# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef 'alb09pub.cif' # 1. SUBMISSION DETAILS _publ_contact_author ; Prof. Dr. Martin Albrecht School of Chemistry and Chemical Biology University College Dublin Belfield Dublin 4 Ireland ; _publ_contact_author_phone '00353 1 716-2504' _publ_contact_author_fax '00353 1 716-2501' _publ_contact_author_email martin.albrecht@ucd.ie _publ_requested_coeditor_name ? # 2. TITLE AND AUTHOR LIST _publ_section_title ; ; loop_ _publ_author_name _publ_author_address 'Lucile Bernet' ; School of Chemistry and Chemical Biology University College Dublin Belfield Dublin 4 Ireland ; 'Ralte Lalrempuia' ; School of Chemistry and Chemical Biology University College Dublin Belfield Dublin 4 Ireland ; 'Wadih Ghattas' ; School of Chemistry and Chemical Biology University College Dublin Belfield Dublin 4 Ireland ; H.Muller-Bunz ; School of Chemistry and Chemical Biology University College Dublin Belfield Dublin 4 Ireland ; 'Laura Vigara' ; Insitute of Chemical Research in Catalonia Av. Paisos Catalans 16 43007 Tarragona Spain ; ; A.Llobet ; ; Insitute of Chemical Research in Catalonia Av. Paisos Catalans 16 43007 Tarragona Spain ; 'Martin Albrecht' ; School of Chemistry and Chemical Biology University College Dublin Belfield Dublin 4 Ireland ; _publ_contact_author_name 'Prof. Dr. Martin Albrecht' #===END_data_global #TrackingRef 'alb09pub.cif' data_alb09(3d') _database_code_depnum_ccdc_archive 'CCDC 817668' #TrackingRef 'alb09pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H24 N8 Ru, 2 (C24 H20 B), 0.75 (C2 H3 N), 0.25 (C4 H10 O)' _chemical_formula_sum 'C72.50 H68.75 B2 N8.75 O0.25 Ru' _chemical_formula_weight 1189.30 _chemical_absolute_configuration ad 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' B B 0.0013 0.0007 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 35.555(3) _cell_length_b 11.8292(9) _cell_length_c 14.7547(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6205.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7873 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 21.96 _exptl_crystal_description block _exptl_crystal_colour green _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 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2484 _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9144 _exptl_absorpt_correction_T_max 0.9703 _exptl_absorpt_process_details ? _exptl_special_details ; The PLATON "squeeze" procedure was used to treat regions of diffuse solvent(s) which could not be modelled in terms of atomic sites. The number of electrons thus located, 104 per unit cell, is included in the formula, formula weight, calculated density, \m and F(000). This residual electron density was assigned to 3 molecules of acetonitrile and one molecule of diethylether per unit cell. Three acetonitriles and one diethylether would give 108 e^-^. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93844 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.83 _reflns_number_total 10681 _reflns_number_gt 10270 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0425P)^2^+3.5134P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(2) _refine_ls_number_reflns 10681 _refine_ls_number_parameters 735 _refine_ls_number_restraints 221 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.003 _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 Ru Ru 0.864982(6) 0.578000(18) 0.92069(2) 0.02047(7) Uani 1 1 d U . . N1 N 0.86012(9) 0.7133(3) 0.8307(2) 0.0356(7) Uani 1 1 d U . . C1 C 0.83498(14) 0.7180(4) 0.7640(3) 0.0518(12) Uani 1 1 d U . . H1 H 0.8165 0.6627 0.7599 0.062 Uiso 1 1 calc R . . C2 C 0.83608(18) 0.8062(5) 0.6990(3) 0.0747(17) Uani 1 1 d U . . H2 H 0.8185 0.8080 0.6522 0.090 Uiso 1 1 calc R . . C3 C 0.8627(2) 0.8882(5) 0.7048(4) 0.085(2) Uani 1 1 d U . . H3 H 0.8638 0.9456 0.6618 0.102 Uiso 1 1 calc R . . C4 C 0.88763(18) 0.8851(3) 0.7742(3) 0.0688(16) Uani 1 1 d U . . H4 H 0.9058 0.9412 0.7794 0.083 Uiso 1 1 calc R . . C5 C 0.88608(13) 0.7982(3) 0.8376(3) 0.0467(10) Uani 1 1 d U . . C6 C 0.90938(11) 0.7805(2) 0.9157(4) 0.0400(8) Uani 1 1 d U . . C7 C 0.90439(9) 0.6829(3) 0.9683(2) 0.0258(7) Uani 1 1 d U . . N2 N 0.93569(12) 0.8444(3) 0.9579(3) 0.0551(11) Uani 1 1 d U . . C9 C 0.95215(19) 0.9537(3) 0.9315(5) 0.099(2) Uani 1 1 d U . . H9A H 0.9695 0.9782 0.9774 0.148 Uiso 1 1 calc R . . H9B H 0.9325 1.0088 0.9249 0.148 Uiso 1 1 calc R . . H9C H 0.9652 0.9455 0.8750 0.148 Uiso 1 1 calc R . . N8 N 0.94828(10) 0.7978(3) 1.0326(3) 0.0516(10) Uani 1 1 d U . . N3 N 0.92878(8) 0.7006(2) 1.0370(2) 0.0314(7) Uani 1 1 d U . . C10 C 0.93486(9) 0.6319(3) 1.1153(3) 0.0327(8) Uani 1 1 d U . . C11 C 0.92936(12) 0.6764(4) 1.2002(3) 0.0472(11) Uani 1 1 d U . . H11 H 0.9223 0.7516 1.2068 0.057 Uiso 1 1 calc R . . C12 C 0.93432(14) 0.6095(4) 1.2753(3) 0.0561(12) Uani 1 1 d U . . H12 H 0.9309 0.6394 1.3330 0.067 Uiso 1 1 calc R . . C13 C 0.94449(12) 0.4963(4) 1.2645(3) 0.0493(11) Uani 1 1 d U . . H13 H 0.9474 0.4499 1.3148 0.059 Uiso 1 1 calc R . . C14 C 0.95025(10) 0.4538(3) 1.1782(3) 0.0370(9) Uani 1 1 d U . . H14 H 0.9574 0.3787 1.1712 0.044 Uiso 1 1 calc R . . C15 C 0.94570(9) 0.5194(3) 1.1039(3) 0.0330(8) Uani 1 1 d U . . H15 H 0.9497 0.4901 1.0463 0.040 Uiso 1 1 calc R . . N4 N 0.87141(7) 0.4452(2) 1.00554(18) 0.0188(6) Uani 1 1 d U . . C16 C 0.87333(8) 0.3669(3) 1.0503(2) 0.0236(7) Uani 1 1 d U . . C17 C 0.87681(10) 0.2670(3) 1.1067(3) 0.0350(9) Uani 1 1 d U . . H17A H 0.8872 0.2062 1.0717 0.052 Uiso 1 1 calc R . . H17B H 0.8524 0.2456 1.1289 0.052 Uiso 1 1 calc R . . H17C H 0.8931 0.2831 1.1570 0.052 Uiso 1 1 calc R . . N5 N 0.82158(8) 0.4852(2) 0.85986(18) 0.0257(6) Uani 1 1 d U . . C18 C 0.79771(10) 0.4337(3) 0.8294(2) 0.0263(7) Uani 1 1 d U . . C19 C 0.76735(10) 0.3681(3) 0.7891(2) 0.0276(7) Uani 1 1 d U . . H19A H 0.7534 0.4150 0.7480 0.041 Uiso 1 1 calc R . . H19B H 0.7509 0.3412 0.8361 0.041 Uiso 1 1 calc R . . H19C H 0.7777 0.3050 0.7568 0.041 Uiso 1 1 calc R . . N6 N 0.90324(8) 0.5126(2) 0.83467(18) 0.0232(6) Uani 1 1 d U . . C20 C 0.92715(10) 0.4829(3) 0.7892(2) 0.0274(8) Uani 1 1 d U . . C21 C 0.95860(12) 0.4478(3) 0.7317(3) 0.0463(11) Uani 1 1 d U . . H21A H 0.9662 0.5099 0.6939 0.069 Uiso 1 1 calc R . . H21B H 0.9509 0.3856 0.6942 0.069 Uiso 1 1 calc R . . H21C H 0.9793 0.4249 0.7691 0.069 Uiso 1 1 calc R . . N7 N 0.82892(7) 0.6480(2) 1.00979(18) 0.0219(6) Uani 1 1 d U . . C22 C 0.81157(9) 0.6893(3) 1.0647(2) 0.0234(7) Uani 1 1 d U . . C23 C 0.78934(10) 0.7431(3) 1.1356(2) 0.0279(8) Uani 1 1 d U . . H23A H 0.8036 0.8032 1.1625 0.042 Uiso 1 1 calc R . . H23B H 0.7831 0.6882 1.1812 0.042 Uiso 1 1 calc R . . H23C H 0.7666 0.7731 1.1099 0.042 Uiso 1 1 calc R . . B1 B 0.77517(11) 0.0676(3) 0.9734(3) 0.0235(8) Uani 1 1 d U . . C24 C 0.80469(9) 0.0448(3) 1.0557(2) 0.0218(7) Uani 1 1 d U . . C25 C 0.79726(11) 0.0724(3) 1.1464(3) 0.0232(8) Uani 1 1 d U . . H25 H 0.7751 0.1108 1.1596 0.028 Uiso 1 1 calc R . . C26 C 0.82122(10) 0.0456(3) 1.2171(2) 0.0285(8) Uani 1 1 d U . . H26 H 0.8150 0.0665 1.2760 0.034 Uiso 1 1 calc R . . C27 C 0.85457(10) -0.0125(3) 1.2005(2) 0.0293(8) Uani 1 1 d U . . H27 H 0.8708 -0.0308 1.2476 0.035 Uiso 1 1 calc R . . C28 C 0.86283(10) -0.0423(3) 1.1125(3) 0.0293(8) Uani 1 1 d U . . H28 H 0.8849 -0.0813 1.0999 0.035 Uiso 1 1 calc R . . C29 C 0.83846(9) -0.0146(3) 1.0427(2) 0.0242(7) Uani 1 1 d U . . H29 H 0.8448 -0.0365 0.9841 0.029 Uiso 1 1 calc R . . C30 C 0.74879(9) -0.0468(3) 0.9745(2) 0.0224(7) Uani 1 1 d U . . C31 C 0.71793(9) -0.0575(3) 1.0334(2) 0.0256(7) Uani 1 1 d U . . H31 H 0.7110 0.0048 1.0680 0.031 Uiso 1 1 calc R . . C32 C 0.69763(9) -0.1549(3) 1.0425(2) 0.0276(7) Uani 1 1 d U . . H32 H 0.6775 -0.1576 1.0827 0.033 Uiso 1 1 calc R . . C33 C 0.70689(10) -0.2500(3) 0.9917(3) 0.0314(8) Uani 1 1 d U . . H33 H 0.6932 -0.3166 0.9976 0.038 Uiso 1 1 calc R . . C34 C 0.73692(9) -0.2432(3) 0.9324(3) 0.0319(8) Uani 1 1 d U . . H34 H 0.7433 -0.3056 0.8972 0.038 Uiso 1 1 calc R . . C35 C 0.75769(8) -0.1439(2) 0.9249(3) 0.0262(6) Uani 1 1 d U . . H35 H 0.7781 -0.1421 0.8856 0.031 Uiso 1 1 calc R . . C36 C 0.79606(9) 0.0892(3) 0.8760(2) 0.0212(7) Uani 1 1 d U . . C37 C 0.78001(10) 0.0590(3) 0.7930(2) 0.0247(7) Uani 1 1 d U . . H37 H 0.7575 0.0187 0.7929 0.030 Uiso 1 1 calc R . . C38 C 0.79631(12) 0.0867(3) 0.7112(3) 0.0279(9) Uani 1 1 d U . . H38 H 0.7847 0.0647 0.6575 0.033 Uiso 1 1 calc R . . C39 C 0.82952(9) 0.1465(3) 0.7079(2) 0.0251(7) Uani 1 1 d U . . H39 H 0.8407 0.1634 0.6526 0.030 Uiso 1 1 calc R . . C40 C 0.84583(9) 0.1807(3) 0.7882(2) 0.0267(7) Uani 1 1 d U . . H40 H 0.8677 0.2236 0.7873 0.032 Uiso 1 1 calc R . . C41 C 0.82957(9) 0.1511(3) 0.8702(2) 0.0223(7) Uani 1 1 d U . . H41 H 0.8414 0.1733 0.9236 0.027 Uiso 1 1 calc R . . C42 C 0.75002(9) 0.1829(3) 0.9879(2) 0.0216(7) Uani 1 1 d U . . C43 C 0.71370(9) 0.1945(3) 0.9527(2) 0.0268(8) Uani 1 1 d U . . H43 H 0.7022 0.1317 0.9267 0.032 Uiso 1 1 calc R . . C44 C 0.69416(9) 0.2965(3) 0.9551(2) 0.0310(8) Uani 1 1 d U . . H44 H 0.6699 0.3005 0.9319 0.037 Uiso 1 1 calc R . . C45 C 0.71050(10) 0.3911(3) 0.9914(3) 0.0312(8) Uani 1 1 d U . . H45 H 0.6974 0.4591 0.9930 0.037 Uiso 1 1 calc R . . C46 C 0.74629(10) 0.3847(3) 1.0254(2) 0.0282(8) Uani 1 1 d U . . H46 H 0.7577 0.4487 1.0496 0.034 Uiso 1 1 calc R . . C47 C 0.76572(9) 0.2817(3) 1.0235(2) 0.0246(7) Uani 1 1 d U . . H47 H 0.7900 0.2789 1.0469 0.030 Uiso 1 1 calc R . . B2 B 0.96771(10) 0.7961(3) 0.5412(3) 0.0219(7) Uani 1 1 d U . . C48 C 0.94498(9) 0.6743(3) 0.5346(2) 0.0231(7) Uani 1 1 d U . . C49 C 0.90804(10) 0.6604(3) 0.5652(3) 0.0328(8) Uani 1 1 d U . . H49 H 0.8953 0.7232 0.5877 0.039 Uiso 1 1 calc R . . C50 C 0.88947(11) 0.5571(3) 0.5636(3) 0.0410(10) Uani 1 1 d U . . H50 H 0.8649 0.5518 0.5846 0.049 Uiso 1 1 calc R . . C51 C 0.90761(12) 0.4622(3) 0.5306(3) 0.0440(10) Uani 1 1 d U . . H51 H 0.8952 0.3931 0.5284 0.053 Uiso 1 1 calc R . . C52 C 0.94432(11) 0.4712(3) 0.5011(3) 0.0361(9) Uani 1 1 d U . . H52 H 0.9571 0.4077 0.4803 0.043 Uiso 1 1 calc R . . C53 C 0.96210(10) 0.5758(3) 0.5025(2) 0.0278(7) Uani 1 1 d U . . H53 H 0.9866 0.5804 0.4810 0.033 Uiso 1 1 calc R . . C54 C 0.98940(9) 0.8010(3) 0.6405(2) 0.0215(7) Uani 1 1 d U . . C55 C 0.97557(9) 0.7453(3) 0.7172(2) 0.0251(7) Uani 1 1 d U . . H55 H 0.9533 0.7046 0.7119 0.030 Uiso 1 1 calc R . . C56 C 0.99338(11) 0.7478(3) 0.8006(3) 0.0355(8) Uani 1 1 d U . . H56 H 0.9830 0.7086 0.8491 0.043 Uiso 1 1 calc R . . C57 C 1.02628(11) 0.8078(3) 0.8125(2) 0.0351(8) Uani 1 1 d U . . H57 H 1.0386 0.8088 0.8681 0.042 Uiso 1 1 calc R . . C58 C 1.04045(10) 0.8670(3) 0.7380(2) 0.0322(8) Uani 1 1 d U . . H58 H 1.0622 0.9100 0.7444 0.039 Uiso 1 1 calc R . . C59 C 1.02259(9) 0.8625(3) 0.6552(2) 0.0234(7) Uani 1 1 d U . . H59 H 1.0330 0.9020 0.6069 0.028 Uiso 1 1 calc R . . C60 C 0.93958(9) 0.9057(3) 0.5319(2) 0.0222(7) Uani 1 1 d U . . C61 C 0.90855(9) 0.9076(3) 0.4742(2) 0.0273(7) Uani 1 1 d U . . H61 H 0.9018 0.8410 0.4449 0.033 Uiso 1 1 calc R . . C62 C 0.88730(9) 1.0034(3) 0.4581(2) 0.0292(7) Uani 1 1 d U . . H62 H 0.8667 0.9998 0.4195 0.035 Uiso 1 1 calc R . . C63 C 0.89665(9) 1.1052(3) 0.4996(2) 0.0289(8) Uani 1 1 d U . . H63 H 0.8827 1.1702 0.4886 0.035 Uiso 1 1 calc R . . C64 C 0.92705(10) 1.1077(3) 0.5573(2) 0.0290(8) Uani 1 1 d U . . H64 H 0.9337 1.1748 0.5859 0.035 Uiso 1 1 calc R . . C65 C 0.94796(9) 1.0091(3) 0.5730(2) 0.0236(7) Uani 1 1 d U . . H65 H 0.9683 1.0128 0.6124 0.028 Uiso 1 1 calc R . . C66 C 0.99777(9) 0.8013(3) 0.4560(2) 0.0213(7) Uani 1 1 d U . . C67 C 0.98839(9) 0.8472(3) 0.3720(2) 0.0248(7) Uani 1 1 d U . . H67 H 0.9643 0.8762 0.3642 0.030 Uiso 1 1 calc R . . C68 C 1.01297(10) 0.8518(3) 0.2998(2) 0.0281(7) Uani 1 1 d U . . H68 H 1.0051 0.8825 0.2450 0.034 Uiso 1 1 calc R . . C69 C 1.04927(10) 0.8109(3) 0.3085(2) 0.0277(7) Uani 1 1 d U . . H69 H 1.0663 0.8163 0.2608 0.033 Uiso 1 1 calc R . . C70 C 1.05960(10) 0.7622(3) 0.3894(2) 0.0264(7) Uani 1 1 d U . . H70 H 1.0837 0.7326 0.3963 0.032 Uiso 1 1 calc R . . C71 C 1.03429(10) 0.7570(3) 0.4608(2) 0.0245(7) Uani 1 1 d U . . H71 H 1.0419 0.7224 0.5143 0.029 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 Ru 0.02350(12) 0.01552(11) 0.02239(12) 0.00251(13) 0.00315(13) 0.00433(9) N1 0.0509(19) 0.0286(16) 0.0273(17) 0.0076(13) 0.0151(14) 0.0251(14) C1 0.070(3) 0.055(3) 0.030(2) 0.0100(19) 0.007(2) 0.046(2) C2 0.104(4) 0.091(4) 0.029(2) 0.026(2) 0.027(2) 0.080(3) C3 0.145(6) 0.051(3) 0.061(3) 0.041(3) 0.068(3) 0.069(3) C4 0.125(4) 0.022(2) 0.059(3) 0.019(2) 0.061(3) 0.034(2) C5 0.075(3) 0.0142(17) 0.050(2) 0.0074(16) 0.034(2) 0.0223(18) C6 0.060(2) 0.0136(14) 0.047(2) 0.0004(19) 0.030(2) 0.0005(14) C7 0.0317(18) 0.0139(15) 0.0319(18) -0.0033(13) 0.0134(15) 0.0032(13) N2 0.086(3) 0.0154(16) 0.064(2) -0.0142(15) 0.047(2) -0.0254(17) C9 0.173(6) 0.024(2) 0.100(5) -0.016(3) 0.076(5) -0.055(3) N8 0.062(2) 0.0290(18) 0.064(2) -0.0212(17) 0.0282(19) -0.0256(16) N3 0.0311(16) 0.0184(14) 0.0446(18) -0.0137(13) 0.0118(14) -0.0094(12) C10 0.0253(18) 0.0264(18) 0.047(2) -0.0144(16) -0.0054(16) -0.0004(14) C11 0.058(3) 0.037(2) 0.046(2) -0.0193(18) -0.012(2) 0.013(2) C12 0.072(3) 0.055(3) 0.041(2) -0.023(2) -0.012(2) 0.022(2) C13 0.057(3) 0.044(2) 0.048(3) -0.016(2) -0.019(2) 0.018(2) C14 0.032(2) 0.033(2) 0.046(2) -0.0157(18) -0.0152(18) 0.0076(16) C15 0.0200(17) 0.0312(19) 0.048(2) -0.0180(17) -0.0052(16) 0.0010(15) N4 0.0176(13) 0.0168(14) 0.0220(14) -0.0001(11) -0.0003(10) -0.0016(10) C16 0.0163(15) 0.0241(18) 0.0303(18) 0.0003(15) -0.0039(13) -0.0061(13) C17 0.037(2) 0.0267(19) 0.041(2) 0.0154(16) -0.0108(17) -0.0042(16) N5 0.0254(15) 0.0303(16) 0.0212(15) 0.0003(12) 0.0005(12) 0.0074(12) C18 0.0253(18) 0.0303(19) 0.0231(17) -0.0004(14) -0.0001(14) 0.0111(14) C19 0.0305(19) 0.0275(18) 0.0247(18) 0.0023(15) -0.0031(14) 0.0033(15) N6 0.0315(15) 0.0141(13) 0.0240(15) 0.0042(11) -0.0001(12) 0.0017(11) C20 0.0351(19) 0.0137(16) 0.033(2) 0.0068(14) 0.0095(16) 0.0008(14) C21 0.051(3) 0.033(2) 0.055(3) 0.006(2) 0.027(2) 0.0100(19) N7 0.0224(14) 0.0202(14) 0.0229(15) 0.0009(11) -0.0006(12) 0.0036(11) C22 0.0190(16) 0.0204(16) 0.0307(19) 0.0066(14) 0.0002(14) -0.0012(13) C23 0.0310(19) 0.0249(18) 0.0279(18) -0.0002(14) 0.0065(15) 0.0036(14) B1 0.0211(19) 0.0188(18) 0.031(2) 0.0014(15) -0.0007(16) 0.0007(14) C24 0.0244(17) 0.0152(15) 0.0258(17) 0.0023(13) 0.0007(14) -0.0035(13) C25 0.0265(19) 0.0154(18) 0.0277(19) 0.0041(14) 0.0024(15) -0.0021(13) C26 0.0356(19) 0.0293(18) 0.0208(17) 0.0025(14) 0.0037(14) -0.0051(15) C27 0.0273(18) 0.0281(18) 0.0325(19) 0.0091(15) -0.0061(15) -0.0024(15) C28 0.0267(18) 0.0235(18) 0.038(2) 0.0070(16) -0.0002(15) 0.0030(14) C29 0.0278(17) 0.0191(16) 0.0256(17) 0.0039(14) -0.0005(14) 0.0020(13) C30 0.0230(16) 0.0208(17) 0.0235(18) 0.0034(13) -0.0015(13) 0.0007(13) C31 0.0256(17) 0.0225(17) 0.0286(18) -0.0011(14) 0.0015(14) 0.0055(13) C32 0.0203(16) 0.0299(18) 0.0325(19) 0.0033(15) 0.0030(14) 0.0000(14) C33 0.0291(18) 0.0224(17) 0.043(2) 0.0053(15) -0.0042(16) -0.0064(14) C34 0.0379(17) 0.0196(15) 0.038(2) 0.0002(16) -0.0056(18) 0.0022(13) C35 0.0251(14) 0.0212(14) 0.0321(17) 0.0022(18) 0.0013(18) 0.0005(11) C36 0.0189(16) 0.0143(15) 0.0303(17) 0.0012(13) 0.0012(13) 0.0050(12) C37 0.0243(17) 0.0172(16) 0.0325(19) 0.0000(14) 0.0003(14) 0.0021(13) C38 0.030(2) 0.024(2) 0.030(2) -0.0039(15) -0.0063(16) 0.0063(15) C39 0.0287(18) 0.0218(17) 0.0247(17) 0.0056(14) 0.0054(14) 0.0087(14) C40 0.0222(17) 0.0261(18) 0.0319(19) -0.0012(15) 0.0004(14) -0.0003(13) C41 0.0218(16) 0.0210(16) 0.0241(17) 0.0006(13) -0.0038(13) -0.0004(13) C42 0.0209(15) 0.0225(16) 0.0215(16) 0.0024(13) 0.0074(12) 0.0000(13) C43 0.0247(16) 0.0224(16) 0.0333(19) 0.0004(13) 0.0013(13) 0.0016(13) C44 0.0196(16) 0.0290(19) 0.044(2) 0.0046(15) 0.0039(14) 0.0061(13) C45 0.0313(19) 0.0239(18) 0.038(2) 0.0003(15) 0.0110(16) 0.0093(14) C46 0.0323(19) 0.0206(17) 0.0315(19) 0.0005(14) 0.0057(15) 0.0007(14) C47 0.0250(17) 0.0240(17) 0.0249(17) 0.0020(14) 0.0007(14) 0.0035(13) B2 0.0234(18) 0.0167(17) 0.0258(19) 0.0000(15) 0.0031(15) -0.0044(14) C48 0.0273(17) 0.0196(16) 0.0224(17) 0.0014(13) -0.0016(13) -0.0047(13) C49 0.0290(18) 0.0235(17) 0.046(2) -0.0033(16) 0.0020(16) -0.0054(14) C50 0.031(2) 0.031(2) 0.060(3) -0.0015(18) 0.0047(18) -0.0137(15) C51 0.052(2) 0.0272(19) 0.053(3) -0.0093(18) 0.004(2) -0.0202(18) C52 0.050(2) 0.0229(18) 0.036(2) -0.0065(15) 0.0049(18) -0.0025(16) C53 0.0288(18) 0.0239(17) 0.0308(19) 0.0002(14) 0.0041(15) -0.0043(14) C54 0.0260(17) 0.0146(15) 0.0238(16) -0.0037(13) 0.0006(13) 0.0025(13) C55 0.0249(17) 0.0214(17) 0.0291(18) -0.0046(14) 0.0012(14) 0.0005(13) C56 0.046(2) 0.035(2) 0.0254(18) 0.0005(16) 0.0052(16) 0.0063(16) C57 0.046(2) 0.042(2) 0.0177(17) -0.0074(16) -0.0073(15) 0.0067(17) C58 0.0308(19) 0.0305(19) 0.035(2) -0.0090(16) -0.0068(15) -0.0002(15) C59 0.0307(17) 0.0157(15) 0.0237(17) -0.0025(13) -0.0015(14) 0.0011(13) C60 0.0245(16) 0.0191(15) 0.0230(17) 0.0005(13) 0.0034(13) -0.0028(13) C61 0.0256(17) 0.0278(18) 0.0283(19) -0.0045(15) 0.0009(14) -0.0012(14) C62 0.0231(17) 0.0346(19) 0.0298(17) 0.0042(15) 0.0018(14) 0.0006(14) C63 0.0287(18) 0.0253(18) 0.033(2) 0.0088(15) 0.0028(15) 0.0068(14) C64 0.040(2) 0.0174(16) 0.0296(19) -0.0032(14) 0.0038(15) -0.0017(14) C65 0.0297(17) 0.0223(16) 0.0186(17) -0.0014(13) -0.0044(13) 0.0006(13) C66 0.0270(17) 0.0129(15) 0.0241(16) -0.0041(12) 0.0017(13) -0.0047(13) C67 0.0237(17) 0.0226(18) 0.0281(18) 0.0030(15) -0.0032(14) -0.0023(14) C68 0.0352(19) 0.0270(18) 0.0222(17) 0.0041(14) -0.0027(14) -0.0013(15) C69 0.0347(19) 0.0203(17) 0.0280(18) -0.0010(14) 0.0106(15) 0.0014(14) C70 0.0304(18) 0.0179(16) 0.0308(19) -0.0025(13) 0.0057(14) 0.0061(14) C71 0.0367(19) 0.0138(15) 0.0229(15) 0.0009(13) -0.0018(15) 0.0032(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C7 1.999(3) . ? Ru N7 2.014(3) . ? Ru N6 2.015(3) . ? Ru N4 2.022(3) . ? Ru N1 2.086(3) . ? Ru N5 2.096(3) . ? N1 C1 1.331(5) . ? N1 C5 1.368(5) . ? C1 C2 1.418(6) . ? C1 H1 0.9300 . ? C2 C3 1.358(9) . ? C2 H2 0.9300 . ? C3 C4 1.354(9) . ? C3 H3 0.9300 . ? C4 C5 1.392(5) . ? C4 H4 0.9300 . ? C5 C6 1.434(7) . ? C6 N2 1.354(6) . ? C6 C7 1.402(5) . ? C7 N3 1.351(5) . ? N2 N8 1.311(6) . ? N2 C9 1.472(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? N8 N3 1.345(4) . ? N3 C10 1.428(5) . ? C10 C11 1.373(5) . ? C10 C15 1.395(5) . ? C11 C12 1.372(6) . ? C11 H11 0.9300 . ? C12 C13 1.396(6) . ? C12 H12 0.9300 . ? C13 C14 1.383(6) . ? C13 H13 0.9300 . ? C14 C15 1.353(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? N4 C16 1.140(4) . ? C16 C17 1.451(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? N5 C18 1.137(4) . ? C18 C19 1.456(5) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? N6 C20 1.138(4) . ? C20 C21 1.464(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? N7 C22 1.130(4) . ? C22 C23 1.457(5) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? B1 C24 1.628(5) . ? B1 C36 1.637(5) . ? B1 C42 1.645(5) . ? B1 C30 1.646(5) . ? C24 C25 1.403(5) . ? C24 C29 1.404(5) . ? C25 C26 1.384(5) . ? C25 H25 0.9300 . ? C26 C27 1.393(5) . ? C26 H26 0.9300 . ? C27 C28 1.376(5) . ? C27 H27 0.9300 . ? C28 C29 1.386(5) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C35 1.399(5) . ? C30 C31 1.405(5) . ? C31 C32 1.366(5) . ? C31 H31 0.9300 . ? C32 C33 1.391(5) . ? C32 H32 0.9300 . ? C33 C34 1.383(5) . ? C33 H33 0.9300 . ? C34 C35 1.392(4) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.398(5) . ? C36 C41 1.402(5) . ? C37 C38 1.378(5) . ? C37 H37 0.9300 . ? C38 C39 1.377(5) . ? C38 H38 0.9300 . ? C39 C40 1.381(5) . ? C39 H39 0.9300 . ? C40 C41 1.386(5) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C47 1.397(5) . ? C42 C43 1.399(4) . ? C43 C44 1.393(5) . ? C43 H43 0.9300 . ? C44 C45 1.370(5) . ? C44 H44 0.9300 . ? C45 C46 1.370(5) . ? C45 H45 0.9300 . ? C46 C47 1.402(5) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? B2 C60 1.642(5) . ? B2 C66 1.651(5) . ? B2 C48 1.655(4) . ? B2 C54 1.658(5) . ? C48 C53 1.397(5) . ? C48 C49 1.399(5) . ? C49 C50 1.389(5) . ? C49 H49 0.9300 . ? C50 C51 1.383(6) . ? C50 H50 0.9300 . ? C51 C52 1.380(5) . ? C51 H51 0.9300 . ? C52 C53 1.389(5) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 C55 1.397(5) . ? C54 C59 1.403(4) . ? C55 C56 1.384(5) . ? C55 H55 0.9300 . ? C56 C57 1.379(5) . ? C56 H56 0.9300 . ? C57 C58 1.397(5) . ? C57 H57 0.9300 . ? C58 C59 1.378(5) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C60 C61 1.394(5) . ? C60 C65 1.398(4) . ? C61 C62 1.382(5) . ? C61 H61 0.9300 . ? C62 C63 1.391(5) . ? C62 H62 0.9300 . ? C63 C64 1.376(5) . ? C63 H63 0.9300 . ? C64 C65 1.402(5) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C66 C67 1.394(4) . ? C66 C71 1.402(5) . ? C67 C68 1.379(5) . ? C67 H67 0.9300 . ? C68 C69 1.384(5) . ? C68 H68 0.9300 . ? C69 C70 1.375(5) . ? C69 H69 0.9300 . ? C70 C71 1.387(4) . ? C70 H70 0.9300 . ? C71 H71 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 C7 Ru N7 87.82(12) . . ? C7 Ru N6 89.22(12) . . ? N7 Ru N6 177.00(11) . . ? C7 Ru N4 100.70(12) . . ? N7 Ru N4 89.27(10) . . ? N6 Ru N4 90.87(10) . . ? C7 Ru N1 78.77(14) . . ? N7 Ru N1 92.71(10) . . ? N6 Ru N1 87.13(10) . . ? N4 Ru N1 177.94(11) . . ? C7 Ru N5 172.62(13) . . ? N7 Ru N5 91.50(10) . . ? N6 Ru N5 91.50(11) . . ? N4 Ru N5 86.63(10) . . ? N1 Ru N5 93.92(12) . . ? C1 N1 C5 118.5(4) . . ? C1 N1 Ru 124.0(3) . . ? C5 N1 Ru 117.4(3) . . ? N1 C1 C2 120.8(5) . . ? N1 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? C3 C2 C1 120.1(6) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 119.0(5) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.2(6) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? N1 C5 C4 121.3(5) . . ? N1 C5 C6 110.1(3) . . ? C4 C5 C6 128.7(5) . . ? N2 C6 C7 107.0(4) . . ? N2 C6 C5 133.4(4) . . ? C7 C6 C5 119.4(4) . . ? N3 C7 C6 101.9(3) . . ? N3 C7 Ru 144.1(3) . . ? C6 C7 Ru 114.0(3) . . ? N8 N2 C6 112.8(3) . . ? N8 N2 C9 117.1(5) . . ? C6 N2 C9 130.0(5) . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 N8 N3 103.0(3) . . ? N8 N3 C7 115.3(3) . . ? N8 N3 C10 116.6(3) . . ? C7 N3 C10 128.0(3) . . ? C11 C10 C15 120.9(4) . . ? C11 C10 N3 119.9(3) . . ? C15 C10 N3 119.1(3) . . ? C12 C11 C10 119.9(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 119.5(4) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C15 C14 C13 121.3(4) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C10 118.9(4) . . ? C14 C15 H15 120.6 . . ? C10 C15 H15 120.6 . . ? C16 N4 Ru 175.7(3) . . ? N4 C16 C17 178.5(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C18 N5 Ru 177.9(3) . . ? N5 C18 C19 179.2(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C20 N6 Ru 173.6(3) . . ? N6 C20 C21 178.2(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 N7 Ru 173.5(3) . . ? N7 C22 C23 179.7(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C24 B1 C36 112.8(3) . . ? C24 B1 C42 113.0(3) . . ? C36 B1 C42 103.4(3) . . ? C24 B1 C30 102.9(3) . . ? C36 B1 C30 113.3(3) . . ? C42 B1 C30 111.7(3) . . ? C25 C24 C29 114.1(3) . . ? C25 C24 B1 123.5(3) . . ? C29 C24 B1 122.2(3) . . ? C26 C25 C24 123.3(3) . . ? C26 C25 H25 118.3 . . ? C24 C25 H25 118.3 . . ? C25 C26 C27 120.3(3) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 118.3(3) . . ? C28 C27 H27 120.9 . . ? C26 C27 H27 120.9 . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C24 123.5(3) . . ? C28 C29 H29 118.3 . . ? C24 C29 H29 118.3 . . ? C35 C30 C31 115.2(3) . . ? C35 C30 B1 122.7(3) . . ? C31 C30 B1 121.7(3) . . ? C32 C31 C30 123.3(3) . . ? C32 C31 H31 118.3 . . ? C30 C31 H31 118.3 . . ? C31 C32 C33 120.3(3) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 118.5(3) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? C33 C34 C35 120.5(3) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C30 122.1(3) . . ? C34 C35 H35 118.9 . . ? C30 C35 H35 118.9 . . ? C37 C36 C41 115.3(3) . . ? C37 C36 B1 122.9(3) . . ? C41 C36 B1 121.4(3) . . ? C38 C37 C36 122.3(3) . . ? C38 C37 H37 118.8 . . ? C36 C37 H37 118.8 . . ? C39 C38 C37 120.9(4) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C38 C39 C40 118.7(3) . . ? C38 C39 H39 120.7 . . ? C40 C39 H39 120.7 . . ? C39 C40 C41 120.0(3) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C40 C41 C36 122.7(3) . . ? C40 C41 H41 118.7 . . ? C36 C41 H41 118.7 . . ? C47 C42 C43 115.3(3) . . ? C47 C42 B1 121.7(3) . . ? C43 C42 B1 122.3(3) . . ? C44 C43 C42 122.4(3) . . ? C44 C43 H43 118.8 . . ? C42 C43 H43 118.8 . . ? C45 C44 C43 120.4(3) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C46 119.5(3) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C45 C46 C47 119.9(3) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C42 C47 C46 122.5(3) . . ? C42 C47 H47 118.7 . . ? C46 C47 H47 118.7 . . ? C60 B2 C66 107.5(3) . . ? C60 B2 C48 112.6(3) . . ? C66 B2 C48 107.7(3) . . ? C60 B2 C54 109.3(3) . . ? C66 B2 C54 111.8(3) . . ? C48 B2 C54 108.0(3) . . ? C53 C48 C49 114.9(3) . . ? C53 C48 B2 122.2(3) . . ? C49 C48 B2 122.8(3) . . ? C50 C49 C48 122.9(3) . . ? C50 C49 H49 118.5 . . ? C48 C49 H49 118.5 . . ? C51 C50 C49 119.9(4) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C52 C51 C50 119.3(3) . . ? C52 C51 H51 120.3 . . ? C50 C51 H51 120.3 . . ? C51 C52 C53 119.6(3) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C52 C53 C48 123.3(3) . . ? C52 C53 H53 118.3 . . ? C48 C53 H53 118.3 . . ? C55 C54 C59 114.5(3) . . ? C55 C54 B2 122.4(3) . . ? C59 C54 B2 123.1(3) . . ? C56 C55 C54 123.2(3) . . ? C56 C55 H55 118.4 . . ? C54 C55 H55 118.4 . . ? C57 C56 C55 120.8(3) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C56 C57 C58 117.6(3) . . ? C56 C57 H57 121.2 . . ? C58 C57 H57 121.2 . . ? C59 C58 C57 120.8(3) . . ? C59 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? C58 C59 C54 123.0(3) . . ? C58 C59 H59 118.5 . . ? C54 C59 H59 118.5 . . ? C61 C60 C65 114.8(3) . . ? C61 C60 B2 123.1(3) . . ? C65 C60 B2 121.7(3) . . ? C62 C61 C60 123.4(3) . . ? C62 C61 H61 118.3 . . ? C60 C61 H61 118.3 . . ? C61 C62 C63 120.2(3) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C64 C63 C62 118.6(3) . . ? C64 C63 H63 120.7 . . ? C62 C63 H63 120.7 . . ? C63 C64 C65 120.1(3) . . ? C63 C64 H64 120.0 . . ? C65 C64 H64 120.0 . . ? C60 C65 C64 122.9(3) . . ? C60 C65 H65 118.5 . . ? C64 C65 H65 118.5 . . ? C67 C66 C71 114.3(3) . . ? C67 C66 B2 122.5(3) . . ? C71 C66 B2 123.2(3) . . ? C68 C67 C66 123.4(3) . . ? C68 C67 H67 118.3 . . ? C66 C67 H67 118.3 . . ? C67 C68 C69 120.4(3) . . ? C67 C68 H68 119.8 . . ? C69 C68 H68 119.8 . . ? C70 C69 C68 118.4(3) . . ? C70 C69 H69 120.8 . . ? C68 C69 H69 120.8 . . ? C69 C70 C71 120.3(3) . . ? C69 C70 H70 119.9 . . ? C71 C70 H70 119.9 . . ? C70 C71 C66 123.1(3) . . ? C70 C71 H71 118.4 . . ? C66 C71 H71 118.4 . . ? 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 C7 Ru N1 C1 -178.1(3) . . . . ? N7 Ru N1 C1 -90.8(3) . . . . ? N6 Ru N1 C1 92.2(3) . . . . ? N5 Ru N1 C1 0.9(3) . . . . ? C7 Ru N1 C5 6.5(2) . . . . ? N7 Ru N1 C5 93.7(2) . . . . ? N6 Ru N1 C5 -83.3(2) . . . . ? N4 Ru N1 C5 -69(4) . . . . ? N5 Ru N1 C5 -174.6(2) . . . . ? C5 N1 C1 C2 2.8(5) . . . . ? Ru N1 C1 C2 -172.6(3) . . . . ? N1 C1 C2 C3 -0.8(6) . . . . ? C1 C2 C3 C4 -1.0(7) . . . . ? C2 C3 C4 C5 0.8(7) . . . . ? C1 N1 C5 C4 -3.1(5) . . . . ? Ru N1 C5 C4 172.7(3) . . . . ? C1 N1 C5 C6 177.4(3) . . . . ? Ru N1 C5 C6 -6.9(4) . . . . ? C3 C4 C5 N1 1.3(6) . . . . ? C3 C4 C5 C6 -179.2(4) . . . . ? N1 C5 C6 N2 -171.3(4) . . . . ? C4 C5 C6 N2 9.2(7) . . . . ? N1 C5 C6 C7 3.3(5) . . . . ? C4 C5 C6 C7 -176.3(4) . . . . ? N2 C6 C7 N3 0.1(4) . . . . ? C5 C6 C7 N3 -175.8(3) . . . . ? N2 C6 C7 Ru 177.8(2) . . . . ? C5 C6 C7 Ru 1.9(4) . . . . ? N7 Ru C7 N3 78.8(4) . . . . ? N6 Ru C7 N3 -100.8(4) . . . . ? N4 Ru C7 N3 -10.1(4) . . . . ? N1 Ru C7 N3 171.9(4) . . . . ? N7 Ru C7 C6 -97.4(2) . . . . ? N6 Ru C7 C6 83.0(2) . . . . ? N4 Ru C7 C6 173.7(2) . . . . ? N1 Ru C7 C6 -4.2(2) . . . . ? C7 C6 N2 N8 0.0(4) . . . . ? C5 C6 N2 N8 175.0(4) . . . . ? C7 C6 N2 C9 178.6(4) . . . . ? C5 C6 N2 C9 -6.4(7) . . . . ? C6 N2 N8 N3 -0.1(4) . . . . ? C9 N2 N8 N3 -178.9(4) . . . . ? N2 N8 N3 C7 0.2(4) . . . . ? N2 N8 N3 C10 -176.7(3) . . . . ? C6 C7 N3 N8 -0.2(4) . . . . ? Ru C7 N3 N8 -176.6(3) . . . . ? C6 C7 N3 C10 176.3(3) . . . . ? Ru C7 N3 C10 -0.1(6) . . . . ? N8 N3 C10 C11 56.0(5) . . . . ? C7 N3 C10 C11 -120.4(4) . . . . ? N8 N3 C10 C15 -125.2(3) . . . . ? C7 N3 C10 C15 58.4(5) . . . . ? C15 C10 C11 C12 -0.4(6) . . . . ? N3 C10 C11 C12 178.4(4) . . . . ? C10 C11 C12 C13 -0.8(7) . . . . ? C11 C12 C13 C14 1.4(7) . . . . ? C12 C13 C14 C15 -0.9(6) . . . . ? C13 C14 C15 C10 -0.2(6) . . . . ? C11 C10 C15 C14 0.9(5) . . . . ? N3 C10 C15 C14 -177.9(3) . . . . ? C36 B1 C24 C25 150.9(3) . . . . ? C42 B1 C24 C25 34.1(4) . . . . ? C30 B1 C24 C25 -86.6(3) . . . . ? C36 B1 C24 C29 -35.4(4) . . . . ? C42 B1 C24 C29 -152.2(3) . . . . ? C30 B1 C24 C29 87.1(4) . . . . ? C29 C24 C25 C26 1.0(5) . . . . ? B1 C24 C25 C26 175.2(3) . . . . ? C24 C25 C26 C27 -0.5(5) . . . . ? C25 C26 C27 C28 -0.1(5) . . . . ? C26 C27 C28 C29 0.1(5) . . . . ? C27 C28 C29 C24 0.5(5) . . . . ? C25 C24 C29 C28 -1.0(5) . . . . ? B1 C24 C29 C28 -175.2(3) . . . . ? C24 B1 C30 C35 -89.2(4) . . . . ? C36 B1 C30 C35 33.0(4) . . . . ? C42 B1 C30 C35 149.3(3) . . . . ? C24 B1 C30 C31 83.8(4) . . . . ? C36 B1 C30 C31 -154.1(3) . . . . ? C42 B1 C30 C31 -37.8(4) . . . . ? C35 C30 C31 C32 -0.1(5) . . . . ? B1 C30 C31 C32 -173.5(3) . . . . ? C30 C31 C32 C33 -0.4(5) . . . . ? C31 C32 C33 C34 0.0(5) . . . . ? C32 C33 C34 C35 1.0(5) . . . . ? C33 C34 C35 C30 -1.6(6) . . . . ? C31 C30 C35 C34 1.1(5) . . . . ? B1 C30 C35 C34 174.4(3) . . . . ? C24 B1 C36 C37 149.1(3) . . . . ? C42 B1 C36 C37 -88.5(3) . . . . ? C30 B1 C36 C37 32.6(4) . . . . ? C24 B1 C36 C41 -38.2(4) . . . . ? C42 B1 C36 C41 84.2(3) . . . . ? C30 B1 C36 C41 -154.7(3) . . . . ? C41 C36 C37 C38 0.9(5) . . . . ? B1 C36 C37 C38 174.0(3) . . . . ? C36 C37 C38 C39 -0.2(5) . . . . ? C37 C38 C39 C40 -1.5(5) . . . . ? C38 C39 C40 C41 2.5(5) . . . . ? C39 C40 C41 C36 -1.7(5) . . . . ? C37 C36 C41 C40 0.0(4) . . . . ? B1 C36 C41 C40 -173.2(3) . . . . ? C24 B1 C42 C47 39.5(4) . . . . ? C36 B1 C42 C47 -82.8(4) . . . . ? C30 B1 C42 C47 155.0(3) . . . . ? C24 B1 C42 C43 -150.9(3) . . . . ? C36 B1 C42 C43 86.8(3) . . . . ? C30 B1 C42 C43 -35.4(4) . . . . ? C47 C42 C43 C44 -1.6(5) . . . . ? B1 C42 C43 C44 -171.9(3) . . . . ? C42 C43 C44 C45 1.1(5) . . . . ? C43 C44 C45 C46 0.1(5) . . . . ? C44 C45 C46 C47 -0.6(5) . . . . ? C43 C42 C47 C46 1.1(5) . . . . ? B1 C42 C47 C46 171.4(3) . . . . ? C45 C46 C47 C42 0.0(5) . . . . ? C60 B2 C48 C53 152.0(3) . . . . ? C66 B2 C48 C53 33.6(4) . . . . ? C54 B2 C48 C53 -87.2(4) . . . . ? C60 B2 C48 C49 -31.6(4) . . . . ? C66 B2 C48 C49 -150.0(3) . . . . ? C54 B2 C48 C49 89.2(4) . . . . ? C53 C48 C49 C50 -0.3(5) . . . . ? B2 C48 C49 C50 -177.0(3) . . . . ? C48 C49 C50 C51 0.0(6) . . . . ? C49 C50 C51 C52 1.1(7) . . . . ? C50 C51 C52 C53 -1.7(6) . . . . ? C51 C52 C53 C48 1.4(6) . . . . ? C49 C48 C53 C52 -0.4(5) . . . . ? B2 C48 C53 C52 176.3(3) . . . . ? C60 B2 C54 C55 93.5(3) . . . . ? C66 B2 C54 C55 -147.6(3) . . . . ? C48 B2 C54 C55 -29.4(4) . . . . ? C60 B2 C54 C59 -85.3(3) . . . . ? C66 B2 C54 C59 33.6(4) . . . . ? C48 B2 C54 C59 151.8(3) . . . . ? C59 C54 C55 C56 -1.5(5) . . . . ? B2 C54 C55 C56 179.6(3) . . . . ? C54 C55 C56 C57 0.7(5) . . . . ? C55 C56 C57 C58 1.0(5) . . . . ? C56 C57 C58 C59 -1.8(5) . . . . ? C57 C58 C59 C54 0.9(5) . . . . ? C55 C54 C59 C58 0.7(5) . . . . ? B2 C54 C59 C58 179.6(3) . . . . ? C66 B2 C60 C61 81.5(4) . . . . ? C48 B2 C60 C61 -37.0(4) . . . . ? C54 B2 C60 C61 -157.0(3) . . . . ? C66 B2 C60 C65 -90.1(4) . . . . ? C48 B2 C60 C65 151.4(3) . . . . ? C54 B2 C60 C65 31.4(4) . . . . ? C65 C60 C61 C62 -0.2(5) . . . . ? B2 C60 C61 C62 -172.3(3) . . . . ? C60 C61 C62 C63 0.7(5) . . . . ? C61 C62 C63 C64 -0.7(5) . . . . ? C62 C63 C64 C65 0.2(5) . . . . ? C61 C60 C65 C64 -0.3(5) . . . . ? B2 C60 C65 C64 171.9(3) . . . . ? C63 C64 C65 C60 0.3(5) . . . . ? C60 B2 C66 C67 -31.1(4) . . . . ? C48 B2 C66 C67 90.5(3) . . . . ? C54 B2 C66 C67 -151.1(3) . . . . ? C60 B2 C66 C71 151.1(3) . . . . ? C48 B2 C66 C71 -87.3(4) . . . . ? C54 B2 C66 C71 31.1(4) . . . . ? C71 C66 C67 C68 -1.6(5) . . . . ? B2 C66 C67 C68 -179.6(3) . . . . ? C66 C67 C68 C69 -0.8(5) . . . . ? C67 C68 C69 C70 2.4(5) . . . . ? C68 C69 C70 C71 -1.5(5) . . . . ? C69 C70 C71 C66 -1.1(5) . . . . ? C67 C66 C71 C70 2.6(4) . . . . ? B2 C66 C71 C70 -179.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.83 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.504 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.058 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.335 0.070 0.285 130 26 ' 0.75 (C2 H3 N), 0.25 (C4 H10 O) ' 2 0.665 -0.070 0.785 130 26 ' 0.75 (C2 H3 N), 0.25 (C4 H10 O) ' 3 0.835 0.430 0.285 130 26 ' 0.75 (C2 H3 N), 0.25 (C4 H10 O) ' 4 0.165 0.570 0.785 130 26 ' 0.75 (C2 H3 N), 0.25 (C4 H10 O) ' _platon_squeeze_details ; ; #===END data_alb52(3a) _database_code_depnum_ccdc_archive 'CCDC 817669' #TrackingRef 'alb09pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H22 N8 Ru, 2 (C F3 O3 S)' _chemical_formula_sum 'C19 H22 F6 N8 O6 Ru S2' _chemical_formula_weight 737.64 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' F F 0.0171 0.0103 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8566(5) _cell_length_b 11.8285(4) _cell_length_c 12.7801(5) _cell_angle_alpha 71.673(3) _cell_angle_beta 72.374(4) _cell_angle_gamma 65.259(4) _cell_volume 1386.76(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16260 _cell_measurement_theta_min 3.3317 _cell_measurement_theta_max 32.9188 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2558 _exptl_crystal_size_mid 0.1536 _exptl_crystal_size_min 0.0943 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31523 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 32.99 _reflns_number_total 9541 _reflns_number_gt 8090 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0320P)^2^+0.1147P] 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 9541 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _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 Ru Ru 0.584447(10) 0.732931(10) 0.695731(9) 0.00976(3) Uani 1 1 d . . . N1 N 0.41950(11) 0.89801(11) 0.73319(9) 0.0113(2) Uani 1 1 d . . . C1 C 0.41640(15) 1.01759(13) 0.68482(12) 0.0156(3) Uani 1 1 d . . . H1 H 0.4926 1.0292 0.6277 0.019 Uiso 1 1 calc R . . C2 C 0.30772(15) 1.12462(14) 0.71418(13) 0.0182(3) Uani 1 1 d . . . H2 H 0.3098 1.2075 0.6781 0.022 Uiso 1 1 calc R . . C3 C 0.19629(16) 1.10884(14) 0.79678(13) 0.0186(3) Uani 1 1 d . . . H3 H 0.1207 1.1809 0.8185 0.022 Uiso 1 1 calc R . . C4 C 0.19577(15) 0.98687(13) 0.84779(12) 0.0161(3) Uani 1 1 d . . . H4 H 0.1197 0.9743 0.9045 0.019 Uiso 1 1 calc R . . C5 C 0.30804(14) 0.88313(13) 0.81484(11) 0.0117(2) Uani 1 1 d . . . C6 C 0.33049(13) 0.74835(13) 0.85809(11) 0.0114(2) Uani 1 1 d . . . C7 C 0.45332(13) 0.65987(13) 0.81427(11) 0.0112(2) Uani 1 1 d . . . N2 N 0.25597(11) 0.68313(11) 0.93981(9) 0.0121(2) Uani 1 1 d . . . C8 C 0.12167(15) 0.72943(15) 1.01451(12) 0.0184(3) Uani 1 1 d . . . H8A H 0.0931 0.6572 1.0592 0.028 Uiso 1 1 calc R . . H8B H 0.0524 0.7894 0.9694 0.028 Uiso 1 1 calc R . . H8C H 0.1298 0.7726 1.0648 0.028 Uiso 1 1 calc R . . N3 N 0.32192(12) 0.55835(11) 0.95234(10) 0.0137(2) Uani 1 1 d . . . N4 N 0.44065(12) 0.54718(11) 0.87609(9) 0.0117(2) Uani 1 1 d . . . C9 C 0.53829(15) 0.41928(13) 0.86615(12) 0.0158(3) Uani 1 1 d . . . H9A H 0.5238 0.3588 0.9372 0.024 Uiso 1 1 calc R . . H9B H 0.6331 0.4182 0.8489 0.024 Uiso 1 1 calc R . . H9C H 0.5236 0.3949 0.8056 0.024 Uiso 1 1 calc R . . N5 N 0.70639(12) 0.83552(11) 0.57797(10) 0.0136(2) Uani 1 1 d . . . C10 C 0.77477(14) 0.89208(14) 0.52325(11) 0.0148(3) Uani 1 1 d . . . C11 C 0.86096(17) 0.96602(16) 0.45466(13) 0.0232(3) Uani 1 1 d . . . H11A H 0.8215 1.0216 0.3887 0.035 Uiso 1 1 calc R . . H11B H 0.9546 0.9081 0.4300 0.035 Uiso 1 1 calc R . . H11C H 0.8649 1.0181 0.4990 0.035 Uiso 1 1 calc R . . N6 N 0.74201(12) 0.56971(11) 0.66392(9) 0.0125(2) Uani 1 1 d . . . C12 C 0.83534(14) 0.48388(13) 0.63947(11) 0.0130(2) Uani 1 1 d . . . C13 C 0.95418(14) 0.37414(13) 0.60737(12) 0.0157(3) Uani 1 1 d . . . H13A H 0.9538 0.3671 0.5331 0.024 Uiso 1 1 calc R . . H13B H 0.9489 0.2964 0.6628 0.024 Uiso 1 1 calc R . . H13C H 1.0397 0.3852 0.6047 0.024 Uiso 1 1 calc R . . N7 N 0.50171(12) 0.72663(11) 0.57558(10) 0.0135(2) Uani 1 1 d . . . C14 C 0.46111(14) 0.70412(14) 0.51476(12) 0.0152(3) Uani 1 1 d . . . C15 C 0.41094(16) 0.67220(16) 0.43822(13) 0.0213(3) Uani 1 1 d . . . H15A H 0.4885 0.6380 0.3794 0.032 Uiso 1 1 calc R . . H15B H 0.3419 0.7490 0.4037 0.032 Uiso 1 1 calc R . . H15C H 0.3686 0.6081 0.4801 0.032 Uiso 1 1 calc R . . N8 N 0.67218(11) 0.72338(11) 0.81845(9) 0.0120(2) Uani 1 1 d . . . C16 C 0.72375(14) 0.70756(13) 0.89000(12) 0.0146(3) Uani 1 1 d . . . C17 C 0.78832(17) 0.68873(16) 0.98174(13) 0.0237(3) Uani 1 1 d . . . H17A H 0.8223 0.7581 0.9675 0.036 Uiso 1 1 calc R . . H17B H 0.8660 0.6071 0.9870 0.036 Uiso 1 1 calc R . . H17C H 0.7202 0.6884 1.0525 0.036 Uiso 1 1 calc R . . O1 O 0.79099(11) 0.52193(11) 0.40226(9) 0.0210(2) Uani 1 1 d . . . O2 O 0.91494(12) 0.56960(11) 0.21017(9) 0.0258(2) Uani 1 1 d . . . O3 O 0.69373(11) 0.54348(12) 0.24639(10) 0.0258(3) Uani 1 1 d . . . C18 C 0.90644(16) 0.34377(15) 0.29057(14) 0.0210(3) Uani 1 1 d . . . F1 F 1.02278(10) 0.29952(10) 0.32839(9) 0.0336(2) Uani 1 1 d . . . F2 F 0.93908(11) 0.32117(11) 0.18808(10) 0.0397(3) Uani 1 1 d . . . F3 F 0.82869(12) 0.27666(10) 0.35654(11) 0.0473(3) Uani 1 1 d . . . S1 S 0.81648(4) 0.51424(3) 0.28666(3) 0.01435(7) Uani 1 1 d . . . O4 O 0.81243(13) 0.18570(11) 0.78782(11) 0.0321(3) Uani 1 1 d . . . O5 O 0.81665(13) 0.03613(14) 0.69295(11) 0.0366(3) Uani 1 1 d . . . O6 O 0.89220(13) -0.04038(12) 0.87175(11) 0.0361(3) Uani 1 1 d . . . S2 S 0.80947(4) 0.06246(3) 0.79735(3) 0.01677(7) Uani 1 1 d . . . C19 C 0.63309(15) 0.07725(14) 0.87372(13) 0.0180(3) Uani 1 1 d . . . F4 F 0.53904(10) 0.16720(9) 0.81491(9) 0.0289(2) Uani 1 1 d . . . F5 F 0.60715(11) 0.11171(10) 0.97022(8) 0.0316(2) Uani 1 1 d . . . F6 F 0.61162(11) -0.03045(10) 0.89562(11) 0.0413(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.00920(5) 0.01008(5) 0.00966(5) -0.00233(4) -0.00122(4) -0.00343(4) N1 0.0116(5) 0.0113(5) 0.0108(5) -0.0021(4) -0.0025(4) -0.0038(4) C1 0.0142(6) 0.0137(6) 0.0167(6) -0.0020(5) -0.0007(5) -0.0054(5) C2 0.0193(7) 0.0116(6) 0.0222(7) -0.0032(5) -0.0043(6) -0.0044(5) C3 0.0183(7) 0.0142(7) 0.0199(7) -0.0056(5) -0.0023(6) -0.0023(6) C4 0.0142(6) 0.0158(7) 0.0150(6) -0.0035(5) -0.0006(5) -0.0037(5) C5 0.0125(6) 0.0131(6) 0.0104(6) -0.0018(5) -0.0034(5) -0.0051(5) C6 0.0111(6) 0.0126(6) 0.0106(6) -0.0018(5) -0.0022(5) -0.0049(5) C7 0.0121(6) 0.0125(6) 0.0106(6) -0.0027(5) -0.0041(5) -0.0047(5) N2 0.0105(5) 0.0139(5) 0.0111(5) -0.0016(4) -0.0014(4) -0.0050(4) C8 0.0131(6) 0.0228(7) 0.0155(7) -0.0044(6) 0.0026(5) -0.0063(6) N3 0.0134(5) 0.0139(6) 0.0139(5) -0.0014(4) -0.0031(4) -0.0058(4) N4 0.0120(5) 0.0114(5) 0.0123(5) -0.0018(4) -0.0034(4) -0.0048(4) C9 0.0166(6) 0.0105(6) 0.0199(7) -0.0037(5) -0.0065(5) -0.0022(5) N5 0.0123(5) 0.0153(6) 0.0120(5) -0.0037(4) -0.0018(4) -0.0036(4) C10 0.0149(6) 0.0167(7) 0.0127(6) -0.0029(5) -0.0027(5) -0.0059(5) C11 0.0271(8) 0.0286(8) 0.0191(7) -0.0031(6) -0.0002(6) -0.0194(7) N6 0.0130(5) 0.0137(5) 0.0114(5) -0.0024(4) -0.0019(4) -0.0060(4) C12 0.0148(6) 0.0134(6) 0.0122(6) -0.0013(5) -0.0036(5) -0.0068(5) C13 0.0145(6) 0.0127(6) 0.0173(6) -0.0034(5) -0.0025(5) -0.0028(5) N7 0.0122(5) 0.0143(6) 0.0117(5) -0.0026(4) -0.0002(4) -0.0043(4) C14 0.0123(6) 0.0170(7) 0.0135(6) -0.0030(5) -0.0007(5) -0.0039(5) C15 0.0203(7) 0.0309(8) 0.0156(7) -0.0074(6) -0.0043(6) -0.0097(6) N8 0.0115(5) 0.0110(5) 0.0128(5) -0.0025(4) -0.0005(4) -0.0046(4) C16 0.0143(6) 0.0139(6) 0.0149(6) -0.0015(5) -0.0010(5) -0.0068(5) C17 0.0287(8) 0.0285(8) 0.0205(7) 0.0026(6) -0.0130(6) -0.0165(7) O1 0.0248(6) 0.0252(6) 0.0151(5) -0.0077(4) -0.0043(4) -0.0084(5) O2 0.0277(6) 0.0282(6) 0.0213(6) 0.0018(5) -0.0026(5) -0.0164(5) O3 0.0156(5) 0.0373(7) 0.0233(6) -0.0099(5) -0.0084(4) -0.0027(5) C18 0.0160(7) 0.0223(8) 0.0253(8) -0.0101(6) 0.0011(6) -0.0073(6) F1 0.0227(5) 0.0287(6) 0.0402(6) -0.0065(5) -0.0134(5) 0.0036(4) F2 0.0339(6) 0.0483(7) 0.0411(6) -0.0339(6) -0.0024(5) -0.0049(5) F3 0.0363(6) 0.0231(6) 0.0733(9) -0.0163(6) 0.0183(6) -0.0180(5) S1 0.01413(15) 0.01669(17) 0.01235(15) -0.00250(12) -0.00397(12) -0.00517(13) O4 0.0305(7) 0.0247(6) 0.0443(8) -0.0083(6) 0.0027(6) -0.0192(5) O5 0.0278(6) 0.0546(9) 0.0288(7) -0.0241(6) 0.0024(5) -0.0109(6) O6 0.0206(6) 0.0332(7) 0.0419(8) 0.0079(6) -0.0128(6) -0.0047(5) S2 0.01446(16) 0.01711(17) 0.01801(17) -0.00267(13) -0.00152(13) -0.00697(13) C19 0.0175(7) 0.0146(7) 0.0234(7) -0.0042(6) -0.0014(6) -0.0088(6) F4 0.0172(4) 0.0285(5) 0.0366(6) -0.0072(4) -0.0083(4) -0.0019(4) F5 0.0302(5) 0.0415(6) 0.0205(5) -0.0094(4) 0.0033(4) -0.0142(5) F6 0.0269(5) 0.0199(5) 0.0747(9) -0.0151(5) 0.0085(6) -0.0155(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C7 1.9922(13) . ? Ru N8 2.0206(11) . ? Ru N6 2.0315(11) . ? Ru N7 2.0331(12) . ? Ru N1 2.0954(11) . ? Ru N5 2.1166(12) . ? N1 C1 1.3443(18) . ? N1 C5 1.3720(17) . ? C1 C2 1.3842(19) . ? C1 H1 0.9500 . ? C2 C3 1.380(2) . ? C2 H2 0.9500 . ? C3 C4 1.385(2) . ? C3 H3 0.9500 . ? C4 C5 1.3896(19) . ? C4 H4 0.9500 . ? C5 C6 1.4521(18) . ? C6 N2 1.3581(17) . ? C6 C7 1.3912(18) . ? C7 N4 1.3584(17) . ? N2 N3 1.3240(16) . ? N2 C8 1.4680(17) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N3 N4 1.3440(16) . ? N4 C9 1.4579(17) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? N5 C10 1.1378(18) . ? C10 C11 1.454(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N6 C12 1.1409(18) . ? C12 C13 1.4597(19) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? N7 C14 1.1425(18) . ? C14 C15 1.457(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N8 C16 1.1400(18) . ? C16 C17 1.456(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O1 S1 1.4434(11) . ? O2 S1 1.4414(12) . ? O3 S1 1.4416(11) . ? C18 F1 1.3267(18) . ? C18 F3 1.3276(19) . ? C18 F2 1.3314(18) . ? C18 S1 1.8277(16) . ? O4 S2 1.4373(12) . ? O5 S2 1.4358(13) . ? O6 S2 1.4373(13) . ? S2 C19 1.8290(15) . ? C19 F6 1.3192(17) . ? C19 F5 1.3326(17) . ? C19 F4 1.3388(18) . ? 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 C7 Ru N8 88.27(5) . . ? C7 Ru N6 99.97(5) . . ? N8 Ru N6 88.37(4) . . ? C7 Ru N7 89.75(5) . . ? N8 Ru N7 175.29(4) . . ? N6 Ru N7 87.77(4) . . ? C7 Ru N1 78.34(5) . . ? N8 Ru N1 91.07(4) . . ? N6 Ru N1 178.23(4) . . ? N7 Ru N1 92.71(4) . . ? C7 Ru N5 171.67(5) . . ? N8 Ru N5 89.58(4) . . ? N6 Ru N5 88.02(4) . . ? N7 Ru N5 92.97(5) . . ? N1 Ru N5 93.66(4) . . ? C1 N1 C5 117.55(12) . . ? C1 N1 Ru 124.67(9) . . ? C5 N1 Ru 117.76(9) . . ? N1 C1 C2 123.24(13) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 118.86(14) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.36(13) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.12(13) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.87(12) . . ? N1 C5 C6 109.73(11) . . ? C4 C5 C6 128.39(12) . . ? N2 C6 C7 107.92(12) . . ? N2 C6 C5 133.40(12) . . ? C7 C6 C5 118.64(12) . . ? N4 C7 C6 102.30(11) . . ? N4 C7 Ru 142.09(10) . . ? C6 C7 Ru 115.53(10) . . ? N3 N2 C6 111.50(11) . . ? N3 N2 C8 118.05(12) . . ? C6 N2 C8 130.43(12) . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 N3 N4 103.75(11) . . ? N3 N4 C7 114.53(11) . . ? N3 N4 C9 118.06(11) . . ? C7 N4 C9 127.38(12) . . ? N4 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C10 N5 Ru 173.47(11) . . ? N5 C10 C11 178.94(15) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 N6 Ru 174.66(12) . . ? N6 C12 C13 179.47(15) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C14 N7 Ru 169.83(12) . . ? N7 C14 C15 178.64(16) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C16 N8 Ru 174.41(11) . . ? N8 C16 C17 179.32(17) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? F1 C18 F3 107.80(14) . . ? F1 C18 F2 107.76(12) . . ? F3 C18 F2 107.56(13) . . ? F1 C18 S1 111.30(11) . . ? F3 C18 S1 111.66(10) . . ? F2 C18 S1 110.58(12) . . ? O2 S1 O3 115.36(7) . . ? O2 S1 O1 115.00(7) . . ? O3 S1 O1 114.35(7) . . ? O2 S1 C18 103.22(7) . . ? O3 S1 C18 103.15(7) . . ? O1 S1 C18 103.41(7) . . ? O5 S2 O4 114.66(9) . . ? O5 S2 O6 115.85(9) . . ? O4 S2 O6 114.92(8) . . ? O5 S2 C19 103.72(7) . . ? O4 S2 C19 102.53(7) . . ? O6 S2 C19 102.54(7) . . ? F6 C19 F5 108.82(13) . . ? F6 C19 F4 107.32(12) . . ? F5 C19 F4 106.49(12) . . ? F6 C19 S2 111.74(10) . . ? F5 C19 S2 110.70(10) . . ? F4 C19 S2 111.56(10) . . ? 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 C7 Ru N1 C1 179.09(12) . . . . ? N8 Ru N1 C1 91.07(11) . . . . ? N7 Ru N1 C1 -91.73(11) . . . . ? N5 Ru N1 C1 1.43(11) . . . . ? C7 Ru N1 C5 0.76(9) . . . . ? N8 Ru N1 C5 -87.25(10) . . . . ? N7 Ru N1 C5 89.94(10) . . . . ? N5 Ru N1 C5 -176.90(9) . . . . ? C5 N1 C1 C2 0.6(2) . . . . ? Ru N1 C1 C2 -177.75(11) . . . . ? N1 C1 C2 C3 -0.3(2) . . . . ? C1 C2 C3 C4 -0.2(2) . . . . ? C2 C3 C4 C5 0.3(2) . . . . ? C1 N1 C5 C4 -0.45(19) . . . . ? Ru N1 C5 C4 178.00(10) . . . . ? C1 N1 C5 C6 -179.26(12) . . . . ? Ru N1 C5 C6 -0.81(14) . . . . ? C3 C4 C5 N1 0.0(2) . . . . ? C3 C4 C5 C6 178.59(13) . . . . ? N1 C5 C6 N2 177.90(13) . . . . ? C4 C5 C6 N2 -0.8(2) . . . . ? N1 C5 C6 C7 0.39(17) . . . . ? C4 C5 C6 C7 -178.32(13) . . . . ? N2 C6 C7 N4 -0.40(14) . . . . ? C5 C6 C7 N4 177.71(11) . . . . ? N2 C6 C7 Ru -177.87(8) . . . . ? C5 C6 C7 Ru 0.23(16) . . . . ? N8 Ru C7 N4 -85.04(16) . . . . ? N6 Ru C7 N4 3.00(16) . . . . ? N7 Ru C7 N4 90.69(16) . . . . ? N1 Ru C7 N4 -176.49(16) . . . . ? N8 Ru C7 C6 90.95(10) . . . . ? N6 Ru C7 C6 178.99(10) . . . . ? N7 Ru C7 C6 -93.32(10) . . . . ? N1 Ru C7 C6 -0.50(9) . . . . ? C7 C6 N2 N3 0.12(15) . . . . ? C5 C6 N2 N3 -177.59(14) . . . . ? C7 C6 N2 C8 178.03(13) . . . . ? C5 C6 N2 C8 0.3(2) . . . . ? C6 N2 N3 N4 0.22(14) . . . . ? C8 N2 N3 N4 -177.98(11) . . . . ? N2 N3 N4 C7 -0.51(14) . . . . ? N2 N3 N4 C9 -178.89(11) . . . . ? C6 C7 N4 N3 0.57(15) . . . . ? Ru C7 N4 N3 176.87(11) . . . . ? C6 C7 N4 C9 178.77(12) . . . . ? Ru C7 N4 C9 -4.9(2) . . . . ? F1 C18 S1 O2 60.70(12) . . . . ? F3 C18 S1 O2 -178.78(12) . . . . ? F2 C18 S1 O2 -59.04(12) . . . . ? F1 C18 S1 O3 -178.85(11) . . . . ? F3 C18 S1 O3 -58.33(13) . . . . ? F2 C18 S1 O3 61.40(12) . . . . ? F1 C18 S1 O1 -59.45(12) . . . . ? F3 C18 S1 O1 61.07(13) . . . . ? F2 C18 S1 O1 -179.19(11) . . . . ? O5 S2 C19 F6 63.28(13) . . . . ? O4 S2 C19 F6 -177.09(12) . . . . ? O6 S2 C19 F6 -57.65(13) . . . . ? O5 S2 C19 F5 -175.25(11) . . . . ? O4 S2 C19 F5 -55.63(12) . . . . ? O6 S2 C19 F5 63.81(12) . . . . ? O5 S2 C19 F4 -56.86(12) . . . . ? O4 S2 C19 F4 62.76(12) . . . . ? O6 S2 C19 F4 -177.80(11) . . . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.652 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.079 #===END data_alb65(4) _database_code_depnum_ccdc_archive 'CCDC 817670' #TrackingRef 'alb09pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H21 N7 Ru, 2 (F6 P)' _chemical_formula_sum 'C17 H21 F12 N7 P2 Ru' _chemical_formula_weight 714.42 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' F F 0.0171 0.0103 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1535(2) _cell_length_b 11.7781(3) _cell_length_c 12.9329(3) _cell_angle_alpha 84.914(2) _cell_angle_beta 71.896(2) _cell_angle_gamma 85.969(2) _cell_volume 1318.72(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20907 _cell_measurement_theta_min 3.3161 _cell_measurement_theta_max 28.2436 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2576 _exptl_crystal_size_mid 0.1793 _exptl_crystal_size_min 0.1321 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; The disordered ligands were restrained to have the same shape using SAME. DELU restraints were applied to the atoms of the disordered ligand. P-F distances in the disordered anios were restrained to be equal using SADI. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34786 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6320 _reflns_number_gt 5820 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^)+(0.0303P)^2^+2.1621P] 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 6320 _refine_ls_number_parameters 531 _refine_ls_number_restraints 98 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0775 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _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 Ru Ru 0.94808(2) 0.735094(15) 0.733641(14) 0.02124(6) Uani 1 1 d U . . N1A N 1.0363(14) 0.6771(6) 0.5813(4) 0.0194(12) Uani 0.715(4) 1 d PD A 1 C1A C 1.1282(4) 0.5829(3) 0.5541(3) 0.0246(7) Uani 0.715(4) 1 d PD A 1 H1A H 1.1562 0.5371 0.6099 0.029 Uiso 0.715(4) 1 calc PR A 1 C2A C 1.1829(4) 0.5506(3) 0.4493(3) 0.0286(8) Uani 0.715(4) 1 d PD A 1 H2A H 1.2462 0.4830 0.4333 0.034 Uiso 0.715(4) 1 calc PR A 1 C3A C 1.1452(5) 0.6169(3) 0.3674(3) 0.0275(8) Uani 0.715(4) 1 d PD A 1 H3A H 1.1815 0.5949 0.2945 0.033 Uiso 0.715(4) 1 calc PR A 1 C4A C 1.0551(9) 0.7150(5) 0.3916(4) 0.0252(10) Uani 0.715(4) 1 d PD A 1 H4A H 1.0299 0.7628 0.3359 0.030 Uiso 0.715(4) 1 calc PR A 1 C5A C 1.0015(8) 0.7426(4) 0.4995(3) 0.0204(8) Uani 0.715(4) 1 d PD A 1 N2A N 0.9117(7) 0.8400(4) 0.5357(3) 0.0220(8) Uani 0.715(4) 1 d PD A 1 C6A C 0.8795(18) 0.8607(7) 0.6435(5) 0.0215(13) Uani 0.715(4) 1 d PD A 1 C7A C 0.8554(10) 0.9285(5) 0.4783(4) 0.0249(10) Uani 0.715(4) 1 d PD A 1 H7A H 0.8665 0.9344 0.4025 0.030 Uiso 0.715(4) 1 calc PR A 1 C8A C 0.7824(5) 1.0037(4) 0.5508(3) 0.0268(8) Uani 0.715(4) 1 d PD A 1 H8A H 0.7309 1.0733 0.5362 0.032 Uiso 0.715(4) 1 calc PR A 1 N3A N 0.7957(3) 0.9608(2) 0.6527(3) 0.0254(7) Uani 0.715(4) 1 d PD A 1 C9A C 0.7318(4) 1.0194(3) 0.7531(3) 0.0334(8) Uani 0.715(4) 1 d PD A 1 H9A1 H 0.6557 0.9720 0.8063 0.050 Uiso 0.715(4) 1 calc PR A 1 H9A2 H 0.6822 1.0925 0.7372 0.050 Uiso 0.715(4) 1 calc PR A 1 H9A3 H 0.8146 1.0331 0.7829 0.050 Uiso 0.715(4) 1 calc PR A 1 N1B N 0.859(4) 0.8729(17) 0.6612(11) 0.0174(16) Uani 0.285(4) 1 d PDU A 2 C1B C 0.7893(9) 0.9663(7) 0.7110(8) 0.0203(13) Uani 0.285(4) 1 d PDU A 2 H1B H 0.7794 0.9706 0.7859 0.024 Uiso 0.285(4) 1 calc PR A 2 C2B C 0.7323(9) 1.0553(6) 0.6576(6) 0.0238(14) Uani 0.285(4) 1 d PDU A 2 H2B H 0.6809 1.1194 0.6954 0.029 Uiso 0.285(4) 1 calc PR A 2 C3B C 0.7501(12) 1.0511(9) 0.5495(8) 0.0228(16) Uani 0.285(4) 1 d PDU A 2 H3B H 0.7088 1.1115 0.5118 0.027 Uiso 0.285(4) 1 calc PR A 2 C4B C 0.828(2) 0.9597(14) 0.4953(11) 0.0232(18) Uani 0.285(4) 1 d PDU A 2 H4B H 0.8403 0.9555 0.4200 0.028 Uiso 0.285(4) 1 calc PR A 2 C5B C 0.888(2) 0.8728(12) 0.5528(9) 0.0188(16) Uani 0.285(4) 1 d PDU A 2 N2B N 0.9731(16) 0.7792(10) 0.5069(8) 0.0205(16) Uani 0.285(4) 1 d PDU A 2 C6B C 1.030(4) 0.702(2) 0.5707(13) 0.020(2) Uani 0.285(4) 1 d PDU A 2 C7B C 1.028(2) 0.7511(14) 0.3985(10) 0.025(2) Uani 0.285(4) 1 d PDU A 2 H7B H 1.0043 0.7910 0.3380 0.031 Uiso 0.285(4) 1 calc PR A 2 C8B C 1.1175(12) 0.6587(11) 0.3963(8) 0.0272(18) Uani 0.285(4) 1 d PDU A 2 H8B H 1.1743 0.6212 0.3330 0.033 Uiso 0.285(4) 1 calc PR A 2 N3B N 1.1152(7) 0.6250(6) 0.5041(6) 0.0227(12) Uani 0.285(4) 1 d PDU A 2 C9B C 1.2033(10) 0.5273(7) 0.5337(8) 0.0320(19) Uani 0.285(4) 1 d PDU A 2 H9B1 H 1.2929 0.5535 0.5494 0.048 Uiso 0.285(4) 1 calc PR A 2 H9B2 H 1.2378 0.4774 0.4731 0.048 Uiso 0.285(4) 1 calc PR A 2 H9B3 H 1.1386 0.4849 0.5985 0.048 Uiso 0.285(4) 1 calc PR A 2 N4 N 0.8529(3) 0.79821(18) 0.88493(17) 0.0314(5) Uani 1 1 d . A . C10 C 0.7978(4) 0.8332(2) 0.9672(2) 0.0447(7) Uani 1 1 d . . . C11 C 0.7248(7) 0.8792(3) 1.0735(3) 0.0845(16) Uani 1 1 d . A . H11A H 0.6986 0.9606 1.0632 0.127 Uiso 1 1 calc R . . H11B H 0.7960 0.8690 1.1170 0.127 Uiso 1 1 calc R . . H11C H 0.6310 0.8387 1.1116 0.127 Uiso 1 1 calc R . . N5 N 1.1482(2) 0.80891(16) 0.71671(15) 0.0234(4) Uani 1 1 d . A . C12 C 1.2650(3) 0.8409(2) 0.71046(18) 0.0259(5) Uani 1 1 d . . . C13 C 1.4155(3) 0.8811(3) 0.7027(2) 0.0363(6) Uani 1 1 d . A . H13A H 1.4389 0.8592 0.7709 0.054 Uiso 1 1 calc R . . H13B H 1.4145 0.9644 0.6898 0.054 Uiso 1 1 calc R . . H13C H 1.4941 0.8468 0.6421 0.054 Uiso 1 1 calc R . . N6 N 1.0331(2) 0.59102(18) 0.80762(17) 0.0292(4) Uani 1 1 d . A . C14 C 1.0819(3) 0.5140(2) 0.8466(2) 0.0314(5) Uani 1 1 d . . . C15 C 1.1444(3) 0.4143(2) 0.8972(2) 0.0407(6) Uani 1 1 d . A . H15A H 1.1860 0.4387 0.9526 0.061 Uiso 1 1 calc R . . H15B H 1.2266 0.3763 0.8414 0.061 Uiso 1 1 calc R . . H15C H 1.0625 0.3612 0.9317 0.061 Uiso 1 1 calc R . . N7 N 0.7517(2) 0.65556(17) 0.75330(16) 0.0259(4) Uani 1 1 d . A . C16 C 0.6418(3) 0.6103(2) 0.7635(2) 0.0330(6) Uani 1 1 d . . . C17 C 0.5022(3) 0.5507(3) 0.7750(3) 0.0528(9) Uani 1 1 d . A . H17A H 0.4816 0.5557 0.7047 0.079 Uiso 1 1 calc R . . H17B H 0.4152 0.5860 0.8295 0.079 Uiso 1 1 calc R . . H17C H 0.5163 0.4703 0.7985 0.079 Uiso 1 1 calc R . . P1 P 0.58496(9) 0.72934(8) 0.40286(6) 0.0441(2) Uani 1 1 d . . . F1 F 0.6575(2) 0.71475(15) 0.50034(13) 0.0430(4) Uani 1 1 d . . . F2 F 0.5141(3) 0.7428(3) 0.3046(2) 0.1012(11) Uani 1 1 d . . . F3 F 0.4167(2) 0.7247(2) 0.48603(18) 0.0728(7) Uani 1 1 d . . . F4 F 0.5738(3) 0.8641(2) 0.4137(3) 0.1011(11) Uani 1 1 d . . . F5 F 0.7525(3) 0.7417(4) 0.31965(18) 0.1219(15) Uani 1 1 d . . . F6 F 0.5947(4) 0.5971(3) 0.3942(3) 0.1057(11) Uani 1 1 d . . . P2A P 0.2912(8) 0.7333(6) 0.0413(6) 0.0356(8) Uani 0.497(9) 1 d PD B 1 F7A F 0.1290(11) 0.7791(11) 0.1132(10) 0.130(5) Uani 0.497(9) 1 d PD B 1 F8A F 0.4566(8) 0.6927(12) -0.0274(9) 0.126(5) Uani 0.497(9) 1 d PD B 1 F9A F 0.2618(12) 0.6053(5) 0.0715(7) 0.123(4) Uani 0.497(9) 1 d PD B 1 F10A F 0.3582(11) 0.7387(7) 0.1376(5) 0.0600(19) Uani 0.497(9) 1 d PD B 1 F11A F 0.3199(17) 0.8613(6) 0.0112(9) 0.163(5) Uani 0.497(9) 1 d PD B 1 F12A F 0.2258(7) 0.7245(6) -0.0572(4) 0.0691(18) Uani 0.497(9) 1 d PD B 1 P2B P 0.2827(9) 0.7566(6) 0.0391(6) 0.0512(16) Uani 0.503(9) 1 d PD B 2 F7B F 0.1980(7) 0.8273(9) -0.0387(5) 0.113(4) Uani 0.503(9) 1 d PD B 2 F8B F 0.3558(15) 0.6956(12) 0.1228(10) 0.144(5) Uani 0.503(9) 1 d PD B 2 F9B F 0.4331(8) 0.7589(7) -0.0577(5) 0.073(2) Uani 0.503(9) 1 d PD B 2 F10B F 0.3327(10) 0.8741(7) 0.0652(8) 0.111(3) Uani 0.503(9) 1 d PD B 2 F11B F 0.1245(10) 0.7522(10) 0.1325(5) 0.093(3) Uani 0.503(9) 1 d PD B 2 F12B F 0.2320(7) 0.6426(8) 0.0073(8) 0.115(5) Uani 0.503(9) 1 d PD 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 Ru 0.02219(10) 0.02122(10) 0.01819(9) -0.00100(6) -0.00205(6) -0.00649(6) N1A 0.0203(19) 0.017(3) 0.0202(16) 0.0018(17) -0.0039(15) -0.009(2) C1A 0.0245(17) 0.0224(17) 0.0242(17) 0.0015(14) -0.0036(14) -0.0055(14) C2A 0.0266(16) 0.0280(17) 0.0268(17) -0.0045(13) -0.0003(13) -0.0045(13) C3A 0.0297(19) 0.028(2) 0.0203(17) -0.0054(14) 0.0005(15) -0.0074(16) C4A 0.025(4) 0.029(4) 0.0199(17) -0.0041(17) -0.0036(18) -0.003(2) C5A 0.020(2) 0.019(3) 0.0217(16) -0.0034(15) -0.0028(15) -0.0073(17) N2A 0.024(3) 0.021(3) 0.0212(16) -0.0033(13) -0.0064(18) -0.0058(19) C6A 0.016(4) 0.021(2) 0.022(3) -0.0032(16) 0.003(3) -0.0057(17) C7A 0.024(4) 0.025(3) 0.027(2) -0.0021(16) -0.008(2) -0.0050(18) C8A 0.023(2) 0.022(2) 0.036(2) -0.0026(18) -0.0087(17) -0.0024(17) N3A 0.0229(14) 0.0234(14) 0.0291(18) -0.0045(12) -0.0054(13) -0.0045(11) C9A 0.0333(19) 0.0278(18) 0.0360(19) -0.0104(15) -0.0039(15) -0.0008(14) N1B 0.004(6) 0.028(4) 0.016(2) -0.003(2) 0.004(5) -0.002(3) C1B 0.021(4) 0.021(2) 0.015(3) -0.002(2) 0.000(3) -0.006(2) C2B 0.022(4) 0.021(3) 0.026(3) 0.000(2) -0.003(3) -0.007(2) C3B 0.018(4) 0.024(4) 0.028(3) 0.002(3) -0.010(3) -0.003(3) C4B 0.014(7) 0.031(7) 0.023(3) 0.000(2) -0.005(5) -0.002(5) C5B 0.020(6) 0.017(6) 0.018(2) -0.0031(19) -0.003(4) -0.006(4) N2B 0.023(6) 0.021(6) 0.0175(13) -0.006(2) -0.004(3) -0.005(3) C6B 0.019(6) 0.015(8) 0.0185(17) 0.000(4) 0.005(4) -0.008(5) C7B 0.018(7) 0.037(9) 0.0180(15) -0.008(3) 0.001(3) -0.003(5) C8B 0.023(5) 0.030(6) 0.0237(17) -0.011(3) 0.003(3) -0.005(3) N3B 0.016(3) 0.020(3) 0.0257(18) -0.005(2) 0.004(2) -0.007(2) C9B 0.026(4) 0.023(4) 0.038(4) -0.005(3) 0.003(3) 0.000(3) N4 0.0374(11) 0.0291(11) 0.0237(10) -0.0030(8) -0.0025(9) -0.0057(9) C10 0.070(2) 0.0318(14) 0.0242(13) -0.0002(11) -0.0033(13) 0.0014(13) C11 0.157(5) 0.046(2) 0.0267(16) -0.0099(14) 0.003(2) 0.023(2) N5 0.0277(10) 0.0242(9) 0.0184(9) -0.0013(7) -0.0064(7) -0.0049(8) C12 0.0302(12) 0.0266(11) 0.0212(10) -0.0006(9) -0.0076(9) -0.0060(9) C13 0.0303(13) 0.0426(15) 0.0375(14) -0.0004(11) -0.0102(11) -0.0154(11) N6 0.0289(10) 0.0265(10) 0.0295(10) 0.0020(8) -0.0048(8) -0.0073(8) C14 0.0298(12) 0.0309(13) 0.0290(12) 0.0016(10) -0.0020(10) -0.0074(10) C15 0.0388(15) 0.0372(15) 0.0377(15) 0.0119(12) -0.0038(12) -0.0001(12) N7 0.0246(10) 0.0235(10) 0.0257(10) -0.0029(8) -0.0012(8) -0.0043(8) C16 0.0284(12) 0.0306(13) 0.0346(13) -0.0095(10) 0.0012(10) -0.0073(10) C17 0.0287(14) 0.0524(18) 0.071(2) -0.0280(17) 0.0033(14) -0.0179(13) P1 0.0335(4) 0.0708(6) 0.0297(3) 0.0000(3) -0.0089(3) -0.0218(4) F1 0.0571(10) 0.0437(9) 0.0336(8) -0.0052(7) -0.0190(8) -0.0106(8) F2 0.0587(14) 0.205(3) 0.0518(13) 0.0134(17) -0.0336(11) -0.0385(18) F3 0.0428(11) 0.114(2) 0.0575(12) -0.0281(13) 0.0037(9) -0.0368(12) F4 0.0940(19) 0.0670(16) 0.174(3) 0.0487(18) -0.095(2) -0.0395(14) F5 0.0398(12) 0.289(5) 0.0371(12) -0.0034(18) -0.0051(9) -0.0453(19) F6 0.123(2) 0.0873(19) 0.141(3) -0.0712(19) -0.075(2) 0.0054(17) P2A 0.0491(15) 0.0324(15) 0.0229(14) -0.0049(10) -0.0053(10) -0.0080(10) F7A 0.078(6) 0.170(9) 0.169(10) -0.133(8) -0.057(6) 0.061(6) F8A 0.049(3) 0.209(11) 0.124(8) -0.124(8) -0.001(4) -0.001(6) F9A 0.240(10) 0.050(3) 0.128(6) 0.018(3) -0.127(7) -0.047(4) F10A 0.072(3) 0.078(4) 0.036(2) -0.014(3) -0.020(2) -0.014(3) F11A 0.350(15) 0.044(4) 0.155(8) 0.048(5) -0.168(10) -0.074(6) F12A 0.100(4) 0.080(5) 0.041(2) -0.009(2) -0.039(3) 0.001(3) P2B 0.060(2) 0.064(4) 0.0292(15) 0.003(2) -0.0096(14) -0.021(2) F7B 0.081(4) 0.191(10) 0.059(3) 0.029(4) -0.021(3) 0.005(5) F8B 0.126(7) 0.160(12) 0.148(10) 0.097(8) -0.072(7) -0.014(8) F9B 0.053(4) 0.095(5) 0.053(3) 0.003(3) 0.010(2) -0.024(3) F10B 0.130(6) 0.085(5) 0.127(7) -0.017(5) -0.043(5) -0.048(4) F11B 0.072(5) 0.176(9) 0.017(2) 0.008(3) 0.012(2) -0.040(5) F12B 0.058(3) 0.120(7) 0.151(9) -0.093(7) 0.021(4) -0.037(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C6A 1.990(7) . ? Ru N7 2.021(2) . ? Ru N5 2.0250(19) . ? Ru N1A 2.043(5) . ? Ru N1B 2.049(15) . ? Ru N4 2.061(2) . ? Ru C6B 2.067(15) . ? Ru N6 2.095(2) . ? N1A C1A 1.348(5) . ? N1A C5A 1.358(5) . ? C1A C2A 1.370(5) . ? C1A H1A 0.9500 . ? C2A C3A 1.376(5) . ? C2A H2A 0.9500 . ? C3A C4A 1.372(6) . ? C3A H3A 0.9500 . ? C4A C5A 1.388(5) . ? C4A H4A 0.9500 . ? C5A N2A 1.391(5) . ? N2A C6A 1.373(6) . ? N2A C7A 1.389(5) . ? C6A N3A 1.354(6) . ? C7A C8A 1.335(5) . ? C7A H7A 0.9500 . ? C8A N3A 1.407(5) . ? C8A H8A 0.9500 . ? N3A C9A 1.461(5) . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? N1B C1B 1.342(13) . ? N1B C5B 1.344(13) . ? C1B C2B 1.367(10) . ? C1B H1B 0.9500 . ? C2B C3B 1.361(11) . ? C2B H2B 0.9500 . ? C3B C4B 1.368(12) . ? C3B H3B 0.9500 . ? C4B C5B 1.395(13) . ? C4B H4B 0.9500 . ? C5B N2B 1.371(11) . ? N2B C6B 1.357(14) . ? N2B C7B 1.396(12) . ? C6B N3B 1.342(14) . ? C7B C8B 1.314(12) . ? C7B H7B 0.9500 . ? C8B N3B 1.410(11) . ? C8B H8B 0.9500 . ? N3B C9B 1.450(10) . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? N4 C10 1.128(3) . ? C10 C11 1.463(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N5 C12 1.136(3) . ? C12 C13 1.458(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? N6 C14 1.131(3) . ? C14 C15 1.462(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N7 C16 1.137(3) . ? C16 C17 1.462(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? P1 F6 1.565(3) . ? P1 F3 1.582(2) . ? P1 F5 1.584(2) . ? P1 F2 1.588(2) . ? P1 F1 1.5890(18) . ? P1 F4 1.599(3) . ? P2A F11A 1.544(8) . ? P2A F9A 1.544(8) . ? P2A F10A 1.557(8) . ? P2A F8A 1.564(8) . ? P2A F7A 1.575(9) . ? P2A F12A 1.581(8) . ? P2B F8B 1.542(10) . ? P2B F9B 1.546(9) . ? P2B F11B 1.572(8) . ? P2B F12B 1.579(8) . ? P2B F10B 1.583(8) . ? P2B F7B 1.598(9) . ? 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 C6A Ru N7 89.5(5) . . ? C6A Ru N5 92.8(5) . . ? N7 Ru N5 177.64(8) . . ? C6A Ru N1A 78.70(15) . . ? N7 Ru N1A 89.5(4) . . ? N5 Ru N1A 90.5(4) . . ? N7 Ru N1B 88.2(10) . . ? N5 Ru N1B 94.2(10) . . ? C6A Ru N4 99.03(14) . . ? N7 Ru N4 89.68(8) . . ? N5 Ru N4 90.35(8) . . ? N1A Ru N4 177.60(16) . . ? N1B Ru N4 91.1(3) . . ? N7 Ru C6B 91.6(12) . . ? N5 Ru C6B 88.8(12) . . ? N1B Ru C6B 77.9(4) . . ? N4 Ru C6B 168.9(4) . . ? C6A Ru N6 171.75(14) . . ? N7 Ru N6 89.91(8) . . ? N5 Ru N6 87.74(8) . . ? N1A Ru N6 93.07(11) . . ? N1B Ru N6 178.1(10) . . ? N4 Ru N6 89.20(9) . . ? C6B Ru N6 101.9(4) . . ? C1A N1A C5A 117.4(4) . . ? C1A N1A Ru 126.5(3) . . ? C5A N1A Ru 116.0(3) . . ? N1A C1A C2A 122.6(4) . . ? N1A C1A H1A 118.7 . . ? C2A C1A H1A 118.7 . . ? C1A C2A C3A 119.4(4) . . ? C1A C2A H2A 120.3 . . ? C3A C2A H2A 120.3 . . ? C4A C3A C2A 119.6(4) . . ? C4A C3A H3A 120.2 . . ? C2A C3A H3A 120.2 . . ? C3A C4A C5A 118.3(4) . . ? C3A C4A H4A 120.8 . . ? C5A C4A H4A 120.8 . . ? N1A C5A C4A 122.6(4) . . ? N1A C5A N2A 112.7(3) . . ? C4A C5A N2A 124.7(4) . . ? C6A N2A C7A 111.6(4) . . ? C6A N2A C5A 117.8(4) . . ? C7A N2A C5A 130.4(3) . . ? N3A C6A N2A 103.9(5) . . ? N3A C6A Ru 141.4(4) . . ? N2A C6A Ru 114.4(3) . . ? C8A C7A N2A 106.4(4) . . ? C8A C7A H7A 126.8 . . ? N2A C7A H7A 126.8 . . ? C7A C8A N3A 107.4(4) . . ? C7A C8A H8A 126.3 . . ? N3A C8A H8A 126.3 . . ? C6A N3A C8A 110.7(4) . . ? C6A N3A C9A 125.3(4) . . ? C8A N3A C9A 124.0(3) . . ? C1B N1B C5B 118.5(12) . . ? C1B N1B Ru 125.3(10) . . ? C5B N1B Ru 115.8(8) . . ? N1B C1B C2B 122.2(10) . . ? N1B C1B H1B 118.9 . . ? C2B C1B H1B 118.9 . . ? C3B C2B C1B 119.2(8) . . ? C3B C2B H2B 120.4 . . ? C1B C2B H2B 120.4 . . ? C2B C3B C4B 119.8(9) . . ? C2B C3B H3B 120.1 . . ? C4B C3B H3B 120.1 . . ? C3B C4B C5B 118.7(10) . . ? C3B C4B H4B 120.7 . . ? C5B C4B H4B 120.7 . . ? N1B C5B N2B 114.7(10) . . ? N1B C5B C4B 121.0(10) . . ? N2B C5B C4B 124.3(10) . . ? C6B N2B C5B 118.7(10) . . ? C6B N2B C7B 110.1(10) . . ? C5B N2B C7B 130.9(10) . . ? N3B C6B N2B 106.0(12) . . ? N3B C6B Ru 141.5(10) . . ? N2B C6B Ru 112.4(8) . . ? C8B C7B N2B 106.7(10) . . ? C8B C7B H7B 126.6 . . ? N2B C7B H7B 126.6 . . ? C7B C8B N3B 108.1(10) . . ? C7B C8B H8B 125.9 . . ? N3B C8B H8B 125.9 . . ? C6B N3B C8B 109.0(9) . . ? C6B N3B C9B 126.8(9) . . ? C8B N3B C9B 124.0(8) . . ? N3B C9B H9B1 109.5 . . ? N3B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? N3B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C10 N4 Ru 178.5(3) . . ? N4 C10 C11 179.3(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 N5 Ru 173.8(2) . . ? N5 C12 C13 179.5(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C14 N6 Ru 178.6(2) . . ? N6 C14 C15 179.8(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C16 N7 Ru 179.4(2) . . ? N7 C16 C17 178.9(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? F6 P1 F3 91.60(17) . . ? F6 P1 F5 91.6(2) . . ? F3 P1 F5 176.7(2) . . ? F6 P1 F2 88.37(18) . . ? F3 P1 F2 89.52(13) . . ? F5 P1 F2 90.31(13) . . ? F6 P1 F1 91.12(13) . . ? F3 P1 F1 91.02(12) . . ? F5 P1 F1 89.19(11) . . ? F2 P1 F1 179.27(16) . . ? F6 P1 F4 179.1(2) . . ? F3 P1 F4 87.77(16) . . ? F5 P1 F4 89.0(2) . . ? F2 P1 F4 92.21(18) . . ? F1 P1 F4 88.31(12) . . ? F11A P2A F9A 179.8(8) . . ? F11A P2A F10A 89.3(6) . . ? F9A P2A F10A 90.9(5) . . ? F11A P2A F8A 94.4(8) . . ? F9A P2A F8A 85.9(7) . . ? F10A P2A F8A 86.8(6) . . ? F11A P2A F7A 83.5(8) . . ? F9A P2A F7A 96.3(8) . . ? F10A P2A F7A 90.8(7) . . ? F8A P2A F7A 176.8(7) . . ? F11A P2A F12A 91.9(6) . . ? F9A P2A F12A 88.0(5) . . ? F10A P2A F12A 178.4(6) . . ? F8A P2A F12A 92.0(5) . . ? F7A P2A F12A 90.4(6) . . ? F8B P2B F9B 95.7(7) . . ? F8B P2B F11B 87.0(8) . . ? F9B P2B F11B 176.4(8) . . ? F8B P2B F12B 94.1(8) . . ? F9B P2B F12B 93.2(5) . . ? F11B P2B F12B 84.2(6) . . ? F8B P2B F10B 88.7(7) . . ? F9B P2B F10B 85.5(6) . . ? F11B P2B F10B 97.0(7) . . ? F12B P2B F10B 177.0(8) . . ? F8B P2B F7B 174.6(9) . . ? F9B P2B F7B 88.4(5) . . ? F11B P2B F7B 89.1(5) . . ? F12B P2B F7B 89.2(7) . . ? F10B P2B F7B 88.0(6) . . ? 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 C6A Ru N1A C1A 174.5(12) . . . . ? N7 Ru N1A C1A -95.9(10) . . . . ? N5 Ru N1A C1A 81.8(10) . . . . ? N1B Ru N1A C1A 175.9(15) . . . . ? C6B Ru N1A C1A 161(11) . . . . ? N6 Ru N1A C1A -6.0(11) . . . . ? C6A Ru N1A C5A -3.5(10) . . . . ? N7 Ru N1A C5A 86.1(9) . . . . ? N5 Ru N1A C5A -96.2(9) . . . . ? N1B Ru N1A C5A -2.1(14) . . . . ? C6B Ru N1A C5A -17(9) . . . . ? N6 Ru N1A C5A 176.0(9) . . . . ? C5A N1A C1A C2A -1.7(14) . . . . ? Ru N1A C1A C2A -179.7(6) . . . . ? N1A C1A C2A C3A 0.9(9) . . . . ? C1A C2A C3A C4A 0.7(7) . . . . ? C2A C3A C4A C5A -1.5(10) . . . . ? C1A N1A C5A C4A 0.9(16) . . . . ? Ru N1A C5A C4A 179.1(7) . . . . ? C1A N1A C5A N2A -177.4(8) . . . . ? Ru N1A C5A N2A 0.8(11) . . . . ? C3A C4A C5A N1A 0.7(13) . . . . ? C3A C4A C5A N2A 178.7(6) . . . . ? N1A C5A N2A C6A 4.0(13) . . . . ? C4A C5A N2A C6A -174.2(11) . . . . ? N1A C5A N2A C7A 178.6(10) . . . . ? C4A C5A N2A C7A 0.4(12) . . . . ? C7A N2A C6A N3A 2.9(14) . . . . ? C5A N2A C6A N3A 178.4(7) . . . . ? C7A N2A C6A Ru 177.5(8) . . . . ? C5A N2A C6A Ru -7.0(14) . . . . ? N7 Ru C6A N3A 87.4(19) . . . . ? N5 Ru C6A N3A -93.0(19) . . . . ? N1A Ru C6A N3A 177(2) . . . . ? N1B Ru C6A N3A 7(9) . . . . ? N4 Ru C6A N3A -2(2) . . . . ? C6B Ru C6A N3A 179(2) . . . . ? N7 Ru C6A N2A -84.2(11) . . . . ? N5 Ru C6A N2A 95.4(11) . . . . ? N1A Ru C6A N2A 5.5(11) . . . . ? N1B Ru C6A N2A -164(12) . . . . ? N4 Ru C6A N2A -173.8(10) . . . . ? C6B Ru C6A N2A 7.7(16) . . . . ? C6A N2A C7A C8A -2.1(12) . . . . ? C5A N2A C7A C8A -176.9(6) . . . . ? N2A C7A C8A N3A 0.5(9) . . . . ? N2A C6A N3A C8A -2.6(13) . . . . ? Ru C6A N3A C8A -174.6(15) . . . . ? N2A C6A N3A C9A 179.5(6) . . . . ? Ru C6A N3A C9A 7(2) . . . . ? C7A C8A N3A C6A 1.4(10) . . . . ? C7A C8A N3A C9A 179.4(5) . . . . ? C6A Ru N1B C1B -162(13) . . . . ? N7 Ru N1B C1B 98(3) . . . . ? N5 Ru N1B C1B -82(3) . . . . ? N1A Ru N1B C1B -172(3) . . . . ? N4 Ru N1B C1B 8(3) . . . . ? C6B Ru N1B C1B -170(3) . . . . ? C6A Ru N1B C5B 10(9) . . . . ? N7 Ru N1B C5B -89(2) . . . . ? N5 Ru N1B C5B 91(2) . . . . ? N1A Ru N1B C5B 0(2) . . . . ? N4 Ru N1B C5B -179(2) . . . . ? C6B Ru N1B C5B 3(3) . . . . ? C5B N1B C1B C2B 7(4) . . . . ? Ru N1B C1B C2B 180.0(14) . . . . ? N1B C1B C2B C3B -2(2) . . . . ? C1B C2B C3B C4B -1.6(17) . . . . ? C2B C3B C4B C5B 0(3) . . . . ? C1B N1B C5B N2B 174(2) . . . . ? Ru N1B C5B N2B 0(3) . . . . ? C1B N1B C5B C4B -9(4) . . . . ? Ru N1B C5B C4B 177.3(19) . . . . ? C3B C4B C5B N1B 6(4) . . . . ? C3B C4B C5B N2B -177.3(16) . . . . ? N1B C5B N2B C6B -5(3) . . . . ? C4B C5B N2B C6B 178(3) . . . . ? N1B C5B N2B C7B -178(3) . . . . ? C4B C5B N2B C7B 5(3) . . . . ? C5B N2B C6B N3B -176.1(19) . . . . ? C7B N2B C6B N3B -2(3) . . . . ? C5B N2B C6B Ru 7(3) . . . . ? C7B N2B C6B Ru -178.0(18) . . . . ? C6A Ru C6B N3B 179(5) . . . . ? N7 Ru C6B N3B -92(5) . . . . ? N5 Ru C6B N3B 86(5) . . . . ? N1A Ru C6B N3B -15(5) . . . . ? N1B Ru C6B N3B -180(5) . . . . ? N4 Ru C6B N3B 171.7(17) . . . . ? N6 Ru C6B N3B -2(5) . . . . ? C6A Ru C6B N2B -6(2) . . . . ? N7 Ru C6B N2B 83(3) . . . . ? N5 Ru C6B N2B -100(3) . . . . ? N1A Ru C6B N2B 160(12) . . . . ? N1B Ru C6B N2B -5(3) . . . . ? N4 Ru C6B N2B -14(9) . . . . ? N6 Ru C6B N2B 173(2) . . . . ? C6B N2B C7B C8B -1(3) . . . . ? C5B N2B C7B C8B 173.0(16) . . . . ? N2B C7B C8B N3B 3(2) . . . . ? N2B C6B N3B C8B 3(3) . . . . ? Ru C6B N3B C8B 178(4) . . . . ? N2B C6B N3B C9B 178.1(14) . . . . ? Ru C6B N3B C9B -7(6) . . . . ? C7B C8B N3B C6B -4(2) . . . . ? C7B C8B N3B C9B -178.8(13) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.780 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.074 #===END data_alb76(2a) _database_code_depnum_ccdc_archive 'CCDC 817671' #TrackingRef 'alb09pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H24 Cl N4 Ru, C F3 O3 S' _chemical_formula_sum 'C20 H24 Cl F3 N4 O3 Ru S' _chemical_formula_weight 594.01 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' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0688(2) _cell_length_b 9.8428(2) _cell_length_c 13.7787(3) _cell_angle_alpha 85.827(2) _cell_angle_beta 84.744(2) _cell_angle_gamma 70.410(2) _cell_volume 1152.70(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21265 _cell_measurement_theta_min 3.6106 _cell_measurement_theta_max 37.7445 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2190 _exptl_crystal_size_mid 0.1486 _exptl_crystal_size_min 0.1165 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 0.941 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41596 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 37.83 _reflns_number_total 11813 _reflns_number_gt 10305 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^)+(0.0245P)^2^+0.5432P] 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 11813 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.003 _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 Ru Ru 0.525805(11) 0.758802(10) 0.731576(6) 0.01064(2) Uani 1 1 d . . . Cl Cl 0.65350(4) 0.77619(4) 0.57269(2) 0.01960(6) Uani 1 1 d . . . C1 C 0.33810(14) 0.77445(13) 0.65610(8) 0.01283(19) Uani 1 1 d . . . N1 N 0.21166(12) 0.87445(12) 0.61766(8) 0.01418(18) Uani 1 1 d . . . C2 C 0.16436(17) 1.03145(14) 0.62058(11) 0.0202(2) Uani 1 1 d . . . H2A H 0.0865 1.0761 0.5728 0.030 Uiso 1 1 calc R . . H2B H 0.2563 1.0622 0.6049 0.030 Uiso 1 1 calc R . . H2C H 0.1185 1.0614 0.6860 0.030 Uiso 1 1 calc R . . N2 N 0.12523(13) 0.81818(12) 0.56950(8) 0.01567(18) Uani 1 1 d . . . N3 N 0.19890(12) 0.67725(12) 0.57653(8) 0.01418(18) Uani 1 1 d . . . C3 C 0.13004(17) 0.58133(16) 0.53476(10) 0.0195(2) Uani 1 1 d . . . H3A H 0.0263 0.6379 0.5131 0.029 Uiso 1 1 calc R . . H3B H 0.1196 0.5079 0.5843 0.029 Uiso 1 1 calc R . . H3C H 0.1982 0.5342 0.4790 0.029 Uiso 1 1 calc R . . C4 C 0.32918(14) 0.64552(13) 0.62666(8) 0.01305(19) Uani 1 1 d . . . C5 C 0.45765(14) 0.51374(13) 0.64495(8) 0.01306(19) Uani 1 1 d . . . C6 C 0.48289(16) 0.37808(14) 0.61048(9) 0.0163(2) Uani 1 1 d . . . H6 H 0.4089 0.3618 0.5723 0.020 Uiso 1 1 calc R . . C7 C 0.61864(17) 0.26659(14) 0.63301(10) 0.0187(2) Uani 1 1 d . . . H7 H 0.6395 0.1730 0.6096 0.022 Uiso 1 1 calc R . . C8 C 0.72334(17) 0.29350(14) 0.69001(10) 0.0189(2) Uani 1 1 d . . . H8 H 0.8152 0.2179 0.7077 0.023 Uiso 1 1 calc R . . C9 C 0.69249(15) 0.43218(14) 0.72093(9) 0.0161(2) Uani 1 1 d . . . H9 H 0.7655 0.4503 0.7591 0.019 Uiso 1 1 calc R . . N4 N 0.56265(12) 0.54165(11) 0.69867(8) 0.01324(17) Uani 1 1 d . . . C10 C 0.41889(14) 0.79878(14) 0.88396(8) 0.01373(19) Uani 1 1 d . . . C16 C 0.28437(15) 0.76816(15) 0.94418(9) 0.0176(2) Uani 1 1 d . . . H16 H 0.3183 0.6624 0.9618 0.021 Uiso 1 1 calc R . . C17 C 0.13384(18) 0.8069(2) 0.89218(12) 0.0275(3) Uani 1 1 d . . . H17A H 0.0969 0.9107 0.8751 0.041 Uiso 1 1 calc R . . H17B H 0.0535 0.7822 0.9353 0.041 Uiso 1 1 calc R . . H17C H 0.1541 0.7529 0.8326 0.041 Uiso 1 1 calc R . . C18 C 0.2565(2) 0.8489(2) 1.03923(11) 0.0288(3) Uani 1 1 d . . . H18A H 0.3541 0.8196 1.0725 0.043 Uiso 1 1 calc R . . H18B H 0.1748 0.8254 1.0818 0.043 Uiso 1 1 calc R . . H18C H 0.2228 0.9531 1.0240 0.043 Uiso 1 1 calc R . . C11 C 0.40019(14) 0.93186(13) 0.82980(9) 0.01378(19) Uani 1 1 d . . . H11 H 0.2980 1.0005 0.8256 0.017 Uiso 1 1 calc R . . C12 C 0.53007(15) 0.96390(13) 0.78231(9) 0.0143(2) Uani 1 1 d . . . H12 H 0.5142 1.0526 0.7457 0.017 Uiso 1 1 calc R . . C13 C 0.68591(14) 0.86328(14) 0.78900(9) 0.0142(2) Uani 1 1 d . . . C19 C 0.82434(15) 0.89475(16) 0.73736(10) 0.0186(2) Uani 1 1 d . . . H19A H 0.8504 0.9649 0.7734 0.028 Uiso 1 1 calc R . . H19B H 0.7989 0.9346 0.6714 0.028 Uiso 1 1 calc R . . H19C H 0.9143 0.8054 0.7335 0.028 Uiso 1 1 calc R . . C14 C 0.70661(14) 0.73027(14) 0.84039(9) 0.0145(2) Uani 1 1 d . . . H14 H 0.8090 0.6626 0.8462 0.017 Uiso 1 1 calc R . . C15 C 0.57312(15) 0.69770(14) 0.88368(9) 0.0144(2) Uani 1 1 d . . . H15 H 0.5879 0.6045 0.9136 0.017 Uiso 1 1 calc R . . O1 O 0.24053(14) 0.27142(13) 0.71779(8) 0.0265(2) Uani 1 1 d . . . O2 O 0.05023(18) 0.50131(15) 0.76219(9) 0.0428(4) Uani 1 1 d . . . O3 O 0.02197(18) 0.2760(2) 0.83257(11) 0.0550(5) Uani 1 1 d . . . S S 0.12417(4) 0.35174(4) 0.78942(2) 0.02076(7) Uani 1 1 d . . . C20 C 0.24060(17) 0.35797(15) 0.88977(10) 0.0201(2) Uani 1 1 d . . . F1 F 0.31100(14) 0.22596(11) 0.92756(8) 0.0364(3) Uani 1 1 d . . . F2 F 0.15405(14) 0.43730(13) 0.96139(7) 0.0381(3) Uani 1 1 d . . . F3 F 0.35231(14) 0.41485(14) 0.85916(8) 0.0404(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01015(4) 0.01221(4) 0.00940(4) -0.00106(3) -0.00201(3) -0.00304(3) Cl 0.02420(15) 0.02705(15) 0.01176(12) -0.00327(10) 0.00179(10) -0.01435(12) C1 0.0117(4) 0.0147(5) 0.0117(4) -0.0010(4) -0.0023(4) -0.0033(4) N1 0.0124(4) 0.0155(4) 0.0140(4) -0.0020(3) -0.0036(3) -0.0029(3) C2 0.0196(6) 0.0154(5) 0.0236(6) -0.0017(4) -0.0081(5) -0.0014(4) N2 0.0131(4) 0.0198(5) 0.0145(4) -0.0023(4) -0.0033(3) -0.0050(4) N3 0.0136(4) 0.0177(5) 0.0127(4) -0.0016(3) -0.0025(3) -0.0065(4) C3 0.0217(6) 0.0246(6) 0.0175(5) -0.0020(5) -0.0051(5) -0.0137(5) C4 0.0123(4) 0.0161(5) 0.0113(4) -0.0015(4) -0.0017(4) -0.0051(4) C5 0.0148(5) 0.0149(5) 0.0104(4) -0.0004(4) -0.0006(4) -0.0062(4) C6 0.0215(6) 0.0160(5) 0.0138(5) -0.0011(4) -0.0010(4) -0.0090(4) C7 0.0247(6) 0.0133(5) 0.0172(5) -0.0011(4) 0.0023(5) -0.0061(5) C8 0.0198(6) 0.0142(5) 0.0197(6) 0.0001(4) 0.0004(5) -0.0021(4) C9 0.0147(5) 0.0151(5) 0.0164(5) -0.0001(4) -0.0023(4) -0.0022(4) N4 0.0132(4) 0.0134(4) 0.0128(4) -0.0004(3) -0.0011(3) -0.0040(3) C10 0.0134(5) 0.0176(5) 0.0105(4) -0.0028(4) -0.0011(4) -0.0049(4) C16 0.0156(5) 0.0233(6) 0.0152(5) -0.0024(4) 0.0013(4) -0.0084(5) C17 0.0169(6) 0.0441(9) 0.0243(7) -0.0010(6) -0.0014(5) -0.0138(6) C18 0.0263(7) 0.0461(10) 0.0186(6) -0.0096(6) 0.0071(5) -0.0184(7) C11 0.0129(5) 0.0146(5) 0.0132(5) -0.0037(4) -0.0017(4) -0.0030(4) C12 0.0146(5) 0.0146(5) 0.0141(5) -0.0027(4) -0.0017(4) -0.0047(4) C13 0.0131(5) 0.0179(5) 0.0130(5) -0.0030(4) -0.0024(4) -0.0061(4) C19 0.0145(5) 0.0241(6) 0.0190(6) -0.0019(5) -0.0003(4) -0.0088(5) C14 0.0127(5) 0.0180(5) 0.0124(5) -0.0013(4) -0.0039(4) -0.0036(4) C15 0.0153(5) 0.0171(5) 0.0101(4) -0.0002(4) -0.0033(4) -0.0037(4) O1 0.0301(6) 0.0261(5) 0.0242(5) -0.0079(4) -0.0038(4) -0.0087(4) O2 0.0472(8) 0.0347(7) 0.0244(6) 0.0010(5) -0.0080(5) 0.0164(6) O3 0.0423(8) 0.1095(15) 0.0330(7) 0.0231(8) -0.0099(6) -0.0547(9) S 0.01397(13) 0.03152(18) 0.01642(14) 0.00565(12) -0.00282(11) -0.00798(12) C20 0.0190(6) 0.0200(6) 0.0189(6) -0.0040(4) -0.0017(5) -0.0027(5) F1 0.0480(6) 0.0225(5) 0.0335(5) -0.0019(4) -0.0249(5) 0.0010(4) F2 0.0400(6) 0.0410(6) 0.0181(4) -0.0079(4) 0.0017(4) 0.0070(5) F3 0.0416(6) 0.0597(8) 0.0348(6) -0.0134(5) -0.0004(5) -0.0348(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C1 2.0318(12) . ? Ru N4 2.1260(11) . ? Ru C15 2.1786(12) . ? Ru C11 2.1869(12) . ? Ru C12 2.1973(12) . ? Ru C10 2.2349(12) . ? Ru C14 2.2573(12) . ? Ru C13 2.2631(12) . ? Ru Cl 2.4036(3) . ? C1 N1 1.3575(15) . ? C1 C4 1.3898(17) . ? N1 N2 1.3421(15) . ? N1 C2 1.4612(17) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? N2 N3 1.3231(16) . ? N3 C4 1.3568(15) . ? N3 C3 1.4673(16) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.4479(17) . ? C5 N4 1.3654(16) . ? C5 C6 1.3886(18) . ? C6 C7 1.3895(19) . ? C6 H6 0.9500 . ? C7 C8 1.387(2) . ? C7 H7 0.9500 . ? C8 C9 1.3892(19) . ? C8 H8 0.9500 . ? C9 N4 1.3449(16) . ? C9 H9 0.9500 . ? C10 C15 1.4187(17) . ? C10 C11 1.4260(17) . ? C10 C16 1.5141(18) . ? C16 C17 1.521(2) . ? C16 C18 1.538(2) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C11 C12 1.4117(18) . ? C11 H11 0.9500 . ? C12 C13 1.4348(18) . ? C12 H12 0.9500 . ? C13 C14 1.4053(18) . ? C13 C19 1.4978(18) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C14 C15 1.4228(18) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? O1 S 1.4408(12) . ? O2 S 1.4358(13) . ? O3 S 1.4377(14) . ? S C20 1.8313(14) . ? C20 F2 1.3261(17) . ? C20 F1 1.3316(17) . ? C20 F3 1.3361(18) . ? 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 C1 Ru N4 76.53(4) . . ? C1 Ru C15 131.55(5) . . ? N4 Ru C15 91.93(4) . . ? C1 Ru C11 95.86(5) . . ? N4 Ru C11 144.94(4) . . ? C15 Ru C11 67.37(5) . . ? C1 Ru C12 115.04(5) . . ? N4 Ru C12 168.39(4) . . ? C15 Ru C12 79.62(5) . . ? C11 Ru C12 37.57(5) . . ? C1 Ru C10 102.57(5) . . ? N4 Ru C10 109.85(4) . . ? C15 Ru C10 37.47(5) . . ? C11 Ru C10 37.61(5) . . ? C12 Ru C10 67.91(5) . . ? C1 Ru C14 168.90(5) . . ? N4 Ru C14 101.84(4) . . ? C15 Ru C14 37.36(5) . . ? C11 Ru C14 79.12(4) . . ? C12 Ru C14 66.64(5) . . ? C10 Ru C14 67.42(4) . . ? C1 Ru C13 149.91(5) . . ? N4 Ru C13 131.53(4) . . ? C15 Ru C13 66.70(5) . . ? C11 Ru C13 67.40(5) . . ? C12 Ru C13 37.49(5) . . ? C10 Ru C13 79.70(4) . . ? C14 Ru C13 36.23(5) . . ? C1 Ru Cl 84.27(3) . . ? N4 Ru Cl 85.26(3) . . ? C15 Ru Cl 142.33(3) . . ? C11 Ru Cl 128.57(3) . . ? C12 Ru Cl 96.53(3) . . ? C10 Ru Cl 164.42(3) . . ? C14 Ru Cl 106.63(3) . . ? C13 Ru Cl 87.40(3) . . ? N1 C1 C4 102.67(10) . . ? N1 C1 Ru 141.04(9) . . ? C4 C1 Ru 116.20(8) . . ? N2 N1 C1 113.99(10) . . ? N2 N1 C2 118.17(10) . . ? C1 N1 C2 127.81(11) . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N3 N2 N1 104.23(10) . . ? N2 N3 C4 111.25(10) . . ? N2 N3 C3 118.50(10) . . ? C4 N3 C3 130.21(11) . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 C1 107.83(11) . . ? N3 C4 C5 133.41(11) . . ? C1 C4 C5 118.46(10) . . ? N4 C5 C6 122.30(11) . . ? N4 C5 C4 109.78(10) . . ? C6 C5 C4 127.81(11) . . ? C5 C6 C7 118.64(12) . . ? C5 C6 H6 120.7 . . ? C7 C6 H6 120.7 . . ? C8 C7 C6 119.22(12) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 119.31(12) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? N4 C9 C8 122.16(12) . . ? N4 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 N4 C5 118.33(11) . . ? C9 N4 Ru 122.62(9) . . ? C5 N4 Ru 118.77(8) . . ? C15 C10 C11 116.69(11) . . ? C15 C10 C16 120.72(11) . . ? C11 C10 C16 122.49(11) . . ? C15 C10 Ru 69.11(7) . . ? C11 C10 Ru 69.37(7) . . ? C16 C10 Ru 135.49(9) . . ? C10 C16 C17 114.44(11) . . ? C10 C16 C18 107.75(11) . . ? C17 C16 C18 111.00(12) . . ? C10 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C18 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C11 C10 121.48(11) . . ? C12 C11 Ru 71.61(7) . . ? C10 C11 Ru 73.02(7) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? Ru C11 H11 128.4 . . ? C11 C12 C13 120.39(11) . . ? C11 C12 Ru 70.82(7) . . ? C13 C12 Ru 73.74(7) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? Ru C12 H12 127.7 . . ? C14 C13 C12 119.01(11) . . ? C14 C13 C19 119.99(11) . . ? C12 C13 C19 120.90(11) . . ? C14 C13 Ru 71.66(7) . . ? C12 C13 Ru 68.76(7) . . ? C19 C13 Ru 128.78(9) . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C13 C14 C15 119.49(11) . . ? C13 C14 Ru 72.11(7) . . ? C15 C14 Ru 68.32(7) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? Ru C14 H14 132.2 . . ? C10 C15 C14 122.66(11) . . ? C10 C15 Ru 73.42(7) . . ? C14 C15 Ru 74.32(7) . . ? C10 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? Ru C15 H15 125.4 . . ? O2 S O3 116.16(11) . . ? O2 S O1 114.63(8) . . ? O3 S O1 113.70(10) . . ? O2 S C20 103.28(8) . . ? O3 S C20 103.57(8) . . ? O1 S C20 103.21(7) . . ? F2 C20 F1 107.67(12) . . ? F2 C20 F3 107.00(13) . . ? F1 C20 F3 107.56(13) . . ? F2 C20 S 112.34(10) . . ? F1 C20 S 110.91(10) . . ? F3 C20 S 111.12(10) . . ? 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 Ru C1 N1 -174.42(15) . . . . ? C15 Ru C1 N1 105.14(15) . . . . ? C11 Ru C1 N1 40.34(15) . . . . ? C12 Ru C1 N1 6.60(16) . . . . ? C10 Ru C1 N1 77.87(15) . . . . ? C14 Ru C1 N1 102.8(3) . . . . ? C13 Ru C1 N1 -13.3(2) . . . . ? Cl Ru C1 N1 -87.94(14) . . . . ? N4 Ru C1 C4 1.55(9) . . . . ? C15 Ru C1 C4 -78.89(11) . . . . ? C11 Ru C1 C4 -143.69(9) . . . . ? C12 Ru C1 C4 -177.43(9) . . . . ? C10 Ru C1 C4 -106.16(10) . . . . ? C14 Ru C1 C4 -81.3(3) . . . . ? C13 Ru C1 C4 162.71(9) . . . . ? Cl Ru C1 C4 88.03(9) . . . . ? C4 C1 N1 N2 1.31(14) . . . . ? Ru C1 N1 N2 177.60(11) . . . . ? C4 C1 N1 C2 -176.68(12) . . . . ? Ru C1 N1 C2 -0.4(2) . . . . ? C1 N1 N2 N3 -0.41(14) . . . . ? C2 N1 N2 N3 177.78(11) . . . . ? N1 N2 N3 C4 -0.73(13) . . . . ? N1 N2 N3 C3 177.18(11) . . . . ? N2 N3 C4 C1 1.56(14) . . . . ? C3 N3 C4 C1 -176.03(12) . . . . ? N2 N3 C4 C5 -171.72(13) . . . . ? C3 N3 C4 C5 10.7(2) . . . . ? N1 C1 C4 N3 -1.66(13) . . . . ? Ru C1 C4 N3 -179.07(8) . . . . ? N1 C1 C4 C5 172.79(11) . . . . ? Ru C1 C4 C5 -4.61(15) . . . . ? N3 C4 C5 N4 178.46(13) . . . . ? C1 C4 C5 N4 5.74(16) . . . . ? N3 C4 C5 C6 2.2(2) . . . . ? C1 C4 C5 C6 -170.49(12) . . . . ? N4 C5 C6 C7 1.11(19) . . . . ? C4 C5 C6 C7 176.91(12) . . . . ? C5 C6 C7 C8 0.83(19) . . . . ? C6 C7 C8 C9 -1.9(2) . . . . ? C7 C8 C9 N4 1.0(2) . . . . ? C8 C9 N4 C5 0.87(19) . . . . ? C8 C9 N4 Ru -172.96(10) . . . . ? C6 C5 N4 C9 -1.96(18) . . . . ? C4 C5 N4 C9 -178.43(11) . . . . ? C6 C5 N4 Ru 172.11(9) . . . . ? C4 C5 N4 Ru -4.36(13) . . . . ? C1 Ru N4 C9 175.56(11) . . . . ? C15 Ru N4 C9 -52.04(10) . . . . ? C11 Ru N4 C9 -103.57(11) . . . . ? C12 Ru N4 C9 -9.0(3) . . . . ? C10 Ru N4 C9 -85.73(10) . . . . ? C14 Ru N4 C9 -15.70(11) . . . . ? C13 Ru N4 C9 8.04(12) . . . . ? Cl Ru N4 C9 90.33(10) . . . . ? C1 Ru N4 C5 1.75(9) . . . . ? C15 Ru N4 C5 134.16(9) . . . . ? C11 Ru N4 C5 82.63(11) . . . . ? C12 Ru N4 C5 177.16(19) . . . . ? C10 Ru N4 C5 100.47(9) . . . . ? C14 Ru N4 C5 170.50(9) . . . . ? C13 Ru N4 C5 -165.76(8) . . . . ? Cl Ru N4 C5 -83.48(9) . . . . ? C1 Ru C10 C15 145.70(7) . . . . ? N4 Ru C10 C15 65.67(8) . . . . ? C11 Ru C10 C15 -131.09(11) . . . . ? C12 Ru C10 C15 -102.12(8) . . . . ? C14 Ru C10 C15 -29.26(7) . . . . ? C13 Ru C10 C15 -64.93(8) . . . . ? Cl Ru C10 C15 -99.54(13) . . . . ? C1 Ru C10 C11 -83.21(7) . . . . ? N4 Ru C10 C11 -163.23(7) . . . . ? C15 Ru C10 C11 131.09(11) . . . . ? C12 Ru C10 C11 28.97(7) . . . . ? C14 Ru C10 C11 101.83(8) . . . . ? C13 Ru C10 C11 66.16(7) . . . . ? Cl Ru C10 C11 31.56(16) . . . . ? C1 Ru C10 C16 32.63(13) . . . . ? N4 Ru C10 C16 -47.40(13) . . . . ? C15 Ru C10 C16 -113.07(15) . . . . ? C11 Ru C10 C16 115.84(15) . . . . ? C12 Ru C10 C16 144.81(14) . . . . ? C14 Ru C10 C16 -142.33(14) . . . . ? C13 Ru C10 C16 -178.00(13) . . . . ? Cl Ru C10 C16 147.39(10) . . . . ? C15 C10 C16 C17 -137.03(13) . . . . ? C11 C10 C16 C17 46.69(17) . . . . ? Ru C10 C16 C17 -46.29(18) . . . . ? C15 C10 C16 C18 99.00(14) . . . . ? C11 C10 C16 C18 -77.28(15) . . . . ? Ru C10 C16 C18 -170.26(11) . . . . ? C15 C10 C11 C12 -2.99(17) . . . . ? C16 C10 C11 C12 173.43(11) . . . . ? Ru C10 C11 C12 -54.99(10) . . . . ? C15 C10 C11 Ru 52.00(9) . . . . ? C16 C10 C11 Ru -131.58(11) . . . . ? C1 Ru C11 C12 -124.37(7) . . . . ? N4 Ru C11 C12 160.78(7) . . . . ? C15 Ru C11 C12 102.82(8) . . . . ? C10 Ru C11 C12 132.60(10) . . . . ? C14 Ru C11 C12 65.64(7) . . . . ? C13 Ru C11 C12 29.71(7) . . . . ? Cl Ru C11 C12 -37.04(8) . . . . ? C1 Ru C11 C10 103.03(7) . . . . ? N4 Ru C11 C10 28.18(11) . . . . ? C15 Ru C11 C10 -29.78(7) . . . . ? C12 Ru C11 C10 -132.60(10) . . . . ? C14 Ru C11 C10 -66.96(7) . . . . ? C13 Ru C11 C10 -102.89(8) . . . . ? Cl Ru C11 C10 -169.64(5) . . . . ? C10 C11 C12 C13 -1.16(18) . . . . ? Ru C11 C12 C13 -56.80(10) . . . . ? C10 C11 C12 Ru 55.64(10) . . . . ? C1 Ru C12 C11 65.00(8) . . . . ? N4 Ru C12 C11 -110.1(2) . . . . ? C15 Ru C12 C11 -66.21(7) . . . . ? C10 Ru C12 C11 -29.00(7) . . . . ? C14 Ru C12 C11 -102.97(8) . . . . ? C13 Ru C12 C11 -131.25(11) . . . . ? Cl Ru C12 C11 151.70(6) . . . . ? C1 Ru C12 C13 -163.75(7) . . . . ? N4 Ru C12 C13 21.2(2) . . . . ? C15 Ru C12 C13 65.05(7) . . . . ? C11 Ru C12 C13 131.25(11) . . . . ? C10 Ru C12 C13 102.25(8) . . . . ? C14 Ru C12 C13 28.28(7) . . . . ? Cl Ru C12 C13 -77.05(7) . . . . ? C11 C12 C13 C14 2.38(17) . . . . ? Ru C12 C13 C14 -53.03(10) . . . . ? C11 C12 C13 C19 178.81(11) . . . . ? Ru C12 C13 C19 123.40(11) . . . . ? C11 C12 C13 Ru 55.41(10) . . . . ? C1 Ru C13 C14 162.98(9) . . . . ? N4 Ru C13 C14 -41.82(9) . . . . ? C15 Ru C13 C14 28.77(7) . . . . ? C11 Ru C13 C14 102.84(8) . . . . ? C12 Ru C13 C14 132.61(11) . . . . ? C10 Ru C13 C14 65.64(8) . . . . ? Cl Ru C13 C14 -123.15(7) . . . . ? C1 Ru C13 C12 30.37(13) . . . . ? N4 Ru C13 C12 -174.42(7) . . . . ? C15 Ru C13 C12 -103.84(8) . . . . ? C11 Ru C13 C12 -29.77(7) . . . . ? C10 Ru C13 C12 -66.97(7) . . . . ? C14 Ru C13 C12 -132.61(11) . . . . ? Cl Ru C13 C12 104.25(7) . . . . ? C1 Ru C13 C19 -82.86(15) . . . . ? N4 Ru C13 C19 72.34(13) . . . . ? C15 Ru C13 C19 142.93(13) . . . . ? C11 Ru C13 C19 -143.00(13) . . . . ? C12 Ru C13 C19 -113.24(14) . . . . ? C10 Ru C13 C19 179.80(12) . . . . ? C14 Ru C13 C19 114.16(14) . . . . ? Cl Ru C13 C19 -8.99(11) . . . . ? C12 C13 C14 C15 0.63(17) . . . . ? C19 C13 C14 C15 -175.84(11) . . . . ? Ru C13 C14 C15 -51.05(10) . . . . ? C12 C13 C14 Ru 51.67(10) . . . . ? C19 C13 C14 Ru -124.79(11) . . . . ? C1 Ru C14 C13 -130.3(2) . . . . ? N4 Ru C14 C13 149.33(7) . . . . ? C15 Ru C14 C13 -133.24(11) . . . . ? C11 Ru C14 C13 -66.44(8) . . . . ? C12 Ru C14 C13 -29.21(7) . . . . ? C10 Ru C14 C13 -103.90(8) . . . . ? Cl Ru C14 C13 60.80(7) . . . . ? C1 Ru C14 C15 2.9(3) . . . . ? N4 Ru C14 C15 -77.42(8) . . . . ? C11 Ru C14 C15 66.81(8) . . . . ? C12 Ru C14 C15 104.03(8) . . . . ? C10 Ru C14 C15 29.35(7) . . . . ? C13 Ru C14 C15 133.24(11) . . . . ? Cl Ru C14 C15 -165.95(6) . . . . ? C11 C10 C15 C14 6.15(17) . . . . ? C16 C10 C15 C14 -170.34(11) . . . . ? Ru C10 C15 C14 58.28(10) . . . . ? C11 C10 C15 Ru -52.13(9) . . . . ? C16 C10 C15 Ru 131.38(11) . . . . ? C13 C14 C15 C10 -5.07(18) . . . . ? Ru C14 C15 C10 -57.86(10) . . . . ? C13 C14 C15 Ru 52.79(10) . . . . ? C1 Ru C15 C10 -47.31(10) . . . . ? N4 Ru C15 C10 -120.95(7) . . . . ? C11 Ru C15 C10 29.88(7) . . . . ? C12 Ru C15 C10 67.07(7) . . . . ? C14 Ru C15 C10 131.95(11) . . . . ? C13 Ru C15 C10 104.00(8) . . . . ? Cl Ru C15 C10 154.31(6) . . . . ? C1 Ru C15 C14 -179.25(7) . . . . ? N4 Ru C15 C14 107.10(7) . . . . ? C11 Ru C15 C14 -102.06(8) . . . . ? C12 Ru C15 C14 -64.88(8) . . . . ? C10 Ru C15 C14 -131.95(11) . . . . ? C13 Ru C15 C14 -27.95(7) . . . . ? Cl Ru C15 C14 22.37(10) . . . . ? O2 S C20 F2 55.96(13) . . . . ? O3 S C20 F2 -65.57(14) . . . . ? O1 S C20 F2 175.65(11) . . . . ? O2 S C20 F1 176.52(12) . . . . ? O3 S C20 F1 54.99(14) . . . . ? O1 S C20 F1 -63.79(12) . . . . ? O2 S C20 F3 -63.88(12) . . . . ? O3 S C20 F3 174.59(13) . . . . ? O1 S C20 F3 55.81(12) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 35.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.170 _refine_diff_density_min -1.094 _refine_diff_density_rms 0.099 #===END data_alb79(2b) _database_code_depnum_ccdc_archive 'CCDC 817672' #TrackingRef 'alb09pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H26 Cl N4 Ru, C F3 O3 S, C2 H3 N' _chemical_formula_sum 'C23 H29 Cl F3 N5 O3 Ru S' _chemical_formula_weight 649.09 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' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9511(2) _cell_length_b 11.3181(3) _cell_length_c 15.6143(5) _cell_angle_alpha 83.120(2) _cell_angle_beta 75.630(2) _cell_angle_gamma 80.116(2) _cell_volume 1336.59(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8382 _cell_measurement_theta_min 3.3237 _cell_measurement_theta_max 26.3269 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1182 _exptl_crystal_size_mid 0.0682 _exptl_crystal_size_min 0.0358 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.935 _exptl_absorpt_correction_T_max 0.974 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22534 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 26.38 _reflns_number_total 5452 _reflns_number_gt 4374 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^)+(0.0180P)^2^+1.3487P] 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 5452 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _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 Ru Ru 0.38926(3) 0.40276(2) 0.762599(17) 0.00994(7) Uani 1 1 d . . . Cl Cl 0.15894(9) 0.45034(7) 0.89176(5) 0.01531(17) Uani 1 1 d . . . N1 N 0.5197(3) 0.5256(2) 0.80669(16) 0.0110(5) Uani 1 1 d . . . C1 C 0.5023(4) 0.6442(3) 0.7814(2) 0.0137(6) Uani 1 1 d . . . H1 H 0.4343 0.6746 0.7392 0.016 Uiso 1 1 calc R . . C2 C 0.5803(4) 0.7236(3) 0.8148(2) 0.0165(7) Uani 1 1 d . . . H2 H 0.5667 0.8068 0.7954 0.020 Uiso 1 1 calc R . . C3 C 0.6778(4) 0.6800(3) 0.8766(2) 0.0163(7) Uani 1 1 d . . . H3 H 0.7331 0.7330 0.8996 0.020 Uiso 1 1 calc R . . C4 C 0.6949(4) 0.5588(3) 0.9050(2) 0.0134(6) Uani 1 1 d . . . H4 H 0.7596 0.5276 0.9484 0.016 Uiso 1 1 calc R . . C5 C 0.6152(3) 0.4845(3) 0.86839(19) 0.0110(6) Uani 1 1 d . . . C6 C 0.6128(4) 0.3560(3) 0.88890(19) 0.0108(6) Uani 1 1 d . . . C7 C 0.5167(4) 0.2979(3) 0.8487(2) 0.0113(6) Uani 1 1 d . . . N2 N 0.6812(3) 0.2747(2) 0.94726(16) 0.0114(5) Uani 1 1 d . . . C8 C 0.7951(4) 0.2890(3) 1.0052(2) 0.0173(7) Uani 1 1 d . . . H8A H 0.8177 0.2131 1.0407 0.026 Uiso 1 1 calc R . . H8B H 0.7370 0.3525 1.0447 0.026 Uiso 1 1 calc R . . H8C H 0.9065 0.3110 0.9689 0.026 Uiso 1 1 calc R . . N3 N 0.6336(3) 0.1679(2) 0.94903(17) 0.0133(5) Uani 1 1 d . . . N4 N 0.5349(3) 0.1839(2) 0.88863(16) 0.0114(5) Uani 1 1 d . . . C9 C 0.4504(4) 0.0815(3) 0.8801(2) 0.0152(7) Uani 1 1 d . . . H9A H 0.5081 0.0070 0.9074 0.018 Uiso 1 1 calc R . . H9B H 0.4645 0.0710 0.8166 0.018 Uiso 1 1 calc R . . C10 C 0.2577(4) 0.1016(3) 0.9250(2) 0.0217(7) Uani 1 1 d . . . H10A H 0.2440 0.1084 0.9884 0.033 Uiso 1 1 calc R . . H10B H 0.2031 0.0336 0.9172 0.033 Uiso 1 1 calc R . . H10C H 0.2010 0.1759 0.8986 0.033 Uiso 1 1 calc R . . C11 C 0.5267(4) 0.3067(3) 0.6444(2) 0.0123(6) Uani 1 1 d . . . C17 C 0.6980(4) 0.2213(3) 0.6273(2) 0.0157(7) Uani 1 1 d . . . H17 H 0.6850 0.1502 0.6718 0.019 Uiso 1 1 calc R . . C18 C 0.8534(4) 0.2770(3) 0.6363(3) 0.0256(8) Uani 1 1 d . . . H18A H 0.8781 0.3405 0.5885 0.038 Uiso 1 1 calc R . . H18B H 0.9567 0.2149 0.6326 0.038 Uiso 1 1 calc R . . H18C H 0.8254 0.3115 0.6938 0.038 Uiso 1 1 calc R . . C19 C 0.7298(5) 0.1773(3) 0.5352(2) 0.0325(9) Uani 1 1 d . . . H19A H 0.6295 0.1401 0.5315 0.049 Uiso 1 1 calc R . . H19B H 0.8366 0.1180 0.5246 0.049 Uiso 1 1 calc R . . H19C H 0.7437 0.2456 0.4904 0.049 Uiso 1 1 calc R . . C12 C 0.3649(4) 0.2620(3) 0.6832(2) 0.0144(7) Uani 1 1 d . . . H12 H 0.3651 0.1780 0.6976 0.017 Uiso 1 1 calc R . . C13 C 0.2062(4) 0.3405(3) 0.7001(2) 0.0158(7) Uani 1 1 d . . . H13 H 0.1016 0.3097 0.7303 0.019 Uiso 1 1 calc R . . C14 C 0.1980(4) 0.4670(3) 0.6729(2) 0.0159(7) Uani 1 1 d . . . C20 C 0.0252(4) 0.5489(3) 0.6901(2) 0.0220(8) Uani 1 1 d . . . H20A H 0.0461 0.6324 0.6861 0.033 Uiso 1 1 calc R . . H20B H -0.0438 0.5275 0.7495 0.033 Uiso 1 1 calc R . . H20C H -0.0393 0.5401 0.6458 0.033 Uiso 1 1 calc R . . C15 C 0.3553(4) 0.5097(3) 0.6344(2) 0.0136(6) Uani 1 1 d . . . H15 H 0.3540 0.5927 0.6153 0.016 Uiso 1 1 calc R . . C16 C 0.5187(4) 0.4317(3) 0.6228(2) 0.0133(6) Uani 1 1 d . . . H16 H 0.6247 0.4647 0.6001 0.016 Uiso 1 1 calc R . . O1 O 0.3286(3) 0.9566(2) 0.73842(16) 0.0261(6) Uani 1 1 d . . . O2 O 0.1973(3) 0.80882(19) 0.68665(17) 0.0279(6) Uani 1 1 d . . . O3 O 0.1646(3) 1.0169(2) 0.62475(15) 0.0308(6) Uani 1 1 d . . . S S 0.19448(10) 0.93338(7) 0.69777(5) 0.01746(18) Uani 1 1 d . . . C21 C -0.0063(4) 0.9686(3) 0.7828(2) 0.0243(8) Uani 1 1 d . . . F1 F -0.0313(2) 1.08338(18) 0.80208(13) 0.0336(5) Uani 1 1 d . . . F2 F -0.1489(2) 0.9517(2) 0.75777(15) 0.0407(6) Uani 1 1 d . . . F3 F -0.0038(3) 0.9002(2) 0.85877(14) 0.0379(6) Uani 1 1 d . . . N5 N 0.7315(5) 0.6499(4) 0.5358(3) 0.0570(11) Uani 1 1 d . . . C22 C 0.7376(5) 0.7422(4) 0.5541(2) 0.0323(9) Uani 1 1 d . . . C23 C 0.7500(6) 0.8598(4) 0.5779(3) 0.0494(12) Uani 1 1 d . . . H23A H 0.8459 0.8529 0.6082 0.074 Uiso 1 1 calc R . . H23B H 0.6393 0.8914 0.6175 0.074 Uiso 1 1 calc R . . H23C H 0.7732 0.9145 0.5241 0.074 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 Ru 0.01028(12) 0.01013(12) 0.01079(13) -0.00009(9) -0.00469(9) -0.00251(9) Cl 0.0119(3) 0.0203(4) 0.0140(4) -0.0030(3) -0.0018(3) -0.0038(3) N1 0.0100(12) 0.0130(13) 0.0099(14) 0.0000(10) -0.0014(10) -0.0033(10) C1 0.0131(15) 0.0122(15) 0.0142(17) 0.0013(12) -0.0016(12) -0.0011(12) C2 0.0194(16) 0.0095(15) 0.0202(18) -0.0001(13) -0.0024(14) -0.0051(13) C3 0.0150(15) 0.0162(16) 0.0198(18) -0.0058(13) -0.0032(13) -0.0063(13) C4 0.0103(14) 0.0170(16) 0.0142(17) -0.0009(13) -0.0048(12) -0.0029(12) C5 0.0071(13) 0.0152(15) 0.0091(16) -0.0012(12) 0.0007(12) -0.0011(12) C6 0.0101(14) 0.0135(15) 0.0077(15) -0.0010(12) -0.0013(12) 0.0003(12) C7 0.0105(14) 0.0119(15) 0.0103(16) -0.0007(12) -0.0013(12) -0.0003(12) N2 0.0107(12) 0.0124(13) 0.0122(14) 0.0003(10) -0.0042(10) -0.0034(10) C8 0.0160(15) 0.0208(17) 0.0191(18) 0.0015(13) -0.0115(13) -0.0052(13) N3 0.0140(12) 0.0148(13) 0.0124(14) 0.0008(10) -0.0059(11) -0.0027(10) N4 0.0127(12) 0.0117(12) 0.0120(14) -0.0005(10) -0.0057(10) -0.0040(10) C9 0.0217(16) 0.0083(15) 0.0171(18) 0.0022(12) -0.0058(13) -0.0065(12) C10 0.0226(17) 0.0188(17) 0.026(2) 0.0027(14) -0.0079(15) -0.0100(14) C11 0.0167(15) 0.0144(15) 0.0086(16) -0.0026(12) -0.0085(12) -0.0010(12) C17 0.0198(16) 0.0125(15) 0.0158(17) -0.0020(13) -0.0066(13) -0.0005(13) C18 0.0150(16) 0.0253(19) 0.037(2) -0.0113(16) -0.0077(15) 0.0033(14) C19 0.036(2) 0.033(2) 0.027(2) -0.0144(17) -0.0123(17) 0.0121(17) C12 0.0203(16) 0.0130(15) 0.0138(17) -0.0019(12) -0.0106(13) -0.0025(13) C13 0.0153(15) 0.0198(17) 0.0153(17) 0.0016(13) -0.0085(13) -0.0058(13) C14 0.0166(15) 0.0202(17) 0.0132(17) -0.0010(13) -0.0081(13) -0.0028(13) C20 0.0171(16) 0.0232(18) 0.028(2) -0.0040(15) -0.0121(15) 0.0021(14) C15 0.0208(16) 0.0121(15) 0.0101(16) 0.0021(12) -0.0089(13) -0.0026(12) C16 0.0166(15) 0.0151(16) 0.0095(16) -0.0003(12) -0.0051(12) -0.0034(12) O1 0.0189(11) 0.0268(13) 0.0343(15) -0.0093(11) -0.0054(11) -0.0043(10) O2 0.0430(15) 0.0124(11) 0.0348(16) -0.0037(10) -0.0209(12) -0.0033(10) O3 0.0479(15) 0.0208(13) 0.0156(13) 0.0032(10) -0.0008(11) 0.0041(11) S 0.0236(4) 0.0132(4) 0.0155(4) -0.0011(3) -0.0047(3) -0.0022(3) C21 0.0213(17) 0.029(2) 0.022(2) 0.0026(15) -0.0073(15) -0.0034(15) F1 0.0321(11) 0.0387(13) 0.0249(12) -0.0086(9) -0.0006(9) 0.0045(10) F2 0.0212(11) 0.0581(15) 0.0483(15) 0.0052(12) -0.0179(10) -0.0125(10) F3 0.0332(11) 0.0552(14) 0.0210(12) 0.0172(10) -0.0058(9) -0.0096(10) N5 0.090(3) 0.057(3) 0.039(2) 0.021(2) -0.026(2) -0.054(2) C22 0.029(2) 0.050(3) 0.020(2) 0.0175(19) -0.0108(16) -0.0192(18) C23 0.067(3) 0.040(3) 0.034(3) 0.001(2) 0.005(2) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C7 2.031(3) . ? Ru N1 2.136(2) . ? Ru C16 2.181(3) . ? Ru C13 2.188(3) . ? Ru C12 2.194(3) . ? Ru C11 2.203(3) . ? Ru C15 2.263(3) . ? Ru C14 2.288(3) . ? Ru Cl 2.4082(8) . ? N1 C1 1.346(4) . ? N1 C5 1.362(4) . ? C1 C2 1.389(4) . ? C1 H1 0.9500 . ? C2 C3 1.379(4) . ? C2 H2 0.9500 . ? C3 C4 1.384(4) . ? C3 H3 0.9500 . ? C4 C5 1.383(4) . ? C4 H4 0.9500 . ? C5 C6 1.453(4) . ? C6 N2 1.359(4) . ? C6 C7 1.386(4) . ? C7 N4 1.364(4) . ? N2 N3 1.323(3) . ? N2 C8 1.468(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N3 N4 1.348(3) . ? N4 C9 1.470(4) . ? C9 C10 1.508(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.409(4) . ? C11 C12 1.429(4) . ? C11 C17 1.513(4) . ? C17 C18 1.523(4) . ? C17 C19 1.526(5) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C12 C13 1.399(4) . ? C12 H12 0.9500 . ? C13 C14 1.439(4) . ? C13 H13 0.9500 . ? C14 C15 1.387(4) . ? C14 C20 1.503(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C15 C16 1.424(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? O1 S 1.443(2) . ? O2 S 1.437(2) . ? O3 S 1.432(2) . ? S C21 1.824(3) . ? C21 F2 1.337(4) . ? C21 F3 1.339(4) . ? C21 F1 1.339(4) . ? N5 C22 1.127(5) . ? C22 C23 1.449(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? 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 C7 Ru N1 76.65(10) . . ? C7 Ru C16 120.88(11) . . ? N1 Ru C16 94.90(10) . . ? C7 Ru C13 123.94(11) . . ? N1 Ru C13 158.69(10) . . ? C16 Ru C13 79.40(11) . . ? C7 Ru C12 98.58(11) . . ? N1 Ru C12 156.29(10) . . ? C16 Ru C12 67.28(11) . . ? C13 Ru C12 37.25(11) . . ? C7 Ru C11 96.48(11) . . ? N1 Ru C11 118.80(10) . . ? C16 Ru C11 37.48(11) . . ? C13 Ru C11 68.08(11) . . ? C12 Ru C11 37.92(11) . . ? C7 Ru C15 157.63(11) . . ? N1 Ru C15 97.36(10) . . ? C16 Ru C15 37.32(10) . . ? C13 Ru C15 65.68(11) . . ? C12 Ru C15 78.13(11) . . ? C11 Ru C15 67.17(10) . . ? C7 Ru C14 160.99(11) . . ? N1 Ru C14 121.57(10) . . ? C16 Ru C14 66.46(11) . . ? C13 Ru C14 37.41(11) . . ? C12 Ru C14 67.02(11) . . ? C11 Ru C14 79.81(11) . . ? C15 Ru C14 35.48(11) . . ? C7 Ru Cl 85.56(8) . . ? N1 Ru Cl 84.61(7) . . ? C16 Ru Cl 152.80(8) . . ? C13 Ru Cl 91.23(8) . . ? C12 Ru Cl 118.49(8) . . ? C11 Ru Cl 156.40(8) . . ? C15 Ru Cl 115.65(8) . . ? C14 Ru Cl 90.61(8) . . ? C1 N1 C5 117.8(3) . . ? C1 N1 Ru 123.2(2) . . ? C5 N1 Ru 118.80(18) . . ? N1 C1 C2 122.2(3) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.1(3) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.8(3) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 118.2(3) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? N1 C5 C4 122.9(3) . . ? N1 C5 C6 109.3(2) . . ? C4 C5 C6 127.8(3) . . ? N2 C6 C7 108.0(2) . . ? N2 C6 C5 132.4(3) . . ? C7 C6 C5 119.4(3) . . ? N4 C7 C6 102.4(2) . . ? N4 C7 Ru 141.6(2) . . ? C6 C7 Ru 115.8(2) . . ? N3 N2 C6 111.6(2) . . ? N3 N2 C8 118.3(2) . . ? C6 N2 C8 130.1(2) . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 N3 N4 103.8(2) . . ? N3 N4 C7 114.2(2) . . ? N3 N4 C9 116.7(2) . . ? C7 N4 C9 128.9(2) . . ? N4 C9 C10 110.7(2) . . ? N4 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 117.3(3) . . ? C16 C11 C17 122.3(3) . . ? C12 C11 C17 120.4(3) . . ? C16 C11 Ru 70.41(17) . . ? C12 C11 Ru 70.67(17) . . ? C17 C11 Ru 130.1(2) . . ? C11 C17 C18 113.2(2) . . ? C11 C17 C19 108.5(3) . . ? C18 C17 C19 111.0(3) . . ? C11 C17 H17 108.0 . . ? C18 C17 H17 108.0 . . ? C19 C17 H17 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C13 C12 C11 120.7(3) . . ? C13 C12 Ru 71.14(18) . . ? C11 C12 Ru 71.41(17) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? Ru C12 H12 130.5 . . ? C12 C13 C14 121.5(3) . . ? C12 C13 Ru 71.60(17) . . ? C14 C13 Ru 75.10(18) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? Ru C13 H13 125.9 . . ? C15 C14 C13 117.4(3) . . ? C15 C14 C20 122.1(3) . . ? C13 C14 C20 120.4(3) . . ? C15 C14 Ru 71.28(17) . . ? C13 C14 Ru 67.49(16) . . ? C20 C14 Ru 130.1(2) . . ? C14 C20 H20A 109.5 . . ? C14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C15 C16 121.3(3) . . ? C14 C15 Ru 73.24(17) . . ? C16 C15 Ru 68.20(16) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? Ru C15 H15 132.3 . . ? C11 C16 C15 121.5(3) . . ? C11 C16 Ru 72.11(17) . . ? C15 C16 Ru 74.47(17) . . ? C11 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? Ru C16 H16 126.0 . . ? O3 S O2 116.03(15) . . ? O3 S O1 114.89(15) . . ? O2 S O1 114.78(14) . . ? O3 S C21 102.49(15) . . ? O2 S C21 103.16(16) . . ? O1 S C21 102.77(15) . . ? F2 C21 F3 106.7(3) . . ? F2 C21 F1 106.8(3) . . ? F3 C21 F1 107.0(3) . . ? F2 C21 S 112.2(3) . . ? F3 C21 S 112.1(2) . . ? F1 C21 S 111.7(2) . . ? N5 C22 C23 178.5(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? 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 C7 Ru N1 C1 -177.0(2) . . . . ? C16 Ru N1 C1 62.4(2) . . . . ? C13 Ru N1 C1 -10.8(4) . . . . ? C12 Ru N1 C1 102.2(3) . . . . ? C11 Ru N1 C1 92.9(2) . . . . ? C15 Ru N1 C1 25.0(2) . . . . ? C14 Ru N1 C1 -2.9(3) . . . . ? Cl Ru N1 C1 -90.3(2) . . . . ? C7 Ru N1 C5 -2.0(2) . . . . ? C16 Ru N1 C5 -122.6(2) . . . . ? C13 Ru N1 C5 164.2(3) . . . . ? C12 Ru N1 C5 -82.8(3) . . . . ? C11 Ru N1 C5 -92.1(2) . . . . ? C15 Ru N1 C5 -160.0(2) . . . . ? C14 Ru N1 C5 172.14(19) . . . . ? Cl Ru N1 C5 84.75(19) . . . . ? C5 N1 C1 C2 1.2(4) . . . . ? Ru N1 C1 C2 176.2(2) . . . . ? N1 C1 C2 C3 -0.6(5) . . . . ? C1 C2 C3 C4 -0.7(4) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C1 N1 C5 C4 -0.5(4) . . . . ? Ru N1 C5 C4 -175.8(2) . . . . ? C1 N1 C5 C6 177.9(2) . . . . ? Ru N1 C5 C6 2.6(3) . . . . ? C3 C4 C5 N1 -0.7(4) . . . . ? C3 C4 C5 C6 -178.8(3) . . . . ? N1 C5 C6 N2 -177.3(3) . . . . ? C4 C5 C6 N2 1.1(5) . . . . ? N1 C5 C6 C7 -2.1(4) . . . . ? C4 C5 C6 C7 176.3(3) . . . . ? N2 C6 C7 N4 0.8(3) . . . . ? C5 C6 C7 N4 -175.5(2) . . . . ? N2 C6 C7 Ru 176.85(18) . . . . ? C5 C6 C7 Ru 0.6(3) . . . . ? N1 Ru C7 N4 174.5(4) . . . . ? C16 Ru C7 N4 -97.8(3) . . . . ? C13 Ru C7 N4 0.5(4) . . . . ? C12 Ru C7 N4 -29.2(4) . . . . ? C11 Ru C7 N4 -67.4(3) . . . . ? C15 Ru C7 N4 -108.8(4) . . . . ? C14 Ru C7 N4 10.1(6) . . . . ? Cl Ru C7 N4 89.0(3) . . . . ? N1 Ru C7 C6 0.7(2) . . . . ? C16 Ru C7 C6 88.4(2) . . . . ? C13 Ru C7 C6 -173.3(2) . . . . ? C12 Ru C7 C6 157.0(2) . . . . ? C11 Ru C7 C6 118.8(2) . . . . ? C15 Ru C7 C6 77.3(4) . . . . ? C14 Ru C7 C6 -163.7(3) . . . . ? Cl Ru C7 C6 -84.8(2) . . . . ? C7 C6 N2 N3 -1.1(3) . . . . ? C5 C6 N2 N3 174.5(3) . . . . ? C7 C6 N2 C8 178.7(3) . . . . ? C5 C6 N2 C8 -5.7(5) . . . . ? C6 N2 N3 N4 1.0(3) . . . . ? C8 N2 N3 N4 -178.9(2) . . . . ? N2 N3 N4 C7 -0.4(3) . . . . ? N2 N3 N4 C9 -175.5(2) . . . . ? C6 C7 N4 N3 -0.2(3) . . . . ? Ru C7 N4 N3 -174.5(3) . . . . ? C6 C7 N4 C9 174.1(3) . . . . ? Ru C7 N4 C9 -0.2(5) . . . . ? N3 N4 C9 C10 103.4(3) . . . . ? C7 N4 C9 C10 -70.8(4) . . . . ? C7 Ru C11 C16 -134.48(18) . . . . ? N1 Ru C11 C16 -56.17(19) . . . . ? C13 Ru C11 C16 101.47(19) . . . . ? C12 Ru C11 C16 129.9(2) . . . . ? C15 Ru C11 C16 29.66(17) . . . . ? C14 Ru C11 C16 64.37(17) . . . . ? Cl Ru C11 C16 131.77(19) . . . . ? C7 Ru C11 C12 95.66(17) . . . . ? N1 Ru C11 C12 173.96(15) . . . . ? C16 Ru C11 C12 -129.9(2) . . . . ? C13 Ru C11 C12 -28.40(16) . . . . ? C15 Ru C11 C12 -100.21(18) . . . . ? C14 Ru C11 C12 -65.50(17) . . . . ? Cl Ru C11 C12 1.9(3) . . . . ? C7 Ru C11 C17 -18.3(3) . . . . ? N1 Ru C11 C17 60.0(3) . . . . ? C16 Ru C11 C17 116.2(3) . . . . ? C13 Ru C11 C17 -142.3(3) . . . . ? C12 Ru C11 C17 -113.9(3) . . . . ? C15 Ru C11 C17 145.8(3) . . . . ? C14 Ru C11 C17 -179.4(3) . . . . ? Cl Ru C11 C17 -112.0(3) . . . . ? C16 C11 C17 C18 32.7(4) . . . . ? C12 C11 C17 C18 -147.7(3) . . . . ? Ru C11 C17 C18 -58.1(4) . . . . ? C16 C11 C17 C19 -90.9(4) . . . . ? C12 C11 C17 C19 88.7(3) . . . . ? Ru C11 C17 C19 178.3(2) . . . . ? C16 C11 C12 C13 -1.1(4) . . . . ? C17 C11 C12 C13 179.3(3) . . . . ? Ru C11 C12 C13 53.4(3) . . . . ? C16 C11 C12 Ru -54.5(2) . . . . ? C17 C11 C12 Ru 125.9(3) . . . . ? C7 Ru C12 C13 137.25(18) . . . . ? N1 Ru C12 C13 -146.4(2) . . . . ? C16 Ru C12 C13 -102.8(2) . . . . ? C11 Ru C12 C13 -133.2(3) . . . . ? C15 Ru C12 C13 -65.24(18) . . . . ? C14 Ru C12 C13 -29.80(18) . . . . ? Cl Ru C12 C13 47.67(19) . . . . ? C7 Ru C12 C11 -89.55(17) . . . . ? N1 Ru C12 C11 -13.2(3) . . . . ? C16 Ru C12 C11 30.42(16) . . . . ? C13 Ru C12 C11 133.2(3) . . . . ? C15 Ru C12 C11 67.96(17) . . . . ? C14 Ru C12 C11 103.40(18) . . . . ? Cl Ru C12 C11 -179.13(13) . . . . ? C11 C12 C13 C14 5.1(5) . . . . ? Ru C12 C13 C14 58.6(3) . . . . ? C11 C12 C13 Ru -53.5(3) . . . . ? C7 Ru C13 C12 -54.0(2) . . . . ? N1 Ru C13 C12 142.3(3) . . . . ? C16 Ru C13 C12 66.23(18) . . . . ? C11 Ru C13 C12 28.87(18) . . . . ? C15 Ru C13 C12 102.8(2) . . . . ? C14 Ru C13 C12 131.1(3) . . . . ? Cl Ru C13 C12 -139.47(17) . . . . ? C7 Ru C13 C14 174.87(17) . . . . ? N1 Ru C13 C14 11.2(4) . . . . ? C16 Ru C13 C14 -64.90(18) . . . . ? C12 Ru C13 C14 -131.1(3) . . . . ? C11 Ru C13 C14 -102.26(19) . . . . ? C15 Ru C13 C14 -28.34(17) . . . . ? Cl Ru C13 C14 89.40(17) . . . . ? C12 C13 C14 C15 -4.2(5) . . . . ? Ru C13 C14 C15 52.7(3) . . . . ? C12 C13 C14 C20 178.6(3) . . . . ? Ru C13 C14 C20 -124.5(3) . . . . ? C12 C13 C14 Ru -56.9(3) . . . . ? C7 Ru C14 C15 -145.0(3) . . . . ? N1 Ru C14 C15 52.9(2) . . . . ? C16 Ru C14 C15 -27.96(17) . . . . ? C13 Ru C14 C15 -131.8(3) . . . . ? C12 Ru C14 C15 -102.1(2) . . . . ? C11 Ru C14 C15 -64.73(18) . . . . ? Cl Ru C14 C15 136.97(17) . . . . ? C7 Ru C14 C13 -13.2(4) . . . . ? N1 Ru C14 C13 -175.27(16) . . . . ? C16 Ru C14 C13 103.8(2) . . . . ? C12 Ru C14 C13 29.68(18) . . . . ? C11 Ru C14 C13 67.09(19) . . . . ? C15 Ru C14 C13 131.8(3) . . . . ? Cl Ru C14 C13 -91.22(17) . . . . ? C7 Ru C14 C20 98.3(4) . . . . ? N1 Ru C14 C20 -63.8(3) . . . . ? C16 Ru C14 C20 -144.6(3) . . . . ? C13 Ru C14 C20 111.5(4) . . . . ? C12 Ru C14 C20 141.2(3) . . . . ? C11 Ru C14 C20 178.6(3) . . . . ? C15 Ru C14 C20 -116.7(4) . . . . ? Cl Ru C14 C20 20.3(3) . . . . ? C13 C14 C15 C16 -0.5(4) . . . . ? C20 C14 C15 C16 176.6(3) . . . . ? Ru C14 C15 C16 50.4(3) . . . . ? C13 C14 C15 Ru -50.9(3) . . . . ? C20 C14 C15 Ru 126.2(3) . . . . ? C7 Ru C15 C14 150.6(3) . . . . ? N1 Ru C15 C14 -136.73(18) . . . . ? C16 Ru C15 C14 134.8(3) . . . . ? C13 Ru C15 C14 29.79(18) . . . . ? C12 Ru C15 C14 66.89(19) . . . . ? C11 Ru C15 C14 105.1(2) . . . . ? Cl Ru C15 C14 -49.20(19) . . . . ? C7 Ru C15 C16 15.7(4) . . . . ? N1 Ru C15 C16 88.42(18) . . . . ? C13 Ru C15 C16 -105.05(19) . . . . ? C12 Ru C15 C16 -67.95(18) . . . . ? C11 Ru C15 C16 -29.78(17) . . . . ? C14 Ru C15 C16 -134.8(3) . . . . ? Cl Ru C15 C16 175.96(15) . . . . ? C12 C11 C16 C15 -3.6(4) . . . . ? C17 C11 C16 C15 176.0(3) . . . . ? Ru C11 C16 C15 -58.2(3) . . . . ? C12 C11 C16 Ru 54.6(2) . . . . ? C17 C11 C16 Ru -125.8(3) . . . . ? C14 C15 C16 C11 4.4(5) . . . . ? Ru C15 C16 C11 57.1(3) . . . . ? C14 C15 C16 Ru -52.6(3) . . . . ? C7 Ru C16 C11 55.7(2) . . . . ? N1 Ru C16 C11 133.06(17) . . . . ? C13 Ru C16 C11 -67.67(17) . . . . ? C12 Ru C16 C11 -30.76(16) . . . . ? C15 Ru C16 C11 -131.2(3) . . . . ? C14 Ru C16 C11 -104.54(19) . . . . ? Cl Ru C16 C11 -139.21(16) . . . . ? C7 Ru C16 C15 -173.09(17) . . . . ? N1 Ru C16 C15 -95.73(17) . . . . ? C13 Ru C16 C15 63.55(18) . . . . ? C12 Ru C16 C15 100.46(19) . . . . ? C11 Ru C16 C15 131.2(3) . . . . ? C14 Ru C16 C15 26.67(17) . . . . ? Cl Ru C16 C15 -8.0(3) . . . . ? O3 S C21 F2 61.0(3) . . . . ? O2 S C21 F2 -59.9(3) . . . . ? O1 S C21 F2 -179.6(2) . . . . ? O3 S C21 F3 -179.0(2) . . . . ? O2 S C21 F3 60.1(3) . . . . ? O1 S C21 F3 -59.5(3) . . . . ? O3 S C21 F1 -59.0(3) . . . . ? O2 S C21 F1 -179.9(2) . . . . ? O1 S C21 F1 60.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.587 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.105 #===END data_alb81(3b) _database_code_depnum_ccdc_archive 'CCDC 817673' #TrackingRef 'alb09pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H24 N8 Ru, 2 (C F3 O3 S)' _chemical_formula_sum 'C20 H24 F6 N8 O6 Ru S2' _chemical_formula_weight 751.66 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' F F 0.0171 0.0103 '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' 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 'P 21/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 12.2612(1) _cell_length_b 15.4601(2) _cell_length_c 16.5297(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.760(1) _cell_angle_gamma 90.00 _cell_volume 2984.03(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20284 _cell_measurement_theta_min 3.3243 _cell_measurement_theta_max 29.7447 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1874 _exptl_crystal_size_mid 0.1525 _exptl_crystal_size_min 0.1278 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.902 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37720 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 29.81 _reflns_number_total 7486 _reflns_number_gt 6941 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^)+(0.0199P)^2^+2.1465P] 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 7486 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0524 _refine_ls_wR_factor_gt 0.0507 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.004 _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 Ru Ru 0.199820(9) 0.634020(7) 0.368300(6) 0.01169(4) Uani 1 1 d . . . N1 N 0.04649(10) 0.57705(8) 0.37110(7) 0.0145(2) Uani 1 1 d . . . C1 C 0.03653(12) 0.49468(9) 0.39349(9) 0.0184(3) Uani 1 1 d . . . H1 H 0.1024 0.4587 0.4075 0.022 Uiso 1 1 calc R . . C2 C -0.06630(13) 0.46014(10) 0.39692(10) 0.0227(3) Uani 1 1 d . . . H2 H -0.0703 0.4017 0.4135 0.027 Uiso 1 1 calc R . . C3 C -0.16279(13) 0.51157(11) 0.37603(10) 0.0241(3) Uani 1 1 d . . . H3 H -0.2337 0.4893 0.3790 0.029 Uiso 1 1 calc R . . C4 C -0.15485(12) 0.59607(10) 0.35064(10) 0.0215(3) Uani 1 1 d . . . H4 H -0.2207 0.6321 0.3349 0.026 Uiso 1 1 calc R . . C5 C -0.04987(12) 0.62768(9) 0.34833(9) 0.0164(3) Uani 1 1 d . . . C6 C -0.02224(12) 0.71367(9) 0.32603(8) 0.0161(3) Uani 1 1 d . . . C7 C 0.09035(12) 0.73282(9) 0.33107(8) 0.0148(3) Uani 1 1 d . . . N2 N 0.08587(10) 0.81895(8) 0.31421(7) 0.0173(2) Uani 1 1 d . . . C8 C 0.18103(14) 0.87813(10) 0.31901(10) 0.0223(3) Uani 1 1 d . . . H8A H 0.1506 0.9332 0.2905 0.027 Uiso 1 1 calc R . . H8B H 0.2317 0.8524 0.2889 0.027 Uiso 1 1 calc R . . C9 C 0.24964(15) 0.89591(11) 0.41062(11) 0.0281(3) Uani 1 1 d . . . H9A H 0.1994 0.9211 0.4405 0.042 Uiso 1 1 calc R . . H9B H 0.3117 0.9365 0.4123 0.042 Uiso 1 1 calc R . . H9C H 0.2821 0.8416 0.4383 0.042 Uiso 1 1 calc R . . N3 N -0.01915(11) 0.85366(8) 0.29811(8) 0.0205(3) Uani 1 1 d . . . N4 N -0.08380(10) 0.78770(8) 0.30542(8) 0.0189(2) Uani 1 1 d . . . C10 C -0.20526(13) 0.80439(11) 0.29301(10) 0.0258(3) Uani 1 1 d . . . H10A H -0.2217 0.7963 0.3469 0.039 Uiso 1 1 calc R . . H10B H -0.2518 0.7641 0.2506 0.039 Uiso 1 1 calc R . . H10C H -0.2237 0.8639 0.2733 0.039 Uiso 1 1 calc R . . N5 N 0.34495(10) 0.69199(7) 0.35996(7) 0.0154(2) Uani 1 1 d . . . C11 C 0.42931(12) 0.71773(9) 0.35430(9) 0.0188(3) Uani 1 1 d . . . C12 C 0.53907(13) 0.74830(11) 0.34794(12) 0.0302(4) Uani 1 1 d . . . H12A H 0.5894 0.6987 0.3493 0.045 Uiso 1 1 calc R . . H12B H 0.5748 0.7868 0.3958 0.045 Uiso 1 1 calc R . . H12C H 0.5267 0.7799 0.2945 0.045 Uiso 1 1 calc R . . N6 N 0.29774(10) 0.52191(8) 0.41175(7) 0.0160(2) Uani 1 1 d . . . C13 C 0.35111(12) 0.46115(10) 0.43179(9) 0.0192(3) Uani 1 1 d . . . C14 C 0.41904(15) 0.38311(11) 0.45805(13) 0.0343(4) Uani 1 1 d . . . H14A H 0.4763 0.3928 0.5134 0.052 Uiso 1 1 calc R . . H14B H 0.4577 0.3687 0.4159 0.052 Uiso 1 1 calc R . . H14C H 0.3688 0.3352 0.4625 0.052 Uiso 1 1 calc R . . N7 N 0.22840(10) 0.67716(7) 0.48810(7) 0.0153(2) Uani 1 1 d . . . C15 C 0.23588(12) 0.70643(9) 0.55290(9) 0.0162(3) Uani 1 1 d . . . C16 C 0.24412(14) 0.74443(10) 0.63508(9) 0.0229(3) Uani 1 1 d . . . H16A H 0.2735 0.8036 0.6374 0.034 Uiso 1 1 calc R . . H16B H 0.2963 0.7098 0.6802 0.034 Uiso 1 1 calc R . . H16C H 0.1681 0.7455 0.6430 0.034 Uiso 1 1 calc R . . N8 N 0.16803(9) 0.58780(7) 0.24931(7) 0.0145(2) Uani 1 1 d . . . C17 C 0.15071(12) 0.55671(9) 0.18424(9) 0.0167(3) Uani 1 1 d . . . C18 C 0.13022(14) 0.51894(10) 0.10014(9) 0.0238(3) Uani 1 1 d . . . H18A H 0.0894 0.5607 0.0569 0.036 Uiso 1 1 calc R . . H18B H 0.0839 0.4665 0.0955 0.036 Uiso 1 1 calc R . . H18C H 0.2036 0.5043 0.0915 0.036 Uiso 1 1 calc R . . O1 O 0.40253(11) -0.09043(8) 0.23528(9) 0.0393(3) Uani 1 1 d . . . O2 O 0.45109(11) 0.03433(10) 0.16475(10) 0.0435(3) Uani 1 1 d . . . O3 O 0.60148(11) -0.05977(11) 0.25117(10) 0.0515(4) Uani 1 1 d . . . S1 S 0.89410(3) 0.72871(2) 0.04318(2) 0.01884(7) Uani 1 1 d . . . C19 C 0.81514(14) 0.64592(10) 0.08049(10) 0.0243(3) Uani 1 1 d . . . F1 F 0.39487(13) 0.07142(11) 0.32253(10) 0.0744(5) Uani 1 1 d . . . F2 F 0.52883(13) -0.00995(12) 0.39721(8) 0.0681(4) Uani 1 1 d . . . F3 F 0.57026(16) 0.10175(11) 0.33529(14) 0.1003(7) Uani 1 1 d . . . O4 O 0.96563(11) 0.76661(8) 0.12044(8) 0.0336(3) Uani 1 1 d . . . O5 O 0.80355(11) 0.78311(8) -0.00752(8) 0.0349(3) Uani 1 1 d . . . O6 O 0.95431(10) 0.67985(8) -0.00415(7) 0.0297(3) Uani 1 1 d . . . S2 S 0.48714(3) -0.02657(3) 0.23346(3) 0.02729(9) Uani 1 1 d . . . C20 C 0.49523(18) 0.03699(14) 0.32671(15) 0.0465(5) Uani 1 1 d . . . F4 F 0.74131(9) 0.60472(7) 0.01584(7) 0.0361(2) Uani 1 1 d . . . F5 F 0.88417(10) 0.58724(7) 0.12870(7) 0.0437(3) Uani 1 1 d . . . F6 F 0.75454(10) 0.68087(8) 0.12682(7) 0.0447(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01074(6) 0.01288(6) 0.01204(6) -0.00018(4) 0.00437(4) 0.00049(4) N1 0.0132(5) 0.0175(6) 0.0133(5) -0.0035(4) 0.0048(4) -0.0004(4) C1 0.0176(7) 0.0184(7) 0.0203(7) -0.0031(5) 0.0072(6) -0.0011(5) C2 0.0219(7) 0.0208(7) 0.0277(8) -0.0056(6) 0.0112(6) -0.0076(6) C3 0.0161(7) 0.0293(8) 0.0288(8) -0.0097(6) 0.0096(6) -0.0082(6) C4 0.0129(6) 0.0272(8) 0.0243(7) -0.0083(6) 0.0055(6) 0.0002(6) C5 0.0145(6) 0.0209(7) 0.0136(6) -0.0057(5) 0.0040(5) 0.0006(5) C6 0.0149(6) 0.0189(7) 0.0137(6) -0.0027(5) 0.0032(5) 0.0040(5) C7 0.0172(6) 0.0168(6) 0.0110(6) -0.0014(5) 0.0051(5) 0.0022(5) N2 0.0207(6) 0.0174(6) 0.0152(5) 0.0006(4) 0.0075(5) 0.0048(5) C8 0.0294(8) 0.0169(7) 0.0256(8) 0.0029(6) 0.0159(7) 0.0020(6) C9 0.0328(9) 0.0203(7) 0.0317(9) -0.0025(6) 0.0106(7) -0.0063(7) N3 0.0238(6) 0.0216(6) 0.0166(6) 0.0006(5) 0.0067(5) 0.0081(5) N4 0.0178(6) 0.0223(6) 0.0161(6) -0.0017(5) 0.0043(5) 0.0064(5) C10 0.0160(7) 0.0322(8) 0.0265(8) -0.0054(7) 0.0023(6) 0.0098(6) N5 0.0152(6) 0.0151(5) 0.0154(5) 0.0017(4) 0.0040(4) 0.0013(4) C11 0.0180(7) 0.0176(7) 0.0196(7) 0.0044(5) 0.0038(6) 0.0014(5) C12 0.0158(7) 0.0305(9) 0.0436(10) 0.0133(7) 0.0082(7) -0.0036(6) N6 0.0139(5) 0.0184(6) 0.0162(5) 0.0009(4) 0.0054(4) -0.0016(5) C13 0.0159(7) 0.0203(7) 0.0201(7) 0.0026(6) 0.0039(6) -0.0025(6) C14 0.0284(9) 0.0244(8) 0.0471(11) 0.0155(8) 0.0069(8) 0.0084(7) N7 0.0135(5) 0.0152(5) 0.0177(6) 0.0012(4) 0.0054(5) -0.0005(4) C15 0.0158(6) 0.0148(6) 0.0185(7) 0.0017(5) 0.0057(5) -0.0007(5) C16 0.0292(8) 0.0234(7) 0.0169(7) -0.0053(6) 0.0083(6) -0.0010(6) N8 0.0128(5) 0.0146(5) 0.0170(6) 0.0011(4) 0.0060(4) 0.0011(4) C17 0.0165(6) 0.0154(6) 0.0193(7) 0.0027(5) 0.0072(5) 0.0008(5) C18 0.0314(8) 0.0239(7) 0.0165(7) -0.0038(6) 0.0078(6) -0.0006(6) O1 0.0335(7) 0.0248(6) 0.0513(8) 0.0065(6) 0.0006(6) -0.0060(5) O2 0.0302(7) 0.0476(8) 0.0556(9) 0.0263(7) 0.0172(6) 0.0091(6) O3 0.0289(7) 0.0707(11) 0.0619(10) 0.0238(8) 0.0241(7) 0.0268(7) S1 0.02057(17) 0.01773(16) 0.01816(16) 0.00155(13) 0.00583(14) -0.00148(13) C19 0.0278(8) 0.0233(7) 0.0224(7) -0.0022(6) 0.0086(6) -0.0061(6) F1 0.0683(9) 0.0784(11) 0.0798(10) -0.0200(9) 0.0272(8) 0.0339(8) F2 0.0594(9) 0.0979(12) 0.0396(7) -0.0077(8) 0.0038(6) 0.0086(8) F3 0.0883(13) 0.0635(10) 0.1321(17) -0.0342(11) 0.0085(12) -0.0446(10) O4 0.0368(7) 0.0354(7) 0.0263(6) -0.0068(5) 0.0062(5) -0.0165(5) O5 0.0313(6) 0.0310(6) 0.0413(7) 0.0148(6) 0.0097(6) 0.0088(5) O6 0.0314(6) 0.0347(7) 0.0271(6) 0.0011(5) 0.0153(5) 0.0032(5) S2 0.01836(18) 0.0273(2) 0.0381(2) 0.00785(17) 0.01138(16) 0.00585(15) C20 0.0363(11) 0.0429(11) 0.0566(13) -0.0118(10) 0.0085(10) -0.0039(9) F4 0.0346(6) 0.0329(5) 0.0380(6) -0.0093(5) 0.0068(5) -0.0152(4) F5 0.0453(6) 0.0338(6) 0.0469(7) 0.0216(5) 0.0064(5) -0.0046(5) F6 0.0514(7) 0.0505(7) 0.0464(6) -0.0118(5) 0.0361(6) -0.0149(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C7 2.0024(14) . ? Ru N8 2.0158(12) . ? Ru N7 2.0164(12) . ? Ru N5 2.0343(12) . ? Ru N1 2.0893(11) . ? Ru N6 2.1061(12) . ? N1 C1 1.3421(19) . ? N1 C5 1.3708(18) . ? C1 C2 1.386(2) . ? C1 H1 0.9500 . ? C2 C3 1.379(2) . ? C2 H2 0.9500 . ? C3 C4 1.385(2) . ? C3 H3 0.9500 . ? C4 C5 1.388(2) . ? C4 H4 0.9500 . ? C5 C6 1.447(2) . ? C6 N4 1.3560(18) . ? C6 C7 1.3894(19) . ? C7 N2 1.3580(18) . ? N2 N3 1.3446(17) . ? N2 C8 1.4656(19) . ? C8 C9 1.516(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? N3 N4 1.3195(18) . ? N4 C10 1.4630(18) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N5 C11 1.1384(19) . ? C11 C12 1.460(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N6 C13 1.1349(19) . ? C13 C14 1.455(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N7 C15 1.1403(18) . ? C15 C16 1.4551(19) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N8 C17 1.1374(18) . ? C17 C18 1.457(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O1 S2 1.4391(13) . ? O2 S2 1.4371(13) . ? O3 S2 1.4368(13) . ? S1 O4 1.4353(12) . ? S1 O5 1.4403(12) . ? S1 O6 1.4422(12) . ? S1 C19 1.8222(16) . ? C19 F5 1.3278(19) . ? C19 F4 1.3330(18) . ? C19 F6 1.3333(19) . ? F1 C20 1.323(2) . ? F2 C20 1.327(3) . ? F3 C20 1.338(3) . ? S2 C20 1.805(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 C7 Ru N8 93.36(5) . . ? C7 Ru N7 87.07(5) . . ? N8 Ru N7 178.13(5) . . ? C7 Ru N5 99.28(5) . . ? N8 Ru N5 90.16(5) . . ? N7 Ru N5 91.57(5) . . ? C7 Ru N1 78.76(5) . . ? N8 Ru N1 87.98(4) . . ? N7 Ru N1 90.32(4) . . ? N5 Ru N1 177.21(4) . . ? C7 Ru N6 172.56(5) . . ? N8 Ru N6 87.79(5) . . ? N7 Ru N6 91.55(5) . . ? N5 Ru N6 88.06(4) . . ? N1 Ru N6 93.94(4) . . ? C1 N1 C5 118.31(12) . . ? C1 N1 Ru 124.35(9) . . ? C5 N1 Ru 117.34(9) . . ? N1 C1 C2 122.49(14) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 119.29(14) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.05(14) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 119.47(14) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 121.35(13) . . ? N1 C5 C6 110.20(12) . . ? C4 C5 C6 128.42(13) . . ? N4 C6 C7 107.57(13) . . ? N4 C6 C5 133.14(13) . . ? C7 C6 C5 119.08(12) . . ? N2 C7 C6 102.68(12) . . ? N2 C7 Ru 142.40(11) . . ? C6 C7 Ru 114.61(10) . . ? N3 N2 C7 114.09(12) . . ? N3 N2 C8 117.39(12) . . ? C7 N2 C8 128.27(12) . . ? N2 C8 C9 110.93(12) . . ? N2 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N4 N3 N2 103.84(11) . . ? N3 N4 C6 111.80(12) . . ? N3 N4 C10 117.72(12) . . ? C6 N4 C10 130.45(13) . . ? N4 C10 H10A 109.5 . . ? N4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 N5 Ru 174.29(12) . . ? N5 C11 C12 178.32(16) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C13 N6 Ru 177.04(12) . . ? N6 C13 C14 179.49(17) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 N7 Ru 173.60(11) . . ? N7 C15 C16 179.27(17) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 N8 Ru 175.77(11) . . ? N8 C17 C18 178.36(15) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 S1 O5 115.64(8) . . ? O4 S1 O6 114.93(8) . . ? O5 S1 O6 114.93(8) . . ? O4 S1 C19 103.24(7) . . ? O5 S1 C19 102.25(8) . . ? O6 S1 C19 103.21(7) . . ? F5 C19 F4 107.90(13) . . ? F5 C19 F6 107.28(13) . . ? F4 C19 F6 107.04(13) . . ? F5 C19 S1 112.08(11) . . ? F4 C19 S1 111.42(11) . . ? F6 C19 S1 110.89(11) . . ? O3 S2 O2 116.16(8) . . ? O3 S2 O1 114.54(9) . . ? O2 S2 O1 114.58(8) . . ? O3 S2 C20 102.97(10) . . ? O2 S2 C20 104.00(10) . . ? O1 S2 C20 101.99(10) . . ? F1 C20 F2 107.5(2) . . ? F1 C20 F3 107.6(2) . . ? F2 C20 F3 107.27(19) . . ? F1 C20 S2 111.50(15) . . ? F2 C20 S2 111.95(15) . . ? F3 C20 S2 110.77(18) . . ? 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 C7 Ru N1 C1 -179.94(12) . . . . ? N8 Ru N1 C1 86.23(11) . . . . ? N7 Ru N1 C1 -92.99(11) . . . . ? N6 Ru N1 C1 -1.41(11) . . . . ? C7 Ru N1 C5 0.16(10) . . . . ? N8 Ru N1 C5 -93.66(10) . . . . ? N7 Ru N1 C5 87.11(10) . . . . ? N6 Ru N1 C5 178.69(10) . . . . ? C5 N1 C1 C2 -2.1(2) . . . . ? Ru N1 C1 C2 178.03(11) . . . . ? N1 C1 C2 C3 0.5(2) . . . . ? C1 C2 C3 C4 1.2(2) . . . . ? C2 C3 C4 C5 -1.2(2) . . . . ? C1 N1 C5 C4 2.0(2) . . . . ? Ru N1 C5 C4 -178.13(10) . . . . ? C1 N1 C5 C6 -179.71(12) . . . . ? Ru N1 C5 C6 0.19(14) . . . . ? C3 C4 C5 N1 -0.3(2) . . . . ? C3 C4 C5 C6 -178.32(14) . . . . ? N1 C5 C6 N4 -174.70(14) . . . . ? C4 C5 C6 N4 3.5(3) . . . . ? N1 C5 C6 C7 -0.65(17) . . . . ? C4 C5 C6 C7 177.52(14) . . . . ? N4 C6 C7 N2 1.17(14) . . . . ? C5 C6 C7 N2 -174.28(12) . . . . ? N4 C6 C7 Ru 176.26(9) . . . . ? C5 C6 C7 Ru 0.81(16) . . . . ? N8 Ru C7 N2 -101.10(16) . . . . ? N7 Ru C7 N2 80.72(16) . . . . ? N5 Ru C7 N2 -10.39(17) . . . . ? N1 Ru C7 N2 171.63(17) . . . . ? N8 Ru C7 C6 86.77(10) . . . . ? N7 Ru C7 C6 -91.42(10) . . . . ? N5 Ru C7 C6 177.48(10) . . . . ? N1 Ru C7 C6 -0.50(10) . . . . ? C6 C7 N2 N3 -0.98(15) . . . . ? Ru C7 N2 N3 -173.65(12) . . . . ? C6 C7 N2 C8 173.04(13) . . . . ? Ru C7 N2 C8 0.4(2) . . . . ? N3 N2 C8 C9 101.62(15) . . . . ? C7 N2 C8 C9 -72.23(18) . . . . ? C7 N2 N3 N4 0.38(15) . . . . ? C8 N2 N3 N4 -174.33(11) . . . . ? N2 N3 N4 C6 0.43(15) . . . . ? N2 N3 N4 C10 178.88(12) . . . . ? C7 C6 N4 N3 -1.05(16) . . . . ? C5 C6 N4 N3 173.50(14) . . . . ? C7 C6 N4 C10 -179.25(14) . . . . ? C5 C6 N4 C10 -4.7(3) . . . . ? O4 S1 C19 F5 -60.38(13) . . . . ? O5 S1 C19 F5 179.22(12) . . . . ? O6 S1 C19 F5 59.62(13) . . . . ? O4 S1 C19 F4 178.60(12) . . . . ? O5 S1 C19 F4 58.20(13) . . . . ? O6 S1 C19 F4 -61.41(13) . . . . ? O4 S1 C19 F6 59.48(13) . . . . ? O5 S1 C19 F6 -60.91(13) . . . . ? O6 S1 C19 F6 179.48(11) . . . . ? O3 S2 C20 F1 -178.35(17) . . . . ? O2 S2 C20 F1 60.06(18) . . . . ? O1 S2 C20 F1 -59.36(18) . . . . ? O3 S2 C20 F2 -57.89(17) . . . . ? O2 S2 C20 F2 -179.47(14) . . . . ? O1 S2 C20 F2 61.11(16) . . . . ? O3 S2 C20 F3 61.80(19) . . . . ? O2 S2 C20 F3 -59.79(18) . . . . ? O1 S2 C20 F3 -179.21(16) . . . . ? _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.487 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.056 #===END data_alb85(3c) _database_code_depnum_ccdc_archive 'CCDC 817674' #TrackingRef 'alb09pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H26 N8 Ru, 2 (C F3 O3 S), 0.76 (C2 H3 N), 0.25 (H2 O)' _chemical_formula_sum 'C22.51 H28.76 F6 N8.76 O6.25 Ru S2' _chemical_formula_weight 801.16 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' F F 0.0171 0.0103 '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' 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 'P 21/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 8.5421(1) _cell_length_b 24.5273(2) _cell_length_c 16.1468(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.379(1) _cell_angle_gamma 90.00 _cell_volume 3304.34(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13832 _cell_measurement_theta_min 3.2524 _cell_measurement_theta_max 29.6265 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.3686 _exptl_crystal_size_mid 0.2922 _exptl_crystal_size_min 0.1886 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 0.686 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.826 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; The hydrogen atoms of the water molecules could not be detected. The sum of the occupancy factors of all solvent molecules was restrained to be 1. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32309 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 29.69 _reflns_number_total 8218 _reflns_number_gt 6912 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^)+(0.0276P)^2^+2.6256P] 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 8218 _refine_ls_number_parameters 498 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.004 _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 Ru Ru 0.042350(18) 0.660700(6) 0.565224(9) 0.01557(5) Uani 1 1 d . . . N1 N 0.12954(19) 0.73683(7) 0.61214(11) 0.0179(3) Uani 1 1 d . . . C1 C 0.2064(2) 0.74625(9) 0.69264(13) 0.0204(4) Uani 1 1 d . . . H1 H 0.2249 0.7165 0.7312 0.025 Uiso 1 1 calc R . . C2 C 0.2596(3) 0.79741(9) 0.72145(14) 0.0248(5) Uani 1 1 d . . . H2 H 0.3137 0.8025 0.7788 0.030 Uiso 1 1 calc R . . C3 C 0.2337(3) 0.84110(9) 0.66629(15) 0.0266(5) Uani 1 1 d . . . H3 H 0.2710 0.8765 0.6848 0.032 Uiso 1 1 calc R . . C4 C 0.1518(3) 0.83241(9) 0.58306(15) 0.0254(5) Uani 1 1 d . . . H4 H 0.1310 0.8620 0.5442 0.031 Uiso 1 1 calc R . . C5 C 0.1010(2) 0.78037(9) 0.55747(13) 0.0196(4) Uani 1 1 d . . . C6 C 0.0131(2) 0.76226(9) 0.47488(13) 0.0200(4) Uani 1 1 d . . . C7 C -0.0364(2) 0.70855(9) 0.46443(12) 0.0185(4) Uani 1 1 d . . . N2 N -0.0317(2) 0.78767(8) 0.39835(11) 0.0233(4) Uani 1 1 d . . . C8 C -0.0141(3) 0.84447(10) 0.37461(16) 0.0307(5) Uani 1 1 d . . . H8A H -0.0385 0.8477 0.3127 0.046 Uiso 1 1 calc R . . H8B H 0.0962 0.8565 0.3972 0.046 Uiso 1 1 calc R . . H8C H -0.0883 0.8673 0.3980 0.046 Uiso 1 1 calc R . . N3 N -0.1064(2) 0.75375(8) 0.33930(11) 0.0238(4) Uani 1 1 d . . . N4 N -0.1080(2) 0.70645(7) 0.38036(11) 0.0208(4) Uani 1 1 d . . . C9 C -0.1819(3) 0.65802(9) 0.33208(13) 0.0234(5) Uani 1 1 d . . . H9 H -0.2341 0.6358 0.3706 0.028 Uiso 1 1 calc R . . C10 C -0.3106(3) 0.67433(12) 0.25613(15) 0.0369(6) Uani 1 1 d . . . H10A H -0.3865 0.6992 0.2743 0.055 Uiso 1 1 calc R . . H10B H -0.3675 0.6417 0.2306 0.055 Uiso 1 1 calc R . . H10C H -0.2609 0.6927 0.2143 0.055 Uiso 1 1 calc R . . C11 C -0.0526(3) 0.62313(11) 0.30726(15) 0.0321(5) Uani 1 1 d . . . H11A H -0.0056 0.6427 0.2656 0.048 Uiso 1 1 calc R . . H11B H -0.0997 0.5888 0.2825 0.048 Uiso 1 1 calc R . . H11C H 0.0311 0.6153 0.3577 0.048 Uiso 1 1 calc R . . N5 N 0.1622(2) 0.61761(7) 0.67427(10) 0.0188(4) Uani 1 1 d . . . C12 C 0.2389(2) 0.59259(9) 0.72722(13) 0.0206(4) Uani 1 1 d . . . C13 C 0.3361(3) 0.55947(10) 0.79415(14) 0.0295(5) Uani 1 1 d . . . H13A H 0.2689 0.5459 0.8319 0.044 Uiso 1 1 calc R . . H13B H 0.4231 0.5817 0.8267 0.044 Uiso 1 1 calc R . . H13C H 0.3813 0.5286 0.7687 0.044 Uiso 1 1 calc R . . N6 N -0.0607(2) 0.59079(7) 0.51241(11) 0.0201(4) Uani 1 1 d . . . C14 C -0.1268(3) 0.55415(9) 0.47825(13) 0.0237(5) Uani 1 1 d . . . C15 C -0.2126(3) 0.50923(10) 0.42975(17) 0.0389(6) Uani 1 1 d . . . H15A H -0.3061 0.5234 0.3894 0.058 Uiso 1 1 calc R . . H15B H -0.2479 0.4835 0.4684 0.058 Uiso 1 1 calc R . . H15C H -0.1414 0.4905 0.3987 0.058 Uiso 1 1 calc R . . N7 N -0.1509(2) 0.67203(7) 0.61733(11) 0.0195(4) Uani 1 1 d . . . C16 C -0.2568(3) 0.67466(9) 0.64932(13) 0.0211(4) Uani 1 1 d . . . C17 C -0.3924(3) 0.67605(10) 0.69121(15) 0.0286(5) Uani 1 1 d . . . H17A H -0.4354 0.6391 0.6932 0.043 Uiso 1 1 calc R . . H17B H -0.4761 0.7000 0.6595 0.043 Uiso 1 1 calc R . . H17C H -0.3567 0.6900 0.7491 0.043 Uiso 1 1 calc R . . N8 N 0.2394(2) 0.64682(7) 0.51782(10) 0.0187(4) Uani 1 1 d . . . C18 C 0.3520(2) 0.63850(8) 0.49251(12) 0.0189(4) Uani 1 1 d . . . C19 C 0.4983(3) 0.62816(9) 0.46265(14) 0.0247(5) Uani 1 1 d . . . H19A H 0.5674 0.6035 0.5021 0.037 Uiso 1 1 calc R . . H19B H 0.5546 0.6626 0.4595 0.037 Uiso 1 1 calc R . . H19C H 0.4713 0.6114 0.4063 0.037 Uiso 1 1 calc R . . O1 O 0.2446(2) 0.52837(8) 0.38304(12) 0.0460(5) Uani 1 1 d . . . O2 O 0.4372(2) 0.54075(7) 0.29362(11) 0.0339(4) Uani 1 1 d . . . O3 O 0.4130(2) 0.45295(7) 0.35801(12) 0.0431(5) Uani 1 1 d . . . S1 S 0.33744(7) 0.50370(2) 0.32857(4) 0.02838(13) Uani 1 1 d . . . C20 C 0.1862(3) 0.48388(10) 0.23591(16) 0.0317(5) Uani 1 1 d . . . F1 F 0.10592(19) 0.52715(6) 0.19818(10) 0.0455(4) Uani 1 1 d . . . F2 F 0.25159(18) 0.45872(7) 0.17859(10) 0.0451(4) Uani 1 1 d . . . F3 F 0.0794(2) 0.44979(7) 0.25617(12) 0.0559(5) Uani 1 1 d . . . O4 O 0.3403(2) 0.68432(8) 0.88551(11) 0.0398(4) Uani 1 1 d . . . O5 O 0.5593(2) 0.74810(8) 0.89180(12) 0.0455(5) Uani 1 1 d . . . O6A O 0.6072(3) 0.65205(10) 0.88739(14) 0.0333(6) Uani 0.842(4) 1 d P A 1 S2A S 0.50776(11) 0.69517(5) 0.90905(7) 0.0235(3) Uani 0.842(4) 1 d P A 1 C21A C 0.5536(3) 0.69299(12) 1.02388(17) 0.0290(7) Uani 0.842(4) 1 d P A 1 F4A F 0.4774(3) 0.73222(10) 1.05676(16) 0.0455(6) Uani 0.842(4) 1 d P A 1 F5A F 0.5116(3) 0.64555(12) 1.05316(14) 0.0369(5) Uani 0.842(4) 1 d P A 1 F6A F 0.7109(3) 0.69979(14) 1.05448(15) 0.0471(7) Uani 0.842(4) 1 d P A 1 O6B O 0.432(2) 0.7372(6) 1.0056(14) 0.053(4) Uani 0.158(4) 1 d P A 2 S2B S 0.4798(6) 0.7096(3) 0.9393(5) 0.0339(14) Uani 0.158(4) 1 d P A 2 C21B C 0.5994(19) 0.6534(7) 0.9907(10) 0.035(4) Uani 0.158(4) 1 d P A 2 F4B F 0.6463(15) 0.6222(6) 0.9330(10) 0.067(4) Uani 0.158(4) 1 d P A 2 F5B F 0.7297(17) 0.6697(7) 1.0419(9) 0.047(4) Uani 0.158(4) 1 d P A 2 F6B F 0.5206(18) 0.6209(5) 1.0317(9) 0.045(3) Uani 0.158(4) 1 d P A 2 N9 N 0.8348(6) 0.45578(16) 0.0179(2) 0.0668(13) Uani 0.755(5) 1 d P B 1 C22 C 0.8211(5) 0.50124(14) 0.0219(2) 0.0451(11) Uani 0.755(5) 1 d P B 1 C23 C 0.7879(5) 0.55573(17) 0.0374(3) 0.0525(11) Uani 0.755(5) 1 d P B 1 H23A H 0.7314 0.5576 0.0842 0.079 Uiso 0.755(5) 1 calc PR B 1 H23B H 0.7205 0.5716 -0.0137 0.079 Uiso 0.755(5) 1 calc PR B 1 H23C H 0.8885 0.5762 0.0526 0.079 Uiso 0.755(5) 1 calc PR B 1 O7 O 0.9528(13) 0.4690(4) -0.0111(7) 0.033(4) Uiso 0.158(5) 1 d P C -3 O8 O 0.669(2) 0.4741(7) -0.0152(11) 0.027(6) Uiso 0.088(5) 1 d P D -4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01319(8) 0.01797(9) 0.01497(8) -0.00046(6) 0.00170(6) 0.00138(6) N1 0.0131(8) 0.0203(8) 0.0205(8) 0.0005(7) 0.0041(6) 0.0022(7) C1 0.0166(10) 0.0241(11) 0.0205(10) -0.0015(8) 0.0037(8) 0.0025(8) C2 0.0205(11) 0.0283(12) 0.0251(11) -0.0070(9) 0.0038(9) 0.0012(9) C3 0.0207(11) 0.0214(11) 0.0385(13) -0.0064(9) 0.0077(9) -0.0027(9) C4 0.0202(11) 0.0221(11) 0.0340(12) 0.0039(9) 0.0060(9) 0.0003(9) C5 0.0146(10) 0.0229(10) 0.0224(10) 0.0025(8) 0.0065(8) 0.0025(8) C6 0.0154(10) 0.0236(10) 0.0212(10) 0.0052(8) 0.0048(8) 0.0039(8) C7 0.0131(9) 0.0265(11) 0.0164(9) -0.0003(8) 0.0041(7) 0.0045(8) N2 0.0174(9) 0.0285(10) 0.0236(9) 0.0079(8) 0.0038(7) 0.0031(8) C8 0.0262(12) 0.0297(12) 0.0357(13) 0.0131(10) 0.0053(10) 0.0019(10) N3 0.0189(9) 0.0326(10) 0.0197(9) 0.0056(8) 0.0038(7) 0.0036(8) N4 0.0157(8) 0.0290(10) 0.0179(8) 0.0027(7) 0.0039(7) 0.0032(7) C9 0.0187(10) 0.0316(12) 0.0184(10) -0.0019(9) 0.0009(8) -0.0005(9) C10 0.0303(13) 0.0495(16) 0.0256(12) -0.0040(11) -0.0058(10) 0.0042(12) C11 0.0275(12) 0.0403(14) 0.0301(12) -0.0065(10) 0.0097(10) 0.0024(11) N5 0.0185(9) 0.0190(8) 0.0190(8) -0.0027(7) 0.0038(7) -0.0016(7) C12 0.0200(10) 0.0216(10) 0.0206(10) -0.0023(8) 0.0055(8) -0.0022(9) C13 0.0319(13) 0.0309(12) 0.0244(11) 0.0070(9) 0.0033(9) 0.0077(10) N6 0.0161(8) 0.0238(9) 0.0193(8) -0.0001(7) 0.0017(7) 0.0037(7) C14 0.0218(11) 0.0222(11) 0.0243(10) -0.0019(9) -0.0014(9) 0.0047(9) C15 0.0407(15) 0.0233(12) 0.0418(14) -0.0081(10) -0.0154(12) 0.0013(11) N7 0.0170(9) 0.0212(9) 0.0185(8) -0.0013(7) -0.0002(7) -0.0002(7) C16 0.0189(10) 0.0224(10) 0.0205(10) -0.0050(8) 0.0006(8) -0.0017(8) C17 0.0213(11) 0.0344(13) 0.0327(12) -0.0091(10) 0.0113(9) -0.0049(10) N8 0.0171(9) 0.0196(8) 0.0173(8) 0.0003(7) -0.0008(7) 0.0010(7) C18 0.0182(10) 0.0181(10) 0.0191(9) -0.0028(8) 0.0009(8) -0.0012(8) C19 0.0195(11) 0.0292(12) 0.0274(11) -0.0062(9) 0.0094(9) 0.0000(9) O1 0.0523(12) 0.0496(12) 0.0387(10) -0.0110(9) 0.0153(9) 0.0034(10) O2 0.0317(9) 0.0294(9) 0.0380(9) -0.0013(7) 0.0015(7) -0.0093(7) O3 0.0464(11) 0.0301(9) 0.0483(11) 0.0076(8) -0.0001(9) 0.0048(8) S1 0.0304(3) 0.0223(3) 0.0311(3) -0.0006(2) 0.0036(2) 0.0001(2) C20 0.0260(12) 0.0260(12) 0.0427(14) -0.0072(10) 0.0066(10) -0.0033(10) F1 0.0403(9) 0.0387(9) 0.0497(9) -0.0046(7) -0.0077(7) 0.0078(7) F2 0.0409(9) 0.0472(9) 0.0463(9) -0.0218(7) 0.0072(7) -0.0008(7) F3 0.0399(9) 0.0513(10) 0.0778(12) -0.0046(9) 0.0157(9) -0.0254(8) O4 0.0244(9) 0.0534(12) 0.0364(10) -0.0007(8) -0.0050(7) -0.0025(8) O5 0.0505(12) 0.0443(11) 0.0445(11) 0.0066(9) 0.0167(9) -0.0115(9) O6A 0.0347(12) 0.0395(13) 0.0279(11) -0.0042(10) 0.0115(9) 0.0070(10) S2A 0.0214(4) 0.0305(5) 0.0180(5) 0.0007(3) 0.0030(3) -0.0008(3) C21A 0.0254(14) 0.0405(17) 0.0215(13) -0.0026(12) 0.0057(11) -0.0078(12) F4A 0.0516(14) 0.0512(13) 0.0410(13) -0.0221(12) 0.0261(11) -0.0126(10) F5A 0.0389(11) 0.0451(14) 0.0294(11) 0.0085(10) 0.0135(8) -0.0022(11) F6A 0.0297(11) 0.084(2) 0.0245(10) -0.0038(13) -0.0006(8) -0.0182(14) O6B 0.069(11) 0.027(7) 0.077(12) -0.022(8) 0.045(11) -0.004(7) S2B 0.029(2) 0.036(3) 0.041(3) -0.011(2) 0.017(2) -0.0110(19) C21B 0.030(8) 0.043(10) 0.033(8) -0.006(7) 0.005(7) -0.010(7) F4B 0.058(8) 0.068(9) 0.080(10) -0.017(8) 0.026(7) 0.026(7) F5B 0.036(7) 0.062(9) 0.036(6) -0.008(6) -0.009(5) -0.017(7) F6B 0.059(8) 0.026(6) 0.055(8) -0.003(6) 0.025(6) -0.004(6) N9 0.095(3) 0.053(2) 0.057(2) 0.0046(18) 0.027(2) 0.004(2) C22 0.075(3) 0.0198(16) 0.0351(19) 0.0033(14) -0.0012(18) 0.0092(17) C23 0.061(3) 0.052(3) 0.046(2) 0.0098(19) 0.0147(19) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C7 2.002(2) . ? Ru N8 2.0217(18) . ? Ru N7 2.0266(18) . ? Ru N6 2.0298(18) . ? Ru N1 2.0913(17) . ? Ru N5 2.1196(17) . ? N1 C1 1.345(3) . ? N1 C5 1.374(3) . ? C1 C2 1.381(3) . ? C1 H1 0.9500 . ? C2 C3 1.381(3) . ? C2 H2 0.9500 . ? C3 C4 1.392(3) . ? C3 H3 0.9500 . ? C4 C5 1.383(3) . ? C4 H4 0.9500 . ? C5 C6 1.452(3) . ? C6 N2 1.364(3) . ? C6 C7 1.383(3) . ? C7 N4 1.365(2) . ? N2 N3 1.322(3) . ? N2 C8 1.461(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N3 N4 1.338(2) . ? N4 C9 1.485(3) . ? C9 C10 1.514(3) . ? C9 C11 1.518(3) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N5 C12 1.139(3) . ? C12 C13 1.460(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? N6 C14 1.139(3) . ? C14 C15 1.455(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N7 C16 1.135(3) . ? C16 C17 1.461(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? N8 C18 1.141(3) . ? C18 C19 1.455(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O1 S1 1.4378(19) . ? O2 S1 1.4410(18) . ? O3 S1 1.4353(18) . ? S1 C20 1.820(2) . ? C20 F3 1.330(3) . ? C20 F2 1.331(3) . ? C20 F1 1.338(3) . ? O4 S2A 1.4241(19) . ? O4 S2B 1.454(6) . ? O5 S2A 1.418(2) . ? O5 S2B 1.471(6) . ? O6A S2A 1.446(3) . ? S2A C21A 1.812(3) . ? C21A F5A 1.334(4) . ? C21A F4A 1.334(4) . ? C21A F6A 1.339(4) . ? O6B S2B 1.40(2) . ? S2B C21B 1.809(19) . ? C21B F5B 1.30(2) . ? C21B F6B 1.31(2) . ? C21B F4B 1.33(2) . ? N9 C22 1.125(5) . ? C22 C23 1.400(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? 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 C7 Ru N8 87.29(7) . . ? C7 Ru N7 95.48(7) . . ? N8 Ru N7 177.22(7) . . ? C7 Ru N6 96.54(8) . . ? N8 Ru N6 91.13(7) . . ? N7 Ru N6 88.38(7) . . ? C7 Ru N1 78.61(7) . . ? N8 Ru N1 91.54(7) . . ? N7 Ru N1 89.19(7) . . ? N6 Ru N1 174.34(6) . . ? C7 Ru N5 170.31(7) . . ? N8 Ru N5 86.41(7) . . ? N7 Ru N5 90.86(7) . . ? N6 Ru N5 90.94(6) . . ? N1 Ru N5 94.20(6) . . ? C1 N1 C5 118.06(18) . . ? C1 N1 Ru 124.45(14) . . ? C5 N1 Ru 117.45(13) . . ? N1 C1 C2 122.6(2) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.5(2) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 118.8(2) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.4(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N1 C5 C4 121.63(19) . . ? N1 C5 C6 109.74(18) . . ? C4 C5 C6 128.62(19) . . ? N2 C6 C7 107.80(18) . . ? N2 C6 C5 133.0(2) . . ? C7 C6 C5 119.20(18) . . ? N4 C7 C6 102.57(17) . . ? N4 C7 Ru 141.90(16) . . ? C6 C7 Ru 114.74(14) . . ? N3 N2 C6 111.37(18) . . ? N3 N2 C8 118.14(18) . . ? C6 N2 C8 130.5(2) . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 N3 N4 104.07(16) . . ? N3 N4 C7 114.20(17) . . ? N3 N4 C9 118.81(16) . . ? C7 N4 C9 126.98(18) . . ? N4 C9 C10 111.50(19) . . ? N4 C9 C11 109.76(18) . . ? C10 C9 C11 112.21(19) . . ? N4 C9 H9 107.7 . . ? C10 C9 H9 107.7 . . ? C11 C9 H9 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 N5 Ru 171.95(17) . . ? N5 C12 C13 178.8(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C14 N6 Ru 174.44(17) . . ? N6 C14 C15 176.5(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C16 N7 Ru 174.86(18) . . ? N7 C16 C17 178.0(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C18 N8 Ru 178.66(17) . . ? N8 C18 C19 178.4(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O3 S1 O1 115.47(12) . . ? O3 S1 O2 114.53(12) . . ? O1 S1 O2 115.08(12) . . ? O3 S1 C20 103.30(11) . . ? O1 S1 C20 103.18(12) . . ? O2 S1 C20 102.80(11) . . ? F3 C20 F2 107.0(2) . . ? F3 C20 F1 107.4(2) . . ? F2 C20 F1 107.6(2) . . ? F3 C20 S1 111.68(18) . . ? F2 C20 S1 111.46(16) . . ? F1 C20 S1 111.51(16) . . ? O5 S2A O4 117.09(13) . . ? O5 S2A O6A 113.50(14) . . ? O4 S2A O6A 114.05(14) . . ? O5 S2A C21A 102.71(14) . . ? O4 S2A C21A 104.60(14) . . ? O6A S2A C21A 102.51(15) . . ? F5A C21A F4A 107.3(3) . . ? F5A C21A F6A 107.6(3) . . ? F4A C21A F6A 107.5(3) . . ? F5A C21A S2A 111.9(2) . . ? F4A C21A S2A 111.7(2) . . ? F6A C21A S2A 110.7(2) . . ? O6B S2B O4 109.2(8) . . ? O6B S2B O5 109.3(7) . . ? O4 S2B O5 111.9(5) . . ? O6B S2B C21B 104.3(12) . . ? O4 S2B C21B 105.0(6) . . ? O5 S2B C21B 116.7(7) . . ? F5B C21B F6B 109.2(15) . . ? F5B C21B F4B 106.1(15) . . ? F6B C21B F4B 105.6(16) . . ? F5B C21B S2B 112.3(13) . . ? F6B C21B S2B 113.2(12) . . ? F4B C21B S2B 109.9(13) . . ? N9 C22 C23 169.9(5) . . ? 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 C7 Ru N1 C1 175.68(17) . . . . ? N8 Ru N1 C1 -97.39(16) . . . . ? N7 Ru N1 C1 79.92(16) . . . . ? N5 Ru N1 C1 -10.88(17) . . . . ? C7 Ru N1 C5 -1.92(14) . . . . ? N8 Ru N1 C5 85.00(15) . . . . ? N7 Ru N1 C5 -97.68(15) . . . . ? N5 Ru N1 C5 171.52(14) . . . . ? C5 N1 C1 C2 -1.2(3) . . . . ? Ru N1 C1 C2 -178.81(15) . . . . ? N1 C1 C2 C3 0.1(3) . . . . ? C1 C2 C3 C4 1.0(3) . . . . ? C2 C3 C4 C5 -1.0(3) . . . . ? C1 N1 C5 C4 1.2(3) . . . . ? Ru N1 C5 C4 178.99(16) . . . . ? C1 N1 C5 C6 -178.30(17) . . . . ? Ru N1 C5 C6 -0.5(2) . . . . ? C3 C4 C5 N1 -0.1(3) . . . . ? C3 C4 C5 C6 179.3(2) . . . . ? N1 C5 C6 N2 -173.5(2) . . . . ? C4 C5 C6 N2 7.0(4) . . . . ? N1 C5 C6 C7 4.2(3) . . . . ? C4 C5 C6 C7 -175.3(2) . . . . ? N2 C6 C7 N4 0.1(2) . . . . ? C5 C6 C7 N4 -178.09(17) . . . . ? N2 C6 C7 Ru 172.22(13) . . . . ? C5 C6 C7 Ru -6.0(2) . . . . ? N8 Ru C7 N4 79.4(2) . . . . ? N7 Ru C7 N4 -100.4(2) . . . . ? N6 Ru C7 N4 -11.4(2) . . . . ? N1 Ru C7 N4 171.5(2) . . . . ? N8 Ru C7 C6 -88.03(16) . . . . ? N7 Ru C7 C6 92.14(16) . . . . ? N6 Ru C7 C6 -178.86(15) . . . . ? N1 Ru C7 C6 4.08(15) . . . . ? C7 C6 N2 N3 -0.2(2) . . . . ? C5 C6 N2 N3 177.7(2) . . . . ? C7 C6 N2 C8 177.7(2) . . . . ? C5 C6 N2 C8 -4.5(4) . . . . ? C6 N2 N3 N4 0.2(2) . . . . ? C8 N2 N3 N4 -177.96(18) . . . . ? N2 N3 N4 C7 -0.1(2) . . . . ? N2 N3 N4 C9 -179.00(17) . . . . ? C6 C7 N4 N3 0.0(2) . . . . ? Ru C7 N4 N3 -168.33(18) . . . . ? C6 C7 N4 C9 178.77(19) . . . . ? Ru C7 N4 C9 10.4(4) . . . . ? N3 N4 C9 C10 -27.4(3) . . . . ? C7 N4 C9 C10 153.9(2) . . . . ? N3 N4 C9 C11 97.6(2) . . . . ? C7 N4 C9 C11 -81.1(3) . . . . ? O3 S1 C20 F3 61.7(2) . . . . ? O1 S1 C20 F3 -58.9(2) . . . . ? O2 S1 C20 F3 -178.85(17) . . . . ? O3 S1 C20 F2 -57.9(2) . . . . ? O1 S1 C20 F2 -178.48(18) . . . . ? O2 S1 C20 F2 61.54(19) . . . . ? O3 S1 C20 F1 -178.11(18) . . . . ? O1 S1 C20 F1 61.3(2) . . . . ? O2 S1 C20 F1 -58.70(19) . . . . ? S2B O5 S2A O4 72.1(5) . . . . ? S2B O5 S2A O6A -151.7(5) . . . . ? S2B O5 S2A C21A -41.8(4) . . . . ? S2B O4 S2A O5 -73.2(5) . . . . ? S2B O4 S2A O6A 150.8(5) . . . . ? S2B O4 S2A C21A 39.6(5) . . . . ? O5 S2A C21A F5A 179.4(2) . . . . ? O4 S2A C21A F5A 56.6(2) . . . . ? O6A S2A C21A F5A -62.6(2) . . . . ? O5 S2A C21A F4A 59.2(2) . . . . ? O4 S2A C21A F4A -63.6(2) . . . . ? O6A S2A C21A F4A 177.1(2) . . . . ? O5 S2A C21A F6A -60.5(3) . . . . ? O4 S2A C21A F6A 176.7(3) . . . . ? O6A S2A C21A F6A 57.4(3) . . . . ? S2A O4 S2B O6B -176.6(11) . . . . ? S2A O4 S2B O5 62.3(6) . . . . ? S2A O4 S2B C21B -65.3(7) . . . . ? S2A O5 S2B O6B 175.6(12) . . . . ? S2A O5 S2B O4 -63.4(6) . . . . ? S2A O5 S2B C21B 57.6(8) . . . . ? O6B S2B C21B F5B -64.9(15) . . . . ? O4 S2B C21B F5B -179.7(13) . . . . ? O5 S2B C21B F5B 55.8(15) . . . . ? O6B S2B C21B F6B 59.4(14) . . . . ? O4 S2B C21B F6B -55.4(13) . . . . ? O5 S2B C21B F6B -180.0(12) . . . . ? O6B S2B C21B F4B 177.2(13) . . . . ? O4 S2B C21B F4B 62.4(13) . . . . ? O5 S2B C21B F4B -62.1(13) . . . . ? _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.883 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.075 #===END data_alb89(2c) _database_code_depnum_ccdc_archive 'CCDC 817675' #TrackingRef 'alb09pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H28 Cl N4 Ru, C F3 O3 S, C2 H3 N' _chemical_formula_sum 'C24 H31 Cl F3 N5 O3 Ru S' _chemical_formula_weight 663.12 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' F F 0.0171 0.0103 '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' 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 'P 21/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 9.2210(1) _cell_length_b 10.6901(1) _cell_length_c 27.7904(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.849(1) _cell_angle_gamma 90.00 _cell_volume 2736.01(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17905 _cell_measurement_theta_min 3.2117 _cell_measurement_theta_max 29.8329 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2514 _exptl_crystal_size_mid 0.2154 _exptl_crystal_size_min 0.1275 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.803 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 0.918 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46079 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 29.90 _reflns_number_total 7126 _reflns_number_gt 6116 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^)+(0.0136P)^2^+2.3089P] 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 7126 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0502 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.004 _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 Ru Ru 1.017358(14) 0.774929(12) 0.113855(5) 0.00752(4) Uani 1 1 d . . . Cl Cl 1.08615(4) 0.82550(4) 0.033967(14) 0.01250(9) Uani 1 1 d . . . N1 N 1.09747(15) 0.59403(13) 0.09809(5) 0.0094(3) Uani 1 1 d . . . C1 C 1.23587(19) 0.55983(16) 0.10813(6) 0.0124(3) Uani 1 1 d . . . H1 H 1.2984 0.6162 0.1255 0.015 Uiso 1 1 calc R . . C2 C 1.29097(19) 0.44608(16) 0.09419(6) 0.0142(4) Uani 1 1 d . . . H2 H 1.3892 0.4246 0.1022 0.017 Uiso 1 1 calc R . . C3 C 1.20093(19) 0.36384(16) 0.06844(6) 0.0136(4) Uani 1 1 d . . . H3 H 1.2374 0.2858 0.0580 0.016 Uiso 1 1 calc R . . C4 C 1.05697(19) 0.39618(16) 0.05799(6) 0.0116(3) Uani 1 1 d . . . H4 H 0.9933 0.3405 0.0407 0.014 Uiso 1 1 calc R . . C5 C 1.00788(18) 0.51169(15) 0.07333(6) 0.0095(3) Uani 1 1 d . . . C6 C 0.86580(18) 0.56824(15) 0.06501(6) 0.0091(3) Uani 1 1 d . . . C7 C 0.84579(18) 0.69052(16) 0.07946(6) 0.0096(3) Uani 1 1 d . . . N2 N 0.74035(15) 0.52964(13) 0.04198(5) 0.0099(3) Uani 1 1 d . . . C8 C 0.70181(19) 0.40860(16) 0.02040(6) 0.0139(4) Uani 1 1 d . . . H8A H 0.6045 0.4136 0.0046 0.021 Uiso 1 1 calc R . . H8B H 0.7028 0.3444 0.0456 0.021 Uiso 1 1 calc R . . H8C H 0.7723 0.3867 -0.0035 0.021 Uiso 1 1 calc R . . N3 N 0.64192(15) 0.61980(13) 0.04029(5) 0.0116(3) Uani 1 1 d . . . N4 N 0.70800(15) 0.71630(13) 0.06306(5) 0.0098(3) Uani 1 1 d . . . C9 C 0.63441(19) 0.84024(16) 0.06394(6) 0.0126(3) Uani 1 1 d . . . H9 H 0.6657 0.8826 0.0948 0.015 Uiso 1 1 calc R . . C10 C 0.6842(2) 0.92003(19) 0.02300(8) 0.0244(4) Uani 1 1 d . . . H10A H 0.7905 0.9209 0.0236 0.037 Uiso 1 1 calc R . . H10B H 0.6481 1.0056 0.0266 0.037 Uiso 1 1 calc R . . H10C H 0.6462 0.8853 -0.0077 0.037 Uiso 1 1 calc R . . C11 C 0.4717(2) 0.82582(19) 0.06309(9) 0.0260(5) Uani 1 1 d . . . H11A H 0.4369 0.7921 0.0318 0.039 Uiso 1 1 calc R . . H11B H 0.4269 0.9076 0.0682 0.039 Uiso 1 1 calc R . . H11C H 0.4456 0.7684 0.0887 0.039 Uiso 1 1 calc R . . C12 C 0.97362(19) 0.76140(16) 0.19101(6) 0.0114(3) Uani 1 1 d . . . C18 C 0.9057(2) 0.65543(17) 0.21808(6) 0.0161(4) Uani 1 1 d . . . H18 H 0.8151 0.6303 0.1993 0.019 Uiso 1 1 calc R . . C19 C 0.8606(2) 0.70256(19) 0.26712(7) 0.0218(4) Uani 1 1 d . . . H19A H 0.9474 0.7244 0.2871 0.033 Uiso 1 1 calc R . . H19B H 0.8066 0.6368 0.2831 0.033 Uiso 1 1 calc R . . H19C H 0.7989 0.7767 0.2626 0.033 Uiso 1 1 calc R . . C20 C 1.0012(2) 0.53945(18) 0.22356(7) 0.0256(5) Uani 1 1 d . . . H20A H 1.0302 0.5123 0.1918 0.038 Uiso 1 1 calc R . . H20B H 0.9468 0.4723 0.2385 0.038 Uiso 1 1 calc R . . H20C H 1.0879 0.5592 0.2439 0.038 Uiso 1 1 calc R . . C13 C 1.12576(18) 0.77571(16) 0.18604(6) 0.0121(3) Uani 1 1 d . . . H13 H 1.1897 0.7148 0.2002 0.014 Uiso 1 1 calc R . . C14 C 1.18512(19) 0.87672(16) 0.16096(6) 0.0128(3) Uani 1 1 d . . . H14 H 1.2874 0.8853 0.1597 0.015 Uiso 1 1 calc R . . C15 C 1.0913(2) 0.96543(16) 0.13761(6) 0.0134(4) Uani 1 1 d . . . C21 C 1.1496(2) 1.06853(17) 0.10766(7) 0.0192(4) Uani 1 1 d . . . H21A H 1.0804 1.0867 0.0807 0.029 Uiso 1 1 calc R . . H21B H 1.2426 1.0427 0.0952 0.029 Uiso 1 1 calc R . . H21C H 1.1641 1.1437 0.1275 0.029 Uiso 1 1 calc R . . C16 C 0.93947(19) 0.95388(16) 0.14194(6) 0.0122(3) Uani 1 1 d . . . H16 H 0.8756 1.0140 0.1272 0.015 Uiso 1 1 calc R . . C17 C 0.88266(19) 0.85289(16) 0.16815(6) 0.0119(3) Uani 1 1 d . . . H17 H 0.7805 0.8463 0.1705 0.014 Uiso 1 1 calc R . . N5 N 0.4928(2) 0.6825(2) 0.19098(8) 0.0399(5) Uani 1 1 d . . . C23 C 0.4988(2) 0.5959(2) 0.21468(8) 0.0277(5) Uani 1 1 d . . . C24 C 0.5065(3) 0.4834(2) 0.24411(8) 0.0355(5) Uani 1 1 d . . . H24A H 0.4611 0.4137 0.2261 0.053 Uiso 1 1 calc R . . H24B H 0.4551 0.4974 0.2737 0.053 Uiso 1 1 calc R . . H24C H 0.6083 0.4632 0.2524 0.053 Uiso 1 1 calc R . . O1 O 0.61481(15) 0.05704(12) 0.14776(5) 0.0229(3) Uani 1 1 d . . . O2 O 0.44869(14) 0.22092(13) 0.17044(5) 0.0218(3) Uani 1 1 d . . . O3 O 0.52676(15) 0.20936(13) 0.08819(5) 0.0225(3) Uani 1 1 d . . . S S 0.55684(5) 0.18034(4) 0.138333(16) 0.01503(9) Uani 1 1 d . . . C22 C 0.7112(2) 0.28181(18) 0.15483(7) 0.0178(4) Uani 1 1 d . . . F1 F 0.82627(12) 0.25702(11) 0.12879(4) 0.0274(3) Uani 1 1 d . . . F2 F 0.75350(13) 0.26933(12) 0.20127(4) 0.0309(3) Uani 1 1 d . . . F3 F 0.67796(13) 0.40281(10) 0.14741(4) 0.0269(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.00736(7) 0.00695(7) 0.00816(6) -0.00047(5) -0.00036(5) 0.00039(5) Cl 0.0147(2) 0.0126(2) 0.01037(18) -0.00020(16) 0.00225(15) -0.00057(16) N1 0.0095(7) 0.0098(7) 0.0088(7) 0.0011(6) -0.0004(5) 0.0008(5) C1 0.0118(9) 0.0134(9) 0.0117(8) 0.0015(7) -0.0015(7) 0.0002(7) C2 0.0107(9) 0.0147(9) 0.0173(9) 0.0046(7) 0.0016(7) 0.0038(7) C3 0.0168(9) 0.0094(8) 0.0151(8) 0.0028(7) 0.0051(7) 0.0030(7) C4 0.0140(9) 0.0092(8) 0.0118(8) 0.0008(7) 0.0015(7) -0.0007(6) C5 0.0103(8) 0.0100(8) 0.0083(7) 0.0016(6) 0.0016(6) -0.0003(6) C6 0.0091(8) 0.0105(8) 0.0078(7) 0.0003(6) 0.0001(6) -0.0009(6) C7 0.0079(8) 0.0123(8) 0.0087(7) 0.0013(6) 0.0008(6) 0.0000(6) N2 0.0100(7) 0.0088(7) 0.0109(7) -0.0014(6) -0.0003(5) -0.0005(5) C8 0.0148(9) 0.0098(8) 0.0168(9) -0.0040(7) -0.0019(7) -0.0021(7) N3 0.0102(7) 0.0115(7) 0.0129(7) -0.0017(6) 0.0001(6) 0.0004(6) N4 0.0090(7) 0.0091(7) 0.0114(7) -0.0007(6) -0.0004(5) 0.0000(5) C9 0.0122(9) 0.0101(8) 0.0154(8) -0.0016(7) -0.0015(7) 0.0041(6) C10 0.0235(11) 0.0186(10) 0.0321(11) 0.0102(9) 0.0102(9) 0.0080(8) C11 0.0106(9) 0.0169(10) 0.0509(14) 0.0025(10) 0.0071(9) 0.0054(7) C12 0.0134(8) 0.0131(8) 0.0078(7) -0.0025(7) 0.0006(6) -0.0008(7) C18 0.0167(9) 0.0169(9) 0.0145(8) 0.0026(7) 0.0000(7) -0.0055(7) C19 0.0242(11) 0.0258(11) 0.0157(9) 0.0046(8) 0.0055(8) -0.0030(8) C20 0.0376(13) 0.0161(10) 0.0237(10) 0.0066(8) 0.0071(9) 0.0010(9) C13 0.0128(8) 0.0133(8) 0.0096(8) -0.0022(7) -0.0031(6) 0.0018(7) C14 0.0112(8) 0.0151(9) 0.0121(8) -0.0052(7) -0.0006(7) -0.0023(7) C15 0.0206(9) 0.0090(8) 0.0109(8) -0.0039(7) 0.0023(7) -0.0027(7) C21 0.0283(11) 0.0133(9) 0.0166(9) -0.0012(8) 0.0054(8) -0.0056(8) C16 0.0165(9) 0.0096(8) 0.0106(8) -0.0018(7) 0.0009(7) 0.0034(7) C17 0.0105(8) 0.0156(9) 0.0097(8) -0.0044(7) 0.0013(6) 0.0008(7) N5 0.0365(12) 0.0404(12) 0.0411(12) -0.0010(10) -0.0170(9) 0.0070(9) C23 0.0176(10) 0.0352(13) 0.0295(11) -0.0113(10) -0.0058(9) 0.0038(9) C24 0.0459(15) 0.0319(12) 0.0290(12) -0.0094(10) 0.0061(11) -0.0015(11) O1 0.0268(8) 0.0140(7) 0.0286(8) 0.0023(6) 0.0075(6) 0.0045(6) O2 0.0170(7) 0.0234(7) 0.0256(7) -0.0029(6) 0.0081(6) 0.0023(6) O3 0.0230(7) 0.0267(8) 0.0176(7) 0.0002(6) -0.0018(6) -0.0001(6) S 0.0149(2) 0.0140(2) 0.0164(2) -0.00030(18) 0.00265(17) 0.00188(17) C22 0.0178(9) 0.0187(9) 0.0170(9) 0.0009(8) 0.0003(7) 0.0016(8) F1 0.0157(6) 0.0331(7) 0.0340(7) 0.0024(5) 0.0078(5) 0.0002(5) F2 0.0284(7) 0.0419(7) 0.0214(6) 0.0010(6) -0.0080(5) -0.0036(6) F3 0.0306(7) 0.0145(6) 0.0357(7) -0.0012(5) 0.0021(5) -0.0015(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 Ru C7 2.0201(16) . ? Ru N1 2.1236(14) . ? Ru C17 2.1680(17) . ? Ru C13 2.1964(16) . ? Ru C16 2.2000(17) . ? Ru C12 2.2062(16) . ? Ru C15 2.2369(17) . ? Ru C14 2.2560(17) . ? Ru Cl 2.4007(4) . ? N1 C1 1.343(2) . ? N1 C5 1.369(2) . ? C1 C2 1.381(2) . ? C1 H1 0.9500 . ? C2 C3 1.384(3) . ? C2 H2 0.9500 . ? C3 C4 1.388(2) . ? C3 H3 0.9500 . ? C4 C5 1.389(2) . ? C4 H4 0.9500 . ? C5 C6 1.451(2) . ? C6 N2 1.358(2) . ? C6 C7 1.382(2) . ? C7 N4 1.357(2) . ? N2 N3 1.3231(19) . ? N2 C8 1.463(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N3 N4 1.341(2) . ? N4 C9 1.489(2) . ? C9 C11 1.507(2) . ? C9 C10 1.512(3) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.418(2) . ? C12 C13 1.425(2) . ? C12 C18 1.513(2) . ? C18 C20 1.524(3) . ? C18 C19 1.530(3) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C13 C14 1.410(2) . ? C13 H13 0.9500 . ? C14 C15 1.419(2) . ? C14 H14 0.9500 . ? C15 C16 1.417(3) . ? C15 C21 1.497(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C16 C17 1.417(2) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? N5 C23 1.135(3) . ? C23 C24 1.455(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? O1 S 1.4414(14) . ? O2 S 1.4377(13) . ? O3 S 1.4411(14) . ? S C22 1.830(2) . ? C22 F2 1.336(2) . ? C22 F1 1.340(2) . ? C22 F3 1.343(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 C7 Ru N1 76.58(6) . . ? C7 Ru C17 92.22(7) . . ? N1 Ru C17 135.31(6) . . ? C7 Ru C13 138.08(7) . . ? N1 Ru C13 92.57(6) . . ? C17 Ru C13 67.25(6) . . ? C7 Ru C16 107.13(7) . . ? N1 Ru C16 171.14(6) . . ? C17 Ru C16 37.86(6) . . ? C13 Ru C16 79.30(6) . . ? C7 Ru C12 104.71(6) . . ? N1 Ru C12 102.89(6) . . ? C17 Ru C12 37.82(6) . . ? C13 Ru C12 37.76(6) . . ? C16 Ru C12 68.50(6) . . ? C7 Ru C15 140.04(7) . . ? N1 Ru C15 141.80(6) . . ? C17 Ru C15 67.75(6) . . ? C13 Ru C15 66.97(6) . . ? C16 Ru C15 37.23(6) . . ? C12 Ru C15 80.83(6) . . ? C7 Ru C14 171.25(6) . . ? N1 Ru C14 108.87(6) . . ? C17 Ru C14 79.09(6) . . ? C13 Ru C14 36.90(6) . . ? C16 Ru C14 66.50(6) . . ? C12 Ru C14 67.72(6) . . ? C15 Ru C14 36.81(6) . . ? C7 Ru Cl 84.24(5) . . ? N1 Ru Cl 84.47(4) . . ? C17 Ru Cl 138.06(5) . . ? C13 Ru Cl 135.61(5) . . ? C16 Ru Cl 103.78(5) . . ? C12 Ru Cl 169.43(5) . . ? C15 Ru Cl 88.70(5) . . ? C14 Ru Cl 102.88(5) . . ? C1 N1 C5 118.21(14) . . ? C1 N1 Ru 122.79(11) . . ? C5 N1 Ru 118.80(11) . . ? N1 C1 C2 122.71(16) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 119.00(16) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 119.53(16) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 118.67(16) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 121.87(15) . . ? N1 C5 C6 109.25(14) . . ? C4 C5 C6 128.81(15) . . ? N2 C6 C7 107.54(14) . . ? N2 C6 C5 133.60(15) . . ? C7 C6 C5 118.69(15) . . ? N4 C7 C6 103.34(14) . . ? N4 C7 Ru 140.05(13) . . ? C6 C7 Ru 116.56(12) . . ? N3 N2 C6 111.23(13) . . ? N3 N2 C8 118.53(13) . . ? C6 N2 C8 130.24(14) . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 N3 N4 104.41(13) . . ? N3 N4 C7 113.47(14) . . ? N3 N4 C9 119.71(13) . . ? C7 N4 C9 126.52(14) . . ? N4 C9 C11 111.27(14) . . ? N4 C9 C10 109.50(14) . . ? C11 C9 C10 112.65(16) . . ? N4 C9 H9 107.7 . . ? C11 C9 H9 107.7 . . ? C10 C9 H9 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 116.48(15) . . ? C17 C12 C18 119.28(15) . . ? C13 C12 C18 124.23(15) . . ? C17 C12 Ru 69.63(9) . . ? C13 C12 Ru 70.75(9) . . ? C18 C12 Ru 129.24(12) . . ? C12 C18 C20 114.06(16) . . ? C12 C18 C19 109.51(15) . . ? C20 C18 C19 111.11(16) . . ? C12 C18 H18 107.3 . . ? C20 C18 H18 107.3 . . ? C19 C18 H18 107.3 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C13 C12 122.57(16) . . ? C14 C13 Ru 73.85(10) . . ? C12 C13 Ru 71.49(9) . . ? C14 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? Ru C13 H13 128.3 . . ? C13 C14 C15 119.67(16) . . ? C13 C14 Ru 69.25(9) . . ? C15 C14 Ru 70.86(10) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? Ru C14 H14 132.7 . . ? C16 C15 C14 119.05(16) . . ? C16 C15 C21 119.68(16) . . ? C14 C15 C21 121.26(17) . . ? C16 C15 Ru 69.97(10) . . ? C14 C15 Ru 72.33(10) . . ? C21 C15 Ru 128.23(12) . . ? C15 C21 H21A 109.5 . . ? C15 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C15 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C16 C17 120.15(16) . . ? C15 C16 Ru 72.80(10) . . ? C17 C16 Ru 69.85(9) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? Ru C16 H16 129.9 . . ? C16 C17 C12 122.01(16) . . ? C16 C17 Ru 72.30(10) . . ? C12 C17 Ru 72.55(10) . . ? C16 C17 H17 119.0 . . ? C12 C17 H17 119.0 . . ? Ru C17 H17 128.5 . . ? N5 C23 C24 178.8(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 S O3 115.40(8) . . ? O2 S O1 115.18(8) . . ? O3 S O1 115.12(8) . . ? O2 S C22 102.74(8) . . ? O3 S C22 102.98(8) . . ? O1 S C22 102.70(9) . . ? F2 C22 F1 107.50(15) . . ? F2 C22 F3 107.33(15) . . ? F1 C22 F3 106.76(15) . . ? F2 C22 S 111.65(13) . . ? F1 C22 S 111.99(13) . . ? F3 C22 S 111.34(13) . . ? 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 C7 Ru N1 C1 176.31(14) . . . . ? C17 Ru N1 C1 -104.32(14) . . . . ? C13 Ru N1 C1 -44.66(14) . . . . ? C12 Ru N1 C1 -81.38(14) . . . . ? C15 Ru N1 C1 10.14(18) . . . . ? C14 Ru N1 C1 -10.82(15) . . . . ? Cl Ru N1 C1 90.93(13) . . . . ? C7 Ru N1 C5 1.50(12) . . . . ? C17 Ru N1 C5 80.87(14) . . . . ? C13 Ru N1 C5 140.53(12) . . . . ? C12 Ru N1 C5 103.81(12) . . . . ? C15 Ru N1 C5 -164.67(11) . . . . ? C14 Ru N1 C5 174.37(12) . . . . ? Cl Ru N1 C5 -83.88(12) . . . . ? C5 N1 C1 C2 0.5(2) . . . . ? Ru N1 C1 C2 -174.32(13) . . . . ? N1 C1 C2 C3 0.6(3) . . . . ? C1 C2 C3 C4 -1.2(3) . . . . ? C2 C3 C4 C5 0.8(3) . . . . ? C1 N1 C5 C4 -1.0(2) . . . . ? Ru N1 C5 C4 174.06(12) . . . . ? C1 N1 C5 C6 -178.20(14) . . . . ? Ru N1 C5 C6 -3.15(17) . . . . ? C3 C4 C5 N1 0.3(2) . . . . ? C3 C4 C5 C6 176.97(16) . . . . ? N1 C5 C6 N2 178.52(17) . . . . ? C4 C5 C6 N2 1.6(3) . . . . ? N1 C5 C6 C7 3.8(2) . . . . ? C4 C5 C6 C7 -173.17(17) . . . . ? N2 C6 C7 N4 -0.78(18) . . . . ? C5 C6 C7 N4 175.21(14) . . . . ? N2 C6 C7 Ru -178.78(11) . . . . ? C5 C6 C7 Ru -2.8(2) . . . . ? N1 Ru C7 N4 -176.3(2) . . . . ? C17 Ru C7 N4 47.51(19) . . . . ? C13 Ru C7 N4 105.10(19) . . . . ? C16 Ru C7 N4 12.1(2) . . . . ? C12 Ru C7 N4 83.69(19) . . . . ? C15 Ru C7 N4 -9.6(2) . . . . ? Cl Ru C7 N4 -90.59(19) . . . . ? N1 Ru C7 C6 0.72(12) . . . . ? C17 Ru C7 C6 -135.51(13) . . . . ? C13 Ru C7 C6 -77.92(16) . . . . ? C16 Ru C7 C6 -170.93(12) . . . . ? C12 Ru C7 C6 -99.33(13) . . . . ? C15 Ru C7 C6 167.42(11) . . . . ? Cl Ru C7 C6 86.39(12) . . . . ? C7 C6 N2 N3 0.71(19) . . . . ? C5 C6 N2 N3 -174.44(17) . . . . ? C7 C6 N2 C8 -178.86(16) . . . . ? C5 C6 N2 C8 6.0(3) . . . . ? C6 N2 N3 N4 -0.31(18) . . . . ? C8 N2 N3 N4 179.32(14) . . . . ? N2 N3 N4 C7 -0.22(18) . . . . ? N2 N3 N4 C9 173.84(13) . . . . ? C6 C7 N4 N3 0.63(18) . . . . ? Ru C7 N4 N3 177.86(14) . . . . ? C6 C7 N4 C9 -172.95(15) . . . . ? Ru C7 N4 C9 4.3(3) . . . . ? N3 N4 C9 C11 30.9(2) . . . . ? C7 N4 C9 C11 -155.88(17) . . . . ? N3 N4 C9 C10 -94.30(18) . . . . ? C7 N4 C9 C10 78.9(2) . . . . ? C7 Ru C12 C17 -74.16(11) . . . . ? N1 Ru C12 C17 -153.44(10) . . . . ? C13 Ru C12 C17 129.30(15) . . . . ? C16 Ru C12 C17 28.77(10) . . . . ? C15 Ru C12 C17 65.33(10) . . . . ? C14 Ru C12 C17 101.21(11) . . . . ? Cl Ru C12 C17 73.1(3) . . . . ? C7 Ru C12 C13 156.53(10) . . . . ? N1 Ru C12 C13 77.26(10) . . . . ? C17 Ru C12 C13 -129.30(15) . . . . ? C16 Ru C12 C13 -100.53(11) . . . . ? C15 Ru C12 C13 -63.97(10) . . . . ? C14 Ru C12 C13 -28.09(10) . . . . ? Cl Ru C12 C13 -56.2(3) . . . . ? C7 Ru C12 C18 37.58(17) . . . . ? N1 Ru C12 C18 -41.69(16) . . . . ? C17 Ru C12 C18 111.74(19) . . . . ? C13 Ru C12 C18 -119.0(2) . . . . ? C16 Ru C12 C18 140.51(17) . . . . ? C15 Ru C12 C18 177.07(16) . . . . ? C14 Ru C12 C18 -147.05(17) . . . . ? Cl Ru C12 C18 -175.14(16) . . . . ? C17 C12 C18 C20 156.88(16) . . . . ? C13 C12 C18 C20 -22.2(2) . . . . ? Ru C12 C18 C20 70.2(2) . . . . ? C17 C12 C18 C19 -77.9(2) . . . . ? C13 C12 C18 C19 103.04(19) . . . . ? Ru C12 C18 C19 -164.62(13) . . . . ? C17 C12 C13 C14 1.7(2) . . . . ? C18 C12 C13 C14 -179.25(16) . . . . ? Ru C12 C13 C14 55.81(15) . . . . ? C17 C12 C13 Ru -54.14(13) . . . . ? C18 C12 C13 Ru 124.95(16) . . . . ? C7 Ru C13 C14 -168.68(10) . . . . ? N1 Ru C13 C14 118.65(10) . . . . ? C17 Ru C13 C14 -102.51(11) . . . . ? C16 Ru C13 C14 -64.89(10) . . . . ? C12 Ru C13 C14 -133.47(15) . . . . ? C15 Ru C13 C14 -28.04(10) . . . . ? Cl Ru C13 C14 33.94(13) . . . . ? C7 Ru C13 C12 -35.20(14) . . . . ? N1 Ru C13 C12 -107.87(10) . . . . ? C17 Ru C13 C12 30.96(10) . . . . ? C16 Ru C13 C12 68.58(10) . . . . ? C15 Ru C13 C12 105.43(11) . . . . ? C14 Ru C13 C12 133.47(15) . . . . ? Cl Ru C13 C12 167.41(8) . . . . ? C12 C13 C14 C15 -3.0(2) . . . . ? Ru C13 C14 C15 51.73(14) . . . . ? C12 C13 C14 Ru -54.74(14) . . . . ? N1 Ru C14 C13 -67.89(11) . . . . ? C17 Ru C14 C13 66.47(10) . . . . ? C16 Ru C14 C13 104.01(11) . . . . ? C12 Ru C14 C13 28.70(10) . . . . ? C15 Ru C14 C13 133.77(15) . . . . ? Cl Ru C14 C13 -156.38(9) . . . . ? N1 Ru C14 C15 158.34(10) . . . . ? C17 Ru C14 C15 -67.30(11) . . . . ? C13 Ru C14 C15 -133.77(15) . . . . ? C16 Ru C14 C15 -29.77(10) . . . . ? C12 Ru C14 C15 -105.07(11) . . . . ? Cl Ru C14 C15 69.85(10) . . . . ? C13 C14 C15 C16 3.0(2) . . . . ? Ru C14 C15 C16 53.98(14) . . . . ? C13 C14 C15 C21 -175.49(16) . . . . ? Ru C14 C15 C21 -124.50(16) . . . . ? C13 C14 C15 Ru -51.00(14) . . . . ? C7 Ru C15 C16 35.64(15) . . . . ? N1 Ru C15 C16 -165.58(10) . . . . ? C17 Ru C15 C16 -29.34(10) . . . . ? C13 Ru C15 C16 -103.08(11) . . . . ? C12 Ru C15 C16 -66.35(10) . . . . ? C14 Ru C15 C16 -131.19(15) . . . . ? Cl Ru C15 C16 115.07(9) . . . . ? C7 Ru C15 C14 166.83(11) . . . . ? N1 Ru C15 C14 -34.39(15) . . . . ? C17 Ru C15 C14 101.84(11) . . . . ? C13 Ru C15 C14 28.11(10) . . . . ? C16 Ru C15 C14 131.19(15) . . . . ? C12 Ru C15 C14 64.83(10) . . . . ? Cl Ru C15 C14 -113.74(10) . . . . ? C7 Ru C15 C21 -76.93(19) . . . . ? N1 Ru C15 C21 81.86(19) . . . . ? C17 Ru C15 C21 -141.91(18) . . . . ? C13 Ru C15 C21 144.36(18) . . . . ? C16 Ru C15 C21 -112.6(2) . . . . ? C12 Ru C15 C21 -178.92(17) . . . . ? C14 Ru C15 C21 116.2(2) . . . . ? Cl Ru C15 C21 2.51(16) . . . . ? C14 C15 C16 C17 -1.8(2) . . . . ? C21 C15 C16 C17 176.75(15) . . . . ? Ru C15 C16 C17 53.36(14) . . . . ? C14 C15 C16 Ru -55.11(14) . . . . ? C21 C15 C16 Ru 123.39(15) . . . . ? C7 Ru C16 C15 -156.94(10) . . . . ? C17 Ru C16 C15 132.35(15) . . . . ? C13 Ru C16 C15 65.82(10) . . . . ? C12 Ru C16 C15 103.60(11) . . . . ? C14 Ru C16 C15 29.45(10) . . . . ? Cl Ru C16 C15 -68.81(10) . . . . ? C7 Ru C16 C17 70.71(11) . . . . ? C13 Ru C16 C17 -66.53(10) . . . . ? C12 Ru C16 C17 -28.75(10) . . . . ? C15 Ru C16 C17 -132.35(15) . . . . ? C14 Ru C16 C17 -102.89(11) . . . . ? Cl Ru C16 C17 158.84(9) . . . . ? C15 C16 C17 C12 0.5(2) . . . . ? Ru C16 C17 C12 55.19(14) . . . . ? C15 C16 C17 Ru -54.73(14) . . . . ? C13 C12 C17 C16 -0.4(2) . . . . ? C18 C12 C17 C16 -179.51(15) . . . . ? Ru C12 C17 C16 -55.08(14) . . . . ? C13 C12 C17 Ru 54.70(13) . . . . ? C18 C12 C17 Ru -124.43(15) . . . . ? C7 Ru C17 C16 -115.49(10) . . . . ? N1 Ru C17 C16 171.43(9) . . . . ? C13 Ru C17 C16 102.21(11) . . . . ? C12 Ru C17 C16 133.13(15) . . . . ? C15 Ru C17 C16 28.89(10) . . . . ? C14 Ru C17 C16 65.56(10) . . . . ? Cl Ru C17 C16 -31.64(13) . . . . ? C7 Ru C17 C12 111.38(10) . . . . ? N1 Ru C17 C12 38.30(13) . . . . ? C13 Ru C17 C12 -30.92(10) . . . . ? C16 Ru C17 C12 -133.13(15) . . . . ? C15 Ru C17 C12 -104.25(11) . . . . ? C14 Ru C17 C12 -67.57(10) . . . . ? Cl Ru C17 C12 -164.77(8) . . . . ? O2 S C22 F2 58.60(15) . . . . ? O3 S C22 F2 178.83(13) . . . . ? O1 S C22 F2 -61.28(15) . . . . ? O2 S C22 F1 179.21(13) . . . . ? O3 S C22 F1 -60.56(14) . . . . ? O1 S C22 F1 59.33(14) . . . . ? O2 S C22 F3 -61.34(14) . . . . ? O3 S C22 F3 58.89(14) . . . . ? O1 S C22 F3 178.78(13) . . . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.499 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.082