# 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 _publ_contact_author_name 'Kenneth Caulton' _publ_contact_author_email CAULTON@INDIANA.EDU _publ_section_title ; Synthesis and Reactivity of a Ru(I) Dimer Devoid of pi-acid Ligands ; loop_ _publ_author_name 'Kenneth Caulton' 'Maren Pink' 'Amy G. Walstrom' 'Xiaofan Yang' # Attachment '08055.txt' data_08055 _database_code_depnum_ccdc_archive 'CCDC 719526' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 N6 Ru, 2 Cl, 4 (C H2 Cl2)' _chemical_formula_sum 'C34 H30 Cl10 N6 Ru' _chemical_formula_weight 978.21 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 9.9397(7) _cell_length_b 17.9554(15) _cell_length_c 22.2596(17) _cell_angle_alpha 90.00 _cell_angle_beta 91.402(4) _cell_angle_gamma 90.00 _cell_volume 3971.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3110 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 1.103 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.8347 _exptl_absorpt_correction_T_max 0.8977 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 60 seconds each' _diffrn_measurement_method 'omega and phi scans' _diffrn_measurement_device 'APEX Kappa Duo' _diffrn_measurement_device_type Kappa _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker APEXII' _diffrn_detector_area_resol_mean 83.33 _diffrn_reflns_number 20441 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6929 _reflns_number_gt 4521 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2007)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2007)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2007)' _computing_structure_solution 'SIR-2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2008)' _computing_publication_material 'SHELXTL (Bruker, 2008)' _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^)+(0.0634P)^2^+4.3202P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6929 _refine_ls_number_parameters 480 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1374 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.011 _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 0.00452(4) 0.78374(2) 0.355304(17) 0.03702(14) Uani 1 1 d . . . N1 N 0.1474(4) 0.7154(3) 0.31805(18) 0.0428(10) Uani 1 1 d . . . N2 N 0.0103(4) 0.7012(2) 0.41361(18) 0.0428(11) Uani 1 1 d . . . N3 N -0.1358(4) 0.8199(3) 0.41599(18) 0.0421(10) Uani 1 1 d . . . N4 N -0.1414(4) 0.7493(2) 0.29277(18) 0.0399(10) Uani 1 1 d . . . N5 N 0.0042(4) 0.8682(2) 0.29863(17) 0.0365(10) Uani 1 1 d . . . N6 N 0.1507(4) 0.8507(2) 0.39461(17) 0.0385(10) Uani 1 1 d . . . C1 C 0.2116(5) 0.7263(3) 0.2664(2) 0.0500(14) Uani 1 1 d . . . H1 H 0.1948 0.7707 0.2443 0.060 Uiso 1 1 calc R . . C2 C 0.3013(6) 0.6751(4) 0.2442(3) 0.0561(16) Uani 1 1 d . . . H2 H 0.3446 0.6841 0.2074 0.067 Uiso 1 1 calc R . . C3 C 0.3271(6) 0.6115(4) 0.2759(3) 0.0614(17) Uani 1 1 d . . . H3 H 0.3885 0.5758 0.2609 0.074 Uiso 1 1 calc R . . C4 C 0.2645(6) 0.5989(3) 0.3293(3) 0.0555(15) Uani 1 1 d . . . H4 H 0.2825 0.5549 0.3518 0.067 Uiso 1 1 calc R . . C5 C 0.1737(5) 0.6523(3) 0.3501(2) 0.0435(13) Uani 1 1 d . . . C6 C 0.0978(6) 0.6445(3) 0.4059(2) 0.0478(13) Uani 1 1 d . . . C7 C 0.1116(7) 0.5887(3) 0.4486(3) 0.0609(16) Uani 1 1 d . . . H7 H 0.1727 0.5486 0.4435 0.073 Uiso 1 1 calc R . . C8 C 0.0332(8) 0.5934(4) 0.4989(3) 0.072(2) Uani 1 1 d . . . H8 H 0.0430 0.5566 0.5293 0.086 Uiso 1 1 calc R . . C9 C -0.0591(7) 0.6502(4) 0.5064(3) 0.0600(17) Uani 1 1 d . . . H9 H -0.1144 0.6513 0.5406 0.072 Uiso 1 1 calc R . . C10 C -0.0694(5) 0.7053(3) 0.4633(2) 0.0474(14) Uani 1 1 d . . . C11 C -0.1542(5) 0.7722(3) 0.4633(2) 0.0457(14) Uani 1 1 d . . . C12 C -0.2458(6) 0.7892(4) 0.5077(2) 0.0573(16) Uani 1 1 d . . . H12 H -0.2590 0.7553 0.5399 0.069 Uiso 1 1 calc R . . C13 C -0.3167(6) 0.8545(4) 0.5051(3) 0.0640(18) Uani 1 1 d . . . H13 H -0.3793 0.8663 0.5352 0.077 Uiso 1 1 calc R . . C14 C -0.2957(6) 0.9030(4) 0.4581(3) 0.0622(17) Uani 1 1 d . . . H14 H -0.3426 0.9491 0.4559 0.075 Uiso 1 1 calc R . . C15 C -0.2062(5) 0.8839(4) 0.4143(2) 0.0507(14) Uani 1 1 d . . . H15 H -0.1938 0.9172 0.3818 0.061 Uiso 1 1 calc R . . C16 C -0.2119(5) 0.6863(3) 0.2929(3) 0.0466(13) Uani 1 1 d . . . H16 H -0.1988 0.6525 0.3253 0.056 Uiso 1 1 calc R . . C17 C -0.3039(6) 0.6681(3) 0.2473(3) 0.0555(15) Uani 1 1 d . . . H17 H -0.3514 0.6222 0.2482 0.067 Uiso 1 1 calc R . . C18 C -0.3254(5) 0.7176(4) 0.2007(3) 0.0533(15) Uani 1 1 d . . . H18 H -0.3876 0.7060 0.1690 0.064 Uiso 1 1 calc R . . C19 C -0.2566(6) 0.7832(3) 0.2006(2) 0.0481(13) Uani 1 1 d . . . H19 H -0.2723 0.8183 0.1692 0.058 Uiso 1 1 calc R . . C20 C -0.1628(5) 0.7987(3) 0.2468(2) 0.0398(12) Uani 1 1 d . . . C21 C -0.0810(5) 0.8671(3) 0.2498(2) 0.0398(12) Uani 1 1 d . . . C22 C -0.0820(6) 0.9261(3) 0.2099(3) 0.0534(15) Uani 1 1 d . . . H22 H -0.1401 0.9256 0.1754 0.064 Uiso 1 1 calc R . . C23 C 0.0026(6) 0.9857(4) 0.2211(3) 0.0605(17) Uani 1 1 d . . . H23 H 0.0023 1.0266 0.1941 0.073 Uiso 1 1 calc R . . C24 C 0.0886(6) 0.9866(3) 0.2715(3) 0.0527(15) Uani 1 1 d . . . H24 H 0.1464 1.0278 0.2791 0.063 Uiso 1 1 calc R . . C25 C 0.0882(5) 0.9270(3) 0.3100(2) 0.0403(12) Uani 1 1 d . . . C26 C 0.1725(5) 0.9159(3) 0.3643(2) 0.0418(12) Uani 1 1 d . . . C27 C 0.2681(5) 0.9656(3) 0.3849(2) 0.0435(13) Uani 1 1 d . . . H27 H 0.2830 1.0104 0.3634 0.052 Uiso 1 1 calc R . . C28 C 0.3426(5) 0.9506(4) 0.4364(2) 0.0508(15) Uani 1 1 d . . . H28 H 0.4088 0.9849 0.4507 0.061 Uiso 1 1 calc R . . C29 C 0.3201(6) 0.8856(4) 0.4670(2) 0.0548(16) Uani 1 1 d . . . H29 H 0.3694 0.8746 0.5030 0.066 Uiso 1 1 calc R . . C30 C 0.2248(5) 0.8367(4) 0.4445(2) 0.0505(14) Uani 1 1 d . . . H30 H 0.2109 0.7912 0.4652 0.061 Uiso 1 1 calc R . . Cl2 Cl 0.32616(15) 0.42673(9) 0.40955(6) 0.0569(4) Uani 1 1 d . . . Cl1 Cl 0.44432(14) 0.58371(9) 0.12122(6) 0.0562(4) Uani 1 1 d . . . Cl1S Cl 0.03167(19) 0.56060(11) 0.05467(9) 0.0848(6) Uani 1 1 d . . . Cl2S Cl -0.0196(2) 0.66778(14) 0.14687(10) 0.0995(7) Uani 1 1 d . . . C1S C 0.0997(8) 0.6282(5) 0.1030(4) 0.103(3) Uani 1 1 d . . . H1S1 H 0.1700 0.6051 0.1292 0.124 Uiso 1 1 calc R . . H1S2 H 0.1429 0.6675 0.0790 0.124 Uiso 1 1 calc R . . Cl3S Cl 0.5793(2) 0.44364(13) 0.26306(8) 0.0887(6) Uani 1 1 d . . . Cl4S Cl 0.4921(2) 0.32909(11) 0.17714(10) 0.0897(6) Uani 1 1 d . . . C2S C 0.4564(7) 0.4170(4) 0.2088(4) 0.080(2) Uani 1 1 d . . . H2S1 H 0.4519 0.4549 0.1765 0.096 Uiso 1 1 calc R . . H2S2 H 0.3674 0.4151 0.2278 0.096 Uiso 1 1 calc R . . Cl5S Cl 0.4386(7) 0.3364(4) 0.5963(3) 0.0967(14) Uani 0.636(11) 1 d PDU A 1 Cl6S Cl 0.2663(14) 0.4683(9) 0.5953(8) 0.095(2) Uani 0.636(11) 1 d PDU A 1 C3S C 0.4082(15) 0.4249(8) 0.5627(11) 0.087(4) Uani 0.636(11) 1 d PDU A 1 H3S1 H 0.3915 0.4186 0.5189 0.105 Uiso 0.636(11) 1 calc PR A 1 H3S2 H 0.4885 0.4569 0.5685 0.105 Uiso 0.636(11) 1 calc PR A 1 Cl5D Cl 0.4772(12) 0.3374(8) 0.5732(5) 0.0967(14) Uani 0.364(11) 1 d PDU A 2 Cl6D Cl 0.301(3) 0.4632(17) 0.6019(15) 0.095(2) Uani 0.364(11) 1 d PDU A 2 C3D C 0.446(3) 0.4342(13) 0.563(2) 0.087(4) Uani 0.364(11) 1 d PDU A 2 H3D1 H 0.4325 0.4446 0.5193 0.105 Uiso 0.364(11) 1 calc PR A 2 H3D2 H 0.5250 0.4630 0.5773 0.105 Uiso 0.364(11) 1 calc PR A 2 Cl7S Cl 0.1879(5) 0.8571(3) 0.1315(2) 0.0801(12) Uani 0.589(3) 1 d PDU B 1 Cl8S Cl 0.3922(3) 0.76061(19) 0.08333(15) 0.0797(7) Uani 0.589(3) 1 d PDU B 1 C4S C 0.3380(11) 0.8529(6) 0.0897(5) 0.068(3) Uani 0.589(3) 1 d PDU B 1 H4S1 H 0.3213 0.8741 0.0492 0.082 Uiso 0.589(3) 1 calc PR B 1 H4S2 H 0.4091 0.8829 0.1101 0.082 Uiso 0.589(3) 1 calc PR B 1 Cl7D Cl 0.2192(7) 0.8200(4) 0.1287(3) 0.0801(12) Uani 0.411(3) 1 d PDU B 2 Cl8D Cl 0.3908(5) 0.8053(3) 0.0264(2) 0.0797(7) Uani 0.411(3) 1 d PDU B 2 C4D C 0.3862(14) 0.8112(12) 0.1059(6) 0.068(3) Uani 0.411(3) 1 d PDU B 2 H4D1 H 0.4269 0.7659 0.1240 0.082 Uiso 0.411(3) 1 calc PR B 2 H4D2 H 0.4391 0.8548 0.1200 0.082 Uiso 0.411(3) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0314(2) 0.0455(3) 0.0341(2) 0.00236(19) -0.00039(15) 0.0005(2) N1 0.034(2) 0.049(3) 0.045(2) -0.001(2) -0.0053(18) -0.001(2) N2 0.036(2) 0.050(3) 0.042(2) 0.008(2) -0.0073(19) -0.009(2) N3 0.036(2) 0.053(3) 0.038(2) -0.001(2) -0.0040(18) 0.000(2) N4 0.033(2) 0.043(3) 0.044(2) 0.000(2) 0.0000(18) 0.003(2) N5 0.029(2) 0.048(3) 0.033(2) 0.0008(19) 0.0026(17) 0.0064(19) N6 0.031(2) 0.050(3) 0.034(2) -0.0004(19) 0.0034(18) -0.0003(19) C1 0.042(3) 0.060(4) 0.048(3) 0.000(3) 0.001(2) 0.006(3) C2 0.046(3) 0.069(5) 0.053(3) -0.010(3) 0.006(3) 0.004(3) C3 0.040(3) 0.067(5) 0.078(4) -0.017(4) 0.001(3) 0.007(3) C4 0.043(3) 0.051(4) 0.072(4) -0.006(3) -0.019(3) 0.003(3) C5 0.036(3) 0.046(3) 0.048(3) -0.006(3) -0.008(2) 0.000(2) C6 0.045(3) 0.049(4) 0.049(3) 0.002(3) -0.013(2) -0.003(3) C7 0.083(5) 0.047(4) 0.052(4) 0.006(3) -0.013(3) 0.002(3) C8 0.109(6) 0.051(4) 0.054(4) 0.013(3) -0.015(4) -0.012(4) C9 0.084(5) 0.056(4) 0.040(3) 0.006(3) -0.004(3) -0.021(4) C10 0.045(3) 0.061(4) 0.035(3) 0.004(3) -0.006(2) -0.012(3) C11 0.036(3) 0.065(4) 0.036(3) -0.004(3) -0.001(2) -0.013(3) C12 0.047(3) 0.089(5) 0.036(3) -0.006(3) 0.005(2) -0.017(4) C13 0.041(3) 0.107(6) 0.045(3) -0.013(4) 0.008(3) -0.004(4) C14 0.045(3) 0.087(5) 0.055(4) -0.008(3) 0.004(3) 0.014(3) C15 0.041(3) 0.068(4) 0.044(3) -0.002(3) 0.005(2) 0.006(3) C16 0.041(3) 0.044(3) 0.055(3) 0.000(3) 0.000(3) 0.001(3) C17 0.043(3) 0.047(4) 0.077(4) -0.011(3) -0.001(3) -0.002(3) C18 0.039(3) 0.066(4) 0.055(3) -0.012(3) -0.013(2) 0.013(3) C19 0.049(3) 0.055(4) 0.040(3) -0.004(3) -0.005(2) 0.007(3) C20 0.035(3) 0.048(3) 0.036(3) -0.005(2) 0.002(2) 0.009(2) C21 0.032(3) 0.052(3) 0.036(3) 0.001(2) 0.001(2) 0.004(2) C22 0.044(3) 0.067(4) 0.048(3) 0.011(3) -0.012(3) 0.004(3) C23 0.053(4) 0.062(4) 0.067(4) 0.030(3) -0.012(3) -0.009(3) C24 0.044(3) 0.050(4) 0.064(4) 0.017(3) -0.003(3) -0.006(3) C25 0.030(3) 0.047(3) 0.044(3) 0.001(2) 0.000(2) 0.004(2) C26 0.030(3) 0.052(4) 0.043(3) -0.003(2) 0.003(2) 0.001(2) C27 0.035(3) 0.053(4) 0.043(3) -0.002(2) 0.004(2) 0.002(2) C28 0.035(3) 0.073(4) 0.045(3) -0.013(3) 0.003(2) -0.009(3) C29 0.041(3) 0.086(5) 0.037(3) 0.005(3) -0.003(2) -0.010(3) C30 0.040(3) 0.070(4) 0.041(3) 0.008(3) -0.002(2) -0.005(3) Cl2 0.0601(9) 0.0643(10) 0.0453(8) -0.0029(7) -0.0149(6) 0.0111(7) Cl1 0.0431(8) 0.0876(12) 0.0379(7) -0.0023(7) 0.0034(6) 0.0050(7) Cl1S 0.0648(11) 0.0870(14) 0.1029(14) -0.0264(11) 0.0092(10) -0.0130(10) Cl2S 0.0747(13) 0.130(2) 0.0944(14) -0.0368(13) 0.0155(11) 0.0006(12) C1S 0.059(5) 0.127(8) 0.123(7) -0.060(6) 0.008(4) -0.010(5) Cl3S 0.0821(13) 0.1188(17) 0.0651(11) 0.0203(11) 0.0027(9) 0.0149(12) Cl4S 0.0756(12) 0.0774(14) 0.1165(16) 0.0236(12) 0.0086(11) -0.0059(10) C2S 0.043(4) 0.083(5) 0.116(6) 0.024(4) 0.005(4) 0.000(3) Cl5S 0.076(4) 0.123(2) 0.090(4) 0.000(3) -0.012(2) -0.021(2) Cl6S 0.102(8) 0.107(3) 0.076(4) 0.019(3) -0.017(4) -0.009(4) C3S 0.064(11) 0.132(7) 0.065(5) 0.008(5) -0.032(8) -0.044(7) Cl5D 0.076(4) 0.123(2) 0.090(4) 0.000(3) -0.012(2) -0.021(2) Cl6D 0.102(8) 0.107(3) 0.076(4) 0.019(3) -0.017(4) -0.009(4) C3D 0.064(11) 0.132(7) 0.065(5) 0.008(5) -0.032(8) -0.044(7) Cl7S 0.066(2) 0.105(4) 0.0691(13) 0.020(3) 0.0019(14) 0.002(2) Cl8S 0.0784(16) 0.0723(18) 0.0875(17) -0.0133(13) -0.0126(14) -0.0015(13) C4S 0.056(6) 0.070(7) 0.078(6) -0.007(6) 0.000(5) 0.003(5) Cl7D 0.066(2) 0.105(4) 0.0691(13) 0.020(3) 0.0019(14) 0.002(2) Cl8D 0.0784(16) 0.0723(18) 0.0875(17) -0.0133(13) -0.0126(14) -0.0015(13) C4D 0.056(6) 0.070(7) 0.078(6) -0.007(6) 0.000(5) 0.003(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 N2 1.969(4) . ? Ru1 N5 1.973(4) . ? Ru1 N6 2.064(4) . ? Ru1 N1 2.066(4) . ? Ru1 N3 2.070(4) . ? Ru1 N4 2.080(4) . ? N1 C1 1.343(6) . ? N1 C5 1.362(7) . ? N2 C6 1.353(7) . ? N2 C10 1.378(6) . ? N3 C15 1.345(7) . ? N3 C11 1.373(7) . ? N4 C16 1.331(7) . ? N4 C20 1.368(6) . ? N5 C21 1.361(6) . ? N5 C25 1.366(7) . ? N6 C30 1.341(7) . ? N6 C26 1.371(7) . ? C1 C2 1.380(8) . ? C1 H1 0.9500 . ? C2 C3 1.362(9) . ? C2 H2 0.9500 . ? C3 C4 1.376(9) . ? C3 H3 0.9500 . ? C4 C5 1.403(8) . ? C4 H4 0.9500 . ? C5 C6 1.475(7) . ? C6 C7 1.386(8) . ? C7 C8 1.382(9) . ? C7 H7 0.9500 . ? C8 C9 1.385(10) . ? C8 H8 0.9500 . ? C9 C10 1.379(8) . ? C9 H9 0.9500 . ? C10 C11 1.468(8) . ? C11 C12 1.394(7) . ? C12 C13 1.368(9) . ? C12 H12 0.9500 . ? C13 C14 1.382(9) . ? C13 H13 0.9500 . ? C14 C15 1.378(7) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.388(8) . ? C16 H16 0.9500 . ? C17 C18 1.378(8) . ? C17 H17 0.9500 . ? C18 C19 1.363(8) . ? C18 H18 0.9500 . ? C19 C20 1.399(7) . ? C19 H19 0.9500 . ? C20 C21 1.473(7) . ? C21 C22 1.382(7) . ? C22 C23 1.380(8) . ? C22 H22 0.9500 . ? C23 C24 1.394(8) . ? C23 H23 0.9500 . ? C24 C25 1.371(7) . ? C24 H24 0.9500 . ? C25 C26 1.468(7) . ? C26 C27 1.374(7) . ? C27 C28 1.377(8) . ? C27 H27 0.9500 . ? C28 C29 1.371(8) . ? C28 H28 0.9500 . ? C29 C30 1.377(8) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? Cl1S C1S 1.747(8) . ? Cl2S C1S 1.709(7) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? Cl3S C2S 1.763(8) . ? Cl4S C2S 1.768(8) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? Cl5S C3S 1.780(12) . ? Cl6S C3S 1.783(11) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? Cl5D C3D 1.780(15) . ? Cl6D C3D 1.781(15) . ? C3D H3D1 0.9900 . ? C3D H3D2 0.9900 . ? Cl7S C4S 1.778(10) . ? Cl8S C4S 1.749(10) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? Cl7D C4D 1.755(12) . ? Cl8D C4D 1.774(12) . ? C4D H4D1 0.9900 . ? C4D H4D2 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 N2 Ru1 N5 177.88(17) . . ? N2 Ru1 N6 98.63(17) . . ? N5 Ru1 N6 79.26(17) . . ? N2 Ru1 N1 78.97(18) . . ? N5 Ru1 N1 100.97(16) . . ? N6 Ru1 N1 91.86(16) . . ? N2 Ru1 N3 79.37(18) . . ? N5 Ru1 N3 100.67(16) . . ? N6 Ru1 N3 91.10(16) . . ? N1 Ru1 N3 158.33(18) . . ? N2 Ru1 N4 103.06(17) . . ? N5 Ru1 N4 79.06(17) . . ? N6 Ru1 N4 158.31(17) . . ? N1 Ru1 N4 91.71(16) . . ? N3 Ru1 N4 93.43(16) . . ? C1 N1 C5 118.7(5) . . ? C1 N1 Ru1 127.1(4) . . ? C5 N1 Ru1 114.1(3) . . ? C6 N2 C10 121.7(5) . . ? C6 N2 Ru1 119.4(4) . . ? C10 N2 Ru1 118.8(4) . . ? C15 N3 C11 118.3(5) . . ? C15 N3 Ru1 127.5(4) . . ? C11 N3 Ru1 114.1(4) . . ? C16 N4 C20 118.7(5) . . ? C16 N4 Ru1 127.6(4) . . ? C20 N4 Ru1 113.7(3) . . ? C21 N5 C25 121.6(4) . . ? C21 N5 Ru1 119.4(4) . . ? C25 N5 Ru1 119.0(3) . . ? C30 N6 C26 118.5(5) . . ? C30 N6 Ru1 127.5(4) . . ? C26 N6 Ru1 114.0(3) . . ? N1 C1 C2 122.3(6) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.3(6) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 120.1(6) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 118.8(6) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 120.8(5) . . ? N1 C5 C6 115.1(5) . . ? C4 C5 C6 124.0(5) . . ? N2 C6 C7 120.7(5) . . ? N2 C6 C5 112.3(5) . . ? C7 C6 C5 127.0(5) . . ? C8 C7 C6 117.6(6) . . ? C8 C7 H7 121.2 . . ? C6 C7 H7 121.2 . . ? C7 C8 C9 122.1(6) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C10 C9 C8 118.9(6) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? N2 C10 C9 119.1(5) . . ? N2 C10 C11 112.6(4) . . ? C9 C10 C11 128.3(5) . . ? N3 C11 C12 120.6(6) . . ? N3 C11 C10 115.1(4) . . ? C12 C11 C10 124.3(5) . . ? C13 C12 C11 120.1(6) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 119.0(5) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C15 C14 C13 119.3(6) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? N3 C15 C14 122.5(6) . . ? N3 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? N4 C16 C17 122.4(5) . . ? N4 C16 H16 118.8 . . ? C17 C16 H16 118.8 . . ? C18 C17 C16 119.0(6) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C19 C18 C17 119.4(5) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 119.7(5) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? N4 C20 C19 120.6(5) . . ? N4 C20 C21 115.5(4) . . ? C19 C20 C21 123.8(5) . . ? N5 C21 C22 119.8(5) . . ? N5 C21 C20 112.4(4) . . ? C22 C21 C20 127.8(5) . . ? C23 C22 C21 118.9(5) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C22 C23 C24 120.9(5) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 118.9(5) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? N5 C25 C24 119.9(5) . . ? N5 C25 C26 112.4(5) . . ? C24 C25 C26 127.6(5) . . ? N6 C26 C27 120.5(5) . . ? N6 C26 C25 115.3(5) . . ? C27 C26 C25 124.2(5) . . ? C26 C27 C28 120.3(5) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 119.2(5) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C30 118.8(5) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? N6 C30 C29 122.7(5) . . ? N6 C30 H30 118.7 . . ? C29 C30 H30 118.7 . . ? Cl2S C1S Cl1S 112.2(4) . . ? Cl2S C1S H1S1 109.2 . . ? Cl1S C1S H1S1 109.2 . . ? Cl2S C1S H1S2 109.2 . . ? Cl1S C1S H1S2 109.2 . . ? H1S1 C1S H1S2 107.9 . . ? Cl3S C2S Cl4S 111.9(4) . . ? Cl3S C2S H2S1 109.2 . . ? Cl4S C2S H2S1 109.2 . . ? Cl3S C2S H2S2 109.2 . . ? Cl4S C2S H2S2 109.2 . . ? H2S1 C2S H2S2 107.9 . . ? Cl5S C3S Cl6S 110.3(9) . . ? Cl5S C3S H3S1 109.6 . . ? Cl6S C3S H3S1 109.6 . . ? Cl5S C3S H3S2 109.6 . . ? Cl6S C3S H3S2 109.6 . . ? H3S1 C3S H3S2 108.1 . . ? Cl5D C3D Cl6D 111.2(15) . . ? Cl5D C3D H3D1 109.4 . . ? Cl6D C3D H3D1 109.4 . . ? Cl5D C3D H3D2 109.4 . . ? Cl6D C3D H3D2 109.4 . . ? H3D1 C3D H3D2 108.0 . . ? Cl8S C4S Cl7S 110.3(6) . . ? Cl8S C4S H4S1 109.6 . . ? Cl7S C4S H4S1 109.6 . . ? Cl8S C4S H4S2 109.6 . . ? Cl7S C4S H4S2 109.6 . . ? H4S1 C4S H4S2 108.1 . . ? Cl7D C4D Cl8D 110.0(9) . . ? Cl7D C4D H4D1 109.7 . . ? Cl8D C4D H4D1 109.7 . . ? Cl7D C4D H4D2 109.7 . . ? Cl8D C4D H4D2 109.7 . . ? H4D1 C4D H4D2 108.2 . . ? 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 Ru1 N1 C1 177.7(5) . . . . ? N5 Ru1 N1 C1 -4.4(5) . . . . ? N6 Ru1 N1 C1 -83.8(4) . . . . ? N3 Ru1 N1 C1 178.5(4) . . . . ? N4 Ru1 N1 C1 74.8(4) . . . . ? N2 Ru1 N1 C5 -0.5(3) . . . . ? N5 Ru1 N1 C5 177.3(3) . . . . ? N6 Ru1 N1 C5 97.9(4) . . . . ? N3 Ru1 N1 C5 0.2(7) . . . . ? N4 Ru1 N1 C5 -103.5(4) . . . . ? N5 Ru1 N2 C6 -86(5) . . . . ? N6 Ru1 N2 C6 -88.0(4) . . . . ? N1 Ru1 N2 C6 2.2(4) . . . . ? N3 Ru1 N2 C6 -177.5(4) . . . . ? N4 Ru1 N2 C6 91.4(4) . . . . ? N5 Ru1 N2 C10 90(5) . . . . ? N6 Ru1 N2 C10 88.0(4) . . . . ? N1 Ru1 N2 C10 178.2(4) . . . . ? N3 Ru1 N2 C10 -1.5(4) . . . . ? N4 Ru1 N2 C10 -92.6(4) . . . . ? N2 Ru1 N3 C15 178.6(5) . . . . ? N5 Ru1 N3 C15 0.8(5) . . . . ? N6 Ru1 N3 C15 80.1(5) . . . . ? N1 Ru1 N3 C15 177.9(4) . . . . ? N4 Ru1 N3 C15 -78.7(5) . . . . ? N2 Ru1 N3 C11 0.0(3) . . . . ? N5 Ru1 N3 C11 -177.8(3) . . . . ? N6 Ru1 N3 C11 -98.6(4) . . . . ? N1 Ru1 N3 C11 -0.7(7) . . . . ? N4 Ru1 N3 C11 102.7(4) . . . . ? N2 Ru1 N4 C16 -0.4(4) . . . . ? N5 Ru1 N4 C16 179.5(4) . . . . ? N6 Ru1 N4 C16 178.1(4) . . . . ? N1 Ru1 N4 C16 78.7(4) . . . . ? N3 Ru1 N4 C16 -80.3(4) . . . . ? N2 Ru1 N4 C20 -179.7(3) . . . . ? N5 Ru1 N4 C20 0.2(3) . . . . ? N6 Ru1 N4 C20 -1.2(6) . . . . ? N1 Ru1 N4 C20 -100.6(3) . . . . ? N3 Ru1 N4 C20 100.4(3) . . . . ? N2 Ru1 N5 C21 178(100) . . . . ? N6 Ru1 N5 C21 179.6(4) . . . . ? N1 Ru1 N5 C21 89.8(3) . . . . ? N3 Ru1 N5 C21 -91.3(3) . . . . ? N4 Ru1 N5 C21 0.2(3) . . . . ? N2 Ru1 N5 C25 -3(5) . . . . ? N6 Ru1 N5 C25 -1.4(3) . . . . ? N1 Ru1 N5 C25 -91.2(4) . . . . ? N3 Ru1 N5 C25 87.7(4) . . . . ? N4 Ru1 N5 C25 179.2(4) . . . . ? N2 Ru1 N6 C30 1.3(4) . . . . ? N5 Ru1 N6 C30 -178.6(4) . . . . ? N1 Ru1 N6 C30 -77.8(4) . . . . ? N3 Ru1 N6 C30 80.7(4) . . . . ? N4 Ru1 N6 C30 -177.2(4) . . . . ? N2 Ru1 N6 C26 -179.7(3) . . . . ? N5 Ru1 N6 C26 0.4(3) . . . . ? N1 Ru1 N6 C26 101.2(3) . . . . ? N3 Ru1 N6 C26 -100.3(3) . . . . ? N4 Ru1 N6 C26 1.9(6) . . . . ? C5 N1 C1 C2 1.2(8) . . . . ? Ru1 N1 C1 C2 -177.0(4) . . . . ? N1 C1 C2 C3 -0.6(9) . . . . ? C1 C2 C3 C4 -0.2(9) . . . . ? C2 C3 C4 C5 0.5(9) . . . . ? C1 N1 C5 C4 -1.0(8) . . . . ? Ru1 N1 C5 C4 177.5(4) . . . . ? C1 N1 C5 C6 -179.4(5) . . . . ? Ru1 N1 C5 C6 -1.0(6) . . . . ? C3 C4 C5 N1 0.1(8) . . . . ? C3 C4 C5 C6 178.4(5) . . . . ? C10 N2 C6 C7 -1.0(8) . . . . ? Ru1 N2 C6 C7 174.9(4) . . . . ? C10 N2 C6 C5 -179.1(4) . . . . ? Ru1 N2 C6 C5 -3.2(6) . . . . ? N1 C5 C6 N2 2.6(7) . . . . ? C4 C5 C6 N2 -175.8(5) . . . . ? N1 C5 C6 C7 -175.4(5) . . . . ? C4 C5 C6 C7 6.2(9) . . . . ? N2 C6 C7 C8 -0.1(9) . . . . ? C5 C6 C7 C8 177.8(6) . . . . ? C6 C7 C8 C9 1.9(10) . . . . ? C7 C8 C9 C10 -2.5(10) . . . . ? C6 N2 C10 C9 0.3(8) . . . . ? Ru1 N2 C10 C9 -175.6(4) . . . . ? C6 N2 C10 C11 178.5(5) . . . . ? Ru1 N2 C10 C11 2.6(6) . . . . ? C8 C9 C10 N2 1.4(9) . . . . ? C8 C9 C10 C11 -176.5(6) . . . . ? C15 N3 C11 C12 1.3(7) . . . . ? Ru1 N3 C11 C12 -179.9(4) . . . . ? C15 N3 C11 C10 -177.4(5) . . . . ? Ru1 N3 C11 C10 1.3(6) . . . . ? N2 C10 C11 N3 -2.5(6) . . . . ? C9 C10 C11 N3 175.5(5) . . . . ? N2 C10 C11 C12 178.8(5) . . . . ? C9 C10 C11 C12 -3.2(9) . . . . ? N3 C11 C12 C13 -1.2(8) . . . . ? C10 C11 C12 C13 177.4(5) . . . . ? C11 C12 C13 C14 -0.1(9) . . . . ? C12 C13 C14 C15 1.3(9) . . . . ? C11 N3 C15 C14 -0.1(8) . . . . ? Ru1 N3 C15 C14 -178.7(4) . . . . ? C13 C14 C15 N3 -1.2(9) . . . . ? C20 N4 C16 C17 1.6(7) . . . . ? Ru1 N4 C16 C17 -177.7(4) . . . . ? N4 C16 C17 C18 -1.3(8) . . . . ? C16 C17 C18 C19 -0.4(8) . . . . ? C17 C18 C19 C20 1.6(8) . . . . ? C16 N4 C20 C19 -0.2(7) . . . . ? Ru1 N4 C20 C19 179.1(4) . . . . ? C16 N4 C20 C21 -179.9(4) . . . . ? Ru1 N4 C20 C21 -0.6(5) . . . . ? C18 C19 C20 N4 -1.4(7) . . . . ? C18 C19 C20 C21 178.3(5) . . . . ? C25 N5 C21 C22 0.9(7) . . . . ? Ru1 N5 C21 C22 179.9(4) . . . . ? C25 N5 C21 C20 -179.5(4) . . . . ? Ru1 N5 C21 C20 -0.5(5) . . . . ? N4 C20 C21 N5 0.7(6) . . . . ? C19 C20 C21 N5 -179.0(4) . . . . ? N4 C20 C21 C22 -179.7(5) . . . . ? C19 C20 C21 C22 0.6(8) . . . . ? N5 C21 C22 C23 -0.9(8) . . . . ? C20 C21 C22 C23 179.6(5) . . . . ? C21 C22 C23 C24 0.3(9) . . . . ? C22 C23 C24 C25 0.2(9) . . . . ? C21 N5 C25 C24 -0.3(7) . . . . ? Ru1 N5 C25 C24 -179.3(4) . . . . ? C21 N5 C25 C26 -179.0(4) . . . . ? Ru1 N5 C25 C26 2.0(5) . . . . ? C23 C24 C25 N5 -0.2(8) . . . . ? C23 C24 C25 C26 178.2(5) . . . . ? C30 N6 C26 C27 -0.1(7) . . . . ? Ru1 N6 C26 C27 -179.2(4) . . . . ? C30 N6 C26 C25 179.7(4) . . . . ? Ru1 N6 C26 C25 0.5(5) . . . . ? N5 C25 C26 N6 -1.6(6) . . . . ? C24 C25 C26 N6 179.9(5) . . . . ? N5 C25 C26 C27 178.2(5) . . . . ? C24 C25 C26 C27 -0.4(8) . . . . ? N6 C26 C27 C28 -0.4(7) . . . . ? C25 C26 C27 C28 179.9(5) . . . . ? C26 C27 C28 C29 0.0(8) . . . . ? C27 C28 C29 C30 0.9(8) . . . . ? C26 N6 C30 C29 1.1(8) . . . . ? Ru1 N6 C30 C29 -179.9(4) . . . . ? C28 C29 C30 N6 -1.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.695 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.088 #===END