# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Yih-Hsing Lo' _publ_contact_author_email yhlo@tmue.edu.tw _publ_author_name 'Yih-Hsing Lo' data_a11316 _database_code_depnum_ccdc_archive 'CCDC 824345' #TrackingRef '- 4b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H40 B N6 O2 P Ru D 0.79(C~7~H~8~)' _chemical_formula_sum 'C50.53 H46.32 B N6 O2 P Ru' _chemical_formula_weight 912.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1964(4) _cell_length_b 12.4327(4) _cell_length_c 18.4795(7) _cell_angle_alpha 89.086(2) _cell_angle_beta 77.852(2) _cell_angle_gamma 83.264(2) _cell_volume 2274.27(14) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown(dark) _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 943 _exptl_absorpt_coefficient_mu 0.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9046 _exptl_absorpt_correction_T_max 0.9790 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15791 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 24.93 _reflns_number_total 7759 _reflns_number_gt 5892 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Squeezed half toluene. 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^)+(0.0457P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7759 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 C1 C 0.0185(3) 0.5559(2) 0.11695(18) 0.0323(8) Uani 1 1 d . . . H1 H 0.0585 0.5893 0.0725 0.039 Uiso 1 1 calc R . . C2 C -0.0163(3) 0.4508(3) 0.1217(2) 0.0398(8) Uani 1 1 d . . . H2 H -0.0054 0.4000 0.0824 0.048 Uiso 1 1 calc R . . C3 C -0.0694(3) 0.4362(2) 0.1949(2) 0.0388(9) Uani 1 1 d . . . H3 H -0.1024 0.3719 0.2160 0.047 Uiso 1 1 calc R . . C4 C 0.1536(4) 0.6811(3) 0.36400(19) 0.0464(9) Uani 1 1 d . . . H4 H 0.2133 0.7353 0.3578 0.056 Uiso 1 1 calc R . . C5 C 0.1462(4) 0.6034(3) 0.4184(2) 0.0570(11) Uani 1 1 d . . . H5 H 0.1980 0.5935 0.4557 0.068 Uiso 1 1 calc R . . C6 C 0.0469(4) 0.5430(3) 0.40673(19) 0.0496(10) Uani 1 1 d . . . H6 H 0.0171 0.4828 0.4352 0.060 Uiso 1 1 calc R . . C7 C -0.2984(4) 0.8219(3) 0.30208(18) 0.0422(9) Uani 1 1 d . . . H7 H -0.3034 0.8937 0.2837 0.051 Uiso 1 1 calc R . . C8 C -0.4044(4) 0.7774(3) 0.3489(2) 0.0510(10) Uani 1 1 d . . . H8 H -0.4929 0.8118 0.3681 0.061 Uiso 1 1 calc R . . C9 C -0.3534(4) 0.6742(3) 0.36111(19) 0.0455(9) Uani 1 1 d . . . H9 H -0.4011 0.6228 0.3912 0.055 Uiso 1 1 calc R . . C10 C 0.3434(3) 0.6305(2) 0.19284(16) 0.0294(7) Uani 1 1 d . . . C11 C 0.2960(3) 0.5308(2) 0.21031(17) 0.0366(8) Uani 1 1 d . . . H11 H 0.2076 0.5208 0.2049 0.044 Uiso 1 1 calc R . . C12 C 0.3745(4) 0.4463(3) 0.23523(18) 0.0421(9) Uani 1 1 d . . . H12 H 0.3397 0.3792 0.2476 0.051 Uiso 1 1 calc R . . C13 C 0.5051(4) 0.4596(3) 0.24227(17) 0.0435(9) Uani 1 1 d . . . H13 H 0.5595 0.4021 0.2601 0.052 Uiso 1 1 calc R . . C14 C 0.5545(4) 0.5566(3) 0.22319(19) 0.0463(9) Uani 1 1 d . . . H14 H 0.6444 0.5652 0.2265 0.056 Uiso 1 1 calc R . . C15 C 0.4754(3) 0.6415(3) 0.19934(17) 0.0371(8) Uani 1 1 d . . . H15 H 0.5108 0.7084 0.1872 0.044 Uiso 1 1 calc R . . C16 C 0.2657(3) 0.7183(2) 0.06161(16) 0.0301(7) Uani 1 1 d . . . C17 C 0.3349(3) 0.6240(3) 0.02680(18) 0.0381(8) Uani 1 1 d . . . H17 H 0.3725 0.5690 0.0553 0.046 Uiso 1 1 calc R . . C18 C 0.3502(4) 0.6086(3) -0.04909(18) 0.0435(9) Uani 1 1 d . . . H18 H 0.3963 0.5431 -0.0721 0.052 Uiso 1 1 calc R . . C19 C 0.2977(4) 0.6892(3) -0.09050(19) 0.0488(10) Uani 1 1 d . . . H19 H 0.3084 0.6795 -0.1424 0.059 Uiso 1 1 calc R . . C20 C 0.2300(4) 0.7834(3) -0.0571(2) 0.0549(11) Uani 1 1 d . . . H20 H 0.1939 0.8385 -0.0860 0.066 Uiso 1 1 calc R . . C21 C 0.2142(4) 0.7987(3) 0.01822(19) 0.0438(9) Uani 1 1 d . . . H21 H 0.1677 0.8644 0.0407 0.053 Uiso 1 1 calc R . . C22 C 0.3289(3) 0.8583(2) 0.16676(19) 0.0352(8) Uani 1 1 d . . . C23 C 0.4261(4) 0.8887(3) 0.1071(2) 0.0468(9) Uani 1 1 d . . . H23 H 0.4391 0.8527 0.0607 0.056 Uiso 1 1 calc R . . C24 C 0.5042(4) 0.9713(3) 0.1148(2) 0.0586(11) Uani 1 1 d . . . H24 H 0.5706 0.9908 0.0740 0.070 Uiso 1 1 calc R . . C25 C 0.4843(4) 1.0238(3) 0.1814(3) 0.0589(11) Uani 1 1 d . . . H25 H 0.5370 1.0803 0.1865 0.071 Uiso 1 1 calc R . . C26 C 0.3893(4) 0.9960(3) 0.2408(2) 0.0528(10) Uani 1 1 d . . . H26 H 0.3767 1.0332 0.2867 0.063 Uiso 1 1 calc R . . C27 C 0.3111(3) 0.9131(3) 0.2342(2) 0.0424(9) Uani 1 1 d . . . H27 H 0.2457 0.8939 0.2756 0.051 Uiso 1 1 calc R . . C28 C -0.0196(3) 0.9817(2) 0.22957(17) 0.0344(8) Uani 1 1 d . . . C29 C -0.0150(4) 1.0970(3) 0.25321(19) 0.0457(9) Uani 1 1 d . . . C30 C 0.0449(4) 1.1225(3) 0.31720(19) 0.0433(9) Uani 1 1 d . . . C31 C 0.0501(4) 1.0552(3) 0.37751(19) 0.0524(10) Uani 1 1 d . . . H31 H 0.0189 0.9860 0.3783 0.063 Uiso 1 1 calc R . . C32 C 0.1003(4) 1.0885(3) 0.4364(2) 0.0644(12) Uani 1 1 d . . . H32 H 0.1027 1.0417 0.4774 0.077 Uiso 1 1 calc R . . C33 C 0.1473(4) 1.1887(3) 0.4368(2) 0.0588(11) Uani 1 1 d . . . C34 C 0.1994(5) 1.2237(4) 0.5032(2) 0.0876(16) Uani 1 1 d . . . H34A H 0.1894 1.1676 0.5412 0.131 Uiso 1 1 calc R . . H34B H 0.1473 1.2918 0.5236 0.131 Uiso 1 1 calc R . . H34C H 0.2949 1.2342 0.4876 0.131 Uiso 1 1 calc R . . C35 C 0.1467(4) 1.2527(3) 0.3756(2) 0.0592(11) Uani 1 1 d . . . H35 H 0.1831 1.3199 0.3735 0.071 Uiso 1 1 calc R . . C36 C 0.0945(4) 1.2220(3) 0.3170(2) 0.0533(10) Uani 1 1 d . . . H36 H 0.0924 1.2693 0.2762 0.064 Uiso 1 1 calc R . . C37 C -0.0608(3) 0.9588(2) 0.16501(17) 0.0354(8) Uani 1 1 d . . . H37 H -0.0858 1.0138 0.1326 0.042 Uiso 1 1 calc R . . C38 C -0.0629(3) 0.8484(2) 0.15120(16) 0.0274(7) Uani 1 1 d . . . C39 C -0.1295(3) 0.8212(2) 0.09071(16) 0.0276(7) Uani 1 1 d . . . C40 C -0.1183(3) 0.8813(3) 0.02542(17) 0.0384(8) Uani 1 1 d . . . H40 H -0.0697 0.9426 0.0205 0.046 Uiso 1 1 calc R . . C41 C -0.1759(3) 0.8541(3) -0.03211(18) 0.0416(9) Uani 1 1 d . . . H41 H -0.1628 0.8950 -0.0764 0.050 Uiso 1 1 calc R . . C42 C -0.2524(3) 0.7681(3) -0.02636(18) 0.0374(8) Uani 1 1 d . . . C43 C -0.3149(4) 0.7390(3) -0.0893(2) 0.0590(11) Uani 1 1 d . . . H43A H -0.2916 0.7886 -0.1305 0.089 Uiso 1 1 calc R . . H43B H -0.4133 0.7449 -0.0726 0.089 Uiso 1 1 calc R . . H43C H -0.2805 0.6645 -0.1057 0.089 Uiso 1 1 calc R . . C44 C -0.2692(3) 0.7114(3) 0.03888(19) 0.0390(8) Uani 1 1 d . . . H44 H -0.3236 0.6535 0.0446 0.047 Uiso 1 1 calc R . . C45 C -0.2090(3) 0.7359(2) 0.09701(17) 0.0322(8) Uani 1 1 d . . . H45 H -0.2222 0.6944 0.1410 0.039 Uiso 1 1 calc R . . N1 N -0.0125(2) 0.60358(18) 0.18397(13) 0.0277(6) Uani 1 1 d . . . N2 N -0.0674(3) 0.52813(19) 0.23269(14) 0.0325(6) Uani 1 1 d . . . N3 N 0.0654(3) 0.66991(19) 0.32112(14) 0.0326(6) Uani 1 1 d . . . N4 N -0.0003(3) 0.5840(2) 0.34816(14) 0.0364(7) Uani 1 1 d . . . N5 N -0.1896(3) 0.7493(2) 0.28698(13) 0.0323(6) Uani 1 1 d . . . N6 N -0.2235(3) 0.6566(2) 0.32340(14) 0.0352(7) Uani 1 1 d . . . O1 O 0.0144(2) 0.90287(15) 0.27014(11) 0.0321(5) Uani 1 1 d . . . O2 O -0.0576(3) 1.17042(19) 0.21683(16) 0.0767(10) Uani 1 1 d . . . P1 P 0.23389(8) 0.74264(6) 0.16174(4) 0.0287(2) Uani 1 1 d . . . Ru1 Ru 0.00848(3) 0.753675(19) 0.224880(13) 0.02646(9) Uani 1 1 d . . . B1 B -0.1183(4) 0.5563(3) 0.3156(2) 0.0375(10) Uani 1 1 d . . . H1A H -0.1592 0.4939 0.3425 0.045 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 C1 0.0310(19) 0.0279(17) 0.040(2) -0.0030(15) -0.0115(16) -0.0031(15) C2 0.042(2) 0.0317(18) 0.048(2) -0.0114(16) -0.0133(18) -0.0054(17) C3 0.039(2) 0.0235(17) 0.060(2) -0.0002(16) -0.0225(19) -0.0070(16) C4 0.053(2) 0.049(2) 0.046(2) 0.0055(18) -0.026(2) -0.0123(19) C5 0.074(3) 0.064(3) 0.043(2) 0.017(2) -0.034(2) -0.012(2) C6 0.073(3) 0.041(2) 0.040(2) 0.0177(17) -0.024(2) -0.010(2) C7 0.043(2) 0.039(2) 0.041(2) -0.0074(17) -0.0067(18) 0.0077(18) C8 0.037(2) 0.066(3) 0.045(2) -0.009(2) 0.0015(18) -0.002(2) C9 0.043(2) 0.053(2) 0.039(2) -0.0009(18) 0.0010(18) -0.019(2) C10 0.0311(19) 0.0273(16) 0.0297(18) -0.0036(14) -0.0094(15) 0.0037(15) C11 0.037(2) 0.0323(18) 0.043(2) -0.0004(15) -0.0147(17) 0.0009(16) C12 0.048(2) 0.0302(18) 0.046(2) 0.0062(16) -0.0094(18) 0.0016(17) C13 0.049(2) 0.048(2) 0.0316(19) -0.0041(16) -0.0164(18) 0.0164(19) C14 0.040(2) 0.052(2) 0.053(2) -0.0034(19) -0.0256(19) -0.0014(19) C15 0.038(2) 0.0366(19) 0.038(2) -0.0017(15) -0.0127(17) -0.0031(17) C16 0.0284(18) 0.0296(17) 0.0331(18) 0.0022(14) -0.0080(15) -0.0039(15) C17 0.042(2) 0.0327(18) 0.042(2) 0.0028(15) -0.0147(17) -0.0032(17) C18 0.053(2) 0.039(2) 0.037(2) -0.0081(16) -0.0092(18) -0.0013(18) C19 0.047(2) 0.066(3) 0.032(2) 0.0013(19) -0.0108(18) -0.001(2) C20 0.056(3) 0.063(3) 0.037(2) 0.0122(19) -0.0071(19) 0.019(2) C21 0.047(2) 0.0362(19) 0.042(2) 0.0041(16) -0.0033(18) 0.0096(17) C22 0.0310(19) 0.0258(17) 0.050(2) -0.0007(15) -0.0121(17) -0.0034(15) C23 0.041(2) 0.037(2) 0.063(3) 0.0016(18) -0.0068(19) -0.0091(18) C24 0.050(3) 0.044(2) 0.079(3) 0.009(2) -0.003(2) -0.019(2) C25 0.050(3) 0.040(2) 0.092(3) 0.001(2) -0.021(3) -0.018(2) C26 0.052(3) 0.043(2) 0.070(3) -0.014(2) -0.021(2) -0.012(2) C27 0.038(2) 0.039(2) 0.053(2) -0.0021(17) -0.0110(18) -0.0097(17) C28 0.041(2) 0.0259(17) 0.0363(19) -0.0009(15) -0.0081(16) -0.0035(16) C29 0.068(3) 0.0286(19) 0.045(2) 0.0025(16) -0.021(2) -0.0074(19) C30 0.054(2) 0.0326(19) 0.043(2) -0.0082(16) -0.0087(19) -0.0056(18) C31 0.078(3) 0.042(2) 0.040(2) -0.0044(17) -0.013(2) -0.020(2) C32 0.097(4) 0.059(3) 0.043(2) -0.001(2) -0.020(2) -0.023(3) C33 0.059(3) 0.063(3) 0.057(3) -0.025(2) -0.017(2) -0.006(2) C34 0.111(4) 0.093(4) 0.072(3) -0.031(3) -0.042(3) -0.021(3) C35 0.072(3) 0.039(2) 0.072(3) -0.010(2) -0.024(2) -0.012(2) C36 0.071(3) 0.034(2) 0.058(2) -0.0047(18) -0.019(2) -0.009(2) C37 0.046(2) 0.0264(17) 0.0357(19) 0.0060(14) -0.0139(17) -0.0029(16) C38 0.0253(17) 0.0276(16) 0.0279(17) 0.0007(13) -0.0013(14) -0.0051(14) C39 0.0268(18) 0.0259(16) 0.0302(17) 0.0013(13) -0.0071(14) -0.0013(14) C40 0.045(2) 0.0372(19) 0.038(2) 0.0093(15) -0.0129(17) -0.0184(17) C41 0.047(2) 0.048(2) 0.0322(19) 0.0114(16) -0.0124(17) -0.0107(19) C42 0.034(2) 0.042(2) 0.039(2) -0.0041(16) -0.0163(17) 0.0004(17) C43 0.067(3) 0.067(3) 0.054(2) -0.006(2) -0.034(2) -0.014(2) C44 0.034(2) 0.0312(18) 0.056(2) 0.0026(16) -0.0167(18) -0.0094(16) C45 0.0300(19) 0.0300(17) 0.0375(19) 0.0064(14) -0.0085(16) -0.0055(15) N1 0.0284(15) 0.0249(13) 0.0311(15) 0.0024(11) -0.0096(12) -0.0019(12) N2 0.0372(17) 0.0251(14) 0.0384(16) 0.0057(12) -0.0123(13) -0.0093(13) N3 0.0371(16) 0.0276(14) 0.0352(15) 0.0039(12) -0.0128(13) -0.0032(13) N4 0.0479(18) 0.0302(15) 0.0352(16) 0.0073(12) -0.0156(14) -0.0104(14) N5 0.0385(17) 0.0275(14) 0.0324(15) 0.0020(12) -0.0091(13) -0.0074(13) N6 0.0370(17) 0.0358(16) 0.0330(15) 0.0017(12) -0.0042(13) -0.0109(14) O1 0.0430(14) 0.0241(11) 0.0323(12) 0.0016(9) -0.0139(11) -0.0055(10) O2 0.141(3) 0.0249(14) 0.080(2) 0.0031(13) -0.062(2) -0.0073(16) P1 0.0315(5) 0.0231(4) 0.0324(5) 0.0012(3) -0.0093(4) -0.0027(4) Ru1 0.03185(16) 0.02044(13) 0.02848(15) 0.00234(10) -0.00920(11) -0.00394(11) B1 0.042(3) 0.031(2) 0.041(2) 0.0067(17) -0.009(2) -0.0119(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 C1 N1 1.342(4) . ? C1 C2 1.390(4) . ? C1 H1 0.9500 . ? C2 C3 1.366(5) . ? C2 H2 0.9500 . ? C3 N2 1.353(4) . ? C3 H3 0.9500 . ? C4 N3 1.337(4) . ? C4 C5 1.380(5) . ? C4 H4 0.9500 . ? C5 C6 1.382(5) . ? C5 H5 0.9500 . ? C6 N4 1.344(4) . ? C6 H6 0.9500 . ? C7 N5 1.329(4) . ? C7 C8 1.398(5) . ? C7 H7 0.9500 . ? C8 C9 1.361(5) . ? C8 H8 0.9500 . ? C9 N6 1.355(4) . ? C9 H9 0.9500 . ? C10 C11 1.391(4) . ? C10 C15 1.398(4) . ? C10 P1 1.844(3) . ? C11 C12 1.378(4) . ? C11 H11 0.9500 . ? C12 C13 1.395(5) . ? C12 H12 0.9500 . ? C13 C14 1.374(5) . ? C13 H13 0.9500 . ? C14 C15 1.376(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.388(4) . ? C16 C21 1.395(4) . ? C16 P1 1.834(3) . ? C17 C18 1.392(4) . ? C17 H17 0.9500 . ? C18 C19 1.379(5) . ? C18 H18 0.9500 . ? C19 C20 1.372(5) . ? C19 H19 0.9500 . ? C20 C21 1.381(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.398(4) . ? C22 C23 1.398(5) . ? C22 P1 1.839(3) . ? C23 C24 1.398(4) . ? C23 H23 0.9500 . ? C24 C25 1.368(5) . ? C24 H24 0.9500 . ? C25 C26 1.373(5) . ? C25 H25 0.9500 . ? C26 C27 1.397(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 O1 1.284(3) . ? C28 C37 1.390(4) . ? C28 C29 1.514(4) . ? C29 O2 1.218(4) . ? C29 C30 1.495(4) . ? C30 C36 1.390(4) . ? C30 C31 1.390(5) . ? C31 C32 1.385(5) . ? C31 H31 0.9500 . ? C32 C33 1.387(5) . ? C32 H32 0.9500 . ? C33 C35 1.374(5) . ? C33 C34 1.523(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.380(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.404(4) . ? C37 H37 0.9500 . ? C38 C39 1.487(4) . ? C38 Ru1 1.984(3) . ? C39 C45 1.398(4) . ? C39 C40 1.400(4) . ? C40 C41 1.382(4) . ? C40 H40 0.9500 . ? C41 C42 1.386(4) . ? C41 H41 0.9500 . ? C42 C44 1.376(4) . ? C42 C43 1.506(4) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.399(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? N1 N2 1.374(3) . ? N1 Ru1 2.075(2) . ? N2 B1 1.542(4) . ? N3 N4 1.360(3) . ? N3 Ru1 2.195(2) . ? N4 B1 1.529(4) . ? N5 N6 1.367(3) . ? N5 Ru1 2.109(3) . ? N6 B1 1.534(5) . ? O1 Ru1 2.0593(19) . ? P1 Ru1 2.3378(9) . ? B1 H1A 1.0000 . ? 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 C1 C2 110.5(3) . . ? N1 C1 H1 124.7 . . ? C2 C1 H1 124.7 . . ? C3 C2 C1 105.2(3) . . ? C3 C2 H2 127.4 . . ? C1 C2 H2 127.4 . . ? N2 C3 C2 109.0(3) . . ? N2 C3 H3 125.5 . . ? C2 C3 H3 125.5 . . ? N3 C4 C5 111.0(3) . . ? N3 C4 H4 124.5 . . ? C5 C4 H4 124.5 . . ? C4 C5 C6 104.7(3) . . ? C4 C5 H5 127.6 . . ? C6 C5 H5 127.6 . . ? N4 C6 C5 108.3(3) . . ? N4 C6 H6 125.8 . . ? C5 C6 H6 125.8 . . ? N5 C7 C8 110.2(3) . . ? N5 C7 H7 124.9 . . ? C8 C7 H7 124.9 . . ? C9 C8 C7 105.1(3) . . ? C9 C8 H8 127.5 . . ? C7 C8 H8 127.5 . . ? N6 C9 C8 109.0(3) . . ? N6 C9 H9 125.5 . . ? C8 C9 H9 125.5 . . ? C11 C10 C15 117.8(3) . . ? C11 C10 P1 120.1(2) . . ? C15 C10 P1 122.0(2) . . ? C12 C11 C10 121.4(3) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 119.8(3) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 119.3(3) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C15 C14 C13 120.9(3) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C10 120.7(3) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? C17 C16 C21 118.2(3) . . ? C17 C16 P1 124.0(2) . . ? C21 C16 P1 117.8(2) . . ? C16 C17 C18 121.1(3) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C19 C18 C17 119.4(3) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C20 C19 C18 120.3(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 120.4(3) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C16 120.6(3) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C27 C22 C23 118.4(3) . . ? C27 C22 P1 119.0(3) . . ? C23 C22 P1 122.5(3) . . ? C24 C23 C22 120.9(4) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 C23 119.5(4) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.9(3) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C27 120.3(4) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 120.0(3) . . ? C26 C27 H27 120.0 . . ? C22 C27 H27 120.0 . . ? O1 C28 C37 118.9(3) . . ? O1 C28 C29 119.5(3) . . ? C37 C28 C29 121.6(3) . . ? O2 C29 C30 119.7(3) . . ? O2 C29 C28 118.2(3) . . ? C30 C29 C28 122.1(3) . . ? C36 C30 C31 118.3(3) . . ? C36 C30 C29 117.3(3) . . ? C31 C30 C29 124.3(3) . . ? C32 C31 C30 120.2(3) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 121.4(4) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C35 C33 C32 117.7(3) . . ? C35 C33 C34 122.3(4) . . ? C32 C33 C34 120.0(4) . . ? 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 C36 121.7(4) . . ? C33 C35 H35 119.1 . . ? C36 C35 H35 119.1 . . ? C35 C36 C30 120.5(4) . . ? C35 C36 H36 119.8 . . ? C30 C36 H36 119.8 . . ? C28 C37 C38 115.1(3) . . ? C28 C37 H37 122.4 . . ? C38 C37 H37 122.4 . . ? C37 C38 C39 116.8(3) . . ? C37 C38 Ru1 112.6(2) . . ? C39 C38 Ru1 130.3(2) . . ? C45 C39 C40 116.7(3) . . ? C45 C39 C38 121.6(3) . . ? C40 C39 C38 121.7(3) . . ? C41 C40 C39 121.9(3) . . ? C41 C40 H40 119.0 . . ? C39 C40 H40 119.0 . . ? C40 C41 C42 121.1(3) . . ? C40 C41 H41 119.4 . . ? C42 C41 H41 119.4 . . ? C44 C42 C41 117.4(3) . . ? C44 C42 C43 121.7(3) . . ? C41 C42 C43 120.8(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 C45 122.3(3) . . ? C42 C44 H44 118.9 . . ? C45 C44 H44 118.9 . . ? C44 C45 C39 120.3(3) . . ? C44 C45 H45 119.8 . . ? C39 C45 H45 119.8 . . ? C1 N1 N2 106.3(2) . . ? C1 N1 Ru1 135.0(2) . . ? N2 N1 Ru1 118.69(18) . . ? C3 N2 N1 109.0(2) . . ? C3 N2 B1 130.4(3) . . ? N1 N2 B1 120.6(2) . . ? C4 N3 N4 106.2(2) . . ? C4 N3 Ru1 136.0(2) . . ? N4 N3 Ru1 117.84(18) . . ? C6 N4 N3 109.8(2) . . ? C6 N4 B1 130.6(3) . . ? N3 N4 B1 119.3(2) . . ? C7 N5 N6 106.9(3) . . ? C7 N5 Ru1 133.6(2) . . ? N6 N5 Ru1 119.4(2) . . ? C9 N6 N5 108.8(3) . . ? C9 N6 B1 131.9(3) . . ? N5 N6 B1 119.3(3) . . ? C28 O1 Ru1 112.72(18) . . ? C22 P1 C16 101.71(14) . . ? C22 P1 C10 101.71(14) . . ? C16 P1 C10 102.46(14) . . ? C22 P1 Ru1 118.84(11) . . ? C16 P1 Ru1 116.24(10) . . ? C10 P1 Ru1 113.54(10) . . ? C38 Ru1 O1 80.41(10) . . ? C38 Ru1 N1 99.49(10) . . ? O1 Ru1 N1 175.61(9) . . ? C38 Ru1 N5 90.07(11) . . ? O1 Ru1 N5 90.15(9) . . ? N1 Ru1 N5 85.47(9) . . ? C38 Ru1 N3 169.69(11) . . ? O1 Ru1 N3 91.61(8) . . ? N1 Ru1 N3 87.97(9) . . ? N5 Ru1 N3 83.39(10) . . ? C38 Ru1 P1 95.14(9) . . ? O1 Ru1 P1 92.85(6) . . ? N1 Ru1 P1 91.53(7) . . ? N5 Ru1 P1 174.36(7) . . ? N3 Ru1 P1 91.74(7) . . ? N4 B1 N6 108.1(3) . . ? N4 B1 N2 109.3(3) . . ? N6 B1 N2 108.9(3) . . ? N4 B1 H1A 110.2 . . ? N6 B1 H1A 110.2 . . ? N2 B1 H1A 110.2 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 24.93 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.849 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.064 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.708 0.500 400.0 78.9 _platon_squeeze_details ; ? ; # Attachment '- 5.cif' data_a11066 _database_code_depnum_ccdc_archive 'CCDC 824346' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H39 B N7 O P Ru' _chemical_formula_sum 'C43 H39 B N7 O P Ru' _chemical_formula_weight 812.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7013(7) _cell_length_b 14.1739(9) _cell_length_c 23.4437(13) _cell_angle_alpha 90.00 _cell_angle_beta 104.301(2) _cell_angle_gamma 90.00 _cell_volume 3767.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7453 _exptl_absorpt_correction_T_max 0.9016 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21592 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6479 _reflns_number_gt 5754 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0312P)^2^+2.8952P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6479 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.7918(2) 0.6076(2) 0.55245(13) 0.0331(6) Uani 1 1 d . . . H1' H 0.8149 0.5667 0.5882 0.040 Uiso 1 1 calc R . . C1 C 0.9930(2) 0.69298(18) 0.46886(12) 0.0358(6) Uani 1 1 d . . . H1 H 1.0098 0.7280 0.4373 0.043 Uiso 1 1 calc R . . C2 C 1.0762(2) 0.6428(2) 0.51083(13) 0.0426(7) Uani 1 1 d . . . H2 H 1.1583 0.6370 0.5136 0.051 Uiso 1 1 calc R . . C3 C 1.0139(2) 0.60371(19) 0.54715(12) 0.0386(6) Uani 1 1 d . . . H3 H 1.0456 0.5648 0.5803 0.046 Uiso 1 1 calc R . . C4 C 0.6730(2) 0.84310(19) 0.55107(12) 0.0366(6) Uani 1 1 d . . . H4 H 0.6432 0.9001 0.5316 0.044 Uiso 1 1 calc R . . C5 C 0.6917(3) 0.8276(2) 0.61102(12) 0.0477(7) Uani 1 1 d . . . H5 H 0.6774 0.8702 0.6398 0.057 Uiso 1 1 calc R . . C6 C 0.7349(2) 0.7381(2) 0.61987(12) 0.0443(7) Uani 1 1 d . . . H6 H 0.7572 0.7068 0.6568 0.053 Uiso 1 1 calc R . . C7 C 0.5773(2) 0.53554(16) 0.41927(11) 0.0303(5) Uani 1 1 d . . . H7 H 0.5315 0.5452 0.3802 0.036 Uiso 1 1 calc R . . C8 C 0.5748(2) 0.45414(17) 0.45152(11) 0.0345(6) Uani 1 1 d . . . H8 H 0.5291 0.3989 0.4395 0.041 Uiso 1 1 calc R . . C9 C 0.6528(2) 0.47091(17) 0.50463(11) 0.0334(6) Uani 1 1 d . . . H9 H 0.6714 0.4281 0.5368 0.040 Uiso 1 1 calc R . . C10 C 0.42786(19) 0.82534(16) 0.43055(11) 0.0295(5) Uani 1 1 d . . . C11 C 0.4265(2) 0.77284(18) 0.48051(12) 0.0341(6) Uani 1 1 d . . . H11 H 0.4833 0.7244 0.4931 0.041 Uiso 1 1 calc R . . C12 C 0.3430(2) 0.7905(2) 0.51221(13) 0.0441(7) Uani 1 1 d . . . H12 H 0.3435 0.7545 0.5464 0.053 Uiso 1 1 calc R . . C13 C 0.2594(3) 0.8602(2) 0.49427(15) 0.0525(8) Uani 1 1 d . . . H13 H 0.2026 0.8723 0.5161 0.063 Uiso 1 1 calc R . . C14 C 0.2588(3) 0.9121(2) 0.44457(15) 0.0535(8) Uani 1 1 d . . . H14 H 0.2009 0.9596 0.4319 0.064 Uiso 1 1 calc R . . C15 C 0.3425(2) 0.89513(18) 0.41271(13) 0.0411(6) Uani 1 1 d . . . H15 H 0.3415 0.9314 0.3785 0.049 Uiso 1 1 calc R . . C16 C 0.4373(2) 0.70748(17) 0.33554(11) 0.0308(5) Uani 1 1 d . . . C17 C 0.4804(2) 0.66342(18) 0.29203(11) 0.0361(6) Uani 1 1 d . . . H17 H 0.5554 0.6808 0.2867 0.043 Uiso 1 1 calc R . . C18 C 0.4150(3) 0.5944(2) 0.25630(12) 0.0455(7) Uani 1 1 d . . . H18 H 0.4447 0.5654 0.2264 0.055 Uiso 1 1 calc R . . C19 C 0.3058(3) 0.5677(2) 0.26446(13) 0.0536(8) Uani 1 1 d . . . H19 H 0.2612 0.5199 0.2405 0.064 Uiso 1 1 calc R . . C20 C 0.2628(3) 0.6107(2) 0.30736(14) 0.0547(8) Uani 1 1 d . . . H20 H 0.1882 0.5924 0.3130 0.066 Uiso 1 1 calc R . . C21 C 0.3272(2) 0.68061(19) 0.34249(12) 0.0418(6) Uani 1 1 d . . . H21 H 0.2958 0.7105 0.3716 0.050 Uiso 1 1 calc R . . C22 C 0.53032(19) 0.89718(16) 0.34119(11) 0.0292(5) Uani 1 1 d . . . C23 C 0.5590(2) 0.98374(17) 0.36962(12) 0.0356(6) Uani 1 1 d . . . H23 H 0.5788 0.9863 0.4114 0.043 Uiso 1 1 calc R . . C24 C 0.5590(2) 1.06600(19) 0.33745(14) 0.0443(7) Uani 1 1 d . . . H24 H 0.5772 1.1246 0.3573 0.053 Uiso 1 1 calc R . . C25 C 0.5326(2) 1.0629(2) 0.27678(14) 0.0480(8) Uani 1 1 d . . . H25 H 0.5336 1.1191 0.2548 0.058 Uiso 1 1 calc R . . C26 C 0.5049(2) 0.9781(2) 0.24826(13) 0.0435(7) Uani 1 1 d . . . H26 H 0.4869 0.9758 0.2065 0.052 Uiso 1 1 calc R . . C27 C 0.5029(2) 0.89560(19) 0.28005(11) 0.0371(6) Uani 1 1 d . . . H27 H 0.4827 0.8376 0.2598 0.045 Uiso 1 1 calc R . . C28 C 0.82750(19) 0.88647(16) 0.38398(10) 0.0251(5) Uani 1 1 d . . . C29 C 0.87524(19) 0.98122(16) 0.37651(10) 0.0256(5) Uani 1 1 d . . . C30 C 0.9605(2) 1.02289(17) 0.42107(11) 0.0326(6) Uani 1 1 d . . . H30 H 0.9945 0.9878 0.4556 0.039 Uiso 1 1 calc R . . C31 C 0.9970(2) 1.11476(19) 0.41616(12) 0.0412(7) Uani 1 1 d . . . H31 H 1.0557 1.1422 0.4471 0.049 Uiso 1 1 calc R . . C32 C 0.9483(3) 1.16597(19) 0.36658(13) 0.0450(7) Uani 1 1 d . . . H32 H 0.9720 1.2295 0.3634 0.054 Uiso 1 1 calc R . . C33 C 0.8649(2) 1.12520(18) 0.32130(12) 0.0411(6) Uani 1 1 d . . . H33 H 0.8314 1.1608 0.2869 0.049 Uiso 1 1 calc R . . C34 C 0.8297(2) 1.03339(17) 0.32555(11) 0.0336(6) Uani 1 1 d . . . H34 H 0.7740 1.0054 0.2936 0.040 Uiso 1 1 calc R . . C35 C 0.8188(2) 0.81209(16) 0.34241(10) 0.0271(5) Uani 1 1 d . . . C36 C 0.8762(2) 0.81844(16) 0.29214(11) 0.0299(5) Uani 1 1 d . . . C37 C 0.9986(2) 0.82054(19) 0.30189(13) 0.0422(7) Uani 1 1 d . . . H37 H 1.0461 0.8179 0.3411 0.051 Uiso 1 1 calc R . . C38 C 1.0526(3) 0.8264(2) 0.25540(15) 0.0532(8) Uani 1 1 d . . . H38 H 1.1362 0.8271 0.2629 0.064 Uiso 1 1 calc R . . C39 C 0.9846(3) 0.8312(2) 0.19840(15) 0.0561(9) Uani 1 1 d . . . H39 H 1.0211 0.8356 0.1665 0.067 Uiso 1 1 calc R . . C40 C 0.8635(3) 0.8295(2) 0.18792(13) 0.0502(8) Uani 1 1 d . . . H40 H 0.8165 0.8323 0.1486 0.060 Uiso 1 1 calc R . . C41 C 0.8096(3) 0.82364(18) 0.23453(11) 0.0391(6) Uani 1 1 d . . . H41 H 0.7260 0.8232 0.2267 0.047 Uiso 1 1 calc R . . C42 C 0.7699(2) 0.72961(16) 0.35963(10) 0.0259(5) Uani 1 1 d . . . C43 C 0.7673(3) 0.56175(17) 0.34131(12) 0.0399(6) Uani 1 1 d . . . H43A H 0.7786 0.5181 0.3107 0.060 Uiso 1 1 calc R . . H43B H 0.6877 0.5539 0.3471 0.060 Uiso 1 1 calc R . . H43C H 0.8256 0.5483 0.3783 0.060 Uiso 1 1 calc R . . N1 N 0.88638(16) 0.68466(13) 0.47947(8) 0.0271(4) Uani 1 1 d . . . N2 N 0.90011(17) 0.62955(14) 0.52820(9) 0.0309(5) Uani 1 1 d . . . N3 N 0.70260(17) 0.76706(14) 0.52435(9) 0.0289(4) Uani 1 1 d . . . N4 N 0.74066(18) 0.70147(15) 0.56747(8) 0.0318(5) Uani 1 1 d . . . N5 N 0.65234(16) 0.59868(13) 0.44995(8) 0.0264(4) Uani 1 1 d . . . N6 N 0.69872(17) 0.55749(14) 0.50384(8) 0.0291(4) Uani 1 1 d . . . N7 N 0.78839(16) 0.86655(13) 0.43020(8) 0.0255(4) Uani 1 1 d . . . H7' H 0.7929 0.9084 0.4584 0.031 Uiso 1 1 calc R . . O1 O 0.78187(15) 0.65589(11) 0.32371(7) 0.0343(4) Uani 1 1 d . . . P1 P 0.53290(5) 0.79084(4) 0.38673(3) 0.02534(14) Uani 1 1 d . . . Ru1 Ru 0.716952(15) 0.737121(12) 0.435766(8) 0.02231(7) 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 0.0326(15) 0.0375(16) 0.0290(16) 0.0112(13) 0.0069(12) 0.0060(12) C1 0.0272(13) 0.0390(15) 0.0433(16) -0.0026(12) 0.0129(11) -0.0008(11) C2 0.0230(13) 0.0473(16) 0.0557(18) -0.0017(14) 0.0062(12) 0.0043(12) C3 0.0293(13) 0.0375(15) 0.0438(16) 0.0029(12) -0.0009(11) 0.0092(11) C4 0.0323(13) 0.0366(14) 0.0421(16) -0.0094(12) 0.0118(12) 0.0024(11) C5 0.0488(17) 0.0572(19) 0.0404(17) -0.0187(14) 0.0173(13) 0.0016(14) C6 0.0435(16) 0.063(2) 0.0278(15) -0.0042(13) 0.0118(12) -0.0009(14) C7 0.0306(13) 0.0283(13) 0.0326(14) 0.0005(11) 0.0088(11) 0.0000(10) C8 0.0356(14) 0.0272(13) 0.0439(16) 0.0013(11) 0.0158(12) -0.0017(11) C9 0.0345(14) 0.0295(14) 0.0401(15) 0.0115(11) 0.0167(12) 0.0059(11) C10 0.0224(12) 0.0257(12) 0.0418(15) -0.0009(11) 0.0106(10) -0.0010(10) C11 0.0278(13) 0.0332(14) 0.0432(16) 0.0004(12) 0.0123(11) -0.0038(10) C12 0.0436(16) 0.0439(16) 0.0518(18) -0.0038(14) 0.0252(14) -0.0101(13) C13 0.0454(17) 0.0426(17) 0.082(2) -0.0119(16) 0.0398(17) -0.0047(14) C14 0.0378(16) 0.0331(15) 0.097(3) 0.0016(16) 0.0310(16) 0.0062(12) C15 0.0324(14) 0.0312(14) 0.0627(19) 0.0089(13) 0.0176(13) 0.0070(11) C16 0.0284(12) 0.0269(13) 0.0332(14) 0.0042(11) 0.0000(10) 0.0007(10) C17 0.0340(14) 0.0363(14) 0.0347(15) 0.0038(12) 0.0024(11) -0.0022(11) C18 0.0531(18) 0.0427(16) 0.0359(16) -0.0038(13) 0.0019(13) -0.0045(13) C19 0.0521(18) 0.0544(19) 0.0460(19) -0.0076(15) -0.0036(15) -0.0176(15) C20 0.0383(16) 0.063(2) 0.060(2) -0.0070(16) 0.0056(14) -0.0183(15) C21 0.0319(14) 0.0435(16) 0.0475(17) -0.0022(13) 0.0050(12) -0.0038(12) C22 0.0199(11) 0.0292(13) 0.0384(15) 0.0082(11) 0.0073(10) 0.0038(10) C23 0.0317(13) 0.0325(14) 0.0437(16) 0.0065(12) 0.0113(12) 0.0029(11) C24 0.0397(15) 0.0302(14) 0.063(2) 0.0105(13) 0.0140(14) 0.0017(12) C25 0.0379(16) 0.0421(17) 0.065(2) 0.0266(15) 0.0137(14) 0.0061(13) C26 0.0363(15) 0.0521(18) 0.0415(16) 0.0192(14) 0.0085(12) 0.0071(13) C27 0.0309(13) 0.0387(15) 0.0411(16) 0.0093(12) 0.0076(11) 0.0048(11) C28 0.0214(11) 0.0261(12) 0.0275(13) 0.0030(10) 0.0056(9) 0.0029(9) C29 0.0235(11) 0.0281(12) 0.0274(13) -0.0022(10) 0.0105(10) 0.0008(9) C30 0.0310(13) 0.0344(14) 0.0317(14) -0.0040(11) 0.0065(11) -0.0006(11) C31 0.0351(14) 0.0442(16) 0.0443(17) -0.0139(13) 0.0099(12) -0.0115(12) C32 0.0542(17) 0.0306(14) 0.0561(19) -0.0033(13) 0.0251(15) -0.0099(13) C33 0.0515(17) 0.0332(15) 0.0407(16) 0.0076(12) 0.0153(13) 0.0009(13) C34 0.0360(14) 0.0329(14) 0.0312(14) 0.0008(11) 0.0070(11) -0.0019(11) C35 0.0289(12) 0.0263(12) 0.0280(13) 0.0013(10) 0.0103(10) -0.0001(10) C36 0.0410(14) 0.0205(12) 0.0309(14) -0.0014(10) 0.0142(11) -0.0004(10) C37 0.0428(15) 0.0450(16) 0.0427(16) 0.0009(13) 0.0181(13) -0.0018(13) C38 0.0525(18) 0.0508(18) 0.068(2) 0.0058(16) 0.0368(17) 0.0001(14) C39 0.086(2) 0.0438(17) 0.056(2) 0.0086(15) 0.0494(19) 0.0097(16) C40 0.081(2) 0.0414(16) 0.0330(16) 0.0035(13) 0.0238(15) 0.0114(15) C41 0.0513(16) 0.0317(14) 0.0360(16) -0.0006(11) 0.0141(13) 0.0035(12) C42 0.0245(12) 0.0286(12) 0.0236(12) -0.0021(10) 0.0040(9) 0.0039(9) C43 0.0546(17) 0.0261(13) 0.0441(16) 0.0002(12) 0.0221(14) 0.0069(12) N1 0.0245(10) 0.0290(11) 0.0283(11) 0.0018(9) 0.0072(8) 0.0032(8) N2 0.0273(10) 0.0319(11) 0.0316(12) 0.0042(9) 0.0036(9) 0.0053(9) N3 0.0252(10) 0.0322(11) 0.0306(11) 0.0004(9) 0.0091(9) 0.0032(8) N4 0.0317(11) 0.0398(12) 0.0253(11) 0.0029(9) 0.0097(9) 0.0012(9) N5 0.0252(10) 0.0263(10) 0.0286(11) 0.0044(8) 0.0085(8) 0.0039(8) N6 0.0288(10) 0.0288(11) 0.0304(11) 0.0064(9) 0.0088(9) 0.0038(8) N7 0.0256(10) 0.0263(10) 0.0251(11) -0.0030(8) 0.0072(8) -0.0014(8) O1 0.0489(11) 0.0244(9) 0.0329(10) -0.0037(7) 0.0163(8) -0.0021(8) P1 0.0224(3) 0.0233(3) 0.0306(3) 0.0035(3) 0.0071(2) 0.0019(2) Ru1 0.02102(11) 0.02246(11) 0.02429(12) 0.00161(7) 0.00723(8) 0.00155(7) _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 N4 1.536(4) . ? B1 N6 1.541(4) . ? B1 N2 1.544(3) . ? B1 H1' 1.0000 . ? C1 N1 1.337(3) . ? C1 C2 1.396(4) . ? C1 H1 0.9500 . ? C2 C3 1.368(4) . ? C2 H2 0.9500 . ? C3 N2 1.346(3) . ? C3 H3 0.9500 . ? C4 N3 1.335(3) . ? C4 C5 1.386(4) . ? C4 H4 0.9500 . ? C5 C6 1.361(4) . ? C5 H5 0.9500 . ? C6 N4 1.351(3) . ? C6 H6 0.9500 . ? C7 N5 1.333(3) . ? C7 C8 1.384(3) . ? C7 H7 0.9500 . ? C8 C9 1.371(4) . ? C8 H8 0.9500 . ? C9 N6 1.342(3) . ? C9 H9 0.9500 . ? C10 C11 1.391(3) . ? C10 C15 1.395(3) . ? C10 P1 1.852(2) . ? C11 C12 1.388(3) . ? C11 H11 0.9500 . ? C12 C13 1.381(4) . ? C12 H12 0.9500 . ? C13 C14 1.376(4) . ? C13 H13 0.9500 . ? C14 C15 1.391(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.392(3) . ? C16 C17 1.392(4) . ? C16 P1 1.850(2) . ? C17 C18 1.389(4) . ? C17 H17 0.9500 . ? C18 C19 1.389(4) . ? C18 H18 0.9500 . ? C19 C20 1.374(4) . ? C19 H19 0.9500 . ? C20 C21 1.386(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.390(4) . ? C22 C23 1.397(4) . ? C22 P1 1.843(2) . ? C23 C24 1.388(4) . ? C23 H23 0.9500 . ? C24 C25 1.380(4) . ? C24 H24 0.9500 . ? C25 C26 1.375(4) . ? C25 H25 0.9500 . ? C26 C27 1.389(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 N7 1.307(3) . ? C28 C35 1.422(3) . ? C28 C29 1.481(3) . ? C29 C30 1.386(3) . ? C29 C34 1.394(3) . ? C30 C31 1.384(4) . ? C30 H30 0.9500 . ? C31 C32 1.370(4) . ? C31 H31 0.9500 . ? C32 C33 1.379(4) . ? C32 H32 0.9500 . ? C33 C34 1.376(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C42 1.404(3) . ? C35 C36 1.496(3) . ? C36 C41 1.384(4) . ? C36 C37 1.394(4) . ? C37 C38 1.390(4) . ? C37 H37 0.9500 . ? C38 C39 1.377(5) . ? C38 H38 0.9500 . ? C39 C40 1.377(5) . ? C39 H39 0.9500 . ? C40 C41 1.393(4) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 O1 1.370(3) . ? C42 Ru1 2.032(2) . ? C43 O1 1.419(3) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? N1 N2 1.360(3) . ? N1 Ru1 2.1282(19) . ? N3 N4 1.365(3) . ? N3 Ru1 2.1663(19) . ? N5 N6 1.376(3) . ? N5 Ru1 2.1580(19) . ? N7 Ru1 2.0334(18) . ? N7 H7' 0.8800 . ? P1 Ru1 2.3058(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 B1 N6 108.9(2) . . ? N4 B1 N2 108.1(2) . . ? N6 B1 N2 108.4(2) . . ? N4 B1 H1' 110.4 . . ? N6 B1 H1' 110.4 . . ? N2 B1 H1' 110.4 . . ? N1 C1 C2 110.2(2) . . ? N1 C1 H1 124.9 . . ? C2 C1 H1 124.9 . . ? C3 C2 C1 105.0(2) . . ? C3 C2 H2 127.5 . . ? C1 C2 H2 127.5 . . ? N2 C3 C2 108.7(2) . . ? N2 C3 H3 125.7 . . ? C2 C3 H3 125.7 . . ? N3 C4 C5 110.7(2) . . ? N3 C4 H4 124.6 . . ? C5 C4 H4 124.6 . . ? C6 C5 C4 105.2(2) . . ? C6 C5 H5 127.4 . . ? C4 C5 H5 127.4 . . ? N4 C6 C5 108.7(2) . . ? N4 C6 H6 125.7 . . ? C5 C6 H6 125.7 . . ? N5 C7 C8 111.4(2) . . ? N5 C7 H7 124.3 . . ? C8 C7 H7 124.3 . . ? C9 C8 C7 104.6(2) . . ? C9 C8 H8 127.7 . . ? C7 C8 H8 127.7 . . ? N6 C9 C8 109.0(2) . . ? N6 C9 H9 125.5 . . ? C8 C9 H9 125.5 . . ? C11 C10 C15 118.4(2) . . ? C11 C10 P1 118.22(18) . . ? C15 C10 P1 123.05(19) . . ? C12 C11 C10 120.7(2) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 119.7(2) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 120.3(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C10 120.6(3) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? C21 C16 C17 118.4(2) . . ? C21 C16 P1 121.8(2) . . ? C17 C16 P1 119.46(18) . . ? C18 C17 C16 120.9(2) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 119.8(3) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 119.7(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.6(3) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C16 120.6(3) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C27 C22 C23 118.2(2) . . ? C27 C22 P1 123.43(19) . . ? C23 C22 P1 118.32(19) . . ? C24 C23 C22 120.7(3) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 C23 120.2(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 C24 119.7(2) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.5(3) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C22 C27 C26 120.6(3) . . ? C22 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? N7 C28 C35 115.3(2) . . ? N7 C28 C29 120.9(2) . . ? C35 C28 C29 123.80(19) . . ? C30 C29 C34 118.1(2) . . ? C30 C29 C28 121.3(2) . . ? C34 C29 C28 120.4(2) . . ? C31 C30 C29 121.2(2) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C32 C31 C30 119.8(3) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 119.9(3) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 120.5(3) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C29 120.4(2) . . ? C33 C34 H34 119.8 . . ? C29 C34 H34 119.8 . . ? C42 C35 C28 112.68(19) . . ? C42 C35 C36 124.8(2) . . ? C28 C35 C36 121.7(2) . . ? C41 C36 C37 117.8(2) . . ? C41 C36 C35 121.2(2) . . ? C37 C36 C35 121.0(2) . . ? C38 C37 C36 121.3(3) . . ? C38 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? C39 C38 C37 119.9(3) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 119.6(3) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 120.4(3) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C36 C41 C40 120.9(3) . . ? C36 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? O1 C42 C35 110.34(19) . . ? O1 C42 Ru1 132.78(16) . . ? C35 C42 Ru1 116.32(16) . . ? O1 C43 H43A 109.5 . . ? O1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C1 N1 N2 106.55(19) . . ? C1 N1 Ru1 132.94(17) . . ? N2 N1 Ru1 120.50(13) . . ? C3 N2 N1 109.60(19) . . ? C3 N2 B1 131.2(2) . . ? N1 N2 B1 119.20(18) . . ? C4 N3 N4 106.1(2) . . ? C4 N3 Ru1 134.32(17) . . ? N4 N3 Ru1 119.23(14) . . ? C6 N4 N3 109.3(2) . . ? C6 N4 B1 130.7(2) . . ? N3 N4 B1 119.67(18) . . ? C7 N5 N6 105.57(18) . . ? C7 N5 Ru1 137.43(16) . . ? N6 N5 Ru1 116.98(14) . . ? C9 N6 N5 109.4(2) . . ? C9 N6 B1 128.6(2) . . ? N5 N6 B1 122.01(19) . . ? C28 N7 Ru1 118.79(15) . . ? C28 N7 H7' 120.6 . . ? Ru1 N7 H7' 120.6 . . ? C42 O1 C43 120.03(18) . . ? C22 P1 C16 103.05(11) . . ? C22 P1 C10 100.79(10) . . ? C16 P1 C10 98.68(11) . . ? C22 P1 Ru1 116.01(7) . . ? C16 P1 Ru1 116.93(8) . . ? C10 P1 Ru1 118.48(8) . . ? C42 Ru1 N7 76.79(8) . . ? C42 Ru1 N1 87.39(8) . . ? N7 Ru1 N1 89.84(7) . . ? C42 Ru1 N5 106.40(8) . . ? N7 Ru1 N5 174.52(7) . . ? N1 Ru1 N5 85.89(7) . . ? C42 Ru1 N3 164.82(8) . . ? N7 Ru1 N3 90.87(7) . . ? N1 Ru1 N3 83.72(7) . . ? N5 Ru1 N3 85.25(7) . . ? C42 Ru1 P1 91.69(7) . . ? N7 Ru1 P1 91.05(5) . . ? N1 Ru1 P1 178.54(5) . . ? N5 Ru1 P1 93.29(5) . . ? N3 Ru1 P1 97.42(5) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.648 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.052 # Attachment '- 6.cif' data_a12437 _database_code_depnum_ccdc_archive 'CCDC 830357' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H42 B N6 O P Ru' _chemical_formula_sum 'C45 H42 B N6 O P Ru' _chemical_formula_weight 825.70 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 24.6370(10) _cell_length_b 10.0656(4) _cell_length_c 32.0278(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.513(2) _cell_angle_gamma 90.00 _cell_volume 7939.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour green(dark) _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8243 _exptl_absorpt_correction_T_max 0.9765 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53461 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13970 _reflns_number_gt 10303 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0542P)^2^+0.0772P] 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 13970 _refine_ls_number_parameters 995 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.013 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 C1 C 0.34924(16) -0.1363(4) 0.05887(13) 0.0301(10) Uani 1 1 d . . . H1 H 0.3283 -0.1386 0.0833 0.036 Uiso 1 1 calc R . . C2 C 0.39083(16) -0.2247(4) 0.05017(13) 0.0375(11) Uani 1 1 d . . . H2 H 0.4035 -0.2966 0.0669 0.045 Uiso 1 1 calc R . . C3 C 0.40955(16) -0.1855(4) 0.01215(14) 0.0347(11) Uani 1 1 d . . . H3 H 0.4383 -0.2262 -0.0023 0.042 Uiso 1 1 calc R . . C4 C 0.24057(17) 0.0513(4) -0.06766(13) 0.0305(10) Uani 1 1 d . . . H4 H 0.2044 0.0749 -0.0613 0.037 Uiso 1 1 calc R . . C5 C 0.25634(18) 0.0037(4) -0.10601(13) 0.0381(11) Uani 1 1 d . . . H5 H 0.2342 -0.0108 -0.1303 0.046 Uiso 1 1 calc R . . C6 C 0.31093(18) -0.0181(4) -0.10118(13) 0.0364(11) Uani 1 1 d . . . H6 H 0.3339 -0.0512 -0.1221 0.044 Uiso 1 1 calc R . . C7 C 0.39671(15) 0.3315(4) 0.00637(13) 0.0295(10) Uani 1 1 d . . . H7 H 0.3843 0.4006 0.0239 0.035 Uiso 1 1 calc R . . C8 C 0.44466(16) 0.3360(4) -0.01558(13) 0.0383(11) Uani 1 1 d . . . H8 H 0.4706 0.4058 -0.0159 0.046 Uiso 1 1 calc R . . C9 C 0.44621(16) 0.2174(4) -0.03674(13) 0.0363(11) Uani 1 1 d . . . H9 H 0.4740 0.1898 -0.0548 0.044 Uiso 1 1 calc R . . C10 C 0.27905(14) 0.4279(4) -0.03107(12) 0.0231(9) Uani 1 1 d . . . C11 C 0.29607(15) 0.3721(4) -0.06849(12) 0.0262(9) Uani 1 1 d . . . H11 H 0.2896 0.2807 -0.0741 0.031 Uiso 1 1 calc R . . C12 C 0.32223(15) 0.4496(4) -0.09747(13) 0.0326(10) Uani 1 1 d . . . H12 H 0.3335 0.4111 -0.1229 0.039 Uiso 1 1 calc R . . C13 C 0.33214(15) 0.5834(4) -0.08962(14) 0.0335(11) Uani 1 1 d . . . H13 H 0.3503 0.6363 -0.1095 0.040 Uiso 1 1 calc R . . C14 C 0.31537(15) 0.6385(4) -0.05281(14) 0.0322(10) Uani 1 1 d . . . H14 H 0.3221 0.7299 -0.0474 0.039 Uiso 1 1 calc R . . C15 C 0.28890(15) 0.5626(4) -0.02357(13) 0.0297(10) Uani 1 1 d . . . H15 H 0.2774 0.6023 0.0016 0.036 Uiso 1 1 calc R . . C16 C 0.24105(15) 0.4363(3) 0.05242(12) 0.0237(9) Uani 1 1 d . . . C17 C 0.28538(16) 0.4554(4) 0.08008(12) 0.0304(10) Uani 1 1 d . . . H17 H 0.3166 0.4008 0.0778 0.036 Uiso 1 1 calc R . . C18 C 0.28437(19) 0.5524(4) 0.11066(14) 0.0433(12) Uani 1 1 d . . . H18 H 0.3147 0.5633 0.1293 0.052 Uiso 1 1 calc R . . C19 C 0.23970(19) 0.6328(4) 0.11415(14) 0.0431(12) Uani 1 1 d . . . H19 H 0.2393 0.6998 0.1350 0.052 Uiso 1 1 calc R . . C20 C 0.19555(18) 0.6168(4) 0.08751(14) 0.0406(12) Uani 1 1 d . . . H20 H 0.1647 0.6724 0.0901 0.049 Uiso 1 1 calc R . . C21 C 0.19605(16) 0.5192(4) 0.05685(13) 0.0320(10) Uani 1 1 d . . . H21 H 0.1653 0.5086 0.0386 0.038 Uiso 1 1 calc R . . C22 C 0.17690(14) 0.3059(3) -0.01045(12) 0.0234(9) Uani 1 1 d . . . C23 C 0.13833(15) 0.2624(4) 0.01791(13) 0.0301(10) Uani 1 1 d . . . H23 H 0.1491 0.2435 0.0460 0.036 Uiso 1 1 calc R . . C24 C 0.08441(16) 0.2470(4) 0.00518(14) 0.0362(11) Uani 1 1 d . . . H24 H 0.0585 0.2191 0.0248 0.043 Uiso 1 1 calc R . . C25 C 0.06811(17) 0.2718(4) -0.03558(15) 0.0375(11) Uani 1 1 d . . . H25 H 0.0311 0.2609 -0.0441 0.045 Uiso 1 1 calc R . . C26 C 0.10571(16) 0.3122(4) -0.06383(14) 0.0359(11) Uani 1 1 d . . . H26 H 0.0948 0.3279 -0.0921 0.043 Uiso 1 1 calc R . . C27 C 0.16000(16) 0.3306(4) -0.05125(13) 0.0316(10) Uani 1 1 d . . . H27 H 0.1855 0.3602 -0.0709 0.038 Uiso 1 1 calc R . . C28 C 0.27459(15) 0.1232(4) 0.10737(12) 0.0254(9) Uani 1 1 d . . . C29 C 0.28349(17) 0.1427(4) 0.15398(12) 0.0325(10) Uani 1 1 d . . . H29A H 0.2504 0.1811 0.1660 0.039 Uiso 1 1 calc R . . H29B H 0.3138 0.2055 0.1591 0.039 Uiso 1 1 calc R . . C30 C 0.29649(16) 0.0109(4) 0.17494(12) 0.0295(10) Uani 1 1 d . . . C31 C 0.34758(16) -0.0444(5) 0.17271(13) 0.0407(12) Uani 1 1 d . . . H31 H 0.3754 0.0025 0.1589 0.049 Uiso 1 1 calc R . . C32 C 0.35893(18) -0.1672(5) 0.19031(14) 0.0474(13) Uani 1 1 d . . . H32 H 0.3943 -0.2035 0.1882 0.057 Uiso 1 1 calc R . . C33 C 0.31951(19) -0.2387(5) 0.21107(14) 0.0425(12) Uani 1 1 d . . . C34 C 0.3321(2) -0.3721(5) 0.23014(16) 0.0622(15) Uani 1 1 d . . . H34A H 0.3306 -0.3656 0.2606 0.093 Uiso 1 1 calc R . . H34B H 0.3685 -0.4002 0.2223 0.093 Uiso 1 1 calc R . . H34C H 0.3053 -0.4373 0.2199 0.093 Uiso 1 1 calc R . . C35 C 0.26872(18) -0.1815(5) 0.21373(14) 0.0443(12) Uani 1 1 d . . . H35 H 0.2411 -0.2275 0.2280 0.053 Uiso 1 1 calc R . . C36 C 0.25718(16) -0.0591(4) 0.19617(13) 0.0356(11) Uani 1 1 d . . . H36 H 0.2219 -0.0223 0.1986 0.043 Uiso 1 1 calc R . . C37 C 0.23083(15) 0.0514(4) 0.08972(12) 0.0262(9) Uani 1 1 d . . . H37 H 0.2022 0.0180 0.1060 0.031 Uiso 1 1 calc R . . C38 C 0.23242(14) 0.0327(3) 0.04660(11) 0.0208(9) Uani 1 1 d . . . C39 C 0.19163(14) -0.0590(3) 0.02738(11) 0.0200(8) Uani 1 1 d . . . C40 C 0.20718(15) -0.1553(4) -0.00147(12) 0.0269(9) Uani 1 1 d . . . H40 H 0.2440 -0.1593 -0.0095 0.032 Uiso 1 1 calc R . . C41 C 0.17006(15) -0.2450(4) -0.01862(12) 0.0282(10) Uani 1 1 d . . . H41 H 0.1820 -0.3098 -0.0379 0.034 Uiso 1 1 calc R . . C42 C 0.11558(15) -0.2418(4) -0.00807(12) 0.0262(9) Uani 1 1 d . . . C43 C 0.10000(15) -0.1456(4) 0.02010(12) 0.0274(10) Uani 1 1 d . . . H43 H 0.0629 -0.1396 0.0272 0.033 Uiso 1 1 calc R . . C44 C 0.13695(14) -0.0581(4) 0.03819(12) 0.0250(9) Uani 1 1 d . . . H44 H 0.1250 0.0039 0.0583 0.030 Uiso 1 1 calc R . . C45 C 0.07536(17) -0.3398(4) -0.02677(15) 0.0447(12) Uani 1 1 d . . . H45A H 0.0517 -0.3725 -0.0049 0.067 Uiso 1 1 calc R . . H45B H 0.0950 -0.4147 -0.0389 0.067 Uiso 1 1 calc R . . H45C H 0.0534 -0.2959 -0.0487 0.067 Uiso 1 1 calc R . . C46 C 0.45095(16) 0.3946(4) 0.24523(13) 0.0324(10) Uani 1 1 d . . . H46 H 0.4702 0.3903 0.2199 0.039 Uiso 1 1 calc R . . C47 C 0.41090(17) 0.3058(4) 0.25679(14) 0.0396(11) Uani 1 1 d . . . H47 H 0.3978 0.2310 0.2415 0.047 Uiso 1 1 calc R . . C48 C 0.39422(16) 0.3486(4) 0.29495(14) 0.0351(11) Uani 1 1 d . . . H48 H 0.3668 0.3085 0.3111 0.042 Uiso 1 1 calc R . . C49 C 0.40399(16) 0.8636(4) 0.29598(13) 0.0305(10) Uani 1 1 d . . . H49 H 0.4133 0.9292 0.2761 0.037 Uiso 1 1 calc R . . C50 C 0.36002(17) 0.8730(4) 0.32224(14) 0.0392(11) Uani 1 1 d . . . H50 H 0.3344 0.9433 0.3238 0.047 Uiso 1 1 calc R . . C51 C 0.36194(15) 0.7587(4) 0.34519(13) 0.0366(11) Uani 1 1 d . . . H51 H 0.3373 0.7349 0.3662 0.044 Uiso 1 1 calc R . . C52 C 0.56830(16) 0.5923(3) 0.36484(12) 0.0254(9) Uani 1 1 d . . . H52 H 0.6036 0.6177 0.3566 0.031 Uiso 1 1 calc R . . C53 C 0.55635(17) 0.5430(4) 0.40396(13) 0.0344(10) Uani 1 1 d . . . H53 H 0.5806 0.5291 0.4271 0.041 Uiso 1 1 calc R . . C54 C 0.50117(17) 0.5188(4) 0.40159(13) 0.0347(11) Uani 1 1 d . . . H54 H 0.4803 0.4839 0.4236 0.042 Uiso 1 1 calc R . . C55 C 0.52004(15) 0.9672(4) 0.33046(12) 0.0239(9) Uani 1 1 d . . . C56 C 0.49989(15) 0.9114(4) 0.36676(12) 0.0303(10) Uani 1 1 d . . . H56 H 0.5044 0.8190 0.3717 0.036 Uiso 1 1 calc R . . C57 C 0.47340(16) 0.9884(4) 0.39565(13) 0.0358(11) Uani 1 1 d . . . H57 H 0.4597 0.9486 0.4201 0.043 Uiso 1 1 calc R . . C58 C 0.46695(16) 1.1233(4) 0.38890(14) 0.0360(11) Uani 1 1 d . . . H58 H 0.4482 1.1765 0.4083 0.043 Uiso 1 1 calc R . . C59 C 0.48811(16) 1.1798(4) 0.35351(14) 0.0379(11) Uani 1 1 d . . . H59 H 0.4847 1.2728 0.3492 0.045 Uiso 1 1 calc R . . C60 C 0.51421(15) 1.1032(4) 0.32434(13) 0.0296(10) Uani 1 1 d . . . H60 H 0.5282 1.1436 0.3001 0.036 Uiso 1 1 calc R . . C61 C 0.56074(16) 0.9731(4) 0.24762(12) 0.0259(9) Uani 1 1 d . . . C62 C 0.51591(17) 0.9968(4) 0.22118(12) 0.0354(11) Uani 1 1 d . . . H62 H 0.4836 0.9469 0.2243 0.043 Uiso 1 1 calc R . . C63 C 0.5184(2) 1.0935(4) 0.19031(14) 0.0485(13) Uani 1 1 d . . . H63 H 0.4877 1.1100 0.1726 0.058 Uiso 1 1 calc R . . C64 C 0.5653(2) 1.1654(5) 0.18532(15) 0.0542(14) Uani 1 1 d . . . H64 H 0.5667 1.2312 0.1641 0.065 Uiso 1 1 calc R . . C65 C 0.6099(2) 1.1427(4) 0.21076(15) 0.0511(13) Uani 1 1 d . . . H65 H 0.6422 1.1920 0.2070 0.061 Uiso 1 1 calc R . . C66 C 0.60769(17) 1.0475(4) 0.24213(13) 0.0358(11) Uani 1 1 d . . . H66 H 0.6385 1.0330 0.2600 0.043 Uiso 1 1 calc R . . C67 C 0.62196(15) 0.8473(3) 0.31298(12) 0.0240(9) Uani 1 1 d . . . C68 C 0.63906(17) 0.8973(4) 0.35159(13) 0.0333(10) Uani 1 1 d . . . H68 H 0.6143 0.9459 0.3680 0.040 Uiso 1 1 calc R . . C69 C 0.69203(18) 0.8770(4) 0.36654(14) 0.0388(11) Uani 1 1 d . . . H69 H 0.7031 0.9118 0.3930 0.047 Uiso 1 1 calc R . . C70 C 0.72839(17) 0.8068(4) 0.34321(14) 0.0378(11) Uani 1 1 d . . . H70 H 0.7644 0.7924 0.3535 0.045 Uiso 1 1 calc R . . C71 C 0.71208(16) 0.7575(4) 0.30475(14) 0.0370(11) Uani 1 1 d . . . H71 H 0.7370 0.7089 0.2886 0.044 Uiso 1 1 calc R . . C72 C 0.65966(16) 0.7781(4) 0.28941(13) 0.0308(10) Uani 1 1 d . . . H72 H 0.6492 0.7450 0.2626 0.037 Uiso 1 1 calc R . . C73 C 0.51807(16) 0.6573(4) 0.19183(12) 0.0264(9) Uani 1 1 d . . . C74 C 0.50418(17) 0.6712(4) 0.14569(12) 0.0341(10) Uani 1 1 d . . . H74A H 0.5355 0.7092 0.1311 0.041 Uiso 1 1 calc R . . H74B H 0.4730 0.7323 0.1417 0.041 Uiso 1 1 calc R . . C75 C 0.49006(16) 0.5363(4) 0.12728(12) 0.0290(10) Uani 1 1 d . . . C76 C 0.44096(16) 0.4738(5) 0.13484(13) 0.0389(11) Uani 1 1 d . . . H76 H 0.4142 0.5189 0.1503 0.047 Uiso 1 1 calc R . . C77 C 0.43050(17) 0.3468(5) 0.12017(14) 0.0420(12) Uani 1 1 d . . . H77 H 0.3966 0.3065 0.1259 0.050 Uiso 1 1 calc R . . C78 C 0.46777(17) 0.2773(4) 0.09756(13) 0.0346(10) Uani 1 1 d . . . C79 C 0.45661(19) 0.1375(4) 0.08197(15) 0.0496(13) Uani 1 1 d . . . H79A H 0.4776 0.0740 0.0990 0.074 Uiso 1 1 calc R . . H79B H 0.4672 0.1302 0.0528 0.074 Uiso 1 1 calc R . . H79C H 0.4178 0.1179 0.0840 0.074 Uiso 1 1 calc R . . C80 C 0.51623(17) 0.3399(4) 0.08956(13) 0.0362(11) Uani 1 1 d . . . H80 H 0.5428 0.2946 0.0740 0.043 Uiso 1 1 calc R . . C81 C 0.52692(16) 0.4673(4) 0.10382(12) 0.0329(10) Uani 1 1 d . . . H81 H 0.5604 0.5083 0.0973 0.040 Uiso 1 1 calc R . . C82 C 0.56352(15) 0.5864(4) 0.20720(12) 0.0284(10) Uani 1 1 d . . . H82 H 0.5902 0.5518 0.1893 0.034 Uiso 1 1 calc R . . C83 C 0.56680(14) 0.5702(3) 0.25021(12) 0.0213(9) Uani 1 1 d . . . C84 C 0.60966(15) 0.4794(4) 0.26656(12) 0.0242(9) Uani 1 1 d . . . C85 C 0.59915(16) 0.3870(4) 0.29786(12) 0.0267(9) Uani 1 1 d . . . H85 H 0.5637 0.3817 0.3087 0.032 Uiso 1 1 calc R . . C86 C 0.63955(17) 0.3025(4) 0.31344(13) 0.0338(10) Uani 1 1 d . . . H86 H 0.6309 0.2393 0.3343 0.041 Uiso 1 1 calc R . . C87 C 0.69207(17) 0.3084(4) 0.29931(14) 0.0365(11) Uani 1 1 d . . . C88 C 0.70272(16) 0.4002(4) 0.26834(14) 0.0386(11) Uani 1 1 d . . . H88 H 0.7386 0.4076 0.2585 0.046 Uiso 1 1 calc R . . C89 C 0.66244(15) 0.4813(4) 0.25138(12) 0.0295(10) Uani 1 1 d . . . H89 H 0.6708 0.5392 0.2290 0.035 Uiso 1 1 calc R . . C90 C 0.73613(19) 0.2186(5) 0.31712(16) 0.0581(14) Uani 1 1 d . . . H90A H 0.7280 0.1959 0.3461 0.087 Uiso 1 1 calc R . . H90B H 0.7712 0.2645 0.3164 0.087 Uiso 1 1 calc R . . H90C H 0.7378 0.1372 0.3004 0.087 Uiso 1 1 calc R . . B1 B 0.38393(18) 0.0064(5) -0.04079(15) 0.0310(12) Uani 1 1 d . . . H1A H 0.4106 -0.0326 -0.0604 0.037 Uiso 1 1 calc R . . B2 B 0.42322(19) 0.5446(5) 0.34478(15) 0.0316(12) Uani 1 1 d . . . H2A H 0.3983 0.5056 0.3657 0.038 Uiso 1 1 calc R . . N1 N 0.34295(11) -0.0484(3) 0.02824(10) 0.0242(8) Uani 1 1 d . . . N2 N 0.38029(12) -0.0790(3) -0.00138(10) 0.0264(8) Uani 1 1 d . . . N3 N 0.28281(12) 0.0599(3) -0.04072(9) 0.0227(7) Uani 1 1 d . . . N4 N 0.32691(12) 0.0148(3) -0.06201(10) 0.0265(8) Uani 1 1 d . . . N5 N 0.37046(11) 0.2175(3) -0.00051(9) 0.0230(7) Uani 1 1 d . . . N6 N 0.40158(12) 0.1465(3) -0.02747(10) 0.0279(8) Uani 1 1 d . . . N7 N 0.45862(12) 0.4868(3) 0.27468(10) 0.0245(7) Uani 1 1 d . . . N8 N 0.42343(12) 0.4581(3) 0.30585(10) 0.0270(8) Uani 1 1 d . . . N9 N 0.43132(12) 0.7506(3) 0.30237(9) 0.0245(8) Uani 1 1 d . . . N10 N 0.40452(12) 0.6849(3) 0.33316(10) 0.0287(8) Uani 1 1 d . . . N11 N 0.52380(12) 0.5993(3) 0.34032(9) 0.0219(7) Uani 1 1 d . . . N12 N 0.48165(12) 0.5521(3) 0.36356(9) 0.0243(8) Uani 1 1 d . . . O1 O 0.31064(10) 0.1677(2) 0.08307(8) 0.0240(6) Uani 1 1 d . . . O2 O 0.48483(9) 0.7050(2) 0.21787(8) 0.0246(6) Uani 1 1 d . . . P1 P 0.24768(4) 0.31991(9) 0.00861(3) 0.0214(2) Uani 1 1 d . . . P2 P 0.55234(4) 0.85844(9) 0.29180(3) 0.0220(2) Uani 1 1 d . . . Ru1 Ru 0.294732(12) 0.12466(3) 0.020214(10) 0.01962(9) Uani 1 1 d . . . Ru2 Ru 0.506197(12) 0.66149(3) 0.279908(9) 0.01965(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 C1 0.032(2) 0.030(2) 0.027(2) 0.0082(19) -0.0057(19) 0.0003(19) C2 0.043(3) 0.032(2) 0.036(3) 0.004(2) -0.007(2) 0.015(2) C3 0.030(2) 0.031(2) 0.043(3) -0.005(2) -0.005(2) 0.0153(19) C4 0.036(2) 0.019(2) 0.036(3) -0.0030(19) -0.011(2) -0.0022(18) C5 0.052(3) 0.029(2) 0.032(3) -0.003(2) -0.020(2) -0.003(2) C6 0.055(3) 0.033(2) 0.021(2) -0.004(2) 0.001(2) 0.007(2) C7 0.030(2) 0.026(2) 0.032(3) 0.0051(19) -0.0119(19) -0.0051(18) C8 0.034(3) 0.041(3) 0.040(3) 0.010(2) -0.004(2) -0.018(2) C9 0.026(2) 0.051(3) 0.032(3) 0.007(2) 0.002(2) -0.009(2) C10 0.020(2) 0.023(2) 0.026(2) 0.0067(18) -0.0074(17) 0.0001(17) C11 0.029(2) 0.020(2) 0.029(2) 0.0019(18) -0.0055(18) -0.0060(17) C12 0.031(2) 0.037(3) 0.030(3) 0.004(2) 0.000(2) 0.000(2) C13 0.023(2) 0.035(2) 0.043(3) 0.014(2) 0.000(2) -0.0043(19) C14 0.029(2) 0.019(2) 0.048(3) 0.008(2) -0.005(2) -0.0026(18) C15 0.029(2) 0.022(2) 0.038(3) -0.0011(19) -0.004(2) 0.0000(18) C16 0.030(2) 0.018(2) 0.023(2) 0.0036(17) 0.0005(18) -0.0020(17) C17 0.037(3) 0.024(2) 0.030(2) -0.0031(19) -0.005(2) 0.0007(19) C18 0.055(3) 0.037(3) 0.038(3) -0.008(2) -0.013(2) -0.002(2) C19 0.059(3) 0.036(3) 0.034(3) -0.013(2) -0.003(2) 0.002(2) C20 0.046(3) 0.034(3) 0.042(3) -0.009(2) 0.004(2) 0.009(2) C21 0.032(2) 0.030(2) 0.034(3) 0.000(2) -0.001(2) 0.0041(19) C22 0.023(2) 0.0150(19) 0.032(3) 0.0017(17) -0.0025(18) 0.0019(16) C23 0.029(2) 0.029(2) 0.032(3) 0.0061(19) -0.0039(19) 0.0011(18) C24 0.025(2) 0.034(3) 0.050(3) 0.009(2) 0.002(2) -0.0021(19) C25 0.025(2) 0.033(2) 0.054(3) -0.001(2) -0.011(2) -0.0048(19) C26 0.035(3) 0.039(3) 0.033(3) -0.003(2) -0.013(2) 0.002(2) C27 0.032(2) 0.033(2) 0.029(3) 0.000(2) -0.006(2) 0.0005(19) C28 0.028(2) 0.023(2) 0.025(2) -0.0024(18) -0.0049(18) 0.0060(18) C29 0.033(2) 0.036(3) 0.027(2) -0.005(2) -0.0040(19) 0.0002(19) C30 0.030(2) 0.040(3) 0.018(2) -0.0079(19) -0.0056(18) 0.003(2) C31 0.030(2) 0.059(3) 0.033(3) 0.015(2) 0.001(2) 0.003(2) C32 0.038(3) 0.068(3) 0.036(3) 0.006(3) -0.005(2) 0.015(3) C33 0.052(3) 0.046(3) 0.028(3) 0.006(2) -0.012(2) 0.004(2) C34 0.076(4) 0.054(3) 0.055(4) 0.014(3) -0.013(3) 0.007(3) C35 0.045(3) 0.056(3) 0.032(3) 0.010(2) 0.004(2) -0.006(2) C36 0.026(2) 0.051(3) 0.029(3) 0.000(2) 0.0030(19) 0.003(2) C37 0.027(2) 0.027(2) 0.025(2) -0.0007(18) 0.0051(18) 0.0018(18) C38 0.022(2) 0.0157(19) 0.025(2) 0.0011(17) -0.0021(17) 0.0080(16) C39 0.024(2) 0.0162(19) 0.020(2) 0.0064(16) -0.0001(17) 0.0006(16) C40 0.026(2) 0.021(2) 0.033(3) 0.0019(18) 0.0046(19) 0.0027(17) C41 0.034(2) 0.021(2) 0.030(2) -0.0053(18) 0.0038(19) 0.0001(18) C42 0.026(2) 0.019(2) 0.034(3) 0.0025(18) -0.0041(18) -0.0058(17) C43 0.023(2) 0.028(2) 0.030(2) -0.0034(19) 0.0004(18) 0.0001(18) C44 0.027(2) 0.021(2) 0.028(2) -0.0021(18) 0.0046(18) -0.0018(17) C45 0.037(3) 0.041(3) 0.056(3) -0.014(2) -0.004(2) -0.008(2) C46 0.037(3) 0.025(2) 0.035(3) -0.005(2) -0.002(2) 0.0007(19) C47 0.043(3) 0.025(2) 0.051(3) -0.007(2) -0.008(2) -0.008(2) C48 0.032(2) 0.025(2) 0.049(3) 0.009(2) -0.003(2) -0.0095(19) C49 0.031(2) 0.030(2) 0.029(2) 0.0023(19) -0.0056(19) 0.0050(19) C50 0.034(3) 0.034(3) 0.049(3) -0.002(2) 0.003(2) 0.012(2) C51 0.028(2) 0.044(3) 0.038(3) -0.007(2) 0.009(2) 0.005(2) C52 0.030(2) 0.017(2) 0.029(2) 0.0033(18) -0.0050(19) 0.0028(17) C53 0.048(3) 0.029(2) 0.026(3) 0.0052(19) -0.007(2) 0.003(2) C54 0.050(3) 0.032(2) 0.022(2) 0.007(2) 0.005(2) -0.001(2) C55 0.028(2) 0.024(2) 0.019(2) -0.0016(17) -0.0062(17) 0.0033(17) C56 0.038(2) 0.022(2) 0.031(2) -0.0029(19) 0.000(2) 0.0047(19) C57 0.041(3) 0.038(3) 0.028(3) -0.006(2) 0.001(2) 0.001(2) C58 0.026(2) 0.042(3) 0.039(3) -0.018(2) -0.005(2) 0.008(2) C59 0.041(3) 0.024(2) 0.048(3) -0.004(2) -0.012(2) 0.009(2) C60 0.037(2) 0.019(2) 0.032(3) -0.0013(19) -0.005(2) 0.0043(18) C61 0.041(2) 0.018(2) 0.019(2) -0.0011(17) 0.0042(19) -0.0005(18) C62 0.046(3) 0.032(2) 0.028(3) 0.009(2) -0.006(2) 0.003(2) C63 0.074(4) 0.042(3) 0.029(3) 0.009(2) -0.012(3) 0.004(3) C64 0.092(4) 0.040(3) 0.031(3) 0.019(2) -0.002(3) -0.007(3) C65 0.068(4) 0.042(3) 0.044(3) 0.011(2) 0.005(3) -0.017(3) C66 0.046(3) 0.032(2) 0.029(3) 0.008(2) -0.002(2) -0.002(2) C67 0.031(2) 0.016(2) 0.024(2) 0.0049(17) -0.0041(18) -0.0036(17) C68 0.038(3) 0.031(2) 0.031(3) 0.002(2) -0.002(2) -0.001(2) C69 0.046(3) 0.041(3) 0.029(3) 0.004(2) -0.014(2) -0.009(2) C70 0.034(3) 0.034(3) 0.045(3) 0.004(2) -0.009(2) -0.002(2) C71 0.032(3) 0.032(2) 0.047(3) -0.002(2) 0.002(2) 0.002(2) C72 0.033(2) 0.027(2) 0.032(3) -0.0014(19) 0.000(2) -0.0035(19) C73 0.035(2) 0.020(2) 0.024(2) 0.0006(18) -0.0013(19) -0.0034(18) C74 0.044(3) 0.039(3) 0.019(2) 0.008(2) -0.003(2) 0.009(2) C75 0.032(2) 0.040(3) 0.015(2) 0.0008(19) -0.0086(18) 0.002(2) C76 0.031(2) 0.053(3) 0.033(3) 0.004(2) -0.001(2) 0.007(2) C77 0.029(2) 0.061(3) 0.036(3) 0.004(2) -0.005(2) -0.011(2) C78 0.036(3) 0.042(3) 0.025(2) 0.001(2) -0.012(2) 0.003(2) C79 0.056(3) 0.047(3) 0.044(3) 0.002(2) -0.018(2) -0.008(2) C80 0.033(3) 0.053(3) 0.023(2) -0.006(2) -0.0001(19) 0.003(2) C81 0.030(2) 0.046(3) 0.023(2) 0.000(2) -0.0006(19) 0.001(2) C82 0.029(2) 0.028(2) 0.028(2) 0.0018(19) 0.0072(19) 0.0066(18) C83 0.022(2) 0.0162(19) 0.026(2) 0.0010(17) -0.0018(17) -0.0024(16) C84 0.030(2) 0.019(2) 0.023(2) -0.0046(17) 0.0010(18) 0.0005(17) C85 0.033(2) 0.022(2) 0.026(2) -0.0018(18) 0.0006(19) 0.0052(18) C86 0.051(3) 0.022(2) 0.028(3) 0.0029(19) 0.001(2) 0.007(2) C87 0.040(3) 0.032(2) 0.038(3) -0.009(2) -0.005(2) 0.016(2) C88 0.026(2) 0.037(3) 0.052(3) -0.008(2) 0.001(2) 0.010(2) C89 0.029(2) 0.028(2) 0.032(3) -0.0001(19) 0.0083(19) 0.0046(18) C90 0.060(3) 0.051(3) 0.062(4) 0.000(3) -0.012(3) 0.029(3) B1 0.028(3) 0.034(3) 0.031(3) -0.003(2) 0.003(2) 0.002(2) B2 0.032(3) 0.035(3) 0.029(3) 0.010(2) 0.006(2) 0.000(2) N1 0.0208(17) 0.0259(18) 0.0261(19) 0.0012(15) 0.0015(15) 0.0007(14) N2 0.0246(18) 0.0242(18) 0.030(2) -0.0039(15) 0.0008(15) 0.0025(15) N3 0.0257(18) 0.0181(16) 0.0241(19) -0.0018(14) -0.0050(15) -0.0030(14) N4 0.0339(19) 0.0236(18) 0.0220(19) -0.0016(15) 0.0020(16) 0.0007(15) N5 0.0218(17) 0.0250(18) 0.0220(19) 0.0015(15) -0.0038(14) 0.0003(14) N6 0.0263(19) 0.0301(19) 0.027(2) 0.0016(16) 0.0024(15) -0.0023(15) N7 0.0265(18) 0.0243(18) 0.0227(19) 0.0041(15) -0.0014(15) 0.0019(14) N8 0.0258(18) 0.0231(18) 0.032(2) 0.0053(16) -0.0005(16) 0.0005(15) N9 0.0267(18) 0.0249(18) 0.0220(19) 0.0039(15) -0.0004(15) 0.0037(15) N10 0.0279(19) 0.0311(19) 0.027(2) 0.0028(16) 0.0039(16) 0.0051(16) N11 0.0255(18) 0.0178(16) 0.0225(18) 0.0036(14) 0.0041(15) 0.0030(14) N12 0.0332(19) 0.0219(17) 0.0179(18) 0.0039(14) 0.0030(15) 0.0027(15) O1 0.0254(14) 0.0231(14) 0.0232(15) 0.0012(12) -0.0043(12) 0.0004(11) O2 0.0278(15) 0.0251(14) 0.0209(15) -0.0005(12) -0.0009(12) 0.0047(12) P1 0.0232(5) 0.0177(5) 0.0231(6) 0.0003(4) -0.0046(4) -0.0007(4) P2 0.0293(6) 0.0180(5) 0.0185(6) 0.0030(4) -0.0017(4) 0.0015(4) Ru1 0.02011(17) 0.01725(17) 0.02135(19) 0.00026(13) -0.00244(13) -0.00088(13) Ru2 0.02316(18) 0.01737(17) 0.01838(18) 0.00157(13) -0.00002(13) 0.00201(13) _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 C1 N1 1.327(4) . ? C1 C2 1.390(5) . ? C1 H1 0.9500 . ? C2 C3 1.371(5) . ? C2 H2 0.9500 . ? C3 N2 1.357(5) . ? C3 H3 0.9500 . ? C4 N3 1.337(5) . ? C4 C5 1.384(5) . ? C4 H4 0.9500 . ? C5 C6 1.367(5) . ? C5 H5 0.9500 . ? C6 N4 1.346(5) . ? C6 H6 0.9500 . ? C7 N5 1.333(4) . ? C7 C8 1.391(5) . ? C7 H7 0.9500 . ? C8 C9 1.374(6) . ? C8 H8 0.9500 . ? C9 N6 1.350(5) . ? C9 H9 0.9500 . ? C10 C11 1.398(5) . ? C10 C15 1.397(5) . ? C10 P1 1.856(4) . ? C11 C12 1.385(5) . ? C11 H11 0.9500 . ? C12 C13 1.391(5) . ? C12 H12 0.9500 . ? C13 C14 1.376(5) . ? C13 H13 0.9500 . ? C14 C15 1.385(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.398(5) . ? C16 C17 1.401(5) . ? C16 P1 1.839(4) . ? C17 C18 1.384(5) . ? C17 H17 0.9500 . ? C18 C19 1.373(6) . ? C18 H18 0.9500 . ? C19 C20 1.374(6) . ? C19 H19 0.9500 . ? C20 C21 1.389(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.383(5) . ? C22 C23 1.402(5) . ? C22 P1 1.838(4) . ? C23 C24 1.388(5) . ? C23 H23 0.9500 . ? C24 C25 1.378(6) . ? C24 H24 0.9500 . ? C25 C26 1.374(5) . ? C25 H25 0.9500 . ? C26 C27 1.399(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 O1 1.278(4) . ? C28 C37 1.404(5) . ? C28 C29 1.516(5) . ? C29 C30 1.517(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.380(5) . ? C30 C36 1.390(5) . ? C31 C32 1.385(6) . ? C31 H31 0.9500 . ? C32 C33 1.392(6) . ? C32 H32 0.9500 . ? C33 C35 1.382(6) . ? C33 C34 1.503(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.381(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.396(5) . ? C37 H37 0.9500 . ? C38 C39 1.486(5) . ? C38 Ru1 1.999(3) . ? C39 C40 1.399(5) . ? C39 C44 1.400(4) . ? C40 C41 1.388(5) . ? C40 H40 0.9500 . ? C41 C42 1.393(5) . ? C41 H41 0.9500 . ? C42 C43 1.384(5) . ? C42 C45 1.511(5) . ? C43 C44 1.383(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 N7 1.333(5) . ? C46 C47 1.389(5) . ? C46 H46 0.9500 . ? C47 C48 1.369(6) . ? C47 H47 0.9500 . ? C48 N8 1.357(5) . ? C48 H48 0.9500 . ? C49 N9 1.335(4) . ? C49 C50 1.392(5) . ? C49 H49 0.9500 . ? C50 C51 1.366(6) . ? C50 H50 0.9500 . ? C51 N10 1.350(4) . ? C51 H51 0.9500 . ? C52 N11 1.334(5) . ? C52 C53 1.386(5) . ? C52 H52 0.9500 . ? C53 C54 1.381(5) . ? C53 H53 0.9500 . ? C54 N12 1.340(5) . ? C54 H54 0.9500 . ? C55 C60 1.390(5) . ? C55 C56 1.395(5) . ? C55 P2 1.849(4) . ? C56 C57 1.384(5) . ? C56 H56 0.9500 . ? C57 C58 1.384(5) . ? C57 H57 0.9500 . ? C58 C59 1.382(6) . ? C58 H58 0.9500 . ? C59 C60 1.383(5) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C66 1.393(5) . ? C61 C62 1.394(5) . ? C61 P2 1.842(4) . ? C62 C63 1.390(5) . ? C62 H62 0.9500 . ? C63 C64 1.375(6) . ? C63 H63 0.9500 . ? C64 C65 1.369(7) . ? C64 H64 0.9500 . ? C65 C66 1.391(6) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.390(5) . ? C67 C72 1.398(5) . ? C67 P2 1.831(4) . ? C68 C69 1.393(5) . ? C68 H68 0.9500 . ? C69 C70 1.377(6) . ? C69 H69 0.9500 . ? C70 C71 1.378(6) . ? C70 H70 0.9500 . ? C71 C72 1.385(5) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 O2 1.278(4) . ? C73 C82 1.406(5) . ? C73 C74 1.514(5) . ? C74 C75 1.517(5) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C81 1.381(5) . ? C75 C76 1.390(5) . ? C76 C77 1.384(6) . ? C76 H76 0.9500 . ? C77 C78 1.376(6) . ? C77 H77 0.9500 . ? C78 C80 1.380(5) . ? C78 C79 1.516(6) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C81 1.384(5) . ? C80 H80 0.9500 . ? C81 H81 0.9500 . ? C82 C83 1.387(5) . ? C82 H82 0.9500 . ? C83 C84 1.482(5) . ? C83 Ru2 2.013(3) . ? C84 C85 1.397(5) . ? C84 C89 1.400(5) . ? C85 C86 1.391(5) . ? C85 H85 0.9500 . ? C86 C87 1.383(5) . ? C86 H86 0.9500 . ? C87 C88 1.385(6) . ? C87 C90 1.513(6) . ? C88 C89 1.385(5) . ? C88 H88 0.9500 . ? C89 H89 0.9500 . ? C90 H90A 0.9801 . ? C90 H90B 0.9801 . ? C90 H90C 0.9801 . ? B1 N6 1.533(5) . ? B1 N2 1.531(5) . ? B1 N4 1.547(5) . ? B1 H1A 1.0000 . ? B2 N8 1.521(6) . ? B2 N10 1.528(5) . ? B2 N12 1.547(5) . ? B2 H2A 1.0000 . ? N1 N2 1.374(4) . ? N1 Ru1 2.121(3) . ? N3 N4 1.375(4) . ? N3 Ru1 2.071(3) . ? N5 N6 1.371(4) . ? N5 Ru1 2.205(3) . ? N7 N8 1.370(4) . ? N7 Ru2 2.117(3) . ? N9 N10 1.371(4) . ? N9 Ru2 2.190(3) . ? N11 N12 1.378(4) . ? N11 Ru2 2.069(3) . ? O1 Ru1 2.086(3) . ? O2 Ru2 2.088(2) . ? P1 Ru1 2.3069(10) . ? P2 Ru2 2.3119(10) . ? 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 C1 C2 110.5(4) . . ? N1 C1 H1 124.7 . . ? C2 C1 H1 124.7 . . ? C3 C2 C1 105.1(4) . . ? C3 C2 H2 127.4 . . ? C1 C2 H2 127.4 . . ? N2 C3 C2 108.8(3) . . ? N2 C3 H3 125.6 . . ? C2 C3 H3 125.6 . . ? N3 C4 C5 111.3(4) . . ? N3 C4 H4 124.3 . . ? C5 C4 H4 124.4 . . ? C6 C5 C4 104.7(4) . . ? C6 C5 H5 127.7 . . ? C4 C5 H5 127.7 . . ? N4 C6 C5 109.2(4) . . ? N4 C6 H6 125.4 . . ? C5 C6 H6 125.4 . . ? N5 C7 C8 111.1(4) . . ? N5 C7 H7 124.5 . . ? C8 C7 H7 124.5 . . ? C9 C8 C7 104.8(4) . . ? C9 C8 H8 127.6 . . ? C7 C8 H8 127.6 . . ? N6 C9 C8 108.5(4) . . ? N6 C9 H9 125.7 . . ? C8 C9 H9 125.8 . . ? C11 C10 C15 118.9(3) . . ? C11 C10 P1 119.4(3) . . ? C15 C10 P1 121.6(3) . . ? C12 C11 C10 120.2(4) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.5(4) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 119.3(4) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 121.0(4) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C10 120.1(4) . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 119.9 . . ? C21 C16 C17 117.5(4) . . ? C21 C16 P1 123.0(3) . . ? C17 C16 P1 119.1(3) . . ? C18 C17 C16 121.1(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C19 C18 C17 120.2(4) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.2(4) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C21 120.0(4) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C16 121.0(4) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? C27 C22 C23 118.4(4) . . ? C27 C22 P1 124.0(3) . . ? C23 C22 P1 117.5(3) . . ? C24 C23 C22 120.3(4) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 120.7(4) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C26 C25 C24 119.5(4) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.4(4) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C22 C27 C26 120.7(4) . . ? C22 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? O1 C28 C37 118.3(3) . . ? O1 C28 C29 118.0(3) . . ? C37 C28 C29 123.6(3) . . ? C28 C29 C30 110.2(3) . . ? C28 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? C28 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C31 C30 C36 118.0(4) . . ? C31 C30 C29 120.8(4) . . ? C36 C30 C29 121.2(4) . . ? C30 C31 C32 120.9(4) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C31 C32 C33 121.4(4) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C35 C33 C32 117.3(4) . . ? C35 C33 C34 121.6(4) . . ? C32 C33 C34 121.1(4) . . ? 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 . . ? C36 C35 C33 121.6(4) . . ? C36 C35 H35 119.2 . . ? C33 C35 H35 119.2 . . ? C35 C36 C30 120.9(4) . . ? C35 C36 H36 119.6 . . ? C30 C36 H36 119.6 . . ? C38 C37 C28 115.2(3) . . ? C38 C37 H37 122.4 . . ? C28 C37 H37 122.4 . . ? C37 C38 C39 117.2(3) . . ? C37 C38 Ru1 113.4(3) . . ? C39 C38 Ru1 129.1(3) . . ? C40 C39 C44 116.8(3) . . ? C40 C39 C38 120.6(3) . . ? C44 C39 C38 122.5(3) . . ? C41 C40 C39 121.5(3) . . ? C41 C40 H40 119.2 . . ? C39 C40 H40 119.2 . . ? C40 C41 C42 121.2(3) . . ? C40 C41 H41 119.4 . . ? C42 C41 H41 119.4 . . ? C43 C42 C41 117.4(3) . . ? C43 C42 C45 121.6(3) . . ? C41 C42 C45 121.0(3) . . ? C44 C43 C42 121.9(3) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C43 C44 C39 121.3(3) . . ? C43 C44 H44 119.4 . . ? C39 C44 H44 119.4 . . ? 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 . . ? N7 C46 C47 110.4(4) . . ? N7 C46 H46 124.8 . . ? C47 C46 H46 124.8 . . ? C48 C47 C46 105.5(4) . . ? C48 C47 H47 127.3 . . ? C46 C47 H47 127.3 . . ? N8 C48 C47 108.4(4) . . ? N8 C48 H48 125.8 . . ? C47 C48 H48 125.8 . . ? N9 C49 C50 111.3(4) . . ? N9 C49 H49 124.4 . . ? C50 C49 H49 124.4 . . ? C51 C50 C49 104.6(4) . . ? C51 C50 H50 127.7 . . ? C49 C50 H50 127.7 . . ? N10 C51 C50 109.0(4) . . ? N10 C51 H51 125.5 . . ? C50 C51 H51 125.5 . . ? N11 C52 C53 111.1(3) . . ? N11 C52 H52 124.4 . . ? C53 C52 H52 124.4 . . ? C54 C53 C52 104.2(4) . . ? C54 C53 H53 127.9 . . ? C52 C53 H53 127.9 . . ? N12 C54 C53 109.6(3) . . ? N12 C54 H54 125.2 . . ? C53 C54 H54 125.2 . . ? C60 C55 C56 118.5(3) . . ? C60 C55 P2 122.3(3) . . ? C56 C55 P2 119.3(3) . . ? C57 C56 C55 121.1(4) . . ? C57 C56 H56 119.4 . . ? C55 C56 H56 119.5 . . ? C58 C57 C56 120.0(4) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C59 C58 C57 119.2(4) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C58 C59 C60 121.1(4) . . ? C58 C59 H59 119.4 . . ? C60 C59 H59 119.4 . . ? C59 C60 C55 120.1(4) . . ? C59 C60 H60 119.9 . . ? C55 C60 H60 119.9 . . ? C66 C61 C62 118.6(4) . . ? C66 C61 P2 123.0(3) . . ? C62 C61 P2 118.1(3) . . ? C63 C62 C61 120.1(4) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? C64 C63 C62 120.3(5) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C65 C64 C63 120.4(4) . . ? C65 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C64 C65 C66 119.9(4) . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C65 C66 C61 120.6(4) . . ? C65 C66 H66 119.7 . . ? C61 C66 H66 119.7 . . ? C68 C67 C72 118.1(4) . . ? C68 C67 P2 124.5(3) . . ? C72 C67 P2 117.4(3) . . ? C67 C68 C69 120.8(4) . . ? C67 C68 H68 119.6 . . ? C69 C68 H68 119.6 . . ? C70 C69 C68 120.4(4) . . ? C70 C69 H69 119.8 . . ? C68 C69 H69 119.8 . . ? C69 C70 C71 119.4(4) . . ? C69 C70 H70 120.3 . . ? C71 C70 H70 120.3 . . ? C70 C71 C72 120.7(4) . . ? C70 C71 H71 119.7 . . ? C72 C71 H71 119.7 . . ? C71 C72 C67 120.6(4) . . ? C71 C72 H72 119.7 . . ? C67 C72 H72 119.7 . . ? O2 C73 C82 118.7(4) . . ? O2 C73 C74 118.0(3) . . ? C82 C73 C74 123.1(3) . . ? C73 C74 C75 109.9(3) . . ? C73 C74 H74A 109.7 . . ? C75 C74 H74A 109.7 . . ? C73 C74 H74B 109.7 . . ? C75 C74 H74B 109.7 . . ? H74A C74 H74B 108.2 . . ? C81 C75 C76 117.1(4) . . ? C81 C75 C74 120.9(4) . . ? C76 C75 C74 121.9(4) . . ? C77 C76 C75 120.9(4) . . ? C77 C76 H76 119.5 . . ? C75 C76 H76 119.6 . . ? C78 C77 C76 121.9(4) . . ? C78 C77 H77 119.1 . . ? C76 C77 H77 119.1 . . ? C77 C78 C80 117.2(4) . . ? C77 C78 C79 121.9(4) . . ? C80 C78 C79 120.9(4) . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C78 C80 C81 121.3(4) . . ? C78 C80 H80 119.3 . . ? C81 C80 H80 119.3 . . ? C75 C81 C80 121.5(4) . . ? C75 C81 H81 119.2 . . ? C80 C81 H81 119.2 . . ? C83 C82 C73 115.6(3) . . ? C83 C82 H82 122.2 . . ? C73 C82 H82 122.2 . . ? C82 C83 C84 116.4(3) . . ? C82 C83 Ru2 113.0(3) . . ? C84 C83 Ru2 130.2(3) . . ? C85 C84 C89 116.7(3) . . ? C85 C84 C83 121.4(3) . . ? C89 C84 C83 121.9(3) . . ? C86 C85 C84 121.3(4) . . ? C86 C85 H85 119.3 . . ? C84 C85 H85 119.3 . . ? C87 C86 C85 121.5(4) . . ? C87 C86 H86 119.2 . . ? C85 C86 H86 119.2 . . ? C86 C87 C88 117.4(4) . . ? C86 C87 C90 121.3(4) . . ? C88 C87 C90 121.4(4) . . ? C89 C88 C87 121.8(4) . . ? C89 C88 H88 119.1 . . ? C87 C88 H88 119.1 . . ? C88 C89 C84 121.2(4) . . ? C88 C89 H89 119.4 . . ? C84 C89 H89 119.4 . . ? C87 C90 H90A 109.5 . . ? C87 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C87 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? N6 B1 N2 108.0(3) . . ? N6 B1 N4 108.7(3) . . ? N2 B1 N4 108.7(3) . . ? N6 B1 H1A 110.5 . . ? N2 B1 H1A 110.5 . . ? N4 B1 H1A 110.5 . . ? N8 B2 N10 109.7(3) . . ? N8 B2 N12 108.8(3) . . ? N10 B2 N12 108.7(3) . . ? N8 B2 H2A 109.8 . . ? N10 B2 H2A 109.8 . . ? N12 B2 H2A 109.8 . . ? C1 N1 N2 107.1(3) . . ? C1 N1 Ru1 133.7(3) . . ? N2 N1 Ru1 118.9(2) . . ? C3 N2 N1 108.4(3) . . ? C3 N2 B1 131.6(3) . . ? N1 N2 B1 119.9(3) . . ? C4 N3 N4 105.7(3) . . ? C4 N3 Ru1 135.8(3) . . ? N4 N3 Ru1 118.5(2) . . ? C6 N4 N3 109.1(3) . . ? C6 N4 B1 129.5(3) . . ? N3 N4 B1 121.4(3) . . ? C7 N5 N6 106.0(3) . . ? C7 N5 Ru1 136.6(3) . . ? N6 N5 Ru1 117.4(2) . . ? C9 N6 N5 109.6(3) . . ? C9 N6 B1 130.7(3) . . ? N5 N6 B1 119.7(3) . . ? C46 N7 N8 106.7(3) . . ? C46 N7 Ru2 134.6(3) . . ? N8 N7 Ru2 118.5(2) . . ? C48 N8 N7 109.0(3) . . ? C48 N8 B2 131.5(3) . . ? N7 N8 B2 119.5(3) . . ? C49 N9 N10 105.7(3) . . ? C49 N9 Ru2 136.4(3) . . ? N10 N9 Ru2 117.7(2) . . ? C51 N10 N9 109.4(3) . . ? C51 N10 B2 132.1(3) . . ? N9 N10 B2 118.2(3) . . ? C52 N11 N12 106.5(3) . . ? C52 N11 Ru2 135.7(2) . . ? N12 N11 Ru2 117.8(2) . . ? C54 N12 N11 108.6(3) . . ? C54 N12 B2 130.5(3) . . ? N11 N12 B2 120.9(3) . . ? C28 O1 Ru1 113.5(2) . . ? C73 O2 Ru2 113.1(2) . . ? C16 P1 C22 101.52(17) . . ? C16 P1 C10 101.31(16) . . ? C22 P1 C10 103.06(17) . . ? C16 P1 Ru1 118.32(13) . . ? C22 P1 Ru1 117.17(12) . . ? C10 P1 Ru1 113.12(12) . . ? C67 P2 C61 101.55(17) . . ? C67 P2 C55 101.76(17) . . ? C61 P2 C55 101.69(16) . . ? C67 P2 Ru2 117.39(12) . . ? C61 P2 Ru2 118.39(13) . . ? C55 P2 Ru2 113.56(12) . . ? C38 Ru1 N3 99.28(13) . . ? C38 Ru1 O1 79.35(13) . . ? N3 Ru1 O1 173.22(10) . . ? C38 Ru1 N1 90.13(12) . . ? N3 Ru1 N1 85.45(12) . . ? O1 Ru1 N1 87.91(11) . . ? C38 Ru1 N5 171.50(13) . . ? N3 Ru1 N5 87.12(11) . . ? O1 Ru1 N5 93.64(10) . . ? N1 Ru1 N5 84.77(11) . . ? C38 Ru1 P1 94.27(10) . . ? N3 Ru1 P1 93.33(9) . . ? O1 Ru1 P1 93.40(7) . . ? N1 Ru1 P1 175.57(8) . . ? N5 Ru1 P1 90.91(8) . . ? C83 Ru2 N11 99.45(13) . . ? C83 Ru2 O2 79.49(12) . . ? N11 Ru2 O2 174.08(11) . . ? C83 Ru2 N7 89.99(12) . . ? N11 Ru2 N7 85.68(12) . . ? O2 Ru2 N7 88.49(11) . . ? C83 Ru2 N9 169.69(14) . . ? N11 Ru2 N9 88.52(11) . . ? O2 Ru2 N9 91.92(10) . . ? N7 Ru2 N9 84.07(11) . . ? C83 Ru2 P2 95.82(10) . . ? N11 Ru2 P2 90.88(9) . . ? O2 Ru2 P2 95.02(7) . . ? N7 Ru2 P2 173.68(8) . . ? N9 Ru2 P2 90.55(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.751 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.152