# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2288 #Paper communicated to J.C.S.Dalton Transactions. #title of the paper: #Ruthenium mononitro and mononitroso terpyridine complexes #incorporating azo-imine based ancillary ligands. Synthesis, #crystal structure , spectroelectrochemical properties and kinetic aspects #By Biplab Mondal, Himadri Paul, Vedavati G. Puranik and Goutam Kumar Lahiri _publ_contact_author ; Prof.G.K.Lahiri address: ; _publ_contact_author_email 'lahiri@ether.chem.iitb.ernet.in' _publ_contact_author_fax ' 91-022-5783480 ' _publ_contact_author_phone ' 91-022-5767159 ' data_C33H28ClN7O6Ru _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Ru(trpy)(L2)(NO2)] ClO4 ; _chemical_name_common 'Ruthenium Complex.' _chemical_formula_moiety 'C33 H28 Cl N7 O6 Ru' _chemical_formula_sum 'C33 H28 Cl N7 O6 Ru' _chemical_formula_weight 755.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4520(10) _cell_length_b 11.8070(10) _cell_length_c 13.265(2) _cell_angle_alpha 82.366(9) _cell_angle_beta 67.565(8) _cell_angle_gamma 77.581(7) _cell_volume 1616.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'crystal Apprence...'? _exptl_crystal_colour 'color ....'? _exptl_crystal_size_max '0.45' _exptl_crystal_size_mid '0.34' _exptl_crystal_size_min '0.14' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.624 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w/2\q-scan' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% '<4%' _diffrn_reflns_number 5678 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1917 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.93 _reflns_number_total 5678 _reflns_number_gt 3142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software' _computing_data_reduction 'NRCVAX (PC Version) Gabe, E. J. et al., 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, L and Pritzkow, H, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5678 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1476 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1223 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.16607(6) 0.18335(5) 0.04437(5) 0.03043(19) Uani 1 d . . . Cl Cl 0.7127(2) 0.2228(2) 0.46061(18) 0.0633(6) Uani 1 d . . . O1 O -0.1004(5) 0.2274(4) 0.0644(4) 0.0528(14) Uani 1 d . . . O2 O 0.0247(5) 0.1895(4) -0.0984(5) 0.0589(15) Uani 1 d . . . O3 O 0.8383(5) 0.2140(6) 0.4573(5) 0.098(2) Uani 1 d . . . O4 O 0.6304(7) 0.2961(10) 0.5376(9) 0.211(6) Uani 1 d . . . O5 O 0.7054(6) 0.2596(6) 0.3587(6) 0.111(2) Uani 1 d . . . O6 O 0.6702(8) 0.1151(7) 0.4912(7) 0.144(3) Uani 1 d . . . N1 N 0.2703(5) 0.0794(5) -0.0857(4) 0.0333(14) Uani 1 d . . . N2 N 0.2376(5) 0.2995(5) -0.0718(4) 0.0307(13) Uani 1 d . . . N3 N 0.0781(5) 0.3350(4) 0.1263(4) 0.0328(13) Uani 1 d . . . N4 N 0.1039(5) 0.0669(4) 0.1745(4) 0.0331(14) Uani 1 d . . . N5 N 0.2855(5) 0.0980(5) 0.2020(5) 0.0418(15) Uani 1 d . . . N6 N 0.2980(5) 0.1576(5) 0.1123(5) 0.0367(15) Uani 1 d . . . N7 N 0.0121(6) 0.2000(4) -0.0037(5) 0.0383(15) Uani 1 d . . . C1 C 0.2733(7) -0.0353(6) -0.0889(7) 0.0433(19) Uani 1 d . . . C2 C 0.3385(9) -0.0902(8) -0.1858(8) 0.059(3) Uani 1 d . . . C3 C 0.4031(9) -0.0333(8) -0.2786(8) 0.065(3) Uani 1 d . . . C4 C 0.4005(8) 0.0837(8) -0.2750(7) 0.056(2) Uani 1 d . . . C5 C 0.3303(6) 0.1404(6) -0.1805(5) 0.0372(17) Uani 1 d . . . C6 C 0.3130(6) 0.2644(6) -0.1716(5) 0.0354(17) Uani 1 d . . . C7 C 0.3655(7) 0.3457(7) -0.2539(6) 0.047(2) Uani 1 d . . . C8 C 0.3336(8) 0.4613(8) -0.2297(7) 0.050(2) Uani 1 d . . . C9 C 0.2549(7) 0.4958(7) -0.1281(6) 0.0411(19) Uani 1 d . . . C10 C 0.2057(6) 0.4136(5) -0.0472(5) 0.0294(16) Uani 1 d . . . C11 C 0.1192(6) 0.4316(6) 0.0660(5) 0.0336(17) Uani 1 d . . . C12 C 0.0774(7) 0.5402(7) 0.1101(7) 0.0390(19) Uani 1 d . . . C13 C -0.0075(7) 0.5490(7) 0.2165(7) 0.045(2) Uani 1 d . . . C14 C -0.0515(7) 0.4520(8) 0.2747(7) 0.051(2) Uani 1 d . . . C15 C -0.0054(7) 0.3458(7) 0.2276(6) 0.0434(19) Uani 1 d . . . C16 C 0.0012(7) 0.0171(6) 0.2077(7) 0.046(2) Uani 1 d . . . C17 C -0.0310(9) -0.0541(8) 0.3013(7) 0.059(3) Uani 1 d . . . C18 C 0.0448(10) -0.0754(8) 0.3621(8) 0.063(3) Uani 1 d . . . C19 C 0.1526(8) -0.0257(7) 0.3301(6) 0.053(2) Uani 1 d . . . C20 C 0.1790(7) 0.0445(6) 0.2351(6) 0.0421(18) Uani 1 d . . . C21 C 0.3997(6) 0.2254(6) 0.0812(6) 0.0376(17) Uani 1 d . . . C22 C 0.3986(7) 0.2994(6) 0.1525(6) 0.0434(19) Uani 1 d . . . C23 C 0.4913(8) 0.3691(7) 0.1185(7) 0.056(2) Uani 1 d . . . C24 C 0.5800(9) 0.3636(8) 0.0159(8) 0.058(3) Uani 1 d . . . C25 C 0.5855(7) 0.2870(6) -0.0564(6) 0.049(2) Uani 1 d . . . C26 C 0.4914(7) 0.2174(7) -0.0224(7) 0.045(2) Uani 1 d . . . C27 C 0.6886(12) 0.2819(15) -0.1688(10) 0.088(4) Uani 1 d . . . C28 C 0.1513(12) 0.3105(18) 0.4446(9) 0.103(5) Uani 1 d . . . C29 C 0.1573(15) 0.4236(17) 0.4274(10) 0.109(5) Uani 1 d . . . C30 C 0.2629(17) 0.4584(11) 0.4320(9) 0.094(4) Uani 1 d . . . C31 C 0.3536(12) 0.3844(16) 0.4538(9) 0.095(4) Uani 1 d . . . C32 C 0.3484(13) 0.2662(15) 0.4709(9) 0.094(4) Uani 1 d . . . C33 C 0.2439(16) 0.2320(13) 0.4635(9) 0.096(4) Uani 1 d . . . H1 H 0.227(5) -0.073(5) -0.016(5) 0.034(19) Uiso 1 d . . . H2 H 0.332(6) -0.157(5) -0.182(5) 0.03(2) Uiso 1 d . . . H3 H 0.443(8) -0.068(7) -0.347(7) 0.09(3) Uiso 1 d . . . H4 H 0.437(6) 0.126(5) -0.334(5) 0.030(19) Uiso 1 d . . . H7 H 0.420(5) 0.319(4) -0.324(4) 0.021(16) Uiso 1 d . . . H8 H 0.361(6) 0.507(5) -0.273(5) 0.03(2) Uiso 1 d . . . H9 H 0.234(6) 0.573(6) -0.121(5) 0.05(2) Uiso 1 d . . . H12 H 0.107(7) 0.596(6) 0.068(6) 0.06(3) Uiso 1 d . . . H13 H -0.040(7) 0.630(7) 0.245(6) 0.09(3) Uiso 1 d . . . H14 H -0.108(5) 0.458(4) 0.350(5) 0.024(16) Uiso 1 d . . . H15 H -0.033(4) 0.281(4) 0.267(4) 0.006(14) Uiso 1 d . . . H16 H -0.040(6) 0.031(5) 0.156(5) 0.04(2) Uiso 1 d . . . H17 H -0.100(8) -0.088(7) 0.331(7) 0.09(3) Uiso 1 d . . . H18 H 0.029(7) -0.118(7) 0.421(6) 0.07(3) Uiso 1 d . . . H19 H 0.208(5) -0.033(5) 0.375(5) 0.034(18) Uiso 1 d . . . H22 H 0.343(4) 0.301(4) 0.227(4) 0.005(13) Uiso 1 d . . . H23 H 0.483(5) 0.410(4) 0.172(4) 0.012(15) Uiso 1 d . . . H24 H 0.639(8) 0.399(7) -0.011(7) 0.08(3) Uiso 1 d . . . H26 H 0.490(6) 0.168(6) -0.072(6) 0.06(2) Uiso 1 d . . . H271 H 0.762(9) 0.260(9) -0.167(8) 0.11(5) Uiso 1 d . . . H272 H 0.669(9) 0.356(9) -0.222(9) 0.13(4) Uiso 1 d . . . H273 H 0.665(8) 0.252(8) -0.212(7) 0.08(4) Uiso 1 d . . . H28 H 0.082(7) 0.304(6) 0.425(6) 0.07(3) Uiso 1 d . . . H29 H 0.131(8) 0.489(7) 0.388(7) 0.08(3) Uiso 1 d . . . H30 H 0.249(6) 0.542(6) 0.419(5) 0.05(2) Uiso 1 d . . . H31 H 0.435(11) 0.388(9) 0.463(9) 0.15(5) Uiso 1 d . . . H32 H 0.437(11) 0.207(10) 0.484(9) 0.17(5) Uiso 1 d . . . H33 H 0.257(10) 0.155(8) 0.478(8) 0.12(5) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0323(3) 0.0274(3) 0.0321(3) -0.0013(2) -0.0098(3) -0.0104(2) Cl 0.0501(14) 0.0811(17) 0.0520(15) 0.0017(13) -0.0084(12) -0.0205(12) O1 0.033(3) 0.054(3) 0.070(4) -0.004(3) -0.014(3) -0.011(3) O2 0.069(4) 0.060(4) 0.060(4) -0.016(3) -0.040(3) 0.001(3) O3 0.053(4) 0.148(6) 0.094(5) 0.045(4) -0.032(4) -0.042(4) O4 0.077(6) 0.296(13) 0.245(11) -0.206(11) 0.019(7) -0.032(7) O5 0.107(6) 0.149(7) 0.087(5) 0.051(5) -0.050(4) -0.048(5) O6 0.146(7) 0.143(7) 0.163(8) 0.071(6) -0.071(6) -0.090(6) N1 0.034(3) 0.028(3) 0.040(4) -0.004(3) -0.016(3) -0.004(3) N2 0.034(3) 0.035(3) 0.027(3) 0.009(3) -0.011(3) -0.019(3) N3 0.034(3) 0.035(3) 0.034(4) -0.007(3) -0.015(3) -0.008(3) N4 0.040(4) 0.033(3) 0.031(3) 0.000(3) -0.013(3) -0.015(3) N5 0.048(4) 0.045(4) 0.037(4) 0.010(3) -0.020(3) -0.017(3) N6 0.043(4) 0.029(3) 0.038(4) 0.004(3) -0.013(3) -0.011(3) N7 0.048(4) 0.024(3) 0.050(4) 0.006(3) -0.026(4) -0.012(3) C1 0.042(5) 0.035(5) 0.055(6) -0.008(4) -0.022(4) 0.001(4) C2 0.067(6) 0.037(6) 0.069(7) -0.015(5) -0.024(5) 0.000(5) C3 0.068(6) 0.059(6) 0.056(6) -0.031(5) -0.004(5) -0.007(5) C4 0.054(5) 0.059(6) 0.038(5) -0.009(5) 0.003(4) -0.012(4) C5 0.041(4) 0.045(5) 0.029(4) -0.007(4) -0.014(4) -0.011(4) C6 0.033(4) 0.042(4) 0.028(4) 0.002(3) -0.005(3) -0.015(3) C7 0.037(5) 0.065(6) 0.032(5) -0.008(4) 0.000(4) -0.014(4) C8 0.062(6) 0.048(6) 0.040(6) 0.009(5) -0.011(5) -0.030(5) C9 0.050(5) 0.037(5) 0.045(5) 0.005(4) -0.021(4) -0.022(4) C10 0.030(4) 0.027(4) 0.033(4) 0.006(3) -0.012(3) -0.015(3) C11 0.032(4) 0.034(4) 0.038(4) 0.002(3) -0.013(3) -0.014(3) C12 0.046(5) 0.037(5) 0.040(5) -0.012(4) -0.020(4) -0.008(4) C13 0.049(5) 0.039(5) 0.051(6) -0.014(4) -0.023(4) 0.000(4) C14 0.042(5) 0.076(7) 0.028(5) -0.013(5) -0.006(4) 0.000(5) C15 0.043(5) 0.044(5) 0.039(5) -0.001(4) -0.009(4) -0.010(4) C16 0.049(5) 0.046(5) 0.044(5) -0.002(4) -0.017(4) -0.013(4) C17 0.069(7) 0.059(6) 0.049(6) 0.009(5) -0.012(5) -0.033(5) C18 0.092(8) 0.048(6) 0.044(6) 0.015(5) -0.016(6) -0.028(5) C19 0.070(6) 0.059(5) 0.041(5) 0.009(4) -0.031(5) -0.024(5) C20 0.052(5) 0.038(4) 0.036(4) -0.003(4) -0.013(4) -0.013(4) C21 0.031(4) 0.040(4) 0.050(5) 0.001(4) -0.025(4) -0.005(3) C22 0.041(5) 0.057(5) 0.034(5) -0.006(4) -0.007(4) -0.021(4) C23 0.059(6) 0.061(6) 0.057(6) -0.021(5) -0.017(5) -0.024(5) C24 0.045(6) 0.054(6) 0.075(7) 0.003(5) -0.017(5) -0.023(5) C25 0.039(5) 0.049(5) 0.054(5) -0.003(4) -0.010(4) -0.011(4) C26 0.031(4) 0.051(5) 0.055(6) -0.010(4) -0.013(4) -0.012(4) C27 0.054(8) 0.142(12) 0.059(8) -0.007(8) -0.002(6) -0.036(8) C28 0.072(9) 0.180(16) 0.075(8) 0.022(9) -0.044(7) -0.046(10) C29 0.100(11) 0.151(15) 0.052(7) 0.000(9) -0.029(7) 0.027(11) C30 0.125(12) 0.080(10) 0.070(8) -0.017(7) -0.031(8) -0.004(9) C31 0.068(9) 0.158(14) 0.060(7) -0.028(8) -0.026(6) -0.001(10) C32 0.078(9) 0.128(12) 0.068(8) -0.012(8) -0.032(7) 0.016(9) C33 0.119(12) 0.105(12) 0.060(7) 0.011(7) -0.027(8) -0.030(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N2 1.971(5) . ? Ru N6 1.989(6) . ? Ru N7 2.057(6) . ? Ru N4 2.057(5) . ? Ru N1 2.067(5) . ? Ru N3 2.076(5) . ? Cl O4 1.352(8) . ? Cl O5 1.392(6) . ? Cl O3 1.403(6) . ? Cl O6 1.414(7) . ? O1 N7 1.261(7) . ? O2 N7 1.230(7) . ? N1 C1 1.353(8) . ? N1 C5 1.373(8) . ? N2 C6 1.338(7) . ? N2 C10 1.366(7) . ? N3 C15 1.322(8) . ? N3 C11 1.364(7) . ? N4 C16 1.326(8) . ? N4 C20 1.352(8) . ? N5 N6 1.274(7) . ? N5 C20 1.389(8) . ? N6 C21 1.454(8) . ? C1 C2 1.382(11) . ? C2 C3 1.347(12) . ? C3 C4 1.382(11) . ? C4 C5 1.374(9) . ? C5 C6 1.448(9) . ? C6 C7 1.394(9) . ? C7 C8 1.383(11) . ? C8 C9 1.362(10) . ? C9 C10 1.381(8) . ? C10 C11 1.464(9) . ? C11 C12 1.392(9) . ? C12 C13 1.377(10) . ? C13 C14 1.370(10) . ? C14 C15 1.383(10) . ? C16 C17 1.375(11) . ? C17 C18 1.361(12) . ? C18 C19 1.376(11) . ? C19 C20 1.380(10) . ? C21 C22 1.364(9) . ? C21 C26 1.375(10) . ? C22 C23 1.385(10) . ? C23 C24 1.352(11) . ? C24 C25 1.380(11) . ? C25 C26 1.396(9) . ? C25 C27 1.506(12) . ? C28 C33 1.328(17) . ? C28 C29 1.336(18) . ? C29 C30 1.382(17) . ? C30 C31 1.303(16) . ? C31 C32 1.394(16) . ? C32 C33 1.383(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru N6 98.1(2) . . ? N2 Ru N7 90.0(2) . . ? N6 Ru N7 171.3(2) . . ? N2 Ru N4 173.4(2) . . ? N6 Ru N4 75.6(2) . . ? N7 Ru N4 96.1(2) . . ? N2 Ru N1 78.9(2) . . ? N6 Ru N1 97.2(2) . . ? N7 Ru N1 87.3(2) . . ? N4 Ru N1 103.8(2) . . ? N2 Ru N3 79.6(2) . . ? N6 Ru N3 89.8(2) . . ? N7 Ru N3 88.6(2) . . ? N4 Ru N3 98.0(2) . . ? N1 Ru N3 158.1(2) . . ? O4 Cl O5 110.9(7) . . ? O4 Cl O3 109.9(5) . . ? O5 Cl O3 110.8(4) . . ? O4 Cl O6 105.8(6) . . ? O5 Cl O6 107.5(5) . . ? O3 Cl O6 111.7(5) . . ? C1 N1 C5 119.0(6) . . ? C1 N1 Ru 127.3(5) . . ? C5 N1 Ru 113.3(4) . . ? C6 N2 C10 122.6(5) . . ? C6 N2 Ru 119.1(4) . . ? C10 N2 Ru 118.3(4) . . ? C15 N3 C11 119.1(6) . . ? C15 N3 Ru 127.7(5) . . ? C11 N3 Ru 113.1(4) . . ? C16 N4 C20 117.9(6) . . ? C16 N4 Ru 129.5(5) . . ? C20 N4 Ru 112.6(4) . . ? N6 N5 C20 110.7(6) . . ? N5 N6 C21 112.3(6) . . ? N5 N6 Ru 122.3(4) . . ? C21 N6 Ru 123.7(4) . . ? O2 N7 O1 117.6(6) . . ? O2 N7 Ru 122.7(5) . . ? O1 N7 Ru 119.7(5) . . ? N1 C1 C2 120.2(8) . . ? C3 C2 C1 121.9(9) . . ? C2 C3 C4 117.8(9) . . ? C5 C4 C3 120.7(8) . . ? N1 C5 C4 120.2(7) . . ? N1 C5 C6 115.3(6) . . ? C4 C5 C6 124.5(7) . . ? N2 C6 C7 119.5(6) . . ? N2 C6 C5 113.4(6) . . ? C7 C6 C5 127.1(6) . . ? C8 C7 C6 118.2(7) . . ? C9 C8 C7 121.5(8) . . ? C8 C9 C10 119.4(8) . . ? N2 C10 C9 118.8(6) . . ? N2 C10 C11 112.9(5) . . ? C9 C10 C11 128.3(6) . . ? N3 C11 C12 121.3(6) . . ? N3 C11 C10 115.8(6) . . ? C12 C11 C10 122.9(6) . . ? C13 C12 C11 118.6(8) . . ? C14 C13 C12 119.5(8) . . ? C13 C14 C15 119.6(7) . . ? N3 C15 C14 121.9(7) . . ? N4 C16 C17 122.1(8) . . ? C18 C17 C16 119.6(9) . . ? C17 C18 C19 120.1(9) . . ? C18 C19 C20 117.1(8) . . ? N4 C20 C19 123.3(7) . . ? N4 C20 N5 118.3(6) . . ? C19 C20 N5 118.4(7) . . ? C22 C21 C26 121.6(7) . . ? C22 C21 N6 119.8(6) . . ? C26 C21 N6 118.5(6) . . ? C21 C22 C23 118.9(7) . . ? C24 C23 C22 119.8(8) . . ? C23 C24 C25 122.3(8) . . ? C24 C25 C26 117.7(8) . . ? C24 C25 C27 120.2(9) . . ? C26 C25 C27 122.1(9) . . ? C21 C26 C25 119.6(7) . . ? C33 C28 C29 122.1(13) . . ? C28 C29 C30 118.0(13) . . ? C31 C30 C29 121.7(14) . . ? C30 C31 C32 120.6(14) . . ? C33 C32 C31 117.2(14) . . ? C28 C33 C32 120.3(14) . . ? 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 N2 Ru N1 C1 -173.5(6) . . . . ? N6 Ru N1 C1 89.6(6) . . . . ? N7 Ru N1 C1 -83.0(6) . . . . ? N4 Ru N1 C1 12.7(6) . . . . ? N3 Ru N1 C1 -162.5(5) . . . . ? N2 Ru N1 C5 -0.9(4) . . . . ? N6 Ru N1 C5 -97.8(4) . . . . ? N7 Ru N1 C5 89.6(4) . . . . ? N4 Ru N1 C5 -174.8(4) . . . . ? N3 Ru N1 C5 10.0(8) . . . . ? N6 Ru N2 C6 95.8(5) . . . . ? N7 Ru N2 C6 -87.3(5) . . . . ? N4 Ru N2 C6 115(2) . . . . ? N1 Ru N2 C6 0.0(5) . . . . ? N3 Ru N2 C6 -175.8(5) . . . . ? N6 Ru N2 C10 -85.5(5) . . . . ? N7 Ru N2 C10 91.4(5) . . . . ? N4 Ru N2 C10 -66(2) . . . . ? N1 Ru N2 C10 178.7(5) . . . . ? N3 Ru N2 C10 2.8(4) . . . . ? N2 Ru N3 C15 178.1(6) . . . . ? N6 Ru N3 C15 -83.6(6) . . . . ? N7 Ru N3 C15 87.9(6) . . . . ? N4 Ru N3 C15 -8.1(6) . . . . ? N1 Ru N3 C15 167.2(6) . . . . ? N2 Ru N3 C11 -4.8(4) . . . . ? N6 Ru N3 C11 93.4(4) . . . . ? N7 Ru N3 C11 -95.1(4) . . . . ? N4 Ru N3 C11 168.9(4) . . . . ? N1 Ru N3 C11 -15.8(8) . . . . ? N2 Ru N4 C16 161.0(19) . . . . ? N6 Ru N4 C16 -179.2(6) . . . . ? N7 Ru N4 C16 3.6(6) . . . . ? N1 Ru N4 C16 -85.2(6) . . . . ? N3 Ru N4 C16 93.0(6) . . . . ? N2 Ru N4 C20 -16(2) . . . . ? N6 Ru N4 C20 3.9(4) . . . . ? N7 Ru N4 C20 -173.3(5) . . . . ? N1 Ru N4 C20 97.9(4) . . . . ? N3 Ru N4 C20 -83.9(5) . . . . ? C20 N5 N6 C21 173.5(5) . . . . ? C20 N5 N6 Ru 7.4(7) . . . . ? N2 Ru N6 N5 171.2(5) . . . . ? N7 Ru N6 N5 12.2(19) . . . . ? N4 Ru N6 N5 -6.6(5) . . . . ? N1 Ru N6 N5 -109.1(5) . . . . ? N3 Ru N6 N5 91.7(5) . . . . ? N2 Ru N6 C21 6.7(5) . . . . ? N7 Ru N6 C21 -152.3(14) . . . . ? N4 Ru N6 C21 -171.1(5) . . . . ? N1 Ru N6 C21 86.4(5) . . . . ? N3 Ru N6 C21 -72.8(5) . . . . ? N2 Ru N7 O2 53.2(5) . . . . ? N6 Ru N7 O2 -147.6(14) . . . . ? N4 Ru N7 O2 -129.3(5) . . . . ? N1 Ru N7 O2 -25.7(5) . . . . ? N3 Ru N7 O2 132.8(5) . . . . ? N2 Ru N7 O1 -123.4(5) . . . . ? N6 Ru N7 O1 35.8(18) . . . . ? N4 Ru N7 O1 54.1(5) . . . . ? N1 Ru N7 O1 157.7(5) . . . . ? N3 Ru N7 O1 -43.8(5) . . . . ? C5 N1 C1 C2 1.6(10) . . . . ? Ru N1 C1 C2 173.7(6) . . . . ? N1 C1 C2 C3 1.5(13) . . . . ? C1 C2 C3 C4 -1.2(14) . . . . ? C2 C3 C4 C5 -2.3(14) . . . . ? C1 N1 C5 C4 -5.0(10) . . . . ? Ru N1 C5 C4 -178.2(6) . . . . ? C1 N1 C5 C6 174.8(6) . . . . ? Ru N1 C5 C6 1.6(7) . . . . ? C3 C4 C5 N1 5.4(12) . . . . ? C3 C4 C5 C6 -174.4(7) . . . . ? C10 N2 C6 C7 2.3(10) . . . . ? Ru N2 C6 C7 -179.1(5) . . . . ? C10 N2 C6 C5 -177.7(5) . . . . ? Ru N2 C6 C5 0.8(7) . . . . ? N1 C5 C6 N2 -1.6(8) . . . . ? C4 C5 C6 N2 178.2(7) . . . . ? N1 C5 C6 C7 178.3(7) . . . . ? C4 C5 C6 C7 -1.9(12) . . . . ? N2 C6 C7 C8 -2.2(11) . . . . ? C5 C6 C7 C8 177.9(7) . . . . ? C6 C7 C8 C9 1.1(12) . . . . ? C7 C8 C9 C10 0.0(12) . . . . ? C6 N2 C10 C9 -1.2(9) . . . . ? Ru N2 C10 C9 -179.8(5) . . . . ? C6 N2 C10 C11 178.2(6) . . . . ? Ru N2 C10 C11 -0.3(7) . . . . ? C8 C9 C10 N2 0.0(10) . . . . ? C8 C9 C10 C11 -179.3(7) . . . . ? C15 N3 C11 C12 1.7(9) . . . . ? Ru N3 C11 C12 -175.6(5) . . . . ? C15 N3 C11 C10 -176.5(6) . . . . ? Ru N3 C11 C10 6.1(7) . . . . ? N2 C10 C11 N3 -4.0(8) . . . . ? C9 C10 C11 N3 175.4(6) . . . . ? N2 C10 C11 C12 177.8(6) . . . . ? C9 C10 C11 C12 -2.8(11) . . . . ? N3 C11 C12 C13 -0.4(10) . . . . ? C10 C11 C12 C13 177.7(6) . . . . ? C11 C12 C13 C14 -2.0(11) . . . . ? C12 C13 C14 C15 3.0(11) . . . . ? C11 N3 C15 C14 -0.7(10) . . . . ? Ru N3 C15 C14 176.2(5) . . . . ? C13 C14 C15 N3 -1.6(11) . . . . ? C20 N4 C16 C17 0.9(11) . . . . ? Ru N4 C16 C17 -175.9(6) . . . . ? N4 C16 C17 C18 -0.5(13) . . . . ? C16 C17 C18 C19 0.2(14) . . . . ? C17 C18 C19 C20 -0.3(13) . . . . ? C16 N4 C20 C19 -1.1(10) . . . . ? Ru N4 C20 C19 176.2(6) . . . . ? C16 N4 C20 N5 -178.9(6) . . . . ? Ru N4 C20 N5 -1.6(7) . . . . ? C18 C19 C20 N4 0.8(12) . . . . ? C18 C19 C20 N5 178.6(7) . . . . ? N6 N5 C20 N4 -3.4(8) . . . . ? N6 N5 C20 C19 178.7(6) . . . . ? N5 N6 C21 C22 -54.7(8) . . . . ? Ru N6 C21 C22 111.2(7) . . . . ? N5 N6 C21 C26 128.8(7) . . . . ? Ru N6 C21 C26 -65.3(8) . . . . ? C26 C21 C22 C23 0.9(11) . . . . ? N6 C21 C22 C23 -175.6(7) . . . . ? C21 C22 C23 C24 0.7(13) . . . . ? C22 C23 C24 C25 -2.7(14) . . . . ? C23 C24 C25 C26 3.1(13) . . . . ? C23 C24 C25 C27 -178.2(10) . . . . ? C22 C21 C26 C25 -0.4(11) . . . . ? N6 C21 C26 C25 176.1(6) . . . . ? C24 C25 C26 C21 -1.5(11) . . . . ? C27 C25 C26 C21 179.8(10) . . . . ? C33 C28 C29 C30 -1(2) . . . . ? C28 C29 C30 C31 -1.0(18) . . . . ? C29 C30 C31 C32 1.5(18) . . . . ? C30 C31 C32 C33 0.1(16) . . . . ? C29 C28 C33 C32 3(2) . . . . ? C31 C32 C33 C28 -2.3(17) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.93 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.710 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.111