Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Shie-Ming Peng' _publ_contact_author_address ; Department of Chemistry National Taiwan University 1 Sec. 4 Roosevelt Road Taipei 106 TAIWAN ; _publ_contact_author_email smpeng@ntu.edu.tw _publ_section_title ; Synthesis, structures, magnetism and electrochemical properties of triruthenium-acetylide complexes ; loop_ _publ_author_name 'Ching-Kuo Kuo' 'Jung-Che Chang' 'Chen-Yu Yeh' 'Gene-Hsiang Lee' ; Chih-Chieh Wang ; 'Shie-Ming Peng' data_ic10154 #(compound 1) _database_code_depnum_ccdc_archive 'CCDC 270949' _chemical_name_common (Ru3(CCFc))2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H60 Cl10 Fe2 N12 Ru3' _chemical_formula_weight 1826.70 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 23.9110(5) _cell_length_b 27.1780(5) _cell_length_c 21.8541(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14202.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7296 _exptl_absorpt_coefficient_mu 1.450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.611 _exptl_absorpt_correction_T_max 0.828 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26079 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7342 _reflns_number_gt 5813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.1705P)^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 mixed _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 -0.02(5) _refine_ls_number_reflns 7342 _refine_ls_number_parameters 407 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2338 _refine_ls_wR_factor_gt 0.2113 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.012 _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 0.04184(3) 0.42148(2) -0.27877(3) 0.0327(2) Uani 1 1 d . . . Ru2 Ru 0.0000 0.5000 -0.27841(5) 0.0319(3) Uani 1 2 d S . . Fe1 Fe 0.05909(7) 0.20491(6) -0.24560(11) 0.0594(5) Uani 1 1 d . . . N1 N -0.0359(3) 0.3947(3) -0.3131(4) 0.0370(18) Uani 1 1 d . . . N2 N -0.0772(3) 0.4673(3) -0.2812(5) 0.0367(16) Uani 1 1 d . . . N3 N -0.1153(3) 0.5437(3) -0.2501(4) 0.0351(17) Uani 1 1 d . . . N4 N 0.0168(3) 0.4152(3) -0.1875(4) 0.0340(17) Uani 1 1 d . . . N5 N 0.0000 0.5000 -0.1850(6) 0.035(3) Uani 1 2 d S . . N6 N 0.0650(3) 0.4358(3) -0.3698(4) 0.0342(16) Uani 1 1 d . . . N7 N 0.0000 0.5000 -0.3696(5) 0.031(2) Uani 1 2 d S . . C1 C -0.0380(4) 0.3520(4) -0.3432(5) 0.043(2) Uani 1 1 d . . . H1A H -0.0055 0.3320 -0.3445 0.051 Uiso 1 1 calc R . . C2 C -0.0850(5) 0.3362(4) -0.3720(6) 0.048(3) Uani 1 1 d . . . H2A H -0.0856 0.3044 -0.3901 0.058 Uiso 1 1 calc R . . C3 C -0.1323(4) 0.3662(4) -0.3754(5) 0.048(3) Uani 1 1 d . . . H3A H -0.1644 0.3564 -0.3980 0.057 Uiso 1 1 calc R . . C4 C -0.1307(4) 0.4106(4) -0.3444(5) 0.043(2) Uani 1 1 d . . . H4A H -0.1625 0.4315 -0.3444 0.052 Uiso 1 1 calc R . . C5 C -0.0821(4) 0.4248(4) -0.3130(4) 0.035(2) Uani 1 1 d . . . C6 C -0.1226(4) 0.4948(4) -0.2585(5) 0.038(2) Uani 1 1 d . . . C7 C -0.1723(4) 0.4699(4) -0.2388(6) 0.049(3) Uani 1 1 d . . . H7A H -0.1751 0.4351 -0.2415 0.059 Uiso 1 1 calc R . . C8 C -0.2161(5) 0.4976(4) -0.2159(6) 0.051(3) Uani 1 1 d . . . H8A H -0.2503 0.4822 -0.2045 0.061 Uiso 1 1 calc R . . C9 C -0.2091(4) 0.5503(4) -0.2096(6) 0.049(3) Uani 1 1 d . . . H9A H -0.2392 0.5706 -0.1966 0.059 Uiso 1 1 calc R . . C10 C -0.1574(4) 0.5703(4) -0.2230(5) 0.041(2) Uani 1 1 d . . . H10A H -0.1507 0.6039 -0.2131 0.050 Uiso 1 1 calc R . . C11 C 0.0154(4) 0.3709(4) -0.1569(5) 0.044(2) Uani 1 1 d . . . H11A H 0.0280 0.3428 -0.1789 0.053 Uiso 1 1 calc R . . C12 C -0.0017(4) 0.3631(5) -0.0998(6) 0.049(3) Uani 1 1 d . . . H12A H -0.0004 0.3314 -0.0815 0.059 Uiso 1 1 calc R . . C13 C -0.0221(4) 0.4055(5) -0.0673(5) 0.050(3) Uani 1 1 d . . . H13A H -0.0346 0.4022 -0.0263 0.060 Uiso 1 1 calc R . . C14 C -0.0238(4) 0.4509(4) -0.0954(5) 0.042(2) Uani 1 1 d . . . H14A H -0.0393 0.4785 -0.0750 0.051 Uiso 1 1 calc R . . C15 C -0.0019(3) 0.4555(4) -0.1550(4) 0.033(2) Uani 1 1 d . . . C16 C 0.1074(4) 0.4100(4) -0.3968(6) 0.048(3) Uani 1 1 d . . . H16A H 0.1243 0.3839 -0.3747 0.057 Uiso 1 1 calc R . . C17 C 0.1262(4) 0.4202(4) -0.4536(5) 0.046(3) Uani 1 1 d . . . H17A H 0.1550 0.4008 -0.4713 0.055 Uiso 1 1 calc R . . C18 C 0.1026(4) 0.4596(4) -0.4864(5) 0.045(2) Uani 1 1 d . . . H18A H 0.1159 0.4671 -0.5262 0.054 Uiso 1 1 calc R . . C19 C 0.0605(5) 0.4874(5) -0.4610(5) 0.053(3) Uani 1 1 d . . . H19A H 0.0452 0.5144 -0.4829 0.063 Uiso 1 1 calc R . . C20 C 0.0396(4) 0.4751(4) -0.4007(5) 0.042(2) Uani 1 1 d . . . C21 C 0.0753(3) 0.3540(3) -0.2780(6) 0.0352(19) Uani 1 1 d . . . C22 C 0.0934(4) 0.3127(4) -0.2735(5) 0.041(2) Uani 1 1 d . . . C23 C 0.1090(4) 0.2623(4) -0.2697(6) 0.048(3) Uani 1 1 d . . . C24 C 0.1330(5) 0.2363(6) -0.2176(6) 0.061(3) Uani 1 1 d . . . H24A H 0.1406 0.2507 -0.1763 0.073 Uiso 1 1 calc R . . C25 C 0.1401(5) 0.1862(5) -0.2347(9) 0.071(4) Uani 1 1 d . . . H25A H 0.1540 0.1596 -0.2070 0.086 Uiso 1 1 calc R . . C26 C 0.1240(6) 0.1795(5) -0.2960(9) 0.077(5) Uani 1 1 d . . . H26A H 0.1254 0.1482 -0.3200 0.093 Uiso 1 1 calc R . . C27 C 0.1059(5) 0.2269(4) -0.3175(6) 0.055(3) Uani 1 1 d . . . H27A H 0.0910 0.2336 -0.3595 0.066 Uiso 1 1 calc R . . C28 C -0.0032(7) 0.1569(6) -0.2518(14) 0.115(9) Uani 1 1 d . . . H28A H -0.0013 0.1263 -0.2772 0.138 Uiso 1 1 calc R . . C29 C 0.0175(7) 0.1595(7) -0.1843(11) 0.094(6) Uani 1 1 d . . . H29A H 0.0333 0.1324 -0.1587 0.113 Uiso 1 1 calc R . . C30 C 0.0095(8) 0.2078(9) -0.1685(13) 0.131(11) Uani 1 1 d . . . H30A H 0.0178 0.2241 -0.1285 0.157 Uiso 1 1 calc R . . C31 C -0.0186(7) 0.2321(6) -0.2293(14) 0.111(9) Uani 1 1 d . . . H31A H -0.0268 0.2681 -0.2320 0.134 Uiso 1 1 calc R . . C32 C -0.0216(5) 0.2044(5) -0.2758(10) 0.074(4) Uani 1 1 d . . . H32A H -0.0361 0.2123 -0.3175 0.089 Uiso 1 1 calc R . . C33 C 0.3412(7) 0.1406(6) 0.2166(9) 0.081(4) Uani 1 1 d . . . H33A H 0.3440 0.1646 0.1826 0.097 Uiso 1 1 calc R . . H33B H 0.3617 0.1540 0.2522 0.097 Uiso 1 1 calc R . . Cl1 Cl 0.2695(2) 0.1313(2) 0.2361(3) 0.1035(15) Uani 1 1 d . . . Cl2 Cl 0.3695(3) 0.0861(3) 0.1952(4) 0.139(3) Uani 1 1 d . . . C34 C 0.0714(9) 0.3000(19) 0.0066(8) 0.250 Uiso 1 1 d D . . H34A H 0.0484 0.3298 -0.0004 0.300 Uiso 1 1 calc R . . H34B H 0.0461 0.2713 0.0080 0.300 Uiso 1 1 calc R . . Cl3 Cl 0.1056(7) 0.3053(6) 0.0746(7) 0.241(6) Uiso 1 1 d D . . Cl4 Cl 0.1176(6) 0.2931(5) -0.0523(6) 0.207(4) Uiso 1 1 d D . . C35 C 0.2500 0.2500 0.1211(8) 0.21(2) Uiso 1 2 d SD . . H35A H 0.2816 0.2404 0.1625 0.251 Uiso 0.50 1 d P . . H35B H 0.2184 0.2596 0.1625 0.251 Uiso 0.50 1 d P . . Cl5 Cl 0.2724 0.2974 0.0764 0.250 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0259(3) 0.0272(4) 0.0450(4) -0.0009(4) 0.0001(3) 0.0016(3) Ru2 0.0247(4) 0.0267(5) 0.0442(5) 0.000 0.000 0.0023(3) Fe1 0.0381(8) 0.0388(9) 0.1013(14) 0.0090(9) 0.0105(9) 0.0039(7) N1 0.029(4) 0.029(4) 0.053(5) 0.000(4) 0.001(3) -0.002(3) N2 0.023(3) 0.031(4) 0.056(4) 0.014(4) 0.001(4) -0.003(3) N3 0.036(4) 0.026(4) 0.044(4) 0.005(3) 0.000(3) 0.000(3) N4 0.027(4) 0.036(4) 0.039(4) 0.002(4) -0.001(3) 0.001(3) N5 0.019(5) 0.040(7) 0.045(7) 0.000 0.000 0.001(4) N6 0.024(3) 0.035(4) 0.044(4) -0.002(4) 0.000(3) -0.001(3) N7 0.038(6) 0.016(5) 0.039(6) 0.000 0.000 0.003(4) C1 0.028(4) 0.032(5) 0.068(7) -0.001(5) -0.003(4) -0.002(4) C2 0.042(5) 0.039(6) 0.063(7) -0.021(5) -0.004(5) -0.002(5) C3 0.030(5) 0.042(6) 0.070(7) -0.026(5) -0.001(5) -0.006(4) C4 0.034(5) 0.037(5) 0.059(6) -0.013(5) -0.001(4) -0.003(4) C5 0.026(4) 0.045(6) 0.033(5) -0.004(4) -0.003(4) 0.003(4) C6 0.029(4) 0.031(5) 0.054(6) 0.010(4) -0.004(4) -0.001(4) C7 0.039(5) 0.037(5) 0.072(7) 0.015(5) 0.007(5) -0.008(4) C8 0.040(5) 0.034(5) 0.080(8) 0.011(5) 0.016(5) 0.006(4) C9 0.034(5) 0.041(6) 0.072(7) 0.002(5) 0.009(5) 0.002(4) C10 0.037(5) 0.030(5) 0.057(6) 0.007(5) 0.010(4) 0.009(4) C11 0.037(5) 0.037(6) 0.059(7) -0.004(5) -0.001(4) 0.002(4) C12 0.037(5) 0.051(7) 0.059(7) 0.019(5) 0.008(4) 0.000(5) C13 0.035(5) 0.056(7) 0.058(7) 0.010(6) 0.008(5) 0.000(5) C14 0.022(4) 0.043(6) 0.061(7) 0.007(5) 0.009(4) 0.007(4) C15 0.017(4) 0.039(5) 0.043(5) 0.009(4) -0.005(3) 0.001(3) C16 0.035(5) 0.038(6) 0.071(7) -0.012(5) 0.007(5) 0.004(4) C17 0.032(5) 0.051(6) 0.055(6) -0.008(5) 0.012(4) 0.003(4) C18 0.040(5) 0.044(6) 0.051(6) -0.004(5) 0.006(4) 0.007(5) C19 0.040(6) 0.069(8) 0.049(6) 0.012(6) 0.008(5) -0.004(5) C20 0.039(5) 0.038(5) 0.050(6) -0.001(5) 0.005(4) -0.007(4) C21 0.030(4) 0.029(5) 0.047(5) -0.016(5) 0.006(5) -0.005(3) C22 0.030(4) 0.044(5) 0.049(6) 0.003(5) 0.012(4) -0.002(4) C23 0.040(5) 0.035(5) 0.068(8) 0.011(5) 0.008(5) 0.006(4) C24 0.041(6) 0.082(9) 0.060(7) 0.014(7) 0.001(5) 0.005(6) C25 0.039(6) 0.046(7) 0.129(14) 0.020(8) 0.022(7) 0.018(5) C26 0.067(9) 0.046(7) 0.119(14) -0.011(8) 0.020(9) 0.009(6) C27 0.053(6) 0.036(6) 0.076(8) 0.001(6) -0.003(6) -0.011(5) C28 0.067(10) 0.044(8) 0.23(3) -0.035(12) 0.030(14) -0.019(7) C29 0.061(9) 0.063(10) 0.159(19) 0.018(11) 0.021(11) 0.002(8) C30 0.085(13) 0.119(18) 0.19(2) -0.068(18) 0.084(16) -0.038(13) C31 0.062(9) 0.051(9) 0.22(3) 0.036(14) 0.048(13) 0.028(8) C32 0.041(6) 0.057(8) 0.125(12) -0.019(10) -0.003(8) -0.013(5) C33 0.076(9) 0.090(11) 0.077(9) 0.002(10) -0.001(8) 0.002(8) Cl1 0.074(3) 0.096(3) 0.140(4) -0.004(3) -0.006(2) -0.016(2) Cl2 0.125(5) 0.121(5) 0.172(6) -0.049(4) -0.020(4) 0.036(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 C21 2.000(9) . ? Ru1 N4 2.090(8) . ? Ru1 N3 2.091(8) 2_565 ? Ru1 N6 2.101(8) . ? Ru1 N1 2.133(8) . ? Ru1 Ru2 2.3568(6) . ? Ru2 N7 1.994(12) . ? Ru2 N5 2.041(12) . ? Ru2 N2 2.050(7) 2_565 ? Ru2 N2 2.050(7) . ? Ru2 Ru1 2.3568(6) 2_565 ? Fe1 C28 1.985(15) . ? Fe1 C25 2.017(12) . ? Fe1 C27 2.020(13) . ? Fe1 C26 2.025(14) . ? Fe1 C31 2.030(14) . ? Fe1 C23 2.033(11) . ? Fe1 C32 2.038(14) . ? Fe1 C24 2.055(14) . ? Fe1 C30 2.06(2) . ? Fe1 C29 2.075(19) . ? N1 C1 1.333(14) . ? N1 C5 1.375(12) . ? N2 C5 1.353(13) . ? N2 C6 1.409(13) . ? N3 C6 1.352(13) . ? N3 C10 1.376(12) . ? N3 Ru1 2.091(8) 2_565 ? N4 C15 1.379(13) . ? N4 C11 1.379(14) . ? N5 C15 1.377(11) 2_565 ? N5 C15 1.377(11) . ? N6 C16 1.365(13) . ? N6 C20 1.403(14) . ? N7 C20 1.347(12) 2_565 ? N7 C20 1.347(12) . ? C1 C2 1.357(14) . ? C2 C3 1.397(16) . ? C3 C4 1.385(14) . ? C4 C5 1.404(14) . ? C6 C7 1.434(14) . ? C7 C8 1.383(16) . ? C8 C9 1.451(16) . ? C9 C10 1.381(15) . ? C11 C12 1.328(17) . ? C12 C13 1.439(18) . ? C13 C14 1.379(16) . ? C14 C15 1.408(15) . ? C16 C17 1.348(17) . ? C17 C18 1.407(16) . ? C18 C19 1.374(16) . ? C19 C20 1.448(16) . ? C21 C22 1.207(15) . ? C22 C23 1.424(16) . ? C23 C27 1.422(18) . ? C23 C24 1.458(18) . ? C24 C25 1.42(2) . ? C25 C26 1.41(3) . ? C26 C27 1.44(2) . ? C28 C32 1.46(3) . ? C28 C29 1.56(4) . ? C29 C30 1.37(3) . ? C30 C31 1.63(4) . ? C31 C32 1.27(3) . ? C33 Cl2 1.694(18) . ? C33 Cl1 1.783(17) . ? C34 Cl3 1.703(10) . ? C34 Cl4 1.706(10) . ? C35 Cl5 1.704(10) 14 ? C35 Cl5 1.704(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Ru1 N4 91.8(4) . . ? C21 Ru1 N3 94.4(3) . 2_565 ? N4 Ru1 N3 89.5(3) . 2_565 ? C21 Ru1 N6 94.1(4) . . ? N4 Ru1 N6 173.9(3) . . ? N3 Ru1 N6 88.7(3) 2_565 . ? C21 Ru1 N1 92.2(3) . . ? N4 Ru1 N1 93.4(3) . . ? N3 Ru1 N1 172.7(3) 2_565 . ? N6 Ru1 N1 87.7(3) . . ? C21 Ru1 Ru2 178.3(3) . . ? N4 Ru1 Ru2 87.1(2) . . ? N3 Ru1 Ru2 86.9(2) 2_565 . ? N6 Ru1 Ru2 87.0(2) . . ? N1 Ru1 Ru2 86.6(2) . . ? N7 Ru2 N5 180.000(1) . . ? N7 Ru2 N2 88.3(3) . 2_565 ? N5 Ru2 N2 91.7(3) . 2_565 ? N7 Ru2 N2 88.3(3) . . ? N5 Ru2 N2 91.7(3) . . ? N2 Ru2 N2 176.5(6) 2_565 . ? N7 Ru2 Ru1 89.81(3) . 2_565 ? N5 Ru2 Ru1 90.19(3) . 2_565 ? N2 Ru2 Ru1 89.4(2) 2_565 2_565 ? N2 Ru2 Ru1 90.6(2) . 2_565 ? N7 Ru2 Ru1 89.81(3) . . ? N5 Ru2 Ru1 90.19(3) . . ? N2 Ru2 Ru1 90.6(2) 2_565 . ? N2 Ru2 Ru1 89.4(2) . . ? Ru1 Ru2 Ru1 179.61(7) 2_565 . ? C28 Fe1 C25 124.3(7) . . ? C28 Fe1 C27 123.8(9) . . ? C25 Fe1 C27 68.6(6) . . ? C28 Fe1 C26 108.3(7) . . ? C25 Fe1 C26 40.8(7) . . ? C27 Fe1 C26 41.6(6) . . ? C28 Fe1 C31 64.2(7) . . ? C25 Fe1 C31 161.7(11) . . ? C27 Fe1 C31 122.4(8) . . ? C26 Fe1 C31 157.0(11) . . ? C28 Fe1 C23 158.0(10) . . ? C25 Fe1 C23 70.1(5) . . ? C27 Fe1 C23 41.1(5) . . ? C26 Fe1 C23 70.7(5) . . ? C31 Fe1 C23 107.7(6) . . ? C28 Fe1 C32 42.5(8) . . ? C25 Fe1 C32 161.0(7) . . ? C27 Fe1 C32 105.9(7) . . ? C26 Fe1 C32 123.2(8) . . ? C31 Fe1 C32 36.3(9) . . ? C23 Fe1 C32 118.5(6) . . ? C28 Fe1 C24 159.8(9) . . ? C25 Fe1 C24 40.9(6) . . ? C27 Fe1 C24 68.5(5) . . ? C26 Fe1 C24 69.2(6) . . ? C31 Fe1 C24 125.7(9) . . ? C23 Fe1 C24 41.8(5) . . ? C32 Fe1 C24 155.9(6) . . ? C28 Fe1 C30 69.5(9) . . ? C25 Fe1 C30 117.7(10) . . ? C27 Fe1 C30 160.6(7) . . ? C26 Fe1 C30 154.0(10) . . ? C31 Fe1 C30 46.8(11) . . ? C23 Fe1 C30 121.3(7) . . ? C32 Fe1 C30 73.7(10) . . ? C24 Fe1 C30 103.6(8) . . ? C28 Fe1 C29 45.1(10) . . ? C25 Fe1 C29 103.6(7) . . ? C27 Fe1 C29 160.7(7) . . ? C26 Fe1 C29 121.1(7) . . ? C31 Fe1 C29 70.4(7) . . ? C23 Fe1 C29 154.8(8) . . ? C32 Fe1 C29 75.6(8) . . ? C24 Fe1 C29 117.8(7) . . ? C30 Fe1 C29 38.7(8) . . ? C1 N1 C5 119.2(8) . . ? C1 N1 Ru1 120.3(6) . . ? C5 N1 Ru1 119.7(6) . . ? C5 N2 C6 124.6(7) . . ? C5 N2 Ru2 117.6(6) . . ? C6 N2 Ru2 116.9(6) . . ? C6 N3 C10 118.7(8) . . ? C6 N3 Ru1 120.9(6) . 2_565 ? C10 N3 Ru1 120.3(6) . 2_565 ? C15 N4 C11 115.8(8) . . ? C15 N4 Ru1 121.3(6) . . ? C11 N4 Ru1 122.8(7) . . ? C15 N5 C15 123.2(12) 2_565 . ? C15 N5 Ru2 118.4(6) 2_565 . ? C15 N5 Ru2 118.4(6) . . ? C16 N6 C20 120.2(9) . . ? C16 N6 Ru1 120.7(7) . . ? C20 N6 Ru1 118.8(6) . . ? C20 N7 C20 119.6(13) 2_565 . ? C20 N7 Ru2 120.2(7) 2_565 . ? C20 N7 Ru2 120.2(7) . . ? N1 C1 C2 122.4(9) . . ? C1 C2 C3 120.7(10) . . ? C4 C3 C2 117.3(9) . . ? C3 C4 C5 120.1(10) . . ? N2 C5 N1 116.1(8) . . ? N2 C5 C4 123.8(8) . . ? N1 C5 C4 120.1(9) . . ? N3 C6 N2 118.0(8) . . ? N3 C6 C7 122.1(10) . . ? N2 C6 C7 119.6(9) . . ? C8 C7 C6 118.7(10) . . ? C7 C8 C9 118.9(10) . . ? C10 C9 C8 118.2(10) . . ? N3 C10 C9 122.6(10) . . ? C12 C11 N4 127.0(10) . . ? C11 C12 C13 116.1(11) . . ? C14 C13 C12 120.4(10) . . ? C13 C14 C15 118.7(10) . . ? N5 C15 N4 116.2(9) . . ? N5 C15 C14 122.0(9) . . ? N4 C15 C14 121.7(9) . . ? C17 C16 N6 122.7(11) . . ? C16 C17 C18 119.4(10) . . ? C19 C18 C17 120.4(10) . . ? C18 C19 C20 119.6(11) . . ? N7 C20 N6 116.4(10) . . ? N7 C20 C19 125.8(11) . . ? N6 C20 C19 117.6(10) . . ? C22 C21 Ru1 175.1(10) . . ? C21 C22 C23 174.1(11) . . ? C27 C23 C22 126.5(11) . . ? C27 C23 C24 105.5(11) . . ? C22 C23 C24 127.9(12) . . ? C27 C23 Fe1 69.0(7) . . ? C22 C23 Fe1 126.8(7) . . ? C24 C23 Fe1 69.9(7) . . ? C25 C24 C23 107.8(13) . . ? C25 C24 Fe1 68.1(8) . . ? C23 C24 Fe1 68.3(7) . . ? C26 C25 C24 110.0(12) . . ? C26 C25 Fe1 69.9(8) . . ? C24 C25 Fe1 71.0(7) . . ? C25 C26 C27 106.2(13) . . ? C25 C26 Fe1 69.3(8) . . ? C27 C26 Fe1 69.0(8) . . ? C23 C27 C26 110.4(13) . . ? C23 C27 Fe1 69.9(7) . . ? C26 C27 Fe1 69.4(8) . . ? C32 C28 C29 113.2(15) . . ? C32 C28 Fe1 70.7(8) . . ? C29 C28 Fe1 70.5(10) . . ? C30 C29 C28 104(2) . . ? C30 C29 Fe1 70.1(12) . . ? C28 C29 Fe1 64.4(10) . . ? C29 C30 C31 104(2) . . ? C29 C30 Fe1 71.2(12) . . ? C31 C30 Fe1 65.6(11) . . ? C32 C31 C30 115.9(14) . . ? C32 C31 Fe1 72.2(9) . . ? C30 C31 Fe1 67.6(8) . . ? C31 C32 C28 102.8(19) . . ? C31 C32 Fe1 71.5(10) . . ? C28 C32 Fe1 66.8(9) . . ? Cl2 C33 Cl1 109.0(10) . . ? Cl3 C34 Cl4 110.9(14) . . ? Cl5 C35 Cl5 110.0(9) 14 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.762 _refine_diff_density_min -1.647 _refine_diff_density_rms 0.325 #===END data_ic10132 #(compound 2) _database_code_depnum_ccdc_archive 'CCDC 270950' _chemical_name_common (Ru3(CCPh)2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H62 N12 O10 Ru3' _chemical_formula_weight 1366.39 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' 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 Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 25.4999(7) _cell_length_b 26.1497(7) _cell_length_c 21.5252(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14353.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.46 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5552 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.611 _exptl_absorpt_correction_T_max 0.828 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31911 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7841 _reflns_number_gt 6114 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.1669P)^2^+45.7318P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00167(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(7) _refine_ls_number_reflns 7841 _refine_ls_number_parameters 325 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1079 _refine_ls_R_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.2444 _refine_ls_wR_factor_gt 0.2215 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.03999(2) 0.08095(2) 0.04116(3) 0.0509(3) Uani 1 1 d . . . Ru2 Ru 0.0000 0.0000 0.04104(5) 0.0486(3) Uani 1 2 d S . . N1 N 0.1092(3) 0.0438(3) 0.0100(4) 0.0552(17) Uani 1 1 d . . . N2 N 0.0720(2) -0.0332(2) 0.0436(4) 0.0518(14) Uani 1 1 d . . . N3 N 0.0316(3) -0.1088(3) 0.0764(4) 0.0563(17) Uani 1 1 d . . . N4 N 0.0132(3) 0.0879(3) -0.0510(4) 0.0537(17) Uani 1 1 d . . . N5 N 0.0000 0.0000 -0.0516(5) 0.051(2) Uani 1 2 d S . . N6 N 0.0638(3) 0.0646(3) 0.1313(4) 0.0538(16) Uani 1 1 d . . . N7 N 0.0000 0.0000 0.1359(5) 0.051(2) Uani 1 2 d S . . C1 C 0.1482(4) 0.0687(4) -0.0172(5) 0.060(2) Uani 1 1 d . . . H1A H 0.1437 0.1043 -0.0247 0.072 Uiso 1 1 calc R . . C2 C 0.1936(4) 0.0471(4) -0.0350(5) 0.068(2) Uani 1 1 d . . . H2A H 0.2210 0.0674 -0.0517 0.082 Uiso 1 1 calc R . . C3 C 0.1998(4) -0.0044(4) -0.0288(6) 0.071(3) Uani 1 1 d . . . H3A H 0.2303 -0.0210 -0.0440 0.085 Uiso 1 1 calc R . . C4 C 0.1608(3) -0.0317(4) 0.0000(5) 0.065(2) Uani 1 1 d . . . H4A H 0.1652 -0.0673 0.0072 0.078 Uiso 1 1 calc R . . C5 C 0.1151(3) -0.0075(3) 0.0186(5) 0.058(2) Uani 1 1 d . . . C6 C 0.0761(3) -0.0800(3) 0.0760(4) 0.0512(19) Uani 1 1 d . . . C7 C 0.1205(4) -0.0954(4) 0.1077(5) 0.064(2) Uani 1 1 d . . . H7A H 0.1508 -0.0742 0.1074 0.077 Uiso 1 1 calc R . . C8 C 0.1217(5) -0.1388(5) 0.1383(6) 0.079(3) Uani 1 1 d . . . H8A H 0.1518 -0.1484 0.1615 0.095 Uiso 1 1 calc R . . C9 C 0.0770(4) -0.1710(4) 0.1360(5) 0.064(2) Uani 1 1 d . . . H9A H 0.0772 -0.2040 0.1544 0.077 Uiso 1 1 calc R . . C10 C 0.0341(3) -0.1528(4) 0.1066(5) 0.062(2) Uani 1 1 d . . . H10A H 0.0033 -0.1732 0.1076 0.074 Uiso 1 1 calc R . . C11 C 0.0082(4) 0.1355(3) -0.0799(5) 0.062(2) Uani 1 1 d . . . H11A H 0.0188 0.1650 -0.0574 0.074 Uiso 1 1 calc R . . C12 C -0.0106(4) 0.1419(4) -0.1373(5) 0.065(2) Uani 1 1 d . . . H12A H -0.0121 0.1747 -0.1562 0.078 Uiso 1 1 calc R . . C13 C -0.0278(4) 0.0987(4) -0.1679(5) 0.064(2) Uani 1 1 d . . . H13A H -0.0428 0.1025 -0.2080 0.077 Uiso 1 1 calc R . . C14 C -0.0244(3) 0.0509(4) -0.1434(5) 0.064(2) Uani 1 1 d . . . H14A H -0.0361 0.0218 -0.1658 0.076 Uiso 1 1 calc R . . C15 C -0.0026(3) 0.0463(3) -0.0829(4) 0.0490(19) Uani 1 1 d . . . C16 C 0.1040(3) 0.0884(4) 0.1583(5) 0.061(2) Uani 1 1 d . . . H16A H 0.1199 0.1160 0.1367 0.073 Uiso 1 1 calc R . . C17 C 0.1239(5) 0.0754(4) 0.2154(6) 0.075(3) Uani 1 1 d . . . H17A H 0.1531 0.0936 0.2316 0.090 Uiso 1 1 calc R . . C18 C 0.1018(5) 0.0358(5) 0.2496(6) 0.081(3) Uani 1 1 d . . . H18A H 0.1159 0.0251 0.2883 0.097 Uiso 1 1 calc R . . C19 C 0.0576(5) 0.0127(4) 0.2237(6) 0.077(3) Uani 1 1 d . . . H19A H 0.0401 -0.0132 0.2467 0.092 Uiso 1 1 calc R . . C20 C 0.0384(3) 0.0257(3) 0.1664(5) 0.055(2) Uani 1 1 d . . . C21 C 0.0734(3) 0.1515(3) 0.0416(6) 0.0577(18) Uani 1 1 d . . . C22 C 0.0934(2) 0.1898(2) 0.0326(3) 0.063(2) Uani 1 1 d . . . C23 C 0.1214(2) 0.2410(2) 0.0174(3) 0.074(3) Uani 1 1 d R . . C24 C 0.1491(2) 0.2539(2) -0.0361(3) 0.131(6) Uiso 1 1 d R . . H24A H 0.1530 0.2296 -0.0686 0.158 Uiso 1 1 calc R . . C25 C 0.1709(2) 0.3024(2) -0.0419(3) 0.177(10) Uiso 1 1 d R . . H25A H 0.1898 0.3112 -0.0784 0.213 Uiso 1 1 calc R . . C26 C 0.1652(2) 0.3379(2) 0.0056(3) 0.126(6) Uiso 1 1 d R . . H26A H 0.1801 0.3710 0.0016 0.151 Uiso 1 1 calc R . . C27 C 0.1376(2) 0.3250(2) 0.0591(3) 0.125(6) Uiso 1 1 d R . . H27A H 0.1336 0.3492 0.0916 0.150 Uiso 1 1 calc R . . C28 C 0.1157(2) 0.2765(2) 0.0649(3) 0.094(4) Uiso 1 1 d R . . H28A H 0.0968 0.2677 0.1014 0.113 Uiso 1 1 calc R . . O1 O 0.0126(4) 0.3755(3) -0.2118(8) 0.135(4) Uani 1 1 d . . . H1 H 0.0443 0.3600 -0.2038 0.202 Uiso 1 1 d . . . H1' H 0.0114 0.3834 -0.2544 0.202 Uiso 1 1 d . . . O2 O -0.0077(3) 0.2793(3) -0.0838(6) 0.125(5) Uani 1 1 d . . . H2 H 0.0178 0.2588 -0.1142 0.187 Uiso 1 1 d . . . H2' H -0.0025 0.2655 -0.0323 0.187 Uiso 1 1 d . . . O3 O 0.0912(4) 0.2210(4) -0.2172(11) 0.172(7) Uani 1 1 d . . . H3 H 0.1228 0.2283 -0.2360 0.098 Uiso 1 1 d . . . H3' H 0.0758 0.2519 -0.2113 0.024 Uiso 1 1 d . . . O4 O 0.1810(4) 0.4340(4) -0.1408(6) 0.118(3) Uani 1 1 d . . . H4 H 0.1471 0.4240 -0.1331 0.177 Uiso 1 1 d . . . H4' H 0.1952 0.4383 -0.1005 0.177 Uiso 1 1 d . . . O5 O 0.2889(5) 0.3381(5) -0.1487(7) 0.130(4) Uani 1 1 d . . . H5 H 0.2712 0.3585 -0.1117 0.195 Uiso 1 1 d . . . H5' H 0.3168 0.3230 -0.1304 0.021 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0376(3) 0.0422(3) 0.0729(4) -0.0020(3) -0.0016(3) -0.0037(2) Ru2 0.0340(4) 0.0422(4) 0.0696(6) 0.000 0.000 -0.0029(3) N1 0.040(3) 0.045(3) 0.081(5) -0.008(3) -0.004(3) -0.005(3) N2 0.034(3) 0.039(3) 0.082(4) -0.003(4) 0.006(4) 0.001(2) N3 0.044(4) 0.044(3) 0.081(5) 0.004(3) 0.008(3) 0.003(3) N4 0.043(4) 0.042(3) 0.076(5) 0.005(3) -0.003(3) 0.001(3) N5 0.046(6) 0.048(5) 0.059(6) 0.000 0.000 -0.014(4) N6 0.044(4) 0.044(3) 0.073(4) -0.005(3) 0.001(3) 0.001(3) N7 0.039(5) 0.049(5) 0.066(6) 0.000 0.000 0.004(4) C1 0.054(5) 0.051(4) 0.075(6) -0.004(4) 0.006(4) -0.008(4) C2 0.045(5) 0.077(6) 0.082(6) -0.005(5) 0.011(4) -0.017(4) C3 0.044(5) 0.074(6) 0.095(7) -0.018(6) 0.010(5) -0.005(4) C4 0.041(4) 0.059(5) 0.095(7) -0.006(5) 0.001(5) 0.004(4) C5 0.047(4) 0.047(4) 0.079(6) 0.007(4) -0.002(4) -0.002(3) C6 0.035(4) 0.055(4) 0.064(5) -0.004(4) 0.005(4) 0.008(3) C7 0.052(5) 0.052(5) 0.088(7) 0.000(5) -0.015(5) 0.000(4) C8 0.068(6) 0.081(7) 0.088(7) 0.018(6) -0.010(6) 0.022(6) C9 0.050(5) 0.056(5) 0.086(7) 0.023(5) 0.001(5) 0.002(4) C10 0.043(4) 0.054(5) 0.087(7) 0.013(4) 0.004(4) -0.002(4) C11 0.054(5) 0.040(4) 0.092(7) 0.005(4) -0.004(5) 0.007(4) C12 0.054(5) 0.056(5) 0.086(7) 0.016(5) -0.011(5) 0.010(4) C13 0.062(5) 0.052(5) 0.079(6) 0.004(4) 0.006(5) 0.007(4) C14 0.044(5) 0.058(5) 0.089(7) -0.005(5) -0.005(4) -0.008(4) C15 0.032(4) 0.044(4) 0.071(6) -0.001(4) 0.004(4) -0.002(3) C16 0.035(4) 0.059(5) 0.088(7) -0.011(4) -0.003(4) -0.010(3) C17 0.067(6) 0.069(6) 0.090(7) -0.003(5) -0.027(6) -0.024(5) C18 0.079(7) 0.077(7) 0.086(8) -0.008(6) -0.022(6) -0.010(6) C19 0.072(7) 0.066(6) 0.091(7) 0.001(5) -0.004(6) -0.009(5) C20 0.051(5) 0.046(4) 0.068(6) -0.004(4) -0.002(4) -0.002(4) C21 0.048(4) 0.045(4) 0.080(5) 0.002(5) -0.013(5) -0.009(3) C22 0.049(4) 0.056(4) 0.085(7) 0.004(5) -0.004(5) 0.001(4) C23 0.054(5) 0.045(4) 0.121(9) 0.013(5) -0.024(5) -0.003(4) O1 0.078(5) 0.055(4) 0.271(14) 0.008(8) -0.024(8) -0.026(4) O2 0.073(5) 0.045(4) 0.255(14) -0.010(5) -0.084(7) 0.024(3) O3 0.101(7) 0.073(5) 0.34(2) -0.004(10) 0.030(11) 0.022(5) O4 0.102(7) 0.108(7) 0.144(9) 0.033(7) -0.028(6) 0.016(6) O5 0.124(9) 0.119(8) 0.148(10) 0.029(7) -0.008(7) -0.057(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C21 2.031(7) . ? Ru1 N6 2.079(8) . ? Ru1 N4 2.106(8) . ? Ru1 N3 2.106(7) 2 ? Ru1 N1 2.125(7) . ? Ru1 Ru2 2.3497(5) . ? Ru2 N5 1.993(10) . ? Ru2 N2 2.031(6) 2 ? Ru2 N2 2.031(6) . ? Ru2 N7 2.041(12) . ? Ru2 Ru1 2.3497(5) 2 ? N1 C1 1.325(12) . ? N1 C5 1.361(11) . ? N2 C5 1.397(11) . ? N2 C6 1.412(11) . ? N3 C10 1.322(12) . ? N3 C6 1.364(11) . ? N3 Ru1 2.106(7) 2 ? N4 C15 1.349(11) . ? N4 C11 1.395(11) . ? N5 C15 1.388(10) . ? N5 C15 1.388(10) 2 ? N6 C16 1.332(11) . ? N6 C20 1.423(12) . ? N7 C20 1.357(10) . ? N7 C20 1.357(10) 2 ? C1 C2 1.345(14) . ? C2 C3 1.362(16) . ? C3 C4 1.370(15) . ? C4 C5 1.386(13) . ? C6 C7 1.383(13) . ? C7 C8 1.313(15) . ? C8 C9 1.418(16) . ? C9 C10 1.351(13) . ? C11 C12 1.336(15) . ? C12 C13 1.379(14) . ? C13 C14 1.358(14) . ? C14 C15 1.420(15) . ? C16 C17 1.371(16) . ? C17 C18 1.391(17) . ? C18 C19 1.394(16) . ? C19 C20 1.369(16) . ? C21 C22 1.141(9) . ? C22 C23 1.5527 . ? C23 C24 1.3900 . ? C23 C28 1.3901 . ? C24 C25 1.3900 . ? C25 C26 1.3901 . ? C26 C27 1.3900 . ? C27 C28 1.3899 . ? 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 C21 Ru1 N6 93.5(4) . . ? C21 Ru1 N4 93.5(4) . . ? N6 Ru1 N4 172.9(3) . . ? C21 Ru1 N3 92.7(3) . 2 ? N6 Ru1 N3 89.3(3) . 2 ? N4 Ru1 N3 91.6(3) . 2 ? C21 Ru1 N1 93.9(3) . . ? N6 Ru1 N1 87.6(3) . . ? N4 Ru1 N1 90.7(3) . . ? N3 Ru1 N1 172.8(3) 2 . ? C21 Ru1 Ru2 179.0(3) . . ? N6 Ru1 Ru2 86.7(2) . . ? N4 Ru1 Ru2 86.34(19) . . ? N3 Ru1 Ru2 86.31(19) 2 . ? N1 Ru1 Ru2 87.03(18) . . ? N5 Ru2 N2 91.6(3) . 2 ? N5 Ru2 N2 91.6(3) . . ? N2 Ru2 N2 176.8(5) 2 . ? N5 Ru2 N7 180.0 . . ? N2 Ru2 N7 88.4(3) 2 . ? N2 Ru2 N7 88.4(3) . . ? N5 Ru2 Ru1 90.06(3) . . ? N2 Ru2 Ru1 90.42(16) 2 . ? N2 Ru2 Ru1 89.58(16) . . ? N7 Ru2 Ru1 89.94(3) . . ? N5 Ru2 Ru1 90.06(3) . 2 ? N2 Ru2 Ru1 89.58(16) 2 2 ? N2 Ru2 Ru1 90.42(16) . 2 ? N7 Ru2 Ru1 89.94(3) . 2 ? Ru1 Ru2 Ru1 179.87(7) . 2 ? C1 N1 C5 117.6(8) . . ? C1 N1 Ru1 122.5(6) . . ? C5 N1 Ru1 119.9(6) . . ? C5 N2 C6 123.2(6) . . ? C5 N2 Ru2 119.7(5) . . ? C6 N2 Ru2 116.9(5) . . ? C10 N3 C6 116.3(8) . . ? C10 N3 Ru1 121.3(6) . 2 ? C6 N3 Ru1 121.9(5) . 2 ? C15 N4 C11 117.7(8) . . ? C15 N4 Ru1 120.5(6) . . ? C11 N4 Ru1 121.8(6) . . ? C15 N5 C15 121.8(11) . 2 ? C15 N5 Ru2 119.1(5) . . ? C15 N5 Ru2 119.1(5) 2 . ? C16 N6 C20 116.9(8) . . ? C16 N6 Ru1 122.4(7) . . ? C20 N6 Ru1 120.6(6) . . ? C20 N7 C20 122.1(12) . 2 ? C20 N7 Ru2 119.0(6) . . ? C20 N7 Ru2 119.0(6) 2 . ? N1 C1 C2 124.3(9) . . ? C1 C2 C3 119.3(9) . . ? C2 C3 C4 118.3(9) . . ? C3 C4 C5 120.2(10) . . ? N1 C5 C4 120.1(8) . . ? N1 C5 N2 116.1(8) . . ? C4 C5 N2 123.7(8) . . ? N3 C6 C7 121.2(8) . . ? N3 C6 N2 114.8(7) . . ? C7 C6 N2 123.9(8) . . ? C8 C7 C6 121.2(9) . . ? C7 C8 C9 118.6(9) . . ? C10 C9 C8 117.2(8) . . ? N3 C10 C9 125.2(8) . . ? C12 C11 N4 123.8(9) . . ? C11 C12 C13 116.9(9) . . ? C14 C13 C12 123.2(10) . . ? C13 C14 C15 117.3(9) . . ? N4 C15 N5 116.2(8) . . ? N4 C15 C14 121.0(8) . . ? N5 C15 C14 122.6(8) . . ? N6 C16 C17 124.0(9) . . ? C16 C17 C18 120.5(9) . . ? C17 C18 C19 116.0(11) . . ? C20 C19 C18 122.8(11) . . ? N7 C20 C19 124.9(9) . . ? N7 C20 N6 115.2(9) . . ? C19 C20 N6 119.4(8) . . ? C22 C21 Ru1 169.8(11) . . ? C21 C22 C23 177.4(8) . . ? C24 C23 C28 120.0 . . ? C24 C23 C22 128.1 . . ? C28 C23 C22 111.9 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C23 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.260 _refine_diff_density_min -1.506 _refine_diff_density_rms 0.378 #===END data_ic10266 #(compound 3) _database_code_depnum_ccdc_archive 'CCDC 270951' _chemical_name_common (Ru3(CCPhOCH3)2)(BF4) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H58 B Cl8 F4 N12 O4 Ru3' _chemical_formula_weight 1708.82 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 24.3107(5) _cell_length_b 24.5552(5) _cell_length_c 23.5200(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14040.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.46 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6840 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.703 _exptl_absorpt_correction_T_max 0.869 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24086 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7497 _reflns_number_gt 6311 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.1152P)^2^+44.9097P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00066(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) _refine_ls_number_reflns 7497 _refine_ls_number_parameters 427 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1725 _refine_ls_wR_factor_gt 0.1582 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.005 _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 1.160604(19) -0.212831(18) -0.040022(19) 0.03253(17) Uani 1 1 d . . . Ru2 Ru 1.2500 -0.2500 -0.03980(3) 0.03037(19) Uani 1 2 d S . . N1 N 1.1336(2) -0.2901(2) -0.0096(3) 0.0363(12) Uani 1 1 d . . . N2 N 1.2179(2) -0.3261(2) -0.0374(3) 0.0353(10) Uani 1 1 d . . . N3 N 1.3031(2) -0.3606(2) -0.0674(3) 0.0373(13) Uani 1 1 d . . . N4 N 1.1758(2) -0.1895(2) 0.0447(2) 0.0340(12) Uani 1 1 d . . . N5 N 1.2500 -0.2500 0.0451(3) 0.0326(18) Uani 1 2 d S . . N6 N 1.1546(2) -0.2376(2) -0.1251(3) 0.0366(13) Uani 1 1 d . . . N7 N 1.2500 -0.2500 -0.1266(4) 0.037(2) Uani 1 2 d S . . O1 O 0.8156(3) -0.1046(4) -0.0402(7) 0.130(4) Uani 1 1 d . . . C1 C 1.0842(3) -0.2950(3) 0.0168(3) 0.0438(17) Uani 1 1 d . . . H1A H 1.0594 -0.2651 0.0159 0.053 Uiso 1 1 calc R . . C2 C 1.0690(3) -0.3409(3) 0.0442(3) 0.0478(18) Uani 1 1 d . . . H2A H 1.0333 -0.3435 0.0605 0.057 Uiso 1 1 calc R . . C3 C 1.1051(3) -0.3839(3) 0.0486(4) 0.0457(18) Uani 1 1 d . . . H3A H 1.0954 -0.4155 0.0696 0.055 Uiso 1 1 calc R . . C4 C 1.1559(3) -0.3804(3) 0.0219(3) 0.0412(16) Uani 1 1 d . . . H4A H 1.1817 -0.4093 0.0245 0.049 Uiso 1 1 calc R . . C5 C 1.1683(3) -0.3327(3) -0.0093(3) 0.0347(15) Uani 1 1 d . . . C6 C 1.2480(3) -0.3694(3) -0.0596(3) 0.0362(15) Uani 1 1 d . . . C7 C 1.2253(3) -0.4186(3) -0.0778(3) 0.0422(16) Uani 1 1 d . . . H7A H 1.1872 -0.4250 -0.0718 0.051 Uiso 1 1 calc R . . C8 C 1.2564(3) -0.4582(3) -0.1042(4) 0.051(2) Uani 1 1 d . . . H8A H 1.2403 -0.4913 -0.1170 0.061 Uiso 1 1 calc R . . C9 C 1.3109(4) -0.4479(4) -0.1111(4) 0.055(2) Uani 1 1 d . . . H9A H 1.3340 -0.4750 -0.1273 0.066 Uiso 1 1 calc R . . C10 C 1.3334(3) -0.3983(3) -0.0947(3) 0.0411(16) Uani 1 1 d . . . H10A H 1.3709 -0.3908 -0.1031 0.049 Uiso 1 1 calc R . . C11 C 1.1453(3) -0.1508(3) 0.0694(3) 0.0442(17) Uani 1 1 d . . . H11A H 1.1145 -0.1369 0.0492 0.053 Uiso 1 1 calc R . . C12 C 1.1567(4) -0.1301(3) 0.1232(4) 0.053(2) Uani 1 1 d . . . H12A H 1.1341 -0.1027 0.1395 0.064 Uiso 1 1 calc R . . C13 C 1.2006(4) -0.1499(4) 0.1518(3) 0.0521(19) Uani 1 1 d . . . H13A H 1.2099 -0.1354 0.1880 0.062 Uiso 1 1 calc R . . C14 C 1.2329(3) -0.1920(3) 0.1279(3) 0.0464(18) Uani 1 1 d . . . H14A H 1.2630 -0.2070 0.1483 0.056 Uiso 1 1 calc R . . C15 C 1.2194(3) -0.2112(3) 0.0739(3) 0.0367(15) Uani 1 1 d . . . C16 C 1.1050(3) -0.2404(3) -0.1523(4) 0.0463(18) Uani 1 1 d . . . H16A H 1.0729 -0.2298 -0.1319 0.056 Uiso 1 1 calc R . . C17 C 1.0991(4) -0.2574(3) -0.2069(4) 0.0509(19) Uani 1 1 d . . . H17A H 1.0643 -0.2562 -0.2252 0.061 Uiso 1 1 calc R . . C18 C 1.1446(4) -0.2763(3) -0.2346(4) 0.0513(19) Uani 1 1 d . . . H18A H 1.1407 -0.2903 -0.2720 0.062 Uiso 1 1 calc R . . C19 C 1.1953(3) -0.2756(3) -0.2103(3) 0.0408(16) Uani 1 1 d . . . H19A H 1.2265 -0.2893 -0.2299 0.049 Uiso 1 1 calc R . . C20 C 1.2004(3) -0.2538(3) -0.1547(3) 0.0369(15) Uani 1 1 d . . . C21 C 1.0837(3) -0.1798(3) -0.0409(4) 0.0394(14) Uani 1 1 d . . . C22 C 1.0386(3) -0.1620(3) -0.0414(4) 0.0432(15) Uani 1 1 d . . . C23 C 0.9820(3) -0.1455(3) -0.0437(4) 0.0441(16) Uani 1 1 d . . . C24 C 0.9540(7) -0.1389(11) -0.0911(7) 0.171(11) Uani 1 1 d . . . H24A H 0.9726 -0.1383 -0.1267 0.205 Uiso 1 1 calc R . . C25 C 0.8931(6) -0.1325(7) -0.0889(6) 0.107(5) Uani 1 1 d . . . H25A H 0.8717 -0.1382 -0.1222 0.129 Uiso 1 1 calc R . . C26 C 0.8699(4) -0.1193(4) -0.0429(6) 0.077(3) Uani 1 1 d . . . C27 C 0.8991(4) -0.1213(5) 0.0093(6) 0.073(3) Uani 1 1 d . . . H27A H 0.8817 -0.1128 0.0443 0.088 Uiso 1 1 calc R . . C28 C 0.9537(4) -0.1362(4) 0.0070(5) 0.074(3) Uani 1 1 d . . . H28A H 0.9731 -0.1403 0.0418 0.089 Uiso 1 1 calc R . . C29 C 0.7838(6) -0.1105(6) -0.0830(8) 0.126(7) Uani 1 1 d . . . H29A H 0.7469 -0.0973 -0.0733 0.189 Uiso 1 1 calc R . . H29B H 0.7819 -0.1491 -0.0933 0.189 Uiso 1 1 calc R . . H29C H 0.7982 -0.0895 -0.1152 0.189 Uiso 1 1 calc R . . B1 B 0.5000 0.0000 0.0800(10) 0.078(5) Uani 1 2 d S . . F1 F 0.5472(3) 0.0041(4) 0.1089(4) 0.121(3) Uani 1 1 d . . . F2 F 0.4969(4) 0.0437(4) 0.0436(6) 0.163(5) Uani 1 1 d . . . C30 C 0.6205(7) -0.0345(7) -0.0202(8) 0.137(8) Uani 1 1 d . . . H30A H 0.5958 -0.0642 -0.0076 0.164 Uiso 1 1 calc R . . H30B H 0.5993 -0.0002 -0.0165 0.164 Uiso 1 1 calc R . . Cl1 Cl 0.63052(11) -0.04314(14) -0.08426(15) 0.0860(9) Uani 1 1 d . . . Cl2 Cl 0.6746(2) -0.03102(16) 0.03013(18) 0.1143(14) Uani 1 1 d . . . C31 C 0.6492(8) 0.0294(7) 0.1975(7) 0.115(5) Uani 1 1 d . . . H31A H 0.6479 -0.0108 0.1997 0.138 Uiso 1 1 calc R . . H31B H 0.6157 0.0421 0.1774 0.138 Uiso 1 1 calc R . . Cl3 Cl 0.7047(3) 0.0488(2) 0.1619(3) 0.158(2) Uani 1 1 d . . . Cl4 Cl 0.6510(6) 0.0569(3) 0.2657(4) 0.252(5) Uani 1 1 d . . . O2 O 1.0368(5) -0.0400(7) -0.1542(11) 0.221(11) Uani 1 1 d . . . H2 H 1.0468 -0.0060 -0.1574 0.332 Uiso 1 1 d . . . H2' H 1.0508 -0.0408 -0.1236 0.332 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0316(3) 0.0286(3) 0.0374(3) -0.0003(2) 0.0008(2) 0.00162(19) Ru2 0.0312(3) 0.0259(3) 0.0340(3) 0.000 0.000 0.0011(2) N1 0.035(3) 0.036(3) 0.037(3) -0.002(2) 0.000(2) 0.000(2) N2 0.037(3) 0.029(2) 0.039(3) 0.002(3) -0.002(3) -0.002(2) N3 0.040(3) 0.030(3) 0.042(3) 0.005(2) -0.007(2) 0.006(2) N4 0.036(3) 0.029(3) 0.037(3) -0.005(2) 0.010(2) -0.002(2) N5 0.026(4) 0.042(5) 0.030(4) 0.000 0.000 0.003(3) N6 0.036(3) 0.031(3) 0.043(3) 0.004(2) -0.003(2) -0.004(2) N7 0.044(5) 0.033(4) 0.033(4) 0.000 0.000 -0.005(4) O1 0.064(4) 0.110(7) 0.216(11) -0.082(8) -0.046(7) 0.037(4) C1 0.039(4) 0.043(4) 0.049(4) -0.008(3) 0.002(3) -0.012(3) C2 0.044(4) 0.052(4) 0.048(4) -0.004(3) 0.011(3) -0.011(4) C3 0.048(4) 0.043(4) 0.046(4) 0.004(3) -0.004(3) -0.013(4) C4 0.048(4) 0.031(4) 0.045(4) 0.004(3) -0.008(3) -0.009(3) C5 0.034(3) 0.033(3) 0.037(4) -0.005(3) -0.011(3) -0.004(3) C6 0.041(4) 0.031(3) 0.036(3) 0.002(3) -0.006(3) 0.001(3) C7 0.044(4) 0.033(4) 0.050(4) -0.007(3) -0.013(3) 0.002(3) C8 0.051(5) 0.025(4) 0.077(6) -0.014(3) -0.015(4) 0.012(3) C9 0.058(5) 0.045(4) 0.061(5) -0.016(4) -0.006(4) 0.010(4) C10 0.041(4) 0.037(4) 0.046(4) -0.001(3) -0.008(3) 0.006(3) C11 0.046(4) 0.034(4) 0.052(4) -0.001(3) 0.013(3) 0.001(3) C12 0.058(5) 0.047(5) 0.053(5) -0.013(4) 0.020(4) -0.001(4) C13 0.052(5) 0.067(5) 0.037(4) -0.013(4) 0.010(3) -0.012(4) C14 0.036(4) 0.061(5) 0.042(4) -0.014(3) 0.001(3) -0.011(3) C15 0.037(4) 0.038(4) 0.035(4) 0.000(3) 0.004(3) -0.002(3) C16 0.041(4) 0.044(4) 0.054(4) 0.001(3) -0.012(3) 0.001(3) C17 0.048(4) 0.056(5) 0.049(5) -0.014(4) -0.014(4) 0.000(4) C18 0.062(5) 0.052(5) 0.040(4) -0.005(3) -0.006(4) -0.012(4) C19 0.053(4) 0.031(3) 0.038(4) -0.006(3) -0.003(3) -0.001(3) C20 0.042(4) 0.028(3) 0.040(4) 0.001(3) -0.003(3) 0.000(3) C21 0.039(3) 0.043(3) 0.036(3) -0.001(4) -0.001(4) 0.002(3) C22 0.046(4) 0.033(3) 0.050(4) -0.008(4) -0.004(4) 0.002(3) C23 0.038(3) 0.038(3) 0.057(4) -0.008(4) -0.010(4) 0.006(3) C24 0.112(12) 0.33(3) 0.074(9) -0.041(13) -0.030(8) 0.135(17) C25 0.092(9) 0.142(13) 0.087(9) -0.030(9) -0.035(8) 0.048(9) C26 0.046(5) 0.081(6) 0.105(8) -0.033(7) -0.007(6) -0.002(4) C27 0.053(6) 0.080(7) 0.087(8) -0.007(6) 0.014(5) -0.005(5) C28 0.051(5) 0.082(7) 0.090(8) 0.039(6) -0.004(5) 0.017(5) C29 0.080(8) 0.103(10) 0.196(18) -0.031(10) -0.080(11) 0.025(8) B1 0.066(11) 0.064(11) 0.104(14) 0.000 0.000 -0.014(8) F1 0.087(5) 0.147(7) 0.129(7) 0.052(6) -0.037(4) -0.061(5) F2 0.092(6) 0.116(7) 0.281(14) 0.080(8) -0.086(8) -0.046(5) C30 0.127(13) 0.129(12) 0.155(16) 0.074(11) -0.076(12) -0.076(10) Cl1 0.0548(15) 0.112(2) 0.091(2) -0.0183(17) -0.0011(13) 0.0014(14) Cl2 0.149(4) 0.090(2) 0.104(3) 0.0176(19) -0.031(3) -0.014(2) C31 0.131(12) 0.108(11) 0.105(11) -0.008(9) -0.008(9) -0.038(9) Cl3 0.160(5) 0.144(4) 0.171(5) 0.065(3) -0.058(4) -0.068(4) Cl4 0.432(17) 0.181(6) 0.143(5) -0.027(5) -0.009(7) -0.064(8) O2 0.084(8) 0.187(13) 0.39(3) 0.152(16) -0.047(12) 0.014(8) _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 C21 2.038(6) . ? Ru1 N6 2.097(6) . ? Ru1 N4 2.107(6) . ? Ru1 N3 2.108(6) 14_745 ? Ru1 N1 2.131(6) . ? Ru1 Ru2 2.3572(5) . ? Ru2 N5 1.996(8) . ? Ru2 N2 2.026(5) . ? Ru2 N2 2.026(5) 14_745 ? Ru2 N7 2.042(8) . ? Ru2 Ru1 2.3572(5) 14_745 ? N1 C5 1.344(9) . ? N1 C1 1.357(9) . ? N2 C5 1.386(9) . ? N2 C6 1.391(9) . ? N3 C10 1.346(9) . ? N3 C6 1.369(9) . ? N3 Ru1 2.108(6) 14_745 ? N4 C11 1.337(9) . ? N4 C15 1.370(9) . ? N5 C15 1.387(8) . ? N5 C15 1.387(8) 14_745 ? N6 C16 1.367(10) . ? N6 C20 1.371(10) . ? N7 C20 1.378(8) . ? N7 C20 1.378(8) 14_745 ? O1 C29 1.278(17) . ? O1 C26 1.369(12) . ? C1 C2 1.350(12) . ? C2 C3 1.377(12) . ? C3 C4 1.388(11) . ? C4 C5 1.414(10) . ? C6 C7 1.397(10) . ? C7 C8 1.380(11) . ? C8 C9 1.360(13) . ? C9 C10 1.390(12) . ? C11 C12 1.393(12) . ? C12 C13 1.352(14) . ? C13 C14 1.414(12) . ? C14 C15 1.394(10) . ? C16 C17 1.358(12) . ? C17 C18 1.365(13) . ? C18 C19 1.360(12) . ? C19 C20 1.419(10) . ? C21 C22 1.180(9) . ? C22 C23 1.436(10) . ? C23 C24 1.317(17) . ? C23 C28 1.396(15) . ? C24 C25 1.49(2) . ? C25 C26 1.263(18) . ? C26 C27 1.418(18) . ? C27 C28 1.376(15) . ? B1 F1 1.337(13) 2_655 ? B1 F1 1.337(13) . ? B1 F2 1.375(16) . ? B1 F2 1.375(16) 2_655 ? C30 Cl1 1.54(2) . ? C30 Cl2 1.772(14) . ? C31 Cl3 1.658(18) . ? C31 Cl4 1.741(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Ru1 N6 92.4(3) . . ? C21 Ru1 N4 93.6(3) . . ? N6 Ru1 N4 173.8(2) . . ? C21 Ru1 N3 92.3(3) . 14_745 ? N6 Ru1 N3 89.2(2) . 14_745 ? N4 Ru1 N3 89.0(2) . 14_745 ? C21 Ru1 N1 94.3(3) . . ? N6 Ru1 N1 92.3(2) . . ? N4 Ru1 N1 88.7(2) . . ? N3 Ru1 N1 173.1(2) 14_745 . ? C21 Ru1 Ru2 179.2(2) . . ? N6 Ru1 Ru2 87.35(16) . . ? N4 Ru1 Ru2 86.65(16) . . ? N3 Ru1 Ru2 86.92(16) 14_745 . ? N1 Ru1 Ru2 86.47(16) . . ? N5 Ru2 N2 88.4(2) . . ? N5 Ru2 N2 88.4(2) . 14_745 ? N2 Ru2 N2 176.8(4) . 14_745 ? N5 Ru2 N7 180.000(1) . . ? N2 Ru2 N7 91.6(2) . . ? N2 Ru2 N7 91.6(2) 14_745 . ? N5 Ru2 Ru1 90.12(2) . . ? N2 Ru2 Ru1 90.15(14) . . ? N2 Ru2 Ru1 89.86(14) 14_745 . ? N7 Ru2 Ru1 89.88(2) . . ? N5 Ru2 Ru1 90.12(2) . 14_745 ? N2 Ru2 Ru1 89.86(14) . 14_745 ? N2 Ru2 Ru1 90.15(14) 14_745 14_745 ? N7 Ru2 Ru1 89.88(2) . 14_745 ? Ru1 Ru2 Ru1 179.75(4) . 14_745 ? C5 N1 C1 118.9(6) . . ? C5 N1 Ru1 120.2(5) . . ? C1 N1 Ru1 120.4(5) . . ? C5 N2 C6 123.2(5) . . ? C5 N2 Ru2 117.2(4) . . ? C6 N2 Ru2 119.4(4) . . ? C10 N3 C6 119.4(6) . . ? C10 N3 Ru1 120.4(5) . 14_745 ? C6 N3 Ru1 120.2(5) . 14_745 ? C11 N4 C15 119.2(6) . . ? C11 N4 Ru1 120.4(5) . . ? C15 N4 Ru1 120.3(4) . . ? C15 N5 C15 121.4(8) . 14_745 ? C15 N5 Ru2 119.3(4) . . ? C15 N5 Ru2 119.3(4) 14_745 . ? C16 N6 C20 117.7(6) . . ? C16 N6 Ru1 121.5(5) . . ? C20 N6 Ru1 120.8(5) . . ? C20 N7 C20 122.8(9) . 14_745 ? C20 N7 Ru2 118.6(4) . . ? C20 N7 Ru2 118.6(4) 14_745 . ? C29 O1 C26 121.1(14) . . ? C2 C1 N1 122.4(7) . . ? C1 C2 C3 120.1(7) . . ? C2 C3 C4 119.0(7) . . ? C3 C4 C5 118.4(7) . . ? N1 C5 N2 116.9(6) . . ? N1 C5 C4 121.0(7) . . ? N2 C5 C4 122.0(6) . . ? N3 C6 N2 116.4(6) . . ? N3 C6 C7 118.8(6) . . ? N2 C6 C7 124.6(6) . . ? C8 C7 C6 122.1(8) . . ? C9 C8 C7 117.2(7) . . ? C8 C9 C10 120.9(7) . . ? N3 C10 C9 121.4(7) . . ? N4 C11 C12 123.0(8) . . ? C13 C12 C11 118.5(8) . . ? C12 C13 C14 120.3(8) . . ? C15 C14 C13 118.6(8) . . ? N4 C15 N5 115.9(6) . . ? N4 C15 C14 120.5(7) . . ? N5 C15 C14 123.5(7) . . ? C17 C16 N6 123.4(8) . . ? C16 C17 C18 118.1(8) . . ? C19 C18 C17 121.9(8) . . ? C18 C19 C20 118.1(7) . . ? N6 C20 N7 116.6(6) . . ? N6 C20 C19 120.4(7) . . ? N7 C20 C19 122.9(7) . . ? C22 C21 Ru1 178.3(6) . . ? C21 C22 C23 174.4(7) . . ? C24 C23 C28 116.7(9) . . ? C24 C23 C22 124.1(10) . . ? C28 C23 C22 119.2(8) . . ? C23 C24 C25 119.8(14) . . ? C26 C25 C24 120.0(12) . . ? C25 C26 O1 122.5(13) . . ? C25 C26 C27 120.6(9) . . ? O1 C26 C27 116.8(12) . . ? C28 C27 C26 117.3(11) . . ? C27 C28 C23 123.5(11) . . ? F1 B1 F1 118.9(19) 2_655 . ? F1 B1 F2 109.1(8) 2_655 . ? F1 B1 F2 107.8(5) . . ? F1 B1 F2 107.8(5) 2_655 2_655 ? F1 B1 F2 109.1(8) . 2_655 ? F2 B1 F2 103(2) . 2_655 ? Cl1 C30 Cl2 122.8(13) . . ? Cl3 C31 Cl4 109.4(10) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.310 _refine_diff_density_min -1.111 _refine_diff_density_rms 0.262 #===END data_ic11436 #(compound 4) _database_code_depnum_ccdc_archive 'CCDC 270952' _chemical_name_common (Ru3(CCPhC5H11)2)(BF4) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H70 B Cl8 F4 N12 Ru3' _chemical_formula_weight 1753.00 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' 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 Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 23.6843(5) _cell_length_b 25.8795(5) _cell_length_c 23.3208(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14294.2(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.500 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7064 _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.826 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29798 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7484 _reflns_number_gt 6294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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^)+(0.0885P)^2^+19.2377P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_number_reflns 7484 _refine_ls_number_parameters 484 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.007 _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 -0.092788(15) -0.467616(14) 0.770653(15) 0.03505(12) Uani 1 1 d . . . Ru2 Ru 0.0000 -0.5000 0.77043(3) 0.03286(13) Uani 1 2 d S . . N1 N -0.11777(18) -0.54156(17) 0.73993(19) 0.0371(9) Uani 1 1 d . . . N2 N -0.02974(16) -0.57382(14) 0.7679(2) 0.0348(8) Uani 1 1 d . . . N3 N 0.05810(18) -0.60214(16) 0.79895(18) 0.0365(9) Uani 1 1 d . . . N4 N -0.09852(19) -0.49269(17) 0.85608(19) 0.0381(10) Uani 1 1 d . . . N5 N 0.0000 -0.5000 0.8578(3) 0.0383(15) Uani 1 2 d S . . N6 N -0.07697(19) -0.44391(17) 0.68594(18) 0.0370(10) Uani 1 1 d . . . N7 N 0.0000 -0.5000 0.6844(3) 0.0327(13) Uani 1 2 d S . . C1 C -0.1688(2) -0.5484(2) 0.7140(2) 0.0418(12) Uani 1 1 d . . . H1A H -0.1955 -0.5210 0.7152 0.050 Uiso 1 1 calc R . . C2 C -0.1832(3) -0.5926(3) 0.6865(3) 0.0523(15) Uani 1 1 d . . . H2A H -0.2196 -0.5962 0.6701 0.063 Uiso 1 1 calc R . . C3 C -0.1443(3) -0.6326(3) 0.6824(3) 0.0499(15) Uani 1 1 d . . . H3A H -0.1530 -0.6631 0.6617 0.060 Uiso 1 1 calc R . . C4 C -0.0931(2) -0.6269(2) 0.7091(2) 0.0455(13) Uani 1 1 d . . . H4A H -0.0657 -0.6536 0.7068 0.055 Uiso 1 1 calc R . . C5 C -0.0812(2) -0.5815(2) 0.7398(2) 0.0369(11) Uani 1 1 d . . . C6 C 0.0014(2) -0.6144(2) 0.7909(2) 0.0407(12) Uani 1 1 d . . . C7 C -0.0198(2) -0.6607(2) 0.8095(3) 0.0468(13) Uani 1 1 d . . . H7A H -0.0584 -0.6685 0.8032 0.056 Uiso 1 1 calc R . . C8 C 0.0144(3) -0.6964(2) 0.8375(3) 0.0519(15) Uani 1 1 d . . . H8A H -0.0005 -0.7287 0.8497 0.062 Uiso 1 1 calc R . . C9 C 0.0688(3) -0.6844(2) 0.8469(3) 0.0507(14) Uani 1 1 d . . . H9A H 0.0926 -0.7080 0.8665 0.061 Uiso 1 1 calc R . . C10 C 0.0902(2) -0.6379(2) 0.8282(2) 0.0432(13) Uani 1 1 d . . . H10A H 0.1287 -0.6302 0.8357 0.052 Uiso 1 1 calc R . . C11 C -0.1493(2) -0.4995(2) 0.8817(2) 0.0426(12) Uani 1 1 d . . . H11A H -0.1824 -0.4910 0.8608 0.051 Uiso 1 1 calc R . . C12 C -0.1553(3) -0.5182(3) 0.9364(3) 0.0505(14) Uani 1 1 d . . . H12A H -0.1916 -0.5214 0.9534 0.061 Uiso 1 1 calc R . . C13 C -0.1072(3) -0.5322(3) 0.9662(3) 0.0537(15) Uani 1 1 d . . . H13A H -0.1102 -0.5455 1.0041 0.064 Uiso 1 1 calc R . . C14 C -0.0564(3) -0.5271(2) 0.9414(3) 0.0500(14) Uani 1 1 d . . . H14A H -0.0236 -0.5380 0.9616 0.060 Uiso 1 1 calc R . . C15 C -0.0506(2) -0.5058(2) 0.8859(2) 0.0374(11) Uani 1 1 d . . . C16 C -0.1073(3) -0.4051(2) 0.6615(3) 0.0484(14) Uani 1 1 d . . . H16A H -0.1388 -0.3916 0.6818 0.058 Uiso 1 1 calc R . . C17 C -0.0943(3) -0.3845(2) 0.6086(3) 0.0525(16) Uani 1 1 d . . . H17A H -0.1164 -0.3572 0.5932 0.063 Uiso 1 1 calc R . . C18 C -0.0492(3) -0.4037(3) 0.5783(3) 0.0538(15) Uani 1 1 d . . . H18A H -0.0397 -0.3898 0.5418 0.065 Uiso 1 1 calc R . . C19 C -0.0180(3) -0.4431(2) 0.6012(2) 0.0476(13) Uani 1 1 d . . . H19A H 0.0132 -0.4567 0.5806 0.057 Uiso 1 1 calc R . . C20 C -0.0319(2) -0.4638(2) 0.6557(2) 0.0399(12) Uani 1 1 d . . . C21 C -0.1719(2) -0.43864(19) 0.7710(3) 0.0407(10) Uani 1 1 d . . . C22 C -0.2194(2) -0.4222(2) 0.7709(3) 0.0538(13) Uani 1 1 d . . . C23 C -0.2760(2) -0.4044(3) 0.7741(4) 0.0659(18) Uani 1 1 d . . . C24 C -0.3012(2) -0.3782(2) 0.7289(3) 0.0482(14) Uani 1 1 d . C . H24A H -0.2795 -0.3716 0.6955 0.058 Uiso 0.50 1 calc PR A 1 H24B H -0.2795 -0.3714 0.6955 0.058 Uiso 0.50 1 d PR A 2 C25 C -0.3564(3) -0.3614(3) 0.7306(3) 0.0643(19) Uani 1 1 d . . . H25A H -0.3691 -0.3363 0.7039 0.077 Uiso 0.50 1 calc PR B 1 H25B H -0.3755 -0.3505 0.6969 0.077 Uiso 0.50 1 d PR B 2 C26 C -0.3942(9) -0.3813(7) 0.7721(11) 0.056(5) Uani 0.50 1 d P C 1 C27 C -0.3708(10) -0.4091(11) 0.8140(14) 0.093(9) Uani 0.50 1 d P C 1 H27A H -0.3952 -0.4208 0.8435 0.112 Uiso 0.50 1 calc PR C 1 C28 C -0.3146(11) -0.4225(9) 0.8186(14) 0.083(9) Uani 0.50 1 d P C 1 H28A H -0.3015 -0.4429 0.8497 0.100 Uiso 0.50 1 calc PR C 1 C29 C -0.4537(5) -0.3635(4) 0.7751(7) 0.052(3) Uiso 0.50 1 d PD C 1 H29A H -0.4587 -0.3317 0.7519 0.063 Uiso 0.50 1 calc PR C 1 H29B H -0.4642 -0.3558 0.8152 0.063 Uiso 0.50 1 calc PR C 1 C30 C -0.4905(9) -0.4071(7) 0.7513(8) 0.077(5) Uiso 0.50 1 d PD C 1 H30A H -0.5280 -0.4073 0.7700 0.093 Uiso 0.50 1 calc PR C 1 H30B H -0.4723 -0.4411 0.7576 0.093 Uiso 0.50 1 calc PR C 1 C31 C -0.4961(14) -0.3957(10) 0.6866(7) 0.143(10) Uiso 0.50 1 d PD C 1 H31A H -0.4672 -0.3690 0.6789 0.171 Uiso 0.50 1 calc PR C 1 H31B H -0.5329 -0.3780 0.6829 0.171 Uiso 0.50 1 calc PR C 1 C32 C -0.4933(16) -0.4318(10) 0.6338(12) 0.147(11) Uiso 0.50 1 d PD C 1 H32A H -0.5249 -0.4152 0.6130 0.177 Uiso 0.50 1 calc PR C 1 H32B H -0.4595 -0.4155 0.6168 0.177 Uiso 0.50 1 calc PR C 1 C33 C -0.4915(17) -0.4804(10) 0.5959(13) 0.158(12) Uiso 0.50 1 d PD . 1 H33A H -0.4786 -0.4735 0.5586 0.237 Uiso 0.50 1 d P D 1 H33B H -0.4715 -0.5083 0.6131 0.237 Uiso 0.50 1 d P E 1 H33C H -0.5320 -0.4925 0.5922 0.237 Uiso 0.50 1 d P F 1 C26' C -0.3864(10) -0.3614(8) 0.7850(11) 0.064(6) Uani 0.50 1 d P C 2 C27' C -0.3583(12) -0.3823(13) 0.8337(12) 0.106(11) Uani 0.50 1 d P C 2 H27B H -0.3783 -0.3875 0.8686 0.127 Uiso 0.50 1 calc PR C 2 C28' C -0.2998(12) -0.3957(12) 0.8297(14) 0.094(10) Uani 0.50 1 d P C 2 H28B H -0.2773 -0.3987 0.8632 0.113 Uiso 0.50 1 calc PR C 2 C29' C -0.4447(6) -0.3403(6) 0.7942(7) 0.064(4) Uiso 0.50 1 d PD C 2 H29C H -0.4545 -0.3153 0.7636 0.076 Uiso 0.50 1 calc PR C 2 H29D H -0.4473 -0.3226 0.8317 0.076 Uiso 0.50 1 calc PR C 2 C30' C -0.4847(9) -0.3866(7) 0.7925(10) 0.114(7) Uiso 0.50 1 d PD C 2 H30C H -0.5236 -0.3733 0.7976 0.137 Uiso 0.50 1 calc PR C 2 H30D H -0.4761 -0.4085 0.8261 0.137 Uiso 0.50 1 calc PR C 2 C31' C -0.4848(15) -0.4219(11) 0.7389(9) 0.132(12) Uiso 0.50 1 d PD C 2 H31C H -0.4632 -0.4518 0.7538 0.158 Uiso 0.50 1 calc PR C 2 H31D H -0.5246 -0.4337 0.7393 0.158 Uiso 0.50 1 calc PR C 2 C32' C -0.4718(11) -0.4267(10) 0.6746(9) 0.121(7) Uiso 0.50 1 d PD C 2 H32C H -0.4764 -0.3931 0.6548 0.145 Uiso 0.50 1 calc PR C 2 H32D H -0.4329 -0.4395 0.6683 0.145 Uiso 0.50 1 calc PR C 2 C33' C -0.5155(12) -0.4661(11) 0.6535(14) 0.144(10) Uiso 0.50 1 d PD . 2 H33D H -0.5048 -0.4713 0.6112 0.216 Uiso 0.50 1 d P G 2 H33E H -0.5000 -0.5000 0.6698 0.216 Uiso 1 2 d S H 2 H33F H -0.5492 -0.4614 0.6598 0.216 Uiso 0.50 1 d P I 2 B1 B -0.5000 -0.5000 0.9105(7) 0.072(3) Uani 1 2 d S . . F1 F -0.5481(6) -0.4947(5) 0.8814(8) 0.053(3) Uani 0.50 1 d P . . F2 F -0.4553(11) -0.5106(12) 0.8659(13) 0.150(13) Uani 0.50 1 d P . . F3 F -0.4842(6) -0.4460(5) 0.9249(8) 0.110(4) Uani 0.50 1 d P . . F4 F -0.4946(5) -0.5283(6) 0.9549(5) 0.092(4) Uani 0.50 1 d P . . C34 C -0.6214(4) -0.5254(5) 0.9955(4) 0.099(3) Uani 1 1 d . . . H34A H -0.6014 -0.5563 0.9808 0.119 Uiso 1 1 calc R . . H34B H -0.5957 -0.4955 0.9916 0.119 Uiso 1 1 calc R . . Cl1 Cl -0.68155(10) -0.51466(8) 0.95411(9) 0.0782(6) Uani 1 1 d . . . Cl2 Cl -0.63723(10) -0.53457(11) 1.06772(11) 0.0939(7) Uani 1 1 d . . . C35 C -0.6453(5) -0.4679(6) 0.7795(6) 0.133(4) Uani 1 1 d . . . H35A H -0.6431 -0.5059 0.7834 0.160 Uiso 1 1 calc R . . H35B H -0.6097 -0.4528 0.7943 0.160 Uiso 1 1 calc R . . Cl3 Cl -0.70146(18) -0.44473(19) 0.81814(18) 0.1562(15) Uani 1 1 d . . . Cl4 Cl -0.6544(2) -0.4508(2) 0.7061(2) 0.190(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 0.02780(18) 0.0469(2) 0.0305(2) 0.00093(19) -0.00217(18) 0.00362(15) Ru2 0.0278(2) 0.0445(3) 0.0263(3) 0.000 0.000 0.0034(2) N1 0.031(2) 0.051(2) 0.029(2) 0.0025(18) -0.0026(18) 0.0006(19) N2 0.0317(18) 0.0396(18) 0.033(2) 0.002(2) 0.004(2) 0.0015(15) N3 0.032(2) 0.044(2) 0.034(2) -0.0015(18) 0.0057(18) 0.0047(18) N4 0.034(2) 0.048(2) 0.032(2) -0.0013(19) 0.0016(18) 0.0045(18) N5 0.036(4) 0.057(4) 0.022(3) 0.000 0.000 0.007(3) N6 0.036(2) 0.049(2) 0.025(2) 0.0020(18) -0.0098(17) -0.0020(19) N7 0.034(3) 0.042(3) 0.022(3) 0.000 0.000 -0.001(3) C1 0.033(3) 0.051(3) 0.041(3) 0.003(2) -0.003(2) -0.005(2) C2 0.046(3) 0.072(4) 0.039(3) 0.007(3) -0.004(3) -0.010(3) C3 0.056(4) 0.056(3) 0.038(3) 0.005(3) -0.006(3) -0.016(3) C4 0.040(3) 0.057(3) 0.040(3) 0.005(3) 0.003(2) -0.002(2) C5 0.038(3) 0.048(3) 0.025(3) 0.003(2) 0.002(2) -0.003(2) C6 0.040(3) 0.052(3) 0.030(3) -0.001(2) 0.006(2) 0.007(2) C7 0.035(3) 0.058(3) 0.048(3) 0.002(3) 0.007(2) 0.000(2) C8 0.056(4) 0.051(3) 0.049(4) 0.011(3) 0.016(3) 0.010(3) C9 0.046(3) 0.063(3) 0.043(3) 0.015(3) 0.005(3) 0.019(3) C10 0.042(3) 0.053(3) 0.034(3) -0.001(2) 0.004(2) 0.012(2) C11 0.031(3) 0.056(3) 0.040(3) -0.005(2) 0.007(2) 0.002(2) C12 0.042(3) 0.063(3) 0.047(4) 0.001(3) 0.010(3) -0.006(3) C13 0.050(4) 0.072(4) 0.039(3) 0.007(3) 0.005(3) -0.004(3) C14 0.051(3) 0.065(3) 0.034(3) 0.011(3) 0.002(3) 0.007(3) C15 0.036(3) 0.046(3) 0.030(3) 0.000(2) 0.002(2) 0.007(2) C16 0.045(3) 0.052(3) 0.048(3) -0.004(3) -0.012(3) 0.002(3) C17 0.058(4) 0.058(3) 0.041(4) 0.012(3) -0.020(3) -0.003(3) C18 0.056(4) 0.068(4) 0.037(3) 0.016(3) -0.011(3) -0.013(3) C19 0.049(3) 0.062(3) 0.033(3) 0.004(2) -0.001(2) -0.009(3) C20 0.038(3) 0.057(3) 0.025(3) -0.001(2) 0.001(2) -0.005(2) C21 0.039(2) 0.045(2) 0.038(3) -0.001(3) -0.003(3) 0.006(2) C22 0.038(3) 0.081(4) 0.043(3) 0.011(4) 0.007(3) 0.009(3) C23 0.039(3) 0.104(5) 0.054(4) 0.021(4) 0.016(4) 0.026(3) C24 0.035(3) 0.063(3) 0.047(4) 0.006(3) 0.007(3) 0.005(3) C25 0.042(3) 0.082(5) 0.069(5) 0.024(4) 0.000(3) 0.014(3) C26 0.042(8) 0.047(9) 0.079(12) -0.002(10) -0.004(9) 0.014(8) C27 0.030(8) 0.12(2) 0.13(3) 0.040(16) 0.042(12) 0.006(11) C28 0.048(13) 0.097(16) 0.104(18) 0.065(16) 0.029(12) 0.038(11) C26' 0.049(10) 0.062(12) 0.082(16) 0.006(10) 0.032(10) 0.008(9) C27' 0.079(19) 0.17(3) 0.072(17) 0.041(17) 0.046(14) 0.059(19) C28' 0.056(15) 0.15(2) 0.079(15) 0.07(2) 0.018(11) 0.050(16) B1 0.043(6) 0.079(8) 0.092(10) 0.000 0.000 0.019(6) F1 0.036(5) 0.063(5) 0.059(7) -0.015(4) -0.007(4) 0.005(4) F2 0.117(18) 0.23(2) 0.11(2) 0.018(13) 0.052(13) 0.069(15) F3 0.073(8) 0.095(8) 0.162(14) -0.034(8) -0.033(8) 0.022(6) F4 0.059(6) 0.148(11) 0.070(7) 0.038(6) 0.003(5) 0.014(7) C34 0.063(5) 0.154(9) 0.080(6) 0.011(6) 0.001(4) 0.006(6) Cl1 0.0939(15) 0.0746(10) 0.0660(12) 0.0007(9) -0.0200(11) -0.0113(11) Cl2 0.0659(12) 0.147(2) 0.0687(13) 0.0245(13) -0.0065(11) -0.0068(13) C35 0.098(8) 0.172(11) 0.129(11) 0.006(9) 0.006(9) 0.011(8) Cl3 0.134(3) 0.212(4) 0.123(3) -0.036(3) -0.031(2) 0.062(3) Cl4 0.160(4) 0.273(6) 0.136(4) -0.004(4) 0.003(3) 0.003(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 C21 2.019(5) . ? Ru1 N3 2.090(4) 2_545 ? Ru1 N4 2.100(4) . ? Ru1 N6 2.102(4) . ? Ru1 N1 2.127(4) . ? Ru1 Ru2 2.3520(4) . ? Ru2 N7 2.006(6) . ? Ru2 N2 2.037(4) 2_545 ? Ru2 N2 2.037(4) . ? Ru2 N5 2.038(6) . ? Ru2 Ru1 2.3520(4) 2_545 ? N1 C5 1.348(7) . ? N1 C1 1.364(7) . ? N2 C6 1.392(7) . ? N2 C5 1.398(7) . ? N3 C10 1.379(7) . ? N3 C6 1.392(7) . ? N3 Ru1 2.090(4) 2_545 ? N4 C11 1.354(7) . ? N4 C15 1.373(7) . ? N5 C15 1.374(6) 2_545 ? N5 C15 1.374(6) . ? N6 C16 1.359(7) . ? N6 C20 1.378(7) . ? N7 C20 1.377(6) . ? N7 C20 1.377(6) 2_545 ? C1 C2 1.353(9) . ? C2 C3 1.387(10) . ? C3 C4 1.372(9) . ? C4 C5 1.405(8) . ? C6 C7 1.368(8) . ? C7 C8 1.391(9) . ? C8 C9 1.345(9) . ? C9 C10 1.376(9) . ? C11 C12 1.372(9) . ? C12 C13 1.381(9) . ? C13 C14 1.343(9) . ? C14 C15 1.415(8) . ? C16 C17 1.379(9) . ? C17 C18 1.375(10) . ? C18 C19 1.368(9) . ? C19 C20 1.418(8) . ? C21 C22 1.202(7) . ? C22 C23 1.420(8) . ? C23 C24 1.387(10) . ? C23 C28' 1.43(3) . ? C23 C28 1.46(3) . ? C24 C25 1.379(9) . ? C25 C26 1.41(3) . ? C25 C26' 1.45(2) . ? C26 C27 1.33(4) . ? C26 C29 1.48(2) . ? C27 C28 1.38(4) . ? C29 C30 1.531(10) . ? C30 C31 1.544(10) . ? C31 C32 1.546(10) . ? C32 C33 1.537(10) . ? C33 C33 1.09(5) 2_445 ? C26' C27' 1.42(4) . ? C26' C29' 1.50(3) . ? C27' C28' 1.43(4) . ? C29' C30' 1.527(10) . ? C30' C31' 1.548(10) . ? C31' C32' 1.536(10) . ? C32' C33' 1.532(10) . ? C33' C33' 1.90(6) 2_445 ? B1 F4 1.275(16) 2_445 ? B1 F4 1.275(16) . ? B1 F1 1.332(17) . ? B1 F1 1.332(17) 2_445 ? B1 F3 1.486(13) . ? B1 F3 1.486(13) 2_445 ? B1 F2 1.51(3) 2_445 ? B1 F2 1.51(3) . ? F1 F2 0.40(4) 2_445 ? F2 F1 0.40(4) 2_445 ? F3 F4 1.089(17) 2_445 ? F4 F3 1.089(17) 2_445 ? F4 F4 1.48(3) 2_445 ? C34 Cl2 1.742(10) . ? C34 Cl1 1.743(10) . ? C35 Cl3 1.714(14) . ? C35 Cl4 1.780(16) . ? 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 C21 Ru1 N3 92.45(19) . 2_545 ? C21 Ru1 N4 92.9(2) . . ? N3 Ru1 N4 89.59(17) 2_545 . ? C21 Ru1 N6 93.5(2) . . ? N3 Ru1 N6 88.55(17) 2_545 . ? N4 Ru1 N6 173.39(18) . . ? C21 Ru1 N1 94.43(19) . . ? N3 Ru1 N1 173.00(17) 2_545 . ? N4 Ru1 N1 91.35(17) . . ? N6 Ru1 N1 89.74(17) . . ? C21 Ru1 Ru2 179.06(15) . . ? N3 Ru1 Ru2 86.63(11) 2_545 . ? N4 Ru1 Ru2 87.27(12) . . ? N6 Ru1 Ru2 86.30(12) . . ? N1 Ru1 Ru2 86.48(12) . . ? N7 Ru2 N2 88.33(15) . 2_545 ? N7 Ru2 N2 88.33(15) . . ? N2 Ru2 N2 176.7(3) 2_545 . ? N7 Ru2 N5 180.000(1) . . ? N2 Ru2 N5 91.67(15) 2_545 . ? N2 Ru2 N5 91.67(15) . . ? N7 Ru2 Ru1 90.124(17) . . ? N2 Ru2 Ru1 89.37(10) 2_545 . ? N2 Ru2 Ru1 90.64(10) . . ? N5 Ru2 Ru1 89.876(17) . . ? N7 Ru2 Ru1 90.124(17) . 2_545 ? N2 Ru2 Ru1 90.64(10) 2_545 2_545 ? N2 Ru2 Ru1 89.37(10) . 2_545 ? N5 Ru2 Ru1 89.876(17) . 2_545 ? Ru1 Ru2 Ru1 179.75(3) . 2_545 ? C5 N1 C1 118.0(5) . . ? C5 N1 Ru1 120.8(3) . . ? C1 N1 Ru1 120.9(4) . . ? C6 N2 C5 122.4(4) . . ? C6 N2 Ru2 120.9(3) . . ? C5 N2 Ru2 116.6(3) . . ? C10 N3 C6 116.4(5) . . ? C10 N3 Ru1 121.3(4) . 2_545 ? C6 N3 Ru1 122.2(3) . 2_545 ? C11 N4 C15 118.6(5) . . ? C11 N4 Ru1 121.1(4) . . ? C15 N4 Ru1 120.2(3) . . ? C15 N5 C15 123.1(6) 2_545 . ? C15 N5 Ru2 118.4(3) 2_545 . ? C15 N5 Ru2 118.4(3) . . ? C16 N6 C20 118.1(5) . . ? C16 N6 Ru1 121.0(4) . . ? C20 N6 Ru1 120.6(3) . . ? C20 N7 C20 121.9(6) . 2_545 ? C20 N7 Ru2 119.1(3) . . ? C20 N7 Ru2 119.1(3) 2_545 . ? C2 C1 N1 122.9(5) . . ? C1 C2 C3 119.7(6) . . ? C4 C3 C2 118.4(6) . . ? C3 C4 C5 119.9(6) . . ? N1 C5 N2 116.8(4) . . ? N1 C5 C4 120.9(5) . . ? N2 C5 C4 122.1(5) . . ? C7 C6 N2 126.1(5) . . ? C7 C6 N3 120.7(5) . . ? N2 C6 N3 113.0(5) . . ? C6 C7 C8 121.2(6) . . ? C9 C8 C7 118.6(6) . . ? C8 C9 C10 120.3(5) . . ? C9 C10 N3 122.7(5) . . ? N4 C11 C12 123.3(5) . . ? C11 C12 C13 118.3(6) . . ? C14 C13 C12 119.8(6) . . ? C13 C14 C15 121.3(6) . . ? N4 C15 N5 116.9(5) . . ? N4 C15 C14 118.7(5) . . ? N5 C15 C14 124.3(5) . . ? N6 C16 C17 122.8(6) . . ? C18 C17 C16 119.7(6) . . ? C19 C18 C17 119.2(6) . . ? C18 C19 C20 120.4(6) . . ? N7 C20 N6 115.5(5) . . ? N7 C20 C19 124.4(5) . . ? N6 C20 C19 119.8(5) . . ? C22 C21 Ru1 178.9(6) . . ? C21 C22 C23 176.4(8) . . ? C24 C23 C22 121.6(7) . . ? C24 C23 C28' 116.2(11) . . ? C22 C23 C28' 118.1(13) . . ? C24 C23 C28 115.3(12) . . ? C22 C23 C28 121.6(11) . . ? C28' C23 C28 33.0(16) . . ? C25 C24 C23 122.7(6) . . ? C24 C25 C26 120.3(9) . . ? C24 C25 C26' 119.3(11) . . ? C26 C25 C26' 25.2(8) . . ? C27 C26 C25 115.7(17) . . ? C27 C26 C29 122(2) . . ? C25 C26 C29 121.3(16) . . ? C26 C27 C28 126(2) . . ? C27 C28 C23 118(2) . . ? C26 C29 C30 107.0(13) . . ? C29 C30 C31 105.2(15) . . ? C30 C31 C32 131(2) . . ? C33 C32 C31 162(3) . . ? C33 C33 C32 139(3) 2_445 . ? C27' C26' C25 117.9(18) . . ? C27' C26' C29' 117.1(18) . . ? C25 C26' C29' 125.1(19) . . ? C26' C27' C28' 119(2) . . ? C23 C28' C27' 119(2) . . ? C26' C29' C30' 106.4(15) . . ? C29' C30' C31' 119(2) . . ? C32' C31' C30' 147(3) . . ? C33' C32' C31' 103(2) . . ? C32' C33' C33' 111(3) . 2_445 ? F4 B1 F4 71.2(16) 2_445 . ? F4 B1 F1 105.6(8) 2_445 . ? F4 B1 F1 123.9(9) . . ? F4 B1 F1 123.9(9) 2_445 2_445 ? F4 B1 F1 105.6(8) . 2_445 ? F1 B1 F1 118.9(18) . 2_445 ? F4 B1 F3 45.6(7) 2_445 . ? F4 B1 F3 109.2(15) . . ? F1 B1 F3 103.5(7) . . ? F1 B1 F3 89.8(9) 2_445 . ? F4 B1 F3 109.2(15) 2_445 2_445 ? F4 B1 F3 45.6(7) . 2_445 ? F1 B1 F3 89.8(9) . 2_445 ? F1 B1 F3 103.5(7) 2_445 2_445 ? F3 B1 F3 153.7(19) . 2_445 ? F4 B1 F2 112.7(13) 2_445 2_445 ? F4 B1 F2 137.3(13) . 2_445 ? F1 B1 F2 14.4(16) . 2_445 ? F1 B1 F2 105.6(14) 2_445 2_445 ? F3 B1 F2 99.3(13) . 2_445 ? F3 B1 F2 98.7(14) 2_445 2_445 ? F4 B1 F2 137.3(13) 2_445 . ? F4 B1 F2 112.7(13) . . ? F1 B1 F2 105.6(14) . . ? F1 B1 F2 14.4(16) 2_445 . ? F3 B1 F2 98.7(14) . . ? F3 B1 F2 99.3(13) 2_445 . ? F2 B1 F2 93(2) 2_445 . ? F2 F1 B1 109(6) 2_445 . ? F1 F2 B1 57(5) 2_445 . ? F4 F3 B1 56.9(10) 2_445 . ? F3 F4 B1 77.5(11) 2_445 . ? F3 F4 F4 121.6(12) 2_445 2_445 ? B1 F4 F4 54.4(8) . 2_445 ? Cl2 C34 Cl1 112.4(6) . . ? Cl3 C35 Cl4 109.0(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.941 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.178 #===END data_ic10772 #(compound 5) _database_code_depnum_ccdc_archive 'CCDC 270953' _chemical_name_common (Ru3(CCPhCN)2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H40 Cl4 N14 Ru3' _chemical_formula_weight 1402.07 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' 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 Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 24.6541(9) _cell_length_b 25.7043(9) _cell_length_c 21.6051(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13691.5(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5584 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.723 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19311 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5427 _reflns_number_gt 3998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.1911P)^2^+31.1184P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(12) _refine_ls_number_reflns 5427 _refine_ls_number_parameters 278 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1156 _refine_ls_R_factor_gt 0.0903 _refine_ls_wR_factor_ref 0.2823 _refine_ls_wR_factor_gt 0.2488 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.08545(4) 0.53877(4) 0.13838(5) 0.0753(4) Uani 1 1 d . . . Ru2 Ru 0.0000 0.5000 0.13822(8) 0.0712(4) Uani 1 2 d S . . N1 N 0.1164(5) 0.4672(4) 0.1740(6) 0.079(3) Uani 1 1 d . . . N2 N 0.0335(4) 0.4292(3) 0.1395(7) 0.077(3) Uani 1 1 d . . . N3 N -0.0466(5) 0.3929(5) 0.1071(6) 0.084(3) Uani 1 1 d . . . N4 N 0.0681(4) 0.5618(4) 0.2296(5) 0.071(3) Uani 1 1 d . . . N5 N 0.0000 0.5000 0.2294(8) 0.077(5) Uani 1 2 d S . . N6 N 0.0929(5) 0.5132(5) 0.0447(6) 0.085(3) Uani 1 1 d . . . N7 N 0.0000 0.5000 0.0433(9) 0.077(5) Uani 1 2 d S . . N8 N 0.4603(7) 0.6809(15) 0.0889(18) 0.252(16) Uiso 1 1 d D . . C1 C 0.1602(6) 0.4641(6) 0.2057(8) 0.089(4) Uani 1 1 d . . . H1A H 0.1824 0.4943 0.2077 0.107 Uiso 1 1 calc R . . C2 C 0.1770(7) 0.4227(7) 0.2355(9) 0.095(5) Uani 1 1 d . . . H2A H 0.2107 0.4232 0.2568 0.114 Uiso 1 1 calc R . . C3 C 0.1467(9) 0.3803(7) 0.2355(9) 0.107(6) Uani 1 1 d . . . H3A H 0.1593 0.3495 0.2551 0.128 Uiso 1 1 calc R . . C4 C 0.0962(6) 0.3810(5) 0.2065(8) 0.082(4) Uani 1 1 d . . . H4A H 0.0723 0.3522 0.2108 0.098 Uiso 1 1 calc R . . C5 C 0.0809(6) 0.4227(5) 0.1721(7) 0.078(3) Uani 1 1 d . . . C6 C 0.0071(6) 0.3868(6) 0.1158(7) 0.079(4) Uani 1 1 d . . . C7 C 0.0323(7) 0.3390(6) 0.0976(8) 0.097(5) Uani 1 1 d . . . H7A H 0.0697 0.3334 0.1060 0.116 Uiso 1 1 calc R . . C8 C 0.0037(7) 0.3027(7) 0.0691(10) 0.105(6) Uani 1 1 d . . . H8A H 0.0204 0.2711 0.0566 0.126 Uiso 1 1 calc R . . C9 C -0.0510(12) 0.3110(7) 0.0577(10) 0.138(9) Uani 1 1 d . . . H9A H -0.0710 0.2842 0.0377 0.166 Uiso 1 1 calc R . . C10 C -0.0785(7) 0.3566(6) 0.0741(8) 0.092(4) Uani 1 1 d . . . H10A H -0.1154 0.3627 0.0640 0.111 Uiso 1 1 calc R . . C11 C 0.0923(6) 0.6060(6) 0.2538(8) 0.088(4) Uani 1 1 d . . . H11A H 0.1205 0.6228 0.2316 0.105 Uiso 1 1 calc R . . C12 C 0.0752(8) 0.6260(7) 0.3111(9) 0.100(5) Uani 1 1 d . . . H12A H 0.0930 0.6556 0.3279 0.120 Uiso 1 1 calc R . . C13 C 0.0356(7) 0.6049(7) 0.3412(7) 0.094(4) Uani 1 1 d . . . H13A H 0.0239 0.6202 0.3789 0.112 Uiso 1 1 calc R . . C14 C 0.0092(6) 0.5596(5) 0.3194(7) 0.083(4) Uani 1 1 d . . . H14A H -0.0188 0.5433 0.3426 0.100 Uiso 1 1 calc R . . C15 C 0.0264(5) 0.5395(5) 0.2615(7) 0.070(3) Uani 1 1 d . . . C16 C 0.1433(8) 0.5094(6) 0.0189(8) 0.097(5) Uani 1 1 d . . . H16A H 0.1748 0.5195 0.0411 0.116 Uiso 1 1 calc R . . C17 C 0.1469(8) 0.4898(7) -0.0418(10) 0.102(5) Uani 1 1 d . . . H17A H 0.1820 0.4870 -0.0596 0.123 Uiso 1 1 calc R . . C18 C 0.1083(9) 0.4761(7) -0.0735(9) 0.107(6) Uani 1 1 d . . . H18A H 0.1138 0.4652 -0.1150 0.129 Uiso 1 1 calc R . . C19 C 0.0509(7) 0.4764(6) -0.0457(8) 0.094(4) Uani 1 1 d . . . H19A H 0.0204 0.4624 -0.0668 0.112 Uiso 1 1 calc R . . C20 C 0.0469(7) 0.4991(6) 0.0131(7) 0.083(4) Uani 1 1 d . . . C21 C 0.1581(5) 0.5702(6) 0.1376(10) 0.092(4) Uani 1 1 d . . . C22 C 0.2021(4) 0.5901(3) 0.1252(4) 0.117(6) Uani 1 1 d . . . C23 C 0.2597(4) 0.6109(3) 0.1136(4) 0.130(7) Uani 1 1 d R . . C24 C 0.3008(4) 0.5929(3) 0.1522(4) 0.200 Uiso 1 1 d R . . H24A H 0.2934 0.5664 0.1817 0.240 Uiso 1 1 calc R . . C25 C 0.3527(4) 0.6136(3) 0.1476(4) 0.200 Uiso 1 1 d R . . H25A H 0.3808 0.6013 0.1739 0.240 Uiso 1 1 calc R . . C26 C 0.3636(4) 0.6524(3) 0.1044(4) 0.200 Uiso 1 1 d RD . . C27 C 0.3225(4) 0.6704(3) 0.0659(4) 0.200 Uiso 1 1 d R . . H27A H 0.3299 0.6969 0.0364 0.240 Uiso 1 1 calc R . . C28 C 0.2706(4) 0.6496(3) 0.0705(4) 0.200 Uiso 1 1 d R . . H28A H 0.2425 0.6619 0.0442 0.240 Uiso 1 1 calc R . . C29 C 0.4156(4) 0.6650(3) 0.0881(4) 0.200 Uiso 1 1 d RD . . C30 C 0.0627(4) 0.2200(3) 0.1655(4) 0.300 Uiso 1 1 d RD . . Cl1 Cl 0.1260(4) 0.2398(3) 0.1428(4) 0.300 Uiso 1 1 d RD . . Cl2 Cl 0.0518(4) 0.2312(3) 0.2422(4) 0.300 Uiso 1 1 d RD . . 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 0.0799(6) 0.0694(6) 0.0766(7) -0.0033(6) -0.0001(6) -0.0120(4) Ru2 0.0808(8) 0.0668(7) 0.0660(8) 0.000 0.000 -0.0122(6) N1 0.082(8) 0.074(7) 0.082(8) -0.009(5) 0.016(6) -0.012(5) N2 0.086(6) 0.065(5) 0.079(6) -0.015(6) 0.023(7) -0.010(5) N3 0.091(9) 0.083(7) 0.078(8) -0.007(6) 0.010(6) -0.017(6) N4 0.078(6) 0.066(6) 0.067(6) -0.009(5) -0.015(5) 0.002(5) N5 0.062(9) 0.102(12) 0.066(10) 0.000 0.000 -0.001(8) N6 0.100(9) 0.078(8) 0.077(8) -0.001(6) 0.022(7) -0.013(6) N7 0.097(13) 0.054(9) 0.082(12) 0.000 0.000 -0.004(7) C1 0.072(9) 0.095(11) 0.100(12) -0.019(9) -0.002(8) 0.002(7) C2 0.087(10) 0.084(10) 0.113(13) 0.010(9) 0.003(8) 0.014(8) C3 0.139(16) 0.080(10) 0.102(13) -0.011(9) -0.019(11) 0.034(11) C4 0.090(9) 0.062(7) 0.094(11) 0.007(7) 0.021(8) 0.002(6) C5 0.086(9) 0.068(7) 0.080(9) -0.004(7) 0.008(7) -0.004(6) C6 0.089(10) 0.082(9) 0.066(8) -0.004(6) 0.007(6) -0.005(7) C7 0.095(10) 0.098(11) 0.098(12) -0.030(9) 0.034(8) -0.025(8) C8 0.081(10) 0.094(11) 0.142(17) -0.034(11) 0.039(10) -0.018(8) C9 0.21(2) 0.092(12) 0.113(15) -0.055(11) 0.054(15) -0.064(14) C10 0.116(12) 0.072(9) 0.088(11) -0.005(8) 0.016(9) -0.014(8) C11 0.084(9) 0.084(9) 0.094(11) -0.007(8) -0.017(7) -0.024(7) C12 0.135(15) 0.074(9) 0.090(12) -0.028(8) -0.037(10) -0.017(9) C13 0.096(10) 0.116(12) 0.069(9) -0.004(8) 0.000(8) -0.004(9) C14 0.092(9) 0.072(8) 0.085(10) -0.016(7) -0.004(7) 0.002(7) C15 0.069(7) 0.059(7) 0.081(9) 0.002(6) -0.015(6) -0.003(5) C16 0.107(11) 0.082(9) 0.101(12) -0.001(8) 0.029(9) 0.005(8) C17 0.086(11) 0.119(13) 0.101(13) 0.007(10) 0.032(10) 0.024(10) C18 0.128(15) 0.109(12) 0.084(12) -0.018(9) 0.006(10) 0.047(11) C19 0.119(13) 0.088(10) 0.074(10) 0.015(7) -0.011(8) -0.010(9) C20 0.109(11) 0.068(8) 0.072(9) -0.004(7) 0.012(8) -0.022(7) C21 0.084(8) 0.115(10) 0.077(9) -0.015(10) 0.013(10) -0.021(7) C22 0.151(17) 0.099(11) 0.102(16) -0.012(9) 0.036(12) -0.036(11) C23 0.132(15) 0.115(14) 0.14(2) 0.017(12) 0.013(13) -0.012(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C21 1.965(13) . ? Ru1 N4 2.102(11) . ? Ru1 N3 2.113(12) 2_565 ? Ru1 N1 2.134(13) . ? Ru1 N6 2.137(13) . ? Ru1 Ru2 2.3304(9) . ? Ru2 N5 1.971(18) . ? Ru2 N2 1.999(10) . ? Ru2 N2 1.999(10) 2_565 ? Ru2 N7 2.050(19) . ? Ru2 Ru1 2.3304(9) 2_565 ? N1 C1 1.282(19) . ? N1 C5 1.441(18) . ? N2 C6 1.370(18) . ? N2 C5 1.38(2) . ? N3 C6 1.345(19) . ? N3 C10 1.41(2) . ? N3 Ru1 2.113(12) 2_565 ? N4 C15 1.364(18) . ? N4 C11 1.384(17) . ? N5 C15 1.392(16) . ? N5 C15 1.392(16) 2_565 ? N6 C16 1.37(2) . ? N6 C20 1.37(2) . ? N7 C20 1.329(18) 2_565 ? N7 C20 1.329(18) . ? N8 C29 1.176(8) . ? C1 C2 1.31(2) . ? C2 C3 1.32(3) . ? C3 C4 1.40(2) . ? C4 C5 1.36(2) . ? C6 C7 1.43(2) . ? C7 C8 1.32(2) . ? C8 C9 1.39(3) . ? C9 C10 1.40(3) . ? C11 C12 1.40(3) . ? C12 C13 1.29(2) . ? C13 C14 1.41(2) . ? C14 C15 1.42(2) . ? C16 C17 1.41(3) . ? C17 C18 1.23(3) . ? C18 C19 1.54(3) . ? C19 C20 1.40(2) . ? C21 C22 1.229(15) . ? C22 C23 1.5384 . ? C23 C28 1.3899 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3899 . ? C26 C29 1.3699 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C30 Cl2 1.7038 . ? C30 Cl1 1.7126 . ? 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 C21 Ru1 N4 94.5(7) . . ? C21 Ru1 N3 94.0(6) . 2_565 ? N4 Ru1 N3 88.5(5) . 2_565 ? C21 Ru1 N1 91.8(6) . . ? N4 Ru1 N1 88.7(4) . . ? N3 Ru1 N1 173.8(5) 2_565 . ? C21 Ru1 N6 92.3(7) . . ? N4 Ru1 N6 173.1(5) . . ? N3 Ru1 N6 89.5(5) 2_565 . ? N1 Ru1 N6 92.6(5) . . ? C21 Ru1 Ru2 178.8(5) . . ? N4 Ru1 Ru2 86.5(3) . . ? N3 Ru1 Ru2 86.9(3) 2_565 . ? N1 Ru1 Ru2 87.4(3) . . ? N6 Ru1 Ru2 86.8(3) . . ? N5 Ru2 N2 89.2(4) . . ? N5 Ru2 N2 89.2(4) . 2_565 ? N2 Ru2 N2 178.4(9) . 2_565 ? N5 Ru2 N7 180.000(3) . . ? N2 Ru2 N7 90.8(4) . . ? N2 Ru2 N7 90.8(4) 2_565 . ? N5 Ru2 Ru1 89.91(5) . 2_565 ? N2 Ru2 Ru1 89.1(3) . 2_565 ? N2 Ru2 Ru1 90.9(3) 2_565 2_565 ? N7 Ru2 Ru1 90.09(5) . 2_565 ? N5 Ru2 Ru1 89.91(5) . . ? N2 Ru2 Ru1 90.9(3) . . ? N2 Ru2 Ru1 89.1(3) 2_565 . ? N7 Ru2 Ru1 90.09(5) . . ? Ru1 Ru2 Ru1 179.83(10) 2_565 . ? C1 N1 C5 118.4(14) . . ? C1 N1 Ru1 123.3(10) . . ? C5 N1 Ru1 117.3(10) . . ? C6 N2 C5 120.0(11) . . ? C6 N2 Ru2 121.5(10) . . ? C5 N2 Ru2 117.9(8) . . ? C6 N3 C10 122.8(13) . . ? C6 N3 Ru1 119.9(9) . 2_565 ? C10 N3 Ru1 117.2(10) . 2_565 ? C15 N4 C11 118.5(12) . . ? C15 N4 Ru1 120.6(8) . . ? C11 N4 Ru1 119.9(10) . . ? C15 N5 C15 120.2(18) . 2_565 ? C15 N5 Ru2 119.9(9) . . ? C15 N5 Ru2 119.9(9) 2_565 . ? C16 N6 C20 122.0(14) . . ? C16 N6 Ru1 119.1(12) . . ? C20 N6 Ru1 118.9(9) . . ? C20 N7 C20 121(2) 2_565 . ? C20 N7 Ru2 119.4(10) 2_565 . ? C20 N7 Ru2 119.4(10) . . ? N1 C1 C2 125.5(16) . . ? C1 C2 C3 119.5(17) . . ? C2 C3 C4 119.5(15) . . ? C5 C4 C3 120.2(14) . . ? C4 C5 N2 127.7(13) . . ? C4 C5 N1 116.4(14) . . ? N2 C5 N1 115.7(12) . . ? N3 C6 N2 115.3(12) . . ? N3 C6 C7 119.3(13) . . ? N2 C6 C7 125.4(13) . . ? C8 C7 C6 120.1(17) . . ? C7 C8 C9 119.5(16) . . ? C8 C9 C10 123.7(16) . . ? C9 C10 N3 114.2(17) . . ? N4 C11 C12 120.3(15) . . ? C13 C12 C11 121.1(14) . . ? C12 C13 C14 121.7(16) . . ? C13 C14 C15 117.1(14) . . ? N4 C15 N5 114.0(13) . . ? N4 C15 C14 121.2(11) . . ? N5 C15 C14 124.4(13) . . ? N6 C16 C17 117.6(18) . . ? C18 C17 C16 125.1(17) . . ? C17 C18 C19 119.7(17) . . ? C20 C19 C18 114.9(16) . . ? N7 C20 N6 118.0(14) . . ? N7 C20 C19 120.9(15) . . ? N6 C20 C19 120.3(15) . . ? C22 C21 Ru1 167.9(18) . . ? C21 C22 C23 174.4(11) . . ? C28 C23 C24 120.0 . . ? C28 C23 C22 122.4 . . ? C24 C23 C22 117.4 . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C29 C26 C25 121.6 . . ? C29 C26 C27 116.6 . . ? C25 C26 C27 120.0 . . ? C26 C27 C28 120.0 . . ? C23 C28 C27 120.0 . . ? N8 C29 C26 163.1(19) . . ? Cl2 C30 Cl1 111.9 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.320 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.177 #===END data_ic11424 #(compound 6) _database_code_depnum_ccdc_archive 'CCDC 270954' _chemical_name_common (Ru3(CCPhNO2)2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59.50 H51 Cl5 N14 O6 Ru3' _chemical_formula_weight 1538.60 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 Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 18.1581(4) _cell_length_b 19.5166(4) _cell_length_c 19.0706(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.5956(11) _cell_angle_gamma 90.00 _cell_volume 6540.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3084 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58926 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11501 _reflns_number_gt 7329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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^)+(0.1668P)^2^+51.4380P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11501 _refine_ls_number_parameters 718 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1330 _refine_ls_R_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.2880 _refine_ls_wR_factor_gt 0.2441 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.004 _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 0.63177(4) 0.57390(4) 0.30085(4) 0.0380(3) Uani 1 1 d . . . Ru2 Ru 0.5000 0.57563(6) 0.2500 0.0367(3) Uani 1 2 d S . . N1 N 0.6397(4) 0.5378(5) 0.1992(4) 0.045(2) Uani 1 1 d . . . N2 N 0.5177(4) 0.5792(4) 0.1489(4) 0.0373(18) Uani 1 1 d . . . N3 N 0.3911(4) 0.6125(5) 0.1041(4) 0.0420(19) Uani 1 1 d . . . N4 N 0.6301(4) 0.6756(5) 0.2623(4) 0.044(2) Uani 1 1 d . . . N5 N 0.5000 0.6785(6) 0.2500 0.040(3) Uani 1 2 d S . . N6 N 0.6173(4) 0.4731(4) 0.3347(4) 0.0393(19) Uani 1 1 d . . . N7 N 0.5000 0.4715(6) 0.2500 0.040(3) Uani 1 2 d S . . N8 N 1.1290(8) 0.5571(8) 0.4816(8) 0.112(6) Uani 1 1 d D . . O1 O 1.1683(6) 0.5136(8) 0.4628(7) 0.121(5) Uani 1 1 d D . . O2 O 1.1577(7) 0.5989(9) 0.5294(9) 0.142(6) Uani 1 1 d D . . C1 C 0.7010(6) 0.4999(6) 0.1929(6) 0.049(3) Uani 1 1 d . . . H1A H 0.7390 0.4889 0.2356 0.059 Uiso 1 1 calc R . . C2 C 0.7103(7) 0.4768(6) 0.1270(7) 0.059(3) Uani 1 1 d . . . H2A H 0.7536 0.4505 0.1245 0.070 Uiso 1 1 calc R . . C3 C 0.6561(6) 0.4925(7) 0.0663(6) 0.059(3) Uani 1 1 d . . . H3A H 0.6621 0.4786 0.0203 0.071 Uiso 1 1 calc R . . C4 C 0.5925(6) 0.5285(6) 0.0708(6) 0.049(3) Uani 1 1 d . . . H4A H 0.5547 0.5389 0.0277 0.058 Uiso 1 1 calc R . . C5 C 0.5824(5) 0.5497(5) 0.1367(5) 0.040(2) Uani 1 1 d . . . C6 C 0.4646(6) 0.6105(6) 0.0950(5) 0.045(2) Uani 1 1 d . . . C7 C 0.4814(7) 0.6482(6) 0.0383(6) 0.055(3) Uani 1 1 d . . . H7A H 0.5327 0.6520 0.0352 0.066 Uiso 1 1 calc R . . C8 C 0.4242(7) 0.6799(7) -0.0130(6) 0.060(3) Uani 1 1 d . . . H8A H 0.4358 0.7035 -0.0525 0.072 Uiso 1 1 calc R . . C9 C 0.3508(7) 0.6772(7) -0.0067(6) 0.061(3) Uani 1 1 d . . . H9A H 0.3105 0.6974 -0.0425 0.073 Uiso 1 1 calc R . . C10 C 0.3363(6) 0.6443(6) 0.0531(6) 0.049(3) Uani 1 1 d . . . H10A H 0.2857 0.6442 0.0585 0.059 Uiso 1 1 calc R . . C11 C 0.6942(6) 0.7040(6) 0.2505(6) 0.048(3) Uani 1 1 d . . . H11A H 0.7407 0.6794 0.2652 0.058 Uiso 1 1 calc R . . C12 C 0.6950(6) 0.7666(6) 0.2182(7) 0.057(3) Uani 1 1 d . . . H12A H 0.7410 0.7847 0.2109 0.069 Uiso 1 1 calc R . . C13 C 0.6273(7) 0.8035(7) 0.1964(7) 0.061(3) Uani 1 1 d . . . H13A H 0.6264 0.8470 0.1739 0.074 Uiso 1 1 calc R . . C14 C 0.5628(6) 0.7759(6) 0.2081(6) 0.053(3) Uani 1 1 d . . . H14A H 0.5160 0.8000 0.1931 0.064 Uiso 1 1 calc R . . C15 C 0.5652(5) 0.7121(5) 0.2422(5) 0.039(2) Uani 1 1 d . . . C16 C 0.6687(6) 0.4442(5) 0.3896(5) 0.043(2) Uani 1 1 d . . . H16A H 0.7144 0.4684 0.4103 0.052 Uiso 1 1 calc R . . C17 C 0.6585(7) 0.3821(7) 0.4167(6) 0.060(3) Uani 1 1 d . . . H17A H 0.6964 0.3634 0.4557 0.072 Uiso 1 1 calc R . . C18 C 0.5905(7) 0.3449(7) 0.3868(7) 0.063(3) Uani 1 1 d . . . H18A H 0.5820 0.3011 0.4050 0.075 Uiso 1 1 calc R . . C19 C 0.5381(6) 0.3742(6) 0.3310(7) 0.056(3) Uani 1 1 d . . . H19A H 0.4916 0.3511 0.3105 0.067 Uiso 1 1 calc R . . C20 C 0.5523(5) 0.4377(5) 0.3037(5) 0.041(2) Uani 1 1 d . . . C21 C 0.7445(6) 0.5706(5) 0.3400(6) 0.046(3) Uani 1 1 d . . . C22 C 0.8141(6) 0.5643(6) 0.3631(6) 0.050(3) Uani 1 1 d . . . C23 C 0.8943(6) 0.5597(7) 0.3905(7) 0.059(3) Uani 1 1 d . . . C24 C 0.9382(8) 0.5185(10) 0.3620(8) 0.090(5) Uani 1 1 d . . . H24A H 0.9166 0.4908 0.3210 0.108 Uiso 1 1 calc R . . C25 C 1.0209(9) 0.5172(10) 0.3958(10) 0.094(5) Uani 1 1 d . . . H25A H 1.0537 0.4870 0.3789 0.113 Uiso 1 1 calc R . . C26 C 1.0470(8) 0.5583(9) 0.4490(8) 0.073(4) Uani 1 1 d . . . C27 C 1.0062(8) 0.6001(8) 0.4823(11) 0.097(6) Uani 1 1 d . . . H27A H 1.0282 0.6267 0.5241 0.117 Uiso 1 1 calc R . . C28 C 0.9301(8) 0.5995(8) 0.4492(10) 0.099(6) Uani 1 1 d . . . H28A H 0.8987 0.6294 0.4683 0.119 Uiso 1 1 calc R . . Ru3 Ru 0.91740(5) 0.13977(5) 0.63304(5) 0.0451(3) Uani 1 1 d . . . Ru4 Ru 1.0000 0.13924(6) 0.7500 0.0430(3) Uani 1 2 d S . . N9 N 1.0117(5) 0.1761(5) 0.5974(5) 0.049(2) Uani 1 1 d . . . N10 N 1.0914(5) 0.1365(5) 0.7074(5) 0.050(2) Uani 1 1 d . . . N11 N 1.1668(5) 0.1018(5) 0.8195(5) 0.049(2) Uani 1 1 d . . . N12 N 0.8919(5) 0.2425(5) 0.6535(4) 0.046(2) Uani 1 1 d . . . N13 N 1.0000 0.2426(6) 0.7500 0.045(3) Uani 1 2 d S . . N14 N 0.9503(5) 0.0370(5) 0.6246(5) 0.053(2) Uani 1 1 d . . . N15 N 1.0000 0.0361(6) 0.7500 0.049(3) Uani 1 2 d S . . C29 C 1.0034(7) 0.2104(6) 0.5343(6) 0.056(3) Uani 1 1 d . . . H29A H 0.9532 0.2194 0.5060 0.067 Uiso 1 1 calc R . . C30 C 1.0625(8) 0.2328(6) 0.5090(7) 0.061(3) Uani 1 1 d . . . H30A H 1.0534 0.2542 0.4629 0.073 Uiso 1 1 calc R . . C31 C 1.1343(8) 0.2247(7) 0.5498(7) 0.065(3) Uani 1 1 d . . . H31A H 1.1757 0.2418 0.5329 0.078 Uiso 1 1 calc R . . C32 C 1.1484(7) 0.1912(7) 0.6172(7) 0.066(3) Uani 1 1 d . . . H32A H 1.1986 0.1852 0.6466 0.079 Uiso 1 1 calc R . . C33 C 1.0840(7) 0.1668(6) 0.6393(6) 0.054(3) Uani 1 1 d . . . C34 C 1.1563(6) 0.1040(6) 0.7452(6) 0.053(3) Uani 1 1 d . . . C35 C 1.2060(7) 0.0699(7) 0.7134(7) 0.066(3) Uani 1 1 d . . . H35A H 1.1975 0.0700 0.6622 0.079 Uiso 1 1 calc R . . C36 C 1.2684(7) 0.0356(8) 0.7560(8) 0.076(4) Uani 1 1 d . . . H36A H 1.3028 0.0116 0.7347 0.092 Uiso 1 1 calc R . . C37 C 1.2789(8) 0.0373(8) 0.8297(8) 0.076(4) Uani 1 1 d . . . H37A H 1.3223 0.0160 0.8602 0.092 Uiso 1 1 calc R . . C38 C 1.2287(6) 0.0684(6) 0.8585(7) 0.055(3) Uani 1 1 d . . . H38A H 1.2367 0.0670 0.9097 0.065 Uiso 1 1 calc R . . C39 C 0.8290(6) 0.2740(6) 0.6136(6) 0.051(3) Uani 1 1 d . . . H39A H 0.7980 0.2500 0.5735 0.061 Uiso 1 1 calc R . . C40 C 0.8076(6) 0.3383(6) 0.6278(6) 0.054(3) Uani 1 1 d . . . H40A H 0.7640 0.3594 0.5974 0.065 Uiso 1 1 calc R . . C41 C 0.8517(7) 0.3724(6) 0.6883(6) 0.057(3) Uani 1 1 d . . . H41A H 0.8374 0.4167 0.7009 0.069 Uiso 1 1 calc R . . C42 C 0.9145(6) 0.3418(6) 0.7285(6) 0.050(3) Uani 1 1 d . . . H42A H 0.9442 0.3648 0.7700 0.060 Uiso 1 1 calc R . . C43 C 0.9371(6) 0.2774(6) 0.7108(6) 0.047(3) Uani 1 1 d . . . C44 C 0.9347(7) 0.0057(7) 0.5605(7) 0.061(3) Uani 1 1 d . . . H44A H 0.9063 0.0291 0.5187 0.073 Uiso 1 1 calc R . . C45 C 0.9595(9) -0.0612(8) 0.5542(8) 0.077(4) Uani 1 1 d . . . H45A H 0.9445 -0.0841 0.5088 0.092 Uiso 1 1 calc R . . C46 C 1.0042(10) -0.0935(8) 0.6111(8) 0.085(5) Uani 1 1 d . . . H46A H 1.0253 -0.1369 0.6048 0.102 Uiso 1 1 calc R . . C47 C 1.0193(8) -0.0647(7) 0.6771(7) 0.072(4) Uani 1 1 d . . . H47A H 1.0499 -0.0876 0.7182 0.087 Uiso 1 1 calc R . . C48 C 0.9876(7) 0.0021(6) 0.6839(6) 0.052(3) Uani 1 1 d . . . C49 C 0.8495(6) 0.1420(6) 0.5315(6) 0.051(3) Uani 1 1 d . . . C50 C 0.8150(4) 0.1481(4) 0.4696(4) 0.069(4) Uani 1 1 d . . . C51 C 0.7694(4) 0.1692(4) 0.3994(4) 0.091(5) Uani 1 1 d R . . C52 C 0.7770(4) 0.2369(4) 0.3797(4) 0.128(7) Uiso 1 1 d R C . H52A H 0.8147 0.2660 0.4083 0.153 Uiso 1 1 calc R C . C53 C 0.7276(4) 0.2602(4) 0.3172(4) 0.127(7) Uiso 1 1 d R C . H53A H 0.7113 0.3066 0.3123 0.153 Uiso 0.50 1 calc PR A 1 H53B H 0.7354 0.3054 0.3018 0.153 Uiso 0.50 1 d PR B 2 C54 C 0.7026(4) 0.2133(4) 0.2614(4) 0.122(13) Uiso 0.50 1 d PRD C 1 C55 C 0.7198(4) 0.1442(4) 0.2730(4) 0.087(9) Uiso 0.50 1 d PR C 1 H55A H 0.7027 0.1122 0.2349 0.104 Uiso 0.50 1 calc PR D 1 C56 C 0.7620(4) 0.1220(4) 0.3405(4) 0.064(7) Uiso 0.50 1 d PR C 1 H56A H 0.7847 0.0778 0.3472 0.077 Uiso 0.50 1 calc PR C 1 N16 N 0.6446(11) 0.2701(8) 0.2224(17) 0.120 Uiso 0.50 1 d PD C 1 O3 O 0.5836(15) 0.2365(16) 0.1940(18) 0.159(12) Uiso 0.50 1 d PD C 1 O4 O 0.6753(8) 0.3297(8) 0.2215(8) 0.075(5) Uiso 0.50 1 d PD C 1 C54' C 0.6708(8) 0.2254(8) 0.2770(8) 0.110(12) Uiso 0.50 1 d PRD C 2 C55' C 0.6633(8) 0.1577(8) 0.2967(8) 0.121(13) Uiso 0.50 1 d PR C 2 H55B H 0.6238 0.1299 0.2684 0.145 Uiso 0.50 1 calc PR C 2 C56' C 0.7135(8) 0.1305(8) 0.3578(8) 0.119(13) Uiso 0.50 1 d PR C 2 H56B H 0.7084 0.0840 0.3705 0.143 Uiso 0.50 1 calc PR C 2 N16' N 0.651(2) 0.2299(16) 0.1923(9) 0.120 Uiso 0.50 1 d PD C 2 O3' O 0.6412(19) 0.2933(15) 0.1783(18) 0.145(11) Uiso 0.50 1 d PD C 2 O4' O 0.637(2) 0.1816(18) 0.146(2) 0.196(15) Uiso 0.50 1 d PD C 2 C57 C 0.630(4) 0.144(2) 0.971(2) 0.50(5) Uiso 1 1 d D . . H57A H 0.6643 0.1585 1.0176 0.604 Uiso 1 1 calc R . . H57B H 0.5757 0.1475 0.9715 0.604 Uiso 1 1 calc R . . C58 C 0.6525(15) 0.078(3) 0.939(3) 0.37(3) Uiso 1 1 d D . . H58A H 0.6436 0.0854 0.8861 0.440 Uiso 1 1 calc R . . H58B H 0.6155 0.0425 0.9451 0.440 Uiso 1 1 calc R . . Cl1 Cl 0.6518(3) 0.1789(3) 0.8938(4) 0.135(2) Uani 1 1 d D . . Cl2 Cl 0.7429(4) 0.0407(3) 0.9682(3) 0.142(2) Uani 1 1 d D . . C59 C 0.564(3) -0.1293(16) -0.0104(15) 0.35(3) Uiso 1 1 d D . . H59A H 0.5153 -0.1490 -0.0381 0.426 Uiso 1 1 calc R . . H59B H 0.5857 -0.1051 -0.0464 0.426 Uiso 1 1 calc R . . Cl3 Cl 0.6245(6) -0.2005(5) 0.0172(5) 0.209(4) Uiso 1 1 d D . . Cl4 Cl 0.5388(9) -0.0636(8) 0.0432(9) 0.327(7) Uiso 1 1 d D . . C60 C 0.5000 -0.0431(17) 0.2500 0.26(3) Uiso 1 2 d SD . . H60A H 0.5386 -0.0377 0.2938 0.313 Uiso 1 1 d . . . Cl5 Cl 0.538(2) -0.0580(19) 0.1782(14) 0.46(2) Uiso 0.50 1 d PD . . Cl6 Cl 0.4403(13) 0.0286(14) 0.2270(14) 0.283(12) Uiso 0.50 1 d PD . . O7 O 1.1424(9) 0.3383(10) 0.3921(9) 0.168(7) Uani 1 1 d . . . H7 H 1.1044 0.3512 0.3498 0.253 Uiso 1 1 d . . . H7' H 1.1650 0.3034 0.3942 0.253 Uiso 1 1 d . . . O8 O 0.8364(15) 0.1945(16) 0.1528(14) 0.278(14) Uani 1 1 d . . . H8 H 0.7811 0.1789 0.1296 0.417 Uiso 1 1 d . . . H8' H 0.8185 0.2240 0.1758 0.417 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0241(4) 0.0545(5) 0.0326(4) 0.0006(4) 0.0018(3) 0.0000(3) Ru2 0.0237(5) 0.0534(7) 0.0304(6) 0.000 0.0019(4) 0.000 N1 0.033(4) 0.065(6) 0.038(5) 0.004(4) 0.011(4) -0.005(4) N2 0.028(4) 0.049(5) 0.032(4) 0.004(4) 0.003(3) 0.003(3) N3 0.037(4) 0.056(5) 0.028(4) -0.002(4) -0.002(3) -0.002(4) N4 0.028(4) 0.067(6) 0.033(4) 0.003(4) 0.003(3) -0.002(4) N5 0.040(6) 0.048(7) 0.028(6) 0.000 0.002(5) 0.000 N6 0.034(4) 0.051(5) 0.033(4) 0.002(4) 0.010(4) 0.008(4) N7 0.027(6) 0.051(7) 0.041(7) 0.000 0.007(5) 0.000 N8 0.058(9) 0.164(17) 0.106(12) 0.065(12) 0.004(9) -0.002(10) O1 0.057(6) 0.194(14) 0.114(10) 0.061(10) 0.025(6) 0.045(8) O2 0.052(7) 0.205(16) 0.143(13) 0.065(12) -0.025(7) -0.018(8) C1 0.036(5) 0.064(7) 0.046(6) -0.001(5) 0.006(5) 0.000(5) C2 0.054(7) 0.069(8) 0.057(7) -0.011(6) 0.021(6) 0.006(6) C3 0.049(7) 0.081(9) 0.049(7) -0.011(6) 0.016(6) -0.002(6) C4 0.038(6) 0.068(7) 0.038(6) -0.006(5) 0.006(4) -0.003(5) C5 0.032(5) 0.051(6) 0.036(5) 0.003(5) 0.005(4) -0.008(4) C6 0.044(6) 0.057(6) 0.031(5) -0.012(5) 0.005(4) -0.004(5) C7 0.047(6) 0.079(8) 0.038(6) 0.002(6) 0.010(5) -0.003(6) C8 0.069(8) 0.078(8) 0.033(6) 0.025(6) 0.014(5) 0.007(6) C9 0.053(7) 0.076(8) 0.047(7) 0.004(6) 0.002(5) 0.007(6) C10 0.044(6) 0.060(7) 0.041(6) 0.008(5) 0.005(5) -0.005(5) C11 0.032(5) 0.062(7) 0.048(6) -0.004(5) 0.006(5) -0.010(5) C12 0.045(6) 0.065(8) 0.063(8) 0.002(6) 0.014(6) -0.008(6) C13 0.059(7) 0.062(8) 0.064(8) 0.012(6) 0.016(6) -0.009(6) C14 0.038(6) 0.066(7) 0.052(7) 0.012(6) 0.004(5) 0.002(5) C15 0.028(5) 0.047(6) 0.038(5) 0.001(5) 0.001(4) -0.002(4) C16 0.042(6) 0.056(7) 0.029(5) 0.007(5) 0.005(4) 0.010(5) C17 0.055(7) 0.082(9) 0.041(6) 0.020(6) 0.008(5) 0.017(6) C18 0.050(7) 0.070(8) 0.071(8) 0.025(7) 0.020(6) 0.003(6) C19 0.043(6) 0.067(8) 0.055(7) 0.017(6) 0.011(5) 0.000(5) C20 0.033(5) 0.052(6) 0.039(6) 0.001(5) 0.012(4) 0.006(4) C21 0.042(6) 0.051(6) 0.048(6) 0.003(5) 0.013(5) -0.003(5) C22 0.030(6) 0.060(7) 0.053(7) 0.009(5) -0.002(5) -0.004(5) C23 0.034(6) 0.076(8) 0.064(8) 0.029(7) 0.009(6) 0.010(6) C24 0.053(8) 0.146(15) 0.074(10) 0.029(10) 0.021(7) 0.031(9) C25 0.072(10) 0.127(15) 0.098(13) 0.022(12) 0.049(10) 0.013(10) C26 0.051(8) 0.104(12) 0.061(9) 0.021(8) 0.006(7) -0.018(8) C27 0.056(9) 0.078(10) 0.137(16) 0.011(10) -0.015(10) -0.001(8) C28 0.061(9) 0.080(10) 0.125(15) 0.016(10) -0.034(9) -0.015(8) Ru3 0.0430(5) 0.0534(6) 0.0352(5) -0.0017(4) 0.0029(4) -0.0009(4) Ru4 0.0407(6) 0.0505(7) 0.0347(6) 0.000 0.0039(5) 0.000 N9 0.041(5) 0.061(6) 0.042(5) -0.004(4) 0.007(4) 0.000(4) N10 0.048(5) 0.054(5) 0.047(5) -0.004(4) 0.012(4) -0.004(4) N11 0.034(5) 0.060(6) 0.049(5) -0.001(5) 0.003(4) -0.004(4) N12 0.047(5) 0.059(6) 0.030(4) 0.000(4) 0.008(4) -0.002(4) N13 0.043(7) 0.049(7) 0.039(7) 0.000 0.003(5) 0.000 N14 0.051(5) 0.059(6) 0.045(5) -0.008(5) 0.004(4) -0.003(5) N15 0.054(8) 0.046(7) 0.040(7) 0.000 0.002(6) 0.000 C29 0.063(7) 0.051(7) 0.051(7) -0.005(6) 0.011(6) -0.006(6) C30 0.075(9) 0.058(7) 0.048(7) 0.000(6) 0.012(6) -0.005(6) C31 0.068(8) 0.068(8) 0.062(8) -0.007(7) 0.025(7) -0.025(7) C32 0.059(7) 0.090(10) 0.050(7) 0.000(7) 0.015(6) -0.016(7) C33 0.056(7) 0.070(8) 0.038(6) -0.005(5) 0.016(5) -0.007(6) C34 0.039(6) 0.065(7) 0.053(7) 0.001(6) 0.007(5) -0.004(5) C35 0.059(8) 0.082(9) 0.057(8) -0.015(7) 0.015(6) -0.004(7) C36 0.047(7) 0.107(11) 0.074(10) -0.015(8) 0.013(7) 0.019(7) C37 0.065(9) 0.092(10) 0.067(9) -0.008(8) 0.007(7) 0.017(8) C38 0.050(7) 0.050(7) 0.058(7) 0.007(6) 0.005(6) 0.008(5) C39 0.042(6) 0.068(8) 0.038(6) 0.005(5) 0.001(5) 0.002(5) C40 0.046(6) 0.067(8) 0.045(6) 0.006(6) 0.003(5) 0.013(6) C41 0.062(7) 0.062(7) 0.052(7) -0.006(6) 0.022(6) 0.008(6) C42 0.049(6) 0.060(7) 0.040(6) 0.005(5) 0.011(5) 0.006(5) C43 0.051(6) 0.049(6) 0.041(6) 0.004(5) 0.014(5) 0.000(5) C44 0.063(7) 0.063(8) 0.052(7) -0.015(6) 0.006(6) -0.007(6) C45 0.091(10) 0.080(10) 0.054(8) -0.019(7) 0.008(7) 0.003(8) C46 0.112(12) 0.071(9) 0.059(9) -0.009(7) 0.000(8) 0.029(9) C47 0.079(9) 0.068(9) 0.059(8) -0.005(7) -0.003(7) 0.012(7) C48 0.055(6) 0.047(6) 0.050(7) -0.005(5) 0.006(5) -0.004(5) C49 0.055(7) 0.059(7) 0.035(6) -0.003(5) 0.005(5) -0.004(5) C50 0.073(9) 0.075(9) 0.050(8) 0.002(7) 0.002(7) 0.009(7) C51 0.108(12) 0.107(12) 0.047(8) 0.003(8) 0.001(8) 0.020(10) Cl1 0.093(3) 0.131(4) 0.155(5) 0.040(4) -0.015(3) 0.004(3) Cl2 0.135(4) 0.173(5) 0.126(4) 0.068(4) 0.050(4) 0.071(4) O7 0.139(13) 0.245(18) 0.142(13) 0.002(12) 0.075(11) -0.092(13) O8 0.27(3) 0.36(4) 0.28(3) 0.00(3) 0.21(3) 0.06(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C21 1.996(11) . ? Ru1 N3 2.099(8) 2_655 ? Ru1 N1 2.102(8) . ? Ru1 N6 2.107(8) . ? Ru1 N4 2.114(9) . ? Ru1 Ru2 2.3445(7) . ? Ru2 N5 2.007(12) . ? Ru2 N7 2.033(12) . ? Ru2 N2 2.033(8) . ? Ru2 N2 2.033(8) 2_655 ? Ru2 Ru1 2.3445(7) 2_655 ? N1 C1 1.367(13) . ? N1 C5 1.390(13) . ? N2 C6 1.364(13) . ? N2 C5 1.380(13) . ? N3 C10 1.352(13) . ? N3 C6 1.390(13) . ? N3 Ru1 2.099(8) 2_655 ? N4 C15 1.347(12) . ? N4 C11 1.360(13) . ? N5 C15 1.395(11) . ? N5 C15 1.395(11) 2_655 ? N6 C16 1.339(12) . ? N6 C20 1.367(13) . ? N7 C20 1.377(11) 2_655 ? N7 C20 1.377(11) . ? N8 O1 1.220(9) . ? N8 O2 1.237(9) . ? N8 C26 1.462(19) . ? C1 C2 1.385(15) . ? C2 C3 1.352(17) . ? C3 C4 1.372(15) . ? C4 C5 1.379(14) . ? C6 C7 1.404(15) . ? C7 C8 1.381(16) . ? C8 C9 1.370(16) . ? C9 C10 1.390(16) . ? C11 C12 1.369(16) . ? C12 C13 1.393(16) . ? C13 C14 1.357(16) . ? C14 C15 1.401(15) . ? C16 C17 1.349(16) . ? C17 C18 1.421(17) . ? C18 C19 1.361(16) . ? C19 C20 1.394(15) . ? C21 C22 1.234(15) . ? C22 C23 1.422(15) . ? C23 C24 1.340(19) . ? C23 C28 1.38(2) . ? C24 C25 1.48(2) . ? C25 C26 1.29(2) . ? C26 C27 1.36(2) . ? C27 C28 1.37(2) . ? Ru3 C49 2.017(11) . ? Ru3 N11 2.099(9) 2_756 ? Ru3 N14 2.110(10) . ? Ru3 N12 2.116(9) . ? Ru3 N9 2.117(9) . ? Ru3 Ru4 2.3534(8) . ? Ru4 N15 2.013(12) . ? Ru4 N13 2.016(12) . ? Ru4 N10 2.024(9) . ? Ru4 N10 2.024(9) 2_756 ? Ru4 Ru3 2.3534(8) 2_756 ? N9 C29 1.353(14) . ? N9 C33 1.368(14) . ? N10 C34 1.373(14) . ? N10 C33 1.401(14) . ? N11 C38 1.348(14) . ? N11 C34 1.383(14) . ? N11 Ru3 2.099(9) 2_756 ? N12 C39 1.351(13) . ? N12 C43 1.370(13) . ? N13 C43 1.377(12) 2_756 ? N13 C43 1.377(12) . ? N14 C44 1.331(14) . ? N14 C48 1.348(14) . ? N15 C48 1.391(12) . ? N15 C48 1.391(12) 2_756 ? C29 C30 1.355(17) . ? C30 C31 1.349(18) . ? C31 C32 1.407(18) . ? C32 C33 1.421(16) . ? C34 C35 1.377(17) . ? C35 C36 1.389(18) . ? C36 C37 1.369(19) . ? C37 C38 1.325(17) . ? C39 C40 1.361(16) . ? C40 C41 1.396(17) . ? C41 C42 1.343(16) . ? C42 C43 1.391(15) . ? C44 C45 1.397(18) . ? C45 C46 1.338(19) . ? C46 C47 1.342(19) . ? C47 C48 1.444(17) . ? C49 C50 1.195(13) . ? C50 C51 1.4451 . ? C51 C56' 1.351(16) . ? C51 C52 1.3899 . ? C51 C56 1.4340 . ? C52 C53 1.3756 . ? C53 C54' 1.310(16) . ? C53 C54 1.3900 . ? C54 C55 1.3899 . ? C54 N16 1.580(10) . ? C55 C56 1.3900 . ? N16 O3 1.284(10) . ? N16 O4 1.293(10) . ? C54' C55' 1.3900 . ? C54' N16' 1.566(10) . ? C55' C56' 1.3899 . ? N16' O4' 1.268(10) . ? N16' O3' 1.270(10) . ? C57 C58 1.534(10) . ? C57 Cl1 1.750(10) . ? C58 Cl2 1.752(10) . ? C58 Cl1 2.15(5) . ? C59 Cl3 1.765(10) . ? C59 Cl4 1.773(10) . ? C60 Cl5 1.706(10) . ? C60 Cl5 1.706(10) 2_655 ? C60 Cl6 1.757(10) 2_655 ? C60 Cl6 1.757(10) . ? Cl5 Cl6 2.43(4) 2_655 ? Cl6 Cl6 2.13(5) 2_655 ? Cl6 Cl5 2.43(4) 2_655 ? 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 C21 Ru1 N3 95.5(4) . 2_655 ? C21 Ru1 N1 91.8(4) . . ? N3 Ru1 N1 172.6(3) 2_655 . ? C21 Ru1 N6 92.9(4) . . ? N3 Ru1 N6 90.2(3) 2_655 . ? N1 Ru1 N6 90.7(3) . . ? C21 Ru1 N4 94.8(4) . . ? N3 Ru1 N4 88.5(3) 2_655 . ? N1 Ru1 N4 89.6(3) . . ? N6 Ru1 N4 172.3(3) . . ? C21 Ru1 Ru2 177.4(3) . . ? N3 Ru1 Ru2 87.1(2) 2_655 . ? N1 Ru1 Ru2 85.6(2) . . ? N6 Ru1 Ru2 87.0(2) . . ? N4 Ru1 Ru2 85.3(2) . . ? N5 Ru2 N7 180.000(2) . . ? N5 Ru2 N2 88.1(2) . . ? N7 Ru2 N2 91.9(2) . . ? N5 Ru2 N2 88.1(2) . 2_655 ? N7 Ru2 N2 91.9(2) . 2_655 ? N2 Ru2 N2 176.1(5) . 2_655 ? N5 Ru2 Ru1 90.82(4) . 2_655 ? N7 Ru2 Ru1 89.18(4) . 2_655 ? N2 Ru2 Ru1 89.8(2) . 2_655 ? N2 Ru2 Ru1 90.2(2) 2_655 2_655 ? N5 Ru2 Ru1 90.82(4) . . ? N7 Ru2 Ru1 89.18(4) . . ? N2 Ru2 Ru1 90.2(2) . . ? N2 Ru2 Ru1 89.8(2) 2_655 . ? Ru1 Ru2 Ru1 178.35(7) 2_655 . ? C1 N1 C5 117.7(9) . . ? C1 N1 Ru1 120.6(7) . . ? C5 N1 Ru1 121.6(7) . . ? C6 N2 C5 121.9(8) . . ? C6 N2 Ru2 118.7(6) . . ? C5 N2 Ru2 119.4(6) . . ? C10 N3 C6 118.6(9) . . ? C10 N3 Ru1 121.1(7) . 2_655 ? C6 N3 Ru1 120.1(6) . 2_655 ? C15 N4 C11 117.4(9) . . ? C15 N4 Ru1 122.1(6) . . ? C11 N4 Ru1 120.2(7) . . ? C15 N5 C15 123.8(12) . 2_655 ? C15 N5 Ru2 118.1(6) . . ? C15 N5 Ru2 118.1(6) 2_655 . ? C16 N6 C20 118.7(9) . . ? C16 N6 Ru1 121.1(7) . . ? C20 N6 Ru1 120.0(6) . . ? C20 N7 C20 122.8(12) 2_655 . ? C20 N7 Ru2 118.6(6) 2_655 . ? C20 N7 Ru2 118.6(6) . . ? O1 N8 O2 120.4(17) . . ? O1 N8 C26 119.7(16) . . ? O2 N8 C26 119.8(14) . . ? N1 C1 C2 123.0(10) . . ? C3 C2 C1 118.3(11) . . ? C2 C3 C4 120.4(11) . . ? C3 C4 C5 121.1(10) . . ? C4 C5 N2 126.4(9) . . ? C4 C5 N1 119.3(9) . . ? N2 C5 N1 114.2(8) . . ? N2 C6 N3 116.0(9) . . ? N2 C6 C7 124.5(9) . . ? N3 C6 C7 118.9(10) . . ? C8 C7 C6 120.6(11) . . ? C9 C8 C7 119.8(10) . . ? C8 C9 C10 118.6(11) . . ? N3 C10 C9 123.0(10) . . ? N4 C11 C12 123.0(10) . . ? C11 C12 C13 119.2(10) . . ? C14 C13 C12 118.6(11) . . ? C13 C14 C15 120.1(10) . . ? N4 C15 N5 115.2(9) . . ? N4 C15 C14 121.7(9) . . ? N5 C15 C14 122.7(9) . . ? N6 C16 C17 122.8(10) . . ? C16 C17 C18 119.6(10) . . ? C19 C18 C17 117.7(11) . . ? C18 C19 C20 120.5(11) . . ? N6 C20 N7 116.0(9) . . ? N6 C20 C19 120.6(9) . . ? N7 C20 C19 123.1(9) . . ? C22 C21 Ru1 176.1(10) . . ? C21 C22 C23 177.9(13) . . ? C24 C23 C28 117.4(13) . . ? C24 C23 C22 123.2(14) . . ? C28 C23 C22 119.4(13) . . ? C23 C24 C25 118.4(16) . . ? C26 C25 C24 117.7(16) . . ? C25 C26 C27 127.4(15) . . ? C25 C26 N8 117.2(17) . . ? C27 C26 N8 115.2(15) . . ? C26 C27 C28 112.5(17) . . ? C27 C28 C23 126.4(19) . . ? C49 Ru3 N11 94.9(4) . 2_756 ? C49 Ru3 N14 93.6(4) . . ? N11 Ru3 N14 87.0(4) 2_756 . ? C49 Ru3 N12 92.7(4) . . ? N11 Ru3 N12 92.2(3) 2_756 . ? N14 Ru3 N12 173.6(3) . . ? C49 Ru3 N9 91.9(4) . . ? N11 Ru3 N9 173.1(3) 2_756 . ? N14 Ru3 N9 91.5(4) . . ? N12 Ru3 N9 88.5(3) . . ? C49 Ru3 Ru4 178.0(3) . . ? N11 Ru3 Ru4 87.1(2) 2_756 . ? N14 Ru3 Ru4 86.7(2) . . ? N12 Ru3 Ru4 86.9(2) . . ? N9 Ru3 Ru4 86.1(2) . . ? N15 Ru4 N13 180.000(3) . . ? N15 Ru4 N10 88.5(3) . . ? N13 Ru4 N10 91.5(3) . . ? N15 Ru4 N10 88.5(3) . 2_756 ? N13 Ru4 N10 91.5(3) . 2_756 ? N10 Ru4 N10 177.0(5) . 2_756 ? N15 Ru4 Ru3 90.25(4) . . ? N13 Ru4 Ru3 89.75(4) . . ? N10 Ru4 Ru3 90.6(3) . . ? N10 Ru4 Ru3 89.4(3) 2_756 . ? N15 Ru4 Ru3 90.25(4) . 2_756 ? N13 Ru4 Ru3 89.75(4) . 2_756 ? N10 Ru4 Ru3 89.4(3) . 2_756 ? N10 Ru4 Ru3 90.6(3) 2_756 2_756 ? Ru3 Ru4 Ru3 179.49(8) . 2_756 ? C29 N9 C33 117.5(10) . . ? C29 N9 Ru3 122.3(7) . . ? C33 N9 Ru3 120.2(7) . . ? C34 N10 C33 123.4(9) . . ? C34 N10 Ru4 118.9(7) . . ? C33 N10 Ru4 117.7(7) . . ? C38 N11 C34 117.4(10) . . ? C38 N11 Ru3 122.0(8) . 2_756 ? C34 N11 Ru3 120.2(7) . 2_756 ? C39 N12 C43 118.4(10) . . ? C39 N12 Ru3 121.3(7) . . ? C43 N12 Ru3 120.2(7) . . ? C43 N13 C43 120.8(13) 2_756 . ? C43 N13 Ru4 119.6(6) 2_756 . ? C43 N13 Ru4 119.6(6) . . ? C44 N14 C48 118.9(10) . . ? C44 N14 Ru3 120.5(8) . . ? C48 N14 Ru3 120.6(7) . . ? C48 N15 C48 123.1(13) . 2_756 ? C48 N15 Ru4 118.5(7) . . ? C48 N15 Ru4 118.5(7) 2_756 . ? N9 C29 C30 123.7(12) . . ? C31 C30 C29 119.7(12) . . ? C30 C31 C32 120.5(12) . . ? C31 C32 C33 117.0(12) . . ? N9 C33 N10 116.8(10) . . ? N9 C33 C32 121.5(11) . . ? N10 C33 C32 121.6(11) . . ? N10 C34 C35 124.3(11) . . ? N10 C34 N11 115.5(10) . . ? C35 C34 N11 120.0(11) . . ? C34 C35 C36 120.3(12) . . ? C37 C36 C35 118.0(12) . . ? C38 C37 C36 120.3(13) . . ? C37 C38 N11 123.9(12) . . ? N12 C39 C40 123.3(11) . . ? C39 C40 C41 118.2(10) . . ? C42 C41 C40 119.1(11) . . ? C41 C42 C43 121.6(11) . . ? N12 C43 N13 115.8(10) . . ? N12 C43 C42 119.3(10) . . ? N13 C43 C42 124.7(10) . . ? N14 C44 C45 120.7(12) . . ? C46 C45 C44 120.8(13) . . ? C45 C46 C47 120.2(14) . . ? C46 C47 C48 118.1(12) . . ? N14 C48 N15 116.8(10) . . ? N14 C48 C47 120.5(11) . . ? N15 C48 C47 122.3(11) . . ? C50 C49 Ru3 172.7(10) . . ? C49 C50 C51 168.2(7) . . ? C56' C51 C52 118.9(7) . . ? C56' C51 C56 43.2(7) . . ? C52 C51 C56 113.3 . . ? C56' C51 C50 123.7(7) . . ? C52 C51 C50 116.7 . . ? C56 C51 C50 117.4 . . ? C53 C52 C51 117.5 . . ? C54' C53 C52 125.4(8) . . ? C54' C53 C54 32.1(7) . . ? C52 C53 C54 117.5 . . ? C55 C54 C53 120.0 . . ? C55 C54 N16 148.4(8) . . ? C53 C54 N16 87.1(11) . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 116.4 . . ? O3 N16 O4 142(2) . . ? O3 N16 C54 104.0(19) . . ? O4 N16 C54 113.5(14) . . ? C53 C54' C55' 116.9(8) . . ? C53 C54' N16' 121.3(17) . . ? C55' C54' N16' 108.6(13) . . ? C56' C55' C54' 120.0 . . ? C51 C56' C55' 121.1(7) . . ? O4' N16' O3' 126(3) . . ? O4' N16' C54' 129(3) . . ? O3' N16' C54' 105(2) . . ? C58 C57 Cl1 82(3) . . ? C57 C58 Cl2 123(5) . . ? C57 C58 Cl1 53.6(15) . . ? Cl2 C58 Cl1 115(3) . . ? C57 Cl1 C58 44.9(11) . . ? Cl3 C59 Cl4 129.0(17) . . ? Cl5 C60 Cl5 160(3) . 2_655 ? Cl5 C60 Cl6 89.2(19) . 2_655 ? Cl5 C60 Cl6 106.5(8) 2_655 2_655 ? Cl5 C60 Cl6 106.5(8) . . ? Cl5 C60 Cl6 89.2(19) 2_655 . ? Cl6 C60 Cl6 74(2) 2_655 . ? C60 Cl5 Cl6 46.2(10) . 2_655 ? C60 Cl6 Cl6 52.8(10) . 2_655 ? C60 Cl6 Cl5 44.5(9) . 2_655 ? Cl6 Cl6 Cl5 74.7(13) 2_655 2_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.025 _refine_diff_density_min -1.364 _refine_diff_density_rms 0.260