# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mpmsg2final _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H30 Cl F6 N2 P Ru' _chemical_formula_weight 664.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 38.416(3) _cell_length_b 7.5479(5) _cell_length_c 20.9677(13) _cell_angle_alpha 90.00 _cell_angle_beta 120.4000(10) _cell_angle_gamma 90.00 _cell_volume 5243.9(6) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2456 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 24.56 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8330 _exptl_absorpt_correction_T_max 0.9678 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD DIFFARCTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12527 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_unetI/netI 0.0308 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4604 _reflns_number_gt 4391 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0302P)^2^+19.0569P] 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 4604 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.199 _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 0.942461(7) 0.05813(3) 0.563022(13) 0.01266(9) Uani 1 1 d . . . P1 P 0.90717(3) 0.55075(13) 0.74574(5) 0.0232(2) Uani 1 1 d . . . Cl1 Cl 0.93481(2) -0.12289(11) 0.46187(4) 0.01847(18) Uani 1 1 d . . . F1 F 0.88254(8) 0.6464(4) 0.66719(13) 0.0567(8) Uani 1 1 d . . . F2 F 0.89444(9) 0.3619(4) 0.70740(15) 0.0563(8) Uani 1 1 d . . . F3 F 0.86880(7) 0.5566(3) 0.75542(13) 0.0417(6) Uani 1 1 d . . . F4 F 0.94627(8) 0.5450(3) 0.73631(15) 0.0417(6) Uani 1 1 d . . . F5 F 0.92107(8) 0.7394(3) 0.78460(15) 0.0457(6) Uani 1 1 d . . . F6 F 0.93260(8) 0.4567(4) 0.82400(13) 0.0470(7) Uani 1 1 d . . . N1 N 0.87724(8) 0.0848(3) 0.50382(14) 0.0134(6) Uani 1 1 d . . . N2 N 0.92843(8) 0.2874(4) 0.49270(14) 0.0159(6) Uani 1 1 d . . . C1 C 0.96053(10) -0.1454(5) 0.65063(17) 0.0208(7) Uani 1 1 d . . . H1 H 0.9454 -0.2567 0.6396 0.025 Uiso 1 1 calc R . . C2 C 0.94639(10) 0.0061(5) 0.66938(17) 0.0199(7) Uani 1 1 d . . . H2 H 0.9215 -0.0017 0.6713 0.024 Uiso 1 1 calc R . . C3 C 0.96314(10) 0.1745(5) 0.67219(17) 0.0215(8) Uani 1 1 d . . . H3 H 0.9502 0.2815 0.6769 0.026 Uiso 1 1 calc R . . C4 C 0.99389(10) 0.1885(5) 0.65450(18) 0.0252(8) Uani 1 1 d . . . H4 H 1.0017 0.3064 0.6466 0.030 Uiso 1 1 calc R . . C5 C 1.00866(10) 0.0389(5) 0.63597(19) 0.0257(8) Uani 1 1 d . . . H5 H 1.0265 0.0531 0.6155 0.031 Uiso 1 1 calc R . . C6 C 0.99131(10) -0.1270(5) 0.63347(18) 0.0241(8) Uani 1 1 d . . . H6 H 0.9970 -0.2265 0.6101 0.029 Uiso 1 1 calc R . . C7 C 0.91725(10) 0.4397(4) 0.52487(19) 0.0197(7) Uani 1 1 d . . . H7A H 0.9173 0.5482 0.5001 0.024 Uiso 1 1 calc R . . H7B H 0.9375 0.4516 0.5768 0.024 Uiso 1 1 calc R . . C8 C 0.87588(10) 0.4165(4) 0.51735(19) 0.0187(7) Uani 1 1 d . . . H8A H 0.8733 0.5042 0.5485 0.022 Uiso 1 1 calc R . . H8B H 0.8556 0.4434 0.4667 0.022 Uiso 1 1 calc R . . C9 C 0.86602(10) 0.2362(4) 0.53659(17) 0.0151(7) Uani 1 1 d . . . H9A H 0.8803 0.2232 0.5899 0.018 Uiso 1 1 calc R . . H9B H 0.8373 0.2306 0.5189 0.018 Uiso 1 1 calc R . . C10 C 0.86262(10) 0.1274(4) 0.42436(17) 0.0163(7) Uani 1 1 d . . . H10A H 0.8367 0.1869 0.4029 0.020 Uiso 1 1 calc R . . H10B H 0.8590 0.0186 0.3971 0.020 Uiso 1 1 calc R . . C11 C 0.89314(10) 0.2472(5) 0.41800(17) 0.0183(7) Uani 1 1 d . . . H11A H 0.9024 0.1886 0.3882 0.022 Uiso 1 1 calc R . . H11B H 0.8800 0.3569 0.3936 0.022 Uiso 1 1 calc R . . C12 C 0.96314(11) 0.3423(5) 0.4846(2) 0.0248(8) Uani 1 1 d . . . H12A H 0.9727 0.2423 0.4695 0.037 Uiso 1 1 calc R . . H12B H 0.9845 0.3860 0.5311 0.037 Uiso 1 1 calc R . . H12C H 0.9547 0.4340 0.4480 0.037 Uiso 1 1 calc R . . C13 C 0.85911(9) -0.0885(4) 0.51111(17) 0.0140(7) Uani 1 1 d . . . H13A H 0.8696 -0.1842 0.4947 0.017 Uiso 1 1 calc R . . H13B H 0.8686 -0.1079 0.5631 0.017 Uiso 1 1 calc R . . C14 C 0.81346(10) -0.1011(4) 0.46900(18) 0.0159(7) Uani 1 1 d . . . C15 C 0.79151(10) -0.0437(4) 0.50268(19) 0.0184(7) Uani 1 1 d . . . C16 C 0.80956(10) 0.0146(4) 0.57816(19) 0.0192(7) Uani 1 1 d . . . H16 H 0.8375 0.0129 0.6080 0.023 Uiso 1 1 calc R . . C17 C 0.78685(12) 0.0721(5) 0.6072(2) 0.0262(8) Uani 1 1 d . . . H17 H 0.7995 0.1107 0.6560 0.031 Uiso 1 1 calc R . . C18 C 0.74412(12) 0.0739(5) 0.5637(2) 0.0283(9) Uani 1 1 d . . . H18 H 0.7289 0.1150 0.5839 0.034 Uiso 1 1 calc R . . C19 C 0.72547(11) 0.0161(5) 0.4932(2) 0.0254(8) Uani 1 1 d . . . H19 H 0.6974 0.0171 0.4654 0.030 Uiso 1 1 calc R . . C20 C 0.74787(10) -0.0468(4) 0.4601(2) 0.0205(7) Uani 1 1 d . . . C21 C 0.72838(10) -0.1114(5) 0.3884(2) 0.0225(8) Uani 1 1 d . . . H21 H 0.7003 -0.1087 0.3609 0.027 Uiso 1 1 calc R . . C22 C 0.74957(10) -0.1801(4) 0.35648(19) 0.0211(7) Uani 1 1 d . . . C23 C 0.72880(11) -0.2561(5) 0.2844(2) 0.0271(8) Uani 1 1 d . . . H23 H 0.7007 -0.2566 0.2580 0.033 Uiso 1 1 calc R . . C24 C 0.74912(12) -0.3277(5) 0.2534(2) 0.0308(9) Uani 1 1 d . . . H24 H 0.7350 -0.3768 0.2063 0.037 Uiso 1 1 calc R . . C25 C 0.79203(11) -0.3280(5) 0.29282(19) 0.0254(8) Uani 1 1 d . . . H25 H 0.8058 -0.3783 0.2715 0.030 Uiso 1 1 calc R . . C26 C 0.81310(10) -0.2547(5) 0.36181(19) 0.0212(7) Uani 1 1 d . . . H26 H 0.8412 -0.2553 0.3865 0.025 Uiso 1 1 calc R . . C27 C 0.79311(10) -0.1766(4) 0.39721(18) 0.0169(7) 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 0.01148(14) 0.01396(15) 0.01255(14) 0.00051(10) 0.00608(11) -0.00059(10) P1 0.0235(5) 0.0283(5) 0.0195(5) -0.0037(4) 0.0121(4) -0.0010(4) Cl1 0.0218(4) 0.0175(4) 0.0197(4) -0.0021(3) 0.0131(3) -0.0004(3) F1 0.0602(18) 0.078(2) 0.0309(14) 0.0183(14) 0.0223(13) 0.0258(16) F2 0.077(2) 0.0483(17) 0.0612(18) -0.0311(14) 0.0483(16) -0.0294(15) F3 0.0250(12) 0.0660(18) 0.0381(13) -0.0101(12) 0.0189(11) -0.0077(11) F4 0.0472(15) 0.0347(14) 0.0647(17) 0.0047(12) 0.0442(14) 0.0062(11) F5 0.0458(15) 0.0325(14) 0.0653(17) -0.0206(12) 0.0330(14) -0.0075(11) F6 0.0520(16) 0.0587(17) 0.0296(13) 0.0118(12) 0.0202(12) 0.0232(13) N1 0.0125(13) 0.0119(14) 0.0136(13) 0.0005(10) 0.0049(11) -0.0012(10) N2 0.0147(14) 0.0163(15) 0.0165(14) 0.0013(11) 0.0077(12) -0.0042(11) C1 0.0214(18) 0.0235(19) 0.0114(16) 0.0038(14) 0.0038(14) 0.0004(15) C2 0.0124(16) 0.035(2) 0.0076(15) 0.0013(14) 0.0015(13) 0.0006(15) C3 0.0191(18) 0.0269(19) 0.0096(16) -0.0016(14) 0.0007(14) 0.0042(15) C4 0.0188(18) 0.028(2) 0.0152(17) 0.0020(15) -0.0015(14) -0.0084(15) C5 0.0120(17) 0.044(2) 0.0189(18) 0.0076(16) 0.0059(14) 0.0039(16) C6 0.0219(19) 0.030(2) 0.0146(17) 0.0047(15) 0.0048(15) 0.0081(15) C7 0.0230(18) 0.0136(17) 0.0218(18) -0.0018(14) 0.0109(15) -0.0058(14) C8 0.0211(18) 0.0105(16) 0.0258(18) 0.0003(14) 0.0128(15) 0.0003(13) C9 0.0150(16) 0.0160(17) 0.0150(16) -0.0008(13) 0.0080(13) 0.0010(13) C10 0.0175(17) 0.0158(17) 0.0120(16) 0.0009(13) 0.0049(13) -0.0006(13) C11 0.0216(18) 0.0176(17) 0.0145(16) 0.0031(13) 0.0082(14) -0.0007(14) C12 0.0240(19) 0.029(2) 0.0255(19) 0.0007(16) 0.0157(16) -0.0059(16) C13 0.0132(16) 0.0120(16) 0.0151(16) 0.0028(13) 0.0059(13) 0.0000(12) C14 0.0136(16) 0.0110(16) 0.0218(17) 0.0034(13) 0.0079(14) -0.0001(12) C15 0.0170(17) 0.0128(17) 0.0261(18) 0.0027(14) 0.0113(15) -0.0012(13) C16 0.0197(17) 0.0150(17) 0.0257(18) 0.0043(14) 0.0136(15) -0.0044(14) C17 0.033(2) 0.0211(19) 0.035(2) 0.0045(16) 0.0247(18) 0.0000(16) C18 0.031(2) 0.023(2) 0.044(2) 0.0066(17) 0.0285(19) 0.0053(16) C19 0.0198(18) 0.0169(18) 0.044(2) 0.0085(16) 0.0196(17) 0.0039(14) C20 0.0175(17) 0.0127(17) 0.032(2) 0.0077(14) 0.0129(16) 0.0004(13) C21 0.0130(17) 0.0159(17) 0.032(2) 0.0045(15) 0.0069(15) -0.0007(13) C22 0.0164(17) 0.0112(16) 0.0302(19) 0.0025(14) 0.0077(15) -0.0018(13) C23 0.0181(18) 0.0162(18) 0.030(2) 0.0009(15) -0.0003(16) -0.0024(15) C24 0.032(2) 0.0221(19) 0.0221(19) -0.0064(16) 0.0015(16) -0.0034(17) C25 0.0269(19) 0.0199(19) 0.0239(19) -0.0050(15) 0.0089(16) 0.0000(15) C26 0.0185(17) 0.0170(18) 0.0241(18) 0.0002(14) 0.0078(15) -0.0023(14) C27 0.0162(17) 0.0074(16) 0.0226(18) 0.0034(13) 0.0065(14) -0.0003(13) _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 N2 2.157(3) . ? Ru1 N1 2.171(3) . ? Ru1 C4 2.172(3) . ? Ru1 C3 2.191(3) . ? Ru1 C2 2.193(3) . ? Ru1 C6 2.202(3) . ? Ru1 C5 2.212(3) . ? Ru1 C1 2.219(3) . ? Ru1 Cl1 2.4126(8) . ? P1 F2 1.587(3) . ? P1 F3 1.587(2) . ? P1 F6 1.590(2) . ? P1 F5 1.593(2) . ? P1 F1 1.598(3) . ? P1 F4 1.612(2) . ? N1 C10 1.499(4) . ? N1 C9 1.505(4) . ? N1 C13 1.525(4) . ? N2 C12 1.486(4) . ? N2 C11 1.495(4) . ? N2 C7 1.502(4) . ? C1 C2 1.405(5) . ? C1 C6 1.406(5) . ? C1 H1 0.9800 . ? C2 C3 1.412(5) . ? C2 H2 0.9800 . ? C3 C4 1.410(5) . ? C3 H3 0.9800 . ? C4 C5 1.404(5) . ? C4 H4 0.9800 . ? C5 C6 1.407(5) . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C7 C8 1.526(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.521(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.539(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.516(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.414(5) . ? C14 C27 1.418(5) . ? C15 C16 1.438(5) . ? C15 C20 1.447(5) . ? C16 C17 1.363(5) . ? C16 H16 0.9300 . ? C17 C18 1.418(5) . ? C17 H17 0.9300 . ? C18 C19 1.347(6) . ? C18 H18 0.9300 . ? C19 C20 1.433(5) . ? C19 H19 0.9300 . ? C20 C21 1.385(5) . ? C21 C22 1.390(5) . ? C21 H21 0.9300 . ? C22 C23 1.425(5) . ? C22 C27 1.443(5) . ? C23 C24 1.355(6) . ? C23 H23 0.9300 . ? C24 C25 1.422(5) . ? C24 H24 0.9300 . ? C25 C26 1.367(5) . ? C25 H25 0.9300 . ? C26 C27 1.437(5) . ? C26 H26 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru1 N1 73.61(10) . . ? N2 Ru1 C4 92.37(12) . . ? N1 Ru1 C4 137.23(12) . . ? N2 Ru1 C3 103.04(12) . . ? N1 Ru1 C3 105.28(11) . . ? C4 Ru1 C3 37.71(13) . . ? N2 Ru1 C2 134.70(12) . . ? N1 Ru1 C2 93.65(11) . . ? C4 Ru1 C2 67.62(13) . . ? C3 Ru1 C2 37.57(13) . . ? N2 Ru1 C6 143.19(12) . . ? N1 Ru1 C6 141.96(12) . . ? C4 Ru1 C6 67.01(14) . . ? C3 Ru1 C6 79.53(13) . . ? C2 Ru1 C6 66.90(13) . . ? N2 Ru1 C5 109.12(12) . . ? N1 Ru1 C5 172.83(12) . . ? C4 Ru1 C5 37.34(14) . . ? C3 Ru1 C5 67.77(13) . . ? C2 Ru1 C5 79.72(13) . . ? C6 Ru1 C5 37.17(14) . . ? N2 Ru1 C1 170.46(11) . . ? N1 Ru1 C1 108.94(11) . . ? C4 Ru1 C1 79.56(13) . . ? C3 Ru1 C1 67.45(13) . . ? C2 Ru1 C1 37.12(13) . . ? C6 Ru1 C1 37.09(13) . . ? C5 Ru1 C1 67.27(13) . . ? N2 Ru1 Cl1 88.64(7) . . ? N1 Ru1 Cl1 87.59(7) . . ? C4 Ru1 Cl1 133.22(10) . . ? C3 Ru1 Cl1 164.54(9) . . ? C2 Ru1 Cl1 135.05(10) . . ? C6 Ru1 Cl1 85.06(10) . . ? C5 Ru1 Cl1 99.02(10) . . ? C1 Ru1 Cl1 100.58(9) . . ? F2 P1 F3 91.25(14) . . ? F2 P1 F6 89.59(16) . . ? F3 P1 F6 90.34(14) . . ? F2 P1 F5 178.55(15) . . ? F3 P1 F5 90.13(13) . . ? F6 P1 F5 89.96(15) . . ? F2 P1 F1 90.79(17) . . ? F3 P1 F1 90.88(14) . . ? F6 P1 F1 178.71(17) . . ? F5 P1 F1 89.63(16) . . ? F2 P1 F4 88.91(14) . . ? F3 P1 F4 179.74(15) . . ? F6 P1 F4 89.46(14) . . ? F5 P1 F4 89.70(13) . . ? F1 P1 F4 89.32(14) . . ? C10 N1 C9 108.2(2) . . ? C10 N1 C13 111.2(2) . . ? C9 N1 C13 110.8(2) . . ? C10 N1 Ru1 109.28(19) . . ? C9 N1 Ru1 108.89(18) . . ? C13 N1 Ru1 108.46(18) . . ? C12 N2 C11 109.1(2) . . ? C12 N2 C7 108.4(3) . . ? C11 N2 C7 108.2(3) . . ? C12 N2 Ru1 111.9(2) . . ? C11 N2 Ru1 109.52(19) . . ? C7 N2 Ru1 109.67(19) . . ? C2 C1 C6 119.0(3) . . ? C2 C1 Ru1 70.43(19) . . ? C6 C1 Ru1 70.80(19) . . ? C2 C1 H1 119.9 . . ? C6 C1 H1 119.9 . . ? Ru1 C1 H1 119.9 . . ? C1 C2 C3 120.8(3) . . ? C1 C2 Ru1 72.44(18) . . ? C3 C2 Ru1 71.15(19) . . ? C1 C2 H2 119.1 . . ? C3 C2 H2 119.1 . . ? Ru1 C2 H2 119.1 . . ? C4 C3 C2 118.8(3) . . ? C4 C3 Ru1 70.38(19) . . ? C2 C3 Ru1 71.28(19) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? Ru1 C3 H3 120.1 . . ? C5 C4 C3 121.5(3) . . ? C5 C4 Ru1 72.9(2) . . ? C3 C4 Ru1 71.91(19) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? Ru1 C4 H4 118.8 . . ? C4 C5 C6 118.4(3) . . ? C4 C5 Ru1 69.78(19) . . ? C6 C5 Ru1 71.1(2) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? Ru1 C5 H5 120.2 . . ? C1 C6 C5 121.5(3) . . ? C1 C6 Ru1 72.11(19) . . ? C5 C6 Ru1 71.8(2) . . ? C1 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? Ru1 C6 H6 118.7 . . ? N2 C7 C8 112.6(3) . . ? N2 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N2 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C7 117.5(3) . . ? C9 C8 H8A 107.9 . . ? C7 C8 H8A 107.9 . . ? C9 C8 H8B 107.9 . . ? C7 C8 H8B 107.9 . . ? H8A C8 H8B 107.2 . . ? N1 C9 C8 113.0(2) . . ? N1 C9 H9A 109.0 . . ? C8 C9 H9A 109.0 . . ? N1 C9 H9B 109.0 . . ? C8 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N1 C10 C11 110.4(2) . . ? N1 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N1 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? N2 C11 C10 110.8(2) . . ? N2 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N1 116.6(3) . . ? C14 C13 H13A 108.1 . . ? N1 C13 H13A 108.1 . . ? C14 C13 H13B 108.1 . . ? N1 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C15 C14 C27 120.4(3) . . ? C15 C14 C13 119.8(3) . . ? C27 C14 C13 119.8(3) . . ? C14 C15 C16 124.5(3) . . ? C14 C15 C20 118.9(3) . . ? C16 C15 C20 116.6(3) . . ? C17 C16 C15 121.8(3) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 120.7(4) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 120.1(3) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 121.5(3) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C21 C20 C19 121.0(3) . . ? C21 C20 C15 119.8(3) . . ? C19 C20 C15 119.2(3) . . ? C20 C21 C22 121.8(3) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C21 C22 C23 120.8(3) . . ? C21 C22 C27 119.6(3) . . ? C23 C22 C27 119.6(3) . . ? C24 C23 C22 121.3(3) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.4(3) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 121.8(3) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C14 C27 C26 124.2(3) . . ? C14 C27 C22 119.1(3) . . ? C26 C27 C22 116.7(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.760 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.086 _database_code_depnum_ccdc_archive 'CCDC 927197' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2ru_iso _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H76 Cl2 F12 N4 P2 Ru2' _chemical_formula_weight 1440.25 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' Cl Cl 0.1484 0.1585 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8707(2) _cell_length_b 19.8808(2) _cell_length_c 20.3162(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.3170(10) _cell_angle_gamma 90.00 _cell_volume 6285.57(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1765 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 24.68 _exptl_crystal_description plates _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.694 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9465 _exptl_absorpt_correction_T_max 0.9661 _exptl_absorpt_process_details 'BRUKER SADABS' 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 1 0.000 0.000 0.000 19.6 -0.5 2 0.000 0.000 0.500 139.0 21.9 3 0.000 0.500 1.000 139.0 22.7 4 0.000 0.500 0.500 19.6 -0.7 5 0.333 0.667 0.021 6.8 0.0 6 0.333 0.833 0.521 6.8 -0.1 7 0.667 0.167 0.479 6.8 -0.1 8 0.667 0.333 0.979 6.8 -0.1 _platon_squeeze_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER-SMART APEX CCD' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63157 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12350 _reflns_number_gt 8768 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0602P)^2^+1.3849P] 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 12350 _refine_ls_number_parameters 761 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.87178(6) 0.31362(5) 0.13385(6) 0.0487(3) Uani 1 1 d . . . F1 F 0.9222(2) 0.27833(19) 0.19779(16) 0.1289(13) Uani 1 1 d . . . F2 F 0.92997(16) 0.37881(14) 0.15062(16) 0.0913(10) Uani 1 1 d . . . F3 F 0.80748(17) 0.34346(15) 0.17695(16) 0.0964(10) Uani 1 1 d . . . F4 F 0.93643(17) 0.28334(14) 0.09122(15) 0.0862(8) Uani 1 1 d . . . F5 F 0.8118(2) 0.25017(15) 0.11540(16) 0.1019(11) Uani 1 1 d . . . F6 F 0.8207(2) 0.34868(18) 0.06913(17) 0.1122(11) Uani 1 1 d . . . Ru2 Ru 0.654336(17) 0.082633(14) 0.186329(14) 0.03282(10) Uani 1 1 d . . . Ru1 Ru 0.818107(16) 0.584926(13) 0.219541(14) 0.03189(9) Uani 1 1 d . . . Cl1 Cl 0.68482(5) 0.54574(5) 0.24643(4) 0.0422(2) Uani 1 1 d . . . Cl2 Cl 0.80206(5) 0.04535(5) 0.21490(5) 0.0464(2) Uani 1 1 d . . . N1 N 0.82728(18) 0.65123(15) 0.30525(15) 0.0412(7) Uani 1 1 d . . . N2 N 0.88374(17) 0.52840(13) 0.30646(13) 0.0325(6) Uani 1 1 d . . . N3 N 0.68639(19) 0.15462(15) 0.26802(15) 0.0444(8) Uani 1 1 d . . . N4 N 0.63418(17) 0.03110(13) 0.27662(14) 0.0346(7) Uani 1 1 d . . . C1 C 0.8341(3) 0.6623(2) 0.14772(19) 0.0538(11) Uani 1 1 d . . . H1 H 0.8317 0.7096 0.1609 0.065 Uiso 1 1 calc R . . C2 C 0.9139(3) 0.6282(2) 0.1629(2) 0.0557(11) Uani 1 1 d . . . C3 C 0.9110(2) 0.5586(2) 0.15732(19) 0.0511(11) Uani 1 1 d . . . H3 H 0.9620 0.5326 0.1775 0.061 Uiso 1 1 calc R . . C4 C 0.8342(2) 0.5238(2) 0.13201(17) 0.0431(9) Uani 1 1 d . . . H4 H 0.8335 0.4747 0.1355 0.052 Uiso 1 1 calc R . . C5 C 0.7564(2) 0.55828(18) 0.11259(16) 0.0379(8) Uani 1 1 d . . . C6 C 0.7570(2) 0.6287(2) 0.12236(18) 0.0456(10) Uani 1 1 d . . . H6 H 0.7024 0.6527 0.1186 0.055 Uiso 1 1 calc R . . C7 C 0.9984(3) 0.6664(3) 0.1806(3) 0.0914(18) Uani 1 1 d . . . H7A H 1.0385 0.6410 0.2127 0.137 Uiso 1 1 calc R . . H7B H 0.9886 0.7093 0.1994 0.137 Uiso 1 1 calc R . . H7C H 1.0215 0.6730 0.1407 0.137 Uiso 1 1 calc R . . C8 C 0.6762(3) 0.5186(2) 0.08353(18) 0.0515(10) Uani 1 1 d . . . H8 H 0.6736 0.4803 0.1135 0.062 Uiso 1 1 calc R . . C9 C 0.5925(3) 0.5562(3) 0.0770(2) 0.0718(13) Uani 1 1 d . . . H9A H 0.5890 0.5763 0.1194 0.108 Uiso 1 1 calc R . . H9B H 0.5455 0.5255 0.0640 0.108 Uiso 1 1 calc R . . H9C H 0.5897 0.5907 0.0436 0.108 Uiso 1 1 calc R . . C10 C 0.6862(3) 0.4899(2) 0.0153(2) 0.0731(14) Uani 1 1 d . . . H10A H 0.6387 0.4607 -0.0016 0.110 Uiso 1 1 calc R . . H10B H 0.7389 0.4650 0.0205 0.110 Uiso 1 1 calc R . . H10C H 0.6872 0.5261 -0.0158 0.110 Uiso 1 1 calc R . . C11 C 0.9175(2) 0.67694(18) 0.3259(2) 0.0512(10) Uani 1 1 d . . . H11A H 0.9180 0.7137 0.3574 0.061 Uiso 1 1 calc R . . H11B H 0.9364 0.6946 0.2867 0.061 Uiso 1 1 calc R . . C12 C 0.9803(2) 0.62327(19) 0.3580(2) 0.0546(11) Uani 1 1 d . . . H12A H 0.9736 0.6181 0.4042 0.066 Uiso 1 1 calc R . . H12B H 1.0379 0.6402 0.3592 0.066 Uiso 1 1 calc R . . C13 C 0.9749(2) 0.55358(18) 0.32650(19) 0.0399(9) Uani 1 1 d . . . H13A H 1.0008 0.5548 0.2871 0.048 Uiso 1 1 calc R . . H13B H 1.0076 0.5223 0.3582 0.048 Uiso 1 1 calc R . . C14 C 0.8395(2) 0.54030(18) 0.36445(16) 0.0383(8) Uani 1 1 d . . . H14A H 0.8796 0.5326 0.4064 0.046 Uiso 1 1 calc R . . H14B H 0.7922 0.5089 0.3621 0.046 Uiso 1 1 calc R . . C15 C 0.8057(2) 0.61214(19) 0.36266(18) 0.0441(9) Uani 1 1 d . . . H15A H 0.7438 0.6112 0.3588 0.053 Uiso 1 1 calc R . . H15B H 0.8303 0.6345 0.4044 0.053 Uiso 1 1 calc R . . C16 C 0.7675(3) 0.7100(2) 0.2912(2) 0.0579(11) Uani 1 1 d . . . H16A H 0.7111 0.6945 0.2710 0.087 Uiso 1 1 calc R . . H16B H 0.7879 0.7405 0.2611 0.087 Uiso 1 1 calc R . . H16C H 0.7652 0.7328 0.3325 0.087 Uiso 1 1 calc R . . C17 C 0.8818(2) 0.45424(16) 0.28718(16) 0.0329(8) Uani 1 1 d . . . H17A H 0.8246 0.4441 0.2623 0.039 Uiso 1 1 calc R . . H17B H 0.9211 0.4480 0.2567 0.039 Uiso 1 1 calc R . . C18 C 0.9040(2) 0.40289(17) 0.34263(16) 0.0337(8) Uani 1 1 d . . . C19 C 0.9899(2) 0.38110(17) 0.36486(17) 0.0359(8) Uani 1 1 d . . . C20 C 1.0596(2) 0.39930(19) 0.3337(2) 0.0443(9) Uani 1 1 d . . . H20 H 1.0490 0.4274 0.2964 0.053 Uiso 1 1 calc R . . C21 C 1.1406(2) 0.3772(2) 0.3563(2) 0.0515(10) Uani 1 1 d . . . H21 H 1.1840 0.3884 0.3335 0.062 Uiso 1 1 calc R . . C22 C 1.1595(2) 0.3369(2) 0.4150(2) 0.0550(11) Uani 1 1 d . . . H22 H 1.2160 0.3243 0.4322 0.066 Uiso 1 1 calc R . . C23 C 1.0962(3) 0.3168(2) 0.4460(2) 0.0523(10) Uani 1 1 d . . . H23 H 1.1096 0.2903 0.4843 0.063 Uiso 1 1 calc R . . C24 C 1.0087(2) 0.33559(18) 0.42076(18) 0.0420(9) Uani 1 1 d . . . C25 C 0.9434(2) 0.30922(18) 0.44842(18) 0.0448(9) Uani 1 1 d . . . H25 H 0.9569 0.2803 0.4849 0.054 Uiso 1 1 calc R . . C26 C 0.8578(2) 0.32479(18) 0.42318(18) 0.0412(9) Uani 1 1 d . . . C27 C 0.7901(3) 0.2927(2) 0.4496(2) 0.0526(10) Uani 1 1 d . . . H27 H 0.8039 0.2616 0.4842 0.063 Uiso 1 1 calc R . . C28 C 0.7072(3) 0.3072(2) 0.4248(2) 0.0610(12) Uani 1 1 d . . . H28 H 0.6640 0.2862 0.4422 0.073 Uiso 1 1 calc R . . C29 C 0.6862(3) 0.3543(2) 0.3722(2) 0.0537(11) Uani 1 1 d . . . H29 H 0.6287 0.3640 0.3552 0.064 Uiso 1 1 calc R . . C30 C 0.7475(2) 0.38576(19) 0.34584(19) 0.0432(9) Uani 1 1 d . . . H30 H 0.7310 0.4166 0.3113 0.052 Uiso 1 1 calc R . . C31 C 0.8370(2) 0.37294(17) 0.36968(16) 0.0361(8) Uani 1 1 d . . . C32 C 0.5306(2) 0.0524(2) 0.1257(2) 0.0519(10) Uani 1 1 d . . . H32 H 0.4904 0.0275 0.1476 0.062 Uiso 1 1 calc R . . C33 C 0.5287(2) 0.1224(2) 0.1270(2) 0.0561(11) Uani 1 1 d . . . C34 C 0.5997(3) 0.1559(2) 0.10967(19) 0.0516(10) Uani 1 1 d . . . H34 H 0.6076 0.2039 0.1201 0.062 Uiso 1 1 calc R . . C35 C 0.6651(2) 0.12139(19) 0.08641(17) 0.0426(9) Uani 1 1 d . . . H35 H 0.7171 0.1455 0.0809 0.051 Uiso 1 1 calc R . . C36 C 0.6623(2) 0.05017(19) 0.08088(17) 0.0412(9) Uani 1 1 d . . . C37 C 0.5943(2) 0.0164(2) 0.10254(17) 0.0443(9) Uani 1 1 d . . . H37 H 0.5975 -0.0325 0.1087 0.053 Uiso 1 1 calc R . . C38 C 0.4518(3) 0.1603(3) 0.1421(3) 0.0873(17) Uani 1 1 d . . . H38A H 0.4094 0.1652 0.1016 0.131 Uiso 1 1 calc R . . H38B H 0.4698 0.2040 0.1597 0.131 Uiso 1 1 calc R . . H38C H 0.4277 0.1358 0.1747 0.131 Uiso 1 1 calc R . . C39 C 0.7268(3) 0.0088(2) 0.05345(19) 0.0547(11) Uani 1 1 d . . . H39 H 0.7449 -0.0281 0.0851 0.066 Uiso 1 1 calc R . . C40 C 0.6815(4) -0.0228(3) -0.0131(2) 0.0884(17) Uani 1 1 d . . . H40A H 0.6299 -0.0449 -0.0067 0.133 Uiso 1 1 calc R . . H40B H 0.7189 -0.0549 -0.0278 0.133 Uiso 1 1 calc R . . H40C H 0.6672 0.0118 -0.0464 0.133 Uiso 1 1 calc R . . C41 C 0.8075(3) 0.0458(3) 0.0441(2) 0.0707(13) Uani 1 1 d . . . H41A H 0.7927 0.0788 0.0093 0.106 Uiso 1 1 calc R . . H41B H 0.8475 0.0143 0.0319 0.106 Uiso 1 1 calc R . . H41C H 0.8331 0.0677 0.0853 0.106 Uiso 1 1 calc R . . C42 C 0.6049(3) 0.18052(19) 0.2861(2) 0.0589(11) Uani 1 1 d . . . H42A H 0.5662 0.1949 0.2455 0.071 Uiso 1 1 calc R . . H42B H 0.6183 0.2195 0.3150 0.071 Uiso 1 1 calc R . . C43 C 0.5595(3) 0.12796(19) 0.3219(2) 0.0607(12) Uani 1 1 d . . . H43A H 0.5888 0.1264 0.3685 0.073 Uiso 1 1 calc R . . H43B H 0.5015 0.1439 0.3213 0.073 Uiso 1 1 calc R . . C44 C 0.5531(2) 0.05612(18) 0.2951(2) 0.0448(9) Uani 1 1 d . . . H44A H 0.5378 0.0266 0.3288 0.054 Uiso 1 1 calc R . . H44B H 0.5072 0.0539 0.2558 0.054 Uiso 1 1 calc R . . C45 C 0.7370(3) 0.1198(2) 0.32795(19) 0.0495(10) Uani 1 1 d . . . H45A H 0.7314 0.1443 0.3681 0.059 Uiso 1 1 calc R . . H45B H 0.7973 0.1197 0.3250 0.059 Uiso 1 1 calc R . . C46 C 0.7070(2) 0.04784(19) 0.33349(17) 0.0424(9) Uani 1 1 d . . . H46A H 0.7545 0.0173 0.3328 0.051 Uiso 1 1 calc R . . H46B H 0.6884 0.0420 0.3758 0.051 Uiso 1 1 calc R . . C47 C 0.7364(3) 0.21280(19) 0.2508(2) 0.0574(11) Uani 1 1 d . . . H47A H 0.7536 0.2406 0.2897 0.086 Uiso 1 1 calc R . . H47B H 0.7014 0.2386 0.2158 0.086 Uiso 1 1 calc R . . H47C H 0.7864 0.1969 0.2357 0.086 Uiso 1 1 calc R . . C48 C 0.6285(2) -0.04410(16) 0.26255(16) 0.0343(8) Uani 1 1 d . . . H48A H 0.6750 -0.0562 0.2401 0.041 Uiso 1 1 calc R . . H48B H 0.5750 -0.0528 0.2314 0.041 Uiso 1 1 calc R . . C49 C 0.6326(2) -0.09060(16) 0.32295(17) 0.0344(8) Uani 1 1 d . . . C50 C 0.7135(2) -0.11463(17) 0.35706(17) 0.0375(8) Uani 1 1 d . . . C51 C 0.7923(2) -0.10453(19) 0.3345(2) 0.0499(10) Uani 1 1 d . . . H51 H 0.7913 -0.0819 0.2943 0.060 Uiso 1 1 calc R . . C52 C 0.8681(3) -0.1269(2) 0.3697(2) 0.0623(12) Uani 1 1 d . . . H52 H 0.9180 -0.1203 0.3530 0.075 Uiso 1 1 calc R . . C53 C 0.8727(3) -0.1603(2) 0.4318(2) 0.0634(12) Uani 1 1 d . . . H53 H 0.9257 -0.1728 0.4571 0.076 Uiso 1 1 calc R . . C54 C 0.8002(3) -0.1739(2) 0.4539(2) 0.0549(11) Uani 1 1 d . . . H54 H 0.8035 -0.1974 0.4939 0.066 Uiso 1 1 calc R . . C55 C 0.7178(2) -0.15308(18) 0.41718(18) 0.0407(9) Uani 1 1 d . . . C56 C 0.6439(2) -0.16996(18) 0.43935(18) 0.0421(9) Uani 1 1 d . . . H56 H 0.6480 -0.1943 0.4790 0.050 Uiso 1 1 calc R . . C57 C 0.5630(2) -0.15133(17) 0.40357(17) 0.0364(8) Uani 1 1 d . . . C58 C 0.4869(2) -0.17094(18) 0.42584(19) 0.0450(9) Uani 1 1 d . . . H58 H 0.4913 -0.1953 0.4655 0.054 Uiso 1 1 calc R . . C59 C 0.4088(2) -0.15476(19) 0.3904(2) 0.0476(10) Uani 1 1 d . . . H59 H 0.3597 -0.1669 0.4061 0.057 Uiso 1 1 calc R . . C60 C 0.4015(2) -0.11972(18) 0.3300(2) 0.0451(9) Uani 1 1 d . . . H60 H 0.3471 -0.1112 0.3046 0.054 Uiso 1 1 calc R . . C61 C 0.4715(2) -0.09784(18) 0.30728(19) 0.0425(9) Uani 1 1 d . . . H61 H 0.4641 -0.0737 0.2674 0.051 Uiso 1 1 calc R . . C62 C 0.5568(2) -0.11122(17) 0.34357(16) 0.0336(8) Uani 1 1 d . . . F7 F 0.4978(2) 0.75689(17) 0.08411(19) 0.1223(12) Uani 1 1 d . A . F8 F 0.65192(19) 0.84877(19) 0.1452(2) 0.1348(15) Uani 1 1 d . A . F9 F 0.5205(4) 0.8639(3) 0.1345(3) 0.0907(17) Uiso 0.50 1 d P A 1 F9A F 0.5761(5) 0.8391(5) 0.0457(4) 0.134(3) Uiso 0.50 1 d P A 1 F10 F 0.6360(4) 0.7496(4) 0.0933(4) 0.103(2) Uiso 0.50 1 d P A 1 F10A F 0.5751(7) 0.7688(6) 0.1841(5) 0.172(4) Uiso 0.50 1 d P A 1 F11 F 0.5178(5) 0.8604(4) 0.0747(4) 0.117(2) Uiso 0.50 1 d P A 2 F11A F 0.6215(5) 0.7833(4) 0.0536(4) 0.121(2) Uiso 0.50 1 d P A 2 F12 F 0.5291(4) 0.8160(4) 0.1744(3) 0.0953(18) Uiso 0.50 1 d P A 2 F12A F 0.6246(5) 0.7417(4) 0.1565(4) 0.121(2) Uiso 0.50 1 d P A 2 P2 P 0.57549(7) 0.80291(6) 0.11394(6) 0.0559(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0453(6) 0.0397(6) 0.0630(7) -0.0098(5) 0.0150(5) -0.0004(5) F1 0.159(3) 0.134(3) 0.081(2) 0.013(2) -0.010(2) 0.053(3) F2 0.0613(16) 0.0680(19) 0.152(3) -0.0437(19) 0.0403(17) -0.0217(14) F3 0.0713(17) 0.098(2) 0.133(3) -0.055(2) 0.0508(17) -0.0147(16) F4 0.0814(18) 0.079(2) 0.109(2) -0.0289(17) 0.0451(16) 0.0054(15) F5 0.128(2) 0.077(2) 0.115(2) -0.0403(18) 0.059(2) -0.0516(18) F6 0.108(2) 0.110(3) 0.107(2) 0.022(2) -0.009(2) 0.020(2) Ru2 0.03415(16) 0.02490(17) 0.04107(18) 0.00441(12) 0.01148(13) 0.00083(11) Ru1 0.03183(15) 0.02733(18) 0.03624(17) 0.00431(12) 0.00603(12) 0.00047(11) Cl1 0.0347(4) 0.0491(6) 0.0425(5) 0.0009(4) 0.0065(4) -0.0050(4) Cl2 0.0382(5) 0.0555(6) 0.0467(5) 0.0007(5) 0.0110(4) 0.0074(4) N1 0.0391(16) 0.0307(18) 0.0520(19) -0.0030(14) 0.0049(14) 0.0012(13) N2 0.0334(14) 0.0276(16) 0.0354(16) 0.0026(13) 0.0037(12) -0.0022(12) N3 0.0513(18) 0.0301(18) 0.055(2) -0.0045(15) 0.0191(16) -0.0042(14) N4 0.0393(16) 0.0261(17) 0.0419(17) 0.0016(13) 0.0165(13) 0.0017(12) C1 0.078(3) 0.040(2) 0.045(2) 0.0120(19) 0.016(2) -0.011(2) C2 0.053(2) 0.068(3) 0.048(2) 0.013(2) 0.015(2) -0.014(2) C3 0.041(2) 0.070(3) 0.046(2) 0.016(2) 0.0153(18) 0.015(2) C4 0.053(2) 0.045(2) 0.035(2) 0.0059(17) 0.0156(18) 0.0082(19) C5 0.050(2) 0.036(2) 0.0286(19) 0.0057(16) 0.0089(16) -0.0003(17) C6 0.053(2) 0.045(3) 0.040(2) 0.0156(18) 0.0100(18) 0.0098(19) C7 0.067(3) 0.122(5) 0.087(4) 0.015(3) 0.018(3) -0.045(3) C8 0.060(3) 0.056(3) 0.036(2) -0.0007(19) 0.0045(19) -0.017(2) C9 0.049(3) 0.109(4) 0.054(3) 0.004(3) 0.003(2) -0.008(3) C10 0.098(4) 0.071(3) 0.046(3) -0.010(2) 0.005(2) -0.016(3) C11 0.046(2) 0.030(2) 0.073(3) -0.012(2) 0.002(2) -0.0078(17) C12 0.045(2) 0.041(3) 0.072(3) -0.004(2) -0.003(2) -0.0091(18) C13 0.0298(18) 0.035(2) 0.052(2) 0.0041(18) -0.0011(16) 0.0008(15) C14 0.044(2) 0.038(2) 0.0317(19) -0.0004(16) 0.0060(16) -0.0007(16) C15 0.052(2) 0.041(2) 0.039(2) -0.0079(18) 0.0084(17) 0.0012(18) C16 0.060(3) 0.034(2) 0.077(3) -0.003(2) 0.008(2) 0.014(2) C17 0.0400(18) 0.0238(19) 0.0338(19) -0.0012(15) 0.0046(15) 0.0004(15) C18 0.0385(18) 0.029(2) 0.0326(19) 0.0018(15) 0.0039(15) -0.0006(15) C19 0.047(2) 0.025(2) 0.0344(19) -0.0031(16) 0.0049(16) 0.0000(16) C20 0.043(2) 0.038(2) 0.053(2) 0.0058(18) 0.0130(18) 0.0035(17) C21 0.047(2) 0.040(2) 0.070(3) -0.003(2) 0.018(2) 0.0042(18) C22 0.038(2) 0.043(3) 0.079(3) -0.006(2) 0.001(2) 0.0084(18) C23 0.059(3) 0.044(3) 0.050(2) 0.0071(19) 0.000(2) 0.013(2) C24 0.048(2) 0.032(2) 0.044(2) 0.0024(17) 0.0023(18) 0.0048(17) C25 0.058(2) 0.038(2) 0.039(2) 0.0110(17) 0.0083(18) 0.0061(18) C26 0.053(2) 0.031(2) 0.042(2) 0.0019(17) 0.0138(18) -0.0028(17) C27 0.068(3) 0.046(3) 0.047(2) 0.0071(19) 0.019(2) -0.012(2) C28 0.063(3) 0.059(3) 0.067(3) -0.008(2) 0.026(2) -0.024(2) C29 0.045(2) 0.052(3) 0.062(3) -0.009(2) 0.008(2) -0.0093(19) C30 0.040(2) 0.039(2) 0.049(2) -0.0010(18) 0.0048(17) -0.0055(17) C31 0.044(2) 0.028(2) 0.0342(19) -0.0047(16) 0.0031(16) -0.0019(16) C32 0.043(2) 0.058(3) 0.051(2) 0.017(2) 0.0009(19) -0.010(2) C33 0.042(2) 0.059(3) 0.066(3) 0.023(2) 0.010(2) 0.013(2) C34 0.060(3) 0.038(2) 0.056(3) 0.016(2) 0.010(2) 0.0058(19) C35 0.047(2) 0.040(2) 0.042(2) 0.0140(18) 0.0126(17) -0.0054(17) C36 0.049(2) 0.041(2) 0.0296(19) 0.0058(17) 0.0001(16) 0.0031(18) C37 0.050(2) 0.040(2) 0.038(2) 0.0116(17) -0.0050(18) -0.0071(18) C38 0.056(3) 0.100(4) 0.108(4) 0.018(3) 0.020(3) 0.031(3) C39 0.070(3) 0.055(3) 0.041(2) 0.000(2) 0.017(2) 0.012(2) C40 0.116(4) 0.092(4) 0.062(3) -0.029(3) 0.027(3) -0.013(3) C41 0.062(3) 0.092(4) 0.063(3) 0.005(3) 0.025(2) 0.013(3) C42 0.067(3) 0.030(2) 0.088(3) -0.010(2) 0.035(2) 0.001(2) C43 0.071(3) 0.037(2) 0.087(3) -0.007(2) 0.047(3) 0.000(2) C44 0.050(2) 0.030(2) 0.063(3) 0.0004(19) 0.0305(19) 0.0018(17) C45 0.060(2) 0.047(3) 0.044(2) -0.009(2) 0.0172(19) -0.005(2) C46 0.055(2) 0.040(2) 0.034(2) -0.0033(17) 0.0116(17) -0.0038(18) C47 0.071(3) 0.032(2) 0.075(3) -0.002(2) 0.027(2) -0.015(2) C48 0.0422(19) 0.026(2) 0.0367(19) -0.0013(15) 0.0116(16) 0.0004(15) C49 0.0419(19) 0.024(2) 0.039(2) 0.0007(15) 0.0114(16) 0.0016(15) C50 0.046(2) 0.028(2) 0.041(2) 0.0014(16) 0.0139(17) 0.0065(16) C51 0.051(2) 0.040(2) 0.063(3) 0.004(2) 0.023(2) 0.0089(18) C52 0.045(2) 0.056(3) 0.090(3) 0.008(3) 0.023(2) 0.013(2) C53 0.045(2) 0.063(3) 0.079(3) 0.007(3) 0.003(2) 0.020(2) C54 0.055(2) 0.050(3) 0.055(3) 0.010(2) 0.002(2) 0.021(2) C55 0.046(2) 0.032(2) 0.043(2) -0.0005(17) 0.0075(17) 0.0087(16) C56 0.056(2) 0.036(2) 0.035(2) 0.0048(17) 0.0125(18) 0.0069(18) C57 0.044(2) 0.027(2) 0.040(2) 0.0015(16) 0.0115(16) 0.0002(15) C58 0.060(2) 0.033(2) 0.045(2) 0.0048(18) 0.0167(19) -0.0076(18) C59 0.049(2) 0.037(2) 0.061(3) 0.004(2) 0.019(2) -0.0077(18) C60 0.0345(19) 0.037(2) 0.062(3) -0.002(2) 0.0049(18) -0.0020(16) C61 0.045(2) 0.039(2) 0.041(2) 0.0044(17) 0.0026(17) -0.0007(17) C62 0.0392(18) 0.0252(19) 0.0362(19) 0.0010(15) 0.0068(15) 0.0009(15) F7 0.092(2) 0.109(3) 0.162(3) -0.042(2) 0.015(2) -0.042(2) F8 0.0682(19) 0.121(3) 0.217(4) -0.095(3) 0.033(2) -0.0323(19) P2 0.0525(6) 0.0404(7) 0.0779(8) -0.0115(6) 0.0200(6) 0.0014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 F1 1.553(3) . ? P1 F6 1.567(3) . ? P1 F5 1.581(3) . ? P1 F3 1.584(3) . ? P1 F4 1.586(3) . ? P1 F2 1.589(3) . ? Ru2 N3 2.175(3) . ? Ru2 N4 2.179(3) . ? Ru2 C34 2.184(4) . ? Ru2 C32 2.188(4) . ? Ru2 C35 2.209(3) . ? Ru2 C37 2.214(4) . ? Ru2 C33 2.261(4) . ? Ru2 C36 2.264(3) . ? Ru2 Cl2 2.4185(9) . ? Ru1 N1 2.166(3) . ? Ru1 C1 2.170(4) . ? Ru1 N2 2.178(3) . ? Ru1 C3 2.185(4) . ? Ru1 C6 2.200(3) . ? Ru1 C4 2.210(4) . ? Ru1 C2 2.250(4) . ? Ru1 C5 2.264(3) . ? Ru1 Cl1 2.4153(9) . ? N1 C15 1.496(5) . ? N1 C16 1.497(5) . ? N1 C11 1.500(4) . ? N2 C14 1.504(4) . ? N2 C13 1.509(4) . ? N2 C17 1.524(4) . ? N3 C47 1.483(5) . ? N3 C45 1.491(5) . ? N3 C42 1.503(5) . ? N4 C44 1.495(4) . ? N4 C46 1.503(4) . ? N4 C48 1.521(4) . ? C1 C6 1.401(5) . ? C1 C2 1.416(6) . ? C1 H1 0.9800 . ? C2 C3 1.388(6) . ? C2 C7 1.522(5) . ? C3 C4 1.407(5) . ? C3 H3 0.9800 . ? C4 C5 1.400(5) . ? C4 H4 0.9800 . ? C5 C6 1.413(5) . ? C5 C8 1.516(5) . ? C6 H6 0.9800 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.506(6) . ? C8 C10 1.537(5) . ? C8 H8 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.518(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.522(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.524(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.510(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.417(5) . ? C18 C31 1.419(5) . ? C19 C20 1.426(5) . ? C19 C24 1.437(5) . ? C20 C21 1.350(5) . ? C20 H20 0.9300 . ? C21 C22 1.418(6) . ? C21 H21 0.9300 . ? C22 C23 1.346(5) . ? C22 H22 0.9300 . ? C23 C24 1.432(5) . ? C23 H23 0.9300 . ? C24 C25 1.376(5) . ? C25 C26 1.390(5) . ? C25 H25 0.9300 . ? C26 C31 1.437(5) . ? C26 C27 1.441(5) . ? C27 C28 1.344(6) . ? C27 H27 0.9300 . ? C28 C29 1.412(6) . ? C28 H28 0.9300 . ? C29 C30 1.351(5) . ? C29 H29 0.9300 . ? C30 C31 1.432(5) . ? C30 H30 0.9300 . ? C32 C33 1.393(6) . ? C32 C37 1.394(5) . ? C32 H32 0.9800 . ? C33 C34 1.413(5) . ? C33 C38 1.516(6) . ? C34 C35 1.401(5) . ? C34 H34 0.9800 . ? C35 C36 1.420(5) . ? C35 H35 0.9800 . ? C36 C37 1.411(5) . ? C36 C39 1.504(5) . ? C37 H37 0.9800 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C41 1.520(6) . ? C39 C40 1.535(6) . ? C39 H39 0.9800 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.532(5) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.525(5) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.519(5) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.527(5) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C62 1.410(4) . ? C49 C50 1.417(5) . ? C50 C51 1.428(5) . ? C50 C55 1.431(5) . ? C51 C52 1.349(5) . ? C51 H51 0.9300 . ? C52 C53 1.413(6) . ? C52 H52 0.9300 . ? C53 C54 1.343(6) . ? C53 H53 0.9300 . ? C54 C55 1.434(5) . ? C54 H54 0.9300 . ? C55 C56 1.378(5) . ? C56 C57 1.395(5) . ? C56 H56 0.9300 . ? C57 C58 1.425(5) . ? C57 C62 1.444(5) . ? C58 C59 1.345(5) . ? C58 H58 0.9300 . ? C59 C60 1.396(5) . ? C59 H59 0.9300 . ? C60 C61 1.355(5) . ? C60 H60 0.9300 . ? C61 C62 1.434(5) . ? C61 H61 0.9300 . ? F7 P2 1.559(3) . ? F8 P2 1.550(3) . ? F9 P2 1.596(6) . ? F9A P2 1.564(8) . ? F10 P2 1.542(7) . ? F10A P2 1.580(11) . ? F11 P2 1.579(7) . ? F11A P2 1.594(8) . ? F12 P2 1.574(6) . ? F12A P2 1.603(8) . ? 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 F1 P1 F6 179.6(2) . . ? F1 P1 F5 91.5(2) . . ? F6 P1 F5 88.12(19) . . ? F1 P1 F3 89.38(19) . . ? F6 P1 F3 90.78(19) . . ? F5 P1 F3 90.37(15) . . ? F1 P1 F4 90.15(18) . . ? F6 P1 F4 89.69(18) . . ? F5 P1 F4 89.53(16) . . ? F3 P1 F4 179.5(2) . . ? F1 P1 F2 90.4(2) . . ? F6 P1 F2 90.03(19) . . ? F5 P1 F2 178.1(2) . . ? F3 P1 F2 89.22(15) . . ? F4 P1 F2 90.89(15) . . ? N3 Ru2 N4 73.62(11) . . ? N3 Ru2 C34 96.07(14) . . ? N4 Ru2 C34 144.18(13) . . ? N3 Ru2 C32 131.33(14) . . ? N4 Ru2 C32 94.63(12) . . ? C34 Ru2 C32 66.14(15) . . ? N3 Ru2 C35 115.03(13) . . ? N4 Ru2 C35 171.22(12) . . ? C34 Ru2 C35 37.18(13) . . ? C32 Ru2 C35 78.53(14) . . ? N3 Ru2 C37 168.22(13) . . ? N4 Ru2 C37 104.81(12) . . ? C34 Ru2 C37 78.35(15) . . ? C32 Ru2 C37 36.91(14) . . ? C35 Ru2 C37 66.42(14) . . ? N3 Ru2 C33 103.09(14) . . ? N4 Ru2 C33 110.70(12) . . ? C34 Ru2 C33 37.01(14) . . ? C32 Ru2 C33 36.46(15) . . ? C35 Ru2 C33 66.86(14) . . ? C37 Ru2 C33 66.22(15) . . ? N3 Ru2 C36 149.48(13) . . ? N4 Ru2 C36 135.00(12) . . ? C34 Ru2 C36 66.64(14) . . ? C32 Ru2 C36 66.38(14) . . ? C35 Ru2 C36 37.00(14) . . ? C37 Ru2 C36 36.72(13) . . ? C33 Ru2 C36 78.59(14) . . ? N3 Ru2 Cl2 87.02(8) . . ? N4 Ru2 Cl2 87.10(7) . . ? C34 Ru2 Cl2 127.29(11) . . ? C32 Ru2 Cl2 140.49(12) . . ? C35 Ru2 Cl2 94.68(10) . . ? C37 Ru2 Cl2 104.64(10) . . ? C33 Ru2 Cl2 161.31(11) . . ? C36 Ru2 Cl2 84.75(9) . . ? N1 Ru1 C1 96.36(14) . . ? N1 Ru1 N2 73.51(11) . . ? C1 Ru1 N2 144.16(14) . . ? N1 Ru1 C3 131.63(14) . . ? C1 Ru1 C3 66.40(16) . . ? N2 Ru1 C3 94.35(12) . . ? N1 Ru1 C6 115.41(13) . . ? C1 Ru1 C6 37.39(14) . . ? N2 Ru1 C6 170.97(13) . . ? C3 Ru1 C6 78.69(14) . . ? N1 Ru1 C4 168.95(13) . . ? C1 Ru1 C4 78.54(15) . . ? N2 Ru1 C4 104.85(12) . . ? C3 Ru1 C4 37.33(14) . . ? C6 Ru1 C4 66.13(14) . . ? N1 Ru1 C2 103.47(14) . . ? C1 Ru1 C2 37.31(15) . . ? N2 Ru1 C2 110.39(13) . . ? C3 Ru1 C2 36.45(16) . . ? C6 Ru1 C2 67.21(14) . . ? C4 Ru1 C2 66.53(16) . . ? N1 Ru1 C5 149.56(12) . . ? C1 Ru1 C5 66.81(14) . . ? N2 Ru1 C5 134.85(12) . . ? C3 Ru1 C5 66.57(14) . . ? C6 Ru1 C5 36.87(13) . . ? C4 Ru1 C5 36.44(13) . . ? C2 Ru1 C5 78.86(14) . . ? N1 Ru1 Cl1 86.45(8) . . ? C1 Ru1 Cl1 127.17(12) . . ? N2 Ru1 Cl1 87.19(7) . . ? C3 Ru1 Cl1 140.68(12) . . ? C6 Ru1 Cl1 94.55(10) . . ? C4 Ru1 Cl1 104.46(10) . . ? C2 Ru1 Cl1 161.56(11) . . ? C5 Ru1 Cl1 84.76(9) . . ? C15 N1 C16 108.7(3) . . ? C15 N1 C11 108.1(3) . . ? C16 N1 C11 108.8(3) . . ? C15 N1 Ru1 108.7(2) . . ? C16 N1 Ru1 112.4(2) . . ? C11 N1 Ru1 110.0(2) . . ? C14 N2 C13 107.8(3) . . ? C14 N2 C17 111.4(2) . . ? C13 N2 C17 111.1(2) . . ? C14 N2 Ru1 109.35(19) . . ? C13 N2 Ru1 109.2(2) . . ? C17 N2 Ru1 107.96(18) . . ? C47 N3 C45 109.1(3) . . ? C47 N3 C42 108.4(3) . . ? C45 N3 C42 108.1(3) . . ? C47 N3 Ru2 112.9(2) . . ? C45 N3 Ru2 109.0(2) . . ? C42 N3 Ru2 109.2(2) . . ? C44 N4 C46 107.7(3) . . ? C44 N4 C48 110.6(2) . . ? C46 N4 C48 111.7(3) . . ? C44 N4 Ru2 109.3(2) . . ? C46 N4 Ru2 108.99(19) . . ? C48 N4 Ru2 108.48(19) . . ? C6 C1 C2 122.0(4) . . ? C6 C1 Ru1 72.5(2) . . ? C2 C1 Ru1 74.4(2) . . ? C6 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? Ru1 C1 H1 118.8 . . ? C3 C2 C1 116.5(4) . . ? C3 C2 C7 122.0(4) . . ? C1 C2 C7 121.4(4) . . ? C3 C2 Ru1 69.2(2) . . ? C1 C2 Ru1 68.3(2) . . ? C7 C2 Ru1 136.3(3) . . ? C2 C3 C4 122.2(4) . . ? C2 C3 Ru1 74.3(2) . . ? C4 C3 Ru1 72.3(2) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? Ru1 C3 H3 118.6 . . ? C5 C4 C3 121.0(4) . . ? C5 C4 Ru1 73.9(2) . . ? C3 C4 Ru1 70.4(2) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? Ru1 C4 H4 119.1 . . ? C4 C5 C6 117.6(3) . . ? C4 C5 C8 118.9(3) . . ? C6 C5 C8 123.5(3) . . ? C4 C5 Ru1 69.7(2) . . ? C6 C5 Ru1 69.1(2) . . ? C8 C5 Ru1 131.9(2) . . ? C1 C6 C5 120.4(3) . . ? C1 C6 Ru1 70.1(2) . . ? C5 C6 Ru1 74.0(2) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? Ru1 C6 H6 119.4 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C5 115.8(4) . . ? C9 C8 C10 110.5(4) . . ? C5 C8 C10 108.5(3) . . ? C9 C8 H8 107.2 . . ? C5 C8 H8 107.2 . . ? C10 C8 H8 107.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 113.0(3) . . ? N1 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N1 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C13 118.8(3) . . ? C11 C12 H12A 107.6 . . ? C13 C12 H12A 107.6 . . ? C11 C12 H12B 107.6 . . ? C13 C12 H12B 107.6 . . ? H12A C12 H12B 107.1 . . ? N2 C13 C12 112.8(3) . . ? N2 C13 H13A 109.0 . . ? C12 C13 H13A 109.0 . . ? N2 C13 H13B 109.0 . . ? C12 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? N2 C14 C15 110.2(3) . . ? N2 C14 H14A 109.6 . . ? C15 C14 H14A 109.6 . . ? N2 C14 H14B 109.6 . . ? C15 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? N1 C15 C14 111.8(3) . . ? N1 C15 H15A 109.2 . . ? C14 C15 H15A 109.2 . . ? N1 C15 H15B 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N2 118.2(3) . . ? C18 C17 H17A 107.8 . . ? N2 C17 H17A 107.8 . . ? C18 C17 H17B 107.8 . . ? N2 C17 H17B 107.8 . . ? H17A C17 H17B 107.1 . . ? C19 C18 C31 119.6(3) . . ? C19 C18 C17 120.9(3) . . ? C31 C18 C17 119.4(3) . . ? C18 C19 C20 124.3(3) . . ? C18 C19 C24 118.9(3) . . ? C20 C19 C24 116.8(3) . . ? C21 C20 C19 122.4(4) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C22 120.1(4) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.4(4) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 121.0(4) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 120.7(3) . . ? C25 C24 C19 120.4(3) . . ? C23 C24 C19 118.9(3) . . ? C24 C25 C26 121.6(3) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? C25 C26 C31 119.3(3) . . ? C25 C26 C27 120.7(3) . . ? C31 C26 C27 119.9(3) . . ? C28 C27 C26 120.8(4) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 119.7(4) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 121.7(4) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C29 C30 C31 121.8(4) . . ? C29 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C18 C31 C30 124.3(3) . . ? C18 C31 C26 119.6(3) . . ? C30 C31 C26 116.1(3) . . ? C33 C32 C37 122.6(4) . . ? C33 C32 Ru2 74.6(2) . . ? C37 C32 Ru2 72.6(2) . . ? C33 C32 H32 118.4 . . ? C37 C32 H32 118.4 . . ? Ru2 C32 H32 118.4 . . ? C32 C33 C34 116.5(4) . . ? C32 C33 C38 121.5(4) . . ? C34 C33 C38 122.0(4) . . ? C32 C33 Ru2 68.9(2) . . ? C34 C33 Ru2 68.6(2) . . ? C38 C33 Ru2 136.6(3) . . ? C35 C34 C33 122.2(4) . . ? C35 C34 Ru2 72.4(2) . . ? C33 C34 Ru2 74.4(2) . . ? C35 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? Ru2 C34 H34 118.6 . . ? C34 C35 C36 120.1(3) . . ? C34 C35 Ru2 70.5(2) . . ? C36 C35 Ru2 73.62(19) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? Ru2 C35 H35 119.6 . . ? C37 C36 C35 117.6(3) . . ? C37 C36 C39 118.2(4) . . ? C35 C36 C39 124.2(3) . . ? C37 C36 Ru2 69.7(2) . . ? C35 C36 Ru2 69.4(2) . . ? C39 C36 Ru2 132.4(2) . . ? C32 C37 C36 120.7(4) . . ? C32 C37 Ru2 70.5(2) . . ? C36 C37 Ru2 73.6(2) . . ? C32 C37 H37 119.2 . . ? C36 C37 H37 119.2 . . ? Ru2 C37 H37 119.2 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 C41 115.6(4) . . ? C36 C39 C40 108.3(4) . . ? C41 C39 C40 110.4(4) . . ? C36 C39 H39 107.4 . . ? C41 C39 H39 107.4 . . ? C40 C39 H39 107.4 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 C43 113.0(3) . . ? N3 C42 H42A 109.0 . . ? C43 C42 H42A 109.0 . . ? N3 C42 H42B 109.0 . . ? C43 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? C44 C43 C42 118.3(3) . . ? C44 C43 H43A 107.7 . . ? C42 C43 H43A 107.7 . . ? C44 C43 H43B 107.7 . . ? C42 C43 H43B 107.7 . . ? H43A C43 H43B 107.1 . . ? N4 C44 C43 113.6(3) . . ? N4 C44 H44A 108.8 . . ? C43 C44 H44A 108.8 . . ? N4 C44 H44B 108.8 . . ? C43 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? N3 C45 C46 111.8(3) . . ? N3 C45 H45A 109.3 . . ? C46 C45 H45A 109.3 . . ? N3 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 107.9 . . ? N4 C46 C45 110.9(3) . . ? N4 C46 H46A 109.5 . . ? C45 C46 H46A 109.5 . . ? N4 C46 H46B 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 108.0 . . ? N3 C47 H47A 109.5 . . ? N3 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N3 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N4 C48 C49 116.9(3) . . ? N4 C48 H48A 108.1 . . ? C49 C48 H48A 108.1 . . ? N4 C48 H48B 108.1 . . ? C49 C48 H48B 108.1 . . ? H48A C48 H48B 107.3 . . ? C62 C49 C50 120.0(3) . . ? C62 C49 C48 120.7(3) . . ? C50 C49 C48 119.3(3) . . ? C49 C50 C51 124.2(3) . . ? C49 C50 C55 118.9(3) . . ? C51 C50 C55 116.8(3) . . ? C52 C51 C50 122.0(4) . . ? C52 C51 H51 119.0 . . ? C50 C51 H51 119.0 . . ? C51 C52 C53 120.8(4) . . ? C51 C52 H52 119.6 . . ? C53 C52 H52 119.6 . . ? C54 C53 C52 119.7(4) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C53 C54 C55 121.5(4) . . ? C53 C54 H54 119.3 . . ? C55 C54 H54 119.3 . . ? C56 C55 C50 120.6(3) . . ? C56 C55 C54 120.5(3) . . ? C50 C55 C54 118.9(3) . . ? C55 C56 C57 121.3(3) . . ? C55 C56 H56 119.3 . . ? C57 C56 H56 119.3 . . ? C56 C57 C58 120.8(3) . . ? C56 C57 C62 119.3(3) . . ? C58 C57 C62 119.8(3) . . ? C59 C58 C57 120.9(3) . . ? C59 C58 H58 119.5 . . ? C57 C58 H58 119.5 . . ? C58 C59 C60 119.9(3) . . ? C58 C59 H59 120.0 . . ? C60 C59 H59 120.0 . . ? C61 C60 C59 121.8(3) . . ? C61 C60 H60 119.1 . . ? C59 C60 H60 119.1 . . ? C60 C61 C62 121.3(3) . . ? C60 C61 H61 119.3 . . ? C62 C61 H61 119.3 . . ? C49 C62 C61 124.6(3) . . ? C49 C62 C57 119.4(3) . . ? C61 C62 C57 115.9(3) . . ? F10 P2 F8 92.1(3) . . ? F10 P2 F7 88.8(3) . . ? F8 P2 F7 178.6(2) . . ? F10 P2 F9A 87.9(4) . . ? F8 P2 F9A 87.2(3) . . ? F7 P2 F9A 93.9(3) . . ? F8 P2 F12 91.8(3) . . ? F7 P2 F12 86.8(3) . . ? F8 P2 F11 96.4(3) . . ? F7 P2 F11 83.8(3) . . ? F12 P2 F11 87.8(4) . . ? F10 P2 F10A 93.6(5) . . ? F8 P2 F10A 91.4(4) . . ? F7 P2 F10A 87.5(4) . . ? F9A P2 F10A 178.0(5) . . ? F10 P2 F9 173.8(3) . . ? F8 P2 F9 82.5(3) . . ? F7 P2 F9 96.7(3) . . ? F9A P2 F9 88.9(4) . . ? F10A P2 F9 89.5(5) . . ? F8 P2 F11A 91.1(3) . . ? F7 P2 F11A 90.2(3) . . ? F12 P2 F11A 175.3(4) . . ? F11 P2 F11A 95.5(4) . . ? F8 P2 F12A 88.1(3) . . ? F7 P2 F12A 91.6(3) . . ? F12 P2 F12A 87.5(4) . . ? F11 P2 F12A 173.6(4) . . ? F11A P2 F12A 88.9(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.129 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.075 _database_code_depnum_ccdc_archive 'CCDC 927198' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1ru _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H28 Cl F6 N2 P Ru' _chemical_formula_weight 529.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pna21 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' _cell_length_a 20.6176(2) _cell_length_b 11.03910(10) _cell_length_c 8.79290(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2001.26(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1846 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 26.67 _exptl_crystal_description Blocks _exptl_crystal_colour Orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.055 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7289 _exptl_absorpt_correction_T_max 0.9590 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19175 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_unetI/netI 0.0199 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3925 _reflns_number_gt 3761 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0239P)^2^+1.0021P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(3) _refine_ls_number_reflns 3925 _refine_ls_number_parameters 248 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0222 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_ref 0.0506 _refine_ls_wR_factor_gt 0.0499 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.76712(3) 0.39223(6) -0.07724(11) 0.0449(2) Uani 1 1 d . . . F6 F 0.97571(10) 0.63937(17) -0.0618(4) 0.0675(5) Uani 1 1 d . . . F1 F 0.95337(9) 0.83827(17) -0.0542(4) 0.0680(5) Uani 1 1 d . . . N2 N 0.90239(10) 0.2458(2) -0.0823(3) 0.0339(6) Uani 1 1 d . . . H2 H 0.9085 0.2632 -0.1825 0.041 Uiso 1 1 calc R . . F4 F 0.94372(14) 0.6220(2) 0.1815(3) 0.0880(8) Uani 1 1 d . . . F2 F 1.02084(10) 0.7557(2) 0.1172(3) 0.0747(7) Uani 1 1 d . . . C13 C 0.89040(13) 0.1332(3) 0.2194(4) 0.0420(7) Uani 1 1 d . . . H13A H 0.8705 0.0544 0.2044 0.050 Uiso 1 1 calc R . . H13B H 0.8990 0.1424 0.3273 0.050 Uiso 1 1 calc R . . C11 C 0.95032(11) 0.1509(3) -0.0378(5) 0.0416(7) Uani 1 1 d . . . H11A H 0.9927 0.1724 -0.0773 0.050 Uiso 1 1 calc R . . H11B H 0.9378 0.0741 -0.0827 0.050 Uiso 1 1 calc R . . C12 C 0.95451(14) 0.1368(3) 0.1337(4) 0.0477(8) Uani 1 1 d . . . H12A H 0.9801 0.2034 0.1736 0.057 Uiso 1 1 calc R . . H12B H 0.9779 0.0626 0.1556 0.057 Uiso 1 1 calc R . . N1 N 0.84328(11) 0.2297(2) 0.1706(3) 0.0342(5) Uani 1 1 d . . . C6 C 0.70902(12) 0.1400(3) -0.1532(4) 0.0332(6) Uani 1 1 d . . . H6 H 0.6741 0.1906 -0.1741 0.040 Uiso 1 1 calc R . . C5 C 0.71143(12) 0.0816(2) -0.0131(3) 0.0280(6) Uani 1 1 d . . . C15 C 0.87826(16) 0.3489(3) 0.1583(4) 0.0459(8) Uani 1 1 d . . . H15A H 0.9095 0.3558 0.2402 0.055 Uiso 1 1 calc R . . H15B H 0.8474 0.4147 0.1682 0.055 Uiso 1 1 calc R . . C7 C 0.86417(14) 0.0378(3) -0.3550(4) 0.0469(8) Uani 1 1 d . . . H7A H 0.8476 -0.0060 -0.4409 0.070 Uiso 1 1 calc R . . H7B H 0.9002 -0.0054 -0.3122 0.070 Uiso 1 1 calc R . . H7C H 0.8782 0.1168 -0.3870 0.070 Uiso 1 1 calc R . . C4 C 0.76686(12) 0.0072(2) 0.0147(3) 0.0302(5) Uani 1 1 d . . . H4 H 0.7710 -0.0310 0.1085 0.036 Uiso 1 1 calc R . . C16 C 0.79244(15) 0.2396(4) 0.2885(4) 0.0483(8) Uani 1 1 d . . . H16A H 0.8115 0.2672 0.3819 0.072 Uiso 1 1 calc R . . H16B H 0.7728 0.1618 0.3041 0.072 Uiso 1 1 calc R . . H16C H 0.7600 0.2964 0.2559 0.072 Uiso 1 1 calc R . . C1 C 0.75794(12) 0.1253(3) -0.2656(3) 0.0332(6) Uani 1 1 d . . . H1 H 0.7543 0.1653 -0.3583 0.040 Uiso 1 1 calc R . . C2 C 0.81169(12) 0.0506(3) -0.2370(4) 0.0328(6) Uani 1 1 d . . . F5 F 0.87666(10) 0.7041(3) 0.0097(3) 0.0924(10) Uani 1 1 d . . . C8 C 0.65834(13) 0.0920(3) 0.1056(3) 0.0365(6) Uani 1 1 d . . . H8 H 0.6786 0.0862 0.2061 0.044 Uiso 1 1 calc R . . C14 C 0.91299(15) 0.3590(3) 0.0065(4) 0.0443(7) Uani 1 1 d . . . H14A H 0.8964 0.4279 -0.0498 0.053 Uiso 1 1 calc R . . H14B H 0.9590 0.3711 0.0231 0.053 Uiso 1 1 calc R . . F3 F 0.92076(13) 0.8201(2) 0.1874(3) 0.0790(8) Uani 1 1 d . . . C9 C 0.61196(17) -0.0142(4) 0.0882(5) 0.0638(11) Uani 1 1 d . . . H9A H 0.5917 -0.0108 -0.0100 0.096 Uiso 1 1 calc R . . H9B H 0.5793 -0.0102 0.1659 0.096 Uiso 1 1 calc R . . H9C H 0.6356 -0.0888 0.0977 0.096 Uiso 1 1 calc R . . C10 C 0.62200(19) 0.2120(4) 0.0976(6) 0.0689(12) Uani 1 1 d . . . H10A H 0.6522 0.2776 0.1087 0.103 Uiso 1 1 calc R . . H10B H 0.5905 0.2154 0.1778 0.103 Uiso 1 1 calc R . . H10C H 0.6005 0.2185 0.0011 0.103 Uiso 1 1 calc R . . Ru1 Ru 0.803432(7) 0.184837(14) -0.05350(4) 0.02300(5) Uani 1 1 d . . . C3 C 0.81508(12) -0.0099(2) -0.0950(3) 0.0343(7) Uani 1 1 d . . . H3 H 0.8497 -0.0614 -0.0747 0.041 Uiso 1 1 calc R . . P1 P 0.94851(4) 0.72949(7) 0.06327(10) 0.03807(17) 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 Cl1 0.0515(4) 0.0262(3) 0.0571(6) 0.0057(4) 0.0034(4) 0.0067(3) F6 0.0795(12) 0.0578(10) 0.0651(13) -0.0163(16) 0.0026(16) 0.0135(9) F1 0.0762(12) 0.0561(11) 0.0717(13) 0.0242(16) 0.0182(18) 0.0171(9) N2 0.0313(10) 0.0382(11) 0.0321(17) -0.0024(10) 0.0019(9) -0.0074(9) F4 0.119(2) 0.0633(15) 0.0820(19) 0.0360(14) 0.0170(16) 0.0028(14) F2 0.0502(11) 0.0824(16) 0.0916(19) -0.0087(14) -0.0254(12) -0.0031(11) C13 0.0391(14) 0.0525(18) 0.0344(17) 0.0043(15) -0.0094(13) -0.0009(13) C11 0.0245(10) 0.0507(15) 0.050(2) -0.0055(19) -0.0017(16) -0.0031(10) C12 0.0309(14) 0.059(2) 0.053(2) 0.0034(17) -0.0091(13) 0.0008(14) N1 0.0359(12) 0.0393(13) 0.0275(12) -0.0048(11) -0.0008(10) -0.0023(10) C6 0.0254(12) 0.0406(16) 0.0336(15) -0.0020(13) -0.0049(11) -0.0007(11) C5 0.0238(11) 0.0285(12) 0.0316(18) -0.0027(10) -0.0005(9) -0.0045(9) C15 0.0516(18) 0.0382(16) 0.048(2) -0.0156(15) -0.0036(15) -0.0097(14) C7 0.0404(15) 0.054(2) 0.047(2) -0.0213(16) 0.0113(14) -0.0099(14) C4 0.0310(13) 0.0239(12) 0.0357(14) 0.0052(11) -0.0016(10) -0.0056(10) C16 0.0495(17) 0.060(2) 0.0351(18) -0.0075(16) 0.0051(13) -0.0043(15) C1 0.0338(13) 0.0382(15) 0.0275(14) -0.0012(12) -0.0021(11) -0.0062(11) C2 0.0313(12) 0.0304(14) 0.0367(16) -0.0101(12) 0.0024(11) -0.0069(11) F5 0.0418(11) 0.120(2) 0.115(3) -0.0014(17) -0.0103(12) -0.0157(13) C8 0.0276(12) 0.0451(16) 0.0368(16) -0.0002(13) 0.0058(11) -0.0048(12) C14 0.0432(15) 0.0374(15) 0.0525(19) -0.0042(14) -0.0011(13) -0.0167(13) F3 0.1001(19) 0.0673(15) 0.0698(17) -0.0140(13) 0.0241(14) 0.0180(13) C9 0.0512(19) 0.078(3) 0.062(2) -0.014(2) 0.0212(17) -0.0314(18) C10 0.054(2) 0.076(3) 0.076(3) 0.008(2) 0.028(2) 0.028(2) Ru1 0.02326(8) 0.02144(8) 0.02429(9) 0.00008(12) 0.00007(11) -0.00036(6) C3 0.0296(12) 0.0240(12) 0.049(2) -0.0049(11) -0.0003(11) 0.0008(10) P1 0.0361(4) 0.0364(4) 0.0417(5) 0.0028(3) -0.0002(3) 0.0015(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 Cl1 Ru1 2.4178(6) . ? F6 P1 1.586(3) . ? F1 P1 1.587(3) . ? N2 C14 1.489(4) . ? N2 C11 1.493(4) . ? N2 Ru1 2.163(2) . ? N2 H2 0.9100 . ? F4 P1 1.580(2) . ? F2 P1 1.591(2) . ? C13 N1 1.504(4) . ? C13 C12 1.522(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C11 C12 1.518(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? N1 C16 1.478(4) . ? N1 C15 1.505(4) . ? N1 Ru1 2.192(2) . ? C6 C5 1.392(4) . ? C6 C1 1.421(4) . ? C6 Ru1 2.192(3) . ? C6 H6 0.9300 . ? C5 C4 1.428(4) . ? C5 C8 1.517(4) . ? C5 Ru1 2.241(2) . ? C15 C14 1.519(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C7 C2 1.505(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C4 C3 1.398(4) . ? C4 Ru1 2.185(3) . ? C4 H4 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C1 C2 1.404(4) . ? C1 Ru1 2.188(3) . ? C1 H1 0.9300 . ? C2 C3 1.418(4) . ? C2 Ru1 2.197(3) . ? F5 P1 1.580(2) . ? C8 C9 1.521(4) . ? C8 C10 1.524(4) . ? C8 H8 0.9800 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? F3 P1 1.587(2) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? Ru1 C3 2.194(3) . ? C3 H3 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 N2 C11 110.7(2) . . ? C14 N2 Ru1 109.76(17) . . ? C11 N2 Ru1 112.03(16) . . ? C14 N2 H2 108.1 . . ? C11 N2 H2 108.1 . . ? Ru1 N2 H2 108.1 . . ? N1 C13 C12 113.6(3) . . ? N1 C13 H13A 108.8 . . ? C12 C13 H13A 108.8 . . ? N1 C13 H13B 108.8 . . ? C12 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? N2 C11 C12 111.7(3) . . ? N2 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N2 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C11 C12 C13 116.4(2) . . ? C11 C12 H12A 108.2 . . ? C13 C12 H12A 108.2 . . ? C11 C12 H12B 108.2 . . ? C13 C12 H12B 108.2 . . ? H12A C12 H12B 107.3 . . ? C16 N1 C15 109.0(2) . . ? C16 N1 C13 108.1(2) . . ? C15 N1 C13 109.3(2) . . ? C16 N1 Ru1 112.42(18) . . ? C15 N1 Ru1 108.19(18) . . ? C13 N1 Ru1 109.80(18) . . ? C5 C6 C1 122.5(3) . . ? C5 C6 Ru1 73.67(16) . . ? C1 C6 Ru1 70.94(15) . . ? C5 C6 H6 118.8 . . ? C1 C6 H6 118.8 . . ? Ru1 C6 H6 129.2 . . ? C6 C5 C4 116.5(2) . . ? C6 C5 C8 123.2(2) . . ? C4 C5 C8 120.2(2) . . ? C6 C5 Ru1 69.76(15) . . ? C4 C5 Ru1 69.05(14) . . ? C8 C5 Ru1 132.93(19) . . ? N1 C15 C14 110.7(2) . . ? N1 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C4 C5 121.9(3) . . ? C3 C4 Ru1 71.71(15) . . ? C5 C4 Ru1 73.32(15) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? Ru1 C4 H4 128.2 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C2 C1 C6 120.2(3) . . ? C2 C1 Ru1 71.68(16) . . ? C6 C1 Ru1 71.19(16) . . ? C2 C1 H1 119.9 . . ? C6 C1 H1 119.9 . . ? Ru1 C1 H1 129.7 . . ? C1 C2 C3 118.2(2) . . ? C1 C2 C7 120.0(3) . . ? C3 C2 C7 121.8(3) . . ? C1 C2 Ru1 70.98(16) . . ? C3 C2 Ru1 71.02(16) . . ? C7 C2 Ru1 128.67(19) . . ? C5 C8 C9 109.0(3) . . ? C5 C8 C10 112.9(3) . . ? C9 C8 C10 110.9(3) . . ? C5 C8 H8 108.0 . . ? C9 C8 H8 108.0 . . ? C10 C8 H8 108.0 . . ? N2 C14 C15 109.3(2) . . ? N2 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? N2 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 Ru1 C4 129.56(9) . . ? N2 Ru1 C1 113.44(9) . . ? C4 Ru1 C1 79.43(11) . . ? N2 Ru1 C6 149.43(10) . . ? C4 Ru1 C6 66.47(11) . . ? C1 Ru1 C6 37.87(10) . . ? N2 Ru1 N1 71.43(9) . . ? C4 Ru1 N1 94.89(10) . . ? C1 Ru1 N1 174.09(9) . . ? C6 Ru1 N1 138.04(10) . . ? N2 Ru1 C3 100.50(9) . . ? C4 Ru1 C3 37.24(10) . . ? C1 Ru1 C3 67.10(11) . . ? C6 Ru1 C3 79.01(11) . . ? N1 Ru1 C3 109.26(10) . . ? N2 Ru1 C2 92.91(9) . . ? C4 Ru1 C2 67.86(11) . . ? C1 Ru1 C2 37.34(10) . . ? C6 Ru1 C2 67.84(10) . . ? N1 Ru1 C2 141.59(10) . . ? C3 Ru1 C2 37.68(11) . . ? N2 Ru1 C5 167.16(9) . . ? C4 Ru1 C5 37.62(9) . . ? C1 Ru1 C5 67.64(10) . . ? C6 Ru1 C5 36.57(11) . . ? N1 Ru1 C5 106.84(9) . . ? C3 Ru1 C5 67.70(9) . . ? C2 Ru1 C5 80.73(9) . . ? N2 Ru1 Cl1 89.26(6) . . ? C4 Ru1 Cl1 140.07(7) . . ? C1 Ru1 Cl1 94.47(8) . . ? C6 Ru1 Cl1 84.50(9) . . ? N1 Ru1 Cl1 88.85(7) . . ? C3 Ru1 Cl1 161.35(8) . . ? C2 Ru1 Cl1 126.80(8) . . ? C5 Ru1 Cl1 103.49(7) . . ? C4 C3 C2 120.6(2) . . ? C4 C3 Ru1 71.05(15) . . ? C2 C3 Ru1 71.30(15) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? Ru1 C3 H3 130.7 . . ? F5 P1 F4 90.24(16) . . ? F5 P1 F6 90.75(14) . . ? F4 P1 F6 90.43(15) . . ? F5 P1 F3 88.80(15) . . ? F4 P1 F3 89.90(16) . . ? F6 P1 F3 179.44(17) . . ? F5 P1 F1 89.96(14) . . ? F4 P1 F1 179.48(19) . . ? F6 P1 F1 90.05(16) . . ? F3 P1 F1 89.62(15) . . ? F5 P1 F2 179.78(16) . . ? F4 P1 F2 89.93(15) . . ? F6 P1 F2 89.39(13) . . ? F3 P1 F2 91.06(15) . . ? F1 P1 F2 89.86(13) . . ? 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 C14 N2 C11 C12 48.6(3) . . . . ? Ru1 N2 C11 C12 -74.3(3) . . . . ? N2 C11 C12 C13 44.7(4) . . . . ? N1 C13 C12 C11 -45.8(4) . . . . ? C12 C13 N1 C16 -163.9(3) . . . . ? C12 C13 N1 C15 -45.4(3) . . . . ? C12 C13 N1 Ru1 73.1(3) . . . . ? C1 C6 C5 C4 1.4(4) . . . . ? Ru1 C6 C5 C4 -52.4(2) . . . . ? C1 C6 C5 C8 -177.4(3) . . . . ? Ru1 C6 C5 C8 128.8(3) . . . . ? C1 C6 C5 Ru1 53.8(2) . . . . ? C16 N1 C15 C14 -159.8(3) . . . . ? C13 N1 C15 C14 82.3(3) . . . . ? Ru1 N1 C15 C14 -37.3(3) . . . . ? C6 C5 C4 C3 -2.4(4) . . . . ? C8 C5 C4 C3 176.5(2) . . . . ? Ru1 C5 C4 C3 -55.1(2) . . . . ? C6 C5 C4 Ru1 52.8(2) . . . . ? C8 C5 C4 Ru1 -128.4(2) . . . . ? C5 C6 C1 C2 -0.7(4) . . . . ? Ru1 C6 C1 C2 54.4(2) . . . . ? C5 C6 C1 Ru1 -55.1(2) . . . . ? C6 C1 C2 C3 0.7(4) . . . . ? Ru1 C1 C2 C3 54.9(2) . . . . ? C6 C1 C2 C7 -178.5(3) . . . . ? Ru1 C1 C2 C7 -124.3(2) . . . . ? C6 C1 C2 Ru1 -54.1(2) . . . . ? C6 C5 C8 C9 94.9(3) . . . . ? C4 C5 C8 C9 -83.9(3) . . . . ? Ru1 C5 C8 C9 -172.5(2) . . . . ? C6 C5 C8 C10 -28.8(4) . . . . ? C4 C5 C8 C10 152.4(3) . . . . ? Ru1 C5 C8 C10 63.7(4) . . . . ? C11 N2 C14 C15 -84.3(3) . . . . ? Ru1 N2 C14 C15 39.8(3) . . . . ? N1 C15 C14 N2 -1.0(4) . . . . ? C14 N2 Ru1 C4 -127.8(2) . . . . ? C11 N2 Ru1 C4 -4.3(3) . . . . ? C14 N2 Ru1 C1 136.6(2) . . . . ? C11 N2 Ru1 C1 -100.0(2) . . . . ? C14 N2 Ru1 C6 119.9(2) . . . . ? C11 N2 Ru1 C6 -116.7(3) . . . . ? C14 N2 Ru1 N1 -47.0(2) . . . . ? C11 N2 Ru1 N1 76.4(2) . . . . ? C14 N2 Ru1 C3 -154.0(2) . . . . ? C11 N2 Ru1 C3 -30.5(2) . . . . ? C14 N2 Ru1 C2 168.8(2) . . . . ? C11 N2 Ru1 C2 -67.7(2) . . . . ? C14 N2 Ru1 C5 -131.3(4) . . . . ? C11 N2 Ru1 C5 -7.9(5) . . . . ? C14 N2 Ru1 Cl1 42.02(19) . . . . ? C11 N2 Ru1 Cl1 165.5(2) . . . . ? C3 C4 Ru1 N2 -45.9(2) . . . . ? C5 C4 Ru1 N2 -178.69(14) . . . . ? C3 C4 Ru1 C1 65.88(17) . . . . ? C5 C4 Ru1 C1 -66.93(16) . . . . ? C3 C4 Ru1 C6 103.26(19) . . . . ? C5 C4 Ru1 C6 -29.55(15) . . . . ? C3 C4 Ru1 N1 -115.76(16) . . . . ? C5 C4 Ru1 N1 111.42(16) . . . . ? C5 C4 Ru1 C3 -132.8(2) . . . . ? C3 C4 Ru1 C2 28.75(15) . . . . ? C5 C4 Ru1 C2 -104.06(17) . . . . ? C3 C4 Ru1 C5 132.8(2) . . . . ? C3 C4 Ru1 Cl1 150.18(13) . . . . ? C5 C4 Ru1 Cl1 17.4(2) . . . . ? C2 C1 Ru1 N2 61.50(18) . . . . ? C6 C1 Ru1 N2 -166.24(17) . . . . ? C2 C1 Ru1 C4 -67.21(17) . . . . ? C6 C1 Ru1 C4 65.06(18) . . . . ? C2 C1 Ru1 C6 -132.3(3) . . . . ? C2 C1 Ru1 N1 -83.3(9) . . . . ? C6 C1 Ru1 N1 48.9(10) . . . . ? C2 C1 Ru1 C3 -30.37(16) . . . . ? C6 C1 Ru1 C3 101.90(19) . . . . ? C6 C1 Ru1 C2 132.3(3) . . . . ? C2 C1 Ru1 C5 -104.60(18) . . . . ? C6 C1 Ru1 C5 27.66(16) . . . . ? C2 C1 Ru1 Cl1 152.64(15) . . . . ? C6 C1 Ru1 Cl1 -75.10(17) . . . . ? C5 C6 Ru1 N2 159.31(18) . . . . ? C1 C6 Ru1 N2 25.4(3) . . . . ? C5 C6 Ru1 C4 30.35(15) . . . . ? C1 C6 Ru1 C4 -103.54(19) . . . . ? C5 C6 Ru1 C1 133.9(2) . . . . ? C5 C6 Ru1 N1 -39.4(2) . . . . ? C1 C6 Ru1 N1 -173.33(16) . . . . ? C5 C6 Ru1 C3 67.23(16) . . . . ? C1 C6 Ru1 C3 -66.67(18) . . . . ? C5 C6 Ru1 C2 104.90(18) . . . . ? C1 C6 Ru1 C2 -28.99(17) . . . . ? C1 C6 Ru1 C5 -133.9(2) . . . . ? C5 C6 Ru1 Cl1 -121.55(15) . . . . ? C1 C6 Ru1 Cl1 104.56(17) . . . . ? C16 N1 Ru1 N2 165.7(2) . . . . ? C15 N1 Ru1 N2 45.31(18) . . . . ? C13 N1 Ru1 N2 -73.90(18) . . . . ? C16 N1 Ru1 C4 -64.1(2) . . . . ? C15 N1 Ru1 C4 175.53(19) . . . . ? C13 N1 Ru1 C4 56.31(19) . . . . ? C16 N1 Ru1 C1 -48.2(10) . . . . ? C15 N1 Ru1 C1 -168.6(9) . . . . ? C13 N1 Ru1 C1 72.2(9) . . . . ? C16 N1 Ru1 C6 -4.4(3) . . . . ? C15 N1 Ru1 C6 -124.8(2) . . . . ? C13 N1 Ru1 C6 116.0(2) . . . . ? C16 N1 Ru1 C3 -99.3(2) . . . . ? C15 N1 Ru1 C3 140.26(19) . . . . ? C13 N1 Ru1 C3 21.1(2) . . . . ? C16 N1 Ru1 C2 -124.0(2) . . . . ? C15 N1 Ru1 C2 115.6(2) . . . . ? C13 N1 Ru1 C2 -3.6(3) . . . . ? C16 N1 Ru1 C5 -27.6(2) . . . . ? C15 N1 Ru1 C5 -148.05(19) . . . . ? C13 N1 Ru1 C5 92.74(19) . . . . ? C16 N1 Ru1 Cl1 76.1(2) . . . . ? C15 N1 Ru1 Cl1 -44.30(18) . . . . ? C13 N1 Ru1 Cl1 -163.51(18) . . . . ? C1 C2 Ru1 N2 -126.16(16) . . . . ? C3 C2 Ru1 N2 103.47(15) . . . . ? C7 C2 Ru1 N2 -12.5(3) . . . . ? C1 C2 Ru1 C4 101.93(17) . . . . ? C3 C2 Ru1 C4 -28.44(14) . . . . ? C7 C2 Ru1 C4 -144.4(3) . . . . ? C3 C2 Ru1 C1 -130.4(2) . . . . ? C7 C2 Ru1 C1 113.6(4) . . . . ? C1 C2 Ru1 C6 29.38(16) . . . . ? C3 C2 Ru1 C6 -101.00(17) . . . . ? C7 C2 Ru1 C6 143.0(3) . . . . ? C1 C2 Ru1 N1 170.52(15) . . . . ? C3 C2 Ru1 N1 40.2(2) . . . . ? C7 C2 Ru1 N1 -75.9(3) . . . . ? C1 C2 Ru1 C3 130.4(2) . . . . ? C7 C2 Ru1 C3 -116.0(3) . . . . ? C1 C2 Ru1 C5 65.06(16) . . . . ? C3 C2 Ru1 C5 -65.31(15) . . . . ? C7 C2 Ru1 C5 178.7(3) . . . . ? C1 C2 Ru1 Cl1 -34.91(18) . . . . ? C3 C2 Ru1 Cl1 -165.28(11) . . . . ? C7 C2 Ru1 Cl1 78.7(3) . . . . ? C6 C5 Ru1 N2 -126.1(4) . . . . ? C4 C5 Ru1 N2 4.5(5) . . . . ? C8 C5 Ru1 N2 116.9(4) . . . . ? C6 C5 Ru1 C4 -130.6(2) . . . . ? C8 C5 Ru1 C4 112.3(3) . . . . ? C6 C5 Ru1 C1 -28.58(17) . . . . ? C4 C5 Ru1 C1 102.05(18) . . . . ? C8 C5 Ru1 C1 -145.6(3) . . . . ? C4 C5 Ru1 C6 130.6(2) . . . . ? C8 C5 Ru1 C6 -117.1(3) . . . . ? C6 C5 Ru1 N1 153.66(16) . . . . ? C4 C5 Ru1 N1 -75.71(17) . . . . ? C8 C5 Ru1 N1 36.6(3) . . . . ? C6 C5 Ru1 C3 -101.96(18) . . . . ? C4 C5 Ru1 C3 28.67(16) . . . . ? C8 C5 Ru1 C3 141.0(3) . . . . ? C6 C5 Ru1 C2 -65.07(17) . . . . ? C4 C5 Ru1 C2 65.56(17) . . . . ? C8 C5 Ru1 C2 177.9(3) . . . . ? C6 C5 Ru1 Cl1 60.74(16) . . . . ? C4 C5 Ru1 Cl1 -168.63(15) . . . . ? C8 C5 Ru1 Cl1 -56.3(3) . . . . ? C5 C4 C3 C2 2.5(4) . . . . ? Ru1 C4 C3 C2 -53.3(2) . . . . ? C5 C4 C3 Ru1 55.8(2) . . . . ? C1 C2 C3 C4 -1.6(4) . . . . ? C7 C2 C3 C4 177.6(3) . . . . ? Ru1 C2 C3 C4 53.2(2) . . . . ? C1 C2 C3 Ru1 -54.8(2) . . . . ? C7 C2 C3 Ru1 124.3(3) . . . . ? N2 Ru1 C3 C4 145.75(16) . . . . ? C1 Ru1 C3 C4 -103.10(17) . . . . ? C6 Ru1 C3 C4 -65.37(17) . . . . ? N1 Ru1 C3 C4 71.90(17) . . . . ? C2 Ru1 C3 C4 -133.2(2) . . . . ? C5 Ru1 C3 C4 -28.95(15) . . . . ? Cl1 Ru1 C3 C4 -93.7(3) . . . . ? N2 Ru1 C3 C2 -81.04(15) . . . . ? C4 Ru1 C3 C2 133.2(2) . . . . ? C1 Ru1 C3 C2 30.11(14) . . . . ? C6 Ru1 C3 C2 67.84(15) . . . . ? N1 Ru1 C3 C2 -154.89(14) . . . . ? C5 Ru1 C3 C2 104.26(16) . . . . ? Cl1 Ru1 C3 C2 39.5(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.695 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.047 _database_code_depnum_ccdc_archive 'CCDC 927199' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2ru_aniso _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H76 Cl2 F12 N4 P2 Ru2' _chemical_formula_weight 1440.25 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' Cl Cl 0.1484 0.1585 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8707(2) _cell_length_b 19.8808(2) _cell_length_c 20.3162(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.3170(10) _cell_angle_gamma 90.00 _cell_volume 6285.57(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1765 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 24.68 _exptl_crystal_description plates _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.694 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9465 _exptl_absorpt_correction_T_max 0.9661 _exptl_absorpt_process_details 'BRUKER SADABS' 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 1 0.000 0.000 0.000 19.6 -0.5 2 0.000 0.000 0.500 139.0 21.9 3 0.000 0.500 1.000 139.0 22.7 4 0.000 0.500 0.500 19.6 -0.7 5 0.333 0.667 0.021 6.8 0.0 6 0.333 0.833 0.521 6.8 -0.1 7 0.667 0.167 0.479 6.8 -0.1 8 0.667 0.333 0.979 6.8 -0.1 _platon_squeeze_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63157 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12350 _reflns_number_gt 8768 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0457P)^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 12350 _refine_ls_number_parameters 801 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.87176(5) 0.31362(4) 0.13381(5) 0.0487(2) Uani 1 1 d . . . F1 F 0.92262(19) 0.27836(15) 0.19783(13) 0.1300(10) Uani 1 1 d . . . F2 F 0.92986(12) 0.37884(10) 0.15046(12) 0.0908(7) Uani 1 1 d . . . F3 F 0.80733(13) 0.34361(12) 0.17665(12) 0.0969(8) Uani 1 1 d . . . F4 F 0.93658(13) 0.28334(11) 0.09138(11) 0.0844(7) Uani 1 1 d . . . F5 F 0.81196(16) 0.25031(11) 0.11564(12) 0.1024(8) Uani 1 1 d . . . F6 F 0.82073(16) 0.34871(14) 0.06915(13) 0.1129(9) Uani 1 1 d . . . Ru2 Ru 0.654329(13) 0.082630(11) 0.186336(11) 0.03292(8) Uani 1 1 d . . . Ru1 Ru 0.818102(13) 0.584903(11) 0.219547(11) 0.03194(8) Uani 1 1 d . . . Cl1 Cl 0.68486(4) 0.54577(4) 0.24640(3) 0.04243(18) Uani 1 1 d . . . Cl2 Cl 0.80205(4) 0.04531(4) 0.21489(4) 0.04673(19) Uani 1 1 d . . . N1 N 0.82718(14) 0.65123(12) 0.30524(12) 0.0410(6) Uani 1 1 d . . . N2 N 0.88374(13) 0.52840(11) 0.30650(11) 0.0326(5) Uani 1 1 d . . . N3 N 0.68624(15) 0.15447(12) 0.26806(12) 0.0438(6) Uani 1 1 d . . . N4 N 0.63410(14) 0.03107(11) 0.27661(11) 0.0343(5) Uani 1 1 d . . . C1 C 0.8342(2) 0.66253(16) 0.14768(15) 0.0538(9) Uani 1 1 d . . . H1 H 0.8318 0.7098 0.1608 0.065 Uiso 1 1 calc R . . C2 C 0.9141(2) 0.6283(2) 0.16288(15) 0.0561(9) Uani 1 1 d . . . C3 C 0.91079(19) 0.55852(18) 0.15738(15) 0.0507(8) Uani 1 1 d . . . H3 H 0.9617 0.5324 0.1776 0.061 Uiso 1 1 calc R . . C4 C 0.83420(19) 0.52396(16) 0.13214(13) 0.0425(7) Uani 1 1 d . . . H4 H 0.8333 0.4748 0.1355 0.051 Uiso 1 1 calc R . . C5 C 0.75661(18) 0.55844(15) 0.11253(13) 0.0375(7) Uani 1 1 d . . . C6 C 0.75704(19) 0.62854(15) 0.12236(14) 0.0438(7) Uani 1 1 d . . . H6 H 0.7023 0.6525 0.1185 0.053 Uiso 1 1 calc R . . C7 C 0.9984(2) 0.6665(2) 0.18056(19) 0.0915(14) Uani 1 1 d . . . H7A H 1.0383 0.6414 0.2130 0.137 Uiso 1 1 calc R . . H7B H 0.9883 0.7096 0.1990 0.137 Uiso 1 1 calc R . . H7C H 1.0217 0.6728 0.1408 0.137 Uiso 1 1 calc R . . C8 C 0.6762(2) 0.51851(17) 0.08343(14) 0.0512(8) Uani 1 1 d . . . H8 H 0.6737 0.4802 0.1133 0.061 Uiso 1 1 calc R . . C9 C 0.5923(2) 0.5562(2) 0.07696(17) 0.0731(11) Uani 1 1 d . . . H9A H 0.5892 0.5769 0.1191 0.110 Uiso 1 1 calc R . . H9B H 0.5453 0.5254 0.0646 0.110 Uiso 1 1 calc R . . H9C H 0.5892 0.5903 0.0431 0.110 Uiso 1 1 calc R . . C10 C 0.6861(3) 0.49017(19) 0.01522(16) 0.0733(11) Uani 1 1 d . . . H10A H 0.6380 0.4617 -0.0021 0.110 Uiso 1 1 calc R . . H10B H 0.7383 0.4646 0.0205 0.110 Uiso 1 1 calc R . . H10C H 0.6882 0.5266 -0.0155 0.110 Uiso 1 1 calc R . . C11 C 0.91752(18) 0.67723(14) 0.32578(17) 0.0508(8) Uani 1 1 d . . . H11A H 0.9181 0.7139 0.3574 0.061 Uiso 1 1 calc R . . H11B H 0.9363 0.6950 0.2866 0.061 Uiso 1 1 calc R . . C12 C 0.98046(19) 0.62327(15) 0.35786(17) 0.0544(9) Uani 1 1 d . . . H12A H 1.0381 0.6401 0.3589 0.065 Uiso 1 1 calc R . . H12B H 0.9740 0.6182 0.4041 0.065 Uiso 1 1 calc R . . C13 C 0.97461(16) 0.55365(14) 0.32645(15) 0.0402(7) Uani 1 1 d . . . H13A H 1.0005 0.5548 0.2870 0.048 Uiso 1 1 calc R . . H13B H 1.0073 0.5223 0.3582 0.048 Uiso 1 1 calc R . . C14 C 0.83969(18) 0.54039(14) 0.36454(13) 0.0390(7) Uani 1 1 d . . . H14A H 0.8799 0.5327 0.4064 0.047 Uiso 1 1 calc R . . H14B H 0.7924 0.5090 0.3623 0.047 Uiso 1 1 calc R . . C15 C 0.80573(19) 0.61222(15) 0.36296(14) 0.0433(7) Uani 1 1 d . . . H15A H 0.7439 0.6112 0.3592 0.052 Uiso 1 1 calc R . . H15B H 0.8305 0.6346 0.4047 0.052 Uiso 1 1 calc R . . C16 C 0.7675(2) 0.71000(15) 0.29135(17) 0.0571(9) Uani 1 1 d . . . H16A H 0.7106 0.6943 0.2728 0.086 Uiso 1 1 calc R . . H16B H 0.7866 0.7396 0.2599 0.086 Uiso 1 1 calc R . . H16C H 0.7670 0.7338 0.3324 0.086 Uiso 1 1 calc R . . C17 C 0.88176(17) 0.45426(13) 0.28702(13) 0.0326(6) Uani 1 1 d . . . H17A H 0.8245 0.4441 0.2621 0.039 Uiso 1 1 calc R . . H17B H 0.9211 0.4480 0.2566 0.039 Uiso 1 1 calc R . . C18 C 0.90390(17) 0.40288(13) 0.34262(13) 0.0327(6) Uani 1 1 d . . . C19 C 0.98977(17) 0.38109(13) 0.36502(13) 0.0352(7) Uani 1 1 d . . . C20 C 1.05943(18) 0.39924(15) 0.33342(15) 0.0444(7) Uani 1 1 d . . . H20 H 1.0487 0.4271 0.2959 0.053 Uiso 1 1 calc R . . C21 C 1.14045(19) 0.37712(15) 0.35643(17) 0.0519(8) Uani 1 1 d . . . H21 H 1.1839 0.3885 0.3338 0.062 Uiso 1 1 calc R . . C22 C 1.1594(2) 0.33672(16) 0.41474(18) 0.0556(9) Uani 1 1 d . . . H22 H 1.2158 0.3238 0.4317 0.067 Uiso 1 1 calc R . . C23 C 1.0963(2) 0.31688(16) 0.44584(16) 0.0534(8) Uani 1 1 d . . . H23 H 1.1096 0.2905 0.4843 0.064 Uiso 1 1 calc R . . C24 C 1.00876(18) 0.33577(15) 0.42066(14) 0.0416(7) Uani 1 1 d . . . C25 C 0.94340(19) 0.30920(15) 0.44830(14) 0.0453(8) Uani 1 1 d . . . H25 H 0.9569 0.2801 0.4847 0.054 Uiso 1 1 calc R . . C26 C 0.85767(19) 0.32485(14) 0.42305(14) 0.0412(7) Uani 1 1 d . . . C27 C 0.7904(2) 0.29265(16) 0.44954(15) 0.0527(8) Uani 1 1 d . . . H27 H 0.8043 0.2614 0.4841 0.063 Uiso 1 1 calc R . . C28 C 0.7071(2) 0.30736(18) 0.42473(17) 0.0608(10) Uani 1 1 d . . . H28 H 0.6638 0.2864 0.4421 0.073 Uiso 1 1 calc R . . C29 C 0.6863(2) 0.35456(17) 0.37249(16) 0.0538(9) Uani 1 1 d . . . H29 H 0.6288 0.3645 0.3557 0.065 Uiso 1 1 calc R . . C30 C 0.74758(17) 0.38586(15) 0.34598(15) 0.0431(7) Uani 1 1 d . . . H30 H 0.7312 0.4167 0.3114 0.052 Uiso 1 1 calc R . . C31 C 0.83702(17) 0.37278(13) 0.36978(13) 0.0350(7) Uani 1 1 d . . . C32 C 0.53047(19) 0.05248(17) 0.12592(15) 0.0513(8) Uani 1 1 d . . . H32 H 0.4902 0.0278 0.1479 0.062 Uiso 1 1 calc R . . C33 C 0.52876(19) 0.12242(18) 0.12711(17) 0.0560(9) Uani 1 1 d . . . C34 C 0.5998(2) 0.15602(16) 0.10978(15) 0.0516(8) Uani 1 1 d . . . H34 H 0.6077 0.2040 0.1202 0.062 Uiso 1 1 calc R . . C35 C 0.66510(18) 0.12136(15) 0.08657(14) 0.0428(7) Uani 1 1 d . . . H35 H 0.7172 0.1455 0.0812 0.051 Uiso 1 1 calc R . . C36 C 0.66226(18) 0.05028(15) 0.08097(13) 0.0404(7) Uani 1 1 d . . . C37 C 0.59442(19) 0.01612(16) 0.10257(14) 0.0444(8) Uani 1 1 d . . . H37 H 0.5976 -0.0328 0.1086 0.053 Uiso 1 1 calc R . . C38 C 0.4522(2) 0.1608(2) 0.1426(2) 0.0878(13) Uani 1 1 d . . . H38A H 0.4090 0.1649 0.1025 0.132 Uiso 1 1 calc R . . H38B H 0.4703 0.2048 0.1591 0.132 Uiso 1 1 calc R . . H38C H 0.4290 0.1369 0.1761 0.132 Uiso 1 1 calc R . . C39 C 0.7267(2) 0.00898(17) 0.05364(15) 0.0535(8) Uani 1 1 d . . . H39 H 0.7448 -0.0278 0.0854 0.064 Uiso 1 1 calc R . . C40 C 0.6809(3) -0.0230(2) -0.01302(18) 0.0904(13) Uani 1 1 d . . . H40A H 0.6300 -0.0458 -0.0062 0.136 Uiso 1 1 calc R . . H40B H 0.7188 -0.0547 -0.0280 0.136 Uiso 1 1 calc R . . H40C H 0.6656 0.0115 -0.0463 0.136 Uiso 1 1 calc R . . C41 C 0.8074(2) 0.0460(2) 0.04437(18) 0.0713(11) Uani 1 1 d . . . H41A H 0.7925 0.0795 0.0100 0.107 Uiso 1 1 calc R . . H41B H 0.8471 0.0146 0.0315 0.107 Uiso 1 1 calc R . . H41C H 0.8334 0.0674 0.0858 0.107 Uiso 1 1 calc R . . C42 C 0.6049(2) 0.18050(15) 0.28628(18) 0.0589(9) Uani 1 1 d . . . H42A H 0.5662 0.1950 0.2458 0.071 Uiso 1 1 calc R . . H42B H 0.6184 0.2194 0.3153 0.071 Uiso 1 1 calc R . . C43 C 0.5594(2) 0.12797(15) 0.32193(18) 0.0602(9) Uani 1 1 d . . . H43A H 0.5887 0.1263 0.3685 0.072 Uiso 1 1 calc R . . H43B H 0.5015 0.1439 0.3214 0.072 Uiso 1 1 calc R . . C44 C 0.55293(18) 0.05608(14) 0.29485(16) 0.0443(8) Uani 1 1 d . . . H44A H 0.5374 0.0264 0.3285 0.053 Uiso 1 1 calc R . . H44B H 0.5072 0.0540 0.2554 0.053 Uiso 1 1 calc R . . C45 C 0.7371(2) 0.11976(15) 0.32789(15) 0.0488(8) Uani 1 1 d . . . H45A H 0.7317 0.1444 0.3681 0.059 Uiso 1 1 calc R . . H45B H 0.7973 0.1196 0.3247 0.059 Uiso 1 1 calc R . . C46 C 0.70701(18) 0.04761(14) 0.33359(14) 0.0419(7) Uani 1 1 d . . . H46A H 0.7544 0.0170 0.3329 0.050 Uiso 1 1 calc R . . H46B H 0.6884 0.0418 0.3759 0.050 Uiso 1 1 calc R . . C47 C 0.7366(2) 0.21265(15) 0.25081(17) 0.0575(9) Uani 1 1 d . . . H47A H 0.7543 0.2403 0.2898 0.086 Uiso 1 1 calc R . . H47B H 0.7017 0.2387 0.2160 0.086 Uiso 1 1 calc R . . H47C H 0.7865 0.1966 0.2355 0.086 Uiso 1 1 calc R . . C48 C 0.62838(17) -0.04427(13) 0.26262(13) 0.0341(6) Uani 1 1 d . . . H48A H 0.5748 -0.0530 0.2316 0.041 Uiso 1 1 calc R . . H48B H 0.6747 -0.0564 0.2401 0.041 Uiso 1 1 calc R . . C49 C 0.63273(17) -0.09048(13) 0.32282(13) 0.0342(6) Uani 1 1 d . . . C50 C 0.71345(17) -0.11471(14) 0.35700(14) 0.0371(7) Uani 1 1 d . . . C51 C 0.79230(19) -0.10441(15) 0.33446(17) 0.0497(8) Uani 1 1 d . . . H51 H 0.7914 -0.0816 0.2944 0.060 Uiso 1 1 calc R . . C52 C 0.8683(2) -0.12699(17) 0.36987(19) 0.0628(10) Uani 1 1 d . . . H52 H 0.9182 -0.1205 0.3531 0.075 Uiso 1 1 calc R . . C53 C 0.8728(2) -0.16014(18) 0.43177(19) 0.0642(10) Uani 1 1 d . . . H53 H 0.9258 -0.1725 0.4572 0.077 Uiso 1 1 calc R . . C54 C 0.8000(2) -0.17389(16) 0.45412(16) 0.0539(9) Uani 1 1 d . . . H54 H 0.8033 -0.1973 0.4942 0.065 Uiso 1 1 calc R . . C55 C 0.71794(18) -0.15308(14) 0.41743(14) 0.0400(7) Uani 1 1 d . . . C56 C 0.64383(19) -0.16986(14) 0.43939(14) 0.0418(7) Uani 1 1 d . . . H56 H 0.6478 -0.1942 0.4790 0.050 Uiso 1 1 calc R . . C57 C 0.56318(17) -0.15118(14) 0.40373(14) 0.0359(7) Uani 1 1 d . . . C58 C 0.4869(2) -0.17085(14) 0.42595(15) 0.0452(8) Uani 1 1 d . . . H58 H 0.4912 -0.1951 0.4656 0.054 Uiso 1 1 calc R . . C59 C 0.4088(2) -0.15483(15) 0.39024(16) 0.0476(8) Uani 1 1 d . . . H59 H 0.3596 -0.1672 0.4058 0.057 Uiso 1 1 calc R . . C60 C 0.40144(18) -0.11969(15) 0.32983(15) 0.0454(8) Uani 1 1 d . . . H60 H 0.3471 -0.1109 0.3045 0.055 Uiso 1 1 calc R . . C61 C 0.47182(18) -0.09815(14) 0.30740(15) 0.0411(7) Uani 1 1 d . . . H61 H 0.4646 -0.0742 0.2673 0.049 Uiso 1 1 calc R . . C62 C 0.55681(17) -0.11130(13) 0.34376(13) 0.0333(6) Uani 1 1 d . . . F7 F 0.49790(15) 0.75693(14) 0.08399(15) 0.1226(10) Uani 1 1 d . A . F8 F 0.65194(15) 0.84870(15) 0.14526(17) 0.1361(12) Uani 1 1 d . A . F9 F 0.5163(5) 0.8672(3) 0.1116(12) 0.148(6) Uani 0.50 1 d P A 1 F9A F 0.5989(8) 0.8223(12) 0.0463(5) 0.194(6) Uani 0.50 1 d P A 1 F10 F 0.6312(7) 0.7447(5) 0.1172(12) 0.204(7) Uani 0.50 1 d P A 1 F10A F 0.5515(12) 0.7842(9) 0.1781(5) 0.182(6) Uani 0.50 1 d P A 1 F11 F 0.5379(11) 0.8483(5) 0.0576(6) 0.171(5) Uani 0.50 1 d P A 2 F11A F 0.6320(6) 0.7661(6) 0.0707(7) 0.125(5) Uani 0.50 1 d P A 2 F12 F 0.5271(5) 0.8313(10) 0.1657(8) 0.164(8) Uani 0.50 1 d P A 2 F12A F 0.6148(8) 0.7475(6) 0.1681(6) 0.148(4) Uani 0.50 1 d P A 2 P2 P 0.57553(6) 0.80285(5) 0.11396(5) 0.0575(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0453(5) 0.0397(5) 0.0628(6) -0.0096(4) 0.0148(4) -0.0003(4) F1 0.162(3) 0.133(2) 0.0819(18) 0.0145(17) -0.0075(17) 0.056(2) F2 0.0613(12) 0.0660(15) 0.154(2) -0.0441(14) 0.0420(13) -0.0216(11) F3 0.0710(14) 0.0967(18) 0.136(2) -0.0560(16) 0.0528(13) -0.0153(12) F4 0.0792(14) 0.0784(15) 0.1065(17) -0.0308(13) 0.0446(13) 0.0041(11) F5 0.132(2) 0.0737(16) 0.1156(19) -0.0405(14) 0.0586(16) -0.0540(14) F6 0.1094(19) 0.109(2) 0.1074(19) 0.0235(16) -0.0108(15) 0.0218(16) Ru2 0.03423(13) 0.02503(14) 0.04118(15) 0.00438(10) 0.01150(10) 0.00076(9) Ru1 0.03208(13) 0.02731(14) 0.03616(14) 0.00435(10) 0.00603(10) 0.00048(9) Cl1 0.0349(4) 0.0491(5) 0.0428(4) 0.0012(3) 0.0065(3) -0.0048(3) Cl2 0.0384(4) 0.0559(5) 0.0471(5) 0.0005(4) 0.0114(3) 0.0073(3) N1 0.0395(13) 0.0296(14) 0.0526(16) -0.0025(12) 0.0052(12) 0.0004(11) N2 0.0341(12) 0.0275(14) 0.0348(13) 0.0020(10) 0.0035(10) -0.0022(10) N3 0.0508(15) 0.0295(14) 0.0549(16) -0.0049(12) 0.0196(13) -0.0041(11) N4 0.0393(13) 0.0268(14) 0.0403(14) 0.0015(11) 0.0160(11) 0.0013(10) C1 0.082(3) 0.036(2) 0.0449(19) 0.0117(15) 0.0156(18) -0.0098(18) C2 0.052(2) 0.071(3) 0.047(2) 0.0147(18) 0.0142(16) -0.0122(18) C3 0.0421(18) 0.069(3) 0.0435(19) 0.0169(17) 0.0147(15) 0.0162(17) C4 0.0524(19) 0.043(2) 0.0346(17) 0.0062(14) 0.0155(14) 0.0092(15) C5 0.0511(18) 0.0348(18) 0.0272(15) 0.0053(13) 0.0095(13) 0.0007(14) C6 0.0501(18) 0.042(2) 0.0395(18) 0.0140(15) 0.0100(14) 0.0086(15) C7 0.068(3) 0.124(4) 0.083(3) 0.017(3) 0.016(2) -0.044(2) C8 0.061(2) 0.056(2) 0.0345(18) 0.0001(15) 0.0045(15) -0.0160(17) C9 0.050(2) 0.113(3) 0.054(2) 0.003(2) 0.0030(17) -0.012(2) C10 0.101(3) 0.069(3) 0.047(2) -0.0107(19) 0.008(2) -0.015(2) C11 0.0458(18) 0.0300(18) 0.073(2) -0.0106(16) 0.0015(16) -0.0078(14) C12 0.0456(18) 0.039(2) 0.073(2) -0.0037(17) -0.0027(16) -0.0089(15) C13 0.0302(15) 0.0358(18) 0.0507(18) 0.0044(15) -0.0016(13) -0.0006(13) C14 0.0451(16) 0.0393(19) 0.0320(16) -0.0005(13) 0.0060(13) -0.0020(13) C15 0.0513(18) 0.0401(19) 0.0386(17) -0.0074(14) 0.0086(14) 0.0016(14) C16 0.061(2) 0.0339(19) 0.075(2) -0.0028(17) 0.0104(18) 0.0136(16) C17 0.0397(15) 0.0234(16) 0.0340(15) -0.0016(12) 0.0054(12) -0.0004(12) C18 0.0384(15) 0.0274(16) 0.0312(15) 0.0011(12) 0.0042(12) -0.0001(12) C19 0.0448(16) 0.0243(16) 0.0356(16) -0.0025(13) 0.0054(13) 0.0014(13) C20 0.0437(17) 0.0379(19) 0.0530(19) 0.0064(15) 0.0128(15) 0.0030(14) C21 0.0452(18) 0.040(2) 0.073(2) -0.0037(18) 0.0183(17) 0.0040(15) C22 0.0391(18) 0.044(2) 0.079(3) -0.0050(19) -0.0005(17) 0.0093(15) C23 0.058(2) 0.045(2) 0.052(2) 0.0072(16) -0.0011(17) 0.0132(16) C24 0.0457(17) 0.0333(18) 0.0438(18) 0.0026(14) 0.0039(14) 0.0044(14) C25 0.059(2) 0.0366(19) 0.0399(18) 0.0119(14) 0.0087(15) 0.0071(15) C26 0.0519(18) 0.0318(18) 0.0413(17) 0.0008(14) 0.0122(15) -0.0036(14) C27 0.069(2) 0.045(2) 0.0472(19) 0.0069(16) 0.0196(17) -0.0111(17) C28 0.063(2) 0.061(3) 0.063(2) -0.009(2) 0.0242(19) -0.0251(19) C29 0.0465(18) 0.053(2) 0.060(2) -0.0084(18) 0.0078(17) -0.0087(16) C30 0.0410(17) 0.0394(19) 0.0477(18) -0.0018(15) 0.0056(14) -0.0066(14) C31 0.0425(16) 0.0270(17) 0.0338(16) -0.0030(13) 0.0032(13) -0.0021(13) C32 0.0433(18) 0.057(2) 0.051(2) 0.0174(17) 0.0019(15) -0.0089(16) C33 0.0427(18) 0.059(2) 0.066(2) 0.0231(18) 0.0099(16) 0.0127(16) C34 0.058(2) 0.040(2) 0.055(2) 0.0169(16) 0.0091(17) 0.0062(16) C35 0.0471(17) 0.041(2) 0.0415(18) 0.0149(15) 0.0108(14) -0.0032(14) C36 0.0476(17) 0.040(2) 0.0302(16) 0.0058(14) 0.0000(13) 0.0024(14) C37 0.0517(18) 0.0388(19) 0.0371(17) 0.0116(14) -0.0050(15) -0.0086(15) C38 0.056(2) 0.102(3) 0.107(3) 0.018(3) 0.020(2) 0.033(2) C39 0.070(2) 0.054(2) 0.0386(18) 0.0012(16) 0.0166(16) 0.0127(17) C40 0.120(4) 0.094(3) 0.060(3) -0.027(2) 0.024(2) -0.009(3) C41 0.063(2) 0.091(3) 0.065(2) 0.005(2) 0.0263(19) 0.013(2) C42 0.068(2) 0.0301(19) 0.087(3) -0.0105(18) 0.0362(19) 0.0006(16) C43 0.070(2) 0.037(2) 0.087(3) -0.0066(18) 0.047(2) 0.0014(16) C44 0.0491(17) 0.0298(17) 0.062(2) 0.0009(15) 0.0292(16) 0.0017(14) C45 0.0595(19) 0.045(2) 0.0437(19) -0.0100(16) 0.0156(16) -0.0065(16) C46 0.0540(18) 0.0381(19) 0.0351(17) -0.0029(14) 0.0125(14) -0.0031(14) C47 0.071(2) 0.0311(19) 0.076(2) -0.0022(17) 0.0280(19) -0.0152(16) C48 0.0420(16) 0.0257(17) 0.0365(16) -0.0021(13) 0.0125(13) 0.0001(12) C49 0.0416(16) 0.0241(16) 0.0380(16) 0.0003(13) 0.0105(13) 0.0017(12) C50 0.0453(16) 0.0263(16) 0.0417(17) 0.0012(13) 0.0135(14) 0.0055(13) C51 0.0513(19) 0.0397(19) 0.063(2) 0.0059(16) 0.0230(17) 0.0102(15) C52 0.0440(19) 0.056(2) 0.093(3) 0.009(2) 0.0241(19) 0.0134(17) C53 0.0436(19) 0.066(3) 0.079(3) 0.008(2) 0.0010(19) 0.0207(17) C54 0.055(2) 0.050(2) 0.053(2) 0.0085(16) 0.0033(17) 0.0218(16) C55 0.0458(17) 0.0301(17) 0.0428(18) -0.0004(14) 0.0060(14) 0.0100(13) C56 0.0553(19) 0.0378(19) 0.0335(16) 0.0049(14) 0.0118(14) 0.0061(15) C57 0.0432(16) 0.0274(17) 0.0383(16) -0.0002(13) 0.0107(13) -0.0005(13) C58 0.059(2) 0.0317(18) 0.0467(19) 0.0062(14) 0.0163(16) -0.0061(15) C59 0.0490(19) 0.0354(19) 0.062(2) 0.0025(16) 0.0210(17) -0.0074(15) C60 0.0365(16) 0.0355(19) 0.062(2) -0.0014(16) 0.0034(15) -0.0021(13) C61 0.0450(17) 0.0352(18) 0.0411(17) 0.0054(14) 0.0033(14) -0.0006(13) C62 0.0397(15) 0.0241(15) 0.0360(16) -0.0003(13) 0.0070(13) -0.0002(12) F7 0.0940(18) 0.113(2) 0.158(3) -0.0452(19) 0.0179(17) -0.0425(16) F8 0.0707(15) 0.124(2) 0.217(3) -0.097(2) 0.0365(18) -0.0328(15) F9 0.063(4) 0.038(3) 0.345(19) 0.002(6) 0.047(8) 0.003(2) F9A 0.152(10) 0.323(19) 0.119(6) 0.064(10) 0.058(7) -0.029(10) F10 0.194(9) 0.097(6) 0.34(2) 0.022(11) 0.088(13) 0.112(6) F10A 0.218(15) 0.222(16) 0.133(7) 0.008(9) 0.098(9) -0.064(10) F11 0.216(13) 0.126(7) 0.141(9) 0.070(6) -0.038(8) 0.019(9) F11A 0.102(5) 0.136(9) 0.151(8) -0.105(8) 0.063(6) -0.033(6) F12 0.064(4) 0.250(17) 0.188(12) -0.164(13) 0.046(6) 0.000(8) F12A 0.129(7) 0.185(10) 0.113(7) 0.056(7) -0.023(6) 0.019(7) P2 0.0517(5) 0.0426(6) 0.0805(7) -0.0146(5) 0.0188(5) -0.0020(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 P1 F1 1.556(2) . ? P1 F6 1.566(2) . ? P1 F5 1.576(2) . ? P1 F3 1.584(2) . ? P1 F4 1.5848(19) . ? P1 F2 1.589(2) . ? Ru2 N3 2.173(2) . ? Ru2 N4 2.179(2) . ? Ru2 C34 2.184(3) . ? Ru2 C32 2.187(3) . ? Ru2 C35 2.206(3) . ? Ru2 C37 2.217(3) . ? Ru2 C33 2.259(3) . ? Ru2 C36 2.262(3) . ? Ru2 Cl2 2.4185(7) . ? Ru1 N1 2.166(2) . ? Ru1 C1 2.174(3) . ? Ru1 N2 2.178(2) . ? Ru1 C3 2.183(3) . ? Ru1 C6 2.200(3) . ? Ru1 C4 2.206(3) . ? Ru1 C2 2.254(3) . ? Ru1 C5 2.263(3) . ? Ru1 Cl1 2.4140(7) . ? N1 C16 1.496(4) . ? N1 C15 1.500(3) . ? N1 C11 1.504(3) . ? N2 C14 1.503(3) . ? N2 C13 1.505(3) . ? N2 C17 1.525(3) . ? N3 C47 1.487(3) . ? N3 C45 1.490(4) . ? N3 C42 1.503(4) . ? N4 C44 1.494(3) . ? N4 C46 1.504(3) . ? N4 C48 1.524(3) . ? C1 C6 1.405(4) . ? C1 C2 1.419(4) . ? C1 H1 0.9800 . ? C2 C3 1.391(5) . ? C2 C7 1.519(4) . ? C3 C4 1.403(4) . ? C3 H3 0.9800 . ? C4 C5 1.397(4) . ? C4 H4 0.9800 . ? C5 C6 1.408(4) . ? C5 C8 1.521(4) . ? C6 H6 0.9800 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.510(4) . ? C8 C10 1.532(4) . ? C8 H8 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.523(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.519(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.524(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.512(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.417(4) . ? C18 C31 1.421(4) . ? C19 C20 1.429(4) . ? C19 C24 1.431(4) . ? C20 C21 1.353(4) . ? C20 H20 0.9300 . ? C21 C22 1.414(4) . ? C21 H21 0.9300 . ? C22 C23 1.344(4) . ? C22 H22 0.9300 . ? C23 C24 1.433(4) . ? C23 H23 0.9300 . ? C24 C25 1.378(4) . ? C25 C26 1.392(4) . ? C25 H25 0.9300 . ? C26 C31 1.431(4) . ? C26 C27 1.437(4) . ? C27 C28 1.351(4) . ? C27 H27 0.9300 . ? C28 C29 1.407(4) . ? C28 H28 0.9300 . ? C29 C30 1.353(4) . ? C29 H29 0.9300 . ? C30 C31 1.431(4) . ? C30 H30 0.9300 . ? C32 C33 1.391(4) . ? C32 C37 1.402(4) . ? C32 H32 0.9800 . ? C33 C34 1.413(4) . ? C33 C38 1.518(4) . ? C34 C35 1.401(4) . ? C34 H34 0.9800 . ? C35 C36 1.418(4) . ? C35 H35 0.9800 . ? C36 C37 1.414(4) . ? C36 C39 1.501(4) . ? C37 H37 0.9800 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C41 1.520(4) . ? C39 C40 1.543(4) . ? C39 H39 0.9800 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.531(4) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.528(4) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.523(4) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.520(4) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C62 1.416(4) . ? C49 C50 1.416(4) . ? C50 C51 1.429(4) . ? C50 C55 1.435(4) . ? C51 C52 1.354(4) . ? C51 H51 0.9300 . ? C52 C53 1.409(5) . ? C52 H52 0.9300 . ? C53 C54 1.349(4) . ? C53 H53 0.9300 . ? C54 C55 1.429(4) . ? C54 H54 0.9300 . ? C55 C56 1.378(4) . ? C56 C57 1.392(4) . ? C56 H56 0.9300 . ? C57 C58 1.428(4) . ? C57 C62 1.440(4) . ? C58 C59 1.346(4) . ? C58 H58 0.9300 . ? C59 C60 1.397(4) . ? C59 H59 0.9300 . ? C60 C61 1.356(4) . ? C60 H60 0.9300 . ? C61 C62 1.429(4) . ? C61 H61 0.9300 . ? F7 P2 1.558(2) . ? F8 P2 1.550(2) . ? F9 P2 1.582(6) . ? F9A P2 1.542(9) . ? F10 P2 1.448(7) . ? F10A P2 1.475(9) . ? F11 P2 1.490(7) . ? F11A P2 1.555(7) . ? F12 P2 1.526(7) . ? F12A P2 1.593(8) . ? 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 F1 P1 F6 179.65(17) . . ? F1 P1 F5 91.48(16) . . ? F6 P1 F5 88.32(15) . . ? F1 P1 F3 89.73(15) . . ? F6 P1 F3 90.56(15) . . ? F5 P1 F3 90.30(12) . . ? F1 P1 F4 89.89(14) . . ? F6 P1 F4 89.83(14) . . ? F5 P1 F4 89.69(12) . . ? F3 P1 F4 179.61(16) . . ? F1 P1 F2 90.32(15) . . ? F6 P1 F2 89.88(15) . . ? F5 P1 F2 178.14(15) . . ? F3 P1 F2 89.20(11) . . ? F4 P1 F2 90.82(11) . . ? N3 Ru2 N4 73.55(9) . . ? N3 Ru2 C34 96.05(11) . . ? N4 Ru2 C34 144.14(10) . . ? N3 Ru2 C32 131.14(11) . . ? N4 Ru2 C32 94.51(10) . . ? C34 Ru2 C32 66.20(12) . . ? N3 Ru2 C35 115.09(10) . . ? N4 Ru2 C35 171.22(10) . . ? C34 Ru2 C35 37.23(10) . . ? C32 Ru2 C35 78.66(11) . . ? N3 Ru2 C37 168.27(10) . . ? N4 Ru2 C37 104.70(9) . . ? C34 Ru2 C37 78.55(12) . . ? C32 Ru2 C37 37.13(11) . . ? C35 Ru2 C37 66.53(11) . . ? N3 Ru2 C33 103.05(11) . . ? N4 Ru2 C33 110.65(10) . . ? C34 Ru2 C33 37.04(11) . . ? C32 Ru2 C33 36.42(12) . . ? C35 Ru2 C33 66.91(11) . . ? C37 Ru2 C33 66.38(12) . . ? N3 Ru2 C36 149.53(10) . . ? N4 Ru2 C36 135.03(10) . . ? C34 Ru2 C36 66.67(11) . . ? C32 Ru2 C36 66.54(11) . . ? C35 Ru2 C36 36.98(11) . . ? C37 Ru2 C36 36.78(10) . . ? C33 Ru2 C36 78.62(11) . . ? N3 Ru2 Cl2 87.06(6) . . ? N4 Ru2 Cl2 87.13(6) . . ? C34 Ru2 Cl2 127.29(8) . . ? C32 Ru2 Cl2 140.60(10) . . ? C35 Ru2 Cl2 94.65(8) . . ? C37 Ru2 Cl2 104.52(8) . . ? C33 Ru2 Cl2 161.33(8) . . ? C36 Ru2 Cl2 84.74(7) . . ? N1 Ru1 C1 96.29(11) . . ? N1 Ru1 N2 73.52(8) . . ? C1 Ru1 N2 144.11(11) . . ? N1 Ru1 C3 131.71(11) . . ? C1 Ru1 C3 66.45(12) . . ? N2 Ru1 C3 94.36(10) . . ? N1 Ru1 C6 115.43(10) . . ? C1 Ru1 C6 37.48(11) . . ? N2 Ru1 C6 170.95(10) . . ? C3 Ru1 C6 78.68(11) . . ? N1 Ru1 C4 168.98(10) . . ? C1 Ru1 C4 78.56(12) . . ? N2 Ru1 C4 104.90(9) . . ? C3 Ru1 C4 37.28(11) . . ? C6 Ru1 C4 66.06(11) . . ? N1 Ru1 C2 103.46(11) . . ? C1 Ru1 C2 37.33(12) . . ? N2 Ru1 C2 110.35(10) . . ? C3 Ru1 C2 36.51(12) . . ? C6 Ru1 C2 67.27(11) . . ? C4 Ru1 C2 66.55(12) . . ? N1 Ru1 C5 149.50(10) . . ? C1 Ru1 C5 66.75(11) . . ? N2 Ru1 C5 134.95(9) . . ? C3 Ru1 C5 66.47(11) . . ? C6 Ru1 C5 36.73(10) . . ? C4 Ru1 C5 36.41(10) . . ? C2 Ru1 C5 78.79(11) . . ? N1 Ru1 Cl1 86.42(6) . . ? C1 Ru1 Cl1 127.18(10) . . ? N2 Ru1 Cl1 87.21(6) . . ? C3 Ru1 Cl1 140.64(10) . . ? C6 Ru1 Cl1 94.52(8) . . ? C4 Ru1 Cl1 104.47(8) . . ? C2 Ru1 Cl1 161.59(8) . . ? C5 Ru1 Cl1 84.86(7) . . ? C16 N1 C15 108.6(2) . . ? C16 N1 C11 108.5(2) . . ? C15 N1 C11 108.1(2) . . ? C16 N1 Ru1 112.58(18) . . ? C15 N1 Ru1 108.91(16) . . ? C11 N1 Ru1 109.98(18) . . ? C14 N2 C13 107.7(2) . . ? C14 N2 C17 111.58(19) . . ? C13 N2 C17 111.23(19) . . ? C14 N2 Ru1 109.41(15) . . ? C13 N2 Ru1 109.07(16) . . ? C17 N2 Ru1 107.80(15) . . ? C47 N3 C45 108.8(2) . . ? C47 N3 C42 108.5(2) . . ? C45 N3 C42 108.2(2) . . ? C47 N3 Ru2 112.75(18) . . ? C45 N3 Ru2 109.06(17) . . ? C42 N3 Ru2 109.38(19) . . ? C44 N4 C46 107.9(2) . . ? C44 N4 C48 110.53(19) . . ? C46 N4 C48 111.5(2) . . ? C44 N4 Ru2 109.21(16) . . ? C46 N4 Ru2 109.08(15) . . ? C48 N4 Ru2 108.58(15) . . ? C6 C1 C2 121.8(3) . . ? C6 C1 Ru1 72.27(16) . . ? C2 C1 Ru1 74.40(18) . . ? C6 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? Ru1 C1 H1 118.9 . . ? C3 C2 C1 116.3(3) . . ? C3 C2 C7 122.4(3) . . ? C1 C2 C7 121.2(4) . . ? C3 C2 Ru1 68.96(16) . . ? C1 C2 Ru1 68.27(16) . . ? C7 C2 Ru1 136.3(2) . . ? C2 C3 C4 122.3(3) . . ? C2 C3 Ru1 74.53(18) . . ? C4 C3 Ru1 72.25(16) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? Ru1 C3 H3 118.6 . . ? C5 C4 C3 121.1(3) . . ? C5 C4 Ru1 74.05(16) . . ? C3 C4 Ru1 70.46(17) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? Ru1 C4 H4 119.1 . . ? C4 C5 C6 117.8(3) . . ? C4 C5 C8 118.7(3) . . ? C6 C5 C8 123.5(3) . . ? C4 C5 Ru1 69.54(16) . . ? C6 C5 Ru1 69.17(16) . . ? C8 C5 Ru1 131.72(19) . . ? C1 C6 C5 120.5(3) . . ? C1 C6 Ru1 70.26(16) . . ? C5 C6 Ru1 74.09(16) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? Ru1 C6 H6 119.4 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C5 115.7(3) . . ? C9 C8 C10 110.4(3) . . ? C5 C8 C10 108.4(3) . . ? C9 C8 H8 107.3 . . ? C5 C8 H8 107.3 . . ? C10 C8 H8 107.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 112.7(2) . . ? N1 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N1 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C13 C12 C11 118.8(2) . . ? C13 C12 H12A 107.6 . . ? C11 C12 H12A 107.6 . . ? C13 C12 H12B 107.6 . . ? C11 C12 H12B 107.6 . . ? H12A C12 H12B 107.1 . . ? N2 C13 C12 113.1(2) . . ? N2 C13 H13A 108.9 . . ? C12 C13 H13A 108.9 . . ? N2 C13 H13B 108.9 . . ? C12 C13 H13B 108.9 . . ? H13A C13 H13B 107.8 . . ? N2 C14 C15 110.4(2) . . ? N2 C14 H14A 109.6 . . ? C15 C14 H14A 109.6 . . ? N2 C14 H14B 109.6 . . ? C15 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? N1 C15 C14 111.6(2) . . ? N1 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? N1 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N2 118.0(2) . . ? C18 C17 H17A 107.8 . . ? N2 C17 H17A 107.8 . . ? C18 C17 H17B 107.8 . . ? N2 C17 H17B 107.8 . . ? H17A C17 H17B 107.2 . . ? C19 C18 C31 119.4(2) . . ? C19 C18 C17 120.9(2) . . ? C31 C18 C17 119.5(2) . . ? C18 C19 C20 123.9(3) . . ? C18 C19 C24 119.1(2) . . ? C20 C19 C24 116.9(2) . . ? C21 C20 C19 122.0(3) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C22 120.4(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 120.3(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 121.0(3) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C19 120.3(3) . . ? C25 C24 C23 120.6(3) . . ? C19 C24 C23 119.1(3) . . ? C24 C25 C26 121.6(3) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? C25 C26 C31 119.3(3) . . ? C25 C26 C27 120.5(3) . . ? C31 C26 C27 120.2(3) . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.6(3) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 121.8(3) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C29 C30 C31 121.7(3) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C18 C31 C26 119.8(2) . . ? C18 C31 C30 124.0(3) . . ? C26 C31 C30 116.2(2) . . ? C33 C32 C37 122.6(3) . . ? C33 C32 Ru2 74.62(18) . . ? C37 C32 Ru2 72.58(17) . . ? C33 C32 H32 118.4 . . ? C37 C32 H32 118.4 . . ? Ru2 C32 H32 118.4 . . ? C32 C33 C34 116.7(3) . . ? C32 C33 C38 121.6(3) . . ? C34 C33 C38 121.6(3) . . ? C32 C33 Ru2 68.96(17) . . ? C34 C33 Ru2 68.57(16) . . ? C38 C33 Ru2 136.3(3) . . ? C35 C34 C33 122.0(3) . . ? C35 C34 Ru2 72.25(16) . . ? C33 C34 Ru2 74.39(18) . . ? C35 C34 H34 118.7 . . ? C33 C34 H34 118.7 . . ? Ru2 C34 H34 118.7 . . ? C34 C35 C36 120.2(3) . . ? C34 C35 Ru2 70.53(16) . . ? C36 C35 Ru2 73.67(15) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? Ru2 C35 H35 119.5 . . ? C37 C36 C35 117.9(3) . . ? C37 C36 C39 117.9(3) . . ? C35 C36 C39 124.2(3) . . ? C37 C36 Ru2 69.86(16) . . ? C35 C36 Ru2 69.36(16) . . ? C39 C36 Ru2 132.4(2) . . ? C32 C37 C36 120.2(3) . . ? C32 C37 Ru2 70.29(18) . . ? C36 C37 Ru2 73.36(17) . . ? C32 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? Ru2 C37 H37 119.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 C41 115.6(3) . . ? C36 C39 C40 108.2(3) . . ? C41 C39 C40 110.7(3) . . ? C36 C39 H39 107.3 . . ? C41 C39 H39 107.3 . . ? C40 C39 H39 107.3 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 C43 112.9(2) . . ? N3 C42 H42A 109.0 . . ? C43 C42 H42A 109.0 . . ? N3 C42 H42B 109.0 . . ? C43 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? C44 C43 C42 118.2(3) . . ? C44 C43 H43A 107.8 . . ? C42 C43 H43A 107.8 . . ? C44 C43 H43B 107.8 . . ? C42 C43 H43B 107.8 . . ? H43A C43 H43B 107.1 . . ? N4 C44 C43 113.6(2) . . ? N4 C44 H44A 108.8 . . ? C43 C44 H44A 108.8 . . ? N4 C44 H44B 108.8 . . ? C43 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? N3 C45 C46 111.7(2) . . ? N3 C45 H45A 109.3 . . ? C46 C45 H45A 109.3 . . ? N3 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 107.9 . . ? N4 C46 C45 110.6(2) . . ? N4 C46 H46A 109.5 . . ? C45 C46 H46A 109.5 . . ? N4 C46 H46B 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? N3 C47 H47A 109.5 . . ? N3 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N3 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 N4 116.9(2) . . ? C49 C48 H48A 108.1 . . ? N4 C48 H48A 108.1 . . ? C49 C48 H48B 108.1 . . ? N4 C48 H48B 108.1 . . ? H48A C48 H48B 107.3 . . ? C62 C49 C50 119.6(2) . . ? C62 C49 C48 120.8(2) . . ? C50 C49 C48 119.6(2) . . ? C49 C50 C51 124.0(3) . . ? C49 C50 C55 119.2(2) . . ? C51 C50 C55 116.8(3) . . ? C52 C51 C50 121.8(3) . . ? C52 C51 H51 119.1 . . ? C50 C51 H51 119.1 . . ? C51 C52 C53 120.9(3) . . ? C51 C52 H52 119.6 . . ? C53 C52 H52 119.6 . . ? C54 C53 C52 119.9(3) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C53 C54 C55 121.2(3) . . ? C53 C54 H54 119.4 . . ? C55 C54 H54 119.4 . . ? C56 C55 C54 120.6(3) . . ? C56 C55 C50 120.2(3) . . ? C54 C55 C50 119.2(3) . . ? C55 C56 C57 121.5(3) . . ? C55 C56 H56 119.2 . . ? C57 C56 H56 119.2 . . ? C56 C57 C58 120.9(3) . . ? C56 C57 C62 119.5(2) . . ? C58 C57 C62 119.7(3) . . ? C59 C58 C57 120.9(3) . . ? C59 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? C58 C59 C60 120.1(3) . . ? C58 C59 H59 120.0 . . ? C60 C59 H59 120.0 . . ? C61 C60 C59 121.4(3) . . ? C61 C60 H60 119.3 . . ? C59 C60 H60 119.3 . . ? C60 C61 C62 121.6(3) . . ? C60 C61 H61 119.2 . . ? C62 C61 H61 119.2 . . ? C49 C62 C61 124.3(2) . . ? C49 C62 C57 119.5(2) . . ? C61 C62 C57 116.1(2) . . ? F10 P2 F10A 91.2(7) . . ? F11 P2 F12 97.1(6) . . ? F10 P2 F9A 89.4(7) . . ? F10A P2 F9A 178.9(7) . . ? F10 P2 F8 91.7(6) . . ? F10A P2 F8 95.9(5) . . ? F11 P2 F8 97.0(5) . . ? F12 P2 F8 87.7(4) . . ? F9A P2 F8 85.0(5) . . ? F11 P2 F11A 92.2(6) . . ? F12 P2 F11A 170.6(7) . . ? F8 P2 F11A 91.0(3) . . ? F10 P2 F7 88.8(5) . . ? F10A P2 F7 82.9(5) . . ? F11 P2 F7 83.6(5) . . ? F12 P2 F7 91.1(4) . . ? F9A P2 F7 96.2(5) . . ? F8 P2 F7 178.71(17) . . ? F11A P2 F7 90.2(3) . . ? F10 P2 F9 178.7(7) . . ? F10A P2 F9 88.6(6) . . ? F9A P2 F9 90.9(7) . . ? F8 P2 F9 87.1(4) . . ? F7 P2 F9 92.4(4) . . ? F11 P2 F12A 173.5(6) . . ? F12 P2 F12A 87.8(7) . . ? F8 P2 F12A 87.4(4) . . ? F11A P2 F12A 82.9(6) . . ? F7 P2 F12A 92.1(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.527 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.064 _database_code_depnum_ccdc_archive 'CCDC 961677'