# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Sven Rau' _publ_contact_author_email SVEN.RAU@CHEMIE.UNI-ERLANGEN.DE _publ_section_title ; Synthesis and Characterization of Regioselective Substituted Tetrapyridophenazine Ligands and their Ru(II) Complexes ; loop_ _publ_author_name 'Sven Rau' 'Benjamin Dietzek' 'Helmar Gorls' 'Frank W Heinemann' 'Michael Karnahl' 'Sven Krieck' ; C.Kuhnt ; 'J Popp' 'Michael Schmitt' 'Matthias Schwalbe' 'Stefanie Tschierlei' #===END OF ALL DATA # Attachment 'dalton_7.cif' data_FO3019 _database_code_depnum_ccdc_archive 'CCDC 721368' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C60 H58 Br2 N10 Ru),3(C3 H6 O),4(F6 P)' _chemical_formula_sum 'C64.50 H67 Br2 F12 N10 O1.50 P2 Ru' _chemical_formula_weight 1557.11 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' O O 0.0106 0.0060 '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' Br Br -0.2901 2.4595 '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 -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3267(5) _cell_length_b 18.3922(12) _cell_length_c 20.7064(13) _cell_angle_alpha 96.501(2) _cell_angle_beta 102.542(4) _cell_angle_gamma 106.290(4) _cell_volume 3620.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 23385 _cell_measurement_theta_min 4.29 _cell_measurement_theta_max 27.52 _exptl_crystal_description prism _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 1.442 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23385 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.1174 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.29 _diffrn_reflns_theta_max 27.52 _reflns_number_total 15657 _reflns_number_gt 8511 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1073P)^2^+9.6169P] 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 15657 _refine_ls_number_parameters 900 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1740 _refine_ls_R_factor_gt 0.0906 _refine_ls_wR_factor_ref 0.2620 _refine_ls_wR_factor_gt 0.2126 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.78158(6) 0.24638(4) 0.75141(3) 0.0433(2) Uani 1 1 d . . . Br1 Br 1.44890(10) 0.37180(6) 0.36662(5) 0.0707(3) Uani 1 1 d . . . Br2 Br 1.14547(13) 0.82834(6) 0.58634(6) 0.0817(3) Uani 1 1 d . . . N1 N 0.9134(6) 0.2462(4) 0.6890(3) 0.0451(14) Uani 1 1 d . . . N2 N 0.8247(6) 0.3581(3) 0.7346(3) 0.0437(14) Uani 1 1 d . . . N3 N 1.1543(6) 0.4062(3) 0.5542(3) 0.0415(14) Uani 1 1 d . . . N4 N 1.0700(6) 0.5271(3) 0.6090(3) 0.0438(14) Uani 1 1 d . . . N5 N 1.3905(7) 0.5774(4) 0.4247(3) 0.0557(17) Uani 1 1 d . . . N6 N 1.3034(7) 0.6924(4) 0.4778(4) 0.0588(18) Uani 1 1 d . . . N7 N 0.6127(6) 0.1979(3) 0.6691(3) 0.0440(14) Uani 1 1 d . . . N8 N 0.7349(7) 0.1311(4) 0.7568(3) 0.0481(15) Uani 1 1 d . . . N9 N 0.6616(6) 0.2497(4) 0.8189(3) 0.0439(14) Uani 1 1 d . . . N10 N 0.9357(6) 0.2895(4) 0.8416(3) 0.0483(15) Uani 1 1 d . . . C1 C 0.9611(9) 0.1899(5) 0.6701(4) 0.054(2) Uani 1 1 d . . . H1A H 0.9339 0.1431 0.6862 0.065 Uiso 1 1 calc R . . C2 C 1.0496(9) 0.1963(5) 0.6274(4) 0.055(2) Uani 1 1 d . . . H2A H 1.0836 0.1550 0.6159 0.066 Uiso 1 1 calc R . . C3 C 1.0876(9) 0.2631(5) 0.6021(4) 0.0524(19) Uani 1 1 d . . . H3A H 1.1454 0.2677 0.5718 0.063 Uiso 1 1 calc R . . C4 C 1.0406(7) 0.3230(4) 0.6212(4) 0.0434(17) Uani 1 1 d . . . C5 C 1.0758(7) 0.3970(4) 0.5990(3) 0.0422(16) Uani 1 1 d . . . C6 C 1.0342(7) 0.4580(4) 0.6262(3) 0.0417(16) Uani 1 1 d . . . C7 C 0.9486(7) 0.4468(4) 0.6742(4) 0.0441(17) Uani 1 1 d . . . C8 C 0.9022(8) 0.5047(5) 0.7016(4) 0.0493(18) Uani 1 1 d . . . H8A H 0.9261 0.5544 0.6902 0.059 Uiso 1 1 calc R . . C9 C 0.8203(8) 0.4870(5) 0.7457(4) 0.0509(19) Uani 1 1 d . . . H9A H 0.7893 0.5256 0.7660 0.061 Uiso 1 1 calc R . . C10 C 0.7832(8) 0.4146(4) 0.7608(4) 0.0464(18) Uani 1 1 d . . . H10A H 0.7257 0.4042 0.7909 0.056 Uiso 1 1 calc R . . C11 C 0.9087(7) 0.3748(4) 0.6912(3) 0.0398(16) Uani 1 1 d . . . C12 C 0.9551(7) 0.3131(4) 0.6661(3) 0.0411(16) Uani 1 1 d . . . C13 C 1.1877(7) 0.4755(5) 0.5358(4) 0.0466(18) Uani 1 1 d . . . C14 C 1.2691(7) 0.4879(5) 0.4859(3) 0.0439(17) Uani 1 1 d . . . C15 C 1.3078(8) 0.4300(5) 0.4557(4) 0.0498(19) Uani 1 1 d . . . H15A H 1.2797 0.3795 0.4653 0.060 Uiso 1 1 calc R . . C16 C 1.3897(9) 0.4474(5) 0.4105(4) 0.053(2) Uani 1 1 d . . . C17 C 1.4283(8) 0.5216(6) 0.3976(4) 0.057(2) Uani 1 1 d . . . H17A H 1.4853 0.5326 0.3673 0.068 Uiso 1 1 calc R . . C18 C 1.3095(8) 0.5614(5) 0.4689(4) 0.0495(19) Uani 1 1 d . . . C19 C 1.2664(8) 0.6242(5) 0.4972(4) 0.0473(18) Uani 1 1 d . . . C20 C 1.2655(10) 0.7476(5) 0.5044(5) 0.064(2) Uani 1 1 d . . . H20A H 1.2919 0.7958 0.4903 0.077 Uiso 1 1 calc R . . C21 C 1.1909(9) 0.7416(5) 0.5511(5) 0.057(2) Uani 1 1 d . . . C22 C 1.1474(8) 0.6731(4) 0.5721(4) 0.0494(18) Uani 1 1 d . . . H22A H 1.0928 0.6672 0.6037 0.059 Uiso 1 1 calc R . . C25 C 0.5576(8) 0.2355(4) 0.6248(4) 0.0445(17) Uani 1 1 d . . . H25A H 0.5940 0.2902 0.6326 0.053 Uiso 1 1 calc R . . C23 C 1.1867(8) 0.6121(5) 0.5450(4) 0.0481(18) Uani 1 1 d . . . C24 C 1.1468(7) 0.5364(4) 0.5642(3) 0.0433(17) Uani 1 1 d . . . C26 C 0.4486(8) 0.1978(5) 0.5674(4) 0.0497(19) Uani 1 1 d . . . H26A H 0.4113 0.2268 0.5375 0.060 Uiso 1 1 calc R . . C27 C 0.3948(8) 0.1173(4) 0.5542(3) 0.0461(18) Uani 1 1 d . . . C28 C 0.4489(8) 0.0801(4) 0.6020(4) 0.0470(18) Uani 1 1 d . . . H28A H 0.4126 0.0255 0.5958 0.056 Uiso 1 1 calc R . . C29 C 0.5543(8) 0.1196(4) 0.6587(3) 0.0434(17) Uani 1 1 d . . . C30 C 0.6170(7) 0.0831(4) 0.7116(3) 0.0434(17) Uani 1 1 d . . . C31 C 0.5642(9) 0.0073(5) 0.7165(4) 0.056(2) Uani 1 1 d . . . H31A H 0.4812 -0.0246 0.6844 0.067 Uiso 1 1 calc R . . C32 C 0.6291(9) -0.0243(5) 0.7673(4) 0.056(2) Uani 1 1 d . . . C33 C 0.7525(10) 0.0239(6) 0.8098(5) 0.066(2) Uani 1 1 d . . . H33A H 0.8046 0.0044 0.8434 0.079 Uiso 1 1 calc R . . C34 C 0.8023(9) 0.1010(5) 0.8044(4) 0.060(2) Uani 1 1 d . . . H34A H 0.8866 0.1333 0.8353 0.072 Uiso 1 1 calc R . . C35 C 0.2838(8) 0.0757(5) 0.4883(4) 0.053(2) Uani 1 1 d . . . C36 C 0.1573(14) 0.0955(9) 0.4860(7) 0.110(4) Uiso 1 1 d . . . H36A H 0.1750 0.1501 0.4832 0.164 Uiso 1 1 calc R . . H36B H 0.1271 0.0860 0.5268 0.164 Uiso 1 1 calc R . . H36C H 0.0839 0.0638 0.4464 0.164 Uiso 1 1 calc R . . C37 C 0.3489(13) 0.0919(9) 0.4305(5) 0.106(4) Uani 1 1 d . . . H37A H 0.3716 0.1469 0.4288 0.159 Uiso 1 1 calc R . . H37B H 0.2828 0.0618 0.3881 0.159 Uiso 1 1 calc R . . H37C H 0.4345 0.0773 0.4372 0.159 Uiso 1 1 calc R . . C38 C 0.2499(14) -0.0140(7) 0.4829(6) 0.108(4) Uani 1 1 d . . . H38A H 0.1918 -0.0401 0.4377 0.162 Uiso 1 1 calc R . . H38B H 0.1995 -0.0310 0.5163 0.162 Uiso 1 1 calc R . . H38C H 0.3372 -0.0269 0.4914 0.162 Uiso 1 1 calc R . . C39 C 0.5657(11) -0.1077(6) 0.7748(5) 0.072(3) Uani 1 1 d . . . C40 C 0.5054(17) -0.1616(9) 0.7071(8) 0.125(5) Uiso 1 1 d . . . H40A H 0.4784 -0.2151 0.7139 0.187 Uiso 1 1 calc R . . H40B H 0.5757 -0.1540 0.6813 0.187 Uiso 1 1 calc R . . H40C H 0.4229 -0.1506 0.6822 0.187 Uiso 1 1 calc R . . C41 C 0.4497(18) -0.1092(8) 0.8093(11) 0.145(7) Uani 1 1 d . . . H41A H 0.4204 -0.1587 0.8239 0.217 Uiso 1 1 calc R . . H41B H 0.3700 -0.1026 0.7777 0.217 Uiso 1 1 calc R . . H41C H 0.4838 -0.0672 0.8485 0.217 Uiso 1 1 calc R . . C42 C 0.6690(16) -0.1363(7) 0.8199(7) 0.107(4) Uani 1 1 d . . . H42A H 0.6243 -0.1901 0.8224 0.160 Uiso 1 1 calc R . . H42B H 0.6999 -0.1046 0.8651 0.160 Uiso 1 1 calc R . . H42C H 0.7498 -0.1327 0.8014 0.160 Uiso 1 1 calc R . . C43 C 0.5231(8) 0.2224(5) 0.8038(4) 0.0512(19) Uani 1 1 d . . . H43A H 0.4718 0.2140 0.7582 0.061 Uiso 1 1 calc R . . C44 C 0.4506(8) 0.2059(5) 0.8520(4) 0.055(2) Uani 1 1 d . . . H44A H 0.3514 0.1867 0.8389 0.066 Uiso 1 1 calc R . . C45 C 0.5214(9) 0.2169(5) 0.9192(4) 0.057(2) Uani 1 1 d . . . C46 C 0.6659(8) 0.2493(5) 0.9349(4) 0.057(2) Uani 1 1 d . . . H46A H 0.7192 0.2603 0.9804 0.069 Uiso 1 1 calc R . . C47 C 0.7319(8) 0.2653(4) 0.8850(4) 0.0487(18) Uani 1 1 d . . . C48 C 0.8861(8) 0.2963(5) 0.8973(4) 0.0501(19) Uani 1 1 d . . . C49 C 0.9785(9) 0.3318(5) 0.9595(4) 0.060(2) Uani 1 1 d . . . H49A H 0.9424 0.3359 0.9977 0.073 Uiso 1 1 calc R . . C50 C 1.1202(9) 0.3612(6) 0.9681(4) 0.064(2) Uani 1 1 d . . . C51 C 1.1669(9) 0.3514(6) 0.9104(4) 0.069(3) Uani 1 1 d . . . H51A H 1.2641 0.3683 0.9133 0.083 Uiso 1 1 calc R . . C52 C 1.0705(8) 0.3167(5) 0.8484(4) 0.057(2) Uani 1 1 d . . . H52A H 1.1041 0.3126 0.8094 0.069 Uiso 1 1 calc R . . C53 C 0.4486(10) 0.1843(6) 0.9712(5) 0.074(3) Uani 1 1 d . . . C54 C 0.4663(14) 0.1038(8) 0.9762(7) 0.105(4) Uani 1 1 d . . . H54A H 0.4375 0.0723 0.9310 0.158 Uiso 1 1 calc R . . H54B H 0.4080 0.0784 1.0039 0.158 Uiso 1 1 calc R . . H54C H 0.5645 0.1100 0.9970 0.158 Uiso 1 1 calc R . . C55 C 0.2948(12) 0.1797(8) 0.9515(6) 0.098(4) Uani 1 1 d . . . H55A H 0.2875 0.2305 0.9452 0.146 Uiso 1 1 calc R . . H55B H 0.2513 0.1631 0.9872 0.146 Uiso 1 1 calc R . . H55C H 0.2468 0.1424 0.9094 0.146 Uiso 1 1 calc R . . C56 C 0.5177(12) 0.2360(8) 1.0405(5) 0.102(4) Uani 1 1 d . . . H56A H 0.5233 0.2895 1.0369 0.153 Uiso 1 1 calc R . . H56B H 0.6121 0.2329 1.0571 0.153 Uiso 1 1 calc R . . H56C H 0.4621 0.2189 1.0720 0.153 Uiso 1 1 calc R . . C57 C 1.2203(10) 0.4022(7) 1.0361(5) 0.079(3) Uani 1 1 d . . . C58 C 1.1734(12) 0.4697(8) 1.0606(6) 0.112(5) Uani 1 1 d . . . H58A H 1.0734 0.4512 1.0583 0.167 Uiso 1 1 calc R . . H58B H 1.1901 0.5085 1.0320 0.167 Uiso 1 1 calc R . . H58C H 1.2264 0.4928 1.1072 0.167 Uiso 1 1 calc R . . C59 C 1.3730(10) 0.4323(8) 1.0314(6) 0.103(4) Uani 1 1 d . . . H59A H 1.4349 0.4554 1.0765 0.154 Uiso 1 1 calc R . . H59B H 1.3808 0.4713 1.0026 0.154 Uiso 1 1 calc R . . H59C H 1.3999 0.3894 1.0120 0.154 Uiso 1 1 calc R . . C60 C 1.2147(12) 0.3470(8) 1.0858(5) 0.099(4) Uani 1 1 d . . . H60A H 1.1209 0.3311 1.0931 0.148 Uiso 1 1 calc R . . H60B H 1.2834 0.3730 1.1287 0.148 Uiso 1 1 calc R . . H60C H 1.2362 0.3015 1.0677 0.148 Uiso 1 1 calc R . . P1 P 0.4079(2) 0.41701(17) 0.76949(12) 0.0673(7) Uani 1 1 d . . . F11 F 0.3594(8) 0.4557(5) 0.8277(4) 0.122(3) Uani 1 1 d . . . F12 F 0.5345(6) 0.4924(3) 0.7781(3) 0.0828(16) Uani 1 1 d . . . F13 F 0.2846(6) 0.3373(4) 0.7601(3) 0.097(2) Uani 1 1 d . . . F14 F 0.3159(9) 0.4455(5) 0.7136(5) 0.152(4) Uani 1 1 d . . . F15 F 0.5039(7) 0.3886(4) 0.8258(3) 0.104(2) Uani 1 1 d . . . F16 F 0.4601(7) 0.3745(4) 0.7140(3) 0.109(2) Uani 1 1 d . . . P2 P 0.1314(3) 0.02517(15) 0.72938(14) 0.0731(7) Uani 1 1 d . . . F21 F 0.1579(12) -0.0367(6) 0.6810(6) 0.181(5) Uani 1 1 d . . . F22 F 0.1061(8) 0.0889(5) 0.7780(4) 0.123(3) Uani 1 1 d . . . F23 F 0.0326(11) -0.0397(6) 0.7536(6) 0.182(5) Uani 1 1 d . . . F24 F 0.2583(10) 0.0250(5) 0.7867(5) 0.150(4) Uani 1 1 d . . . F25 F 0.0019(8) 0.0261(4) 0.6736(4) 0.117(3) Uani 1 1 d . . . F26 F 0.2333(8) 0.0927(5) 0.7078(4) 0.123(3) Uani 1 1 d . . . O1CA O 0.8625(10) 0.3372(6) 1.1150(5) 0.049(2) Uani 0.50 1 d P . . C1CA C 0.823(2) 0.4560(13) 1.1204(14) 0.090(7) Uani 0.50 1 d P . . H1CA H 0.8525 0.4555 1.0784 0.135 Uiso 0.50 1 calc PR . . H1CB H 0.8912 0.4983 1.1550 0.135 Uiso 0.50 1 calc PR . . H1CC H 0.7311 0.4632 1.1127 0.135 Uiso 0.50 1 calc PR . . C2CA C 0.8165(13) 0.3859(9) 1.1419(7) 0.041(3) Uani 0.50 1 d P . . C3CA C 0.7535(14) 0.3666(9) 1.2006(7) 0.045(4) Uani 0.50 1 d P . . H3CA H 0.7816 0.3242 1.2177 0.067 Uiso 0.50 1 calc PR . . H3CB H 0.6513 0.3511 1.1850 0.067 Uiso 0.50 1 calc PR . . H3CC H 0.7871 0.4121 1.2366 0.067 Uiso 0.50 1 calc PR . . O1CB O 0.9542(12) 0.6848(6) 0.6785(6) 0.057(3) Uani 0.50 1 d P . . C1CB C 0.950(5) 0.7596(19) 0.7750(13) 0.157(16) Uani 0.50 1 d P . . H1CD H 0.9680 0.7176 0.7969 0.235 Uiso 0.50 1 calc PR . . H1CE H 0.8666 0.7692 0.7842 0.235 Uiso 0.50 1 calc PR . . H1CF H 1.0307 0.8064 0.7927 0.235 Uiso 0.50 1 calc PR . . C2CB C 0.928(2) 0.7381(9) 0.7017(10) 0.063(5) Uani 0.50 1 d P . . C3CB C 0.8633(19) 0.7875(10) 0.6610(11) 0.070(5) Uani 0.50 1 d P . . H3CD H 0.8561 0.7713 0.6133 0.105 Uiso 0.50 1 calc PR . . H3CE H 0.9217 0.8415 0.6760 0.105 Uiso 0.50 1 calc PR . . H3CF H 0.7699 0.7819 0.6673 0.105 Uiso 0.50 1 calc PR . . O1CC O 0.829(2) 0.0072(12) 0.9709(8) 0.117(7) Uani 0.50 1 d P . . C1CC C 0.910(3) 0.0458(14) 1.0860(11) 0.100(8) Uani 0.50 1 d P . . H1CG H 0.8867 -0.0101 1.0833 0.151 Uiso 0.50 1 calc PR . . H1CH H 0.8533 0.0654 1.1115 0.151 Uiso 0.50 1 calc PR . . H1CI H 1.0093 0.0706 1.1088 0.151 Uiso 0.50 1 calc PR . . C2CC C 0.882(2) 0.0625(14) 1.0201(10) 0.079(6) Uani 0.50 1 d P . . C3CC C 0.924(3) 0.1410(14) 1.0111(14) 0.099(8) Uani 0.50 1 d P . . H3CG H 0.9205 0.1424 0.9636 0.149 Uiso 0.50 1 calc PR . . H3CH H 1.0195 0.1675 1.0388 0.149 Uiso 0.50 1 calc PR . . H3CI H 0.8605 0.1668 1.0248 0.149 Uiso 0.50 1 calc PR . . 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 0.0471(4) 0.0433(4) 0.0310(3) 0.0032(2) 0.0103(2) 0.0024(2) Br1 0.0680(6) 0.0924(7) 0.0509(5) -0.0047(5) 0.0224(4) 0.0258(5) Br2 0.1116(9) 0.0534(6) 0.0931(8) 0.0211(5) 0.0439(6) 0.0304(5) N1 0.054(4) 0.042(4) 0.035(3) 0.004(3) 0.010(3) 0.011(3) N2 0.041(3) 0.045(3) 0.036(3) 0.002(3) 0.012(2) 0.000(3) N3 0.045(3) 0.045(3) 0.032(3) 0.003(3) 0.013(2) 0.009(3) N4 0.040(3) 0.045(4) 0.039(3) 0.003(3) 0.009(3) 0.003(3) N5 0.055(4) 0.062(4) 0.048(4) 0.016(3) 0.017(3) 0.012(3) N6 0.066(4) 0.056(4) 0.053(4) 0.022(4) 0.020(3) 0.009(3) N7 0.049(4) 0.041(3) 0.034(3) 0.007(3) 0.013(3) 0.002(3) N8 0.054(4) 0.056(4) 0.031(3) 0.014(3) 0.011(3) 0.010(3) N9 0.041(3) 0.046(3) 0.035(3) 0.005(3) 0.007(2) 0.002(3) N10 0.045(4) 0.050(4) 0.042(3) 0.005(3) 0.014(3) 0.002(3) C1 0.064(5) 0.047(5) 0.047(4) 0.008(4) 0.016(4) 0.009(4) C2 0.076(6) 0.039(4) 0.051(5) 0.002(4) 0.023(4) 0.014(4) C3 0.062(5) 0.054(5) 0.043(4) 0.005(4) 0.021(4) 0.017(4) C4 0.047(4) 0.042(4) 0.034(4) -0.003(3) 0.011(3) 0.007(3) C5 0.040(4) 0.046(4) 0.034(4) 0.006(3) 0.007(3) 0.007(3) C6 0.039(4) 0.047(4) 0.036(4) 0.004(3) 0.013(3) 0.007(3) C7 0.038(4) 0.047(4) 0.038(4) 0.004(3) 0.004(3) 0.004(3) C8 0.053(5) 0.042(4) 0.051(5) 0.003(3) 0.019(4) 0.010(3) C9 0.056(5) 0.053(5) 0.043(4) -0.002(4) 0.018(3) 0.017(4) C10 0.046(4) 0.042(4) 0.050(4) 0.002(3) 0.020(3) 0.007(3) C11 0.044(4) 0.039(4) 0.029(3) -0.001(3) 0.010(3) 0.005(3) C12 0.044(4) 0.042(4) 0.031(3) 0.005(3) 0.007(3) 0.006(3) C13 0.039(4) 0.056(5) 0.038(4) 0.005(3) 0.008(3) 0.008(3) C14 0.043(4) 0.055(5) 0.030(4) 0.007(3) 0.009(3) 0.011(3) C15 0.050(4) 0.056(5) 0.036(4) 0.003(3) 0.011(3) 0.006(3) C16 0.059(5) 0.070(6) 0.027(4) -0.002(4) 0.012(3) 0.021(4) C17 0.052(5) 0.076(6) 0.042(4) 0.016(4) 0.015(4) 0.015(4) C18 0.044(4) 0.069(5) 0.035(4) 0.017(4) 0.013(3) 0.012(4) C19 0.047(4) 0.050(5) 0.040(4) 0.013(3) 0.010(3) 0.006(3) C20 0.080(6) 0.048(5) 0.063(6) 0.016(4) 0.019(5) 0.016(4) C21 0.054(5) 0.051(5) 0.061(5) 0.007(4) 0.014(4) 0.010(4) C22 0.056(5) 0.048(5) 0.043(4) 0.008(4) 0.016(3) 0.012(3) C25 0.049(4) 0.041(4) 0.037(4) 0.012(3) 0.008(3) 0.005(3) C23 0.047(4) 0.058(5) 0.037(4) 0.016(4) 0.005(3) 0.015(3) C24 0.036(4) 0.050(4) 0.034(4) 0.005(3) 0.006(3) 0.002(3) C26 0.053(5) 0.058(5) 0.031(4) 0.010(3) 0.007(3) 0.008(4) C27 0.049(4) 0.047(4) 0.032(4) 0.003(3) 0.014(3) -0.002(3) C28 0.049(4) 0.045(4) 0.037(4) 0.002(3) 0.010(3) 0.002(3) C29 0.052(4) 0.043(4) 0.032(4) 0.006(3) 0.014(3) 0.008(3) C30 0.047(4) 0.044(4) 0.034(4) 0.006(3) 0.008(3) 0.008(3) C31 0.068(5) 0.049(5) 0.048(5) 0.011(4) 0.018(4) 0.010(4) C32 0.071(6) 0.043(4) 0.057(5) 0.015(4) 0.025(4) 0.015(4) C33 0.081(6) 0.067(6) 0.053(5) 0.023(5) 0.013(4) 0.026(5) C34 0.068(5) 0.063(6) 0.046(5) 0.020(4) 0.009(4) 0.015(4) C35 0.055(5) 0.052(5) 0.037(4) -0.003(3) 0.003(3) 0.005(4) C37 0.093(8) 0.135(11) 0.053(6) -0.020(7) 0.011(5) 0.000(7) C38 0.127(10) 0.070(7) 0.081(8) -0.012(6) -0.016(7) 0.002(7) C39 0.097(7) 0.061(6) 0.059(6) 0.020(5) 0.019(5) 0.025(5) C41 0.160(14) 0.096(10) 0.25(2) 0.093(12) 0.146(15) 0.052(9) C42 0.154(12) 0.077(8) 0.106(10) 0.046(7) 0.037(9) 0.048(8) C43 0.057(5) 0.057(5) 0.036(4) 0.007(3) 0.012(3) 0.013(4) C44 0.046(4) 0.062(5) 0.050(5) 0.008(4) 0.014(3) 0.005(4) C45 0.059(5) 0.068(6) 0.043(4) 0.014(4) 0.020(4) 0.012(4) C46 0.054(5) 0.072(6) 0.036(4) 0.004(4) 0.015(3) 0.003(4) C47 0.053(4) 0.050(4) 0.034(4) 0.001(3) 0.012(3) 0.004(3) C48 0.051(4) 0.055(5) 0.031(4) 0.003(3) 0.011(3) -0.002(3) C49 0.056(5) 0.079(6) 0.034(4) -0.005(4) 0.011(3) 0.009(4) C50 0.061(5) 0.070(6) 0.043(5) -0.005(4) 0.009(4) 0.003(4) C51 0.050(5) 0.093(7) 0.050(5) -0.003(5) 0.015(4) 0.003(4) C52 0.048(5) 0.070(6) 0.041(4) 0.003(4) 0.011(3) 0.002(4) C53 0.072(6) 0.086(7) 0.054(5) 0.013(5) 0.028(5) 0.004(5) C54 0.113(10) 0.103(9) 0.121(11) 0.059(8) 0.060(8) 0.030(7) C55 0.084(8) 0.142(11) 0.066(7) 0.023(7) 0.043(6) 0.016(7) C56 0.092(8) 0.150(12) 0.050(6) 0.009(7) 0.035(5) 0.006(7) C57 0.061(6) 0.105(8) 0.044(5) -0.013(5) 0.007(4) -0.001(5) C58 0.079(8) 0.128(11) 0.079(8) -0.050(8) 0.002(6) -0.003(7) C59 0.055(6) 0.147(12) 0.062(6) -0.019(7) -0.006(5) -0.006(6) C60 0.070(7) 0.136(11) 0.059(6) 0.003(7) -0.004(5) 0.005(6) P1 0.0524(13) 0.0880(18) 0.0488(13) 0.0012(12) 0.0146(10) 0.0059(12) F11 0.104(5) 0.135(6) 0.121(6) -0.021(5) 0.065(4) 0.015(4) F12 0.074(4) 0.077(4) 0.079(4) 0.008(3) 0.014(3) 0.001(3) F13 0.078(4) 0.100(5) 0.096(5) 0.002(4) 0.037(3) -0.004(3) F14 0.126(6) 0.146(7) 0.130(7) 0.011(6) -0.058(5) 0.034(5) F15 0.116(5) 0.096(5) 0.076(4) 0.009(4) 0.000(4) 0.020(4) F16 0.119(5) 0.100(5) 0.091(5) -0.017(4) 0.062(4) -0.004(4) P2 0.0869(18) 0.0583(15) 0.0663(16) 0.0044(12) 0.0034(13) 0.0260(13) F21 0.190(10) 0.152(8) 0.178(10) -0.066(8) 0.003(8) 0.092(8) F22 0.106(5) 0.142(7) 0.091(5) -0.042(5) 0.008(4) 0.033(5) F23 0.169(9) 0.134(8) 0.209(11) 0.102(8) 0.007(8) -0.002(6) F24 0.153(7) 0.116(6) 0.151(8) 0.014(6) -0.037(6) 0.055(6) F25 0.138(6) 0.073(4) 0.094(5) -0.011(4) -0.042(4) 0.027(4) F26 0.124(6) 0.110(6) 0.105(5) 0.023(5) 0.024(4) -0.006(4) O1CA 0.048(6) 0.054(6) 0.043(6) 0.001(5) 0.012(5) 0.014(5) C1CA 0.099(16) 0.092(16) 0.14(2) 0.054(15) 0.076(15) 0.071(13) C2CA 0.025(7) 0.050(9) 0.033(7) 0.002(6) 0.001(5) -0.005(6) C3CA 0.038(8) 0.045(8) 0.036(7) -0.014(6) 0.009(6) -0.004(6) O1CB 0.086(8) 0.026(5) 0.070(7) 0.006(5) 0.046(6) 0.018(5) C1CB 0.31(5) 0.14(3) 0.080(18) 0.041(18) 0.03(2) 0.17(3) C2CB 0.091(13) 0.029(8) 0.082(13) 0.010(8) 0.052(11) 0.017(8) C3CB 0.062(11) 0.045(10) 0.097(15) 0.010(10) 0.018(10) 0.010(8) O1CC 0.130(14) 0.126(15) 0.053(9) 0.026(9) -0.003(9) -0.010(11) C1CC 0.125(19) 0.074(15) 0.063(13) 0.017(11) -0.002(13) -0.012(13) C2CC 0.077(13) 0.092(16) 0.056(12) 0.026(11) 0.012(10) 0.006(11) C3CC 0.093(16) 0.085(16) 0.12(2) 0.056(15) 0.016(14) 0.024(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N7 2.057(6) . ? Ru N8 2.060(7) . ? Ru N2 2.064(6) . ? Ru N9 2.066(6) . ? Ru N1 2.070(6) . ? Ru N10 2.078(6) . ? Br1 C16 1.888(8) . ? Br2 C21 1.898(9) . ? N1 C1 1.322(10) . ? N1 C12 1.358(9) . ? N2 C10 1.333(10) . ? N2 C11 1.382(9) . ? N3 C13 1.346(10) . ? N3 C5 1.353(9) . ? N4 C6 1.332(10) . ? N4 C24 1.340(9) . ? N5 C17 1.306(11) . ? N5 C18 1.372(10) . ? N6 C20 1.296(11) . ? N6 C19 1.338(10) . ? N7 C25 1.335(9) . ? N7 C29 1.366(9) . ? N8 C34 1.342(10) . ? N8 C30 1.361(9) . ? N9 C43 1.328(10) . ? N9 C47 1.359(9) . ? N10 C52 1.310(10) . ? N10 C48 1.367(9) . ? C1 C2 1.394(11) . ? C2 C3 1.380(11) . ? C3 C4 1.376(11) . ? C4 C12 1.408(10) . ? C4 C5 1.460(11) . ? C5 C6 1.413(10) . ? C6 C7 1.462(10) . ? C7 C11 1.380(10) . ? C7 C8 1.397(11) . ? C8 C9 1.380(11) . ? C9 C10 1.371(11) . ? C11 C12 1.438(10) . ? C13 C24 1.415(11) . ? C13 C14 1.465(10) . ? C14 C15 1.371(11) . ? C14 C18 1.408(11) . ? C15 C16 1.399(11) . ? C16 C17 1.385(12) . ? C18 C19 1.457(12) . ? C19 C23 1.417(11) . ? C20 C21 1.357(13) . ? C21 C22 1.366(12) . ? C22 C23 1.395(11) . ? C25 C26 1.398(10) . ? C23 C24 1.464(11) . ? C26 C27 1.398(11) . ? C27 C28 1.374(11) . ? C27 C35 1.534(10) . ? C28 C29 1.378(10) . ? C29 C30 1.474(10) . ? C30 C31 1.372(11) . ? C31 C32 1.395(12) . ? C32 C33 1.374(13) . ? C32 C39 1.530(12) . ? C33 C34 1.394(13) . ? C35 C36 1.443(15) . ? C35 C37 1.514(14) . ? C35 C38 1.574(15) . ? C39 C42 1.509(16) . ? C39 C40 1.517(18) . ? C39 C41 1.518(16) . ? C43 C44 1.382(11) . ? C44 C45 1.387(12) . ? C45 C46 1.391(11) . ? C45 C53 1.527(12) . ? C46 C47 1.371(10) . ? C47 C48 1.485(11) . ? C48 C49 1.385(10) . ? C49 C50 1.373(12) . ? C50 C51 1.393(12) . ? C50 C57 1.520(12) . ? C51 C52 1.396(11) . ? C53 C55 1.527(16) . ? C53 C56 1.530(14) . ? C53 C54 1.553(17) . ? C57 C58 1.529(17) . ? C57 C60 1.525(17) . ? C57 C59 1.546(14) . ? P1 F14 1.566(8) . ? P1 F12 1.578(6) . ? P1 F11 1.574(7) . ? P1 F16 1.589(6) . ? P1 F15 1.595(7) . ? P1 F13 1.609(6) . ? P2 F23 1.546(10) . ? P2 F21 1.552(9) . ? P2 F26 1.564(8) . ? P2 F24 1.566(8) . ? P2 F22 1.573(7) . ? P2 F25 1.571(7) . ? O1CA C2CA 1.258(18) . ? C1CA C2CA 1.40(3) . ? C2CA C3CA 1.529(19) . ? O1CB C2CB 1.167(18) . ? C1CB C2CB 1.48(3) . ? C2CB C3CB 1.50(3) . ? O1CC C2CC 1.26(3) . ? C1CC C2CC 1.42(3) . ? C2CC C3CC 1.43(3) . ? 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 N7 Ru N8 78.4(2) . . ? N7 Ru N2 96.9(2) . . ? N8 Ru N2 173.6(2) . . ? N7 Ru N9 94.5(2) . . ? N8 Ru N9 84.5(2) . . ? N2 Ru N9 100.2(2) . . ? N7 Ru N1 89.3(2) . . ? N8 Ru N1 96.3(2) . . ? N2 Ru N1 79.3(2) . . ? N9 Ru N1 176.2(2) . . ? N7 Ru N10 172.9(2) . . ? N8 Ru N10 97.9(2) . . ? N2 Ru N10 87.2(2) . . ? N9 Ru N10 79.0(2) . . ? N1 Ru N10 97.2(2) . . ? C1 N1 C12 117.7(7) . . ? C1 N1 Ru 127.8(5) . . ? C12 N1 Ru 114.5(5) . . ? C10 N2 C11 117.6(6) . . ? C10 N2 Ru 128.2(5) . . ? C11 N2 Ru 114.1(5) . . ? C13 N3 C5 116.8(6) . . ? C6 N4 C24 117.2(6) . . ? C17 N5 C18 118.0(7) . . ? C20 N6 C19 118.2(8) . . ? C25 N7 C29 117.6(6) . . ? C25 N7 Ru 126.0(5) . . ? C29 N7 Ru 116.3(5) . . ? C34 N8 C30 117.9(7) . . ? C34 N8 Ru 125.8(6) . . ? C30 N8 Ru 115.9(5) . . ? C43 N9 C47 117.4(6) . . ? C43 N9 Ru 125.3(5) . . ? C47 N9 Ru 115.6(5) . . ? C52 N10 C48 118.9(6) . . ? C52 N10 Ru 126.3(5) . . ? C48 N10 Ru 114.5(5) . . ? N1 C1 C2 122.8(8) . . ? C3 C2 C1 119.5(8) . . ? C4 C3 C2 119.1(7) . . ? C3 C4 C12 118.1(7) . . ? C3 C4 C5 124.2(7) . . ? C12 C4 C5 117.8(7) . . ? N3 C5 C6 121.4(6) . . ? N3 C5 C4 118.1(7) . . ? C6 C5 C4 120.4(6) . . ? N4 C6 C5 121.7(6) . . ? N4 C6 C7 117.8(7) . . ? C5 C6 C7 120.5(7) . . ? C11 C7 C8 119.1(7) . . ? C11 C7 C6 118.0(7) . . ? C8 C7 C6 122.8(7) . . ? C9 C8 C7 117.7(7) . . ? C10 C9 C8 121.0(7) . . ? N2 C10 C9 122.4(7) . . ? C7 C11 N2 122.2(7) . . ? C7 C11 C12 122.1(6) . . ? N2 C11 C12 115.7(6) . . ? N1 C12 C4 122.8(7) . . ? N1 C12 C11 116.3(6) . . ? C4 C12 C11 121.0(6) . . ? N3 C13 C24 121.1(7) . . ? N3 C13 C14 119.0(7) . . ? C24 C13 C14 119.8(7) . . ? C15 C14 C18 119.1(7) . . ? C15 C14 C13 121.8(7) . . ? C18 C14 C13 119.1(7) . . ? C14 C15 C16 118.2(8) . . ? C17 C16 C15 119.4(8) . . ? C17 C16 Br1 119.2(6) . . ? C15 C16 Br1 121.4(7) . . ? N5 C17 C16 123.6(8) . . ? N5 C18 C14 121.7(8) . . ? N5 C18 C19 116.7(7) . . ? C14 C18 C19 121.5(6) . . ? N6 C19 C23 121.2(8) . . ? N6 C19 C18 119.4(7) . . ? C23 C19 C18 119.4(7) . . ? N6 C20 C21 124.6(8) . . ? C20 C21 C22 120.1(8) . . ? C20 C21 Br2 119.6(7) . . ? C22 C21 Br2 120.3(7) . . ? C21 C22 C23 117.2(7) . . ? N7 C25 C26 122.7(7) . . ? C22 C23 C19 118.6(7) . . ? C22 C23 C24 121.8(7) . . ? C19 C23 C24 119.5(7) . . ? N4 C24 C13 121.8(7) . . ? N4 C24 C23 117.6(7) . . ? C13 C24 C23 120.6(7) . . ? C25 C26 C27 119.8(7) . . ? C28 C27 C26 116.4(7) . . ? C28 C27 C35 123.9(7) . . ? C26 C27 C35 119.7(7) . . ? C27 C28 C29 121.9(7) . . ? N7 C29 C28 121.4(7) . . ? N7 C29 C30 114.1(6) . . ? C28 C29 C30 124.5(7) . . ? N8 C30 C31 121.2(7) . . ? N8 C30 C29 114.5(6) . . ? C31 C30 C29 124.3(7) . . ? C30 C31 C32 121.7(8) . . ? C33 C32 C31 116.0(8) . . ? C33 C32 C39 122.4(8) . . ? C31 C32 C39 121.6(8) . . ? C32 C33 C34 120.8(8) . . ? N8 C34 C33 122.1(8) . . ? C36 C35 C37 115.9(10) . . ? C36 C35 C27 110.5(8) . . ? C37 C35 C27 108.0(7) . . ? C36 C35 C38 109.2(9) . . ? C37 C35 C38 103.3(9) . . ? C27 C35 C38 109.7(7) . . ? C42 C39 C40 109.8(11) . . ? C42 C39 C41 106.3(11) . . ? C40 C39 C41 109.2(12) . . ? C42 C39 C32 112.5(9) . . ? C40 C39 C32 111.6(9) . . ? C41 C39 C32 107.1(9) . . ? N9 C43 C44 122.6(7) . . ? C43 C44 C45 120.6(8) . . ? C44 C45 C46 116.2(7) . . ? C44 C45 C53 121.9(8) . . ? C46 C45 C53 121.2(8) . . ? C47 C46 C45 120.5(7) . . ? N9 C47 C46 122.5(7) . . ? N9 C47 C48 113.8(6) . . ? C46 C47 C48 123.6(7) . . ? N10 C48 C49 119.7(7) . . ? N10 C48 C47 115.4(6) . . ? C49 C48 C47 124.8(7) . . ? C50 C49 C48 122.7(8) . . ? C49 C50 C51 115.9(8) . . ? C49 C50 C57 122.3(8) . . ? C51 C50 C57 121.8(8) . . ? C50 C51 C52 119.8(8) . . ? N10 C52 C51 123.0(8) . . ? C55 C53 C45 110.3(8) . . ? C55 C53 C56 108.6(9) . . ? C45 C53 C56 110.2(8) . . ? C55 C53 C54 111.7(10) . . ? C45 C53 C54 108.3(9) . . ? C56 C53 C54 107.8(10) . . ? C50 C57 C58 107.2(9) . . ? C50 C57 C60 110.0(9) . . ? C58 C57 C60 110.0(10) . . ? C50 C57 C59 111.9(8) . . ? C58 C57 C59 109.8(10) . . ? C60 C57 C59 107.9(10) . . ? F14 P1 F12 90.2(4) . . ? F14 P1 F11 93.2(6) . . ? F12 P1 F11 91.0(4) . . ? F14 P1 F16 90.3(5) . . ? F12 P1 F16 90.1(3) . . ? F11 P1 F16 176.3(5) . . ? F14 P1 F15 178.9(5) . . ? F12 P1 F15 89.0(4) . . ? F11 P1 F15 87.5(5) . . ? F16 P1 F15 89.0(4) . . ? F14 P1 F13 91.8(5) . . ? F12 P1 F13 176.7(4) . . ? F11 P1 F13 91.5(4) . . ? F16 P1 F13 87.2(4) . . ? F15 P1 F13 89.0(4) . . ? F23 P2 F21 89.5(7) . . ? F23 P2 F26 177.7(6) . . ? F21 P2 F26 92.4(7) . . ? F23 P2 F24 90.5(6) . . ? F21 P2 F24 90.9(6) . . ? F26 P2 F24 88.1(5) . . ? F23 P2 F22 91.4(7) . . ? F21 P2 F22 179.1(7) . . ? F26 P2 F22 86.7(5) . . ? F24 P2 F22 89.1(5) . . ? F23 P2 F25 88.7(5) . . ? F21 P2 F25 90.6(5) . . ? F26 P2 F25 92.6(5) . . ? F24 P2 F25 178.2(6) . . ? F22 P2 F25 89.4(4) . . ? O1CA C2CA C1CA 122.2(14) . . ? O1CA C2CA C3CA 117.5(14) . . ? C1CA C2CA C3CA 120.3(15) . . ? O1CB C2CB C1CB 121.4(19) . . ? O1CB C2CB C3CB 124.2(18) . . ? C1CB C2CB C3CB 114.3(16) . . ? O1CC C2CC C1CC 119(2) . . ? O1CC C2CC C3CC 122(2) . . ? C1CC C2CC C3CC 119(2) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.274 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.108 # Attachment '6_1.cif' # # Paper Ref.: B917484B # data_mk0802sq _database_code_depnum_ccdc_archive 'CCDC 730640' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H58 Br2 N10 Ru, 2.0(F6 P)' _chemical_formula_sum 'C60 H58 Br2 F12 N10 P2 Ru' _chemical_formula_weight 1469.99 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' Br Br -0.2901 2.4595 '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 -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.6539(14) _cell_length_b 15.9733(16) _cell_length_c 16.3583(6) _cell_angle_alpha 75.624(6) _cell_angle_beta 74.766(4) _cell_angle_gamma 75.583(8) _cell_volume 3748.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 237 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 1.387 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.602 _exptl_absorpt_correction_T_max 0.800 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 2.00 \% and 120 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 80953 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13207 _reflns_number_gt 8609 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' # SQUEEZE RESULTS (APPEND TO CIF) 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 1 -0.066 0.500 0.500 783.8 13.2 2 0.363 0.000 0.958 8.2 0.2 3 0.637 0.000 0.042 8.2 0.0 _platon_squeeze_details ; Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; _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. PLATON analysis revealed the presence of large solvent accessible voids that are very likely occupied by strongly disordered solvent water molecules. A refinement of distinct positions was not successful, however. Therefore, the SQUEEZE procedure (see above) was applied. The three highest residual electron density maxima are located close to the atoms Ru1, Br1 and Br2 indicating a small amount (less than 5 %) of disorder of the complex cation. Attempts to refine a split model here weren't successful. ; _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^)+(0.1127P)^2^+5.2350P] 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 13207 _refine_ls_number_parameters 906 _refine_ls_number_restraints 308 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_ref 0.2487 _refine_ls_wR_factor_gt 0.2267 _refine_ls_goodness_of_fit_ref 1.301 _refine_ls_restrained_S_all 1.319 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.27446(4) 0.24278(4) 0.14360(3) 0.0395(2) Uani 1 1 d . . . Br1 Br 0.27576(8) 0.43794(8) 0.40554(6) 0.0875(4) Uani 1 1 d . . . Br2 Br 0.47542(6) -0.11219(6) 0.09677(6) 0.0615(3) Uani 1 1 d . . . N1 N 0.3168(4) 0.2632(5) 0.2466(4) 0.0521(17) Uani 1 1 d . . . N2 N 0.5287(5) 0.1275(6) 0.4335(4) 0.065(2) Uani 1 1 d . . . N3 N 0.7451(6) -0.0215(8) 0.6124(5) 0.091(3) Uani 1 1 d . . . N4 N 0.7968(5) -0.1625(6) 0.5297(4) 0.070(2) Uani 1 1 d . . . N5 N 0.5791(4) -0.0188(5) 0.3519(4) 0.060(2) Uani 1 1 d . . . N6 N 0.2353(3) 0.2022(3) 0.0509(3) 0.0345(12) Uani 1 1 d . . . N7 N 0.1650(4) 0.1889(4) 0.2167(4) 0.0482(15) Uani 1 1 d . . . N8 N 0.2008(4) 0.3680(4) 0.1100(4) 0.0478(15) Uani 1 1 d . . . N9 N 0.3714(4) 0.3037(4) 0.0544(3) 0.0460(15) Uani 1 1 d . . . N10 N 0.3634(4) 0.1250(4) 0.1727(3) 0.0419(14) Uani 1 1 d . . . C1 C 0.3813(4) 0.1973(5) 0.2763(4) 0.0418(16) Uani 1 1 d . . . C2 C 0.2877(6) 0.3347(6) 0.2834(5) 0.058(2) Uani 1 1 d . . . H2B H 0.2431 0.3823 0.2634 0.070 Uiso 1 1 calc R . . C3 C 0.3255(7) 0.3374(7) 0.3536(5) 0.069(3) Uani 1 1 d . . . C4 C 0.3912(6) 0.2718(7) 0.3827(5) 0.062(2) Uani 1 1 d . . . H4B H 0.4161 0.2764 0.4281 0.074 Uiso 1 1 calc R . . C5 C 0.4907(5) 0.1237(7) 0.3691(5) 0.061(2) Uani 1 1 d . . . C6 C 0.5158(5) 0.0524(7) 0.3292(4) 0.058(2) Uani 1 1 d . . . C7 C 0.4953(5) -0.0214(5) 0.2182(4) 0.0458(17) Uani 1 1 d . . . H7A H 0.5398 -0.0714 0.2337 0.055 Uiso 1 1 calc R . . C8 C 0.4502(5) -0.0176(5) 0.1538(4) 0.0450(17) Uani 1 1 d . . . C9 C 0.3849(4) 0.0557(5) 0.1336(4) 0.0431(17) Uani 1 1 d . . . H9A H 0.3540 0.0570 0.0903 0.052 Uiso 1 1 calc R . . C10 C 0.4080(4) 0.1213(5) 0.2353(4) 0.0448(18) Uani 1 1 d . . . C11 C 0.4215(5) 0.1974(6) 0.3444(4) 0.051(2) Uani 1 1 d . . . C12 C 0.4733(4) 0.0497(5) 0.2586(4) 0.0448(18) Uani 1 1 d . . . C13 C 0.5931(5) 0.0551(7) 0.4545(5) 0.065(3) Uani 1 1 d . . . C14 C 0.6366(6) 0.0556(7) 0.5245(5) 0.065(3) Uani 1 1 d . . . C15 C 0.6130(7) 0.1237(8) 0.5677(5) 0.079(3) Uani 1 1 d . . . H15A H 0.5661 0.1721 0.5543 0.094 Uiso 1 1 calc R . . C16 C 0.6577(7) 0.1222(10) 0.6318(6) 0.086(4) Uani 1 1 d . . . H16A H 0.6445 0.1700 0.6609 0.103 Uiso 1 1 calc R . . C17 C 0.7211(7) 0.0490(9) 0.6504(6) 0.078(3) Uani 1 1 d . . . H17A H 0.7512 0.0475 0.6943 0.094 Uiso 1 1 calc R . . C18 C 0.7037(5) -0.0182(8) 0.5482(5) 0.068(3) Uani 1 1 d . . . C19 C 0.7311(6) -0.0943(8) 0.5060(5) 0.074(3) Uani 1 1 d . . . C20 C 0.8187(7) -0.2305(9) 0.4920(7) 0.086(3) Uani 1 1 d . . . H20A H 0.8654 -0.2778 0.5082 0.103 Uiso 1 1 calc R . . C21 C 0.7761(6) -0.2367(8) 0.4287(6) 0.080(3) Uani 1 1 d . . . H21A H 0.7928 -0.2882 0.4044 0.097 Uiso 1 1 calc R . . C22 C 0.7109(6) -0.1686(7) 0.4021(5) 0.064(2) Uani 1 1 d . . . H22A H 0.6819 -0.1716 0.3589 0.077 Uiso 1 1 calc R . . C23 C 0.6880(5) -0.0954(7) 0.4394(5) 0.064(3) Uani 1 1 d . . . C24 C 0.6178(5) -0.0199(7) 0.4145(5) 0.060(2) Uani 1 1 d . . . C25 C 0.2739(4) 0.2129(5) -0.0339(4) 0.0431(17) Uani 1 1 d . . . H25A H 0.3191 0.2478 -0.0553 0.052 Uiso 1 1 calc R . . C26 C 0.2517(5) 0.1764(6) -0.0911(5) 0.057(2) Uani 1 1 d . . . H26A H 0.2825 0.1846 -0.1500 0.068 Uiso 1 1 calc R . . C27 C 0.1852(5) 0.1280(6) -0.0630(5) 0.057(2) Uani 1 1 d . . . C28 C 0.1443(5) 0.1192(5) 0.0227(5) 0.0480(18) Uani 1 1 d . . . H28A H 0.0978 0.0859 0.0446 0.058 Uiso 1 1 calc R . . C29 C 0.1681(4) 0.1564(4) 0.0781(4) 0.0371(15) Uani 1 1 d . . . C30 C 0.1250(5) 0.1530(5) 0.1718(5) 0.0462(17) Uani 1 1 d . . . C31 C 0.0479(5) 0.1206(6) 0.2124(5) 0.058(2) Uani 1 1 d . . . H31A H 0.0204 0.0963 0.1809 0.069 Uiso 1 1 calc R . . C32 C 0.0090(5) 0.1230(7) 0.3001(5) 0.067(2) Uani 1 1 d . A . C33 C 0.0516(6) 0.1569(7) 0.3416(5) 0.067(3) Uani 1 1 d . . . H33A H 0.0290 0.1583 0.4012 0.080 Uiso 1 1 calc R . . C34 C 0.1300(5) 0.1904(6) 0.2968(5) 0.060(2) Uani 1 1 d . . . H34A H 0.1582 0.2152 0.3273 0.072 Uiso 1 1 calc R . . C35 C 0.1616(6) 0.0845(8) -0.1282(6) 0.081(3) Uani 1 1 d . . . C36 C 0.2457(6) 0.0296(7) -0.1715(6) 0.077(3) Uani 1 1 d DU . . H36A H 0.2690 -0.0193 -0.1283 0.116 Uiso 1 1 calc R . . H36B H 0.2913 0.0662 -0.1989 0.116 Uiso 1 1 calc R . . H36C H 0.2319 0.0062 -0.2154 0.116 Uiso 1 1 calc R . . C37 C 0.1240(8) 0.1621(9) -0.1983(7) 0.099(4) Uani 1 1 d DU . . H37A H 0.1076 0.1378 -0.2402 0.148 Uiso 1 1 calc R . . H37B H 0.1704 0.1971 -0.2282 0.148 Uiso 1 1 calc R . . H37C H 0.0704 0.1997 -0.1700 0.148 Uiso 1 1 calc R . . C38 C 0.0886(8) 0.0337(9) -0.0861(7) 0.099(4) Uani 1 1 d DU . . H38A H 0.1093 -0.0155 -0.0418 0.149 Uiso 1 1 calc R . . H38B H 0.0733 0.0107 -0.1295 0.149 Uiso 1 1 calc R . . H38C H 0.0351 0.0723 -0.0591 0.149 Uiso 1 1 calc R . . C39 C -0.0788(7) 0.0894(9) 0.3462(6) 0.094(4) Uani 1 1 d . . . C40 C -0.1487(13) 0.1282(17) 0.2876(13) 0.102(5) Uani 0.600(11) 1 d PU A 1 H40A H -0.1399 0.0900 0.2463 0.154 Uiso 0.600(11) 1 calc PR A 1 H40B H -0.1403 0.1873 0.2562 0.154 Uiso 0.600(11) 1 calc PR A 1 H40C H -0.2100 0.1316 0.3235 0.154 Uiso 0.600(11) 1 calc PR A 1 C41 C -0.0569(13) -0.0111(14) 0.3514(13) 0.102(5) Uani 0.600(11) 1 d PU A 1 H41A H 0.0006 -0.0273 0.3116 0.152 Uiso 0.600(11) 1 calc PR A 1 H41B H -0.1050 -0.0286 0.3354 0.152 Uiso 0.600(11) 1 calc PR A 1 H41C H -0.0522 -0.0412 0.4105 0.152 Uiso 0.600(11) 1 calc PR A 1 C42 C -0.1180(13) 0.1135(16) 0.4324(13) 0.094(5) Uani 0.600(11) 1 d PU A 1 H42A H -0.0919 0.0680 0.4764 0.141 Uiso 0.600(11) 1 calc PR A 1 H42B H -0.1836 0.1180 0.4457 0.141 Uiso 0.600(11) 1 calc PR A 1 H42C H -0.1043 0.1703 0.4319 0.141 Uiso 0.600(11) 1 calc PR A 1 C40A C -0.1210(19) 0.056(2) 0.3015(17) 0.096(5) Uani 0.400(11) 1 d PDU A 2 H40D H -0.0765 0.0130 0.2703 0.144 Uiso 0.400(11) 1 calc PR A 2 H40E H -0.1485 0.1036 0.2603 0.144 Uiso 0.400(11) 1 calc PR A 2 H40F H -0.1679 0.0264 0.3422 0.144 Uiso 0.400(11) 1 calc PR A 2 C41A C -0.0611(19) 0.032(2) 0.4320(17) 0.099(5) Uani 0.400(11) 1 d PDU A 2 H41D H -0.0175 -0.0222 0.4212 0.149 Uiso 0.400(11) 1 calc PR A 2 H41E H -0.1178 0.0164 0.4685 0.149 Uiso 0.400(11) 1 calc PR A 2 H41F H -0.0367 0.0641 0.4613 0.149 Uiso 0.400(11) 1 calc PR A 2 C42A C -0.1518(19) 0.1737(19) 0.382(2) 0.103(6) Uani 0.400(11) 1 d PDU A 2 H42D H -0.2091 0.1555 0.4124 0.154 Uiso 0.400(11) 1 calc PR A 2 H42E H -0.1618 0.2222 0.3333 0.154 Uiso 0.400(11) 1 calc PR A 2 H42F H -0.1275 0.1935 0.4220 0.154 Uiso 0.400(11) 1 calc PR A 2 C43 C 0.1144(5) 0.3965(6) 0.1450(6) 0.065(2) Uani 1 1 d . . . H43A H 0.0832 0.3574 0.1899 0.078 Uiso 1 1 calc R . . C44 C 0.0677(6) 0.4829(6) 0.1179(6) 0.067(2) Uani 1 1 d . . . H44A H 0.0067 0.5016 0.1455 0.080 Uiso 1 1 calc R . . C45 C 0.1107(5) 0.5401(6) 0.0511(6) 0.065(2) Uani 1 1 d . . . C46 C 0.2013(5) 0.5105(6) 0.0149(6) 0.059(2) Uani 1 1 d . . . H46A H 0.2336 0.5488 -0.0299 0.071 Uiso 1 1 calc R . . C47 C 0.2439(5) 0.4258(5) 0.0440(5) 0.0480(18) Uani 1 1 d . . . C48 C 0.3395(5) 0.3895(5) 0.0110(4) 0.0464(17) Uani 1 1 d . . . C49 C 0.3961(5) 0.4336(5) -0.0583(5) 0.054(2) Uani 1 1 d . . . H49A H 0.3731 0.4908 -0.0876 0.065 Uiso 1 1 calc R . . C50 C 0.4879(5) 0.3933(6) -0.0851(5) 0.058(2) Uani 1 1 d . B . C51 C 0.5164(5) 0.3158(6) -0.0364(5) 0.056(2) Uani 1 1 d . . . H51A H 0.5783 0.2885 -0.0495 0.067 Uiso 1 1 calc R . . C52 C 0.4580(5) 0.2733(6) 0.0335(5) 0.055(2) Uani 1 1 d . . . H52A H 0.4829 0.2197 0.0673 0.066 Uiso 1 1 calc R . . C53 C 0.0624(7) 0.6346(7) 0.0209(8) 0.087(3) Uani 1 1 d . . . C54 C -0.0425(7) 0.6441(8) 0.0558(10) 0.114(4) Uani 1 1 d U . . H54A H -0.0556 0.6269 0.1189 0.171 Uiso 1 1 calc R . . H54B H -0.0650 0.6058 0.0314 0.171 Uiso 1 1 calc R . . H54C H -0.0722 0.7054 0.0387 0.171 Uiso 1 1 calc R . . C55 C 0.0834(7) 0.6605(8) -0.0774(8) 0.099(4) Uani 1 1 d U . . H55A H 0.1488 0.6546 -0.0989 0.148 Uiso 1 1 calc R . . H55B H 0.0537 0.7217 -0.0950 0.148 Uiso 1 1 calc R . . H55C H 0.0612 0.6217 -0.1016 0.148 Uiso 1 1 calc R . . C56 C 0.0970(8) 0.6982(7) 0.0566(9) 0.105(4) Uani 1 1 d U . . H56A H 0.0848 0.6826 0.1198 0.157 Uiso 1 1 calc R . . H56B H 0.0660 0.7589 0.0385 0.157 Uiso 1 1 calc R . . H56C H 0.1622 0.6935 0.0339 0.157 Uiso 1 1 calc R . . C57 C 0.5509(6) 0.4390(6) -0.1614(6) 0.066(2) Uani 1 1 d D . . C58 C 0.4964(10) 0.4988(12) -0.2331(9) 0.083(4) Uani 0.683(13) 1 d PU B 1 H58A H 0.4416 0.4768 -0.2273 0.125 Uiso 0.683(13) 1 calc PR B 1 H58B H 0.5345 0.4960 -0.2908 0.125 Uiso 0.683(13) 1 calc PR B 1 H58C H 0.4800 0.5599 -0.2249 0.125 Uiso 0.683(13) 1 calc PR B 1 C59 C 0.5899(12) 0.4963(13) -0.1274(10) 0.095(5) Uani 0.683(13) 1 d PU B 1 H59A H 0.5512 0.5551 -0.1305 0.142 Uiso 0.683(13) 1 calc PR B 1 H59B H 0.6505 0.5010 -0.1623 0.142 Uiso 0.683(13) 1 calc PR B 1 H59C H 0.5936 0.4704 -0.0672 0.142 Uiso 0.683(13) 1 calc PR B 1 C60 C 0.6202(12) 0.3725(13) -0.2054(12) 0.116(8) Uani 0.683(13) 1 d PDU B 1 H60A H 0.5944 0.3537 -0.2448 0.173 Uiso 0.683(13) 1 calc PR B 1 H60B H 0.6393 0.3214 -0.1621 0.173 Uiso 0.683(13) 1 calc PR B 1 H60C H 0.6724 0.3987 -0.2383 0.173 Uiso 0.683(13) 1 calc PR B 1 C58A C 0.520(2) 0.527(2) -0.184(2) 0.100(6) Uani 0.317(13) 1 d PDU B 2 H58D H 0.4647 0.5362 -0.2061 0.151 Uiso 0.317(13) 1 calc PR B 2 H58E H 0.5657 0.5530 -0.2295 0.151 Uiso 0.317(13) 1 calc PR B 2 H58F H 0.5060 0.5541 -0.1338 0.151 Uiso 0.317(13) 1 calc PR B 2 C59A C 0.645(2) 0.424(2) -0.128(2) 0.088(7) Uani 0.317(13) 1 d PDU B 2 H59D H 0.6487 0.3720 -0.0812 0.132 Uiso 0.317(13) 1 calc PR B 2 H59E H 0.6460 0.4759 -0.1070 0.132 Uiso 0.317(13) 1 calc PR B 2 H59F H 0.6969 0.4146 -0.1762 0.132 Uiso 0.317(13) 1 calc PR B 2 C60A C 0.567(3) 0.378(2) -0.219(2) 0.110(9) Uani 0.317(13) 1 d PDU B 2 H60D H 0.5127 0.3865 -0.2427 0.166 Uiso 0.317(13) 1 calc PR B 2 H60E H 0.5793 0.3170 -0.1874 0.166 Uiso 0.317(13) 1 calc PR B 2 H60F H 0.6182 0.3885 -0.2670 0.166 Uiso 0.317(13) 1 calc PR B 2 P1 P 0.3972(5) 0.3104(5) 0.6798(4) 0.107(2) Uani 0.552(7) 1 d PD C 1 F11 F 0.2948(9) 0.3237(10) 0.6919(10) 0.153(6) Uani 0.552(7) 1 d PDU C 1 F12 F 0.5046(9) 0.2981(13) 0.6698(11) 0.168(7) Uani 0.552(7) 1 d PDU C 1 F13 F 0.4057(8) 0.2155(7) 0.7146(6) 0.097(4) Uani 0.552(7) 1 d PDU C 1 F14 F 0.3766(10) 0.3297(9) 0.7752(7) 0.135(5) Uani 0.552(7) 1 d PDU C 1 F15 F 0.3910(14) 0.4121(9) 0.6430(10) 0.178(7) Uani 0.552(7) 1 d PDU C 1 F16 F 0.4193(12) 0.2989(11) 0.5804(8) 0.163(7) Uani 0.552(7) 1 d PDU C 1 P2 P 0.6588(2) 0.2458(2) 0.1507(3) 0.0874(13) Uani 0.799(6) 1 d PD D 2 F21 F 0.5564(5) 0.2904(6) 0.1807(7) 0.114(3) Uani 0.799(6) 1 d PDU D 2 F22 F 0.7610(4) 0.2011(5) 0.1180(5) 0.093(2) Uani 0.799(6) 1 d PDU D 2 F23 F 0.6638(6) 0.3136(6) 0.0649(7) 0.133(4) Uani 0.799(6) 1 d PDU D 2 F24 F 0.6901(6) 0.3147(7) 0.1859(8) 0.141(4) Uani 0.799(6) 1 d PDU D 2 F25 F 0.6539(6) 0.1769(7) 0.2375(6) 0.141(4) Uani 0.799(6) 1 d PDU D 2 F26 F 0.6254(6) 0.1796(5) 0.1133(7) 0.122(3) Uani 0.799(6) 1 d PDU D 2 P3 P 0.1929(10) -0.1323(7) 0.1591(11) 0.242(7) Uani 0.648(8) 1 d PD E 3 F31 F 0.1030(12) -0.0721(15) 0.1444(17) 0.266(11) Uani 0.648(8) 1 d PDU E 3 F32 F 0.281(2) -0.194(2) 0.191(3) 0.68(5) Uani 0.648(8) 1 d PDU E 3 F33 F 0.2392(16) -0.1401(16) 0.0706(13) 0.259(11) Uani 0.648(8) 1 d PDU E 3 F34 F 0.2265(11) -0.0475(9) 0.1601(11) 0.170(6) Uani 0.648(8) 1 d PDU E 3 F35 F 0.144(2) -0.137(2) 0.2605(15) 0.42(2) Uani 0.648(8) 1 d PDU E 3 F36 F 0.1488(19) -0.2170(15) 0.177(2) 0.328(15) Uani 0.648(8) 1 d PDU E 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0297(3) 0.0545(4) 0.0376(3) -0.0094(2) -0.0050(2) -0.0160(2) Br1 0.1205(9) 0.0971(8) 0.0570(6) -0.0382(5) 0.0109(5) -0.0516(7) Br2 0.0551(5) 0.0666(6) 0.0645(5) -0.0201(4) -0.0206(4) 0.0008(4) N1 0.051(4) 0.078(5) 0.037(3) -0.026(3) 0.012(3) -0.038(4) N2 0.053(4) 0.129(7) 0.028(3) -0.019(4) 0.004(3) -0.053(5) N3 0.067(5) 0.172(10) 0.042(4) 0.018(5) -0.025(4) -0.063(6) N4 0.041(4) 0.119(7) 0.040(4) 0.017(4) -0.012(3) -0.025(4) N5 0.033(3) 0.120(6) 0.026(3) 0.011(3) -0.012(3) -0.036(4) N6 0.028(3) 0.037(3) 0.037(3) -0.005(2) -0.010(2) -0.004(2) N7 0.033(3) 0.060(4) 0.046(4) 0.006(3) -0.005(3) -0.019(3) N8 0.035(3) 0.049(4) 0.058(4) -0.014(3) -0.010(3) -0.002(3) N9 0.036(3) 0.072(4) 0.031(3) -0.010(3) 0.000(2) -0.018(3) N10 0.035(3) 0.066(4) 0.033(3) -0.011(3) -0.005(2) -0.026(3) C1 0.032(4) 0.064(5) 0.032(4) -0.007(3) -0.003(3) -0.023(3) C2 0.057(5) 0.076(6) 0.044(4) -0.021(4) 0.013(4) -0.035(4) C3 0.088(7) 0.083(7) 0.050(5) -0.038(5) 0.021(5) -0.057(6) C4 0.055(5) 0.101(7) 0.038(4) -0.011(4) 0.001(4) -0.046(5) C5 0.040(4) 0.126(8) 0.029(4) -0.009(4) 0.000(3) -0.049(5) C6 0.047(4) 0.116(8) 0.024(4) 0.002(4) -0.007(3) -0.054(5) C7 0.031(3) 0.067(5) 0.036(4) -0.002(3) -0.006(3) -0.012(3) C8 0.035(4) 0.065(5) 0.037(4) -0.010(3) -0.009(3) -0.014(4) C9 0.033(4) 0.070(5) 0.033(4) -0.012(3) -0.005(3) -0.022(4) C10 0.030(3) 0.074(5) 0.035(4) -0.008(3) -0.001(3) -0.028(4) C11 0.048(4) 0.087(6) 0.033(4) -0.024(4) 0.011(3) -0.048(4) C12 0.028(3) 0.073(5) 0.033(4) 0.001(3) -0.005(3) -0.023(4) C13 0.035(4) 0.120(8) 0.044(4) 0.010(5) -0.007(4) -0.048(5) C14 0.053(5) 0.124(8) 0.029(4) -0.005(5) 0.000(3) -0.056(6) C15 0.072(6) 0.136(9) 0.045(5) -0.011(5) -0.004(4) -0.067(6) C16 0.069(6) 0.158(11) 0.045(5) -0.005(6) -0.011(5) -0.063(8) C17 0.076(7) 0.131(10) 0.046(5) -0.017(6) -0.006(5) -0.061(7) C18 0.033(4) 0.132(9) 0.035(4) 0.011(5) -0.005(3) -0.040(5) C19 0.053(5) 0.128(9) 0.040(5) 0.009(5) -0.004(4) -0.047(6) C20 0.066(6) 0.136(10) 0.057(6) -0.017(6) -0.007(5) -0.029(7) C21 0.066(6) 0.116(8) 0.045(5) 0.018(5) -0.015(4) -0.023(6) C22 0.055(5) 0.102(7) 0.032(4) 0.000(4) -0.013(4) -0.019(5) C23 0.033(4) 0.121(8) 0.031(4) 0.022(5) -0.008(3) -0.038(5) C24 0.042(4) 0.112(7) 0.031(4) -0.010(4) 0.004(3) -0.039(5) C25 0.023(3) 0.052(4) 0.041(4) 0.002(3) 0.001(3) -0.001(3) C26 0.042(4) 0.094(6) 0.033(4) -0.013(4) 0.001(3) -0.019(4) C27 0.030(4) 0.101(7) 0.045(4) -0.023(4) -0.002(3) -0.019(4) C28 0.033(4) 0.064(5) 0.051(4) -0.020(4) 0.001(3) -0.016(3) C29 0.027(3) 0.045(4) 0.036(4) -0.006(3) -0.003(3) -0.007(3) C30 0.036(4) 0.059(5) 0.045(4) -0.006(3) -0.008(3) -0.016(3) C31 0.055(5) 0.083(6) 0.040(4) -0.010(4) 0.001(3) -0.036(4) C32 0.047(5) 0.102(7) 0.058(5) -0.007(5) -0.005(4) -0.044(5) C33 0.053(5) 0.117(8) 0.029(4) 0.001(4) -0.003(3) -0.035(5) C34 0.055(5) 0.101(7) 0.033(4) -0.005(4) -0.011(3) -0.037(5) C35 0.064(6) 0.134(9) 0.055(5) -0.048(6) 0.003(4) -0.029(6) C36 0.078(6) 0.103(7) 0.068(6) -0.050(5) -0.007(5) -0.025(5) C37 0.080(7) 0.153(10) 0.065(6) -0.039(6) -0.024(5) -0.001(7) C38 0.091(7) 0.149(10) 0.090(7) -0.060(7) -0.001(6) -0.063(7) C39 0.079(7) 0.167(12) 0.053(6) -0.008(6) 0.004(5) -0.084(8) C40 0.077(8) 0.143(11) 0.103(9) -0.017(9) -0.009(7) -0.068(9) C41 0.093(8) 0.121(9) 0.094(8) 0.003(7) -0.001(7) -0.071(7) C42 0.077(8) 0.116(9) 0.096(8) -0.017(7) 0.011(7) -0.065(7) C40A 0.076(8) 0.129(10) 0.098(9) -0.006(9) -0.009(7) -0.074(8) C41A 0.090(8) 0.118(9) 0.093(8) 0.002(8) 0.000(7) -0.067(8) C42A 0.084(10) 0.123(11) 0.102(11) -0.024(9) 0.014(9) -0.054(9) C43 0.047(5) 0.078(6) 0.073(6) -0.029(5) 0.004(4) -0.020(4) C44 0.039(4) 0.066(6) 0.083(6) -0.002(5) -0.009(4) -0.006(4) C45 0.042(4) 0.060(5) 0.093(7) -0.022(5) -0.003(4) -0.014(4) C46 0.047(4) 0.061(5) 0.067(5) -0.003(4) -0.013(4) -0.018(4) C47 0.041(4) 0.050(5) 0.056(4) -0.011(4) -0.010(3) -0.015(4) C48 0.045(4) 0.057(5) 0.037(4) -0.007(3) 0.001(3) -0.022(4) C49 0.049(4) 0.058(5) 0.046(4) -0.005(4) 0.005(3) -0.015(4) C50 0.044(4) 0.065(5) 0.053(5) -0.011(4) 0.006(4) -0.006(4) C51 0.033(4) 0.072(6) 0.065(5) -0.017(4) 0.001(4) -0.023(4) C52 0.047(5) 0.059(5) 0.056(5) 0.004(4) -0.011(4) -0.022(4) C53 0.059(6) 0.082(7) 0.109(9) -0.003(6) -0.021(6) -0.009(5) C54 0.066(6) 0.084(7) 0.159(11) 0.007(7) -0.015(7) 0.005(6) C55 0.071(6) 0.098(8) 0.116(9) 0.011(7) -0.035(6) -0.011(6) C56 0.092(8) 0.065(6) 0.150(10) -0.034(7) -0.008(7) -0.009(6) C57 0.053(5) 0.066(6) 0.062(5) -0.003(4) 0.015(4) -0.018(4) C58 0.079(8) 0.117(11) 0.043(7) 0.012(7) -0.001(6) -0.039(8) C59 0.082(9) 0.127(11) 0.079(8) 0.019(9) -0.010(7) -0.074(8) C60 0.068(12) 0.147(14) 0.072(10) 0.015(9) 0.049(11) -0.017(12) C58A 0.085(10) 0.127(11) 0.073(9) 0.020(9) 0.000(8) -0.048(9) C59A 0.068(12) 0.118(14) 0.078(11) 0.013(12) 0.003(10) -0.073(10) C60A 0.069(15) 0.150(16) 0.071(12) 0.008(12) 0.033(14) -0.027(16) P1 0.141(6) 0.127(6) 0.071(4) 0.004(3) -0.037(4) -0.065(5) F11 0.149(12) 0.140(11) 0.154(12) -0.022(9) -0.036(10) 0.000(10) F12 0.136(11) 0.227(15) 0.168(13) -0.050(11) -0.023(10) -0.080(11) F13 0.123(9) 0.115(8) 0.051(5) 0.003(5) -0.020(5) -0.041(7) F14 0.189(12) 0.157(11) 0.080(7) -0.003(7) -0.023(8) -0.101(10) F15 0.276(17) 0.125(11) 0.130(11) 0.009(9) -0.040(11) -0.072(11) F16 0.235(15) 0.165(12) 0.118(10) -0.051(9) -0.085(10) -0.021(11) P2 0.0528(19) 0.084(2) 0.124(3) -0.008(2) -0.0085(19) -0.0330(17) F21 0.067(5) 0.107(6) 0.173(8) -0.048(6) -0.002(5) -0.032(4) F22 0.055(4) 0.104(5) 0.111(6) -0.001(4) -0.010(4) -0.028(4) F23 0.085(6) 0.114(7) 0.178(9) 0.033(6) -0.027(6) -0.042(5) F24 0.101(6) 0.146(8) 0.198(10) -0.070(7) 0.001(6) -0.062(6) F25 0.117(7) 0.161(9) 0.123(7) -0.002(6) 0.026(6) -0.070(6) F26 0.091(5) 0.079(5) 0.213(10) -0.015(6) -0.066(6) -0.025(4) P3 0.284(17) 0.153(9) 0.32(2) -0.073(11) -0.152(15) 0.019(10) F31 0.198(15) 0.275(18) 0.300(19) -0.009(15) -0.092(14) -0.007(14) F32 0.67(5) 0.67(5) 0.68(5) -0.12(2) -0.15(2) -0.12(2) F33 0.30(2) 0.280(19) 0.223(16) -0.095(15) -0.039(14) -0.082(15) F34 0.184(12) 0.138(10) 0.199(13) -0.021(9) -0.070(10) -0.035(9) F35 0.40(3) 0.46(3) 0.38(3) -0.085(19) -0.085(19) -0.094(19) F36 0.33(2) 0.29(2) 0.38(2) -0.082(17) -0.050(17) -0.120(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N9 2.060(5) . ? Ru1 N7 2.063(5) . ? Ru1 N8 2.066(6) . ? Ru1 N6 2.067(5) . ? Ru1 N10 2.075(6) . ? Ru1 N1 2.086(6) . ? Br1 C3 1.902(9) . ? Br2 C8 1.875(8) . ? N1 C2 1.346(10) . ? N1 C1 1.355(10) . ? N2 C5 1.358(10) . ? N2 C13 1.370(12) . ? N3 C17 1.344(14) . ? N3 C18 1.357(11) . ? N4 C20 1.309(14) . ? N4 C19 1.355(13) . ? N5 C24 1.315(9) . ? N5 C6 1.355(12) . ? N6 C25 1.345(8) . ? N6 C29 1.348(8) . ? N7 C34 1.285(9) . ? N7 C30 1.374(9) . ? N8 C43 1.334(10) . ? N8 C47 1.381(9) . ? N9 C52 1.304(10) . ? N9 C48 1.412(10) . ? N10 C9 1.342(9) . ? N10 C10 1.365(8) . ? C1 C11 1.417(10) . ? C1 C10 1.451(11) . ? C2 C3 1.437(12) . ? C2 H2B 0.9500 . ? C3 C4 1.363(14) . ? C4 C11 1.401(12) . ? C4 H4B 0.9500 . ? C5 C6 1.375(13) . ? C5 C11 1.442(13) . ? C6 C12 1.489(9) . ? C7 C12 1.381(11) . ? C7 C8 1.397(10) . ? C7 H7A 0.9500 . ? C8 C9 1.383(10) . ? C9 H9A 0.9500 . ? C10 C12 1.379(11) . ? C13 C24 1.429(14) . ? C13 C14 1.481(11) . ? C14 C15 1.365(14) . ? C14 C18 1.419(14) . ? C15 C16 1.397(12) . ? C15 H15A 0.9500 . ? C16 C17 1.359(16) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.463(15) . ? C19 C23 1.429(12) . ? C20 C21 1.405(14) . ? C20 H20A 0.9500 . ? C21 C22 1.364(13) . ? C21 H21A 0.9500 . ? C22 C23 1.379(14) . ? C22 H22A 0.9500 . ? C23 C24 1.469(13) . ? C25 C26 1.372(11) . ? C25 H25A 0.9500 . ? C26 C27 1.366(11) . ? C26 H26A 0.9500 . ? C27 C28 1.368(10) . ? C27 C35 1.569(12) . ? C28 C29 1.366(10) . ? C28 H28A 0.9500 . ? C29 C30 1.497(9) . ? C30 C31 1.372(10) . ? C31 C32 1.410(11) . ? C31 H31A 0.9500 . ? C32 C33 1.341(12) . ? C32 C39 1.539(11) . ? C33 C34 1.410(11) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C38 1.486(14) . ? C35 C36 1.499(13) . ? C35 C37 1.576(16) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40A 1.37(3) . ? C39 C42 1.49(2) . ? C39 C41A 1.53(3) . ? C39 C41 1.54(2) . ? C39 C40 1.55(2) . ? C39 C42A 1.65(3) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C40A H40D 0.9800 . ? C40A H40E 0.9800 . ? C40A H40F 0.9800 . ? C41A H41D 0.9800 . ? C41A H41E 0.9800 . ? C41A H41F 0.9800 . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C43 C44 1.415(13) . ? C43 H43A 0.9500 . ? C44 C45 1.381(12) . ? C44 H44A 0.9500 . ? C45 C46 1.396(11) . ? C45 C53 1.534(14) . ? C46 C47 1.379(11) . ? C46 H46A 0.9500 . ? C47 C48 1.471(10) . ? C48 C49 1.398(10) . ? C49 C50 1.422(11) . ? C49 H49A 0.9500 . ? C50 C51 1.336(12) . ? C50 C57 1.524(11) . ? C51 C52 1.407(10) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? C53 C55 1.526(16) . ? C53 C56 1.550(16) . ? C53 C54 1.572(14) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58A 1.35(3) . ? C57 C60A 1.46(2) . ? C57 C60 1.489(17) . ? C57 C59 1.493(19) . ? C57 C58 1.606(17) . ? C57 C59A 1.65(3) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C58A H58D 0.9800 . ? C58A H58E 0.9800 . ? C58A H58F 0.9800 . ? C59A H59D 0.9800 . ? C59A H59E 0.9800 . ? C59A H59F 0.9800 . ? C60A H60D 0.9800 . ? C60A H60E 0.9800 . ? C60A H60F 0.9800 . ? P1 F13 1.466(11) . ? P1 F11 1.529(13) . ? P1 F15 1.574(13) . ? P1 F14 1.599(11) . ? P1 F12 1.612(13) . ? P1 F16 1.618(12) . ? P2 F23 1.543(9) . ? P2 F25 1.562(10) . ? P2 F21 1.584(8) . ? P2 F24 1.586(9) . ? P2 F22 1.590(7) . ? P2 F26 1.591(8) . ? P3 F33 1.459(14) . ? P3 F31 1.534(14) . ? P3 F34 1.575(13) . ? P3 F36 1.598(15) . ? P3 F32 1.610(17) . ? P3 F35 1.624(17) . ? 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 N9 Ru1 N7 170.3(2) . . ? N9 Ru1 N8 78.6(2) . . ? N7 Ru1 N8 95.5(2) . . ? N9 Ru1 N6 93.2(2) . . ? N7 Ru1 N6 78.8(2) . . ? N8 Ru1 N6 89.8(2) . . ? N9 Ru1 N10 94.5(2) . . ? N7 Ru1 N10 91.7(2) . . ? N8 Ru1 N10 172.3(2) . . ? N6 Ru1 N10 93.9(2) . . ? N9 Ru1 N1 92.0(2) . . ? N7 Ru1 N1 96.6(2) . . ? N8 Ru1 N1 98.3(3) . . ? N6 Ru1 N1 171.1(2) . . ? N10 Ru1 N1 78.5(3) . . ? C2 N1 C1 118.9(7) . . ? C2 N1 Ru1 126.4(6) . . ? C1 N1 Ru1 114.8(5) . . ? C5 N2 C13 114.4(8) . . ? C17 N3 C18 116.8(10) . . ? C20 N4 C19 118.9(9) . . ? C24 N5 C6 118.9(8) . . ? C25 N6 C29 116.5(6) . . ? C25 N6 Ru1 126.1(5) . . ? C29 N6 Ru1 117.3(4) . . ? C34 N7 C30 119.2(6) . . ? C34 N7 Ru1 126.0(5) . . ? C30 N7 Ru1 114.7(5) . . ? C43 N8 C47 117.5(7) . . ? C43 N8 Ru1 125.4(6) . . ? C47 N8 Ru1 117.1(5) . . ? C52 N9 C48 116.3(6) . . ? C52 N9 Ru1 128.3(5) . . ? C48 N9 Ru1 115.4(4) . . ? C9 N10 C10 117.7(6) . . ? C9 N10 Ru1 127.1(5) . . ? C10 N10 Ru1 115.0(5) . . ? N1 C1 C11 124.9(7) . . ? N1 C1 C10 116.0(6) . . ? C11 C1 C10 119.1(7) . . ? N1 C2 C3 118.4(9) . . ? N1 C2 H2B 120.8 . . ? C3 C2 H2B 120.8 . . ? C4 C3 C2 122.7(8) . . ? C4 C3 Br1 121.7(7) . . ? C2 C3 Br1 115.5(8) . . ? C3 C4 C11 118.8(8) . . ? C3 C4 H4B 120.6 . . ? C11 C4 H4B 120.6 . . ? N2 C5 C6 122.0(9) . . ? N2 C5 C11 117.4(9) . . ? C6 C5 C11 120.7(7) . . ? N5 C6 C5 122.4(7) . . ? N5 C6 C12 116.7(8) . . ? C5 C6 C12 121.0(8) . . ? C12 C7 C8 118.0(7) . . ? C12 C7 H7A 121.0 . . ? C8 C7 H7A 121.0 . . ? C9 C8 C7 119.5(7) . . ? C9 C8 Br2 120.0(5) . . ? C7 C8 Br2 120.5(6) . . ? N10 C9 C8 122.6(6) . . ? N10 C9 H9A 118.7 . . ? C8 C9 H9A 118.7 . . ? N10 C10 C12 122.4(7) . . ? N10 C10 C1 115.4(7) . . ? C12 C10 C1 122.2(6) . . ? C4 C11 C1 116.3(8) . . ? C4 C11 C5 124.2(7) . . ? C1 C11 C5 119.5(7) . . ? C10 C12 C7 119.8(6) . . ? C10 C12 C6 117.5(8) . . ? C7 C12 C6 122.7(7) . . ? N2 C13 C24 123.7(7) . . ? N2 C13 C14 116.7(9) . . ? C24 C13 C14 119.5(9) . . ? C15 C14 C18 119.3(8) . . ? C15 C14 C13 122.2(10) . . ? C18 C14 C13 118.5(9) . . ? C14 C15 C16 120.0(12) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C17 C16 C15 116.7(12) . . ? C17 C16 H16A 121.6 . . ? C15 C16 H16A 121.6 . . ? N3 C17 C16 126.1(10) . . ? N3 C17 H17A 117.0 . . ? C16 C17 H17A 117.0 . . ? N3 C18 C14 120.9(11) . . ? N3 C18 C19 116.7(10) . . ? C14 C18 C19 122.4(8) . . ? N4 C19 C23 120.7(11) . . ? N4 C19 C18 120.2(8) . . ? C23 C19 C18 119.1(10) . . ? N4 C20 C21 122.9(11) . . ? N4 C20 H20A 118.6 . . ? C21 C20 H20A 118.6 . . ? C22 C21 C20 119.8(12) . . ? C22 C21 H21A 120.1 . . ? C20 C21 H21A 120.1 . . ? C21 C22 C23 118.3(9) . . ? C21 C22 H22A 120.8 . . ? C23 C22 H22A 120.8 . . ? C22 C23 C19 119.3(9) . . ? C22 C23 C24 121.3(7) . . ? C19 C23 C24 119.4(10) . . ? N5 C24 C13 118.6(9) . . ? N5 C24 C23 120.2(9) . . ? C13 C24 C23 121.1(8) . . ? N6 C25 C26 123.7(6) . . ? N6 C25 H25A 118.2 . . ? C26 C25 H25A 118.2 . . ? C27 C26 C25 119.7(7) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C26 C27 C28 116.5(7) . . ? C26 C27 C35 119.5(7) . . ? C28 C27 C35 124.0(7) . . ? C29 C28 C27 122.4(7) . . ? C29 C28 H28A 118.8 . . ? C27 C28 H28A 118.8 . . ? N6 C29 C28 121.1(6) . . ? N6 C29 C30 112.8(6) . . ? C28 C29 C30 126.1(6) . . ? C31 C30 N7 119.9(7) . . ? C31 C30 C29 124.1(7) . . ? N7 C30 C29 115.9(6) . . ? C30 C31 C32 121.0(7) . . ? C30 C31 H31A 119.5 . . ? C32 C31 H31A 119.5 . . ? C33 C32 C31 116.9(7) . . ? C33 C32 C39 121.3(8) . . ? C31 C32 C39 121.9(8) . . ? C32 C33 C34 120.1(7) . . ? C32 C33 H33A 119.9 . . ? C34 C33 H33A 119.9 . . ? N7 C34 C33 123.0(7) . . ? N7 C34 H34A 118.5 . . ? C33 C34 H34A 118.5 . . ? C38 C35 C36 112.6(10) . . ? C38 C35 C27 112.0(7) . . ? C36 C35 C27 109.5(7) . . ? C38 C35 C37 106.8(9) . . ? C36 C35 C37 109.1(8) . . ? C27 C35 C37 106.7(9) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40A C39 C42 126.0(14) . . ? C40A C39 C41A 115.9(18) . . ? C42 C39 C41A 54.7(13) . . ? C40A C39 C32 119.7(13) . . ? C42 C39 C32 113.3(10) . . ? C41A C39 C32 105.8(12) . . ? C40A C39 C41 62.0(16) . . ? C42 C39 C41 112.3(14) . . ? C41A C39 C41 63.3(15) . . ? C32 C39 C41 106.7(11) . . ? C42 C39 C40 109.4(15) . . ? C41A C39 C40 145.8(13) . . ? C32 C39 C40 108.4(10) . . ? C41 C39 C40 106.4(14) . . ? C40A C39 C42A 107.3(18) . . ? C41A C39 C42A 99.6(16) . . ? C32 C39 C42A 106.4(13) . . ? C41 C39 C42A 145.9(13) . . ? C40 C39 C42A 70.4(16) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C39 C40A H40D 109.5 . . ? C39 C40A H40E 109.5 . . ? H40D C40A H40E 109.5 . . ? C39 C40A H40F 109.5 . . ? H40D C40A H40F 109.5 . . ? H40E C40A H40F 109.5 . . ? C39 C41A H41D 109.5 . . ? C39 C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C39 C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? C39 C42A H42D 109.5 . . ? C39 C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C39 C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? N8 C43 C44 122.3(8) . . ? N8 C43 H43A 118.8 . . ? C44 C43 H43A 118.8 . . ? C45 C44 C43 119.9(8) . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C44 C45 C46 117.7(8) . . ? C44 C45 C53 121.2(8) . . ? C46 C45 C53 121.0(8) . . ? C47 C46 C45 120.0(8) . . ? C47 C46 H46A 120.0 . . ? C45 C46 H46A 120.0 . . ? C46 C47 N8 122.4(7) . . ? C46 C47 C48 123.9(7) . . ? N8 C47 C48 113.7(6) . . ? C49 C48 N9 121.0(7) . . ? C49 C48 C47 124.4(7) . . ? N9 C48 C47 114.6(6) . . ? C48 C49 C50 120.2(8) . . ? C48 C49 H49A 119.9 . . ? C50 C49 H49A 119.9 . . ? C51 C50 C49 115.9(7) . . ? C51 C50 C57 122.4(7) . . ? C49 C50 C57 121.5(8) . . ? C50 C51 C52 122.4(8) . . ? C50 C51 H51A 118.8 . . ? C52 C51 H51A 118.8 . . ? N9 C52 C51 123.3(8) . . ? N9 C52 H52A 118.3 . . ? C51 C52 H52A 118.3 . . ? C55 C53 C45 111.0(9) . . ? C55 C53 C56 107.9(10) . . ? C45 C53 C56 108.6(9) . . ? C55 C53 C54 109.7(10) . . ? C45 C53 C54 110.3(8) . . ? C56 C53 C54 109.2(10) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58A C57 C60A 123(2) . . ? C58A C57 C60 134.2(17) . . ? C58A C57 C59 65.0(17) . . ? C60A C57 C59 147.1(17) . . ? C60 C57 C59 113.6(13) . . ? C58A C57 C50 113.5(15) . . ? C60A C57 C50 98.3(16) . . ? C60 C57 C50 110.3(9) . . ? C59 C57 C50 107.2(9) . . ? C58A C57 C58 45.7(17) . . ? C60A C57 C58 79.4(19) . . ? C60 C57 C58 105.7(12) . . ? C59 C57 C58 109.3(11) . . ? C50 C57 C58 110.7(8) . . ? C58A C57 C59A 108.9(18) . . ? C60A C57 C59A 106.9(19) . . ? C60 C57 C59A 71.4(16) . . ? C59 C57 C59A 47.0(14) . . ? C50 C57 C59A 104.7(11) . . ? C58 C57 C59A 142.7(12) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C57 C58A H58D 109.5 . . ? C57 C58A H58E 109.5 . . ? H58D C58A H58E 109.5 . . ? C57 C58A H58F 109.5 . . ? H58D C58A H58F 109.5 . . ? H58E C58A H58F 109.5 . . ? C57 C59A H59D 109.5 . . ? C57 C59A H59E 109.5 . . ? H59D C59A H59E 109.5 . . ? C57 C59A H59F 109.5 . . ? H59D C59A H59F 109.5 . . ? H59E C59A H59F 109.5 . . ? C57 C60A H60D 109.5 . . ? C57 C60A H60E 109.5 . . ? H60D C60A H60E 109.5 . . ? C57 C60A H60F 109.5 . . ? H60D C60A H60F 109.5 . . ? H60E C60A H60F 109.5 . . ? F13 P1 F11 92.2(8) . . ? F13 P1 F15 178.2(10) . . ? F11 P1 F15 89.5(10) . . ? F13 P1 F14 90.7(7) . . ? F11 P1 F14 85.9(8) . . ? F15 P1 F14 88.9(8) . . ? F13 P1 F12 88.3(9) . . ? F11 P1 F12 178.1(10) . . ? F15 P1 F12 90.0(10) . . ? F14 P1 F12 92.2(8) . . ? F13 P1 F16 93.7(8) . . ? F11 P1 F16 95.0(9) . . ? F15 P1 F16 86.6(8) . . ? F14 P1 F16 175.4(9) . . ? F12 P1 F16 86.8(9) . . ? F23 P2 F25 179.8(8) . . ? F23 P2 F21 89.4(5) . . ? F25 P2 F21 90.7(5) . . ? F23 P2 F24 85.8(6) . . ? F25 P2 F24 94.3(6) . . ? F21 P2 F24 90.3(5) . . ? F23 P2 F22 89.4(5) . . ? F25 P2 F22 90.5(5) . . ? F21 P2 F22 178.3(6) . . ? F24 P2 F22 90.8(5) . . ? F23 P2 F26 92.4(6) . . ? F25 P2 F26 87.5(6) . . ? F21 P2 F26 88.5(5) . . ? F24 P2 F26 177.9(6) . . ? F22 P2 F26 90.4(5) . . ? F33 P3 F31 100.9(14) . . ? F33 P3 F34 96.6(13) . . ? F31 P3 F34 87.8(11) . . ? F33 P3 F36 94.5(13) . . ? F31 P3 F36 90.2(13) . . ? F34 P3 F36 168.9(15) . . ? F33 P3 F32 88.3(15) . . ? F31 P3 F32 170.8(18) . . ? F34 P3 F32 90.5(15) . . ? F36 P3 F32 89.8(15) . . ? F33 P3 F35 172.6(16) . . ? F31 P3 F35 83.7(14) . . ? F34 P3 F35 89.3(13) . . ? F36 P3 F35 79.6(14) . . ? F32 P3 F35 87.2(15) . . ? 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 N9 Ru1 N1 C2 88.3(6) . . . . ? N7 Ru1 N1 C2 -87.1(6) . . . . ? N8 Ru1 N1 C2 9.5(6) . . . . ? N10 Ru1 N1 C2 -177.5(6) . . . . ? N9 Ru1 N1 C1 -90.1(5) . . . . ? N7 Ru1 N1 C1 94.5(5) . . . . ? N8 Ru1 N1 C1 -168.9(4) . . . . ? N10 Ru1 N1 C1 4.0(4) . . . . ? N9 Ru1 N6 C25 4.3(6) . . . . ? N7 Ru1 N6 C25 178.6(6) . . . . ? N8 Ru1 N6 C25 83.0(5) . . . . ? N10 Ru1 N6 C25 -90.4(5) . . . . ? N9 Ru1 N6 C29 -179.7(5) . . . . ? N7 Ru1 N6 C29 -5.4(5) . . . . ? N8 Ru1 N6 C29 -101.0(5) . . . . ? N10 Ru1 N6 C29 85.6(5) . . . . ? N8 Ru1 N7 C34 -85.7(7) . . . . ? N6 Ru1 N7 C34 -174.5(7) . . . . ? N10 Ru1 N7 C34 91.9(7) . . . . ? N1 Ru1 N7 C34 13.3(7) . . . . ? N8 Ru1 N7 C30 90.6(5) . . . . ? N6 Ru1 N7 C30 1.8(5) . . . . ? N10 Ru1 N7 C30 -91.8(5) . . . . ? N1 Ru1 N7 C30 -170.4(5) . . . . ? N9 Ru1 N8 C43 -176.4(7) . . . . ? N7 Ru1 N8 C43 11.5(7) . . . . ? N6 Ru1 N8 C43 90.3(7) . . . . ? N1 Ru1 N8 C43 -86.0(7) . . . . ? N9 Ru1 N8 C47 5.6(5) . . . . ? N7 Ru1 N8 C47 -166.5(5) . . . . ? N6 Ru1 N8 C47 -87.7(5) . . . . ? N1 Ru1 N8 C47 96.0(5) . . . . ? N8 Ru1 N9 C52 172.7(7) . . . . ? N6 Ru1 N9 C52 -98.1(7) . . . . ? N10 Ru1 N9 C52 -3.9(7) . . . . ? N1 Ru1 N9 C52 74.7(7) . . . . ? N8 Ru1 N9 C48 -6.8(5) . . . . ? N6 Ru1 N9 C48 82.4(5) . . . . ? N10 Ru1 N9 C48 176.6(5) . . . . ? N1 Ru1 N9 C48 -104.8(5) . . . . ? N9 Ru1 N10 C9 -89.4(5) . . . . ? N7 Ru1 N10 C9 83.1(5) . . . . ? N6 Ru1 N10 C9 4.2(5) . . . . ? N1 Ru1 N10 C9 179.5(5) . . . . ? N9 Ru1 N10 C10 86.5(4) . . . . ? N7 Ru1 N10 C10 -101.0(5) . . . . ? N6 Ru1 N10 C10 -180.0(4) . . . . ? N1 Ru1 N10 C10 -4.6(4) . . . . ? C2 N1 C1 C11 0.1(10) . . . . ? Ru1 N1 C1 C11 178.7(5) . . . . ? C2 N1 C1 C10 178.5(6) . . . . ? Ru1 N1 C1 C10 -2.9(7) . . . . ? C1 N1 C2 C3 -0.9(9) . . . . ? Ru1 N1 C2 C3 -179.4(5) . . . . ? N1 C2 C3 C4 1.9(11) . . . . ? N1 C2 C3 Br1 -176.8(5) . . . . ? C2 C3 C4 C11 -1.9(11) . . . . ? Br1 C3 C4 C11 176.7(5) . . . . ? C13 N2 C5 C6 0.1(10) . . . . ? C13 N2 C5 C11 179.3(6) . . . . ? C24 N5 C6 C5 0.1(10) . . . . ? C24 N5 C6 C12 -179.3(6) . . . . ? N2 C5 C6 N5 0.7(11) . . . . ? C11 C5 C6 N5 -178.6(6) . . . . ? N2 C5 C6 C12 -179.9(6) . . . . ? C11 C5 C6 C12 0.8(10) . . . . ? C12 C7 C8 C9 -0.9(10) . . . . ? C12 C7 C8 Br2 -179.3(5) . . . . ? C10 N10 C9 C8 -0.6(9) . . . . ? Ru1 N10 C9 C8 175.1(5) . . . . ? C7 C8 C9 N10 1.0(10) . . . . ? Br2 C8 C9 N10 179.4(5) . . . . ? C9 N10 C10 C12 0.1(9) . . . . ? Ru1 N10 C10 C12 -176.1(5) . . . . ? C9 N10 C10 C1 -179.2(5) . . . . ? Ru1 N10 C10 C1 4.6(7) . . . . ? N1 C1 C10 N10 -1.1(8) . . . . ? C11 C1 C10 N10 177.4(5) . . . . ? N1 C1 C10 C12 179.6(6) . . . . ? C11 C1 C10 C12 -1.9(9) . . . . ? C3 C4 C11 C1 1.0(10) . . . . ? C3 C4 C11 C5 179.9(7) . . . . ? N1 C1 C11 C4 -0.1(9) . . . . ? C10 C1 C11 C4 -178.5(6) . . . . ? N1 C1 C11 C5 -179.0(6) . . . . ? C10 C1 C11 C5 2.6(9) . . . . ? N2 C5 C11 C4 -0.2(10) . . . . ? C6 C5 C11 C4 179.0(7) . . . . ? N2 C5 C11 C1 178.6(6) . . . . ? C6 C5 C11 C1 -2.1(10) . . . . ? N10 C10 C12 C7 0.0(10) . . . . ? C1 C10 C12 C7 179.2(6) . . . . ? N10 C10 C12 C6 -178.6(6) . . . . ? C1 C10 C12 C6 0.6(9) . . . . ? C8 C7 C12 C10 0.4(10) . . . . ? C8 C7 C12 C6 179.0(6) . . . . ? N5 C6 C12 C10 179.3(6) . . . . ? C5 C6 C12 C10 -0.1(9) . . . . ? N5 C6 C12 C7 0.8(9) . . . . ? C5 C6 C12 C7 -178.6(6) . . . . ? C5 N2 C13 C24 -1.6(10) . . . . ? C5 N2 C13 C14 -179.8(6) . . . . ? N2 C13 C14 C15 1.2(10) . . . . ? C24 C13 C14 C15 -177.0(7) . . . . ? N2 C13 C14 C18 179.9(6) . . . . ? C24 C13 C14 C18 1.6(10) . . . . ? C18 C14 C15 C16 3.1(11) . . . . ? C13 C14 C15 C16 -178.3(7) . . . . ? C14 C15 C16 C17 -3.0(12) . . . . ? C18 N3 C17 C16 1.7(14) . . . . ? C15 C16 C17 N3 0.6(14) . . . . ? C17 N3 C18 C14 -1.6(11) . . . . ? C17 N3 C18 C19 178.9(7) . . . . ? C15 C14 C18 N3 -0.7(11) . . . . ? C13 C14 C18 N3 -179.4(6) . . . . ? C15 C14 C18 C19 178.7(7) . . . . ? C13 C14 C18 C19 0.0(10) . . . . ? C20 N4 C19 C23 -1.5(12) . . . . ? C20 N4 C19 C18 178.7(8) . . . . ? N3 C18 C19 N4 -1.8(11) . . . . ? C14 C18 C19 N4 178.7(7) . . . . ? N3 C18 C19 C23 178.4(6) . . . . ? C14 C18 C19 C23 -1.1(11) . . . . ? C19 N4 C20 C21 -1.0(14) . . . . ? N4 C20 C21 C22 2.2(15) . . . . ? C20 C21 C22 C23 -0.6(13) . . . . ? C21 C22 C23 C19 -1.8(11) . . . . ? C21 C22 C23 C24 -179.5(7) . . . . ? N4 C19 C23 C22 3.0(11) . . . . ? C18 C19 C23 C22 -177.2(7) . . . . ? N4 C19 C23 C24 -179.3(6) . . . . ? C18 C19 C23 C24 0.5(10) . . . . ? C6 N5 C24 C13 -1.6(10) . . . . ? C6 N5 C24 C23 -178.7(6) . . . . ? N2 C13 C24 N5 2.4(11) . . . . ? C14 C13 C24 N5 -179.4(6) . . . . ? N2 C13 C24 C23 179.6(6) . . . . ? C14 C13 C24 C23 -2.2(10) . . . . ? C22 C23 C24 N5 -4.1(11) . . . . ? C19 C23 C24 N5 178.3(6) . . . . ? C22 C23 C24 C13 178.8(7) . . . . ? C19 C23 C24 C13 1.2(10) . . . . ? C29 N6 C25 C26 -3.5(10) . . . . ? Ru1 N6 C25 C26 172.6(6) . . . . ? N6 C25 C26 C27 1.9(12) . . . . ? C25 C26 C27 C28 -0.1(13) . . . . ? C25 C26 C27 C35 -178.6(8) . . . . ? C26 C27 C28 C29 0.1(12) . . . . ? C35 C27 C28 C29 178.4(8) . . . . ? C25 N6 C29 C28 3.3(9) . . . . ? Ru1 N6 C29 C28 -173.1(5) . . . . ? C25 N6 C29 C30 -176.1(6) . . . . ? Ru1 N6 C29 C30 7.5(7) . . . . ? C27 C28 C29 N6 -1.8(11) . . . . ? C27 C28 C29 C30 177.6(8) . . . . ? C34 N7 C30 C31 1.0(12) . . . . ? Ru1 N7 C30 C31 -175.6(6) . . . . ? C34 N7 C30 C29 178.1(7) . . . . ? Ru1 N7 C30 C29 1.5(8) . . . . ? N6 C29 C30 C31 171.1(7) . . . . ? C28 C29 C30 C31 -8.3(12) . . . . ? N6 C29 C30 N7 -5.9(9) . . . . ? C28 C29 C30 N7 174.7(7) . . . . ? N7 C30 C31 C32 -0.4(13) . . . . ? C29 C30 C31 C32 -177.3(8) . . . . ? C30 C31 C32 C33 -1.0(14) . . . . ? C30 C31 C32 C39 178.3(10) . . . . ? C31 C32 C33 C34 1.9(15) . . . . ? C39 C32 C33 C34 -177.4(10) . . . . ? C30 N7 C34 C33 -0.1(13) . . . . ? Ru1 N7 C34 C33 176.0(7) . . . . ? C32 C33 C34 N7 -1.4(15) . . . . ? C26 C27 C35 C38 179.3(10) . . . . ? C28 C27 C35 C38 1.0(14) . . . . ? C26 C27 C35 C36 53.7(13) . . . . ? C28 C27 C35 C36 -124.6(10) . . . . ? C26 C27 C35 C37 -64.2(11) . . . . ? C28 C27 C35 C37 117.5(10) . . . . ? C33 C32 C39 C40A 180(2) . . . . ? C31 C32 C39 C40A 0(2) . . . . ? C33 C32 C39 C42 10.6(19) . . . . ? C31 C32 C39 C42 -168.7(14) . . . . ? C33 C32 C39 C41A -47.3(19) . . . . ? C31 C32 C39 C41A 133.4(16) . . . . ? C33 C32 C39 C41 -113.6(13) . . . . ? C31 C32 C39 C41 67.2(14) . . . . ? C33 C32 C39 C40 132.2(14) . . . . ? C31 C32 C39 C40 -47.1(17) . . . . ? C33 C32 C39 C42A 57.9(18) . . . . ? C31 C32 C39 C42A -121.3(16) . . . . ? C47 N8 C43 C44 -1.0(12) . . . . ? Ru1 N8 C43 C44 -179.0(7) . . . . ? N8 C43 C44 C45 1.9(14) . . . . ? C43 C44 C45 C46 -2.4(14) . . . . ? C43 C44 C45 C53 -179.1(9) . . . . ? C44 C45 C46 C47 2.1(13) . . . . ? C53 C45 C46 C47 178.8(9) . . . . ? C45 C46 C47 N8 -1.3(12) . . . . ? C45 C46 C47 C48 -178.8(8) . . . . ? C43 N8 C47 C46 0.7(11) . . . . ? Ru1 N8 C47 C46 178.9(6) . . . . ? C43 N8 C47 C48 178.4(7) . . . . ? Ru1 N8 C47 C48 -3.4(8) . . . . ? C52 N9 C48 C49 8.4(10) . . . . ? Ru1 N9 C48 C49 -172.1(6) . . . . ? C52 N9 C48 C47 -172.5(7) . . . . ? Ru1 N9 C48 C47 7.0(8) . . . . ? C46 C47 C48 C49 -5.6(12) . . . . ? N8 C47 C48 C49 176.7(7) . . . . ? C46 C47 C48 N9 175.3(7) . . . . ? N8 C47 C48 N9 -2.4(9) . . . . ? N9 C48 C49 C50 -1.5(12) . . . . ? C47 C48 C49 C50 179.5(7) . . . . ? C48 C49 C50 C51 -4.8(12) . . . . ? C48 C49 C50 C57 178.9(8) . . . . ? C49 C50 C51 C52 4.4(13) . . . . ? C57 C50 C51 C52 -179.4(8) . . . . ? C48 N9 C52 C51 -9.2(11) . . . . ? Ru1 N9 C52 C51 171.4(6) . . . . ? C50 C51 C52 N9 2.9(13) . . . . ? C44 C45 C53 C55 -138.2(10) . . . . ? C46 C45 C53 C55 45.2(13) . . . . ? C44 C45 C53 C56 103.4(11) . . . . ? C46 C45 C53 C56 -73.2(12) . . . . ? C44 C45 C53 C54 -16.3(15) . . . . ? C46 C45 C53 C54 167.1(10) . . . . ? C51 C50 C57 C58A -159(2) . . . . ? C49 C50 C57 C58A 17(2) . . . . ? C51 C50 C57 C60A 70(2) . . . . ? C49 C50 C57 C60A -114.4(19) . . . . ? C51 C50 C57 C60 34.7(16) . . . . ? C49 C50 C57 C60 -149.3(13) . . . . ? C51 C50 C57 C59 -89.5(13) . . . . ? C49 C50 C57 C59 86.5(13) . . . . ? C51 C50 C57 C58 151.3(10) . . . . ? C49 C50 C57 C58 -32.7(13) . . . . ? C51 C50 C57 C59A -40.5(18) . . . . ? C49 C50 C57 C59A 135.5(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.122 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.128 #===END OF ALL DATA # Attachment '6_2.cif' # # Paper Ref.: B917484B # data_mk0801 _database_code_depnum_ccdc_archive 'CCDC 730641' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49.94 H55.88 Br2 N6 O3 Ru, 2(F6 P)' _chemical_formula_sum 'C49.94 H55.88 Br2 F12 N6 O3 P2 Ru' _chemical_formula_weight 1338.99 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2440(7) _cell_length_b 16.7226(17) _cell_length_c 16.7455(14) _cell_angle_alpha 72.255(7) _cell_angle_beta 87.076(5) _cell_angle_gamma 71.488(7) _cell_volume 2840.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 113 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1347 _exptl_absorpt_coefficient_mu 1.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.666 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \w-rotations with 2.00 \% and 120 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66504 _diffrn_reflns_av_R_equivalents 0.1129 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 25.68 _reflns_number_total 10765 _reflns_number_gt 7198 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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. Considerable disorder indicates high reactivity of the compound and the presence of a mixture of compounds within the crystal structure. Details are discussed in the paper. ; _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^)+(0.0915P)^2^+24.1781P] 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 10765 _refine_ls_number_parameters 856 _refine_ls_number_restraints 558 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_gt 0.0893 _refine_ls_wR_factor_ref 0.2500 _refine_ls_wR_factor_gt 0.2233 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.114 _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 Ru1 Ru 0.08495(6) 0.31854(4) 0.30338(4) 0.0283(2) Uani 1 1 d . . . Br1 Br 0.21632(15) 0.48137(12) -0.03674(8) 0.0891(5) Uani 1 1 d . . . Br2 Br -0.19174(13) 0.48325(10) 0.54874(9) 0.0807(5) Uani 1 1 d . . . N1 N 0.0855(7) 0.4231(5) 0.2003(5) 0.0410(18) Uani 1 1 d . . . N2 N 0.2368(6) 0.3181(5) 0.3676(4) 0.0335(16) Uani 1 1 d . . . N3 N 0.0847(6) 0.2254(4) 0.4161(4) 0.0283(14) Uani 1 1 d . . . N4 N 0.1818(6) 0.2187(5) 0.2554(4) 0.0313(15) Uani 1 1 d . . . N5 N -0.0561(6) 0.3020(4) 0.2428(4) 0.0311(15) Uani 1 1 d . . . N10 N -0.0211(7) 0.4244(5) 0.3426(5) 0.0386(17) Uani 1 1 d . . . C1 C 0.0205(10) 0.5042(6) 0.2063(7) 0.052(3) Uani 1 1 d . E . C2 C 0.1415(10) 0.4181(7) 0.1271(6) 0.047(2) Uani 1 1 d . . . H2A H 0.1874 0.3618 0.1214 0.056 Uiso 1 1 calc R . . C3 C 0.1322(12) 0.4956(9) 0.0595(7) 0.062(3) Uani 1 1 d . . . C4 C 0.0685(16) 0.5762(9) 0.0680(9) 0.090(5) Uani 1 1 d . E . H4A H 0.0651 0.6285 0.0236 0.108 Uiso 1 1 calc R . . C7 C -0.1502(14) 0.5760(9) 0.3848(10) 0.085(4) Uani 1 1 d . E . H7A H -0.1984 0.6279 0.3981 0.102 Uiso 1 1 calc R . . C8 C -0.1303(10) 0.4962(7) 0.4423(7) 0.056(3) Uani 1 1 d . . . C9 C -0.0700(8) 0.4213(6) 0.4178(6) 0.043(2) Uani 1 1 d . . . H9A H -0.0631 0.3649 0.4565 0.051 Uiso 1 1 calc R . . C10 C -0.0368(11) 0.5041(7) 0.2878(7) 0.056(3) Uani 1 1 d . E . C11 C 0.0068(14) 0.5825(8) 0.1435(9) 0.080(4) Uani 1 1 d . . . C12 C -0.1005(15) 0.5832(7) 0.3056(9) 0.083(4) Uani 1 1 d . . . C13 C 0.3183(9) 0.3638(6) 0.3352(6) 0.044(2) Uani 1 1 d . . . H13A H 0.3028 0.4027 0.2793 0.053 Uiso 1 1 calc R . . C14 C 0.4231(9) 0.3554(7) 0.3811(6) 0.044(2) Uani 1 1 d . . . H14A H 0.4780 0.3881 0.3562 0.052 Uiso 1 1 calc R . . C15 C 0.4484(8) 0.2999(6) 0.4626(7) 0.044(2) Uani 1 1 d . A . C16 C 0.3629(8) 0.2554(6) 0.4960(6) 0.0355(19) Uani 1 1 d . . . H16A H 0.3755 0.2181 0.5525 0.043 Uiso 1 1 calc R . . C17 C 0.2593(7) 0.2646(5) 0.4480(5) 0.0292(17) Uani 1 1 d . . . C18 C 0.1724(7) 0.2130(5) 0.4767(5) 0.0310(18) Uani 1 1 d . . . C19 C 0.1779(8) 0.1557(6) 0.5563(5) 0.037(2) Uani 1 1 d . . . H19A H 0.2366 0.1512 0.5976 0.044 Uiso 1 1 calc R . . C20 C 0.0979(9) 0.1041(6) 0.5768(6) 0.043(2) Uani 1 1 d . . . C21 C 0.0106(8) 0.1168(6) 0.5148(6) 0.042(2) Uani 1 1 d . . . H21A H -0.0471 0.0843 0.5267 0.051 Uiso 1 1 calc R . . C22 C 0.0065(8) 0.1762(6) 0.4356(6) 0.039(2) Uani 1 1 d . . . H22A H -0.0529 0.1825 0.3940 0.047 Uiso 1 1 calc R . . C23 C 0.5664(10) 0.2884(8) 0.5122(8) 0.059(3) Uani 1 1 d D . . C24 C 0.6816(17) 0.2661(15) 0.4621(13) 0.091(6) Uani 0.786(13) 1 d PU A 1 H24A H 0.6650 0.3065 0.4046 0.136 Uiso 0.786(13) 1 calc PR A 1 H24B H 0.7017 0.2050 0.4610 0.136 Uiso 0.786(13) 1 calc PR A 1 H24C H 0.7527 0.2724 0.4884 0.136 Uiso 0.786(13) 1 calc PR A 1 C25 C 0.5776(15) 0.2229(11) 0.6001(10) 0.067(4) Uani 0.786(13) 1 d PDU A 1 H25A H 0.5046 0.2445 0.6313 0.101 Uiso 0.786(13) 1 calc PR A 1 H25B H 0.6544 0.2171 0.6297 0.101 Uiso 0.786(13) 1 calc PR A 1 H25C H 0.5811 0.1651 0.5958 0.101 Uiso 0.786(13) 1 calc PR A 1 C26 C 0.5493(15) 0.3829(10) 0.5232(11) 0.069(4) Uani 0.786(13) 1 d PU A 1 H26A H 0.5462 0.4261 0.4679 0.103 Uiso 0.786(13) 1 calc PR A 1 H26B H 0.6203 0.3786 0.5576 0.103 Uiso 0.786(13) 1 calc PR A 1 H26C H 0.4710 0.4018 0.5508 0.103 Uiso 0.786(13) 1 calc PR A 1 C24A C 0.667(7) 0.330(6) 0.466(5) 0.090(8) Uani 0.214(13) 1 d PU A 2 H24D H 0.6388 0.3938 0.4595 0.136 Uiso 0.214(13) 1 calc PR A 2 H24E H 0.6782 0.3214 0.4105 0.136 Uiso 0.214(13) 1 calc PR A 2 H24F H 0.7470 0.3017 0.4990 0.136 Uiso 0.214(13) 1 calc PR A 2 C25A C 0.636(5) 0.1884(14) 0.542(4) 0.070(7) Uani 0.214(13) 1 d PDU A 2 H25D H 0.6254 0.1623 0.4991 0.105 Uiso 0.214(13) 1 calc PR A 2 H25E H 0.6003 0.1612 0.5943 0.105 Uiso 0.214(13) 1 calc PR A 2 H25F H 0.7250 0.1780 0.5527 0.105 Uiso 0.214(13) 1 calc PR A 2 C26A C 0.531(6) 0.304(4) 0.596(4) 0.069(5) Uani 0.214(13) 1 d PU A 2 H26D H 0.4559 0.3560 0.5877 0.104 Uiso 0.214(13) 1 calc PR A 2 H26E H 0.6006 0.3147 0.6196 0.104 Uiso 0.214(13) 1 calc PR A 2 H26F H 0.5144 0.2521 0.6343 0.104 Uiso 0.214(13) 1 calc PR A 2 C27 C 0.1088(12) 0.0332(9) 0.6638(8) 0.070(3) Uani 1 1 d . . . C28 C 0.1795(17) -0.0570(8) 0.6497(9) 0.097(5) Uani 1 1 d . . . H28A H 0.1775 -0.1051 0.7004 0.146 Uiso 1 1 calc R . . H28B H 0.2669 -0.0604 0.6377 0.146 Uiso 1 1 calc R . . H28C H 0.1388 -0.0626 0.6022 0.146 Uiso 1 1 calc R . . C29 C 0.1852(15) 0.0441(9) 0.7266(7) 0.084(4) Uani 1 1 d . . . H29A H 0.1439 0.1010 0.7367 0.126 Uiso 1 1 calc R . . H29B H 0.2686 0.0426 0.7055 0.126 Uiso 1 1 calc R . . H29C H 0.1938 -0.0040 0.7792 0.126 Uiso 1 1 calc R . . C30 C -0.0086(18) 0.0291(17) 0.6986(10) 0.161(10) Uani 1 1 d . . . H30A H -0.0551 0.0858 0.7078 0.241 Uiso 1 1 calc R . . H30B H 0.0065 -0.0183 0.7523 0.241 Uiso 1 1 calc R . . H30C H -0.0579 0.0170 0.6597 0.241 Uiso 1 1 calc R . . C31 C 0.3067(8) 0.1727(6) 0.2706(6) 0.041(2) Uani 1 1 d . . . H31A H 0.3540 0.1886 0.3051 0.049 Uiso 1 1 calc R . . C32 C 0.3675(8) 0.1053(6) 0.2392(6) 0.043(2) Uani 1 1 d . . . H32A H 0.4543 0.0748 0.2533 0.052 Uiso 1 1 calc R . . C33 C 0.3040(9) 0.0810(7) 0.1869(6) 0.046(2) Uani 1 1 d . . . C34 C 0.1755(8) 0.1279(6) 0.1699(6) 0.041(2) Uani 1 1 d . . . H34A H 0.1279 0.1138 0.1341 0.050 Uiso 1 1 calc R . . C35 C 0.1173(8) 0.1952(5) 0.2056(5) 0.0307(18) Uani 1 1 d . . . C36 C -0.0197(8) 0.2444(5) 0.1966(5) 0.0319(18) Uani 1 1 d . . . C37 C -0.1079(9) 0.2334(6) 0.1482(6) 0.040(2) Uani 1 1 d . . . H37A H -0.0805 0.1936 0.1160 0.048 Uiso 1 1 calc R . . C38 C -0.2345(9) 0.2797(6) 0.1467(6) 0.043(2) Uani 1 1 d . B . C39 C -0.2695(8) 0.3359(6) 0.1960(6) 0.044(2) Uani 1 1 d . . . H39A H -0.3558 0.3673 0.1981 0.053 Uiso 1 1 calc R . . C40 C -0.1808(8) 0.3469(7) 0.2419(5) 0.042(2) Uani 1 1 d . . . H40A H -0.2075 0.3869 0.2740 0.050 Uiso 1 1 calc R . . C41 C 0.3684(11) 0.0065(8) 0.1476(9) 0.068(3) Uani 1 1 d . . . C42 C 0.5093(12) -0.0330(13) 0.1708(13) 0.122(7) Uani 1 1 d . . . H42A H 0.5489 0.0135 0.1504 0.183 Uiso 1 1 calc R . . H42B H 0.5466 -0.0799 0.1449 0.183 Uiso 1 1 calc R . . H42C H 0.5226 -0.0578 0.2320 0.183 Uiso 1 1 calc R . . C43 C 0.3461(14) 0.0444(12) 0.0513(9) 0.102(5) Uani 1 1 d . . . H43A H 0.3861 0.0904 0.0298 0.152 Uiso 1 1 calc R . . H43B H 0.2557 0.0699 0.0370 0.152 Uiso 1 1 calc R . . H43C H 0.3823 -0.0032 0.0260 0.152 Uiso 1 1 calc R . . C44 C 0.3063(12) -0.0643(8) 0.1786(11) 0.086(5) Uani 1 1 d . . . H44A H 0.2150 -0.0373 0.1693 0.129 Uiso 1 1 calc R . . H44B H 0.3274 -0.0940 0.2387 0.129 Uiso 1 1 calc R . . H44C H 0.3361 -0.1078 0.1478 0.129 Uiso 1 1 calc R . . C45 C -0.3333(11) 0.2706(8) 0.0933(8) 0.070(4) Uani 1 1 d . . . C46 C -0.2833(18) 0.2023(13) 0.0490(13) 0.075(4) Uani 0.698(13) 1 d PU B 1 H46A H -0.2458 0.1442 0.0903 0.112 Uiso 0.698(13) 1 calc PR B 1 H46B H -0.2193 0.2176 0.0109 0.112 Uiso 0.698(13) 1 calc PR B 1 H46C H -0.3520 0.2003 0.0166 0.112 Uiso 0.698(13) 1 calc PR B 1 C47 C -0.396(2) 0.3611(14) 0.0312(14) 0.081(4) Uani 0.698(13) 1 d PU B 1 H47A H -0.4277 0.4048 0.0616 0.121 Uiso 0.698(13) 1 calc PR B 1 H47B H -0.4665 0.3587 0.0007 0.121 Uiso 0.698(13) 1 calc PR B 1 H47C H -0.3353 0.3783 -0.0087 0.121 Uiso 0.698(13) 1 calc PR B 1 C48 C -0.4365(18) 0.2433(14) 0.1546(13) 0.082(4) Uani 0.698(13) 1 d PU B 1 H48A H -0.4641 0.2835 0.1889 0.123 Uiso 0.698(13) 1 calc PR B 1 H48B H -0.4004 0.1825 0.1913 0.123 Uiso 0.698(13) 1 calc PR B 1 H48C H -0.5086 0.2473 0.1214 0.123 Uiso 0.698(13) 1 calc PR B 1 C46A C -0.322(4) 0.172(3) 0.120(3) 0.077(5) Uani 0.302(13) 1 d PU B 2 H46D H -0.3247 0.1497 0.1807 0.116 Uiso 0.302(13) 1 calc PR B 2 H46E H -0.2417 0.1387 0.1019 0.116 Uiso 0.302(13) 1 calc PR B 2 H46F H -0.3912 0.1644 0.0929 0.116 Uiso 0.302(13) 1 calc PR B 2 C47A C -0.282(4) 0.292(3) -0.003(3) 0.078(5) Uani 0.302(13) 1 d PU B 2 H47D H -0.3077 0.3560 -0.0300 0.118 Uiso 0.302(13) 1 calc PR B 2 H47E H -0.3181 0.2646 -0.0357 0.118 Uiso 0.302(13) 1 calc PR B 2 H47F H -0.1903 0.2674 -0.0004 0.118 Uiso 0.302(13) 1 calc PR B 2 C48A C -0.452(5) 0.342(3) 0.081(3) 0.085(6) Uani 0.302(13) 1 d PU B 2 H48D H -0.4833 0.3470 0.1351 0.128 Uiso 0.302(13) 1 calc PR B 2 H48E H -0.5137 0.3281 0.0516 0.128 Uiso 0.302(13) 1 calc PR B 2 H48F H -0.4407 0.3973 0.0466 0.128 Uiso 0.302(13) 1 calc PR B 2 P1 P 0.5000 0.0000 0.5000 0.0646(12) Uani 1 2 d SD . . F11 F 0.4587(7) 0.0431(4) 0.5745(4) 0.075(2) Uani 1 1 d D . . F12 F 0.4926(8) -0.0926(4) 0.5601(5) 0.087(2) Uani 1 1 d D . . F13 F 0.6428(7) -0.0293(5) 0.5310(5) 0.085(2) Uani 1 1 d D . . P2 P 0.0000 0.0000 0.0000 0.122(3) Uani 1 2 d SD . . F21 F 0.023(3) 0.0740(17) 0.036(2) 0.096(6) Uani 0.51(4) 1 d PDU C 1 F21A F -0.002(3) 0.045(2) 0.072(2) 0.099(7) Uani 0.49(4) 1 d PDU C 2 F22 F 0.1251(18) -0.069(2) 0.044(3) 0.207(8) Uani 0.51(4) 1 d PDU C 1 F22A F 0.121(2) -0.073(3) 0.038(3) 0.208(8) Uani 0.49(4) 1 d PDU C 2 F23 F -0.080(2) -0.0498(14) 0.0746(13) 0.308(11) Uani 1 1 d DU C . P3 P -0.4401(8) 0.5808(5) 0.2356(5) 0.1156(19) Uani 0.751(6) 1 d PDU D 1 F31 F -0.5708(14) 0.5839(10) 0.2897(9) 0.129(3) Uani 0.751(6) 1 d PDU D 1 F32 F -0.3073(13) 0.5703(9) 0.1908(8) 0.122(3) Uani 0.751(6) 1 d PDU D 1 F33 F -0.3706(13) 0.4968(9) 0.3102(9) 0.121(4) Uani 0.751(6) 1 d PDU D 1 F34 F -0.4107(13) 0.6448(9) 0.2767(9) 0.125(4) Uani 0.751(6) 1 d PDU D 1 F35 F -0.5157(14) 0.6664(10) 0.1615(9) 0.136(4) Uani 0.751(6) 1 d PDU D 1 F36 F -0.4735(15) 0.5134(10) 0.1964(10) 0.133(3) Uani 0.751(6) 1 d PDU D 1 P3A P -0.534(2) 0.5615(13) 0.2268(13) 0.122(3) Uani 0.249(6) 1 d PDU D 2 F31A F -0.569(3) 0.481(2) 0.201(2) 0.124(5) Uani 0.249(6) 1 d PDU D 2 F32A F -0.520(4) 0.646(2) 0.247(2) 0.127(4) Uani 0.249(6) 1 d PDU D 2 F33A F -0.644(3) 0.629(2) 0.163(2) 0.138(6) Uani 0.249(6) 1 d PDU D 2 F34A F -0.434(3) 0.561(2) 0.1576(19) 0.120(4) Uani 0.249(6) 1 d PDU D 2 F35A F -0.421(3) 0.488(2) 0.290(2) 0.121(4) Uani 0.249(6) 1 d PDU D 2 F36A F -0.638(3) 0.550(2) 0.295(2) 0.127(5) Uani 0.249(6) 1 d PDU D 2 O100 O 0.127(2) 0.6337(15) 0.2564(14) 0.135(7) Uani 0.646(13) 1 d PU E 1 C101 C 0.003(2) 0.7392(17) 0.1345(16) 0.093(7) Uani 0.646(13) 1 d PU E 1 H10A H 0.0488 0.7347 0.0832 0.111 Uiso 0.646(13) 1 calc PR E 1 H10B H -0.0488 0.8016 0.1261 0.111 Uiso 0.646(13) 1 calc PR E 1 C102 C 0.095(3) 0.704(2) 0.213(2) 0.133(11) Uani 0.646(13) 1 d PU E 1 C103 C 0.1818(9) 0.7606(6) 0.2100(6) 0.138(11) Uani 0.646(13) 1 d PU E 1 H10C H 0.1493 0.8178 0.1664 0.206 Uiso 0.646(13) 1 calc PR E 1 H10D H 0.2668 0.7294 0.1973 0.206 Uiso 0.646(13) 1 calc PR E 1 H10E H 0.1842 0.7704 0.2646 0.206 Uiso 0.646(13) 1 calc PR E 1 C5 C -0.0812(9) 0.6750(6) 0.1581(6) 0.118(6) Uani 0.646(13) 1 d PRU E 1 C6 C -0.1054(9) 0.6686(6) 0.2324(6) 0.121(6) Uani 0.646(13) 1 d PRU E 1 O1 O -0.1740(9) 0.7232(6) 0.0931(6) 0.134(6) Uani 0.646(13) 1 d PRU E 1 H1 H -0.1428 0.7212 0.0468 0.201 Uiso 0.646(13) 1 calc PR E 1 O3 O -0.2178(9) 0.7520(6) 0.2531(6) 0.127(6) Uani 0.646(13) 1 d PRU E 1 O1A O -0.1092(9) 0.7337(6) 0.0324(6) 0.130(12) Uani 0.354(13) 1 d PRU E 2 O3A O -0.2487(9) 0.7443(6) 0.2270(6) 0.089(7) Uani 0.354(13) 1 d PRU E 2 O4A O -0.0575(9) 0.7270(6) 0.2834(6) 0.087(7) Uani 0.354(13) 1 d PRU E 2 C5A C 0.0081(9) 0.6800(6) 0.1350(6) 0.051(7) Uani 0.354(13) 1 d PRU E 2 C6A C -0.1637(9) 0.6820(6) 0.2697(6) 0.061(6) Uani 0.354(13) 1 d PRU E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0317(4) 0.0278(3) 0.0266(4) -0.0076(3) 0.0015(2) -0.0119(3) Br1 0.1123(11) 0.1281(13) 0.0374(7) -0.0013(7) 0.0165(7) -0.0769(10) Br2 0.0783(9) 0.1083(11) 0.0908(10) -0.0769(9) 0.0309(7) -0.0369(8) N1 0.050(5) 0.037(4) 0.040(4) -0.010(3) 0.002(3) -0.021(4) N2 0.034(4) 0.040(4) 0.035(4) -0.019(3) 0.007(3) -0.017(3) N3 0.026(3) 0.029(4) 0.031(4) -0.008(3) 0.004(3) -0.012(3) N4 0.037(4) 0.037(4) 0.026(4) -0.009(3) 0.002(3) -0.020(3) N5 0.032(4) 0.034(4) 0.027(4) -0.006(3) 0.007(3) -0.013(3) N10 0.043(4) 0.027(4) 0.045(5) -0.013(3) 0.000(3) -0.009(3) C1 0.062(7) 0.038(5) 0.054(6) -0.006(5) -0.008(5) -0.018(5) C2 0.060(6) 0.056(6) 0.030(5) -0.006(4) 0.001(4) -0.033(5) C3 0.071(8) 0.076(8) 0.048(6) -0.008(6) 0.010(5) -0.046(7) C4 0.128(13) 0.059(8) 0.065(9) 0.023(7) -0.016(8) -0.041(9) C7 0.105(11) 0.051(7) 0.095(11) -0.040(8) 0.027(9) -0.005(7) C8 0.047(6) 0.053(6) 0.061(7) -0.025(5) 0.015(5) -0.002(5) C9 0.043(5) 0.046(5) 0.044(5) -0.027(5) 0.002(4) -0.010(4) C10 0.075(8) 0.039(6) 0.054(7) -0.015(5) 0.001(5) -0.018(5) C11 0.107(11) 0.047(7) 0.065(8) 0.012(6) -0.007(7) -0.024(7) C12 0.121(12) 0.027(6) 0.092(10) -0.020(6) -0.005(9) -0.006(6) C13 0.058(6) 0.050(6) 0.039(5) -0.020(4) 0.005(4) -0.030(5) C14 0.049(5) 0.053(6) 0.045(6) -0.023(5) 0.011(4) -0.032(5) C15 0.036(5) 0.047(5) 0.063(7) -0.030(5) 0.005(4) -0.020(4) C16 0.036(5) 0.040(5) 0.036(5) -0.021(4) -0.005(4) -0.010(4) C17 0.028(4) 0.032(4) 0.029(4) -0.015(3) 0.003(3) -0.006(3) C18 0.028(4) 0.034(4) 0.032(4) -0.014(4) 0.000(3) -0.007(4) C19 0.037(5) 0.044(5) 0.028(4) -0.009(4) 0.005(4) -0.015(4) C20 0.050(5) 0.050(6) 0.032(5) -0.008(4) 0.002(4) -0.022(5) C21 0.034(5) 0.044(5) 0.048(6) -0.001(4) 0.004(4) -0.022(4) C22 0.037(5) 0.032(5) 0.043(5) -0.005(4) -0.004(4) -0.010(4) C23 0.042(6) 0.084(8) 0.072(8) -0.036(6) -0.001(5) -0.035(6) C24 0.071(8) 0.101(9) 0.098(8) -0.027(7) 0.006(6) -0.027(7) C25 0.063(6) 0.072(6) 0.073(6) -0.019(5) -0.015(5) -0.031(5) C26 0.073(7) 0.070(7) 0.080(7) -0.027(5) -0.016(5) -0.038(5) C24A 0.079(10) 0.097(11) 0.095(10) -0.027(8) 0.004(8) -0.030(8) C25A 0.066(9) 0.074(9) 0.074(9) -0.019(7) -0.007(7) -0.030(7) C26A 0.070(7) 0.073(7) 0.073(7) -0.024(6) -0.010(6) -0.029(6) C27 0.072(8) 0.076(8) 0.056(7) 0.007(6) -0.004(6) -0.041(7) C28 0.160(16) 0.050(8) 0.074(9) 0.006(7) -0.022(9) -0.042(9) C29 0.133(12) 0.089(10) 0.030(6) 0.007(6) -0.019(7) -0.057(9) C30 0.127(15) 0.27(3) 0.060(10) 0.030(13) 0.036(10) -0.114(18) C31 0.028(4) 0.053(6) 0.049(6) -0.020(5) 0.003(4) -0.020(4) C32 0.027(4) 0.044(5) 0.059(6) -0.019(5) 0.010(4) -0.011(4) C33 0.045(5) 0.054(6) 0.043(6) -0.019(5) 0.016(4) -0.022(5) C34 0.039(5) 0.055(6) 0.046(5) -0.026(5) 0.008(4) -0.028(5) C35 0.036(4) 0.037(5) 0.024(4) -0.011(3) 0.006(3) -0.018(4) C36 0.037(5) 0.035(4) 0.022(4) -0.001(3) 0.001(3) -0.015(4) C37 0.047(5) 0.042(5) 0.035(5) -0.007(4) -0.001(4) -0.022(4) C38 0.047(6) 0.048(6) 0.030(5) 0.009(4) -0.014(4) -0.025(5) C39 0.030(5) 0.049(6) 0.042(5) -0.001(4) -0.008(4) -0.009(4) C40 0.039(5) 0.053(6) 0.028(5) -0.003(4) 0.001(4) -0.015(4) C41 0.054(7) 0.080(8) 0.094(9) -0.066(8) 0.013(6) -0.017(6) C42 0.044(7) 0.166(17) 0.20(2) -0.147(16) 0.013(9) -0.005(9) C43 0.085(10) 0.163(16) 0.077(10) -0.080(11) 0.024(8) -0.028(10) C44 0.065(8) 0.063(8) 0.139(13) -0.061(9) -0.017(8) -0.001(7) C45 0.059(7) 0.063(7) 0.081(9) -0.003(6) -0.041(6) -0.022(6) C46 0.071(6) 0.083(7) 0.078(7) -0.029(6) -0.012(5) -0.028(5) C47 0.075(7) 0.087(7) 0.081(7) -0.019(6) -0.018(6) -0.029(6) C48 0.074(6) 0.091(7) 0.085(7) -0.020(6) -0.002(6) -0.038(6) C46A 0.073(7) 0.084(7) 0.082(7) -0.025(6) -0.007(6) -0.034(6) C47A 0.075(7) 0.085(7) 0.079(7) -0.024(6) -0.011(6) -0.028(6) C48A 0.079(7) 0.090(8) 0.086(8) -0.023(6) -0.007(6) -0.029(6) P1 0.069(3) 0.049(2) 0.055(3) -0.014(2) 0.002(2) 0.007(2) F11 0.084(5) 0.059(4) 0.064(4) -0.025(3) -0.003(3) 0.011(3) F12 0.118(6) 0.055(4) 0.073(5) -0.016(4) 0.007(4) -0.011(4) F13 0.071(5) 0.082(5) 0.088(5) -0.036(4) 0.000(4) 0.002(4) P2 0.113(5) 0.118(5) 0.140(6) -0.088(5) -0.070(5) 0.015(4) F21 0.109(10) 0.101(11) 0.100(13) -0.060(10) -0.018(9) -0.031(8) F21A 0.113(10) 0.105(11) 0.097(12) -0.056(10) -0.024(9) -0.028(8) F22 0.222(12) 0.193(12) 0.230(13) -0.142(10) -0.112(10) -0.004(9) F22A 0.220(12) 0.196(12) 0.228(13) -0.139(10) -0.115(10) -0.003(10) F23 0.40(2) 0.319(18) 0.282(18) -0.142(15) 0.083(15) -0.174(16) P3 0.117(3) 0.115(3) 0.107(3) -0.049(2) 0.011(2) -0.012(2) F31 0.125(5) 0.128(5) 0.124(5) -0.047(4) 0.018(4) -0.021(4) F32 0.122(6) 0.129(6) 0.096(5) -0.039(5) 0.028(5) -0.015(5) F33 0.116(6) 0.119(6) 0.109(6) -0.034(5) 0.012(5) -0.016(5) F34 0.125(6) 0.121(6) 0.122(6) -0.048(5) 0.008(5) -0.019(5) F35 0.145(6) 0.128(6) 0.118(6) -0.041(5) -0.004(5) -0.014(5) F36 0.135(5) 0.127(5) 0.127(5) -0.049(4) 0.006(4) -0.020(4) P3A 0.125(3) 0.119(3) 0.117(3) -0.045(3) 0.014(3) -0.025(3) F31A 0.127(7) 0.122(7) 0.122(7) -0.044(6) 0.013(6) -0.034(6) F32A 0.130(5) 0.121(5) 0.120(5) -0.045(4) 0.011(5) -0.021(4) F33A 0.136(8) 0.132(8) 0.131(8) -0.039(7) 0.016(7) -0.026(7) F34A 0.122(5) 0.120(5) 0.111(5) -0.041(5) 0.018(5) -0.024(5) F35A 0.122(5) 0.119(5) 0.116(5) -0.043(5) 0.011(5) -0.023(5) F36A 0.128(7) 0.124(7) 0.124(7) -0.045(6) 0.017(6) -0.028(6) O100 0.145(11) 0.133(11) 0.137(11) -0.012(8) -0.017(8) -0.081(9) C101 0.096(8) 0.087(8) 0.098(8) -0.027(5) 0.000(5) -0.033(5) C102 0.135(12) 0.131(12) 0.134(12) -0.043(6) 0.003(5) -0.041(6) C103 0.135(14) 0.129(14) 0.155(15) -0.048(10) 0.002(9) -0.047(10) C5 0.123(6) 0.112(6) 0.121(6) -0.036(4) 0.003(4) -0.037(4) C6 0.127(6) 0.114(6) 0.124(6) -0.037(4) 0.005(4) -0.038(4) O1 0.133(8) 0.124(8) 0.140(8) -0.045(6) -0.017(7) -0.025(6) O3 0.146(8) 0.110(8) 0.137(8) -0.048(6) 0.013(7) -0.048(6) O1A 0.118(15) 0.117(15) 0.133(15) -0.002(9) 0.020(9) -0.043(10) O3A 0.084(9) 0.081(9) 0.087(9) -0.011(7) 0.000(7) -0.019(7) O4A 0.093(9) 0.076(9) 0.088(9) -0.019(7) 0.004(7) -0.027(7) C5A 0.062(11) 0.035(10) 0.053(11) -0.024(8) -0.014(8) 0.004(8) C6A 0.061(7) 0.060(7) 0.064(7) -0.016(4) -0.001(4) -0.025(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N4 2.048(7) . ? Ru1 N3 2.049(6) . ? Ru1 N1 2.051(7) . ? Ru1 N5 2.058(7) . ? Ru1 N2 2.060(7) . ? Ru1 N10 2.069(7) . ? Br1 C3 1.866(12) . ? Br2 C8 1.853(11) . ? N1 C1 1.353(12) . ? N1 C2 1.361(12) . ? N2 C17 1.355(11) . ? N2 C13 1.363(11) . ? N3 C22 1.350(11) . ? N3 C18 1.374(10) . ? N4 C35 1.349(10) . ? N4 C31 1.364(11) . ? N5 C40 1.363(11) . ? N5 C36 1.365(11) . ? N10 C10 1.331(12) . ? N10 C9 1.340(12) . ? C1 C11 1.376(15) . ? C1 C10 1.479(16) . ? C2 C3 1.415(14) . ? C2 H2A 0.9500 . ? C3 C4 1.359(19) . ? C4 C11 1.43(2) . ? C4 H4A 0.9500 . ? C7 C8 1.344(17) . ? C7 C12 1.400(19) . ? C7 H7A 0.9500 . ? C8 C9 1.395(13) . ? C9 H9A 0.9500 . ? C10 C12 1.401(15) . ? C11 C5A 1.597(15) . ? C11 C5 1.633(17) . ? C12 C6A 1.513(14) . ? C12 C6 1.561(15) . ? C13 C14 1.386(13) . ? C13 H13A 0.9500 . ? C14 C15 1.380(14) . ? C14 H14A 0.9500 . ? C15 C16 1.393(13) . ? C15 C23 1.530(13) . ? C16 C17 1.389(11) . ? C16 H16A 0.9500 . ? C17 C18 1.472(11) . ? C18 C19 1.375(12) . ? C19 C20 1.397(13) . ? C19 H19A 0.9500 . ? C20 C21 1.388(13) . ? C20 C27 1.554(14) . ? C21 C22 1.386(12) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C26A 1.51(6) . ? C23 C24 1.51(2) . ? C23 C25 1.527(18) . ? C23 C25A 1.53(2) . ? C23 C24A 1.57(7) . ? C23 C26 1.595(18) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25A H25D 0.9800 . ? C25A H25E 0.9800 . ? C25A H25F 0.9800 . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 0.9800 . ? C27 C30 1.430(19) . ? C27 C29 1.479(17) . ? C27 C28 1.55(2) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.359(13) . ? C31 H31A 0.9500 . ? C32 C33 1.381(14) . ? C32 H32A 0.9500 . ? C33 C34 1.403(13) . ? C33 C41 1.545(14) . ? C34 C35 1.397(12) . ? C34 H34A 0.9500 . ? C35 C36 1.489(12) . ? C36 C37 1.401(12) . ? C37 C38 1.384(13) . ? C37 H37A 0.9500 . ? C38 C39 1.386(14) . ? C38 C45 1.533(13) . ? C39 C40 1.379(13) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C44 1.508(18) . ? C41 C42 1.529(17) . ? C41 C43 1.543(19) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C48A 1.45(5) . ? C45 C46 1.50(2) . ? C45 C47 1.52(2) . ? C45 C46A 1.54(5) . ? C45 C48 1.59(2) . ? C45 C47A 1.66(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C46A H46D 0.9800 . ? C46A H46E 0.9800 . ? C46A H46F 0.9800 . ? C47A H47D 0.9800 . ? C47A H47E 0.9800 . ? C47A H47F 0.9800 . ? C48A H48D 0.9800 . ? C48A H48E 0.9800 . ? C48A H48F 0.9800 . ? P1 F13 1.587(7) . ? P1 F13 1.587(7) 2_656 ? P1 F12 1.594(7) . ? P1 F12 1.594(7) 2_656 ? P1 F11 1.603(6) . ? P1 F11 1.603(6) 2_656 ? P2 F22A 1.52(2) 2 ? P2 F22A 1.52(2) . ? P2 F22 1.551(15) . ? P2 F22 1.551(15) 2 ? P2 F21A 1.602(16) . ? P2 F21A 1.602(16) 2 ? P2 F21 1.619(15) . ? P2 F21 1.619(15) 2 ? P2 F23 1.672(16) . ? P2 F23 1.672(16) 2 ? P3 F34 1.558(16) . ? P3 F33 1.574(15) . ? P3 F35 1.600(15) . ? P3 F36 1.608(17) . ? P3 F32 1.619(14) . ? P3 F31 1.683(17) . ? P3A F33A 1.56(2) . ? P3A F34A 1.57(2) . ? P3A F32A 1.61(2) . ? P3A F35A 1.61(2) . ? P3A F36A 1.61(2) . ? P3A F31A 1.69(2) . ? O100 C102 1.13(4) . ? C101 C102 1.55(4) . ? C101 C5 1.60(2) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 C103 1.56(4) . ? C103 H10C 0.9800 . ? C103 H10D 0.9800 . ? C103 H10E 0.9800 . ? C5 C6 1.2392 . ? C5 O1 1.4043 . ? C6 O3 1.6710 . ? O1 H1 0.8400 . ? O3A C6A 1.2227 . ? O4A C6A 1.6581 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ru1 N3 89.1(3) . . ? N4 Ru1 N1 97.8(3) . . ? N3 Ru1 N1 172.0(3) . . ? N4 Ru1 N5 77.8(3) . . ? N3 Ru1 N5 97.2(3) . . ? N1 Ru1 N5 88.4(3) . . ? N4 Ru1 N2 96.2(3) . . ? N3 Ru1 N2 78.5(3) . . ? N1 Ru1 N2 96.6(3) . . ? N5 Ru1 N2 172.8(3) . . ? N4 Ru1 N10 175.4(3) . . ? N3 Ru1 N10 94.5(3) . . ? N1 Ru1 N10 78.9(3) . . ? N5 Ru1 N10 98.7(3) . . ? N2 Ru1 N10 87.4(3) . . ? C1 N1 C2 118.1(8) . . ? C1 N1 Ru1 115.5(6) . . ? C2 N1 Ru1 126.4(6) . . ? C17 N2 C13 117.9(7) . . ? C17 N2 Ru1 116.3(5) . . ? C13 N2 Ru1 125.8(6) . . ? C22 N3 C18 117.9(7) . . ? C22 N3 Ru1 125.9(6) . . ? C18 N3 Ru1 116.2(5) . . ? C35 N4 C31 116.9(7) . . ? C35 N4 Ru1 117.8(6) . . ? C31 N4 Ru1 125.3(6) . . ? C40 N5 C36 118.1(7) . . ? C40 N5 Ru1 125.3(6) . . ? C36 N5 Ru1 116.5(5) . . ? C10 N10 C9 117.3(8) . . ? C10 N10 Ru1 115.5(7) . . ? C9 N10 Ru1 127.2(6) . . ? N1 C1 C11 124.5(11) . . ? N1 C1 C10 114.8(9) . . ? C11 C1 C10 120.7(11) . . ? N1 C2 C3 120.9(10) . . ? N1 C2 H2A 119.5 . . ? C3 C2 H2A 119.5 . . ? C4 C3 C2 119.7(11) . . ? C4 C3 Br1 122.8(10) . . ? C2 C3 Br1 117.4(10) . . ? C3 C4 C11 120.1(11) . . ? C3 C4 H4A 120.0 . . ? C11 C4 H4A 120.0 . . ? C8 C7 C12 120.5(11) . . ? C8 C7 H7A 119.8 . . ? C12 C7 H7A 119.8 . . ? C7 C8 C9 118.0(10) . . ? C7 C8 Br2 122.2(9) . . ? C9 C8 Br2 119.6(8) . . ? N10 C9 C8 123.7(9) . . ? N10 C9 H9A 118.2 . . ? C8 C9 H9A 118.2 . . ? N10 C10 C12 123.1(11) . . ? N10 C10 C1 115.3(9) . . ? C12 C10 C1 121.5(10) . . ? C1 C11 C4 116.7(12) . . ? C1 C11 C5A 137.8(12) . . ? C4 C11 C5A 96.4(10) . . ? C1 C11 C5 118.9(12) . . ? C4 C11 C5 124.4(10) . . ? C7 C12 C10 117.2(11) . . ? C7 C12 C6A 95.5(10) . . ? C10 C12 C6A 146.1(13) . . ? C7 C12 C6 128.6(10) . . ? C10 C12 C6 114.2(12) . . ? N2 C13 C14 122.2(9) . . ? N2 C13 H13A 118.9 . . ? C14 C13 H13A 118.9 . . ? C15 C14 C13 120.6(8) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C14 C15 C16 116.9(8) . . ? C14 C15 C23 120.5(9) . . ? C16 C15 C23 122.6(9) . . ? C17 C16 C15 121.1(9) . . ? C17 C16 H16A 119.5 . . ? C15 C16 H16A 119.5 . . ? N2 C17 C16 121.4(8) . . ? N2 C17 C18 114.7(7) . . ? C16 C17 C18 123.7(8) . . ? N3 C18 C19 121.9(8) . . ? N3 C18 C17 114.1(7) . . ? C19 C18 C17 123.9(7) . . ? C18 C19 C20 120.5(8) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C21 C20 C19 116.9(8) . . ? C21 C20 C27 121.2(9) . . ? C19 C20 C27 121.9(9) . . ? C22 C21 C20 120.9(8) . . ? C22 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? N3 C22 C21 121.8(8) . . ? N3 C22 H22A 119.1 . . ? C21 C22 H22A 119.1 . . ? C26A C23 C24 140(2) . . ? C26A C23 C25 49(2) . . ? C24 C23 C25 113.5(13) . . ? C26A C23 C15 110(2) . . ? C24 C23 C15 110.4(11) . . ? C25 C23 C15 112.0(9) . . ? C26A C23 C25A 100(3) . . ? C24 C23 C25A 70(3) . . ? C25 C23 C25A 51(2) . . ? C15 C23 C25A 106(2) . . ? C26A C23 C24A 115(4) . . ? C25 C23 C24A 128(3) . . ? C15 C23 C24A 119(3) . . ? C25A C23 C24A 105(4) . . ? C26A C23 C26 60(2) . . ? C24 C23 C26 107.4(13) . . ? C25 C23 C26 107.2(11) . . ? C15 C23 C26 105.8(10) . . ? C25A C23 C26 147(2) . . ? C24A C23 C26 68(3) . . ? 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 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C24A H24D 109.5 . . ? C23 C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C23 C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C23 C25A H25D 109.5 . . ? C23 C25A H25E 109.5 . . ? H25D C25A H25E 109.5 . . ? C23 C25A H25F 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? C23 C26A H26D 109.5 . . ? C23 C26A H26E 109.5 . . ? H26D C26A H26E 109.5 . . ? C23 C26A H26F 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? C30 C27 C29 108.3(14) . . ? C30 C27 C28 108.2(15) . . ? C29 C27 C28 107.0(11) . . ? C30 C27 C20 114.7(12) . . ? C29 C27 C20 112.4(9) . . ? C28 C27 C20 105.9(10) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 N4 123.8(8) . . ? C32 C31 H31A 118.1 . . ? N4 C31 H31A 118.1 . . ? C31 C32 C33 120.4(9) . . ? C31 C32 H32A 119.8 . . ? C33 C32 H32A 119.8 . . ? C32 C33 C34 116.7(9) . . ? C32 C33 C41 122.9(9) . . ? C34 C33 C41 120.4(9) . . ? C35 C34 C33 120.3(8) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? N4 C35 C34 121.8(8) . . ? N4 C35 C36 113.5(7) . . ? C34 C35 C36 124.6(7) . . ? N5 C36 C37 120.8(8) . . ? N5 C36 C35 113.9(7) . . ? C37 C36 C35 125.3(8) . . ? C38 C37 C36 121.0(9) . . ? C38 C37 H37A 119.5 . . ? C36 C37 H37A 119.5 . . ? C37 C38 C39 117.1(8) . . ? C37 C38 C45 122.4(10) . . ? C39 C38 C45 120.5(9) . . ? C40 C39 C38 120.9(9) . . ? C40 C39 H39A 119.6 . . ? C38 C39 H39A 119.6 . . ? N5 C40 C39 122.0(9) . . ? N5 C40 H40A 119.0 . . ? C39 C40 H40A 119.0 . . ? C44 C41 C42 110.0(13) . . ? C44 C41 C43 108.1(11) . . ? C42 C41 C43 110.0(12) . . ? C44 C41 C33 107.9(9) . . ? C42 C41 C33 111.9(9) . . ? C43 C41 C33 108.8(11) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C48A C45 C46 130(2) . . ? C46 C45 C47 110.9(14) . . ? C48A C45 C38 114(2) . . ? C46 C45 C38 114.6(11) . . ? C47 C45 C38 107.8(11) . . ? C48A C45 C46A 124(3) . . ? C46 C45 C46A 48.7(19) . . ? C47 C45 C46A 145(2) . . ? C38 C45 C46A 107.0(18) . . ? C48A C45 C48 67(2) . . ? C46 C45 C48 108.0(13) . . ? C47 C45 C48 108.0(14) . . ? C38 C45 C48 107.4(12) . . ? C46A C45 C48 65(2) . . ? C48A C45 C47A 101(3) . . ? C46 C45 C47A 56.0(18) . . ? C47 C45 C47A 62.2(19) . . ? C38 C45 C47A 104.6(17) . . ? C46A C45 C47A 105(3) . . ? C48 C45 C47A 148.0(18) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C45 C46A H46D 109.5 . . ? C45 C46A H46E 109.5 . . ? H46D C46A H46E 109.5 . . ? C45 C46A H46F 109.5 . . ? H46D C46A H46F 109.5 . . ? H46E C46A H46F 109.5 . . ? C45 C47A H47D 109.5 . . ? C45 C47A H47E 109.5 . . ? H47D C47A H47E 109.5 . . ? C45 C47A H47F 109.5 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? C45 C48A H48D 109.5 . . ? C45 C48A H48E 109.5 . . ? H48D C48A H48E 109.5 . . ? C45 C48A H48F 109.5 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.5 . . ? F13 P1 F13 179.997(1) . 2_656 ? F13 P1 F12 88.7(4) . . ? F13 P1 F12 91.3(4) 2_656 . ? F13 P1 F12 91.3(4) . 2_656 ? F13 P1 F12 88.7(4) 2_656 2_656 ? F12 P1 F12 179.999(1) . 2_656 ? F13 P1 F11 89.9(4) . . ? F13 P1 F11 90.1(4) 2_656 . ? F12 P1 F11 90.2(4) . . ? F12 P1 F11 89.8(4) 2_656 . ? F13 P1 F11 90.1(4) . 2_656 ? F13 P1 F11 89.9(4) 2_656 2_656 ? F12 P1 F11 89.8(4) . 2_656 ? F12 P1 F11 90.2(4) 2_656 2_656 ? F11 P1 F11 179.997(2) . 2_656 ? F22A P2 F22A 180(3) 2 . ? F22A P2 F22 174(5) 2 . ? F22A P2 F22 174(5) . 2 ? F22 P2 F22 179.995(2) . 2 ? F22A P2 F21A 88(3) 2 . ? F22A P2 F21A 92(3) . . ? F22 P2 F21A 86(3) . . ? F22 P2 F21A 94(3) 2 . ? F22A P2 F21A 92(3) 2 2 ? F22A P2 F21A 88(3) . 2 ? F22 P2 F21A 94(3) . 2 ? F22 P2 F21A 86(3) 2 2 ? F21A P2 F21A 179.997(2) . 2 ? F22A P2 F21 83(3) 2 . ? F22A P2 F21 97(3) . . ? F22 P2 F21 91(2) . . ? F22 P2 F21 89(2) 2 . ? F21A P2 F21 152.7(11) 2 . ? F22A P2 F21 97(3) 2 2 ? F22A P2 F21 83(3) . 2 ? F22 P2 F21 89(2) . 2 ? F22 P2 F21 91(2) 2 2 ? F21A P2 F21 152.7(11) . 2 ? F21 P2 F21 179.997(3) . 2 ? F22A P2 F23 89.9(7) 2 . ? F22A P2 F23 90.1(7) . . ? F22 P2 F23 90.1(7) . . ? F22 P2 F23 89.9(7) 2 . ? F21A P2 F23 76.5(18) . . ? F21A P2 F23 103.5(18) 2 . ? F21 P2 F23 103.3(16) . . ? F21 P2 F23 76.7(16) 2 . ? F22A P2 F23 90.1(7) 2 2 ? F22A P2 F23 89.9(7) . 2 ? F22 P2 F23 89.9(7) . 2 ? F22 P2 F23 90.1(7) 2 2 ? F21A P2 F23 103.5(18) . 2 ? F21A P2 F23 76.5(18) 2 2 ? F21 P2 F23 76.7(16) . 2 ? F21 P2 F23 103.3(16) 2 2 ? F23 P2 F23 180.0(17) . 2 ? F34 P3 F33 92.5(9) . . ? F34 P3 F35 87.7(8) . . ? F33 P3 F35 177.8(10) . . ? F34 P3 F36 177.6(10) . . ? F33 P3 F36 86.3(8) . . ? F35 P3 F36 93.4(9) . . ? F34 P3 F32 89.2(9) . . ? F33 P3 F32 88.0(8) . . ? F35 P3 F32 94.2(8) . . ? F36 P3 F32 92.8(9) . . ? F34 P3 F31 90.7(8) . . ? F33 P3 F31 86.6(8) . . ? F35 P3 F31 91.1(8) . . ? F36 P3 F31 87.2(9) . . ? F32 P3 F31 174.7(9) . . ? F33A P3A F34A 93.1(17) . . ? F33A P3A F32A 86.5(17) . . ? F34A P3A F32A 94.7(18) . . ? F33A P3A F35A 176(2) . . ? F34A P3A F35A 86.0(17) . . ? F32A P3A F35A 97.0(17) . . ? F33A P3A F36A 87.3(17) . . ? F34A P3A F36A 172(2) . . ? F32A P3A F36A 92.9(18) . . ? F35A P3A F36A 93.1(17) . . ? F33A P3A F31A 86.6(17) . . ? F34A P3A F31A 88.8(17) . . ? F32A P3A F31A 172.4(19) . . ? F35A P3A F31A 89.9(17) . . ? F36A P3A F31A 83.7(17) . . ? C102 C101 C5 103(2) . . ? C102 C101 H10A 111.3 . . ? C5 C101 H10A 111.3 . . ? C102 C101 H10B 111.3 . . ? C5 C101 H10B 111.3 . . ? H10A C101 H10B 109.2 . . ? O100 C102 C101 126(3) . . ? O100 C102 C103 116(3) . . ? C101 C102 C103 114(3) . . ? C102 C103 H10C 109.5 . . ? C102 C103 H10D 109.5 . . ? H10C C103 H10D 109.5 . . ? C102 C103 H10E 109.5 . . ? H10C C103 H10E 109.5 . . ? H10D C103 H10E 109.5 . . ? C6 C5 O1 121.2 . . ? C6 C5 C101 104.7(10) . . ? O1 C5 C101 97.5(9) . . ? C6 C5 C11 114.0(6) . . ? O1 C5 C11 111.4(6) . . ? C101 C5 C11 105.1(12) . . ? C5 C6 C12 127.9(6) . . ? C5 C6 O3 118.3 . . ? C12 C6 O3 106.7(6) . . ? C5 O1 H1 109.5 . . ? O3A C6A C12 149.8(7) . . ? O3A C6A O4A 104.3 . . ? C12 C6A O4A 105.0(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Ru1 N1 C1 175.9(7) . . . . ? N5 Ru1 N1 C1 98.5(7) . . . . ? N2 Ru1 N1 C1 -86.9(7) . . . . ? N10 Ru1 N1 C1 -0.8(7) . . . . ? N4 Ru1 N1 C2 -2.2(8) . . . . ? N5 Ru1 N1 C2 -79.7(8) . . . . ? N2 Ru1 N1 C2 95.0(8) . . . . ? N10 Ru1 N1 C2 -178.9(8) . . . . ? N4 Ru1 N2 C17 -90.6(6) . . . . ? N3 Ru1 N2 C17 -2.8(6) . . . . ? N1 Ru1 N2 C17 170.8(6) . . . . ? N10 Ru1 N2 C17 92.3(6) . . . . ? N4 Ru1 N2 C13 86.6(7) . . . . ? N3 Ru1 N2 C13 174.3(8) . . . . ? N1 Ru1 N2 C13 -12.0(7) . . . . ? N10 Ru1 N2 C13 -90.5(7) . . . . ? N4 Ru1 N3 C22 -79.7(7) . . . . ? N5 Ru1 N3 C22 -2.1(7) . . . . ? N2 Ru1 N3 C22 -176.2(7) . . . . ? N10 Ru1 N3 C22 97.3(7) . . . . ? N4 Ru1 N3 C18 100.5(6) . . . . ? N5 Ru1 N3 C18 178.1(6) . . . . ? N2 Ru1 N3 C18 4.0(5) . . . . ? N10 Ru1 N3 C18 -82.5(6) . . . . ? N3 Ru1 N4 C35 102.4(6) . . . . ? N1 Ru1 N4 C35 -81.8(6) . . . . ? N5 Ru1 N4 C35 4.8(6) . . . . ? N2 Ru1 N4 C35 -179.3(6) . . . . ? N3 Ru1 N4 C31 -76.7(7) . . . . ? N1 Ru1 N4 C31 99.2(7) . . . . ? N5 Ru1 N4 C31 -174.2(7) . . . . ? N2 Ru1 N4 C31 1.7(7) . . . . ? N4 Ru1 N5 C40 177.3(7) . . . . ? N3 Ru1 N5 C40 89.8(7) . . . . ? N1 Ru1 N5 C40 -84.3(7) . . . . ? N10 Ru1 N5 C40 -5.9(7) . . . . ? N4 Ru1 N5 C36 -6.1(5) . . . . ? N3 Ru1 N5 C36 -93.6(6) . . . . ? N1 Ru1 N5 C36 92.2(6) . . . . ? N10 Ru1 N5 C36 170.7(6) . . . . ? N3 Ru1 N10 C10 174.7(7) . . . . ? N1 Ru1 N10 C10 -0.8(7) . . . . ? N5 Ru1 N10 C10 -87.4(7) . . . . ? N2 Ru1 N10 C10 96.4(7) . . . . ? N3 Ru1 N10 C9 -2.0(8) . . . . ? N1 Ru1 N10 C9 -177.4(8) . . . . ? N5 Ru1 N10 C9 96.0(8) . . . . ? N2 Ru1 N10 C9 -80.2(8) . . . . ? C2 N1 C1 C11 -0.1(16) . . . . ? Ru1 N1 C1 C11 -178.4(10) . . . . ? C2 N1 C1 C10 -179.6(9) . . . . ? Ru1 N1 C1 C10 2.1(11) . . . . ? C1 N1 C2 C3 0.2(14) . . . . ? Ru1 N1 C2 C3 178.3(7) . . . . ? N1 C2 C3 C4 1.2(17) . . . . ? N1 C2 C3 Br1 178.2(7) . . . . ? C2 C3 C4 C11 -3(2) . . . . ? Br1 C3 C4 C11 -179.6(11) . . . . ? C12 C7 C8 C9 -6(2) . . . . ? C12 C7 C8 Br2 178.9(12) . . . . ? C10 N10 C9 C8 -3.0(14) . . . . ? Ru1 N10 C9 C8 173.6(8) . . . . ? C7 C8 C9 N10 6.1(17) . . . . ? Br2 C8 C9 N10 -179.0(7) . . . . ? C9 N10 C10 C12 0.3(16) . . . . ? Ru1 N10 C10 C12 -176.7(10) . . . . ? C9 N10 C10 C1 179.1(9) . . . . ? Ru1 N10 C10 C1 2.1(12) . . . . ? N1 C1 C10 N10 -2.8(14) . . . . ? C11 C1 C10 N10 177.7(11) . . . . ? N1 C1 C10 C12 176.0(11) . . . . ? C11 C1 C10 C12 -3.5(19) . . . . ? N1 C1 C11 C4 -1(2) . . . . ? C10 C1 C11 C4 178.2(12) . . . . ? N1 C1 C11 C5A -139.0(15) . . . . ? C10 C1 C11 C5A 40(2) . . . . ? N1 C1 C11 C5 176.6(9) . . . . ? C10 C1 C11 C5 -3.9(18) . . . . ? C3 C4 C11 C1 3(2) . . . . ? C3 C4 C11 C5A 155.7(13) . . . . ? C3 C4 C11 C5 -175.1(12) . . . . ? C8 C7 C12 C10 4(2) . . . . ? C8 C7 C12 C6A 174.5(13) . . . . ? C8 C7 C12 C6 -175.9(13) . . . . ? N10 C10 C12 C7 -1(2) . . . . ? C1 C10 C12 C7 -179.4(13) . . . . ? N10 C10 C12 C6A -163.9(18) . . . . ? C1 C10 C12 C6A 17(3) . . . . ? N10 C10 C12 C6 179.1(10) . . . . ? C1 C10 C12 C6 0.4(18) . . . . ? C17 N2 C13 C14 1.5(13) . . . . ? Ru1 N2 C13 C14 -175.7(7) . . . . ? N2 C13 C14 C15 -0.3(15) . . . . ? C13 C14 C15 C16 -1.5(14) . . . . ? C13 C14 C15 C23 178.1(9) . . . . ? C14 C15 C16 C17 2.1(13) . . . . ? C23 C15 C16 C17 -177.4(9) . . . . ? C13 N2 C17 C16 -0.8(12) . . . . ? Ru1 N2 C17 C16 176.6(6) . . . . ? C13 N2 C17 C18 -176.1(7) . . . . ? Ru1 N2 C17 C18 1.3(9) . . . . ? C15 C16 C17 N2 -1.0(12) . . . . ? C15 C16 C17 C18 173.8(8) . . . . ? C22 N3 C18 C19 -3.1(12) . . . . ? Ru1 N3 C18 C19 176.7(6) . . . . ? C22 N3 C18 C17 175.8(7) . . . . ? Ru1 N3 C18 C17 -4.4(9) . . . . ? N2 C17 C18 N3 2.0(10) . . . . ? C16 C17 C18 N3 -173.1(7) . . . . ? N2 C17 C18 C19 -179.2(8) . . . . ? C16 C17 C18 C19 5.7(13) . . . . ? N3 C18 C19 C20 3.6(13) . . . . ? C17 C18 C19 C20 -175.2(8) . . . . ? C18 C19 C20 C21 -2.8(14) . . . . ? C18 C19 C20 C27 174.9(10) . . . . ? C19 C20 C21 C22 1.8(14) . . . . ? C27 C20 C21 C22 -175.9(10) . . . . ? C18 N3 C22 C21 2.1(12) . . . . ? Ru1 N3 C22 C21 -177.7(7) . . . . ? C20 C21 C22 N3 -1.5(15) . . . . ? C14 C15 C23 C26A 128(3) . . . . ? C16 C15 C23 C26A -53(3) . . . . ? C14 C15 C23 C24 -51.3(16) . . . . ? C16 C15 C23 C24 128.2(13) . . . . ? C14 C15 C23 C25 -178.9(11) . . . . ? C16 C15 C23 C25 0.6(15) . . . . ? C14 C15 C23 C25A -125(3) . . . . ? C16 C15 C23 C25A 54(3) . . . . ? C14 C15 C23 C24A -8(4) . . . . ? C16 C15 C23 C24A 171(4) . . . . ? C14 C15 C23 C26 64.7(13) . . . . ? C16 C15 C23 C26 -115.8(11) . . . . ? C21 C20 C27 C30 -42.5(19) . . . . ? C19 C20 C27 C30 139.9(15) . . . . ? C21 C20 C27 C29 -166.8(11) . . . . ? C19 C20 C27 C29 15.6(17) . . . . ? C21 C20 C27 C28 76.7(13) . . . . ? C19 C20 C27 C28 -100.9(12) . . . . ? C35 N4 C31 C32 -0.6(13) . . . . ? Ru1 N4 C31 C32 178.5(7) . . . . ? N4 C31 C32 C33 1.7(15) . . . . ? C31 C32 C33 C34 -1.1(14) . . . . ? C31 C32 C33 C41 178.6(10) . . . . ? C32 C33 C34 C35 -0.3(14) . . . . ? C41 C33 C34 C35 179.9(9) . . . . ? C31 N4 C35 C34 -1.0(12) . . . . ? Ru1 N4 C35 C34 179.9(6) . . . . ? C31 N4 C35 C36 176.2(7) . . . . ? Ru1 N4 C35 C36 -2.9(9) . . . . ? C33 C34 C35 N4 1.4(13) . . . . ? C33 C34 C35 C36 -175.5(8) . . . . ? C40 N5 C36 C37 1.4(11) . . . . ? Ru1 N5 C36 C37 -175.4(6) . . . . ? C40 N5 C36 C35 -176.8(7) . . . . ? Ru1 N5 C36 C35 6.4(8) . . . . ? N4 C35 C36 N5 -2.3(10) . . . . ? C34 C35 C36 N5 174.8(8) . . . . ? N4 C35 C36 C37 179.6(7) . . . . ? C34 C35 C36 C37 -3.3(13) . . . . ? N5 C36 C37 C38 -0.8(12) . . . . ? C35 C36 C37 C38 177.2(8) . . . . ? C36 C37 C38 C39 -1.0(13) . . . . ? C36 C37 C38 C45 178.9(9) . . . . ? C37 C38 C39 C40 2.2(13) . . . . ? C45 C38 C39 C40 -177.8(9) . . . . ? C36 N5 C40 C39 -0.3(12) . . . . ? Ru1 N5 C40 C39 176.2(6) . . . . ? C38 C39 C40 N5 -1.6(14) . . . . ? C32 C33 C41 C44 118.8(11) . . . . ? C34 C33 C41 C44 -61.5(14) . . . . ? C32 C33 C41 C42 -2.4(18) . . . . ? C34 C33 C41 C42 177.4(12) . . . . ? C32 C33 C41 C43 -124.1(12) . . . . ? C34 C33 C41 C43 55.6(14) . . . . ? C37 C38 C45 C48A -163(3) . . . . ? C39 C38 C45 C48A 17(3) . . . . ? C37 C38 C45 C46 4.8(17) . . . . ? C39 C38 C45 C46 -175.3(12) . . . . ? C37 C38 C45 C47 -119.1(14) . . . . ? C39 C38 C45 C47 60.8(16) . . . . ? C37 C38 C45 C46A 57(2) . . . . ? C39 C38 C45 C46A -124(2) . . . . ? C37 C38 C45 C48 124.7(12) . . . . ? C39 C38 C45 C48 -55.3(14) . . . . ? C37 C38 C45 C47A -54(2) . . . . ? C39 C38 C45 C47A 126(2) . . . . ? C5 C101 C102 O100 28(4) . . . . ? C5 C101 C102 C103 -174.9(19) . . . . ? C102 C101 C5 C6 44(2) . . . . ? C102 C101 C5 O1 168.7(18) . . . . ? C102 C101 C5 C11 -77(2) . . . . ? C1 C11 C5 C6 15.8(14) . . . . ? C4 C11 C5 C6 -166.5(12) . . . . ? C5A C11 C5 C6 -115.9(3) . . . . ? C1 C11 C5 O1 -125.7(10) . . . . ? C4 C11 C5 O1 52.1(15) . . . . ? C5A C11 C5 O1 102.7(3) . . . . ? C1 C11 C5 C101 129.8(15) . . . . ? C4 C11 C5 C101 -52.4(18) . . . . ? C5A C11 C5 C101 -1.8(11) . . . . ? O1 C5 C6 C12 116.1(9) . . . . ? C101 C5 C6 C12 -135.5(14) . . . . ? C11 C5 C6 C12 -21.2(10) . . . . ? O1 C5 C6 O3 -30.1 . . . . ? C101 C5 C6 O3 78.3(10) . . . . ? C11 C5 C6 O3 -167.4(7) . . . . ? C7 C12 C6 C5 -166.1(12) . . . . ? C10 C12 C6 C5 14.2(16) . . . . ? C6A C12 C6 C5 -148.9(3) . . . . ? C7 C12 C6 O3 -16.8(18) . . . . ? C10 C12 C6 O3 163.5(10) . . . . ? C6A C12 C6 O3 0.3(4) . . . . ? C7 C12 C6A O3A -99.7(14) . . . . ? C10 C12 C6A O3A 65(3) . . . . ? C6 C12 C6A O3A 93.7(12) . . . . ? C7 C12 C6A O4A 95.3(10) . . . . ? C10 C12 C6A O4A -100(2) . . . . ? C6 C12 C6A O4A -71.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.601 _refine_diff_density_min -1.229 _refine_diff_density_rms 0.148