# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'B. Wang' _publ_contact_author_email BQWANG@NANKAI.EDU.CN _publ_section_title ; The Intramolecular sp2 and sp3 C-H Bond Activation of (p-Cymene)Ruthenium(II) N-Heterocyclic Carbene Complexes ; loop_ _publ_author_name 'B. Wang' 'Bin Li.' 'Hai-Bin Song.' 'Shansheng Xu.' 'Congying Zhang.' ; Yang Zhao ; #===END data_071221a _database_code_depnum_ccdc_archive 'CCDC 675611' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H27 I N2 Ru' _chemical_formula_weight 499.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.331(2) _cell_length_b 8.5497(15) _cell_length_c 17.376(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.401(3) _cell_angle_gamma 90.00 _cell_volume 1934.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5256 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 26.39 _exptl_crystal_description block _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 2.406 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.689154 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 10851 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.40 _reflns_number_total 3944 _reflns_number_gt 3293 _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^)+(0.0321P)^2^+0.7520P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0069(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3944 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0599 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.294327(17) 0.48200(3) 0.226293(13) 0.02487(8) Uani 1 1 d . . . I1 I 0.16385(2) 0.29160(3) 0.123720(14) 0.05633(11) Uani 1 1 d . . . N1 N 0.10682(18) 0.5494(3) 0.30444(15) 0.0321(5) Uani 1 1 d . . . N2 N 0.20198(18) 0.3569(3) 0.35336(14) 0.0304(5) Uani 1 1 d . . . C1 C 0.5106(3) 0.5897(5) 0.3558(2) 0.0580(10) Uani 1 1 d . . . H1A H 0.5675 0.6594 0.3578 0.087 Uiso 1 1 calc R . . H1B H 0.5352 0.4839 0.3621 0.087 Uiso 1 1 calc R . . H1C H 0.4764 0.6150 0.3975 0.087 Uiso 1 1 calc R . . C2 C 0.4363(2) 0.6065(4) 0.27748(18) 0.0364(7) Uani 1 1 d . . . C3 C 0.3519(3) 0.7093(3) 0.26686(19) 0.0362(7) Uani 1 1 d . . . H3 H 0.3365 0.7580 0.3108 0.043 Uiso 1 1 calc R . . C4 C 0.2895(2) 0.7411(3) 0.19138(19) 0.0353(7) Uani 1 1 d . . . H4 H 0.2391 0.8180 0.1856 0.042 Uiso 1 1 calc R . . C5 C 0.3040(2) 0.6568(4) 0.12580(18) 0.0341(7) Uani 1 1 d . . . C6 C 0.3864(2) 0.5473(4) 0.13664(18) 0.0350(7) Uani 1 1 d . . . H6 H 0.3966 0.4893 0.0937 0.042 Uiso 1 1 calc R . . C7 C 0.4521(2) 0.5245(4) 0.20960(19) 0.0356(7) Uani 1 1 d . . . H7 H 0.5068 0.4551 0.2141 0.043 Uiso 1 1 calc R . . C8 C 0.2384(3) 0.6812(4) 0.0437(2) 0.0484(9) Uani 1 1 d . . . H8 H 0.2302 0.5790 0.0175 0.058 Uiso 1 1 calc R . . C9 C 0.1316(3) 0.7446(7) 0.0420(3) 0.0843(15) Uani 1 1 d . . . H9A H 0.0979 0.6791 0.0735 0.126 Uiso 1 1 calc R . . H9B H 0.0926 0.7457 -0.0113 0.126 Uiso 1 1 calc R . . H9C H 0.1368 0.8491 0.0627 0.126 Uiso 1 1 calc R . . C10 C 0.2960(4) 0.7867(6) -0.0032(2) 0.0741(13) Uani 1 1 d . . . H10A H 0.3062 0.8877 0.0213 0.111 Uiso 1 1 calc R . . H10B H 0.2565 0.7976 -0.0561 0.111 Uiso 1 1 calc R . . H10C H 0.3614 0.7409 -0.0044 0.111 Uiso 1 1 calc R . . C11 C 0.1923(2) 0.4687(3) 0.29706(17) 0.0268(6) Uani 1 1 d . . . C12 C 0.0648(2) 0.4865(4) 0.36424(19) 0.0380(7) Uani 1 1 d . . . H12 H 0.0061 0.5211 0.3799 0.046 Uiso 1 1 calc R . . C13 C 0.1243(2) 0.3673(4) 0.39478(18) 0.0369(7) Uani 1 1 d . . . H13 H 0.1155 0.3033 0.4361 0.044 Uiso 1 1 calc R . . C14 C 0.0611(3) 0.6789(5) 0.2547(2) 0.0564(10) Uani 1 1 d . . . H14A H 0.1065 0.7672 0.2637 0.085 Uiso 1 1 calc R . . H14B H -0.0033 0.7065 0.2673 0.085 Uiso 1 1 calc R . . H14C H 0.0499 0.6482 0.2004 0.085 Uiso 1 1 calc R . . C15 C 0.2865(2) 0.2427(4) 0.36151(19) 0.0365(7) Uani 1 1 d . . . C16 C 0.3436(3) 0.2785(3) 0.2952(2) 0.0370(7) Uani 1 1 d . . . H16A H 0.3362 0.1890 0.2601 0.044 Uiso 1 1 calc R . . H16B H 0.4161 0.2897 0.3186 0.044 Uiso 1 1 calc R . . C17 C 0.3556(3) 0.2637(6) 0.4436(2) 0.0651(12) Uani 1 1 d . . . H17A H 0.3820 0.3685 0.4489 0.098 Uiso 1 1 calc R . . H17B H 0.4116 0.1909 0.4503 0.098 Uiso 1 1 calc R . . H17C H 0.3164 0.2448 0.4830 0.098 Uiso 1 1 calc R . . C18 C 0.2389(3) 0.0790(4) 0.3522(3) 0.0660(12) Uani 1 1 d . . . H18A H 0.1982 0.0638 0.3909 0.099 Uiso 1 1 calc R . . H18B H 0.2925 0.0020 0.3593 0.099 Uiso 1 1 calc R . . H18C H 0.1961 0.0686 0.3004 0.099 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 0.02359(13) 0.02668(13) 0.02561(13) -0.00148(9) 0.00813(9) -0.00022(9) I1 0.06059(18) 0.0712(2) 0.03931(15) -0.01538(11) 0.01537(11) -0.03810(13) N1 0.0271(13) 0.0374(14) 0.0338(13) 0.0019(11) 0.0111(10) 0.0062(11) N2 0.0324(13) 0.0304(13) 0.0305(13) 0.0022(10) 0.0113(10) 0.0034(11) C1 0.046(2) 0.071(3) 0.050(2) 0.0023(19) -0.0058(18) -0.0132(19) C2 0.0309(16) 0.0396(18) 0.0373(17) 0.0012(13) 0.0047(13) -0.0094(14) C3 0.0459(19) 0.0297(16) 0.0356(17) -0.0090(13) 0.0144(14) -0.0096(14) C4 0.0363(17) 0.0278(15) 0.0439(18) 0.0022(13) 0.0129(14) 0.0008(13) C5 0.0344(16) 0.0348(17) 0.0336(16) 0.0046(13) 0.0087(13) -0.0056(13) C6 0.0353(17) 0.0404(18) 0.0345(16) -0.0045(14) 0.0190(13) -0.0089(14) C7 0.0243(15) 0.0386(17) 0.0462(19) 0.0010(14) 0.0126(13) -0.0030(13) C8 0.050(2) 0.057(2) 0.0360(19) 0.0094(16) 0.0055(16) -0.0079(17) C9 0.051(3) 0.139(5) 0.058(3) 0.034(3) 0.002(2) 0.012(3) C10 0.076(3) 0.099(4) 0.047(2) 0.031(2) 0.014(2) -0.008(3) C11 0.0260(15) 0.0268(14) 0.0272(14) -0.0015(11) 0.0049(11) 0.0003(11) C12 0.0345(17) 0.0452(19) 0.0397(18) -0.0028(14) 0.0199(14) -0.0006(14) C13 0.0426(18) 0.0408(18) 0.0317(16) 0.0019(13) 0.0179(14) 0.0000(15) C14 0.044(2) 0.063(2) 0.069(3) 0.026(2) 0.0269(19) 0.0261(18) C15 0.0387(18) 0.0321(16) 0.0407(18) 0.0087(13) 0.0133(14) 0.0102(14) C16 0.0391(18) 0.0324(17) 0.0436(18) 0.0030(13) 0.0180(14) 0.0106(13) C17 0.055(3) 0.093(3) 0.044(2) 0.011(2) 0.0032(19) 0.025(2) C18 0.088(3) 0.0283(18) 0.095(3) 0.0061(19) 0.049(3) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C11 2.023(3) . ? Ru1 C16 2.134(3) . ? Ru1 C3 2.152(3) . ? Ru1 C2 2.187(3) . ? Ru1 C7 2.214(3) . ? Ru1 C6 2.251(3) . ? Ru1 C4 2.294(3) . ? Ru1 C5 2.323(3) . ? Ru1 I1 2.7423(4) . ? N1 C11 1.362(4) . ? N1 C12 1.390(4) . ? N1 C14 1.455(4) . ? N2 C11 1.354(4) . ? N2 C13 1.385(4) . ? N2 C15 1.475(4) . ? C1 C2 1.508(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.409(4) . ? C2 C7 1.426(4) . ? C3 C4 1.420(4) . ? C3 H3 0.9300 . ? C4 C5 1.396(4) . ? C4 H4 0.9300 . ? C5 C6 1.425(4) . ? C5 C8 1.519(4) . ? C6 C7 1.391(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.518(6) . ? C8 C10 1.528(5) . ? C8 H8 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C12 C13 1.330(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C18 1.531(5) . ? C15 C17 1.533(5) . ? C15 C16 1.542(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? 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 C11 Ru1 C16 77.24(11) . . ? C11 Ru1 C3 95.21(12) . . ? C16 Ru1 C3 120.51(13) . . ? C11 Ru1 C2 114.61(12) . . ? C16 Ru1 C2 91.93(12) . . ? C3 Ru1 C2 37.89(12) . . ? C11 Ru1 C7 150.51(12) . . ? C16 Ru1 C7 91.19(12) . . ? C3 Ru1 C7 67.23(12) . . ? C2 Ru1 C7 37.80(12) . . ? C11 Ru1 C6 166.49(11) . . ? C16 Ru1 C6 116.27(12) . . ? C3 Ru1 C6 78.10(12) . . ? C2 Ru1 C6 66.90(12) . . ? C7 Ru1 C6 36.30(11) . . ? C11 Ru1 C4 103.35(11) . . ? C16 Ru1 C4 157.44(12) . . ? C3 Ru1 C4 37.08(12) . . ? C2 Ru1 C4 67.06(11) . . ? C7 Ru1 C4 77.31(11) . . ? C6 Ru1 C4 64.28(11) . . ? C11 Ru1 C5 130.26(11) . . ? C16 Ru1 C5 152.39(12) . . ? C3 Ru1 C5 65.91(11) . . ? C2 Ru1 C5 79.03(11) . . ? C7 Ru1 C5 65.69(11) . . ? C6 Ru1 C5 36.26(11) . . ? C4 Ru1 C5 35.20(11) . . ? C11 Ru1 I1 86.92(8) . . ? C16 Ru1 I1 87.49(10) . . ? C3 Ru1 I1 151.74(9) . . ? C2 Ru1 I1 157.79(9) . . ? C7 Ru1 I1 120.00(8) . . ? C6 Ru1 I1 93.52(8) . . ? C4 Ru1 I1 115.06(8) . . ? C5 Ru1 I1 91.33(8) . . ? C11 N1 C12 110.7(2) . . ? C11 N1 C14 125.6(3) . . ? C12 N1 C14 123.6(3) . . ? C11 N2 C13 111.4(2) . . ? C11 N2 C15 119.3(2) . . ? C13 N2 C15 129.3(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 117.0(3) . . ? C3 C2 C1 121.9(3) . . ? C7 C2 C1 121.0(3) . . ? C3 C2 Ru1 69.69(17) . . ? C7 C2 Ru1 72.10(17) . . ? C1 C2 Ru1 131.6(2) . . ? C2 C3 C4 122.2(3) . . ? C2 C3 Ru1 72.42(17) . . ? C4 C3 Ru1 76.91(17) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? Ru1 C3 H3 123.2 . . ? C5 C4 C3 119.9(3) . . ? C5 C4 Ru1 73.52(18) . . ? C3 C4 Ru1 66.01(16) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? Ru1 C4 H4 133.6 . . ? C4 C5 C6 118.0(3) . . ? C4 C5 C8 122.9(3) . . ? C6 C5 C8 119.1(3) . . ? C4 C5 Ru1 71.27(17) . . ? C6 C5 Ru1 69.12(17) . . ? C8 C5 Ru1 132.9(2) . . ? C7 C6 C5 121.9(3) . . ? C7 C6 Ru1 70.40(17) . . ? C5 C6 Ru1 74.62(17) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? Ru1 C6 H6 128.2 . . ? C6 C7 C2 120.6(3) . . ? C6 C7 Ru1 73.31(17) . . ? C2 C7 Ru1 70.09(17) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? Ru1 C7 H7 129.3 . . ? C9 C8 C5 114.6(3) . . ? C9 C8 C10 110.8(3) . . ? C5 C8 C10 109.2(3) . . ? C9 C8 H8 107.3 . . ? C5 C8 H8 107.3 . . ? C10 C8 H8 107.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 N1 104.0(2) . . ? N2 C11 Ru1 120.5(2) . . ? N1 C11 Ru1 135.6(2) . . ? C13 C12 N1 107.0(3) . . ? C13 C12 H12 126.5 . . ? N1 C12 H12 126.5 . . ? C12 C13 N2 106.9(3) . . ? C12 C13 H13 126.5 . . ? N2 C13 H13 126.5 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C18 107.7(3) . . ? N2 C15 C17 107.8(3) . . ? C18 C15 C17 111.0(3) . . ? N2 C15 C16 106.6(2) . . ? C18 C15 C16 111.2(3) . . ? C17 C15 C16 112.2(3) . . ? C15 C16 Ru1 116.1(2) . . ? C15 C16 H16A 108.3 . . ? Ru1 C16 H16A 108.3 . . ? C15 C16 H16B 108.3 . . ? Ru1 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Ru1 C2 C3 -64.8(2) . . . . ? C16 Ru1 C2 C3 -141.62(19) . . . . ? C7 Ru1 C2 C3 128.9(3) . . . . ? C6 Ru1 C2 C3 100.5(2) . . . . ? C4 Ru1 C2 C3 29.92(18) . . . . ? C5 Ru1 C2 C3 64.66(19) . . . . ? I1 Ru1 C2 C3 130.3(2) . . . . ? C11 Ru1 C2 C7 166.30(18) . . . . ? C16 Ru1 C2 C7 89.46(19) . . . . ? C3 Ru1 C2 C7 -128.9(3) . . . . ? C6 Ru1 C2 C7 -28.38(18) . . . . ? C4 Ru1 C2 C7 -99.0(2) . . . . ? C5 Ru1 C2 C7 -64.26(19) . . . . ? I1 Ru1 C2 C7 1.4(3) . . . . ? C11 Ru1 C2 C1 50.4(4) . . . . ? C16 Ru1 C2 C1 -26.5(3) . . . . ? C3 Ru1 C2 C1 115.1(4) . . . . ? C7 Ru1 C2 C1 -115.9(4) . . . . ? C6 Ru1 C2 C1 -144.3(4) . . . . ? C4 Ru1 C2 C1 145.1(4) . . . . ? C5 Ru1 C2 C1 179.8(4) . . . . ? I1 Ru1 C2 C1 -114.5(3) . . . . ? C7 C2 C3 C4 -5.1(4) . . . . ? C1 C2 C3 C4 171.6(3) . . . . ? Ru1 C2 C3 C4 -61.3(3) . . . . ? C7 C2 C3 Ru1 56.2(2) . . . . ? C1 C2 C3 Ru1 -127.1(3) . . . . ? C11 Ru1 C3 C2 124.32(19) . . . . ? C16 Ru1 C3 C2 46.1(2) . . . . ? C7 Ru1 C3 C2 -31.15(18) . . . . ? C6 Ru1 C3 C2 -67.55(19) . . . . ? C4 Ru1 C3 C2 -130.4(3) . . . . ? C5 Ru1 C3 C2 -103.6(2) . . . . ? I1 Ru1 C3 C2 -142.50(17) . . . . ? C11 Ru1 C3 C4 -105.31(19) . . . . ? C16 Ru1 C3 C4 176.45(17) . . . . ? C2 Ru1 C3 C4 130.4(3) . . . . ? C7 Ru1 C3 C4 99.2(2) . . . . ? C6 Ru1 C3 C4 62.82(19) . . . . ? C5 Ru1 C3 C4 26.77(18) . . . . ? I1 Ru1 C3 C4 -12.1(3) . . . . ? C2 C3 C4 C5 7.0(5) . . . . ? Ru1 C3 C4 C5 -52.1(3) . . . . ? C2 C3 C4 Ru1 59.1(3) . . . . ? C11 Ru1 C4 C5 -144.66(18) . . . . ? C16 Ru1 C4 C5 126.5(3) . . . . ? C3 Ru1 C4 C5 134.5(3) . . . . ? C2 Ru1 C4 C5 104.0(2) . . . . ? C7 Ru1 C4 C5 65.62(19) . . . . ? C6 Ru1 C4 C5 29.57(18) . . . . ? I1 Ru1 C4 C5 -51.80(19) . . . . ? C11 Ru1 C4 C3 80.8(2) . . . . ? C16 Ru1 C4 C3 -8.0(4) . . . . ? C2 Ru1 C4 C3 -30.53(19) . . . . ? C7 Ru1 C4 C3 -68.9(2) . . . . ? C6 Ru1 C4 C3 -104.9(2) . . . . ? C5 Ru1 C4 C3 -134.5(3) . . . . ? I1 Ru1 C4 C3 173.69(16) . . . . ? C3 C4 C5 C6 -3.9(4) . . . . ? Ru1 C4 C5 C6 -52.7(2) . . . . ? C3 C4 C5 C8 178.3(3) . . . . ? Ru1 C4 C5 C8 129.5(3) . . . . ? C3 C4 C5 Ru1 48.7(3) . . . . ? C11 Ru1 C5 C4 47.5(2) . . . . ? C16 Ru1 C5 C4 -138.3(3) . . . . ? C3 Ru1 C5 C4 -28.10(19) . . . . ? C2 Ru1 C5 C4 -65.55(19) . . . . ? C7 Ru1 C5 C4 -102.8(2) . . . . ? C6 Ru1 C5 C4 -131.3(3) . . . . ? I1 Ru1 C5 C4 134.60(18) . . . . ? C11 Ru1 C5 C6 178.77(17) . . . . ? C16 Ru1 C5 C6 -7.0(3) . . . . ? C3 Ru1 C5 C6 103.2(2) . . . . ? C2 Ru1 C5 C6 65.71(18) . . . . ? C7 Ru1 C5 C6 28.42(18) . . . . ? C4 Ru1 C5 C6 131.3(3) . . . . ? I1 Ru1 C5 C6 -94.14(17) . . . . ? C11 Ru1 C5 C8 -70.4(4) . . . . ? C16 Ru1 C5 C8 103.8(4) . . . . ? C3 Ru1 C5 C8 -146.0(4) . . . . ? C2 Ru1 C5 C8 176.6(3) . . . . ? C7 Ru1 C5 C8 139.3(4) . . . . ? C6 Ru1 C5 C8 110.8(4) . . . . ? C4 Ru1 C5 C8 -117.9(4) . . . . ? I1 Ru1 C5 C8 16.7(3) . . . . ? C4 C5 C6 C7 -0.7(4) . . . . ? C8 C5 C6 C7 177.1(3) . . . . ? Ru1 C5 C6 C7 -54.4(3) . . . . ? C4 C5 C6 Ru1 53.7(2) . . . . ? C8 C5 C6 Ru1 -128.4(3) . . . . ? C11 Ru1 C6 C7 128.9(4) . . . . ? C16 Ru1 C6 C7 -50.7(2) . . . . ? C3 Ru1 C6 C7 67.6(2) . . . . ? C2 Ru1 C6 C7 29.49(18) . . . . ? C4 Ru1 C6 C7 104.1(2) . . . . ? C5 Ru1 C6 C7 132.9(3) . . . . ? I1 Ru1 C6 C7 -139.68(18) . . . . ? C11 Ru1 C6 C5 -4.0(5) . . . . ? C16 Ru1 C6 C5 176.38(18) . . . . ? C3 Ru1 C6 C5 -65.29(18) . . . . ? C2 Ru1 C6 C5 -103.4(2) . . . . ? C7 Ru1 C6 C5 -132.9(3) . . . . ? C4 Ru1 C6 C5 -28.75(17) . . . . ? I1 Ru1 C6 C5 87.44(17) . . . . ? C5 C6 C7 C2 2.6(5) . . . . ? Ru1 C6 C7 C2 -53.8(3) . . . . ? C5 C6 C7 Ru1 56.4(3) . . . . ? C3 C2 C7 C6 0.3(4) . . . . ? C1 C2 C7 C6 -176.4(3) . . . . ? Ru1 C2 C7 C6 55.3(3) . . . . ? C3 C2 C7 Ru1 -55.0(2) . . . . ? C1 C2 C7 Ru1 128.3(3) . . . . ? C11 Ru1 C7 C6 -158.3(2) . . . . ? C16 Ru1 C7 C6 136.0(2) . . . . ? C3 Ru1 C7 C6 -101.2(2) . . . . ? C2 Ru1 C7 C6 -132.4(3) . . . . ? C4 Ru1 C7 C6 -63.57(19) . . . . ? C5 Ru1 C7 C6 -28.40(18) . . . . ? I1 Ru1 C7 C6 48.2(2) . . . . ? C11 Ru1 C7 C2 -25.9(3) . . . . ? C16 Ru1 C7 C2 -91.61(19) . . . . ? C3 Ru1 C7 C2 31.21(18) . . . . ? C6 Ru1 C7 C2 132.4(3) . . . . ? C4 Ru1 C7 C2 68.81(19) . . . . ? C5 Ru1 C7 C2 104.0(2) . . . . ? I1 Ru1 C7 C2 -179.39(15) . . . . ? C4 C5 C8 C9 -25.8(5) . . . . ? C6 C5 C8 C9 156.5(4) . . . . ? Ru1 C5 C8 C9 68.7(5) . . . . ? C4 C5 C8 C10 99.1(4) . . . . ? C6 C5 C8 C10 -78.6(4) . . . . ? Ru1 C5 C8 C10 -166.4(3) . . . . ? C13 N2 C11 N1 0.1(3) . . . . ? C15 N2 C11 N1 178.4(2) . . . . ? C13 N2 C11 Ru1 -179.6(2) . . . . ? C15 N2 C11 Ru1 -1.3(4) . . . . ? C12 N1 C11 N2 -0.4(3) . . . . ? C14 N1 C11 N2 -177.4(3) . . . . ? C12 N1 C11 Ru1 179.3(2) . . . . ? C14 N1 C11 Ru1 2.2(5) . . . . ? C16 Ru1 C11 N2 3.7(2) . . . . ? C3 Ru1 C11 N2 -116.5(2) . . . . ? C2 Ru1 C11 N2 -82.6(2) . . . . ? C7 Ru1 C11 N2 -65.4(3) . . . . ? C6 Ru1 C11 N2 -176.0(4) . . . . ? C4 Ru1 C11 N2 -153.2(2) . . . . ? C5 Ru1 C11 N2 -179.09(19) . . . . ? I1 Ru1 C11 N2 91.8(2) . . . . ? C16 Ru1 C11 N1 -176.0(3) . . . . ? C3 Ru1 C11 N1 63.9(3) . . . . ? C2 Ru1 C11 N1 97.8(3) . . . . ? C7 Ru1 C11 N1 115.0(3) . . . . ? C6 Ru1 C11 N1 4.4(7) . . . . ? C4 Ru1 C11 N1 27.2(3) . . . . ? C5 Ru1 C11 N1 1.3(4) . . . . ? I1 Ru1 C11 N1 -87.8(3) . . . . ? C11 N1 C12 C13 0.5(4) . . . . ? C14 N1 C12 C13 177.6(3) . . . . ? N1 C12 C13 N2 -0.4(4) . . . . ? C11 N2 C13 C12 0.2(4) . . . . ? C15 N2 C13 C12 -177.9(3) . . . . ? C11 N2 C15 C18 -122.5(3) . . . . ? C13 N2 C15 C18 55.4(4) . . . . ? C11 N2 C15 C17 117.6(3) . . . . ? C13 N2 C15 C17 -64.4(4) . . . . ? C11 N2 C15 C16 -3.1(4) . . . . ? C13 N2 C15 C16 174.9(3) . . . . ? N2 C15 C16 Ru1 5.9(3) . . . . ? C18 C15 C16 Ru1 123.0(3) . . . . ? C17 C15 C16 Ru1 -112.0(3) . . . . ? C11 Ru1 C16 C15 -5.3(2) . . . . ? C3 Ru1 C16 C15 83.3(3) . . . . ? C2 Ru1 C16 C15 109.6(3) . . . . ? C7 Ru1 C16 C15 147.4(3) . . . . ? C6 Ru1 C16 C15 174.7(2) . . . . ? C4 Ru1 C16 C15 88.9(4) . . . . ? C5 Ru1 C16 C15 179.3(2) . . . . ? I1 Ru1 C16 C15 -92.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.127 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.093 #===END data_R071206c _database_code_depnum_ccdc_archive 'CCDC 675612' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 Cl2 I2 N2 Ru' _chemical_formula_sum 'C24 H32 Cl2 I2 N2 Ru' _chemical_formula_weight 774.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8274(17) _cell_length_b 11.8707(18) _cell_length_c 14.782(3) _cell_angle_alpha 67.695(8) _cell_angle_beta 83.695(10) _cell_angle_gamma 70.037(7) _cell_volume 1346.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 4049 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour black-red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 3.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6064 _exptl_absorpt_correction_T_max 0.6379 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12738 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4754 _reflns_number_gt 4181 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0246P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4754 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0551 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.79471(3) 0.46548(2) 0.304171(17) 0.01138(7) Uani 1 1 d . . . I1 I 0.46887(2) 0.50859(2) 0.298389(15) 0.01744(7) Uani 1 1 d . . . I2 I 0.83109(3) 0.29377(2) 0.214957(15) 0.01979(7) Uani 1 1 d . . . N1 N 0.9397(3) 0.5925(3) 0.10711(19) 0.0173(6) Uani 1 1 d . . . N2 N 0.6926(3) 0.7105(2) 0.10405(18) 0.0154(6) Uani 1 1 d . . . C1 C 0.9968(4) 0.6590(3) 0.3171(2) 0.0228(8) Uani 1 1 d . . . H1A H 1.0920 0.6467 0.3528 0.034 Uiso 1 1 calc R . . H1B H 0.9103 0.7361 0.3191 0.034 Uiso 1 1 calc R . . H1C H 1.0242 0.6695 0.2490 0.034 Uiso 1 1 calc R . . C2 C 0.9414(4) 0.5434(3) 0.3640(2) 0.0162(7) Uani 1 1 d . . . C3 C 1.0384(4) 0.4213(3) 0.3624(2) 0.0175(7) Uani 1 1 d . . . H3 H 1.1314 0.4165 0.3172 0.021 Uiso 1 1 calc R . . C4 C 0.9866(4) 0.3129(3) 0.4055(2) 0.0152(7) Uani 1 1 d . . . H4 H 1.0456 0.2335 0.3909 0.018 Uiso 1 1 calc R . . C5 C 0.8415(4) 0.3184(3) 0.4591(2) 0.0148(7) Uani 1 1 d . . . C6 C 0.7473(4) 0.4401(3) 0.4606(2) 0.0148(7) Uani 1 1 d . . . H6 H 0.6339 0.4521 0.4832 0.018 Uiso 1 1 calc R . . C7 C 0.7943(4) 0.5515(3) 0.4137(2) 0.0161(7) Uani 1 1 d . . . H7 H 0.7146 0.6382 0.4060 0.019 Uiso 1 1 calc R . . C8 C 0.7942(4) 0.1984(3) 0.5061(2) 0.0184(7) Uani 1 1 d . . . H8 H 0.7916 0.1644 0.4541 0.022 Uiso 1 1 calc R . . C9 C 0.9208(4) 0.0942(3) 0.5841(2) 0.0271(8) Uani 1 1 d . . . H9A H 1.0271 0.0772 0.5545 0.041 Uiso 1 1 calc R . . H9B H 0.8925 0.0150 0.6105 0.041 Uiso 1 1 calc R . . H9C H 0.9236 0.1241 0.6371 0.041 Uiso 1 1 calc R . . C10 C 0.6283(4) 0.2224(3) 0.5518(2) 0.0232(8) Uani 1 1 d . . . H10A H 0.6280 0.2547 0.6038 0.035 Uiso 1 1 calc R . . H10B H 0.6035 0.1416 0.5794 0.035 Uiso 1 1 calc R . . H10C H 0.5469 0.2862 0.5015 0.035 Uiso 1 1 calc R . . C11 C 1.0979(4) 0.4934(3) 0.1297(2) 0.0233(8) Uani 1 1 d . . . H11A H 1.1678 0.5196 0.1593 0.035 Uiso 1 1 calc R . . H11B H 1.1459 0.4822 0.0694 0.035 Uiso 1 1 calc R . . H11C H 1.0864 0.4119 0.1756 0.035 Uiso 1 1 calc R . . C12 C 0.9129(4) 0.6968(3) 0.0199(2) 0.0213(8) Uani 1 1 d . . . H12 H 0.9898 0.7131 -0.0293 0.026 Uiso 1 1 calc R . . C13 C 0.7601(4) 0.7699(3) 0.0173(2) 0.0208(8) Uani 1 1 d . . . H13 H 0.7070 0.8480 -0.0340 0.025 Uiso 1 1 calc R . . C14 C 0.8043(4) 0.5983(3) 0.1625(2) 0.0153(7) Uani 1 1 d . . . C15 C 0.5228(4) 0.7673(3) 0.1170(2) 0.0143(7) Uani 1 1 d . . . C16 C 0.4142(4) 0.7431(3) 0.0712(2) 0.0197(7) Uani 1 1 d . . . C17 C 0.2501(4) 0.8058(3) 0.0778(2) 0.0210(8) Uani 1 1 d . . . H17 H 0.1734 0.7906 0.0476 0.025 Uiso 1 1 calc R . . C18 C 0.1964(4) 0.8908(3) 0.1281(2) 0.0198(7) Uani 1 1 d . . . C19 C 0.3093(4) 0.9140(3) 0.1703(2) 0.0185(7) Uani 1 1 d . . . H19 H 0.2733 0.9717 0.2044 0.022 Uiso 1 1 calc R . . C20 C 0.4742(4) 0.8552(3) 0.1644(2) 0.0162(7) Uani 1 1 d . . . C21 C 0.4692(4) 0.6504(3) 0.0180(3) 0.0275(9) Uani 1 1 d . . . H21A H 0.5363 0.6815 -0.0368 0.041 Uiso 1 1 calc R . . H21B H 0.3750 0.6442 -0.0067 0.041 Uiso 1 1 calc R . . H21C H 0.5321 0.5653 0.0631 0.041 Uiso 1 1 calc R . . C22 C 0.0191(4) 0.9585(3) 0.1341(3) 0.0264(8) Uani 1 1 d . . . H22A H -0.0115 0.9363 0.2028 0.040 Uiso 1 1 calc R . . H22B H -0.0428 0.9312 0.1001 0.040 Uiso 1 1 calc R . . H22C H -0.0037 1.0518 0.1033 0.040 Uiso 1 1 calc R . . C23 C 0.5945(4) 0.8870(3) 0.2072(2) 0.0239(8) Uani 1 1 d . . . H23A H 0.5388 0.9621 0.2253 0.036 Uiso 1 1 calc R . . H23B H 0.6761 0.9063 0.1587 0.036 Uiso 1 1 calc R . . H23C H 0.6468 0.8133 0.2655 0.036 Uiso 1 1 calc R . . C24 C 0.4981(5) 0.1558(4) 0.3542(3) 0.0449(11) Uani 1 1 d . . . H24A H 0.5533 0.2174 0.3133 0.054 Uiso 1 1 calc R . . H24B H 0.4523 0.1810 0.4106 0.054 Uiso 1 1 calc R . . Cl1 Cl 0.33903(12) 0.16654(10) 0.28440(8) 0.0406(3) Uani 1 1 d . . . Cl2 Cl 0.63888(12) 0.00153(10) 0.39711(8) 0.0397(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01004(14) 0.01332(15) 0.01111(14) -0.00516(11) 0.00118(10) -0.00370(11) I1 0.01219(12) 0.02055(13) 0.01781(13) -0.00444(10) -0.00051(9) -0.00585(10) I2 0.02550(13) 0.02066(13) 0.01817(13) -0.01154(10) 0.00534(9) -0.00996(10) N1 0.0157(15) 0.0200(15) 0.0180(15) -0.0094(13) 0.0036(11) -0.0062(12) N2 0.0189(15) 0.0139(15) 0.0118(15) -0.0029(12) -0.0007(11) -0.0050(12) C1 0.0222(19) 0.0236(19) 0.026(2) -0.0082(16) -0.0057(15) -0.0112(16) C2 0.0157(17) 0.0204(18) 0.0134(17) -0.0052(15) -0.0052(13) -0.0064(15) C3 0.0132(17) 0.0237(19) 0.0151(17) -0.0076(15) -0.0005(13) -0.0046(15) C4 0.0129(17) 0.0158(17) 0.0156(17) -0.0061(14) -0.0060(13) -0.0007(14) C5 0.0181(17) 0.0180(18) 0.0066(16) -0.0040(14) -0.0025(13) -0.0034(14) C6 0.0155(17) 0.0198(18) 0.0088(16) -0.0047(14) -0.0002(13) -0.0060(14) C7 0.0161(17) 0.0184(18) 0.0155(17) -0.0097(15) -0.0034(13) -0.0025(14) C8 0.0237(19) 0.0176(18) 0.0141(18) -0.0033(15) -0.0039(14) -0.0083(15) C9 0.031(2) 0.020(2) 0.024(2) -0.0008(16) -0.0036(16) -0.0082(17) C10 0.0248(19) 0.023(2) 0.0194(19) -0.0026(16) 0.0033(15) -0.0111(16) C11 0.0144(18) 0.029(2) 0.029(2) -0.0144(17) 0.0090(15) -0.0079(16) C12 0.030(2) 0.024(2) 0.0101(18) -0.0041(15) 0.0061(14) -0.0138(17) C13 0.028(2) 0.0201(19) 0.0116(17) -0.0007(15) 0.0039(14) -0.0106(16) C14 0.0165(17) 0.0179(18) 0.0146(17) -0.0081(15) 0.0022(13) -0.0075(15) C15 0.0137(17) 0.0118(16) 0.0124(17) 0.0000(14) -0.0006(13) -0.0030(14) C16 0.028(2) 0.0099(17) 0.0173(18) -0.0022(15) -0.0042(14) -0.0029(15) C17 0.0213(19) 0.0171(18) 0.0193(19) 0.0005(15) -0.0088(14) -0.0051(15) C18 0.0191(18) 0.0146(18) 0.0176(18) 0.0015(15) 0.0006(14) -0.0043(15) C19 0.0229(19) 0.0147(18) 0.0141(18) -0.0018(15) 0.0001(14) -0.0054(15) C20 0.0210(18) 0.0131(17) 0.0112(17) 0.0005(14) -0.0019(13) -0.0065(15) C21 0.032(2) 0.026(2) 0.030(2) -0.0155(18) -0.0054(17) -0.0077(17) C22 0.0196(19) 0.024(2) 0.024(2) 0.0017(17) -0.0038(15) -0.0048(16) C23 0.023(2) 0.025(2) 0.028(2) -0.0151(17) -0.0002(16) -0.0069(16) C24 0.038(3) 0.040(3) 0.062(3) -0.019(2) -0.001(2) -0.017(2) Cl1 0.0292(5) 0.0346(6) 0.0598(7) -0.0270(5) -0.0030(5) -0.0002(4) Cl2 0.0308(6) 0.0426(6) 0.0524(7) -0.0220(5) -0.0050(5) -0.0131(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C14 2.103(3) . ? Ru1 C4 2.190(3) . ? Ru1 C7 2.217(3) . ? Ru1 C3 2.221(3) . ? Ru1 C6 2.226(3) . ? Ru1 C2 2.238(3) . ? Ru1 C5 2.267(3) . ? Ru1 I2 2.7381(5) . ? Ru1 I1 2.7492(6) . ? N1 C14 1.370(4) . ? N1 C12 1.381(4) . ? N1 C11 1.459(4) . ? N2 C14 1.381(4) . ? N2 C13 1.389(4) . ? N2 C15 1.444(4) . ? C1 C2 1.504(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.412(4) . ? C2 C3 1.418(4) . ? C3 C4 1.409(4) . ? C3 H3 1.0000 . ? C4 C5 1.425(4) . ? C4 H4 1.0000 . ? C5 C6 1.407(4) . ? C5 C8 1.509(4) . ? C6 C7 1.420(4) . ? C6 H6 1.0000 . ? C7 H7 1.0000 . ? C8 C10 1.524(4) . ? C8 C9 1.538(4) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.328(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C15 C16 1.392(4) . ? C15 C20 1.396(4) . ? C16 C17 1.396(5) . ? C16 C21 1.507(4) . ? C17 C18 1.401(5) . ? C17 H17 0.9500 . ? C18 C19 1.382(4) . ? C18 C22 1.505(4) . ? C19 C20 1.392(4) . ? C19 H19 0.9500 . ? C20 C23 1.508(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 Cl2 1.743(4) . ? C24 Cl1 1.774(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Ru1 C4 131.12(12) . . ? C14 Ru1 C7 109.79(12) . . ? C4 Ru1 C7 78.97(11) . . ? C14 Ru1 C3 100.60(12) . . ? C4 Ru1 C3 37.24(11) . . ? C7 Ru1 C3 66.14(11) . . ? C14 Ru1 C6 145.20(11) . . ? C4 Ru1 C6 65.98(11) . . ? C7 Ru1 C6 37.28(11) . . ? C3 Ru1 C6 77.75(11) . . ? C14 Ru1 C2 90.68(11) . . ? C4 Ru1 C2 67.54(11) . . ? C7 Ru1 C2 36.97(11) . . ? C3 Ru1 C2 37.08(11) . . ? C6 Ru1 C2 66.85(11) . . ? C14 Ru1 C5 167.50(12) . . ? C4 Ru1 C5 37.25(11) . . ? C7 Ru1 C5 67.12(11) . . ? C3 Ru1 C5 66.95(11) . . ? C6 Ru1 C5 36.48(11) . . ? C2 Ru1 C5 79.94(11) . . ? C14 Ru1 I2 85.68(8) . . ? C4 Ru1 I2 85.80(8) . . ? C7 Ru1 I2 163.14(9) . . ? C3 Ru1 I2 105.37(8) . . ? C6 Ru1 I2 128.66(8) . . ? C2 Ru1 I2 140.68(8) . . ? C5 Ru1 I2 96.32(8) . . ? C14 Ru1 I1 95.83(8) . . ? C4 Ru1 I1 131.53(8) . . ? C7 Ru1 I1 97.91(8) . . ? C3 Ru1 I1 160.18(8) . . ? C6 Ru1 I1 82.43(8) . . ? C2 Ru1 I1 132.55(8) . . ? C5 Ru1 I1 96.60(8) . . ? I2 Ru1 I1 86.748(12) . . ? C14 N1 C12 111.7(3) . . ? C14 N1 C11 128.4(3) . . ? C12 N1 C11 119.9(3) . . ? C14 N2 C13 111.3(3) . . ? C14 N2 C15 130.6(3) . . ? C13 N2 C15 117.9(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 117.7(3) . . ? C7 C2 C1 121.5(3) . . ? C3 C2 C1 120.8(3) . . ? C7 C2 Ru1 70.72(17) . . ? C3 C2 Ru1 70.83(17) . . ? C1 C2 Ru1 131.2(2) . . ? C4 C3 C2 121.1(3) . . ? C4 C3 Ru1 70.17(17) . . ? C2 C3 Ru1 72.09(17) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? Ru1 C3 H3 118.7 . . ? C3 C4 C5 121.8(3) . . ? C3 C4 Ru1 72.60(18) . . ? C5 C4 Ru1 74.34(17) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? Ru1 C4 H4 118.9 . . ? C6 C5 C4 116.2(3) . . ? C6 C5 C8 124.2(3) . . ? C4 C5 C8 119.6(3) . . ? C6 C5 Ru1 70.15(17) . . ? C4 C5 Ru1 68.42(17) . . ? C8 C5 Ru1 129.6(2) . . ? C5 C6 C7 122.6(3) . . ? C5 C6 Ru1 73.37(17) . . ? C7 C6 Ru1 71.01(17) . . ? C5 C6 H6 118.1 . . ? C7 C6 H6 118.1 . . ? Ru1 C6 H6 118.1 . . ? C2 C7 C6 120.5(3) . . ? C2 C7 Ru1 72.32(17) . . ? C6 C7 Ru1 71.71(17) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? Ru1 C7 H7 119.3 . . ? C5 C8 C10 113.4(3) . . ? C5 C8 C9 110.5(3) . . ? C10 C8 C9 109.4(3) . . ? C5 C8 H8 107.8 . . ? C10 C8 H8 107.8 . . ? C9 C8 H8 107.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 N1 107.5(3) . . ? C13 C12 H12 126.2 . . ? N1 C12 H12 126.2 . . ? C12 C13 N2 106.9(3) . . ? C12 C13 H13 126.6 . . ? N2 C13 H13 126.6 . . ? N1 C14 N2 102.6(3) . . ? N1 C14 Ru1 124.5(2) . . ? N2 C14 Ru1 132.9(2) . . ? C16 C15 C20 122.7(3) . . ? C16 C15 N2 117.8(3) . . ? C20 C15 N2 119.1(3) . . ? C15 C16 C17 117.6(3) . . ? C15 C16 C21 121.9(3) . . ? C17 C16 C21 120.4(3) . . ? C16 C17 C18 121.3(3) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C19 C18 C17 118.8(3) . . ? C19 C18 C22 120.5(3) . . ? C17 C18 C22 120.7(3) . . ? C18 C19 C20 122.0(3) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C19 C20 C15 117.5(3) . . ? C19 C20 C23 120.7(3) . . ? C15 C20 C23 121.7(3) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Cl2 C24 Cl1 112.6(2) . . ? Cl2 C24 H24A 109.1 . . ? Cl1 C24 H24A 109.1 . . ? Cl2 C24 H24B 109.1 . . ? Cl1 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Ru1 C2 C7 123.2(2) . . . . ? C4 Ru1 C2 C7 -101.8(2) . . . . ? C3 Ru1 C2 C7 -130.0(3) . . . . ? C6 Ru1 C2 C7 -29.43(19) . . . . ? C5 Ru1 C2 C7 -65.11(19) . . . . ? I2 Ru1 C2 C7 -152.80(15) . . . . ? I1 Ru1 C2 C7 24.6(2) . . . . ? C14 Ru1 C2 C3 -106.8(2) . . . . ? C4 Ru1 C2 C3 28.14(18) . . . . ? C7 Ru1 C2 C3 130.0(3) . . . . ? C6 Ru1 C2 C3 100.6(2) . . . . ? C5 Ru1 C2 C3 64.87(19) . . . . ? I2 Ru1 C2 C3 -22.8(2) . . . . ? I1 Ru1 C2 C3 154.61(15) . . . . ? C14 Ru1 C2 C1 7.8(3) . . . . ? C4 Ru1 C2 C1 142.8(3) . . . . ? C7 Ru1 C2 C1 -115.4(4) . . . . ? C3 Ru1 C2 C1 114.6(4) . . . . ? C6 Ru1 C2 C1 -144.8(3) . . . . ? C5 Ru1 C2 C1 179.5(3) . . . . ? I2 Ru1 C2 C1 91.8(3) . . . . ? I1 Ru1 C2 C1 -90.7(3) . . . . ? C7 C2 C3 C4 2.4(4) . . . . ? C1 C2 C3 C4 -179.5(3) . . . . ? Ru1 C2 C3 C4 -52.3(3) . . . . ? C7 C2 C3 Ru1 54.8(2) . . . . ? C1 C2 C3 Ru1 -127.2(3) . . . . ? C14 Ru1 C3 C4 -149.24(18) . . . . ? C7 Ru1 C3 C4 103.7(2) . . . . ? C6 Ru1 C3 C4 66.25(19) . . . . ? C2 Ru1 C3 C4 133.9(3) . . . . ? C5 Ru1 C3 C4 29.55(17) . . . . ? I2 Ru1 C3 C4 -60.85(18) . . . . ? I1 Ru1 C3 C4 65.2(3) . . . . ? C14 Ru1 C3 C2 76.8(2) . . . . ? C4 Ru1 C3 C2 -133.9(3) . . . . ? C7 Ru1 C3 C2 -30.25(18) . . . . ? C6 Ru1 C3 C2 -67.67(19) . . . . ? C5 Ru1 C3 C2 -104.4(2) . . . . ? I2 Ru1 C3 C2 165.23(16) . . . . ? I1 Ru1 C3 C2 -68.7(3) . . . . ? C2 C3 C4 C5 -5.0(5) . . . . ? Ru1 C3 C4 C5 -58.2(3) . . . . ? C2 C3 C4 Ru1 53.2(3) . . . . ? C14 Ru1 C4 C3 41.9(2) . . . . ? C7 Ru1 C4 C3 -64.88(19) . . . . ? C6 Ru1 C4 C3 -101.7(2) . . . . ? C2 Ru1 C4 C3 -28.03(18) . . . . ? C5 Ru1 C4 C3 -131.4(3) . . . . ? I2 Ru1 C4 C3 122.39(17) . . . . ? I1 Ru1 C4 C3 -155.71(15) . . . . ? C14 Ru1 C4 C5 173.27(17) . . . . ? C7 Ru1 C4 C5 66.54(18) . . . . ? C3 Ru1 C4 C5 131.4(3) . . . . ? C6 Ru1 C4 C5 29.73(17) . . . . ? C2 Ru1 C4 C5 103.38(19) . . . . ? I2 Ru1 C4 C5 -106.19(16) . . . . ? I1 Ru1 C4 C5 -24.3(2) . . . . ? C3 C4 C5 C6 4.3(4) . . . . ? Ru1 C4 C5 C6 -53.0(2) . . . . ? C3 C4 C5 C8 -178.3(3) . . . . ? Ru1 C4 C5 C8 124.4(3) . . . . ? C3 C4 C5 Ru1 57.4(3) . . . . ? C14 Ru1 C5 C6 106.3(5) . . . . ? C4 Ru1 C5 C6 130.4(3) . . . . ? C7 Ru1 C5 C6 28.13(18) . . . . ? C3 Ru1 C5 C6 100.8(2) . . . . ? C2 Ru1 C5 C6 64.43(19) . . . . ? I2 Ru1 C5 C6 -155.14(17) . . . . ? I1 Ru1 C5 C6 -67.70(17) . . . . ? C14 Ru1 C5 C4 -24.1(6) . . . . ? C7 Ru1 C5 C4 -102.24(19) . . . . ? C3 Ru1 C5 C4 -29.55(17) . . . . ? C6 Ru1 C5 C4 -130.4(3) . . . . ? C2 Ru1 C5 C4 -65.93(18) . . . . ? I2 Ru1 C5 C4 74.50(16) . . . . ? I1 Ru1 C5 C4 161.94(16) . . . . ? C14 Ru1 C5 C8 -135.3(5) . . . . ? C4 Ru1 C5 C8 -111.2(3) . . . . ? C7 Ru1 C5 C8 146.6(3) . . . . ? C3 Ru1 C5 C8 -140.7(3) . . . . ? C6 Ru1 C5 C8 118.4(4) . . . . ? C2 Ru1 C5 C8 -177.1(3) . . . . ? I2 Ru1 C5 C8 -36.7(3) . . . . ? I1 Ru1 C5 C8 50.7(3) . . . . ? C4 C5 C6 C7 -1.4(4) . . . . ? C8 C5 C6 C7 -178.7(3) . . . . ? Ru1 C5 C6 C7 -53.6(3) . . . . ? C4 C5 C6 Ru1 52.2(2) . . . . ? C8 C5 C6 Ru1 -125.1(3) . . . . ? C14 Ru1 C6 C5 -158.7(2) . . . . ? C4 Ru1 C6 C5 -30.33(17) . . . . ? C7 Ru1 C6 C5 -134.2(3) . . . . ? C3 Ru1 C6 C5 -67.65(19) . . . . ? C2 Ru1 C6 C5 -105.0(2) . . . . ? I2 Ru1 C6 C5 32.3(2) . . . . ? I1 Ru1 C6 C5 112.00(17) . . . . ? C14 Ru1 C6 C7 -24.5(3) . . . . ? C4 Ru1 C6 C7 103.9(2) . . . . ? C3 Ru1 C6 C7 66.54(19) . . . . ? C2 Ru1 C6 C7 29.20(18) . . . . ? C5 Ru1 C6 C7 134.2(3) . . . . ? I2 Ru1 C6 C7 166.54(14) . . . . ? I1 Ru1 C6 C7 -113.81(18) . . . . ? C3 C2 C7 C6 0.4(4) . . . . ? C1 C2 C7 C6 -177.6(3) . . . . ? Ru1 C2 C7 C6 55.3(3) . . . . ? C3 C2 C7 Ru1 -54.8(2) . . . . ? C1 C2 C7 Ru1 127.1(3) . . . . ? C5 C6 C7 C2 -0.9(4) . . . . ? Ru1 C6 C7 C2 -55.5(3) . . . . ? C5 C6 C7 Ru1 54.6(3) . . . . ? C14 Ru1 C7 C2 -62.8(2) . . . . ? C4 Ru1 C7 C2 67.14(19) . . . . ? C3 Ru1 C7 C2 30.34(18) . . . . ? C6 Ru1 C7 C2 131.8(3) . . . . ? C5 Ru1 C7 C2 104.2(2) . . . . ? I2 Ru1 C7 C2 92.9(3) . . . . ? I1 Ru1 C7 C2 -161.94(17) . . . . ? C14 Ru1 C7 C6 165.45(18) . . . . ? C4 Ru1 C7 C6 -64.62(19) . . . . ? C3 Ru1 C7 C6 -101.4(2) . . . . ? C2 Ru1 C7 C6 -131.8(3) . . . . ? C5 Ru1 C7 C6 -27.56(18) . . . . ? I2 Ru1 C7 C6 -38.8(4) . . . . ? I1 Ru1 C7 C6 66.30(18) . . . . ? C6 C5 C8 C10 3.0(4) . . . . ? C4 C5 C8 C10 -174.1(3) . . . . ? Ru1 C5 C8 C10 -88.6(3) . . . . ? C6 C5 C8 C9 -120.2(3) . . . . ? C4 C5 C8 C9 62.6(4) . . . . ? Ru1 C5 C8 C9 148.1(2) . . . . ? C14 N1 C12 C13 -0.8(4) . . . . ? C11 N1 C12 C13 178.9(3) . . . . ? N1 C12 C13 N2 0.4(4) . . . . ? C14 N2 C13 C12 0.2(4) . . . . ? C15 N2 C13 C12 -176.3(3) . . . . ? C12 N1 C14 N2 0.9(3) . . . . ? C11 N1 C14 N2 -178.8(3) . . . . ? C12 N1 C14 Ru1 -176.1(2) . . . . ? C11 N1 C14 Ru1 4.2(4) . . . . ? C13 N2 C14 N1 -0.6(3) . . . . ? C15 N2 C14 N1 175.3(3) . . . . ? C13 N2 C14 Ru1 176.0(2) . . . . ? C15 N2 C14 Ru1 -8.1(5) . . . . ? C4 Ru1 C14 N1 10.9(3) . . . . ? C7 Ru1 C14 N1 103.5(3) . . . . ? C3 Ru1 C14 N1 35.2(3) . . . . ? C6 Ru1 C14 N1 118.9(3) . . . . ? C2 Ru1 C14 N1 71.1(2) . . . . ? C5 Ru1 C14 N1 30.1(7) . . . . ? I2 Ru1 C14 N1 -69.7(2) . . . . ? I1 Ru1 C14 N1 -156.0(2) . . . . ? C4 Ru1 C14 N2 -165.1(2) . . . . ? C7 Ru1 C14 N2 -72.5(3) . . . . ? C3 Ru1 C14 N2 -140.8(3) . . . . ? C6 Ru1 C14 N2 -57.1(4) . . . . ? C2 Ru1 C14 N2 -104.9(3) . . . . ? C5 Ru1 C14 N2 -145.9(4) . . . . ? I2 Ru1 C14 N2 114.3(3) . . . . ? I1 Ru1 C14 N2 28.0(3) . . . . ? C14 N2 C15 C16 -96.3(4) . . . . ? C13 N2 C15 C16 79.4(4) . . . . ? C14 N2 C15 C20 91.2(4) . . . . ? C13 N2 C15 C20 -93.1(3) . . . . ? C20 C15 C16 C17 -3.1(5) . . . . ? N2 C15 C16 C17 -175.4(3) . . . . ? C20 C15 C16 C21 178.4(3) . . . . ? N2 C15 C16 C21 6.1(5) . . . . ? C15 C16 C17 C18 0.5(5) . . . . ? C21 C16 C17 C18 179.0(3) . . . . ? C16 C17 C18 C19 1.1(5) . . . . ? C16 C17 C18 C22 179.6(3) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C22 C18 C19 C20 -178.6(3) . . . . ? C18 C19 C20 C15 -2.3(5) . . . . ? C18 C19 C20 C23 177.2(3) . . . . ? C16 C15 C20 C19 4.0(5) . . . . ? N2 C15 C20 C19 176.2(3) . . . . ? C16 C15 C20 C23 -175.5(3) . . . . ? N2 C15 C20 C23 -3.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.630 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.102 #===END data_071227d _database_code_depnum_ccdc_archive 'CCDC 675613' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H30 I2 N2 Ru' _chemical_formula_weight 653.33 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.958(6) _cell_length_b 24.186(8) _cell_length_c 10.345(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4743(3) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3780 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 26.50 _exptl_crystal_description block _exptl_crystal_colour black-red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 3.270 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.646383 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18648 _diffrn_reflns_av_R_equivalents 0.1413 _diffrn_reflns_av_sigmaI/netI 0.2097 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8095 _reflns_number_gt 3497 _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^)+(0.0340P)^2^+169.4393P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00137(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(8) _refine_ls_number_reflns 8095 _refine_ls_number_parameters 460 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.2499 _refine_ls_R_factor_gt 0.0948 _refine_ls_wR_factor_ref 0.2366 _refine_ls_wR_factor_gt 0.1629 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.61915(14) 0.60328(10) 0.8236(3) 0.0496(7) Uani 1 1 d . . . Ru2 Ru 0.07483(14) 0.38053(10) 0.8196(3) 0.0477(7) Uani 1 1 d . . . I1 I 0.68680(13) 0.67001(9) 0.6430(2) 0.0666(7) Uani 1 1 d . . . I2 I 0.54658(16) 0.56372(12) 0.6087(3) 0.0975(11) Uani 1 1 d . . . I3 I 0.15590(12) 0.31498(9) 0.6562(2) 0.0619(7) Uani 1 1 d . . . I4 I 0.00457(15) 0.41168(10) 0.5942(3) 0.0735(8) Uani 1 1 d . . . N1 N 0.472(2) 0.6530(13) 0.884(3) 0.076(10) Uani 1 1 d . . . N2 N 0.5460(18) 0.7172(12) 0.903(3) 0.062(8) Uani 1 1 d . . . N3 N -0.0697(14) 0.3235(10) 0.863(2) 0.045(7) Uani 1 1 d . . . N4 N 0.0138(16) 0.2624(12) 0.895(3) 0.054(8) Uani 1 1 d U . . C1 C 0.431(2) 0.5999(14) 0.871(4) 0.100(17) Uani 1 1 d . . . H1A H 0.4400 0.5770 0.9450 0.150 Uiso 1 1 calc R . . H1B H 0.4466 0.5808 0.7942 0.150 Uiso 1 1 calc R . . H1C H 0.3820 0.6079 0.8646 0.150 Uiso 1 1 calc R . . C2 C 0.436(2) 0.6996(19) 0.925(4) 0.079(13) Uani 1 1 d . . . H2 H 0.3877 0.7029 0.9372 0.095 Uiso 1 1 calc R . . C3 C 0.483(3) 0.7377(19) 0.943(4) 0.080(13) Uani 1 1 d . . . H3 H 0.4748 0.7728 0.9765 0.095 Uiso 1 1 calc R . . C4 C 0.543(2) 0.6594(14) 0.865(3) 0.057(11) Uani 1 1 d . . . C5 C 0.6110(19) 0.7479(14) 0.906(3) 0.052(9) Uani 1 1 d . . . H5 H 0.6487 0.7227 0.8780 0.062 Uiso 1 1 calc R . . C6 C 0.632(2) 0.7707(16) 1.043(3) 0.086(14) Uani 1 1 d . . . H6A H 0.5943 0.7950 1.0724 0.104 Uiso 1 1 calc R . . H6B H 0.6341 0.7399 1.1026 0.104 Uiso 1 1 calc R . . C7 C 0.702(2) 0.803(2) 1.050(5) 0.104(18) Uani 1 1 d . . . H7A H 0.7416 0.7780 1.0331 0.125 Uiso 1 1 calc R . . H7B H 0.7084 0.8192 1.1343 0.125 Uiso 1 1 calc R . . C8 C 0.698(3) 0.849(2) 0.941(8) 0.16(3) Uani 1 1 d . . . H8A H 0.6614 0.8754 0.9651 0.196 Uiso 1 1 calc R . . H8B H 0.7423 0.8689 0.9387 0.196 Uiso 1 1 calc R . . C9 C 0.682(2) 0.8268(17) 0.806(5) 0.102(16) Uani 1 1 d . . . H9A H 0.7190 0.8020 0.7784 0.122 Uiso 1 1 calc R . . H9B H 0.6787 0.8571 0.7449 0.122 Uiso 1 1 calc R . . C10 C 0.610(2) 0.7952(15) 0.813(4) 0.078(12) Uani 1 1 d . . . H10A H 0.5728 0.8208 0.8383 0.094 Uiso 1 1 calc R . . H10B H 0.5980 0.7814 0.7273 0.094 Uiso 1 1 calc R . . C11 C 0.558(2) 0.5962(14) 1.140(3) 0.097(14) Uani 1 1 d . . . H11A H 0.5440 0.6340 1.1288 0.146 Uiso 1 1 calc R . . H11B H 0.5773 0.5912 1.2249 0.146 Uiso 1 1 calc R . . H11C H 0.5181 0.5724 1.1288 0.146 Uiso 1 1 calc R . . C12 C 0.615(2) 0.5816(14) 1.039(3) 0.061(10) Uani 1 1 d . . . C13 C 0.601(2) 0.5347(18) 0.953(4) 0.086(13) Uani 1 1 d . . . H13 H 0.5574 0.5166 0.9560 0.104 Uiso 1 1 calc R . . C14 C 0.6562(18) 0.5162(14) 0.861(3) 0.061(10) Uani 1 1 d U . . H14 H 0.6501 0.4834 0.8153 0.073 Uiso 1 1 calc R . . C15 C 0.7167(17) 0.5469(12) 0.842(3) 0.044(8) Uani 1 1 d U . . C16 C 0.7217(17) 0.5972(13) 0.912(3) 0.050(9) Uani 1 1 d U . . H16 H 0.7584 0.6212 0.8914 0.060 Uiso 1 1 calc R . . C17 C 0.6730(17) 0.6135(13) 1.013(3) 0.050(8) Uani 1 1 d U . . H17 H 0.6812 0.6455 1.0601 0.060 Uiso 1 1 calc R . . C18 C 0.775(2) 0.5286(17) 0.744(4) 0.076(12) Uani 1 1 d U . . H18 H 0.7781 0.5597 0.6838 0.091 Uiso 1 1 calc R . . C19 C 0.7516(19) 0.4797(15) 0.659(4) 0.090(13) Uani 1 1 d . . . H19A H 0.7553 0.4459 0.7069 0.136 Uiso 1 1 calc R . . H19B H 0.7813 0.4777 0.5837 0.136 Uiso 1 1 calc R . . H19C H 0.7035 0.4850 0.6321 0.136 Uiso 1 1 calc R . . C20 C 0.848(2) 0.5253(19) 0.802(5) 0.120(18) Uani 1 1 d . . . H20A H 0.8451 0.5068 0.8843 0.179 Uiso 1 1 calc R . . H20B H 0.8658 0.5620 0.8145 0.179 Uiso 1 1 calc R . . H20C H 0.8781 0.5051 0.7453 0.179 Uiso 1 1 calc R . . C21 C -0.1155(17) 0.3728(14) 0.846(3) 0.069(12) Uani 1 1 d . . . H21A H -0.1406 0.3699 0.7659 0.104 Uiso 1 1 calc R . . H21B H -0.0869 0.4055 0.8453 0.104 Uiso 1 1 calc R . . H21C H -0.1485 0.3748 0.9163 0.104 Uiso 1 1 calc R . . C22 C -0.1038(19) 0.2737(14) 0.901(3) 0.062(11) Uani 1 1 d . . . H22 H -0.1518 0.2675 0.9126 0.074 Uiso 1 1 calc R . . C23 C -0.051(2) 0.2377(17) 0.917(4) 0.068(11) Uani 1 1 d U . . H23 H -0.0567 0.2008 0.9399 0.082 Uiso 1 1 calc R . . C24 C 0.0018(17) 0.3204(14) 0.855(3) 0.052(9) Uani 1 1 d . . . C25 C 0.081(2) 0.2348(15) 0.910(4) 0.070(11) Uani 1 1 d . . . H25 H 0.1186 0.2604 0.8869 0.084 Uiso 1 1 calc R . . C26 C 0.0872(19) 0.1831(15) 0.830(4) 0.072(11) Uani 1 1 d . . . H26A H 0.0826 0.1921 0.7390 0.087 Uiso 1 1 calc R . . H26B H 0.0500 0.1573 0.8527 0.087 Uiso 1 1 calc R . . C27 C 0.161(2) 0.1564(17) 0.857(5) 0.109(19) Uani 1 1 d . . . H27A H 0.1673 0.1237 0.8032 0.131 Uiso 1 1 calc R . . H27B H 0.1984 0.1825 0.8346 0.131 Uiso 1 1 calc R . . C28 C 0.168(2) 0.140(2) 1.001(6) 0.12(2) Uani 1 1 d . . . H28A H 0.1309 0.1141 1.0230 0.143 Uiso 1 1 calc R . . H28B H 0.2130 0.1230 1.0165 0.143 Uiso 1 1 calc R . . C29 C 0.161(2) 0.1899(18) 1.079(4) 0.104(17) Uani 1 1 d . . . H29A H 0.1985 0.2154 1.0582 0.124 Uiso 1 1 calc R . . H29B H 0.1650 0.1802 1.1698 0.124 Uiso 1 1 calc R . . C30 C 0.087(2) 0.2191(15) 1.056(4) 0.074(12) Uani 1 1 d . . . H30A H 0.0493 0.1943 1.0797 0.089 Uiso 1 1 calc R . . H30B H 0.0838 0.2521 1.1085 0.089 Uiso 1 1 calc R . . C31 C 0.007(2) 0.3852(16) 1.127(3) 0.100(15) Uani 1 1 d . . . H31A H 0.0246 0.3910 1.2129 0.151 Uiso 1 1 calc R . . H31B H -0.0014 0.3465 1.1134 0.151 Uiso 1 1 calc R . . H31C H -0.0359 0.4055 1.1152 0.151 Uiso 1 1 calc R . . C32 C 0.061(2) 0.4051(18) 1.031(3) 0.090(15) Uani 1 1 d . . . C33 C 0.126(2) 0.3765(15) 1.008(3) 0.064(10) Uani 1 1 d U . . H33 H 0.1358 0.3441 1.0529 0.077 Uiso 1 1 calc R . . C34 C 0.1762(19) 0.3980(14) 0.916(3) 0.061(10) Uani 1 1 d . . . H34 H 0.2178 0.3783 0.9038 0.073 Uiso 1 1 calc R . . C35 C 0.1663(18) 0.4479(13) 0.842(4) 0.057(10) Uani 1 1 d . . . C36 C 0.0993(19) 0.4672(16) 0.852(3) 0.066(11) Uani 1 1 d . . . H36 H 0.0864 0.4946 0.7934 0.079 Uiso 1 1 calc R . . C37 C 0.044(2) 0.4502(17) 0.945(4) 0.084(12) Uani 1 1 d U . . H37 H 0.0005 0.4678 0.9483 0.101 Uiso 1 1 calc R . . C38 C 0.219(2) 0.4703(17) 0.749(4) 0.082(13) Uani 1 1 d . . . H38 H 0.2351 0.4383 0.6991 0.099 Uiso 1 1 calc R . . C39 C 0.190(3) 0.5116(16) 0.648(4) 0.13(2) Uani 1 1 d . . . H39A H 0.1823 0.5468 0.6882 0.195 Uiso 1 1 calc R . . H39B H 0.1464 0.4978 0.6138 0.195 Uiso 1 1 calc R . . H39C H 0.2237 0.5157 0.5791 0.195 Uiso 1 1 calc R . . C40 C 0.284(2) 0.490(2) 0.821(5) 0.16(3) Uani 1 1 d . . . H40A H 0.2959 0.4634 0.8861 0.236 Uiso 1 1 calc R . . H40B H 0.2738 0.5249 0.8607 0.236 Uiso 1 1 calc R . . H40C H 0.3221 0.4940 0.7613 0.236 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 0.0412(17) 0.0496(16) 0.0579(16) -0.0047(16) -0.0023(16) -0.0021(13) Ru2 0.0469(18) 0.0459(16) 0.0504(15) -0.0021(15) 0.0037(16) -0.0005(13) I1 0.0746(18) 0.0651(15) 0.0600(15) 0.0101(14) 0.0099(15) 0.0137(12) I2 0.089(2) 0.098(2) 0.106(3) -0.040(2) -0.036(2) -0.0019(17) I3 0.0616(17) 0.0566(14) 0.0674(16) -0.0110(13) 0.0184(15) -0.0064(12) I4 0.079(2) 0.0683(17) 0.0737(16) 0.0160(15) -0.0162(16) -0.0064(14) N1 0.11(3) 0.05(2) 0.07(2) -0.015(16) -0.01(2) -0.01(2) N2 0.07(3) 0.05(2) 0.06(2) -0.008(16) 0.003(18) -0.011(18) N3 0.050(19) 0.035(15) 0.049(16) 0.013(12) 0.022(14) 0.009(13) N4 0.047(11) 0.055(11) 0.059(10) 0.002(8) 0.001(8) -0.008(9) C1 0.15(4) 0.03(2) 0.12(4) -0.02(2) -0.06(3) -0.01(2) C2 0.05(3) 0.08(3) 0.11(4) -0.01(3) 0.00(3) 0.02(3) C3 0.09(4) 0.08(3) 0.06(3) -0.03(2) 0.01(3) 0.00(3) C4 0.09(3) 0.06(2) 0.025(17) 0.003(14) -0.010(18) -0.04(2) C5 0.05(3) 0.06(2) 0.04(2) 0.008(17) 0.001(18) 0.02(2) C6 0.12(4) 0.07(3) 0.07(3) 0.01(2) -0.04(3) 0.02(3) C7 0.08(4) 0.10(4) 0.13(4) -0.07(3) -0.05(3) 0.02(3) C8 0.09(4) 0.07(4) 0.33(10) -0.04(5) -0.07(5) -0.02(3) C9 0.10(4) 0.06(3) 0.14(4) 0.01(3) 0.03(4) -0.02(2) C10 0.09(3) 0.07(3) 0.08(3) 0.02(2) 0.00(3) 0.01(2) C11 0.16(4) 0.08(3) 0.05(2) 0.01(2) 0.05(3) 0.03(3) C12 0.08(3) 0.06(2) 0.04(2) 0.019(18) -0.01(2) -0.03(2) C13 0.06(3) 0.11(4) 0.09(3) 0.01(3) 0.02(3) -0.01(3) C14 0.060(13) 0.058(13) 0.064(13) 0.002(9) 0.002(9) 0.002(9) C15 0.048(11) 0.043(11) 0.040(11) -0.005(9) 0.008(9) -0.008(8) C16 0.048(12) 0.050(12) 0.053(11) -0.003(9) 0.006(9) 0.006(9) C17 0.052(12) 0.049(11) 0.049(11) 0.010(9) 0.000(9) 0.008(9) C18 0.073(14) 0.079(14) 0.074(14) 0.003(9) 0.001(9) 0.003(9) C19 0.08(3) 0.10(3) 0.09(3) -0.01(3) 0.00(3) -0.01(2) C20 0.13(5) 0.12(4) 0.11(4) -0.02(4) 0.00(4) 0.05(3) C21 0.05(2) 0.09(3) 0.07(3) -0.02(2) -0.03(2) 0.03(2) C22 0.04(2) 0.05(2) 0.09(3) 0.05(2) 0.01(2) -0.010(18) C23 0.068(11) 0.068(11) 0.068(11) 0.0000(10) 0.0000(10) 0.0000(10) C24 0.04(2) 0.08(3) 0.031(17) 0.003(16) 0.012(15) 0.029(18) C25 0.08(3) 0.05(2) 0.08(3) 0.01(2) -0.01(2) 0.01(2) C26 0.07(3) 0.08(3) 0.07(2) -0.02(2) 0.04(2) -0.01(2) C27 0.10(4) 0.08(3) 0.15(5) 0.03(3) 0.08(4) 0.04(3) C28 0.05(3) 0.13(5) 0.19(6) 0.08(4) 0.01(3) 0.00(3) C29 0.12(4) 0.08(3) 0.11(4) 0.06(3) -0.03(3) 0.02(3) C30 0.08(3) 0.05(2) 0.09(3) 0.01(2) -0.01(2) 0.00(2) C31 0.12(4) 0.13(4) 0.06(3) -0.03(2) 0.06(3) -0.04(3) C32 0.13(4) 0.11(4) 0.032(19) -0.05(2) 0.03(2) -0.04(3) C33 0.061(13) 0.065(13) 0.066(13) -0.004(9) 0.002(9) -0.005(9) C34 0.07(3) 0.05(2) 0.06(2) 0.022(18) -0.01(2) -0.007(19) C35 0.04(2) 0.05(2) 0.08(3) -0.01(2) -0.01(2) -0.005(16) C36 0.06(3) 0.11(3) 0.03(2) 0.008(19) -0.001(17) -0.02(2) C37 0.084(12) 0.084(12) 0.084(12) 0.0000(10) 0.0000(10) 0.0001(10) C38 0.09(3) 0.08(3) 0.08(3) 0.00(2) 0.04(3) -0.04(3) C39 0.25(6) 0.09(3) 0.05(2) 0.02(3) -0.01(4) -0.06(4) C40 0.13(5) 0.25(7) 0.09(3) -0.06(4) 0.07(4) -0.14(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C4 2.03(4) . ? Ru1 C16 2.15(3) . ? Ru1 C13 2.16(4) . ? Ru1 C17 2.22(3) . ? Ru1 C14 2.25(3) . ? Ru1 C12 2.29(3) . ? Ru1 C15 2.31(3) . ? Ru1 I1 2.782(4) . ? Ru1 I2 2.784(4) . ? Ru2 C24 2.04(4) . ? Ru2 C36 2.17(4) . ? Ru2 C33 2.18(4) . ? Ru2 C34 2.21(3) . ? Ru2 C37 2.21(4) . ? Ru2 C32 2.28(3) . ? Ru2 C35 2.39(3) . ? Ru2 I3 2.781(3) . ? Ru2 I4 2.790(4) . ? N1 C4 1.37(4) . ? N1 C2 1.38(5) . ? N1 C1 1.50(4) . ? N2 C3 1.36(5) . ? N2 C5 1.44(4) . ? N2 C4 1.45(4) . ? N3 C24 1.36(4) . ? N3 C22 1.42(4) . ? N3 C21 1.49(4) . ? N4 C23 1.38(4) . ? N4 C25 1.44(4) . ? N4 C24 1.48(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.29(5) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C5 C10 1.50(4) . ? C5 C6 1.57(4) . ? C5 H5 0.9800 . ? C6 C7 1.55(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.59(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.53(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.57(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.54(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C17 1.38(4) . ? C12 C13 1.46(5) . ? C13 C14 1.49(5) . ? C13 H13 0.9300 . ? C14 C15 1.38(4) . ? C14 H14 0.9300 . ? C15 C16 1.42(4) . ? C15 C18 1.56(5) . ? C16 C17 1.45(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C20 1.50(5) . ? C18 C19 1.54(5) . ? C18 H18 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.34(5) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C25 C26 1.50(4) . ? C25 C30 1.56(5) . ? C25 H25 0.9800 . ? C26 C27 1.57(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.54(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.46(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.58(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.50(5) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.43(5) . ? C32 C37 1.44(5) . ? C33 C34 1.44(4) . ? C33 H33 0.9300 . ? C34 C35 1.44(4) . ? C34 H34 0.9300 . ? C35 C36 1.36(4) . ? C35 C38 1.49(5) . ? C36 C37 1.48(5) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C40 1.50(5) . ? C38 C39 1.55(5) . ? C38 H38 0.9800 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? 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 C4 Ru1 C16 126.8(12) . . ? C4 Ru1 C13 105.5(14) . . ? C16 Ru1 C13 80.4(14) . . ? C4 Ru1 C17 93.9(12) . . ? C16 Ru1 C17 38.7(11) . . ? C13 Ru1 C17 67.4(14) . . ? C4 Ru1 C14 144.3(13) . . ? C16 Ru1 C14 65.3(12) . . ? C13 Ru1 C14 39.4(12) . . ? C17 Ru1 C14 79.0(12) . . ? C4 Ru1 C12 85.5(13) . . ? C16 Ru1 C12 66.8(13) . . ? C13 Ru1 C12 38.3(13) . . ? C17 Ru1 C12 35.5(11) . . ? C14 Ru1 C12 68.3(12) . . ? C4 Ru1 C15 161.8(11) . . ? C16 Ru1 C15 36.9(10) . . ? C13 Ru1 C15 68.0(13) . . ? C17 Ru1 C15 67.9(11) . . ? C14 Ru1 C15 35.2(10) . . ? C12 Ru1 C15 79.3(13) . . ? C4 Ru1 I1 94.7(9) . . ? C16 Ru1 I1 84.7(9) . . ? C13 Ru1 I1 159.5(11) . . ? C17 Ru1 I1 108.4(8) . . ? C14 Ru1 I1 120.9(9) . . ? C12 Ru1 I1 143.5(9) . . ? C15 Ru1 I1 91.7(7) . . ? C4 Ru1 I2 92.7(9) . . ? C16 Ru1 I2 139.6(8) . . ? C13 Ru1 I2 98.6(12) . . ? C17 Ru1 I2 165.7(8) . . ? C14 Ru1 I2 88.3(9) . . ? C12 Ru1 I2 132.8(9) . . ? C15 Ru1 I2 105.0(7) . . ? I1 Ru1 I2 83.72(13) . . ? C24 Ru2 C36 143.5(13) . . ? C24 Ru2 C33 96.2(13) . . ? C36 Ru2 C33 79.0(13) . . ? C24 Ru2 C34 130.2(12) . . ? C36 Ru2 C34 63.9(13) . . ? C33 Ru2 C34 38.5(12) . . ? C24 Ru2 C37 105.0(14) . . ? C36 Ru2 C37 39.5(12) . . ? C33 Ru2 C37 67.9(14) . . ? C34 Ru2 C37 79.5(15) . . ? C24 Ru2 C32 86.2(13) . . ? C36 Ru2 C32 68.0(13) . . ? C33 Ru2 C32 37.3(13) . . ? C34 Ru2 C32 67.4(15) . . ? C37 Ru2 C32 37.5(14) . . ? C24 Ru2 C35 163.8(12) . . ? C36 Ru2 C35 34.2(11) . . ? C33 Ru2 C35 67.8(13) . . ? C34 Ru2 C35 36.3(11) . . ? C37 Ru2 C35 67.3(14) . . ? C32 Ru2 C35 79.3(13) . . ? C24 Ru2 I3 94.5(8) . . ? C36 Ru2 I3 121.7(9) . . ? C33 Ru2 I3 105.9(10) . . ? C34 Ru2 I3 84.4(10) . . ? C37 Ru2 I3 160.0(11) . . ? C32 Ru2 I3 142.6(13) . . ? C35 Ru2 I3 92.6(9) . . ? C24 Ru2 I4 91.1(8) . . ? C36 Ru2 I4 88.3(9) . . ? C33 Ru2 I4 166.5(10) . . ? C34 Ru2 I4 137.9(8) . . ? C37 Ru2 I4 99.2(11) . . ? C32 Ru2 I4 132.6(13) . . ? C35 Ru2 I4 104.0(9) . . ? I3 Ru2 I4 84.81(12) . . ? C4 N1 C2 116(3) . . ? C4 N1 C1 126(3) . . ? C2 N1 C1 118(4) . . ? C3 N2 C5 124(3) . . ? C3 N2 C4 113(3) . . ? C5 N2 C4 122(3) . . ? C24 N3 C22 115(3) . . ? C24 N3 C21 128(3) . . ? C22 N3 C21 117(3) . . ? C23 N4 C25 124(3) . . ? C23 N4 C24 109(3) . . ? C25 N4 C24 127(3) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 N1 107(4) . . ? C3 C2 H2 126.6 . . ? N1 C2 H2 126.6 . . ? C2 C3 N2 107(4) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? N1 C4 N2 96(3) . . ? N1 C4 Ru1 131(3) . . ? N2 C4 Ru1 132(3) . . ? N2 C5 C10 111(3) . . ? N2 C5 C6 114(3) . . ? C10 C5 C6 108(3) . . ? N2 C5 H5 107.4 . . ? C10 C5 H5 107.4 . . ? C6 C5 H5 107.4 . . ? C7 C6 C5 116(3) . . ? C7 C6 H6A 108.4 . . ? C5 C6 H6A 108.4 . . ? C7 C6 H6B 108.4 . . ? C5 C6 H6B 108.4 . . ? H6A C6 H6B 107.4 . . ? C6 C7 C8 106(3) . . ? C6 C7 H7A 110.5 . . ? C8 C7 H7A 110.5 . . ? C6 C7 H7B 110.5 . . ? C8 C7 H7B 110.5 . . ? H7A C7 H7B 108.7 . . ? C9 C8 C7 114(4) . . ? C9 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C8 C9 C10 108(4) . . ? C8 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? C8 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? C5 C10 C9 113(3) . . ? C5 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? C5 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 118(3) . . ? C17 C12 C11 124(3) . . ? C13 C12 C11 118(3) . . ? C17 C12 Ru1 69.6(18) . . ? C13 C12 Ru1 66(2) . . ? C11 C12 Ru1 129(2) . . ? C12 C13 C14 119(4) . . ? C12 C13 Ru1 75(2) . . ? C14 C13 Ru1 74(2) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? Ru1 C13 H13 121.7 . . ? C15 C14 C13 121(3) . . ? C15 C14 Ru1 74(2) . . ? C13 C14 Ru1 67(2) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? Ru1 C14 H14 132.1 . . ? C14 C15 C16 116(3) . . ? C14 C15 C18 122(3) . . ? C16 C15 C18 122(3) . . ? C14 C15 Ru1 70.3(19) . . ? C16 C15 Ru1 65.6(18) . . ? C18 C15 Ru1 133(2) . . ? C15 C16 C17 124(3) . . ? C15 C16 Ru1 77.5(19) . . ? C17 C16 Ru1 73.2(18) . . ? C15 C16 H16 118.1 . . ? C17 C16 H16 118.1 . . ? Ru1 C16 H16 122.5 . . ? C12 C17 C16 120(3) . . ? C12 C17 Ru1 75(2) . . ? C16 C17 Ru1 68.1(17) . . ? C12 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? Ru1 C17 H17 129.4 . . ? C20 C18 C19 117(3) . . ? C20 C18 C15 114(3) . . ? C19 C18 C15 113(3) . . ? C20 C18 H18 103.9 . . ? C19 C18 H18 103.9 . . ? C15 C18 H18 103.9 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 N3 104(3) . . ? C23 C22 H22 128.0 . . ? N3 C22 H22 128.0 . . ? C22 C23 N4 111(4) . . ? C22 C23 H23 124.3 . . ? N4 C23 H23 124.3 . . ? N3 C24 N4 101(3) . . ? N3 C24 Ru2 130(2) . . ? N4 C24 Ru2 128(2) . . ? N4 C25 C26 114(3) . . ? N4 C25 C30 107(3) . . ? C26 C25 C30 109(3) . . ? N4 C25 H25 109.2 . . ? C26 C25 H25 109.2 . . ? C30 C25 H25 109.2 . . ? C25 C26 C27 109(3) . . ? C25 C26 H26A 110.0 . . ? C27 C26 H26A 110.0 . . ? C25 C26 H26B 110.0 . . ? C27 C26 H26B 110.0 . . ? H26A C26 H26B 108.3 . . ? C28 C27 C26 110(3) . . ? C28 C27 H27A 109.7 . . ? C26 C27 H27A 109.7 . . ? C28 C27 H27B 109.7 . . ? C26 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? C29 C28 C27 109(4) . . ? C29 C28 H28A 109.9 . . ? C27 C28 H28A 109.9 . . ? C29 C28 H28B 109.9 . . ? C27 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? C28 C29 C30 111(4) . . ? C28 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? C28 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C25 C30 C29 109(3) . . ? C25 C30 H30A 109.8 . . ? C29 C30 H30A 109.8 . . ? C25 C30 H30B 109.8 . . ? C29 C30 H30B 109.8 . . ? H30A C30 H30B 108.3 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 117(3) . . ? C33 C32 C31 123(4) . . ? C37 C32 C31 120(4) . . ? C33 C32 Ru2 67.5(18) . . ? C37 C32 Ru2 68(2) . . ? C31 C32 Ru2 129(2) . . ? C32 C33 C34 120(4) . . ? C32 C33 Ru2 75(2) . . ? C34 C33 Ru2 72(2) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? Ru2 C33 H33 124.8 . . ? C35 C34 C33 125(3) . . ? C35 C34 Ru2 78.8(19) . . ? C33 C34 Ru2 70(2) . . ? C35 C34 H34 117.7 . . ? C33 C34 H34 117.7 . . ? Ru2 C34 H34 125.4 . . ? C36 C35 C34 111(3) . . ? C36 C35 C38 124(4) . . ? C34 C35 C38 124(3) . . ? C36 C35 Ru2 64(2) . . ? C34 C35 Ru2 64.8(18) . . ? C38 C35 Ru2 133(3) . . ? C35 C36 C37 128(4) . . ? C35 C36 Ru2 82(2) . . ? C37 C36 Ru2 71(2) . . ? C35 C36 H36 115.9 . . ? C37 C36 H36 115.9 . . ? Ru2 C36 H36 121.9 . . ? C32 C37 C36 117(4) . . ? C32 C37 Ru2 74(2) . . ? C36 C37 Ru2 69(2) . . ? C32 C37 H37 121.5 . . ? C36 C37 H37 121.5 . . ? Ru2 C37 H37 127.2 . . ? C35 C38 C40 110(3) . . ? C35 C38 C39 115(4) . . ? C40 C38 C39 115(4) . . ? C35 C38 H38 105.1 . . ? C40 C38 H38 105.1 . . ? C39 C38 H38 105.1 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C2 C3 -4(5) . . . . ? C1 N1 C2 C3 173(3) . . . . ? N1 C2 C3 N2 5(5) . . . . ? C5 N2 C3 C2 179(4) . . . . ? C4 N2 C3 C2 -5(5) . . . . ? C2 N1 C4 N2 1(4) . . . . ? C1 N1 C4 N2 -176(3) . . . . ? C2 N1 C4 Ru1 173(3) . . . . ? C1 N1 C4 Ru1 -4(5) . . . . ? C3 N2 C4 N1 2(4) . . . . ? C5 N2 C4 N1 178(3) . . . . ? C3 N2 C4 Ru1 -170(3) . . . . ? C5 N2 C4 Ru1 7(4) . . . . ? C16 Ru1 C4 N1 -135(3) . . . . ? C13 Ru1 C4 N1 -45(3) . . . . ? C17 Ru1 C4 N1 -113(3) . . . . ? C14 Ru1 C4 N1 -36(4) . . . . ? C12 Ru1 C4 N1 -78(3) . . . . ? C15 Ru1 C4 N1 -112(4) . . . . ? I1 Ru1 C4 N1 138(3) . . . . ? I2 Ru1 C4 N1 54(3) . . . . ? C16 Ru1 C4 N2 34(3) . . . . ? C13 Ru1 C4 N2 124(3) . . . . ? C17 Ru1 C4 N2 56(3) . . . . ? C14 Ru1 C4 N2 133(3) . . . . ? C12 Ru1 C4 N2 91(3) . . . . ? C15 Ru1 C4 N2 58(5) . . . . ? I1 Ru1 C4 N2 -52(3) . . . . ? I2 Ru1 C4 N2 -136(3) . . . . ? C3 N2 C5 C10 -67(5) . . . . ? C4 N2 C5 C10 118(3) . . . . ? C3 N2 C5 C6 57(5) . . . . ? C4 N2 C5 C6 -119(3) . . . . ? N2 C5 C6 C7 179(3) . . . . ? C10 C5 C6 C7 -56(4) . . . . ? C5 C6 C7 C8 53(5) . . . . ? C6 C7 C8 C9 -55(6) . . . . ? C7 C8 C9 C10 59(6) . . . . ? N2 C5 C10 C9 -176(3) . . . . ? C6 C5 C10 C9 57(4) . . . . ? C8 C9 C10 C5 -60(5) . . . . ? C4 Ru1 C12 C17 -103(2) . . . . ? C16 Ru1 C12 C17 30(2) . . . . ? C13 Ru1 C12 C17 135(4) . . . . ? C14 Ru1 C12 C17 102(2) . . . . ? C15 Ru1 C12 C17 67(2) . . . . ? I1 Ru1 C12 C17 -11(3) . . . . ? I2 Ru1 C12 C17 167.5(15) . . . . ? C4 Ru1 C12 C13 122(2) . . . . ? C16 Ru1 C12 C13 -104(3) . . . . ? C17 Ru1 C12 C13 -135(4) . . . . ? C14 Ru1 C12 C13 -33(2) . . . . ? C15 Ru1 C12 C13 -68(2) . . . . ? I1 Ru1 C12 C13 -146.0(19) . . . . ? I2 Ru1 C12 C13 33(3) . . . . ? C4 Ru1 C12 C11 15(3) . . . . ? C16 Ru1 C12 C11 149(4) . . . . ? C13 Ru1 C12 C11 -107(4) . . . . ? C17 Ru1 C12 C11 118(4) . . . . ? C14 Ru1 C12 C11 -140(3) . . . . ? C15 Ru1 C12 C11 -175(3) . . . . ? I1 Ru1 C12 C11 107(3) . . . . ? I2 Ru1 C12 C11 -74(3) . . . . ? C17 C12 C13 C14 13(5) . . . . ? C11 C12 C13 C14 -175(3) . . . . ? Ru1 C12 C13 C14 61(3) . . . . ? C17 C12 C13 Ru1 -49(3) . . . . ? C11 C12 C13 Ru1 124(3) . . . . ? C4 Ru1 C13 C12 -61(3) . . . . ? C16 Ru1 C13 C12 65(2) . . . . ? C17 Ru1 C13 C12 27(2) . . . . ? C14 Ru1 C13 C12 127(3) . . . . ? C15 Ru1 C13 C12 101(2) . . . . ? I1 Ru1 C13 C12 108(3) . . . . ? I2 Ru1 C13 C12 -156(2) . . . . ? C4 Ru1 C13 C14 172(2) . . . . ? C16 Ru1 C13 C14 -63(2) . . . . ? C17 Ru1 C13 C14 -101(2) . . . . ? C12 Ru1 C13 C14 -127(3) . . . . ? C15 Ru1 C13 C14 -26.3(19) . . . . ? I1 Ru1 C13 C14 -19(5) . . . . ? I2 Ru1 C13 C14 77(2) . . . . ? C12 C13 C14 C15 -9(5) . . . . ? Ru1 C13 C14 C15 53(3) . . . . ? C12 C13 C14 Ru1 -62(3) . . . . ? C4 Ru1 C14 C15 -148(2) . . . . ? C16 Ru1 C14 C15 -28.9(18) . . . . ? C13 Ru1 C14 C15 -135(3) . . . . ? C17 Ru1 C14 C15 -67(2) . . . . ? C12 Ru1 C14 C15 -102(2) . . . . ? I1 Ru1 C14 C15 38(2) . . . . ? I2 Ru1 C14 C15 119.6(18) . . . . ? C4 Ru1 C14 C13 -14(3) . . . . ? C16 Ru1 C14 C13 106(2) . . . . ? C17 Ru1 C14 C13 68(2) . . . . ? C12 Ru1 C14 C13 32(2) . . . . ? C15 Ru1 C14 C13 135(3) . . . . ? I1 Ru1 C14 C13 172(2) . . . . ? I2 Ru1 C14 C13 -106(2) . . . . ? C13 C14 C15 C16 -2(5) . . . . ? Ru1 C14 C15 C16 48(3) . . . . ? C13 C14 C15 C18 -179(3) . . . . ? Ru1 C14 C15 C18 -129(3) . . . . ? C13 C14 C15 Ru1 -50(3) . . . . ? C4 Ru1 C15 C14 101(4) . . . . ? C16 Ru1 C15 C14 133(3) . . . . ? C13 Ru1 C15 C14 29(2) . . . . ? C17 Ru1 C15 C14 103(2) . . . . ? C12 Ru1 C15 C14 67(2) . . . . ? I1 Ru1 C15 C14 -148.1(19) . . . . ? I2 Ru1 C15 C14 -64.2(19) . . . . ? C4 Ru1 C15 C16 -32(5) . . . . ? C13 Ru1 C15 C16 -104(2) . . . . ? C17 Ru1 C15 C16 -30.3(18) . . . . ? C14 Ru1 C15 C16 -133(3) . . . . ? C12 Ru1 C15 C16 -65.5(19) . . . . ? I1 Ru1 C15 C16 78.9(17) . . . . ? I2 Ru1 C15 C16 162.8(17) . . . . ? C4 Ru1 C15 C18 -143(4) . . . . ? C16 Ru1 C15 C18 -111(4) . . . . ? C13 Ru1 C15 C18 145(4) . . . . ? C17 Ru1 C15 C18 -142(3) . . . . ? C14 Ru1 C15 C18 116(4) . . . . ? C12 Ru1 C15 C18 -177(3) . . . . ? I1 Ru1 C15 C18 -33(3) . . . . ? I2 Ru1 C15 C18 51(3) . . . . ? C14 C15 C16 C17 9(5) . . . . ? C18 C15 C16 C17 -174(3) . . . . ? Ru1 C15 C16 C17 60(3) . . . . ? C14 C15 C16 Ru1 -50(3) . . . . ? C18 C15 C16 Ru1 127(3) . . . . ? C4 Ru1 C16 C15 168.2(17) . . . . ? C13 Ru1 C16 C15 66(2) . . . . ? C17 Ru1 C16 C15 132(3) . . . . ? C14 Ru1 C16 C15 27.6(17) . . . . ? C12 Ru1 C16 C15 103(2) . . . . ? I1 Ru1 C16 C15 -100.0(17) . . . . ? I2 Ru1 C16 C15 -26(2) . . . . ? C4 Ru1 C16 C17 37(2) . . . . ? C13 Ru1 C16 C17 -66(2) . . . . ? C14 Ru1 C16 C17 -104(2) . . . . ? C12 Ru1 C16 C17 -28.1(18) . . . . ? C15 Ru1 C16 C17 -132(3) . . . . ? I1 Ru1 C16 C17 128.5(18) . . . . ? I2 Ru1 C16 C17 -157.6(14) . . . . ? C13 C12 C17 C16 -6(5) . . . . ? C11 C12 C17 C16 -178(3) . . . . ? Ru1 C12 C17 C16 -53(3) . . . . ? C13 C12 C17 Ru1 47(3) . . . . ? C11 C12 C17 Ru1 -125(3) . . . . ? C15 C16 C17 C12 -6(5) . . . . ? Ru1 C16 C17 C12 56(3) . . . . ? C15 C16 C17 Ru1 -62(3) . . . . ? C4 Ru1 C17 C12 77(2) . . . . ? C16 Ru1 C17 C12 -132(3) . . . . ? C13 Ru1 C17 C12 -28(2) . . . . ? C14 Ru1 C17 C12 -68(2) . . . . ? C15 Ru1 C17 C12 -103(2) . . . . ? I1 Ru1 C17 C12 173(2) . . . . ? I2 Ru1 C17 C12 -40(5) . . . . ? C4 Ru1 C17 C16 -151(2) . . . . ? C13 Ru1 C17 C16 103(2) . . . . ? C14 Ru1 C17 C16 63.9(19) . . . . ? C12 Ru1 C17 C16 132(3) . . . . ? C15 Ru1 C17 C16 29.0(18) . . . . ? I1 Ru1 C17 C16 -55.2(19) . . . . ? I2 Ru1 C17 C16 92(4) . . . . ? C14 C15 C18 C20 -127(4) . . . . ? C16 C15 C18 C20 56(5) . . . . ? Ru1 C15 C18 C20 141(3) . . . . ? C14 C15 C18 C19 9(5) . . . . ? C16 C15 C18 C19 -167(3) . . . . ? Ru1 C15 C18 C19 -83(4) . . . . ? C24 N3 C22 C23 -1(4) . . . . ? C21 N3 C22 C23 -176(3) . . . . ? N3 C22 C23 N4 2(4) . . . . ? C25 N4 C23 C22 177(3) . . . . ? C24 N4 C23 C22 -2(4) . . . . ? C22 N3 C24 N4 -1(3) . . . . ? C21 N3 C24 N4 174(3) . . . . ? C22 N3 C24 Ru2 -175(2) . . . . ? C21 N3 C24 Ru2 1(5) . . . . ? C23 N4 C24 N3 2(3) . . . . ? C25 N4 C24 N3 -178(3) . . . . ? C23 N4 C24 Ru2 176(2) . . . . ? C25 N4 C24 Ru2 -4(5) . . . . ? C36 Ru2 C24 N3 35(4) . . . . ? C33 Ru2 C24 N3 115(3) . . . . ? C34 Ru2 C24 N3 135(3) . . . . ? C37 Ru2 C24 N3 46(3) . . . . ? C32 Ru2 C24 N3 79(3) . . . . ? C35 Ru2 C24 N3 106(5) . . . . ? I3 Ru2 C24 N3 -138(3) . . . . ? I4 Ru2 C24 N3 -53(3) . . . . ? C36 Ru2 C24 N4 -137(2) . . . . ? C33 Ru2 C24 N4 -57(3) . . . . ? C34 Ru2 C24 N4 -37(3) . . . . ? C37 Ru2 C24 N4 -126(3) . . . . ? C32 Ru2 C24 N4 -93(3) . . . . ? C35 Ru2 C24 N4 -66(5) . . . . ? I3 Ru2 C24 N4 50(2) . . . . ? I4 Ru2 C24 N4 134(2) . . . . ? C23 N4 C25 C26 57(5) . . . . ? C24 N4 C25 C26 -124(3) . . . . ? C23 N4 C25 C30 -63(4) . . . . ? C24 N4 C25 C30 116(3) . . . . ? N4 C25 C26 C27 -179(3) . . . . ? C30 C25 C26 C27 -60(4) . . . . ? C25 C26 C27 C28 62(5) . . . . ? C26 C27 C28 C29 -61(5) . . . . ? C27 C28 C29 C30 60(5) . . . . ? N4 C25 C30 C29 -179(3) . . . . ? C26 C25 C30 C29 59(4) . . . . ? C28 C29 C30 C25 -59(5) . . . . ? C24 Ru2 C32 C33 105(2) . . . . ? C36 Ru2 C32 C33 -101(2) . . . . ? C34 Ru2 C32 C33 -31(2) . . . . ? C37 Ru2 C32 C33 -134(4) . . . . ? C35 Ru2 C32 C33 -67(2) . . . . ? I3 Ru2 C32 C33 13(3) . . . . ? I4 Ru2 C32 C33 -166.6(17) . . . . ? C24 Ru2 C32 C37 -121(3) . . . . ? C36 Ru2 C32 C37 33(2) . . . . ? C33 Ru2 C32 C37 134(4) . . . . ? C34 Ru2 C32 C37 103(3) . . . . ? C35 Ru2 C32 C37 67(2) . . . . ? I3 Ru2 C32 C37 147(2) . . . . ? I4 Ru2 C32 C37 -33(3) . . . . ? C24 Ru2 C32 C31 -9(4) . . . . ? C36 Ru2 C32 C31 144(5) . . . . ? C33 Ru2 C32 C31 -115(5) . . . . ? C34 Ru2 C32 C31 -146(5) . . . . ? C37 Ru2 C32 C31 112(6) . . . . ? C35 Ru2 C32 C31 178(5) . . . . ? I3 Ru2 C32 C31 -102(4) . . . . ? I4 Ru2 C32 C31 79(5) . . . . ? C37 C32 C33 C34 9(5) . . . . ? C31 C32 C33 C34 -179(3) . . . . ? Ru2 C32 C33 C34 58(3) . . . . ? C37 C32 C33 Ru2 -49(3) . . . . ? C31 C32 C33 Ru2 123(3) . . . . ? C24 Ru2 C33 C32 -75(2) . . . . ? C36 Ru2 C33 C32 68(2) . . . . ? C34 Ru2 C33 C32 129(3) . . . . ? C37 Ru2 C33 C32 28(2) . . . . ? C35 Ru2 C33 C32 102(2) . . . . ? I3 Ru2 C33 C32 -172(2) . . . . ? I4 Ru2 C33 C32 47(5) . . . . ? C24 Ru2 C33 C34 155(2) . . . . ? C36 Ru2 C33 C34 -61(2) . . . . ? C37 Ru2 C33 C34 -101(2) . . . . ? C32 Ru2 C33 C34 -129(3) . . . . ? C35 Ru2 C33 C34 -28(2) . . . . ? I3 Ru2 C33 C34 59(2) . . . . ? I4 Ru2 C33 C34 -82(5) . . . . ? C32 C33 C34 C35 0(5) . . . . ? Ru2 C33 C34 C35 60(3) . . . . ? C32 C33 C34 Ru2 -60(3) . . . . ? C24 Ru2 C34 C35 -166.7(19) . . . . ? C36 Ru2 C34 C35 -27.4(19) . . . . ? C33 Ru2 C34 C35 -134(3) . . . . ? C37 Ru2 C34 C35 -66(2) . . . . ? C32 Ru2 C34 C35 -103(2) . . . . ? I3 Ru2 C34 C35 102(2) . . . . ? I4 Ru2 C34 C35 26(3) . . . . ? C24 Ru2 C34 C33 -33(3) . . . . ? C36 Ru2 C34 C33 106(2) . . . . ? C37 Ru2 C34 C33 68(2) . . . . ? C32 Ru2 C34 C33 30(2) . . . . ? C35 Ru2 C34 C33 134(3) . . . . ? I3 Ru2 C34 C33 -124(2) . . . . ? I4 Ru2 C34 C33 159.7(16) . . . . ? C33 C34 C35 C36 -10(5) . . . . ? Ru2 C34 C35 C36 45(3) . . . . ? C33 C34 C35 C38 179(3) . . . . ? Ru2 C34 C35 C38 -126(3) . . . . ? C33 C34 C35 Ru2 -56(3) . . . . ? C24 Ru2 C35 C36 -93(5) . . . . ? C33 Ru2 C35 C36 -104(2) . . . . ? C34 Ru2 C35 C36 -133(3) . . . . ? C37 Ru2 C35 C36 -29(2) . . . . ? C32 Ru2 C35 C36 -66(2) . . . . ? I3 Ru2 C35 C36 150(2) . . . . ? I4 Ru2 C35 C36 65(2) . . . . ? C24 Ru2 C35 C34 39(5) . . . . ? C36 Ru2 C35 C34 133(3) . . . . ? C33 Ru2 C35 C34 29(2) . . . . ? C37 Ru2 C35 C34 103(2) . . . . ? C32 Ru2 C35 C34 66(2) . . . . ? I3 Ru2 C35 C34 -77(2) . . . . ? I4 Ru2 C35 C34 -162.2(19) . . . . ? C24 Ru2 C35 C38 153(4) . . . . ? C36 Ru2 C35 C38 -113(4) . . . . ? C33 Ru2 C35 C38 143(4) . . . . ? C34 Ru2 C35 C38 114(4) . . . . ? C37 Ru2 C35 C38 -142(4) . . . . ? C32 Ru2 C35 C38 -180(4) . . . . ? I3 Ru2 C35 C38 37(4) . . . . ? I4 Ru2 C35 C38 -48(4) . . . . ? C34 C35 C36 C37 13(5) . . . . ? C38 C35 C36 C37 -176(3) . . . . ? Ru2 C35 C36 C37 58(3) . . . . ? C34 C35 C36 Ru2 -46(3) . . . . ? C38 C35 C36 Ru2 125(3) . . . . ? C24 Ru2 C36 C35 152(2) . . . . ? C33 Ru2 C36 C35 67(2) . . . . ? C34 Ru2 C36 C35 29(2) . . . . ? C37 Ru2 C36 C35 135(3) . . . . ? C32 Ru2 C36 C35 104(3) . . . . ? I3 Ru2 C36 C35 -35(2) . . . . ? I4 Ru2 C36 C35 -118(2) . . . . ? C24 Ru2 C36 C37 17(3) . . . . ? C33 Ru2 C36 C37 -68(2) . . . . ? C34 Ru2 C36 C37 -106(2) . . . . ? C32 Ru2 C36 C37 -31(2) . . . . ? C35 Ru2 C36 C37 -135(3) . . . . ? I3 Ru2 C36 C37 -170.5(19) . . . . ? I4 Ru2 C36 C37 107(2) . . . . ? C33 C32 C37 C36 -7(5) . . . . ? C31 C32 C37 C36 -179(3) . . . . ? Ru2 C32 C37 C36 -56(3) . . . . ? C33 C32 C37 Ru2 48(3) . . . . ? C31 C32 C37 Ru2 -123(3) . . . . ? C35 C36 C37 C32 -4(6) . . . . ? Ru2 C36 C37 C32 58(3) . . . . ? C35 C36 C37 Ru2 -63(4) . . . . ? C24 Ru2 C37 C32 63(3) . . . . ? C36 Ru2 C37 C32 -128(3) . . . . ? C33 Ru2 C37 C32 -28(2) . . . . ? C34 Ru2 C37 C32 -66(2) . . . . ? C35 Ru2 C37 C32 -102(3) . . . . ? I3 Ru2 C37 C32 -104(4) . . . . ? I4 Ru2 C37 C32 156(2) . . . . ? C24 Ru2 C37 C36 -170(2) . . . . ? C33 Ru2 C37 C36 100(2) . . . . ? C34 Ru2 C37 C36 61(2) . . . . ? C32 Ru2 C37 C36 128(3) . . . . ? C35 Ru2 C37 C36 26(2) . . . . ? I3 Ru2 C37 C36 24(5) . . . . ? I4 Ru2 C37 C36 -76(2) . . . . ? C36 C35 C38 C40 123(4) . . . . ? C34 C35 C38 C40 -68(5) . . . . ? Ru2 C35 C38 C40 -153(3) . . . . ? C36 C35 C38 C39 -9(5) . . . . ? C34 C35 C38 C39 160(3) . . . . ? Ru2 C35 C38 C39 75(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.731 _refine_diff_density_min -1.706 _refine_diff_density_rms 0.242 # Attachment 'Dalton_ZhangCY.cif' data_R071122b _database_code_depnum_ccdc_archive 'CCDC 705186' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H23 I N2 Ru' _chemical_formula_sum 'C20 H23 I N2 Ru' _chemical_formula_weight 519.37 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y, z+1/2' _cell_length_a 7.729(3) _cell_length_b 14.184(6) _cell_length_c 17.532(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1922.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5708 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 2.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9092 _exptl_absorpt_correction_T_max 0.9531 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22777 _diffrn_reflns_av_R_equivalents 0.1006 _diffrn_reflns_av_sigmaI/netI 0.0933 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.86 _reflns_number_total 4572 _reflns_number_gt 4154 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0314P)^2^+2.2112P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.34(4) _refine_ls_number_reflns 4572 _refine_ls_number_parameters 223 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1277 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.55481(8) 0.53137(4) 0.22764(4) 0.02361(14) Uani 1 1 d . . . I1 I 0.84740(7) 0.51306(4) 0.31276(4) 0.03025(14) Uani 1 1 d . . . N1 N 0.5468(10) 0.3267(5) 0.2178(5) 0.0353(18) Uani 1 1 d . . . N2 N 0.4134(9) 0.3565(5) 0.3203(5) 0.0310(15) Uani 1 1 d . . . C1 C 0.5195(12) 0.7032(7) 0.3702(6) 0.038(2) Uani 1 1 d . . . H1A H 0.4901 0.7703 0.3737 0.056 Uiso 1 1 calc R . . H1B H 0.6439 0.6950 0.3785 0.056 Uiso 1 1 calc R . . H1C H 0.4552 0.6680 0.4090 0.056 Uiso 1 1 calc R . . C2 C 0.4713(10) 0.6663(6) 0.2909(5) 0.0267(19) Uani 1 1 d . . . C3 C 0.3266(10) 0.6095(6) 0.2767(5) 0.0284(18) Uani 1 1 d . . . H3 H 0.2662 0.5809 0.3215 0.034 Uiso 1 1 calc R . . C4 C 0.2893(11) 0.5724(6) 0.2036(5) 0.0263(17) Uani 1 1 d . . . H4 H 0.1983 0.5227 0.1980 0.032 Uiso 1 1 calc R . . C5 C 0.3925(12) 0.5977(6) 0.1394(5) 0.0309(18) Uani 1 1 d . . . C6 C 0.5357(10) 0.6590(5) 0.1545(5) 0.0257(17) Uani 1 1 d . . . H6 H 0.6241 0.6678 0.1135 0.031 Uiso 1 1 calc R . . C7 C 0.5767(11) 0.6892(6) 0.2280(6) 0.0316(17) Uani 1 1 d . . . H7 H 0.6924 0.7186 0.2374 0.038 Uiso 1 1 calc R . . C8 C 0.3529(13) 0.5672(7) 0.0593(6) 0.041(2) Uani 1 1 d . . . H8 H 0.4645 0.5657 0.0304 0.049 Uiso 1 1 calc R . . C9 C 0.2755(15) 0.4702(7) 0.0555(6) 0.043(2) Uani 1 1 d . . . H9A H 0.3592 0.4241 0.0747 0.064 Uiso 1 1 calc R . . H9B H 0.2461 0.4551 0.0025 0.064 Uiso 1 1 calc R . . H9C H 0.1705 0.4681 0.0869 0.064 Uiso 1 1 calc R . . C10 C 0.2352(17) 0.6411(8) 0.0210(6) 0.063(4) Uani 1 1 d . . . H10A H 0.2137 0.6228 -0.0321 0.095 Uiso 1 1 calc R . . H10B H 0.2920 0.7028 0.0222 0.095 Uiso 1 1 calc R . . H10C H 0.1250 0.6446 0.0485 0.095 Uiso 1 1 calc R . . C11 C 0.6719(10) 0.4489(7) 0.1458(5) 0.0292(18) Uani 1 1 d . . . C12 C 0.7714(13) 0.4766(8) 0.0835(6) 0.040(2) Uani 1 1 d . . . H12 H 0.7982 0.5416 0.0777 0.048 Uiso 1 1 calc R . . C13 C 0.8337(13) 0.4127(11) 0.0289(6) 0.056(4) Uani 1 1 d . . . H13 H 0.8993 0.4347 -0.0133 0.068 Uiso 1 1 calc R . . C14 C 0.7986(13) 0.3156(9) 0.0369(6) 0.052(3) Uani 1 1 d . . . H14 H 0.8378 0.2720 -0.0004 0.063 Uiso 1 1 calc R . . C15 C 0.7048(13) 0.2840(8) 0.1007(5) 0.042(2) Uani 1 1 d . . . H15 H 0.6833 0.2188 0.1085 0.051 Uiso 1 1 calc R . . C16 C 0.6447(11) 0.3507(6) 0.1521(5) 0.0312(19) Uani 1 1 d . . . C17 C 0.4974(13) 0.2400(7) 0.2462(6) 0.042(3) Uani 1 1 d . . . H17 H 0.5182 0.1797 0.2244 0.051 Uiso 1 1 calc R . . C18 C 0.4131(12) 0.2597(6) 0.3119(7) 0.039(2) Uani 1 1 d . . . H18 H 0.3631 0.2153 0.3459 0.047 Uiso 1 1 calc R . . C19 C 0.4942(11) 0.3994(6) 0.2590(5) 0.0288(18) Uani 1 1 d . . . C20 C 0.3345(13) 0.4035(7) 0.3851(6) 0.040(2) Uani 1 1 d . . . H20A H 0.4046 0.4582 0.3995 0.060 Uiso 1 1 calc R . . H20B H 0.3280 0.3596 0.4281 0.060 Uiso 1 1 calc R . . H20C H 0.2177 0.4243 0.3713 0.060 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 0.0229(3) 0.0221(3) 0.0259(3) -0.0010(3) 0.0007(3) -0.0004(2) I1 0.0249(3) 0.0307(3) 0.0352(3) -0.0015(3) -0.0025(2) 0.0013(2) N1 0.035(4) 0.028(4) 0.043(5) -0.005(4) -0.013(3) 0.000(3) N2 0.027(3) 0.023(3) 0.043(4) 0.005(4) -0.006(3) -0.007(3) C1 0.040(5) 0.028(5) 0.044(5) -0.006(4) -0.011(4) 0.006(4) C2 0.017(4) 0.023(4) 0.041(5) -0.011(3) -0.008(3) 0.012(3) C3 0.022(4) 0.022(4) 0.042(5) -0.005(4) 0.010(4) -0.001(3) C4 0.025(4) 0.020(4) 0.034(4) -0.001(3) -0.004(3) -0.002(3) C5 0.045(5) 0.024(4) 0.024(4) 0.001(4) -0.006(4) 0.006(4) C6 0.028(4) 0.019(4) 0.030(4) 0.005(3) 0.009(3) -0.004(3) C7 0.034(4) 0.024(4) 0.037(4) 0.000(5) 0.002(4) -0.010(3) C8 0.049(6) 0.022(4) 0.051(6) -0.003(4) -0.018(5) 0.008(4) C9 0.042(6) 0.043(6) 0.044(6) -0.014(5) -0.011(5) 0.005(5) C10 0.091(9) 0.056(7) 0.043(6) 0.000(6) -0.034(6) 0.028(8) C11 0.025(4) 0.033(5) 0.029(4) -0.004(4) -0.007(3) 0.008(3) C12 0.032(5) 0.059(7) 0.029(5) -0.005(4) 0.000(4) 0.005(5) C13 0.033(6) 0.110(12) 0.026(5) 0.001(6) -0.002(4) 0.006(6) C14 0.039(6) 0.075(9) 0.044(6) -0.022(6) -0.009(5) 0.017(6) C15 0.048(6) 0.040(6) 0.039(5) -0.019(4) -0.010(5) 0.014(5) C16 0.031(5) 0.028(5) 0.035(5) -0.014(4) -0.005(4) 0.005(4) C17 0.036(5) 0.022(5) 0.069(8) -0.005(5) -0.015(5) -0.003(4) C18 0.036(5) 0.025(4) 0.055(6) 0.006(5) -0.015(5) -0.005(3) C19 0.033(5) 0.014(4) 0.040(4) -0.001(3) -0.010(4) 0.000(3) C20 0.046(6) 0.031(5) 0.043(6) 0.012(4) -0.001(4) -0.010(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 C19 2.006(8) . ? Ru1 C11 2.061(9) . ? Ru1 C4 2.175(8) . ? Ru1 C5 2.203(8) . ? Ru1 C6 2.223(8) . ? Ru1 C7 2.245(8) . ? Ru1 C3 2.253(8) . ? Ru1 C2 2.304(8) . ? Ru1 I1 2.7218(12) . ? N1 C19 1.323(11) . ? N1 C17 1.382(12) . ? N1 C16 1.420(12) . ? N2 C18 1.382(10) . ? N2 C19 1.384(11) . ? N2 C20 1.450(12) . ? C1 C2 1.531(12) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.401(11) . ? C2 C7 1.409(13) . ? C3 C4 1.415(11) . ? C3 H3 1.0000 . ? C4 C5 1.425(12) . ? C4 H4 1.0000 . ? C5 C6 1.432(12) . ? C5 C8 1.501(12) . ? C6 C7 1.395(13) . ? C6 H6 1.0000 . ? C7 H7 1.0000 . ? C8 C9 1.502(13) . ? C8 C10 1.542(13) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.392(13) . ? C11 C16 1.413(13) . ? C12 C13 1.404(15) . ? C12 H12 0.9500 . ? C13 C14 1.410(18) . ? C13 H13 0.9500 . ? C14 C15 1.406(14) . ? C14 H14 0.9500 . ? C15 C16 1.386(11) . ? C15 H15 0.9500 . ? C17 C18 1.352(15) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 Ru1 C11 76.3(4) . . ? C19 Ru1 C4 94.7(3) . . ? C11 Ru1 C4 115.5(3) . . ? C19 Ru1 C5 117.2(3) . . ? C11 Ru1 C5 90.2(3) . . ? C4 Ru1 C5 38.0(3) . . ? C19 Ru1 C6 154.4(3) . . ? C11 Ru1 C6 95.1(3) . . ? C4 Ru1 C6 66.9(3) . . ? C5 Ru1 C6 37.8(3) . . ? C19 Ru1 C7 161.3(4) . . ? C11 Ru1 C7 122.3(4) . . ? C4 Ru1 C7 78.8(3) . . ? C5 Ru1 C7 67.6(3) . . ? C6 Ru1 C7 36.4(3) . . ? C19 Ru1 C3 99.9(3) . . ? C11 Ru1 C3 152.7(3) . . ? C4 Ru1 C3 37.2(3) . . ? C5 Ru1 C3 67.2(3) . . ? C6 Ru1 C3 76.6(3) . . ? C7 Ru1 C3 64.4(3) . . ? C19 Ru1 C2 125.3(4) . . ? C11 Ru1 C2 158.4(4) . . ? C4 Ru1 C2 66.9(3) . . ? C5 Ru1 C2 79.9(3) . . ? C6 Ru1 C2 65.4(3) . . ? C7 Ru1 C2 36.1(3) . . ? C3 Ru1 C2 35.8(3) . . ? C19 Ru1 I1 87.4(2) . . ? C11 Ru1 I1 87.9(2) . . ? C4 Ru1 I1 156.4(2) . . ? C5 Ru1 I1 154.0(2) . . ? C6 Ru1 I1 116.7(2) . . ? C7 Ru1 I1 91.8(2) . . ? C3 Ru1 I1 119.2(2) . . ? C2 Ru1 I1 92.75(19) . . ? C19 N1 C17 114.4(9) . . ? C19 N1 C16 114.8(8) . . ? C17 N1 C16 130.8(9) . . ? C18 N2 C19 110.8(8) . . ? C18 N2 C20 122.6(8) . . ? C19 N2 C20 126.6(7) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 117.0(8) . . ? C3 C2 C1 123.6(8) . . ? C7 C2 C1 119.4(8) . . ? C3 C2 Ru1 70.1(5) . . ? C7 C2 Ru1 69.7(5) . . ? C1 C2 Ru1 130.8(6) . . ? C2 C3 C4 122.6(8) . . ? C2 C3 Ru1 74.1(5) . . ? C4 C3 Ru1 68.4(5) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? Ru1 C3 H3 117.7 . . ? C3 C4 C5 120.5(8) . . ? C3 C4 Ru1 74.4(5) . . ? C5 C4 Ru1 72.1(5) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? Ru1 C4 H4 119.6 . . ? C4 C5 C6 116.1(8) . . ? C4 C5 C8 123.5(9) . . ? C6 C5 C8 120.4(8) . . ? C4 C5 Ru1 69.9(5) . . ? C6 C5 Ru1 71.9(5) . . ? C8 C5 Ru1 130.6(6) . . ? C7 C6 C5 122.2(7) . . ? C7 C6 Ru1 72.7(5) . . ? C5 C6 Ru1 70.3(5) . . ? C7 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? Ru1 C6 H6 118.1 . . ? C6 C7 C2 121.4(8) . . ? C6 C7 Ru1 71.0(5) . . ? C2 C7 Ru1 74.2(5) . . ? C6 C7 H7 118.9 . . ? C2 C7 H7 118.9 . . ? Ru1 C7 H7 118.9 . . ? C9 C8 C5 112.7(9) . . ? C9 C8 C10 111.6(9) . . ? C5 C8 C10 109.4(8) . . ? C9 C8 H8 107.6 . . ? C5 C8 H8 107.6 . . ? C10 C8 H8 107.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 114.9(9) . . ? C12 C11 Ru1 129.0(7) . . ? C16 C11 Ru1 116.1(7) . . ? C11 C12 C13 122.8(10) . . ? C11 C12 H12 118.6 . . ? C13 C12 H12 118.6 . . ? C12 C13 C14 119.8(10) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 119.3(10) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C16 C15 C14 118.2(10) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C15 C16 C11 124.9(10) . . ? C15 C16 N1 122.8(9) . . ? C11 C16 N1 112.3(7) . . ? C18 C17 N1 104.8(9) . . ? C18 C17 H17 127.6 . . ? N1 C17 H17 127.6 . . ? C17 C18 N2 107.2(9) . . ? C17 C18 H18 126.4 . . ? N2 C18 H18 126.4 . . ? N1 C19 N2 102.7(7) . . ? N1 C19 Ru1 120.4(7) . . ? N2 C19 Ru1 136.7(6) . . ? N2 C20 H20A 109.5 . . ? N2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 Ru1 C2 C3 -51.5(7) . . . . ? C11 Ru1 C2 C3 128.6(8) . . . . ? C4 Ru1 C2 C3 27.4(5) . . . . ? C5 Ru1 C2 C3 64.8(6) . . . . ? C6 Ru1 C2 C3 101.5(6) . . . . ? C7 Ru1 C2 C3 130.5(8) . . . . ? I1 Ru1 C2 C3 -140.3(5) . . . . ? C19 Ru1 C2 C7 178.0(5) . . . . ? C11 Ru1 C2 C7 -1.9(10) . . . . ? C4 Ru1 C2 C7 -103.1(6) . . . . ? C5 Ru1 C2 C7 -65.7(6) . . . . ? C6 Ru1 C2 C7 -29.0(5) . . . . ? C3 Ru1 C2 C7 -130.5(8) . . . . ? I1 Ru1 C2 C7 89.2(5) . . . . ? C19 Ru1 C2 C1 66.2(9) . . . . ? C11 Ru1 C2 C1 -113.7(10) . . . . ? C4 Ru1 C2 C1 145.1(9) . . . . ? C5 Ru1 C2 C1 -177.5(9) . . . . ? C6 Ru1 C2 C1 -140.8(9) . . . . ? C7 Ru1 C2 C1 -111.8(10) . . . . ? C3 Ru1 C2 C1 117.7(11) . . . . ? I1 Ru1 C2 C1 -22.6(8) . . . . ? C7 C2 C3 C4 2.8(12) . . . . ? C1 C2 C3 C4 -176.9(8) . . . . ? Ru1 C2 C3 C4 -50.4(7) . . . . ? C7 C2 C3 Ru1 53.2(7) . . . . ? C1 C2 C3 Ru1 -126.4(8) . . . . ? C19 Ru1 C3 C2 139.6(6) . . . . ? C11 Ru1 C3 C2 -141.1(7) . . . . ? C4 Ru1 C3 C2 -135.7(8) . . . . ? C5 Ru1 C3 C2 -104.9(6) . . . . ? C6 Ru1 C3 C2 -66.3(5) . . . . ? C7 Ru1 C3 C2 -29.8(5) . . . . ? I1 Ru1 C3 C2 47.0(6) . . . . ? C19 Ru1 C3 C4 -84.8(5) . . . . ? C11 Ru1 C3 C4 -5.5(10) . . . . ? C5 Ru1 C3 C4 30.7(5) . . . . ? C6 Ru1 C3 C4 69.4(5) . . . . ? C7 Ru1 C3 C4 105.9(6) . . . . ? C2 Ru1 C3 C4 135.7(8) . . . . ? I1 Ru1 C3 C4 -177.3(4) . . . . ? C2 C3 C4 C5 -4.8(13) . . . . ? Ru1 C3 C4 C5 -57.6(7) . . . . ? C2 C3 C4 Ru1 52.9(7) . . . . ? C19 Ru1 C4 C3 100.1(5) . . . . ? C11 Ru1 C4 C3 177.2(5) . . . . ? C5 Ru1 C4 C3 -130.1(7) . . . . ? C6 Ru1 C4 C3 -98.3(5) . . . . ? C7 Ru1 C4 C3 -62.2(5) . . . . ? C2 Ru1 C4 C3 -26.4(5) . . . . ? I1 Ru1 C4 C3 5.8(9) . . . . ? C19 Ru1 C4 C5 -129.8(5) . . . . ? C11 Ru1 C4 C5 -52.7(6) . . . . ? C6 Ru1 C4 C5 31.8(5) . . . . ? C7 Ru1 C4 C5 67.9(5) . . . . ? C3 Ru1 C4 C5 130.1(7) . . . . ? C2 Ru1 C4 C5 103.7(6) . . . . ? I1 Ru1 C4 C5 135.8(5) . . . . ? C3 C4 C5 C6 1.9(12) . . . . ? Ru1 C4 C5 C6 -56.9(7) . . . . ? C3 C4 C5 C8 -175.2(8) . . . . ? Ru1 C4 C5 C8 126.1(9) . . . . ? C3 C4 C5 Ru1 58.8(7) . . . . ? C19 Ru1 C5 C4 59.4(6) . . . . ? C11 Ru1 C5 C4 134.1(5) . . . . ? C6 Ru1 C5 C4 -127.7(7) . . . . ? C7 Ru1 C5 C4 -100.6(5) . . . . ? C3 Ru1 C5 C4 -30.2(5) . . . . ? C2 Ru1 C5 C4 -65.2(5) . . . . ? I1 Ru1 C5 C4 -140.4(5) . . . . ? C19 Ru1 C5 C6 -172.9(5) . . . . ? C11 Ru1 C5 C6 -98.2(5) . . . . ? C4 Ru1 C5 C6 127.7(7) . . . . ? C7 Ru1 C5 C6 27.1(5) . . . . ? C3 Ru1 C5 C6 97.5(5) . . . . ? C2 Ru1 C5 C6 62.5(5) . . . . ? I1 Ru1 C5 C6 -12.7(8) . . . . ? C19 Ru1 C5 C8 -58.0(10) . . . . ? C11 Ru1 C5 C8 16.7(9) . . . . ? C4 Ru1 C5 C8 -117.4(11) . . . . ? C6 Ru1 C5 C8 114.9(11) . . . . ? C7 Ru1 C5 C8 141.9(10) . . . . ? C3 Ru1 C5 C8 -147.6(10) . . . . ? C2 Ru1 C5 C8 177.4(10) . . . . ? I1 Ru1 C5 C8 102.2(9) . . . . ? C4 C5 C6 C7 2.6(12) . . . . ? C8 C5 C6 C7 179.8(8) . . . . ? Ru1 C5 C6 C7 -53.2(8) . . . . ? C4 C5 C6 Ru1 55.8(7) . . . . ? C8 C5 C6 Ru1 -127.0(8) . . . . ? C19 Ru1 C6 C7 149.6(8) . . . . ? C11 Ru1 C6 C7 -141.6(5) . . . . ? C4 Ru1 C6 C7 102.8(6) . . . . ? C5 Ru1 C6 C7 134.8(7) . . . . ? C3 Ru1 C6 C7 64.8(5) . . . . ? C2 Ru1 C6 C7 28.7(5) . . . . ? I1 Ru1 C6 C7 -51.4(5) . . . . ? C19 Ru1 C6 C5 14.8(10) . . . . ? C11 Ru1 C6 C5 83.6(5) . . . . ? C4 Ru1 C6 C5 -32.0(5) . . . . ? C7 Ru1 C6 C5 -134.8(7) . . . . ? C3 Ru1 C6 C5 -70.0(5) . . . . ? C2 Ru1 C6 C5 -106.1(5) . . . . ? I1 Ru1 C6 C5 173.8(4) . . . . ? C5 C6 C7 C2 -4.7(13) . . . . ? Ru1 C6 C7 C2 -56.8(8) . . . . ? C5 C6 C7 Ru1 52.2(7) . . . . ? C3 C2 C7 C6 1.8(12) . . . . ? C1 C2 C7 C6 -178.5(8) . . . . ? Ru1 C2 C7 C6 55.3(7) . . . . ? C3 C2 C7 Ru1 -53.4(7) . . . . ? C1 C2 C7 Ru1 126.2(7) . . . . ? C19 Ru1 C7 C6 -137.1(10) . . . . ? C11 Ru1 C7 C6 47.1(6) . . . . ? C4 Ru1 C7 C6 -66.1(5) . . . . ? C5 Ru1 C7 C6 -28.0(5) . . . . ? C3 Ru1 C7 C6 -102.5(6) . . . . ? C2 Ru1 C7 C6 -132.1(8) . . . . ? I1 Ru1 C7 C6 135.7(5) . . . . ? C19 Ru1 C7 C2 -5.0(13) . . . . ? C11 Ru1 C7 C2 179.2(5) . . . . ? C4 Ru1 C7 C2 65.9(5) . . . . ? C5 Ru1 C7 C2 104.0(6) . . . . ? C6 Ru1 C7 C2 132.1(8) . . . . ? C3 Ru1 C7 C2 29.6(5) . . . . ? I1 Ru1 C7 C2 -92.2(5) . . . . ? C4 C5 C8 C9 -34.7(13) . . . . ? C6 C5 C8 C9 148.3(9) . . . . ? Ru1 C5 C8 C9 56.7(12) . . . . ? C4 C5 C8 C10 90.1(11) . . . . ? C6 C5 C8 C10 -86.9(12) . . . . ? Ru1 C5 C8 C10 -178.5(8) . . . . ? C19 Ru1 C11 C12 -179.5(9) . . . . ? C4 Ru1 C11 C12 91.8(9) . . . . ? C5 Ru1 C11 C12 62.5(9) . . . . ? C6 Ru1 C11 C12 25.0(9) . . . . ? C7 Ru1 C11 C12 -0.9(10) . . . . ? C3 Ru1 C11 C12 95.5(11) . . . . ? C2 Ru1 C11 C12 0.4(14) . . . . ? I1 Ru1 C11 C12 -91.6(8) . . . . ? C19 Ru1 C11 C16 2.3(6) . . . . ? C4 Ru1 C11 C16 -86.4(7) . . . . ? C5 Ru1 C11 C16 -115.7(7) . . . . ? C6 Ru1 C11 C16 -153.2(6) . . . . ? C7 Ru1 C11 C16 -179.1(6) . . . . ? C3 Ru1 C11 C16 -82.7(10) . . . . ? C2 Ru1 C11 C16 -177.8(6) . . . . ? I1 Ru1 C11 C16 90.2(6) . . . . ? C16 C11 C12 C13 2.8(14) . . . . ? Ru1 C11 C12 C13 -175.4(7) . . . . ? C11 C12 C13 C14 -1.2(16) . . . . ? C12 C13 C14 C15 -1.5(15) . . . . ? C13 C14 C15 C16 2.4(14) . . . . ? C14 C15 C16 C11 -0.7(14) . . . . ? C14 C15 C16 N1 179.1(8) . . . . ? C12 C11 C16 C15 -1.9(13) . . . . ? Ru1 C11 C16 C15 176.6(7) . . . . ? C12 C11 C16 N1 178.3(8) . . . . ? Ru1 C11 C16 N1 -3.2(9) . . . . ? C19 N1 C16 C15 -177.5(8) . . . . ? C17 N1 C16 C15 2.8(15) . . . . ? C19 N1 C16 C11 2.3(11) . . . . ? C17 N1 C16 C11 -177.4(9) . . . . ? C19 N1 C17 C18 -2.5(11) . . . . ? C16 N1 C17 C18 177.3(8) . . . . ? N1 C17 C18 N2 0.5(10) . . . . ? C19 N2 C18 C17 1.5(10) . . . . ? C20 N2 C18 C17 -179.7(8) . . . . ? C17 N1 C19 N2 3.3(10) . . . . ? C16 N1 C19 N2 -176.5(7) . . . . ? C17 N1 C19 Ru1 179.4(6) . . . . ? C16 N1 C19 Ru1 -0.4(10) . . . . ? C18 N2 C19 N1 -2.9(9) . . . . ? C20 N2 C19 N1 178.4(8) . . . . ? C18 N2 C19 Ru1 -178.0(7) . . . . ? C20 N2 C19 Ru1 3.3(14) . . . . ? C11 Ru1 C19 N1 -1.1(7) . . . . ? C4 Ru1 C19 N1 114.1(7) . . . . ? C5 Ru1 C19 N1 82.0(8) . . . . ? C6 Ru1 C19 N1 71.8(11) . . . . ? C7 Ru1 C19 N1 -177.4(9) . . . . ? C3 Ru1 C19 N1 151.3(7) . . . . ? C2 Ru1 C19 N1 179.0(6) . . . . ? I1 Ru1 C19 N1 -89.5(7) . . . . ? C11 Ru1 C19 N2 173.4(10) . . . . ? C4 Ru1 C19 N2 -71.5(9) . . . . ? C5 Ru1 C19 N2 -103.6(9) . . . . ? C6 Ru1 C19 N2 -113.7(10) . . . . ? C7 Ru1 C19 N2 -3.0(17) . . . . ? C3 Ru1 C19 N2 -34.3(9) . . . . ? C2 Ru1 C19 N2 -6.6(11) . . . . ? I1 Ru1 C19 N2 84.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.318 _refine_diff_density_min -1.421 _refine_diff_density_rms 0.169 #===END data_r080210b _database_code_depnum_ccdc_archive 'CCDC 705187' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H30 I2 N2 Ru' _chemical_formula_weight 641.32 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.7376(17) _cell_length_b 14.070(3) _cell_length_c 17.591(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.91(3) _cell_angle_gamma 90.00 _cell_volume 2130.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6441 _cell_measurement_theta_min 1.175 _cell_measurement_theta_max 27.904 _exptl_crystal_description block _exptl_crystal_colour black-red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 3.638 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7595 _exptl_absorpt_correction_T_max 0.8681 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 15091 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.88 _reflns_number_total 5063 _reflns_number_gt 4312 _reflns_threshold_expression >2sigma(I) _computing_data_collection crystalclear _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _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^)+(0.0185P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5063 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0455 _refine_ls_wR_factor_gt 0.0445 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.33855(2) 0.017291(12) 0.711715(10) 0.00913(5) Uani 1 1 d . . . I1 I 0.445451(18) -0.110163(10) 0.827386(8) 0.01359(5) Uani 1 1 d . . . I2 I 0.512915(18) -0.089744(10) 0.628096(8) 0.01464(5) Uani 1 1 d . . . N1 N 0.5640(2) 0.15333(13) 0.81893(11) 0.0132(4) Uani 1 1 d . . . N2 N 0.6060(2) 0.16451(13) 0.70257(10) 0.0127(4) Uani 1 1 d . . . C1 C 0.2212(3) 0.08981(17) 0.52698(14) 0.0199(5) Uani 1 1 d . . . H1A H 0.2590 0.1538 0.5262 0.030 Uiso 1 1 calc R . . H1B H 0.1285 0.0832 0.4892 0.030 Uiso 1 1 calc R . . H1C H 0.2989 0.0466 0.5153 0.030 Uiso 1 1 calc R . . C2 C 0.1855(3) 0.06770(16) 0.60559(13) 0.0147(5) Uani 1 1 d . . . C3 C 0.1931(3) 0.13627(16) 0.66416(13) 0.0150(5) Uani 1 1 d . . . H3 H 0.2252 0.1976 0.6550 0.018 Uiso 1 1 calc R . . C4 C 0.1531(3) 0.11424(16) 0.73710(14) 0.0149(5) Uani 1 1 d . . . H4 H 0.1567 0.1615 0.7743 0.018 Uiso 1 1 calc R . . C5 C 0.1080(3) 0.02151(16) 0.75336(13) 0.0142(5) Uani 1 1 d . . . C6 C 0.1030(3) -0.04884(16) 0.69447(13) 0.0148(5) Uani 1 1 d . . . H6 H 0.0735 -0.1106 0.7041 0.018 Uiso 1 1 calc R . . C7 C 0.1414(3) -0.02673(16) 0.62300(13) 0.0159(5) Uani 1 1 d . . . H7 H 0.1384 -0.0741 0.5859 0.019 Uiso 1 1 calc R . . C8 C 0.0488(3) -0.00677(17) 0.82641(14) 0.0188(5) Uani 1 1 d . . . H8 H 0.0907 -0.0697 0.8421 0.023 Uiso 1 1 calc R . . C9 C 0.0917(3) 0.0604(2) 0.89419(15) 0.0318(7) Uani 1 1 d . . . H9A H 0.2026 0.0623 0.9091 0.048 Uiso 1 1 calc R . . H9B H 0.0458 0.0384 0.9368 0.048 Uiso 1 1 calc R . . H9C H 0.0537 0.1229 0.8796 0.048 Uiso 1 1 calc R . . C10 C -0.1281(3) -0.01510(17) 0.80511(15) 0.0213(5) Uani 1 1 d . . . H10A H -0.1719 0.0465 0.7919 0.032 Uiso 1 1 calc R . . H10B H -0.1691 -0.0400 0.8483 0.032 Uiso 1 1 calc R . . H10C H -0.1542 -0.0571 0.7618 0.032 Uiso 1 1 calc R . . C11 C 0.5184(3) 0.11509(14) 0.74721(13) 0.0109(4) Uani 1 1 d . . . C12 C 0.6774(3) 0.22198(16) 0.81857(14) 0.0169(5) Uani 1 1 d . . . H12 H 0.7266 0.2567 0.8608 0.020 Uiso 1 1 calc R . . C13 C 0.7029(3) 0.22898(16) 0.74618(13) 0.0163(5) Uani 1 1 d . . . H13 H 0.7729 0.2697 0.7284 0.020 Uiso 1 1 calc R . . C14 C 0.5995(3) 0.15859(16) 0.61845(13) 0.0153(5) Uani 1 1 d . . . H14 H 0.5241 0.1094 0.5979 0.018 Uiso 1 1 calc R . . C15 C 0.5460(3) 0.25285(16) 0.58026(14) 0.0217(6) Uani 1 1 d . . . H15A H 0.4505 0.2719 0.5958 0.033 Uiso 1 1 calc R . . H15B H 0.5301 0.2456 0.5252 0.033 Uiso 1 1 calc R . . H15C H 0.6239 0.3004 0.5958 0.033 Uiso 1 1 calc R . . C16 C 0.7582(3) 0.13050(18) 0.60016(14) 0.0221(6) Uani 1 1 d . . . H16A H 0.8338 0.1776 0.6205 0.033 Uiso 1 1 calc R . . H16B H 0.7523 0.1263 0.5453 0.033 Uiso 1 1 calc R . . H16C H 0.7884 0.0700 0.6232 0.033 Uiso 1 1 calc R . . C17 C 0.5048(3) 0.13011(16) 0.89081(13) 0.0157(5) Uani 1 1 d . . . H17 H 0.4269 0.0797 0.8793 0.019 Uiso 1 1 calc R . . C18 C 0.6354(3) 0.09418(18) 0.95221(14) 0.0241(6) Uani 1 1 d . . . H18A H 0.6809 0.0386 0.9336 0.036 Uiso 1 1 calc R . . H18B H 0.5949 0.0784 0.9980 0.036 Uiso 1 1 calc R . . H18C H 0.7131 0.1427 0.9639 0.036 Uiso 1 1 calc R . . C19 C 0.4259(3) 0.21813(17) 0.91855(15) 0.0233(6) Uani 1 1 d . . . H19A H 0.5010 0.2681 0.9306 0.035 Uiso 1 1 calc R . . H19B H 0.3837 0.2023 0.9638 0.035 Uiso 1 1 calc R . . H19C H 0.3438 0.2390 0.8786 0.035 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 0.00998(10) 0.00784(9) 0.01030(9) -0.00065(6) 0.00379(7) -0.00013(7) I1 0.01733(9) 0.01116(8) 0.01342(8) 0.00234(5) 0.00589(6) 0.00120(6) I2 0.01786(9) 0.01391(8) 0.01337(8) -0.00157(6) 0.00616(6) 0.00418(6) N1 0.0145(11) 0.0133(9) 0.0131(10) -0.0012(7) 0.0057(8) -0.0030(8) N2 0.0140(11) 0.0130(9) 0.0116(9) 0.0006(7) 0.0040(8) -0.0033(8) C1 0.0193(14) 0.0235(13) 0.0155(12) 0.0029(10) -0.0011(10) 0.0017(11) C2 0.0117(12) 0.0170(11) 0.0144(11) 0.0024(9) -0.0003(9) 0.0026(9) C3 0.0122(12) 0.0123(11) 0.0209(12) 0.0022(9) 0.0043(9) 0.0051(9) C4 0.0112(12) 0.0161(11) 0.0182(12) -0.0021(9) 0.0047(9) 0.0037(9) C5 0.0094(12) 0.0155(11) 0.0183(12) 0.0020(9) 0.0037(9) 0.0016(9) C6 0.0103(12) 0.0121(11) 0.0219(12) -0.0004(9) 0.0023(9) -0.0032(9) C7 0.0115(13) 0.0168(11) 0.0182(12) -0.0038(9) -0.0004(9) 0.0009(10) C8 0.0138(13) 0.0216(12) 0.0232(13) 0.0057(10) 0.0092(10) 0.0028(10) C9 0.0283(17) 0.0542(18) 0.0160(13) -0.0030(13) 0.0123(12) -0.0109(14) C10 0.0147(14) 0.0227(13) 0.0290(14) 0.0004(11) 0.0106(11) -0.0013(10) C11 0.0137(12) 0.0094(10) 0.0110(10) 0.0004(8) 0.0061(8) 0.0023(9) C12 0.0199(14) 0.0145(11) 0.0169(12) -0.0047(9) 0.0048(10) -0.0065(10) C13 0.0183(14) 0.0125(11) 0.0189(12) -0.0015(9) 0.0059(10) -0.0065(10) C14 0.0194(13) 0.0145(11) 0.0133(11) -0.0006(9) 0.0066(9) -0.0039(10) C15 0.0336(17) 0.0161(12) 0.0157(12) 0.0019(10) 0.0051(11) -0.0013(11) C16 0.0224(15) 0.0266(13) 0.0204(13) -0.0029(11) 0.0119(11) -0.0051(11) C17 0.0217(14) 0.0152(11) 0.0129(11) -0.0021(9) 0.0104(10) -0.0052(10) C18 0.0286(16) 0.0295(14) 0.0151(13) -0.0009(10) 0.0063(11) -0.0031(12) C19 0.0287(16) 0.0201(12) 0.0244(14) -0.0089(11) 0.0142(12) -0.0045(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C11 2.101(2) . ? Ru1 C3 2.180(2) . ? Ru1 C7 2.205(3) . ? Ru1 C2 2.217(2) . ? Ru1 C4 2.222(2) . ? Ru1 C6 2.232(2) . ? Ru1 C5 2.260(2) . ? Ru1 I2 2.7431(6) . ? Ru1 I1 2.7521(6) . ? N1 C11 1.366(3) . ? N1 C12 1.385(3) . ? N1 C17 1.483(3) . ? N2 C11 1.376(3) . ? N2 C13 1.380(3) . ? N2 C14 1.473(3) . ? C1 C2 1.502(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.405(3) . ? C2 C7 1.431(3) . ? C3 C4 1.421(3) . ? C3 H3 0.9300 . ? C4 C5 1.406(3) . ? C4 H4 0.9300 . ? C5 C6 1.428(3) . ? C5 C8 1.518(3) . ? C6 C7 1.391(3) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.517(4) . ? C8 C10 1.531(4) . ? C8 H8 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C12 C13 1.333(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.523(3) . ? C14 C16 1.529(3) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.517(4) . ? C17 C19 1.537(3) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? 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 C11 Ru1 C3 88.15(9) . . ? C11 Ru1 C7 147.95(9) . . ? C3 Ru1 C7 67.13(9) . . ? C11 Ru1 C2 110.64(9) . . ? C3 Ru1 C2 37.24(8) . . ? C7 Ru1 C2 37.77(8) . . ? C11 Ru1 C4 94.15(9) . . ? C3 Ru1 C4 37.66(8) . . ? C7 Ru1 C4 78.85(9) . . ? C2 Ru1 C4 67.52(9) . . ? C11 Ru1 C6 159.82(8) . . ? C3 Ru1 C6 78.75(9) . . ? C7 Ru1 C6 36.55(8) . . ? C2 Ru1 C6 67.07(9) . . ? C4 Ru1 C6 66.15(9) . . ? C11 Ru1 C5 123.32(8) . . ? C3 Ru1 C5 67.10(8) . . ? C7 Ru1 C5 66.75(9) . . ? C2 Ru1 C5 79.77(9) . . ? C4 Ru1 C5 36.57(8) . . ? C6 Ru1 C5 37.07(8) . . ? C11 Ru1 I2 93.61(6) . . ? C3 Ru1 I2 123.83(6) . . ? C7 Ru1 I2 84.53(6) . . ? C2 Ru1 I2 91.97(6) . . ? C4 Ru1 I2 159.49(6) . . ? C6 Ru1 I2 106.42(6) . . ? C5 Ru1 I2 142.81(6) . . ? C11 Ru1 I1 93.77(7) . . ? C3 Ru1 I1 152.31(6) . . ? C7 Ru1 I1 117.68(6) . . ? C2 Ru1 I1 155.45(6) . . ? C4 Ru1 I1 114.70(6) . . ? C6 Ru1 I1 90.94(7) . . ? C5 Ru1 I1 89.17(6) . . ? I2 Ru1 I1 83.660(17) . . ? C11 N1 C12 111.43(18) . . ? C11 N1 C17 127.71(19) . . ? C12 N1 C17 120.85(19) . . ? C11 N2 C13 111.30(18) . . ? C11 N2 C14 128.01(19) . . ? C13 N2 C14 120.61(17) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 117.5(2) . . ? C3 C2 C1 122.8(2) . . ? C7 C2 C1 119.7(2) . . ? C3 C2 Ru1 69.92(14) . . ? C7 C2 Ru1 70.64(13) . . ? C1 C2 Ru1 130.59(17) . . ? C2 C3 C4 121.6(2) . . ? C2 C3 Ru1 72.84(13) . . ? C4 C3 Ru1 72.78(13) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? Ru1 C3 H3 127.3 . . ? C5 C4 C3 120.5(2) . . ? C5 C4 Ru1 73.19(13) . . ? C3 C4 Ru1 69.56(12) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? Ru1 C4 H4 130.0 . . ? C4 C5 C6 118.1(2) . . ? C4 C5 C8 124.3(2) . . ? C6 C5 C8 117.4(2) . . ? C4 C5 Ru1 70.24(13) . . ? C6 C5 Ru1 70.39(13) . . ? C8 C5 Ru1 136.03(17) . . ? C7 C6 C5 121.2(2) . . ? C7 C6 Ru1 70.68(14) . . ? C5 C6 Ru1 72.54(13) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? Ru1 C6 H6 130.0 . . ? C6 C7 C2 121.1(2) . . ? C6 C7 Ru1 72.78(14) . . ? C2 C7 Ru1 71.60(14) . . ? C6 C7 H7 119.4 . . ? C2 C7 H7 119.4 . . ? Ru1 C7 H7 128.5 . . ? C9 C8 C5 115.4(2) . . ? C9 C8 C10 110.0(2) . . ? C5 C8 C10 106.8(2) . . ? C9 C8 H8 108.1 . . ? C5 C8 H8 108.1 . . ? C10 C8 H8 108.1 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 N2 103.05(19) . . ? N1 C11 Ru1 128.05(15) . . ? N2 C11 Ru1 128.49(16) . . ? C13 C12 N1 107.0(2) . . ? C13 C12 H12 126.5 . . ? N1 C12 H12 126.5 . . ? C12 C13 N2 107.15(19) . . ? C12 C13 H13 126.4 . . ? N2 C13 H13 126.4 . . ? N2 C14 C15 110.46(18) . . ? N2 C14 C16 110.3(2) . . ? C15 C14 C16 110.7(2) . . ? N2 C14 H14 108.5 . . ? C15 C14 H14 108.5 . . ? C16 C14 H14 108.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 110.5(2) . . ? N1 C17 C19 109.54(18) . . ? C18 C17 C19 111.5(2) . . ? N1 C17 H17 108.4 . . ? C18 C17 H17 108.4 . . ? C19 C17 H17 108.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Ru1 C2 C3 -56.47(15) . . . . ? C7 Ru1 C2 C3 130.5(2) . . . . ? C4 Ru1 C2 C3 29.39(13) . . . . ? C6 Ru1 C2 C3 101.92(15) . . . . ? C5 Ru1 C2 C3 65.43(14) . . . . ? I2 Ru1 C2 C3 -151.07(13) . . . . ? I1 Ru1 C2 C3 129.92(14) . . . . ? C11 Ru1 C2 C7 173.05(12) . . . . ? C3 Ru1 C2 C7 -130.5(2) . . . . ? C4 Ru1 C2 C7 -101.09(14) . . . . ? C6 Ru1 C2 C7 -28.56(13) . . . . ? C5 Ru1 C2 C7 -65.05(13) . . . . ? I2 Ru1 C2 C7 78.45(12) . . . . ? I1 Ru1 C2 C7 -0.6(2) . . . . ? C11 Ru1 C2 C1 60.1(2) . . . . ? C3 Ru1 C2 C1 116.5(3) . . . . ? C7 Ru1 C2 C1 -113.0(3) . . . . ? C4 Ru1 C2 C1 145.9(2) . . . . ? C6 Ru1 C2 C1 -141.6(2) . . . . ? C5 Ru1 C2 C1 -178.0(2) . . . . ? I2 Ru1 C2 C1 -34.5(2) . . . . ? I1 Ru1 C2 C1 -113.6(2) . . . . ? C7 C2 C3 C4 -2.4(4) . . . . ? C1 C2 C3 C4 177.6(2) . . . . ? Ru1 C2 C3 C4 -56.3(2) . . . . ? C7 C2 C3 Ru1 54.0(2) . . . . ? C1 C2 C3 Ru1 -126.1(2) . . . . ? C11 Ru1 C3 C2 128.69(14) . . . . ? C7 Ru1 C3 C2 -30.37(13) . . . . ? C4 Ru1 C3 C2 -132.1(2) . . . . ? C6 Ru1 C3 C2 -66.75(14) . . . . ? C5 Ru1 C3 C2 -103.70(15) . . . . ? I2 Ru1 C3 C2 35.59(15) . . . . ? I1 Ru1 C3 C2 -136.71(13) . . . . ? C11 Ru1 C3 C4 -99.22(15) . . . . ? C7 Ru1 C3 C4 101.72(15) . . . . ? C2 Ru1 C3 C4 132.1(2) . . . . ? C6 Ru1 C3 C4 65.34(14) . . . . ? C5 Ru1 C3 C4 28.39(14) . . . . ? I2 Ru1 C3 C4 167.68(11) . . . . ? I1 Ru1 C3 C4 -4.6(2) . . . . ? C2 C3 C4 C5 1.6(4) . . . . ? Ru1 C3 C4 C5 -54.7(2) . . . . ? C2 C3 C4 Ru1 56.4(2) . . . . ? C11 Ru1 C4 C5 -145.76(15) . . . . ? C3 Ru1 C4 C5 132.7(2) . . . . ? C7 Ru1 C4 C5 65.82(15) . . . . ? C2 Ru1 C4 C5 103.60(16) . . . . ? C6 Ru1 C4 C5 29.74(14) . . . . ? I2 Ru1 C4 C5 102.29(19) . . . . ? I1 Ru1 C4 C5 -49.68(15) . . . . ? C11 Ru1 C4 C3 81.56(15) . . . . ? C7 Ru1 C4 C3 -66.86(14) . . . . ? C2 Ru1 C4 C3 -29.08(14) . . . . ? C6 Ru1 C4 C3 -102.94(16) . . . . ? C5 Ru1 C4 C3 -132.7(2) . . . . ? I2 Ru1 C4 C3 -30.4(3) . . . . ? I1 Ru1 C4 C3 177.64(12) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? Ru1 C4 C5 C6 -53.4(2) . . . . ? C3 C4 C5 C8 -174.0(2) . . . . ? Ru1 C4 C5 C8 132.9(2) . . . . ? C3 C4 C5 Ru1 53.1(2) . . . . ? C11 Ru1 C5 C4 42.18(18) . . . . ? C3 Ru1 C5 C4 -29.18(14) . . . . ? C7 Ru1 C5 C4 -103.06(16) . . . . ? C2 Ru1 C5 C4 -65.87(15) . . . . ? C6 Ru1 C5 C4 -131.2(2) . . . . ? I2 Ru1 C5 C4 -145.49(12) . . . . ? I1 Ru1 C5 C4 136.15(14) . . . . ? C11 Ru1 C5 C6 173.37(13) . . . . ? C3 Ru1 C5 C6 102.00(15) . . . . ? C7 Ru1 C5 C6 28.13(13) . . . . ? C2 Ru1 C5 C6 65.31(14) . . . . ? C4 Ru1 C5 C6 131.2(2) . . . . ? I2 Ru1 C5 C6 -14.31(19) . . . . ? I1 Ru1 C5 C6 -92.67(13) . . . . ? C11 Ru1 C5 C8 -77.1(2) . . . . ? C3 Ru1 C5 C8 -148.5(3) . . . . ? C7 Ru1 C5 C8 137.6(3) . . . . ? C2 Ru1 C5 C8 174.8(2) . . . . ? C4 Ru1 C5 C8 -119.3(3) . . . . ? C6 Ru1 C5 C8 109.5(3) . . . . ? I2 Ru1 C5 C8 95.2(2) . . . . ? I1 Ru1 C5 C8 16.8(2) . . . . ? C4 C5 C6 C7 0.0(4) . . . . ? C8 C5 C6 C7 174.1(2) . . . . ? Ru1 C5 C6 C7 -53.4(2) . . . . ? C4 C5 C6 Ru1 53.4(2) . . . . ? C8 C5 C6 Ru1 -132.5(2) . . . . ? C11 Ru1 C6 C7 117.1(2) . . . . ? C3 Ru1 C6 C7 66.59(14) . . . . ? C2 Ru1 C6 C7 29.45(13) . . . . ? C4 Ru1 C6 C7 103.97(15) . . . . ? C5 Ru1 C6 C7 133.3(2) . . . . ? I2 Ru1 C6 C7 -55.63(13) . . . . ? I1 Ru1 C6 C7 -139.30(13) . . . . ? C11 Ru1 C6 C5 -16.3(3) . . . . ? C3 Ru1 C6 C5 -66.74(14) . . . . ? C7 Ru1 C6 C5 -133.3(2) . . . . ? C2 Ru1 C6 C5 -103.88(15) . . . . ? C4 Ru1 C6 C5 -29.36(13) . . . . ? I2 Ru1 C6 C5 171.04(12) . . . . ? I1 Ru1 C6 C5 87.37(13) . . . . ? C5 C6 C7 C2 -0.8(4) . . . . ? Ru1 C6 C7 C2 -55.0(2) . . . . ? C5 C6 C7 Ru1 54.2(2) . . . . ? C3 C2 C7 C6 1.9(3) . . . . ? C1 C2 C7 C6 -178.0(2) . . . . ? Ru1 C2 C7 C6 55.6(2) . . . . ? C3 C2 C7 Ru1 -53.6(2) . . . . ? C1 C2 C7 Ru1 126.4(2) . . . . ? C11 Ru1 C7 C6 -144.63(15) . . . . ? C3 Ru1 C7 C6 -102.34(15) . . . . ? C2 Ru1 C7 C6 -132.3(2) . . . . ? C4 Ru1 C7 C6 -64.77(14) . . . . ? C5 Ru1 C7 C6 -28.50(13) . . . . ? I2 Ru1 C7 C6 127.31(13) . . . . ? I1 Ru1 C7 C6 47.42(14) . . . . ? C11 Ru1 C7 C2 -12.3(2) . . . . ? C3 Ru1 C7 C2 29.98(13) . . . . ? C4 Ru1 C7 C2 67.55(13) . . . . ? C6 Ru1 C7 C2 132.3(2) . . . . ? C5 Ru1 C7 C2 103.81(14) . . . . ? I2 Ru1 C7 C2 -100.37(12) . . . . ? I1 Ru1 C7 C2 179.74(11) . . . . ? C4 C5 C8 C9 -20.6(4) . . . . ? C6 C5 C8 C9 165.7(2) . . . . ? Ru1 C5 C8 C9 76.2(3) . . . . ? C4 C5 C8 C10 102.0(3) . . . . ? C6 C5 C8 C10 -71.7(3) . . . . ? Ru1 C5 C8 C10 -161.24(18) . . . . ? C12 N1 C11 N2 -1.3(2) . . . . ? C17 N1 C11 N2 177.8(2) . . . . ? C12 N1 C11 Ru1 -174.40(16) . . . . ? C17 N1 C11 Ru1 4.7(3) . . . . ? C13 N2 C11 N1 1.1(2) . . . . ? C14 N2 C11 N1 -175.6(2) . . . . ? C13 N2 C11 Ru1 174.16(16) . . . . ? C14 N2 C11 Ru1 -2.5(3) . . . . ? C3 Ru1 C11 N1 99.5(2) . . . . ? C7 Ru1 C11 N1 137.83(19) . . . . ? C2 Ru1 C11 N1 129.80(19) . . . . ? C4 Ru1 C11 N1 62.3(2) . . . . ? C6 Ru1 C11 N1 50.3(4) . . . . ? C5 Ru1 C11 N1 38.6(2) . . . . ? I2 Ru1 C11 N1 -136.73(19) . . . . ? I1 Ru1 C11 N1 -52.85(19) . . . . ? C3 Ru1 C11 N2 -71.9(2) . . . . ? C7 Ru1 C11 N2 -33.6(3) . . . . ? C2 Ru1 C11 N2 -41.6(2) . . . . ? C4 Ru1 C11 N2 -109.15(19) . . . . ? C6 Ru1 C11 N2 -121.1(2) . . . . ? C5 Ru1 C11 N2 -132.79(18) . . . . ? I2 Ru1 C11 N2 51.84(19) . . . . ? I1 Ru1 C11 N2 135.72(18) . . . . ? C11 N1 C12 C13 1.0(3) . . . . ? C17 N1 C12 C13 -178.1(2) . . . . ? N1 C12 C13 N2 -0.3(3) . . . . ? C11 N2 C13 C12 -0.5(3) . . . . ? C14 N2 C13 C12 176.4(2) . . . . ? C11 N2 C14 C15 115.5(2) . . . . ? C13 N2 C14 C15 -60.8(3) . . . . ? C11 N2 C14 C16 -121.8(2) . . . . ? C13 N2 C14 C16 61.8(3) . . . . ? C11 N1 C17 C18 120.5(2) . . . . ? C12 N1 C17 C18 -60.5(3) . . . . ? C11 N1 C17 C19 -116.3(2) . . . . ? C12 N1 C17 C19 62.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.612 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.109 #===END data_r080513b _database_code_depnum_ccdc_archive 'CCDC 705188' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H31 I N2 Ru' _chemical_formula_weight 563.47 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.538(3) _cell_length_b 9.827(2) _cell_length_c 15.987(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.10(3) _cell_angle_gamma 90.00 _cell_volume 2241.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7065 _cell_measurement_theta_min 2.446 _cell_measurement_theta_max 27.422 _exptl_crystal_description prism _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 2.087 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7588 _exptl_absorpt_correction_T_max 0.8508 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25938 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5133 _reflns_number_gt 4438 _reflns_threshold_expression >2sigma(I) _computing_data_collection crystalclear _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _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^)+(0.0257P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5133 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0586 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.353664(11) 0.204585(18) 1.136544(10) 0.02240(6) Uani 1 1 d . . . Ru1 Ru 0.215686(13) 0.160817(19) 0.996152(12) 0.01421(6) Uani 1 1 d . . . N1 N 0.37159(14) 0.1095(2) 0.89272(13) 0.0187(4) Uani 1 1 d . . . N2 N 0.32453(14) -0.0683(2) 0.95374(12) 0.0182(4) Uani 1 1 d . . . C1 C 0.37442(19) 0.2758(3) 0.78199(17) 0.0247(6) Uani 1 1 d . . . H1 H 0.3601 0.2065 0.7419 0.030 Uiso 1 1 calc R . . C2 C 0.38527(19) 0.4089(3) 0.75518(17) 0.0277(6) Uani 1 1 d . . . H2 H 0.3773 0.4287 0.6973 0.033 Uiso 1 1 calc R . . C3 C 0.40777(18) 0.5106(3) 0.81441(16) 0.0261(6) Uani 1 1 d . . . H3 H 0.4152 0.5995 0.7968 0.031 Uiso 1 1 calc R . . C4 C 0.41946(17) 0.4803(3) 0.90096(16) 0.0215(6) Uani 1 1 d . . . H4 H 0.4346 0.5494 0.9410 0.026 Uiso 1 1 calc R . . C5 C 0.40872(16) 0.3485(2) 0.92805(16) 0.0181(5) Uani 1 1 d . . . H5 H 0.4174 0.3285 0.9859 0.022 Uiso 1 1 calc R . . C6 C 0.38487(17) 0.2465(2) 0.86773(16) 0.0168(5) Uani 1 1 d . . . C7 C 0.31280(16) 0.0659(2) 0.94320(14) 0.0158(5) Uani 1 1 d . . . C8 C 0.39043(19) -0.1264(3) 0.90445(17) 0.0259(6) Uani 1 1 d . . . H8A H 0.3584 -0.1844 0.8589 0.031 Uiso 1 1 calc R . . H8B H 0.4393 -0.1783 0.9406 0.031 Uiso 1 1 calc R . . C9 C 0.4301(2) -0.0005(3) 0.86936(18) 0.0277(6) Uani 1 1 d . . . H9A H 0.4955 0.0127 0.8954 0.033 Uiso 1 1 calc R . . H9B H 0.4244 -0.0064 0.8080 0.033 Uiso 1 1 calc R . . C10 C 0.25748(17) -0.1461(2) 0.99227(15) 0.0177(5) Uani 1 1 d . . . C11 C 0.18663(19) -0.2149(3) 0.92213(17) 0.0268(6) Uani 1 1 d . . . H11A H 0.1543 -0.1470 0.8843 0.040 Uiso 1 1 calc R . . H11B H 0.1422 -0.2651 0.9473 0.040 Uiso 1 1 calc R . . H11C H 0.2188 -0.2759 0.8907 0.040 Uiso 1 1 calc R . . C12 C 0.31027(19) -0.2538(3) 1.05163(16) 0.0241(6) Uani 1 1 d . . . H12A H 0.3336 -0.3225 1.0185 0.036 Uiso 1 1 calc R . . H12B H 0.2686 -0.2945 1.0843 0.036 Uiso 1 1 calc R . . H12C H 0.3618 -0.2120 1.0895 0.036 Uiso 1 1 calc R . . C13 C 0.21006(18) -0.0421(2) 1.04141(16) 0.0211(6) Uani 1 1 d . . . H13A H 0.2401 -0.0451 1.1011 0.025 Uiso 1 1 calc R . . H13B H 0.1450 -0.0678 1.0375 0.025 Uiso 1 1 calc R . . C14 C 0.1286(2) 0.1550(3) 0.78671(16) 0.0305(7) Uani 1 1 d . . . H14A H 0.1081 0.0620 0.7847 0.046 Uiso 1 1 calc R . . H14B H 0.1912 0.1592 0.7760 0.046 Uiso 1 1 calc R . . H14C H 0.0875 0.2067 0.7442 0.046 Uiso 1 1 calc R . . C15 C 0.12685(17) 0.2131(3) 0.87329(16) 0.0206(6) Uani 1 1 d . . . C16 C 0.17786(17) 0.3340(3) 0.90175(16) 0.0194(5) Uani 1 1 d . . . H16 H 0.2110 0.3793 0.8659 0.023 Uiso 1 1 calc R . . C17 C 0.17806(17) 0.3844(3) 0.98370(15) 0.0199(5) Uani 1 1 d . . . H17 H 0.2147 0.4600 1.0027 0.024 Uiso 1 1 calc R . . C18 C 0.12308(17) 0.3226(3) 1.03936(16) 0.0193(5) Uani 1 1 d . . . C19 C 0.06937(17) 0.2087(3) 1.00957(17) 0.0217(6) Uani 1 1 d . . . H19 H 0.0313 0.1689 1.0433 0.026 Uiso 1 1 calc R . . C20 C 0.07249(17) 0.1524(3) 0.92728(16) 0.0212(6) Uani 1 1 d . . . H20 H 0.0380 0.0745 0.9092 0.025 Uiso 1 1 calc R . . C21 C 0.12737(18) 0.3831(3) 1.12681(16) 0.0259(6) Uani 1 1 d . . . H21 H 0.1923 0.4116 1.1480 0.031 Uiso 1 1 calc R . . C22 C 0.1014(2) 0.2820(3) 1.19130(19) 0.0408(8) Uani 1 1 d . . . H22A H 0.0368 0.2562 1.1742 0.061 Uiso 1 1 calc R . . H22B H 0.1108 0.3236 1.2466 0.061 Uiso 1 1 calc R . . H22C H 0.1403 0.2026 1.1936 0.061 Uiso 1 1 calc R . . C23 C 0.0658(2) 0.5109(3) 1.12055(19) 0.0457(9) Uani 1 1 d . . . H23A H 0.0855 0.5746 1.0820 0.068 Uiso 1 1 calc R . . H23B H 0.0719 0.5518 1.1759 0.068 Uiso 1 1 calc R . . H23C H 0.0016 0.4863 1.0999 0.068 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 I1 0.02107(10) 0.02808(11) 0.01694(10) -0.00374(7) 0.00091(7) 0.00595(7) Ru1 0.01543(11) 0.01331(11) 0.01442(11) 0.00029(8) 0.00417(8) 0.00153(8) N1 0.0221(11) 0.0140(11) 0.0233(11) -0.0013(9) 0.0126(9) 0.0030(9) N2 0.0242(11) 0.0131(10) 0.0202(11) 0.0000(8) 0.0113(9) 0.0020(9) C1 0.0321(16) 0.0227(15) 0.0213(14) -0.0045(11) 0.0103(12) -0.0071(12) C2 0.0390(17) 0.0267(16) 0.0185(14) 0.0024(11) 0.0085(12) -0.0090(12) C3 0.0332(16) 0.0165(14) 0.0293(15) 0.0025(11) 0.0077(12) -0.0028(11) C4 0.0225(14) 0.0177(13) 0.0240(14) -0.0042(11) 0.0032(10) -0.0009(10) C5 0.0161(13) 0.0207(14) 0.0172(13) 0.0010(10) 0.0026(10) 0.0007(10) C6 0.0154(12) 0.0145(12) 0.0220(13) 0.0023(10) 0.0072(10) -0.0001(10) C7 0.0173(12) 0.0151(12) 0.0142(12) -0.0013(10) 0.0015(9) -0.0001(10) C8 0.0313(16) 0.0190(14) 0.0311(16) -0.0023(12) 0.0157(12) 0.0050(12) C9 0.0366(16) 0.0160(14) 0.0358(16) -0.0016(12) 0.0201(13) 0.0056(12) C10 0.0198(13) 0.0134(13) 0.0205(14) 0.0008(10) 0.0052(10) -0.0006(10) C11 0.0279(15) 0.0265(15) 0.0246(15) -0.0015(11) 0.0013(12) -0.0046(12) C12 0.0319(16) 0.0192(13) 0.0219(14) 0.0043(11) 0.0065(11) 0.0035(12) C13 0.0275(14) 0.0165(13) 0.0219(14) 0.0023(10) 0.0112(11) 0.0011(11) C14 0.0333(17) 0.0362(17) 0.0183(15) -0.0017(12) -0.0045(12) 0.0038(13) C15 0.0149(13) 0.0255(15) 0.0197(14) 0.0028(11) -0.0008(10) 0.0049(10) C16 0.0163(13) 0.0215(14) 0.0205(14) 0.0074(11) 0.0034(10) 0.0050(10) C17 0.0208(13) 0.0154(12) 0.0234(14) 0.0030(10) 0.0038(10) 0.0086(10) C18 0.0165(13) 0.0219(14) 0.0201(14) 0.0029(10) 0.0054(10) 0.0111(10) C19 0.0145(13) 0.0266(15) 0.0252(15) 0.0044(11) 0.0067(11) 0.0048(10) C20 0.0173(13) 0.0184(14) 0.0263(14) -0.0013(11) 0.0007(10) -0.0013(10) C21 0.0237(14) 0.0337(16) 0.0198(14) -0.0033(12) 0.0029(11) 0.0130(12) C22 0.042(2) 0.058(2) 0.0252(17) 0.0008(15) 0.0129(14) 0.0113(16) C23 0.054(2) 0.048(2) 0.0335(18) -0.0126(15) 0.0051(15) 0.0284(17) _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 I1 Ru1 2.7408(9) . ? Ru1 C7 2.010(2) . ? Ru1 C13 2.128(2) . ? Ru1 C20 2.161(3) . ? Ru1 C15 2.194(3) . ? Ru1 C19 2.229(2) . ? Ru1 C17 2.264(2) . ? Ru1 C16 2.271(2) . ? Ru1 C18 2.275(2) . ? N1 C7 1.353(3) . ? N1 C6 1.428(3) . ? N1 C9 1.467(3) . ? N2 C7 1.336(3) . ? N2 C10 1.464(3) . ? N2 C8 1.468(3) . ? C1 C6 1.380(4) . ? C1 C2 1.395(4) . ? C1 H1 0.9300 . ? C2 C3 1.372(4) . ? C2 H2 0.9300 . ? C3 C4 1.393(3) . ? C3 H3 0.9300 . ? C4 C5 1.384(3) . ? C4 H4 0.9300 . ? C5 C6 1.388(3) . ? C5 H5 0.9300 . ? C8 C9 1.517(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C12 1.526(3) . ? C10 C11 1.527(4) . ? C10 C13 1.531(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.502(4) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.410(3) . ? C15 C16 1.427(4) . ? C16 C17 1.400(3) . ? C16 H16 0.9300 . ? C17 C18 1.440(3) . ? C17 H17 0.9300 . ? C18 C19 1.395(4) . ? C18 C21 1.509(3) . ? C19 C20 1.436(4) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.531(4) . ? C21 C23 1.534(4) . ? C21 H21 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? 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 C7 Ru1 C13 77.54(9) . . ? C7 Ru1 C20 116.97(9) . . ? C13 Ru1 C20 92.35(10) . . ? C7 Ru1 C15 94.12(10) . . ? C13 Ru1 C15 118.00(10) . . ? C20 Ru1 C15 37.78(9) . . ? C7 Ru1 C19 154.05(10) . . ? C13 Ru1 C19 93.73(9) . . ? C20 Ru1 C19 38.14(9) . . ? C15 Ru1 C19 68.20(10) . . ? C7 Ru1 C17 126.22(9) . . ? C13 Ru1 C17 156.19(9) . . ? C20 Ru1 C17 78.44(9) . . ? C15 Ru1 C17 66.62(9) . . ? C19 Ru1 C17 65.47(9) . . ? C7 Ru1 C16 99.66(9) . . ? C13 Ru1 C16 155.22(10) . . ? C20 Ru1 C16 66.66(9) . . ? C15 Ru1 C16 37.24(9) . . ? C19 Ru1 C16 78.02(9) . . ? C17 Ru1 C16 35.97(9) . . ? C7 Ru1 C18 163.14(10) . . ? C13 Ru1 C18 119.19(9) . . ? C20 Ru1 C18 67.23(9) . . ? C15 Ru1 C18 80.06(9) . . ? C19 Ru1 C18 36.07(9) . . ? C17 Ru1 C18 37.00(8) . . ? C16 Ru1 C18 66.20(9) . . ? C7 Ru1 I1 87.42(7) . . ? C13 Ru1 I1 86.48(7) . . ? C20 Ru1 I1 154.76(7) . . ? C15 Ru1 I1 155.25(7) . . ? C19 Ru1 I1 116.72(7) . . ? C17 Ru1 I1 92.64(7) . . ? C16 Ru1 I1 118.16(7) . . ? C18 Ru1 I1 91.39(7) . . ? C7 N1 C6 126.9(2) . . ? C7 N1 C9 112.5(2) . . ? C6 N1 C9 120.45(19) . . ? C7 N2 C10 119.26(19) . . ? C7 N2 C8 113.4(2) . . ? C10 N2 C8 125.4(2) . . ? C6 C1 C2 120.2(2) . . ? C6 C1 H1 119.9 . . ? C2 C1 H1 119.9 . . ? C3 C2 C1 119.8(2) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.8(2) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.7(2) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 119.1(2) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C1 C6 C5 120.3(2) . . ? C1 C6 N1 118.7(2) . . ? C5 C6 N1 121.0(2) . . ? N2 C7 N1 107.9(2) . . ? N2 C7 Ru1 119.21(17) . . ? N1 C7 Ru1 132.81(18) . . ? N2 C8 C9 102.4(2) . . ? N2 C8 H8A 111.3 . . ? C9 C8 H8A 111.3 . . ? N2 C8 H8B 111.3 . . ? C9 C8 H8B 111.3 . . ? H8A C8 H8B 109.2 . . ? N1 C9 C8 103.1(2) . . ? N1 C9 H9A 111.2 . . ? C8 C9 H9A 111.2 . . ? N1 C9 H9B 111.2 . . ? C8 C9 H9B 111.2 . . ? H9A C9 H9B 109.1 . . ? N2 C10 C12 109.1(2) . . ? N2 C10 C11 109.4(2) . . ? C12 C10 C11 109.7(2) . . ? N2 C10 C13 105.65(19) . . ? C12 C10 C13 111.5(2) . . ? C11 C10 C13 111.4(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 Ru1 113.58(16) . . ? C10 C13 H13A 108.8 . . ? Ru1 C13 H13A 108.8 . . ? C10 C13 H13B 108.8 . . ? Ru1 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 118.4(2) . . ? C20 C15 C14 120.9(2) . . ? C16 C15 C14 120.7(2) . . ? C20 C15 Ru1 69.85(14) . . ? C16 C15 Ru1 74.31(14) . . ? C14 C15 Ru1 128.64(18) . . ? C17 C16 C15 120.0(2) . . ? C17 C16 Ru1 71.74(14) . . ? C15 C16 Ru1 68.45(14) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? Ru1 C16 H16 132.9 . . ? C16 C17 C18 121.8(2) . . ? C16 C17 Ru1 72.29(14) . . ? C18 C17 Ru1 71.91(14) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? Ru1 C17 H17 129.2 . . ? C19 C18 C17 117.9(2) . . ? C19 C18 C21 123.6(2) . . ? C17 C18 C21 118.5(2) . . ? C19 C18 Ru1 70.17(14) . . ? C17 C18 Ru1 71.09(13) . . ? C21 C18 Ru1 129.44(17) . . ? C18 C19 C20 120.5(2) . . ? C18 C19 Ru1 73.76(14) . . ? C20 C19 Ru1 68.37(14) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? Ru1 C19 H19 130.8 . . ? C15 C20 C19 121.2(2) . . ? C15 C20 Ru1 72.37(14) . . ? C19 C20 Ru1 73.49(15) . . ? C15 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? Ru1 C20 H20 126.7 . . ? C18 C21 C22 113.4(2) . . ? C18 C21 C23 110.0(2) . . ? C22 C21 C23 111.1(2) . . ? C18 C21 H21 107.4 . . ? C22 C21 H21 107.4 . . ? C23 C21 H21 107.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.0(4) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C2 C1 C6 C5 -1.8(4) . . . . ? C2 C1 C6 N1 178.9(2) . . . . ? C4 C5 C6 C1 1.7(4) . . . . ? C4 C5 C6 N1 -179.0(2) . . . . ? C7 N1 C6 C1 -125.7(3) . . . . ? C9 N1 C6 C1 59.5(3) . . . . ? C7 N1 C6 C5 55.0(3) . . . . ? C9 N1 C6 C5 -119.9(3) . . . . ? C10 N2 C7 N1 -168.6(2) . . . . ? C8 N2 C7 N1 -3.8(3) . . . . ? C10 N2 C7 Ru1 9.1(3) . . . . ? C8 N2 C7 Ru1 173.94(16) . . . . ? C6 N1 C7 N2 -177.4(2) . . . . ? C9 N1 C7 N2 -2.2(3) . . . . ? C6 N1 C7 Ru1 5.3(4) . . . . ? C9 N1 C7 Ru1 -179.50(19) . . . . ? C13 Ru1 C7 N2 4.22(18) . . . . ? C20 Ru1 C7 N2 -82.0(2) . . . . ? C15 Ru1 C7 N2 -113.56(19) . . . . ? C19 Ru1 C7 N2 -68.2(3) . . . . ? C17 Ru1 C7 N2 -177.43(17) . . . . ? C16 Ru1 C7 N2 -150.68(19) . . . . ? C18 Ru1 C7 N2 177.5(3) . . . . ? I1 Ru1 C7 N2 91.18(18) . . . . ? C13 Ru1 C7 N1 -178.7(2) . . . . ? C20 Ru1 C7 N1 95.0(2) . . . . ? C15 Ru1 C7 N1 63.5(2) . . . . ? C19 Ru1 C7 N1 108.8(3) . . . . ? C17 Ru1 C7 N1 -0.4(3) . . . . ? C16 Ru1 C7 N1 26.4(2) . . . . ? C18 Ru1 C7 N1 -5.5(5) . . . . ? I1 Ru1 C7 N1 -91.8(2) . . . . ? C7 N2 C8 C9 7.7(3) . . . . ? C10 N2 C8 C9 171.5(2) . . . . ? C7 N1 C9 C8 6.8(3) . . . . ? C6 N1 C9 C8 -177.7(2) . . . . ? N2 C8 C9 N1 -8.1(3) . . . . ? C7 N2 C10 C12 -140.9(2) . . . . ? C8 N2 C10 C12 56.3(3) . . . . ? C7 N2 C10 C11 99.1(3) . . . . ? C8 N2 C10 C11 -63.7(3) . . . . ? C7 N2 C10 C13 -20.9(3) . . . . ? C8 N2 C10 C13 176.2(2) . . . . ? N2 C10 C13 Ru1 23.1(2) . . . . ? C12 C10 C13 Ru1 141.46(18) . . . . ? C11 C10 C13 Ru1 -95.6(2) . . . . ? C7 Ru1 C13 C10 -15.69(18) . . . . ? C20 Ru1 C13 C10 101.42(19) . . . . ? C15 Ru1 C13 C10 72.4(2) . . . . ? C19 Ru1 C13 C10 139.60(18) . . . . ? C17 Ru1 C13 C10 167.61(19) . . . . ? C16 Ru1 C13 C10 70.4(3) . . . . ? C18 Ru1 C13 C10 166.54(16) . . . . ? I1 Ru1 C13 C10 -103.83(18) . . . . ? C7 Ru1 C15 C20 130.48(15) . . . . ? C13 Ru1 C15 C20 52.41(17) . . . . ? C19 Ru1 C15 C20 -29.93(14) . . . . ? C17 Ru1 C15 C20 -101.62(16) . . . . ? C16 Ru1 C15 C20 -129.0(2) . . . . ? C18 Ru1 C15 C20 -65.47(15) . . . . ? I1 Ru1 C15 C20 -136.73(15) . . . . ? C7 Ru1 C15 C16 -100.56(15) . . . . ? C13 Ru1 C15 C16 -178.64(14) . . . . ? C20 Ru1 C15 C16 129.0(2) . . . . ? C19 Ru1 C15 C16 99.02(16) . . . . ? C17 Ru1 C15 C16 27.34(14) . . . . ? C18 Ru1 C15 C16 63.48(15) . . . . ? I1 Ru1 C15 C16 -7.8(3) . . . . ? C7 Ru1 C15 C14 16.5(2) . . . . ? C13 Ru1 C15 C14 -61.6(3) . . . . ? C20 Ru1 C15 C14 -114.0(3) . . . . ? C19 Ru1 C15 C14 -144.0(3) . . . . ? C17 Ru1 C15 C14 144.4(3) . . . . ? C16 Ru1 C15 C14 117.0(3) . . . . ? C18 Ru1 C15 C14 -179.5(3) . . . . ? I1 Ru1 C15 C14 109.2(2) . . . . ? C20 C15 C16 C17 4.2(3) . . . . ? C14 C15 C16 C17 -177.9(2) . . . . ? Ru1 C15 C16 C17 -51.9(2) . . . . ? C20 C15 C16 Ru1 56.1(2) . . . . ? C14 C15 C16 Ru1 -126.0(2) . . . . ? C7 Ru1 C16 C17 -141.81(15) . . . . ? C13 Ru1 C16 C17 137.0(2) . . . . ? C20 Ru1 C16 C17 102.88(16) . . . . ? C15 Ru1 C16 C17 134.1(2) . . . . ? C19 Ru1 C16 C17 64.51(15) . . . . ? C18 Ru1 C16 C17 28.56(14) . . . . ? I1 Ru1 C16 C17 -49.55(15) . . . . ? C7 Ru1 C16 C15 84.06(16) . . . . ? C13 Ru1 C16 C15 2.9(3) . . . . ? C20 Ru1 C16 C15 -31.25(15) . . . . ? C19 Ru1 C16 C15 -69.62(15) . . . . ? C17 Ru1 C16 C15 -134.1(2) . . . . ? C18 Ru1 C16 C15 -105.57(16) . . . . ? I1 Ru1 C16 C15 176.32(12) . . . . ? C15 C16 C17 C18 -4.0(3) . . . . ? Ru1 C16 C17 C18 -54.4(2) . . . . ? C15 C16 C17 Ru1 50.4(2) . . . . ? C7 Ru1 C17 C16 49.07(18) . . . . ? C13 Ru1 C17 C16 -134.9(2) . . . . ? C20 Ru1 C17 C16 -66.01(15) . . . . ? C15 Ru1 C17 C16 -28.24(14) . . . . ? C19 Ru1 C17 C16 -103.91(16) . . . . ? C18 Ru1 C17 C16 -133.4(2) . . . . ? I1 Ru1 C17 C16 137.81(13) . . . . ? C7 Ru1 C17 C18 -177.55(14) . . . . ? C13 Ru1 C17 C18 -1.5(3) . . . . ? C20 Ru1 C17 C18 67.36(15) . . . . ? C15 Ru1 C17 C18 105.13(16) . . . . ? C19 Ru1 C17 C18 29.46(15) . . . . ? C16 Ru1 C17 C18 133.4(2) . . . . ? I1 Ru1 C17 C18 -88.81(14) . . . . ? C16 C17 C18 C19 0.6(3) . . . . ? Ru1 C17 C18 C19 -54.0(2) . . . . ? C16 C17 C18 C21 179.9(2) . . . . ? Ru1 C17 C18 C21 125.3(2) . . . . ? C16 C17 C18 Ru1 54.6(2) . . . . ? C7 Ru1 C18 C19 137.4(3) . . . . ? C13 Ru1 C18 C19 -50.18(18) . . . . ? C20 Ru1 C18 C19 29.25(15) . . . . ? C15 Ru1 C18 C19 66.43(16) . . . . ? C17 Ru1 C18 C19 130.5(2) . . . . ? C16 Ru1 C18 C19 102.72(17) . . . . ? I1 Ru1 C18 C19 -136.93(14) . . . . ? C7 Ru1 C18 C17 6.8(4) . . . . ? C13 Ru1 C18 C17 179.28(14) . . . . ? C20 Ru1 C18 C17 -101.29(16) . . . . ? C15 Ru1 C18 C17 -64.10(15) . . . . ? C19 Ru1 C18 C17 -130.5(2) . . . . ? C16 Ru1 C18 C17 -27.82(14) . . . . ? I1 Ru1 C18 C17 92.54(14) . . . . ? C7 Ru1 C18 C21 -105.0(4) . . . . ? C13 Ru1 C18 C21 67.5(3) . . . . ? C20 Ru1 C18 C21 146.9(3) . . . . ? C15 Ru1 C18 C21 -175.9(3) . . . . ? C19 Ru1 C18 C21 117.7(3) . . . . ? C17 Ru1 C18 C21 -111.8(3) . . . . ? C16 Ru1 C18 C21 -139.6(3) . . . . ? I1 Ru1 C18 C21 -19.3(2) . . . . ? C17 C18 C19 C20 2.6(4) . . . . ? C21 C18 C19 C20 -176.7(2) . . . . ? Ru1 C18 C19 C20 -51.9(2) . . . . ? C17 C18 C19 Ru1 54.5(2) . . . . ? C21 C18 C19 Ru1 -124.8(2) . . . . ? C7 Ru1 C19 C18 -153.3(2) . . . . ? C13 Ru1 C19 C18 137.78(16) . . . . ? C20 Ru1 C19 C18 -133.2(2) . . . . ? C15 Ru1 C19 C18 -103.49(16) . . . . ? C17 Ru1 C19 C18 -30.18(14) . . . . ? C16 Ru1 C19 C18 -65.83(15) . . . . ? I1 Ru1 C19 C18 49.85(16) . . . . ? C7 Ru1 C19 C20 -20.2(3) . . . . ? C13 Ru1 C19 C20 -89.06(15) . . . . ? C15 Ru1 C19 C20 29.67(14) . . . . ? C17 Ru1 C19 C20 102.98(16) . . . . ? C16 Ru1 C19 C20 67.33(15) . . . . ? C18 Ru1 C19 C20 133.2(2) . . . . ? I1 Ru1 C19 C20 -176.99(12) . . . . ? C16 C15 C20 C19 -1.1(4) . . . . ? C14 C15 C20 C19 -179.0(2) . . . . ? Ru1 C15 C20 C19 57.2(2) . . . . ? C16 C15 C20 Ru1 -58.3(2) . . . . ? C14 C15 C20 Ru1 123.8(2) . . . . ? C18 C19 C20 C15 -2.3(4) . . . . ? Ru1 C19 C20 C15 -56.7(2) . . . . ? C18 C19 C20 Ru1 54.4(2) . . . . ? C7 Ru1 C20 C15 -58.34(17) . . . . ? C13 Ru1 C20 C15 -135.56(15) . . . . ? C19 Ru1 C20 C15 131.4(2) . . . . ? C17 Ru1 C20 C15 66.60(15) . . . . ? C16 Ru1 C20 C15 30.83(15) . . . . ? C18 Ru1 C20 C15 103.64(16) . . . . ? I1 Ru1 C20 C15 137.71(15) . . . . ? C7 Ru1 C20 C19 170.26(14) . . . . ? C13 Ru1 C20 C19 93.05(15) . . . . ? C15 Ru1 C20 C19 -131.4(2) . . . . ? C17 Ru1 C20 C19 -64.80(14) . . . . ? C16 Ru1 C20 C19 -100.56(16) . . . . ? C18 Ru1 C20 C19 -27.76(14) . . . . ? I1 Ru1 C20 C19 6.3(3) . . . . ? C19 C18 C21 C22 22.9(3) . . . . ? C17 C18 C21 C22 -156.4(2) . . . . ? Ru1 C18 C21 C22 -68.2(3) . . . . ? C19 C18 C21 C23 -102.1(3) . . . . ? C17 C18 C21 C23 78.6(3) . . . . ? Ru1 C18 C21 C23 166.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.747 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.097 #===END