# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email chenwzz@zju.edu.cn _publ_contact_author_name 'Wanzhi Chen' loop_ _publ_author_name 'Wanzhi Chen' 'Xiaolong Liu' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 834943' #TrackingRef '- cif-Rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H26 F12 N10 P2 Ru' _chemical_formula_weight 857.57 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.3495(6) _cell_length_b 15.8744(4) _cell_length_c 13.4608(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.229(3) _cell_angle_gamma 90.00 _cell_volume 3414.32(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.653 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7444 _exptl_absorpt_correction_T_max 0.8382 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8390 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3014 _reflns_number_gt 2455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1084P)^2^+3.0370P] 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 3014 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1526 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.5000 0.84308(3) 0.7500 0.0360(2) Uani 1 2 d S . . C1 C 0.5000 1.0644(5) 0.7500 0.060(2) Uani 1 2 d S . . H1A H 0.4578 1.1004 0.7688 0.072 Uiso 0.50 1 calc PR . . H1B H 0.5422 1.1004 0.7312 0.072 Uiso 0.50 1 calc PR . . C2 C 0.5798(4) 1.0490(3) 0.9300(5) 0.0603(15) Uani 1 1 d . . . H2 H 0.5844 1.1061 0.9453 0.072 Uiso 1 1 calc R . . C3 C 0.6111(4) 0.9869(3) 0.9922(4) 0.0598(15) Uani 1 1 d . . . H3 H 0.6418 0.9919 1.0585 0.072 Uiso 1 1 calc R . . C4 C 0.5448(3) 0.9301(3) 0.8440(4) 0.0399(11) Uani 1 1 d . . . C5 C 0.3948(3) 0.8260(3) 0.5379(4) 0.0430(11) Uani 1 1 d . . . C6 C 0.3456(4) 0.7999(4) 0.4478(4) 0.0606(15) Uani 1 1 d . . . H6 H 0.3224 0.8386 0.3979 0.073 Uiso 1 1 calc R . . C7 C 0.3315(4) 0.7149(4) 0.4334(4) 0.0677(17) Uani 1 1 d . . . H7 H 0.2987 0.6949 0.3729 0.081 Uiso 1 1 calc R . . C8 C 0.3667(4) 0.6596(3) 0.5097(5) 0.0645(16) Uani 1 1 d . . . H8 H 0.3577 0.6019 0.5016 0.077 Uiso 1 1 calc R . . C9 C 0.4152(3) 0.6910(3) 0.5978(4) 0.0489(12) Uani 1 1 d . . . H9 H 0.4388 0.6535 0.6489 0.059 Uiso 1 1 calc R . . C10 C 0.3372(4) 0.8289(3) 0.8393(4) 0.0481(12) Uani 1 1 d . . . C11 C 0.2627(4) 0.8183(4) 0.8808(6) 0.0741(18) Uani 1 1 d . . . H11A H 0.2290 0.7738 0.8452 0.111 Uiso 1 1 calc R . . H11B H 0.2311 0.8698 0.8728 0.111 Uiso 1 1 calc R . . H11C H 0.2787 0.8044 0.9516 0.111 Uiso 1 1 calc R . . C12 C 0.0529(5) 0.8257(5) 0.9025(8) 0.095(3) Uani 1 1 d . . . C13 C 0.0438(5) 0.9154(5) 0.9008(7) 0.101(3) Uani 1 1 d . . . H13A H 0.0531 0.9362 0.9692 0.151 Uiso 1 1 calc R . . H13B H -0.0118 0.9300 0.8655 0.151 Uiso 1 1 calc R . . H13C H 0.0838 0.9401 0.8666 0.151 Uiso 1 1 calc R . . F1 F 0.7907(5) 0.0692(6) 0.9070(4) 0.178(3) Uani 1 1 d . . . F2 F 0.7012(4) 0.0440(8) 0.7602(6) 0.243(6) Uani 1 1 d . . . F3 F 0.7975(4) 0.0343(4) 0.6793(4) 0.1322(19) Uani 1 1 d . . . F4 F 0.8897(4) 0.0633(7) 0.8226(6) 0.216(4) Uani 1 1 d . . . F5 F 0.7863(7) 0.1434(3) 0.7665(7) 0.220(5) Uani 1 1 d . . . F6 F 0.8039(10) -0.0386(4) 0.8168(6) 0.315(8) Uani 1 1 d . . . N1 N 0.5888(3) 0.9124(2) 0.9383(3) 0.0436(10) Uani 1 1 d . . . N2 N 0.5389(3) 1.0144(2) 0.8381(3) 0.0452(10) Uani 1 1 d . . . N3 N 0.4298(2) 0.7734(2) 0.6132(3) 0.0402(9) Uani 1 1 d . . . N4 N 0.3961(3) 0.8368(2) 0.8072(3) 0.0416(9) Uani 1 1 d . . . N5 N 0.0627(6) 0.7569(5) 0.9035(10) 0.161(5) Uani 1 1 d . . . P1 P 0.79395(10) 0.05152(10) 0.79535(12) 0.0626(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 0.0424(3) 0.0320(3) 0.0332(3) 0.000 0.0074(2) 0.000 C1 0.064(5) 0.044(4) 0.070(6) 0.000 0.009(4) 0.000 C2 0.077(4) 0.040(3) 0.063(4) -0.017(3) 0.012(3) -0.014(3) C3 0.069(4) 0.057(3) 0.050(3) -0.018(3) 0.003(3) -0.013(3) C4 0.043(3) 0.038(2) 0.042(3) -0.005(2) 0.014(2) -0.0009(19) C5 0.046(3) 0.050(3) 0.034(3) 0.001(2) 0.010(2) 0.002(2) C6 0.066(4) 0.065(4) 0.044(3) 0.002(3) -0.003(3) 0.006(3) C7 0.075(4) 0.077(4) 0.043(3) -0.017(3) -0.004(3) -0.011(3) C8 0.078(4) 0.056(3) 0.056(4) -0.014(3) 0.007(3) -0.008(3) C9 0.061(3) 0.043(3) 0.043(3) -0.001(2) 0.011(2) -0.001(2) C10 0.054(3) 0.047(3) 0.043(3) 0.000(2) 0.010(2) -0.002(2) C11 0.068(4) 0.085(4) 0.079(5) 0.000(4) 0.034(4) -0.008(3) C12 0.075(5) 0.076(5) 0.142(8) -0.002(5) 0.041(5) -0.001(4) C13 0.091(6) 0.075(5) 0.129(7) 0.012(5) 0.008(5) 0.016(4) F1 0.158(6) 0.306(10) 0.071(4) -0.034(5) 0.031(3) -0.042(6) F2 0.073(4) 0.528(18) 0.126(6) 0.034(8) 0.017(4) -0.055(6) F3 0.170(5) 0.149(4) 0.073(3) -0.006(3) 0.015(3) 0.028(4) F4 0.090(4) 0.378(14) 0.161(7) -0.001(7) -0.016(4) 0.001(6) F5 0.350(14) 0.072(3) 0.194(8) -0.027(4) -0.044(8) 0.028(5) F6 0.63(2) 0.081(4) 0.161(7) 0.058(4) -0.089(10) -0.029(7) N1 0.049(2) 0.039(2) 0.041(2) -0.0068(17) 0.0058(18) -0.0068(17) N2 0.049(2) 0.035(2) 0.053(3) -0.0043(18) 0.015(2) -0.0028(17) N3 0.045(2) 0.040(2) 0.036(2) -0.0009(17) 0.0080(17) 0.0018(17) N4 0.048(2) 0.037(2) 0.039(2) -0.0020(16) 0.0090(19) -0.0015(17) N5 0.140(8) 0.066(4) 0.295(15) 0.004(6) 0.085(9) 0.017(5) P1 0.0638(10) 0.0613(9) 0.0557(10) 0.0088(7) -0.0034(7) 0.0034(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C4 1.912(4) . ? Ru1 C4 1.912(4) 2_656 ? Ru1 N4 2.010(4) . ? Ru1 N4 2.010(4) 2_656 ? Ru1 N3 2.244(4) . ? Ru1 N3 2.244(4) 2_656 ? C1 N2 1.456(6) 2_656 ? C1 N2 1.456(6) . ? C2 C3 1.324(8) . ? C2 N2 1.388(7) . ? C3 N1 1.395(6) . ? C4 N2 1.343(6) . ? C4 N1 1.349(6) . ? C5 N3 1.344(6) . ? C5 C6 1.369(7) . ? C5 N1 1.422(6) 2_656 ? C6 C7 1.376(9) . ? C7 C8 1.382(9) . ? C8 C9 1.373(8) . ? C9 N3 1.338(6) . ? C10 N4 1.143(7) . ? C10 C11 1.453(8) . ? C12 N5 1.104(9) . ? C12 C13 1.431(10) . ? F1 P1 1.541(6) . ? F2 P1 1.494(6) . ? F3 P1 1.599(5) . ? F4 P1 1.543(7) . ? F5 P1 1.507(6) . ? F6 P1 1.462(6) . ? N1 C5 1.422(6) 2_656 ? 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 Ru1 C4 87.4(3) . 2_656 ? C4 Ru1 N4 91.10(17) . . ? C4 Ru1 N4 93.03(18) 2_656 . ? C4 Ru1 N4 93.03(18) . 2_656 ? C4 Ru1 N4 91.10(17) 2_656 2_656 ? N4 Ru1 N4 174.3(2) . 2_656 ? C4 Ru1 N3 163.14(17) . . ? C4 Ru1 N3 75.84(17) 2_656 . ? N4 Ru1 N3 87.86(15) . . ? N4 Ru1 N3 89.33(15) 2_656 . ? C4 Ru1 N3 75.84(17) . 2_656 ? C4 Ru1 N3 163.14(17) 2_656 2_656 ? N4 Ru1 N3 89.33(15) . 2_656 ? N4 Ru1 N3 87.86(15) 2_656 2_656 ? N3 Ru1 N3 120.95(19) . 2_656 ? N2 C1 N2 114.0(6) 2_656 . ? C3 C2 N2 108.6(4) . . ? C2 C3 N1 106.2(5) . . ? N2 C4 N1 106.3(4) . . ? N2 C4 Ru1 132.0(4) . . ? N1 C4 Ru1 121.7(3) . . ? N3 C5 C6 123.8(5) . . ? N3 C5 N1 113.5(4) . 2_656 ? C6 C5 N1 122.6(5) . 2_656 ? C5 C6 C7 118.1(5) . . ? C6 C7 C8 119.2(5) . . ? C9 C8 C7 119.0(5) . . ? N3 C9 C8 122.8(5) . . ? N4 C10 C11 179.5(7) . . ? N5 C12 C13 177.7(10) . . ? C4 N1 C3 110.0(4) . . ? C4 N1 C5 116.8(4) . 2_656 ? C3 N1 C5 133.2(4) . 2_656 ? C4 N2 C2 109.0(4) . . ? C4 N2 C1 127.2(4) . . ? C2 N2 C1 123.8(4) . . ? C9 N3 C5 117.2(4) . . ? C9 N3 Ru1 130.7(3) . . ? C5 N3 Ru1 112.0(3) . . ? C10 N4 Ru1 176.6(4) . . ? F6 P1 F2 92.7(7) . . ? F6 P1 F5 175.9(7) . . ? F2 P1 F5 88.4(6) . . ? F6 P1 F1 90.6(5) . . ? F2 P1 F1 94.6(4) . . ? F5 P1 F1 93.2(5) . . ? F6 P1 F4 90.4(7) . . ? F2 P1 F4 174.9(5) . . ? F5 P1 F4 88.2(6) . . ? F1 P1 F4 89.4(4) . . ? F6 P1 F3 90.0(5) . . ? F2 P1 F3 85.5(4) . . ? F5 P1 F3 86.1(4) . . ? F1 P1 F3 179.3(4) . . ? F4 P1 F3 90.5(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.010 _refine_diff_density_min -0.624 _refine_diff_density_rms 0.101 #===END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 834944' #TrackingRef '- cif-Rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46.50 Cl2 F12 N7.50 P2 Ru2' _chemical_formula_weight 1195.33 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1071(3) _cell_length_b 17.3056(6) _cell_length_c 19.5857(6) _cell_angle_alpha 65.606(3) _cell_angle_beta 87.553(3) _cell_angle_gamma 84.694(3) _cell_volume 2491.77(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1198 _exptl_absorpt_coefficient_mu 0.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6831 _exptl_absorpt_correction_T_max 0.8819 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24608 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8775 _reflns_number_gt 5870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. The following restraints have been used to DFIX the bond distances and to solve PLAT220 ALERT: simu 0.005 0.01 3.8 $C DFIX N8 C40 2.70 0.01 DFIX C40 C41 1.40 0.01 DFIX N8 C41 1.10 0.01 ; _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^)+(0.0844P)^2^+2.6138P] 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 8775 _refine_ls_number_parameters 597 _refine_ls_number_restraints 724 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.066 _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 -0.07843(5) 0.48043(3) 0.28905(3) 0.03470(16) Uani 1 1 d . . . Ru2 Ru 0.23964(6) 0.05946(3) 0.29500(3) 0.03862(17) Uani 1 1 d . . . C1 C 0.1694(10) -0.1240(5) 0.3957(4) 0.0635(13) Uani 1 1 d U . . H1 H 0.2701 -0.1386 0.3778 0.076 Uiso 1 1 calc R . . C2 C 0.0786(10) -0.1872(5) 0.4442(4) 0.0659(14) Uani 1 1 d U . . H2 H 0.1178 -0.2440 0.4594 0.079 Uiso 1 1 calc R . . C3 C -0.0691(10) -0.1660(5) 0.4697(4) 0.0678(14) Uani 1 1 d U . . H3 H -0.1345 -0.2087 0.5003 0.081 Uiso 1 1 calc R . . C4 C -0.1233(9) -0.0818(5) 0.4506(4) 0.0608(12) Uani 1 1 d U . . H4 H -0.2232 -0.0664 0.4687 0.073 Uiso 1 1 calc R . . C5 C -0.0235(9) -0.0220(4) 0.4039(4) 0.0535(11) Uani 1 1 d U . . C6 C 0.0488(8) 0.1188(4) 0.3304(4) 0.0505(10) Uani 1 1 d U . . C7 C -0.1750(8) 0.1107(4) 0.4065(4) 0.0530(12) Uani 1 1 d U . . H7 H -0.2584 0.0885 0.4414 0.064 Uiso 1 1 calc R . . C8 C -0.1446(8) 0.1921(4) 0.3707(4) 0.0519(12) Uani 1 1 d U . . H8 H -0.2041 0.2379 0.3760 0.062 Uiso 1 1 calc R . . C9 C 0.0600(8) 0.2757(4) 0.2747(4) 0.0498(10) Uani 1 1 d U . . H9A H 0.1349 0.2646 0.2392 0.060 Uiso 1 1 calc R . . H9B H -0.0287 0.3167 0.2465 0.060 Uiso 1 1 calc R . . C10 C 0.2928(8) 0.2722(4) 0.3555(4) 0.0462(11) Uani 1 1 d U . . H10 H 0.3466 0.2208 0.3591 0.055 Uiso 1 1 calc R . . C11 C 0.3411(8) 0.3211(4) 0.3873(4) 0.0458(11) Uani 1 1 d U . . H11 H 0.4335 0.3109 0.4173 0.055 Uiso 1 1 calc R . . C12 C 0.1049(7) 0.3855(4) 0.3210(4) 0.0425(10) Uani 1 1 d U . . C13 C 0.1991(7) 0.4569(4) 0.3900(4) 0.0422(10) Uani 1 1 d U . . C14 C 0.3085(8) 0.4699(4) 0.4363(4) 0.0480(11) Uani 1 1 d U . . H14 H 0.4077 0.4362 0.4514 0.058 Uiso 1 1 calc R . . C15 C 0.2650(8) 0.5335(4) 0.4586(4) 0.0538(12) Uani 1 1 d U . . H15 H 0.3356 0.5446 0.4891 0.065 Uiso 1 1 calc R . . C16 C 0.1180(8) 0.5813(4) 0.4364(4) 0.0505(12) Uani 1 1 d U . . H16 H 0.0882 0.6247 0.4520 0.061 Uiso 1 1 calc R . . C17 C 0.0135(8) 0.5652(4) 0.3910(4) 0.0488(11) Uani 1 1 d U . . H17 H -0.0877 0.5973 0.3768 0.059 Uiso 1 1 calc R . . C18 C -0.0402(8) 0.6085(4) 0.2014(4) 0.0527(11) Uani 1 1 d U . . C19 C 0.0000(8) 0.5469(4) 0.1724(4) 0.0514(11) Uani 1 1 d U . . H19 H 0.1039 0.5441 0.1510 0.062 Uiso 1 1 calc R . . C20 C -0.1149(8) 0.4896(4) 0.1753(4) 0.0502(11) Uani 1 1 d U . . H20 H -0.0856 0.4500 0.1553 0.060 Uiso 1 1 calc R . . C21 C -0.2720(8) 0.4903(4) 0.2075(4) 0.0544(12) Uani 1 1 d U . . C22 C -0.3124(9) 0.5535(4) 0.2356(4) 0.0556(12) Uani 1 1 d U . . H22 H -0.4156 0.5556 0.2577 0.067 Uiso 1 1 calc R . . C23 C -0.2014(8) 0.6123(4) 0.2311(4) 0.0560(11) Uani 1 1 d U . . H23 H -0.2337 0.6546 0.2477 0.067 Uiso 1 1 calc R . . C24 C -0.3926(10) 0.4266(5) 0.2145(5) 0.076(2) Uani 1 1 d U . . H24A H -0.3445 0.3884 0.1936 0.114 Uiso 1 1 calc R . . H24B H -0.4923 0.4558 0.1880 0.114 Uiso 1 1 calc R . . H24C H -0.4182 0.3949 0.2665 0.114 Uiso 1 1 calc R . . C25 C 0.0791(9) 0.6723(4) 0.1996(4) 0.0599(13) Uani 1 1 d U . . H25 H 0.0559 0.6833 0.2445 0.072 Uiso 1 1 calc R . . C26 C 0.2566(10) 0.6431(5) 0.2021(5) 0.078(2) Uani 1 1 d U . . H26A H 0.2762 0.5886 0.2433 0.117 Uiso 1 1 calc R . . H26B H 0.3212 0.6835 0.2084 0.117 Uiso 1 1 calc R . . H26C H 0.2880 0.6383 0.1561 0.117 Uiso 1 1 calc R . . C27 C 0.0380(11) 0.7556(5) 0.1327(5) 0.085(2) Uani 1 1 d U . . H27A H 0.1083 0.7973 0.1325 0.127 Uiso 1 1 calc R . . H27B H -0.0757 0.7750 0.1358 0.127 Uiso 1 1 calc R . . H27C H 0.0553 0.7472 0.0874 0.127 Uiso 1 1 calc R . . C28 C 0.6242(11) 0.1275(7) 0.2492(5) 0.098(2) Uani 1 1 d U . . H28A H 0.6565 0.0871 0.2986 0.148 Uiso 1 1 calc R . . H28B H 0.6026 0.1830 0.2491 0.148 Uiso 1 1 calc R . . H28C H 0.7118 0.1286 0.2143 0.148 Uiso 1 1 calc R . . C29 C 0.4680(10) 0.1016(6) 0.2264(4) 0.0686(14) Uani 1 1 d U . . C30 C 0.4551(10) 0.0164(5) 0.2420(4) 0.0710(14) Uani 1 1 d U . . H30 H 0.5437 -0.0232 0.2644 0.085 Uiso 1 1 calc R . . C31 C 0.3146(10) -0.0108(5) 0.2251(4) 0.0697(12) Uani 1 1 d U . . H31 H 0.3099 -0.0682 0.2362 0.084 Uiso 1 1 calc R . . C32 C 0.1767(10) 0.0472(6) 0.1911(4) 0.0689(12) Uani 1 1 d U . . C33 C 0.1927(10) 0.1315(5) 0.1768(4) 0.0701(12) Uani 1 1 d U . . H33 H 0.1040 0.1716 0.1559 0.084 Uiso 1 1 calc R . . C34 C 0.3391(10) 0.1584(5) 0.1928(4) 0.0666(12) Uani 1 1 d U . . H34 H 0.3473 0.2160 0.1802 0.080 Uiso 1 1 calc R . . C35 C 0.0191(12) 0.0247(6) 0.1668(5) 0.0854(16) Uani 1 1 d U . . H35 H -0.0641 0.0717 0.1615 0.103 Uiso 1 1 calc R . . C36 C 0.0486(13) 0.0291(7) 0.0880(5) 0.105(2) Uani 1 1 d U . . H36A H 0.1251 -0.0175 0.0900 0.158 Uiso 1 1 calc R . . H36B H 0.0937 0.0819 0.0569 0.158 Uiso 1 1 calc R . . H36C H -0.0545 0.0258 0.0674 0.158 Uiso 1 1 calc R . . C37 C -0.0513(13) -0.0482(7) 0.2137(6) 0.102(2) Uani 1 1 d U . . H37A H 0.0294 -0.0961 0.2260 0.153 Uiso 1 1 calc R . . H37B H -0.1435 -0.0566 0.1890 0.153 Uiso 1 1 calc R . . H37C H -0.0891 -0.0428 0.2588 0.153 Uiso 1 1 calc R . . C38 C 0.2831(10) 0.4002(5) 0.0791(6) 0.071(2) Uani 1 1 d U . . C39 C 0.3138(12) 0.4079(7) 0.0032(5) 0.094(3) Uani 1 1 d U . . H39A H 0.4184 0.4311 -0.0140 0.141 Uiso 1 1 calc R . . H39B H 0.2272 0.4449 -0.0289 0.141 Uiso 1 1 calc R . . H39C H 0.3160 0.3527 0.0024 0.141 Uiso 1 1 calc R . . C40 C 0.516(4) 0.857(2) 0.034(2) 0.210(13) Uiso 0.50 1 d PDU . . H40A H 0.4490 0.8622 -0.0071 0.314 Uiso 0.50 1 calc PR . . H40B H 0.4650 0.8227 0.0804 0.314 Uiso 0.50 1 calc PR . . H40C H 0.6241 0.8317 0.0302 0.314 Uiso 0.50 1 calc PR . . C41 C 0.531(5) 0.942(2) 0.031(3) 0.221(14) Uiso 0.50 1 d PDU . . Cl1 Cl 0.3850(2) 0.04933(11) 0.40329(10) 0.0510(4) Uani 1 1 d . . . Cl2 Cl -0.23043(19) 0.38711(10) 0.39430(9) 0.0471(4) Uani 1 1 d . . . F1 F 0.7671(15) 0.2306(5) 0.0710(5) 0.210(5) Uani 1 1 d . . . F2 F 0.8875(8) 0.2826(5) 0.1374(3) 0.127(2) Uani 1 1 d . . . F3 F 0.8832(14) 0.4044(5) 0.0417(6) 0.204(4) Uani 1 1 d . . . F4 F 0.7400(9) 0.3562(5) -0.0237(3) 0.148(3) Uani 1 1 d . . . F5 F 0.6538(8) 0.3433(8) 0.0856(4) 0.222(5) Uani 1 1 d . . . F6 F 0.9850(9) 0.2948(6) 0.0262(4) 0.159(3) Uani 1 1 d . . . F7 F 0.5977(8) 0.8307(3) 0.3656(4) 0.120(2) Uani 1 1 d . . . F8 F 0.7214(10) 0.7607(4) 0.3018(5) 0.163(3) Uani 1 1 d . . . F9 F 0.5906(7) 0.6471(3) 0.3686(3) 0.0993(17) Uani 1 1 d . . . F10 F 0.4726(7) 0.7120(4) 0.4375(3) 0.1128(19) Uani 1 1 d . . . F11 F 0.4398(9) 0.7718(4) 0.3162(4) 0.143(3) Uani 1 1 d . . . F12 F 0.7476(7) 0.7040(4) 0.4234(4) 0.128(2) Uani 1 1 d . . . N1 N 0.1162(6) -0.0403(3) 0.3732(3) 0.0445(13) Uani 1 1 d . . . N2 N -0.0566(6) 0.0662(3) 0.3808(3) 0.0428(12) Uani 1 1 d . . . N3 N -0.0096(6) 0.1967(3) 0.3243(3) 0.0414(12) Uani 1 1 d . . . N4 N 0.1482(6) 0.3113(3) 0.3159(3) 0.0370(11) Uani 1 1 d . . . N5 N 0.2228(5) 0.3913(3) 0.3659(3) 0.0326(11) Uani 1 1 d . . . N6 N 0.0563(5) 0.5035(3) 0.3669(3) 0.0351(11) Uani 1 1 d . . . N7 N 0.2602(9) 0.3926(5) 0.1390(5) 0.086(2) Uani 1 1 d . . . N8 N 0.529(6) 1.014(3) 0.029(3) 0.32(2) Uiso 0.50 1 d PD . . P1 P 0.8134(3) 0.31902(17) 0.05598(14) 0.0782(7) Uani 1 1 d . . . P2 P 0.5937(3) 0.73829(13) 0.36709(14) 0.0731(6) 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 0.0381(3) 0.0348(3) 0.0339(3) -0.0177(2) -0.0031(2) 0.00281(19) Ru2 0.0449(3) 0.0321(3) 0.0389(3) -0.0158(2) 0.0073(2) -0.0010(2) C1 0.080(2) 0.054(2) 0.059(2) -0.027(2) 0.017(2) -0.013(2) C2 0.086(3) 0.051(3) 0.062(3) -0.024(2) 0.014(2) -0.016(2) C3 0.084(3) 0.055(3) 0.064(3) -0.022(2) 0.016(2) -0.021(2) C4 0.072(2) 0.055(2) 0.059(2) -0.027(2) 0.016(2) -0.017(2) C5 0.067(2) 0.049(2) 0.055(2) -0.0311(18) 0.0120(19) -0.0147(18) C6 0.0607(19) 0.0528(18) 0.0500(19) -0.0329(16) 0.0071(17) -0.0091(17) C7 0.058(2) 0.053(2) 0.057(2) -0.033(2) 0.012(2) -0.009(2) C8 0.057(2) 0.053(2) 0.058(2) -0.036(2) 0.007(2) -0.004(2) C9 0.0592(18) 0.0487(18) 0.0499(18) -0.0291(16) 0.0021(17) -0.0042(16) C10 0.050(2) 0.042(2) 0.050(2) -0.0226(19) 0.002(2) -0.0004(19) C11 0.047(2) 0.041(2) 0.050(2) -0.0206(19) 0.000(2) -0.0012(19) C12 0.0474(18) 0.0424(18) 0.0440(18) -0.0242(16) -0.0017(16) -0.0013(16) C13 0.050(2) 0.0393(19) 0.047(2) -0.0262(17) -0.0015(18) -0.0048(17) C14 0.054(2) 0.044(2) 0.052(2) -0.0253(18) -0.0060(19) -0.0047(18) C15 0.062(2) 0.051(2) 0.056(2) -0.028(2) -0.009(2) -0.006(2) C16 0.062(2) 0.046(2) 0.053(2) -0.030(2) -0.006(2) -0.004(2) C17 0.060(2) 0.044(2) 0.050(2) -0.0270(17) -0.0052(18) -0.0019(18) C18 0.0598(19) 0.0495(19) 0.048(2) -0.0200(17) -0.0061(18) 0.0010(17) C19 0.058(2) 0.051(2) 0.046(2) -0.0213(18) -0.0055(18) 0.0029(18) C20 0.059(2) 0.050(2) 0.044(2) -0.0235(17) -0.0054(18) 0.0031(18) C21 0.057(2) 0.056(2) 0.050(2) -0.0206(19) -0.0105(19) -0.0025(19) C22 0.056(2) 0.061(2) 0.047(2) -0.020(2) -0.006(2) 0.006(2) C23 0.062(2) 0.052(2) 0.051(2) -0.0192(18) -0.0065(19) 0.0065(18) C24 0.069(4) 0.088(4) 0.067(4) -0.024(4) -0.016(3) -0.018(3) C25 0.070(2) 0.051(2) 0.055(2) -0.019(2) -0.004(2) -0.002(2) C26 0.081(4) 0.066(4) 0.074(4) -0.012(3) -0.006(3) -0.019(3) C27 0.098(4) 0.059(4) 0.078(4) -0.010(3) 0.000(4) -0.004(3) C28 0.091(4) 0.114(5) 0.077(4) -0.024(4) 0.018(4) -0.027(4) C29 0.074(3) 0.081(3) 0.052(2) -0.029(2) 0.019(2) -0.013(2) C30 0.077(3) 0.079(3) 0.053(2) -0.026(2) 0.021(2) 0.003(2) C31 0.087(2) 0.074(2) 0.054(2) -0.0339(19) 0.020(2) -0.007(2) C32 0.079(2) 0.081(2) 0.053(2) -0.034(2) 0.012(2) -0.011(2) C33 0.079(2) 0.077(2) 0.053(2) -0.0280(19) 0.0130(19) -0.0002(19) C34 0.080(2) 0.068(2) 0.053(2) -0.0277(19) 0.017(2) -0.008(2) C35 0.098(3) 0.096(3) 0.063(3) -0.033(3) 0.008(3) -0.014(3) C36 0.118(4) 0.121(4) 0.074(4) -0.037(4) 0.005(4) -0.021(4) C37 0.115(4) 0.108(4) 0.080(4) -0.032(3) 0.003(4) -0.027(4) C38 0.067(5) 0.069(5) 0.067(5) -0.017(5) -0.010(4) -0.003(4) C39 0.091(6) 0.105(6) 0.069(6) -0.020(5) -0.014(5) 0.002(5) Cl1 0.0545(9) 0.0513(10) 0.0474(10) -0.0213(8) 0.0003(8) -0.0003(7) Cl2 0.0530(9) 0.0475(9) 0.0456(10) -0.0240(8) 0.0065(7) -0.0069(7) F1 0.367(14) 0.151(7) 0.138(7) -0.061(6) -0.001(8) -0.136(8) F2 0.133(5) 0.173(6) 0.091(4) -0.075(4) -0.046(4) 0.038(4) F3 0.276(11) 0.115(6) 0.231(10) -0.073(7) -0.035(9) -0.038(7) F4 0.146(6) 0.205(8) 0.073(4) -0.041(5) -0.023(4) 0.019(5) F5 0.097(5) 0.461(16) 0.128(6) -0.166(9) -0.033(4) 0.110(7) F6 0.120(5) 0.225(9) 0.153(7) -0.103(6) 0.027(5) 0.000(5) F7 0.146(5) 0.054(3) 0.157(6) -0.048(4) 0.011(4) 0.017(3) F8 0.208(7) 0.099(5) 0.187(7) -0.070(5) 0.128(6) -0.045(5) F9 0.107(4) 0.065(3) 0.137(5) -0.055(3) 0.022(3) -0.001(3) F10 0.121(4) 0.100(4) 0.108(4) -0.041(4) 0.044(4) 0.005(3) F11 0.168(6) 0.113(5) 0.150(6) -0.061(5) -0.065(5) 0.051(4) F12 0.109(4) 0.082(4) 0.194(7) -0.058(4) -0.038(4) 0.016(3) N1 0.054(3) 0.031(3) 0.047(3) -0.015(3) 0.006(3) -0.005(2) N2 0.038(3) 0.046(3) 0.053(3) -0.029(3) 0.011(2) -0.007(2) N3 0.043(3) 0.041(3) 0.051(3) -0.030(3) -0.002(2) 0.001(2) N4 0.039(3) 0.035(3) 0.040(3) -0.020(2) 0.000(2) 0.001(2) N5 0.034(2) 0.030(3) 0.035(3) -0.015(2) -0.004(2) 0.0026(19) N6 0.038(3) 0.033(3) 0.038(3) -0.017(2) -0.001(2) -0.001(2) N7 0.076(5) 0.102(6) 0.079(6) -0.032(5) 0.001(4) -0.018(4) P1 0.0856(16) 0.0884(18) 0.0664(16) -0.0377(14) -0.0073(12) -0.0034(13) P2 0.0800(15) 0.0465(12) 0.0841(17) -0.0234(11) 0.0164(13) 0.0125(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C12 2.020(6) . ? Ru1 N6 2.098(4) . ? Ru1 C19 2.188(7) . ? Ru1 C20 2.197(7) . ? Ru1 C18 2.212(7) . ? Ru1 C22 2.219(7) . ? Ru1 C21 2.233(6) . ? Ru1 C23 2.242(7) . ? Ru1 Cl2 2.4035(16) . ? Ru2 C6 2.032(7) . ? Ru2 N1 2.081(5) . ? Ru2 C33 2.160(8) . ? Ru2 C34 2.208(8) . ? Ru2 C31 2.210(8) . ? Ru2 C32 2.215(8) . ? Ru2 C30 2.220(7) . ? Ru2 C29 2.235(7) . ? Ru2 Cl1 2.4054(17) . ? C1 N1 1.361(9) . ? C1 C2 1.367(10) . ? C2 C3 1.355(10) . ? C3 C4 1.379(10) . ? C4 C5 1.369(9) . ? C5 N1 1.333(8) . ? C5 N2 1.404(8) . ? C6 N3 1.345(8) . ? C6 N2 1.366(8) . ? C7 C8 1.331(9) . ? C7 N2 1.382(8) . ? C8 N3 1.379(8) . ? C9 N4 1.443(7) . ? C9 N3 1.459(8) . ? C10 C11 1.333(8) . ? C10 N4 1.390(8) . ? C11 N5 1.403(7) . ? C12 N4 1.342(7) . ? C12 N5 1.364(7) . ? C13 N6 1.329(7) . ? C13 C14 1.390(8) . ? C13 N5 1.395(7) . ? C14 C15 1.357(9) . ? C15 C16 1.362(9) . ? C16 C17 1.378(9) . ? C17 N6 1.348(7) . ? C18 C19 1.410(9) . ? C18 C23 1.414(9) . ? C18 C25 1.522(9) . ? C19 C20 1.404(9) . ? C20 C21 1.398(9) . ? C21 C22 1.423(10) . ? C21 C24 1.501(9) . ? C22 C23 1.393(9) . ? C25 C26 1.476(10) . ? C25 C27 1.515(10) . ? C28 C29 1.524(11) . ? C29 C34 1.351(11) . ? C29 C30 1.390(11) . ? C30 C31 1.374(11) . ? C31 C32 1.415(11) . ? C32 C33 1.384(11) . ? C32 C35 1.520(11) . ? C33 C34 1.407(11) . ? C35 C37 1.376(12) . ? C35 C36 1.524(12) . ? C38 N7 1.133(11) . ? C38 C39 1.449(13) . ? C40 C41 1.460(9) . ? C41 N8 1.20(5) 2_675 ? C41 N8 1.220(9) . ? C41 C41 1.90(8) 2_675 ? F1 P1 1.514(7) . ? F2 P1 1.575(6) . ? F3 P1 1.543(8) . ? F4 P1 1.544(6) . ? F5 P1 1.492(6) . ? F6 P1 1.574(7) . ? F7 P2 1.590(5) . ? F8 P2 1.552(6) . ? F9 P2 1.569(5) . ? F10 P2 1.587(6) . ? F11 P2 1.543(7) . ? F12 P2 1.602(6) . ? N8 C41 1.20(5) 2_675 ? N8 N8 1.50(9) 2_675 ? 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 C12 Ru1 N6 76.3(2) . . ? C12 Ru1 C19 97.7(3) . . ? N6 Ru1 C19 114.5(2) . . ? C12 Ru1 C20 98.1(2) . . ? N6 Ru1 C20 151.2(2) . . ? C19 Ru1 C20 37.4(2) . . ? C12 Ru1 C18 121.9(3) . . ? N6 Ru1 C18 91.3(2) . . ? C19 Ru1 C18 37.4(2) . . ? C20 Ru1 C18 67.4(2) . . ? C12 Ru1 C22 158.5(2) . . ? N6 Ru1 C22 124.7(2) . . ? C19 Ru1 C22 78.4(3) . . ? C20 Ru1 C22 65.9(3) . . ? C18 Ru1 C22 66.9(3) . . ? C12 Ru1 C21 121.6(3) . . ? N6 Ru1 C21 162.0(2) . . ? C19 Ru1 C21 67.3(3) . . ? C20 Ru1 C21 36.8(2) . . ? C18 Ru1 C21 80.3(2) . . ? C22 Ru1 C21 37.3(2) . . ? C12 Ru1 C23 158.6(3) . . ? N6 Ru1 C23 97.1(2) . . ? C19 Ru1 C23 66.1(3) . . ? C20 Ru1 C23 77.8(3) . . ? C18 Ru1 C23 37.0(2) . . ? C22 Ru1 C23 36.4(2) . . ? C21 Ru1 C23 66.7(3) . . ? C12 Ru1 Cl2 85.77(18) . . ? N6 Ru1 Cl2 86.81(13) . . ? C19 Ru1 Cl2 158.62(18) . . ? C20 Ru1 Cl2 121.32(18) . . ? C18 Ru1 Cl2 150.96(19) . . ? C22 Ru1 Cl2 90.64(19) . . ? C21 Ru1 Cl2 92.83(19) . . ? C23 Ru1 Cl2 114.53(19) . . ? C6 Ru2 N1 76.1(2) . . ? C6 Ru2 C33 95.7(3) . . ? N1 Ru2 C33 129.5(3) . . ? C6 Ru2 C34 106.1(3) . . ? N1 Ru2 C34 166.4(3) . . ? C33 Ru2 C34 37.5(3) . . ? C6 Ru2 C31 146.0(3) . . ? N1 Ru2 C31 93.6(3) . . ? C33 Ru2 C31 65.8(3) . . ? C34 Ru2 C31 77.1(3) . . ? C6 Ru2 C32 111.6(3) . . ? N1 Ru2 C32 99.6(3) . . ? C33 Ru2 C32 36.9(3) . . ? C34 Ru2 C32 67.0(3) . . ? C31 Ru2 C32 37.3(3) . . ? C6 Ru2 C30 170.4(3) . . ? N1 Ru2 C30 113.4(3) . . ? C33 Ru2 C30 77.2(3) . . ? C34 Ru2 C30 64.3(3) . . ? C31 Ru2 C30 36.1(3) . . ? C32 Ru2 C30 66.4(3) . . ? C6 Ru2 C29 134.7(3) . . ? N1 Ru2 C29 147.8(3) . . ? C33 Ru2 C29 66.1(3) . . ? C34 Ru2 C29 35.4(3) . . ? C31 Ru2 C29 65.7(3) . . ? C32 Ru2 C29 79.1(3) . . ? C30 Ru2 C29 36.4(3) . . ? C6 Ru2 Cl1 85.93(19) . . ? N1 Ru2 Cl1 83.54(15) . . ? C33 Ru2 Cl1 146.4(2) . . ? C34 Ru2 Cl1 109.9(2) . . ? C31 Ru2 Cl1 125.6(2) . . ? C32 Ru2 Cl1 162.4(2) . . ? C30 Ru2 Cl1 96.4(2) . . ? C29 Ru2 Cl1 89.1(2) . . ? N1 C1 C2 121.7(7) . . ? C3 C2 C1 119.2(7) . . ? C2 C3 C4 120.6(7) . . ? C5 C4 C3 116.9(7) . . ? N1 C5 C4 124.0(6) . . ? N1 C5 N2 111.4(5) . . ? C4 C5 N2 124.5(6) . . ? N3 C6 N2 103.5(5) . . ? N3 C6 Ru2 141.0(5) . . ? N2 C6 Ru2 115.4(5) . . ? C8 C7 N2 105.5(6) . . ? C7 C8 N3 108.0(6) . . ? N4 C9 N3 111.9(5) . . ? C11 C10 N4 108.2(6) . . ? C10 C11 N5 105.3(6) . . ? N4 C12 N5 104.4(5) . . ? N4 C12 Ru1 140.1(4) . . ? N5 C12 Ru1 115.4(4) . . ? N6 C13 C14 123.4(6) . . ? N6 C13 N5 112.6(5) . . ? C14 C13 N5 123.9(6) . . ? C15 C14 C13 117.4(6) . . ? C14 C15 C16 120.1(6) . . ? C15 C16 C17 120.1(6) . . ? N6 C17 C16 120.6(6) . . ? C19 C18 C23 117.7(6) . . ? C19 C18 C25 123.1(6) . . ? C23 C18 C25 119.2(6) . . ? C19 C18 Ru1 70.4(4) . . ? C23 C18 Ru1 72.7(4) . . ? C25 C18 Ru1 129.7(5) . . ? C20 C19 C18 120.7(6) . . ? C20 C19 Ru1 71.7(4) . . ? C18 C19 Ru1 72.2(4) . . ? C21 C20 C19 122.0(6) . . ? C21 C20 Ru1 73.0(4) . . ? C19 C20 Ru1 71.0(4) . . ? C20 C21 C22 116.8(6) . . ? C20 C21 C24 122.5(7) . . ? C22 C21 C24 120.6(7) . . ? C20 C21 Ru1 70.2(4) . . ? C22 C21 Ru1 70.9(4) . . ? C24 C21 Ru1 128.0(5) . . ? C23 C22 C21 121.8(7) . . ? C23 C22 Ru1 72.7(4) . . ? C21 C22 Ru1 71.9(4) . . ? C22 C23 C18 120.8(7) . . ? C22 C23 Ru1 70.9(4) . . ? C18 C23 Ru1 70.3(4) . . ? C26 C25 C27 112.1(7) . . ? C26 C25 C18 115.4(6) . . ? C27 C25 C18 108.6(6) . . ? C34 C29 C30 118.5(8) . . ? C34 C29 C28 122.3(8) . . ? C30 C29 C28 119.2(8) . . ? C34 C29 Ru2 71.2(5) . . ? C30 C29 Ru2 71.3(4) . . ? C28 C29 Ru2 127.6(6) . . ? C31 C30 C29 121.5(8) . . ? C31 C30 Ru2 71.5(4) . . ? C29 C30 Ru2 72.4(5) . . ? C30 C31 C32 121.1(8) . . ? C30 C31 Ru2 72.3(5) . . ? C32 C31 Ru2 71.5(5) . . ? C33 C32 C31 116.0(8) . . ? C33 C32 C35 118.6(8) . . ? C31 C32 C35 125.4(8) . . ? C33 C32 Ru2 69.4(5) . . ? C31 C32 Ru2 71.2(5) . . ? C35 C32 Ru2 131.6(5) . . ? C32 C33 C34 122.0(8) . . ? C32 C33 Ru2 73.7(5) . . ? C34 C33 Ru2 73.1(5) . . ? C29 C34 C33 120.7(8) . . ? C29 C34 Ru2 73.4(5) . . ? C33 C34 Ru2 69.4(5) . . ? C37 C35 C32 119.1(9) . . ? C37 C35 C36 112.5(9) . . ? C32 C35 C36 107.5(7) . . ? N7 C38 C39 178.7(11) . . ? N8 C41 N8 76(5) 2_675 . ? N8 C41 C40 101(5) 2_675 . ? N8 C41 C40 175(5) . . ? N8 C41 C41 39(3) 2_675 2_675 ? N8 C41 C41 38(3) . 2_675 ? C40 C41 C41 139(6) . 2_675 ? C5 N1 C1 117.2(6) . . ? C5 N1 Ru2 118.7(4) . . ? C1 N1 Ru2 124.1(5) . . ? C6 N2 C7 111.8(5) . . ? C6 N2 C5 118.2(5) . . ? C7 N2 C5 129.7(5) . . ? C6 N3 C8 111.1(5) . . ? C6 N3 C9 124.5(5) . . ? C8 N3 C9 124.5(5) . . ? C12 N4 C10 110.9(5) . . ? C12 N4 C9 125.7(5) . . ? C10 N4 C9 123.5(5) . . ? C12 N5 C13 117.9(5) . . ? C12 N5 C11 111.3(5) . . ? C13 N5 C11 130.3(5) . . ? C13 N6 C17 118.3(5) . . ? C13 N6 Ru1 116.8(4) . . ? C17 N6 Ru1 124.7(4) . . ? C41 N8 C41 104(5) 2_675 . ? C41 N8 N8 52(3) 2_675 2_675 ? C41 N8 N8 51(3) . 2_675 ? F5 P1 F1 94.0(7) . . ? F5 P1 F3 92.3(7) . . ? F1 P1 F3 172.9(7) . . ? F5 P1 F4 90.2(4) . . ? F1 P1 F4 91.9(5) . . ? F3 P1 F4 91.3(5) . . ? F5 P1 F6 178.1(5) . . ? F1 P1 F6 87.4(6) . . ? F3 P1 F6 86.2(5) . . ? F4 P1 F6 91.0(4) . . ? F5 P1 F2 89.2(4) . . ? F1 P1 F2 89.0(4) . . ? F3 P1 F2 87.9(5) . . ? F4 P1 F2 179.0(4) . . ? F6 P1 F2 89.5(4) . . ? F11 P2 F8 95.3(5) . . ? F11 P2 F9 91.8(3) . . ? F8 P2 F9 89.7(3) . . ? F11 P2 F10 88.3(4) . . ? F8 P2 F10 176.3(5) . . ? F9 P2 F10 89.5(3) . . ? F11 P2 F7 88.4(4) . . ? F8 P2 F7 90.2(4) . . ? F9 P2 F7 179.7(4) . . ? F10 P2 F7 90.6(3) . . ? F11 P2 F12 177.0(4) . . ? F8 P2 F12 87.5(4) . . ? F9 P2 F12 89.3(3) . . ? F10 P2 F12 88.9(4) . . ? F7 P2 F12 90.5(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.893 _refine_diff_density_min -1.091 _refine_diff_density_rms 0.104 #===END data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 834945' #TrackingRef '- cif-Rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H44 F12 N6 P4 Ru' _chemical_formula_weight 1217.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.5296(7) _cell_length_b 21.6088(6) _cell_length_c 24.4791(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.963(4) _cell_angle_gamma 90.00 _cell_volume 10770.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4927 _exptl_absorpt_coefficient_mu 0.494 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8345 _exptl_absorpt_correction_T_max 0.8991 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21011 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9484 _reflns_number_gt 6719 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. The following restraints have been used to DFIX the P-F and the C-C bond distances. DFIX P4 F12 1.56 0.01 DFIX P4 F11 1.56 0.01 DFIX P4 F10 1.56 0.01 DFIX P4 F9 1.56 0.01 DFIX P4 F8 1.56 0.01 DFIX P4 F7 1.56 0.01 DFIX P4' F12' 1.56 0.01 DFIX P4' F11' 1.56 0.01 DFIX P4' F10' 1.56 0.01 DFIX P4' F9' 1.56 0.01 DFIX P4' F8' 1.56 0.01 DFIX P4' F7' 1.60 0.01 DFIX H46 H96 1.90 0.01 DFIX C24 C25 1.38 0.01 DFIX C26 C27 1.38 0.01 DFIX C27 C28 1.38 0.01 DFIX C42 C43 1.38 0.01 DFIX C44 C45 1.38 0.01 DFIX C45 C46 1.38 0.01 DFIX C48 C53 1.38 0.01 DFIX C51 C52 1.38 0.01 DFIX C50 C51 1.38 0.01 DFIX C30 C35 1.38 0.01 DFIX C32 C33 1.38 0.01 ; _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^)+(0.0432P)^2^+42.1674P] 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 9484 _refine_ls_number_parameters 748 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1562 _refine_ls_wR_factor_gt 0.1276 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.728727(19) 0.091726(18) 0.685713(18) 0.04357(15) Uani 1 1 d . . . C1 C 0.8404(3) 0.1709(3) 0.7891(2) 0.0587(14) Uani 1 1 d . . . H17 H 0.8286 0.1480 0.8164 0.070 Uiso 1 1 calc R . . C2 C 0.8891(3) 0.2142(3) 0.8083(3) 0.0731(18) Uani 1 1 d . . . H27 H 0.9098 0.2202 0.8477 0.088 Uiso 1 1 calc R . . C3 C 0.9066(3) 0.2483(3) 0.7693(3) 0.085(2) Uani 1 1 d . . . H8 H 0.9390 0.2785 0.7816 0.102 Uiso 1 1 calc R . . C4 C 0.8764(3) 0.2381(3) 0.7115(3) 0.0778(19) Uani 1 1 d . . . H20 H 0.8882 0.2608 0.6841 0.093 Uiso 1 1 calc R . . C5 C 0.8276(3) 0.1930(3) 0.6948(2) 0.0534(13) Uani 1 1 d . . . C6 C 0.7516(2) 0.1331(2) 0.6264(2) 0.0440(11) Uani 1 1 d . . . C7 C 0.8019(3) 0.2018(3) 0.5854(3) 0.0783(19) Uani 1 1 d . . . H28 H 0.8295 0.2334 0.5815 0.094 Uiso 1 1 calc R . . C8 C 0.7605(3) 0.1696(3) 0.5433(3) 0.0781(19) Uani 1 1 d . . . H39 H 0.7536 0.1743 0.5040 0.094 Uiso 1 1 calc R . . C9 C 0.6862(3) 0.0794(3) 0.5356(3) 0.0796(19) Uani 1 1 d . . . H14A H 0.6554 0.0977 0.5013 0.096 Uiso 1 1 calc R . . H14B H 0.7122 0.0492 0.5232 0.096 Uiso 1 1 calc R . . C10 C 0.6654(2) 0.0474(2) 0.6255(3) 0.0554(14) Uani 1 1 d . . . C11 C 0.5823(4) -0.0188(3) 0.5840(4) 0.100(3) Uani 1 1 d . . . H24 H 0.5498 -0.0484 0.5802 0.120 Uiso 1 1 calc R . . C12 C 0.5984(4) 0.0072(3) 0.5428(4) 0.099(3) Uani 1 1 d . . . H48 H 0.5788 -0.0002 0.5035 0.119 Uiso 1 1 calc R . . C13 C 0.6299(3) -0.0039(3) 0.6921(4) 0.0764(19) Uani 1 1 d . . . C14 C 0.5908(4) -0.0464(4) 0.7098(5) 0.111(3) Uani 1 1 d . . . H29 H 0.5577 -0.0680 0.6823 0.133 Uiso 1 1 calc R . . C15 C 0.6013(5) -0.0561(4) 0.7667(6) 0.126(4) Uani 1 1 d . . . H15 H 0.5758 -0.0845 0.7785 0.152 Uiso 1 1 calc R . . C16 C 0.6498(4) -0.0237(4) 0.8071(4) 0.105(3) Uani 1 1 d . . . H58 H 0.6579 -0.0300 0.8464 0.127 Uiso 1 1 calc R . . C17 C 0.6865(3) 0.0188(3) 0.7876(3) 0.0790(19) Uani 1 1 d . . . H57 H 0.7189 0.0412 0.8149 0.095 Uiso 1 1 calc R . . C18 C 0.8636(3) -0.0132(3) 0.7604(4) 0.085(2) Uani 1 1 d . . . C19 C 0.9105(5) -0.0574(5) 0.7621(5) 0.174(5) Uani 1 1 d . . . H59 H 0.9151 -0.0726 0.7281 0.209 Uiso 1 1 calc R . . C20 C 0.9506(7) -0.0785(7) 0.8153(7) 0.212(8) Uani 1 1 d . . . H61 H 0.9806 -0.1098 0.8163 0.254 Uiso 1 1 calc R . . C21 C 0.9478(6) -0.0562(6) 0.8642(6) 0.171(6) Uani 1 1 d . . . H65 H 0.9769 -0.0703 0.8991 0.205 Uiso 1 1 calc R . . C22 C 0.9018(4) -0.0121(4) 0.8638(4) 0.123(3) Uani 1 1 d . . . H36 H 0.8988 0.0034 0.8983 0.147 Uiso 1 1 calc R . . C23 C 0.8594(4) 0.0093(4) 0.8107(4) 0.094(2) Uani 1 1 d . . . H37 H 0.8281 0.0392 0.8100 0.113 Uiso 1 1 calc R . . C24 C 0.8698(3) 0.0376(3) 0.6563(4) 0.093(3) Uani 1 1 d D . . C25 C 0.8675(4) 0.0259(6) 0.6022(4) 0.160(5) Uani 1 1 d D . . H63 H 0.8360 -0.0013 0.5797 0.191 Uiso 1 1 calc R . . C26 C 0.9115(6) 0.0535(8) 0.5785(5) 0.212(7) Uani 1 1 d D . . H53 H 0.9093 0.0450 0.5407 0.254 Uiso 1 1 calc R . . C27 C 0.9574(6) 0.0927(6) 0.6114(7) 0.189(8) Uani 1 1 d D . . H45 H 0.9852 0.1136 0.5954 0.227 Uiso 1 1 calc R . . C28 C 0.9630(6) 0.1018(6) 0.6678(8) 0.228(9) Uani 1 1 d D . . H60 H 0.9972 0.1251 0.6920 0.273 Uiso 1 1 calc R . . C29 C 0.9176(5) 0.0761(4) 0.6874(7) 0.197(7) Uani 1 1 d . . . H26 H 0.9192 0.0854 0.7249 0.236 Uiso 1 1 calc R . . C30 C 0.7717(3) -0.0604(2) 0.6592(3) 0.0677(16) Uani 1 1 d D . . C31 C 0.7498(4) -0.0987(3) 0.6937(4) 0.109(3) Uani 1 1 d . . . H13 H 0.7597 -0.0888 0.7326 0.130 Uiso 1 1 calc R . . C32 C 0.7144(5) -0.1501(4) 0.6734(5) 0.135(4) Uani 1 1 d D . . H62 H 0.6999 -0.1744 0.6982 0.162 Uiso 1 1 calc R . . C33 C 0.6997(5) -0.1671(4) 0.6169(5) 0.128(4) Uani 1 1 d D . . H55 H 0.6761 -0.2031 0.6031 0.153 Uiso 1 1 calc R . . C34 C 0.7196(6) -0.1314(4) 0.5828(5) 0.160(5) Uani 1 1 d . . . H64 H 0.7094 -0.1421 0.5441 0.192 Uiso 1 1 calc R . . C35 C 0.7560(6) -0.0772(4) 0.6029(4) 0.148(4) Uani 1 1 d D . . H31 H 0.7694 -0.0527 0.5775 0.177 Uiso 1 1 calc R . . C36 C 0.6442(3) 0.2017(3) 0.7498(3) 0.0661(16) Uani 1 1 d . . . C37 C 0.6842(4) 0.1810(3) 0.8017(3) 0.0769(18) Uani 1 1 d . . . H33 H 0.7143 0.1498 0.8028 0.092 Uiso 1 1 calc R . . C38 C 0.6810(5) 0.2054(4) 0.8533(4) 0.113(3) Uani 1 1 d . . . H32 H 0.7091 0.1909 0.8885 0.136 Uiso 1 1 calc R . . C39 C 0.6365(6) 0.2507(5) 0.8520(5) 0.130(4) Uani 1 1 d . . . H30 H 0.6338 0.2672 0.8862 0.156 Uiso 1 1 calc R . . C40 C 0.5967(5) 0.2712(5) 0.8010(5) 0.136(4) Uani 1 1 d . . . H18 H 0.5662 0.3019 0.8004 0.163 Uiso 1 1 calc R . . C41 C 0.5994(4) 0.2479(4) 0.7491(4) 0.119(3) Uani 1 1 d . . . H43 H 0.5716 0.2632 0.7142 0.143 Uiso 1 1 calc R . . C42 C 0.5629(3) 0.1453(3) 0.6472(3) 0.0633(15) Uani 1 1 d D . . C43 C 0.5310(4) 0.1426(4) 0.5898(3) 0.134(4) Uani 1 1 d D . . H96 H 0.5532 0.1561 0.5652 0.161 Uiso 1 1 calc RD . . C44 C 0.4689(5) 0.1217(6) 0.5657(4) 0.158(4) Uani 1 1 d D . . H40 H 0.4487 0.1232 0.5259 0.189 Uiso 1 1 calc R . . C45 C 0.4363(4) 0.0988(5) 0.5999(5) 0.131(4) Uani 1 1 d D . . H51 H 0.3930 0.0855 0.5845 0.157 Uiso 1 1 calc R . . C46 C 0.4686(4) 0.0956(5) 0.6572(5) 0.141(4) Uani 1 1 d D . . H50 H 0.4486 0.0770 0.6814 0.169 Uiso 1 1 calc R . . C47 C 0.5298(4) 0.1193(4) 0.6798(4) 0.112(3) Uani 1 1 d . . . H25 H 0.5500 0.1176 0.7196 0.135 Uiso 1 1 calc R . . C48 C 0.6587(3) 0.2419(2) 0.6445(3) 0.0666(16) Uani 1 1 d D . . C49 C 0.6991(5) 0.2859(3) 0.6747(4) 0.123(3) Uani 1 1 d . . . H35 H 0.7189 0.2801 0.7142 0.148 Uiso 1 1 calc R . . C50 C 0.7128(6) 0.3392(4) 0.6501(6) 0.154(4) Uani 1 1 d D . . H44 H 0.7414 0.3685 0.6727 0.184 Uiso 1 1 calc R . . C51 C 0.6844(6) 0.3488(4) 0.5926(6) 0.147(5) Uani 1 1 d D . . H49 H 0.6926 0.3849 0.5755 0.177 Uiso 1 1 calc R . . C52 C 0.6443(7) 0.3053(6) 0.5610(5) 0.175(5) Uani 1 1 d D . . H38 H 0.6244 0.3105 0.5214 0.210 Uiso 1 1 calc R . . C53 C 0.6331(5) 0.2535(4) 0.5875(3) 0.148(4) Uani 1 1 d D . . H46 H 0.6056 0.2237 0.5646 0.178 Uiso 1 1 calc RD . . F1 F 0.9315(3) 0.3305(3) 0.5313(2) 0.165(2) Uani 1 1 d . . . F2 F 0.9673(2) 0.3460(2) 0.66493(16) 0.1085(14) Uani 1 1 d . . . F3 F 0.87412(18) 0.3384(2) 0.5903(2) 0.1170(16) Uani 1 1 d . . . F4 F 0.9458(2) 0.41040(18) 0.5892(2) 0.1205(17) Uani 1 1 d . . . F5 F 1.02541(19) 0.3384(2) 0.6059(2) 0.1127(15) Uani 1 1 d . . . F6 F 0.9526(2) 0.26559(17) 0.6069(2) 0.1087(14) Uani 1 1 d . . . F7 F 0.5789(13) 0.3379(13) -0.0457(6) 0.373(19) Uani 0.50 1 d PD A 1 F8 F 0.5693(15) 0.3979(14) 0.0232(10) 0.347(17) Uani 0.50 1 d PD A 1 F9 F 0.6655(16) 0.3936(15) -0.0062(11) 0.297(15) Uani 0.50 1 d PD A 1 F10 F 0.6634(15) 0.373(2) 0.0783(8) 0.39(3) Uani 0.50 1 d PD A 1 F11 F 0.6619(16) 0.2932(11) 0.0172(11) 0.348(15) Uani 0.50 1 d PD A 1 F12 F 0.5771(19) 0.3055(18) 0.038(2) 0.48(3) Uani 0.50 1 d PD A 1 F7' F 0.6336(9) 0.4566(16) 0.0208(11) 0.314(15) Uani 0.50 1 d PD B 2 F8' F 0.7184(10) 0.5024(6) 0.0874(8) 0.253(8) Uani 0.50 1 d PD B 2 F9' F 0.6995(10) 0.4066(8) 0.1053(5) 0.187(7) Uani 0.50 1 d PD B 2 F10' F 0.7219(16) 0.3774(8) 0.0314(9) 0.276(14) Uani 0.50 1 d PD B 2 F11' F 0.7817(8) 0.4345(10) 0.0833(9) 0.308(14) Uani 0.50 1 d PD B 2 F12' F 0.7363(13) 0.4815(11) 0.0147(7) 0.322(14) Uani 0.50 1 d PD B 2 N1 N 0.8089(2) 0.15970(18) 0.73328(17) 0.0468(10) Uani 1 1 d . . . N2 N 0.7958(2) 0.1791(2) 0.63692(17) 0.0529(11) Uani 1 1 d . . . N3 N 0.7294(2) 0.1275(2) 0.56831(19) 0.0570(11) Uani 1 1 d . . . N4 N 0.6500(2) 0.0481(2) 0.5672(2) 0.0670(13) Uani 1 1 d . . . N5 N 0.6230(2) 0.0063(2) 0.6348(3) 0.0717(14) Uani 1 1 d . . . N6 N 0.6777(2) 0.0291(2) 0.7321(2) 0.0614(12) Uani 1 1 d . . . P1 P 0.80930(7) 0.01291(6) 0.69037(7) 0.0574(4) Uani 1 1 d . . . P2 P 0.64783(7) 0.17062(6) 0.68150(6) 0.0496(3) Uani 1 1 d . . . P3 P 0.94974(8) 0.33771(7) 0.59778(7) 0.0666(5) Uani 1 1 d . . . P4 P 0.6207(5) 0.3515(5) 0.0180(3) 0.228(6) Uani 0.50 1 d PD A 1 P4' P 0.7073(7) 0.4414(6) 0.0521(4) 0.235(7) Uani 0.50 1 d PD 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 Ru1 0.0363(2) 0.0332(2) 0.0644(3) 0.00188(19) 0.02084(18) -0.00672(17) C1 0.065(4) 0.052(3) 0.061(4) 0.000(3) 0.024(3) 0.002(3) C2 0.070(4) 0.062(4) 0.076(4) -0.022(3) 0.007(3) -0.006(3) C3 0.072(5) 0.062(4) 0.109(6) -0.010(4) 0.013(4) -0.034(3) C4 0.072(4) 0.071(4) 0.088(5) 0.002(4) 0.023(4) -0.040(4) C5 0.049(3) 0.059(3) 0.054(3) 0.006(3) 0.020(3) -0.001(3) C6 0.035(3) 0.042(3) 0.057(3) -0.001(2) 0.019(2) 0.001(2) C7 0.078(5) 0.091(5) 0.070(4) 0.020(4) 0.029(3) -0.027(4) C8 0.075(4) 0.101(5) 0.065(4) 0.015(4) 0.031(3) -0.011(4) C9 0.077(5) 0.083(5) 0.069(4) -0.009(4) 0.010(3) -0.010(4) C10 0.036(3) 0.036(3) 0.093(4) -0.001(3) 0.019(3) -0.006(2) C11 0.063(5) 0.057(4) 0.156(8) -0.010(5) 0.004(5) -0.030(4) C12 0.069(5) 0.071(5) 0.126(7) -0.024(5) -0.010(4) -0.022(4) C13 0.046(4) 0.046(3) 0.132(6) 0.009(4) 0.021(4) -0.001(3) C14 0.077(5) 0.078(5) 0.186(9) 0.019(6) 0.056(6) -0.037(4) C15 0.097(7) 0.086(6) 0.226(12) 0.059(7) 0.094(8) -0.008(5) C16 0.100(6) 0.086(5) 0.157(8) 0.044(5) 0.078(6) 0.003(5) C17 0.071(4) 0.067(4) 0.114(6) 0.031(4) 0.051(4) 0.004(3) C18 0.056(4) 0.056(4) 0.127(6) 0.000(4) 0.007(4) 0.010(3) C19 0.129(9) 0.156(9) 0.184(10) -0.035(8) -0.024(7) 0.095(8) C20 0.146(11) 0.166(12) 0.239(16) -0.026(12) -0.053(12) 0.100(10) C21 0.117(9) 0.131(10) 0.188(13) 0.027(9) -0.054(9) 0.026(8) C22 0.097(7) 0.112(7) 0.129(7) 0.032(6) -0.005(6) 0.002(6) C23 0.065(5) 0.078(5) 0.127(7) 0.027(5) 0.015(5) -0.002(4) C24 0.059(4) 0.048(4) 0.193(8) 0.006(5) 0.071(5) 0.002(3) C25 0.083(6) 0.267(15) 0.138(8) 0.047(9) 0.049(6) -0.043(8) C26 0.103(9) 0.34(2) 0.218(13) 0.110(14) 0.088(9) -0.022(11) C27 0.109(9) 0.144(11) 0.36(2) 0.123(14) 0.140(13) 0.021(8) C28 0.157(12) 0.124(10) 0.49(3) -0.070(14) 0.220(17) -0.066(8) C29 0.146(9) 0.117(7) 0.42(2) -0.111(10) 0.212(12) -0.082(7) C30 0.058(4) 0.038(3) 0.115(5) -0.002(3) 0.038(4) 0.003(3) C31 0.140(7) 0.060(4) 0.155(7) -0.015(5) 0.088(6) -0.046(5) C32 0.157(9) 0.069(6) 0.212(12) -0.015(7) 0.102(9) -0.050(6) C33 0.121(8) 0.057(5) 0.195(11) -0.011(7) 0.037(8) -0.028(5) C34 0.240(14) 0.082(7) 0.153(9) -0.040(6) 0.057(9) -0.056(8) C35 0.253(13) 0.081(6) 0.131(8) -0.030(6) 0.091(8) -0.073(7) C36 0.060(4) 0.054(4) 0.095(5) -0.009(3) 0.040(3) -0.003(3) C37 0.086(5) 0.067(4) 0.095(5) -0.005(4) 0.054(4) -0.004(4) C38 0.136(8) 0.110(7) 0.117(7) -0.021(5) 0.074(6) -0.008(6) C39 0.151(10) 0.131(9) 0.133(8) -0.051(7) 0.082(8) -0.008(7) C40 0.133(9) 0.117(8) 0.180(10) -0.041(8) 0.082(8) 0.037(7) C41 0.115(7) 0.115(7) 0.135(7) -0.029(6) 0.050(6) 0.045(6) C42 0.042(3) 0.054(3) 0.097(5) 0.004(3) 0.026(3) 0.004(3) C43 0.084(6) 0.197(10) 0.107(7) 0.014(6) 0.012(5) -0.062(7) C44 0.098(8) 0.211(12) 0.129(8) -0.002(8) -0.011(6) -0.053(8) C45 0.055(5) 0.141(9) 0.196(11) -0.054(8) 0.038(7) -0.027(5) C46 0.073(6) 0.174(10) 0.191(11) -0.028(9) 0.064(7) -0.056(7) C47 0.071(5) 0.147(8) 0.127(6) 0.015(6) 0.043(5) -0.040(5) C48 0.069(4) 0.038(3) 0.109(5) 0.009(3) 0.050(4) 0.006(3) C49 0.132(8) 0.065(5) 0.166(8) 0.018(5) 0.040(6) -0.037(5) C50 0.204(12) 0.060(6) 0.222(13) -0.004(7) 0.105(11) -0.048(6) C51 0.234(14) 0.065(6) 0.208(13) 0.011(8) 0.162(12) -0.016(7) C52 0.256(16) 0.144(10) 0.138(9) 0.059(8) 0.081(10) -0.032(10) C53 0.226(12) 0.121(8) 0.097(6) 0.025(6) 0.050(7) -0.072(8) F1 0.195(6) 0.211(6) 0.078(3) 0.004(3) 0.028(3) 0.013(5) F2 0.111(3) 0.124(4) 0.079(3) -0.004(2) 0.015(2) 0.025(3) F3 0.053(2) 0.108(3) 0.177(4) 0.049(3) 0.018(2) -0.022(2) F4 0.078(3) 0.070(3) 0.191(5) 0.047(3) 0.012(3) -0.020(2) F5 0.068(3) 0.106(3) 0.175(4) 0.027(3) 0.054(3) -0.009(2) F6 0.099(3) 0.062(2) 0.159(4) 0.012(2) 0.034(3) -0.016(2) F7 0.46(4) 0.49(4) 0.138(15) 0.006(18) 0.053(18) 0.30(3) F8 0.53(5) 0.32(3) 0.28(3) 0.06(2) 0.25(3) 0.22(3) F9 0.30(3) 0.45(5) 0.19(2) 0.09(3) 0.15(2) -0.02(3) F10 0.34(4) 0.71(8) 0.101(17) 0.03(3) 0.05(2) 0.16(5) F11 0.39(4) 0.33(3) 0.33(3) 0.14(3) 0.12(3) 0.22(3) F12 0.52(6) 0.51(6) 0.50(6) 0.24(5) 0.29(5) 0.03(5) F7' 0.26(3) 0.47(4) 0.18(2) 0.16(3) 0.049(19) 0.10(3) F8' 0.24(2) 0.193(16) 0.31(2) 0.072(16) 0.060(18) 0.050(14) F9' 0.26(2) 0.239(17) 0.073(9) 0.044(10) 0.073(11) 0.043(13) F10' 0.41(4) 0.29(3) 0.112(13) -0.042(15) 0.076(18) 0.02(3) F11' 0.35(3) 0.211(19) 0.49(4) -0.07(2) 0.32(3) 0.00(2) F12' 0.44(3) 0.41(3) 0.121(12) 0.023(15) 0.098(16) -0.16(3) N1 0.046(2) 0.044(2) 0.053(3) 0.002(2) 0.020(2) -0.0035(19) N2 0.052(3) 0.059(3) 0.049(3) 0.005(2) 0.019(2) -0.019(2) N3 0.050(3) 0.058(3) 0.062(3) -0.001(2) 0.017(2) -0.004(2) N4 0.051(3) 0.054(3) 0.085(4) -0.017(3) 0.006(3) -0.010(2) N5 0.057(3) 0.047(3) 0.105(4) 0.000(3) 0.018(3) -0.016(2) N6 0.048(3) 0.050(3) 0.093(4) 0.014(3) 0.033(3) -0.001(2) P1 0.0417(8) 0.0379(7) 0.0966(11) 0.0021(7) 0.0278(7) -0.0058(6) P2 0.0441(8) 0.0362(7) 0.0760(9) 0.0015(7) 0.0299(7) -0.0039(6) P3 0.0544(9) 0.0612(10) 0.0780(11) 0.0175(8) 0.0127(8) -0.0204(8) P4 0.306(13) 0.292(12) 0.127(7) 0.097(7) 0.125(8) 0.163(11) P4' 0.353(18) 0.282(14) 0.092(5) 0.020(7) 0.102(8) 0.133(14) _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 C6 1.901(5) . ? Ru1 C10 1.909(6) . ? Ru1 N6 2.266(4) . ? Ru1 N1 2.278(4) . ? Ru1 P1 2.4071(15) . ? Ru1 P2 2.4153(14) . ? C1 N1 1.335(6) . ? C1 C2 1.370(8) . ? C1 H17 0.9300 . ? C2 C3 1.353(9) . ? C2 H27 0.9300 . ? C3 C4 1.368(9) . ? C3 H8 0.9300 . ? C4 C5 1.395(7) . ? C4 H20 0.9300 . ? C5 N1 1.345(6) . ? C5 N2 1.392(6) . ? C6 N2 1.342(6) . ? C6 N3 1.351(6) . ? C7 C8 1.320(8) . ? C7 N2 1.399(7) . ? C7 H28 0.9300 . ? C8 N3 1.386(7) . ? C8 H39 0.9300 . ? C9 N4 1.432(8) . ? C9 N3 1.450(7) . ? C9 H14A 0.9700 . ? C9 H14B 0.9700 . ? C10 N5 1.344(7) . ? C10 N4 1.357(7) . ? C11 C12 1.298(10) . ? C11 N5 1.378(9) . ? C11 H24 0.9300 . ? C12 N4 1.394(8) . ? C12 H48 0.9300 . ? C13 N6 1.368(8) . ? C13 N5 1.380(8) . ? C13 C14 1.407(9) . ? C14 C15 1.354(12) . ? C14 H29 0.9300 . ? C15 C16 1.372(12) . ? C15 H15 0.9300 . ? C16 C17 1.394(9) . ? C16 H58 0.9300 . ? C17 N6 1.330(8) . ? C17 H57 0.9300 . ? C18 C23 1.355(10) . ? C18 C19 1.380(10) . ? C18 P1 1.823(8) . ? C19 C20 1.385(15) . ? C19 H59 0.9300 . ? C20 C21 1.311(17) . ? C20 H61 0.9300 . ? C21 C22 1.372(15) . ? C21 H65 0.9300 . ? C22 C23 1.403(10) . ? C22 H36 0.9300 . ? C23 H37 0.9300 . ? C24 C25 1.336(8) . ? C24 C29 1.349(12) . ? C24 P1 1.838(7) . ? C25 C26 1.395(12) . ? C25 H63 0.9300 . ? C26 C27 1.352(9) . ? C26 H53 0.9300 . ? C27 C28 1.361(9) . ? C27 H45 0.9300 . ? C28 C29 1.341(13) . ? C28 H60 0.9300 . ? C29 H26 0.9300 . ? C30 C35 1.358(7) . ? C30 C31 1.371(9) . ? C30 P1 1.829(6) . ? C31 C32 1.348(10) . ? C31 H13 0.9300 . ? C32 C33 1.363(8) . ? C32 H62 0.9300 . ? C33 C34 1.308(12) . ? C33 H55 0.9300 . ? C34 C35 1.406(11) . ? C34 H64 0.9300 . ? C35 H31 0.9300 . ? C36 C37 1.358(9) . ? C36 C41 1.385(9) . ? C36 P2 1.826(6) . ? C37 C38 1.391(9) . ? C37 H33 0.9300 . ? C38 C39 1.362(12) . ? C38 H32 0.9300 . ? C39 C40 1.340(13) . ? C39 H30 0.9300 . ? C40 C41 1.385(12) . ? C40 H18 0.9300 . ? C41 H43 0.9300 . ? C42 C43 1.350(7) . ? C42 C47 1.353(8) . ? C42 P2 1.830(6) . ? C43 C44 1.352(11) . ? C43 H96 0.9300 . ? C44 C45 1.348(8) . ? C44 H40 0.9300 . ? C45 C46 1.351(8) . ? C45 H51 0.9300 . ? C46 C47 1.351(10) . ? C46 H50 0.9300 . ? C47 H25 0.9300 . ? C48 C53 1.348(7) . ? C48 C49 1.337(10) . ? C48 P2 1.840(6) . ? C49 C50 1.377(11) . ? C49 H35 0.9300 . ? C50 C51 1.354(8) . ? C50 H44 0.9300 . ? C51 C52 1.341(8) . ? C51 H49 0.9300 . ? C52 C53 1.353(11) . ? C52 H38 0.9300 . ? C53 H46 0.9300 . ? F1 P3 1.552(5) . ? F2 P3 1.573(4) . ? F3 P3 1.578(4) . ? F4 P3 1.583(4) . ? F5 P3 1.576(4) . ? F6 P3 1.573(4) . ? F7 P4 1.554(10) . ? F8 P4 1.529(9) . ? F9 P4 1.575(10) . ? F10 P4 1.534(10) . ? F11 P4 1.545(10) . ? F12 P4 1.549(10) . ? F7' P4' 1.556(10) . ? F8' P4' 1.552(10) . ? F9' P4' 1.561(9) . ? F10' P4' 1.540(10) . ? F11' P4' 1.543(10) . ? F12' P4' 1.532(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Ru1 C10 86.8(2) . . ? C6 Ru1 N6 162.0(2) . . ? C10 Ru1 N6 75.3(2) . . ? C6 Ru1 N1 75.24(18) . . ? C10 Ru1 N1 162.0(2) . . ? N6 Ru1 N1 122.64(17) . . ? C6 Ru1 P1 90.44(14) . . ? C10 Ru1 P1 90.28(16) . . ? N6 Ru1 P1 90.72(12) . . ? N1 Ru1 P1 90.98(11) . . ? C6 Ru1 P2 89.84(14) . . ? C10 Ru1 P2 89.81(16) . . ? N6 Ru1 P2 89.03(12) . . ? N1 Ru1 P2 89.03(11) . . ? P1 Ru1 P2 179.71(5) . . ? N1 C1 C2 123.5(5) . . ? N1 C1 H17 118.3 . . ? C2 C1 H17 118.3 . . ? C3 C2 C1 119.2(6) . . ? C3 C2 H27 120.4 . . ? C1 C2 H27 120.4 . . ? C2 C3 C4 119.6(6) . . ? C2 C3 H8 120.2 . . ? C4 C3 H8 120.2 . . ? C3 C4 C5 118.4(6) . . ? C3 C4 H20 120.8 . . ? C5 C4 H20 120.8 . . ? N1 C5 N2 116.0(5) . . ? N1 C5 C4 122.5(5) . . ? N2 C5 C4 121.5(5) . . ? N2 C6 N3 104.8(4) . . ? N2 C6 Ru1 123.1(4) . . ? N3 C6 Ru1 132.1(4) . . ? C8 C7 N2 106.4(5) . . ? C8 C7 H28 126.8 . . ? N2 C7 H28 126.8 . . ? C7 C8 N3 107.5(5) . . ? C7 C8 H39 126.2 . . ? N3 C8 H39 126.2 . . ? N4 C9 N3 113.9(5) . . ? N4 C9 H14A 108.8 . . ? N3 C9 H14A 108.8 . . ? N4 C9 H14B 108.8 . . ? N3 C9 H14B 108.8 . . ? H14A C9 H14B 107.7 . . ? N5 C10 N4 103.8(5) . . ? N5 C10 Ru1 123.7(5) . . ? N4 C10 Ru1 132.5(4) . . ? C12 C11 N5 106.2(6) . . ? C12 C11 H24 126.9 . . ? N5 C11 H24 126.9 . . ? C11 C12 N4 108.6(7) . . ? C11 C12 H48 125.7 . . ? N4 C12 H48 125.7 . . ? N6 C13 N5 116.8(5) . . ? N6 C13 C14 120.5(8) . . ? N5 C13 C14 122.7(7) . . ? C15 C14 C13 120.0(8) . . ? C15 C14 H29 120.0 . . ? C13 C14 H29 120.0 . . ? C14 C15 C16 119.8(7) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C17 118.2(8) . . ? C15 C16 H58 120.9 . . ? C17 C16 H58 120.9 . . ? N6 C17 C16 123.5(8) . . ? N6 C17 H57 118.2 . . ? C16 C17 H57 118.2 . . ? C23 C18 C19 119.1(8) . . ? C23 C18 P1 122.1(5) . . ? C19 C18 P1 118.8(8) . . ? C18 C19 C20 118.8(11) . . ? C18 C19 H59 120.6 . . ? C20 C19 H59 120.6 . . ? C21 C20 C19 122.6(12) . . ? C21 C20 H61 118.7 . . ? C19 C20 H61 118.7 . . ? C20 C21 C22 119.7(11) . . ? C20 C21 H65 120.1 . . ? C22 C21 H65 120.1 . . ? C21 C22 C23 119.2(11) . . ? C21 C22 H36 120.4 . . ? C23 C22 H36 120.4 . . ? C18 C23 C22 120.5(8) . . ? C18 C23 H37 119.7 . . ? C22 C23 H37 119.7 . . ? C25 C24 C29 116.8(8) . . ? C25 C24 P1 126.3(6) . . ? C29 C24 P1 116.5(7) . . ? C24 C25 C26 121.4(11) . . ? C24 C25 H63 119.3 . . ? C26 C25 H63 119.3 . . ? C27 C26 C25 119.0(11) . . ? C27 C26 H53 120.5 . . ? C25 C26 H53 120.5 . . ? C26 C27 C28 120.1(11) . . ? C26 C27 H45 120.0 . . ? C28 C27 H45 120.0 . . ? C27 C28 C29 118.0(12) . . ? C27 C28 H60 121.0 . . ? C29 C28 H60 121.0 . . ? C28 C29 C24 124.4(12) . . ? C28 C29 H26 117.8 . . ? C24 C29 H26 117.8 . . ? C35 C30 C31 116.3(7) . . ? C35 C30 P1 125.8(5) . . ? C31 C30 P1 117.4(5) . . ? C32 C31 C30 122.4(8) . . ? C32 C31 H13 118.8 . . ? C30 C31 H13 118.8 . . ? C33 C32 C31 121.0(9) . . ? C33 C32 H62 119.5 . . ? C31 C32 H62 119.5 . . ? C34 C33 C32 118.1(9) . . ? C34 C33 H55 120.9 . . ? C32 C33 H55 120.9 . . ? C33 C34 C35 122.0(10) . . ? C33 C34 H64 119.0 . . ? C35 C34 H64 119.0 . . ? C30 C35 C34 120.3(8) . . ? C30 C35 H31 119.9 . . ? C34 C35 H31 119.9 . . ? C37 C36 C41 118.4(7) . . ? C37 C36 P2 122.3(5) . . ? C41 C36 P2 119.3(6) . . ? C36 C37 C38 121.5(7) . . ? C36 C37 H33 119.2 . . ? C38 C37 H33 119.2 . . ? C39 C38 C37 119.4(9) . . ? C39 C38 H32 120.3 . . ? C37 C38 H32 120.3 . . ? C40 C39 C38 119.6(9) . . ? C40 C39 H30 120.2 . . ? C38 C39 H30 120.2 . . ? C39 C40 C41 121.9(9) . . ? C39 C40 H18 119.0 . . ? C41 C40 H18 119.0 . . ? C36 C41 C40 119.1(9) . . ? C36 C41 H43 120.4 . . ? C40 C41 H43 120.4 . . ? C43 C42 C47 114.1(6) . . ? C43 C42 P2 125.8(5) . . ? C47 C42 P2 119.6(5) . . ? C42 C43 C44 124.4(8) . . ? C42 C43 H96 117.8 . . ? C44 C43 H96 117.8 . . ? C45 C44 C43 119.5(9) . . ? C45 C44 H40 120.3 . . ? C43 C44 H40 120.3 . . ? C44 C45 C46 117.8(9) . . ? C44 C45 H51 121.1 . . ? C46 C45 H51 121.1 . . ? C45 C46 C47 120.7(9) . . ? C45 C46 H50 119.7 . . ? C47 C46 H50 119.7 . . ? C42 C47 C46 123.1(9) . . ? C42 C47 H25 118.4 . . ? C46 C47 H25 118.4 . . ? C53 C48 C49 114.5(7) . . ? C53 C48 P2 126.2(5) . . ? C49 C48 P2 119.1(6) . . ? C48 C49 C50 123.1(9) . . ? C48 C49 H35 118.4 . . ? C50 C49 H35 118.4 . . ? C51 C50 C49 119.6(10) . . ? C51 C50 H44 120.2 . . ? C49 C50 H44 120.2 . . ? C52 C51 C50 118.9(10) . . ? C52 C51 H49 120.6 . . ? C50 C51 H49 120.6 . . ? C51 C52 C53 118.9(10) . . ? C51 C52 H38 120.5 . . ? C53 C52 H38 120.5 . . ? C48 C53 C52 125.1(8) . . ? C48 C53 H46 117.5 . . ? C52 C53 H46 117.5 . . ? C1 N1 C5 116.9(5) . . ? C1 N1 Ru1 133.5(3) . . ? C5 N1 Ru1 109.6(3) . . ? C6 N2 C5 115.9(4) . . ? C6 N2 C7 110.8(4) . . ? C5 N2 C7 133.3(5) . . ? C6 N3 C8 110.5(5) . . ? C6 N3 C9 126.1(5) . . ? C8 N3 C9 122.9(5) . . ? C10 N4 C12 109.3(6) . . ? C10 N4 C9 125.7(5) . . ? C12 N4 C9 124.5(6) . . ? C10 N5 C11 112.1(6) . . ? C10 N5 C13 115.0(5) . . ? C11 N5 C13 132.9(6) . . ? C17 N6 C13 117.9(6) . . ? C17 N6 Ru1 132.9(4) . . ? C13 N6 Ru1 109.1(4) . . ? C18 P1 C30 100.7(3) . . ? C18 P1 C24 100.6(4) . . ? C30 P1 C24 110.2(3) . . ? C18 P1 Ru1 119.7(3) . . ? C30 P1 Ru1 112.26(19) . . ? C24 P1 Ru1 112.3(2) . . ? C36 P2 C42 101.3(3) . . ? C36 P2 C48 101.1(3) . . ? C42 P2 C48 107.0(3) . . ? C36 P2 Ru1 117.7(2) . . ? C42 P2 Ru1 114.03(19) . . ? C48 P2 Ru1 114.04(18) . . ? F1 P3 F6 92.0(3) . . ? F1 P3 F2 178.9(3) . . ? F6 P3 F2 88.8(3) . . ? F1 P3 F5 91.9(3) . . ? F6 P3 F5 90.1(2) . . ? F2 P3 F5 88.8(3) . . ? F1 P3 F3 88.8(3) . . ? F6 P3 F3 90.9(2) . . ? F2 P3 F3 90.5(3) . . ? F5 P3 F3 178.8(3) . . ? F1 P3 F4 88.6(3) . . ? F6 P3 F4 178.8(3) . . ? F2 P3 F4 90.5(3) . . ? F5 P3 F4 90.9(2) . . ? F3 P3 F4 88.1(2) . . ? F8 P4 F10 86.9(18) . . ? F8 P4 F11 166(2) . . ? F10 P4 F11 95.2(19) . . ? F8 P4 F12 82(2) . . ? F10 P4 F12 97.4(19) . . ? F11 P4 F12 83.6(19) . . ? F8 P4 F7 90.5(13) . . ? F10 P4 F7 173(2) . . ? F11 P4 F7 88.9(13) . . ? F12 P4 F7 89(2) . . ? F8 P4 F9 101.6(18) . . ? F10 P4 F9 86.6(16) . . ? F11 P4 F9 92.4(19) . . ? F12 P4 F9 175(2) . . ? F7 P4 F9 87.6(15) . . ? F12' P4' F10' 98.4(15) . . ? F12' P4' F11' 78.0(14) . . ? F10' P4' F11' 77.6(14) . . ? F12' P4' F8' 80.4(13) . . ? F10' P4' F8' 159.2(17) . . ? F11' P4' F8' 81.9(12) . . ? F12' P4' F7' 97.7(15) . . ? F10' P4' F7' 108.2(19) . . ? F11' P4' F7' 173.4(17) . . ? F8' P4' F7' 92.5(17) . . ? F12' P4' F9' 161.2(14) . . ? F10' P4' F9' 86.0(12) . . ? F11' P4' F9' 85.2(12) . . ? F8' P4' F9' 89.0(10) . . ? F7' P4' F9' 98.2(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.590 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.074 #===END data_complex_5a _database_code_depnum_ccdc_archive 'CCDC 834946' #TrackingRef '- cif-Rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H53 F24 N19 P4 Ru2' _chemical_formula_weight 1870.27 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.4226(18) _cell_length_b 11.4357(3) _cell_length_c 24.2032(13) _cell_angle_alpha 90.00 _cell_angle_beta 127.318(8) _cell_angle_gamma 90.00 _cell_volume 7356.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3736 _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8230 _exptl_absorpt_correction_T_max 0.8716 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16439 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6476 _reflns_number_gt 5289 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0416P)^2^+9.6453P] 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 6476 _refine_ls_number_parameters 513 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.017 _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 0.156416(8) 0.48319(2) 1.029799(11) 0.03138(9) Uani 1 1 d . . . C1 C 0.04934(11) 0.3828(3) 0.92700(15) 0.0431(8) Uani 1 1 d . . . H18 H 0.0421 0.4495 0.9004 0.052 Uiso 1 1 calc R . . C2 C 0.01391(13) 0.2965(3) 0.90078(18) 0.0548(9) Uani 1 1 d . . . H19 H -0.0172 0.3058 0.8577 0.066 Uiso 1 1 calc R . . C3 C 0.02457(15) 0.1962(3) 0.93834(19) 0.0634(11) Uani 1 1 d . . . H20 H 0.0008 0.1366 0.9208 0.076 Uiso 1 1 calc R . . C4 C 0.07043(14) 0.1842(3) 1.00200(19) 0.0558(9) Uani 1 1 d . . . H21 H 0.0787 0.1162 1.0279 0.067 Uiso 1 1 calc R . . C5 C 0.10376(11) 0.2754(3) 1.02630(15) 0.0388(7) Uani 1 1 d . . . C6 C 0.18038(11) 0.3707(3) 1.10399(15) 0.0358(7) Uani 1 1 d . . . C7 C 0.20201(13) 0.2971(3) 1.20519(17) 0.0514(9) Uani 1 1 d . . . H3 H 0.2181 0.2888 1.2526 0.062 Uiso 1 1 calc R . . C8 C 0.16370(14) 0.2329(3) 1.15470(17) 0.0491(8) Uani 1 1 d . . . H4 H 0.1487 0.1700 1.1601 0.059 Uiso 1 1 calc R . . C9 C 0.23542(11) 0.4944(3) 1.20057(16) 0.0436(8) Uani 1 1 d . . . H40A H 0.2575 0.5142 1.1885 0.052 Uiso 1 1 calc R . . H40B H 0.2550 0.4955 1.2508 0.052 Uiso 1 1 calc R . . C10 C 0.15512(10) 0.5818(2) 1.09982(14) 0.0339(7) Uani 1 1 d . . . C11 C 0.18682(13) 0.6547(3) 1.20682(16) 0.0465(8) Uani 1 1 d . . . H9 H 0.2082 0.6662 1.2547 0.056 Uiso 1 1 calc R . . C12 C 0.14338(13) 0.7089(3) 1.16143(17) 0.0481(8) Uani 1 1 d . . . H8 H 0.1288 0.7664 1.1711 0.058 Uiso 1 1 calc R . . C13 C 0.07472(11) 0.6930(3) 1.03602(16) 0.0406(7) Uani 1 1 d . . . C14 C 0.06264(14) 0.8088(3) 1.01838(19) 0.0544(9) Uani 1 1 d . . . H11 H 0.0855 0.8678 1.0457 0.065 Uiso 1 1 calc R . . C15 C 0.01587(16) 0.8338(4) 0.9593(2) 0.0712(12) Uani 1 1 d . . . H16 H 0.0063 0.9108 0.9449 0.085 Uiso 1 1 calc R . . C16 C -0.01704(16) 0.7436(4) 0.9213(2) 0.0711(12) Uani 1 1 d . . . H15 H -0.0491 0.7587 0.8807 0.085 Uiso 1 1 calc R . . C17 C -0.00192(14) 0.6322(4) 0.9440(2) 0.0671(11) Uani 1 1 d . . . H14 H -0.0246 0.5719 0.9183 0.080 Uiso 1 1 calc R . . C18 C 0.10325(13) 0.7039(3) 0.92911(19) 0.0514(9) Uani 1 1 d . . . H38 H 0.1061 0.7403 0.9658 0.062 Uiso 1 1 calc R . . C19 C 0.07997(15) 0.7652(3) 0.8667(2) 0.0643(11) Uani 1 1 d . . . H34 H 0.0668 0.8394 0.8619 0.077 Uiso 1 1 calc R . . C20 C 0.07673(15) 0.7152(4) 0.8133(2) 0.0652(11) Uani 1 1 d . . . H33 H 0.0608 0.7544 0.7712 0.078 Uiso 1 1 calc R . . C21 C 0.09746(13) 0.6049(3) 0.82201(17) 0.0535(9) Uani 1 1 d . . . C22 C 0.09853(17) 0.5487(5) 0.7706(2) 0.0746(13) Uani 1 1 d . . . H23 H 0.0842 0.5855 0.7282 0.090 Uiso 1 1 calc R . . C23 C 0.11946(11) 0.5487(3) 0.88585(15) 0.0406(7) Uani 1 1 d . . . C24 C 0.11982(17) 0.4438(5) 0.7822(2) 0.0763(13) Uani 1 1 d . . . H24 H 0.1200 0.4096 0.7475 0.092 Uiso 1 1 calc R . . C25 C 0.14236(13) 0.3822(3) 0.84624(18) 0.0543(9) Uani 1 1 d . . . C26 C 0.14197(11) 0.4361(3) 0.89778(15) 0.0418(8) Uani 1 1 d . . . C27 C 0.16478(15) 0.2722(4) 0.8612(2) 0.0683(12) Uani 1 1 d . . . H26 H 0.1659 0.2337 0.8283 0.082 Uiso 1 1 calc R . . C28 C 0.18474(15) 0.2219(3) 0.9232(2) 0.0637(11) Uani 1 1 d . . . H27 H 0.1994 0.1482 0.9331 0.076 Uiso 1 1 calc R . . C29 C 0.18325(13) 0.2812(3) 0.97256(19) 0.0527(9) Uani 1 1 d . . . H28 H 0.1971 0.2456 1.0152 0.063 Uiso 1 1 calc R . . C30 C 0.25439(12) 0.6184(3) 1.07555(15) 0.0411(7) Uani 1 1 d . . . C31 C 0.29779(13) 0.6833(3) 1.09163(19) 0.0599(10) Uani 1 1 d . . . H37A H 0.2890 0.7643 1.0802 0.090 Uiso 1 1 calc R . . H37B H 0.3080 0.6524 1.0650 0.090 Uiso 1 1 calc R . . H37C H 0.3250 0.6761 1.1403 0.090 Uiso 1 1 calc R . . C32 C 1.0000 0.2939(11) 0.7500 0.107(3) Uani 1 2 d S . . C33 C 1.0000 0.1697(11) 0.7500 0.215(7) Uani 1 2 d S . . H42A H 0.9991 0.1417 0.7866 0.323 Uiso 0.50 1 calc PR . . H42B H 1.0299 0.1417 0.7572 0.323 Uiso 0.50 1 calc PR . . H42C H 0.9710 0.1417 0.7061 0.323 Uiso 0.50 1 calc PR . . F1 F 0.41162(10) 0.50240(19) 0.35126(11) 0.0723(7) Uani 1 1 d . . . F2 F 0.34387(8) 0.4560(2) 0.24354(14) 0.0920(8) Uani 1 1 d . . . F3 F 0.38151(11) 0.63102(19) 0.26493(12) 0.0866(8) Uani 1 1 d . . . F4 F 0.45466(9) 0.5384(2) 0.30967(14) 0.0866(8) Uani 1 1 d . . . F5 F 0.38659(11) 0.49502(19) 0.20224(12) 0.0839(8) Uani 1 1 d . . . F6 F 0.41630(8) 0.36595(17) 0.28851(11) 0.0636(6) Uani 1 1 d . . . F7 F 0.23063(13) 1.0951(3) 0.11555(17) 0.1196(11) Uani 1 1 d . . . F8 F 0.16329(13) 1.0198(3) 0.02053(17) 0.1471(15) Uani 1 1 d . . . F9 F 0.18573(14) 0.9617(3) 0.12158(18) 0.1318(12) Uani 1 1 d . . . F10 F 0.26205(12) 0.9211(4) 0.15217(16) 0.1393(13) Uani 1 1 d . . . F11 F 0.23939(14) 0.9793(3) 0.05101(18) 0.1316(13) Uani 1 1 d . . . F12 F 0.19432(15) 0.8443(3) 0.0549(2) 0.1560(15) Uani 1 1 d . . . N1 N 0.09443(9) 0.3747(2) 0.99013(12) 0.0349(6) Uani 1 1 d . . . N2 N 0.15053(9) 0.2785(2) 1.09207(12) 0.0382(6) Uani 1 1 d . . . N3 N 0.21371(9) 0.3794(2) 1.17395(12) 0.0411(6) Uani 1 1 d . . . N4 N 0.19425(9) 0.5781(2) 1.16960(12) 0.0381(6) Uani 1 1 d . . . N5 N 0.12407(9) 0.6627(2) 1.09666(12) 0.0371(6) Uani 1 1 d . . . N6 N 0.04409(10) 0.6044(2) 1.00172(14) 0.0521(7) Uani 1 1 d . . . N7 N 0.12138(9) 0.5970(2) 0.93867(12) 0.0373(6) Uani 1 1 d . . . N8 N 0.16287(9) 0.3860(2) 0.96079(13) 0.0385(6) Uani 1 1 d . . . N9 N 0.22093(10) 0.5679(2) 1.06336(12) 0.0377(6) Uani 1 1 d . . . N10 N 1.0000 0.3889(8) 0.7500 0.122(3) Uani 1 2 d S . . P1 P 0.39860(3) 0.49848(7) 0.27597(5) 0.0457(2) Uani 1 1 d . . . P2 P 0.21211(4) 0.96716(9) 0.08527(5) 0.0573(3) 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 0.03174(14) 0.03330(14) 0.02899(14) -0.00211(9) 0.01835(11) -0.00265(10) C1 0.0398(17) 0.0488(19) 0.0356(17) -0.0017(14) 0.0201(15) -0.0037(15) C2 0.045(2) 0.065(2) 0.0426(19) -0.0084(17) 0.0206(16) -0.0146(18) C3 0.059(2) 0.064(2) 0.058(2) -0.0159(19) 0.031(2) -0.031(2) C4 0.066(2) 0.0419(19) 0.058(2) -0.0023(16) 0.037(2) -0.0151(17) C5 0.0422(18) 0.0386(17) 0.0393(17) -0.0050(13) 0.0268(15) -0.0040(14) C6 0.0339(16) 0.0371(16) 0.0353(16) -0.0013(13) 0.0204(14) 0.0026(13) C7 0.058(2) 0.056(2) 0.0390(18) 0.0140(16) 0.0288(18) 0.0150(18) C8 0.060(2) 0.0412(18) 0.051(2) 0.0136(16) 0.0363(19) 0.0070(17) C9 0.0317(16) 0.057(2) 0.0301(16) -0.0014(14) 0.0127(14) 0.0000(14) C10 0.0315(15) 0.0329(15) 0.0347(16) -0.0014(12) 0.0187(13) -0.0056(13) C11 0.051(2) 0.053(2) 0.0356(17) -0.0119(15) 0.0261(16) -0.0089(17) C12 0.058(2) 0.0474(19) 0.048(2) -0.0110(16) 0.0364(18) -0.0002(17) C13 0.0396(17) 0.0458(18) 0.0421(18) 0.0035(14) 0.0276(15) 0.0062(15) C14 0.058(2) 0.0415(19) 0.062(2) 0.0062(16) 0.0357(19) 0.0095(17) C15 0.072(3) 0.060(3) 0.073(3) 0.020(2) 0.040(2) 0.031(2) C16 0.055(2) 0.081(3) 0.057(2) 0.011(2) 0.023(2) 0.029(2) C17 0.044(2) 0.072(3) 0.063(2) -0.007(2) 0.0205(19) 0.0041(19) C18 0.062(2) 0.044(2) 0.060(2) 0.0089(16) 0.0430(19) 0.0010(17) C19 0.068(3) 0.056(2) 0.075(3) 0.024(2) 0.047(2) 0.0082(19) C20 0.060(2) 0.081(3) 0.051(2) 0.024(2) 0.032(2) -0.002(2) C21 0.049(2) 0.072(3) 0.0371(18) 0.0041(17) 0.0253(16) -0.0114(19) C22 0.074(3) 0.113(4) 0.042(2) 0.004(2) 0.037(2) -0.008(3) C23 0.0365(17) 0.0508(19) 0.0354(16) -0.0027(14) 0.0223(14) -0.0129(15) C24 0.082(3) 0.114(4) 0.048(2) -0.019(2) 0.047(2) -0.015(3) C25 0.052(2) 0.074(3) 0.047(2) -0.0200(18) 0.0347(18) -0.0173(19) C26 0.0378(17) 0.055(2) 0.0333(16) -0.0118(15) 0.0221(14) -0.0155(15) C27 0.072(3) 0.079(3) 0.068(3) -0.035(2) 0.050(2) -0.018(2) C28 0.072(3) 0.051(2) 0.076(3) -0.021(2) 0.050(2) -0.002(2) C29 0.056(2) 0.047(2) 0.060(2) -0.0085(17) 0.0374(19) -0.0013(17) C30 0.0392(18) 0.0452(18) 0.0353(17) 0.0016(14) 0.0208(14) -0.0017(15) C31 0.0413(19) 0.069(2) 0.063(2) 0.0047(19) 0.0284(18) -0.0146(18) C32 0.136(7) 0.126(8) 0.118(7) 0.000 0.108(6) 0.000 C33 0.36(2) 0.148(11) 0.37(2) 0.000 0.340(19) 0.000 F1 0.0954(18) 0.0770(16) 0.0540(13) 0.0057(10) 0.0503(13) 0.0036(12) F2 0.0423(12) 0.1044(19) 0.1044(19) -0.0092(16) 0.0315(13) 0.0039(12) F3 0.141(2) 0.0490(13) 0.0789(16) 0.0140(11) 0.0716(17) 0.0301(14) F4 0.0758(16) 0.0915(18) 0.1033(19) -0.0238(15) 0.0599(15) -0.0313(14) F5 0.127(2) 0.0724(16) 0.0525(13) 0.0067(11) 0.0549(15) 0.0189(14) F6 0.0626(13) 0.0442(11) 0.0706(14) 0.0087(10) 0.0334(11) 0.0106(10) F7 0.139(3) 0.083(2) 0.141(3) -0.0379(18) 0.087(2) -0.0203(19) F8 0.101(3) 0.168(4) 0.094(2) 0.030(2) 0.018(2) 0.039(2) F9 0.144(3) 0.172(3) 0.130(3) -0.023(2) 0.109(3) -0.038(3) F10 0.107(2) 0.169(3) 0.093(2) 0.052(2) 0.0349(19) 0.038(2) F11 0.148(3) 0.184(4) 0.113(3) -0.035(2) 0.105(2) -0.031(2) F12 0.172(3) 0.070(2) 0.208(4) -0.061(2) 0.106(3) -0.038(2) N1 0.0358(13) 0.0362(13) 0.0327(13) -0.0031(10) 0.0207(11) -0.0032(11) N2 0.0431(15) 0.0332(13) 0.0386(14) 0.0026(11) 0.0250(12) 0.0009(12) N3 0.0376(14) 0.0444(15) 0.0346(14) 0.0035(11) 0.0184(12) 0.0056(12) N4 0.0342(13) 0.0448(15) 0.0315(13) -0.0082(11) 0.0180(11) -0.0052(11) N5 0.0379(14) 0.0365(14) 0.0362(14) -0.0013(11) 0.0221(12) 0.0011(11) N6 0.0422(16) 0.0495(17) 0.0517(17) 0.0001(14) 0.0218(14) 0.0030(13) N7 0.0389(14) 0.0401(15) 0.0345(13) 0.0012(11) 0.0230(12) -0.0040(12) N8 0.0387(14) 0.0400(15) 0.0409(15) -0.0084(11) 0.0263(12) -0.0078(12) N9 0.0376(14) 0.0402(14) 0.0361(14) -0.0039(11) 0.0228(12) -0.0031(12) N10 0.122(6) 0.154(8) 0.107(5) 0.000 0.078(5) 0.000 P1 0.0501(5) 0.0420(5) 0.0412(5) 0.0036(4) 0.0258(4) 0.0037(4) P2 0.0664(6) 0.0539(6) 0.0454(5) -0.0033(4) 0.0306(5) 0.0011(5) _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 C6 1.943(3) . ? Ru1 N9 2.031(3) . ? Ru1 C10 2.058(3) . ? Ru1 N1 2.084(2) . ? Ru1 N8 2.123(2) . ? Ru1 N7 2.190(2) . ? C1 N1 1.350(4) . ? C1 C2 1.367(5) . ? C2 C3 1.370(5) . ? C3 C4 1.371(5) . ? C4 C5 1.372(4) . ? C5 N1 1.350(4) . ? C5 N2 1.401(4) . ? C6 N3 1.353(4) . ? C6 N2 1.357(4) . ? C7 C8 1.332(5) . ? C7 N3 1.404(4) . ? C8 N2 1.398(4) . ? C9 N3 1.450(4) . ? C9 N4 1.456(4) . ? C10 N5 1.357(4) . ? C10 N4 1.373(3) . ? C11 C12 1.329(5) . ? C11 N4 1.383(4) . ? C12 N5 1.388(4) . ? C13 N6 1.317(4) . ? C13 C14 1.374(4) . ? C13 N5 1.435(4) . ? C14 C15 1.364(5) . ? C15 C16 1.376(6) . ? C16 C17 1.358(5) . ? C17 N6 1.346(4) . ? C18 N7 1.322(4) . ? C18 C19 1.397(5) . ? C19 C20 1.356(6) . ? C20 C21 1.393(6) . ? C21 C23 1.401(4) . ? C21 C22 1.420(6) . ? C22 C24 1.334(7) . ? C23 N7 1.358(4) . ? C23 C26 1.430(5) . ? C24 C25 1.433(6) . ? C25 C27 1.395(6) . ? C25 C26 1.398(4) . ? C26 N8 1.360(4) . ? C27 C28 1.347(6) . ? C28 C29 1.401(5) . ? C29 N8 1.321(4) . ? C30 N9 1.127(4) . ? C30 C31 1.457(5) . ? C32 N10 1.086(11) . ? C32 C33 1.421(13) . ? F1 P1 1.597(2) . ? F2 P1 1.568(3) . ? F3 P1 1.584(2) . ? F4 P1 1.591(3) . ? F5 P1 1.574(2) . ? F6 P1 1.588(2) . ? F7 P2 1.584(3) . ? F8 P2 1.543(3) . ? F9 P2 1.579(3) . ? F10 P2 1.552(3) . ? F11 P2 1.567(3) . ? F12 P2 1.530(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Ru1 N9 101.73(11) . . ? C6 Ru1 C10 78.71(12) . . ? N9 Ru1 C10 87.52(10) . . ? C6 Ru1 N1 76.66(11) . . ? N9 Ru1 N1 170.52(10) . . ? C10 Ru1 N1 101.20(10) . . ? C6 Ru1 N8 101.47(11) . . ? N9 Ru1 N8 88.55(9) . . ? C10 Ru1 N8 176.01(10) . . ? N1 Ru1 N8 82.68(9) . . ? C6 Ru1 N7 173.18(11) . . ? N9 Ru1 N7 84.79(9) . . ? C10 Ru1 N7 103.80(10) . . ? N1 Ru1 N7 96.58(9) . . ? N8 Ru1 N7 76.47(10) . . ? N1 C1 C2 122.3(3) . . ? C1 C2 C3 119.5(3) . . ? C2 C3 C4 119.5(3) . . ? C3 C4 C5 118.0(3) . . ? N1 C5 C4 123.6(3) . . ? N1 C5 N2 112.1(2) . . ? C4 C5 N2 124.3(3) . . ? N3 C6 N2 105.4(2) . . ? N3 C6 Ru1 132.3(2) . . ? N2 C6 Ru1 118.7(2) . . ? C8 C7 N3 107.6(3) . . ? C7 C8 N2 106.5(3) . . ? N3 C9 N4 107.8(2) . . ? N5 C10 N4 102.5(2) . . ? N5 C10 Ru1 136.4(2) . . ? N4 C10 Ru1 121.1(2) . . ? C12 C11 N4 107.1(3) . . ? C11 C12 N5 106.5(3) . . ? N6 C13 C14 125.2(3) . . ? N6 C13 N5 115.5(3) . . ? C14 C13 N5 119.3(3) . . ? C15 C14 C13 117.5(4) . . ? C14 C15 C16 119.2(4) . . ? C17 C16 C15 118.8(4) . . ? N6 C17 C16 123.5(4) . . ? N7 C18 C19 123.3(4) . . ? C20 C19 C18 119.3(4) . . ? C19 C20 C21 119.5(3) . . ? C20 C21 C23 117.6(3) . . ? C20 C21 C22 123.5(4) . . ? C23 C21 C22 118.9(4) . . ? C24 C22 C21 121.1(4) . . ? N7 C23 C21 123.0(3) . . ? N7 C23 C26 117.2(3) . . ? C21 C23 C26 119.7(3) . . ? C22 C24 C25 122.2(4) . . ? C27 C25 C26 117.4(3) . . ? C27 C25 C24 124.8(4) . . ? C26 C25 C24 117.8(4) . . ? N8 C26 C25 122.6(3) . . ? N8 C26 C23 117.1(3) . . ? C25 C26 C23 120.3(3) . . ? C28 C27 C25 119.9(3) . . ? C27 C28 C29 119.6(4) . . ? N8 C29 C28 122.4(4) . . ? N9 C30 C31 179.7(5) . . ? N10 C32 C33 180.0(10) . . ? C5 N1 C1 116.9(3) . . ? C5 N1 Ru1 115.32(19) . . ? C1 N1 Ru1 126.6(2) . . ? C6 N2 C8 110.6(3) . . ? C6 N2 C5 115.6(2) . . ? C8 N2 C5 128.6(3) . . ? C6 N3 C7 109.7(3) . . ? C6 N3 C9 115.7(2) . . ? C7 N3 C9 126.6(3) . . ? C10 N4 C11 111.6(3) . . ? C10 N4 C9 123.5(2) . . ? C11 N4 C9 124.6(3) . . ? C10 N5 C12 112.3(3) . . ? C10 N5 C13 126.0(2) . . ? C12 N5 C13 121.5(3) . . ? C13 N6 C17 115.8(3) . . ? C18 N7 C23 117.2(3) . . ? C18 N7 Ru1 129.4(2) . . ? C23 N7 Ru1 113.4(2) . . ? C29 N8 C26 118.1(3) . . ? C29 N8 Ru1 126.2(2) . . ? C26 N8 Ru1 115.7(2) . . ? C30 N9 Ru1 173.3(2) . . ? F2 P1 F5 90.37(16) . . ? F2 P1 F3 91.17(15) . . ? F5 P1 F3 90.85(12) . . ? F2 P1 F6 89.21(13) . . ? F5 P1 F6 90.12(12) . . ? F3 P1 F6 178.96(13) . . ? F2 P1 F4 178.53(16) . . ? F5 P1 F4 90.01(16) . . ? F3 P1 F4 90.24(16) . . ? F6 P1 F4 89.38(13) . . ? F2 P1 F1 90.45(16) . . ? F5 P1 F1 179.17(17) . . ? F3 P1 F1 89.23(12) . . ? F6 P1 F1 89.80(12) . . ? F4 P1 F1 89.16(14) . . ? F12 P2 F8 90.4(2) . . ? F12 P2 F10 92.8(2) . . ? F8 P2 F10 176.8(2) . . ? F12 P2 F11 90.5(2) . . ? F8 P2 F11 91.4(2) . . ? F10 P2 F11 88.8(2) . . ? F12 P2 F9 92.6(2) . . ? F8 P2 F9 88.7(2) . . ? F10 P2 F9 90.9(2) . . ? F11 P2 F9 176.9(2) . . ? F12 P2 F7 178.8(2) . . ? F8 P2 F7 89.2(2) . . ? F10 P2 F7 87.7(2) . . ? F11 P2 F7 88.46(19) . . ? F9 P2 F7 88.41(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.570 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.062 #===END data_complex5a+5b _database_code_depnum_ccdc_archive 'CCDC 834947' #TrackingRef '- cif-Rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H60 F24 N18 O P4 Ru2' _chemical_formula_weight 1903.34 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7209(5) _cell_length_b 15.8088(6) _cell_length_c 19.1257(8) _cell_angle_alpha 86.483(3) _cell_angle_beta 81.993(3) _cell_angle_gamma 84.403(3) _cell_volume 3786.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1908 _exptl_absorpt_coefficient_mu 0.599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7620 _exptl_absorpt_correction_T_max 0.8315 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37104 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.01 _reflns_number_total 13312 _reflns_number_gt 9648 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0607P)^2^+5.6571P] 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 13312 _refine_ls_number_parameters 1040 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1373 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.015 _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 0.65617(3) 0.51145(2) 0.273424(19) 0.03317(11) Uani 1 1 d . . . Ru2 Ru 0.19205(3) 0.05846(2) 0.26685(2) 0.03558(11) Uani 1 1 d . . . C1 C -0.0670(4) 0.2188(3) 0.2282(3) 0.0550(14) Uani 1 1 d . . . H1 H -0.1141 0.2406 0.1971 0.066 Uiso 1 1 calc R . . C2 C -0.0806(4) 0.2249(3) 0.2971(3) 0.0561(14) Uani 1 1 d . . . H2 H -0.1399 0.2519 0.3236 0.067 Uiso 1 1 calc R . . C3 C 0.0671(4) 0.1216(3) 0.1534(2) 0.0391(11) Uani 1 1 d . . . C4 C 0.0372(4) 0.1378(3) 0.0876(3) 0.0501(13) Uani 1 1 d . . . H4 H -0.0080 0.1857 0.0780 0.060 Uiso 1 1 calc R . . C5 C 0.1672(4) -0.0018(3) 0.1194(2) 0.0395(11) Uani 1 1 d . . . H5 H 0.2103 -0.0505 0.1301 0.047 Uiso 1 1 calc R . . C6 C 0.0158(5) 0.1425(3) 0.3932(3) 0.0541(14) Uani 1 1 d . . . H6A H -0.0436 0.1643 0.4267 0.065 Uiso 1 1 calc R . . H6B H 0.0815 0.1536 0.4098 0.065 Uiso 1 1 calc R . . C8 C 0.0760(4) 0.0042(3) 0.3365(2) 0.0396(11) Uani 1 1 d . . . C10 C -0.0599(4) 0.0027(4) 0.4273(3) 0.0574(14) Uani 1 1 d . . . H10 H -0.1115 0.0215 0.4637 0.069 Uiso 1 1 calc R . . C11 C 0.0761(4) -0.1484(3) 0.3088(3) 0.0428(11) Uani 1 1 d . . . C13 C 0.5370(4) 0.5138(3) 0.3480(3) 0.0425(11) Uani 1 1 d . . . C16 C 0.4033(4) 0.5385(4) 0.4361(3) 0.0577(14) Uani 1 1 d . . . H16 H 0.3608 0.5646 0.4737 0.069 Uiso 1 1 calc R . . C17 C 0.3880(4) 0.4660(4) 0.4092(3) 0.0602(15) Uani 1 1 d . . . H17 H 0.3321 0.4324 0.4237 0.072 Uiso 1 1 calc R . . C18 C 0.5586(4) 0.6325(3) 0.4150(3) 0.0497(12) Uani 1 1 d . . . H18A H 0.6114 0.6066 0.4437 0.060 Uiso 1 1 calc R . . H18B H 0.5133 0.6748 0.4425 0.060 Uiso 1 1 calc R . . C20 C 0.6681(3) 0.6338(3) 0.2948(2) 0.0369(10) Uani 1 1 d . . . C22 C 0.6834(4) 0.7775(3) 0.2878(3) 0.0505(13) Uani 1 1 d . . . H22 H 0.7036 0.8307 0.2708 0.061 Uiso 1 1 calc R . . C23 C 0.6221(4) 0.7597(3) 0.3476(3) 0.0494(13) Uani 1 1 d . . . H23 H 0.5913 0.7985 0.3809 0.059 Uiso 1 1 calc R . . C25 C 0.7783(4) 0.6952(3) 0.1891(3) 0.0413(11) Uani 1 1 d . . . C26 C 0.8821(4) 0.6616(3) 0.1863(3) 0.0567(14) Uani 1 1 d . . . H26 H 0.9094 0.6392 0.2269 0.068 Uiso 1 1 calc R . . C29 C 0.7256(4) 0.5117(3) 0.1203(2) 0.0376(10) Uani 1 1 d . . . C30 C 0.6179(4) 0.5475(3) 0.1278(2) 0.0386(11) Uani 1 1 d . . . C33 C 0.8274(5) 0.4460(3) 0.3743(3) 0.0540(13) Uani 1 1 d . . . C34 C 0.4658(4) 0.0816(4) 0.1078(3) 0.0597(15) Uani 1 1 d . . . C35 C 0.4571(5) 0.1667(4) 0.0818(4) 0.0780(19) Uani 1 1 d . . . H35 H 0.5046 0.1848 0.0437 0.094 Uiso 1 1 calc R . . C36 C 0.3788(5) 0.2223(4) 0.1126(4) 0.0764(19) Uani 1 1 d . . . H36 H 0.3730 0.2789 0.0961 0.092 Uiso 1 1 calc R . . C37 C 0.3076(5) 0.1945(3) 0.1688(3) 0.0607(15) Uani 1 1 d . . . H37 H 0.2542 0.2335 0.1890 0.073 Uiso 1 1 calc R . . C38 C 0.3905(4) 0.0586(3) 0.1643(3) 0.0445(12) Uani 1 1 d . . . C39 C 0.3931(4) -0.0268(3) 0.1938(3) 0.0441(12) Uani 1 1 d . . . C40 C 0.3254(4) -0.1220(3) 0.2793(3) 0.0507(13) Uani 1 1 d . . . H40 H 0.2772 -0.1341 0.3190 0.061 Uiso 1 1 calc R . . C41 C 0.0787(4) 0.1500(3) 0.2703(3) 0.0403(11) Uani 1 1 d . . . C42 C 0.1422(4) 0.0115(3) 0.0519(3) 0.0472(12) Uani 1 1 d . . . H42 H 0.1699 -0.0264 0.0173 0.057 Uiso 1 1 calc R . . C43 C 0.0757(4) 0.0818(4) 0.0361(3) 0.0555(14) Uani 1 1 d . . . H43 H 0.0568 0.0914 -0.0092 0.067 Uiso 1 1 calc R . . C44 C -0.0422(5) -0.0753(4) 0.4042(3) 0.0596(15) Uani 1 1 d . . . H44 H -0.0781 -0.1221 0.4221 0.072 Uiso 1 1 calc R . . C45 C 0.1216(5) -0.2077(4) 0.2042(3) 0.0629(15) Uani 1 1 d . . . H45 H 0.1333 -0.2021 0.1551 0.075 Uiso 1 1 calc R . . C46 C 0.1374(5) -0.2869(4) 0.2350(4) 0.0694(17) Uani 1 1 d . . . H46 H 0.1586 -0.3337 0.2076 0.083 Uiso 1 1 calc R . . C47 C 0.1214(5) -0.2962(3) 0.3072(4) 0.0691(17) Uani 1 1 d . . . H47 H 0.1314 -0.3497 0.3297 0.083 Uiso 1 1 calc R . . C48 C 0.0903(5) -0.2256(3) 0.3462(3) 0.0613(15) Uani 1 1 d . . . H48 H 0.0794 -0.2294 0.3953 0.074 Uiso 1 1 calc R . . C49 C 0.3542(6) 0.0917(5) 0.4637(4) 0.091(2) Uani 1 1 d . . . H49A H 0.3037 0.1166 0.5004 0.136 Uiso 1 1 calc R . . H49B H 0.4123 0.1267 0.4522 0.136 Uiso 1 1 calc R . . H49C H 0.3808 0.0359 0.4796 0.136 Uiso 1 1 calc R . . C50 C 0.3025(4) 0.0852(3) 0.4013(3) 0.0573(14) Uani 1 1 d . . . C51 C 0.6314(4) 0.3250(3) 0.2267(3) 0.0535(13) Uani 1 1 d . . . H51 H 0.6928 0.3310 0.1948 0.064 Uiso 1 1 calc R . . C52 C 0.5820(5) 0.2512(4) 0.2289(3) 0.0667(16) Uani 1 1 d . . . H52 H 0.6101 0.2074 0.1996 0.080 Uiso 1 1 calc R . . C53 C 0.4907(6) 0.2430(4) 0.2751(4) 0.0736(18) Uani 1 1 d . . . H53 H 0.4570 0.1931 0.2773 0.088 Uiso 1 1 calc R . . C54 C 0.4482(5) 0.3080(4) 0.3181(3) 0.0589(15) Uani 1 1 d . . . H54 H 0.3857 0.3038 0.3492 0.071 Uiso 1 1 calc R . . C55 C 0.5035(4) 0.3798(3) 0.3125(3) 0.0440(12) Uani 1 1 d . . . C56 C 0.7975(6) 0.7276(4) 0.0717(3) 0.0681(17) Uani 1 1 d . . . H56 H 0.7688 0.7504 0.0318 0.082 Uiso 1 1 calc R . . C57 C 0.9014(5) 0.6957(4) 0.0639(4) 0.0688(18) Uani 1 1 d . . . H57 H 0.9421 0.6969 0.0195 0.083 Uiso 1 1 calc R . . C58 C 0.9449(5) 0.6623(4) 0.1212(4) 0.0704(18) Uani 1 1 d . . . H58 H 1.0158 0.6402 0.1169 0.084 Uiso 1 1 calc R . . C59 C 0.4655(4) 0.5883(3) 0.2020(3) 0.0565(14) Uani 1 1 d . . . H59 H 0.4281 0.5927 0.2472 0.068 Uiso 1 1 calc R . . C60 C 0.4132(5) 0.6165(4) 0.1446(4) 0.0711(18) Uani 1 1 d . . . H60 H 0.3433 0.6408 0.1520 0.085 Uiso 1 1 calc R . . C61 C 0.4642(5) 0.6086(4) 0.0784(4) 0.0678(17) Uani 1 1 d . . . H61 H 0.4290 0.6269 0.0400 0.081 Uiso 1 1 calc R . . C62 C 0.5695(5) 0.5731(3) 0.0673(3) 0.0515(13) Uani 1 1 d . . . C63 C 0.6288(6) 0.5586(4) -0.0003(3) 0.0664(17) Uani 1 1 d . . . H63 H 0.5969 0.5741 -0.0406 0.080 Uiso 1 1 calc R . . C64 C 0.7293(6) 0.5233(4) -0.0072(3) 0.0646(17) Uani 1 1 d . . . H64 H 0.7657 0.5148 -0.0522 0.078 Uiso 1 1 calc R . . C65 C 0.7818(4) 0.4984(3) 0.0528(3) 0.0491(13) Uani 1 1 d . . . C66 C 0.8858(5) 0.4607(3) 0.0496(3) 0.0590(15) Uani 1 1 d . . . H66 H 0.9255 0.4494 0.0060 0.071 Uiso 1 1 calc R . . C67 C 0.9291(4) 0.4404(3) 0.1095(3) 0.0575(14) Uani 1 1 d . . . H67 H 0.9986 0.4152 0.1073 0.069 Uiso 1 1 calc R . . C68 C 0.8701(4) 0.4572(3) 0.1744(3) 0.0484(12) Uani 1 1 d . . . H68 H 0.9018 0.4436 0.2151 0.058 Uiso 1 1 calc R . . C69 C 0.9116(6) 0.4216(4) 0.4182(4) 0.085(2) Uani 1 1 d . . . H69A H 0.9776 0.4080 0.3884 0.128 Uiso 1 1 calc R . . H69B H 0.8935 0.3727 0.4481 0.128 Uiso 1 1 calc R . . H69C H 0.9190 0.4679 0.4468 0.128 Uiso 1 1 calc R . . C70 C 0.4751(4) -0.0872(3) 0.1670(3) 0.0520(13) Uani 1 1 d . . . C71 C 0.5461(5) 0.0183(5) 0.0808(3) 0.0750(18) Uani 1 1 d . . . H71 H 0.5969 0.0327 0.0432 0.090 Uiso 1 1 calc R . . C72 C 0.5499(5) -0.0620(5) 0.1088(3) 0.0734(18) Uani 1 1 d . . . H72 H 0.6028 -0.1021 0.0896 0.088 Uiso 1 1 calc R . . C73 C 0.4757(5) -0.1695(4) 0.1987(4) 0.0667(17) Uani 1 1 d . . . H73 H 0.5255 -0.2126 0.1809 0.080 Uiso 1 1 calc R . . C74 C 0.4030(5) -0.1856(3) 0.2555(3) 0.0609(15) Uani 1 1 d . . . H74 H 0.4050 -0.2392 0.2785 0.073 Uiso 1 1 calc R . . C75 C 0.8344(7) 0.9897(6) 0.2163(5) 0.120(3) Uani 1 1 d . . . H75A H 0.8840 0.9713 0.2495 0.144 Uiso 1 1 calc R . . H75B H 0.8393 1.0501 0.2053 0.144 Uiso 1 1 calc R . . C76 C 0.8645(7) 0.9459(7) 0.1544(4) 0.121(3) Uani 1 1 d . . . H76A H 0.8636 0.8859 0.1652 0.182 Uiso 1 1 calc R . . H76B H 0.9350 0.9583 0.1341 0.182 Uiso 1 1 calc R . . H76C H 0.8154 0.9635 0.1213 0.182 Uiso 1 1 calc R . . C78 C 0.5827(8) 1.0069(6) 0.3325(6) 0.139(4) Uani 1 1 d . . . H78A H 0.5388 1.0325 0.2985 0.208 Uiso 1 1 calc R . . H78B H 0.5618 1.0329 0.3769 0.208 Uiso 1 1 calc R . . H78C H 0.5741 0.9471 0.3384 0.208 Uiso 1 1 calc R . . C79 C 0.6928(9) 1.0190(8) 0.3078(6) 0.157(5) Uani 1 1 d . . . H79A H 0.6999 1.0794 0.2985 0.188 Uiso 1 1 calc R . . H79B H 0.7356 0.9993 0.3448 0.188 Uiso 1 1 calc R . . F1 F 0.8693(3) 0.1871(2) -0.01888(19) 0.0725(9) Uani 1 1 d . . . F2 F 0.6568(3) 0.2885(2) 0.05109(18) 0.0807(10) Uani 1 1 d . . . F3 F 0.8274(3) 0.2754(2) 0.07067(19) 0.0797(11) Uani 1 1 d . . . F4 F 0.6974(3) 0.1989(2) -0.03693(19) 0.0820(11) Uani 1 1 d . . . F5 F 0.7415(3) 0.1589(2) 0.0698(2) 0.0919(12) Uani 1 1 d . . . F6 F 0.2406(6) 0.8749(4) 0.4645(3) 0.170(3) Uani 1 1 d . . . F7 F 0.2842(6) 0.8517(5) 0.5698(3) 0.211(4) Uani 1 1 d . . . F8 F 0.3385(4) 0.7603(3) 0.4309(2) 0.1293(19) Uani 1 1 d . . . F9 F 0.3836(8) 0.7372(6) 0.5346(3) 0.239(5) Uani 1 1 d . . . F10 F 0.4104(6) 0.8504(7) 0.4783(6) 0.267(5) Uani 1 1 d . . . F11 F 0.0715(4) 0.4555(5) 0.2687(3) 0.171(3) Uani 1 1 d . . . F12 F 0.1588(5) 0.5122(2) 0.1748(2) 0.1245(18) Uani 1 1 d . . . F13 F 0.1439(5) 0.3753(3) 0.1782(3) 0.149(2) Uani 1 1 d . . . F14 F 0.2991(4) 0.4163(4) 0.1867(3) 0.1341(18) Uani 1 1 d . . . F15 F 0.2299(5) 0.4983(3) 0.2749(3) 0.142(2) Uani 1 1 d . . . F16 F 0.2123(4) 0.3591(3) 0.2803(3) 0.1344(19) Uani 1 1 d . . . F17 F 0.0392(4) 0.3379(6) 0.5335(4) 0.218(4) Uani 1 1 d . . . F18 F 0.1534(5) 0.3936(5) 0.4636(4) 0.191(3) Uani 1 1 d . . . F19 F 0.7840(3) 0.3158(2) -0.03733(19) 0.0760(10) Uani 1 1 d . . . F20 F 0.2142(6) 0.7610(5) 0.5219(5) 0.229(4) Uani 1 1 d . . . F21 F 0.2833(4) 0.2970(3) 0.4945(3) 0.1184(16) Uani 1 1 d . . . F22 F 0.1884(7) 0.3728(7) 0.5659(5) 0.274(6) Uani 1 1 d . . . F23 F 0.1641(5) 0.2459(7) 0.5668(6) 0.299(7) Uani 1 1 d . . . F24 F 0.1376(10) 0.2633(7) 0.4638(7) 0.356(8) Uani 1 1 d . . . N1 N 0.0093(3) 0.1839(2) 0.3240(2) 0.0479(10) Uani 1 1 d . . . N2 N 0.0327(3) 0.1728(2) 0.2105(2) 0.0437(10) Uani 1 1 d . . . N3 N 0.1320(3) 0.0524(2) 0.17106(19) 0.0365(9) Uani 1 1 d . . . N4 N 0.0126(3) 0.0506(2) 0.3871(2) 0.0446(10) Uani 1 1 d . . . N5 N 0.0398(3) -0.0740(2) 0.3483(2) 0.0453(10) Uani 1 1 d . . . N6 N 0.3168(3) -0.0449(2) 0.2481(2) 0.0396(9) Uani 1 1 d . . . N7 N 0.3120(3) 0.1149(2) 0.1951(2) 0.0422(9) Uani 1 1 d . . . N8 N 0.2610(3) 0.0793(2) 0.3535(2) 0.0474(10) Uani 1 1 d . . . N9 N 0.7115(3) 0.7002(2) 0.2555(2) 0.0400(9) Uani 1 1 d . . . N10 N 0.6119(3) 0.6735(2) 0.3518(2) 0.0412(9) Uani 1 1 d . . . N11 N 0.4949(3) 0.5682(3) 0.3975(2) 0.0465(10) Uani 1 1 d . . . N12 N 0.4717(3) 0.4496(3) 0.3550(2) 0.0476(10) Uani 1 1 d . . . N13 N 0.5938(3) 0.3886(2) 0.2691(2) 0.0411(9) Uani 1 1 d . . . N14 N 0.7637(3) 0.4671(2) 0.3398(2) 0.0444(10) Uani 1 1 d . . . N15 N 0.5656(3) 0.5554(2) 0.1956(2) 0.0386(9) Uani 1 1 d . . . N16 N 0.7699(3) 0.4919(2) 0.1809(2) 0.0364(9) Uani 1 1 d . . . N17 N 0.0904(4) -0.1373(3) 0.2399(2) 0.0518(11) Uani 1 1 d . . . N18 N 0.7338(4) 0.7278(3) 0.1344(2) 0.0532(11) Uani 1 1 d . . . O1 O 0.7313(4) 0.9774(3) 0.2483(3) 0.0870(14) Uani 1 1 d . . . P1 P 0.15853(13) 0.31843(11) 0.51473(9) 0.0682(5) Uani 1 1 d . . . P3 P 0.76257(11) 0.23776(8) 0.01627(7) 0.0479(3) Uani 1 1 d . . . P4 P 0.18436(14) 0.43668(10) 0.22930(9) 0.0653(4) Uani 1 1 d . . . P6 P 0.31415(14) 0.80667(12) 0.50152(10) 0.0737(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0291(2) 0.0356(2) 0.0339(2) -0.00113(15) -0.00180(15) -0.00237(15) Ru2 0.0334(2) 0.0335(2) 0.0399(2) -0.00514(16) -0.00618(16) 0.00050(15) C1 0.050(3) 0.048(3) 0.064(4) -0.004(3) -0.011(3) 0.017(2) C2 0.049(3) 0.042(3) 0.074(4) -0.014(3) -0.006(3) 0.016(2) C3 0.036(3) 0.038(3) 0.043(3) -0.001(2) -0.005(2) -0.002(2) C4 0.050(3) 0.049(3) 0.052(3) 0.004(2) -0.016(3) 0.002(2) C5 0.038(3) 0.037(2) 0.043(3) -0.002(2) -0.003(2) -0.004(2) C6 0.057(3) 0.053(3) 0.052(3) -0.021(3) -0.004(3) 0.005(3) C8 0.040(3) 0.042(3) 0.037(3) -0.004(2) -0.008(2) 0.001(2) C10 0.054(3) 0.064(4) 0.049(3) -0.009(3) 0.014(3) -0.003(3) C11 0.041(3) 0.038(3) 0.048(3) -0.007(2) 0.002(2) -0.004(2) C13 0.039(3) 0.045(3) 0.043(3) -0.003(2) -0.003(2) -0.006(2) C16 0.049(3) 0.069(4) 0.049(3) -0.002(3) 0.017(3) -0.010(3) C17 0.045(3) 0.072(4) 0.057(4) 0.007(3) 0.019(3) -0.017(3) C18 0.057(3) 0.050(3) 0.039(3) -0.007(2) 0.006(2) -0.003(2) C20 0.029(2) 0.042(3) 0.039(3) -0.001(2) -0.003(2) -0.0021(19) C22 0.059(3) 0.035(3) 0.057(3) -0.002(2) -0.003(3) -0.006(2) C23 0.054(3) 0.042(3) 0.052(3) -0.010(2) -0.007(3) 0.001(2) C25 0.040(3) 0.035(2) 0.048(3) -0.001(2) 0.003(2) -0.012(2) C26 0.040(3) 0.058(3) 0.071(4) -0.005(3) -0.005(3) -0.004(2) C29 0.045(3) 0.034(2) 0.036(3) -0.0007(19) -0.003(2) -0.012(2) C30 0.043(3) 0.031(2) 0.043(3) 0.002(2) -0.008(2) -0.007(2) C33 0.061(4) 0.052(3) 0.051(3) -0.003(3) -0.017(3) -0.001(3) C34 0.038(3) 0.081(4) 0.059(4) 0.001(3) 0.001(3) -0.017(3) C35 0.066(4) 0.088(5) 0.081(5) 0.019(4) -0.002(4) -0.034(4) C36 0.069(4) 0.060(4) 0.100(5) 0.020(4) -0.005(4) -0.023(3) C37 0.055(3) 0.044(3) 0.085(4) 0.003(3) -0.012(3) -0.011(3) C38 0.033(3) 0.051(3) 0.052(3) -0.006(2) -0.009(2) -0.007(2) C39 0.033(3) 0.054(3) 0.047(3) -0.009(2) -0.011(2) -0.001(2) C40 0.042(3) 0.052(3) 0.059(3) 0.003(3) -0.014(3) 0.001(2) C41 0.048(3) 0.028(2) 0.046(3) -0.006(2) -0.008(2) -0.005(2) C42 0.049(3) 0.052(3) 0.042(3) -0.007(2) -0.006(2) -0.006(2) C43 0.063(4) 0.066(4) 0.040(3) 0.004(3) -0.016(3) -0.005(3) C44 0.059(4) 0.058(3) 0.056(4) -0.001(3) 0.013(3) -0.010(3) C45 0.070(4) 0.062(4) 0.056(4) -0.022(3) 0.003(3) -0.012(3) C46 0.067(4) 0.048(3) 0.091(5) -0.027(3) 0.013(4) -0.013(3) C47 0.071(4) 0.038(3) 0.094(5) -0.002(3) 0.005(4) -0.006(3) C48 0.069(4) 0.048(3) 0.062(4) 0.001(3) 0.009(3) -0.008(3) C49 0.089(5) 0.117(6) 0.075(5) -0.026(4) -0.045(4) 0.009(4) C50 0.051(3) 0.059(3) 0.065(4) -0.017(3) -0.016(3) 0.001(3) C51 0.056(3) 0.047(3) 0.058(3) -0.004(3) -0.009(3) -0.006(3) C52 0.087(5) 0.048(3) 0.068(4) -0.011(3) -0.010(4) -0.017(3) C53 0.095(5) 0.057(4) 0.077(5) 0.001(3) -0.021(4) -0.031(4) C54 0.060(4) 0.062(3) 0.058(4) 0.009(3) -0.007(3) -0.030(3) C55 0.045(3) 0.045(3) 0.043(3) 0.008(2) -0.012(2) -0.011(2) C56 0.091(5) 0.059(4) 0.047(4) 0.008(3) 0.006(3) -0.002(3) C57 0.074(4) 0.054(3) 0.070(4) -0.007(3) 0.032(4) -0.014(3) C58 0.042(3) 0.067(4) 0.097(5) -0.014(4) 0.015(3) -0.008(3) C59 0.038(3) 0.058(3) 0.072(4) -0.004(3) -0.010(3) 0.005(2) C60 0.044(3) 0.073(4) 0.096(5) 0.004(4) -0.024(4) 0.011(3) C61 0.071(4) 0.059(4) 0.079(5) 0.014(3) -0.042(4) -0.003(3) C62 0.070(4) 0.042(3) 0.048(3) 0.005(2) -0.023(3) -0.012(3) C63 0.101(5) 0.061(4) 0.043(3) 0.011(3) -0.025(4) -0.023(4) C64 0.097(5) 0.063(4) 0.034(3) -0.005(3) 0.006(3) -0.027(4) C65 0.060(3) 0.046(3) 0.040(3) -0.007(2) 0.006(3) -0.017(3) C66 0.062(4) 0.058(3) 0.052(4) -0.021(3) 0.025(3) -0.016(3) C67 0.040(3) 0.056(3) 0.072(4) -0.017(3) 0.015(3) -0.004(2) C68 0.037(3) 0.046(3) 0.061(3) -0.008(2) -0.005(2) 0.001(2) C69 0.085(5) 0.092(5) 0.085(5) 0.001(4) -0.049(4) 0.008(4) C70 0.032(3) 0.064(4) 0.057(3) -0.013(3) -0.003(2) 0.010(2) C71 0.043(3) 0.112(6) 0.066(4) -0.007(4) 0.011(3) -0.010(3) C72 0.044(3) 0.101(5) 0.070(4) -0.021(4) 0.001(3) 0.017(3) C73 0.052(4) 0.062(4) 0.085(5) -0.020(3) -0.014(3) 0.020(3) C74 0.053(3) 0.045(3) 0.083(4) -0.001(3) -0.018(3) 0.012(3) C75 0.094(7) 0.136(8) 0.137(9) -0.036(6) -0.005(6) -0.038(6) C76 0.103(7) 0.189(10) 0.074(6) -0.019(6) 0.015(5) -0.062(6) C78 0.123(9) 0.123(8) 0.157(10) -0.045(7) 0.016(7) 0.023(6) C79 0.130(9) 0.175(10) 0.170(11) -0.105(9) -0.018(8) 0.023(8) F1 0.058(2) 0.076(2) 0.082(2) -0.0181(18) -0.0124(18) 0.0169(17) F2 0.064(2) 0.104(3) 0.066(2) -0.0028(19) -0.0010(18) 0.0247(19) F3 0.089(3) 0.068(2) 0.091(3) -0.0234(19) -0.047(2) 0.0089(18) F4 0.069(2) 0.103(3) 0.082(3) -0.016(2) -0.027(2) -0.019(2) F5 0.121(3) 0.066(2) 0.085(3) 0.0279(19) -0.010(2) -0.016(2) F6 0.209(7) 0.156(5) 0.119(4) -0.019(4) -0.007(4) 0.100(5) F7 0.204(7) 0.280(8) 0.149(5) -0.151(6) -0.044(5) 0.092(6) F8 0.141(4) 0.148(4) 0.091(3) -0.044(3) -0.021(3) 0.055(3) F9 0.294(10) 0.299(10) 0.084(4) -0.027(5) -0.032(5) 0.201(8) F10 0.139(6) 0.309(11) 0.360(13) -0.101(10) 0.052(7) -0.124(7) F11 0.077(3) 0.280(8) 0.135(5) 0.010(5) 0.019(3) 0.021(4) F12 0.212(6) 0.068(2) 0.088(3) 0.001(2) -0.036(3) 0.036(3) F13 0.187(6) 0.086(3) 0.197(6) -0.031(3) -0.114(5) 0.010(3) F14 0.106(4) 0.153(4) 0.126(4) -0.007(3) 0.021(3) 0.026(3) F15 0.151(5) 0.143(4) 0.146(5) -0.065(4) -0.071(4) 0.015(4) F16 0.153(5) 0.129(4) 0.111(4) 0.057(3) -0.027(3) 0.010(3) F17 0.052(3) 0.365(10) 0.214(7) 0.193(7) -0.019(3) -0.034(4) F18 0.111(4) 0.222(7) 0.220(7) 0.144(6) -0.005(4) -0.035(4) F19 0.079(2) 0.065(2) 0.080(2) 0.0189(18) -0.009(2) -0.0036(18) F20 0.179(7) 0.230(8) 0.266(9) -0.033(7) 0.083(7) -0.097(6) F21 0.086(3) 0.110(3) 0.150(4) -0.009(3) 0.017(3) -0.009(3) F22 0.191(7) 0.389(13) 0.269(9) -0.231(10) -0.141(7) 0.131(8) F23 0.097(4) 0.334(11) 0.437(14) 0.315(11) -0.054(7) -0.064(6) F24 0.370(15) 0.296(12) 0.479(18) -0.253(13) -0.250(14) 0.012(10) N1 0.047(2) 0.040(2) 0.056(3) -0.014(2) -0.006(2) 0.0074(19) N2 0.041(2) 0.037(2) 0.053(3) -0.0017(19) -0.009(2) 0.0034(17) N3 0.035(2) 0.034(2) 0.041(2) -0.0040(17) -0.0055(17) -0.0020(16) N4 0.048(2) 0.043(2) 0.042(2) -0.0111(18) -0.0024(19) 0.0018(19) N5 0.045(2) 0.042(2) 0.047(2) -0.0027(18) 0.002(2) -0.0045(18) N6 0.037(2) 0.037(2) 0.045(2) -0.0017(18) -0.0096(19) 0.0004(17) N7 0.039(2) 0.038(2) 0.052(3) -0.0005(18) -0.0100(19) -0.0080(17) N8 0.043(2) 0.045(2) 0.055(3) -0.010(2) -0.011(2) 0.0030(19) N9 0.036(2) 0.039(2) 0.043(2) -0.0010(17) -0.0004(18) -0.0056(17) N10 0.042(2) 0.042(2) 0.040(2) -0.0053(17) -0.0012(18) -0.0040(17) N11 0.044(2) 0.052(2) 0.042(2) -0.0056(19) 0.0073(19) -0.0108(19) N12 0.045(2) 0.053(3) 0.044(2) 0.002(2) 0.004(2) -0.011(2) N13 0.045(2) 0.040(2) 0.040(2) 0.0002(18) -0.0085(19) -0.0047(18) N14 0.047(2) 0.041(2) 0.045(2) -0.0025(19) -0.012(2) 0.0009(18) N15 0.032(2) 0.036(2) 0.048(2) 0.0006(17) -0.0074(18) -0.0039(16) N16 0.030(2) 0.036(2) 0.044(2) -0.0021(17) -0.0027(17) -0.0042(16) N17 0.065(3) 0.046(2) 0.046(3) -0.007(2) -0.006(2) -0.010(2) N18 0.054(3) 0.052(3) 0.049(3) 0.006(2) 0.001(2) 0.000(2) O1 0.098(4) 0.078(3) 0.085(3) -0.018(3) 0.007(3) -0.025(3) P1 0.0565(10) 0.0820(11) 0.0711(11) 0.0186(9) -0.0166(8) -0.0342(8) P3 0.0447(8) 0.0479(7) 0.0509(8) 0.0004(6) -0.0106(6) 0.0005(6) P4 0.0676(10) 0.0664(10) 0.0612(10) 0.0012(8) -0.0122(8) 0.0000(8) P6 0.0613(10) 0.0831(12) 0.0711(12) -0.0241(9) 0.0100(9) 0.0066(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C13 1.930(5) . ? Ru1 C20 2.025(4) . ? Ru1 N14 2.040(4) . ? Ru1 N15 2.054(4) . ? Ru1 N16 2.142(4) . ? Ru1 N13 2.178(4) . ? Ru2 C41 1.938(5) . ? Ru2 N8 2.038(4) . ? Ru2 C8 2.061(5) . ? Ru2 N3 2.092(4) . ? Ru2 N7 2.130(4) . ? Ru2 N6 2.174(4) . ? C1 C2 1.313(8) . ? C1 N2 1.408(6) . ? C2 N1 1.404(6) . ? C3 N3 1.360(6) . ? C3 C4 1.366(7) . ? C3 N2 1.395(6) . ? C4 C43 1.372(7) . ? C5 N3 1.348(6) . ? C5 C42 1.372(6) . ? C6 N1 1.450(7) . ? C6 N4 1.469(6) . ? C8 N5 1.356(6) . ? C8 N4 1.371(6) . ? C10 C44 1.323(7) . ? C10 N4 1.372(7) . ? C11 N17 1.308(6) . ? C11 C48 1.385(7) . ? C11 N5 1.440(6) . ? C13 N11 1.338(6) . ? C13 N12 1.363(6) . ? C16 C17 1.326(8) . ? C16 N11 1.397(6) . ? C17 N12 1.394(6) . ? C18 N11 1.442(6) . ? C18 N10 1.451(6) . ? C20 N10 1.368(6) . ? C20 N9 1.369(6) . ? C22 C23 1.323(7) . ? C22 N9 1.398(6) . ? C23 N10 1.378(6) . ? C25 N18 1.312(6) . ? C25 C26 1.370(7) . ? C25 N9 1.428(6) . ? C26 C58 1.383(8) . ? C29 N16 1.364(6) . ? C29 C65 1.402(7) . ? C29 C30 1.423(6) . ? C30 N15 1.379(6) . ? C30 C62 1.404(6) . ? C33 N14 1.129(6) . ? C33 C69 1.459(8) . ? C34 C38 1.396(7) . ? C34 C35 1.405(9) . ? C34 C71 1.424(9) . ? C35 C36 1.357(9) . ? C36 C37 1.384(8) . ? C37 N7 1.325(6) . ? C38 N7 1.365(6) . ? C38 C39 1.432(7) . ? C39 N6 1.356(6) . ? C39 C70 1.406(7) . ? C40 N6 1.325(6) . ? C40 C74 1.389(7) . ? C41 N1 1.357(6) . ? C41 N2 1.369(6) . ? C42 C43 1.375(7) . ? C44 N5 1.387(6) . ? C45 N17 1.340(7) . ? C45 C46 1.359(8) . ? C46 C47 1.369(9) . ? C47 C48 1.376(8) . ? C49 C50 1.453(8) . ? C50 N8 1.131(6) . ? C51 N13 1.341(6) . ? C51 C52 1.374(7) . ? C52 C53 1.369(9) . ? C53 C54 1.377(8) . ? C54 C55 1.384(7) . ? C55 N13 1.334(6) . ? C55 N12 1.405(6) . ? C56 N18 1.350(7) . ? C56 C57 1.358(9) . ? C57 C58 1.352(9) . ? C59 N15 1.319(6) . ? C59 C60 1.390(8) . ? C60 C61 1.348(9) . ? C61 C62 1.394(8) . ? C62 C63 1.423(8) . ? C63 C64 1.337(9) . ? C64 C65 1.423(8) . ? C65 C66 1.392(8) . ? C66 C67 1.347(8) . ? C67 C68 1.384(7) . ? C68 N16 1.331(6) . ? C70 C73 1.401(8) . ? C70 C72 1.425(8) . ? C71 C72 1.346(9) . ? C73 C74 1.353(8) . ? C75 O1 1.395(9) . ? C75 C76 1.397(10) . ? C78 C79 1.442(13) . ? C79 O1 1.357(10) . ? F1 P3 1.593(3) . ? F2 P3 1.582(3) . ? F3 P3 1.590(3) . ? F4 P3 1.585(3) . ? F5 P3 1.583(4) . ? F6 P6 1.561(6) . ? F7 P6 1.510(5) . ? F8 P6 1.555(4) . ? F9 P6 1.506(6) . ? F10 P6 1.466(7) . ? F11 P4 1.537(5) . ? F12 P4 1.576(4) . ? F13 P4 1.586(5) . ? F14 P4 1.584(5) . ? F15 P4 1.549(5) . ? F16 P4 1.564(4) . ? F17 P1 1.516(5) . ? F18 P1 1.494(5) . ? F19 P3 1.575(3) . ? F20 P6 1.515(7) . ? F21 P1 1.589(5) . ? F22 P1 1.453(7) . ? F23 P1 1.475(6) . ? F24 P1 1.414(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Ru1 C20 86.27(19) . . ? C13 Ru1 N14 93.44(18) . . ? C20 Ru1 N14 91.98(16) . . ? C13 Ru1 N15 94.55(18) . . ? C20 Ru1 N15 88.66(16) . . ? N14 Ru1 N15 172.01(16) . . ? C13 Ru1 N16 168.23(16) . . ? C20 Ru1 N16 103.40(16) . . ? N14 Ru1 N16 92.91(15) . . ? N15 Ru1 N16 79.20(15) . . ? C13 Ru1 N13 76.43(17) . . ? C20 Ru1 N13 161.89(17) . . ? N14 Ru1 N13 94.35(15) . . ? N15 Ru1 N13 87.41(14) . . ? N16 Ru1 N13 93.22(14) . . ? C41 Ru2 N8 101.35(17) . . ? C41 Ru2 C8 79.60(19) . . ? N8 Ru2 C8 86.31(17) . . ? C41 Ru2 N3 76.52(17) . . ? N8 Ru2 N3 171.70(15) . . ? C8 Ru2 N3 101.06(16) . . ? C41 Ru2 N7 100.31(17) . . ? N8 Ru2 N7 93.55(16) . . ? C8 Ru2 N7 179.81(17) . . ? N3 Ru2 N7 79.07(14) . . ? C41 Ru2 N6 172.35(17) . . ? N8 Ru2 N6 85.83(15) . . ? C8 Ru2 N6 103.71(16) . . ? N3 Ru2 N6 96.00(14) . . ? N7 Ru2 N6 76.41(15) . . ? C2 C1 N2 106.6(5) . . ? C1 C2 N1 108.6(5) . . ? N3 C3 C4 123.6(4) . . ? N3 C3 N2 112.3(4) . . ? C4 C3 N2 124.1(4) . . ? C3 C4 C43 118.4(5) . . ? N3 C5 C42 123.0(4) . . ? N1 C6 N4 108.1(4) . . ? N5 C8 N4 102.6(4) . . ? N5 C8 Ru2 136.1(3) . . ? N4 C8 Ru2 121.4(3) . . ? C44 C10 N4 106.8(5) . . ? N17 C11 C48 125.4(5) . . ? N17 C11 N5 116.6(4) . . ? C48 C11 N5 117.9(5) . . ? N11 C13 N12 105.5(4) . . ? N11 C13 Ru1 135.3(4) . . ? N12 C13 Ru1 119.1(3) . . ? C17 C16 N11 107.3(5) . . ? C16 C17 N12 107.1(4) . . ? N11 C18 N10 111.2(4) . . ? N10 C20 N9 102.2(4) . . ? N10 C20 Ru1 124.1(3) . . ? N9 C20 Ru1 132.6(3) . . ? C23 C22 N9 106.0(4) . . ? C22 C23 N10 107.8(4) . . ? N18 C25 C26 124.8(5) . . ? N18 C25 N9 115.1(4) . . ? C26 C25 N9 120.0(5) . . ? C25 C26 C58 117.7(6) . . ? N16 C29 C65 122.8(5) . . ? N16 C29 C30 117.0(4) . . ? C65 C29 C30 120.2(4) . . ? N15 C30 C62 123.0(5) . . ? N15 C30 C29 117.3(4) . . ? C62 C30 C29 119.7(5) . . ? N14 C33 C69 178.0(6) . . ? C38 C34 C35 117.0(6) . . ? C38 C34 C71 118.5(6) . . ? C35 C34 C71 124.5(6) . . ? C36 C35 C34 119.6(6) . . ? C35 C36 C37 119.7(6) . . ? N7 C37 C36 123.1(6) . . ? N7 C38 C34 123.1(5) . . ? N7 C38 C39 116.2(4) . . ? C34 C38 C39 120.7(5) . . ? N6 C39 C70 123.1(5) . . ? N6 C39 C38 117.6(4) . . ? C70 C39 C38 119.2(5) . . ? N6 C40 C74 123.1(5) . . ? N1 C41 N2 105.0(4) . . ? N1 C41 Ru2 133.1(4) . . ? N2 C41 Ru2 118.9(3) . . ? C5 C42 C43 119.0(5) . . ? C4 C43 C42 119.5(5) . . ? C10 C44 N5 107.1(5) . . ? N17 C45 C46 124.3(6) . . ? C45 C46 C47 118.6(5) . . ? C46 C47 C48 119.2(6) . . ? C47 C48 C11 116.9(6) . . ? N8 C50 C49 178.7(7) . . ? N13 C51 C52 121.9(6) . . ? C53 C52 C51 119.0(6) . . ? C52 C53 C54 120.7(5) . . ? C53 C54 C55 116.4(6) . . ? N13 C55 C54 124.1(5) . . ? N13 C55 N12 113.3(4) . . ? C54 C55 N12 122.6(5) . . ? N18 C56 C57 123.5(6) . . ? C58 C57 C56 119.2(6) . . ? C57 C58 C26 118.9(6) . . ? N15 C59 C60 123.3(6) . . ? C61 C60 C59 119.8(6) . . ? C60 C61 C62 120.2(5) . . ? C61 C62 C30 116.8(5) . . ? C61 C62 C63 124.6(5) . . ? C30 C62 C63 118.6(5) . . ? C64 C63 C62 121.6(5) . . ? C63 C64 C65 121.4(5) . . ? C66 C65 C29 117.0(5) . . ? C66 C65 C64 124.6(5) . . ? C29 C65 C64 118.5(5) . . ? C67 C66 C65 120.2(5) . . ? C66 C67 C68 120.0(5) . . ? N16 C68 C67 122.6(5) . . ? C73 C70 C39 117.1(5) . . ? C73 C70 C72 124.3(5) . . ? C39 C70 C72 118.6(5) . . ? C72 C71 C34 121.2(6) . . ? C71 C72 C70 121.7(6) . . ? C74 C73 C70 119.3(5) . . ? C73 C74 C40 119.9(5) . . ? O1 C75 C76 113.4(7) . . ? O1 C79 C78 113.0(9) . . ? C41 N1 C2 109.6(4) . . ? C41 N1 C6 115.5(4) . . ? C2 N1 C6 128.4(5) . . ? C41 N2 C3 115.2(4) . . ? C41 N2 C1 110.2(4) . . ? C3 N2 C1 128.8(4) . . ? C5 N3 C3 116.4(4) . . ? C5 N3 Ru2 127.1(3) . . ? C3 N3 Ru2 114.8(3) . . ? C8 N4 C10 112.0(4) . . ? C8 N4 C6 123.8(4) . . ? C10 N4 C6 124.0(4) . . ? C8 N5 C44 111.5(4) . . ? C8 N5 C11 126.9(4) . . ? C44 N5 C11 121.6(4) . . ? C40 N6 C39 117.2(4) . . ? C40 N6 Ru2 129.7(4) . . ? C39 N6 Ru2 113.1(3) . . ? C37 N7 C38 117.5(5) . . ? C37 N7 Ru2 126.5(4) . . ? C38 N7 Ru2 114.8(3) . . ? C50 N8 Ru2 175.2(4) . . ? C20 N9 C22 112.0(4) . . ? C20 N9 C25 126.4(4) . . ? C22 N9 C25 121.5(4) . . ? C20 N10 C23 112.0(4) . . ? C20 N10 C18 126.4(4) . . ? C23 N10 C18 121.1(4) . . ? C13 N11 C16 110.3(4) . . ? C13 N11 C18 118.8(4) . . ? C16 N11 C18 128.8(4) . . ? C13 N12 C17 109.8(4) . . ? C13 N12 C55 116.9(4) . . ? C17 N12 C55 133.1(4) . . ? C55 N13 C51 117.9(4) . . ? C55 N13 Ru1 113.6(3) . . ? C51 N13 Ru1 128.4(3) . . ? C33 N14 Ru1 175.6(4) . . ? C59 N15 C30 116.8(4) . . ? C59 N15 Ru1 128.9(4) . . ? C30 N15 Ru1 114.2(3) . . ? C68 N16 C29 117.5(4) . . ? C68 N16 Ru1 130.2(3) . . ? C29 N16 Ru1 112.0(3) . . ? C11 N17 C45 115.6(5) . . ? C25 N18 C56 115.8(5) . . ? C79 O1 C75 118.2(7) . . ? F24 P1 F22 175.7(6) . . ? F24 P1 F23 90.0(8) . . ? F22 P1 F23 89.3(7) . . ? F24 P1 F18 91.8(7) . . ? F22 P1 F18 89.0(6) . . ? F23 P1 F18 178.3(7) . . ? F24 P1 F17 88.3(6) . . ? F22 P1 F17 95.9(5) . . ? F23 P1 F17 93.7(4) . . ? F18 P1 F17 86.3(3) . . ? F24 P1 F21 91.0(6) . . ? F22 P1 F21 84.8(4) . . ? F23 P1 F21 86.1(3) . . ? F18 P1 F21 93.9(3) . . ? F17 P1 F21 179.2(5) . . ? F19 P3 F2 89.6(2) . . ? F19 P3 F5 179.6(3) . . ? F2 P3 F5 90.7(2) . . ? F19 P3 F4 90.4(2) . . ? F2 P3 F4 90.0(2) . . ? F5 P3 F4 89.5(2) . . ? F19 P3 F3 90.7(2) . . ? F2 P3 F3 89.9(2) . . ? F5 P3 F3 89.5(2) . . ? F4 P3 F3 178.9(2) . . ? F19 P3 F1 90.2(2) . . ? F2 P3 F1 179.7(3) . . ? F5 P3 F1 89.5(2) . . ? F4 P3 F1 90.1(2) . . ? F3 P3 F1 89.93(19) . . ? F11 P4 F15 91.4(4) . . ? F11 P4 F16 93.7(3) . . ? F15 P4 F16 91.4(3) . . ? F11 P4 F12 88.3(3) . . ? F15 P4 F12 90.5(3) . . ? F16 P4 F12 177.2(3) . . ? F11 P4 F14 178.2(4) . . ? F15 P4 F14 90.3(3) . . ? F16 P4 F14 86.9(3) . . ? F12 P4 F14 91.0(3) . . ? F11 P4 F13 92.0(4) . . ? F15 P4 F13 176.0(4) . . ? F16 P4 F13 90.5(3) . . ? F12 P4 F13 87.5(3) . . ? F14 P4 F13 86.3(3) . . ? F10 P6 F9 87.9(6) . . ? F10 P6 F7 95.5(5) . . ? F9 P6 F7 93.0(4) . . ? F10 P6 F20 177.3(6) . . ? F9 P6 F20 93.3(6) . . ? F7 P6 F20 86.9(5) . . ? F10 P6 F8 87.0(5) . . ? F9 P6 F8 88.8(3) . . ? F7 P6 F8 176.9(4) . . ? F20 P6 F8 90.5(4) . . ? F10 P6 F6 93.6(6) . . ? F9 P6 F6 176.8(5) . . ? F7 P6 F6 89.6(4) . . ? F20 P6 F6 85.2(5) . . ? F8 P6 F6 88.5(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.024 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.084 #===END data_complex_6 _database_code_depnum_ccdc_archive 'CCDC 834948' #TrackingRef '- cif-Rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H26.50 F12 N9.50 O P2 Ru' _chemical_formula_weight 963.15 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7158(7) _cell_length_b 11.7418(9) _cell_length_c 14.8628(11) _cell_angle_alpha 107.818(7) _cell_angle_beta 90.493(6) _cell_angle_gamma 96.708(6) _cell_volume 1931.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 962 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7650 _exptl_absorpt_correction_T_max 0.9116 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13018 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6793 _reflns_number_gt 5315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. The following restraints have been used to DFIX some bond distances and to solve PLAT241, PLAT230, and PLAT234: DFIX C33 C34 1.45 0.01 DFIX N10 C33 1.10 0.01 DFIX N10 C34 2.70 0.01 simu 0.005 0.01 3.8 C15 delu 0.02 0.01 C14 C15 delu 0.001 P2 F9 delu 0.001 P2 F8 ; _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^)+(0.1177P)^2^+0.8286P] 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 6793 _refine_ls_number_parameters 528 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1911 _refine_ls_wR_factor_gt 0.1702 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.061 _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 0.87388(3) 0.99589(4) 0.72695(3) 0.04321(19) Uani 1 1 d . . . C1 C 0.8358(5) 0.8460(5) 0.8738(4) 0.0531(13) Uani 1 1 d . . . H1 H 0.8289 0.7766 0.8219 0.064 Uiso 1 1 calc R . . C2 C 0.8212(6) 0.8358(7) 0.9617(5) 0.0684(17) Uani 1 1 d . . . H2 H 0.8040 0.7601 0.9694 0.082 Uiso 1 1 calc R . . C3 C 0.8318(6) 0.9370(7) 1.0390(4) 0.076(2) Uani 1 1 d . . . H3 H 0.8223 0.9300 1.0992 0.091 Uiso 1 1 calc R . . C4 C 0.8564(6) 1.0487(6) 1.0277(4) 0.0649(16) Uani 1 1 d . . . H4 H 0.8630 1.1189 1.0789 0.078 Uiso 1 1 calc R . . C5 C 0.8709(5) 1.0514(5) 0.9367(4) 0.0538(13) Uani 1 1 d . . . C6 C 0.9099(5) 1.1510(5) 0.8230(4) 0.0516(13) Uani 1 1 d . . . C7 C 0.9289(7) 1.2780(6) 0.9719(5) 0.083(2) Uani 1 1 d . . . H7 H 0.9275 1.3074 1.0375 0.100 Uiso 1 1 calc R . . C8 C 0.9601(8) 1.3409(6) 0.9134(5) 0.093(3) Uani 1 1 d . . . H8 H 0.9877 1.4225 0.9310 0.112 Uiso 1 1 calc R . . C9 C 0.9824(7) 1.2861(7) 0.7360(5) 0.080(2) Uani 1 1 d . . . H9A H 1.0614 1.2695 0.7268 0.096 Uiso 1 1 calc R . . H9B H 0.9800 1.3703 0.7418 0.096 Uiso 1 1 calc R . . C10 C 0.8710(5) 1.0890(5) 0.6318(4) 0.0481(12) Uani 1 1 d . . . C11 C 0.8769(7) 1.2566(6) 0.5841(5) 0.0732(19) Uani 1 1 d . . . H11 H 0.8934 1.3359 0.5839 0.088 Uiso 1 1 calc R . . C12 C 0.8173(6) 1.1660(6) 0.5170(4) 0.0703(18) Uani 1 1 d . . . H12 H 0.7839 1.1699 0.4613 0.084 Uiso 1 1 calc R . . C13 C 0.7522(5) 0.9521(5) 0.4944(4) 0.0520(13) Uani 1 1 d . . . C14 C 0.6409(5) 0.9485(6) 0.4857(5) 0.0650(16) Uani 1 1 d U . . H14 H 0.6036 1.0154 0.5138 0.078 Uiso 1 1 calc R . . C15 C 0.5825(8) 0.8418(12) 0.4332(7) 0.111(3) Uani 1 1 d U . . H15 H 0.5032 0.8366 0.4244 0.133 Uiso 1 1 calc R . . C16 C 0.6351(10) 0.7410(9) 0.3926(6) 0.098(3) Uani 1 1 d . . . H16 H 0.5919 0.6685 0.3590 0.118 Uiso 1 1 calc R . . C17 C 0.7516(9) 0.7488(7) 0.4024(5) 0.086(2) Uani 1 1 d . . . H17 H 0.7891 0.6819 0.3746 0.104 Uiso 1 1 calc R . . C18 C 0.6338(6) 1.0860(7) 0.7637(5) 0.0694(17) Uani 1 1 d . . . H18 H 0.6735 1.1630 0.7891 0.083 Uiso 1 1 calc R . . C19 C 0.5136(8) 1.0715(10) 0.7637(6) 0.099(3) Uani 1 1 d . . . H19 H 0.4750 1.1379 0.7900 0.119 Uiso 1 1 calc R . . C20 C 0.4553(7) 0.9647(10) 0.7266(7) 0.099(3) Uani 1 1 d . . . H20 H 0.3754 0.9558 0.7255 0.119 Uiso 1 1 calc R . . C21 C 0.5138(6) 0.8616(8) 0.6880(5) 0.079(2) Uani 1 1 d . . . C22 C 0.6332(5) 0.8843(6) 0.6903(4) 0.0535(14) Uani 1 1 d . . . C23 C 0.4584(7) 0.7418(11) 0.6508(7) 0.103(3) Uani 1 1 d . . . H23 H 0.3788 0.7268 0.6518 0.123 Uiso 1 1 calc R . . C24 C 0.5192(8) 0.6500(10) 0.6141(6) 0.103(3) Uani 1 1 d . . . H24 H 0.4807 0.5722 0.5914 0.123 Uiso 1 1 calc R . . C25 C 0.6418(6) 0.6682(6) 0.6090(5) 0.0688(18) Uani 1 1 d . . . C26 C 0.6972(5) 0.7863(5) 0.6482(4) 0.0540(14) Uani 1 1 d . . . C27 C 0.7110(8) 0.5794(6) 0.5687(5) 0.083(2) Uani 1 1 d . . . H27 H 0.6777 0.4997 0.5439 0.100 Uiso 1 1 calc R . . C28 C 0.8238(8) 0.6061(6) 0.5648(5) 0.076(2) Uani 1 1 d . . . H28 H 0.8688 0.5461 0.5357 0.092 Uiso 1 1 calc R . . C29 C 0.8739(6) 0.7250(5) 0.6049(4) 0.0599(15) Uani 1 1 d . . . H29 H 0.9531 0.7429 0.6031 0.072 Uiso 1 1 calc R . . C30 C 1.0305(5) 0.9828(5) 0.7126(4) 0.0500(13) Uani 1 1 d . . . C31 C 0.2808(9) 0.3547(12) 0.8663(7) 0.106(3) Uani 1 1 d . . . C32 C 0.3363(9) 0.4752(10) 0.8956(7) 0.118(3) Uani 1 1 d . . . H32A H 0.3023 0.5207 0.8610 0.178 Uiso 1 1 calc R . . H32B H 0.4166 0.4754 0.8836 0.178 Uiso 1 1 calc R . . H32C H 0.3273 0.5111 0.9621 0.178 Uiso 1 1 calc R . . C33 C 0.467(3) 0.906(2) 0.982(3) 0.206(14) Uiso 0.50 1 d PD . . C34 C 0.480(2) 0.779(2) 0.9312(19) 0.158(9) Uiso 0.50 1 d PD . . H34A H 0.4418 0.7566 0.8697 0.238 Uiso 0.50 1 calc PR . . H34B H 0.4460 0.7288 0.9662 0.238 Uiso 0.50 1 calc PR . . H34C H 0.5601 0.7705 0.9246 0.238 Uiso 0.50 1 calc PR . . F1 F 0.0375(4) 0.7043(5) 0.7597(3) 0.1065(15) Uani 1 1 d . . . F2 F 0.1552(4) 0.6778(4) 0.6396(3) 0.0985(14) Uani 1 1 d . . . F3 F 0.2250(4) 0.7203(4) 0.7895(4) 0.1108(16) Uani 1 1 d . . . F4 F 0.2365(4) 0.5436(4) 0.6863(4) 0.1048(15) Uani 1 1 d . . . F5 F 0.1123(5) 0.5614(5) 0.8044(3) 0.1108(16) Uani 1 1 d . . . F6 F 0.0456(4) 0.5187(5) 0.6552(3) 0.1049(15) Uani 1 1 d . . . F7 F 0.6382(9) 0.5568(8) 0.8901(7) 0.220(4) Uani 1 1 d . . . F8 F 0.5928(14) 0.4539(19) 0.7298(12) 0.378(12) Uani 1 1 d U . . F9 F 0.7825(12) 0.5065(17) 0.8786(10) 0.319(8) Uani 1 1 d U . . F10 F 0.7471(12) 0.5527(13) 0.7673(8) 0.329(9) Uani 1 1 d . . . F11 F 0.6030(16) 0.3809(9) 0.8379(11) 0.352(11) Uani 1 1 d . . . F12 F 0.7329(16) 0.3679(11) 0.7526(14) 0.352(10) Uani 1 1 d . . . N1 N 0.8601(4) 0.9541(4) 0.8600(3) 0.0477(10) Uani 1 1 d . . . N2 N 0.8992(4) 1.1606(4) 0.9157(3) 0.0563(12) Uani 1 1 d . . . N3 N 0.9442(5) 1.2636(4) 0.8219(4) 0.0691(14) Uani 1 1 d . . . N4 N 0.9097(5) 1.2102(4) 0.6541(3) 0.0604(12) Uani 1 1 d . . . N5 N 0.8150(4) 1.0640(4) 0.5471(3) 0.0512(11) Uani 1 1 d . . . N6 N 0.8137(6) 0.8572(5) 0.4541(4) 0.0788(16) Uani 1 1 d . . . N7 N 0.6923(4) 0.9953(4) 0.7294(3) 0.0510(11) Uani 1 1 d . . . N8 N 0.8124(4) 0.8142(4) 0.6459(3) 0.0474(10) Uani 1 1 d . . . N9 N 0.2366(11) 0.2621(12) 0.8406(7) 0.156(4) Uani 1 1 d . . . N10 N 0.469(3) 1.010(2) 1.019(2) 0.207(12) Uiso 0.50 1 d PD . . O1 O 1.1252(4) 0.9747(5) 0.7028(3) 0.0738(12) Uani 1 1 d . . . P1 P 0.13525(14) 0.62139(15) 0.72187(11) 0.0580(4) Uani 1 1 d . . . P2 P 0.6806(3) 0.4687(3) 0.8058(2) 0.1129(8) Uani 1 1 d U . . 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 0.0515(3) 0.0392(3) 0.0364(3) 0.00938(18) 0.00104(18) 0.00193(19) C1 0.063(3) 0.051(3) 0.045(3) 0.016(3) -0.002(2) 0.002(3) C2 0.081(4) 0.072(4) 0.057(4) 0.033(3) -0.006(3) -0.005(3) C3 0.087(5) 0.101(6) 0.041(4) 0.028(4) -0.001(3) -0.001(4) C4 0.082(4) 0.069(4) 0.037(3) 0.009(3) 0.004(3) 0.005(3) C5 0.060(3) 0.057(3) 0.042(3) 0.012(3) 0.005(2) 0.010(3) C6 0.067(4) 0.040(3) 0.044(3) 0.010(2) 0.000(2) 0.000(3) C7 0.132(7) 0.058(4) 0.044(4) -0.002(3) -0.003(4) 0.002(4) C8 0.146(8) 0.048(4) 0.061(4) -0.006(3) -0.009(4) -0.018(4) C9 0.109(6) 0.064(4) 0.061(4) 0.023(3) -0.001(4) -0.024(4) C10 0.058(3) 0.045(3) 0.043(3) 0.015(2) 0.010(2) 0.009(2) C11 0.114(6) 0.045(3) 0.066(4) 0.027(3) 0.013(4) 0.009(4) C12 0.102(5) 0.066(4) 0.052(4) 0.028(3) 0.010(3) 0.021(4) C13 0.075(4) 0.049(3) 0.034(3) 0.014(2) 0.006(2) 0.015(3) C14 0.058(4) 0.068(4) 0.074(4) 0.027(3) -0.009(3) 0.016(3) C15 0.085(6) 0.151(9) 0.113(7) 0.075(7) -0.030(5) -0.015(6) C16 0.139(8) 0.087(6) 0.058(5) 0.023(4) -0.028(5) -0.028(6) C17 0.143(8) 0.055(4) 0.050(4) 0.005(3) 0.013(4) -0.002(5) C18 0.070(4) 0.078(5) 0.062(4) 0.022(3) 0.005(3) 0.016(4) C19 0.085(6) 0.131(8) 0.097(6) 0.042(6) 0.029(5) 0.051(6) C20 0.048(4) 0.155(9) 0.105(7) 0.056(7) 0.006(4) 0.010(5) C21 0.060(4) 0.108(6) 0.071(5) 0.033(4) -0.002(3) 0.005(4) C22 0.048(3) 0.069(4) 0.044(3) 0.025(3) -0.006(2) -0.009(3) C23 0.061(5) 0.136(9) 0.102(7) 0.040(6) -0.013(4) -0.029(5) C24 0.099(7) 0.112(7) 0.090(6) 0.043(6) -0.023(5) -0.045(6) C25 0.080(5) 0.060(4) 0.058(4) 0.019(3) -0.018(3) -0.023(4) C26 0.063(4) 0.057(3) 0.041(3) 0.021(3) -0.010(2) -0.007(3) C27 0.120(7) 0.048(4) 0.067(5) 0.006(3) -0.025(4) -0.015(4) C28 0.113(6) 0.049(4) 0.064(4) 0.012(3) -0.014(4) 0.012(4) C29 0.081(4) 0.047(3) 0.047(3) 0.007(3) -0.007(3) 0.013(3) C30 0.062(4) 0.040(3) 0.044(3) 0.008(2) 0.001(2) 0.002(3) C31 0.107(7) 0.135(9) 0.087(6) 0.064(7) -0.009(5) -0.013(7) C32 0.116(8) 0.139(9) 0.113(8) 0.058(7) -0.001(6) 0.014(7) F1 0.085(3) 0.135(4) 0.099(3) 0.024(3) 0.019(2) 0.045(3) F2 0.109(3) 0.106(3) 0.101(3) 0.061(3) 0.024(3) 0.013(3) F3 0.090(3) 0.088(3) 0.117(4) -0.017(3) -0.013(3) -0.007(2) F4 0.108(3) 0.087(3) 0.113(4) 0.010(3) 0.010(3) 0.045(3) F5 0.142(4) 0.121(4) 0.077(3) 0.049(3) -0.005(3) -0.004(3) F6 0.110(3) 0.100(3) 0.085(3) 0.021(3) -0.021(2) -0.043(3) F7 0.222(9) 0.169(8) 0.224(10) -0.014(7) 0.027(7) 0.044(7) F8 0.309(16) 0.46(2) 0.366(19) 0.230(17) -0.195(14) -0.217(18) F9 0.243(12) 0.49(2) 0.259(13) 0.134(14) -0.064(8) 0.135(13) F10 0.418(18) 0.366(17) 0.193(9) 0.180(11) -0.092(10) -0.242(15) F11 0.55(2) 0.135(7) 0.349(17) 0.058(9) 0.291(18) -0.014(11) F12 0.39(2) 0.176(10) 0.45(2) 0.001(12) 0.235(18) 0.113(12) N1 0.051(3) 0.052(3) 0.038(2) 0.012(2) -0.0004(18) 0.003(2) N2 0.077(3) 0.044(3) 0.038(2) 0.000(2) 0.003(2) 0.003(2) N3 0.102(4) 0.043(3) 0.052(3) 0.005(2) 0.000(3) -0.008(3) N4 0.086(4) 0.046(3) 0.048(3) 0.017(2) 0.007(2) -0.001(2) N5 0.069(3) 0.047(3) 0.039(2) 0.014(2) 0.005(2) 0.011(2) N6 0.110(5) 0.067(4) 0.058(3) 0.019(3) 0.012(3) 0.007(3) N7 0.055(3) 0.056(3) 0.046(3) 0.019(2) 0.007(2) 0.015(2) N8 0.060(3) 0.045(2) 0.036(2) 0.0119(19) -0.0027(19) 0.005(2) N9 0.206(12) 0.166(10) 0.110(7) 0.078(8) -0.003(7) -0.022(9) O1 0.054(3) 0.083(3) 0.078(3) 0.016(2) 0.006(2) 0.007(2) P1 0.0631(10) 0.0527(9) 0.0549(9) 0.0120(7) 0.0037(7) 0.0067(7) P2 0.132(2) 0.0919(17) 0.131(2) 0.0477(17) 0.0475(16) 0.0402(16) _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 C30 1.868(6) . ? Ru1 C6 1.937(5) . ? Ru1 C10 2.038(5) . ? Ru1 N7 2.127(5) . ? Ru1 N8 2.139(4) . ? Ru1 N1 2.181(4) . ? C1 N1 1.344(7) . ? C1 C2 1.359(8) . ? C2 C3 1.369(10) . ? C3 C4 1.370(9) . ? C4 C5 1.374(8) . ? C5 N1 1.337(7) . ? C5 N2 1.414(7) . ? C6 N3 1.341(7) . ? C6 N2 1.356(7) . ? C7 C8 1.330(10) . ? C7 N2 1.378(8) . ? C8 N3 1.381(8) . ? C9 N3 1.445(8) . ? C9 N4 1.464(8) . ? C10 N5 1.347(7) . ? C10 N4 1.378(7) . ? C11 C12 1.334(9) . ? C11 N4 1.383(8) . ? C12 N5 1.398(7) . ? C13 C14 1.304(8) . ? C13 N6 1.381(8) . ? C13 N5 1.419(7) . ? C14 C15 1.356(12) . ? C15 C16 1.373(14) . ? C16 C17 1.361(13) . ? C17 N6 1.385(9) . ? C18 N7 1.308(8) . ? C18 C19 1.399(11) . ? C19 C20 1.309(13) . ? C20 C21 1.428(12) . ? C21 C22 1.391(9) . ? C21 C23 1.417(12) . ? C22 N7 1.354(7) . ? C22 C26 1.431(9) . ? C23 C24 1.339(13) . ? C24 C25 1.433(12) . ? C25 C27 1.389(11) . ? C25 C26 1.404(8) . ? C26 N8 1.354(7) . ? C27 C28 1.328(11) . ? C28 C29 1.394(9) . ? C29 N8 1.334(7) . ? C30 O1 1.132(7) . ? C31 N9 1.098(13) . ? C31 C32 1.421(14) . ? C33 N10 1.168(9) . ? C33 N10 1.17(4) 2_677 ? C33 C34 1.475(9) . ? F1 P1 1.585(5) . ? F2 P1 1.566(4) . ? F3 P1 1.564(4) . ? F4 P1 1.577(4) . ? F5 P1 1.601(5) . ? F6 P1 1.579(4) . ? F7 P2 1.491(9) . ? F8 P2 1.477(12) . ? F9 P2 1.534(11) . ? F10 P2 1.443(9) . ? F11 P2 1.485(9) . ? F12 P2 1.416(9) . ? N10 N10 0.93(6) 2_677 ? N10 C33 1.17(4) 2_677 ? 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 C30 Ru1 C6 90.5(2) . . ? C30 Ru1 C10 92.1(2) . . ? C6 Ru1 C10 86.7(2) . . ? C30 Ru1 N7 173.84(19) . . ? C6 Ru1 N7 95.5(2) . . ? C10 Ru1 N7 86.80(19) . . ? C30 Ru1 N8 96.8(2) . . ? C6 Ru1 N8 166.9(2) . . ? C10 Ru1 N8 103.92(19) . . ? N7 Ru1 N8 77.65(18) . . ? C30 Ru1 N1 97.2(2) . . ? C6 Ru1 N1 75.9(2) . . ? C10 Ru1 N1 160.34(19) . . ? N7 Ru1 N1 85.76(16) . . ? N8 Ru1 N1 92.22(16) . . ? N1 C1 C2 121.6(6) . . ? C1 C2 C3 120.0(6) . . ? C2 C3 C4 120.0(6) . . ? C3 C4 C5 116.5(6) . . ? N1 C5 C4 124.7(6) . . ? N1 C5 N2 113.3(5) . . ? C4 C5 N2 122.0(5) . . ? N3 C6 N2 105.0(5) . . ? N3 C6 Ru1 134.8(4) . . ? N2 C6 Ru1 120.2(4) . . ? C8 C7 N2 106.1(6) . . ? C7 C8 N3 108.0(6) . . ? N3 C9 N4 111.0(5) . . ? N5 C10 N4 103.2(4) . . ? N5 C10 Ru1 132.3(4) . . ? N4 C10 Ru1 123.0(4) . . ? C12 C11 N4 107.0(5) . . ? C11 C12 N5 106.5(5) . . ? C14 C13 N6 125.3(6) . . ? C14 C13 N5 117.0(5) . . ? N6 C13 N5 117.7(5) . . ? C13 C14 C15 116.3(7) . . ? C14 C15 C16 123.0(9) . . ? C17 C16 C15 118.9(8) . . ? C16 C17 N6 119.3(8) . . ? N7 C18 C19 122.3(8) . . ? C20 C19 C18 120.2(8) . . ? C19 C20 C21 120.4(7) . . ? C22 C21 C23 120.0(8) . . ? C22 C21 C20 115.6(8) . . ? C23 C21 C20 124.4(8) . . ? N7 C22 C21 123.3(6) . . ? N7 C22 C26 118.1(5) . . ? C21 C22 C26 118.7(6) . . ? C24 C23 C21 120.8(8) . . ? C23 C24 C25 121.9(8) . . ? C27 C25 C26 116.9(7) . . ? C27 C25 C24 125.8(7) . . ? C26 C25 C24 117.3(8) . . ? N8 C26 C25 122.3(6) . . ? N8 C26 C22 116.5(5) . . ? C25 C26 C22 121.1(6) . . ? C28 C27 C25 121.3(7) . . ? C27 C28 C29 119.2(7) . . ? N8 C29 C28 122.5(7) . . ? O1 C30 Ru1 179.1(5) . . ? N9 C31 C32 177.3(11) . . ? N10 C33 N10 47(3) . 2_677 ? N10 C33 C34 173(5) . . ? N10 C33 C34 126(4) 2_677 . ? C5 N1 C1 117.2(5) . . ? C5 N1 Ru1 113.9(4) . . ? C1 N1 Ru1 128.8(4) . . ? C6 N2 C7 110.8(5) . . ? C6 N2 C5 116.2(4) . . ? C7 N2 C5 132.7(5) . . ? C6 N3 C8 109.9(5) . . ? C6 N3 C9 120.7(5) . . ? C8 N3 C9 127.9(6) . . ? C10 N4 C11 111.3(5) . . ? C10 N4 C9 128.0(5) . . ? C11 N4 C9 120.6(5) . . ? C10 N5 C12 111.9(5) . . ? C10 N5 C13 126.6(4) . . ? C12 N5 C13 121.4(5) . . ? C13 N6 C17 117.1(7) . . ? C18 N7 C22 118.2(5) . . ? C18 N7 Ru1 128.5(5) . . ? C22 N7 Ru1 113.3(4) . . ? C29 N8 C26 117.9(5) . . ? C29 N8 Ru1 128.1(4) . . ? C26 N8 Ru1 113.5(4) . . ? N10 N10 C33 67(3) 2_677 . ? N10 N10 C33 66(3) 2_677 2_677 ? C33 N10 C33 133(3) . 2_677 ? F3 P1 F2 92.0(3) . . ? F3 P1 F4 88.4(3) . . ? F2 P1 F4 89.3(3) . . ? F3 P1 F6 178.2(3) . . ? F2 P1 F6 89.5(3) . . ? F4 P1 F6 90.7(3) . . ? F3 P1 F1 89.3(3) . . ? F2 P1 F1 90.2(3) . . ? F4 P1 F1 177.6(3) . . ? F6 P1 F1 91.7(3) . . ? F3 P1 F5 89.4(3) . . ? F2 P1 F5 178.6(3) . . ? F4 P1 F5 90.9(3) . . ? F6 P1 F5 89.1(3) . . ? F1 P1 F5 89.6(3) . . ? F12 P2 F10 94.5(9) . . ? F12 P2 F8 93.1(12) . . ? F10 P2 F8 86.7(7) . . ? F12 P2 F11 86.0(7) . . ? F10 P2 F11 174.3(10) . . ? F8 P2 F11 87.5(10) . . ? F12 P2 F7 158.7(10) . . ? F10 P2 F7 98.8(8) . . ? F8 P2 F7 104.2(11) . . ? F11 P2 F7 82.5(6) . . ? F12 P2 F9 90.4(11) . . ? F10 P2 F9 81.7(8) . . ? F8 P2 F9 168.1(9) . . ? F11 P2 F9 104.1(11) . . ? F7 P2 F9 75.2(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.116 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.105 #===END data_complex_7 _database_code_depnum_ccdc_archive 'CCDC 834949' #TrackingRef '- cif-Rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H50 F12 N10 P4 Ru' _chemical_formula_weight 1255.96 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2411(3) _cell_length_b 15.6921(7) _cell_length_c 16.1366(8) _cell_angle_alpha 66.734(4) _cell_angle_beta 77.441(3) _cell_angle_gamma 77.248(3) _cell_volume 2747.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8476 _exptl_absorpt_correction_T_max 0.8753 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23698 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9669 _reflns_number_gt 7948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0608P)^2^+2.3224P] 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 9669 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8344(5) 0.8464(5) 0.8995(4) 0.0812(16) Uani 1 1 d . . . H1 H 0.8862 0.8067 0.9378 0.097 Uiso 1 1 calc R . . C2 C 0.7610(7) 0.9108(6) 0.9269(4) 0.099(2) Uani 1 1 d . . . H2 H 0.7637 0.9159 0.9818 0.119 Uiso 1 1 calc R . . C3 C 0.6824(6) 0.9686(5) 0.8730(5) 0.106(2) Uani 1 1 d . . . H3 H 0.6294 1.0127 0.8913 0.127 Uiso 1 1 calc R . . C4 C 0.6832(5) 0.9603(4) 0.7903(4) 0.0809(15) Uani 1 1 d . . . H4 H 0.6318 0.9990 0.7511 0.097 Uiso 1 1 calc R . . C5 C 0.7627(3) 0.8930(3) 0.7688(3) 0.0448(9) Uani 1 1 d . . . C6 C 0.7276(2) 0.8407(2) 0.6484(2) 0.0319(7) Uani 1 1 d . . . C7 C 0.8451(3) 0.9490(3) 0.6090(3) 0.0463(9) Uani 1 1 d . . . H7 H 0.8871 0.9888 0.6143 0.056 Uiso 1 1 calc R . . C8 C 0.8389(3) 0.9377(3) 0.5336(3) 0.0429(9) Uani 1 1 d . . . H8 H 0.8756 0.9679 0.4755 0.052 Uiso 1 1 calc R . . C9 C 0.7255(3) 0.8530(2) 0.4898(2) 0.0374(8) Uani 1 1 d . . . H9A H 0.7525 0.7885 0.4947 0.045 Uiso 1 1 calc R . . H9B H 0.7534 0.8938 0.4291 0.045 Uiso 1 1 calc R . . C10 C 0.5358(3) 0.8376(2) 0.5870(2) 0.0299(7) Uani 1 1 d . . . C11 C 0.4316(3) 0.9225(2) 0.4728(2) 0.0400(8) Uani 1 1 d . . . H11 H 0.3690 0.9519 0.4426 0.048 Uiso 1 1 calc R . . C12 C 0.5392(3) 0.9209(2) 0.4350(2) 0.0380(8) Uani 1 1 d . . . H12 H 0.5668 0.9491 0.3736 0.046 Uiso 1 1 calc R . . C13 C 0.3217(3) 0.8658(2) 0.6242(3) 0.0405(9) Uani 1 1 d . . . C14 C 0.2416(3) 0.8291(3) 0.6056(3) 0.0554(11) Uani 1 1 d . . . H14 H 0.2588 0.8015 0.5619 0.066 Uiso 1 1 calc R . . C15 C 0.1337(4) 0.8352(3) 0.6551(4) 0.0747(16) Uani 1 1 d . . . H15 H 0.0764 0.8119 0.6448 0.090 Uiso 1 1 calc R . . C16 C 0.1131(4) 0.8756(4) 0.7184(4) 0.0805(17) Uani 1 1 d . . . H16 H 0.0413 0.8810 0.7516 0.097 Uiso 1 1 calc R . . C17 C 0.1992(4) 0.9081(4) 0.7327(3) 0.0738(14) Uani 1 1 d . . . H17 H 0.1847 0.9332 0.7781 0.089 Uiso 1 1 calc R . . C18 C 0.4402(3) 0.6040(2) 0.6649(3) 0.0409(8) Uani 1 1 d . . . C19 C 0.4636(3) 0.6556(3) 0.5725(3) 0.0481(9) Uani 1 1 d . . . H19 H 0.5015 0.7069 0.5538 0.058 Uiso 1 1 calc R . . C20 C 0.4322(4) 0.6328(3) 0.5078(3) 0.0617(12) Uani 1 1 d . . . H20 H 0.4470 0.6691 0.4462 0.074 Uiso 1 1 calc R . . C21 C 0.3789(4) 0.5557(4) 0.5354(4) 0.0726(14) Uani 1 1 d . . . H21 H 0.3565 0.5405 0.4921 0.087 Uiso 1 1 calc R . . C22 C 0.3581(4) 0.5011(3) 0.6256(4) 0.0690(14) Uani 1 1 d . . . H22 H 0.3233 0.4483 0.6434 0.083 Uiso 1 1 calc R . . C23 C 0.3895(3) 0.5248(3) 0.6907(3) 0.0573(11) Uani 1 1 d . . . H23 H 0.3764 0.4872 0.7521 0.069 Uiso 1 1 calc R . . C24 C 0.3425(3) 0.6545(2) 0.8237(3) 0.0418(9) Uani 1 1 d . . . C25 C 0.2402(3) 0.6417(3) 0.8108(3) 0.0523(10) Uani 1 1 d . . . H25 H 0.2370 0.6248 0.7624 0.063 Uiso 1 1 calc R . . C26 C 0.1421(3) 0.6538(3) 0.8697(4) 0.0648(13) Uani 1 1 d . . . H26 H 0.0736 0.6448 0.8607 0.078 Uiso 1 1 calc R . . C27 C 0.1460(4) 0.6792(3) 0.9414(3) 0.0655(13) Uani 1 1 d . . . H27 H 0.0801 0.6876 0.9805 0.079 Uiso 1 1 calc R . . C28 C 0.2459(4) 0.6921(3) 0.9552(3) 0.0587(11) Uani 1 1 d . . . H28 H 0.2481 0.7089 1.0039 0.070 Uiso 1 1 calc R . . C29 C 0.3446(3) 0.6801(3) 0.8969(3) 0.0490(10) Uani 1 1 d . . . H29 H 0.4126 0.6891 0.9066 0.059 Uiso 1 1 calc R . . C30 C 0.5481(3) 0.5236(2) 0.8235(3) 0.0454(9) Uani 1 1 d . . . H30A H 0.4920 0.4827 0.8583 0.054 Uiso 1 1 calc R . . H30B H 0.6016 0.4938 0.7855 0.054 Uiso 1 1 calc R . . C31 C 0.6091(3) 0.5378(3) 0.8877(3) 0.0441(9) Uani 1 1 d . . . H31A H 0.6547 0.4791 0.9187 0.053 Uiso 1 1 calc R . . H31B H 0.5540 0.5556 0.9334 0.053 Uiso 1 1 calc R . . C32 C 0.7347(3) 0.6402(3) 0.9272(2) 0.0403(8) Uani 1 1 d . . . C33 C 0.6541(3) 0.6875(3) 0.9749(3) 0.0545(10) Uani 1 1 d . . . H33 H 0.5867 0.7185 0.9521 0.065 Uiso 1 1 calc R . . C34 C 0.6717(4) 0.6896(3) 1.0558(3) 0.0630(12) Uani 1 1 d . . . H34 H 0.6164 0.7214 1.0871 0.076 Uiso 1 1 calc R . . C35 C 0.7721(4) 0.6442(3) 1.0903(3) 0.0615(12) Uani 1 1 d . . . H35 H 0.7851 0.6460 1.1442 0.074 Uiso 1 1 calc R . . C36 C 0.8520(4) 0.5966(3) 1.0434(3) 0.0606(11) Uani 1 1 d . . . H36 H 0.9192 0.5654 1.0663 0.073 Uiso 1 1 calc R . . C37 C 0.8341(3) 0.5944(3) 0.9630(3) 0.0500(10) Uani 1 1 d . . . H37 H 0.8894 0.5618 0.9324 0.060 Uiso 1 1 calc R . . C38 C 0.8340(3) 0.5681(3) 0.7860(3) 0.0400(8) Uani 1 1 d . . . C39 C 0.8523(4) 0.4731(3) 0.8011(3) 0.0587(11) Uani 1 1 d . . . H39 H 0.7959 0.4369 0.8352 0.070 Uiso 1 1 calc R . . C40 C 0.9533(4) 0.4318(4) 0.7661(4) 0.0761(15) Uani 1 1 d . . . H40 H 0.9642 0.3680 0.7768 0.091 Uiso 1 1 calc R . . C41 C 1.0367(4) 0.4833(4) 0.7162(4) 0.0743(15) Uani 1 1 d . . . H41 H 1.1043 0.4547 0.6927 0.089 Uiso 1 1 calc R . . C42 C 1.0218(3) 0.5784(4) 0.7001(3) 0.0644(12) Uani 1 1 d . . . H42 H 1.0793 0.6137 0.6666 0.077 Uiso 1 1 calc R . . C43 C 0.9194(3) 0.6201(3) 0.7348(3) 0.0503(10) Uani 1 1 d . . . H43 H 0.9083 0.6841 0.7233 0.060 Uiso 1 1 calc R . . C44 C 0.7514(3) 0.6202(3) 0.5926(3) 0.0423(9) Uani 1 1 d . . . C45 C 0.8207(4) 0.5647(4) 0.5408(4) 0.0754(15) Uani 1 1 d . . . H45A H 0.7898 0.5794 0.4861 0.113 Uiso 1 1 calc R . . H45B H 0.8213 0.4992 0.5770 0.113 Uiso 1 1 calc R . . H45C H 0.8966 0.5788 0.5252 0.113 Uiso 1 1 calc R . . C46 C 0.4657(4) 0.8658(3) 0.8180(3) 0.0535(10) Uani 1 1 d . . . C47 C 0.3949(5) 0.9164(4) 0.8744(4) 0.0859(17) Uani 1 1 d . . . H47A H 0.3361 0.8810 0.9131 0.129 Uiso 1 1 calc R . . H47B H 0.3615 0.9766 0.8359 0.129 Uiso 1 1 calc R . . H47C H 0.4405 0.9247 0.9113 0.129 Uiso 1 1 calc R . . C48 C 0.3666(6) 0.7308(6) 0.1706(7) 0.117(3) Uani 1 1 d . . . C49 C 0.3656(7) 0.7053(9) 0.2640(7) 0.190(5) Uani 1 1 d . . . H49A H 0.3005 0.6755 0.2971 0.285 Uiso 1 1 calc R . . H49B H 0.3625 0.7603 0.2773 0.285 Uiso 1 1 calc R . . H49C H 0.4331 0.6626 0.2819 0.285 Uiso 1 1 calc R . . F1 F 0.6530(4) 0.7471(2) 0.3716(2) 0.1099(12) Uani 1 1 d . . . F2 F 0.7958(3) 0.7327(3) 0.2633(3) 0.1292(14) Uani 1 1 d . . . F3 F 0.7316(3) 0.8732(2) 0.2783(2) 0.0923(9) Uani 1 1 d . . . F4 F 0.6234(4) 0.7209(3) 0.2513(3) 0.1128(12) Uani 1 1 d . . . F5 F 0.5584(3) 0.8603(3) 0.2674(3) 0.1088(11) Uani 1 1 d . . . F6 F 0.7009(4) 0.8478(3) 0.1588(2) 0.1314(15) Uani 1 1 d . . . F7 F -0.0019(6) 0.8698(4) 0.3756(4) 0.212(3) Uani 1 1 d . . . F8 F -0.0371(4) 0.7415(5) 0.4560(9) 0.318(6) Uani 1 1 d . . . F9 F 0.1384(6) 0.6781(5) 0.4587(5) 0.245(4) Uani 1 1 d . . . F10 F 0.0960(6) 0.7530(6) 0.3316(4) 0.242(4) Uani 1 1 d . . . F11 F 0.1787(6) 0.8114(7) 0.3880(8) 0.307(6) Uani 1 1 d . . . F12 F 0.0524(8) 0.7988(8) 0.4984(6) 0.312(6) Uani 1 1 d . . . N1 N 0.8378(3) 0.8358(3) 0.8203(2) 0.0596(9) Uani 1 1 d . . . N2 N 0.7767(2) 0.8899(2) 0.6795(2) 0.0376(7) Uani 1 1 d . . . N3 N 0.7673(2) 0.87207(19) 0.55753(19) 0.0343(6) Uani 1 1 d . . . N4 N 0.6019(2) 0.86927(18) 0.50460(19) 0.0322(6) Uani 1 1 d . . . N5 N 0.4294(2) 0.87226(18) 0.56541(19) 0.0335(6) Uani 1 1 d . . . N6 N 0.3044(3) 0.9061(2) 0.6845(2) 0.0519(8) Uani 1 1 d . . . N7 N 0.5202(2) 0.8235(2) 0.7761(2) 0.0385(7) Uani 1 1 d . . . N8 N 0.6991(2) 0.6670(2) 0.62995(19) 0.0344(6) Uani 1 1 d . . . N9 N 0.3715(8) 0.7434(8) 0.0979(7) 0.197(4) Uani 1 1 d . . . P1 P 0.70102(7) 0.62909(6) 0.82704(6) 0.0346(2) Uani 1 1 d . . . P2 P 0.47775(7) 0.63772(6) 0.75070(6) 0.0361(2) Uani 1 1 d . . . P3 P 0.67871(13) 0.79677(9) 0.26443(9) 0.0687(4) Uani 1 1 d . . . P4 P 0.06921(12) 0.77287(12) 0.41625(11) 0.0827(4) Uani 1 1 d . . . Ru1 Ru 0.60870(2) 0.746153(18) 0.702951(18) 0.03022(10) Uani 1 1 d . . . C50 C 0.0506(12) 0.8843(9) 0.0652(14) 0.209(6) Uani 1 1 d . . . C51 C -0.0017(11) 0.8947(12) 0.1437(7) 0.232(7) Uani 1 1 d . . . H51A H 0.0537 0.8856 0.1816 0.349 Uiso 1 1 calc R . . H51B H -0.0523 0.8493 0.1749 0.349 Uiso 1 1 calc R . . H51C H -0.0439 0.9567 0.1308 0.349 Uiso 1 1 calc R . . N10 N 0.0979(15) 0.8938(13) -0.0130(15) 0.368(12) 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 0.088(4) 0.108(5) 0.048(3) -0.012(3) -0.021(3) -0.034(3) C2 0.133(6) 0.127(6) 0.066(4) -0.050(4) -0.005(4) -0.059(5) C3 0.134(6) 0.106(5) 0.098(5) -0.070(4) -0.007(4) -0.003(4) C4 0.089(4) 0.084(4) 0.081(4) -0.049(3) -0.024(3) 0.012(3) C5 0.043(2) 0.047(2) 0.048(2) -0.0157(19) -0.0088(17) -0.0140(17) C6 0.0275(15) 0.0295(17) 0.0314(19) -0.0056(15) -0.0075(13) 0.0033(13) C7 0.0340(18) 0.044(2) 0.058(3) -0.0111(19) -0.0065(17) -0.0152(16) C8 0.0296(17) 0.039(2) 0.048(2) -0.0040(18) -0.0014(15) -0.0082(15) C9 0.0373(17) 0.0373(19) 0.0293(19) -0.0069(15) 0.0017(14) -0.0057(15) C10 0.0321(16) 0.0257(16) 0.0316(18) -0.0102(14) -0.0013(13) -0.0076(13) C11 0.0429(19) 0.038(2) 0.037(2) -0.0101(17) -0.0167(16) 0.0014(15) C12 0.046(2) 0.039(2) 0.0251(19) -0.0071(16) -0.0084(15) -0.0024(16) C13 0.0293(17) 0.0318(19) 0.047(2) -0.0022(17) -0.0064(15) -0.0002(14) C14 0.044(2) 0.041(2) 0.069(3) -0.002(2) -0.0152(19) -0.0086(17) C15 0.040(2) 0.057(3) 0.101(4) 0.005(3) -0.016(2) -0.015(2) C16 0.039(2) 0.076(4) 0.084(4) 0.004(3) 0.008(2) -0.004(2) C17 0.049(3) 0.088(4) 0.062(3) -0.021(3) 0.011(2) 0.004(2) C18 0.0351(18) 0.0341(19) 0.052(2) -0.0145(18) -0.0084(16) -0.0028(15) C19 0.050(2) 0.040(2) 0.058(3) -0.019(2) -0.0111(18) -0.0068(17) C20 0.073(3) 0.060(3) 0.061(3) -0.027(2) -0.018(2) -0.011(2) C21 0.071(3) 0.074(3) 0.097(4) -0.049(3) -0.022(3) -0.015(3) C22 0.063(3) 0.056(3) 0.104(4) -0.040(3) -0.012(3) -0.020(2) C23 0.053(2) 0.046(2) 0.071(3) -0.018(2) -0.004(2) -0.0163(19) C24 0.0369(18) 0.0329(19) 0.042(2) -0.0013(16) -0.0008(15) -0.0064(15) C25 0.040(2) 0.051(2) 0.058(3) -0.011(2) -0.0015(18) -0.0120(18) C26 0.039(2) 0.067(3) 0.078(4) -0.018(3) 0.000(2) -0.012(2) C27 0.046(2) 0.055(3) 0.064(3) -0.002(2) 0.011(2) -0.004(2) C28 0.062(3) 0.050(2) 0.042(2) -0.004(2) 0.0025(19) 0.000(2) C29 0.045(2) 0.044(2) 0.045(2) -0.0028(19) -0.0072(17) -0.0050(17) C30 0.0416(19) 0.0276(18) 0.055(2) -0.0006(17) -0.0075(17) -0.0083(15) C31 0.0425(19) 0.0337(19) 0.040(2) 0.0038(16) -0.0060(16) -0.0055(15) C32 0.0404(19) 0.040(2) 0.034(2) -0.0069(16) -0.0048(15) -0.0054(16) C33 0.046(2) 0.066(3) 0.047(3) -0.022(2) -0.0098(18) 0.0050(19) C34 0.061(3) 0.077(3) 0.051(3) -0.032(3) -0.001(2) -0.001(2) C35 0.070(3) 0.076(3) 0.043(3) -0.022(2) -0.015(2) -0.012(2) C36 0.057(2) 0.070(3) 0.051(3) -0.016(2) -0.021(2) 0.001(2) C37 0.046(2) 0.055(2) 0.046(2) -0.018(2) -0.0115(17) 0.0036(18) C38 0.0372(18) 0.041(2) 0.038(2) -0.0122(17) -0.0089(15) 0.0013(15) C39 0.056(2) 0.048(3) 0.064(3) -0.018(2) -0.009(2) 0.004(2) C40 0.072(3) 0.060(3) 0.090(4) -0.035(3) -0.013(3) 0.018(3) C41 0.054(3) 0.093(4) 0.071(3) -0.042(3) -0.010(2) 0.021(3) C42 0.039(2) 0.083(4) 0.062(3) -0.024(3) -0.0010(19) -0.001(2) C43 0.042(2) 0.050(2) 0.049(2) -0.012(2) -0.0043(17) -0.0015(17) C44 0.044(2) 0.040(2) 0.046(2) -0.0182(19) -0.0088(17) -0.0041(17) C45 0.071(3) 0.084(4) 0.089(4) -0.061(3) -0.001(3) -0.002(3) C46 0.067(3) 0.037(2) 0.041(2) -0.0068(19) -0.003(2) 0.0020(19) C47 0.108(4) 0.070(3) 0.069(4) -0.038(3) 0.007(3) 0.013(3) C48 0.084(4) 0.157(7) 0.115(7) -0.053(6) -0.038(4) 0.004(4) C49 0.104(6) 0.344(16) 0.140(8) -0.136(10) -0.007(5) 0.010(8) F1 0.173(3) 0.090(2) 0.059(2) -0.0181(18) -0.008(2) -0.031(2) F2 0.119(3) 0.103(3) 0.173(4) -0.080(3) -0.021(3) 0.027(2) F3 0.108(2) 0.088(2) 0.098(2) -0.053(2) 0.0003(18) -0.0274(18) F4 0.163(3) 0.091(2) 0.110(3) -0.055(2) -0.019(2) -0.037(2) F5 0.102(2) 0.115(3) 0.128(3) -0.071(3) -0.033(2) 0.013(2) F6 0.230(5) 0.106(3) 0.052(2) -0.028(2) 0.004(2) -0.039(3) F7 0.252(6) 0.155(5) 0.126(4) -0.022(4) 0.010(4) 0.082(5) F8 0.080(3) 0.163(6) 0.606(17) -0.091(8) 0.075(6) -0.029(3) F9 0.207(6) 0.210(7) 0.195(6) -0.034(5) -0.022(5) 0.126(6) F10 0.237(6) 0.350(9) 0.184(6) -0.197(7) -0.096(5) 0.116(7) F11 0.166(6) 0.318(11) 0.533(16) -0.288(12) 0.084(8) -0.104(6) F12 0.273(9) 0.482(15) 0.216(7) -0.247(10) -0.097(7) 0.164(10) N1 0.058(2) 0.066(2) 0.047(2) -0.0076(19) -0.0119(17) -0.0151(18) N2 0.0344(14) 0.0366(16) 0.0420(18) -0.0118(14) -0.0085(12) -0.0076(12) N3 0.0305(14) 0.0331(15) 0.0337(17) -0.0062(13) -0.0039(12) -0.0059(12) N4 0.0319(14) 0.0296(15) 0.0313(16) -0.0087(12) -0.0049(11) -0.0013(11) N5 0.0320(14) 0.0282(14) 0.0356(17) -0.0063(13) -0.0059(12) -0.0038(11) N6 0.0424(17) 0.055(2) 0.048(2) -0.0153(17) 0.0038(15) -0.0032(15) N7 0.0429(16) 0.0313(16) 0.0321(17) -0.0045(14) -0.0043(13) -0.0019(13) N8 0.0345(14) 0.0323(15) 0.0328(16) -0.0059(13) -0.0075(12) -0.0063(12) N9 0.180(8) 0.277(12) 0.134(7) -0.060(8) -0.075(7) -0.011(7) P1 0.0324(4) 0.0317(5) 0.0314(5) -0.0041(4) -0.0042(4) -0.0028(4) P2 0.0330(4) 0.0293(5) 0.0388(5) -0.0042(4) -0.0041(4) -0.0072(4) P3 0.0998(10) 0.0551(7) 0.0537(8) -0.0273(6) -0.0040(7) -0.0094(7) P4 0.0599(8) 0.1014(12) 0.0830(11) -0.0427(9) -0.0010(7) 0.0035(8) Ru1 0.02981(15) 0.02601(16) 0.02907(17) -0.00472(11) -0.00287(11) -0.00422(10) C50 0.188(12) 0.139(9) 0.253(17) -0.070(11) -0.050(12) 0.084(9) C51 0.209(13) 0.319(19) 0.102(8) -0.018(10) 0.019(8) -0.060(12) N10 0.310(18) 0.35(2) 0.46(3) -0.28(2) 0.046(18) 0.076(15) _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 N1 1.343(6) . ? C1 C2 1.342(9) . ? C2 C3 1.363(9) . ? C3 C4 1.389(8) . ? C4 C5 1.369(6) . ? C5 N1 1.311(5) . ? C5 N2 1.433(5) . ? C6 N2 1.361(4) . ? C6 N3 1.361(4) . ? C6 Ru1 2.112(3) . ? C7 C8 1.317(5) . ? C7 N2 1.396(5) . ? C8 N3 1.384(4) . ? C9 N3 1.454(4) . ? C9 N4 1.460(4) . ? C10 N5 1.360(4) . ? C10 N4 1.363(4) . ? C10 Ru1 2.097(3) . ? C11 C12 1.325(5) . ? C11 N5 1.384(4) . ? C12 N4 1.374(4) . ? C13 N6 1.316(5) . ? C13 C14 1.377(5) . ? C13 N5 1.445(4) . ? C14 C15 1.392(6) . ? C15 C16 1.356(8) . ? C16 C17 1.365(8) . ? C17 N6 1.352(5) . ? C18 C19 1.387(6) . ? C18 C23 1.386(5) . ? C18 P2 1.836(4) . ? C19 C20 1.378(6) . ? C20 C21 1.372(6) . ? C21 C22 1.367(7) . ? C22 C23 1.392(7) . ? C24 C25 1.382(5) . ? C24 C29 1.396(6) . ? C24 P2 1.844(4) . ? C25 C26 1.388(6) . ? C26 C27 1.378(7) . ? C27 C28 1.360(7) . ? C28 C29 1.388(6) . ? C30 C31 1.506(5) . ? C30 P2 1.851(4) . ? C31 P1 1.844(4) . ? C32 C33 1.383(5) . ? C32 C37 1.388(5) . ? C32 P1 1.832(4) . ? C33 C34 1.384(6) . ? C34 C35 1.387(6) . ? C35 C36 1.375(6) . ? C36 C37 1.376(6) . ? C38 C43 1.382(5) . ? C38 C39 1.386(5) . ? C38 P1 1.829(3) . ? C39 C40 1.377(6) . ? C40 C41 1.355(7) . ? C41 C42 1.387(7) . ? C42 C43 1.390(6) . ? C44 N8 1.134(4) . ? C44 C45 1.455(6) . ? C46 N7 1.141(5) . ? C46 C47 1.461(6) . ? C48 N9 1.100(10) . ? C48 C49 1.397(11) . ? F1 P3 1.583(3) . ? F2 P3 1.560(4) . ? F3 P3 1.589(3) . ? F4 P3 1.593(3) . ? F5 P3 1.589(4) . ? F6 P3 1.562(4) . ? F7 P4 1.542(5) . ? F8 P4 1.420(5) . ? F9 P4 1.513(5) . ? F10 P4 1.472(5) . ? F11 P4 1.498(7) . ? F12 P4 1.495(7) . ? N7 Ru1 2.009(3) . ? N8 Ru1 2.034(3) . ? P1 Ru1 2.4131(9) . ? P2 Ru1 2.3853(9) . ? C50 N10 1.23(2) . ? C50 C51 1.344(17) . ? 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 N1 C1 C2 124.2(6) . . ? C1 C2 C3 119.2(6) . . ? C2 C3 C4 118.6(6) . . ? C5 C4 C3 117.2(5) . . ? N1 C5 C4 125.1(4) . . ? N1 C5 N2 115.3(3) . . ? C4 C5 N2 119.2(4) . . ? N2 C6 N3 102.6(3) . . ? N2 C6 Ru1 136.7(2) . . ? N3 C6 Ru1 120.5(2) . . ? C8 C7 N2 107.1(3) . . ? C7 C8 N3 106.7(3) . . ? N3 C9 N4 109.3(3) . . ? N5 C10 N4 102.6(3) . . ? N5 C10 Ru1 136.7(2) . . ? N4 C10 Ru1 120.4(2) . . ? C12 C11 N5 107.4(3) . . ? C11 C12 N4 106.3(3) . . ? N6 C13 C14 125.4(4) . . ? N6 C13 N5 116.1(3) . . ? C14 C13 N5 118.1(4) . . ? C13 C14 C15 117.0(5) . . ? C16 C15 C14 119.2(5) . . ? C15 C16 C17 119.1(4) . . ? N6 C17 C16 123.8(5) . . ? C19 C18 C23 118.0(4) . . ? C19 C18 P2 121.1(3) . . ? C23 C18 P2 120.8(3) . . ? C20 C19 C18 121.6(4) . . ? C21 C20 C19 119.1(5) . . ? C22 C21 C20 121.0(5) . . ? C21 C22 C23 119.6(4) . . ? C18 C23 C22 120.6(4) . . ? C25 C24 C29 118.5(3) . . ? C25 C24 P2 123.7(3) . . ? C29 C24 P2 117.8(3) . . ? C24 C25 C26 120.5(4) . . ? C27 C26 C25 120.1(4) . . ? C28 C27 C26 120.3(4) . . ? C27 C28 C29 120.2(5) . . ? C28 C29 C24 120.5(4) . . ? C31 C30 P2 110.2(3) . . ? C30 C31 P1 111.8(3) . . ? C33 C32 C37 118.1(4) . . ? C33 C32 P1 119.4(3) . . ? C37 C32 P1 122.1(3) . . ? C34 C33 C32 121.2(4) . . ? C33 C34 C35 120.0(4) . . ? C36 C35 C34 118.9(4) . . ? C37 C36 C35 121.0(4) . . ? C36 C37 C32 120.7(4) . . ? C43 C38 C39 118.2(4) . . ? C43 C38 P1 118.3(3) . . ? C39 C38 P1 123.5(3) . . ? C40 C39 C38 120.7(4) . . ? C41 C40 C39 120.6(5) . . ? C40 C41 C42 120.3(4) . . ? C41 C42 C43 118.9(4) . . ? C38 C43 C42 121.2(4) . . ? N8 C44 C45 177.0(4) . . ? N7 C46 C47 177.7(5) . . ? N9 C48 C49 174.1(12) . . ? C5 N1 C1 115.8(4) . . ? C6 N2 C7 111.4(3) . . ? C6 N2 C5 130.0(3) . . ? C7 N2 C5 118.5(3) . . ? C6 N3 C8 112.2(3) . . ? C6 N3 C9 124.7(3) . . ? C8 N3 C9 122.2(3) . . ? C10 N4 C12 112.4(3) . . ? C10 N4 C9 125.1(3) . . ? C12 N4 C9 122.5(3) . . ? C10 N5 C11 111.3(3) . . ? C10 N5 C13 129.6(3) . . ? C11 N5 C13 119.1(3) . . ? C13 N6 C17 115.5(4) . . ? C46 N7 Ru1 176.9(3) . . ? C44 N8 Ru1 177.0(3) . . ? C38 P1 C32 102.66(16) . . ? C38 P1 C31 104.99(17) . . ? C32 P1 C31 97.83(17) . . ? C38 P1 Ru1 111.83(12) . . ? C32 P1 Ru1 129.30(12) . . ? C31 P1 Ru1 107.32(12) . . ? C18 P2 C24 104.56(17) . . ? C18 P2 C30 100.81(17) . . ? C24 P2 C30 102.18(17) . . ? C18 P2 Ru1 118.76(12) . . ? C24 P2 Ru1 120.65(12) . . ? C30 P2 Ru1 106.88(12) . . ? F2 P3 F6 91.3(3) . . ? F2 P3 F1 90.4(2) . . ? F6 P3 F1 178.4(3) . . ? F2 P3 F3 91.7(2) . . ? F6 P3 F3 90.5(2) . . ? F1 P3 F3 89.26(19) . . ? F2 P3 F5 178.8(3) . . ? F6 P3 F5 89.8(2) . . ? F1 P3 F5 88.6(2) . . ? F3 P3 F5 88.82(19) . . ? F2 P3 F4 89.2(2) . . ? F6 P3 F4 89.9(2) . . ? F1 P3 F4 90.3(2) . . ? F3 P3 F4 178.9(2) . . ? F5 P3 F4 90.2(2) . . ? F8 P4 F10 103.2(7) . . ? F8 P4 F12 82.8(6) . . ? F10 P4 F12 173.9(6) . . ? F8 P4 F11 170.1(7) . . ? F10 P4 F11 86.7(5) . . ? F12 P4 F11 87.2(6) . . ? F8 P4 F9 94.8(5) . . ? F10 P4 F9 86.0(4) . . ? F12 P4 F9 94.6(5) . . ? F11 P4 F9 86.4(5) . . ? F8 P4 F7 84.8(4) . . ? F10 P4 F7 95.6(4) . . ? F12 P4 F7 83.7(4) . . ? F11 P4 F7 93.7(5) . . ? F9 P4 F7 178.3(4) . . ? N7 Ru1 N8 179.42(12) . . ? N7 Ru1 C10 91.34(12) . . ? N8 Ru1 C10 89.24(11) . . ? N7 Ru1 C6 89.04(12) . . ? N8 Ru1 C6 91.02(12) . . ? C10 Ru1 C6 81.83(12) . . ? N7 Ru1 P2 95.50(9) . . ? N8 Ru1 P2 84.47(8) . . ? C10 Ru1 P2 94.92(8) . . ? C6 Ru1 P2 174.49(9) . . ? N7 Ru1 P1 95.03(8) . . ? N8 Ru1 P1 84.39(8) . . ? C10 Ru1 P1 173.53(9) . . ? C6 Ru1 P1 99.41(9) . . ? P2 Ru1 P1 83.32(3) . . ? N10 C50 C51 167.2(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.004 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.072 #===END data_complex_8 _database_code_depnum_ccdc_archive 'CCDC 834950' #TrackingRef '- cif-Rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H36 F12 N12 P2 Ru' _chemical_formula_weight 895.67 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0111(5) _cell_length_b 12.4027(4) _cell_length_c 13.1637(4) _cell_angle_alpha 90.600(3) _cell_angle_beta 93.233(3) _cell_angle_gamma 113.242(4) _cell_volume 1797.84(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7533 _exptl_absorpt_correction_T_max 0.7970 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12177 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6342 _reflns_number_gt 5396 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. The restraints which are DFIX C22 C23 1.4 0.01, DFIX N10 C20 1.2 0.01 and DFIX N11 C23 1.5 0.01 have been used to DFIX the C-C or C-N bond distances. ; _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^)+(0.0737P)^2^+2.5350P] 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 6342 _refine_ls_number_parameters 471 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.006 _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 0.96223(3) 0.71515(3) 0.72815(2) 0.03711(14) Uani 1 1 d . . . C1 C 1.0785(5) 0.7886(4) 0.5205(4) 0.0531(12) Uani 1 1 d . . . H1 H 1.1393 0.8512 0.5563 0.064 Uiso 1 1 calc R . . C2 C 1.0789(6) 0.7838(6) 0.4167(4) 0.0668(16) Uani 1 1 d . . . H2 H 1.1387 0.8423 0.3833 0.080 Uiso 1 1 calc R . . C3 C 0.9912(7) 0.6930(6) 0.3627(4) 0.0784(19) Uani 1 1 d . . . H3 H 0.9904 0.6888 0.2920 0.094 Uiso 1 1 calc R . . C4 C 0.9038(7) 0.6076(6) 0.4132(4) 0.0757(18) Uani 1 1 d . . . H4 H 0.8427 0.5448 0.3778 0.091 Uiso 1 1 calc R . . C5 C 0.9092(5) 0.6175(5) 0.5180(4) 0.0530(12) Uani 1 1 d . . . C6 C 0.8437(4) 0.5639(4) 0.6813(3) 0.0436(10) Uani 1 1 d . . . C7 C 0.7688(6) 0.4127(5) 0.5637(5) 0.0718(16) Uani 1 1 d . . . H7 H 0.7477 0.3716 0.5013 0.086 Uiso 1 1 calc R . . C8 C 0.7488(5) 0.3671(5) 0.6548(5) 0.0672(15) Uani 1 1 d . . . H8 H 0.7118 0.2876 0.6678 0.081 Uiso 1 1 calc R . . C9 C 0.8395(4) 0.4562(4) 0.8318(4) 0.0483(11) Uani 1 1 d . . . H9A H 0.8109 0.3756 0.8531 0.058 Uiso 1 1 calc R . . H9B H 0.8106 0.4999 0.8775 0.058 Uiso 1 1 calc R . . C10 C 1.0384(4) 0.6111(4) 0.7911(3) 0.0366(9) Uani 1 1 d . . . C11 C 1.0465(5) 0.4615(4) 0.8854(4) 0.0494(11) Uani 1 1 d . . . H11 H 1.0215 0.3930 0.9218 0.059 Uiso 1 1 calc R . . C12 C 1.1602(5) 0.5327(4) 0.8713(4) 0.0506(12) Uani 1 1 d . . . H12 H 1.2300 0.5238 0.8961 0.061 Uiso 1 1 calc R . . C13 C 1.2616(4) 0.7169(4) 0.7791(3) 0.0397(10) Uani 1 1 d . . . C14 C 1.3470(5) 0.7865(5) 0.8514(4) 0.0632(14) Uani 1 1 d . . . H14 H 1.3358 0.7761 0.9205 0.076 Uiso 1 1 calc R . . C15 C 1.4496(6) 0.8720(6) 0.8178(6) 0.085(2) Uani 1 1 d . . . H15 H 1.5100 0.9211 0.8643 0.102 Uiso 1 1 calc R . . C16 C 1.4627(5) 0.8849(6) 0.7159(5) 0.0775(18) Uani 1 1 d . . . H16 H 1.5329 0.9404 0.6916 0.093 Uiso 1 1 calc R . . C17 C 1.3703(6) 0.8142(6) 0.6511(5) 0.0741(17) Uani 1 1 d . . . H17 H 1.3770 0.8264 0.5817 0.089 Uiso 1 1 calc R . . C18 C 1.0629(5) 0.9798(4) 0.7696(4) 0.0599(14) Uani 1 1 d . . . H18A H 1.0218 0.9787 0.8312 0.072 Uiso 1 1 calc R . . H18B H 1.1287 1.0564 0.7662 0.072 Uiso 1 1 calc R . . C19 C 0.9760(6) 0.9582(5) 0.6789(4) 0.0628(14) Uani 1 1 d . . . H19A H 0.9392 1.0152 0.6794 0.075 Uiso 1 1 calc R . . H19B H 1.0188 0.9669 0.6172 0.075 Uiso 1 1 calc R . . C20 C 0.8000(9) 0.7135(6) 0.8998(6) 0.109(3) Uani 1 1 d D . . C21 C 0.7776(8) 0.7445(6) 1.0088(6) 0.098(3) Uani 1 1 d . . . H21A H 0.8466 0.7535 1.0539 0.147 Uiso 1 1 calc R . . H21B H 0.7067 0.6827 1.0315 0.147 Uiso 1 1 calc R . . H21C H 0.7656 0.8166 1.0086 0.147 Uiso 1 1 calc R . . C22 C 0.5697(9) 0.6273(12) 0.8239(13) 0.168(5) Uani 1 1 d D . . H22A H 0.5463 0.5946 0.8899 0.202 Uiso 1 1 calc R . . H22B H 0.5588 0.7008 0.8242 0.202 Uiso 1 1 calc R . . C23 C 0.4746(17) 0.552(2) 0.7542(11) 0.37(2) Uani 1 1 d D . . H23A H 0.4154 0.5858 0.7388 0.439 Uiso 1 1 calc R . . H23B H 0.4337 0.4757 0.7826 0.439 Uiso 1 1 calc R . . C24 C 0.5307(10) 0.2868(15) 0.9063(9) 0.121(4) Uani 1 1 d . . . C25 C 0.4614(12) 0.1710(15) 0.8609(9) 0.172(5) Uani 1 1 d . . . H25A H 0.4460 0.1136 0.9125 0.258 Uiso 1 1 calc R . . H25B H 0.5066 0.1544 0.8095 0.258 Uiso 1 1 calc R . . H25C H 0.3856 0.1681 0.8307 0.258 Uiso 1 1 calc R . . F1 F 0.3029(5) 0.9640(4) 0.0293(4) 0.146(2) Uani 1 1 d . . . F2 F 0.2672(6) 0.8563(5) 0.1630(5) 0.159(3) Uani 1 1 d . . . F3 F 0.2308(4) 1.0178(3) 0.1620(3) 0.0953(12) Uani 1 1 d . . . F4 F 0.1124(5) 0.9487(4) 0.0210(4) 0.140(2) Uani 1 1 d . . . F5 F 0.1498(3) 0.7875(3) 0.0204(3) 0.0822(10) Uani 1 1 d . . . F6 F 0.0778(5) 0.8411(4) 0.1548(4) 0.1238(18) Uani 1 1 d . . . F7 F 0.6770(9) 0.9278(11) 0.5302(6) 0.245(5) Uani 1 1 d . . . F8 F 0.5274(6) 0.8299(11) 0.4225(7) 0.245(5) Uani 1 1 d . . . F9 F 0.6979(4) 0.9437(4) 0.3643(4) 0.1204(16) Uani 1 1 d . . . F10 F 0.6448(14) 0.7587(7) 0.3524(7) 0.280(7) Uani 1 1 d . . . F11 F 0.7967(6) 0.8654(9) 0.4614(5) 0.199(4) Uani 1 1 d . . . F12 F 0.6273(10) 0.7502(10) 0.5190(8) 0.319(8) Uani 1 1 d . . . N1 N 0.9949(4) 0.7076(3) 0.5734(3) 0.0438(9) Uani 1 1 d . . . N2 N 0.8275(4) 0.5341(4) 0.5792(3) 0.0528(10) Uani 1 1 d . . . N3 N 0.7933(3) 0.4597(3) 0.7283(3) 0.0489(9) Uani 1 1 d . . . N4 N 0.9728(3) 0.5081(3) 0.8360(3) 0.0410(8) Uani 1 1 d . . . N7 N 1.1123(4) 0.8869(3) 0.7717(3) 0.0473(9) Uani 1 1 d . . . H7A H 1.1445 0.8842 0.8346 0.057 Uiso 1 1 calc R . . H7B H 1.1712 0.9031 0.7279 0.057 Uiso 1 1 calc R . . N5 N 1.1551(3) 0.6235(3) 0.8122(3) 0.0395(8) Uani 1 1 d . . . N8 N 0.8803(4) 0.8377(4) 0.6808(3) 0.0529(10) Uani 1 1 d . . . H8A H 0.8423 0.8158 0.6185 0.063 Uiso 1 1 calc R . . H8B H 0.8248 0.8364 0.7246 0.063 Uiso 1 1 calc R . . N6 N 1.2690(4) 0.7271(4) 0.6809(3) 0.0608(12) Uani 1 1 d . . . N10 N 0.7029(7) 0.6638(8) 0.8290(7) 0.134(3) Uani 1 1 d D . . H10 H 0.7266 0.6501 0.7716 0.160 Uiso 1 1 calc R . . N11 N 0.5330(10) 0.5420(10) 0.6631(10) 0.188(4) Uani 1 1 d D . . H11A H 0.6103 0.5782 0.6607 0.226 Uiso 1 1 calc R . . H11B H 0.4903 0.4997 0.6116 0.226 Uiso 1 1 calc R . . N9 N 0.9016(4) 0.7290(3) 0.8698(3) 0.0452(9) Uani 1 1 d . . . H9 H 0.9582 0.7497 0.9179 0.054 Uiso 1 1 calc R . . N12 N 0.5884(9) 0.3796(12) 0.9468(9) 0.153(4) Uani 1 1 d . . . P1 P 0.19110(12) 0.90348(11) 0.09248(10) 0.0504(3) Uani 1 1 d . . . P2 P 0.6596(2) 0.8433(2) 0.44142(17) 0.1103(9) 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 0.0408(2) 0.0361(2) 0.0340(2) 0.00022(14) 0.00264(14) 0.01471(16) C1 0.068(3) 0.051(3) 0.047(3) 0.007(2) 0.012(2) 0.030(3) C2 0.097(5) 0.073(4) 0.047(3) 0.013(3) 0.024(3) 0.049(4) C3 0.117(6) 0.093(5) 0.039(3) 0.004(3) 0.013(3) 0.054(5) C4 0.100(5) 0.081(4) 0.047(3) -0.018(3) -0.014(3) 0.040(4) C5 0.068(3) 0.063(3) 0.039(3) -0.002(2) -0.003(2) 0.038(3) C6 0.040(2) 0.048(3) 0.043(3) 0.000(2) -0.0029(19) 0.018(2) C7 0.075(4) 0.058(3) 0.068(4) -0.020(3) -0.018(3) 0.014(3) C8 0.058(3) 0.045(3) 0.086(4) -0.012(3) -0.008(3) 0.008(3) C9 0.041(3) 0.041(2) 0.053(3) 0.009(2) 0.007(2) 0.005(2) C10 0.040(2) 0.036(2) 0.032(2) -0.0012(17) 0.0043(17) 0.0123(19) C11 0.059(3) 0.042(2) 0.046(3) 0.011(2) 0.001(2) 0.017(2) C12 0.051(3) 0.055(3) 0.050(3) 0.010(2) -0.003(2) 0.027(2) C13 0.034(2) 0.040(2) 0.045(3) -0.0017(19) 0.0036(18) 0.0140(19) C14 0.049(3) 0.072(4) 0.054(3) -0.007(3) -0.002(2) 0.009(3) C15 0.049(3) 0.084(5) 0.089(5) -0.012(4) -0.005(3) -0.008(3) C16 0.049(3) 0.068(4) 0.093(5) 0.003(3) 0.016(3) -0.003(3) C17 0.069(4) 0.076(4) 0.057(3) 0.011(3) 0.018(3) 0.005(3) C18 0.076(4) 0.040(3) 0.066(3) 0.001(2) 0.014(3) 0.024(3) C19 0.087(4) 0.053(3) 0.064(3) 0.013(3) 0.014(3) 0.043(3) C20 0.157(8) 0.074(5) 0.131(7) 0.045(5) 0.099(7) 0.070(5) C21 0.131(7) 0.089(5) 0.097(5) 0.021(4) 0.070(5) 0.060(5) C22 0.098(8) 0.178(12) 0.257(16) 0.026(11) 0.057(9) 0.078(8) C23 0.52(4) 0.57(5) 0.152(15) -0.16(2) -0.12(2) 0.40(4) C24 0.081(7) 0.205(14) 0.095(7) 0.046(8) 0.021(5) 0.073(8) C25 0.140(10) 0.249(17) 0.122(9) -0.021(10) 0.006(8) 0.073(12) F1 0.116(4) 0.117(4) 0.141(4) -0.041(3) 0.076(3) -0.032(3) F2 0.188(6) 0.132(4) 0.177(5) -0.014(4) -0.087(5) 0.099(4) F3 0.101(3) 0.074(2) 0.095(3) -0.033(2) 0.004(2) 0.019(2) F4 0.175(5) 0.103(3) 0.137(4) -0.001(3) -0.074(4) 0.061(4) F5 0.080(2) 0.062(2) 0.086(2) -0.0206(18) 0.0194(19) 0.0074(18) F6 0.122(4) 0.097(3) 0.118(4) -0.011(3) 0.068(3) 0.000(3) F7 0.214(8) 0.364(14) 0.133(6) -0.086(8) 0.011(5) 0.093(9) F8 0.081(4) 0.350(13) 0.209(8) 0.090(8) -0.004(4) -0.016(6) F9 0.107(3) 0.117(4) 0.121(4) 0.045(3) 0.021(3) 0.025(3) F10 0.502(19) 0.133(6) 0.184(8) -0.041(6) -0.100(10) 0.120(9) F11 0.145(5) 0.327(11) 0.133(5) 0.086(6) 0.000(4) 0.100(6) F12 0.303(12) 0.268(11) 0.248(10) 0.193(10) -0.029(9) -0.032(9) N1 0.055(2) 0.045(2) 0.035(2) 0.0009(17) 0.0055(17) 0.0232(19) N2 0.054(2) 0.051(2) 0.047(2) -0.0099(19) -0.0092(19) 0.016(2) N3 0.039(2) 0.041(2) 0.058(3) -0.0016(18) 0.0004(18) 0.0083(18) N4 0.039(2) 0.0354(19) 0.045(2) 0.0037(16) 0.0050(16) 0.0108(16) N7 0.049(2) 0.038(2) 0.049(2) -0.0022(17) 0.0064(18) 0.0112(18) N5 0.040(2) 0.0394(19) 0.0377(19) 0.0013(15) 0.0016(15) 0.0148(16) N8 0.058(3) 0.060(3) 0.050(2) 0.006(2) 0.0051(19) 0.033(2) N6 0.057(3) 0.060(3) 0.048(3) 0.002(2) 0.010(2) 0.003(2) N10 0.086(5) 0.156(8) 0.158(8) -0.021(6) 0.003(5) 0.048(5) N11 0.150(9) 0.176(10) 0.230(13) -0.006(9) 0.004(9) 0.055(8) N9 0.046(2) 0.047(2) 0.043(2) 0.0013(17) 0.0036(17) 0.0188(18) N12 0.090(7) 0.228(13) 0.143(9) 0.050(9) 0.021(6) 0.063(8) P1 0.0525(8) 0.0475(7) 0.0445(7) 0.0012(6) 0.0045(6) 0.0125(6) P2 0.0883(15) 0.1163(17) 0.0785(14) 0.0379(13) -0.0076(11) -0.0096(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C6 1.922(5) . ? Ru1 C10 2.015(4) . ? Ru1 N9 2.069(4) . ? Ru1 N1 2.105(4) . ? Ru1 N8 2.190(4) . ? Ru1 N7 2.223(4) . ? C1 N1 1.341(6) . ? C1 C2 1.368(7) . ? C2 C3 1.359(9) . ? C3 C4 1.372(9) . ? C4 C5 1.379(7) . ? C5 N1 1.353(6) . ? C5 N2 1.410(7) . ? C6 N3 1.364(6) . ? C6 N2 1.372(6) . ? C7 C8 1.324(9) . ? C7 N2 1.395(7) . ? C8 N3 1.406(7) . ? C9 N3 1.450(6) . ? C9 N4 1.469(6) . ? C10 N5 1.360(6) . ? C10 N4 1.369(5) . ? C11 C12 1.326(7) . ? C11 N4 1.375(6) . ? C12 N5 1.393(6) . ? C13 N6 1.305(6) . ? C13 C14 1.369(7) . ? C13 N5 1.440(5) . ? C14 C15 1.371(8) . ? C15 C16 1.363(9) . ? C16 C17 1.356(9) . ? C17 N6 1.351(7) . ? C18 C19 1.489(8) . ? C18 N7 1.490(6) . ? C19 N8 1.485(7) . ? C20 N9 1.246(8) . ? C20 N10 1.381(8) . ? C20 C21 1.547(10) . ? C22 C23 1.429(10) . ? C22 N10 1.478(12) . ? C23 N11 1.451(10) . ? C24 N12 1.186(16) . ? C24 C25 1.448(18) . ? F1 P1 1.550(4) . ? F2 P1 1.542(5) . ? F3 P1 1.570(4) . ? F4 P1 1.557(4) . ? F5 P1 1.604(3) . ? F6 P1 1.560(4) . ? F7 P2 1.510(8) . ? F8 P2 1.534(8) . ? F9 P2 1.556(5) . ? F10 P2 1.520(9) . ? F11 P2 1.565(7) . ? F12 P2 1.497(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Ru1 C10 80.09(18) . . ? C6 Ru1 N9 100.38(18) . . ? C10 Ru1 N9 87.43(16) . . ? C6 Ru1 N1 76.82(17) . . ? C10 Ru1 N1 102.45(15) . . ? N9 Ru1 N1 168.95(15) . . ? C6 Ru1 N8 104.12(18) . . ? C10 Ru1 N8 172.18(15) . . ? N9 Ru1 N8 85.33(15) . . ? N1 Ru1 N8 85.02(15) . . ? C6 Ru1 N7 174.06(17) . . ? C10 Ru1 N7 97.71(16) . . ? N9 Ru1 N7 84.97(15) . . ? N1 Ru1 N7 98.40(15) . . ? N8 Ru1 N7 78.73(16) . . ? N1 C1 C2 123.4(5) . . ? C3 C2 C1 119.4(6) . . ? C2 C3 C4 119.5(5) . . ? C3 C4 C5 118.1(6) . . ? N1 C5 C4 123.6(5) . . ? N1 C5 N2 112.6(4) . . ? C4 C5 N2 123.8(5) . . ? N3 C6 N2 104.8(4) . . ? N3 C6 Ru1 132.2(3) . . ? N2 C6 Ru1 119.6(3) . . ? C8 C7 N2 107.0(5) . . ? C7 C8 N3 108.1(5) . . ? N3 C9 N4 108.8(4) . . ? N5 C10 N4 102.9(4) . . ? N5 C10 Ru1 133.7(3) . . ? N4 C10 Ru1 123.0(3) . . ? C12 C11 N4 106.9(4) . . ? C11 C12 N5 107.0(4) . . ? N6 C13 C14 125.3(5) . . ? N6 C13 N5 116.2(4) . . ? C14 C13 N5 118.5(4) . . ? C13 C14 C15 117.3(5) . . ? C16 C15 C14 119.7(6) . . ? C17 C16 C15 117.9(5) . . ? N6 C17 C16 124.1(6) . . ? C19 C18 N7 109.2(4) . . ? N8 C19 C18 109.5(4) . . ? N9 C20 N10 115.9(7) . . ? N9 C20 C21 124.5(9) . . ? N10 C20 C21 119.6(8) . . ? C23 C22 N10 132.5(13) . . ? C22 C23 N11 105.8(16) . . ? N12 C24 C25 177.4(13) . . ? C1 N1 C5 116.1(4) . . ? C1 N1 Ru1 128.3(3) . . ? C5 N1 Ru1 114.8(3) . . ? C6 N2 C7 110.5(5) . . ? C6 N2 C5 114.7(4) . . ? C7 N2 C5 129.3(5) . . ? C6 N3 C8 109.5(4) . . ? C6 N3 C9 116.5(4) . . ? C8 N3 C9 127.3(4) . . ? C10 N4 C11 111.9(4) . . ? C10 N4 C9 123.1(4) . . ? C11 N4 C9 124.9(4) . . ? C18 N7 Ru1 108.7(3) . . ? C10 N5 C12 111.2(4) . . ? C10 N5 C13 125.7(4) . . ? C12 N5 C13 123.0(4) . . ? C19 N8 Ru1 109.7(3) . . ? C13 N6 C17 115.5(5) . . ? C20 N10 C22 138.0(10) . . ? C20 N9 Ru1 133.3(5) . . ? F2 P1 F1 89.7(4) . . ? F2 P1 F4 178.9(3) . . ? F1 P1 F4 91.0(4) . . ? F2 P1 F6 90.5(4) . . ? F1 P1 F6 179.2(3) . . ? F4 P1 F6 88.8(4) . . ? F2 P1 F3 90.6(3) . . ? F1 P1 F3 89.8(2) . . ? F4 P1 F3 90.2(3) . . ? F6 P1 F3 91.0(2) . . ? F2 P1 F5 90.1(3) . . ? F1 P1 F5 90.1(2) . . ? F4 P1 F5 89.1(2) . . ? F6 P1 F5 89.1(2) . . ? F3 P1 F5 179.3(3) . . ? F12 P2 F7 85.6(7) . . ? F12 P2 F10 94.4(7) . . ? F7 P2 F10 178.8(7) . . ? F12 P2 F8 92.7(6) . . ? F7 P2 F8 90.4(6) . . ? F10 P2 F8 90.8(7) . . ? F12 P2 F9 177.4(5) . . ? F7 P2 F9 92.5(5) . . ? F10 P2 F9 87.5(4) . . ? F8 P2 F9 89.0(4) . . ? F12 P2 F11 89.6(6) . . ? F7 P2 F11 87.1(5) . . ? F10 P2 F11 91.6(7) . . ? F8 P2 F11 176.5(6) . . ? F9 P2 F11 88.6(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.052 _refine_diff_density_min -1.156 _refine_diff_density_rms 0.085 #===END data_complex_9 _database_code_depnum_ccdc_archive 'CCDC 834951' #TrackingRef '- cif-Rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H40 F12 N12 P2 Ru' _chemical_formula_weight 923.72 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3876(6) _cell_length_b 12.7519(5) _cell_length_c 13.4337(5) _cell_angle_alpha 90.291(3) _cell_angle_beta 93.539(3) _cell_angle_gamma 116.079(4) _cell_volume 1901.15(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9006 _exptl_absorpt_correction_T_max 0.9430 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16400 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6683 _reflns_number_gt 5387 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. The restraints which are DFIX N11 H11A 0.86 0.02 and DFIX N11 H11B 0.86 0.02 have been used to DFIX the N-H bond distances. ; _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^)+(0.0947P)^2^+2.3020P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6683 _refine_ls_number_parameters 497 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1692 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.95779(3) 0.70893(3) 0.71892(3) 0.04317(17) Uani 1 1 d . . . C1 C 1.3661(6) 0.8258(6) 0.6482(5) 0.0757(18) Uani 1 1 d . . . H1 H 1.3715 0.8387 0.5803 0.091 Uiso 1 1 calc R . . C2 C 1.4612(5) 0.8960(5) 0.7112(6) 0.0766(18) Uani 1 1 d . . . H2 H 1.5310 0.9525 0.6867 0.092 Uiso 1 1 calc R . . C3 C 1.4515(5) 0.8814(6) 0.8109(6) 0.0789(19) Uani 1 1 d . . . H3 H 1.5143 0.9292 0.8559 0.095 Uiso 1 1 calc R . . C4 C 1.3483(5) 0.7955(5) 0.8447(4) 0.0647(15) Uani 1 1 d . . . H4 H 1.3395 0.7841 0.9126 0.078 Uiso 1 1 calc R . . C5 C 1.2585(4) 0.7271(4) 0.7751(4) 0.0443(11) Uani 1 1 d . . . C6 C 1.0362(4) 0.6160(4) 0.7866(3) 0.0405(10) Uani 1 1 d . . . C7 C 1.1576(5) 0.5472(5) 0.8686(4) 0.0544(12) Uani 1 1 d . . . H7 H 1.2269 0.5425 0.8937 0.065 Uiso 1 1 calc R . . C8 C 1.0444(5) 0.4726(5) 0.8834(4) 0.0549(12) Uani 1 1 d . . . H8 H 1.0192 0.4055 0.9203 0.066 Uiso 1 1 calc R . . C9 C 0.8394(4) 0.4567(5) 0.8271(4) 0.0593(14) Uani 1 1 d . . . H9A H 0.8110 0.3784 0.8519 0.071 Uiso 1 1 calc R . . H9B H 0.8098 0.5001 0.8679 0.071 Uiso 1 1 calc R . . C10 C 0.8441(4) 0.5544(5) 0.6759(4) 0.0494(12) Uani 1 1 d . . . C11 C 0.7530(5) 0.3569(6) 0.6558(6) 0.0791(19) Uani 1 1 d . . . H11 H 0.7171 0.2783 0.6711 0.095 Uiso 1 1 calc R . . C12 C 0.7742(6) 0.3994(6) 0.5638(6) 0.0788(19) Uani 1 1 d . . . H12 H 0.7553 0.3564 0.5038 0.095 Uiso 1 1 calc R . . C13 C 0.9092(5) 0.6040(5) 0.5151(4) 0.0589(14) Uani 1 1 d . . . C14 C 0.9037(6) 0.5901(7) 0.4127(4) 0.0776(19) Uani 1 1 d . . . H14 H 0.8463 0.5227 0.3793 0.093 Uiso 1 1 calc R . . C15 C 0.9866(8) 0.6801(8) 0.3620(5) 0.087(2) Uani 1 1 d . . . H15 H 0.9851 0.6743 0.2929 0.105 Uiso 1 1 calc R . . C16 C 1.0718(6) 0.7784(6) 0.4129(4) 0.0758(18) Uani 1 1 d . . . H16 H 1.1279 0.8392 0.3787 0.091 Uiso 1 1 calc R . . C17 C 1.0727(5) 0.7854(5) 0.5153(4) 0.0591(13) Uani 1 1 d . . . H17 H 1.1310 0.8516 0.5496 0.071 Uiso 1 1 calc R . . C18 C 1.0815(6) 0.9814(5) 0.7888(5) 0.0689(16) Uani 1 1 d . . . H18A H 1.0416 0.9642 0.8507 0.083 Uiso 1 1 calc R . . H18B H 1.1562 1.0521 0.8004 0.083 Uiso 1 1 calc R . . C19 C 1.0041(7) 1.0025(6) 0.7121(6) 0.089(2) Uani 1 1 d . . . H19A H 1.0381 1.0072 0.6482 0.107 Uiso 1 1 calc R . . H19B H 1.0062 1.0779 0.7270 0.107 Uiso 1 1 calc R . . C20 C 0.8739(7) 0.9118(6) 0.7021(5) 0.083(2) Uani 1 1 d . . . H20A H 0.8427 0.8959 0.7677 0.100 Uiso 1 1 calc R . . H20B H 0.8264 0.9419 0.6623 0.100 Uiso 1 1 calc R . . C21 C 0.7945(6) 0.7008(5) 0.8887(4) 0.0621(14) Uani 1 1 d . . . C22 C 0.7808(7) 0.7352(7) 0.9924(5) 0.091(2) Uani 1 1 d . . . H22A H 0.8584 0.7710 1.0286 0.136 Uiso 1 1 calc R . . H22B H 0.7287 0.6671 1.0260 0.136 Uiso 1 1 calc R . . H22C H 0.7466 0.7897 0.9891 0.136 Uiso 1 1 calc R . . C23 C 0.5746(7) 0.6251(9) 0.8479(7) 0.103(3) Uani 1 1 d . . . H23A H 0.5662 0.6971 0.8444 0.124 Uiso 1 1 calc R . . H23B H 0.5604 0.5976 0.9152 0.124 Uiso 1 1 calc R . . C24 C 0.4803(7) 0.5333(12) 0.7739(8) 0.141(4) Uani 1 1 d . . . H24A H 0.4903 0.4621 0.7791 0.170 Uiso 1 1 calc R . . H24B H 0.4012 0.5161 0.7957 0.170 Uiso 1 1 calc R . . C25 C 0.4808(7) 0.5602(10) 0.6723(8) 0.121(3) Uani 1 1 d . . . H25A H 0.4805 0.6358 0.6660 0.145 Uiso 1 1 calc R . . H25B H 0.4081 0.5024 0.6368 0.145 Uiso 1 1 calc R . . C26 C 0.5367(7) 0.2921(9) 0.9218(6) 0.085(2) Uani 1 1 d . . . C27 C 0.4628(10) 0.1814(11) 0.8764(9) 0.143(4) Uani 1 1 d . . . H27A H 0.5049 0.1647 0.8258 0.214 Uiso 1 1 calc R . . H27B H 0.3902 0.1813 0.8467 0.214 Uiso 1 1 calc R . . H27C H 0.4428 0.1230 0.9259 0.214 Uiso 1 1 calc R . . F1 F 0.2766(9) 0.9579(6) 0.0038(6) 0.229(5) Uani 1 1 d . . . F2 F 0.2561(5) 0.9944(5) 0.1545(5) 0.157(3) Uani 1 1 d . . . F3 F 0.1144(8) 0.8138(6) 0.1596(5) 0.194(4) Uani 1 1 d . . . F4 F 0.1364(4) 0.7797(4) 0.0071(4) 0.1283(19) Uani 1 1 d . . . F5 F 0.0974(6) 0.9288(7) 0.0522(6) 0.172(3) Uani 1 1 d . . . F6 F 0.2927(7) 0.8475(7) 0.1094(7) 0.200(4) Uani 1 1 d . . . F7 F 0.6798(16) 0.9535(13) 0.5025(9) 0.353(9) Uani 1 1 d . . . F8 F 0.5975(12) 0.7884(12) 0.5283(8) 0.282(6) Uani 1 1 d . . . F9 F 0.5890(14) 0.7446(9) 0.3617(9) 0.322(8) Uani 1 1 d . . . F10 F 0.6879(6) 0.9335(7) 0.3522(5) 0.183(3) Uani 1 1 d . . . F11 F 0.7549(11) 0.8369(18) 0.4534(6) 0.350(9) Uani 1 1 d . . . F12 F 0.5171(7) 0.8587(9) 0.4118(8) 0.220(4) Uani 1 1 d . . . N1 N 0.9923(4) 0.6999(4) 0.5677(3) 0.0531(10) Uani 1 1 d . . . N2 N 0.8299(4) 0.5205(4) 0.5763(3) 0.0577(11) Uani 1 1 d . . . N3 N 0.7943(4) 0.4512(4) 0.7238(4) 0.0578(11) Uani 1 1 d . . . N4 N 0.9722(3) 0.5147(4) 0.8333(3) 0.0478(9) Uani 1 1 d . . . N5 N 1.1525(3) 0.6334(3) 0.8084(3) 0.0436(9) Uani 1 1 d . . . N6 N 1.2644(4) 0.7386(4) 0.6779(3) 0.0624(12) Uani 1 1 d . . . N7 N 1.1098(4) 0.8842(4) 0.7617(3) 0.0522(10) Uani 1 1 d . . . H7A H 1.1536 0.8747 0.8138 0.063 Uiso 1 1 calc R . . H7B H 1.1576 0.9069 0.7104 0.063 Uiso 1 1 calc R . . N8 N 0.8627(4) 0.8053(4) 0.6558(3) 0.0622(12) Uani 1 1 d . . . H8A H 0.8850 0.8219 0.5930 0.075 Uiso 1 1 calc R . . H8B H 0.7837 0.7556 0.6508 0.075 Uiso 1 1 calc R . . N9 N 0.9002(4) 0.7227(4) 0.8599(3) 0.0540(10) Uani 1 1 d . . . H9 H 0.9568 0.7471 0.9070 0.065 Uiso 1 1 calc R . . N10 N 0.6968(4) 0.6482(5) 0.8261(4) 0.0700(13) Uani 1 1 d . . . H10 H 0.7066 0.6260 0.7682 0.084 Uiso 1 1 calc R . . N11 N 0.5871(6) 0.5625(8) 0.6262(6) 0.0950(19) Uani 1 1 d D . . N12 N 0.5963(7) 0.3786(8) 0.9579(6) 0.106(2) Uani 1 1 d . . . P1 P 0.19615(14) 0.88825(14) 0.08166(11) 0.0623(4) Uani 1 1 d . . . P2 P 0.6382(3) 0.8439(3) 0.4316(2) 0.1239(10) Uani 1 1 d . . . H11B H 0.567(8) 0.488(3) 0.627(7) 0.12(4) Uiso 1 1 d D . . H11A H 0.560(10) 0.573(10) 0.569(4) 0.17(5) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0423(2) 0.0455(3) 0.0433(2) -0.00221(16) 0.00311(16) 0.02089(18) C1 0.065(4) 0.070(4) 0.072(4) 0.011(3) 0.022(3) 0.009(3) C2 0.048(3) 0.056(4) 0.111(6) 0.010(4) 0.016(3) 0.008(3) C3 0.050(3) 0.065(4) 0.102(5) -0.012(4) -0.010(3) 0.009(3) C4 0.051(3) 0.067(4) 0.064(3) -0.011(3) -0.005(3) 0.016(3) C5 0.038(2) 0.040(3) 0.056(3) -0.004(2) 0.005(2) 0.019(2) C6 0.036(2) 0.040(2) 0.042(2) -0.0026(19) 0.0045(19) 0.0133(19) C7 0.053(3) 0.058(3) 0.056(3) 0.008(2) -0.002(2) 0.029(3) C8 0.058(3) 0.054(3) 0.052(3) 0.011(2) 0.006(2) 0.024(3) C9 0.045(3) 0.052(3) 0.075(4) 0.014(3) 0.018(3) 0.014(2) C10 0.037(2) 0.053(3) 0.057(3) -0.008(2) -0.003(2) 0.020(2) C11 0.051(3) 0.054(4) 0.116(6) -0.012(4) -0.007(4) 0.010(3) C12 0.071(4) 0.061(4) 0.092(5) -0.033(4) -0.021(4) 0.022(3) C13 0.061(3) 0.073(4) 0.052(3) -0.012(3) -0.003(3) 0.038(3) C14 0.082(4) 0.104(5) 0.054(3) -0.021(3) -0.011(3) 0.049(4) C15 0.113(6) 0.128(7) 0.046(3) -0.010(4) 0.004(4) 0.076(5) C16 0.096(5) 0.089(5) 0.059(3) 0.019(3) 0.023(3) 0.053(4) C17 0.071(3) 0.064(3) 0.055(3) 0.009(3) 0.016(3) 0.040(3) C18 0.074(4) 0.049(3) 0.083(4) -0.010(3) 0.004(3) 0.027(3) C19 0.092(5) 0.067(4) 0.111(6) 0.010(4) 0.001(4) 0.039(4) C20 0.103(5) 0.094(5) 0.077(4) -0.009(4) -0.005(4) 0.067(5) C21 0.070(4) 0.064(4) 0.062(3) 0.009(3) 0.020(3) 0.037(3) C22 0.101(5) 0.116(6) 0.071(4) -0.001(4) 0.031(4) 0.059(5) C23 0.075(5) 0.144(8) 0.116(6) 0.009(5) 0.031(5) 0.068(5) C24 0.058(5) 0.220(13) 0.145(9) 0.012(9) 0.017(5) 0.059(6) C25 0.071(5) 0.161(9) 0.136(8) 0.036(7) 0.009(5) 0.055(6) C26 0.062(4) 0.109(7) 0.085(5) 0.020(5) 0.015(4) 0.039(4) C27 0.128(9) 0.153(10) 0.144(9) -0.013(8) 0.004(7) 0.060(8) F1 0.310(10) 0.110(5) 0.214(7) 0.026(5) 0.180(8) 0.025(6) F2 0.099(3) 0.150(5) 0.199(6) -0.109(5) -0.015(4) 0.038(3) F3 0.267(9) 0.137(5) 0.128(4) 0.015(4) 0.113(5) 0.030(5) F4 0.112(3) 0.115(4) 0.113(3) -0.051(3) 0.018(3) 0.009(3) F5 0.148(5) 0.206(7) 0.200(7) -0.041(5) -0.051(5) 0.120(5) F6 0.167(6) 0.191(7) 0.280(9) -0.074(7) -0.099(6) 0.129(6) F7 0.40(2) 0.293(15) 0.184(9) -0.037(10) -0.084(11) 0.006(13) F8 0.365(14) 0.392(16) 0.212(9) 0.188(10) 0.153(9) 0.262(13) F9 0.51(2) 0.200(10) 0.280(12) -0.120(9) -0.164(13) 0.208(12) F10 0.153(5) 0.188(7) 0.174(6) 0.099(5) 0.048(5) 0.038(5) F11 0.313(12) 0.80(3) 0.137(6) 0.082(11) 0.042(7) 0.423(18) F12 0.115(5) 0.223(9) 0.281(10) 0.077(8) -0.002(6) 0.038(5) N1 0.061(3) 0.060(3) 0.049(2) 0.001(2) 0.006(2) 0.035(2) N2 0.055(3) 0.060(3) 0.058(3) -0.017(2) -0.010(2) 0.027(2) N3 0.038(2) 0.050(3) 0.079(3) 0.001(2) 0.004(2) 0.0144(19) N4 0.039(2) 0.046(2) 0.055(2) 0.0090(19) 0.0077(18) 0.0150(18) N5 0.040(2) 0.047(2) 0.045(2) 0.0017(17) 0.0054(17) 0.0190(17) N6 0.056(3) 0.058(3) 0.056(3) 0.004(2) 0.011(2) 0.009(2) N7 0.054(2) 0.046(2) 0.054(2) -0.0033(19) -0.0006(19) 0.0212(19) N8 0.063(3) 0.075(3) 0.063(3) 0.004(2) 0.002(2) 0.043(3) N9 0.053(2) 0.064(3) 0.048(2) 0.001(2) 0.0074(19) 0.028(2) N10 0.054(3) 0.093(4) 0.071(3) -0.006(3) 0.012(2) 0.039(3) N11 0.060(3) 0.110(6) 0.108(5) 0.000(5) -0.006(3) 0.032(4) N12 0.086(5) 0.133(7) 0.106(5) 0.030(5) 0.024(4) 0.053(5) P1 0.0587(9) 0.0602(9) 0.0579(8) -0.0014(7) -0.0001(7) 0.0177(7) P2 0.1053(18) 0.116(2) 0.1003(17) 0.0394(16) -0.0065(14) 0.0047(15) _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 C10 1.910(5) . ? Ru1 C6 2.022(5) . ? Ru1 N9 2.097(4) . ? Ru1 N1 2.114(4) . ? Ru1 N8 2.186(4) . ? Ru1 N7 2.242(4) . ? C1 N6 1.349(7) . ? C1 C2 1.358(9) . ? C2 C3 1.359(9) . ? C3 C4 1.373(9) . ? C4 C5 1.372(7) . ? C5 N6 1.317(6) . ? C5 N5 1.432(6) . ? C6 N4 1.364(6) . ? C6 N5 1.370(6) . ? C7 C8 1.333(7) . ? C7 N5 1.389(6) . ? C8 N4 1.375(7) . ? C9 N3 1.453(7) . ? C9 N4 1.474(6) . ? C10 N3 1.367(7) . ? C10 N2 1.381(6) . ? C11 C12 1.346(10) . ? C11 N3 1.391(8) . ? C12 N2 1.390(8) . ? C13 N1 1.360(7) . ? C13 C14 1.380(8) . ? C13 N2 1.401(7) . ? C14 C15 1.376(11) . ? C15 C16 1.376(10) . ? C16 C17 1.377(8) . ? C17 N1 1.348(7) . ? C18 C19 1.469(9) . ? C18 N7 1.478(7) . ? C19 C20 1.514(10) . ? C20 N8 1.437(8) . ? C21 N9 1.299(7) . ? C21 N10 1.333(7) . ? C21 C22 1.500(8) . ? C23 N10 1.458(8) . ? C23 C24 1.538(14) . ? C24 C25 1.409(12) . ? C25 N11 1.478(11) . ? C26 N12 1.110(11) . ? C26 C27 1.410(14) . ? F1 P1 1.495(6) . ? F2 P1 1.534(5) . ? F3 P1 1.523(6) . ? F4 P1 1.568(4) . ? F5 P1 1.555(6) . ? F6 P1 1.527(6) . ? F7 P2 1.556(14) . ? F8 P2 1.491(8) . ? F9 P2 1.447(9) . ? F10 P2 1.515(6) . ? F11 P2 1.498(8) . ? F12 P2 1.599(9) . ? 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 C10 Ru1 C6 80.02(19) . . ? C10 Ru1 N9 101.3(2) . . ? C6 Ru1 N9 85.79(17) . . ? C10 Ru1 N1 76.9(2) . . ? C6 Ru1 N1 102.64(17) . . ? N9 Ru1 N1 170.80(16) . . ? C10 Ru1 N8 99.0(2) . . ? C6 Ru1 N8 175.22(17) . . ? N9 Ru1 N8 89.83(17) . . ? N1 Ru1 N8 81.60(17) . . ? C10 Ru1 N7 172.41(18) . . ? C6 Ru1 N7 95.31(17) . . ? N9 Ru1 N7 84.20(17) . . ? N1 Ru1 N7 98.49(17) . . ? N8 Ru1 N7 86.15(18) . . ? N6 C1 C2 124.2(6) . . ? C1 C2 C3 118.2(6) . . ? C2 C3 C4 119.6(6) . . ? C5 C4 C3 117.9(6) . . ? N6 C5 C4 124.4(5) . . ? N6 C5 N5 116.7(4) . . ? C4 C5 N5 118.9(5) . . ? N4 C6 N5 102.0(4) . . ? N4 C6 Ru1 122.6(3) . . ? N5 C6 Ru1 135.0(3) . . ? C8 C7 N5 107.0(4) . . ? C7 C8 N4 106.3(5) . . ? N3 C9 N4 109.2(4) . . ? N3 C10 N2 103.9(4) . . ? N3 C10 Ru1 132.9(4) . . ? N2 C10 Ru1 119.9(4) . . ? C12 C11 N3 107.8(6) . . ? C11 C12 N2 106.4(5) . . ? N1 C13 C14 123.8(6) . . ? N1 C13 N2 112.6(4) . . ? C14 C13 N2 123.6(6) . . ? C15 C14 C13 117.2(6) . . ? C16 C15 C14 120.5(6) . . ? C15 C16 C17 119.0(6) . . ? N1 C17 C16 122.4(6) . . ? C19 C18 N7 113.5(5) . . ? C18 C19 C20 115.6(6) . . ? N8 C20 C19 110.9(6) . . ? N9 C21 N10 120.3(5) . . ? N9 C21 C22 120.5(6) . . ? N10 C21 C22 119.2(5) . . ? N10 C23 C24 111.4(7) . . ? C25 C24 C23 118.2(10) . . ? C24 C25 N11 111.9(8) . . ? N12 C26 C27 178.9(11) . . ? C17 N1 C13 117.1(5) . . ? C17 N1 Ru1 127.4(4) . . ? C13 N1 Ru1 114.5(4) . . ? C10 N2 C12 111.2(5) . . ? C10 N2 C13 114.9(4) . . ? C12 N2 C13 129.0(5) . . ? C10 N3 C11 110.7(5) . . ? C10 N3 C9 114.9(4) . . ? C11 N3 C9 127.9(5) . . ? C6 N4 C8 113.0(4) . . ? C6 N4 C9 122.4(4) . . ? C8 N4 C9 124.6(4) . . ? C6 N5 C7 111.6(4) . . ? C6 N5 C5 126.1(4) . . ? C7 N5 C5 122.2(4) . . ? C5 N6 C1 115.7(5) . . ? C18 N7 Ru1 118.8(3) . . ? C20 N8 Ru1 121.9(4) . . ? C21 N9 Ru1 131.5(4) . . ? C21 N10 C23 125.3(6) . . ? F1 P1 F3 178.1(4) . . ? F1 P1 F6 86.2(6) . . ? F3 P1 F6 92.7(6) . . ? F1 P1 F2 89.3(4) . . ? F3 P1 F2 92.2(4) . . ? F6 P1 F2 92.0(4) . . ? F1 P1 F5 93.6(6) . . ? F3 P1 F5 87.5(5) . . ? F6 P1 F5 179.3(4) . . ? F2 P1 F5 88.6(4) . . ? F1 P1 F4 90.3(4) . . ? F3 P1 F4 88.2(3) . . ? F6 P1 F4 87.4(4) . . ? F2 P1 F4 179.3(3) . . ? F5 P1 F4 92.0(4) . . ? F9 P2 F8 102.4(8) . . ? F9 P2 F11 94.4(9) . . ? F8 P2 F11 89.0(6) . . ? F9 P2 F10 94.7(7) . . ? F8 P2 F10 162.5(7) . . ? F11 P2 F10 93.7(7) . . ? F9 P2 F7 173.8(10) . . ? F8 P2 F7 79.0(7) . . ? F11 P2 F7 91.6(9) . . ? F10 P2 F7 83.6(6) . . ? F9 P2 F12 88.9(7) . . ? F8 P2 F12 90.8(6) . . ? F11 P2 F12 176.6(9) . . ? F10 P2 F12 85.5(5) . . ? F7 P2 F12 85.0(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.961 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.091 #===END data_complex_10 _database_code_depnum_ccdc_archive 'CCDC 834952' #TrackingRef '- cif-Rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H28 F12 N10 P2 Ru' _chemical_formula_weight 871.59 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5759(3) _cell_length_b 9.1184(3) _cell_length_c 21.2088(7) _cell_angle_alpha 95.762(3) _cell_angle_beta 93.358(3) _cell_angle_gamma 94.656(3) _cell_volume 1640.94(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8115 _exptl_absorpt_correction_T_max 0.9227 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14769 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5778 _reflns_number_gt 5151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0536P)^2^+6.4905P] 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 5778 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.85438(4) 0.74449(3) 0.721535(15) 0.01736(12) Uani 1 1 d . . . C1 C 1.1875(5) 0.6120(5) 0.7321(2) 0.0228(9) Uani 1 1 d . . . H1 H 1.1813 0.6238 0.7759 0.027 Uiso 1 1 calc R . . C2 C 1.3157(5) 0.5496(5) 0.7079(2) 0.0268(10) Uani 1 1 d . . . H2 H 1.3946 0.5214 0.7349 0.032 Uiso 1 1 calc R . . C3 C 1.3249(5) 0.5299(5) 0.6433(2) 0.0298(10) Uani 1 1 d . . . H3 H 1.4091 0.4859 0.6260 0.036 Uiso 1 1 calc R . . C4 C 1.2084(6) 0.5758(6) 0.6039(2) 0.0309(11) Uani 1 1 d . . . H4 H 1.2131 0.5653 0.5600 0.037 Uiso 1 1 calc R . . C5 C 1.0845(5) 0.6381(5) 0.6322(2) 0.0243(9) Uani 1 1 d . . . C6 C 0.8350(5) 0.7311(4) 0.6307(2) 0.0201(9) Uani 1 1 d . . . C7 C 0.9258(6) 0.6891(7) 0.5324(2) 0.0415(13) Uani 1 1 d . . . H7 H 0.9902 0.6624 0.5001 0.050 Uiso 1 1 calc R . . C8 C 0.7845(6) 0.7396(7) 0.5258(2) 0.0389(13) Uani 1 1 d . . . H8 H 0.7319 0.7554 0.4878 0.047 Uiso 1 1 calc R . . C9 C 0.5773(5) 0.8085(5) 0.5994(2) 0.0254(10) Uani 1 1 d . . . H9A H 0.5005 0.7248 0.5873 0.030 Uiso 1 1 calc R . . H9B H 0.5531 0.8861 0.5733 0.030 Uiso 1 1 calc R . . C10 C 0.6458(5) 0.8324(4) 0.71989(19) 0.0195(9) Uani 1 1 d . . . C11 C 0.4367(6) 0.9428(5) 0.6803(2) 0.0298(10) Uani 1 1 d . . . H11 H 0.3652 0.9753 0.6513 0.036 Uiso 1 1 calc R . . C12 C 0.4373(6) 0.9651(5) 0.7430(2) 0.0313(11) Uani 1 1 d . . . H12 H 0.3669 1.0165 0.7664 0.038 Uiso 1 1 calc R . . C13 C 0.5953(5) 0.8956(5) 0.8342(2) 0.0248(10) Uani 1 1 d . . . C14 C 0.5470(5) 0.7715(5) 0.8628(2) 0.0269(10) Uani 1 1 d . . . H14 H 0.5004 0.6866 0.8387 0.032 Uiso 1 1 calc R . . C15 C 0.5699(6) 0.7772(5) 0.9281(2) 0.0323(11) Uani 1 1 d . . . H15 H 0.5405 0.6954 0.9489 0.039 Uiso 1 1 calc R . . C16 C 0.6369(7) 0.9055(5) 0.9615(2) 0.0358(12) Uani 1 1 d . . . H16 H 0.6532 0.9128 1.0055 0.043 Uiso 1 1 calc R . . C17 C 0.6793(7) 1.0228(6) 0.9286(2) 0.0415(13) Uani 1 1 d . . . H17 H 0.7246 1.1095 0.9516 0.050 Uiso 1 1 calc R . . C18 C 1.0432(7) 0.9378(6) 0.8768(2) 0.0409(13) Uani 1 1 d . . . H18A H 1.1477 0.9322 0.8634 0.061 Uiso 1 1 calc R . . H18B H 1.0476 0.9842 0.9197 0.061 Uiso 1 1 calc R . . H18C H 0.9859 0.9950 0.8494 0.061 Uiso 1 1 calc R . . C19 C 0.9642(5) 0.7880(5) 0.8739(2) 0.0278(10) Uani 1 1 d . . . C20 C 0.9483(5) 0.6962(5) 0.9236(2) 0.0283(10) Uani 1 1 d . . . H20 H 0.9847 0.7211 0.9658 0.034 Uiso 1 1 calc R . . C21 C 0.8707(5) 0.5659(5) 0.8989(2) 0.0263(10) Uani 1 1 d . . . C22 C 0.8223(6) 0.4341(6) 0.9320(2) 0.0340(11) Uani 1 1 d . . . H22A H 0.8459 0.4566 0.9769 0.051 Uiso 1 1 calc R . . H22B H 0.8781 0.3521 0.9166 0.051 Uiso 1 1 calc R . . H22C H 0.7116 0.4087 0.9237 0.051 Uiso 1 1 calc R . . C23 C 0.7744(5) 0.4789(5) 0.7837(2) 0.0235(9) Uani 1 1 d . . . C24 C 0.7280(6) 0.3227(5) 0.7928(2) 0.0292(10) Uani 1 1 d . . . H24A H 0.6919 0.2691 0.7526 0.044 Uiso 1 1 calc R . . H24B H 0.6453 0.3189 0.8214 0.044 Uiso 1 1 calc R . . H24C H 0.8166 0.2788 0.8103 0.044 Uiso 1 1 calc R . . C25 C 1.0102(5) 1.0675(5) 0.7095(2) 0.0234(9) Uani 1 1 d . . . C26 C 1.0784(6) 1.2115(5) 0.6966(2) 0.0352(12) Uani 1 1 d . . . H26A H 1.1781 1.2012 0.6791 0.053 Uiso 1 1 calc R . . H26B H 1.0924 1.2766 0.7354 0.053 Uiso 1 1 calc R . . H26C H 1.0097 1.2520 0.6668 0.053 Uiso 1 1 calc R . . F1 F 0.7272(4) 0.1933(4) 0.50205(14) 0.0511(9) Uani 1 1 d . . . F2 F 0.5819(3) 0.3757(3) 0.53747(14) 0.0412(7) Uani 1 1 d . . . F3 F 0.8218(3) 0.3559(3) 0.58583(15) 0.0423(7) Uani 1 1 d . . . F4 F 0.6006(3) 0.3025(3) 0.63620(12) 0.0347(6) Uani 1 1 d . . . F5 F 0.7469(4) 0.1201(3) 0.60119(15) 0.0415(7) Uani 1 1 d . . . F6 F 0.5081(3) 0.1397(3) 0.55290(13) 0.0345(6) Uani 1 1 d . . . F7 F 0.1695(4) 0.2863(4) 0.93151(16) 0.0539(9) Uani 1 1 d . . . F8 F 0.2809(6) 0.1949(5) 0.8450(3) 0.111(2) Uani 1 1 d . . . F9 F 0.3936(4) 0.4148(5) 0.83301(19) 0.0687(12) Uani 1 1 d . . . F10 F 0.1321(5) 0.3843(6) 0.84097(19) 0.0913(16) Uani 1 1 d . . . F11 F 0.4281(5) 0.3201(7) 0.9227(2) 0.1046(19) Uani 1 1 d . . . F12 F 0.2795(7) 0.5060(5) 0.9181(3) 0.122(2) Uani 1 1 d . . . N1 N 1.0716(4) 0.6563(4) 0.69551(16) 0.0197(7) Uani 1 1 d . . . N2 N 0.9571(4) 0.6845(4) 0.59729(17) 0.0265(8) Uani 1 1 d . . . N3 N 0.7304(4) 0.7644(4) 0.58639(16) 0.0220(8) Uani 1 1 d . . . N4 N 0.5629(4) 0.8617(4) 0.66601(16) 0.0211(8) Uani 1 1 d . . . N5 N 0.5634(4) 0.8970(4) 0.76701(17) 0.0230(8) Uani 1 1 d . . . N6 N 0.6594(6) 1.0203(4) 0.86553(19) 0.0359(10) Uani 1 1 d . . . N7 N 0.8959(4) 0.7177(4) 0.82057(17) 0.0225(8) Uani 1 1 d . . . N8 N 0.8395(4) 0.5783(4) 0.83496(17) 0.0227(8) Uani 1 1 d . . . N9 N 0.7648(4) 0.5346(4) 0.73107(16) 0.0197(7) Uani 1 1 d . . . H9 H 0.7188 0.4817 0.6983 0.024 Uiso 1 1 calc R . . N10 N 0.9564(4) 0.9532(4) 0.71817(16) 0.0207(8) Uani 1 1 d . . . P1 P 0.66528(14) 0.24756(13) 0.56922(5) 0.0262(3) Uani 1 1 d . . . P2 P 0.28079(15) 0.34757(14) 0.88177(6) 0.0308(3) 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 0.0172(2) 0.01942(19) 0.01637(19) 0.00581(13) 0.00028(13) 0.00267(13) C1 0.021(2) 0.023(2) 0.024(2) 0.0076(17) -0.0030(18) -0.0011(17) C2 0.021(2) 0.028(2) 0.032(2) 0.0112(19) -0.0009(19) 0.0059(19) C3 0.021(2) 0.032(2) 0.038(3) 0.004(2) 0.006(2) 0.0070(19) C4 0.025(3) 0.046(3) 0.023(2) 0.005(2) 0.0055(19) 0.010(2) C5 0.022(2) 0.027(2) 0.024(2) 0.0049(18) -0.0021(18) 0.0031(18) C6 0.017(2) 0.020(2) 0.024(2) 0.0061(16) 0.0009(17) 0.0000(16) C7 0.031(3) 0.080(4) 0.016(2) 0.006(2) 0.003(2) 0.021(3) C8 0.029(3) 0.073(4) 0.017(2) 0.009(2) 0.002(2) 0.012(3) C9 0.023(2) 0.032(2) 0.022(2) 0.0052(18) -0.0008(18) 0.0055(19) C10 0.021(2) 0.017(2) 0.021(2) 0.0053(16) 0.0019(17) -0.0007(16) C11 0.025(2) 0.037(3) 0.032(3) 0.014(2) 0.003(2) 0.016(2) C12 0.030(3) 0.037(3) 0.032(3) 0.012(2) 0.008(2) 0.018(2) C13 0.026(2) 0.025(2) 0.027(2) 0.0083(18) 0.0057(19) 0.0105(18) C14 0.026(2) 0.029(2) 0.028(2) 0.0083(19) 0.0018(19) 0.0063(19) C15 0.033(3) 0.036(3) 0.033(3) 0.017(2) 0.009(2) 0.011(2) C16 0.052(3) 0.033(3) 0.024(2) 0.003(2) 0.005(2) 0.014(2) C17 0.064(4) 0.029(3) 0.031(3) 0.000(2) -0.001(3) 0.006(2) C18 0.052(3) 0.044(3) 0.023(2) 0.001(2) -0.002(2) -0.009(3) C19 0.026(2) 0.036(3) 0.022(2) 0.0067(19) -0.0001(19) 0.005(2) C20 0.026(3) 0.038(3) 0.021(2) 0.0036(19) 0.0015(19) 0.004(2) C21 0.023(2) 0.038(3) 0.021(2) 0.0108(19) 0.0051(18) 0.013(2) C22 0.037(3) 0.043(3) 0.027(2) 0.015(2) 0.006(2) 0.011(2) C23 0.017(2) 0.026(2) 0.030(2) 0.0091(18) 0.0056(18) 0.0067(17) C24 0.031(3) 0.025(2) 0.034(3) 0.0122(19) 0.004(2) 0.0035(19) C25 0.021(2) 0.027(2) 0.021(2) 0.0032(18) -0.0032(18) 0.0027(19) C26 0.037(3) 0.025(2) 0.042(3) 0.009(2) -0.004(2) -0.005(2) F1 0.0368(18) 0.083(2) 0.0337(16) -0.0027(16) 0.0053(14) 0.0171(17) F2 0.0362(17) 0.0451(17) 0.0462(18) 0.0227(14) -0.0008(14) 0.0079(14) F3 0.0306(16) 0.0473(18) 0.0486(18) 0.0133(14) -0.0030(14) -0.0047(13) F4 0.0374(16) 0.0392(16) 0.0262(14) -0.0010(12) 0.0011(12) 0.0021(13) F5 0.0372(17) 0.0369(16) 0.0502(18) 0.0077(13) -0.0158(14) 0.0112(13) F6 0.0328(16) 0.0361(15) 0.0339(15) 0.0043(12) -0.0078(12) 0.0054(12) F7 0.047(2) 0.076(2) 0.0472(19) 0.0285(17) 0.0208(16) 0.0158(17) F8 0.105(4) 0.052(2) 0.173(5) -0.038(3) 0.089(4) -0.018(2) F9 0.052(2) 0.095(3) 0.073(3) 0.051(2) 0.028(2) 0.019(2) F10 0.052(2) 0.179(5) 0.056(2) 0.045(3) 0.013(2) 0.041(3) F11 0.036(2) 0.226(6) 0.061(3) 0.056(3) -0.0020(19) 0.020(3) F12 0.114(4) 0.058(3) 0.191(6) -0.028(3) 0.087(4) -0.017(3) N1 0.0177(18) 0.0196(17) 0.0220(18) 0.0054(14) 0.0008(14) -0.0007(14) N2 0.021(2) 0.042(2) 0.0173(18) 0.0046(16) 0.0001(15) 0.0059(17) N3 0.0168(18) 0.032(2) 0.0185(18) 0.0067(15) -0.0001(14) 0.0047(15) N4 0.0186(19) 0.0258(19) 0.0205(18) 0.0071(14) 0.0021(14) 0.0053(15) N5 0.025(2) 0.0229(18) 0.0236(19) 0.0087(15) 0.0045(15) 0.0091(15) N6 0.053(3) 0.024(2) 0.031(2) 0.0056(17) 0.002(2) 0.0042(19) N7 0.0203(19) 0.0259(19) 0.0217(18) 0.0068(15) 0.0000(15) 0.0010(15) N8 0.023(2) 0.0243(19) 0.0233(19) 0.0104(15) 0.0041(15) 0.0058(15) N9 0.0167(18) 0.0223(18) 0.0208(18) 0.0050(14) 0.0000(14) 0.0031(14) N10 0.0201(19) 0.0213(19) 0.0205(18) 0.0020(14) -0.0009(14) 0.0025(15) P1 0.0231(6) 0.0330(6) 0.0236(6) 0.0056(5) -0.0016(5) 0.0070(5) P2 0.0287(7) 0.0381(7) 0.0277(6) 0.0111(5) 0.0042(5) 0.0043(5) _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 C6 1.914(4) . ? Ru1 C10 2.019(4) . ? Ru1 N9 2.038(3) . ? Ru1 N10 2.039(4) . ? Ru1 N7 2.151(3) . ? Ru1 N1 2.167(4) . ? C1 N1 1.338(5) . ? C1 C2 1.380(6) . ? C2 C3 1.372(7) . ? C3 C4 1.382(7) . ? C4 C5 1.383(6) . ? C5 N1 1.349(6) . ? C5 N2 1.402(6) . ? C6 N3 1.336(5) . ? C6 N2 1.371(6) . ? C7 C8 1.335(7) . ? C7 N2 1.393(6) . ? C8 N3 1.396(6) . ? C9 N3 1.437(6) . ? C9 N4 1.463(5) . ? C10 N5 1.369(5) . ? C10 N4 1.371(5) . ? C11 C12 1.325(7) . ? C11 N4 1.391(6) . ? C12 N5 1.387(6) . ? C13 N6 1.319(6) . ? C13 C14 1.382(6) . ? C13 N5 1.437(6) . ? C14 C15 1.383(7) . ? C15 C16 1.370(7) . ? C16 C17 1.372(7) . ? C17 N6 1.336(6) . ? C18 C19 1.468(7) . ? C19 N7 1.323(6) . ? C19 C20 1.417(6) . ? C20 C21 1.355(7) . ? C21 N8 1.385(6) . ? C21 C22 1.494(6) . ? C23 N9 1.273(5) . ? C23 N8 1.401(6) . ? C23 C24 1.482(6) . ? C25 N10 1.141(6) . ? C25 C26 1.452(6) . ? F1 P1 1.596(3) . ? F2 P1 1.602(3) . ? F3 P1 1.600(3) . ? F4 P1 1.603(3) . ? F5 P1 1.593(3) . ? F6 P1 1.602(3) . ? F7 P2 1.576(3) . ? F8 P2 1.526(4) . ? F9 P2 1.590(3) . ? F10 P2 1.576(4) . ? F11 P2 1.542(4) . ? F12 P2 1.569(5) . ? N7 N8 1.393(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 C6 Ru1 C10 86.85(17) . . ? C6 Ru1 N9 97.57(16) . . ? C10 Ru1 N9 95.56(15) . . ? C6 Ru1 N10 86.20(16) . . ? C10 Ru1 N10 87.38(15) . . ? N9 Ru1 N10 175.33(14) . . ? C6 Ru1 N7 168.51(16) . . ? C10 Ru1 N7 102.16(15) . . ? N9 Ru1 N7 74.69(14) . . ? N10 Ru1 N7 101.17(14) . . ? C6 Ru1 N1 77.44(15) . . ? C10 Ru1 N1 164.14(15) . . ? N9 Ru1 N1 88.72(13) . . ? N10 Ru1 N1 89.41(13) . . ? N7 Ru1 N1 93.70(13) . . ? N1 C1 C2 123.2(4) . . ? C3 C2 C1 118.9(4) . . ? C2 C3 C4 119.7(4) . . ? C3 C4 C5 117.6(4) . . ? N1 C5 C4 123.8(4) . . ? N1 C5 N2 113.3(4) . . ? C4 C5 N2 122.9(4) . . ? N3 C6 N2 104.4(4) . . ? N3 C6 Ru1 136.5(3) . . ? N2 C6 Ru1 118.9(3) . . ? C8 C7 N2 106.1(4) . . ? C7 C8 N3 107.4(4) . . ? N3 C9 N4 113.6(3) . . ? N5 C10 N4 102.3(3) . . ? N5 C10 Ru1 132.2(3) . . ? N4 C10 Ru1 124.9(3) . . ? C12 C11 N4 107.2(4) . . ? C11 C12 N5 106.6(4) . . ? N6 C13 C14 124.0(4) . . ? N6 C13 N5 116.3(4) . . ? C14 C13 N5 119.4(4) . . ? C13 C14 C15 118.1(5) . . ? C16 C15 C14 118.8(4) . . ? C15 C16 C17 118.5(5) . . ? N6 C17 C16 124.1(5) . . ? N7 C19 C20 109.4(4) . . ? N7 C19 C18 122.3(4) . . ? C20 C19 C18 128.3(4) . . ? C21 C20 C19 108.0(4) . . ? C20 C21 N8 106.0(4) . . ? C20 C21 C22 128.8(4) . . ? N8 C21 C22 125.2(4) . . ? N9 C23 N8 114.1(4) . . ? N9 C23 C24 125.4(4) . . ? N8 C23 C24 120.4(4) . . ? N10 C25 C26 178.4(5) . . ? C1 N1 C5 116.8(4) . . ? C1 N1 Ru1 130.0(3) . . ? C5 N1 Ru1 113.1(3) . . ? C6 N2 C7 110.9(4) . . ? C6 N2 C5 117.1(4) . . ? C7 N2 C5 132.0(4) . . ? C6 N3 C8 111.1(4) . . ? C6 N3 C9 124.0(4) . . ? C8 N3 C9 124.7(4) . . ? C10 N4 C11 111.6(4) . . ? C10 N4 C9 130.4(4) . . ? C11 N4 C9 117.6(4) . . ? C10 N5 C12 112.2(4) . . ? C10 N5 C13 126.5(4) . . ? C12 N5 C13 121.2(4) . . ? C13 N6 C17 116.5(4) . . ? C19 N7 N8 106.5(3) . . ? C19 N7 Ru1 141.2(3) . . ? N8 N7 Ru1 112.3(3) . . ? C21 N8 N7 110.0(4) . . ? C21 N8 C23 133.5(4) . . ? N7 N8 C23 116.3(3) . . ? C23 N9 Ru1 122.4(3) . . ? C25 N10 Ru1 172.8(3) . . ? F5 P1 F1 90.79(18) . . ? F5 P1 F3 89.84(17) . . ? F1 P1 F3 90.16(18) . . ? F5 P1 F6 90.27(16) . . ? F1 P1 F6 90.15(17) . . ? F3 P1 F6 179.7(2) . . ? F5 P1 F2 179.51(19) . . ? F1 P1 F2 89.62(18) . . ? F3 P1 F2 90.44(17) . . ? F6 P1 F2 89.46(16) . . ? F5 P1 F4 89.85(16) . . ? F1 P1 F4 179.14(18) . . ? F3 P1 F4 90.41(17) . . ? F6 P1 F4 89.27(15) . . ? F2 P1 F4 89.74(16) . . ? F8 P2 F11 90.6(4) . . ? F8 P2 F12 178.7(4) . . ? F11 P2 F12 90.4(4) . . ? F8 P2 F10 92.1(3) . . ? F11 P2 F10 177.1(4) . . ? F12 P2 F10 86.8(3) . . ? F8 P2 F7 92.2(2) . . ? F11 P2 F7 91.5(2) . . ? F12 P2 F7 88.6(2) . . ? F10 P2 F7 89.3(2) . . ? F8 P2 F9 89.7(3) . . ? F11 P2 F9 88.3(2) . . ? F12 P2 F9 89.5(3) . . ? F10 P2 F9 90.8(2) . . ? F7 P2 F9 178.0(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.845 _refine_diff_density_min -1.086 _refine_diff_density_rms 0.112 #===END