# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Gregory Solan' _publ_contact_author_email GAS8@LE.AC.UK _publ_section_title ; N-Heterocyclic carbene-containing ruthenium difluoride complexes and their reactivity towards BF3 ; loop_ _publ_author_name 'Gregory Solan' 'John Fawcett' 'Duncan A.J. Harding' 'Eric G Hope' 'Kuldip Singh' # Attachment '05022cc.cif' data_05022 _database_code_depnum_ccdc_archive 'CCDC 723424' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C56 H72 F2 N4 O2 Ru) (H2 O)' _chemical_formula_sum 'C56 H74 F2 N4 O3 Ru' _chemical_formula_weight 990.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cc 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 38.437(6) _cell_length_b 14.532(2) _cell_length_c 20.864(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.921(3) _cell_angle_gamma 90.00 _cell_volume 10734(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 918 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 21.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4192 _exptl_absorpt_coefficient_mu 0.344 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.781 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; absorption correction based on 12843 reflections (SADABS); Rint 0.037 before correction and 0.030 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37997 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.1011 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18554 _reflns_number_gt 12793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1544P)^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 constrained _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 0.48(6) _refine_ls_number_reflns 18554 _refine_ls_number_parameters 541 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1174 _refine_ls_R_factor_gt 0.0855 _refine_ls_wR_factor_ref 0.2522 _refine_ls_wR_factor_gt 0.2243 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.824913(17) 0.23542(7) 0.10323(3) 0.0228(3) Uiso 1 1 d . . . F1 F 0.8263(2) 0.3126(5) 0.0222(4) 0.047(2) Uiso 1 1 d . . . F2 F 0.7819(2) 0.3300(5) 0.0867(4) 0.050(2) Uiso 1 1 d . . . N1 N 0.7780(3) 0.1403(7) -0.0403(5) 0.027(2) Uiso 1 1 d . . . N2 N 0.7552(3) 0.1002(6) 0.0328(5) 0.023(2) Uiso 1 1 d . . . N3 N 0.9028(3) 0.3284(8) 0.1967(6) 0.040(3) Uiso 1 1 d . . . N4 N 0.8569(3) 0.4113(7) 0.2010(5) 0.029(2) Uiso 1 1 d . . . O1 O 0.8785(2) 0.0799(6) 0.1207(5) 0.051(2) Uiso 1 1 d . . . O2 O 0.8285(3) 0.1444(6) 0.2342(5) 0.052(2) Uiso 1 1 d . . . O4 O 0.7360(3) 0.4169(7) 0.0063(5) 0.046(3) Uiso 1 1 d . . . C1 C 0.8598(4) 0.1442(10) 0.1134(7) 0.044(4) Uiso 1 1 d . . . C2 C 0.8190(3) 0.1852(8) 0.1808(6) 0.029(3) Uiso 1 1 d . . . C3 C 0.7838(3) 0.1477(9) 0.0279(6) 0.025(3) Uiso 1 1 d . . . C4 C 0.7471(3) 0.0768(9) -0.0721(6) 0.030(3) Uiso 1 1 d . . . C5 C 0.7316(4) 0.0605(9) -0.0269(7) 0.030(3) Uiso 1 1 d . . . C6 C 0.7992(4) 0.1730(9) -0.0831(7) 0.035(3) Uiso 1 1 d . . . C7 C 0.7857(4) 0.2557(9) -0.1201(7) 0.041(4) Uiso 1 1 d . . . C8 C 0.8049(4) 0.2816(10) -0.1652(8) 0.052(4) Uiso 1 1 d . . . C9 C 0.8401(4) 0.1933(11) -0.1595(8) 0.062(4) Uiso 1 1 d . . . C10 C 0.8469(4) 0.1172(11) -0.1267(8) 0.069(5) Uiso 1 1 d . . . C11 C 0.8263(4) 0.1083(10) -0.0873(7) 0.036(3) Uiso 1 1 d . . . C12 C 0.7553(4) 0.3109(10) -0.1110(7) 0.049(4) Uiso 1 1 d . . . C13 C 0.7614(4) 0.4130(9) -0.1155(7) 0.059(4) Uiso 1 1 d . . . C14 C 0.7235(6) 0.2922(15) -0.1890(11) 0.104(7) Uiso 1 1 d . . . C15 C 0.8383(4) 0.0264(9) -0.0516(6) 0.044(3) Uiso 1 1 d . . . C16 C 0.8791(5) -0.0173(12) -0.0165(9) 0.078(5) Uiso 1 1 d . . . C17 C 0.8186(4) -0.0585(10) -0.0999(7) 0.059(4) Uiso 1 1 d . . . C18 C 0.7511(4) 0.0845(10) 0.0990(7) 0.036(4) Uiso 1 1 d . . . C19 C 0.7271(4) 0.1429(9) 0.1161(7) 0.031(3) Uiso 1 1 d . . . C20 C 0.7219(3) 0.1166(8) 0.1778(6) 0.032(3) Uiso 1 1 d . . . C21 C 0.7375(4) 0.0428(10) 0.2142(7) 0.046(4) Uiso 1 1 d . . . C22 C 0.7627(3) -0.0153(8) 0.1960(6) 0.035(3) Uiso 1 1 d . . . C23 C 0.7673(3) 0.0059(8) 0.1390(6) 0.025(3) Uiso 1 1 d . . . C24 C 0.7039(5) 0.2229(11) 0.0677(9) 0.047(5) Uiso 1 1 d . . . C25 C 0.6668(4) 0.1824(11) 0.0187(8) 0.050(4) Uiso 1 1 d . . . C26 C 0.6973(3) 0.3018(8) 0.1018(6) 0.037(3) Uiso 1 1 d . . . C27 C 0.8305(4) -0.0790(9) 0.1681(6) 0.043(3) Uiso 1 1 d . . . C28 C 0.7899(3) -0.0589(8) 0.1174(6) 0.036(3) Uiso 1 1 d . . . C29 C 0.7735(4) -0.1381(9) 0.0755(7) 0.061(4) Uiso 1 1 d . . . C30 C 0.8634(3) 0.3319(8) 0.1718(6) 0.020(3) Uiso 1 1 d . . . C31 C 0.9206(4) 0.4047(10) 0.2401(7) 0.049(4) Uiso 1 1 d . . . C32 C 0.8887(4) 0.4655(9) 0.2332(7) 0.045(4) Uiso 1 1 d . . . C33 C 0.8190(4) 0.4527(9) 0.1937(6) 0.041(3) Uiso 1 1 d . . . C34 C 0.8053(4) 0.4289(9) 0.2361(7) 0.035(3) Uiso 1 1 d . . . C35 C 0.7698(4) 0.4858(9) 0.2203(7) 0.046(4) Uiso 1 1 d . . . C36 C 0.7586(4) 0.5543(9) 0.1710(7) 0.053(4) Uiso 1 1 d . . . C37 C 0.7801(4) 0.5779(10) 0.1324(8) 0.064(4) Uiso 1 1 d . . . C38 C 0.8109(4) 0.5317(11) 0.1439(8) 0.050(4) Uiso 1 1 d . . . C39 C 0.8186(4) 0.3614(9) 0.2886(7) 0.040(3) Uiso 1 1 d . . . C40 C 0.8488(5) 0.4240(13) 0.3555(10) 0.080(6) Uiso 1 1 d . . . C41 C 0.7858(4) 0.2952(10) 0.2909(7) 0.066(4) Uiso 1 1 d . . . C42 C 0.8371(4) 0.5630(10) 0.1047(8) 0.072(4) Uiso 1 1 d . . . C43 C 0.8416(6) 0.5172(15) 0.0556(11) 0.117(7) Uiso 1 1 d . . . C44 C 0.8575(6) 0.6549(14) 0.1399(11) 0.111(6) Uiso 1 1 d . . . C45 C 0.9255(4) 0.2551(9) 0.1922(7) 0.050(4) Uiso 1 1 d . . . C46 C 0.9313(4) 0.2742(9) 0.1132(7) 0.039(3) Uiso 1 1 d . . . C47 C 0.9594(7) 0.2008(17) 0.1227(12) 0.114(8) Uiso 1 1 d . . . C48 C 0.9724(6) 0.1362(15) 0.1750(11) 0.107(7) Uiso 1 1 d . . . C49 C 0.9682(6) 0.1364(15) 0.2366(11) 0.104(7) Uiso 1 1 d . . . C50 C 0.9426(3) 0.2019(8) 0.2307(6) 0.035(3) Uiso 1 1 d . . . C51 C 0.9169(5) 0.3300(11) 0.0724(8) 0.067(5) Uiso 1 1 d . . . C52 C 0.8986(4) 0.3135(9) -0.0118(6) 0.050(3) Uiso 1 1 d . . . C53 C 0.9487(7) 0.4080(16) 0.0739(12) 0.126(8) Uiso 1 1 d . . . C54 C 0.9361(4) 0.1898(11) 0.2923(8) 0.065(4) Uiso 1 1 d . . . C55 C 0.9271(7) 0.0906(18) 0.3100(14) 0.122(8) Uiso 1 1 d . . . C56 C 0.9705(7) 0.2250(16) 0.3636(13) 0.114(7) Uiso 1 1 d . . . Ru2 Ru 0.577677(17) 0.26400(7) 0.34714(3) 0.0232(3) Uiso 1 1 d . . . F1A F 0.62118(19) 0.1786(5) 0.3561(3) 0.0367(18) Uiso 1 1 d . . . F2A F 0.5718(2) 0.2012(5) 0.4255(4) 0.0417(19) Uiso 1 1 d . . . N1A N 0.6477(3) 0.3941(7) 0.4146(6) 0.033(3) Uiso 1 1 d . . . N2A N 0.6233(3) 0.3678(7) 0.4923(5) 0.032(3) Uiso 1 1 d . . . N3A N 0.5015(3) 0.1653(7) 0.2590(5) 0.027(3) Uiso 1 1 d . . . N4A N 0.5464(3) 0.0816(8) 0.2570(5) 0.041(3) Uiso 1 1 d . . . O3 O 0.6698(3) 0.0881(7) 0.4448(5) 0.046(3) Uiso 1 1 d . . . O1A O 0.5819(3) 0.3431(6) 0.2180(5) 0.056(3) Uiso 1 1 d . . . O2A O 0.5220(3) 0.4097(6) 0.3426(5) 0.051(2) Uiso 1 1 d . . . C1A C 0.5765(3) 0.3213(8) 0.2690(6) 0.030(3) Uiso 1 1 d . . . C2A C 0.5419(3) 0.3467(9) 0.3432(6) 0.031(3) Uiso 1 1 d . . . C3A C 0.6175(3) 0.3457(8) 0.4234(6) 0.019(3) Uiso 1 1 d . . . C4A C 0.6703(4) 0.4393(11) 0.4782(8) 0.045(4) Uiso 1 1 d . . . C5A C 0.6557(4) 0.4133(9) 0.5278(7) 0.040(4) Uiso 1 1 d . . . C6A C 0.6541(3) 0.4146(9) 0.3540(6) 0.023(3) Uiso 1 1 d . . . C7A C 0.6797(4) 0.3561(9) 0.3379(7) 0.033(3) Uiso 1 1 d . . . C8A C 0.6858(4) 0.3728(10) 0.2791(7) 0.047(4) Uiso 1 1 d . . . C9A C 0.6671(4) 0.4505(11) 0.2348(8) 0.049(4) Uiso 1 1 d . . . C10A C 0.6450(4) 0.5055(10) 0.2510(7) 0.046(4) Uiso 1 1 d . . . C11A C 0.6354(4) 0.4880(10) 0.3174(8) 0.046(4) Uiso 1 1 d . . . C12A C 0.6977(4) 0.2816(9) 0.3824(7) 0.030(3) Uiso 1 1 d . . . C13A C 0.7388(5) 0.3119(13) 0.4309(9) 0.064(5) Uiso 1 1 d . . . C14A C 0.6985(4) 0.1874(10) 0.3334(7) 0.056(4) Uiso 1 1 d . . . C15A C 0.6080(4) 0.5499(9) 0.3400(7) 0.045(4) Uiso 1 1 d . . . C16A C 0.5761(4) 0.5804(10) 0.2700(7) 0.054(4) Uiso 1 1 d . . . C17A C 0.6365(5) 0.6531(11) 0.3578(9) 0.085(5) Uiso 1 1 d . . . C18A C 0.6016(3) 0.3375(9) 0.5292(6) 0.030(3) Uiso 1 1 d . . . C19A C 0.5738(5) 0.3949(13) 0.5363(9) 0.062(5) Uiso 1 1 d . . . C20A C 0.5583(3) 0.3567(8) 0.5855(6) 0.035(3) Uiso 1 1 d . . . C21A C 0.5701(3) 0.2741(8) 0.6223(6) 0.040(3) Uiso 1 1 d . . . C22A C 0.5922(4) 0.2338(10) 0.6106(8) 0.053(4) Uiso 1 1 d . . . C23A C 0.6115(4) 0.2556(9) 0.5685(7) 0.036(3) Uiso 1 1 d . . . C24A C 0.5666(4) 0.4933(10) 0.4950(8) 0.057(4) Uiso 1 1 d . . . C25A C 0.5925(5) 0.5684(11) 0.5459(8) 0.074(5) Uiso 1 1 d . . . C26A C 0.5203(4) 0.4868(10) 0.4753(7) 0.060(4) Uiso 1 1 d . . . C27A C 0.6420(4) 0.1953(10) 0.5680(7) 0.046(4) Uiso 1 1 d . . . C28A C 0.6282(4) 0.0872(9) 0.5591(7) 0.059(4) Uiso 1 1 d . . . C29A C 0.6819(5) 0.2102(13) 0.6266(9) 0.079(5) Uiso 1 1 d . . . C30A C 0.5386(4) 0.1626(9) 0.2822(7) 0.029(3) Uiso 1 1 d . . . C31A C 0.4850(4) 0.0884(9) 0.2211(7) 0.039(3) Uiso 1 1 d . . . C32A C 0.5108(4) 0.0480(10) 0.2083(8) 0.050(4) Uiso 1 1 d . . . C33A C 0.4770(3) 0.2317(7) 0.2731(5) 0.023(2) Uiso 1 1 d . A . C34A C 0.4687(5) 0.2341(10) 0.3209(9) 0.059(5) Uiso 1 1 d . . . C35A C 0.4435(4) 0.2842(9) 0.3441(7) 0.049(3) Uiso 1 1 d . . . C36A C 0.4267(4) 0.3457(9) 0.2916(6) 0.049(3) Uiso 1 1 d . . . C37A C 0.4330(4) 0.3594(10) 0.2317(8) 0.057(4) Uiso 1 1 d . A . C38A C 0.4606(6) 0.2969(13) 0.2060(10) 0.089(6) Uiso 1 1 d . . . C39A C 0.4912(3) 0.1499(9) 0.3880(6) 0.040(3) Uiso 1 1 d . . . C40A C 0.4999(6) 0.2178(13) 0.4531(11) 0.101(6) Uiso 1 1 d . . . C41A C 0.4646(4) 0.0695(10) 0.3816(7) 0.062(4) Uiso 1 1 d . . . C42A C 0.4715(6) 0.2958(15) 0.1490(10) 0.057(3) Uiso 0.80 1 d P A 1 C43A C 0.4780(6) 0.4018(14) 0.1406(10) 0.057(3) Uiso 0.80 1 d P A 1 C44A C 0.4422(5) 0.2427(11) 0.0821(9) 0.057(3) Uiso 0.80 1 d P A 1 C42B C 0.483(2) 0.291(5) 0.137(4) 0.057(3) Uiso 0.20 1 d P A 2 C43B C 0.4901(18) 0.386(4) 0.108(3) 0.057(3) Uiso 0.20 1 d P A 2 C44B C 0.431(2) 0.283(5) 0.099(4) 0.057(3) Uiso 0.20 1 d P A 2 C45A C 0.5800(3) 0.0382(7) 0.2645(5) 0.021(2) Uiso 1 1 d . . . C46A C 0.5998(4) 0.0627(10) 0.2191(7) 0.040(4) Uiso 1 1 d . B . C47A C 0.6317(4) 0.0268(9) 0.2193(7) 0.046(4) Uiso 1 1 d . . . C48A C 0.6490(4) -0.0390(9) 0.2682(7) 0.054(4) Uiso 1 1 d . . . C49A C 0.6316(4) -0.0712(9) 0.3133(7) 0.055(4) Uiso 1 1 d . . . C50A C 0.5954(4) -0.0243(11) 0.3101(8) 0.050(4) Uiso 1 1 d . . . C51A C 0.5763(4) 0.1318(11) 0.1533(8) 0.060(4) Uiso 1 1 d . . . C52A C 0.6048(5) 0.1856(11) 0.1338(9) 0.079(5) Uiso 1 1 d . B . C53A C 0.5630(6) 0.0996(14) 0.0882(10) 0.046(5) Uiso 0.60 1 d P B 1 C53B C 0.5441(9) 0.070(2) 0.0880(16) 0.043(8) Uiso 0.40 1 d P B 2 C54A C 0.5812(6) -0.0707(14) 0.3663(12) 0.108(7) Uiso 1 1 d . . . C55A C 0.5621(5) -0.1614(13) 0.3406(10) 0.096(5) Uiso 1 1 d . . . C56A C 0.5849(7) -0.0487(17) 0.4232(14) 0.147(9) Uiso 1 1 d . . . _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.839(15) . ? Ru1 C2 1.868(11) . ? Ru1 F1 2.047(7) . ? Ru1 F2 2.073(8) . ? Ru1 C30 2.134(12) . ? Ru1 C3 2.157(13) . ? N1 C3 1.357(15) . ? N1 C4 1.446(15) . ? N1 C6 1.503(15) . ? N2 C3 1.336(15) . ? N2 C5 1.353(16) . ? N2 C18 1.469(16) . ? N3 C30 1.396(15) . ? N3 C45 1.403(17) . ? N3 C31 1.427(18) . ? N4 C30 1.374(14) . ? N4 C32 1.390(16) . ? N4 C33 1.527(15) . ? O1 C1 1.152(15) . ? O2 C2 1.187(13) . ? C4 C5 1.318(16) . ? C6 C7 1.413(18) . ? C6 C11 1.429(17) . ? C7 C8 1.453(18) . ? C7 C12 1.490(19) . ? C8 C9 1.83(2) . ? C9 C10 1.27(2) . ? C10 C11 1.351(19) . ? C11 C15 1.385(18) . ? C12 C13 1.510(18) . ? C12 C14 1.63(2) . ? C15 C16 1.58(2) . ? C15 C17 1.586(18) . ? C18 C19 1.396(18) . ? C18 C23 1.409(18) . ? C19 C20 1.430(16) . ? C19 C24 1.57(2) . ? C20 C21 1.316(18) . ? C21 C22 1.442(17) . ? C22 C23 1.304(15) . ? C23 C28 1.467(16) . ? C24 C26 1.423(19) . ? C24 C25 1.51(2) . ? C27 C28 1.534(17) . ? C28 C29 1.435(17) . ? C31 C32 1.472(19) . ? C33 C34 1.242(16) . ? C33 C38 1.497(19) . ? C34 C39 1.409(17) . ? C34 C35 1.518(18) . ? C35 C36 1.375(18) . ? C36 C37 1.405(19) . ? C37 C38 1.297(19) . ? C38 C42 1.59(2) . ? C39 C41 1.601(18) . ? C39 C40 1.69(2) . ? C42 C43 1.29(2) . ? C42 C44 1.58(2) . ? C45 C50 1.123(16) . ? C45 C46 1.769(19) . ? C46 C51 1.150(18) . ? C46 C47 1.47(3) . ? C47 C48 1.38(3) . ? C48 C49 1.36(3) . ? C49 C50 1.34(2) . ? C50 C54 1.410(18) . ? C51 C52 1.63(2) . ? C51 C53 1.66(3) . ? C54 C55 1.56(3) . ? C54 C56 1.64(3) . ? Ru2 C2A 1.805(13) . ? Ru2 C1A 1.816(11) . ? Ru2 F2A 1.960(7) . ? Ru2 F1A 2.032(7) . ? Ru2 C3A 2.094(12) . ? Ru2 C30A 2.163(13) . ? N1A C6A 1.411(15) . ? N1A C3A 1.430(15) . ? N1A C4A 1.432(18) . ? N2A C5A 1.348(16) . ? N2A C3A 1.403(14) . ? N2A C18A 1.408(14) . ? N3A C30A 1.316(15) . ? N3A C31A 1.373(16) . ? N3A C33A 1.457(13) . ? N4A C30A 1.369(16) . ? N4A C45A 1.392(14) . ? N4A C32A 1.435(18) . ? O1A C1A 1.203(13) . ? O2A C2A 1.189(14) . ? C4A C5A 1.409(19) . ? C6A C11A 1.346(19) . ? C6A C7A 1.434(16) . ? C7A C8A 1.359(17) . ? C7A C12A 1.418(18) . ? C8A C9A 1.46(2) . ? C9A C10A 1.302(19) . ? C10A C11A 1.588(18) . ? C11A C15A 1.589(19) . ? C12A C13A 1.57(2) . ? C12A C14A 1.72(2) . ? C15A C16A 1.561(18) . ? C15A C17A 1.81(2) . ? C18A C19A 1.41(2) . ? C18A C23A 1.411(17) . ? C19A C20A 1.48(2) . ? C19A C24A 1.64(2) . ? C20A C21A 1.401(16) . ? C21A C22A 1.136(17) . ? C22A C23A 1.389(18) . ? C23A C27A 1.467(18) . ? C24A C25A 1.58(2) . ? C24A C26A 1.66(2) . ? C27A C29A 1.56(2) . ? C27A C28A 1.646(18) . ? C31A C32A 1.268(17) . ? C33A C34A 1.159(17) . ? C33A C38A 1.60(2) . ? C34A C35A 1.44(2) . ? C34A C39A 1.807(19) . ? C35A C36A 1.366(19) . ? C36A C37A 1.376(18) . ? C37A C38A 1.64(2) . ? C38A C42A 1.41(2) . ? C38A C42B 1.93(7) . ? C39A C41A 1.523(18) . ? C39A C40A 1.60(2) . ? C42A C43A 1.58(3) . ? C42A C44A 1.61(3) . ? C42B C43B 1.57(9) . ? C42B C44B 1.83(11) . ? C45A C50A 1.281(18) . ? C45A C46A 1.471(17) . ? C46A C47A 1.329(18) . ? C46A C51A 1.66(2) . ? C47A C48A 1.368(18) . ? C48A C49A 1.430(18) . ? C49A C50A 1.53(2) . ? C50A C54A 1.62(3) . ? C51A C53A 1.34(2) . ? C51A C52A 1.52(2) . ? C51A C53B 1.70(3) . ? C54A C56A 1.18(3) . ? C54A C55A 1.50(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 87.1(5) . . ? C1 Ru1 F1 103.7(5) . . ? C2 Ru1 F1 168.7(4) . . ? C1 Ru1 F2 174.9(5) . . ? C2 Ru1 F2 92.6(4) . . ? F1 Ru1 F2 77.0(3) . . ? C1 Ru1 C30 96.4(5) . . ? C2 Ru1 C30 87.9(5) . . ? F1 Ru1 C30 87.6(4) . . ? F2 Ru1 C30 88.6(4) . . ? C1 Ru1 C3 87.3(6) . . ? C2 Ru1 C3 95.7(5) . . ? F1 Ru1 C3 88.3(4) . . ? F2 Ru1 C3 87.7(4) . . ? C30 Ru1 C3 175.0(5) . . ? C3 N1 C4 107.6(9) . . ? C3 N1 C6 133.9(10) . . ? C4 N1 C6 117.9(9) . . ? C3 N2 C5 115.4(10) . . ? C3 N2 C18 123.1(10) . . ? C5 N2 C18 121.4(10) . . ? C30 N3 C45 128.0(12) . . ? C30 N3 C31 113.0(11) . . ? C45 N3 C31 118.3(12) . . ? C30 N4 C32 114.3(10) . . ? C30 N4 C33 128.3(10) . . ? C32 N4 C33 116.8(10) . . ? O1 C1 Ru1 171.5(13) . . ? O2 C2 Ru1 155.6(10) . . ? N2 C3 N1 103.6(10) . . ? N2 C3 Ru1 129.9(8) . . ? N1 C3 Ru1 125.8(9) . . ? C5 C4 N1 107.9(11) . . ? C4 C5 N2 104.7(11) . . ? C7 C6 C11 130.3(12) . . ? C7 C6 N1 115.1(11) . . ? C11 C6 N1 113.9(10) . . ? C6 C7 C8 113.7(12) . . ? C6 C7 C12 121.9(12) . . ? C8 C7 C12 124.4(12) . . ? C7 C8 C9 109.0(11) . . ? C10 C9 C8 129.4(13) . . ? C9 C10 C11 111.3(14) . . ? C10 C11 C15 105.0(13) . . ? C10 C11 C6 125.9(13) . . ? C15 C11 C6 129.0(12) . . ? C7 C12 C13 111.8(12) . . ? C7 C12 C14 96.0(12) . . ? C13 C12 C14 100.2(13) . . ? C11 C15 C16 131.0(12) . . ? C11 C15 C17 110.5(11) . . ? C16 C15 C17 97.1(11) . . ? C19 C18 C23 121.7(12) . . ? C19 C18 N2 118.1(12) . . ? C23 C18 N2 119.8(12) . . ? C18 C19 C20 113.9(12) . . ? C18 C19 C24 123.5(12) . . ? C20 C19 C24 122.2(12) . . ? C21 C20 C19 122.9(12) . . ? C20 C21 C22 121.9(13) . . ? C23 C22 C21 116.4(12) . . ? C22 C23 C18 123.0(12) . . ? C22 C23 C28 115.8(11) . . ? C18 C23 C28 121.2(11) . . ? C26 C24 C25 110.2(13) . . ? C26 C24 C19 116.2(13) . . ? C25 C24 C19 107.3(12) . . ? C29 C28 C23 122.0(11) . . ? C29 C28 C27 110.8(11) . . ? C23 C28 C27 118.5(10) . . ? N4 C30 N3 103.0(10) . . ? N4 C30 Ru1 130.5(8) . . ? N3 C30 Ru1 126.4(9) . . ? N3 C31 C32 103.3(12) . . ? N4 C32 C31 104.5(11) . . ? C34 C33 C38 132.6(13) . . ? C34 C33 N4 118.1(11) . . ? C38 C33 N4 107.7(10) . . ? C33 C34 C39 128.5(13) . . ? C33 C34 C35 106.7(12) . . ? C39 C34 C35 124.8(11) . . ? C36 C35 C34 123.5(12) . . ? C35 C36 C37 121.4(13) . . ? C38 C37 C36 117.8(14) . . ? C37 C38 C33 117.0(13) . . ? C37 C38 C42 118.0(14) . . ? C33 C38 C42 125.0(13) . . ? C34 C39 C41 113.0(11) . . ? C34 C39 C40 101.0(11) . . ? C41 C39 C40 126.4(11) . . ? C43 C42 C44 127.6(17) . . ? C43 C42 C38 124.7(16) . . ? C44 C42 C38 107.5(13) . . ? C50 C45 N3 132.7(14) . . ? C50 C45 C46 121.7(13) . . ? N3 C45 C46 104.5(10) . . ? C51 C46 C47 136.5(16) . . ? C51 C46 C45 127.1(13) . . ? C47 C46 C45 96.4(12) . . ? C48 C47 C46 128(2) . . ? C49 C48 C47 127(2) . . ? C50 C49 C48 105.7(18) . . ? C45 C50 C49 139.1(15) . . ? C45 C50 C54 118.5(13) . . ? C49 C50 C54 102.3(13) . . ? C46 C51 C52 125.1(15) . . ? C46 C51 C53 109.2(16) . . ? C52 C51 C53 97.3(13) . . ? C50 C54 C55 117.8(14) . . ? C50 C54 C56 115.0(14) . . ? C55 C54 C56 104.3(16) . . ? C2A Ru2 C1A 84.4(5) . . ? C2A Ru2 F2A 90.9(4) . . ? C1A Ru2 F2A 172.6(4) . . ? C2A Ru2 F1A 175.3(4) . . ? C1A Ru2 F1A 95.4(4) . . ? F2A Ru2 F1A 89.8(3) . . ? C2A Ru2 C3A 88.6(5) . . ? C1A Ru2 C3A 100.2(5) . . ? F2A Ru2 C3A 85.3(4) . . ? F1A Ru2 C3A 86.8(4) . . ? C2A Ru2 C30A 95.4(5) . . ? C1A Ru2 C30A 89.0(5) . . ? F2A Ru2 C30A 85.9(4) . . ? F1A Ru2 C30A 89.3(4) . . ? C3A Ru2 C30A 170.3(5) . . ? C6A N1A C3A 130.7(11) . . ? C6A N1A C4A 118.6(11) . . ? C3A N1A C4A 109.7(10) . . ? C5A N2A C3A 114.9(10) . . ? C5A N2A C18A 118.0(10) . . ? C3A N2A C18A 126.6(10) . . ? C30A N3A C31A 112.4(11) . . ? C30A N3A C33A 129.6(11) . . ? C31A N3A C33A 117.7(10) . . ? C30A N4A C45A 132.7(11) . . ? C30A N4A C32A 105.9(11) . . ? C45A N4A C32A 120.9(11) . . ? O1A C1A Ru2 164.2(10) . . ? O2A C2A Ru2 171.3(11) . . ? N2A C3A N1A 101.8(10) . . ? N2A C3A Ru2 133.3(8) . . ? N1A C3A Ru2 124.8(8) . . ? C5A C4A N1A 106.6(13) . . ? N2A C5A C4A 106.0(12) . . ? C11A C6A N1A 115.7(11) . . ? C11A C6A C7A 127.0(12) . . ? N1A C6A C7A 117.3(11) . . ? C8A C7A C12A 121.0(13) . . ? C8A C7A C6A 118.7(12) . . ? C12A C7A C6A 120.3(11) . . ? C7A C8A C9A 119.7(13) . . ? C10A C9A C8A 121.4(14) . . ? C9A C10A C11A 121.7(13) . . ? C6A C11A C10A 111.5(12) . . ? C6A C11A C15A 123.4(12) . . ? C10A C11A C15A 125.1(12) . . ? C7A C12A C13A 108.7(12) . . ? C7A C12A C14A 109.7(11) . . ? C13A C12A C14A 111.2(11) . . ? C16A C15A C11A 104.6(11) . . ? C16A C15A C17A 98.5(10) . . ? C11A C15A C17A 96.4(10) . . ? N2A C18A C19A 120.5(12) . . ? N2A C18A C23A 120.0(11) . . ? C19A C18A C23A 118.8(12) . . ? C18A C19A C20A 112.2(14) . . ? C18A C19A C24A 116.2(13) . . ? C20A C19A C24A 131.4(14) . . ? C21A C20A C19A 124.6(11) . . ? C22A C21A C20A 115.8(12) . . ? C21A C22A C23A 130.3(15) . . ? C22A C23A C18A 118.1(12) . . ? C22A C23A C27A 119.5(12) . . ? C18A C23A C27A 122.3(12) . . ? C25A C24A C19A 108.5(12) . . ? C25A C24A C26A 122.6(12) . . ? C19A C24A C26A 91.6(11) . . ? C23A C27A C29A 117.2(13) . . ? C23A C27A C28A 110.3(11) . . ? C29A C27A C28A 113.3(12) . . ? N3A C30A N4A 104.5(11) . . ? N3A C30A Ru2 126.8(10) . . ? N4A C30A Ru2 128.7(9) . . ? C32A C31A N3A 105.8(12) . . ? C31A C32A N4A 107.6(13) . . ? C34A C33A N3A 127.6(12) . . ? C34A C33A C38A 126.0(13) . . ? N3A C33A C38A 106.2(10) . . ? C33A C34A C35A 138.8(15) . . ? C33A C34A C39A 115.9(13) . . ? C35A C34A C39A 105.3(12) . . ? C36A C35A C34A 103.3(12) . . ? C35A C36A C37A 128.9(13) . . ? C36A C37A C38A 125.7(13) . . ? C42A C38A C33A 125.9(17) . . ? C42A C38A C37A 136.8(18) . . ? C33A C38A C37A 97.2(12) . . ? C42A C38A C42B 8(3) . . ? C33A C38A C42B 119(2) . . ? C37A C38A C42B 143(3) . . ? C41A C39A C40A 117.3(12) . . ? C41A C39A C34A 110.4(10) . . ? C40A C39A C34A 96.7(11) . . ? C38A C42A C43A 101.2(17) . . ? C38A C42A C44A 113.6(16) . . ? C43A C42A C44A 117.3(16) . . ? C43B C42B C44B 102(5) . . ? C43B C42B C38A 116(5) . . ? C44B C42B C38A 68(3) . . ? C50A C45A N4A 122.9(11) . . ? C50A C45A C46A 116.5(12) . . ? N4A C45A C46A 120.6(10) . . ? C47A C46A C45A 127.6(13) . . ? C47A C46A C51A 116.4(12) . . ? C45A C46A C51A 115.4(11) . . ? C46A C47A C48A 117.2(13) . . ? C47A C48A C49A 120.1(13) . . ? C48A C49A C50A 118.6(12) . . ? C45A C50A C49A 119.8(13) . . ? C45A C50A C54A 130.2(14) . . ? C49A C50A C54A 109.9(13) . . ? C53A C51A C52A 86.5(14) . . ? C53A C51A C46A 120.0(15) . . ? C52A C51A C46A 108.4(12) . . ? C53A C51A C53B 29.3(13) . . ? C52A C51A C53B 115.6(15) . . ? C46A C51A C53B 109.5(15) . . ? C56A C54A C55A 117(2) . . ? C56A C54A C50A 132(2) . . ? C55A C54A C50A 111.2(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.588 _refine_diff_density_min -1.230 _refine_diff_density_rms 0.147 # Attachment '05070ab.cif' data_05070ab _database_code_depnum_ccdc_archive 'CCDC 723425' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C40 H40 Cl2 N4 O2 Ru)2(C H Cl3)3(H2 O)' _chemical_formula_sum 'C42 H48 Cl8 N4 O5 Ru' _chemical_formula_weight 1073.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 30.931(6) _cell_length_b 20.639(3) _cell_length_c 16.117(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.708(11) _cell_angle_gamma 90.00 _cell_volume 9191(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 645 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 20.50 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4384 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; absorption correction based on 2730 reflections (SADABS); Rint 0.032 before correction and 0.026 after. ; _exptl_special_details ; The data crystal was lost during data collection, as a consequence data is only 87% complete. subsequent data collections were on inferior crystals and did not refine successfully. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11344 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.1415 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7725 _reflns_number_gt 4484 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disordered CHCL3 and H2O was omitted using the SQUEEZE option of PLATON.The solvent accessible voids are 2360.2 \%A3 with an estimated 1114e/cell to be added. Sixteen solvent CHCl3 molecules and twenty four H2O molecules /unit cell accounting for 1168e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34 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^)+(0.0461P)^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 7725 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1294 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.841 _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 0.362327(16) 0.84562(2) 0.81580(3) 0.02546(14) Uani 1 1 d . . . Cl1 Cl 0.37846(6) 0.92903(8) 0.93325(10) 0.0425(4) Uani 1 1 d . . . Cl2 Cl 0.27677(5) 0.87312(7) 0.72806(9) 0.0362(4) Uani 1 1 d . . . N1 N 0.38560(18) 0.7526(3) 0.9873(3) 0.0467(14) Uani 1 1 d . . . N2 N 0.31229(16) 0.7838(2) 0.9352(3) 0.0335(12) Uani 1 1 d . . . N4 N 0.36343(15) 0.8977(2) 0.6310(3) 0.0310(12) Uani 1 1 d . . . N3 N 0.38318(16) 0.9757(3) 0.7271(3) 0.0350(13) Uani 1 1 d . . . O1 O 0.46712(16) 0.8265(2) 0.8907(3) 0.0435(12) Uani 1 1 d . . . C1 C 0.4302(2) 0.8321(3) 0.8696(3) 0.0304(15) Uani 1 1 d . . . O2 O 0.33767(15) 0.7249(2) 0.7014(3) 0.0452(12) Uani 1 1 d . . . C2 C 0.34831(19) 0.7735(3) 0.7419(4) 0.0291(14) Uani 1 1 d . . . C3 C 0.35123(19) 0.7881(3) 0.9168(4) 0.0306(14) Uani 1 1 d . . . C4 C 0.3676(2) 0.7254(4) 1.0452(5) 0.072(3) Uani 1 1 d . . . H4 H 0.3844 0.6982 1.0976 0.087 Uiso 1 1 calc R . . C5 C 0.3217(2) 0.7456(3) 1.0112(4) 0.055(2) Uani 1 1 d . . . H5 H 0.2996 0.7354 1.0354 0.065 Uiso 1 1 calc R . . C6 C 0.4361(2) 0.7391(4) 1.0104(5) 0.055(2) Uani 1 1 d . . . C7 C 0.4463(3) 0.6867(4) 0.9674(5) 0.059(2) Uani 1 1 d . . . C8 C 0.4957(3) 0.6750(5) 0.9959(6) 0.089(3) Uani 1 1 d . . . H8 H 0.5046 0.6407 0.9676 0.107 Uiso 1 1 calc R . . C9 C 0.5308(3) 0.7107(4) 1.0619(6) 0.072(2) Uani 1 1 d . . . H9 H 0.5638 0.7017 1.0785 0.086 Uiso 1 1 calc R . . C10 C 0.5191(3) 0.7604(4) 1.1056(5) 0.060(2) Uani 1 1 d . . . H10 H 0.5443 0.7838 1.1540 0.072 Uiso 1 1 calc R . . C11 C 0.4712(2) 0.7767(3) 1.0800(5) 0.0482(18) Uani 1 1 d . . . C12 C 0.4087(3) 0.6448(4) 0.8991(5) 0.078(3) Uani 1 1 d . . . H12A H 0.3797 0.6463 0.9089 0.117 Uiso 1 1 calc R . . H12B H 0.4207 0.6001 0.9067 0.117 Uiso 1 1 calc R . . H12C H 0.4008 0.6599 0.8362 0.117 Uiso 1 1 calc R . . C13 C 0.4591(2) 0.8300(3) 1.1277(4) 0.059(2) Uani 1 1 d . . . H13A H 0.4889 0.8508 1.1727 0.088 Uiso 1 1 calc R . . H13B H 0.4414 0.8124 1.1602 0.088 Uiso 1 1 calc R . . H13C H 0.4389 0.8621 1.0818 0.088 Uiso 1 1 calc R . . C14 C 0.2620(2) 0.8035(3) 0.8801(4) 0.0314(15) Uani 1 1 d . . . C15 C 0.2319(2) 0.7610(3) 0.8115(4) 0.0364(15) Uani 1 1 d . . . C16 C 0.1833(2) 0.7786(4) 0.7645(4) 0.0491(19) Uani 1 1 d . . . H16 H 0.1614 0.7513 0.7166 0.059 Uiso 1 1 calc R . . C17 C 0.1658(2) 0.8355(5) 0.7861(5) 0.065(2) Uani 1 1 d . . . H17 H 0.1324 0.8459 0.7525 0.078 Uiso 1 1 calc R . . C18 C 0.1957(3) 0.8763(4) 0.8543(5) 0.058(2) Uani 1 1 d . . . H18 H 0.1832 0.9147 0.8682 0.069 Uiso 1 1 calc R . . C19 C 0.2451(2) 0.8611(3) 0.9038(4) 0.0426(17) Uani 1 1 d . . . C20 C 0.2510(3) 0.7005(3) 0.7917(5) 0.062(2) Uani 1 1 d . . . H20A H 0.2649 0.6735 0.8477 0.093 Uiso 1 1 calc R . . H20B H 0.2762 0.7109 0.7727 0.093 Uiso 1 1 calc R . . H20C H 0.2247 0.6769 0.7417 0.093 Uiso 1 1 calc R . . C21 C 0.2801(3) 0.9020(4) 0.9855(5) 0.081(3) Uani 1 1 d . . . H21A H 0.2623 0.9369 0.9977 0.121 Uiso 1 1 calc R . . H21B H 0.3048 0.9207 0.9703 0.121 Uiso 1 1 calc R . . H21C H 0.2957 0.8746 1.0408 0.121 Uiso 1 1 calc R . . C22 C 0.37129(19) 0.9099(3) 0.7199(4) 0.0267(14) Uani 1 1 d . . . C23 C 0.3826(2) 0.9987(3) 0.6469(4) 0.0384(16) Uani 1 1 d . . . H23 H 0.3898 1.0419 0.6366 0.046 Uiso 1 1 calc R . . C24 C 0.3707(2) 0.9518(3) 0.5880(4) 0.0383(16) Uani 1 1 d . . . H24 H 0.3675 0.9540 0.5266 0.046 Uiso 1 1 calc R . . C25 C 0.3975(2) 1.0196(3) 0.8052(3) 0.0288(14) Uani 1 1 d . . . C26 C 0.3623(2) 1.0555(3) 0.8135(4) 0.0376(15) Uani 1 1 d . . . C27 C 0.3781(2) 1.1034(3) 0.8829(4) 0.0395(16) Uani 1 1 d . . . H27 H 0.3549 1.1303 0.8896 0.047 Uiso 1 1 calc R . . C28 C 0.4264(3) 1.1121(3) 0.9413(5) 0.056(2) Uani 1 1 d . . . H28 H 0.4361 1.1434 0.9894 0.068 Uiso 1 1 calc R . . C29 C 0.4607(2) 1.0763(3) 0.9309(4) 0.053(2) Uani 1 1 d . . . H29 H 0.4940 1.0834 0.9711 0.064 Uiso 1 1 calc R . . C30 C 0.4470(2) 1.0291(3) 0.8612(4) 0.0409(17) Uani 1 1 d . . . C31 C 0.3098(2) 1.0435(3) 0.7531(4) 0.0418(16) Uani 1 1 d . . . H31A H 0.3034 0.9968 0.7495 0.063 Uiso 1 1 calc R . . H31B H 0.3009 1.0604 0.6907 0.063 Uiso 1 1 calc R . . H31C H 0.2907 1.0653 0.7794 0.063 Uiso 1 1 calc R . . C32 C 0.4851(2) 0.9886(4) 0.8472(4) 0.062(2) Uani 1 1 d . . . H32A H 0.4831 0.9433 0.8637 0.094 Uiso 1 1 calc R . . H32B H 0.5174 1.0056 0.8870 0.094 Uiso 1 1 calc R . . H32C H 0.4788 0.9910 0.7821 0.094 Uiso 1 1 calc R . . C33 C 0.3507(2) 0.8360(3) 0.5806(3) 0.0308(14) Uani 1 1 d . . . C34 C 0.3028(2) 0.8285(3) 0.5129(4) 0.0363(16) Uani 1 1 d . . . C35 C 0.2914(2) 0.7705(4) 0.4593(4) 0.054(2) Uani 1 1 d . . . H35 H 0.2591 0.7629 0.4136 0.064 Uiso 1 1 calc R . . C36 C 0.3268(3) 0.7257(4) 0.4734(4) 0.055(2) Uani 1 1 d . . . H36 H 0.3187 0.6869 0.4380 0.066 Uiso 1 1 calc R . . C37 C 0.3733(2) 0.7364(3) 0.5376(4) 0.0440(17) Uani 1 1 d . . . H37 H 0.3973 0.7050 0.5452 0.053 Uiso 1 1 calc R . . C38 C 0.3868(2) 0.7918(3) 0.5925(4) 0.0331(15) Uani 1 1 d . . . C39 C 0.2650(2) 0.8787(4) 0.4958(4) 0.057(2) Uani 1 1 d . . . H39A H 0.2710 0.9163 0.4653 0.085 Uiso 1 1 calc R . . H39B H 0.2661 0.8921 0.5550 0.085 Uiso 1 1 calc R . . H39C H 0.2330 0.8606 0.4557 0.085 Uiso 1 1 calc R . . C40 C 0.4393(2) 0.8013(3) 0.6632(4) 0.0457(17) Uani 1 1 d . . . H40A H 0.4477 0.8474 0.6667 0.069 Uiso 1 1 calc R . . H40B H 0.4603 0.7763 0.6443 0.069 Uiso 1 1 calc R . . H40C H 0.4438 0.7864 0.7243 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0207(2) 0.0324(3) 0.0203(2) 0.0000(3) 0.00665(17) -0.0040(2) Cl1 0.0529(10) 0.0433(11) 0.0344(8) -0.0019(8) 0.0222(8) -0.0115(8) Cl2 0.0264(7) 0.0447(11) 0.0344(8) 0.0085(7) 0.0109(7) -0.0003(7) N1 0.035(3) 0.052(4) 0.043(3) 0.018(3) 0.009(3) -0.003(3) N2 0.030(3) 0.042(4) 0.022(2) 0.006(2) 0.006(2) -0.005(2) N4 0.027(3) 0.033(3) 0.027(3) -0.003(2) 0.007(2) -0.003(2) N3 0.032(3) 0.047(4) 0.027(3) -0.004(3) 0.014(2) -0.005(3) O1 0.040(3) 0.056(3) 0.029(2) -0.002(2) 0.010(2) -0.010(2) C1 0.041(4) 0.033(4) 0.011(3) 0.002(3) 0.006(3) -0.008(3) O2 0.045(3) 0.039(3) 0.050(3) -0.007(2) 0.019(2) -0.006(2) C2 0.026(3) 0.025(4) 0.030(3) 0.007(3) 0.007(3) 0.004(3) C3 0.021(3) 0.037(4) 0.024(3) 0.001(3) 0.001(3) -0.008(3) C4 0.041(4) 0.118(7) 0.051(4) 0.046(5) 0.014(4) -0.007(5) C5 0.029(4) 0.076(6) 0.049(4) 0.035(4) 0.009(3) -0.003(4) C6 0.028(4) 0.085(6) 0.043(4) 0.029(4) 0.009(3) 0.004(4) C7 0.042(4) 0.059(6) 0.061(5) 0.025(4) 0.010(4) 0.012(4) C8 0.063(6) 0.132(9) 0.072(6) 0.019(6) 0.030(5) 0.031(6) C9 0.023(4) 0.103(8) 0.069(5) 0.001(5) 0.002(4) -0.004(4) C10 0.040(4) 0.082(6) 0.035(4) 0.012(4) -0.004(3) -0.006(4) C11 0.029(4) 0.061(5) 0.049(4) 0.002(4) 0.013(3) -0.004(4) C12 0.059(5) 0.042(6) 0.090(6) -0.003(5) -0.005(4) -0.007(4) C13 0.056(5) 0.075(6) 0.034(4) 0.011(4) 0.010(3) -0.001(4) C14 0.024(3) 0.040(4) 0.030(3) 0.014(3) 0.011(3) 0.005(3) C15 0.034(4) 0.031(4) 0.040(4) 0.000(3) 0.013(3) -0.012(3) C16 0.033(4) 0.072(6) 0.035(4) 0.008(4) 0.008(3) -0.018(4) C17 0.034(4) 0.114(8) 0.043(4) 0.038(5) 0.013(4) 0.022(5) C18 0.052(5) 0.077(6) 0.062(5) 0.022(5) 0.042(4) 0.014(4) C19 0.045(4) 0.051(5) 0.036(4) -0.004(3) 0.022(3) -0.020(4) C20 0.060(5) 0.041(5) 0.081(5) -0.026(4) 0.028(4) -0.029(4) C21 0.099(7) 0.082(6) 0.093(6) -0.024(5) 0.072(6) -0.006(5) C22 0.029(3) 0.027(4) 0.027(3) -0.010(3) 0.015(3) -0.011(3) C23 0.052(4) 0.041(5) 0.024(3) 0.005(3) 0.018(3) -0.004(3) C24 0.051(4) 0.041(5) 0.026(3) 0.007(3) 0.020(3) -0.004(3) C25 0.040(4) 0.029(4) 0.020(3) -0.001(3) 0.016(3) -0.010(3) C26 0.050(4) 0.032(4) 0.032(3) 0.012(3) 0.019(3) -0.002(4) C27 0.058(4) 0.032(4) 0.034(4) -0.008(3) 0.025(3) -0.004(3) C28 0.080(6) 0.050(5) 0.057(5) -0.027(4) 0.046(4) -0.025(4) C29 0.049(4) 0.074(6) 0.039(4) -0.024(4) 0.021(3) -0.030(4) C30 0.042(4) 0.054(5) 0.031(3) -0.008(3) 0.021(3) -0.020(3) C31 0.056(4) 0.026(4) 0.039(4) 0.004(3) 0.017(3) 0.004(3) C32 0.040(4) 0.111(7) 0.047(4) -0.018(4) 0.029(4) -0.016(4) C33 0.032(3) 0.035(4) 0.022(3) -0.008(3) 0.009(3) -0.012(3) C34 0.029(3) 0.050(5) 0.028(3) -0.004(3) 0.011(3) 0.000(3) C35 0.037(4) 0.089(6) 0.029(4) -0.014(4) 0.009(3) -0.023(4) C36 0.061(5) 0.067(6) 0.048(4) -0.034(4) 0.033(4) -0.023(4) C37 0.052(4) 0.045(5) 0.035(4) -0.009(3) 0.019(3) -0.004(4) C38 0.032(3) 0.043(5) 0.028(3) -0.003(3) 0.016(3) -0.002(3) C39 0.039(4) 0.092(6) 0.034(4) -0.008(4) 0.012(3) -0.006(4) C40 0.031(3) 0.071(5) 0.036(4) -0.003(4) 0.016(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 1.833(7) . ? Ru1 C1 1.899(6) . ? Ru1 C22 2.148(5) . ? Ru1 C3 2.163(5) . ? Ru1 Cl1 2.4386(16) . ? Ru1 Cl2 2.4416(15) . ? N1 C3 1.368(7) . ? N1 C4 1.403(7) . ? N1 C6 1.461(8) . ? N2 C3 1.366(6) . ? N2 C5 1.374(7) . ? N2 C14 1.459(6) . ? N4 C22 1.365(6) . ? N4 C24 1.385(7) . ? N4 C33 1.466(7) . ? N3 C23 1.370(6) . ? N3 C22 1.397(7) . ? N3 C25 1.448(6) . ? O1 C1 1.040(6) . ? O2 C2 1.161(6) . ? C4 C5 1.336(9) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.395(10) . ? C6 C11 1.395(9) . ? C7 C8 1.403(9) . ? C7 C12 1.471(9) . ? C8 C9 1.348(10) . ? C8 H8 0.9500 . ? C9 C10 1.381(10) . ? C9 H9 0.9500 . ? C10 C11 1.389(9) . ? C10 H10 0.9500 . ? C11 C13 1.485(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.391(8) . ? C14 C19 1.420(8) . ? C15 C16 1.395(8) . ? C15 C20 1.476(8) . ? C16 C17 1.401(10) . ? C16 H16 0.9500 . ? C17 C18 1.363(10) . ? C17 H17 0.9500 . ? C18 C19 1.406(9) . ? C18 H18 0.9500 . ? C19 C21 1.528(9) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 C24 1.289(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.374(8) . ? C25 C30 1.397(7) . ? C26 C27 1.406(8) . ? C26 C31 1.491(8) . ? C27 C28 1.373(9) . ? C27 H27 0.9500 . ? C28 C29 1.362(9) . ? C28 H28 0.9500 . ? C29 C30 1.401(8) . ? C29 H29 0.9500 . ? C30 C32 1.541(8) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C38 1.385(8) . ? C33 C34 1.401(7) . ? C34 C35 1.424(8) . ? C34 C39 1.491(8) . ? C35 C36 1.371(9) . ? C35 H35 0.9500 . ? C36 C37 1.362(8) . ? C36 H36 0.9500 . ? C37 C38 1.391(8) . ? C37 H37 0.9500 . ? C38 C40 1.520(7) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? 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 C2 Ru1 C1 93.9(2) . . ? C2 Ru1 C22 95.9(2) . . ? C1 Ru1 C22 86.9(2) . . ? C2 Ru1 C3 88.4(2) . . ? C1 Ru1 C3 95.3(2) . . ? C22 Ru1 C3 175.0(2) . . ? C2 Ru1 Cl1 169.76(17) . . ? C1 Ru1 Cl1 87.20(17) . . ? C22 Ru1 Cl1 94.30(15) . . ? C3 Ru1 Cl1 81.33(15) . . ? C2 Ru1 Cl2 86.22(17) . . ? C1 Ru1 Cl2 170.87(16) . . ? C22 Ru1 Cl2 84.05(14) . . ? C3 Ru1 Cl2 93.79(15) . . ? Cl1 Ru1 Cl2 94.35(6) . . ? C3 N1 C4 112.0(5) . . ? C3 N1 C6 131.1(5) . . ? C4 N1 C6 116.9(5) . . ? C3 N2 C5 112.1(5) . . ? C3 N2 C14 130.7(4) . . ? C5 N2 C14 116.3(4) . . ? C22 N4 C24 112.6(5) . . ? C22 N4 C33 128.3(5) . . ? C24 N4 C33 119.1(4) . . ? C23 N3 C22 111.5(5) . . ? C23 N3 C25 118.1(5) . . ? C22 N3 C25 130.3(4) . . ? O1 C1 Ru1 172.5(5) . . ? O2 C2 Ru1 172.7(5) . . ? N2 C3 N1 102.6(4) . . ? N2 C3 Ru1 130.7(4) . . ? N1 C3 Ru1 126.3(4) . . ? C5 C4 N1 105.6(6) . . ? C5 C4 H4 127.2 . . ? N1 C4 H4 127.2 . . ? C4 C5 N2 107.8(6) . . ? C4 C5 H5 126.1 . . ? N2 C5 H5 126.1 . . ? C7 C6 C11 124.2(7) . . ? C7 C6 N1 118.4(7) . . ? C11 C6 N1 117.1(7) . . ? C6 C7 C8 115.3(8) . . ? C6 C7 C12 123.3(7) . . ? C8 C7 C12 121.4(8) . . ? C9 C8 C7 122.5(9) . . ? C9 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C8 C9 C10 120.3(8) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 121.2(7) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 116.5(7) . . ? C10 C11 C13 120.7(7) . . ? C6 C11 C13 122.8(6) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 123.1(5) . . ? C15 C14 N2 117.2(5) . . ? C19 C14 N2 119.4(5) . . ? C14 C15 C16 116.2(6) . . ? C14 C15 C20 121.0(6) . . ? C16 C15 C20 122.9(6) . . ? C15 C16 C17 121.8(6) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C18 C17 C16 121.4(7) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 119.4(7) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C14 118.2(6) . . ? C18 C19 C21 122.4(7) . . ? C14 C19 C21 119.3(6) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 N3 100.6(4) . . ? N4 C22 Ru1 128.4(4) . . ? N3 C22 Ru1 130.9(4) . . ? C24 C23 N3 108.2(6) . . ? C24 C23 H23 125.9 . . ? N3 C23 H23 125.9 . . ? C23 C24 N4 107.1(5) . . ? C23 C24 H24 126.5 . . ? N4 C24 H24 126.5 . . ? C26 C25 C30 123.2(6) . . ? C26 C25 N3 118.4(5) . . ? C30 C25 N3 118.0(5) . . ? C25 C26 C27 116.7(6) . . ? C25 C26 C31 121.7(6) . . ? C27 C26 C31 121.6(6) . . ? C28 C27 C26 121.3(6) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C29 C28 C27 120.8(6) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.3(6) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 117.7(6) . . ? C25 C30 C32 121.0(5) . . ? C29 C30 C32 121.3(6) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C38 C33 C34 122.7(6) . . ? C38 C33 N4 119.8(5) . . ? C34 C33 N4 117.0(5) . . ? C33 C34 C35 116.9(6) . . ? C33 C34 C39 122.4(6) . . ? C35 C34 C39 120.8(6) . . ? C36 C35 C34 120.3(6) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 120.6(7) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 121.9(6) . . ? C36 C37 H37 119.0 . . ? C38 C37 H37 119.0 . . ? C33 C38 C37 117.4(5) . . ? C33 C38 C40 122.8(5) . . ? C37 C38 C40 119.8(5) . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N2 C3 N1 -2.0(6) . . . . ? C14 N2 C3 N1 -170.8(6) . . . . ? C5 N2 C3 Ru1 -174.5(5) . . . . ? C14 N2 C3 Ru1 16.8(9) . . . . ? C4 N1 C3 N2 2.1(7) . . . . ? C6 N1 C3 N2 -178.1(7) . . . . ? C4 N1 C3 Ru1 175.0(5) . . . . ? C6 N1 C3 Ru1 -5.2(10) . . . . ? C2 Ru1 C3 N2 -100.0(5) . . . . ? C1 Ru1 C3 N2 166.3(5) . . . . ? Cl1 Ru1 C3 N2 80.0(5) . . . . ? Cl2 Ru1 C3 N2 -13.9(5) . . . . ? C2 Ru1 C3 N1 89.2(5) . . . . ? C1 Ru1 C3 N1 -4.5(5) . . . . ? Cl1 Ru1 C3 N1 -90.8(5) . . . . ? Cl2 Ru1 C3 N1 175.3(5) . . . . ? C3 N1 C4 C5 -1.4(9) . . . . ? C6 N1 C4 C5 178.8(6) . . . . ? N1 C4 C5 N2 0.1(9) . . . . ? C3 N2 C5 C4 1.3(8) . . . . ? C14 N2 C5 C4 171.8(6) . . . . ? C3 N1 C6 C7 -86.1(9) . . . . ? C4 N1 C6 C7 93.8(8) . . . . ? C3 N1 C6 C11 98.8(8) . . . . ? C4 N1 C6 C11 -81.4(8) . . . . ? C11 C6 C7 C8 -2.7(10) . . . . ? N1 C6 C7 C8 -177.5(6) . . . . ? C11 C6 C7 C12 175.3(6) . . . . ? N1 C6 C7 C12 0.6(10) . . . . ? C6 C7 C8 C9 1.7(12) . . . . ? C12 C7 C8 C9 -176.4(8) . . . . ? C7 C8 C9 C10 1.0(13) . . . . ? C8 C9 C10 C11 -2.9(12) . . . . ? C9 C10 C11 C6 1.9(10) . . . . ? C9 C10 C11 C13 179.8(7) . . . . ? C7 C6 C11 C10 1.0(10) . . . . ? N1 C6 C11 C10 175.8(6) . . . . ? C7 C6 C11 C13 -176.8(6) . . . . ? N1 C6 C11 C13 -2.0(9) . . . . ? C3 N2 C14 C15 82.5(7) . . . . ? C5 N2 C14 C15 -85.8(6) . . . . ? C3 N2 C14 C19 -103.2(7) . . . . ? C5 N2 C14 C19 88.4(7) . . . . ? C19 C14 C15 C16 1.4(8) . . . . ? N2 C14 C15 C16 175.4(5) . . . . ? C19 C14 C15 C20 -177.9(6) . . . . ? N2 C14 C15 C20 -3.8(8) . . . . ? C14 C15 C16 C17 -0.8(9) . . . . ? C20 C15 C16 C17 178.5(6) . . . . ? C15 C16 C17 C18 0.0(10) . . . . ? C16 C17 C18 C19 0.2(9) . . . . ? C17 C18 C19 C14 0.4(8) . . . . ? C17 C18 C19 C21 -175.7(6) . . . . ? C15 C14 C19 C18 -1.2(8) . . . . ? N2 C14 C19 C18 -175.2(5) . . . . ? C15 C14 C19 C21 175.0(5) . . . . ? N2 C14 C19 C21 1.1(8) . . . . ? C24 N4 C22 N3 0.8(6) . . . . ? C33 N4 C22 N3 178.2(5) . . . . ? C24 N4 C22 Ru1 177.0(4) . . . . ? C33 N4 C22 Ru1 -5.6(8) . . . . ? C23 N3 C22 N4 -0.8(6) . . . . ? C25 N3 C22 N4 -177.5(5) . . . . ? C23 N3 C22 Ru1 -176.8(4) . . . . ? C25 N3 C22 Ru1 6.5(8) . . . . ? C2 Ru1 C22 N4 5.6(5) . . . . ? C1 Ru1 C22 N4 99.2(5) . . . . ? Cl1 Ru1 C22 N4 -173.9(5) . . . . ? Cl2 Ru1 C22 N4 -79.9(5) . . . . ? C2 Ru1 C22 N3 -179.4(5) . . . . ? C1 Ru1 C22 N3 -85.8(5) . . . . ? Cl1 Ru1 C22 N3 1.1(5) . . . . ? Cl2 Ru1 C22 N3 95.1(5) . . . . ? C22 N3 C23 C24 0.5(7) . . . . ? C25 N3 C23 C24 177.6(5) . . . . ? N3 C23 C24 N4 0.1(7) . . . . ? C22 N4 C24 C23 -0.6(7) . . . . ? C33 N4 C24 C23 -178.2(5) . . . . ? C23 N3 C25 C26 90.5(6) . . . . ? C22 N3 C25 C26 -92.9(7) . . . . ? C23 N3 C25 C30 -81.6(7) . . . . ? C22 N3 C25 C30 94.9(7) . . . . ? C30 C25 C26 C27 -0.3(8) . . . . ? N3 C25 C26 C27 -172.1(5) . . . . ? C30 C25 C26 C31 -179.3(5) . . . . ? N3 C25 C26 C31 8.9(8) . . . . ? C25 C26 C27 C28 -2.2(8) . . . . ? C31 C26 C27 C28 176.8(6) . . . . ? C26 C27 C28 C29 3.0(10) . . . . ? C27 C28 C29 C30 -1.2(10) . . . . ? C26 C25 C30 C29 2.0(9) . . . . ? N3 C25 C30 C29 173.8(5) . . . . ? C26 C25 C30 C32 -178.4(5) . . . . ? N3 C25 C30 C32 -6.7(8) . . . . ? C28 C29 C30 C25 -1.3(9) . . . . ? C28 C29 C30 C32 179.2(6) . . . . ? C22 N4 C33 C38 -83.0(7) . . . . ? C24 N4 C33 C38 94.3(6) . . . . ? C22 N4 C33 C34 105.2(6) . . . . ? C24 N4 C33 C34 -77.6(6) . . . . ? C38 C33 C34 C35 3.9(8) . . . . ? N4 C33 C34 C35 175.4(5) . . . . ? C38 C33 C34 C39 -175.2(5) . . . . ? N4 C33 C34 C39 -3.6(8) . . . . ? C33 C34 C35 C36 -1.4(9) . . . . ? C39 C34 C35 C36 177.7(6) . . . . ? C34 C35 C36 C37 -1.1(10) . . . . ? C35 C36 C37 C38 1.3(10) . . . . ? C34 C33 C38 C37 -3.7(8) . . . . ? N4 C33 C38 C37 -175.0(5) . . . . ? C34 C33 C38 C40 177.4(5) . . . . ? N4 C33 C38 C40 6.1(8) . . . . ? C36 C37 C38 C33 1.0(9) . . . . ? C36 C37 C38 C40 179.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.854 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.854 _refine_diff_density_max 0.634 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.096 # Attachment '05082.cif' data_05082 _database_code_depnum_ccdc_archive 'CCDC 723426' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H96 Cl4 N4 O4 Ru2' _chemical_formula_sum 'C70 H96 Cl4 N4 O4 Ru2' _chemical_formula_weight 1401.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 31.316(3) _cell_length_b 31.316(3) _cell_length_c 14.834(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14547(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 972 _cell_measurement_theta_min 2.713 _cell_measurement_theta_max 20.982 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5856 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.669 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; absorption correction based on 7302 reflections(SADABS);Rint 0.0304 before correction and 0.0224 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56148 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7156 _reflns_number_gt 5213 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0951P)^2^+39.8164P] 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 7156 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1159 _refine_ls_R_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.2085 _refine_ls_wR_factor_gt 0.1909 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _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 0.035173(15) 0.482785(15) 0.09166(4) 0.04576(19) Uani 1 1 d . . . Cl1 Cl 0.02168(5) 0.46555(6) -0.06721(12) 0.0616(5) Uani 1 1 d . . . Cl2 Cl 0.08479(6) 0.53761(6) 0.04134(15) 0.0725(5) Uani 1 1 d . . . O1 O 0.03134(19) 0.52386(19) 0.2732(4) 0.0873(18) Uani 1 1 d . . . O2 O -0.02705(18) 0.42210(19) 0.1482(5) 0.0747(19) Uani 1 1 d . . . N1 N 0.09972(16) 0.40946(16) 0.0534(3) 0.0485(12) Uani 1 1 d . . . N2 N 0.10812(16) 0.43367(16) 0.1872(3) 0.0472(12) Uani 1 1 d . . . C1 C 0.0362(2) 0.5057(2) 0.2084(6) 0.0620(18) Uani 1 1 d . . . C2 C -0.0077(3) 0.4397(3) 0.1304(6) 0.063(2) Uani 1 1 d . . . C3 C 0.08411(18) 0.43943(17) 0.1116(4) 0.0431(13) Uani 1 1 d . . . C4 C 0.1314(2) 0.3852(2) 0.0932(5) 0.0597(18) Uani 1 1 d . . . H4 H 0.1465 0.3620 0.0668 0.072 Uiso 1 1 calc R . . C5 C 0.1365(2) 0.4008(2) 0.1764(5) 0.0619(19) Uani 1 1 d . . . H5 H 0.1563 0.3908 0.2201 0.074 Uiso 1 1 calc R . . C6 C 0.0899(2) 0.40045(19) -0.0408(4) 0.0488(15) Uani 1 1 d . . . C7 C 0.1122(2) 0.4221(2) -0.1072(4) 0.0528(16) Uani 1 1 d . . . C8 C 0.1051(2) 0.4096(2) -0.1958(5) 0.0627(18) Uani 1 1 d . . . H8 H 0.1202 0.4238 -0.2424 0.075 Uiso 1 1 calc R . . C9 C 0.0771(2) 0.3779(3) -0.2187(5) 0.0669(19) Uani 1 1 d . . . C10 C 0.0556(2) 0.3574(2) -0.1502(5) 0.071(2) Uani 1 1 d . . . H10 H 0.0360 0.3354 -0.1655 0.085 Uiso 1 1 calc R . . C11 C 0.0612(2) 0.3678(2) -0.0587(5) 0.0575(17) Uani 1 1 d . . . C12 C 0.1435(2) 0.4574(2) -0.0865(5) 0.0576(17) Uani 1 1 d . . . H12 H 0.1373 0.4679 -0.0242 0.069 Uiso 1 1 calc R . . C13 C 0.1890(3) 0.4408(3) -0.0877(7) 0.096(3) Uani 1 1 d . . . H13A H 0.1917 0.4169 -0.0453 0.144 Uiso 1 1 calc R . . H13B H 0.2086 0.4637 -0.0700 0.144 Uiso 1 1 calc R . . H13C H 0.1962 0.4310 -0.1486 0.144 Uiso 1 1 calc R . . C14 C 0.1397(3) 0.4952(2) -0.1504(5) 0.079(2) Uani 1 1 d . . . H14A H 0.1472 0.4862 -0.2116 0.118 Uiso 1 1 calc R . . H14B H 0.1592 0.5179 -0.1309 0.118 Uiso 1 1 calc R . . H14C H 0.1103 0.5059 -0.1497 0.118 Uiso 1 1 calc R . . C15 C 0.0693(3) 0.3672(3) -0.3185(6) 0.088(3) Uani 1 1 d . . . H15 H 0.0919 0.3810 -0.3561 0.105 Uiso 1 1 calc R . . C16 C 0.0692(5) 0.3215(4) -0.3353(9) 0.150(5) Uiso 1 1 d . . . H16A H 0.0497 0.3075 -0.2930 0.225 Uiso 1 1 calc R . . H16B H 0.0981 0.3102 -0.3269 0.225 Uiso 1 1 calc R . . H16C H 0.0598 0.3160 -0.3972 0.225 Uiso 1 1 calc R . . C17 C 0.0264(3) 0.3841(4) -0.3462(6) 0.115(4) Uani 1 1 d . . . H17A H 0.0198 0.3743 -0.4073 0.172 Uiso 1 1 calc R . . H17B H 0.0269 0.4154 -0.3450 0.172 Uiso 1 1 calc R . . H17C H 0.0046 0.3737 -0.3043 0.172 Uiso 1 1 calc R . . C18 C 0.0356(2) 0.3451(2) 0.0130(6) 0.070(2) Uani 1 1 d . . . H18 H 0.0399 0.3601 0.0717 0.084 Uiso 1 1 calc R . . C19 C 0.0512(3) 0.2987(3) 0.0228(7) 0.093(3) Uani 1 1 d . . . H19A H 0.0470 0.2836 -0.0343 0.139 Uiso 1 1 calc R . . H19B H 0.0350 0.2844 0.0705 0.139 Uiso 1 1 calc R . . H19C H 0.0816 0.2987 0.0384 0.139 Uiso 1 1 calc R . . C20 C -0.0121(3) 0.3453(3) -0.0091(7) 0.090(3) Uani 1 1 d . . . H20A H -0.0210 0.3742 -0.0259 0.135 Uiso 1 1 calc R . . H20B H -0.0284 0.3359 0.0439 0.135 Uiso 1 1 calc R . . H20C H -0.0177 0.3257 -0.0594 0.135 Uiso 1 1 calc R . . C21 C 0.1046(2) 0.4558(2) 0.2723(4) 0.0481(14) Uani 1 1 d . . . C22 C 0.0793(2) 0.4374(2) 0.3394(4) 0.0550(16) Uani 1 1 d . . . C23 C 0.0769(2) 0.4587(2) 0.4219(5) 0.0653(19) Uani 1 1 d . . . H23 H 0.0591 0.4476 0.4680 0.078 Uiso 1 1 calc R . . C24 C 0.0996(3) 0.4954(3) 0.4383(5) 0.072(2) Uani 1 1 d . B . C25 C 0.1256(3) 0.5110(2) 0.3708(6) 0.071(2) Uani 1 1 d . . . H25 H 0.1422 0.5359 0.3825 0.086 Uiso 1 1 calc R . . C26 C 0.1286(2) 0.4922(2) 0.2872(5) 0.0585(17) Uani 1 1 d . . . C27 C 0.0560(3) 0.3956(2) 0.3273(5) 0.069(2) Uani 1 1 d . . . H27 H 0.0562 0.3885 0.2616 0.083 Uiso 1 1 calc R . . C28 C 0.0093(3) 0.3979(3) 0.3582(6) 0.090(3) Uani 1 1 d . . . H28A H 0.0082 0.4058 0.4221 0.134 Uiso 1 1 calc R . . H28B H -0.0043 0.3700 0.3497 0.134 Uiso 1 1 calc R . . H28C H -0.0059 0.4194 0.3224 0.134 Uiso 1 1 calc R . . C29 C 0.0791(3) 0.3599(3) 0.3769(7) 0.095(3) Uani 1 1 d . . . H29A H 0.1077 0.3561 0.3510 0.142 Uiso 1 1 calc R . . H29B H 0.0629 0.3333 0.3708 0.142 Uiso 1 1 calc R . . H29C H 0.0817 0.3673 0.4409 0.142 Uiso 1 1 calc R . . C30 C 0.0952(4) 0.5190(4) 0.5285(7) 0.105(3) Uani 1 1 d . . . H30 H 0.1252 0.5299 0.5264 0.126 Uiso 1 1 calc R A 1 C31 C 0.0770(5) 0.5612(4) 0.5117(10) 0.166(6) Uani 1 1 d . B . H31A H 0.0461 0.5604 0.5229 0.249 Uiso 1 1 calc R . . H31B H 0.0822 0.5694 0.4489 0.249 Uiso 1 1 calc R . . H31C H 0.0903 0.5821 0.5519 0.249 Uiso 1 1 calc R . . C32A C 0.1032(12) 0.4933(12) 0.6016(18) 0.162(19) Uani 0.50 1 d P B 1 H32A H 0.1328 0.4972 0.6211 0.242 Uiso 0.50 1 calc PR B 1 H32B H 0.0986 0.4634 0.5849 0.242 Uiso 0.50 1 calc PR B 1 H32C H 0.0839 0.5011 0.6510 0.242 Uiso 0.50 1 calc PR B 1 C32B C 0.0691(10) 0.4957(9) 0.6004(17) 0.111(10) Uani 0.50 1 d P B 2 H32D H 0.0395 0.4925 0.5796 0.166 Uiso 0.50 1 calc PR B 2 H32E H 0.0694 0.5123 0.6565 0.166 Uiso 0.50 1 calc PR B 2 H32F H 0.0815 0.4675 0.6114 0.166 Uiso 0.50 1 calc PR B 2 C33 C 0.1590(2) 0.5098(2) 0.2162(5) 0.0675(19) Uani 1 1 d . . . H33 H 0.1502 0.4987 0.1559 0.081 Uiso 1 1 calc R . . C34 C 0.1583(3) 0.5588(3) 0.2131(7) 0.092(3) Uani 1 1 d . . . H34A H 0.1288 0.5687 0.2063 0.139 Uiso 1 1 calc R . . H34B H 0.1754 0.5687 0.1618 0.139 Uiso 1 1 calc R . . H34C H 0.1704 0.5702 0.2692 0.139 Uiso 1 1 calc R . . C35 C 0.2043(3) 0.4948(4) 0.2356(7) 0.104(3) Uani 1 1 d . . . H35A H 0.2136 0.5057 0.2943 0.156 Uiso 1 1 calc R . . H35B H 0.2236 0.5054 0.1885 0.156 Uiso 1 1 calc R . . H35C H 0.2050 0.4635 0.2364 0.156 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0395(3) 0.0403(3) 0.0575(3) 0.0117(2) -0.0007(2) 0.0077(2) Cl1 0.0525(9) 0.0616(10) 0.0707(11) 0.0134(8) -0.0088(8) 0.0145(8) Cl2 0.0699(12) 0.0613(11) 0.0862(13) 0.0123(10) -0.0011(10) 0.0083(9) O1 0.094(4) 0.092(4) 0.076(4) -0.017(3) 0.000(3) 0.046(3) O2 0.048(3) 0.064(4) 0.113(5) 0.010(3) -0.024(3) 0.004(3) N1 0.052(3) 0.051(3) 0.042(3) -0.001(2) -0.011(2) 0.014(2) N2 0.050(3) 0.053(3) 0.039(3) 0.001(2) -0.008(2) 0.015(2) C1 0.060(4) 0.047(4) 0.079(5) 0.001(4) 0.001(4) 0.023(3) C2 0.056(5) 0.082(6) 0.052(4) 0.005(4) -0.008(4) 0.040(4) C3 0.043(3) 0.036(3) 0.050(4) 0.005(3) -0.002(3) 0.010(2) C4 0.061(4) 0.063(4) 0.055(4) -0.006(3) -0.009(3) 0.024(3) C5 0.060(4) 0.072(5) 0.054(4) 0.001(3) -0.015(3) 0.033(4) C6 0.053(4) 0.044(3) 0.050(4) -0.006(3) -0.012(3) 0.012(3) C7 0.058(4) 0.056(4) 0.044(4) -0.004(3) -0.008(3) 0.011(3) C8 0.076(5) 0.063(4) 0.050(4) 0.000(3) -0.007(3) 0.009(4) C9 0.067(5) 0.077(5) 0.056(4) -0.011(4) -0.016(4) 0.004(4) C10 0.067(5) 0.066(5) 0.078(5) -0.014(4) -0.022(4) -0.006(4) C11 0.054(4) 0.058(4) 0.061(4) 0.002(3) -0.011(3) 0.011(3) C12 0.070(4) 0.047(4) 0.056(4) -0.005(3) -0.005(3) 0.008(3) C13 0.076(6) 0.063(5) 0.149(9) -0.023(5) -0.015(6) 0.005(4) C14 0.102(6) 0.060(5) 0.074(5) 0.006(4) -0.009(5) -0.015(4) C15 0.112(7) 0.080(6) 0.070(5) -0.025(4) -0.022(5) 0.002(5) C17 0.112(8) 0.167(11) 0.066(6) -0.002(6) -0.029(5) 0.016(7) C18 0.052(4) 0.070(5) 0.088(6) 0.007(4) -0.008(4) -0.001(4) C19 0.074(6) 0.082(6) 0.123(8) 0.032(5) -0.001(5) 0.003(4) C20 0.063(5) 0.091(6) 0.116(7) 0.012(5) -0.012(5) -0.004(4) C21 0.053(4) 0.050(4) 0.041(3) -0.003(3) -0.008(3) 0.012(3) C22 0.064(4) 0.054(4) 0.047(4) -0.001(3) -0.007(3) 0.005(3) C23 0.078(5) 0.071(5) 0.046(4) -0.005(3) -0.004(3) 0.007(4) C24 0.080(5) 0.072(5) 0.064(5) -0.020(4) -0.008(4) 0.007(4) C25 0.076(5) 0.062(5) 0.077(5) -0.008(4) -0.015(4) -0.002(4) C26 0.061(4) 0.050(4) 0.065(4) 0.004(3) -0.008(3) 0.009(3) C27 0.085(5) 0.077(5) 0.046(4) -0.010(4) 0.008(4) -0.009(4) C28 0.102(7) 0.100(7) 0.067(5) 0.001(5) -0.001(5) -0.023(5) C29 0.121(8) 0.049(5) 0.114(7) -0.004(5) 0.009(6) 0.002(5) C30 0.114(8) 0.115(8) 0.086(7) -0.052(6) -0.018(6) 0.003(7) C31 0.228(16) 0.108(9) 0.162(13) -0.057(9) 0.064(11) 0.023(10) C32A 0.28(5) 0.17(3) 0.043(12) -0.023(15) -0.01(2) -0.12(4) C32B 0.19(3) 0.092(16) 0.050(12) -0.036(11) -0.010(18) 0.01(2) C33 0.066(5) 0.068(5) 0.069(5) 0.010(4) -0.002(4) 0.000(4) C34 0.101(7) 0.072(6) 0.104(7) 0.018(5) -0.005(6) -0.013(5) C35 0.068(6) 0.131(9) 0.114(8) 0.030(7) 0.005(5) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.875(8) . ? Ru1 C2 1.990(11) . ? Ru1 C3 2.069(5) . ? Ru1 Cl1 2.4327(16) 9_565 ? Ru1 Cl2 2.433(2) . ? Ru1 Cl1 2.454(2) . ? Cl1 Ru1 2.4327(16) 9_565 ? O1 C1 1.127(8) . ? O2 C2 0.859(9) . ? N1 C3 1.365(7) . ? N1 C4 1.382(8) . ? N1 C6 1.459(8) . ? N2 C3 1.362(7) . ? N2 C5 1.370(8) . ? N2 C21 1.444(8) . ? C4 C5 1.336(9) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.385(9) . ? C6 C11 1.387(9) . ? C7 C8 1.388(9) . ? C7 C12 1.510(9) . ? C8 C9 1.367(10) . ? C8 H8 0.9500 . ? C9 C10 1.378(11) . ? C9 C15 1.537(10) . ? C10 C11 1.407(10) . ? C10 H10 0.9500 . ? C11 C18 1.510(10) . ? C12 C13 1.517(10) . ? C12 C14 1.522(10) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.454(14) . ? C15 C17 1.499(13) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.530(10) . ? C18 C19 1.539(11) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.383(9) . ? C21 C22 1.396(9) . ? C22 C23 1.397(9) . ? C22 C27 1.510(10) . ? C23 C24 1.372(11) . ? C23 H23 0.9500 . ? C24 C25 1.380(11) . ? C24 C30 1.535(11) . ? C25 C26 1.377(10) . ? C25 H25 0.9500 . ? C26 C33 1.524(10) . ? C27 C29 1.521(11) . ? C27 C28 1.537(11) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32A 1.37(4) . ? C30 C31 1.461(16) . ? C30 C32B 1.53(3) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C33 C35 1.523(11) . ? C33 C34 1.534(11) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 90.2(3) . . ? C1 Ru1 C3 96.1(3) . . ? C2 Ru1 C3 90.8(3) . . ? C1 Ru1 Cl1 84.0(2) . 9_565 ? C2 Ru1 Cl1 90.0(2) . 9_565 ? C3 Ru1 Cl1 179.21(17) . 9_565 ? C1 Ru1 Cl2 90.2(2) . . ? C2 Ru1 Cl2 177.2(2) . . ? C3 Ru1 Cl2 91.95(17) . . ? Cl1 Ru1 Cl2 87.27(6) 9_565 . ? C1 Ru1 Cl1 166.95(19) . . ? C2 Ru1 Cl1 90.7(2) . . ? C3 Ru1 Cl1 96.93(17) . . ? Cl1 Ru1 Cl1 82.94(7) 9_565 . ? Cl2 Ru1 Cl1 88.31(7) . . ? Ru1 Cl1 Ru1 97.06(7) 9_565 . ? C3 N1 C4 111.4(5) . . ? C3 N1 C6 131.5(5) . . ? C4 N1 C6 117.0(5) . . ? C3 N2 C5 111.2(5) . . ? C3 N2 C21 127.9(5) . . ? C5 N2 C21 120.8(5) . . ? O1 C1 Ru1 168.0(6) . . ? O2 C2 Ru1 177.1(11) . . ? N2 C3 N1 103.4(4) . . ? N2 C3 Ru1 127.9(4) . . ? N1 C3 Ru1 128.8(4) . . ? C5 C4 N1 106.2(6) . . ? C5 C4 H4 126.9 . . ? N1 C4 H4 126.9 . . ? C4 C5 N2 107.8(5) . . ? C4 C5 H5 126.1 . . ? N2 C5 H5 126.1 . . ? C7 C6 C11 123.4(6) . . ? C7 C6 N1 118.7(6) . . ? C11 C6 N1 117.6(6) . . ? C6 C7 C8 117.1(6) . . ? C6 C7 C12 122.7(6) . . ? C8 C7 C12 120.2(6) . . ? C9 C8 C7 122.9(7) . . ? C9 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? C8 C9 C10 117.9(7) . . ? C8 C9 C15 120.0(8) . . ? C10 C9 C15 122.1(7) . . ? C9 C10 C11 122.9(7) . . ? C9 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C6 C11 C10 115.8(7) . . ? C6 C11 C18 123.8(6) . . ? C10 C11 C18 120.4(7) . . ? C7 C12 C13 110.9(6) . . ? C7 C12 C14 113.2(6) . . ? C13 C12 C14 109.4(7) . . ? C7 C12 H12 107.7 . . ? C13 C12 H12 107.7 . . ? C14 C12 H12 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C17 107.4(9) . . ? C16 C15 C9 112.2(9) . . ? C17 C15 C9 109.3(8) . . ? C16 C15 H15 109.3 . . ? C17 C15 H15 109.3 . . ? C9 C15 H15 109.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C11 C18 C20 111.5(7) . . ? C11 C18 C19 109.9(7) . . ? C20 C18 C19 109.6(7) . . ? C11 C18 H18 108.6 . . ? C20 C18 H18 108.6 . . ? C19 C18 H18 108.6 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 122.2(6) . . ? C26 C21 N2 119.6(6) . . ? C22 C21 N2 118.0(6) . . ? C21 C22 C23 117.3(6) . . ? C21 C22 C27 123.1(6) . . ? C23 C22 C27 119.6(6) . . ? C24 C23 C22 121.8(7) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 118.3(7) . . ? C23 C24 C30 120.7(9) . . ? C25 C24 C30 121.0(8) . . ? C26 C25 C24 122.7(7) . . ? C26 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? C25 C26 C21 117.5(7) . . ? C25 C26 C33 120.5(7) . . ? C21 C26 C33 121.9(6) . . ? C22 C27 C29 110.6(7) . . ? C22 C27 C28 112.5(6) . . ? C29 C27 C28 110.2(7) . . ? C22 C27 H27 107.8 . . ? C29 C27 H27 107.8 . . ? C28 C27 H27 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32A C30 C31 137.4(18) . . ? C32A C30 C32B 42.9(17) . . ? C31 C30 C32B 109.9(14) . . ? C32A C30 C24 112.9(16) . . ? C31 C30 C24 108.8(9) . . ? C32B C30 C24 115.3(12) . . ? C32A C30 H30 93.0 . . ? C31 C30 H30 93.0 . . ? C32B C30 H30 133.4 . . ? C24 C30 H30 93.0 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C35 C33 C26 109.9(6) . . ? C35 C33 C34 109.2(7) . . ? C26 C33 C34 112.0(7) . . ? C35 C33 H33 108.6 . . ? C26 C33 H33 108.6 . . ? C34 C33 H33 108.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ru1 Cl1 Ru1 -4.1(11) . . . 9_565 ? C2 Ru1 Cl1 Ru1 89.9(2) . . . 9_565 ? C3 Ru1 Cl1 Ru1 -179.21(17) . . . 9_565 ? Cl1 Ru1 Cl1 Ru1 0.0 9_565 . . 9_565 ? Cl2 Ru1 Cl1 Ru1 -87.46(7) . . . 9_565 ? C2 Ru1 C1 O1 -90(4) . . . . ? C3 Ru1 C1 O1 179(100) . . . . ? Cl1 Ru1 C1 O1 0(4) 9_565 . . . ? Cl2 Ru1 C1 O1 87(4) . . . . ? Cl1 Ru1 C1 O1 4(5) . . . . ? C1 Ru1 C2 O2 54(22) . . . . ? C3 Ru1 C2 O2 150(22) . . . . ? Cl1 Ru1 C2 O2 -30(22) 9_565 . . . ? Cl2 Ru1 C2 O2 -44(26) . . . . ? Cl1 Ru1 C2 O2 -113(22) . . . . ? C5 N2 C3 N1 -1.5(7) . . . . ? C21 N2 C3 N1 -177.6(6) . . . . ? C5 N2 C3 Ru1 177.7(5) . . . . ? C21 N2 C3 Ru1 1.5(9) . . . . ? C4 N1 C3 N2 1.9(7) . . . . ? C6 N1 C3 N2 -175.6(6) . . . . ? C4 N1 C3 Ru1 -177.3(5) . . . . ? C6 N1 C3 Ru1 5.3(10) . . . . ? C1 Ru1 C3 N2 -2.4(6) . . . . ? C2 Ru1 C3 N2 -92.7(6) . . . . ? Cl1 Ru1 C3 N2 96(13) 9_565 . . . ? Cl2 Ru1 C3 N2 88.0(5) . . . . ? Cl1 Ru1 C3 N2 176.5(5) . . . . ? C1 Ru1 C3 N1 176.6(6) . . . . ? C2 Ru1 C3 N1 86.3(6) . . . . ? Cl1 Ru1 C3 N1 -85(14) 9_565 . . . ? Cl2 Ru1 C3 N1 -93.0(5) . . . . ? Cl1 Ru1 C3 N1 -4.5(6) . . . . ? C3 N1 C4 C5 -1.6(8) . . . . ? C6 N1 C4 C5 176.3(6) . . . . ? N1 C4 C5 N2 0.6(8) . . . . ? C3 N2 C5 C4 0.6(8) . . . . ? C21 N2 C5 C4 177.0(6) . . . . ? C3 N1 C6 C7 87.9(8) . . . . ? C4 N1 C6 C7 -89.4(7) . . . . ? C3 N1 C6 C11 -97.8(8) . . . . ? C4 N1 C6 C11 84.9(7) . . . . ? C11 C6 C7 C8 -0.3(9) . . . . ? N1 C6 C7 C8 173.7(5) . . . . ? C11 C6 C7 C12 -179.6(6) . . . . ? N1 C6 C7 C12 -5.6(9) . . . . ? C6 C7 C8 C9 0.6(10) . . . . ? C12 C7 C8 C9 180.0(7) . . . . ? C7 C8 C9 C10 -0.4(11) . . . . ? C7 C8 C9 C15 177.1(7) . . . . ? C8 C9 C10 C11 -0.2(12) . . . . ? C15 C9 C10 C11 -177.6(7) . . . . ? C7 C6 C11 C10 -0.3(9) . . . . ? N1 C6 C11 C10 -174.3(6) . . . . ? C7 C6 C11 C18 -177.8(6) . . . . ? N1 C6 C11 C18 8.2(9) . . . . ? C9 C10 C11 C6 0.5(11) . . . . ? C9 C10 C11 C18 178.1(7) . . . . ? C6 C7 C12 C13 99.0(8) . . . . ? C8 C7 C12 C13 -80.3(9) . . . . ? C6 C7 C12 C14 -137.6(7) . . . . ? C8 C7 C12 C14 43.1(9) . . . . ? C8 C9 C15 C16 135.4(10) . . . . ? C10 C9 C15 C16 -47.2(13) . . . . ? C8 C9 C15 C17 -105.5(10) . . . . ? C10 C9 C15 C17 71.9(11) . . . . ? C6 C11 C18 C20 127.1(7) . . . . ? C10 C11 C18 C20 -50.2(10) . . . . ? C6 C11 C18 C19 -111.1(8) . . . . ? C10 C11 C18 C19 71.5(9) . . . . ? C3 N2 C21 C26 -91.7(8) . . . . ? C5 N2 C21 C26 92.5(8) . . . . ? C3 N2 C21 C22 93.3(8) . . . . ? C5 N2 C21 C22 -82.5(8) . . . . ? C26 C21 C22 C23 3.8(10) . . . . ? N2 C21 C22 C23 178.7(6) . . . . ? C26 C21 C22 C27 -174.3(6) . . . . ? N2 C21 C22 C27 0.7(9) . . . . ? C21 C22 C23 C24 -2.4(11) . . . . ? C27 C22 C23 C24 175.8(7) . . . . ? C22 C23 C24 C25 -0.5(12) . . . . ? C22 C23 C24 C30 177.9(8) . . . . ? C23 C24 C25 C26 2.2(12) . . . . ? C30 C24 C25 C26 -176.2(8) . . . . ? C24 C25 C26 C21 -0.8(11) . . . . ? C24 C25 C26 C33 -177.8(7) . . . . ? C22 C21 C26 C25 -2.3(10) . . . . ? N2 C21 C26 C25 -177.1(6) . . . . ? C22 C21 C26 C33 174.6(6) . . . . ? N2 C21 C26 C33 -0.2(9) . . . . ? C21 C22 C27 C29 103.7(8) . . . . ? C23 C22 C27 C29 -74.3(9) . . . . ? C21 C22 C27 C28 -132.7(7) . . . . ? C23 C22 C27 C28 49.3(9) . . . . ? C23 C24 C30 C32A 55(2) . . . . ? C25 C24 C30 C32A -126.7(19) . . . . ? C23 C24 C30 C31 -116.2(11) . . . . ? C25 C24 C30 C31 62.1(13) . . . . ? C23 C24 C30 C32B 7.8(18) . . . . ? C25 C24 C30 C32B -173.9(15) . . . . ? C25 C26 C33 C35 79.6(9) . . . . ? C21 C26 C33 C35 -97.3(8) . . . . ? C25 C26 C33 C34 -42.0(9) . . . . ? C21 C26 C33 C34 141.2(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.550 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.120 # Attachment '04113a.cif' data_04113a _database_code_depnum_ccdc_archive 'CCDC 723427' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C45 H48 B F4 N4 O3 Ru)+ (B F4)- 3(C H Cl3)' _chemical_formula_sum 'C48 H51 B2 Cl9 F8 N4 O3 Ru' _chemical_formula_weight 1325.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 16.372(2) _cell_length_b 14.6632(18) _cell_length_c 24.624(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5911.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 920 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 20.47 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ; absorption correction based on 13317 reflections (SADABS); Rint 0.047 before correction and 0.037 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35580 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 23.27 _reflns_number_total 4446 _reflns_number_gt 3729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+17.6559P] 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 4446 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1655 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 0.82231(3) 0.2500 0.79871(2) 0.0240(2) Uani 1 2 d S . . N1 N 0.8069(3) 0.0474(3) 0.75272(19) 0.0347(11) Uani 1 1 d . . . N2 N 0.8043(3) 0.0429(3) 0.83926(18) 0.0343(11) Uani 1 1 d . . . O1 O 0.9438(4) 0.2500 0.7022(2) 0.0399(14) Uani 1 2 d S . . O2 O 0.9675(3) 0.2500 0.8733(2) 0.0404(14) Uani 1 2 d S . . O3 O 0.7047(3) 0.2500 0.8975(2) 0.0380(13) Uani 1 2 d S . . C1 C 0.8140(3) 0.1019(4) 0.7970(2) 0.0314(13) Uani 1 1 d . . . C2 C 0.7924(4) -0.0425(4) 0.7676(3) 0.0464(16) Uani 1 1 d . . . H2 H 0.7854 -0.0917 0.7443 0.056 Uiso 1 1 calc R . . C3 C 0.7903(4) -0.0449(4) 0.8214(3) 0.0482(16) Uani 1 1 d . . . H3 H 0.7811 -0.0960 0.8429 0.058 Uiso 1 1 calc R . . C4 C 0.8984(5) 0.2500 0.7359(3) 0.0290(18) Uani 1 2 d S . . C5 C 0.9122(5) 0.2500 0.8446(3) 0.0312(18) Uani 1 2 d S . . C6 C 0.7472(5) 0.2500 0.8616(3) 0.0300(18) Uani 1 2 d S . . C7 C 0.8251(4) 0.0688(4) 0.6964(2) 0.0379(14) Uani 1 1 d . . . C8 C 0.9062(4) 0.0604(4) 0.6799(3) 0.0468(16) Uani 1 1 d . . . C9 C 0.9241(5) 0.0767(5) 0.6268(3) 0.068(2) Uani 1 1 d . . . H9 H 0.9782 0.0731 0.6156 0.082 Uiso 1 1 calc R . . C10 C 0.8651(7) 0.0983(6) 0.5892(3) 0.083(3) Uani 1 1 d . . . C11 C 0.7843(6) 0.1013(5) 0.6064(3) 0.069(2) Uani 1 1 d . . . H11 H 0.7438 0.1150 0.5813 0.083 Uiso 1 1 calc R . . C12 C 0.7618(4) 0.0841(4) 0.6607(2) 0.0470(16) Uani 1 1 d . . . C13 C 0.9729(4) 0.0322(5) 0.7187(3) 0.060(2) Uani 1 1 d . . . H13A H 0.9839 0.0813 0.7434 0.090 Uiso 1 1 d R . . H13B H 1.0215 0.0179 0.6987 0.090 Uiso 1 1 d R . . H13C H 0.9557 -0.0205 0.7388 0.090 Uiso 1 1 d R . . C14 C 0.8855(8) 0.1164(9) 0.5302(3) 0.137(5) Uani 1 1 d . . . H14A H 0.9151 0.0657 0.5154 0.205 Uiso 1 1 d R . . H14B H 0.9183 0.1705 0.5276 0.205 Uiso 1 1 d R . . H14C H 0.8357 0.1249 0.5103 0.205 Uiso 1 1 d R . . C15 C 0.6733(4) 0.0752(6) 0.6765(3) 0.062(2) Uani 1 1 d . . . H15A H 0.6523 0.0179 0.6638 0.094 Uiso 1 1 d R . . H15B H 0.6425 0.1242 0.6607 0.094 Uiso 1 1 d R . . H15C H 0.6688 0.0779 0.7154 0.094 Uiso 1 1 d R . . C16 C 0.8129(3) 0.0615(4) 0.8968(2) 0.0355(14) Uani 1 1 d . . . C17 C 0.8913(4) 0.0658(4) 0.9183(2) 0.0415(15) Uani 1 1 d . . . C18 C 0.8993(4) 0.0831(5) 0.9732(3) 0.0475(16) Uani 1 1 d . . . H18 H 0.9513 0.0883 0.9880 0.057 Uiso 1 1 calc R . . C19 C 0.8321(4) 0.0928(5) 1.0065(3) 0.0487(16) Uani 1 1 d . . . C20 C 0.7556(4) 0.0814(4) 0.9845(2) 0.0441(16) Uani 1 1 d . . . H20 H 0.7103 0.0857 1.0071 0.053 Uiso 1 1 calc R . . C21 C 0.7435(3) 0.0635(4) 0.9294(2) 0.0374(14) Uani 1 1 d . . . C22 C 0.9658(4) 0.0437(5) 0.8845(3) 0.0503(17) Uani 1 1 d . . . H22A H 0.9707 -0.0212 0.8808 0.075 Uiso 1 1 d R . . H22B H 1.0138 0.0674 0.9020 0.075 Uiso 1 1 d R . . H22C H 0.9604 0.0708 0.8492 0.075 Uiso 1 1 d R . . C23 C 0.8412(5) 0.1143(6) 1.0665(3) 0.064(2) Uani 1 1 d . . . H23A H 0.7897 0.1060 1.0844 0.096 Uiso 1 1 d R . . H23B H 0.8586 0.1765 1.0706 0.096 Uiso 1 1 d R . . H23C H 0.8811 0.0744 1.0823 0.096 Uiso 1 1 d R . . C24 C 0.6595(3) 0.0479(4) 0.9070(2) 0.0436(15) Uani 1 1 d . . . H24A H 0.6555 0.0741 0.8714 0.065 Uiso 1 1 d R . . H24B H 0.6201 0.0761 0.9305 0.065 Uiso 1 1 d R . . H24C H 0.6488 -0.0164 0.9050 0.065 Uiso 1 1 d R . . B1 B 0.6338(6) 0.2500 0.7661(4) 0.037(2) Uani 1 2 d S . . F1 F 0.7195(3) 0.2500 0.7456(2) 0.0492(13) Uani 1 2 d S . . F2 F 0.6228(2) 0.1725(3) 0.79686(13) 0.0473(9) Uani 1 1 d . . . F3 F 0.5811(3) 0.2500 0.72127(19) 0.0462(13) Uani 1 2 d S . . B2 B 0.6690(8) 0.7500 0.8772(5) 0.067(4) Uani 1 2 d S . . F4 F 0.7238(4) 0.7500 0.8360(3) 0.090(2) Uani 1 2 d S A . F5 F 0.6067(6) 0.8141(7) 0.8549(4) 0.081(3) Uani 0.50 1 d P A 1 F6 F 0.7071(6) 0.8191(6) 0.9143(4) 0.066(2) Uani 0.50 1 d P A 1 F7' F 0.6397(10) 0.8123(8) 0.8989(6) 0.121(5) Uani 0.50 1 d P A 2 C25 C 0.9359(8) 0.7500 0.5921(7) 0.106(5) Uani 1 2 d S . . H25 H 0.9954 0.7500 0.5969 0.128 Uiso 1 2 calc SR . . Cl1 Cl 0.9159(3) 0.7500 0.5191(2) 0.1306(16) Uani 1 2 d S . . Cl2 Cl 0.9011(3) 0.8502(2) 0.61476(17) 0.1688(18) Uani 1 1 d . . . C26 C 0.616(2) 0.7500 0.7299(9) 0.071(7) Uani 0.50 2 d SP . 1 Cl3 Cl 0.7101(4) 0.7500 0.69300(19) 0.0640(14) Uani 0.50 2 d SP . 1 C26' C 0.5541(18) 0.7500 0.7385(9) 0.062(6) Uani 0.50 2 d SP . 2 Cl3' Cl 0.4490(4) 0.7500 0.7369(3) 0.103(2) Uani 0.50 2 d SP . 2 Cl4 Cl 0.5803(3) 0.8478(3) 0.70921(19) 0.1728(17) Uani 1 1 d . . . H26 H 0.5930 0.7500 0.7715 0.207 Uiso 1 2 d SR . . C27 C 0.8658(6) 0.7500 0.9652(4) 0.058(3) Uani 1 2 d S . . H27 H 0.8057 0.7500 0.9437 0.069 Uiso 1 2 d SR . . Cl5 Cl 0.8607(3) 0.8631(3) 0.97102(18) 0.0767(12) Uani 0.50 1 d P . . Cl6 Cl 0.9364(3) 0.7160(4) 0.9151(2) 0.111(2) Uani 0.50 1 d P . . Cl7 Cl 0.8955(3) 0.7035(4) 1.0290(2) 0.1111(19) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0227(3) 0.0287(4) 0.0205(3) 0.000 -0.0020(3) 0.000 N1 0.034(3) 0.035(3) 0.035(3) -0.004(2) 0.004(2) -0.003(2) N2 0.039(3) 0.032(3) 0.031(3) 0.005(2) 0.000(2) -0.003(2) O1 0.039(3) 0.043(3) 0.038(3) 0.000 0.010(3) 0.000 O2 0.037(3) 0.051(4) 0.033(3) 0.000 -0.011(3) 0.000 O3 0.039(3) 0.044(3) 0.031(3) 0.000 0.006(3) 0.000 C1 0.022(3) 0.038(3) 0.034(3) -0.003(3) -0.004(2) -0.001(2) C2 0.050(4) 0.037(4) 0.052(4) -0.006(3) 0.001(3) -0.014(3) C3 0.057(4) 0.035(4) 0.053(4) 0.004(3) -0.001(3) -0.006(3) C4 0.028(4) 0.030(4) 0.029(5) 0.000 -0.006(4) 0.000 C5 0.028(4) 0.042(5) 0.023(4) 0.000 0.004(4) 0.000 C6 0.029(4) 0.026(4) 0.035(5) 0.000 -0.006(4) 0.000 C7 0.043(3) 0.035(3) 0.036(3) -0.005(3) 0.001(3) -0.010(3) C8 0.049(4) 0.047(4) 0.044(4) -0.016(3) 0.010(3) -0.013(3) C9 0.071(5) 0.076(5) 0.058(5) -0.036(4) 0.027(4) -0.042(4) C10 0.118(8) 0.088(6) 0.042(5) -0.033(4) 0.029(5) -0.060(6) C11 0.103(6) 0.069(5) 0.036(4) -0.012(4) -0.021(4) -0.026(5) C12 0.058(4) 0.048(4) 0.035(4) -0.012(3) -0.010(3) -0.011(3) C13 0.038(4) 0.051(4) 0.091(6) -0.011(4) 0.015(4) -0.002(3) C14 0.193(13) 0.173(12) 0.044(5) -0.008(6) 0.024(6) -0.105(10) C15 0.052(4) 0.073(5) 0.061(5) -0.025(4) -0.013(4) -0.003(4) C16 0.037(3) 0.034(3) 0.036(3) 0.010(3) -0.004(3) 0.002(3) C17 0.044(4) 0.042(4) 0.039(4) 0.015(3) -0.001(3) 0.004(3) C18 0.041(4) 0.055(4) 0.047(4) 0.013(3) -0.011(3) 0.003(3) C19 0.053(4) 0.048(4) 0.045(4) 0.013(3) -0.007(3) 0.003(3) C20 0.049(4) 0.048(4) 0.035(4) 0.012(3) 0.005(3) 0.007(3) C21 0.037(3) 0.035(3) 0.041(3) 0.014(3) 0.002(3) 0.006(3) C22 0.037(3) 0.053(4) 0.061(4) 0.010(3) 0.002(3) 0.011(3) C23 0.073(5) 0.078(5) 0.042(4) 0.010(4) -0.009(4) 0.000(4) C24 0.036(3) 0.050(4) 0.044(4) 0.010(3) 0.001(3) -0.001(3) B1 0.027(5) 0.058(7) 0.026(5) 0.000 -0.004(4) 0.000 F1 0.042(3) 0.061(3) 0.044(3) 0.000 -0.007(2) 0.000 F2 0.0366(19) 0.060(2) 0.045(2) 0.0112(18) -0.0042(15) -0.0080(17) F3 0.030(3) 0.068(3) 0.041(3) 0.000 -0.013(2) 0.000 B2 0.056(8) 0.105(12) 0.039(7) 0.000 0.010(6) 0.000 F4 0.102(5) 0.068(4) 0.098(5) 0.000 0.047(5) 0.000 F5 0.077(6) 0.107(7) 0.058(6) -0.010(5) -0.026(5) 0.021(5) F6 0.076(6) 0.056(5) 0.068(6) -0.010(4) -0.019(5) 0.008(5) F7' 0.148(13) 0.076(8) 0.137(12) -0.036(8) 0.047(11) 0.035(9) C25 0.073(9) 0.063(8) 0.183(16) 0.000 -0.039(10) 0.000 Cl1 0.100(3) 0.143(4) 0.150(4) 0.000 -0.010(3) 0.000 Cl2 0.207(4) 0.117(3) 0.183(4) -0.056(3) -0.078(3) 0.073(3) C26 0.12(2) 0.056(14) 0.033(12) 0.000 -0.013(15) 0.000 Cl3 0.085(4) 0.067(3) 0.039(3) 0.000 0.000(3) 0.000 C26' 0.093(18) 0.057(14) 0.037(12) 0.000 0.021(13) 0.000 Cl3' 0.078(4) 0.109(6) 0.122(6) 0.000 0.030(4) 0.000 Cl4 0.187(4) 0.101(2) 0.230(5) 0.049(3) 0.036(3) 0.023(2) C27 0.053(6) 0.054(6) 0.067(7) 0.000 -0.008(5) 0.000 Cl5 0.099(3) 0.047(2) 0.084(3) 0.002(2) 0.013(2) 0.010(2) Cl6 0.101(3) 0.123(5) 0.110(3) -0.052(3) 0.030(3) 0.006(3) Cl7 0.105(4) 0.122(4) 0.107(4) 0.058(3) -0.012(3) 0.030(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C5 1.857(8) . ? Ru1 C6 1.978(9) . ? Ru1 C4 1.986(8) . ? Ru1 F1 2.132(5) . ? Ru1 C1 2.177(6) . ? Ru1 C1 2.177(6) 7_565 ? N1 C1 1.358(7) . ? N1 C2 1.388(8) . ? N1 C7 1.452(7) . ? N2 C1 1.362(7) . ? N2 C3 1.380(8) . ? N2 C16 1.449(7) . ? O1 C4 1.113(9) . ? O2 C5 1.148(9) . ? O3 C6 1.124(9) . ? C2 C3 1.324(9) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C7 C12 1.379(8) . ? C7 C8 1.393(9) . ? C8 C9 1.361(9) . ? C8 C13 1.509(10) . ? C9 C10 1.375(12) . ? C9 H9 0.9300 . ? C10 C11 1.390(12) . ? C10 C14 1.513(10) . ? C11 C12 1.408(9) . ? C11 H11 0.9300 . ? C12 C15 1.506(9) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.391(8) . ? C16 C21 1.392(8) . ? C17 C18 1.380(9) . ? C17 C22 1.512(8) . ? C18 C19 1.381(9) . ? C18 H18 0.9300 . ? C19 C20 1.375(9) . ? C19 C23 1.518(9) . ? C20 C21 1.396(8) . ? C20 H20 0.9300 . ? C21 C24 1.500(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? B1 F2 1.378(6) . ? B1 F2 1.378(6) 7_565 ? B1 F3 1.402(10) . ? B1 F1 1.491(11) . ? B2 F7' 1.162(12) 7_575 ? B2 F7' 1.162(11) . ? B2 F4 1.354(14) . ? B2 F5 1.492(14) 7_575 ? B2 F5 1.492(14) . ? B2 F6 1.500(13) . ? B2 F6 1.500(13) 7_575 ? C25 Cl2 1.672(9) 7_575 ? C25 Cl2 1.672(9) . ? C25 Cl1 1.826(17) . ? C25 H25 0.9800 . ? C26 Cl4 1.633(13) 7_575 ? C26 Cl4 1.633(13) . ? C26 Cl3 1.78(3) . ? C26 H26 1.0930 . ? C26' Cl4 1.661(12) 7_575 ? C26' Cl4 1.661(12) . ? C26' Cl3' 1.72(3) . ? C26' H26 1.0317 . ? C27 Cl5 1.667(4) 7_575 ? C27 Cl5 1.667(4) . ? C27 Cl6 1.763(11) . ? C27 Cl6 1.763(11) 7_575 ? C27 Cl7 1.779(10) 7_575 ? C27 Cl7 1.779(10) . ? C27 H27 1.1164 . ? Cl5 Cl7 1.821(7) 7_575 ? Cl5 Cl6 2.185(7) 7_575 ? Cl6 Cl6 0.998(10) 7_575 ? Cl6 Cl5 2.185(7) 7_575 ? Cl7 Cl7 1.363(11) 7_575 ? Cl7 Cl5 1.821(7) 7_575 ? 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 C5 Ru1 C6 90.9(3) . . ? C5 Ru1 C4 88.7(3) . . ? C6 Ru1 C4 179.6(3) . . ? C5 Ru1 F1 179.7(3) . . ? C6 Ru1 F1 89.4(3) . . ? C4 Ru1 F1 91.0(3) . . ? C5 Ru1 C1 93.49(13) . . ? C6 Ru1 C1 88.63(14) . . ? C4 Ru1 C1 91.39(14) . . ? F1 Ru1 C1 86.52(13) . . ? C5 Ru1 C1 93.49(14) . 7_565 ? C6 Ru1 C1 88.63(14) . 7_565 ? C4 Ru1 C1 91.39(14) . 7_565 ? F1 Ru1 C1 86.52(13) . 7_565 ? C1 Ru1 C1 172.5(3) . 7_565 ? C1 N1 C2 111.2(5) . . ? C1 N1 C7 128.5(5) . . ? C2 N1 C7 119.5(5) . . ? C1 N2 C3 111.6(5) . . ? C1 N2 C16 128.0(5) . . ? C3 N2 C16 120.2(5) . . ? N1 C1 N2 103.3(5) . . ? N1 C1 Ru1 127.4(4) . . ? N2 C1 Ru1 128.8(4) . . ? C3 C2 N1 107.1(6) . . ? C3 C2 H2 126.4 . . ? N1 C2 H2 126.4 . . ? C2 C3 N2 106.8(6) . . ? C2 C3 H3 126.6 . . ? N2 C3 H3 126.6 . . ? O1 C4 Ru1 176.9(7) . . ? O2 C5 Ru1 179.6(6) . . ? O3 C6 Ru1 179.8(7) . . ? C12 C7 C8 123.0(6) . . ? C12 C7 N1 119.4(5) . . ? C8 C7 N1 117.1(5) . . ? C9 C8 C7 118.0(7) . . ? C9 C8 C13 120.0(7) . . ? C7 C8 C13 121.9(6) . . ? C8 C9 C10 122.5(7) . . ? C8 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? C9 C10 C11 118.0(7) . . ? C9 C10 C14 122.1(9) . . ? C11 C10 C14 119.9(10) . . ? C10 C11 C12 122.3(8) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C7 C12 C11 116.0(6) . . ? C7 C12 C15 122.9(6) . . ? C11 C12 C15 120.9(6) . . ? C8 C13 H13A 109.3 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.6 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 H14A 109.9 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.1 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.6 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.2 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 122.2(5) . . ? C17 C16 N2 118.2(5) . . ? C21 C16 N2 119.2(5) . . ? C18 C17 C16 118.0(6) . . ? C18 C17 C22 120.1(6) . . ? C16 C17 C22 121.6(5) . . ? C17 C18 C19 121.7(6) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C20 C19 C18 118.6(6) . . ? C20 C19 C23 119.9(6) . . ? C18 C19 C23 121.4(6) . . ? C19 C20 C21 122.4(6) . . ? C19 C20 H20 118.8 . . ? C21 C20 H20 118.8 . . ? C16 C21 C20 116.7(6) . . ? C16 C21 C24 122.3(5) . . ? C20 C21 C24 121.0(5) . . ? C17 C22 H22A 109.4 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.6 . . ? C19 C23 H23B 109.2 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.6 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.6 . . ? C21 C24 H24B 109.2 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.6 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F2 B1 F2 111.2(7) . 7_565 ? F2 B1 F3 110.6(5) . . ? F2 B1 F3 110.6(5) 7_565 . ? F2 B1 F1 108.0(5) . . ? F2 B1 F1 108.0(5) 7_565 . ? F3 B1 F1 108.2(6) . . ? B1 F1 Ru1 122.3(4) . . ? F7' B2 F7' 103.7(17) 7_575 . ? F7' B2 F4 128.1(8) 7_575 . ? F7' B2 F4 128.1(8) . . ? F7' B2 F5 52.5(10) 7_575 7_575 ? F7' B2 F5 112.5(14) . 7_575 ? F4 B2 F5 100.2(8) . 7_575 ? F7' B2 F5 112.5(14) 7_575 . ? F7' B2 F5 52.5(10) . . ? F4 B2 F5 100.2(8) . . ? F5 B2 F5 78.1(11) 7_575 . ? F7' B2 F6 115.0(13) 7_575 . ? F7' B2 F6 50.2(9) . . ? F4 B2 F6 100.4(9) . . ? F5 B2 F6 159.1(12) 7_575 . ? F5 B2 F6 94.7(6) . . ? F7' B2 F6 50.2(9) 7_575 7_575 ? F7' B2 F6 115.0(13) . 7_575 ? F4 B2 F6 100.4(9) . 7_575 ? F5 B2 F6 94.7(6) 7_575 7_575 ? F5 B2 F6 159.1(12) . 7_575 ? F6 B2 F6 85.0(10) . 7_575 ? Cl2 C25 Cl2 122.9(11) 7_575 . ? Cl2 C25 Cl1 105.5(6) 7_575 . ? Cl2 C25 Cl1 105.5(6) . . ? Cl2 C25 H25 107.4 7_575 . ? Cl2 C25 H25 107.4 . . ? Cl1 C25 H25 107.4 . . ? Cl4 C26 Cl4 122.8(17) 7_575 . ? Cl4 C26 Cl3 98.8(11) 7_575 . ? Cl4 C26 Cl3 98.8(11) . . ? Cl4 C26 H26 99.5 7_575 . ? Cl4 C26 H26 99.5 . . ? Cl3 C26 H26 141.3 . . ? Cl4 C26' Cl4 119.3(13) 7_575 . ? Cl4 C26' Cl3' 104.3(11) 7_575 . ? Cl4 C26' Cl3' 104.3(11) . . ? Cl4 C26' H26 100.5 7_575 . ? Cl4 C26' H26 100.5 . . ? Cl3' C26' H26 129.5 . . ? C26 Cl4 C26' 36.9(11) . . ? Cl5 C27 Cl5 168.6(8) 7_575 . ? Cl5 C27 Cl6 79.1(4) 7_575 . ? Cl5 C27 Cl6 112.0(5) . . ? Cl5 C27 Cl6 112.0(5) 7_575 7_575 ? Cl5 C27 Cl6 79.1(4) . 7_575 ? Cl6 C27 Cl6 32.9(4) . 7_575 ? Cl5 C27 Cl7 108.6(6) 7_575 7_575 ? Cl5 C27 Cl7 63.7(3) . 7_575 ? Cl6 C27 Cl7 123.2(6) . 7_575 ? Cl6 C27 Cl7 109.3(5) 7_575 7_575 ? Cl5 C27 Cl7 63.7(3) 7_575 . ? Cl5 C27 Cl7 108.6(6) . . ? Cl6 C27 Cl7 109.3(5) . . ? Cl6 C27 Cl7 123.2(6) 7_575 . ? Cl7 C27 Cl7 45.0(5) 7_575 . ? Cl5 C27 H27 89.8 7_575 . ? Cl5 C27 H27 89.8 . . ? Cl6 C27 H27 104.2 . . ? Cl6 C27 H27 104.2 7_575 . ? Cl7 C27 H27 131.2 7_575 . ? Cl7 C27 H27 131.2 . . ? C27 Cl5 Cl7 61.2(4) . 7_575 ? C27 Cl5 Cl6 52.4(4) . 7_575 ? Cl7 Cl5 Cl6 91.8(3) 7_575 7_575 ? Cl6 Cl6 C27 73.6(2) 7_575 . ? Cl6 Cl6 Cl5 122.04(16) 7_575 7_575 ? C27 Cl6 Cl5 48.50(19) . 7_575 ? Cl7 Cl7 C27 67.5(2) 7_575 . ? Cl7 Cl7 Cl5 122.44(19) 7_575 7_575 ? C27 Cl7 Cl5 55.1(2) . 7_575 ? 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 C2 N1 C1 N2 0.5(6) . . . . ? C7 N1 C1 N2 -168.7(5) . . . . ? C2 N1 C1 Ru1 -172.0(4) . . . . ? C7 N1 C1 Ru1 18.7(8) . . . . ? C3 N2 C1 N1 -0.9(6) . . . . ? C16 N2 C1 N1 174.2(5) . . . . ? C3 N2 C1 Ru1 171.5(4) . . . . ? C16 N2 C1 Ru1 -13.4(8) . . . . ? C5 Ru1 C1 N1 -131.1(5) . . . . ? C6 Ru1 C1 N1 138.1(5) . . . . ? C4 Ru1 C1 N1 -42.3(5) . . . . ? F1 Ru1 C1 N1 48.6(5) . . . . ? C1 Ru1 C1 N1 70(2) 7_565 . . . ? C5 Ru1 C1 N2 58.2(5) . . . . ? C6 Ru1 C1 N2 -32.6(5) . . . . ? C4 Ru1 C1 N2 147.0(5) . . . . ? F1 Ru1 C1 N2 -122.1(5) . . . . ? C1 Ru1 C1 N2 -101(2) 7_565 . . . ? C1 N1 C2 C3 0.0(7) . . . . ? C7 N1 C2 C3 170.4(5) . . . . ? N1 C2 C3 N2 -0.6(7) . . . . ? C1 N2 C3 C2 1.0(7) . . . . ? C16 N2 C3 C2 -174.5(5) . . . . ? C5 Ru1 C4 O1 0.00(3) . . . . ? C6 Ru1 C4 O1 0.0(2) . . . . ? F1 Ru1 C4 O1 180.00(3) . . . . ? C1 Ru1 C4 O1 -93.46(14) . . . . ? C1 Ru1 C4 O1 93.46(14) 7_565 . . . ? C6 Ru1 C5 O2 0(3) . . . . ? C4 Ru1 C5 O2 180(100) . . . . ? F1 Ru1 C5 O2 180(100) . . . . ? C1 Ru1 C5 O2 -89(3) . . . . ? C1 Ru1 C5 O2 89(3) 7_565 . . . ? C5 Ru1 C6 O3 0(100) . . . . ? C4 Ru1 C6 O3 0(100) . . . . ? F1 Ru1 C6 O3 180(100) . . . . ? C1 Ru1 C6 O3 93(100) . . . . ? C1 Ru1 C6 O3 -93(100) 7_565 . . . ? C1 N1 C7 C12 -105.1(7) . . . . ? C2 N1 C7 C12 86.4(7) . . . . ? C1 N1 C7 C8 83.5(7) . . . . ? C2 N1 C7 C8 -85.0(7) . . . . ? C12 C7 C8 C9 6.3(10) . . . . ? N1 C7 C8 C9 177.5(6) . . . . ? C12 C7 C8 C13 -172.3(6) . . . . ? N1 C7 C8 C13 -1.1(9) . . . . ? C7 C8 C9 C10 -1.9(11) . . . . ? C13 C8 C9 C10 176.7(7) . . . . ? C8 C9 C10 C11 -1.5(12) . . . . ? C8 C9 C10 C14 179.9(8) . . . . ? C9 C10 C11 C12 0.8(12) . . . . ? C14 C10 C11 C12 179.4(8) . . . . ? C8 C7 C12 C11 -6.9(9) . . . . ? N1 C7 C12 C11 -177.8(6) . . . . ? C8 C7 C12 C15 167.8(6) . . . . ? N1 C7 C12 C15 -3.1(9) . . . . ? C10 C11 C12 C7 3.3(10) . . . . ? C10 C11 C12 C15 -171.6(7) . . . . ? C1 N2 C16 C17 -78.7(7) . . . . ? C3 N2 C16 C17 96.0(7) . . . . ? C1 N2 C16 C21 108.9(6) . . . . ? C3 N2 C16 C21 -76.3(7) . . . . ? C21 C16 C17 C18 -7.6(9) . . . . ? N2 C16 C17 C18 -179.7(5) . . . . ? C21 C16 C17 C22 166.8(6) . . . . ? N2 C16 C17 C22 -5.3(8) . . . . ? C16 C17 C18 C19 2.2(10) . . . . ? C22 C17 C18 C19 -172.2(6) . . . . ? C17 C18 C19 C20 2.6(10) . . . . ? C17 C18 C19 C23 -178.3(6) . . . . ? C18 C19 C20 C21 -2.3(10) . . . . ? C23 C19 C20 C21 178.6(6) . . . . ? C17 C16 C21 C20 7.7(9) . . . . ? N2 C16 C21 C20 179.8(5) . . . . ? C17 C16 C21 C24 -172.7(6) . . . . ? N2 C16 C21 C24 -0.6(8) . . . . ? C19 C20 C21 C16 -2.7(9) . . . . ? C19 C20 C21 C24 177.7(6) . . . . ? F2 B1 F1 Ru1 -60.2(5) . . . . ? F2 B1 F1 Ru1 60.2(5) 7_565 . . . ? F3 B1 F1 Ru1 180.000(2) . . . . ? C5 Ru1 F1 B1 180.00(18) . . . . ? C6 Ru1 F1 B1 0.000(2) . . . . ? C4 Ru1 F1 B1 180.000(2) . . . . ? C1 Ru1 F1 B1 88.66(14) . . . . ? C1 Ru1 F1 B1 -88.66(14) 7_565 . . . ? Cl4 C26 Cl4 C26' 56(2) 7_575 . . . ? Cl3 C26 Cl4 C26' 162(2) . . . . ? Cl4 C26' Cl4 C26 -51.8(16) 7_575 . . . ? Cl3' C26' Cl4 C26 -168(2) . . . . ? Cl5 C27 Cl5 Cl7 50(4) 7_575 . . 7_575 ? Cl6 C27 Cl5 Cl7 -117.3(7) . . . 7_575 ? Cl6 C27 Cl5 Cl7 -118.0(5) 7_575 . . 7_575 ? Cl7 C27 Cl5 Cl7 3.5(3) . . . 7_575 ? Cl5 C27 Cl5 Cl6 168(4) 7_575 . . 7_575 ? Cl6 C27 Cl5 Cl6 0.7(3) . . . 7_575 ? Cl7 C27 Cl5 Cl6 118.0(5) 7_575 . . 7_575 ? Cl7 C27 Cl5 Cl6 121.5(7) . . . 7_575 ? Cl5 C27 Cl6 Cl6 -178.7(4) 7_575 . . 7_575 ? Cl5 C27 Cl6 Cl6 -1.4(5) . . . 7_575 ? Cl7 C27 Cl6 Cl6 -73.5(3) 7_575 . . 7_575 ? Cl7 C27 Cl6 Cl6 -121.8(4) . . . 7_575 ? Cl5 C27 Cl6 Cl5 177.4(9) . . . 7_575 ? Cl6 C27 Cl6 Cl5 178.7(4) 7_575 . . 7_575 ? Cl7 C27 Cl6 Cl5 105.2(6) 7_575 . . 7_575 ? Cl7 C27 Cl6 Cl5 57.0(3) . . . 7_575 ? Cl5 C27 Cl7 Cl7 -175.3(4) 7_575 . . 7_575 ? Cl5 C27 Cl7 Cl7 -4.4(4) . . . 7_575 ? Cl6 C27 Cl7 Cl7 118.0(5) . . . 7_575 ? Cl6 C27 Cl7 Cl7 84.5(4) 7_575 . . 7_575 ? Cl5 C27 Cl7 Cl5 170.9(8) . . . 7_575 ? Cl6 C27 Cl7 Cl5 -66.7(3) . . . 7_575 ? Cl6 C27 Cl7 Cl5 -100.2(5) 7_575 . . 7_575 ? Cl7 C27 Cl7 Cl5 175.3(4) 7_575 . . 7_575 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.307 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.093 # Attachment '04198.cif' data_04198 _database_code_depnum_ccdc_archive 'CCDC 723428' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C58 H72 Cl3 N4 O4 Ru2)(F )4(C H2 Cl2)' _chemical_formula_sum 'C62 H80 Cl11 F N4 O4 Ru2' _chemical_formula_weight 1556.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.11(2) _cell_length_b 34.04(5) _cell_length_c 15.18(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.74(3) _cell_angle_gamma 90.00 _cell_volume 7161(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 958 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 21.43 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 0.880 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; absorption correction based on 12956 rerflections (SADABS); Rint 0.051 before correction and 0.032 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14063 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0976 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14063 _reflns_number_gt 6773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disordered CH2Cl2 was omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 1595.6 \%A3 with an estimated 693e/cell to be added. Sixteen solvent CH2Cl2 molecules/unit cell accounting for 672e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46,C-34. 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^)+(0.0958P)^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 14063 _refine_ls_number_parameters 651 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1714 _refine_ls_wR_factor_gt 0.1576 _refine_ls_goodness_of_fit_ref 0.838 _refine_ls_restrained_S_all 0.838 _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 0.68067(4) 0.132108(12) 0.94963(3) 0.06072(18) Uani 1 1 d . . . Ru2 Ru 0.60499(4) 0.154543(12) 0.73768(3) 0.05820(18) Uani 1 1 d . . . Cl1 Cl 0.73269(11) 0.18351(3) 0.85776(9) 0.0571(4) Uani 1 1 d . . . Cl2 Cl 0.51790(12) 0.15039(4) 0.86248(10) 0.0683(5) Uani 1 1 d . . . Cl3 Cl 0.67995(15) 0.09481(4) 0.81027(10) 0.0817(6) Uani 1 1 d . . . N1 N 0.8879(5) 0.09433(14) 0.9974(4) 0.086(2) Uani 1 1 d . . . N2 N 0.8660(4) 0.13504(15) 1.0992(3) 0.0750(17) Uani 1 1 d . . . N3 N 0.4786(6) 0.09130(16) 0.6195(4) 0.103(2) Uani 1 1 d . . . N4 N 0.4252(5) 0.14926(18) 0.5840(4) 0.0805(18) Uani 1 1 d . . . O1 O 0.6033(4) 0.06706(12) 1.0500(3) 0.0958(17) Uani 1 1 d . . . O2 O 0.6191(3) 0.18949(11) 1.0781(3) 0.0678(11) Uani 1 1 d . . . O3 O 0.5543(3) 0.24016(11) 0.7118(3) 0.0656(11) Uani 1 1 d . . . O4 O 0.7273(3) 0.15978(12) 0.5953(3) 0.0750(13) Uani 1 1 d . . . C1 C 0.6335(5) 0.09122(17) 1.0123(4) 0.076(2) Uani 1 1 d . . . C2 C 0.6496(4) 0.16776(16) 1.0357(4) 0.0563(16) Uani 1 1 d . . . C3 C 0.8206(5) 0.12030(16) 1.0187(4) 0.070(2) Uani 1 1 d . . . C4 C 0.9680(7) 0.0932(2) 1.0644(6) 0.116(3) Uani 1 1 d . . . H4 H 1.0222 0.0766 1.0654 0.139 Uiso 1 1 calc R . . C5 C 0.9577(6) 0.1193(2) 1.1285(5) 0.099(3) Uani 1 1 d . . . H5 H 1.0026 0.1255 1.1815 0.119 Uiso 1 1 calc R . . C6 C 0.5642(4) 0.20675(17) 0.7129(3) 0.0533(14) Uani 1 1 d . . . C7 C 0.6800(5) 0.15700(15) 0.6486(4) 0.0597(16) Uani 1 1 d . . . C8 C 0.4957(6) 0.13008(18) 0.6431(4) 0.074(2) Uani 1 1 d . . . C9 C 0.3997(7) 0.0884(3) 0.5480(5) 0.116(4) Uani 1 1 d . . . H9 H 0.3734 0.0646 0.5214 0.139 Uiso 1 1 calc R . . C10 C 0.3682(7) 0.1234(3) 0.5237(5) 0.108(3) Uani 1 1 d . . . H10 H 0.3175 0.1301 0.4756 0.129 Uiso 1 1 calc R . . C11 C 0.8833(6) 0.06929(17) 0.9165(5) 0.093(3) Uani 1 1 d . . . C12A C 0.9304(6) 0.08326(18) 0.8501(5) 0.088(2) Uani 1 1 d . . . C13 C 0.9384(6) 0.0568(2) 0.7806(5) 0.111(3) Uani 1 1 d . . . H13 H 0.9694 0.0648 0.7331 0.133 Uiso 1 1 calc R . . C14 C 0.9017(7) 0.0198(2) 0.7815(7) 0.146(4) Uani 1 1 d . . . H14 H 0.9077 0.0024 0.7339 0.175 Uiso 1 1 calc R . . C15 C 0.8568(8) 0.0068(2) 0.8483(6) 0.148(4) Uani 1 1 d . . . H15 H 0.8328 -0.0193 0.8467 0.177 Uiso 1 1 calc R . . C16 C 0.8460(7) 0.03137(18) 0.9180(5) 0.116(3) Uani 1 1 d . . . C17 C 0.9758(6) 0.12348(18) 0.8507(4) 0.092(3) Uani 1 1 d . . . H17 H 0.9537 0.1390 0.8990 0.110 Uiso 1 1 calc R . . C18 C 1.0873(7) 0.1225(2) 0.8728(6) 0.128(3) Uani 1 1 d . . . H18A H 1.1057 0.1057 0.9256 0.191 Uiso 1 1 d R . . H18B H 1.1103 0.1493 0.8874 0.191 Uiso 1 1 d R . . H18C H 1.1163 0.1124 0.8235 0.191 Uiso 1 1 d R . . C19 C 0.9406(6) 0.14567(19) 0.7605(4) 0.090(2) Uani 1 1 d . . . H19A H 0.9571 0.1736 0.7662 0.135 Uiso 1 1 d R . . H19B H 0.8704 0.1427 0.7450 0.135 Uiso 1 1 d R . . H19C H 0.9703 0.1340 0.7133 0.135 Uiso 1 1 d R . . C20 C 0.7973(9) 0.0154(2) 0.9944(7) 0.164(6) Uani 1 1 d . . . H20 H 0.7837 0.0384 1.0310 0.197 Uiso 1 1 calc R . . C21 C 0.7031(11) -0.0050(2) 0.9615(8) 0.212(8) Uani 1 1 d . . . H21A H 0.7144 -0.0324 0.9464 0.319 Uiso 1 1 d R . . H21B H 0.6689 0.0087 0.9081 0.319 Uiso 1 1 d R . . H21C H 0.6640 -0.0042 1.0086 0.319 Uiso 1 1 d R . . C22 C 0.8723(10) -0.0112(4) 1.0562(9) 0.292(11) Uani 1 1 d . . . H22A H 0.8568 -0.0389 1.0430 0.438 Uiso 1 1 d R . . H22B H 0.8697 -0.0058 1.1191 0.438 Uiso 1 1 d R . . H22C H 0.9373 -0.0056 1.0453 0.438 Uiso 1 1 d R . . C23 C 0.8308(5) 0.16461(17) 1.1545(4) 0.0663(18) Uani 1 1 d . . . C24 C 0.7854(5) 0.15178(18) 1.2232(4) 0.0698(18) Uani 1 1 d . . . C25 C 0.7588(5) 0.17992(19) 1.2804(4) 0.0730(18) Uani 1 1 d . . . H25 H 0.7263 0.1724 1.3272 0.088 Uiso 1 1 calc R . . C26 C 0.7796(5) 0.2181(2) 1.2686(4) 0.077(2) Uani 1 1 d . . . H26 H 0.7620 0.2372 1.3084 0.093 Uiso 1 1 calc R . . C27 C 0.8246(5) 0.23014(19) 1.2022(5) 0.078(2) Uani 1 1 d . . . H27 H 0.8377 0.2573 1.1967 0.094 Uiso 1 1 calc R . . C28 C 0.8525(5) 0.20361(19) 1.1410(4) 0.0727(19) Uani 1 1 d . . . C29 C 0.7665(6) 0.10894(18) 1.2410(4) 0.085(2) Uani 1 1 d . . . H29 H 0.7725 0.0939 1.1857 0.103 Uiso 1 1 calc R . . C30 C 0.6628(7) 0.1036(2) 1.2563(5) 0.111(3) Uani 1 1 d . . . H30A H 0.6648 0.1024 1.3211 0.166 Uiso 1 1 d R . . H30B H 0.6326 0.0796 1.2281 0.166 Uiso 1 1 d R . . H30C H 0.6252 0.1265 1.2313 0.166 Uiso 1 1 d R . . C31 C 0.8401(8) 0.0920(2) 1.3178(5) 0.141(4) Uani 1 1 d . . . H31A H 0.8927 0.0804 1.2925 0.212 Uiso 1 1 d R . . H31B H 0.8131 0.0721 1.3528 0.212 Uiso 1 1 d R . . H31C H 0.8649 0.1141 1.3568 0.212 Uiso 1 1 d R . . C32 C 0.9087(5) 0.2157(2) 1.0677(5) 0.082(2) Uani 1 1 d . . . H32 H 0.9040 0.1940 1.0227 0.098 Uiso 1 1 calc R . . C33 C 1.0155(6) 0.2214(3) 1.1110(7) 0.151(4) Uani 1 1 d . . . H33A H 1.0270 0.2497 1.1176 0.227 Uiso 1 1 d R . . H33B H 1.0601 0.2100 1.0756 0.227 Uiso 1 1 d R . . H33C H 1.0260 0.2091 1.1704 0.227 Uiso 1 1 d R . . C34 C 0.8702(5) 0.2536(2) 1.0188(5) 0.092(2) Uani 1 1 d . . . H34A H 0.8007 0.2515 0.9959 0.138 Uiso 1 1 d R . . H34B H 0.9037 0.2584 0.9688 0.138 Uiso 1 1 d R . . H34C H 0.8826 0.2754 1.0616 0.138 Uiso 1 1 d R . . C35 C 0.5258(7) 0.05631(18) 0.6595(5) 0.104(3) Uani 1 1 d . . . C36 C 0.6041(7) 0.04063(18) 0.6254(5) 0.118(4) Uani 1 1 d . . . C37 C 0.6408(9) 0.0041(2) 0.6576(6) 0.163(5) Uani 1 1 d . . . H37 H 0.6940 -0.0073 0.6367 0.196 Uiso 1 1 calc R . . C38 C 0.5978(9) -0.01513(19) 0.7208(6) 0.158(5) Uani 1 1 d . . . H38 H 0.6216 -0.0401 0.7426 0.189 Uiso 1 1 calc R . . C39 C 0.5214(9) 0.0012(2) 0.7526(5) 0.140(4) Uani 1 1 d . . . H39 H 0.4945 -0.0128 0.7962 0.168 Uiso 1 1 calc R . . C40 C 0.4828(8) 0.0367(2) 0.7239(5) 0.118(3) Uani 1 1 d . . . C41 C 0.4009(7) 0.0529(2) 0.7604(5) 0.116(3) Uani 1 1 d . . . H41 H 0.3914 0.0809 0.7404 0.139 Uiso 1 1 calc R . . C42 C 0.3067(8) 0.0298(3) 0.7223(7) 0.173(5) Uani 1 1 d . . . H42A H 0.3290 0.0045 0.7033 0.259 Uiso 1 1 d R . . H42B H 0.2657 0.0426 0.6711 0.259 Uiso 1 1 d R . . H42C H 0.2698 0.0256 0.7701 0.259 Uiso 1 1 d R . . C43 C 0.4186(8) 0.0521(2) 0.8620(6) 0.154(5) Uani 1 1 d . . . H43A H 0.3648 0.0381 0.8802 0.231 Uiso 1 1 d R . . H43B H 0.4211 0.0791 0.8850 0.231 Uiso 1 1 d R . . H43C H 0.4792 0.0387 0.8864 0.231 Uiso 1 1 d R . . C44 C 0.6454(9) 0.0610(2) 0.5493(5) 0.124(4) Uani 1 1 d . . . H44 H 0.6170 0.0879 0.5410 0.149 Uiso 1 1 calc R . . C45 C 0.7555(8) 0.0652(2) 0.5719(6) 0.144(4) Uani 1 1 d . . . H45A H 0.7752 0.0752 0.6332 0.216 Uiso 1 1 d R . . H45B H 0.7785 0.0831 0.5298 0.216 Uiso 1 1 d R . . H45C H 0.7832 0.0391 0.5674 0.216 Uiso 1 1 d R . . C46 C 0.6098(11) 0.0374(3) 0.4611(6) 0.249(9) Uani 1 1 d . . . H46A H 0.5874 0.0114 0.4759 0.373 Uiso 1 1 d R . . H46B H 0.6625 0.0344 0.4276 0.373 Uiso 1 1 d R . . H46C H 0.5564 0.0517 0.4245 0.373 Uiso 1 1 d R . . C47 C 0.4066(5) 0.1909(2) 0.5774(5) 0.0739(19) Uani 1 1 d . . . C48 C 0.3396(6) 0.2070(3) 0.6283(5) 0.100(3) Uani 1 1 d . . . C49 C 0.3159(7) 0.2482(3) 0.6104(8) 0.124(4) Uani 1 1 d . . . H49 H 0.2724 0.2613 0.6411 0.149 Uiso 1 1 calc R . . C50 C 0.3581(8) 0.2677(3) 0.5478(8) 0.129(4) Uani 1 1 d . . . H50 H 0.3431 0.2947 0.5371 0.155 Uiso 1 1 calc R . . C51 C 0.4184(6) 0.2509(3) 0.5018(6) 0.099(3) Uani 1 1 d . . . H51 H 0.4452 0.2661 0.4600 0.118 Uiso 1 1 calc R . . C52 C 0.4423(5) 0.2127(2) 0.5130(5) 0.0729(19) Uani 1 1 d . . . C53 C 0.2994(6) 0.1813(3) 0.6944(6) 0.122(3) Uani 1 1 d . . . H53 H 0.3429 0.1580 0.7072 0.147 Uiso 1 1 calc R . . C54 C 0.2970(7) 0.2019(3) 0.7872(7) 0.164(5) Uani 1 1 d . . . H54A H 0.3619 0.2076 0.8206 0.246 Uiso 1 1 d R . . H54B H 0.2631 0.1849 0.8233 0.246 Uiso 1 1 d R . . H54C H 0.2612 0.2265 0.7737 0.246 Uiso 1 1 d R . . C55 C 0.1963(7) 0.1655(4) 0.6548(7) 0.192(6) Uani 1 1 d . . . H55A H 0.1539 0.1884 0.6427 0.289 Uiso 1 1 d R . . H55B H 0.1735 0.1484 0.6985 0.289 Uiso 1 1 d R . . H55C H 0.1956 0.1509 0.5989 0.289 Uiso 1 1 d R . . C56 C 0.5070(5) 0.19558(19) 0.4561(4) 0.0745(19) Uani 1 1 d . . . H56 H 0.5312 0.1699 0.4833 0.089 Uiso 1 1 calc R . . C57 C 0.4541(6) 0.1874(2) 0.3590(4) 0.106(3) Uani 1 1 d . . . H57A H 0.4122 0.1644 0.3580 0.158 Uiso 1 1 d R . . H57B H 0.5012 0.1827 0.3202 0.158 Uiso 1 1 d R . . H57C H 0.4149 0.2104 0.3373 0.158 Uiso 1 1 d R . . C58 C 0.5962(5) 0.22185(19) 0.4523(5) 0.085(2) Uani 1 1 d . . . H58A H 0.5754 0.2455 0.4172 0.128 Uiso 1 1 d R . . H58B H 0.6414 0.2070 0.4232 0.128 Uiso 1 1 d R . . H58C H 0.6280 0.2294 0.5129 0.128 Uiso 1 1 d R . . F1 F 0.0755(4) 0.24348(11) 0.8684(4) 0.143(2) 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 0.1084(5) 0.0282(2) 0.0601(3) 0.0052(2) 0.0535(3) 0.0083(2) Ru2 0.0996(4) 0.0303(2) 0.0563(3) -0.0057(2) 0.0446(3) -0.0135(2) Cl1 0.0911(11) 0.0297(6) 0.0580(9) 0.0077(6) 0.0334(8) 0.0028(7) Cl2 0.1022(13) 0.0541(8) 0.0603(9) -0.0110(7) 0.0451(9) -0.0178(8) Cl3 0.1659(18) 0.0263(6) 0.0737(10) -0.0023(6) 0.0760(11) -0.0001(9) N1 0.149(6) 0.050(3) 0.080(4) 0.033(3) 0.075(4) 0.057(3) N2 0.109(5) 0.071(3) 0.055(3) 0.027(3) 0.041(3) 0.050(3) N3 0.199(7) 0.056(4) 0.073(4) -0.022(3) 0.075(5) -0.062(4) N4 0.109(5) 0.076(4) 0.066(4) -0.027(3) 0.038(4) -0.055(4) O1 0.168(5) 0.044(2) 0.101(3) 0.016(2) 0.090(4) 0.011(3) O2 0.091(3) 0.054(2) 0.065(3) -0.008(2) 0.031(2) 0.020(2) O3 0.086(3) 0.037(2) 0.072(3) -0.002(2) 0.009(2) -0.002(2) O4 0.107(4) 0.062(3) 0.069(3) 0.001(2) 0.050(3) -0.006(2) C1 0.136(6) 0.036(3) 0.073(4) 0.000(3) 0.068(4) 0.000(4) C2 0.080(4) 0.042(3) 0.057(4) 0.002(3) 0.037(3) 0.011(3) C3 0.119(6) 0.040(3) 0.068(4) 0.027(3) 0.060(4) 0.036(3) C4 0.166(9) 0.106(6) 0.093(6) 0.050(5) 0.071(6) 0.100(6) C5 0.121(7) 0.122(6) 0.066(5) 0.042(4) 0.048(4) 0.081(5) C6 0.069(4) 0.048(3) 0.045(3) 0.001(3) 0.016(3) -0.010(3) C7 0.094(5) 0.039(3) 0.055(4) -0.001(3) 0.035(4) -0.006(3) C8 0.124(6) 0.052(4) 0.061(4) -0.018(3) 0.058(4) -0.039(4) C9 0.197(10) 0.091(6) 0.065(5) -0.031(4) 0.040(6) -0.097(7) C10 0.147(8) 0.105(6) 0.073(5) -0.021(5) 0.028(5) -0.090(6) C11 0.161(7) 0.047(4) 0.097(5) 0.027(3) 0.090(5) 0.051(4) C12A 0.144(7) 0.049(4) 0.094(5) 0.026(4) 0.079(5) 0.027(4) C13 0.190(9) 0.056(4) 0.121(6) 0.004(4) 0.118(6) 0.013(5) C14 0.242(11) 0.055(5) 0.194(9) -0.009(5) 0.174(9) 0.014(6) C15 0.260(11) 0.044(4) 0.197(9) 0.006(5) 0.193(9) 0.014(5) C16 0.202(9) 0.042(4) 0.147(7) 0.028(4) 0.143(7) 0.046(5) C17 0.164(8) 0.055(4) 0.077(5) 0.018(3) 0.076(5) 0.026(5) C18 0.136(8) 0.088(6) 0.162(9) 0.058(6) 0.039(7) 0.041(6) C19 0.125(6) 0.067(4) 0.093(5) 0.032(4) 0.055(5) 0.016(4) C20 0.284(14) 0.064(5) 0.209(10) 0.070(6) 0.210(11) 0.088(7) C21 0.39(2) 0.047(5) 0.283(14) -0.020(7) 0.283(15) -0.040(8) C22 0.370(18) 0.263(14) 0.335(17) 0.257(14) 0.306(16) 0.269(15) C23 0.093(5) 0.053(4) 0.059(4) 0.015(3) 0.031(4) 0.032(3) C24 0.094(5) 0.068(4) 0.053(4) 0.004(3) 0.029(4) 0.026(4) C25 0.093(5) 0.069(4) 0.060(4) 0.001(3) 0.025(4) 0.012(4) C26 0.107(6) 0.070(5) 0.060(4) -0.007(3) 0.026(4) 0.009(4) C27 0.096(6) 0.057(4) 0.080(5) 0.009(4) 0.013(4) 0.019(4) C28 0.080(5) 0.063(4) 0.078(5) 0.024(4) 0.022(4) 0.016(4) C29 0.139(7) 0.057(4) 0.075(5) 0.020(3) 0.058(5) 0.022(4) C30 0.187(9) 0.064(5) 0.103(6) 0.007(4) 0.081(6) -0.008(5) C31 0.242(11) 0.096(6) 0.091(6) 0.056(5) 0.044(7) 0.050(7) C32 0.064(5) 0.088(5) 0.095(5) 0.038(4) 0.018(4) 0.019(4) C33 0.085(7) 0.210(11) 0.167(9) 0.102(8) 0.042(6) 0.011(7) C34 0.112(6) 0.074(5) 0.093(5) 0.021(4) 0.026(5) 0.000(4) C35 0.216(9) 0.040(4) 0.080(5) -0.025(3) 0.092(6) -0.052(5) C36 0.246(10) 0.036(3) 0.108(6) -0.024(4) 0.121(7) -0.051(5) C37 0.346(15) 0.045(4) 0.146(8) -0.027(5) 0.168(9) -0.039(7) C38 0.338(15) 0.026(3) 0.151(8) -0.002(4) 0.154(10) -0.031(6) C39 0.292(13) 0.055(5) 0.108(6) -0.023(4) 0.125(8) -0.063(7) C40 0.244(10) 0.052(4) 0.087(5) -0.027(4) 0.104(6) -0.066(5) C41 0.211(10) 0.070(5) 0.095(6) -0.035(4) 0.099(6) -0.064(6) C42 0.223(12) 0.151(10) 0.172(10) -0.076(8) 0.109(9) -0.031(9) C43 0.268(13) 0.106(7) 0.125(7) -0.039(6) 0.130(8) -0.087(8) C44 0.261(12) 0.055(4) 0.088(5) -0.016(4) 0.112(7) -0.054(6) C45 0.254(13) 0.064(5) 0.161(9) 0.000(5) 0.160(9) -0.012(7) C46 0.53(2) 0.144(9) 0.119(8) -0.072(7) 0.193(12) -0.197(13) C47 0.073(5) 0.073(5) 0.076(5) -0.029(4) 0.014(4) -0.015(4) C48 0.076(6) 0.146(8) 0.077(5) -0.028(5) 0.013(5) -0.051(6) C49 0.092(7) 0.120(8) 0.150(10) -0.053(7) -0.003(6) 0.030(6) C50 0.147(10) 0.088(7) 0.143(10) 0.024(7) 0.003(8) 0.005(7) C51 0.113(7) 0.085(6) 0.099(6) -0.007(5) 0.026(5) 0.015(5) C52 0.073(5) 0.071(5) 0.073(5) -0.015(4) 0.007(4) -0.016(4) C53 0.093(7) 0.177(9) 0.106(7) -0.045(6) 0.040(5) -0.043(6) C54 0.131(8) 0.240(13) 0.139(9) -0.062(9) 0.072(7) -0.005(8) C55 0.143(9) 0.309(17) 0.139(9) -0.042(10) 0.061(8) -0.113(10) C56 0.097(5) 0.063(4) 0.065(4) -0.007(3) 0.019(4) -0.017(4) C57 0.139(7) 0.119(7) 0.058(5) -0.014(4) 0.015(5) -0.038(6) C58 0.117(6) 0.060(4) 0.081(5) -0.004(3) 0.024(4) -0.029(4) F1 0.221(5) 0.057(2) 0.194(5) 0.031(3) 0.154(4) 0.040(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.877(6) . ? Ru1 C2 1.893(6) . ? Ru1 C3 2.095(8) . ? Ru1 Cl1 2.434(3) . ? Ru1 Cl3 2.465(3) . ? Ru1 Cl2 2.506(4) . ? Ru2 C7 1.867(6) . ? Ru2 C6 1.885(6) . ? Ru2 C8 2.075(8) . ? Ru2 Cl2 2.446(3) . ? Ru2 Cl3 2.456(3) . ? Ru2 Cl1 2.513(3) . ? N1 C4 1.373(10) . ? N1 C3 1.378(7) . ? N1 C11 1.486(8) . ? N2 C3 1.365(8) . ? N2 C5 1.395(8) . ? N2 C23 1.456(7) . ? N3 C8 1.378(8) . ? N3 C9 1.406(10) . ? N3 C35 1.443(10) . ? N4 C8 1.374(9) . ? N4 C10 1.409(8) . ? N4 C47 1.442(9) . ? O1 C1 1.129(6) . ? O2 C2 1.117(6) . ? O3 C6 1.146(6) . ? O4 C7 1.144(6) . ? C4 C5 1.344(10) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C9 C10 1.299(12) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12A 1.391(8) . ? C11 C16 1.396(10) . ? C12A C13 1.406(9) . ? C12A C17 1.510(9) . ? C13 C14 1.363(10) . ? C13 H13 0.9500 . ? C14 C15 1.366(9) . ? C14 H14 0.9500 . ? C15 C16 1.380(10) . ? C15 H15 0.9500 . ? C16 C20 1.551(9) . ? C17 C18 1.547(11) . ? C17 C19 1.561(9) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.499(17) . ? C20 C22 1.565(14) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C28 1.387(8) . ? C23 C24 1.390(8) . ? C24 C25 1.391(8) . ? C24 C29 1.516(9) . ? C25 C26 1.353(9) . ? C25 H25 0.9500 . ? C26 C27 1.351(9) . ? C26 H26 0.9500 . ? C27 C28 1.403(9) . ? C27 H27 0.9500 . ? C28 C32 1.537(9) . ? C29 C31 1.521(10) . ? C29 C30 1.534(10) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C34 1.536(9) . ? C32 C33 1.540(10) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C40 1.409(8) . ? C35 C36 1.410(11) . ? C36 C37 1.401(12) . ? C36 C44 1.550(9) . ? C37 C38 1.391(10) . ? C37 H37 0.9500 . ? C38 C39 1.377(13) . ? C38 H38 0.9500 . ? C39 C40 1.363(12) . ? C39 H39 0.9500 . ? C40 C41 1.479(12) . ? C41 C43 1.516(10) . ? C41 C42 1.559(12) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.534(13) . ? C44 C46 1.560(11) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C52 1.395(9) . ? C47 C48 1.436(10) . ? C48 C49 1.453(12) . ? C48 C53 1.519(11) . ? C49 C50 1.383(13) . ? C49 H49 0.9500 . ? C50 C51 1.327(12) . ? C50 H50 0.9500 . ? C51 C52 1.345(10) . ? C51 H51 0.9500 . ? C52 C56 1.488(9) . ? C53 C55 1.562(11) . ? C53 C54 1.577(11) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.547(9) . ? C56 C58 1.553(8) . ? C56 H56 1.0000 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 88.6(3) . . ? C1 Ru1 C3 89.7(3) . . ? C2 Ru1 C3 95.5(3) . . ? C1 Ru1 Cl1 175.4(2) . . ? C2 Ru1 Cl1 93.9(2) . . ? C3 Ru1 Cl1 93.89(17) . . ? C1 Ru1 Cl3 96.2(2) . . ? C2 Ru1 Cl3 163.26(19) . . ? C3 Ru1 Cl3 100.55(18) . . ? Cl1 Ru1 Cl3 80.35(12) . . ? C1 Ru1 Cl2 94.3(2) . . ? C2 Ru1 Cl2 84.1(2) . . ? C3 Ru1 Cl2 175.99(15) . . ? Cl1 Ru1 Cl2 82.16(10) . . ? Cl3 Ru1 Cl2 79.53(9) . . ? C7 Ru2 C6 90.4(2) . . ? C7 Ru2 C8 88.0(3) . . ? C6 Ru2 C8 94.6(3) . . ? C7 Ru2 Cl2 175.7(2) . . ? C6 Ru2 Cl2 91.72(17) . . ? C8 Ru2 Cl2 95.53(19) . . ? C7 Ru2 Cl3 96.14(19) . . ? C6 Ru2 Cl3 163.82(17) . . ? C8 Ru2 Cl3 100.4(2) . . ? Cl2 Ru2 Cl3 80.87(9) . . ? C7 Ru2 Cl1 94.6(2) . . ? C6 Ru2 Cl1 85.75(19) . . ? C8 Ru2 Cl1 177.29(16) . . ? Cl2 Ru2 Cl1 81.77(12) . . ? Cl3 Ru2 Cl1 78.99(11) . . ? Ru1 Cl1 Ru2 83.19(11) . . ? Ru2 Cl2 Ru1 83.10(12) . . ? Ru2 Cl3 Ru1 83.74(11) . . ? C4 N1 C3 110.6(6) . . ? C4 N1 C11 119.9(6) . . ? C3 N1 C11 129.5(7) . . ? C3 N2 C5 113.3(5) . . ? C3 N2 C23 128.1(5) . . ? C5 N2 C23 118.6(6) . . ? C8 N3 C9 110.1(7) . . ? C8 N3 C35 129.5(8) . . ? C9 N3 C35 120.4(6) . . ? C8 N4 C10 112.5(7) . . ? C8 N4 C47 127.8(5) . . ? C10 N4 C47 119.7(7) . . ? O1 C1 Ru1 178.5(6) . . ? O2 C2 Ru1 170.0(6) . . ? N2 C3 N1 102.6(6) . . ? N2 C3 Ru1 128.2(4) . . ? N1 C3 Ru1 129.2(6) . . ? C5 C4 N1 109.4(7) . . ? C5 C4 H4 125.3 . . ? N1 C4 H4 125.3 . . ? C4 C5 N2 104.0(7) . . ? C4 C5 H5 128.0 . . ? N2 C5 H5 128.0 . . ? O3 C6 Ru2 166.2(5) . . ? O4 C7 Ru2 177.5(5) . . ? N4 C8 N3 102.4(7) . . ? N4 C8 Ru2 127.9(4) . . ? N3 C8 Ru2 129.6(7) . . ? C10 C9 N3 109.6(7) . . ? C10 C9 H9 125.2 . . ? N3 C9 H9 125.2 . . ? C9 C10 N4 105.4(8) . . ? C9 C10 H10 127.3 . . ? N4 C10 H10 127.3 . . ? C12A C11 C16 124.1(6) . . ? C12A C11 N1 116.7(6) . . ? C16 C11 N1 118.4(5) . . ? C11 C12A C13 116.1(6) . . ? C11 C12A C17 124.3(6) . . ? C13 C12A C17 119.5(6) . . ? C14 C13 C12A 120.0(6) . . ? C14 C13 H13 120.0 . . ? C12A C13 H13 120.0 . . ? C13 C14 C15 122.5(7) . . ? C13 C14 H14 118.7 . . ? C15 C14 H14 118.7 . . ? C14 C15 C16 120.3(7) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 116.9(6) . . ? C15 C16 C20 119.2(7) . . ? C11 C16 C20 123.9(7) . . ? C12A C17 C18 113.2(6) . . ? C12A C17 C19 111.6(7) . . ? C18 C17 C19 110.1(6) . . ? C12A C17 H17 107.2 . . ? C18 C17 H17 107.2 . . ? C19 C17 H17 107.2 . . ? C17 C18 H18A 107.1 . . ? C17 C18 H18B 108.0 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 113.2 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 111.2 . . ? C17 C19 H19B 107.6 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.6 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C16 113.7(10) . . ? C21 C20 C22 113.0(9) . . ? C16 C20 C22 107.9(8) . . ? C21 C20 H20 107.3 . . ? C16 C20 H20 107.3 . . ? C22 C20 H20 107.3 . . ? C20 C21 H21A 110.2 . . ? C20 C21 H21B 109.0 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.3 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.4 . . ? C20 C22 H22B 109.4 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.6 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 123.9(6) . . ? C28 C23 N2 117.9(6) . . ? C24 C23 N2 117.9(5) . . ? C23 C24 C25 117.8(6) . . ? C23 C24 C29 123.8(5) . . ? C25 C24 C29 118.3(6) . . ? C26 C25 C24 119.3(6) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C27 C26 C25 122.3(6) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C26 C27 C28 121.9(6) . . ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C23 C28 C27 114.9(6) . . ? C23 C28 C32 121.4(6) . . ? C27 C28 C32 123.6(6) . . ? C24 C29 C31 112.6(7) . . ? C24 C29 C30 110.2(6) . . ? C31 C29 C30 111.9(6) . . ? C24 C29 H29 107.3 . . ? C31 C29 H29 107.3 . . ? C30 C29 H29 107.3 . . ? C29 C30 H30A 107.8 . . ? C29 C30 H30B 112.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 108.0 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 108.2 . . ? C29 C31 H31B 113.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 106.7 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C32 C28 113.0(6) . . ? C34 C32 C33 109.3(6) . . ? C28 C32 C33 108.7(6) . . ? C34 C32 H32 108.6 . . ? C28 C32 H32 108.6 . . ? C33 C32 H32 108.6 . . ? C32 C33 H33A 107.3 . . ? C32 C33 H33B 113.2 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 107.8 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 110.6 . . ? C32 C34 H34B 109.6 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 108.2 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 122.9(8) . . ? C40 C35 N3 117.3(8) . . ? C36 C35 N3 119.3(6) . . ? C37 C36 C35 118.2(6) . . ? C37 C36 C44 119.4(8) . . ? C35 C36 C44 122.3(8) . . ? C38 C37 C36 118.5(9) . . ? C38 C37 H37 120.7 . . ? C36 C37 H37 120.7 . . ? C39 C38 C37 121.5(8) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C40 C39 C38 122.5(7) . . ? C40 C39 H39 118.7 . . ? C38 C39 H39 118.7 . . ? C39 C40 C35 116.3(8) . . ? C39 C40 C41 120.3(7) . . ? C35 C40 C41 123.4(8) . . ? C40 C41 C43 112.5(9) . . ? C40 C41 C42 110.1(6) . . ? C43 C41 C42 109.7(7) . . ? C40 C41 H41 108.2 . . ? C43 C41 H41 108.2 . . ? C42 C41 H41 108.2 . . ? C41 C42 H42A 104.9 . . ? C41 C42 H42B 114.0 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.4 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 107.8 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 111.1 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C36 112.4(8) . . ? C45 C44 C46 113.0(9) . . ? C36 C44 C46 107.7(6) . . ? C45 C44 H44 107.9 . . ? C36 C44 H44 107.9 . . ? C46 C44 H44 107.9 . . ? C44 C45 H45A 110.0 . . ? C44 C45 H45B 111.0 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 107.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 110.1 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 108.7 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C52 C47 C48 122.2(8) . . ? C52 C47 N4 119.1(6) . . ? C48 C47 N4 118.0(7) . . ? C47 C48 C49 114.8(8) . . ? C47 C48 C53 119.9(9) . . ? C49 C48 C53 125.2(9) . . ? C50 C49 C48 118.6(9) . . ? C50 C49 H49 120.7 . . ? C48 C49 H49 120.7 . . ? C51 C50 C49 123.6(10) . . ? C51 C50 H50 118.2 . . ? C49 C50 H50 118.2 . . ? C50 C51 C52 121.4(9) . . ? C50 C51 H51 119.3 . . ? C52 C51 H51 119.3 . . ? C51 C52 C47 119.2(7) . . ? C51 C52 C56 118.2(7) . . ? C47 C52 C56 122.6(7) . . ? C48 C53 C55 112.4(8) . . ? C48 C53 C54 114.0(8) . . ? C55 C53 C54 108.9(7) . . ? C48 C53 H53 107.1 . . ? C55 C53 H53 107.1 . . ? C54 C53 H53 107.1 . . ? C53 C54 H54A 112.1 . . ? C53 C54 H54B 109.4 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 106.8 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 106.8 . . ? C53 C55 H55B 110.1 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 111.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C52 C56 C57 112.6(6) . . ? C52 C56 C58 112.6(5) . . ? C57 C56 C58 108.6(6) . . ? C52 C56 H56 107.6 . . ? C57 C56 H56 107.6 . . ? C58 C56 H56 107.6 . . ? C56 C57 H57A 110.0 . . ? C56 C57 H57B 109.9 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 108.6 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.3 . . ? C56 C58 H58B 108.7 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 110.4 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Ru1 Cl1 Ru2 -122.6(2) . . . . ? C3 Ru1 Cl1 Ru2 141.67(17) . . . . ? Cl3 Ru1 Cl1 Ru2 41.61(8) . . . . ? Cl2 Ru1 Cl1 Ru2 -39.03(6) . . . . ? C7 Ru2 Cl1 Ru1 -137.39(18) . . . . ? C6 Ru2 Cl1 Ru1 132.57(18) . . . . ? Cl2 Ru2 Cl1 Ru1 40.21(6) . . . . ? Cl3 Ru2 Cl1 Ru1 -42.02(7) . . . . ? C6 Ru2 Cl2 Ru1 -124.31(17) . . . . ? C8 Ru2 Cl2 Ru1 140.9(2) . . . . ? Cl3 Ru2 Cl2 Ru1 41.23(6) . . . . ? Cl1 Ru2 Cl2 Ru1 -38.85(8) . . . . ? C1 Ru1 Cl2 Ru2 -136.77(17) . . . . ? C2 Ru1 Cl2 Ru2 135.06(18) . . . . ? Cl1 Ru1 Cl2 Ru2 40.32(6) . . . . ? Cl3 Ru1 Cl2 Ru2 -41.25(8) . . . . ? C7 Ru2 Cl3 Ru1 134.9(2) . . . . ? C6 Ru2 Cl3 Ru1 21.6(6) . . . . ? C8 Ru2 Cl3 Ru1 -136.00(17) . . . . ? Cl2 Ru2 Cl3 Ru1 -42.00(8) . . . . ? Cl1 Ru2 Cl3 Ru1 41.32(7) . . . . ? C1 Ru1 Cl3 Ru2 134.2(2) . . . . ? C2 Ru1 Cl3 Ru2 28.2(6) . . . . ? C3 Ru1 Cl3 Ru2 -134.93(15) . . . . ? Cl1 Ru1 Cl3 Ru2 -42.74(9) . . . . ? Cl2 Ru1 Cl3 Ru2 40.99(5) . . . . ? C1 Ru1 C2 O2 -94(3) . . . . ? C3 Ru1 C2 O2 176(3) . . . . ? Cl1 Ru1 C2 O2 82(3) . . . . ? Cl3 Ru1 C2 O2 13(3) . . . . ? Cl2 Ru1 C2 O2 1(3) . . . . ? C5 N2 C3 N1 -0.2(7) . . . . ? C23 N2 C3 N1 178.8(5) . . . . ? C5 N2 C3 Ru1 176.6(4) . . . . ? C23 N2 C3 Ru1 -4.4(9) . . . . ? C4 N1 C3 N2 1.8(7) . . . . ? C11 N1 C3 N2 -178.5(5) . . . . ? C4 N1 C3 Ru1 -175.0(5) . . . . ? C11 N1 C3 Ru1 4.7(9) . . . . ? C1 Ru1 C3 N2 -88.1(5) . . . . ? C2 Ru1 C3 N2 0.5(5) . . . . ? Cl1 Ru1 C3 N2 94.8(5) . . . . ? Cl3 Ru1 C3 N2 175.7(5) . . . . ? C1 Ru1 C3 N1 87.9(5) . . . . ? C2 Ru1 C3 N1 176.5(5) . . . . ? Cl1 Ru1 C3 N1 -89.3(5) . . . . ? Cl3 Ru1 C3 N1 -8.4(5) . . . . ? C3 N1 C4 C5 -2.8(9) . . . . ? C11 N1 C4 C5 177.4(6) . . . . ? N1 C4 C5 N2 2.5(9) . . . . ? C3 N2 C5 C4 -1.5(8) . . . . ? C23 N2 C5 C4 179.4(6) . . . . ? C7 Ru2 C6 O3 -95(2) . . . . ? C8 Ru2 C6 O3 177(2) . . . . ? Cl2 Ru2 C6 O3 81(2) . . . . ? Cl3 Ru2 C6 O3 19(3) . . . . ? Cl1 Ru2 C6 O3 -1(2) . . . . ? C10 N4 C8 N3 -1.9(7) . . . . ? C47 N4 C8 N3 179.3(6) . . . . ? C10 N4 C8 Ru2 174.5(4) . . . . ? C47 N4 C8 Ru2 -4.4(9) . . . . ? C9 N3 C8 N4 0.1(7) . . . . ? C35 N3 C8 N4 -176.9(6) . . . . ? C9 N3 C8 Ru2 -176.2(5) . . . . ? C35 N3 C8 Ru2 6.9(10) . . . . ? C7 Ru2 C8 N4 -87.5(6) . . . . ? C6 Ru2 C8 N4 2.7(6) . . . . ? Cl2 Ru2 C8 N4 94.9(5) . . . . ? Cl3 Ru2 C8 N4 176.6(5) . . . . ? C7 Ru2 C8 N3 87.9(5) . . . . ? C6 Ru2 C8 N3 178.1(5) . . . . ? Cl2 Ru2 C8 N3 -89.7(5) . . . . ? Cl3 Ru2 C8 N3 -8.0(5) . . . . ? C8 N3 C9 C10 1.9(9) . . . . ? C35 N3 C9 C10 179.1(7) . . . . ? N3 C9 C10 N4 -2.9(9) . . . . ? C8 N4 C10 C9 3.1(9) . . . . ? C47 N4 C10 C9 -178.0(7) . . . . ? C4 N1 C11 C12A -81.4(8) . . . . ? C3 N1 C11 C12A 99.0(9) . . . . ? C4 N1 C11 C16 88.9(9) . . . . ? C3 N1 C11 C16 -90.7(8) . . . . ? C16 C11 C12A C13 0.8(13) . . . . ? N1 C11 C12A C13 170.5(7) . . . . ? C16 C11 C12A C17 -176.5(8) . . . . ? N1 C11 C12A C17 -6.8(11) . . . . ? C11 C12A C13 C14 -0.5(13) . . . . ? C17 C12A C13 C14 177.0(9) . . . . ? C12A C13 C14 C15 -0.2(16) . . . . ? C13 C14 C15 C16 0.7(18) . . . . ? C14 C15 C16 C11 -0.4(16) . . . . ? C14 C15 C16 C20 -178.2(10) . . . . ? C12A C11 C16 C15 -0.4(14) . . . . ? N1 C11 C16 C15 -169.9(8) . . . . ? C12A C11 C16 C20 177.3(9) . . . . ? N1 C11 C16 C20 7.8(13) . . . . ? C11 C12A C17 C18 106.7(8) . . . . ? C13 C12A C17 C18 -70.6(10) . . . . ? C11 C12A C17 C19 -128.4(8) . . . . ? C13 C12A C17 C19 54.3(10) . . . . ? C15 C16 C20 C21 -50.0(12) . . . . ? C11 C16 C20 C21 132.3(10) . . . . ? C15 C16 C20 C22 76.1(14) . . . . ? C11 C16 C20 C22 -101.6(11) . . . . ? C3 N2 C23 C28 -90.8(8) . . . . ? C5 N2 C23 C28 88.1(7) . . . . ? C3 N2 C23 C24 95.1(7) . . . . ? C5 N2 C23 C24 -86.0(8) . . . . ? C28 C23 C24 C25 1.3(10) . . . . ? N2 C23 C24 C25 175.0(6) . . . . ? C28 C23 C24 C29 -176.6(7) . . . . ? N2 C23 C24 C29 -2.9(10) . . . . ? C23 C24 C25 C26 -1.5(10) . . . . ? C29 C24 C25 C26 176.5(7) . . . . ? C24 C25 C26 C27 0.8(11) . . . . ? C25 C26 C27 C28 0.1(11) . . . . ? C24 C23 C28 C27 -0.4(10) . . . . ? N2 C23 C28 C27 -174.1(6) . . . . ? C24 C23 C28 C32 175.9(6) . . . . ? N2 C23 C28 C32 2.2(9) . . . . ? C26 C27 C28 C23 -0.3(10) . . . . ? C26 C27 C28 C32 -176.6(6) . . . . ? C23 C24 C29 C31 100.1(8) . . . . ? C25 C24 C29 C31 -77.7(8) . . . . ? C23 C24 C29 C30 -134.1(7) . . . . ? C25 C24 C29 C30 48.0(9) . . . . ? C23 C28 C32 C34 140.3(7) . . . . ? C27 C28 C32 C34 -43.7(10) . . . . ? C23 C28 C32 C33 -98.2(8) . . . . ? C27 C28 C32 C33 77.7(9) . . . . ? C8 N3 C35 C40 94.9(9) . . . . ? C9 N3 C35 C40 -81.7(8) . . . . ? C8 N3 C35 C36 -93.0(8) . . . . ? C9 N3 C35 C36 90.3(9) . . . . ? C40 C35 C36 C37 -0.5(13) . . . . ? N3 C35 C36 C37 -172.0(8) . . . . ? C40 C35 C36 C44 175.1(7) . . . . ? N3 C35 C36 C44 3.5(12) . . . . ? C35 C36 C37 C38 0.7(14) . . . . ? C44 C36 C37 C38 -175.0(9) . . . . ? C36 C37 C38 C39 -0.7(16) . . . . ? C37 C38 C39 C40 0.6(17) . . . . ? C38 C39 C40 C35 -0.3(14) . . . . ? C38 C39 C40 C41 -179.9(9) . . . . ? C36 C35 C40 C39 0.3(13) . . . . ? N3 C35 C40 C39 172.0(7) . . . . ? C36 C35 C40 C41 179.8(8) . . . . ? N3 C35 C40 C41 -8.4(11) . . . . ? C39 C40 C41 C43 49.9(10) . . . . ? C35 C40 C41 C43 -129.6(8) . . . . ? C39 C40 C41 C42 -72.7(11) . . . . ? C35 C40 C41 C42 107.8(9) . . . . ? C37 C36 C44 C45 -53.9(10) . . . . ? C35 C36 C44 C45 130.6(9) . . . . ? C37 C36 C44 C46 71.2(13) . . . . ? C35 C36 C44 C46 -104.3(10) . . . . ? C8 N4 C47 C52 98.4(8) . . . . ? C10 N4 C47 C52 -80.4(8) . . . . ? C8 N4 C47 C48 -91.0(8) . . . . ? C10 N4 C47 C48 90.2(8) . . . . ? C52 C47 C48 C49 -2.8(10) . . . . ? N4 C47 C48 C49 -173.2(6) . . . . ? C52 C47 C48 C53 177.1(6) . . . . ? N4 C47 C48 C53 6.7(10) . . . . ? C47 C48 C49 C50 0.2(12) . . . . ? C53 C48 C49 C50 -179.7(8) . . . . ? C48 C49 C50 C51 1.0(15) . . . . ? C49 C50 C51 C52 0.5(16) . . . . ? C50 C51 C52 C47 -3.1(12) . . . . ? C50 C51 C52 C56 177.4(8) . . . . ? C48 C47 C52 C51 4.4(10) . . . . ? N4 C47 C52 C51 174.6(6) . . . . ? C48 C47 C52 C56 -176.2(6) . . . . ? N4 C47 C52 C56 -6.0(10) . . . . ? C47 C48 C53 C55 -99.3(10) . . . . ? C49 C48 C53 C55 80.6(11) . . . . ? C47 C48 C53 C54 136.2(8) . . . . ? C49 C48 C53 C54 -43.9(12) . . . . ? C51 C52 C56 C57 -76.3(8) . . . . ? C47 C52 C56 C57 104.3(8) . . . . ? C51 C52 C56 C58 46.9(9) . . . . ? C47 C52 C56 C58 -132.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.516 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.091 # Attachment '05032.cif' data_05032 _database_code_depnum_ccdc_archive 'CCDC 723429' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C46 H48 N4 O4 Ru, 2(B2 F7)' _chemical_formula_sum 'C46 H48 B4 F14 N4 O4 Ru' _chemical_formula_weight 1131.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 16.579(4) _cell_length_b 17.136(4) _cell_length_c 17.631(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5008.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 893 _cell_measurement_theta_min 2.310 _cell_measurement_theta_max 21.661 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ; absorption correction based on 6841 reflections(SADABS);Rint 0.048 before correction and 0.0415 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29933 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.0962 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 23.34 _reflns_number_total 7220 _reflns_number_gt 5055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.43(5) _refine_ls_number_reflns 7220 _refine_ls_number_parameters 653 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.00858(3) 0.74601(3) 0.52125(7) 0.02968(16) Uani 1 1 d . . . N1 N 0.0771(4) 0.9161(4) 0.4892(4) 0.0379(18) Uani 1 1 d . . . N2 N -0.0377(4) 0.9241(4) 0.5431(3) 0.0302(18) Uani 1 1 d . . . N3 N -0.0437(4) 0.5782(4) 0.4668(4) 0.0349(18) Uani 1 1 d . . . N4 N 0.0100(4) 0.5699(4) 0.5770(4) 0.0346(18) Uani 1 1 d . . . O1 O 0.1720(4) 0.7079(3) 0.4489(4) 0.0527(18) Uani 1 1 d . . . O2 O 0.0968(4) 0.7614(3) 0.6744(4) 0.0530(18) Uani 1 1 d . . . O3 O -0.1580(4) 0.7336(3) 0.5975(4) 0.063(2) Uani 1 1 d . . . O4 O -0.0704(4) 0.7828(3) 0.3662(4) 0.0466(17) Uani 1 1 d . . . C1 C 0.1136(5) 0.7264(5) 0.4740(5) 0.031(2) Uani 1 1 d . . . C2 C 0.0624(5) 0.7496(5) 0.6203(5) 0.041(2) Uani 1 1 d . . . C3 C -0.0983(6) 0.7453(5) 0.5692(6) 0.047(3) Uani 1 1 d . . . C4 C -0.0419(5) 0.7621(5) 0.4216(6) 0.041(2) Uani 1 1 d . . . C5 C 0.0190(4) 0.8694(4) 0.5197(7) 0.0319(18) Uani 1 1 d . . . C6 C 0.0577(5) 0.9946(5) 0.4947(5) 0.046(2) Uani 1 1 d . . . H6 H 0.0901 1.0368 0.4776 0.055 Uiso 1 1 calc R . . C7 C -0.0135(5) 1.0006(5) 0.5277(7) 0.046(2) Uani 1 1 d . . . H7 H -0.0423 1.0472 0.5387 0.055 Uiso 1 1 calc R . . C8 C 0.1527(5) 0.8900(5) 0.4563(5) 0.038(2) Uani 1 1 d . . . C9 C 0.2194(5) 0.8831(4) 0.5052(5) 0.035(2) Uani 1 1 d . . . C10 C 0.2917(5) 0.8635(4) 0.4738(5) 0.036(2) Uani 1 1 d . . . H10 H 0.3369 0.8569 0.5062 0.043 Uiso 1 1 calc R . . C11 C 0.3018(5) 0.8529(5) 0.3969(5) 0.047(2) Uani 1 1 d . . . C12 C 0.2364(6) 0.8657(5) 0.3511(5) 0.050(3) Uani 1 1 d . . . H12 H 0.2438 0.8616 0.2978 0.060 Uiso 1 1 calc R . . C13 C 0.1604(5) 0.8840(5) 0.3775(5) 0.042(2) Uani 1 1 d . . . C14 C 0.2130(5) 0.8963(5) 0.5922(5) 0.040(2) Uani 1 1 d . . . H14A H 0.2177 0.8461 0.6184 0.060 Uiso 1 1 d R . . H14B H 0.1607 0.9200 0.6041 0.060 Uiso 1 1 d R . . H14C H 0.2564 0.9311 0.6088 0.060 Uiso 1 1 d R . . C15 C 0.3822(6) 0.8332(7) 0.3632(6) 0.080(4) Uani 1 1 d . . . H15A H 0.3758 0.7910 0.3262 0.120 Uiso 1 1 d R . . H15B H 0.4188 0.8164 0.4036 0.120 Uiso 1 1 d R . . H15C H 0.4045 0.8793 0.3379 0.120 Uiso 1 1 d R . . C16 C 0.0913(6) 0.9000(7) 0.3274(6) 0.071(3) Uani 1 1 d . . . H16A H 0.0408 0.8927 0.3555 0.107 Uiso 1 1 d R . . H16B H 0.0928 0.8639 0.2843 0.107 Uiso 1 1 d R . . H16C H 0.0943 0.9538 0.3089 0.107 Uiso 1 1 d R . . C17 C -0.1100(5) 0.9110(4) 0.5855(5) 0.037(2) Uani 1 1 d . . . C18 C -0.1040(5) 0.9132(5) 0.6638(6) 0.045(3) Uani 1 1 d . . . C19 C -0.1752(6) 0.9041(5) 0.7041(6) 0.048(3) Uani 1 1 d . . . H19 H -0.1725 0.9039 0.7579 0.058 Uiso 1 1 calc R . . C20 C -0.2479(6) 0.8955(5) 0.6712(7) 0.053(3) Uani 1 1 d . . . C21 C -0.2514(6) 0.8972(6) 0.5943(7) 0.057(3) Uani 1 1 d . . . H21 H -0.3025 0.8927 0.5704 0.069 Uiso 1 1 calc R . . C22 C -0.1822(6) 0.9054(5) 0.5485(5) 0.041(3) Uani 1 1 d . . . C23 C -0.0239(5) 0.9254(6) 0.7049(6) 0.051(3) Uani 1 1 d . . . H23A H 0.0189 0.8974 0.6779 0.077 Uiso 1 1 d R . . H23B H -0.0282 0.9052 0.7568 0.077 Uiso 1 1 d R . . H23C H -0.0111 0.9812 0.7065 0.077 Uiso 1 1 d R . . C24 C -0.3235(6) 0.8868(6) 0.7219(7) 0.083(4) Uani 1 1 d . . . H24A H -0.3167 0.8421 0.7560 0.124 Uiso 1 1 d R . . H24B H -0.3709 0.8785 0.6897 0.124 Uiso 1 1 d R . . H24C H -0.3310 0.9344 0.7520 0.124 Uiso 1 1 d R . . C25 C -0.1908(5) 0.9110(6) 0.4648(5) 0.059(3) Uani 1 1 d . . . H25A H -0.1376 0.9202 0.4422 0.089 Uiso 1 1 d R . . H25B H -0.2268 0.9545 0.4523 0.089 Uiso 1 1 d R . . H25C H -0.2134 0.8623 0.4448 0.089 Uiso 1 1 d R . . C26 C -0.0075(4) 0.6212(4) 0.5216(8) 0.0308(18) Uani 1 1 d . . . C27 C -0.0472(6) 0.5022(6) 0.4910(6) 0.055(3) Uani 1 1 d . . . H27 H -0.0693 0.4600 0.4628 0.066 Uiso 1 1 calc R . . C28 C -0.0142(6) 0.4964(6) 0.5615(6) 0.050(3) Uani 1 1 d . . . H28 H -0.0093 0.4513 0.5925 0.060 Uiso 1 1 calc R . . C29 C -0.0783(6) 0.6003(5) 0.3970(6) 0.042(2) Uani 1 1 d . . . C30 C -0.0296(6) 0.6021(5) 0.3309(6) 0.040(3) Uani 1 1 d . . . C31 C -0.0694(6) 0.6242(5) 0.2658(6) 0.051(3) Uani 1 1 d . . . H31 H -0.0389 0.6296 0.2205 0.061 Uiso 1 1 calc R . . C32 C -0.1504(6) 0.6389(5) 0.2627(6) 0.049(3) Uani 1 1 d . . . C33 C -0.1926(6) 0.6332(6) 0.3274(6) 0.054(3) Uani 1 1 d . . . H33 H -0.2489 0.6433 0.3250 0.064 Uiso 1 1 calc R . . C34 C -0.1622(5) 0.6146(5) 0.3939(5) 0.044(2) Uani 1 1 d . . . C35 C 0.0589(5) 0.5844(6) 0.3328(6) 0.064(3) Uani 1 1 d . . . H35A H 0.0771 0.5699 0.2818 0.096 Uiso 1 1 d R . . H35B H 0.0688 0.5410 0.3678 0.096 Uiso 1 1 d R . . H35C H 0.0885 0.6306 0.3500 0.096 Uiso 1 1 d R . . C36 C -0.1894(7) 0.6624(7) 0.1886(6) 0.090(4) Uani 1 1 d . . . H36A H -0.2138 0.6164 0.1649 0.135 Uiso 1 1 d R . . H36B H -0.1488 0.6846 0.1545 0.135 Uiso 1 1 d R . . H36C H -0.2313 0.7015 0.1986 0.135 Uiso 1 1 d R . . C37 C -0.2158(6) 0.6096(7) 0.4646(6) 0.074(4) Uani 1 1 d . . . H37A H -0.2284 0.6623 0.4827 0.112 Uiso 1 1 d R . . H37B H -0.1871 0.5809 0.5044 0.112 Uiso 1 1 d R . . H37C H -0.2659 0.5823 0.4521 0.112 Uiso 1 1 d R . . C38 C 0.0577(5) 0.5844(5) 0.6463(5) 0.039(2) Uani 1 1 d . . . C39 C 0.1383(5) 0.5714(4) 0.6414(5) 0.034(2) Uani 1 1 d . . . C40 C 0.1827(5) 0.5820(5) 0.7079(5) 0.039(2) Uani 1 1 d . . . H40 H 0.2396 0.5757 0.7067 0.047 Uiso 1 1 calc R . . C41 C 0.1453(5) 0.6016(5) 0.7759(5) 0.036(2) Uani 1 1 d . . . C42 C 0.0642(5) 0.6094(5) 0.7783(5) 0.038(2) Uani 1 1 d . . . H42 H 0.0385 0.6218 0.8249 0.045 Uiso 1 1 calc R . . C43 C 0.0175(5) 0.5991(5) 0.7124(5) 0.032(2) Uani 1 1 d . . . C44 C 0.1805(5) 0.5448(5) 0.5710(4) 0.051(3) Uani 1 1 d . . . H44A H 0.1481 0.5046 0.5458 0.076 Uiso 1 1 d R . . H44B H 0.2333 0.5232 0.5845 0.076 Uiso 1 1 d R . . H44C H 0.1877 0.5892 0.5367 0.076 Uiso 1 1 d R . . C45 C 0.1954(5) 0.6150(6) 0.8468(5) 0.060(3) Uani 1 1 d . . . H45A H 0.1617 0.6389 0.8861 0.090 Uiso 1 1 d R . . H45B H 0.2405 0.6499 0.8347 0.090 Uiso 1 1 d R . . H45C H 0.2165 0.5650 0.8652 0.090 Uiso 1 1 d R . . C46 C -0.0728(5) 0.6028(6) 0.7159(6) 0.056(3) Uani 1 1 d . . . H46A H -0.0930 0.6346 0.6738 0.084 Uiso 1 1 d R . . H46B H -0.0893 0.6263 0.7642 0.084 Uiso 1 1 d R . . H46C H -0.0952 0.5500 0.7122 0.084 Uiso 1 1 d R . . B1 B 0.4645(9) 0.8078(8) 0.6296(10) 0.083(3) Uani 1 1 d . . . B2 B 0.3513(10) 0.6974(8) 0.6309(11) 0.083(3) Uani 1 1 d . . . F1 F 0.4162(3) 0.8722(3) 0.6376(3) 0.0569(15) Uani 1 1 d . . . F2 F 0.5067(3) 0.7894(4) 0.6895(3) 0.0817(19) Uani 1 1 d . . . F3 F 0.5223(4) 0.8231(3) 0.5643(4) 0.085(2) Uani 1 1 d . . . F4 F 0.4193(4) 0.7428(3) 0.5960(4) 0.0805(19) Uani 1 1 d . . . F5 F 0.2846(4) 0.7090(4) 0.5904(4) 0.0836(19) Uani 1 1 d . . . F6 F 0.3396(5) 0.7354(4) 0.7050(5) 0.132(3) Uani 1 1 d . . . F7 F 0.3715(3) 0.6223(3) 0.6416(4) 0.0765(19) Uani 1 1 d . . . B3 B 0.5667(8) 0.6753(8) 0.4667(9) 0.066(4) Uani 1 1 d . . . B4 B 0.6141(9) 0.7951(8) 0.3789(9) 0.068(4) Uani 1 1 d . . . F8 F 0.4780(4) 0.6740(3) 0.4698(3) 0.0760(18) Uani 1 1 d . . . F9 F 0.5944(4) 0.6495(3) 0.5349(3) 0.0873(19) Uani 1 1 d . . . F10 F 0.5881(4) 0.6236(3) 0.4070(3) 0.0813(19) Uani 1 1 d . . . F11 F 0.5920(4) 0.7539(4) 0.4512(4) 0.107(2) Uani 1 1 d . . . F12 F 0.6106(4) 0.8677(3) 0.3927(3) 0.079(2) Uani 1 1 d . . . F13 F 0.5664(5) 0.7686(4) 0.3208(4) 0.100(2) Uani 1 1 d . . . F14 F 0.6955(4) 0.7713(4) 0.3622(5) 0.108(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0293(3) 0.0264(3) 0.0334(3) 0.0005(4) 0.0033(5) 0.0001(3) N1 0.042(5) 0.042(5) 0.030(4) 0.007(3) 0.002(3) 0.005(4) N2 0.022(3) 0.041(4) 0.028(5) 0.003(3) 0.003(3) 0.002(3) N3 0.035(5) 0.038(5) 0.032(5) -0.002(4) -0.008(4) -0.002(4) N4 0.037(4) 0.026(4) 0.041(5) -0.006(3) -0.007(4) -0.009(4) O1 0.060(5) 0.029(4) 0.069(5) -0.004(3) 0.014(4) 0.002(3) O2 0.075(4) 0.038(4) 0.046(4) -0.007(3) -0.007(3) -0.007(4) O3 0.042(4) 0.036(4) 0.110(6) 0.010(4) 0.034(4) -0.008(3) O4 0.067(4) 0.030(4) 0.043(4) -0.004(3) -0.008(3) 0.006(3) C1 0.029(5) 0.033(6) 0.031(6) -0.004(4) 0.001(4) 0.001(4) C2 0.048(5) 0.036(6) 0.038(6) -0.011(5) 0.005(4) -0.009(5) C3 0.066(7) 0.011(5) 0.064(7) 0.007(5) -0.002(5) -0.006(5) C4 0.049(5) 0.015(5) 0.059(7) -0.004(5) 0.010(5) 0.004(4) C5 0.022(4) 0.036(4) 0.038(4) 0.018(6) 0.008(6) -0.003(3) C6 0.054(6) 0.024(5) 0.059(7) 0.023(4) -0.001(5) 0.003(4) C7 0.035(5) 0.041(5) 0.061(7) 0.040(7) -0.006(6) 0.002(4) C8 0.033(5) 0.032(5) 0.050(7) 0.023(5) 0.011(5) -0.009(4) C9 0.034(5) 0.019(4) 0.051(7) 0.008(4) 0.001(4) -0.001(3) C10 0.036(5) 0.032(5) 0.041(6) 0.009(4) 0.001(4) -0.005(4) C11 0.033(5) 0.068(7) 0.039(6) -0.007(5) -0.002(5) 0.003(5) C12 0.059(7) 0.048(6) 0.043(7) -0.001(5) 0.018(5) -0.008(5) C13 0.055(6) 0.048(6) 0.024(5) 0.020(5) 0.002(4) -0.009(5) C14 0.065(7) 0.031(5) 0.023(5) -0.019(4) 0.004(4) -0.004(5) C15 0.049(7) 0.114(11) 0.077(8) 0.011(8) 0.021(6) -0.012(7) C16 0.070(8) 0.095(9) 0.049(7) 0.012(6) -0.021(6) 0.000(7) C17 0.055(7) 0.013(5) 0.041(6) 0.002(4) -0.008(5) 0.008(4) C18 0.039(6) 0.023(5) 0.073(8) -0.007(5) -0.004(5) 0.002(4) C19 0.064(7) 0.024(5) 0.057(7) -0.009(5) 0.018(6) 0.004(5) C20 0.036(6) 0.028(5) 0.094(10) -0.006(6) 0.014(6) -0.001(4) C21 0.036(6) 0.054(7) 0.083(9) -0.005(6) -0.013(6) 0.021(5) C22 0.037(6) 0.029(5) 0.058(7) -0.002(4) 0.008(5) 0.003(4) C23 0.045(6) 0.054(7) 0.055(7) -0.011(5) 0.003(5) -0.005(5) C24 0.045(6) 0.085(9) 0.118(11) -0.016(7) 0.034(7) 0.013(6) C25 0.026(6) 0.081(8) 0.071(9) -0.017(6) -0.029(5) 0.026(5) C26 0.022(4) 0.032(4) 0.038(4) -0.017(7) 0.006(5) -0.017(3) C27 0.069(8) 0.029(6) 0.066(7) 0.006(5) -0.010(6) -0.017(5) C28 0.069(7) 0.029(6) 0.050(6) 0.012(5) -0.032(5) -0.001(5) C29 0.047(6) 0.032(5) 0.047(7) 0.001(5) -0.010(5) -0.013(4) C30 0.037(6) 0.031(6) 0.051(7) -0.011(5) -0.015(6) -0.001(5) C31 0.079(8) 0.035(6) 0.040(7) -0.018(5) -0.007(5) 0.003(5) C32 0.061(7) 0.028(6) 0.058(8) -0.004(5) -0.031(6) 0.003(5) C33 0.041(6) 0.058(7) 0.061(8) 0.002(6) -0.016(6) 0.002(5) C34 0.044(6) 0.043(6) 0.045(6) -0.002(5) -0.011(5) -0.015(5) C35 0.048(7) 0.071(8) 0.074(9) -0.035(6) -0.002(6) 0.010(6) C36 0.116(10) 0.072(9) 0.082(10) -0.017(7) -0.040(8) 0.017(7) C37 0.037(6) 0.111(10) 0.075(9) 0.019(7) 0.002(6) -0.009(6) C38 0.041(6) 0.027(5) 0.048(7) 0.014(5) -0.017(5) -0.009(4) C39 0.048(6) 0.015(5) 0.039(6) -0.006(4) 0.003(5) -0.002(4) C40 0.031(5) 0.030(5) 0.056(6) 0.010(5) -0.003(5) -0.006(4) C41 0.035(5) 0.032(5) 0.041(6) 0.005(4) -0.002(4) -0.005(4) C42 0.052(6) 0.025(5) 0.036(6) 0.006(4) -0.002(5) 0.001(4) C43 0.023(5) 0.037(6) 0.037(6) 0.011(4) 0.012(5) -0.014(5) C44 0.072(7) 0.038(6) 0.042(6) -0.011(5) -0.004(5) -0.003(5) C45 0.066(7) 0.071(8) 0.043(7) 0.003(5) -0.007(5) -0.019(6) C46 0.032(6) 0.089(9) 0.048(7) 0.038(6) 0.002(5) 0.011(6) B1 0.090(8) 0.045(6) 0.114(10) 0.018(6) 0.015(7) -0.007(6) B2 0.090(8) 0.045(6) 0.114(10) 0.018(6) 0.015(7) -0.007(6) F1 0.080(4) 0.036(3) 0.055(4) 0.001(3) -0.003(3) 0.007(3) F2 0.066(4) 0.114(5) 0.065(4) 0.021(4) -0.029(3) 0.018(4) F3 0.093(5) 0.072(4) 0.089(5) 0.004(3) 0.019(4) -0.017(4) F4 0.094(4) 0.064(4) 0.084(5) -0.011(4) 0.016(3) -0.031(4) F5 0.068(4) 0.079(4) 0.104(5) 0.034(4) 0.000(4) -0.005(3) F6 0.181(8) 0.103(6) 0.113(7) -0.008(5) 0.081(6) -0.007(5) F7 0.068(4) 0.055(4) 0.106(5) 0.018(4) 0.029(4) 0.008(3) B3 0.050(8) 0.049(9) 0.099(13) -0.002(8) 0.007(8) 0.015(7) B4 0.090(11) 0.039(8) 0.076(11) 0.007(8) 0.028(8) -0.021(8) F8 0.090(5) 0.060(4) 0.078(4) -0.012(3) 0.002(4) -0.004(3) F9 0.132(5) 0.079(4) 0.051(5) 0.000(3) -0.028(4) 0.006(4) F10 0.097(5) 0.070(4) 0.077(5) -0.010(4) 0.006(4) 0.007(4) F11 0.129(6) 0.079(5) 0.111(6) 0.017(5) 0.035(5) 0.010(5) F12 0.107(5) 0.051(4) 0.080(5) -0.012(3) 0.028(4) 0.010(4) F13 0.141(7) 0.073(5) 0.086(5) -0.010(4) -0.033(5) -0.004(4) F14 0.084(5) 0.077(5) 0.164(7) 0.003(5) 0.033(5) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.959(9) . ? Ru1 C2 1.962(10) . ? Ru1 C3 1.963(10) . ? Ru1 C4 1.965(11) . ? Ru1 C5 2.121(7) . ? Ru1 C26 2.156(6) . ? N1 C5 1.364(9) . ? N1 C6 1.386(10) . ? N1 C8 1.452(10) . ? N2 C5 1.391(9) . ? N2 C7 1.398(9) . ? N2 C17 1.429(10) . ? N3 C26 1.355(12) . ? N3 C27 1.372(11) . ? N3 C29 1.410(11) . ? N4 C26 1.345(12) . ? N4 C28 1.350(11) . ? N4 C38 1.477(10) . ? O1 C1 1.110(8) . ? O2 C2 1.130(10) . ? O3 C3 1.126(10) . ? O4 C4 1.142(10) . ? C6 C7 1.321(11) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.399(12) . ? C8 C9 1.406(11) . ? C9 C10 1.363(10) . ? C9 C14 1.554(11) . ? C10 C11 1.378(11) . ? C10 H10 0.9500 . ? C11 C12 1.371(12) . ? C11 C15 1.497(12) . ? C12 C13 1.379(12) . ? C12 H12 0.9500 . ? C13 C16 1.472(11) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.367(11) . ? C17 C18 1.386(12) . ? C18 C19 1.386(12) . ? C18 C23 1.527(12) . ? C19 C20 1.345(13) . ? C19 H19 0.9500 . ? C20 C21 1.356(12) . ? C20 C24 1.548(13) . ? C21 C22 1.409(12) . ? C21 H21 0.9500 . ? C22 C25 1.485(12) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C27 C28 1.363(11) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.413(12) . ? C29 C30 1.419(13) . ? C30 C31 1.376(12) . ? C30 C35 1.498(11) . ? C31 C32 1.368(12) . ? C31 H31 0.9500 . ? C32 C33 1.342(12) . ? C32 C36 1.512(13) . ? C33 C34 1.315(12) . ? C33 H33 0.9500 . ? C34 C37 1.534(12) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.356(11) . ? C38 C43 1.366(12) . ? C39 C40 1.396(11) . ? C39 C44 1.496(10) . ? C40 C41 1.392(11) . ? C40 H40 0.9500 . ? C41 C42 1.351(11) . ? C41 C45 1.518(11) . ? C42 C43 1.407(11) . ? C42 H42 0.9500 . ? C43 C46 1.501(10) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? B1 F2 1.304(17) . ? B1 F1 1.371(14) . ? B1 F4 1.467(15) . ? B1 F3 1.520(15) . ? B2 F5 1.331(16) . ? B2 F7 1.343(15) . ? B2 F6 1.472(18) . ? B2 F4 1.502(14) . ? B3 F9 1.360(15) . ? B3 F10 1.421(15) . ? B3 F11 1.438(14) . ? B3 F8 1.472(13) . ? B4 F12 1.268(13) . ? B4 F13 1.372(15) . ? B4 F14 1.440(15) . ? B4 F11 1.503(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 88.8(3) . . ? C1 Ru1 C3 169.8(3) . . ? C2 Ru1 C3 91.6(4) . . ? C1 Ru1 C4 91.3(4) . . ? C2 Ru1 C4 170.0(3) . . ? C3 Ru1 C4 90.1(4) . . ? C1 Ru1 C5 95.3(3) . . ? C2 Ru1 C5 86.7(4) . . ? C3 Ru1 C5 94.9(3) . . ? C4 Ru1 C5 83.3(4) . . ? C1 Ru1 C26 86.7(3) . . ? C2 Ru1 C26 94.9(4) . . ? C3 Ru1 C26 83.1(3) . . ? C4 Ru1 C26 95.1(4) . . ? C5 Ru1 C26 177.5(3) . . ? C5 N1 C6 112.3(7) . . ? C5 N1 C8 125.9(7) . . ? C6 N1 C8 121.8(7) . . ? C5 N2 C7 112.3(6) . . ? C5 N2 C17 128.0(7) . . ? C7 N2 C17 119.3(7) . . ? C26 N3 C27 108.3(8) . . ? C26 N3 C29 131.0(8) . . ? C27 N3 C29 120.6(8) . . ? C26 N4 C28 113.5(7) . . ? C26 N4 C38 127.4(7) . . ? C28 N4 C38 118.9(7) . . ? O1 C1 Ru1 173.2(8) . . ? O2 C2 Ru1 170.7(8) . . ? O3 C3 Ru1 170.1(8) . . ? O4 C4 Ru1 170.0(7) . . ? N1 C5 N2 101.5(6) . . ? N1 C5 Ru1 130.4(6) . . ? N2 C5 Ru1 127.8(5) . . ? C7 C6 N1 108.3(8) . . ? C7 C6 H6 125.9 . . ? N1 C6 H6 125.9 . . ? C6 C7 N2 105.7(8) . . ? C6 C7 H7 127.2 . . ? N2 C7 H7 127.2 . . ? C13 C8 C9 122.1(8) . . ? C13 C8 N1 119.9(8) . . ? C9 C8 N1 117.3(8) . . ? C10 C9 C8 117.6(8) . . ? C10 C9 C14 119.8(7) . . ? C8 C9 C14 122.6(7) . . ? C9 C10 C11 122.6(8) . . ? C9 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C12 C11 C10 117.5(8) . . ? C12 C11 C15 120.4(9) . . ? C10 C11 C15 121.9(8) . . ? C11 C12 C13 124.1(9) . . ? C11 C12 H12 118.0 . . ? C13 C12 H12 118.0 . . ? C12 C13 C8 115.8(8) . . ? C12 C13 C16 123.4(9) . . ? C8 C13 C16 120.7(9) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.4 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.3 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.6 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.7 . . ? C13 C16 H16B 109.2 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 122.7(9) . . ? C22 C17 N2 119.8(8) . . ? C18 C17 N2 117.1(8) . . ? C19 C18 C17 116.5(9) . . ? C19 C18 C23 120.9(9) . . ? C17 C18 C23 122.6(9) . . ? C20 C19 C18 123.7(10) . . ? C20 C19 H19 118.2 . . ? C18 C19 H19 118.2 . . ? C19 C20 C21 117.8(10) . . ? C19 C20 C24 119.1(11) . . ? C21 C20 C24 123.1(10) . . ? C20 C21 C22 122.7(10) . . ? C20 C21 H21 118.6 . . ? C22 C21 H21 118.6 . . ? C17 C22 C21 116.5(9) . . ? C17 C22 C25 123.5(8) . . ? C21 C22 C25 119.9(9) . . ? C18 C23 H23A 109.4 . . ? C18 C23 H23B 109.4 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.6 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.7 . . ? C20 C24 H24B 109.1 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.6 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.2 . . ? C22 C25 H25B 109.3 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.9 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N4 C26 N3 104.9(6) . . ? N4 C26 Ru1 128.6(8) . . ? N3 C26 Ru1 126.3(8) . . ? C28 C27 N3 109.5(10) . . ? C28 C27 H27 125.2 . . ? N3 C27 H27 125.2 . . ? N4 C28 C27 103.7(9) . . ? N4 C28 H28 128.2 . . ? C27 C28 H28 128.2 . . ? N3 C29 C34 118.7(8) . . ? N3 C29 C30 119.4(8) . . ? C34 C29 C30 121.6(9) . . ? C31 C30 C29 114.7(9) . . ? C31 C30 C35 123.0(10) . . ? C29 C30 C35 122.3(9) . . ? C32 C31 C30 123.7(10) . . ? C32 C31 H31 118.1 . . ? C30 C31 H31 118.1 . . ? C33 C32 C31 117.6(9) . . ? C33 C32 C36 122.1(10) . . ? C31 C32 C36 120.3(10) . . ? C34 C33 C32 125.1(9) . . ? C34 C33 H33 117.4 . . ? C32 C33 H33 117.4 . . ? C33 C34 C29 117.0(9) . . ? C33 C34 C37 121.1(9) . . ? C29 C34 C37 121.9(8) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.4 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C36 H36A 109.3 . . ? C32 C36 H36B 109.8 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.3 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.6 . . ? C34 C37 H37B 109.3 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C43 124.4(8) . . ? C39 C38 N4 116.5(8) . . ? C43 C38 N4 118.4(8) . . ? C38 C39 C40 116.4(8) . . ? C38 C39 C44 124.3(8) . . ? C40 C39 C44 119.3(8) . . ? C41 C40 C39 121.3(8) . . ? C41 C40 H40 119.4 . . ? C39 C40 H40 119.4 . . ? C42 C41 C40 119.7(8) . . ? C42 C41 C45 120.3(8) . . ? C40 C41 C45 120.1(8) . . ? C41 C42 C43 120.6(8) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C38 C43 C42 117.3(8) . . ? C38 C43 C46 122.0(8) . . ? C42 C43 C46 120.7(8) . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.4 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C41 C45 H45A 109.4 . . ? C41 C45 H45B 109.3 . . ? H45A C45 H45B 109.5 . . ? C41 C45 H45C 109.7 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.3 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.6 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? F2 B1 F1 115.1(13) . . ? F2 B1 F4 114.6(10) . . ? F1 B1 F4 110.8(11) . . ? F2 B1 F3 108.5(11) . . ? F1 B1 F3 107.9(10) . . ? F4 B1 F3 98.5(11) . . ? F5 B2 F7 115.2(13) . . ? F5 B2 F6 107.5(12) . . ? F7 B2 F6 109.4(13) . . ? F5 B2 F4 109.1(11) . . ? F7 B2 F4 111.5(11) . . ? F6 B2 F4 103.5(11) . . ? B1 F4 B2 127.7(10) . . ? F9 B3 F10 111.6(9) . . ? F9 B3 F11 112.0(11) . . ? F10 B3 F11 111.8(11) . . ? F9 B3 F8 107.4(11) . . ? F10 B3 F8 105.5(10) . . ? F11 B3 F8 108.2(9) . . ? F12 B4 F13 116.2(13) . . ? F12 B4 F14 111.1(10) . . ? F13 B4 F14 107.1(11) . . ? F12 B4 F11 106.6(11) . . ? F13 B4 F11 109.7(9) . . ? F14 B4 F11 105.6(11) . . ? B3 F11 B4 132.3(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ru1 C4 O4 -102(5) . . . . ? C3 Ru1 C4 O4 88(5) . . . . ? C5 Ru1 C4 O4 -7(5) . . . . ? C26 Ru1 C4 O4 171(5) . . . . ? C6 N1 C5 N2 0.9(10) . . . . ? C8 N1 C5 N2 179.0(8) . . . . ? C6 N1 C5 Ru1 174.6(8) . . . . ? C8 N1 C5 Ru1 -7.3(15) . . . . ? C7 N2 C5 N1 -0.7(11) . . . . ? C17 N2 C5 N1 -174.2(7) . . . . ? C7 N2 C5 Ru1 -174.6(8) . . . . ? C17 N2 C5 Ru1 11.9(14) . . . . ? C1 Ru1 C5 N1 5.2(10) . . . . ? C2 Ru1 C5 N1 93.7(10) . . . . ? C3 Ru1 C5 N1 -175.0(10) . . . . ? C4 Ru1 C5 N1 -85.5(10) . . . . ? C1 Ru1 C5 N2 177.3(9) . . . . ? C2 Ru1 C5 N2 -94.2(10) . . . . ? C3 Ru1 C5 N2 -2.9(10) . . . . ? C4 Ru1 C5 N2 86.7(10) . . . . ? C5 N1 C6 C7 -0.9(11) . . . . ? C8 N1 C6 C7 -179.1(9) . . . . ? N1 C6 C7 N2 0.4(11) . . . . ? C5 N2 C7 C6 0.2(12) . . . . ? C17 N2 C7 C6 174.4(8) . . . . ? C5 N1 C8 C13 99.9(11) . . . . ? C6 N1 C8 C13 -82.1(10) . . . . ? C5 N1 C8 C9 -89.5(11) . . . . ? C6 N1 C8 C9 88.4(9) . . . . ? C13 C8 C9 C10 -5.6(12) . . . . ? N1 C8 C9 C10 -175.9(7) . . . . ? C13 C8 C9 C14 174.9(7) . . . . ? N1 C8 C9 C14 4.6(11) . . . . ? C8 C9 C10 C11 2.1(12) . . . . ? C14 C9 C10 C11 -178.4(8) . . . . ? C9 C10 C11 C12 2.4(13) . . . . ? C9 C10 C11 C15 178.5(9) . . . . ? C10 C11 C12 C13 -3.8(14) . . . . ? C15 C11 C12 C13 180.0(9) . . . . ? C11 C12 C13 C8 0.6(14) . . . . ? C11 C12 C13 C16 178.0(10) . . . . ? C9 C8 C13 C12 4.2(13) . . . . ? N1 C8 C13 C12 174.3(7) . . . . ? C9 C8 C13 C16 -173.3(8) . . . . ? N1 C8 C13 C16 -3.2(13) . . . . ? C5 N2 C17 C22 -98.3(11) . . . . ? C7 N2 C17 C22 88.6(10) . . . . ? C5 N2 C17 C18 88.8(11) . . . . ? C7 N2 C17 C18 -84.4(10) . . . . ? C22 C17 C18 C19 4.3(12) . . . . ? N2 C17 C18 C19 177.0(7) . . . . ? C22 C17 C18 C23 -175.4(8) . . . . ? N2 C17 C18 C23 -2.7(12) . . . . ? C17 C18 C19 C20 -1.8(13) . . . . ? C23 C18 C19 C20 177.9(8) . . . . ? C18 C19 C20 C21 -1.1(14) . . . . ? C18 C19 C20 C24 -179.2(8) . . . . ? C19 C20 C21 C22 1.7(15) . . . . ? C24 C20 C21 C22 179.8(8) . . . . ? C18 C17 C22 C21 -3.7(13) . . . . ? N2 C17 C22 C21 -176.3(8) . . . . ? C18 C17 C22 C25 173.6(9) . . . . ? N2 C17 C22 C25 1.0(13) . . . . ? C20 C21 C22 C17 0.6(14) . . . . ? C20 C21 C22 C25 -176.8(9) . . . . ? C28 N4 C26 N3 -1.2(10) . . . . ? C38 N4 C26 N3 172.8(7) . . . . ? C28 N4 C26 Ru1 174.5(6) . . . . ? C38 N4 C26 Ru1 -11.5(12) . . . . ? C27 N3 C26 N4 0.3(10) . . . . ? C29 N3 C26 N4 176.9(8) . . . . ? C27 N3 C26 Ru1 -175.5(6) . . . . ? C29 N3 C26 Ru1 1.1(13) . . . . ? C1 Ru1 C26 N4 93.0(7) . . . . ? C2 Ru1 C26 N4 4.5(8) . . . . ? C3 Ru1 C26 N4 -86.6(8) . . . . ? C4 Ru1 C26 N4 -176.1(7) . . . . ? C1 Ru1 C26 N3 -92.3(8) . . . . ? C2 Ru1 C26 N3 179.2(7) . . . . ? C3 Ru1 C26 N3 88.2(8) . . . . ? C4 Ru1 C26 N3 -1.3(8) . . . . ? C26 N3 C27 C28 0.7(11) . . . . ? C29 N3 C27 C28 -176.4(8) . . . . ? C26 N4 C28 C27 1.5(11) . . . . ? C38 N4 C28 C27 -173.0(8) . . . . ? N3 C27 C28 N4 -1.3(11) . . . . ? C26 N3 C29 C34 -94.6(11) . . . . ? C27 N3 C29 C34 81.6(11) . . . . ? C26 N3 C29 C30 90.0(12) . . . . ? C27 N3 C29 C30 -93.8(11) . . . . ? N3 C29 C30 C31 179.8(8) . . . . ? C34 C29 C30 C31 4.5(13) . . . . ? N3 C29 C30 C35 -2.6(14) . . . . ? C34 C29 C30 C35 -177.8(9) . . . . ? C29 C30 C31 C32 -3.9(14) . . . . ? C35 C30 C31 C32 178.5(9) . . . . ? C30 C31 C32 C33 1.7(15) . . . . ? C30 C31 C32 C36 -179.6(9) . . . . ? C31 C32 C33 C34 0.1(16) . . . . ? C36 C32 C33 C34 -178.5(10) . . . . ? C32 C33 C34 C29 0.5(15) . . . . ? C32 C33 C34 C37 180.0(10) . . . . ? N3 C29 C34 C33 -178.3(8) . . . . ? C30 C29 C34 C33 -3.0(13) . . . . ? N3 C29 C34 C37 2.3(13) . . . . ? C30 C29 C34 C37 177.6(9) . . . . ? C26 N4 C38 C39 -90.2(11) . . . . ? C28 N4 C38 C39 83.5(10) . . . . ? C26 N4 C38 C43 98.6(10) . . . . ? C28 N4 C38 C43 -87.7(10) . . . . ? C43 C38 C39 C40 -6.8(13) . . . . ? N4 C38 C39 C40 -177.4(7) . . . . ? C43 C38 C39 C44 171.3(8) . . . . ? N4 C38 C39 C44 0.8(12) . . . . ? C38 C39 C40 C41 2.6(12) . . . . ? C44 C39 C40 C41 -175.6(7) . . . . ? C39 C40 C41 C42 1.1(12) . . . . ? C39 C40 C41 C45 -178.3(8) . . . . ? C40 C41 C42 C43 -1.1(13) . . . . ? C45 C41 C42 C43 178.3(8) . . . . ? C39 C38 C43 C42 6.9(13) . . . . ? N4 C38 C43 C42 177.3(7) . . . . ? C39 C38 C43 C46 -171.9(8) . . . . ? N4 C38 C43 C46 -1.5(13) . . . . ? C41 C42 C43 C38 -2.6(12) . . . . ? C41 C42 C43 C46 176.2(8) . . . . ? F2 B1 F4 B2 64.6(16) . . . . ? F1 B1 F4 B2 -67.7(16) . . . . ? F3 B1 F4 B2 179.5(10) . . . . ? F5 B2 F4 B1 116.0(14) . . . . ? F7 B2 F4 B1 -115.7(14) . . . . ? F6 B2 F4 B1 1.8(17) . . . . ? F9 B3 F11 B4 145.9(12) . . . . ? F10 B3 F11 B4 19.9(17) . . . . ? F8 B3 F11 B4 -95.9(14) . . . . ? F12 B4 F11 B3 162.6(10) . . . . ? F13 B4 F11 B3 36.0(17) . . . . ? F14 B4 F11 B3 -79.1(15) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.672 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.076