Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Mallayan Andavar' _publ_contact_author_address ; Chemistry Bharathidasan University School of Chemistry Bharathidasan University Tiruchirappalli Southern 620 024 INDIA ; _publ_contact_author_email PALANIM51@YAHOO.COM _publ_section_title ; Mixed ligand ruthenium(II) complexes of bis(pyrid-2-yl)-/bis(benzimidazol-2-yl)-dithioether and diimines: Study of non-covalent DNA binding and cytotoxicity ; loop_ _publ_author_name 'Mallayan Andavar' 'Mariappan Murali' 'Venugopal Rajendiran' 'Sarika Shinka' 'Kumaravel Somasundaram' ; E.Suresh ; data_a _database_code_depnum_ccdc_archive 'CCDC 653788' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 F12 N4 O3 P2 Ru S2' _chemical_formula_weight 923.67 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 '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 11.0191(16) _cell_length_b 11.9487(15) _cell_length_c 15.368(4) _cell_angle_alpha 69.991(14) _cell_angle_beta 87.531(17) _cell_angle_gamma 73.954(12) _cell_volume 1824.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plates _exptl_crystal_colour RED _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8108 _exptl_absorpt_correction_T_max 0.9306 _exptl_special_details ; ? ; _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 'Enraf-Noinus-CAD4 CCD diffractometer ' _diffrn_measurement_method 'OMEGA-Two Theta SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6841 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 24.98 _reflns_number_total 6402 _reflns_number_gt 5653 _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 ORTEP _computing_publication_material ? _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^)+(0.0879P)^2^+2.4901P] 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 6402 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1519 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.006 _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 Ru1 Ru 0.89200(3) 0.66019(3) 0.68703(2) 0.03338(14) Uani 1 d . . . N1 N 1.0905(3) 0.5634(3) 0.7104(2) 0.0350(7) Uani 1 d . . . N2 N 0.6959(4) 0.7588(3) 0.6561(3) 0.0413(8) Uani 1 d . . . N3 N 0.8842(3) 0.7082(3) 0.8084(3) 0.0383(8) Uani 1 d . . . N4 N 0.8541(3) 0.5041(3) 0.7872(2) 0.0349(7) Uani 1 d . . . S1 S 0.93122(13) 0.83834(10) 0.58495(8) 0.0506(3) Uani 1 d . . . S2 S 0.90112(13) 0.59101(10) 0.56361(7) 0.0458(3) Uani 1 d . . . C1 C 1.1242(4) 0.4429(4) 0.7218(3) 0.0400(9) Uani 1 d . . . H1 H 1.0606 0.4050 0.7229 0.065(3) Uiso 1 calc R . . C2 C 1.2489(5) 0.3711(5) 0.7320(4) 0.0512(11) Uani 1 d . . . H2 H 1.2685 0.2874 0.7394 0.065(3) Uiso 1 calc R . . C3 C 1.3420(5) 0.4265(6) 0.7310(4) 0.0645(15) Uani 1 d . . . H3 H 1.4266 0.3811 0.7380 0.065(3) Uiso 1 calc R . . C4 C 1.3090(5) 0.5492(5) 0.7194(4) 0.0595(13) Uani 1 d . . . H4 H 1.3720 0.5876 0.7188 0.065(3) Uiso 1 calc R . . C5 C 1.1862(5) 0.6164(4) 0.7088(3) 0.0436(10) Uani 1 d . . . C6 C 1.1544(5) 0.7527(5) 0.6924(4) 0.0589(14) Uani 1 d . . . H6A H 1.2305 0.7736 0.7022 0.065(3) Uiso 1 calc R . . H6B H 1.0947 0.7725 0.7368 0.065(3) Uiso 1 calc R . . C7 C 1.0980(6) 0.8298(5) 0.5950(5) 0.0737(18) Uani 1 d . . . H7A H 1.1439 0.7936 0.5515 0.065(3) Uiso 1 calc R . . H7B H 1.1069 0.9129 0.5792 0.065(3) Uiso 1 calc R . . C8 C 0.9223(8) 0.8261(5) 0.4712(4) 0.079(2) Uani 1 d . . . H8A H 0.8350 0.8592 0.4469 0.065(3) Uiso 1 calc R . . H8B H 0.9713 0.8758 0.4297 0.065(3) Uiso 1 calc R . . C9 C 0.9705(7) 0.6956(5) 0.4734(4) 0.0714(18) Uani 1 d . . . H9A H 1.0617 0.6685 0.4842 0.065(3) Uiso 1 calc R . . H9B H 0.9510 0.6920 0.4136 0.065(3) Uiso 1 calc R . . C10 C 0.7446(6) 0.6207(6) 0.5148(4) 0.0739(18) Uani 1 d . . . H10A H 0.7202 0.7027 0.4678 0.065(3) Uiso 1 calc R . . H10B H 0.7450 0.5607 0.4853 0.065(3) Uiso 1 calc R . . C11 C 0.6498(5) 0.6127(5) 0.5886(4) 0.0608(14) Uani 1 d . . . H11A H 0.5756 0.5999 0.5661 0.065(3) Uiso 1 calc R . . H11B H 0.6861 0.5409 0.6429 0.065(3) Uiso 1 calc R . . C12 C 0.6097(5) 0.7250(5) 0.6165(3) 0.0482(11) Uani 1 d . . . C13 C 0.4850(5) 0.7962(6) 0.5973(4) 0.0635(14) Uani 1 d . . . H13 H 0.4284 0.7724 0.5691 0.065(3) Uiso 1 calc R . . C14 C 0.4448(5) 0.9017(6) 0.6198(5) 0.0743(18) Uani 1 d . . . H14 H 0.3609 0.9493 0.6083 0.065(3) Uiso 1 calc R . . C15 C 0.5315(5) 0.9352(5) 0.6597(5) 0.0671(15) Uani 1 d . . . H15 H 0.5073 1.0061 0.6759 0.065(3) Uiso 1 calc R . . C16 C 0.6537(5) 0.8631(4) 0.6752(4) 0.0500(11) Uani 1 d . . . H16 H 0.7116 0.8884 0.7010 0.065(3) Uiso 1 calc R . . C17 C 0.8449(4) 0.3999(4) 0.7778(3) 0.0431(10) Uani 1 d . . . H17 H 0.8515 0.3937 0.7191 0.065(3) Uiso 1 calc R . . C18 C 0.8260(5) 0.3003(5) 0.8508(4) 0.0543(12) Uani 1 d . . . H18 H 0.8208 0.2294 0.8405 0.065(3) Uiso 1 calc R . . C19 C 0.8154(5) 0.3068(5) 0.9367(4) 0.0586(13) Uani 1 d . . . H19 H 0.8032 0.2403 0.9863 0.065(3) Uiso 1 calc R . . C20 C 0.8228(4) 0.4149(5) 0.9506(3) 0.0480(11) Uani 1 d . . . C21 C 0.8454(4) 0.5103(4) 0.8741(3) 0.0363(9) Uani 1 d . . . C22 C 0.8591(4) 0.6199(4) 0.8851(3) 0.0382(9) Uani 1 d . . . C23 C 0.8456(4) 0.6339(5) 0.9721(3) 0.0491(11) Uani 1 d . . . C24 C 0.8580(5) 0.7438(6) 0.9790(4) 0.0633(15) Uani 1 d . . . H24 H 0.8493 0.7569 1.0355 0.065(3) Uiso 1 calc R . . C25 C 0.8827(5) 0.8312(6) 0.9025(4) 0.0595(14) Uani 1 d . . . H25 H 0.8914 0.9047 0.9062 0.065(3) Uiso 1 calc R . . C26 C 0.8950(5) 0.8105(5) 0.8190(4) 0.0491(11) Uani 1 d . . . H26 H 0.9117 0.8718 0.7673 0.065(3) Uiso 1 calc R . . C27 C 0.8199(5) 0.5367(6) 1.0478(3) 0.0634(15) Uani 1 d . . . H27 H 0.8103 0.5454 1.1058 0.065(3) Uiso 1 calc R . . C28 C 0.8091(5) 0.4326(6) 1.0380(3) 0.0646(15) Uani 1 d . . . H28 H 0.7922 0.3708 1.0892 0.065(3) Uiso 1 calc R . . P1 P 1.16058(16) 1.03541(14) 0.81095(11) 0.0611(4) Uani 1 d . . . P2 P 0.67817(13) 1.22902(14) 0.63527(11) 0.0566(4) Uani 1 d . . . F1 F 0.7224(5) 1.1321(4) 0.5855(4) 0.1074(15) Uani 1 d . . . F2 F 0.5375(4) 1.2327(5) 0.6184(4) 0.1062(15) Uani 1 d . . . F3 F 0.6370(4) 1.3240(5) 0.6883(4) 0.1108(17) Uani 1 d . . . F4 F 0.8173(4) 1.2316(6) 0.6499(4) 0.1207(18) Uani 1 d . . . F5 F 0.6697(6) 1.3319(5) 0.5373(4) 0.131(2) Uani 1 d . . . F6 F 0.6885(6) 1.1199(5) 0.7297(3) 0.1289(19) Uani 1 d . . . F7 F 1.0832(5) 1.1747(4) 0.7658(5) 0.1226(19) Uani 1 d . . . F8 F 1.2521(6) 1.0607(6) 0.7334(5) 0.156(3) Uani 1 d . . . F9 F 1.0783(7) 1.0030(5) 0.7471(4) 0.156(3) Uani 1 d . . . F10 F 1.2312(7) 0.8955(5) 0.8531(5) 0.158(3) Uani 1 d . . . F11 F 1.2387(9) 1.0708(7) 0.8699(5) 0.201(4) Uani 1 d . . . F12 F 1.0624(7) 1.0129(7) 0.8856(5) 0.171(3) Uani 1 d . . . O1A O 1.522(2) 0.779(3) 0.921(2) 0.181(9) Uiso 0.40 d P . . O1 O 1.4904(17) 0.7025(19) 0.9820(14) 0.193(7) Uiso 0.60 d P . . O2 O 1.5251(14) 0.5680(15) 0.8537(11) 0.132(5) Uiso 0.50 d P . . O2A O 1.5116(18) 0.645(2) 0.8820(15) 0.175(7) Uiso 0.50 d P . . O3 O 1.540(3) 1.052(4) 0.924(3) 0.260(15) Uiso 0.40 d P . . O3A O 1.492(2) 1.133(2) 1.0099(19) 0.270(11) Uiso 0.60 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 0.0482(2) 0.0269(2) 0.0269(2) -0.01152(14) 0.00530(14) -0.01106(14) N1 0.0470(19) 0.0260(16) 0.0327(17) -0.0119(14) 0.0093(15) -0.0103(14) N2 0.052(2) 0.0302(18) 0.0386(19) -0.0118(15) -0.0002(16) -0.0058(16) N3 0.0418(19) 0.0386(19) 0.040(2) -0.0213(16) 0.0074(15) -0.0114(15) N4 0.0407(18) 0.0352(18) 0.0304(17) -0.0112(14) 0.0032(14) -0.0136(15) S1 0.0770(8) 0.0264(5) 0.0434(6) -0.0100(5) 0.0171(6) -0.0111(5) S2 0.0724(8) 0.0345(6) 0.0290(5) -0.0149(4) 0.0029(5) -0.0072(5) C1 0.049(2) 0.040(2) 0.035(2) -0.0159(18) 0.0046(18) -0.0146(19) C2 0.055(3) 0.043(3) 0.053(3) -0.019(2) 0.009(2) -0.008(2) C3 0.046(3) 0.066(4) 0.078(4) -0.027(3) 0.014(3) -0.009(3) C4 0.051(3) 0.061(3) 0.071(3) -0.021(3) 0.015(3) -0.026(3) C5 0.056(3) 0.037(2) 0.041(2) -0.0133(19) 0.014(2) -0.019(2) C6 0.063(3) 0.046(3) 0.080(4) -0.028(3) 0.021(3) -0.029(2) C7 0.084(4) 0.036(3) 0.091(5) -0.008(3) 0.036(4) -0.025(3) C8 0.141(6) 0.041(3) 0.040(3) -0.005(2) 0.017(3) -0.015(3) C9 0.124(5) 0.047(3) 0.038(3) -0.016(2) 0.029(3) -0.019(3) C10 0.090(4) 0.076(4) 0.058(3) -0.043(3) -0.023(3) 0.003(3) C11 0.068(3) 0.056(3) 0.065(3) -0.028(3) -0.016(3) -0.014(3) C12 0.057(3) 0.046(3) 0.042(2) -0.013(2) -0.001(2) -0.017(2) C13 0.053(3) 0.065(4) 0.074(4) -0.025(3) -0.003(3) -0.017(3) C14 0.045(3) 0.066(4) 0.110(5) -0.034(4) -0.002(3) -0.007(3) C15 0.061(3) 0.048(3) 0.093(4) -0.031(3) 0.014(3) -0.010(3) C16 0.052(3) 0.044(3) 0.058(3) -0.023(2) 0.008(2) -0.013(2) C17 0.052(3) 0.038(2) 0.042(2) -0.0114(19) -0.0010(19) -0.018(2) C18 0.062(3) 0.042(3) 0.060(3) -0.011(2) -0.005(2) -0.023(2) C19 0.064(3) 0.054(3) 0.048(3) 0.004(2) -0.002(2) -0.029(3) C20 0.045(2) 0.060(3) 0.034(2) -0.005(2) -0.0013(19) -0.021(2) C21 0.033(2) 0.043(2) 0.033(2) -0.0112(18) 0.0002(16) -0.0123(17) C22 0.036(2) 0.051(3) 0.032(2) -0.0172(19) 0.0025(17) -0.0158(19) C23 0.042(2) 0.076(3) 0.037(2) -0.030(2) 0.0034(19) -0.016(2) C24 0.063(3) 0.096(4) 0.052(3) -0.051(3) 0.010(3) -0.024(3) C25 0.060(3) 0.069(4) 0.074(4) -0.052(3) 0.007(3) -0.022(3) C26 0.053(3) 0.054(3) 0.056(3) -0.034(2) 0.015(2) -0.022(2) C27 0.065(3) 0.099(5) 0.032(2) -0.025(3) 0.008(2) -0.030(3) C28 0.066(3) 0.093(4) 0.029(2) -0.007(3) 0.003(2) -0.031(3) P1 0.0764(10) 0.0469(8) 0.0593(8) -0.0147(6) 0.0020(7) -0.0204(7) P2 0.0510(7) 0.0587(8) 0.0710(9) -0.0302(7) 0.0085(6) -0.0229(6) F1 0.129(4) 0.093(3) 0.121(4) -0.065(3) 0.039(3) -0.033(3) F2 0.063(2) 0.131(4) 0.150(4) -0.072(3) -0.001(2) -0.036(2) F3 0.085(3) 0.126(4) 0.171(5) -0.109(4) 0.026(3) -0.038(3) F4 0.059(2) 0.190(5) 0.144(4) -0.085(4) 0.016(3) -0.050(3) F5 0.178(5) 0.093(3) 0.107(4) 0.001(3) -0.019(4) -0.057(4) F6 0.168(5) 0.123(4) 0.081(3) -0.006(3) 0.011(3) -0.056(4) F7 0.107(3) 0.056(2) 0.192(6) -0.034(3) 0.007(3) -0.014(2) F8 0.142(5) 0.147(5) 0.150(5) -0.037(4) 0.081(4) -0.024(4) F9 0.234(7) 0.102(4) 0.138(5) -0.015(3) -0.079(5) -0.078(4) F10 0.193(6) 0.065(3) 0.148(5) 0.019(3) -0.041(4) 0.008(3) F11 0.296(9) 0.195(7) 0.137(5) -0.018(5) -0.097(6) -0.139(7) F12 0.214(7) 0.160(6) 0.162(6) -0.052(5) 0.101(5) -0.104(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 N4 2.105(3) . ? Ru1 N3 2.123(4) . ? Ru1 N2 2.141(4) . ? Ru1 N1 2.153(4) . ? Ru1 S2 2.3026(12) . ? Ru1 S1 2.3117(12) . ? N1 C1 1.335(5) . ? N1 C5 1.366(6) . ? N2 C16 1.333(6) . ? N2 C12 1.365(6) . ? N3 C26 1.323(6) . ? N3 C22 1.365(6) . ? N4 C17 1.332(6) . ? N4 C21 1.361(5) . ? S1 C8 1.812(6) . ? S1 C7 1.822(7) . ? S2 C10 1.804(6) . ? S2 C9 1.822(6) . ? C1 C2 1.387(7) . ? C1 H1 0.9300 . ? C2 C3 1.363(8) . ? C2 H2 0.9300 . ? C3 C4 1.358(8) . ? C3 H3 0.9300 . ? C4 C5 1.354(7) . ? C4 H4 0.9300 . ? C5 C6 1.500(7) . ? C6 C7 1.514(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.491(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.505(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.494(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.383(7) . ? C13 C14 1.372(9) . ? C13 H13 0.9300 . ? C14 C15 1.370(9) . ? C14 H14 0.9300 . ? C15 C16 1.364(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.386(7) . ? C17 H17 0.9300 . ? C18 C19 1.347(8) . ? C18 H18 0.9300 . ? C19 C20 1.403(8) . ? C19 H19 0.9300 . ? C20 C21 1.400(6) . ? C20 C28 1.425(7) . ? C21 C22 1.424(6) . ? C22 C23 1.400(6) . ? C23 C24 1.396(8) . ? C23 C27 1.419(8) . ? C24 C25 1.355(9) . ? C24 H24 0.9300 . ? C25 C26 1.383(7) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.339(9) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? P1 F11 1.506(5) . ? P1 F8 1.532(5) . ? P1 F10 1.550(5) . ? P1 F12 1.550(6) . ? P1 F7 1.567(5) . ? P1 F9 1.569(5) . ? P2 F1 1.557(4) . ? P2 F6 1.567(5) . ? P2 F2 1.568(4) . ? P2 F4 1.570(4) . ? P2 F5 1.571(5) . ? P2 F3 1.573(4) . ? O1A O1 1.18(3) . ? O1A O3A 1.71(3) 2_877 ? O2 O2A 1.12(2) . ? O3A O1A 1.71(3) 2_877 ? 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 N4 Ru1 N3 78.54(14) . . ? N4 Ru1 N2 93.31(14) . . ? N3 Ru1 N2 88.89(14) . . ? N4 Ru1 N1 88.72(13) . . ? N3 Ru1 N1 93.76(13) . . ? N2 Ru1 N1 176.94(13) . . ? N4 Ru1 S2 96.64(10) . . ? N3 Ru1 S2 175.06(10) . . ? N2 Ru1 S2 92.52(11) . . ? N1 Ru1 S2 84.97(10) . . ? N4 Ru1 S1 175.91(9) . . ? N3 Ru1 S1 97.41(10) . . ? N2 Ru1 S1 85.97(11) . . ? N1 Ru1 S1 92.16(10) . . ? S2 Ru1 S1 87.41(5) . . ? C1 N1 C5 116.8(4) . . ? C1 N1 Ru1 117.5(3) . . ? C5 N1 Ru1 125.6(3) . . ? C16 N2 C12 116.6(4) . . ? C16 N2 Ru1 117.9(3) . . ? C12 N2 Ru1 125.5(3) . . ? C26 N3 C22 117.0(4) . . ? C26 N3 Ru1 130.0(3) . . ? C22 N3 Ru1 113.0(3) . . ? C17 N4 C21 116.9(4) . . ? C17 N4 Ru1 129.2(3) . . ? C21 N4 Ru1 113.8(3) . . ? C8 S1 C7 100.4(4) . . ? C8 S1 Ru1 105.1(2) . . ? C7 S1 Ru1 110.13(18) . . ? C10 S2 C9 103.5(3) . . ? C10 S2 Ru1 110.86(19) . . ? C9 S2 Ru1 104.44(19) . . ? N1 C1 C2 123.5(4) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 118.2(5) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C4 C3 C2 118.9(5) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C5 C4 C3 121.1(5) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 N1 121.5(4) . . ? C4 C5 C6 119.3(4) . . ? N1 C5 C6 119.3(4) . . ? C5 C6 C7 111.8(5) . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C6 C7 S1 111.3(4) . . ? C6 C7 H7A 109.4 . . ? S1 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? S1 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C9 C8 S1 112.4(4) . . ? C9 C8 H8A 109.1 . . ? S1 C8 H8A 109.1 . . ? C9 C8 H8B 109.1 . . ? S1 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? C8 C9 S2 111.9(4) . . ? C8 C9 H9A 109.2 . . ? S2 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? S2 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C11 C10 S2 111.0(4) . . ? C11 C10 H10A 109.4 . . ? S2 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? S2 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 113.9(5) . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? C10 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N2 C12 C13 121.4(5) . . ? N2 C12 C11 120.3(4) . . ? C13 C12 C11 118.2(5) . . ? C14 C13 C12 120.2(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 118.3(5) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C16 C15 C14 119.1(5) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? N2 C16 C15 124.4(5) . . ? N2 C16 H16 117.8 . . ? C15 C16 H16 117.8 . . ? N4 C17 C18 123.7(4) . . ? N4 C17 H17 118.2 . . ? C18 C17 H17 118.2 . . ? C19 C18 C17 119.6(5) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 119.3(5) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C21 C20 C19 117.9(4) . . ? C21 C20 C28 118.3(5) . . ? C19 C20 C28 123.8(5) . . ? N4 C21 C20 122.6(4) . . ? N4 C21 C22 117.3(4) . . ? C20 C21 C22 120.2(4) . . ? N3 C22 C23 122.7(4) . . ? N3 C22 C21 117.4(4) . . ? C23 C22 C21 119.9(4) . . ? C24 C23 C22 117.7(5) . . ? C24 C23 C27 123.8(5) . . ? C22 C23 C27 118.5(5) . . ? C25 C24 C23 119.4(5) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 119.6(5) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? N3 C26 C25 123.6(5) . . ? N3 C26 H26 118.2 . . ? C25 C26 H26 118.2 . . ? C28 C27 C23 121.8(5) . . ? C28 C27 H27 119.1 . . ? C23 C27 H27 119.1 . . ? C27 C28 C20 121.3(5) . . ? C27 C28 H28 119.4 . . ? C20 C28 H28 119.4 . . ? F11 P1 F8 89.4(5) . . ? F11 P1 F10 93.1(4) . . ? F8 P1 F10 93.8(4) . . ? F11 P1 F12 92.8(5) . . ? F8 P1 F12 177.1(5) . . ? F10 P1 F12 88.0(4) . . ? F11 P1 F7 90.2(4) . . ? F8 P1 F7 87.0(3) . . ? F10 P1 F7 176.7(4) . . ? F12 P1 F7 91.2(4) . . ? F11 P1 F9 178.1(4) . . ? F8 P1 F9 89.7(4) . . ? F10 P1 F9 88.6(4) . . ? F12 P1 F9 88.1(4) . . ? F7 P1 F9 88.1(3) . . ? F1 P2 F6 89.2(3) . . ? F1 P2 F2 89.3(3) . . ? F6 P2 F2 90.2(3) . . ? F1 P2 F4 92.1(3) . . ? F6 P2 F4 91.9(3) . . ? F2 P2 F4 177.5(3) . . ? F1 P2 F5 87.1(3) . . ? F6 P2 F5 176.2(3) . . ? F2 P2 F5 89.3(3) . . ? F4 P2 F5 88.7(3) . . ? F1 P2 F3 178.0(3) . . ? F6 P2 F3 89.4(3) . . ? F2 P2 F3 92.0(2) . . ? F4 P2 F3 86.6(3) . . ? F5 P2 F3 94.4(3) . . ? O1 O1A O3A 90(2) . 2_877 ? 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 N4 Ru1 N1 C1 40.4(3) . . . . ? N3 Ru1 N1 C1 118.8(3) . . . . ? N2 Ru1 N1 C1 -91(2) . . . . ? S2 Ru1 N1 C1 -56.4(3) . . . . ? S1 Ru1 N1 C1 -143.6(3) . . . . ? N4 Ru1 N1 C5 -143.9(3) . . . . ? N3 Ru1 N1 C5 -65.5(4) . . . . ? N2 Ru1 N1 C5 85(2) . . . . ? S2 Ru1 N1 C5 119.3(3) . . . . ? S1 Ru1 N1 C5 32.1(3) . . . . ? N4 Ru1 N2 C16 115.7(4) . . . . ? N3 Ru1 N2 C16 37.2(4) . . . . ? N1 Ru1 N2 C16 -113(2) . . . . ? S2 Ru1 N2 C16 -147.5(3) . . . . ? S1 Ru1 N2 C16 -60.3(3) . . . . ? N4 Ru1 N2 C12 -65.5(4) . . . . ? N3 Ru1 N2 C12 -144.0(4) . . . . ? N1 Ru1 N2 C12 66(2) . . . . ? S2 Ru1 N2 C12 31.3(4) . . . . ? S1 Ru1 N2 C12 118.5(4) . . . . ? N4 Ru1 N3 C26 -177.6(4) . . . . ? N2 Ru1 N3 C26 -84.0(4) . . . . ? N1 Ru1 N3 C26 94.5(4) . . . . ? S2 Ru1 N3 C26 169.5(10) . . . . ? S1 Ru1 N3 C26 1.8(4) . . . . ? N4 Ru1 N3 C22 -0.5(3) . . . . ? N2 Ru1 N3 C22 93.1(3) . . . . ? N1 Ru1 N3 C22 -88.5(3) . . . . ? S2 Ru1 N3 C22 -13.5(14) . . . . ? S1 Ru1 N3 C22 178.9(3) . . . . ? N3 Ru1 N4 C17 -176.5(4) . . . . ? N2 Ru1 N4 C17 95.3(4) . . . . ? N1 Ru1 N4 C17 -82.4(4) . . . . ? S2 Ru1 N4 C17 2.4(4) . . . . ? S1 Ru1 N4 C17 175.1(12) . . . . ? N3 Ru1 N4 C21 -0.6(3) . . . . ? N2 Ru1 N4 C21 -88.8(3) . . . . ? N1 Ru1 N4 C21 93.5(3) . . . . ? S2 Ru1 N4 C21 178.2(3) . . . . ? S1 Ru1 N4 C21 -9.0(16) . . . . ? N4 Ru1 S1 C8 -164.8(14) . . . . ? N3 Ru1 S1 C8 -173.1(3) . . . . ? N2 Ru1 S1 C8 -84.8(3) . . . . ? N1 Ru1 S1 C8 92.8(3) . . . . ? S2 Ru1 S1 C8 7.9(3) . . . . ? N4 Ru1 S1 C7 87.9(14) . . . . ? N3 Ru1 S1 C7 79.6(3) . . . . ? N2 Ru1 S1 C7 167.9(3) . . . . ? N1 Ru1 S1 C7 -14.5(3) . . . . ? S2 Ru1 S1 C7 -99.4(2) . . . . ? N4 Ru1 S2 C10 82.3(3) . . . . ? N3 Ru1 S2 C10 95.1(12) . . . . ? N2 Ru1 S2 C10 -11.3(3) . . . . ? N1 Ru1 S2 C10 170.4(3) . . . . ? S1 Ru1 S2 C10 -97.2(3) . . . . ? N4 Ru1 S2 C9 -166.9(3) . . . . ? N3 Ru1 S2 C9 -154.0(12) . . . . ? N2 Ru1 S2 C9 99.5(3) . . . . ? N1 Ru1 S2 C9 -78.7(3) . . . . ? S1 Ru1 S2 C9 13.7(2) . . . . ? C5 N1 C1 C2 0.1(6) . . . . ? Ru1 N1 C1 C2 176.2(3) . . . . ? N1 C1 C2 C3 0.5(7) . . . . ? C1 C2 C3 C4 -0.4(8) . . . . ? C2 C3 C4 C5 -0.2(9) . . . . ? C3 C4 C5 N1 0.8(8) . . . . ? C3 C4 C5 C6 -177.5(5) . . . . ? C1 N1 C5 C4 -0.7(7) . . . . ? Ru1 N1 C5 C4 -176.4(4) . . . . ? C1 N1 C5 C6 177.5(4) . . . . ? Ru1 N1 C5 C6 1.8(6) . . . . ? C4 C5 C6 C7 111.2(6) . . . . ? N1 C5 C6 C7 -67.1(6) . . . . ? C5 C6 C7 S1 79.5(5) . . . . ? C8 S1 C7 C6 -140.4(4) . . . . ? Ru1 S1 C7 C6 -30.0(5) . . . . ? C7 S1 C8 C9 79.7(6) . . . . ? Ru1 S1 C8 C9 -34.6(6) . . . . ? S1 C8 C9 S2 49.5(7) . . . . ? C10 S2 C9 C8 77.0(6) . . . . ? Ru1 S2 C9 C8 -39.2(6) . . . . ? C9 S2 C10 C11 -143.9(4) . . . . ? Ru1 S2 C10 C11 -32.5(5) . . . . ? S2 C10 C11 C12 78.3(5) . . . . ? C16 N2 C12 C13 0.1(7) . . . . ? Ru1 N2 C12 C13 -178.7(4) . . . . ? C16 N2 C12 C11 177.1(5) . . . . ? Ru1 N2 C12 C11 -1.7(6) . . . . ? C10 C11 C12 N2 -62.5(6) . . . . ? C10 C11 C12 C13 114.6(6) . . . . ? N2 C12 C13 C14 -1.4(9) . . . . ? C11 C12 C13 C14 -178.5(6) . . . . ? C12 C13 C14 C15 1.2(10) . . . . ? C13 C14 C15 C16 0.2(10) . . . . ? C12 N2 C16 C15 1.4(8) . . . . ? Ru1 N2 C16 C15 -179.7(4) . . . . ? C14 C15 C16 N2 -1.5(9) . . . . ? C21 N4 C17 C18 0.7(7) . . . . ? Ru1 N4 C17 C18 176.4(4) . . . . ? N4 C17 C18 C19 0.4(8) . . . . ? C17 C18 C19 C20 0.4(8) . . . . ? C18 C19 C20 C21 -2.1(8) . . . . ? C18 C19 C20 C28 178.1(5) . . . . ? C17 N4 C21 C20 -2.5(6) . . . . ? Ru1 N4 C21 C20 -178.9(3) . . . . ? C17 N4 C21 C22 178.1(4) . . . . ? Ru1 N4 C21 C22 1.7(5) . . . . ? C19 C20 C21 N4 3.3(7) . . . . ? C28 C20 C21 N4 -176.9(4) . . . . ? C19 C20 C21 C22 -177.4(4) . . . . ? C28 C20 C21 C22 2.4(7) . . . . ? C26 N3 C22 C23 -0.4(6) . . . . ? Ru1 N3 C22 C23 -177.9(3) . . . . ? C26 N3 C22 C21 179.1(4) . . . . ? Ru1 N3 C22 C21 1.6(5) . . . . ? N4 C21 C22 N3 -2.3(6) . . . . ? C20 C21 C22 N3 178.4(4) . . . . ? N4 C21 C22 C23 177.2(4) . . . . ? C20 C21 C22 C23 -2.1(6) . . . . ? N3 C22 C23 C24 0.4(7) . . . . ? C21 C22 C23 C24 -179.1(4) . . . . ? N3 C22 C23 C27 -179.8(4) . . . . ? C21 C22 C23 C27 0.7(7) . . . . ? C22 C23 C24 C25 -0.3(8) . . . . ? C27 C23 C24 C25 179.9(5) . . . . ? C23 C24 C25 C26 0.2(8) . . . . ? C22 N3 C26 C25 0.3(7) . . . . ? Ru1 N3 C26 C25 177.2(4) . . . . ? C24 C25 C26 N3 -0.2(8) . . . . ? C24 C23 C27 C28 -179.9(6) . . . . ? C22 C23 C27 C28 0.3(8) . . . . ? C23 C27 C28 C20 -0.1(9) . . . . ? C21 C20 C28 C27 -1.3(8) . . . . ? C19 C20 C28 C27 178.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.118 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.108 # Attachment 'MP_Dalton_Complex_4a.CIF' data_sag _database_code_depnum_ccdc_archive 'CCDC 653789' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H35 F12 N7 O P2 Ru S2' _chemical_formula_weight 1012.82 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 14.886(4) _cell_length_b 18.276(8) _cell_length_c 16.665(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.44(2) _cell_angle_gamma 90.00 _cell_volume 4094(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 0.657 _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 0.71073 _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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6720 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 24.97 _reflns_number_total 6422 _reflns_number_gt 4095 _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 ZORTEP _computing_publication_material ? _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^)+(0.0439P)^2^+41.2994P] 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 6422 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1276 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2064 _refine_ls_wR_factor_gt 0.1690 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.000 _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 Ru1 Ru 0.78564(6) 0.91385(4) 0.26299(5) 0.0320(2) Uani 1 d . . . N1 N 0.8244(6) 0.9191(5) 0.1553(5) 0.0363(19) Uani 1 d . . . N2 N 0.8748(7) 0.9661(5) 0.0591(6) 0.051(2) Uani 1 d . . . H2 H 0.9018 0.9960 0.0362 0.062(6) Uiso 1 calc R . . N3 N 0.7537(6) 0.9047(5) 0.3760(5) 0.039(2) Uani 1 d . . . N4 N 0.7288(8) 0.8516(6) 0.4839(7) 0.068(3) Uani 1 d . . . H4 H 0.7221 0.8175 0.5165 0.062(6) Uiso 1 calc R . . N5 N 0.6387(6) 0.8760(4) 0.1840(5) 0.0365(19) Uani 1 d . . . N6 N 0.7082(6) 1.0129(4) 0.2187(5) 0.0344(19) Uani 1 d . . . S1 S 0.8684(2) 0.80221(14) 0.29345(17) 0.0440(7) Uani 1 d . . . S2 S 0.9347(2) 0.96725(17) 0.35591(18) 0.0499(7) Uani 1 d . . . C1 C 0.7354(9) 1.0348(6) 0.4233(7) 0.055(3) Uani 1 d . . . H1 H 0.7459 1.0589 0.3788 0.062(6) Uiso 1 calc R . . C2 C 0.7160(10) 1.0737(7) 0.4839(9) 0.068(4) Uani 1 d . . . H2A H 0.7113 1.1245 0.4797 0.062(6) Uiso 1 calc R . . C3 C 0.7033(12) 1.0382(9) 0.5514(10) 0.088(5) Uani 1 d . . . H3 H 0.6917 1.0661 0.5927 0.062(6) Uiso 1 calc R . . C4 C 0.7072(12) 0.9642(9) 0.5600(9) 0.084(5) Uani 1 d . . . H4A H 0.6991 0.9408 0.6060 0.062(6) Uiso 1 calc R . . C5 C 0.7239(9) 0.9260(7) 0.4966(7) 0.060(3) Uani 1 d . . . C6 C 0.7394(7) 0.9599(6) 0.4284(6) 0.042(3) Uani 1 d . . . C7 C 0.7459(8) 0.8418(6) 0.4125(7) 0.050(3) Uani 1 d . . . C8 C 0.7569(9) 0.7663(6) 0.3850(8) 0.059(3) Uani 1 d . . . H8A H 0.7034 0.7568 0.3268 0.062(6) Uiso 1 calc R . . H8B H 0.7501 0.7319 0.4264 0.062(6) Uiso 1 calc R . . C9 C 0.8544(9) 0.7525(6) 0.3810(7) 0.054(3) Uani 1 d . . . H9A H 0.8604 0.7006 0.3725 0.062(6) Uiso 1 calc R . . H9B H 0.9081 0.7661 0.4376 0.062(6) Uiso 1 calc R . . C10 C 0.9992(8) 0.8265(7) 0.3539(9) 0.065(4) Uani 1 d . . . H10A H 1.0356 0.7849 0.3888 0.062(6) Uiso 1 calc R . . H10B H 1.0262 0.8382 0.3118 0.062(6) Uiso 1 calc R . . C11 C 1.0131(9) 0.8908(7) 0.4143(8) 0.070(4) Uani 1 d . . . H11A H 1.0822 0.9060 0.4395 0.062(6) Uiso 1 calc R . . H11B H 0.9974 0.8762 0.4628 0.062(6) Uiso 1 calc R . . C12 C 1.0034(9) 0.9976(7) 0.2959(8) 0.063(3) Uani 1 d . . . H12A H 1.0497 1.0353 0.3307 0.062(6) Uiso 1 calc R . . H12B H 1.0422 0.9568 0.2907 0.062(6) Uiso 1 calc R . . C13 C 0.9408(9) 1.0280(7) 0.2032(8) 0.057(3) Uani 1 d . . . H13A H 0.8986 1.0667 0.2074 0.062(6) Uiso 1 calc R . . H13B H 0.9847 1.0491 0.1801 0.062(6) Uiso 1 calc R . . C14 C 0.8780(8) 0.9716(6) 0.1406(7) 0.045(3) Uani 1 d . . . C15 C 0.8216(7) 0.9049(6) 0.0185(7) 0.042(2) Uani 1 d . . . C16 C 0.7902(7) 0.8742(6) 0.0783(6) 0.037(2) Uani 1 d . . . C17 C 0.7380(8) 0.8086(6) 0.0591(6) 0.045(3) Uani 1 d . . . H17 H 0.7193 0.7860 0.0996 0.062(6) Uiso 1 calc R . . C18 C 0.7155(8) 0.7789(6) -0.0233(8) 0.054(3) Uani 1 d . . . H18 H 0.6800 0.7353 -0.0386 0.062(6) Uiso 1 calc R . . C19 C 0.7436(9) 0.8115(7) -0.0846(7) 0.057(3) Uani 1 d . . . H19 H 0.7253 0.7897 -0.1399 0.062(6) Uiso 1 calc R . . C20 C 0.7981(9) 0.8756(7) -0.0647(7) 0.059(3) Uani 1 d . . . H20 H 0.8179 0.8977 -0.1048 0.062(6) Uiso 1 calc R . . C21 C 0.7420(8) 1.0813(6) 0.2327(7) 0.048(3) Uani 1 d . . . H21 H 0.8090 1.0889 0.2695 0.062(6) Uiso 1 calc R . . C22 C 0.6835(10) 1.1410(6) 0.1958(8) 0.058(3) Uani 1 d . . . H22 H 0.7115 1.1876 0.2072 0.062(6) Uiso 1 calc R . . C23 C 0.5858(10) 1.1331(7) 0.1433(8) 0.059(3) Uani 1 d . . . H23 H 0.5463 1.1741 0.1197 0.062(6) Uiso 1 calc R . . C24 C 0.5441(9) 1.0641(6) 0.1242(7) 0.046(3) Uani 1 d . . . C25 C 0.6093(8) 1.0055(5) 0.1647(6) 0.035(2) Uani 1 d . . . C26 C 0.5721(7) 0.9309(5) 0.1483(6) 0.037(2) Uani 1 d . . . C27 C 0.4697(8) 0.9193(7) 0.0965(7) 0.049(3) Uani 1 d . . . C28 C 0.4353(8) 0.8471(7) 0.0823(7) 0.055(3) Uani 1 d . . . H28 H 0.3685 0.8364 0.0483 0.062(6) Uiso 1 calc R . . C29 C 0.5040(9) 0.7928(6) 0.1205(8) 0.058(3) Uani 1 d . . . H29 H 0.4829 0.7443 0.1138 0.062(6) Uiso 1 calc R . . C30 C 0.6036(8) 0.8084(6) 0.1685(7) 0.044(3) Uani 1 d . . . H30 H 0.6480 0.7697 0.1910 0.062(6) Uiso 1 calc R . . C31 C 0.4064(9) 0.9818(7) 0.0585(7) 0.057(3) Uani 1 d . . . H31 H 0.3387 0.9746 0.0239 0.062(6) Uiso 1 calc R . . C32 C 0.4430(10) 1.0495(8) 0.0721(8) 0.067(4) Uani 1 d . . . H32 H 0.4000 1.0885 0.0463 0.062(6) Uiso 1 calc R . . P1 P 1.0021(4) 1.2393(3) 0.3240(3) 0.0873(13) Uani 1 d . . . P2 P 0.6586(2) 0.58958(18) 0.1476(2) 0.0546(8) Uani 1 d . . . F1 F 0.7395(6) 0.5596(6) 0.1206(7) 0.121(4) Uani 1 d . . . F2 F 0.6855(10) 0.5286(6) 0.2176(8) 0.162(5) Uani 1 d . . . F3 F 0.5805(6) 0.5378(6) 0.0774(7) 0.120(4) Uani 1 d . . . F4 F 0.5764(6) 0.6179(4) 0.1755(6) 0.094(3) Uani 1 d . . . F5 F 0.7343(8) 0.6426(7) 0.2154(9) 0.178(6) Uani 1 d . . . F6 F 0.6307(10) 0.6529(6) 0.0809(8) 0.164(5) Uani 1 d . . . F7 F 0.9185(13) 1.2032(7) 0.2541(13) 0.286(12) Uani 1 d . . . F8 F 1.0658(17) 1.1931(14) 0.2989(19) 0.330(15) Uani 1 d . . . F9 F 0.9973(19) 1.1749(8) 0.3791(12) 0.269(10) Uani 1 d . . . F10 F 0.9302(17) 1.2804(11) 0.3451(19) 0.297(13) Uani 1 d . . . F11 F 1.0020(16) 1.3047(8) 0.2751(11) 0.253(10) Uani 1 d . . . F12 F 1.0776(17) 1.2680(9) 0.4035(11) 0.322(15) Uani 1 d . . . O1 O 0.7020(11) 0.7351(7) 0.5832(8) 0.139(5) Uani 1 d . . . C33 C 0.9576(13) 0.4965(12) 0.3087(12) 0.116(6) Uani 1 d . . . H33A H 0.8871 0.4917 0.2892 0.18(5) Uiso 1 calc R . . H33B H 0.9918 0.4714 0.3643 0.18(5) Uiso 1 calc R . . H33C H 0.9760 0.4755 0.2651 0.18(5) Uiso 1 calc R . . C34 C 0.9848(14) 0.5739(13) 0.3202(13) 0.096(6) Uani 1 d . . . N7 N 1.0038(13) 0.6335(11) 0.3287(12) 0.131(7) Uani 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 0.0265(5) 0.0353(4) 0.0329(4) 0.0012(4) 0.0115(3) 0.0005(4) N1 0.026(5) 0.048(5) 0.034(4) -0.004(4) 0.011(3) -0.002(4) N2 0.046(6) 0.062(6) 0.052(5) 0.008(5) 0.029(5) -0.008(5) N3 0.034(5) 0.050(5) 0.032(4) -0.003(4) 0.013(4) 0.006(4) N4 0.093(9) 0.066(7) 0.065(7) 0.026(6) 0.052(6) 0.025(6) N5 0.030(5) 0.043(5) 0.038(4) 0.001(4) 0.015(4) -0.004(4) N6 0.034(5) 0.033(4) 0.035(4) 0.002(3) 0.013(4) 0.004(4) S1 0.0372(17) 0.0447(15) 0.0483(15) 0.0054(12) 0.0167(12) 0.0116(12) S2 0.0350(17) 0.0636(18) 0.0451(15) -0.0088(13) 0.0114(12) -0.0078(14) C1 0.061(8) 0.049(7) 0.049(6) -0.012(5) 0.018(6) -0.009(6) C2 0.084(10) 0.051(8) 0.071(8) -0.016(6) 0.036(8) 0.003(7) C3 0.103(13) 0.103(12) 0.075(10) -0.033(9) 0.055(9) 0.007(10) C4 0.122(14) 0.087(11) 0.070(9) 0.009(8) 0.068(9) 0.023(10) C5 0.059(9) 0.087(10) 0.047(6) -0.004(6) 0.034(6) 0.008(7) C6 0.035(7) 0.055(7) 0.035(5) -0.004(5) 0.015(5) 0.005(5) C7 0.044(7) 0.062(8) 0.047(6) 0.022(6) 0.024(5) 0.014(6) C8 0.075(9) 0.047(7) 0.063(7) 0.015(6) 0.038(7) 0.004(6) C9 0.063(8) 0.047(7) 0.051(6) 0.006(5) 0.023(6) 0.011(6) C10 0.028(7) 0.072(9) 0.083(9) 0.014(7) 0.013(6) 0.014(6) C11 0.042(8) 0.084(10) 0.054(7) 0.003(7) -0.007(6) -0.007(6) C12 0.049(8) 0.071(8) 0.069(8) -0.029(7) 0.025(7) -0.020(6) C13 0.053(8) 0.069(8) 0.066(8) -0.006(6) 0.041(7) -0.020(6) C14 0.036(7) 0.052(7) 0.052(6) 0.008(5) 0.023(5) -0.002(5) C15 0.030(6) 0.054(7) 0.048(6) 0.004(5) 0.021(5) 0.004(5) C16 0.024(6) 0.048(6) 0.041(6) 0.003(5) 0.016(4) 0.010(5) C17 0.051(7) 0.043(6) 0.040(6) 0.000(5) 0.019(5) 0.016(5) C18 0.050(8) 0.048(7) 0.064(8) -0.008(6) 0.024(6) 0.007(6) C19 0.070(9) 0.061(8) 0.043(6) -0.015(6) 0.026(6) 0.003(7) C20 0.068(9) 0.076(9) 0.045(6) 0.000(6) 0.035(6) 0.006(7) C21 0.049(7) 0.042(6) 0.053(6) -0.001(5) 0.023(5) -0.002(5) C22 0.073(9) 0.026(6) 0.079(8) 0.006(5) 0.037(8) 0.008(6) C23 0.063(9) 0.053(8) 0.065(8) 0.016(6) 0.032(7) 0.023(6) C24 0.047(8) 0.045(6) 0.051(6) 0.013(5) 0.025(6) 0.015(5) C25 0.036(7) 0.038(5) 0.043(6) 0.009(4) 0.029(5) 0.004(5) C26 0.025(6) 0.049(6) 0.035(5) 0.008(4) 0.012(4) 0.006(4) C27 0.033(7) 0.066(7) 0.046(6) -0.001(6) 0.016(5) -0.003(6) C28 0.028(7) 0.071(8) 0.057(7) -0.008(6) 0.011(5) -0.013(6) C29 0.058(9) 0.043(7) 0.067(8) -0.007(6) 0.023(7) -0.009(6) C30 0.032(7) 0.040(6) 0.058(7) -0.003(5) 0.018(5) -0.004(5) C31 0.028(7) 0.087(10) 0.054(7) 0.005(7) 0.014(5) 0.015(6) C32 0.059(9) 0.078(9) 0.061(8) 0.009(7) 0.022(7) 0.030(7) P1 0.081(3) 0.094(3) 0.069(2) 0.006(2) 0.015(2) -0.024(3) P2 0.053(2) 0.0541(18) 0.0622(18) -0.0116(16) 0.0300(16) -0.0073(16) F1 0.063(6) 0.152(9) 0.176(9) -0.064(7) 0.077(6) -0.025(6) F2 0.236(14) 0.142(10) 0.140(9) 0.066(8) 0.110(10) 0.092(10) F3 0.059(5) 0.157(9) 0.155(8) -0.104(7) 0.056(6) -0.041(5) F4 0.101(7) 0.085(6) 0.122(7) -0.033(5) 0.071(6) -0.007(5) F5 0.092(8) 0.173(11) 0.236(14) -0.131(11) 0.037(8) -0.035(7) F6 0.237(14) 0.137(10) 0.160(11) 0.064(8) 0.126(11) 0.032(10) F7 0.210(16) 0.110(10) 0.30(2) -0.003(12) -0.114(15) -0.018(11) F8 0.29(3) 0.35(3) 0.48(4) -0.20(3) 0.29(3) -0.08(2) F9 0.48(3) 0.141(12) 0.204(16) 0.071(12) 0.16(2) 0.000(17) F10 0.33(3) 0.222(19) 0.52(4) 0.03(2) 0.36(3) 0.061(19) F11 0.44(3) 0.136(12) 0.196(14) 0.037(11) 0.144(17) -0.092(15) F12 0.36(3) 0.186(16) 0.159(13) -0.007(12) -0.132(15) -0.069(17) O1 0.185(14) 0.137(11) 0.121(10) 0.030(8) 0.092(10) -0.012(10) C33 0.090(14) 0.15(2) 0.116(15) 0.015(14) 0.050(12) 0.009(13) C34 0.066(12) 0.122(17) 0.102(13) -0.010(13) 0.037(10) 0.027(12) N7 0.091(12) 0.137(15) 0.142(15) -0.015(13) 0.027(10) 0.042(12) _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 2.103(7) . ? Ru1 N1 2.110(7) . ? Ru1 N5 2.126(8) . ? Ru1 N3 2.138(8) . ? Ru1 S2 2.307(3) . ? Ru1 S1 2.324(3) . ? N1 C14 1.337(12) . ? N1 C16 1.421(12) . ? N2 C14 1.342(13) . ? N2 C15 1.368(13) . ? N3 C7 1.328(13) . ? N3 C6 1.409(12) . ? N4 C7 1.331(13) . ? N4 C5 1.384(15) . ? N5 C30 1.324(12) . ? N5 C26 1.355(12) . ? N6 C21 1.329(12) . ? N6 C25 1.363(12) . ? S1 C9 1.805(11) . ? S1 C10 1.821(12) . ? S2 C12 1.797(12) . ? S2 C11 1.812(12) . ? C1 C2 1.364(15) . ? C1 C6 1.372(15) . ? C2 C3 1.380(18) . ? C3 C4 1.360(19) . ? C4 C5 1.374(16) . ? C5 C6 1.398(15) . ? C7 C8 1.486(15) . ? C8 C9 1.501(15) . ? C10 C11 1.503(16) . ? C12 C13 1.525(16) . ? C13 C14 1.479(15) . ? C15 C20 1.384(14) . ? C15 C16 1.389(13) . ? C16 C17 1.389(14) . ? C17 C18 1.376(14) . ? C18 C19 1.393(15) . ? C19 C20 1.383(16) . ? C21 C22 1.366(14) . ? C22 C23 1.345(16) . ? C23 C24 1.380(16) . ? C24 C32 1.404(17) . ? C24 C25 1.408(13) . ? C25 C26 1.452(13) . ? C26 C27 1.408(14) . ? C27 C28 1.397(15) . ? C27 C31 1.443(15) . ? C28 C29 1.370(15) . ? C29 C30 1.378(15) . ? C31 C32 1.333(17) . ? P1 F12 1.419(12) . ? P1 F11 1.447(12) . ? P1 F7 1.448(13) . ? P1 F8 1.459(17) . ? P1 F10 1.468(14) . ? P1 F9 1.513(14) . ? P2 F6 1.533(10) . ? P2 F2 1.537(10) . ? P2 F5 1.546(10) . ? P2 F1 1.553(8) . ? P2 F3 1.563(8) . ? P2 F4 1.572(8) . ? C33 C34 1.46(2) . ? C34 N7 1.12(2) . ? 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 N1 88.4(3) . . ? N6 Ru1 N5 78.4(3) . . ? N1 Ru1 N5 94.1(3) . . ? N6 Ru1 N3 94.7(3) . . ? N1 Ru1 N3 176.7(3) . . ? N5 Ru1 N3 87.8(3) . . ? N6 Ru1 S2 95.5(2) . . ? N1 Ru1 S2 90.9(2) . . ? N5 Ru1 S2 171.9(2) . . ? N3 Ru1 S2 87.5(2) . . ? N6 Ru1 S1 172.7(2) . . ? N1 Ru1 S1 85.0(2) . . ? N5 Ru1 S1 99.1(2) . . ? N3 Ru1 S1 92.1(2) . . ? S2 Ru1 S1 87.60(11) . . ? C14 N1 C16 105.0(8) . . ? C14 N1 Ru1 126.2(7) . . ? C16 N1 Ru1 128.3(6) . . ? C14 N2 C15 108.9(9) . . ? C7 N3 C6 105.6(8) . . ? C7 N3 Ru1 124.6(7) . . ? C6 N3 Ru1 129.7(7) . . ? C7 N4 C5 108.1(10) . . ? C30 N5 C26 116.8(9) . . ? C30 N5 Ru1 129.8(7) . . ? C26 N5 Ru1 113.3(6) . . ? C21 N6 C25 115.4(8) . . ? C21 N6 Ru1 129.7(7) . . ? C25 N6 Ru1 114.8(6) . . ? C9 S1 C10 98.2(6) . . ? C9 S1 Ru1 112.6(4) . . ? C10 S1 Ru1 104.3(4) . . ? C12 S2 C11 98.5(6) . . ? C12 S2 Ru1 111.7(4) . . ? C11 S2 Ru1 104.2(4) . . ? C2 C1 C6 119.4(12) . . ? C1 C2 C3 120.3(12) . . ? C4 C3 C2 122.7(12) . . ? C3 C4 C5 115.9(13) . . ? C4 C5 N4 130.9(12) . . ? C4 C5 C6 123.2(13) . . ? N4 C5 C6 105.8(9) . . ? C1 C6 C5 118.3(10) . . ? C1 C6 N3 133.7(10) . . ? C5 C6 N3 108.0(10) . . ? N3 C7 N4 112.4(10) . . ? N3 C7 C8 128.2(10) . . ? N4 C7 C8 119.3(10) . . ? C7 C8 C9 114.0(10) . . ? C8 C9 S1 113.6(8) . . ? C11 C10 S1 111.6(8) . . ? C10 C11 S2 111.8(8) . . ? C13 C12 S2 115.5(8) . . ? C14 C13 C12 112.8(10) . . ? N1 C14 N2 111.5(9) . . ? N1 C14 C13 128.1(9) . . ? N2 C14 C13 120.2(9) . . ? N2 C15 C20 131.0(10) . . ? N2 C15 C16 106.1(9) . . ? C20 C15 C16 123.0(11) . . ? C15 C16 C17 120.8(10) . . ? C15 C16 N1 108.3(9) . . ? C17 C16 N1 130.9(9) . . ? C18 C17 C16 116.2(10) . . ? C17 C18 C19 122.8(11) . . ? C20 C19 C18 121.0(10) . . ? C19 C20 C15 116.0(11) . . ? N6 C21 C22 123.5(11) . . ? C23 C22 C21 120.6(11) . . ? C22 C23 C24 120.1(11) . . ? C23 C24 C32 124.9(11) . . ? C23 C24 C25 115.8(10) . . ? C32 C24 C25 119.2(11) . . ? N6 C25 C24 124.5(9) . . ? N6 C25 C26 115.8(8) . . ? C24 C25 C26 119.7(9) . . ? N5 C26 C27 123.6(9) . . ? N5 C26 C25 117.6(8) . . ? C27 C26 C25 118.8(9) . . ? C28 C27 C26 117.9(10) . . ? C28 C27 C31 123.4(10) . . ? C26 C27 C31 118.7(11) . . ? C29 C28 C27 117.3(10) . . ? C28 C29 C30 121.4(11) . . ? N5 C30 C29 122.9(10) . . ? C32 C31 C27 121.3(11) . . ? C31 C32 C24 122.2(11) . . ? F12 P1 F11 91.7(10) . . ? F12 P1 F7 169.2(15) . . ? F11 P1 F7 97.5(10) . . ? F12 P1 F8 97.4(15) . . ? F11 P1 F8 99.1(14) . . ? F7 P1 F8 86.8(12) . . ? F12 P1 F10 87.4(14) . . ? F11 P1 F10 83.6(11) . . ? F7 P1 F10 87.9(14) . . ? F8 P1 F10 174.4(13) . . ? F12 P1 F9 86.9(11) . . ? F11 P1 F9 174.9(12) . . ? F7 P1 F9 83.4(11) . . ? F8 P1 F9 85.9(13) . . ? F10 P1 F9 91.4(12) . . ? F6 P2 F2 177.1(7) . . ? F6 P2 F5 86.7(8) . . ? F2 P2 F5 91.6(8) . . ? F6 P2 F1 93.4(6) . . ? F2 P2 F1 89.0(6) . . ? F5 P2 F1 91.2(6) . . ? F6 P2 F3 91.8(7) . . ? F2 P2 F3 89.8(7) . . ? F5 P2 F3 178.4(7) . . ? F1 P2 F3 89.4(5) . . ? F6 P2 F4 87.9(6) . . ? F2 P2 F4 89.7(6) . . ? F5 P2 F4 89.6(5) . . ? F1 P2 F4 178.5(6) . . ? F3 P2 F4 89.8(4) . . ? N7 C34 C33 179(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 N6 Ru1 N1 C14 61.4(8) . . . . ? N5 Ru1 N1 C14 139.7(8) . . . . ? N3 Ru1 N1 C14 -95(6) . . . . ? S2 Ru1 N1 C14 -34.0(8) . . . . ? S1 Ru1 N1 C14 -121.5(8) . . . . ? N6 Ru1 N1 C16 -110.0(8) . . . . ? N5 Ru1 N1 C16 -31.7(8) . . . . ? N3 Ru1 N1 C16 94(5) . . . . ? S2 Ru1 N1 C16 154.5(7) . . . . ? S1 Ru1 N1 C16 67.0(7) . . . . ? N6 Ru1 N3 C7 150.9(8) . . . . ? N1 Ru1 N3 C7 -53(6) . . . . ? N5 Ru1 N3 C7 72.7(9) . . . . ? S2 Ru1 N3 C7 -113.8(8) . . . . ? S1 Ru1 N3 C7 -26.3(8) . . . . ? N6 Ru1 N3 C6 -30.9(8) . . . . ? N1 Ru1 N3 C6 125(5) . . . . ? N5 Ru1 N3 C6 -109.2(8) . . . . ? S2 Ru1 N3 C6 64.3(8) . . . . ? S1 Ru1 N3 C6 151.8(8) . . . . ? N6 Ru1 N5 C30 -178.1(9) . . . . ? N1 Ru1 N5 C30 94.4(9) . . . . ? N3 Ru1 N5 C30 -82.9(9) . . . . ? S2 Ru1 N5 C30 -136.7(14) . . . . ? S1 Ru1 N5 C30 8.9(9) . . . . ? N6 Ru1 N5 C26 -1.4(6) . . . . ? N1 Ru1 N5 C26 -88.8(7) . . . . ? N3 Ru1 N5 C26 93.9(7) . . . . ? S2 Ru1 N5 C26 40.1(19) . . . . ? S1 Ru1 N5 C26 -174.4(6) . . . . ? N1 Ru1 N6 C21 -82.8(9) . . . . ? N5 Ru1 N6 C21 -177.4(9) . . . . ? N3 Ru1 N6 C21 95.8(9) . . . . ? S2 Ru1 N6 C21 7.9(9) . . . . ? S1 Ru1 N6 C21 -106.7(18) . . . . ? N1 Ru1 N6 C25 94.3(6) . . . . ? N5 Ru1 N6 C25 -0.3(6) . . . . ? N3 Ru1 N6 C25 -87.1(6) . . . . ? S2 Ru1 N6 C25 -175.0(6) . . . . ? S1 Ru1 N6 C25 70(2) . . . . ? N6 Ru1 S1 C9 -148.8(19) . . . . ? N1 Ru1 S1 C9 -172.8(5) . . . . ? N5 Ru1 S1 C9 -79.3(5) . . . . ? N3 Ru1 S1 C9 8.7(5) . . . . ? S2 Ru1 S1 C9 96.1(4) . . . . ? N6 Ru1 S1 C10 105.8(19) . . . . ? N1 Ru1 S1 C10 81.8(5) . . . . ? N5 Ru1 S1 C10 175.3(5) . . . . ? N3 Ru1 S1 C10 -96.7(5) . . . . ? S2 Ru1 S1 C10 -9.3(5) . . . . ? N6 Ru1 S2 C12 -81.3(5) . . . . ? N1 Ru1 S2 C12 7.1(5) . . . . ? N5 Ru1 S2 C12 -121.9(16) . . . . ? N3 Ru1 S2 C12 -175.7(5) . . . . ? S1 Ru1 S2 C12 92.1(5) . . . . ? N6 Ru1 S2 C11 173.3(5) . . . . ? N1 Ru1 S2 C11 -98.3(5) . . . . ? N5 Ru1 S2 C11 132.7(16) . . . . ? N3 Ru1 S2 C11 78.9(5) . . . . ? S1 Ru1 S2 C11 -13.3(5) . . . . ? C6 C1 C2 C3 2(2) . . . . ? C1 C2 C3 C4 -1(2) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C3 C4 C5 N4 -177.6(14) . . . . ? C3 C4 C5 C6 2(2) . . . . ? C7 N4 C5 C4 179.5(14) . . . . ? C7 N4 C5 C6 -0.2(14) . . . . ? C2 C1 C6 C5 -0.4(17) . . . . ? C2 C1 C6 N3 177.3(11) . . . . ? C4 C5 C6 C1 -1.7(19) . . . . ? N4 C5 C6 C1 178.1(10) . . . . ? C4 C5 C6 N3 -179.9(12) . . . . ? N4 C5 C6 N3 -0.1(13) . . . . ? C7 N3 C6 C1 -177.4(12) . . . . ? Ru1 N3 C6 C1 4.1(17) . . . . ? C7 N3 C6 C5 0.4(11) . . . . ? Ru1 N3 C6 C5 -178.0(7) . . . . ? C6 N3 C7 N4 -0.6(12) . . . . ? Ru1 N3 C7 N4 177.9(7) . . . . ? C6 N3 C7 C8 -178.5(12) . . . . ? Ru1 N3 C7 C8 0.0(16) . . . . ? C5 N4 C7 N3 0.5(14) . . . . ? C5 N4 C7 C8 178.6(11) . . . . ? N3 C7 C8 C9 55.8(16) . . . . ? N4 C7 C8 C9 -121.9(12) . . . . ? C7 C8 C9 S1 -68.0(12) . . . . ? C10 S1 C9 C8 140.7(9) . . . . ? Ru1 S1 C9 C8 31.4(10) . . . . ? C9 S1 C10 C11 -79.4(10) . . . . ? Ru1 S1 C10 C11 36.6(10) . . . . ? S1 C10 C11 S2 -51.8(12) . . . . ? C12 S2 C11 C10 -75.0(10) . . . . ? Ru1 S2 C11 C10 40.1(10) . . . . ? C11 S2 C12 C13 145.1(9) . . . . ? Ru1 S2 C12 C13 36.0(10) . . . . ? S2 C12 C13 C14 -66.8(12) . . . . ? C16 N1 C14 N2 4.0(11) . . . . ? Ru1 N1 C14 N2 -169.0(7) . . . . ? C16 N1 C14 C13 -171.9(11) . . . . ? Ru1 N1 C14 C13 15.0(16) . . . . ? C15 N2 C14 N1 -3.5(12) . . . . ? C15 N2 C14 C13 172.8(10) . . . . ? C12 C13 C14 N1 42.6(16) . . . . ? C12 C13 C14 N2 -133.0(11) . . . . ? C14 N2 C15 C20 -179.6(11) . . . . ? C14 N2 C15 C16 1.4(12) . . . . ? N2 C15 C16 C17 -176.7(9) . . . . ? C20 C15 C16 C17 4.2(16) . . . . ? N2 C15 C16 N1 1.0(11) . . . . ? C20 C15 C16 N1 -178.1(10) . . . . ? C14 N1 C16 C15 -3.0(10) . . . . ? Ru1 N1 C16 C15 169.8(6) . . . . ? C14 N1 C16 C17 174.4(10) . . . . ? Ru1 N1 C16 C17 -12.8(15) . . . . ? C15 C16 C17 C18 -3.2(14) . . . . ? N1 C16 C17 C18 179.6(10) . . . . ? C16 C17 C18 C19 0.6(16) . . . . ? C17 C18 C19 C20 1.3(18) . . . . ? C18 C19 C20 C15 -0.5(18) . . . . ? N2 C15 C20 C19 179.0(11) . . . . ? C16 C15 C20 C19 -2.1(17) . . . . ? C25 N6 C21 C22 -0.5(15) . . . . ? Ru1 N6 C21 C22 176.6(8) . . . . ? N6 C21 C22 C23 1.1(18) . . . . ? C21 C22 C23 C24 -1.6(18) . . . . ? C22 C23 C24 C32 178.4(11) . . . . ? C22 C23 C24 C25 1.6(17) . . . . ? C21 N6 C25 C24 0.5(14) . . . . ? Ru1 N6 C25 C24 -177.1(8) . . . . ? C21 N6 C25 C26 179.4(8) . . . . ? Ru1 N6 C25 C26 1.8(10) . . . . ? C23 C24 C25 N6 -1.0(15) . . . . ? C32 C24 C25 N6 -178.0(10) . . . . ? C23 C24 C25 C26 -179.9(9) . . . . ? C32 C24 C25 C26 3.1(15) . . . . ? C30 N5 C26 C27 -0.3(14) . . . . ? Ru1 N5 C26 C27 -177.5(8) . . . . ? C30 N5 C26 C25 180.0(9) . . . . ? Ru1 N5 C26 C25 2.8(11) . . . . ? N6 C25 C26 N5 -3.1(13) . . . . ? C24 C25 C26 N5 175.8(9) . . . . ? N6 C25 C26 C27 177.1(8) . . . . ? C24 C25 C26 C27 -3.9(14) . . . . ? N5 C26 C27 C28 0.9(15) . . . . ? C25 C26 C27 C28 -179.4(9) . . . . ? N5 C26 C27 C31 -177.2(9) . . . . ? C25 C26 C27 C31 2.5(14) . . . . ? C26 C27 C28 C29 0.3(16) . . . . ? C31 C27 C28 C29 178.3(11) . . . . ? C27 C28 C29 C30 -2.1(18) . . . . ? C26 N5 C30 C29 -1.6(15) . . . . ? Ru1 N5 C30 C29 175.1(8) . . . . ? C28 C29 C30 N5 2.9(18) . . . . ? C28 C27 C31 C32 -178.4(12) . . . . ? C26 C27 C31 C32 -0.4(17) . . . . ? C27 C31 C32 C24 -0.5(19) . . . . ? C23 C24 C32 C31 -177.7(12) . . . . ? C25 C24 C32 C31 -1.0(18) . . . . ? _diffrn_measured_fraction_theta_max 0.863 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.863 _refine_diff_density_max 0.909 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.122 # Attachment 'MP_Dalton_complex_2a.cif' data_137mpvrm _database_code_depnum_ccdc_archive 'CCDC 653790' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H28 Cl F6 N6 P Ru S2' _chemical_formula_weight 818.19 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P21/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 14.9570(13) _cell_length_b 9.0588(8) _cell_length_c 23.1298(19) _cell_angle_alpha 90.00 _cell_angle_beta 100.962(2) _cell_angle_gamma 90.00 _cell_volume 3076.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATES _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8475 _exptl_absorpt_correction_T_max 0.9666 _exptl_absorpt_process_details BRUKER-SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'BRUKER SMART APEX CCD DIFFRACTIOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18125 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0925 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 28.33 _reflns_number_total 7198 _reflns_number_gt 5762 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7198 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.1681 _refine_ls_wR_factor_gt 0.1587 _refine_ls_goodness_of_fit_ref 1.223 _refine_ls_restrained_S_all 1.223 _refine_ls_shift/su_max 0.000 _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 Ru1 Ru 0.14872(3) 0.43884(5) 0.134058(19) 0.00832(13) Uani 1 d . . . S1 S 0.05162(9) 0.35661(16) 0.05047(6) 0.0112(3) Uani 1 d . . . S2 S 0.17710(9) 0.19217(16) 0.15969(6) 0.0127(3) Uani 1 d . . . Cl1 Cl 0.11578(9) 0.69366(15) 0.10486(6) 0.0121(3) Uani 1 d . . . N1 N 0.2609(3) 0.4484(5) 0.0935(2) 0.0124(10) Uani 1 d . . . N2 N 0.2468(3) 0.5351(5) 0.20131(19) 0.0108(10) Uani 1 d . . . N3 N 0.5835(3) 0.5622(6) 0.1310(2) 0.0225(12) Uani 1 d . . . N4 N 0.5615(3) 0.7059(6) 0.2366(2) 0.0248(13) Uani 1 d . . . N5 N 0.0426(3) 0.4255(5) 0.1836(2) 0.0139(10) Uani 1 d . . . N6 N 0.4592(3) -0.0315(6) 0.1391(2) 0.0199(12) Uani 1 d . . . C1 C 0.2659(4) 0.4086(6) 0.0384(3) 0.0162(13) Uani 1 d . . . H1 H 0.2126 0.3831 0.0126 0.019 Uiso 1 calc R . . C2 C 0.3477(4) 0.4040(7) 0.0183(3) 0.0200(14) Uani 1 d . . . H2 H 0.3488 0.3727 -0.0198 0.024 Uiso 1 calc R . . C3 C 0.4264(4) 0.4456(7) 0.0548(3) 0.0227(15) Uani 1 d . . . H3 H 0.4818 0.4401 0.0421 0.027 Uiso 1 calc R . . C4 C 0.4229(4) 0.4965(6) 0.1112(3) 0.0140(12) Uani 1 d . . . C5 C 0.3388(4) 0.4961(6) 0.1288(2) 0.0121(12) Uani 1 d . . . C6 C 0.3314(4) 0.5503(6) 0.1858(3) 0.0149(12) Uani 1 d . . . C7 C 0.2360(4) 0.5988(6) 0.2509(2) 0.0142(12) Uani 1 d . . . H7 H 0.1789 0.5936 0.2612 0.017 Uiso 1 calc R . . C8 C 0.3058(4) 0.6740(7) 0.2892(2) 0.0161(13) Uani 1 d . . . H8 H 0.2944 0.7164 0.3237 0.019 Uiso 1 calc R . . C9 C 0.3902(4) 0.6839(7) 0.2751(3) 0.0199(14) Uani 1 d . . . H9 H 0.4375 0.7312 0.3002 0.024 Uiso 1 calc R . . C10 C 0.4043(4) 0.6218(7) 0.2221(2) 0.0156(12) Uani 1 d . . . C11 C 0.4910(4) 0.6281(7) 0.2023(3) 0.0193(13) Uani 1 d . . . C12 C 0.5009(4) 0.5609(7) 0.1499(3) 0.0190(13) Uani 1 d . . . C13 C 0.6484(4) 0.6376(8) 0.1648(3) 0.0284(16) Uani 1 d . . . H13 H 0.7051 0.6423 0.1540 0.034 Uiso 1 calc R . . C14 C 0.6371(4) 0.7106(8) 0.2157(3) 0.0320(18) Uani 1 d . . . H14 H 0.6856 0.7656 0.2360 0.038 Uiso 1 calc R . . C15 C 0.0656(4) 0.3722(6) 0.2397(2) 0.0111(11) Uani 1 d . . . H15 H 0.1263 0.3478 0.2538 0.013 Uiso 1 calc R . . C16 C 0.0050(4) 0.3526(6) 0.2762(2) 0.0133(12) Uani 1 d . . . H16 H 0.0243 0.3151 0.3140 0.016 Uiso 1 calc R . . C17 C -0.0855(4) 0.3889(7) 0.2565(3) 0.0186(13) Uani 1 d . . . H17 H -0.1283 0.3777 0.2806 0.022 Uiso 1 calc R . . C18 C -0.1100(4) 0.4422(7) 0.2001(3) 0.0186(13) Uani 1 d . . . H18 H -0.1704 0.4682 0.1860 0.022 Uiso 1 calc R . . C19 C -0.0472(4) 0.4580(6) 0.1639(2) 0.0123(12) Uani 1 d . . . C20 C -0.0779(4) 0.5009(7) 0.1002(2) 0.0136(12) Uani 1 d . . . H20A H -0.0426 0.5847 0.0912 0.016 Uiso 1 calc R . . H20B H -0.1414 0.5301 0.0935 0.016 Uiso 1 calc R . . C23 C 0.0830(4) 0.0963(6) 0.1128(3) 0.0135(12) Uani 1 d . . . H23A H 0.0978 -0.0078 0.1115 0.016 Uiso 1 calc R . . H23B H 0.0289 0.1050 0.1300 0.016 Uiso 1 calc R . . C22 C 0.0625(4) 0.1565(7) 0.0506(3) 0.0180(13) Uani 1 d . . . H22A H 0.0063 0.1134 0.0295 0.022 Uiso 1 calc R . . H22B H 0.1110 0.1288 0.0302 0.022 Uiso 1 calc R . . C21 C -0.0663(4) 0.3731(7) 0.0595(2) 0.0145(12) Uani 1 d . . . H21A H -0.1051 0.3888 0.0214 0.017 Uiso 1 calc R . . H21B H -0.0851 0.2820 0.0757 0.017 Uiso 1 calc R . . C24 C 0.2735(4) 0.1232(6) 0.1302(3) 0.0136(12) Uani 1 d . . . H24A H 0.2585 0.1275 0.0876 0.016 Uiso 1 calc R . . H24B H 0.3252 0.1878 0.1430 0.016 Uiso 1 calc R . . C25 C 0.3013(4) -0.0350(6) 0.1488(3) 0.0151(12) Uani 1 d . . . H25A H 0.3236 -0.0394 0.1910 0.018 Uiso 1 calc R . . H25B H 0.2493 -0.1005 0.1391 0.018 Uiso 1 calc R . . C26 C 0.3749(4) -0.0811(7) 0.1164(3) 0.0151(12) Uani 1 d . . . C27 C 0.3534(4) -0.1556(7) 0.0633(3) 0.0206(14) Uani 1 d . . . H27 H 0.2944 -0.1887 0.0495 0.025 Uiso 1 calc R . . C28 C 0.4213(4) -0.1803(7) 0.0309(3) 0.0227(14) Uani 1 d . . . H28 H 0.4087 -0.2295 -0.0051 0.027 Uiso 1 calc R . . C29 C 0.5079(4) -0.1298(7) 0.0535(3) 0.0232(14) Uani 1 d . . . H29 H 0.5552 -0.1447 0.0332 0.028 Uiso 1 calc R . . C30 C 0.5230(4) -0.0569(7) 0.1067(3) 0.0269(15) Uani 1 d . . . H30 H 0.5817 -0.0228 0.1213 0.032 Uiso 1 calc R . . P1 P 0.19720(10) 0.47342(18) 0.41518(7) 0.0165(3) Uani 1 d . . . F4 F 0.1663(2) 0.5601(4) 0.46826(15) 0.0240(8) Uani 1 d . . . F6 F 0.1344(2) 0.5774(4) 0.36798(15) 0.0238(8) Uani 1 d . . . F2 F 0.2790(2) 0.5847(6) 0.41707(17) 0.0453(13) Uani 1 d . . . F1 F 0.2277(3) 0.3862(5) 0.36194(17) 0.0461(12) Uani 1 d . . . F5 F 0.1141(3) 0.3637(5) 0.41354(16) 0.0457(13) Uani 1 d . . . F3 F 0.2597(3) 0.3692(6) 0.46179(17) 0.0526(14) Uani 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 0.0069(2) 0.0085(2) 0.0099(2) 0.00021(18) 0.00244(16) -0.00055(18) S1 0.0114(6) 0.0116(7) 0.0109(6) 0.0003(5) 0.0028(5) -0.0009(6) S2 0.0108(6) 0.0113(7) 0.0168(7) 0.0008(6) 0.0047(5) 0.0006(6) Cl1 0.0123(6) 0.0093(7) 0.0142(6) 0.0012(5) 0.0017(5) -0.0009(5) N1 0.012(2) 0.008(2) 0.018(2) 0.002(2) 0.0034(19) 0.0000(19) N2 0.010(2) 0.011(3) 0.011(2) 0.0014(19) 0.0018(18) -0.0014(19) N3 0.015(3) 0.014(3) 0.039(3) 0.007(3) 0.008(2) -0.004(2) N4 0.021(3) 0.025(3) 0.026(3) 0.012(2) -0.001(2) -0.009(2) N5 0.016(2) 0.011(2) 0.015(2) -0.003(2) 0.0044(19) 0.002(2) N6 0.013(2) 0.015(3) 0.032(3) -0.001(2) 0.004(2) 0.000(2) C1 0.016(3) 0.013(3) 0.021(3) 0.000(2) 0.006(2) -0.002(2) C2 0.025(3) 0.018(3) 0.022(3) 0.000(3) 0.016(3) 0.001(3) C3 0.019(3) 0.014(3) 0.042(4) 0.000(3) 0.023(3) 0.000(3) C4 0.013(3) 0.006(3) 0.026(3) 0.004(2) 0.013(2) -0.001(2) C5 0.009(3) 0.007(3) 0.021(3) 0.003(2) 0.004(2) 0.002(2) C6 0.018(3) 0.007(3) 0.020(3) 0.005(2) 0.004(2) 0.002(2) C7 0.019(3) 0.012(3) 0.013(3) 0.004(2) 0.006(2) 0.002(2) C8 0.020(3) 0.019(3) 0.008(3) -0.002(2) -0.001(2) -0.002(3) C9 0.014(3) 0.021(3) 0.021(3) 0.003(3) -0.004(2) -0.008(3) C10 0.016(3) 0.015(3) 0.015(3) 0.006(2) 0.001(2) -0.001(2) C11 0.014(3) 0.019(3) 0.024(3) 0.013(3) 0.000(2) -0.001(3) C12 0.009(3) 0.013(3) 0.035(4) 0.003(3) 0.006(3) 0.001(2) C13 0.010(3) 0.027(4) 0.049(5) 0.013(3) 0.006(3) -0.002(3) C14 0.013(3) 0.035(4) 0.045(4) 0.023(4) -0.001(3) -0.014(3) C15 0.012(3) 0.014(3) 0.008(3) -0.002(2) 0.003(2) 0.000(2) C16 0.020(3) 0.009(3) 0.012(3) -0.004(2) 0.005(2) -0.005(2) C17 0.021(3) 0.018(3) 0.021(3) -0.003(3) 0.012(3) -0.006(3) C18 0.011(3) 0.027(4) 0.020(3) -0.007(3) 0.007(2) -0.006(3) C19 0.011(3) 0.011(3) 0.015(3) -0.003(2) 0.004(2) -0.001(2) C20 0.006(2) 0.017(3) 0.018(3) 0.003(2) 0.003(2) 0.001(2) C23 0.012(3) 0.007(3) 0.023(3) -0.004(2) 0.005(2) 0.000(2) C22 0.016(3) 0.018(3) 0.020(3) -0.010(3) 0.004(2) -0.004(3) C21 0.012(3) 0.016(3) 0.015(3) 0.004(2) 0.000(2) -0.005(2) C24 0.009(3) 0.012(3) 0.022(3) 0.000(2) 0.008(2) -0.002(2) C25 0.013(3) 0.007(3) 0.026(3) 0.000(2) 0.006(2) -0.001(2) C26 0.013(3) 0.015(3) 0.018(3) 0.004(2) 0.006(2) 0.008(2) C27 0.017(3) 0.018(3) 0.027(3) -0.004(3) 0.005(3) 0.002(3) C28 0.029(3) 0.021(4) 0.019(3) 0.002(3) 0.005(3) 0.006(3) C29 0.021(3) 0.020(4) 0.032(4) 0.008(3) 0.013(3) 0.004(3) C30 0.014(3) 0.024(4) 0.043(4) 0.005(3) 0.007(3) -0.003(3) P1 0.0188(8) 0.0158(8) 0.0157(8) 0.0031(6) 0.0052(6) 0.0052(6) F4 0.0285(19) 0.028(2) 0.0170(18) -0.0037(16) 0.0072(15) 0.0039(17) F6 0.0199(18) 0.031(2) 0.0193(18) 0.0037(16) 0.0009(14) 0.0080(17) F2 0.022(2) 0.088(4) 0.024(2) 0.011(2) -0.0013(17) -0.030(2) F1 0.069(3) 0.045(3) 0.029(2) 0.002(2) 0.020(2) 0.038(2) F5 0.069(3) 0.045(3) 0.022(2) -0.001(2) 0.006(2) -0.041(2) F3 0.067(3) 0.064(3) 0.027(2) 0.019(2) 0.009(2) 0.048(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 N1 2.074(4) . ? Ru1 N2 2.113(4) . ? Ru1 N5 2.131(5) . ? Ru1 S1 2.3095(14) . ? Ru1 S2 2.3301(15) . ? Ru1 Cl1 2.4292(14) . ? S1 C22 1.820(6) . ? S1 C21 1.821(5) . ? S2 C24 1.819(5) . ? S2 C23 1.825(6) . ? N1 C1 1.340(7) . ? N1 C5 1.360(7) . ? N2 C7 1.322(7) . ? N2 C6 1.386(7) . ? N3 C13 1.316(8) . ? N3 C12 1.386(7) . ? N4 C14 1.313(8) . ? N4 C11 1.386(8) . ? N5 C15 1.364(7) . ? N5 C19 1.365(7) . ? N6 C30 1.341(8) . ? N6 C26 1.346(7) . ? C1 C2 1.389(7) . ? C1 H1 0.9300 . ? C2 C3 1.364(9) . ? C2 H2 0.9300 . ? C3 C4 1.395(8) . ? C3 H3 0.9300 . ? C4 C5 1.394(7) . ? C4 C12 1.451(8) . ? C5 C6 1.429(8) . ? C6 C10 1.402(8) . ? C7 C8 1.409(8) . ? C7 H7 0.9300 . ? C8 C9 1.367(8) . ? C8 H8 0.9300 . ? C9 C10 1.399(8) . ? C9 H9 0.9300 . ? C10 C11 1.458(8) . ? C11 C12 1.390(9) . ? C13 C14 1.388(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.364(7) . ? C15 H15 0.9300 . ? C16 C17 1.384(8) . ? C16 H16 0.9300 . ? C17 C18 1.374(8) . ? C17 H17 0.9300 . ? C18 C19 1.381(7) . ? C18 H18 0.9300 . ? C19 C20 1.508(8) . ? C20 C21 1.522(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C23 C22 1.515(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C24 C25 1.531(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.505(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.386(8) . ? C27 C28 1.391(8) . ? C27 H27 0.9300 . ? C28 C29 1.380(8) . ? C28 H28 0.9300 . ? C29 C30 1.378(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? P1 F2 1.580(4) . ? P1 F5 1.586(4) . ? P1 F3 1.595(4) . ? P1 F4 1.598(4) . ? P1 F1 1.601(4) . ? P1 F6 1.603(4) . ? 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 N1 Ru1 N2 78.89(17) . . ? N1 Ru1 N5 174.37(18) . . ? N2 Ru1 N5 96.39(17) . . ? N1 Ru1 S1 93.97(13) . . ? N2 Ru1 S1 170.91(12) . . ? N5 Ru1 S1 91.02(13) . . ? N1 Ru1 S2 91.79(13) . . ? N2 Ru1 S2 98.11(13) . . ? N5 Ru1 S2 85.82(13) . . ? S1 Ru1 S2 87.64(5) . . ? N1 Ru1 Cl1 88.47(13) . . ? N2 Ru1 Cl1 83.58(13) . . ? N5 Ru1 Cl1 94.07(13) . . ? S1 Ru1 Cl1 90.67(5) . . ? S2 Ru1 Cl1 178.31(5) . . ? C22 S1 C21 99.8(3) . . ? C22 S1 Ru1 106.17(19) . . ? C21 S1 Ru1 110.24(19) . . ? C24 S2 C23 101.0(3) . . ? C24 S2 Ru1 110.67(19) . . ? C23 S2 Ru1 102.86(19) . . ? C1 N1 C5 117.4(5) . . ? C1 N1 Ru1 128.0(4) . . ? C5 N1 Ru1 114.6(4) . . ? C7 N2 C6 116.7(5) . . ? C7 N2 Ru1 129.6(4) . . ? C6 N2 Ru1 113.0(3) . . ? C13 N3 C12 114.7(6) . . ? C14 N4 C11 114.8(6) . . ? C15 N5 C19 116.7(5) . . ? C15 N5 Ru1 116.8(4) . . ? C19 N5 Ru1 126.4(4) . . ? C30 N6 C26 116.1(5) . . ? N1 C1 C2 122.6(5) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.7(6) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.2(5) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 118.0(5) . . ? C5 C4 C12 119.0(5) . . ? C3 C4 C12 122.7(5) . . ? N1 C5 C4 122.8(5) . . ? N1 C5 C6 117.1(5) . . ? C4 C5 C6 120.1(5) . . ? N2 C6 C10 122.3(5) . . ? N2 C6 C5 116.0(5) . . ? C10 C6 C5 121.6(5) . . ? N2 C7 C8 124.0(5) . . ? N2 C7 H7 118.0 . . ? C8 C7 H7 118.0 . . ? C9 C8 C7 119.3(5) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 118.8(5) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C9 C10 C6 118.8(5) . . ? C9 C10 C11 123.4(5) . . ? C6 C10 C11 117.8(5) . . ? N4 C11 C12 121.8(5) . . ? N4 C11 C10 117.8(6) . . ? C12 C11 C10 120.4(5) . . ? N3 C12 C11 121.3(5) . . ? N3 C12 C4 118.0(5) . . ? C11 C12 C4 120.5(5) . . ? N3 C13 C14 123.8(6) . . ? N3 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? N4 C14 C13 123.3(6) . . ? N4 C14 H14 118.3 . . ? C13 C14 H14 118.3 . . ? C16 C15 N5 123.9(5) . . ? C16 C15 H15 118.1 . . ? N5 C15 H15 118.1 . . ? C15 C16 C17 119.3(5) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 117.6(5) . . ? C18 C17 H17 121.2 . . ? C16 C17 H17 121.2 . . ? C17 C18 C19 121.6(5) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? N5 C19 C18 120.9(5) . . ? N5 C19 C20 118.7(5) . . ? C18 C19 C20 120.2(5) . . ? C19 C20 C21 111.0(5) . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C22 C23 S2 112.8(4) . . ? C22 C23 H23A 109.0 . . ? S2 C23 H23A 109.0 . . ? C22 C23 H23B 109.0 . . ? S2 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C23 C22 S1 111.2(4) . . ? C23 C22 H22A 109.4 . . ? S1 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? S1 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C20 C21 S1 111.1(4) . . ? C20 C21 H21A 109.4 . . ? S1 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? S1 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C25 C24 S2 114.1(4) . . ? C25 C24 H24A 108.7 . . ? S2 C24 H24A 108.7 . . ? C25 C24 H24B 108.7 . . ? S2 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C26 C25 C24 107.7(5) . . ? C26 C25 H25A 110.2 . . ? C24 C25 H25A 110.2 . . ? C26 C25 H25B 110.2 . . ? C24 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? N6 C26 C27 123.4(5) . . ? N6 C26 C25 115.7(5) . . ? C27 C26 C25 120.5(5) . . ? C26 C27 C28 119.1(6) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? C29 C28 C27 118.1(6) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? C30 C29 C28 118.7(6) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? N6 C30 C29 124.6(6) . . ? N6 C30 H30 117.7 . . ? C29 C30 H30 117.7 . . ? F2 P1 F5 179.1(3) . . ? F2 P1 F3 90.5(3) . . ? F5 P1 F3 90.1(3) . . ? F2 P1 F4 90.0(2) . . ? F5 P1 F4 89.2(2) . . ? F3 P1 F4 89.4(2) . . ? F2 P1 F1 90.2(3) . . ? F5 P1 F1 90.5(3) . . ? F3 P1 F1 90.7(2) . . ? F4 P1 F1 179.8(2) . . ? F2 P1 F6 89.7(2) . . ? F5 P1 F6 89.8(2) . . ? F3 P1 F6 179.6(2) . . ? F4 P1 F6 90.97(19) . . ? F1 P1 F6 89.0(2) . . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.884 _refine_diff_density_max 0.936 _refine_diff_density_min -1.275 _refine_diff_density_rms 0.248 # Attachment 'MP_Dalton_complex_5.cif' data_mrpvru2f _database_code_depnum_ccdc_archive 'CCDC 653791' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 Cl2 N8 O8 Ru S2' _chemical_formula_weight 914.75 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' 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' S S 0.1246 0.1234 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 29.804(7) _cell_length_b 14.946(4) _cell_length_c 15.875(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7072(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8855 _exptl_absorpt_correction_T_max 0.9547 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26753 _diffrn_reflns_av_R_equivalents 0.2012 _diffrn_reflns_av_sigmaI/netI 0.1357 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4636 _reflns_number_gt 2581 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+11.4823P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4636 _refine_ls_number_parameters 507 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1449 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.1660 _refine_ls_wR_factor_gt 0.1365 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _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 0.11009(3) 0.13058(5) 0.48401(5) 0.0335(3) Uani 1 1 d . . . S2 S 0.03380(9) 0.10614(18) 0.47889(19) 0.0476(8) Uani 1 1 d . . . S1 S 0.10689(11) 0.16391(19) 0.34187(17) 0.0533(8) Uani 1 1 d . . . N1 N 0.1793(3) 0.1311(6) 0.5060(5) 0.040(2) Uani 1 1 d . . . N4 N 0.1132(3) 0.1244(5) 0.6157(4) 0.0331(19) Uani 1 1 d . . . N5 N 0.1173(3) -0.0103(5) 0.4568(5) 0.038(2) Uani 1 1 d . . . N6 N 0.1312(3) -0.1368(6) 0.3903(6) 0.064(3) Uani 1 1 d . . . H6C H 0.1378 -0.1730 0.3501 0.077 Uiso 1 1 calc R . . N7 N 0.1024(3) 0.2725(5) 0.4958(5) 0.037(2) Uani 1 1 d . . . N8 N 0.0685(3) 0.4031(6) 0.5079(5) 0.054(3) Uani 1 1 d . . . H8C H 0.0482 0.4422 0.5190 0.064 Uiso 1 1 calc R . . C1 C 0.1913(3) 0.1282(6) 0.5897(6) 0.034(2) Uani 1 1 d . . . C2 C 0.2134(4) 0.1230(7) 0.4513(7) 0.048(3) Uani 1 1 d . . . H2 H 0.2068 0.1211 0.3941 0.058 Uiso 1 1 calc R . . C3 C 0.2583(4) 0.1172(8) 0.4756(8) 0.061(3) Uani 1 1 d . . . H3 H 0.2807 0.1135 0.4350 0.073 Uiso 1 1 calc R . . C4 C 0.2693(4) 0.1171(8) 0.5583(9) 0.062(4) Uani 1 1 d . . . H4 H 0.2992 0.1132 0.5748 0.074 Uiso 1 1 calc R . . C5 C 0.2359(4) 0.1229(7) 0.6179(7) 0.045(3) Uani 1 1 d . . . C6 C 0.2440(4) 0.1213(8) 0.7080(8) 0.055(3) Uani 1 1 d . . . C9 C 0.2081(4) 0.1300(8) 0.7656(7) 0.055(3) Uani 1 1 d . . . C10 C 0.1631(4) 0.1336(7) 0.7354(7) 0.045(3) Uani 1 1 d . . . C11 C 0.1270(4) 0.1333(8) 0.7913(7) 0.058(3) Uani 1 1 d . . . H11 H 0.1313 0.1352 0.8493 0.070 Uiso 1 1 calc R . . C12 C 0.0846(4) 0.1300(7) 0.7563(7) 0.051(3) Uani 1 1 d . . . H12 H 0.0596 0.1315 0.7913 0.061 Uiso 1 1 calc R . . C13 C 0.0789(4) 0.1244(7) 0.6707(7) 0.046(3) Uani 1 1 d . . . H13 H 0.0498 0.1205 0.6497 0.055 Uiso 1 1 calc R . . C14 C 0.1547(3) 0.1293(7) 0.6491(6) 0.037(3) Uani 1 1 d . . . C15 C 0.1150(3) -0.0811(6) 0.5152(7) 0.039(3) Uani 1 1 d . . . C16 C 0.1048(4) -0.0848(8) 0.5998(7) 0.051(3) Uani 1 1 d . . . H16 H 0.0984 -0.0334 0.6304 0.061 Uiso 1 1 calc R . . C17 C 0.1047(4) -0.1688(9) 0.6374(8) 0.064(4) Uani 1 1 d . . . H17 H 0.0971 -0.1732 0.6940 0.077 Uiso 1 1 calc R . . C18 C 0.1153(4) -0.2462(8) 0.5940(11) 0.070(4) Uani 1 1 d . . . H18 H 0.1162 -0.3007 0.6221 0.085 Uiso 1 1 calc R . . C19 C 0.1245(4) -0.2424(8) 0.5106(10) 0.071(4) Uani 1 1 d . . . H19 H 0.1311 -0.2941 0.4805 0.085 Uiso 1 1 calc R . . C20 C 0.1236(4) -0.1610(8) 0.4716(8) 0.051(3) Uani 1 1 d . . . C21 C 0.1269(4) -0.0490(8) 0.3824(7) 0.053(3) Uani 1 1 d . . . C22 C 0.1260(7) -0.0073(10) 0.2967(9) 0.135(8) Uani 1 1 d . . . H22A H 0.1482 -0.0396 0.2640 0.162 Uiso 1 1 calc R . . H22B H 0.0971 -0.0231 0.2730 0.162 Uiso 1 1 calc R . . C23 C 0.1322(5) 0.0803(11) 0.2773(8) 0.099(5) Uani 1 1 d . . . H23A H 0.1214 0.0893 0.2202 0.118 Uiso 1 1 calc R . . H23B H 0.1642 0.0915 0.2768 0.118 Uiso 1 1 calc R . . C24 C 0.0484(4) 0.1529(9) 0.3151(7) 0.073(4) Uani 1 1 d . . . H24A H 0.0342 0.2111 0.3203 0.088 Uiso 1 1 calc R . . H24B H 0.0461 0.1348 0.2566 0.088 Uiso 1 1 calc R . . C25 C 0.0228(4) 0.0870(9) 0.3684(7) 0.070(4) Uani 1 1 d . . . H25A H 0.0317 0.0266 0.3535 0.084 Uiso 1 1 calc R . . H25B H -0.0091 0.0930 0.3575 0.084 Uiso 1 1 calc R . . C26 C 0.0008(3) 0.2068(7) 0.4959(7) 0.054(3) Uani 1 1 d . . . H26A H -0.0051 0.2346 0.4418 0.065 Uiso 1 1 calc R . . H26B H -0.0278 0.1900 0.5202 0.065 Uiso 1 1 calc R . . C27 C 0.0227(3) 0.2744(7) 0.5523(7) 0.049(3) Uani 1 1 d . . . H27A H 0.0014 0.3222 0.5631 0.059 Uiso 1 1 calc R . . H27B H 0.0293 0.2460 0.6059 0.059 Uiso 1 1 calc R . . C28 C 0.0649(3) 0.3146(7) 0.5189(6) 0.034(3) Uani 1 1 d . . . C29 C 0.1110(4) 0.4205(7) 0.4750(6) 0.045(3) Uani 1 1 d . . . C30 C 0.1297(5) 0.5019(7) 0.4543(8) 0.063(4) Uani 1 1 d . . . H30 H 0.1143 0.5555 0.4613 0.076 Uiso 1 1 calc R . . C31 C 0.1725(5) 0.4986(9) 0.4225(8) 0.070(4) Uani 1 1 d . . . H31 H 0.1868 0.5513 0.4065 0.085 Uiso 1 1 calc R . . C32 C 0.1946(4) 0.4184(9) 0.4141(7) 0.063(4) Uani 1 1 d . . . H32 H 0.2237 0.4186 0.3933 0.075 Uiso 1 1 calc R . . C33 C 0.1753(4) 0.3380(8) 0.4352(7) 0.056(3) Uani 1 1 d . . . H33 H 0.1908 0.2846 0.4280 0.067 Uiso 1 1 calc R . . C34 C 0.1324(4) 0.3389(7) 0.4673(6) 0.037(3) Uani 1 1 d . . . Cl1 Cl 0.03201(16) 0.5740(2) 0.6418(2) 0.0805(12) Uani 1 1 d . . . O3 O 0.0331(3) 0.5750(6) 0.5520(6) 0.094(3) Uani 1 1 d . . . O2 O 0.0039(4) 0.5062(7) 0.6690(9) 0.151(5) Uani 1 1 d . . . O4 O 0.0196(4) 0.6605(6) 0.6693(6) 0.126(4) Uani 1 1 d . . . O1 O 0.0783(4) 0.5554(7) 0.6695(8) 0.132(4) Uani 1 1 d . . . Cl2 Cl 0.0537(2) 0.7500 0.2500 0.102(2) Uani 1 2 d S . . O6 O 0.0304(5) 0.6809(10) 0.2070(9) 0.209(8) Uani 1 1 d . . . O5 O 0.0800(5) 0.7939(9) 0.1923(9) 0.201(7) Uani 1 1 d . . . Cl3 Cl 0.2250(2) 0.7500 0.2500 0.126(3) Uani 1 2 d S . . O7 O 0.2670(7) 0.7500 0.2500 0.196(10) Uani 1 2 d S . . O9 O 0.2148(8) 0.7733(16) 0.1583(15) 0.106(7) Uani 0.50 1 d P . . O8 O 0.2295(8) 0.6489(16) 0.2286(13) 0.128(9) Uani 0.50 1 d P . . O10 O 0.1906(10) 0.7500 0.2500 0.43(5) Uani 1 2 d S . . N3 N 0.2157(4) 0.1347(8) 0.8500(6) 0.078(3) Uani 1 1 d . . . N2 N 0.2874(4) 0.1112(8) 0.7337(8) 0.092(4) Uani 1 1 d . . . C8 C 0.2583(7) 0.1264(12) 0.8727(11) 0.111(6) Uani 1 1 d . . . H8 H 0.2654 0.1295 0.9297 0.134 Uiso 1 1 calc R . . C7 C 0.2930(6) 0.1134(11) 0.8147(12) 0.106(6) Uani 1 1 d . . . H7 H 0.3220 0.1058 0.8356 0.127 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0353(5) 0.0295(5) 0.0356(5) 0.0009(4) 0.0010(4) 0.0009(5) S2 0.0363(17) 0.043(2) 0.0635(19) -0.0013(14) -0.0057(15) -0.0064(14) S1 0.069(2) 0.0490(19) 0.0419(17) 0.0045(13) -0.0057(17) 0.0028(18) N1 0.032(5) 0.044(6) 0.045(6) 0.004(5) 0.009(4) 0.012(5) N4 0.034(5) 0.029(5) 0.036(5) -0.004(4) 0.004(5) 0.004(5) N5 0.043(6) 0.020(5) 0.052(6) -0.005(4) 0.001(5) -0.008(4) N6 0.081(8) 0.030(7) 0.081(8) -0.025(6) 0.010(6) 0.005(6) N7 0.045(6) 0.017(5) 0.050(6) -0.003(4) -0.009(5) 0.004(5) N8 0.056(7) 0.029(6) 0.077(7) -0.010(5) 0.014(6) 0.005(5) C1 0.039(7) 0.030(6) 0.033(6) -0.001(5) 0.001(5) -0.001(6) C2 0.033(7) 0.058(8) 0.054(7) 0.000(6) 0.009(6) 0.008(7) C3 0.049(8) 0.069(9) 0.064(9) 0.007(7) 0.028(7) 0.017(7) C4 0.020(7) 0.078(10) 0.087(10) 0.028(8) -0.004(7) 0.004(7) C5 0.035(7) 0.039(7) 0.062(8) 0.001(6) -0.010(6) -0.005(6) C6 0.034(7) 0.067(9) 0.064(9) 0.010(7) -0.026(7) -0.019(7) C9 0.065(9) 0.051(8) 0.049(8) 0.008(7) -0.020(7) -0.007(8) C10 0.053(8) 0.045(7) 0.038(7) 0.009(6) -0.005(6) -0.001(7) C11 0.083(10) 0.070(9) 0.022(6) 0.006(6) 0.003(7) 0.017(8) C12 0.059(9) 0.047(8) 0.047(8) 0.010(6) 0.020(6) 0.009(7) C13 0.050(8) 0.042(7) 0.045(7) 0.010(6) 0.002(6) 0.000(7) C14 0.036(7) 0.029(6) 0.047(7) -0.001(6) -0.002(6) -0.001(6) C15 0.036(7) 0.026(6) 0.056(7) -0.003(6) 0.005(6) -0.003(6) C16 0.043(7) 0.046(8) 0.063(9) 0.016(6) 0.010(6) 0.005(7) C17 0.067(9) 0.054(9) 0.072(9) 0.020(7) 0.011(8) -0.003(8) C18 0.061(10) 0.037(9) 0.113(12) 0.019(8) -0.011(9) 0.008(8) C19 0.069(11) 0.031(8) 0.113(13) -0.009(8) -0.012(9) 0.007(7) C20 0.032(7) 0.048(9) 0.073(9) -0.006(7) -0.002(6) 0.001(6) C21 0.070(10) 0.035(8) 0.052(8) -0.016(6) 0.020(6) 0.007(6) C22 0.27(3) 0.058(11) 0.074(11) -0.018(8) 0.092(13) -0.023(13) C23 0.135(14) 0.111(14) 0.050(9) -0.001(8) 0.027(9) 0.023(12) C24 0.074(10) 0.099(12) 0.047(8) -0.004(7) -0.023(7) 0.034(9) C25 0.039(8) 0.110(12) 0.061(9) -0.027(8) -0.024(7) -0.006(8) C26 0.034(7) 0.063(8) 0.065(8) -0.011(6) 0.004(6) 0.011(6) C27 0.031(7) 0.058(8) 0.058(8) 0.002(6) 0.010(6) 0.000(6) C28 0.030(7) 0.032(7) 0.041(6) 0.000(5) -0.010(5) 0.008(6) C29 0.056(8) 0.029(7) 0.050(7) -0.007(5) -0.004(7) -0.005(7) C30 0.082(11) 0.021(7) 0.087(10) -0.008(6) 0.015(8) -0.013(7) C31 0.082(12) 0.037(9) 0.092(11) 0.004(7) -0.007(9) -0.024(9) C32 0.067(9) 0.051(9) 0.070(9) 0.018(7) -0.001(7) -0.007(9) C33 0.054(9) 0.042(8) 0.071(9) 0.002(6) -0.007(7) 0.010(7) C34 0.046(8) 0.018(6) 0.046(7) 0.003(4) -0.002(6) -0.003(6) Cl1 0.116(4) 0.048(3) 0.077(3) 0.0036(18) 0.018(2) 0.018(3) O3 0.129(9) 0.095(8) 0.059(6) -0.015(5) -0.015(6) 0.046(6) O2 0.152(12) 0.071(8) 0.230(14) 0.038(8) 0.076(10) 0.003(8) O4 0.196(12) 0.063(7) 0.119(9) -0.007(6) 0.076(8) 0.031(7) O1 0.130(10) 0.096(9) 0.168(11) 0.025(7) -0.053(9) 0.014(8) Cl2 0.058(4) 0.160(7) 0.090(5) 0.006(4) 0.000 0.000 O6 0.177(13) 0.246(17) 0.204(15) 0.112(12) -0.118(11) -0.143(12) O5 0.204(14) 0.177(15) 0.222(15) -0.083(10) 0.169(12) -0.090(11) Cl3 0.042(4) 0.217(10) 0.118(7) -0.080(6) 0.000 0.000 O7 0.096(16) 0.29(3) 0.20(2) 0.09(2) 0.000 0.000 O9 0.10(2) 0.112(19) 0.105(19) -0.026(13) -0.033(14) 0.002(16) O8 0.16(2) 0.13(2) 0.103(17) -0.063(15) -0.003(15) 0.055(17) O10 0.07(2) 0.34(5) 0.87(13) -0.37(7) 0.000 0.000 N3 0.068(8) 0.111(10) 0.056(7) 0.013(7) -0.023(6) -0.017(8) N2 0.055(8) 0.125(12) 0.097(10) 0.016(8) -0.032(7) -0.008(7) C8 0.106(15) 0.141(16) 0.088(13) 0.013(12) -0.042(12) -0.024(14) C7 0.073(12) 0.134(16) 0.111(15) 0.007(13) -0.056(12) -0.031(12) _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 N1 2.092(8) . ? Ru1 N4 2.095(7) . ? Ru1 N7 2.141(7) . ? Ru1 N5 2.160(8) . ? Ru1 S2 2.304(3) . ? Ru1 S1 2.313(3) . ? S2 C25 1.808(11) . ? S2 C26 1.817(10) . ? S1 C23 1.782(13) . ? S1 C24 1.802(12) . ? N1 C2 1.342(11) . ? N1 C1 1.377(11) . ? N4 C13 1.345(12) . ? N4 C14 1.348(11) . ? N5 C21 1.346(12) . ? N5 C15 1.408(12) . ? N6 C21 1.325(13) . ? N6 C20 1.359(14) . ? N6 H6C 0.8600 . ? N7 C28 1.333(11) . ? N7 C34 1.412(12) . ? N8 C28 1.337(12) . ? N8 C29 1.396(13) . ? N8 H8C 0.8600 . ? C1 C5 1.404(13) . ? C1 C14 1.442(13) . ? C2 C3 1.396(14) . ? C2 H2 0.9300 . ? C3 C4 1.353(15) . ? C3 H3 0.9300 . ? C4 C5 1.376(14) . ? C4 H4 0.9300 . ? C5 C6 1.451(14) . ? C6 N2 1.365(13) . ? C6 C9 1.415(15) . ? C9 N3 1.360(13) . ? C9 C10 1.425(14) . ? C10 C11 1.394(14) . ? C10 C14 1.396(13) . ? C11 C12 1.382(14) . ? C11 H11 0.9300 . ? C12 C13 1.372(13) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.378(13) . ? C15 C20 1.404(14) . ? C16 C17 1.390(14) . ? C16 H16 0.9300 . ? C17 C18 1.383(16) . ? C17 H17 0.9300 . ? C18 C19 1.353(16) . ? C18 H18 0.9300 . ? C19 C20 1.365(16) . ? C19 H19 0.9300 . ? C21 C22 1.497(17) . ? C22 C23 1.358(17) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.506(15) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.499(13) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.492(13) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C29 C30 1.378(14) . ? C29 C34 1.381(13) . ? C30 C31 1.374(16) . ? C30 H30 0.9300 . ? C31 C32 1.372(15) . ? C31 H31 0.9300 . ? C32 C33 1.373(14) . ? C32 H32 0.9300 . ? C33 C34 1.376(14) . ? C33 H33 0.9300 . ? Cl1 O2 1.384(11) . ? Cl1 O4 1.413(9) . ? Cl1 O3 1.426(9) . ? Cl1 O1 1.474(11) . ? Cl2 O5 1.372(11) . ? Cl2 O5 1.372(11) 3_565 ? Cl2 O6 1.421(12) 3_565 ? Cl2 O6 1.421(12) . ? Cl3 O10 1.02(3) . ? Cl3 O7 1.252(18) . ? Cl3 O9 1.53(3) . ? Cl3 O9 1.53(3) 3_565 ? Cl3 O8 1.55(2) 3_565 ? Cl3 O8 1.55(2) . ? O9 O10 1.66(2) . ? O10 O9 1.66(2) 3_565 ? N3 C8 1.327(17) . ? N2 C7 1.298(17) . ? C8 C7 1.40(2) . ? C8 H8 0.9300 . ? C7 H7 0.9300 . ? 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 N1 Ru1 N4 77.9(3) . . ? N1 Ru1 N7 95.1(3) . . ? N4 Ru1 N7 87.8(3) . . ? N1 Ru1 N5 86.5(3) . . ? N4 Ru1 N5 98.8(3) . . ? N7 Ru1 N5 173.5(3) . . ? N1 Ru1 S2 168.3(2) . . ? N4 Ru1 S2 94.1(2) . . ? N7 Ru1 S2 93.1(2) . . ? N5 Ru1 S2 86.4(2) . . ? N1 Ru1 S1 101.7(2) . . ? N4 Ru1 S1 170.1(2) . . ? N7 Ru1 S1 82.4(2) . . ? N5 Ru1 S1 91.1(2) . . ? S2 Ru1 S1 87.66(12) . . ? C25 S2 C26 100.2(5) . . ? C25 S2 Ru1 103.8(4) . . ? C26 S2 Ru1 113.4(4) . . ? C23 S1 C24 102.1(7) . . ? C23 S1 Ru1 113.1(5) . . ? C24 S1 Ru1 104.5(4) . . ? C2 N1 C1 115.1(9) . . ? C2 N1 Ru1 129.7(7) . . ? C1 N1 Ru1 114.6(6) . . ? C13 N4 C14 116.3(9) . . ? C13 N4 Ru1 127.9(7) . . ? C14 N4 Ru1 115.5(7) . . ? C21 N5 C15 105.3(9) . . ? C21 N5 Ru1 128.0(7) . . ? C15 N5 Ru1 126.6(7) . . ? C21 N6 C20 109.7(9) . . ? C21 N6 H6C 125.1 . . ? C20 N6 H6C 125.1 . . ? C28 N7 C34 106.7(8) . . ? C28 N7 Ru1 125.6(7) . . ? C34 N7 Ru1 126.9(7) . . ? C28 N8 C29 107.8(9) . . ? C28 N8 H8C 126.1 . . ? C29 N8 H8C 126.1 . . ? N1 C1 C5 123.8(9) . . ? N1 C1 C14 115.7(9) . . ? C5 C1 C14 120.5(10) . . ? N1 C2 C3 123.6(10) . . ? N1 C2 H2 118.2 . . ? C3 C2 H2 118.2 . . ? C4 C3 C2 120.0(10) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.5(11) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C1 117.9(10) . . ? C4 C5 C6 123.7(11) . . ? C1 C5 C6 118.3(10) . . ? N2 C6 C9 122.3(11) . . ? N2 C6 C5 117.1(12) . . ? C9 C6 C5 120.6(10) . . ? N3 C9 C6 121.0(11) . . ? N3 C9 C10 119.1(12) . . ? C6 C9 C10 119.9(10) . . ? C11 C10 C14 119.1(11) . . ? C11 C10 C9 120.8(11) . . ? C14 C10 C9 119.8(11) . . ? C12 C11 C10 116.8(10) . . ? C12 C11 H11 121.6 . . ? C10 C11 H11 121.6 . . ? C13 C12 C11 120.9(10) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? N4 C13 C12 123.3(10) . . ? N4 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? N4 C14 C10 123.6(9) . . ? N4 C14 C1 115.9(9) . . ? C10 C14 C1 120.5(10) . . ? C16 C15 C20 119.1(10) . . ? C16 C15 N5 133.0(9) . . ? C20 C15 N5 107.8(10) . . ? C15 C16 C17 117.1(11) . . ? C15 C16 H16 121.4 . . ? C17 C16 H16 121.4 . . ? C18 C17 C16 122.7(12) . . ? C18 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C19 C18 C17 119.9(12) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 118.5(12) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? N6 C20 C19 131.6(12) . . ? N6 C20 C15 105.8(10) . . ? C19 C20 C15 122.6(13) . . ? N6 C21 N5 111.3(10) . . ? N6 C21 C22 120.0(10) . . ? N5 C21 C22 127.9(11) . . ? C23 C22 C21 127.3(13) . . ? C23 C22 H22A 105.5 . . ? C21 C22 H22A 105.5 . . ? C23 C22 H22B 105.5 . . ? C21 C22 H22B 105.5 . . ? H22A C22 H22B 106.1 . . ? C22 C23 S1 119.2(11) . . ? C22 C23 H23A 107.5 . . ? S1 C23 H23A 107.5 . . ? C22 C23 H23B 107.5 . . ? S1 C23 H23B 107.5 . . ? H23A C23 H23B 107.0 . . ? C25 C24 S1 114.6(8) . . ? C25 C24 H24A 108.6 . . ? S1 C24 H24A 108.6 . . ? C25 C24 H24B 108.6 . . ? S1 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? C24 C25 S2 110.5(8) . . ? C24 C25 H25A 109.6 . . ? S2 C25 H25A 109.6 . . ? C24 C25 H25B 109.6 . . ? S2 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C27 C26 S2 114.3(7) . . ? C27 C26 H26A 108.7 . . ? S2 C26 H26A 108.7 . . ? C27 C26 H26B 108.7 . . ? S2 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C28 C27 C26 115.2(9) . . ? C28 C27 H27A 108.5 . . ? C26 C27 H27A 108.5 . . ? C28 C27 H27B 108.5 . . ? C26 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? N7 C28 N8 111.4(9) . . ? N7 C28 C27 127.8(9) . . ? N8 C28 C27 120.8(10) . . ? C30 C29 C34 124.9(12) . . ? C30 C29 N8 128.4(11) . . ? C34 C29 N8 106.7(9) . . ? C31 C30 C29 115.5(12) . . ? C31 C30 H30 122.2 . . ? C29 C30 H30 122.2 . . ? C32 C31 C30 120.8(12) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C33 122.7(13) . . ? C31 C32 H32 118.6 . . ? C33 C32 H32 118.6 . . ? C32 C33 C34 118.0(11) . . ? C32 C33 H33 121.0 . . ? C34 C33 H33 121.0 . . ? C33 C34 C29 118.0(10) . . ? C33 C34 N7 134.5(10) . . ? C29 C34 N7 107.4(9) . . ? O2 Cl1 O4 114.6(7) . . ? O2 Cl1 O3 109.5(8) . . ? O4 Cl1 O3 107.8(6) . . ? O2 Cl1 O1 109.5(7) . . ? O4 Cl1 O1 109.0(8) . . ? O3 Cl1 O1 106.2(7) . . ? O5 Cl2 O5 110.5(15) . 3_565 ? O5 Cl2 O6 104.6(8) . 3_565 ? O5 Cl2 O6 107.9(8) 3_565 3_565 ? O5 Cl2 O6 107.9(8) . . ? O5 Cl2 O6 104.6(8) 3_565 . ? O6 Cl2 O6 121.3(15) 3_565 . ? O10 Cl3 O7 180.000(1) . . ? O10 Cl3 O9 78.6(10) . . ? O7 Cl3 O9 101.4(10) . . ? O10 Cl3 O9 78.6(10) . 3_565 ? O7 Cl3 O9 101.4(10) . 3_565 ? O9 Cl3 O9 157(2) . 3_565 ? O10 Cl3 O8 94.9(10) . 3_565 ? O7 Cl3 O8 85.1(10) . 3_565 ? O9 Cl3 O8 90.2(12) . 3_565 ? O9 Cl3 O8 91.7(12) 3_565 3_565 ? O10 Cl3 O8 94.9(10) . . ? O7 Cl3 O8 85.1(10) . . ? O9 Cl3 O8 91.7(12) . . ? O9 Cl3 O8 90.2(12) 3_565 . ? O8 Cl3 O8 170.2(19) 3_565 . ? O9 O10 O9 129(3) . 3_565 ? C8 N3 C9 115.0(13) . . ? C7 N2 C6 114.5(13) . . ? N3 C8 C7 122.8(15) . . ? N3 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? N2 C7 C8 124.1(15) . . ? N2 C7 H7 117.9 . . ? C8 C7 H7 117.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.692 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.102