# 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_name 'Wanzhi Chen' _publ_contact_author_email chenwzz@zju.edu.cn loop_ _publ_author_name 'Wanzhi Chen' 'Shaojin Gu' 'Bo Liu' 'Huayue Wu' 'Jiuxi Chen' data_080714b _database_code_depnum_ccdc_archive 'CCDC 832963' #TrackingRef '- Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H21 Cl F6 N7 P Ru' _chemical_formula_weight 700.98 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' 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' 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 8.6224(10) _cell_length_b 13.2160(15) _cell_length_c 13.6700(16) _cell_angle_alpha 73.4140(10) _cell_angle_beta 75.458(2) _cell_angle_gamma 74.0600(10) _cell_volume 1410.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4095 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.3 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7214 _exptl_absorpt_correction_T_max 0.7674 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7373 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4893 _reflns_number_gt 4142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0584P)^2^+3.8773P] 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 4893 _refine_ls_number_parameters 427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.066 _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 0.93629(5) 0.28780(3) 0.81030(3) 0.03135(14) Uani 1 1 d . . . Cl1 Cl 1.18724(14) 0.23659(9) 0.87608(9) 0.0380(3) Uani 1 1 d . . . F1 F 0.698(3) 0.7565(13) 0.5189(19) 0.172(13) Uani 0.56(2) 1 d P A 1 F2 F 0.418(2) 0.6794(17) 0.6897(10) 0.121(6) Uani 0.56(2) 1 d P A 1 F3 F 0.6209(17) 0.7449(18) 0.6897(13) 0.131(7) Uani 0.56(2) 1 d P A 1 F4 F 0.6721(19) 0.6059(10) 0.6194(13) 0.129(6) Uani 0.56(2) 1 d P A 1 F5 F 0.486(2) 0.693(2) 0.5261(13) 0.149(8) Uani 0.56(2) 1 d P A 1 F6 F 0.457(3) 0.8364(13) 0.5835(15) 0.171(9) Uani 0.56(2) 1 d P A 1 F1' F 0.7436(19) 0.712(2) 0.5732(17) 0.133(9) Uani 0.44(2) 1 d P A 2 F2' F 0.374(3) 0.733(2) 0.642(3) 0.153(9) Uani 0.44(2) 1 d P A 2 F3' F 0.584(3) 0.655(2) 0.7148(12) 0.145(11) Uani 0.44(2) 1 d P A 2 F4' F 0.540(3) 0.8246(17) 0.638(2) 0.131(9) Uani 0.44(2) 1 d P A 2 F5' F 0.542(4) 0.783(2) 0.4954(15) 0.160(11) Uani 0.44(2) 1 d P A 2 F6' F 0.572(3) 0.6167(14) 0.5737(17) 0.134(11) Uani 0.44(2) 1 d P A 2 N1 N 0.7431(5) 0.2539(3) 1.0142(3) 0.0405(10) Uani 1 1 d . . . N2 N 0.7874(5) 0.1000(3) 0.9757(3) 0.0419(10) Uani 1 1 d . . . N3 N 0.8460(5) 0.3907(3) 0.9014(3) 0.0308(8) Uani 1 1 d . . . N4 N 1.0167(4) 0.4329(3) 0.7104(3) 0.0313(8) Uani 1 1 d . . . N5 N 0.6121(6) 0.0961(4) 0.8214(4) 0.0596(13) Uani 1 1 d . . . N6 N 0.7307(5) 0.3362(3) 0.7483(3) 0.0328(9) Uani 1 1 d . . . N7 N 1.0380(5) 0.1799(3) 0.7165(3) 0.0364(9) Uani 1 1 d . . . P1 P 0.5580(2) 0.72065(14) 0.60544(13) 0.0583(4) Uani 1 1 d . . . C1 C 0.8235(6) 0.1986(4) 0.9356(3) 0.0336(10) Uani 1 1 d . . . C2 C 0.6889(8) 0.0937(5) 1.0742(4) 0.0613(17) Uani 1 1 d . . . H2 H 0.6488 0.0338 1.1158 0.074 Uiso 1 1 calc R . . C3 C 0.6624(8) 0.1879(5) 1.0983(4) 0.0607(16) Uani 1 1 d . . . H3 H 0.6014 0.2064 1.1596 0.073 Uiso 1 1 calc R . . C4 C 0.7592(6) 0.3608(4) 0.9957(4) 0.0380(11) Uani 1 1 d . . . C5 C 0.7000(8) 0.4320(5) 1.0633(5) 0.0596(16) Uani 1 1 d . . . H5 H 0.6393 0.4112 1.1293 0.071 Uiso 1 1 calc R . . C6 C 0.7351(8) 0.5330(5) 1.0283(5) 0.0576(16) Uani 1 1 d . . . H6 H 0.6947 0.5818 1.0709 0.069 Uiso 1 1 calc R . . C7 C 0.8310(7) 0.5648(4) 0.9292(4) 0.0480(13) Uani 1 1 d . . . C8 C 0.8821(6) 0.4892(4) 0.8672(4) 0.0352(10) Uani 1 1 d . . . C9 C 0.9748(6) 0.5121(4) 0.7642(4) 0.0350(10) Uani 1 1 d . . . C10 C 1.0152(6) 0.6139(4) 0.7233(4) 0.0427(12) Uani 1 1 d . . . C11 C 1.1004(7) 0.6330(4) 0.6203(5) 0.0509(14) Uani 1 1 d . . . H11 H 1.1320 0.6985 0.5894 0.061 Uiso 1 1 calc R . . C12 C 1.1362(6) 0.5564(5) 0.5665(4) 0.0476(13) Uani 1 1 d . . . H12 H 1.1888 0.5703 0.4973 0.057 Uiso 1 1 calc R . . C13 C 1.0955(6) 0.4557(4) 0.6133(4) 0.0385(11) Uani 1 1 d . . . H13 H 1.1248 0.4032 0.5748 0.046 Uiso 1 1 calc R . . C14 C 0.8788(8) 0.6670(4) 0.8856(5) 0.0582(16) Uani 1 1 d . . . H14 H 0.8491 0.7186 0.9250 0.070 Uiso 1 1 calc R . . C15 C 0.9655(8) 0.6884(4) 0.7889(5) 0.0571(16) Uani 1 1 d . . . H15 H 0.9948 0.7551 0.7632 0.069 Uiso 1 1 calc R . . C16 C 0.8490(7) 0.0123(4) 0.9212(4) 0.0456(13) Uani 1 1 d . . . H16A H 0.8404 -0.0556 0.9714 0.055 Uiso 1 1 calc R . . H16B H 0.9646 0.0093 0.8920 0.055 Uiso 1 1 calc R . . C17 C 0.7609(6) 0.0223(4) 0.8351(4) 0.0410(12) Uani 1 1 d . . . C18 C 0.8359(7) -0.0449(4) 0.7742(4) 0.0474(13) Uani 1 1 d . . . H18 H 0.9342 -0.0935 0.7856 0.057 Uiso 1 1 calc R . . C19 C 0.7674(9) -0.0416(6) 0.6957(6) 0.078(2) Uani 1 1 d . . . H19 H 0.8188 -0.0906 0.6541 0.093 Uiso 1 1 calc R . . C20 C 0.6245(8) 0.0304(5) 0.6730(5) 0.0632(17) Uani 1 1 d . . . H20 H 0.5824 0.0317 0.6162 0.076 Uiso 1 1 calc R . . C21 C 0.5470(7) 0.0993(5) 0.7359(5) 0.0499(13) Uani 1 1 d . . . H21 H 0.4504 0.1488 0.7223 0.060 Uiso 1 1 calc R . . C22 C 0.6134(6) 0.3654(4) 0.7164(4) 0.0391(11) Uani 1 1 d . . . C23 C 0.4636(8) 0.4011(6) 0.6766(5) 0.0661(18) Uani 1 1 d . . . H23A H 0.3929 0.3517 0.7123 0.099 Uiso 1 1 calc R . . H23B H 0.4878 0.4033 0.6036 0.099 Uiso 1 1 calc R . . H23C H 0.4098 0.4720 0.6873 0.099 Uiso 1 1 calc R . . C24 C 1.1007(7) 0.1195(4) 0.6679(4) 0.0494(13) Uani 1 1 d . . . C25 C 1.1792(10) 0.0378(6) 0.6068(6) 0.089(3) Uani 1 1 d . . . H25A H 1.2337 -0.0264 0.6498 0.134 Uiso 1 1 calc R . . H25B H 1.2580 0.0656 0.5491 0.134 Uiso 1 1 calc R . . H25C H 1.0973 0.0208 0.5816 0.134 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0360(2) 0.0316(2) 0.0279(2) -0.00997(15) -0.00384(15) -0.00846(16) Cl1 0.0369(6) 0.0385(6) 0.0392(6) -0.0100(5) -0.0111(5) -0.0047(5) F1 0.149(19) 0.101(10) 0.18(2) 0.007(11) 0.088(16) -0.036(11) F2 0.111(14) 0.173(16) 0.073(8) -0.010(8) 0.014(7) -0.071(12) F3 0.130(10) 0.163(18) 0.140(12) -0.064(13) -0.064(9) -0.031(11) F4 0.131(11) 0.091(8) 0.152(13) -0.018(8) -0.057(9) 0.015(7) F5 0.178(14) 0.19(2) 0.110(11) -0.063(13) -0.065(10) -0.023(13) F6 0.174(17) 0.112(11) 0.163(17) -0.031(10) -0.031(12) 0.071(11) F1' 0.064(8) 0.16(2) 0.123(15) 0.002(12) -0.014(9) 0.014(10) F2' 0.094(11) 0.18(2) 0.18(3) -0.009(18) -0.028(14) -0.047(13) F3' 0.143(18) 0.16(2) 0.084(10) 0.011(10) -0.007(9) -0.001(13) F4' 0.15(2) 0.093(14) 0.17(2) -0.071(14) -0.007(14) -0.039(13) F5' 0.19(2) 0.15(2) 0.111(14) 0.022(13) -0.064(15) -0.026(18) F6' 0.20(3) 0.077(11) 0.130(16) -0.041(10) 0.004(15) -0.051(13) N1 0.046(2) 0.050(3) 0.027(2) -0.0120(18) 0.0017(18) -0.018(2) N2 0.053(3) 0.042(2) 0.032(2) 0.0014(18) -0.0113(19) -0.022(2) N3 0.034(2) 0.031(2) 0.030(2) -0.0129(16) -0.0074(16) -0.0046(16) N4 0.0279(19) 0.033(2) 0.035(2) -0.0078(16) -0.0097(16) -0.0062(16) N5 0.059(3) 0.058(3) 0.066(3) -0.016(3) -0.007(3) -0.020(3) N6 0.044(2) 0.031(2) 0.0252(19) -0.0070(15) -0.0027(18) -0.0133(18) N7 0.044(2) 0.035(2) 0.033(2) -0.0130(18) -0.0031(18) -0.0116(18) P1 0.0634(10) 0.0569(9) 0.0549(9) -0.0212(8) 0.0019(8) -0.0171(8) C1 0.037(3) 0.038(3) 0.028(2) -0.0077(19) -0.0073(19) -0.010(2) C2 0.080(4) 0.069(4) 0.034(3) 0.004(3) 0.001(3) -0.042(4) C3 0.070(4) 0.075(4) 0.034(3) -0.009(3) 0.010(3) -0.034(3) C4 0.040(3) 0.045(3) 0.030(2) -0.015(2) -0.005(2) -0.006(2) C5 0.063(4) 0.074(4) 0.038(3) -0.028(3) -0.003(3) -0.002(3) C6 0.074(4) 0.053(3) 0.053(4) -0.036(3) -0.015(3) 0.002(3) C7 0.057(3) 0.041(3) 0.053(3) -0.024(2) -0.021(3) 0.001(2) C8 0.039(3) 0.031(2) 0.040(3) -0.012(2) -0.015(2) -0.002(2) C9 0.037(3) 0.031(2) 0.040(3) -0.005(2) -0.015(2) -0.008(2) C10 0.043(3) 0.033(3) 0.056(3) -0.002(2) -0.026(3) -0.010(2) C11 0.046(3) 0.039(3) 0.066(4) 0.009(3) -0.026(3) -0.016(2) C12 0.039(3) 0.055(3) 0.043(3) 0.004(3) -0.008(2) -0.017(2) C13 0.033(3) 0.044(3) 0.038(3) -0.004(2) -0.012(2) -0.009(2) C14 0.074(4) 0.036(3) 0.077(5) -0.028(3) -0.033(4) 0.000(3) C15 0.071(4) 0.030(3) 0.080(5) -0.009(3) -0.038(4) -0.009(3) C16 0.060(3) 0.028(2) 0.051(3) -0.001(2) -0.022(3) -0.011(2) C17 0.048(3) 0.030(2) 0.049(3) -0.001(2) -0.016(2) -0.018(2) C18 0.049(3) 0.034(3) 0.066(4) -0.024(3) -0.032(3) 0.012(2) C19 0.086(5) 0.068(4) 0.092(5) -0.049(4) -0.037(4) 0.013(4) C20 0.068(4) 0.071(4) 0.061(4) -0.025(3) -0.028(3) -0.009(3) C21 0.043(3) 0.048(3) 0.063(4) -0.013(3) -0.021(3) -0.007(2) C22 0.041(3) 0.041(3) 0.035(3) -0.001(2) -0.007(2) -0.017(2) C23 0.050(4) 0.074(4) 0.076(4) -0.001(3) -0.025(3) -0.020(3) C24 0.061(4) 0.046(3) 0.047(3) -0.022(3) 0.002(3) -0.018(3) C25 0.101(6) 0.075(5) 0.101(6) -0.066(5) 0.033(5) -0.035(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N3 1.976(4) . ? Ru1 C1 1.978(5) . ? Ru1 N6 2.023(4) . ? Ru1 N7 2.059(4) . ? Ru1 N4 2.187(4) . ? Ru1 Cl1 2.4029(12) . ? F1 P1 1.533(12) . ? F2 P1 1.544(12) . ? F3 P1 1.531(10) . ? F4 P1 1.554(11) . ? F5 P1 1.543(11) . ? F6 P1 1.526(12) . ? F1' P1 1.531(18) . ? F2' P1 1.52(2) . ? F3' P1 1.535(14) . ? F4' P1 1.521(13) . ? F5' P1 1.516(16) . ? F6' P1 1.521(13) . ? N1 C3 1.387(7) . ? N1 C4 1.402(6) . ? N1 C1 1.402(6) . ? N2 C1 1.350(6) . ? N2 C2 1.394(7) . ? N2 C16 1.462(7) . ? N3 C4 1.328(6) . ? N3 C8 1.347(6) . ? N4 C13 1.321(6) . ? N4 C9 1.366(6) . ? N5 C17 1.401(7) . ? N5 C21 1.404(7) . ? N6 C22 1.128(6) . ? N7 C24 1.121(6) . ? C2 C3 1.322(9) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.413(7) . ? C5 C6 1.373(9) . ? C5 H5 0.9300 . ? C6 C7 1.414(8) . ? C6 H6 0.9300 . ? C7 C8 1.401(7) . ? C7 C14 1.439(8) . ? C8 C9 1.428(7) . ? C9 C10 1.404(7) . ? C10 C11 1.403(8) . ? C10 C15 1.427(8) . ? C11 C12 1.342(8) . ? C11 H11 0.9300 . ? C12 C13 1.401(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.339(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.513(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.318(7) . ? C18 C19 1.334(8) . ? C18 H18 0.9300 . ? C19 C20 1.378(9) . ? C19 H19 0.9300 . ? C20 C21 1.356(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.435(8) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.466(7) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ru1 C1 78.45(17) . . ? N3 Ru1 N6 91.35(15) . . ? C1 Ru1 N6 90.53(17) . . ? N3 Ru1 N7 178.09(15) . . ? C1 Ru1 N7 102.00(17) . . ? N6 Ru1 N7 90.51(15) . . ? N3 Ru1 N4 78.64(15) . . ? C1 Ru1 N4 157.06(17) . . ? N6 Ru1 N4 88.82(14) . . ? N7 Ru1 N4 100.93(15) . . ? N3 Ru1 Cl1 89.08(11) . . ? C1 Ru1 Cl1 92.51(14) . . ? N6 Ru1 Cl1 176.95(11) . . ? N7 Ru1 Cl1 89.04(12) . . ? N4 Ru1 Cl1 88.31(10) . . ? C3 N1 C4 132.5(4) . . ? C3 N1 C1 110.8(4) . . ? C4 N1 C1 116.8(4) . . ? C1 N2 C2 111.4(5) . . ? C1 N2 C16 122.9(4) . . ? C2 N2 C16 125.7(4) . . ? C4 N3 C8 121.3(4) . . ? C4 N3 Ru1 120.4(3) . . ? C8 N3 Ru1 118.1(3) . . ? C13 N4 C9 117.3(4) . . ? C13 N4 Ru1 132.9(3) . . ? C9 N4 Ru1 109.7(3) . . ? C17 N5 C21 116.9(5) . . ? C22 N6 Ru1 177.5(4) . . ? C24 N7 Ru1 176.2(4) . . ? F5' P1 F2' 93.4(16) . . ? F5' P1 F6' 89.0(12) . . ? F2' P1 F6' 91.4(14) . . ? F5' P1 F4' 91.2(14) . . ? F2' P1 F4' 87.4(13) . . ? F6' P1 F4' 178.8(12) . . ? F5' P1 F6 59.0(10) . . ? F2' P1 F6 64.7(11) . . ? F6' P1 F6 136.5(15) . . ? F4' P1 F6 42.9(9) . . ? F5' P1 F3 131.7(14) . . ? F2' P1 F3 105.9(12) . . ? F6' P1 F3 132.9(14) . . ? F4' P1 F3 47.5(9) . . ? F6 P1 F3 89.9(10) . . ? F5' P1 F1' 88.3(11) . . ? F2' P1 F1' 176.5(15) . . ? F6' P1 F1' 91.7(13) . . ? F4' P1 F1' 89.5(13) . . ? F6 P1 F1' 113.8(13) . . ? F3 P1 F1' 70.7(10) . . ? F5' P1 F1 54.1(11) . . ? F2' P1 F1 146.7(14) . . ? F6' P1 F1 94.7(10) . . ? F4' P1 F1 86.4(10) . . ? F6 P1 F1 89.2(10) . . ? F3 P1 F1 93.6(13) . . ? F1' P1 F1 34.5(8) . . ? F5' P1 F3' 177.0(13) . . ? F2' P1 F3' 89.4(12) . . ? F6' P1 F3' 90.0(14) . . ? F4' P1 F3' 89.8(12) . . ? F6 P1 F3' 123.3(10) . . ? F3 P1 F3' 48.0(9) . . ? F1' P1 F3' 89.0(11) . . ? F1 P1 F3' 123.2(14) . . ? F5' P1 F5 51.2(10) . . ? F2' P1 F5 71.1(12) . . ? F6' P1 F5 46.2(9) . . ? F4' P1 F5 133.4(15) . . ? F6 P1 F5 90.6(13) . . ? F3 P1 F5 176.3(10) . . ? F1' P1 F5 112.3(11) . . ? F1 P1 F5 90.0(12) . . ? F3' P1 F5 129.2(15) . . ? F5' P1 F2 125.2(13) . . ? F2' P1 F2 33.5(8) . . ? F6' P1 F2 82.1(9) . . ? F4' P1 F2 96.8(10) . . ? F6 P1 F2 92.8(10) . . ? F3 P1 F2 88.9(8) . . ? F1' P1 F2 145.6(10) . . ? F1 P1 F2 176.8(11) . . ? F3' P1 F2 57.4(8) . . ? F5 P1 F2 87.5(9) . . ? F5' P1 F4 117.2(12) . . ? F2' P1 F4 119.6(12) . . ? F6' P1 F4 43.6(10) . . ? F4' P1 F4 137.1(13) . . ? F6 P1 F4 175.1(10) . . ? F3 P1 F4 91.0(10) . . ? F1' P1 F4 62.1(10) . . ? F1 P1 F4 85.9(8) . . ? F3' P1 F4 60.4(8) . . ? F5 P1 F4 88.8(9) . . ? F2 P1 F4 92.0(10) . . ? N2 C1 N1 103.0(4) . . ? N2 C1 Ru1 143.2(4) . . ? N1 C1 Ru1 113.7(3) . . ? C3 C2 N2 108.0(5) . . ? C3 C2 H2 126.0 . . ? N2 C2 H2 126.0 . . ? C2 C3 N1 106.8(5) . . ? C2 C3 H3 126.6 . . ? N1 C3 H3 126.6 . . ? N3 C4 N1 110.5(4) . . ? N3 C4 C5 121.0(5) . . ? N1 C4 C5 128.4(5) . . ? C6 C5 C4 117.8(5) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.1 . . ? C5 C6 C7 121.7(5) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C8 C7 C6 116.3(5) . . ? C8 C7 C14 117.2(5) . . ? C6 C7 C14 126.5(5) . . ? N3 C8 C7 121.8(5) . . ? N3 C8 C9 116.1(4) . . ? C7 C8 C9 122.1(5) . . ? N4 C9 C10 123.9(5) . . ? N4 C9 C8 117.1(4) . . ? C10 C9 C8 119.0(4) . . ? C11 C10 C9 116.3(5) . . ? C11 C10 C15 125.9(5) . . ? C9 C10 C15 117.9(5) . . ? C12 C11 C10 119.7(5) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 120.8(5) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? N4 C13 C12 122.0(5) . . ? N4 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C15 C14 C7 120.6(5) . . ? C15 C14 H14 119.7 . . ? C7 C14 H14 119.7 . . ? C14 C15 C10 123.2(5) . . ? C14 C15 H15 118.4 . . ? C10 C15 H15 118.4 . . ? N2 C16 C17 114.8(4) . . ? N2 C16 H16A 108.6 . . ? C17 C16 H16A 108.6 . . ? N2 C16 H16B 108.6 . . ? C17 C16 H16B 108.6 . . ? H16A C16 H16B 107.5 . . ? C18 C17 N5 122.8(5) . . ? C18 C17 C16 114.2(5) . . ? N5 C17 C16 123.1(5) . . ? C17 C18 C19 118.4(5) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C18 C19 C20 123.5(6) . . ? C18 C19 H19 118.2 . . ? C20 C19 H19 118.2 . . ? C21 C20 C19 118.1(6) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C20 C21 N5 120.2(5) . . ? C20 C21 H21 119.9 . . ? N5 C21 H21 119.9 . . ? N6 C22 C23 179.2(6) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N7 C24 C25 178.0(6) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ru1 N3 C4 0.0(4) . . . . ? N6 Ru1 N3 C4 90.2(4) . . . . ? N7 Ru1 N3 C4 -104(5) . . . . ? N4 Ru1 N3 C4 178.8(4) . . . . ? Cl1 Ru1 N3 C4 -92.8(3) . . . . ? C1 Ru1 N3 C8 176.6(4) . . . . ? N6 Ru1 N3 C8 -93.1(3) . . . . ? N7 Ru1 N3 C8 73(5) . . . . ? N4 Ru1 N3 C8 -4.6(3) . . . . ? Cl1 Ru1 N3 C8 83.9(3) . . . . ? N3 Ru1 N4 C13 -176.3(4) . . . . ? C1 Ru1 N4 C13 -173.3(4) . . . . ? N6 Ru1 N4 C13 -84.7(4) . . . . ? N7 Ru1 N4 C13 5.6(4) . . . . ? Cl1 Ru1 N4 C13 94.3(4) . . . . ? N3 Ru1 N4 C9 4.5(3) . . . . ? C1 Ru1 N4 C9 7.5(6) . . . . ? N6 Ru1 N4 C9 96.1(3) . . . . ? N7 Ru1 N4 C9 -173.6(3) . . . . ? Cl1 Ru1 N4 C9 -84.9(3) . . . . ? N3 Ru1 N6 C22 -9(9) . . . . ? C1 Ru1 N6 C22 70(9) . . . . ? N7 Ru1 N6 C22 172(9) . . . . ? N4 Ru1 N6 C22 -87(9) . . . . ? Cl1 Ru1 N6 C22 -107(9) . . . . ? N3 Ru1 N7 C24 15(10) . . . . ? C1 Ru1 N7 C24 -89(7) . . . . ? N6 Ru1 N7 C24 -179(100) . . . . ? N4 Ru1 N7 C24 92(7) . . . . ? Cl1 Ru1 N7 C24 4(7) . . . . ? C2 N2 C1 N1 0.2(6) . . . . ? C16 N2 C1 N1 -178.6(4) . . . . ? C2 N2 C1 Ru1 -176.6(5) . . . . ? C16 N2 C1 Ru1 4.6(9) . . . . ? C3 N1 C1 N2 0.1(6) . . . . ? C4 N1 C1 N2 179.4(4) . . . . ? C3 N1 C1 Ru1 178.1(4) . . . . ? C4 N1 C1 Ru1 -2.7(5) . . . . ? N3 Ru1 C1 N2 178.1(6) . . . . ? N6 Ru1 C1 N2 86.8(6) . . . . ? N7 Ru1 C1 N2 -3.8(6) . . . . ? N4 Ru1 C1 N2 175.0(4) . . . . ? Cl1 Ru1 C1 N2 -93.4(6) . . . . ? N3 Ru1 C1 N1 1.4(3) . . . . ? N6 Ru1 C1 N1 -89.8(3) . . . . ? N7 Ru1 C1 N1 179.5(3) . . . . ? N4 Ru1 C1 N1 -1.6(6) . . . . ? Cl1 Ru1 C1 N1 90.0(3) . . . . ? C1 N2 C2 C3 -0.5(7) . . . . ? C16 N2 C2 C3 178.2(5) . . . . ? N2 C2 C3 N1 0.6(7) . . . . ? C4 N1 C3 C2 -179.5(6) . . . . ? C1 N1 C3 C2 -0.5(7) . . . . ? C8 N3 C4 N1 -177.9(4) . . . . ? Ru1 N3 C4 N1 -1.4(5) . . . . ? C8 N3 C4 C5 0.7(7) . . . . ? Ru1 N3 C4 C5 177.2(4) . . . . ? C3 N1 C4 N3 -178.4(5) . . . . ? C1 N1 C4 N3 2.6(6) . . . . ? C3 N1 C4 C5 3.2(10) . . . . ? C1 N1 C4 C5 -175.8(5) . . . . ? N3 C4 C5 C6 0.0(8) . . . . ? N1 C4 C5 C6 178.3(5) . . . . ? C4 C5 C6 C7 -1.8(9) . . . . ? C5 C6 C7 C8 2.7(9) . . . . ? C5 C6 C7 C14 -178.4(6) . . . . ? C4 N3 C8 C7 0.4(7) . . . . ? Ru1 N3 C8 C7 -176.2(4) . . . . ? C4 N3 C8 C9 -179.5(4) . . . . ? Ru1 N3 C8 C9 3.9(5) . . . . ? C6 C7 C8 N3 -2.0(7) . . . . ? C14 C7 C8 N3 179.0(5) . . . . ? C6 C7 C8 C9 177.9(5) . . . . ? C14 C7 C8 C9 -1.2(7) . . . . ? C13 N4 C9 C10 -2.1(7) . . . . ? Ru1 N4 C9 C10 177.3(4) . . . . ? C13 N4 C9 C8 176.7(4) . . . . ? Ru1 N4 C9 C8 -3.9(5) . . . . ? N3 C8 C9 N4 0.4(6) . . . . ? C7 C8 C9 N4 -179.4(4) . . . . ? N3 C8 C9 C10 179.3(4) . . . . ? C7 C8 C9 C10 -0.5(7) . . . . ? N4 C9 C10 C11 1.4(7) . . . . ? C8 C9 C10 C11 -177.4(4) . . . . ? N4 C9 C10 C15 -179.1(4) . . . . ? C8 C9 C10 C15 2.1(7) . . . . ? C9 C10 C11 C12 1.0(7) . . . . ? C15 C10 C11 C12 -178.4(5) . . . . ? C10 C11 C12 C13 -2.7(8) . . . . ? C9 N4 C13 C12 0.4(7) . . . . ? Ru1 N4 C13 C12 -178.8(3) . . . . ? C11 C12 C13 N4 2.0(8) . . . . ? C8 C7 C14 C15 1.3(8) . . . . ? C6 C7 C14 C15 -177.6(6) . . . . ? C7 C14 C15 C10 0.3(9) . . . . ? C11 C10 C15 C14 177.4(5) . . . . ? C9 C10 C15 C14 -2.0(8) . . . . ? C1 N2 C16 C17 -77.4(6) . . . . ? C2 N2 C16 C17 104.0(6) . . . . ? C21 N5 C17 C18 -2.6(8) . . . . ? C21 N5 C17 C16 177.8(5) . . . . ? N2 C16 C17 C18 167.8(5) . . . . ? N2 C16 C17 N5 -12.5(7) . . . . ? N5 C17 C18 C19 0.6(9) . . . . ? C16 C17 C18 C19 -179.7(6) . . . . ? C17 C18 C19 C20 1.9(12) . . . . ? C18 C19 C20 C21 -2.1(12) . . . . ? C19 C20 C21 N5 -0.1(10) . . . . ? C17 N5 C21 C20 2.3(8) . . . . ? Ru1 N6 C22 C23 -98(48) . . . . ? Ru1 N7 C24 C25 99(21) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.959 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.097 #===END data_100521_gsjr1224-sr _database_code_depnum_ccdc_archive 'CCDC 832964' #TrackingRef '- Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H48 Ag2 Cl2 F24 N16 P4 Ru2' _chemical_formula_weight 1989.74 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.3914(5) _cell_length_b 12.4815(5) _cell_length_c 14.0312(5) _cell_angle_alpha 64.465(4) _cell_angle_beta 84.530(3) _cell_angle_gamma 88.815(3) _cell_volume 1948.72(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4797 _cell_measurement_theta_min 3.2265 _cell_measurement_theta_max 29.2730 _exptl_crystal_description PLATELET _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 1.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7140 _exptl_absorpt_correction_T_max 0.8859 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17182 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6861 _reflns_number_gt 3962 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro(Oxford Diffraction Ltd.)' _computing_cell_refinement 'CrysAlisPro(Oxford Diffraction Ltd.)' _computing_data_reduction 'CrysAlisPro(Oxford Diffraction Ltd.)' _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^)+(0.0850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6861 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0986 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1648 _refine_ls_wR_factor_gt 0.1534 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 218 39 ' ' _platon_squeeze_details ; ; 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 F20 F 0.3482(8) 0.2126(9) 0.1604(7) 0.201(3) Uiso 1 1 d . . . Ru1 Ru 0.71070(4) 0.75514(5) 0.39980(4) 0.0475(2) Uani 1 1 d . . . Ag1 Ag 0.53938(5) 0.53692(6) 0.36337(5) 0.0741(2) Uani 1 1 d . . . Cl1 Cl 0.64966(13) 0.54995(16) 0.49873(13) 0.0589(5) Uani 1 1 d . . . N1 N 0.5652(5) 0.8038(5) 0.4502(4) 0.0584(15) Uani 1 1 d . . . N3 N 0.6206(6) 0.7884(5) 0.1856(5) 0.0689(17) Uani 1 1 d . . . N4 N 0.7799(6) 0.7279(6) 0.2125(5) 0.0642(16) Uani 1 1 d . . . N5 N 0.8542(4) 0.7047(5) 0.3603(5) 0.0575(15) Uani 1 1 d . . . N6 N 0.7998(4) 0.7305(5) 0.5341(4) 0.0541(14) Uani 1 1 d . . . N7 N 0.7614(5) 0.9233(6) 0.3254(5) 0.0559(15) Uani 1 1 d . . . N8 N 0.6483(7) 0.4397(8) 0.2720(7) 0.109(3) Uani 1 1 d . . . N9 N 0.4345(5) 0.6350(7) 0.2291(5) 0.0697(17) Uani 1 1 d . . . C1 C 0.5141(8) 0.8246(7) 0.1963(7) 0.087(3) Uani 1 1 d . . . H1A H 0.5084 0.9069 0.1458 0.104 Uiso 1 1 calc R . . H1B H 0.4987 0.8203 0.2670 0.104 Uiso 1 1 calc R . . C2 C 0.7697(6) 0.7399(7) 0.6232(5) 0.064(2) Uani 1 1 d . . . H2 H 0.6999 0.7643 0.6334 0.077 Uiso 1 1 calc R . . C3 C 0.9023(6) 0.6949(6) 0.5202(6) 0.0585(18) Uani 1 1 d . . . C4 C 0.9404(10) 0.6834(8) 0.6875(8) 0.092(3) Uani 1 1 d . . . H4 H 0.9874 0.6692 0.7393 0.111 Uiso 1 1 calc R . . C5 C 0.9329(5) 0.6826(6) 0.4280(6) 0.0588(19) Uani 1 1 d . . . C6 C 1.0331(7) 0.6478(7) 0.4035(8) 0.079(2) Uani 1 1 d . . . C8 C 0.8712(8) 0.6965(7) 0.2674(7) 0.073(2) Uani 1 1 d . . . C10 C 0.7699(9) 0.7405(9) 0.1121(7) 0.089(3) Uani 1 1 d . . . H10 H 0.8217 0.7272 0.0662 0.107 Uiso 1 1 calc R . . C11 C 0.9755(8) 0.6609(7) 0.2400(8) 0.093(3) Uani 1 1 d . . . H11 H 0.9906 0.6531 0.1771 0.112 Uiso 1 1 calc R . . C12 C 0.6895(6) 0.7584(6) 0.2582(5) 0.0565(18) Uani 1 1 d . . . C14 C 0.7924(6) 1.0205(8) 0.2783(7) 0.073(2) Uani 1 1 d . . . C15 C 0.8339(9) 1.1426(8) 0.2214(9) 0.117(4) Uani 1 1 d . . . H15A H 0.8913 1.1547 0.2573 0.175 Uiso 1 1 calc R . . H15B H 0.7765 1.1962 0.2190 0.175 Uiso 1 1 calc R . . H15C H 0.8611 1.1571 0.1504 0.175 Uiso 1 1 calc R . . C17 C 0.4867(6) 0.8277(7) 0.4854(6) 0.066(2) Uani 1 1 d . . . C20 C 0.4278(7) 0.7491(8) 0.1784(6) 0.072(2) Uani 1 1 d . . . C21 C 0.3451(8) 0.7989(10) 0.1108(7) 0.096(3) Uani 1 1 d . . . H21 H 0.3385 0.8810 0.0780 0.115 Uiso 1 1 calc R . . C22 C 0.2760(7) 0.7302(12) 0.0931(7) 0.096(3) Uani 1 1 d . . . H22 H 0.2227 0.7639 0.0471 0.115 Uiso 1 1 calc R . . C23 C 0.2846(7) 0.6130(11) 0.1422(7) 0.091(3) Uani 1 1 d . . . H23 H 0.2368 0.5636 0.1316 0.110 Uiso 1 1 calc R . . C24 C 0.3663(7) 0.5647(9) 0.2098(6) 0.081(2) Uani 1 1 d . . . H24 H 0.3740 0.4828 0.2422 0.097 Uiso 1 1 calc R . . C25 C 1.0537(8) 0.6384(8) 0.3109(11) 0.109(4) Uani 1 1 d . . . H25 H 1.1224 0.6162 0.2941 0.131 Uiso 1 1 calc R . . C50 C 0.6585(8) 0.4833(9) 0.0792(7) 0.095(3) Uani 1 1 d . . . H50A H 0.6592 0.5678 0.0377 0.143 Uiso 1 1 calc R . . H50B H 0.5965 0.4485 0.0662 0.143 Uiso 1 1 calc R . . H50C H 0.7234 0.4512 0.0597 0.143 Uiso 1 1 calc R . . C52 C 0.6532(7) 0.4574(8) 0.1876(8) 0.078(2) Uani 1 1 d . . . C54 C 0.6715(11) 0.7753(8) 0.0960(6) 0.094(3) Uani 1 1 d . . . H54 H 0.6389 0.7897 0.0347 0.112 Uiso 1 1 calc R . . C60 C 0.3881(7) 0.8668(9) 0.5274(8) 0.107(3) Uani 1 1 d . . . H60A H 0.4079 0.9100 0.5657 0.161 Uiso 1 1 calc R . . H60B H 0.3440 0.7987 0.5741 0.161 Uiso 1 1 calc R . . H60C H 0.3481 0.9171 0.4697 0.161 Uiso 1 1 calc R . . C70 C 0.9778(7) 0.6714(7) 0.5963(8) 0.077(2) Uani 1 1 d . . . C71 C 1.1123(8) 0.6244(8) 0.4808(11) 0.109(4) Uani 1 1 d . . . H71 H 1.1822 0.6022 0.4677 0.131 Uiso 1 1 calc R . . C75 C 0.8400(9) 0.7143(8) 0.7028(6) 0.086(3) Uani 1 1 d . . . H75 H 0.8161 0.7190 0.7657 0.103 Uiso 1 1 calc R . . C76 C 1.0839(8) 0.6350(8) 0.5693(11) 0.103(4) Uani 1 1 d . . . H76 H 1.1353 0.6181 0.6177 0.124 Uiso 1 1 calc R . . F1 F 0.5709(8) 0.1439(19) 0.2048(10) 0.407(12) Uani 1 1 d . . . F6 F 0.4972(7) 0.2743(7) 0.0700(5) 0.167(3) Uani 1 1 d . . . F8 F 0.4593(7) 0.2724(9) 0.2271(7) 0.209(4) Uani 1 1 d . . . F21 F 1.0687(6) 0.5578(9) 0.0523(7) 0.184(3) Uani 1 1 d . . . F11 F 0.9208(5) 0.4540(8) 0.1030(4) 0.172(3) Uani 1 1 d . . . F12 F 1.0775(6) 0.3951(7) 0.0483(5) 0.152(3) Uani 1 1 d . . . F13 F 0.4176(12) 0.0921(9) 0.2916(6) 0.267(6) Uani 1 1 d . . . F15 F -0.0546(9) 0.9472(7) 0.1140(9) 0.222(5) Uani 1 1 d . . . F90 F 0.1134(8) 0.9722(11) 0.0327(14) 0.277(7) Uani 1 1 d . . . F123 F -0.0096(7) 0.8775(6) -0.0033(8) 0.199(4) Uani 1 1 d . . . P3 P 1.0000 0.5000 0.0000 0.0684(8) Uani 1 2 d S . . P4 P 0.0000 1.0000 0.0000 0.137(2) Uani 1 2 d S . . P5 P 0.4639(2) 0.1768(2) 0.18753(19) 0.0862(7) Uani 1 1 d . . . F10 F 0.4555(8) 0.1009(9) 0.1331(8) 0.197(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0451(3) 0.0534(4) 0.0437(3) -0.0213(3) -0.0002(2) 0.0013(3) Ag1 0.0727(4) 0.0804(5) 0.0610(4) -0.0230(3) -0.0049(3) 0.0006(3) Cl1 0.0521(10) 0.0613(11) 0.0566(10) -0.0199(9) 0.0004(8) -0.0043(8) N1 0.050(3) 0.062(4) 0.058(4) -0.022(3) -0.005(3) 0.004(3) N3 0.094(5) 0.057(4) 0.051(4) -0.018(3) -0.010(4) -0.013(4) N4 0.078(5) 0.068(4) 0.049(4) -0.031(3) 0.017(3) -0.025(4) N5 0.049(3) 0.045(3) 0.066(4) -0.017(3) 0.021(3) -0.011(3) N6 0.054(4) 0.054(4) 0.047(3) -0.014(3) -0.010(3) -0.002(3) N7 0.057(4) 0.051(4) 0.059(4) -0.023(3) -0.003(3) 0.006(3) N8 0.141(8) 0.101(6) 0.089(6) -0.049(5) 0.014(6) 0.000(5) N9 0.074(4) 0.078(5) 0.061(4) -0.033(4) -0.012(3) -0.003(4) C1 0.129(8) 0.065(6) 0.076(5) -0.034(5) -0.048(6) 0.025(6) C2 0.069(5) 0.073(5) 0.050(4) -0.024(4) -0.010(4) -0.008(4) C3 0.048(4) 0.048(4) 0.069(5) -0.015(4) -0.003(4) -0.002(3) C4 0.112(8) 0.069(6) 0.079(7) -0.007(5) -0.047(6) -0.016(6) C5 0.036(4) 0.041(4) 0.085(5) -0.014(4) -0.001(4) -0.004(3) C6 0.055(5) 0.058(5) 0.102(7) -0.018(5) 0.019(5) -0.004(4) C8 0.097(7) 0.044(4) 0.070(5) -0.024(4) 0.033(5) -0.023(4) C10 0.109(8) 0.098(8) 0.070(6) -0.050(6) 0.024(6) -0.054(7) C11 0.092(7) 0.060(5) 0.116(7) -0.043(5) 0.076(6) -0.029(5) C12 0.077(5) 0.047(4) 0.045(4) -0.017(3) -0.008(4) -0.015(4) C14 0.063(5) 0.071(6) 0.081(6) -0.031(5) -0.008(4) 0.014(5) C15 0.128(9) 0.052(6) 0.143(9) -0.015(6) -0.012(7) -0.028(6) C17 0.053(5) 0.077(6) 0.061(5) -0.023(4) -0.001(4) 0.006(4) C20 0.088(6) 0.079(6) 0.052(4) -0.029(4) -0.024(4) 0.019(5) C21 0.100(7) 0.106(8) 0.088(6) -0.043(6) -0.037(6) 0.019(6) C22 0.066(6) 0.157(11) 0.059(5) -0.040(7) -0.017(4) 0.008(7) C23 0.072(6) 0.133(10) 0.069(6) -0.044(6) 0.007(5) -0.026(6) C24 0.067(5) 0.099(7) 0.069(5) -0.031(5) 0.013(4) -0.013(5) C25 0.055(6) 0.067(6) 0.167(11) -0.023(7) 0.036(7) -0.007(5) C50 0.100(7) 0.104(7) 0.091(7) -0.049(6) -0.017(5) 0.000(6) C52 0.075(6) 0.079(6) 0.086(7) -0.044(6) 0.005(5) -0.002(5) C54 0.169(10) 0.072(6) 0.039(4) -0.023(4) 0.000(6) -0.061(7) C60 0.082(6) 0.124(9) 0.094(6) -0.031(6) 0.010(5) 0.035(6) C70 0.057(5) 0.054(5) 0.100(7) -0.010(5) -0.032(5) -0.004(4) C71 0.053(6) 0.056(6) 0.171(11) -0.006(7) 0.007(7) -0.003(4) C75 0.116(8) 0.079(6) 0.062(5) -0.027(5) -0.022(6) -0.013(6) C76 0.061(7) 0.061(6) 0.143(10) 0.002(7) -0.023(6) -0.022(5) F1 0.158(8) 0.81(3) 0.258(12) -0.230(18) -0.125(9) 0.261(15) F6 0.198(7) 0.184(7) 0.113(5) -0.060(5) 0.000(5) -0.050(6) F8 0.210(8) 0.252(10) 0.237(9) -0.189(9) 0.091(7) -0.098(7) F21 0.163(7) 0.256(9) 0.212(8) -0.165(8) -0.064(6) -0.016(6) F11 0.100(4) 0.283(10) 0.068(3) -0.017(4) -0.001(3) 0.042(5) F12 0.144(5) 0.162(6) 0.120(5) -0.034(4) -0.021(4) 0.077(5) F13 0.437(18) 0.186(9) 0.101(6) 0.010(6) 0.006(8) -0.116(10) F15 0.273(11) 0.096(5) 0.242(10) -0.045(6) 0.114(9) -0.073(7) F90 0.149(8) 0.243(13) 0.45(2) -0.155(14) -0.073(11) 0.063(9) F123 0.190(8) 0.082(5) 0.270(10) -0.048(5) 0.098(7) -0.051(5) P3 0.0695(18) 0.092(2) 0.0526(16) -0.0379(16) -0.0136(14) 0.0030(17) P4 0.092(3) 0.057(3) 0.200(5) -0.009(3) 0.052(3) -0.012(2) P5 0.1055(19) 0.0963(19) 0.0670(15) -0.0443(15) -0.0126(13) 0.0079(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 F20 P5 1.527(10) . ? Ru1 N7 1.983(7) . ? Ru1 N5 1.983(5) . ? Ru1 C12 2.012(6) . ? Ru1 N1 2.049(6) . ? Ru1 N6 2.178(5) . ? Ru1 Cl1 2.4234(19) . ? Ag1 N9 2.269(6) . ? Ag1 N8 2.425(9) . ? Ag1 Cl1 2.5043(18) . ? Ag1 Cl1 2.7998(18) 2_666 ? Cl1 Ag1 2.7998(18) 2_666 ? N1 C17 1.142(8) . ? N3 C12 1.316(8) . ? N3 C1 1.402(10) . ? N3 C54 1.424(11) . ? N4 C10 1.365(10) . ? N4 C12 1.366(9) . ? N4 C8 1.384(10) . ? N5 C8 1.348(9) . ? N5 C5 1.367(9) . ? N6 C2 1.324(8) . ? N6 C3 1.362(8) . ? N7 C14 1.156(10) . ? N8 C52 1.103(10) . ? N9 C20 1.294(10) . ? N9 C24 1.355(10) . ? C1 C20 1.546(12) . ? C2 C75 1.406(10) . ? C3 C5 1.384(10) . ? C3 C70 1.417(10) . ? C4 C75 1.320(13) . ? C4 C70 1.387(13) . ? C5 C6 1.369(10) . ? C6 C25 1.354(14) . ? C6 C71 1.464(14) . ? C8 C11 1.430(12) . ? C10 C54 1.292(13) . ? C11 C25 1.393(14) . ? C14 C15 1.459(13) . ? C17 C60 1.471(11) . ? C20 C21 1.410(11) . ? C21 C22 1.336(13) . ? C22 C23 1.328(13) . ? C23 C24 1.398(12) . ? C50 C52 1.407(13) . ? C70 C76 1.451(14) . ? C71 C76 1.319(15) . ? F1 P5 1.392(8) . ? F6 P5 1.591(8) . ? F8 P5 1.516(8) . ? F21 P3 1.544(6) . ? F11 P3 1.556(6) . ? F12 P3 1.550(6) . ? F13 P5 1.454(8) . ? F15 P4 1.535(9) . ? F90 P4 1.507(10) . ? F123 P4 1.557(8) . ? P3 F21 1.544(6) 2_765 ? P3 F12 1.550(6) 2_765 ? P3 F11 1.556(6) 2_765 ? P4 F90 1.507(10) 2_575 ? P4 F15 1.535(9) 2_575 ? P4 F123 1.557(8) 2_575 ? P5 F10 1.461(10) . ? 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 N7 Ru1 N5 89.8(2) . . ? N7 Ru1 C12 88.9(3) . . ? N5 Ru1 C12 78.2(3) . . ? N7 Ru1 N1 91.1(2) . . ? N5 Ru1 N1 176.3(2) . . ? C12 Ru1 N1 105.4(3) . . ? N7 Ru1 N6 90.4(2) . . ? N5 Ru1 N6 77.8(2) . . ? C12 Ru1 N6 156.0(3) . . ? N1 Ru1 N6 98.6(2) . . ? N7 Ru1 Cl1 177.25(16) . . ? N5 Ru1 Cl1 90.91(16) . . ? C12 Ru1 Cl1 93.8(2) . . ? N1 Ru1 Cl1 88.05(17) . . ? N6 Ru1 Cl1 87.17(15) . . ? N9 Ag1 N8 95.5(3) . . ? N9 Ag1 Cl1 146.44(19) . . ? N8 Ag1 Cl1 107.5(2) . . ? N9 Ag1 Cl1 88.90(17) . 2_666 ? N8 Ag1 Cl1 127.9(2) . 2_666 ? Cl1 Ag1 Cl1 95.44(5) . 2_666 ? Ru1 Cl1 Ag1 97.99(6) . . ? Ru1 Cl1 Ag1 127.62(7) . 2_666 ? Ag1 Cl1 Ag1 84.56(5) . 2_666 ? C17 N1 Ru1 175.0(6) . . ? C12 N3 C1 125.3(7) . . ? C12 N3 C54 108.6(8) . . ? C1 N3 C54 126.1(8) . . ? C10 N4 C12 113.8(8) . . ? C10 N4 C8 127.6(8) . . ? C12 N4 C8 118.4(6) . . ? C8 N5 C5 122.7(7) . . ? C8 N5 Ru1 119.1(6) . . ? C5 N5 Ru1 118.1(5) . . ? C2 N6 C3 118.3(6) . . ? C2 N6 Ru1 131.4(5) . . ? C3 N6 Ru1 110.2(4) . . ? C14 N7 Ru1 177.1(6) . . ? C52 N8 Ag1 128.8(8) . . ? C20 N9 C24 118.9(7) . . ? C20 N9 Ag1 125.9(5) . . ? C24 N9 Ag1 114.8(6) . . ? N3 C1 C20 113.6(7) . . ? N6 C2 C75 122.1(8) . . ? N6 C3 C5 118.2(6) . . ? N6 C3 C70 122.1(8) . . ? C5 C3 C70 119.7(7) . . ? C75 C4 C70 121.8(8) . . ? N5 C5 C6 119.9(8) . . ? N5 C5 C3 115.6(6) . . ? C6 C5 C3 124.6(8) . . ? C25 C6 C5 119.3(9) . . ? C25 C6 C71 124.3(10) . . ? C5 C6 C71 116.4(10) . . ? N5 C8 N4 111.0(7) . . ? N5 C8 C11 118.3(9) . . ? N4 C8 C11 130.7(9) . . ? C54 C10 N4 103.8(9) . . ? C25 C11 C8 117.5(9) . . ? N3 C12 N4 103.6(6) . . ? N3 C12 Ru1 142.9(6) . . ? N4 C12 Ru1 113.3(5) . . ? N7 C14 C15 178.2(9) . . ? N1 C17 C60 176.2(9) . . ? N9 C20 C21 120.2(9) . . ? N9 C20 C1 116.6(6) . . ? C21 C20 C1 123.2(8) . . ? C22 C21 C20 121.1(10) . . ? C23 C22 C21 119.0(9) . . ? C22 C23 C24 119.4(10) . . ? N9 C24 C23 121.3(9) . . ? C6 C25 C11 122.2(9) . . ? N8 C52 C50 178.3(11) . . ? C10 C54 N3 110.1(8) . . ? C4 C70 C3 116.3(8) . . ? C4 C70 C76 128.4(9) . . ? C3 C70 C76 115.4(10) . . ? C76 C71 C6 119.6(10) . . ? C4 C75 C2 119.4(9) . . ? C71 C76 C70 124.4(10) . . ? F21 P3 F21 180.000(1) . 2_765 ? F21 P3 F12 96.7(4) . 2_765 ? F21 P3 F12 83.3(4) 2_765 2_765 ? F21 P3 F12 83.3(4) . . ? F21 P3 F12 96.7(4) 2_765 . ? F12 P3 F12 180.0(5) 2_765 . ? F21 P3 F11 87.5(5) . . ? F21 P3 F11 92.5(5) 2_765 . ? F12 P3 F11 87.4(4) 2_765 . ? F12 P3 F11 92.6(4) . . ? F21 P3 F11 92.5(5) . 2_765 ? F21 P3 F11 87.5(5) 2_765 2_765 ? F12 P3 F11 92.6(4) 2_765 2_765 ? F12 P3 F11 87.4(4) . 2_765 ? F11 P3 F11 180.0(3) . 2_765 ? F90 P4 F90 180.000(1) . 2_575 ? F90 P4 F15 94.6(7) . . ? F90 P4 F15 85.4(7) 2_575 . ? F90 P4 F15 85.4(7) . 2_575 ? F90 P4 F15 94.6(7) 2_575 2_575 ? F15 P4 F15 180.000(2) . 2_575 ? F90 P4 F123 89.8(6) . 2_575 ? F90 P4 F123 90.2(6) 2_575 2_575 ? F15 P4 F123 89.5(4) . 2_575 ? F15 P4 F123 90.5(4) 2_575 2_575 ? F90 P4 F123 90.2(6) . . ? F90 P4 F123 89.8(6) 2_575 . ? F15 P4 F123 90.5(4) . . ? F15 P4 F123 89.5(4) 2_575 . ? F123 P4 F123 180.0(7) 2_575 . ? F1 P5 F13 95.5(8) . . ? F1 P5 F10 90.6(8) . . ? F13 P5 F10 97.1(6) . . ? F1 P5 F8 98.2(9) . . ? F13 P5 F8 89.3(6) . . ? F10 P5 F8 168.6(6) . . ? F1 P5 F20 175.6(6) . . ? F13 P5 F20 87.5(7) . . ? F10 P5 F20 85.9(5) . . ? F8 P5 F20 84.9(5) . . ? F1 P5 F6 92.6(8) . . ? F13 P5 F6 171.8(7) . . ? F10 P5 F6 82.3(5) . . ? F8 P5 F6 90.1(5) . . ? F20 P5 F6 84.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 Ru1 Cl1 Ag1 155(3) . . . . ? N5 Ru1 Cl1 Ag1 -101.12(19) . . . . ? C12 Ru1 Cl1 Ag1 -22.9(2) . . . . ? N1 Ru1 Cl1 Ag1 82.38(16) . . . . ? N6 Ru1 Cl1 Ag1 -178.89(16) . . . . ? N7 Ru1 Cl1 Ag1 65(3) . . . 2_666 ? N5 Ru1 Cl1 Ag1 169.6(2) . . . 2_666 ? C12 Ru1 Cl1 Ag1 -112.2(2) . . . 2_666 ? N1 Ru1 Cl1 Ag1 -6.89(17) . . . 2_666 ? N6 Ru1 Cl1 Ag1 91.84(17) . . . 2_666 ? N9 Ag1 Cl1 Ru1 -31.1(3) . . . . ? N8 Ag1 Cl1 Ru1 100.0(2) . . . . ? Cl1 Ag1 Cl1 Ru1 -127.29(8) 2_666 . . . ? N9 Ag1 Cl1 Ag1 96.2(3) . . . 2_666 ? N8 Ag1 Cl1 Ag1 -132.7(2) . . . 2_666 ? Cl1 Ag1 Cl1 Ag1 0.0 2_666 . . 2_666 ? N7 Ru1 N1 C17 -107(7) . . . . ? N5 Ru1 N1 C17 -3(10) . . . . ? C12 Ru1 N1 C17 164(7) . . . . ? N6 Ru1 N1 C17 -16(7) . . . . ? Cl1 Ru1 N1 C17 71(7) . . . . ? N7 Ru1 N5 C8 -88.8(5) . . . . ? C12 Ru1 N5 C8 0.1(5) . . . . ? N1 Ru1 N5 C8 167(3) . . . . ? N6 Ru1 N5 C8 -179.3(5) . . . . ? Cl1 Ru1 N5 C8 93.8(5) . . . . ? N7 Ru1 N5 C5 89.5(5) . . . . ? C12 Ru1 N5 C5 178.5(5) . . . . ? N1 Ru1 N5 C5 -14(4) . . . . ? N6 Ru1 N5 C5 -0.9(5) . . . . ? Cl1 Ru1 N5 C5 -87.8(5) . . . . ? N7 Ru1 N6 C2 93.1(6) . . . . ? N5 Ru1 N6 C2 -177.2(7) . . . . ? C12 Ru1 N6 C2 -178.7(6) . . . . ? N1 Ru1 N6 C2 1.9(7) . . . . ? Cl1 Ru1 N6 C2 -85.7(6) . . . . ? N7 Ru1 N6 C3 -89.8(5) . . . . ? N5 Ru1 N6 C3 -0.1(4) . . . . ? C12 Ru1 N6 C3 -1.6(8) . . . . ? N1 Ru1 N6 C3 179.0(5) . . . . ? Cl1 Ru1 N6 C3 91.4(4) . . . . ? N5 Ru1 N7 C14 51(12) . . . . ? C12 Ru1 N7 C14 -28(12) . . . . ? N1 Ru1 N7 C14 -133(12) . . . . ? N6 Ru1 N7 C14 128(12) . . . . ? Cl1 Ru1 N7 C14 155(10) . . . . ? N9 Ag1 N8 C52 11.8(11) . . . . ? Cl1 Ag1 N8 C52 -143.4(10) . . . . ? Cl1 Ag1 N8 C52 104.7(10) 2_666 . . . ? N8 Ag1 N9 C20 -118.5(7) . . . . ? Cl1 Ag1 N9 C20 15.3(9) . . . . ? Cl1 Ag1 N9 C20 113.5(7) 2_666 . . . ? N8 Ag1 N9 C24 68.3(6) . . . . ? Cl1 Ag1 N9 C24 -157.9(4) . . . . ? Cl1 Ag1 N9 C24 -59.7(5) 2_666 . . . ? C12 N3 C1 C20 -124.0(8) . . . . ? C54 N3 C1 C20 54.5(10) . . . . ? C3 N6 C2 C75 -0.1(11) . . . . ? Ru1 N6 C2 C75 176.9(5) . . . . ? C2 N6 C3 C5 178.7(6) . . . . ? Ru1 N6 C3 C5 1.1(8) . . . . ? C2 N6 C3 C70 -2.0(10) . . . . ? Ru1 N6 C3 C70 -179.5(6) . . . . ? C8 N5 C5 C6 -1.7(10) . . . . ? Ru1 N5 C5 C6 -179.9(5) . . . . ? C8 N5 C5 C3 -179.9(6) . . . . ? Ru1 N5 C5 C3 1.8(8) . . . . ? N6 C3 C5 N5 -1.9(10) . . . . ? C70 C3 C5 N5 178.7(6) . . . . ? N6 C3 C5 C6 179.9(7) . . . . ? C70 C3 C5 C6 0.5(11) . . . . ? N5 C5 C6 C25 1.6(12) . . . . ? C3 C5 C6 C25 179.7(8) . . . . ? N5 C5 C6 C71 -179.2(7) . . . . ? C3 C5 C6 C71 -1.1(12) . . . . ? C5 N5 C8 N4 -177.6(6) . . . . ? Ru1 N5 C8 N4 0.7(8) . . . . ? C5 N5 C8 C11 1.2(10) . . . . ? Ru1 N5 C8 C11 179.5(5) . . . . ? C10 N4 C8 N5 173.7(7) . . . . ? C12 N4 C8 N5 -1.5(9) . . . . ? C10 N4 C8 C11 -5.0(13) . . . . ? C12 N4 C8 C11 179.9(7) . . . . ? C12 N4 C10 C54 -2.0(10) . . . . ? C8 N4 C10 C54 -177.4(8) . . . . ? N5 C8 C11 C25 -0.8(11) . . . . ? N4 C8 C11 C25 177.8(8) . . . . ? C1 N3 C12 N4 178.7(7) . . . . ? C54 N3 C12 N4 0.0(8) . . . . ? C1 N3 C12 Ru1 -8.2(13) . . . . ? C54 N3 C12 Ru1 173.0(7) . . . . ? C10 N4 C12 N3 1.3(8) . . . . ? C8 N4 C12 N3 177.1(6) . . . . ? C10 N4 C12 Ru1 -174.2(5) . . . . ? C8 N4 C12 Ru1 1.6(8) . . . . ? N7 Ru1 C12 N3 -83.6(9) . . . . ? N5 Ru1 C12 N3 -173.6(9) . . . . ? N1 Ru1 C12 N3 7.2(9) . . . . ? N6 Ru1 C12 N3 -172.1(7) . . . . ? Cl1 Ru1 C12 N3 96.3(9) . . . . ? N7 Ru1 C12 N4 89.1(5) . . . . ? N5 Ru1 C12 N4 -0.9(5) . . . . ? N1 Ru1 C12 N4 179.9(5) . . . . ? N6 Ru1 C12 N4 0.6(9) . . . . ? Cl1 Ru1 C12 N4 -91.0(5) . . . . ? Ru1 N7 C14 C15 -119(32) . . . . ? Ru1 N1 C17 C60 105(13) . . . . ? C24 N9 C20 C21 5.1(12) . . . . ? Ag1 N9 C20 C21 -167.9(6) . . . . ? C24 N9 C20 C1 -174.8(7) . . . . ? Ag1 N9 C20 C1 12.2(10) . . . . ? N3 C1 C20 N9 49.1(10) . . . . ? N3 C1 C20 C21 -130.9(8) . . . . ? N9 C20 C21 C22 -3.7(14) . . . . ? C1 C20 C21 C22 176.2(9) . . . . ? C20 C21 C22 C23 1.5(14) . . . . ? C21 C22 C23 C24 -0.8(14) . . . . ? C20 N9 C24 C23 -4.5(11) . . . . ? Ag1 N9 C24 C23 169.2(6) . . . . ? C22 C23 C24 N9 2.3(13) . . . . ? C5 C6 C25 C11 -1.3(14) . . . . ? C71 C6 C25 C11 179.6(8) . . . . ? C8 C11 C25 C6 0.8(14) . . . . ? Ag1 N8 C52 C50 24(39) . . . . ? N4 C10 C54 N3 1.9(10) . . . . ? C12 N3 C54 C10 -1.2(10) . . . . ? C1 N3 C54 C10 -180.0(8) . . . . ? C75 C4 C70 C3 0.3(13) . . . . ? C75 C4 C70 C76 -178.0(9) . . . . ? N6 C3 C70 C4 1.9(11) . . . . ? C5 C3 C70 C4 -178.8(7) . . . . ? N6 C3 C70 C76 -179.6(7) . . . . ? C5 C3 C70 C76 -0.2(11) . . . . ? C25 C6 C71 C76 -179.4(10) . . . . ? C5 C6 C71 C76 1.5(13) . . . . ? C70 C4 C75 C2 -2.3(14) . . . . ? N6 C2 C75 C4 2.2(13) . . . . ? C6 C71 C76 C70 -1.3(16) . . . . ? C4 C70 C76 C71 179.0(10) . . . . ? C3 C70 C76 C71 0.6(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.986 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.105 #===END data_080709g _database_code_depnum_ccdc_archive 'CCDC 832965' #TrackingRef '- Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H27 F12 N9 P2 Ru' _chemical_formula_weight 892.61 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' 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' _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 8.1643(12) _cell_length_b 9.0931(15) _cell_length_c 24.710(3) _cell_angle_alpha 80.7460(10) _cell_angle_beta 82.5950(10) _cell_angle_gamma 89.961(2) _cell_volume 1795.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2089 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 20.4 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7838 _exptl_absorpt_correction_T_max 0.9576 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9460 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0935 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6243 _reflns_number_gt 3823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0979P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6243 _refine_ls_number_parameters 592 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1833 _refine_ls_wR_factor_gt 0.1556 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 0.15027(7) 0.09938(6) 0.74004(2) 0.0444(2) Uani 1 1 d . . . F1 F 0.646(3) 0.685(4) 0.5821(13) 0.164(15) Uani 0.42(3) 1 d P A 1 F2 F 0.281(4) 0.704(4) 0.6377(15) 0.172(16) Uani 0.42(3) 1 d P A 1 F3 F 0.503(5) 0.832(3) 0.6312(13) 0.150(13) Uani 0.42(3) 1 d P A 1 F4 F 0.489(5) 0.547(4) 0.6488(10) 0.158(13) Uani 0.42(3) 1 d P A 1 F5 F 0.437(4) 0.548(3) 0.5809(14) 0.162(12) Uani 0.42(3) 1 d P A 1 F6 F 0.412(4) 0.805(4) 0.5547(13) 0.130(11) Uani 0.42(3) 1 d P A 1 F7 F 0.285(3) 0.617(2) 0.9155(9) 0.131(8) Uani 0.63(2) 1 d P B 1 F8 F 0.446(3) 0.881(3) 0.9599(8) 0.144(9) Uani 0.63(2) 1 d P B 1 F9 F 0.539(2) 0.701(2) 0.9129(10) 0.167(9) Uani 0.63(2) 1 d P B 1 F10 F 0.370(3) 0.6632(19) 0.9973(7) 0.176(8) Uani 0.63(2) 1 d P B 1 F11 F 0.1951(18) 0.8103(19) 0.9565(7) 0.113(5) Uani 0.63(2) 1 d P B 1 F12 F 0.373(2) 0.8590(15) 0.8807(4) 0.121(7) Uani 0.63(2) 1 d P B 1 F1' F 0.582(3) 0.634(3) 0.6454(9) 0.145(9) Uani 0.58(3) 1 d P A 2 F2' F 0.325(4) 0.759(4) 0.5711(12) 0.168(11) Uani 0.58(3) 1 d P A 2 F3' F 0.343(3) 0.548(2) 0.6269(11) 0.180(11) Uani 0.58(3) 1 d P A 2 F4' F 0.374(4) 0.764(3) 0.6528(7) 0.151(10) Uani 0.58(3) 1 d P A 2 F5' F 0.569(3) 0.829(3) 0.5825(13) 0.192(12) Uani 0.58(3) 1 d P A 2 F6' F 0.533(3) 0.612(2) 0.5562(5) 0.135(9) Uani 0.58(3) 1 d P A 2 F7' F 0.226(3) 0.772(3) 0.8926(9) 0.143(13) Uani 0.37(2) 1 d P B 2 F8' F 0.500(4) 0.720(4) 0.9676(12) 0.139(12) Uani 0.37(2) 1 d P B 2 F9' F 0.391(4) 0.912(4) 0.9336(16) 0.146(13) Uani 0.37(2) 1 d P B 2 F10' F 0.493(4) 0.752(4) 0.8802(11) 0.143(13) Uani 0.37(2) 1 d P B 2 F11' F 0.338(5) 0.589(4) 0.9420(15) 0.134(11) Uani 0.37(2) 1 d P B 2 F12' F 0.229(4) 0.732(4) 0.9821(13) 0.140(11) Uani 0.37(2) 1 d P B 2 N1 N -0.1726(7) -0.0147(6) 0.7824(2) 0.0490(14) Uani 1 1 d . . . N2 N -0.1532(7) -0.0464(6) 0.6981(2) 0.0539(15) Uani 1 1 d . . . N3 N 0.0349(6) 0.0873(5) 0.8160(2) 0.0405(12) Uani 1 1 d . . . N4 N 0.3355(7) 0.1952(6) 0.7819(2) 0.0512(14) Uani 1 1 d . . . N5 N -0.2069(11) 0.2035(9) 0.6272(3) 0.097(2) Uani 1 1 d . . . N6 N 0.2707(7) 0.1194(6) 0.6609(2) 0.0545(15) Uani 1 1 d . . . N7 N 0.2382(7) -0.1070(6) 0.7593(2) 0.0464(13) Uani 1 1 d . . . N8 N 0.0646(7) 0.3065(6) 0.7192(2) 0.0504(14) Uani 1 1 d . . . N9 N 0.9102(16) 0.5361(15) 0.8260(5) 0.172(5) Uani 1 1 d . . . P1 P 0.4550(4) 0.6874(4) 0.60570(12) 0.1016(9) Uani 1 1 d . . . P2 P 0.3637(3) 0.7487(3) 0.93565(10) 0.0739(7) Uani 1 1 d . . . C1 C -0.0649(8) 0.0062(7) 0.7335(3) 0.0491(17) Uani 1 1 d . . . C2 C -0.3073(10) -0.0956(8) 0.7235(3) 0.064(2) Uani 1 1 d . . . H2 H -0.3888 -0.1353 0.7067 0.077 Uiso 1 1 calc R . . C3 C -0.3203(9) -0.0774(8) 0.7751(3) 0.0589(19) Uani 1 1 d . . . H3 H -0.4113 -0.1020 0.8019 0.071 Uiso 1 1 calc R . . C4 C -0.1162(8) 0.0295(7) 0.8286(3) 0.0459(16) Uani 1 1 d . . . C5 C -0.2020(9) 0.0207(8) 0.8813(3) 0.0583(19) Uani 1 1 d . . . H5 H -0.3079 -0.0211 0.8901 0.070 Uiso 1 1 calc R . . C6 C -0.1233(10) 0.0767(8) 0.9204(3) 0.060(2) Uani 1 1 d . . . H6 H -0.1784 0.0726 0.9560 0.072 Uiso 1 1 calc R . . C7 C 0.0355(10) 0.1389(8) 0.9080(3) 0.0559(18) Uani 1 1 d . . . C8 C 0.1119(8) 0.1396(7) 0.8543(3) 0.0477(16) Uani 1 1 d . . . C9 C 0.2740(9) 0.1977(7) 0.8355(3) 0.0495(17) Uani 1 1 d . . . C10 C 0.3610(10) 0.2542(8) 0.8739(3) 0.060(2) Uani 1 1 d . . . C11 C 0.5198(10) 0.3104(8) 0.8528(4) 0.070(2) Uani 1 1 d . . . H11 H 0.5837 0.3503 0.8756 0.084 Uiso 1 1 calc R . . C12 C 0.5816(10) 0.3072(9) 0.7995(4) 0.072(2) Uani 1 1 d . . . H12 H 0.6879 0.3438 0.7860 0.087 Uiso 1 1 calc R . . C13 C 0.4860(10) 0.2493(8) 0.7647(3) 0.064(2) Uani 1 1 d . . . H13 H 0.5301 0.2488 0.7281 0.076 Uiso 1 1 calc R . . C14 C 0.1273(11) 0.1953(9) 0.9453(3) 0.068(2) Uani 1 1 d . . . H14 H 0.0808 0.1946 0.9817 0.081 Uiso 1 1 calc R . . C15 C 0.2798(11) 0.2493(9) 0.9284(3) 0.068(2) Uani 1 1 d . . . H15 H 0.3365 0.2861 0.9538 0.082 Uiso 1 1 calc R . . C16 C -0.0924(10) -0.0442(8) 0.6401(3) 0.064(2) Uani 1 1 d . . . H16A H -0.1483 -0.1229 0.6268 0.076 Uiso 1 1 calc R . . H16B H 0.0246 -0.0655 0.6366 0.076 Uiso 1 1 calc R . . C17 C -0.1170(11) 0.1005(10) 0.6042(4) 0.073(2) Uani 1 1 d . . . C18 C -0.0492(14) 0.1203(12) 0.5512(4) 0.106(3) Uani 1 1 d . . . H18 H 0.0118 0.0460 0.5367 0.127 Uiso 1 1 calc R . . C19 C -0.0733(18) 0.2563(16) 0.5185(5) 0.128(4) Uani 1 1 d . . . H19 H -0.0241 0.2756 0.4819 0.154 Uiso 1 1 calc R . . C20 C -0.1650(17) 0.3567(15) 0.5391(6) 0.127(4) Uani 1 1 d . . . H20 H -0.1849 0.4455 0.5167 0.153 Uiso 1 1 calc R . . C21 C -0.2326(16) 0.3318(13) 0.5942(5) 0.121(4) Uani 1 1 d . . . H21 H -0.2966 0.4046 0.6085 0.145 Uiso 1 1 calc R . . C22 C 0.3303(11) 0.1399(10) 0.6166(3) 0.076(2) Uani 1 1 d . . . C23 C 0.4061(13) 0.1672(13) 0.5598(4) 0.122(4) Uani 1 1 d . . . H23A H 0.3838 0.0840 0.5422 0.183 Uiso 1 1 calc R . . H23B H 0.5233 0.1800 0.5586 0.183 Uiso 1 1 calc R . . H23C H 0.3618 0.2558 0.5409 0.183 Uiso 1 1 calc R . . C24 C 0.2794(9) -0.2253(8) 0.7692(3) 0.0517(17) Uani 1 1 d . . . C25 C 0.3342(11) -0.3759(8) 0.7823(3) 0.076(2) Uani 1 1 d . . . H25A H 0.4054 -0.4009 0.7511 0.114 Uiso 1 1 calc R . . H25B H 0.2402 -0.4429 0.7906 0.114 Uiso 1 1 calc R . . H25C H 0.3935 -0.3844 0.8137 0.114 Uiso 1 1 calc R . . C26 C 0.0160(10) 0.4198(9) 0.7045(3) 0.067(2) Uani 1 1 d . . . C27 C -0.0441(12) 0.5667(10) 0.6879(4) 0.104(3) Uani 1 1 d . . . H27A H -0.0329 0.6263 0.7160 0.155 Uiso 1 1 calc R . . H27B H -0.1584 0.5599 0.6829 0.155 Uiso 1 1 calc R . . H27C H 0.0188 0.6119 0.6538 0.155 Uiso 1 1 calc R . . C28 C 0.8921(15) 0.5534(15) 0.8704(6) 0.117(4) Uani 1 1 d . . . C29 C 0.8824(13) 0.5792(13) 0.9245(5) 0.116(4) Uani 1 1 d . . . H29A H 0.9305 0.6753 0.9249 0.174 Uiso 1 1 calc R . . H29B H 0.9414 0.5037 0.9455 0.174 Uiso 1 1 calc R . . H29C H 0.7687 0.5766 0.9405 0.174 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0457(4) 0.0444(3) 0.0418(3) -0.0038(2) -0.0044(2) 0.0031(2) F1 0.133(19) 0.17(3) 0.17(3) -0.014(19) 0.017(16) -0.006(16) F2 0.14(2) 0.18(3) 0.17(3) 0.00(2) 0.029(19) -0.002(19) F3 0.17(3) 0.17(2) 0.12(2) -0.052(18) -0.045(19) -0.012(17) F4 0.17(3) 0.18(3) 0.104(16) 0.023(16) -0.010(18) 0.00(2) F5 0.19(3) 0.16(2) 0.14(3) -0.047(19) -0.01(2) -0.028(19) F6 0.14(3) 0.17(2) 0.080(13) -0.011(12) 0.000(16) 0.000(18) F7 0.138(15) 0.119(16) 0.146(17) -0.055(14) -0.011(11) -0.026(12) F8 0.157(18) 0.17(2) 0.114(13) -0.023(12) -0.045(9) -0.065(16) F9 0.114(11) 0.182(14) 0.18(2) 0.014(15) 0.016(13) 0.059(9) F10 0.18(2) 0.186(14) 0.134(13) 0.071(11) -0.055(13) -0.015(13) F11 0.086(8) 0.135(12) 0.118(13) -0.034(9) 0.007(8) 0.030(8) F12 0.154(16) 0.124(10) 0.073(7) 0.020(6) -0.017(7) 0.025(9) F1' 0.154(18) 0.17(2) 0.126(15) -0.041(14) -0.058(14) 0.022(13) F2' 0.16(2) 0.22(3) 0.14(3) -0.036(19) -0.065(18) 0.022(19) F3' 0.17(2) 0.158(18) 0.19(2) -0.025(13) 0.048(16) -0.050(16) F4' 0.18(3) 0.17(2) 0.102(10) -0.066(12) 0.011(14) 0.012(17) F5' 0.19(2) 0.19(2) 0.18(2) -0.012(16) 0.004(18) -0.046(17) F6' 0.18(2) 0.149(16) 0.061(8) -0.013(8) 0.018(9) 0.013(14) F7' 0.114(19) 0.18(3) 0.127(18) 0.027(15) -0.047(14) 0.020(17) F8' 0.12(2) 0.19(3) 0.11(2) -0.007(19) -0.080(19) 0.017(19) F9' 0.14(2) 0.14(2) 0.16(4) 0.01(2) -0.04(2) -0.002(16) F10' 0.13(2) 0.19(3) 0.105(18) 0.003(17) -0.002(15) -0.01(2) F11' 0.16(3) 0.101(16) 0.15(3) -0.003(18) -0.041(19) -0.015(16) F12' 0.12(2) 0.16(3) 0.13(2) -0.024(19) 0.016(19) 0.02(2) N1 0.046(3) 0.051(3) 0.049(3) -0.010(3) -0.005(3) -0.002(3) N2 0.060(4) 0.052(3) 0.053(3) -0.010(3) -0.017(3) -0.004(3) N3 0.043(3) 0.040(3) 0.040(3) -0.007(2) -0.008(2) 0.006(2) N4 0.047(4) 0.047(3) 0.061(4) -0.007(3) -0.010(3) 0.005(3) N5 0.119(7) 0.081(6) 0.092(6) -0.001(5) -0.036(5) 0.015(5) N6 0.054(4) 0.059(4) 0.050(4) -0.010(3) -0.001(3) 0.000(3) N7 0.047(3) 0.046(3) 0.045(3) -0.007(3) -0.003(3) 0.001(3) N8 0.046(4) 0.050(4) 0.054(4) -0.002(3) -0.009(3) 0.001(3) N9 0.148(11) 0.229(14) 0.138(10) -0.055(10) 0.011(9) -0.034(9) P1 0.113(3) 0.135(3) 0.0639(17) -0.0361(19) -0.0117(18) 0.006(2) P2 0.0680(16) 0.0750(17) 0.0722(16) -0.0014(12) 0.0019(13) -0.0026(13) C1 0.055(4) 0.044(4) 0.050(4) -0.008(3) -0.013(3) 0.003(3) C2 0.060(5) 0.066(5) 0.070(5) -0.014(4) -0.018(4) -0.009(4) C3 0.051(5) 0.059(5) 0.065(5) -0.008(4) -0.006(4) -0.008(4) C4 0.045(4) 0.047(4) 0.044(4) -0.003(3) -0.006(3) 0.001(3) C5 0.055(5) 0.064(5) 0.052(4) -0.006(4) 0.006(4) 0.000(4) C6 0.069(5) 0.059(5) 0.048(4) -0.007(4) 0.005(4) 0.007(4) C7 0.067(5) 0.058(4) 0.044(4) -0.009(3) -0.010(4) 0.008(4) C8 0.054(5) 0.040(4) 0.051(4) -0.008(3) -0.014(3) 0.006(3) C9 0.050(4) 0.044(4) 0.059(4) -0.011(3) -0.018(4) 0.008(3) C10 0.062(5) 0.048(4) 0.075(5) -0.008(4) -0.028(4) 0.006(4) C11 0.070(6) 0.059(5) 0.088(6) -0.014(4) -0.038(5) 0.005(4) C12 0.050(5) 0.065(5) 0.102(7) -0.005(5) -0.023(5) -0.004(4) C13 0.055(5) 0.054(4) 0.080(5) -0.006(4) -0.007(4) -0.001(4) C14 0.086(7) 0.068(5) 0.054(5) -0.015(4) -0.018(4) 0.009(5) C15 0.080(6) 0.067(5) 0.064(5) -0.015(4) -0.033(5) 0.008(5) C16 0.076(6) 0.063(5) 0.056(5) -0.014(4) -0.016(4) -0.003(4) C17 0.084(6) 0.074(6) 0.066(6) -0.012(5) -0.027(5) -0.002(5) C18 0.135(10) 0.100(8) 0.075(7) 0.008(6) -0.008(7) 0.006(7) C19 0.155(13) 0.130(11) 0.089(8) 0.013(8) -0.016(8) -0.003(9) C20 0.144(12) 0.106(10) 0.121(11) 0.028(8) -0.037(9) 0.000(8) C21 0.148(11) 0.100(9) 0.115(10) 0.001(7) -0.040(9) 0.014(8) C22 0.075(6) 0.094(6) 0.053(5) -0.005(5) 0.001(4) -0.001(5) C23 0.123(9) 0.167(11) 0.059(6) 0.005(6) 0.028(6) -0.016(8) C24 0.051(4) 0.050(4) 0.055(4) -0.007(3) -0.012(3) 0.004(4) C25 0.097(7) 0.051(5) 0.082(6) -0.012(4) -0.019(5) 0.021(4) C26 0.071(6) 0.055(5) 0.073(5) -0.003(4) -0.014(4) -0.002(4) C27 0.107(8) 0.068(6) 0.128(9) 0.009(6) -0.020(7) 0.015(6) C28 0.088(8) 0.156(11) 0.103(9) -0.039(9) 0.019(7) -0.026(7) C29 0.096(8) 0.139(10) 0.116(9) -0.022(8) -0.020(7) -0.003(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 N3 1.974(5) . ? Ru1 C1 1.987(7) . ? Ru1 N7 2.015(6) . ? Ru1 N8 2.020(6) . ? Ru1 N6 2.052(6) . ? Ru1 N4 2.194(6) . ? F1 P1 1.60(2) . ? F2 P1 1.55(3) . ? F3 P1 1.62(2) . ? F4 P1 1.58(2) . ? F5 P1 1.51(2) . ? F6 P1 1.59(4) . ? F7 P2 1.544(19) . ? F8 P2 1.610(18) . ? F9 P2 1.560(15) . ? F10 P2 1.601(13) . ? F11 P2 1.544(14) . ? F12 P2 1.547(10) . ? F1' P1 1.544(16) . ? F2' P1 1.53(3) . ? F3' P1 1.539(16) . ? F4' P1 1.532(16) . ? F5' P1 1.575(19) . ? F6' P1 1.561(13) . ? F7' P2 1.639(19) . ? F8' P2 1.443(17) . ? F9' P2 1.49(4) . ? F10' P2 1.61(3) . ? F11' P2 1.45(4) . ? F12' P2 1.47(3) . ? N1 C3 1.379(8) . ? N1 C1 1.386(8) . ? N1 C4 1.399(8) . ? N2 C1 1.346(8) . ? N2 C2 1.373(9) . ? N2 C16 1.453(8) . ? N3 C4 1.321(8) . ? N3 C8 1.349(8) . ? N4 C13 1.316(9) . ? N4 C9 1.357(8) . ? N5 C17 1.342(10) . ? N5 C21 1.345(12) . ? N6 C22 1.127(9) . ? N7 C24 1.126(7) . ? N8 C26 1.126(8) . ? N9 C28 1.126(14) . ? C2 C3 1.303(9) . ? C4 C5 1.389(9) . ? C5 C6 1.386(10) . ? C6 C7 1.392(10) . ? C7 C8 1.390(9) . ? C7 C14 1.416(10) . ? C8 C9 1.418(9) . ? C9 C10 1.414(9) . ? C10 C11 1.399(11) . ? C10 C15 1.416(10) . ? C11 C12 1.353(11) . ? C12 C13 1.394(11) . ? C14 C15 1.329(11) . ? C16 C17 1.492(10) . ? C17 C18 1.339(11) . ? C18 C19 1.393(14) . ? C19 C20 1.305(15) . ? C20 C21 1.384(15) . ? C22 C23 1.440(11) . ? C24 C25 1.440(9) . ? C26 C27 1.438(10) . ? C28 C29 1.385(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ru1 C1 78.4(2) . . ? N3 Ru1 N7 90.5(2) . . ? C1 Ru1 N7 88.4(2) . . ? N3 Ru1 N8 90.7(2) . . ? C1 Ru1 N8 91.9(2) . . ? N7 Ru1 N8 178.9(2) . . ? N3 Ru1 N6 178.1(2) . . ? C1 Ru1 N6 102.5(3) . . ? N7 Ru1 N6 91.2(2) . . ? N8 Ru1 N6 87.7(2) . . ? N3 Ru1 N4 77.9(2) . . ? C1 Ru1 N4 156.3(2) . . ? N7 Ru1 N4 91.5(2) . . ? N8 Ru1 N4 88.7(2) . . ? N6 Ru1 N4 101.2(2) . . ? C3 N1 C1 110.8(6) . . ? C3 N1 C4 132.1(6) . . ? C1 N1 C4 117.1(6) . . ? C1 N2 C2 111.3(6) . . ? C1 N2 C16 123.3(6) . . ? C2 N2 C16 125.4(6) . . ? C4 N3 C8 120.8(6) . . ? C4 N3 Ru1 120.0(4) . . ? C8 N3 Ru1 119.2(4) . . ? C13 N4 C9 117.6(7) . . ? C13 N4 Ru1 132.5(5) . . ? C9 N4 Ru1 109.8(4) . . ? C17 N5 C21 117.3(10) . . ? C22 N6 Ru1 174.8(7) . . ? C24 N7 Ru1 176.1(6) . . ? C26 N8 Ru1 175.8(6) . . ? F5 P1 F2' 88.2(15) . . ? F5 P1 F4' 140.2(19) . . ? F2' P1 F4' 87.5(14) . . ? F5 P1 F3' 49.8(13) . . ? F2' P1 F3' 91.1(19) . . ? F4' P1 F3' 90.8(13) . . ? F5 P1 F1' 99.9(13) . . ? F2' P1 F1' 171.7(13) . . ? F4' P1 F1' 85.0(12) . . ? F3' P1 F1' 92.6(14) . . ? F5 P1 F2 103(2) . . ? F2' P1 F2 63.9(15) . . ? F4' P1 F2 40.6(11) . . ? F3' P1 F2 60.6(13) . . ? F1' P1 F2 111.7(17) . . ? F5 P1 F6' 39.8(10) . . ? F2' P1 F6' 90.3(13) . . ? F4' P1 F6' 177.8(11) . . ? F3' P1 F6' 89.5(12) . . ? F1' P1 F6' 97.2(10) . . ? F2 P1 F6' 138(2) . . ? F5 P1 F5' 128.9(17) . . ? F2' P1 F5' 88.3(13) . . ? F4' P1 F5' 90.5(12) . . ? F3' P1 F5' 178.6(15) . . ? F1' P1 F5' 88.2(14) . . ? F2 P1 F5' 120.2(16) . . ? F6' P1 F5' 89.2(13) . . ? F5 P1 F4 70.6(19) . . ? F2' P1 F4 143.1(18) . . ? F4' P1 F4 90.2(14) . . ? F3' P1 F4 52.2(14) . . ? F1' P1 F4 40.7(10) . . ? F2 P1 F4 91.3(16) . . ? F6' P1 F4 91.7(13) . . ? F5' P1 F4 128.6(18) . . ? F5 P1 F6 97.7(19) . . ? F2' P1 F6 31.4(11) . . ? F4' P1 F6 98.8(15) . . ? F3' P1 F6 119.8(19) . . ? F1' P1 F6 147.1(15) . . ? F2 P1 F6 90.7(15) . . ? F6' P1 F6 79.2(13) . . ? F5' P1 F6 59.2(13) . . ? F4 P1 F6 168.3(18) . . ? F5 P1 F1 86.1(14) . . ? F2' P1 F1 122.9(15) . . ? F4' P1 F1 128.3(17) . . ? F3' P1 F1 124.9(15) . . ? F1' P1 F1 60.2(11) . . ? F2 P1 F1 169(2) . . ? F6' P1 F1 52.9(10) . . ? F5' P1 F1 54.6(9) . . ? F4 P1 F1 86.5(14) . . ? F6 P1 F1 93.7(14) . . ? F5 P1 F3 171.8(17) . . ? F2' P1 F3 98.0(15) . . ? F4' P1 F3 46.1(10) . . ? F3' P1 F3 134.9(17) . . ? F1' P1 F3 74.2(11) . . ? F2 P1 F3 84.2(14) . . ? F6' P1 F3 134.2(18) . . ? F5' P1 F3 46.5(11) . . ? F4 P1 F3 106.6(18) . . ? F6 P1 F3 85.0(16) . . ? F1 P1 F3 86.0(17) . . ? F8' P2 F11' 87.6(18) . . ? F8' P2 F12' 97.9(17) . . ? F11' P2 F12' 82(2) . . ? F8' P2 F9' 89.4(15) . . ? F11' P2 F9' 175.7(18) . . ? F12' P2 F9' 95(2) . . ? F8' P2 F11 125.2(14) . . ? F11' P2 F11 105.4(18) . . ? F12' P2 F11 36.0(11) . . ? F9' P2 F11 73.8(15) . . ? F8' P2 F7 118.4(16) . . ? F11' P2 F7 32.4(10) . . ? F12' P2 F7 87.9(15) . . ? F9' P2 F7 151.3(15) . . ? F11 P2 F7 93.4(10) . . ? F8' P2 F12 124.1(16) . . ? F11' P2 F12 125.7(14) . . ? F12' P2 F12 127.0(16) . . ? F9' P2 F12 58.6(14) . . ? F11 P2 F12 91.0(9) . . ? F7 P2 F12 96.9(9) . . ? F8' P2 F9 54.8(12) . . ? F11' P2 F9 79.6(18) . . ? F12' P2 F9 147.3(16) . . ? F9' P2 F9 101.2(16) . . ? F11 P2 F9 175.0(10) . . ? F7 P2 F9 90.6(12) . . ? F12 P2 F9 85.5(8) . . ? F8' P2 F10 48.8(11) . . ? F11' P2 F10 66.0(14) . . ? F12' P2 F10 53.0(13) . . ? F9' P2 F10 109.7(16) . . ? F11 P2 F10 88.0(9) . . ? F7 P2 F10 95.1(10) . . ? F12 P2 F10 168.0(9) . . ? F9 P2 F10 94.7(11) . . ? F8' P2 F8 59.3(12) . . ? F11' P2 F8 144.7(14) . . ? F12' P2 F8 90.2(15) . . ? F9' P2 F8 31.5(10) . . ? F11 P2 F8 86.6(11) . . ? F7 P2 F8 176.9(11) . . ? F12 P2 F8 86.2(8) . . ? F9 P2 F8 89.5(12) . . ? F10 P2 F8 81.8(10) . . ? F8' P2 F10' 88.7(15) . . ? F11' P2 F10' 92(2) . . ? F12' P2 F10' 171.1(17) . . ? F9' P2 F10' 90.6(19) . . ? F11 P2 F10' 141.4(14) . . ? F7 P2 F10' 83.6(13) . . ? F12 P2 F10' 51.6(12) . . ? F9 P2 F10' 36.2(9) . . ? F10 P2 F10' 130.6(15) . . ? F8 P2 F10' 98.3(13) . . ? F8' P2 F7' 172.1(16) . . ? F11' P2 F7' 89.7(14) . . ? F12' P2 F7' 89.0(15) . . ? F9' P2 F7' 93.7(17) . . ? F11 P2 F7' 62.7(9) . . ? F7 P2 F7' 57.8(11) . . ? F12 P2 F7' 52.6(8) . . ? F9 P2 F7' 117.4(12) . . ? F10 P2 F7' 135.9(12) . . ? F8 P2 F7' 124.7(14) . . ? F10' P2 F7' 84.0(13) . . ? N2 C1 N1 102.7(6) . . ? N2 C1 Ru1 143.8(5) . . ? N1 C1 Ru1 113.5(5) . . ? C3 C2 N2 108.5(7) . . ? C2 C3 N1 106.6(7) . . ? N3 C4 C5 121.7(6) . . ? N3 C4 N1 111.0(6) . . ? C5 C4 N1 127.2(6) . . ? C6 C5 C4 117.3(7) . . ? C5 C6 C7 122.1(7) . . ? C8 C7 C6 116.1(7) . . ? C8 C7 C14 117.6(7) . . ? C6 C7 C14 126.2(7) . . ? N3 C8 C7 122.0(6) . . ? N3 C8 C9 115.1(6) . . ? C7 C8 C9 122.9(7) . . ? N4 C9 C10 124.4(7) . . ? N4 C9 C8 118.0(6) . . ? C10 C9 C8 117.7(7) . . ? C11 C10 C9 115.0(7) . . ? C11 C10 C15 127.3(8) . . ? C9 C10 C15 117.7(7) . . ? C12 C11 C10 120.7(8) . . ? C11 C12 C13 120.1(8) . . ? N4 C13 C12 122.3(8) . . ? C15 C14 C7 120.2(8) . . ? C14 C15 C10 123.9(8) . . ? N2 C16 C17 113.7(6) . . ? C18 C17 N5 123.7(9) . . ? C18 C17 C16 118.6(9) . . ? N5 C17 C16 117.7(8) . . ? C17 C18 C19 117.7(11) . . ? C20 C19 C18 120.0(13) . . ? C19 C20 C21 120.4(12) . . ? N5 C21 C20 120.8(12) . . ? N6 C22 C23 179.6(10) . . ? N7 C24 C25 179.2(8) . . ? N8 C26 C27 177.4(9) . . ? N9 C28 C29 175.5(15) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.768 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.095 #===END data_100111_lgb1231r1 _database_code_depnum_ccdc_archive 'CCDC 832966' #TrackingRef '- Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H39 F12 N9 P2 Ru' _chemical_formula_weight 1036.81 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 19.5793(9) _cell_length_b 14.3329(6) _cell_length_c 16.3835(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.407(4) _cell_angle_gamma 90.00 _cell_volume 4596.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5491 _cell_measurement_theta_min 3.0210 _cell_measurement_theta_max 29.4792 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.499 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8687 _exptl_absorpt_correction_T_max 0.9289 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10462 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4049 _reflns_number_gt 3502 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro(Oxford Diffraction Ltd.)' _computing_cell_refinement 'CrysAlisPro(Oxford Diffraction Ltd.)' _computing_data_reduction 'CrysAlisPro(Oxford Diffraction Ltd.)' _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^)+(0.1458P)^2^+14.8245P] 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 4049 _refine_ls_number_parameters 287 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.2199 _refine_ls_wR_factor_gt 0.2077 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.002 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 0.69789(4) 0.7500 0.0318(3) Uani 1 2 d S . . P1 P 0.27155(9) 0.86549(12) 0.12754(11) 0.0534(5) Uani 1 1 d . . . F1 F 0.2821(4) 0.8830(5) 0.0335(4) 0.127(2) Uani 1 1 d . . . F2 F 0.2490(3) 0.9719(3) 0.1363(4) 0.0897(15) Uani 1 1 d . . . F3 F 0.1950(3) 0.8441(4) 0.1103(5) 0.120(2) Uani 1 1 d . . . F4 F 0.2613(5) 0.8528(7) 0.2196(4) 0.169(4) Uani 1 1 d . . . F5 F 0.3484(3) 0.8922(5) 0.1404(5) 0.135(3) Uani 1 1 d . . . F6 F 0.2932(3) 0.7617(4) 0.1179(4) 0.1094(19) Uani 1 1 d . . . N1 N 0.3882(3) 0.8564(4) 0.7193(3) 0.0509(13) Uani 1 1 d . . . N2 N 0.4048(2) 0.8060(3) 0.8410(3) 0.0409(11) Uani 1 1 d . . . N3 N 0.4838(2) 0.6982(3) 0.8702(3) 0.0340(10) Uani 1 1 d . . . N4 N 0.5713(2) 0.5913(3) 0.7960(3) 0.0368(10) Uani 1 1 d . . . N5 N 0.5000 0.168(3) 0.7500 0.38(2) Uani 1 2 d SDU . . C1 C 0.4260(3) 0.7951(4) 0.7612(4) 0.0385(12) Uani 1 1 d . . . C3 C 0.6136(3) 0.5352(4) 0.7588(4) 0.0470(14) Uani 1 1 d . . . H3 H 0.6162 0.5388 0.7023 0.056 Uiso 1 1 calc R . . C4 C 0.6551(3) 0.4699(5) 0.8008(5) 0.0593(17) Uani 1 1 d . . . H4 H 0.6830 0.4301 0.7716 0.071 Uiso 1 1 calc R . . C5 C 0.6546(3) 0.4645(5) 0.8829(5) 0.0610(18) Uani 1 1 d . . . H5 H 0.6829 0.4226 0.9107 0.073 Uiso 1 1 calc R . . C6 C 0.6101(3) 0.5240(4) 0.9262(4) 0.0514(15) Uani 1 1 d . . . C7 C 0.6036(4) 0.5255(6) 1.0129(5) 0.069(2) Uani 1 1 d . . . H7 H 0.6314 0.4866 1.0446 0.082 Uiso 1 1 calc R . . C8 C 0.5586(4) 0.5815(6) 1.0503(4) 0.0644(19) Uani 1 1 d . . . H8 H 0.5559 0.5798 1.1069 0.077 Uiso 1 1 calc R . . C9 C 0.5153(3) 0.6428(5) 1.0048(4) 0.0508(15) Uani 1 1 d . . . C10 C 0.4639(4) 0.7001(4) 1.0358(4) 0.0537(16) Uani 1 1 d . . . H10 H 0.4564 0.7004 1.0917 0.064 Uiso 1 1 calc R . . C11 C 0.4247(3) 0.7555(5) 0.9855(4) 0.0534(15) Uani 1 1 d . . . H11 H 0.3910 0.7937 1.0066 0.064 Uiso 1 1 calc R . . C12 C 0.4365(3) 0.7535(4) 0.9021(3) 0.0395(12) Uani 1 1 d . . . C13 C 0.3547(3) 0.8752(5) 0.8453(5) 0.0562(16) Uani 1 1 d . . . H13 H 0.3328 0.8956 0.8917 0.067 Uiso 1 1 calc R . . C14 C 0.3449(4) 0.9056(5) 0.7698(4) 0.0614(18) Uani 1 1 d . . . H14 H 0.3143 0.9520 0.7533 0.074 Uiso 1 1 calc R . . C15 C 0.3907(6) 0.8695(8) 0.6304(6) 0.115(3) Uani 1 1 d DU . . H15A H 0.4338 0.8466 0.6103 0.138 Uiso 1 1 calc R . . H15B H 0.3868 0.9352 0.6170 0.138 Uiso 1 1 calc R . . C16 C 0.3309(8) 0.8148(11) 0.5911(9) 0.155(4) Uani 1 1 d DU . . H16A H 0.3314 0.7512 0.6115 0.186 Uiso 1 1 calc R . . H16B H 0.2881 0.8433 0.6063 0.186 Uiso 1 1 calc R . . C17 C 0.3353(11) 0.8136(11) 0.5002(10) 0.170(4) Uani 1 1 d DU . . H17A H 0.3132 0.7564 0.4820 0.204 Uiso 1 1 calc R . . H17B H 0.3833 0.8068 0.4884 0.204 Uiso 1 1 calc R . . C18 C 0.3082(11) 0.8901(14) 0.4446(13) 0.211(6) Uiso 1 1 d DU . . H18A H 0.2757 0.9271 0.4732 0.316 Uiso 1 1 calc R . . H18B H 0.2864 0.8627 0.3972 0.316 Uiso 1 1 calc R . . H18C H 0.3453 0.9289 0.4281 0.316 Uiso 1 1 calc R . . C19 C 0.5222(3) 0.6423(4) 0.9199(3) 0.0405(12) Uani 1 1 d . . . C20 C 0.5692(3) 0.5850(4) 0.8794(3) 0.0404(12) Uani 1 1 d . . . C21 C 0.5000 0.346(3) 0.7500 0.37(2) Uani 1 2 d SDU . . H21A H 0.5011 0.3619 0.6949 0.555 Uiso 0.50 1 d PR . . H21B H 0.5395 0.3619 0.7800 0.555 Uiso 0.50 1 d PR . . H21C H 0.4594 0.3619 0.7753 0.555 Uiso 0.50 1 d PR . . C22 C 0.5000 0.244(3) 0.7500 0.35(2) Uani 1 2 d SDU . . 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 0.0310(4) 0.0375(4) 0.0269(4) 0.000 0.0021(2) 0.000 P1 0.0474(9) 0.0573(10) 0.0559(10) -0.0105(8) 0.0059(8) -0.0013(7) F1 0.169(6) 0.140(5) 0.074(3) 0.013(3) 0.044(4) 0.055(5) F2 0.085(3) 0.067(3) 0.117(4) -0.034(3) 0.006(3) -0.001(2) F3 0.064(3) 0.089(4) 0.206(8) -0.013(4) -0.010(4) -0.023(3) F4 0.228(9) 0.211(8) 0.069(4) 0.030(5) 0.042(5) 0.103(8) F5 0.066(3) 0.122(5) 0.214(8) -0.016(5) -0.033(4) -0.005(3) F6 0.116(4) 0.064(3) 0.149(6) -0.008(3) 0.026(4) 0.024(3) N1 0.048(3) 0.054(3) 0.050(3) 0.010(2) 0.002(2) 0.018(2) N2 0.035(2) 0.046(3) 0.042(3) -0.0029(19) 0.007(2) 0.0062(19) N3 0.034(2) 0.038(2) 0.029(2) 0.0006(17) 0.0021(19) -0.0039(17) N4 0.034(2) 0.041(2) 0.036(2) -0.0001(19) 0.0051(18) -0.0024(19) N5 0.58(4) 0.36(5) 0.190(16) 0.000 -0.23(2) 0.000 C1 0.035(3) 0.045(3) 0.037(3) 0.000(2) 0.003(2) 0.000(2) C3 0.038(3) 0.049(3) 0.055(4) -0.001(3) 0.008(3) 0.003(3) C4 0.048(4) 0.061(4) 0.070(5) 0.002(3) 0.011(3) 0.014(3) C5 0.049(4) 0.058(4) 0.075(5) 0.012(3) -0.005(3) 0.013(3) C6 0.043(3) 0.055(3) 0.056(4) 0.013(3) -0.003(3) 0.000(3) C7 0.068(5) 0.081(5) 0.055(4) 0.024(4) -0.012(4) 0.009(4) C8 0.069(4) 0.086(5) 0.038(3) 0.012(3) -0.006(3) 0.006(4) C9 0.058(4) 0.061(4) 0.034(3) 0.007(3) -0.004(3) -0.009(3) C10 0.065(4) 0.066(4) 0.031(3) -0.001(3) 0.010(3) 0.002(3) C11 0.057(4) 0.062(4) 0.042(3) -0.010(3) 0.017(3) -0.002(3) C12 0.039(3) 0.042(3) 0.038(3) -0.001(2) 0.005(2) -0.003(2) C13 0.048(4) 0.054(3) 0.067(4) -0.005(3) 0.014(3) 0.015(3) C14 0.055(4) 0.068(4) 0.062(4) 0.010(3) 0.008(3) 0.026(3) C15 0.136(7) 0.140(7) 0.067(5) -0.009(5) -0.026(5) 0.086(6) C16 0.171(8) 0.181(8) 0.112(7) -0.017(6) -0.031(7) 0.068(7) C17 0.186(8) 0.194(8) 0.128(7) -0.014(7) -0.021(7) 0.062(7) C19 0.039(3) 0.045(3) 0.037(3) 0.005(2) 0.000(2) -0.002(2) C20 0.040(3) 0.043(3) 0.038(3) 0.006(2) -0.004(2) -0.002(2) C21 0.58(4) 0.36(5) 0.158(16) 0.000 -0.20(2) 0.000 C22 0.57(4) 0.33(5) 0.129(14) 0.000 -0.24(2) 0.000 _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 N3 2.003(5) 2_656 ? Ru1 N3 2.003(5) . ? Ru1 C1 2.022(6) 2_656 ? Ru1 C1 2.022(5) . ? Ru1 N4 2.190(4) 2_656 ? Ru1 N4 2.190(4) . ? P1 F4 1.537(6) . ? P1 F3 1.550(5) . ? P1 F6 1.557(5) . ? P1 F5 1.562(6) . ? P1 F1 1.579(6) . ? P1 F2 1.595(5) . ? N1 C1 1.328(7) . ? N1 C14 1.391(8) . ? N1 C15 1.470(11) . ? N2 C12 1.387(7) . ? N2 C1 1.390(8) . ? N2 C13 1.397(7) . ? N3 C12 1.335(7) . ? N3 C19 1.356(7) . ? N4 C3 1.314(7) . ? N4 C20 1.371(7) . ? N5 C22 1.09(2) . ? C3 C4 1.408(9) . ? C3 H3 0.9300 . ? C4 C5 1.347(10) . ? C4 H4 0.9300 . ? C5 C6 1.422(10) . ? C5 H5 0.9300 . ? C6 C20 1.401(8) . ? C6 C7 1.428(10) . ? C7 C8 1.350(11) . ? C7 H7 0.9300 . ? C8 C9 1.421(9) . ? C8 H8 0.9300 . ? C9 C19 1.401(8) . ? C9 C10 1.404(10) . ? C10 C11 1.366(10) . ? C10 H10 0.9300 . ? C11 C12 1.393(8) . ? C11 H11 0.9300 . ? C13 C14 1.321(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.538(15) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.494(15) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.513(16) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.411(8) . ? C21 C22 1.46(2) . ? C21 H21A 0.9331 . ? C21 H21B 0.9346 . ? C21 H21C 0.9349 . ? 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 N3 Ru1 N3 179.8(2) 2_656 . ? N3 Ru1 C1 77.2(2) 2_656 2_656 ? N3 Ru1 C1 102.7(2) . 2_656 ? N3 Ru1 C1 102.7(2) 2_656 . ? N3 Ru1 C1 77.2(2) . . ? C1 Ru1 C1 92.9(3) 2_656 . ? N3 Ru1 N4 77.18(17) 2_656 2_656 ? N3 Ru1 N4 102.99(17) . 2_656 ? C1 Ru1 N4 154.3(2) 2_656 2_656 ? C1 Ru1 N4 93.44(19) . 2_656 ? N3 Ru1 N4 102.99(16) 2_656 . ? N3 Ru1 N4 77.18(17) . . ? C1 Ru1 N4 93.44(19) 2_656 . ? C1 Ru1 N4 154.3(2) . . ? N4 Ru1 N4 91.5(2) 2_656 . ? F4 P1 F3 90.3(5) . . ? F4 P1 F6 91.6(4) . . ? F3 P1 F6 93.3(3) . . ? F4 P1 F5 92.6(5) . . ? F3 P1 F5 176.2(4) . . ? F6 P1 F5 89.1(4) . . ? F4 P1 F1 177.7(5) . . ? F3 P1 F1 90.2(4) . . ? F6 P1 F1 90.6(4) . . ? F5 P1 F1 86.8(5) . . ? F4 P1 F2 89.0(4) . . ? F3 P1 F2 86.4(3) . . ? F6 P1 F2 179.3(4) . . ? F5 P1 F2 91.2(3) . . ? F1 P1 F2 88.8(3) . . ? C1 N1 C14 111.6(5) . . ? C1 N1 C15 124.4(6) . . ? C14 N1 C15 124.0(6) . . ? C12 N2 C1 118.6(4) . . ? C12 N2 C13 130.6(5) . . ? C1 N2 C13 110.7(5) . . ? C12 N3 C19 119.8(5) . . ? C12 N3 Ru1 120.9(4) . . ? C19 N3 Ru1 119.3(4) . . ? C3 N4 C20 117.1(5) . . ? C3 N4 Ru1 132.1(4) . . ? C20 N4 Ru1 110.8(3) . . ? N1 C1 N2 103.7(5) . . ? N1 C1 Ru1 143.1(5) . . ? N2 C1 Ru1 113.2(4) . . ? N4 C3 C4 122.9(6) . . ? N4 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? C5 C4 C3 120.4(6) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 119.0(6) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C20 C6 C5 116.7(6) . . ? C20 C6 C7 118.1(6) . . ? C5 C6 C7 125.2(6) . . ? C8 C7 C6 122.4(6) . . ? C8 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C7 C8 C9 121.1(6) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C19 C9 C10 116.8(6) . . ? C19 C9 C8 116.5(6) . . ? C10 C9 C8 126.6(6) . . ? C11 C10 C9 121.2(6) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 118.5(6) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? N3 C12 N2 110.0(5) . . ? N3 C12 C11 121.9(5) . . ? N2 C12 C11 128.0(5) . . ? C14 C13 N2 105.9(6) . . ? C14 C13 H13 127.1 . . ? N2 C13 H13 127.1 . . ? C13 C14 N1 108.2(5) . . ? C13 C14 H14 125.9 . . ? N1 C14 H14 125.9 . . ? N1 C15 C16 107.8(10) . . ? N1 C15 H15A 110.1 . . ? C16 C15 H15A 110.1 . . ? N1 C15 H15B 110.1 . . ? C16 C15 H15B 110.1 . . ? H15A C15 H15B 108.5 . . ? C17 C16 C15 111.2(14) . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C18 124.3(15) . . ? C16 C17 H17A 106.3 . . ? C18 C17 H17A 106.3 . . ? C16 C17 H17B 106.2 . . ? C18 C17 H17B 106.2 . . ? H17A C17 H17B 106.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C9 121.8(5) . . ? N3 C19 C20 114.9(5) . . ? C9 C19 C20 123.4(5) . . ? N4 C20 C6 123.8(5) . . ? N4 C20 C19 117.8(5) . . ? C6 C20 C19 118.4(5) . . ? C22 C21 H21A 104.4 . . ? C22 C21 H21B 104.3 . . ? H21A C21 H21B 114.1 . . ? C22 C21 H21C 104.3 . . ? H21A C21 H21C 114.1 . . ? H21B C21 H21C 114.0 . . ? N5 C22 C21 180.00(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ru1 N3 C12 46.3(6) 2_656 . . . ? C1 Ru1 N3 C12 91.4(4) 2_656 . . . ? C1 Ru1 N3 C12 1.3(4) . . . . ? N4 Ru1 N3 C12 -89.4(4) 2_656 . . . ? N4 Ru1 N3 C12 -178.0(4) . . . . ? N3 Ru1 N3 C19 -132.8(6) 2_656 . . . ? C1 Ru1 N3 C19 -87.7(4) 2_656 . . . ? C1 Ru1 N3 C19 -177.8(4) . . . . ? N4 Ru1 N3 C19 91.6(4) 2_656 . . . ? N4 Ru1 N3 C19 3.0(4) . . . . ? N3 Ru1 N4 C3 -2.9(5) 2_656 . . . ? N3 Ru1 N4 C3 177.3(5) . . . . ? C1 Ru1 N4 C3 -80.5(5) 2_656 . . . ? C1 Ru1 N4 C3 175.5(5) . . . . ? N4 Ru1 N4 C3 74.3(5) 2_656 . . . ? N3 Ru1 N4 C20 177.1(3) 2_656 . . . ? N3 Ru1 N4 C20 -2.7(3) . . . . ? C1 Ru1 N4 C20 99.5(4) 2_656 . . . ? C1 Ru1 N4 C20 -4.5(6) . . . . ? N4 Ru1 N4 C20 -105.7(4) 2_656 . . . ? C14 N1 C1 N2 0.6(7) . . . . ? C15 N1 C1 N2 -178.3(8) . . . . ? C14 N1 C1 Ru1 -178.6(6) . . . . ? C15 N1 C1 Ru1 2.5(12) . . . . ? C12 N2 C1 N1 -177.8(5) . . . . ? C13 N2 C1 N1 -0.7(6) . . . . ? C12 N2 C1 Ru1 1.7(6) . . . . ? C13 N2 C1 Ru1 178.8(4) . . . . ? N3 Ru1 C1 N1 -2.1(8) 2_656 . . . ? N3 Ru1 C1 N1 177.7(8) . . . . ? C1 Ru1 C1 N1 75.4(7) 2_656 . . . ? N4 Ru1 C1 N1 -79.8(7) 2_656 . . . ? N4 Ru1 C1 N1 179.5(6) . . . . ? N3 Ru1 C1 N2 178.7(4) 2_656 . . . ? N3 Ru1 C1 N2 -1.5(4) . . . . ? C1 Ru1 C1 N2 -103.8(4) 2_656 . . . ? N4 Ru1 C1 N2 101.1(4) 2_656 . . . ? N4 Ru1 C1 N2 0.3(7) . . . . ? C20 N4 C3 C4 0.8(8) . . . . ? Ru1 N4 C3 C4 -179.3(5) . . . . ? N4 C3 C4 C5 -2.3(10) . . . . ? C3 C4 C5 C6 1.8(11) . . . . ? C4 C5 C6 C20 0.1(10) . . . . ? C4 C5 C6 C7 179.4(7) . . . . ? C20 C6 C7 C8 1.7(11) . . . . ? C5 C6 C7 C8 -177.6(7) . . . . ? C6 C7 C8 C9 -0.5(12) . . . . ? C7 C8 C9 C19 -0.3(10) . . . . ? C7 C8 C9 C10 176.0(7) . . . . ? C19 C9 C10 C11 -2.7(10) . . . . ? C8 C9 C10 C11 -179.1(7) . . . . ? C9 C10 C11 C12 0.5(10) . . . . ? C19 N3 C12 N2 178.4(5) . . . . ? Ru1 N3 C12 N2 -0.7(6) . . . . ? C19 N3 C12 C11 -0.3(8) . . . . ? Ru1 N3 C12 C11 -179.4(4) . . . . ? C1 N2 C12 N3 -0.7(7) . . . . ? C13 N2 C12 N3 -177.2(6) . . . . ? C1 N2 C12 C11 177.9(6) . . . . ? C13 N2 C12 C11 1.4(10) . . . . ? C10 C11 C12 N3 1.1(9) . . . . ? C10 C11 C12 N2 -177.3(6) . . . . ? C12 N2 C13 C14 177.1(6) . . . . ? C1 N2 C13 C14 0.5(7) . . . . ? N2 C13 C14 N1 -0.1(8) . . . . ? C1 N1 C14 C13 -0.4(9) . . . . ? C15 N1 C14 C13 178.5(8) . . . . ? C1 N1 C15 C16 98.5(10) . . . . ? C14 N1 C15 C16 -80.3(11) . . . . ? N1 C15 C16 C17 -172.2(10) . . . . ? C15 C16 C17 C18 -85(2) . . . . ? C12 N3 C19 C9 -2.1(8) . . . . ? Ru1 N3 C19 C9 177.0(4) . . . . ? C12 N3 C19 C20 178.3(5) . . . . ? Ru1 N3 C19 C20 -2.7(6) . . . . ? C10 C9 C19 N3 3.6(9) . . . . ? C8 C9 C19 N3 -179.7(6) . . . . ? C10 C9 C19 C20 -176.8(6) . . . . ? C8 C9 C19 C20 -0.1(9) . . . . ? C3 N4 C20 C6 1.2(8) . . . . ? Ru1 N4 C20 C6 -178.8(5) . . . . ? C3 N4 C20 C19 -177.7(5) . . . . ? Ru1 N4 C20 C19 2.3(6) . . . . ? C5 C6 C20 N4 -1.6(9) . . . . ? C7 C6 C20 N4 179.0(6) . . . . ? C5 C6 C20 C19 177.3(6) . . . . ? C7 C6 C20 C19 -2.1(9) . . . . ? N3 C19 C20 N4 0.0(7) . . . . ? C9 C19 C20 N4 -179.7(5) . . . . ? N3 C19 C20 C6 -179.0(5) . . . . ? C9 C19 C20 C6 1.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.590 _refine_diff_density_min -1.326 _refine_diff_density_rms 0.158 #===END data_090805b _database_code_depnum_ccdc_archive 'CCDC 832967' #TrackingRef '- Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H36 Cl F6 N7 P2 Ru' _chemical_formula_weight 963.25 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 22.613(2) _cell_length_b 12.4255(14) _cell_length_c 29.170(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8196.1(14) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5163 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.4 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3904 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7838 _exptl_absorpt_correction_T_max 0.9266 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33859 _diffrn_reflns_av_R_equivalents 0.0798 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7234 _reflns_number_gt 4250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0917P)^2^+59.6935P] 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 7234 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1303 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2289 _refine_ls_wR_factor_gt 0.1814 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.50569(3) 0.52581(5) 0.85579(2) 0.0340(2) Uani 1 1 d . . . Cl1 Cl 0.54685(10) 0.59440(18) 0.78546(7) 0.0447(5) Uani 1 1 d . . . F1 F 0.6284(6) 0.1890(11) 1.0297(4) 0.180(5) Uani 1 1 d . . . F2 F 0.6071(6) 0.1973(12) 0.9290(3) 0.195(5) Uani 1 1 d . . . F3 F 0.5625(4) 0.1215(9) 0.9844(4) 0.159(4) Uani 1 1 d . . . F4 F 0.6557(5) 0.0943(9) 0.9724(4) 0.164(4) Uani 1 1 d . . . F5 F 0.6699(4) 0.2701(8) 0.9714(4) 0.159(4) Uani 1 1 d . . . F6 F 0.5794(5) 0.2913(10) 0.9951(5) 0.182(5) Uani 1 1 d . . . N1 N 0.5861(3) 0.3483(6) 0.8426(2) 0.0460(18) Uani 1 1 d . . . N2 N 0.5033(3) 0.2781(6) 0.8244(2) 0.0473(18) Uani 1 1 d . . . N3 N 0.5925(3) 0.5145(6) 0.8738(2) 0.0408(17) Uani 1 1 d . . . N4 N 0.5245(3) 0.6841(6) 0.8878(2) 0.0428(17) Uani 1 1 d . . . N5 N 0.3619(4) 0.1467(8) 0.8512(3) 0.070(3) Uani 1 1 d . . . N6 N 0.4768(3) 0.4689(6) 0.9167(2) 0.0427(17) Uani 1 1 d . . . N7 N 0.1818(7) 0.8408(16) 0.2549(6) 0.151(7) Uani 1 1 d . . . P1 P 0.40788(9) 0.55206(18) 0.83109(7) 0.0366(5) Uani 1 1 d . . . P2 P 0.61623(14) 0.1970(3) 0.97778(11) 0.0724(9) Uani 1 1 d . . . C1 C 0.5256(4) 0.3741(7) 0.8370(3) 0.042(2) Uani 1 1 d . . . C2 C 0.5467(5) 0.1990(8) 0.8195(3) 0.057(3) Uani 1 1 d . . . H2 H 0.5407 0.1283 0.8102 0.068 Uiso 1 1 calc R . . C3 C 0.5982(5) 0.2434(8) 0.8308(3) 0.057(3) Uani 1 1 d . . . H3 H 0.6351 0.2102 0.8307 0.069 Uiso 1 1 calc R . . C4 C 0.6225(4) 0.4275(8) 0.8618(3) 0.051(2) Uani 1 1 d . . . C5 C 0.6835(5) 0.4192(10) 0.8699(4) 0.064(3) Uani 1 1 d . . . H5 H 0.7048 0.3580 0.8619 0.077 Uiso 1 1 calc R . . C6 C 0.7099(5) 0.5061(10) 0.8902(4) 0.065(3) Uani 1 1 d . . . H6 H 0.7502 0.5026 0.8965 0.078 Uiso 1 1 calc R . . C7 C 0.6796(4) 0.5991(10) 0.9019(3) 0.060(3) Uani 1 1 d . . . C8 C 0.6200(4) 0.6010(8) 0.8921(3) 0.049(2) Uani 1 1 d . . . C9 C 0.5824(4) 0.6903(8) 0.8995(3) 0.049(2) Uani 1 1 d . . . C10 C 0.6083(5) 0.7825(9) 0.9203(3) 0.056(3) Uani 1 1 d . . . C11 C 0.5704(5) 0.8692(9) 0.9289(3) 0.064(3) Uani 1 1 d . . . H11 H 0.5854 0.9320 0.9419 0.076 Uiso 1 1 calc R . . C12 C 0.5131(5) 0.8626(9) 0.9188(3) 0.064(3) Uani 1 1 d . . . H12 H 0.4878 0.9197 0.9250 0.076 Uiso 1 1 calc R . . C13 C 0.4912(4) 0.7666(7) 0.8982(3) 0.050(2) Uani 1 1 d . . . H13 H 0.4510 0.7623 0.8919 0.060 Uiso 1 1 calc R . . C14 C 0.7034(5) 0.6939(11) 0.9232(4) 0.070(3) Uani 1 1 d . . . H14 H 0.7432 0.6949 0.9313 0.084 Uiso 1 1 calc R . . C15 C 0.6708(5) 0.7794(10) 0.9315(3) 0.066(3) Uani 1 1 d . . . H15 H 0.6883 0.8394 0.9449 0.079 Uiso 1 1 calc R . . C16 C 0.4413(4) 0.2517(8) 0.8200(3) 0.052(2) Uani 1 1 d . . . H16A H 0.4357 0.2119 0.7917 0.063 Uiso 1 1 calc R . . H16B H 0.4190 0.3181 0.8175 0.063 Uiso 1 1 calc R . . C17 C 0.4162(4) 0.1864(8) 0.8591(3) 0.054(2) Uani 1 1 d . . . C18 C 0.4459(5) 0.1724(8) 0.8999(3) 0.061(3) Uani 1 1 d . . . H18 H 0.4834 0.2015 0.9043 0.073 Uiso 1 1 calc R . . C19 C 0.4184(5) 0.1142(10) 0.9338(4) 0.075(3) Uani 1 1 d . . . H19 H 0.4375 0.1035 0.9617 0.090 Uiso 1 1 calc R . . C20 C 0.3631(6) 0.0718(10) 0.9270(4) 0.080(4) Uani 1 1 d . . . H20 H 0.3438 0.0321 0.9495 0.096 Uiso 1 1 calc R . . C21 C 0.3376(6) 0.0912(10) 0.8849(4) 0.079(3) Uani 1 1 d . . . H21 H 0.3001 0.0629 0.8798 0.095 Uiso 1 1 calc R . . C22 C 0.3855(4) 0.6899(8) 0.8190(3) 0.050(2) Uani 1 1 d . . . C23 C 0.3288(5) 0.7268(10) 0.8247(4) 0.076(3) Uani 1 1 d . . . H23 H 0.3008 0.6822 0.8383 0.091 Uiso 1 1 calc R . . C24 C 0.3122(6) 0.8292(11) 0.8106(5) 0.093(4) Uani 1 1 d . . . H24 H 0.2737 0.8527 0.8153 0.112 Uiso 1 1 calc R . . C25 C 0.3524(6) 0.8961(10) 0.7898(5) 0.086(4) Uani 1 1 d . . . H25 H 0.3412 0.9645 0.7802 0.103 Uiso 1 1 calc R . . C26 C 0.4089(5) 0.8613(9) 0.7835(4) 0.070(3) Uani 1 1 d . . . H26 H 0.4366 0.9061 0.7696 0.084 Uiso 1 1 calc R . . C27 C 0.4250(4) 0.7594(8) 0.7976(3) 0.053(2) Uani 1 1 d . . . H27 H 0.4636 0.7364 0.7926 0.063 Uiso 1 1 calc R . . C28 C 0.3536(4) 0.5068(8) 0.8735(3) 0.046(2) Uani 1 1 d . . . C29 C 0.3463(4) 0.5680(9) 0.9134(3) 0.060(3) Uani 1 1 d . . . H29 H 0.3656 0.6338 0.9161 0.072 Uiso 1 1 calc R . . C30 C 0.3109(5) 0.5318(11) 0.9486(4) 0.072(3) Uani 1 1 d . . . H30 H 0.3064 0.5740 0.9746 0.087 Uiso 1 1 calc R . . C31 C 0.2828(5) 0.4363(11) 0.9459(4) 0.073(3) Uani 1 1 d . . . H31 H 0.2587 0.4131 0.9698 0.087 Uiso 1 1 calc R . . C32 C 0.2901(5) 0.3739(10) 0.9075(4) 0.072(3) Uani 1 1 d . . . H32 H 0.2715 0.3073 0.9056 0.087 Uiso 1 1 calc R . . C33 C 0.3252(4) 0.4099(8) 0.8712(3) 0.057(3) Uani 1 1 d . . . H33 H 0.3294 0.3674 0.8452 0.069 Uiso 1 1 calc R . . C34 C 0.3834(4) 0.4916(7) 0.7768(3) 0.047(2) Uani 1 1 d . . . C35 C 0.4237(4) 0.4474(8) 0.7466(3) 0.051(2) Uani 1 1 d . . . H35 H 0.4633 0.4440 0.7550 0.061 Uiso 1 1 calc R . . C36 C 0.4069(5) 0.4084(9) 0.7047(3) 0.065(3) Uani 1 1 d . . . H36 H 0.4349 0.3795 0.6849 0.078 Uiso 1 1 calc R . . C37 C 0.3494(6) 0.4122(11) 0.6924(4) 0.080(4) Uani 1 1 d . . . H37 H 0.3378 0.3844 0.6642 0.096 Uiso 1 1 calc R . . C38 C 0.3079(6) 0.4564(11) 0.7209(4) 0.082(4) Uani 1 1 d . . . H38 H 0.2684 0.4597 0.7120 0.099 Uiso 1 1 calc R . . C39 C 0.3253(5) 0.4960(9) 0.7631(4) 0.069(3) Uani 1 1 d . . . H39 H 0.2972 0.5262 0.7825 0.082 Uiso 1 1 calc R . . C40 C 0.4612(5) 0.4330(9) 0.9494(3) 0.056(3) Uani 1 1 d . . . C41 C 0.4400(6) 0.3881(10) 0.9924(3) 0.075(3) Uani 1 1 d . . . H41A H 0.4251 0.4450 1.0114 0.113 Uiso 1 1 calc R . . H41B H 0.4720 0.3524 1.0078 0.113 Uiso 1 1 calc R . . H41C H 0.4090 0.3374 0.9863 0.113 Uiso 1 1 calc R . . C42 C 0.2165(13) 0.821(3) 0.2269(12) 0.215(13) Uani 1 1 d . . . C43 C 0.2613(11) 0.795(2) 0.1912(9) 0.215(12) Uani 1 1 d . . . H43A H 0.2814 0.8589 0.1819 0.322 Uiso 1 1 calc R . . H43B H 0.2419 0.7631 0.1651 0.322 Uiso 1 1 calc R . . H43C H 0.2894 0.7443 0.2035 0.322 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0377(4) 0.0371(4) 0.0271(3) 0.0000(3) 0.0034(3) -0.0026(3) Cl1 0.0511(13) 0.0499(13) 0.0332(10) 0.0069(10) 0.0099(9) -0.0018(10) F1 0.227(13) 0.194(12) 0.119(8) -0.010(8) -0.027(8) -0.018(10) F2 0.243(14) 0.240(14) 0.102(7) 0.032(8) -0.032(8) -0.046(11) F3 0.122(8) 0.171(10) 0.184(10) -0.032(8) 0.031(7) -0.060(7) F4 0.142(9) 0.127(9) 0.222(12) -0.039(8) 0.018(8) 0.012(7) F5 0.125(7) 0.142(9) 0.209(11) -0.050(8) 0.066(8) -0.054(7) F6 0.151(9) 0.147(10) 0.247(14) -0.007(10) 0.023(9) 0.050(8) N1 0.050(5) 0.048(5) 0.039(4) 0.005(3) 0.007(3) 0.002(4) N2 0.059(5) 0.044(4) 0.040(4) -0.002(3) 0.005(4) 0.004(4) N3 0.035(4) 0.056(5) 0.032(3) 0.009(3) 0.004(3) -0.002(4) N4 0.049(5) 0.045(5) 0.034(4) -0.001(3) 0.007(3) -0.010(4) N5 0.071(6) 0.066(6) 0.073(6) 0.011(5) 0.001(5) -0.016(5) N6 0.049(4) 0.043(4) 0.036(4) -0.001(4) -0.004(3) -0.005(4) N7 0.096(11) 0.194(17) 0.163(15) -0.050(13) 0.052(10) 0.001(11) P1 0.0362(12) 0.0411(13) 0.0327(11) -0.0023(9) 0.0049(9) -0.0024(9) P2 0.0645(19) 0.091(2) 0.0614(19) 0.0070(17) 0.0038(15) -0.0020(18) C1 0.050(5) 0.043(5) 0.032(4) 0.001(4) 0.010(4) 0.002(4) C2 0.070(7) 0.049(6) 0.052(6) -0.003(5) 0.009(5) 0.011(5) C3 0.065(7) 0.051(6) 0.055(6) 0.005(5) 0.011(5) 0.022(5) C4 0.055(6) 0.056(6) 0.043(5) 0.011(5) 0.007(5) 0.001(5) C5 0.053(6) 0.073(8) 0.065(7) 0.012(6) 0.003(5) 0.004(6) C6 0.050(6) 0.083(9) 0.062(7) 0.013(6) -0.010(5) -0.010(6) C7 0.052(6) 0.078(8) 0.049(6) 0.009(6) -0.003(5) -0.014(6) C8 0.050(6) 0.060(6) 0.036(5) 0.008(5) -0.001(4) -0.011(5) C9 0.057(6) 0.057(6) 0.032(5) 0.006(4) 0.002(4) -0.016(5) C10 0.066(7) 0.064(7) 0.039(5) 0.000(5) 0.003(5) -0.023(5) C11 0.080(8) 0.061(7) 0.051(6) -0.003(5) 0.006(6) -0.022(6) C12 0.082(8) 0.060(7) 0.049(6) -0.012(5) 0.008(6) -0.011(6) C13 0.057(6) 0.050(6) 0.044(5) -0.008(4) 0.004(4) -0.004(5) C14 0.064(7) 0.088(9) 0.057(7) 0.010(6) -0.010(6) -0.021(7) C15 0.073(8) 0.079(9) 0.048(6) 0.004(6) -0.004(6) -0.030(7) C16 0.064(6) 0.045(6) 0.048(5) -0.002(5) 0.003(5) -0.002(5) C17 0.063(6) 0.045(6) 0.054(6) 0.003(5) 0.003(5) 0.000(5) C18 0.066(7) 0.061(7) 0.056(6) 0.008(5) 0.001(5) -0.004(5) C19 0.080(8) 0.074(8) 0.071(7) 0.015(6) 0.002(6) -0.005(7) C20 0.084(9) 0.074(9) 0.082(9) 0.022(7) 0.011(7) -0.013(7) C21 0.075(8) 0.077(9) 0.085(9) 0.016(7) 0.005(7) -0.017(7) C22 0.048(6) 0.049(6) 0.054(6) -0.003(5) 0.006(5) 0.007(4) C23 0.069(8) 0.067(8) 0.092(9) 0.014(7) 0.017(7) 0.011(6) C24 0.078(9) 0.077(9) 0.125(11) 0.021(8) 0.020(8) 0.034(7) C25 0.087(9) 0.060(8) 0.111(10) 0.021(7) 0.020(8) 0.023(7) C26 0.075(8) 0.062(7) 0.073(7) 0.015(6) 0.016(6) 0.006(6) C27 0.052(6) 0.052(6) 0.054(6) 0.007(5) 0.009(5) 0.004(5) C28 0.040(5) 0.054(6) 0.045(5) 0.002(4) 0.001(4) 0.004(4) C29 0.056(6) 0.069(7) 0.055(6) -0.002(5) 0.010(5) -0.012(5) C30 0.066(7) 0.093(9) 0.057(6) -0.009(6) 0.017(6) -0.009(7) C31 0.056(7) 0.092(9) 0.070(8) 0.025(7) 0.017(6) -0.007(6) C32 0.062(7) 0.075(8) 0.081(8) 0.018(7) 0.013(6) -0.013(6) C33 0.051(6) 0.060(7) 0.060(6) 0.002(5) 0.010(5) -0.008(5) C34 0.051(5) 0.048(6) 0.042(5) 0.002(4) -0.004(4) -0.002(4) C35 0.059(6) 0.054(6) 0.041(5) -0.002(4) 0.003(4) -0.001(5) C36 0.075(8) 0.078(8) 0.042(5) -0.013(5) 0.000(5) 0.000(6) C37 0.091(9) 0.097(10) 0.053(7) -0.018(7) -0.012(7) 0.002(8) C38 0.074(8) 0.105(10) 0.069(7) -0.024(7) -0.024(6) 0.006(7) C39 0.063(7) 0.082(8) 0.060(7) -0.014(6) -0.006(5) 0.008(6) C40 0.063(7) 0.068(7) 0.039(5) 0.006(5) 0.001(5) -0.008(5) C41 0.091(9) 0.095(9) 0.040(6) 0.012(6) 0.014(6) -0.016(7) C42 0.16(3) 0.22(3) 0.27(4) -0.05(3) 0.02(2) -0.03(2) C43 0.16(2) 0.22(3) 0.26(3) -0.05(3) 0.02(2) -0.03(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 2.014(9) . ? Ru1 N6 2.020(7) . ? Ru1 N3 2.036(7) . ? Ru1 N4 2.218(7) . ? Ru1 P1 2.349(2) . ? Ru1 Cl1 2.409(2) . ? F1 P2 1.543(11) . ? F2 P2 1.437(10) . ? F3 P2 1.547(9) . ? F4 P2 1.566(11) . ? F5 P2 1.527(9) . ? F6 P2 1.523(11) . ? N1 C3 1.376(12) . ? N1 C4 1.402(12) . ? N1 C1 1.414(11) . ? N2 C1 1.347(11) . ? N2 C2 1.395(12) . ? N2 C16 1.445(11) . ? N3 C4 1.323(12) . ? N3 C8 1.352(11) . ? N4 C13 1.308(11) . ? N4 C9 1.356(12) . ? N5 C21 1.320(13) . ? N5 C17 1.343(13) . ? N6 C40 1.111(11) . ? N7 C42 1.16(3) . ? P1 C22 1.821(10) . ? P1 C28 1.832(9) . ? P1 C34 1.838(9) . ? C2 C3 1.330(14) . ? C4 C5 1.403(14) . ? C5 C6 1.369(15) . ? C6 C7 1.385(15) . ? C7 C8 1.379(13) . ? C7 C14 1.436(15) . ? C8 C9 1.414(14) . ? C9 C10 1.421(13) . ? C10 C11 1.400(15) . ? C10 C15 1.450(15) . ? C11 C12 1.331(15) . ? C12 C13 1.423(13) . ? C14 C15 1.316(16) . ? C16 C17 1.511(13) . ? C17 C18 1.378(13) . ? C18 C19 1.375(14) . ? C19 C20 1.372(16) . ? C20 C21 1.377(16) . ? C22 C23 1.372(14) . ? C22 C27 1.391(13) . ? C23 C24 1.389(16) . ? C24 C25 1.373(17) . ? C25 C26 1.361(15) . ? C26 C27 1.381(14) . ? C28 C33 1.365(13) . ? C28 C29 1.399(13) . ? C29 C30 1.377(14) . ? C30 C31 1.349(16) . ? C31 C32 1.373(16) . ? C32 C33 1.397(14) . ? C34 C39 1.375(14) . ? C34 C35 1.381(13) . ? C35 C36 1.369(13) . ? C36 C37 1.349(15) . ? C37 C38 1.369(16) . ? C38 C39 1.382(15) . ? C40 C41 1.452(13) . ? C42 C43 1.49(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 C1 Ru1 N6 89.1(3) . . ? C1 Ru1 N3 77.9(3) . . ? N6 Ru1 N3 93.4(3) . . ? C1 Ru1 N4 154.4(3) . . ? N6 Ru1 N4 90.1(3) . . ? N3 Ru1 N4 76.6(3) . . ? C1 Ru1 P1 104.9(3) . . ? N6 Ru1 P1 90.8(2) . . ? N3 Ru1 P1 175.0(2) . . ? N4 Ru1 P1 100.8(2) . . ? C1 Ru1 Cl1 90.7(2) . . ? N6 Ru1 Cl1 176.0(2) . . ? N3 Ru1 Cl1 82.65(19) . . ? N4 Ru1 Cl1 88.31(18) . . ? P1 Ru1 Cl1 93.06(8) . . ? C3 N1 C4 130.4(9) . . ? C3 N1 C1 112.3(8) . . ? C4 N1 C1 117.1(8) . . ? C1 N2 C2 112.9(8) . . ? C1 N2 C16 126.0(8) . . ? C2 N2 C16 120.9(8) . . ? C4 N3 C8 121.1(8) . . ? C4 N3 Ru1 118.9(6) . . ? C8 N3 Ru1 119.3(6) . . ? C13 N4 C9 116.9(8) . . ? C13 N4 Ru1 133.0(6) . . ? C9 N4 Ru1 110.0(6) . . ? C21 N5 C17 116.3(10) . . ? C40 N6 Ru1 176.8(8) . . ? C22 P1 C28 103.5(4) . . ? C22 P1 C34 97.7(4) . . ? C28 P1 C34 104.7(4) . . ? C22 P1 Ru1 116.9(3) . . ? C28 P1 Ru1 112.4(3) . . ? C34 P1 Ru1 119.4(3) . . ? F2 P2 F6 104.3(8) . . ? F2 P2 F5 89.5(7) . . ? F6 P2 F5 90.9(7) . . ? F2 P2 F1 175.9(9) . . ? F6 P2 F1 79.8(7) . . ? F5 P2 F1 90.9(7) . . ? F2 P2 F3 90.7(7) . . ? F6 P2 F3 89.8(7) . . ? F5 P2 F3 179.2(8) . . ? F1 P2 F3 88.7(7) . . ? F2 P2 F4 89.2(8) . . ? F6 P2 F4 166.4(7) . . ? F5 P2 F4 91.1(6) . . ? F1 P2 F4 86.8(7) . . ? F3 P2 F4 88.1(6) . . ? N2 C1 N1 101.1(7) . . ? N2 C1 Ru1 145.1(7) . . ? N1 C1 Ru1 113.4(6) . . ? C3 C2 N2 107.4(9) . . ? C2 C3 N1 106.2(9) . . ? N3 C4 N1 112.1(8) . . ? N3 C4 C5 121.4(10) . . ? N1 C4 C5 126.4(10) . . ? C6 C5 C4 116.3(11) . . ? C5 C6 C7 123.3(10) . . ? C8 C7 C6 116.6(10) . . ? C8 C7 C14 116.2(11) . . ? C6 C7 C14 127.2(10) . . ? N3 C8 C7 121.2(10) . . ? N3 C8 C9 114.1(8) . . ? C7 C8 C9 124.7(10) . . ? N4 C9 C8 119.7(9) . . ? N4 C9 C10 123.5(10) . . ? C8 C9 C10 116.8(9) . . ? C11 C10 C9 116.4(10) . . ? C11 C10 C15 125.2(10) . . ? C9 C10 C15 118.4(10) . . ? C12 C11 C10 120.5(10) . . ? C11 C12 C13 119.0(11) . . ? N4 C13 C12 123.6(10) . . ? C15 C14 C7 122.1(11) . . ? C14 C15 C10 121.7(11) . . ? N2 C16 C17 114.9(8) . . ? N5 C17 C18 123.3(10) . . ? N5 C17 C16 114.3(9) . . ? C18 C17 C16 122.4(9) . . ? C19 C18 C17 117.9(10) . . ? C20 C19 C18 120.6(12) . . ? C19 C20 C21 116.4(11) . . ? N5 C21 C20 125.6(12) . . ? C23 C22 C27 116.6(9) . . ? C23 C22 P1 123.4(8) . . ? C27 C22 P1 119.5(7) . . ? C22 C23 C24 121.4(11) . . ? C25 C24 C23 120.5(12) . . ? C26 C25 C24 119.3(11) . . ? C25 C26 C27 119.9(11) . . ? C26 C27 C22 122.3(9) . . ? C33 C28 C29 117.8(9) . . ? C33 C28 P1 123.5(7) . . ? C29 C28 P1 118.2(7) . . ? C30 C29 C28 120.6(10) . . ? C31 C30 C29 121.3(11) . . ? C30 C31 C32 119.1(10) . . ? C31 C32 C33 120.4(11) . . ? C28 C33 C32 120.8(10) . . ? C39 C34 C35 117.5(9) . . ? C39 C34 P1 121.5(8) . . ? C35 C34 P1 120.9(7) . . ? C36 C35 C34 121.8(10) . . ? C37 C36 C35 119.5(11) . . ? C36 C37 C38 120.9(11) . . ? C37 C38 C39 119.2(11) . . ? C34 C39 C38 121.1(11) . . ? N6 C40 C41 178.8(13) . . ? N7 C42 C43 179(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ru1 N3 C4 7.2(6) . . . . ? N6 Ru1 N3 C4 95.5(6) . . . . ? N4 Ru1 N3 C4 -175.2(7) . . . . ? P1 Ru1 N3 C4 -117(2) . . . . ? Cl1 Ru1 N3 C4 -85.2(6) . . . . ? C1 Ru1 N3 C8 178.4(7) . . . . ? N6 Ru1 N3 C8 -93.3(6) . . . . ? N4 Ru1 N3 C8 -4.0(6) . . . . ? P1 Ru1 N3 C8 55(3) . . . . ? Cl1 Ru1 N3 C8 86.1(6) . . . . ? C1 Ru1 N4 C13 -168.9(8) . . . . ? N6 Ru1 N4 C13 -80.7(8) . . . . ? N3 Ru1 N4 C13 -174.2(8) . . . . ? P1 Ru1 N4 C13 10.1(8) . . . . ? Cl1 Ru1 N4 C13 102.9(8) . . . . ? C1 Ru1 N4 C9 8.5(10) . . . . ? N6 Ru1 N4 C9 96.7(6) . . . . ? N3 Ru1 N4 C9 3.2(5) . . . . ? P1 Ru1 N4 C9 -172.5(5) . . . . ? Cl1 Ru1 N4 C9 -79.7(5) . . . . ? C1 Ru1 N6 C40 -10(14) . . . . ? N3 Ru1 N6 C40 -88(14) . . . . ? N4 Ru1 N6 C40 -165(14) . . . . ? P1 Ru1 N6 C40 94(14) . . . . ? Cl1 Ru1 N6 C40 -98(14) . . . . ? C1 Ru1 P1 C22 -153.8(4) . . . . ? N6 Ru1 P1 C22 116.9(4) . . . . ? N3 Ru1 P1 C22 -31(3) . . . . ? N4 Ru1 P1 C22 26.6(4) . . . . ? Cl1 Ru1 P1 C22 -62.3(3) . . . . ? C1 Ru1 P1 C28 86.7(4) . . . . ? N6 Ru1 P1 C28 -2.6(4) . . . . ? N3 Ru1 P1 C28 -150(2) . . . . ? N4 Ru1 P1 C28 -92.9(4) . . . . ? Cl1 Ru1 P1 C28 178.3(3) . . . . ? C1 Ru1 P1 C34 -36.6(4) . . . . ? N6 Ru1 P1 C34 -125.9(4) . . . . ? N3 Ru1 P1 C34 86(2) . . . . ? N4 Ru1 P1 C34 143.9(4) . . . . ? Cl1 Ru1 P1 C34 55.0(3) . . . . ? C2 N2 C1 N1 -3.5(9) . . . . ? C16 N2 C1 N1 170.9(8) . . . . ? C2 N2 C1 Ru1 -174.7(9) . . . . ? C16 N2 C1 Ru1 -0.3(16) . . . . ? C3 N1 C1 N2 3.7(9) . . . . ? C4 N1 C1 N2 -171.8(7) . . . . ? C3 N1 C1 Ru1 178.2(6) . . . . ? C4 N1 C1 Ru1 2.8(9) . . . . ? N6 Ru1 C1 N2 71.9(11) . . . . ? N3 Ru1 C1 N2 165.7(11) . . . . ? N4 Ru1 C1 N2 160.3(8) . . . . ? P1 Ru1 C1 N2 -18.7(11) . . . . ? Cl1 Ru1 C1 N2 -112.0(11) . . . . ? N6 Ru1 C1 N1 -98.7(6) . . . . ? N3 Ru1 C1 N1 -4.9(5) . . . . ? N4 Ru1 C1 N1 -10.3(11) . . . . ? P1 Ru1 C1 N1 170.7(5) . . . . ? Cl1 Ru1 C1 N1 77.4(6) . . . . ? C1 N2 C2 C3 2.1(11) . . . . ? C16 N2 C2 C3 -172.5(8) . . . . ? N2 C2 C3 N1 0.3(11) . . . . ? C4 N1 C3 C2 172.1(9) . . . . ? C1 N1 C3 C2 -2.6(11) . . . . ? C8 N3 C4 N1 -178.6(7) . . . . ? Ru1 N3 C4 N1 -7.5(10) . . . . ? C8 N3 C4 C5 3.6(13) . . . . ? Ru1 N3 C4 C5 174.6(7) . . . . ? C3 N1 C4 N3 -171.5(8) . . . . ? C1 N1 C4 N3 2.9(11) . . . . ? C3 N1 C4 C5 6.2(15) . . . . ? C1 N1 C4 C5 -179.4(9) . . . . ? N3 C4 C5 C6 -0.8(14) . . . . ? N1 C4 C5 C6 -178.4(9) . . . . ? C4 C5 C6 C7 -1.0(16) . . . . ? C5 C6 C7 C8 0.2(16) . . . . ? C5 C6 C7 C14 -179.9(10) . . . . ? C4 N3 C8 C7 -4.5(13) . . . . ? Ru1 N3 C8 C7 -175.5(7) . . . . ? C4 N3 C8 C9 175.0(8) . . . . ? Ru1 N3 C8 C9 4.0(10) . . . . ? C6 C7 C8 N3 2.5(14) . . . . ? C14 C7 C8 N3 -177.3(8) . . . . ? C6 C7 C8 C9 -176.9(9) . . . . ? C14 C7 C8 C9 3.2(14) . . . . ? C13 N4 C9 C8 175.6(8) . . . . ? Ru1 N4 C9 C8 -2.3(10) . . . . ? C13 N4 C9 C10 -2.9(12) . . . . ? Ru1 N4 C9 C10 179.2(7) . . . . ? N3 C8 C9 N4 -0.8(12) . . . . ? C7 C8 C9 N4 178.7(8) . . . . ? N3 C8 C9 C10 177.8(7) . . . . ? C7 C8 C9 C10 -2.7(13) . . . . ? N4 C9 C10 C11 0.7(13) . . . . ? C8 C9 C10 C11 -177.9(8) . . . . ? N4 C9 C10 C15 179.8(8) . . . . ? C8 C9 C10 C15 1.2(12) . . . . ? C9 C10 C11 C12 1.4(14) . . . . ? C15 C10 C11 C12 -177.6(10) . . . . ? C10 C11 C12 C13 -1.1(15) . . . . ? C9 N4 C13 C12 3.3(13) . . . . ? Ru1 N4 C13 C12 -179.5(7) . . . . ? C11 C12 C13 N4 -1.3(15) . . . . ? C8 C7 C14 C15 -2.3(15) . . . . ? C6 C7 C14 C15 177.9(11) . . . . ? C7 C14 C15 C10 1.0(17) . . . . ? C11 C10 C15 C14 178.5(10) . . . . ? C9 C10 C15 C14 -0.4(15) . . . . ? C1 N2 C16 C17 -102.9(10) . . . . ? C2 N2 C16 C17 71.0(11) . . . . ? C21 N5 C17 C18 -0.6(16) . . . . ? C21 N5 C17 C16 -178.4(10) . . . . ? N2 C16 C17 N5 -169.1(9) . . . . ? N2 C16 C17 C18 13.1(14) . . . . ? N5 C17 C18 C19 0.5(17) . . . . ? C16 C17 C18 C19 178.1(10) . . . . ? C17 C18 C19 C20 0.0(18) . . . . ? C18 C19 C20 C21 -0.2(19) . . . . ? C17 N5 C21 C20 0.4(19) . . . . ? C19 C20 C21 N5 0(2) . . . . ? C28 P1 C22 C23 -25.2(10) . . . . ? C34 P1 C22 C23 82.0(10) . . . . ? Ru1 P1 C22 C23 -149.4(9) . . . . ? C28 P1 C22 C27 163.1(8) . . . . ? C34 P1 C22 C27 -89.7(8) . . . . ? Ru1 P1 C22 C27 39.0(9) . . . . ? C27 C22 C23 C24 -1.3(18) . . . . ? P1 C22 C23 C24 -173.2(10) . . . . ? C22 C23 C24 C25 1(2) . . . . ? C23 C24 C25 C26 -1(2) . . . . ? C24 C25 C26 C27 0(2) . . . . ? C25 C26 C27 C22 -0.9(18) . . . . ? C23 C22 C27 C26 1.3(16) . . . . ? P1 C22 C27 C26 173.5(8) . . . . ? C22 P1 C28 C33 133.7(8) . . . . ? C34 P1 C28 C33 31.9(9) . . . . ? Ru1 P1 C28 C33 -99.3(8) . . . . ? C22 P1 C28 C29 -54.8(9) . . . . ? C34 P1 C28 C29 -156.7(8) . . . . ? Ru1 P1 C28 C29 72.2(8) . . . . ? C33 C28 C29 C30 -1.1(15) . . . . ? P1 C28 C29 C30 -173.0(9) . . . . ? C28 C29 C30 C31 0.7(18) . . . . ? C29 C30 C31 C32 0.6(18) . . . . ? C30 C31 C32 C33 -1.3(18) . . . . ? C29 C28 C33 C32 0.3(15) . . . . ? P1 C28 C33 C32 171.7(8) . . . . ? C31 C32 C33 C28 0.9(17) . . . . ? C22 P1 C34 C39 -59.4(9) . . . . ? C28 P1 C34 C39 46.8(10) . . . . ? Ru1 P1 C34 C39 173.7(8) . . . . ? C22 P1 C34 C35 115.5(8) . . . . ? C28 P1 C34 C35 -138.3(8) . . . . ? Ru1 P1 C34 C35 -11.4(9) . . . . ? C39 C34 C35 C36 -0.5(15) . . . . ? P1 C34 C35 C36 -175.6(8) . . . . ? C34 C35 C36 C37 -0.5(17) . . . . ? C35 C36 C37 C38 1.3(19) . . . . ? C36 C37 C38 C39 -1(2) . . . . ? C35 C34 C39 C38 0.8(17) . . . . ? P1 C34 C39 C38 175.8(10) . . . . ? C37 C38 C39 C34 0(2) . . . . ? Ru1 N6 C40 C41 -155(51) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.303 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.124 #===END data_090610c _database_code_depnum_ccdc_archive 'CCDC 832968' #TrackingRef '- Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H18 Cl F6 N6 O2 P Ru' _chemical_formula_weight 715.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 22.247(2) _cell_length_b 7.5266(9) _cell_length_c 33.040(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5532.5(10) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6859 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 20.2 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7408 _exptl_absorpt_correction_T_max 0.9174 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21198 _diffrn_reflns_av_R_equivalents 0.1074 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4875 _reflns_number_gt 3343 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0316P)^2^+53.6705P] 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 4875 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1279 _refine_ls_R_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.2050 _refine_ls_wR_factor_gt 0.1862 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.192 _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 0.62903(3) 0.20885(12) 0.09351(2) 0.0417(3) Uani 1 1 d . . . Cl1 Cl 0.65492(11) -0.0723(4) 0.06190(8) 0.0529(7) Uani 1 1 d . . . P1 P 0.41348(14) 0.4264(5) 0.17422(9) 0.0566(8) Uani 1 1 d . . . F1 F 0.3540(3) 0.4382(12) 0.2004(2) 0.091(3) Uani 1 1 d . A . F2 F 0.4732(4) 0.4137(12) 0.1483(2) 0.099(3) Uani 1 1 d . A . F3 F 0.3818(9) 0.309(5) 0.1416(8) 0.096(12) Uani 0.60(6) 1 d P A 1 F4 F 0.3969(13) 0.598(4) 0.1469(8) 0.099(9) Uani 0.60(6) 1 d P A 1 F5 F 0.4491(11) 0.560(4) 0.2034(8) 0.091(9) Uani 0.60(6) 1 d P A 1 F6 F 0.4373(9) 0.263(4) 0.1985(11) 0.095(11) Uani 0.60(6) 1 d P A 1 F3' F 0.3964(13) 0.230(4) 0.1641(16) 0.089(14) Uani 0.40(6) 1 d P A 2 F4' F 0.4435(13) 0.359(8) 0.2157(9) 0.086(13) Uani 0.40(6) 1 d P A 2 F5' F 0.424(2) 0.615(5) 0.1858(15) 0.104(15) Uani 0.40(6) 1 d P A 2 F6' F 0.375(2) 0.501(8) 0.1392(11) 0.108(17) Uani 0.40(6) 1 d P A 2 N1 N 0.5204(4) 0.0379(11) 0.1206(3) 0.047(2) Uani 1 1 d . . . N2 N 0.5807(4) -0.0077(12) 0.1699(3) 0.049(2) Uani 1 1 d . . . N3 N 0.5482(3) 0.1862(11) 0.0651(2) 0.0396(19) Uani 1 1 d . . . N4 N 0.6466(3) 0.3362(11) 0.0350(2) 0.043(2) Uani 1 1 d . . . N5 N 0.6962(5) 0.2322(15) 0.2234(3) 0.072(3) Uani 1 1 d . . . N6 N 0.3109(10) 0.940(4) 0.0862(7) 0.185(10) Uani 1 1 d . . . O1 O 0.7529(4) 0.1962(14) 0.1331(2) 0.083(3) Uani 1 1 d . . . O2 O 0.6017(4) 0.5605(13) 0.1315(3) 0.073(2) Uani 1 1 d . . . C1 C 0.5781(4) 0.0732(14) 0.1347(3) 0.047(3) Uani 1 1 d . . . C2 C 0.4892(5) -0.0644(16) 0.1491(4) 0.059(3) Uani 1 1 d . . . H2 H 0.4499 -0.1051 0.1469 0.071 Uiso 1 1 calc R . . C3 C 0.5264(5) -0.0920(16) 0.1795(4) 0.061(3) Uani 1 1 d . . . H3 H 0.5181 -0.1556 0.2029 0.073 Uiso 1 1 calc R . . C4 C 0.5036(4) 0.1014(14) 0.0825(3) 0.044(3) Uani 1 1 d . . . C5 C 0.4469(5) 0.0844(14) 0.0634(3) 0.050(3) Uani 1 1 d . . . H5 H 0.4147 0.0301 0.0764 0.060 Uiso 1 1 calc R . . C6 C 0.4413(5) 0.1505(13) 0.0252(3) 0.049(3) Uani 1 1 d . . . H6 H 0.4044 0.1406 0.0120 0.058 Uiso 1 1 calc R . . C7 C 0.4898(4) 0.2338(13) 0.0048(3) 0.042(2) Uani 1 1 d . . . C8 C 0.5433(4) 0.2490(12) 0.0265(3) 0.040(2) Uani 1 1 d . . . C9 C 0.5959(4) 0.3282(13) 0.0104(3) 0.041(2) Uani 1 1 d . . . C10 C 0.5945(5) 0.3934(15) -0.0292(3) 0.049(3) Uani 1 1 d . . . C11 C 0.6476(5) 0.4738(16) -0.0434(3) 0.056(3) Uani 1 1 d . . . H11 H 0.6488 0.5213 -0.0693 0.067 Uiso 1 1 calc R . . C12 C 0.6970(5) 0.4825(16) -0.0194(3) 0.061(3) Uani 1 1 d . . . H12 H 0.7320 0.5353 -0.0289 0.074 Uiso 1 1 calc R . . C13 C 0.6951(5) 0.4115(15) 0.0199(3) 0.052(3) Uani 1 1 d . . . H13 H 0.7294 0.4180 0.0359 0.063 Uiso 1 1 calc R . . C14 C 0.4895(5) 0.3011(15) -0.0356(3) 0.051(3) Uani 1 1 d . . . H14 H 0.4548 0.2932 -0.0512 0.061 Uiso 1 1 calc R . . C15 C 0.5390(5) 0.3756(14) -0.0510(3) 0.050(3) Uani 1 1 d . . . H15 H 0.5373 0.4184 -0.0773 0.060 Uiso 1 1 calc R . . C16 C 0.6326(5) 0.0066(15) 0.1975(3) 0.057(3) Uani 1 1 d . . . H16A H 0.6279 -0.0790 0.2193 0.068 Uiso 1 1 calc R . . H16B H 0.6689 -0.0237 0.1828 0.068 Uiso 1 1 calc R . . C17 C 0.6396(5) 0.1836(15) 0.2150(3) 0.053(3) Uani 1 1 d . . . C18 C 0.5930(5) 0.2995(17) 0.2221(3) 0.063(3) Uani 1 1 d . . . H18 H 0.5541 0.2643 0.2156 0.075 Uiso 1 1 calc R . . C19 C 0.6017(7) 0.4640(19) 0.2382(4) 0.076(4) Uani 1 1 d . . . H19 H 0.5699 0.5417 0.2426 0.091 Uiso 1 1 calc R . . C20 C 0.6591(7) 0.5088(19) 0.2475(4) 0.084(4) Uani 1 1 d . . . H20 H 0.6671 0.6186 0.2592 0.101 Uiso 1 1 calc R . . C21 C 0.7040(7) 0.397(2) 0.2400(4) 0.081(4) Uani 1 1 d . . . H21 H 0.7429 0.4334 0.2463 0.097 Uiso 1 1 calc R . . C22 C 0.7063(5) 0.2062(16) 0.1193(3) 0.053(3) Uani 1 1 d . . . C23 C 0.6110(5) 0.4254(17) 0.1179(3) 0.047(3) Uani 1 1 d . . . C24 C 0.2976(12) 0.891(5) 0.1155(9) 0.165(11) Uani 1 1 d . . . C25 C 0.2783(11) 0.829(4) 0.1554(7) 0.193(11) Uani 1 1 d . . . H25A H 0.2504 0.7329 0.1523 0.290 Uiso 1 1 calc R . . H25B H 0.2592 0.9250 0.1697 0.290 Uiso 1 1 calc R . . H25C H 0.3127 0.7893 0.1705 0.290 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0339(4) 0.0556(5) 0.0358(4) -0.0001(4) -0.0009(4) -0.0034(4) Cl1 0.0395(13) 0.0633(18) 0.0559(16) -0.0115(14) -0.0021(12) 0.0057(13) P1 0.0619(19) 0.061(2) 0.0465(16) -0.0010(16) 0.0065(14) -0.0005(16) F1 0.071(5) 0.129(7) 0.074(5) 0.000(5) 0.022(4) 0.006(5) F2 0.086(5) 0.118(7) 0.092(6) 0.003(5) 0.032(5) 0.006(5) F3 0.105(12) 0.10(3) 0.081(14) -0.023(15) -0.011(10) -0.023(13) F4 0.089(16) 0.11(2) 0.100(17) 0.027(14) 0.006(12) 0.004(12) F5 0.091(13) 0.10(2) 0.082(14) -0.027(12) -0.011(10) -0.010(11) F6 0.100(13) 0.078(17) 0.11(2) 0.036(15) 0.012(14) 0.019(12) F3' 0.094(19) 0.069(17) 0.10(3) 0.008(17) 0.008(18) 0.010(13) F4' 0.080(15) 0.11(4) 0.068(16) 0.005(17) -0.006(12) 0.010(17) F5' 0.11(3) 0.10(2) 0.11(3) 0.01(2) 0.01(2) -0.010(18) F6' 0.11(3) 0.13(5) 0.079(17) 0.02(2) -0.007(17) 0.02(3) N1 0.047(5) 0.047(6) 0.047(5) 0.000(4) 0.011(4) -0.005(4) N2 0.056(6) 0.045(5) 0.047(5) 0.001(4) 0.004(4) 0.003(4) N3 0.034(4) 0.041(5) 0.044(5) -0.006(4) 0.003(3) 0.005(4) N4 0.043(5) 0.048(6) 0.037(4) -0.001(4) 0.003(4) 0.000(4) N5 0.068(7) 0.073(8) 0.077(7) -0.005(6) 0.005(6) 0.001(6) N6 0.135(17) 0.26(3) 0.16(2) 0.02(2) -0.005(16) -0.037(16) O1 0.050(5) 0.126(8) 0.073(5) 0.012(6) -0.017(5) -0.008(5) O2 0.083(6) 0.069(6) 0.069(6) 0.000(5) 0.014(5) -0.008(5) C1 0.044(6) 0.049(7) 0.050(6) -0.004(5) 0.011(5) 0.000(5) C2 0.054(7) 0.056(8) 0.067(8) -0.004(6) 0.017(6) -0.007(6) C3 0.064(8) 0.054(8) 0.063(8) 0.002(6) 0.018(6) -0.005(6) C4 0.041(6) 0.041(6) 0.050(6) -0.013(5) 0.007(5) -0.002(5) C5 0.043(6) 0.045(6) 0.061(7) -0.015(6) 0.002(5) -0.003(5) C6 0.040(6) 0.044(6) 0.062(7) -0.017(5) -0.009(5) 0.004(5) C7 0.043(5) 0.032(6) 0.051(6) -0.016(5) -0.003(5) 0.009(4) C8 0.043(5) 0.035(6) 0.042(5) -0.007(4) 0.002(4) 0.005(4) C9 0.044(6) 0.042(6) 0.038(5) -0.007(4) -0.004(4) 0.004(5) C10 0.057(7) 0.051(7) 0.040(6) -0.004(5) 0.001(5) 0.004(6) C11 0.064(7) 0.061(8) 0.043(6) 0.002(6) 0.008(6) 0.004(6) C12 0.062(7) 0.071(8) 0.051(7) 0.008(6) 0.013(6) -0.008(6) C13 0.050(6) 0.063(8) 0.044(6) 0.003(6) 0.006(5) -0.011(6) C14 0.053(6) 0.045(7) 0.055(6) -0.011(6) -0.017(5) 0.013(6) C15 0.062(7) 0.049(7) 0.040(6) -0.002(5) -0.008(5) 0.010(6) C16 0.065(7) 0.051(7) 0.053(6) 0.005(6) 0.007(6) 0.005(6) C17 0.063(7) 0.045(7) 0.051(6) -0.002(5) 0.006(5) 0.017(6) C18 0.059(7) 0.063(8) 0.066(7) -0.003(7) 0.003(6) 0.006(7) C19 0.085(10) 0.072(10) 0.072(9) -0.007(8) 0.005(8) 0.015(8) C20 0.097(11) 0.062(9) 0.093(11) -0.018(8) -0.003(9) 0.004(9) C21 0.077(9) 0.078(11) 0.087(10) -0.008(9) 0.007(8) -0.004(8) C22 0.053(6) 0.061(7) 0.046(6) 0.001(6) 0.005(5) -0.006(6) C23 0.046(6) 0.053(7) 0.043(6) -0.001(6) 0.004(5) -0.008(5) C24 0.13(2) 0.23(3) 0.13(2) 0.05(2) 0.012(18) 0.006(19) C25 0.17(2) 0.25(3) 0.16(2) 0.03(2) 0.018(19) 0.03(2) _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 C23 1.862(13) . ? Ru1 C22 1.918(11) . ? Ru1 N3 2.035(7) . ? Ru1 C1 2.042(10) . ? Ru1 N4 2.193(8) . ? Ru1 Cl1 2.429(3) . ? P1 F5' 1.49(3) . ? P1 F6' 1.54(4) . ? P1 F3 1.559(15) . ? P1 F3' 1.56(2) . ? P1 F6 1.561(17) . ? P1 F2 1.583(8) . ? P1 F1 1.584(7) . ? P1 F5 1.605(18) . ? P1 F4' 1.61(3) . ? P1 F4 1.62(2) . ? N1 C1 1.392(13) . ? N1 C4 1.398(13) . ? N1 C2 1.399(13) . ? N2 C1 1.315(13) . ? N2 C3 1.401(13) . ? N2 C16 1.476(13) . ? N3 C4 1.313(12) . ? N3 C8 1.365(12) . ? N4 C13 1.315(12) . ? N4 C9 1.394(12) . ? N5 C17 1.342(14) . ? N5 C21 1.368(16) . ? N6 C24 1.08(3) . ? O1 C22 1.137(12) . ? O2 C23 1.130(12) . ? C2 C3 1.318(16) . ? C4 C5 1.416(14) . ? C5 C6 1.363(15) . ? C6 C7 1.418(14) . ? C7 C8 1.396(13) . ? C7 C14 1.426(14) . ? C8 C9 1.416(13) . ? C9 C10 1.398(13) . ? C10 C11 1.406(15) . ? C10 C15 1.435(14) . ? C11 C12 1.357(15) . ? C12 C13 1.405(14) . ? C14 C15 1.336(14) . ? C16 C17 1.461(15) . ? C17 C18 1.374(15) . ? C18 C19 1.361(17) . ? C19 C20 1.356(18) . ? C20 C21 1.329(18) . ? C24 C25 1.46(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 C23 Ru1 C22 90.5(5) . . ? C23 Ru1 N3 94.7(4) . . ? C22 Ru1 N3 174.5(4) . . ? C23 Ru1 C1 91.7(4) . . ? C22 Ru1 C1 101.3(4) . . ? N3 Ru1 C1 77.0(4) . . ? C23 Ru1 N4 92.1(4) . . ? C22 Ru1 N4 103.6(4) . . ? N3 Ru1 N4 77.8(3) . . ? C1 Ru1 N4 154.7(4) . . ? C23 Ru1 Cl1 178.7(3) . . ? C22 Ru1 Cl1 88.2(4) . . ? N3 Ru1 Cl1 86.5(2) . . ? C1 Ru1 Cl1 89.0(3) . . ? N4 Ru1 Cl1 87.7(2) . . ? F5' P1 F6' 86.0(18) . . ? F5' P1 F3 141.9(18) . . ? F6' P1 F3 55.9(15) . . ? F5' P1 F3' 174.5(19) . . ? F6' P1 F3' 92.9(17) . . ? F3 P1 F3' 37.6(10) . . ? F5' P1 F6 124.5(17) . . ? F6' P1 F6 149.4(18) . . ? F3 P1 F6 93.6(11) . . ? F3' P1 F6 56.4(12) . . ? F5' P1 F2 93.7(14) . . ? F6' P1 F2 94.7(16) . . ? F3 P1 F2 88.4(7) . . ? F3' P1 F2 91.8(10) . . ? F6 P1 F2 86.9(9) . . ? F5' P1 F1 86.4(14) . . ? F6' P1 F1 85.8(16) . . ? F3 P1 F1 91.8(7) . . ? F3' P1 F1 88.1(10) . . ? F6 P1 F1 92.7(9) . . ? F2 P1 F1 179.5(5) . . ? F5' P1 F5 33.8(15) . . ? F6' P1 F5 119.5(18) . . ? F3 P1 F5 173.2(11) . . ? F3' P1 F5 147.5(14) . . ? F6 P1 F5 91.1(10) . . ? F2 P1 F5 87.0(8) . . ? F1 P1 F5 92.8(8) . . ? F5' P1 F4' 91.0(16) . . ? F6' P1 F4' 170(2) . . ? F3 P1 F4' 126.7(15) . . ? F3' P1 F4' 89.2(14) . . ? F6 P1 F4' 34.1(10) . . ? F2 P1 F4' 95.3(12) . . ? F1 P1 F4' 84.2(11) . . ? F5 P1 F4' 58.7(13) . . ? F5' P1 F4 54.5(17) . . ? F6' P1 F4 33.3(15) . . ? F3 P1 F4 87.8(11) . . ? F3' P1 F4 125.4(15) . . ? F6 P1 F4 173.1(12) . . ? F2 P1 F4 86.4(9) . . ? F1 P1 F4 94.0(9) . . ? F5 P1 F4 87.0(11) . . ? F4' P1 F4 145.4(16) . . ? C1 N1 C4 118.8(8) . . ? C1 N1 C2 109.9(9) . . ? C4 N1 C2 131.4(9) . . ? C1 N2 C3 111.8(9) . . ? C1 N2 C16 123.2(9) . . ? C3 N2 C16 124.6(9) . . ? C4 N3 C8 121.2(8) . . ? C4 N3 Ru1 120.5(7) . . ? C8 N3 Ru1 118.1(6) . . ? C13 N4 C9 117.5(8) . . ? C13 N4 Ru1 131.9(7) . . ? C9 N4 Ru1 110.6(6) . . ? C17 N5 C21 116.7(11) . . ? N2 C1 N1 104.3(9) . . ? N2 C1 Ru1 142.8(8) . . ? N1 C1 Ru1 112.7(7) . . ? C3 C2 N1 106.7(10) . . ? C2 C3 N2 107.4(10) . . ? N3 C4 N1 111.0(8) . . ? N3 C4 C5 121.4(10) . . ? N1 C4 C5 127.6(9) . . ? C6 C5 C4 117.6(10) . . ? C5 C6 C7 122.1(10) . . ? C8 C7 C6 116.2(9) . . ? C8 C7 C14 117.1(9) . . ? C6 C7 C14 126.7(10) . . ? N3 C8 C7 121.3(9) . . ? N3 C8 C9 115.6(8) . . ? C7 C8 C9 123.0(9) . . ? N4 C9 C10 123.3(9) . . ? N4 C9 C8 117.8(8) . . ? C10 C9 C8 118.9(9) . . ? C9 C10 C11 116.3(10) . . ? C9 C10 C15 117.0(10) . . ? C11 C10 C15 126.7(10) . . ? C12 C11 C10 120.5(10) . . ? C11 C12 C13 119.8(11) . . ? N4 C13 C12 122.6(10) . . ? C15 C14 C7 120.1(10) . . ? C14 C15 C10 124.0(10) . . ? C17 C16 N2 113.2(9) . . ? N5 C17 C18 120.0(11) . . ? N5 C17 C16 115.5(10) . . ? C18 C17 C16 124.5(11) . . ? C19 C18 C17 122.4(12) . . ? C20 C19 C18 116.7(13) . . ? C21 C20 C19 120.6(14) . . ? C20 C21 N5 123.5(14) . . ? O1 C22 Ru1 175.9(11) . . ? O2 C23 Ru1 176.9(10) . . ? N6 C24 C25 178(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C23 Ru1 N3 C4 -92.1(8) . . . . ? C22 Ru1 N3 C4 71(4) . . . . ? C1 Ru1 N3 C4 -1.4(7) . . . . ? N4 Ru1 N3 C4 176.7(8) . . . . ? Cl1 Ru1 N3 C4 88.3(7) . . . . ? C23 Ru1 N3 C8 93.0(7) . . . . ? C22 Ru1 N3 C8 -104(4) . . . . ? C1 Ru1 N3 C8 -176.3(8) . . . . ? N4 Ru1 N3 C8 1.8(7) . . . . ? Cl1 Ru1 N3 C8 -86.5(7) . . . . ? C23 Ru1 N4 C13 85.2(10) . . . . ? C22 Ru1 N4 C13 -5.9(10) . . . . ? N3 Ru1 N4 C13 179.6(10) . . . . ? C1 Ru1 N4 C13 -176.2(10) . . . . ? Cl1 Ru1 N4 C13 -93.5(9) . . . . ? C23 Ru1 N4 C9 -96.3(7) . . . . ? C22 Ru1 N4 C9 172.6(7) . . . . ? N3 Ru1 N4 C9 -2.0(6) . . . . ? C1 Ru1 N4 C9 2.3(12) . . . . ? Cl1 Ru1 N4 C9 84.9(6) . . . . ? C3 N2 C1 N1 -0.9(12) . . . . ? C16 N2 C1 N1 -174.6(9) . . . . ? C3 N2 C1 Ru1 -174.2(10) . . . . ? C16 N2 C1 Ru1 12.0(19) . . . . ? C4 N1 C1 N2 -177.9(8) . . . . ? C2 N1 C1 N2 0.7(11) . . . . ? C4 N1 C1 Ru1 -2.2(11) . . . . ? C2 N1 C1 Ru1 176.3(7) . . . . ? C23 Ru1 C1 N2 -90.7(13) . . . . ? C22 Ru1 C1 N2 0.2(14) . . . . ? N3 Ru1 C1 N2 174.8(14) . . . . ? N4 Ru1 C1 N2 170.6(10) . . . . ? Cl1 Ru1 C1 N2 88.2(13) . . . . ? C23 Ru1 C1 N1 96.3(8) . . . . ? C22 Ru1 C1 N1 -172.8(7) . . . . ? N3 Ru1 C1 N1 1.8(7) . . . . ? N4 Ru1 C1 N1 -2.4(14) . . . . ? Cl1 Ru1 C1 N1 -84.8(7) . . . . ? C1 N1 C2 C3 -0.2(13) . . . . ? C4 N1 C2 C3 178.1(10) . . . . ? N1 C2 C3 N2 -0.3(13) . . . . ? C1 N2 C3 C2 0.8(13) . . . . ? C16 N2 C3 C2 174.4(10) . . . . ? C8 N3 C4 N1 175.4(8) . . . . ? Ru1 N3 C4 N1 0.7(11) . . . . ? C8 N3 C4 C5 -5.4(14) . . . . ? Ru1 N3 C4 C5 179.9(7) . . . . ? C1 N1 C4 N3 1.1(13) . . . . ? C2 N1 C4 N3 -177.1(10) . . . . ? C1 N1 C4 C5 -178.1(10) . . . . ? C2 N1 C4 C5 3.8(17) . . . . ? N3 C4 C5 C6 3.7(15) . . . . ? N1 C4 C5 C6 -177.2(9) . . . . ? C4 C5 C6 C7 0.0(15) . . . . ? C5 C6 C7 C8 -1.8(14) . . . . ? C5 C6 C7 C14 177.4(10) . . . . ? C4 N3 C8 C7 3.5(14) . . . . ? Ru1 N3 C8 C7 178.3(7) . . . . ? C4 N3 C8 C9 -176.2(9) . . . . ? Ru1 N3 C8 C9 -1.4(11) . . . . ? C6 C7 C8 N3 0.1(13) . . . . ? C14 C7 C8 N3 -179.1(8) . . . . ? C6 C7 C8 C9 179.8(9) . . . . ? C14 C7 C8 C9 0.5(14) . . . . ? C13 N4 C9 C10 0.9(15) . . . . ? Ru1 N4 C9 C10 -177.8(8) . . . . ? C13 N4 C9 C8 -179.4(9) . . . . ? Ru1 N4 C9 C8 1.9(10) . . . . ? N3 C8 C9 N4 -0.5(13) . . . . ? C7 C8 C9 N4 179.8(8) . . . . ? N3 C8 C9 C10 179.2(9) . . . . ? C7 C8 C9 C10 -0.5(14) . . . . ? N4 C9 C10 C11 -1.5(15) . . . . ? C8 C9 C10 C11 178.8(9) . . . . ? N4 C9 C10 C15 179.9(9) . . . . ? C8 C9 C10 C15 0.2(14) . . . . ? C9 C10 C11 C12 1.2(16) . . . . ? C15 C10 C11 C12 179.6(11) . . . . ? C10 C11 C12 C13 -0.3(18) . . . . ? C9 N4 C13 C12 0.0(16) . . . . ? Ru1 N4 C13 C12 178.4(8) . . . . ? C11 C12 C13 N4 -0.3(18) . . . . ? C8 C7 C14 C15 -0.3(14) . . . . ? C6 C7 C14 C15 -179.5(10) . . . . ? C7 C14 C15 C10 0.1(17) . . . . ? C9 C10 C15 C14 0.0(16) . . . . ? C11 C10 C15 C14 -178.5(11) . . . . ? C1 N2 C16 C17 68.3(13) . . . . ? C3 N2 C16 C17 -104.6(12) . . . . ? C21 N5 C17 C18 1.8(17) . . . . ? C21 N5 C17 C16 -179.8(11) . . . . ? N2 C16 C17 N5 -149.3(10) . . . . ? N2 C16 C17 C18 29.1(15) . . . . ? N5 C17 C18 C19 -1.2(19) . . . . ? C16 C17 C18 C19 -179.5(11) . . . . ? C17 C18 C19 C20 -1(2) . . . . ? C18 C19 C20 C21 2(2) . . . . ? C19 C20 C21 N5 -1(2) . . . . ? C17 N5 C21 C20 -1(2) . . . . ? C23 Ru1 C22 O1 -171(15) . . . . ? N3 Ru1 C22 O1 26(18) . . . . ? C1 Ru1 C22 O1 97(15) . . . . ? N4 Ru1 C22 O1 -79(15) . . . . ? Cl1 Ru1 C22 O1 8(15) . . . . ? C22 Ru1 C23 O2 77(21) . . . . ? N3 Ru1 C23 O2 -105(21) . . . . ? C1 Ru1 C23 O2 178(100) . . . . ? N4 Ru1 C23 O2 -27(21) . . . . ? Cl1 Ru1 C23 O2 56(31) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.264 _refine_diff_density_min -1.141 _refine_diff_density_rms 0.121 #===END data_100113_gsjr1286 _database_code_depnum_ccdc_archive 'CCDC 832969' #TrackingRef '- Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H33 Cl F6 N6 O P2 Ru' _chemical_formula_weight 950.20 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' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4399(3) _cell_length_b 13.3041(3) _cell_length_c 29.3523(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.634(3) _cell_angle_gamma 90.00 _cell_volume 4030.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4584 _cell_measurement_theta_min 3.0914 _cell_measurement_theta_max 28.7464 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7938 _exptl_absorpt_correction_T_max 0.9200 _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 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15113 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7095 _reflns_number_gt 4535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro(Oxford Diffraction Ltd.)' _computing_cell_refinement 'CrysAlisPro(Oxford Diffraction Ltd.)' _computing_data_reduction 'CrysAlisPro(Oxford Diffraction Ltd.)' _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^)+(0.1347P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7095 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1049 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.2179 _refine_ls_wR_factor_gt 0.1978 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 -0.05011(5) 0.05197(4) 0.826532(19) 0.0358(2) Uani 1 1 d . . . O1 O -0.0429(7) -0.0227(5) 0.9235(2) 0.0812(19) Uani 1 1 d . . . Cl2 Cl -0.29087(12) 0.02327(9) 0.81180(5) 0.0228(3) Uani 1 1 d . . . P1 P 0.17300(18) 0.06974(12) 0.83643(6) 0.0370(4) Uani 1 1 d . . . P3 P 0.5662(3) 0.14415(18) 0.57800(9) 0.0691(7) Uani 1 1 d . . . N1 N -0.0731(5) 0.1063(4) 0.76076(19) 0.0383(13) Uani 1 1 d . . . N3 N -0.0952(5) 0.2547(4) 0.7943(2) 0.0442(15) Uani 1 1 d . . . N4 N -0.0784(6) 0.2738(4) 0.8676(2) 0.0518(16) Uani 1 1 d . . . N6 N -0.2889(6) 0.2129(5) 0.9099(2) 0.0580(18) Uani 1 1 d . . . N30 N 0.0588(11) 0.0759(7) 0.5523(4) 0.106(3) Uani 1 1 d . . . F1 F 0.5362(8) 0.1570(7) 0.5248(2) 0.146(3) Uani 1 1 d . . . F2 F 0.7009(10) 0.1718(12) 0.5739(3) 0.235(7) Uani 1 1 d . . . F3 F 0.4311(10) 0.1159(16) 0.5835(4) 0.279(8) Uani 1 1 d . . . F4 F 0.5987(8) 0.1245(6) 0.6315(2) 0.132(3) Uani 1 1 d . . . F5 F 0.5891(16) 0.0369(6) 0.5711(4) 0.245(7) Uani 1 1 d . . . F6 F 0.540(3) 0.2457(8) 0.5878(4) 0.348(12) Uani 1 1 d . . . C1 C 0.2280(7) 0.0922(5) 0.7810(2) 0.0429(17) Uani 1 1 d . . . C2 C 0.2045(7) 0.1849(5) 0.7575(3) 0.0499(19) Uani 1 1 d . . . H2 H 0.1730 0.2392 0.7724 0.060 Uiso 1 1 calc R . . C3 C 0.2282(8) 0.1953(6) 0.7126(3) 0.059(2) Uani 1 1 d . . . H3 H 0.2120 0.2563 0.6973 0.071 Uiso 1 1 calc R . . C4 C 0.2781(8) 0.0147(6) 0.7580(3) 0.058(2) Uani 1 1 d . . . H4 H 0.2990 -0.0461 0.7729 0.070 Uiso 1 1 calc R . . C8 C 0.2354(7) 0.1678(5) 0.8780(2) 0.0441(17) Uani 1 1 d . . . C9 C 0.2595(9) 0.2655(5) 0.8675(3) 0.063(2) Uani 1 1 d . . . H9 H 0.2520 0.2861 0.8369 0.076 Uiso 1 1 calc R . . C10 C 0.2962(11) 0.3352(7) 0.9039(4) 0.091(3) Uani 1 1 d . . . H10 H 0.3139 0.4013 0.8966 0.109 Uiso 1 1 calc R . . C11 C 0.3063(10) 0.3082(7) 0.9488(4) 0.080(3) Uani 1 1 d . . . H11 H 0.3287 0.3555 0.9720 0.096 Uiso 1 1 calc R . . C12 C 0.2830(9) 0.2106(7) 0.9596(3) 0.073(3) Uani 1 1 d . . . H12 H 0.2911 0.1903 0.9902 0.088 Uiso 1 1 calc R . . C14 C -0.0751(7) 0.2020(5) 0.8353(2) 0.0418(17) Uani 1 1 d . . . C15 C -0.0698(6) 0.0423(5) 0.7260(2) 0.0374(16) Uani 1 1 d . . . C16 C -0.0538(6) -0.0598(5) 0.7384(2) 0.0396(16) Uani 1 1 d . . . C17 C -0.1717(9) 0.2048(6) 0.9344(3) 0.056(2) Uani 1 1 d . . . C18 C -0.1505(11) 0.1541(8) 0.9752(3) 0.082(3) Uani 1 1 d . . . H18 H -0.0676 0.1500 0.9920 0.099 Uiso 1 1 calc R . . C19 C -0.2560(15) 0.1082(8) 0.9916(4) 0.101(4) Uani 1 1 d . . . H19 H -0.2449 0.0738 1.0195 0.122 Uiso 1 1 calc R . . C20 C -0.3746(12) 0.1153(8) 0.9655(4) 0.090(3) Uani 1 1 d . . . H20 H -0.4462 0.0837 0.9745 0.108 Uiso 1 1 calc R . . C21 C -0.3860(10) 0.1694(7) 0.9263(4) 0.078(3) Uani 1 1 d . . . H21 H -0.4685 0.1767 0.9096 0.094 Uiso 1 1 calc R . . C23 C -0.0608(8) 0.2568(6) 0.9167(3) 0.065(2) Uani 1 1 d . . . H23A H -0.0465 0.3211 0.9322 0.077 Uiso 1 1 calc R . . H23B H 0.0168 0.2168 0.9251 0.077 Uiso 1 1 calc R . . C25 C -0.0862(7) 0.0742(6) 0.6804(3) 0.0502(19) Uani 1 1 d . . . C26 C -0.0828(8) 0.0004(7) 0.6458(3) 0.063(2) Uani 1 1 d . . . H26 H -0.0898 0.0199 0.6151 0.076 Uiso 1 1 calc R . . C29 C -0.1182(7) 0.2431(6) 0.7081(3) 0.054(2) Uani 1 1 d . . . H29 H -0.1373 0.3108 0.7027 0.065 Uiso 1 1 calc R . . C31 C -0.1117(8) 0.3581(5) 0.8019(4) 0.062(2) Uani 1 1 d . . . H31 H -0.1283 0.4082 0.7798 0.074 Uiso 1 1 calc R . . C32 C -0.0986(8) 0.3689(5) 0.8471(4) 0.067(3) Uani 1 1 d . . . H32 H -0.1023 0.4294 0.8627 0.081 Uiso 1 1 calc R . . C34 C -0.0447(7) 0.0058(5) 0.8872(3) 0.0471(18) Uani 1 1 d . . . C35 C -0.1094(7) 0.1790(6) 0.6730(3) 0.057(2) Uani 1 1 d . . . H35 H -0.1188 0.2040 0.6430 0.068 Uiso 1 1 calc R . . C37 C -0.0695(8) -0.0988(7) 0.6570(3) 0.060(2) Uani 1 1 d . . . H37 H -0.0668 -0.1457 0.6337 0.072 Uiso 1 1 calc R . . C38 C -0.0593(7) -0.1328(6) 0.7037(3) 0.053(2) Uani 1 1 d . . . C39 C -0.0607(8) -0.2341(6) 0.7169(3) 0.059(2) Uani 1 1 d . . . H39 H -0.0643 -0.2850 0.6950 0.071 Uiso 1 1 calc R . . C40 C -0.0568(7) -0.2562(6) 0.7616(3) 0.060(2) Uani 1 1 d . . . H40 H -0.0607 -0.3232 0.7704 0.072 Uiso 1 1 calc R . . C41 C -0.0472(7) -0.1814(5) 0.7955(3) 0.0459(18) Uani 1 1 d . . . H41 H -0.0424 -0.2000 0.8262 0.055 Uiso 1 1 calc R . . N42 N -0.0447(5) -0.0830(4) 0.78458(19) 0.0406(14) Uani 1 1 d . . . C43 C 0.2264(8) -0.1179(5) 0.8792(2) 0.0467(18) Uani 1 1 d . . . H43 H 0.1371 -0.1246 0.8776 0.056 Uiso 1 1 calc R . . C44 C 0.4083(7) -0.0257(5) 0.8620(3) 0.0508(19) Uani 1 1 d . . . H44 H 0.4428 0.0286 0.8480 0.061 Uiso 1 1 calc R . . C45 C 0.2775(7) -0.0350(5) 0.8603(2) 0.0400(17) Uani 1 1 d . . . C46 C 0.4897(8) -0.0987(6) 0.8850(3) 0.064(2) Uani 1 1 d . . . H46 H 0.5790 -0.0916 0.8873 0.077 Uiso 1 1 calc R . . C47 C 0.4384(9) -0.1812(6) 0.9044(3) 0.063(2) Uani 1 1 d . . . H47 H 0.4935 -0.2292 0.9198 0.075 Uiso 1 1 calc R . . C48 C 0.2469(8) 0.1419(6) 0.9242(3) 0.062(2) Uani 1 1 d . . . H48 H 0.2299 0.0759 0.9319 0.074 Uiso 1 1 calc R . . C49 C 0.2758(8) 0.1154(7) 0.6903(3) 0.063(2) Uani 1 1 d . . . H49 H 0.2926 0.1231 0.6603 0.076 Uiso 1 1 calc R . . C50 C 0.2977(9) 0.0275(8) 0.7116(3) 0.074(3) Uani 1 1 d . . . H50 H 0.3264 -0.0266 0.6958 0.088 Uiso 1 1 calc R . . C51 C 0.3097(8) -0.1926(5) 0.9010(3) 0.0493(19) Uani 1 1 d . . . H51 H 0.2755 -0.2495 0.9131 0.059 Uiso 1 1 calc R . . C52 C 0.1280(11) 0.0767(7) 0.5260(3) 0.070(3) Uani 1 1 d . . . C53 C 0.2169(12) 0.0737(9) 0.4923(4) 0.104(4) Uani 1 1 d . . . H53A H 0.2557 0.1387 0.4903 0.156 Uiso 1 1 calc R . . H53B H 0.1703 0.0556 0.4627 0.156 Uiso 1 1 calc R . . H53C H 0.2834 0.0248 0.5016 0.156 Uiso 1 1 calc R . . C600 C -0.0971(7) 0.2032(5) 0.7534(3) 0.0447(18) 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 0.0419(4) 0.0299(3) 0.0369(3) -0.0024(2) 0.0096(2) -0.0032(2) O1 0.122(6) 0.073(4) 0.055(4) 0.016(3) 0.034(4) 0.011(4) Cl2 0.0153(7) 0.0148(6) 0.0396(8) -0.0027(5) 0.0084(6) -0.0034(5) P1 0.0429(11) 0.0333(9) 0.0356(10) -0.0010(7) 0.0089(8) -0.0039(8) P3 0.0741(18) 0.0662(15) 0.0645(16) -0.0022(12) 0.0016(13) 0.0281(13) N1 0.041(3) 0.033(3) 0.042(3) 0.004(2) 0.009(3) -0.005(3) N3 0.041(3) 0.027(3) 0.067(4) -0.005(3) 0.016(3) -0.001(3) N4 0.050(4) 0.048(4) 0.062(4) -0.020(3) 0.022(3) -0.006(3) N6 0.051(4) 0.062(4) 0.057(4) 0.011(3) -0.003(3) 0.000(3) N30 0.129(9) 0.094(7) 0.102(8) -0.024(6) 0.046(7) -0.021(6) F1 0.160(7) 0.207(8) 0.067(4) 0.021(5) 0.000(4) 0.022(6) F2 0.132(8) 0.43(2) 0.133(8) 0.034(10) -0.005(6) -0.109(10) F3 0.104(7) 0.59(3) 0.134(9) 0.028(13) 0.001(6) -0.062(11) F4 0.154(7) 0.157(6) 0.075(5) 0.000(4) -0.015(4) -0.009(5) F5 0.51(2) 0.115(6) 0.147(9) 0.029(6) 0.171(11) 0.075(9) F6 0.77(4) 0.121(8) 0.185(12) 0.013(7) 0.184(17) 0.161(14) C1 0.040(4) 0.045(4) 0.043(4) 0.003(3) 0.007(3) -0.008(3) C2 0.055(5) 0.046(4) 0.050(5) 0.004(3) 0.012(4) -0.007(4) C3 0.068(6) 0.066(5) 0.046(5) 0.009(4) 0.015(4) -0.014(4) C4 0.078(6) 0.055(5) 0.046(5) 0.003(4) 0.026(4) 0.008(4) C8 0.040(4) 0.043(4) 0.048(4) -0.011(3) 0.003(3) -0.004(3) C9 0.089(7) 0.035(4) 0.062(6) -0.005(4) 0.001(5) -0.012(4) C10 0.123(9) 0.045(5) 0.103(9) -0.014(5) 0.010(7) -0.020(6) C11 0.101(8) 0.069(6) 0.068(7) -0.032(5) 0.008(6) -0.007(6) C12 0.080(7) 0.079(6) 0.057(6) -0.019(5) -0.003(5) -0.010(5) C14 0.040(4) 0.036(4) 0.051(5) -0.009(3) 0.010(3) -0.008(3) C15 0.032(4) 0.044(4) 0.036(4) -0.003(3) 0.005(3) -0.005(3) C16 0.030(4) 0.044(4) 0.044(4) -0.004(3) 0.002(3) -0.002(3) C17 0.068(6) 0.054(5) 0.044(5) -0.015(4) 0.006(4) 0.011(4) C18 0.094(8) 0.096(7) 0.053(6) -0.012(5) -0.005(5) 0.034(6) C19 0.168(13) 0.083(7) 0.057(7) 0.011(5) 0.027(8) 0.015(8) C20 0.105(9) 0.095(8) 0.075(8) 0.012(6) 0.028(7) -0.020(7) C21 0.066(6) 0.087(7) 0.083(7) 0.011(6) 0.017(5) -0.013(5) C23 0.053(5) 0.069(5) 0.070(6) -0.033(5) 0.004(4) 0.010(4) C25 0.041(4) 0.069(5) 0.040(4) 0.002(4) 0.005(3) -0.011(4) C26 0.064(6) 0.086(6) 0.039(5) -0.009(4) 0.008(4) -0.027(5) C29 0.046(5) 0.050(4) 0.067(6) 0.019(4) 0.007(4) -0.010(4) C31 0.058(5) 0.032(4) 0.098(7) 0.001(4) 0.020(5) 0.001(4) C32 0.066(6) 0.031(4) 0.108(8) -0.020(5) 0.023(5) 0.000(4) C34 0.054(5) 0.050(4) 0.039(4) -0.001(4) 0.015(4) -0.001(4) C35 0.044(5) 0.072(5) 0.052(5) 0.014(4) 0.001(4) -0.010(4) C37 0.059(5) 0.075(6) 0.050(5) -0.025(4) 0.017(4) -0.014(5) C38 0.040(4) 0.060(5) 0.060(5) -0.025(4) 0.013(4) -0.009(4) C39 0.055(5) 0.049(5) 0.075(6) -0.032(4) 0.016(4) -0.008(4) C40 0.046(5) 0.034(4) 0.098(7) -0.007(4) 0.006(5) 0.001(4) C41 0.041(4) 0.030(4) 0.064(5) 0.003(3) 0.000(4) -0.005(3) N42 0.040(3) 0.037(3) 0.046(4) -0.006(3) 0.008(3) -0.003(3) C43 0.053(5) 0.044(4) 0.043(4) -0.002(3) 0.005(4) -0.005(4) C44 0.051(5) 0.041(4) 0.061(5) 0.014(4) 0.013(4) 0.006(4) C45 0.043(4) 0.039(4) 0.038(4) 0.001(3) 0.004(3) -0.003(3) C46 0.046(5) 0.069(5) 0.078(6) -0.001(5) 0.013(4) 0.014(4) C47 0.075(7) 0.050(5) 0.063(6) 0.009(4) 0.014(5) 0.013(5) C48 0.070(6) 0.052(5) 0.058(5) -0.004(4) -0.004(4) -0.009(4) C49 0.067(6) 0.082(6) 0.043(5) 0.009(5) 0.017(4) -0.007(5) C50 0.078(7) 0.092(7) 0.055(6) -0.020(5) 0.020(5) 0.005(5) C51 0.062(5) 0.043(4) 0.044(4) 0.005(3) 0.013(4) 0.007(4) C52 0.090(8) 0.055(5) 0.062(6) 0.004(5) 0.000(5) -0.024(5) C53 0.132(10) 0.115(9) 0.069(7) 0.010(6) 0.030(7) -0.045(8) C600 0.030(4) 0.041(4) 0.064(5) 0.005(4) 0.011(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C34 1.875(7) . ? Ru1 C14 2.035(7) . ? Ru1 N1 2.041(5) . ? Ru1 N42 2.183(5) . ? Ru1 P1 2.3158(19) . ? Ru1 Cl2 2.5148(14) . ? O1 C34 1.131(8) . ? P1 C1 1.829(7) . ? P1 C8 1.838(7) . ? P1 C45 1.842(7) . ? P3 F6 1.415(9) . ? P3 F5 1.465(8) . ? P3 F2 1.475(9) . ? P3 F3 1.492(10) . ? P3 F1 1.555(7) . ? P3 F4 1.577(7) . ? N1 C600 1.326(8) . ? N1 C15 1.334(8) . ? N3 C14 1.380(9) . ? N3 C600 1.382(9) . ? N3 C31 1.408(9) . ? N4 C14 1.349(8) . ? N4 C32 1.404(10) . ? N4 C23 1.443(10) . ? N6 C21 1.319(11) . ? N6 C17 1.326(10) . ? N30 C52 1.134(12) . ? C1 C4 1.378(10) . ? C1 C2 1.415(9) . ? C2 C3 1.387(10) . ? C3 C49 1.378(12) . ? C4 C50 1.418(11) . ? C8 C9 1.368(10) . ? C8 C48 1.387(11) . ? C9 C10 1.423(12) . ? C10 C11 1.355(13) . ? C11 C12 1.368(13) . ? C12 C48 1.391(11) . ? C15 C25 1.390(10) . ? C15 C16 1.410(9) . ? C16 N42 1.378(9) . ? C16 C38 1.403(9) . ? C17 C18 1.366(12) . ? C17 C23 1.506(12) . ? C18 C19 1.406(15) . ? C19 C20 1.357(16) . ? C20 C21 1.348(13) . ? C25 C26 1.415(11) . ? C25 C35 1.426(11) . ? C26 C37 1.362(12) . ? C29 C35 1.352(11) . ? C29 C600 1.418(10) . ? C31 C32 1.319(12) . ? C37 C38 1.431(11) . ? C38 C39 1.404(11) . ? C39 C40 1.341(11) . ? C40 C41 1.400(11) . ? C41 N42 1.349(8) . ? C43 C45 1.377(9) . ? C43 C51 1.410(10) . ? C44 C45 1.365(10) . ? C44 C46 1.396(10) . ? C46 C47 1.381(11) . ? C47 C51 1.341(11) . ? C49 C50 1.330(12) . ? C52 C53 1.455(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C34 Ru1 C14 100.8(3) . . ? C34 Ru1 N1 174.7(3) . . ? C14 Ru1 N1 76.9(3) . . ? C34 Ru1 N42 105.5(3) . . ? C14 Ru1 N42 153.3(3) . . ? N1 Ru1 N42 76.5(2) . . ? C34 Ru1 P1 91.6(2) . . ? C14 Ru1 P1 91.7(2) . . ? N1 Ru1 P1 93.20(16) . . ? N42 Ru1 P1 92.53(15) . . ? C34 Ru1 Cl2 90.0(2) . . ? C14 Ru1 Cl2 91.54(19) . . ? N1 Ru1 Cl2 85.32(16) . . ? N42 Ru1 Cl2 83.56(15) . . ? P1 Ru1 Cl2 176.05(6) . . ? C1 P1 C8 110.3(3) . . ? C1 P1 C45 102.4(3) . . ? C8 P1 C45 98.9(3) . . ? C1 P1 Ru1 110.4(2) . . ? C8 P1 Ru1 113.9(2) . . ? C45 P1 Ru1 119.8(2) . . ? F6 P3 F5 175.6(7) . . ? F6 P3 F2 89.5(11) . . ? F5 P3 F2 93.2(9) . . ? F6 P3 F3 90.4(11) . . ? F5 P3 F3 86.9(10) . . ? F2 P3 F3 178.4(6) . . ? F6 P3 F1 94.8(6) . . ? F5 P3 F1 88.9(5) . . ? F2 P3 F1 86.7(5) . . ? F3 P3 F1 94.9(5) . . ? F6 P3 F4 88.5(6) . . ? F5 P3 F4 87.7(5) . . ? F2 P3 F4 93.3(5) . . ? F3 P3 F4 85.2(5) . . ? F1 P3 F4 176.7(5) . . ? C600 N1 C15 121.4(6) . . ? C600 N1 Ru1 119.5(5) . . ? C15 N1 Ru1 119.0(4) . . ? C14 N3 C600 119.2(6) . . ? C14 N3 C31 111.4(7) . . ? C600 N3 C31 129.5(7) . . ? C14 N4 C32 110.8(7) . . ? C14 N4 C23 125.3(7) . . ? C32 N4 C23 124.0(7) . . ? C21 N6 C17 117.7(8) . . ? C4 C1 C2 117.7(7) . . ? C4 C1 P1 120.4(5) . . ? C2 C1 P1 121.4(6) . . ? C3 C2 C1 120.5(7) . . ? C49 C3 C2 120.2(8) . . ? C1 C4 C50 120.0(8) . . ? C9 C8 C48 117.8(7) . . ? C9 C8 P1 125.7(6) . . ? C48 C8 P1 116.3(5) . . ? C8 C9 C10 119.1(8) . . ? C11 C10 C9 122.0(8) . . ? C10 C11 C12 119.1(8) . . ? C11 C12 C48 119.3(9) . . ? N4 C14 N3 103.7(6) . . ? N4 C14 Ru1 143.2(6) . . ? N3 C14 Ru1 113.2(5) . . ? N1 C15 C25 121.9(6) . . ? N1 C15 C16 115.5(6) . . ? C25 C15 C16 122.5(7) . . ? N42 C16 C38 123.3(6) . . ? N42 C16 C15 117.3(6) . . ? C38 C16 C15 119.1(7) . . ? N6 C17 C18 122.0(9) . . ? N6 C17 C23 118.1(8) . . ? C18 C17 C23 119.8(9) . . ? C17 C18 C19 118.9(10) . . ? C20 C19 C18 118.2(10) . . ? C21 C20 C19 118.4(11) . . ? N6 C21 C20 124.8(10) . . ? N4 C23 C17 115.3(6) . . ? C15 C25 C26 117.7(7) . . ? C15 C25 C35 116.0(7) . . ? C26 C25 C35 126.2(8) . . ? C37 C26 C25 120.8(8) . . ? C35 C29 C600 117.4(7) . . ? C32 C31 N3 105.6(7) . . ? C31 C32 N4 108.6(7) . . ? O1 C34 Ru1 179.0(8) . . ? C29 C35 C25 122.1(7) . . ? C26 C37 C38 121.8(7) . . ? C16 C38 C39 117.7(8) . . ? C16 C38 C37 117.8(7) . . ? C39 C38 C37 124.4(7) . . ? C40 C39 C38 118.7(7) . . ? C39 C40 C41 121.9(7) . . ? N42 C41 C40 121.6(7) . . ? C41 N42 C16 116.7(6) . . ? C41 N42 Ru1 131.4(5) . . ? C16 N42 Ru1 111.5(4) . . ? C45 C43 C51 119.8(7) . . ? C45 C44 C46 119.2(7) . . ? C44 C45 C43 120.3(7) . . ? C44 C45 P1 118.5(5) . . ? C43 C45 P1 121.1(6) . . ? C47 C46 C44 120.5(8) . . ? C51 C47 C46 120.4(8) . . ? C8 C48 C12 122.7(8) . . ? C50 C49 C3 120.3(8) . . ? C49 C50 C4 121.2(9) . . ? C47 C51 C43 119.8(7) . . ? N30 C52 C53 177.9(11) . . ? N1 C600 N3 111.2(6) . . ? N1 C600 C29 121.1(7) . . ? N3 C600 C29 127.6(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C34 Ru1 P1 C1 168.9(3) . . . . ? C14 Ru1 P1 C1 -90.3(3) . . . . ? N1 Ru1 P1 C1 -13.3(3) . . . . ? N42 Ru1 P1 C1 63.3(3) . . . . ? Cl2 Ru1 P1 C1 54.6(9) . . . . ? C34 Ru1 P1 C8 -66.4(3) . . . . ? C14 Ru1 P1 C8 34.5(3) . . . . ? N1 Ru1 P1 C8 111.5(3) . . . . ? N42 Ru1 P1 C8 -171.9(3) . . . . ? Cl2 Ru1 P1 C8 179(100) . . . . ? C34 Ru1 P1 C45 50.3(3) . . . . ? C14 Ru1 P1 C45 151.1(3) . . . . ? N1 Ru1 P1 C45 -131.9(3) . . . . ? N42 Ru1 P1 C45 -55.2(3) . . . . ? Cl2 Ru1 P1 C45 -63.9(9) . . . . ? C34 Ru1 N1 C600 62(3) . . . . ? C14 Ru1 N1 C600 -2.6(5) . . . . ? N42 Ru1 N1 C600 174.5(5) . . . . ? P1 Ru1 N1 C600 -93.6(5) . . . . ? Cl2 Ru1 N1 C600 90.0(5) . . . . ? C34 Ru1 N1 C15 -115(3) . . . . ? C14 Ru1 N1 C15 -179.5(5) . . . . ? N42 Ru1 N1 C15 -2.3(5) . . . . ? P1 Ru1 N1 C15 89.5(5) . . . . ? Cl2 Ru1 N1 C15 -86.8(5) . . . . ? C8 P1 C1 C4 133.7(6) . . . . ? C45 P1 C1 C4 29.2(7) . . . . ? Ru1 P1 C1 C4 -99.5(6) . . . . ? C8 P1 C1 C2 -55.1(7) . . . . ? C45 P1 C1 C2 -159.6(6) . . . . ? Ru1 P1 C1 C2 71.7(6) . . . . ? C4 C1 C2 C3 1.7(11) . . . . ? P1 C1 C2 C3 -169.7(6) . . . . ? C1 C2 C3 C49 -0.4(12) . . . . ? C2 C1 C4 C50 -3.4(12) . . . . ? P1 C1 C4 C50 168.1(6) . . . . ? C1 P1 C8 C9 31.2(8) . . . . ? C45 P1 C8 C9 138.0(7) . . . . ? Ru1 P1 C8 C9 -93.7(7) . . . . ? C1 P1 C8 C48 -155.3(6) . . . . ? C45 P1 C8 C48 -48.4(7) . . . . ? Ru1 P1 C8 C48 79.9(6) . . . . ? C48 C8 C9 C10 0.7(13) . . . . ? P1 C8 C9 C10 174.1(7) . . . . ? C8 C9 C10 C11 -1.0(16) . . . . ? C9 C10 C11 C12 1.3(17) . . . . ? C10 C11 C12 C48 -1.3(16) . . . . ? C32 N4 C14 N3 -0.6(8) . . . . ? C23 N4 C14 N3 -179.4(6) . . . . ? C32 N4 C14 Ru1 178.4(7) . . . . ? C23 N4 C14 Ru1 -0.4(13) . . . . ? C600 N3 C14 N4 179.7(6) . . . . ? C31 N3 C14 N4 -0.5(8) . . . . ? C600 N3 C14 Ru1 0.3(8) . . . . ? C31 N3 C14 Ru1 -179.8(5) . . . . ? C34 Ru1 C14 N4 7.0(9) . . . . ? N1 Ru1 C14 N4 -177.8(9) . . . . ? N42 Ru1 C14 N4 176.0(7) . . . . ? P1 Ru1 C14 N4 -84.9(9) . . . . ? Cl2 Ru1 C14 N4 97.3(9) . . . . ? C34 Ru1 C14 N3 -174.0(5) . . . . ? N1 Ru1 C14 N3 1.1(5) . . . . ? N42 Ru1 C14 N3 -5.0(9) . . . . ? P1 Ru1 C14 N3 94.0(5) . . . . ? Cl2 Ru1 C14 N3 -83.7(5) . . . . ? C600 N1 C15 C25 2.5(10) . . . . ? Ru1 N1 C15 C25 179.3(5) . . . . ? C600 N1 C15 C16 -175.1(6) . . . . ? Ru1 N1 C15 C16 1.7(8) . . . . ? N1 C15 C16 N42 0.7(9) . . . . ? C25 C15 C16 N42 -176.9(6) . . . . ? N1 C15 C16 C38 175.1(6) . . . . ? C25 C15 C16 C38 -2.5(10) . . . . ? C21 N6 C17 C18 -0.4(12) . . . . ? C21 N6 C17 C23 -178.1(8) . . . . ? N6 C17 C18 C19 0.8(13) . . . . ? C23 C17 C18 C19 178.5(8) . . . . ? C17 C18 C19 C20 0.8(16) . . . . ? C18 C19 C20 C21 -2.7(17) . . . . ? C17 N6 C21 C20 -1.6(15) . . . . ? C19 C20 C21 N6 3.2(18) . . . . ? C14 N4 C23 C17 -72.0(9) . . . . ? C32 N4 C23 C17 109.4(8) . . . . ? N6 C17 C23 N4 -25.2(10) . . . . ? C18 C17 C23 N4 157.1(7) . . . . ? N1 C15 C25 C26 -179.2(6) . . . . ? C16 C15 C25 C26 -1.8(11) . . . . ? N1 C15 C25 C35 -1.2(10) . . . . ? C16 C15 C25 C35 176.2(6) . . . . ? C15 C25 C26 C37 2.7(12) . . . . ? C35 C25 C26 C37 -175.0(8) . . . . ? C14 N3 C31 C32 1.5(9) . . . . ? C600 N3 C31 C32 -178.7(7) . . . . ? N3 C31 C32 N4 -1.8(9) . . . . ? C14 N4 C32 C31 1.6(9) . . . . ? C23 N4 C32 C31 -179.6(7) . . . . ? C14 Ru1 C34 O1 119(48) . . . . ? N1 Ru1 C34 O1 55(50) . . . . ? N42 Ru1 C34 O1 -56(49) . . . . ? P1 Ru1 C34 O1 -149(48) . . . . ? Cl2 Ru1 C34 O1 27(48) . . . . ? C600 C29 C35 C25 3.0(11) . . . . ? C15 C25 C35 C29 -1.6(11) . . . . ? C26 C25 C35 C29 176.1(8) . . . . ? C25 C26 C37 C38 0.5(12) . . . . ? N42 C16 C38 C39 2.5(11) . . . . ? C15 C16 C38 C39 -171.5(7) . . . . ? N42 C16 C38 C37 179.6(7) . . . . ? C15 C16 C38 C37 5.6(10) . . . . ? C26 C37 C38 C16 -4.7(11) . . . . ? C26 C37 C38 C39 172.2(8) . . . . ? C16 C38 C39 C40 0.1(11) . . . . ? C37 C38 C39 C40 -176.8(8) . . . . ? C38 C39 C40 C41 -2.1(12) . . . . ? C39 C40 C41 N42 1.8(12) . . . . ? C40 C41 N42 C16 0.8(10) . . . . ? C40 C41 N42 Ru1 173.0(5) . . . . ? C38 C16 N42 C41 -2.9(10) . . . . ? C15 C16 N42 C41 171.2(6) . . . . ? C38 C16 N42 Ru1 -176.6(5) . . . . ? C15 C16 N42 Ru1 -2.5(7) . . . . ? C34 Ru1 N42 C41 4.9(7) . . . . ? C14 Ru1 N42 C41 -163.9(6) . . . . ? N1 Ru1 N42 C41 -170.0(6) . . . . ? P1 Ru1 N42 C41 97.3(6) . . . . ? Cl2 Ru1 N42 C41 -83.3(6) . . . . ? C34 Ru1 N42 C16 177.4(5) . . . . ? C14 Ru1 N42 C16 8.6(8) . . . . ? N1 Ru1 N42 C16 2.5(4) . . . . ? P1 Ru1 N42 C16 -90.2(4) . . . . ? Cl2 Ru1 N42 C16 89.2(4) . . . . ? C46 C44 C45 C43 -3.0(11) . . . . ? C46 C44 C45 P1 172.2(6) . . . . ? C51 C43 C45 C44 1.0(11) . . . . ? C51 C43 C45 P1 -174.1(5) . . . . ? C1 P1 C45 C44 51.8(6) . . . . ? C8 P1 C45 C44 -61.4(6) . . . . ? Ru1 P1 C45 C44 174.4(5) . . . . ? C1 P1 C45 C43 -133.0(6) . . . . ? C8 P1 C45 C43 113.7(6) . . . . ? Ru1 P1 C45 C43 -10.5(7) . . . . ? C45 C44 C46 C47 2.4(12) . . . . ? C44 C46 C47 C51 0.4(13) . . . . ? C9 C8 C48 C12 -0.7(13) . . . . ? P1 C8 C48 C12 -174.8(7) . . . . ? C11 C12 C48 C8 1.1(14) . . . . ? C2 C3 C49 C50 0.9(13) . . . . ? C3 C49 C50 C4 -2.6(14) . . . . ? C1 C4 C50 C49 4.0(14) . . . . ? C46 C47 C51 C43 -2.4(12) . . . . ? C45 C43 C51 C47 1.7(11) . . . . ? C15 N1 C600 N3 -179.8(6) . . . . ? Ru1 N1 C600 N3 3.4(8) . . . . ? C15 N1 C600 C29 -1.0(10) . . . . ? Ru1 N1 C600 C29 -177.8(5) . . . . ? C14 N3 C600 N1 -2.4(9) . . . . ? C31 N3 C600 N1 177.8(7) . . . . ? C14 N3 C600 C29 178.9(7) . . . . ? C31 N3 C600 C29 -0.9(12) . . . . ? C35 C29 C600 N1 -1.7(11) . . . . ? C35 C29 C600 N3 176.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.930 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.122