# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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 _database_code_depnum_ccdc_archive 'CCDC 892890' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H60 Co3 N12 O19' _chemical_formula_sum 'C78 H60 Co3 N12 O19' _chemical_formula_weight 1646.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 37.985(7) _cell_length_b 14.570(3) _cell_length_c 27.895(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15438(5) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 32448 _cell_measurement_theta_min 2.0904 _cell_measurement_theta_max 27.6413 _exptl_crystal_description Prism _exptl_crystal_colour 'blue violet' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6760 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.716 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83559 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13550 _reflns_number_gt 12552 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1900P)^2^+47.3920P] 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 13550 _refine_ls_number_parameters 1043 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.2843 _refine_ls_wR_factor_gt 0.2765 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.084 _refine_ls_shift/su_mean 0.003 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 Co3 Co 0.087331(17) 0.85706(4) 0.44861(2) 0.0303(2) Uani 1 1 d . . . Co2 Co 0.09382(2) 0.63495(5) 0.56926(3) 0.0398(2) Uani 1 1 d . . . Co1 Co 0.182416(18) 0.24970(4) 0.50603(3) 0.0312(2) Uani 1 1 d . . . O5 O 0.10890(9) 0.7317(2) 0.44946(14) 0.0384(8) Uani 1 1 d . . . O1 O 0.16554(11) 0.3122(2) 0.44675(13) 0.0423(9) Uani 1 1 d . . . O2 O 0.13318(10) 0.3832(2) 0.50125(13) 0.0396(8) Uani 1 1 d . . . O4 O 0.14626(9) 0.5808(2) 0.51179(13) 0.0352(8) Uani 1 1 d . . . O9 O 0.08801(8) 0.9224(2) 0.51178(13) 0.0348(8) Uani 1 1 d . . . O12 O 0.16345(10) 1.1850(2) 0.56297(13) 0.0387(8) Uani 1 1 d . . . O10 O 0.14528(9) 0.9129(2) 0.49591(12) 0.0338(8) Uani 1 1 d . . . O3 O 0.08849(9) 0.5689(2) 0.50498(14) 0.0391(8) Uani 1 1 d . . . O7 O 0.11515(10) 0.7588(2) 0.55914(14) 0.0412(9) Uani 1 1 d . . . O6 O 0.08390(11) 0.7359(3) 0.37761(16) 0.0505(10) Uani 1 1 d . . . O11 O 0.12775(12) 1.1131(2) 0.51242(12) 0.0436(9) Uani 1 1 d . . . O8 O 0.10148(16) 0.7440(3) 0.63562(16) 0.0682(15) Uani 1 1 d . . . N3 N 0.28658(11) 0.3504(3) 0.97760(15) 0.0311(9) Uani 1 1 d . . . N4 N 0.26880(11) 0.4852(3) 0.95128(14) 0.0319(9) Uani 1 1 d . . . N1 N 0.21406(11) 0.3478(3) 0.53572(15) 0.0318(9) Uani 1 1 d . . . N9 N 0.10373(12) 0.9456(3) 0.39689(16) 0.0383(10) Uani 1 1 d . . . N5 N 0.03365(12) 0.8536(3) 0.44538(18) 0.0411(11) Uani 1 1 d . . . N2 N 0.23113(12) 0.4827(3) 0.56241(14) 0.0356(9) Uani 1 1 d . . . N11 N 0.39143(12) 0.9600(3) 0.11903(17) 0.0411(10) Uani 1 1 d . . . N7 N 0.04122(14) 1.3494(3) 0.07875(19) 0.0500(12) Uani 1 1 d . . . N10 N 0.12292(12) 1.0730(3) 0.36309(18) 0.0422(10) Uani 1 1 d . . . N12 N 0.37688(13) 1.0908(3) 0.1532(2) 0.0482(12) Uani 1 1 d . . . N6 N -0.02079(13) 0.8542(4) 0.4193(2) 0.0550(14) Uani 1 1 d . . . N8 N -0.01298(15) 1.3515(5) 0.1068(2) 0.0711(18) Uani 1 1 d . . . C70 C -0.0588(2) 1.2297(6) 0.2548(3) 0.081(2) Uani 1 1 d . . . H52 H -0.0672 1.2423 0.2862 0.097 Uiso 1 1 calc R . . C55 C 0.36313(17) 1.1871(4) 0.1630(2) 0.0556(11) Uani 1 1 d . . . H39 H 0.3588 1.2187 0.1322 0.067 Uiso 1 1 calc R . . H38 H 0.3813 1.2223 0.1807 0.067 Uiso 1 1 calc R . . C71 C -0.03724(18) 1.1223(6) 0.1960(3) 0.072(2) Uani 1 1 d . . . H53 H -0.0306 1.0621 0.1865 0.087 Uiso 1 1 calc R . . C73 C -0.0359(2) 1.1939(7) 0.1631(3) 0.083(3) Uani 1 1 d . . . H55 H -0.0291 1.1807 0.1311 0.100 Uiso 1 1 calc R . . C72 C -0.0570(2) 1.3004(7) 0.2216(3) 0.086(3) Uani 1 1 d . . . H54 H -0.0647 1.3601 0.2305 0.103 Uiso 1 1 calc R . . C33 C 0.12032(12) 0.9283(3) 0.52382(17) 0.0298(10) Uani 1 1 d . . . C32 C 0.12856(11) 0.9532(3) 0.57519(16) 0.0272(9) Uani 1 1 d . . . C18 C 0.29531(13) 0.4394(3) 0.97114(16) 0.0286(9) Uani 1 1 d . . . H16 H 0.3173 0.4656 0.9796 0.034 Uiso 1 1 calc R . . C24 C 0.11954(12) 0.5638(3) 0.48802(18) 0.0299(10) Uani 1 1 d . . . C1 C 0.20485(13) 0.4356(3) 0.54186(16) 0.0299(10) Uani 1 1 d . . . H1 H 0.1828 0.4610 0.5329 0.036 Uiso 1 1 calc R . . C34 C 0.13988(12) 1.0428(3) 0.58818(17) 0.0283(9) Uani 1 1 d . . . C35 C 0.14311(13) 1.1175(3) 0.55132(18) 0.0323(11) Uani 1 1 d . . . C20 C 0.24148(13) 0.4248(4) 0.94376(18) 0.0349(11) Uani 1 1 d . . . H17 H 0.2192 0.4384 0.9301 0.042 Uiso 1 1 calc R . . C22 C 0.13628(14) 0.4487(3) 0.42277(18) 0.0352(11) Uani 1 1 d . . . C23 C 0.12364(13) 0.5367(3) 0.43558(18) 0.0326(10) Uani 1 1 d . . . C2 C 0.24806(14) 0.3398(3) 0.5534(2) 0.0394(12) Uani 1 1 d . . . H2 H 0.2616 0.2849 0.5540 0.047 Uiso 1 1 calc R . . C19 C 0.25272(13) 0.3424(3) 0.9597(2) 0.0367(11) Uani 1 1 d . . . H18 H 0.2394 0.2872 0.9588 0.044 Uiso 1 1 calc R . . C21 C 0.14526(14) 0.3777(3) 0.45987(19) 0.0338(11) Uani 1 1 d . . . C10 C 0.24480(16) 0.5890(4) 0.7300(2) 0.0472(13) Uani 1 1 d . . . C15 C 0.23198(17) 0.6104(4) 0.8647(2) 0.0513(14) Uani 1 1 d . . . H13 H 0.2133 0.6229 0.8864 0.062 Uiso 1 1 calc R . . C30 C 0.11341(16) 0.7905(4) 0.6016(2) 0.0424(12) Uani 1 1 d . . . C76 C 0.02047(16) 1.3691(4) 0.1151(2) 0.0508(15) Uani 1 1 d . . . H58 H 0.0288 1.3937 0.1445 0.061 Uiso 1 1 calc R . . C26 C 0.10147(14) 0.6954(4) 0.4097(2) 0.0389(12) Uani 1 1 d . . . C47 C 0.20000(17) 1.1945(4) 0.2514(2) 0.0523(14) Uani 1 1 d . . . H33 H 0.1995 1.2103 0.2184 0.063 Uiso 1 1 calc R . . C36 C 0.14801(16) 1.0621(4) 0.6359(2) 0.0446(13) Uani 1 1 d . . . H24 H 0.1552 1.1224 0.6444 0.054 Uiso 1 1 calc R . . C3 C 0.25891(15) 0.4227(4) 0.56960(18) 0.0394(12) Uani 1 1 d . . . H3 H 0.2812 0.4368 0.5832 0.047 Uiso 1 1 calc R . . C39 C 0.11575(13) 1.0300(3) 0.4048(2) 0.0379(11) Uani 1 1 d . . . H25 H 0.1189 1.0564 0.4357 0.045 Uiso 1 1 calc R . . C54 C 0.32849(18) 1.1860(4) 0.1927(2) 0.0556(11) Uani 1 1 d . . . C31 C 0.12619(15) 0.8861(3) 0.61140(19) 0.0383(11) Uani 1 1 d . . . C6 C 0.26461(17) 0.6113(4) 0.6494(2) 0.0498(14) Uani 1 1 d . . . H6 H 0.2833 0.6262 0.6282 0.060 Uiso 1 1 calc R . . C11 C 0.25199(16) 0.5897(4) 0.7831(2) 0.0491(14) Uani 1 1 d . . . C56 C 0.38042(13) 1.0452(4) 0.1120(2) 0.0454(14) Uani 1 1 d . . . H41 H 0.3756 1.0708 0.0813 0.055 Uiso 1 1 calc R . . C43 C 0.1677(2) 1.1737(4) 0.3257(2) 0.0563(17) Uani 1 1 d . . . C38 C 0.13442(18) 0.9075(4) 0.6588(2) 0.0512(15) Uani 1 1 d . . . H22 H 0.1322 0.8617 0.6829 0.061 Uiso 1 1 calc R . . C25 C 0.11492(15) 0.5999(4) 0.3994(2) 0.0402(12) Uani 1 1 d . . . C5 C 0.23122(15) 0.5900(4) 0.6297(2) 0.0464(14) Uani 1 1 d . . . C59 C 0.01270(14) 0.8329(4) 0.4099(2) 0.0489(14) Uani 1 1 d . . . H43 H 0.0204 0.8057 0.3807 0.059 Uiso 1 1 calc R . . C50 C 0.29718(18) 1.1977(4) 0.2665(2) 0.0546(15) Uani 1 1 d . . . H34 H 0.2975 1.2110 0.2999 0.066 Uiso 1 1 calc R . . C4 C 0.22881(19) 0.5797(4) 0.5762(2) 0.0513(16) Uani 1 1 d . . . H4 H 0.2062 0.6056 0.5648 0.062 Uiso 1 1 calc R . . H5 H 0.2482 0.6144 0.5608 0.062 Uiso 1 1 calc R . . C58 C 0.39545(17) 0.9526(4) 0.1675(2) 0.0494(14) Uani 1 1 d . . . H42 H 0.4030 0.8990 0.1840 0.059 Uiso 1 1 calc R . . C7 C 0.20515(16) 0.5690(4) 0.6627(2) 0.0507(14) Uani 1 1 d . . . H7 H 0.1822 0.5544 0.6516 0.061 Uiso 1 1 calc R . . C17 C 0.26953(17) 0.5832(3) 0.93732(19) 0.0430(13) Uani 1 1 d . . . H14 H 0.2919 0.6113 0.9481 0.052 Uiso 1 1 calc R . . H15 H 0.2499 0.6161 0.9531 0.052 Uiso 1 1 calc R . . C13 C 0.22544(16) 0.6100(4) 0.8160(2) 0.0493(14) Uani 1 1 d . . . H11 H 0.2024 0.6238 0.8047 0.059 Uiso 1 1 calc R . . C9 C 0.21202(18) 0.5689(5) 0.7128(2) 0.0572(16) Uani 1 1 d . . . H9 H 0.1936 0.5547 0.7345 0.069 Uiso 1 1 calc R . . C48 C 0.23162(18) 1.1726(5) 0.2718(2) 0.0533(15) Uani 1 1 d . . . C41 C 0.11505(18) 1.0148(4) 0.3265(2) 0.0512(15) Uani 1 1 d . . . H27 H 0.1171 1.0265 0.2931 0.061 Uiso 1 1 calc R . . C45 C 0.16910(18) 1.1947(4) 0.2763(2) 0.0529(15) Uani 1 1 d . . . H31 H 0.1479 1.2095 0.2599 0.063 Uiso 1 1 calc R . . C8 C 0.27108(17) 0.6114(4) 0.6977(2) 0.0496(14) Uani 1 1 d . . . H8 H 0.2939 0.6271 0.7091 0.060 Uiso 1 1 calc R . . C49 C 0.26540(19) 1.1738(5) 0.2443(2) 0.0540(15) Uani 1 1 d . . . C51 C 0.26628(19) 1.1565(5) 0.1949(2) 0.0587(16) Uani 1 1 d . . . H35 H 0.2451 1.1413 0.1787 0.070 Uiso 1 1 calc R . . C40 C 0.10371(19) 0.9367(4) 0.3477(2) 0.0533(16) Uani 1 1 d . . . H26 H 0.0967 0.8830 0.3309 0.064 Uiso 1 1 calc R . . C37 C 0.1458(2) 0.9948(4) 0.6713(2) 0.0581(17) Uani 1 1 d . . . H23 H 0.1520 1.0086 0.7035 0.070 Uiso 1 1 calc R . . C53 C 0.29734(19) 1.1611(5) 0.1692(2) 0.0579(16) Uani 1 1 d . . . H37 H 0.2975 1.1475 0.1359 0.069 Uiso 1 1 calc R . . C52 C 0.32793(19) 1.2019(4) 0.2404(2) 0.0549(15) Uani 1 1 d . . . H36 H 0.3493 1.2165 0.2564 0.066 Uiso 1 1 calc R . . C12 C 0.28563(16) 0.5741(5) 0.8014(2) 0.0570(16) Uani 1 1 d . . . H10 H 0.3046 0.5634 0.7799 0.068 Uiso 1 1 calc R . . C29 C 0.14089(18) 0.4262(4) 0.3745(2) 0.0517(15) Uani 1 1 d . . . H19 H 0.1503 0.3680 0.3660 0.062 Uiso 1 1 calc R . . C16 C 0.26619(18) 0.5922(4) 0.8830(2) 0.0548(16) Uani 1 1 d . . . C28 C 0.1318(2) 0.4882(4) 0.3390(2) 0.0618(18) Uani 1 1 d . . . H20 H 0.1341 0.4715 0.3062 0.074 Uiso 1 1 calc R . . C60 C 0.01127(15) 0.8920(5) 0.4799(2) 0.0556(15) Uani 1 1 d . . . H44 H 0.0185 0.9139 0.5104 0.067 Uiso 1 1 calc R . . C68 C -0.04868(15) 1.0638(5) 0.2793(3) 0.0619(18) Uani 1 1 d . . . C57 C 0.38699(18) 1.0339(4) 0.1886(3) 0.0554(16) Uani 1 1 d . . . H40 H 0.3880 1.0477 0.2218 0.066 Uiso 1 1 calc R . . C44 C 0.2006(2) 1.1514(5) 0.3465(3) 0.0667(19) Uani 1 1 d . . . H30 H 0.2013 1.1357 0.3796 0.080 Uiso 1 1 calc R . . C66 C -0.04822(19) 1.0830(6) 0.3284(3) 0.0697(19) Uani 1 1 d . . . H50 H -0.0477 1.1451 0.3388 0.084 Uiso 1 1 calc R . . C42 C 0.13543(16) 1.1695(4) 0.3560(3) 0.0590(18) Uani 1 1 d . . . H29 H 0.1165 1.2058 0.3406 0.071 Uiso 1 1 calc R . . H28 H 0.1405 1.1974 0.3876 0.071 Uiso 1 1 calc R . . C63 C -0.04913(15) 0.9208(6) 0.3479(3) 0.0657(19) Uani 1 1 d . . . C46 C 0.2316(2) 1.1513(5) 0.3211(3) 0.0635(18) Uani 1 1 d . . . H32 H 0.2531 1.1369 0.3368 0.076 Uiso 1 1 calc R . . C67 C -0.0495(2) 0.9717(7) 0.2655(3) 0.078(2) Uani 1 1 d . . . H51 H -0.0497 0.9565 0.2324 0.094 Uiso 1 1 calc R . . C14 C 0.29196(19) 0.5737(5) 0.8500(2) 0.0576(16) Uani 1 1 d . . . H12 H 0.3150 0.5602 0.8611 0.069 Uiso 1 1 calc R . . C27 C 0.11938(19) 0.5747(4) 0.3511(2) 0.0553(16) Uani 1 1 d . . . H21 H 0.1138 0.6174 0.3264 0.066 Uiso 1 1 calc R . . C69 C -0.04828(16) 1.1387(6) 0.2430(3) 0.0621(19) Uani 1 1 d . . . C62 C -0.05038(17) 0.8457(6) 0.3846(3) 0.073(2) Uani 1 1 d . . . H47 H -0.0730 0.8487 0.4021 0.087 Uiso 1 1 calc R . . H46 H -0.0490 0.7854 0.3684 0.087 Uiso 1 1 calc R . . C78 C 0.0189(3) 1.3130(7) 0.0460(3) 0.095(3) Uani 1 1 d . . . H60 H 0.0256 1.2901 0.0155 0.114 Uiso 1 1 calc R . . C75 C -0.0423(2) 1.3632(7) 0.1405(3) 0.091(3) Uani 1 1 d . . . H57 H -0.0647 1.3668 0.1224 0.109 Uiso 1 1 calc R . . H56 H -0.0393 1.4215 0.1582 0.109 Uiso 1 1 calc R . . C65 C -0.04847(17) 1.0134(6) 0.3623(3) 0.069(2) Uani 1 1 d . . . H49 H -0.0482 1.0282 0.3955 0.083 Uiso 1 1 calc R . . C77 C -0.0142(2) 1.3143(9) 0.0635(3) 0.106(4) Uani 1 1 d . . . H59 H -0.0347 1.2924 0.0477 0.127 Uiso 1 1 calc R . . C61 C -0.02247(17) 0.8931(5) 0.4629(3) 0.0643(18) Uani 1 1 d . . . H45 H -0.0428 0.9165 0.4786 0.077 Uiso 1 1 calc R . . C64 C -0.0500(2) 0.9003(6) 0.3002(3) 0.077(2) Uani 1 1 d . . . H48 H -0.0509 0.8381 0.2902 0.093 Uiso 1 1 calc R . . C74 C -0.04431(17) 1.2857(6) 0.1754(3) 0.080(3) Uani 1 1 d . . . O18 O 0.18585(10) 0.7478(2) 0.50281(16) 0.0469(11) Uani 1 1 d . . . O17 O 0.07818(17) 0.2685(5) 0.5131(4) 0.083(3) Uani 0.848(17) 1 d P A 1 O19 O 0.4622(2) 1.0331(6) 0.2524(3) 0.124(3) Uani 1 1 d . . . O16 O 0.0429(2) 0.4155(7) 0.5506(4) 0.057(4) Uani 0.49(2) 1 d P B 1 O15 O 0.0307(3) 0.5486(8) 0.4357(5) 0.072(5) Uiso 0.53(3) 1 d P C 1 O14' O -0.0387(3) 0.6141(9) 0.3473(5) 0.057(5) Uani 0.44(3) 1 d P D 1 O13 O 0.0345(3) 0.6114(8) 0.3464(5) 0.101(5) Uani 0.580(14) 1 d P E 1 O14 O -0.0314(4) 0.6621(17) 0.3151(12) 0.162(14) Uani 0.56(3) 1 d P D 2 O13' O 0.0405(4) 0.7154(14) 0.2980(5) 0.106(7) Uani 0.420(14) 1 d P E 2 O16' O 0.0341(5) 0.3754(12) 0.5883(10) 0.155(11) Uani 0.51(2) 1 d P B 2 O15' O 0.0262(8) 0.521(2) 0.4651(15) 0.196(13) Uiso 0.47(3) 1 d P C 2 O17' O 0.0813(8) 0.227(3) 0.469(2) 0.082(19) Uani 0.152(17) 1 d P A 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 Co3 0.0322(4) 0.0218(4) 0.0369(4) 0.0005(2) -0.0105(3) 0.0023(2) Co2 0.0464(4) 0.0234(4) 0.0495(5) -0.0044(3) 0.0222(3) -0.0039(3) Co1 0.0334(4) 0.0188(4) 0.0415(4) -0.0025(2) 0.0037(3) 0.0003(2) O5 0.0380(19) 0.0274(17) 0.050(2) -0.0055(16) -0.0127(16) 0.0063(15) O1 0.057(2) 0.0253(18) 0.044(2) -0.0005(15) 0.0066(17) 0.0102(16) O2 0.055(2) 0.0230(17) 0.040(2) -0.0026(14) 0.0038(17) -0.0007(15) O4 0.0419(19) 0.0204(16) 0.0432(19) -0.0005(14) -0.0072(16) 0.0011(14) O9 0.0304(17) 0.0326(18) 0.041(2) -0.0039(15) -0.0029(14) 0.0002(14) O12 0.049(2) 0.0214(17) 0.046(2) -0.0010(14) 0.0019(16) -0.0037(15) O10 0.0412(19) 0.0219(16) 0.0383(18) 0.0024(13) 0.0115(15) 0.0000(14) O3 0.0327(18) 0.0341(19) 0.051(2) -0.0083(16) 0.0096(15) -0.0025(14) O7 0.051(2) 0.0264(18) 0.047(2) -0.0045(15) 0.0183(18) -0.0038(15) O6 0.061(3) 0.036(2) 0.055(3) 0.0000(18) -0.016(2) 0.0106(18) O11 0.081(3) 0.0220(17) 0.0275(18) -0.0001(14) -0.0088(18) 0.0006(17) O8 0.131(5) 0.033(2) 0.040(2) 0.0017(17) 0.022(3) -0.019(2) N3 0.033(2) 0.0220(19) 0.038(2) 0.0035(16) 0.0002(17) -0.0012(16) N4 0.046(2) 0.0205(19) 0.029(2) 0.0005(15) -0.0025(17) 0.0017(17) N1 0.038(2) 0.0210(19) 0.037(2) -0.0010(16) 0.0059(18) 0.0024(16) N9 0.048(2) 0.030(2) 0.037(2) -0.0027(18) -0.0119(19) -0.0025(18) N5 0.037(2) 0.032(2) 0.054(3) 0.0058(19) -0.009(2) 0.0008(18) N2 0.059(3) 0.020(2) 0.028(2) 0.0024(16) -0.0029(19) 0.0008(18) N11 0.039(2) 0.032(2) 0.052(3) 0.012(2) -0.010(2) -0.0023(18) N7 0.050(3) 0.046(3) 0.054(3) -0.008(2) 0.016(2) -0.016(2) N10 0.048(3) 0.027(2) 0.051(3) -0.0012(19) 0.008(2) -0.0016(19) N12 0.047(3) 0.034(2) 0.064(3) 0.004(2) -0.015(2) 0.004(2) N6 0.032(2) 0.066(4) 0.067(4) 0.007(3) -0.012(2) 0.003(2) N8 0.043(3) 0.115(5) 0.055(4) 0.012(3) 0.007(3) -0.017(3) C70 0.089(6) 0.093(6) 0.061(5) 0.011(4) 0.010(4) 0.003(5) C55 0.061(3) 0.046(2) 0.061(3) 0.004(2) -0.013(2) 0.004(2) C71 0.047(4) 0.099(6) 0.071(5) 0.020(4) 0.014(3) 0.012(4) C73 0.057(4) 0.127(8) 0.065(5) 0.021(5) 0.028(4) 0.016(5) C72 0.080(5) 0.104(7) 0.073(5) 0.018(5) 0.017(4) -0.004(5) C33 0.035(2) 0.017(2) 0.037(3) 0.0008(18) 0.000(2) -0.0003(18) C32 0.026(2) 0.023(2) 0.032(2) 0.0026(18) 0.0025(18) 0.0002(17) C18 0.038(2) 0.019(2) 0.029(2) 0.0023(17) -0.0038(19) -0.0015(18) C24 0.032(2) 0.020(2) 0.038(3) 0.0011(19) 0.006(2) 0.0030(18) C1 0.038(2) 0.024(2) 0.027(2) -0.0022(18) -0.0007(19) 0.0031(19) C34 0.030(2) 0.023(2) 0.033(2) 0.0010(18) -0.0012(18) -0.0007(17) C35 0.038(3) 0.017(2) 0.042(3) -0.0023(19) 0.006(2) 0.0017(19) C20 0.034(3) 0.035(3) 0.036(3) 0.008(2) -0.001(2) 0.003(2) C22 0.043(3) 0.027(2) 0.036(3) -0.003(2) 0.004(2) 0.006(2) C23 0.034(2) 0.024(2) 0.040(3) -0.004(2) 0.003(2) 0.0022(19) C2 0.035(3) 0.024(2) 0.058(3) -0.001(2) 0.004(2) 0.004(2) C19 0.034(3) 0.027(2) 0.049(3) 0.002(2) -0.001(2) -0.004(2) C21 0.043(3) 0.019(2) 0.039(3) -0.0066(19) 0.004(2) 0.001(2) C10 0.052(3) 0.042(3) 0.047(3) 0.002(3) 0.000(3) -0.001(3) C15 0.056(3) 0.053(4) 0.045(3) 0.012(3) 0.000(3) 0.014(3) C30 0.059(3) 0.027(3) 0.041(3) 0.002(2) 0.005(3) -0.002(2) C76 0.046(3) 0.056(4) 0.051(3) 0.013(3) 0.020(3) 0.008(3) C26 0.041(3) 0.031(3) 0.044(3) 0.000(2) -0.003(2) 0.003(2) C47 0.061(4) 0.041(3) 0.054(3) -0.004(3) -0.003(3) -0.006(3) C36 0.056(3) 0.029(3) 0.049(3) 0.003(2) -0.014(3) -0.008(2) C3 0.045(3) 0.038(3) 0.035(3) -0.001(2) -0.001(2) -0.009(2) C39 0.040(3) 0.030(3) 0.044(3) -0.013(2) -0.001(2) -0.002(2) C54 0.061(3) 0.046(2) 0.061(3) 0.004(2) -0.013(2) 0.004(2) C31 0.051(3) 0.027(2) 0.037(3) 0.004(2) 0.003(2) 0.001(2) C6 0.058(4) 0.049(3) 0.042(3) -0.003(3) 0.002(3) -0.006(3) C11 0.055(3) 0.047(3) 0.046(3) 0.003(3) 0.002(3) 0.003(3) C56 0.033(3) 0.036(3) 0.067(4) 0.026(3) -0.015(2) -0.005(2) C43 0.090(5) 0.044(3) 0.035(3) 0.005(2) -0.010(3) -0.023(3) C38 0.080(4) 0.039(3) 0.035(3) 0.011(2) -0.010(3) -0.003(3) C25 0.049(3) 0.029(3) 0.043(3) 0.001(2) 0.000(2) 0.002(2) C5 0.042(3) 0.044(3) 0.053(3) -0.021(3) 0.006(3) -0.007(2) C59 0.037(3) 0.059(4) 0.051(3) 0.003(3) -0.014(3) 0.006(3) C50 0.064(4) 0.054(4) 0.046(3) -0.002(3) -0.006(3) 0.010(3) C4 0.087(4) 0.025(3) 0.043(3) -0.005(2) -0.024(3) 0.010(3) C58 0.064(4) 0.034(3) 0.050(3) 0.006(2) -0.006(3) 0.012(3) C7 0.043(3) 0.050(3) 0.059(4) 0.002(3) -0.006(3) -0.003(3) C17 0.071(4) 0.024(3) 0.035(3) 0.007(2) -0.013(3) 0.001(2) C13 0.048(3) 0.051(3) 0.049(3) 0.005(3) -0.004(3) 0.004(3) C9 0.057(4) 0.064(4) 0.051(3) -0.004(3) 0.005(3) -0.001(3) C48 0.063(4) 0.050(4) 0.047(3) -0.002(3) 0.004(3) -0.003(3) C41 0.077(4) 0.041(3) 0.036(3) -0.002(2) 0.001(3) -0.005(3) C45 0.058(4) 0.050(3) 0.051(3) -0.005(3) -0.004(3) -0.004(3) C8 0.052(3) 0.056(4) 0.041(3) -0.006(3) -0.005(3) -0.001(3) C49 0.067(4) 0.052(4) 0.043(3) -0.002(3) -0.002(3) -0.002(3) C51 0.063(4) 0.061(4) 0.053(4) -0.003(3) 0.000(3) -0.001(3) C40 0.086(5) 0.036(3) 0.038(3) -0.003(2) -0.014(3) -0.013(3) C37 0.094(5) 0.046(3) 0.035(3) 0.007(3) -0.020(3) -0.011(3) C53 0.072(4) 0.059(4) 0.042(3) -0.006(3) 0.004(3) 0.007(3) C52 0.067(4) 0.055(4) 0.043(3) 0.000(3) -0.005(3) 0.007(3) C12 0.041(3) 0.085(5) 0.046(3) 0.014(3) 0.004(3) 0.009(3) C29 0.069(4) 0.035(3) 0.050(3) -0.002(3) 0.010(3) 0.012(3) C16 0.065(4) 0.042(3) 0.057(4) 0.019(3) 0.018(3) 0.023(3) C28 0.099(5) 0.048(4) 0.039(3) 0.002(3) 0.007(3) 0.020(3) C60 0.040(3) 0.071(4) 0.056(4) -0.002(3) 0.000(3) 0.006(3) C68 0.033(3) 0.082(5) 0.070(4) 0.018(4) -0.009(3) 0.002(3) C57 0.065(4) 0.038(3) 0.063(4) 0.002(3) -0.016(3) 0.015(3) C44 0.067(4) 0.071(5) 0.062(4) 0.007(4) 0.002(4) 0.004(4) C66 0.058(4) 0.088(5) 0.064(4) 0.007(4) 0.005(3) 0.000(4) C42 0.048(3) 0.029(3) 0.100(5) -0.003(3) 0.011(3) -0.001(2) C63 0.027(3) 0.090(5) 0.081(5) 0.006(4) -0.013(3) -0.001(3) C46 0.072(5) 0.064(4) 0.054(4) 0.003(3) 0.000(3) 0.012(3) C67 0.067(5) 0.108(7) 0.060(4) 0.005(4) -0.014(4) 0.021(4) C14 0.065(4) 0.062(4) 0.046(3) 0.005(3) -0.003(3) 0.012(3) C27 0.086(5) 0.040(3) 0.041(3) 0.001(3) -0.001(3) 0.014(3) C69 0.032(3) 0.098(6) 0.056(4) 0.003(4) 0.001(3) 0.004(3) C62 0.037(3) 0.088(5) 0.093(6) 0.019(4) -0.023(3) 0.000(3) C78 0.124(8) 0.110(7) 0.050(4) -0.016(4) 0.023(5) -0.047(6) C75 0.044(4) 0.132(8) 0.097(6) 0.057(6) 0.030(4) 0.012(4) C65 0.047(4) 0.102(6) 0.059(4) 0.014(4) -0.001(3) 0.000(4) C77 0.073(5) 0.176(11) 0.067(5) 0.017(6) -0.010(4) -0.069(7) C61 0.039(3) 0.082(5) 0.072(5) -0.004(4) 0.000(3) 0.009(3) C64 0.070(5) 0.084(6) 0.078(5) 0.004(4) -0.023(4) 0.013(4) C74 0.036(3) 0.102(6) 0.102(6) 0.037(5) 0.021(4) 0.015(4) O18 0.030(2) 0.028(2) 0.083(3) 0.0087(18) 0.0040(18) 0.0032(13) O17 0.050(3) 0.078(5) 0.121(8) 0.024(5) -0.013(4) -0.009(3) O19 0.174(8) 0.106(5) 0.091(5) -0.005(4) -0.005(5) -0.034(5) O16 0.049(6) 0.060(7) 0.064(7) 0.000(5) -0.002(4) -0.017(4) O14' 0.044(6) 0.057(7) 0.070(9) 0.009(6) -0.006(5) -0.014(5) O13 0.072(7) 0.094(8) 0.138(11) -0.050(7) -0.031(6) -0.001(5) O14 0.094(10) 0.141(18) 0.25(3) -0.09(2) 0.015(13) -0.025(10) O13' 0.073(9) 0.179(18) 0.067(9) 0.035(10) -0.014(7) -0.008(10) O16' 0.131(14) 0.107(13) 0.23(3) -0.003(15) 0.008(16) -0.029(10) O17' 0.033(15) 0.09(3) 0.12(4) 0.03(3) -0.026(18) 0.009(16) _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 Co3 O5 2.002(3) . ? Co3 O9 2.003(4) . ? Co3 N9 2.033(5) . ? Co3 N5 2.042(5) . ? Co2 O7 1.998(4) . ? Co2 N7 2.028(5) 8_576 ? Co2 N11 2.038(5) 2_565 ? Co2 O3 2.045(4) . ? Co1 O12 1.983(4) 1_545 ? Co1 O1 1.993(4) . ? Co1 N3 2.036(4) 2_554 ? Co1 N1 2.043(4) . ? O5 C26 1.262(7) . ? O1 C21 1.280(6) . ? O2 C21 1.245(6) . ? O4 C24 1.237(6) . ? O9 C33 1.275(6) . ? O12 C35 1.293(6) . ? O12 Co1 1.983(4) 1_565 ? O10 C33 1.247(6) . ? O3 C24 1.273(6) . ? O7 C30 1.273(7) . ? O6 C26 1.261(7) . ? O11 C35 1.234(6) . ? O8 C30 1.252(7) . ? N3 C18 1.349(6) . ? N3 C19 1.385(7) . ? N3 Co1 2.036(4) 2 ? N4 C18 1.329(6) . ? N4 C20 1.376(7) . ? N4 C17 1.480(6) . ? N1 C1 1.338(6) . ? N1 C2 1.388(7) . ? N9 C39 1.331(6) . ? N9 C40 1.378(7) . ? N5 C59 1.306(7) . ? N5 C60 1.401(8) . ? N2 C1 1.340(6) . ? N2 C3 1.386(7) . ? N2 C4 1.467(6) . ? N11 C56 1.326(7) . ? N11 C58 1.366(8) . ? N11 Co2 2.038(5) 2_564 ? N7 C76 1.317(8) . ? N7 C78 1.353(10) . ? N7 Co2 2.028(5) 8_575 ? N10 C39 1.350(7) . ? N10 C41 1.360(7) . ? N10 C42 1.498(7) . ? N12 C56 1.336(8) . ? N12 C57 1.345(8) . ? N12 C55 1.522(8) . ? N6 C59 1.336(8) . ? N6 C61 1.343(9) . ? N6 C62 1.489(8) . ? N8 C76 1.317(8) . ? N8 C77 1.324(12) . ? N8 C75 1.468(9) . ? C70 C72 1.387(12) . ? C70 C69 1.423(12) . ? C70 H52 0.9500 . ? C55 C54 1.554(10) . ? C55 H39 0.9900 . ? C55 H38 0.9900 . ? C71 C73 1.390(11) . ? C71 C69 1.397(10) . ? C71 H53 0.9500 . ? C73 C74 1.417(13) . ? C73 H55 0.9500 . ? C72 C74 1.393(12) . ? C72 H54 0.9500 . ? C33 C32 1.511(7) . ? C32 C31 1.409(7) . ? C32 C34 1.421(6) . ? C18 H16 0.9500 . ? C24 C23 1.523(7) . ? C1 H1 0.9500 . ? C34 C36 1.394(7) . ? C34 C35 1.502(7) . ? C20 C19 1.351(7) . ? C20 H17 0.9500 . ? C22 C29 1.396(8) . ? C22 C23 1.416(7) . ? C22 C21 1.502(7) . ? C23 C25 1.405(7) . ? C2 C3 1.354(8) . ? C2 H2 0.9500 . ? C19 H18 0.9500 . ? C10 C9 1.367(9) . ? C10 C8 1.385(9) . ? C10 C11 1.504(9) . ? C15 C13 1.381(9) . ? C15 C16 1.421(9) . ? C15 H13 0.9500 . ? C30 C31 1.500(7) . ? C76 H58 0.9500 . ? C26 C25 1.510(7) . ? C47 C45 1.363(9) . ? C47 C48 1.366(9) . ? C47 H33 0.9500 . ? C36 C37 1.394(8) . ? C36 H24 0.9500 . ? C3 H3 0.9500 . ? C39 H25 0.9500 . ? C54 C52 1.352(9) . ? C54 C53 1.400(10) . ? C31 C38 1.395(8) . ? C6 C8 1.370(8) . ? C6 C5 1.417(8) . ? C6 H6 0.9500 . ? C11 C12 1.396(9) . ? C11 C13 1.396(9) . ? C56 H41 0.9500 . ? C43 C45 1.414(9) . ? C43 C44 1.416(10) . ? C43 C42 1.488(9) . ? C38 C37 1.389(8) . ? C38 H22 0.9500 . ? C25 C27 1.409(8) . ? C5 C7 1.387(9) . ? C5 C4 1.501(8) . ? C59 H43 0.9500 . ? C50 C52 1.378(9) . ? C50 C49 1.401(9) . ? C50 H34 0.9500 . ? C4 H4 0.9900 . ? C4 H5 0.9900 . ? C58 C57 1.360(9) . ? C58 H42 0.9500 . ? C7 C9 1.421(9) . ? C7 H7 0.9500 . ? C17 C16 1.525(8) . ? C17 H14 0.9900 . ? C17 H15 0.9900 . ? C13 H11 0.9500 . ? C9 H9 0.9500 . ? C48 C46 1.410(9) . ? C48 C49 1.495(10) . ? C41 C40 1.352(8) . ? C41 H27 0.9500 . ? C45 H31 0.9500 . ? C8 H8 0.9500 . ? C49 C51 1.401(9) . ? C51 C53 1.382(10) . ? C51 H35 0.9500 . ? C40 H26 0.9500 . ? C37 H23 0.9500 . ? C53 H37 0.9500 . ? C52 H36 0.9500 . ? C12 C14 1.377(9) . ? C12 H10 0.9500 . ? C29 C28 1.386(9) . ? C29 H19 0.9500 . ? C16 C14 1.371(9) . ? C28 C27 1.387(9) . ? C28 H20 0.9500 . ? C60 C61 1.366(9) . ? C60 H44 0.9500 . ? C68 C67 1.396(12) . ? C68 C66 1.398(10) . ? C68 C69 1.488(10) . ? C57 H40 0.9500 . ? C44 C46 1.374(11) . ? C44 H30 0.9500 . ? C66 C65 1.387(10) . ? C66 H50 0.9500 . ? C42 H29 0.9900 . ? C42 H28 0.9900 . ? C63 C64 1.362(11) . ? C63 C65 1.408(11) . ? C63 C62 1.500(11) . ? C46 H32 0.9500 . ? C67 C64 1.421(12) . ? C67 H51 0.9500 . ? C14 H12 0.9500 . ? C27 H21 0.9500 . ? C62 H47 0.9900 . ? C62 H46 0.9900 . ? C78 C77 1.350(13) . ? C78 H60 0.9500 . ? C75 C74 1.493(11) . ? C75 H57 0.9900 . ? C75 H56 0.9900 . ? C65 H49 0.9500 . ? C77 H59 0.9500 . ? C61 H45 0.9500 . ? C64 H48 0.9500 . ? 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 O5 Co3 O9 114.70(15) . . ? O5 Co3 N9 117.50(17) . . ? O9 Co3 N9 108.61(16) . . ? O5 Co3 N5 112.75(16) . . ? O9 Co3 N5 93.63(17) . . ? N9 Co3 N5 106.87(18) . . ? O7 Co2 N7 108.46(18) . 8_576 ? O7 Co2 N11 126.69(18) . 2_565 ? N7 Co2 N11 104.96(19) 8_576 2_565 ? O7 Co2 O3 109.95(16) . . ? N7 Co2 O3 93.99(19) 8_576 . ? N11 Co2 O3 107.78(16) 2_565 . ? O12 Co1 O1 139.89(18) 1_545 . ? O12 Co1 N3 100.46(16) 1_545 2_554 ? O1 Co1 N3 100.97(16) . 2_554 ? O12 Co1 N1 102.80(16) 1_545 . ? O1 Co1 N1 101.89(16) . . ? N3 Co1 N1 108.61(17) 2_554 . ? C26 O5 Co3 106.3(3) . . ? C21 O1 Co1 107.3(3) . . ? C33 O9 Co3 106.0(3) . . ? C35 O12 Co1 112.2(3) . 1_565 ? C24 O3 Co2 105.2(3) . . ? C30 O7 Co2 100.1(3) . . ? C18 N3 C19 105.2(4) . . ? C18 N3 Co1 126.7(3) . 2 ? C19 N3 Co1 128.1(3) . 2 ? C18 N4 C20 108.3(4) . . ? C18 N4 C17 125.4(4) . . ? C20 N4 C17 126.2(4) . . ? C1 N1 C2 106.2(4) . . ? C1 N1 Co1 124.6(3) . . ? C2 N1 Co1 129.3(3) . . ? C39 N9 C40 104.7(5) . . ? C39 N9 Co3 125.0(4) . . ? C40 N9 Co3 130.3(4) . . ? C59 N5 C60 104.1(5) . . ? C59 N5 Co3 130.4(4) . . ? C60 N5 Co3 124.5(4) . . ? C1 N2 C3 107.8(4) . . ? C1 N2 C4 124.1(5) . . ? C3 N2 C4 128.0(5) . . ? C56 N11 C58 104.8(5) . . ? C56 N11 Co2 128.4(4) . 2_564 ? C58 N11 Co2 126.2(4) . 2_564 ? C76 N7 C78 103.3(6) . . ? C76 N7 Co2 131.7(5) . 8_575 ? C78 N7 Co2 124.9(5) . 8_575 ? C39 N10 C41 108.3(4) . . ? C39 N10 C42 127.9(5) . . ? C41 N10 C42 123.8(5) . . ? C56 N12 C57 107.2(5) . . ? C56 N12 C55 130.4(5) . . ? C57 N12 C55 122.3(5) . . ? C59 N6 C61 108.8(5) . . ? C59 N6 C62 124.8(6) . . ? C61 N6 C62 126.0(6) . . ? C76 N8 C77 106.0(6) . . ? C76 N8 C75 126.6(7) . . ? C77 N8 C75 127.2(7) . . ? C72 C70 C69 121.7(8) . . ? C72 C70 H52 119.2 . . ? C69 C70 H52 119.2 . . ? N12 C55 C54 112.1(5) . . ? N12 C55 H39 109.2 . . ? C54 C55 H39 109.2 . . ? N12 C55 H38 109.2 . . ? C54 C55 H38 109.2 . . ? H39 C55 H38 107.9 . . ? C73 C71 C69 120.2(8) . . ? C73 C71 H53 119.9 . . ? C69 C71 H53 119.9 . . ? C71 C73 C74 122.7(8) . . ? C71 C73 H55 118.6 . . ? C74 C73 H55 118.6 . . ? C70 C72 C74 121.3(9) . . ? C70 C72 H54 119.4 . . ? C74 C72 H54 119.4 . . ? O10 C33 O9 123.7(5) . . ? O10 C33 C32 118.5(4) . . ? O9 C33 C32 117.7(4) . . ? C31 C32 C34 118.3(4) . . ? C31 C32 C33 120.0(4) . . ? C34 C32 C33 121.7(4) . . ? N4 C18 N3 110.6(4) . . ? N4 C18 H16 124.7 . . ? N3 C18 H16 124.7 . . ? O4 C24 O3 123.3(5) . . ? O4 C24 C23 118.9(4) . . ? O3 C24 C23 117.8(4) . . ? N1 C1 N2 110.5(4) . . ? N1 C1 H1 124.8 . . ? N2 C1 H1 124.8 . . ? C36 C34 C32 119.7(4) . . ? C36 C34 C35 119.3(4) . . ? C32 C34 C35 121.0(4) . . ? O11 C35 O12 122.9(5) . . ? O11 C35 C34 121.7(4) . . ? O12 C35 C34 115.3(4) . . ? C19 C20 N4 106.2(4) . . ? C19 C20 H17 126.9 . . ? N4 C20 H17 126.9 . . ? C29 C22 C23 119.9(5) . . ? C29 C22 C21 118.3(4) . . ? C23 C22 C21 121.8(4) . . ? C25 C23 C22 119.5(5) . . ? C25 C23 C24 119.7(4) . . ? C22 C23 C24 120.8(4) . . ? C3 C2 N1 109.1(5) . . ? C3 C2 H2 125.5 . . ? N1 C2 H2 125.5 . . ? C20 C19 N3 109.7(4) . . ? C20 C19 H18 125.2 . . ? N3 C19 H18 125.2 . . ? O2 C21 O1 122.4(5) . . ? O2 C21 C22 120.7(4) . . ? O1 C21 C22 116.9(4) . . ? C9 C10 C8 118.5(6) . . ? C9 C10 C11 120.9(6) . . ? C8 C10 C11 120.5(6) . . ? C13 C15 C16 121.2(6) . . ? C13 C15 H13 119.4 . . ? C16 C15 H13 119.4 . . ? O8 C30 O7 121.8(5) . . ? O8 C30 C31 118.8(5) . . ? O7 C30 C31 119.4(5) . . ? N8 C76 N7 113.5(7) . . ? N8 C76 H58 123.3 . . ? N7 C76 H58 123.2 . . ? O5 C26 O6 123.1(5) . . ? O5 C26 C25 118.5(5) . . ? O6 C26 C25 118.4(5) . . ? C45 C47 C48 123.2(6) . . ? C45 C47 H33 118.4 . . ? C48 C47 H33 118.4 . . ? C37 C36 C34 121.4(5) . . ? C37 C36 H24 119.3 . . ? C34 C36 H24 119.3 . . ? C2 C3 N2 106.5(5) . . ? C2 C3 H3 126.8 . . ? N2 C3 H3 126.8 . . ? N9 C39 N10 110.7(5) . . ? N9 C39 H25 124.6 . . ? N10 C39 H25 124.6 . . ? C52 C54 C53 119.5(7) . . ? C52 C54 C55 122.4(6) . . ? C53 C54 C55 118.0(6) . . ? C38 C31 C32 120.7(5) . . ? C38 C31 C30 116.9(5) . . ? C32 C31 C30 122.3(5) . . ? C8 C6 C5 122.9(6) . . ? C8 C6 H6 118.6 . . ? C5 C6 H6 118.6 . . ? C12 C11 C13 117.0(6) . . ? C12 C11 C10 121.7(6) . . ? C13 C11 C10 121.2(6) . . ? N11 C56 N12 111.7(5) . . ? N11 C56 H41 124.2 . . ? N12 C56 H41 124.2 . . ? C45 C43 C44 114.5(7) . . ? C45 C43 C42 126.4(7) . . ? C44 C43 C42 119.0(6) . . ? C37 C38 C31 120.8(5) . . ? C37 C38 H22 119.6 . . ? C31 C38 H22 119.6 . . ? C23 C25 C27 119.2(5) . . ? C23 C25 C26 123.2(5) . . ? C27 C25 C26 117.5(5) . . ? C7 C5 C6 115.4(6) . . ? C7 C5 C4 126.5(6) . . ? C6 C5 C4 117.5(5) . . ? N5 C59 N6 112.1(6) . . ? N5 C59 H43 123.9 . . ? N6 C59 H43 123.9 . . ? C52 C50 C49 120.5(6) . . ? C52 C50 H34 119.7 . . ? C49 C50 H34 119.7 . . ? N2 C4 C5 110.7(5) . . ? N2 C4 H4 109.5 . . ? C5 C4 H4 109.5 . . ? N2 C4 H5 109.5 . . ? C5 C4 H5 109.5 . . ? H4 C4 H5 108.1 . . ? C57 C58 N11 109.4(5) . . ? C57 C58 H42 125.3 . . ? N11 C58 H42 125.3 . . ? C5 C7 C9 121.5(6) . . ? C5 C7 H7 119.3 . . ? C9 C7 H7 119.3 . . ? N4 C17 C16 110.1(4) . . ? N4 C17 H14 109.6 . . ? C16 C17 H14 109.6 . . ? N4 C17 H15 109.6 . . ? C16 C17 H15 109.6 . . ? H14 C17 H15 108.2 . . ? C15 C13 C11 121.2(6) . . ? C15 C13 H11 119.4 . . ? C11 C13 H11 119.4 . . ? C10 C9 C7 120.9(6) . . ? C10 C9 H9 119.5 . . ? C7 C9 H9 119.5 . . ? C47 C48 C46 117.1(6) . . ? C47 C48 C49 122.7(6) . . ? C46 C48 C49 120.3(6) . . ? C40 C41 N10 105.5(5) . . ? C40 C41 H27 127.2 . . ? N10 C41 H27 127.2 . . ? C47 C45 C43 121.9(7) . . ? C47 C45 H31 119.1 . . ? C43 C45 H31 119.1 . . ? C6 C8 C10 120.8(6) . . ? C6 C8 H8 119.6 . . ? C10 C8 H8 119.6 . . ? C50 C49 C51 117.4(6) . . ? C50 C49 C48 121.1(6) . . ? C51 C49 C48 121.5(6) . . ? C53 C51 C49 121.4(7) . . ? C53 C51 H35 119.3 . . ? C49 C51 H35 119.3 . . ? C41 C40 N9 110.8(5) . . ? C41 C40 H26 124.6 . . ? N9 C40 H26 124.6 . . ? C38 C37 C36 119.1(5) . . ? C38 C37 H23 120.5 . . ? C36 C37 H23 120.5 . . ? C51 C53 C54 119.4(6) . . ? C51 C53 H37 120.3 . . ? C54 C53 H37 120.3 . . ? C54 C52 C50 121.7(7) . . ? C54 C52 H36 119.1 . . ? C50 C52 H36 119.1 . . ? C14 C12 C11 121.4(6) . . ? C14 C12 H10 119.3 . . ? C11 C12 H10 119.3 . . ? C28 C29 C22 120.4(5) . . ? C28 C29 H19 119.8 . . ? C22 C29 H19 119.8 . . ? C14 C16 C15 116.6(6) . . ? C14 C16 C17 126.2(6) . . ? C15 C16 C17 116.7(5) . . ? C29 C28 C27 120.2(6) . . ? C29 C28 H20 119.9 . . ? C27 C28 H20 119.9 . . ? C61 C60 N5 109.7(6) . . ? C61 C60 H44 125.2 . . ? N5 C60 H44 125.2 . . ? C67 C68 C66 117.5(7) . . ? C67 C68 C69 121.2(7) . . ? C66 C68 C69 121.3(8) . . ? N12 C57 C58 106.8(6) . . ? N12 C57 H40 126.6 . . ? C58 C57 H40 126.6 . . ? C46 C44 C43 123.0(7) . . ? C46 C44 H30 118.5 . . ? C43 C44 H30 118.5 . . ? C65 C66 C68 121.4(8) . . ? C65 C66 H50 119.3 . . ? C68 C66 H50 119.3 . . ? C43 C42 N10 112.0(5) . . ? C43 C42 H29 109.2 . . ? N10 C42 H29 109.2 . . ? C43 C42 H28 109.2 . . ? N10 C42 H28 109.2 . . ? H29 C42 H28 107.9 . . ? C64 C63 C65 119.3(8) . . ? C64 C63 C62 120.4(8) . . ? C65 C63 C62 120.2(7) . . ? C44 C46 C48 120.4(7) . . ? C44 C46 H32 119.8 . . ? C48 C46 H32 119.8 . . ? C68 C67 C64 121.1(8) . . ? C68 C67 H51 119.5 . . ? C64 C67 H51 119.5 . . ? C16 C14 C12 122.4(6) . . ? C16 C14 H12 118.8 . . ? C12 C14 H12 118.8 . . ? C28 C27 C25 120.7(6) . . ? C28 C27 H21 119.7 . . ? C25 C27 H21 119.7 . . ? C71 C69 C70 117.3(7) . . ? C71 C69 C68 121.1(7) . . ? C70 C69 C68 121.6(7) . . ? N6 C62 C63 111.1(6) . . ? N6 C62 H47 109.4 . . ? C63 C62 H47 109.4 . . ? N6 C62 H46 109.4 . . ? C63 C62 H46 109.4 . . ? H47 C62 H46 108.0 . . ? C77 C78 N7 109.6(7) . . ? C77 C78 H60 125.2 . . ? N7 C78 H60 125.2 . . ? N8 C75 C74 111.6(7) . . ? N8 C75 H57 109.3 . . ? C74 C75 H57 109.3 . . ? N8 C75 H56 109.3 . . ? C74 C75 H56 109.3 . . ? H57 C75 H56 108.0 . . ? C66 C65 C63 120.3(8) . . ? C66 C65 H49 119.8 . . ? C63 C65 H49 119.8 . . ? N8 C77 C78 107.5(7) . . ? N8 C77 H59 126.2 . . ? C78 C77 H59 126.2 . . ? N6 C61 C60 105.3(6) . . ? N6 C61 H45 127.4 . . ? C60 C61 H45 127.4 . . ? C63 C64 C67 120.3(9) . . ? C63 C64 H48 119.9 . . ? C67 C64 H48 119.9 . . ? C72 C74 C73 116.6(8) . . ? C72 C74 C75 120.3(9) . . ? C73 C74 C75 123.0(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.531 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.141