# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sar50 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15.31 H9 F3 N4 O0.31' _chemical_formula_weight 311.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 15.3175(7) _cell_length_b 15.3175(7) _cell_length_c 23.0865(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5416.7(4) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2776 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2534 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 Kappa ApexII duo' _diffrn_measurement_method 'omega psi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19474 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.39 _reflns_number_total 2776 _reflns_number_gt 2107 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0465P)^2^+8.0123P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2776 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C8 C 0.66382(16) 0.08379(15) 0.25427(13) 0.0456(7) Uani 1 1 d . . . H8A H 0.6380 0.0545 0.2862 0.055 Uiso 1 1 calc R . . C7 C 0.72596(17) 0.04004(15) 0.22264(12) 0.0471(7) Uani 1 1 d . . . H7A H 0.7420 -0.0181 0.2323 0.056 Uiso 1 1 calc R . . C6 C 0.7642(2) 0.08202(17) 0.17698(12) 0.0527(8) Uani 1 1 d . . . H6A H 0.8072 0.0533 0.1543 0.063 Uiso 1 1 calc R . . C5 C 0.73970(18) 0.16626(16) 0.16434(10) 0.0430(6) Uani 1 1 d . . . H5A H 0.7661 0.1970 0.1332 0.052 Uiso 1 1 calc R . . C4 C 0.67564(14) 0.20559(13) 0.19801(9) 0.0287(5) Uani 1 1 d . . . C3 C 0.64684(13) 0.29523(13) 0.18601(8) 0.0243(4) Uani 1 1 d . . . C1 C 0.58378(13) 0.34410(12) 0.21252(9) 0.0248(4) Uani 1 1 d . . . H1A H 0.5472 0.3274 0.2438 0.030 Uiso 1 1 calc R . . C9 C 0.53308(12) 0.49713(12) 0.19504(8) 0.0221(4) Uani 1 1 d . . . C10 C 0.54297(13) 0.54041(13) 0.24697(9) 0.0282(5) Uani 1 1 d . . . H10A H 0.5827 0.5190 0.2752 0.034 Uiso 1 1 calc R . . C11 C 0.49489(14) 0.61531(14) 0.25797(10) 0.0328(5) Uani 1 1 d . . . H11A H 0.5015 0.6451 0.2938 0.039 Uiso 1 1 calc R . . C12 C 0.43772(14) 0.64647(14) 0.21701(10) 0.0346(5) Uani 1 1 d . . . H12A H 0.4056 0.6984 0.2243 0.042 Uiso 1 1 calc R . . C13 C 0.42683(14) 0.60239(13) 0.16507(10) 0.0316(5) Uani 1 1 d . . . H13A H 0.3867 0.6239 0.1371 0.038 Uiso 1 1 calc R . . C14 C 0.47412(13) 0.52712(13) 0.15356(9) 0.0247(4) Uani 1 1 d . . . C15 C 0.45897(14) 0.47909(14) 0.09771(9) 0.0321(5) Uani 1 1 d . . . C16 C 0.5590(2) 0.2148(3) 0.34225(15) 0.0234(8) Uani 0.66 1 d P . . C17 C 0.61024(19) 0.2203(2) 0.38432(12) 0.0254(7) Uani 0.66 1 d P . . N2 N 0.63731(12) 0.16568(12) 0.24267(9) 0.0366(5) Uani 1 1 d . . . N1 N 0.68333(12) 0.34451(12) 0.14336(8) 0.0322(4) Uani 1 1 d . . . N3 N 0.64631(12) 0.42111(11) 0.14237(7) 0.0305(4) Uani 1 1 d . . . N5 N 0.58498(10) 0.42106(10) 0.18455(7) 0.0223(4) Uani 1 1 d . . . F1 F 0.45426(9) 0.39253(8) 0.10474(5) 0.0398(3) Uani 1 1 d . . . F2 F 0.52236(9) 0.49330(9) 0.05888(5) 0.0423(4) Uani 1 1 d . . . F3 F 0.38450(10) 0.50349(10) 0.07231(6) 0.0518(4) Uani 1 1 d . . . O1 O 0.5000 0.2500 0.4055(3) 0.208(7) Uani 0.66 2 d SP . . 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 C8 0.0385(13) 0.0329(13) 0.0653(17) 0.0119(12) -0.0207(13) -0.0102(10) C7 0.0499(15) 0.0238(12) 0.0675(18) -0.0030(12) -0.0313(14) 0.0026(11) C6 0.0700(19) 0.0395(14) 0.0485(16) -0.0169(13) -0.0228(14) 0.0266(13) C5 0.0617(16) 0.0384(13) 0.0288(12) -0.0067(10) -0.0073(11) 0.0194(12) C4 0.0345(11) 0.0242(10) 0.0276(10) -0.0060(9) -0.0126(9) 0.0002(9) C3 0.0278(10) 0.0245(10) 0.0206(10) -0.0045(8) -0.0033(8) -0.0003(8) C1 0.0263(10) 0.0247(10) 0.0236(10) 0.0005(8) 0.0015(8) -0.0030(8) C9 0.0212(9) 0.0204(9) 0.0249(10) -0.0003(8) 0.0026(8) -0.0001(7) C10 0.0254(10) 0.0327(11) 0.0264(10) -0.0045(9) -0.0024(8) 0.0047(8) C11 0.0315(12) 0.0339(12) 0.0331(12) -0.0102(10) -0.0006(9) 0.0037(9) C12 0.0307(11) 0.0270(11) 0.0462(14) -0.0044(10) -0.0006(10) 0.0067(9) C13 0.0287(11) 0.0292(11) 0.0369(12) 0.0060(9) -0.0056(9) 0.0022(9) C14 0.0244(10) 0.0246(10) 0.0251(10) 0.0032(8) -0.0011(8) -0.0038(8) C15 0.0349(12) 0.0339(12) 0.0276(11) 0.0041(9) -0.0084(9) -0.0034(9) C16 0.0166(14) 0.0244(18) 0.0291(18) 0.0027(13) 0.0086(13) 0.0058(12) C17 0.0189(14) 0.0430(19) 0.0144(14) -0.0030(13) 0.0007(11) 0.0079(12) N2 0.0323(10) 0.0290(10) 0.0485(12) 0.0055(9) -0.0099(9) -0.0053(8) N1 0.0387(10) 0.0319(10) 0.0261(9) -0.0002(8) 0.0070(8) 0.0088(8) N3 0.0334(10) 0.0321(10) 0.0262(9) 0.0029(7) 0.0108(8) 0.0057(8) N5 0.0229(8) 0.0245(8) 0.0194(8) -0.0018(7) 0.0017(7) 0.0007(6) F1 0.0549(9) 0.0309(7) 0.0334(7) -0.0031(6) -0.0090(6) -0.0132(6) F2 0.0558(9) 0.0503(8) 0.0209(6) 0.0022(6) 0.0025(6) -0.0100(7) F3 0.0495(9) 0.0612(10) 0.0446(9) -0.0045(7) -0.0265(7) 0.0036(7) O1 0.118(9) 0.44(2) 0.069(5) 0.000 0.000 0.127(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C8 N2 1.345(3) . ? C8 C7 1.374(4) . ? C7 C6 1.367(4) . ? C6 C5 1.375(3) . ? C5 C4 1.389(3) . ? C4 N2 1.335(3) . ? C4 C3 1.468(3) . ? C3 N1 1.361(3) . ? C3 C1 1.367(3) . ? C1 N5 1.344(2) . ? C9 C10 1.378(3) . ? C9 C14 1.394(3) . ? C9 N5 1.431(2) . ? C10 C11 1.387(3) . ? C11 C12 1.374(3) . ? C12 C13 1.386(3) . ? C13 C14 1.387(3) . ? C14 C15 1.503(3) . ? C15 F3 1.336(2) . ? C15 F1 1.338(2) . ? C15 F2 1.339(3) . ? C16 O1 1.053(3) 11_666 ? C16 C17 1.252(5) . ? C16 O1 1.800(6) . ? C16 C17 1.860(5) 11_666 ? C17 O1 1.816(3) . ? C17 C16 1.860(5) 16_656 ? N1 N3 1.303(2) . ? N3 N5 1.353(2) . ? O1 C16 1.053(3) 16_656 ? O1 C16 1.053(3) 11_666 ? O1 O1 1.410(16) 11_666 ? O1 C16 1.800(6) 6_554 ? O1 C17 1.816(3) 6_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C8 C7 123.9(3) . . ? C6 C7 C8 118.5(2) . . ? C7 C6 C5 119.2(3) . . ? C6 C5 C4 118.8(3) . . ? N2 C4 C5 123.0(2) . . ? N2 C4 C3 116.22(19) . . ? C5 C4 C3 120.8(2) . . ? N1 C3 C1 108.09(17) . . ? N1 C3 C4 122.12(18) . . ? C1 C3 C4 129.79(19) . . ? N5 C1 C3 104.80(17) . . ? C10 C9 C14 120.67(18) . . ? C10 C9 N5 118.55(17) . . ? C14 C9 N5 120.78(17) . . ? C9 C10 C11 119.93(19) . . ? C12 C11 C10 120.0(2) . . ? C11 C12 C13 120.2(2) . . ? C12 C13 C14 120.5(2) . . ? C13 C14 C9 118.71(19) . . ? C13 C14 C15 119.39(18) . . ? C9 C14 C15 121.88(18) . . ? F3 C15 F1 106.53(17) . . ? F3 C15 F2 106.24(17) . . ? F1 C15 F2 106.34(18) . . ? F3 C15 C14 111.80(18) . . ? F1 C15 C14 112.93(17) . . ? F2 C15 C14 112.51(17) . . ? O1 C16 C17 117.8(6) 11_666 . ? O1 C16 O1 51.5(6) 11_666 . ? C17 C16 O1 70.4(2) . . ? O1 C16 C17 71.1(3) 11_666 11_666 ? C17 C16 C17 105.9(2) . 11_666 ? O1 C16 C17 65.32(15) . 11_666 ? C16 C17 O1 69.1(3) . . ? C16 C17 C16 83.5(3) . 16_656 ? O1 C17 C16 33.27(11) . 16_656 ? C4 N2 C8 116.6(2) . . ? N3 N1 C3 109.47(17) . . ? N1 N3 N5 106.80(16) . . ? C1 N5 N3 110.84(16) . . ? C1 N5 C9 128.68(16) . . ? N3 N5 C9 120.46(16) . . ? C16 O1 C16 174.4(11) 16_656 11_666 ? C16 O1 O1 92.8(5) 16_656 11_666 ? C16 O1 O1 92.8(5) 11_666 11_666 ? C16 O1 C16 92.3(4) 16_656 . ? C16 O1 C16 92.3(4) 11_666 . ? O1 O1 C16 35.76(15) 11_666 . ? C16 O1 C16 92.3(4) 16_656 6_554 ? C16 O1 C16 92.3(4) 11_666 6_554 ? O1 O1 C16 35.76(15) 11_666 6_554 ? C16 O1 C16 71.5(3) . 6_554 ? C16 O1 C17 105.9(3) 16_656 6_554 ? C16 O1 C17 75.7(3) 11_666 6_554 ? O1 O1 C17 74.4(3) 11_666 6_554 ? C16 O1 C17 108.8(4) . 6_554 ? C16 O1 C17 40.49(19) 6_554 6_554 ? C16 O1 C17 75.7(3) 16_656 . ? C16 O1 C17 105.9(3) 11_666 . ? O1 O1 C17 74.4(3) 11_666 . ? C16 O1 C17 40.49(19) . . ? C16 O1 C17 108.8(4) 6_554 . ? C17 O1 C17 148.7(5) 6_554 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.228 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.049 _database_code_depnum_ccdc_archive 'CCDC 846891' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c:\rechne\sar56 #TrackingRef 'SH16.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H25 Cl2 F3 N8 O8 Ru' _chemical_formula_weight 902.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6547(12) _cell_length_b 11.6352(12) _cell_length_c 14.5178(16) _cell_angle_alpha 89.532(5) _cell_angle_beta 77.126(5) _cell_angle_gamma 87.806(4) _cell_volume 1753.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7226 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27 _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.696 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 Kappa Apex II duo' _diffrn_measurement_method 'omega psi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24195 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0791 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 26.60 _reflns_number_total 7226 _reflns_number_gt 5206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Kappa Apex II suite, 2008' _computing_cell_refinement 'Bruker Kappa Apex II suite, 2008' _computing_data_reduction 'Bruker Kappa Apex II suite, 2008' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0250P)^2^+0.7795P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7226 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0684(3) 0.2465(3) 0.0236(2) 0.0186(8) Uani 1 1 d . . . H1 H 1.1365 0.1940 0.0301 0.022 Uiso 1 1 calc R . . C2 C 1.0700(3) 0.2930(3) -0.0638(2) 0.0227(8) Uani 1 1 d . . . H2 H 1.1383 0.2739 -0.1163 0.027 Uiso 1 1 calc R . . C3 C 0.9704(3) 0.3680(3) -0.0742(2) 0.0221(8) Uani 1 1 d . . . H3 H 0.9688 0.3997 -0.1344 0.026 Uiso 1 1 calc R . . C4 C 0.8735(3) 0.3967(3) 0.0030(2) 0.0207(8) Uani 1 1 d . . . H4 H 0.8045 0.4482 -0.0031 0.025 Uiso 1 1 calc R . . C5 C 0.8789(3) 0.3488(3) 0.0896(2) 0.0152(7) Uani 1 1 d . . . C6 C 0.7861(3) 0.3735(3) 0.1769(2) 0.0142(7) Uani 1 1 d . . . C7 C 0.6738(3) 0.4381(2) 0.2026(2) 0.0145(7) Uani 1 1 d . . . H7 H 0.6333 0.4855 0.1633 0.017 Uiso 1 1 calc R . . C8 C 0.5143(3) 0.4607(3) 0.3550(2) 0.0151(7) Uani 1 1 d . . . C9 C 0.4953(3) 0.5786(3) 0.3685(2) 0.0218(8) Uani 1 1 d . . . H9 H 0.5621 0.6292 0.3427 0.026 Uiso 1 1 calc R . . C10 C 0.3782(3) 0.6215(3) 0.4201(2) 0.0249(9) Uani 1 1 d . . . H10 H 0.3639 0.7021 0.4294 0.030 Uiso 1 1 calc R . . C11 C 0.2824(3) 0.5480(3) 0.4579(2) 0.0256(9) Uani 1 1 d . . . H11 H 0.2021 0.5780 0.4933 0.031 Uiso 1 1 calc R . . C12 C 0.3020(3) 0.4307(3) 0.4448(2) 0.0222(8) Uani 1 1 d . . . H12 H 0.2351 0.3806 0.4715 0.027 Uiso 1 1 calc R . . C13 C 0.4183(3) 0.3856(3) 0.3931(2) 0.0179(8) Uani 1 1 d . . . C14 C 0.4345(3) 0.2574(3) 0.3803(2) 0.0203(8) Uani 1 1 d . . . C15 C 1.1180(3) -0.0173(3) 0.1849(2) 0.0186(8) Uani 1 1 d . . . H15 H 1.0385 -0.0551 0.1983 0.022 Uiso 1 1 calc R . . C16 C 1.2302(3) -0.0813(3) 0.1508(3) 0.0245(9) Uani 1 1 d . . . H16 H 1.2276 -0.1615 0.1399 0.029 Uiso 1 1 calc R . . C17 C 1.3458(3) -0.0273(3) 0.1326(2) 0.0234(8) Uani 1 1 d . . . H17 H 1.4240 -0.0696 0.1085 0.028 Uiso 1 1 calc R . . C18 C 1.3468(3) 0.0889(3) 0.1498(2) 0.0189(8) Uani 1 1 d . . . H18 H 1.4260 0.1271 0.1386 0.023 Uiso 1 1 calc R . . C19 C 1.2317(3) 0.1496(3) 0.1835(2) 0.0150(7) Uani 1 1 d . . . C20 C 1.2204(3) 0.2738(3) 0.2037(2) 0.0146(7) Uani 1 1 d . . . C21 C 1.3212(3) 0.3475(3) 0.1810(2) 0.0183(8) Uani 1 1 d . . . H21 H 1.4044 0.3191 0.1496 0.022 Uiso 1 1 calc R . . C22 C 1.3008(3) 0.4625(3) 0.2041(2) 0.0191(8) Uani 1 1 d . . . H22 H 1.3687 0.5146 0.1869 0.023 Uiso 1 1 calc R . . C23 C 1.1805(3) 0.5006(3) 0.2526(2) 0.0173(8) Uani 1 1 d . . . H23 H 1.1654 0.5785 0.2724 0.021 Uiso 1 1 calc R . . C24 C 1.0821(3) 0.4241(3) 0.2720(2) 0.0173(8) Uani 1 1 d . . . H24 H 0.9990 0.4511 0.3046 0.021 Uiso 1 1 calc R . . C25 C 0.7886(3) 0.0609(3) 0.1426(2) 0.0192(8) Uani 1 1 d . . . H25 H 0.8302 0.0976 0.0859 0.023 Uiso 1 1 calc R . . C26 C 0.6951(3) -0.0158(3) 0.1390(3) 0.0237(8) Uani 1 1 d . . . H26 H 0.6735 -0.0326 0.0806 0.028 Uiso 1 1 calc R . . C27 C 0.6327(3) -0.0682(3) 0.2215(3) 0.0227(8) Uani 1 1 d . . . H27 H 0.5676 -0.1215 0.2207 0.027 Uiso 1 1 calc R . . C28 C 0.6667(3) -0.0420(3) 0.3043(2) 0.0194(8) Uani 1 1 d . . . H28 H 0.6240 -0.0763 0.3618 0.023 Uiso 1 1 calc R . . C29 C 0.7634(3) 0.0348(2) 0.3042(2) 0.0135(7) Uani 1 1 d . . . C30 C 0.8097(3) 0.0658(3) 0.3884(2) 0.0146(7) Uani 1 1 d . . . C31 C 0.7607(3) 0.0225(3) 0.4778(2) 0.0217(8) Uani 1 1 d . . . H31 H 0.6938 -0.0310 0.4873 0.026 Uiso 1 1 calc R . . C32 C 0.8093(4) 0.0574(3) 0.5529(2) 0.0253(8) Uani 1 1 d . . . H32 H 0.7764 0.0288 0.6147 0.030 Uiso 1 1 calc R . . C33 C 0.9073(3) 0.1352(3) 0.5366(2) 0.0240(8) Uani 1 1 d . . . H33 H 0.9422 0.1612 0.5871 0.029 Uiso 1 1 calc R . . C34 C 0.9531(3) 0.1742(3) 0.4459(2) 0.0201(8) Uani 1 1 d . . . H134 H 1.0211 0.2266 0.4352 0.024 Uiso 1 1 calc R . . N1 N 0.9746(2) 0.2718(2) 0.10096(18) 0.0146(6) Uani 1 1 d . . . N2 N 0.8070(2) 0.3202(2) 0.25657(18) 0.0134(6) Uani 1 1 d . . . N3 N 0.7143(3) 0.3475(2) 0.32989(18) 0.0144(6) Uani 1 1 d . . . N4 N 0.6337(2) 0.4198(2) 0.29557(18) 0.0141(6) Uani 1 1 d . . . N8 N 1.1168(3) 0.0969(2) 0.20006(18) 0.0149(6) Uani 1 1 d . . . N7 N 1.0996(3) 0.3132(2) 0.24657(18) 0.0140(6) Uani 1 1 d . . . N10 N 0.8237(2) 0.0861(2) 0.22354(19) 0.0148(6) Uani 1 1 d . . . N9 N 0.9063(2) 0.1416(2) 0.37200(18) 0.0143(6) Uani 1 1 d . . . O1 O 0.5368(3) 0.2961(2) -0.16189(16) 0.0348(7) Uani 1 1 d . . . O2 O 0.4132(3) 0.41573(18) -0.04364(17) 0.0318(7) Uani 1 1 d . . . O3 O 0.5751(2) 0.2923(2) -0.00883(18) 0.0345(7) Uani 1 1 d . . . O4 O 0.3876(2) 0.21720(19) -0.03682(17) 0.0286(6) Uani 1 1 d . . . O5 O 0.8313(2) 0.61466(19) 0.28317(17) 0.0299(6) Uani 1 1 d . . . O6 O 0.9487(2) 0.6411(2) 0.39903(17) 0.0289(6) Uani 1 1 d . . . O7 O 0.9520(3) 0.7786(2) 0.27920(18) 0.0444(8) Uani 1 1 d . . . O8 O 0.7636(3) 0.7570(2) 0.39747(18) 0.0491(9) Uani 1 1 d . . . F1 F 0.50468(18) 0.22560(15) 0.29456(13) 0.0214(4) Uani 1 1 d . . . F2 F 0.32032(18) 0.20793(16) 0.38878(14) 0.0271(5) Uani 1 1 d . . . F3 F 0.49153(19) 0.20576(15) 0.44380(13) 0.0266(5) Uani 1 1 d . . . Cl1 Cl 0.47822(8) 0.30617(6) -0.06277(6) 0.01957(19) Uani 1 1 d . . . Cl2 Cl 0.87378(9) 0.69828(7) 0.33954(6) 0.0232(2) Uani 1 1 d . . . Ru1 Ru 0.95662(3) 0.20342(2) 0.23661(2) 0.01298(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 C1 0.0143(19) 0.0222(18) 0.0196(19) 0.0010(15) -0.0040(16) -0.0019(15) C2 0.022(2) 0.0285(19) 0.0161(19) -0.0022(15) -0.0011(16) 0.0007(16) C3 0.025(2) 0.0271(19) 0.0146(19) 0.0039(15) -0.0054(17) -0.0020(17) C4 0.022(2) 0.0232(18) 0.0178(19) 0.0008(15) -0.0065(16) 0.0033(16) C5 0.0107(18) 0.0163(16) 0.0194(18) 0.0006(14) -0.0048(15) -0.0035(14) C6 0.0139(18) 0.0144(16) 0.0141(18) 0.0007(13) -0.0015(15) -0.0061(14) C7 0.0164(19) 0.0108(15) 0.0169(18) 0.0030(13) -0.0045(15) -0.0032(14) C8 0.0122(18) 0.0204(17) 0.0134(17) -0.0005(14) -0.0046(15) 0.0028(15) C9 0.019(2) 0.0226(18) 0.026(2) -0.0027(16) -0.0084(17) -0.0020(16) C10 0.025(2) 0.0245(19) 0.027(2) -0.0079(16) -0.0101(18) 0.0065(17) C11 0.019(2) 0.039(2) 0.017(2) -0.0051(17) -0.0018(16) 0.0065(18) C12 0.017(2) 0.034(2) 0.0141(18) 0.0030(15) -0.0017(16) -0.0005(16) C13 0.0177(19) 0.0232(18) 0.0137(18) 0.0015(14) -0.0058(15) -0.0006(15) C14 0.017(2) 0.0286(19) 0.0164(19) 0.0031(15) -0.0053(16) -0.0025(16) C15 0.0158(19) 0.0159(16) 0.024(2) 0.0018(14) -0.0030(16) -0.0058(15) C16 0.020(2) 0.0162(18) 0.038(2) -0.0019(16) -0.0095(18) 0.0046(16) C17 0.016(2) 0.0216(18) 0.033(2) -0.0041(16) -0.0057(17) 0.0076(16) C18 0.0091(18) 0.0237(18) 0.025(2) 0.0011(15) -0.0063(16) 0.0000(15) C19 0.0158(19) 0.0142(16) 0.0166(18) 0.0024(13) -0.0071(15) -0.0027(14) C20 0.0149(19) 0.0177(16) 0.0127(17) 0.0018(13) -0.0064(15) -0.0026(14) C21 0.0161(19) 0.0232(18) 0.0162(18) 0.0038(14) -0.0052(15) -0.0020(15) C22 0.024(2) 0.0171(17) 0.0209(19) 0.0069(14) -0.0139(17) -0.0080(15) C23 0.025(2) 0.0109(16) 0.0197(19) 0.0038(14) -0.0127(17) -0.0018(15) C24 0.020(2) 0.0138(16) 0.0191(18) 0.0009(14) -0.0064(16) 0.0015(15) C25 0.020(2) 0.0220(18) 0.0162(19) -0.0016(14) -0.0060(16) -0.0006(15) C26 0.029(2) 0.0211(18) 0.024(2) -0.0026(16) -0.0116(18) -0.0031(16) C27 0.020(2) 0.0155(17) 0.036(2) -0.0009(16) -0.0134(18) -0.0064(15) C28 0.019(2) 0.0152(17) 0.025(2) 0.0037(15) -0.0071(16) -0.0021(15) C29 0.0099(18) 0.0116(15) 0.0196(18) 0.0034(13) -0.0049(15) 0.0002(13) C30 0.0136(18) 0.0133(16) 0.0173(18) 0.0024(13) -0.0044(15) 0.0017(14) C31 0.021(2) 0.0204(18) 0.024(2) 0.0037(15) -0.0060(17) -0.0051(15) C32 0.030(2) 0.0274(19) 0.018(2) 0.0065(16) -0.0040(17) -0.0047(17) C33 0.030(2) 0.0250(19) 0.020(2) 0.0027(15) -0.0125(17) -0.0049(17) C34 0.019(2) 0.0202(17) 0.024(2) 0.0009(15) -0.0101(16) -0.0018(15) N1 0.0130(15) 0.0153(14) 0.0157(15) -0.0010(11) -0.0033(13) -0.0026(12) N2 0.0130(15) 0.0128(13) 0.0151(15) -0.0005(11) -0.0039(13) -0.0053(12) N3 0.0135(15) 0.0149(13) 0.0150(15) -0.0005(11) -0.0042(13) 0.0015(12) N4 0.0102(15) 0.0149(13) 0.0168(15) 0.0007(12) -0.0021(12) -0.0005(12) N8 0.0151(16) 0.0137(13) 0.0163(15) 0.0008(11) -0.0042(13) -0.0014(12) N7 0.0157(16) 0.0127(13) 0.0148(15) 0.0018(11) -0.0055(12) -0.0044(12) N10 0.0128(15) 0.0137(13) 0.0189(16) -0.0014(12) -0.0058(13) 0.0011(12) N9 0.0133(15) 0.0130(13) 0.0173(15) 0.0017(11) -0.0045(13) -0.0015(12) O1 0.0532(19) 0.0289(14) 0.0170(14) -0.0006(11) 0.0060(13) -0.0157(13) O2 0.0507(18) 0.0171(12) 0.0303(15) -0.0022(11) -0.0163(14) 0.0106(12) O3 0.0233(15) 0.0412(15) 0.0427(17) -0.0063(13) -0.0157(13) 0.0049(12) O4 0.0275(15) 0.0247(13) 0.0298(15) -0.0001(11) 0.0038(12) -0.0133(12) O5 0.0330(16) 0.0277(13) 0.0296(15) -0.0025(11) -0.0063(13) -0.0141(12) O6 0.0275(15) 0.0338(14) 0.0256(15) 0.0006(12) -0.0054(12) -0.0055(12) O7 0.073(2) 0.0384(16) 0.0228(15) 0.0106(12) -0.0081(15) -0.0397(15) O8 0.073(2) 0.0372(16) 0.0243(16) 0.0038(12) 0.0106(15) 0.0327(15) F1 0.0229(11) 0.0212(10) 0.0194(11) -0.0019(8) -0.0024(9) -0.0034(9) F2 0.0219(12) 0.0314(11) 0.0280(12) 0.0072(9) -0.0044(10) -0.0095(9) F3 0.0317(13) 0.0250(11) 0.0266(12) 0.0087(9) -0.0137(10) -0.0020(9) Cl1 0.0232(5) 0.0144(4) 0.0213(5) 0.0006(3) -0.0046(4) -0.0035(4) Cl2 0.0336(5) 0.0163(4) 0.0167(5) 0.0001(3) 0.0015(4) -0.0051(4) Ru1 0.01159(15) 0.01252(13) 0.01543(15) 0.00110(10) -0.00408(11) -0.00203(11) _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 C1 N1 1.353(4) . ? C1 C2 1.373(4) . ? C2 C3 1.381(5) . ? C3 C4 1.378(4) . ? C4 C5 1.382(4) . ? C5 N1 1.368(4) . ? C5 C6 1.446(4) . ? C6 N2 1.366(4) . ? C6 C7 1.369(4) . ? C7 N4 1.340(4) . ? C8 C9 1.388(4) . ? C8 C13 1.387(4) . ? C8 N4 1.436(4) . ? C9 C10 1.381(5) . ? C10 C11 1.373(5) . ? C11 C12 1.380(5) . ? C12 C13 1.386(4) . ? C13 C14 1.503(4) . ? C14 F3 1.339(4) . ? C14 F2 1.346(4) . ? C14 F1 1.348(4) . ? C15 N8 1.347(4) . ? C15 C16 1.380(4) . ? C16 C17 1.376(5) . ? C17 C18 1.377(4) . ? C18 C19 1.383(4) . ? C19 N8 1.363(4) . ? C19 C20 1.472(4) . ? C20 N7 1.363(4) . ? C20 C21 1.381(4) . ? C21 C22 1.379(4) . ? C22 C23 1.376(5) . ? C23 C24 1.381(4) . ? C24 N7 1.340(4) . ? C25 N10 1.347(4) . ? C25 C26 1.373(4) . ? C26 C27 1.383(5) . ? C27 C28 1.371(5) . ? C28 C29 1.389(4) . ? C29 N10 1.351(4) . ? C29 C30 1.469(4) . ? C30 N9 1.360(4) . ? C30 C31 1.385(4) . ? C31 C32 1.377(5) . ? C32 C33 1.387(5) . ? C33 C34 1.378(5) . ? C34 N9 1.343(4) . ? N1 Ru1 2.090(3) . ? N2 N3 1.313(3) . ? N2 Ru1 2.026(3) . ? N3 N4 1.350(3) . ? N8 Ru1 2.043(2) . ? N7 Ru1 2.055(3) . ? N10 Ru1 2.044(3) . ? N9 Ru1 2.051(3) . ? O1 Cl1 1.439(2) . ? O2 Cl1 1.426(2) . ? O3 Cl1 1.432(3) . ? O4 Cl1 1.433(2) . ? O5 Cl2 1.426(2) . ? O6 Cl2 1.443(3) . ? O7 Cl2 1.434(3) . ? O8 Cl2 1.435(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 C1 C2 123.1(3) . . ? C1 C2 C3 118.8(3) . . ? C4 C3 C2 119.9(3) . . ? C3 C4 C5 118.5(3) . . ? N1 C5 C4 122.6(3) . . ? N1 C5 C6 112.9(3) . . ? C4 C5 C6 124.5(3) . . ? N2 C6 C7 107.1(3) . . ? N2 C6 C5 117.0(3) . . ? C7 C6 C5 135.8(3) . . ? N4 C7 C6 104.7(3) . . ? C9 C8 C13 121.2(3) . . ? C9 C8 N4 117.7(3) . . ? C13 C8 N4 121.1(3) . . ? C10 C9 C8 119.2(3) . . ? C11 C10 C9 120.2(3) . . ? C10 C11 C12 120.5(3) . . ? C11 C12 C13 120.5(3) . . ? C12 C13 C8 118.5(3) . . ? C12 C13 C14 118.5(3) . . ? C8 C13 C14 123.0(3) . . ? F3 C14 F2 106.2(3) . . ? F3 C14 F1 106.4(3) . . ? F2 C14 F1 105.5(3) . . ? F3 C14 C13 113.2(3) . . ? F2 C14 C13 111.6(3) . . ? F1 C14 C13 113.3(3) . . ? N8 C15 C16 122.5(3) . . ? C17 C16 C15 119.0(3) . . ? C16 C17 C18 119.3(3) . . ? C17 C18 C19 119.6(3) . . ? N8 C19 C18 121.4(3) . . ? N8 C19 C20 114.0(3) . . ? C18 C19 C20 124.6(3) . . ? N7 C20 C21 121.0(3) . . ? N7 C20 C19 114.6(3) . . ? C21 C20 C19 124.3(3) . . ? C22 C21 C20 119.8(3) . . ? C23 C22 C21 118.9(3) . . ? C22 C23 C24 119.1(3) . . ? N7 C24 C23 122.4(3) . . ? N10 C25 C26 122.5(3) . . ? C25 C26 C27 119.1(3) . . ? C28 C27 C26 118.8(3) . . ? C27 C28 C29 120.1(3) . . ? N10 C29 C28 120.9(3) . . ? N10 C29 C30 114.8(3) . . ? C28 C29 C30 124.3(3) . . ? N9 C30 C31 121.8(3) . . ? N9 C30 C29 114.5(3) . . ? C31 C30 C29 123.7(3) . . ? C32 C31 C30 119.7(3) . . ? C31 C32 C33 118.7(3) . . ? C34 C33 C32 119.0(3) . . ? N9 C34 C33 123.1(3) . . ? C1 N1 C5 117.1(3) . . ? C1 N1 Ru1 127.1(2) . . ? C5 N1 Ru1 115.8(2) . . ? N3 N2 C6 110.8(2) . . ? N3 N2 Ru1 133.0(2) . . ? C6 N2 Ru1 115.7(2) . . ? N2 N3 N4 104.9(2) . . ? C7 N4 N3 112.5(3) . . ? C7 N4 C8 126.7(3) . . ? N3 N4 C8 120.6(3) . . ? C15 N8 C19 118.2(3) . . ? C15 N8 Ru1 126.0(2) . . ? C19 N8 Ru1 115.63(19) . . ? C24 N7 C20 118.5(3) . . ? C24 N7 Ru1 125.8(2) . . ? C20 N7 Ru1 114.10(19) . . ? C25 N10 C29 118.6(3) . . ? C25 N10 Ru1 125.2(2) . . ? C29 N10 Ru1 116.1(2) . . ? C34 N9 C30 117.7(3) . . ? C34 N9 Ru1 126.5(2) . . ? C30 N9 Ru1 115.6(2) . . ? O2 Cl1 O3 109.95(15) . . ? O2 Cl1 O4 109.50(15) . . ? O3 Cl1 O4 108.74(16) . . ? O2 Cl1 O1 109.99(15) . . ? O3 Cl1 O1 109.65(16) . . ? O4 Cl1 O1 108.99(14) . . ? O5 Cl2 O8 109.17(17) . . ? O5 Cl2 O7 109.42(15) . . ? O8 Cl2 O7 110.17(17) . . ? O5 Cl2 O6 109.09(14) . . ? O8 Cl2 O6 109.46(15) . . ? O7 Cl2 O6 109.51(16) . . ? N2 Ru1 N8 172.38(11) . . ? N2 Ru1 N10 85.44(10) . . ? N8 Ru1 N10 97.49(10) . . ? N2 Ru1 N9 93.44(10) . . ? N8 Ru1 N9 94.03(10) . . ? N10 Ru1 N9 78.76(10) . . ? N2 Ru1 N7 98.27(10) . . ? N8 Ru1 N7 78.74(10) . . ? N10 Ru1 N7 176.23(10) . . ? N9 Ru1 N7 101.64(10) . . ? N2 Ru1 N1 78.30(10) . . ? N8 Ru1 N1 94.38(10) . . ? N10 Ru1 N1 95.42(10) . . ? N9 Ru1 N1 170.34(10) . . ? N7 Ru1 N1 84.68(10) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.60 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.523 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.102 _database_code_depnum_ccdc_archive 'CCDC 846892' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c:\x-step\sar76 #TrackingRef 'SH23.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 Cl2 N10 O8 Ru' _chemical_formula_weight 1068.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.5069(12) _cell_length_b 15.2755(11) _cell_length_c 19.3531(13) _cell_angle_alpha 90.00 _cell_angle_beta 116.969(4) _cell_angle_gamma 90.00 _cell_volume 4876.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8249 _cell_measurement_theta_min 3 _cell_measurement_theta_max 66 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 4.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.488 _exptl_absorpt_correction_T_max 0.753 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa Apex II duo' _diffrn_measurement_method 'omega psi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28019 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 66.62 _reflns_number_total 8249 _reflns_number_gt 5749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Kappa Apex II suite, 2008' _computing_cell_refinement 'Bruker Kappa Apex II suite, 2008' _computing_data_reduction 'Bruker Kappa Apex II suite, 2008' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+2.7807P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8249 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1228 _refine_ls_wR_factor_gt 0.1087 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.161403(18) -0.00318(2) 0.787994(17) 0.01682(10) Uani 1 1 d . . . N2 N 0.0881(2) 0.0691(2) 0.8201(2) 0.0205(8) Uani 1 1 d . . . N9 N 0.1752(2) 0.0914(2) 0.71885(19) 0.0180(8) Uani 1 1 d . . . N1 N 0.1311(2) -0.0911(2) 0.8517(2) 0.0194(8) Uani 1 1 d . . . N7 N 0.2693(2) 0.0106(2) 0.8883(2) 0.0196(8) Uani 1 1 d . . . N8 N 0.2386(2) -0.0793(2) 0.7633(2) 0.0200(8) Uani 1 1 d . . . N10 N 0.0552(2) -0.0190(2) 0.6865(2) 0.0211(8) Uani 1 1 d . . . Cl1 Cl 0.04670(6) -0.27521(7) 0.59717(6) 0.0258(3) Uani 1 1 d . . . Cl2 Cl 0.15120(7) 0.07414(8) 1.09900(7) 0.0336(3) Uani 1 1 d . . . O1 O 0.0823(2) -0.2483(2) 0.67700(17) 0.0320(8) Uani 1 1 d . . . N6 N 0.0069(2) 0.1590(2) 0.8309(2) 0.0213(8) Uani 1 1 d . . . O2 O -0.04053(19) -0.2757(2) 0.56486(19) 0.0335(8) Uani 1 1 d . . . C5 C 0.1328(3) -0.2815(3) 0.9511(3) 0.0253(10) Uani 1 1 d . . . O3 O 0.0747(2) -0.3615(2) 0.5922(2) 0.0401(9) Uani 1 1 d . . . N4 N 0.0623(2) 0.1503(2) 0.8042(2) 0.0197(8) Uani 1 1 d . . . N5 N 0.1149(2) -0.1956(2) 0.9146(2) 0.0229(8) Uani 1 1 d . . . C35 C 0.0423(3) 0.0417(3) 0.6298(2) 0.0211(9) Uani 1 1 d . . . O4 O 0.0703(2) -0.2152(2) 0.55458(18) 0.0409(9) Uani 1 1 d . . . C2 C -0.0019(3) 0.0844(3) 0.8639(2) 0.0220(10) Uani 1 1 d . . . H2A H -0.0370 0.0743 0.8868 0.026 Uiso 1 1 calc R . . N3 N 0.1556(2) -0.1709(2) 0.8748(2) 0.0216(8) Uani 1 1 d . . . O5 O 0.1959(3) 0.0133(3) 1.1577(3) 0.0744(14) Uani 1 1 d . . . C34 C 0.1115(3) 0.1002(3) 0.6474(2) 0.0208(9) Uani 1 1 d . . . C47 C 0.4087(3) -0.0098(3) 1.0278(3) 0.0273(10) Uani 1 1 d . . . H7A H 0.4560 -0.0175 1.0757 0.033 Uiso 1 1 calc R . . C37 C -0.0918(3) -0.0132(3) 0.5531(3) 0.0302(11) Uani 1 1 d . . . H8A H -0.1425 -0.0107 0.5080 0.036 Uiso 1 1 calc R . . C36 C -0.0310(3) 0.0456(3) 0.5628(3) 0.0264(10) Uani 1 1 d . . . H9A H -0.0394 0.0882 0.5241 0.032 Uiso 1 1 calc R . . O6 O 0.0748(2) 0.0395(4) 1.0465(2) 0.0708(15) Uani 1 1 d . . . C44 C 0.3166(3) -0.0830(3) 0.8197(3) 0.0220(10) Uani 1 1 d . . . C4 C 0.0510(3) 0.0265(3) 0.8571(2) 0.0198(9) Uani 1 1 d . . . C49 C 0.2779(3) 0.0524(3) 0.9533(2) 0.0236(10) Uani 1 1 d . . . H11A H 0.2353 0.0891 0.9506 0.028 Uiso 1 1 calc R . . C30 C 0.2422(3) 0.1393(3) 0.7380(3) 0.0209(9) Uani 1 1 d . . . H12A H 0.2863 0.1334 0.7883 0.025 Uiso 1 1 calc R . . C38 C -0.0783(3) -0.0754(3) 0.6091(3) 0.0285(11) Uani 1 1 d . . . H13A H -0.1191 -0.1169 0.6029 0.034 Uiso 1 1 calc R . . C31 C 0.2488(3) 0.1975(3) 0.6860(3) 0.0239(10) Uani 1 1 d . . . H14A H 0.2972 0.2301 0.7003 0.029 Uiso 1 1 calc R . . C1 C 0.0660(3) -0.1311(3) 0.9176(3) 0.0252(10) Uani 1 1 d . . . H1A H 0.0320 -0.1328 0.9425 0.030 Uiso 1 1 calc R . . C11 C 0.0518(3) -0.3483(3) 0.8162(3) 0.0343(12) Uani 1 1 d . . . H27A H 0.0714 -0.2968 0.7975 0.041 Uiso 1 1 calc R . . C17 C -0.0362(3) 0.2420(3) 0.8156(3) 0.0198(9) Uani 1 1 d . . . C33 C 0.1140(3) 0.1586(3) 0.5939(3) 0.0248(10) Uani 1 1 d . . . H15A H 0.0684 0.1653 0.5445 0.030 Uiso 1 1 calc R . . C10 C 0.1036(3) -0.3555(3) 0.9027(3) 0.0261(10) Uani 1 1 d . . . C46 C 0.4011(3) -0.0510(3) 0.9617(3) 0.0260(10) Uani 1 1 d . . . H16A H 0.4438 -0.0872 0.9637 0.031 Uiso 1 1 calc R . . O7 O 0.1948(2) 0.0991(3) 1.0581(2) 0.0592(12) Uani 1 1 d . . . C23 C -0.1211(3) 0.1880(3) 0.6767(3) 0.0298(11) Uani 1 1 d . . . H24A H -0.0760 0.1446 0.6929 0.036 Uiso 1 1 calc R . . C45 C 0.3323(3) -0.0403(3) 0.8929(3) 0.0219(10) Uani 1 1 d . . . C32 C 0.1842(3) 0.2073(3) 0.6133(3) 0.0260(10) Uani 1 1 d . . . H18A H 0.1875 0.2469 0.5769 0.031 Uiso 1 1 calc R . . C40 C 0.2200(3) -0.1178(3) 0.6949(3) 0.0259(10) Uani 1 1 d . . . H19A H 0.1653 -0.1158 0.6557 0.031 Uiso 1 1 calc R . . C48 C 0.3460(3) 0.0434(3) 1.0231(3) 0.0270(10) Uani 1 1 d . . . H20A H 0.3501 0.0734 1.0677 0.032 Uiso 1 1 calc R . . C41 C 0.2762(3) -0.1599(3) 0.6790(3) 0.0308(11) Uani 1 1 d . . . H21A H 0.2607 -0.1864 0.6299 0.037 Uiso 1 1 calc R . . C22 C -0.0962(3) 0.2567(3) 0.7406(3) 0.0250(10) Uani 1 1 d . . . C19 C -0.0557(3) 0.3810(3) 0.8580(3) 0.0296(11) Uani 1 1 d . . . H29A H -0.0426 0.4245 0.8969 0.035 Uiso 1 1 calc R . . C18 C -0.0134(3) 0.3017(3) 0.8769(3) 0.0236(10) Uani 1 1 d . . . C6 C 0.1799(3) -0.2837(3) 1.0316(3) 0.0251(10) Uani 1 1 d . . . C26 C 0.0540(3) 0.2828(3) 0.9564(3) 0.0280(11) Uani 1 1 d . . . H32A H 0.0493 0.2200 0.9684 0.034 Uiso 1 1 calc R . . C39 C -0.0042(3) -0.0765(3) 0.6747(3) 0.0267(10) Uani 1 1 d . . . H39A H 0.0050 -0.1197 0.7131 0.032 Uiso 1 1 calc R . . C20 C -0.1156(3) 0.3976(3) 0.7846(3) 0.0306(11) Uani 1 1 d . . . H33A H -0.1432 0.4521 0.7739 0.037 Uiso 1 1 calc R . . C24 C -0.1342(3) 0.2265(3) 0.5995(3) 0.0396(13) Uani 1 1 d . . . H34C H -0.1500 0.1799 0.5606 0.048 Uiso 1 1 calc R . . H34B H -0.0839 0.2538 0.6052 0.048 Uiso 1 1 calc R . . H34A H -0.1772 0.2707 0.5828 0.048 Uiso 1 1 calc R . . C9 C 0.1251(3) -0.4357(3) 0.9411(3) 0.0353(12) Uani 1 1 d . . . H35A H 0.1082 -0.4882 0.9118 0.042 Uiso 1 1 calc R . . C14 C 0.2117(3) -0.2011(3) 1.0802(3) 0.0276(11) Uani 1 1 d . . . H36A H 0.1674 -0.1565 1.0596 0.033 Uiso 1 1 calc R . . C3 C 0.0764(3) -0.0631(3) 0.8769(3) 0.0242(10) Uani 1 1 d . . . C21 C -0.1365(3) 0.3369(3) 0.7264(3) 0.0294(11) Uani 1 1 d . . . H37A H -0.1786 0.3496 0.6762 0.035 Uiso 1 1 calc R . . C28 C 0.1372(3) 0.2948(3) 0.9575(3) 0.0325(12) Uani 1 1 d . . . H44C H 0.1804 0.2821 1.0095 0.039 Uiso 1 1 calc R . . H44B H 0.1426 0.3553 0.9435 0.039 Uiso 1 1 calc R . . H44A H 0.1417 0.2547 0.9200 0.039 Uiso 1 1 calc R . . C7 C 0.1983(3) -0.3670(3) 1.0659(3) 0.0341(12) Uani 1 1 d . . . H40A H 0.2301 -0.3725 1.1204 0.041 Uiso 1 1 calc R . . C43 C 0.3755(3) -0.1251(3) 0.8062(3) 0.0291(11) Uani 1 1 d . . . H45A H 0.4297 -0.1276 0.8461 0.035 Uiso 1 1 calc R . . C16 C 0.2354(3) -0.2144(4) 1.1660(3) 0.0407(13) Uani 1 1 d . . . H41C H 0.2551 -0.1590 1.1937 0.049 Uiso 1 1 calc R . . H41B H 0.2784 -0.2586 1.1876 0.049 Uiso 1 1 calc R . . H41A H 0.1881 -0.2342 1.1717 0.049 Uiso 1 1 calc R . . C8 C 0.1702(3) -0.4407(3) 1.0204(3) 0.0376(13) Uani 1 1 d . . . H42A H 0.1823 -0.4966 1.0445 0.045 Uiso 1 1 calc R . . C15 C 0.2838(3) -0.1639(3) 1.0717(3) 0.0391(13) Uani 1 1 d . . . H43C H 0.3030 -0.1107 1.1031 0.047 Uiso 1 1 calc R . . H43B H 0.2671 -0.1499 1.0172 0.047 Uiso 1 1 calc R . . H43A H 0.3275 -0.2073 1.0896 0.047 Uiso 1 1 calc R . . C42 C 0.3561(3) -0.1631(3) 0.7360(3) 0.0346(12) Uani 1 1 d . . . H46A H 0.3965 -0.1911 0.7264 0.042 Uiso 1 1 calc R . . C27 C 0.0510(3) 0.3380(4) 1.0204(3) 0.0381(13) Uani 1 1 d . . . H47C H 0.0964 0.3221 1.0703 0.046 Uiso 1 1 calc R . . H47B H -0.0003 0.3273 1.0224 0.046 Uiso 1 1 calc R . . H47A H 0.0549 0.4001 1.0099 0.046 Uiso 1 1 calc R . . O8 O 0.1383(3) 0.1505(3) 1.1353(3) 0.0826(16) Uani 1 1 d . . . C25 C -0.1967(3) 0.1390(4) 0.6694(3) 0.0463(14) Uani 1 1 d . . . H48C H -0.2124 0.0948 0.6284 0.056 Uiso 1 1 calc R . . H48B H -0.2413 0.1806 0.6565 0.056 Uiso 1 1 calc R . . H48A H -0.1846 0.1102 0.7187 0.056 Uiso 1 1 calc R . . C12 C 0.0570(4) -0.4287(3) 0.7722(3) 0.0472(15) Uani 1 1 d . . . H49C H 0.0229 -0.4201 0.7165 0.057 Uiso 1 1 calc R . . H49B H 0.0382 -0.4803 0.7896 0.057 Uiso 1 1 calc R . . H49A H 0.1134 -0.4376 0.7822 0.057 Uiso 1 1 calc R . . C13 C -0.0374(3) -0.3315(4) 0.7967(3) 0.0494(15) Uani 1 1 d . . . H50C H -0.0699 -0.3269 0.7404 0.059 Uiso 1 1 calc R . . H50B H -0.0415 -0.2769 0.8212 0.059 Uiso 1 1 calc R . . H50A H -0.0576 -0.3802 0.8162 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01538(17) 0.01528(16) 0.01918(17) 0.00060(14) 0.00729(12) 0.00035(15) N2 0.0178(19) 0.0205(19) 0.022(2) 0.0024(15) 0.0084(16) 0.0014(16) N9 0.0161(18) 0.0186(18) 0.0190(19) 0.0001(15) 0.0079(15) -0.0005(15) N1 0.0173(19) 0.0189(19) 0.0211(19) 0.0027(15) 0.0078(16) 0.0000(15) N7 0.0186(18) 0.0173(18) 0.0236(19) 0.0029(16) 0.0102(15) -0.0003(16) N8 0.021(2) 0.0151(18) 0.026(2) -0.0005(15) 0.0135(17) -0.0012(15) N10 0.0178(19) 0.020(2) 0.027(2) -0.0008(15) 0.0109(16) -0.0001(15) Cl1 0.0218(6) 0.0244(6) 0.0251(6) -0.0019(4) 0.0052(4) -0.0011(5) Cl2 0.0235(6) 0.0370(7) 0.0366(7) 0.0016(5) 0.0104(5) -0.0044(5) O1 0.0336(19) 0.0319(19) 0.0213(17) -0.0028(14) 0.0043(14) -0.0018(15) N6 0.0176(19) 0.0194(19) 0.024(2) -0.0008(16) 0.0066(16) -0.0007(16) O2 0.0197(17) 0.0322(19) 0.040(2) 0.0002(16) 0.0063(15) 0.0006(15) C5 0.025(2) 0.021(2) 0.033(3) 0.009(2) 0.016(2) 0.005(2) O3 0.031(2) 0.032(2) 0.043(2) -0.0119(17) 0.0044(16) 0.0047(16) N4 0.0190(19) 0.0170(18) 0.024(2) -0.0010(15) 0.0108(16) 0.0008(15) N5 0.022(2) 0.0198(19) 0.030(2) 0.0057(16) 0.0148(17) 0.0052(16) C35 0.018(2) 0.020(2) 0.022(2) 0.0004(19) 0.0067(19) 0.0035(19) O4 0.033(2) 0.056(2) 0.0251(18) 0.0075(17) 0.0053(16) -0.0100(18) C2 0.018(2) 0.019(2) 0.027(2) 0.0040(19) 0.0091(19) 0.0006(18) N3 0.023(2) 0.0192(19) 0.024(2) 0.0026(16) 0.0118(16) 0.0007(16) O5 0.081(3) 0.052(3) 0.067(3) 0.024(2) 0.013(3) 0.011(2) C34 0.015(2) 0.021(2) 0.024(2) -0.0032(19) 0.0067(18) -0.0001(18) C47 0.021(2) 0.026(2) 0.026(2) 0.008(2) 0.0016(19) -0.002(2) C37 0.021(2) 0.033(3) 0.028(2) -0.012(2) 0.0043(19) 0.001(2) C36 0.024(2) 0.028(3) 0.025(2) -0.003(2) 0.009(2) -0.001(2) O6 0.041(2) 0.122(4) 0.042(2) -0.009(3) 0.012(2) -0.045(3) C44 0.021(2) 0.017(2) 0.031(3) 0.0025(19) 0.015(2) 0.0009(18) C4 0.018(2) 0.019(2) 0.020(2) 0.0028(17) 0.0062(18) -0.0013(17) C49 0.023(2) 0.021(2) 0.026(2) 0.0008(19) 0.010(2) 0.003(2) C30 0.019(2) 0.019(2) 0.023(2) -0.0011(19) 0.0085(19) -0.0029(19) C38 0.019(2) 0.027(3) 0.037(3) -0.009(2) 0.010(2) -0.009(2) C31 0.021(2) 0.023(2) 0.027(2) 0.0000(19) 0.010(2) -0.0031(19) C1 0.026(3) 0.024(2) 0.028(3) 0.006(2) 0.015(2) 0.003(2) C11 0.047(3) 0.023(3) 0.034(3) 0.004(2) 0.019(2) -0.002(2) C17 0.016(2) 0.013(2) 0.033(3) 0.0028(18) 0.0127(19) 0.0000(17) C33 0.024(2) 0.024(2) 0.024(2) 0.0002(19) 0.008(2) 0.000(2) C10 0.026(3) 0.023(2) 0.034(3) 0.003(2) 0.017(2) 0.002(2) C46 0.021(2) 0.025(2) 0.029(3) 0.008(2) 0.009(2) 0.003(2) O7 0.040(2) 0.092(3) 0.054(3) -0.010(2) 0.028(2) -0.024(2) C23 0.024(3) 0.031(3) 0.028(3) -0.001(2) 0.006(2) 0.006(2) C45 0.019(2) 0.016(2) 0.031(3) 0.0021(19) 0.011(2) -0.0004(19) C32 0.033(3) 0.022(2) 0.025(2) 0.0054(19) 0.015(2) 0.001(2) C40 0.028(3) 0.021(2) 0.030(3) -0.001(2) 0.015(2) -0.004(2) C48 0.030(3) 0.024(2) 0.023(2) -0.001(2) 0.009(2) -0.004(2) C41 0.036(3) 0.026(3) 0.034(3) -0.011(2) 0.019(2) -0.002(2) C22 0.022(2) 0.026(2) 0.028(2) 0.003(2) 0.012(2) 0.002(2) C19 0.031(3) 0.019(2) 0.039(3) -0.004(2) 0.017(2) -0.003(2) C18 0.018(2) 0.024(2) 0.030(3) 0.000(2) 0.012(2) -0.0026(19) C6 0.020(2) 0.027(2) 0.031(3) 0.005(2) 0.014(2) 0.002(2) C26 0.026(3) 0.025(2) 0.031(3) 0.004(2) 0.012(2) 0.002(2) C39 0.025(2) 0.019(2) 0.038(3) -0.004(2) 0.016(2) -0.005(2) C20 0.032(3) 0.022(2) 0.039(3) 0.006(2) 0.018(2) 0.009(2) C24 0.044(3) 0.039(3) 0.033(3) 0.001(2) 0.016(3) 0.006(3) C9 0.038(3) 0.020(2) 0.049(3) 0.003(2) 0.021(3) 0.002(2) C14 0.018(2) 0.027(3) 0.033(3) 0.004(2) 0.007(2) 0.003(2) C3 0.023(2) 0.025(2) 0.026(2) -0.002(2) 0.013(2) 0.000(2) C21 0.031(3) 0.027(3) 0.029(3) 0.010(2) 0.012(2) 0.006(2) C28 0.026(3) 0.039(3) 0.029(3) -0.004(2) 0.009(2) -0.001(2) C7 0.023(3) 0.035(3) 0.039(3) 0.011(2) 0.009(2) 0.006(2) C43 0.022(2) 0.024(2) 0.041(3) 0.003(2) 0.014(2) 0.005(2) C16 0.039(3) 0.045(3) 0.037(3) -0.002(3) 0.016(3) -0.010(3) C8 0.034(3) 0.023(3) 0.049(3) 0.011(2) 0.013(3) 0.004(2) C15 0.044(3) 0.036(3) 0.036(3) -0.006(2) 0.017(3) -0.017(3) C42 0.037(3) 0.024(3) 0.052(3) -0.003(2) 0.029(3) 0.003(2) C27 0.031(3) 0.049(3) 0.033(3) -0.004(2) 0.014(2) -0.006(3) O8 0.084(4) 0.074(3) 0.099(4) -0.021(3) 0.049(3) 0.012(3) C25 0.051(4) 0.046(3) 0.037(3) -0.007(3) 0.016(3) -0.017(3) C12 0.077(4) 0.033(3) 0.047(3) -0.007(3) 0.040(3) -0.016(3) C13 0.042(3) 0.055(4) 0.039(3) -0.007(3) 0.008(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N2 2.052(3) . ? Ru1 N8 2.059(3) . ? Ru1 N9 2.062(3) . ? Ru1 N1 2.065(3) . ? Ru1 N10 2.068(4) . ? Ru1 N7 2.070(3) . ? N2 N4 1.315(5) . ? N2 C4 1.361(5) . ? N9 C30 1.340(5) . ? N9 C34 1.357(5) . ? N1 N3 1.306(5) . ? N1 C3 1.376(5) . ? N7 C49 1.355(5) . ? N7 C45 1.368(5) . ? N8 C40 1.342(6) . ? N8 C44 1.360(6) . ? N10 C39 1.343(5) . ? N10 C35 1.373(6) . ? Cl1 O4 1.428(3) . ? Cl1 O3 1.435(3) . ? Cl1 O1 1.438(3) . ? Cl1 O2 1.443(3) . ? Cl2 O5 1.409(4) . ? Cl2 O7 1.416(4) . ? Cl2 O6 1.417(4) . ? Cl2 O8 1.437(5) . ? N6 N4 1.348(5) . ? N6 C2 1.352(5) . ? N6 C17 1.455(5) . ? C5 C6 1.400(6) . ? C5 C10 1.410(6) . ? C5 N5 1.455(5) . ? N5 N3 1.353(5) . ? N5 C1 1.357(6) . ? C35 C36 1.390(6) . ? C35 C34 1.469(6) . ? C2 C4 1.370(6) . ? C34 C33 1.384(6) . ? C47 C46 1.374(6) . ? C47 C48 1.385(7) . ? C37 C38 1.377(7) . ? C37 C36 1.384(7) . ? C44 C43 1.388(6) . ? C44 C45 1.466(6) . ? C4 C3 1.442(6) . ? C49 C48 1.374(6) . ? C30 C31 1.388(6) . ? C38 C39 1.383(6) . ? C31 C32 1.381(6) . ? C1 C3 1.371(6) . ? C11 C10 1.509(6) . ? C11 C12 1.523(7) . ? C11 C13 1.539(7) . ? C17 C22 1.390(6) . ? C17 C18 1.401(6) . ? C33 C32 1.393(6) . ? C10 C9 1.394(6) . ? C46 C45 1.373(6) . ? C23 C24 1.520(7) . ? C23 C22 1.524(6) . ? C23 C25 1.536(7) . ? C40 C41 1.371(6) . ? C41 C42 1.387(7) . ? C22 C21 1.394(6) . ? C19 C20 1.372(7) . ? C19 C18 1.398(6) . ? C18 C26 1.506(6) . ? C6 C7 1.403(6) . ? C6 C14 1.522(6) . ? C26 C27 1.521(7) . ? C26 C28 1.542(6) . ? C20 C21 1.372(7) . ? C9 C8 1.377(7) . ? C14 C15 1.525(7) . ? C14 C16 1.527(7) . ? C7 C8 1.377(7) . ? C43 C42 1.368(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru1 N8 176.11(14) . . ? N2 Ru1 N9 96.48(14) . . ? N8 Ru1 N9 86.66(13) . . ? N2 Ru1 N1 76.92(14) . . ? N8 Ru1 N1 100.14(14) . . ? N9 Ru1 N1 171.88(13) . . ? N2 Ru1 N10 82.89(14) . . ? N8 Ru1 N10 100.01(14) . . ? N9 Ru1 N10 79.03(13) . . ? N1 Ru1 N10 95.31(14) . . ? N2 Ru1 N7 98.69(14) . . ? N8 Ru1 N7 78.42(14) . . ? N9 Ru1 N7 100.73(13) . . ? N1 Ru1 N7 85.09(13) . . ? N10 Ru1 N7 178.42(14) . . ? N4 N2 C4 111.0(3) . . ? N4 N2 Ru1 131.1(3) . . ? C4 N2 Ru1 117.5(3) . . ? C30 N9 C34 119.7(4) . . ? C30 N9 Ru1 125.1(3) . . ? C34 N9 Ru1 115.1(3) . . ? N3 N1 C3 111.4(3) . . ? N3 N1 Ru1 131.7(3) . . ? C3 N1 Ru1 116.8(3) . . ? C49 N7 C45 117.9(4) . . ? C49 N7 Ru1 125.1(3) . . ? C45 N7 Ru1 115.7(3) . . ? C40 N8 C44 118.5(4) . . ? C40 N8 Ru1 125.6(3) . . ? C44 N8 Ru1 115.7(3) . . ? C39 N10 C35 118.2(4) . . ? C39 N10 Ru1 126.2(3) . . ? C35 N10 Ru1 115.2(3) . . ? O4 Cl1 O3 109.7(2) . . ? O4 Cl1 O1 109.0(2) . . ? O3 Cl1 O1 109.4(2) . . ? O4 Cl1 O2 109.2(2) . . ? O3 Cl1 O2 109.5(2) . . ? O1 Cl1 O2 110.1(2) . . ? O5 Cl2 O7 110.7(3) . . ? O5 Cl2 O6 111.2(3) . . ? O7 Cl2 O6 109.6(2) . . ? O5 Cl2 O8 108.0(3) . . ? O7 Cl2 O8 108.6(3) . . ? O6 Cl2 O8 108.7(3) . . ? N4 N6 C2 112.0(3) . . ? N4 N6 C17 116.7(3) . . ? C2 N6 C17 131.2(4) . . ? C6 C5 C10 125.3(4) . . ? C6 C5 N5 116.9(4) . . ? C10 C5 N5 117.8(4) . . ? N2 N4 N6 105.2(3) . . ? N3 N5 C1 112.1(3) . . ? N3 N5 C5 117.7(3) . . ? C1 N5 C5 130.0(4) . . ? N10 C35 C36 121.2(4) . . ? N10 C35 C34 114.1(4) . . ? C36 C35 C34 124.7(4) . . ? N6 C2 C4 104.6(4) . . ? N1 N3 N5 105.0(3) . . ? N9 C34 C33 121.2(4) . . ? N9 C34 C35 116.1(4) . . ? C33 C34 C35 122.7(4) . . ? C46 C47 C48 118.6(4) . . ? C38 C37 C36 119.7(4) . . ? C37 C36 C35 119.2(4) . . ? N8 C44 C43 120.5(4) . . ? N8 C44 C45 115.4(4) . . ? C43 C44 C45 124.1(4) . . ? N2 C4 C2 107.2(4) . . ? N2 C4 C3 114.3(4) . . ? C2 C4 C3 138.4(4) . . ? N7 C49 C48 122.3(4) . . ? N9 C30 C31 121.6(4) . . ? C37 C38 C39 118.8(4) . . ? C32 C31 C30 119.2(4) . . ? N5 C1 C3 104.8(4) . . ? C10 C11 C12 113.1(4) . . ? C10 C11 C13 110.8(4) . . ? C12 C11 C13 109.2(5) . . ? C22 C17 C18 124.8(4) . . ? C22 C17 N6 117.3(4) . . ? C18 C17 N6 118.0(4) . . ? C34 C33 C32 119.1(4) . . ? C9 C10 C5 114.8(4) . . ? C9 C10 C11 122.6(4) . . ? C5 C10 C11 122.5(4) . . ? C45 C46 C47 120.4(4) . . ? C24 C23 C22 112.7(4) . . ? C24 C23 C25 111.4(4) . . ? C22 C23 C25 109.8(4) . . ? N7 C45 C46 121.3(4) . . ? N7 C45 C44 113.6(4) . . ? C46 C45 C44 125.0(4) . . ? C31 C32 C33 119.1(4) . . ? N8 C40 C41 123.0(4) . . ? C49 C48 C47 119.4(4) . . ? C40 C41 C42 118.8(5) . . ? C17 C22 C21 116.8(4) . . ? C17 C22 C23 122.7(4) . . ? C21 C22 C23 120.5(4) . . ? C20 C19 C18 121.6(4) . . ? C19 C18 C17 115.1(4) . . ? C19 C18 C26 122.7(4) . . ? C17 C18 C26 122.1(4) . . ? C5 C6 C7 116.3(4) . . ? C5 C6 C14 122.5(4) . . ? C7 C6 C14 121.1(4) . . ? C18 C26 C27 113.9(4) . . ? C18 C26 C28 110.6(4) . . ? C27 C26 C28 109.2(4) . . ? N10 C39 C38 122.9(4) . . ? C19 C20 C21 121.3(4) . . ? C8 C9 C10 121.7(5) . . ? C6 C14 C15 110.8(4) . . ? C6 C14 C16 113.6(4) . . ? C15 C14 C16 109.3(4) . . ? C1 C3 N1 106.7(4) . . ? C1 C3 C4 139.4(4) . . ? N1 C3 C4 113.9(4) . . ? C20 C21 C22 120.4(4) . . ? C8 C7 C6 119.9(5) . . ? C42 C43 C44 120.6(5) . . ? C9 C8 C7 121.9(5) . . ? C43 C42 C41 118.6(5) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 66.62 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.152 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 892295' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ru9a #TrackingRef 'SH25.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H28 Cl4 F6 N10 O8 Ru' _chemical_formula_weight 1121.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.199(2) _cell_length_b 12.433(2) _cell_length_c 16.087(3) _cell_angle_alpha 89.218(4) _cell_angle_beta 87.674(4) _cell_angle_gamma 88.700(4) _cell_volume 2237.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10966 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28 _exptl_crystal_description platelett _exptl_crystal_colour red _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.646 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 AXS' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31477 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 28.33 _reflns_number_total 10966 _reflns_number_gt 9419 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.1382P)^2^+11.8134P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10966 _refine_ls_number_parameters 646 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.2396 _refine_ls_wR_factor_gt 0.2254 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8135(5) 0.5170(4) 0.8022(3) 0.0341(11) Uani 1 1 d . . . H1 H 0.8652 0.4944 0.8447 0.041 Uiso 1 1 calc R . . C2 C 0.8353(5) 0.7747(4) 0.8826(3) 0.0350(11) Uani 1 1 d . . . H2 H 0.8883 0.7431 0.9210 0.042 Uiso 1 1 calc R . . C3 C 0.7735(4) 0.6195(4) 0.7844(3) 0.0287(9) Uani 1 1 d . . . C4 C 0.7802(5) 0.7259(4) 0.8191(3) 0.0288(9) Uani 1 1 d . . . C5 C 0.7694(5) 0.3410(4) 0.7366(3) 0.0312(10) Uani 1 1 d . . . C6 C 0.8496(9) 0.2974(6) 0.6810(6) 0.082(3) Uani 1 1 d . . . H6 H 0.8992 0.3427 0.6472 0.098 Uiso 1 1 calc R . . C7 C 0.8593(12) 0.1875(6) 0.6734(6) 0.100(4) Uani 1 1 d . . . H7 H 0.9196 0.1570 0.6371 0.120 Uiso 1 1 calc R . . C8 C 0.7829(8) 0.1219(5) 0.7175(4) 0.0515(17) Uani 1 1 d . . . H8 H 0.7877 0.0461 0.7104 0.062 Uiso 1 1 calc R . . C9 C 0.7020(7) 0.1649(5) 0.7704(4) 0.0474(14) Uani 1 1 d . . . H9 H 0.6496 0.1189 0.8014 0.057 Uiso 1 1 calc R . . C10 C 0.6918(6) 0.2753(5) 0.7817(4) 0.0435(13) Uani 1 1 d . . . C11 C 0.6009(14) 0.3222(8) 0.8422(11) 0.131(7) Uani 1 1 d . . . C12 C 0.8240(5) 0.9693(4) 0.9288(3) 0.0328(10) Uani 1 1 d . . . C13 C 0.9109(6) 1.0379(5) 0.8992(3) 0.0384(12) Uani 1 1 d . . . H13 H 0.9550 1.0233 0.8488 0.046 Uiso 1 1 calc R . . C14 C 0.9327(6) 1.1297(5) 0.9453(4) 0.0442(14) Uani 1 1 d . . . H14 H 0.9916 1.1786 0.9256 0.053 Uiso 1 1 calc R . . C15 C 0.8700(6) 1.1495(6) 1.0183(4) 0.0493(15) Uani 1 1 d . . . H15 H 0.8849 1.2123 1.0489 0.059 Uiso 1 1 calc R . . C16 C 0.7848(6) 1.0781(6) 1.0478(4) 0.0502(16) Uani 1 1 d . . . H16 H 0.7433 1.0914 1.0994 0.060 Uiso 1 1 calc R . . C17 C 0.7591(6) 0.9877(5) 1.0032(4) 0.0411(12) Uani 1 1 d . . . C18 C 0.6676(7) 0.9104(7) 1.0362(4) 0.0558(17) Uani 1 1 d . . . C30 C 0.4600(6) 0.7021(5) 0.8430(3) 0.0388(12) Uani 1 1 d . . . H30 H 0.5229 0.7321 0.8724 0.047 Uiso 1 1 calc R . . C31 C 0.3619(7) 0.6640(5) 0.8875(4) 0.0496(15) Uani 1 1 d . . . H31 H 0.3587 0.6664 0.9465 0.060 Uiso 1 1 calc R . . C32 C 0.2693(7) 0.6227(6) 0.8465(5) 0.0574(18) Uani 1 1 d . . . H32 H 0.2007 0.5968 0.8765 0.069 Uiso 1 1 calc R . . C33 C 0.2770(6) 0.6191(6) 0.7605(5) 0.0512(16) Uani 1 1 d . . . H33 H 0.2134 0.5912 0.7306 0.061 Uiso 1 1 calc R . . C34 C 0.3785(5) 0.6565(4) 0.7183(4) 0.0354(11) Uani 1 1 d . . . C35 C 0.3979(5) 0.6507(4) 0.6273(4) 0.0354(11) Uani 1 1 d . . . C36 C 0.3144(6) 0.6107(6) 0.5744(4) 0.0498(15) Uani 1 1 d . . . H36 H 0.2377 0.5903 0.5956 0.060 Uiso 1 1 calc R . . C37 C 0.3450(6) 0.6012(6) 0.4908(4) 0.0512(16) Uani 1 1 d . . . H37 H 0.2888 0.5757 0.4535 0.061 Uiso 1 1 calc R . . C38 C 0.4580(6) 0.6291(5) 0.4618(4) 0.0419(13) Uani 1 1 d . . . H38 H 0.4819 0.6200 0.4049 0.050 Uiso 1 1 calc R . . C39 C 0.5362(5) 0.6708(4) 0.5175(3) 0.0329(10) Uani 1 1 d . . . H39 H 0.6133 0.6912 0.4972 0.040 Uiso 1 1 calc R . . C40 C 0.4290(5) 0.9369(4) 0.6955(3) 0.0364(11) Uani 1 1 d . . . H40 H 0.3852 0.8912 0.7327 0.044 Uiso 1 1 calc R . . C41 C 0.3831(6) 1.0396(5) 0.6793(4) 0.0424(13) Uani 1 1 d . . . H41 H 0.3096 1.0637 0.7050 0.051 Uiso 1 1 calc R . . C42 C 0.4467(6) 1.1052(5) 0.6251(4) 0.0460(14) Uani 1 1 d . . . H42 H 0.4180 1.1762 0.6138 0.055 Uiso 1 1 calc R . . C43 C 0.5521(6) 1.0681(4) 0.5871(4) 0.0414(13) Uani 1 1 d . . . H43 H 0.5958 1.1127 0.5488 0.050 Uiso 1 1 calc R . . C44 C 0.5939(5) 0.9641(4) 0.6055(3) 0.0320(10) Uani 1 1 d . . . C45 C 0.7057(5) 0.9161(4) 0.5703(3) 0.0314(10) Uani 1 1 d . . . C46 C 0.7785(6) 0.9672(5) 0.5105(3) 0.0389(12) Uani 1 1 d . . . H46 H 0.7576 1.0372 0.4907 0.047 Uiso 1 1 calc R . . C47 C 0.8812(6) 0.9153(5) 0.4802(4) 0.0417(13) Uani 1 1 d . . . H47 H 0.9308 0.9483 0.4384 0.050 Uiso 1 1 calc R . . C48 C 0.9110(6) 0.8136(5) 0.5121(4) 0.0411(12) Uani 1 1 d . . . H48 H 0.9824 0.7773 0.4933 0.049 Uiso 1 1 calc R . . C49 C 0.8359(5) 0.7668(5) 0.5710(3) 0.0367(11) Uani 1 1 d . . . H49 H 0.8565 0.6974 0.5921 0.044 Uiso 1 1 calc R . . C100 C 1.1641(13) 0.3393(8) 0.7714(9) 0.150(6) Uani 1 1 d DU . . H10A H 1.2031 0.3513 0.8245 0.180 Uiso 1 1 calc R . . H10B H 1.0962 0.3909 0.7656 0.180 Uiso 1 1 calc R . . N1 N 0.7016(4) 0.6139(3) 0.7178(2) 0.0250(7) Uani 1 1 d . . . N2 N 0.7109(4) 0.8025(3) 0.7808(2) 0.0265(8) Uani 1 1 d . . . N3 N 0.6940(4) 0.5143(3) 0.6937(2) 0.0269(8) Uani 1 1 d . . . N4 N 0.7197(4) 0.8958(3) 0.8161(2) 0.0290(8) Uani 1 1 d . . . N5 N 0.7625(4) 0.4557(3) 0.7453(3) 0.0288(8) Uani 1 1 d . . . N6 N 0.7964(4) 0.8789(3) 0.8778(3) 0.0312(9) Uani 1 1 d . . . N7 N 0.4698(4) 0.6984(3) 0.7594(3) 0.0290(8) Uani 1 1 d . . . N8 N 0.5076(4) 0.6834(3) 0.5984(3) 0.0269(8) Uani 1 1 d . . . N9 N 0.5328(4) 0.8995(3) 0.6607(2) 0.0281(8) Uani 1 1 d . . . N10 N 0.7333(4) 0.8159(3) 0.6001(3) 0.0288(8) Uani 1 1 d . . . O1 O 0.1241(16) 0.4600(13) 0.0061(9) 0.096(5) Uani 0.50 1 d P . . O2 O 0.0004(8) 0.5804(7) -0.0571(6) 0.0444(19) Uani 0.50 1 d P . . O3 O -0.0802(18) 0.4197(14) -0.0187(9) 0.115(7) Uani 0.50 1 d P . . O4 O -0.0359(10) 0.5492(13) 0.0824(6) 0.075(4) Uani 0.50 1 d P . . O5 O 0.0245(7) 0.7629(7) 0.7269(6) 0.107(3) Uani 1 1 d . . . O6 O 0.1545(7) 0.8874(9) 0.7701(4) 0.113(3) Uani 1 1 d . . . O7 O 0.1557(5) 0.8473(5) 0.6324(3) 0.0608(13) Uani 1 1 d . . . O8 O -0.0105(6) 0.9372(6) 0.6908(4) 0.083(2) Uani 1 1 d . . . F1 F 0.5385(8) 0.2486(5) 0.8828(6) 0.149(4) Uani 1 1 d . . . F2 F 0.6449(18) 0.3791(8) 0.8957(8) 0.282(12) Uani 1 1 d . . . F3 F 0.5284(12) 0.3893(9) 0.8032(12) 0.293(12) Uani 1 1 d . . . F4 F 0.5825(4) 0.8928(4) 0.9826(3) 0.0671(13) Uani 1 1 d . . . F5 F 0.7168(5) 0.8124(4) 1.0530(3) 0.0705(13) Uani 1 1 d . . . F6 F 0.6114(5) 0.9437(5) 1.1065(3) 0.0715(14) Uani 1 1 d . . . Cl1 Cl 0.0000 0.5000 0.0000 0.0599(7) Uani 1 2 d S . . Cl2 Cl 0.08305(14) 0.86570(17) 0.70590(10) 0.0535(4) Uani 1 1 d . . . Cl5 Cl 1.1218(4) 0.2051(3) 0.7604(3) 0.1284(14) Uani 1 1 d D . . Cl6 Cl 1.2659(10) 0.3431(4) 0.6852(7) 0.393(9) Uani 1 1 d D . . Ru1 Ru 0.61030(3) 0.75214(3) 0.68483(2) 0.02412(14) Uani 1 1 d . . . Cl3 Cl 0.0267(4) 0.4904(3) 0.5399(3) 0.0650(10) Uani 0.50 1 d P . . O10 O 0.0549(5) 0.5828(5) 0.4943(4) 0.0709(16) Uani 1 1 d . . . O11 O 0.0024(13) 0.5356(10) 0.6494(18) 0.174(13) Uani 0.50 1 d P . . O9 O 0.1308(14) 0.4293(10) 0.5555(11) 0.090(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.044(3) 0.029(2) 0.029(2) 0.0037(19) -0.015(2) 0.000(2) C2 0.045(3) 0.030(2) 0.031(2) 0.0037(19) -0.014(2) -0.003(2) C3 0.034(2) 0.026(2) 0.027(2) 0.0045(17) -0.0084(18) -0.0024(18) C4 0.036(2) 0.025(2) 0.025(2) 0.0039(17) -0.0090(18) -0.0017(18) C5 0.043(3) 0.024(2) 0.027(2) 0.0047(18) -0.0047(19) 0.0022(19) C6 0.112(7) 0.035(4) 0.091(6) 0.016(4) 0.065(6) 0.018(4) C7 0.175(11) 0.035(4) 0.082(6) 0.006(4) 0.075(7) 0.021(5) C8 0.091(5) 0.026(3) 0.038(3) 0.003(2) -0.011(3) 0.004(3) C9 0.062(4) 0.033(3) 0.047(3) 0.010(2) -0.003(3) -0.011(3) C10 0.054(3) 0.033(3) 0.043(3) 0.008(2) 0.004(3) -0.006(2) C11 0.160(12) 0.035(4) 0.187(14) 0.020(7) 0.124(12) 0.001(6) C12 0.044(3) 0.028(2) 0.028(2) -0.0022(18) -0.011(2) -0.004(2) C13 0.053(3) 0.032(3) 0.031(2) -0.001(2) -0.008(2) -0.009(2) C14 0.056(4) 0.032(3) 0.047(3) -0.003(2) -0.018(3) -0.010(2) C15 0.053(4) 0.045(3) 0.052(4) -0.019(3) -0.016(3) 0.000(3) C16 0.052(4) 0.059(4) 0.040(3) -0.021(3) -0.006(3) -0.003(3) C17 0.045(3) 0.047(3) 0.033(3) -0.006(2) -0.009(2) -0.007(2) C18 0.063(4) 0.069(5) 0.036(3) -0.006(3) 0.002(3) -0.015(4) C30 0.051(3) 0.037(3) 0.028(2) 0.004(2) 0.001(2) -0.004(2) C31 0.064(4) 0.046(3) 0.037(3) 0.003(3) 0.014(3) -0.004(3) C32 0.053(4) 0.057(4) 0.061(4) -0.004(3) 0.026(3) -0.014(3) C33 0.040(3) 0.055(4) 0.058(4) -0.016(3) 0.010(3) -0.010(3) C34 0.035(3) 0.031(3) 0.040(3) -0.003(2) 0.000(2) 0.001(2) C35 0.035(3) 0.033(3) 0.038(3) -0.007(2) -0.005(2) 0.001(2) C36 0.038(3) 0.061(4) 0.051(4) -0.016(3) -0.008(3) -0.006(3) C37 0.049(3) 0.060(4) 0.047(3) -0.017(3) -0.018(3) -0.003(3) C38 0.056(3) 0.040(3) 0.031(3) -0.005(2) -0.011(2) -0.002(3) C39 0.045(3) 0.029(2) 0.026(2) 0.0012(18) -0.006(2) -0.002(2) C40 0.044(3) 0.031(3) 0.034(3) 0.003(2) -0.006(2) 0.002(2) C41 0.048(3) 0.035(3) 0.044(3) 0.002(2) -0.007(2) 0.008(2) C42 0.060(4) 0.029(3) 0.048(3) 0.007(2) -0.011(3) 0.007(3) C43 0.056(3) 0.025(2) 0.043(3) 0.009(2) -0.009(3) -0.001(2) C44 0.044(3) 0.027(2) 0.026(2) 0.0044(18) -0.010(2) -0.005(2) C45 0.041(3) 0.028(2) 0.026(2) 0.0031(18) -0.0085(19) -0.005(2) C46 0.051(3) 0.035(3) 0.031(2) 0.008(2) -0.005(2) -0.008(2) C47 0.053(3) 0.039(3) 0.033(3) 0.003(2) 0.004(2) -0.011(2) C48 0.043(3) 0.046(3) 0.034(3) 0.004(2) 0.001(2) -0.001(2) C49 0.043(3) 0.035(3) 0.032(2) 0.003(2) -0.003(2) -0.001(2) C100 0.145(9) 0.112(8) 0.196(10) 0.019(8) -0.054(8) -0.017(7) N1 0.0314(19) 0.0224(18) 0.0211(17) 0.0033(14) -0.0033(14) -0.0012(15) N2 0.035(2) 0.0248(19) 0.0206(17) 0.0030(14) -0.0066(15) -0.0045(15) N3 0.033(2) 0.0226(18) 0.0256(18) 0.0032(15) -0.0054(15) -0.0006(15) N4 0.041(2) 0.0247(19) 0.0219(18) 0.0043(15) -0.0072(16) -0.0052(16) N5 0.036(2) 0.0247(19) 0.0263(19) 0.0049(15) -0.0048(16) -0.0010(16) N6 0.043(2) 0.026(2) 0.0250(19) 0.0014(15) -0.0095(17) -0.0069(17) N7 0.036(2) 0.0223(19) 0.0282(19) 0.0007(15) -0.0016(16) 0.0013(16) N8 0.032(2) 0.0219(18) 0.0270(19) 0.0021(15) -0.0063(15) 0.0014(15) N9 0.039(2) 0.0236(19) 0.0223(18) 0.0020(14) -0.0081(15) 0.0004(16) N10 0.035(2) 0.028(2) 0.0237(18) 0.0031(15) -0.0064(15) -0.0035(16) O1 0.126(12) 0.096(10) 0.066(8) 0.001(7) -0.035(8) 0.054(9) O2 0.041(4) 0.045(5) 0.048(5) 0.016(4) -0.012(4) -0.010(4) O3 0.170(16) 0.105(11) 0.077(9) 0.030(8) -0.040(10) -0.098(12) O4 0.051(6) 0.136(12) 0.038(5) 0.000(6) -0.010(4) 0.004(6) O5 0.085(5) 0.094(5) 0.141(7) 0.049(5) 0.015(5) -0.018(4) O6 0.072(4) 0.213(10) 0.057(4) -0.035(5) -0.011(3) 0.004(5) O7 0.063(3) 0.073(4) 0.045(3) 0.006(2) 0.010(2) 0.005(3) O8 0.088(4) 0.100(5) 0.061(3) -0.016(3) -0.003(3) 0.038(4) F1 0.169(7) 0.067(4) 0.200(8) 0.025(4) 0.138(7) -0.010(4) F2 0.52(3) 0.084(6) 0.226(12) -0.086(7) 0.296(16) -0.127(10) F3 0.242(13) 0.146(8) 0.46(2) 0.179(12) 0.289(16) 0.124(9) F4 0.060(3) 0.098(4) 0.044(2) -0.013(2) 0.0016(18) -0.035(2) F5 0.089(3) 0.063(3) 0.059(3) 0.010(2) 0.011(2) -0.018(2) F6 0.079(3) 0.097(4) 0.039(2) -0.018(2) 0.013(2) -0.023(3) Cl1 0.0748(16) 0.0613(14) 0.0466(12) 0.0267(10) -0.0299(11) -0.0356(12) Cl2 0.0419(8) 0.0804(12) 0.0370(7) 0.0176(7) 0.0032(6) 0.0044(7) Cl5 0.120(3) 0.103(2) 0.157(4) -0.008(2) 0.041(3) 0.016(2) Cl6 0.512(15) 0.095(3) 0.530(15) 0.034(6) 0.434(14) 0.085(6) Ru1 0.0318(2) 0.0206(2) 0.02025(19) 0.00312(13) -0.00622(13) -0.00161(14) Cl3 0.056(2) 0.0469(18) 0.091(3) -0.0071(18) 0.0216(19) -0.0162(15) O10 0.059(3) 0.084(4) 0.071(4) 0.000(3) -0.007(3) -0.010(3) O11 0.083(9) 0.045(7) 0.38(3) 0.089(12) 0.137(15) 0.035(6) O9 0.095(10) 0.053(7) 0.126(12) -0.004(7) -0.025(9) -0.022(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N5 1.351(7) . ? C1 C3 1.371(7) . ? C1 H1 0.9500 . ? C2 N6 1.360(7) . ? C2 C4 1.369(7) . ? C2 H2 0.9500 . ? C3 N1 1.369(6) . ? C3 C4 1.448(7) . ? C4 N2 1.370(6) . ? C5 C6 1.352(9) . ? C5 C10 1.383(8) . ? C5 N5 1.435(6) . ? C6 C7 1.374(11) . ? C6 H6 0.9500 . ? C7 C8 1.368(12) . ? C7 H7 0.9500 . ? C8 C9 1.326(10) . ? C8 H8 0.9500 . ? C9 C10 1.389(9) . ? C9 H9 0.9500 . ? C10 C11 1.494(12) . ? C11 F2 1.25(2) . ? C11 F1 1.315(10) . ? C11 F3 1.32(2) . ? C12 C13 1.375(8) . ? C12 C17 1.393(8) . ? C12 N6 1.447(6) . ? C13 C14 1.402(8) . ? C13 H13 0.9500 . ? C14 C15 1.366(10) . ? C14 H14 0.9500 . ? C15 C16 1.383(10) . ? C15 H15 0.9500 . ? C16 C17 1.384(8) . ? C16 H16 0.9500 . ? C17 C18 1.497(10) . ? C18 F4 1.335(8) . ? C18 F6 1.338(8) . ? C18 F5 1.354(10) . ? C30 N7 1.348(7) . ? C30 C31 1.375(9) . ? C30 H30 0.9500 . ? C31 C32 1.365(11) . ? C31 H31 0.9500 . ? C32 C33 1.384(10) . ? C32 H32 0.9500 . ? C33 C34 1.386(8) . ? C33 H33 0.9500 . ? C34 N7 1.357(7) . ? C34 C35 1.475(8) . ? C35 N8 1.364(7) . ? C35 C36 1.394(8) . ? C36 C37 1.380(10) . ? C36 H36 0.9500 . ? C37 C38 1.381(10) . ? C37 H37 0.9500 . ? C38 C39 1.391(7) . ? C38 H38 0.9500 . ? C39 N8 1.337(6) . ? C39 H39 0.9500 . ? C40 N9 1.344(7) . ? C40 C41 1.391(8) . ? C40 H40 0.9500 . ? C41 C42 1.374(9) . ? C41 H41 0.9500 . ? C42 C43 1.381(10) . ? C42 H42 0.9500 . ? C43 C44 1.397(7) . ? C43 H43 0.9500 . ? C44 N9 1.363(6) . ? C44 C45 1.470(8) . ? C45 N10 1.362(6) . ? C45 C46 1.392(7) . ? C46 C47 1.380(9) . ? C46 H46 0.9500 . ? C47 C48 1.397(9) . ? C47 H47 0.9500 . ? C48 C49 1.373(8) . ? C48 H48 0.9500 . ? C49 N10 1.359(7) . ? C49 H49 0.9500 . ? C100 Cl5 1.758(9) . ? C100 Cl6 1.761(9) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? N1 N3 1.309(6) . ? N1 Ru1 2.054(4) . ? N2 N4 1.306(6) . ? N2 Ru1 2.060(4) . ? N3 N5 1.349(6) . ? N4 N6 1.350(6) . ? N7 Ru1 2.057(4) . ? N8 Ru1 2.048(4) . ? N9 Ru1 2.049(4) . ? N10 Ru1 2.062(4) . ? O1 Cl1 1.472(15) . ? O1 O3 1.58(2) 2_565 ? O1 O2 1.67(2) 2_565 ? O1 O4 1.771(17) 2_565 ? O2 Cl1 1.348(8) . ? O2 O3 1.542(17) 2_565 ? O2 O1 1.67(2) 2_565 ? O2 O4 1.702(18) 2_565 ? O3 Cl1 1.402(12) . ? O3 O2 1.542(17) 2_565 ? O3 O1 1.58(2) 2_565 ? O3 O4 1.67(2) 2_565 ? O4 Cl1 1.503(12) . ? O4 O3 1.67(2) 2_565 ? O4 O2 1.702(18) 2_565 ? O4 O1 1.771(17) 2_565 ? O5 Cl2 1.478(7) . ? O6 Cl2 1.365(7) . ? O7 Cl2 1.426(5) . ? O8 Cl2 1.385(6) . ? Cl1 O2 1.348(8) 2_565 ? Cl1 O3 1.402(12) 2_565 ? Cl1 O1 1.472(15) 2_565 ? Cl1 O4 1.503(12) 2_565 ? Cl3 O10 1.390(7) . ? Cl3 O9 1.406(16) . ? Cl3 O10 1.434(7) 2_566 ? Cl3 Cl3 1.453(10) 2_566 ? Cl3 O11 1.86(3) . ? O10 Cl3 1.434(7) 2_566 ? 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 N5 C1 C3 104.2(4) . . ? N5 C1 H1 127.9 . . ? C3 C1 H1 127.9 . . ? N6 C2 C4 103.9(4) . . ? N6 C2 H2 128.0 . . ? C4 C2 H2 128.0 . . ? N1 C3 C1 107.6(4) . . ? N1 C3 C4 114.3(4) . . ? C1 C3 C4 138.0(4) . . ? C2 C4 N2 107.6(4) . . ? C2 C4 C3 138.2(5) . . ? N2 C4 C3 114.2(4) . . ? C6 C5 C10 119.8(6) . . ? C6 C5 N5 119.2(5) . . ? C10 C5 N5 120.9(5) . . ? C5 C6 C7 119.9(7) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 120.6(8) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 119.4(6) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 121.8(6) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C5 C10 C9 118.4(6) . . ? C5 C10 C11 120.6(6) . . ? C9 C10 C11 121.0(6) . . ? F2 C11 F1 106.6(14) . . ? F2 C11 F3 103.7(13) . . ? F1 C11 F3 109.8(14) . . ? F2 C11 C10 113.4(14) . . ? F1 C11 C10 112.9(8) . . ? F3 C11 C10 110.0(13) . . ? C13 C12 C17 122.2(5) . . ? C13 C12 N6 117.7(5) . . ? C17 C12 N6 120.0(5) . . ? C12 C13 C14 118.2(6) . . ? C12 C13 H13 120.9 . . ? C14 C13 H13 120.9 . . ? C15 C14 C13 120.6(6) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.0(6) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 121.1(6) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C16 C17 C12 117.8(6) . . ? C16 C17 C18 120.6(6) . . ? C12 C17 C18 121.5(5) . . ? F4 C18 F6 106.3(6) . . ? F4 C18 F5 105.6(6) . . ? F6 C18 F5 106.7(6) . . ? F4 C18 C17 113.0(6) . . ? F6 C18 C17 112.8(6) . . ? F5 C18 C17 111.9(6) . . ? N7 C30 C31 122.3(6) . . ? N7 C30 H30 118.9 . . ? C31 C30 H30 118.9 . . ? C32 C31 C30 119.8(6) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 118.8(6) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.6 . . ? C32 C33 C34 119.4(6) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? N7 C34 C33 121.5(5) . . ? N7 C34 C35 115.0(5) . . ? C33 C34 C35 123.4(5) . . ? N8 C35 C36 121.9(5) . . ? N8 C35 C34 114.5(5) . . ? C36 C35 C34 123.6(5) . . ? C37 C36 C35 118.9(6) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C36 C37 C38 119.5(6) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C37 C38 C39 118.6(6) . . ? C37 C38 H38 120.7 . . ? C39 C38 H38 120.7 . . ? N8 C39 C38 123.0(5) . . ? N8 C39 H39 118.5 . . ? C38 C39 H39 118.5 . . ? N9 C40 C41 122.9(5) . . ? N9 C40 H40 118.6 . . ? C41 C40 H40 118.6 . . ? C42 C41 C40 118.3(6) . . ? C42 C41 H41 120.9 . . ? C40 C41 H41 120.9 . . ? C41 C42 C43 120.1(5) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C42 C43 C44 119.2(5) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? N9 C44 C43 121.0(5) . . ? N9 C44 C45 114.6(4) . . ? C43 C44 C45 124.3(5) . . ? N10 C45 C46 121.7(5) . . ? N10 C45 C44 114.9(4) . . ? C46 C45 C44 123.4(5) . . ? C47 C46 C45 119.4(5) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C46 C47 C48 118.9(5) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? C49 C48 C47 119.2(6) . . ? C49 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? N10 C49 C48 122.5(5) . . ? N10 C49 H49 118.7 . . ? C48 C49 H49 118.7 . . ? Cl5 C100 Cl6 96.8(6) . . ? Cl5 C100 H10A 112.4 . . ? Cl6 C100 H10A 112.4 . . ? Cl5 C100 H10B 112.4 . . ? Cl6 C100 H10B 112.4 . . ? H10A C100 H10B 110.0 . . ? N3 N1 C3 110.5(4) . . ? N3 N1 Ru1 131.8(3) . . ? C3 N1 Ru1 117.1(3) . . ? N4 N2 C4 110.8(4) . . ? N4 N2 Ru1 132.2(3) . . ? C4 N2 Ru1 116.9(3) . . ? N1 N3 N5 105.4(4) . . ? N2 N4 N6 105.3(4) . . ? N3 N5 C1 112.4(4) . . ? N3 N5 C5 119.1(4) . . ? C1 N5 C5 128.5(4) . . ? N4 N6 C2 112.3(4) . . ? N4 N6 C12 118.1(4) . . ? C2 N6 C12 129.6(4) . . ? C30 N7 C34 118.1(5) . . ? C30 N7 Ru1 126.6(4) . . ? C34 N7 Ru1 115.2(3) . . ? C39 N8 C35 118.0(4) . . ? C39 N8 Ru1 126.6(4) . . ? C35 N8 Ru1 115.4(3) . . ? C40 N9 C44 118.5(4) . . ? C40 N9 Ru1 125.4(4) . . ? C44 N9 Ru1 116.1(4) . . ? C49 N10 C45 118.2(4) . . ? C49 N10 Ru1 126.2(4) . . ? C45 N10 Ru1 115.5(4) . . ? Cl1 O1 O3 54.6(7) . 2_565 ? Cl1 O1 O2 50.3(6) . 2_565 ? O3 O1 O2 89.0(10) 2_565 2_565 ? Cl1 O1 O4 54.3(6) . 2_565 ? O3 O1 O4 90.4(9) 2_565 2_565 ? O2 O1 O4 83.5(9) 2_565 2_565 ? Cl1 O2 O3 57.6(6) . 2_565 ? Cl1 O2 O1 57.1(5) . 2_565 ? O3 O2 O1 96.8(9) 2_565 2_565 ? Cl1 O2 O4 57.7(5) . 2_565 ? O3 O2 O4 94.2(9) 2_565 2_565 ? O1 O2 O4 90.2(8) 2_565 2_565 ? Cl1 O3 O2 54.3(6) . 2_565 ? Cl1 O3 O1 58.9(9) . 2_565 ? O2 O3 O1 93.6(10) 2_565 2_565 ? Cl1 O3 O4 57.8(7) . 2_565 ? O2 O3 O4 91.0(10) 2_565 2_565 ? O1 O3 O4 94.7(11) 2_565 2_565 ? Cl1 O4 O3 52.1(6) . 2_565 ? Cl1 O4 O2 49.3(5) . 2_565 ? O3 O4 O2 85.0(9) 2_565 2_565 ? Cl1 O4 O1 52.6(6) . 2_565 ? O3 O4 O1 88.5(9) 2_565 2_565 ? O2 O4 O1 81.8(8) 2_565 2_565 ? O2 Cl1 O2 180.0(7) 2_565 . ? O2 Cl1 O3 111.9(7) 2_565 2_565 ? O2 Cl1 O3 68.1(7) . 2_565 ? O2 Cl1 O3 68.1(7) 2_565 . ? O2 Cl1 O3 111.9(7) . . ? O3 Cl1 O3 180.0(12) 2_565 . ? O2 Cl1 O1 72.6(7) 2_565 . ? O2 Cl1 O1 107.4(7) . . ? O3 Cl1 O1 66.5(11) 2_565 . ? O3 Cl1 O1 113.5(11) . . ? O2 Cl1 O1 107.4(7) 2_565 2_565 ? O2 Cl1 O1 72.6(7) . 2_565 ? O3 Cl1 O1 113.5(11) 2_565 2_565 ? O3 Cl1 O1 66.5(11) . 2_565 ? O1 Cl1 O1 180.0(11) . 2_565 ? O2 Cl1 O4 106.9(7) 2_565 2_565 ? O2 Cl1 O4 73.1(7) . 2_565 ? O3 Cl1 O4 109.9(10) 2_565 2_565 ? O3 Cl1 O4 70.1(10) . 2_565 ? O1 Cl1 O4 73.1(7) . 2_565 ? O1 Cl1 O4 106.9(7) 2_565 2_565 ? O2 Cl1 O4 73.1(7) 2_565 . ? O2 Cl1 O4 106.9(7) . . ? O3 Cl1 O4 70.1(10) 2_565 . ? O3 Cl1 O4 109.9(10) . . ? O1 Cl1 O4 106.9(7) . . ? O1 Cl1 O4 73.1(7) 2_565 . ? O4 Cl1 O4 180.0(11) 2_565 . ? O6 Cl2 O8 117.7(5) . . ? O6 Cl2 O7 109.3(4) . . ? O8 Cl2 O7 111.3(4) . . ? O6 Cl2 O5 106.7(6) . . ? O8 Cl2 O5 104.5(5) . . ? O7 Cl2 O5 106.5(5) . . ? N8 Ru1 N9 90.32(16) . . ? N8 Ru1 N1 96.49(15) . . ? N9 Ru1 N1 173.14(16) . . ? N8 Ru1 N7 79.16(17) . . ? N9 Ru1 N7 94.91(17) . . ? N1 Ru1 N7 87.22(16) . . ? N8 Ru1 N2 172.33(15) . . ? N9 Ru1 N2 95.88(16) . . ? N1 Ru1 N2 77.40(16) . . ? N7 Ru1 N2 95.77(16) . . ? N8 Ru1 N10 95.80(16) . . ? N9 Ru1 N10 78.87(17) . . ? N1 Ru1 N10 99.53(16) . . ? N7 Ru1 N10 172.05(16) . . ? N2 Ru1 N10 89.84(16) . . ? O10 Cl3 O9 110.5(7) . . ? O10 Cl3 O10 118.1(4) . 2_566 ? O9 Cl3 O10 106.0(6) . 2_566 ? O10 Cl3 Cl3 60.6(4) . 2_566 ? O9 Cl3 Cl3 127.3(8) . 2_566 ? O10 Cl3 Cl3 57.6(4) 2_566 2_566 ? O10 Cl3 O11 105.3(5) . . ? O9 Cl3 O11 94.7(9) . . ? O10 Cl3 O11 119.7(6) 2_566 . ? Cl3 Cl3 O11 137.8(7) 2_566 . ? Cl3 O10 Cl3 61.9(4) . 2_566 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 4.828 _refine_diff_density_min -2.990 _refine_diff_density_rms 0.170 _database_code_depnum_ccdc_archive 'CCDC 906187'