# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H42 N10 Ru, 2(F6 P), 4(C4 H10 O)' _chemical_formula_sum 'C86 H82 F12 N10 O4 P2 Ru' _chemical_formula_weight 1710.63 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' F F 0.0171 0.0103 '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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Fddd ' _symmetry_space_group_name_Hall '-F 2uv 2vw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 21.841(3) _cell_length_b 25.024(2) _cell_length_c 34.582(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 18900(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8136 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 24.98 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7056 _exptl_absorpt_coefficient_mu 0.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7 _exptl_absorpt_correction_T_max 0.8 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD ' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37508 _diffrn_reflns_av_R_equivalents 0.0978 _diffrn_reflns_av_sigmaI/netI 0.0924 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4660 _reflns_number_gt 2980 _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^)+(0.04P)^2^+1.22P] 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 4660 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 1.02999(13) 0.03499(11) 0.11214(9) 0.0396(8) Uani 1 1 d . . . H1 H 1.0363 0.0403 0.0858 0.048 Uiso 1 1 calc R . . C2 C 0.99113(14) -0.00381(12) 0.12324(9) 0.0415(8) Uani 1 1 d . . . H2 H 0.9718 -0.0250 0.1048 0.050 Uiso 1 1 calc R . . C3 C 0.97986(13) -0.01227(12) 0.16269(9) 0.0450(8) Uani 1 1 d . . . H3 H 0.9531 -0.0389 0.1709 0.054 Uiso 1 1 calc R . . C4 C 1.00975(13) 0.02010(12) 0.18914(9) 0.0422(8) Uani 1 1 d . . . H4 H 1.0025 0.0163 0.2155 0.051 Uiso 1 1 calc R . . C5 C 1.05046(12) 0.05807(11) 0.17589(9) 0.0394(7) Uani 1 1 d . . . C6 C 1.08767(12) 0.09197(11) 0.20151(9) 0.0385(8) Uani 1 1 d . . . C7 C 1.08696(12) 0.09183(11) 0.24136(9) 0.0354(7) Uani 1 1 d . . . H7 H 1.0604 0.0690 0.2543 0.042 Uiso 1 1 calc R . . C8 C 1.1250 0.1250 0.26248(13) 0.0379(10) Uani 1 2 d S . . C9 C 1.1250 0.1250 0.30510(11) 0.0353(10) Uani 1 2 d S . . C10 C 1.07333(12) 0.11067(11) 0.32583(9) 0.0374(7) Uani 1 1 d . . . H10 H 1.0383 0.1003 0.3125 0.045 Uiso 1 1 calc R . . C11 C 1.07208(13) 0.11132(11) 0.36668(9) 0.0369(7) Uani 1 1 d . . . C12 C 1.1250 0.1250 0.38594(13) 0.0377(10) Uani 1 2 d S . . H12 H 1.1250 0.1250 0.4128 0.045 Uiso 1 2 calc SR . . C13 C 1.01605(14) 0.09797(12) 0.38721(9) 0.0414(8) Uani 1 1 d . . . C14 C 0.97094(14) 0.08889(12) 0.40353(9) 0.0408(8) Uani 1 1 d . . . C15 C 0.91561(13) 0.07630(12) 0.42428(9) 0.0429(8) Uani 1 1 d . . . C16 C 0.88372(12) 0.11496(13) 0.44512(9) 0.0419(8) Uani 1 1 d . . . H16 H 0.8972 0.1502 0.4455 0.050 Uiso 1 1 calc R . . C17 C 0.83274(13) 0.10040(14) 0.46489(9) 0.0460(8) Uani 1 1 d . . . H17 H 0.8115 0.1270 0.4781 0.055 Uiso 1 1 calc R . . C18 C 0.84222(14) 0.01555(13) 0.44841(9) 0.0448(8) Uani 1 1 d . . . H18 H 0.8287 -0.0196 0.4502 0.054 Uiso 1 1 calc R . . C19 C 0.89231(13) 0.02548(13) 0.42710(9) 0.0457(8) Uani 1 1 d . . . H19 H 0.9115 -0.0024 0.4141 0.055 Uiso 1 1 calc R . . F1 F 0.50376(7) 0.30654(6) 0.77109(5) 0.0474(5) Uani 1 1 d . . . F2 F 0.46446(7) 0.27692(6) 0.71578(5) 0.0490(5) Uani 1 1 d . . . F3 F 0.56211(7) 0.26146(6) 0.72730(5) 0.0469(5) Uani 1 1 d . . . N1 N 1.05999(10) 0.06638(9) 0.13724(7) 0.0374(6) Uani 1 1 d . . . N2 N 1.1250 0.1250 0.18278(10) 0.0342(8) Uani 1 2 d S . . N3 N 0.81145(11) 0.05226(11) 0.46675(8) 0.0481(7) Uani 1 1 d . . . P1 P 0.5000 0.2500 0.7500 0.0420(3) Uani 1 2 d S . . Ru1 Ru 1.1250 0.1250 0.1250 0.03617(17) Uani 1 4 d S . . O1 O 0.99902(19) 0.13231(17) 0.51456(14) 0.0606(13) Uani 0.50 1 d P A 1 C20 C 1.0442(3) 0.0485(2) 0.48415(19) 0.0534(18) Uani 0.50 1 d P A 1 H20A H 1.0221 0.0448 0.4603 0.080 Uiso 0.50 1 calc PR A 1 H20B H 1.0224 0.0305 0.5044 0.080 Uiso 0.50 1 calc PR A 1 H20C H 1.0842 0.0330 0.4814 0.080 Uiso 0.50 1 calc PR A 1 C21 C 1.0503(3) 0.1076(3) 0.4942(2) 0.0542(18) Uani 0.50 1 d P A 1 H21A H 1.0867 0.1120 0.5100 0.065 Uiso 0.50 1 calc PR A 1 H21B H 1.0570 0.1272 0.4704 0.065 Uiso 0.50 1 calc PR A 1 C22 C 0.9458(3) 0.0986(3) 0.5212(2) 0.0593(19) Uani 0.50 1 d P A 1 H22A H 0.9585 0.0640 0.5308 0.071 Uiso 0.50 1 calc PR A 1 H22B H 0.9236 0.0934 0.4972 0.071 Uiso 0.50 1 calc PR A 1 C23 C 0.9039(3) 0.1271(3) 0.5516(2) 0.071(2) Uani 0.50 1 d P A 1 H23A H 0.8663 0.1076 0.5543 0.106 Uiso 0.50 1 calc PR A 1 H23B H 0.8953 0.1628 0.5431 0.106 Uiso 0.50 1 calc PR A 1 H23C H 0.9245 0.1283 0.5761 0.106 Uiso 0.50 1 calc PR A 1 O2 O 0.9652(2) 0.0719(2) 0.60820(16) 0.0706(14) Uani 0.50 1 d P . 2 C24 C 1.0106(3) 0.1598(3) 0.6185(2) 0.068(2) Uani 0.50 1 d P . 2 H24A H 1.0097 0.1910 0.6346 0.102 Uiso 0.50 1 d PR . 2 H24B H 1.0507 0.1441 0.6193 0.102 Uiso 0.50 1 d PR . 2 H24C H 1.0010 0.1697 0.5923 0.102 Uiso 0.50 1 d PR . 2 C25 C 0.9632(3) 0.1192(8) 0.6334(5) 0.070(4) Uani 0.50 1 d P . 2 H25A H 0.9724 0.1094 0.6595 0.084 Uiso 0.50 1 d PR . 2 H25B H 0.9231 0.1348 0.6328 0.084 Uiso 0.50 1 d PR . 2 C26 C 0.9088(3) 0.0391(3) 0.6085(2) 0.061(2) Uani 0.50 1 d P . 2 H26A H 0.8810 0.0491 0.6292 0.073 Uiso 0.50 1 calc PR . 2 H26B H 0.9175 0.0011 0.6099 0.073 Uiso 0.50 1 calc PR . 2 C27 C 0.8850(3) 0.0564(3) 0.5679(2) 0.063(2) Uani 0.50 1 d P . 2 H27A H 0.8604 0.0880 0.5705 0.094 Uiso 0.50 1 calc PR . 2 H27B H 0.8608 0.0282 0.5570 0.094 Uiso 0.50 1 calc PR . 2 H27C H 0.9192 0.0638 0.5513 0.094 Uiso 0.50 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0440(17) 0.0436(19) 0.0314(19) -0.0092(14) -0.0110(14) -0.0069(15) C2 0.0492(18) 0.0428(19) 0.032(2) -0.0069(14) -0.0096(15) -0.0141(15) C3 0.0494(18) 0.0454(19) 0.040(2) -0.0141(16) 0.0100(16) -0.0158(16) C4 0.0493(18) 0.0487(19) 0.0286(19) -0.0106(15) 0.0081(15) -0.0123(16) C5 0.0416(16) 0.0445(18) 0.032(2) -0.0125(15) -0.0096(15) -0.0104(15) C6 0.0378(17) 0.0376(18) 0.040(2) 0.0050(14) -0.0123(15) -0.0146(15) C7 0.0418(17) 0.0358(17) 0.0285(19) -0.0065(13) -0.0074(14) 0.0074(14) C8 0.045(2) 0.039(2) 0.030(3) 0.000 0.000 0.010(2) C9 0.052(2) 0.039(2) 0.015(2) 0.000 0.000 0.009(2) C10 0.0348(15) 0.0454(18) 0.0318(19) -0.0120(14) 0.0085(14) 0.0036(14) C11 0.0416(17) 0.0347(17) 0.034(2) -0.0089(14) 0.0135(15) 0.0096(14) C12 0.039(2) 0.044(3) 0.029(3) 0.000 0.000 0.014(2) C13 0.0415(18) 0.0434(19) 0.039(2) -0.0104(15) -0.0072(16) -0.0096(16) C14 0.0424(18) 0.046(2) 0.034(2) 0.0074(15) 0.0087(15) 0.0138(15) C15 0.0406(16) 0.0449(19) 0.043(2) 0.0125(16) 0.0137(15) 0.0111(15) C16 0.0365(17) 0.047(2) 0.043(2) -0.0085(15) -0.0034(15) 0.0053(15) C17 0.0439(18) 0.052(2) 0.043(2) -0.0138(17) 0.0019(16) -0.0038(17) C18 0.0473(18) 0.0380(18) 0.049(2) 0.0084(15) 0.0183(17) -0.0044(16) C19 0.0462(18) 0.045(2) 0.046(2) 0.0071(16) 0.0134(16) 0.0086(16) F1 0.0489(10) 0.0524(10) 0.0409(11) -0.0084(8) 0.0143(8) 0.0134(9) F2 0.0550(10) 0.0490(10) 0.0429(12) 0.0086(8) -0.0059(9) 0.0161(9) F3 0.0476(10) 0.0473(10) 0.0459(12) 0.0079(8) 0.0141(9) 0.0126(8) N1 0.0408(13) 0.0428(15) 0.0286(15) -0.0126(11) -0.0048(12) -0.0096(12) N2 0.0429(19) 0.0338(19) 0.026(2) 0.000 0.000 -0.0108(17) N3 0.0431(14) 0.0534(18) 0.0480(19) 0.0078(14) 0.0066(13) -0.0062(14) P1 0.0505(7) 0.0421(7) 0.0334(7) 0.0070(5) 0.0075(6) 0.0156(6) Ru1 0.0416(3) 0.0384(3) 0.0286(3) 0.000 0.000 0.000 O1 0.057(3) 0.066(3) 0.059(4) -0.011(2) 0.011(3) -0.016(2) C20 0.054(4) 0.060(4) 0.046(5) -0.007(3) 0.009(3) -0.013(3) C21 0.056(4) 0.063(4) 0.043(5) -0.011(3) 0.008(3) -0.017(4) C22 0.053(4) 0.070(5) 0.056(5) 0.005(4) -0.016(4) -0.023(4) C23 0.070(5) 0.067(5) 0.076(6) -0.030(4) -0.027(5) 0.022(4) O2 0.071(3) 0.069(4) 0.072(4) -0.025(3) -0.013(3) -0.014(3) C24 0.065(5) 0.077(5) 0.063(6) -0.020(4) 0.018(4) -0.029(4) C25 0.084(5) 0.044(8) 0.082(15) 0.021(7) 0.032(6) 0.008(6) C26 0.046(4) 0.058(5) 0.080(6) 0.010(4) 0.000(4) 0.003(4) C27 0.050(4) 0.054(4) 0.085(7) -0.014(4) 0.009(4) -0.007(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 C1 N1 1.342(3) . ? C1 C2 1.346(4) . ? C1 H1 0.9300 . ? C2 C3 1.402(4) . ? C2 H2 0.9300 . ? C3 C4 1.385(4) . ? C3 H3 0.9300 . ? C4 C5 1.379(4) . ? C4 H4 0.9300 . ? C5 N1 1.369(4) . ? C5 C6 1.471(4) . ? C6 N2 1.329(3) . ? C6 C7 1.378(4) . ? C7 C8 1.383(3) . ? C7 H7 0.9300 . ? C8 C7 1.383(3) 2_755 ? C8 C9 1.474(6) . ? C9 C10 1.384(3) . ? C9 C10 1.384(3) 2_755 ? C10 C11 1.413(4) . ? C10 H10 0.9300 . ? C11 C12 1.377(4) . ? C11 C13 1.454(4) . ? C12 C11 1.377(4) 2_755 ? C12 H12 0.9300 . ? C13 C14 1.158(4) . ? C14 C15 1.440(4) . ? C15 C19 1.373(4) . ? C15 C16 1.393(4) . ? C16 C17 1.357(4) . ? C16 H16 0.9300 . ? C17 N3 1.293(4) . ? C17 H17 0.9300 . ? C18 N3 1.303(4) . ? C18 C19 1.342(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? F1 P1 1.5940(16) . ? F2 P1 1.5675(16) . ? F3 P1 1.5933(16) . ? N1 Ru1 2.085(2) . ? N2 C6 1.329(3) 2_755 ? N2 Ru1 1.998(3) . ? P1 F2 1.5675(16) 21_656 ? P1 F3 1.5933(16) 21_656 ? P1 F1 1.5940(16) 21_656 ? Ru1 N2 1.998(3) 3 ? Ru1 N1 2.085(2) 2_755 ? Ru1 N1 2.085(2) 3 ? Ru1 N1 2.085(2) 4_755 ? O1 C22 1.454(7) . ? O1 C21 1.460(7) . ? C20 C21 1.525(8) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.566(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? O2 C24 1.359(8) 3_556 ? O2 C25 1.47(2) . ? O2 C26 1.480(8) . ? O2 C25 1.50(2) 3_556 ? C24 C25 1.265(13) 3_556 ? C24 O2 1.358(8) 3_556 ? C24 C25 1.538(12) . ? C24 C24 1.800(15) 3_556 ? C24 H24A 0.9601 . ? C24 H24B 0.9599 . ? C24 H24C 0.9600 . ? C25 C25 0.65(2) 3_556 ? C25 C24 1.265(13) 3_556 ? C25 O2 1.50(2) 3_556 ? C25 H25A 0.9599 . ? C25 H25B 0.9599 . ? C26 C27 1.559(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 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 N1 C1 C2 123.1(3) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 119.8(3) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 118.1(3) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C5 C4 C3 119.2(3) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 114.6(3) . . ? C4 C5 C6 123.6(3) . . ? N2 C6 C7 119.7(3) . . ? N2 C6 C5 113.8(3) . . ? C7 C6 C5 126.5(3) . . ? C6 C7 C8 121.3(3) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C7 116.3(4) 2_755 . ? C7 C8 C9 121.9(2) 2_755 . ? C7 C8 C9 121.9(2) . . ? C10 C9 C10 117.6(4) . 2_755 ? C10 C9 C8 121.20(19) . . ? C10 C9 C8 121.20(19) 2_755 . ? C9 C10 C11 122.0(3) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C12 C11 C10 118.1(3) . . ? C12 C11 C13 121.8(3) . . ? C10 C11 C13 120.1(3) . . ? C11 C12 C11 122.1(4) 2_755 . ? C11 C12 H12 118.9 2_755 . ? C11 C12 H12 118.9 . . ? C14 C13 C11 178.0(3) . . ? C13 C14 C15 178.4(3) . . ? C19 C15 C16 114.9(3) . . ? C19 C15 C14 123.3(3) . . ? C16 C15 C14 121.7(3) . . ? C17 C16 C15 119.0(3) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? N3 C17 C16 124.8(3) . . ? N3 C17 H17 117.6 . . ? C16 C17 H17 117.6 . . ? N3 C18 C19 123.9(3) . . ? N3 C18 H18 118.1 . . ? C19 C18 H18 118.1 . . ? C18 C19 C15 120.8(3) . . ? C18 C19 H19 119.6 . . ? C15 C19 H19 119.6 . . ? C1 N1 C5 117.9(3) . . ? C1 N1 Ru1 127.8(2) . . ? C5 N1 Ru1 114.13(17) . . ? C6 N2 C6 121.7(4) . 2_755 ? C6 N2 Ru1 119.15(18) . . ? C6 N2 Ru1 119.15(18) 2_755 . ? C17 N3 C18 116.6(3) . . ? F2 P1 F2 179.997(1) . 21_656 ? F2 P1 F3 88.41(9) . . ? F2 P1 F3 91.59(9) 21_656 . ? F2 P1 F3 91.60(9) . 21_656 ? F2 P1 F3 88.40(9) 21_656 21_656 ? F3 P1 F3 179.995(1) . 21_656 ? F2 P1 F1 89.40(8) . . ? F2 P1 F1 90.60(8) 21_656 . ? F3 P1 F1 91.25(8) . . ? F3 P1 F1 88.75(8) 21_656 . ? F2 P1 F1 90.60(8) . 21_656 ? F2 P1 F1 89.40(8) 21_656 21_656 ? F3 P1 F1 88.75(8) . 21_656 ? F3 P1 F1 91.26(8) 21_656 21_656 ? F1 P1 F1 180.00(10) . 21_656 ? N2 Ru1 N2 180.0 . 3 ? N2 Ru1 N1 78.29(7) . . ? N2 Ru1 N1 101.71(7) 3 . ? N2 Ru1 N1 78.29(7) . 2_755 ? N2 Ru1 N1 101.71(7) 3 2_755 ? N1 Ru1 N1 156.58(13) . 2_755 ? N2 Ru1 N1 101.71(7) . 3 ? N2 Ru1 N1 78.29(7) 3 3 ? N1 Ru1 N1 94.16(13) . 3 ? N1 Ru1 N1 90.57(13) 2_755 3 ? N2 Ru1 N1 101.71(7) . 4_755 ? N2 Ru1 N1 78.29(7) 3 4_755 ? N1 Ru1 N1 90.57(13) . 4_755 ? N1 Ru1 N1 94.16(13) 2_755 4_755 ? N1 Ru1 N1 156.58(13) 3 4_755 ? C22 O1 C21 116.4(5) . . ? O1 C21 C20 116.9(5) . . ? O1 C21 H21A 108.1 . . ? C20 C21 H21A 108.1 . . ? O1 C21 H21B 108.1 . . ? C20 C21 H21B 108.1 . . ? H21A C21 H21B 107.3 . . ? O1 C22 C23 108.0(5) . . ? O1 C22 H22A 110.1 . . ? C23 C22 H22A 110.1 . . ? O1 C22 H22B 110.1 . . ? C23 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? C24 O2 C25 53.0(4) 3_556 . ? C24 O2 C26 142.2(6) 3_556 . ? C25 O2 C26 114.8(5) . . ? C24 O2 C25 64.8(5) 3_556 3_556 ? C26 O2 C25 121.3(5) . 3_556 ? C25 C24 O2 68.1(10) 3_556 3_556 ? O2 C24 C25 62.1(8) 3_556 . ? C25 C24 C24 57.1(7) 3_556 3_556 ? O2 C24 C24 100.2(5) 3_556 3_556 ? C25 C24 H24A 118.6 3_556 . ? O2 C24 H24A 50.6 3_556 . ? C25 C24 H24A 109.1 . . ? C24 C24 H24A 129.8 3_556 . ? C25 C24 H24B 120.8 3_556 . ? O2 C24 H24B 141.8 3_556 . ? C25 C24 H24B 109.5 . . ? C24 C24 H24B 66.2 3_556 . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 85.6 3_556 . ? O2 C24 H24C 108.2 3_556 . ? C25 C24 H24C 109.8 . . ? C24 C24 H24C 119.1 3_556 . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 C25 C24 102(3) 3_556 3_556 ? C25 C25 O2 80(4) 3_556 . ? C24 C25 O2 59.0(9) 3_556 . ? C25 C25 O2 75(4) 3_556 3_556 ? C24 C25 O2 123.4(11) 3_556 3_556 ? O2 C25 O2 154.7(8) . 3_556 ? C25 C25 C24 53.5(19) 3_556 . ? C24 C25 C24 79.2(8) 3_556 . ? O2 C25 C24 108.3(10) . . ? O2 C25 C24 53.1(7) 3_556 . ? C25 C25 H25A 163.6 3_556 . ? C24 C25 H25A 74.2 3_556 . ? O2 C25 H25A 110.2 . . ? O2 C25 H25A 93.6 3_556 . ? C24 C25 H25A 110.2 . . ? C25 C25 H25B 78.5 3_556 . ? C24 C25 H25B 168.1 3_556 . ? O2 C25 H25B 109.9 . . ? O2 C25 H25B 68.4 3_556 . ? C24 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? O2 C26 C27 96.7(5) . . ? O2 C26 H26A 112.4 . . ? C27 C26 H26A 112.4 . . ? O2 C26 H26B 112.4 . . ? C27 C26 H26B 112.4 . . ? H26A C26 H26B 110.0 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 1.0(5) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C2 C3 C4 C5 -1.8(4) . . . . ? C3 C4 C5 N1 3.1(4) . . . . ? C3 C4 C5 C6 -175.7(3) . . . . ? N1 C5 C6 N2 -0.5(3) . . . . ? C4 C5 C6 N2 178.4(2) . . . . ? N1 C5 C6 C7 179.8(3) . . . . ? C4 C5 C6 C7 -1.2(5) . . . . ? N2 C6 C7 C8 -0.8(4) . . . . ? C5 C6 C7 C8 178.8(2) . . . . ? C6 C7 C8 C7 0.41(18) . . . 2_755 ? C6 C7 C8 C9 -179.59(18) . . . . ? C7 C8 C9 C10 152.65(18) 2_755 . . . ? C7 C8 C9 C10 -27.35(18) . . . . ? C7 C8 C9 C10 -27.35(18) 2_755 . . 2_755 ? C7 C8 C9 C10 152.65(18) . . . 2_755 ? C10 C9 C10 C11 1.14(18) 2_755 . . . ? C8 C9 C10 C11 -178.86(18) . . . . ? C9 C10 C11 C12 -2.2(4) . . . . ? C9 C10 C11 C13 177.6(2) . . . . ? C10 C11 C12 C11 1.07(17) . . . 2_755 ? C13 C11 C12 C11 -178.7(3) . . . 2_755 ? C19 C15 C16 C17 -2.1(4) . . . . ? C14 C15 C16 C17 -178.3(3) . . . . ? C15 C16 C17 N3 1.6(5) . . . . ? N3 C18 C19 C15 2.0(5) . . . . ? C16 C15 C19 C18 0.4(5) . . . . ? C14 C15 C19 C18 176.7(3) . . . . ? C2 C1 N1 C5 0.2(4) . . . . ? C2 C1 N1 Ru1 176.3(2) . . . . ? C4 C5 N1 C1 -2.3(4) . . . . ? C6 C5 N1 C1 176.6(2) . . . . ? C4 C5 N1 Ru1 -178.9(2) . . . . ? C6 C5 N1 Ru1 0.1(3) . . . . ? C7 C6 N2 C6 0.40(18) . . . 2_755 ? C5 C6 N2 C6 -179.3(3) . . . 2_755 ? C7 C6 N2 Ru1 -179.59(18) . . . . ? C5 C6 N2 Ru1 0.7(3) . . . . ? C16 C17 N3 C18 0.7(5) . . . . ? C19 C18 N3 C17 -2.5(5) . . . . ? C6 N2 Ru1 N1 -0.55(15) . . . . ? C6 N2 Ru1 N1 179.46(15) 2_755 . . . ? C6 N2 Ru1 N1 179.45(15) . . . 2_755 ? C6 N2 Ru1 N1 -0.54(15) 2_755 . . 2_755 ? C6 N2 Ru1 N1 91.32(15) . . . 3 ? C6 N2 Ru1 N1 -88.67(15) 2_755 . . 3 ? C6 N2 Ru1 N1 -88.68(15) . . . 4_755 ? C6 N2 Ru1 N1 91.33(15) 2_755 . . 4_755 ? C1 N1 Ru1 N2 -175.9(2) . . . . ? C5 N1 Ru1 N2 0.23(18) . . . . ? C1 N1 Ru1 N2 4.1(2) . . . 3 ? C5 N1 Ru1 N2 -179.77(18) . . . 3 ? C1 N1 Ru1 N1 -175.9(2) . . . 2_755 ? C5 N1 Ru1 N1 0.23(18) . . . 2_755 ? C1 N1 Ru1 N1 83.0(2) . . . 3 ? C5 N1 Ru1 N1 -100.9(2) . . . 3 ? C1 N1 Ru1 N1 -74.1(2) . . . 4_755 ? C5 N1 Ru1 N1 102.1(2) . . . 4_755 ? C22 O1 C21 C20 -3.4(8) . . . . ? C21 O1 C22 C23 166.2(6) . . . . ? C24 O2 C25 C25 110.8(5) 3_556 . . 3_556 ? C26 O2 C25 C25 -111.3(5) . . . 3_556 ? C26 O2 C25 C24 137.9(7) . . . 3_556 ? C25 O2 C25 C24 -110.8(5) 3_556 . . 3_556 ? C24 O2 C25 O2 103.3(17) 3_556 . . 3_556 ? C26 O2 C25 O2 -118.8(16) . . . 3_556 ? C25 O2 C25 O2 -7.5(17) 3_556 . . 3_556 ? C24 O2 C25 C24 64.6(8) 3_556 . . . ? C26 O2 C25 C24 -157.5(6) . . . . ? C25 O2 C25 C24 -46.2(6) 3_556 . . . ? O2 C24 C25 C25 98(4) 3_556 . . 3_556 ? C24 C24 C25 C25 -114(5) 3_556 . . 3_556 ? C25 C24 C25 C24 114(5) 3_556 . . 3_556 ? O2 C24 C25 C24 -147.5(12) 3_556 . . 3_556 ? C25 C24 C25 O2 62(4) 3_556 . . . ? O2 C24 C25 O2 160.5(8) 3_556 . . . ? C24 C24 C25 O2 -52.0(8) 3_556 . . . ? C25 C24 C25 O2 -98(4) 3_556 . . 3_556 ? C24 C24 C25 O2 147.5(12) 3_556 . . 3_556 ? C24 O2 C26 C27 166.9(8) 3_556 . . . ? C25 O2 C26 C27 106.1(7) . . . . ? C25 O2 C26 C27 78.6(9) 3_556 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.853 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.077 _database_code_depnum_ccdc_archive 'CCDC 948457' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rusr _audit_update_record ; 2013-07-03 # Formatted by publCIF ; _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H42 N10 P2 Ru, 2(P F6), 8.25(H2 O)' _chemical_formula_sum 'C62 H58.50 F12 N10 O8.25 P2 Ru' _chemical_formula_weight 1466.69 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_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 32.008(5) _cell_length_b 17.136(3) _cell_length_c 26.226(5) _cell_angle_alpha 90 _cell_angle_beta 105.545(3) _cell_angle_gamma 90 _cell_volume 13858(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1200 _cell_measurement_theta_min 4.12 _cell_measurement_theta_max 20.41 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_F_000 5988 _exptl_absorpt_coefficient_mu 0.363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9646 _exptl_absorpt_correction_T_max 0.9928 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 -0.027 0.250 771 388 ' ' 2 0.000 0.527 -0.250 771 380 ' ' 3 1.000 0.473 0.250 771 388 ' ' 4 0.500 0.027 -0.250 771 380 ' ' _platon_squeeze_details ; inlcuded as water and anions ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-APEX II' _diffrn_measurement_method \w+\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 54479 _diffrn_reflns_av_unetI/netI 0.2063 _diffrn_reflns_av_R_equivalents 0.1853 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.925 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_point_group_measured_fraction_full 0.990 _reflns_number_total 13990 _reflns_number_gt 6183 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT (Bruker-Nonius, 2003)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1297P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 13990 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1900 _refine_ls_R_factor_gt 0.0969 _refine_ls_wR_factor_ref 0.2739 _refine_ls_wR_factor_gt 0.2344 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C7 C 0.8688(2) 1.0565(4) 0.7747(3) 0.0381(16) Uani 1 1 d . . . . . C50 C 0.5781(2) 1.1228(4) 0.4046(3) 0.0491(19) Uani 1 1 d . . . . . H7 H 0.5581 1.1220 0.3716 0.059 Uiso 1 1 calc R U . . . C19 C 1.0283(2) 1.1178(4) 0.9799(3) 0.0444(17) Uani 1 1 d . . . . . H8 H 1.0547 1.1219 1.0054 0.053 Uiso 1 1 calc R U . . . C56 C 0.5267(3) 1.3449(5) 0.3338(3) 0.076(3) Uani 1 1 d . . . . . H9 H 0.4997 1.3480 0.3095 0.092 Uiso 1 1 calc R U . . . C39 C 0.6697(2) 1.0714(4) 0.5934(3) 0.0470(18) Uani 1 1 d . . . . . H10 H 0.6463 1.0375 0.5884 0.056 Uiso 1 1 calc R U . . . C8 C 0.9060(2) 1.0576(4) 0.8149(3) 0.0454(18) Uani 1 1 d . . . . . H13 H 0.9298 1.0285 0.8123 0.054 Uiso 1 1 calc R U . . . C32 C 0.7774(2) 1.2239(4) 0.6281(3) 0.0411(16) Uani 1 1 d . . . . . C9 C 0.9081(2) 1.1034(4) 0.8606(3) 0.0413(16) Uani 1 1 d . . . . . C49 C 0.5936(2) 1.1933(4) 0.4267(3) 0.0455(18) Uani 1 1 d . . . . . C47 C 0.6385(2) 1.1258(4) 0.5022(3) 0.0456(18) Uani 1 1 d . . . . . C16 C 0.9490(2) 1.1074(4) 0.9038(3) 0.0459(17) Uani 1 1 d . . . . . C38 C 0.7029(2) 1.0694(4) 0.6391(2) 0.0384(16) Uani 1 1 d . . . . . C11 C 0.8608(2) 1.0116(4) 0.7253(3) 0.0427(17) Uani 1 1 d . . . . . C46 C 0.6776(2) 0.9550(4) 0.6848(3) 0.057(2) Uani 1 1 d . . . . . H22 H 0.6528 0.9491 0.6569 0.068 Uiso 1 1 calc R U . . . C29 C 1.0538(3) 1.3296(6) 1.0733(4) 0.082(3) Uani 1 1 d . . . . . H23 H 1.0713 1.3295 1.1080 0.098 Uiso 1 1 calc R U . . . C13 C 0.8386(3) 0.9268(4) 0.6331(3) 0.057(2) Uani 1 1 d . . . . . H24 H 0.8306 0.8986 0.6016 0.068 Uiso 1 1 calc R U . . . C21 C 0.9608(2) 1.1754(4) 0.9330(3) 0.0433(17) Uani 1 1 d . . . . . H25 H 0.9417 1.2175 0.9271 0.052 Uiso 1 1 calc R U . . . C41 C 0.7061(2) 1.1793(4) 0.5637(3) 0.0437(17) Uani 1 1 d . . . . . H26 H 0.7072 1.2171 0.5387 0.052 Uiso 1 1 calc R U . . . C22 C 1.0486(2) 0.9823(4) 0.9607(3) 0.0453(17) Uani 1 1 d . . . . . C20 C 0.9998(2) 1.1817(4) 0.9702(3) 0.0433(17) Uani 1 1 d . . . . . C51 C 0.5918(2) 1.0524(4) 0.4306(3) 0.0447(17) Uani 1 1 d . . . . . C52 C 0.6229(2) 1.0559(4) 0.4787(3) 0.0479(18) Uani 1 1 d . . . . . H30 H 0.6337 1.0096 0.4958 0.058 Uiso 1 1 calc R U . . . C43 C 0.7498(2) 0.9755(4) 0.7669(3) 0.057(2) Uani 1 1 d . . . . . H31 H 0.7736 0.9835 0.7957 0.069 Uiso 1 1 calc R U . . . C3 C 0.7201(3) 1.2803(5) 0.7922(3) 0.072(3) Uani 1 1 d . . . . . H32 H 0.6943 1.3085 0.7848 0.087 Uiso 1 1 calc R U . . . C27 C 1.0142(2) 1.2566(4) 0.9984(3) 0.0456(18) Uani 1 1 d . . . . . C48 C 0.6237(2) 1.1957(4) 0.4752(3) 0.0461(18) Uani 1 1 d . . . . . H35 H 0.6342 1.2435 0.4901 0.055 Uiso 1 1 calc R U . . . C42 C 0.7073(2) 1.0135(4) 0.6841(3) 0.0418(17) Uani 1 1 d . . . . . C18 C 1.0175(2) 1.0476(4) 0.9516(3) 0.0411(16) Uani 1 1 d . . . . . C36 C 0.7851(3) 1.2884(4) 0.5997(3) 0.054(2) Uani 1 1 d . . . . . H39 H 0.7657 1.3011 0.5674 0.065 Uiso 1 1 calc R U . . . C37 C 0.7384(2) 1.1753(4) 0.6109(3) 0.0464(18) Uani 1 1 d . . . . . C57 C 0.5391(3) 1.2762(4) 0.3611(3) 0.063(2) Uani 1 1 d . . . . . H41 H 0.5202 1.2339 0.3551 0.076 Uiso 1 1 calc R U . . . C33 C 0.8420(2) 1.2463(4) 0.6926(3) 0.0474(18) Uani 1 1 d . . . . . H42 H 0.8618 1.2316 0.7240 0.057 Uiso 1 1 calc R U . . . C1 C 0.7960(2) 1.1950(4) 0.8116(3) 0.0420(17) Uani 1 1 d . . . . . C6 C 0.8359(2) 1.1482(4) 0.8187(3) 0.0440(17) Uani 1 1 d . . . . . C44 C 0.7214(3) 0.9151(5) 0.7683(3) 0.064(2) Uani 1 1 d . . . . . H45 H 0.7271 0.8812 0.7970 0.076 Uiso 1 1 calc R U . . . C31 C 1.0021(3) 1.3256(4) 0.9735(3) 0.058(2) Uani 1 1 d . . . . . H46 H 0.9838 1.3265 0.9393 0.070 Uiso 1 1 calc R U . . . C24 C 1.0704(3) 0.8570(5) 0.9394(4) 0.080(3) Uani 1 1 d . . . . . H47 H 1.0635 0.8125 0.9185 0.096 Uiso 1 1 calc R U . . . C2 C 0.7300(2) 1.2297(4) 0.7545(3) 0.061(2) Uani 1 1 d . . . . . H49 H 0.7101 1.2259 0.7215 0.073 Uiso 1 1 calc R U . . . C15 C 0.8877(3) 0.9528(4) 0.7165(3) 0.054(2) Uani 1 1 d . . . . . H50 H 0.9134 0.9417 0.7421 0.065 Uiso 1 1 calc R U . . . C40 C 0.6722(2) 1.1266(4) 0.5541(3) 0.0459(18) Uani 1 1 d . . . . . C10 C 0.8723(2) 1.1490(4) 0.8614(3) 0.0486(18) Uani 1 1 d . . . . . H52 H 0.8728 1.1799 0.8907 0.058 Uiso 1 1 calc R U . . . C17 C 0.9769(2) 1.0440(4) 0.9144(3) 0.0478(18) Uani 1 1 d . . . . . H53 H 0.9684 0.9976 0.8962 0.057 Uiso 1 1 calc R U . . . C34 C 0.8507(2) 1.3114(4) 0.6673(3) 0.053(2) Uani 1 1 d . . . . . H54 H 0.8757 1.3405 0.6815 0.064 Uiso 1 1 calc R U . . . C28 C 1.0405(3) 1.2589(4) 1.0495(3) 0.062(2) Uani 1 1 d . . . . . H55 H 1.0493 1.2127 1.0679 0.075 Uiso 1 1 calc R U . . . C35 C 0.8217(3) 1.3337(5) 0.6196(3) 0.063(2) Uani 1 1 d . . . . . H57 H 0.8268 1.3779 0.6017 0.075 Uiso 1 1 calc R U . . . C14 C 0.8769(3) 0.9111(4) 0.6707(3) 0.064(2) Uani 1 1 d . . . . . H59 H 0.8953 0.8722 0.6648 0.077 Uiso 1 1 calc R U . . . C26 C 1.0881(3) 0.9857(5) 0.9954(4) 0.073(3) Uani 1 1 d . . . . . H61 H 1.0962 1.0305 1.0157 0.087 Uiso 1 1 calc R U . . . C53 C 0.5793(3) 1.2698(4) 0.3973(3) 0.052(2) Uani 1 1 d . . . . . C4 C 0.7499(3) 1.2859(6) 0.8395(3) 0.082(3) Uani 1 1 d . . . . . H64 H 0.7444 1.3181 0.8655 0.099 Uiso 1 1 calc R U . . . C55 C 0.5931(3) 1.4026(4) 0.3766(4) 0.064(2) Uani 1 1 d . . . . . H66 H 0.6117 1.4453 0.3823 0.077 Uiso 1 1 calc R U . . . C54 C 0.6061(3) 1.3330(4) 0.4038(3) 0.056(2) Uani 1 1 d . . . . . H68 H 0.6337 1.3296 0.4269 0.067 Uiso 1 1 calc R U . . . C45 C 0.6854(3) 0.9057(5) 0.7278(4) 0.068(2) Uani 1 1 d . . . . . H69 H 0.6660 0.8659 0.7289 0.082 Uiso 1 1 calc R U . . . C25 C 1.1167(3) 0.9244(6) 1.0015(4) 0.082(3) Uani 1 1 d . . . . . H71 H 1.1432 0.9293 1.0270 0.098 Uiso 1 1 calc R U . . . C5 C 0.7883(3) 1.2446(5) 0.8501(3) 0.068(2) Uani 1 1 d . . . . . H72 H 0.8088 1.2499 0.8825 0.081 Uiso 1 1 calc R U . . . C23 C 1.0402(3) 0.9140(5) 0.9320(3) 0.063(2) Uani 1 1 d . . . . . H73 H 1.0135 0.9071 0.9074 0.075 Uiso 1 1 calc R U . . . C12 C 0.8124(2) 0.9853(4) 0.6433(3) 0.0490(19) Uani 1 1 d . . . . . H79 H 0.7868 0.9967 0.6178 0.059 Uiso 1 1 calc R U . . . C30 C 1.0174(3) 1.3958(5) 0.9994(4) 0.087(3) Uani 1 1 d . . . . . H82 H 1.0094 1.4424 0.9812 0.104 Uiso 1 1 calc R U . . . N1 N 0.76618(18) 1.1868(3) 0.7633(2) 0.0476(15) Uani 1 1 d . . . . . N2 N 0.83487(17) 1.1031(3) 0.7759(2) 0.0411(13) Uani 1 1 d . . . . . N3 N 0.82219(18) 1.0266(3) 0.6887(2) 0.0417(14) Uani 1 1 d . . . . . N8 N 0.74345(17) 1.0235(3) 0.7240(2) 0.0403(14) Uani 1 1 d . . . . . N7 N 0.73653(17) 1.1194(3) 0.6481(2) 0.0423(14) Uani 1 1 d . . . . . N6 N 0.80596(18) 1.2018(3) 0.6746(2) 0.0452(15) Uani 1 1 d . . . . . N4 N 1.1095(3) 0.8596(4) 0.9742(3) 0.075(2) Uani 1 1 d . . . . . N5 N 1.0429(3) 1.3989(4) 1.0492(3) 0.081(2) Uani 1 1 d . . . . . N9 N 0.5533(3) 1.4079(4) 0.3419(3) 0.075(2) Uani 1 1 d . . . . . Ru1 Ru 0.78481(2) 1.11051(3) 0.71267(2) 0.0416(2) Uani 1 1 d . . . . . O1 O 0.5743(3) 0.9625(5) 0.5992(4) 0.183(5) Uani 1 1 d . . . . . C62B C 0.5681(4) 0.9185(5) 0.4404(3) 0.042(3) Uani 0.5 1 d G . P A 1 H502 H 0.5770 0.9260 0.4768 0.050 Uiso 0.5 1 calc R U P A 1 C58B C 0.5725(4) 0.9783(4) 0.4064(4) 0.0750(15) Uani 0.5 1 d G . P A 1 C59B C 0.5592(4) 0.9670(5) 0.3519(4) 0.0750(15) Uani 0.5 1 d G . P A 1 H506 H 0.5622 1.0070 0.3292 0.090 Uiso 0.5 1 calc R U P A 1 C60B C 0.5414(4) 0.8959(6) 0.3315(3) 0.0750(15) Uani 0.5 1 d G . P A 1 H505 H 0.5325 0.8884 0.2950 0.090 Uiso 0.5 1 calc R U P A 1 N10B N 0.5369(4) 0.8361(5) 0.3654(4) 0.0750(15) Uani 0.5 1 d G . P A 1 C61B C 0.5503(4) 0.8474(5) 0.4199(4) 0.0750(15) Uani 0.5 1 d G . P A 1 H503 H 0.5473 0.8074 0.4426 0.090 Uiso 0.5 1 calc R U P A 1 C58A C 0.5771(4) 0.9748(5) 0.4053(5) 0.0750(15) Uani 0.5 1 d G . P A 2 C62A C 0.6054(3) 0.9116(6) 0.4141(5) 0.0750(15) Uani 0.5 1 d G . P A 2 H402 H 0.6334 0.9172 0.4358 0.090 Uiso 0.5 1 calc R U P A 2 C61A C 0.5917(3) 0.8400(5) 0.3905(5) 0.0750(15) Uani 0.5 1 d G . P A 2 H403 H 0.6106 0.7978 0.3964 0.090 Uiso 0.5 1 calc R U P A 2 N10A N 0.5498(3) 0.8317(5) 0.3581(4) 0.0750(15) Uani 0.5 1 d G . P A 2 C60A C 0.5215(3) 0.8949(6) 0.3493(4) 0.0750(15) Uani 0.5 1 d G . P A 2 H405 H 0.4934 0.8893 0.3277 0.090 Uiso 0.5 1 calc R U P A 2 C59A C 0.5352(4) 0.9664(5) 0.3729(5) 0.0750(15) Uani 0.5 1 d G . P A 2 H406 H 0.5163 1.0087 0.3670 0.090 Uiso 0.5 1 calc R U P A 2 P1 P 0.65008(8) 1.36720(13) 0.62788(10) 0.0718(7) Uani 1 1 d . . . . . F1 F 0.6583(2) 1.3810(3) 0.6900(2) 0.1025(19) Uani 1 1 d . . . . . F2 F 0.6422(2) 1.3532(4) 0.5657(2) 0.119(2) Uani 1 1 d . . . . . F3 F 0.60077(18) 1.3890(3) 0.6193(3) 0.111(2) Uani 1 1 d . . . . . F4 F 0.69996(17) 1.3469(3) 0.6367(2) 0.1015(19) Uani 1 1 d . . . . . F5 F 0.6605(2) 1.4560(3) 0.6204(2) 0.108(2) Uani 1 1 d . . . . . F6 F 0.6394(2) 1.2777(3) 0.6361(2) 0.117(2) Uani 1 1 d . . . . . O3 O 0.99949(19) 0.9598(3) 0.8026(2) 0.0676(16) Uani 1 1 d . . . . . O2 O 0.7593(14) 0.815(2) 0.5183(16) 0.159(14) Uiso 0.25 1 d . . P B 1 O5 O 1.0275(5) 0.8049(7) 0.8039(5) 0.078(4) Uiso 0.5 1 d . . P C 2 O4 O 0.9978(6) 0.7995(9) 0.8063(6) 0.112(5) Uiso 0.5 1 d . . P D 3 O9 O 0.8486(11) 1.3833(17) 0.9465(13) 0.114(10) Uiso 0.25 1 d . . P E 1 O10 O 0.8039(4) 1.3951(6) 0.9534(4) 0.112(3) Uiso 0.75 1 d . . P F 2 O8 O 0.8278(5) 1.2507(7) 0.9963(6) 0.208(8) Uani 0.75 1 d . . P . . O7 O 0.8827(6) 1.3348(9) 0.9305(7) 0.120(5) Uiso 0.5 1 d . . P G 2 O6 O 0.8921(11) 1.3323(18) 0.8975(15) 0.036(8) Uiso 0.125 1 d . . P H 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C7 0.035(4) 0.035(4) 0.042(4) -0.003(3) 0.006(3) 0.005(3) C50 0.051(4) 0.038(4) 0.048(5) 0.005(3) -0.004(3) -0.005(3) C19 0.038(4) 0.055(4) 0.038(4) 0.004(3) 0.006(3) 0.010(3) C56 0.090(7) 0.063(6) 0.064(6) 0.014(5) 0.000(5) 0.017(5) C39 0.045(4) 0.037(4) 0.048(5) 0.005(3) -0.005(3) -0.006(3) C8 0.043(4) 0.046(4) 0.041(5) -0.009(3) 0.001(3) 0.001(3) C32 0.039(4) 0.043(4) 0.038(4) -0.007(3) 0.006(3) -0.003(3) C9 0.038(4) 0.037(4) 0.044(4) 0.002(3) 0.003(3) 0.002(3) C49 0.055(4) 0.040(4) 0.039(4) 0.011(3) 0.008(3) 0.005(3) C47 0.049(4) 0.044(4) 0.039(4) -0.003(3) 0.004(3) -0.003(3) C16 0.041(4) 0.041(4) 0.049(5) -0.007(3) 0.001(3) 0.005(3) C38 0.047(4) 0.035(4) 0.030(4) 0.006(3) 0.005(3) -0.006(3) C11 0.037(4) 0.042(4) 0.041(5) 0.002(3) -0.001(3) 0.001(3) C46 0.056(5) 0.060(5) 0.044(5) 0.023(4) -0.005(4) -0.017(4) C29 0.071(6) 0.076(7) 0.077(7) -0.023(5) -0.017(5) 0.006(5) C13 0.057(5) 0.054(5) 0.056(5) -0.016(4) 0.009(4) -0.007(4) C21 0.038(4) 0.043(4) 0.046(5) -0.003(3) 0.006(3) 0.008(3) C41 0.050(4) 0.037(4) 0.034(4) 0.006(3) -0.006(3) -0.006(3) C22 0.050(4) 0.044(4) 0.040(4) 0.007(3) 0.010(3) 0.008(3) C20 0.048(4) 0.048(4) 0.032(4) 0.005(3) 0.007(3) 0.005(3) C51 0.056(4) 0.043(4) 0.031(4) -0.004(3) 0.004(3) -0.010(3) C52 0.060(5) 0.034(4) 0.040(5) 0.006(3) -0.003(4) 0.002(3) C43 0.051(5) 0.062(5) 0.051(5) 0.009(4) 0.000(4) -0.004(4) C3 0.054(5) 0.092(7) 0.064(6) -0.018(5) 0.004(4) 0.029(5) C27 0.045(4) 0.036(4) 0.052(5) -0.004(3) 0.007(3) 0.003(3) C48 0.051(4) 0.047(4) 0.034(4) -0.001(3) 0.002(3) -0.008(3) C42 0.042(4) 0.043(4) 0.037(4) 0.012(3) 0.004(3) -0.004(3) C18 0.036(4) 0.048(4) 0.037(4) -0.001(3) 0.005(3) 0.006(3) C36 0.061(5) 0.053(5) 0.046(5) 0.006(4) 0.011(4) -0.004(4) C37 0.057(5) 0.032(4) 0.048(5) 0.002(3) 0.010(4) -0.005(3) C57 0.080(6) 0.046(5) 0.054(5) 0.006(4) 0.000(4) 0.006(4) C33 0.036(4) 0.056(5) 0.048(5) -0.014(4) 0.008(3) -0.006(3) C1 0.037(4) 0.043(4) 0.039(4) -0.004(3) -0.001(3) 0.008(3) C6 0.040(4) 0.055(4) 0.036(4) -0.006(3) 0.010(3) 0.003(3) C44 0.052(5) 0.084(6) 0.051(5) 0.030(4) 0.009(4) -0.003(4) C31 0.068(5) 0.057(5) 0.047(5) -0.015(4) 0.009(4) -0.003(4) C24 0.081(7) 0.074(6) 0.075(7) -0.011(5) 0.005(5) 0.021(5) C2 0.051(5) 0.062(5) 0.055(5) 0.008(4) -0.012(4) 0.009(4) C15 0.054(5) 0.048(4) 0.058(5) -0.008(4) 0.010(4) -0.001(4) C40 0.042(4) 0.041(4) 0.046(5) 0.007(3) -0.003(3) -0.006(3) C10 0.037(4) 0.053(4) 0.051(5) -0.011(4) 0.005(3) 0.006(3) C17 0.049(4) 0.041(4) 0.049(5) -0.001(3) 0.005(3) 0.006(3) C34 0.049(5) 0.045(4) 0.066(6) -0.015(4) 0.017(4) -0.019(3) C28 0.070(5) 0.049(5) 0.052(5) -0.009(4) -0.013(4) 0.007(4) C35 0.070(6) 0.053(5) 0.069(6) 0.001(4) 0.026(5) -0.010(4) C14 0.083(6) 0.042(5) 0.072(6) -0.015(4) 0.029(5) 0.010(4) C26 0.058(5) 0.059(5) 0.085(7) -0.010(4) -0.008(5) 0.016(4) C53 0.071(5) 0.041(4) 0.043(5) 0.002(3) 0.011(4) 0.008(4) C4 0.068(6) 0.118(8) 0.052(6) -0.020(5) 0.000(5) 0.038(6) C55 0.076(6) 0.046(5) 0.078(6) 0.020(4) 0.032(5) 0.014(4) C54 0.065(5) 0.043(4) 0.062(6) 0.008(4) 0.020(4) 0.004(4) C45 0.059(5) 0.070(6) 0.074(6) 0.030(5) 0.015(5) -0.019(4) C25 0.064(6) 0.076(6) 0.086(7) 0.002(5) -0.016(5) 0.019(5) C5 0.057(5) 0.073(6) 0.066(6) -0.015(4) 0.005(4) 0.011(4) C23 0.067(5) 0.062(5) 0.051(5) -0.007(4) 0.001(4) 0.023(4) C12 0.056(5) 0.051(4) 0.036(5) -0.006(3) 0.006(4) -0.006(4) C30 0.090(7) 0.063(6) 0.092(8) -0.007(5) -0.003(6) 0.013(5) N1 0.042(3) 0.051(4) 0.044(4) 0.003(3) 0.000(3) 0.005(3) N2 0.037(3) 0.045(3) 0.038(3) -0.004(3) 0.004(2) 0.003(3) N3 0.044(3) 0.039(3) 0.043(4) -0.007(3) 0.013(3) -0.005(2) N8 0.036(3) 0.038(3) 0.042(4) 0.017(3) 0.001(3) -0.005(2) N7 0.038(3) 0.041(3) 0.044(4) 0.001(3) 0.004(3) -0.004(2) N6 0.048(4) 0.037(3) 0.047(4) -0.003(3) 0.005(3) -0.009(3) N4 0.080(5) 0.066(5) 0.073(5) 0.010(4) 0.011(4) 0.028(4) N5 0.078(5) 0.071(5) 0.084(6) -0.026(4) 0.005(5) -0.003(4) N9 0.100(6) 0.061(5) 0.063(5) 0.021(4) 0.020(4) 0.025(4) Ru1 0.0382(3) 0.0422(3) 0.0375(4) -0.0009(3) -0.0016(2) -0.0019(3) O1 0.156(8) 0.087(6) 0.226(11) 0.064(6) -0.088(8) -0.021(5) C62B 0.064(9) 0.035(7) 0.029(8) 0.002(6) 0.015(7) -0.005(6) C58B 0.082(4) 0.057(3) 0.073(3) -0.010(2) -0.002(3) -0.013(2) C59B 0.082(4) 0.057(3) 0.073(3) -0.010(2) -0.002(3) -0.013(2) C60B 0.082(4) 0.057(3) 0.073(3) -0.010(2) -0.002(3) -0.013(2) N10B 0.082(4) 0.057(3) 0.073(3) -0.010(2) -0.002(3) -0.013(2) C61B 0.082(4) 0.057(3) 0.073(3) -0.010(2) -0.002(3) -0.013(2) C58A 0.082(4) 0.057(3) 0.073(3) -0.010(2) -0.002(3) -0.013(2) C62A 0.082(4) 0.057(3) 0.073(3) -0.010(2) -0.002(3) -0.013(2) C61A 0.082(4) 0.057(3) 0.073(3) -0.010(2) -0.002(3) -0.013(2) N10A 0.082(4) 0.057(3) 0.073(3) -0.010(2) -0.002(3) -0.013(2) C60A 0.082(4) 0.057(3) 0.073(3) -0.010(2) -0.002(3) -0.013(2) C59A 0.082(4) 0.057(3) 0.073(3) -0.010(2) -0.002(3) -0.013(2) P1 0.0651(15) 0.0620(14) 0.0660(18) -0.0146(11) -0.0210(12) 0.0067(11) F1 0.118(5) 0.104(4) 0.073(4) -0.021(3) 0.003(3) 0.000(3) F2 0.132(5) 0.120(5) 0.072(4) -0.030(3) -0.028(4) 0.026(4) F3 0.065(3) 0.111(5) 0.131(5) -0.040(4) -0.019(3) 0.006(3) F4 0.067(4) 0.112(4) 0.106(5) -0.025(3) -0.011(3) 0.018(3) F5 0.121(5) 0.068(3) 0.108(5) -0.002(3) -0.019(4) 0.008(3) F6 0.135(6) 0.078(4) 0.113(5) -0.006(3) -0.007(4) -0.018(4) O3 0.081(4) 0.056(3) 0.058(4) -0.010(3) 0.005(3) -0.002(3) O8 0.216(15) 0.126(10) 0.212(14) -0.018(9) -0.063(12) 0.108(10) _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 C7 N2 1.355(8) . ? C7 C8 1.361(9) . ? C7 C11 1.470(9) . ? C50 C49 1.373(9) . ? C50 C51 1.398(9) . ? C50 H7 0.9300 . ? C19 C20 1.406(9) . ? C19 C18 1.408(9) . ? C19 H8 0.9300 . ? C56 N9 1.355(11) . ? C56 C57 1.378(10) . ? C56 H9 0.9300 . ? C39 C38 1.372(9) . ? C39 C40 1.418(9) . ? C39 H10 0.9300 . ? C8 C9 1.420(9) . ? C8 H13 0.9300 . ? C32 N6 1.367(8) . ? C32 C36 1.391(9) . ? C32 C37 1.466(9) . ? C9 C10 1.392(9) . ? C9 C16 1.487(9) . ? C49 C48 1.375(9) . ? C49 C53 1.527(9) . ? C47 C52 1.378(9) . ? C47 C48 1.408(9) . ? C47 C40 1.491(9) . ? C16 C17 1.388(9) . ? C16 C21 1.388(9) . ? C38 N7 1.346(8) . ? C38 C42 1.497(9) . ? C11 N3 1.369(8) . ? C11 C15 1.386(10) . ? C46 C45 1.376(10) . ? C46 C42 1.385(9) . ? C46 H22 0.9300 . ? C29 N5 1.346(11) . ? C29 C28 1.377(11) . ? C29 H23 0.9300 . ? C13 C12 1.380(10) . ? C13 C14 1.380(11) . ? C13 H24 0.9300 . ? C21 C20 1.367(9) . ? C21 H25 0.9300 . ? C41 C40 1.381(9) . ? C41 C37 1.387(9) . ? C41 H26 0.9300 . ? C22 C26 1.347(10) . ? C22 C23 1.378(10) . ? C22 C18 1.475(9) . ? C20 C27 1.492(9) . ? C51 C52 1.384(9) . ? C51 C58B 1.478(9) . ? C51 C58A 1.504(9) . ? C52 H30 0.9300 . ? C43 N8 1.365(8) . ? C43 C44 1.384(10) . ? C43 H31 0.9300 . ? C3 C4 1.351(11) . ? C3 C2 1.413(11) . ? C3 H32 0.9300 . ? C27 C31 1.357(10) . ? C27 C28 1.381(10) . ? C48 H35 0.9300 . ? C42 N8 1.348(8) . ? C18 C17 1.402(9) . ? C36 C35 1.385(10) . ? C36 H39 0.9300 . ? C37 N7 1.379(8) . ? C57 C53 1.384(10) . ? C57 H41 0.9300 . ? C33 N6 1.357(8) . ? C33 C34 1.366(10) . ? C33 H42 0.9300 . ? C1 N1 1.373(8) . ? C1 C5 1.391(10) . ? C1 C6 1.477(9) . ? C6 N2 1.355(8) . ? C6 C10 1.384(9) . ? C44 C45 1.350(11) . ? C44 H45 0.9300 . ? C31 C30 1.403(11) . ? C31 H46 0.9300 . ? C24 N4 1.337(11) . ? C24 C23 1.351(11) . ? C24 H47 0.9300 . ? C2 N1 1.338(9) . ? C2 H49 0.9300 . ? C15 C14 1.360(10) . ? C15 H50 0.9300 . ? C10 H52 0.9300 . ? C17 H53 0.9300 . ? C34 C35 1.396(11) . ? C34 H54 0.9300 . ? C28 H55 0.9300 . ? C35 H57 0.9300 . ? C14 H59 0.9300 . ? C26 C25 1.375(11) . ? C26 H61 0.9300 . ? C53 C54 1.364(10) . ? C4 C5 1.380(11) . ? C4 H64 0.9300 . ? C55 N9 1.357(11) . ? C55 C54 1.394(10) . ? C55 H66 0.9300 . ? C54 H68 0.9300 . ? C45 H69 0.9300 . ? C25 N4 1.309(11) . ? C25 H71 0.9300 . ? C5 H72 0.9300 . ? C23 H73 0.9300 . ? C12 N3 1.348(8) . ? C12 H79 0.9300 . ? C30 N5 1.344(11) . ? C30 H82 0.9300 . ? N1 Ru1 2.063(6) . ? N2 Ru1 1.977(5) . ? N3 Ru1 2.073(5) . ? N8 Ru1 2.067(5) . ? N7 Ru1 1.969(5) . ? N6 Ru1 2.066(5) . ? C62B C58B 1.3900 . ? C62B C61B 1.3900 . ? C62B H502 0.9300 . ? C58B C59B 1.3900 . ? C59B C60B 1.3900 . ? C59B H506 0.9300 . ? C60B N10B 1.3900 . ? C60B H505 0.9300 . ? N10B C61B 1.3900 . ? C61B H503 0.9300 . ? C58A C62A 1.3900 . ? C58A C59A 1.3900 . ? C62A C61A 1.3900 . ? C62A H402 0.9300 . ? C61A N10A 1.3900 . ? C61A H403 0.9300 . ? N10A C60A 1.3900 . ? C60A C59A 1.3900 . ? C60A H405 0.9300 . ? C59A H406 0.9300 . ? P1 F3 1.578(6) . ? P1 F5 1.582(6) . ? P1 F4 1.589(6) . ? P1 F1 1.597(6) . ? P1 F6 1.598(6) . ? P1 F2 1.599(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 N2 C7 C8 120.9(6) . . ? N2 C7 C11 112.1(5) . . ? C8 C7 C11 126.8(6) . . ? C49 C50 C51 121.6(6) . . ? C49 C50 H7 119.2 . . ? C51 C50 H7 119.2 . . ? C20 C19 C18 120.9(6) . . ? C20 C19 H8 119.5 . . ? C18 C19 H8 119.5 . . ? N9 C56 C57 121.3(8) . . ? N9 C56 H9 119.4 . . ? C57 C56 H9 119.4 . . ? C38 C39 C40 118.1(6) . . ? C38 C39 H10 120.9 . . ? C40 C39 H10 120.9 . . ? C7 C8 C9 119.6(6) . . ? C7 C8 H13 120.2 . . ? C9 C8 H13 120.2 . . ? N6 C32 C36 121.6(6) . . ? N6 C32 C37 115.3(6) . . ? C36 C32 C37 123.1(6) . . ? C10 C9 C8 118.1(6) . . ? C10 C9 C16 121.5(6) . . ? C8 C9 C16 120.2(6) . . ? C50 C49 C48 120.0(6) . . ? C50 C49 C53 121.1(6) . . ? C48 C49 C53 118.8(6) . . ? C52 C47 C48 118.8(6) . . ? C52 C47 C40 120.2(6) . . ? C48 C47 C40 120.9(6) . . ? C17 C16 C21 118.8(6) . . ? C17 C16 C9 120.2(6) . . ? C21 C16 C9 120.9(6) . . ? N7 C38 C39 122.2(6) . . ? N7 C38 C42 111.6(5) . . ? C39 C38 C42 126.2(6) . . ? N3 C11 C15 120.3(6) . . ? N3 C11 C7 115.6(6) . . ? C15 C11 C7 123.8(6) . . ? C45 C46 C42 118.7(7) . . ? C45 C46 H22 120.6 . . ? C42 C46 H22 120.6 . . ? N5 C29 C28 123.6(8) . . ? N5 C29 H23 118.2 . . ? C28 C29 H23 118.2 . . ? C12 C13 C14 118.2(7) . . ? C12 C13 H24 120.9 . . ? C14 C13 H24 120.9 . . ? C20 C21 C16 121.4(6) . . ? C20 C21 H25 119.3 . . ? C16 C21 H25 119.3 . . ? C40 C41 C37 119.6(6) . . ? C40 C41 H26 120.2 . . ? C37 C41 H26 120.2 . . ? C26 C22 C23 114.7(7) . . ? C26 C22 C18 123.2(7) . . ? C23 C22 C18 122.1(7) . . ? C21 C20 C19 119.6(6) . . ? C21 C20 C27 121.6(6) . . ? C19 C20 C27 118.7(6) . . ? C52 C51 C50 117.5(6) . . ? C52 C51 C58B 123.0(7) . . ? C50 C51 C58B 119.5(7) . . ? C52 C51 C58A 120.3(7) . . ? C50 C51 C58A 121.9(7) . . ? C47 C52 C51 122.1(6) . . ? C47 C52 H30 118.9 . . ? C51 C52 H30 118.9 . . ? N8 C43 C44 121.4(7) . . ? N8 C43 H31 119.3 . . ? C44 C43 H31 119.3 . . ? C4 C3 C2 116.8(7) . . ? C4 C3 H32 121.6 . . ? C2 C3 H32 121.6 . . ? C31 C27 C28 117.7(7) . . ? C31 C27 C20 120.1(7) . . ? C28 C27 C20 122.2(6) . . ? C49 C48 C47 119.8(6) . . ? C49 C48 H35 120.1 . . ? C47 C48 H35 120.1 . . ? N8 C42 C46 122.1(6) . . ? N8 C42 C38 114.2(5) . . ? C46 C42 C38 123.7(6) . . ? C17 C18 C19 117.1(6) . . ? C17 C18 C22 122.7(6) . . ? C19 C18 C22 120.2(6) . . ? C35 C36 C32 119.7(7) . . ? C35 C36 H39 120.1 . . ? C32 C36 H39 120.1 . . ? N7 C37 C41 120.1(6) . . ? N7 C37 C32 111.9(6) . . ? C41 C37 C32 128.0(6) . . ? C56 C57 C53 120.6(8) . . ? C56 C57 H41 119.7 . . ? C53 C57 H41 119.7 . . ? N6 C33 C34 123.7(7) . . ? N6 C33 H42 118.2 . . ? C34 C33 H42 118.2 . . ? N1 C1 C5 121.1(6) . . ? N1 C1 C6 115.1(6) . . ? C5 C1 C6 123.8(6) . . ? N2 C6 C10 120.3(6) . . ? N2 C6 C1 112.2(6) . . ? C10 C6 C1 127.5(6) . . ? C45 C44 C43 119.6(7) . . ? C45 C44 H45 120.2 . . ? C43 C44 H45 120.2 . . ? C27 C31 C30 119.7(8) . . ? C27 C31 H46 120.1 . . ? C30 C31 H46 120.1 . . ? N4 C24 C23 125.2(9) . . ? N4 C24 H47 117.4 . . ? C23 C24 H47 117.4 . . ? N1 C2 C3 124.2(7) . . ? N1 C2 H49 117.9 . . ? C3 C2 H49 117.9 . . ? C14 C15 C11 120.4(7) . . ? C14 C15 H50 119.8 . . ? C11 C15 H50 119.8 . . ? C41 C40 C39 119.8(6) . . ? C41 C40 C47 120.9(6) . . ? C39 C40 C47 119.4(6) . . ? C6 C10 C9 119.9(7) . . ? C6 C10 H52 120.0 . . ? C9 C10 H52 120.0 . . ? C16 C17 C18 122.1(6) . . ? C16 C17 H53 118.9 . . ? C18 C17 H53 118.9 . . ? C33 C34 C35 119.0(7) . . ? C33 C34 H54 120.5 . . ? C35 C34 H54 120.5 . . ? C29 C28 C27 119.9(8) . . ? C29 C28 H55 120.0 . . ? C27 C28 H55 120.0 . . ? C36 C35 C34 118.6(7) . . ? C36 C35 H57 120.7 . . ? C34 C35 H57 120.7 . . ? C15 C14 C13 119.8(7) . . ? C15 C14 H59 120.1 . . ? C13 C14 H59 120.1 . . ? C22 C26 C25 121.3(8) . . ? C22 C26 H61 119.3 . . ? C25 C26 H61 119.3 . . ? C54 C53 C57 117.4(7) . . ? C54 C53 C49 121.7(7) . . ? C57 C53 C49 120.8(7) . . ? C3 C4 C5 121.3(8) . . ? C3 C4 H64 119.4 . . ? C5 C4 H64 119.4 . . ? N9 C55 C54 119.9(8) . . ? N9 C55 H66 120.0 . . ? C54 C55 H66 120.0 . . ? C53 C54 C55 121.5(8) . . ? C53 C54 H68 119.2 . . ? C55 C54 H68 119.2 . . ? C44 C45 C46 120.1(7) . . ? C44 C45 H69 120.0 . . ? C46 C45 H69 120.0 . . ? N4 C25 C26 124.8(8) . . ? N4 C25 H71 117.6 . . ? C26 C25 H71 117.6 . . ? C4 C5 C1 119.3(8) . . ? C4 C5 H72 120.4 . . ? C1 C5 H72 120.4 . . ? C24 C23 C22 120.5(8) . . ? C24 C23 H73 119.8 . . ? C22 C23 H73 119.8 . . ? N3 C12 C13 122.9(7) . . ? N3 C12 H79 118.5 . . ? C13 C12 H79 118.5 . . ? N5 C30 C31 123.2(9) . . ? N5 C30 H82 118.4 . . ? C31 C30 H82 118.4 . . ? C2 N1 C1 117.3(6) . . ? C2 N1 Ru1 128.6(5) . . ? C1 N1 Ru1 114.1(4) . . ? C7 N2 C6 120.9(6) . . ? C7 N2 Ru1 119.6(4) . . ? C6 N2 Ru1 119.5(4) . . ? C12 N3 C11 118.2(6) . . ? C12 N3 Ru1 127.9(5) . . ? C11 N3 Ru1 113.8(4) . . ? C42 N8 C43 118.0(6) . . ? C42 N8 Ru1 115.5(4) . . ? C43 N8 Ru1 126.5(5) . . ? C38 N7 C37 120.1(6) . . ? C38 N7 Ru1 120.5(4) . . ? C37 N7 Ru1 119.3(4) . . ? C33 N6 C32 117.4(6) . . ? C33 N6 Ru1 127.9(5) . . ? C32 N6 Ru1 114.4(4) . . ? C25 N4 C24 113.5(7) . . ? C30 N5 C29 115.8(8) . . ? C56 N9 C55 119.2(7) . . ? N7 Ru1 N2 177.7(2) . . ? N7 Ru1 N1 102.1(2) . . ? N2 Ru1 N1 79.0(2) . . ? N7 Ru1 N6 79.0(2) . . ? N2 Ru1 N6 99.1(2) . . ? N1 Ru1 N6 91.2(2) . . ? N7 Ru1 N8 78.1(2) . . ? N2 Ru1 N8 103.9(2) . . ? N1 Ru1 N8 93.3(2) . . ? N6 Ru1 N8 157.1(2) . . ? N7 Ru1 N3 100.2(2) . . ? N2 Ru1 N3 78.8(2) . . ? N1 Ru1 N3 157.6(2) . . ? N6 Ru1 N3 95.1(2) . . ? N8 Ru1 N3 89.3(2) . . ? C58B C62B C61B 120.0 . . ? C58B C62B H502 120.0 . . ? C61B C62B H502 120.0 . . ? C59B C58B C62B 120.0 . . ? C59B C58B C51 122.6(7) . . ? C62B C58B C51 117.4(7) . . ? C60B C59B C58B 120.0 . . ? C60B C59B H506 120.0 . . ? C58B C59B H506 120.0 . . ? C59B C60B N10B 120.0 . . ? C59B C60B H505 120.0 . . ? N10B C60B H505 120.0 . . ? C61B N10B C60B 120.0 . . ? N10B C61B C62B 120.0 . . ? N10B C61B H503 120.0 . . ? C62B C61B H503 120.0 . . ? C62A C58A C59A 120.0 . . ? C62A C58A C51 120.2(8) . . ? C59A C58A C51 119.8(8) . . ? C58A C62A C61A 120.0 . . ? C58A C62A H402 120.0 . . ? C61A C62A H402 120.0 . . ? C62A C61A N10A 120.0 . . ? C62A C61A H403 120.0 . . ? N10A C61A H403 120.0 . . ? C61A N10A C60A 120.0 . . ? N10A C60A C59A 120.0 . . ? N10A C60A H405 120.0 . . ? C59A C60A H405 120.0 . . ? C60A C59A C58A 120.0 . . ? C60A C59A H406 120.0 . . ? C58A C59A H406 120.0 . . ? F3 P1 F5 89.4(3) . . ? F3 P1 F4 178.9(3) . . ? F5 P1 F4 89.5(3) . . ? F3 P1 F1 89.7(4) . . ? F5 P1 F1 90.0(3) . . ? F4 P1 F1 90.0(3) . . ? F3 P1 F6 90.3(4) . . ? F5 P1 F6 179.3(4) . . ? F4 P1 F6 90.8(4) . . ? F1 P1 F6 89.3(3) . . ? F3 P1 F2 90.6(4) . . ? F5 P1 F2 90.0(3) . . ? F4 P1 F2 89.7(4) . . ? F1 P1 F2 179.7(4) . . ? F6 P1 F2 90.7(3) . . ? 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 N2 C7 C8 C9 5.2(10) . . . . ? C11 C7 C8 C9 -178.9(6) . . . . ? C7 C8 C9 C10 -3.2(10) . . . . ? C7 C8 C9 C16 -177.7(6) . . . . ? C51 C50 C49 C48 1.0(12) . . . . ? C51 C50 C49 C53 178.3(7) . . . . ? C10 C9 C16 C17 154.1(7) . . . . ? C8 C9 C16 C17 -31.5(10) . . . . ? C10 C9 C16 C21 -28.4(11) . . . . ? C8 C9 C16 C21 146.0(7) . . . . ? C40 C39 C38 N7 2.2(11) . . . . ? C40 C39 C38 C42 -177.2(7) . . . . ? N2 C7 C11 N3 2.6(9) . . . . ? C8 C7 C11 N3 -173.5(7) . . . . ? N2 C7 C11 C15 -171.8(7) . . . . ? C8 C7 C11 C15 12.0(12) . . . . ? C17 C16 C21 C20 2.4(11) . . . . ? C9 C16 C21 C20 -175.1(7) . . . . ? C16 C21 C20 C19 -1.1(11) . . . . ? C16 C21 C20 C27 174.9(7) . . . . ? C18 C19 C20 C21 0.6(11) . . . . ? C18 C19 C20 C27 -175.5(7) . . . . ? C49 C50 C51 C52 -2.6(11) . . . . ? C49 C50 C51 C58B 177.0(8) . . . . ? C49 C50 C51 C58A -176.2(9) . . . . ? C48 C47 C52 C51 -2.9(12) . . . . ? C40 C47 C52 C51 -179.9(7) . . . . ? C50 C51 C52 C47 3.6(11) . . . . ? C58B C51 C52 C47 -176.0(8) . . . . ? C58A C51 C52 C47 177.3(9) . . . . ? C21 C20 C27 C31 -32.0(11) . . . . ? C19 C20 C27 C31 143.9(7) . . . . ? C21 C20 C27 C28 149.3(8) . . . . ? C19 C20 C27 C28 -34.7(11) . . . . ? C50 C49 C48 C47 -0.2(11) . . . . ? C53 C49 C48 C47 -177.6(7) . . . . ? C52 C47 C48 C49 1.1(11) . . . . ? C40 C47 C48 C49 178.1(7) . . . . ? C45 C46 C42 N8 0.0(13) . . . . ? C45 C46 C42 C38 178.5(8) . . . . ? N7 C38 C42 N8 -0.3(9) . . . . ? C39 C38 C42 N8 179.1(7) . . . . ? N7 C38 C42 C46 -179.0(7) . . . . ? C39 C38 C42 C46 0.5(12) . . . . ? C20 C19 C18 C17 -1.4(10) . . . . ? C20 C19 C18 C22 177.4(6) . . . . ? C26 C22 C18 C17 178.4(8) . . . . ? C23 C22 C18 C17 1.9(11) . . . . ? C26 C22 C18 C19 -0.3(11) . . . . ? C23 C22 C18 C19 -176.8(7) . . . . ? N6 C32 C36 C35 -2.5(11) . . . . ? C37 C32 C36 C35 176.9(7) . . . . ? C40 C41 C37 N7 -0.4(11) . . . . ? C40 C41 C37 C32 178.2(7) . . . . ? N6 C32 C37 N7 5.0(9) . . . . ? C36 C32 C37 N7 -174.5(7) . . . . ? N6 C32 C37 C41 -173.7(7) . . . . ? C36 C32 C37 C41 6.8(12) . . . . ? N9 C56 C57 C53 -0.5(14) . . . . ? N1 C1 C6 N2 -2.2(9) . . . . ? C5 C1 C6 N2 178.3(7) . . . . ? N1 C1 C6 C10 175.3(7) . . . . ? C5 C1 C6 C10 -4.3(13) . . . . ? N8 C43 C44 C45 -3.5(13) . . . . ? C28 C27 C31 C30 1.6(12) . . . . ? C20 C27 C31 C30 -177.1(8) . . . . ? C4 C3 C2 N1 1.1(14) . . . . ? N3 C11 C15 C14 2.3(11) . . . . ? C7 C11 C15 C14 176.5(7) . . . . ? C37 C41 C40 C39 2.9(11) . . . . ? C37 C41 C40 C47 -175.7(7) . . . . ? C38 C39 C40 C41 -3.7(11) . . . . ? C38 C39 C40 C47 174.9(6) . . . . ? C52 C47 C40 C41 139.6(8) . . . . ? C48 C47 C40 C41 -37.4(11) . . . . ? C52 C47 C40 C39 -39.1(11) . . . . ? C48 C47 C40 C39 144.0(7) . . . . ? N2 C6 C10 C9 0.2(11) . . . . ? C1 C6 C10 C9 -177.1(7) . . . . ? C8 C9 C10 C6 0.5(11) . . . . ? C16 C9 C10 C6 175.0(7) . . . . ? C21 C16 C17 C18 -3.3(11) . . . . ? C9 C16 C17 C18 174.3(7) . . . . ? C19 C18 C17 C16 2.8(11) . . . . ? C22 C18 C17 C16 -176.0(7) . . . . ? N6 C33 C34 C35 -1.0(12) . . . . ? N5 C29 C28 C27 -0.8(15) . . . . ? C31 C27 C28 C29 -0.3(13) . . . . ? C20 C27 C28 C29 178.4(8) . . . . ? C32 C36 C35 C34 2.1(12) . . . . ? C33 C34 C35 C36 -0.4(12) . . . . ? C11 C15 C14 C13 -0.9(12) . . . . ? C12 C13 C14 C15 0.3(12) . . . . ? C23 C22 C26 C25 -1.2(13) . . . . ? C18 C22 C26 C25 -177.9(8) . . . . ? C56 C57 C53 C54 -1.3(12) . . . . ? C56 C57 C53 C49 -178.7(8) . . . . ? C50 C49 C53 C54 -148.9(8) . . . . ? C48 C49 C53 C54 28.5(11) . . . . ? C50 C49 C53 C57 28.5(11) . . . . ? C48 C49 C53 C57 -154.2(8) . . . . ? C2 C3 C4 C5 0.8(16) . . . . ? C57 C53 C54 C55 2.3(12) . . . . ? C49 C53 C54 C55 179.7(7) . . . . ? N9 C55 C54 C53 -1.5(12) . . . . ? C43 C44 C45 C46 1.4(14) . . . . ? C42 C46 C45 C44 0.4(14) . . . . ? C22 C26 C25 N4 2.2(16) . . . . ? C3 C4 C5 C1 -1.5(15) . . . . ? N1 C1 C5 C4 0.4(13) . . . . ? C6 C1 C5 C4 180.0(8) . . . . ? N4 C24 C23 C22 1.4(15) . . . . ? C26 C22 C23 C24 -0.5(13) . . . . ? C18 C22 C23 C24 176.3(8) . . . . ? C14 C13 C12 N3 -1.2(12) . . . . ? C27 C31 C30 N5 -2.0(15) . . . . ? C3 C2 N1 C1 -2.1(12) . . . . ? C3 C2 N1 Ru1 179.7(6) . . . . ? C5 C1 N1 C2 1.3(11) . . . . ? C6 C1 N1 C2 -178.2(6) . . . . ? C5 C1 N1 Ru1 179.7(6) . . . . ? C6 C1 N1 Ru1 0.2(8) . . . . ? C8 C7 N2 C6 -4.5(10) . . . . ? C11 C7 N2 C6 179.1(6) . . . . ? C8 C7 N2 Ru1 171.6(5) . . . . ? C11 C7 N2 Ru1 -4.9(8) . . . . ? C10 C6 N2 C7 1.8(10) . . . . ? C1 C6 N2 C7 179.4(6) . . . . ? C10 C6 N2 Ru1 -174.3(5) . . . . ? C1 C6 N2 Ru1 3.4(8) . . . . ? C13 C12 N3 C11 2.6(10) . . . . ? C13 C12 N3 Ru1 -175.4(6) . . . . ? C15 C11 N3 C12 -3.1(10) . . . . ? C7 C11 N3 C12 -177.7(6) . . . . ? C15 C11 N3 Ru1 175.2(5) . . . . ? C7 C11 N3 Ru1 0.5(7) . . . . ? C46 C42 N8 C43 -2.0(11) . . . . ? C38 C42 N8 C43 179.3(6) . . . . ? C46 C42 N8 Ru1 176.8(6) . . . . ? C38 C42 N8 Ru1 -1.9(8) . . . . ? C44 C43 N8 C42 3.8(11) . . . . ? C44 C43 N8 Ru1 -174.8(6) . . . . ? C39 C38 N7 C37 0.2(10) . . . . ? C42 C38 N7 C37 179.7(6) . . . . ? C39 C38 N7 Ru1 -176.8(5) . . . . ? C42 C38 N7 Ru1 2.6(8) . . . . ? C41 C37 N7 C38 -1.2(10) . . . . ? C32 C37 N7 C38 -180.0(6) . . . . ? C41 C37 N7 Ru1 175.9(5) . . . . ? C32 C37 N7 Ru1 -2.9(8) . . . . ? C34 C33 N6 C32 0.7(10) . . . . ? C34 C33 N6 Ru1 -171.9(5) . . . . ? C36 C32 N6 C33 1.1(10) . . . . ? C37 C32 N6 C33 -178.4(6) . . . . ? C36 C32 N6 Ru1 174.7(6) . . . . ? C37 C32 N6 Ru1 -4.8(8) . . . . ? C26 C25 N4 C24 -1.3(15) . . . . ? C23 C24 N4 C25 -0.4(15) . . . . ? C31 C30 N5 C29 0.9(15) . . . . ? C28 C29 N5 C30 0.5(15) . . . . ? C57 C56 N9 C55 1.4(13) . . . . ? C54 C55 N9 C56 -0.4(13) . . . . ? C61B C62B C58B C59B 0.0 . . . . ? C61B C62B C58B C51 -179.9(10) . . . . ? C52 C51 C58B C59B -147.7(7) . . . . ? C50 C51 C58B C59B 32.7(11) . . . . ? C58A C51 C58B C59B -81(6) . . . . ? C52 C51 C58B C62B 32.2(12) . . . . ? C50 C51 C58B C62B -147.3(7) . . . . ? C58A C51 C58B C62B 99(6) . . . . ? C62B C58B C59B C60B 0.0 . . . . ? C51 C58B C59B C60B 179.9(11) . . . . ? C58B C59B C60B N10B 0.0 . . . . ? C59B C60B N10B C61B 0.0 . . . . ? C60B N10B C61B C62B 0.0 . . . . ? C58B C62B C61B N10B 0.0 . . . . ? C52 C51 C58A C62A -29.5(12) . . . . ? C50 C51 C58A C62A 143.9(8) . . . . ? C58B C51 C58A C62A -146(7) . . . . ? C52 C51 C58A C59A 150.6(8) . . . . ? C50 C51 C58A C59A -36.0(12) . . . . ? C58B C51 C58A C59A 34(6) . . . . ? C59A C58A C62A C61A 0.0 . . . . ? C51 C58A C62A C61A -179.9(11) . . . . ? C58A C62A C61A N10A 0.0 . . . . ? C62A C61A N10A C60A 0.0 . . . . ? C61A N10A C60A C59A 0.0 . . . . ? N10A C60A C59A C58A 0.0 . . . . ? C62A C58A C59A C60A 0.0 . . . . ? C51 C58A C59A C60A 179.9(11) . . . . ? _refine_diff_density_max 0.986 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.108 _database_code_depnum_ccdc_archive 'CCDC 948463' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_squeezed _audit_update_record ; 2013-07-03 # Formatted by publCIF ; _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H42 N10 P2 Fe, 2(P F6), 6(C H3 N O2), 12.5(H2 O)' _chemical_formula_sum 'C68 H81 F12 Fe N16 O22.50 P2' _chemical_formula_weight 1828.27 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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 C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_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 31.977(4) _cell_length_b 16.992(2) _cell_length_c 26.943(3) _cell_angle_alpha 90 _cell_angle_beta 106.844(2) _cell_angle_gamma 90 _cell_volume 14011(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1125 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 22.16 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_F_000 7560 _exptl_absorpt_coefficient_mu 0.389 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9523 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.270 -0.250 0.020 1294 336 ' ' 2 0.770 0.250 0.020 1294 336 ' ' _platon_squeeze_details ; included as disordered anions and solvent ; _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-APEX II' _diffrn_measurement_method \w+\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 57055 _diffrn_reflns_av_unetI/netI 0.1096 _diffrn_reflns_av_R_equivalents 0.0957 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.959 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.994 _reflns_number_total 14269 _reflns_number_gt 6998 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT (Bruker-Nonius, 2003)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1810P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 14269 _refine_ls_number_parameters 788 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1529 _refine_ls_R_factor_gt 0.0968 _refine_ls_wR_factor_ref 0.3023 _refine_ls_wR_factor_gt 0.2683 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.967 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.64167(14) 0.5088(3) 0.77510(17) 0.0467(10) Uani 1 1 d . . . . . C7 C 0.63326(14) 0.5558(3) 0.72680(16) 0.0470(10) Uani 1 1 d . . . . . C8 C 0.59535(14) 0.5551(3) 0.68594(17) 0.0508(11) Uani 1 1 d . . . . . H79 H 0.5721 0.5230 0.6871 0.061 Uiso 1 1 calc R U . . . C37 C 0.79501(14) 0.5699(3) 0.85755(16) 0.0494(11) Uani 1 1 d . . . . . C51 C 0.90531(16) 0.5530(3) 1.06516(17) 0.0563(12) Uani 1 1 d . . . . . C41 C 0.82785(16) 0.5715(3) 0.90480(17) 0.0549(12) Uani 1 1 d . . . . . H82 H 0.8511 0.5364 0.9110 0.066 Uiso 1 1 calc R U . . . C47 C 0.85830(15) 0.6259(3) 0.99406(17) 0.0529(12) Uani 1 1 d . . . . . C40 C 0.82547(15) 0.6259(3) 0.94249(16) 0.0500(11) Uani 1 1 d . . . . . C9 C 0.59213(14) 0.6029(3) 0.64284(18) 0.0514(11) Uani 1 1 d . . . . . C48 C 0.87285(15) 0.6949(3) 1.02100(17) 0.0515(11) Uani 1 1 d . . . . . H87 H 0.8619 0.7428 1.0062 0.062 Uiso 1 1 calc R U . . . C49 C 0.90348(14) 0.6940(3) 1.06963(16) 0.0471(10) Uani 1 1 d . . . . . C39 C 0.79056(14) 0.6780(3) 0.93166(16) 0.0489(11) Uani 1 1 d . . . . . H89 H 0.7888 0.7161 0.9558 0.059 Uiso 1 1 calc R U . . . C20 C 0.49963(15) 0.6810(3) 0.53293(17) 0.0511(11) Uani 1 1 d . . . . . C34 C 0.7776(2) 0.4264(4) 0.7275(2) 0.0803(17) Uani 1 1 d . . . . . H91 H 0.7724 0.3957 0.6977 0.096 Uiso 1 1 calc R U . . . C38 C 0.75830(14) 0.6728(3) 0.88449(16) 0.0482(10) Uani 1 1 d . . . . . C52 C 0.87491(16) 0.5539(3) 1.01707(17) 0.0546(12) Uani 1 1 d . . . . . H94 H 0.8654 0.5068 0.9998 0.066 Uiso 1 1 calc R U . . . C53 C 0.91798(15) 0.7693(3) 1.09861(16) 0.0501(11) Uani 1 1 d . . . . . C6 C 0.66507(14) 0.6496(3) 0.68628(17) 0.0502(11) Uani 1 1 d . . . . . C16 C 0.55154(15) 0.6069(3) 0.59894(16) 0.0511(11) Uani 1 1 d . . . . . C13 C 0.66623(19) 0.4280(3) 0.8658(2) 0.0680(14) Uani 1 1 d . . . . . H99 H 0.6753 0.4015 0.8973 0.082 Uiso 1 1 calc R U . . . C17 C 0.52336(16) 0.5424(3) 0.58774(18) 0.0555(12) Uani 1 1 d . . . . . H101 H 0.5315 0.4958 0.6062 0.067 Uiso 1 1 calc R U . . . C21 C 0.53918(15) 0.6753(3) 0.57076(18) 0.0568(12) Uani 1 1 d . . . . . H102 H 0.5579 0.7184 0.5774 0.068 Uiso 1 1 calc R U . . . C32 C 0.79125(15) 0.5161(3) 0.81434(17) 0.0538(12) Uani 1 1 d . . . . . C18 C 0.48333(15) 0.5461(3) 0.54965(17) 0.0524(11) Uani 1 1 d . . . . . C1 C 0.70479(15) 0.6969(3) 0.69432(18) 0.0559(12) Uani 1 1 d . . . . . C10 C 0.62809(15) 0.6503(3) 0.64329(17) 0.0566(12) Uani 1 1 d . . . . . H106 H 0.6273 0.6822 0.6150 0.068 Uiso 1 1 calc R U . . . C42 C 0.71839(14) 0.7211(3) 0.86628(17) 0.0484(11) Uani 1 1 d . . . . . C27 C 0.48615(16) 0.7573(3) 0.5047(2) 0.0621(13) Uani 1 1 d . . . . . C5 C 0.71288(18) 0.7490(3) 0.6592(2) 0.0756(16) Uani 1 1 d . . . . . H109 H 0.6925 0.7551 0.6268 0.091 Uiso 1 1 calc R U . . . C54 C 0.89176(17) 0.8353(3) 1.0909(2) 0.0613(13) Uani 1 1 d . . . . . H110 H 0.8644 0.8347 1.0665 0.074 Uiso 1 1 calc R U . . . C55 C 0.9062(2) 0.9014(3) 1.1194(2) 0.0717(15) Uani 1 1 d . . . . . H111 H 0.8876 0.9446 1.1140 0.086 Uiso 1 1 calc R U . . . C22 C 0.45291(16) 0.4774(3) 0.53980(18) 0.0574(12) Uani 1 1 d . . . . . C43 C 0.65394(15) 0.7379(3) 0.80019(19) 0.0550(12) Uani 1 1 d . . . . . H113 H 0.6342 0.7212 0.7694 0.066 Uiso 1 1 calc R U . . . C25 C 0.3867(2) 0.4130(5) 0.4934(4) 0.118(3) Uani 1 1 d . . . . . H114 H 0.3623 0.4123 0.4645 0.141 Uiso 1 1 calc R U . . . C12 C 0.69166(17) 0.4870(3) 0.85458(19) 0.0593(12) Uani 1 1 d . . . . . H115 H 0.7180 0.4991 0.8792 0.071 Uiso 1 1 calc R U . . . C14 C 0.62722(19) 0.4085(3) 0.8300(2) 0.0702(14) Uani 1 1 d . . . . . H116 H 0.6098 0.3681 0.8362 0.084 Uiso 1 1 calc R U . . . C33 C 0.74785(17) 0.4839(3) 0.73094(19) 0.0627(13) Uani 1 1 d . . . . . H117 H 0.7229 0.4914 0.7032 0.075 Uiso 1 1 calc R U . . . C44 C 0.64410(16) 0.8037(3) 0.8244(2) 0.0621(13) Uani 1 1 d . . . . . H118 H 0.6189 0.8323 0.8089 0.075 Uiso 1 1 calc R U . . . C46 C 0.70895(15) 0.7855(3) 0.89237(18) 0.0551(12) Uani 1 1 d . . . . . H119 H 0.7281 0.8006 0.9240 0.066 Uiso 1 1 calc R U . . . C36 C 0.82148(17) 0.4610(3) 0.8110(2) 0.0718(15) Uani 1 1 d . . . . . H120 H 0.8468 0.4547 0.8384 0.086 Uiso 1 1 calc R U . . . C3 C 0.7794(2) 0.7843(4) 0.7210(2) 0.0869(19) Uani 1 1 d . . . . . H122 H 0.8046 0.8147 0.7310 0.104 Uiso 1 1 calc R U . . . C2 C 0.77022(15) 0.7314(3) 0.7552(2) 0.0632(13) Uani 1 1 d . . . . . H123 H 0.7900 0.7258 0.7879 0.076 Uiso 1 1 calc R U . . . C45 C 0.67123(16) 0.8269(3) 0.8713(2) 0.0604(13) Uani 1 1 d . . . . . H124 H 0.6642 0.8701 0.8885 0.072 Uiso 1 1 calc R U . . . C4 C 0.7504(2) 0.7917(4) 0.6713(2) 0.093(2) Uani 1 1 d . . . . . H126 H 0.7566 0.8252 0.6470 0.111 Uiso 1 1 calc R U . . . C56 C 0.9701(2) 0.8443(3) 1.1614(2) 0.0750(16) Uani 1 1 d . . . . . H128 H 0.9974 0.8466 1.1860 0.090 Uiso 1 1 calc R U . . . C15 C 0.61502(17) 0.4520(3) 0.78410(19) 0.0606(13) Uani 1 1 d . . . . . H129 H 0.5884 0.4419 0.7595 0.073 Uiso 1 1 calc R U . . . C35 C 0.81459(19) 0.4150(4) 0.7677(2) 0.0798(18) Uani 1 1 d . . . . . H130 H 0.8347 0.3765 0.7656 0.096 Uiso 1 1 calc R U . . . C23 C 0.4606(3) 0.4129(4) 0.5702(3) 0.113(3) Uani 1 1 d . . . . . H131 H 0.4866 0.4073 0.5965 0.136 Uiso 1 1 calc R U . . . C31 C 0.49857(19) 0.8273(3) 0.5286(2) 0.0777(17) Uani 1 1 d . . . . . H133 H 0.5179 0.8285 0.5619 0.093 Uiso 1 1 calc R U . . . C29 C 0.4453(2) 0.8304(5) 0.4312(3) 0.099(2) Uani 1 1 d . . . . . H134 H 0.4262 0.8301 0.3978 0.119 Uiso 1 1 calc R U . . . C24 C 0.4285(3) 0.3544(5) 0.5613(3) 0.142(4) Uani 1 1 d . . . . . H138 H 0.4338 0.3124 0.5843 0.170 Uiso 1 1 calc R U . . . C30 C 0.4829(2) 0.8960(4) 0.5042(3) 0.100(2) Uani 1 1 d . . . . . H140 H 0.4895 0.9429 0.5226 0.120 Uiso 1 1 calc R U . . . C28 C 0.45892(19) 0.7593(4) 0.4545(2) 0.0808(17) Uani 1 1 d . . . . . H1 H 0.4499 0.7127 0.4365 0.097 Uiso 1 1 calc R U . . . C26 C 0.41425(19) 0.4796(4) 0.4996(2) 0.0853(18) Uani 1 1 d . . . . . H2 H 0.4068 0.5229 0.4776 0.102 Uiso 1 1 calc R U . . . C19 C 0.47216(15) 0.6169(3) 0.52268(16) 0.0503(11) Uani 1 1 d . . . . . H3 H 0.4455 0.6209 0.4972 0.060 Uiso 1 1 calc R U . . . C57 C 0.95841(16) 0.7763(3) 1.13541(19) 0.0606(13) Uani 1 1 d . . . . . H4 H 0.9775 0.7337 1.1421 0.073 Uiso 1 1 calc R U . . . C50 C 0.91976(15) 0.6234(2) 1.09060(17) 0.0509(11) Uani 1 1 d . . . . . H5 H 0.9410 0.6224 1.1226 0.061 Uiso 1 1 calc R U . . . N9 N 0.94496(18) 0.9087(3) 1.15427(19) 0.0768(13) Uani 1 1 d . . . . . N4 N 0.3922(2) 0.3528(4) 0.5242(2) 0.105(2) Uani 1 1 d . . . . . N5 N 0.45761(19) 0.8982(4) 0.4533(3) 0.110(2) Uani 1 1 d . . . . . N1 N 0.73316(12) 0.6871(2) 0.74252(14) 0.0545(10) Uani 1 1 d . . . . . N2 N 0.66714(12) 0.6025(2) 0.72709(13) 0.0469(9) Uani 1 1 d . . . . . N3 N 0.68059(12) 0.5280(2) 0.81023(13) 0.0468(9) Uani 1 1 d . . . . . N6 N 0.75407(12) 0.5291(2) 0.77358(14) 0.0517(9) Uani 1 1 d . . . . . N8 N 0.69129(12) 0.6970(2) 0.81960(14) 0.0492(9) Uani 1 1 d . . . . . N7 N 0.76064(12) 0.6193(2) 0.84853(14) 0.0479(9) Uani 1 1 d . . . . . C62A C 0.9301(11) 0.4152(15) 1.0576(12) 0.1062(12) Uani 0.25 1 d . . P A 1 H502 H 0.9238 0.4203 1.0219 0.127 Uiso 0.25 1 calc R U P A 1 C58A C 0.9226(3) 0.4752(4) 1.0898(3) 0.1062(12) Uani 0.25 1 d . . P A 1 C59A C 0.9330(11) 0.4627(16) 1.1451(12) 0.1062(12) Uani 0.25 1 d . . P A 1 H506 H 0.9290 0.5027 1.1669 0.127 Uiso 0.25 1 calc R U P A 1 C60A C 0.9479(11) 0.3951(16) 1.1636(13) 0.1062(12) Uani 0.25 1 d . . P A 1 H505 H 0.9538 0.3872 1.1991 0.127 Uiso 0.25 1 calc R U P A 1 N10A N 0.9559(2) 0.3326(3) 1.1335(2) 0.1062(12) Uani 0.25 1 d . . P A 1 C61A C 0.9485(11) 0.3451(15) 1.0853(12) 0.1062(12) Uani 0.25 1 d . . P A 1 H503 H 0.9558 0.3049 1.0659 0.127 Uiso 0.25 1 calc R U P A 1 Fe1 Fe 0.71468(2) 0.61015(4) 0.78687(2) 0.0476(2) Uani 1 1 d . . . . . C58B C 0.9226(3) 0.4752(4) 1.0898(3) 0.1062(12) Uani 0.75 1 d . . P A 2 C62B C 0.8963(4) 0.4086(5) 1.0793(4) 0.1062(12) Uani 0.75 1 d . . P A 2 H402 H 0.8685 0.4109 1.0560 0.127 Uiso 0.75 1 calc R U P A 2 C61B C 0.9122(4) 0.3390(5) 1.1038(4) 0.1062(12) Uani 0.75 1 d . . P A 2 H403 H 0.8937 0.2959 1.1007 0.127 Uiso 0.75 1 calc R U P A 2 N10B N 0.9559(2) 0.3326(3) 1.1335(2) 0.1062(12) Uani 0.75 1 d . . P A 2 C60B C 0.9714(4) 0.3918(5) 1.1490(4) 0.1062(12) Uani 0.75 1 d . . P A 2 H405 H 0.9944 0.3902 1.1794 0.127 Uiso 0.75 1 calc R U P A 2 C59B C 0.9598(4) 0.4656(5) 1.1276(4) 0.1062(12) Uani 0.75 1 d . . P A 2 H406 H 0.9779 0.5085 1.1397 0.127 Uiso 0.75 1 calc R U P A 2 P1 P 0.34812(6) 0.62877(10) 0.37809(7) 0.0830(5) Uani 1 1 d . . . . . F1 F 0.34077(15) 0.6158(2) 0.31754(15) 0.1146(14) Uani 1 1 d . . . . . F2 F 0.39856(13) 0.6090(2) 0.38707(19) 0.1281(16) Uani 1 1 d . . . . . F3 F 0.33877(15) 0.5385(2) 0.38274(16) 0.1168(14) Uani 1 1 d . . . . . F4 F 0.29829(13) 0.6493(3) 0.36678(17) 0.1216(14) Uani 1 1 d . . . . . F5 F 0.35833(16) 0.7191(2) 0.3719(2) 0.1337(16) Uani 1 1 d . . . . . F6 F 0.35704(16) 0.6421(3) 0.43690(16) 0.1292(16) Uani 1 1 d . . . . . O1 O 0.49883(13) 0.4612(2) 0.69848(14) 0.0771(11) Uani 1 1 d . . . . . O2 O 0.3771(4) 0.1917(7) 0.4503(5) 0.141(4) Uiso 0.5 1 d . . P B 1 O3 O 0.3832(8) 0.1639(14) 0.4164(10) 0.129(7) Uiso 0.25 1 d . . P C 2 O4 O 0.3273(13) 0.256(2) 0.4920(16) 0.220(14) Uiso 0.25 1 d . . P . . O5 O 0.21694(16) 0.3863(3) 0.53969(19) 0.1138(17) Uani 1 1 d D . . . . N11 N 0.0669(2) 0.6616(5) 0.1827(2) 0.101(2) Uani 1 1 d . . . . . O6 O 0.0394(5) 0.6183(7) 0.1628(6) 0.276(6) Uani 1 1 d . . . . . O7 O 0.0996(4) 0.6828(6) 0.1678(7) 0.328(9) Uani 1 1 d D . . . . C63 C 0.0604(4) 0.7153(8) 0.2108(5) 0.234(8) Uani 1 1 d D . . . . H55A H 0.0542 0.7632 0.1912 0.351 Uiso 1 1 calc R U . . . H55B H 0.0859 0.7223 0.2398 0.351 Uiso 1 1 calc R U . . . H55C H 0.0360 0.7019 0.2231 0.351 Uiso 1 1 calc R U . . . O8 O 0.0827(2) 0.4577(4) 0.5885(3) 0.215(4) Uani 1 1 d . . . . . O9 O 0.0214(9) 0.6158(15) 0.2534(13) 0.167(11) Uiso 0.25 1 d . . P . . O10 O 0.6980(14) 0.090(2) 0.8607(16) 0.227(15) Uiso 0.25 1 d . . P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.046(2) 0.041(2) 0.048(3) 0.001(2) 0.0053(19) 0.004(2) C7 0.045(2) 0.048(3) 0.043(2) 0.004(2) 0.0050(19) 0.001(2) C8 0.040(2) 0.055(3) 0.048(3) 0.005(2) -0.0020(19) 0.000(2) C37 0.045(3) 0.052(3) 0.041(2) -0.005(2) -0.0033(19) 0.005(2) C51 0.064(3) 0.053(3) 0.043(3) 0.001(2) 0.000(2) 0.016(2) C41 0.057(3) 0.046(3) 0.048(3) -0.008(2) -0.007(2) 0.012(2) C47 0.053(3) 0.054(3) 0.039(2) -0.003(2) -0.0058(19) 0.010(2) C40 0.049(3) 0.051(3) 0.039(2) -0.005(2) -0.0048(19) 0.006(2) C9 0.040(2) 0.057(3) 0.048(3) -0.001(2) -0.0015(19) -0.005(2) C48 0.055(3) 0.042(3) 0.049(3) -0.001(2) 0.001(2) 0.011(2) C49 0.049(3) 0.048(3) 0.038(2) -0.002(2) 0.0034(19) 0.000(2) C39 0.052(3) 0.046(3) 0.039(2) -0.0044(19) -0.0004(19) 0.005(2) C20 0.047(3) 0.056(3) 0.043(2) 0.001(2) 0.0017(19) -0.008(2) C34 0.075(4) 0.091(4) 0.065(3) -0.035(3) 0.004(3) 0.008(3) C38 0.047(3) 0.047(3) 0.043(2) 0.005(2) 0.0016(19) 0.006(2) C52 0.064(3) 0.043(3) 0.047(3) -0.007(2) -0.001(2) 0.004(2) C53 0.055(3) 0.052(3) 0.038(2) 0.001(2) 0.006(2) -0.002(2) C6 0.042(2) 0.052(3) 0.048(3) 0.002(2) 0.0019(19) -0.005(2) C16 0.045(2) 0.062(3) 0.038(2) 0.000(2) -0.0015(19) -0.006(2) C13 0.080(4) 0.062(3) 0.057(3) 0.016(3) 0.011(3) 0.008(3) C17 0.055(3) 0.049(3) 0.051(3) 0.003(2) -0.002(2) -0.002(2) C21 0.053(3) 0.056(3) 0.052(3) 0.006(2) -0.002(2) -0.009(2) C32 0.043(3) 0.060(3) 0.051(3) -0.011(2) 0.002(2) 0.000(2) C18 0.048(3) 0.060(3) 0.044(2) -0.006(2) 0.005(2) -0.010(2) C1 0.051(3) 0.057(3) 0.049(3) 0.003(2) -0.003(2) -0.006(2) C10 0.052(3) 0.065(3) 0.042(2) 0.009(2) -0.004(2) -0.002(2) C42 0.048(3) 0.049(3) 0.044(2) 0.005(2) 0.006(2) 0.003(2) C27 0.049(3) 0.065(3) 0.059(3) 0.016(3) -0.005(2) -0.007(2) C5 0.068(4) 0.089(4) 0.055(3) 0.011(3) -0.004(3) -0.029(3) C54 0.060(3) 0.050(3) 0.066(3) -0.005(2) 0.006(2) 0.001(2) C55 0.072(4) 0.055(3) 0.083(4) -0.014(3) 0.015(3) 0.002(3) C22 0.057(3) 0.063(3) 0.048(3) -0.007(2) 0.007(2) -0.013(2) C43 0.045(3) 0.060(3) 0.053(3) 0.008(2) 0.004(2) 0.002(2) C25 0.071(4) 0.105(6) 0.147(7) -0.012(5) -0.016(4) -0.029(4) C12 0.061(3) 0.056(3) 0.053(3) 0.004(2) 0.002(2) 0.010(2) C14 0.075(4) 0.066(3) 0.067(3) 0.010(3) 0.015(3) 0.002(3) C33 0.057(3) 0.071(3) 0.049(3) -0.020(3) -0.001(2) -0.006(3) C44 0.051(3) 0.058(3) 0.070(3) 0.017(3) 0.006(2) 0.011(2) C46 0.052(3) 0.055(3) 0.052(3) -0.001(2) 0.004(2) 0.002(2) C36 0.055(3) 0.083(4) 0.063(3) -0.019(3) -0.008(2) 0.018(3) C3 0.068(4) 0.105(5) 0.075(4) 0.011(3) 0.000(3) -0.031(3) C2 0.044(3) 0.078(4) 0.057(3) 0.001(3) -0.003(2) -0.015(3) C45 0.059(3) 0.049(3) 0.072(3) 0.004(2) 0.018(3) 0.012(2) C4 0.076(4) 0.117(5) 0.074(4) 0.019(4) 0.003(3) -0.042(4) C56 0.086(4) 0.067(4) 0.057(3) -0.018(3) -0.002(3) -0.013(3) C15 0.061(3) 0.058(3) 0.053(3) 0.008(2) 0.001(2) -0.004(2) C35 0.067(4) 0.090(4) 0.071(4) -0.034(3) 0.001(3) 0.023(3) C23 0.135(6) 0.093(5) 0.071(4) 0.032(4) -0.034(4) -0.061(5) C31 0.070(4) 0.065(4) 0.082(4) 0.020(3) -0.004(3) -0.012(3) C29 0.080(4) 0.108(6) 0.082(4) 0.034(4) -0.018(3) -0.012(4) C24 0.180(9) 0.129(7) 0.078(5) 0.036(5) -0.025(5) -0.091(7) C30 0.092(5) 0.076(4) 0.117(6) 0.026(4) 0.008(4) -0.013(4) C28 0.075(4) 0.076(4) 0.063(3) 0.016(3) -0.024(3) -0.012(3) C26 0.060(3) 0.081(4) 0.094(4) 0.006(3) -0.010(3) -0.022(3) C19 0.044(2) 0.060(3) 0.038(2) 0.007(2) -0.0016(18) -0.009(2) C57 0.059(3) 0.055(3) 0.056(3) -0.004(2) -0.002(2) 0.004(2) C50 0.058(3) 0.045(3) 0.037(2) -0.0055(19) -0.005(2) 0.006(2) N9 0.094(4) 0.060(3) 0.071(3) -0.014(2) 0.016(3) -0.014(3) N4 0.122(5) 0.093(4) 0.087(4) 0.004(3) 0.007(4) -0.052(4) N5 0.078(4) 0.094(4) 0.133(6) 0.055(4) -0.012(4) -0.005(3) N1 0.043(2) 0.061(3) 0.050(2) -0.0026(19) -0.0008(17) 0.0014(18) N2 0.044(2) 0.049(2) 0.042(2) 0.0050(17) 0.0032(15) -0.0003(17) N3 0.048(2) 0.046(2) 0.043(2) 0.0040(16) 0.0077(16) 0.0132(17) N6 0.045(2) 0.058(2) 0.044(2) -0.0053(18) -0.0002(16) 0.0009(18) N8 0.045(2) 0.051(2) 0.046(2) 0.0058(17) 0.0042(16) 0.0040(17) N7 0.041(2) 0.047(2) 0.047(2) -0.0028(17) 0.0007(16) 0.0070(17) C62A 0.124(3) 0.0653(18) 0.097(2) 0.0060(18) -0.018(2) 0.016(2) C58A 0.124(3) 0.0653(18) 0.097(2) 0.0060(18) -0.018(2) 0.016(2) C59A 0.124(3) 0.0653(18) 0.097(2) 0.0060(18) -0.018(2) 0.016(2) C60A 0.124(3) 0.0653(18) 0.097(2) 0.0060(18) -0.018(2) 0.016(2) N10A 0.124(3) 0.0653(18) 0.097(2) 0.0060(18) -0.018(2) 0.016(2) C61A 0.124(3) 0.0653(18) 0.097(2) 0.0060(18) -0.018(2) 0.016(2) Fe1 0.0411(4) 0.0514(4) 0.0408(4) -0.0001(3) -0.0033(3) 0.0022(3) C58B 0.124(3) 0.0653(18) 0.097(2) 0.0060(18) -0.018(2) 0.016(2) C62B 0.124(3) 0.0653(18) 0.097(2) 0.0060(18) -0.018(2) 0.016(2) C61B 0.124(3) 0.0653(18) 0.097(2) 0.0060(18) -0.018(2) 0.016(2) N10B 0.124(3) 0.0653(18) 0.097(2) 0.0060(18) -0.018(2) 0.016(2) C60B 0.124(3) 0.0653(18) 0.097(2) 0.0060(18) -0.018(2) 0.016(2) C59B 0.124(3) 0.0653(18) 0.097(2) 0.0060(18) -0.018(2) 0.016(2) P1 0.0725(10) 0.0736(11) 0.0749(11) -0.0119(8) -0.0229(8) 0.0043(8) F1 0.121(3) 0.126(3) 0.073(2) -0.012(2) -0.009(2) -0.001(2) F2 0.080(3) 0.123(3) 0.145(4) -0.032(3) -0.024(2) 0.018(2) F3 0.135(4) 0.083(3) 0.109(3) -0.004(2) -0.001(3) -0.002(2) F4 0.086(3) 0.126(3) 0.129(3) -0.021(3) -0.007(2) 0.019(2) F5 0.127(4) 0.088(3) 0.153(4) -0.003(3) -0.011(3) -0.010(3) F6 0.138(4) 0.133(3) 0.087(3) -0.027(3) -0.015(2) 0.011(3) O1 0.094(3) 0.063(2) 0.064(2) 0.0049(18) 0.007(2) 0.000(2) O5 0.101(4) 0.108(4) 0.099(3) 0.035(3) -0.023(3) -0.020(3) N11 0.057(3) 0.130(6) 0.083(4) -0.037(4) -0.032(3) 0.022(4) O6 0.263(14) 0.234(11) 0.314(15) -0.079(10) 0.056(12) -0.027(10) O7 0.189(11) 0.175(9) 0.56(3) 0.024(12) 0.017(14) 0.003(8) C63 0.188(12) 0.223(13) 0.179(11) -0.094(11) -0.123(9) 0.088(11) O8 0.166(6) 0.148(6) 0.229(8) 0.094(5) -0.101(6) -0.078(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 C15 1.355(6) . ? C11 N3 1.367(5) . ? C11 C7 1.483(6) . ? C7 N2 1.342(6) . ? C7 C8 1.381(6) . ? C8 C9 1.396(6) . ? C8 H79 0.9300 . ? C37 N7 1.347(5) . ? C37 C41 1.396(6) . ? C37 C32 1.458(6) . ? C51 C52 1.376(6) . ? C51 C50 1.390(6) . ? C51 C58A 1.509(7) . ? C41 C40 1.392(6) . ? C41 H82 0.9300 . ? C47 C48 1.386(6) . ? C47 C52 1.405(6) . ? C47 C40 1.479(6) . ? C40 C39 1.388(6) . ? C9 C10 1.402(6) . ? C9 C16 1.483(6) . ? C48 C49 1.390(6) . ? C48 H87 0.9300 . ? C49 C50 1.363(6) . ? C49 C53 1.501(6) . ? C39 C38 1.388(6) . ? C39 H89 0.9300 . ? C20 C19 1.375(6) . ? C20 C21 1.378(6) . ? C20 C27 1.501(7) . ? C34 C35 1.367(8) . ? C34 C33 1.385(8) . ? C34 H91 0.9300 . ? C38 N7 1.347(5) . ? C38 C42 1.476(6) . ? C52 H94 0.9300 . ? C53 C54 1.379(6) . ? C53 C57 1.387(6) . ? C6 N2 1.345(6) . ? C6 C10 1.395(6) . ? C6 C1 1.465(6) . ? C16 C21 1.383(6) . ? C16 C17 1.395(6) . ? C13 C14 1.378(8) . ? C13 C12 1.379(7) . ? C13 H99 0.9300 . ? C17 C18 1.391(6) . ? C17 H101 0.9300 . ? C21 H102 0.9300 . ? C32 C36 1.367(7) . ? C32 N6 1.383(5) . ? C18 C19 1.398(6) . ? C18 C22 1.492(6) . ? C1 N1 1.362(6) . ? C1 C5 1.375(7) . ? C10 H106 0.9300 . ? C42 N8 1.367(6) . ? C42 C46 1.381(6) . ? C27 C31 1.357(7) . ? C27 C28 1.382(7) . ? C5 C4 1.358(7) . ? C5 H109 0.9300 . ? C54 C55 1.364(7) . ? C54 H110 0.9300 . ? C55 N9 1.326(7) . ? C55 H111 0.9300 . ? C22 C23 1.348(7) . ? C22 C26 1.389(7) . ? C43 N8 1.350(6) . ? C43 C44 1.375(7) . ? C43 H113 0.9300 . ? C25 N4 1.296(9) . ? C25 C26 1.414(9) . ? C25 H114 0.9300 . ? C12 N3 1.339(6) . ? C12 H115 0.9300 . ? C14 C15 1.395(7) . ? C14 H116 0.9300 . ? C33 N6 1.349(6) . ? C33 H117 0.9300 . ? C44 C45 1.367(7) . ? C44 H118 0.9300 . ? C46 C45 1.370(6) . ? C46 H119 0.9300 . ? C36 C35 1.370(7) . ? C36 H120 0.9300 . ? C3 C2 1.377(7) . ? C3 C4 1.398(8) . ? C3 H122 0.9300 . ? C2 N1 1.361(6) . ? C2 H123 0.9300 . ? C45 H124 0.9300 . ? C4 H126 0.9300 . ? C56 N9 1.339(7) . ? C56 C57 1.347(7) . ? C56 H128 0.9300 . ? C15 H129 0.9300 . ? C35 H130 0.9300 . ? C23 C24 1.397(9) . ? C23 H131 0.9300 . ? C31 C30 1.362(8) . ? C31 H133 0.9300 . ? C29 N5 1.304(9) . ? C29 C28 1.371(8) . ? C29 H134 0.9300 . ? C24 N4 1.294(9) . ? C24 H138 0.9300 . ? C30 N5 1.377(9) . ? C30 H140 0.9300 . ? C28 H1 0.9300 . ? C26 H2 0.9300 . ? C19 H3 0.9300 . ? C57 H4 0.9300 . ? C50 H5 0.9300 . ? N1 Fe1 1.974(4) . ? N2 Fe1 1.872(4) . ? N3 Fe1 1.983(4) . ? N6 Fe1 1.968(4) . ? N8 Fe1 1.974(4) . ? N7 Fe1 1.879(4) . ? C62A C58A 1.40(3) . ? C62A C61A 1.44(3) . ? C62A H502 0.9300 . ? C58A C59A 1.45(3) . ? C59A C60A 1.29(3) . ? C59A H506 0.9300 . ? C60A N10A 1.40(3) . ? C60A H505 0.9300 . ? N10A C61A 1.27(3) . ? C61A H503 0.9300 . ? C62B C61B 1.379(11) . ? C62B H402 0.9300 . ? C61B H403 0.9300 . ? C60B C59B 1.385(12) . ? C60B H405 0.9300 . ? C59B H406 0.9300 . ? P1 F6 1.543(4) . ? P1 F4 1.572(4) . ? P1 F3 1.575(4) . ? P1 F5 1.588(4) . ? P1 F1 1.595(4) . ? P1 F2 1.596(5) . ? N11 O6 1.154(11) . ? N11 C63 1.241(12) . ? N11 O7 1.276(15) . ? C63 H55A 0.9600 . ? C63 H55B 0.9600 . ? C63 H55C 0.9600 . ? O9 O9 1.32(5) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 C11 N3 122.7(4) . . ? C15 C11 C7 125.2(4) . . ? N3 C11 C7 112.1(4) . . ? N2 C7 C8 122.0(4) . . ? N2 C7 C11 111.9(4) . . ? C8 C7 C11 126.1(4) . . ? C7 C8 C9 119.6(4) . . ? C7 C8 H79 120.2 . . ? C9 C8 H79 120.2 . . ? N7 C37 C41 120.8(4) . . ? N7 C37 C32 111.9(4) . . ? C41 C37 C32 127.3(4) . . ? C52 C51 C50 119.9(4) . . ? C52 C51 C58A 119.5(5) . . ? C50 C51 C58A 120.7(5) . . ? C40 C41 C37 119.5(4) . . ? C40 C41 H82 120.3 . . ? C37 C41 H82 120.3 . . ? C48 C47 C52 118.6(4) . . ? C48 C47 C40 122.1(4) . . ? C52 C47 C40 119.3(4) . . ? C39 C40 C41 118.8(4) . . ? C39 C40 C47 120.4(4) . . ? C41 C40 C47 120.8(4) . . ? C8 C9 C10 117.7(4) . . ? C8 C9 C16 121.8(4) . . ? C10 C9 C16 120.5(4) . . ? C47 C48 C49 121.5(4) . . ? C47 C48 H87 119.3 . . ? C49 C48 H87 119.3 . . ? C50 C49 C48 118.7(4) . . ? C50 C49 C53 120.7(4) . . ? C48 C49 C53 120.5(4) . . ? C38 C39 C40 119.4(4) . . ? C38 C39 H89 120.3 . . ? C40 C39 H89 120.3 . . ? C19 C20 C21 119.3(4) . . ? C19 C20 C27 120.6(4) . . ? C21 C20 C27 120.1(4) . . ? C35 C34 C33 120.0(5) . . ? C35 C34 H91 120.0 . . ? C33 C34 H91 120.0 . . ? N7 C38 C39 121.3(4) . . ? N7 C38 C42 111.0(4) . . ? C39 C38 C42 127.6(4) . . ? C51 C52 C47 119.9(4) . . ? C51 C52 H94 120.1 . . ? C47 C52 H94 120.1 . . ? C54 C53 C57 116.0(4) . . ? C54 C53 C49 122.2(4) . . ? C57 C53 C49 121.8(4) . . ? N2 C6 C10 120.9(4) . . ? N2 C6 C1 111.7(4) . . ? C10 C6 C1 127.4(4) . . ? C21 C16 C17 118.6(4) . . ? C21 C16 C9 121.4(4) . . ? C17 C16 C9 119.9(4) . . ? C14 C13 C12 119.5(5) . . ? C14 C13 H99 120.2 . . ? C12 C13 H99 120.2 . . ? C18 C17 C16 121.5(4) . . ? C18 C17 H101 119.2 . . ? C16 C17 H101 119.2 . . ? C20 C21 C16 121.3(4) . . ? C20 C21 H102 119.3 . . ? C16 C21 H102 119.3 . . ? C36 C32 N6 121.3(4) . . ? C36 C32 C37 125.8(4) . . ? N6 C32 C37 112.7(4) . . ? C17 C18 C19 117.7(4) . . ? C17 C18 C22 120.6(4) . . ? C19 C18 C22 121.7(4) . . ? N1 C1 C5 121.9(4) . . ? N1 C1 C6 112.5(4) . . ? C5 C1 C6 125.4(4) . . ? C6 C10 C9 119.8(4) . . ? C6 C10 H106 120.1 . . ? C9 C10 H106 120.1 . . ? N8 C42 C46 122.1(4) . . ? N8 C42 C38 113.3(4) . . ? C46 C42 C38 124.5(4) . . ? C31 C27 C28 117.2(5) . . ? C31 C27 C20 121.1(5) . . ? C28 C27 C20 121.7(5) . . ? C4 C5 C1 120.6(5) . . ? C4 C5 H109 119.7 . . ? C1 C5 H109 119.7 . . ? C55 C54 C53 119.5(5) . . ? C55 C54 H110 120.2 . . ? C53 C54 H110 120.2 . . ? N9 C55 C54 124.8(5) . . ? N9 C55 H111 117.6 . . ? C54 C55 H111 117.6 . . ? C23 C22 C26 117.4(5) . . ? C23 C22 C18 122.3(5) . . ? C26 C22 C18 120.3(5) . . ? N8 C43 C44 122.2(5) . . ? N8 C43 H113 118.9 . . ? C44 C43 H113 118.9 . . ? N4 C25 C26 126.4(7) . . ? N4 C25 H114 116.8 . . ? C26 C25 H114 116.8 . . ? N3 C12 C13 123.6(5) . . ? N3 C12 H115 118.2 . . ? C13 C12 H115 118.2 . . ? C13 C14 C15 117.2(5) . . ? C13 C14 H116 121.4 . . ? C15 C14 H116 121.4 . . ? N6 C33 C34 121.7(5) . . ? N6 C33 H117 119.2 . . ? C34 C33 H117 119.2 . . ? C45 C44 C43 120.1(5) . . ? C45 C44 H118 119.9 . . ? C43 C44 H118 119.9 . . ? C45 C46 C42 119.5(5) . . ? C45 C46 H119 120.2 . . ? C42 C46 H119 120.2 . . ? C32 C36 C35 120.3(5) . . ? C32 C36 H120 119.8 . . ? C35 C36 H120 119.8 . . ? C2 C3 C4 119.3(5) . . ? C2 C3 H122 120.4 . . ? C4 C3 H122 120.4 . . ? N1 C2 C3 122.1(5) . . ? N1 C2 H123 118.9 . . ? C3 C2 H123 118.9 . . ? C44 C45 C46 118.8(5) . . ? C44 C45 H124 120.6 . . ? C46 C45 H124 120.6 . . ? C5 C4 C3 118.4(6) . . ? C5 C4 H126 120.8 . . ? C3 C4 H126 120.8 . . ? N9 C56 C57 124.2(5) . . ? N9 C56 H128 117.9 . . ? C57 C56 H128 117.9 . . ? C11 C15 C14 120.5(5) . . ? C11 C15 H129 119.8 . . ? C14 C15 H129 119.8 . . ? C34 C35 C36 118.9(5) . . ? C34 C35 H130 120.6 . . ? C36 C35 H130 120.6 . . ? C22 C23 C24 118.6(6) . . ? C22 C23 H131 120.7 . . ? C24 C23 H131 120.7 . . ? C27 C31 C30 120.5(6) . . ? C27 C31 H133 119.8 . . ? C30 C31 H133 119.8 . . ? N5 C29 C28 123.8(6) . . ? N5 C29 H134 118.1 . . ? C28 C29 H134 118.1 . . ? N4 C24 C23 126.8(7) . . ? N4 C24 H138 116.6 . . ? C23 C24 H138 116.6 . . ? C31 C30 N5 122.2(7) . . ? C31 C30 H140 118.9 . . ? N5 C30 H140 118.9 . . ? C29 C28 C27 119.8(6) . . ? C29 C28 H1 120.1 . . ? C27 C28 H1 120.1 . . ? C22 C26 C25 116.9(6) . . ? C22 C26 H2 121.5 . . ? C25 C26 H2 121.5 . . ? C20 C19 C18 121.6(4) . . ? C20 C19 H3 119.2 . . ? C18 C19 H3 119.2 . . ? C56 C57 C53 120.4(5) . . ? C56 C57 H4 119.8 . . ? C53 C57 H4 119.8 . . ? C49 C50 C51 121.4(4) . . ? C49 C50 H5 119.3 . . ? C51 C50 H5 119.3 . . ? C55 N9 C56 115.1(5) . . ? C24 N4 C25 113.6(6) . . ? C29 N5 C30 116.2(6) . . ? C2 N1 C1 117.6(4) . . ? C2 N1 Fe1 127.3(3) . . ? C1 N1 Fe1 115.1(3) . . ? C7 N2 C6 119.9(4) . . ? C7 N2 Fe1 119.9(3) . . ? C6 N2 Fe1 119.8(3) . . ? C12 N3 C11 116.5(4) . . ? C12 N3 Fe1 128.5(3) . . ? C11 N3 Fe1 115.0(3) . . ? C33 N6 C32 117.8(4) . . ? C33 N6 Fe1 127.6(3) . . ? C32 N6 Fe1 114.6(3) . . ? C43 N8 C42 117.1(4) . . ? C43 N8 Fe1 128.3(3) . . ? C42 N8 Fe1 114.4(3) . . ? C38 N7 C37 120.2(4) . . ? C38 N7 Fe1 120.0(3) . . ? C37 N7 Fe1 119.8(3) . . ? C58A C62A C61A 114(3) . . ? C58A C62A H502 123.2 . . ? C61A C62A H502 123.2 . . ? C62A C58A C59A 120.0(17) . . ? C62A C58A C51 118.1(13) . . ? C59A C58A C51 121.9(13) . . ? C60A C59A C58A 119(3) . . ? C60A C59A H506 120.7 . . ? C58A C59A H506 120.7 . . ? C59A C60A N10A 124(3) . . ? C59A C60A H505 118.0 . . ? N10A C60A H505 118.0 . . ? C61A N10A C60A 117.0(19) . . ? N10A C61A C62A 127(3) . . ? N10A C61A H503 116.7 . . ? C62A C61A H503 116.7 . . ? N2 Fe1 N7 177.41(16) . . ? N2 Fe1 N6 101.43(15) . . ? N7 Fe1 N6 80.83(15) . . ? N2 Fe1 N8 96.77(15) . . ? N7 Fe1 N8 81.01(15) . . ? N6 Fe1 N8 161.75(15) . . ? N2 Fe1 N1 80.56(15) . . ? N7 Fe1 N1 100.70(16) . . ? N6 Fe1 N1 91.93(16) . . ? N8 Fe1 N1 89.64(16) . . ? N2 Fe1 N3 80.81(15) . . ? N7 Fe1 N3 97.97(16) . . ? N6 Fe1 N3 90.29(16) . . ? N8 Fe1 N3 94.03(15) . . ? N1 Fe1 N3 161.31(15) . . ? C61B C62B H402 120.5 . . ? C62B C61B H403 119.7 . . ? C59B C60B H405 116.3 . . ? C60B C59B H406 119.9 . . ? F6 P1 F4 92.4(3) . . ? F6 P1 F3 92.5(3) . . ? F4 P1 F3 91.5(3) . . ? F6 P1 F5 89.1(3) . . ? F4 P1 F5 89.6(3) . . ? F3 P1 F5 178.0(3) . . ? F6 P1 F1 177.8(3) . . ? F4 P1 F1 89.5(2) . . ? F3 P1 F1 88.4(2) . . ? F5 P1 F1 90.0(3) . . ? F6 P1 F2 89.8(3) . . ? F4 P1 F2 177.5(3) . . ? F3 P1 F2 89.4(2) . . ? F5 P1 F2 89.4(3) . . ? F1 P1 F2 88.2(3) . . ? O6 N11 C63 120.7(12) . . ? O6 N11 O7 128.2(12) . . ? C63 N11 O7 106.4(12) . . ? N11 C63 H55A 109.5 . . ? N11 C63 H55B 109.5 . . ? H55A C63 H55B 109.5 . . ? N11 C63 H55C 109.5 . . ? H55A C63 H55C 109.5 . . ? H55B C63 H55C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 C11 C7 N2 -174.3(4) . . . . ? N3 C11 C7 N2 4.4(5) . . . . ? C15 C11 C7 C8 7.2(7) . . . . ? N3 C11 C7 C8 -174.1(4) . . . . ? N2 C7 C8 C9 1.5(7) . . . . ? C11 C7 C8 C9 179.9(4) . . . . ? N7 C37 C41 C40 -1.5(7) . . . . ? C32 C37 C41 C40 -178.1(5) . . . . ? C37 C41 C40 C39 -0.8(7) . . . . ? C37 C41 C40 C47 176.3(4) . . . . ? C48 C47 C40 C39 -38.6(7) . . . . ? C52 C47 C40 C39 140.4(5) . . . . ? C48 C47 C40 C41 144.3(5) . . . . ? C52 C47 C40 C41 -36.7(7) . . . . ? C7 C8 C9 C10 -0.3(7) . . . . ? C7 C8 C9 C16 -177.4(4) . . . . ? C52 C47 C48 C49 0.5(7) . . . . ? C40 C47 C48 C49 179.5(4) . . . . ? C47 C48 C49 C50 0.9(7) . . . . ? C47 C48 C49 C53 -178.6(4) . . . . ? C41 C40 C39 C38 2.2(7) . . . . ? C47 C40 C39 C38 -174.9(4) . . . . ? C40 C39 C38 N7 -1.4(7) . . . . ? C40 C39 C38 C42 178.4(4) . . . . ? C50 C51 C52 C47 -0.6(7) . . . . ? C58A C51 C52 C47 179.3(6) . . . . ? C48 C47 C52 C51 -0.6(7) . . . . ? C40 C47 C52 C51 -179.7(4) . . . . ? C50 C49 C53 C54 -152.9(5) . . . . ? C48 C49 C53 C54 26.5(7) . . . . ? C50 C49 C53 C57 26.0(7) . . . . ? C48 C49 C53 C57 -154.5(5) . . . . ? C8 C9 C16 C21 147.5(5) . . . . ? C10 C9 C16 C21 -29.5(7) . . . . ? C8 C9 C16 C17 -27.9(7) . . . . ? C10 C9 C16 C17 155.1(5) . . . . ? C21 C16 C17 C18 -0.8(7) . . . . ? C9 C16 C17 C18 174.7(4) . . . . ? C19 C20 C21 C16 -0.7(7) . . . . ? C27 C20 C21 C16 177.0(5) . . . . ? C17 C16 C21 C20 1.1(7) . . . . ? C9 C16 C21 C20 -174.3(4) . . . . ? N7 C37 C32 C36 177.6(5) . . . . ? C41 C37 C32 C36 -5.6(9) . . . . ? N7 C37 C32 N6 1.6(6) . . . . ? C41 C37 C32 N6 178.4(5) . . . . ? C16 C17 C18 C19 0.1(7) . . . . ? C16 C17 C18 C22 -177.5(4) . . . . ? N2 C6 C1 N1 -4.8(6) . . . . ? C10 C6 C1 N1 174.4(5) . . . . ? N2 C6 C1 C5 178.4(5) . . . . ? C10 C6 C1 C5 -2.4(9) . . . . ? N2 C6 C10 C9 1.4(7) . . . . ? C1 C6 C10 C9 -177.7(5) . . . . ? C8 C9 C10 C6 -1.1(7) . . . . ? C16 C9 C10 C6 176.0(4) . . . . ? N7 C38 C42 N8 5.0(5) . . . . ? C39 C38 C42 N8 -174.8(4) . . . . ? N7 C38 C42 C46 -173.6(4) . . . . ? C39 C38 C42 C46 6.5(8) . . . . ? C19 C20 C27 C31 145.7(5) . . . . ? C21 C20 C27 C31 -32.0(8) . . . . ? C19 C20 C27 C28 -31.1(8) . . . . ? C21 C20 C27 C28 151.2(5) . . . . ? N1 C1 C5 C4 1.4(9) . . . . ? C6 C1 C5 C4 178.0(6) . . . . ? C57 C53 C54 C55 -0.8(7) . . . . ? C49 C53 C54 C55 178.2(5) . . . . ? C53 C54 C55 N9 1.5(9) . . . . ? C17 C18 C22 C23 6.8(8) . . . . ? C19 C18 C22 C23 -170.7(6) . . . . ? C17 C18 C22 C26 -175.9(5) . . . . ? C19 C18 C22 C26 6.6(7) . . . . ? C14 C13 C12 N3 0.4(8) . . . . ? C12 C13 C14 C15 -1.6(8) . . . . ? C35 C34 C33 N6 -0.6(9) . . . . ? N8 C43 C44 C45 -4.0(7) . . . . ? N8 C42 C46 C45 0.2(7) . . . . ? C38 C42 C46 C45 178.8(4) . . . . ? N6 C32 C36 C35 -2.7(9) . . . . ? C37 C32 C36 C35 -178.4(5) . . . . ? C4 C3 C2 N1 -1.6(10) . . . . ? C43 C44 C45 C46 2.6(7) . . . . ? C42 C46 C45 C44 -0.8(7) . . . . ? C1 C5 C4 C3 -3.1(10) . . . . ? C2 C3 C4 C5 3.2(11) . . . . ? N3 C11 C15 C14 -1.9(7) . . . . ? C7 C11 C15 C14 176.7(5) . . . . ? C13 C14 C15 C11 2.3(8) . . . . ? C33 C34 C35 C36 0.0(10) . . . . ? C32 C36 C35 C34 1.6(10) . . . . ? C26 C22 C23 C24 -3.3(11) . . . . ? C18 C22 C23 C24 174.1(7) . . . . ? C28 C27 C31 C30 2.9(9) . . . . ? C20 C27 C31 C30 -174.0(6) . . . . ? C22 C23 C24 N4 4.4(16) . . . . ? C27 C31 C30 N5 -6.4(11) . . . . ? N5 C29 C28 C27 2.1(11) . . . . ? C31 C27 C28 C29 -0.7(9) . . . . ? C20 C27 C28 C29 176.1(6) . . . . ? C23 C22 C26 C25 -1.2(10) . . . . ? C18 C22 C26 C25 -178.7(6) . . . . ? N4 C25 C26 C22 6.1(13) . . . . ? C21 C20 C19 C18 -0.1(7) . . . . ? C27 C20 C19 C18 -177.8(5) . . . . ? C17 C18 C19 C20 0.4(7) . . . . ? C22 C18 C19 C20 177.9(4) . . . . ? N9 C56 C57 C53 -0.4(9) . . . . ? C54 C53 C57 C56 0.3(7) . . . . ? C49 C53 C57 C56 -178.7(5) . . . . ? C48 C49 C50 C51 -2.1(7) . . . . ? C53 C49 C50 C51 177.3(4) . . . . ? C52 C51 C50 C49 2.0(7) . . . . ? C58A C51 C50 C49 -177.9(6) . . . . ? C54 C55 N9 C56 -1.6(9) . . . . ? C57 C56 N9 C55 1.0(9) . . . . ? C23 C24 N4 C25 0.0(15) . . . . ? C26 C25 N4 C24 -5.3(14) . . . . ? C28 C29 N5 C30 -5.3(12) . . . . ? C31 C30 N5 C29 7.4(11) . . . . ? C3 C2 N1 C1 -0.2(8) . . . . ? C3 C2 N1 Fe1 -179.1(4) . . . . ? C5 C1 N1 C2 0.3(7) . . . . ? C6 C1 N1 C2 -176.7(4) . . . . ? C5 C1 N1 Fe1 179.3(4) . . . . ? C6 C1 N1 Fe1 2.3(5) . . . . ? C8 C7 N2 C6 -1.2(7) . . . . ? C11 C7 N2 C6 -179.8(4) . . . . ? C8 C7 N2 Fe1 172.3(3) . . . . ? C11 C7 N2 Fe1 -6.2(5) . . . . ? C10 C6 N2 C7 -0.3(7) . . . . ? C1 C6 N2 C7 179.0(4) . . . . ? C10 C6 N2 Fe1 -173.8(4) . . . . ? C1 C6 N2 Fe1 5.4(5) . . . . ? C13 C12 N3 C11 0.2(7) . . . . ? C13 C12 N3 Fe1 -176.6(4) . . . . ? C15 C11 N3 C12 0.6(6) . . . . ? C7 C11 N3 C12 -178.2(4) . . . . ? C15 C11 N3 Fe1 177.7(4) . . . . ? C7 C11 N3 Fe1 -1.0(4) . . . . ? C34 C33 N6 C32 -0.5(8) . . . . ? C34 C33 N6 Fe1 -177.3(4) . . . . ? C36 C32 N6 C33 2.1(7) . . . . ? C37 C32 N6 C33 178.4(4) . . . . ? C36 C32 N6 Fe1 179.3(4) . . . . ? C37 C32 N6 Fe1 -4.4(5) . . . . ? C44 C43 N8 C42 3.3(7) . . . . ? C44 C43 N8 Fe1 -171.7(3) . . . . ? C46 C42 N8 C43 -1.5(6) . . . . ? C38 C42 N8 C43 179.9(4) . . . . ? C46 C42 N8 Fe1 174.3(3) . . . . ? C38 C42 N8 Fe1 -4.4(5) . . . . ? C39 C38 N7 C37 -0.8(7) . . . . ? C42 C38 N7 C37 179.3(4) . . . . ? C39 C38 N7 Fe1 176.3(3) . . . . ? C42 C38 N7 Fe1 -3.5(5) . . . . ? C41 C37 N7 C38 2.3(7) . . . . ? C32 C37 N7 C38 179.4(4) . . . . ? C41 C37 N7 Fe1 -174.9(4) . . . . ? C32 C37 N7 Fe1 2.2(5) . . . . ? C61A C62A C58A C59A 0(4) . . . . ? C61A C62A C58A C51 177(2) . . . . ? C52 C51 C58A C62A 38.1(18) . . . . ? C50 C51 C58A C62A -142.0(17) . . . . ? C52 C51 C58A C59A -144.4(18) . . . . ? C50 C51 C58A C59A 35(2) . . . . ? C62A C58A C59A C60A -2(4) . . . . ? C51 C58A C59A C60A -179(3) . . . . ? C58A C59A C60A N10A 2(5) . . . . ? C59A C60A N10A C61A 1(5) . . . . ? C60A N10A C61A C62A -4(4) . . . . ? C58A C62A C61A N10A 4(5) . . . . ? C7 N2 Fe1 N6 93.0(3) . . . . ? C6 N2 Fe1 N6 -93.4(4) . . . . ? C7 N2 Fe1 N8 -88.4(3) . . . . ? C6 N2 Fe1 N8 85.1(4) . . . . ? C7 N2 Fe1 N1 -176.9(4) . . . . ? C6 N2 Fe1 N1 -3.4(3) . . . . ? C7 N2 Fe1 N3 4.6(3) . . . . ? C6 N2 Fe1 N3 178.1(4) . . . . ? C38 N7 Fe1 N6 179.2(4) . . . . ? C37 N7 Fe1 N6 -3.6(3) . . . . ? C38 N7 Fe1 N8 1.0(3) . . . . ? C37 N7 Fe1 N8 178.2(4) . . . . ? C38 N7 Fe1 N1 88.9(4) . . . . ? C37 N7 Fe1 N1 -93.9(4) . . . . ? C38 N7 Fe1 N3 -91.8(3) . . . . ? C37 N7 Fe1 N3 85.3(4) . . . . ? _refine_diff_density_max 1.027 _refine_diff_density_min -0.842 _refine_diff_density_rms 0.097 _database_code_depnum_ccdc_archive 'CCDC 948464' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_twin5 _audit_update_record ; 2013-07-03 # Formatted by publCIF ; _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C186 H126 Ru3 N30, (N O3), 5(P F6)' _chemical_formula_sum 'C186 H126 F30 N31 O3 P5 Ru3' _chemical_formula_weight 3871.23 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' F F 0.0171 0.0103 '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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 19.323(5) _cell_length_b 20.548(6) _cell_length_c 26.542(7) _cell_angle_alpha 81.138(5) _cell_angle_beta 81.923(5) _cell_angle_gamma 84.253(5) _cell_volume 10276(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3853 _cell_measurement_theta_min 2.157 _cell_measurement_theta_max 17.600 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_F_000 3920 _exptl_absorpt_coefficient_mu 0.339 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.358723 _exptl_absorpt_correction_T_max 0.428305 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2008)' _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-APEX II' _diffrn_measurement_method \w+\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21222 _diffrn_reflns_av_unetI/netI 0.1063 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.937 _diffrn_reflns_theta_max 20.816 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.576 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.576 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.576 _reflns_number_total 21222 _reflns_number_gt 12407 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_cell_refinement 'SAINT (Bruker-Nonius, 2003)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _refine_special_details ; Refined as a 2-component twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 21222 _refine_ls_number_parameters 1232 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1947 _refine_ls_R_factor_gt 0.1204 _refine_ls_wR_factor_ref 0.3787 _refine_ls_wR_factor_gt 0.3256 _refine_ls_goodness_of_fit_ref 1.289 _refine_ls_restrained_S_all 1.289 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.0205(12) 0.1285(10) 0.0919(8) 0.070(3) Uani 1 1 d . . . . . H1 H -0.0231 0.1113 0.0987 0.084 Uiso 1 1 calc R U . . . C3 C 0.0676(11) 0.1062(11) 0.0571(8) 0.070(3) Uani 1 1 d . . . . . H2 H 0.0592 0.0704 0.0419 0.084 Uiso 1 1 calc R U . . . C4 C 0.1344(12) 0.1375(10) 0.0420(8) 0.070(3) Uani 1 1 d . . . . . H3 H 0.1668 0.1238 0.0156 0.084 Uiso 1 1 calc R U . . . C5 C 0.1478(12) 0.1862(10) 0.0670(8) 0.070(3) Uani 1 1 d . . . . . H4 H 0.1900 0.2057 0.0586 0.084 Uiso 1 1 calc R U . . . C1 C 0.0977(12) 0.2069(11) 0.1052(9) 0.070(3) Uani 1 1 d . . . . . C6 C 0.1059(12) 0.2575(11) 0.1332(9) 0.069(7) Uani 1 1 d . . . . . C10 C 0.1587(10) 0.3024(9) 0.1242(8) 0.056(6) Uani 1 1 d . . . . . H7 H 0.1928 0.3010 0.0959 0.067 Uiso 1 1 calc R U . . . C9 C 0.1604(12) 0.3505(10) 0.1583(11) 0.071(7) Uani 1 1 d . . . . . C8 C 0.1085(10) 0.3524(10) 0.1982(8) 0.051(6) Uani 1 1 d . . . . . H9 H 0.1097 0.3812 0.2218 0.061 Uiso 1 1 calc R U . . . C7 C 0.0523(11) 0.3112(9) 0.2045(8) 0.057(6) Uani 1 1 d . . . . . C11 C -0.0113(9) 0.3125(10) 0.2425(7) 0.042(5) Uani 1 1 d . . . . . C15 C -0.0227(13) 0.3512(10) 0.2829(9) 0.068(6) Uani 1 1 d . . . . . H12 H 0.0097 0.3800 0.2867 0.081 Uiso 1 1 calc R U . . . C14 C -0.0805(13) 0.3449(11) 0.3146(9) 0.073(7) Uani 1 1 d . . . . . H13 H -0.0851 0.3636 0.3448 0.088 Uiso 1 1 calc R U . . . C13 C -0.1360(11) 0.3112(13) 0.3050(9) 0.076(7) Uani 1 1 d . . . . . H14 H -0.1799 0.3134 0.3245 0.092 Uiso 1 1 calc R U . . . C12 C -0.1213(12) 0.2760(13) 0.2663(11) 0.088(8) Uani 1 1 d . . . . . H15 H -0.1548 0.2487 0.2617 0.105 Uiso 1 1 calc R U . . . C33 C -0.0574(11) 0.3394(10) 0.0944(8) 0.067(3) Uani 1 1 d . . . . . H16 H -0.0217 0.3581 0.1058 0.081 Uiso 1 1 calc R U . . . C34 C -0.0912(11) 0.3756(10) 0.0507(8) 0.067(3) Uani 1 1 d . . . . . H17 H -0.0738 0.4141 0.0323 0.081 Uiso 1 1 calc R U . . . C35 C -0.1450(11) 0.3528(10) 0.0385(8) 0.067(3) Uani 1 1 d . . . . . H18 H -0.1687 0.3759 0.0123 0.081 Uiso 1 1 calc R U . . . C36 C -0.1670(11) 0.2954(10) 0.0638(8) 0.067(3) Uani 1 1 d . . . . . H19 H -0.2061 0.2798 0.0543 0.081 Uiso 1 1 calc R U . . . C32 C -0.1340(11) 0.2574(11) 0.1041(8) 0.067(3) Uani 1 1 d . . . . . C37 C -0.1523(11) 0.1953(9) 0.1325(7) 0.053(6) Uani 1 1 d . . . . . C41 C -0.2070(11) 0.1584(11) 0.1247(8) 0.067(7) Uani 1 1 d . . . . . H22 H -0.2359 0.1743 0.0996 0.080 Uiso 1 1 calc R U . . . C40 C -0.2165(11) 0.0974(12) 0.1558(8) 0.066(7) Uani 1 1 d . . . . . C39 C -0.1735(11) 0.0740(11) 0.1969(9) 0.063(6) Uani 1 1 d . . . . . H24 H -0.1786 0.0336 0.2177 0.075 Uiso 1 1 calc R U . . . C38 C -0.1253(9) 0.1154(10) 0.2029(7) 0.048(6) Uani 1 1 d . . . . . C42 C -0.0756(13) 0.1014(12) 0.2390(9) 0.073(7) Uani 1 1 d . . . . . C46 C -0.0818(12) 0.0538(10) 0.2831(11) 0.079(7) Uani 1 1 d . . . . . H27 H -0.1202 0.0284 0.2889 0.095 Uiso 1 1 calc R U . . . C45 C -0.0327(15) 0.0422(13) 0.3191(10) 0.096(9) Uani 1 1 d . . . . . H28 H -0.0376 0.0096 0.3476 0.115 Uiso 1 1 calc R U . . . C44 C 0.0212(16) 0.0808(12) 0.3099(10) 0.094(8) Uani 1 1 d . . . . . H29 H 0.0543 0.0761 0.3327 0.113 Uiso 1 1 calc R U . . . C43 C 0.0273(11) 0.1301(12) 0.2640(9) 0.072(7) Uani 1 1 d . . . . . H30 H 0.0657 0.1554 0.2576 0.086 Uiso 1 1 calc R U . . . C74 C 0.3450(12) 0.8585(11) 0.3754(9) 0.081(3) Uani 1 1 d . . . . . H31 H 0.3771 0.8836 0.3532 0.097 Uiso 1 1 calc R U . . . C75 C 0.3706(12) 0.8162(11) 0.4174(9) 0.081(3) Uani 1 1 d . . . . . H32 H 0.4177 0.8127 0.4221 0.097 Uiso 1 1 calc R U . . . C76 C 0.3218(11) 0.7801(11) 0.4513(9) 0.081(3) Uani 1 1 d . . . . . H33 H 0.3347 0.7539 0.4809 0.097 Uiso 1 1 calc R U . . . C77 C 0.2492(12) 0.7844(12) 0.4392(9) 0.081(3) Uani 1 1 d . . . . . H34 H 0.2169 0.7567 0.4583 0.097 Uiso 1 1 calc R U . . . C73 C 0.2309(12) 0.8280(12) 0.4010(9) 0.081(3) Uani 1 1 d . . . . . C69 C 0.1613(11) 0.8357(10) 0.3828(8) 0.056(6) Uani 1 1 d . . . . . C70 C 0.1030(11) 0.8039(10) 0.4106(7) 0.065(6) Uani 1 1 d . . . . . H37 H 0.1056 0.7749 0.4409 0.078 Uiso 1 1 calc R U . . . C71 C 0.0393(11) 0.8207(9) 0.3876(9) 0.059(6) Uani 1 1 d . . . . . C72 C 0.0375(9) 0.8600(10) 0.3431(8) 0.048(5) Uani 1 1 d . . . . . H39 H -0.0049 0.8704 0.3299 0.057 Uiso 1 1 calc R U . . . C68 C 0.0953(12) 0.8849(10) 0.3170(8) 0.062(7) Uani 1 1 d . . . . . C63 C 0.1023(12) 0.9278(11) 0.2647(8) 0.069(3) Uani 1 1 d . . . . . C67 C 0.0530(12) 0.9431(10) 0.2343(8) 0.069(3) Uani 1 1 d . . . . . H42 H 0.0100 0.9251 0.2444 0.083 Uiso 1 1 calc R U . . . C66 C 0.0613(12) 0.9811(10) 0.1922(8) 0.069(3) Uani 1 1 d . . . . . H43 H 0.0260 0.9889 0.1710 0.083 Uiso 1 1 calc R U . . . C65 C 0.1262(11) 1.0122(10) 0.1772(9) 0.069(3) Uani 1 1 d . . . . . H44 H 0.1334 1.0413 0.1468 0.083 Uiso 1 1 calc R U . . . C64 C 0.1771(12) 0.9971(10) 0.2098(8) 0.069(3) Uani 1 1 d . . . . . H45 H 0.2185 1.0182 0.2013 0.083 Uiso 1 1 calc R U . . . C95 C 0.2671(15) 0.7947(13) 0.2516(11) 0.122(7) Uani 1 1 d . . . . . H46 H 0.2319 0.7773 0.2761 0.146 Uiso 1 1 calc R U . . . C96 C 0.3007(15) 0.7565(13) 0.2130(11) 0.122(7) Uani 1 1 d . . . . . H47 H 0.2854 0.7155 0.2114 0.146 Uiso 1 1 calc R U . . . C97 C 0.3544(16) 0.7796(11) 0.1787(10) 0.121(11) Uani 1 1 d . . . . . H48 H 0.3756 0.7557 0.1528 0.146 Uiso 1 1 calc R U . . . C98 C 0.3778(12) 0.8426(11) 0.1837(9) 0.094(8) Uani 1 1 d . . . . . H49 H 0.4173 0.8585 0.1631 0.113 Uiso 1 1 calc R U . . . C94 C 0.3407(12) 0.8786(10) 0.2193(8) 0.073(6) Uani 1 1 d . . . . . C99 C 0.3590(11) 0.9445(10) 0.2256(9) 0.062(6) Uani 1 1 d . . . . . C103 C 0.4052(11) 0.9801(12) 0.1953(9) 0.075(7) Uani 1 1 d . . . . . H52 H 0.4317 0.9629 0.1676 0.090 Uiso 1 1 calc R U . . . C102 C 0.4150(11) 1.0442(13) 0.2046(9) 0.074(7) Uani 1 1 d . . . . . C101 C 0.3779(10) 1.0686(9) 0.2486(7) 0.048(5) Uani 1 1 d . . . . . H54 H 0.3871 1.1087 0.2574 0.057 Uiso 1 1 calc R U . . . C100 C 0.3265(9) 1.0300(10) 0.2787(7) 0.047(5) Uani 1 1 d . . . . . C104 C 0.2796(11) 1.0474(12) 0.3201(8) 0.069(3) Uani 1 1 d . . . . . C108 C 0.2828(11) 1.1011(11) 0.3439(8) 0.069(3) Uani 1 1 d . . . . . H57 H 0.3167 1.1307 0.3314 0.082 Uiso 1 1 calc R U . . . C107 C 0.2323(11) 1.1124(11) 0.3896(7) 0.069(3) Uani 1 1 d . . . . . H58 H 0.2360 1.1475 0.4070 0.082 Uiso 1 1 calc R U . . . C106 C 0.1843(11) 1.0743(10) 0.4048(8) 0.069(3) Uani 1 1 d . . . . . H59 H 0.1501 1.0832 0.4318 0.082 Uiso 1 1 calc R U . . . C105 C 0.1823(11) 1.0155(11) 0.3798(8) 0.069(3) Uani 1 1 d . . . . . H60 H 0.1470 0.9875 0.3926 0.082 Uiso 1 1 calc R U . . . C152 C 0.7434(15) 0.4345(11) 0.2071(10) 0.084(8) Uani 1 1 d . . . . . H61 H 0.7029 0.4224 0.1970 0.101 Uiso 1 1 calc R U . . . C153 C 0.8082(16) 0.4290(14) 0.1732(12) 0.106(9) Uani 1 1 d . . . . . H62 H 0.8101 0.4127 0.1422 0.127 Uiso 1 1 calc R U . . . C154 C 0.8622(11) 0.4469(12) 0.1871(9) 0.077(7) Uani 1 1 d . . . . . H63 H 0.9044 0.4425 0.1657 0.093 Uiso 1 1 calc R U . . . C155 C 0.8623(11) 0.4725(11) 0.2316(9) 0.069(6) Uani 1 1 d . . . . . H64 H 0.9027 0.4869 0.2401 0.082 Uiso 1 1 calc R U . . . C151 C 0.7969(11) 0.4760(10) 0.2646(8) 0.055(5) Uani 1 1 d . . . . . C156 C 0.7904(10) 0.5005(10) 0.3139(9) 0.058(6) Uani 1 1 d . . . . . C160 C 0.8414(12) 0.5225(10) 0.3388(10) 0.071(7) Uani 1 1 d . . . . . H67 H 0.8875 0.5230 0.3230 0.085 Uiso 1 1 calc R U . . . C159 C 0.8238(12) 0.5433(11) 0.3864(8) 0.062(6) Uani 1 1 d . . . . . C158 C 0.7553(12) 0.5431(10) 0.4050(8) 0.066(6) Uani 1 1 d . . . . . H69 H 0.7418 0.5546 0.4378 0.079 Uiso 1 1 calc R U . . . C157 C 0.7052(10) 0.5276(11) 0.3796(9) 0.065(6) Uani 1 1 d . . . . . C161 C 0.6302(10) 0.5271(9) 0.3955(7) 0.051(5) Uani 1 1 d . . . . . C165 C 0.5942(13) 0.5521(11) 0.4423(9) 0.085(7) Uani 1 1 d . . . . . H72 H 0.6193 0.5669 0.4651 0.101 Uiso 1 1 calc R U . . . C164 C 0.5235(13) 0.5528(14) 0.4509(10) 0.097(8) Uani 1 1 d . . . . . H73 H 0.4995 0.5713 0.4789 0.117 Uiso 1 1 calc R U . . . C163 C 0.4894(12) 0.5291(14) 0.4218(11) 0.093(8) Uani 1 1 d . . . . . H74 H 0.4412 0.5280 0.4309 0.111 Uiso 1 1 calc R U . . . C162 C 0.5185(13) 0.5050(14) 0.3783(10) 0.094(8) Uani 1 1 d . . . . . H75 H 0.4916 0.4881 0.3577 0.113 Uiso 1 1 calc R U . . . C136 C 0.6903(11) 0.3484(10) 0.3744(8) 0.069(3) Uani 1 1 d . . . . . H76 H 0.7215 0.3737 0.3848 0.083 Uiso 1 1 calc R U . . . C139 C 0.5971(11) 0.2732(11) 0.3415(8) 0.069(3) Uani 1 1 d . . . . . H79 H 0.5647 0.2489 0.3312 0.083 Uiso 1 1 calc R U . . . C135 C 0.6070(12) 0.3386(11) 0.3211(8) 0.069(3) Uani 1 1 d . . . . . C131 C 0.5688(10) 0.3731(10) 0.2766(8) 0.057(2) Uani 1 1 d . . . . . C132 C 0.5321(10) 0.3462(10) 0.2466(8) 0.057(2) Uani 1 1 d . . . . . H82 H 0.5235 0.3018 0.2543 0.069 Uiso 1 1 calc R U . . . C133 C 0.5080(10) 0.3833(10) 0.2059(8) 0.057(2) Uani 1 1 d . . . . . C134 C 0.5208(10) 0.4471(9) 0.1938(7) 0.057(2) Uani 1 1 d . . . . . H84 H 0.5050 0.4729 0.1651 0.069 Uiso 1 1 calc R U . . . C130 C 0.5597(10) 0.4743(10) 0.2270(8) 0.057(2) Uani 1 1 d . . . . . N21 N 0.6199(7) 0.5551(6) 0.2556(5) 0.0797(7) Uani 1 1 d G . . . . C125 C 0.5748(7) 0.5441(5) 0.2219(6) 0.0797(7) Uani 1 1 d G . . . . C129 C 0.5498(7) 0.5964(7) 0.1876(5) 0.0797(7) Uani 1 1 d G . . . . H87 H 0.5196 0.5890 0.1650 0.096 Uiso 1 1 calc R U . . . C128 C 0.5700(7) 0.6596(6) 0.1870(5) 0.0797(7) Uani 1 1 d G . . . . H88 H 0.5533 0.6945 0.1640 0.096 Uiso 1 1 calc R U . . . C127 C 0.6151(8) 0.6706(5) 0.2207(6) 0.0797(7) Uani 1 1 d G . . . . H89 H 0.6286 0.7129 0.2203 0.096 Uiso 1 1 calc R U . . . C126 C 0.6400(7) 0.6183(7) 0.2550(5) 0.0797(7) Uani 1 1 d G . . . . H90 H 0.6702 0.6257 0.2775 0.096 Uiso 1 1 calc R U . . . C21 C 0.2347(12) 0.4204(11) 0.0943(9) 0.0797(7) Uani 1 1 d . . . . . H91 H 0.2165 0.4047 0.0683 0.096 Uiso 1 1 calc R U . . . C20 C 0.2843(12) 0.4714(11) 0.0813(9) 0.0797(7) Uani 1 1 d . . . . . C19 C 0.3103(12) 0.4917(11) 0.1218(9) 0.0797(7) Uani 1 1 d . . . . . H93 H 0.3410 0.5249 0.1137 0.096 Uiso 1 1 calc R U . . . C18 C 0.2949(12) 0.4670(11) 0.1736(9) 0.0797(7) Uani 1 1 d . . . . . C17 C 0.2438(11) 0.4178(11) 0.1838(9) 0.0797(7) Uani 1 1 d . . . . . H95 H 0.2296 0.4002 0.2177 0.096 Uiso 1 1 calc R U . . . C16 C 0.2149(12) 0.3957(12) 0.1441(10) 0.0797(7) Uani 1 1 d . . . . . C47 C -0.2666(12) 0.0533(11) 0.1418(10) 0.0797(7) Uani 1 1 d . . . . . C52 C -0.2671(12) 0.0463(11) 0.0902(9) 0.0797(7) Uani 1 1 d . . . . . H98 H -0.2387 0.0707 0.0643 0.096 Uiso 1 1 calc R U . . . C51 C -0.3109(12) 0.0022(11) 0.0780(9) 0.0797(7) Uani 1 1 d . . . . . C50 C -0.3557(12) -0.0272(11) 0.1147(9) 0.0797(7) Uani 1 1 d . . . . . H100 H -0.3876 -0.0530 0.1057 0.096 Uiso 1 1 calc R U . . . C49 C -0.3570(12) -0.0212(11) 0.1659(9) 0.0797(7) Uani 1 1 d . . . . . C48 C -0.3123(11) 0.0202(11) 0.1812(10) 0.0797(7) Uani 1 1 d . . . . . H102 H -0.3130 0.0253 0.2155 0.096 Uiso 1 1 calc R U . . . C78 C -0.0242(12) 0.7909(11) 0.4165(9) 0.0797(7) Uani 1 1 d . . . . . C83 C -0.0351(12) 0.7820(10) 0.4707(9) 0.0797(7) Uani 1 1 d . . . . . H110 H -0.0014 0.7949 0.4881 0.096 Uiso 1 1 calc R U . . . C82 C -0.0949(12) 0.7544(11) 0.4998(9) 0.0797(7) Uani 1 1 d . . . . . C81 C -0.1418(11) 0.7367(10) 0.4742(8) 0.0797(7) Uani 1 1 d . . . . . H112 H -0.1800 0.7163 0.4930 0.096 Uiso 1 1 calc R U . . . C80 C -0.1380(12) 0.7467(11) 0.4200(9) 0.0797(7) Uani 1 1 d . . . . . C79 C -0.0776(11) 0.7721(10) 0.3925(9) 0.0797(7) Uani 1 1 d . . . . . H114 H -0.0724 0.7768 0.3568 0.096 Uiso 1 1 calc R U . . . C110 C 0.5110(11) 1.1251(11) 0.1885(10) 0.0797(7) Uani 1 1 d . . . . . H115 H 0.5072 1.1256 0.2237 0.096 Uiso 1 1 calc R U . . . C111 C 0.5600(12) 1.1603(11) 0.1557(9) 0.0797(7) Uani 1 1 d . . . . . C112 C 0.5648(11) 1.1603(11) 0.1041(6) 0.0797(7) Uani 1 1 d D . . . . H117 H 0.5981 1.1844 0.0823 0.096 Uiso 1 1 calc R U . . . C113 C 0.5186(12) 1.1232(10) 0.0825(5) 0.0797(7) Uani 1 1 d D . . . . C114 C 0.4724(11) 1.0885(10) 0.1139(6) 0.0797(7) Uani 1 1 d D . . . . H119 H 0.4435 1.0639 0.1003 0.096 Uiso 1 1 calc R U . . . C109 C 0.4658(12) 1.0876(11) 0.1678(9) 0.0797(7) Uani 1 1 d . . . . . C140 C 0.4713(12) 0.3557(11) 0.1713(10) 0.0797(7) Uani 1 1 d . . . . . C141 C 0.4194(12) 0.3098(11) 0.1893(10) 0.0797(7) Uani 1 1 d . . . . . H122 H 0.4087 0.2970 0.2245 0.096 Uiso 1 1 calc R U . . . C142 C 0.3841(12) 0.2836(11) 0.1552(9) 0.0797(7) Uani 1 1 d . . . . . C143 C 0.4011(10) 0.3035(10) 0.1019(7) 0.0797(7) Uani 1 1 d D . . . . H124 H 0.3760 0.2885 0.0792 0.096 Uiso 1 1 calc R U . . . C144 C 0.4545(11) 0.3453(11) 0.0822(5) 0.0797(7) Uani 1 1 d D . . . . C145 C 0.4873(12) 0.3712(10) 0.1152(6) 0.0797(7) Uani 1 1 d D . . . . H126 H 0.5215 0.4002 0.1018 0.096 Uiso 1 1 calc R U . . . C166 C 0.8796(12) 0.5616(11) 0.4124(9) 0.0797(7) Uani 1 1 d . . . . . C171 C 0.9384(12) 0.5856(10) 0.3858(9) 0.0797(7) Uani 1 1 d . . . . . H129 H 0.9455 0.5879 0.3502 0.096 Uiso 1 1 calc R U . . . C170 C 0.9909(12) 0.6082(11) 0.4121(9) 0.0797(7) Uani 1 1 d . . . . . C169 C 0.9827(11) 0.6002(10) 0.4605(9) 0.0797(7) Uani 1 1 d . . . . . H131 H 1.0165 0.6145 0.4771 0.096 Uiso 1 1 calc R U . . . C168 C 0.9257(11) 0.5710(10) 0.4909(9) 0.0797(7) Uani 1 1 d . . . . . C167 C 0.8723(12) 0.5526(10) 0.4644(9) 0.0797(7) Uani 1 1 d . . . . . H133 H 0.8327 0.5346 0.4831 0.096 Uiso 1 1 calc R U . . . C22 C 0.3276(7) 0.4844(7) 0.2154(5) 0.0797(7) Uani 1 1 d G . . . . C26 C 0.3377(8) 0.4413(5) 0.2600(6) 0.0797(7) Uani 1 1 d G . . . . H201 H 0.3254 0.3981 0.2637 0.096 Uiso 1 1 calc R U . . . C25 C 0.3664(7) 0.4629(6) 0.2991(4) 0.0797(7) Uani 1 1 d G . . . . H202 H 0.3732 0.4341 0.3290 0.096 Uiso 1 1 calc R U . . . N4 N 0.3849(7) 0.5275(6) 0.2936(4) 0.0797(7) Uani 1 1 d G . . . . C24 C 0.3748(7) 0.5705(5) 0.2489(5) 0.0797(7) Uani 1 1 d G . . . . H203 H 0.3871 0.6138 0.2453 0.096 Uiso 1 1 calc R U . . . C23 C 0.3461(7) 0.5490(6) 0.2098(4) 0.0797(7) Uani 1 1 d G . . . . H204 H 0.3393 0.5778 0.1800 0.096 Uiso 1 1 calc R U . . . C31 C 0.3088(7) 0.5661(7) 0.0179(4) 0.0797(7) Uani 1 1 d G . . . . H205 H 0.3057 0.5896 0.0455 0.096 Uiso 1 1 calc R U . . . C30 C 0.3213(7) 0.5986(5) -0.0321(5) 0.0797(7) Uani 1 1 d G . . . . H206 H 0.3266 0.6437 -0.0379 0.096 Uiso 1 1 calc R U . . . N5 N 0.3259(7) 0.5636(6) -0.0735(4) 0.0797(7) Uani 1 1 d G . . . . C29 C 0.3179(7) 0.4961(6) -0.0648(5) 0.0797(7) Uani 1 1 d G . . . . H207 H 0.3210 0.4727 -0.0925 0.096 Uiso 1 1 calc R U . . . C28 C 0.3054(7) 0.4637(5) -0.0148(6) 0.0797(7) Uani 1 1 d G . . . . H208 H 0.3001 0.4185 -0.0090 0.096 Uiso 1 1 calc R U . . . C27 C 0.3009(7) 0.4987(7) 0.0265(4) 0.0797(7) Uani 1 1 d G . . . . C58 C -0.3034(8) -0.0096(7) 0.0226(4) 0.0797(7) Uani 1 1 d G . . . . C62 C -0.3173(7) -0.0683(6) 0.0075(4) 0.0797(7) Uani 1 1 d G . . . . H211 H -0.3291 -0.1041 0.0322 0.096 Uiso 1 1 calc R U . . . C61 C -0.3134(7) -0.0735(5) -0.0444(5) 0.0797(7) Uani 1 1 d G . . . . H212 H -0.3227 -0.1128 -0.0545 0.096 Uiso 1 1 calc R U . . . N10 N -0.2957(7) -0.0200(6) -0.0812(4) 0.0797(7) Uani 1 1 d G . . . . C60 C -0.2819(7) 0.0388(5) -0.0661(5) 0.0797(7) Uani 1 1 d G . . . . H210 H -0.2701 0.0746 -0.0908 0.096 Uiso 1 1 calc R U . . . C59 C -0.2857(7) 0.0439(6) -0.0142(5) 0.0797(7) Uani 1 1 d G . . . . H209 H -0.2765 0.0832 -0.0041 0.096 Uiso 1 1 calc R U . . . C53 C -0.4068(6) -0.0574(7) 0.2082(5) 0.0797(7) Uani 1 1 d G . . . . C54 C -0.4295(7) -0.1175(7) 0.2022(4) 0.0797(7) Uani 1 1 d G . . . . H213 H -0.4127 -0.1368 0.1729 0.096 Uiso 1 1 calc R U . . . C55 C -0.4772(7) -0.1488(5) 0.2400(5) 0.0797(7) Uani 1 1 d G . . . . H214 H -0.4924 -0.1890 0.2361 0.096 Uiso 1 1 calc R U . . . N9 N -0.5022(6) -0.1200(6) 0.2838(4) 0.0797(7) Uani 1 1 d G . . . . C56 C -0.4795(7) -0.0599(6) 0.2898(4) 0.0797(7) Uani 1 1 d G . . . . H215 H -0.4963 -0.0406 0.3191 0.096 Uiso 1 1 calc R U . . . C57 C -0.4318(7) -0.0285(5) 0.2519(6) 0.0797(7) Uani 1 1 d G . . . . H216 H -0.4166 0.0117 0.2559 0.096 Uiso 1 1 calc R U . . . C84 C -0.1953(6) 0.7301(7) 0.3917(5) 0.0797(7) Uani 1 1 d G . . . . C85 C -0.1795(5) 0.7135(7) 0.3423(5) 0.0797(7) Uani 1 1 d G . . . . H217 H -0.1336 0.7133 0.3261 0.096 Uiso 1 1 calc R U . . . C86 C -0.2324(7) 0.6973(6) 0.3171(4) 0.0797(7) Uani 1 1 d G . . . . H218 H -0.2219 0.6861 0.2841 0.096 Uiso 1 1 calc R U . . . N14 N -0.3011(6) 0.6976(6) 0.3413(5) 0.0797(7) Uani 1 1 d G . . . . C87 C -0.3168(5) 0.7142(6) 0.3907(5) 0.0797(7) Uani 1 1 d G . . . . H220 H -0.3627 0.7145 0.4069 0.096 Uiso 1 1 calc R U . . . C88 C -0.2639(7) 0.7305(7) 0.4159(4) 0.0797(7) Uani 1 1 d G . . . . H221 H -0.2744 0.7416 0.4489 0.096 Uiso 1 1 calc R U . . . C93 C -0.0544(12) 0.7687(10) 0.5815(9) 0.0797(7) Uani 1 1 d . . . . . H222 H -0.0124 0.7827 0.5635 0.096 Uiso 1 1 calc R U . . . C92 C -0.0660(12) 0.7667(10) 0.6334(9) 0.0797(7) Uani 1 1 d . . . . . H223 H -0.0355 0.7855 0.6501 0.096 Uiso 1 1 calc R U . . . C90 C -0.1560(12) 0.7245(10) 0.5892(10) 0.0797(7) Uani 1 1 d . . . . . H224 H -0.1904 0.7071 0.5753 0.096 Uiso 1 1 calc R U . . . C91 C -0.1621(16) 0.7219(17) 0.6369(12) 0.130(12) Uani 1 1 d . . . . . H225 H -0.2030 0.7059 0.6553 0.156 Uiso 1 1 calc R U . . . C116 C 0.6342(12) 1.1756(10) 0.2203(8) 0.077(3) Uani 1 1 d . . . . . H226 H 0.6186 1.1380 0.2412 0.092 Uiso 1 1 calc R U . . . C117 C 0.6831(12) 1.2105(10) 0.2337(8) 0.077(3) Uani 1 1 d . . . . . H227 H 0.7003 1.1933 0.2644 0.092 Uiso 1 1 calc R U . . . C118 C 0.6805(12) 1.2838(11) 0.1666(8) 0.077(3) Uani 1 1 d . . . . . H228 H 0.6938 1.3233 0.1473 0.092 Uiso 1 1 calc R U . . . C119 C 0.6353(11) 1.2548(10) 0.1477(8) 0.077(3) Uani 1 1 d . . . . . H229 H 0.6210 1.2721 0.1160 0.092 Uiso 1 1 calc R U . . . C146 C 0.3270(5) 0.2384(5) 0.1745(5) 0.042(4) Uani 1 1 d G . . . . C147 C 0.2859(7) 0.2434(5) 0.2213(4) 0.043(4) Uani 1 1 d G . . . . H244 H 0.2945 0.2743 0.2414 0.051 Uiso 1 1 calc R U . . . C148 C 0.2320(6) 0.2022(7) 0.2382(4) 0.073(6) Uani 1 1 d G . . . . H242 H 0.2045 0.2055 0.2695 0.088 Uiso 1 1 calc R U . . . N24 N 0.2191(7) 0.1560(6) 0.2082(6) 0.094(6) Uani 1 1 d G . . . . C149 C 0.2602(8) 0.1510(6) 0.1614(6) 0.081(7) Uani 1 1 d G . . . . H245 H 0.2516 0.1201 0.1413 0.098 Uiso 1 1 calc R U . . . C150 C 0.3142(7) 0.1922(6) 0.1445(4) 0.061(5) Uani 1 1 d G . . . . H260 H 0.3417 0.1888 0.1132 0.073 Uiso 1 1 calc R U . . . C172 C 0.9148(11) 0.5701(9) 0.5489(5) 0.124(5) Uani 1 1 d G . . . . C176 C 0.9737(8) 0.5691(9) 0.5737(7) 0.124(5) Uani 1 1 d G . . . . H257 H 1.0173 0.5752 0.5546 0.149 Uiso 1 1 calc R U . . . C175 C 0.9673(8) 0.5588(8) 0.6271(7) 0.124(5) Uani 1 1 d G . . . . H266 H 1.0067 0.5581 0.6437 0.149 Uiso 1 1 calc R U . . . N29 N 0.9021(10) 0.5496(8) 0.6556(5) 0.124(5) Uani 1 1 d G . . . . C174 C 0.8433(8) 0.5506(8) 0.6308(7) 0.124(5) Uani 1 1 d G . . . . H254 H 0.7996 0.5444 0.6499 0.149 Uiso 1 1 calc R U . . . C173 C 0.8496(9) 0.5609(8) 0.5774(7) 0.124(5) Uani 1 1 d G . . . . H255 H 0.8102 0.5616 0.5608 0.149 Uiso 1 1 calc R U . . . C89 C -0.1025(9) 0.7510(9) 0.5564(7) 0.057(5) Uani 1 1 d . . . . . C115 C 0.6092(12) 1.1985(11) 0.1747(8) 0.077(3) Uani 1 1 d . . . . . C10B C 0.5269(17) 1.1070(17) 0.0289(7) 0.094(5) Uani 0.5 1 d DG . P A 1 C14B C 0.5137(17) 1.0484(13) 0.0132(9) 0.094(5) Uani 0.5 1 d G . P A 1 H902 H 0.5085 1.0105 0.0371 0.112 Uiso 0.5 1 calc R U P A 1 C13B C 0.5083(16) 1.0465(13) -0.0382(10) 0.094(5) Uani 0.5 1 d G . P A 1 H901 H 0.4994 1.0074 -0.0487 0.112 Uiso 0.5 1 calc R U P A 1 N20B N 0.5161(16) 1.1032(17) -0.0739(6) 0.094(5) Uani 0.5 1 d G . P A 1 C12B C 0.5293(16) 1.1617(13) -0.0582(10) 0.094(5) Uani 0.5 1 d G . P A 1 H235 H 0.5345 1.1997 -0.0821 0.112 Uiso 0.5 1 calc R U P A 1 C11B C 0.5347(17) 1.1636(13) -0.0068(12) 0.094(5) Uani 0.5 1 d G . P A 1 H237 H 0.5436 1.2028 0.0037 0.112 Uiso 0.5 1 calc R U P A 1 C10A C 0.5138(12) 1.1443(13) 0.0258(4) 0.094(5) Uani 0.5 1 d DG . P A 2 C14A C 0.4539(10) 1.1567(14) 0.0012(7) 0.094(5) Uani 0.5 1 d G . P A 2 H311 H 0.4100 1.1619 0.0203 0.112 Uiso 0.5 1 calc R U P A 2 C13A C 0.4597(13) 1.1614(16) -0.0520(8) 0.094(5) Uani 0.5 1 d G . P A 2 H310 H 0.4196 1.1697 -0.0685 0.112 Uiso 0.5 1 calc R U P A 2 N20A N 0.5252(16) 1.1537(15) -0.0806(5) 0.094(5) Uani 0.5 1 d G . P A 2 C12A C 0.5851(12) 1.1413(15) -0.0559(8) 0.094(5) Uani 0.5 1 d G . P A 2 H312 H 0.6289 1.1361 -0.0750 0.112 Uiso 0.5 1 calc R U P A 2 C11A C 0.5793(10) 1.1366(14) -0.0027(8) 0.094(5) Uani 0.5 1 d G . P A 2 H313 H 0.6194 1.1283 0.0138 0.112 Uiso 0.5 1 calc R U P A 2 C16B C 0.4730(16) 0.3768(17) 0.0280(7) 0.102(5) Uani 0.5 1 d DG . P B 1 C17B C 0.4839(16) 0.3326(12) -0.0076(12) 0.102(5) Uani 0.5 1 d G . P B 1 H261 H 0.4777 0.2881 0.0030 0.122 Uiso 0.5 1 calc R U P B 1 C18B C 0.5041(16) 0.3551(15) -0.0592(10) 0.102(5) Uani 0.5 1 d G . P B 1 H253 H 0.5114 0.3256 -0.0831 0.122 Uiso 0.5 1 calc R U P B 1 N25B N 0.5134(15) 0.4217(17) -0.0752(6) 0.102(5) Uani 0.5 1 d G . P B 1 C19B C 0.5025(16) 0.4658(12) -0.0395(11) 0.102(5) Uani 0.5 1 d G . P B 1 H904 H 0.5088 0.5103 -0.0502 0.122 Uiso 0.5 1 calc R U P B 1 C15B C 0.4823(17) 0.4433(16) 0.0121(9) 0.102(5) Uani 0.5 1 d G . P B 1 H903 H 0.4750 0.4729 0.0359 0.122 Uiso 0.5 1 calc R U P B 1 C16A C 0.4810(12) 0.3508(13) 0.0255(4) 0.102(5) Uani 0.5 1 d DG . P B 2 C15A C 0.5505(10) 0.3444(15) 0.0033(7) 0.102(5) Uani 0.5 1 d G . P B 2 H315 H 0.5861 0.3335 0.0240 0.122 Uiso 0.5 1 calc R U P B 2 C19A C 0.5666(11) 0.3543(16) -0.0499(8) 0.102(5) Uani 0.5 1 d G . P B 2 H316 H 0.6131 0.3500 -0.0647 0.122 Uiso 0.5 1 calc R U P B 2 N25A N 0.5133(16) 0.3706(15) -0.0808(4) 0.102(5) Uani 0.5 1 d G . P B 2 C18A C 0.4439(14) 0.3770(16) -0.0586(8) 0.102(5) Uani 0.5 1 d G . P B 2 H318 H 0.4082 0.3879 -0.0793 0.122 Uiso 0.5 1 calc R U P B 2 C17A C 0.4277(10) 0.3671(15) -0.0054(8) 0.102(5) Uani 0.5 1 d G . P B 2 H319 H 0.3813 0.3713 0.0094 0.122 Uiso 0.5 1 calc R U P B 2 C177 C 1.0537(8) 0.6362(9) 0.3754(7) 0.131(4) Uani 1 1 d G . . . . C181 C 1.1169(10) 0.6315(9) 0.3955(6) 0.131(4) Uani 1 1 d G . . . . H251 H 1.1209 0.6086 0.4281 0.157 Uiso 1 1 calc R U . . . C180 C 1.1742(7) 0.6611(9) 0.3668(7) 0.131(4) Uani 1 1 d G . . . . H250 H 1.2165 0.6580 0.3802 0.157 Uiso 1 1 calc R U . . . N30 N 1.1683(7) 0.6954(8) 0.3180(7) 0.131(4) Uani 1 1 d G . . . . C179 C 1.1050(9) 0.7001(9) 0.2979(6) 0.131(4) Uani 1 1 d G . . . . H252 H 1.1011 0.7230 0.2652 0.157 Uiso 1 1 calc R U . . . C178 C 1.0477(7) 0.6704(10) 0.3265(8) 0.131(4) Uani 1 1 d G . . . . H263 H 1.0054 0.6735 0.3131 0.157 Uiso 1 1 calc R U . . . N1 N 0.0343(9) 0.1781(9) 0.1191(7) 0.070(3) Uani 1 1 d . . . . . N2 N 0.0533(8) 0.2657(8) 0.1719(7) 0.062(5) Uani 1 1 d . . . . . N3 N -0.0628(9) 0.2768(8) 0.2338(6) 0.061(5) Uani 1 1 d . . . . . N6 N -0.0764(9) 0.2811(8) 0.1178(7) 0.067(3) Uani 1 1 d . . . . . N7 N -0.1127(8) 0.1707(8) 0.1721(6) 0.058(5) Uani 1 1 d . . . . . N8 N -0.0210(9) 0.1404(8) 0.2303(7) 0.059(5) Uani 1 1 d . . . . . N16 N 0.2860(8) 0.8545(9) 0.2527(6) 0.064(4) Uani 1 1 d . . . . . N17 N 0.3177(9) 0.9687(9) 0.2648(6) 0.060(4) Uani 1 1 d . . . . . N18 N 0.2276(9) 0.9999(9) 0.3400(6) 0.069(3) Uani 1 1 d . . . . . N11 N 0.1702(9) 0.9543(8) 0.2525(6) 0.069(3) Uani 1 1 d . . . . . N12 N 0.1577(9) 0.8751(9) 0.3401(7) 0.061(5) Uani 1 1 d . . . . . N13 N 0.2793(10) 0.8655(9) 0.3649(7) 0.081(3) Uani 1 1 d . . . . . N22 N 0.5842(8) 0.4369(8) 0.2674(6) 0.057(2) Uani 1 1 d . . . . . N23 N 0.6499(9) 0.3746(8) 0.3374(7) 0.069(3) Uani 1 1 d . . . . . N27 N 0.7227(9) 0.5062(8) 0.3346(7) 0.056(5) Uani 1 1 d . . . . . N26 N 0.7391(9) 0.4558(7) 0.2520(6) 0.053(4) Uani 1 1 d . . . . . N28 N 0.5911(9) 0.5068(7) 0.3658(6) 0.056(4) Uani 1 1 d . . . . . N15 N -0.1218(14) 0.7374(13) 0.6605(7) 0.123(9) Uani 1 1 d . . . . . N19 N 0.7105(9) 1.2663(8) 0.2090(7) 0.077(3) Uani 1 1 d . . . . . P1 P 0.0000 1.0000 0.5000 0.108(4) Uani 1 2 d S . P . . F2 F 0.0201(15) 1.0643(13) 0.4874(13) 0.246(13) Uani 1 1 d . . . . . F1 F 0.0766(10) 0.9817(13) 0.4935(9) 0.224(12) Uani 1 1 d . . . . . F3 F 0.0008(17) 1.003(3) 0.4420(9) 0.37(3) Uani 1 1 d . . . . . N1A N -0.1411(13) 0.3340(11) 0.4576(9) 0.085(7) Uani 1 1 d . . . . . O1A O -0.1786(14) 0.2988(14) 0.4419(10) 0.183(11) Uani 1 1 d . . . . . O2A O -0.1371(16) 0.3872(14) 0.4371(12) 0.216(14) Uani 1 1 d . . . . . O3A O -0.1110(19) 0.3100(19) 0.4875(12) 0.27(2) Uani 1 1 d . . . . . P2A P 0.704(2) 0.6101(19) 0.5187(17) 0.132(12) Uiso 0.25 1 d . . P . . P2B P 0.306(2) 0.245(2) 0.0045(18) 0.141(14) Uiso 0.25 1 d . . P . . P2C P 0.7128(18) 1.2430(17) -0.0202(15) 0.104(10) Uiso 0.25 1 d . . P . . P3 P 0.4536(15) 1.1864(14) 0.3045(9) 0.085(7) Uiso 0.25 1 d . . P . . P3A P 0.736(2) 1.195(2) 0.0028(17) 0.138(13) Uiso 0.25 1 d . . P . . P3B P -0.3525(18) 0.7175(15) 0.6703(12) 0.113(10) Uiso 0.25 1 d . . P . . P3C P 0.4797(16) 1.1405(16) 0.3292(11) 0.096(8) Uiso 0.25 1 d . . P . . P4A P 0.669(2) 0.614(2) 0.5538(17) 0.126(12) Uiso 0.25 1 d . . P . . P4B P 0.679(4) 0.566(4) 0.548(3) 0.14(2) Uiso 0.15 1 d . . P . . P4C P 0.3224(18) 0.5949(15) 0.4888(13) 0.113(10) Uiso 0.25 1 d . . P . . P4D P 0.687(3) 0.656(3) 0.572(2) 0.130(19) Uiso 0.15 1 d . . P . . P5A P 0.279(2) 0.2831(19) -0.0156(17) 0.081(10) Uiso 0.2 1 d . . P . . P5B P 0.701(2) 1.221(2) -0.0576(18) 0.086(13) Uiso 0.15 1 d . . P . . P5C P 1.053(3) 0.509(2) 0.1027(19) 0.105(15) Uiso 0.15 1 d . . P . . P5D P 0.289(4) 0.313(4) -0.054(3) 0.09(2) Uiso 0.1 1 d . . P . . P6A P 1.016(4) 0.536(4) 0.251(3) 0.10(2) Uiso 0.1 1 d . . P . . P6B P 0.364(2) 0.6111(19) 0.5053(16) 0.076(11) Uiso 0.15 1 d . . P . . P6C P -0.242(3) 0.898(2) 0.4649(19) 0.098(14) Uiso 0.15 1 d . . P . . P6D P 0.2764(18) 0.2903(17) 0.0232(14) 0.047(8) Uiso 0.15 1 d . . P . . P7A P -0.066(3) 0.993(3) 0.093(2) 0.083(18) Uiso 0.1 1 d . . P . . P7B P 0.501(3) 1.090(2) 0.3228(17) 0.045(12) Uiso 0.1 1 d . . P . . P7C P -0.123(3) 0.884(3) 0.272(3) 0.086(19) Uiso 0.1 1 d . . P . . P7D P 0.398(4) 0.688(3) 0.338(3) 0.10(2) Uiso 0.1 1 d . . P . . P8A P -0.530(4) -0.306(4) 0.327(3) 0.10(2) Uiso 0.1 1 d . . P . . P8B P 0.697(3) 1.229(3) 0.019(2) 0.045(13) Uiso 0.1 1 d . . P . . P8C P 0.281(3) 0.575(2) 0.4636(18) 0.051(12) Uiso 0.1 1 d . . P . . P8D P -0.171(3) 0.928(3) 0.428(2) 0.080(18) Uiso 0.1 1 d . . P . . P9A P 0.318(5) 0.266(4) -0.043(4) 0.11(3) Uiso 0.1 1 d . . P . . P9B P 0.794(4) 0.149(3) 0.345(3) 0.09(2) Uiso 0.1 1 d . . P . . P9C P 1.100(4) 0.563(4) 0.102(3) 0.11(2) Uiso 0.1 1 d . . P . . Ru1 Ru -0.03090(10) 0.21889(10) 0.17476(5) 0.0569(4) Uani 1 1 d . . . . . Ru2 Ru 0.24038(8) 0.91959(8) 0.30285(7) 0.0574(6) Uani 1 1 d . . . . . Ru3 Ru 0.65095(9) 0.47190(9) 0.30223(7) 0.0599(6) Uani 1 1 d . . . . . C137 C 0.6847(11) 0.2857(10) 0.3956(8) 0.069(3) Uani 1 1 d . . . . . H77 H 0.7105 0.2666 0.4219 0.083 Uiso 1 1 calc R U . . . C138 C 0.6380(11) 0.2489(11) 0.3766(8) 0.069(3) Uani 1 1 d . . . . . H78 H 0.6362 0.2045 0.3901 0.083 Uiso 1 1 calc R U . . . 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 C2 0.072(7) 0.083(7) 0.061(7) -0.016(5) -0.007(5) -0.024(6) C3 0.072(7) 0.083(7) 0.061(7) -0.016(5) -0.007(5) -0.024(6) C4 0.072(7) 0.083(7) 0.061(7) -0.016(5) -0.007(5) -0.024(6) C5 0.072(7) 0.083(7) 0.061(7) -0.016(5) -0.007(5) -0.024(6) C1 0.072(7) 0.083(7) 0.061(7) -0.016(5) -0.007(5) -0.024(6) C6 0.052(16) 0.083(17) 0.074(18) 0.009(14) -0.015(14) -0.044(14) C10 0.035(12) 0.059(14) 0.074(16) 0.002(12) -0.004(11) -0.025(11) C9 0.061(17) 0.048(14) 0.11(2) -0.004(14) -0.026(16) -0.023(12) C8 0.029(12) 0.071(15) 0.053(15) -0.008(11) -0.010(11) -0.003(12) C7 0.077(18) 0.042(13) 0.061(16) -0.001(12) -0.022(14) -0.032(13) C11 0.017(11) 0.073(14) 0.032(12) -0.004(10) 0.008(9) -0.006(10) C15 0.071(18) 0.073(16) 0.063(17) -0.013(13) -0.006(14) -0.023(13) C14 0.071(18) 0.088(17) 0.064(17) -0.030(13) 0.007(14) -0.021(14) C13 0.037(14) 0.13(2) 0.055(15) -0.007(15) 0.023(12) -0.009(14) C12 0.050(17) 0.11(2) 0.09(2) 0.005(17) 0.034(16) -0.026(15) C33 0.061(6) 0.080(7) 0.065(7) -0.001(5) -0.011(5) -0.034(5) C34 0.061(6) 0.080(7) 0.065(7) -0.001(5) -0.011(5) -0.034(5) C35 0.061(6) 0.080(7) 0.065(7) -0.001(5) -0.011(5) -0.034(5) C36 0.061(6) 0.080(7) 0.065(7) -0.001(5) -0.011(5) -0.034(5) C32 0.061(6) 0.080(7) 0.065(7) -0.001(5) -0.011(5) -0.034(5) C37 0.066(15) 0.055(14) 0.039(13) -0.002(11) -0.009(12) -0.017(12) C41 0.071(16) 0.097(18) 0.033(13) 0.004(13) -0.006(12) -0.029(14) C40 0.058(15) 0.113(19) 0.040(14) -0.026(13) 0.008(12) -0.060(14) C39 0.049(14) 0.078(16) 0.071(18) -0.021(12) -0.017(13) -0.024(13) C38 0.030(12) 0.069(15) 0.041(14) -0.001(12) -0.005(11) 0.006(12) C42 0.079(18) 0.083(17) 0.060(17) -0.004(14) 0.005(14) -0.045(15) C46 0.068(17) 0.055(15) 0.12(2) -0.012(15) -0.020(16) 0.001(13) C45 0.11(2) 0.09(2) 0.10(2) -0.016(16) -0.044(19) -0.019(18) C44 0.13(3) 0.070(17) 0.09(2) -0.009(15) -0.022(18) -0.009(17) C43 0.035(13) 0.11(2) 0.074(17) -0.018(15) 0.004(13) -0.011(13) C74 0.065(7) 0.104(8) 0.075(7) -0.007(5) -0.012(5) -0.015(6) C75 0.065(7) 0.104(8) 0.075(7) -0.007(5) -0.012(5) -0.015(6) C76 0.065(7) 0.104(8) 0.075(7) -0.007(5) -0.012(5) -0.015(6) C77 0.065(7) 0.104(8) 0.075(7) -0.007(5) -0.012(5) -0.015(6) C73 0.065(7) 0.104(8) 0.075(7) -0.007(5) -0.012(5) -0.015(6) C69 0.066(16) 0.052(13) 0.050(15) -0.016(11) -0.003(12) 0.005(12) C70 0.067(16) 0.095(16) 0.038(12) -0.011(11) 0.011(12) -0.052(14) C71 0.052(15) 0.054(13) 0.070(17) -0.002(12) 0.010(13) -0.033(11) C72 0.017(11) 0.086(15) 0.044(13) -0.004(12) -0.009(10) -0.019(11) C68 0.069(18) 0.068(15) 0.056(15) -0.021(12) -0.004(13) -0.033(14) C63 0.067(6) 0.079(7) 0.056(6) 0.009(5) -0.006(5) -0.017(5) C67 0.067(6) 0.079(7) 0.056(6) 0.009(5) -0.006(5) -0.017(5) C66 0.067(6) 0.079(7) 0.056(6) 0.009(5) -0.006(5) -0.017(5) C65 0.067(6) 0.079(7) 0.056(6) 0.009(5) -0.006(5) -0.017(5) C64 0.067(6) 0.079(7) 0.056(6) 0.009(5) -0.006(5) -0.017(5) C95 0.123(17) 0.111(16) 0.141(19) -0.060(12) 0.043(13) -0.073(14) C96 0.123(17) 0.111(16) 0.141(19) -0.060(12) 0.043(13) -0.073(14) C97 0.18(3) 0.071(16) 0.12(2) -0.062(15) 0.05(2) -0.052(18) C98 0.073(16) 0.089(17) 0.11(2) -0.044(15) 0.051(15) -0.018(14) C94 0.075(16) 0.086(16) 0.057(13) -0.013(12) 0.012(12) -0.028(13) C99 0.048(13) 0.068(14) 0.074(16) -0.002(12) -0.009(12) -0.032(12) C103 0.053(14) 0.114(19) 0.069(15) -0.039(14) 0.013(11) -0.043(14) C102 0.054(14) 0.116(19) 0.051(14) 0.016(13) 0.000(11) -0.059(13) C101 0.040(11) 0.060(12) 0.043(12) 0.004(10) -0.009(10) -0.017(10) C100 0.041(12) 0.059(13) 0.042(11) -0.013(10) -0.007(9) 0.002(10) C104 0.061(6) 0.093(7) 0.051(6) -0.015(5) 0.003(4) -0.011(5) C108 0.061(6) 0.093(7) 0.051(6) -0.015(5) 0.003(4) -0.011(5) C107 0.061(6) 0.093(7) 0.051(6) -0.015(5) 0.003(4) -0.011(5) C106 0.061(6) 0.093(7) 0.051(6) -0.015(5) 0.003(4) -0.011(5) C105 0.061(6) 0.093(7) 0.051(6) -0.015(5) 0.003(4) -0.011(5) C152 0.11(2) 0.067(15) 0.087(19) 0.015(14) -0.046(17) -0.057(15) C153 0.08(2) 0.13(2) 0.11(2) -0.045(18) 0.003(19) 0.008(18) C154 0.025(13) 0.13(2) 0.078(18) -0.032(15) 0.005(11) -0.016(13) C155 0.038(13) 0.093(16) 0.083(17) -0.021(13) -0.004(12) -0.035(11) C151 0.053(14) 0.065(13) 0.054(13) -0.011(10) -0.019(11) -0.018(11) C156 0.030(13) 0.075(15) 0.077(17) -0.024(13) -0.019(12) -0.005(12) C160 0.059(16) 0.056(14) 0.10(2) 0.007(13) -0.035(15) -0.020(12) C159 0.060(17) 0.084(16) 0.042(14) -0.003(12) 0.000(12) -0.028(13) C158 0.055(16) 0.081(16) 0.062(15) -0.018(12) -0.018(14) 0.024(12) C157 0.033(14) 0.091(17) 0.074(18) -0.011(14) -0.016(13) -0.011(12) C161 0.054(13) 0.063(12) 0.040(12) 0.008(9) -0.032(11) -0.016(10) C165 0.073(19) 0.102(18) 0.089(18) -0.044(14) -0.003(14) -0.021(14) C164 0.047(17) 0.16(2) 0.10(2) -0.053(17) -0.001(15) 0.002(16) C163 0.036(14) 0.16(2) 0.09(2) -0.030(17) 0.006(14) -0.018(15) C162 0.058(17) 0.15(2) 0.083(19) -0.013(17) -0.018(14) -0.039(16) C136 0.076(7) 0.079(7) 0.058(6) -0.002(5) -0.023(5) -0.022(5) C139 0.076(7) 0.079(7) 0.058(6) -0.002(5) -0.023(5) -0.022(5) C135 0.076(7) 0.079(7) 0.058(6) -0.002(5) -0.023(5) -0.022(5) C131 0.056(6) 0.068(6) 0.051(6) 0.009(4) -0.020(4) -0.026(5) C132 0.056(6) 0.068(6) 0.051(6) 0.009(4) -0.020(4) -0.026(5) C133 0.056(6) 0.068(6) 0.051(6) 0.009(4) -0.020(4) -0.026(5) C134 0.056(6) 0.068(6) 0.051(6) 0.009(4) -0.020(4) -0.026(5) C130 0.056(6) 0.068(6) 0.051(6) 0.009(4) -0.020(4) -0.026(5) N21 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C125 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C129 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C128 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C127 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C126 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C21 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C20 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C19 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C18 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C17 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C16 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C47 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C52 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C51 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C50 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C49 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C48 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C78 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C83 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C82 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C81 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C80 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C79 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C110 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C111 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C112 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C113 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C114 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C109 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C140 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C141 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C142 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C143 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C144 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C145 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C166 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C171 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C170 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C169 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C168 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C167 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C22 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C26 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C25 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) N4 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C24 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C23 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C31 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C30 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) N5 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C29 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C28 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C27 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C58 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C62 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C61 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) N10 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C60 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C59 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C53 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C54 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C55 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) N9 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C56 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C57 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C84 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C85 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C86 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) N14 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C87 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C88 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C93 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C92 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C90 0.0724(16) 0.0899(16) 0.0799(16) -0.0036(18) -0.0142(18) -0.0282(13) C91 0.11(2) 0.21(3) 0.08(2) 0.00(2) -0.042(18) -0.02(2) C116 0.087(8) 0.085(7) 0.060(7) -0.006(6) 0.005(5) -0.040(5) C117 0.087(8) 0.085(7) 0.060(7) -0.006(6) 0.005(5) -0.040(5) C118 0.087(8) 0.085(7) 0.060(7) -0.006(6) 0.005(5) -0.040(5) C119 0.087(8) 0.085(7) 0.060(7) -0.006(6) 0.005(5) -0.040(5) C146 0.036(10) 0.044(11) 0.051(12) -0.009(9) -0.022(9) 0.004(9) C147 0.058(12) 0.041(10) 0.031(10) -0.015(8) 0.005(9) -0.011(9) C148 0.091(17) 0.093(16) 0.037(12) -0.007(12) 0.004(11) -0.036(14) N24 0.096(16) 0.112(16) 0.081(15) 0.003(12) -0.021(13) -0.056(13) C149 0.13(2) 0.040(12) 0.094(19) -0.024(12) -0.033(16) -0.027(13) C150 0.066(14) 0.058(13) 0.062(13) -0.005(11) -0.021(11) -0.006(11) C172 0.141(11) 0.134(8) 0.122(10) -0.064(8) -0.068(9) 0.014(9) C176 0.141(11) 0.134(8) 0.122(10) -0.064(8) -0.068(9) 0.014(9) C175 0.141(11) 0.134(8) 0.122(10) -0.064(8) -0.068(9) 0.014(9) N29 0.141(11) 0.134(8) 0.122(10) -0.064(8) -0.068(9) 0.014(9) C174 0.141(11) 0.134(8) 0.122(10) -0.064(8) -0.068(9) 0.014(9) C173 0.141(11) 0.134(8) 0.122(10) -0.064(8) -0.068(9) 0.014(9) C89 0.043(12) 0.071(13) 0.046(11) -0.004(10) 0.019(9) 0.005(10) C115 0.087(8) 0.085(7) 0.060(7) -0.006(6) 0.005(5) -0.040(5) C10B 0.088(10) 0.141(13) 0.054(9) -0.012(10) -0.003(8) -0.028(12) C14B 0.088(10) 0.141(13) 0.054(9) -0.012(10) -0.003(8) -0.028(12) C13B 0.088(10) 0.141(13) 0.054(9) -0.012(10) -0.003(8) -0.028(12) N20B 0.088(10) 0.141(13) 0.054(9) -0.012(10) -0.003(8) -0.028(12) C12B 0.088(10) 0.141(13) 0.054(9) -0.012(10) -0.003(8) -0.028(12) C11B 0.088(10) 0.141(13) 0.054(9) -0.012(10) -0.003(8) -0.028(12) C10A 0.088(10) 0.141(13) 0.054(9) -0.012(10) -0.003(8) -0.028(12) C14A 0.088(10) 0.141(13) 0.054(9) -0.012(10) -0.003(8) -0.028(12) C13A 0.088(10) 0.141(13) 0.054(9) -0.012(10) -0.003(8) -0.028(12) N20A 0.088(10) 0.141(13) 0.054(9) -0.012(10) -0.003(8) -0.028(12) C12A 0.088(10) 0.141(13) 0.054(9) -0.012(10) -0.003(8) -0.028(12) C11A 0.088(10) 0.141(13) 0.054(9) -0.012(10) -0.003(8) -0.028(12) C16B 0.092(10) 0.143(13) 0.062(10) 0.029(9) -0.017(9) -0.021(12) C17B 0.092(10) 0.143(13) 0.062(10) 0.029(9) -0.017(9) -0.021(12) C18B 0.092(10) 0.143(13) 0.062(10) 0.029(9) -0.017(9) -0.021(12) N25B 0.092(10) 0.143(13) 0.062(10) 0.029(9) -0.017(9) -0.021(12) C19B 0.092(10) 0.143(13) 0.062(10) 0.029(9) -0.017(9) -0.021(12) C15B 0.092(10) 0.143(13) 0.062(10) 0.029(9) -0.017(9) -0.021(12) C16A 0.092(10) 0.143(13) 0.062(10) 0.029(9) -0.017(9) -0.021(12) C15A 0.092(10) 0.143(13) 0.062(10) 0.029(9) -0.017(9) -0.021(12) C19A 0.092(10) 0.143(13) 0.062(10) 0.029(9) -0.017(9) -0.021(12) N25A 0.092(10) 0.143(13) 0.062(10) 0.029(9) -0.017(9) -0.021(12) C18A 0.092(10) 0.143(13) 0.062(10) 0.029(9) -0.017(9) -0.021(12) C17A 0.092(10) 0.143(13) 0.062(10) 0.029(9) -0.017(9) -0.021(12) C177 0.095(8) 0.140(10) 0.164(13) -0.005(8) -0.025(8) -0.049(8) C181 0.095(8) 0.140(10) 0.164(13) -0.005(8) -0.025(8) -0.049(8) C180 0.095(8) 0.140(10) 0.164(13) -0.005(8) -0.025(8) -0.049(8) N30 0.095(8) 0.140(10) 0.164(13) -0.005(8) -0.025(8) -0.049(8) C179 0.095(8) 0.140(10) 0.164(13) -0.005(8) -0.025(8) -0.049(8) C178 0.095(8) 0.140(10) 0.164(13) -0.005(8) -0.025(8) -0.049(8) N1 0.072(7) 0.083(7) 0.061(7) -0.016(5) -0.007(5) -0.024(6) N2 0.043(12) 0.065(12) 0.069(13) 0.022(11) 0.000(11) -0.028(10) N3 0.044(12) 0.089(13) 0.057(13) -0.009(10) -0.017(10) -0.025(10) N6 0.061(6) 0.080(7) 0.065(7) -0.001(5) -0.011(5) -0.034(5) N7 0.043(11) 0.079(13) 0.050(12) 0.019(10) -0.011(9) -0.031(9) N8 0.054(11) 0.068(12) 0.066(13) -0.021(9) -0.017(10) -0.029(10) N16 0.046(10) 0.096(13) 0.052(10) -0.020(9) 0.006(8) -0.015(9) N17 0.058(11) 0.088(13) 0.037(10) -0.008(9) 0.000(9) -0.028(10) N18 0.061(6) 0.093(7) 0.051(6) -0.015(5) 0.003(4) -0.011(5) N11 0.067(6) 0.079(7) 0.056(6) 0.009(5) -0.006(5) -0.017(5) N12 0.043(12) 0.094(14) 0.040(12) -0.009(11) 0.009(9) -0.005(10) N13 0.065(7) 0.104(8) 0.075(7) -0.007(5) -0.012(5) -0.015(6) N22 0.056(6) 0.068(6) 0.051(6) 0.009(4) -0.020(4) -0.026(5) N23 0.076(7) 0.079(7) 0.058(6) -0.002(5) -0.023(5) -0.022(5) N27 0.060(14) 0.068(12) 0.045(12) -0.010(9) -0.014(10) -0.021(10) N26 0.073(12) 0.051(10) 0.048(11) -0.016(8) -0.027(9) -0.023(9) N28 0.053(12) 0.046(9) 0.071(12) -0.012(8) -0.009(9) -0.003(8) N15 0.14(2) 0.17(2) 0.041(13) 0.037(14) 0.006(14) 0.006(18) N19 0.087(8) 0.085(7) 0.060(7) -0.006(6) 0.005(5) -0.040(5) P1 0.091(9) 0.118(10) 0.108(10) 0.007(7) 0.006(7) -0.036(7) F2 0.26(3) 0.19(2) 0.29(4) -0.03(2) -0.01(3) -0.11(2) F1 0.103(16) 0.28(3) 0.22(2) 0.092(19) 0.045(15) 0.031(16) F3 0.24(3) 0.79(9) 0.085(17) 0.02(3) -0.006(18) -0.17(4) N1A 0.13(2) 0.062(14) 0.063(14) 0.007(11) -0.012(13) -0.039(14) O1A 0.18(3) 0.20(2) 0.19(3) -0.03(2) -0.05(2) -0.07(2) O2A 0.23(3) 0.13(2) 0.26(3) 0.01(2) 0.01(2) 0.03(2) O3A 0.30(4) 0.34(4) 0.18(3) 0.13(3) -0.16(3) -0.13(3) Ru1 0.0460(9) 0.0763(10) 0.0537(8) -0.0086(12) -0.0080(12) -0.0287(7) Ru2 0.0453(11) 0.0744(13) 0.0534(12) -0.0071(10) 0.0017(9) -0.0234(9) Ru3 0.0490(11) 0.0752(13) 0.0609(13) -0.0023(10) -0.0199(10) -0.0236(10) C137 0.076(7) 0.079(7) 0.058(6) -0.002(5) -0.023(5) -0.022(5) C138 0.076(7) 0.079(7) 0.058(6) -0.002(5) -0.023(5) -0.022(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 C3 1.30(3) . ? C2 N1 1.40(2) . ? C2 H1 0.9300 . ? C3 C4 1.48(3) . ? C3 H2 0.9300 . ? C4 C5 1.35(3) . ? C4 H3 0.9300 . ? C5 C1 1.39(3) . ? C5 H4 0.9300 . ? C1 C6 1.40(3) . ? C1 N1 1.39(3) . ? C6 N2 1.36(3) . ? C6 C10 1.41(2) . ? C10 C9 1.44(3) . ? C10 H7 0.9300 . ? C9 C8 1.35(3) . ? C9 C16 1.45(3) . ? C8 C7 1.42(2) . ? C8 H9 0.9300 . ? C7 N2 1.37(2) . ? C7 C11 1.48(3) . ? C11 N3 1.36(2) . ? C11 C15 1.41(3) . ? C15 C14 1.30(3) . ? C15 H12 0.9300 . ? C14 C13 1.40(3) . ? C14 H13 0.9300 . ? C13 C12 1.33(3) . ? C13 H14 0.9300 . ? C12 N3 1.32(3) . ? C12 H15 0.9300 . ? C33 N6 1.32(2) . ? C33 C34 1.47(3) . ? C33 H16 0.9300 . ? C34 C35 1.28(2) . ? C34 H17 0.9300 . ? C35 C36 1.34(2) . ? C35 H18 0.9300 . ? C36 C32 1.41(3) . ? C36 H19 0.9300 . ? C32 N6 1.37(2) . ? C32 C37 1.43(3) . ? C37 N7 1.39(2) . ? C37 C41 1.42(3) . ? C41 C40 1.40(3) . ? C41 H22 0.9300 . ? C40 C39 1.46(3) . ? C40 C47 1.51(3) . ? C39 C38 1.36(2) . ? C39 H24 0.9300 . ? C38 N7 1.32(2) . ? C38 C42 1.43(3) . ? C42 N8 1.36(2) . ? C42 C46 1.40(3) . ? C46 C45 1.42(3) . ? C46 H27 0.9300 . ? C45 C44 1.35(3) . ? C45 H28 0.9300 . ? C44 C43 1.46(3) . ? C44 H29 0.9300 . ? C43 N8 1.36(2) . ? C43 H30 0.9300 . ? C74 N13 1.33(2) . ? C74 C75 1.42(3) . ? C74 H31 0.9300 . ? C75 C76 1.40(3) . ? C75 H32 0.9300 . ? C76 C77 1.47(3) . ? C76 H33 0.9300 . ? C77 C73 1.31(3) . ? C77 H34 0.9300 . ? C73 N13 1.43(3) . ? C73 C69 1.48(3) . ? C69 N12 1.29(2) . ? C69 C70 1.42(3) . ? C70 C71 1.44(3) . ? C70 H37 0.9300 . ? C71 C72 1.33(3) . ? C71 C78 1.49(3) . ? C72 C68 1.33(3) . ? C72 H39 0.9300 . ? C68 N12 1.41(2) . ? C68 C63 1.52(3) . ? C63 C67 1.32(3) . ? C63 N11 1.45(3) . ? C67 C66 1.26(2) . ? C67 H42 0.9300 . ? C66 C65 1.44(3) . ? C66 H43 0.9300 . ? C65 C64 1.38(3) . ? C65 H44 0.9300 . ? C64 N11 1.32(2) . ? C64 H45 0.9300 . ? C95 N16 1.32(2) . ? C95 C96 1.43(3) . ? C95 H46 0.9300 . ? C96 C97 1.35(3) . ? C96 H47 0.9300 . ? C97 C98 1.44(3) . ? C97 H48 0.9300 . ? C98 C94 1.37(3) . ? C98 H49 0.9300 . ? C94 N16 1.36(2) . ? C94 C99 1.47(3) . ? C99 C103 1.31(3) . ? C99 N17 1.34(3) . ? C103 C102 1.41(3) . ? C103 H52 0.9300 . ? C102 C101 1.42(3) . ? C102 C109 1.53(3) . ? C101 C100 1.41(2) . ? C101 H54 0.9300 . ? C100 N17 1.40(2) . ? C100 C104 1.39(3) . ? C104 C108 1.36(3) . ? C104 N18 1.46(2) . ? C108 C107 1.48(3) . ? C108 H57 0.9300 . ? C107 C106 1.26(3) . ? C107 H58 0.9300 . ? C106 C105 1.47(3) . ? C106 H59 0.9300 . ? C105 N18 1.33(2) . ? C105 H60 0.9300 . ? C152 N26 1.32(3) . ? C152 C153 1.44(3) . ? C152 H61 0.9300 . ? C153 C154 1.26(3) . ? C153 H62 0.9300 . ? C154 C155 1.37(3) . ? C154 H63 0.9300 . ? C155 C151 1.43(3) . ? C155 H64 0.9300 . ? C151 N26 1.33(2) . ? C151 C156 1.46(3) . ? C156 N27 1.35(2) . ? C156 C160 1.40(3) . ? C160 C159 1.38(3) . ? C160 H67 0.9300 . ? C159 C158 1.35(3) . ? C159 C166 1.46(3) . ? C158 C157 1.35(3) . ? C158 H69 0.9300 . ? C157 N27 1.32(3) . ? C157 C161 1.45(3) . ? C161 N28 1.30(2) . ? C161 C165 1.47(3) . ? C165 C164 1.35(3) . ? C165 H72 0.9300 . ? C164 C163 1.26(3) . ? C164 H73 0.9300 . ? C163 C162 1.35(3) . ? C163 H74 0.9300 . ? C162 N28 1.40(3) . ? C162 H75 0.9300 . ? C136 C137 1.33(2) . ? C136 N23 1.35(2) . ? C136 H76 0.9300 . ? C139 C138 1.31(3) . ? C139 C135 1.39(3) . ? C139 H79 0.9300 . ? C135 N23 1.32(2) . ? C135 C131 1.52(3) . ? C131 C132 1.35(2) . ? C131 N22 1.35(2) . ? C132 C133 1.33(2) . ? C132 H82 0.9300 . ? C133 C134 1.34(2) . ? C133 C140 1.45(3) . ? C134 C130 1.44(2) . ? C134 H84 0.9300 . ? C130 N22 1.33(2) . ? C130 C125 1.47(2) . ? N21 C125 1.3900 . ? N21 C126 1.3900 . ? N21 Ru3 2.042(10) . ? C125 C129 1.3900 . ? C129 C128 1.3900 . ? C129 H87 0.9300 . ? C128 C127 1.3900 . ? C128 H88 0.9300 . ? C127 C126 1.3900 . ? C127 H89 0.9300 . ? C126 H90 0.9300 . ? C21 C16 1.36(3) . ? C21 C20 1.46(3) . ? C21 H91 0.9300 . ? C20 C19 1.38(3) . ? C20 C27 1.48(2) . ? C19 C18 1.39(3) . ? C19 H93 0.9300 . ? C18 C22 1.46(2) . ? C18 C17 1.45(3) . ? C17 C16 1.41(3) . ? C17 H95 0.9300 . ? C47 C52 1.40(3) . ? C47 C48 1.41(3) . ? C52 C51 1.40(3) . ? C52 H98 0.9300 . ? C51 C50 1.32(3) . ? C51 C58 1.51(3) . ? C50 C49 1.38(3) . ? C50 H100 0.9300 . ? C49 C48 1.41(3) . ? C49 C53 1.52(2) . ? C48 H102 0.9300 . ? C78 C83 1.41(3) . ? C78 C79 1.40(3) . ? C83 C82 1.41(3) . ? C83 H110 0.9300 . ? C82 C81 1.32(3) . ? C82 C89 1.48(3) . ? C81 C80 1.41(3) . ? C81 H112 0.9300 . ? C80 C79 1.39(3) . ? C80 C84 1.52(2) . ? C79 H114 0.9300 . ? C110 C111 1.37(3) . ? C110 C109 1.43(3) . ? C110 H115 0.9300 . ? C111 C112 1.36(3) . ? C111 C115 1.48(3) . ? C112 C113 1.46(2) . ? C112 H117 0.9300 . ? C113 C114 1.32(2) . ? C113 C10B 1.495(10) . ? C113 C10A 1.514(9) . ? C114 C109 1.42(3) . ? C114 H119 0.9300 . ? C140 C141 1.43(3) . ? C140 C145 1.47(3) . ? C141 C142 1.40(3) . ? C141 H122 0.9300 . ? C142 C143 1.41(3) . ? C142 C146 1.50(2) . ? C143 C144 1.40(2) . ? C143 H124 0.9300 . ? C144 C145 1.35(2) . ? C144 C16B 1.492(9) . ? C144 C16A 1.509(9) . ? C145 H126 0.9300 . ? C166 C171 1.35(3) . ? C166 C167 1.35(3) . ? C171 C170 1.46(3) . ? C171 H129 0.9300 . ? C170 C169 1.26(3) . ? C170 C177 1.54(2) . ? C169 C168 1.40(3) . ? C169 H131 0.9300 . ? C168 C167 1.44(3) . ? C168 C172 1.52(2) . ? C167 H133 0.9300 . ? C22 C26 1.3900 . ? C22 C23 1.3900 . ? C26 C25 1.3900 . ? C26 H201 0.9300 . ? C25 N4 1.3900 . ? C25 H202 0.9300 . ? N4 C24 1.3900 . ? C24 C23 1.3900 . ? C24 H203 0.9300 . ? C23 H204 0.9300 . ? C31 C30 1.3900 . ? C31 C27 1.3900 . ? C31 H205 0.9300 . ? C30 N5 1.3900 . ? C30 H206 0.9300 . ? N5 C29 1.3900 . ? C29 C28 1.3900 . ? C29 H207 0.9300 . ? C28 C27 1.3900 . ? C28 H208 0.9300 . ? C58 C62 1.3900 . ? C58 C59 1.3900 . ? C62 C61 1.3900 . ? C62 H211 0.9300 . ? C61 N10 1.3900 . ? C61 H212 0.9300 . ? N10 C60 1.3900 . ? C60 C59 1.3900 . ? C60 H210 0.9300 . ? C59 H209 0.9300 . ? C53 C54 1.3900 . ? C53 C57 1.3900 . ? C54 C55 1.3900 . ? C54 H213 0.9300 . ? C55 N9 1.3900 . ? C55 H214 0.9300 . ? N9 C56 1.3900 . ? C56 C57 1.3900 . ? C56 H215 0.9300 . ? C57 H216 0.9300 . ? C84 C85 1.3900 . ? C84 C88 1.3900 . ? C85 C86 1.3900 . ? C85 H217 0.9300 . ? C86 N14 1.3900 . ? C86 H218 0.9300 . ? N14 C87 1.3900 . ? C87 C88 1.3900 . ? C87 H220 0.9300 . ? C88 H221 0.9300 . ? C93 C89 1.33(2) . ? C93 C92 1.36(3) . ? C93 H222 0.9300 . ? C92 N15 1.35(3) . ? C92 H223 0.9300 . ? C90 C91 1.25(3) . ? C90 C89 1.35(3) . ? C90 H224 0.9300 . ? C91 N15 1.16(3) . ? C91 H225 0.9300 . ? C116 C117 1.36(3) . ? C116 C115 1.36(3) . ? C116 H226 0.9300 . ? C117 N19 1.35(2) . ? C117 H227 0.9300 . ? C118 C119 1.30(3) . ? C118 N19 1.32(2) . ? C118 H228 0.9300 . ? C119 C115 1.37(2) . ? C119 H229 0.9300 . ? C146 C147 1.3900 . ? C146 C150 1.3900 . ? C147 C148 1.3900 . ? C147 H244 0.9300 . ? C148 N24 1.3900 . ? C148 H242 0.9300 . ? N24 C149 1.3900 . ? C149 C150 1.3900 . ? C149 H245 0.9300 . ? C150 H260 0.9300 . ? C172 C176 1.3900 . ? C172 C173 1.3900 . ? C176 C175 1.3900 . ? C176 H257 0.9300 . ? C175 N29 1.3900 . ? C175 H266 0.9300 . ? N29 C174 1.3900 . ? C174 C173 1.3900 . ? C174 H254 0.9300 . ? C173 H255 0.9300 . ? C10B C14B 1.3900 . ? C10B C11B 1.3900 . ? C14B C13B 1.3900 . ? C14B C13B 2.03(5) 2_675 ? C14B H902 0.9300 . ? C13B N20B 1.3900 . ? C13B C14B 2.03(5) 2_675 ? C13B H901 0.9300 . ? N20B C12B 1.3900 . ? C12B C11B 1.3900 . ? C12B H235 0.9300 . ? C11B H237 0.9300 . ? C10A C14A 1.3900 . ? C10A C11A 1.3900 . ? C14A C13A 1.3900 . ? C14A H311 0.9300 . ? C13A N20A 1.3900 . ? C13A H310 0.9300 . ? N20A C12A 1.3900 . ? C12A C11A 1.3900 . ? C12A H312 0.9300 . ? C11A H313 0.9300 . ? C16B C17B 1.3900 . ? C16B C15B 1.3900 . ? C17B C18B 1.3900 . ? C17B H261 0.9300 . ? C18B N25B 1.3900 . ? C18B H253 0.9300 . ? N25B C19B 1.3900 . ? C19B C15B 1.3900 . ? C19B H904 0.9300 . ? C15B H903 0.9300 . ? C16A C15A 1.3900 . ? C16A C17A 1.3900 . ? C15A C19A 1.3900 . ? C15A H315 0.9300 . ? C19A N25A 1.3900 . ? C19A H316 0.9300 . ? N25A C18A 1.3900 . ? C18A C17A 1.3900 . ? C18A H318 0.9300 . ? C17A H319 0.9300 . ? C177 C181 1.3900 . ? C177 C178 1.3900 . ? C181 C180 1.3900 . ? C181 H251 0.9300 . ? C180 N30 1.3900 . ? C180 H250 0.9300 . ? N30 C179 1.3900 . ? C179 C178 1.3900 . ? C179 H252 0.9300 . ? C178 H263 0.9300 . ? N1 Ru1 2.029(18) . ? N2 Ru1 1.958(15) . ? N3 Ru1 2.099(18) . ? N6 Ru1 2.061(17) . ? N7 Ru1 1.962(14) . ? N8 Ru1 2.023(17) . ? N16 Ru2 2.078(16) . ? N17 Ru2 1.959(16) . ? N18 Ru2 2.025(17) . ? N11 Ru2 2.037(17) . ? N12 Ru2 1.984(17) . ? N13 Ru2 2.032(18) . ? N22 Ru3 1.940(14) . ? N23 Ru3 2.072(16) . ? N27 Ru3 1.968(16) . ? N26 Ru3 2.043(17) . ? N28 Ru3 2.087(17) . ? P1 F2 1.39(2) 2_576 ? P1 F2 1.39(2) . ? P1 F1 1.48(2) 2_576 ? P1 F1 1.48(2) . ? P1 F3 1.53(2) . ? P1 F3 1.53(2) 2_576 ? N1A O3A 1.08(3) . ? N1A O2A 1.15(3) . ? N1A O1A 1.23(3) . ? P2A P4A 1.08(5) . ? P2A P4B 1.19(7) . ? P2A P4D 1.79(8) . ? P2B P5A 1.02(5) . ? P2B P6D 1.18(5) . ? P2B P9A 1.26(9) . ? P2B P5D 1.96(8) . ? P2C P8B 1.06(5) . ? P2C P3A 1.16(4) . ? P2C P5B 1.21(5) . ? P3 P3C 1.18(3) . ? P3 P7B 2.11(5) . ? P3A P8B 1.06(6) . ? P3A P5B 1.81(6) . ? P3C P7B 1.10(5) . ? P4A P4B 1.02(7) . ? P4A P4D 1.14(6) . ? P4B P4D 2.06(10) . ? P4C P6B 1.07(4) . ? P4C P8C 1.25(5) . ? P5A P6D 1.06(4) . ? P5A P9A 1.03(9) . ? P5A P5D 1.11(7) . ? P5B P8B 2.06(7) . ? P5C P9C 1.51(9) . ? P5D P9A 1.08(9) . ? P5D P6D 2.02(8) . ? P6B P8C 2.32(6) . ? P6C P8D 1.68(8) . ? P6D P9A 1.93(10) . ? P7D P8A 1.38(9) 1_665 ? P8A P7D 1.38(9) 1_445 ? C137 C138 1.42(2) . ? C137 H77 0.9300 . ? C138 H78 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 C3 C2 N1 121(2) . . ? C3 C2 H1 119.4 . . ? N1 C2 H1 119.4 . . ? C2 C3 C4 120(2) . . ? C2 C3 H2 120.0 . . ? C4 C3 H2 120.0 . . ? C5 C4 C3 119(2) . . ? C5 C4 H3 120.4 . . ? C3 C4 H3 120.4 . . ? C4 C5 C1 119(2) . . ? C4 C5 H4 120.4 . . ? C1 C5 H4 120.4 . . ? C5 C1 C6 124(2) . . ? C5 C1 N1 122(2) . . ? C6 C1 N1 114(2) . . ? N2 C6 C1 114.0(19) . . ? N2 C6 C10 117(2) . . ? C1 C6 C10 129(2) . . ? C6 C10 C9 121(2) . . ? C6 C10 H7 119.4 . . ? C9 C10 H7 119.4 . . ? C8 C9 C10 117.7(18) . . ? C8 C9 C16 126(2) . . ? C10 C9 C16 116(2) . . ? C9 C8 C7 121(2) . . ? C9 C8 H9 119.5 . . ? C7 C8 H9 119.5 . . ? N2 C7 C8 119(2) . . ? N2 C7 C11 113.4(17) . . ? C8 C7 C11 127(2) . . ? N3 C11 C15 120.4(17) . . ? N3 C11 C7 114.8(18) . . ? C15 C11 C7 124.7(19) . . ? C14 C15 C11 117(2) . . ? C14 C15 H12 121.3 . . ? C11 C15 H12 121.3 . . ? C15 C14 C13 123(2) . . ? C15 C14 H13 118.6 . . ? C13 C14 H13 118.6 . . ? C12 C13 C14 115(2) . . ? C12 C13 H14 122.3 . . ? C14 C13 H14 122.3 . . ? C13 C12 N3 125(2) . . ? C13 C12 H15 117.5 . . ? N3 C12 H15 117.5 . . ? N6 C33 C34 122.0(19) . . ? N6 C33 H16 119.0 . . ? C34 C33 H16 119.0 . . ? C35 C34 C33 118.5(19) . . ? C35 C34 H17 120.7 . . ? C33 C34 H17 120.7 . . ? C34 C35 C36 120(2) . . ? C34 C35 H18 120.1 . . ? C36 C35 H18 120.1 . . ? C35 C36 C32 124(2) . . ? C35 C36 H19 118.2 . . ? C32 C36 H19 118.2 . . ? N6 C32 C36 117.6(18) . . ? N6 C32 C37 114.6(19) . . ? C36 C32 C37 127.8(19) . . ? N7 C37 C41 118.3(17) . . ? N7 C37 C32 115.4(18) . . ? C41 C37 C32 126.3(19) . . ? C37 C41 C40 118.5(19) . . ? C37 C41 H22 120.8 . . ? C40 C41 H22 120.8 . . ? C41 C40 C39 120.8(17) . . ? C41 C40 C47 118(2) . . ? C39 C40 C47 121(2) . . ? C38 C39 C40 115.6(19) . . ? C38 C39 H24 122.2 . . ? C40 C39 H24 122.2 . . ? N7 C38 C39 124.2(18) . . ? N7 C38 C42 110.2(18) . . ? C39 C38 C42 125(2) . . ? N8 C42 C46 119(2) . . ? N8 C42 C38 116(2) . . ? C46 C42 C38 125(2) . . ? C42 C46 C45 124(2) . . ? C42 C46 H27 118.2 . . ? C45 C46 H27 118.2 . . ? C44 C45 C46 116(3) . . ? C44 C45 H28 121.8 . . ? C46 C45 H28 121.8 . . ? C45 C44 C43 120(3) . . ? C45 C44 H29 120.2 . . ? C43 C44 H29 120.2 . . ? N8 C43 C44 123(2) . . ? N8 C43 H30 118.7 . . ? C44 C43 H30 118.7 . . ? N13 C74 C75 126(2) . . ? N13 C74 H31 117.1 . . ? C75 C74 H31 117.1 . . ? C76 C75 C74 117(2) . . ? C76 C75 H32 121.6 . . ? C74 C75 H32 121.6 . . ? C75 C76 C77 118(2) . . ? C75 C76 H33 120.8 . . ? C77 C76 H33 120.8 . . ? C73 C77 C76 119(2) . . ? C73 C77 H34 120.6 . . ? C76 C77 H34 120.6 . . ? C77 C73 N13 124(2) . . ? C77 C73 C69 125(2) . . ? N13 C73 C69 110.0(19) . . ? N12 C69 C70 123(2) . . ? N12 C69 C73 114(2) . . ? C70 C69 C73 123(2) . . ? C69 C70 C71 113.8(18) . . ? C69 C70 H37 123.1 . . ? C71 C70 H37 123.1 . . ? C72 C71 C70 122.0(17) . . ? C72 C71 C78 122(2) . . ? C70 C71 C78 116.0(19) . . ? C71 C72 C68 121.3(19) . . ? C71 C72 H39 119.3 . . ? C68 C72 H39 119.3 . . ? C72 C68 N12 118.9(19) . . ? C72 C68 C63 127(2) . . ? N12 C68 C63 113.6(18) . . ? C67 C63 N11 122(2) . . ? C67 C63 C68 126(2) . . ? N11 C63 C68 111.5(18) . . ? C66 C67 C63 123(2) . . ? C66 C67 H42 118.5 . . ? C63 C67 H42 118.5 . . ? C67 C66 C65 119(2) . . ? C67 C66 H43 120.4 . . ? C65 C66 H43 120.4 . . ? C64 C65 C66 117(2) . . ? C64 C65 H44 121.3 . . ? C66 C65 H44 121.3 . . ? N11 C64 C65 123(2) . . ? N11 C64 H45 118.3 . . ? C65 C64 H45 118.3 . . ? N16 C95 C96 120(2) . . ? N16 C95 H46 119.9 . . ? C96 C95 H46 119.9 . . ? C97 C96 C95 121(2) . . ? C97 C96 H47 119.7 . . ? C95 C96 H47 119.7 . . ? C96 C97 C98 118(2) . . ? C96 C97 H48 121.2 . . ? C98 C97 H48 121.2 . . ? C94 C98 C97 119(2) . . ? C94 C98 H49 120.6 . . ? C97 C98 H49 120.6 . . ? C98 C94 N16 122.0(19) . . ? C98 C94 C99 122(2) . . ? N16 C94 C99 115.5(19) . . ? C103 C99 N17 122(2) . . ? C103 C99 C94 126(2) . . ? N17 C99 C94 111.9(18) . . ? C99 C103 C102 120(2) . . ? C99 C103 H52 119.8 . . ? C102 C103 H52 119.8 . . ? C103 C102 C101 119.7(18) . . ? C103 C102 C109 121(2) . . ? C101 C102 C109 119(2) . . ? C100 C101 C102 117.7(18) . . ? C100 C101 H54 121.1 . . ? C102 C101 H54 121.1 . . ? N17 C100 C104 114.6(19) . . ? N17 C100 C101 118.2(17) . . ? C104 C100 C101 127(2) . . ? C108 C104 C100 125(2) . . ? C108 C104 N18 121(2) . . ? C100 C104 N18 114(2) . . ? C104 C108 C107 120(2) . . ? C104 C108 H57 120.0 . . ? C107 C108 H57 120.0 . . ? C106 C107 C108 120(2) . . ? C106 C107 H58 120.1 . . ? C108 C107 H58 120.1 . . ? C107 C106 C105 120(2) . . ? C107 C106 H59 120.1 . . ? C105 C106 H59 120.1 . . ? N18 C105 C106 124(2) . . ? N18 C105 H60 117.9 . . ? C106 C105 H60 117.9 . . ? N26 C152 C153 123(2) . . ? N26 C152 H61 118.6 . . ? C153 C152 H61 118.6 . . ? C154 C153 C152 118(3) . . ? C154 C153 H62 121.1 . . ? C152 C153 H62 121.1 . . ? C153 C154 C155 124(2) . . ? C153 C154 H63 118.1 . . ? C155 C154 H63 118.1 . . ? C154 C155 C151 116.6(18) . . ? C154 C155 H64 121.7 . . ? C151 C155 H64 121.7 . . ? N26 C151 C155 121.5(19) . . ? N26 C151 C156 116.5(19) . . ? C155 C151 C156 122.0(19) . . ? N27 C156 C160 119(2) . . ? N27 C156 C151 110.6(17) . . ? C160 C156 C151 130(2) . . ? C159 C160 C156 121(2) . . ? C159 C160 H67 119.6 . . ? C156 C160 H67 119.6 . . ? C158 C159 C160 115(2) . . ? C158 C159 C166 126(2) . . ? C160 C159 C166 119(2) . . ? C159 C158 C157 125(2) . . ? C159 C158 H69 117.7 . . ? C157 C158 H69 117.7 . . ? N27 C157 C158 120(2) . . ? N27 C157 C161 111.0(19) . . ? C158 C157 C161 129(2) . . ? N28 C161 C157 119(2) . . ? N28 C161 C165 117.2(19) . . ? C157 C161 C165 123.8(19) . . ? C164 C165 C161 118(2) . . ? C164 C165 H72 121.1 . . ? C161 C165 H72 121.1 . . ? C163 C164 C165 121(3) . . ? C163 C164 H73 119.3 . . ? C165 C164 H73 119.3 . . ? C164 C163 C162 124(2) . . ? C164 C163 H74 117.9 . . ? C162 C163 H74 117.9 . . ? C163 C162 N28 117(2) . . ? C163 C162 H75 121.6 . . ? N28 C162 H75 121.6 . . ? C137 C136 N23 119(2) . . ? C137 C136 H76 120.5 . . ? N23 C136 H76 120.5 . . ? C138 C139 C135 113(2) . . ? C138 C139 H79 123.3 . . ? C135 C139 H79 123.3 . . ? N23 C135 C139 124(2) . . ? N23 C135 C131 115.4(19) . . ? C139 C135 C131 120.8(19) . . ? C132 C131 N22 123.2(17) . . ? C132 C131 C135 128.4(19) . . ? N22 C131 C135 108.0(17) . . ? C133 C132 C131 120.0(19) . . ? C133 C132 H82 120.0 . . ? C131 C132 H82 120.0 . . ? C134 C133 C132 120.8(19) . . ? C134 C133 C140 117.3(18) . . ? C132 C133 C140 121.8(19) . . ? C133 C134 C130 117.7(18) . . ? C133 C134 H84 121.2 . . ? C130 C134 H84 121.2 . . ? N22 C130 C134 121.2(17) . . ? N22 C130 C125 113.4(16) . . ? C134 C130 C125 125.4(16) . . ? C125 N21 C126 120.0 . . ? C125 N21 Ru3 113.8(8) . . ? C126 N21 Ru3 126.2(8) . . ? N21 C125 C129 120.0 . . ? N21 C125 C130 113.0(12) . . ? C129 C125 C130 127.0(12) . . ? C125 C129 C128 120.0 . . ? C125 C129 H87 120.0 . . ? C128 C129 H87 120.0 . . ? C129 C128 C127 120.0 . . ? C129 C128 H88 120.0 . . ? C127 C128 H88 120.0 . . ? C126 C127 C128 120.0 . . ? C126 C127 H89 120.0 . . ? C128 C127 H89 120.0 . . ? C127 C126 N21 120.0 . . ? C127 C126 H90 120.0 . . ? N21 C126 H90 120.0 . . ? C16 C21 C20 121(2) . . ? C16 C21 H91 119.7 . . ? C20 C21 H91 119.7 . . ? C19 C20 C21 117(2) . . ? C19 C20 C27 125.3(19) . . ? C21 C20 C27 118(2) . . ? C20 C19 C18 126(2) . . ? C20 C19 H93 116.9 . . ? C18 C19 H93 116.9 . . ? C19 C18 C22 125.5(19) . . ? C19 C18 C17 114(2) . . ? C22 C18 C17 120.5(19) . . ? C16 C17 C18 122(2) . . ? C16 C17 H95 118.8 . . ? C18 C17 H95 118.8 . . ? C21 C16 C17 120(2) . . ? C21 C16 C9 122(2) . . ? C17 C16 C9 118(2) . . ? C52 C47 C48 121(2) . . ? C52 C47 C40 120(2) . . ? C48 C47 C40 119(2) . . ? C47 C52 C51 119(2) . . ? C47 C52 H98 120.4 . . ? C51 C52 H98 120.4 . . ? C50 C51 C52 119(2) . . ? C50 C51 C58 123(2) . . ? C52 C51 C58 117(2) . . ? C51 C50 C49 123(2) . . ? C51 C50 H100 118.6 . . ? C49 C50 H100 118.6 . . ? C50 C49 C48 121(2) . . ? C50 C49 C53 122.4(19) . . ? C48 C49 C53 117(2) . . ? C49 C48 C47 116(2) . . ? C49 C48 H102 121.9 . . ? C47 C48 H102 121.9 . . ? C83 C78 C79 116(2) . . ? C83 C78 C71 121(2) . . ? C79 C78 C71 123(2) . . ? C82 C83 C78 123(2) . . ? C82 C83 H110 118.5 . . ? C78 C83 H110 118.5 . . ? C81 C82 C83 117(2) . . ? C81 C82 C89 125(2) . . ? C83 C82 C89 118.2(19) . . ? C82 C81 C80 124(2) . . ? C82 C81 H112 117.8 . . ? C80 C81 H112 117.8 . . ? C79 C80 C81 117(2) . . ? C79 C80 C84 119.8(19) . . ? C81 C80 C84 123.3(18) . . ? C80 C79 C78 122(2) . . ? C80 C79 H114 118.8 . . ? C78 C79 H114 118.8 . . ? C111 C110 C109 119(2) . . ? C111 C110 H115 120.3 . . ? C109 C110 H115 120.3 . . ? C112 C111 C110 120(2) . . ? C112 C111 C115 118(2) . . ? C110 C111 C115 122(2) . . ? C111 C112 C113 121.0(19) . . ? C111 C112 H117 119.5 . . ? C113 C112 H117 119.5 . . ? C114 C113 C112 118.9(14) . . ? C114 C113 C10B 113(2) . . ? C112 C113 C10B 127(2) . . ? C114 C113 C10A 123.9(16) . . ? C112 C113 C10A 114.6(14) . . ? C113 C114 C109 122(2) . . ? C113 C114 H119 119.2 . . ? C109 C114 H119 119.2 . . ? C114 C109 C110 119(2) . . ? C114 C109 C102 122(2) . . ? C110 C109 C102 119(2) . . ? C141 C140 C133 122(2) . . ? C141 C140 C145 116(2) . . ? C133 C140 C145 121.9(19) . . ? C142 C141 C140 122(2) . . ? C142 C141 H122 119.2 . . ? C140 C141 H122 119.2 . . ? C141 C142 C143 118(2) . . ? C141 C142 C146 121(2) . . ? C143 C142 C146 120.2(19) . . ? C144 C143 C142 122.1(19) . . ? C144 C143 H124 118.9 . . ? C142 C143 H124 118.9 . . ? C145 C144 C143 119.0(14) . . ? C145 C144 C16B 112(2) . . ? C143 C144 C16B 128(2) . . ? C145 C144 C16A 122.0(15) . . ? C143 C144 C16A 118.3(15) . . ? C144 C145 C140 122.9(19) . . ? C144 C145 H126 118.6 . . ? C140 C145 H126 118.6 . . ? C171 C166 C167 119(2) . . ? C171 C166 C159 122(2) . . ? C167 C166 C159 119(2) . . ? C166 C171 C170 121(2) . . ? C166 C171 H129 119.6 . . ? C170 C171 H129 119.6 . . ? C169 C170 C171 119(2) . . ? C169 C170 C177 128(2) . . ? C171 C170 C177 114(2) . . ? C170 C169 C168 124(2) . . ? C170 C169 H131 118.1 . . ? C168 C169 H131 118.1 . . ? C169 C168 C167 117(2) . . ? C169 C168 C172 120.8(19) . . ? C167 C168 C172 121.3(19) . . ? C166 C167 C168 120(2) . . ? C166 C167 H133 119.9 . . ? C168 C167 H133 119.9 . . ? C26 C22 C23 120.0 . . ? C26 C22 C18 123.7(13) . . ? C23 C22 C18 116.2(13) . . ? C25 C26 C22 120.0 . . ? C25 C26 H201 120.0 . . ? C22 C26 H201 120.0 . . ? N4 C25 C26 120.0 . . ? N4 C25 H202 120.0 . . ? C26 C25 H202 120.0 . . ? C25 N4 C24 120.0 . . ? C23 C24 N4 120.0 . . ? C23 C24 H203 120.0 . . ? N4 C24 H203 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H204 120.0 . . ? C22 C23 H204 120.0 . . ? C30 C31 C27 120.0 . . ? C30 C31 H205 120.0 . . ? C27 C31 H205 120.0 . . ? C31 C30 N5 120.0 . . ? C31 C30 H206 120.0 . . ? N5 C30 H206 120.0 . . ? C29 N5 C30 120.0 . . ? C28 C29 N5 120.0 . . ? C28 C29 H207 120.0 . . ? N5 C29 H207 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H208 120.0 . . ? C27 C28 H208 120.0 . . ? C28 C27 C31 120.0 . . ? C28 C27 C20 125.8(14) . . ? C31 C27 C20 114.1(14) . . ? C62 C58 C59 120.0 . . ? C62 C58 C51 123.8(13) . . ? C59 C58 C51 116.1(13) . . ? C61 C62 C58 120.0 . . ? C61 C62 H211 120.0 . . ? C58 C62 H211 120.0 . . ? C62 C61 N10 120.0 . . ? C62 C61 H212 120.0 . . ? N10 C61 H212 120.0 . . ? C61 N10 C60 120.0 . . ? C59 C60 N10 120.0 . . ? C59 C60 H210 120.0 . . ? N10 C60 H210 120.0 . . ? C60 C59 C58 120.0 . . ? C60 C59 H209 120.0 . . ? C58 C59 H209 120.0 . . ? C54 C53 C57 120.0 . . ? C54 C53 C49 120.4(13) . . ? C57 C53 C49 119.5(13) . . ? C53 C54 C55 120.0 . . ? C53 C54 H213 120.0 . . ? C55 C54 H213 120.0 . . ? C54 C55 N9 120.0 . . ? C54 C55 H214 120.0 . . ? N9 C55 H214 120.0 . . ? C56 N9 C55 120.0 . . ? C57 C56 N9 120.0 . . ? C57 C56 H215 120.0 . . ? N9 C56 H215 120.0 . . ? C56 C57 C53 120.0 . . ? C56 C57 H216 120.0 . . ? C53 C57 H216 120.0 . . ? C85 C84 C88 120.0 . . ? C85 C84 C80 120.7(13) . . ? C88 C84 C80 119.3(13) . . ? C86 C85 C84 120.0 . . ? C86 C85 H217 120.0 . . ? C84 C85 H217 120.0 . . ? C85 C86 N14 120.0 . . ? C85 C86 H218 120.0 . . ? N14 C86 H218 120.0 . . ? C86 N14 C87 120.0 . . ? C88 C87 N14 120.0 . . ? C88 C87 H220 120.0 . . ? N14 C87 H220 120.0 . . ? C87 C88 C84 120.0 . . ? C87 C88 H221 120.0 . . ? C84 C88 H221 120.0 . . ? C89 C93 C92 121(2) . . ? C89 C93 H222 119.7 . . ? C92 C93 H222 119.7 . . ? N15 C92 C93 120(2) . . ? N15 C92 H223 120.1 . . ? C93 C92 H223 120.1 . . ? C91 C90 C89 124(2) . . ? C91 C90 H224 117.8 . . ? C89 C90 H224 117.8 . . ? N15 C91 C90 126(3) . . ? N15 C91 H225 116.8 . . ? C90 C91 H225 116.8 . . ? C117 C116 C115 116.8(19) . . ? C117 C116 H226 121.6 . . ? C115 C116 H226 121.6 . . ? N19 C117 C116 130(2) . . ? N19 C117 H227 115.2 . . ? C116 C117 H227 115.2 . . ? C119 C118 N19 130(2) . . ? C119 C118 H228 114.8 . . ? N19 C118 H228 114.8 . . ? C118 C119 C115 119(2) . . ? C118 C119 H229 120.3 . . ? C115 C119 H229 120.3 . . ? C147 C146 C150 120.0 . . ? C147 C146 C142 120.6(13) . . ? C150 C146 C142 119.4(13) . . ? C148 C147 C146 120.0 . . ? C148 C147 H244 120.0 . . ? C146 C147 H244 120.0 . . ? C147 C148 N24 120.0 . . ? C147 C148 H242 120.0 . . ? N24 C148 H242 120.0 . . ? C149 N24 C148 120.0 . . ? N24 C149 C150 120.0 . . ? N24 C149 H245 120.0 . . ? C150 C149 H245 120.0 . . ? C149 C150 C146 120.0 . . ? C149 C150 H260 120.0 . . ? C146 C150 H260 120.0 . . ? C176 C172 C173 120.0 . . ? C176 C172 C168 118.0(15) . . ? C173 C172 C168 121.3(15) . . ? C172 C176 C175 120.0 . . ? C172 C176 H257 120.0 . . ? C175 C176 H257 120.0 . . ? N29 C175 C176 120.0 . . ? N29 C175 H266 120.0 . . ? C176 C175 H266 120.0 . . ? C175 N29 C174 120.0 . . ? C173 C174 N29 120.0 . . ? C173 C174 H254 120.0 . . ? N29 C174 H254 120.0 . . ? C174 C173 C172 120.0 . . ? C174 C173 H255 120.0 . . ? C172 C173 H255 120.0 . . ? C93 C89 C90 111.5(19) . . ? C93 C89 C82 123.6(18) . . ? C90 C89 C82 125(2) . . ? C119 C115 C116 116(2) . . ? C119 C115 C111 124(2) . . ? C116 C115 C111 119.8(19) . . ? C14B C10B C11B 120.0 . . ? C14B C10B C113 128(2) . . ? C11B C10B C113 111(2) . . ? C10B C14B C13B 120.0 . . ? C10B C14B C13B 144(3) . 2_675 ? C13B C14B C13B 96(3) . 2_675 ? C10B C14B H902 120.0 . . ? C13B C14B H902 120.0 . . ? C13B C14B H902 24.3 2_675 . ? N20B C13B C14B 120.0 . . ? N20B C13B C14B 156(3) . 2_675 ? C14B C13B C14B 84(3) . 2_675 ? N20B C13B H901 120.0 . . ? C14B C13B H901 120.0 . . ? C14B C13B H901 36.0 2_675 . ? C13B N20B C12B 120.0 . . ? C11B C12B N20B 120.0 . . ? C11B C12B H235 120.0 . . ? N20B C12B H235 120.0 . . ? C12B C11B C10B 120.0 . . ? C12B C11B H237 120.0 . . ? C10B C11B H237 120.0 . . ? C14A C10A C11A 120.0 . . ? C14A C10A C113 128.2(16) . . ? C11A C10A C113 110.5(17) . . ? C13A C14A C10A 120.0 . . ? C13A C14A H311 120.0 . . ? C10A C14A H311 120.0 . . ? C14A C13A N20A 120.0 . . ? C14A C13A H310 120.0 . . ? N20A C13A H310 120.0 . . ? C13A N20A C12A 120.0 . . ? C11A C12A N20A 120.0 . . ? C11A C12A H312 120.0 . . ? N20A C12A H312 120.0 . . ? C12A C11A C10A 120.0 . . ? C12A C11A H313 120.0 . . ? C10A C11A H313 120.0 . . ? C17B C16B C15B 120.0 . . ? C17B C16B C144 114(3) . . ? C15B C16B C144 126(3) . . ? C16B C17B C18B 120.0 . . ? C16B C17B H261 120.0 . . ? C18B C17B H261 120.0 . . ? N25B C18B C17B 120.0 . . ? N25B C18B H253 120.0 . . ? C17B C18B H253 120.0 . . ? C18B N25B C19B 120.0 . . ? C15B C19B N25B 120.0 . . ? C15B C19B H904 120.0 . . ? N25B C19B H904 120.0 . . ? C19B C15B C16B 120.0 . . ? C19B C15B H903 120.0 . . ? C16B C15B H903 120.0 . . ? C15A C16A C17A 120.0 . . ? C15A C16A C144 127.0(17) . . ? C17A C16A C144 113.0(18) . . ? C16A C15A C19A 120.0 . . ? C16A C15A H315 120.0 . . ? C19A C15A H315 120.0 . . ? N25A C19A C15A 120.0 . . ? N25A C19A H316 120.0 . . ? C15A C19A H316 120.0 . . ? C19A N25A C18A 120.0 . . ? N25A C18A C17A 120.0 . . ? N25A C18A H318 120.0 . . ? C17A C18A H318 120.0 . . ? C18A C17A C16A 120.0 . . ? C18A C17A H319 120.0 . . ? C16A C17A H319 120.0 . . ? C181 C177 C178 120.0 . . ? C181 C177 C170 116.3(15) . . ? C178 C177 C170 123.4(15) . . ? C177 C181 C180 120.0 . . ? C177 C181 H251 120.0 . . ? C180 C181 H251 120.0 . . ? N30 C180 C181 120.0 . . ? N30 C180 H250 120.0 . . ? C181 C180 H250 120.0 . . ? C180 N30 C179 120.0 . . ? N30 C179 C178 120.0 . . ? N30 C179 H252 120.0 . . ? C178 C179 H252 120.0 . . ? C179 C178 C177 120.0 . . ? C179 C178 H263 120.0 . . ? C177 C178 H263 120.0 . . ? C1 N1 C2 118(2) . . ? C1 N1 Ru1 114.2(15) . . ? C2 N1 Ru1 127.5(15) . . ? C6 N2 C7 123.2(17) . . ? C6 N2 Ru1 117.9(16) . . ? C7 N2 Ru1 118.3(15) . . ? C12 N3 C11 117.9(19) . . ? C12 N3 Ru1 128.5(17) . . ? C11 N3 Ru1 113.0(13) . . ? C33 N6 C32 118.2(18) . . ? C33 N6 Ru1 128.3(14) . . ? C32 N6 Ru1 113.5(13) . . ? C38 N7 C37 122.3(16) . . ? C38 N7 Ru1 121.9(13) . . ? C37 N7 Ru1 115.6(13) . . ? C42 N8 C43 118.3(19) . . ? C42 N8 Ru1 114.4(15) . . ? C43 N8 Ru1 126.3(14) . . ? C95 N16 C94 120.3(18) . . ? C95 N16 Ru2 126.2(15) . . ? C94 N16 Ru2 113.5(14) . . ? C99 N17 C100 122.0(17) . . ? C99 N17 Ru2 120.3(14) . . ? C100 N17 Ru2 117.6(14) . . ? C105 N18 C104 115.3(19) . . ? C105 N18 Ru2 131.6(15) . . ? C104 N18 Ru2 113.1(14) . . ? C64 N11 C63 114.3(18) . . ? C64 N11 Ru2 130.1(15) . . ? C63 N11 Ru2 115.6(13) . . ? C69 N12 C68 120.6(19) . . ? C69 N12 Ru2 121.6(15) . . ? C68 N12 Ru2 117.7(14) . . ? C74 N13 C73 115(2) . . ? C74 N13 Ru2 128.0(16) . . ? C73 N13 Ru2 116.6(15) . . ? C130 N22 C131 117.0(16) . . ? C130 N22 Ru3 118.8(13) . . ? C131 N22 Ru3 123.4(12) . . ? C135 N23 C136 121.1(19) . . ? C135 N23 Ru3 115.5(15) . . ? C136 N23 Ru3 123.4(14) . . ? C157 N27 C156 120.4(18) . . ? C157 N27 Ru3 119.6(15) . . ? C156 N27 Ru3 119.6(14) . . ? C152 N26 C151 118(2) . . ? C152 N26 Ru3 127.7(17) . . ? C151 N26 Ru3 114.4(14) . . ? C161 N28 C162 122.4(19) . . ? C161 N28 Ru3 111.8(14) . . ? C162 N28 Ru3 125.6(16) . . ? C91 N15 C92 116(2) . . ? C118 N19 C117 107.2(18) . . ? F2 P1 F2 180.0(7) 2_576 . ? F2 P1 F1 83.8(14) 2_576 2_576 ? F2 P1 F1 96.2(14) . 2_576 ? F2 P1 F1 96.2(14) 2_576 . ? F2 P1 F1 83.8(14) . . ? F1 P1 F1 180.0 2_576 . ? F2 P1 F3 95.2(19) 2_576 . ? F2 P1 F3 84.8(19) . . ? F1 P1 F3 91.0(16) 2_576 . ? F1 P1 F3 89.0(16) . . ? F2 P1 F3 84.8(19) 2_576 2_576 ? F2 P1 F3 95.2(19) . 2_576 ? F1 P1 F3 89.0(16) 2_576 2_576 ? F1 P1 F3 91.0(16) . 2_576 ? F3 P1 F3 180(4) . 2_576 ? O3A N1A O2A 126(3) . . ? O3A N1A O1A 116(3) . . ? O2A N1A O1A 118(3) . . ? P4A P2A P4B 53(4) . . ? P4A P2A P4D 37(3) . . ? P4B P2A P4D 85(5) . . ? P5A P2B P6D 57(3) . . ? P5A P2B P9A 53(5) . . ? P6D P2B P9A 105(6) . . ? P5A P2B P5D 24(4) . . ? P6D P2B P5D 75(4) . . ? P9A P2B P5D 30(5) . . ? P8B P2C P3A 57(3) . . ? P8B P2C P5B 131(5) . . ? P3A P2C P5B 100(4) . . ? P3C P3 P7B 21(2) . . ? P8B P3A P2C 57(3) . . ? P8B P3A P5B 88(4) . . ? P2C P3A P5B 41(3) . . ? P7B P3C P3 136(4) . . ? P4B P4A P2A 69(5) . . ? P4B P4A P4D 146(7) . . ? P2A P4A P4D 107(6) . . ? P4A P4B P2A 58(5) . . ? P4A P4B P4D 18(4) . . ? P2A P4B P4D 60(4) . . ? P6B P4C P8C 171(5) . . ? P4A P4D P2A 35(3) . . ? P4A P4D P4B 16(3) . . ? P2A P4D P4B 35(2) . . ? P2B P5A P6D 70(4) . . ? P2B P5A P9A 76(6) . . ? P6D P5A P9A 135(7) . . ? P2B P5A P5D 135(7) . . ? P6D P5A P5D 137(6) . . ? P9A P5A P5D 61(6) . . ? P2C P5B P3A 39(2) . . ? P2C P5B P8B 23(2) . . ? P3A P5B P8B 30.9(18) . . ? P9A P5D P5A 56(6) . . ? P9A P5D P2B 36(6) . . ? P5A P5D P2B 22(3) . . ? P9A P5D P6D 70(7) . . ? P5A P5D P6D 21(3) . . ? P2B P5D P6D 35(2) . . ? P4C P6B P8C 5(3) . . ? P5A P6D P2B 54(3) . . ? P5A P6D P9A 22(3) . . ? P2B P6D P9A 39(3) . . ? P5A P6D P5D 22(3) . . ? P2B P6D P5D 70(3) . . ? P9A P6D P5D 32(3) . . ? P3C P7B P3 23(2) . . ? P2C P8B P3A 66(4) . . ? P2C P8B P5B 26(3) . . ? P3A P8B P5B 62(4) . . ? P4C P8C P6B 4(2) . . ? P5D P9A P5A 63(7) . . ? P5D P9A P2B 114(9) . . ? P5A P9A P2B 52(5) . . ? P5D P9A P6D 78(7) . . ? P5A P9A P6D 23(4) . . ? P2B P9A P6D 36(3) . . ? N2 Ru1 N7 175.5(7) . . ? N2 Ru1 N8 105.0(6) . . ? N7 Ru1 N8 77.0(6) . . ? N2 Ru1 N1 78.7(8) . . ? N7 Ru1 N1 97.2(7) . . ? N8 Ru1 N1 95.7(7) . . ? N2 Ru1 N6 97.7(6) . . ? N7 Ru1 N6 80.4(6) . . ? N8 Ru1 N6 157.4(6) . . ? N1 Ru1 N6 88.5(5) . . ? N2 Ru1 N3 79.6(8) . . ? N7 Ru1 N3 104.5(7) . . ? N8 Ru1 N3 87.4(5) . . ? N1 Ru1 N3 158.2(7) . . ? N6 Ru1 N3 96.9(7) . . ? N17 Ru2 N12 176.2(8) . . ? N17 Ru2 N11 95.7(7) . . ? N12 Ru2 N11 81.3(7) . . ? N17 Ru2 N18 80.4(7) . . ? N12 Ru2 N18 97.5(7) . . ? N11 Ru2 N18 95.9(7) . . ? N17 Ru2 N13 105.8(7) . . ? N12 Ru2 N13 77.3(8) . . ? N11 Ru2 N13 158.5(7) . . ? N18 Ru2 N13 89.3(7) . . ? N17 Ru2 N16 78.7(7) . . ? N12 Ru2 N16 103.5(7) . . ? N11 Ru2 N16 88.8(7) . . ? N18 Ru2 N16 158.9(7) . . ? N13 Ru2 N16 93.9(7) . . ? N22 Ru3 N27 176.9(8) . . ? N22 Ru3 N21 79.7(6) . . ? N27 Ru3 N21 100.3(6) . . ? N22 Ru3 N26 98.5(7) . . ? N27 Ru3 N26 78.4(7) . . ? N21 Ru3 N26 91.3(6) . . ? N22 Ru3 N23 77.4(6) . . ? N27 Ru3 N23 102.7(7) . . ? N21 Ru3 N23 156.9(6) . . ? N26 Ru3 N23 95.0(6) . . ? N22 Ru3 N28 104.9(7) . . ? N27 Ru3 N28 78.2(7) . . ? N21 Ru3 N28 90.6(6) . . ? N26 Ru3 N28 156.5(6) . . ? N23 Ru3 N28 92.4(6) . . ? C136 C137 C138 117.8(19) . . ? C136 C137 H77 121.1 . . ? C138 C137 H77 121.1 . . ? C139 C138 C137 125(2) . . ? C139 C138 H78 117.6 . . ? C137 C138 H78 117.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 -6(3) . . . . ? C2 C3 C4 C5 5(3) . . . . ? C3 C4 C5 C1 -2(3) . . . . ? C4 C5 C1 C6 -179(2) . . . . ? C4 C5 C1 N1 1(3) . . . . ? C5 C1 C6 N2 -174(2) . . . . ? N1 C1 C6 N2 5(3) . . . . ? C5 C1 C6 C10 10(4) . . . . ? N1 C1 C6 C10 -170(2) . . . . ? N2 C6 C10 C9 6(3) . . . . ? C1 C6 C10 C9 -178(2) . . . . ? C6 C10 C9 C8 -2(3) . . . . ? C6 C10 C9 C16 -177(2) . . . . ? C10 C9 C8 C7 -3(3) . . . . ? C16 C9 C8 C7 171(2) . . . . ? C9 C8 C7 N2 5(3) . . . . ? C9 C8 C7 C11 -173.3(19) . . . . ? N2 C7 C11 N3 -10(2) . . . . ? C8 C7 C11 N3 167.7(18) . . . . ? N2 C7 C11 C15 174.8(18) . . . . ? C8 C7 C11 C15 -7(3) . . . . ? N3 C11 C15 C14 8(3) . . . . ? C7 C11 C15 C14 -177.4(19) . . . . ? C11 C15 C14 C13 -12(3) . . . . ? C15 C14 C13 C12 11(4) . . . . ? C14 C13 C12 N3 -8(4) . . . . ? N6 C33 C34 C35 7(3) . . . . ? C33 C34 C35 C36 -3(3) . . . . ? C34 C35 C36 C32 0(4) . . . . ? C35 C36 C32 N6 0(4) . . . . ? C35 C36 C32 C37 -179(2) . . . . ? N6 C32 C37 N7 5(3) . . . . ? C36 C32 C37 N7 -177(2) . . . . ? N6 C32 C37 C41 -177(2) . . . . ? C36 C32 C37 C41 2(4) . . . . ? N7 C37 C41 C40 -3(3) . . . . ? C32 C37 C41 C40 179(2) . . . . ? C37 C41 C40 C39 3(3) . . . . ? C37 C41 C40 C47 -170(2) . . . . ? C41 C40 C39 C38 1(3) . . . . ? C47 C40 C39 C38 174(2) . . . . ? C40 C39 C38 N7 -5(3) . . . . ? C40 C39 C38 C42 -177(2) . . . . ? N7 C38 C42 N8 -9(3) . . . . ? C39 C38 C42 N8 164(2) . . . . ? N7 C38 C42 C46 167(2) . . . . ? C39 C38 C42 C46 -20(4) . . . . ? N8 C42 C46 C45 -2(4) . . . . ? C38 C42 C46 C45 -178(2) . . . . ? C42 C46 C45 C44 2(4) . . . . ? C46 C45 C44 C43 -2(4) . . . . ? C45 C44 C43 N8 2(4) . . . . ? N13 C74 C75 C76 -2(4) . . . . ? C74 C75 C76 C77 5(3) . . . . ? C75 C76 C77 C73 -9(4) . . . . ? C76 C77 C73 N13 10(4) . . . . ? C76 C77 C73 C69 177(2) . . . . ? C77 C73 C69 N12 -170(2) . . . . ? N13 C73 C69 N12 -2(3) . . . . ? C77 C73 C69 C70 11(4) . . . . ? N13 C73 C69 C70 179.6(19) . . . . ? N12 C69 C70 C71 -1(3) . . . . ? C73 C69 C70 C71 177(2) . . . . ? C69 C70 C71 C72 3(3) . . . . ? C69 C70 C71 C78 -177.4(18) . . . . ? C70 C71 C72 C68 1(3) . . . . ? C78 C71 C72 C68 -178(2) . . . . ? C71 C72 C68 N12 -7(3) . . . . ? C71 C72 C68 C63 177(2) . . . . ? C72 C68 C63 C67 -6(4) . . . . ? N12 C68 C63 C67 178(2) . . . . ? C72 C68 C63 N11 171(2) . . . . ? N12 C68 C63 N11 -6(3) . . . . ? N11 C63 C67 C66 1(4) . . . . ? C68 C63 C67 C66 177(2) . . . . ? C63 C67 C66 C65 -3(4) . . . . ? C67 C66 C65 C64 2(3) . . . . ? C66 C65 C64 N11 2(3) . . . . ? N16 C95 C96 C97 3(5) . . . . ? C95 C96 C97 C98 2(5) . . . . ? C96 C97 C98 C94 -6(4) . . . . ? C97 C98 C94 N16 5(4) . . . . ? C97 C98 C94 C99 -177(2) . . . . ? C98 C94 C99 C103 9(4) . . . . ? N16 C94 C99 C103 -174(2) . . . . ? C98 C94 C99 N17 -177(2) . . . . ? N16 C94 C99 N17 1(3) . . . . ? N17 C99 C103 C102 3(4) . . . . ? C94 C99 C103 C102 177(2) . . . . ? C99 C103 C102 C101 4(3) . . . . ? C99 C103 C102 C109 -177(2) . . . . ? C103 C102 C101 C100 -7(3) . . . . ? C109 C102 C101 C100 173.8(17) . . . . ? C102 C101 C100 N17 3(3) . . . . ? C102 C101 C100 C104 -173.2(19) . . . . ? N17 C100 C104 C108 173(2) . . . . ? C101 C100 C104 C108 -11(3) . . . . ? N17 C100 C104 N18 -3(2) . . . . ? C101 C100 C104 N18 173.7(17) . . . . ? C100 C104 C108 C107 -176.4(19) . . . . ? N18 C104 C108 C107 -1(3) . . . . ? C104 C108 C107 C106 -4(3) . . . . ? C108 C107 C106 C105 5(3) . . . . ? C107 C106 C105 N18 -2(3) . . . . ? N26 C152 C153 C154 -2(4) . . . . ? C152 C153 C154 C155 -1(4) . . . . ? C153 C154 C155 C151 3(4) . . . . ? C154 C155 C151 N26 -1(3) . . . . ? C154 C155 C151 C156 178(2) . . . . ? N26 C151 C156 N27 -8(3) . . . . ? C155 C151 C156 N27 172.8(18) . . . . ? N26 C151 C156 C160 177.1(19) . . . . ? C155 C151 C156 C160 -2(4) . . . . ? N27 C156 C160 C159 7(3) . . . . ? C151 C156 C160 C159 -179(2) . . . . ? C156 C160 C159 C158 -2(3) . . . . ? C156 C160 C159 C166 176.0(18) . . . . ? C160 C159 C158 C157 -3(3) . . . . ? C166 C159 C158 C157 178(2) . . . . ? C159 C158 C157 N27 5(4) . . . . ? C159 C158 C157 C161 -179(2) . . . . ? N27 C157 C161 N28 0(3) . . . . ? C158 C157 C161 N28 -176(2) . . . . ? N27 C157 C161 C165 -176.0(19) . . . . ? C158 C157 C161 C165 7(4) . . . . ? N28 C161 C165 C164 -1(3) . . . . ? C157 C161 C165 C164 176(2) . . . . ? C161 C165 C164 C163 5(4) . . . . ? C165 C164 C163 C162 -4(5) . . . . ? C164 C163 C162 N28 0(4) . . . . ? C138 C139 C135 N23 -4(3) . . . . ? C138 C139 C135 C131 175(2) . . . . ? N23 C135 C131 C132 167(2) . . . . ? C139 C135 C131 C132 -11(4) . . . . ? N23 C135 C131 N22 -6(3) . . . . ? C139 C135 C131 N22 176(2) . . . . ? N22 C131 C132 C133 -1(3) . . . . ? C135 C131 C132 C133 -173(2) . . . . ? C131 C132 C133 C134 1(3) . . . . ? C131 C132 C133 C140 177(2) . . . . ? C132 C133 C134 C130 -1(3) . . . . ? C140 C133 C134 C130 -178(2) . . . . ? C133 C134 C130 N22 2(3) . . . . ? C133 C134 C130 C125 -175.8(19) . . . . ? C126 N21 C125 C129 0.0 . . . . ? Ru3 N21 C125 C129 -179.5(9) . . . . ? C126 N21 C125 C130 179.0(15) . . . . ? Ru3 N21 C125 C130 -0.5(13) . . . . ? N22 C130 C125 N21 9(2) . . . . ? C134 C130 C125 N21 -173.3(17) . . . . ? N22 C130 C125 C129 -172.4(13) . . . . ? C134 C130 C125 C129 6(3) . . . . ? N21 C125 C129 C128 0.0 . . . . ? C130 C125 C129 C128 -178.9(17) . . . . ? C125 C129 C128 C127 0.0 . . . . ? C129 C128 C127 C126 0.0 . . . . ? C128 C127 C126 N21 0.0 . . . . ? C125 N21 C126 C127 0.0 . . . . ? Ru3 N21 C126 C127 179.5(11) . . . . ? C16 C21 C20 C19 1(4) . . . . ? C16 C21 C20 C27 -177(2) . . . . ? C21 C20 C19 C18 2(4) . . . . ? C27 C20 C19 C18 179(2) . . . . ? C20 C19 C18 C22 174(2) . . . . ? C20 C19 C18 C17 -3(4) . . . . ? C19 C18 C17 C16 2(3) . . . . ? C22 C18 C17 C16 -175(2) . . . . ? C20 C21 C16 C17 -2(4) . . . . ? C20 C21 C16 C9 173(2) . . . . ? C18 C17 C16 C21 0(4) . . . . ? C18 C17 C16 C9 -175(2) . . . . ? C8 C9 C16 C21 -137(3) . . . . ? C10 C9 C16 C21 38(3) . . . . ? C8 C9 C16 C17 38(4) . . . . ? C10 C9 C16 C17 -147(2) . . . . ? C41 C40 C47 C52 42(3) . . . . ? C39 C40 C47 C52 -132(2) . . . . ? C41 C40 C47 C48 -138(2) . . . . ? C39 C40 C47 C48 49(3) . . . . ? C48 C47 C52 C51 -4(4) . . . . ? C40 C47 C52 C51 176(2) . . . . ? C47 C52 C51 C50 6(4) . . . . ? C47 C52 C51 C58 -173(2) . . . . ? C52 C51 C50 C49 -6(4) . . . . ? C58 C51 C50 C49 173(2) . . . . ? C51 C50 C49 C48 3(4) . . . . ? C51 C50 C49 C53 -178(2) . . . . ? C50 C49 C48 C47 -1(3) . . . . ? C53 C49 C48 C47 179.9(19) . . . . ? C52 C47 C48 C49 1(4) . . . . ? C40 C47 C48 C49 -179(2) . . . . ? C72 C71 C78 C83 -144(2) . . . . ? C70 C71 C78 C83 36(3) . . . . ? C72 C71 C78 C79 33(3) . . . . ? C70 C71 C78 C79 -146(2) . . . . ? C79 C78 C83 C82 2(3) . . . . ? C71 C78 C83 C82 180(2) . . . . ? C78 C83 C82 C81 0(4) . . . . ? C78 C83 C82 C89 -177(2) . . . . ? C83 C82 C81 C80 -3(4) . . . . ? C89 C82 C81 C80 173(2) . . . . ? C82 C81 C80 C79 5(4) . . . . ? C82 C81 C80 C84 -176(2) . . . . ? C81 C80 C79 C78 -4(3) . . . . ? C84 C80 C79 C78 177.3(19) . . . . ? C83 C78 C79 C80 0(3) . . . . ? C71 C78 C79 C80 -177(2) . . . . ? C109 C110 C111 C112 1(4) . . . . ? C109 C110 C111 C115 -178(2) . . . . ? C110 C111 C112 C113 0(4) . . . . ? C115 C111 C112 C113 179(2) . . . . ? C111 C112 C113 C114 -1(3) . . . . ? C111 C112 C113 C10B -166(2) . . . . ? C111 C112 C113 C10A 162(2) . . . . ? C112 C113 C114 C109 1(4) . . . . ? C10B C113 C114 C109 169(2) . . . . ? C10A C113 C114 C109 -160(2) . . . . ? C113 C114 C109 C110 -1(4) . . . . ? C113 C114 C109 C102 -177(2) . . . . ? C111 C110 C109 C114 -1(4) . . . . ? C111 C110 C109 C102 175(2) . . . . ? C103 C102 C109 C114 38(3) . . . . ? C101 C102 C109 C114 -142(2) . . . . ? C103 C102 C109 C110 -138(2) . . . . ? C101 C102 C109 C110 42(3) . . . . ? C134 C133 C140 C141 -141(2) . . . . ? C132 C133 C140 C141 43(3) . . . . ? C134 C133 C140 C145 41(3) . . . . ? C132 C133 C140 C145 -135(2) . . . . ? C133 C140 C141 C142 180(2) . . . . ? C145 C140 C141 C142 -3(3) . . . . ? C140 C141 C142 C143 0(4) . . . . ? C140 C141 C142 C146 -177(2) . . . . ? C141 C142 C143 C144 4(4) . . . . ? C146 C142 C143 C144 -179.5(19) . . . . ? C142 C143 C144 C145 -5(3) . . . . ? C142 C143 C144 C16B -172(3) . . . . ? C142 C143 C144 C16A 165(2) . . . . ? C143 C144 C145 C140 2(4) . . . . ? C16B C144 C145 C140 172(2) . . . . ? C16A C144 C145 C140 -168(2) . . . . ? C141 C140 C145 C144 1(4) . . . . ? C133 C140 C145 C144 179(2) . . . . ? C158 C159 C166 C171 -153(2) . . . . ? C160 C159 C166 C171 29(3) . . . . ? C158 C159 C166 C167 28(4) . . . . ? C160 C159 C166 C167 -150(2) . . . . ? C167 C166 C171 C170 -6(4) . . . . ? C159 C166 C171 C170 175(2) . . . . ? C166 C171 C170 C169 5(4) . . . . ? C166 C171 C170 C177 -178(2) . . . . ? C171 C170 C169 C168 0(4) . . . . ? C177 C170 C169 C168 -176(2) . . . . ? C170 C169 C168 C167 -3(4) . . . . ? C170 C169 C168 C172 -173(2) . . . . ? C171 C166 C167 C168 2(4) . . . . ? C159 C166 C167 C168 -179(2) . . . . ? C169 C168 C167 C166 2(3) . . . . ? C172 C168 C167 C166 172(2) . . . . ? C19 C18 C22 C26 -148.8(19) . . . . ? C17 C18 C22 C26 28(3) . . . . ? C19 C18 C22 C23 34(3) . . . . ? C17 C18 C22 C23 -149.0(17) . . . . ? C23 C22 C26 C25 0.0 . . . . ? C18 C22 C26 C25 -176.9(16) . . . . ? C22 C26 C25 N4 0.0 . . . . ? C26 C25 N4 C24 0.0 . . . . ? C25 N4 C24 C23 0.0 . . . . ? N4 C24 C23 C22 0.0 . . . . ? C26 C22 C23 C24 0.0 . . . . ? C18 C22 C23 C24 177.2(15) . . . . ? C27 C31 C30 N5 0.0 . . . . ? C31 C30 N5 C29 0.0 . . . . ? C30 N5 C29 C28 0.0 . . . . ? N5 C29 C28 C27 0.0 . . . . ? C29 C28 C27 C31 0.0 . . . . ? C29 C28 C27 C20 176.8(16) . . . . ? C30 C31 C27 C28 0.0 . . . . ? C30 C31 C27 C20 -177.1(14) . . . . ? C19 C20 C27 C28 147(2) . . . . ? C21 C20 C27 C28 -35(3) . . . . ? C19 C20 C27 C31 -36(3) . . . . ? C21 C20 C27 C31 142.0(18) . . . . ? C50 C51 C58 C62 -28(3) . . . . ? C52 C51 C58 C62 150.8(16) . . . . ? C50 C51 C58 C59 147(2) . . . . ? C52 C51 C58 C59 -33(2) . . . . ? C59 C58 C62 C61 0.0 . . . . ? C51 C58 C62 C61 175.8(17) . . . . ? C58 C62 C61 N10 0.0 . . . . ? C62 C61 N10 C60 0.0 . . . . ? C61 N10 C60 C59 0.0 . . . . ? N10 C60 C59 C58 0.0 . . . . ? C62 C58 C59 C60 0.0 . . . . ? C51 C58 C59 C60 -176.1(15) . . . . ? C50 C49 C53 C54 29(3) . . . . ? C48 C49 C53 C54 -152.1(16) . . . . ? C50 C49 C53 C57 -148.4(19) . . . . ? C48 C49 C53 C57 31(2) . . . . ? C57 C53 C54 C55 0.0 . . . . ? C49 C53 C54 C55 -177.3(15) . . . . ? C53 C54 C55 N9 0.0 . . . . ? C54 C55 N9 C56 0.0 . . . . ? C55 N9 C56 C57 0.0 . . . . ? N9 C56 C57 C53 0.0 . . . . ? C54 C53 C57 C56 0.0 . . . . ? C49 C53 C57 C56 177.3(14) . . . . ? C79 C80 C84 C85 27(3) . . . . ? C81 C80 C84 C85 -152.3(18) . . . . ? C79 C80 C84 C88 -154.4(17) . . . . ? C81 C80 C84 C88 27(3) . . . . ? C88 C84 C85 C86 0.0 . . . . ? C80 C84 C85 C86 178.8(14) . . . . ? C84 C85 C86 N14 0.0 . . . . ? C85 C86 N14 C87 0.0 . . . . ? C86 N14 C87 C88 0.0 . . . . ? N14 C87 C88 C84 0.0 . . . . ? C85 C84 C88 C87 0.0 . . . . ? C80 C84 C88 C87 -178.8(14) . . . . ? C89 C93 C92 N15 10(3) . . . . ? C89 C90 C91 N15 -5(6) . . . . ? C115 C116 C117 N19 2(4) . . . . ? N19 C118 C119 C115 4(4) . . . . ? C141 C142 C146 C147 29(3) . . . . ? C143 C142 C146 C147 -147.5(18) . . . . ? C141 C142 C146 C150 -152.4(18) . . . . ? C143 C142 C146 C150 31(3) . . . . ? C150 C146 C147 C148 0.0 . . . . ? C142 C146 C147 C148 178.4(14) . . . . ? C146 C147 C148 N24 0.0 . . . . ? C147 C148 N24 C149 0.0 . . . . ? C148 N24 C149 C150 0.0 . . . . ? N24 C149 C150 C146 0.0 . . . . ? C147 C146 C150 C149 0.0 . . . . ? C142 C146 C150 C149 -178.5(14) . . . . ? C169 C168 C172 C176 -30(3) . . . . ? C167 C168 C172 C176 161.3(17) . . . . ? C169 C168 C172 C173 159.6(17) . . . . ? C167 C168 C172 C173 -9(3) . . . . ? C173 C172 C176 C175 0.0 . . . . ? C168 C172 C176 C175 -170.9(17) . . . . ? C172 C176 C175 N29 0.0 . . . . ? C176 C175 N29 C174 0.0 . . . . ? C175 N29 C174 C173 0.0 . . . . ? N29 C174 C173 C172 0.0 . . . . ? C176 C172 C173 C174 0.0 . . . . ? C168 C172 C173 C174 170.6(18) . . . . ? C92 C93 C89 C90 -8(3) . . . . ? C92 C93 C89 C82 177(2) . . . . ? C91 C90 C89 C93 5(4) . . . . ? C91 C90 C89 C82 -180(3) . . . . ? C81 C82 C89 C93 180(2) . . . . ? C83 C82 C89 C93 -4(3) . . . . ? C81 C82 C89 C90 5(3) . . . . ? C83 C82 C89 C90 -178(2) . . . . ? C118 C119 C115 C116 -1(3) . . . . ? C118 C119 C115 C111 -177(2) . . . . ? C117 C116 C115 C119 -1(3) . . . . ? C117 C116 C115 C111 175(2) . . . . ? C112 C111 C115 C119 31(4) . . . . ? C110 C111 C115 C119 -150(2) . . . . ? C112 C111 C115 C116 -145(2) . . . . ? C110 C111 C115 C116 35(4) . . . . ? C114 C113 C10B C14B -25(3) . . . . ? C112 C113 C10B C14B 141(2) . . . . ? C10A C113 C10B C14B -144(4) . . . . ? C114 C113 C10B C11B 141(2) . . . . ? C112 C113 C10B C11B -53(3) . . . . ? C10A C113 C10B C11B 22(2) . . . . ? C11B C10B C14B C13B 0.0 . . . . ? C113 C10B C14B C13B 165(3) . . . . ? C11B C10B C14B C13B -175(6) . . . 2_675 ? C113 C10B C14B C13B -10(6) . . . 2_675 ? C10B C14B C13B N20B 0.0 . . . . ? C13B C14B C13B N20B 177(4) 2_675 . . . ? C10B C14B C13B C14B -177(4) . . . 2_675 ? C13B C14B C13B C14B 0.0(14) 2_675 . . 2_675 ? C14B C13B N20B C12B 0.0 . . . . ? C14B C13B N20B C12B 173(9) 2_675 . . . ? C13B N20B C12B C11B 0.0 . . . . ? N20B C12B C11B C10B 0.0 . . . . ? C14B C10B C11B C12B 0.0 . . . . ? C113 C10B C11B C12B -167(3) . . . . ? C114 C113 C10A C14A 29(4) . . . . ? C112 C113 C10A C14A -133(2) . . . . ? C10B C113 C10A C14A 105(3) . . . . ? C114 C113 C10A C11A -138(2) . . . . ? C112 C113 C10A C11A 60(2) . . . . ? C10B C113 C10A C11A -62(3) . . . . ? C11A C10A C14A C13A 0.0 . . . . ? C113 C10A C14A C13A -166(2) . . . . ? C10A C14A C13A N20A 0.0 . . . . ? C14A C13A N20A C12A 0.0 . . . . ? C13A N20A C12A C11A 0.0 . . . . ? N20A C12A C11A C10A 0.0 . . . . ? C14A C10A C11A C12A 0.0 . . . . ? C113 C10A C11A C12A 168.1(19) . . . . ? C145 C144 C16B C17B 139(2) . . . . ? C143 C144 C16B C17B -53(3) . . . . ? C16A C144 C16B C17B 16(3) . . . . ? C145 C144 C16B C15B -38(3) . . . . ? C143 C144 C16B C15B 130(2) . . . . ? C16A C144 C16B C15B -162(5) . . . . ? C15B C16B C17B C18B 0.0 . . . . ? C144 C16B C17B C18B -177(2) . . . . ? C16B C17B C18B N25B 0.0 . . . . ? C17B C18B N25B C19B 0.0 . . . . ? C18B N25B C19B C15B 0.0 . . . . ? N25B C19B C15B C16B 0.0 . . . . ? C17B C16B C15B C19B 0.0 . . . . ? C144 C16B C15B C19B 177(3) . . . . ? C145 C144 C16A C15A 40(3) . . . . ? C143 C144 C16A C15A -130(2) . . . . ? C16B C144 C16A C15A 106(5) . . . . ? C145 C144 C16A C17A -136(2) . . . . ? C143 C144 C16A C17A 54(3) . . . . ? C16B C144 C16A C17A -70(4) . . . . ? C17A C16A C15A C19A 0.0 . . . . ? C144 C16A C15A C19A -177(2) . . . . ? C16A C15A C19A N25A 0.0 . . . . ? C15A C19A N25A C18A 0.0 . . . . ? C19A N25A C18A C17A 0.0 . . . . ? N25A C18A C17A C16A 0.0 . . . . ? C15A C16A C17A C18A 0.0 . . . . ? C144 C16A C17A C18A 177(2) . . . . ? C169 C170 C177 C181 23(3) . . . . ? C171 C170 C177 C181 -152.8(16) . . . . ? C169 C170 C177 C178 -150(2) . . . . ? C171 C170 C177 C178 34(3) . . . . ? C178 C177 C181 C180 0.0 . . . . ? C170 C177 C181 C180 -173.7(18) . . . . ? C177 C181 C180 N30 0.0 . . . . ? C181 C180 N30 C179 0.0 . . . . ? C180 N30 C179 C178 0.0 . . . . ? N30 C179 C178 C177 0.0 . . . . ? C181 C177 C178 C179 0.0 . . . . ? C170 C177 C178 C179 173.3(19) . . . . ? C5 C1 N1 C2 -2(3) . . . . ? C6 C1 N1 C2 177.7(19) . . . . ? C5 C1 N1 Ru1 -178.4(17) . . . . ? C6 C1 N1 Ru1 2(2) . . . . ? C3 C2 N1 C1 5(3) . . . . ? C3 C2 N1 Ru1 -179.4(16) . . . . ? C1 C6 N2 C7 178.3(19) . . . . ? C10 C6 N2 C7 -5(3) . . . . ? C1 C6 N2 Ru1 -11(2) . . . . ? C10 C6 N2 Ru1 165.7(13) . . . . ? C8 C7 N2 C6 0(3) . . . . ? C11 C7 N2 C6 178.1(17) . . . . ? C8 C7 N2 Ru1 -171.0(13) . . . . ? C11 C7 N2 Ru1 7(2) . . . . ? C13 C12 N3 C11 5(4) . . . . ? C13 C12 N3 Ru1 175.3(19) . . . . ? C15 C11 N3 C12 -5(3) . . . . ? C7 C11 N3 C12 -179.8(18) . . . . ? C15 C11 N3 Ru1 -176.4(15) . . . . ? C7 C11 N3 Ru1 9(2) . . . . ? C34 C33 N6 C32 -7(3) . . . . ? C34 C33 N6 Ru1 174.1(15) . . . . ? C36 C32 N6 C33 3(3) . . . . ? C37 C32 N6 C33 -177.9(19) . . . . ? C36 C32 N6 Ru1 -177.4(16) . . . . ? C37 C32 N6 Ru1 1(2) . . . . ? C39 C38 N7 C37 6(3) . . . . ? C42 C38 N7 C37 178.6(19) . . . . ? C39 C38 N7 Ru1 -167.9(16) . . . . ? C42 C38 N7 Ru1 5(2) . . . . ? C41 C37 N7 C38 -1(3) . . . . ? C32 C37 N7 C38 177.2(19) . . . . ? C41 C37 N7 Ru1 172.6(15) . . . . ? C32 C37 N7 Ru1 -9(2) . . . . ? C46 C42 N8 C43 2(3) . . . . ? C38 C42 N8 C43 178.8(19) . . . . ? C46 C42 N8 Ru1 -167.1(18) . . . . ? C38 C42 N8 Ru1 9(3) . . . . ? C44 C43 N8 C42 -3(3) . . . . ? C44 C43 N8 Ru1 165.5(17) . . . . ? C96 C95 N16 C94 -4(4) . . . . ? C96 C95 N16 Ru2 176(2) . . . . ? C98 C94 N16 C95 0(3) . . . . ? C99 C94 N16 C95 -177(2) . . . . ? C98 C94 N16 Ru2 179.4(19) . . . . ? C99 C94 N16 Ru2 2(2) . . . . ? C103 C99 N17 C100 -7(3) . . . . ? C94 C99 N17 C100 178.5(17) . . . . ? C103 C99 N17 Ru2 171.1(17) . . . . ? C94 C99 N17 Ru2 -4(2) . . . . ? C104 C100 N17 C99 -179.8(19) . . . . ? C101 C100 N17 C99 3(3) . . . . ? C104 C100 N17 Ru2 2(2) . . . . ? C101 C100 N17 Ru2 -174.3(12) . . . . ? C106 C105 N18 C104 -3(3) . . . . ? C106 C105 N18 Ru2 174.7(14) . . . . ? C108 C104 N18 C105 4(3) . . . . ? C100 C104 N18 C105 179.9(17) . . . . ? C108 C104 N18 Ru2 -173.7(16) . . . . ? C100 C104 N18 Ru2 2(2) . . . . ? C65 C64 N11 C63 -4(3) . . . . ? C65 C64 N11 Ru2 174.8(16) . . . . ? C67 C63 N11 C64 3(3) . . . . ? C68 C63 N11 C64 -173.7(19) . . . . ? C67 C63 N11 Ru2 -176.5(19) . . . . ? C68 C63 N11 Ru2 7(2) . . . . ? C70 C69 N12 C68 -4(3) . . . . ? C73 C69 N12 C68 177.2(18) . . . . ? C70 C69 N12 Ru2 179.2(14) . . . . ? C73 C69 N12 Ru2 1(3) . . . . ? C72 C68 N12 C69 9(3) . . . . ? C63 C68 N12 C69 -174.7(19) . . . . ? C72 C68 N12 Ru2 -174.6(16) . . . . ? C63 C68 N12 Ru2 2(2) . . . . ? C75 C74 N13 C73 2(4) . . . . ? C75 C74 N13 Ru2 -175.0(18) . . . . ? C77 C73 N13 C74 -7(4) . . . . ? C69 C73 N13 C74 -175.3(19) . . . . ? C77 C73 N13 Ru2 171(2) . . . . ? C69 C73 N13 Ru2 2(3) . . . . ? C134 C130 N22 C131 -2(3) . . . . ? C125 C130 N22 C131 176.0(17) . . . . ? C134 C130 N22 Ru3 168.2(15) . . . . ? C125 C130 N22 Ru3 -14(2) . . . . ? C132 C131 N22 C130 2(3) . . . . ? C135 C131 N22 C130 175.2(18) . . . . ? C132 C131 N22 Ru3 -168.3(16) . . . . ? C135 C131 N22 Ru3 5(2) . . . . ? C139 C135 N23 C136 3(4) . . . . ? C131 C135 N23 C136 -175.6(19) . . . . ? C139 C135 N23 Ru3 -177.4(18) . . . . ? C131 C135 N23 Ru3 4(3) . . . . ? C137 C136 N23 C135 -2(3) . . . . ? C137 C136 N23 Ru3 178.4(16) . . . . ? C158 C157 N27 C156 -1(3) . . . . ? C161 C157 N27 C156 -177.6(17) . . . . ? C158 C157 N27 Ru3 171.5(15) . . . . ? C161 C157 N27 Ru3 -5(2) . . . . ? C160 C156 N27 C157 -5(3) . . . . ? C151 C156 N27 C157 179.8(18) . . . . ? C160 C156 N27 Ru3 -177.1(14) . . . . ? C151 C156 N27 Ru3 8(2) . . . . ? C153 C152 N26 C151 3(3) . . . . ? C153 C152 N26 Ru3 175.9(18) . . . . ? C155 C151 N26 C152 -2(3) . . . . ? C156 C151 N26 C152 178.8(18) . . . . ? C155 C151 N26 Ru3 -175.7(15) . . . . ? C156 C151 N26 Ru3 5(2) . . . . ? C157 C161 N28 C162 -179.9(19) . . . . ? C165 C161 N28 C162 -3(3) . . . . ? C157 C161 N28 Ru3 4(2) . . . . ? C165 C161 N28 Ru3 -179.1(14) . . . . ? C163 C162 N28 C161 4(3) . . . . ? C163 C162 N28 Ru3 178.8(18) . . . . ? C90 C91 N15 C92 6(6) . . . . ? C93 C92 N15 C91 -9(4) . . . . ? C119 C118 N19 C117 -3(3) . . . . ? C116 C117 N19 C118 0(3) . . . . ? P5B P2C P3A P8B -133(5) . . . . ? P8B P2C P3A P5B 133(5) . . . . ? P4D P2A P4A P4B -144(8) . . . . ? P4B P2A P4A P4D 144(8) . . . . ? P4D P4A P4B P2A -90(13) . . . . ? P2A P4A P4B P4D 90(13) . . . . ? P4D P2A P4B P4A 21(4) . . . . ? P4A P2A P4B P4D -21(4) . . . . ? P4B P4A P4D P2A 78(13) . . . . ? P2A P4A P4D P4B -78(13) . . . . ? P4B P2A P4D P4A -28(6) . . . . ? P4A P2A P4D P4B 28(6) . . . . ? P9A P2B P5A P6D -152(6) . . . . ? P5D P2B P5A P6D -137(8) . . . . ? P6D P2B P5A P9A 152(6) . . . . ? P5D P2B P5A P9A 14(9) . . . . ? P6D P2B P5A P5D 137(8) . . . . ? P9A P2B P5A P5D -14(9) . . . . ? P8B P2C P5B P3A -55(6) . . . . ? P3A P2C P5B P8B 55(6) . . . . ? P8B P3A P5B P2C 38(4) . . . . ? P2C P3A P5B P8B -38(4) . . . . ? P2B P5A P5D P9A 16(9) . . . . ? P6D P5A P5D P9A 126(10) . . . . ? P6D P5A P5D P2B 110(11) . . . . ? P9A P5A P5D P2B -16(9) . . . . ? P2B P5A P5D P6D -110(11) . . . . ? P9A P5A P5D P6D -126(10) . . . . ? P9A P5A P6D P2B -41(9) . . . . ? P5D P5A P6D P2B -135(9) . . . . ? P2B P5A P6D P9A 41(9) . . . . ? P5D P5A P6D P9A -94(11) . . . . ? P2B P5A P6D P5D 135(9) . . . . ? P9A P5A P6D P5D 94(11) . . . . ? P9A P2B P6D P5A 23(5) . . . . ? P5D P2B P6D P5A 16(3) . . . . ? P5A P2B P6D P9A -23(5) . . . . ? P5D P2B P6D P9A -7(5) . . . . ? P5A P2B P6D P5D -16(3) . . . . ? P9A P2B P6D P5D 7(5) . . . . ? P5B P2C P8B P3A 73(7) . . . . ? P3A P2C P8B P5B -73(7) . . . . ? P5B P3A P8B P2C -29(3) . . . . ? P2C P3A P8B P5B 29(3) . . . . ? P2B P5D P9A P5A 10(6) . . . . ? P6D P5D P9A P5A 18(3) . . . . ? P5A P5D P9A P2B -10(6) . . . . ? P6D P5D P9A P2B 8(6) . . . . ? P5A P5D P9A P6D -18(3) . . . . ? P2B P5D P9A P6D -8(6) . . . . ? P2B P5A P9A P5D -168(7) . . . . ? P6D P5A P9A P5D -129(9) . . . . ? P6D P5A P9A P2B 39(8) . . . . ? P5D P5A P9A P2B 168(7) . . . . ? P2B P5A P9A P6D -39(8) . . . . ? P5D P5A P9A P6D 129(9) . . . . ? P5A P2B P9A P5D 11(7) . . . . ? P6D P2B P9A P5D -13(10) . . . . ? P6D P2B P9A P5A -24(5) . . . . ? P5D P2B P9A P5A -11(7) . . . . ? P5A P2B P9A P6D 24(5) . . . . ? P5D P2B P9A P6D 13(10) . . . . ? N23 C136 C137 C138 2(3) . . . . ? C135 C139 C138 C137 4(3) . . . . ? C136 C137 C138 C139 -4(3) . . . . ? _refine_diff_density_max 1.105 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.158 _shelxl_version_number 2013-4 _database_code_depnum_ccdc_archive 'CCDC 948465'