#Supplementary Material (ESI) for Dalton Transactions #This journal is (C) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'M. Pilar Lamata' _publ_contact_author_email PLAMATA@UNIZAR.ES _publ_section_title ; Chiral pyridylamino-ruthenium(II) complexes: synthesis, structure and catalytic properties in Diels-Alder reactions ; loop_ _publ_author_name 'M. Pilar Lamata' 'Daniel Carmona' 'Ricardo Rodriguez' 'Fernando Viguri' data_compound_1a _database_code_depnum_ccdc_archive 'CCDC 678437' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H30 Cl N2 Ru, F6 Sb' _chemical_formula_sum 'C24 H30 Cl F6 N2 Ru Sb' _chemical_formula_weight 718.77 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.4680(11) _cell_length_b 10.7280(12) _cell_length_c 13.8827(16) _cell_angle_alpha 90.00 _cell_angle_beta 109.2470(10) _cell_angle_gamma 90.00 _cell_volume 1331.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7924 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.22 _exptl_crystal_description 'irregular block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 1.740 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6255 _exptl_absorpt_correction_T_max 0.7739 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within SAINT+ package, v. 6.01. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 16173 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.74 _reflns_number_total 6286 _reflns_number_gt 5924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.01 (Bruker AXS, 2000)' _computing_data_reduction 'SAINT+ v. 6.01 (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2001' _computing_publication_material 'XCIF program, SHELXTL v6.12, BrukerAXS' _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. All non-hydrogen atoms, except four F atoms in SbF6^-^, were refined with anisotropic displacement parameters. The sbF6^-^ was found to be disordered and refined with four F atoms in two positions. Complementary occupancy factors were refined for the two different geometries. The hydrogen atoms were included in calculated positions according to their geometry and refined riding on carbon atoms. The maximum electron residual was of 1.56 e/\%A^3^ close to the Sb atom and has no chemical sense. ; _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^)+(0.0773P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0011(3) _refine_ls_number_reflns 6286 _refine_ls_number_parameters 316 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1244 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.034 _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 Ru Ru 0.00069(4) 0.26051(4) 0.32512(3) 0.02982(12) Uani 1 1 d . . . Cl Cl 0.10415(18) 0.07257(15) 0.41131(13) 0.0411(3) Uani 1 1 d . . . N1 N -0.1583(5) 0.1380(5) 0.2326(4) 0.0376(11) Uani 1 1 d . . . N2 N 0.1061(5) 0.1987(5) 0.2166(4) 0.0313(10) Uani 1 1 d . . . H2N H 0.1540 0.1247 0.2435 0.038 Uiso 1 1 calc R . . C1 C -0.1112(7) 0.4411(6) 0.2770(5) 0.0390(13) Uani 1 1 d . . . C2 C 0.0461(8) 0.4581(6) 0.3156(6) 0.0477(17) Uani 1 1 d . . . H2 H 0.0941 0.4990 0.2741 0.057 Uiso 1 1 calc R . . C3 C 0.1337(8) 0.4164(7) 0.4136(6) 0.0510(18) Uani 1 1 d . . . H3 H 0.2388 0.4298 0.4366 0.061 Uiso 1 1 calc R . . C4 C 0.0662(8) 0.3546(7) 0.4782(5) 0.0496(17) Uani 1 1 d . . . C5 C -0.0884(8) 0.3365(7) 0.4381(5) 0.0458(16) Uani 1 1 d . . . H5 H -0.1374 0.2943 0.4783 0.055 Uiso 1 1 calc R . . C6 C -0.1741(7) 0.3788(6) 0.3398(4) 0.0383(13) Uani 1 1 d . . . H6 H -0.2789 0.3638 0.3161 0.046 Uiso 1 1 calc R . . C7 C -0.2016(11) 0.4930(8) 0.1739(6) 0.061(2) Uani 1 1 d . . . H7 H -0.1369 0.4883 0.1298 0.073 Uiso 1 1 calc R . . C8 C -0.2313(16) 0.6343(11) 0.1872(8) 0.098(4) Uani 1 1 d . . . H8A H -0.3394 0.6499 0.1631 0.147 Uiso 1 1 calc R . . H8B H -0.1840 0.6846 0.1473 0.147 Uiso 1 1 calc R . . H8C H -0.1893 0.6571 0.2594 0.147 Uiso 1 1 calc R . . C9 C -0.3316(12) 0.4245(12) 0.1247(8) 0.087(3) Uani 1 1 d . . . H9A H -0.3043 0.3458 0.0996 0.131 Uiso 1 1 calc R . . H9B H -0.3964 0.4729 0.0672 0.131 Uiso 1 1 calc R . . H9C H -0.3847 0.4070 0.1730 0.131 Uiso 1 1 calc R . . C10 C 0.1579(11) 0.3019(10) 0.5787(6) 0.082(3) Uani 1 1 d . . . H10A H 0.1261 0.3388 0.6328 0.124 Uiso 1 1 calc R . . H10B H 0.2637 0.3209 0.5912 0.124 Uiso 1 1 calc R . . H10C H 0.1442 0.2113 0.5781 0.124 Uiso 1 1 calc R . . C11 C -0.2673(8) 0.0873(7) 0.2582(7) 0.0535(18) Uani 1 1 d . . . H11 H -0.2804 0.1125 0.3203 0.064 Uiso 1 1 calc R . . C12 C -0.3631(7) -0.0004(8) 0.1992(7) 0.059(2) Uani 1 1 d . . . H12 H -0.4407 -0.0349 0.2201 0.071 Uiso 1 1 calc R . . C13 C -0.3450(9) -0.0360(9) 0.1123(8) 0.066(2) Uani 1 1 d . . . H13 H -0.4103 -0.0963 0.0703 0.080 Uiso 1 1 calc R . . C14 C -0.2296(8) 0.0153(8) 0.0826(6) 0.0570(19) Uani 1 1 d . . . H14 H -0.2159 -0.0097 0.0207 0.068 Uiso 1 1 calc R . . C15 C -0.1368(7) 0.1022(6) 0.1443(5) 0.0421(14) Uani 1 1 d . . . C16 C -0.0114(7) 0.1624(6) 0.1225(5) 0.0403(13) Uani 1 1 d . . . H16A H 0.0305 0.1042 0.0836 0.048 Uiso 1 1 calc R . . H16B H -0.0481 0.2372 0.0798 0.048 Uiso 1 1 calc R . . C17 C 0.2258(6) 0.2775(6) 0.1954(4) 0.0354(11) Uani 1 1 d . . . H17 H 0.1784 0.3582 0.1654 0.042 Uiso 1 1 calc R . . C18 C 0.2873(8) 0.2168(7) 0.1181(5) 0.0495(16) Uani 1 1 d . . . H18A H 0.3319 0.1360 0.1443 0.074 Uiso 1 1 calc R . . H18B H 0.3638 0.2709 0.1067 0.074 Uiso 1 1 calc R . . H18C H 0.2059 0.2044 0.0535 0.074 Uiso 1 1 calc R . . C19 C 0.3500(6) 0.3072(5) 0.2930(5) 0.0336(12) Uani 1 1 d . . . C20 C 0.4125(6) 0.2178(6) 0.3688(5) 0.0389(13) Uani 1 1 d . . . H20 H 0.3791 0.1338 0.3595 0.047 Uiso 1 1 calc R . . C21 C 0.5233(7) 0.2537(8) 0.4570(5) 0.0486(16) Uani 1 1 d . . . H21 H 0.5651 0.1925 0.5079 0.058 Uiso 1 1 calc R . . C22 C 0.5753(8) 0.3723(8) 0.4744(6) 0.0510(18) Uani 1 1 d . . . H22 H 0.6476 0.3949 0.5377 0.061 Uiso 1 1 calc R . . C23 C 0.5201(8) 0.4597(7) 0.3974(7) 0.057(2) Uani 1 1 d . . . H23 H 0.5603 0.5417 0.4061 0.068 Uiso 1 1 calc R . . C24 C 0.4072(7) 0.4291(6) 0.3080(6) 0.0471(16) Uani 1 1 d . . . H24 H 0.3684 0.4905 0.2568 0.057 Uiso 1 1 calc R . . F1A F 0.230(2) 0.7190(19) 0.3096(13) 0.096(5) Uiso 0.40 1 d P A 1 F2A F 0.248(2) 0.8443(19) 0.0654(14) 0.100(5) Uiso 0.40 1 d P A 1 F3A F 0.422(2) 0.734(2) 0.2182(15) 0.106(6) Uiso 0.40 1 d P A 1 F4A F 0.027(2) 0.8351(19) 0.1468(15) 0.108(5) Uiso 0.40 1 d P A 1 F1B F 0.1513(10) 0.7516(9) 0.2897(6) 0.070(2) Uiso 0.60 1 d P A 2 F2B F 0.3197(11) 0.8063(10) 0.0861(7) 0.077(3) Uiso 0.60 1 d P A 2 F3B F 0.4166(9) 0.7289(8) 0.2710(7) 0.063(2) Uiso 0.60 1 d P A 2 F4B F 0.0445(9) 0.8344(8) 0.0935(7) 0.063(2) Uiso 0.60 1 d P A 2 F5 F 0.2809(6) 0.9460(4) 0.2349(5) 0.0696(14) Uani 1 1 d . A . F6 F 0.1710(7) 0.6241(5) 0.1316(4) 0.0799(16) Uani 1 1 d . A . Sb Sb 0.22558(5) 0.78538(4) 0.18451(3) 0.04149(13) 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 Ru 0.02299(19) 0.0320(2) 0.0351(2) 0.00028(16) 0.01051(15) 0.00242(16) Cl 0.0389(8) 0.0412(8) 0.0444(8) 0.0108(6) 0.0154(6) 0.0057(6) N1 0.026(2) 0.035(3) 0.048(3) 0.001(2) 0.006(2) 0.001(2) N2 0.023(2) 0.033(2) 0.037(2) 0.0017(18) 0.0088(19) 0.0025(18) C1 0.036(3) 0.043(3) 0.037(3) -0.005(3) 0.012(3) 0.007(3) C2 0.048(4) 0.031(3) 0.073(5) -0.013(3) 0.033(4) -0.002(3) C3 0.034(3) 0.043(4) 0.070(5) -0.018(3) 0.010(3) 0.005(3) C4 0.045(4) 0.058(4) 0.041(3) -0.013(3) 0.009(3) 0.015(3) C5 0.044(4) 0.060(4) 0.035(3) -0.005(3) 0.015(3) 0.007(3) C6 0.027(3) 0.053(4) 0.035(3) 0.001(3) 0.010(2) 0.011(3) C7 0.088(6) 0.054(4) 0.041(4) 0.005(3) 0.021(4) 0.031(4) C8 0.146(11) 0.069(7) 0.078(7) 0.019(5) 0.034(7) 0.061(7) C9 0.079(7) 0.090(8) 0.084(7) 0.003(6) 0.016(6) 0.024(6) C10 0.089(6) 0.087(7) 0.048(4) -0.015(4) -0.008(4) 0.035(6) C11 0.032(3) 0.048(4) 0.079(5) 0.008(4) 0.016(3) -0.001(3) C12 0.025(3) 0.055(4) 0.087(6) 0.011(4) 0.004(3) -0.007(3) C13 0.038(4) 0.062(5) 0.087(6) -0.008(5) 0.005(4) -0.016(4) C14 0.042(4) 0.063(5) 0.052(4) -0.011(3) -0.003(3) 0.002(3) C15 0.032(3) 0.037(3) 0.048(4) 0.004(3) 0.000(3) 0.003(2) C16 0.034(3) 0.046(3) 0.041(3) -0.003(3) 0.012(3) -0.002(3) C17 0.029(2) 0.036(3) 0.046(3) 0.010(2) 0.018(2) 0.003(2) C18 0.043(4) 0.065(5) 0.047(4) 0.002(3) 0.024(3) 0.002(3) C19 0.024(2) 0.033(3) 0.047(3) 0.001(2) 0.017(2) 0.000(2) C20 0.028(3) 0.046(3) 0.042(3) 0.000(3) 0.010(2) -0.004(2) C21 0.032(3) 0.066(5) 0.051(3) -0.001(3) 0.017(3) -0.006(3) C22 0.030(3) 0.067(5) 0.060(4) -0.020(4) 0.019(3) -0.009(3) C23 0.039(4) 0.049(4) 0.094(6) -0.030(4) 0.037(4) -0.017(3) C24 0.035(3) 0.031(3) 0.081(5) 0.001(3) 0.027(3) -0.001(3) F5 0.087(4) 0.032(2) 0.095(4) -0.014(2) 0.038(3) -0.010(2) F6 0.105(4) 0.048(3) 0.077(3) -0.019(3) 0.016(3) -0.025(3) Sb 0.0466(2) 0.0316(2) 0.0428(2) 0.00055(15) 0.01000(17) -0.00628(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N1 2.090(5) . ? Ru C6 2.148(6) . ? Ru N2 2.167(5) . ? Ru C5 2.170(6) . ? Ru C2 2.176(7) . ? Ru C1 2.204(7) . ? Ru C3 2.207(7) . ? Ru C4 2.247(6) . ? Ru Cl 2.3841(16) . ? N1 C11 1.315(9) . ? N1 C15 1.363(9) . ? N2 C16 1.463(8) . ? N2 C17 1.519(7) . ? N2 H2N 0.9300 . ? C1 C6 1.380(9) . ? C1 C2 1.418(9) . ? C1 C7 1.511(10) . ? C2 C3 1.412(11) . ? C2 H2 0.9500 . ? C3 C4 1.425(12) . ? C3 H3 0.9500 . ? C4 C5 1.397(10) . ? C4 C10 1.491(10) . ? C5 C6 1.413(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C9 1.402(14) . ? C7 C8 1.564(13) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.374(11) . ? C11 H11 0.9500 . ? C12 C13 1.330(13) . ? C12 H12 0.9500 . ? C13 C14 1.401(12) . ? C13 H13 0.9500 . ? C14 C15 1.370(10) . ? C14 H14 0.9500 . ? C15 C16 1.468(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C19 1.507(8) . ? C17 C18 1.526(9) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.404(9) . ? C19 C20 1.403(9) . ? C20 C21 1.378(9) . ? C20 H20 0.9500 . ? C21 C22 1.357(11) . ? C21 H21 0.9500 . ? C22 C23 1.389(12) . ? C22 H22 0.9500 . ? C23 C24 1.384(11) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? F1A Sb 1.866(18) . ? F2A Sb 1.847(18) . ? F3A Sb 1.845(18) . ? F4A Sb 1.85(2) . ? F1B Sb 1.854(8) . ? F2B Sb 1.875(10) . ? F3B Sb 1.910(8) . ? F4B Sb 1.839(8) . ? F5 Sb 1.868(4) . ? F6 Sb 1.884(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru C6 90.5(2) . . ? N1 Ru N2 77.5(2) . . ? C6 Ru N2 142.4(2) . . ? N1 Ru C5 107.9(2) . . ? C6 Ru C5 38.2(2) . . ? N2 Ru C5 174.4(2) . . ? N1 Ru C2 133.8(3) . . ? C6 Ru C2 66.7(3) . . ? N2 Ru C2 96.3(2) . . ? C5 Ru C2 79.0(3) . . ? N1 Ru C1 101.0(2) . . ? C6 Ru C1 37.0(2) . . ? N2 Ru C1 110.1(2) . . ? C5 Ru C1 68.0(3) . . ? C2 Ru C1 37.8(3) . . ? N1 Ru C3 169.0(2) . . ? C6 Ru C3 79.4(3) . . ? N2 Ru C3 108.0(3) . . ? C5 Ru C3 66.4(3) . . ? C2 Ru C3 37.6(3) . . ? C1 Ru C3 68.4(3) . . ? N1 Ru C4 141.4(3) . . ? C6 Ru C4 68.0(2) . . ? N2 Ru C4 138.4(2) . . ? C5 Ru C4 36.8(3) . . ? C2 Ru C4 67.8(3) . . ? C1 Ru C4 81.2(2) . . ? C3 Ru C4 37.3(3) . . ? N1 Ru Cl 82.53(15) . . ? C6 Ru Cl 130.83(17) . . ? N2 Ru Cl 83.28(14) . . ? C5 Ru Cl 98.5(2) . . ? C2 Ru Cl 142.9(2) . . ? C1 Ru Cl 166.57(17) . . ? C3 Ru Cl 107.3(2) . . ? C4 Ru Cl 88.0(2) . . ? C11 N1 C15 119.3(6) . . ? C11 N1 Ru 124.4(5) . . ? C15 N1 Ru 116.1(4) . . ? C16 N2 C17 111.8(5) . . ? C16 N2 Ru 108.3(3) . . ? C17 N2 Ru 120.6(4) . . ? C16 N2 H2N 104.9 . . ? C17 N2 H2N 104.9 . . ? Ru N2 H2N 104.9 . . ? C6 C1 C2 116.2(6) . . ? C6 C1 C7 123.3(6) . . ? C2 C1 C7 120.4(7) . . ? C6 C1 Ru 69.3(4) . . ? C2 C1 Ru 70.1(4) . . ? C7 C1 Ru 132.6(5) . . ? C3 C2 C1 122.2(7) . . ? C3 C2 Ru 72.4(4) . . ? C1 C2 Ru 72.2(4) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? Ru C2 H2 129.0 . . ? C2 C3 C4 120.7(7) . . ? C2 C3 Ru 70.0(4) . . ? C4 C3 Ru 72.8(4) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? Ru C3 H3 130.1 . . ? C5 C4 C3 116.2(7) . . ? C5 C4 C10 122.0(8) . . ? C3 C4 C10 121.5(8) . . ? C5 C4 Ru 68.6(4) . . ? C3 C4 Ru 69.8(4) . . ? C10 C4 Ru 127.5(6) . . ? C4 C5 C6 122.2(7) . . ? C4 C5 Ru 74.6(4) . . ? C6 C5 Ru 70.1(3) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? Ru C5 H5 128.9 . . ? C1 C6 C5 122.4(6) . . ? C1 C6 Ru 73.7(3) . . ? C5 C6 Ru 71.7(4) . . ? C1 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? Ru C6 H6 128.0 . . ? C9 C7 C1 113.6(8) . . ? C9 C7 C8 113.7(9) . . ? C1 C7 C8 108.3(7) . . ? C9 C7 H7 106.9 . . ? C1 C7 H7 106.9 . . ? C8 C7 H7 106.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 123.0(8) . . ? N1 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C13 C12 C11 118.7(8) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 120.0(7) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 119.0(8) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? N1 C15 C14 119.9(7) . . ? N1 C15 C16 115.6(6) . . ? C14 C15 C16 124.4(7) . . ? N2 C16 C15 111.2(5) . . ? N2 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? N2 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C19 C17 N2 110.7(4) . . ? C19 C17 C18 110.9(5) . . ? N2 C17 C18 112.4(6) . . ? C19 C17 H17 107.5 . . ? N2 C17 H17 107.5 . . ? C18 C17 H17 107.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 118.6(6) . . ? C24 C19 C17 118.6(6) . . ? C20 C19 C17 122.8(5) . . ? C21 C20 C19 119.0(6) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C22 C21 C20 123.1(7) . . ? C22 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? C21 C22 C23 118.3(7) . . ? C21 C22 H22 120.9 . . ? C23 C22 H22 120.9 . . ? C24 C23 C22 120.9(7) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C19 120.0(7) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? F4B Sb F3A 153.2(7) . . ? F4B Sb F2A 69.1(6) . . ? F3A Sb F2A 85.7(9) . . ? F4B Sb F1B 95.0(4) . . ? F3A Sb F1B 110.7(7) . . ? F2A Sb F1B 163.3(7) . . ? F4B Sb F4A 25.3(6) . . ? F3A Sb F4A 178.3(9) . . ? F2A Sb F4A 93.0(9) . . ? F1B Sb F4A 70.6(7) . . ? F4B Sb F5 94.4(3) . . ? F3A Sb F5 92.5(7) . . ? F2A Sb F5 85.3(7) . . ? F1B Sb F5 91.0(3) . . ? F4A Sb F5 88.5(7) . . ? F4B Sb F1A 118.5(6) . . ? F3A Sb F1A 86.6(9) . . ? F2A Sb F1A 172.3(8) . . ? F1B Sb F1A 24.3(5) . . ? F4A Sb F1A 94.7(9) . . ? F5 Sb F1A 95.0(6) . . ? F4B Sb F2B 91.4(4) . . ? F3A Sb F2B 62.6(7) . . ? F2A Sb F2B 23.6(6) . . ? F1B Sb F2B 173.1(4) . . ? F4A Sb F2B 116.1(7) . . ? F5 Sb F2B 91.2(4) . . ? F1A Sb F2B 148.8(7) . . ? F4B Sb F6 85.5(3) . . ? F3A Sb F6 87.1(7) . . ? F2A Sb F6 93.6(7) . . ? F1B Sb F6 90.1(3) . . ? F4A Sb F6 91.8(7) . . ? F5 Sb F6 178.9(3) . . ? F1A Sb F6 86.0(6) . . ? F2B Sb F6 87.8(4) . . ? F4B Sb F3B 175.9(4) . . ? F3A Sb F3B 23.1(6) . . ? F2A Sb F3B 107.9(7) . . ? F1B Sb F3B 88.2(4) . . ? F4A Sb F3B 158.4(7) . . ? F5 Sb F3B 88.1(3) . . ? F1A Sb F3B 64.5(6) . . ? F2B Sb F3B 85.3(4) . . ? F6 Sb F3B 92.0(3) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.565 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.148 # Attachment 'Compd5a_revised.cif' data_compound_5a _database_code_depnum_ccdc_archive 'CCDC 678438' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H38 Cl N2 Ru, F6 Sb ' _chemical_formula_sum 'C26 H38 Cl F6 N2 Ru Sb' _chemical_formula_weight 750.85 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.9604(8) _cell_length_b 10.8946(7) _cell_length_c 12.1915(8) _cell_angle_alpha 90.00 _cell_angle_beta 116.7890(10) _cell_angle_gamma 90.00 _cell_volume 1418.10(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1290 _cell_measurement_theta_min 5 _cell_measurement_theta_max 21 _exptl_crystal_description 'irregular block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 1.637 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6439 _exptl_absorpt_correction_T_max 0.7207 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within SAINT+ package, v. 6.01. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 6991 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 26.50 _reflns_number_total 4478 _reflns_number_gt 4347 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.01 (Bruker AXS, 2000)' _computing_data_reduction 'SAINT+ v. 6.01 (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2001' _computing_publication_material 'XCIF program, SHELXTL v6.12, BrukerAXS' _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. All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms were found from difference Fourier maps and refined as free isotropic atoms or with positional parameters riding on carbon atoms. The maximum electron residual was of 0.54 e/\%A^3^ close to the Ru atom and has no chemical sense. ; _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^)+(0.0346P)^2^+1.2108P] 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 0.0010(3) _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 -0.01(2) _refine_ls_number_reflns 4478 _refine_ls_number_parameters 416 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.010 _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 Ru Ru 0.51825(3) 0.09447(3) 0.21526(3) 0.01850(9) Uani 1 1 d . . . Cl Cl 0.48034(10) 0.06835(11) 0.00643(9) 0.0293(3) Uani 1 1 d . . . N1 N 0.3931(3) 0.2411(4) 0.1466(3) 0.0214(8) Uani 1 1 d . . . N2 N 0.6345(3) 0.2434(4) 0.2106(3) 0.0196(8) Uani 1 1 d . . . H2N H 0.618(4) 0.247(5) 0.136(4) 0.018(11) Uiso 1 1 d . . . C1 C 0.4684(4) 0.0648(4) 0.3678(4) 0.0215(9) Uani 1 1 d . . . C2 C 0.5997(4) 0.0702(4) 0.4146(4) 0.0240(10) Uani 1 1 d . . . H2 H 0.6442 0.1230 0.4746 0.029 Uiso 1 1 d R . . C3 C 0.6637(4) -0.0098(5) 0.3682(4) 0.0228(9) Uani 1 1 d . . . H3 H 0.746(5) 0.002(5) 0.392(5) 0.027 Uiso 1 1 d . . . C4 C 0.5988(4) -0.0938(5) 0.2731(4) 0.0270(10) Uani 1 1 d . . . C5 C 0.4653(4) -0.0958(4) 0.2245(4) 0.0258(9) Uani 1 1 d . . . H5 H 0.421(5) -0.143(6) 0.160(5) 0.031 Uiso 1 1 d . . . C6 C 0.4018(4) -0.0206(4) 0.2711(4) 0.0222(9) Uani 1 1 d . . . H6 H 0.310(5) -0.019(5) 0.238(4) 0.027 Uiso 1 1 d . . . C7 C 0.3983(4) 0.1420(5) 0.4206(4) 0.0237(9) Uani 1 1 d . . . H7 H 0.312(5) 0.138(5) 0.362(5) 0.024(13) Uiso 1 1 d . . . C8 C 0.4133(5) 0.0799(5) 0.5398(4) 0.0348(11) Uani 1 1 d . . . H8A H 0.4999 0.0874 0.6018 0.055(18) Uiso 1 1 d R . . H8B H 0.3836 0.0015 0.5218 0.06(2) Uiso 1 1 d R . . H8C H 0.3606 0.1193 0.5713 0.035(14) Uiso 1 1 d R . . C9 C 0.4403(4) 0.2756(5) 0.4470(4) 0.0286(10) Uani 1 1 d . . . H9A H 0.5298 0.2801 0.5018 0.037(14) Uiso 1 1 d R . . H9B H 0.3890 0.3140 0.4796 0.047(17) Uiso 1 1 d R . . H9C H 0.4248 0.3165 0.3715 0.042(16) Uiso 1 1 d R . . C10 C 0.6638(5) -0.1744(5) 0.2195(5) 0.0370(12) Uani 1 1 d . . . H10A H 0.7618 -0.1525 0.2530 0.047(17) Uiso 1 1 d R . . H10B H 0.6277 -0.1575 0.1303 0.045(17) Uiso 1 1 d R . . H10C H 0.6549 -0.2559 0.2387 0.048(17) Uiso 1 1 d R . . C11 C 0.2675(4) 0.2294(5) 0.0843(4) 0.0266(10) Uani 1 1 d . . . H11 H 0.239(6) 0.142(6) 0.067(6) 0.046(17) Uiso 1 1 d . . . C12 C 0.1898(4) 0.3303(5) 0.0543(4) 0.0320(11) Uani 1 1 d . . . H12 H 0.099(6) 0.320(6) 0.017(5) 0.040(16) Uiso 1 1 d . . . C13 C 0.2414(4) 0.4468(5) 0.0876(4) 0.0315(11) Uani 1 1 d . . . H13 H 0.1908 0.5114 0.0712 0.029(14) Uiso 1 1 d R . . C14 C 0.3707(4) 0.4589(5) 0.1457(4) 0.0271(10) Uani 1 1 d . . . H14 H 0.414(5) 0.531(5) 0.168(4) 0.020(12) Uiso 1 1 d . . . C15 C 0.4442(4) 0.3536(4) 0.1737(4) 0.0218(9) Uani 1 1 d . . . C16 C 0.5854(4) 0.3565(4) 0.2403(4) 0.0213(9) Uani 1 1 d . . . H16A H 0.614(5) 0.428(6) 0.208(5) 0.041(15) Uiso 1 1 d . . . H16B H 0.619(4) 0.361(5) 0.337(4) 0.022(12) Uiso 1 1 d . . . C17 C 0.7751(4) 0.2300(4) 0.2797(4) 0.0210(9) Uani 1 1 d . . . H17 H 0.794(4) 0.216(5) 0.364(5) 0.025 Uiso 1 1 d . . . C18 C 0.8178(4) 0.1190(5) 0.2264(5) 0.0280(10) Uani 1 1 d . . . H18A H 0.8544 0.0648 0.2880 0.06(2) Uiso 1 1 d R . . H18B H 0.7478 0.0840 0.1543 0.018(11) Uiso 1 1 d R . . C19 C 0.9156(4) 0.1770(5) 0.1931(5) 0.0307(11) Uani 1 1 d . . . H19 H 0.966(5) 0.115(6) 0.176(5) 0.042(16) Uiso 1 1 d . . . C20 C 0.8451(5) 0.2589(6) 0.0807(4) 0.0347(11) Uani 1 1 d . . . H20A H 0.887(6) 0.275(8) 0.035(6) 0.07(2) Uiso 1 1 d . . . H20B H 0.767(5) 0.220(5) 0.013(5) 0.035(14) Uiso 1 1 d . . . C21 C 0.8084(5) 0.3729(5) 0.1350(5) 0.0306(11) Uani 1 1 d . . . H21A H 0.722(5) 0.381(5) 0.097(4) 0.021(12) Uiso 1 1 d . . . H21B H 0.847(5) 0.445(6) 0.125(5) 0.029(14) Uiso 1 1 d . . . C22 C 0.8563(4) 0.3394(5) 0.2713(4) 0.0258(10) Uani 1 1 d . . . C23 C 0.9811(4) 0.2698(5) 0.2990(4) 0.0291(10) Uani 1 1 d . . . C24 C 0.8731(5) 0.4476(5) 0.3561(5) 0.0341(12) Uani 1 1 d . . . H24A H 0.8807 0.4174 0.4345 0.11(3) Uiso 1 1 d R . . H24B H 0.8001 0.5005 0.3271 0.07(2) Uiso 1 1 d R . . H24C H 0.9443 0.4974 0.3660 0.030(14) Uiso 1 1 d R . . C25 C 1.0784(4) 0.3486(5) 0.2819(5) 0.0350(12) Uani 1 1 d . . . H25A H 1.1420 0.2992 0.2764 0.039(16) Uiso 1 1 d R . . H25B H 1.1211 0.4051 0.3528 0.050(18) Uiso 1 1 d R . . H25C H 1.0443 0.3997 0.2045 0.051(18) Uiso 1 1 d R . . C26 C 1.0456(5) 0.2122(6) 0.4257(5) 0.0391(13) Uani 1 1 d . . . H26A H 0.9914 0.1661 0.4487 0.044(17) Uiso 1 1 d R . . H26B H 1.1029 0.1558 0.4287 0.052(19) Uiso 1 1 d R . . H26C H 1.0918 0.2677 0.4920 0.07(2) Uiso 1 1 d R . . Sb Sb 0.88558(3) 0.26075(3) 0.72125(3) 0.02876(10) Uani 1 1 d . . . F1 F 1.0266(3) 0.3291(4) 0.7185(4) 0.0625(11) Uani 1 1 d . . . F2 F 0.7424(3) 0.1940(4) 0.7236(3) 0.0563(10) Uani 1 1 d . . . F3 F 0.7800(4) 0.3607(4) 0.5919(3) 0.0605(11) Uani 1 1 d . . . F4 F 0.9847(4) 0.1558(4) 0.8495(3) 0.0585(10) Uani 1 1 d . . . F5 F 0.8756(3) 0.1445(3) 0.6039(3) 0.0487(9) Uani 1 1 d . . . F6 F 0.8927(3) 0.3813(3) 0.8350(3) 0.0435(8) 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 Ru 0.01942(15) 0.01762(18) 0.01947(15) -0.00256(14) 0.00965(12) -0.00261(15) Cl 0.0339(5) 0.0331(7) 0.0229(5) -0.0080(4) 0.0147(4) -0.0065(5) N1 0.0206(16) 0.025(2) 0.0182(15) -0.0003(15) 0.0085(13) -0.0006(16) N2 0.0204(16) 0.021(2) 0.0191(17) 0.0019(15) 0.0105(14) 0.0013(16) C1 0.027(2) 0.019(3) 0.0219(19) 0.0029(16) 0.0135(17) -0.0017(17) C2 0.029(2) 0.022(3) 0.0193(19) 0.0031(17) 0.0091(17) -0.0015(19) C3 0.025(2) 0.020(2) 0.024(2) 0.0031(17) 0.0111(18) 0.0002(18) C4 0.032(2) 0.020(3) 0.034(2) -0.0007(19) 0.019(2) -0.0014(19) C5 0.033(2) 0.015(2) 0.032(2) -0.0055(19) 0.018(2) -0.0078(19) C6 0.025(2) 0.018(2) 0.027(2) 0.0021(18) 0.0155(18) -0.0062(18) C7 0.026(2) 0.024(2) 0.025(2) -0.0008(18) 0.0147(19) 0.0004(18) C8 0.049(3) 0.027(3) 0.041(3) 0.002(2) 0.031(2) 0.001(3) C9 0.041(2) 0.021(3) 0.032(2) -0.001(2) 0.024(2) 0.000(2) C10 0.049(3) 0.025(3) 0.043(3) -0.003(2) 0.026(3) 0.004(2) C11 0.020(2) 0.035(3) 0.023(2) -0.0040(19) 0.0081(17) 0.0004(19) C12 0.025(2) 0.044(3) 0.029(2) 0.002(2) 0.013(2) 0.002(2) C13 0.030(2) 0.036(3) 0.031(2) 0.009(2) 0.017(2) 0.013(2) C14 0.028(2) 0.028(3) 0.026(2) 0.009(2) 0.0134(19) 0.006(2) C15 0.025(2) 0.024(3) 0.020(2) 0.0046(17) 0.0132(17) 0.0018(18) C16 0.021(2) 0.017(2) 0.025(2) 0.0032(18) 0.0105(17) 0.0018(18) C17 0.0207(19) 0.020(3) 0.022(2) 0.0030(17) 0.0102(16) 0.0011(17) C18 0.023(2) 0.021(3) 0.043(3) -0.002(2) 0.018(2) 0.0000(18) C19 0.029(2) 0.031(3) 0.037(3) 0.000(2) 0.019(2) 0.005(2) C20 0.036(2) 0.040(3) 0.034(2) -0.002(3) 0.020(2) 0.003(3) C21 0.031(3) 0.028(3) 0.037(3) 0.007(2) 0.019(2) 0.005(2) C22 0.022(2) 0.025(3) 0.033(2) -0.0005(19) 0.0147(19) -0.0024(19) C23 0.024(2) 0.033(3) 0.034(2) -0.003(2) 0.0163(18) -0.003(2) C24 0.033(2) 0.029(3) 0.046(3) -0.017(2) 0.023(2) -0.011(2) C25 0.023(2) 0.034(3) 0.053(3) 0.005(2) 0.021(2) 0.002(2) C26 0.031(2) 0.045(4) 0.039(3) 0.010(2) 0.014(2) 0.005(2) Sb 0.02154(14) 0.03127(19) 0.02938(16) -0.00095(14) 0.00786(12) 0.00291(14) F1 0.048(2) 0.070(3) 0.085(3) -0.021(2) 0.044(2) -0.0190(19) F2 0.0398(18) 0.073(3) 0.058(2) -0.0071(19) 0.0229(16) -0.0206(18) F3 0.062(2) 0.071(3) 0.0431(19) 0.0233(18) 0.0184(17) 0.028(2) F4 0.063(2) 0.039(2) 0.0419(19) 0.0042(16) -0.0036(17) 0.0130(18) F5 0.0406(17) 0.054(2) 0.0433(18) -0.0186(16) 0.0120(14) 0.0035(15) F6 0.0390(16) 0.039(2) 0.0446(17) -0.0111(14) 0.0122(14) 0.0069(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N1 2.089(4) . ? Ru N2 2.154(4) . ? Ru C5 2.185(5) . ? Ru C2 2.189(4) . ? Ru C6 2.198(4) . ? Ru C3 2.207(4) . ? Ru C1 2.218(4) . ? Ru C4 2.241(5) . ? Ru Cl 2.3934(10) . ? N1 C15 1.343(6) . ? N1 C11 1.350(5) . ? N2 C16 1.478(6) . ? N2 C17 1.510(5) . ? N2 H2N 0.84(5) . ? C1 C2 1.410(6) . ? C1 C6 1.430(6) . ? C1 C7 1.520(6) . ? C2 C3 1.434(6) . ? C2 H2 0.8935 . ? C3 C4 1.404(7) . ? C3 H3 0.90(5) . ? C4 C5 1.432(6) . ? C4 C10 1.503(7) . ? C5 C6 1.400(7) . ? C5 H5 0.89(6) . ? C6 H6 0.99(5) . ? C7 C9 1.526(7) . ? C7 C8 1.537(6) . ? C7 H7 0.96(5) . ? C8 H8A 0.9720 . ? C8 H8B 0.9135 . ? C8 H8C 0.9733 . ? C9 H9A 0.9744 . ? C9 H9B 0.9652 . ? C9 H9C 0.9622 . ? C10 H10A 1.0798 . ? C10 H10B 0.9899 . ? C10 H10C 0.9372 . ? C11 C12 1.378(7) . ? C11 H11 1.00(7) . ? C12 C13 1.389(8) . ? C12 H12 0.97(6) . ? C13 C14 1.387(7) . ? C13 H13 0.8904 . ? C14 C15 1.391(7) . ? C14 H14 0.91(6) . ? C15 C16 1.509(6) . ? C16 H16A 0.99(6) . ? C16 H16B 1.06(5) . ? C17 C18 1.563(6) . ? C17 C22 1.570(6) . ? C17 H17 0.96(5) . ? C18 C19 1.536(7) . ? C18 H18A 0.8993 . ? C18 H18B 0.9775 . ? C19 C20 1.531(7) . ? C19 C23 1.546(7) . ? C19 H19 0.99(6) . ? C20 C21 1.560(8) . ? C20 H20A 0.92(7) . ? C20 H20B 1.02(6) . ? C21 C22 1.538(7) . ? C21 H21A 0.92(5) . ? C21 H21B 0.95(6) . ? C22 C24 1.521(7) . ? C22 C23 1.569(6) . ? C23 C26 1.517(7) . ? C23 C25 1.534(7) . ? C24 H24A 0.9756 . ? C24 H24B 0.9703 . ? C24 H24C 0.9703 . ? C25 H25A 0.9581 . ? C25 H25B 0.9948 . ? C25 H25C 1.0109 . ? C26 H26A 0.9570 . ? C26 H26B 0.9092 . ? C26 H26C 0.9588 . ? Sb F1 1.857(3) . ? Sb F3 1.863(3) . ? Sb F4 1.868(3) . ? Sb F2 1.873(3) . ? Sb F5 1.874(3) . ? Sb F6 1.884(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru N2 76.57(14) . . ? N1 Ru C5 125.03(16) . . ? N2 Ru C5 157.16(15) . . ? N1 Ru C2 114.67(15) . . ? N2 Ru C2 98.67(15) . . ? C5 Ru C2 79.75(18) . . ? N1 Ru C6 96.92(16) . . ? N2 Ru C6 160.80(15) . . ? C5 Ru C6 37.24(17) . . ? C2 Ru C6 67.29(16) . . ? N1 Ru C3 151.89(15) . . ? N2 Ru C3 97.90(15) . . ? C5 Ru C3 66.71(18) . . ? C2 Ru C3 38.08(17) . . ? C6 Ru C3 79.24(17) . . ? N1 Ru C1 91.86(15) . . ? N2 Ru C1 123.52(15) . . ? C5 Ru C1 67.95(16) . . ? C2 Ru C1 37.31(16) . . ? C6 Ru C1 37.77(16) . . ? C3 Ru C1 67.93(16) . . ? N1 Ru C4 162.75(15) . . ? N2 Ru C4 120.45(15) . . ? C5 Ru C4 37.73(17) . . ? C2 Ru C4 68.08(17) . . ? C6 Ru C4 67.87(17) . . ? C3 Ru C4 36.81(17) . . ? C1 Ru C4 80.96(16) . . ? N1 Ru Cl 84.64(9) . . ? N2 Ru Cl 82.93(10) . . ? C5 Ru Cl 91.26(13) . . ? C2 Ru Cl 160.54(13) . . ? C6 Ru Cl 114.78(12) . . ? C3 Ru Cl 122.46(12) . . ? C1 Ru Cl 151.78(12) . . ? C4 Ru Cl 94.26(12) . . ? C15 N1 C11 119.5(4) . . ? C15 N1 Ru 115.8(3) . . ? C11 N1 Ru 124.6(3) . . ? C16 N2 C17 114.1(3) . . ? C16 N2 Ru 106.8(2) . . ? C17 N2 Ru 118.8(3) . . ? C16 N2 H2N 107(4) . . ? C17 N2 H2N 106(3) . . ? Ru N2 H2N 103(3) . . ? C2 C1 C6 117.8(4) . . ? C2 C1 C7 122.1(4) . . ? C6 C1 C7 120.0(4) . . ? C2 C1 Ru 70.2(2) . . ? C6 C1 Ru 70.4(2) . . ? C7 C1 Ru 133.1(3) . . ? C1 C2 C3 120.7(4) . . ? C1 C2 Ru 72.4(2) . . ? C3 C2 Ru 71.6(2) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 119.1 . . ? Ru C2 H2 129.3 . . ? C4 C3 C2 121.8(4) . . ? C4 C3 Ru 72.9(3) . . ? C2 C3 Ru 70.3(2) . . ? C4 C3 H3 118(3) . . ? C2 C3 H3 119(4) . . ? Ru C3 H3 122(4) . . ? C3 C4 C5 116.7(4) . . ? C3 C4 C10 122.5(4) . . ? C5 C4 C10 120.7(4) . . ? C3 C4 Ru 70.3(3) . . ? C5 C4 Ru 69.0(3) . . ? C10 C4 Ru 129.1(4) . . ? C6 C5 C4 122.1(4) . . ? C6 C5 Ru 71.9(3) . . ? C4 C5 Ru 73.3(3) . . ? C6 C5 H5 119(3) . . ? C4 C5 H5 119(3) . . ? Ru C5 H5 125(4) . . ? C5 C6 C1 120.9(4) . . ? C5 C6 Ru 70.9(3) . . ? C1 C6 Ru 71.9(2) . . ? C5 C6 H6 124(3) . . ? C1 C6 H6 116(3) . . ? Ru C6 H6 128(3) . . ? C1 C7 C9 115.1(4) . . ? C1 C7 C8 107.7(4) . . ? C9 C7 C8 109.5(4) . . ? C1 C7 H7 106(3) . . ? C9 C7 H7 110(3) . . ? C8 C7 H7 108(3) . . ? C7 C8 H8A 109.1 . . ? C7 C8 H8B 108.5 . . ? H8A C8 H8B 115.3 . . ? C7 C8 H8C 111.0 . . ? H8A C8 H8C 108.0 . . ? H8B C8 H8C 104.8 . . ? C7 C9 H9A 110.4 . . ? C7 C9 H9B 106.9 . . ? H9A C9 H9B 113.6 . . ? C7 C9 H9C 109.7 . . ? H9A C9 H9C 108.2 . . ? H9B C9 H9C 108.0 . . ? C4 C10 H10A 113.1 . . ? C4 C10 H10B 108.3 . . ? H10A C10 H10B 103.7 . . ? C4 C10 H10C 107.8 . . ? H10A C10 H10C 110.0 . . ? H10B C10 H10C 114.1 . . ? N1 C11 C12 121.4(5) . . ? N1 C11 H11 113(4) . . ? C12 C11 H11 125(4) . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12 120(4) . . ? C13 C12 H12 120(4) . . ? C14 C13 C12 118.8(5) . . ? C14 C13 H13 121.8 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 118.9(5) . . ? C13 C14 H14 126(3) . . ? C15 C14 H14 115(3) . . ? N1 C15 C14 121.7(4) . . ? N1 C15 C16 115.2(4) . . ? C14 C15 C16 123.1(4) . . ? N2 C16 C15 108.8(4) . . ? N2 C16 H16A 108(4) . . ? C15 C16 H16A 108(3) . . ? N2 C16 H16B 108(3) . . ? C15 C16 H16B 112(3) . . ? H16A C16 H16B 112(4) . . ? N2 C17 C18 109.5(4) . . ? N2 C17 C22 117.2(4) . . ? C18 C17 C22 103.4(3) . . ? N2 C17 H17 106(3) . . ? C18 C17 H17 111(3) . . ? C22 C17 H17 110(3) . . ? C19 C18 C17 102.8(4) . . ? C19 C18 H18A 110.4 . . ? C17 C18 H18A 106.7 . . ? C19 C18 H18B 111.7 . . ? C17 C18 H18B 111.6 . . ? H18A C18 H18B 113.1 . . ? C20 C19 C18 107.3(4) . . ? C20 C19 C23 103.5(5) . . ? C18 C19 C23 102.0(4) . . ? C20 C19 H19 111(3) . . ? C18 C19 H19 113(4) . . ? C23 C19 H19 119(3) . . ? C19 C20 C21 103.4(4) . . ? C19 C20 H20A 115(5) . . ? C21 C20 H20A 116(6) . . ? C19 C20 H20B 115(3) . . ? C21 C20 H20B 110(3) . . ? H20A C20 H20B 98(5) . . ? C22 C21 C20 103.3(4) . . ? C22 C21 H21A 110(3) . . ? C20 C21 H21A 109(3) . . ? C22 C21 H21B 112(3) . . ? C20 C21 H21B 111(3) . . ? H21A C21 H21B 111(5) . . ? C24 C22 C21 114.9(5) . . ? C24 C22 C23 114.0(4) . . ? C21 C22 C23 101.7(4) . . ? C24 C22 C17 116.1(4) . . ? C21 C22 C17 108.1(4) . . ? C23 C22 C17 100.1(4) . . ? C26 C23 C25 107.5(4) . . ? C26 C23 C19 114.4(5) . . ? C25 C23 C19 112.5(4) . . ? C26 C23 C22 114.7(4) . . ? C25 C23 C22 114.0(5) . . ? C19 C23 C22 93.5(3) . . ? C22 C24 H24A 109.2 . . ? C22 C24 H24B 113.0 . . ? H24A C24 H24B 103.2 . . ? C22 C24 H24C 111.0 . . ? H24A C24 H24C 112.2 . . ? H24B C24 H24C 108.0 . . ? C23 C25 H25A 111.7 . . ? C23 C25 H25B 110.7 . . ? H25A C25 H25B 107.2 . . ? C23 C25 H25C 115.1 . . ? H25A C25 H25C 104.0 . . ? H25B C25 H25C 107.7 . . ? C23 C26 H26A 114.5 . . ? C23 C26 H26B 110.4 . . ? H26A C26 H26B 103.4 . . ? C23 C26 H26C 115.6 . . ? H26A C26 H26C 107.1 . . ? H26B C26 H26C 104.8 . . ? F1 Sb F3 91.4(2) . . ? F1 Sb F4 91.2(2) . . ? F3 Sb F4 177.2(2) . . ? F1 Sb F2 179.2(2) . . ? F3 Sb F2 87.94(18) . . ? F4 Sb F2 89.40(19) . . ? F1 Sb F5 90.16(17) . . ? F3 Sb F5 87.89(17) . . ? F4 Sb F5 91.34(17) . . ? F2 Sb F5 90.32(17) . . ? F1 Sb F6 89.62(16) . . ? F3 Sb F6 90.23(17) . . ? F4 Sb F6 90.55(16) . . ? F2 Sb F6 89.88(16) . . ? F5 Sb F6 178.10(17) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.541 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.073 # Attachment 'Compd12a.cif' data_compound_12a _database_code_depnum_ccdc_archive 'CCDC 678439' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H40 N2 O Ru, C4 H10 O, 2(F6 Sb), C H2 Cl2' _chemical_formula_sum 'C31 H52 Cl2 F12 N2 O2 Ru Sb2' _chemical_formula_weight 1128.22 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 212121' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.395(3) _cell_length_b 11.073(3) _cell_length_c 36.007(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4144.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3337 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 21.19 _exptl_crystal_description 'irregular lamina' _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 1.867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.813 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within SAINT+ package, v. 6.01. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 27547 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.1368 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.56 _reflns_number_total 9745 _reflns_number_gt 6439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.01 (Bruker AXS, 2000)' _computing_data_reduction 'SAINT+ v. 6.01 (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP program, SHELXTL v6.10, Bruker2000' _computing_publication_material 'XCIF program, SHELXTLv6.10, BrukerAXS' _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. All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms were included in calculated positions and refined riding on carbon atoms. In the final steps of the refinement the hydrogen atoms of the coordinated water molecule were included in the model in the positions estimated using the CALC-OH program and refined riding on oxygen atoms. The maximum electron residual was of 1.33 e/\%A^3^ close to the Ru atom and has no chemical sense. ; _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.038(19) _refine_ls_number_reflns 9745 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0591 _refine_ls_goodness_of_fit_ref 0.783 _refine_ls_restrained_S_all 0.783 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.93148(5) 0.79426(5) 0.861603(14) 0.02491(13) Uani 1 1 d . . . O1 O 0.7733(4) 0.8977(4) 0.84148(11) 0.0322(13) Uani 1 1 d . . . H1O1 H 0.6978 0.8907 0.8504 0.039 Uiso 1 1 d R . . H2O1 H 0.7738 0.9598 0.8276 0.039 Uiso 1 1 d R . . N1 N 0.7995(6) 0.6826(4) 0.88377(13) 0.0263(14) Uani 1 1 d . . . N2 N 0.8770(5) 0.8838(4) 0.91172(14) 0.0234(14) Uani 1 1 d . . . H2N H 0.7979 0.9196 0.9067 0.028 Uiso 1 1 calc R . . C1 C 1.0710(7) 0.6496(6) 0.8630(2) 0.0317(17) Uani 1 1 d . . . C2 C 1.1281(6) 0.7542(5) 0.87638(19) 0.0278(18) Uani 1 1 d . . . H2 H 1.1677 0.7544 0.9001 0.033 Uiso 1 1 calc R . . C3 C 1.1272(6) 0.8617(6) 0.85440(19) 0.0284(17) Uani 1 1 d . . . H3 H 1.1683 0.9321 0.8637 0.034 Uiso 1 1 calc R . . C4 C 1.0688(7) 0.8662(6) 0.82036(17) 0.0275(15) Uani 1 1 d . . . C5 C 1.0109(6) 0.7604(6) 0.80686(18) 0.033(2) Uani 1 1 d . . . H5 H 0.9691 0.7619 0.7834 0.040 Uiso 1 1 calc R . . C6 C 1.0136(6) 0.6545(6) 0.82692(19) 0.0339(19) Uani 1 1 d . . . H6 H 0.9767 0.5836 0.8166 0.041 Uiso 1 1 calc R . . C7 C 1.0732(8) 0.5298(5) 0.8829(2) 0.0374(19) Uani 1 1 d . . . H7 H 0.9837 0.4966 0.8826 0.045 Uiso 1 1 calc R . . C8 C 1.1604(7) 0.4391(6) 0.8630(2) 0.062(3) Uani 1 1 d . . . H8A H 1.2501 0.4659 0.8648 0.093 Uiso 1 1 calc R . . H8B H 1.1355 0.4337 0.8368 0.093 Uiso 1 1 calc R . . H8C H 1.1515 0.3595 0.8747 0.093 Uiso 1 1 calc R . . C9 C 1.1158(7) 0.5401(6) 0.9236(2) 0.046(2) Uani 1 1 d . . . H9A H 1.2047 0.5693 0.9247 0.069 Uiso 1 1 calc R . . H9B H 1.1104 0.4606 0.9355 0.069 Uiso 1 1 calc R . . H9C H 1.0594 0.5970 0.9367 0.069 Uiso 1 1 calc R . . C10 C 1.0613(7) 0.9812(5) 0.79765(18) 0.0369(18) Uani 1 1 d . . . H10A H 1.0663 1.0512 0.8142 0.055 Uiso 1 1 calc R . . H10B H 0.9798 0.9832 0.7840 0.055 Uiso 1 1 calc R . . H10C H 1.1331 0.9836 0.7800 0.055 Uiso 1 1 calc R . . C11 C 0.7328(6) 0.5936(6) 0.86561(19) 0.0311(18) Uani 1 1 d . . . H11 H 0.7372 0.5926 0.8393 0.037 Uiso 1 1 calc R . . C12 C 0.6608(7) 0.5065(6) 0.8823(2) 0.0329(19) Uani 1 1 d . . . H12 H 0.6189 0.4455 0.8683 0.040 Uiso 1 1 calc R . . C13 C 0.6509(7) 0.5102(6) 0.9206(2) 0.033(2) Uani 1 1 d . . . H13 H 0.6011 0.4510 0.9332 0.040 Uiso 1 1 calc R . . C14 C 0.7122(6) 0.5984(5) 0.94072(19) 0.0281(17) Uani 1 1 d . . . H14 H 0.7076 0.6010 0.9671 0.034 Uiso 1 1 calc R . . C15 C 0.7822(6) 0.6849(5) 0.92046(17) 0.0217(16) Uani 1 1 d . . . C16 C 0.8500(6) 0.7886(5) 0.93935(16) 0.0255(16) Uani 1 1 d . . . H16A H 0.7952 0.8214 0.9594 0.031 Uiso 1 1 calc R . . H16B H 0.9316 0.7600 0.9505 0.031 Uiso 1 1 calc R . . C17 C 0.9586(6) 0.9814(5) 0.92743(16) 0.0205(16) Uani 1 1 d . . . H17 H 1.0465 0.9474 0.9318 0.025 Uiso 1 1 calc R . . C18 C 0.9717(7) 1.0887(5) 0.89908(17) 0.038(2) Uani 1 1 d . . . H18A H 1.0603 1.0937 0.8891 0.046 Uiso 1 1 calc R . . H18B H 0.9107 1.0793 0.8782 0.046 Uiso 1 1 calc R . . C19 C 0.9398(6) 1.1987(6) 0.92190(16) 0.0263(15) Uani 1 1 d . . . H19 H 0.9729 1.2763 0.9115 0.032 Uiso 1 1 calc R . . C20 C 0.7933(6) 1.1964(6) 0.92871(18) 0.0347(18) Uani 1 1 d . . . H20A H 0.7624 1.2744 0.9388 0.042 Uiso 1 1 calc R . . H20B H 0.7456 1.1776 0.9056 0.042 Uiso 1 1 calc R . . C21 C 0.7797(6) 1.0957(5) 0.95712(18) 0.0294(18) Uani 1 1 d . . . H21A H 0.7234 1.0306 0.9475 0.035 Uiso 1 1 calc R . . H21B H 0.7427 1.1269 0.9806 0.035 Uiso 1 1 calc R . . C22 C 0.9166(7) 1.0488(5) 0.96336(17) 0.0220(16) Uani 1 1 d . . . C23 C 0.9940(6) 1.1661(6) 0.95957(18) 0.0260(18) Uani 1 1 d . . . C24 C 0.9356(8) 0.9815(5) 0.99957(16) 0.040(2) Uani 1 1 d . . . H24A H 1.0202 0.9424 0.9995 0.060 Uiso 1 1 calc R . . H24B H 0.8684 0.9202 1.0023 0.060 Uiso 1 1 calc R . . H24C H 0.9306 1.0386 1.0203 0.060 Uiso 1 1 calc R . . C25 C 0.9652(6) 1.2584(5) 0.98930(17) 0.035(2) Uani 1 1 d . . . H25A H 1.0001 1.3369 0.9819 0.053 Uiso 1 1 calc R . . H25B H 1.0048 1.2331 1.0127 0.053 Uiso 1 1 calc R . . H25C H 0.8719 1.2650 0.9926 0.053 Uiso 1 1 calc R . . C26 C 1.1394(6) 1.1496(6) 0.9597(2) 0.040(2) Uani 1 1 d . . . H26A H 1.1644 1.0955 0.9394 0.060 Uiso 1 1 calc R . . H26B H 1.1663 1.1145 0.9835 0.060 Uiso 1 1 calc R . . H26C H 1.1812 1.2282 0.9564 0.060 Uiso 1 1 calc R . . Sb1 Sb 0.80547(5) 0.29161(4) 0.796897(13) 0.03047(12) Uani 1 1 d . . . F1 F 0.9755(3) 0.2666(3) 0.78384(10) 0.0440(12) Uani 1 1 d . . . F2 F 0.6366(3) 0.3155(3) 0.81000(10) 0.0453(12) Uani 1 1 d . . . F3 F 0.7580(4) 0.2635(3) 0.74845(10) 0.0433(12) Uani 1 1 d . . . F4 F 0.8551(4) 0.3182(3) 0.84549(10) 0.0480(12) Uani 1 1 d . . . F5 F 0.7874(4) 0.1275(3) 0.80793(11) 0.0490(12) Uani 1 1 d . . . F6 F 0.8215(4) 0.4550(3) 0.78703(10) 0.0421(11) Uani 1 1 d . . . Sb2 Sb 0.43305(5) 0.85782(4) 0.945275(13) 0.02643(11) Uani 1 1 d . . . F7 F 0.4154(4) 0.7085(3) 0.92277(10) 0.0416(10) Uani 1 1 d . . . F8 F 0.4492(5) 1.0061(3) 0.96687(12) 0.0552(13) Uani 1 1 d . . . F9 F 0.5782(4) 0.8874(3) 0.91568(10) 0.0372(10) Uani 1 1 d . . . F10 F 0.2875(4) 0.8255(3) 0.97293(11) 0.0509(13) Uani 1 1 d . . . F11 F 0.5378(4) 0.7924(4) 0.98168(9) 0.0453(11) Uani 1 1 d . . . F12 F 0.3335(4) 0.9263(3) 0.90821(11) 0.0383(11) Uani 1 1 d . . . O2 O 0.3998(4) 0.2901(5) 0.69771(13) 0.0446(14) Uani 1 1 d . . . C27 C 0.4271(8) 0.3234(9) 0.7354(2) 0.077(3) Uani 1 1 d . . . H27A H 0.4862 0.3936 0.7359 0.092 Uiso 1 1 calc R . . H27B H 0.4693 0.2554 0.7484 0.092 Uiso 1 1 calc R . . C28 C 0.3054(8) 0.3545(8) 0.75413(19) 0.071(3) Uani 1 1 d . . . H28B H 0.2657 0.4236 0.7416 0.106 Uiso 1 1 calc R . . H28A H 0.3228 0.3753 0.7801 0.106 Uiso 1 1 calc R . . H28C H 0.2469 0.2852 0.7531 0.106 Uiso 1 1 calc R . . C29 C 0.5125(7) 0.2578(7) 0.6779(2) 0.057(3) Uani 1 1 d . . . H29B H 0.5798 0.3194 0.6825 0.069 Uiso 1 1 calc R . . H29A H 0.4932 0.2580 0.6509 0.069 Uiso 1 1 calc R . . C30 C 0.5629(8) 0.1377(7) 0.6885(2) 0.078(3) Uani 1 1 d . . . H30A H 0.5947 0.1405 0.7141 0.118 Uiso 1 1 calc R . . H30B H 0.6334 0.1153 0.6718 0.118 Uiso 1 1 calc R . . H30C H 0.4939 0.0776 0.6866 0.118 Uiso 1 1 calc R . . Cl1 Cl 0.4334(3) 0.2415(2) 0.89558(7) 0.0930(9) Uani 1 1 d . . . Cl2 Cl 0.3642(3) 0.1145(3) 0.82942(9) 0.1313(14) Uani 1 1 d . . . C31 C 0.4805(8) 0.1343(8) 0.8629(2) 0.075(3) Uani 1 1 d . . . H31A H 0.5616 0.1605 0.8510 0.090 Uiso 1 1 calc R . . H31B H 0.4968 0.0563 0.8755 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0227(3) 0.0282(3) 0.0239(3) -0.0037(3) 0.0014(3) -0.0027(3) O1 0.026(3) 0.041(3) 0.030(3) 0.015(2) 0.008(2) 0.002(2) N1 0.056(4) 0.009(3) 0.014(3) -0.003(2) 0.000(3) 0.010(3) N2 0.026(3) 0.018(3) 0.026(3) 0.002(3) -0.001(3) -0.003(3) C1 0.022(4) 0.020(4) 0.053(5) -0.007(4) -0.002(4) 0.000(4) C2 0.023(4) 0.032(5) 0.029(4) -0.009(3) 0.008(3) 0.000(3) C3 0.011(4) 0.032(4) 0.043(5) -0.002(4) 0.006(3) -0.009(3) C4 0.023(4) 0.033(4) 0.027(4) -0.004(3) 0.006(4) -0.011(4) C5 0.034(5) 0.046(5) 0.020(4) -0.001(4) 0.010(3) -0.004(4) C6 0.033(4) 0.032(5) 0.037(4) -0.017(4) 0.012(4) -0.012(4) C7 0.035(5) 0.024(4) 0.053(5) -0.005(4) 0.020(5) -0.002(4) C8 0.060(6) 0.037(5) 0.091(7) 0.017(5) 0.023(6) 0.000(5) C9 0.042(5) 0.028(5) 0.067(6) 0.014(4) 0.002(5) -0.010(4) C10 0.037(5) 0.043(4) 0.030(4) 0.000(4) 0.014(5) 0.000(4) C11 0.035(5) 0.029(4) 0.029(4) -0.001(4) 0.006(4) 0.005(4) C12 0.027(5) 0.031(4) 0.041(5) 0.001(4) 0.001(4) -0.007(3) C13 0.026(5) 0.025(4) 0.048(5) -0.005(4) 0.014(4) 0.002(3) C14 0.033(4) 0.021(4) 0.030(4) -0.005(3) 0.003(4) 0.003(3) C15 0.020(4) 0.020(4) 0.026(4) -0.001(3) -0.001(3) 0.005(3) C16 0.029(4) 0.027(4) 0.021(3) -0.001(4) -0.003(3) 0.000(4) C17 0.018(4) 0.018(4) 0.025(4) -0.001(3) 0.002(3) -0.004(3) C18 0.060(6) 0.030(4) 0.025(4) 0.002(3) 0.010(4) -0.009(4) C19 0.026(4) 0.019(3) 0.033(4) -0.004(3) -0.005(4) -0.002(4) C20 0.031(4) 0.024(4) 0.049(5) 0.010(4) -0.013(4) 0.001(4) C21 0.031(5) 0.027(4) 0.031(4) -0.006(3) 0.009(4) -0.002(4) C22 0.032(5) 0.015(4) 0.019(3) -0.005(3) -0.003(4) 0.001(4) C23 0.024(4) 0.026(5) 0.028(4) -0.006(3) 0.002(3) -0.003(3) C24 0.058(5) 0.040(4) 0.022(4) 0.003(3) 0.000(5) -0.021(5) C25 0.035(5) 0.033(4) 0.039(4) -0.006(4) 0.008(4) -0.006(4) C26 0.023(4) 0.046(5) 0.050(5) 0.001(4) -0.001(4) -0.007(4) Sb1 0.0372(3) 0.0300(3) 0.0242(2) 0.0003(3) 0.0026(3) -0.0021(3) F1 0.035(3) 0.051(3) 0.045(3) 0.000(2) 0.003(2) -0.005(2) F2 0.043(3) 0.042(3) 0.051(3) 0.003(2) 0.012(2) 0.002(2) F3 0.045(3) 0.054(3) 0.031(2) -0.013(2) 0.000(2) -0.011(2) F4 0.064(3) 0.047(3) 0.032(2) -0.006(2) -0.009(2) 0.002(2) F5 0.055(3) 0.040(3) 0.053(3) 0.002(2) 0.009(3) 0.005(2) F6 0.054(3) 0.038(2) 0.034(2) 0.0010(19) -0.002(2) -0.006(2) Sb2 0.0260(3) 0.0257(3) 0.0277(2) 0.0003(2) -0.0015(3) -0.0010(3) F7 0.032(2) 0.037(2) 0.056(3) -0.016(2) -0.004(2) -0.003(2) F8 0.057(3) 0.034(3) 0.075(3) -0.020(2) -0.019(3) 0.010(3) F9 0.027(2) 0.039(2) 0.046(3) 0.0015(19) 0.003(2) -0.002(2) F10 0.041(3) 0.058(3) 0.054(3) 0.006(2) 0.025(2) 0.003(2) F11 0.052(3) 0.051(3) 0.033(2) 0.011(2) -0.013(2) 0.007(3) F12 0.035(3) 0.035(2) 0.045(3) 0.007(2) -0.015(2) -0.008(2) O2 0.043(3) 0.057(3) 0.034(3) -0.009(3) 0.000(3) 0.016(3) C27 0.042(5) 0.135(9) 0.052(6) -0.011(6) -0.002(6) 0.035(7) C28 0.064(6) 0.112(8) 0.036(5) 0.000(5) -0.003(5) 0.004(7) C29 0.044(6) 0.066(7) 0.062(6) -0.019(5) -0.011(5) 0.003(5) C30 0.052(6) 0.072(6) 0.111(8) -0.028(6) -0.030(7) 0.024(6) Cl1 0.0669(18) 0.098(2) 0.114(2) 0.0166(17) 0.014(2) -0.0154(18) Cl2 0.144(3) 0.127(3) 0.123(3) 0.070(2) -0.072(2) -0.087(2) C31 0.078(7) 0.086(7) 0.060(6) 0.036(6) -0.022(6) -0.022(6) _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 Ru N1 2.012(6) . ? Ru N2 2.136(5) . ? Ru O1 2.131(4) . ? Ru C2 2.158(6) . ? Ru C6 2.164(6) . ? Ru C1 2.162(7) . ? Ru C5 2.170(6) . ? Ru C3 2.183(6) . ? Ru C4 2.208(7) . ? O1 H1O1 0.8523 . ? O1 H2O1 0.8495 . ? N1 C15 1.334(7) . ? N1 C11 1.371(7) . ? N2 C16 1.476(7) . ? N2 C17 1.486(7) . ? N2 H2N 0.9300 . ? C1 C2 1.388(7) . ? C1 C6 1.431(9) . ? C1 C7 1.507(8) . ? C2 C3 1.430(8) . ? C2 H2 0.9500 . ? C3 C4 1.368(8) . ? C3 H3 0.9500 . ? C4 C5 1.404(8) . ? C4 C10 1.516(8) . ? C5 C6 1.377(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.531(9) . ? C7 C9 1.535(9) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.362(8) . ? C11 H11 0.9500 . ? C12 C13 1.383(9) . ? C12 H12 0.9500 . ? C13 C14 1.373(8) . ? C13 H13 0.9500 . ? C14 C15 1.406(8) . ? C14 H14 0.9500 . ? C15 C16 1.510(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C22 1.556(8) . ? C17 C18 1.572(8) . ? C17 H17 1.0000 . ? C18 C19 1.506(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C23 1.512(8) . ? C19 C20 1.543(9) . ? C19 H19 1.0000 . ? C20 C21 1.520(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.532(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C24 1.514(7) . ? C22 C23 1.533(8) . ? C23 C25 1.510(8) . ? C23 C26 1.523(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? Sb1 F2 1.837(4) . ? Sb1 F3 1.839(4) . ? Sb1 F4 1.848(4) . ? Sb1 F1 1.850(4) . ? Sb1 F6 1.852(3) . ? Sb1 F5 1.869(4) . ? Sb2 F8 1.824(3) . ? Sb2 F10 1.846(4) . ? Sb2 F7 1.851(4) . ? Sb2 F12 1.851(4) . ? Sb2 F11 1.851(4) . ? Sb2 F9 1.876(4) . ? O2 C29 1.418(8) . ? O2 C27 1.434(8) . ? C27 C28 1.474(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28B 0.9800 . ? C28 H28A 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.480(9) . ? C29 H29B 0.9900 . ? C29 H29A 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? Cl1 C31 1.742(9) . ? Cl2 C31 1.721(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru N2 76.63(19) . . ? N1 Ru O1 86.49(18) . . ? N2 Ru O1 80.39(17) . . ? N1 Ru C2 115.0(2) . . ? N2 Ru C2 98.0(2) . . ? O1 Ru C2 157.7(2) . . ? N1 Ru C6 93.4(2) . . ? N2 Ru C6 157.6(2) . . ? O1 Ru C6 119.5(2) . . ? C2 Ru C6 67.8(2) . . ? N1 Ru C1 89.6(2) . . ? N2 Ru C1 120.1(2) . . ? O1 Ru C1 157.5(2) . . ? C2 Ru C1 37.5(2) . . ? C6 Ru C1 38.7(2) . . ? N1 Ru C5 120.9(2) . . ? N2 Ru C5 161.6(2) . . ? O1 Ru C5 94.5(2) . . ? C2 Ru C5 80.1(2) . . ? C6 Ru C5 37.1(2) . . ? C1 Ru C5 68.8(2) . . ? N1 Ru C3 153.3(2) . . ? N2 Ru C3 100.9(2) . . ? O1 Ru C3 119.6(2) . . ? C2 Ru C3 38.5(2) . . ? C6 Ru C3 79.0(2) . . ? C1 Ru C3 68.4(3) . . ? C5 Ru C3 66.2(2) . . ? N1 Ru C4 158.3(2) . . ? N2 Ru C4 124.9(2) . . ? O1 Ru C4 94.4(2) . . ? C2 Ru C4 68.1(3) . . ? C6 Ru C4 67.3(2) . . ? C1 Ru C4 81.3(3) . . ? C5 Ru C4 37.4(2) . . ? C3 Ru C4 36.3(2) . . ? Ru O1 H1O1 122.3 . . ? Ru O1 H2O1 129.0 . . ? H1O1 O1 H2O1 107.5 . . ? C15 N1 C11 114.7(6) . . ? C15 N1 Ru 118.3(5) . . ? C11 N1 Ru 126.7(4) . . ? C16 N2 C17 111.8(5) . . ? C16 N2 Ru 106.8(3) . . ? C17 N2 Ru 120.5(4) . . ? C16 N2 H2N 105.6 . . ? C17 N2 H2N 105.6 . . ? Ru N2 H2N 105.6 . . ? C2 C1 C6 117.4(6) . . ? C2 C1 C7 124.3(7) . . ? C6 C1 C7 118.1(6) . . ? C2 C1 Ru 71.1(4) . . ? C6 C1 Ru 70.7(4) . . ? C7 C1 Ru 132.3(5) . . ? C1 C2 C3 120.1(7) . . ? C1 C2 Ru 71.4(4) . . ? C3 C2 Ru 71.7(4) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? Ru C2 H2 129.3 . . ? C4 C3 C2 121.9(7) . . ? C4 C3 Ru 72.9(4) . . ? C2 C3 Ru 69.8(4) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? Ru C3 H3 131.2 . . ? C3 C4 C5 118.1(7) . . ? C3 C4 C10 122.4(6) . . ? C5 C4 C10 119.5(6) . . ? C3 C4 Ru 70.8(4) . . ? C5 C4 Ru 69.8(4) . . ? C10 C4 Ru 129.2(5) . . ? C6 C5 C4 121.3(7) . . ? C6 C5 Ru 71.2(4) . . ? C4 C5 Ru 72.8(4) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? Ru C5 H5 129.1 . . ? C5 C6 C1 121.2(6) . . ? C5 C6 Ru 71.7(4) . . ? C1 C6 Ru 70.6(4) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? Ru C6 H6 131.1 . . ? C1 C7 C8 111.4(6) . . ? C1 C7 C9 113.1(6) . . ? C8 C7 C9 108.9(7) . . ? C1 C7 H7 107.8 . . ? C8 C7 H7 107.8 . . ? C9 C7 H7 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 N1 125.2(7) . . ? C12 C11 H11 117.4 . . ? N1 C11 H11 117.4 . . ? C11 C12 C13 117.4(7) . . ? C11 C12 H12 121.3 . . ? C13 C12 H12 121.3 . . ? C14 C13 C12 120.8(7) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 116.8(6) . . ? C13 C14 H14 121.6 . . ? C15 C14 H14 121.6 . . ? N1 C15 C14 124.8(6) . . ? N1 C15 C16 113.4(6) . . ? C14 C15 C16 121.7(6) . . ? N2 C16 C15 109.2(5) . . ? N2 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? N2 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? N2 C17 C22 120.3(5) . . ? N2 C17 C18 110.6(5) . . ? C22 C17 C18 101.6(5) . . ? N2 C17 H17 107.9 . . ? C22 C17 H17 107.9 . . ? C18 C17 H17 107.9 . . ? C19 C18 C17 103.7(5) . . ? C19 C18 H18A 111.0 . . ? C17 C18 H18A 111.0 . . ? C19 C18 H18B 111.0 . . ? C17 C18 H18B 111.0 . . ? H18A C18 H18B 109.0 . . ? C18 C19 C23 102.4(5) . . ? C18 C19 C20 107.0(6) . . ? C23 C19 C20 102.8(5) . . ? C18 C19 H19 114.5 . . ? C23 C19 H19 114.5 . . ? C20 C19 H19 114.5 . . ? C21 C20 C19 102.1(5) . . ? C21 C20 H20A 111.3 . . ? C19 C20 H20A 111.3 . . ? C21 C20 H20B 111.3 . . ? C19 C20 H20B 111.3 . . ? H20A C20 H20B 109.2 . . ? C20 C21 C22 105.1(5) . . ? C20 C21 H21A 110.7 . . ? C22 C21 H21A 110.7 . . ? C20 C21 H21B 110.7 . . ? C22 C21 H21B 110.7 . . ? H21A C21 H21B 108.8 . . ? C24 C22 C21 114.4(6) . . ? C24 C22 C23 115.1(6) . . ? C21 C22 C23 100.8(5) . . ? C24 C22 C17 116.3(5) . . ? C21 C22 C17 107.5(5) . . ? C23 C22 C17 100.7(5) . . ? C25 C23 C19 113.6(6) . . ? C25 C23 C26 106.0(6) . . ? C19 C23 C26 113.7(6) . . ? C25 C23 C22 114.0(6) . . ? C19 C23 C22 95.0(5) . . ? C26 C23 C22 114.8(6) . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? F2 Sb1 F3 90.67(17) . . ? F2 Sb1 F4 90.04(17) . . ? F3 Sb1 F4 179.14(18) . . ? F2 Sb1 F1 179.65(19) . . ? F3 Sb1 F1 89.42(16) . . ? F4 Sb1 F1 89.87(17) . . ? F2 Sb1 F6 89.67(17) . . ? F3 Sb1 F6 90.44(17) . . ? F4 Sb1 F6 90.06(16) . . ? F1 Sb1 F6 90.66(18) . . ? F2 Sb1 F5 89.41(17) . . ? F3 Sb1 F5 90.57(17) . . ? F4 Sb1 F5 88.95(17) . . ? F1 Sb1 F5 90.26(18) . . ? F6 Sb1 F5 178.64(18) . . ? F8 Sb2 F10 91.1(2) . . ? F8 Sb2 F7 179.13(18) . . ? F10 Sb2 F7 88.97(18) . . ? F8 Sb2 F12 89.42(17) . . ? F10 Sb2 F12 90.57(18) . . ? F7 Sb2 F12 89.71(16) . . ? F8 Sb2 F11 89.79(18) . . ? F10 Sb2 F11 91.37(17) . . ? F7 Sb2 F11 91.07(17) . . ? F12 Sb2 F11 177.92(18) . . ? F8 Sb2 F9 90.64(19) . . ? F10 Sb2 F9 177.85(17) . . ? F7 Sb2 F9 89.25(16) . . ? F12 Sb2 F9 88.21(17) . . ? F11 Sb2 F9 89.87(17) . . ? C29 O2 C27 112.2(6) . . ? O2 C27 C28 108.8(7) . . ? O2 C27 H27A 109.9 . . ? C28 C27 H27A 109.9 . . ? O2 C27 H27B 109.9 . . ? C28 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28A 109.5 . . ? H28B C28 H28A 109.5 . . ? C27 C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? O2 C29 C30 112.9(7) . . ? O2 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? O2 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? H29B C29 H29A 107.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Cl2 C31 Cl1 111.2(5) . . ? Cl2 C31 H31A 109.4 . . ? Cl1 C31 H31A 109.4 . . ? Cl2 C31 H31B 109.4 . . ? Cl1 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.434 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.115