0.0085(6) 0.0139(6) C18 0.0231(6) 0.0283(8) 0.0334(8) 0.0066(6) 0.0060(6) 0.0087(5) C19 0.0362(8) 0.0279(8) 0.0302(8) 0.0040(6) 0.0060(6) 0.0068(6) C20 0.0473(9) 0.0375(9) 0.0396(10) 0.0103(7) 0.0058(7) 0.0155(7) C21 0.0648(12) 0.0426(11) 0.0403(10) 0.0144(8) 0.0011(9) 0.0138(9) C22 0.0663(12) 0.0410(10) 0.0307(9) 0.0075(8) 0.0040(8) -0.0032(9) C23 0.0471(9) 0.0420(10) 0.0329(9) -0.0037(8) 0.0105(7) -0.0064(8) C24 0.0352(8) 0.0365(9) 0.0319(9) 0.0005(7) 0.0052(6) 0.0033(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 N1 C19 1.378(2) . ? N1 C17 1.4379(18) . ? N1 C18 1.4390(18) . ? C1 C14 1.385(2) . ? C1 C2 1.391(2) . ? C2 C3 1.377(2) . ? C3 C4 1.388(2) . ? C4 C11 1.387(2) . ? C5 C12 1.381(2) . ? C5 C6 1.386(2) . ? C6 C7 1.379(2) . ? C7 C8 1.389(2) . ? C8 C13 1.381(2) . ? C9 C13 1.5131(19) . ? C9 C14 1.5165(19) . ? C9 C15 1.5587(19) . ? C10 C11 1.509(2) . ? C10 C12 1.509(2) . ? C10 C16 1.5520(19) . ? C11 C14 1.3988(19) . ? C12 C13 1.3995(18) . ? C15 C18 1.530(2) . ? C15 C16 1.5566(18) . ? C16 C17 1.525(2) . ? C19 C24 1.399(2) . ? C19 C20 1.400(2) . ? C20 C21 1.380(2) . ? C21 C22 1.372(3) . ? C22 C23 1.380(3) . ? C23 C24 1.384(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 C19 N1 C17 122.31(12) . . ? C19 N1 C18 122.67(12) . . ? C17 N1 C18 113.55(12) . . ? C14 C1 C2 119.47(15) . . ? C3 C2 C1 120.55(15) . . ? C2 C3 C4 120.31(15) . . ? C11 C4 C3 119.66(15) . . ? C12 C5 C6 119.70(13) . . ? C7 C6 C5 120.12(14) . . ? C6 C7 C8 120.61(14) . . ? C13 C8 C7 119.48(13) . . ? C13 C9 C14 107.23(11) . . ? C13 C9 C15 107.04(11) . . ? C14 C9 C15 106.39(11) . . ? C11 C10 C12 107.47(11) . . ? C11 C10 C16 105.82(11) . . ? C12 C10 C16 107.58(11) . . ? C4 C11 C14 119.98(14) . . ? C4 C11 C10 126.62(13) . . ? C14 C11 C10 113.40(12) . . ? C5 C12 C13 120.15(13) . . ? C5 C12 C10 126.64(12) . . ? C13 C12 C10 113.21(12) . . ? C8 C13 C12 119.92(13) . . ? C8 C13 C9 126.98(12) . . ? C12 C13 C9 113.10(12) . . ? C1 C14 C11 120.02(13) . . ? C1 C14 C9 127.08(13) . . ? C11 C14 C9 112.90(12) . . ? C18 C15 C16 105.81(11) . . ? C18 C15 C9 114.68(11) . . ? C16 C15 C9 109.20(10) . . ? C17 C16 C10 114.11(12) . . ? C17 C16 C15 106.49(11) . . ? C10 C16 C15 109.52(11) . . ? N1 C17 C16 105.87(11) . . ? N1 C18 C15 105.87(11) . . ? N1 C19 C24 121.64(14) . . ? N1 C19 C20 120.37(14) . . ? C24 C19 C20 117.99(15) . . ? C21 C20 C19 120.60(16) . . ? C22 C21 C20 121.04(17) . . ? C21 C22 C23 119.08(16) . . ? C22 C23 C24 120.98(16) . . ? C23 C24 C19 120.29(16) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.226 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.041 data_C1 _database_code_depnum_ccdc_archive 'CCDC 901524' #TrackingRef 'Gomez.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H26 N Ru, F6 P' _chemical_formula_sum 'C29 H26 F6 N P Ru' _chemical_formula_weight 634.55 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.842(2) _cell_length_b 16.472(4) _cell_length_c 15.600(3) _cell_angle_alpha 90 _cell_angle_beta 98.429(10) _cell_angle_gamma 90 _cell_volume 2501.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9488 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 29.78 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_absorpt_correction_T_min 0.8886 _exptl_absorpt_correction_T_max 0.9420 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'Bruker Kappa APEX II Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_unetI/netI 0.0164 _diffrn_reflns_number 38212 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 4558 _reflns_number_gt 4140 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0789P)^2^+4.8283P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4558 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1421 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.245 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.249 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.4153(5) -0.0638(3) 0.2782(3) 0.0452(11) Uani 1 1 d . . . H1 H 1.4291 -0.1009 0.3253 0.054 Uiso 1 1 calc R . . C2 C 1.5227(5) -0.0462(3) 0.2309(4) 0.0556(13) Uani 1 1 d . . . H2 H 1.6091 -0.0724 0.2452 0.067 Uiso 1 1 calc R . . C3 C 1.5031(5) 0.0093(3) 0.1631(4) 0.0546(13) Uani 1 1 d . . . H3 H 1.5763 0.0211 0.1316 0.066 Uiso 1 1 calc R . . C4 C 1.3794(5) 0.0470(3) 0.1416(3) 0.0464(11) Uani 1 1 d . . . H4 H 1.3671 0.0856 0.0959 0.056 Uiso 1 1 calc R . . C5 C 0.9181(4) -0.0148(3) 0.0958(3) 0.0419(10) Uani 1 1 d . . . H5 H 0.9034 0.023 0.0494 0.05 Uiso 1 1 calc R . . C6 C 0.8304(5) -0.0814(4) 0.0971(3) 0.0504(12) Uani 1 1 d . . . H6 H 0.7571 -0.0893 0.0509 0.061 Uiso 1 1 calc R . . C7 C 0.8496(5) -0.1353(3) 0.1647(3) 0.0479(12) Uani 1 1 d . . . H7 H 0.7892 -0.1802 0.1652 0.057 Uiso 1 1 calc R . . C8 C 0.9566(4) -0.1250(3) 0.2324(3) 0.0386(9) Uani 1 1 d . . . H8 H 0.9686 -0.162 0.2795 0.046 Uiso 1 1 calc R . . C9 C 1.1636(4) -0.0375(2) 0.2995(3) 0.0327(8) Uani 1 1 d . . . H9 H 1.1782 -0.0791 0.3467 0.039 Uiso 1 1 calc R . . C10 C 1.1284(4) 0.0650(2) 0.1720(3) 0.0356(9) Uani 1 1 d . . . H10 H 1.1158 0.1023 0.1209 0.043 Uiso 1 1 calc R . . C11 C 1.2704(4) 0.0287(2) 0.1871(3) 0.0364(9) Uani 1 1 d . . . C12 C 1.0253(4) -0.0041(3) 0.1615(3) 0.0344(9) Uani 1 1 d . . . C13 C 1.0461(4) -0.0597(2) 0.2306(3) 0.0314(8) Uani 1 1 d . . . C14 C 1.2905(4) -0.0267(3) 0.2558(3) 0.0372(9) Uani 1 1 d . . . C15 C 1.1304(4) 0.0479(2) 0.3349(3) 0.0332(8) Uani 1 1 d . . . H15 H 1.2075 0.0656 0.3801 0.04 Uiso 1 1 calc R . . C16 C 1.1131(4) 0.1103(2) 0.2576(3) 0.0361(9) Uani 1 1 d . . . H16 H 1.185 0.1534 0.2688 0.043 Uiso 1 1 calc R . . C17 C 0.9711(5) 0.1481(3) 0.2572(3) 0.0415(10) Uani 1 1 d . . . H17A H 0.9793 0.2032 0.2827 0.05 Uiso 1 1 calc R . . H17B H 0.9219 0.1519 0.1972 0.05 Uiso 1 1 calc R . . C18 C 0.9950(4) 0.0497(2) 0.3728(3) 0.0346(9) Uani 1 1 d . . . H18A H 0.9618 -0.0061 0.3808 0.042 Uiso 1 1 calc R . . H18B H 1.0074 0.0779 0.4295 0.042 Uiso 1 1 calc R . . C19 C 0.7715(4) 0.1138(3) 0.3266(3) 0.0362(9) Uani 1 1 d . . . C20 C 0.6928(5) 0.1781(3) 0.2800(3) 0.0454(10) Uani 1 1 d . . . H20 H 0.733 0.2097 0.2393 0.054 Uiso 1 1 calc R . . C21 C 0.5572(5) 0.1947(4) 0.2940(3) 0.0549(13) Uani 1 1 d . . . H21 H 0.5041 0.234 0.2594 0.066 Uiso 1 1 calc R . . C22 C 0.5004(5) 0.1531(3) 0.3591(4) 0.0538(13) Uani 1 1 d . . . H22 H 0.4086 0.164 0.3677 0.065 Uiso 1 1 calc R . . C23 C 0.5792(5) 0.0951(3) 0.4118(4) 0.0505(12) Uani 1 1 d . . . H23 H 0.5416 0.0683 0.4569 0.061 Uiso 1 1 calc R . . C24 C 0.7152(5) 0.0773(3) 0.3967(3) 0.0411(10) Uani 1 1 d . . . H24 H 0.7696 0.0404 0.4339 0.049 Uiso 1 1 calc R . . C25 C 0.8597(5) 0.2937(3) 0.4658(4) 0.0507(12) Uani 1 1 d . . . H25 H 0.9435 0.2966 0.4425 0.061 Uiso 1 1 calc R . . C26 C 0.7388(6) 0.3393(3) 0.4380(4) 0.0548(13) Uani 1 1 d . . . H26 H 0.7271 0.3784 0.3927 0.066 Uiso 1 1 calc R . . C27 C 0.6395(6) 0.3163(3) 0.4897(4) 0.0617(15) Uani 1 1 d . . . H27 H 0.5489 0.3373 0.4854 0.074 Uiso 1 1 calc R . . C28 C 0.6974(6) 0.2569(4) 0.5487(3) 0.0631(16) Uani 1 1 d . . . H28 H 0.6525 0.2305 0.5909 0.076 Uiso 1 1 calc R . . C29 C 0.8325(5) 0.2433(3) 0.5344(3) 0.0527(12) Uani 1 1 d . . . H29 H 0.8954 0.2063 0.5656 0.063 Uiso 1 1 calc R . . N1 N 0.8977(3) 0.0940(2) 0.3095(2) 0.0350(7) Uani 1 1 d . . . F1 F 0.1565(4) 0.2379(2) 0.0836(3) 0.0916(13) Uani 1 1 d . . . F2 F 0.1536(4) 0.3723(2) 0.0742(3) 0.0845(12) Uani 1 1 d . . . F3 F 0.3616(4) 0.3728(3) 0.0371(3) 0.0976(14) Uani 1 1 d . . . F4 F 0.3641(6) 0.2354(3) 0.0436(4) 0.131(2) Uani 1 1 d . . . F5 F 0.1960(5) 0.3000(2) -0.0389(2) 0.0802(12) Uani 1 1 d . . . F6 F 0.3203(5) 0.3073(3) 0.1603(3) 0.1054(15) Uani 1 1 d . . . P1 P 0.26041(12) 0.30397(7) 0.06125(8) 0.0398(3) Uani 1 1 d . . . Ru1 Ru 0.69284(3) 0.21075(2) 0.41808(2) 0.03254(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(2) 0.040(2) 0.054(3) -0.007(2) -0.004(2) 0.0067(19) C2 0.032(2) 0.059(3) 0.073(3) -0.018(3) 0.002(2) 0.008(2) C3 0.040(3) 0.052(3) 0.075(4) -0.015(3) 0.020(2) -0.006(2) C4 0.046(3) 0.043(3) 0.053(3) -0.005(2) 0.015(2) -0.005(2) C5 0.041(2) 0.055(3) 0.030(2) -0.0016(19) 0.0086(17) 0.010(2) C6 0.033(2) 0.074(4) 0.043(3) -0.023(2) 0.0034(19) -0.002(2) C7 0.039(2) 0.048(3) 0.060(3) -0.022(2) 0.017(2) -0.012(2) C8 0.044(2) 0.029(2) 0.045(2) -0.0091(18) 0.0127(19) -0.0031(18) C9 0.038(2) 0.0261(19) 0.033(2) 0.0008(16) 0.0023(16) 0.0023(16) C10 0.042(2) 0.030(2) 0.036(2) 0.0061(17) 0.0106(17) 0.0013(17) C11 0.035(2) 0.030(2) 0.046(2) -0.0042(17) 0.0090(18) -0.0011(16) C12 0.035(2) 0.037(2) 0.032(2) -0.0009(17) 0.0084(16) 0.0066(17) C13 0.036(2) 0.0254(19) 0.034(2) -0.0035(15) 0.0068(16) 0.0020(16) C14 0.037(2) 0.031(2) 0.042(2) -0.0106(17) 0.0032(18) -0.0014(17) C15 0.034(2) 0.029(2) 0.035(2) -0.0045(16) 0.0025(16) -0.0021(16) C16 0.039(2) 0.025(2) 0.046(2) 0.0019(17) 0.0115(18) -0.0025(16) C17 0.053(3) 0.027(2) 0.047(2) 0.0044(18) 0.016(2) 0.0064(19) C18 0.039(2) 0.030(2) 0.034(2) 0.0009(16) 0.0058(17) 0.0005(17) C19 0.036(2) 0.034(2) 0.038(2) -0.0080(17) 0.0040(17) -0.0035(17) C20 0.044(2) 0.055(3) 0.035(2) -0.001(2) 0.0003(19) 0.009(2) C21 0.041(3) 0.074(4) 0.044(3) -0.011(2) -0.013(2) 0.013(2) C22 0.028(2) 0.066(3) 0.066(3) -0.022(3) 0.001(2) -0.006(2) C23 0.041(2) 0.041(3) 0.072(3) -0.017(2) 0.018(2) -0.017(2) C24 0.045(2) 0.029(2) 0.050(2) -0.0038(19) 0.009(2) -0.0045(18) C25 0.045(3) 0.054(3) 0.054(3) -0.011(2) 0.011(2) -0.020(2) C26 0.070(3) 0.031(2) 0.058(3) 0.005(2) -0.006(3) -0.009(2) C27 0.048(3) 0.048(3) 0.089(4) -0.029(3) 0.010(3) 0.003(2) C28 0.079(4) 0.069(4) 0.045(3) -0.022(3) 0.022(3) -0.033(3) C29 0.056(3) 0.048(3) 0.048(3) -0.005(2) -0.013(2) -0.009(2) N1 0.0372(18) 0.0309(17) 0.0377(18) 0.0020(14) 0.0078(14) 0.0024(14) F1 0.085(3) 0.072(2) 0.116(3) 0.040(2) 0.006(2) -0.028(2) F2 0.105(3) 0.070(2) 0.086(3) 0.0073(19) 0.039(2) 0.041(2) F3 0.084(3) 0.107(3) 0.105(3) 0.001(2) 0.027(2) -0.053(2) F4 0.118(4) 0.104(4) 0.183(6) 0.023(4) 0.062(4) 0.066(3) F5 0.130(3) 0.054(2) 0.051(2) -0.0066(15) -0.004(2) -0.0140(19) F6 0.110(4) 0.132(4) 0.061(2) 0.011(2) -0.031(2) -0.011(3) P1 0.0348(6) 0.0371(6) 0.0473(7) 0.0036(5) 0.0049(5) 0.0014(5) Ru1 0.0299(2) 0.0324(2) 0.0348(2) 0.00025(12) 0.00298(14) -0.00104(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C14 1.371(6) . ? C1 C2 1.406(7) . ? C1 H1 0.95 . ? C2 C3 1.390(8) . ? C2 H2 0.95 . ? C3 C4 1.364(7) . ? C3 H3 0.95 . ? C4 C11 1.403(6) . ? C4 H4 0.95 . ? C5 C12 1.370(6) . ? C5 C6 1.398(7) . ? C5 H5 0.95 . ? C6 C7 1.371(8) . ? C6 H6 0.95 . ? C7 C8 1.388(7) . ? C7 H7 0.95 . ? C8 C13 1.393(6) . ? C8 H8 0.95 . ? C9 C13 1.505(6) . ? C9 C14 1.519(6) . ? C9 C15 1.563(5) . ? C9 H9 1 . ? C10 C11 1.507(6) . ? C10 C12 1.518(6) . ? C10 C16 1.557(6) . ? C10 H10 1 . ? C11 C14 1.399(6) . ? C12 C13 1.406(6) . ? C15 C18 1.535(6) . ? C15 C16 1.574(6) . ? C15 H15 1 . ? C16 C17 1.528(6) . ? C16 H16 1 . ? C17 N1 1.468(5) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 N1 1.465(5) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 N1 1.349(5) . ? C19 C24 1.429(6) . ? C19 C20 1.444(6) . ? C19 Ru1 2.347(4) . ? C20 C21 1.410(7) . ? C20 Ru1 2.221(5) . ? C20 H20 0.95 . ? C21 C22 1.407(8) . ? C21 Ru1 2.200(5) . ? C21 H21 0.95 . ? C22 C23 1.414(8) . ? C22 Ru1 2.196(4) . ? C22 H22 0.95 . ? C23 C24 1.424(6) . ? C23 Ru1 2.204(4) . ? C23 H23 0.95 . ? C24 Ru1 2.239(4) . ? C24 H24 0.95 . ? C25 C29 1.410(8) . ? C25 C26 1.421(8) . ? C25 Ru1 2.181(5) . ? C25 H25 0.95 . ? C26 C27 1.407(8) . ? C26 Ru1 2.179(5) . ? C26 H26 0.95 . ? C27 C28 1.406(9) . ? C27 Ru1 2.172(5) . ? C27 H27 0.95 . ? C28 C29 1.399(8) . ? C28 Ru1 2.169(5) . ? C28 H28 0.95 . ? C29 Ru1 2.176(5) . ? C29 H29 0.95 . ? F1 P1 1.567(4) . ? F2 P1 1.573(3) . ? F3 P1 1.591(4) . ? F4 P1 1.573(4) . ? F5 P1 1.598(4) . ? F6 P1 1.573(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 C14 C1 C2 119.2(5) . . ? C14 C1 H1 120.4 . . ? C2 C1 H1 120.4 . . ? C3 C2 C1 120.2(5) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.4(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C11 120.0(5) . . ? C3 C4 H4 120 . . ? C11 C4 H4 120 . . ? C12 C5 C6 120.0(4) . . ? C12 C5 H5 120 . . ? C6 C5 H5 120 . . ? C7 C6 C5 120.2(4) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.6(4) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C7 C8 C13 119.4(4) . . ? C7 C8 H8 120.3 . . ? C13 C8 H8 120.3 . . ? C13 C9 C14 107.7(3) . . ? C13 C9 C15 107.0(3) . . ? C14 C9 C15 106.4(3) . . ? C13 C9 H9 111.8 . . ? C14 C9 H9 111.8 . . ? C15 C9 H9 111.8 . . ? C11 C10 C12 108.1(3) . . ? C11 C10 C16 105.1(3) . . ? C12 C10 C16 107.7(3) . . ? C11 C10 H10 111.9 . . ? C12 C10 H10 111.9 . . ? C16 C10 H10 111.9 . . ? C14 C11 C4 119.6(4) . . ? C14 C11 C10 113.7(4) . . ? C4 C11 C10 126.6(4) . . ? C5 C12 C13 120.0(4) . . ? C5 C12 C10 127.3(4) . . ? C13 C12 C10 112.7(4) . . ? C8 C13 C12 119.7(4) . . ? C8 C13 C9 126.5(4) . . ? C12 C13 C9 113.6(3) . . ? C1 C14 C11 120.5(4) . . ? C1 C14 C9 126.7(4) . . ? C11 C14 C9 112.8(4) . . ? C18 C15 C9 113.1(3) . . ? C18 C15 C16 106.2(3) . . ? C9 C15 C16 108.7(3) . . ? C18 C15 H15 109.6 . . ? C9 C15 H15 109.6 . . ? C16 C15 H15 109.6 . . ? C17 C16 C10 113.2(4) . . ? C17 C16 C15 105.4(3) . . ? C10 C16 C15 109.3(3) . . ? C17 C16 H16 109.6 . . ? C10 C16 H16 109.6 . . ? C15 C16 H16 109.6 . . ? N1 C17 C16 105.9(3) . . ? N1 C17 H17A 110.5 . . ? C16 C17 H17A 110.5 . . ? N1 C17 H17B 110.5 . . ? C16 C17 H17B 110.5 . . ? H17A C17 H17B 108.7 . . ? N1 C18 C15 105.6(3) . . ? N1 C18 H18A 110.6 . . ? C15 C18 H18A 110.6 . . ? N1 C18 H18B 110.6 . . ? C15 C18 H18B 110.6 . . ? H18A C18 H18B 108.8 . . ? N1 C19 C24 121.4(4) . . ? N1 C19 C20 121.3(4) . . ? C24 C19 C20 117.0(4) . . ? N1 C19 Ru1 132.9(3) . . ? C24 C19 Ru1 67.8(2) . . ? C20 C19 Ru1 66.9(2) . . ? C21 C20 C19 120.9(5) . . ? C21 C20 Ru1 70.6(3) . . ? C19 C20 Ru1 76.4(2) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? Ru1 C20 H20 125.1 . . ? C22 C21 C20 120.2(5) . . ? C22 C21 Ru1 71.2(3) . . ? C20 C21 Ru1 72.2(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? Ru1 C21 H21 129.1 . . ? C21 C22 C23 120.4(4) . . ? C21 C22 Ru1 71.5(3) . . ? C23 C22 Ru1 71.5(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? Ru1 C22 H22 129.7 . . ? C22 C23 C24 119.4(5) . . ? C22 C23 Ru1 71.0(3) . . ? C24 C23 Ru1 72.6(2) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? Ru1 C23 H23 128.2 . . ? C23 C24 C19 121.3(4) . . ? C23 C24 Ru1 70.0(3) . . ? C19 C24 Ru1 76.0(2) . . ? C23 C24 H24 119.3 . . ? C19 C24 H24 119.3 . . ? Ru1 C24 H24 126.6 . . ? C29 C25 C26 107.5(5) . . ? C29 C25 Ru1 70.9(3) . . ? C26 C25 Ru1 70.9(3) . . ? C29 C25 H25 126.3 . . ? C26 C25 H25 126.3 . . ? Ru1 C25 H25 123.6 . . ? C27 C26 C25 107.6(5) . . ? C27 C26 Ru1 70.9(3) . . ? C25 C26 Ru1 71.1(3) . . ? C27 C26 H26 126.2 . . ? C25 C26 H26 126.2 . . ? Ru1 C26 H26 123.5 . . ? C28 C27 C26 108.3(5) . . ? C28 C27 Ru1 71.0(3) . . ? C26 C27 Ru1 71.4(3) . . ? C28 C27 H27 125.8 . . ? C26 C27 H27 125.8 . . ? Ru1 C27 H27 123.4 . . ? C29 C28 C27 108.1(5) . . ? C29 C28 Ru1 71.5(3) . . ? C27 C28 Ru1 71.2(3) . . ? C29 C28 H28 126 . . ? C27 C28 H28 126 . . ? Ru1 C28 H28 123 . . ? C28 C29 C25 108.5(5) . . ? C28 C29 Ru1 70.9(3) . . ? C25 C29 Ru1 71.3(3) . . ? C28 C29 H29 125.7 . . ? C25 C29 H29 125.7 . . ? Ru1 C29 H29 123.6 . . ? C19 N1 C18 121.1(3) . . ? C19 N1 C17 120.4(3) . . ? C18 N1 C17 110.5(3) . . ? F1 P1 F2 89.9(2) . . ? F1 P1 F6 88.2(3) . . ? F2 P1 F6 90.6(3) . . ? F1 P1 F4 90.1(3) . . ? F2 P1 F4 177.2(3) . . ? F6 P1 F4 92.2(3) . . ? F1 P1 F3 178.1(3) . . ? F2 P1 F3 88.5(3) . . ? F6 P1 F3 92.9(3) . . ? F4 P1 F3 91.4(3) . . ? F1 P1 F5 90.6(2) . . ? F2 P1 F5 88.7(2) . . ? F6 P1 F5 178.6(3) . . ? F4 P1 F5 88.5(3) . . ? F3 P1 F5 88.3(2) . . ? C28 Ru1 C27 37.8(2) . . ? C28 Ru1 C29 37.6(2) . . ? C27 Ru1 C29 62.9(2) . . ? C28 Ru1 C26 63.3(2) . . ? C27 Ru1 C26 37.7(2) . . ? C29 Ru1 C26 63.2(2) . . ? C28 Ru1 C25 63.2(2) . . ? C27 Ru1 C25 63.2(2) . . ? C29 Ru1 C25 37.8(2) . . ? C26 Ru1 C25 38.0(2) . . ? C28 Ru1 C22 116.3(2) . . ? C27 Ru1 C22 107.6(2) . . ? C29 Ru1 C22 148.9(2) . . ? C26 Ru1 C22 128.9(2) . . ? C25 Ru1 C22 166.8(2) . . ? C28 Ru1 C21 142.6(2) . . ? C27 Ru1 C21 112.8(2) . . ? C29 Ru1 C21 172.1(2) . . ? C26 Ru1 C21 109.2(2) . . ? C25 Ru1 C21 134.8(2) . . ? C22 Ru1 C21 37.3(2) . . ? C28 Ru1 C23 106.5(2) . . ? C27 Ru1 C23 123.7(2) . . ? C29 Ru1 C23 120.3(2) . . ? C26 Ru1 C23 160.1(2) . . ? C25 Ru1 C23 155.2(2) . . ? C22 Ru1 C23 37.5(2) . . ? C21 Ru1 C23 67.6(2) . . ? C28 Ru1 C20 173.4(2) . . ? C27 Ru1 C20 136.6(2) . . ? C29 Ru1 C20 141.1(2) . . ? C26 Ru1 C20 110.1(2) . . ? C25 Ru1 C20 112.1(2) . . ? C22 Ru1 C20 67.14(19) . . ? C21 Ru1 C20 37.21(18) . . ? C23 Ru1 C20 79.6(2) . . ? C28 Ru1 C24 119.7(2) . . ? C27 Ru1 C24 154.0(2) . . ? C29 Ru1 C24 107.59(19) . . ? C26 Ru1 C24 162.3(2) . . ? C25 Ru1 C24 125.47(19) . . ? C22 Ru1 C24 67.06(18) . . ? C21 Ru1 C24 79.1(2) . . ? C23 Ru1 C24 37.37(16) . . ? C20 Ru1 C24 66.65(18) . . ? C28 Ru1 C19 147.8(2) . . ? C27 Ru1 C19 169.5(2) . . ? C29 Ru1 C19 116.74(18) . . ? C26 Ru1 C19 131.90(19) . . ? C25 Ru1 C19 109.55(17) . . ? C22 Ru1 C19 78.00(17) . . ? C21 Ru1 C19 66.10(17) . . ? C23 Ru1 C19 66.16(16) . . ? C20 Ru1 C19 36.72(16) . . ? C24 Ru1 C19 36.21(16) . . ? data_C2 _database_code_depnum_ccdc_archive 'CCDC 901525' #TrackingRef 'Gomez.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H31 N Ru2, 2(F6 P)' _chemical_formula_sum 'C34 H31 F12 N P2 Ru2' _chemical_formula_weight 945.68 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4728(8) _cell_length_b 12.7544(10) _cell_length_c 13.4214(11) _cell_angle_alpha 99.463(3) _cell_angle_beta 95.608(3) _cell_angle_gamma 107.133(2) _cell_volume 1669.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9580 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 26.07 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.096 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_absorpt_correction_T_min 0.8617 _exptl_absorpt_correction_T_max 0.9575 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'Bruker Kappa APEX II Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_unetI/netI 0.0343 _diffrn_reflns_number 24159 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.46 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.974 _diffrn_measured_fraction_theta_max 0.974 _reflns_number_total 6706 _reflns_number_gt 5590 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0667P)^2^+7.8823P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6706 _refine_ls_number_parameters 568 _refine_ls_number_restraints 402 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.616 _refine_diff_density_min -1.316 _refine_diff_density_rms 0.121 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' 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 C14 C 0.1554(5) 0.6539(4) 0.1735(4) 0.0317(11) Uani 1 1 d . . . C1 C 0.1774(6) 0.5516(5) 0.1498(4) 0.0377(13) Uani 1 1 d . . . H1 H 0.2667 0.5476 0.1527 0.045 Uiso 1 1 calc R . . C2 C 0.0662(7) 0.4546(5) 0.1216(5) 0.0442(14) Uani 1 1 d . . . H2 H 0.0802 0.3841 0.1038 0.053 Uiso 1 1 calc R . . C3 C -0.0646(6) 0.4594(5) 0.1191(5) 0.0436(14) Uani 1 1 d . . . H3 H -0.1395 0.3926 0.1005 0.052 Uiso 1 1 calc R . . C4 C -0.0856(6) 0.5637(5) 0.1442(4) 0.0362(12) Uani 1 1 d . . . H4 H -0.1748 0.5676 0.1436 0.043 Uiso 1 1 calc R . . C11 C 0.0239(5) 0.6604(4) 0.1698(4) 0.0309(11) Uani 1 1 d . . . C10 C 0.0198(5) 0.7789(4) 0.1971(4) 0.0301(11) Uani 1 1 d . . . H10 H -0.0749 0.7814 0.1954 0.036 Uiso 1 1 calc R . . C12 C 0.1046(5) 0.8332(4) 0.3007(4) 0.0300(11) Uani 1 1 d . . . C5 C 0.0637(6) 0.8878(4) 0.3857(4) 0.0357(12) Uani 1 1 d . . . H5 H -0.0256 0.8922 0.3822 0.043 Uiso 1 1 calc R . . C6 C 0.1585(7) 0.9362(5) 0.4765(5) 0.0458(15) Uani 1 1 d . . . H6 H 0.1327 0.9743 0.5341 0.055 Uiso 1 1 calc R . . C7 C 0.2899(7) 0.9286(5) 0.4830(5) 0.0438(14) Uani 1 1 d . . . H7 H 0.3519 0.9614 0.5446 0.053 Uiso 1 1 calc R . . C8 C 0.3306(6) 0.8722(4) 0.3976(5) 0.0364(12) Uani 1 1 d . . . H8 H 0.4193 0.8666 0.4018 0.044 Uiso 1 1 calc R . . C13 C 0.2374(5) 0.8247(4) 0.3066(4) 0.0291(11) Uani 1 1 d . . . C9 C 0.2643(5) 0.7660(4) 0.2067(4) 0.0295(11) Uani 1 1 d . . . H9 H 0.3571 0.7587 0.2127 0.035 Uiso 1 1 calc R . . C15 C 0.2428(5) 0.8386(5) 0.1275(4) 0.0341(12) Uani 1 1 d . . . H15 H 0.2599 0.8053 0.0593 0.041 Uiso 1 1 calc R . . C16 C 0.0944(5) 0.8430(5) 0.1186(4) 0.0333(12) Uani 1 1 d . . . H16 H 0.0458 0.807 0.0477 0.04 Uiso 1 1 calc R . . C17 C 0.1068(5) 0.9671(5) 0.1397(5) 0.0341(12) Uani 1 1 d . . . H17A H 0.0972 0.994 0.0751 0.041 Uiso 1 1 calc R . . H17B H 0.0374 0.9813 0.1802 0.041 Uiso 1 1 calc R . . C18 C 0.3332(6) 0.9611(5) 0.1601(5) 0.0373(13) Uani 1 1 d . . . H18A H 0.4082 0.9692 0.2147 0.045 Uiso 1 1 calc R . . H18B H 0.3715 0.989 0.1014 0.045 Uiso 1 1 calc R . . C19 C 0.2882(5) 1.1335(5) 0.2367(4) 0.0333(12) Uani 1 1 d . . . C20 C 0.2008(6) 1.2013(5) 0.2304(5) 0.0371(13) Uani 1 1 d . . . H20 H 0.1114 1.1682 0.194 0.044 Uiso 1 1 calc R . . C21 C 0.2450(7) 1.3156(5) 0.2771(5) 0.0435(14) Uani 1 1 d . . . H21 H 0.1841 1.3579 0.2754 0.052 Uiso 1 1 calc R . . C22 C 0.3788(8) 1.3673(6) 0.3262(5) 0.0521(16) Uani 1 1 d . . . H22 H 0.4083 1.4439 0.3596 0.062 Uiso 1 1 calc R . . C23 C 0.4684(7) 1.3049(6) 0.3255(5) 0.0514(16) Uani 1 1 d . . . H23 H 0.5598 1.3402 0.357 0.062 Uiso 1 1 calc R . . C24 C 0.4254(6) 1.1907(5) 0.2790(5) 0.0448(14) Uani 1 1 d . . . H24 H 0.4894 1.1512 0.2759 0.054 Uiso 1 1 calc R . . C25 C 0.3479(9) 1.2527(7) -0.0004(6) 0.062(2) Uani 1 1 d . . . H25 H 0.2738 1.1937 -0.0408 0.074 Uiso 1 1 calc R . . C26 C 0.3500(9) 1.3632(7) 0.0348(5) 0.061(2) Uani 1 1 d . . . H26 H 0.2772 1.3918 0.022 0.073 Uiso 1 1 calc R . . C27 C 0.4771(10) 1.4241(7) 0.0919(7) 0.069(2) Uani 1 1 d . . . H27 H 0.5058 1.5009 0.1244 0.082 Uiso 1 1 calc R . . C28 C 0.5540(9) 1.3512(9) 0.0922(8) 0.078(3) Uani 1 1 d . . . H28 H 0.6445 1.3699 0.1254 0.094 Uiso 1 1 calc R . . C29 C 0.4740(10) 1.2449(8) 0.0346(7) 0.075(3) Uani 1 1 d . . . H29 H 0.5013 1.1798 0.0219 0.09 Uiso 1 1 calc R . . C33 C 0.1912(7) 0.6130(5) 0.4733(5) 0.0443(14) Uani 1 1 d . . . H33 H 0.2751 0.5997 0.4679 0.053 Uiso 1 1 calc R . . C34 C 0.0769(7) 0.5762(5) 0.3964(5) 0.0485(16) Uani 1 1 d . . . H34 H 0.0713 0.5347 0.3296 0.058 Uiso 1 1 calc R . . C30 C -0.0263(7) 0.6106(5) 0.4341(6) 0.0508(16) Uani 1 1 d . . . H30 H -0.1146 0.5957 0.3983 0.061 Uiso 1 1 calc R . . C31 C 0.0238(8) 0.6719(6) 0.5355(6) 0.0538(18) Uani 1 1 d . . . H31 H -0.0248 0.7061 0.5795 0.065 Uiso 1 1 calc R . . C32 C 0.1584(7) 0.6733(6) 0.5595(5) 0.0485(16) Uani 1 1 d . . . H32 H 0.2166 0.7084 0.6226 0.058 Uiso 1 1 calc R . . N1 N 0.2429(4) 1.0218(4) 0.1978(4) 0.0332(10) Uani 1 1 d . . . P1 P 0.37070(19) 0.29594(17) 0.63085(19) 0.0615(5) Uani 1 1 d DU . . F1 F 0.3798(10) 0.1833(7) 0.6678(8) 0.0663(11) Uani 0.5 1 d PDU A 1 F2 F 0.2330(8) 0.2200(8) 0.5542(8) 0.0701(11) Uani 0.5 1 d PDU A 1 F3 F 0.3678(8) 0.4018(7) 0.5836(8) 0.0669(10) Uani 0.5 1 d PDU A 1 F4 F 0.5171(8) 0.3593(7) 0.6916(8) 0.0679(10) Uani 0.5 1 d PDU A 1 F5 F 0.4488(8) 0.2555(8) 0.5375(7) 0.0690(9) Uani 0.5 1 d PDU A 1 F6 F 0.2863(9) 0.3199(8) 0.7126(7) 0.0689(9) Uani 0.5 1 d PDU A 1 F1' F 0.3880(10) 0.1792(7) 0.6246(8) 0.0681(10) Uani 0.5 1 d PDU A 2 F2' F 0.2563(9) 0.2595(8) 0.5307(7) 0.0706(11) Uani 0.5 1 d PDU A 2 F3' F 0.3508(8) 0.4210(7) 0.6546(8) 0.0673(9) Uani 0.5 1 d PDU A 2 F4' F 0.4758(8) 0.3450(7) 0.7341(7) 0.0671(11) Uani 0.5 1 d PDU A 2 F5' F 0.4866(8) 0.3336(8) 0.5673(8) 0.0696(9) Uani 0.5 1 d PDU A 2 F6' F 0.2442(8) 0.2600(8) 0.6919(8) 0.0685(11) Uani 0.5 1 d PDU A 2 P2 P 0.76881(16) 0.08609(16) 0.18195(12) 0.0453(4) Uani 1 1 d DU . . F7 F 0.7919(7) -0.0312(6) 0.1772(7) 0.092(2) Uani 0.75 1 d PDU B 1 F8 F 0.6443(6) 0.0349(8) 0.0933(5) 0.083(2) Uani 0.75 1 d PDU B 1 F9 F 0.7486(8) 0.2057(6) 0.1915(6) 0.0875(19) Uani 0.75 1 d PDU B 1 F10 F 0.8945(5) 0.1368(7) 0.2718(4) 0.0652(16) Uani 0.75 1 d PDU B 1 F11 F 0.8703(7) 0.1135(9) 0.1034(5) 0.090(2) Uani 0.75 1 d PDU B 1 F12 F 0.6716(7) 0.0615(7) 0.2634(6) 0.0680(19) Uani 0.75 1 d PDU B 1 F7' F 0.667(2) -0.0412(13) 0.1637(17) 0.093(4) Uani 0.25 1 d PDU B 2 F8' F 0.667(2) 0.109(2) 0.1025(15) 0.084(4) Uani 0.25 1 d PDU B 2 F9' F 0.871(2) 0.2053(14) 0.2106(17) 0.094(4) Uani 0.25 1 d PDU B 2 F10' F 0.863(2) 0.049(2) 0.2597(15) 0.086(4) Uani 0.25 1 d PDU B 2 F11' F 0.838(2) 0.041(2) 0.0939(14) 0.083(5) Uani 0.25 1 d PDU B 2 F12' F 0.688(2) 0.116(2) 0.2696(15) 0.075(5) Uani 0.25 1 d PDU B 2 Ru1 Ru 0.38237(4) 1.28976(4) 0.16761(3) 0.03266(14) Uani 1 1 d . . . Ru2 Ru 0.14395(4) 0.75845(4) 0.43417(3) 0.03206(14) 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 C14 0.035(3) 0.028(3) 0.030(3) 0.002(2) 0.005(2) 0.009(2) C1 0.041(3) 0.031(3) 0.038(3) -0.005(2) 0.002(2) 0.013(2) C2 0.055(4) 0.028(3) 0.044(3) -0.004(2) 0.002(3) 0.013(3) C3 0.045(3) 0.027(3) 0.044(3) 0.000(2) -0.004(3) -0.001(3) C4 0.031(3) 0.033(3) 0.038(3) 0.005(2) -0.004(2) 0.004(2) C11 0.035(3) 0.027(3) 0.028(3) 0.004(2) 0.004(2) 0.006(2) C10 0.025(2) 0.027(3) 0.039(3) 0.008(2) 0.005(2) 0.008(2) C12 0.034(3) 0.024(2) 0.036(3) 0.009(2) 0.011(2) 0.011(2) C5 0.045(3) 0.026(3) 0.042(3) 0.008(2) 0.016(3) 0.017(2) C6 0.064(4) 0.028(3) 0.044(3) 0.001(3) 0.016(3) 0.014(3) C7 0.058(4) 0.025(3) 0.037(3) -0.001(2) 0.002(3) 0.001(3) C8 0.034(3) 0.024(3) 0.045(3) 0.003(2) 0.003(2) 0.003(2) C13 0.030(3) 0.020(2) 0.035(3) 0.003(2) 0.005(2) 0.007(2) C9 0.024(2) 0.027(3) 0.036(3) 0.003(2) 0.006(2) 0.009(2) C15 0.033(3) 0.033(3) 0.039(3) 0.010(2) 0.014(2) 0.012(2) C16 0.032(3) 0.033(3) 0.036(3) 0.010(2) 0.007(2) 0.009(2) C17 0.026(3) 0.033(3) 0.044(3) 0.016(2) 0.006(2) 0.007(2) C18 0.031(3) 0.033(3) 0.053(4) 0.015(3) 0.017(2) 0.010(2) C19 0.035(3) 0.032(3) 0.038(3) 0.017(2) 0.010(2) 0.010(2) C20 0.036(3) 0.035(3) 0.046(3) 0.015(3) 0.020(3) 0.012(2) C21 0.056(4) 0.040(3) 0.044(3) 0.014(3) 0.026(3) 0.021(3) C22 0.074(5) 0.040(3) 0.041(4) 0.006(3) 0.012(3) 0.015(3) C23 0.052(4) 0.043(4) 0.046(4) 0.009(3) -0.009(3) 0.001(3) C24 0.042(3) 0.042(3) 0.050(4) 0.016(3) 0.000(3) 0.012(3) C25 0.087(6) 0.059(5) 0.044(4) 0.012(3) 0.031(4) 0.024(4) C26 0.097(6) 0.067(5) 0.045(4) 0.030(4) 0.034(4) 0.050(5) C27 0.094(6) 0.044(4) 0.070(5) 0.026(4) 0.038(5) 0.009(4) C28 0.056(5) 0.098(7) 0.096(7) 0.050(6) 0.044(5) 0.021(5) C29 0.101(7) 0.069(5) 0.090(6) 0.040(5) 0.070(6) 0.048(5) C33 0.053(4) 0.037(3) 0.047(4) 0.013(3) 0.005(3) 0.019(3) C34 0.073(5) 0.026(3) 0.042(3) 0.009(3) 0.006(3) 0.008(3) C30 0.048(4) 0.036(3) 0.065(4) 0.023(3) 0.000(3) 0.003(3) C31 0.070(5) 0.039(4) 0.059(4) 0.019(3) 0.033(4) 0.014(3) C32 0.065(4) 0.043(4) 0.033(3) 0.010(3) -0.001(3) 0.013(3) N1 0.025(2) 0.029(2) 0.047(3) 0.012(2) 0.0093(19) 0.0078(18) P1 0.0425(8) 0.0510(9) 0.0906(13) 0.0172(9) 0.0136(8) 0.0117(7) F1 0.0533(17) 0.0527(17) 0.091(2) 0.0165(18) 0.0162(18) 0.0119(15) F2 0.0510(17) 0.0562(19) 0.094(2) 0.0188(18) 0.0095(17) 0.0024(17) F3 0.0495(17) 0.0539(17) 0.094(2) 0.0182(17) 0.0097(17) 0.0108(16) F4 0.0472(16) 0.0578(16) 0.0937(19) 0.0168(16) 0.0096(15) 0.0089(15) F5 0.0513(15) 0.0580(16) 0.0936(18) 0.0145(16) 0.0139(15) 0.0109(14) F6 0.0490(15) 0.0571(17) 0.0957(18) 0.0119(16) 0.0154(15) 0.0100(14) F1' 0.0524(15) 0.0547(15) 0.0941(19) 0.0138(16) 0.0148(16) 0.0119(14) F2' 0.0516(17) 0.0583(19) 0.093(2) 0.0172(18) 0.0098(17) 0.0037(17) F3' 0.0483(15) 0.0549(16) 0.0959(19) 0.0146(16) 0.0117(15) 0.0120(14) F4' 0.0458(17) 0.0579(18) 0.093(2) 0.0155(18) 0.0098(17) 0.0097(16) F5' 0.0498(15) 0.0594(16) 0.0938(18) 0.0159(16) 0.0146(15) 0.0073(14) F6' 0.0475(17) 0.0565(18) 0.096(2) 0.0136(18) 0.0173(16) 0.0065(16) P2 0.0350(8) 0.0651(11) 0.0367(8) 0.0017(7) 0.0060(6) 0.0219(8) F7 0.077(4) 0.069(4) 0.127(6) -0.003(4) 0.004(4) 0.036(3) F8 0.049(3) 0.121(5) 0.058(3) -0.025(4) -0.011(3) 0.025(4) F9 0.087(4) 0.062(3) 0.118(5) 0.026(3) 0.010(4) 0.027(3) F10 0.039(3) 0.099(4) 0.046(3) -0.009(3) -0.001(2) 0.019(3) F11 0.057(4) 0.160(7) 0.051(3) 0.032(4) 0.019(3) 0.023(4) F12 0.042(3) 0.101(5) 0.067(4) 0.033(4) 0.018(3) 0.022(4) F7' 0.086(8) 0.080(6) 0.096(9) 0.002(7) 0.013(7) 0.007(6) F8' 0.068(8) 0.120(10) 0.077(8) 0.025(8) 0.002(6) 0.049(8) F9' 0.077(8) 0.090(7) 0.097(9) 0.009(7) 0.022(7) 0.001(7) F10' 0.067(8) 0.124(9) 0.077(8) 0.025(8) 0.005(7) 0.047(7) F11' 0.052(8) 0.126(10) 0.070(7) -0.011(8) 0.019(6) 0.040(8) F12' 0.043(8) 0.110(12) 0.059(7) -0.016(9) 0.016(6) 0.020(8) Ru1 0.0320(2) 0.0275(2) 0.0404(3) 0.01115(19) 0.01131(19) 0.00821(18) Ru2 0.0382(3) 0.0253(2) 0.0308(2) 0.00320(17) 0.00488(18) 0.00878(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C14 C1 1.381(8) . ? C14 C11 1.401(8) . ? C14 C9 1.508(7) . ? C1 C2 1.394(8) . ? C1 H1 0.95 . ? C2 C3 1.386(9) . ? C2 H2 0.95 . ? C3 C4 1.403(8) . ? C3 H3 0.95 . ? C4 C11 1.380(7) . ? C4 H4 0.95 . ? C11 C10 1.509(7) . ? C10 C12 1.511(8) . ? C10 C16 1.567(7) . ? C10 H10 1 . ? C12 C5 1.407(7) . ? C12 C13 1.422(7) . ? C12 Ru2 2.222(5) . ? C5 C6 1.417(9) . ? C5 Ru2 2.217(5) . ? C5 H5 0.95 . ? C6 C7 1.403(10) . ? C6 Ru2 2.200(6) . ? C6 H6 0.95 . ? C7 C8 1.420(8) . ? C7 Ru2 2.204(6) . ? C7 H7 0.95 . ? C8 C13 1.410(8) . ? C8 Ru2 2.217(6) . ? C8 H8 0.95 . ? C13 C9 1.518(7) . ? C13 Ru2 2.218(5) . ? C9 C15 1.561(8) . ? C9 H9 1 . ? C15 C18 1.533(8) . ? C15 C16 1.566(7) . ? C15 H15 1 . ? C16 C17 1.525(8) . ? C16 H16 1 . ? C17 N1 1.464(7) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 N1 1.464(7) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 N1 1.355(7) . ? C19 C24 1.416(8) . ? C19 C20 1.438(8) . ? C19 Ru1 2.331(5) . ? C20 C21 1.407(8) . ? C20 Ru1 2.228(5) . ? C20 H20 0.95 . ? C21 C22 1.402(10) . ? C21 Ru1 2.207(6) . ? C21 H21 0.95 . ? C22 C23 1.398(10) . ? C22 Ru1 2.203(7) . ? C22 H22 0.95 . ? C23 C24 1.404(9) . ? C23 Ru1 2.175(7) . ? C23 H23 0.95 . ? C24 Ru1 2.205(6) . ? C24 H24 0.95 . ? C25 C29 1.395(12) . ? C25 C26 1.404(10) . ? C25 Ru1 2.197(7) . ? C25 H25 0.95 . ? C26 C27 1.399(12) . ? C26 Ru1 2.188(7) . ? C26 H26 0.95 . ? C27 C28 1.399(13) . ? C27 Ru1 2.173(7) . ? C27 H27 0.95 . ? C28 C29 1.413(13) . ? C28 Ru1 2.158(7) . ? C28 H28 0.95 . ? C29 Ru1 2.182(7) . ? C29 H29 0.95 . ? C33 C34 1.410(9) . ? C33 C32 1.411(9) . ? C33 Ru2 2.184(6) . ? C33 H33 0.95 . ? C34 C30 1.389(10) . ? C34 Ru2 2.175(6) . ? C34 H34 0.95 . ? C30 C31 1.417(10) . ? C30 Ru2 2.180(6) . ? C30 H30 0.95 . ? C31 C32 1.410(10) . ? C31 Ru2 2.159(6) . ? C31 H31 0.95 . ? C32 Ru2 2.164(6) . ? C32 H32 0.95 . ? P1 F6 1.522(8) . ? P1 F1' 1.542(9) . ? P1 F5' 1.557(8) . ? P1 F4 1.574(8) . ? P1 F3 1.590(8) . ? P1 F4' 1.592(9) . ? P1 F2' 1.615(9) . ? P1 F6' 1.617(8) . ? P1 F1 1.620(8) . ? P1 F2 1.624(8) . ? P1 F3' 1.653(8) . ? P1 F5 1.656(9) . ? P2 F9' 1.540(14) . ? P2 F8' 1.558(13) . ? P2 F11' 1.561(13) . ? P2 F12 1.572(6) . ? P2 F8 1.575(6) . ? P2 F11 1.576(6) . ? P2 F7 1.576(7) . ? P2 F12' 1.577(13) . ? P2 F10' 1.585(13) . ? P2 F9 1.587(7) . ? P2 F10 1.593(5) . ? P2 F7' 1.620(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 C1 C14 C11 120.8(5) . . ? C1 C14 C9 125.4(5) . . ? C11 C14 C9 113.7(5) . . ? C14 C1 C2 118.9(5) . . ? C14 C1 H1 120.6 . . ? C2 C1 H1 120.6 . . ? C3 C2 C1 121.0(6) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 119.6(5) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C11 C4 C3 119.8(5) . . ? C11 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C11 C14 119.9(5) . . ? C4 C11 C10 126.8(5) . . ? C14 C11 C10 113.3(5) . . ? C11 C10 C12 108.4(4) . . ? C11 C10 C16 106.2(4) . . ? C12 C10 C16 106.2(4) . . ? C11 C10 H10 111.9 . . ? C12 C10 H10 111.9 . . ? C16 C10 H10 111.9 . . ? C5 C12 C13 120.7(5) . . ? C5 C12 C10 126.5(5) . . ? C13 C12 C10 112.8(4) . . ? C5 C12 Ru2 71.3(3) . . ? C13 C12 Ru2 71.2(3) . . ? C10 C12 Ru2 130.2(4) . . ? C12 C5 C6 118.5(5) . . ? C12 C5 Ru2 71.7(3) . . ? C6 C5 Ru2 70.6(3) . . ? C12 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? Ru2 C5 H5 129.2 . . ? C7 C6 C5 121.2(5) . . ? C7 C6 Ru2 71.6(3) . . ? C5 C6 Ru2 72.0(3) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? Ru2 C6 H6 129.6 . . ? C6 C7 C8 120.2(6) . . ? C6 C7 Ru2 71.3(3) . . ? C8 C7 Ru2 71.8(3) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? Ru2 C7 H7 129.5 . . ? C13 C8 C7 119.1(5) . . ? C13 C8 Ru2 71.5(3) . . ? C7 C8 Ru2 70.8(3) . . ? C13 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? Ru2 C8 H8 129.6 . . ? C8 C13 C12 120.3(5) . . ? C8 C13 C9 126.5(5) . . ? C12 C13 C9 113.2(5) . . ? C8 C13 Ru2 71.4(3) . . ? C12 C13 Ru2 71.5(3) . . ? C9 C13 Ru2 131.6(3) . . ? C14 C9 C13 108.0(4) . . ? C14 C9 C15 107.0(4) . . ? C13 C9 C15 105.1(4) . . ? C14 C9 H9 112.1 . . ? C13 C9 H9 112.1 . . ? C15 C9 H9 112.1 . . ? C18 C15 C9 112.8(5) . . ? C18 C15 C16 105.3(4) . . ? C9 C15 C16 109.6(4) . . ? C18 C15 H15 109.7 . . ? C9 C15 H15 109.7 . . ? C16 C15 H15 109.7 . . ? C17 C16 C15 105.8(4) . . ? C17 C16 C10 112.9(4) . . ? C15 C16 C10 109.2(4) . . ? C17 C16 H16 109.6 . . ? C15 C16 H16 109.6 . . ? C10 C16 H16 109.6 . . ? N1 C17 C16 103.8(4) . . ? N1 C17 H17A 111 . . ? C16 C17 H17A 111 . . ? N1 C17 H17B 111 . . ? C16 C17 H17B 111 . . ? H17A C17 H17B 109 . . ? N1 C18 C15 104.6(4) . . ? N1 C18 H18A 110.8 . . ? C15 C18 H18A 110.8 . . ? N1 C18 H18B 110.8 . . ? C15 C18 H18B 110.8 . . ? H18A C18 H18B 108.9 . . ? N1 C19 C24 122.1(5) . . ? N1 C19 C20 121.3(5) . . ? C24 C19 C20 116.5(5) . . ? N1 C19 Ru1 133.4(4) . . ? C24 C19 Ru1 67.0(3) . . ? C20 C19 Ru1 67.7(3) . . ? C21 C20 C19 121.3(6) . . ? C21 C20 Ru1 70.7(3) . . ? C19 C20 Ru1 75.6(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? Ru1 C20 H20 126.2 . . ? C22 C21 C20 120.1(6) . . ? C22 C21 Ru1 71.3(4) . . ? C20 C21 Ru1 72.3(3) . . ? C22 C21 H21 120 . . ? C20 C21 H21 120 . . ? Ru1 C21 H21 128.7 . . ? C23 C22 C21 119.3(6) . . ? C23 C22 Ru1 70.3(4) . . ? C21 C22 Ru1 71.6(4) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? Ru1 C22 H22 130.2 . . ? C22 C23 C24 121.0(6) . . ? C22 C23 Ru1 72.5(4) . . ? C24 C23 Ru1 72.5(4) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? Ru1 C23 H23 127.7 . . ? C23 C24 C19 121.1(6) . . ? C23 C24 Ru1 70.1(4) . . ? C19 C24 Ru1 76.8(3) . . ? C23 C24 H24 119.4 . . ? C19 C24 H24 119.4 . . ? Ru1 C24 H24 125.3 . . ? C29 C25 C26 107.8(8) . . ? C29 C25 Ru1 70.8(5) . . ? C26 C25 Ru1 71.0(4) . . ? C29 C25 H25 126.1 . . ? C26 C25 H25 126.1 . . ? Ru1 C25 H25 123.8 . . ? C27 C26 C25 108.6(8) . . ? C27 C26 Ru1 70.7(4) . . ? C25 C26 Ru1 71.7(4) . . ? C27 C26 H26 125.7 . . ? C25 C26 H26 125.7 . . ? Ru1 C26 H26 123.5 . . ? C28 C27 C26 107.5(8) . . ? C28 C27 Ru1 70.6(4) . . ? C26 C27 Ru1 71.9(4) . . ? C28 C27 H27 126.2 . . ? C26 C27 H27 126.2 . . ? Ru1 C27 H27 123 . . ? C27 C28 C29 108.2(8) . . ? C27 C28 Ru1 71.7(4) . . ? C29 C28 Ru1 71.9(4) . . ? C27 C28 H28 125.9 . . ? C29 C28 H28 125.9 . . ? Ru1 C28 H28 122.1 . . ? C25 C29 C28 107.8(7) . . ? C25 C29 Ru1 72.0(4) . . ? C28 C29 Ru1 70.1(4) . . ? C25 C29 H29 126.1 . . ? C28 C29 H29 126.1 . . ? Ru1 C29 H29 123.4 . . ? C34 C33 C32 107.5(6) . . ? C34 C33 Ru2 70.8(3) . . ? C32 C33 Ru2 70.3(4) . . ? C34 C33 H33 126.2 . . ? C32 C33 H33 126.2 . . ? Ru2 C33 H33 124.3 . . ? C30 C34 C33 108.9(6) . . ? C30 C34 Ru2 71.6(4) . . ? C33 C34 Ru2 71.5(3) . . ? C30 C34 H34 125.5 . . ? C33 C34 H34 125.5 . . ? Ru2 C34 H34 123 . . ? C34 C30 C31 107.8(6) . . ? C34 C30 Ru2 71.2(4) . . ? C31 C30 Ru2 70.1(4) . . ? C34 C30 H30 126.1 . . ? C31 C30 H30 126.1 . . ? Ru2 C30 H30 124.1 . . ? C32 C31 C30 107.9(6) . . ? C32 C31 Ru2 71.2(4) . . ? C30 C31 Ru2 71.7(4) . . ? C32 C31 H31 126 . . ? C30 C31 H31 126 . . ? Ru2 C31 H31 122.7 . . ? C31 C32 C33 107.8(6) . . ? C31 C32 Ru2 70.8(4) . . ? C33 C32 Ru2 71.9(4) . . ? C31 C32 H32 126.1 . . ? C33 C32 H32 126.1 . . ? Ru2 C32 H32 123 . . ? C19 N1 C17 121.3(5) . . ? C19 N1 C18 121.9(4) . . ? C17 N1 C18 109.1(5) . . ? F6 P1 F1' 111.6(6) . . ? F6 P1 F5' 152.1(5) . . ? F1' P1 F5' 92.2(5) . . ? F6 P1 F4 100.1(5) . . ? F1' P1 F4 93.7(5) . . ? F5' P1 F4 62.6(5) . . ? F6 P1 F3 93.9(5) . . ? F1' P1 F3 152.4(6) . . ? F5' P1 F3 66.5(5) . . ? F4 P1 F3 91.7(5) . . ? F6 P1 F4' 75.1(5) . . ? F1' P1 F4' 91.6(5) . . ? F3 P1 F4' 105.3(5) . . ? F6 P1 F2' 99.5(5) . . ? F1' P1 F2' 95.4(5) . . ? F5' P1 F2' 92.2(5) . . ? F4 P1 F2' 153.5(5) . . ? F3 P1 F2' 69.3(5) . . ? F4' P1 F2' 172.4(5) . . ? F1' P1 F6' 90.3(5) . . ? F5' P1 F6' 176.2(5) . . ? F4 P1 F6' 120.1(6) . . ? F3 P1 F6' 110.1(5) . . ? F4' P1 F6' 92.3(5) . . ? F2' P1 F6' 84.8(5) . . ? F6 P1 F1 92.2(5) . . ? F5' P1 F1 108.2(5) . . ? F4 P1 F1 88.6(5) . . ? F3 P1 F1 173.7(5) . . ? F4' P1 F1 77.7(5) . . ? F2' P1 F1 108.2(5) . . ? F6' P1 F1 75.0(5) . . ? F6 P1 F2 89.6(5) . . ? F1' P1 F2 80.2(5) . . ? F5' P1 F2 109.4(5) . . ? F4 P1 F2 169.9(5) . . ? F3 P1 F2 90.2(5) . . ? F4' P1 F2 158.7(5) . . ? F6' P1 F2 68.2(5) . . ? F1 P1 F2 88.4(5) . . ? F6 P1 F3' 61.5(5) . . ? F1' P1 F3' 172.0(6) . . ? F5' P1 F3' 93.5(5) . . ? F4 P1 F3' 84.0(5) . . ? F4' P1 F3' 82.8(5) . . ? F2' P1 F3' 90.0(5) . . ? F6' P1 F3' 84.3(5) . . ? F1 P1 F3' 150.7(5) . . ? F2 P1 F3' 103.1(5) . . ? F6 P1 F5 173.3(5) . . ? F1' P1 F5 63.9(5) . . ? F4 P1 F5 85.3(5) . . ? F3 P1 F5 89.7(5) . . ? F4' P1 F5 109.3(5) . . ? F2' P1 F5 76.5(5) . . ? F6' P1 F5 145.9(5) . . ? F1 P1 F5 84.1(5) . . ? F2 P1 F5 84.8(5) . . ? F3' P1 F5 123.4(5) . . ? F9' P2 F8' 97.8(13) . . ? F9' P2 F11' 96.5(11) . . ? F8' P2 F11' 90.3(11) . . ? F9' P2 F12 112.3(8) . . ? F8' P2 F12 96.5(9) . . ? F11' P2 F12 149.0(10) . . ? F9' P2 F8 129.5(10) . . ? F11' P2 F8 79.4(8) . . ? F12 P2 F8 90.2(4) . . ? F9' P2 F11 66.0(8) . . ? F8' P2 F11 84.9(9) . . ? F12 P2 F11 178.0(4) . . ? F8 P2 F11 91.8(4) . . ? F9' P2 F7 130.3(10) . . ? F8' P2 F7 123.5(10) . . ? F11' P2 F7 60.6(10) . . ? F12 P2 F7 90.9(4) . . ? F8 P2 F7 91.6(4) . . ? F11 P2 F7 89.5(5) . . ? F9' P2 F12' 90.7(11) . . ? F8' P2 F12' 90.0(11) . . ? F11' P2 F12' 172.6(13) . . ? F8 P2 F12' 97.0(9) . . ? F11 P2 F12' 155.1(10) . . ? F7 P2 F12' 113.3(10) . . ? F9' P2 F10' 88.3(12) . . ? F8' P2 F10' 173.9(14) . . ? F11' P2 F10' 88.6(11) . . ? F12 P2 F10' 81.5(8) . . ? F8 P2 F10' 141.1(10) . . ? F11 P2 F10' 97.3(8) . . ? F7 P2 F10' 51.0(9) . . ? F12' P2 F10' 90.3(11) . . ? F9' P2 F9 48.4(9) . . ? F8' P2 F9 58.8(10) . . ? F11' P2 F9 120.8(11) . . ? F12 P2 F9 88.1(4) . . ? F8 P2 F9 90.6(4) . . ? F11 P2 F9 91.4(5) . . ? F7 P2 F9 177.6(4) . . ? F12' P2 F9 65.4(10) . . ? F10' P2 F9 126.7(10) . . ? F9' P2 F10 51.0(9) . . ? F8' P2 F10 147.7(10) . . ? F11' P2 F10 100.6(8) . . ? F12 P2 F10 89.6(4) . . ? F8 P2 F10 179.5(5) . . ? F11 P2 F10 88.4(3) . . ? F7 P2 F10 87.9(4) . . ? F12' P2 F10 83.0(9) . . ? F9 P2 F10 89.9(4) . . ? F9' P2 F7' 173.9(12) . . ? F8' P2 F7' 87.8(12) . . ? F11' P2 F7' 85.9(11) . . ? F12 P2 F7' 64.3(8) . . ? F8 P2 F7' 56.5(9) . . ? F11 P2 F7' 117.3(8) . . ? F7 P2 F7' 46.5(8) . . ? F12' P2 F7' 86.7(11) . . ? F10' P2 F7' 86.1(12) . . ? F9 P2 F7' 134.5(9) . . ? F10 P2 F7' 123.0(9) . . ? C28 Ru1 C27 37.7(3) . . ? C28 Ru1 C23 104.9(3) . . ? C27 Ru1 C23 116.7(3) . . ? C28 Ru1 C29 38.0(4) . . ? C27 Ru1 C29 63.1(3) . . ? C23 Ru1 C29 124.9(3) . . ? C28 Ru1 C26 62.6(3) . . ? C27 Ru1 C26 37.4(3) . . ? C23 Ru1 C26 151.3(3) . . ? C29 Ru1 C26 62.4(3) . . ? C28 Ru1 C25 62.8(4) . . ? C27 Ru1 C25 62.8(3) . . ? C23 Ru1 C25 161.8(3) . . ? C29 Ru1 C25 37.2(3) . . ? C26 Ru1 C25 37.3(3) . . ? C28 Ru1 C22 121.0(4) . . ? C27 Ru1 C22 107.3(3) . . ? C23 Ru1 C22 37.2(3) . . ? C29 Ru1 C22 156.4(4) . . ? C26 Ru1 C22 124.4(3) . . ? C25 Ru1 C22 160.2(3) . . ? C28 Ru1 C24 111.6(3) . . ? C27 Ru1 C24 143.1(3) . . ? C23 Ru1 C24 37.4(2) . . ? C29 Ru1 C24 106.6(3) . . ? C26 Ru1 C24 168.4(3) . . ? C25 Ru1 C24 131.5(3) . . ? C22 Ru1 C24 67.2(3) . . ? C28 Ru1 C21 151.7(3) . . ? C27 Ru1 C21 119.6(3) . . ? C23 Ru1 C21 66.9(3) . . ? C29 Ru1 C21 166.6(3) . . ? C26 Ru1 C21 110.9(3) . . ? C25 Ru1 C21 130.4(3) . . ? C22 Ru1 C21 37.1(3) . . ? C24 Ru1 C21 79.1(2) . . ? C28 Ru1 C20 171.3(3) . . ? C27 Ru1 C20 147.5(3) . . ? C23 Ru1 C20 78.7(2) . . ? C29 Ru1 C20 133.6(3) . . ? C26 Ru1 C20 117.7(3) . . ? C25 Ru1 C20 111.7(3) . . ? C22 Ru1 C20 66.6(3) . . ? C24 Ru1 C20 66.4(2) . . ? C21 Ru1 C20 37.0(2) . . ? C28 Ru1 C19 137.4(3) . . ? C27 Ru1 C19 174.1(3) . . ? C23 Ru1 C19 66.0(2) . . ? C29 Ru1 C19 111.0(3) . . ? C26 Ru1 C19 141.3(3) . . ? C25 Ru1 C19 112.9(3) . . ? C22 Ru1 C19 78.1(2) . . ? C24 Ru1 C19 36.3(2) . . ? C21 Ru1 C19 66.2(2) . . ? C20 Ru1 C19 36.7(2) . . ? C31 Ru2 C32 38.1(3) . . ? C31 Ru2 C34 63.1(3) . . ? C32 Ru2 C34 63.2(2) . . ? C31 Ru2 C30 38.1(3) . . ? C32 Ru2 C30 63.5(3) . . ? C34 Ru2 C30 37.2(3) . . ? C31 Ru2 C33 63.3(3) . . ? C32 Ru2 C33 37.9(2) . . ? C34 Ru2 C33 37.7(2) . . ? C30 Ru2 C33 62.9(3) . . ? C31 Ru2 C6 106.9(3) . . ? C32 Ru2 C6 116.1(2) . . ? C34 Ru2 C6 165.7(3) . . ? C30 Ru2 C6 128.7(3) . . ? C33 Ru2 C6 149.4(3) . . ? C31 Ru2 C7 123.3(3) . . ? C32 Ru2 C7 106.8(2) . . ? C34 Ru2 C7 156.6(3) . . ? C30 Ru2 C7 159.9(3) . . ? C33 Ru2 C7 121.3(3) . . ? C6 Ru2 C7 37.1(2) . . ? C31 Ru2 C8 153.6(3) . . ? C32 Ru2 C8 119.3(2) . . ? C34 Ru2 C8 126.4(2) . . ? C30 Ru2 C8 162.5(3) . . ? C33 Ru2 C8 107.8(2) . . ? C6 Ru2 C8 67.3(2) . . ? C7 Ru2 C8 37.5(2) . . ? C31 Ru2 C5 111.6(2) . . ? C32 Ru2 C5 142.0(2) . . ? C34 Ru2 C5 133.9(2) . . ? C30 Ru2 C5 108.4(2) . . ? C33 Ru2 C5 171.1(2) . . ? C6 Ru2 C5 37.4(2) . . ? C7 Ru2 C5 67.5(2) . . ? C8 Ru2 C5 80.0(2) . . ? C31 Ru2 C13 169.0(2) . . ? C32 Ru2 C13 147.6(2) . . ? C34 Ru2 C13 109.2(2) . . ? C30 Ru2 C13 131.1(2) . . ? C33 Ru2 C13 116.1(2) . . ? C6 Ru2 C13 79.0(2) . . ? C7 Ru2 C13 66.9(2) . . ? C8 Ru2 C13 37.1(2) . . ? C5 Ru2 C13 67.32(19) . . ? C31 Ru2 C12 136.1(3) . . ? C32 Ru2 C12 173.4(2) . . ? C34 Ru2 C12 112.5(2) . . ? C30 Ru2 C12 110.0(2) . . ? C33 Ru2 C12 141.5(2) . . ? C6 Ru2 C12 66.6(2) . . ? C7 Ru2 C12 79.0(2) . . ? C8 Ru2 C12 67.2(2) . . ? C5 Ru2 C12 36.97(19) . . ? C13 Ru2 C12 37.34(19) . . ? data_C3 _database_code_depnum_ccdc_archive 'CCDC 901526' #TrackingRef 'Gomez.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C39 H36 N Ru3, 3(F6 P), C3 H6 O' _chemical_formula_sum 'C42 H42 F18 N O P3 Ru3' _chemical_formula_weight 1314.89 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.3186(15) _cell_length_b 10.2557(8) _cell_length_c 22.5063(18) _cell_angle_alpha 90 _cell_angle_beta 97.386(4) _cell_angle_gamma 90 _cell_volume 4422.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9229 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 30.51 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_absorpt_correction_T_min 0.630 _exptl_absorpt_correction_T_max 0.780 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'Bruker Kappa APEX II Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_unetI/netI 0.0164 _diffrn_reflns_number 81728 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 30.57 _diffrn_reflns_theta_full 30.57 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 13502 _reflns_number_gt 12199 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0311P)^2^+3.8937P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 13502 _refine_ls_number_parameters 725 _refine_ls_number_restraints 255 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.069 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.973 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.074 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C11 C 0.34884(9) 0.11922(17) 0.21854(7) 0.0200(3) Uani 1 1 d . . . C4 C 0.41170(9) 0.1731(2) 0.24764(8) 0.0249(3) Uani 1 1 d . . . H4 H 0.4163 0.2647 0.253 0.03 Uiso 1 1 calc R . . C3 C 0.46780(10) 0.0885(2) 0.26878(9) 0.0293(4) Uani 1 1 d . . . H3 H 0.5108 0.1237 0.287 0.035 Uiso 1 1 calc R . . C2 C 0.45959(10) -0.0481(2) 0.26271(9) 0.0292(4) Uani 1 1 d . . . H2 H 0.4971 -0.104 0.2775 0.035 Uiso 1 1 calc R . . C1 C 0.39613(10) -0.10257(19) 0.23490(8) 0.0247(3) Uani 1 1 d . . . H1 H 0.3904 -0.1944 0.2319 0.03 Uiso 1 1 calc R . . C14 C 0.34143(9) -0.01788(17) 0.21172(7) 0.0200(3) Uani 1 1 d . . . C9 C 0.27221(9) -0.05769(17) 0.17732(8) 0.0200(3) Uani 1 1 d . . . H9 H 0.2687 -0.1542 0.1714 0.024 Uiso 1 1 calc R . . C13 C 0.26493(8) 0.01551(17) 0.11812(8) 0.0202(3) Uani 1 1 d . . . C8 C 0.24882(9) -0.0385(2) 0.06022(8) 0.0269(4) Uani 1 1 d . . . H8 H 0.2451 -0.1303 0.055 0.032 Uiso 1 1 calc R . . C7 C 0.23821(10) 0.0460(2) 0.00994(9) 0.0340(4) Uani 1 1 d . . . H7 H 0.2261 0.0106 -0.029 0.041 Uiso 1 1 calc R . . C6 C 0.24550(10) 0.1824(2) 0.01732(9) 0.0337(4) Uani 1 1 d . . . H6 H 0.2381 0.2381 -0.0166 0.04 Uiso 1 1 calc R . . C5 C 0.26380(9) 0.2364(2) 0.07523(9) 0.0274(4) Uani 1 1 d . . . H5 H 0.2699 0.3278 0.0802 0.033 Uiso 1 1 calc R . . C12 C 0.27278(8) 0.15259(17) 0.12539(8) 0.0208(3) Uani 1 1 d . . . C10 C 0.28598(8) 0.19459(17) 0.19041(8) 0.0205(3) Uani 1 1 d . . . H10 H 0.2931 0.2909 0.1945 0.025 Uiso 1 1 calc R . . C16 C 0.22087(9) 0.14768(17) 0.21903(8) 0.0213(3) Uani 1 1 d . . . H16 H 0.2261 0.1724 0.2624 0.026 Uiso 1 1 calc R . . C15 C 0.21357(9) -0.00380(17) 0.21257(8) 0.0206(3) Uani 1 1 d . . . H15 H 0.2181 -0.0445 0.2533 0.025 Uiso 1 1 calc R . . C18 C 0.14002(9) -0.02755(17) 0.18036(8) 0.0233(3) Uani 1 1 d . . . H18A H 0.1399 -0.0998 0.1512 0.028 Uiso 1 1 calc R . . H18B H 0.1072 -0.0488 0.2093 0.028 Uiso 1 1 calc R . . C17 C 0.15207(9) 0.20338(18) 0.18672(9) 0.0248(3) Uani 1 1 d . . . H17A H 0.1209 0.2312 0.216 0.03 Uiso 1 1 calc R . . H17B H 0.1612 0.279 0.1615 0.03 Uiso 1 1 calc R . . C19 C 0.05884(9) 0.10904(19) 0.11391(8) 0.0236(3) Uani 1 1 d . . . C24 C 0.01774(10) -0.0022(2) 0.09409(8) 0.0270(4) Uani 1 1 d . . . H24 H 0.0321 -0.0864 0.1084 0.032 Uiso 1 1 calc R . . C23 C -0.04411(11) 0.0110(2) 0.05334(9) 0.0338(4) Uani 1 1 d . . . H23 H -0.0696 -0.0643 0.0391 0.041 Uiso 1 1 calc R . . C22 C -0.06801(12) 0.1359(3) 0.03390(10) 0.0402(5) Uani 1 1 d . . . H22 H -0.1087 0.1445 0.0057 0.048 Uiso 1 1 calc R . . C21 C -0.03128(11) 0.2474(3) 0.05652(10) 0.0384(5) Uani 1 1 d . . . H21 H -0.0476 0.3316 0.0439 0.046 Uiso 1 1 calc R . . C20 C 0.03022(10) 0.2346(2) 0.09832(10) 0.0303(4) Uani 1 1 d . . . H20 H 0.0524 0.3103 0.116 0.036 Uiso 1 1 calc R . . C29 C -0.0694(2) 0.0573(4) 0.22104(15) 0.0685(10) Uani 1 1 d . . . H29 H -0.0389 -0.0045 0.2421 0.082 Uiso 1 1 calc R . . C28 C -0.1295(2) 0.0287(3) 0.18171(17) 0.0701(11) Uani 1 1 d . . . H28 H -0.147 -0.0561 0.1715 0.084 Uiso 1 1 calc R . . C27 C -0.15916(13) 0.1448(4) 0.16024(14) 0.0601(9) Uani 1 1 d . . . H27 H -0.2006 0.1538 0.1328 0.072 Uiso 1 1 calc R . . C26 C -0.11713(17) 0.2479(3) 0.18617(14) 0.0550(7) Uani 1 1 d . . . H26 H -0.1249 0.3384 0.1792 0.066 Uiso 1 1 calc R . . C25 C -0.06202(15) 0.1918(4) 0.22396(12) 0.0591(8) Uani 1 1 d . . . H25 H -0.0257 0.2379 0.2476 0.071 Uiso 1 1 calc R . . C30 C 0.45012(11) 0.1308(3) 0.09249(11) 0.0497(7) Uani 1 1 d . . . H30 H 0.4642 0.1756 0.129 0.06 Uiso 1 1 calc R . . C34 C 0.44239(12) -0.0055(3) 0.08572(14) 0.0563(8) Uani 1 1 d . . . H34 H 0.4503 -0.0685 0.1168 0.068 Uiso 1 1 calc R . . C33 C 0.42086(13) -0.0315(3) 0.02472(15) 0.0482(6) Uani 1 1 d . . . H33 H 0.4114 -0.1151 0.0074 0.058 Uiso 1 1 calc R . . C32 C 0.41579(11) 0.0882(2) -0.00603(9) 0.0347(4) Uani 1 1 d . . . H32 H 0.4027 0.0993 -0.0479 0.042 Uiso 1 1 calc R . . C31 C 0.43339(11) 0.1887(2) 0.03576(11) 0.0370(5) Uani 1 1 d . . . H31 H 0.4339 0.2794 0.0272 0.044 Uiso 1 1 calc R . . C39 C 0.29165(12) 0.0231(3) 0.36666(10) 0.0394(5) Uani 1 1 d . . . H39 H 0.2434 0.0229 0.3518 0.047 Uiso 1 1 calc R . . C38 C 0.33302(15) 0.1337(3) 0.38078(10) 0.0429(5) Uani 1 1 d . . . H38 H 0.3177 0.2217 0.3771 0.051 Uiso 1 1 calc R . . C37 C 0.40101(14) 0.0918(4) 0.40129(10) 0.0557(8) Uani 1 1 d . . . H37 H 0.4398 0.1466 0.4138 0.067 Uiso 1 1 calc R . . C36 C 0.40177(17) -0.0439(4) 0.40019(11) 0.0623(10) Uani 1 1 d . . . H36 H 0.4412 -0.0976 0.4121 0.075 Uiso 1 1 calc R . . C35 C 0.33436(19) -0.0880(3) 0.37847(12) 0.0551(8) Uani 1 1 d . . . H35 H 0.3202 -0.1763 0.3728 0.066 Uiso 1 1 calc R . . C40 C 0.16712(16) 0.5814(3) 0.16299(11) 0.0470(6) Uani 1 1 d . . . H40A H 0.2112 0.5331 0.1693 0.071 Uiso 1 1 calc R . . H40B H 0.1292 0.5256 0.1732 0.071 Uiso 1 1 calc R . . H40C H 0.1706 0.6591 0.1885 0.071 Uiso 1 1 calc R . . C41 C 0.15242(11) 0.6214(2) 0.09882(10) 0.0335(4) Uani 1 1 d . . . C42 C 0.14085(17) 0.5158(3) 0.05294(12) 0.0492(6) Uani 1 1 d . . . H42A H 0.0908 0.507 0.0396 0.074 Uiso 1 1 calc R . . H42B H 0.159 0.4333 0.0705 0.074 Uiso 1 1 calc R . . H42C H 0.1652 0.5378 0.0186 0.074 Uiso 1 1 calc R . . N1 N 0.12105(8) 0.09585(15) 0.14981(7) 0.0231(3) Uani 1 1 d . . . F7 F 0.40215(8) 0.42188(14) 0.34238(7) 0.0434(3) Uani 1 1 d . . . F8 F 0.32596(11) 0.5638(2) 0.37538(7) 0.0666(5) Uani 1 1 d . . . F9 F 0.29687(7) 0.64035(15) 0.28229(7) 0.0455(3) Uani 1 1 d . . . F10 F 0.37161(10) 0.49489(19) 0.24800(7) 0.0586(4) Uani 1 1 d . . . F11 F 0.28903(9) 0.42400(17) 0.30059(10) 0.0621(5) Uani 1 1 d . . . F12 F 0.40994(8) 0.63635(16) 0.32091(9) 0.0612(5) Uani 1 1 d . . . P2 P 0.34909(3) 0.53103(5) 0.31207(2) 0.02854(10) Uani 1 1 d . . . Ru1 Ru -0.056048(7) 0.128567(16) 0.132431(7) 0.02580(4) Uani 1 1 d . . . Ru2 Ru 0.341738(7) 0.086850(15) 0.058984(6) 0.02205(4) Uani 1 1 d . . . Ru3 Ru 0.375796(7) 0.028273(15) 0.309498(6) 0.02268(4) Uani 1 1 d . . . O1 O 0.14953(12) 0.73478(17) 0.08443(9) 0.0521(5) Uani 1 1 d . . . P3 P 0.37284(3) 0.58647(6) 0.07499(3) 0.03364(11) Uani 1 1 d DU . . F13 F 0.42163(18) 0.4832(3) 0.11306(15) 0.0637(8) Uani 0.838(6) 1 d PDU A 1 F14 F 0.3967(2) 0.6933(4) 0.12530(17) 0.0777(11) Uani 0.838(6) 1 d PDU A 1 F15 F 0.32478(19) 0.6905(3) 0.03763(16) 0.0743(9) Uani 0.838(6) 1 d PDU A 1 F16 F 0.34847(19) 0.4777(4) 0.02623(16) 0.0490(8) Uani 0.838(6) 1 d PDU A 1 F17 F 0.30966(14) 0.5451(4) 0.11058(12) 0.0717(9) Uani 0.838(6) 1 d PDU A 1 F18 F 0.43479(13) 0.6278(4) 0.03952(12) 0.0670(8) Uani 0.838(6) 1 d PDU A 1 F13' F 0.3257(9) 0.495(2) 0.0306(9) 0.057(5) Uani 0.162(6) 1 d PDU A 2 F14' F 0.4385(6) 0.539(2) 0.0404(6) 0.068(4) Uani 0.162(6) 1 d PDU A 2 F15' F 0.4241(9) 0.6825(17) 0.1142(7) 0.066(5) Uani 0.162(6) 1 d PDU A 2 F16' F 0.3115(7) 0.633(2) 0.1062(7) 0.086(4) Uani 0.162(6) 1 d PDU A 2 F17' F 0.3881(11) 0.4674(15) 0.1191(7) 0.074(5) Uani 0.162(6) 1 d PDU A 2 F18' F 0.3602(9) 0.6952(13) 0.0250(6) 0.062(4) Uani 0.162(6) 1 d PDU A 2 P1 P 0.08364(4) 0.13184(6) 0.37702(3) 0.03911(13) Uani 1 1 d U . . F1 F 0.1333(2) 0.0169(8) 0.4063(3) 0.0538(10) Uani 0.839(5) 1 d PU B 1 F2 F 0.0690(2) 0.1829(4) 0.44019(11) 0.0930(11) Uani 0.839(5) 1 d PU B 1 F3 F 0.04047(18) 0.2497(4) 0.34474(18) 0.0599(8) Uani 0.839(5) 1 d PU B 1 F4 F 0.1030(2) 0.0842(3) 0.31324(13) 0.0657(8) Uani 0.839(5) 1 d PU B 1 F5 F 0.01870(16) 0.0415(4) 0.3707(2) 0.0803(10) Uani 0.839(5) 1 d PU B 1 F6 F 0.15214(16) 0.2244(3) 0.38237(17) 0.0816(10) Uani 0.839(5) 1 d PU B 1 F1' F 0.1168(13) 0.017(4) 0.4108(16) 0.048(3) Uani 0.161(5) 1 d PU B 2 F2' F 0.0350(8) 0.1012(18) 0.4318(7) 0.073(3) Uani 0.161(5) 1 d PU B 2 F3' F 0.0164(9) 0.2251(18) 0.3527(9) 0.052(3) Uani 0.161(5) 1 d PU B 2 F4' F 0.1147(10) 0.1371(17) 0.3224(8) 0.064(3) Uani 0.161(5) 1 d PU B 2 F5' F 0.0291(9) 0.0179(15) 0.3421(8) 0.065(3) Uani 0.161(5) 1 d PU B 2 F6' F 0.1218(10) 0.2270(16) 0.4144(8) 0.081(3) Uani 0.161(5) 1 d PU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.0197(7) 0.0217(8) 0.0197(7) -0.0005(6) 0.0062(6) -0.0004(6) C4 0.0209(7) 0.0293(9) 0.0254(8) -0.0024(7) 0.0063(6) -0.0043(7) C3 0.0203(8) 0.0426(11) 0.0256(8) -0.0023(8) 0.0046(6) -0.0012(7) C2 0.0231(8) 0.0401(11) 0.0252(8) 0.0003(8) 0.0055(7) 0.0096(8) C1 0.0265(8) 0.0257(9) 0.0228(8) 0.0011(6) 0.0066(6) 0.0073(7) C14 0.0203(7) 0.0215(8) 0.0191(7) -0.0003(6) 0.0058(6) 0.0015(6) C9 0.0207(7) 0.0164(7) 0.0234(7) -0.0006(6) 0.0049(6) -0.0005(6) C13 0.0170(7) 0.0216(8) 0.0225(7) 0.0002(6) 0.0046(6) -0.0006(6) C8 0.0224(8) 0.0331(10) 0.0253(8) -0.0056(7) 0.0032(6) -0.0042(7) C7 0.0239(9) 0.0541(13) 0.0230(8) -0.0004(8) -0.0014(7) -0.0035(8) C6 0.0252(9) 0.0481(12) 0.0274(9) 0.0130(9) 0.0015(7) 0.0058(8) C5 0.0221(8) 0.0284(9) 0.0322(9) 0.0094(7) 0.0055(7) 0.0043(7) C12 0.0163(7) 0.0216(8) 0.0250(8) 0.0020(6) 0.0045(6) 0.0002(6) C10 0.0197(7) 0.0164(7) 0.0261(8) -0.0006(6) 0.0056(6) -0.0006(6) C16 0.0203(7) 0.0185(8) 0.0261(8) -0.0024(6) 0.0071(6) 0.0003(6) C15 0.0197(7) 0.0186(7) 0.0242(7) 0.0024(6) 0.0058(6) 0.0002(6) C18 0.0203(7) 0.0189(8) 0.0311(9) 0.0036(6) 0.0052(6) -0.0009(6) C17 0.0210(7) 0.0191(8) 0.0353(9) -0.0008(7) 0.0073(7) 0.0018(6) C19 0.0180(7) 0.0291(9) 0.0250(8) 0.0028(7) 0.0081(6) 0.0014(6) C24 0.0233(8) 0.0327(10) 0.0261(8) -0.0033(7) 0.0075(7) 0.0001(7) C23 0.0260(9) 0.0498(13) 0.0261(9) -0.0077(9) 0.0051(7) -0.0013(8) C22 0.0301(10) 0.0634(16) 0.0266(9) 0.0048(10) 0.0010(8) 0.0050(10) C21 0.0287(9) 0.0485(13) 0.0385(11) 0.0163(10) 0.0057(8) 0.0089(9) C20 0.0246(8) 0.0309(10) 0.0365(10) 0.0084(8) 0.0073(7) 0.0023(7) C29 0.077(2) 0.086(2) 0.0525(17) 0.0247(17) 0.0453(17) 0.0317(19) C28 0.085(2) 0.0537(18) 0.087(2) -0.0229(17) 0.068(2) -0.0267(17) C27 0.0255(11) 0.102(3) 0.0560(16) -0.0216(17) 0.0173(11) -0.0017(13) C26 0.0653(17) 0.0463(15) 0.0611(17) -0.0093(13) 0.0378(15) 0.0065(13) C25 0.0440(14) 0.100(3) 0.0369(12) -0.0210(15) 0.0173(11) -0.0158(15) C30 0.0188(9) 0.100(2) 0.0307(10) -0.0091(12) 0.0045(8) -0.0057(11) C34 0.0261(10) 0.085(2) 0.0610(16) 0.0442(16) 0.0195(11) 0.0207(12) C33 0.0361(12) 0.0346(12) 0.0799(19) -0.0042(12) 0.0308(12) 0.0028(9) C32 0.0290(9) 0.0518(13) 0.0255(9) -0.0006(9) 0.0124(7) -0.0015(9) C31 0.0273(9) 0.0397(12) 0.0469(12) -0.0021(10) 0.0158(9) -0.0070(8) C39 0.0304(10) 0.0639(16) 0.0261(9) -0.0005(10) 0.0122(8) -0.0019(10) C38 0.0596(15) 0.0423(13) 0.0315(10) -0.0061(9) 0.0236(10) 0.0037(11) C37 0.0420(13) 0.102(3) 0.0241(10) -0.0170(13) 0.0075(9) -0.0134(14) C36 0.0608(17) 0.103(3) 0.0260(11) 0.0216(13) 0.0146(11) 0.0431(18) C35 0.096(2) 0.0374(13) 0.0399(13) 0.0043(10) 0.0399(15) -0.0005(14) C40 0.0678(17) 0.0423(14) 0.0332(11) 0.0006(10) 0.0149(11) -0.0024(12) C41 0.0345(10) 0.0301(10) 0.0363(10) -0.0005(8) 0.0065(8) -0.0001(8) C42 0.0688(18) 0.0365(13) 0.0393(12) -0.0053(10) -0.0045(12) 0.0050(12) N1 0.0199(6) 0.0186(7) 0.0310(7) 0.0018(6) 0.0038(6) 0.0000(5) F7 0.0481(8) 0.0363(7) 0.0447(8) 0.0037(6) 0.0016(6) 0.0143(6) F8 0.0864(13) 0.0817(13) 0.0339(8) -0.0010(8) 0.0169(8) 0.0377(11) F9 0.0332(7) 0.0440(8) 0.0575(9) 0.0099(7) -0.0015(6) 0.0094(6) F10 0.0638(10) 0.0769(12) 0.0375(8) 0.0025(8) 0.0164(7) 0.0186(9) F11 0.0468(9) 0.0459(9) 0.0925(14) -0.0016(9) 0.0042(9) -0.0145(7) F12 0.0378(8) 0.0413(9) 0.0981(14) 0.0068(9) -0.0153(8) -0.0076(6) P2 0.0261(2) 0.0281(2) 0.0316(2) -0.00003(19) 0.00441(18) 0.00169(18) Ru1 0.01969(7) 0.03145(8) 0.02719(7) -0.00205(6) 0.00662(5) 0.00025(5) Ru2 0.01916(6) 0.02795(8) 0.01959(6) 0.00293(5) 0.00458(5) 0.00059(5) Ru3 0.02170(7) 0.02761(8) 0.01922(6) -0.00069(5) 0.00450(5) 0.00248(5) O1 0.0764(14) 0.0287(9) 0.0507(10) 0.0026(8) 0.0062(9) -0.0006(8) P3 0.0352(3) 0.0317(3) 0.0340(3) -0.0042(2) 0.0044(2) -0.0001(2) F13 0.0687(18) 0.0579(16) 0.0588(14) 0.0107(11) -0.0131(14) 0.0120(14) F14 0.111(3) 0.0574(17) 0.0627(17) -0.0300(13) 0.0037(18) -0.0194(19) F15 0.074(2) 0.0507(14) 0.092(2) 0.0058(13) -0.0107(16) 0.0255(15) F16 0.072(2) 0.0399(12) 0.0354(10) -0.0080(8) 0.0083(13) -0.0090(14) F17 0.0646(14) 0.091(2) 0.0667(14) -0.0188(15) 0.0368(12) -0.0184(15) F18 0.0542(13) 0.085(2) 0.0656(14) 0.0037(14) 0.0214(11) -0.0220(14) F13' 0.060(9) 0.048(8) 0.059(8) 0.005(6) -0.003(7) -0.024(7) F14' 0.051(6) 0.095(10) 0.059(6) -0.017(7) 0.010(5) 0.015(7) F15' 0.080(9) 0.061(7) 0.046(7) -0.013(6) -0.031(7) 0.009(7) F16' 0.063(7) 0.098(10) 0.104(9) -0.035(9) 0.038(6) 0.001(8) F17' 0.105(11) 0.056(7) 0.052(7) 0.013(5) -0.020(8) -0.009(8) F18' 0.082(8) 0.045(6) 0.054(6) 0.010(5) -0.015(6) -0.015(6) P1 0.0480(3) 0.0373(3) 0.0320(3) 0.0023(2) 0.0050(2) 0.0079(3) F1 0.049(2) 0.0592(14) 0.0545(17) 0.0211(12) 0.0096(16) 0.0174(19) F2 0.148(3) 0.090(2) 0.0447(12) -0.0054(13) 0.0258(15) 0.045(2) F3 0.069(2) 0.0422(16) 0.0648(16) 0.0026(12) -0.0075(15) 0.0181(14) F4 0.108(2) 0.0549(17) 0.0378(11) -0.0011(11) 0.0209(12) 0.0199(16) F5 0.0497(13) 0.071(2) 0.121(3) 0.019(2) 0.0170(16) -0.0096(13) F6 0.0704(17) 0.0617(15) 0.105(2) 0.0142(15) -0.0163(15) -0.0209(13) F1' 0.049(7) 0.052(5) 0.042(5) 0.014(5) 0.005(6) 0.010(7) F2' 0.072(5) 0.088(5) 0.066(5) 0.015(5) 0.036(4) 0.021(5) F3' 0.062(7) 0.034(5) 0.056(5) 0.000(4) -0.008(5) 0.016(5) F4' 0.082(6) 0.069(7) 0.049(5) 0.019(5) 0.039(5) 0.015(6) F5' 0.054(5) 0.043(5) 0.089(7) -0.004(5) -0.021(5) 0.005(4) F6' 0.086(5) 0.071(5) 0.078(5) -0.014(5) -0.020(5) -0.002(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C11 C4 1.416(2) . ? C11 C14 1.420(2) . ? C11 C10 1.508(2) . ? C11 Ru3 2.2490(17) . ? C4 C3 1.422(3) . ? C4 Ru3 2.2075(19) . ? C4 H4 0.95 . ? C3 C2 1.414(3) . ? C3 Ru3 2.1908(19) . ? C3 H3 0.95 . ? C2 C1 1.418(3) . ? C2 Ru3 2.1865(18) . ? C2 H2 0.95 . ? C1 C14 1.415(2) . ? C1 Ru3 2.2234(18) . ? C1 H1 0.95 . ? C14 C9 1.513(2) . ? C14 Ru3 2.2655(17) . ? C9 C13 1.520(2) . ? C9 C15 1.565(2) . ? C9 H9 1 . ? C13 C8 1.413(2) . ? C13 C12 1.421(2) . ? C13 Ru2 2.2397(17) . ? C8 C7 1.419(3) . ? C8 Ru2 2.2112(19) . ? C8 H8 0.95 . ? C7 C6 1.414(3) . ? C7 Ru2 2.1970(19) . ? C7 H7 0.95 . ? C6 C5 1.418(3) . ? C6 Ru2 2.2019(19) . ? C6 H6 0.95 . ? C5 C12 1.412(2) . ? C5 Ru2 2.2123(19) . ? C5 H5 0.95 . ? C12 C10 1.515(2) . ? C12 Ru2 2.2304(17) . ? C10 C16 1.561(2) . ? C10 H10 1 . ? C16 C17 1.540(2) . ? C16 C15 1.565(2) . ? C16 H16 1 . ? C15 C18 1.529(2) . ? C15 H15 1 . ? C18 N1 1.464(2) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C17 N1 1.462(2) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C19 N1 1.366(2) . ? C19 C20 1.427(3) . ? C19 C24 1.429(3) . ? C19 Ru1 2.3190(17) . ? C24 C23 1.416(3) . ? C24 Ru1 2.2120(19) . ? C24 H24 0.95 . ? C23 C22 1.411(4) . ? C23 Ru1 2.186(2) . ? C23 H23 0.95 . ? C22 C21 1.407(4) . ? C22 Ru1 2.201(2) . ? C22 H22 0.95 . ? C21 C20 1.424(3) . ? C21 Ru1 2.201(2) . ? C21 H21 0.95 . ? C20 Ru1 2.209(2) . ? C20 H20 0.95 . ? C29 C25 1.387(5) . ? C29 C28 1.398(6) . ? C29 Ru1 2.170(3) . ? C29 H29 0.95 . ? C28 C27 1.382(5) . ? C28 Ru1 2.168(3) . ? C28 H28 0.95 . ? C27 C26 1.413(4) . ? C27 Ru1 2.170(2) . ? C27 H27 0.95 . ? C26 C25 1.398(5) . ? C26 Ru1 2.173(2) . ? C26 H26 0.95 . ? C25 Ru1 2.177(3) . ? C25 H25 0.95 . ? C30 C31 1.407(4) . ? C30 C34 1.412(5) . ? C30 Ru2 2.179(2) . ? C30 H30 0.95 . ? C34 C33 1.408(4) . ? C34 Ru2 2.177(2) . ? C34 H34 0.95 . ? C33 C32 1.406(4) . ? C33 Ru2 2.170(2) . ? C33 H33 0.95 . ? C32 C31 1.407(3) . ? C32 Ru2 2.1740(19) . ? C32 H32 0.95 . ? C31 Ru2 2.177(2) . ? C31 H31 0.95 . ? C39 C38 1.400(4) . ? C39 C35 1.412(4) . ? C39 Ru3 2.200(2) . ? C39 H39 0.95 . ? C38 C37 1.402(4) . ? C38 Ru3 2.183(2) . ? C38 H38 0.95 . ? C37 C36 1.392(5) . ? C37 Ru3 2.161(2) . ? C37 H37 0.95 . ? C36 C35 1.406(5) . ? C36 Ru3 2.168(2) . ? C36 H36 0.95 . ? C35 Ru3 2.189(2) . ? C35 H35 0.95 . ? C40 C41 1.493(3) . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 O1 1.206(3) . ? C41 C42 1.494(3) . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? F7 P2 1.6091(14) . ? F8 P2 1.5831(16) . ? F9 P2 1.5969(14) . ? F10 P2 1.6024(16) . ? F11 P2 1.5939(17) . ? F12 P2 1.5901(16) . ? P3 F16' 1.529(10) . ? P3 F13' 1.573(14) . ? P3 F17' 1.578(12) . ? P3 F18 1.580(2) . ? P3 F18' 1.580(11) . ? P3 F15' 1.583(13) . ? P3 F15 1.583(3) . ? P3 F13 1.593(3) . ? P3 F16 1.593(3) . ? P3 F14 1.601(3) . ? P3 F17 1.601(2) . ? P3 F14' 1.645(10) . ? P1 F6' 1.431(14) . ? P1 F4' 1.436(15) . ? P1 F1' 1.50(4) . ? P1 F5 1.551(3) . ? P1 F2 1.574(2) . ? P1 F3 1.590(4) . ? P1 F4 1.606(3) . ? P1 F1 1.606(7) . ? P1 F6 1.620(3) . ? P1 F3' 1.648(18) . ? P1 F2' 1.672(12) . ? P1 F5' 1.697(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 C4 C11 C14 120.34(16) . . ? C4 C11 C10 126.20(16) . . ? C14 C11 C10 113.43(15) . . ? C4 C11 Ru3 69.89(10) . . ? C14 C11 Ru3 72.30(10) . . ? C10 C11 Ru3 132.40(11) . . ? C11 C4 C3 119.23(18) . . ? C11 C4 Ru3 73.08(10) . . ? C3 C4 Ru3 70.50(11) . . ? C11 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? Ru3 C4 H4 128.1 . . ? C2 C3 C4 120.05(17) . . ? C2 C3 Ru3 70.99(11) . . ? C4 C3 Ru3 71.78(11) . . ? C2 C3 H3 120 . . ? C4 C3 H3 120 . . ? Ru3 C3 H3 129.7 . . ? C3 C2 C1 120.86(17) . . ? C3 C2 Ru3 71.32(11) . . ? C1 C2 Ru3 72.67(10) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? Ru3 C2 H2 128.8 . . ? C14 C1 C2 118.91(18) . . ? C14 C1 Ru3 73.25(10) . . ? C2 C1 Ru3 69.84(11) . . ? C14 C1 H1 120.5 . . ? C2 C1 H1 120.5 . . ? Ru3 C1 H1 128.5 . . ? C1 C14 C11 120.53(16) . . ? C1 C14 C9 126.32(16) . . ? C11 C14 C9 113.13(15) . . ? C1 C14 Ru3 70.02(10) . . ? C11 C14 Ru3 71.04(10) . . ? C9 C14 Ru3 133.07(11) . . ? C14 C9 C13 106.94(14) . . ? C14 C9 C15 107.16(14) . . ? C13 C9 C15 106.17(13) . . ? C14 C9 H9 112.1 . . ? C13 C9 H9 112.1 . . ? C15 C9 H9 112.1 . . ? C8 C13 C12 120.11(16) . . ? C8 C13 C9 126.81(16) . . ? C12 C13 C9 113.02(15) . . ? C8 C13 Ru2 70.39(10) . . ? C12 C13 Ru2 71.11(10) . . ? C9 C13 Ru2 133.51(11) . . ? C13 C8 C7 119.20(19) . . ? C13 C8 Ru2 72.58(10) . . ? C7 C8 Ru2 70.68(11) . . ? C13 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? Ru2 C8 H8 128.5 . . ? C6 C7 C8 120.57(18) . . ? C6 C7 Ru2 71.43(11) . . ? C8 C7 Ru2 71.76(11) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? Ru2 C7 H7 129.6 . . ? C7 C6 C5 120.23(18) . . ? C7 C6 Ru2 71.06(12) . . ? C5 C6 Ru2 71.66(11) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? Ru2 C6 H6 129.9 . . ? C12 C5 C6 119.19(19) . . ? C12 C5 Ru2 72.17(10) . . ? C6 C5 Ru2 70.86(12) . . ? C12 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? Ru2 C5 H5 128.8 . . ? C5 C12 C13 120.65(17) . . ? C5 C12 C10 125.97(17) . . ? C13 C12 C10 113.24(15) . . ? C5 C12 Ru2 70.78(10) . . ? C13 C12 Ru2 71.82(10) . . ? C10 C12 Ru2 133.81(11) . . ? C11 C10 C12 106.63(14) . . ? C11 C10 C16 108.47(14) . . ? C12 C10 C16 105.45(13) . . ? C11 C10 H10 112 . . ? C12 C10 H10 112 . . ? C16 C10 H10 112 . . ? C17 C16 C10 112.52(14) . . ? C17 C16 C15 105.21(14) . . ? C10 C16 C15 109.60(13) . . ? C17 C16 H16 109.8 . . ? C10 C16 H16 109.8 . . ? C15 C16 H16 109.8 . . ? C18 C15 C9 113.10(14) . . ? C18 C15 C16 105.62(14) . . ? C9 C15 C16 109.58(13) . . ? C18 C15 H15 109.5 . . ? C9 C15 H15 109.5 . . ? C16 C15 H15 109.5 . . ? N1 C18 C15 104.25(14) . . ? N1 C18 H18A 110.9 . . ? C15 C18 H18A 110.9 . . ? N1 C18 H18B 110.9 . . ? C15 C18 H18B 110.9 . . ? H18A C18 H18B 108.9 . . ? N1 C17 C16 104.73(14) . . ? N1 C17 H17A 110.8 . . ? C16 C17 H17A 110.8 . . ? N1 C17 H17B 110.8 . . ? C16 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? N1 C19 C20 121.22(17) . . ? N1 C19 C24 121.13(17) . . ? C20 C19 C24 117.51(17) . . ? N1 C19 Ru1 133.77(13) . . ? C20 C19 Ru1 67.47(10) . . ? C24 C19 Ru1 67.60(10) . . ? C23 C24 C19 120.9(2) . . ? C23 C24 Ru1 70.24(12) . . ? C19 C24 Ru1 75.74(11) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? Ru1 C24 H24 126.4 . . ? C22 C23 C24 120.2(2) . . ? C22 C23 Ru1 71.80(13) . . ? C24 C23 Ru1 72.20(11) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? Ru1 C23 H23 128.3 . . ? C21 C22 C23 119.74(19) . . ? C21 C22 Ru1 71.36(13) . . ? C23 C22 Ru1 70.67(12) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? Ru1 C22 H22 130.4 . . ? C22 C21 C20 120.2(2) . . ? C22 C21 Ru1 71.37(13) . . ? C20 C21 Ru1 71.46(12) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? Ru1 C21 H21 129.7 . . ? C21 C20 C19 120.7(2) . . ? C21 C20 Ru1 70.87(12) . . ? C19 C20 Ru1 75.89(11) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? Ru1 C20 H20 125.3 . . ? C25 C29 C28 108.1(3) . . ? C25 C29 Ru1 71.66(17) . . ? C28 C29 Ru1 71.10(18) . . ? C25 C29 H29 126 . . ? C28 C29 H29 126 . . ? Ru1 C29 H29 122.9 . . ? C27 C28 C29 108.3(3) . . ? C27 C28 Ru1 71.51(16) . . ? C29 C28 Ru1 71.28(16) . . ? C27 C28 H28 125.9 . . ? C29 C28 H28 125.9 . . ? Ru1 C28 H28 123 . . ? C28 C27 C26 108.1(3) . . ? C28 C27 Ru1 71.34(15) . . ? C26 C27 Ru1 71.13(14) . . ? C28 C27 H27 126 . . ? C26 C27 H27 126 . . ? Ru1 C27 H27 123.2 . . ? C25 C26 C27 107.2(3) . . ? C25 C26 Ru1 71.41(15) . . ? C27 C26 Ru1 70.90(15) . . ? C25 C26 H26 126.4 . . ? C27 C26 H26 126.4 . . ? Ru1 C26 H26 123 . . ? C29 C25 C26 108.4(3) . . ? C29 C25 Ru1 71.12(17) . . ? C26 C25 Ru1 71.09(15) . . ? C29 C25 H25 125.8 . . ? C26 C25 H25 125.8 . . ? Ru1 C25 H25 123.6 . . ? C31 C30 C34 108.1(2) . . ? C31 C30 Ru2 71.04(12) . . ? C34 C30 Ru2 71.00(14) . . ? C31 C30 H30 125.9 . . ? C34 C30 H30 125.9 . . ? Ru2 C30 H30 123.7 . . ? C33 C34 C30 107.9(2) . . ? C33 C34 Ru2 70.82(14) . . ? C30 C34 Ru2 71.18(14) . . ? C33 C34 H34 126.1 . . ? C30 C34 H34 126.1 . . ? Ru2 C34 H34 123.6 . . ? C32 C33 C34 107.9(2) . . ? C32 C33 Ru2 71.28(13) . . ? C34 C33 Ru2 71.38(14) . . ? C32 C33 H33 126 . . ? C34 C33 H33 126 . . ? Ru2 C33 H33 123 . . ? C33 C32 C31 108.3(2) . . ? C33 C32 Ru2 70.94(12) . . ? C31 C32 Ru2 71.22(11) . . ? C33 C32 H32 125.8 . . ? C31 C32 H32 125.8 . . ? Ru2 C32 H32 123.6 . . ? C32 C31 C30 107.7(2) . . ? C32 C31 Ru2 71.02(12) . . ? C30 C31 Ru2 71.25(13) . . ? C32 C31 H31 126.1 . . ? C30 C31 H31 126.1 . . ? Ru2 C31 H31 123.2 . . ? C38 C39 C35 108.0(2) . . ? C38 C39 Ru3 70.73(12) . . ? C35 C39 Ru3 70.83(13) . . ? C38 C39 H39 126 . . ? C35 C39 H39 126 . . ? Ru3 C39 H39 124 . . ? C39 C38 C37 108.0(3) . . ? C39 C38 Ru3 72.00(13) . . ? C37 C38 Ru3 70.32(13) . . ? C39 C38 H38 126 . . ? C37 C38 H38 126 . . ? Ru3 C38 H38 123.3 . . ? C36 C37 C38 108.2(3) . . ? C36 C37 Ru3 71.52(15) . . ? C38 C37 Ru3 72.02(13) . . ? C36 C37 H37 125.9 . . ? C38 C37 H37 125.9 . . ? Ru3 C37 H37 122.2 . . ? C37 C36 C35 108.5(2) . . ? C37 C36 Ru3 70.96(15) . . ? C35 C36 Ru3 71.98(14) . . ? C37 C36 H36 125.8 . . ? C35 C36 H36 125.8 . . ? Ru3 C36 H36 122.9 . . ? C36 C35 C39 107.4(3) . . ? C36 C35 Ru3 70.39(15) . . ? C39 C35 Ru3 71.64(13) . . ? C36 C35 H35 126.3 . . ? C39 C35 H35 126.3 . . ? Ru3 C35 H35 123.3 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O1 C41 C40 121.4(2) . . ? O1 C41 C42 121.1(2) . . ? C40 C41 C42 117.5(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C19 N1 C17 121.78(15) . . ? C19 N1 C18 120.76(15) . . ? C17 N1 C18 109.00(14) . . ? F8 P2 F12 91.90(12) . . ? F8 P2 F11 90.46(12) . . ? F12 P2 F11 177.64(12) . . ? F8 P2 F9 89.59(9) . . ? F12 P2 F9 89.57(8) . . ? F11 P2 F9 90.46(9) . . ? F8 P2 F10 178.74(12) . . ? F12 P2 F10 89.30(11) . . ? F11 P2 F10 88.35(11) . . ? F9 P2 F10 90.84(9) . . ? F8 P2 F7 90.23(9) . . ? F12 P2 F7 89.95(9) . . ? F11 P2 F7 90.03(9) . . ? F9 P2 F7 179.48(10) . . ? F10 P2 F7 89.35(9) . . ? C28 Ru1 C27 37.15(14) . . ? C28 Ru1 C29 37.62(15) . . ? C27 Ru1 C29 62.55(13) . . ? C28 Ru1 C26 62.82(12) . . ? C27 Ru1 C26 37.97(12) . . ? C29 Ru1 C26 62.67(12) . . ? C28 Ru1 C25 62.53(12) . . ? C27 Ru1 C25 62.73(11) . . ? C29 Ru1 C25 37.22(14) . . ? C26 Ru1 C25 37.50(12) . . ? C28 Ru1 C23 107.49(10) . . ? C27 Ru1 C23 118.29(10) . . ? C29 Ru1 C23 126.87(13) . . ? C26 Ru1 C23 152.31(11) . . ? C25 Ru1 C23 163.47(13) . . ? C28 Ru1 C21 151.75(14) . . ? C27 Ru1 C21 118.72(12) . . ? C29 Ru1 C21 164.39(14) . . ? C26 Ru1 C21 107.93(11) . . ? C25 Ru1 C21 127.79(12) . . ? C23 Ru1 C21 67.50(10) . . ? C28 Ru1 C22 122.73(13) . . ? C27 Ru1 C22 107.85(10) . . ? C29 Ru1 C22 158.10(14) . . ? C26 Ru1 C22 123.20(11) . . ? C25 Ru1 C22 158.71(13) . . ? C23 Ru1 C22 37.53(9) . . ? C21 Ru1 C22 37.28(10) . . ? C28 Ru1 C20 169.57(13) . . ? C27 Ru1 C20 145.51(12) . . ? C29 Ru1 C20 132.00(13) . . ? C26 Ru1 C20 113.85(10) . . ? C25 Ru1 C20 108.45(10) . . ? C23 Ru1 C20 79.93(8) . . ? C21 Ru1 C20 37.67(8) . . ? C22 Ru1 C20 67.62(9) . . ? C28 Ru1 C24 114.22(11) . . ? C27 Ru1 C24 145.15(11) . . ? C29 Ru1 C24 108.23(10) . . ? C26 Ru1 C24 169.18(10) . . ? C25 Ru1 C24 131.69(11) . . ? C23 Ru1 C24 37.56(7) . . ? C21 Ru1 C24 79.51(8) . . ? C22 Ru1 C24 67.48(8) . . ? C20 Ru1 C24 67.05(8) . . ? C28 Ru1 C19 139.11(13) . . ? C27 Ru1 C19 173.64(10) . . ? C29 Ru1 C19 111.44(11) . . ? C26 Ru1 C19 138.56(10) . . ? C25 Ru1 C19 111.36(9) . . ? C23 Ru1 C19 66.58(7) . . ? C21 Ru1 C19 66.40(7) . . ? C22 Ru1 C19 78.51(7) . . ? C20 Ru1 C19 36.64(7) . . ? C24 Ru1 C19 36.66(7) . . ? C33 Ru2 C32 37.78(10) . . ? C33 Ru2 C31 63.32(9) . . ? C32 Ru2 C31 37.75(9) . . ? C33 Ru2 C34 37.80(12) . . ? C32 Ru2 C34 63.07(9) . . ? C31 Ru2 C34 63.24(10) . . ? C33 Ru2 C30 63.21(11) . . ? C32 Ru2 C30 62.97(8) . . ? C31 Ru2 C30 37.70(10) . . ? C34 Ru2 C30 37.82(12) . . ? C33 Ru2 C7 110.62(10) . . ? C32 Ru2 C7 107.36(8) . . ? C31 Ru2 C7 133.40(9) . . ? C34 Ru2 C7 141.17(12) . . ? C30 Ru2 C7 170.18(8) . . ? C33 Ru2 C6 133.84(11) . . ? C32 Ru2 C6 107.65(8) . . ? C31 Ru2 C6 110.64(9) . . ? C34 Ru2 C6 170.63(9) . . ? C30 Ru2 C6 140.92(11) . . ? C7 Ru2 C6 37.50(9) . . ? C33 Ru2 C8 106.82(9) . . ? C32 Ru2 C8 128.14(8) . . ? C31 Ru2 C8 165.67(8) . . ? C34 Ru2 C8 116.19(10) . . ? C30 Ru2 C8 149.46(10) . . ? C7 Ru2 C8 37.56(8) . . ? C6 Ru2 C8 67.78(8) . . ? C33 Ru2 C5 166.43(9) . . ? C32 Ru2 C5 128.87(8) . . ? C31 Ru2 C5 107.39(8) . . ? C34 Ru2 C5 149.16(11) . . ? C30 Ru2 C5 116.32(10) . . ? C7 Ru2 C5 67.69(8) . . ? C6 Ru2 C5 37.48(8) . . ? C8 Ru2 C5 80.22(7) . . ? C33 Ru2 C12 156.35(9) . . ? C32 Ru2 C12 161.90(8) . . ? C31 Ru2 C12 126.17(8) . . ? C34 Ru2 C12 122.38(9) . . ? C30 Ru2 C12 109.61(8) . . ? C7 Ru2 C12 79.09(7) . . ? C6 Ru2 C12 66.82(7) . . ? C8 Ru2 C12 67.15(7) . . ? C5 Ru2 C12 37.05(6) . . ? C33 Ru2 C13 125.40(8) . . ? C32 Ru2 C13 161.02(8) . . ? C31 Ru2 C13 157.08(8) . . ? C34 Ru2 C13 109.28(8) . . ? C30 Ru2 C13 122.85(8) . . ? C7 Ru2 C13 66.81(7) . . ? C6 Ru2 C13 79.09(7) . . ? C8 Ru2 C13 37.02(6) . . ? C5 Ru2 C13 67.13(7) . . ? C12 Ru2 C13 37.08(6) . . ? C37 Ru3 C36 37.51(13) . . ? C37 Ru3 C38 37.66(11) . . ? C36 Ru3 C38 62.68(11) . . ? C37 Ru3 C2 118.59(9) . . ? C36 Ru3 C2 103.59(9) . . ? C38 Ru3 C2 154.80(9) . . ? C37 Ru3 C35 62.91(12) . . ? C36 Ru3 C35 37.64(13) . . ? C38 Ru3 C35 62.70(10) . . ? C2 Ru3 C35 120.48(10) . . ? C37 Ru3 C3 102.69(9) . . ? C36 Ru3 C3 112.82(10) . . ? C38 Ru3 C3 124.88(9) . . ? C2 Ru3 C3 37.70(8) . . ? C35 Ru3 C3 147.19(11) . . ? C37 Ru3 C39 62.67(9) . . ? C36 Ru3 C39 62.63(10) . . ? C38 Ru3 C39 37.27(10) . . ? C2 Ru3 C39 157.17(9) . . ? C35 Ru3 C39 37.54(11) . . ? C3 Ru3 C39 162.15(9) . . ? C37 Ru3 C4 110.45(10) . . ? C36 Ru3 C4 140.33(12) . . ? C38 Ru3 C4 108.02(9) . . ? C2 Ru3 C4 67.99(8) . . ? C35 Ru3 C4 170.71(9) . . ? C3 Ru3 C4 37.72(7) . . ? C39 Ru3 C4 134.49(9) . . ? C37 Ru3 C1 149.75(10) . . ? C36 Ru3 C1 117.57(10) . . ? C38 Ru3 C1 166.93(9) . . ? C2 Ru3 C1 37.49(7) . . ? C35 Ru3 C1 108.84(9) . . ? C3 Ru3 C1 67.83(7) . . ? C39 Ru3 C1 130.00(9) . . ? C4 Ru3 C1 80.18(7) . . ? C37 Ru3 C11 137.93(11) . . ? C36 Ru3 C11 175.43(11) . . ? C38 Ru3 C11 113.46(8) . . ? C2 Ru3 C11 79.00(7) . . ? C35 Ru3 C11 143.94(11) . . ? C3 Ru3 C11 66.90(7) . . ? C39 Ru3 C11 116.12(8) . . ? C4 Ru3 C11 37.03(6) . . ? C1 Ru3 C11 66.77(6) . . ? C37 Ru3 C14 173.43(11) . . ? C36 Ru3 C14 147.84(12) . . ? C38 Ru3 C14 136.55(9) . . ? C2 Ru3 C14 66.42(7) . . ? C35 Ru3 C14 119.13(10) . . ? C3 Ru3 C14 78.74(7) . . ? C39 Ru3 C14 114.63(7) . . ? C4 Ru3 C14 66.71(6) . . ? C1 Ru3 C14 36.73(6) . . ? C11 Ru3 C14 36.65(6) . . ? F16' P3 F13' 93.4(9) . . ? F16' P3 F17' 92.7(10) . . ? F13' P3 F17' 89.1(10) . . ? F16' P3 F18 146.1(8) . . ? F13' P3 F18 104.6(8) . . ? F17' P3 F18 115.7(8) . . ? F16' P3 F18' 92.8(9) . . ? F13' P3 F18' 86.8(9) . . ? F17' P3 F18' 173.4(9) . . ? F18 P3 F18' 60.6(7) . . ? F16' P3 F15' 90.9(8) . . ? F13' P3 F15' 174.3(10) . . ? F17' P3 F15' 94.5(9) . . ? F18 P3 F15' 69.8(7) . . ? F18' P3 F15' 89.2(8) . . ? F16' P3 F15 66.2(8) . . ? F13' P3 F15 79.2(8) . . ? F17' P3 F15 154.9(8) . . ? F18 P3 F15 88.94(17) . . ? F15' P3 F15 99.1(7) . . ? F16' P3 F13 113.6(8) . . ? F13' P3 F13 101.5(8) . . ? F18 P3 F13 90.91(16) . . ? F18' P3 F13 151.5(7) . . ? F15' P3 F13 80.2(7) . . ? F15 P3 F13 179.32(19) . . ? F16' P3 F16 111.0(7) . . ? F17' P3 F16 84.6(7) . . ? F18 P3 F16 90.89(17) . . ? F18' P3 F16 89.9(5) . . ? F15' P3 F16 158.2(7) . . ? F15 P3 F16 90.27(19) . . ? F13 P3 F16 90.40(19) . . ? F16' P3 F14 68.3(7) . . ? F13' P3 F14 161.6(7) . . ? F17' P3 F14 94.1(7) . . ? F18 P3 F14 90.32(17) . . ? F18' P3 F14 91.4(5) . . ? F15 P3 F14 90.6(2) . . ? F13 P3 F14 88.7(2) . . ? F16 P3 F14 178.5(2) . . ? F13' P3 F17 75.1(8) . . ? F17' P3 F17 64.7(8) . . ? F18 P3 F17 179.58(17) . . ? F18' P3 F17 119.0(7) . . ? F15' P3 F17 110.4(7) . . ? F15 P3 F17 90.67(18) . . ? F13 P3 F17 89.49(17) . . ? F16 P3 F17 88.98(17) . . ? F14 P3 F17 89.81(17) . . ? F16' P3 F14' 178.7(9) . . ? F13' P3 F14' 86.6(8) . . ? F17' P3 F14' 88.6(9) . . ? F18' P3 F14' 85.9(8) . . ? F15' P3 F14' 89.0(8) . . ? F15 P3 F14' 112.5(6) . . ? F13 P3 F14' 67.6(6) . . ? F16 P3 F14' 69.2(6) . . ? F14 P3 F14' 111.5(5) . . ? F17 P3 F14' 147.4(7) . . ? F6' P1 F4' 103.7(11) . . ? F6' P1 F1' 94.8(16) . . ? F4' P1 F1' 105.3(14) . . ? F6' P1 F5 144.2(9) . . ? F4' P1 F5 111.5(8) . . ? F1' P1 F5 82.2(12) . . ? F6' P1 F2 51.7(9) . . ? F4' P1 F2 154.6(8) . . ? F1' P1 F2 85.4(13) . . ? F5 P1 F2 92.6(2) . . ? F6' P1 F3 87.2(6) . . ? F4' P1 F3 80.4(7) . . ? F1' P1 F3 173.2(10) . . ? F5 P1 F3 92.38(18) . . ? F2 P1 F3 90.86(18) . . ? F6' P1 F4 124.9(9) . . ? F1' P1 F4 94.6(13) . . ? F5 P1 F4 90.9(2) . . ? F2 P1 F4 176.5(2) . . ? F3 P1 F4 89.54(19) . . ? F6' P1 F1 91.3(7) . . ? F4' P1 F1 94.9(7) . . ? F5 P1 F1 91.8(3) . . ? F2 P1 F1 92.3(3) . . ? F3 P1 F1 174.6(3) . . ? F4' P1 F6 67.3(8) . . ? F1' P1 F6 97.6(12) . . ? F5 P1 F6 178.7(2) . . ? F2 P1 F6 88.7(2) . . ? F3 P1 F6 87.94(16) . . ? F4 P1 F6 87.85(19) . . ? F1 P1 F6 87.8(3) . . ? F6' P1 F3' 97.1(9) . . ? F4' P1 F3' 95.3(10) . . ? F1' P1 F3' 152.9(12) . . ? F5 P1 F3' 73.9(6) . . ? F2 P1 F3' 83.2(7) . . ? F4 P1 F3' 98.3(7) . . ? F1 P1 F3' 164.8(7) . . ? F6 P1 F3' 106.6(6) . . ? F6' P1 F2' 89.4(10) . . ? F4' P1 F2' 166.8(10) . . ? F1' P1 F2' 73.9(12) . . ? F5 P1 F2' 55.4(7) . . ? F3 P1 F2' 99.7(5) . . ? F4 P1 F2' 145.0(7) . . ? F1 P1 F2' 85.5(5) . . ? F6 P1 F2' 125.9(7) . . ? F3' P1 F2' 82.0(8) . . ? F6' P1 F5' 170.0(11) . . ? F4' P1 F5' 86.1(10) . . ? F1' P1 F5' 83.8(15) . . ? F2 P1 F5' 118.3(7) . . ? F3 P1 F5' 93.1(5) . . ? F4 P1 F5' 65.1(7) . . ? F1 P1 F5' 89.2(6) . . ? F6 P1 F5' 152.9(7) . . ? F3' P1 F5' 80.2(8) . . ? F2' P1 F5' 80.7(9) . . ? #===END data_B1 _database_code_depnum_ccdc_archive 'CCDC 901527' #TrackingRef 'Gomez.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H32 Cl2 F6 N O4 P Ru' _chemical_formula_weight 835.55 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.2263(14) _cell_length_b 12.5743(10) _cell_length_c 19.0876(16) _cell_angle_alpha 90.00 _cell_angle_beta 109.481(4) _cell_angle_gamma 90.00 _cell_volume 3445.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9406 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 29.12 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8003 _exptl_absorpt_correction_T_max 0.8800 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 kappa APEX-II CCD Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 54869 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 5.17 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8393 _reflns_number_gt 6747 _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^)+(0.0399P)^2^+2.6911P] 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 8393 _refine_ls_number_parameters 554 _refine_ls_number_restraints 290 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.055 _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 0.222264(13) 0.006910(13) 0.460581(9) 0.03306(7) Uani 1 1 d D A . C25 C 0.3669(6) 0.0030(16) 0.4675(6) 0.053(3) Uani 0.50(2) 1 d PDU A 1 H25 H 0.4168 0.0140 0.5127 0.064 Uiso 0.50(2) 1 calc PR A 1 C26 C 0.3213(12) 0.0811(9) 0.4159(10) 0.056(3) Uani 0.50(2) 1 d PDU A 1 H26 H 0.3357 0.1548 0.4196 0.067 Uiso 0.50(2) 1 calc PR A 1 C27 C 0.2512(11) 0.0326(13) 0.3583(6) 0.056(3) Uani 0.50(2) 1 d PDU A 1 H27 H 0.2094 0.0682 0.3166 0.067 Uiso 0.50(2) 1 calc PR A 1 C28 C 0.2521(10) -0.0755(12) 0.3717(7) 0.054(3) Uani 0.50(2) 1 d PDU A 1 H28 H 0.2114 -0.1267 0.3408 0.065 Uiso 0.50(2) 1 calc PR A 1 C29 C 0.3240(12) -0.0963(10) 0.4391(9) 0.055(3) Uani 0.50(2) 1 d PDU A 1 H29 H 0.3410 -0.1641 0.4616 0.066 Uiso 0.50(2) 1 calc PR A 1 C25' C 0.3601(9) 0.0481(13) 0.4574(8) 0.058(3) Uani 0.50(2) 1 d PDU A 2 H25' H 0.4031 0.0923 0.4929 0.069 Uiso 0.50(2) 1 calc PR A 2 C26' C 0.2924(12) 0.0820(11) 0.3921(10) 0.059(4) Uani 0.50(2) 1 d PDU A 2 H26' H 0.2808 0.1537 0.3759 0.071 Uiso 0.50(2) 1 calc PR A 2 C27' C 0.2447(10) -0.0061(16) 0.3548(5) 0.058(3) Uani 0.50(2) 1 d PDU A 2 H27' H 0.1953 -0.0052 0.3086 0.070 Uiso 0.50(2) 1 calc PR A 2 C28' C 0.2812(12) -0.0957(8) 0.3961(10) 0.056(3) Uani 0.50(2) 1 d PDU A 2 H28' H 0.2609 -0.1666 0.3827 0.067 Uiso 0.50(2) 1 calc PR A 2 C29' C 0.3533(9) -0.0654(13) 0.4614(7) 0.055(3) Uani 0.50(2) 1 d PDU A 2 H29' H 0.3899 -0.1107 0.4999 0.066 Uiso 0.50(2) 1 calc PR A 2 N1 N 0.34638(15) 0.09786(16) 0.80721(10) 0.0396(4) Uani 1 1 d . A . O1 O 0.32689(14) 0.27178(14) 0.77066(10) 0.0523(5) Uani 1 1 d . A . O2 O 0.33779(16) -0.08371(15) 0.81474(9) 0.0564(5) Uani 1 1 d . A . O3 O 0.27999(12) 0.26041(12) 0.60175(10) 0.0407(4) Uani 1 1 d . A . O4 O 0.28005(12) -0.16316(11) 0.65429(9) 0.0378(4) Uani 1 1 d . A . C1 C 0.14155(17) 0.1339(2) 0.48921(14) 0.0403(5) Uani 1 1 d . . . H1 H 0.1419 0.2079 0.4792 0.048 Uiso 1 1 calc R A . C2 C 0.07971(18) 0.0650(2) 0.43718(15) 0.0467(6) Uani 1 1 d . A . H2 H 0.0368 0.0933 0.3928 0.056 Uiso 1 1 calc R . . C3 C 0.08123(19) -0.0451(2) 0.45070(14) 0.0468(6) Uani 1 1 d . A . H3 H 0.0398 -0.0908 0.4151 0.056 Uiso 1 1 calc R . . C4 C 0.14404(18) -0.08808(19) 0.51694(13) 0.0390(5) Uani 1 1 d . . . H4 H 0.1461 -0.1626 0.5255 0.047 Uiso 1 1 calc R A . C5 C 0.45089(18) -0.06296(19) 0.67514(13) 0.0399(5) Uani 1 1 d . . . H5 H 0.4513 -0.1373 0.6842 0.048 Uiso 1 1 calc R . . C6 C 0.53369(19) -0.0085(2) 0.68525(16) 0.0484(6) Uani 1 1 d . . . H6 H 0.5911 -0.0461 0.7008 0.058 Uiso 1 1 calc R . . C7 C 0.53320(18) 0.0996(2) 0.67284(15) 0.0473(6) Uani 1 1 d . . . H7 H 0.5903 0.1359 0.6802 0.057 Uiso 1 1 calc R . . C8 C 0.44987(17) 0.15606(19) 0.64971(13) 0.0387(5) Uani 1 1 d . . . H8 H 0.4498 0.2306 0.6416 0.046 Uiso 1 1 calc R . . C9 C 0.27254(16) 0.15367(16) 0.61945(12) 0.0324(5) Uani 1 1 d . . . C10 C 0.27295(16) -0.05265(16) 0.64500(11) 0.0305(4) Uani 1 1 d . . . C11 C 0.20365(16) -0.01923(17) 0.57030(12) 0.0313(4) Uani 1 1 d . A . C12 C 0.36758(16) -0.00705(16) 0.65169(12) 0.0308(4) Uani 1 1 d . A . C13 C 0.36704(15) 0.10199(16) 0.63865(11) 0.0303(4) Uani 1 1 d . A . C14 C 0.20303(16) 0.09140(17) 0.55644(12) 0.0321(4) Uani 1 1 d . A . C15 C 0.24005(17) 0.13144(17) 0.68802(12) 0.0345(5) Uani 1 1 d . A . H15 H 0.1761 0.1606 0.6787 0.041 Uiso 1 1 calc R . . C16 C 0.24166(17) 0.01061(17) 0.70372(12) 0.0335(5) Uani 1 1 d . A . H16 H 0.1789 -0.0140 0.7030 0.040 Uiso 1 1 calc R . . C17 C 0.31291(19) -0.00246(19) 0.78112(13) 0.0400(5) Uani 1 1 d . . . C18 C 0.30778(17) 0.17962(19) 0.75801(13) 0.0390(5) Uani 1 1 d . . . C19 C 0.4163(2) 0.11649(19) 0.87872(13) 0.0444(6) Uani 1 1 d . . . C20 C 0.5057(2) 0.1390(3) 0.88165(16) 0.0600(8) Uani 1 1 d . A . H20 H 0.5216 0.1408 0.8376 0.072 Uiso 1 1 calc R . . C21 C 0.5721(3) 0.1592(3) 0.94995(19) 0.0764(10) Uani 1 1 d . . . H21 H 0.6340 0.1763 0.9528 0.092 Uiso 1 1 calc R A . C22 C 0.5494(3) 0.1545(3) 1.01371(17) 0.0764(11) Uani 1 1 d . A . H22 H 0.5959 0.1671 1.0605 0.092 Uiso 1 1 calc R . . C23 C 0.4610(3) 0.1321(3) 1.00999(16) 0.0784(12) Uani 1 1 d . . . H23 H 0.4458 0.1292 1.0544 0.094 Uiso 1 1 calc R A . C24 C 0.3916(3) 0.1133(2) 0.94143(15) 0.0588(8) Uani 1 1 d . A . H24 H 0.3293 0.0987 0.9385 0.071 Uiso 1 1 calc R . . C30 C 0.2076(2) 0.3313(2) 0.60477(17) 0.0526(7) Uani 1 1 d . . . H30A H 0.2188 0.3551 0.6565 0.063 Uiso 1 1 calc R A . H30B H 0.1463 0.2953 0.5864 0.063 Uiso 1 1 calc R . . C31 C 0.2096(3) 0.4245(2) 0.5560(2) 0.0722(10) Uani 1 1 d . A . H31A H 0.2697 0.4610 0.5760 0.108 Uiso 1 1 calc R . . H31B H 0.1593 0.4740 0.5546 0.108 Uiso 1 1 calc R . . H31C H 0.2012 0.3993 0.5056 0.108 Uiso 1 1 calc R . . C32 C 0.2091(2) -0.21672(19) 0.67568(14) 0.0450(6) Uani 1 1 d . . . H32A H 0.1463 -0.1938 0.6438 0.054 Uiso 1 1 calc R A . H32B H 0.2162 -0.2008 0.7281 0.054 Uiso 1 1 calc R . . C33 C 0.2224(2) -0.3332(2) 0.66584(17) 0.0565(7) Uani 1 1 d . A . H33A H 0.2165 -0.3473 0.6140 0.085 Uiso 1 1 calc R . . H33B H 0.1749 -0.3736 0.6787 0.085 Uiso 1 1 calc R . . H33C H 0.2844 -0.3548 0.6984 0.085 Uiso 1 1 calc R . . P1 P 0.9594(3) 0.8220(4) 0.2164(3) 0.0487(9) Uani 0.714(6) 1 d PDU B 1 F1 F 1.0379(4) 0.7365(5) 0.2303(4) 0.123(2) Uani 0.714(6) 1 d PDU B 1 F2 F 1.0303(3) 0.9151(4) 0.2299(3) 0.1146(16) Uani 0.714(6) 1 d PDU B 1 F3 F 0.8780(3) 0.9050(4) 0.2001(3) 0.0971(15) Uani 0.714(6) 1 d PDU B 1 F4 F 0.8858(5) 0.7315(4) 0.2018(4) 0.121(2) Uani 0.714(6) 1 d PDU B 1 F5 F 0.9529(6) 0.8236(6) 0.1321(3) 0.0933(18) Uani 0.714(6) 1 d PDU B 1 F6 F 0.9667(5) 0.8185(6) 0.3018(3) 0.096(2) Uani 0.714(6) 1 d PDU B 1 P1' P 0.9653(8) 0.8154(9) 0.2226(7) 0.049(2) Uani 0.286(6) 1 d PDU B 2 F1' F 1.0704(5) 0.8305(14) 0.2640(5) 0.106(4) Uani 0.286(6) 1 d PDU B 2 F2' F 0.9388(12) 0.9298(7) 0.2347(7) 0.108(3) Uani 0.286(6) 1 d PDU B 2 F3' F 0.8593(7) 0.7924(17) 0.1866(7) 0.127(4) Uani 0.286(6) 1 d PDU B 2 F4' F 0.9874(13) 0.6970(7) 0.2176(6) 0.116(4) Uani 0.286(6) 1 d PDU B 2 F5' F 0.9719(13) 0.8437(15) 0.1449(8) 0.095(4) Uani 0.286(6) 1 d PDU B 2 F6' F 0.9523(9) 0.7902(12) 0.3005(7) 0.073(3) Uani 0.286(6) 1 d PDU B 2 C34 C 0.0705(3) 0.6006(3) 0.3985(2) 0.0834(12) Uani 1 1 d . . . H34A H 0.0606 0.5228 0.3945 0.100 Uiso 1 1 calc R . . H34B H 0.0297 0.6335 0.3519 0.100 Uiso 1 1 calc R . . Cl1 Cl 0.04003(7) 0.64945(7) 0.47429(7) 0.0860(3) Uani 1 1 d . . . Cl2 Cl 0.18677(8) 0.62891(10) 0.40984(8) 0.1109(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 0.03915(12) 0.03444(10) 0.02597(10) 0.00187(7) 0.01137(8) 0.00073(8) C25 0.039(4) 0.094(10) 0.034(3) -0.004(6) 0.021(3) 0.007(6) C26 0.070(8) 0.053(4) 0.062(9) -0.002(5) 0.046(7) -0.007(5) C27 0.077(7) 0.066(7) 0.033(5) 0.014(4) 0.029(4) 0.018(6) C28 0.060(6) 0.065(6) 0.041(5) -0.014(5) 0.020(4) 0.006(5) C29 0.070(9) 0.055(5) 0.049(7) 0.013(5) 0.034(6) 0.023(5) C25' 0.057(6) 0.075(8) 0.050(6) -0.014(6) 0.030(4) -0.013(5) C26' 0.081(9) 0.058(5) 0.054(8) 0.017(5) 0.042(6) 0.006(5) C27' 0.061(5) 0.083(10) 0.032(4) -0.009(5) 0.017(3) 0.001(6) C28' 0.069(9) 0.049(4) 0.065(9) -0.014(5) 0.043(7) -0.004(5) C29' 0.055(6) 0.073(7) 0.046(6) 0.012(5) 0.030(5) 0.024(6) N1 0.0494(12) 0.0398(10) 0.0298(10) -0.0074(8) 0.0135(9) -0.0040(9) O1 0.0684(13) 0.0371(9) 0.0474(10) -0.0137(8) 0.0138(9) 0.0002(9) O2 0.0897(15) 0.0438(10) 0.0290(9) 0.0008(7) 0.0108(9) -0.0103(10) O3 0.0441(10) 0.0258(7) 0.0502(10) 0.0028(7) 0.0131(8) 0.0046(7) O4 0.0535(10) 0.0269(7) 0.0358(8) 0.0011(6) 0.0187(8) -0.0023(7) C1 0.0364(13) 0.0426(12) 0.0397(13) 0.0028(10) 0.0097(11) 0.0087(10) C2 0.0351(14) 0.0609(16) 0.0385(13) 0.0041(11) 0.0047(11) 0.0058(12) C3 0.0422(15) 0.0598(16) 0.0356(13) -0.0061(11) 0.0093(11) -0.0110(12) C4 0.0446(14) 0.0411(12) 0.0333(12) -0.0033(9) 0.0157(11) -0.0094(10) C5 0.0458(15) 0.0390(12) 0.0369(12) 0.0061(9) 0.0163(11) 0.0129(10) C6 0.0357(14) 0.0652(17) 0.0459(14) 0.0111(12) 0.0158(12) 0.0167(12) C7 0.0325(14) 0.0649(17) 0.0450(14) 0.0077(12) 0.0134(11) -0.0011(12) C8 0.0394(13) 0.0402(12) 0.0378(12) 0.0059(9) 0.0144(11) -0.0011(10) C9 0.0356(12) 0.0263(9) 0.0351(11) -0.0011(8) 0.0115(10) 0.0021(8) C10 0.0411(13) 0.0267(9) 0.0254(10) -0.0010(8) 0.0135(9) -0.0006(9) C11 0.0328(12) 0.0345(10) 0.0286(10) -0.0014(8) 0.0129(9) -0.0014(9) C12 0.0361(12) 0.0325(10) 0.0267(10) -0.0004(8) 0.0142(9) 0.0022(9) C13 0.0335(12) 0.0316(10) 0.0270(10) 0.0017(8) 0.0115(9) 0.0022(8) C14 0.0327(12) 0.0335(10) 0.0313(11) -0.0001(8) 0.0123(9) 0.0035(9) C15 0.0358(12) 0.0352(11) 0.0344(11) -0.0059(9) 0.0144(10) 0.0027(9) C16 0.0398(13) 0.0345(11) 0.0299(10) -0.0058(8) 0.0166(10) -0.0045(9) C17 0.0539(15) 0.0414(12) 0.0286(11) -0.0051(9) 0.0187(11) -0.0063(11) C18 0.0432(14) 0.0395(12) 0.0365(12) -0.0086(9) 0.0163(11) 0.0020(10) C19 0.0640(18) 0.0379(12) 0.0283(11) -0.0075(9) 0.0113(11) -0.0071(11) C20 0.062(2) 0.075(2) 0.0377(14) -0.0052(13) 0.0093(14) -0.0097(16) C21 0.080(2) 0.082(2) 0.0494(18) -0.0062(16) -0.0023(17) -0.0191(19) C22 0.117(3) 0.0518(17) 0.0371(16) -0.0039(12) -0.0055(18) -0.0255(19) C23 0.150(4) 0.0517(17) 0.0328(15) -0.0112(12) 0.0302(19) -0.024(2) C24 0.092(2) 0.0502(15) 0.0394(14) -0.0136(12) 0.0293(15) -0.0167(15) C30 0.0551(17) 0.0365(12) 0.0612(17) -0.0036(12) 0.0128(14) 0.0170(12) C31 0.081(2) 0.0330(13) 0.092(3) 0.0085(14) 0.014(2) 0.0166(14) C32 0.0657(18) 0.0388(12) 0.0333(12) 0.0002(9) 0.0203(12) -0.0122(12) C33 0.073(2) 0.0366(13) 0.0532(16) 0.0088(11) 0.0128(15) -0.0093(13) P1 0.0433(16) 0.0586(17) 0.0436(13) -0.0130(12) 0.0138(11) 0.0030(11) F1 0.109(3) 0.138(4) 0.150(4) 0.055(3) 0.082(3) 0.075(3) F2 0.087(3) 0.110(3) 0.137(3) -0.037(3) 0.025(3) -0.053(2) F3 0.077(3) 0.127(3) 0.097(3) 0.030(3) 0.043(2) 0.052(2) F4 0.134(5) 0.105(3) 0.135(4) -0.026(3) 0.060(4) -0.067(3) F5 0.132(4) 0.101(3) 0.056(2) -0.0205(19) 0.043(2) -0.021(3) F6 0.089(3) 0.151(5) 0.0421(19) -0.021(2) 0.0125(18) 0.000(3) P1' 0.042(4) 0.052(3) 0.049(4) -0.004(3) 0.011(3) -0.003(3) F1' 0.034(4) 0.195(10) 0.082(5) -0.032(6) 0.007(3) -0.023(5) F2' 0.161(9) 0.057(4) 0.121(7) 0.003(4) 0.066(7) 0.039(5) F3' 0.044(4) 0.210(11) 0.097(6) 0.012(9) -0.015(4) -0.032(6) F4' 0.200(10) 0.063(4) 0.085(6) -0.029(4) 0.047(8) 0.017(6) F5' 0.111(8) 0.119(10) 0.074(6) 0.024(7) 0.056(6) 0.047(8) F6' 0.053(5) 0.098(7) 0.079(5) 0.036(5) 0.039(5) 0.045(5) C34 0.063(2) 0.060(2) 0.098(3) -0.0006(19) -0.012(2) -0.0002(17) Cl1 0.0605(5) 0.0567(5) 0.1161(8) -0.0025(5) -0.0037(5) 0.0040(4) Cl2 0.0727(7) 0.1050(8) 0.1440(11) 0.0329(8) 0.0215(7) -0.0075(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 C26' 2.162(11) . ? Ru1 C28 2.162(10) . ? Ru1 C25 2.163(9) . ? Ru1 C29 2.163(9) . ? Ru1 C27 2.163(10) . ? Ru1 C27' 2.164(10) . ? Ru1 C28' 2.173(9) . ? Ru1 C26 2.174(10) . ? Ru1 C25' 2.182(11) . ? Ru1 C29' 2.188(9) . ? Ru1 C2 2.190(3) . ? Ru1 C3 2.192(3) . ? C25 C26 1.400(12) . ? C25 C29 1.430(12) . ? C26 C27 1.391(12) . ? C27 C28 1.383(12) . ? C28 C29 1.408(11) . ? C25' C26' 1.393(12) . ? C25' C29' 1.434(12) . ? C26' C27' 1.385(12) . ? C27' C28' 1.380(12) . ? C28' C29' 1.411(12) . ? N1 C18 1.384(3) . ? N1 C17 1.389(3) . ? N1 C19 1.443(3) . ? O1 C18 1.200(3) . ? O2 C17 1.199(3) . ? O3 C9 1.398(2) . ? O3 C30 1.434(3) . ? O4 C10 1.400(2) . ? O4 C32 1.443(3) . ? C1 C2 1.414(4) . ? C1 C14 1.417(3) . ? C2 C3 1.407(4) . ? C3 C4 1.414(4) . ? C4 C11 1.412(3) . ? C5 C12 1.387(3) . ? C5 C6 1.391(4) . ? C6 C7 1.379(4) . ? C7 C8 1.391(4) . ? C8 C13 1.386(3) . ? C9 C13 1.508(3) . ? C9 C14 1.527(3) . ? C9 C15 1.571(3) . ? C10 C12 1.516(3) . ? C10 C11 1.523(3) . ? C10 C16 1.572(3) . ? C11 C14 1.415(3) . ? C12 C13 1.393(3) . ? C15 C18 1.515(3) . ? C15 C16 1.547(3) . ? C16 C17 1.522(3) . ? C19 C24 1.369(4) . ? C19 C20 1.373(4) . ? C20 C21 1.381(4) . ? C21 C22 1.373(5) . ? C22 C23 1.354(6) . ? C23 C24 1.401(5) . ? C30 C31 1.504(4) . ? C32 C33 1.499(4) . ? P1 F4 1.554(6) . ? P1 F2 1.556(6) . ? P1 F1 1.563(5) . ? P1 F3 1.570(5) . ? P1 F5 1.581(5) . ? P1 F6 1.596(5) . ? P1' F2' 1.533(12) . ? P1' F4' 1.536(13) . ? P1' F1' 1.543(12) . ? P1' F3' 1.556(13) . ? P1' F5' 1.561(12) . ? P1' F6' 1.595(12) . ? C34 Cl2 1.747(4) . ? C34 Cl1 1.769(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C26' Ru1 C28 57.3(6) . . ? C26' Ru1 C25 49.3(5) . . ? C28 Ru1 C25 64.0(4) . . ? C26' Ru1 C29 67.5(5) . . ? C28 Ru1 C29 38.0(3) . . ? C25 Ru1 C29 38.6(3) . . ? C26' Ru1 C27 25.7(5) . . ? C28 Ru1 C27 37.3(3) . . ? C25 Ru1 C27 63.2(4) . . ? C29 Ru1 C27 62.9(4) . . ? C26' Ru1 C27' 37.4(4) . . ? C28 Ru1 C27' 24.7(5) . . ? C25 Ru1 C27' 65.2(5) . . ? C29 Ru1 C27' 55.3(5) . . ? C27 Ru1 C27' 13.2(5) . . ? C26' Ru1 C28' 62.4(4) . . ? C28 Ru1 C28' 15.5(4) . . ? C25 Ru1 C28' 54.3(4) . . ? C29 Ru1 C28' 22.9(4) . . ? C27 Ru1 C28' 48.0(5) . . ? C27' Ru1 C28' 37.1(3) . . ? C26' Ru1 C26 13.7(5) . . ? C28 Ru1 C26 62.8(4) . . ? C25 Ru1 C26 37.7(3) . . ? C29 Ru1 C26 63.2(4) . . ? C27 Ru1 C26 37.4(4) . . ? C27' Ru1 C26 47.2(6) . . ? C28' Ru1 C26 64.0(5) . . ? C26' Ru1 C25' 37.4(3) . . ? C28 Ru1 C25' 68.6(5) . . ? C25 Ru1 C25' 15.8(3) . . ? C29 Ru1 C25' 51.7(4) . . ? C27 Ru1 C25' 56.8(6) . . ? C27' Ru1 C25' 62.5(4) . . ? C28' Ru1 C25' 62.8(4) . . ? C26 Ru1 C25' 24.2(5) . . ? C26' Ru1 C29' 63.4(4) . . ? C28 Ru1 C29' 51.4(4) . . ? C25 Ru1 C29' 23.4(4) . . ? C29 Ru1 C29' 16.8(3) . . ? C27 Ru1 C29' 67.0(5) . . ? C27' Ru1 C29' 63.1(4) . . ? C28' Ru1 C29' 37.8(3) . . ? C26 Ru1 C29' 55.3(5) . . ? C25' Ru1 C29' 38.3(3) . . ? C26' Ru1 C2 112.8(4) . . ? C28 Ru1 C2 117.0(4) . . ? C25 Ru1 C2 160.0(5) . . ? C29 Ru1 C2 152.3(5) . . ? C27 Ru1 C2 104.6(4) . . ? C27' Ru1 C2 106.8(4) . . ? C28' Ru1 C2 130.6(5) . . ? C26 Ru1 C2 123.1(5) . . ? C25' Ru1 C2 144.3(5) . . ? C29' Ru1 C2 168.3(5) . . ? C26' Ru1 C3 138.2(5) . . ? C28 Ru1 C3 104.2(4) . . ? C25 Ru1 C3 161.3(5) . . ? C29 Ru1 C3 123.2(5) . . ? C27 Ru1 C3 117.1(5) . . ? C27' Ru1 C3 110.6(4) . . ? C28' Ru1 C3 110.6(4) . . ? C26 Ru1 C3 151.9(5) . . ? C25' Ru1 C3 172.8(3) . . ? C29' Ru1 C3 137.9(5) . . ? C2 Ru1 C3 37.46(11) . . ? C26 C25 C29 106.8(8) . . ? C26 C25 Ru1 71.6(5) . . ? C29 C25 Ru1 70.7(5) . . ? C27 C26 C25 108.6(8) . . ? C27 C26 Ru1 70.9(6) . . ? C25 C26 Ru1 70.7(5) . . ? C28 C27 C26 109.1(9) . . ? C28 C27 Ru1 71.3(6) . . ? C26 C27 Ru1 71.7(6) . . ? C27 C28 C29 108.0(10) . . ? C27 C28 Ru1 71.4(6) . . ? C29 C28 Ru1 71.0(5) . . ? C28 C29 C25 107.6(8) . . ? C28 C29 Ru1 71.0(6) . . ? C25 C29 Ru1 70.7(5) . . ? C26' C25' C29' 107.9(9) . . ? C26' C25' Ru1 70.5(6) . . ? C29' C25' Ru1 71.1(6) . . ? C27' C26' C25' 108.6(9) . . ? C27' C26' Ru1 71.4(6) . . ? C25' C26' Ru1 72.1(6) . . ? C28' C27' C26' 108.5(9) . . ? C28' C27' Ru1 71.8(5) . . ? C26' C27' Ru1 71.2(6) . . ? C27' C28' C29' 109.3(8) . . ? C27' C28' Ru1 71.1(6) . . ? C29' C28' Ru1 71.7(5) . . ? C28' C29' C25' 105.7(8) . . ? C28' C29' Ru1 70.5(5) . . ? C25' C29' Ru1 70.6(6) . . ? C18 N1 C17 114.2(2) . . ? C18 N1 C19 122.2(2) . . ? C17 N1 C19 123.6(2) . . ? C9 O3 C30 117.49(19) . . ? C10 O4 C32 117.75(18) . . ? C2 C1 C14 119.3(2) . . ? C2 C1 Ru1 71.08(15) . . ? C14 C1 Ru1 72.24(13) . . ? C3 C2 C1 120.5(2) . . ? C3 C2 Ru1 71.33(15) . . ? C1 C2 Ru1 71.26(14) . . ? C2 C3 C4 120.3(2) . . ? C2 C3 Ru1 71.21(15) . . ? C4 C3 Ru1 71.70(14) . . ? C11 C4 C3 119.4(2) . . ? C11 C4 Ru1 72.41(13) . . ? C3 C4 Ru1 70.78(14) . . ? C12 C5 C6 119.0(2) . . ? C7 C6 C5 120.6(2) . . ? C6 C7 C8 120.6(2) . . ? C13 C8 C7 119.0(2) . . ? O3 C9 C13 108.95(18) . . ? O3 C9 C14 113.14(18) . . ? C13 C9 C14 108.96(17) . . ? O3 C9 C15 116.46(17) . . ? C13 C9 C15 105.12(17) . . ? C14 C9 C15 103.70(18) . . ? O4 C10 C12 109.49(18) . . ? O4 C10 C11 113.11(17) . . ? C12 C10 C11 108.46(17) . . ? O4 C10 C16 116.15(17) . . ? C12 C10 C16 104.71(17) . . ? C11 C10 C16 104.35(17) . . ? C4 C11 C14 120.3(2) . . ? C4 C11 C10 125.74(19) . . ? C14 C11 C10 113.92(19) . . ? C4 C11 Ru1 70.45(12) . . ? C14 C11 Ru1 71.01(12) . . ? C10 C11 Ru1 130.90(15) . . ? C5 C12 C13 120.4(2) . . ? C5 C12 C10 125.2(2) . . ? C13 C12 C10 114.11(19) . . ? C8 C13 C12 120.3(2) . . ? C8 C13 C9 124.86(19) . . ? C12 C13 C9 114.57(19) . . ? C11 C14 C1 120.1(2) . . ? C11 C14 C9 113.40(19) . . ? C1 C14 C9 126.5(2) . . ? C11 C14 Ru1 71.87(12) . . ? C1 C14 Ru1 70.29(13) . . ? C9 C14 Ru1 130.38(15) . . ? C18 C15 C16 105.05(19) . . ? C18 C15 C9 110.64(19) . . ? C16 C15 C9 110.30(17) . . ? C17 C16 C15 104.72(18) . . ? C17 C16 C10 110.47(19) . . ? C15 C16 C10 110.35(17) . . ? O2 C17 N1 124.7(2) . . ? O2 C17 C16 127.4(2) . . ? N1 C17 C16 107.90(19) . . ? O1 C18 N1 124.2(2) . . ? O1 C18 C15 127.7(2) . . ? N1 C18 C15 108.14(19) . . ? C24 C19 C20 121.9(3) . . ? C24 C19 N1 119.4(3) . . ? C20 C19 N1 118.7(2) . . ? C19 C20 C21 118.7(3) . . ? C22 C21 C20 120.5(4) . . ? C23 C22 C21 120.2(3) . . ? C22 C23 C24 120.7(3) . . ? C19 C24 C23 118.1(3) . . ? O3 C30 C31 106.5(3) . . ? O4 C32 C33 106.0(2) . . ? F4 P1 F2 178.1(5) . . ? F4 P1 F1 89.5(4) . . ? F2 P1 F1 92.3(4) . . ? F4 P1 F3 88.7(4) . . ? F2 P1 F3 89.4(4) . . ? F1 P1 F3 177.8(5) . . ? F4 P1 F5 91.7(4) . . ? F2 P1 F5 87.9(4) . . ? F1 P1 F5 88.0(4) . . ? F3 P1 F5 90.7(4) . . ? F4 P1 F6 88.0(4) . . ? F2 P1 F6 92.5(4) . . ? F1 P1 F6 91.1(4) . . ? F3 P1 F6 90.2(4) . . ? F5 P1 F6 179.1(5) . . ? F2' P1' F4' 173.4(11) . . ? F2' P1' F1' 95.0(10) . . ? F4' P1' F1' 86.5(9) . . ? F2' P1' F3' 87.4(10) . . ? F4' P1' F3' 90.5(10) . . ? F1' P1' F3' 174.6(12) . . ? F2' P1' F5' 91.9(10) . . ? F4' P1' F5' 94.4(10) . . ? F1' P1' F5' 94.2(10) . . ? F3' P1' F5' 90.5(10) . . ? F2' P1' F6' 85.7(8) . . ? F4' P1' F6' 87.9(9) . . ? F1' P1' F6' 88.7(9) . . ? F3' P1' F6' 86.7(9) . . ? F5' P1' F6' 176.3(11) . . ? Cl2 C34 Cl1 111.1(2) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.690 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.057 data_ARu1 _database_code_depnum_ccdc_archive 'CCDC 904730' #TrackingRef 'ARu1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H22 F6 N O2 P Ru' _chemical_formula_weight 662.52 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' 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 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 14.9563(6) _cell_length_b 10.1517(4) _cell_length_c 17.2552(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.302(2) _cell_angle_gamma 90.00 _cell_volume 2604.06(18) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 2927 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 21.21 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8668 _exptl_absorpt_correction_T_max 0.9572 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 kappa APEX-II CCD Quazar' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13782 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4176 _reflns_number_gt 2689 _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^)+(0.0873P)^2^+3.9671P] 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 4176 _refine_ls_number_parameters 563 _refine_ls_number_restraints 774 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1644 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.234 _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 O1 O 0.6131(4) 0.8107(6) 0.2769(3) 0.0713(17) Uani 1 1 d . D . O2 O 0.4435(3) 0.8249(5) 0.0402(3) 0.0442(12) Uani 1 1 d . D . Ru1 Ru 0.77051(4) 0.55808(7) 0.03521(4) 0.0563(3) Uani 1 1 d D A . C25 C 0.9141(10) 0.597(3) 0.0432(14) 0.076(4) Uani 0.603(16) 1 d PDU A 1 H25 H 0.9451 0.6465 0.0844 0.091 Uiso 0.603(16) 1 calc PR A 1 C26 C 0.8755(14) 0.647(2) -0.0268(19) 0.081(4) Uani 0.603(16) 1 d PDU A 1 H26 H 0.8763 0.7366 -0.0424 0.098 Uiso 0.603(16) 1 calc PR A 1 C27 C 0.8337(12) 0.539(4) -0.0723(10) 0.086(4) Uani 0.603(16) 1 d PDU A 1 H27 H 0.8019 0.5443 -0.1230 0.103 Uiso 0.603(16) 1 calc PR A 1 C28 C 0.8501(14) 0.424(2) -0.0256(17) 0.085(4) Uani 0.603(16) 1 d PDU A 1 H28 H 0.8298 0.3378 -0.0402 0.103 Uiso 0.603(16) 1 calc PR A 1 C29 C 0.8998(13) 0.456(3) 0.0439(13) 0.081(4) Uani 0.603(16) 1 d PDU A 1 H29 H 0.9207 0.3972 0.0846 0.097 Uiso 0.603(16) 1 calc PR A 1 C25' C 0.8980(19) 0.645(3) 0.014(3) 0.081(4) Uani 0.397(16) 1 d PDU A 2 H25' H 0.9138 0.7335 0.0279 0.097 Uiso 0.397(16) 1 calc PR A 2 C26' C 0.855(2) 0.608(4) -0.057(2) 0.081(4) Uani 0.397(16) 1 d PDU A 2 H26' H 0.8370 0.6643 -0.1004 0.097 Uiso 0.397(16) 1 calc PR A 2 C27' C 0.8412(18) 0.468(5) -0.054(2) 0.083(4) Uani 0.397(16) 1 d PDU A 2 H27' H 0.8119 0.4134 -0.0942 0.099 Uiso 0.397(16) 1 calc PR A 2 C28' C 0.881(2) 0.426(3) 0.021(3) 0.081(4) Uani 0.397(16) 1 d PDU A 2 H28' H 0.8824 0.3377 0.0395 0.098 Uiso 0.397(16) 1 calc PR A 2 C29' C 0.9160(14) 0.533(5) 0.0630(16) 0.080(4) Uani 0.397(16) 1 d PDU A 2 H29' H 0.9462 0.5328 0.1144 0.095 Uiso 0.397(16) 1 calc PR A 2 C1 C 0.6245(5) 0.5876(8) 0.0036(5) 0.054(2) Uani 1 1 d . A . H1 H 0.5919 0.5929 -0.0468 0.065 Uiso 1 1 calc R . . C2 C 0.6390(6) 0.4635(9) 0.0408(6) 0.065(2) Uani 1 1 d . . . H2 H 0.6150 0.3856 0.0159 0.078 Uiso 1 1 calc R A . C3 C 0.6892(5) 0.4563(8) 0.1151(6) 0.060(2) Uani 1 1 d . A . H3 H 0.6988 0.3734 0.1401 0.072 Uiso 1 1 calc R . . C4 C 0.7247(5) 0.5701(8) 0.1517(5) 0.0463(19) Uani 1 1 d . A . H4 H 0.7588 0.5646 0.2014 0.056 Uiso 1 1 calc R . . C10 C 0.7399(5) 0.8267(7) 0.1476(4) 0.0468(19) Uani 1 1 d D . . H10 H 0.7791 0.8200 0.1983 0.056 Uiso 1 1 calc R B 1 C9 C 0.6438(4) 0.8412(8) 0.0130(4) 0.0456(19) Uani 1 1 d D . . H9 H 0.6080 0.8447 -0.0394 0.055 Uiso 1 1 calc R C 1 C5 C 0.8740(12) 0.950(2) 0.0864(13) 0.056(4) Uani 0.473(18) 1 d PDU D 1 H5 H 0.9132 0.9475 0.1336 0.067 Uiso 0.473(18) 1 calc PR D 1 C6 C 0.9025(12) 1.011(2) 0.0215(14) 0.062(4) Uani 0.473(18) 1 d PDU D 1 H6 H 0.9598 1.0524 0.0249 0.074 Uiso 0.473(18) 1 calc PR D 1 C7 C 0.8496(11) 1.012(2) -0.0451(13) 0.059(4) Uani 0.473(18) 1 d PDU D 1 H7 H 0.8695 1.0575 -0.0881 0.071 Uiso 0.473(18) 1 calc PR D 1 C8 C 0.7675(11) 0.951(2) -0.0553(12) 0.054(4) Uani 0.473(18) 1 d PDU D 1 H8 H 0.7336 0.9446 -0.1050 0.065 Uiso 0.473(18) 1 calc PR D 1 C13 C 0.7369(13) 0.898(3) 0.0112(12) 0.051(4) Uani 0.473(18) 1 d PDU D 1 C12 C 0.7879(15) 0.892(3) 0.0839(12) 0.053(4) Uani 0.473(18) 1 d PDU D 1 C5' C 0.8626(11) 0.9805(18) 0.1120(12) 0.057(4) Uani 0.527(18) 1 d PDU D 2 H5' H 0.8943 0.9737 0.1627 0.069 Uiso 0.527(18) 1 calc PR D 2 C6' C 0.8951(11) 1.0574(18) 0.0553(13) 0.063(4) Uani 0.527(18) 1 d PDU D 2 H6' H 0.9510 1.1022 0.0646 0.075 Uiso 0.527(18) 1 calc PR D 2 C7' C 0.8449(11) 1.066(2) -0.0125(13) 0.065(3) Uani 0.527(18) 1 d PDU D 2 H7' H 0.8670 1.1211 -0.0505 0.078 Uiso 0.527(18) 1 calc PR D 2 C8' C 0.7649(11) 1.0042(19) -0.0341(12) 0.057(3) Uani 0.527(18) 1 d PDU D 2 H8' H 0.7337 1.0166 -0.0846 0.068 Uiso 0.527(18) 1 calc PR D 2 C13' C 0.7311(12) 0.923(3) 0.0200(11) 0.052(4) Uani 0.527(18) 1 d PDU D 2 C12' C 0.7812(14) 0.913(3) 0.0924(11) 0.054(4) Uani 0.527(18) 1 d PDU D 2 C11 C 0.7099(4) 0.6926(7) 0.1152(4) 0.0381(17) Uani 1 1 d . A . C14 C 0.6584(4) 0.7016(7) 0.0412(4) 0.0385(17) Uani 1 1 d . A . C15 C 0.5945(4) 0.9110(7) 0.0760(4) 0.0407(17) Uani 1 1 d . D . H15 H 0.5834 1.0053 0.0612 0.049 Uiso 1 1 calc R . . C16 C 0.6512(5) 0.9034(7) 0.1553(4) 0.0457(18) Uani 1 1 d . D . H16 H 0.6659 0.9945 0.1748 0.055 Uiso 1 1 calc R . . C17 C 0.5922(5) 0.8359(8) 0.2091(5) 0.0483(19) Uani 1 1 d . . . C18 C 0.5063(5) 0.8448(6) 0.0881(4) 0.0349(16) Uani 1 1 d . . . N1 N 0.5109(4) 0.8048(6) 0.1661(3) 0.0409(14) Uani 1 1 d D D . C19 C 0.4365(6) 0.7441(8) 0.1974(5) 0.0512(17) Uani 0.495(11) 1 d PDU D 1 C20 C 0.3648(10) 0.8173(17) 0.2164(12) 0.057(3) Uani 0.495(11) 1 d PDU D 1 H20 H 0.3682 0.9106 0.2139 0.068 Uiso 0.495(11) 1 calc PR D 1 C21 C 0.2887(14) 0.7609(18) 0.2387(16) 0.064(3) Uani 0.495(11) 1 d PDU D 1 H21 H 0.2441 0.8156 0.2572 0.077 Uiso 0.495(11) 1 calc PR D 1 C22 C 0.2748(13) 0.6256(17) 0.2349(13) 0.066(3) Uani 0.495(11) 1 d PDU D 1 H22 H 0.2197 0.5873 0.2460 0.079 Uiso 0.495(11) 1 calc PR D 1 C23 C 0.3429(12) 0.5518(16) 0.2147(12) 0.069(3) Uani 0.495(11) 1 d PDU D 1 H23 H 0.3371 0.4586 0.2148 0.082 Uiso 0.495(11) 1 calc PR D 1 C24 C 0.4207(12) 0.6068(14) 0.1939(12) 0.061(3) Uani 0.495(11) 1 d PDU D 1 H24 H 0.4654 0.5508 0.1766 0.073 Uiso 0.495(11) 1 calc PR D 1 C19' C 0.4365(6) 0.7441(8) 0.1974(5) 0.0512(17) Uani 0.505(11) 1 d PDU D 2 C20' C 0.3556(10) 0.8011(18) 0.1882(11) 0.055(3) Uani 0.505(11) 1 d PDU D 2 H20' H 0.3455 0.8812 0.1602 0.066 Uiso 0.505(11) 1 calc PR D 2 C21' C 0.2870(13) 0.7382(18) 0.2215(15) 0.062(3) Uani 0.505(11) 1 d PDU D 2 H21' H 0.2270 0.7700 0.2130 0.075 Uiso 0.505(11) 1 calc PR D 2 C22' C 0.3077(12) 0.6277(18) 0.2674(13) 0.066(3) Uani 0.505(11) 1 d PDU D 2 H22' H 0.2611 0.5872 0.2922 0.080 Uiso 0.505(11) 1 calc PR D 2 C23' C 0.3901(12) 0.5758(16) 0.2784(12) 0.068(3) Uani 0.505(11) 1 d PDU D 2 H23' H 0.4006 0.4988 0.3093 0.082 Uiso 0.505(11) 1 calc PR D 2 C24' C 0.4595(11) 0.6329(15) 0.2454(11) 0.060(3) Uani 0.505(11) 1 d PDU D 2 H24' H 0.5193 0.6002 0.2540 0.072 Uiso 0.505(11) 1 calc PR D 2 P1 P 0.49221(14) 0.2124(2) 0.22141(13) 0.0556(6) Uani 1 1 d DU . . F1 F 0.5506(7) 0.3473(9) 0.2343(8) 0.088(3) Uani 0.556(8) 1 d PDU E 1 F2 F 0.4105(8) 0.2872(12) 0.1748(6) 0.079(3) Uani 0.556(8) 1 d PDU E 1 F3 F 0.4494(9) 0.0875(11) 0.1947(10) 0.107(4) Uani 0.556(8) 1 d PDU E 1 F4 F 0.5764(9) 0.1376(14) 0.2677(9) 0.086(4) Uani 0.556(8) 1 d PDU E 1 F5 F 0.4569(7) 0.2458(13) 0.3015(6) 0.076(3) Uani 0.556(8) 1 d PDU E 1 F6 F 0.5364(8) 0.2013(14) 0.1406(6) 0.096(3) Uani 0.556(8) 1 d PDU E 1 F1' F 0.5142(9) 0.3217(12) 0.1690(9) 0.084(3) Uani 0.444(8) 1 d PDU E 2 F2' F 0.3863(8) 0.2232(17) 0.1912(10) 0.086(4) Uani 0.444(8) 1 d PDU E 2 F3' F 0.4531(10) 0.0858(14) 0.2661(10) 0.107(4) Uani 0.444(8) 1 d PDU E 2 F4' F 0.5848(11) 0.1939(17) 0.2584(14) 0.087(4) Uani 0.444(8) 1 d PDU E 2 F5' F 0.4771(13) 0.3162(17) 0.2860(9) 0.103(5) Uani 0.444(8) 1 d PDU E 2 F6' F 0.4952(10) 0.1071(14) 0.1525(7) 0.069(3) Uani 0.444(8) 1 d PDU E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.086(4) 0.088(4) 0.036(3) 0.001(3) -0.011(3) 0.018(4) O2 0.035(3) 0.055(3) 0.041(3) 0.005(2) -0.005(2) -0.001(2) Ru1 0.0437(4) 0.0791(6) 0.0454(5) -0.0039(4) 0.0018(3) 0.0209(3) C25 0.043(6) 0.135(10) 0.052(8) 0.009(7) 0.011(6) 0.032(7) C26 0.053(7) 0.141(9) 0.052(9) 0.009(7) 0.015(7) 0.031(6) C27 0.068(7) 0.141(10) 0.050(7) 0.001(7) 0.014(6) 0.040(7) C28 0.073(7) 0.135(9) 0.050(9) -0.007(7) 0.011(7) 0.047(7) C29 0.056(6) 0.133(10) 0.055(8) -0.002(7) 0.011(6) 0.045(7) C25' 0.051(7) 0.136(10) 0.057(9) 0.006(8) 0.013(7) 0.026(7) C26' 0.060(7) 0.133(10) 0.050(9) 0.003(8) 0.014(7) 0.034(8) C27' 0.069(7) 0.131(10) 0.050(9) -0.004(8) 0.012(7) 0.045(8) C28' 0.060(8) 0.130(10) 0.054(9) -0.003(7) 0.007(7) 0.047(7) C29' 0.050(7) 0.135(11) 0.055(9) 0.000(8) 0.011(7) 0.036(8) C1 0.045(4) 0.067(6) 0.047(5) -0.007(4) -0.007(4) 0.018(4) C2 0.052(5) 0.065(6) 0.074(7) -0.020(5) -0.006(5) 0.007(4) C3 0.046(5) 0.054(5) 0.079(7) 0.004(5) 0.006(5) 0.008(4) C4 0.036(4) 0.062(5) 0.040(4) 0.001(4) -0.001(3) 0.004(4) C10 0.037(4) 0.056(5) 0.044(5) 0.003(4) -0.011(3) 0.003(4) C9 0.028(4) 0.071(5) 0.037(4) 0.008(4) -0.004(3) 0.003(4) C5 0.037(5) 0.058(7) 0.073(7) -0.002(6) 0.005(5) 0.005(6) C6 0.047(6) 0.064(8) 0.076(8) -0.004(7) 0.019(6) 0.005(6) C7 0.049(5) 0.058(8) 0.074(7) 0.001(7) 0.018(6) 0.009(6) C8 0.046(5) 0.053(8) 0.066(7) 0.007(6) 0.017(5) 0.012(6) C13 0.037(5) 0.051(8) 0.065(6) 0.010(6) 0.010(5) 0.009(6) C12 0.035(5) 0.051(8) 0.071(6) 0.003(6) 0.004(5) 0.005(6) C5' 0.035(5) 0.059(8) 0.077(7) -0.006(6) 0.004(5) 0.008(5) C6' 0.045(6) 0.063(8) 0.082(8) -0.008(7) 0.013(6) 0.002(6) C7' 0.053(6) 0.065(8) 0.077(8) -0.005(6) 0.015(6) 0.013(6) C8' 0.050(5) 0.053(8) 0.070(7) 0.004(6) 0.019(5) 0.011(6) C13' 0.040(5) 0.052(8) 0.065(6) 0.007(6) 0.010(5) 0.014(5) C12' 0.038(5) 0.053(8) 0.072(6) 0.001(6) 0.003(5) 0.007(5) C11 0.026(3) 0.051(5) 0.036(4) 0.005(4) 0.000(3) 0.007(3) C14 0.026(3) 0.056(5) 0.033(4) 0.002(4) 0.001(3) 0.010(3) C15 0.034(4) 0.045(4) 0.040(4) 0.006(3) -0.009(3) 0.005(3) C16 0.045(4) 0.046(4) 0.044(5) -0.002(4) -0.007(4) 0.001(3) C17 0.059(5) 0.051(5) 0.032(4) -0.003(4) -0.006(4) 0.009(4) C18 0.038(4) 0.035(4) 0.032(4) -0.001(3) 0.001(3) 0.003(3) N1 0.045(4) 0.044(3) 0.034(3) 0.004(3) 0.004(3) 0.008(3) C19 0.060(3) 0.044(3) 0.052(4) -0.001(3) 0.020(3) 0.002(3) C20 0.057(5) 0.049(5) 0.067(7) -0.004(6) 0.017(5) -0.002(4) C21 0.062(5) 0.061(5) 0.072(8) -0.007(6) 0.021(5) -0.006(5) C22 0.064(6) 0.062(6) 0.075(8) 0.000(6) 0.024(6) -0.011(5) C23 0.076(6) 0.052(6) 0.082(7) 0.004(6) 0.027(6) -0.007(5) C24 0.068(6) 0.050(5) 0.068(6) -0.001(5) 0.024(5) 0.002(5) C19' 0.060(3) 0.044(3) 0.052(4) -0.001(3) 0.020(3) 0.002(3) C20' 0.056(5) 0.049(5) 0.062(7) -0.004(5) 0.013(5) -0.004(4) C21' 0.060(5) 0.057(6) 0.072(8) -0.008(6) 0.020(5) -0.005(5) C22' 0.066(6) 0.062(5) 0.075(7) 0.004(6) 0.024(6) -0.010(5) C23' 0.073(6) 0.055(6) 0.080(7) 0.013(6) 0.025(6) -0.002(5) C24' 0.065(6) 0.051(6) 0.068(7) 0.008(5) 0.023(6) 0.004(5) P1 0.0533(13) 0.0630(14) 0.0475(13) -0.0109(11) -0.0074(10) 0.0046(11) F1 0.080(6) 0.080(5) 0.108(8) -0.026(5) 0.026(6) -0.015(5) F2 0.090(7) 0.095(8) 0.049(5) -0.004(6) -0.015(5) 0.042(6) F3 0.113(8) 0.073(6) 0.128(9) -0.009(6) -0.018(7) -0.017(5) F4 0.070(7) 0.100(9) 0.082(7) -0.019(7) -0.015(5) 0.049(7) F5 0.063(6) 0.116(9) 0.052(5) 0.020(5) 0.024(4) 0.023(6) F6 0.096(7) 0.117(9) 0.077(6) -0.028(6) 0.021(5) 0.011(6) F1' 0.088(7) 0.069(6) 0.097(8) 0.025(6) 0.017(7) 0.007(6) F2' 0.051(6) 0.108(10) 0.100(9) -0.019(7) 0.013(6) 0.007(6) F3' 0.121(9) 0.110(8) 0.090(9) 0.028(7) 0.003(8) -0.047(7) F4' 0.054(6) 0.086(10) 0.113(9) 0.005(8) -0.035(6) -0.008(6) F5' 0.126(10) 0.108(9) 0.074(8) -0.034(7) 0.001(7) 0.005(8) F6' 0.080(8) 0.069(7) 0.056(6) -0.010(5) 0.001(6) 0.027(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 O1 C17 1.206(8) . ? O2 C18 1.199(8) . ? Ru1 C28 2.156(16) . ? Ru1 C28' 2.16(2) . ? Ru1 C27' 2.17(2) . ? Ru1 C25 2.172(15) . ? Ru1 C25' 2.172(19) . ? Ru1 C27 2.182(15) . ? Ru1 C29 2.183(16) . ? Ru1 C26 2.190(15) . ? Ru1 C29' 2.19(2) . ? Ru1 C3 2.194(9) . ? Ru1 C4 2.197(8) . ? Ru1 C26' 2.20(2) . ? C25 C26 1.38(2) . ? C25 C29 1.44(3) . ? C26 C27 1.45(3) . ? C27 C28 1.43(3) . ? C28 C29 1.38(3) . ? C25' C26' 1.37(3) . ? C25' C29' 1.43(3) . ? C26' C27' 1.44(3) . ? C27' C28' 1.43(3) . ? C28' C29' 1.38(3) . ? C1 C14 1.395(11) . ? C1 C2 1.420(12) . ? C2 C3 1.415(13) . ? C3 C4 1.394(11) . ? C4 C11 1.401(10) . ? C10 C12' 1.475(15) . ? C10 C11 1.520(10) . ? C10 C12 1.529(16) . ? C10 C16 1.556(10) . ? C9 C14 1.506(10) . ? C9 C13 1.511(16) . ? C9 C13' 1.540(15) . ? C9 C15 1.550(10) . ? C5 C6 1.39(2) . ? C5 C12 1.412(17) . ? C6 C7 1.32(2) . ? C7 C8 1.370(19) . ? C8 C13 1.388(18) . ? C13 C12 1.397(17) . ? C5' C6' 1.380(19) . ? C5' C12' 1.408(16) . ? C6' C7' 1.32(2) . ? C7' C8' 1.365(19) . ? C8' C13' 1.383(17) . ? C13' C12' 1.390(17) . ? C11 C14 1.420(9) . ? C15 C18 1.516(10) . ? C15 C16 1.531(10) . ? C16 C17 1.513(11) . ? C17 N1 1.390(9) . ? C18 N1 1.399(9) . ? N1 C19 1.429(9) . ? C19 C20 1.375(15) . ? C19 C24 1.413(16) . ? C20 C21 1.366(17) . ? C21 C22 1.39(2) . ? C22 C23 1.34(2) . ? C23 C24 1.374(19) . ? C20' C21' 1.384(17) . ? C21' C22' 1.39(2) . ? C22' C23' 1.33(2) . ? C23' C24' 1.366(18) . ? P1 F4' 1.471(14) . ? P1 F3 1.472(11) . ? P1 F1' 1.491(10) . ? P1 F5' 1.569(13) . ? P1 F5 1.570(10) . ? P1 F2 1.582(10) . ? P1 F6' 1.603(11) . ? P1 F4 1.606(11) . ? P1 F6 1.611(10) . ? P1 F2' 1.616(12) . ? P1 F1 1.627(9) . ? P1 F3' 1.639(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C28 Ru1 C28' 23.6(8) . . ? C28 Ru1 C27' 17.7(10) . . ? C28' Ru1 C27' 38.6(9) . . ? C28 Ru1 C25 63.3(8) . . ? C28' Ru1 C25 50.0(11) . . ? C27' Ru1 C25 64.3(10) . . ? C28 Ru1 C25' 68.4(10) . . ? C28' Ru1 C25' 62.5(11) . . ? C27' Ru1 C25' 63.0(9) . . ? C25 Ru1 C25' 19.4(8) . . ? C28 Ru1 C27 38.4(8) . . ? C28' Ru1 C27 56.1(11) . . ? C27' Ru1 C27 21.1(8) . . ? C25 Ru1 C27 63.4(7) . . ? C25' Ru1 C27 54.5(9) . . ? C28 Ru1 C29 37.1(8) . . ? C28' Ru1 C29 14.7(10) . . ? C27' Ru1 C29 49.5(10) . . ? C25 Ru1 C29 38.6(8) . . ? C25' Ru1 C29 54.3(12) . . ? C27 Ru1 C29 63.5(8) . . ? C28 Ru1 C26 63.8(8) . . ? C28' Ru1 C26 66.6(11) . . ? C27' Ru1 C26 52.8(11) . . ? C25 Ru1 C26 36.8(6) . . ? C25' Ru1 C26 19.5(8) . . ? C27 Ru1 C26 38.7(7) . . ? C29 Ru1 C26 63.3(7) . . ? C28 Ru1 C29' 56.4(11) . . ? C28' Ru1 C29' 37.0(9) . . ? C27' Ru1 C29' 63.7(10) . . ? C25 Ru1 C29' 19.2(9) . . ? C25' Ru1 C29' 38.2(9) . . ? C27 Ru1 C29' 70.3(9) . . ? C29 Ru1 C29' 23.0(9) . . ? C26 Ru1 C29' 53.5(9) . . ? C28 Ru1 C3 112.4(7) . . ? C28' Ru1 C3 105.1(9) . . ? C27' Ru1 C3 126.5(13) . . ? C25 Ru1 C3 131.1(9) . . ? C25' Ru1 C3 149.0(14) . . ? C27 Ru1 C3 144.6(11) . . ? C29 Ru1 C3 106.4(7) . . ? C26 Ru1 C3 167.9(8) . . ? C29' Ru1 C3 114.5(10) . . ? C28 Ru1 C4 136.5(8) . . ? C28' Ru1 C4 117.2(11) . . ? C27' Ru1 C4 154.2(14) . . ? C25 Ru1 C4 109.7(6) . . ? C25' Ru1 C4 120.1(11) . . ? C27 Ru1 C4 172.3(5) . . ? C29 Ru1 C4 109.0(6) . . ? C26 Ru1 C4 137.4(10) . . ? C29' Ru1 C4 102.0(7) . . ? C3 Ru1 C4 37.0(3) . . ? C28 Ru1 C26' 53.3(10) . . ? C28' Ru1 C26' 63.7(10) . . ? C27' Ru1 C26' 38.6(9) . . ? C25 Ru1 C26' 50.5(10) . . ? C25' Ru1 C26' 36.6(8) . . ? C27 Ru1 C26' 21.0(10) . . ? C29 Ru1 C26' 65.5(10) . . ? C26 Ru1 C26' 18.4(8) . . ? C29' Ru1 C26' 63.3(9) . . ? C3 Ru1 C26' 165.0(13) . . ? C4 Ru1 C26' 155.9(14) . . ? C26 C25 C29 109(2) . . ? C26 C25 Ru1 72.3(9) . . ? C29 C25 Ru1 71.1(10) . . ? C25 C26 C27 108(2) . . ? C25 C26 Ru1 70.9(9) . . ? C27 C26 Ru1 70.4(10) . . ? C28 C27 C26 106.0(19) . . ? C28 C27 Ru1 69.8(10) . . ? C26 C27 Ru1 70.9(9) . . ? C29 C28 C27 110(2) . . ? C29 C28 Ru1 72.5(11) . . ? C27 C28 Ru1 71.8(10) . . ? C28 C29 C25 107(2) . . ? C28 C29 Ru1 70.4(10) . . ? C25 C29 Ru1 70.3(10) . . ? C26' C25' C29' 111(2) . . ? C26' C25' Ru1 72.8(12) . . ? C29' C25' Ru1 71.6(13) . . ? C25' C26' C27' 107(2) . . ? C25' C26' Ru1 70.6(12) . . ? C27' C26' Ru1 69.6(12) . . ? C28' C27' C26' 106(2) . . ? C28' C27' Ru1 70.3(12) . . ? C26' C27' Ru1 71.9(12) . . ? C29' C28' C27' 110(3) . . ? C29' C28' Ru1 72.7(14) . . ? C27' C28' Ru1 71.1(13) . . ? C28' C29' C25' 106(3) . . ? C28' C29' Ru1 70.3(14) . . ? C25' C29' Ru1 70.2(12) . . ? C14 C1 C2 119.8(7) . . ? C14 C1 Ru1 72.5(4) . . ? C2 C1 Ru1 70.8(5) . . ? C3 C2 C1 119.6(8) . . ? C3 C2 Ru1 70.9(5) . . ? C1 C2 Ru1 71.7(5) . . ? C4 C3 C2 120.4(8) . . ? C4 C3 Ru1 71.6(5) . . ? C2 C3 Ru1 71.5(5) . . ? C3 C4 C11 119.9(7) . . ? C3 C4 Ru1 71.3(5) . . ? C11 C4 Ru1 71.8(4) . . ? C12' C10 C11 114.7(13) . . ? C11 C10 C12 105.4(14) . . ? C12' C10 C16 100.4(13) . . ? C11 C10 C16 105.0(6) . . ? C12 C10 C16 108.5(14) . . ? C14 C9 C13 105.3(12) . . ? C14 C9 C13' 112.9(11) . . ? C14 C9 C15 105.5(6) . . ? C13 C9 C15 110.6(13) . . ? C13' C9 C15 99.4(11) . . ? C6 C5 C12 121.4(16) . . ? C7 C6 C5 119.8(16) . . ? C6 C7 C8 123.5(17) . . ? C7 C8 C13 116.2(16) . . ? C8 C13 C12 124.2(13) . . ? C8 C13 C9 123.6(14) . . ? C12 C13 C9 112.2(13) . . ? C13 C12 C5 114.6(13) . . ? C13 C12 C10 114.3(13) . . ? C5 C12 C10 131.1(15) . . ? C6' C5' C12' 118.0(15) . . ? C7' C6' C5' 117.0(15) . . ? C6' C7' C8' 127.4(16) . . ? C7' C8' C13' 117.6(15) . . ? C8' C13' C12' 116.8(13) . . ? C8' C13' C9 129.7(13) . . ? C12' C13' C9 113.4(12) . . ? C13' C12' C5' 123.0(13) . . ? C13' C12' C10 113.8(12) . . ? C5' C12' C10 123.2(13) . . ? C4 C11 C14 120.3(7) . . ? C4 C11 C10 127.1(6) . . ? C14 C11 C10 112.5(6) . . ? C4 C11 Ru1 71.1(4) . . ? C14 C11 Ru1 72.3(4) . . ? C10 C11 Ru1 131.3(5) . . ? C1 C14 C11 119.9(7) . . ? C1 C14 C9 126.7(6) . . ? C11 C14 C9 113.3(6) . . ? C1 C14 Ru1 70.9(4) . . ? C11 C14 Ru1 70.3(4) . . ? C9 C14 Ru1 133.1(5) . . ? C18 C15 C16 105.1(6) . . ? C18 C15 C9 112.5(6) . . ? C16 C15 C9 110.1(6) . . ? C17 C16 C15 105.5(6) . . ? C17 C16 C10 112.7(6) . . ? C15 C16 C10 110.1(6) . . ? O1 C17 N1 126.1(8) . . ? O1 C17 C16 125.8(7) . . ? N1 C17 C16 108.1(6) . . ? O2 C18 N1 124.6(6) . . ? O2 C18 C15 127.4(6) . . ? N1 C18 C15 108.0(6) . . ? C17 N1 C18 113.3(6) . . ? C17 N1 C19 124.6(6) . . ? C18 N1 C19 122.0(6) . . ? C20 C19 C24 114.3(11) . . ? C20 C19 N1 121.2(10) . . ? C24 C19 N1 122.8(9) . . ? C21 C20 C19 122.5(15) . . ? C20 C21 C22 121.7(17) . . ? C23 C22 C21 116.8(15) . . ? C22 C23 C24 122.0(15) . . ? C23 C24 C19 122.1(14) . . ? C20' C21' C22' 118.7(17) . . ? C23' C22' C21' 122.9(15) . . ? C22' C23' C24' 120.4(15) . . ? F4' P1 F3 112.5(9) . . ? F4' P1 F1' 95.6(9) . . ? F3 P1 F1' 124.6(9) . . ? F4' P1 F5' 88.8(11) . . ? F3 P1 F5' 135.2(10) . . ? F1' P1 F5' 89.4(9) . . ? F4' P1 F5 92.1(11) . . ? F3 P1 F5 106.6(9) . . ? F1' P1 F5 119.4(7) . . ? F4' P1 F2 156.8(8) . . ? F3 P1 F2 88.2(7) . . ? F1' P1 F2 62.9(7) . . ? F5' P1 F2 82.8(8) . . ? F5 P1 F2 91.6(6) . . ? F4' P1 F6' 97.8(10) . . ? F1' P1 F6' 91.1(8) . . ? F5' P1 F6' 173.3(8) . . ? F5 P1 F6' 146.8(8) . . ? F2 P1 F6' 91.5(6) . . ? F3 P1 F4 92.3(7) . . ? F1' P1 F4 116.1(8) . . ? F5' P1 F4 97.5(9) . . ? F5 P1 F4 89.1(7) . . ? F2 P1 F4 178.9(8) . . ? F6' P1 F4 88.3(7) . . ? F4' P1 F6 84.9(11) . . ? F3 P1 F6 82.8(8) . . ? F1' P1 F6 52.3(7) . . ? F5' P1 F6 140.1(9) . . ? F5 P1 F6 170.6(7) . . ? F2 P1 F6 87.8(6) . . ? F4 P1 F6 91.4(7) . . ? F4' P1 F2' 172.2(11) . . ? F3 P1 F2' 65.2(8) . . ? F1' P1 F2' 91.6(8) . . ? F5' P1 F2' 88.3(9) . . ? F5 P1 F2' 81.8(8) . . ? F6' P1 F2' 85.0(7) . . ? F4 P1 F2' 151.6(8) . . ? F6 P1 F2' 101.9(7) . . ? F4' P1 F1 65.3(8) . . ? F3 P1 F1 167.7(9) . . ? F1' P1 F1 46.0(6) . . ? F5' P1 F1 56.9(8) . . ? F5 P1 F1 85.7(6) . . ? F2 P1 F1 92.2(6) . . ? F6' P1 F1 127.2(8) . . ? F4 P1 F1 87.1(7) . . ? F6 P1 F1 84.9(6) . . ? F2' P1 F1 118.6(7) . . ? F4' P1 F3' 93.7(9) . . ? F3 P1 F3' 46.1(7) . . ? F1' P1 F3' 169.3(8) . . ? F5' P1 F3' 96.0(9) . . ? F5 P1 F3' 65.4(8) . . ? F2 P1 F3' 108.6(8) . . ? F6' P1 F3' 82.4(8) . . ? F4 P1 F3' 72.4(8) . . ? F6 P1 F3' 123.6(8) . . ? F2' P1 F3' 79.5(8) . . ? F1 P1 F3' 144.1(7) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.747 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.088 #===END