# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2186 data_global loop_ _publ_author_name 'G.K.Lahiri' 'B.Mondai' 'M.G.Walawalkar' _publ_requested_journal 'J.Chem.Soc.,Dalton Trans.' data_gkl005 _database_code_CSD 001984 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20 Cl2 N6 O4 Ru' _chemical_formula_weight 652.45 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' 'O' 'O' 0.0106 0.0060 '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' 'Cl' 'Cl' 0.1484 0.1585 '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 8.5989(18) _cell_length_b 15.974(3) _cell_length_c 19.496(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.388(18) _cell_angle_gamma 90.00 _cell_volume 2642.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour violet _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 92.5% _exptl_absorpt_correction_T_max 100% _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <15% _diffrn_reflns_number 4922 _diffrn_reflns_av_R_equivalents 0.0108 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4640 _reflns_number_gt 3998 _reflns_threshold_expression >2sigma(I) _computing_data_collection Argus _computing_cell_refinement Argus _computing_data_reduction Maxus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Platon _computing_publication_material CIFTAB (Sheldrick,1997) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+1.8497P] 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 4640 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.94968(3) 0.901761(14) 0.187792(11) 0.03263(9) Uani 1 1 d . . . Cl1 Cl 0.82995(9) 1.03468(5) 0.15314(4) 0.04648(19) Uani 1 1 d . . . Cl2 Cl 0.75987(11) 1.31220(6) 0.05360(4) 0.0559(2) Uani 1 1 d . . . N1 N 0.7311(3) 0.85211(16) 0.19596(13) 0.0397(6) Uani 1 1 d . . . N2 N 0.8787(3) 0.86437(15) 0.09129(12) 0.0398(6) Uani 1 1 d . . . N3 N 1.1413(3) 0.93741(16) 0.14222(13) 0.0407(6) Uani 1 1 d . . . N4 N 1.0387(3) 0.93796(16) 0.28765(12) 0.0382(5) Uani 1 1 d . . . N5 N 1.1152(3) 0.79687(17) 0.29528(13) 0.0445(6) Uani 1 1 d . . . N6 N 1.0425(3) 0.79821(15) 0.23113(12) 0.0351(5) Uani 1 1 d . . . C1 C 0.6667(4) 0.8432(2) 0.25410(18) 0.0501(8) Uani 1 1 d . . . H1 H 0.7160 0.8682 0.2950 0.060 Uiso 1 1 calc R . . C2 C 0.5304(4) 0.7981(3) 0.2550(2) 0.0695(11) Uani 1 1 d . . . H2 H 0.4892 0.7923 0.2959 0.083 Uiso 1 1 calc R . . C3 C 0.4564(4) 0.7621(3) 0.1945(3) 0.0775(13) Uani 1 1 d . . . H3 H 0.3644 0.7315 0.1943 0.093 Uiso 1 1 calc R . . C4 C 0.5191(4) 0.7715(2) 0.1340(2) 0.0637(10) Uani 1 1 d . . . H4 H 0.4697 0.7475 0.0927 0.076 Uiso 1 1 calc R . . C5 C 0.6558(4) 0.8170(2) 0.13590(17) 0.0461(7) Uani 1 1 d . . . C6 C 0.7340(4) 0.8296(2) 0.07488(16) 0.0464(7) Uani 1 1 d . . . C7 C 0.6776(5) 0.8098(2) 0.00584(19) 0.0626(10) Uani 1 1 d . . . H7 H 0.5787 0.7856 -0.0068 0.075 Uiso 1 1 calc R . . C8 C 0.7722(6) 0.8271(2) -0.04400(18) 0.0700(12) Uani 1 1 d . . . H8 H 0.7353 0.8146 -0.0904 0.084 Uiso 1 1 calc R . . C9 C 0.9185(5) 0.8620(2) -0.02597(17) 0.0608(10) Uani 1 1 d . . . H9 H 0.9811 0.8729 -0.0596 0.073 Uiso 1 1 calc R . . C10 C 0.9718(4) 0.8811(2) 0.04345(16) 0.0473(8) Uani 1 1 d . . . C11 C 1.1237(4) 0.91848(19) 0.07331(17) 0.0461(7) Uani 1 1 d . . . C12 C 1.2477(5) 0.9324(3) 0.0361(2) 0.0644(11) Uani 1 1 d . . . H12 H 1.2372 0.9187 -0.0108 0.077 Uiso 1 1 calc R . . C13 C 1.3855(5) 0.9669(3) 0.0706(2) 0.0721(12) Uani 1 1 d . . . H13 H 1.4700 0.9749 0.0471 0.087 Uiso 1 1 calc R . . C14 C 1.3998(4) 0.9893(3) 0.1387(2) 0.0635(10) Uani 1 1 d . . . H14 H 1.4911 1.0149 0.1613 0.076 Uiso 1 1 calc R . . C15 C 1.2764(4) 0.9733(2) 0.1730(2) 0.0510(8) Uani 1 1 d . . . H15 H 1.2863 0.9879 0.2197 0.061 Uiso 1 1 calc R . . C16 C 1.0335(4) 1.0130(2) 0.31824(17) 0.0515(8) Uani 1 1 d . . . H16 H 0.9786 1.0563 0.2932 0.062 Uiso 1 1 calc R . . C17 C 1.1065(5) 1.0279(2) 0.38533(19) 0.0644(10) Uani 1 1 d . . . H17 H 1.0985 1.0802 0.4055 0.077 Uiso 1 1 calc R . . C18 C 1.1911(5) 0.9651(3) 0.4223(2) 0.0685(11) Uani 1 1 d . . . H18 H 1.2426 0.9749 0.4674 0.082 Uiso 1 1 calc R . . C19 C 1.1989(5) 0.8886(2) 0.39263(18) 0.0601(10) Uani 1 1 d . . . H19 H 1.2564 0.8455 0.4169 0.072 Uiso 1 1 calc R . . C20 C 1.1196(4) 0.87572(19) 0.32557(15) 0.0411(7) Uani 1 1 d . . . C21 C 1.0089(3) 0.71667(18) 0.20164(15) 0.0369(6) Uani 1 1 d . . . C22 C 0.9302(4) 0.6584(2) 0.23661(18) 0.0519(8) Uani 1 1 d . . . H22 H 0.9068 0.6701 0.2805 0.062 Uiso 1 1 calc R . . C23 C 0.8876(5) 0.5826(2) 0.2047(2) 0.0643(10) Uani 1 1 d . . . H23 H 0.8338 0.5434 0.2271 0.077 Uiso 1 1 calc R . . C24 C 0.9238(5) 0.5644(2) 0.1400(2) 0.0687(11) Uani 1 1 d . . . H24 H 0.8949 0.5131 0.1192 0.082 Uiso 1 1 calc R . . C25 C 1.0022(5) 0.6220(2) 0.10622(19) 0.0573(9) Uani 1 1 d . . . H25 H 1.0271 0.6094 0.0627 0.069 Uiso 1 1 calc R . . C26 C 1.0446(4) 0.6988(2) 0.13641(16) 0.0453(7) Uani 1 1 d . . . H26 H 1.0966 0.7380 0.1131 0.054 Uiso 1 1 calc R . . O1 O 0.6987(7) 1.2550(3) 0.0947(2) 0.169(2) Uani 1 1 d . . . O2 O 0.9118(5) 1.3318(5) 0.0780(2) 0.192(3) Uani 1 1 d . . . O3 O 0.6777(10) 1.3817(4) 0.0600(4) 0.232(4) Uani 1 1 d . . . O4 O 0.7437(5) 1.2869(3) -0.01560(17) 0.1300(16) 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 0.03307(13) 0.03637(14) 0.02839(13) 0.00145(9) 0.00478(9) -0.00088(9) Cl1 0.0517(4) 0.0451(4) 0.0438(4) 0.0076(3) 0.0114(3) 0.0088(3) Cl2 0.0648(5) 0.0566(5) 0.0447(4) -0.0038(4) 0.0039(4) 0.0007(4) N1 0.0358(13) 0.0431(14) 0.0386(13) 0.0040(11) 0.0016(10) -0.0009(11) N2 0.0503(15) 0.0371(13) 0.0299(12) -0.0005(10) 0.0003(11) 0.0060(11) N3 0.0431(14) 0.0398(13) 0.0414(14) 0.0069(11) 0.0131(11) 0.0048(11) N4 0.0376(13) 0.0427(14) 0.0338(12) -0.0010(11) 0.0047(10) -0.0058(11) N5 0.0421(14) 0.0497(15) 0.0382(14) 0.0047(12) -0.0039(11) -0.0015(12) N6 0.0307(12) 0.0397(13) 0.0353(13) 0.0013(10) 0.0064(10) -0.0011(10) C1 0.0382(17) 0.063(2) 0.0492(19) 0.0084(16) 0.0081(14) -0.0034(15) C2 0.046(2) 0.091(3) 0.071(3) 0.023(2) 0.0105(18) -0.012(2) C3 0.043(2) 0.082(3) 0.104(4) 0.019(3) 0.000(2) -0.021(2) C4 0.050(2) 0.060(2) 0.074(3) 0.0023(19) -0.0113(19) -0.0109(18) C5 0.0398(16) 0.0427(17) 0.0509(19) 0.0019(14) -0.0072(14) 0.0000(13) C6 0.0535(19) 0.0405(16) 0.0409(17) -0.0040(13) -0.0053(14) 0.0058(14) C7 0.075(2) 0.051(2) 0.052(2) -0.0107(17) -0.0183(19) 0.0032(18) C8 0.113(4) 0.058(2) 0.0328(18) -0.0086(16) -0.005(2) 0.019(2) C9 0.094(3) 0.053(2) 0.0347(18) 0.0011(15) 0.0100(18) 0.013(2) C10 0.068(2) 0.0412(17) 0.0339(16) 0.0042(13) 0.0115(15) 0.0151(15) C11 0.0556(19) 0.0417(17) 0.0436(17) 0.0123(14) 0.0157(15) 0.0107(14) C12 0.083(3) 0.066(2) 0.052(2) 0.0210(18) 0.035(2) 0.021(2) C13 0.056(2) 0.080(3) 0.088(3) 0.030(2) 0.035(2) 0.005(2) C14 0.048(2) 0.069(2) 0.077(3) 0.020(2) 0.0222(19) -0.0019(18) C15 0.0402(17) 0.0521(19) 0.062(2) 0.0069(16) 0.0133(15) -0.0020(15) C16 0.058(2) 0.0453(18) 0.0490(19) -0.0063(15) 0.0032(16) -0.0007(15) C17 0.081(3) 0.057(2) 0.051(2) -0.0179(18) 0.0001(19) -0.006(2) C18 0.088(3) 0.065(2) 0.044(2) -0.0054(18) -0.0145(19) -0.019(2) C19 0.070(2) 0.058(2) 0.0448(19) 0.0063(16) -0.0131(17) -0.0087(18) C20 0.0426(16) 0.0426(16) 0.0361(16) 0.0023(13) 0.0008(13) -0.0069(14) C21 0.0338(14) 0.0373(15) 0.0385(15) 0.0019(12) 0.0025(12) 0.0026(12) C22 0.058(2) 0.0486(19) 0.0501(19) 0.0022(15) 0.0120(16) -0.0092(16) C23 0.076(3) 0.046(2) 0.071(3) 0.0039(18) 0.013(2) -0.0165(18) C24 0.083(3) 0.045(2) 0.075(3) -0.0126(19) 0.003(2) -0.012(2) C25 0.071(2) 0.0499(19) 0.051(2) -0.0105(16) 0.0107(18) 0.0043(18) C26 0.0472(18) 0.0451(18) 0.0442(17) 0.0036(14) 0.0090(14) 0.0028(14) O1 0.242(6) 0.163(4) 0.093(3) 0.037(3) 0.001(3) -0.108(4) O2 0.104(3) 0.355(9) 0.109(3) -0.059(4) -0.002(3) -0.088(5) O3 0.293(9) 0.156(5) 0.275(9) 0.038(5) 0.128(7) 0.124(6) O4 0.121(3) 0.206(5) 0.061(2) -0.051(3) 0.0090(19) -0.045(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N6 1.966(2) . ? Ru1 N2 1.973(2) . ? Ru1 N4 2.055(2) . ? Ru1 N1 2.070(2) . ? Ru1 N3 2.075(2) . ? Ru1 Cl1 2.4078(9) . ? Cl2 O3 1.333(5) . ? Cl2 O2 1.352(4) . ? Cl2 O1 1.376(4) . ? Cl2 O4 1.393(3) . ? N1 C1 1.348(4) . ? N1 C5 1.363(4) . ? N2 C10 1.351(4) . ? N2 C6 1.352(4) . ? N3 C15 1.346(4) . ? N3 C11 1.361(4) . ? N4 C16 1.342(4) . ? N4 C20 1.361(4) . ? N5 N6 1.304(3) . ? N5 C20 1.389(4) . ? N6 C21 1.434(4) . ? C1 C2 1.378(5) . ? C2 C3 1.370(6) . ? C3 C4 1.383(6) . ? C4 C5 1.377(5) . ? C5 C6 1.473(5) . ? C6 C7 1.391(5) . ? C7 C8 1.393(6) . ? C8 C9 1.369(6) . ? C9 C10 1.390(5) . ? C10 C11 1.468(5) . ? C11 C12 1.401(5) . ? C12 C13 1.379(6) . ? C13 C14 1.361(6) . ? C14 C15 1.367(5) . ? C16 C17 1.376(5) . ? C17 C18 1.372(5) . ? C18 C19 1.360(5) . ? C19 C20 1.388(4) . ? C21 C26 1.386(4) . ? C21 C22 1.393(4) . ? C22 C23 1.382(5) . ? C23 C24 1.378(6) . ? C24 C25 1.371(6) . ? C25 C26 1.383(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ru1 N2 101.29(10) . . ? N6 Ru1 N4 76.55(10) . . ? N2 Ru1 N4 176.13(10) . . ? N6 Ru1 N1 87.40(9) . . ? N2 Ru1 N1 79.27(10) . . ? N4 Ru1 N1 103.73(10) . . ? N6 Ru1 N3 96.88(9) . . ? N2 Ru1 N3 79.56(11) . . ? N4 Ru1 N3 97.44(10) . . ? N1 Ru1 N3 158.82(10) . . ? N6 Ru1 Cl1 170.86(7) . . ? N2 Ru1 Cl1 87.01(7) . . ? N4 Ru1 Cl1 95.38(8) . . ? N1 Ru1 Cl1 90.43(7) . . ? N3 Ru1 Cl1 88.34(7) . . ? O3 Cl2 O2 105.7(5) . . ? O3 Cl2 O1 103.9(4) . . ? O2 Cl2 O1 112.9(4) . . ? O3 Cl2 O4 111.2(4) . . ? O2 Cl2 O4 110.2(3) . . ? O1 Cl2 O4 112.6(3) . . ? C1 N1 C5 118.4(3) . . ? C1 N1 Ru1 127.4(2) . . ? C5 N1 Ru1 113.7(2) . . ? C10 N2 C6 122.9(3) . . ? C10 N2 Ru1 118.2(2) . . ? C6 N2 Ru1 118.6(2) . . ? C15 N3 C11 119.0(3) . . ? C15 N3 Ru1 127.9(2) . . ? C11 N3 Ru1 113.2(2) . . ? C16 N4 C20 117.5(3) . . ? C16 N4 Ru1 129.6(2) . . ? C20 N4 Ru1 112.8(2) . . ? N6 N5 C20 111.6(2) . . ? N5 N6 C21 113.8(2) . . ? N5 N6 Ru1 121.56(19) . . ? C21 N6 Ru1 123.42(18) . . ? N1 C1 C2 122.2(3) . . ? C3 C2 C1 119.0(4) . . ? C2 C3 C4 119.8(4) . . ? C5 C4 C3 119.0(4) . . ? N1 C5 C4 121.6(3) . . ? N1 C5 C6 115.0(3) . . ? C4 C5 C6 123.4(3) . . ? N2 C6 C7 119.0(3) . . ? N2 C6 C5 112.9(3) . . ? C7 C6 C5 128.1(3) . . ? C6 C7 C8 118.6(4) . . ? C9 C8 C7 121.2(3) . . ? C8 C9 C10 118.9(4) . . ? N2 C10 C9 119.4(3) . . ? N2 C10 C11 113.3(3) . . ? C9 C10 C11 127.3(3) . . ? N3 C11 C12 120.3(3) . . ? N3 C11 C10 115.5(3) . . ? C12 C11 C10 124.2(3) . . ? C13 C12 C11 118.4(4) . . ? C14 C13 C12 121.0(4) . . ? C13 C14 C15 118.3(4) . . ? N3 C15 C14 122.9(4) . . ? N4 C16 C17 122.3(3) . . ? C18 C17 C16 119.6(3) . . ? C19 C18 C17 119.5(3) . . ? C18 C19 C20 118.9(3) . . ? N4 C20 C19 122.2(3) . . ? N4 C20 N5 117.1(3) . . ? C19 C20 N5 120.7(3) . . ? C26 C21 C22 120.6(3) . . ? C26 C21 N6 119.7(3) . . ? C22 C21 N6 119.6(3) . . ? C23 C22 C21 118.6(3) . . ? C24 C23 C22 121.0(4) . . ? C25 C24 C23 120.0(3) . . ? C24 C25 C26 120.4(3) . . ? C25 C26 C21 119.4(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.629 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.065 data_gkl10 _database_code_CSD 001985 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H24 Cl2 N6 O10 Ru' _chemical_formula_weight 752.48 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' 'O' 'O' 0.0106 0.0060 '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' _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_cell_setting 'Monoclinic' 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 9.2970(9) _cell_length_b 16.4020(9) _cell_length_c 20.1100(15) _cell_angle_alpha 90.00 _cell_angle_beta 103.076(7) _cell_angle_gamma 90.00 _cell_volume 2987.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.3700 _cell_measurement_theta_max 13.3300 _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.980 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; psi-scan (North, Philips & Mathews, 1968) ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf Nonius CAD4, 1989' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5392 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.92 _reflns_number_total 5236 _reflns_number_gt 3422 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Enraf Nonius CAD4, 1989' _computing_data_collection 'Enraf Nonius CAD4, 1989' _computing_data_reduction 'maXus (Mackay et al., 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maXus (Mackay et al., 1999)' _computing_publication_material ciftab _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^)+(0.0168P)^2^+15.1522P] 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 5236 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.06541(6) 0.19302(3) 0.85817(3) 0.03301(16) Uani 1 1 d . . . O30 O 0.2617(5) 0.1330(3) 0.9120(2) 0.0513(13) Uani 1 1 d . . . H30A H 0.3379 0.1259 0.8919 0.080 Uiso 1 1 d R . . H30B H 0.2679 0.1147 0.9548 0.080 Uiso 1 1 d R . . N1 N 0.1652(6) 0.2058(3) 0.7766(3) 0.0398(13) Uani 1 1 d . . . N2 N 0.0056(6) 0.0902(3) 0.8095(3) 0.0331(12) Uani 1 1 d . . . N3 N -0.0431(6) 0.1355(3) 0.9243(3) 0.0403(14) Uani 1 1 d . . . N4 N 0.1057(6) 0.3067(3) 0.9008(3) 0.0360(12) Uani 1 1 d . . . N5 N -0.1143(6) 0.3332(3) 0.8221(3) 0.0448(15) Uani 1 1 d . . . N6 N -0.1019(6) 0.2574(3) 0.8106(3) 0.0359(13) Uani 1 1 d . . . C1 C 0.2501(9) 0.2676(5) 0.7642(4) 0.056(2) Uani 1 1 d . . . H1 H 0.2789 0.3091 0.7983 0.080 Uiso 1 1 d R . . C2 C 0.2999(9) 0.2727(5) 0.7051(4) 0.062(2) Uani 1 1 d . . . H2 H 0.3586 0.3180 0.6966 0.080 Uiso 1 1 d R . . C3 C 0.2619(10) 0.2125(6) 0.6578(5) 0.070(3) Uani 1 1 d . . . H3 H 0.2975 0.2145 0.6166 0.080 Uiso 1 1 d R . . C4 C 0.1770(9) 0.1477(5) 0.6703(4) 0.053(2) Uani 1 1 d . . . H4 H 0.1498 0.1058 0.6365 0.080 Uiso 1 1 d R . . C5 C 0.1287(8) 0.1440(4) 0.7300(3) 0.0401(16) Uani 1 1 d . . . C6 C 0.0401(7) 0.0787(4) 0.7489(3) 0.0396(16) Uani 1 1 d . . . C7 C -0.0064(9) 0.0099(5) 0.7106(4) 0.055(2) Uani 1 1 d . . . H7 H 0.0127 0.0015 0.6661 0.080 Uiso 1 1 d R . . C8 C -0.0885(9) -0.0461(5) 0.7367(4) 0.063(2) Uani 1 1 d . . . H8 H -0.1226 -0.0948 0.7116 0.080 Uiso 1 1 d R . . C9 C -0.1222(8) -0.0349(5) 0.7994(4) 0.0501(19) Uani 1 1 d . . . H9 H -0.1786 -0.0749 0.8173 0.080 Uiso 1 1 d R . . C10 C -0.0724(8) 0.0353(4) 0.8361(3) 0.0406(16) Uani 1 1 d . . . C11 C -0.0984(7) 0.0609(4) 0.9016(4) 0.0405(16) Uani 1 1 d . . . C12 C -0.1769(9) 0.0153(5) 0.9391(4) 0.058(2) Uani 1 1 d . . . H12 H -0.2195 -0.0364 0.9232 0.080 Uiso 1 1 d R . . C13 C -0.1984(10) 0.0459(6) 1.0010(5) 0.069(3) Uani 1 1 d . . . H13 H -0.2507 0.0148 1.0284 0.080 Uiso 1 1 d R . . C14 C -0.1389(11) 0.1189(6) 1.0232(5) 0.070(3) Uani 1 1 d . . . H14 H -0.1536 0.1408 1.0654 0.080 Uiso 1 1 d R . . C15 C -0.0638(9) 0.1628(5) 0.9841(4) 0.052(2) Uani 1 1 d . . . H15 H -0.0205 0.2141 1.0007 0.080 Uiso 1 1 d R . . C16 C 0.2221(8) 0.3353(5) 0.9475(4) 0.053(2) Uani 1 1 d . . . H16 H 0.3001 0.2977 0.9660 0.080 Uiso 1 1 d R . . C17 C 0.2304(9) 0.4143(5) 0.9692(4) 0.056(2) Uani 1 1 d . . . H17 H 0.3149 0.4318 1.0031 0.080 Uiso 1 1 d R . . C18 C 0.1198(10) 0.4678(5) 0.9429(5) 0.063(2) Uani 1 1 d . . . H18 H 0.1247 0.5234 0.9582 0.080 Uiso 1 1 d R . . C19 C 0.0010(9) 0.4416(5) 0.8943(4) 0.054(2) Uani 1 1 d . . . H19 H -0.0773 0.4788 0.8754 0.080 Uiso 1 1 d R . . C20 C -0.0014(8) 0.3611(4) 0.8737(4) 0.0439(17) Uani 1 1 d . . . C21 C -0.2064(7) 0.2270(4) 0.7503(3) 0.0361(15) Uani 1 1 d . . . C22 C -0.1934(8) 0.2542(5) 0.6878(4) 0.0495(19) Uani 1 1 d . . . H22 H -0.1238 0.2954 0.6822 0.080 Uiso 1 1 d R . . C23 C -0.2832(9) 0.2199(5) 0.6315(4) 0.059(2) Uani 1 1 d . . . H23 H -0.2748 0.2367 0.5868 0.080 Uiso 1 1 d R . . C24 C -0.3844(9) 0.1623(5) 0.6373(4) 0.062(2) Uani 1 1 d . . . H24 H -0.4442 0.1390 0.5965 0.080 Uiso 1 1 d R . . C25 C -0.4000(9) 0.1382(5) 0.7002(5) 0.063(2) Uani 1 1 d . . . H25 H -0.4741 0.0985 0.7033 0.080 Uiso 1 1 d R . . C26 C -0.3080(8) 0.1704(5) 0.7587(4) 0.0492(19) Uani 1 1 d . . . H26 H -0.3196 0.1539 0.8030 0.080 Uiso 1 1 d R . . Cl1 Cl 0.4103(2) -0.02459(13) 0.81975(11) 0.0577(5) Uani 1 1 d . . . O11 O 0.2928(10) -0.0438(5) 0.8501(4) 0.125(3) Uani 1 1 d . . . O12 O 0.4419(9) 0.0588(4) 0.8319(4) 0.099(2) Uani 1 1 d . . . O13 O 0.3608(10) -0.0386(5) 0.7488(4) 0.121(3) Uani 1 1 d . . . O14 O 0.5274(8) -0.0750(5) 0.8453(5) 0.144(4) Uani 1 1 d . . . Cl2 Cl -0.3509(3) 0.34050(14) 0.95776(11) 0.0646(6) Uani 1 1 d . . . O21 O -0.4255(8) 0.3219(7) 1.0077(4) 0.145(4) Uani 1 1 d . . . O22 O -0.3852(12) 0.4183(6) 0.9344(5) 0.166(4) Uani 1 1 d . . . O23 O -0.1967(8) 0.3387(4) 0.9872(4) 0.101(2) Uani 1 1 d . . . O24 O -0.3900(14) 0.2882(8) 0.9063(6) 0.202(6) Uani 1 1 d . . . O27 O 0.4395(8) 0.1728(4) 1.0300(3) 0.094(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 0.0375(3) 0.0285(3) 0.0317(3) -0.0012(2) 0.0051(2) 0.0022(2) O30 0.053(3) 0.057(3) 0.043(3) 0.001(2) 0.008(2) 0.016(3) N1 0.044(3) 0.036(3) 0.039(3) 0.003(3) 0.008(3) 0.004(3) N2 0.034(3) 0.029(3) 0.033(3) -0.007(2) 0.001(2) 0.004(2) N3 0.041(3) 0.040(3) 0.039(3) 0.004(3) 0.008(3) 0.010(3) N4 0.035(3) 0.039(3) 0.032(3) -0.004(3) 0.005(2) -0.002(3) N5 0.046(4) 0.036(3) 0.050(4) -0.002(3) 0.005(3) 0.007(3) N6 0.029(3) 0.040(3) 0.038(3) 0.003(3) 0.006(2) -0.001(2) C1 0.059(5) 0.043(5) 0.070(6) -0.001(4) 0.025(4) -0.006(4) C2 0.065(6) 0.063(5) 0.069(6) 0.004(5) 0.038(5) -0.013(4) C3 0.066(6) 0.094(8) 0.054(5) 0.024(5) 0.020(4) 0.008(5) C4 0.061(5) 0.062(5) 0.038(4) -0.007(4) 0.014(4) 0.004(4) C5 0.044(4) 0.040(4) 0.035(4) 0.001(3) 0.007(3) 0.003(3) C6 0.030(3) 0.043(4) 0.039(4) -0.009(3) -0.006(3) 0.002(3) C7 0.054(5) 0.061(5) 0.050(5) -0.018(4) 0.014(4) -0.007(4) C8 0.057(5) 0.057(5) 0.069(6) -0.024(5) 0.000(4) 0.000(4) C9 0.047(4) 0.043(4) 0.056(5) -0.004(4) 0.003(4) -0.012(4) C10 0.043(4) 0.037(4) 0.041(4) -0.001(3) 0.008(3) -0.008(3) C11 0.037(4) 0.032(4) 0.052(4) 0.001(3) 0.009(3) 0.002(3) C12 0.058(5) 0.048(5) 0.069(6) 0.007(4) 0.018(4) -0.010(4) C13 0.068(6) 0.078(7) 0.072(6) 0.026(5) 0.039(5) 0.017(5) C14 0.093(7) 0.067(6) 0.063(6) 0.003(5) 0.042(5) 0.013(5) C15 0.066(5) 0.053(5) 0.044(4) 0.004(4) 0.025(4) 0.012(4) C16 0.049(5) 0.055(5) 0.050(5) -0.013(4) 0.000(4) 0.007(4) C17 0.061(5) 0.046(5) 0.057(5) -0.020(4) 0.006(4) -0.014(4) C18 0.077(6) 0.032(4) 0.080(6) -0.006(4) 0.018(5) -0.003(4) C19 0.062(5) 0.046(4) 0.053(5) -0.018(4) 0.016(4) 0.005(4) C20 0.044(4) 0.044(4) 0.043(4) 0.002(3) 0.009(3) 0.003(3) C21 0.034(4) 0.034(4) 0.035(4) 0.000(3) -0.001(3) 0.007(3) C22 0.049(4) 0.055(5) 0.041(4) 0.012(4) 0.002(3) -0.005(4) C23 0.071(6) 0.070(6) 0.032(4) 0.000(4) 0.002(4) -0.004(5) C24 0.064(6) 0.062(5) 0.050(5) -0.010(4) -0.005(4) -0.008(4) C25 0.046(5) 0.057(5) 0.080(6) 0.000(5) 0.000(4) -0.008(4) C26 0.045(4) 0.052(5) 0.045(4) 0.008(4) -0.001(3) -0.005(4) Cl1 0.0615(13) 0.0522(12) 0.0620(13) -0.0014(10) 0.0195(10) 0.0119(10) O11 0.146(8) 0.125(7) 0.138(7) -0.005(6) 0.104(6) -0.012(6) O12 0.143(7) 0.059(4) 0.111(6) -0.009(4) 0.061(5) -0.011(4) O13 0.166(8) 0.134(7) 0.062(5) -0.017(5) 0.024(5) -0.010(6) O14 0.079(5) 0.112(7) 0.219(10) -0.029(7) -0.010(6) 0.048(5) Cl2 0.0738(15) 0.0656(14) 0.0546(13) 0.0019(11) 0.0152(11) -0.0043(11) O21 0.077(5) 0.291(13) 0.068(5) 0.047(7) 0.016(4) -0.021(7) O22 0.203(11) 0.109(7) 0.164(9) 0.060(7) -0.001(8) 0.045(7) O23 0.068(5) 0.092(5) 0.144(7) 0.000(5) 0.027(5) 0.001(4) O24 0.223(12) 0.236(14) 0.146(9) -0.110(9) 0.040(8) -0.099(11) O27 0.097(5) 0.101(6) 0.070(4) -0.005(4) -0.013(4) -0.005(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 N6 1.944(5) . ? Ru1 N2 1.967(5) . ? Ru1 N4 2.051(5) . ? Ru1 N1 2.069(6) . ? Ru1 N3 2.069(6) . ? Ru1 O30 2.140(5) . ? O30 H30A 0.9000 . ? O30 H30B 0.9000 . ? N1 C1 1.343(9) . ? N1 C5 1.370(8) . ? N2 C10 1.341(8) . ? N2 C6 1.342(8) . ? N3 C15 1.338(8) . ? N3 C11 1.365(8) . ? N4 C16 1.347(8) . ? N4 C20 1.356(8) . ? N5 N6 1.274(7) . ? N5 C20 1.377(9) . ? N6 C21 1.460(8) . ? C1 C2 1.372(10) . ? C1 H1 0.9603 . ? C2 C3 1.361(12) . ? C2 H2 0.9598 . ? C3 C4 1.380(11) . ? C3 H3 0.9598 . ? C4 C5 1.375(9) . ? C4 H4 0.9594 . ? C5 C6 1.453(10) . ? C6 C7 1.379(10) . ? C7 C8 1.371(11) . ? C7 H7 0.9608 . ? C8 C9 1.378(11) . ? C8 H8 0.9596 . ? C9 C10 1.390(9) . ? C9 H9 0.9594 . ? C10 C11 1.454(9) . ? C11 C12 1.381(10) . ? C12 C13 1.399(12) . ? C12 H12 0.9596 . ? C13 C14 1.352(13) . ? C13 H13 0.9599 . ? C14 C15 1.369(11) . ? C14 H14 0.9593 . ? C15 H15 0.9596 . ? C16 C17 1.364(10) . ? C16 H16 0.9605 . ? C17 C18 1.365(11) . ? C17 H17 0.9602 . ? C18 C19 1.368(11) . ? C18 H18 0.9602 . ? C19 C20 1.383(10) . ? C19 H19 0.9599 . ? C21 C26 1.362(9) . ? C21 C22 1.364(9) . ? C22 C23 1.368(10) . ? C22 H22 0.9597 . ? C23 C24 1.357(11) . ? C23 H23 0.9601 . ? C24 C25 1.365(11) . ? C24 H24 0.9602 . ? C25 C26 1.392(10) . ? C25 H25 0.9602 . ? C26 H26 0.9602 . ? Cl1 O14 1.371(7) . ? Cl1 O11 1.403(7) . ? Cl1 O12 1.408(7) . ? Cl1 O13 1.416(7) . ? Cl2 O24 1.330(9) . ? Cl2 O22 1.372(8) . ? Cl2 O21 1.378(7) . ? Cl2 O23 1.422(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ru1 N2 96.7(2) . . ? N6 Ru1 N4 76.2(2) . . ? N2 Ru1 N4 172.9(2) . . ? N6 Ru1 N1 90.4(2) . . ? N2 Ru1 N1 79.6(2) . . ? N4 Ru1 N1 99.6(2) . . ? N6 Ru1 N3 96.4(2) . . ? N2 Ru1 N3 78.8(2) . . ? N4 Ru1 N3 102.4(2) . . ? N1 Ru1 N3 157.9(2) . . ? N6 Ru1 O30 174.4(2) . . ? N2 Ru1 O30 88.3(2) . . ? N4 Ru1 O30 98.8(2) . . ? N1 Ru1 O30 87.9(2) . . ? N3 Ru1 O30 87.1(2) . . ? Ru1 O30 H30A 120.0 . . ? Ru1 O30 H30B 120.0 . . ? H30A O30 H30B 120.0 . . ? C1 N1 C5 119.7(6) . . ? C1 N1 Ru1 127.7(5) . . ? C5 N1 Ru1 112.4(4) . . ? C10 N2 C6 122.1(6) . . ? C10 N2 Ru1 119.6(4) . . ? C6 N2 Ru1 118.3(5) . . ? C15 N3 C11 118.7(6) . . ? C15 N3 Ru1 128.0(5) . . ? C11 N3 Ru1 113.3(5) . . ? C16 N4 C20 116.9(6) . . ? C16 N4 Ru1 130.5(5) . . ? C20 N4 Ru1 112.5(4) . . ? N6 N5 C20 112.1(6) . . ? N5 N6 C21 114.5(5) . . ? N5 N6 Ru1 122.4(4) . . ? C21 N6 Ru1 122.0(4) . . ? N1 C1 C2 122.3(8) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.5(8) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 121.2 . . ? C2 C3 C4 120.0(8) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 120.5(8) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 119.5 . . ? N1 C5 C4 119.0(7) . . ? N1 C5 C6 115.7(6) . . ? C4 C5 C6 125.2(7) . . ? N2 C6 C7 120.8(7) . . ? N2 C6 C5 113.6(6) . . ? C7 C6 C5 125.7(7) . . ? C8 C7 C6 117.8(7) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 122.4 . . ? C7 C8 C9 121.5(7) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 118.4 . . ? C8 C9 C10 118.6(7) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 119.3(7) . . ? N2 C10 C11 112.6(6) . . ? C9 C10 C11 128.1(7) . . ? N3 C11 C12 120.6(7) . . ? N3 C11 C10 115.7(6) . . ? C12 C11 C10 123.6(7) . . ? C11 C12 C13 119.4(8) . . ? C11 C12 H12 121.7 . . ? C13 C12 H12 118.8 . . ? C14 C13 C12 118.8(8) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.9 . . ? C13 C14 C15 120.0(8) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 120.3 . . ? N3 C15 C14 122.5(8) . . ? N3 C15 H15 118.2 . . ? C14 C15 H15 119.3 . . ? N4 C16 C17 122.2(7) . . ? N4 C16 H16 117.6 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 120.3(8) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 120.4 . . ? C17 C18 C19 119.4(7) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.0 . . ? C18 C19 C20 118.0(8) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 122.0 . . ? N4 C20 N5 116.7(6) . . ? N4 C20 C19 123.2(7) . . ? N5 C20 C19 120.1(7) . . ? C26 C21 C22 123.1(7) . . ? C26 C21 N6 118.6(6) . . ? C22 C21 N6 118.2(6) . . ? C21 C22 C23 117.6(7) . . ? C21 C22 H22 122.8 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 121.4(8) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.2(8) . . ? C23 C24 H24 118.8 . . ? C25 C24 H24 121.0 . . ? C24 C25 C26 120.0(8) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 121.0 . . ? C21 C26 C25 117.6(7) . . ? C21 C26 H26 122.3 . . ? C25 C26 H26 120.0 . . ? O14 Cl1 O11 109.4(6) . . ? O14 Cl1 O12 113.8(5) . . ? O11 Cl1 O12 107.2(5) . . ? O14 Cl1 O13 109.2(6) . . ? O11 Cl1 O13 107.1(6) . . ? O12 Cl1 O13 109.9(5) . . ? O24 Cl2 O22 109.4(8) . . ? O24 Cl2 O21 109.3(7) . . ? O22 Cl2 O21 109.9(7) . . ? O24 Cl2 O23 112.5(7) . . ? O22 Cl2 O23 107.2(6) . . ? O21 Cl2 O23 108.6(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.92 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.910 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.139