# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jing-Lin Zuo' _publ_contact_author_email ZUOJL@NETRA.NJU.EDU.CN _publ_section_title ; Syntheses and Characterization of Neutral Iron(II) and Ruthenium(II) Complexes with Isocyano-triphenylborate Ligand ; loop_ _publ_author_name 'Jing-Lin Zuo.' 'Ling-Chen Kang.' 'Cheng-Hui Li.' 'Hong-Ping Xiao.' ; Xiao-Zeng You ; 'Yan Zhou.' # Attachment 'all-5-new.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 739893' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H53 B2 N7 Ru' _chemical_formula_weight 994.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.506(10) _cell_length_b 16.701(9) _cell_length_c 17.705(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.943(11) _cell_angle_gamma 90.00 _cell_volume 5206(5) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 926 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 23.95 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 0.347 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9152 _exptl_absorpt_correction_T_max 0.9498 _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart apex II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27498 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10202 _reflns_number_gt 7371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Bruker, 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.5500P] 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 10202 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.2751(2) 0.2327(2) 0.0105(2) 0.0446(9) Uani 1 1 d . . . B2 B 0.2466(2) -0.2208(2) 0.3133(2) 0.0418(9) Uani 1 1 d . . . C1 C 0.26722(19) 0.2064(2) -0.0800(2) 0.0421(8) Uani 1 1 d . . . C2 C 0.2074(2) 0.1581(2) -0.1214(2) 0.0507(9) Uani 1 1 d . . . H2 H 0.1743 0.1386 -0.0955 0.061 Uiso 1 1 calc R . . C3 C 0.1951(2) 0.1377(2) -0.2004(2) 0.0498(9) Uani 1 1 d . . . H3 H 0.1536 0.1061 -0.2266 0.060 Uiso 1 1 calc R . . C4 C 0.24315(19) 0.1635(2) -0.2398(2) 0.0446(8) Uani 1 1 d . . . H4 H 0.2351 0.1488 -0.2924 0.053 Uiso 1 1 calc R . . C5 C 0.3025(2) 0.2104(2) -0.2021(2) 0.0467(9) Uani 1 1 d . . . H5 H 0.3361 0.2281 -0.2283 0.056 Uiso 1 1 calc R . . C6 C 0.3130(2) 0.2320(2) -0.1233(2) 0.0480(9) Uani 1 1 d . . . H6 H 0.3533 0.2658 -0.0987 0.058 Uiso 1 1 calc R . . C7 C 0.3550(2) 0.2767(2) 0.0541(2) 0.0489(9) Uani 1 1 d . . . C8 C 0.4237(2) 0.2365(2) 0.0613(2) 0.0488(9) Uani 1 1 d . . . H8 H 0.4217 0.1835 0.0448 0.059 Uiso 1 1 calc R . . C9 C 0.4932(2) 0.2720(2) 0.0915(2) 0.0495(9) Uani 1 1 d . . . H9 H 0.5370 0.2427 0.0958 0.059 Uiso 1 1 calc R . . C10 C 0.4986(2) 0.3481(2) 0.1147(2) 0.0482(9) Uani 1 1 d . . . H10 H 0.5462 0.3721 0.1333 0.058 Uiso 1 1 calc R . . C11 C 0.4343(2) 0.3919(2) 0.1114(2) 0.0481(9) Uani 1 1 d . . . H11 H 0.4383 0.4446 0.1290 0.058 Uiso 1 1 calc R . . C12 C 0.36288(19) 0.3552(2) 0.0809(2) 0.0462(9) Uani 1 1 d . . . H12 H 0.3195 0.3846 0.0786 0.055 Uiso 1 1 calc R . . C13 C 0.2018(2) 0.2832(2) 0.0121(2) 0.0459(8) Uani 1 1 d . . . C14 C 0.1805(2) 0.3515(2) -0.0335(2) 0.0468(9) Uani 1 1 d . . . H14 H 0.2104 0.3677 -0.0644 0.056 Uiso 1 1 calc R . . C15 C 0.1180(2) 0.3969(2) -0.0362(2) 0.0495(9) Uani 1 1 d . . . H15 H 0.1062 0.4418 -0.0689 0.059 Uiso 1 1 calc R . . C16 C 0.0732(2) 0.3763(2) 0.0089(2) 0.0512(9) Uani 1 1 d . . . H16 H 0.0314 0.4076 0.0083 0.061 Uiso 1 1 calc R . . C17 C 0.0906(2) 0.3084(2) 0.0556(2) 0.0470(9) Uani 1 1 d . . . H17 H 0.0600 0.2929 0.0861 0.056 Uiso 1 1 calc R . . C18 C 0.15404(18) 0.2635(2) 0.0566(2) 0.0423(8) Uani 1 1 d . . . H18 H 0.1652 0.2181 0.0886 0.051 Uiso 1 1 calc R . . C19 C 0.36409(19) 0.0341(2) 0.3331(2) 0.0434(8) Uani 1 1 d . . . H19 H 0.3270 0.0005 0.3410 0.052 Uiso 1 1 calc R . . C20 C 0.41572(19) 0.0676(2) 0.3976(2) 0.0476(9) Uani 1 1 d . . . H20 H 0.4136 0.0559 0.4483 0.057 Uiso 1 1 calc R . . C21 C 0.4703(2) 0.1178(2) 0.3886(2) 0.0491(9) Uani 1 1 d . . . H21 H 0.5063 0.1402 0.4323 0.059 Uiso 1 1 calc R . . C22 C 0.4704(2) 0.1343(2) 0.3128(2) 0.0452(8) Uani 1 1 d . . . H22 H 0.5060 0.1696 0.3042 0.054 Uiso 1 1 calc R . . C23 C 0.41834(19) 0.0991(2) 0.2502(2) 0.0469(8) Uani 1 1 d . . . H23 H 0.4196 0.1109 0.1993 0.056 Uiso 1 1 calc R . . C24 C 0.19478(19) 0.1138(2) 0.2244(2) 0.0419(8) Uani 1 1 d . . . H24 H 0.2342 0.1477 0.2228 0.050 Uiso 1 1 calc R . . C25 C 0.13858(19) 0.1444(2) 0.2512(2) 0.0482(9) Uani 1 1 d . . . H25 H 0.1403 0.1974 0.2677 0.058 Uiso 1 1 calc R . . C26 C 0.07992(19) 0.0956(2) 0.2535(2) 0.0441(8) Uani 1 1 d . . . H26 H 0.0409 0.1148 0.2713 0.053 Uiso 1 1 calc R . . C27 C 0.0799(2) 0.0174(2) 0.2287(2) 0.0449(8) Uani 1 1 d . . . H27 H 0.0406 -0.0169 0.2295 0.054 Uiso 1 1 calc R . . C28 C 0.13807(19) -0.0095(2) 0.2029(2) 0.0439(8) Uani 1 1 d . . . H28 H 0.1375 -0.0625 0.1866 0.053 Uiso 1 1 calc R . . C29 C 0.37626(19) -0.0449(2) 0.0488(2) 0.0440(8) Uani 1 1 d . . . H29 H 0.3368 -0.0186 0.0114 0.053 Uiso 1 1 calc R . . C30 C 0.43240(19) -0.0883(2) 0.1742(2) 0.0426(8) Uani 1 1 d . . . H30 H 0.4326 -0.0931 0.2266 0.051 Uiso 1 1 calc R . . C31 C 0.49201(18) -0.12013(19) 0.1545(2) 0.0400(8) Uani 1 1 d . . . H31 H 0.5308 -0.1462 0.1928 0.048 Uiso 1 1 calc R . . C32 C 0.4946(2) -0.1137(2) 0.0794(2) 0.0441(8) Uani 1 1 d . . . H32 H 0.5353 -0.1340 0.0651 0.053 Uiso 1 1 calc R . . C33 C 0.43459(19) -0.0761(2) 0.0247(2) 0.0457(8) Uani 1 1 d . . . H33 H 0.4335 -0.0717 -0.0280 0.055 Uiso 1 1 calc R . . C34 C 0.14384(19) -0.0143(2) 0.0195(2) 0.0478(8) Uani 1 1 d . . . H34 H 0.1404 0.0395 0.0317 0.057 Uiso 1 1 calc R . . C35 C 0.0878(2) -0.0476(2) -0.0434(2) 0.0539(10) Uani 1 1 d . . . H35 H 0.0489 -0.0156 -0.0746 0.065 Uiso 1 1 calc R . . C36 C 0.08965(19) -0.1272(2) -0.0597(2) 0.0468(9) Uani 1 1 d . . . H36 H 0.0513 -0.1509 -0.1005 0.056 Uiso 1 1 calc R . . C37 C 0.14871(19) -0.1704(2) -0.0149(2) 0.0462(8) Uani 1 1 d . . . H37 H 0.1525 -0.2246 -0.0248 0.055 Uiso 1 1 calc R . . C38 C 0.20333(19) -0.1334(2) 0.0457(2) 0.0433(8) Uani 1 1 d . . . H38 H 0.2434 -0.1645 0.0762 0.052 Uiso 1 1 calc R . . C39 C 0.28057(19) 0.0954(2) 0.0963(2) 0.0404(7) Uani 1 1 d . . . C40 C 0.28429(17) -0.10509(18) 0.22424(19) 0.0340(7) Uani 1 1 d . . . C41 C 0.27177(19) -0.1845(2) 0.4029(2) 0.0454(8) Uani 1 1 d . . . C42 C 0.25142(19) -0.1070(2) 0.4158(2) 0.0439(8) Uani 1 1 d . . . H42 H 0.2227 -0.0770 0.3727 0.053 Uiso 1 1 calc R . . C43 C 0.27247(19) -0.0723(2) 0.4910(2) 0.0440(8) Uani 1 1 d . . . H43 H 0.2595 -0.0196 0.4978 0.053 Uiso 1 1 calc R . . C44 C 0.31365(18) -0.1184(2) 0.5565(2) 0.0437(8) Uani 1 1 d . . . H44 H 0.3278 -0.0970 0.6074 0.052 Uiso 1 1 calc R . . C45 C 0.33240(19) -0.1945(2) 0.5441(2) 0.0454(8) Uani 1 1 d . . . H45 H 0.3582 -0.2262 0.5872 0.055 Uiso 1 1 calc R . . C46 C 0.3137(2) -0.2255(2) 0.4683(2) 0.0505(9) Uani 1 1 d . . . H46 H 0.3304 -0.2768 0.4615 0.061 Uiso 1 1 calc R . . C47 C 0.15490(19) -0.2206(2) 0.2687(2) 0.0442(8) Uani 1 1 d . . . C48 C 0.12797(18) -0.2417(2) 0.1877(2) 0.0421(8) Uani 1 1 d . . . H48 H 0.1628 -0.2560 0.1618 0.051 Uiso 1 1 calc R . . C49 C 0.0523(2) -0.2418(2) 0.1460(2) 0.0508(9) Uani 1 1 d . . . H49 H 0.0365 -0.2569 0.0929 0.061 Uiso 1 1 calc R . . C50 C -0.0002(2) -0.2201(2) 0.1818(2) 0.0508(9) Uani 1 1 d . . . H50 H -0.0515 -0.2189 0.1530 0.061 Uiso 1 1 calc R . . C51 C 0.02339(19) -0.1999(2) 0.2602(2) 0.0430(8) Uani 1 1 d . . . H51 H -0.0123 -0.1863 0.2853 0.052 Uiso 1 1 calc R . . C52 C 0.09991(18) -0.19954(19) 0.3030(2) 0.0430(8) Uani 1 1 d . . . H52 H 0.1147 -0.1847 0.3562 0.052 Uiso 1 1 calc R . . C53 C 0.2818(2) -0.3086(2) 0.3078(2) 0.0484(9) Uani 1 1 d . . . C54 C 0.3423(2) -0.3244(2) 0.2807(2) 0.0463(8) Uani 1 1 d . . . H54 H 0.3653 -0.2828 0.2617 0.056 Uiso 1 1 calc R . . C55 C 0.3701(2) -0.4033(2) 0.2814(2) 0.0456(8) Uani 1 1 d . . . H55 H 0.4109 -0.4129 0.2625 0.055 Uiso 1 1 calc R . . C56 C 0.33861(19) -0.4646(2) 0.3089(2) 0.0476(9) Uani 1 1 d . . . H56 H 0.3575 -0.5163 0.3096 0.057 Uiso 1 1 calc R . . C57 C 0.2792(2) -0.4497(2) 0.3355(2) 0.0476(9) Uani 1 1 d . . . H57 H 0.2569 -0.4917 0.3549 0.057 Uiso 1 1 calc R . . C58 C 0.2510(2) -0.3743(2) 0.3345(2) 0.0438(8) Uani 1 1 d . . . H58 H 0.2094 -0.3665 0.3525 0.053 Uiso 1 1 calc R . . C59 C 0.1594(2) 0.5513(2) 0.1269(2) 0.0473(9) Uani 1 1 d . . . H59A H 0.1974 0.5803 0.1667 0.071 Uiso 1 1 calc R . . H59B H 0.1395 0.5845 0.0809 0.071 Uiso 1 1 calc R . . H59C H 0.1817 0.5041 0.1124 0.071 Uiso 1 1 calc R . . C60 C 0.0973(2) 0.5280(2) 0.1585(2) 0.0457(8) Uani 1 1 d . . . N1 N 0.27710(16) 0.15307(17) 0.05934(18) 0.0453(7) Uani 1 1 d . . . N2 N 0.27730(15) -0.15902(17) 0.26167(17) 0.0415(6) Uani 1 1 d . . . N3 N 0.36476(15) 0.04773(16) 0.25839(17) 0.0403(6) Uani 1 1 d . . . N4 N 0.19646(15) 0.03809(16) 0.20029(16) 0.0392(6) Uani 1 1 d . . . N5 N 0.37374(15) -0.05065(16) 0.12327(16) 0.0387(6) Uani 1 1 d . . . N6 N 0.20288(16) -0.05744(17) 0.06333(17) 0.0450(7) Uani 1 1 d . . . N7 N 0.05638(17) 0.51067(17) 0.18758(18) 0.0470(7) Uani 1 1 d . . . Ru1 Ru 0.284905(14) -0.005339(15) 0.160521(15) 0.03494(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.048(2) 0.044(2) 0.040(2) 0.0149(17) 0.0104(18) 0.0036(17) B2 0.045(2) 0.0351(19) 0.042(2) 0.0070(16) 0.0084(17) -0.0030(16) C1 0.0418(18) 0.0388(18) 0.0405(19) 0.0088(14) 0.0051(15) 0.0065(14) C2 0.052(2) 0.050(2) 0.045(2) -0.0044(16) 0.0077(17) 0.0042(17) C3 0.0407(19) 0.059(2) 0.039(2) -0.0054(17) -0.0030(16) 0.0103(16) C4 0.0415(18) 0.0415(19) 0.046(2) -0.0061(15) 0.0070(16) 0.0163(15) C5 0.050(2) 0.0448(19) 0.045(2) 0.0156(16) 0.0143(17) 0.0145(16) C6 0.0415(19) 0.055(2) 0.047(2) 0.0135(17) 0.0128(16) 0.0111(16) C7 0.049(2) 0.058(2) 0.0354(19) 0.0119(16) 0.0070(16) -0.0073(17) C8 0.054(2) 0.043(2) 0.048(2) 0.0043(16) 0.0133(17) -0.0014(16) C9 0.050(2) 0.048(2) 0.046(2) 0.0028(16) 0.0087(17) -0.0131(16) C10 0.0433(19) 0.047(2) 0.042(2) -0.0055(16) -0.0048(16) -0.0187(16) C11 0.050(2) 0.050(2) 0.038(2) -0.0148(16) 0.0044(16) -0.0135(17) C12 0.0392(18) 0.0469(19) 0.042(2) 0.0092(15) -0.0036(15) -0.0149(15) C13 0.0452(19) 0.0441(19) 0.043(2) 0.0014(15) 0.0062(16) -0.0003(15) C14 0.0429(19) 0.0405(19) 0.050(2) 0.0050(16) 0.0035(16) 0.0097(15) C15 0.046(2) 0.046(2) 0.045(2) -0.0087(16) -0.0022(17) 0.0105(16) C16 0.044(2) 0.051(2) 0.047(2) -0.0115(17) -0.0031(17) 0.0110(16) C17 0.047(2) 0.050(2) 0.043(2) -0.0147(16) 0.0129(16) 0.0140(16) C18 0.0384(17) 0.0476(19) 0.0411(19) 0.0002(15) 0.0124(15) 0.0108(14) C19 0.0368(18) 0.0487(19) 0.044(2) -0.0028(16) 0.0119(15) 0.0038(15) C20 0.0400(19) 0.0448(19) 0.050(2) -0.0151(16) 0.0026(16) 0.0075(15) C21 0.045(2) 0.050(2) 0.047(2) -0.0186(17) 0.0085(16) -0.0010(16) C22 0.0465(19) 0.0453(19) 0.047(2) -0.0136(16) 0.0186(16) -0.0129(15) C23 0.049(2) 0.048(2) 0.043(2) -0.0102(16) 0.0143(16) -0.0075(16) C24 0.0449(19) 0.0423(19) 0.041(2) -0.0027(15) 0.0167(15) -0.0079(15) C25 0.0455(19) 0.051(2) 0.046(2) -0.0112(17) 0.0111(16) 0.0015(16) C26 0.0444(19) 0.0418(18) 0.047(2) -0.0020(15) 0.0156(16) 0.0090(15) C27 0.0450(19) 0.0392(18) 0.048(2) 0.0025(15) 0.0116(16) -0.0002(14) C28 0.0481(19) 0.0427(19) 0.0381(18) 0.0041(15) 0.0092(15) -0.0041(15) C29 0.0393(18) 0.050(2) 0.043(2) -0.0016(16) 0.0127(16) -0.0103(15) C30 0.0478(19) 0.0429(19) 0.0396(19) -0.0007(15) 0.0170(16) 0.0081(15) C31 0.0413(18) 0.0407(18) 0.0393(19) -0.0058(14) 0.0143(15) 0.0132(14) C32 0.0470(19) 0.0425(19) 0.045(2) -0.0116(15) 0.0168(16) 0.0064(15) C33 0.0435(19) 0.054(2) 0.0400(19) -0.0180(16) 0.0135(16) -0.0157(16) C34 0.0434(19) 0.048(2) 0.044(2) -0.0004(16) 0.0022(15) -0.0010(15) C35 0.045(2) 0.053(2) 0.046(2) 0.0001(17) -0.0119(17) 0.0019(17) C36 0.0437(19) 0.047(2) 0.039(2) -0.0169(15) -0.0034(15) -0.0181(15) C37 0.0461(19) 0.0463(19) 0.047(2) -0.0153(16) 0.0146(16) -0.0140(16) C38 0.0467(19) 0.0413(19) 0.041(2) -0.0129(15) 0.0123(16) -0.0079(15) C39 0.0450(19) 0.0427(18) 0.0345(18) 0.0066(15) 0.0138(15) -0.0019(15) C40 0.0351(16) 0.0354(16) 0.0315(17) 0.0046(13) 0.0102(13) -0.0001(13) C41 0.0447(19) 0.0430(19) 0.052(2) 0.0040(16) 0.0195(17) -0.0045(15) C42 0.0473(19) 0.0422(19) 0.041(2) 0.0023(15) 0.0123(16) 0.0079(15) C43 0.0440(19) 0.0431(19) 0.044(2) -0.0085(15) 0.0120(16) 0.0010(15) C44 0.0397(18) 0.047(2) 0.042(2) -0.0167(15) 0.0095(15) -0.0093(15) C45 0.045(2) 0.0398(18) 0.041(2) -0.0003(15) -0.0025(16) -0.0031(15) C46 0.046(2) 0.056(2) 0.045(2) 0.0019(17) 0.0076(17) -0.0053(16) C47 0.0466(19) 0.0455(19) 0.0394(19) 0.0110(15) 0.0116(16) -0.0109(15) C48 0.0400(18) 0.0444(19) 0.0372(18) -0.0060(14) 0.0048(15) -0.0122(15) C49 0.0430(19) 0.045(2) 0.051(2) -0.0025(16) -0.0050(17) -0.0170(16) C50 0.049(2) 0.050(2) 0.043(2) 0.0163(16) -0.0004(17) -0.0173(17) C51 0.0433(19) 0.0444(19) 0.042(2) 0.0165(15) 0.0133(15) -0.0043(15) C52 0.0430(19) 0.0383(18) 0.046(2) 0.0153(15) 0.0109(16) 0.0027(14) C53 0.050(2) 0.0428(19) 0.049(2) 0.0027(16) 0.0096(17) -0.0037(16) C54 0.048(2) 0.0430(19) 0.047(2) 0.0049(15) 0.0131(17) 0.0047(15) C55 0.0440(19) 0.047(2) 0.045(2) -0.0055(16) 0.0131(16) 0.0122(16) C56 0.0426(19) 0.050(2) 0.043(2) -0.0034(16) 0.0034(16) 0.0135(16) C57 0.048(2) 0.044(2) 0.051(2) -0.0007(16) 0.0148(17) -0.0087(16) C58 0.0429(19) 0.0438(19) 0.046(2) -0.0006(15) 0.0161(16) -0.0061(15) C59 0.051(2) 0.044(2) 0.047(2) -0.0124(16) 0.0149(17) -0.0150(16) C60 0.047(2) 0.0442(19) 0.049(2) 0.0111(16) 0.0192(18) 0.0130(15) N1 0.0460(16) 0.0431(16) 0.0444(17) 0.0092(14) 0.0102(13) 0.0001(13) N2 0.0398(15) 0.0439(16) 0.0382(16) 0.0018(13) 0.0083(12) -0.0058(12) N3 0.0371(15) 0.0414(15) 0.0401(16) -0.0016(12) 0.0085(12) -0.0002(12) N4 0.0367(14) 0.0362(14) 0.0413(16) 0.0002(12) 0.0071(12) 0.0007(12) N5 0.0420(15) 0.0414(15) 0.0357(15) -0.0073(12) 0.0165(12) -0.0052(12) N6 0.0415(16) 0.0514(17) 0.0374(16) -0.0079(13) 0.0053(13) -0.0061(13) N7 0.0496(17) 0.0473(17) 0.0469(17) 0.0127(14) 0.0189(14) 0.0222(14) Ru1 0.03610(14) 0.03237(14) 0.03460(14) 0.00328(11) 0.00832(10) -0.00327(11) _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 B1 N1 1.581(5) . ? B1 C13 1.605(5) . ? B1 C7 1.617(5) . ? B1 C1 1.624(6) . ? B2 N2 1.594(5) . ? B2 C53 1.619(5) . ? B2 C41 1.627(6) . ? B2 C47 1.636(5) . ? C1 C6 1.375(5) . ? C1 C2 1.384(5) . ? C2 C3 1.389(5) . ? C2 H2 0.9300 . ? C3 C4 1.358(5) . ? C3 H3 0.9300 . ? C4 C5 1.347(5) . ? C4 H4 0.9300 . ? C5 C6 1.396(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.387(5) . ? C7 C8 1.409(5) . ? C8 C9 1.366(5) . ? C8 H8 0.9300 . ? C9 C10 1.331(5) . ? C9 H9 0.9300 . ? C10 C11 1.382(5) . ? C10 H10 0.9300 . ? C11 C12 1.405(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.383(5) . ? C13 C18 1.394(5) . ? C14 C15 1.372(5) . ? C14 H14 0.9300 . ? C15 C16 1.360(6) . ? C15 H15 0.9300 . ? C16 C17 1.383(5) . ? C16 H16 0.9300 . ? C17 C18 1.389(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 N3 1.346(4) . ? C19 C20 1.363(5) . ? C19 H19 0.9300 . ? C20 C21 1.360(5) . ? C20 H20 0.9300 . ? C21 C22 1.371(5) . ? C21 H21 0.9300 . ? C22 C23 1.357(5) . ? C22 H22 0.9300 . ? C23 N3 1.352(4) . ? C23 H23 0.9300 . ? C24 N4 1.338(4) . ? C24 C25 1.368(5) . ? C24 H24 0.9300 . ? C25 C26 1.367(5) . ? C25 H25 0.9300 . ? C26 C27 1.378(5) . ? C26 H26 0.9300 . ? C27 C28 1.368(5) . ? C27 H27 0.9300 . ? C28 N4 1.354(4) . ? C28 H28 0.9300 . ? C29 N5 1.337(4) . ? C29 C33 1.379(5) . ? C29 H29 0.9300 . ? C30 N5 1.336(4) . ? C30 C31 1.363(4) . ? C30 H30 0.9300 . ? C31 C32 1.349(5) . ? C31 H31 0.9300 . ? C32 C33 1.380(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 N6 1.339(4) . ? C34 C35 1.383(5) . ? C34 H34 0.9300 . ? C35 C36 1.363(5) . ? C35 H35 0.9300 . ? C36 C37 1.345(5) . ? C36 H36 0.9300 . ? C37 C38 1.373(4) . ? C37 H37 0.9300 . ? C38 N6 1.307(4) . ? C38 H38 0.9300 . ? C39 N1 1.155(4) . ? C39 Ru1 2.019(3) . ? C40 N2 1.149(4) . ? C40 Ru1 2.014(3) . ? C41 C46 1.364(5) . ? C41 C42 1.387(5) . ? C42 C43 1.393(5) . ? C42 H42 0.9300 . ? C43 C44 1.404(5) . ? C43 H43 0.9300 . ? C44 C45 1.353(5) . ? C44 H44 0.9300 . ? C45 C46 1.380(5) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C52 1.382(5) . ? C47 C48 1.409(5) . ? C48 C49 1.368(4) . ? C48 H48 0.9300 . ? C49 C50 1.361(6) . ? C49 H49 0.9300 . ? C50 C51 1.364(5) . ? C50 H50 0.9300 . ? C51 C52 1.385(5) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.373(5) . ? C53 C58 1.385(5) . ? C54 C55 1.413(5) . ? C54 H54 0.9300 . ? C55 C56 1.341(5) . ? C55 H55 0.9300 . ? C56 C57 1.346(5) . ? C56 H56 0.9300 . ? C57 C58 1.361(5) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? C59 C60 1.478(5) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 N7 1.078(4) . ? N3 Ru1 2.096(3) . ? N4 Ru1 2.100(3) . ? N5 Ru1 2.092(3) . ? N6 Ru1 2.101(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 N1 B1 C13 108.1(3) . . ? N1 B1 C7 104.9(3) . . ? C13 B1 C7 113.9(3) . . ? N1 B1 C1 106.9(3) . . ? C13 B1 C1 109.9(3) . . ? C7 B1 C1 112.7(3) . . ? N2 B2 C53 109.3(3) . . ? N2 B2 C41 105.8(3) . . ? C53 B2 C41 113.3(3) . . ? N2 B2 C47 102.8(3) . . ? C53 B2 C47 110.5(3) . . ? C41 B2 C47 114.4(3) . . ? C6 C1 C2 114.6(4) . . ? C6 C1 B1 125.6(3) . . ? C2 C1 B1 119.7(3) . . ? C1 C2 C3 122.2(4) . . ? C1 C2 H2 118.9 . . ? C3 C2 H2 118.9 . . ? C4 C3 C2 120.7(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 119.6(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 119.1(4) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C1 C6 C5 123.9(4) . . ? C1 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? C12 C7 C8 114.9(3) . . ? C12 C7 B1 125.3(3) . . ? C8 C7 B1 119.6(3) . . ? C9 C8 C7 123.0(4) . . ? C9 C8 H8 118.5 . . ? C7 C8 H8 118.5 . . ? C10 C9 C8 120.5(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.7(3) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C12 118.8(3) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C7 C12 C11 122.1(4) . . ? C7 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C14 C13 C18 114.1(3) . . ? C14 C13 B1 120.9(3) . . ? C18 C13 B1 124.9(3) . . ? C15 C14 C13 124.2(4) . . ? C15 C14 H14 117.9 . . ? C13 C14 H14 117.9 . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 119.2(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C18 119.3(4) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C17 C18 C13 123.2(3) . . ? C17 C18 H18 118.4 . . ? C13 C18 H18 118.4 . . ? N3 C19 C20 122.6(3) . . ? N3 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C21 C20 C19 120.6(4) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 117.7(3) . . ? C20 C21 H21 121.2 . . ? C22 C21 H21 121.2 . . ? C23 C22 C21 119.8(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? N3 C23 C22 123.2(3) . . ? N3 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? N4 C24 C25 123.9(3) . . ? N4 C24 H24 118.0 . . ? C25 C24 H24 118.0 . . ? C26 C25 C24 118.9(3) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C25 C26 C27 118.5(3) . . ? C25 C26 H26 120.8 . . ? C27 C26 H26 120.8 . . ? C28 C27 C26 119.7(3) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? N4 C28 C27 122.4(3) . . ? N4 C28 H28 118.8 . . ? C27 C28 H28 118.8 . . ? N5 C29 C33 123.1(3) . . ? N5 C29 H29 118.5 . . ? C33 C29 H29 118.5 . . ? N5 C30 C31 124.3(3) . . ? N5 C30 H30 117.8 . . ? C31 C30 H30 117.8 . . ? C32 C31 C30 119.9(3) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 117.6(3) . . ? C31 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? C29 C33 C32 119.5(3) . . ? C29 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? N6 C34 C35 121.7(3) . . ? N6 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C36 C35 C34 120.1(3) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 117.8(3) . . ? C37 C36 H36 121.1 . . ? C35 C36 H36 121.1 . . ? C36 C37 C38 119.2(3) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? N6 C38 C37 124.5(4) . . ? N6 C38 H38 117.8 . . ? C37 C38 H38 117.8 . . ? N1 C39 Ru1 179.1(3) . . ? N2 C40 Ru1 173.1(3) . . ? C46 C41 C42 116.2(4) . . ? C46 C41 B2 123.9(3) . . ? C42 C41 B2 119.9(3) . . ? C41 C42 C43 122.4(3) . . ? C41 C42 H42 118.8 . . ? C43 C42 H42 118.8 . . ? C42 C43 C44 118.8(3) . . ? C42 C43 H43 120.6 . . ? C44 C43 H43 120.6 . . ? C45 C44 C43 118.8(3) . . ? C45 C44 H44 120.6 . . ? C43 C44 H44 120.6 . . ? C44 C45 C46 120.7(3) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C41 C46 C45 122.9(4) . . ? C41 C46 H46 118.5 . . ? C45 C46 H46 118.5 . . ? C52 C47 C48 115.7(3) . . ? C52 C47 B2 125.7(3) . . ? C48 C47 B2 118.6(3) . . ? C49 C48 C47 122.1(4) . . ? C49 C48 H48 118.9 . . ? C47 C48 H48 118.9 . . ? C50 C49 C48 120.5(4) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 C51 119.3(3) . . ? C49 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C50 C51 C52 120.7(4) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C47 C52 C51 121.7(4) . . ? C47 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? C54 C53 C58 115.6(3) . . ? C54 C53 B2 125.6(3) . . ? C58 C53 B2 118.8(3) . . ? C53 C54 C55 120.7(3) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C56 C55 C54 121.1(3) . . ? C56 C55 H55 119.4 . . ? C54 C55 H55 119.4 . . ? C55 C56 C57 118.7(3) . . ? C55 C56 H56 120.7 . . ? C57 C56 H56 120.7 . . ? C56 C57 C58 121.1(4) . . ? C56 C57 H57 119.5 . . ? C58 C57 H57 119.5 . . ? C57 C58 C53 122.8(3) . . ? C57 C58 H58 118.6 . . ? C53 C58 H58 118.6 . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N7 C60 C59 174.0(4) . . ? C39 N1 B1 178.1(4) . . ? C40 N2 B2 164.0(3) . . ? C19 N3 C23 116.2(3) . . ? C19 N3 Ru1 121.5(2) . . ? C23 N3 Ru1 122.2(2) . . ? C24 N4 C28 116.6(3) . . ? C24 N4 Ru1 122.0(2) . . ? C28 N4 Ru1 121.4(2) . . ? C30 N5 C29 115.6(3) . . ? C30 N5 Ru1 120.7(2) . . ? C29 N5 Ru1 123.7(2) . . ? C38 N6 C34 116.6(3) . . ? C38 N6 Ru1 122.8(2) . . ? C34 N6 Ru1 120.4(2) . . ? C40 Ru1 C39 177.42(13) . . ? C40 Ru1 N5 91.03(12) . . ? C39 Ru1 N5 91.31(13) . . ? C40 Ru1 N3 90.62(12) . . ? C39 Ru1 N3 90.49(13) . . ? N5 Ru1 N3 89.49(11) . . ? C40 Ru1 N4 87.62(12) . . ? C39 Ru1 N4 90.05(12) . . ? N5 Ru1 N4 178.56(11) . . ? N3 Ru1 N4 90.04(11) . . ? C40 Ru1 N6 89.36(12) . . ? C39 Ru1 N6 89.47(13) . . ? N5 Ru1 N6 91.81(11) . . ? N3 Ru1 N6 178.69(11) . . ? N4 Ru1 N6 88.65(11) . . ? 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 N1 B1 C1 C6 -128.5(3) . . . . ? C13 B1 C1 C6 114.5(4) . . . . ? C7 B1 C1 C6 -13.7(5) . . . . ? N1 B1 C1 C2 56.0(4) . . . . ? C13 B1 C1 C2 -61.0(4) . . . . ? C7 B1 C1 C2 170.7(3) . . . . ? C6 C1 C2 C3 0.0(5) . . . . ? B1 C1 C2 C3 176.0(3) . . . . ? C1 C2 C3 C4 1.4(5) . . . . ? C2 C3 C4 C5 -1.1(5) . . . . ? C3 C4 C5 C6 -0.5(5) . . . . ? C2 C1 C6 C5 -1.7(5) . . . . ? B1 C1 C6 C5 -177.4(3) . . . . ? C4 C5 C6 C1 2.0(5) . . . . ? N1 B1 C7 C12 -127.3(4) . . . . ? C13 B1 C7 C12 -9.3(5) . . . . ? C1 B1 C7 C12 116.7(4) . . . . ? N1 B1 C7 C8 58.0(4) . . . . ? C13 B1 C7 C8 176.0(3) . . . . ? C1 B1 C7 C8 -57.9(4) . . . . ? C12 C7 C8 C9 -0.7(5) . . . . ? B1 C7 C8 C9 174.5(3) . . . . ? C7 C8 C9 C10 -1.0(6) . . . . ? C8 C9 C10 C11 2.3(6) . . . . ? C9 C10 C11 C12 -1.8(6) . . . . ? C8 C7 C12 C11 1.1(5) . . . . ? B1 C7 C12 C11 -173.7(3) . . . . ? C10 C11 C12 C7 0.0(6) . . . . ? N1 B1 C13 C14 -172.4(3) . . . . ? C7 B1 C13 C14 71.4(4) . . . . ? C1 B1 C13 C14 -56.1(4) . . . . ? N1 B1 C13 C18 6.6(5) . . . . ? C7 B1 C13 C18 -109.5(4) . . . . ? C1 B1 C13 C18 123.0(4) . . . . ? C18 C13 C14 C15 -0.3(5) . . . . ? B1 C13 C14 C15 178.9(3) . . . . ? C13 C14 C15 C16 1.1(6) . . . . ? C14 C15 C16 C17 -1.5(5) . . . . ? C15 C16 C17 C18 1.2(5) . . . . ? C16 C17 C18 C13 -0.3(5) . . . . ? C14 C13 C18 C17 -0.1(5) . . . . ? B1 C13 C18 C17 -179.2(3) . . . . ? N3 C19 C20 C21 0.9(5) . . . . ? C19 C20 C21 C22 1.1(5) . . . . ? C20 C21 C22 C23 -1.7(5) . . . . ? C21 C22 C23 N3 0.4(6) . . . . ? N4 C24 C25 C26 -0.5(6) . . . . ? C24 C25 C26 C27 0.2(5) . . . . ? C25 C26 C27 C28 0.2(5) . . . . ? C26 C27 C28 N4 -0.3(5) . . . . ? N5 C30 C31 C32 0.8(5) . . . . ? C30 C31 C32 C33 -1.5(5) . . . . ? N5 C29 C33 C32 -1.4(5) . . . . ? C31 C32 C33 C29 1.8(5) . . . . ? N6 C34 C35 C36 3.4(6) . . . . ? C34 C35 C36 C37 -2.6(6) . . . . ? C35 C36 C37 C38 1.2(6) . . . . ? C36 C37 C38 N6 -0.6(6) . . . . ? N2 B2 C41 C46 -124.3(3) . . . . ? C53 B2 C41 C46 -4.6(5) . . . . ? C47 B2 C41 C46 123.2(4) . . . . ? N2 B2 C41 C42 54.7(4) . . . . ? C53 B2 C41 C42 174.4(3) . . . . ? C47 B2 C41 C42 -57.7(4) . . . . ? C46 C41 C42 C43 0.2(5) . . . . ? B2 C41 C42 C43 -178.9(3) . . . . ? C41 C42 C43 C44 -2.1(5) . . . . ? C42 C43 C44 C45 0.9(5) . . . . ? C43 C44 C45 C46 2.2(5) . . . . ? C42 C41 C46 C45 3.0(5) . . . . ? B2 C41 C46 C45 -177.9(3) . . . . ? C44 C45 C46 C41 -4.3(6) . . . . ? N2 B2 C47 C52 -120.2(3) . . . . ? C53 B2 C47 C52 123.3(4) . . . . ? C41 B2 C47 C52 -6.0(5) . . . . ? N2 B2 C47 C48 58.2(4) . . . . ? C53 B2 C47 C48 -58.3(4) . . . . ? C41 B2 C47 C48 172.4(3) . . . . ? C52 C47 C48 C49 -0.5(5) . . . . ? B2 C47 C48 C49 -179.0(3) . . . . ? C47 C48 C49 C50 1.0(5) . . . . ? C48 C49 C50 C51 -1.6(5) . . . . ? C49 C50 C51 C52 1.6(5) . . . . ? C48 C47 C52 C51 0.5(5) . . . . ? B2 C47 C52 C51 178.9(3) . . . . ? C50 C51 C52 C47 -1.1(5) . . . . ? N2 B2 C53 C54 15.1(5) . . . . ? C41 B2 C53 C54 -102.6(4) . . . . ? C47 B2 C53 C54 127.6(4) . . . . ? N2 B2 C53 C58 -167.0(3) . . . . ? C41 B2 C53 C58 75.4(4) . . . . ? C47 B2 C53 C58 -54.5(4) . . . . ? C58 C53 C54 C55 -0.4(5) . . . . ? B2 C53 C54 C55 177.6(3) . . . . ? C53 C54 C55 C56 -0.4(5) . . . . ? C54 C55 C56 C57 0.5(5) . . . . ? C55 C56 C57 C58 0.2(5) . . . . ? C56 C57 C58 C53 -1.1(6) . . . . ? C54 C53 C58 C57 1.2(5) . . . . ? B2 C53 C58 C57 -177.0(3) . . . . ? Ru1 C39 N1 B1 155(15) . . . . ? C13 B1 N1 C39 -124(11) . . . . ? C7 B1 N1 C39 -2(11) . . . . ? C1 B1 N1 C39 118(11) . . . . ? Ru1 C40 N2 B2 2(3) . . . . ? C53 B2 N2 C40 156.4(11) . . . . ? C41 B2 N2 C40 -81.3(12) . . . . ? C47 B2 N2 C40 39.0(13) . . . . ? C20 C19 N3 C23 -2.2(5) . . . . ? C20 C19 N3 Ru1 179.6(2) . . . . ? C22 C23 N3 C19 1.6(5) . . . . ? C22 C23 N3 Ru1 179.7(3) . . . . ? C25 C24 N4 C28 0.4(5) . . . . ? C25 C24 N4 Ru1 -179.5(3) . . . . ? C27 C28 N4 C24 0.0(5) . . . . ? C27 C28 N4 Ru1 179.9(3) . . . . ? C31 C30 N5 C29 -0.4(5) . . . . ? C31 C30 N5 Ru1 179.3(3) . . . . ? C33 C29 N5 C30 0.7(5) . . . . ? C33 C29 N5 Ru1 -179.0(2) . . . . ? C37 C38 N6 C34 1.3(5) . . . . ? C37 C38 N6 Ru1 176.6(3) . . . . ? C35 C34 N6 C38 -2.7(5) . . . . ? C35 C34 N6 Ru1 -178.1(3) . . . . ? N2 C40 Ru1 C39 -16(5) . . . . ? N2 C40 Ru1 N5 -171(2) . . . . ? N2 C40 Ru1 N3 99(2) . . . . ? N2 C40 Ru1 N4 9(2) . . . . ? N2 C40 Ru1 N6 -79(2) . . . . ? N1 C39 Ru1 C40 -15(22) . . . . ? N1 C39 Ru1 N5 140(20) . . . . ? N1 C39 Ru1 N3 -130(20) . . . . ? N1 C39 Ru1 N4 -40(20) . . . . ? N1 C39 Ru1 N6 49(20) . . . . ? C30 N5 Ru1 C40 -42.5(3) . . . . ? C29 N5 Ru1 C40 137.1(3) . . . . ? C30 N5 Ru1 C39 138.6(3) . . . . ? C29 N5 Ru1 C39 -41.8(3) . . . . ? C30 N5 Ru1 N3 48.1(3) . . . . ? C29 N5 Ru1 N3 -132.3(3) . . . . ? C30 N5 Ru1 N4 -23(4) . . . . ? C29 N5 Ru1 N4 157(4) . . . . ? C30 N5 Ru1 N6 -131.9(3) . . . . ? C29 N5 Ru1 N6 47.7(3) . . . . ? C19 N3 Ru1 C40 -34.8(3) . . . . ? C23 N3 Ru1 C40 147.1(3) . . . . ? C19 N3 Ru1 C39 142.8(3) . . . . ? C23 N3 Ru1 C39 -35.3(3) . . . . ? C19 N3 Ru1 N5 -125.9(3) . . . . ? C23 N3 Ru1 N5 56.0(3) . . . . ? C19 N3 Ru1 N4 52.8(3) . . . . ? C23 N3 Ru1 N4 -125.3(3) . . . . ? C19 N3 Ru1 N6 54(5) . . . . ? C23 N3 Ru1 N6 -124(5) . . . . ? C24 N4 Ru1 C40 137.1(3) . . . . ? C28 N4 Ru1 C40 -42.8(3) . . . . ? C24 N4 Ru1 C39 -44.0(3) . . . . ? C28 N4 Ru1 C39 136.1(3) . . . . ? C24 N4 Ru1 N5 117(4) . . . . ? C28 N4 Ru1 N5 -62(4) . . . . ? C24 N4 Ru1 N3 46.5(3) . . . . ? C28 N4 Ru1 N3 -133.4(3) . . . . ? C24 N4 Ru1 N6 -133.5(3) . . . . ? C28 N4 Ru1 N6 46.6(3) . . . . ? C38 N6 Ru1 C40 -38.1(3) . . . . ? C34 N6 Ru1 C40 137.0(3) . . . . ? C38 N6 Ru1 C39 144.2(3) . . . . ? C34 N6 Ru1 C39 -40.7(3) . . . . ? C38 N6 Ru1 N5 52.9(3) . . . . ? C34 N6 Ru1 N5 -132.0(3) . . . . ? C38 N6 Ru1 N3 -127(5) . . . . ? C34 N6 Ru1 N3 48(5) . . . . ? C38 N6 Ru1 N4 -125.8(3) . . . . ? C34 N6 Ru1 N4 49.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.300 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.061 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 739894' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H58 B2 N6 Ru' _chemical_formula_sum 'C62 H58 B2 N6 Ru' _chemical_formula_weight 1009.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthor _symmetry_space_group_name_H-M 'A b a 2' _symmetry_space_group_name_Hall 'A 2 -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 16.589(3) _cell_length_b 17.758(3) _cell_length_c 18.439(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5432.0(17) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3523 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 26.78 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.333 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.943 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart apex II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14457 _diffrn_reflns_av_R_equivalents 0.1045 _diffrn_reflns_av_sigmaI/netI 0.1941 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.30 _reflns_number_total 5155 _reflns_number_gt 2223 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Bruker, 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0080P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(5) _refine_ls_number_reflns 5155 _refine_ls_number_parameters 323 _refine_ls_number_restraints 229 _refine_ls_R_factor_all 0.1540 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 0.791 _refine_ls_restrained_S_all 0.808 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.5000 1.0000 0.52212(8) 0.0511(2) Uani 1 2 d SU . . B1 B 0.7431(4) 0.8584(4) 0.5356(5) 0.054(2) Uani 1 1 d U . . N1 N 0.6646(3) 0.9110(3) 0.5232(4) 0.0566(14) Uani 1 1 d U . . N2 N 0.4586(4) 0.9277(5) 0.6006(4) 0.060(2) Uani 1 1 d U . . N3 N 0.5453(4) 1.0692(4) 0.4418(3) 0.048(2) Uani 1 1 d U . . C1 C 0.7779(5) 0.8858(5) 0.6142(4) 0.064(2) Uani 1 1 d U . . C2 C 0.7317(5) 0.8810(5) 0.6738(5) 0.091(3) Uani 1 1 d U . . H2 H 0.6813 0.8586 0.6689 0.109 Uiso 1 1 calc R . . C3 C 0.7544(7) 0.9079(5) 0.7449(5) 0.115(4) Uani 1 1 d U . . H3 H 0.7221 0.9025 0.7859 0.139 Uiso 1 1 calc R . . C4 C 0.8267(6) 0.9415(6) 0.7456(6) 0.116(4) Uani 1 1 d U . . H4 H 0.8424 0.9632 0.7892 0.140 Uiso 1 1 calc R . . C5 C 0.8773(7) 0.9470(7) 0.6920(6) 0.123(4) Uani 1 1 d U . . H5 H 0.9276 0.9689 0.6985 0.147 Uiso 1 1 calc R . . C6 C 0.8529(6) 0.9177(6) 0.6213(5) 0.098(3) Uani 1 1 d U . . H6 H 0.8876 0.9206 0.5817 0.118 Uiso 1 1 calc R . . C7 C 0.7105(4) 0.7738(4) 0.5359(4) 0.052(2) Uani 1 1 d U . . C8 C 0.6478(4) 0.7482(5) 0.4904(4) 0.083(3) Uani 1 1 d U . . H8 H 0.6249 0.7817 0.4576 0.100 Uiso 1 1 calc R . . C9 C 0.6190(5) 0.6746(6) 0.4931(5) 0.107(4) Uani 1 1 d U . . H9 H 0.5764 0.6602 0.4634 0.129 Uiso 1 1 calc R . . C10 C 0.6523(5) 0.6246(5) 0.5379(6) 0.106(3) Uani 1 1 d U . . H10 H 0.6326 0.5755 0.5396 0.127 Uiso 1 1 calc R . . C11 C 0.7136(5) 0.6448(6) 0.5803(5) 0.094(3) Uani 1 1 d U . . H11 H 0.7370 0.6101 0.6116 0.113 Uiso 1 1 calc R . . C12 C 0.7418(4) 0.7177(5) 0.5770(4) 0.072(2) Uani 1 1 d U . . H12 H 0.7862 0.7295 0.6056 0.086 Uiso 1 1 calc R . . C13 C 0.8038(5) 0.8767(5) 0.4729(4) 0.057(2) Uani 1 1 d U . . C14 C 0.8592(5) 0.8250(5) 0.4455(5) 0.096(3) Uani 1 1 d U . . H14 H 0.8560 0.7756 0.4619 0.116 Uiso 1 1 calc R . . C15 C 0.9179(5) 0.8420(7) 0.3962(5) 0.121(4) Uani 1 1 d U . . H15 H 0.9531 0.8046 0.3805 0.145 Uiso 1 1 calc R . . C16 C 0.9251(6) 0.9120(7) 0.3703(5) 0.109(4) Uani 1 1 d U . . H16 H 0.9653 0.9232 0.3368 0.131 Uiso 1 1 calc R . . C17 C 0.8739(6) 0.9666(6) 0.3927(5) 0.108(4) Uani 1 1 d U . . H17 H 0.8788 1.0158 0.3760 0.130 Uiso 1 1 calc R . . C18 C 0.8147(5) 0.9468(5) 0.4409(4) 0.083(3) Uani 1 1 d U . . H18 H 0.7780 0.9841 0.4534 0.099 Uiso 1 1 calc R . . C19 C 0.6043(3) 0.9454(3) 0.5221(6) 0.0483(16) Uani 1 1 d U . . C20 C 0.4749(4) 0.8541(5) 0.6043(4) 0.058(2) Uani 1 1 d U . . H20 H 0.5047 0.8338 0.5663 0.070 Uiso 1 1 calc R . . C21 C 0.4522(4) 0.8062(5) 0.6578(4) 0.066(2) Uani 1 1 d U . . H21 H 0.4673 0.7558 0.6553 0.079 Uiso 1 1 calc R . . C22 C 0.4080(5) 0.8307(5) 0.7144(5) 0.063(3) Uani 1 1 d U . . C23 C 0.3860(4) 0.9050(5) 0.7147(4) 0.071(3) Uani 1 1 d U . . H23 H 0.3538 0.9242 0.7517 0.086 Uiso 1 1 calc R . . C24 C 0.4130(4) 0.9520(5) 0.6579(4) 0.062(2) Uani 1 1 d U . . H24 H 0.3989 1.0027 0.6594 0.075 Uiso 1 1 calc R . . C25 C 0.3792(4) 0.7776(5) 0.7733(4) 0.089(3) Uani 1 1 d U . . H25A H 0.3417 0.7421 0.7530 0.134 Uiso 1 1 calc R . . H25B H 0.3532 0.8059 0.8109 0.134 Uiso 1 1 calc R . . H25C H 0.4245 0.7510 0.7932 0.134 Uiso 1 1 calc R . . C26 C 0.6215(4) 1.0942(4) 0.4425(4) 0.065(2) Uani 1 1 d U . . H26 H 0.6533 1.0838 0.4828 0.078 Uiso 1 1 calc R . . C27 C 0.6547(5) 1.1342(5) 0.3867(5) 0.087(3) Uani 1 1 d U . . H27 H 0.7079 1.1502 0.3905 0.105 Uiso 1 1 calc R . . C28 C 0.6130(6) 1.1509(6) 0.3268(6) 0.087(3) Uani 1 1 d U . . C29 C 0.5320(4) 1.1275(5) 0.3253(4) 0.072(3) Uani 1 1 d U . . H29 H 0.4996 1.1379 0.2854 0.087 Uiso 1 1 calc R . . C30 C 0.5018(5) 1.0894(4) 0.3837(4) 0.070(2) Uani 1 1 d U . . H30 H 0.4475 1.0766 0.3831 0.084 Uiso 1 1 calc R . . C31 C 0.6447(6) 1.1895(6) 0.2606(5) 0.132(4) Uani 1 1 d U . . H31A H 0.6880 1.1604 0.2404 0.199 Uiso 1 1 calc R . . H31B H 0.6641 1.2386 0.2734 0.199 Uiso 1 1 calc R . . H31C H 0.6023 1.1941 0.2254 0.199 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0393(3) 0.0500(4) 0.0639(4) 0.000 0.000 0.0087(5) B1 0.051(4) 0.050(4) 0.062(4) 0.004(4) -0.007(3) 0.004(3) N1 0.054(3) 0.055(3) 0.061(3) -0.001(4) 0.001(4) 0.004(2) N2 0.052(4) 0.060(4) 0.068(4) 0.002(4) -0.001(3) 0.004(3) N3 0.040(3) 0.050(4) 0.053(4) -0.004(3) 0.000(3) 0.005(3) C1 0.066(4) 0.061(4) 0.065(4) 0.007(4) 0.000(3) 0.006(4) C2 0.089(4) 0.093(5) 0.090(4) -0.007(4) -0.002(4) 0.010(4) C3 0.118(5) 0.116(5) 0.112(6) -0.001(4) -0.002(4) 0.015(4) C4 0.122(5) 0.112(6) 0.115(5) -0.007(4) -0.014(4) -0.006(4) C5 0.121(6) 0.121(6) 0.126(6) 0.000(5) -0.018(4) -0.010(4) C6 0.098(4) 0.098(5) 0.098(5) -0.002(4) -0.015(4) -0.009(4) C7 0.046(3) 0.057(4) 0.051(4) -0.002(4) -0.001(3) 0.006(3) C8 0.087(4) 0.075(5) 0.088(5) -0.002(4) -0.025(4) 0.003(4) C9 0.101(5) 0.105(5) 0.116(6) 0.000(4) -0.025(4) -0.005(4) C10 0.111(5) 0.095(5) 0.112(5) -0.002(4) -0.009(4) -0.009(4) C11 0.100(5) 0.086(5) 0.097(5) 0.004(4) -0.006(4) 0.010(4) C12 0.067(4) 0.071(4) 0.077(4) -0.001(4) -0.009(3) -0.008(4) C13 0.055(4) 0.055(4) 0.061(4) -0.004(4) -0.004(3) 0.004(3) C14 0.094(4) 0.091(5) 0.104(5) -0.004(4) 0.020(4) 0.000(4) C15 0.111(5) 0.120(6) 0.132(5) -0.007(4) 0.023(4) 0.013(4) C16 0.104(5) 0.112(6) 0.112(5) 0.007(4) 0.018(4) -0.001(4) C17 0.111(5) 0.107(6) 0.107(5) 0.003(4) 0.012(4) -0.004(4) C18 0.080(4) 0.087(5) 0.081(5) 0.005(4) 0.002(4) 0.003(4) C19 0.041(3) 0.044(3) 0.061(3) 0.003(4) 0.000(4) 0.005(3) C20 0.048(4) 0.060(4) 0.067(4) -0.003(4) 0.002(3) 0.002(3) C21 0.060(4) 0.064(4) 0.073(4) 0.000(4) -0.003(4) 0.002(3) C22 0.057(4) 0.069(5) 0.064(4) 0.019(4) -0.010(4) -0.002(4) C23 0.075(4) 0.075(5) 0.064(4) -0.004(4) 0.005(4) -0.003(4) C24 0.059(4) 0.060(4) 0.067(4) 0.001(4) -0.004(4) 0.002(3) C25 0.087(4) 0.087(5) 0.093(5) 0.015(4) -0.006(4) -0.004(4) C26 0.060(4) 0.067(4) 0.069(4) 0.005(4) 0.003(4) -0.003(3) C27 0.078(4) 0.093(5) 0.090(4) 0.005(4) -0.003(4) -0.002(4) C28 0.080(5) 0.091(5) 0.089(5) 0.012(4) 0.015(4) 0.004(4) C29 0.072(4) 0.074(5) 0.071(4) 0.004(4) -0.006(3) 0.002(4) C30 0.068(4) 0.070(4) 0.072(4) 0.005(4) 0.006(4) 0.001(4) C31 0.135(6) 0.138(6) 0.124(5) 0.023(4) 0.018(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C19 1.983(5) 2_675 ? Ru1 C19 1.983(5) . ? Ru1 N2 2.053(7) 2_675 ? Ru1 N2 2.053(7) . ? Ru1 N3 2.065(7) . ? Ru1 N3 2.065(7) 2_675 ? B1 C13 1.567(11) . ? B1 C7 1.597(9) . ? B1 N1 1.618(8) . ? B1 C1 1.634(10) . ? N1 C19 1.174(5) . ? N2 C20 1.337(9) . ? N2 C24 1.368(8) . ? N3 C30 1.340(8) . ? N3 C26 1.341(7) . ? C1 C2 1.342(9) . ? C1 C6 1.372(10) . ? C2 C3 1.446(10) . ? C2 H2 0.9300 . ? C3 C4 1.339(12) . ? C3 H3 0.9300 . ? C4 C5 1.300(12) . ? C4 H4 0.9300 . ? C5 C6 1.461(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.356(9) . ? C7 C8 1.410(8) . ? C8 C9 1.393(11) . ? C8 H8 0.9300 . ? C9 C10 1.333(11) . ? C9 H9 0.9300 . ? C10 C11 1.332(10) . ? C10 H10 0.9300 . ? C11 C12 1.379(11) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.389(11) . ? C13 C14 1.395(10) . ? C14 C15 1.365(10) . ? C14 H14 0.9300 . ? C15 C16 1.337(12) . ? C15 H15 0.9300 . ? C16 C17 1.354(12) . ? C16 H16 0.9300 . ? C17 C18 1.370(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C20 C21 1.356(9) . ? C20 H20 0.9300 . ? C21 C22 1.349(10) . ? C21 H21 0.9300 . ? C22 C23 1.370(10) . ? C22 C25 1.515(10) . ? C23 C24 1.413(9) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.367(10) . ? C26 H26 0.9300 . ? C27 C28 1.336(11) . ? C27 H27 0.9300 . ? C28 C29 1.407(10) . ? C28 C31 1.496(11) . ? C29 C30 1.367(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 C19 Ru1 C19 179.9(6) 2_675 . ? C19 Ru1 N2 89.2(3) 2_675 2_675 ? C19 Ru1 N2 90.8(3) . 2_675 ? C19 Ru1 N2 90.8(3) 2_675 . ? C19 Ru1 N2 89.2(3) . . ? N2 Ru1 N2 90.3(4) 2_675 . ? C19 Ru1 N3 91.5(3) 2_675 . ? C19 Ru1 N3 88.5(3) . . ? N2 Ru1 N3 90.7(2) 2_675 . ? N2 Ru1 N3 177.5(4) . . ? C19 Ru1 N3 88.5(3) 2_675 2_675 ? C19 Ru1 N3 91.5(3) . 2_675 ? N2 Ru1 N3 177.5(4) 2_675 2_675 ? N2 Ru1 N3 90.7(2) . 2_675 ? N3 Ru1 N3 88.4(4) . 2_675 ? C13 B1 C7 114.5(7) . . ? C13 B1 N1 107.0(7) . . ? C7 B1 N1 105.7(5) . . ? C13 B1 C1 111.4(6) . . ? C7 B1 C1 113.4(7) . . ? N1 B1 C1 103.8(7) . . ? C19 N1 B1 171.7(9) . . ? C20 N2 C24 112.4(7) . . ? C20 N2 Ru1 125.4(6) . . ? C24 N2 Ru1 122.2(6) . . ? C30 N3 C26 115.2(7) . . ? C30 N3 Ru1 122.5(6) . . ? C26 N3 Ru1 122.2(6) . . ? C2 C1 C6 117.8(9) . . ? C2 C1 B1 120.3(8) . . ? C6 C1 B1 121.8(8) . . ? C1 C2 C3 124.9(9) . . ? C1 C2 H2 117.5 . . ? C3 C2 H2 117.5 . . ? C4 C3 C2 112.9(10) . . ? C4 C3 H3 123.6 . . ? C2 C3 H3 123.6 . . ? C5 C4 C3 127.2(11) . . ? C5 C4 H4 116.4 . . ? C3 C4 H4 116.4 . . ? C4 C5 C6 118.2(11) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? C1 C6 C5 118.8(9) . . ? C1 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C12 C7 C8 112.2(7) . . ? C12 C7 B1 124.3(7) . . ? C8 C7 B1 123.5(7) . . ? C9 C8 C7 122.3(8) . . ? C9 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C10 C9 C8 120.4(9) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.0(10) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 119.1(10) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C7 C12 C11 125.8(8) . . ? C7 C12 H12 117.1 . . ? C11 C12 H12 117.1 . . ? C18 C13 C14 110.4(8) . . ? C18 C13 B1 125.7(8) . . ? C14 C13 B1 123.7(9) . . ? C15 C14 C13 124.5(10) . . ? C15 C14 H14 117.8 . . ? C13 C14 H14 117.8 . . ? C16 C15 C14 120.4(11) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.1(10) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 117.6(11) . . ? C16 C17 H17 121.2 . . ? C18 C17 H17 121.2 . . ? C17 C18 C13 126.8(9) . . ? C17 C18 H18 116.6 . . ? C13 C18 H18 116.6 . . ? N1 C19 Ru1 177.7(7) . . ? N2 C20 C21 126.5(8) . . ? N2 C20 H20 116.8 . . ? C21 C20 H20 116.8 . . ? C22 C21 C20 120.8(9) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 117.3(9) . . ? C21 C22 C25 121.7(9) . . ? C23 C22 C25 120.9(9) . . ? C22 C23 C24 118.8(8) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? N2 C24 C23 124.2(8) . . ? N2 C24 H24 117.9 . . ? C23 C24 H24 117.9 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 C27 123.0(8) . . ? N3 C26 H26 118.5 . . ? C27 C26 H26 118.5 . . ? C28 C27 C26 122.0(9) . . ? C28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C27 C28 C29 116.5(10) . . ? C27 C28 C31 126.5(10) . . ? C29 C28 C31 117.0(9) . . ? C30 C29 C28 118.7(8) . . ? C30 C29 H29 120.7 . . ? C28 C29 H29 120.7 . . ? N3 C30 C29 124.5(8) . . ? N3 C30 H30 117.8 . . ? C29 C30 H30 117.8 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.580 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.049 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 739895' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C148 H170 B4 N12 O3 Ru2' _chemical_formula_weight 2410.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.973(11) _cell_length_b 19.944(13) _cell_length_c 26.817(14) _cell_angle_alpha 90.000(14) _cell_angle_beta 122.53(3) _cell_angle_gamma 90.000(13) _cell_volume 7203(8) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 4382 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 20.42 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2548 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9373 _exptl_absorpt_correction_T_max 0.9667 _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart apex II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37990 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14107 _reflns_number_gt 11488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Bruker, 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+1.9900P] 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 14107 _refine_ls_number_parameters 763 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1400 _refine_ls_wR_factor_gt 0.1311 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 1.0481(3) 0.21205(19) 0.38201(16) 0.0437(8) Uani 1 1 d . . . B2 B 0.5000(3) -0.06981(16) 0.14949(17) 0.0397(8) Uani 1 1 d . . . C1 C 0.9724(2) 0.27429(16) 0.36316(15) 0.0481(8) Uani 1 1 d . . . C2 C 0.9172(2) 0.28311(18) 0.38897(16) 0.0501(8) Uani 1 1 d . . . H2 H 0.9292 0.2551 0.4199 0.060 Uiso 1 1 calc R . . C3 C 0.8430(2) 0.33378(18) 0.36949(16) 0.0535(9) Uani 1 1 d . . . H3 H 0.8096 0.3399 0.3888 0.064 Uiso 1 1 calc R . . C4 C 0.8219(3) 0.37196(18) 0.32408(17) 0.0569(9) Uani 1 1 d . . . H4 H 0.7712 0.4034 0.3106 0.068 Uiso 1 1 calc R . . C5 C 0.8741(2) 0.36648(17) 0.29543(15) 0.0528(9) Uani 1 1 d . . . H5 H 0.8597 0.3942 0.2639 0.063 Uiso 1 1 calc R . . C6 C 0.9491(3) 0.31717(17) 0.31664(15) 0.0520(8) Uani 1 1 d . . . H6 H 0.9848 0.3132 0.2985 0.062 Uiso 1 1 calc R . . C7 C 1.0995(2) 0.18883(16) 0.45028(14) 0.0451(7) Uani 1 1 d . . . C8 C 1.1428(2) 0.23348(17) 0.49628(14) 0.0467(8) Uani 1 1 d . . . H8 H 1.1385 0.2789 0.4872 0.056 Uiso 1 1 calc R . . C9 C 1.1921(2) 0.21580(18) 0.55476(15) 0.0518(8) Uani 1 1 d . . . H9 H 1.2214 0.2486 0.5840 0.062 Uiso 1 1 calc R . . C10 C 1.1981(2) 0.14848(18) 0.57028(15) 0.0525(8) Uani 1 1 d . . . H10 H 1.2301 0.1360 0.6098 0.063 Uiso 1 1 calc R . . C11 C 1.1567(3) 0.10165(18) 0.52717(15) 0.0531(9) Uani 1 1 d . . . H11 H 1.1592 0.0566 0.5369 0.064 Uiso 1 1 calc R . . C12 C 1.1098(2) 0.12118(17) 0.46745(15) 0.0471(8) Uani 1 1 d . . . H12 H 1.0848 0.0882 0.4384 0.057 Uiso 1 1 calc R . . C13 C 1.13356(13) 0.22432(11) 0.36421(9) 0.0442(7) Uani 1 1 d G . . C14 C 1.20743(16) 0.27169(11) 0.39621(9) 0.0533(9) Uani 1 1 d G . . H14 H 1.2062 0.2977 0.4246 0.064 Uiso 1 1 calc R . . C15 C 1.28317(14) 0.28013(10) 0.38583(10) 0.0558(9) Uani 1 1 d G . . H15 H 1.3326 0.3118 0.4072 0.067 Uiso 1 1 calc R . . C16 C 1.28505(14) 0.24121(12) 0.34345(10) 0.0527(8) Uani 1 1 d G . . H16 H 1.3357 0.2469 0.3365 0.063 Uiso 1 1 calc R . . C17 C 1.21118(16) 0.19385(11) 0.31144(9) 0.0499(8) Uani 1 1 d G . . H17 H 1.2124 0.1678 0.2831 0.060 Uiso 1 1 calc R . . C18 C 1.13544(13) 0.18540(10) 0.32183(9) 0.0494(8) Uani 1 1 d G . . H18 H 1.0860 0.1537 0.3004 0.059 Uiso 1 1 calc R . . C19 C 0.6964(2) 0.02010(14) 0.32252(13) 0.0370(6) Uani 1 1 d . . . H19 H 0.6946 -0.0223 0.3076 0.044 Uiso 1 1 calc R . . C20 C 0.6530(2) 0.02849(16) 0.35377(13) 0.0412(7) Uani 1 1 d . . . H20 H 0.6232 -0.0080 0.3597 0.049 Uiso 1 1 calc R . . C21 C 0.6521(2) 0.09179(16) 0.37763(14) 0.0433(7) Uani 1 1 d . . . C22 C 0.7018(2) 0.14191(15) 0.36763(13) 0.0416(7) Uani 1 1 d . . . H22 H 0.7060 0.1846 0.3827 0.050 Uiso 1 1 calc R . . C23 C 0.7451(2) 0.12963(15) 0.33579(14) 0.0410(7) Uani 1 1 d . . . H23 H 0.7781 0.1648 0.3308 0.049 Uiso 1 1 calc R . . C24 C 0.5964(2) 0.10291(16) 0.40791(15) 0.0453(7) Uani 1 1 d . . . C25 C 0.4808(2) 0.08731(18) 0.35945(16) 0.0516(8) Uani 1 1 d . . . H25A H 0.4757 0.0478 0.3375 0.077 Uiso 1 1 calc R . . H25B H 0.4518 0.1246 0.3329 0.077 Uiso 1 1 calc R . . H25C H 0.4461 0.0802 0.3792 0.077 Uiso 1 1 calc R . . C26 C 0.5943(2) 0.17658(17) 0.42382(16) 0.0503(8) Uani 1 1 d . . . H26A H 0.5456 0.1822 0.4341 0.075 Uiso 1 1 calc R . . H26B H 0.5774 0.2045 0.3905 0.075 Uiso 1 1 calc R . . H26C H 0.6585 0.1891 0.4568 0.075 Uiso 1 1 calc R . . C27 C 0.6345(3) 0.05667(17) 0.45868(16) 0.0518(8) Uani 1 1 d . . . H27A H 0.6475 0.0137 0.4482 0.078 Uiso 1 1 calc R . . H27B H 0.5859 0.0519 0.4691 0.078 Uiso 1 1 calc R . . H27C H 0.6948 0.0744 0.4918 0.078 Uiso 1 1 calc R . . C28 C 0.6130(2) 0.15012(16) 0.18497(14) 0.0417(7) Uani 1 1 d . . . H28 H 0.5804 0.1144 0.1897 0.050 Uiso 1 1 calc R . . C29 C 0.5587(2) 0.20494(14) 0.15404(13) 0.0347(6) Uani 1 1 d . . . H29 H 0.4908 0.2044 0.1384 0.042 Uiso 1 1 calc R . . C30 C 0.5987(2) 0.26087(16) 0.14460(14) 0.0444(7) Uani 1 1 d . . . C31 C 0.7026(2) 0.25747(16) 0.17128(15) 0.0473(8) Uani 1 1 d . . . H31 H 0.7367 0.2934 0.1683 0.057 Uiso 1 1 calc R . . C32 C 0.7528(2) 0.20091(17) 0.20154(14) 0.0455(8) Uani 1 1 d . . . H32 H 0.8212 0.2004 0.2185 0.055 Uiso 1 1 calc R . . C33 C 0.5372(3) 0.32017(18) 0.11037(15) 0.0511(8) Uani 1 1 d . . . C34 C 0.4354(3) 0.29917(17) 0.05913(16) 0.0525(8) Uani 1 1 d . . . H34A H 0.4321 0.3051 0.0226 0.079 Uiso 1 1 calc R . . H34B H 0.3855 0.3263 0.0588 0.079 Uiso 1 1 calc R . . H34C H 0.4242 0.2529 0.0636 0.079 Uiso 1 1 calc R . . C35 C 0.5764(3) 0.35949(17) 0.07890(15) 0.0506(8) Uani 1 1 d . . . H35A H 0.5264 0.3903 0.0516 0.076 Uiso 1 1 calc R . . H35B H 0.5931 0.3292 0.0577 0.076 Uiso 1 1 calc R . . H35C H 0.6345 0.3840 0.1074 0.076 Uiso 1 1 calc R . . C36 C 0.5041(3) 0.36317(18) 0.14318(16) 0.0531(8) Uani 1 1 d . . . H36A H 0.5608 0.3846 0.1760 0.080 Uiso 1 1 calc R . . H36B H 0.4720 0.3355 0.1574 0.080 Uiso 1 1 calc R . . H36C H 0.4584 0.3967 0.1169 0.080 Uiso 1 1 calc R . . C37 C 0.8681(2) -0.08540(16) 0.26802(15) 0.0448(7) Uani 1 1 d . . . H37 H 0.8287 -0.0841 0.2269 0.054 Uiso 1 1 calc R . . C38 C 0.9192(2) -0.14519(16) 0.29504(16) 0.0494(8) Uani 1 1 d . . . H38 H 0.9152 -0.1816 0.2722 0.059 Uiso 1 1 calc R . . C39 C 0.9739(3) -0.14891(17) 0.35429(16) 0.0532(9) Uani 1 1 d . . . C40 C 0.9802(2) -0.09138(17) 0.38660(16) 0.0493(8) Uani 1 1 d . . . H40 H 1.0193 -0.0922 0.4277 0.059 Uiso 1 1 calc R . . C41 C 0.9289(3) -0.03407(17) 0.35792(15) 0.0528(9) Uani 1 1 d . . . H41 H 0.9331 0.0029 0.3803 0.063 Uiso 1 1 calc R . . C42 C 1.0291(2) -0.21290(17) 0.38467(15) 0.0491(8) Uani 1 1 d . . . C43 C 0.9528(3) -0.27173(18) 0.36179(16) 0.0540(9) Uani 1 1 d . . . H43A H 0.9272 -0.2795 0.3207 0.081 Uiso 1 1 calc R . . H43B H 0.8992 -0.2603 0.3666 0.081 Uiso 1 1 calc R . . H43C H 0.9851 -0.3116 0.3840 0.081 Uiso 1 1 calc R . . C44 C 1.1049(2) -0.23025(18) 0.36919(15) 0.0507(8) Uani 1 1 d . . . H44A H 1.0715 -0.2387 0.3275 0.076 Uiso 1 1 calc R . . H44B H 1.1411 -0.2696 0.3906 0.076 Uiso 1 1 calc R . . H44C H 1.1502 -0.1935 0.3796 0.076 Uiso 1 1 calc R . . C45 C 1.0749(3) -0.21451(18) 0.45079(16) 0.0518(8) Uani 1 1 d . . . H45A H 1.0792 -0.2601 0.4635 0.078 Uiso 1 1 calc R . . H45B H 1.0342 -0.1892 0.4604 0.078 Uiso 1 1 calc R . . H45C H 1.1401 -0.1953 0.4705 0.078 Uiso 1 1 calc R . . C46 C 0.9375(2) 0.03898(16) 0.21401(14) 0.0412(7) Uani 1 1 d . . . H46 H 0.9843 0.0362 0.2544 0.049 Uiso 1 1 calc R . . C47 C 0.9700(2) 0.03336(16) 0.17479(14) 0.0427(7) Uani 1 1 d . . . H47 H 1.0376 0.0299 0.1899 0.051 Uiso 1 1 calc R . . C48 C 0.9023(2) 0.03279(16) 0.11303(14) 0.0436(7) Uani 1 1 d . . . C49 C 0.8035(2) 0.04160(16) 0.09588(13) 0.0437(7) Uani 1 1 d . . . H49 H 0.7543 0.0426 0.0558 0.052 Uiso 1 1 calc R . . C50 C 0.7775(2) 0.04874(15) 0.13590(13) 0.0413(7) Uani 1 1 d . . . H50 H 0.7105 0.0545 0.1215 0.050 Uiso 1 1 calc R . . C51 C 0.9350(2) 0.01949(16) 0.06993(14) 0.0463(8) Uani 1 1 d . . . C52 C 0.8753(3) 0.06381(17) 0.01508(15) 0.0480(8) Uani 1 1 d . . . H52A H 0.8077 0.0485 -0.0076 0.072 Uiso 1 1 calc R . . H52B H 0.9036 0.0613 -0.0086 0.072 Uiso 1 1 calc R . . H52C H 0.8770 0.1094 0.0271 0.072 Uiso 1 1 calc R . . C53 C 0.9129(3) -0.05437(16) 0.05143(15) 0.0494(8) Uani 1 1 d . . . H53A H 0.9571 -0.0824 0.0844 0.074 Uiso 1 1 calc R . . H53B H 0.9222 -0.0626 0.0194 0.074 Uiso 1 1 calc R . . H53C H 0.8455 -0.0644 0.0389 0.074 Uiso 1 1 calc R . . C54 C 1.0459(2) 0.03456(17) 0.09685(15) 0.0469(7) Uani 1 1 d . . . H54A H 1.0584 0.0812 0.1069 0.070 Uiso 1 1 calc R . . H54B H 1.0632 0.0238 0.0686 0.070 Uiso 1 1 calc R . . H54C H 1.0852 0.0080 0.1318 0.070 Uiso 1 1 calc R . . C55 C 0.9131(2) 0.11562(14) 0.30917(12) 0.0322(6) Uani 1 1 d . . . C56 C 0.6731(2) 0.00054(15) 0.20247(13) 0.0388(7) Uani 1 1 d . . . C57 C 0.4237(2) -0.01238(15) 0.14609(14) 0.0422(7) Uani 1 1 d . . . C58 C 0.3783(2) 0.03387(17) 0.09985(15) 0.0487(8) Uani 1 1 d . . . H58 H 0.3863 0.0289 0.0681 0.058 Uiso 1 1 calc R . . C59 C 0.3207(2) 0.08807(18) 0.09938(15) 0.0518(9) Uani 1 1 d . . . H59 H 0.2937 0.1189 0.0686 0.062 Uiso 1 1 calc R . . C60 C 0.3054(2) 0.09467(16) 0.14390(15) 0.0475(8) Uani 1 1 d . . . H60 H 0.2648 0.1291 0.1425 0.057 Uiso 1 1 calc R . . C61 C 0.3481(2) 0.05190(16) 0.19099(16) 0.0495(8) Uani 1 1 d . . . H61 H 0.3383 0.0575 0.2219 0.059 Uiso 1 1 calc R . . C62 C 0.4075(2) -0.00115(16) 0.19185(15) 0.0470(8) Uani 1 1 d . . . H62 H 0.4371 -0.0299 0.2242 0.056 Uiso 1 1 calc R . . C63 C 0.5167(2) -0.13350(15) 0.19189(13) 0.0410(7) Uani 1 1 d . . . C64 C 0.4382(2) -0.16424(16) 0.19247(15) 0.0486(8) Uani 1 1 d . . . H64 H 0.3758 -0.1442 0.1715 0.058 Uiso 1 1 calc R . . C65 C 0.4494(2) -0.22307(16) 0.22286(14) 0.0461(7) Uani 1 1 d . . . H65 H 0.3943 -0.2432 0.2198 0.055 Uiso 1 1 calc R . . C66 C 0.5397(2) -0.25133(17) 0.25681(14) 0.0455(7) Uani 1 1 d . . . H66 H 0.5469 -0.2904 0.2776 0.055 Uiso 1 1 calc R . . C67 C 0.6234(2) -0.22188(16) 0.26086(14) 0.0448(7) Uani 1 1 d . . . H67 H 0.6863 -0.2405 0.2849 0.054 Uiso 1 1 calc R . . C68 C 0.6092(2) -0.16351(16) 0.22758(14) 0.0439(7) Uani 1 1 d . . . H68 H 0.6640 -0.1443 0.2295 0.053 Uiso 1 1 calc R . . C69 C 0.46981(15) -0.09746(10) 0.08244(7) 0.0391(7) Uani 1 1 d G . . C70 C 0.52084(13) -0.07664(10) 0.05648(8) 0.0490(8) Uani 1 1 d G . . H70 H 0.5726 -0.0460 0.0759 0.059 Uiso 1 1 calc R . . C71 C 0.49448(15) -0.10157(11) 0.00148(8) 0.0457(7) Uani 1 1 d G . . H71 H 0.5286 -0.0876 -0.0159 0.055 Uiso 1 1 calc R . . C72 C 0.41709(15) -0.14734(11) -0.02756(7) 0.0461(8) Uani 1 1 d G . . H72 H 0.3995 -0.1640 -0.0644 0.055 Uiso 1 1 calc R . . C73 C 0.36606(14) -0.16816(10) -0.00159(9) 0.0537(9) Uani 1 1 d G . . H73 H 0.3143 -0.1988 -0.0210 0.064 Uiso 1 1 calc R . . C74 C 0.39242(15) -0.14323(11) 0.05340(9) 0.0515(8) Uani 1 1 d G . . H74 H 0.3583 -0.1572 0.0708 0.062 Uiso 1 1 calc R . . N1 N 0.97672(18) 0.15125(13) 0.34089(11) 0.0418(6) Uani 1 1 d . . . N2 N 0.60158(19) -0.03163(12) 0.17720(12) 0.0418(6) Uani 1 1 d . . . N3 N 0.74271(19) 0.07053(11) 0.31168(11) 0.0359(5) Uani 1 1 d . . . N4 N 0.71112(17) 0.14533(12) 0.20886(11) 0.0364(5) Uani 1 1 d . . . N5 N 0.87251(18) -0.02968(13) 0.29812(11) 0.0378(5) Uani 1 1 d . . . N6 N 0.84183(17) 0.04815(12) 0.19555(10) 0.0341(5) Uani 1 1 d . . . O1 O 0.9010(3) 0.0491(2) 0.4803(2) 0.0482(11) Uani 0.50 1 d P . . H1D H 0.9109 0.0811 0.4632 0.058 Uiso 0.50 1 d PR . . H1A H 0.9532 0.0253 0.4994 0.058 Uiso 0.50 1 d PR . . O2 O 0.1839(4) 0.9847(2) 0.3511(2) 0.0554(12) Uani 0.50 1 d P A 1 H2B H 0.1560 1.0004 0.3162 0.066 Uiso 0.50 1 d PR A 1 H2C H 0.2181 0.9504 0.3543 0.066 Uiso 0.50 1 d PR A 1 O3 O 0.2805(3) 1.0664(2) 0.4179(2) 0.0515(11) Uani 0.50 1 d P B 2 H3A H 0.2591 1.0762 0.4444 0.062 Uiso 0.50 1 d PR B 2 H3B H 0.2774 1.1064 0.3971 0.062 Uiso 0.50 1 d PR B 2 Ru1 Ru 0.794056(16) 0.058347(12) 0.254249(10) 0.03274(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0329(17) 0.045(2) 0.0361(18) -0.0030(15) 0.0074(14) -0.0020(15) B2 0.0364(17) 0.0252(16) 0.046(2) -0.0051(14) 0.0141(15) -0.0030(13) C1 0.0415(17) 0.0391(17) 0.0429(18) -0.0140(14) 0.0089(14) -0.0082(14) C2 0.0365(16) 0.050(2) 0.0475(19) -0.0165(15) 0.0119(14) -0.0080(14) C3 0.0395(17) 0.047(2) 0.055(2) -0.0184(17) 0.0133(15) -0.0116(15) C4 0.0488(19) 0.0413(19) 0.060(2) -0.0158(17) 0.0152(17) -0.0030(15) C5 0.0424(17) 0.0441(18) 0.0441(19) -0.0137(15) 0.0049(15) -0.0085(15) C6 0.0468(18) 0.0421(18) 0.0425(18) -0.0062(15) 0.0076(15) -0.0003(15) C7 0.0455(17) 0.0416(17) 0.0381(17) -0.0026(13) 0.0157(14) -0.0100(14) C8 0.0409(16) 0.0433(18) 0.0375(17) -0.0070(13) 0.0089(14) -0.0143(14) C9 0.0458(18) 0.052(2) 0.0419(18) -0.0087(15) 0.0129(15) -0.0117(15) C10 0.0412(17) 0.060(2) 0.0404(18) 0.0066(16) 0.0118(14) -0.0081(16) C11 0.0499(19) 0.0482(19) 0.0459(19) 0.0085(15) 0.0156(16) -0.0130(16) C12 0.0406(16) 0.0443(18) 0.0444(18) 0.0043(14) 0.0149(14) -0.0031(14) C13 0.0387(16) 0.0413(17) 0.0389(17) 0.0046(13) 0.0118(13) -0.0036(13) C14 0.0477(18) 0.049(2) 0.0471(19) -0.0044(15) 0.0152(16) -0.0170(16) C15 0.0465(19) 0.052(2) 0.049(2) 0.0017(16) 0.0125(16) -0.0166(16) C16 0.0486(18) 0.047(2) 0.051(2) 0.0083(16) 0.0199(16) -0.0050(15) C17 0.0463(18) 0.050(2) 0.0416(18) -0.0003(14) 0.0160(15) -0.0005(15) C18 0.0452(18) 0.0458(19) 0.0475(19) -0.0022(15) 0.0186(15) 0.0016(15) C19 0.0390(15) 0.0284(15) 0.0420(16) -0.0013(12) 0.0207(13) -0.0047(12) C20 0.0415(16) 0.0398(17) 0.0375(16) -0.0043(13) 0.0180(14) -0.0099(13) C21 0.0470(17) 0.0370(17) 0.0384(17) 0.0003(13) 0.0180(14) 0.0055(14) C22 0.0456(16) 0.0334(16) 0.0323(15) -0.0069(12) 0.0121(13) 0.0002(13) C23 0.0413(16) 0.0309(15) 0.0439(17) -0.0095(13) 0.0185(14) -0.0029(13) C24 0.0428(16) 0.0375(17) 0.0496(19) -0.0001(14) 0.0208(15) 0.0059(14) C25 0.0452(18) 0.0475(19) 0.050(2) -0.0035(15) 0.0173(16) -0.0025(15) C26 0.0418(17) 0.0427(18) 0.052(2) -0.0087(15) 0.0158(15) 0.0086(14) C27 0.0498(19) 0.051(2) 0.0437(19) 0.0052(15) 0.0177(16) 0.0020(16) C28 0.0316(14) 0.0376(16) 0.0461(18) -0.0014(13) 0.0143(13) -0.0006(12) C29 0.0325(14) 0.0316(14) 0.0421(16) -0.0132(12) 0.0214(13) 0.0061(11) C30 0.0418(16) 0.0425(18) 0.0370(16) 0.0022(13) 0.0132(13) 0.0029(14) C31 0.0423(16) 0.0343(16) 0.0427(17) -0.0021(13) 0.0079(14) -0.0076(13) C32 0.0320(15) 0.0491(19) 0.0389(17) 0.0146(14) 0.0081(13) -0.0007(13) C33 0.0499(18) 0.053(2) 0.0397(18) 0.0053(15) 0.0168(15) 0.0063(16) C34 0.0494(19) 0.0416(18) 0.052(2) 0.0073(15) 0.0180(16) 0.0046(15) C35 0.0475(18) 0.0442(19) 0.0468(19) 0.0069(15) 0.0165(15) 0.0035(15) C36 0.0505(19) 0.049(2) 0.0486(19) 0.0046(15) 0.0190(16) 0.0107(16) C37 0.0456(17) 0.0395(17) 0.0412(17) 0.0031(14) 0.0180(14) 0.0068(14) C38 0.0475(18) 0.0361(17) 0.055(2) 0.0014(15) 0.0215(16) 0.0089(14) C39 0.0497(19) 0.0370(18) 0.052(2) 0.0059(15) 0.0135(16) 0.0088(15) C40 0.0383(16) 0.049(2) 0.0470(19) 0.0131(15) 0.0139(15) 0.0154(15) C41 0.057(2) 0.0356(17) 0.0417(18) -0.0008(14) 0.0103(16) 0.0015(15) C42 0.0471(18) 0.0434(18) 0.0485(19) 0.0019(15) 0.0203(15) 0.0095(15) C43 0.058(2) 0.0469(19) 0.0460(19) 0.0141(15) 0.0210(16) 0.0037(16) C44 0.0444(17) 0.053(2) 0.0401(18) 0.0024(15) 0.0128(14) 0.0122(15) C45 0.0490(18) 0.0451(19) 0.054(2) 0.0129(16) 0.0227(16) 0.0103(15) C46 0.0316(14) 0.0448(17) 0.0417(17) -0.0033(13) 0.0160(13) 0.0026(13) C47 0.0359(15) 0.0435(17) 0.0406(17) -0.0059(14) 0.0153(13) 0.0039(13) C48 0.0426(17) 0.0363(16) 0.0438(18) 0.0121(14) 0.0178(14) 0.0086(13) C49 0.0467(17) 0.0399(17) 0.0277(15) 0.0007(12) 0.0090(13) 0.0062(14) C50 0.0407(16) 0.0381(17) 0.0318(15) 0.0082(12) 0.0106(13) 0.0054(13) C51 0.0430(17) 0.0449(18) 0.0328(16) 0.0014(13) 0.0083(13) 0.0106(14) C52 0.0478(18) 0.0492(19) 0.0465(19) 0.0137(15) 0.0250(16) 0.0182(15) C53 0.0458(18) 0.0445(19) 0.0435(19) 0.0041(14) 0.0145(15) 0.0083(15) C54 0.0491(18) 0.0435(17) 0.0424(18) -0.0003(14) 0.0209(15) 0.0057(15) C55 0.0313(13) 0.0285(14) 0.0333(14) -0.0049(11) 0.0151(12) 0.0038(11) C56 0.0334(15) 0.0381(16) 0.0371(16) -0.0011(13) 0.0139(13) 0.0015(13) C57 0.0380(15) 0.0359(16) 0.0430(17) -0.0110(13) 0.0155(14) -0.0042(13) C58 0.0390(16) 0.0429(18) 0.0475(19) -0.0053(15) 0.0122(15) 0.0092(14) C59 0.0408(17) 0.0480(19) 0.0456(19) -0.0163(15) 0.0093(15) 0.0111(15) C60 0.0399(16) 0.0400(18) 0.0457(19) -0.0109(14) 0.0118(14) 0.0022(14) C61 0.0460(18) 0.0424(18) 0.049(2) -0.0081(15) 0.0181(16) 0.0107(14) C62 0.0402(16) 0.0417(18) 0.0465(19) -0.0104(14) 0.0150(14) 0.0069(14) C63 0.0382(15) 0.0355(16) 0.0360(16) -0.0061(12) 0.0112(13) -0.0058(12) C64 0.0433(17) 0.0357(17) 0.0449(18) -0.0028(13) 0.0092(14) -0.0174(14) C65 0.0457(17) 0.0411(17) 0.0386(17) -0.0044(13) 0.0142(14) -0.0138(14) C66 0.0565(19) 0.0410(17) 0.0384(17) 0.0063(13) 0.0250(15) -0.0041(15) C67 0.0424(16) 0.0449(18) 0.0402(17) 0.0124(14) 0.0178(14) 0.0060(14) C68 0.0415(16) 0.0404(17) 0.0421(17) 0.0091(13) 0.0173(14) -0.0006(13) C69 0.0399(15) 0.0279(14) 0.0386(16) -0.0030(12) 0.0139(13) 0.0011(12) C70 0.0462(17) 0.0504(19) 0.0385(17) -0.0056(14) 0.0149(15) -0.0116(15) C71 0.0453(17) 0.0428(18) 0.0384(17) -0.0012(13) 0.0154(14) 0.0105(14) C72 0.0410(16) 0.0416(17) 0.0350(16) -0.0041(13) 0.0067(13) 0.0160(14) C73 0.0493(19) 0.049(2) 0.0443(19) -0.0144(15) 0.0130(16) -0.0076(16) C74 0.0516(19) 0.0469(19) 0.0420(18) -0.0120(15) 0.0159(15) -0.0163(16) N1 0.0357(13) 0.0387(14) 0.0352(13) 0.0004(11) 0.0086(11) 0.0007(11) N2 0.0393(14) 0.0278(12) 0.0434(15) -0.0053(11) 0.0125(12) -0.0025(11) N3 0.0440(13) 0.0278(12) 0.0398(14) -0.0062(10) 0.0250(11) -0.0040(10) N4 0.0293(11) 0.0389(14) 0.0363(13) 0.0045(10) 0.0146(10) 0.0023(10) N5 0.0350(12) 0.0356(13) 0.0391(14) 0.0026(11) 0.0174(11) 0.0009(10) N6 0.0342(12) 0.0349(13) 0.0296(12) -0.0010(9) 0.0148(10) 0.0024(10) O1 0.040(2) 0.055(3) 0.051(3) 0.006(2) 0.025(2) 0.002(2) O2 0.055(3) 0.054(3) 0.050(3) -0.007(2) 0.023(2) -0.015(2) O3 0.050(3) 0.049(3) 0.043(3) -0.007(2) 0.017(2) -0.013(2) Ru1 0.02810(12) 0.03896(14) 0.03193(13) -0.00140(9) 0.01665(10) -0.00019(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 C1 1.613(5) . ? B1 C7 1.620(5) . ? B1 N1 1.623(4) . ? B1 C13 1.689(4) . ? B2 N2 1.571(4) . ? B2 C63 1.628(5) . ? B2 C57 1.638(5) . ? B2 C69 1.685(4) . ? C1 C6 1.388(5) . ? C1 C2 1.394(5) . ? C2 C3 1.426(5) . ? C2 H2 0.9300 . ? C3 C4 1.317(5) . ? C3 H3 0.9300 . ? C4 C5 1.409(6) . ? C4 H4 0.9300 . ? C5 C6 1.413(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.369(4) . ? C7 C12 1.406(5) . ? C8 C9 1.370(5) . ? C8 H8 0.9300 . ? C9 C10 1.394(5) . ? C9 H9 0.9300 . ? C10 C11 1.350(5) . ? C10 H10 0.9300 . ? C11 C12 1.410(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 H16 0.9300 . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.355(4) . ? C19 N3 1.369(4) . ? C19 H19 0.9300 . ? C20 C21 1.419(5) . ? C20 H20 0.9300 . ? C21 C22 1.389(5) . ? C21 C24 1.509(5) . ? C22 C23 1.379(5) . ? C22 H22 0.9300 . ? C23 N3 1.335(4) . ? C23 H23 0.9300 . ? C24 C27 1.478(5) . ? C24 C26 1.536(4) . ? C24 C25 1.618(5) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 N4 1.340(4) . ? C28 C29 1.364(4) . ? C28 H28 0.9300 . ? C29 C30 1.374(4) . ? C29 H29 0.9300 . ? C30 C31 1.412(5) . ? C30 C33 1.495(5) . ? C31 C32 1.369(4) . ? C31 H31 0.9300 . ? C32 N4 1.361(4) . ? C32 H32 0.9300 . ? C33 C35 1.512(5) . ? C33 C36 1.514(5) . ? C33 C34 1.519(5) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N5 1.353(4) . ? C37 C38 1.406(4) . ? C37 H37 0.9300 . ? C38 C39 1.342(5) . ? C38 H38 0.9300 . ? C39 C40 1.409(5) . ? C39 C42 1.516(5) . ? C40 C41 1.375(5) . ? C40 H40 0.9300 . ? C41 N5 1.355(4) . ? C41 H41 0.9300 . ? C42 C45 1.512(5) . ? C42 C44 1.516(5) . ? C42 C43 1.560(5) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 N6 1.342(4) . ? C46 C47 1.405(4) . ? C46 H46 0.9300 . ? C47 C48 1.409(4) . ? C47 H47 0.9300 . ? C48 C49 1.397(5) . ? C48 C51 1.527(5) . ? C49 C50 1.350(5) . ? C49 H49 0.9300 . ? C50 N6 1.359(4) . ? C50 H50 0.9300 . ? C51 C52 1.532(4) . ? C51 C53 1.534(5) . ? C51 C54 1.541(5) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 N1 1.154(4) . ? C55 Ru1 2.019(3) . ? C56 N2 1.159(4) . ? C56 Ru1 2.026(3) . ? C57 C58 1.396(5) . ? C57 C62 1.402(5) . ? C58 C59 1.415(5) . ? C58 H58 0.9300 . ? C59 C60 1.348(5) . ? C59 H59 0.9300 . ? C60 C61 1.364(5) . ? C60 H60 0.9300 . ? C61 C62 1.413(4) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 C68 1.392(4) . ? C63 C64 1.404(5) . ? C64 C65 1.384(5) . ? C64 H64 0.9300 . ? C65 C66 1.347(5) . ? C65 H65 0.9300 . ? C66 C67 1.409(5) . ? C66 H66 0.9300 . ? C67 C68 1.409(4) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? C69 C70 1.3900 . ? C69 C74 1.3900 . ? C70 C71 1.3900 . ? C70 H70 0.9300 . ? C71 C72 1.3900 . ? C71 H71 0.9300 . ? C72 C73 1.3900 . ? C72 H72 0.9300 . ? C73 C74 1.3900 . ? C73 H73 0.9300 . ? C74 H74 0.9300 . ? N3 Ru1 2.112(3) . ? N4 Ru1 2.124(3) . ? N5 Ru1 2.110(3) . ? N6 Ru1 2.096(3) . ? O1 H1D 0.8499 . ? O1 H1A 0.8500 . ? O2 H2B 0.8500 . ? O2 H2C 0.8501 . ? O3 H3A 0.9600 . ? O3 H3B 0.9601 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 B1 C7 114.4(3) . . ? C1 B1 N1 103.1(2) . . ? C7 B1 N1 107.3(3) . . ? C1 B1 C13 112.6(3) . . ? C7 B1 C13 111.4(2) . . ? N1 B1 C13 107.2(3) . . ? N2 B2 C63 108.0(2) . . ? N2 B2 C57 103.6(2) . . ? C63 B2 C57 114.9(3) . . ? N2 B2 C69 107.1(3) . . ? C63 B2 C69 109.6(2) . . ? C57 B2 C69 113.1(2) . . ? C6 C1 C2 115.7(3) . . ? C6 C1 B1 123.3(3) . . ? C2 C1 B1 120.6(3) . . ? C1 C2 C3 122.0(4) . . ? C1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C4 C3 C2 119.8(4) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 121.8(4) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C4 C5 C6 117.2(4) . . ? C4 C5 H5 121.4 . . ? C6 C5 H5 121.4 . . ? C1 C6 C5 123.3(4) . . ? C1 C6 H6 118.3 . . ? C5 C6 H6 118.3 . . ? C8 C7 C12 114.5(3) . . ? C8 C7 B1 122.4(3) . . ? C12 C7 B1 122.9(3) . . ? C7 C8 C9 124.4(3) . . ? C7 C8 H8 117.8 . . ? C9 C8 H8 117.8 . . ? C8 C9 C10 119.7(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 119.2(3) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 119.9(3) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 122.3(3) . . ? C7 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C14 C13 C18 120.0 . . ? C14 C13 B1 118.08(17) . . ? C18 C13 B1 121.76(17) . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C20 C19 N3 123.7(3) . . ? C20 C19 H19 118.1 . . ? N3 C19 H19 118.1 . . ? C19 C20 C21 121.4(3) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C22 C21 C20 114.1(3) . . ? C22 C21 C24 124.2(3) . . ? C20 C21 C24 121.7(3) . . ? C23 C22 C21 121.4(3) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? N3 C23 C22 124.3(3) . . ? N3 C23 H23 117.9 . . ? C22 C23 H23 117.9 . . ? C27 C24 C21 109.6(3) . . ? C27 C24 C26 113.6(3) . . ? C21 C24 C26 113.5(3) . . ? C27 C24 C25 110.3(3) . . ? C21 C24 C25 106.8(3) . . ? C26 C24 C25 102.7(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 C29 123.0(3) . . ? N4 C28 H28 118.5 . . ? C29 C28 H28 118.5 . . ? C28 C29 C30 123.8(3) . . ? C28 C29 H29 118.1 . . ? C30 C29 H29 118.1 . . ? C29 C30 C31 113.8(3) . . ? C29 C30 C33 122.6(3) . . ? C31 C30 C33 123.6(3) . . ? C32 C31 C30 119.6(3) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? N4 C32 C31 125.5(3) . . ? N4 C32 H32 117.3 . . ? C31 C32 H32 117.3 . . ? C30 C33 C35 114.9(3) . . ? C30 C33 C36 114.2(3) . . ? C35 C33 C36 114.2(3) . . ? C30 C33 C34 111.5(3) . . ? C35 C33 C34 101.6(3) . . ? C36 C33 C34 98.2(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 C38 124.0(3) . . ? N5 C37 H37 118.0 . . ? C38 C37 H37 118.0 . . ? C39 C38 C37 119.0(3) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C38 C39 C40 118.0(3) . . ? C38 C39 C42 120.2(3) . . ? C40 C39 C42 121.8(3) . . ? C41 C40 C39 120.6(3) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? N5 C41 C40 122.2(3) . . ? N5 C41 H41 118.9 . . ? C40 C41 H41 118.9 . . ? C45 C42 C39 115.0(3) . . ? C45 C42 C44 111.3(3) . . ? C39 C42 C44 111.4(3) . . ? C45 C42 C43 103.2(3) . . ? C39 C42 C43 108.4(3) . . ? C44 C42 C43 106.9(3) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N6 C46 C47 122.7(3) . . ? N6 C46 H46 118.7 . . ? C47 C46 H46 118.7 . . ? C46 C47 C48 121.4(3) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.3 . . ? C49 C48 C47 113.8(3) . . ? C49 C48 C51 124.0(3) . . ? C47 C48 C51 122.2(3) . . ? C50 C49 C48 121.8(3) . . ? C50 C49 H49 119.1 . . ? C48 C49 H49 119.1 . . ? C49 C50 N6 125.0(3) . . ? C49 C50 H50 117.5 . . ? N6 C50 H50 117.5 . . ? C48 C51 C52 109.7(3) . . ? C48 C51 C53 107.4(3) . . ? C52 C51 C53 109.1(3) . . ? C48 C51 C54 112.8(3) . . ? C52 C51 C54 107.7(3) . . ? C53 C51 C54 110.2(3) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N1 C55 Ru1 175.3(2) . . ? N2 C56 Ru1 173.0(3) . . ? C58 C57 C62 114.8(3) . . ? C58 C57 B2 121.8(3) . . ? C62 C57 B2 123.0(3) . . ? C57 C58 C59 122.5(3) . . ? C57 C58 H58 118.7 . . ? C59 C58 H58 118.7 . . ? C60 C59 C58 119.6(4) . . ? C60 C59 H59 120.2 . . ? C58 C59 H59 120.2 . . ? C59 C60 C61 121.3(3) . . ? C59 C60 H60 119.3 . . ? C61 C60 H60 119.3 . . ? C60 C61 C62 118.7(3) . . ? C60 C61 H61 120.6 . . ? C62 C61 H61 120.6 . . ? C57 C62 C61 123.0(3) . . ? C57 C62 H62 118.5 . . ? C61 C62 H62 118.5 . . ? C68 C63 C64 115.4(3) . . ? C68 C63 B2 122.0(3) . . ? C64 C63 B2 122.5(3) . . ? C65 C64 C63 122.9(3) . . ? C65 C64 H64 118.6 . . ? C63 C64 H64 118.6 . . ? C66 C65 C64 120.3(3) . . ? C66 C65 H65 119.8 . . ? C64 C65 H65 119.8 . . ? C65 C66 C67 120.3(3) . . ? C65 C66 H66 119.9 . . ? C67 C66 H66 119.9 . . ? C66 C67 C68 118.2(3) . . ? C66 C67 H67 120.9 . . ? C68 C67 H67 120.9 . . ? C63 C68 C67 122.7(3) . . ? C63 C68 H68 118.7 . . ? C67 C68 H68 118.7 . . ? C70 C69 C74 120.0 . . ? C70 C69 B2 121.90(17) . . ? C74 C69 B2 118.09(17) . . ? C69 C70 C71 120.0 . . ? C69 C70 H70 120.0 . . ? C71 C70 H70 120.0 . . ? C72 C71 C70 120.0 . . ? C72 C71 H71 120.0 . . ? C70 C71 H71 120.0 . . ? C71 C72 C73 120.0 . . ? C71 C72 H72 120.0 . . ? C73 C72 H72 120.0 . . ? C72 C73 C74 120.0 . . ? C72 C73 H73 120.0 . . ? C74 C73 H73 120.0 . . ? C73 C74 C69 120.0 . . ? C73 C74 H74 120.0 . . ? C69 C74 H74 120.0 . . ? C55 N1 B1 168.3(3) . . ? C56 N2 B2 170.9(3) . . ? C23 N3 C19 115.1(3) . . ? C23 N3 Ru1 122.2(2) . . ? C19 N3 Ru1 122.42(19) . . ? C28 N4 C32 114.2(3) . . ? C28 N4 Ru1 122.7(2) . . ? C32 N4 Ru1 123.05(19) . . ? C37 N5 C41 116.2(3) . . ? C37 N5 Ru1 121.7(2) . . ? C41 N5 Ru1 122.1(2) . . ? C46 N6 C50 115.2(3) . . ? C46 N6 Ru1 122.6(2) . . ? C50 N6 Ru1 122.2(2) . . ? H1D O1 H1A 109.8 . . ? H2B O2 H2C 109.5 . . ? H3A O3 H3B 109.5 . . ? C55 Ru1 C56 177.04(12) . . ? C55 Ru1 N6 91.29(11) . . ? C56 Ru1 N6 91.61(12) . . ? C55 Ru1 N5 91.15(11) . . ? C56 Ru1 N5 88.29(12) . . ? N6 Ru1 N5 89.49(10) . . ? C55 Ru1 N3 89.17(11) . . ? C56 Ru1 N3 87.95(12) . . ? N6 Ru1 N3 178.36(9) . . ? N5 Ru1 N3 92.07(10) . . ? C55 Ru1 N4 90.48(11) . . ? C56 Ru1 N4 90.06(12) . . ? N6 Ru1 N4 90.89(10) . . ? N5 Ru1 N4 178.31(9) . . ? N3 Ru1 N4 87.53(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 B1 C1 C6 155.6(3) . . . . ? N1 B1 C1 C6 -88.2(4) . . . . ? C13 B1 C1 C6 27.0(4) . . . . ? C7 B1 C1 C2 -32.1(4) . . . . ? N1 B1 C1 C2 84.2(3) . . . . ? C13 B1 C1 C2 -160.6(3) . . . . ? C6 C1 C2 C3 -1.1(4) . . . . ? B1 C1 C2 C3 -174.0(3) . . . . ? C1 C2 C3 C4 3.1(5) . . . . ? C2 C3 C4 C5 -3.1(5) . . . . ? C3 C4 C5 C6 1.3(5) . . . . ? C2 C1 C6 C5 -0.7(5) . . . . ? B1 C1 C6 C5 172.0(3) . . . . ? C4 C5 C6 C1 0.7(5) . . . . ? C1 B1 C7 C8 -48.6(4) . . . . ? N1 B1 C7 C8 -162.4(3) . . . . ? C13 B1 C7 C8 80.5(4) . . . . ? C1 B1 C7 C12 136.3(3) . . . . ? N1 B1 C7 C12 22.5(4) . . . . ? C13 B1 C7 C12 -94.6(4) . . . . ? C12 C7 C8 C9 -0.5(5) . . . . ? B1 C7 C8 C9 -176.0(3) . . . . ? C7 C8 C9 C10 -1.7(6) . . . . ? C8 C9 C10 C11 1.4(6) . . . . ? C9 C10 C11 C12 1.1(6) . . . . ? C8 C7 C12 C11 3.0(5) . . . . ? B1 C7 C12 C11 178.5(3) . . . . ? C10 C11 C12 C7 -3.4(6) . . . . ? C1 B1 C13 C14 71.0(3) . . . . ? C7 B1 C13 C14 -59.1(3) . . . . ? N1 B1 C13 C14 -176.29(17) . . . . ? C1 B1 C13 C18 -113.6(2) . . . . ? C7 B1 C13 C18 116.4(2) . . . . ? N1 B1 C13 C18 -0.8(3) . . . . ? C18 C13 C14 C15 0.0 . . . . ? B1 C13 C14 C15 175.6(2) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? B1 C13 C18 C17 -175.4(2) . . . . ? N3 C19 C20 C21 0.4(5) . . . . ? C19 C20 C21 C22 -2.1(4) . . . . ? C19 C20 C21 C24 174.6(3) . . . . ? C20 C21 C22 C23 1.6(4) . . . . ? C24 C21 C22 C23 -175.1(3) . . . . ? C21 C22 C23 N3 0.7(5) . . . . ? C22 C21 C24 C27 -124.7(3) . . . . ? C20 C21 C24 C27 58.9(4) . . . . ? C22 C21 C24 C26 3.4(4) . . . . ? C20 C21 C24 C26 -173.0(3) . . . . ? C22 C21 C24 C25 115.9(3) . . . . ? C20 C21 C24 C25 -60.5(4) . . . . ? N4 C28 C29 C30 -0.6(5) . . . . ? C28 C29 C30 C31 -1.5(5) . . . . ? C28 C29 C30 C33 179.8(3) . . . . ? C29 C30 C31 C32 1.8(5) . . . . ? C33 C30 C31 C32 -179.6(3) . . . . ? C30 C31 C32 N4 0.0(6) . . . . ? C29 C30 C33 C35 -151.1(3) . . . . ? C31 C30 C33 C35 30.4(5) . . . . ? C29 C30 C33 C36 74.1(4) . . . . ? C31 C30 C33 C36 -104.4(4) . . . . ? C29 C30 C33 C34 -36.1(5) . . . . ? C31 C30 C33 C34 145.4(3) . . . . ? N5 C37 C38 C39 2.1(5) . . . . ? C37 C38 C39 C40 -2.3(5) . . . . ? C37 C38 C39 C42 179.4(3) . . . . ? C38 C39 C40 C41 2.1(6) . . . . ? C42 C39 C40 C41 -179.7(3) . . . . ? C39 C40 C41 N5 -1.4(6) . . . . ? C38 C39 C42 C45 -171.0(3) . . . . ? C40 C39 C42 C45 10.8(5) . . . . ? C38 C39 C42 C44 61.2(5) . . . . ? C40 C39 C42 C44 -117.0(4) . . . . ? C38 C39 C42 C43 -56.2(5) . . . . ? C40 C39 C42 C43 125.6(4) . . . . ? N6 C46 C47 C48 -4.1(5) . . . . ? C46 C47 C48 C49 3.0(5) . . . . ? C46 C47 C48 C51 -173.5(3) . . . . ? C47 C48 C49 C50 -1.1(5) . . . . ? C51 C48 C49 C50 175.4(3) . . . . ? C48 C49 C50 N6 -0.1(5) . . . . ? C49 C48 C51 C52 41.2(4) . . . . ? C47 C48 C51 C52 -142.5(3) . . . . ? C49 C48 C51 C53 -77.2(4) . . . . ? C47 C48 C51 C53 99.0(4) . . . . ? C49 C48 C51 C54 161.2(3) . . . . ? C47 C48 C51 C54 -22.6(4) . . . . ? N2 B2 C57 C58 82.1(4) . . . . ? C63 B2 C57 C58 -160.3(3) . . . . ? C69 B2 C57 C58 -33.4(4) . . . . ? N2 B2 C57 C62 -90.7(4) . . . . ? C63 B2 C57 C62 26.8(4) . . . . ? C69 B2 C57 C62 153.7(3) . . . . ? C62 C57 C58 C59 0.3(5) . . . . ? B2 C57 C58 C59 -173.1(3) . . . . ? C57 C58 C59 C60 -2.5(5) . . . . ? C58 C59 C60 C61 3.1(5) . . . . ? C59 C60 C61 C62 -1.6(5) . . . . ? C58 C57 C62 C61 1.3(5) . . . . ? B2 C57 C62 C61 174.6(3) . . . . ? C60 C61 C62 C57 -0.7(5) . . . . ? N2 B2 C63 C68 -26.0(4) . . . . ? C57 B2 C63 C68 -141.1(3) . . . . ? C69 B2 C63 C68 90.3(3) . . . . ? N2 B2 C63 C64 157.7(3) . . . . ? C57 B2 C63 C64 42.7(4) . . . . ? C69 B2 C63 C64 -86.0(4) . . . . ? C68 C63 C64 C65 -4.4(5) . . . . ? B2 C63 C64 C65 172.0(3) . . . . ? C63 C64 C65 C66 4.3(5) . . . . ? C64 C65 C66 C67 -1.1(5) . . . . ? C65 C66 C67 C68 -1.4(5) . . . . ? C64 C63 C68 C67 1.7(5) . . . . ? B2 C63 C68 C67 -174.8(3) . . . . ? C66 C67 C68 C63 1.1(5) . . . . ? N2 B2 C69 C70 -10.6(3) . . . . ? C63 B2 C69 C70 -127.4(2) . . . . ? C57 B2 C69 C70 102.9(3) . . . . ? N2 B2 C69 C74 168.42(17) . . . . ? C63 B2 C69 C74 51.6(3) . . . . ? C57 B2 C69 C74 -78.1(3) . . . . ? C74 C69 C70 C71 0.0 . . . . ? B2 C69 C70 C71 178.9(2) . . . . ? C69 C70 C71 C72 0.0 . . . . ? C70 C71 C72 C73 0.0 . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C69 0.0 . . . . ? C70 C69 C74 C73 0.0 . . . . ? B2 C69 C74 C73 -179.0(2) . . . . ? Ru1 C55 N1 B1 -17(4) . . . . ? C1 B1 N1 C55 -8.2(16) . . . . ? C7 B1 N1 C55 112.9(15) . . . . ? C13 B1 N1 C55 -127.2(14) . . . . ? Ru1 C56 N2 B2 17(4) . . . . ? C63 B2 N2 C56 -82.1(19) . . . . ? C57 B2 N2 C56 40(2) . . . . ? C69 B2 N2 C56 160.0(18) . . . . ? C22 C23 N3 C19 -2.4(4) . . . . ? C22 C23 N3 Ru1 171.9(2) . . . . ? C20 C19 N3 C23 1.8(4) . . . . ? C20 C19 N3 Ru1 -172.4(2) . . . . ? C29 C28 N4 C32 2.3(4) . . . . ? C29 C28 N4 Ru1 -177.7(2) . . . . ? C31 C32 N4 C28 -2.0(5) . . . . ? C31 C32 N4 Ru1 178.0(3) . . . . ? C38 C37 N5 C41 -1.3(5) . . . . ? C38 C37 N5 Ru1 179.6(3) . . . . ? C40 C41 N5 C37 1.0(5) . . . . ? C40 C41 N5 Ru1 -180.0(3) . . . . ? C47 C46 N6 C50 2.7(4) . . . . ? C47 C46 N6 Ru1 -178.8(2) . . . . ? C49 C50 N6 C46 -0.7(4) . . . . ? C49 C50 N6 Ru1 -179.2(2) . . . . ? N1 C55 Ru1 C56 -56(5) . . . . ? N1 C55 Ru1 N6 136(3) . . . . ? N1 C55 Ru1 N5 -135(3) . . . . ? N1 C55 Ru1 N3 -43(3) . . . . ? N1 C55 Ru1 N4 45(3) . . . . ? N2 C56 Ru1 C55 10(4) . . . . ? N2 C56 Ru1 N6 179(100) . . . . ? N2 C56 Ru1 N5 89(2) . . . . ? N2 C56 Ru1 N3 -3(2) . . . . ? N2 C56 Ru1 N4 -90(2) . . . . ? C46 N6 Ru1 C55 40.2(2) . . . . ? C50 N6 Ru1 C55 -141.4(2) . . . . ? C46 N6 Ru1 C56 -139.2(2) . . . . ? C50 N6 Ru1 C56 39.2(2) . . . . ? C46 N6 Ru1 N5 -50.9(2) . . . . ? C50 N6 Ru1 N5 127.5(2) . . . . ? C46 N6 Ru1 N3 147(3) . . . . ? C50 N6 Ru1 N3 -35(3) . . . . ? C46 N6 Ru1 N4 130.7(2) . . . . ? C50 N6 Ru1 N4 -50.9(2) . . . . ? C37 N5 Ru1 C55 -136.4(2) . . . . ? C41 N5 Ru1 C55 44.6(3) . . . . ? C37 N5 Ru1 C56 46.5(3) . . . . ? C41 N5 Ru1 C56 -132.5(3) . . . . ? C37 N5 Ru1 N6 -45.2(2) . . . . ? C41 N5 Ru1 N6 135.9(3) . . . . ? C37 N5 Ru1 N3 134.3(2) . . . . ? C41 N5 Ru1 N3 -44.6(3) . . . . ? C37 N5 Ru1 N4 58(3) . . . . ? C41 N5 Ru1 N4 -121(3) . . . . ? C23 N3 Ru1 C55 43.3(2) . . . . ? C19 N3 Ru1 C55 -142.9(2) . . . . ? C23 N3 Ru1 C56 -137.4(3) . . . . ? C19 N3 Ru1 C56 36.5(2) . . . . ? C23 N3 Ru1 N6 -63(3) . . . . ? C19 N3 Ru1 N6 111(3) . . . . ? C23 N3 Ru1 N5 134.4(2) . . . . ? C19 N3 Ru1 N5 -51.7(2) . . . . ? C23 N3 Ru1 N4 -47.2(2) . . . . ? C19 N3 Ru1 N4 126.6(2) . . . . ? C28 N4 Ru1 C55 -146.8(3) . . . . ? C32 N4 Ru1 C55 33.1(3) . . . . ? C28 N4 Ru1 C56 30.2(3) . . . . ? C32 N4 Ru1 C56 -149.8(3) . . . . ? C28 N4 Ru1 N6 121.9(2) . . . . ? C32 N4 Ru1 N6 -58.2(3) . . . . ? C28 N4 Ru1 N5 19(3) . . . . ? C32 N4 Ru1 N5 -161(3) . . . . ? C28 N4 Ru1 N3 -57.7(2) . . . . ? C32 N4 Ru1 N3 122.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.251 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.052 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 739896' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H46 B2 N6 Ru' _chemical_formula_sum 'C58 H46 B2 N6 Ru' _chemical_formula_weight 949.70 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' Ru Ru -1.2594 0.8363 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.138(14) _cell_length_b 19.056(16) _cell_length_c 17.050(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.02(3) _cell_angle_gamma 90.00 _cell_volume 4986(7) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2794 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 25.31 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 0.358 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9482 _exptl_absorpt_correction_T_max 0.9515 _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart apex II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13240 _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_sigmaI/netI 0.1282 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4867 _reflns_number_gt 2917 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL(Bruker, 2002)' _computing_publication_material 'SHELXTL(Bruker, 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. ; _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^)+(0.0198P)^2] 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 4867 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.0963 _refine_ls_wR_factor_gt 0.0854 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.859 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.5000 0.15457(2) 0.7500 0.04326(16) Uani 1 2 d S . . B1 B 0.2847(3) -0.0061(3) 0.6129(3) 0.0496(13) Uani 1 1 d . . . C1 C 0.3507(3) 0.2633(2) 0.7170(3) 0.0768(16) Uani 1 1 d . . . H1 H 0.3497 0.2526 0.7700 0.092 Uiso 1 1 calc R . . C2 C 0.2911(4) 0.3108(3) 0.6718(4) 0.108(2) Uani 1 1 d . . . H2 H 0.2511 0.3319 0.6937 0.130 Uiso 1 1 calc R . . C3 C 0.2918(4) 0.3264(3) 0.5937(4) 0.126(3) Uani 1 1 d . . . H3 H 0.2515 0.3577 0.5611 0.151 Uiso 1 1 calc R . . C4 C 0.3530(4) 0.2953(3) 0.5641(3) 0.103(2) Uani 1 1 d . . . H4 H 0.3553 0.3063 0.5117 0.124 Uiso 1 1 calc R . . C5 C 0.4111(3) 0.2473(2) 0.6127(3) 0.0663(14) Uani 1 1 d . . . C6 C 0.4775(3) 0.2107(2) 0.5855(3) 0.0572(12) Uani 1 1 d . . . C7 C 0.4908(3) 0.2219(3) 0.5094(3) 0.0886(17) Uani 1 1 d . . . H7 H 0.4564 0.2539 0.4723 0.106 Uiso 1 1 calc R . . C8 C 0.5548(3) 0.1856(3) 0.4898(3) 0.0833(17) Uani 1 1 d . . . H8 H 0.5636 0.1924 0.4390 0.100 Uiso 1 1 calc R . . C9 C 0.6053(3) 0.1398(2) 0.5447(3) 0.0678(14) Uani 1 1 d . . . H9 H 0.6499 0.1153 0.5330 0.081 Uiso 1 1 calc R . . C10 C 0.5885(3) 0.1306(2) 0.6187(3) 0.0569(12) Uani 1 1 d . . . H10 H 0.6226 0.0985 0.6561 0.068 Uiso 1 1 calc R . . C11 C 0.4142(3) 0.0822(2) 0.7016(3) 0.0438(11) Uani 1 1 d . . . C12 C 0.1844(3) 0.0947(3) 0.6384(3) 0.0868(17) Uani 1 1 d . . . H12 H 0.2298 0.1251 0.6395 0.104 Uiso 1 1 calc R . . C13 C 0.1072(5) 0.1228(4) 0.6479(4) 0.109(2) Uani 1 1 d . . . H13 H 0.1027 0.1708 0.6557 0.131 Uiso 1 1 calc R . . C14 C 0.0399(5) 0.0800(5) 0.6456(4) 0.134(3) Uani 1 1 d . . . H14 H -0.0116 0.0985 0.6505 0.161 Uiso 1 1 calc R . . C15 C 0.0477(4) 0.0101(4) 0.6362(4) 0.130(3) Uani 1 1 d . . . H15 H 0.0017 -0.0196 0.6353 0.157 Uiso 1 1 calc R . . C16 C 0.1245(3) -0.0177(3) 0.6278(3) 0.0973(19) Uani 1 1 d . . . H16 H 0.1288 -0.0660 0.6222 0.117 Uiso 1 1 calc R . . C17 C 0.1949(3) 0.0244(3) 0.6275(3) 0.0617(13) Uani 1 1 d . . . C18 C 0.3710(3) -0.1101(2) 0.7073(3) 0.0610(13) Uani 1 1 d . . . H18 H 0.4070 -0.0768 0.7410 0.073 Uiso 1 1 calc R . . C19 C 0.3858(4) -0.1802(3) 0.7280(4) 0.0829(17) Uani 1 1 d . . . H19 H 0.4308 -0.1929 0.7748 0.100 Uiso 1 1 calc R . . C20 C 0.3348(5) -0.2307(3) 0.6801(4) 0.099(2) Uani 1 1 d . . . H20 H 0.3448 -0.2779 0.6936 0.119 Uiso 1 1 calc R . . C21 C 0.2692(4) -0.2108(3) 0.6123(4) 0.096(2) Uani 1 1 d . . . H21 H 0.2337 -0.2448 0.5794 0.115 Uiso 1 1 calc R . . C22 C 0.2545(3) -0.1411(3) 0.5915(3) 0.0757(15) Uani 1 1 d . . . H22 H 0.2094 -0.1295 0.5443 0.091 Uiso 1 1 calc R . . C23 C 0.3046(3) -0.0872(2) 0.6385(3) 0.0502(11) Uani 1 1 d . . . C24 C 0.3573(3) 0.0300(2) 0.4982(3) 0.0554(12) Uani 1 1 d . . . H24 H 0.4078 0.0412 0.5404 0.067 Uiso 1 1 calc R . . C25 C 0.3569(3) 0.0366(2) 0.4163(3) 0.0622(13) Uani 1 1 d . . . H25 H 0.4062 0.0529 0.4049 0.075 Uiso 1 1 calc R . . C26 C 0.2843(4) 0.0193(2) 0.3533(3) 0.0718(15) Uani 1 1 d . . . H26 H 0.2842 0.0232 0.2989 0.086 Uiso 1 1 calc R . . C27 C 0.2108(3) -0.0041(3) 0.3705(3) 0.0834(16) Uani 1 1 d . . . H27 H 0.1613 -0.0166 0.3278 0.100 Uiso 1 1 calc R . . C28 C 0.2114(3) -0.0089(2) 0.4522(3) 0.0732(14) Uani 1 1 d . . . H28 H 0.1609 -0.0234 0.4629 0.088 Uiso 1 1 calc R . . C29 C 0.2843(3) 0.0072(2) 0.5184(3) 0.0504(11) Uani 1 1 d . . . N1 N 0.4102(2) 0.23121(17) 0.6895(2) 0.0580(10) Uani 1 1 d . . . N2 N 0.5271(2) 0.16439(16) 0.63998(19) 0.0448(8) Uani 1 1 d . . . N3 N 0.3619(2) 0.04050(17) 0.6697(2) 0.0496(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0529(3) 0.0402(3) 0.0411(3) 0.000 0.0210(2) 0.000 B1 0.041(3) 0.068(4) 0.040(3) -0.005(3) 0.012(3) -0.006(3) C1 0.099(4) 0.067(3) 0.080(4) 0.016(3) 0.051(4) 0.032(3) C2 0.131(5) 0.100(4) 0.119(6) 0.036(4) 0.074(5) 0.069(4) C3 0.150(6) 0.132(6) 0.114(6) 0.061(5) 0.067(5) 0.089(5) C4 0.132(5) 0.114(4) 0.081(5) 0.041(4) 0.058(4) 0.063(4) C5 0.082(4) 0.062(3) 0.063(4) 0.016(3) 0.034(3) 0.026(3) C6 0.072(3) 0.060(3) 0.047(3) 0.009(2) 0.029(3) 0.011(3) C7 0.103(4) 0.106(4) 0.069(4) 0.032(3) 0.045(4) 0.036(3) C8 0.102(5) 0.108(4) 0.058(4) 0.009(3) 0.050(4) 0.007(3) C9 0.075(4) 0.069(4) 0.074(4) -0.007(3) 0.045(3) 0.003(3) C10 0.070(3) 0.053(3) 0.057(3) 0.000(2) 0.032(3) 0.006(2) C11 0.047(3) 0.051(3) 0.038(3) 0.002(2) 0.019(2) 0.003(2) C12 0.083(4) 0.106(5) 0.073(4) 0.004(3) 0.026(3) 0.026(4) C13 0.106(5) 0.140(6) 0.078(5) 0.001(4) 0.025(5) 0.063(5) C14 0.074(5) 0.239(10) 0.091(6) -0.020(7) 0.028(5) 0.055(7) C15 0.066(5) 0.204(8) 0.131(7) -0.027(6) 0.044(4) 0.008(5) C16 0.056(4) 0.136(5) 0.102(5) -0.014(4) 0.029(4) -0.005(4) C17 0.055(3) 0.089(4) 0.036(3) -0.006(3) 0.007(2) 0.001(3) C18 0.063(3) 0.069(3) 0.056(4) 0.001(3) 0.026(3) -0.009(3) C19 0.099(5) 0.079(4) 0.078(5) 0.022(3) 0.038(4) 0.010(3) C20 0.152(7) 0.071(4) 0.095(6) 0.007(4) 0.067(5) -0.012(4) C21 0.133(6) 0.081(4) 0.090(5) -0.020(4) 0.059(5) -0.047(4) C22 0.084(4) 0.087(4) 0.061(4) -0.005(3) 0.029(3) -0.024(3) C23 0.049(3) 0.066(3) 0.041(3) -0.009(3) 0.022(2) -0.017(2) C24 0.060(3) 0.055(3) 0.052(3) -0.001(2) 0.019(3) 0.005(2) C25 0.070(3) 0.068(3) 0.055(4) 0.002(3) 0.030(3) 0.006(3) C26 0.094(4) 0.082(4) 0.043(3) 0.005(3) 0.027(3) 0.017(3) C27 0.071(4) 0.125(5) 0.045(4) -0.005(3) 0.006(3) 0.003(3) C28 0.057(3) 0.114(4) 0.047(3) -0.001(3) 0.014(3) -0.001(3) C29 0.040(3) 0.062(3) 0.046(3) 0.000(2) 0.009(2) 0.005(2) N1 0.074(3) 0.050(2) 0.060(3) 0.012(2) 0.036(2) 0.0189(19) N2 0.055(2) 0.043(2) 0.044(2) 0.0017(18) 0.0254(19) 0.0057(17) N3 0.050(2) 0.058(2) 0.041(2) 0.0018(19) 0.015(2) 0.0036(19) _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 C11 1.948(4) . ? Ru1 C11 1.948(4) 2_656 ? Ru1 N2 2.062(3) . ? Ru1 N2 2.062(3) 2_656 ? Ru1 N1 2.091(4) 2_656 ? Ru1 N1 2.091(3) . ? B1 N3 1.591(6) . ? B1 C23 1.610(6) . ? B1 C29 1.629(6) . ? B1 C17 1.650(6) . ? C1 N1 1.341(5) . ? C1 C2 1.371(6) . ? C1 H1 0.9300 . ? C2 C3 1.369(7) . ? C2 H2 0.9300 . ? C3 C4 1.375(6) . ? C3 H3 0.9300 . ? C4 C5 1.387(6) . ? C4 H4 0.9300 . ? C5 N1 1.349(5) . ? C5 C6 1.468(6) . ? C6 N2 1.349(5) . ? C6 C7 1.395(6) . ? C7 C8 1.367(6) . ? C7 H7 0.9300 . ? C8 C9 1.353(6) . ? C8 H8 0.9300 . ? C9 C10 1.381(6) . ? C9 H9 0.9300 . ? C10 N2 1.323(4) . ? C10 H10 0.9300 . ? C11 N3 1.164(4) . ? C12 C17 1.371(6) . ? C12 C13 1.410(6) . ? C12 H12 0.9300 . ? C13 C14 1.349(8) . ? C13 H13 0.9300 . ? C14 C15 1.352(8) . ? C14 H14 0.9300 . ? C15 C16 1.396(7) . ? C15 H15 0.9300 . ? C16 C17 1.392(6) . ? C16 H16 0.9300 . ? C18 C19 1.383(6) . ? C18 C23 1.392(5) . ? C18 H18 0.9300 . ? C19 C20 1.361(7) . ? C19 H19 0.9300 . ? C20 C21 1.358(7) . ? C20 H20 0.9300 . ? C21 C22 1.376(7) . ? C21 H21 0.9300 . ? C22 C23 1.396(5) . ? C22 H22 0.9300 . ? C24 C29 1.395(5) . ? C24 C25 1.399(6) . ? C24 H24 0.9300 . ? C25 C26 1.363(6) . ? C25 H25 0.9300 . ? C26 C27 1.380(6) . ? C26 H26 0.9300 . ? C27 C28 1.393(6) . ? C27 H27 0.9300 . ? C28 C29 1.389(5) . ? C28 H28 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Ru1 C11 89.8(2) . 2_656 ? C11 Ru1 N2 90.10(14) . . ? C11 Ru1 N2 97.28(15) 2_656 . ? C11 Ru1 N2 97.28(15) . 2_656 ? C11 Ru1 N2 90.10(14) 2_656 2_656 ? N2 Ru1 N2 169.59(17) . 2_656 ? C11 Ru1 N1 175.52(16) . 2_656 ? C11 Ru1 N1 89.57(15) 2_656 2_656 ? N2 Ru1 N1 94.38(14) . 2_656 ? N2 Ru1 N1 78.28(14) 2_656 2_656 ? C11 Ru1 N1 89.57(15) . . ? C11 Ru1 N1 175.52(16) 2_656 . ? N2 Ru1 N1 78.28(14) . . ? N2 Ru1 N1 94.38(14) 2_656 . ? N1 Ru1 N1 91.4(2) 2_656 . ? N3 B1 C23 108.6(4) . . ? N3 B1 C29 106.1(3) . . ? C23 B1 C29 110.9(4) . . ? N3 B1 C17 105.7(4) . . ? C23 B1 C17 114.1(4) . . ? C29 B1 C17 111.0(4) . . ? N1 C1 C2 123.9(5) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 118.4(5) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.1(5) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.8(5) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 121.4(4) . . ? N1 C5 C6 115.2(4) . . ? C4 C5 C6 123.4(5) . . ? N2 C6 C7 120.8(4) . . ? N2 C6 C5 115.3(4) . . ? C7 C6 C5 123.9(4) . . ? C8 C7 C6 119.6(5) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C9 C8 C7 119.8(5) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 117.8(4) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? N2 C10 C9 124.3(4) . . ? N2 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? N3 C11 Ru1 177.2(4) . . ? C17 C12 C13 122.5(6) . . ? C17 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? C14 C13 C12 120.0(7) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 119.6(8) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 120.3(7) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 122.2(6) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C12 C17 C16 115.3(5) . . ? C12 C17 B1 121.1(5) . . ? C16 C17 B1 123.6(5) . . ? C19 C18 C23 123.0(5) . . ? C19 C18 H18 118.5 . . ? C23 C18 H18 118.5 . . ? C20 C19 C18 120.3(6) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 118.7(6) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C20 C21 C22 121.1(6) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C23 122.6(5) . . ? C21 C22 H22 118.7 . . ? C23 C22 H22 118.7 . . ? C18 C23 C22 114.2(4) . . ? C18 C23 B1 124.5(4) . . ? C22 C23 B1 121.3(4) . . ? C29 C24 C25 122.1(4) . . ? C29 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C26 C25 C24 120.1(5) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 119.8(5) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C28 119.5(5) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C29 C28 C27 122.7(5) . . ? C29 C28 H28 118.7 . . ? C27 C28 H28 118.7 . . ? C28 C29 C24 115.8(4) . . ? C28 C29 B1 120.8(4) . . ? C24 C29 B1 123.2(4) . . ? C1 N1 C5 117.5(4) . . ? C1 N1 Ru1 127.4(3) . . ? C5 N1 Ru1 115.1(3) . . ? C10 N2 C6 117.7(4) . . ? C10 N2 Ru1 126.3(3) . . ? C6 N2 Ru1 116.0(3) . . ? C11 N3 B1 169.5(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.677 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.058 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 739897' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H48 B2 Fe N6 O' _chemical_formula_weight 970.53 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.906(2) _cell_length_b 19.420(3) _cell_length_c 17.408(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.392(3) _cell_angle_gamma 90.00 _cell_volume 5131.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 986 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 22.6 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9504 _exptl_absorpt_correction_T_max 0.9536 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart apex II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13712 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5042 _reflns_number_gt 3802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+1.9900P] 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 5042 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1419 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.2134(2) 0.50634(17) 0.8859(2) 0.0373(7) Uani 1 1 d . . . C1 C 0.1435(2) 0.46406(15) 0.99766(19) 0.0423(7) Uani 1 1 d . . . H1 H 0.0924 0.4541 0.9563 0.051 Uiso 1 1 calc R . . C2 C 0.14391(19) 0.45302(14) 1.07600(17) 0.0371(6) Uani 1 1 d . . . H2 H 0.0946 0.4344 1.0864 0.044 Uiso 1 1 calc R . . C3 C 0.21738(18) 0.46948(15) 1.13897(18) 0.0391(7) Uani 1 1 d . . . H3 H 0.2169 0.4644 1.1920 0.047 Uiso 1 1 calc R . . C4 C 0.2910(2) 0.49349(15) 1.12221(18) 0.0436(7) Uani 1 1 d . . . H4 H 0.3418 0.5034 1.1638 0.052 Uiso 1 1 calc R . . C5 C 0.2892(2) 0.50284(16) 1.04319(18) 0.0429(7) Uani 1 1 d . . . H5 H 0.3400 0.5190 1.0332 0.051 Uiso 1 1 calc R . . C6 C 0.21607(19) 0.48950(16) 0.97775(18) 0.0406(7) Uani 1 1 d . . . C7 C 0.19256(19) 0.58849(15) 0.86427(17) 0.0370(6) Uani 1 1 d . . . C8 C 0.2402(2) 0.63954(15) 0.91369(19) 0.0444(7) Uani 1 1 d . . . H8 H 0.2817 0.6263 0.9615 0.053 Uiso 1 1 calc R . . C9 C 0.2301(2) 0.70911(16) 0.8965(2) 0.0453(7) Uani 1 1 d . . . H9 H 0.2655 0.7415 0.9306 0.054 Uiso 1 1 calc R . . C10 C 0.1670(2) 0.72899(16) 0.8281(2) 0.0447(7) Uani 1 1 d . . . H10 H 0.1581 0.7756 0.8160 0.054 Uiso 1 1 calc R . . C11 C 0.1166(2) 0.68121(15) 0.77716(19) 0.0436(7) Uani 1 1 d . . . H11 H 0.0739 0.6950 0.7304 0.052 Uiso 1 1 calc R . . C12 C 0.12976(19) 0.61158(15) 0.79594(19) 0.0426(7) Uani 1 1 d . . . H12 H 0.0949 0.5794 0.7611 0.051 Uiso 1 1 calc R . . C13 C 0.30508(10) 0.48255(9) 0.86425(12) 0.0376(6) Uani 1 1 d G . . C14 C 0.37762(12) 0.52620(7) 0.88197(13) 0.0425(7) Uani 1 1 d G . . H14 H 0.3739 0.5700 0.9023 0.051 Uiso 1 1 calc R . . C15 C 0.45567(10) 0.50434(9) 0.86938(12) 0.0448(7) Uani 1 1 d G . . H15 H 0.5042 0.5335 0.8812 0.054 Uiso 1 1 calc R . . C16 C 0.46118(10) 0.43884(10) 0.83907(13) 0.0440(7) Uani 1 1 d G . . H16 H 0.5134 0.4242 0.8306 0.053 Uiso 1 1 calc R . . C17 C 0.38864(12) 0.39519(7) 0.82135(12) 0.0448(7) Uani 1 1 d G . . H17 H 0.3923 0.3514 0.8011 0.054 Uiso 1 1 calc R . . C18 C 0.31059(10) 0.41705(8) 0.83394(11) 0.0389(6) Uani 1 1 d G . . H18 H 0.2621 0.3878 0.8221 0.047 Uiso 1 1 calc R . . C19 C 0.08422(18) 0.42405(14) 0.79693(17) 0.0363(6) Uani 1 1 d . . . C20 C -0.0942(2) 0.38265(17) 0.87239(19) 0.0456(7) Uani 1 1 d . . . H20 H -0.1275 0.4153 0.8372 0.055 Uiso 1 1 calc R . . C21 C -0.1111(2) 0.37135(16) 0.94576(19) 0.0450(7) Uani 1 1 d . . . H21 H -0.1550 0.3961 0.9588 0.054 Uiso 1 1 calc R . . C22 C -0.0632(2) 0.32442(16) 0.99709(19) 0.0449(7) Uani 1 1 d . . . H22 H -0.0738 0.3168 1.0462 0.054 Uiso 1 1 calc R . . C23 C 0.0029(2) 0.28652(15) 0.97707(18) 0.0410(7) Uani 1 1 d . . . C24 C 0.0545(2) 0.23384(15) 1.02467(19) 0.0416(7) Uani 1 1 d . . . H24 H 0.0452 0.2216 1.0731 0.050 Uiso 1 1 calc R . . C25 C 0.1172(2) 0.20103(18) 1.0005(2) 0.0528(8) Uani 1 1 d . . . H25 H 0.1518 0.1679 1.0340 0.063 Uiso 1 1 calc R . . C26 C 0.1318(2) 0.21548(15) 0.92614(19) 0.0431(7) Uani 1 1 d . . . C27 C 0.19438(19) 0.18289(15) 0.89673(19) 0.0434(7) Uani 1 1 d . . . H27 H 0.2310 0.1491 0.9271 0.052 Uiso 1 1 calc R . . C28 C 0.2013(2) 0.20096(14) 0.82349(19) 0.0416(7) Uani 1 1 d . . . H28 H 0.2429 0.1798 0.8035 0.050 Uiso 1 1 calc R . . C29 C 0.14650(19) 0.25052(15) 0.77928(19) 0.0413(7) Uani 1 1 d . . . H29 H 0.1526 0.2623 0.7294 0.050 Uiso 1 1 calc R . . C30 C 0.0805(2) 0.26504(16) 0.87707(19) 0.0463(7) Uani 1 1 d . . . C31 C 0.01565(18) 0.30083(14) 0.90244(17) 0.0363(6) Uani 1 1 d . . . Fe1 Fe 0.0000 0.35583(2) 0.7500 0.02755(16) Uani 1 2 d S . . N1 N 0.13558(16) 0.46319(13) 0.82868(14) 0.0393(6) Uani 1 1 d . . . N2 N 0.08582(16) 0.28248(12) 0.80309(15) 0.0398(6) Uani 1 1 d . . . N3 N -0.03160(16) 0.34815(12) 0.85092(14) 0.0361(5) Uani 1 1 d . . . O1 O 0.5181(3) 0.6175(2) 0.7713(3) 0.0551(13) Uani 0.50 1 d P . . H1D H 0.5458 0.6308 0.7463 0.066 Uiso 0.50 1 d PR . . H1C H 0.4718 0.6423 0.7711 0.066 Uiso 0.50 1 d 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 B1 0.0322(16) 0.0420(17) 0.0364(18) 0.0088(14) 0.0084(13) 0.0002(14) C1 0.0405(16) 0.0456(16) 0.0420(17) 0.0053(13) 0.0144(13) -0.0029(13) C2 0.0384(15) 0.0370(14) 0.0387(16) -0.0029(12) 0.0161(12) -0.0030(12) C3 0.0407(16) 0.0416(15) 0.0339(15) -0.0020(12) 0.0093(13) -0.0058(13) C4 0.0408(16) 0.0446(16) 0.0395(18) 0.0007(13) 0.0029(13) -0.0087(14) C5 0.0400(16) 0.0455(16) 0.0410(17) 0.0035(13) 0.0086(13) -0.0012(13) C6 0.0393(16) 0.0474(16) 0.0362(16) 0.0076(13) 0.0130(12) -0.0005(13) C7 0.0419(16) 0.0406(15) 0.0305(14) 0.0036(12) 0.0138(12) 0.0051(12) C8 0.0462(17) 0.0439(16) 0.0441(17) -0.0019(14) 0.0149(14) 0.0109(14) C9 0.0468(17) 0.0442(16) 0.0462(18) -0.0116(14) 0.0157(14) -0.0039(14) C10 0.0498(18) 0.0426(16) 0.0473(18) -0.0060(14) 0.0232(15) 0.0127(14) C11 0.0420(17) 0.0429(16) 0.0441(17) 0.0076(13) 0.0102(14) 0.0096(13) C12 0.0383(16) 0.0437(16) 0.0462(18) 0.0011(13) 0.0134(13) 0.0154(13) C13 0.0441(16) 0.0422(15) 0.0310(15) 0.0026(12) 0.0179(12) 0.0004(13) C14 0.0346(15) 0.0430(15) 0.0450(18) 0.0045(13) 0.0044(13) 0.0081(13) C15 0.0410(17) 0.0466(17) 0.0480(18) 0.0056(14) 0.0153(14) -0.0054(13) C16 0.0468(18) 0.0525(18) 0.0308(15) 0.0052(13) 0.0087(13) 0.0115(14) C17 0.0477(18) 0.0390(15) 0.0394(17) 0.0003(12) 0.0002(14) 0.0187(14) C18 0.0470(17) 0.0338(14) 0.0373(15) 0.0113(12) 0.0148(13) -0.0012(13) C19 0.0336(15) 0.0379(14) 0.0351(15) 0.0026(12) 0.0068(12) -0.0021(12) C20 0.0506(18) 0.0471(17) 0.0394(17) -0.0033(13) 0.0138(14) 0.0132(14) C21 0.0413(16) 0.0494(17) 0.0475(18) -0.0016(14) 0.0181(14) -0.0033(14) C22 0.0403(17) 0.0515(18) 0.0463(18) 0.0003(15) 0.0178(14) -0.0052(14) C23 0.0442(17) 0.0411(15) 0.0370(16) -0.0106(13) 0.0113(13) -0.0092(13) C24 0.0466(17) 0.0372(15) 0.0383(16) -0.0082(12) 0.0085(13) -0.0090(13) C25 0.055(2) 0.056(2) 0.0413(18) 0.0018(15) 0.0052(15) 0.0184(17) C26 0.0463(17) 0.0373(15) 0.0432(18) -0.0049(13) 0.0095(14) -0.0032(13) C27 0.0338(16) 0.0408(16) 0.0492(18) 0.0009(14) 0.0030(13) -0.0047(12) C28 0.0409(16) 0.0358(15) 0.0487(18) -0.0141(13) 0.0143(13) -0.0036(13) C29 0.0338(15) 0.0441(16) 0.0437(18) -0.0078(13) 0.0080(13) -0.0072(13) C30 0.0532(19) 0.0493(17) 0.0343(17) -0.0012(14) 0.0098(14) 0.0134(15) C31 0.0363(15) 0.0392(14) 0.0347(15) 0.0000(12) 0.0127(12) -0.0032(12) Fe1 0.0325(3) 0.0240(3) 0.0282(3) 0.000 0.0121(2) 0.000 N1 0.0399(13) 0.0464(14) 0.0342(13) -0.0032(11) 0.0149(11) -0.0061(12) N2 0.0404(13) 0.0387(12) 0.0432(15) 0.0086(11) 0.0170(11) 0.0091(11) N3 0.0429(13) 0.0358(12) 0.0309(12) -0.0010(9) 0.0132(10) 0.0001(10) O1 0.030(3) 0.055(2) 0.070(5) 0.004(2) -0.002(2) -0.0094(19) _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 B1 N1 1.578(4) . ? B1 C6 1.620(4) . ? B1 C7 1.650(4) . ? B1 C13 1.677(3) . ? C1 C2 1.378(4) . ? C1 C6 1.392(4) . ? C1 H1 0.9300 . ? C2 C3 1.380(4) . ? C2 H2 0.9300 . ? C3 C4 1.370(4) . ? C3 H3 0.9300 . ? C4 C5 1.379(4) . ? C4 H4 0.9300 . ? C5 C6 1.388(4) . ? C5 H5 0.9300 . ? C7 C12 1.380(4) . ? C7 C8 1.381(4) . ? C8 C9 1.383(4) . ? C8 H8 0.9300 . ? C9 C10 1.365(4) . ? C9 H9 0.9300 . ? C10 C11 1.365(4) . ? C10 H10 0.9300 . ? C11 C12 1.392(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 H16 0.9300 . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 N1 1.132(3) . ? C19 Fe1 1.888(3) . ? C20 N3 1.342(4) . ? C20 C21 1.399(4) . ? C20 H20 0.9300 . ? C21 C22 1.342(4) . ? C21 H21 0.9300 . ? C22 C23 1.411(4) . ? C22 H22 0.9300 . ? C23 C31 1.401(4) . ? C23 C24 1.414(4) . ? C24 C25 1.352(4) . ? C24 H24 0.9300 . ? C25 C26 1.410(5) . ? C25 H25 0.9300 . ? C26 C30 1.380(4) . ? C26 C27 1.400(4) . ? C27 C28 1.358(4) . ? C27 H27 0.9300 . ? C28 C29 1.370(4) . ? C28 H28 0.9300 . ? C29 N2 1.314(4) . ? C29 H29 0.9300 . ? C30 N2 1.358(4) . ? C30 C31 1.419(4) . ? C31 N3 1.346(4) . ? Fe1 C19 1.888(3) 2_556 ? Fe1 N3 1.972(2) . ? Fe1 N3 1.972(2) 2_556 ? Fe1 N2 1.998(2) 2_556 ? Fe1 N2 1.998(2) . ? O1 O1 0.791(8) 2_656 ? O1 H1D 0.7524 . ? O1 H1C 0.8792 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 B1 C6 107.5(2) . . ? N1 B1 C7 107.7(2) . . ? C6 B1 C7 111.4(2) . . ? N1 B1 C13 106.4(2) . . ? C6 B1 C13 113.5(2) . . ? C7 B1 C13 110.1(2) . . ? C2 C1 C6 122.8(3) . . ? C2 C1 H1 118.6 . . ? C6 C1 H1 118.6 . . ? C1 C2 C3 120.2(3) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 119.0(3) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.5(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 123.8(3) . . ? C4 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C5 C6 C1 114.6(3) . . ? C5 C6 B1 122.8(3) . . ? C1 C6 B1 122.6(3) . . ? C12 C7 C8 115.1(3) . . ? C12 C7 B1 123.7(3) . . ? C8 C7 B1 121.1(3) . . ? C7 C8 C9 124.0(3) . . ? C7 C8 H8 118.0 . . ? C9 C8 H8 118.0 . . ? C10 C9 C8 118.2(3) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C9 C10 C11 120.7(3) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C12 119.3(3) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C7 C12 C11 122.5(3) . . ? C7 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C14 C13 C18 120.0 . . ? C14 C13 B1 120.15(15) . . ? C18 C13 B1 119.69(15) . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? N1 C19 Fe1 176.5(3) . . ? N3 C20 C21 122.5(3) . . ? N3 C20 H20 118.8 . . ? C21 C20 H20 118.8 . . ? C22 C21 C20 119.3(3) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 120.4(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C31 C23 C22 116.8(3) . . ? C31 C23 C24 117.9(3) . . ? C22 C23 C24 125.3(3) . . ? C25 C24 C23 120.8(3) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 122.0(3) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C30 C26 C27 116.2(3) . . ? C30 C26 C25 118.6(3) . . ? C27 C26 C25 125.2(3) . . ? C28 C27 C26 119.5(3) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 119.5(3) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? N2 C29 C28 123.9(3) . . ? N2 C29 H29 118.0 . . ? C28 C29 H29 118.0 . . ? N2 C30 C26 124.6(3) . . ? N2 C30 C31 115.5(3) . . ? C26 C30 C31 119.9(3) . . ? N3 C31 C23 123.2(3) . . ? N3 C31 C30 116.1(3) . . ? C23 C31 C30 120.7(3) . . ? C19 Fe1 C19 90.84(17) . 2_556 ? C19 Fe1 N3 90.26(11) . . ? C19 Fe1 N3 95.84(11) 2_556 . ? C19 Fe1 N3 95.84(11) . 2_556 ? C19 Fe1 N3 90.26(11) 2_556 2_556 ? N3 Fe1 N3 171.32(13) . 2_556 ? C19 Fe1 N2 177.33(11) . 2_556 ? C19 Fe1 N2 90.10(11) 2_556 2_556 ? N3 Fe1 N2 92.14(10) . 2_556 ? N3 Fe1 N2 81.65(10) 2_556 2_556 ? C19 Fe1 N2 90.10(11) . . ? C19 Fe1 N2 177.33(11) 2_556 . ? N3 Fe1 N2 81.65(10) . . ? N3 Fe1 N2 92.14(10) 2_556 . ? N2 Fe1 N2 89.06(15) 2_556 . ? C19 N1 B1 168.7(3) . . ? C29 N2 C30 116.2(3) . . ? C29 N2 Fe1 130.9(2) . . ? C30 N2 Fe1 112.88(18) . . ? C20 N3 C31 117.9(3) . . ? C20 N3 Fe1 128.2(2) . . ? C31 N3 Fe1 113.90(18) . . ? O1 O1 H1D 81.0 2_656 . ? O1 O1 H1C 67.9 2_656 . ? H1D O1 H1C 116.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 2.3(5) . . . . ? C1 C2 C3 C4 -3.3(4) . . . . ? C2 C3 C4 C5 2.1(5) . . . . ? C3 C4 C5 C6 0.2(5) . . . . ? C4 C5 C6 C1 -1.3(5) . . . . ? C4 C5 C6 B1 175.3(3) . . . . ? C2 C1 C6 C5 0.1(4) . . . . ? C2 C1 C6 B1 -176.5(3) . . . . ? N1 B1 C6 C5 161.7(3) . . . . ? C7 B1 C6 C5 -80.5(4) . . . . ? C13 B1 C6 C5 44.4(4) . . . . ? N1 B1 C6 C1 -22.0(4) . . . . ? C7 B1 C6 C1 95.8(3) . . . . ? C13 B1 C6 C1 -139.3(3) . . . . ? N1 B1 C7 C12 -13.8(4) . . . . ? C6 B1 C7 C12 -131.5(3) . . . . ? C13 B1 C7 C12 101.8(3) . . . . ? N1 B1 C7 C8 168.2(3) . . . . ? C6 B1 C7 C8 50.6(4) . . . . ? C13 B1 C7 C8 -76.2(3) . . . . ? C12 C7 C8 C9 -2.5(4) . . . . ? B1 C7 C8 C9 175.6(3) . . . . ? C7 C8 C9 C10 2.6(5) . . . . ? C8 C9 C10 C11 -1.5(5) . . . . ? C9 C10 C11 C12 0.4(5) . . . . ? C8 C7 C12 C11 1.3(4) . . . . ? B1 C7 C12 C11 -176.7(3) . . . . ? C10 C11 C12 C7 -0.4(5) . . . . ? N1 B1 C13 C14 157.16(16) . . . . ? C6 B1 C13 C14 -84.8(2) . . . . ? C7 B1 C13 C14 40.8(3) . . . . ? N1 B1 C13 C18 -27.5(3) . . . . ? C6 B1 C13 C18 90.5(3) . . . . ? C7 B1 C13 C18 -143.90(19) . . . . ? C18 C13 C14 C15 0.0 . . . . ? B1 C13 C14 C15 175.31(19) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? B1 C13 C18 C17 -175.33(19) . . . . ? N3 C20 C21 C22 0.1(5) . . . . ? C20 C21 C22 C23 -0.5(5) . . . . ? C21 C22 C23 C31 0.4(4) . . . . ? C21 C22 C23 C24 -177.0(3) . . . . ? C31 C23 C24 C25 3.4(4) . . . . ? C22 C23 C24 C25 -179.2(3) . . . . ? C23 C24 C25 C26 -2.6(5) . . . . ? C24 C25 C26 C30 0.4(5) . . . . ? C24 C25 C26 C27 -179.0(3) . . . . ? C30 C26 C27 C28 -0.2(4) . . . . ? C25 C26 C27 C28 179.2(3) . . . . ? C26 C27 C28 C29 -0.4(4) . . . . ? C27 C28 C29 N2 -0.4(4) . . . . ? C27 C26 C30 N2 1.5(5) . . . . ? C25 C26 C30 N2 -177.9(3) . . . . ? C27 C26 C30 C31 -179.7(3) . . . . ? C25 C26 C30 C31 0.8(5) . . . . ? C22 C23 C31 N3 0.1(4) . . . . ? C24 C23 C31 N3 177.7(3) . . . . ? C22 C23 C31 C30 -179.7(3) . . . . ? C24 C23 C31 C30 -2.1(4) . . . . ? N2 C30 C31 N3 -0.9(4) . . . . ? C26 C30 C31 N3 -179.8(3) . . . . ? N2 C30 C31 C23 179.0(3) . . . . ? C26 C30 C31 C23 0.1(5) . . . . ? N1 C19 Fe1 C19 131(4) . . . 2_556 ? N1 C19 Fe1 N3 36(4) . . . . ? N1 C19 Fe1 N3 -138(4) . . . 2_556 ? N1 C19 Fe1 N2 -118(4) . . . 2_556 ? N1 C19 Fe1 N2 -46(4) . . . . ? Fe1 C19 N1 B1 17(5) . . . . ? C6 B1 N1 C19 -38.7(15) . . . . ? C7 B1 N1 C19 -158.8(13) . . . . ? C13 B1 N1 C19 83.2(14) . . . . ? C28 C29 N2 C30 1.6(4) . . . . ? C28 C29 N2 Fe1 179.6(2) . . . . ? C26 C30 N2 C29 -2.2(5) . . . . ? C31 C30 N2 C29 179.0(3) . . . . ? C26 C30 N2 Fe1 179.4(3) . . . . ? C31 C30 N2 Fe1 0.6(4) . . . . ? C19 Fe1 N2 C29 -88.0(3) . . . . ? C19 Fe1 N2 C29 161(2) 2_556 . . . ? N3 Fe1 N2 C29 -178.2(3) . . . . ? N3 Fe1 N2 C29 7.8(3) 2_556 . . . ? N2 Fe1 N2 C29 89.5(3) 2_556 . . . ? C19 Fe1 N2 C30 90.1(2) . . . . ? C19 Fe1 N2 C30 -21(3) 2_556 . . . ? N3 Fe1 N2 C30 -0.2(2) . . . . ? N3 Fe1 N2 C30 -174.1(2) 2_556 . . . ? N2 Fe1 N2 C30 -92.5(2) 2_556 . . . ? C21 C20 N3 C31 0.4(5) . . . . ? C21 C20 N3 Fe1 178.8(2) . . . . ? C23 C31 N3 C20 -0.5(4) . . . . ? C30 C31 N3 C20 179.4(3) . . . . ? C23 C31 N3 Fe1 -179.1(2) . . . . ? C30 C31 N3 Fe1 0.8(3) . . . . ? C19 Fe1 N3 C20 91.2(3) . . . . ? C19 Fe1 N3 C20 0.3(3) 2_556 . . . ? N3 Fe1 N3 C20 -134.1(3) 2_556 . . . ? N2 Fe1 N3 C20 -90.0(3) 2_556 . . . ? N2 Fe1 N3 C20 -178.8(3) . . . . ? C19 Fe1 N3 C31 -90.4(2) . . . . ? C19 Fe1 N3 C31 178.7(2) 2_556 . . . ? N3 Fe1 N3 C31 44.32(19) 2_556 . . . ? N2 Fe1 N3 C31 88.4(2) 2_556 . . . ? N2 Fe1 N3 C31 -0.32(19) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.508 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.048 #===END