Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_fb07m _database_code_CSD 152560 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H34 Cl4 N10 O8 Ru' _chemical_formula_weight 941.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2~1~/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 17.649(2) _cell_length_b 12.0387(16) _cell_length_c 19.374(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.834(3) _cell_angle_gamma 90.00 _cell_volume 4013.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25883 _cell_measurement_theta_min 1.18 _cell_measurement_theta_max 28.29 _exptl_crystal_description pillar _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.8783 _exptl_absorpt_correction_T_max 0.9710 _exptl_absorpt_process_details ? _exptl_special_details ; North et al., (1968), Acta Cryst. A24, 351-359. ; _diffrn_ambient_temperature 293(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 'Siemens SMART CCD' _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 25269 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9575 _reflns_number_gt 5763 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The two H-atoms that are attached to the C~33~ atom are difficult to find in the difference Fourier map, because its ligand is disordered. Hence they are omitted in the atom list. But they should exist in the chemical sense. 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^)+(0.0985P)^2^+8.0655P] 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 9575 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1423 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.2281 _refine_ls_wR_factor_gt 0.1961 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.24101(3) 0.11440(4) 0.04430(3) 0.04765(18) Uani 1 1 d . . . N1 N 0.2659(3) 0.1341(4) -0.0544(3) 0.0493(12) Uani 1 1 d . . . N2 N 0.2346(3) 0.0634(4) -0.1038(3) 0.0499(12) Uani 1 1 d . . . N3 N 0.1666(3) 0.0061(4) -0.0176(3) 0.0542(13) Uani 1 1 d . . . N4 N 0.1436(3) -0.0894(5) -0.1180(3) 0.0622(14) Uani 1 1 d . . . N5 N 0.1774(3) 0.2584(4) 0.0400(3) 0.0496(12) Uani 1 1 d . . . N6 N 0.2039(3) 0.3383(4) 0.0822(3) 0.0556(13) Uani 1 1 d . . . N7 N 0.3153(3) 0.2234(5) 0.1085(3) 0.0547(13) Uani 1 1 d . . . N8 N 0.3199(4) 0.3783(5) 0.1709(3) 0.0757(17) Uani 1 1 d . . . N9 N 0.2081(3) 0.0577(4) 0.1355(3) 0.0524(12) Uani 1 1 d . . . N10 N 0.3176(3) -0.0162(4) 0.0746(3) 0.0542(13) Uani 1 1 d . . . C1 C 0.3109(4) 0.2178(5) -0.0797(3) 0.0487(14) Uani 1 1 d . . . C2 C 0.2869(4) 0.2562(6) -0.1489(3) 0.0601(17) Uani 1 1 d . . . H2 H 0.2415 0.2292 -0.1781 0.072 Uiso 1 1 calc R . . C3 C 0.3302(5) 0.3332(7) -0.1733(4) 0.072(2) Uani 1 1 d . . . H3 H 0.3142 0.3585 -0.2196 0.086 Uiso 1 1 calc R . . C4 C 0.3983(5) 0.3757(6) -0.1309(4) 0.069(2) Uani 1 1 d . . . C5 C 0.4218(5) 0.3352(6) -0.0617(4) 0.0704(19) Uani 1 1 d . . . H5 H 0.4677 0.3610 -0.0327 0.084 Uiso 1 1 calc R . . C6 C 0.3775(4) 0.2575(6) -0.0360(4) 0.0594(17) Uani 1 1 d . . . H6 H 0.3927 0.2322 0.0104 0.071 Uiso 1 1 calc R . . C7 C 0.4468(6) 0.4621(8) -0.1586(5) 0.097(3) Uani 1 1 d . . . H7A H 0.4507 0.4426 -0.2058 0.116 Uiso 1 1 calc R . . H7B H 0.4979 0.4648 -0.1284 0.116 Uiso 1 1 calc R . . H7C H 0.4226 0.5336 -0.1593 0.116 Uiso 1 1 calc R . . C8 C 0.1857(4) -0.0060(5) -0.0803(3) 0.0519(15) Uani 1 1 d . . . C9 C 0.0967(5) -0.1316(6) -0.0770(4) 0.076(2) Uani 1 1 d . . . H9 H 0.0617 -0.1900 -0.0888 0.092 Uiso 1 1 calc R . . C10 C 0.1108(5) -0.0715(7) -0.0154(4) 0.071(2) Uani 1 1 d . . . H10 H 0.0863 -0.0819 0.0219 0.085 Uiso 1 1 calc R . . C11 C 0.1500(5) -0.1278(6) -0.1881(4) 0.071(2) Uani 1 1 d . . . H11A H 0.1883 -0.1856 -0.1831 0.085 Uiso 1 1 calc R . . H11B H 0.1652 -0.0670 -0.2141 0.085 Uiso 1 1 calc R . . H11C H 0.1007 -0.1561 -0.2132 0.085 Uiso 1 1 calc R . . C12 C 0.0993(3) 0.2787(5) 0.0017(3) 0.0483(14) Uani 1 1 d . . . C13 C 0.0715(4) 0.2339(6) -0.0656(3) 0.0646(18) Uani 1 1 d . . . H13 H 0.1037 0.1901 -0.0864 0.077 Uiso 1 1 calc R . . C14 C -0.0039(4) 0.2548(7) -0.1014(4) 0.072(2) Uani 1 1 d . . . H14 H -0.0219 0.2250 -0.1463 0.086 Uiso 1 1 calc R . . C15 C -0.0531(4) 0.3189(6) -0.0717(4) 0.0604(17) Uani 1 1 d . . . C16 C -0.0264(4) 0.3614(6) -0.0047(4) 0.0626(18) Uani 1 1 d . . . H16 H -0.0596 0.4031 0.0163 0.075 Uiso 1 1 calc R . . C17 C 0.0497(4) 0.3427(6) 0.0320(4) 0.0583(16) Uani 1 1 d . . . H17 H 0.0673 0.3730 0.0769 0.070 Uiso 1 1 calc R . . C18 C -0.1360(5) 0.3398(8) -0.1122(5) 0.088(2) Uani 1 1 d . . . H18A H -0.1395 0.3279 -0.1618 0.106 Uiso 1 1 calc R . . H18B H -0.1504 0.4150 -0.1046 0.106 Uiso 1 1 calc R . . H18C H -0.1705 0.2897 -0.0958 0.106 Uiso 1 1 calc R . . C19 C 0.2769(4) 0.3132(6) 0.1198(3) 0.0540(15) Uani 1 1 d . . . C20 C 0.3913(4) 0.3226(8) 0.1923(4) 0.079(2) Uani 1 1 d . . . H20 H 0.4340 0.3460 0.2266 0.095 Uiso 1 1 calc R . . C21 C 0.3857(4) 0.2282(7) 0.1533(4) 0.0650(18) Uani 1 1 d . . . H21 H 0.4246 0.1749 0.1569 0.078 Uiso 1 1 calc R . . C22 C 0.2964(6) 0.4779(8) 0.2013(5) 0.106(3) Uani 1 1 d . . . H22A H 0.2407 0.4812 0.1918 0.127 Uiso 1 1 calc R . . H22B H 0.3159 0.5414 0.1808 0.127 Uiso 1 1 calc R . . H22C H 0.3169 0.4775 0.2515 0.127 Uiso 1 1 calc R . . C23 C 0.1501(4) 0.0968(6) 0.1618(4) 0.0651(18) Uani 1 1 d . . . H23 H 0.1242 0.1602 0.1415 0.078 Uiso 1 1 calc R . . C24 C 0.1268(5) 0.0484(7) 0.2170(4) 0.078(2) Uani 1 1 d . . . H24 H 0.0847 0.0767 0.2329 0.094 Uiso 1 1 calc R . . C25 C 0.1663(5) -0.0426(8) 0.2488(4) 0.085(2) Uani 1 1 d . . . H25 H 0.1517 -0.0771 0.2868 0.102 Uiso 1 1 calc R . . C26 C 0.2272(5) -0.0817(6) 0.2236(4) 0.072(2) Uani 1 1 d . . . H26 H 0.2552 -0.1427 0.2451 0.086 Uiso 1 1 calc R . . C27 C 0.2481(4) -0.0309(5) 0.1660(3) 0.0527(15) Uani 1 1 d . . . C28 C 0.3118(4) -0.0682(5) 0.1351(3) 0.0565(16) Uani 1 1 d . . . C29 C 0.3650(5) -0.1482(7) 0.1643(4) 0.080(2) Uani 1 1 d . . . H29 H 0.3607 -0.1834 0.2059 0.096 Uiso 1 1 calc R . . C30 C 0.4244(6) -0.1763(8) 0.1323(5) 0.100(3) Uani 1 1 d . . . H30 H 0.4604 -0.2303 0.1521 0.120 Uiso 1 1 calc R . . C31 C 0.4299(5) -0.1239(7) 0.0709(5) 0.091(3) Uani 1 1 d . . . H31 H 0.4697 -0.1419 0.0485 0.109 Uiso 1 1 calc R . . C32 C 0.3757(4) -0.0438(6) 0.0427(4) 0.070(2) Uani 1 1 d . . . H32 H 0.3793 -0.0082 0.0009 0.084 Uiso 1 1 calc R . . Cl1 Cl 0.04593(13) 0.37709(18) 0.22454(11) 0.0776(5) Uani 1 1 d . . . O1 O 0.0431(5) 0.4158(6) 0.2926(3) 0.115(2) Uani 1 1 d . . . O2 O 0.0052(6) 0.2837(8) 0.2059(6) 0.177(4) Uani 1 1 d . . . O3 O 0.1202(4) 0.3664(8) 0.2142(4) 0.145(3) Uani 1 1 d . . . O4 O 0.0095(7) 0.4576(10) 0.1771(4) 0.194(5) Uani 1 1 d . . . Cl2 Cl 0.40658(12) 0.6657(2) 0.35281(12) 0.0902(7) Uani 1 1 d . . . O5 O 0.4376(5) 0.6581(10) 0.2921(4) 0.167(4) Uani 1 1 d . . . O6 O 0.4549(5) 0.7203(11) 0.4073(4) 0.192(5) Uani 1 1 d . . . O7 O 0.3927(9) 0.5620(11) 0.3745(5) 0.236(7) Uani 1 1 d . . . O8 O 0.3372(6) 0.7139(11) 0.3304(7) 0.214(5) Uani 1 1 d . . . C33 C 0.3024(10) 0.5974(16) -0.0465(9) 0.185(7) Uani 1 1 d . . . Cl3 Cl 0.3514(3) 0.5597(5) 0.0373(3) 0.2031(19) Uani 1 1 d . . . Cl41 Cl 0.2323(8) 0.6747(14) -0.0458(7) 0.277(8) Uani 0.50 1 d P . . Cl42 Cl 0.2088(6) 0.5279(12) -0.0616(4) 0.201(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0478(3) 0.0510(3) 0.0458(3) 0.0076(2) 0.0141(2) 0.0108(2) N1 0.044(3) 0.049(3) 0.056(3) 0.007(2) 0.013(2) 0.010(2) N2 0.049(3) 0.052(3) 0.047(3) 0.004(2) 0.010(2) 0.011(2) N3 0.057(3) 0.055(3) 0.053(3) 0.009(2) 0.018(2) 0.000(3) N4 0.066(4) 0.054(3) 0.064(4) 0.000(3) 0.010(3) -0.001(3) N5 0.050(3) 0.054(3) 0.046(3) 0.003(2) 0.015(2) 0.004(2) N6 0.049(3) 0.049(3) 0.067(3) -0.002(3) 0.008(3) 0.002(2) N7 0.046(3) 0.066(3) 0.052(3) 0.005(3) 0.010(2) 0.008(3) N8 0.072(4) 0.077(4) 0.074(4) -0.008(3) 0.007(3) -0.004(3) N9 0.064(3) 0.052(3) 0.043(3) 0.008(2) 0.017(2) 0.006(3) N10 0.062(3) 0.053(3) 0.046(3) 0.004(2) 0.007(2) 0.020(3) C1 0.057(4) 0.044(3) 0.049(3) 0.008(3) 0.019(3) 0.008(3) C2 0.064(4) 0.062(4) 0.054(4) 0.013(3) 0.012(3) 0.004(3) C3 0.078(5) 0.078(5) 0.060(4) 0.017(4) 0.019(4) 0.005(4) C4 0.081(5) 0.057(4) 0.078(5) 0.016(4) 0.035(4) 0.011(4) C5 0.067(5) 0.060(4) 0.087(5) 0.000(4) 0.025(4) -0.003(4) C6 0.063(4) 0.059(4) 0.058(4) 0.008(3) 0.019(3) 0.009(3) C7 0.105(7) 0.089(6) 0.102(7) 0.033(5) 0.036(6) 0.004(5) C8 0.052(4) 0.050(4) 0.054(4) 0.006(3) 0.012(3) 0.004(3) C9 0.079(5) 0.067(5) 0.086(6) 0.008(4) 0.024(4) -0.016(4) C10 0.076(5) 0.076(5) 0.066(5) 0.004(4) 0.027(4) -0.016(4) C11 0.084(5) 0.058(4) 0.070(5) -0.013(4) 0.013(4) -0.003(4) C12 0.049(3) 0.045(3) 0.050(3) 0.006(3) 0.009(3) 0.003(3) C13 0.066(4) 0.073(5) 0.052(4) -0.003(3) 0.009(3) 0.021(4) C14 0.068(5) 0.088(5) 0.051(4) -0.006(4) -0.003(3) 0.014(4) C15 0.051(4) 0.063(4) 0.064(4) 0.009(3) 0.008(3) 0.003(3) C16 0.054(4) 0.065(4) 0.069(4) 0.005(3) 0.014(3) 0.014(3) C17 0.057(4) 0.062(4) 0.053(4) 0.000(3) 0.007(3) 0.005(3) C18 0.066(5) 0.106(6) 0.083(6) 0.017(5) -0.002(4) 0.019(5) C19 0.049(4) 0.061(4) 0.049(3) 0.004(3) 0.005(3) -0.003(3) C20 0.051(4) 0.109(7) 0.071(5) 0.007(5) -0.001(4) -0.012(4) C21 0.052(4) 0.088(5) 0.051(4) 0.003(4) 0.005(3) 0.006(4) C22 0.090(7) 0.098(7) 0.113(8) -0.043(6) -0.010(6) 0.001(5) C23 0.071(5) 0.069(5) 0.064(4) 0.010(3) 0.032(4) 0.008(4) C24 0.084(5) 0.086(6) 0.077(5) 0.016(4) 0.045(4) 0.002(5) C25 0.105(7) 0.092(6) 0.067(5) 0.015(4) 0.037(5) -0.013(5) C26 0.092(6) 0.061(4) 0.063(4) 0.020(4) 0.016(4) 0.002(4) C27 0.064(4) 0.050(4) 0.042(3) 0.004(3) 0.006(3) 0.003(3) C28 0.070(4) 0.051(4) 0.043(3) -0.001(3) 0.002(3) 0.009(3) C29 0.099(6) 0.078(5) 0.059(4) 0.010(4) 0.011(4) 0.033(5) C30 0.113(8) 0.089(7) 0.089(6) 0.010(5) 0.007(6) 0.054(6) C31 0.087(6) 0.089(6) 0.096(6) -0.002(5) 0.021(5) 0.040(5) C32 0.070(5) 0.073(5) 0.071(5) 0.003(4) 0.023(4) 0.031(4) Cl1 0.0829(14) 0.0829(13) 0.0674(11) -0.0093(10) 0.0171(10) -0.0112(11) O1 0.149(6) 0.134(6) 0.071(4) -0.014(4) 0.045(4) -0.049(5) O2 0.182(9) 0.150(8) 0.209(10) -0.082(7) 0.066(8) -0.091(7) O3 0.089(5) 0.224(10) 0.124(6) -0.051(6) 0.030(5) -0.006(5) O4 0.274(13) 0.222(11) 0.087(5) 0.041(6) 0.043(7) 0.111(10) Cl2 0.0610(12) 0.1271(19) 0.0783(14) 0.0177(13) 0.0064(10) -0.0196(12) O5 0.104(6) 0.318(12) 0.078(5) -0.008(6) 0.017(4) -0.064(7) O6 0.123(7) 0.355(15) 0.097(5) -0.058(7) 0.024(5) -0.102(8) O7 0.376(19) 0.192(11) 0.131(8) 0.060(8) 0.038(10) -0.057(12) O8 0.118(7) 0.276(15) 0.223(12) -0.008(10) -0.017(7) 0.052(8) C33 0.152(13) 0.26(2) 0.159(14) 0.068(13) 0.056(11) 0.075(14) Cl3 0.196(5) 0.218(5) 0.177(4) 0.017(4) 0.003(3) -0.007(4) Cl41 0.244(11) 0.361(17) 0.275(13) 0.199(13) 0.164(10) 0.205(13) Cl42 0.169(8) 0.334(15) 0.106(5) -0.023(7) 0.043(5) -0.017(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N3 2.040(5) . ? Ru1 N5 2.057(5) . ? Ru1 N7 2.066(6) . ? Ru1 N1 2.069(5) . ? Ru1 N10 2.072(5) . ? Ru1 N9 2.094(5) . ? N1 N2 1.309(7) . ? N1 C1 1.434(7) . ? N2 C8 1.350(8) . ? N3 C8 1.339(8) . ? N3 C10 1.365(9) . ? N4 C8 1.361(8) . ? N4 C9 1.365(9) . ? N4 C11 1.464(9) . ? N5 N6 1.282(7) . ? N5 C12 1.434(8) . ? N6 C19 1.365(8) . ? N7 C19 1.319(8) . ? N7 C21 1.350(8) . ? N8 C19 1.356(9) . ? N8 C20 1.406(10) . ? N8 C22 1.436(10) . ? N9 C23 1.326(8) . ? N9 C27 1.341(8) . ? N10 C32 1.351(8) . ? N10 C28 1.353(8) . ? C1 C6 1.373(9) . ? C1 C2 1.394(8) . ? C2 C3 1.352(10) . ? C2 H2 0.9300 . ? C3 C4 1.393(11) . ? C3 H3 0.9300 . ? C4 C5 1.401(10) . ? C4 C7 1.520(11) . ? C5 C6 1.381(10) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C9 C10 1.370(11) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C17 1.391(9) . ? C12 C13 1.397(9) . ? C13 C14 1.379(9) . ? C13 H13 0.9300 . ? C14 C15 1.379(10) . ? C14 H14 0.9300 . ? C15 C16 1.377(10) . ? C15 C18 1.521(9) . ? C16 C17 1.390(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C20 C21 1.357(11) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.360(9) . ? C23 H23 0.9300 . ? C24 C25 1.369(11) . ? C24 H24 0.9300 . ? C25 C26 1.360(11) . ? C25 H25 0.9300 . ? C26 C27 1.393(9) . ? C26 H26 0.9300 . ? C27 C28 1.456(9) . ? C28 C29 1.375(10) . ? C29 C30 1.373(12) . ? C29 H29 0.9300 . ? C30 C31 1.369(13) . ? C30 H30 0.9300 . ? C31 C32 1.383(10) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? Cl1 O2 1.340(7) . ? Cl1 O3 1.376(8) . ? Cl1 O4 1.391(9) . ? Cl1 O1 1.409(6) . ? Cl2 O8 1.338(10) . ? Cl2 O7 1.357(11) . ? Cl2 O6 1.370(8) . ? Cl2 O5 1.406(8) . ? C33 Cl41 1.551(17) . ? C33 Cl3 1.722(16) . ? C33 Cl42 1.82(2) . ? Cl41 Cl42 1.825(19) . ? 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 N3 Ru1 N5 103.9(2) . . ? N3 Ru1 N7 178.9(2) . . ? N5 Ru1 N7 75.9(2) . . ? N3 Ru1 N1 76.8(2) . . ? N5 Ru1 N1 95.26(18) . . ? N7 Ru1 N1 104.3(2) . . ? N3 Ru1 N10 88.6(2) . . ? N5 Ru1 N10 165.2(2) . . ? N7 Ru1 N10 91.4(2) . . ? N1 Ru1 N10 95.15(19) . . ? N3 Ru1 N9 91.4(2) . . ? N5 Ru1 N9 93.33(19) . . ? N7 Ru1 N9 87.5(2) . . ? N1 Ru1 N9 166.8(2) . . ? N10 Ru1 N9 78.4(2) . . ? N2 N1 C1 112.6(5) . . ? N2 N1 Ru1 117.3(4) . . ? C1 N1 Ru1 130.1(4) . . ? N1 N2 C8 110.7(5) . . ? C8 N3 C10 106.4(6) . . ? C8 N3 Ru1 110.1(4) . . ? C10 N3 Ru1 142.6(5) . . ? C8 N4 C9 107.0(6) . . ? C8 N4 C11 125.8(6) . . ? C9 N4 C11 127.2(6) . . ? N6 N5 C12 112.0(5) . . ? N6 N5 Ru1 119.3(4) . . ? C12 N5 Ru1 128.2(4) . . ? N5 N6 C19 109.9(5) . . ? C19 N7 C21 107.0(6) . . ? C19 N7 Ru1 109.8(4) . . ? C21 N7 Ru1 141.7(5) . . ? C19 N8 C20 105.1(6) . . ? C19 N8 C22 128.0(7) . . ? C20 N8 C22 126.7(7) . . ? C23 N9 C27 119.3(5) . . ? C23 N9 Ru1 126.2(4) . . ? C27 N9 Ru1 114.4(4) . . ? C32 N10 C28 119.6(6) . . ? C32 N10 Ru1 124.8(5) . . ? C28 N10 Ru1 115.2(4) . . ? C6 C1 C2 120.9(6) . . ? C6 C1 N1 119.8(5) . . ? C2 C1 N1 119.3(6) . . ? C3 C2 C1 119.3(7) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 121.8(7) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C3 C4 C5 118.0(7) . . ? C3 C4 C7 121.6(7) . . ? C5 C4 C7 120.4(8) . . ? C6 C5 C4 120.7(7) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C1 C6 C5 119.3(6) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 N2 123.2(6) . . ? N3 C8 N4 110.5(6) . . ? N2 C8 N4 126.1(6) . . ? N4 C9 C10 107.1(7) . . ? N4 C9 H9 126.5 . . ? C10 C9 H9 126.5 . . ? N3 C10 C9 109.1(6) . . ? N3 C10 H10 125.4 . . ? C9 C10 H10 125.4 . . ? N4 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 119.0(6) . . ? C17 C12 N5 120.0(5) . . ? C13 C12 N5 121.0(6) . . ? C14 C13 C12 119.9(6) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 121.2(7) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C16 C15 C14 119.1(6) . . ? C16 C15 C18 120.9(7) . . ? C14 C15 C18 120.0(7) . . ? C15 C16 C17 120.7(6) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C12 120.1(6) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? 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 . . ? N7 C19 N8 111.6(6) . . ? N7 C19 N6 123.5(6) . . ? N8 C19 N6 124.8(6) . . ? C21 C20 N8 106.6(7) . . ? C21 C20 H20 126.7 . . ? N8 C20 H20 126.7 . . ? N7 C21 C20 109.6(7) . . ? N7 C21 H21 125.2 . . ? C20 C21 H21 125.2 . . ? N8 C22 H22A 109.5 . . ? N8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N9 C23 C24 122.9(7) . . ? N9 C23 H23 118.5 . . ? C24 C23 H23 118.5 . . ? C23 C24 C25 119.0(7) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C26 C25 C24 118.7(7) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C27 120.4(7) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? N9 C27 C26 119.7(6) . . ? N9 C27 C28 116.3(5) . . ? C26 C27 C28 124.0(6) . . ? N10 C28 C29 120.2(7) . . ? N10 C28 C27 115.3(5) . . ? C29 C28 C27 124.5(6) . . ? C30 C29 C28 120.5(8) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 119.2(8) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C30 C31 C32 119.2(8) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? N10 C32 C31 121.3(7) . . ? N10 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? O2 Cl1 O3 110.8(6) . . ? O2 Cl1 O4 105.4(8) . . ? O3 Cl1 O4 106.5(7) . . ? O2 Cl1 O1 113.6(5) . . ? O3 Cl1 O1 113.5(5) . . ? O4 Cl1 O1 106.2(5) . . ? O8 Cl2 O7 106.5(9) . . ? O8 Cl2 O6 114.2(8) . . ? O7 Cl2 O6 109.1(7) . . ? O8 Cl2 O5 104.8(7) . . ? O7 Cl2 O5 109.3(8) . . ? O6 Cl2 O5 112.6(5) . . ? Cl41 C33 Cl3 112.7(12) . . ? Cl41 C33 Cl42 65.1(10) . . ? Cl3 C33 Cl42 106.2(10) . . ? C33 Cl41 Cl42 64.5(10) . . ? C33 Cl42 Cl41 50.4(7) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.247 _refine_diff_density_min -1.275 _refine_diff_density_rms 0.105