Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr David Davies' _publ_contact_author_address ; Department of Chemistry University of Leicester University Road Leicester LE1 7RH UNITED KINGDOM ; _publ_contact_author_email DLD3@LE.AC.UK _publ_section_title ; Arene ruthenium complexes with salicyloxazolines: diastereoselective synthesis, configurational stability and applications as asymmetric catalysts for Diels-Alder reactions ; loop_ _publ_author_name 'David Davies' 'Adam J. Davenport' 'John Fawcett' 'David R. Russell' data_2a _database_code_depnum_ccdc_archive 'CCDC 228962' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H26 Cl N O2 Ru' _chemical_formula_weight 460.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 12.272(3) _cell_length_b 12.272(3) _cell_length_c 27.260(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4105(2) _cell_formula_units_Z 8 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 4.78 _cell_measurement_theta_max 13.99 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.908 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.881 _exptl_absorpt_process_details ; based on 341 psi-scan data (XEMP; SHELXTL/PC ver5.0); Rint 0.030 before correction and 0.025 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 9.47 _diffrn_reflns_number 4322 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3511 _reflns_number_gt 2620 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+35.6866P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(13) _refine_ls_number_reflns 3511 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1690 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 0.49925(8) 0.75901(7) 0.08450(3) 0.0334(2) Uani 1 1 d . . . Cl1 Cl 0.5304(3) 0.8630(2) 0.01013(11) 0.0487(8) Uani 1 1 d . . . O1 O 0.3751(6) 0.6893(6) 0.0440(3) 0.0362(18) Uani 1 1 d . . . O2 O 0.2283(7) 0.9670(7) 0.1118(3) 0.056(2) Uani 1 1 d . . . N1 N 0.3882(8) 0.8778(8) 0.1044(3) 0.037(2) Uani 1 1 d . . . C11 C 0.5232(14) 1.1482(12) 0.1400(5) 0.072(5) Uani 1 1 d . . . H11A H 0.5557 1.2064 0.1202 0.109 Uiso 1 1 calc R . . H11B H 0.5790 1.1162 0.1613 0.109 Uiso 1 1 calc R . . H11C H 0.4644 1.1784 0.1602 0.109 Uiso 1 1 calc R . . C12 C 0.4137(13) 1.1101(13) 0.0640(5) 0.068(4) Uani 1 1 d . . . H12A H 0.3825 1.0519 0.0438 0.101 Uiso 1 1 calc R . . H12B H 0.4626 1.1548 0.0440 0.101 Uiso 1 1 calc R . . H12C H 0.3550 1.1558 0.0771 0.101 Uiso 1 1 calc R . . C10 C 0.4773(11) 1.0603(11) 0.1062(4) 0.050(3) Uani 1 1 d . . . H10 H 0.5408 1.0208 0.0916 0.060 Uiso 1 1 calc R . . C8 C 0.4104(9) 0.9764(10) 0.1352(4) 0.041(3) Uani 1 1 d . . . H8 H 0.4517 0.9542 0.1652 0.049 Uiso 1 1 calc R . . C9 C 0.2973(11) 1.0130(13) 0.1497(5) 0.067(4) Uani 1 1 d . . . H9A H 0.2772 0.9844 0.1825 0.080 Uiso 1 1 calc R . . H9B H 0.2921 1.0935 0.1502 0.080 Uiso 1 1 calc R . . C7 C 0.2877(9) 0.8864(9) 0.0905(4) 0.035(3) Uani 1 1 d . . . C6 C 0.2334(10) 0.8239(10) 0.0528(4) 0.041(3) Uani 1 1 d . . . C5 C 0.1290(10) 0.8570(11) 0.0373(4) 0.052(3) Uani 1 1 d . . . H5 H 0.0953 0.9175 0.0529 0.062 Uiso 1 1 calc R . . C4 C 0.0757(11) 0.8048(13) 0.0010(5) 0.060(4) Uani 1 1 d . . . H4 H 0.0057 0.8291 -0.0091 0.072 Uiso 1 1 calc R . . C3 C 0.1235(12) 0.7154(13) -0.0217(5) 0.064(4) Uani 1 1 d . . . H3 H 0.0863 0.6778 -0.0472 0.077 Uiso 1 1 calc R . . C2 C 0.2247(10) 0.6822(10) -0.0070(4) 0.045(3) Uani 1 1 d . . . H2 H 0.2571 0.6220 -0.0233 0.054 Uiso 1 1 calc R . . C1 C 0.2832(9) 0.7327(9) 0.0310(3) 0.036(3) Uani 1 1 d . . . C13 C 0.5705(11) 0.5931(9) 0.0927(4) 0.042(3) Uani 1 1 d . . . C14 C 0.5069(13) 0.6209(10) 0.1336(4) 0.047(3) Uani 1 1 d . . . H14 H 0.4493 0.5736 0.1431 0.057 Uiso 1 1 calc R . . C15 C 0.5251(12) 0.7163(12) 0.1612(4) 0.056(4) Uani 1 1 d . . . C16 C 0.6114(12) 0.7890(11) 0.1455(6) 0.062(5) Uani 1 1 d . . . H16 H 0.6267 0.8527 0.1641 0.075 Uiso 1 1 calc R . . C17 C 0.6714(11) 0.7671(14) 0.1041(6) 0.064(4) Uani 1 1 d . . . C18 C 0.6543(10) 0.6685(13) 0.0779(5) 0.056(4) Uani 1 1 d . . . H18 H 0.6986 0.6521 0.0503 0.068 Uiso 1 1 calc R . . C19 C 0.5454(13) 0.4938(11) 0.0633(4) 0.073(5) Uani 1 1 d . . . H19A H 0.5546 0.4289 0.0839 0.109 Uiso 1 1 calc R . . H19B H 0.5951 0.4897 0.0352 0.109 Uiso 1 1 calc R . . H19C H 0.4701 0.4975 0.0515 0.109 Uiso 1 1 calc R . . C20 C 0.4554(15) 0.7415(15) 0.2050(4) 0.096(6) Uani 1 1 d . . . H20A H 0.3788 0.7276 0.1970 0.144 Uiso 1 1 calc R . . H20B H 0.4646 0.8182 0.2141 0.144 Uiso 1 1 calc R . . H20C H 0.4774 0.6951 0.2325 0.144 Uiso 1 1 calc R . . C21 C 0.7546(12) 0.8470(13) 0.0837(9) 0.117(8) Uani 1 1 d . . . H21A H 0.7334 0.8686 0.0505 0.176 Uiso 1 1 calc R . . H21B H 0.8265 0.8122 0.0828 0.176 Uiso 1 1 calc R . . H21C H 0.7577 0.9116 0.1048 0.176 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 0.0366(5) 0.0377(5) 0.0259(3) 0.0023(4) -0.0019(4) 0.0007(4) Cl1 0.061(2) 0.0481(17) 0.0375(14) 0.0097(13) 0.0166(14) 0.0048(14) O1 0.037(4) 0.039(4) 0.033(4) -0.003(3) -0.005(3) 0.002(4) O2 0.039(5) 0.068(6) 0.059(5) -0.024(5) 0.004(4) 0.006(4) N1 0.035(6) 0.052(6) 0.024(4) 0.001(4) -0.004(4) -0.006(4) C11 0.086(12) 0.067(10) 0.065(9) -0.007(8) -0.041(9) -0.013(9) C12 0.079(11) 0.072(11) 0.052(8) 0.012(7) -0.023(8) -0.010(9) C10 0.053(9) 0.062(8) 0.036(6) -0.006(6) -0.015(6) 0.000(7) C8 0.047(7) 0.046(8) 0.030(5) -0.010(5) -0.007(5) 0.014(6) C9 0.066(9) 0.083(11) 0.052(7) -0.032(8) 0.004(6) -0.012(8) C7 0.037(7) 0.035(6) 0.032(6) -0.008(5) 0.007(5) 0.007(5) C6 0.041(7) 0.050(7) 0.033(6) 0.002(5) 0.003(6) -0.019(6) C5 0.045(8) 0.058(9) 0.053(7) 0.005(7) -0.019(6) 0.007(6) C4 0.047(8) 0.077(10) 0.058(8) 0.000(8) -0.018(7) -0.002(7) C3 0.058(9) 0.086(12) 0.047(8) -0.007(8) -0.017(7) -0.007(8) C2 0.041(7) 0.052(7) 0.042(7) -0.009(6) -0.003(6) -0.009(6) C1 0.045(7) 0.040(7) 0.022(5) 0.001(5) -0.001(4) 0.000(5) C13 0.060(8) 0.028(6) 0.039(7) 0.018(5) 0.001(6) 0.017(6) C14 0.056(8) 0.056(8) 0.031(6) 0.016(6) -0.009(7) 0.013(8) C15 0.073(11) 0.064(9) 0.031(6) 0.009(6) -0.024(6) 0.032(8) C16 0.062(10) 0.045(8) 0.080(11) 0.004(8) -0.062(9) 0.005(7) C17 0.037(8) 0.075(11) 0.078(10) 0.030(9) -0.011(7) 0.005(8) C18 0.036(7) 0.081(10) 0.052(8) 0.021(8) 0.014(6) 0.014(7) C19 0.132(14) 0.037(7) 0.049(7) 0.008(7) -0.023(8) 0.020(9) C20 0.146(16) 0.118(14) 0.024(6) -0.004(8) 0.001(8) 0.064(13) C21 0.032(8) 0.084(13) 0.24(2) 0.082(15) -0.019(13) -0.005(9) _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 N1 2.068(9) . ? Ru1 O1 2.067(7) . ? Ru1 C14 2.161(11) . ? Ru1 C15 2.177(10) . ? Ru1 C17 2.181(13) . ? Ru1 C16 2.189(12) . ? Ru1 C18 2.211(13) . ? Ru1 C13 2.227(11) . ? Ru1 Cl1 2.426(3) . ? O1 C1 1.296(12) . ? O2 C7 1.358(13) . ? O2 C9 1.452(13) . ? N1 C7 1.294(13) . ? N1 C8 1.498(14) . ? C11 C10 1.526(16) . ? C12 C10 1.518(16) . ? C10 C8 1.536(17) . ? C8 C9 1.512(17) . ? C7 C6 1.446(15) . ? C6 C1 1.407(16) . ? C6 C5 1.408(17) . ? C5 C4 1.350(17) . ? C4 C3 1.389(19) . ? C3 C2 1.368(18) . ? C2 C1 1.404(15) . ? C13 C14 1.403(17) . ? C13 C18 1.441(17) . ? C13 C19 1.492(17) . ? C14 C15 1.409(18) . ? C15 C16 1.45(2) . ? C15 C20 1.502(18) . ? C16 C17 1.37(2) . ? C17 C18 1.42(2) . ? C17 C21 1.52(2) . ? 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 Ru1 O1 86.9(3) . . ? N1 Ru1 C14 114.8(4) . . ? O1 Ru1 C14 92.2(4) . . ? N1 Ru1 C15 90.8(4) . . ? O1 Ru1 C15 121.4(5) . . ? C14 Ru1 C15 37.9(5) . . ? N1 Ru1 C17 122.8(6) . . ? O1 Ru1 C17 149.7(5) . . ? C14 Ru1 C17 80.9(6) . . ? C15 Ru1 C17 68.6(6) . . ? N1 Ru1 C16 95.6(5) . . ? O1 Ru1 C16 159.8(5) . . ? C14 Ru1 C16 68.6(5) . . ? C15 Ru1 C16 38.7(5) . . ? C17 Ru1 C16 36.6(6) . . ? N1 Ru1 C18 160.5(5) . . ? O1 Ru1 C18 112.5(5) . . ? C14 Ru1 C18 67.6(5) . . ? C15 Ru1 C18 80.3(5) . . ? C17 Ru1 C18 37.8(5) . . ? C16 Ru1 C18 66.8(6) . . ? N1 Ru1 C13 151.3(4) . . ? O1 Ru1 C13 88.0(4) . . ? C14 Ru1 C13 37.3(4) . . ? C15 Ru1 C13 68.1(4) . . ? C17 Ru1 C13 68.7(6) . . ? C16 Ru1 C13 80.2(5) . . ? C18 Ru1 C13 37.9(5) . . ? N1 Ru1 Cl1 87.2(3) . . ? O1 Ru1 Cl1 83.5(2) . . ? C14 Ru1 Cl1 157.4(4) . . ? C15 Ru1 Cl1 154.9(5) . . ? C17 Ru1 Cl1 91.6(4) . . ? C16 Ru1 Cl1 116.6(5) . . ? C18 Ru1 Cl1 93.5(3) . . ? C13 Ru1 Cl1 120.2(3) . . ? C1 O1 Ru1 128.1(7) . . ? C7 O2 C9 105.9(9) . . ? C7 N1 C8 105.8(9) . . ? C7 N1 Ru1 127.5(8) . . ? C8 N1 Ru1 126.6(7) . . ? C12 C10 C11 111.3(11) . . ? C12 C10 C8 112.7(11) . . ? C11 C10 C8 111.1(10) . . ? N1 C8 C9 102.7(9) . . ? N1 C8 C10 110.5(9) . . ? C9 C8 C10 115.2(11) . . ? O2 C9 C8 103.4(9) . . ? N1 C7 O2 116.5(10) . . ? N1 C7 C6 127.2(10) . . ? O2 C7 C6 116.2(10) . . ? C1 C6 C5 119.9(11) . . ? C1 C6 C7 121.4(11) . . ? C5 C6 C7 118.7(11) . . ? C4 C5 C6 121.6(14) . . ? C5 C4 C3 119.9(14) . . ? C2 C3 C4 119.2(12) . . ? C3 C2 C1 123.3(12) . . ? O1 C1 C2 117.7(10) . . ? O1 C1 C6 126.1(10) . . ? C2 C1 C6 116.1(11) . . ? C14 C13 C18 117.7(13) . . ? C14 C13 C19 120.7(12) . . ? C18 C13 C19 121.4(13) . . ? C14 C13 Ru1 68.8(7) . . ? C18 C13 Ru1 70.4(7) . . ? C19 C13 Ru1 127.7(9) . . ? C13 C14 C15 122.5(14) . . ? C13 C14 Ru1 73.9(6) . . ? C15 C14 Ru1 71.7(7) . . ? C14 C15 C16 118.1(12) . . ? C14 C15 C20 120.3(15) . . ? C16 C15 C20 121.6(14) . . ? C14 C15 Ru1 70.4(6) . . ? C16 C15 Ru1 71.1(7) . . ? C20 C15 Ru1 129.1(9) . . ? C17 C16 C15 120.9(13) . . ? C17 C16 Ru1 71.4(8) . . ? C15 C16 Ru1 70.2(6) . . ? C16 C17 C18 120.0(13) . . ? C16 C17 C21 122.3(17) . . ? C18 C17 C21 117.7(16) . . ? C16 C17 Ru1 72.0(8) . . ? C18 C17 Ru1 72.2(8) . . ? C21 C17 Ru1 126.2(10) . . ? C17 C18 C13 120.7(13) . . ? C17 C18 Ru1 70.0(8) . . ? C13 C18 Ru1 71.7(7) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.947 _refine_diff_density_min -1.396 _refine_diff_density_rms 0.104 #===END data_3b _database_code_depnum_ccdc_archive 'CCDC 228963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H30 Cl N O2 Ru' _chemical_formula_weight 489.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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 6.6660(10) _cell_length_b 17.697(5) _cell_length_c 18.595(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2193.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 5.07 _cell_measurement_theta_max 12.45 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.547 _exptl_absorpt_correction_T_max 0.734 _exptl_absorpt_process_details ; absorption correction based on 200 psi scan data (XEMP; SHELXTL/PC) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(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 P4' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 2500 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2439 _reflns_number_gt 2293 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0587P)^2^+1.9984P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(5) _refine_ls_number_reflns 2439 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.40645(6) 0.35804(2) 0.85005(2) 0.01744(13) Uani 1 1 d . . . Cl1 Cl 0.1277(2) 0.28981(8) 0.79853(8) 0.0293(3) Uani 1 1 d . . . O1 O 0.2235(6) 0.4509(2) 0.83803(19) 0.0259(9) Uani 1 1 d . . . O2 O 0.5761(6) 0.4493(2) 0.6487(2) 0.0273(8) Uani 1 1 d . . . N1 N 0.5079(7) 0.3756(2) 0.7431(2) 0.0184(10) Uani 1 1 d . . . C1 C 0.1824(9) 0.4895(3) 0.7802(3) 0.0207(12) Uani 1 1 d . . . C2 C 0.0256(9) 0.5433(3) 0.7845(3) 0.0271(13) Uani 1 1 d . . . H2 H -0.0430 0.5492 0.8277 0.032 Uiso 1 1 calc R . . C3 C -0.0283(9) 0.5873(3) 0.7261(3) 0.0305(14) Uani 1 1 d . . . H3 H -0.1333 0.6216 0.7303 0.037 Uiso 1 1 calc R . . C4 C 0.0738(10) 0.5805(3) 0.6607(3) 0.0337(14) Uani 1 1 d . . . H4 H 0.0368 0.6097 0.6213 0.040 Uiso 1 1 calc R . . C5 C 0.2297(9) 0.5301(3) 0.6556(3) 0.0274(12) Uani 1 1 d . . . H5 H 0.3004 0.5264 0.6127 0.033 Uiso 1 1 calc R . . C6 C 0.2852(8) 0.4835(3) 0.7142(3) 0.0198(11) Uani 1 1 d . . . C7 C 0.4558(8) 0.4342(3) 0.7055(3) 0.0193(12) Uani 1 1 d . . . C8 C 0.6788(8) 0.3380(3) 0.7056(3) 0.0203(12) Uani 1 1 d . . . H8 H 0.7834 0.3251 0.7406 0.024 Uiso 1 1 calc R . . C9 C 0.7516(9) 0.4023(3) 0.6573(3) 0.0281(13) Uani 1 1 d . . . H9A H 0.8600 0.4301 0.6799 0.034 Uiso 1 1 calc R . . H9B H 0.7974 0.3831 0.6112 0.034 Uiso 1 1 calc R . . C10 C 0.6152(10) 0.2654(3) 0.6629(3) 0.0304(14) Uani 1 1 d . . . C11 C 0.5573(11) 0.2027(3) 0.7145(3) 0.0368(16) Uani 1 1 d . . . H11A H 0.5192 0.1586 0.6876 0.055 Uiso 1 1 calc R . . H11B H 0.4465 0.2189 0.7436 0.055 Uiso 1 1 calc R . . H11C H 0.6695 0.1908 0.7448 0.055 Uiso 1 1 calc R . . C12 C 0.8033(11) 0.2391(4) 0.6208(4) 0.0407(17) Uani 1 1 d . . . H12A H 0.9165 0.2375 0.6527 0.061 Uiso 1 1 calc R . . H12B H 0.8299 0.2738 0.5823 0.061 Uiso 1 1 calc R . . H12C H 0.7799 0.1896 0.6013 0.061 Uiso 1 1 calc R . . C13 C 0.4428(11) 0.2819(4) 0.6110(4) 0.0438(18) Uani 1 1 d . . . H13A H 0.4066 0.2364 0.5861 0.066 Uiso 1 1 calc R . . H13B H 0.4843 0.3195 0.5769 0.066 Uiso 1 1 calc R . . H13C H 0.3292 0.3002 0.6375 0.066 Uiso 1 1 calc R . . C14 C 0.4829(9) 0.2592(3) 0.9179(3) 0.0246(12) Uani 1 1 d . . . C15 C 0.3577(9) 0.3106(3) 0.9567(3) 0.0253(13) Uani 1 1 d . . . H15 H 0.2400 0.2933 0.9779 0.030 Uiso 1 1 calc R . . C16 C 0.4106(10) 0.3868(3) 0.9631(3) 0.0237(12) Uani 1 1 d . . . H16 H 0.3277 0.4189 0.9892 0.028 Uiso 1 1 calc R . . C17 C 0.5882(9) 0.4170(3) 0.9306(3) 0.0224(11) Uani 1 1 d . . . C18 C 0.7092(8) 0.3664(3) 0.8917(3) 0.0226(12) Uani 1 1 d . . . H18 H 0.8238 0.3845 0.8689 0.027 Uiso 1 1 calc R . . C19 C 0.6613(8) 0.2885(3) 0.8861(3) 0.0214(12) Uani 1 1 d . . . H19 H 0.7472 0.2562 0.8613 0.026 Uiso 1 1 calc R . . C20 C 0.4759(11) 0.5501(3) 0.9651(4) 0.0396(17) Uani 1 1 d . . . H20A H 0.3523 0.5402 0.9403 0.059 Uiso 1 1 calc R . . H20B H 0.5110 0.6024 0.9596 0.059 Uiso 1 1 calc R . . H20C H 0.4601 0.5387 1.0152 0.059 Uiso 1 1 calc R . . C21 C 0.8398(10) 0.5097(4) 0.9747(4) 0.0366(16) Uani 1 1 d . . . H21A H 0.8211 0.4943 1.0238 0.055 Uiso 1 1 calc R . . H21B H 0.8814 0.5616 0.9734 0.055 Uiso 1 1 calc R . . H21C H 0.9409 0.4787 0.9527 0.055 Uiso 1 1 calc R . . C22 C 0.6416(9) 0.5009(3) 0.9335(3) 0.0253(13) Uani 1 1 d . . . H22 H 0.6649 0.5178 0.8841 0.030 Uiso 1 1 calc R . . C23 C 0.4212(10) 0.1783(3) 0.9094(3) 0.0344(14) Uani 1 1 d . . . H23A H 0.4476 0.1514 0.9533 0.052 Uiso 1 1 calc R . . H23B H 0.4961 0.1557 0.8709 0.052 Uiso 1 1 calc R . . H23C H 0.2805 0.1758 0.8987 0.052 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 0.0181(2) 0.0187(2) 0.0156(2) 0.00272(18) 0.00055(18) 0.0012(2) Cl1 0.0183(7) 0.0338(7) 0.0357(7) -0.0015(6) -0.0038(6) -0.0017(6) O1 0.031(2) 0.026(2) 0.0204(19) 0.0082(16) 0.0024(18) 0.0069(18) O2 0.029(2) 0.0297(19) 0.0233(18) 0.0074(18) 0.012(2) 0.0033(19) N1 0.017(2) 0.021(2) 0.017(2) -0.0004(18) 0.0021(18) 0.000(2) C1 0.025(3) 0.017(3) 0.020(3) 0.000(2) -0.003(2) 0.000(2) C2 0.028(3) 0.025(3) 0.028(3) 0.003(2) 0.004(3) 0.002(3) C3 0.028(3) 0.021(3) 0.043(3) 0.008(3) 0.001(3) 0.007(2) C4 0.035(3) 0.029(3) 0.037(3) 0.014(3) -0.004(3) 0.006(3) C5 0.032(3) 0.026(3) 0.024(3) 0.009(3) -0.004(3) -0.003(3) C6 0.021(3) 0.014(2) 0.024(3) -0.002(2) -0.003(2) 0.001(2) C7 0.022(3) 0.019(3) 0.017(2) 0.002(2) 0.000(2) -0.001(2) C8 0.018(2) 0.025(3) 0.018(3) 0.000(2) 0.001(2) 0.005(2) C9 0.028(3) 0.026(3) 0.030(3) -0.001(3) 0.008(3) 0.009(2) C10 0.037(3) 0.028(3) 0.027(3) -0.004(2) 0.001(3) 0.005(3) C11 0.045(4) 0.025(3) 0.041(3) -0.001(3) 0.005(3) 0.002(3) C12 0.048(4) 0.038(4) 0.036(3) -0.014(3) 0.012(3) 0.006(3) C13 0.053(5) 0.033(3) 0.046(4) -0.011(3) -0.021(4) 0.002(4) C14 0.026(3) 0.026(3) 0.022(3) 0.008(2) -0.004(2) 0.000(3) C15 0.024(3) 0.032(3) 0.020(3) 0.010(2) 0.001(2) 0.001(2) C16 0.028(3) 0.031(3) 0.012(2) 0.006(2) 0.002(3) 0.006(3) C17 0.025(3) 0.027(3) 0.015(2) 0.003(2) -0.005(3) 0.004(3) C18 0.022(3) 0.030(3) 0.016(2) 0.001(2) -0.006(2) 0.003(3) C19 0.023(3) 0.026(3) 0.015(3) -0.001(2) -0.004(2) 0.012(2) C20 0.052(4) 0.019(3) 0.048(4) -0.009(3) 0.004(3) 0.000(3) C21 0.046(4) 0.030(3) 0.034(3) -0.003(3) -0.008(3) -0.006(3) C22 0.035(3) 0.020(3) 0.021(3) 0.001(2) 0.001(2) -0.004(3) C23 0.040(3) 0.024(3) 0.040(3) 0.005(3) -0.003(3) -0.004(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 O1 2.058(4) . ? Ru1 N1 2.124(4) . ? Ru1 C16 2.162(5) . ? Ru1 C18 2.166(5) . ? Ru1 C15 2.178(5) . ? Ru1 C17 2.191(5) . ? Ru1 C19 2.202(5) . ? Ru1 C14 2.216(6) . ? Ru1 Cl1 2.4145(15) . ? O1 C1 1.303(7) . ? O2 C7 1.353(6) . ? O2 C9 1.444(7) . ? N1 C7 1.298(7) . ? N1 C8 1.492(7) . ? C1 C6 1.410(8) . ? C1 C2 1.415(8) . ? C2 C3 1.384(8) . ? C3 C4 1.399(9) . ? C4 C5 1.373(8) . ? C5 C6 1.414(8) . ? C6 C7 1.443(7) . ? C8 C9 1.530(8) . ? C8 C10 1.569(7) . ? C10 C11 1.517(8) . ? C10 C13 1.528(9) . ? C10 C12 1.550(9) . ? C14 C19 1.426(8) . ? C14 C15 1.430(8) . ? C14 C23 1.498(8) . ? C15 C16 1.398(8) . ? C16 C17 1.432(8) . ? C17 C18 1.406(8) . ? C17 C22 1.527(7) . ? C18 C19 1.418(8) . ? C20 C22 1.524(9) . ? C21 C22 1.535(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 N1 88.30(15) . . ? O1 Ru1 C16 85.72(19) . . ? N1 Ru1 C16 150.7(2) . . ? O1 Ru1 C18 122.44(19) . . ? N1 Ru1 C18 91.60(19) . . ? C16 Ru1 C18 68.0(2) . . ? O1 Ru1 C15 108.54(18) . . ? N1 Ru1 C15 163.09(18) . . ? C16 Ru1 C15 37.6(2) . . ? C18 Ru1 C15 80.8(2) . . ? O1 Ru1 C17 91.25(18) . . ? N1 Ru1 C17 113.3(2) . . ? C16 Ru1 C17 38.4(2) . . ? C18 Ru1 C17 37.7(2) . . ? C15 Ru1 C17 69.1(2) . . ? O1 Ru1 C19 159.42(18) . . ? N1 Ru1 C19 96.93(19) . . ? C16 Ru1 C19 80.0(2) . . ? C18 Ru1 C19 37.9(2) . . ? C15 Ru1 C19 67.9(2) . . ? C17 Ru1 C19 68.4(2) . . ? O1 Ru1 C14 145.90(19) . . ? N1 Ru1 C14 125.13(19) . . ? C16 Ru1 C14 68.2(2) . . ? C18 Ru1 C14 68.7(2) . . ? C15 Ru1 C14 38.0(2) . . ? C17 Ru1 C14 81.9(2) . . ? C19 Ru1 C14 37.7(2) . . ? O1 Ru1 Cl1 84.26(12) . . ? N1 Ru1 Cl1 86.93(13) . . ? C16 Ru1 Cl1 120.87(17) . . ? C18 Ru1 Cl1 153.23(16) . . ? C15 Ru1 Cl1 93.08(16) . . ? C17 Ru1 Cl1 159.24(16) . . ? C19 Ru1 Cl1 115.80(16) . . ? C14 Ru1 Cl1 90.48(16) . . ? C1 O1 Ru1 129.3(3) . . ? C7 O2 C9 106.3(4) . . ? C7 N1 C8 108.0(4) . . ? C7 N1 Ru1 122.4(4) . . ? C8 N1 Ru1 128.0(3) . . ? O1 C1 C6 125.2(5) . . ? O1 C1 C2 117.5(5) . . ? C6 C1 C2 117.3(5) . . ? C3 C2 C1 121.7(5) . . ? C2 C3 C4 120.5(5) . . ? C5 C4 C3 118.9(5) . . ? C4 C5 C6 121.6(6) . . ? C1 C6 C5 120.0(5) . . ? C1 C6 C7 121.7(5) . . ? C5 C6 C7 118.2(5) . . ? N1 C7 O2 114.8(5) . . ? N1 C7 C6 129.4(5) . . ? O2 C7 C6 115.8(4) . . ? N1 C8 C9 100.6(4) . . ? N1 C8 C10 113.3(5) . . ? C9 C8 C10 113.4(5) . . ? O2 C9 C8 103.7(4) . . ? C11 C10 C13 110.4(6) . . ? C11 C10 C12 107.8(5) . . ? C13 C10 C12 110.3(5) . . ? C11 C10 C8 110.3(5) . . ? C13 C10 C8 111.5(5) . . ? C12 C10 C8 106.5(5) . . ? C19 C14 C15 117.7(5) . . ? C19 C14 C23 122.2(5) . . ? C15 C14 C23 120.1(5) . . ? C19 C14 Ru1 70.6(3) . . ? C15 C14 Ru1 69.6(3) . . ? C23 C14 Ru1 129.1(4) . . ? C16 C15 C14 120.6(5) . . ? C16 C15 Ru1 70.6(3) . . ? C14 C15 Ru1 72.5(3) . . ? C15 C16 C17 122.2(5) . . ? C15 C16 Ru1 71.8(3) . . ? C17 C16 Ru1 71.9(3) . . ? C18 C17 C16 116.9(5) . . ? C18 C17 C22 120.2(5) . . ? C16 C17 C22 122.7(5) . . ? C18 C17 Ru1 70.2(3) . . ? C16 C17 Ru1 69.7(3) . . ? C22 C17 Ru1 128.0(4) . . ? C17 C18 C19 121.9(5) . . ? C17 C18 Ru1 72.1(3) . . ? C19 C18 Ru1 72.4(3) . . ? C18 C19 C14 120.7(5) . . ? C18 C19 Ru1 69.7(3) . . ? C14 C19 Ru1 71.7(3) . . ? C20 C22 C17 113.6(5) . . ? C20 C22 C21 111.9(5) . . ? C17 C22 C21 108.5(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.668 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.090 #===END data_5a _database_code_depnum_ccdc_archive 'CCDC 228964' _audit_creation_method shelxl-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H24 Cl N O2 Ru)(C H Cl3)' _chemical_formula_sum 'C25 H25 Cl4 N O2 Ru' _chemical_formula_weight 614.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source c c 0.0033 0.0016 'international tables vol c tables 4.2.6.8 and 6.1.1.4' h h 0.0000 0.0000 'international tables vol c tables 4.2.6.8 and 6.1.1.4' n n 0.0061 0.0033 'international tables vol c tables 4.2.6.8 and 6.1.1.4' o o 0.0106 0.0060 'international tables vol c tables 4.2.6.8 and 6.1.1.4' cl cl 0.1484 0.1585 'international tables vol c tables 4.2.6.8 and 6.1.1.4' ru ru -1.2594 0.8363 'international tables vol c tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.7370(10) _cell_length_b 16.1710(10) _cell_length_c 9.9840(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.380(10) _cell_angle_gamma 90.00 _cell_volume 1247.0(2) _cell_formula_units_z 2 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 41 _cell_measurement_theta_min 5.11 _cell_measurement_theta_max 12.48 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 620 _exptl_absorpt_coefficient_mu 1.081 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_t_min 0.61 _exptl_absorpt_correction_t_max 0.82 _exptl_absorpt_process_details ; absorption correction based on 177 psi scan data (XEMP; SHELXTL/PC) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(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 P4' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 2759 _diffrn_reflns_av_r_equivalents 0.0157 _diffrn_reflns_av_sigmai/neti 0.0117 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2450 _reflns_number_gt 2427 _reflns_threshold_expression >2sigma(i) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0647p)^2^+1.8137p] where p=(fo^2^+2fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'flack h d (1983), acta cryst. a39, 876-881' _refine_ls_abs_structure_flack 0.01(6) _refine_ls_number_reflns 2450 _refine_ls_number_parameters 289 _refine_ls_number_restraints 1 _refine_ls_r_factor_all 0.0364 _refine_ls_r_factor_gt 0.0361 _refine_ls_wr_factor_ref 0.0957 _refine_ls_wr_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_s_all 1.090 _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 0.59477(5) 0.4709 0.86586(4) 0.02423(15) uaNi 1 1 d . . . Cl1 Cl 0.7095(2) 0.57522(11) 1.01924(17) 0.0402(4) uaNi 1 1 d . . . O1 O 0.8127(5) 0.4010(3) 0.9274(4) 0.0318(9) uaNi 1 1 d . . . O2 O 0.9999(6) 0.5272(4) 0.6130(5) 0.0467(13) uaNi 1 1 d . . . N1 N 0.7656(6) 0.5231(3) 0.7326(5) 0.0285(11) uaNi 1 1 d . . . C1 C 0.9009(7) 0.3615(4) 0.8383(6) 0.0255(12) uaNi 1 1 d . . . C2 C 0.9667(9) 0.2819(4) 0.8668(7) 0.0378(15) uaNi 1 1 d . . . H2a H 0.9450 0.2563 0.9476 0.045 uisO 1 1 CalC r . . C3 C 1.0654(9) 0.2410(5) 0.7727(8) 0.0421(17) uaNi 1 1 d . . . H3a H 1.1104 0.1889 0.7928 0.050 uisO 1 1 CalC r . . C4 C 1.0956(8) 0.2765(5) 0.6538(8) 0.0428(18) uaNi 1 1 d . . . H4a H 1.1577 0.2475 0.5921 0.051 uisO 1 1 CalC r . . C5 C 1.0374(8) 0.3531(6) 0.6231(7) 0.0401(17) uaNi 1 1 d . . . H5a H 1.0626 0.3770 0.5418 0.048 uisO 1 1 CalC r . . C6 C 0.9387(7) 0.3973(5) 0.7130(6) 0.0322(14) uaNi 1 1 d . . . C7 C 0.8922(7) 0.4825(5) 0.6869(6) 0.0321(17) uaNi 1 1 d . . . C8 C 0.7747(9) 0.6108(4) 0.6895(7) 0.0361(15) uaNi 1 1 d . . . H8a H 0.7739 0.6473 0.7679 0.043 uisO 1 1 CalC r . . C9 C 0.9532(10) 0.6127(6) 0.6309(10) 0.056(2) uaNi 1 1 d . . . H9a H 0.9479 0.6418 0.5457 0.067 uisO 1 1 CalC r . . H9b H 1.0369 0.6401 0.6920 0.067 uisO 1 1 CalC r . . C10 C 0.6278(8) 0.6345(4) 0.5877(6) 0.0266(12) uaNi 1 1 d . . . C11 C 0.6233(9) 0.6054(5) 0.4566(7) 0.0378(15) uaNi 1 1 d . . . H11a H 0.7116 0.5709 0.4309 0.045 uisO 1 1 CalC r . . C12 C 0.4924(12) 0.6262(6) 0.3638(8) 0.056(2) uaNi 1 1 d . . . H12a H 0.4927 0.6060 0.2765 0.067 uisO 1 1 CalC r . . C13 C 0.3605(11) 0.6771(6) 0.4009(11) 0.063(3) uaNi 1 1 d . . . H13a H 0.2708 0.6907 0.3386 0.076 uisO 1 1 CalC r . . C14 C 0.3603(10) 0.7075(6) 0.5271(12) 0.061(3) uaNi 1 1 d . . . H14a H 0.2713 0.7422 0.5510 0.073 uisO 1 1 CalC r . . C15 C 0.4982(10) 0.6861(5) 0.6247(8) 0.0409(16) uaNi 1 1 d . . . H15a H 0.4990 0.7069 0.7115 0.049 uisO 1 1 CalC r . . C16 C 0.4166(8) 0.4261(5) 0.7031(6) 0.0311(14) uaNi 1 1 d . . . C17 C 0.3511(8) 0.5018(4) 0.7536(6) 0.0301(13) uaNi 1 1 d . . . H17a H 0.3461 0.5508 0.6958 0.036 uisO 1 1 CalC r . . C18 C 0.3270(7) 0.5111(5) 0.8936(7) 0.0332(14) uaNi 1 1 d . . . C19 C 0.3696(8) 0.4430(5) 0.9785(7) 0.0361(15) uaNi 1 1 d . . . H19a H 0.3789 0.4532 1.0754 0.043 uisO 1 1 CalC r . . C20 C 0.4325(8) 0.3687(5) 0.9337(7) 0.0350(14) uaNi 1 1 d . . . C21 C 0.4575(8) 0.3611(5) 0.7911(7) 0.0351(14) uaNi 1 1 d . . . H21a H 0.5244 0.3143 0.7594 0.042 uisO 1 1 CalC r . . C22 C 0.4515(9) 0.4175(5) 0.5553(6) 0.0406(16) uaNi 1 1 d . . . H22a H 0.4158 0.4670 0.5085 0.061 uisO 1 1 CalC r . . H22b H 0.3878 0.3712 0.5178 0.061 uisO 1 1 CalC r . . H22C H 0.5730 0.4088 0.5465 0.061 uisO 1 1 CalC r . . C23 C 0.2614(9) 0.5903(5) 0.9466(8) 0.0439(17) uaNi 1 1 d . . . H23a H 0.2449 0.6294 0.8746 0.066 uisO 1 1 CalC r . . H23b H 0.3438 0.6119 1.0133 0.066 uisO 1 1 CalC r . . H23C H 0.1530 0.5808 0.9862 0.066 uisO 1 1 CalC r . . C24 C 0.4939(7) 0.2994(4) 1.0501(6) 0.084(4) uaNi 1 1 d . . . H24a H 0.5380 0.2512 1.0077 0.125 uisO 1 1 CalC r . . H24b H 0.3964 0.2843 1.1001 0.125 uisO 1 1 CalC r . . H24C H 0.5827 0.3228 1.1098 0.125 uisO 1 1 CalC r . . C25 C 0.9522(7) 0.4233(4) 0.2074(6) 0.0401(16) uaNi 1 1 d r . . H25 H 0.91803(17) 0.43202(10) 0.11239(12) 0.048 uisO 1 1 CalC . a 1 Cl2 Cl 1.07527(17) 0.50425(10) 0.27597(12) 0.0573(5) uaNi 1 1 d r b . Cl3' Cl 0.76887(17) 0.41000(10) 0.30862(12) 0.0514(5) uaNi 0.80 1 d pr b 1 Cl4' Cl 1.08267(17) 0.33315(10) 0.23487(12) 0.0632(7) uaNi 0.80 1 d pr b 1 Cl3" Cl 0.76377(17) 0.41005(10) 0.26986(12) 0.0514(5) uaNi 0.20 1 d pr b 2 Cl4" Cl 1.07797(17) 0.32640(10) 0.19952(12) 0.0632(7) uaNi 0.20 1 d pr b 2 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 0.0230(2) 0.0227(2) 0.0263(2) 0.0008(2) -0.00439(14) -0.0002(2) Cl1 0.0431(8) 0.0348(9) 0.0411(8) -0.0100(7) -0.0109(7) -0.0001(7) O1 0.038(2) 0.034(2) 0.0233(19) 0.0057(19) -0.0028(17) 0.007(2) O2 0.024(2) 0.063(4) 0.053(3) 0.026(3) -0.001(2) -0.003(2) N1 0.021(2) 0.029(3) 0.035(3) 0.006(2) -0.008(2) -0.001(2) C1 0.020(2) 0.028(3) 0.028(3) 0.000(3) -0.008(2) 0.000(2) C2 0.038(4) 0.030(3) 0.044(4) -0.002(3) -0.009(3) 0.000(3) C3 0.033(3) 0.031(4) 0.061(5) -0.015(3) -0.010(3) 0.001(3) C4 0.023(3) 0.054(5) 0.051(4) -0.023(4) -0.003(3) 0.002(3) C5 0.023(3) 0.057(5) 0.039(4) -0.014(4) -0.005(3) -0.004(3) C6 0.018(3) 0.046(4) 0.032(3) -0.002(3) -0.007(2) 0.001(3) C7 0.020(2) 0.049(5) 0.027(2) 0.007(3) -0.0065(19) -0.008(3) C8 0.034(3) 0.026(3) 0.045(4) 0.011(3) -0.018(3) -0.010(3) C9 0.029(4) 0.051(5) 0.084(6) 0.032(5) -0.021(4) -0.007(4) C10 0.028(3) 0.024(3) 0.027(3) 0.006(2) -0.004(2) -0.004(2) C11 0.035(3) 0.038(4) 0.039(3) 0.002(3) -0.004(3) -0.003(3) C12 0.059(5) 0.068(6) 0.039(4) 0.013(4) -0.014(3) -0.020(5) C13 0.040(4) 0.064(6) 0.082(7) 0.036(6) -0.022(4) -0.008(4) C14 0.031(4) 0.043(5) 0.110(8) 0.022(5) 0.012(4) 0.012(4) C15 0.042(4) 0.027(3) 0.054(4) 0.004(3) 0.009(3) 0.001(3) C16 0.024(3) 0.036(4) 0.033(3) -0.003(3) -0.004(2) -0.008(3) C17 0.022(3) 0.035(3) 0.032(3) 0.005(3) -0.005(2) -0.004(3) C18 0.022(3) 0.040(4) 0.037(3) 0.006(3) 0.002(2) -0.002(3) C19 0.032(3) 0.044(4) 0.032(3) -0.003(3) 0.006(3) -0.006(3) C20 0.030(3) 0.032(3) 0.043(3) 0.006(3) 0.000(3) -0.010(3) C21 0.033(3) 0.030(3) 0.041(3) -0.008(3) -0.003(3) -0.008(3) C22 0.042(4) 0.049(4) 0.031(3) -0.004(3) 0.000(3) -0.014(3) C23 0.038(4) 0.050(4) 0.044(4) -0.003(4) 0.005(3) 0.006(4) C24 0.058(6) 0.031(4) 0.163(12) 0.026(6) 0.010(6) -0.007(4) C25 0.043(4) 0.047(5) 0.030(3) -0.003(3) 0.000(3) 0.001(3) Cl2 0.0653(12) 0.0621(12) 0.0439(9) -0.0009(9) -0.0026(8) -0.0118(10) Cl3' 0.0536(11) 0.0711(14) 0.0304(10) -0.0023(11) 0.0103(8) -0.0062(11) Cl4' 0.0839(16) 0.0622(14) 0.0436(13) -0.0063(12) 0.0037(12) 0.0242(13) Cl3" 0.0536(11) 0.0711(14) 0.0304(10) -0.0023(11) 0.0103(8) -0.0062(11) Cl4" 0.0839(16) 0.0622(14) 0.0436(13) -0.0063(12) 0.0037(12) 0.0242(13) _geom_special_details ; all esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. the cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. an approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1 2.092(4) . ? Ru1 N1 2.106(5) . ? Ru1 C19 2.176(6) . ? Ru1 C21 2.178(7) . ? Ru1 C16 2.191(6) . ? Ru1 C17 2.193(6) . ? Ru1 C18 2.204(6) . ? Ru1 C20 2.207(7) . ? Ru1 Cl1 2.4118(16) . ? O1 C1 1.317(7) . ? O2 C7 1.354(8) . ? O2 C9 1.444(12) . ? N1 C7 1.285(9) . ? N1 C8 1.486(9) . ? C1 C2 1.407(9) . ? C1 C6 1.424(9) . ? C2 C3 1.410(11) . ? C3 C4 1.351(12) . ? C4 C5 1.348(12) . ? C5 C6 1.407(10) . ? C6 C7 1.443(11) . ? C8 C10 1.529(8) . ? C8 C9 1.531(11) . ? C10 C15 1.372(10) . ? C10 C11 1.389(10) . ? C11 C12 1.374(11) . ? C12 C13 1.379(15) . ? C13 C14 1.353(15) . ? C14 C15 1.444(13) . ? C16 C21 1.394(10) . ? C16 C17 1.427(10) . ? C16 C22 1.522(9) . ? C17 C18 1.429(9) . ? C18 C19 1.417(10) . ? C18 C23 1.488(11) . ? C19 C20 1.381(11) . ? C20 C21 1.453(9) . ? C20 C24 1.664(9) . ? C25 Cl3" 1.633(6) . ? C25 Cl2 1.735(6) . ? C25 Cl4' 1.785(6) . ? C25 Cl3' 1.802(6) . ? C25 Cl4" 1.849(6) . ? 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 O1 Ru1 N1 82.93(18) . . ? O1 Ru1 C19 113.1(2) . . ? N1 Ru1 C19 164.0(2) . . ? O1 Ru1 C21 91.6(2) . . ? N1 Ru1 C21 114.9(2) . . ? C19 Ru1 C21 67.6(3) . . ? O1 Ru1 C16 120.0(2) . . ? N1 Ru1 C16 93.2(2) . . ? C19 Ru1 C16 80.0(3) . . ? C21 Ru1 C16 37.2(3) . . ? O1 Ru1 C17 157.9(2) . . ? N1 Ru1 C17 98.0(2) . . ? C19 Ru1 C17 67.7(3) . . ? C21 Ru1 C17 67.8(3) . . ? C16 Ru1 C17 38.0(3) . . ? O1 Ru1 C18 150.4(2) . . ? N1 Ru1 C18 126.2(2) . . ? C19 Ru1 C18 37.7(3) . . ? C21 Ru1 C18 80.8(3) . . ? C16 Ru1 C18 68.6(3) . . ? C17 Ru1 C18 37.9(2) . . ? O1 Ru1 C20 88.2(2) . . ? N1 Ru1 C20 152.1(2) . . ? C19 Ru1 C20 36.7(3) . . ? C21 Ru1 C20 38.7(3) . . ? C16 Ru1 C20 68.6(2) . . ? C17 Ru1 C20 80.8(3) . . ? C18 Ru1 C20 68.0(3) . . ? O1 Ru1 Cl1 86.08(13) . . ? N1 Ru1 Cl1 84.25(15) . . ? C19 Ru1 Cl1 95.3(2) . . ? C21 Ru1 Cl1 160.28(18) . . ? C16 Ru1 Cl1 153.4(2) . . ? C17 Ru1 Cl1 116.02(19) . . ? C18 Ru1 Cl1 91.60(19) . . ? C20 Ru1 Cl1 121.60(19) . . ? C1 O1 Ru1 120.3(3) . . ? C7 O2 C9 106.1(6) . . ? C7 N1 C8 109.6(6) . . ? C7 N1 Ru1 122.7(5) . . ? C8 N1 Ru1 127.4(5) . . ? O1 C1 C2 120.1(6) . . ? O1 C1 C6 122.5(6) . . ? C2 C1 C6 117.3(6) . . ? C1 C2 C3 119.8(7) . . ? C4 C3 C2 121.0(7) . . ? C5 C4 C3 121.2(7) . . ? C4 C5 C6 120.6(7) . . ? C5 C6 C1 120.0(7) . . ? C5 C6 C7 120.6(7) . . ? C1 C6 C7 119.0(6) . . ? N1 C7 O2 115.3(7) . . ? N1 C7 C6 127.6(6) . . ? O2 C7 C6 116.9(6) . . ? N1 C8 C10 112.7(5) . . ? N1 C8 C9 100.9(6) . . ? C10 C8 C9 113.1(6) . . ? O2 C9 C8 105.5(6) . . ? C15 C10 C11 118.8(6) . . ? C15 C10 C8 120.0(6) . . ? C11 C10 C8 121.2(6) . . ? C12 C11 C10 122.0(7) . . ? C11 C12 C13 119.5(8) . . ? C14 C13 C12 120.6(7) . . ? C13 C14 C15 120.0(8) . . ? C10 C15 C14 119.1(8) . . ? C21 C16 C17 119.7(6) . . ? C21 C16 C22 119.7(6) . . ? C17 C16 C22 120.5(6) . . ? C21 C16 Ru1 70.9(3) . . ? C17 C16 Ru1 71.1(4) . . ? C22 C16 Ru1 127.5(4) . . ? C16 C17 C18 120.3(6) . . ? C16 C17 Ru1 70.9(3) . . ? C18 C17 Ru1 71.5(3) . . ? C19 C18 C17 117.7(6) . . ? C19 C18 C23 121.9(6) . . ? C17 C18 C23 120.4(6) . . ? C19 C18 Ru1 70.1(4) . . ? C17 C18 Ru1 70.6(3) . . ? C23 C18 Ru1 129.9(5) . . ? C20 C19 C18 123.8(6) . . ? C20 C19 Ru1 72.8(4) . . ? C18 C19 Ru1 72.2(3) . . ? C19 C20 C21 117.4(6) . . ? C19 C20 C24 116.8(6) . . ? C21 C20 C24 125.4(6) . . ? C19 C20 Ru1 70.4(4) . . ? C21 C20 Ru1 69.6(4) . . ? C24 C20 Ru1 125.1(4) . . ? C16 C21 C20 121.1(7) . . ? C16 C21 Ru1 71.9(4) . . ? C20 C21 Ru1 71.7(4) . . ? Cl3" C25 Cl2 115.5(4) . . ? Cl3" C25 Cl4' 110.1(3) . . ? Cl2 C25 Cl4' 105.3(3) . . ? Cl3" C25 Cl3' 11.6 . . ? Cl2 C25 Cl3' 107.5(3) . . ? Cl4' C25 Cl3' 105.8(3) . . ? Cl3" C25 Cl4" 112.9(3) . . ? Cl2 C25 Cl4" 112.2(3) . . ? Cl4' C25 Cl4" 11.5 . . ? Cl3' C25 Cl4" 110.9(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.381 _refine_diff_density_min -1.225 _refine_diff_density_rms 0.109 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 228965' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C27 H33 N2 O2 Ru)+ (F6 Sb)-' _chemical_formula_sum 'C27 H33 F6 N2 O2 Ru Sb' _chemical_formula_weight 754.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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 10.5418(10) _cell_length_b 16.1518(15) _cell_length_c 16.8105(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2862.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4287 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 26.96 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 1.538 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; absorption correction based on 7948 reflections (SADABS); Rint 0.058 before correction and 0.035 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20825 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5033 _reflns_number_gt 4377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 5033 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0640 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _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 0.07496(4) 0.04669(3) 0.87992(2) 0.03163(12) Uani 1 1 d . . . Sb2 Sb 0.60272(4) 0.15741(3) 0.65645(3) 0.04681(13) Uani 1 1 d . . . N1 N 0.0762(4) 0.1342(2) 0.9717(2) 0.0297(10) Uani 1 1 d . . . F1 F 0.6312(4) 0.2004(2) 0.5558(2) 0.0783(13) Uani 1 1 d . . . C23 C -0.1325(5) 0.0431(4) 0.8882(3) 0.0399(14) Uani 1 1 d . . . N2 N 0.2491(4) -0.0064(3) 0.9213(3) 0.0318(11) Uani 1 1 d . . . C17 C 0.3598(5) 0.0103(3) 0.8846(3) 0.0381(14) Uani 1 1 d . . . H17 H 0.3613 0.0522 0.8450 0.046 Uiso 1 1 calc R . . C22 C -0.0855(5) -0.0346(3) 0.9112(3) 0.0385(14) Uani 1 1 d . . . H22 H -0.1083 -0.0566 0.9616 0.046 Uiso 1 1 calc R . . F2 F 0.4432(4) 0.1238(3) 0.6249(3) 0.0980(14) Uani 1 1 d . . . F3 F 0.6672(5) 0.0583(3) 0.6217(3) 0.1244(19) Uani 1 1 d . . . F4 F 0.5753(4) 0.1128(3) 0.7554(2) 0.1058(16) Uani 1 1 d . . . C24 C -0.0970(6) 0.0768(4) 0.8147(3) 0.0442(15) Uani 1 1 d . . . H24 H -0.1288 0.1292 0.7988 0.053 Uiso 1 1 calc R . . F5 F 0.5352(4) 0.2572(3) 0.6874(2) 0.0922(15) Uani 1 1 d . . . C16 C 0.4708(5) -0.0308(3) 0.9021(3) 0.0385(15) Uani 1 1 d . . . H16 H 0.5468 -0.0157 0.8755 0.046 Uiso 1 1 calc R . . F6 F 0.7617(4) 0.1914(3) 0.6864(3) 0.119(2) Uani 1 1 d . . . C19 C -0.0132(6) 0.0323(4) 0.7639(3) 0.0491(17) Uani 1 1 d . . . C13 C 0.2526(6) -0.0658(3) 0.9768(3) 0.0376(15) Uani 1 1 d . . . H13 H 0.1764 -0.0785 1.0044 0.045 Uiso 1 1 calc R . . C20 C 0.0320(5) -0.0447(4) 0.7881(3) 0.0435(15) Uani 1 1 d . . . H20 H 0.0896 -0.0738 0.7548 0.052 Uiso 1 1 calc R . . C21 C -0.0054(5) -0.0806(3) 0.8610(3) 0.0390(15) Uani 1 1 d . . . O1 O 0.1932(4) 0.1282(2) 0.8236(2) 0.0410(10) Uani 1 1 d . . . O2 O 0.0520(4) 0.2621(2) 1.0216(2) 0.0440(11) Uani 1 1 d . . . C7 C 0.0853(6) 0.2127(3) 0.9598(3) 0.0364(14) Uani 1 1 d . . . C5 C 0.1361(5) 0.3411(4) 0.8867(4) 0.0469(16) Uani 1 1 d . . . H5 H 0.0955 0.3722 0.9274 0.056 Uiso 1 1 calc R . . C18 C 0.5921(6) -0.1403(4) 0.9748(3) 0.0540(17) Uani 1 1 d . . . H18A H 0.5899 -0.1933 0.9465 0.081 Uiso 1 1 calc R . . H18B H 0.5978 -0.1505 1.0322 0.081 Uiso 1 1 calc R . . H18C H 0.6660 -0.1083 0.9574 0.081 Uiso 1 1 calc R . . C14 C 0.3600(6) -0.1093(4) 0.9961(3) 0.0434(16) Uani 1 1 d . . . H14 H 0.3570 -0.1508 1.0361 0.052 Uiso 1 1 calc R . . C8 C 0.0442(5) 0.1231(4) 1.0583(3) 0.0384(15) Uani 1 1 d . . . H8 H -0.0269 0.0825 1.0636 0.046 Uiso 1 1 calc R . . C1 C 0.1898(5) 0.2083(4) 0.8269(3) 0.0359(15) Uani 1 1 d . . . C10 C 0.1587(5) 0.0924(4) 1.1058(3) 0.0418(16) Uani 1 1 d . . . H10 H 0.1853 0.0382 1.0822 0.050 Uiso 1 1 calc R . . C9 C -0.0024(6) 0.2086(4) 1.0810(4) 0.0456(17) Uani 1 1 d . . . H9A H -0.0962 0.2112 1.0797 0.055 Uiso 1 1 calc R . . H9B H 0.0273 0.2240 1.1349 0.055 Uiso 1 1 calc R . . C15 C 0.4731(6) -0.0925(4) 0.9570(4) 0.0433(16) Uani 1 1 d . . . C6 C 0.1336(5) 0.2540(3) 0.8891(4) 0.0380(14) Uani 1 1 d . . . C26 C 0.0411(6) -0.1650(4) 0.8814(4) 0.0644(19) Uani 1 1 d . . . H26A H 0.0377 -0.1728 0.9392 0.097 Uiso 1 1 calc R . . H26B H 0.1288 -0.1713 0.8630 0.097 Uiso 1 1 calc R . . H26C H -0.0127 -0.2065 0.8554 0.097 Uiso 1 1 calc R . . C11 C 0.2723(5) 0.1505(5) 1.1013(4) 0.067(2) Uani 1 1 d . . . H11A H 0.2977 0.1575 1.0456 0.100 Uiso 1 1 calc R . . H11B H 0.3431 0.1269 1.1316 0.100 Uiso 1 1 calc R . . H11C H 0.2493 0.2044 1.1238 0.100 Uiso 1 1 calc R . . C2 C 0.2486(5) 0.2538(4) 0.7644(4) 0.0453(16) Uani 1 1 d . . . H2 H 0.2846 0.2247 0.7207 0.054 Uiso 1 1 calc R . . C3 C 0.2542(6) 0.3370(4) 0.7658(4) 0.0553(18) Uani 1 1 d . . . H3 H 0.2981 0.3655 0.7248 0.066 Uiso 1 1 calc R . . C27 C -0.2193(5) 0.0907(4) 0.9412(4) 0.0565(19) Uani 1 1 d . . . H27A H -0.3066 0.0855 0.9217 0.085 Uiso 1 1 calc R . . H27B H -0.1944 0.1491 0.9412 0.085 Uiso 1 1 calc R . . H27C H -0.2140 0.0687 0.9954 0.085 Uiso 1 1 calc R . . C25 C 0.0322(6) 0.0712(5) 0.6870(3) 0.072(2) Uani 1 1 d . . . H25A H -0.0245 0.0550 0.6435 0.108 Uiso 1 1 calc R . . H25B H 0.1185 0.0521 0.6754 0.108 Uiso 1 1 calc R . . H25C H 0.0320 0.1316 0.6923 0.108 Uiso 1 1 calc R . . C12 C 0.1208(6) 0.0760(4) 1.1919(3) 0.0513(18) Uani 1 1 d . . . H12A H 0.1122 0.1288 1.2201 0.077 Uiso 1 1 calc R . . H12B H 0.1861 0.0423 1.2178 0.077 Uiso 1 1 calc R . . H12C H 0.0396 0.0465 1.1931 0.077 Uiso 1 1 calc R . . C4 C 0.1972(6) 0.3813(4) 0.8257(4) 0.056(2) Uani 1 1 d . . . H4 H 0.2000 0.4401 0.8250 0.067 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 0.0328(2) 0.0351(2) 0.0270(2) -0.0003(2) 0.0017(2) 0.0013(2) Sb2 0.0459(3) 0.0486(3) 0.0460(3) 0.0015(2) -0.0012(2) -0.0014(2) N1 0.030(3) 0.027(3) 0.032(2) -0.0004(19) 0.001(2) 0.000(2) F1 0.097(3) 0.071(3) 0.066(3) 0.016(2) 0.017(2) 0.012(2) C23 0.036(3) 0.047(4) 0.036(3) -0.015(3) -0.009(3) 0.000(3) N2 0.033(3) 0.037(3) 0.025(3) -0.003(2) 0.003(2) 0.000(2) C17 0.041(3) 0.041(3) 0.032(3) 0.002(3) 0.006(3) -0.004(3) C22 0.037(3) 0.043(4) 0.035(3) -0.003(3) -0.004(3) -0.011(3) F2 0.089(3) 0.106(3) 0.099(3) -0.010(3) -0.025(3) -0.031(3) F3 0.160(4) 0.064(3) 0.149(5) 0.030(3) 0.045(4) 0.051(3) F4 0.111(4) 0.145(4) 0.061(3) 0.031(3) -0.013(3) -0.055(3) C24 0.040(4) 0.052(4) 0.041(4) -0.001(3) -0.017(3) 0.014(3) F5 0.099(3) 0.079(3) 0.098(3) -0.035(3) 0.021(3) 0.000(3) C16 0.027(3) 0.043(4) 0.045(4) -0.002(3) -0.001(3) -0.007(3) F6 0.061(3) 0.162(5) 0.133(4) 0.083(4) -0.040(3) -0.048(3) C19 0.056(4) 0.061(5) 0.030(4) 0.002(3) -0.007(3) -0.007(4) C13 0.044(4) 0.039(4) 0.030(3) -0.002(3) 0.003(3) -0.002(3) C20 0.043(4) 0.053(4) 0.035(3) -0.019(3) 0.001(3) -0.003(4) C21 0.037(3) 0.036(3) 0.043(4) -0.012(3) -0.009(3) -0.003(3) O1 0.045(2) 0.038(2) 0.040(3) 0.006(2) 0.0112(19) 0.0090(19) O2 0.053(3) 0.039(2) 0.040(2) -0.006(2) -0.003(2) 0.003(2) C7 0.030(3) 0.038(3) 0.041(3) -0.008(3) -0.006(3) 0.003(3) C5 0.040(3) 0.040(4) 0.060(4) 0.002(4) -0.016(3) -0.001(3) C18 0.046(4) 0.059(4) 0.057(4) 0.007(3) -0.023(4) 0.013(4) C14 0.055(4) 0.041(4) 0.035(4) -0.006(3) -0.007(3) 0.002(3) C8 0.039(4) 0.044(4) 0.033(3) -0.007(3) 0.005(3) -0.008(3) C1 0.027(3) 0.049(4) 0.031(4) 0.012(3) -0.010(3) -0.005(3) C10 0.054(4) 0.048(4) 0.023(3) -0.003(3) 0.006(3) 0.006(3) C9 0.040(4) 0.052(4) 0.045(4) -0.009(3) 0.004(3) 0.004(3) C15 0.049(4) 0.041(4) 0.039(4) -0.011(3) -0.014(3) 0.006(3) C6 0.032(3) 0.035(3) 0.047(4) 0.006(3) -0.014(3) -0.001(3) C26 0.077(5) 0.040(4) 0.077(5) -0.010(4) -0.015(4) -0.002(4) C11 0.043(4) 0.109(6) 0.047(4) 0.026(5) -0.006(3) -0.003(5) C2 0.042(4) 0.052(4) 0.042(4) 0.013(3) -0.008(3) -0.005(3) C3 0.051(4) 0.056(5) 0.059(5) 0.019(4) -0.007(4) -0.015(4) C27 0.036(4) 0.067(5) 0.066(5) -0.022(4) -0.003(3) 0.004(3) C25 0.074(5) 0.109(6) 0.034(4) 0.013(4) -0.011(3) -0.003(5) C12 0.065(5) 0.055(4) 0.034(3) 0.000(3) 0.001(3) -0.009(4) C4 0.061(5) 0.034(4) 0.072(5) 0.017(4) -0.026(4) -0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1 2.045(4) . ? Ru1 N1 2.093(4) . ? Ru1 N2 2.142(5) . ? Ru1 C24 2.173(6) . ? Ru1 C19 2.174(6) . ? Ru1 C20 2.183(5) . ? Ru1 C23 2.192(5) . ? Ru1 C22 2.205(5) . ? Ru1 C21 2.246(5) . ? Sb2 F6 1.834(4) . ? Sb2 F3 1.835(4) . ? Sb2 F4 1.836(4) . ? Sb2 F5 1.837(4) . ? Sb2 F2 1.845(4) . ? Sb2 F1 1.853(4) . ? N1 C7 1.288(6) . ? N1 C8 1.505(6) . ? C23 C24 1.402(7) . ? C23 C22 1.404(7) . ? C23 C27 1.490(7) . ? N2 C13 1.339(6) . ? N2 C17 1.346(6) . ? C17 C16 1.377(7) . ? C22 C21 1.404(7) . ? C24 C19 1.422(8) . ? C16 C15 1.358(7) . ? C19 C20 1.393(8) . ? C19 C25 1.515(8) . ? C13 C14 1.372(7) . ? C20 C21 1.412(7) . ? C21 C26 1.489(7) . ? O1 C1 1.295(6) . ? O2 C7 1.355(6) . ? O2 C9 1.440(6) . ? C7 C6 1.455(7) . ? C5 C4 1.373(8) . ? C5 C6 1.408(8) . ? C18 C15 1.503(8) . ? C14 C15 1.389(8) . ? C8 C9 1.515(7) . ? C8 C10 1.529(7) . ? C1 C6 1.411(8) . ? C1 C2 1.424(7) . ? C10 C11 1.524(8) . ? C10 C12 1.525(7) . ? C2 C3 1.345(8) . ? C3 C4 1.375(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 N1 84.42(16) . . ? O1 Ru1 N2 83.43(16) . . ? N1 Ru1 N2 91.47(17) . . ? O1 Ru1 C24 97.50(19) . . ? N1 Ru1 C24 103.09(19) . . ? N2 Ru1 C24 165.43(19) . . ? O1 Ru1 C19 85.1(2) . . ? N1 Ru1 C19 137.5(2) . . ? N2 Ru1 C19 128.0(2) . . ? C24 Ru1 C19 38.2(2) . . ? O1 Ru1 C20 103.55(19) . . ? N1 Ru1 C20 168.34(19) . . ? N2 Ru1 C20 97.8(2) . . ? C24 Ru1 C20 67.8(2) . . ? C19 Ru1 C20 37.3(2) . . ? O1 Ru1 C23 130.9(2) . . ? N1 Ru1 C23 88.69(19) . . ? N2 Ru1 C23 145.5(2) . . ? C24 Ru1 C23 37.5(2) . . ? C19 Ru1 C23 68.1(2) . . ? C20 Ru1 C23 79.7(2) . . ? O1 Ru1 C22 163.98(17) . . ? N1 Ru1 C22 103.39(18) . . ? N2 Ru1 C22 109.98(19) . . ? C24 Ru1 C22 67.3(2) . . ? C19 Ru1 C22 79.8(2) . . ? C20 Ru1 C22 66.8(2) . . ? C23 Ru1 C22 37.2(2) . . ? O1 Ru1 C21 138.91(18) . . ? N1 Ru1 C21 136.45(19) . . ? N2 Ru1 C21 90.17(19) . . ? C24 Ru1 C21 79.5(2) . . ? C19 Ru1 C21 67.3(2) . . ? C20 Ru1 C21 37.15(19) . . ? C23 Ru1 C21 66.9(2) . . ? C22 Ru1 C21 36.77(18) . . ? F6 Sb2 F3 90.6(2) . . ? F6 Sb2 F4 90.72(19) . . ? F3 Sb2 F4 90.2(2) . . ? F6 Sb2 F5 90.8(2) . . ? F3 Sb2 F5 177.8(2) . . ? F4 Sb2 F5 91.6(2) . . ? F6 Sb2 F2 179.2(2) . . ? F3 Sb2 F2 89.4(2) . . ? F4 Sb2 F2 90.09(19) . . ? F5 Sb2 F2 89.24(19) . . ? F6 Sb2 F1 89.5(2) . . ? F3 Sb2 F1 88.7(2) . . ? F4 Sb2 F1 178.87(19) . . ? F5 Sb2 F1 89.54(18) . . ? F2 Sb2 F1 89.74(19) . . ? C7 N1 C8 106.5(4) . . ? C7 N1 Ru1 123.5(4) . . ? C8 N1 Ru1 129.1(3) . . ? C24 C23 C22 119.7(5) . . ? C24 C23 C27 119.4(6) . . ? C22 C23 C27 120.9(6) . . ? C24 C23 Ru1 70.6(3) . . ? C22 C23 Ru1 71.9(3) . . ? C27 C23 Ru1 129.6(4) . . ? C13 N2 C17 116.0(5) . . ? C13 N2 Ru1 122.4(4) . . ? C17 N2 Ru1 120.9(4) . . ? N2 C17 C16 122.8(5) . . ? C23 C22 C21 121.3(5) . . ? C23 C22 Ru1 70.9(3) . . ? C21 C22 Ru1 73.2(3) . . ? C23 C24 C19 120.0(6) . . ? C23 C24 Ru1 72.0(3) . . ? C19 C24 Ru1 70.9(3) . . ? C15 C16 C17 120.9(6) . . ? C20 C19 C24 119.2(6) . . ? C20 C19 C25 120.8(6) . . ? C24 C19 C25 120.0(6) . . ? C20 C19 Ru1 71.7(3) . . ? C24 C19 Ru1 70.9(3) . . ? C25 C19 Ru1 125.9(4) . . ? N2 C13 C14 123.7(6) . . ? C19 C20 C21 121.6(6) . . ? C19 C20 Ru1 71.0(3) . . ? C21 C20 Ru1 73.9(3) . . ? C22 C21 C20 118.2(5) . . ? C22 C21 C26 122.9(6) . . ? C20 C21 C26 118.9(6) . . ? C22 C21 Ru1 70.0(3) . . ? C20 C21 Ru1 69.0(3) . . ? C26 C21 Ru1 132.9(4) . . ? C1 O1 Ru1 127.3(4) . . ? C7 O2 C9 106.3(4) . . ? N1 C7 O2 116.2(5) . . ? N1 C7 C6 127.2(5) . . ? O2 C7 C6 116.5(5) . . ? C4 C5 C6 120.1(6) . . ? C13 C14 C15 119.8(6) . . ? N1 C8 C9 101.9(4) . . ? N1 C8 C10 111.5(4) . . ? C9 C8 C10 114.9(5) . . ? O1 C1 C6 124.5(5) . . ? O1 C1 C2 118.1(6) . . ? C6 C1 C2 117.4(6) . . ? C11 C10 C12 111.1(5) . . ? C11 C10 C8 113.2(5) . . ? C12 C10 C8 110.1(5) . . ? O2 C9 C8 104.1(4) . . ? C16 C15 C14 116.7(6) . . ? C16 C15 C18 121.8(6) . . ? C14 C15 C18 121.4(6) . . ? C5 C6 C1 119.6(6) . . ? C5 C6 C7 119.2(6) . . ? C1 C6 C7 120.8(5) . . ? C3 C2 C1 121.4(6) . . ? C2 C3 C4 120.9(6) . . ? C5 C4 C3 120.4(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.760 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.076 #===END data_1022 _database_code_depnum_ccdc_archive 'CCDC 228966' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C39 H41 N O2 P Ru)(C24 H20 B)' _chemical_formula_sum 'C63 H61 B N O2 P Ru' _chemical_formula_weight 1006.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.8561(6) _cell_length_b 16.7720(7) _cell_length_c 20.3864(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.7740(10) _cell_angle_gamma 90.00 _cell_volume 5005.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5141 _cell_measurement_theta_min 4.40 _cell_measurement_theta_max 39.82 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.392 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; sadabs ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.70 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 42686 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.1436 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 27.00 _reflns_number_total 20957 _reflns_number_gt 13185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.022(19) _refine_ls_number_reflns 20957 _refine_ls_number_parameters 1253 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 0.760 _refine_ls_restrained_S_all 0.760 _refine_ls_shift/su_max 0.171 _refine_ls_shift/su_mean 0.016 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 0.80446(3) 0.22055(2) 0.28233(2) 0.02814(11) Uani 1 1 d . . . P1 P 0.75658(9) 0.09299(8) 0.23993(7) 0.0266(3) Uani 1 1 d . . . C34 C 0.6390(3) 0.0827(3) 0.1957(2) 0.0268(12) Uani 1 1 d . . . O1 O 0.8973(2) 0.1554(2) 0.34660(18) 0.0328(9) Uani 1 1 d . . . N1 N 0.7336(2) 0.2247(3) 0.36307(18) 0.0282(9) Uani 1 1 d . . . O2 O 0.7275(2) 0.2653(2) 0.46775(15) 0.0417(9) Uani 1 1 d . . . C27 C 0.7654(3) 0.0167(3) 0.3611(3) 0.0348(14) Uani 1 1 d . . . H27 H 0.7522 0.0679 0.3771 0.042 Uiso 1 1 calc R . . C6 C 0.8729(3) 0.2224(3) 0.4469(2) 0.0317(12) Uani 1 1 d . . . C1 C 0.9265(4) 0.1812(3) 0.4071(3) 0.0342(13) Uani 1 1 d . . . C23 C 0.7967(3) -0.0690(3) 0.2721(3) 0.0309(13) Uani 1 1 d . . . H23 H 0.8038 -0.0764 0.2271 0.037 Uiso 1 1 calc R . . C29 C 0.9186(3) 0.0517(3) 0.1999(3) 0.0354(13) Uani 1 1 d . . . H29 H 0.9422 0.0583 0.2458 0.042 Uiso 1 1 calc R . . C18 C 0.7395(4) 0.3250(3) 0.2275(3) 0.0430(17) Uani 1 1 d . . . H18 H 0.6723 0.3328 0.2253 0.052 Uiso 1 1 calc R . . C35 C 0.6085(4) 0.0128(3) 0.1630(2) 0.0355(14) Uani 1 1 d . . . H35 H 0.6492 -0.0310 0.1642 0.043 Uiso 1 1 calc R . . C38 C 0.4872(4) 0.1363(4) 0.1606(3) 0.0435(15) Uani 1 1 d . . . H38 H 0.4453 0.1792 0.1597 0.052 Uiso 1 1 calc R . . C20 C 1.0188(3) 0.2519(4) 0.2595(3) 0.0553(17) Uani 1 1 d . . . H20A H 1.0574 0.2950 0.2474 0.083 Uiso 1 1 calc R . . H20B H 1.0255 0.2047 0.2324 0.083 Uiso 1 1 calc R . . H20C H 1.0375 0.2387 0.3067 0.083 Uiso 1 1 calc R . . C10 C 0.5798(3) 0.1628(3) 0.3629(3) 0.0367(14) Uani 1 1 d . . . H10 H 0.5994 0.1270 0.3287 0.044 Uiso 1 1 calc R . . C7 C 0.7779(3) 0.2371(3) 0.4235(3) 0.0325(13) Uani 1 1 d . . . C33 C 0.7942(4) 0.0542(3) 0.1102(3) 0.0350(14) Uani 1 1 d . . . H33 H 0.7313 0.0618 0.0930 0.042 Uiso 1 1 calc R . . C19 C 0.7073(3) 0.2559(4) 0.1173(2) 0.0452(14) Uani 1 1 d . . . H19A H 0.6433 0.2619 0.1228 0.068 Uiso 1 1 calc R . . H19B H 0.7184 0.2005 0.1056 0.068 Uiso 1 1 calc R . . H19C H 0.7200 0.2914 0.0819 0.068 Uiso 1 1 calc R . . C28 C 0.8260(3) 0.0640(3) 0.1772(3) 0.0310(13) Uani 1 1 d . . . C15 C 0.9218(4) 0.2781(3) 0.2476(3) 0.0386(14) Uani 1 1 d . . . C32 C 0.8538(4) 0.0332(3) 0.0679(3) 0.0415(15) Uani 1 1 d . . . H32 H 0.8311 0.0274 0.0217 0.050 Uiso 1 1 calc R . . C22 C 0.7752(3) 0.0070(3) 0.2955(2) 0.0285(12) Uani 1 1 d . . . C4 C 1.0017(4) 0.2334(4) 0.5365(3) 0.0481(17) Uani 1 1 d . . . H4 H 1.0282 0.2515 0.5797 0.058 Uiso 1 1 calc R . . C2 C 1.0184(4) 0.1646(3) 0.4355(3) 0.0392(15) Uani 1 1 d . . . H2 H 1.0559 0.1347 0.4111 0.047 Uiso 1 1 calc R . . C36 C 0.5210(4) 0.0053(4) 0.1292(3) 0.0485(17) Uani 1 1 d . . . H36 H 0.5024 -0.0428 0.1062 0.058 Uiso 1 1 calc R . . C25 C 0.7969(4) -0.1229(3) 0.3801(3) 0.0414(15) Uani 1 1 d . . . H25 H 0.8048 -0.1675 0.4092 0.050 Uiso 1 1 calc R . . C31 C 0.9436(4) 0.0206(4) 0.0906(3) 0.0467(17) Uani 1 1 d . . . H31 H 0.9833 0.0054 0.0609 0.056 Uiso 1 1 calc R . . C37 C 0.4605(4) 0.0666(4) 0.1285(3) 0.0512(17) Uani 1 1 d . . . H37 H 0.3996 0.0608 0.1057 0.061 Uiso 1 1 calc R . . C39 C 0.5770(4) 0.1443(3) 0.1949(2) 0.0346(14) Uani 1 1 d . . . H39 H 0.5953 0.1925 0.2178 0.042 Uiso 1 1 calc R . . C26 C 0.7749(3) -0.0488(3) 0.4040(3) 0.0387(14) Uani 1 1 d . . . H26 H 0.7665 -0.0430 0.4489 0.046 Uiso 1 1 calc R . . C9 C 0.6351(3) 0.2406(3) 0.3645(2) 0.0338(13) Uani 1 1 d . . . H9 H 0.6092 0.2747 0.3256 0.041 Uiso 1 1 calc R . . C11 C 0.5955(4) 0.1188(3) 0.4288(3) 0.0471(16) Uani 1 1 d . . . H11A H 0.6612 0.1118 0.4440 0.071 Uiso 1 1 calc R . . H11B H 0.5659 0.0664 0.4232 0.071 Uiso 1 1 calc R . . H11C H 0.5695 0.1497 0.4619 0.071 Uiso 1 1 calc R . . C17 C 0.7989(5) 0.3552(3) 0.2833(3) 0.0403(15) Uani 1 1 d . . . C30 C 0.9767(4) 0.0301(3) 0.1572(3) 0.0456(16) Uani 1 1 d . . . H30 H 1.0398 0.0218 0.1738 0.055 Uiso 1 1 calc R . . C3 C 1.0533(4) 0.1917(3) 0.4981(3) 0.0485(17) Uani 1 1 d . . . H3 H 1.1156 0.1812 0.5157 0.058 Uiso 1 1 calc R . . C14 C 0.8609(3) 0.2535(3) 0.1911(2) 0.0370(13) Uani 1 1 d . . . H14 H 0.8799 0.2100 0.1628 0.044 Uiso 1 1 calc R . . C12 C 0.4779(3) 0.1820(3) 0.3402(3) 0.0538(17) Uani 1 1 d . . . H12A H 0.4419 0.1331 0.3405 0.081 Uiso 1 1 calc R . . H12B H 0.4688 0.2041 0.2951 0.081 Uiso 1 1 calc R . . H12C H 0.4583 0.2210 0.3707 0.081 Uiso 1 1 calc R . . C8 C 0.6396(4) 0.2881(3) 0.4285(3) 0.0449(15) Uani 1 1 d . . . H8A H 0.6373 0.3461 0.4193 0.054 Uiso 1 1 calc R . . H8B H 0.5886 0.2737 0.4518 0.054 Uiso 1 1 calc R . . C13 C 0.7683(4) 0.2769(3) 0.1811(3) 0.0354(13) Uani 1 1 d . . . C24 C 0.8071(4) -0.1317(3) 0.3161(3) 0.0382(14) Uani 1 1 d . . . H24 H 0.8218 -0.1828 0.3009 0.046 Uiso 1 1 calc R . . C16 C 0.8902(4) 0.3309(3) 0.2928(3) 0.0411(16) Uani 1 1 d . . . H16 H 0.9303 0.3422 0.3364 0.049 Uiso 1 1 calc R . . C5 C 0.9121(4) 0.2484(3) 0.5120(2) 0.0392(14) Uani 1 1 d . . . H5 H 0.8756 0.2764 0.5384 0.047 Uiso 1 1 calc R . . Ru2 Ru 0.24029(3) 0.75820(2) 0.25098(2) 0.03029(11) Uani 1 1 d . . . P1A P 0.24082(9) 0.83334(8) 0.15217(7) 0.0280(3) Uani 1 1 d . . . O1A O 0.1495(2) 0.8463(2) 0.26576(18) 0.0396(10) Uani 1 1 d . . . N1A N 0.3357(3) 0.8279(2) 0.3133(2) 0.0305(11) Uani 1 1 d . . . C27A C 0.0544(4) 0.8205(3) 0.1079(3) 0.0356(14) Uani 1 1 d . . . H27A H 0.0502 0.8502 0.1470 0.043 Uiso 1 1 calc R . . C47A C 0.2473(3) 0.2179(4) 0.3681(2) 0.0324(12) Uani 1 1 d . . . H47A H 0.2105 0.2252 0.3256 0.039 Uiso 1 1 calc R . . C18A C 0.3109(4) 0.6402(3) 0.2555(3) 0.0454(17) Uani 1 1 d . . . H18A H 0.3771 0.6391 0.2516 0.054 Uiso 1 1 calc R . . C45A C 0.4170(3) 0.4510(3) 0.4464(3) 0.0320(13) Uani 1 1 d . . . H45A H 0.3856 0.4426 0.4828 0.038 Uiso 1 1 calc R . . C35A C 0.1885(3) 0.9837(3) 0.0972(3) 0.0295(13) Uani 1 1 d . . . H35A H 0.1670 0.9552 0.0573 0.035 Uiso 1 1 calc R . . C34A C 0.2260(3) 0.9418(3) 0.1540(3) 0.0269(12) Uani 1 1 d . . . C23A C 0.1443(3) 0.7591(3) 0.0360(2) 0.0367(13) Uani 1 1 d . . . H23A H 0.2020 0.7461 0.0246 0.044 Uiso 1 1 calc R . . C28A C 0.3369(3) 0.8218(3) 0.1068(3) 0.0305(13) Uani 1 1 d . . . C40A C 0.3754(3) 0.4247(3) 0.3827(3) 0.0297(13) Uani 1 1 d . . . C1A C 0.1485(3) 0.8814(3) 0.3228(3) 0.0318(13) Uani 1 1 d . . . O2A O 0.3850(2) 0.8804(2) 0.41405(17) 0.0416(10) Uani 1 1 d . . . C22A C 0.1397(3) 0.8030(3) 0.0921(2) 0.0299(12) Uani 1 1 d . . . C13A C 0.1302(4) 0.6750(3) 0.2637(3) 0.0403(15) Uani 1 1 d . . . C16A C 0.1580(4) 0.6559(3) 0.2036(3) 0.0381(15) Uani 1 1 d . . . H16A H 0.1143 0.6661 0.1614 0.046 Uiso 1 1 calc R . . C54A C 0.1238(4) 0.5393(3) 0.4364(3) 0.0476(17) Uani 1 1 d . . . H54A H 0.1233 0.5957 0.4400 0.057 Uiso 1 1 calc R . . C51A C 0.3462(3) 0.2677(3) 0.4623(2) 0.0357(13) Uani 1 1 d . . . H51A H 0.3792 0.3102 0.4860 0.043 Uiso 1 1 calc R . . C29A C 0.4079(3) 0.7702(3) 0.1320(3) 0.0363(13) Uani 1 1 d . . . H29A H 0.4064 0.7426 0.1725 0.044 Uiso 1 1 calc R . . C44A C 0.5010(3) 0.4883(3) 0.4585(3) 0.0356(13) Uani 1 1 d . . . H44A H 0.5270 0.5032 0.5026 0.043 Uiso 1 1 calc R . . C6A C 0.2244(4) 0.8892(3) 0.3749(3) 0.0322(13) Uani 1 1 d . . . C30A C 0.4803(3) 0.7590(4) 0.0985(3) 0.0487(15) Uani 1 1 d . . . H30A H 0.5279 0.7229 0.1153 0.058 Uiso 1 1 calc R . . C41A C 0.4255(3) 0.4436(3) 0.3320(3) 0.0352(13) Uani 1 1 d . . . H41A H 0.4003 0.4290 0.2877 0.042 Uiso 1 1 calc R . . C33A C 0.3420(3) 0.8630(3) 0.0487(3) 0.0344(13) Uani 1 1 d . . . H33A H 0.2945 0.8989 0.0310 0.041 Uiso 1 1 calc R . . C4A C 0.1328(4) 0.9568(3) 0.4449(3) 0.0445(16) Uani 1 1 d . . . H4A H 0.1261 0.9810 0.4859 0.053 Uiso 1 1 calc R . . C57A C 0.1273(3) 0.3765(3) 0.4258(2) 0.0327(13) Uani 1 1 d . . . H57A H 0.1280 0.3199 0.4234 0.039 Uiso 1 1 calc R . . C43A C 0.5473(4) 0.5038(3) 0.4065(3) 0.0410(15) Uani 1 1 d . . . H43A H 0.6053 0.5293 0.4145 0.049 Uiso 1 1 calc R . . C26A C -0.0243(4) 0.7951(3) 0.0670(3) 0.0447(15) Uani 1 1 d . . . H26A H -0.0825 0.8078 0.0776 0.054 Uiso 1 1 calc R . . C9A C 0.4373(3) 0.8232(3) 0.3212(3) 0.0339(13) Uani 1 1 d . . . H9A H 0.4560 0.7678 0.3115 0.041 Uiso 1 1 calc R . . C48A C 0.2538(3) 0.1426(3) 0.3958(3) 0.0341(14) Uani 1 1 d . . . H48A H 0.2212 0.0995 0.3726 0.041 Uiso 1 1 calc R . . C5A C 0.2151(4) 0.9278(3) 0.4353(3) 0.0399(15) Uani 1 1 d . . . H5A H 0.2669 0.9334 0.4694 0.048 Uiso 1 1 calc R . . B1A B 0.2773(4) 0.3759(4) 0.3697(3) 0.0293(14) Uani 1 1 d . . . C50A C 0.3526(4) 0.1931(3) 0.4901(3) 0.0423(15) Uani 1 1 d . . . H50A H 0.3886 0.1851 0.5328 0.051 Uiso 1 1 calc R . . C7A C 0.3135(4) 0.8631(3) 0.3646(3) 0.0340(13) Uani 1 1 d . . . C31A C 0.4830(4) 0.8005(4) 0.0406(3) 0.0454(16) Uani 1 1 d . . . H31A H 0.5326 0.7927 0.0174 0.055 Uiso 1 1 calc R . . C39A C 0.2546(3) 0.9847(3) 0.2115(3) 0.0357(14) Uani 1 1 d . . . H39A H 0.2779 0.9573 0.2516 0.043 Uiso 1 1 calc R . . C24A C 0.0649(4) 0.7336(3) -0.0041(3) 0.0429(15) Uani 1 1 d . . . H24A H 0.0686 0.7032 -0.0429 0.051 Uiso 1 1 calc R . . C32A C 0.4153(3) 0.8525(3) 0.0166(3) 0.0350(14) Uani 1 1 d . . . H32A H 0.4187 0.8818 -0.0228 0.042 Uiso 1 1 calc R . . C46A C 0.2922(3) 0.2834(3) 0.3997(2) 0.0265(12) Uani 1 1 d . . . C53A C 0.1958(4) 0.5010(3) 0.4141(3) 0.0408(15) Uani 1 1 d . . . H53A H 0.2446 0.5325 0.4037 0.049 Uiso 1 1 calc R . . C36A C 0.1819(3) 1.0649(3) 0.0972(3) 0.0388(14) Uani 1 1 d . . . H36A H 0.1562 1.0923 0.0577 0.047 Uiso 1 1 calc R . . C42A C 0.5074(4) 0.4815(3) 0.3421(3) 0.0429(15) Uani 1 1 d . . . H42A H 0.5374 0.4927 0.3056 0.052 Uiso 1 1 calc R . . C63A C 0.2775(4) 0.3285(3) 0.2445(3) 0.0438(15) Uani 1 1 d . . . H63A H 0.3248 0.2923 0.2617 0.053 Uiso 1 1 calc R . . C58A C 0.2393(4) 0.3753(3) 0.2902(3) 0.0301(13) Uani 1 1 d . . . C49A C 0.3073(4) 0.1300(3) 0.4567(3) 0.0401(15) Uani 1 1 d . . . H49A H 0.3130 0.0781 0.4756 0.048 Uiso 1 1 calc R . . C2A C 0.0652(4) 0.9130(3) 0.3343(3) 0.0431(15) Uani 1 1 d . . . H2A H 0.0127 0.9085 0.3007 0.052 Uiso 1 1 calc R . . C8A C 0.4645(4) 0.8408(3) 0.3961(3) 0.0430(16) Uani 1 1 d . . . H8A1 H 0.4781 0.7908 0.4217 0.052 Uiso 1 1 calc R . . H8A2 H 0.5188 0.8759 0.4046 0.052 Uiso 1 1 calc R . . C25A C -0.0180(4) 0.7514(4) 0.0113(3) 0.0481(15) Uani 1 1 d . . . H25A H -0.0719 0.7336 -0.0168 0.058 Uiso 1 1 calc R . . C59A C 0.1713(4) 0.4269(3) 0.2578(3) 0.0432(15) Uani 1 1 d . . . H59A H 0.1433 0.4624 0.2847 0.052 Uiso 1 1 calc R . . C52A C 0.2001(3) 0.4188(3) 0.4063(2) 0.0294(12) Uani 1 1 d . . . C3A C 0.0582(4) 0.9504(3) 0.3933(3) 0.0479(17) Uani 1 1 d . . . H3A H 0.0012 0.9724 0.3990 0.057 Uiso 1 1 calc R . . C37A C 0.2122(4) 1.1066(3) 0.1544(3) 0.0416(16) Uani 1 1 d . . . H37A H 0.2073 1.1630 0.1545 0.050 Uiso 1 1 calc R . . C38A C 0.2496(4) 1.0670(3) 0.2114(3) 0.0434(15) Uani 1 1 d . . . H38A H 0.2720 1.0961 0.2508 0.052 Uiso 1 1 calc R . . C56A C 0.0547(3) 0.4129(3) 0.4483(3) 0.0386(14) Uani 1 1 d . . . H56A H 0.0065 0.3817 0.4602 0.046 Uiso 1 1 calc R . . C14A C 0.2873(4) 0.6568(3) 0.3183(3) 0.0493(17) Uani 1 1 d . . . C19A C 0.3587(4) 0.6555(3) 0.3819(3) 0.064(2) Uani 1 1 d . . . H19D H 0.3644 0.6012 0.3999 0.096 Uiso 1 1 calc R . . H19E H 0.3397 0.6915 0.4149 0.096 Uiso 1 1 calc R . . H19F H 0.4178 0.6730 0.3718 0.096 Uiso 1 1 calc R . . C15A C 0.1968(4) 0.6752(3) 0.3218(3) 0.0441(16) Uani 1 1 d . . . H15A H 0.1808 0.6958 0.3644 0.053 Uiso 1 1 calc R . . C41 C 0.7246(3) 0.7573(4) 0.1267(2) 0.0357(12) Uani 1 1 d . . . H41 H 0.7288 0.7604 0.1737 0.043 Uiso 1 1 calc R . . C50 C 0.8632(4) 0.4222(3) 0.0835(3) 0.0405(15) Uani 1 1 d . . . H50 H 0.8573 0.3662 0.0773 0.049 Uiso 1 1 calc R . . C59 C 0.8149(4) 0.6023(3) 0.2567(3) 0.0470(17) Uani 1 1 d . . . H59 H 0.8653 0.5841 0.2376 0.056 Uiso 1 1 calc R . . C43 C 0.7258(4) 0.8251(4) 0.0242(3) 0.0490(17) Uani 1 1 d . . . H43 H 0.7300 0.8728 -0.0004 0.059 Uiso 1 1 calc R . . C46 C 0.7943(3) 0.5458(3) 0.1133(2) 0.0318(13) Uani 1 1 d . . . C47 C 0.8756(4) 0.5823(3) 0.1017(3) 0.0409(14) Uani 1 1 d . . . H47 H 0.8822 0.6381 0.1086 0.049 Uiso 1 1 calc R . . C40 C 0.7106(3) 0.6827(3) 0.0962(3) 0.0309(13) Uani 1 1 d . . . C57 C 0.5927(4) 0.4900(3) 0.1601(3) 0.0371(14) Uani 1 1 d . . . H57 H 0.6356 0.4788 0.1992 0.045 Uiso 1 1 calc R . . C60 C 0.8274(4) 0.6177(4) 0.3254(3) 0.0535(19) Uani 1 1 d . . . H60 H 0.8858 0.6101 0.3519 0.064 Uiso 1 1 calc R . . B1 B 0.7113(4) 0.5975(4) 0.1356(3) 0.0309(15) Uani 1 1 d . . . C53 C 0.5472(4) 0.5621(3) 0.0622(3) 0.0386(14) Uani 1 1 d . . . H53 H 0.5570 0.6016 0.0308 0.046 Uiso 1 1 calc R . . C58 C 0.7301(4) 0.6131(3) 0.2157(3) 0.0343(14) Uani 1 1 d . . . C44 C 0.7127(4) 0.7526(4) -0.0081(3) 0.0476(15) Uani 1 1 d . . . H44 H 0.7087 0.7502 -0.0550 0.057 Uiso 1 1 calc R . . C62 C 0.6718(5) 0.6555(3) 0.3155(3) 0.0537(17) Uani 1 1 d . . . H62 H 0.6216 0.6737 0.3347 0.064 Uiso 1 1 calc R . . C45 C 0.7053(4) 0.6846(4) 0.0269(3) 0.0414(15) Uani 1 1 d . . . H45 H 0.6961 0.6357 0.0031 0.050 Uiso 1 1 calc R . . C51 C 0.7931(4) 0.4634(3) 0.1040(3) 0.0363(14) Uani 1 1 d . . . H51 H 0.7412 0.4344 0.1121 0.044 Uiso 1 1 calc R . . C52 C 0.6140(4) 0.5495(3) 0.1175(3) 0.0343(14) Uani 1 1 d . . . C55 C 0.4483(4) 0.4612(4) 0.0942(3) 0.0500(17) Uani 1 1 d . . . H55 H 0.3925 0.4323 0.0865 0.060 Uiso 1 1 calc R . . C42 C 0.7327(4) 0.8276(4) 0.0912(3) 0.0433(16) Uani 1 1 d . . . H42 H 0.7430 0.8769 0.1141 0.052 Uiso 1 1 calc R . . C54 C 0.4656(4) 0.5183(4) 0.0511(3) 0.0504(17) Uani 1 1 d . . . H54 H 0.4216 0.5289 0.0126 0.060 Uiso 1 1 calc R . . C48 C 0.9462(4) 0.5412(4) 0.0807(3) 0.0476(16) Uani 1 1 d . . . H48 H 0.9986 0.5692 0.0722 0.057 Uiso 1 1 calc R . . C63 C 0.6609(4) 0.6405(3) 0.2474(3) 0.0449(16) Uani 1 1 d . . . H63 H 0.6025 0.6496 0.2213 0.054 Uiso 1 1 calc R . . C56 C 0.5122(4) 0.4462(4) 0.1484(3) 0.0482(17) Uani 1 1 d . . . H56 H 0.5019 0.4055 0.1787 0.058 Uiso 1 1 calc R . . C49 C 0.9407(4) 0.4587(4) 0.0719(3) 0.0438(16) Uani 1 1 d . . . H49 H 0.9891 0.4293 0.0584 0.053 Uiso 1 1 calc R . . C10A C 0.4767(4) 0.8819(3) 0.2769(3) 0.0375(14) Uani 1 1 d . . . H10A H 0.4379 0.8791 0.2318 0.045 Uiso 1 1 calc R . . C62A C 0.2506(5) 0.3321(4) 0.1767(3) 0.0548(19) Uani 1 1 d . . . H62A H 0.2794 0.2983 0.1491 0.066 Uiso 1 1 calc R . . C61 C 0.7554(5) 0.6438(4) 0.3545(3) 0.0508(18) Uani 1 1 d . . . H61 H 0.7636 0.6536 0.4011 0.061 Uiso 1 1 calc R . . C11A C 0.4766(4) 0.9688(3) 0.2999(3) 0.0513(17) Uani 1 1 d . . . H11D H 0.5261 0.9770 0.3376 0.077 Uiso 1 1 calc R . . H11E H 0.4179 0.9810 0.3135 0.077 Uiso 1 1 calc R . . H11F H 0.4855 1.0040 0.2632 0.077 Uiso 1 1 calc R . . C17A C 0.2485(4) 0.6379(3) 0.1989(3) 0.0427(15) Uani 1 1 d . . . C61A C 0.1843(5) 0.3823(4) 0.1483(3) 0.0579(19) Uani 1 1 d . . . H61A H 0.1670 0.3850 0.1013 0.069 Uiso 1 1 calc R . . C21 C 0.7658(5) 0.4115(3) 0.3321(3) 0.062(2) Uani 1 1 d . . . H21A H 0.8054 0.4070 0.3756 0.093 Uiso 1 1 calc R . . H21B H 0.7030 0.3976 0.3365 0.093 Uiso 1 1 calc R . . H21C H 0.7674 0.4664 0.3158 0.093 Uiso 1 1 calc R . . C60A C 0.1423(4) 0.4298(4) 0.1897(3) 0.0589(19) Uani 1 1 d . . . H60A H 0.0937 0.4642 0.1714 0.071 Uiso 1 1 calc R . . C55A C 0.0529(4) 0.4945(4) 0.4533(3) 0.0480(16) Uani 1 1 d . . . H55A H 0.0032 0.5202 0.4684 0.058 Uiso 1 1 calc R . . C20A C 0.0328(4) 0.6962(4) 0.2665(3) 0.071(2) Uani 1 1 d . . . H20D H -0.0020 0.6989 0.2212 0.107 Uiso 1 1 calc R . . H20E H 0.0307 0.7481 0.2883 0.107 Uiso 1 1 calc R . . H20F H 0.0061 0.6554 0.2918 0.107 Uiso 1 1 calc R . . C21A C 0.2744(5) 0.6092(4) 0.1353(3) 0.064(2) Uani 1 1 d . . . H21D H 0.3398 0.6182 0.1363 0.097 Uiso 1 1 calc R . . H21E H 0.2393 0.6384 0.0978 0.097 Uiso 1 1 calc R . . H21F H 0.2612 0.5521 0.1301 0.097 Uiso 1 1 calc R . . C12A C 0.5720(4) 0.8547(4) 0.2694(3) 0.0606(19) Uani 1 1 d . . . H12D H 0.5989 0.8935 0.2425 0.091 Uiso 1 1 calc R . . H12E H 0.5683 0.8025 0.2474 0.091 Uiso 1 1 calc R . . H12F H 0.6102 0.8505 0.3135 0.091 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 0.0290(2) 0.0264(2) 0.0280(2) 0.0026(2) 0.00195(19) -0.0025(2) P1 0.0253(8) 0.0277(8) 0.0270(8) 0.0015(6) 0.0049(6) -0.0006(6) C34 0.023(3) 0.037(3) 0.019(3) 0.002(2) 0.002(2) 0.000(2) O1 0.024(2) 0.038(2) 0.033(2) -0.0044(18) -0.0036(17) 0.0015(18) N1 0.032(2) 0.024(2) 0.028(2) -0.003(2) 0.0041(19) -0.002(2) O2 0.046(2) 0.044(2) 0.034(2) -0.0134(19) 0.0041(18) 0.002(2) C27 0.032(3) 0.035(3) 0.036(4) -0.002(3) 0.003(3) 0.000(3) C6 0.037(3) 0.027(3) 0.028(3) 0.002(3) -0.002(2) -0.015(3) C1 0.037(3) 0.026(3) 0.038(4) 0.007(3) 0.001(3) -0.012(3) C23 0.028(3) 0.034(3) 0.031(3) 0.000(3) 0.005(3) 0.004(3) C29 0.030(3) 0.040(3) 0.034(3) 0.006(3) -0.002(3) -0.001(3) C18 0.046(4) 0.035(4) 0.046(4) 0.020(3) 0.004(3) 0.003(3) C35 0.030(3) 0.044(4) 0.032(3) -0.007(3) 0.004(3) -0.003(3) C38 0.025(3) 0.061(4) 0.042(4) 0.002(3) -0.002(3) 0.006(3) C20 0.036(3) 0.071(5) 0.057(4) 0.004(4) 0.004(3) -0.018(3) C10 0.034(3) 0.036(3) 0.042(4) -0.003(3) 0.013(3) 0.001(3) C7 0.038(3) 0.022(3) 0.039(3) 0.000(2) 0.011(3) -0.002(2) C33 0.038(3) 0.034(3) 0.032(3) -0.001(3) 0.005(3) 0.000(3) C19 0.054(4) 0.046(3) 0.033(3) 0.015(3) -0.002(3) 0.006(3) C28 0.027(3) 0.028(3) 0.041(3) 0.001(3) 0.014(3) -0.002(2) C15 0.044(4) 0.034(4) 0.039(3) 0.012(3) 0.012(3) -0.014(3) C32 0.051(4) 0.039(4) 0.038(4) 0.000(3) 0.017(3) -0.004(3) C22 0.026(3) 0.029(3) 0.030(3) 0.005(2) 0.005(2) 0.000(2) C4 0.053(4) 0.051(5) 0.033(3) 0.007(3) -0.016(3) -0.020(3) C2 0.036(4) 0.041(4) 0.039(4) 0.007(3) 0.002(3) -0.002(3) C36 0.031(4) 0.063(5) 0.051(4) -0.017(3) 0.007(3) -0.016(3) C25 0.032(3) 0.031(3) 0.059(4) 0.012(3) 0.001(3) 0.001(3) C31 0.050(4) 0.051(4) 0.045(4) 0.004(3) 0.024(3) 0.012(3) C37 0.029(3) 0.077(5) 0.043(4) -0.003(4) -0.007(3) -0.011(3) C39 0.044(4) 0.038(3) 0.021(3) 0.001(3) 0.005(3) 0.003(3) C26 0.035(3) 0.051(4) 0.032(3) 0.010(3) 0.011(3) -0.002(3) C9 0.034(3) 0.038(4) 0.029(3) -0.002(2) 0.006(2) 0.008(2) C11 0.049(4) 0.047(4) 0.049(4) -0.011(3) 0.020(3) -0.013(3) C17 0.068(5) 0.012(3) 0.045(4) 0.000(3) 0.019(3) -0.008(3) C30 0.022(3) 0.053(4) 0.067(5) 0.000(3) 0.020(3) 0.003(3) C3 0.033(4) 0.047(4) 0.059(4) 0.020(3) -0.010(3) -0.013(3) C14 0.039(3) 0.039(3) 0.033(3) 0.005(3) 0.007(2) -0.010(3) C12 0.030(3) 0.068(5) 0.065(4) -0.010(3) 0.012(3) 0.004(3) C8 0.041(4) 0.044(4) 0.051(4) -0.002(3) 0.011(3) 0.009(3) C13 0.052(4) 0.027(3) 0.028(3) 0.007(2) 0.008(3) 0.002(3) C24 0.035(3) 0.032(3) 0.050(4) -0.001(3) 0.013(3) 0.004(3) C16 0.050(4) 0.034(4) 0.034(4) 0.012(3) -0.007(3) -0.016(3) C5 0.048(3) 0.029(3) 0.039(3) 0.007(3) 0.004(3) -0.014(3) Ru2 0.0299(3) 0.0297(2) 0.0313(2) 0.0028(2) 0.0052(2) -0.0037(2) P1A 0.0267(8) 0.0282(8) 0.0293(8) 0.0007(6) 0.0052(6) 0.0000(6) O1A 0.029(2) 0.057(3) 0.034(2) -0.003(2) 0.0072(18) 0.0033(18) N1A 0.028(3) 0.035(3) 0.030(3) -0.001(2) 0.008(2) 0.002(2) C27A 0.038(4) 0.037(3) 0.031(3) -0.001(3) 0.005(3) 0.003(3) C47A 0.030(3) 0.036(3) 0.031(3) -0.007(3) 0.005(2) -0.005(3) C18A 0.049(4) 0.024(3) 0.068(5) 0.009(3) 0.023(4) -0.004(3) C45A 0.035(3) 0.030(3) 0.034(3) 0.004(3) 0.014(3) -0.001(3) C35A 0.028(3) 0.032(3) 0.028(3) -0.002(3) 0.004(2) 0.000(2) C34A 0.021(3) 0.024(3) 0.037(3) 0.001(2) 0.011(2) 0.003(2) C23A 0.038(3) 0.036(3) 0.038(3) -0.007(3) 0.011(3) -0.007(3) C28A 0.026(3) 0.029(3) 0.036(3) -0.002(3) 0.003(3) -0.003(2) C40A 0.029(3) 0.029(3) 0.031(3) 0.006(3) 0.004(3) 0.001(2) C1A 0.029(3) 0.035(3) 0.033(3) 0.007(3) 0.009(3) -0.002(3) O2A 0.039(2) 0.048(3) 0.035(2) -0.0051(19) -0.0003(19) -0.0092(19) C22A 0.031(3) 0.036(3) 0.020(3) 0.001(2) -0.002(2) 0.002(2) C13A 0.038(4) 0.041(4) 0.041(4) 0.000(3) 0.000(3) -0.018(3) C16A 0.059(4) 0.029(3) 0.024(3) 0.000(3) -0.001(3) -0.006(3) C54A 0.063(4) 0.028(3) 0.060(4) 0.009(3) 0.035(4) 0.011(3) C51A 0.039(3) 0.028(4) 0.038(3) 0.001(3) 0.003(3) -0.004(3) C29A 0.036(3) 0.033(3) 0.040(3) -0.004(3) 0.005(3) -0.005(3) C44A 0.037(3) 0.034(3) 0.035(3) -0.006(3) 0.003(3) -0.003(3) C6A 0.038(3) 0.023(3) 0.038(3) -0.002(3) 0.014(3) -0.002(2) C30A 0.028(3) 0.051(4) 0.068(4) -0.015(4) 0.009(3) 0.008(3) C41A 0.038(3) 0.040(3) 0.030(3) -0.003(3) 0.013(3) -0.006(3) C33A 0.032(3) 0.037(3) 0.034(3) -0.007(3) 0.006(3) -0.005(3) C4A 0.065(5) 0.037(4) 0.038(4) -0.007(3) 0.026(4) -0.004(3) C57A 0.034(3) 0.029(3) 0.034(3) -0.002(3) 0.002(3) -0.004(3) C43A 0.026(3) 0.045(4) 0.052(4) -0.003(3) 0.010(3) -0.010(3) C26A 0.031(3) 0.046(4) 0.057(4) -0.002(3) 0.007(3) -0.004(3) C9A 0.024(3) 0.034(3) 0.042(4) 0.000(3) 0.001(3) -0.005(2) C48A 0.028(3) 0.033(3) 0.043(4) -0.001(3) 0.013(3) -0.002(3) C5A 0.056(4) 0.028(3) 0.037(4) 0.001(3) 0.010(3) -0.007(3) B1A 0.026(3) 0.030(4) 0.033(4) 0.000(3) 0.009(3) 0.003(3) C50A 0.045(4) 0.046(4) 0.034(3) 0.008(3) 0.000(3) 0.000(3) C7A 0.031(3) 0.030(3) 0.041(4) -0.001(3) 0.006(3) -0.011(3) C31A 0.034(3) 0.059(4) 0.047(4) -0.016(3) 0.016(3) -0.003(3) C39A 0.037(3) 0.035(3) 0.034(3) 0.003(3) 0.003(3) 0.003(3) C24A 0.051(4) 0.044(4) 0.035(3) -0.009(3) 0.009(3) -0.014(3) C32A 0.027(3) 0.050(4) 0.028(3) -0.006(3) 0.007(3) -0.011(3) C46A 0.022(3) 0.030(3) 0.028(3) 0.001(2) 0.008(2) 0.002(2) C53A 0.044(4) 0.034(3) 0.049(4) 0.006(3) 0.021(3) 0.003(3) C36A 0.038(3) 0.037(4) 0.041(4) 0.004(3) 0.005(3) 0.007(3) C42A 0.049(4) 0.044(4) 0.040(4) -0.003(3) 0.018(3) -0.011(3) C63A 0.046(4) 0.037(4) 0.048(4) 0.000(3) 0.007(3) -0.007(3) C58A 0.035(3) 0.028(3) 0.029(3) -0.001(3) 0.009(3) -0.010(3) C49A 0.037(4) 0.034(3) 0.048(4) 0.009(3) 0.006(3) 0.001(3) C2A 0.041(4) 0.042(4) 0.051(4) 0.000(3) 0.020(3) 0.004(3) C8A 0.032(3) 0.039(4) 0.055(4) 0.003(3) -0.001(3) -0.001(3) C25A 0.036(3) 0.048(4) 0.055(4) 0.006(3) -0.008(3) -0.018(3) C59A 0.042(4) 0.038(4) 0.048(4) 0.000(3) 0.000(3) -0.004(3) C52A 0.037(3) 0.027(3) 0.023(3) 0.000(2) 0.003(2) -0.002(3) C3A 0.045(4) 0.043(4) 0.063(5) 0.005(3) 0.029(4) 0.008(3) C37A 0.045(4) 0.027(3) 0.054(4) 0.009(3) 0.012(3) 0.004(3) C38A 0.047(4) 0.034(4) 0.049(4) -0.018(3) 0.009(3) 0.001(3) C56A 0.026(3) 0.047(4) 0.045(4) -0.002(3) 0.014(3) -0.002(3) C14A 0.052(4) 0.033(4) 0.055(4) 0.018(3) -0.011(4) -0.015(3) C19A 0.072(5) 0.042(4) 0.070(5) 0.032(3) -0.010(4) -0.014(3) C15A 0.056(4) 0.039(4) 0.039(4) -0.004(3) 0.014(3) -0.025(3) C41 0.036(3) 0.039(3) 0.033(3) 0.005(3) 0.011(2) 0.002(3) C50 0.047(4) 0.036(4) 0.038(4) 0.005(3) 0.007(3) 0.002(3) C59 0.045(4) 0.052(4) 0.043(4) 0.004(3) 0.005(3) -0.017(3) C43 0.044(4) 0.043(4) 0.063(5) 0.026(4) 0.016(3) 0.006(3) C46 0.036(3) 0.035(3) 0.023(3) -0.002(2) -0.002(2) -0.002(3) C47 0.044(4) 0.037(3) 0.039(4) 0.001(3) -0.002(3) 0.000(3) C40 0.021(3) 0.043(4) 0.030(3) -0.002(3) 0.005(2) 0.004(3) C57 0.037(4) 0.038(4) 0.036(4) -0.002(3) 0.006(3) -0.002(3) C60 0.041(4) 0.068(5) 0.049(4) 0.006(4) 0.001(3) -0.028(3) B1 0.035(4) 0.033(4) 0.023(3) -0.003(3) 0.001(3) -0.004(3) C53 0.039(4) 0.043(4) 0.033(3) -0.002(3) 0.002(3) 0.005(3) C58 0.035(3) 0.031(3) 0.036(3) 0.011(3) 0.003(3) -0.005(3) C44 0.046(3) 0.065(5) 0.034(3) 0.014(4) 0.012(3) 0.012(3) C62 0.067(5) 0.049(4) 0.045(4) -0.002(3) 0.011(4) -0.002(3) C45 0.049(4) 0.048(4) 0.027(3) 0.006(3) 0.008(3) 0.003(3) C51 0.041(4) 0.030(3) 0.038(3) -0.002(3) 0.005(3) -0.006(3) C52 0.038(3) 0.032(3) 0.036(3) -0.004(3) 0.016(3) 0.007(3) C55 0.033(4) 0.056(5) 0.061(5) -0.017(4) 0.006(3) -0.006(3) C42 0.034(4) 0.036(4) 0.061(4) 0.003(3) 0.011(3) 0.009(3) C54 0.036(4) 0.068(5) 0.044(4) -0.010(4) -0.002(3) 0.004(3) C48 0.027(3) 0.067(5) 0.048(4) 0.008(3) 0.004(3) -0.005(3) C63 0.063(4) 0.038(4) 0.032(4) -0.001(3) 0.004(3) 0.004(3) C56 0.056(4) 0.044(4) 0.051(4) -0.004(3) 0.028(4) -0.006(3) C49 0.046(4) 0.049(4) 0.034(4) 0.002(3) 0.000(3) 0.014(3) C10A 0.038(3) 0.034(3) 0.042(4) 0.000(3) 0.010(3) -0.003(3) C62A 0.081(5) 0.053(5) 0.032(4) -0.004(3) 0.013(4) -0.009(4) C61 0.066(5) 0.053(4) 0.031(4) 0.005(3) 0.002(3) -0.025(4) C11A 0.053(4) 0.040(4) 0.058(4) 0.007(3) 0.004(3) -0.012(3) C17A 0.055(4) 0.030(3) 0.043(4) 0.003(3) 0.009(3) -0.010(3) C61A 0.081(5) 0.058(5) 0.031(4) -0.004(4) -0.003(4) -0.011(4) C21 0.097(6) 0.032(4) 0.059(5) -0.005(3) 0.016(4) -0.011(4) C60A 0.061(5) 0.062(5) 0.043(4) 0.020(4) -0.024(4) -0.014(4) C55A 0.048(4) 0.047(4) 0.052(4) 0.003(3) 0.019(3) 0.014(3) C20A 0.052(4) 0.085(6) 0.082(5) -0.014(4) 0.024(4) -0.030(4) C21A 0.097(6) 0.039(4) 0.061(5) -0.021(3) 0.023(4) 0.002(4) C12A 0.034(4) 0.062(5) 0.087(5) 0.014(4) 0.014(4) -0.007(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 O1 2.049(3) . ? Ru1 N1 2.100(4) . ? Ru1 C18 2.210(6) . ? Ru1 C15 2.211(5) . ? Ru1 C14 2.235(5) . ? Ru1 C16 2.236(5) . ? Ru1 C13 2.251(5) . ? Ru1 C17 2.260(5) . ? Ru1 P1 2.3711(14) . ? P1 C22 1.826(5) . ? P1 C34 1.833(5) . ? P1 C28 1.840(5) . ? C34 C39 1.383(7) . ? C34 C35 1.385(7) . ? O1 C1 1.309(6) . ? N1 C7 1.312(6) . ? N1 C9 1.492(5) . ? O2 C7 1.351(5) . ? O2 C8 1.463(6) . ? C27 C22 1.380(7) . ? C27 C26 1.397(7) . ? C6 C1 1.412(7) . ? C6 C5 1.423(6) . ? C6 C7 1.432(6) . ? C1 C2 1.416(7) . ? C23 C24 1.374(7) . ? C23 C22 1.416(7) . ? C29 C30 1.373(6) . ? C29 C28 1.390(6) . ? C18 C13 1.367(7) . ? C18 C17 1.410(8) . ? C35 C36 1.370(7) . ? C38 C37 1.365(8) . ? C38 C39 1.403(7) . ? C20 C15 1.488(7) . ? C10 C11 1.518(7) . ? C10 C12 1.539(7) . ? C10 C9 1.540(7) . ? C33 C28 1.378(7) . ? C33 C32 1.381(7) . ? C19 C13 1.495(6) . ? C15 C14 1.399(6) . ? C15 C16 1.415(7) . ? C32 C31 1.353(7) . ? C4 C5 1.364(7) . ? C4 C3 1.376(7) . ? C2 C3 1.372(7) . ? C36 C37 1.365(8) . ? C25 C24 1.347(7) . ? C25 C26 1.392(7) . ? C31 C30 1.372(8) . ? C9 C8 1.521(6) . ? C17 C16 1.398(8) . ? C17 C21 1.513(7) . ? C14 C13 1.411(7) . ? Ru2 O1A 2.057(4) . ? Ru2 N1A 2.093(4) . ? Ru2 C15A 2.182(5) . ? Ru2 C13A 2.199(5) . ? Ru2 C14A 2.222(6) . ? Ru2 C16A 2.229(5) . ? Ru2 C18A 2.235(6) . ? Ru2 C17A 2.293(6) . ? Ru2 P1A 2.3774(15) . ? P1A C34A 1.834(5) . ? P1A C28A 1.839(5) . ? P1A C22A 1.841(5) . ? O1A C1A 1.305(6) . ? N1A C7A 1.292(6) . ? N1A C9A 1.491(6) . ? C27A C26A 1.384(7) . ? C27A C22A 1.390(7) . ? C47A C48A 1.380(7) . ? C47A C46A 1.386(7) . ? C18A C17A 1.352(8) . ? C18A C14A 1.413(8) . ? C45A C44A 1.380(7) . ? C45A C40A 1.410(7) . ? C35A C36A 1.365(7) . ? C35A C34A 1.388(6) . ? C34A C39A 1.378(7) . ? C23A C22A 1.374(6) . ? C23A C24A 1.383(6) . ? C28A C33A 1.383(7) . ? C28A C29A 1.392(7) . ? C40A C41A 1.409(6) . ? C40A B1A 1.653(8) . ? C1A C2A 1.401(7) . ? C1A C6A 1.418(7) . ? O2A C7A 1.365(6) . ? O2A C8A 1.455(6) . ? C13A C16A 1.395(7) . ? C13A C15A 1.410(7) . ? C13A C20A 1.501(7) . ? C16A C17A 1.396(8) . ? C54A C55A 1.384(7) . ? C54A C53A 1.388(7) . ? C51A C50A 1.369(7) . ? C51A C46A 1.412(6) . ? C29A C30A 1.381(6) . ? C44A C43A 1.383(7) . ? C6A C5A 1.419(7) . ? C6A C7A 1.443(7) . ? C30A C31A 1.376(7) . ? C41A C42A 1.355(7) . ? C33A C32A 1.376(6) . ? C4A C5A 1.361(7) . ? C4A C3A 1.396(8) . ? C57A C56A 1.384(7) . ? C57A C52A 1.405(6) . ? C43A C42A 1.397(7) . ? C26A C25A 1.368(7) . ? C9A C10A 1.518(7) . ? C9A C8A 1.540(7) . ? C48A C49A 1.374(7) . ? B1A C58A 1.623(8) . ? B1A C52A 1.637(7) . ? B1A C46A 1.669(8) . ? C50A C49A 1.371(7) . ? C31A C32A 1.358(7) . ? C39A C38A 1.383(7) . ? C24A C25A 1.355(7) . ? C53A C52A 1.391(7) . ? C36A C37A 1.367(7) . ? C63A C62A 1.375(7) . ? C63A C58A 1.408(7) . ? C58A C59A 1.408(7) . ? C2A C3A 1.376(7) . ? C59A C60A 1.383(7) . ? C37A C38A 1.372(7) . ? C56A C55A 1.374(7) . ? C14A C15A 1.393(8) . ? C14A C19A 1.529(8) . ? C41 C40 1.396(7) . ? C41 C42 1.399(7) . ? C50 C49 1.360(7) . ? C50 C51 1.372(7) . ? C59 C58 1.401(7) . ? C59 C60 1.405(8) . ? C43 C42 1.353(8) . ? C43 C44 1.381(8) . ? C46 C51 1.396(6) . ? C46 C47 1.408(7) . ? C46 B1 1.634(8) . ? C47 C48 1.382(7) . ? C40 C45 1.403(7) . ? C40 B1 1.638(8) . ? C57 C56 1.390(7) . ? C57 C52 1.394(7) . ? C60 C61 1.381(8) . ? B1 C58 1.630(8) . ? B1 C52 1.641(8) . ? C53 C52 1.385(7) . ? C53 C54 1.402(7) . ? C58 C63 1.383(7) . ? C44 C45 1.359(7) . ? C62 C61 1.370(8) . ? C62 C63 1.392(7) . ? C55 C56 1.352(8) . ? C55 C54 1.352(8) . ? C48 C49 1.396(7) . ? C10A C12A 1.519(7) . ? C10A C11A 1.531(7) . ? C62A C61A 1.349(8) . ? C17A C21A 1.494(7) . ? C61A C60A 1.384(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 N1 83.62(15) . . ? O1 Ru1 C18 159.18(19) . . ? N1 Ru1 C18 97.8(2) . . ? O1 Ru1 C15 87.47(17) . . ? N1 Ru1 C15 139.80(19) . . ? C18 Ru1 C15 78.0(2) . . ? O1 Ru1 C14 110.90(17) . . ? N1 Ru1 C14 162.30(19) . . ? C18 Ru1 C14 64.9(2) . . ? C15 Ru1 C14 36.69(17) . . ? O1 Ru1 C16 93.97(18) . . ? N1 Ru1 C16 104.5(2) . . ? C18 Ru1 C16 65.5(2) . . ? C15 Ru1 C16 37.09(19) . . ? C14 Ru1 C16 65.6(2) . . ? O1 Ru1 C13 147.15(17) . . ? N1 Ru1 C13 129.18(18) . . ? C18 Ru1 C13 35.67(19) . . ? C15 Ru1 C13 66.49(19) . . ? C14 Ru1 C13 36.68(17) . . ? C16 Ru1 C13 77.5(2) . . ? O1 Ru1 C17 123.3(2) . . ? N1 Ru1 C17 86.34(19) . . ? C18 Ru1 C17 36.8(2) . . ? C15 Ru1 C17 66.3(2) . . ? C14 Ru1 C17 77.3(2) . . ? C16 Ru1 C17 36.2(2) . . ? C13 Ru1 C17 65.5(2) . . ? O1 Ru1 P1 83.10(10) . . ? N1 Ru1 P1 99.00(12) . . ? C18 Ru1 P1 116.92(17) . . ? C15 Ru1 P1 118.74(15) . . ? C14 Ru1 P1 92.95(15) . . ? C16 Ru1 P1 155.82(17) . . ? C13 Ru1 P1 91.97(14) . . ? C17 Ru1 P1 153.61(18) . . ? C22 P1 C34 105.2(2) . . ? C22 P1 C28 100.3(2) . . ? C34 P1 C28 103.5(2) . . ? C22 P1 Ru1 118.82(18) . . ? C34 P1 Ru1 117.82(17) . . ? C28 P1 Ru1 108.82(16) . . ? C39 C34 C35 117.6(5) . . ? C39 C34 P1 120.8(4) . . ? C35 C34 P1 121.6(4) . . ? C1 O1 Ru1 120.4(3) . . ? C7 N1 C9 106.9(4) . . ? C7 N1 Ru1 120.3(3) . . ? C9 N1 Ru1 130.1(3) . . ? C7 O2 C8 105.7(4) . . ? C22 C27 C26 119.8(5) . . ? C1 C6 C5 120.3(5) . . ? C1 C6 C7 120.9(5) . . ? C5 C6 C7 118.8(5) . . ? O1 C1 C6 125.0(5) . . ? O1 C1 C2 117.6(5) . . ? C6 C1 C2 117.4(5) . . ? C24 C23 C22 118.4(5) . . ? C30 C29 C28 121.4(5) . . ? C13 C18 C17 123.0(6) . . ? C13 C18 Ru1 73.8(3) . . ? C17 C18 Ru1 73.6(3) . . ? C36 C35 C34 121.7(5) . . ? C37 C38 C39 119.6(5) . . ? C11 C10 C12 111.3(4) . . ? C11 C10 C9 113.1(4) . . ? C12 C10 C9 108.9(4) . . ? N1 C7 O2 115.9(4) . . ? N1 C7 C6 126.4(5) . . ? O2 C7 C6 117.7(4) . . ? C28 C33 C32 120.1(5) . . ? C33 C28 C29 117.7(5) . . ? C33 C28 P1 125.6(4) . . ? C29 C28 P1 116.6(4) . . ? C14 C15 C16 118.8(5) . . ? C14 C15 C20 121.4(5) . . ? C16 C15 C20 119.8(5) . . ? C14 C15 Ru1 72.6(3) . . ? C16 C15 Ru1 72.4(3) . . ? C20 C15 Ru1 127.8(4) . . ? C31 C32 C33 121.7(6) . . ? C27 C22 C23 120.0(5) . . ? C27 C22 P1 118.6(4) . . ? C23 C22 P1 121.4(4) . . ? C5 C4 C3 119.2(5) . . ? C3 C2 C1 120.1(6) . . ? C37 C36 C35 120.2(6) . . ? C24 C25 C26 120.5(5) . . ? C32 C31 C30 119.2(6) . . ? C36 C37 C38 120.2(6) . . ? C34 C39 C38 120.7(5) . . ? C25 C26 C27 119.2(5) . . ? N1 C9 C8 102.1(4) . . ? N1 C9 C10 111.8(4) . . ? C8 C9 C10 114.0(4) . . ? C16 C17 C18 117.8(6) . . ? C16 C17 C21 120.5(6) . . ? C18 C17 C21 121.7(6) . . ? C16 C17 Ru1 71.0(3) . . ? C18 C17 Ru1 69.7(3) . . ? C21 C17 Ru1 130.2(4) . . ? C31 C30 C29 119.9(5) . . ? C2 C3 C4 122.6(6) . . ? C15 C14 C13 121.0(5) . . ? C15 C14 Ru1 70.7(3) . . ? C13 C14 Ru1 72.3(3) . . ? O2 C8 C9 103.7(4) . . ? C18 C13 C14 118.4(5) . . ? C18 C13 C19 121.7(5) . . ? C14 C13 C19 119.6(5) . . ? C18 C13 Ru1 70.5(3) . . ? C14 C13 Ru1 71.0(3) . . ? C19 C13 Ru1 135.5(4) . . ? C25 C24 C23 122.0(5) . . ? C17 C16 C15 120.9(5) . . ? C17 C16 Ru1 72.8(3) . . ? C15 C16 Ru1 70.5(3) . . ? C4 C5 C6 120.3(5) . . ? O1A Ru2 N1A 84.46(15) . . ? O1A Ru2 C15A 94.97(19) . . ? N1A Ru2 C15A 101.57(19) . . ? O1A Ru2 C13A 85.39(18) . . ? N1A Ru2 C13A 136.38(19) . . ? C15A Ru2 C13A 37.54(19) . . ? O1A Ru2 C14A 127.2(2) . . ? N1A Ru2 C14A 86.70(19) . . ? C15A Ru2 C14A 36.9(2) . . ? C13A Ru2 C14A 66.7(2) . . ? O1A Ru2 C16A 106.94(19) . . ? N1A Ru2 C16A 163.36(18) . . ? C15A Ru2 C16A 66.0(2) . . ? C13A Ru2 C16A 36.72(19) . . ? C14A Ru2 C16A 76.8(2) . . ? O1A Ru2 C18A 160.96(18) . . ? N1A Ru2 C18A 101.8(2) . . ? C15A Ru2 C18A 66.3(2) . . ? C13A Ru2 C18A 77.7(2) . . ? C14A Ru2 C18A 37.0(2) . . ? C16A Ru2 C18A 63.6(2) . . ? O1A Ru2 C17A 141.97(19) . . ? N1A Ru2 C17A 133.5(2) . . ? C15A Ru2 C17A 77.9(2) . . ? C13A Ru2 C17A 66.1(2) . . ? C14A Ru2 C17A 65.0(2) . . ? C16A Ru2 C17A 35.94(19) . . ? C18A Ru2 C17A 34.7(2) . . ? O1A Ru2 P1A 80.78(10) . . ? N1A Ru2 P1A 96.84(12) . . ? C15A Ru2 P1A 160.62(16) . . ? C13A Ru2 P1A 123.08(16) . . ? C14A Ru2 P1A 152.0(2) . . ? C16A Ru2 P1A 96.95(14) . . ? C18A Ru2 P1A 115.79(17) . . ? C17A Ru2 P1A 93.80(15) . . ? C34A P1A C28A 102.8(2) . . ? C34A P1A C22A 101.6(2) . . ? C28A P1A C22A 104.6(2) . . ? C34A P1A Ru2 119.39(17) . . ? C28A P1A Ru2 119.03(17) . . ? C22A P1A Ru2 107.28(16) . . ? C1A O1A Ru2 124.2(3) . . ? C7A N1A C9A 109.2(4) . . ? C7A N1A Ru2 120.5(4) . . ? C9A N1A Ru2 127.2(3) . . ? C26A C27A C22A 120.4(5) . . ? C48A C47A C46A 122.7(5) . . ? C17A C18A C14A 122.6(6) . . ? C17A C18A Ru2 75.0(4) . . ? C14A C18A Ru2 71.0(3) . . ? C44A C45A C40A 123.2(5) . . ? C36A C35A C34A 121.5(5) . . ? C39A C34A C35A 117.9(5) . . ? C39A C34A P1A 120.9(4) . . ? C35A C34A P1A 121.1(4) . . ? C22A C23A C24A 120.0(5) . . ? C33A C28A C29A 118.6(5) . . ? C33A C28A P1A 122.5(4) . . ? C29A C28A P1A 118.9(4) . . ? C41A C40A C45A 113.7(5) . . ? C41A C40A B1A 123.7(5) . . ? C45A C40A B1A 122.6(5) . . ? O1A C1A C2A 117.6(5) . . ? O1A C1A C6A 125.5(5) . . ? C2A C1A C6A 116.9(5) . . ? C7A O2A C8A 106.3(4) . . ? C23A C22A C27A 118.9(5) . . ? C23A C22A P1A 123.5(4) . . ? C27A C22A P1A 117.5(4) . . ? C16A C13A C15A 118.0(6) . . ? C16A C13A C20A 121.3(6) . . ? C15A C13A C20A 120.8(6) . . ? C16A C13A Ru2 72.8(3) . . ? C15A C13A Ru2 70.6(3) . . ? C20A C13A Ru2 126.5(4) . . ? C13A C16A C17A 122.8(6) . . ? C13A C16A Ru2 70.5(3) . . ? C17A C16A Ru2 74.5(3) . . ? C55A C54A C53A 119.5(5) . . ? C50A C51A C46A 122.3(5) . . ? C30A C29A C28A 120.4(5) . . ? C45A C44A C43A 120.1(5) . . ? C1A C6A C5A 120.7(5) . . ? C1A C6A C7A 119.7(5) . . ? C5A C6A C7A 119.4(5) . . ? C31A C30A C29A 119.6(5) . . ? C42A C41A C40A 124.5(5) . . ? C32A C33A C28A 120.4(5) . . ? C5A C4A C3A 118.8(5) . . ? C56A C57A C52A 123.5(5) . . ? C44A C43A C42A 118.8(5) . . ? C25A C26A C27A 119.7(5) . . ? N1A C9A C10A 112.8(4) . . ? N1A C9A C8A 100.8(4) . . ? C10A C9A C8A 113.7(4) . . ? C49A C48A C47A 120.0(5) . . ? C4A C5A C6A 120.6(6) . . ? C58A B1A C52A 107.9(4) . . ? C58A B1A C40A 108.1(4) . . ? C52A B1A C40A 112.2(4) . . ? C58A B1A C46A 111.2(4) . . ? C52A B1A C46A 107.5(4) . . ? C40A B1A C46A 110.0(4) . . ? C51A C50A C49A 120.3(5) . . ? N1A C7A O2A 114.9(5) . . ? N1A C7A C6A 128.5(5) . . ? O2A C7A C6A 116.5(5) . . ? C32A C31A C30A 120.4(5) . . ? C34A C39A C38A 120.8(5) . . ? C25A C24A C23A 120.8(5) . . ? C31A C32A C33A 120.5(5) . . ? C47A C46A C51A 115.3(5) . . ? C47A C46A B1A 122.9(5) . . ? C51A C46A B1A 121.6(5) . . ? C54A C53A C52A 123.3(5) . . ? C35A C36A C37A 119.8(5) . . ? C41A C42A C43A 119.7(5) . . ? C62A C63A C58A 124.1(6) . . ? C59A C58A C63A 111.7(5) . . ? C59A C58A B1A 124.3(5) . . ? C63A C58A B1A 123.6(5) . . ? C50A C49A C48A 119.4(5) . . ? C3A C2A C1A 121.2(6) . . ? O2A C8A C9A 104.4(4) . . ? C24A C25A C26A 120.2(5) . . ? C60A C59A C58A 124.6(6) . . ? C53A C52A C57A 114.6(5) . . ? C53A C52A B1A 122.4(5) . . ? C57A C52A B1A 122.7(5) . . ? C2A C3A C4A 121.8(5) . . ? C36A C37A C38A 120.2(6) . . ? C37A C38A C39A 119.8(5) . . ? C55A C56A C57A 119.3(5) . . ? C15A C14A C18A 118.7(6) . . ? C15A C14A C19A 119.8(6) . . ? C18A C14A C19A 121.5(6) . . ? C15A C14A Ru2 70.0(3) . . ? C18A C14A Ru2 72.0(3) . . ? C19A C14A Ru2 129.4(4) . . ? C14A C15A C13A 120.2(6) . . ? C14A C15A Ru2 73.1(3) . . ? C13A C15A Ru2 71.9(3) . . ? C40 C41 C42 123.0(5) . . ? C49 C50 C51 122.3(6) . . ? C58 C59 C60 121.6(6) . . ? C42 C43 C44 119.2(6) . . ? C51 C46 C47 113.5(5) . . ? C51 C46 B1 124.8(5) . . ? C47 C46 B1 121.7(5) . . ? C48 C47 C46 123.5(6) . . ? C41 C40 C45 114.1(5) . . ? C41 C40 B1 125.1(5) . . ? C45 C40 B1 120.5(5) . . ? C56 C57 C52 123.5(6) . . ? C61 C60 C59 120.5(6) . . ? C58 B1 C46 110.7(5) . . ? C58 B1 C40 109.7(4) . . ? C46 B1 C40 105.6(4) . . ? C58 B1 C52 107.4(4) . . ? C46 B1 C52 110.8(4) . . ? C40 B1 C52 112.7(4) . . ? C52 C53 C54 122.1(6) . . ? C63 C58 C59 115.4(5) . . ? C63 C58 B1 120.5(5) . . ? C59 C58 B1 124.1(5) . . ? C45 C44 C43 120.5(5) . . ? C61 C62 C63 119.6(6) . . ? C44 C45 C40 123.4(6) . . ? C50 C51 C46 123.2(5) . . ? C53 C52 C57 114.1(5) . . ? C53 C52 B1 126.2(5) . . ? C57 C52 B1 119.7(5) . . ? C56 C55 C54 118.6(6) . . ? C43 C42 C41 119.9(6) . . ? C55 C54 C53 121.3(6) . . ? C47 C48 C49 120.2(6) . . ? C58 C63 C62 123.8(6) . . ? C55 C56 C57 120.3(6) . . ? C50 C49 C48 117.2(6) . . ? C9A C10A C12A 109.0(4) . . ? C9A C10A C11A 114.5(5) . . ? C12A C10A C11A 111.5(5) . . ? C61A C62A C63A 121.7(7) . . ? C62 C61 C60 119.1(6) . . ? C18A C17A C16A 117.7(6) . . ? C18A C17A C21A 120.5(6) . . ? C16A C17A C21A 121.5(6) . . ? C18A C17A Ru2 70.3(3) . . ? C16A C17A Ru2 69.5(3) . . ? C21A C17A Ru2 136.7(4) . . ? C62A C61A C60A 117.9(6) . . ? C61A C60A C59A 119.8(6) . . ? C56A C55A C54A 119.8(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.891 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.063