Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global loop_ _publ_author_name 'Masci, Bernardo' 'Nierlich, Martine' 'Thuery, Pierre' 'Vicens, Jacques' _publ_contact_author ; Pierre Thu\'ery CEA Saclay, SCM (CNRS URA 331) B\^at. 125 91191 Gif-sur-Yvette France ; _publ_contact_author_phone '16(1)69 08 63 29' _publ_contact_author_fax '16(1)69 08 66 40' _publ_contact_author_email thuery@drecam.cea.fr _journal_coden_Cambridge 186 _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ? data_4 _database_code_CSD 153523 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H106 N2 O8' _chemical_formula_weight 1175.63 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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.8354(19) _cell_length_b 10.1184(6) _cell_length_c 32.3655(27) _cell_angle_alpha 90.00 _cell_angle_beta 91.815(3) _cell_angle_gamma 90.00 _cell_volume 6820(1) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 44684 _cell_measurement_theta_min 5.11 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method ? _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; \f scans with 2\% steps ; _diffrn_ambient_temperature 110(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 44684 _diffrn_reflns_av_R_equivalents 0.148 _diffrn_reflns_av_sigmaI/netI 0.261 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 25.68 _reflns_number_total 12162 _reflns_number_gt 4359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and expanded by subsequent Fourier-difference synthesis. Three tert-butyl groups were found disordered and were modelled with five or six terminal carbon atoms. The acetonitrile solvent molecule is disordered over two sites, the terminal carbon atom being located on a symmetry centre. All non-hydrogen atoms were refined anisotropically, unless the disordered ones. The hydroxyl protons and the one bound to the nitrogen atom of the triethylammonium moiety have been found on the Fourier-difference maps and introduced as riding atoms with a displacement factor equal to 1.2 times that of the parent atom. The other hydrogen atoms were introduced at calculated positions (unless in the disordered parts)as riding atoms with displacement factors equal to 1.2 (CH, CH2) or 1.5 (CH3) times that of the parent atom. 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^)+(0.1357P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12162 _refine_ls_number_parameters 777 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.2750 _refine_ls_R_factor_gt 0.1027 _refine_ls_wR_factor_ref 0.3044 _refine_ls_wR_factor_gt 0.2175 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.580 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.059 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 O1 O 0.82386(18) 0.0386(4) 0.27864(12) 0.0414(10) Uani 1 1 d . . . H1O H 0.8172 0.0744 0.3103 0.050 Uiso 1 1 d R . . O2 O 0.81628(18) 0.1027(4) 0.36174(12) 0.0392(10) Uani 1 1 d . . . H2O H 0.7817 0.1028 0.3815 0.047 Uiso 1 1 d R . . O3 O 0.78345(19) 0.0520(4) 0.43992(12) 0.0393(10) Uani 1 1 d . . . O4 O 0.6601(2) 0.0883(4) 0.39009(12) 0.0424(10) Uani 1 1 d . . . H4O H 0.6333 0.1102 0.3616 0.051 Uiso 1 1 d R . . O5 O 0.58235(18) 0.0951(4) 0.32785(11) 0.0352(9) Uani 1 1 d . . . O6 O 0.58870(18) 0.0909(4) 0.25190(12) 0.0392(10) Uani 1 1 d . . . H6O H 0.5806 0.0828 0.2877 0.047 Uiso 1 1 d R . . O7 O 0.69140(19) 0.0501(4) 0.20986(12) 0.0404(10) Uani 1 1 d . . . H7O H 0.6480 0.0673 0.2301 0.049 Uiso 1 1 d R . . O8 O 0.81142(17) -0.0642(4) 0.18486(11) 0.0333(9) Uani 1 1 d . . . C1 C 0.8856(3) 0.0383(5) 0.26563(17) 0.0326(14) Uani 1 1 d . . . C2 C 0.9342(3) 0.1211(5) 0.28275(18) 0.0349(14) Uani 1 1 d . . . C3 C 0.9957(3) 0.1109(5) 0.26792(17) 0.0320(13) Uani 1 1 d . . . H3 H 1.0269 0.1687 0.2783 0.038 Uiso 1 1 calc R . . C4 C 1.0131(3) 0.0193(6) 0.23856(18) 0.0360(14) Uani 1 1 d . . . C5 C 0.9638(3) -0.0599(6) 0.22144(17) 0.0337(14) Uani 1 1 d . . . H5 H 0.9737 -0.1208 0.2011 0.040 Uiso 1 1 calc R . . C6 C 0.9008(3) -0.0502(5) 0.23398(17) 0.0351(14) Uani 1 1 d . . . C7 C 1.0828(3) -0.0019(6) 0.22453(19) 0.0417(15) Uani 1 1 d . . . C8 C 1.1297(3) 0.0851(7) 0.2488(2) 0.0556(18) Uani 1 1 d . . . H8A H 1.1721 0.0730 0.2387 0.083 Uiso 1 1 calc R . . H8B H 1.1294 0.0612 0.2775 0.083 Uiso 1 1 calc R . . H8C H 1.1172 0.1759 0.2457 0.083 Uiso 1 1 calc R . . C9 C 1.1009(3) -0.1452(6) 0.2320(2) 0.058(2) Uani 1 1 d . . . H9A H 1.0749 -0.2009 0.2142 0.087 Uiso 1 1 calc R . . H9B H 1.0940 -0.1677 0.2603 0.087 Uiso 1 1 calc R . . H9C H 1.1454 -0.1579 0.2260 0.087 Uiso 1 1 calc R . . C10 C 1.0882(3) 0.0342(7) 0.1794(2) 0.0543(18) Uani 1 1 d . . . H10A H 1.1310 0.0159 0.1708 0.081 Uiso 1 1 calc R . . H10B H 1.0791 0.1265 0.1758 0.081 Uiso 1 1 calc R . . H10C H 1.0580 -0.0170 0.1631 0.081 Uiso 1 1 calc R . . C11 C 0.9204(3) 0.2137(6) 0.31789(17) 0.0372(15) Uani 1 1 d . . . H11A H 0.8768 0.2469 0.3149 0.045 Uiso 1 1 calc R . . H11B H 0.9496 0.2882 0.3176 0.045 Uiso 1 1 calc R . . C12 C 0.9290(3) 0.1371(5) 0.35899(18) 0.0381(15) Uani 1 1 d . . . C13 C 0.8776(3) 0.0816(6) 0.37900(19) 0.0375(15) Uani 1 1 d . . . C14 C 0.8869(3) 0.0073(6) 0.41407(18) 0.0363(14) Uani 1 1 d . . . C15 C 0.9489(3) -0.0165(6) 0.42903(19) 0.0398(15) Uani 1 1 d . . . H15 H 0.9549 -0.0669 0.4529 0.048 Uiso 1 1 calc R . . C16 C 1.0030(3) 0.0332(6) 0.40924(19) 0.0398(15) Uani 1 1 d . . . C17 C 0.9902(3) 0.1126(6) 0.37526(18) 0.0391(15) Uani 1 1 d . . . H17 H 1.0248 0.1520 0.3625 0.047 Uiso 1 1 calc R . . C18 C 1.0713(3) 0.0060(7) 0.4249(2) 0.0501(18) Uani 1 1 d . . . C19 C 1.1111(4) -0.0340(8) 0.3877(2) 0.067(2) Uani 1 1 d . . . H19A H 1.0923 -0.1107 0.3747 0.100 Uiso 1 1 calc R . . H19B H 1.1543 -0.0538 0.3970 0.100 Uiso 1 1 calc R . . H19C H 1.1116 0.0375 0.3682 0.100 Uiso 1 1 calc R . . C20 C 1.0982(4) 0.1339(8) 0.4450(3) 0.083(3) Uani 1 1 d . . . H20A H 1.0990 0.2028 0.4246 0.124 Uiso 1 1 calc R . . H20B H 1.1410 0.1181 0.4558 0.124 Uiso 1 1 calc R . . H20C H 1.0713 0.1603 0.4671 0.124 Uiso 1 1 calc R . . C21 C 1.0760(3) -0.1056(7) 0.4568(2) 0.061(2) Uani 1 1 d . . . H21A H 1.0537 -0.0804 0.4811 0.092 Uiso 1 1 calc R . . H21B H 1.1204 -0.1221 0.4640 0.092 Uiso 1 1 calc R . . H21C H 1.0570 -0.1843 0.4452 0.092 Uiso 1 1 calc R . . C22 C 0.8300(3) -0.0511(6) 0.43577(19) 0.0398(15) Uani 1 1 d . . . H22A H 0.8118 -0.1236 0.4197 0.048 Uiso 1 1 calc R . . H22B H 0.8435 -0.0844 0.4628 0.048 Uiso 1 1 calc R . . C23 C 0.7273(3) 0.0086(6) 0.46065(19) 0.0385(15) Uani 1 1 d . . . H23A H 0.7390 -0.0174 0.4887 0.046 Uiso 1 1 calc R . . H23B H 0.7090 -0.0676 0.4464 0.046 Uiso 1 1 calc R . . C24 C 0.6796(3) 0.1155(6) 0.46134(18) 0.0404(15) Uani 1 1 d . . . C25 C 0.6440(3) 0.1491(6) 0.42540(19) 0.0399(15) Uani 1 1 d . . . C26 C 0.5942(3) 0.2445(7) 0.4271(2) 0.0466(16) Uani 1 1 d . . . C27 C 0.5858(3) 0.3084(7) 0.4647(2) 0.0547(18) Uani 1 1 d . . . H27 H 0.5538 0.3722 0.4658 0.066 Uiso 1 1 calc R . . C28 C 0.6221(3) 0.2832(7) 0.50068(17) 0.058(2) Uani 1 1 d D . . C29 C 0.6677(3) 0.1865(7) 0.4977(2) 0.0541(18) Uani 1 1 d . . . H29 H 0.6924 0.1664 0.5213 0.065 Uiso 1 1 calc R . . C30 C 0.6124(3) 0.3590(8) 0.5403(2) 0.079(3) Uani 1 1 d D . . C31A C 0.5510(6) 0.3251(15) 0.5605(4) 0.081(5) Uiso 0.61(2) 1 d PD . . C31B C 0.5830(12) 0.2577(18) 0.5715(4) 0.082(9) Uiso 0.39(2) 1 d PD . . C32A C 0.6721(5) 0.3683(16) 0.5675(4) 0.056(5) Uiso 0.61(2) 1 d PD . . C32B C 0.6759(7) 0.403(2) 0.5605(6) 0.056(8) Uiso 0.39(2) 1 d PD . . C33A C 0.5952(7) 0.5067(9) 0.5287(4) 0.080(6) Uiso 0.61(2) 1 d PD . . C33B C 0.5532(8) 0.439(2) 0.5420(6) 0.088(9) Uiso 0.39(2) 1 d PD . . C34 C 0.5558(3) 0.2869(6) 0.38888(19) 0.0448(17) Uani 1 1 d . . . H34A H 0.5341 0.3689 0.3952 0.054 Uiso 1 1 calc R . . H34B H 0.5857 0.3059 0.3673 0.054 Uiso 1 1 calc R . . C35 C 0.5067(3) 0.1925(6) 0.37174(19) 0.0401(15) Uani 1 1 d . . . C36 C 0.5212(3) 0.1057(6) 0.34054(19) 0.0396(15) Uani 1 1 d . . . C37 C 0.4727(3) 0.0246(6) 0.3220(2) 0.0431(16) Uani 1 1 d . . . C38 C 0.4111(3) 0.0333(7) 0.3363(2) 0.0485(17) Uani 1 1 d . . . H38 H 0.3796 -0.0207 0.3242 0.058 Uiso 1 1 calc R . . C39 C 0.3939(3) 0.1169(7) 0.3672(2) 0.059(2) Uani 1 1 d D . . C40 C 0.4418(4) 0.1981(7) 0.3853(2) 0.0547(19) Uani 1 1 d . . . H40 H 0.4313 0.2562 0.4063 0.066 Uiso 1 1 calc R . . C41 C 0.3224(4) 0.1214(7) 0.3825(2) 0.072(2) Uani 1 1 d D . . C42A C 0.3116(5) 0.2446(10) 0.4074(4) 0.084(5) Uiso 0.77(2) 1 d PD . . C42B C 0.3259(12) 0.150(6) 0.4288(5) 0.14(3) Uiso 0.23(2) 1 d PD . . C43A C 0.3108(6) -0.0086(11) 0.4053(4) 0.109(6) Uiso 0.77(2) 1 d PD . . C43B C 0.2882(13) -0.004(4) 0.368(2) 0.16(3) Uiso 0.23(2) 1 d PD . . C44 C 0.2769(5) 0.1311(10) 0.3434(3) 0.102(3) Uiso 1 1 d . . . C45 C 0.4872(3) -0.0634(6) 0.2865(2) 0.0450(17) Uani 1 1 d . . . H45A H 0.4579 -0.1379 0.2866 0.054 Uiso 1 1 calc R . . H45B H 0.5304 -0.0978 0.2906 0.054 Uiso 1 1 calc R . . C46 C 0.4820(3) 0.0033(6) 0.24471(19) 0.0414(15) Uani 1 1 d . . . C47 C 0.5329(3) 0.0772(5) 0.2297(2) 0.0391(15) Uani 1 1 d . . . C48 C 0.5283(3) 0.1353(6) 0.19023(19) 0.0382(15) Uani 1 1 d . . . C49 C 0.4709(3) 0.1194(6) 0.1665(2) 0.0459(17) Uani 1 1 d . . . H49 H 0.4680 0.1569 0.1403 0.055 Uiso 1 1 calc R . . C50 C 0.4186(3) 0.0498(6) 0.18084(19) 0.0509(18) Uani 1 1 d D . . C51 C 0.4250(3) -0.0085(6) 0.2203(2) 0.0441(16) Uani 1 1 d . . . H51 H 0.3908 -0.0561 0.2305 0.053 Uiso 1 1 calc R . . C52 C 0.3558(4) 0.0325(7) 0.1557(2) 0.072(2) Uani 1 1 d D . . C53A C 0.3664(9) 0.035(3) 0.1095(3) 0.117(10) Uiso 0.57(3) 1 d PD . . C54A C 0.3148(9) -0.079(2) 0.1712(8) 0.149(10) Uiso 0.57(3) 1 d PD . . C55A C 0.3093(5) 0.1448(15) 0.1689(5) 0.075(6) Uiso 0.57(3) 1 d PD . . C55B C 0.2976(5) 0.057(4) 0.1807(7) 0.122(12) Uiso 0.43(3) 1 d PD . . C54B C 0.3429(11) -0.1183(12) 0.1511(8) 0.100(10) Uiso 0.43(3) 1 d PD . . C53B C 0.3628(7) 0.079(2) 0.1111(3) 0.052(6) Uiso 0.43(3) 1 d PD . . C56 C 0.5843(3) 0.2032(6) 0.17214(19) 0.0406(15) Uani 1 1 d . . . H56A H 0.6098 0.2446 0.1941 0.049 Uiso 1 1 calc R . . H56B H 0.5689 0.2722 0.1535 0.049 Uiso 1 1 calc R . . C57 C 0.6263(3) 0.1085(5) 0.14873(17) 0.0316(13) Uani 1 1 d . . . C58 C 0.6746(3) 0.0321(5) 0.16845(17) 0.0344(14) Uani 1 1 d . . . C59 C 0.7086(3) -0.0601(6) 0.14733(18) 0.0356(14) Uani 1 1 d . . . C60 C 0.6941(3) -0.0824(6) 0.10563(18) 0.0377(14) Uani 1 1 d . . . H60 H 0.7169 -0.1468 0.0918 0.045 Uiso 1 1 calc R . . C61 C 0.6467(3) -0.0122(6) 0.08389(18) 0.0389(15) Uani 1 1 d . . . C62 C 0.6139(3) 0.0828(6) 0.10676(18) 0.0399(15) Uani 1 1 d . . . H62 H 0.5819 0.1317 0.0932 0.048 Uiso 1 1 calc R . . C63 C 0.6270(3) -0.0391(5) 0.03866(18) 0.0392(15) Uani 1 1 d . . . C64 C 0.6232(4) 0.0913(6) 0.0142(2) 0.064(2) Uani 1 1 d . . . H64A H 0.6096 0.0734 -0.0139 0.096 Uiso 1 1 calc R . . H64B H 0.6648 0.1323 0.0145 0.096 Uiso 1 1 calc R . . H64C H 0.5930 0.1496 0.0266 0.096 Uiso 1 1 calc R . . C65 C 0.6740(3) -0.1288(7) 0.0176(2) 0.0527(18) Uani 1 1 d . . . H65A H 0.6759 -0.2124 0.0316 0.079 Uiso 1 1 calc R . . H65B H 0.7158 -0.0888 0.0185 0.079 Uiso 1 1 calc R . . H65C H 0.6601 -0.1421 -0.0107 0.079 Uiso 1 1 calc R . . C66 C 0.5604(3) -0.1050(7) 0.0374(2) 0.0583(19) Uani 1 1 d . . . H66A H 0.5613 -0.1815 0.0549 0.087 Uiso 1 1 calc R . . H66B H 0.5494 -0.1309 0.0095 0.087 Uiso 1 1 calc R . . H66C H 0.5291 -0.0435 0.0469 0.087 Uiso 1 1 calc R . . C67 C 0.7584(3) -0.1447(6) 0.16989(19) 0.0372(15) Uani 1 1 d . . . H67A H 0.7389 -0.1888 0.1930 0.045 Uiso 1 1 calc R . . H67B H 0.7739 -0.2119 0.1513 0.045 Uiso 1 1 calc R . . C68 C 0.8485(3) -0.1369(5) 0.21564(17) 0.0329(14) Uani 1 1 d . . . H68A H 0.8673 -0.2142 0.2031 0.039 Uiso 1 1 calc R . . H68B H 0.8207 -0.1665 0.2373 0.039 Uiso 1 1 calc R . . N1 N 0.8285(2) 0.1842(5) 0.14915(16) 0.0405(13) Uani 1 1 d . . . H1N H 0.8206 0.0840 0.1605 0.049 Uiso 1 1 d R . . C69 C 0.7963(3) 0.3009(6) 0.1683(2) 0.0462(16) Uani 1 1 d . . . H69A H 0.8115 0.3808 0.1552 0.055 Uiso 1 1 calc R . . H69B H 0.7505 0.2947 0.1626 0.055 Uiso 1 1 calc R . . C70 C 0.8078(3) 0.3132(7) 0.2140(2) 0.0567(19) Uani 1 1 d . . . H70A H 0.7973 0.2313 0.2271 0.085 Uiso 1 1 calc R . . H70B H 0.7813 0.3825 0.2244 0.085 Uiso 1 1 calc R . . H70C H 0.8521 0.3338 0.2197 0.085 Uiso 1 1 calc R . . C71 C 0.8046(3) 0.1700(6) 0.1050(2) 0.0495(17) Uani 1 1 d . . . H71A H 0.8133 0.2513 0.0904 0.059 Uiso 1 1 calc R . . H71B H 0.7584 0.1580 0.1047 0.059 Uiso 1 1 calc R . . C72 C 0.8344(3) 0.0559(7) 0.0822(2) 0.0538(18) Uani 1 1 d . . . H72A H 0.8781 0.0770 0.0763 0.081 Uiso 1 1 calc R . . H72B H 0.8106 0.0404 0.0568 0.081 Uiso 1 1 calc R . . H72C H 0.8334 -0.0221 0.0991 0.081 Uiso 1 1 calc R . . C73 C 0.9011(3) 0.1847(6) 0.1538(2) 0.0462(16) Uani 1 1 d . . . H73A H 0.9131 0.1981 0.1827 0.055 Uiso 1 1 calc R . . H73B H 0.9172 0.0989 0.1457 0.055 Uiso 1 1 calc R . . C74 C 0.9329(3) 0.2892(6) 0.1285(2) 0.0519(18) Uani 1 1 d . . . H74A H 0.9239 0.2730 0.0997 0.078 Uiso 1 1 calc R . . H74B H 0.9784 0.2868 0.1339 0.078 Uiso 1 1 calc R . . H74C H 0.9165 0.3745 0.1359 0.078 Uiso 1 1 calc R . . N2 N 0.9072(6) 0.3153(12) 0.0140(5) 0.030(4) Uani 0.50 1 d PDU . . C75 C 0.9456(6) 0.3969(13) 0.0054(5) 0.016(4) Uani 0.50 1 d PDU . . C76 C 1.0000 0.5000 0.0000 0.085(7) Uani 0.50 2 d SPDU . . 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 O1 0.028(2) 0.060(3) 0.037(2) -0.0051(19) 0.0032(19) -0.0014(19) O2 0.028(2) 0.051(2) 0.039(2) -0.0008(19) 0.0011(19) 0.0050(19) O3 0.032(2) 0.043(2) 0.043(3) 0.0010(19) 0.0076(19) 0.0017(19) O4 0.047(3) 0.047(2) 0.034(2) -0.0035(19) 0.001(2) 0.006(2) O5 0.030(2) 0.047(2) 0.029(2) -0.0001(18) 0.0012(18) 0.0022(18) O6 0.028(2) 0.054(2) 0.036(2) -0.0018(19) -0.0024(19) -0.0001(19) O7 0.041(3) 0.055(3) 0.025(2) 0.0007(19) -0.0030(19) 0.003(2) O8 0.027(2) 0.041(2) 0.032(2) 0.0015(17) -0.0047(17) -0.0031(17) C1 0.029(3) 0.040(3) 0.030(3) 0.006(3) 0.007(3) 0.001(3) C2 0.035(4) 0.036(3) 0.033(4) 0.002(3) -0.006(3) -0.002(3) C3 0.029(3) 0.039(3) 0.029(3) -0.002(3) 0.001(3) 0.000(3) C4 0.033(4) 0.041(3) 0.034(3) 0.006(3) -0.003(3) 0.006(3) C5 0.027(3) 0.046(4) 0.028(3) -0.006(3) 0.002(3) 0.003(3) C6 0.042(4) 0.037(3) 0.026(3) 0.006(3) -0.006(3) 0.005(3) C7 0.033(4) 0.050(4) 0.043(4) 0.003(3) 0.007(3) 0.000(3) C8 0.034(4) 0.076(5) 0.057(5) -0.008(4) 0.004(3) 0.003(4) C9 0.035(4) 0.059(4) 0.080(6) -0.009(4) 0.006(4) 0.011(3) C10 0.042(4) 0.081(5) 0.040(4) 0.002(3) 0.004(3) -0.010(4) C11 0.035(4) 0.043(3) 0.033(4) 0.003(3) -0.002(3) 0.002(3) C12 0.048(4) 0.037(3) 0.029(3) -0.011(3) 0.005(3) -0.001(3) C13 0.037(4) 0.033(3) 0.042(4) -0.009(3) 0.001(3) -0.001(3) C14 0.036(4) 0.041(3) 0.032(4) -0.004(3) 0.007(3) 0.004(3) C15 0.039(4) 0.044(4) 0.036(4) -0.004(3) 0.000(3) 0.006(3) C16 0.035(4) 0.051(4) 0.034(4) -0.005(3) 0.001(3) 0.002(3) C17 0.037(4) 0.045(4) 0.035(4) -0.005(3) -0.005(3) 0.001(3) C18 0.033(4) 0.060(4) 0.056(5) 0.000(3) -0.009(3) 0.004(3) C19 0.054(5) 0.077(5) 0.068(5) 0.005(4) -0.010(4) 0.009(4) C20 0.064(6) 0.093(6) 0.088(7) -0.008(5) -0.042(5) -0.005(5) C21 0.052(5) 0.069(5) 0.062(5) 0.011(4) -0.010(4) 0.014(4) C22 0.034(4) 0.048(4) 0.038(4) -0.004(3) 0.002(3) 0.009(3) C23 0.033(4) 0.048(4) 0.035(4) 0.009(3) -0.002(3) 0.001(3) C24 0.038(4) 0.059(4) 0.025(3) 0.006(3) 0.008(3) 0.006(3) C25 0.044(4) 0.046(4) 0.031(4) -0.004(3) 0.012(3) 0.000(3) C26 0.042(4) 0.063(4) 0.036(4) -0.005(3) 0.009(3) 0.006(3) C27 0.051(4) 0.070(5) 0.043(4) -0.012(4) 0.005(4) 0.012(4) C28 0.045(4) 0.097(6) 0.032(4) -0.006(4) 0.009(3) 0.013(4) C29 0.041(4) 0.090(5) 0.031(4) -0.009(4) -0.002(3) 0.008(4) C30 0.048(5) 0.149(8) 0.041(5) -0.033(5) 0.007(4) 0.019(5) C34 0.057(4) 0.045(4) 0.032(4) 0.001(3) 0.007(3) 0.022(3) C35 0.034(4) 0.043(4) 0.043(4) 0.006(3) -0.001(3) 0.002(3) C36 0.036(4) 0.046(4) 0.037(4) 0.003(3) 0.003(3) 0.007(3) C37 0.024(4) 0.058(4) 0.047(4) 0.016(3) -0.003(3) 0.003(3) C38 0.047(4) 0.055(4) 0.044(4) 0.011(3) 0.000(3) 0.003(3) C39 0.042(5) 0.074(5) 0.063(5) 0.036(4) 0.011(4) 0.001(4) C40 0.064(5) 0.067(5) 0.034(4) 0.011(3) 0.013(4) 0.026(4) C41 0.071(6) 0.074(5) 0.070(6) 0.024(4) 0.006(4) 0.024(4) C45 0.035(4) 0.044(4) 0.056(4) 0.008(3) -0.015(3) -0.008(3) C46 0.042(4) 0.043(4) 0.039(4) 0.000(3) -0.003(3) -0.007(3) C47 0.034(4) 0.030(3) 0.052(4) -0.003(3) -0.009(3) 0.001(3) C48 0.036(4) 0.037(3) 0.042(4) 0.001(3) -0.002(3) 0.003(3) C49 0.043(4) 0.043(4) 0.051(4) -0.001(3) -0.009(3) -0.003(3) C50 0.055(5) 0.048(4) 0.049(4) 0.007(3) -0.022(4) -0.009(3) C51 0.033(4) 0.046(4) 0.052(4) -0.003(3) 0.000(3) -0.013(3) C52 0.077(6) 0.080(5) 0.058(5) 0.024(4) -0.030(4) -0.030(4) C56 0.038(4) 0.048(4) 0.036(4) 0.004(3) 0.000(3) -0.005(3) C57 0.037(3) 0.031(3) 0.027(3) -0.001(2) -0.006(3) -0.005(3) C58 0.037(4) 0.037(3) 0.029(3) 0.004(3) -0.008(3) -0.012(3) C59 0.032(3) 0.043(3) 0.031(3) -0.002(3) -0.005(3) -0.002(3) C60 0.032(3) 0.045(4) 0.037(4) 0.004(3) -0.003(3) 0.001(3) C61 0.043(4) 0.041(3) 0.033(4) 0.000(3) -0.002(3) -0.004(3) C62 0.034(4) 0.046(4) 0.039(4) -0.003(3) -0.013(3) 0.002(3) C63 0.044(4) 0.039(3) 0.034(4) -0.001(3) -0.013(3) 0.001(3) C64 0.106(7) 0.050(4) 0.036(4) 0.004(3) -0.004(4) 0.004(4) C65 0.049(4) 0.066(4) 0.042(4) -0.011(3) -0.010(3) 0.008(3) C66 0.053(5) 0.071(5) 0.049(4) -0.015(4) -0.016(4) 0.006(4) C67 0.030(3) 0.046(4) 0.036(4) 0.003(3) -0.005(3) -0.004(3) C68 0.035(4) 0.035(3) 0.028(3) 0.007(2) -0.007(3) 0.003(3) N1 0.038(3) 0.035(3) 0.049(3) 0.001(2) 0.000(3) -0.004(2) C69 0.048(4) 0.042(4) 0.049(4) -0.001(3) 0.008(3) 0.000(3) C70 0.045(4) 0.063(4) 0.062(5) -0.010(4) 0.008(4) -0.003(3) C71 0.047(4) 0.050(4) 0.051(4) 0.011(3) -0.005(3) -0.005(3) C72 0.056(5) 0.062(4) 0.043(4) -0.005(3) 0.000(3) -0.015(4) C73 0.033(4) 0.051(4) 0.055(4) -0.002(3) 0.005(3) -0.006(3) C74 0.050(4) 0.050(4) 0.056(5) 0.002(3) 0.001(3) -0.002(3) N2 0.023(8) 0.049(8) 0.018(7) -0.008(6) -0.015(6) 0.025(7) C75 0.018(6) 0.017(5) 0.013(6) 0.002(4) -0.002(4) 0.010(4) C76 0.104(11) 0.072(10) 0.081(10) -0.001(8) 0.031(9) 0.013(8) _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 O1 C1 1.366(7) . ? O1 O2 2.776(6) . ? O2 C13 1.394(7) . ? O2 O3 2.691(6) . ? O3 C23 1.435(7) . ? O3 C22 1.434(7) . ? O4 C25 1.350(7) . ? O4 O5 2.545(5) . ? O5 C36 1.355(7) . ? O5 O6 2.466(5) . ? O6 C47 1.353(7) . ? O6 O7 2.605(6) . ? O7 C58 1.387(6) . ? O8 C68 1.442(6) . ? O8 C67 1.445(6) . ? O8 N1 2.794(6) . ? C1 C6 1.405(8) . ? C1 C2 1.414(8) . ? C2 C3 1.386(8) . ? C2 C11 1.508(8) . ? C3 C4 1.384(8) . ? C4 C5 1.402(8) . ? C4 C7 1.550(8) . ? C5 C6 1.390(8) . ? C6 C68 1.507(8) . ? C7 C10 1.512(9) . ? C7 C8 1.516(9) . ? C7 C9 1.517(9) . ? C11 C12 1.545(8) . ? C12 C17 1.387(8) . ? C12 C13 1.389(8) . ? C13 C14 1.370(8) . ? C14 C15 1.387(8) . ? C14 C22 1.515(8) . ? C15 C16 1.407(8) . ? C16 C17 1.381(8) . ? C16 C18 1.521(8) . ? C18 C21 1.530(9) . ? C18 C19 1.539(10) . ? C18 C20 1.545(10) . ? C23 C24 1.470(8) . ? C24 C29 1.408(9) . ? C24 C25 1.402(8) . ? C25 C26 1.418(9) . ? C26 C27 1.395(9) . ? C26 C34 1.513(8) . ? C27 C28 1.393(9) . ? C28 C29 1.369(9) . ? C28 C30 1.514(8) . ? C30 C33B 1.478(9) . ? C30 C31A 1.495(8) . ? C30 C32A 1.502(8) . ? C30 C31B 1.575(9) . ? C30 C33A 1.581(8) . ? C30 C32B 1.521(9) . ? C34 C35 1.493(9) . ? C35 C36 1.379(8) . ? C35 C40 1.435(9) . ? C36 C37 1.420(9) . ? C37 C38 1.381(9) . ? C37 C45 1.490(9) . ? C38 C39 1.369(9) . ? C39 C40 1.405(10) . ? C39 C41 1.583(10) . ? C41 C43B 1.517(10) . ? C41 C42A 1.506(8) . ? C41 C43A 1.531(8) . ? C41 C44 1.560(12) . ? C41 C42B 1.527(10) . ? C43B C44 1.59(6) . ? C45 C46 1.513(8) . ? C46 C47 1.398(8) . ? C46 C51 1.409(8) . ? C47 C48 1.408(8) . ? C48 C49 1.409(8) . ? C48 C56 1.490(8) . ? C49 C50 1.391(9) . ? C50 C51 1.410(8) . ? C50 C52 1.528(8) . ? C52 C55B 1.500(9) . ? C52 C54A 1.509(9) . ? C52 C53A 1.518(9) . ? C52 C53B 1.529(9) . ? C52 C54B 1.556(9) . ? C52 C55A 1.561(8) . ? C56 C57 1.516(8) . ? C57 C62 1.399(8) . ? C57 C58 1.406(8) . ? C58 C59 1.369(8) . ? C59 C60 1.392(8) . ? C59 C67 1.513(8) . ? C60 C61 1.390(8) . ? C61 C62 1.403(8) . ? C61 C63 1.532(8) . ? C63 C65 1.514(9) . ? C63 C66 1.537(9) . ? C63 C64 1.540(8) . ? N1 C71 1.505(8) . ? N1 C69 1.501(8) . ? N1 C73 1.516(8) . ? C69 C70 1.495(9) . ? C71 C72 1.514(9) . ? C73 C74 1.502(9) . ? N2 C75 1.188(8) . ? C75 C76 1.555(8) . ? C76 C75 1.555(8) 3_765 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 O2 112.5(3) . . ? C13 O2 O3 81.4(3) . . ? C13 O2 O1 105.8(3) . . ? O3 O2 O1 152.90(19) . . ? C23 O3 C22 112.6(4) . . ? C23 O3 O2 137.1(3) . . ? C22 O3 O2 81.8(3) . . ? C25 O4 O5 119.3(4) . . ? C36 O5 O6 112.6(3) . . ? C36 O5 O4 110.1(3) . . ? O6 O5 O4 137.4(2) . . ? C47 O6 O5 117.3(4) . . ? C47 O6 O7 114.4(4) . . ? O5 O6 O7 126.45(19) . . ? C58 O7 O6 109.8(3) . . ? C68 O8 C67 109.4(4) . . ? C68 O8 N1 132.2(3) . . ? C67 O8 N1 118.3(3) . . ? O1 C1 C6 117.6(5) . . ? O1 C1 C2 123.2(5) . . ? C6 C1 C2 119.2(5) . . ? C3 C2 C1 118.6(5) . . ? C3 C2 C11 120.5(5) . . ? C1 C2 C11 120.8(5) . . ? C4 C3 C2 123.6(6) . . ? C3 C4 C5 116.8(5) . . ? C3 C4 C7 124.2(5) . . ? C5 C4 C7 119.1(5) . . ? C6 C5 C4 122.0(5) . . ? C5 C6 C1 119.7(5) . . ? C5 C6 C68 121.5(5) . . ? C1 C6 C68 118.8(5) . . ? C10 C7 C8 107.1(5) . . ? C10 C7 C9 111.0(6) . . ? C8 C7 C9 108.6(5) . . ? C10 C7 C4 110.4(5) . . ? C8 C7 C4 111.2(5) . . ? C9 C7 C4 108.5(5) . . ? C2 C11 C12 108.6(5) . . ? C17 C12 C13 117.7(6) . . ? C17 C12 C11 119.8(6) . . ? C13 C12 C11 122.3(5) . . ? C14 C13 O2 121.3(5) . . ? C14 C13 C12 121.2(6) . . ? O2 C13 C12 117.5(5) . . ? C13 C14 C15 119.3(6) . . ? C13 C14 C22 120.4(5) . . ? C15 C14 C22 120.3(5) . . ? C14 C15 C16 122.0(6) . . ? C17 C16 C15 115.7(5) . . ? C17 C16 C18 121.7(6) . . ? C15 C16 C18 122.5(6) . . ? C12 C17 C16 123.9(6) . . ? C16 C18 C21 113.5(6) . . ? C16 C18 C19 108.0(5) . . ? C21 C18 C19 108.0(6) . . ? C16 C18 C20 108.2(6) . . ? C21 C18 C20 108.7(6) . . ? C19 C18 C20 110.6(6) . . ? O3 C22 C14 107.5(5) . . ? O3 C23 C24 110.1(5) . . ? C29 C24 C25 117.9(6) . . ? C29 C24 C23 121.7(6) . . ? C25 C24 C23 120.4(5) . . ? O4 C25 C24 116.9(5) . . ? O4 C25 C26 122.9(6) . . ? C24 C25 C26 120.1(5) . . ? C27 C26 C25 117.5(6) . . ? C27 C26 C34 120.2(6) . . ? C25 C26 C34 122.0(5) . . ? C26 C27 C28 124.4(6) . . ? C29 C28 C27 115.6(5) . . ? C29 C28 C30 122.1(5) . . ? C27 C28 C30 122.2(6) . . ? C28 C29 C24 124.3(6) . . ? C31A C30 C32A 117.6(9) . . ? C33B C30 C28 116.2(8) . . ? C31A C30 C28 113.0(6) . . ? C32A C30 C28 113.5(6) . . ? C33B C30 C31B 89.4(13) . . ? C28 C30 C31B 106.1(7) . . ? C31A C30 C33A 97.4(9) . . ? C32A C30 C33A 105.0(9) . . ? C28 C30 C33A 108.2(6) . . ? C33B C30 C32B 122.7(12) . . ? C28 C30 C32B 112.0(7) . . ? C31B C30 C32B 105.5(13) . . ? C35 C34 C26 117.4(5) . . ? C36 C35 C40 118.6(6) . . ? C36 C35 C34 121.1(6) . . ? C40 C35 C34 120.2(6) . . ? O5 C36 C35 120.1(6) . . ? O5 C36 C37 119.3(5) . . ? C35 C36 C37 120.6(6) . . ? C38 C37 C36 118.5(6) . . ? C38 C37 C45 120.6(6) . . ? C36 C37 C45 120.8(6) . . ? C39 C38 C37 123.6(7) . . ? C38 C39 C40 117.7(6) . . ? C38 C39 C41 121.1(7) . . ? C40 C39 C41 121.2(6) . . ? C39 C40 C35 121.0(6) . . ? C42A C41 C43A 115.1(8) . . ? C43B C41 C44 62(3) . . ? C42A C41 C44 106.5(7) . . ? C43A C41 C44 110.1(8) . . ? C43B C41 C42B 118(3) . . ? C44 C41 C42B 142.5(14) . . ? C43B C41 C39 108.6(9) . . ? C42A C41 C39 110.4(6) . . ? C43A C41 C39 106.9(6) . . ? C44 C41 C39 107.6(7) . . ? C42B C41 C39 107.2(9) . . ? C44 C43B C41 60.1(16) . . ? C43B C44 C41 57.5(13) . . ? C37 C45 C46 114.3(5) . . ? C47 C46 C51 119.1(6) . . ? C47 C46 C45 121.0(5) . . ? C51 C46 C45 119.9(6) . . ? O6 C47 C46 121.3(5) . . ? O6 C47 C48 118.2(5) . . ? C46 C47 C48 120.5(5) . . ? C47 C48 C49 118.7(6) . . ? C47 C48 C56 121.1(5) . . ? C49 C48 C56 120.0(6) . . ? C50 C49 C48 122.4(6) . . ? C49 C50 C51 117.5(5) . . ? C49 C50 C52 123.2(5) . . ? C51 C50 C52 119.3(5) . . ? C50 C51 C46 121.8(6) . . ? C54A C52 C53A 116.0(14) . . ? C55B C52 C50 112.8(8) . . ? C54A C52 C50 113.1(8) . . ? C53A C52 C50 111.9(8) . . ? C55B C52 C53B 124.1(14) . . ? C50 C52 C53B 111.2(7) . . ? C55B C52 C54B 94.4(16) . . ? C50 C52 C54B 107.8(7) . . ? C53B C52 C54B 103.3(14) . . ? C54A C52 C55A 95.2(13) . . ? C53A C52 C55A 111.7(12) . . ? C50 C52 C55A 107.4(6) . . ? C48 C56 C57 112.1(5) . . ? C62 C57 C58 116.5(5) . . ? C62 C57 C56 120.7(5) . . ? C58 C57 C56 122.4(5) . . ? C59 C58 O7 116.9(5) . . ? C59 C58 C57 121.6(5) . . ? O7 C58 C57 121.5(5) . . ? C58 C59 C60 119.6(5) . . ? C58 C59 C67 120.2(5) . . ? C60 C59 C67 120.1(5) . . ? C61 C60 C59 122.5(6) . . ? C60 C61 C62 115.6(5) . . ? C60 C61 C63 123.8(5) . . ? C62 C61 C63 120.4(5) . . ? C57 C62 C61 124.2(5) . . ? C65 C63 C66 108.9(5) . . ? C65 C63 C61 112.3(5) . . ? C66 C63 C61 108.5(5) . . ? C65 C63 C64 107.7(5) . . ? C66 C63 C64 109.1(5) . . ? C61 C63 C64 110.3(5) . . ? O8 C67 C59 110.3(4) . . ? O8 C68 C6 109.9(4) . . ? C71 N1 C69 109.2(5) . . ? C71 N1 C73 113.2(5) . . ? C69 N1 C73 114.4(5) . . ? C71 N1 O8 105.3(3) . . ? C69 N1 O8 118.2(4) . . ? C73 N1 O8 95.9(3) . . ? C70 C69 N1 114.5(5) . . ? N1 C71 C72 114.0(5) . . ? C74 C73 N1 113.8(5) . . ? N2 C75 C76 172.4(17) . . ? C75 C76 C75 179.998(1) . 3_765 ? #===END data_5 _database_code_CSD 153524 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H125 N5 O10 U' _chemical_formula_weight 1626.94 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' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.5673(5) _cell_length_b 29.5268(16) _cell_length_c 33.0321(18) _cell_angle_alpha 90.00 _cell_angle_beta 99.590(3) _cell_angle_gamma 90.00 _cell_volume 16895(2) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 101135 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 25.68 _exptl_crystal_description 'needle-like' _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method ? _exptl_crystal_F_000 6784 _exptl_absorpt_coefficient_mu 1.979 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.631 _exptl_absorpt_correction_T_max 0.669 _exptl_absorpt_process_details ; program MULABS from PLATON (Spek, 1997) ; _exptl_special_details ; \f scans with 2\% steps ; _diffrn_ambient_temperature 110(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 101135 _diffrn_reflns_av_R_equivalents 0.139 _diffrn_reflns_av_sigmaI/netI 0.131 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.68 _reflns_number_total 29617 _reflns_number_gt 16819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and expanded by subsequent Fourier-difference synthesis. Two tert-butyl substituents and the methylenic carbon atoms of one triethylammonium cation are disordered over two positions each, which have been refined with occupation factors constrained to sum up to unity. In order to keep a number of parameters compatible with the program capacity, all non-hydrogen atoms have been refined anisotropically, except those of the aromatic rings and those in the disordered parts. The phenolic protons and those of the triethylammonium cations have not been found, nor introduced. The other hydrogen atoms were introduced at calculated positions (except those in the disordered parts) as riding atoms with displacement factors equal to 1.2 (CH, CH2) or 1.5 (CH3) times that of the parent atom. 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^)+(0.0512P)^2^+18.0262P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00023(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 29617 _refine_ls_number_parameters 1460 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.1439 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1277 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.007 _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.051 _refine_diff_density_min -1.231 _refine_diff_density_rms 0.137 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 U1 U 0.354329(17) 0.676260(11) 0.212860(10) 0.02496(10) Uani 1 1 d . . . O1A O 0.4180(3) 0.68014(19) 0.27612(17) 0.0281(14) Uani 1 1 d . . . O2A O 0.4459(3) 0.72437(19) 0.19951(18) 0.0281(14) Uani 1 1 d . . . O3A O 0.4197(3) 0.8658(2) 0.18762(18) 0.0347(15) Uani 1 1 d . . . O4A O 0.2585(3) 0.8194(2) 0.12542(18) 0.0339(15) Uani 1 1 d . . . O5A O 0.3106(3) 0.7410(2) 0.10176(17) 0.0294(14) Uani 1 1 d . . . O6A O 0.3087(3) 0.66907(19) 0.14372(17) 0.0280(14) Uani 1 1 d . . . O7A O 0.2485(3) 0.63519(19) 0.22232(17) 0.0270(14) Uani 1 1 d . . . O8A O 0.3482(3) 0.5929(2) 0.30308(18) 0.0318(15) Uani 1 1 d . . . O9A O 0.2956(3) 0.72441(19) 0.21876(18) 0.0293(14) Uani 1 1 d . . . O10A O 0.4094(3) 0.6253(2) 0.20720(17) 0.0303(15) Uani 1 1 d . . . C1A C 0.4745(5) 0.6583(3) 0.3001(3) 0.031(2) Uiso 1 1 d . . . C2A C 0.5529(4) 0.6627(3) 0.2935(3) 0.028(2) Uiso 1 1 d . . . C3A C 0.6111(5) 0.6431(3) 0.3213(3) 0.029(2) Uiso 1 1 d . . . H3A H 0.6617 0.6456 0.3166 0.035 Uiso 1 1 calc R . . C4A C 0.5976(5) 0.6197(3) 0.3561(3) 0.035(2) Uiso 1 1 d . . . C5A C 0.5219(5) 0.6139(3) 0.3608(3) 0.036(2) Uiso 1 1 d . . . H5A H 0.5110 0.5971 0.3830 0.043 Uiso 1 1 calc R . . C6A C 0.4606(5) 0.6325(3) 0.3330(3) 0.033(2) Uiso 1 1 d . . . C7A C 0.6671(5) 0.5999(4) 0.3857(3) 0.044(3) Uiso 1 1 d . . . C8A C 0.6436(5) 0.5814(4) 0.4246(3) 0.066(4) Uani 1 1 d . . . H8A1 H 0.6088 0.5564 0.4179 0.099 Uiso 1 1 calc R . . H8A2 H 0.6184 0.6047 0.4377 0.099 Uiso 1 1 calc R . . H8A3 H 0.6887 0.5712 0.4429 0.099 Uiso 1 1 calc R . . C9A C 0.7296(6) 0.6364(4) 0.3982(4) 0.077(4) Uani 1 1 d U . . H9A1 H 0.7495 0.6464 0.3744 0.116 Uiso 1 1 calc R . . H9A2 H 0.7708 0.6239 0.4177 0.116 Uiso 1 1 calc R . . H9A3 H 0.7074 0.6617 0.4104 0.116 Uiso 1 1 calc R . . C10A C 0.7024(7) 0.5612(5) 0.3641(4) 0.083(4) Uani 1 1 d . . . H10A H 0.7163 0.5722 0.3389 0.124 Uiso 1 1 calc R . . H10B H 0.6654 0.5372 0.3581 0.124 Uiso 1 1 calc R . . H10C H 0.7476 0.5500 0.3816 0.124 Uiso 1 1 calc R . . C11A C 0.5694(5) 0.6864(3) 0.2552(3) 0.033(2) Uani 1 1 d . . . H11A H 0.5384 0.6724 0.2314 0.039 Uiso 1 1 calc R . . H11B H 0.6232 0.6817 0.2530 0.039 Uiso 1 1 calc R . . C12A C 0.5532(4) 0.7368(3) 0.2539(3) 0.0244(19) Uiso 1 1 d . . . C13A C 0.4903(5) 0.7531(3) 0.2254(3) 0.031(2) Uiso 1 1 d . . . C14A C 0.4759(4) 0.7999(3) 0.2240(3) 0.0238(19) Uiso 1 1 d . . . C15A C 0.5252(4) 0.8295(3) 0.2498(3) 0.032(2) Uiso 1 1 d . . . H15A H 0.5160 0.8605 0.2479 0.038 Uiso 1 1 calc R . . C16A C 0.5872(5) 0.8135(3) 0.2780(3) 0.032(2) Uiso 1 1 d . . . C17A C 0.5982(5) 0.7668(3) 0.2793(3) 0.032(2) Uiso 1 1 d . . . H17A H 0.6384 0.7553 0.2984 0.038 Uiso 1 1 calc R . . C18A C 0.6415(5) 0.8454(4) 0.3060(3) 0.043(3) Uiso 1 1 d . . . C19A C 0.6288(7) 0.8387(4) 0.3502(3) 0.073(4) Uani 1 1 d . . . H19A H 0.6397 0.8078 0.3582 0.109 Uiso 1 1 calc R . . H19B H 0.5762 0.8457 0.3522 0.109 Uiso 1 1 calc R . . H19C H 0.6627 0.8584 0.3680 0.109 Uiso 1 1 calc R . . C20A C 0.6286(6) 0.8949(4) 0.2939(3) 0.057(3) Uani 1 1 d . . . H20A H 0.6289 0.8982 0.2651 0.085 Uiso 1 1 calc R . . H20B H 0.6691 0.9129 0.3091 0.085 Uiso 1 1 calc R . . H20C H 0.5798 0.9047 0.3001 0.085 Uiso 1 1 calc R . . C21A C 0.7263(6) 0.8340(4) 0.3036(4) 0.075(4) Uani 1 1 d . . . H21A H 0.7360 0.8027 0.3103 0.113 Uiso 1 1 calc R . . H21B H 0.7598 0.8526 0.3226 0.113 Uiso 1 1 calc R . . H21C H 0.7359 0.8396 0.2762 0.113 Uiso 1 1 calc R . . C22A C 0.4095(5) 0.8177(3) 0.1927(3) 0.032(2) Uani 1 1 d . . . H22A H 0.4084 0.8024 0.1666 0.039 Uiso 1 1 calc R . . H22B H 0.3609 0.8120 0.2020 0.039 Uiso 1 1 calc R . . C23A C 0.3513(5) 0.8886(3) 0.1665(3) 0.036(2) Uani 1 1 d . . . H23A H 0.3550 0.9207 0.1730 0.044 Uiso 1 1 calc R . . H23B H 0.3063 0.8768 0.1764 0.044 Uiso 1 1 calc R . . C24A C 0.3405(4) 0.8829(3) 0.1206(3) 0.027(2) Uiso 1 1 d . . . C25A C 0.2952(5) 0.8471(3) 0.1015(3) 0.029(2) Uiso 1 1 d . . . C26A C 0.2888(4) 0.8407(3) 0.0591(3) 0.0234(19) Uiso 1 1 d . . . C27A C 0.3235(4) 0.8715(3) 0.0363(3) 0.028(2) Uiso 1 1 d . . . H27A H 0.3183 0.8671 0.0081 0.033 Uiso 1 1 calc R . . C28A C 0.3663(4) 0.9092(3) 0.0536(3) 0.028(2) Uiso 1 1 d . . . C29A C 0.3739(4) 0.9128(3) 0.0964(3) 0.0255(19) Uiso 1 1 d . . . H29A H 0.4031 0.9366 0.1093 0.031 Uiso 1 1 calc R . . C30A C 0.4039(4) 0.9440(3) 0.0296(3) 0.030(2) Uiso 1 1 d . . . C31A C 0.3756(6) 0.9918(3) 0.0384(3) 0.048(3) Uani 1 1 d . . . H31A H 0.3965 1.0134 0.0215 0.072 Uiso 1 1 calc R . . H31B H 0.3925 0.9991 0.0668 0.072 Uiso 1 1 calc R . . H31C H 0.3202 0.9927 0.0324 0.072 Uiso 1 1 calc R . . C32A C 0.4932(5) 0.9425(3) 0.0421(3) 0.045(3) Uani 1 1 d . . . H32A H 0.5126 0.9152 0.0317 0.068 Uiso 1 1 calc R . . H32B H 0.5065 0.9430 0.0715 0.068 Uiso 1 1 calc R . . H32C H 0.5155 0.9682 0.0308 0.068 Uiso 1 1 calc R . . C33A C 0.3849(5) 0.9353(4) -0.0166(3) 0.049(3) Uani 1 1 d . . . H33A H 0.3300 0.9366 -0.0253 0.074 Uiso 1 1 calc R . . H33B H 0.4036 0.9060 -0.0227 0.074 Uiso 1 1 calc R . . H33C H 0.4092 0.9581 -0.0309 0.074 Uiso 1 1 calc R . . C34A C 0.2461(4) 0.8002(3) 0.0381(3) 0.033(2) Uani 1 1 d . . . H34A H 0.2173 0.8096 0.0118 0.040 Uiso 1 1 calc R . . H34B H 0.2093 0.7893 0.0547 0.040 Uiso 1 1 calc R . . C35A C 0.3000(4) 0.7616(3) 0.0312(3) 0.0256(19) Uiso 1 1 d . . . C36A C 0.3315(4) 0.7340(3) 0.0641(3) 0.026(2) Uiso 1 1 d . . . C37A C 0.3869(4) 0.7002(3) 0.0584(3) 0.028(2) Uiso 1 1 d . . . C38A C 0.4046(5) 0.6953(3) 0.0198(3) 0.032(2) Uiso 1 1 d . . . H38A H 0.4415 0.6738 0.0160 0.038 Uiso 1 1 calc R . . C39A C 0.3710(5) 0.7201(3) -0.0138(3) 0.032(2) Uiso 1 1 d . . . C40A C 0.3189(5) 0.7545(3) -0.0072(3) 0.033(2) Uiso 1 1 d . . . H40A H 0.2969 0.7727 -0.0290 0.040 Uiso 1 1 calc R . . C41A C 0.3897(5) 0.7107(4) -0.0573(3) 0.047(3) Uiso 1 1 d . . . C42A C 0.3506(9) 0.7457(6) -0.0912(5) 0.065(6) Uiso 0.72(2) 1 d P . . C42I C 0.415(3) 0.7617(17) -0.0741(15) 0.075(16) Uiso 0.28(2) 1 d P . . C43A C 0.3551(9) 0.6623(6) -0.0719(5) 0.073(6) Uiso 0.72(2) 1 d P . . C43I C 0.316(2) 0.6989(16) -0.0867(14) 0.068(15) Uiso 0.28(2) 1 d P . . C44A C 0.4779(8) 0.7096(6) -0.0556(5) 0.059(5) Uiso 0.72(2) 1 d P . . C44I C 0.465(2) 0.6788(17) -0.0549(13) 0.057(13) Uiso 0.28(2) 1 d P . . C45A C 0.4263(4) 0.6722(3) 0.0933(3) 0.031(2) Uani 1 1 d . . . H45A H 0.4326 0.6900 0.1183 0.037 Uiso 1 1 calc R . . H45B H 0.4772 0.6638 0.0882 0.037 Uiso 1 1 calc R . . C46A C 0.3810(4) 0.6298(3) 0.0990(3) 0.028(2) Uiso 1 1 d . . . C47A C 0.3205(4) 0.6314(3) 0.1217(3) 0.029(2) Uiso 1 1 d . . . C48A C 0.2718(5) 0.5937(3) 0.1210(3) 0.033(2) Uiso 1 1 d . . . C49A C 0.2879(5) 0.5552(3) 0.0996(3) 0.035(2) Uiso 1 1 d . . . H49A H 0.2555 0.5303 0.0995 0.042 Uiso 1 1 calc R . . C50A C 0.3494(5) 0.5520(3) 0.0785(3) 0.037(2) Uiso 1 1 d . . . C51A C 0.3945(5) 0.5910(3) 0.0779(3) 0.032(2) Uiso 1 1 d . . . H51A H 0.4349 0.5907 0.0629 0.038 Uiso 1 1 calc R . . C52A C 0.3678(6) 0.5093(4) 0.0548(3) 0.052(3) Uiso 1 1 d . . . C53A C 0.3674(10) 0.5198(6) 0.0097(6) 0.071(6) Uiso 0.705(19) 1 d P . . C53I C 0.431(2) 0.5120(14) 0.0295(12) 0.072(13) Uiso 0.295(19) 1 d P . . C54A C 0.3125(12) 0.4680(7) 0.0596(6) 0.082(7) Uiso 0.705(19) 1 d P . . C54I C 0.283(2) 0.5012(14) 0.0198(12) 0.076(14) Uiso 0.295(19) 1 d P . . C55A C 0.4538(10) 0.4933(7) 0.0733(6) 0.080(7) Uiso 0.705(19) 1 d P . . C55I C 0.3630(18) 0.4656(11) 0.0789(10) 0.048(10) Uiso 0.295(19) 1 d P . . C56A C 0.2017(4) 0.5939(3) 0.1430(3) 0.030(2) Uani 1 1 d . . . H56A H 0.1895 0.6251 0.1485 0.036 Uiso 1 1 calc R . . H56B H 0.1580 0.5816 0.1244 0.036 Uiso 1 1 calc R . . C57A C 0.2103(4) 0.5680(3) 0.1823(3) 0.0259(19) Uiso 1 1 d . . . C58A C 0.2350(4) 0.5897(3) 0.2201(3) 0.0228(19) Uiso 1 1 d . . . C59A C 0.2409(4) 0.5657(3) 0.2568(2) 0.0209(18) Uiso 1 1 d . . . C60A C 0.2229(4) 0.5198(3) 0.2555(3) 0.027(2) Uiso 1 1 d . . . H60A H 0.2255 0.5041 0.2801 0.032 Uiso 1 1 calc R . . C61A C 0.2012(4) 0.4963(3) 0.2186(3) 0.030(2) Uiso 1 1 d . . . C62A C 0.1942(4) 0.5218(3) 0.1823(3) 0.029(2) Uiso 1 1 d . . . H62A H 0.1782 0.5074 0.1573 0.035 Uiso 1 1 calc R . . C63A C 0.1808(5) 0.4455(3) 0.2178(3) 0.030(2) Uiso 1 1 d . . . C64A C 0.1759(6) 0.4253(3) 0.1749(3) 0.041(2) Uani 1 1 d . . . H64A H 0.1337 0.4389 0.1568 0.062 Uiso 1 1 calc R . . H64B H 0.1676 0.3932 0.1761 0.062 Uiso 1 1 calc R . . H64C H 0.2232 0.4310 0.1648 0.062 Uiso 1 1 calc R . . C65A C 0.1019(5) 0.4394(3) 0.2320(3) 0.044(3) Uani 1 1 d . . . H65A H 0.0865 0.4082 0.2291 0.065 Uiso 1 1 calc R . . H65B H 0.0640 0.4580 0.2154 0.065 Uiso 1 1 calc R . . H65C H 0.1063 0.4483 0.2602 0.065 Uiso 1 1 calc R . . C66A C 0.2433(5) 0.4204(3) 0.2474(3) 0.041(2) Uani 1 1 d . . . H66A H 0.2330 0.3885 0.2459 0.061 Uiso 1 1 calc R . . H66B H 0.2431 0.4309 0.2749 0.061 Uiso 1 1 calc R . . H66C H 0.2929 0.4262 0.2399 0.061 Uiso 1 1 calc R . . C67A C 0.2665(4) 0.5885(3) 0.2972(3) 0.027(2) Uani 1 1 d . . . H67A H 0.2427 0.6181 0.2973 0.032 Uiso 1 1 calc R . . H67B H 0.2513 0.5707 0.3192 0.032 Uiso 1 1 calc R . . C68A C 0.3773(4) 0.6231(3) 0.3364(3) 0.031(2) Uani 1 1 d . . . H68A H 0.3739 0.6090 0.3626 0.037 Uiso 1 1 calc R . . H68B H 0.3478 0.6510 0.3341 0.037 Uiso 1 1 calc R . . U2 U -0.171421(17) 0.792259(12) 0.124156(10) 0.02514(10) Uani 1 1 d . . . O1B O -0.1211(3) 0.8584(2) 0.14571(17) 0.0275(14) Uani 1 1 d . . . O2B O -0.0766(3) 0.76153(19) 0.16989(17) 0.0253(13) Uani 1 1 d . . . O3B O -0.1134(3) 0.7109(2) 0.28400(18) 0.0349(15) Uani 1 1 d . . . O4B O -0.2493(3) 0.6529(2) 0.21445(19) 0.0341(15) Uani 1 1 d . . . O5B O -0.1820(3) 0.6518(2) 0.14800(18) 0.0318(15) Uani 1 1 d . . . O6B O -0.2042(3) 0.72061(19) 0.09986(17) 0.0260(14) Uani 1 1 d . . . O7B O -0.2828(3) 0.81457(19) 0.08285(17) 0.0275(14) Uani 1 1 d . . . O8B O -0.1983(3) 0.9037(2) 0.06697(19) 0.0322(15) Uani 1 1 d . . . O9B O -0.2292(3) 0.7911(2) 0.16358(17) 0.0293(14) Uani 1 1 d . . . O10B O -0.1156(3) 0.7945(2) 0.08278(17) 0.0290(14) Uani 1 1 d . . . C1B C -0.0649(5) 0.8862(3) 0.1352(3) 0.030(2) Uiso 1 1 d . . . C2B C 0.0136(4) 0.8737(3) 0.1471(3) 0.027(2) Uiso 1 1 d . . . C3B C 0.0681(5) 0.9018(3) 0.1345(3) 0.027(2) Uiso 1 1 d . . . H3B H 0.1198 0.8937 0.1414 0.033 Uiso 1 1 calc R . . C4B C 0.0505(4) 0.9420(3) 0.1121(3) 0.028(2) Uiso 1 1 d . . . C5B C -0.0284(4) 0.9529(3) 0.1012(3) 0.031(2) Uiso 1 1 d . . . H5B1 H -0.0427 0.9790 0.0862 0.037 Uiso 1 1 calc R . . C6B C -0.0859(4) 0.9246(3) 0.1129(3) 0.027(2) Uiso 1 1 d . . . C7B C 0.1140(5) 0.9702(3) 0.0988(3) 0.034(2) Uiso 1 1 d . . . C8B C 0.1565(5) 0.9424(4) 0.0698(3) 0.051(3) Uani 1 1 d . . . H8B1 H 0.1974 0.9603 0.0620 0.077 Uiso 1 1 calc R . . H8B2 H 0.1208 0.9341 0.0457 0.077 Uiso 1 1 calc R . . H8B3 H 0.1778 0.9155 0.0836 0.077 Uiso 1 1 calc R . . C9B C 0.1730(6) 0.9840(4) 0.1366(3) 0.058(3) Uani 1 1 d . . . H9B1 H 0.2135 1.0014 0.1280 0.088 Uiso 1 1 calc R . . H9B2 H 0.1945 0.9572 0.1506 0.088 Uiso 1 1 calc R . . H9B3 H 0.1478 1.0018 0.1548 0.088 Uiso 1 1 calc R . . C10B C 0.0842(5) 1.0130(3) 0.0754(4) 0.058(3) Uani 1 1 d . . . H10D H 0.1270 1.0299 0.0686 0.087 Uiso 1 1 calc R . . H10E H 0.0568 1.0313 0.0923 0.087 Uiso 1 1 calc R . . H10F H 0.0502 1.0048 0.0507 0.087 Uiso 1 1 calc R . . C11B C 0.0381(5) 0.8289(3) 0.1680(3) 0.032(2) Uani 1 1 d . . . H11C H 0.0234 0.8048 0.1483 0.039 Uiso 1 1 calc R . . H11D H 0.0940 0.8287 0.1747 0.039 Uiso 1 1 calc R . . C12B C 0.0069(4) 0.8174(3) 0.2063(3) 0.0236(19) Uiso 1 1 d . . . C13B C -0.0479(4) 0.7824(3) 0.2060(3) 0.0235(19) Uiso 1 1 d . . . C14B C -0.0695(4) 0.7688(3) 0.2432(3) 0.0251(19) Uiso 1 1 d . . . C15B C -0.0392(4) 0.7905(3) 0.2792(3) 0.030(2) Uiso 1 1 d . . . H15B H -0.0548 0.7813 0.3035 0.036 Uiso 1 1 calc R . . C16B C 0.0146(4) 0.8260(3) 0.2806(3) 0.030(2) Uiso 1 1 d . . . C17B C 0.0363(5) 0.8379(3) 0.2438(3) 0.030(2) Uiso 1 1 d . . . H17B H 0.0725 0.8609 0.2439 0.036 Uiso 1 1 calc R . . C18B C 0.0459(5) 0.8473(3) 0.3224(3) 0.032(2) Uiso 1 1 d . . . C19B C 0.0811(6) 0.8113(3) 0.3530(3) 0.047(3) Uani 1 1 d . . . H19D H 0.1234 0.7969 0.3431 0.070 Uiso 1 1 calc R . . H19E H 0.0427 0.7891 0.3562 0.070 Uiso 1 1 calc R . . H19F H 0.0995 0.8252 0.3791 0.070 Uiso 1 1 calc R . . C20B C 0.1107(6) 0.8817(3) 0.3189(3) 0.052(3) Uani 1 1 d . . . H20D H 0.1290 0.8946 0.3455 0.078 Uiso 1 1 calc R . . H20E H 0.0908 0.9053 0.3001 0.078 Uiso 1 1 calc R . . H20F H 0.1524 0.8666 0.3091 0.078 Uiso 1 1 calc R . . C21B C -0.0181(6) 0.8727(4) 0.3387(3) 0.056(3) Uani 1 1 d . . . H21D H -0.0617 0.8530 0.3384 0.084 Uiso 1 1 calc R . . H21E H -0.0333 0.8985 0.3216 0.084 Uiso 1 1 calc R . . H21F H 0.0003 0.8825 0.3663 0.084 Uiso 1 1 calc R . . C22B C -0.1263(5) 0.7301(3) 0.2433(3) 0.030(2) Uani 1 1 d . . . H22C H -0.1788 0.7411 0.2364 0.036 Uiso 1 1 calc R . . H22D H -0.1180 0.7073 0.2233 0.036 Uiso 1 1 calc R . . C23B C -0.1732(5) 0.6801(3) 0.2925(3) 0.038(2) Uani 1 1 d . . . H23C H -0.2232 0.6920 0.2804 0.046 Uiso 1 1 calc R . . H23D H -0.1716 0.6783 0.3220 0.046 Uiso 1 1 calc R . . C24B C -0.1644(5) 0.6330(3) 0.2760(3) 0.031(2) Uiso 1 1 d . . . C25B C -0.2010(4) 0.6209(3) 0.2357(3) 0.028(2) Uiso 1 1 d . . . C26B C -0.1889(5) 0.5790(3) 0.2192(3) 0.031(2) Uiso 1 1 d . . . C27B C -0.1418(4) 0.5476(3) 0.2439(3) 0.031(2) Uiso 1 1 d . . . H27B H -0.1332 0.5195 0.2328 0.037 Uiso 1 1 calc R . . C28B C -0.1076(5) 0.5568(3) 0.2841(3) 0.037(2) Uiso 1 1 d . . . C29B C -0.1191(5) 0.5999(3) 0.2987(3) 0.033(2) Uiso 1 1 d . . . H29B H -0.0953 0.6072 0.3252 0.039 Uiso 1 1 calc R . . C30B C -0.0544(5) 0.5218(3) 0.3107(3) 0.039(2) Uiso 1 1 d . . . C31B C 0.0293(6) 0.5384(4) 0.3162(4) 0.060(3) Uani 1 1 d . . . H31D H 0.0613 0.5191 0.3353 0.090 Uiso 1 1 calc R . . H31E H 0.0321 0.5689 0.3265 0.090 Uiso 1 1 calc R . . H31F H 0.0469 0.5377 0.2902 0.090 Uiso 1 1 calc R . . C32B C -0.0588(6) 0.4758(3) 0.2898(3) 0.057(3) Uani 1 1 d . . . H32D H -0.1115 0.4658 0.2845 0.085 Uiso 1 1 calc R . . H32E H -0.0283 0.4544 0.3074 0.085 Uiso 1 1 calc R . . H32F H -0.0394 0.4782 0.2644 0.085 Uiso 1 1 calc R . . C33B C -0.0810(6) 0.5183(4) 0.3524(3) 0.058(3) Uani 1 1 d . . . H33D H -0.1343 0.5093 0.3484 0.087 Uiso 1 1 calc R . . H33E H -0.0752 0.5472 0.3659 0.087 Uiso 1 1 calc R . . H33F H -0.0503 0.4961 0.3690 0.087 Uiso 1 1 calc R . . C34B C -0.2215(5) 0.5661(3) 0.1760(3) 0.034(2) Uani 1 1 d . . . H34C H -0.2670 0.5843 0.1667 0.041 Uiso 1 1 calc R . . H34D H -0.2375 0.5346 0.1754 0.041 Uiso 1 1 calc R . . C35B C -0.1642(4) 0.5724(3) 0.1466(3) 0.029(2) Uiso 1 1 d . . . C36B C -0.1446(4) 0.6150(3) 0.1348(3) 0.0256(19) Uiso 1 1 d . . . C37B C -0.0890(5) 0.6216(3) 0.1097(3) 0.032(2) Uiso 1 1 d . . . C38B C -0.0578(5) 0.5824(3) 0.0944(3) 0.031(2) Uiso 1 1 d . . . H38B H -0.0221 0.5862 0.0767 0.037 Uiso 1 1 calc R . . C39B C -0.0772(5) 0.5386(3) 0.1040(3) 0.032(2) Uiso 1 1 d . . . C40B C -0.1299(5) 0.5345(3) 0.1309(3) 0.035(2) Uiso 1 1 d . . . H40B H -0.1431 0.5056 0.1387 0.042 Uiso 1 1 calc R . . C41B C -0.0469(5) 0.4986(3) 0.0837(3) 0.038(2) Uiso 1 1 d . . . C42B C -0.0981(7) 0.4912(5) 0.0420(4) 0.087(4) Uani 1 1 d U . . H42A H -0.1505 0.4867 0.0459 0.131 Uiso 1 1 calc R . . H42B H -0.0806 0.4650 0.0291 0.131 Uiso 1 1 calc R . . H42C H -0.0953 0.5173 0.0250 0.131 Uiso 1 1 calc R . . C43B C 0.0354(7) 0.5064(4) 0.0746(4) 0.078(4) Uani 1 1 d . . . H43A H 0.0511 0.4806 0.0603 0.118 Uiso 1 1 calc R . . H43B H 0.0703 0.5105 0.0999 0.118 Uiso 1 1 calc R . . H43C H 0.0359 0.5329 0.0578 0.118 Uiso 1 1 calc R . . C44B C -0.0458(9) 0.4554(4) 0.1079(4) 0.091(5) Uani 1 1 d . . . H44A H -0.0219 0.4319 0.0943 0.136 Uiso 1 1 calc R . . H44B H -0.0978 0.4467 0.1098 0.136 Uiso 1 1 calc R . . H44C H -0.0171 0.4599 0.1350 0.136 Uiso 1 1 calc R . . C45B C -0.0697(5) 0.6674(3) 0.0949(3) 0.028(2) Uani 1 1 d . . . H45C H -0.0180 0.6669 0.0882 0.033 Uiso 1 1 calc R . . H45D H -0.0704 0.6894 0.1166 0.033 Uiso 1 1 calc R . . C46B C -0.1263(4) 0.6817(3) 0.0574(3) 0.027(2) Uiso 1 1 d . . . C47B C -0.1946(4) 0.7059(3) 0.0621(3) 0.0272(19) Uiso 1 1 d . . . C48B C -0.2501(4) 0.7132(3) 0.0269(2) 0.0237(19) Uiso 1 1 d . . . C49B C -0.2363(5) 0.6974(3) -0.0110(3) 0.030(2) Uiso 1 1 d . . . H49B H -0.2739 0.7025 -0.0339 0.036 Uiso 1 1 calc R . . C50B C -0.1692(4) 0.6745(3) -0.0164(3) 0.0272(19) Uiso 1 1 d . . . C51B C -0.1156(5) 0.6673(3) 0.0190(3) 0.031(2) Uiso 1 1 d . . . H51B H -0.0703 0.6519 0.0167 0.037 Uiso 1 1 calc R . . C52B C -0.1559(5) 0.6546(3) -0.0568(3) 0.032(2) Uiso 1 1 d . . . C53B C -0.2252(5) 0.6613(4) -0.0914(3) 0.048(3) Uani 1 1 d . . . H53A H -0.2141 0.6476 -0.1162 0.073 Uiso 1 1 calc R . . H53B H -0.2344 0.6931 -0.0959 0.073 Uiso 1 1 calc R . . H53C H -0.2701 0.6474 -0.0838 0.073 Uiso 1 1 calc R . . C54B C -0.1406(7) 0.6031(4) -0.0522(3) 0.062(3) Uani 1 1 d . . . H54A H -0.0955 0.5980 -0.0319 0.093 Uiso 1 1 calc R . . H54B H -0.1325 0.5908 -0.0780 0.093 Uiso 1 1 calc R . . H54C H -0.1842 0.5886 -0.0437 0.093 Uiso 1 1 calc R . . C55B C -0.0848(5) 0.6758(4) -0.0702(3) 0.048(3) Uani 1 1 d . . . H55A H -0.0763 0.6621 -0.0955 0.073 Uiso 1 1 calc R . . H55B H -0.0405 0.6709 -0.0494 0.073 Uiso 1 1 calc R . . H55C H -0.0929 0.7078 -0.0743 0.073 Uiso 1 1 calc R . . C56B C -0.3237(4) 0.7380(3) 0.0295(3) 0.028(2) Uani 1 1 d . . . H56C H -0.3320 0.7376 0.0578 0.033 Uiso 1 1 calc R . . H56D H -0.3663 0.7218 0.0133 0.033 Uiso 1 1 calc R . . C57B C -0.3253(4) 0.7866(3) 0.0150(3) 0.027(2) Uiso 1 1 d . . . C58B C -0.3025(4) 0.8221(3) 0.0421(2) 0.0213(18) Uiso 1 1 d . . . C59B C -0.3060(4) 0.8669(3) 0.0269(3) 0.0245(19) Uiso 1 1 d . . . C60B C -0.3315(4) 0.8746(3) -0.0143(3) 0.029(2) Uiso 1 1 d . . . H60B H -0.3321 0.9042 -0.0240 0.035 Uiso 1 1 calc R . . C61B C -0.3568(5) 0.8397(3) -0.0423(3) 0.030(2) Uiso 1 1 d . . . C62B C -0.3522(4) 0.7968(3) -0.0260(3) 0.029(2) Uiso 1 1 d . . . H62B H -0.3682 0.7728 -0.0436 0.035 Uiso 1 1 calc R . . C63B C -0.3894(5) 0.8511(3) -0.0865(3) 0.039(2) Uiso 1 1 d . . . C64B C -0.4103(7) 0.8083(4) -0.1126(3) 0.063(3) Uani 1 1 d . . . H64D H -0.4327 0.8169 -0.1400 0.095 Uiso 1 1 calc R . . H64E H -0.4468 0.7905 -0.1007 0.095 Uiso 1 1 calc R . . H64F H -0.3646 0.7907 -0.1133 0.095 Uiso 1 1 calc R . . C65B C -0.3327(6) 0.8792(4) -0.1058(3) 0.063(4) Uani 1 1 d . . . H65D H -0.3540 0.8855 -0.1339 0.094 Uiso 1 1 calc R . . H65E H -0.2852 0.8627 -0.1046 0.094 Uiso 1 1 calc R . . H65F H -0.3228 0.9071 -0.0910 0.094 Uiso 1 1 calc R . . C66B C -0.4653(5) 0.8780(4) -0.0878(3) 0.056(3) Uani 1 1 d . . . H66D H -0.4868 0.8849 -0.1158 0.084 Uiso 1 1 calc R . . H66E H -0.4548 0.9057 -0.0726 0.084 Uiso 1 1 calc R . . H66F H -0.5014 0.8602 -0.0758 0.084 Uiso 1 1 calc R . . C67B C -0.2800(4) 0.9050(3) 0.0557(3) 0.032(2) Uani 1 1 d . . . H67C H -0.2957 0.9336 0.0426 0.039 Uiso 1 1 calc R . . H67D H -0.3039 0.9023 0.0801 0.039 Uiso 1 1 calc R . . C68B C -0.1691(4) 0.9352(3) 0.0987(3) 0.031(2) Uani 1 1 d . . . H68C H -0.1976 0.9326 0.1214 0.037 Uiso 1 1 calc R . . H68D H -0.1747 0.9660 0.0882 0.037 Uiso 1 1 calc R . . N1 N 0.5031(4) 0.5522(3) 0.2271(3) 0.041(2) Uani 1 1 d . . . N2 N -0.0422(4) 0.8168(3) 0.0210(2) 0.0349(19) Uani 1 1 d . . . N3 N 0.1078(4) 0.6792(3) 0.2157(2) 0.042(2) Uani 1 1 d . . . N4 N 0.5852(4) 0.8004(3) 0.1191(2) 0.0322(19) Uani 1 1 d . . . N5 N 1.1177(9) 0.7634(7) -0.0498(5) 0.155(6) Uani 1 1 d U . . N6 N 0.8189(6) 0.9545(4) 0.2793(4) 0.078(3) Uani 1 1 d . . . N7 N 0.5706(11) 0.6131(6) 0.0237(7) 0.183(9) Uani 1 1 d . . . N8 N 1.3183(7) 0.7346(4) 0.3596(4) 0.089(4) Uani 1 1 d . . . N9 N 0.244(2) 0.5702(16) -0.0860(10) 0.45(3) Uani 1 1 d . . . N10 N 0.0841(6) 0.6259(4) 0.0326(4) 0.105(5) Uani 1 1 d . . . C1 C 0.4697(5) 0.5180(4) 0.1955(3) 0.050(3) Uani 1 1 d . . . H1A H 0.5016 0.4911 0.1987 0.059 Uiso 1 1 calc R . . H1B H 0.4709 0.5303 0.1684 0.059 Uiso 1 1 calc R . . C2 C 0.3878(5) 0.5050(4) 0.1986(4) 0.065(4) Uani 1 1 d . . . H2A H 0.3881 0.4823 0.2194 0.098 Uiso 1 1 calc R . . H2B H 0.3628 0.4933 0.1727 0.098 Uiso 1 1 calc R . . H2C H 0.3604 0.5313 0.2056 0.098 Uiso 1 1 calc R . . C3 C 0.5015(7) 0.5385(4) 0.2715(4) 0.064(4) Uani 1 1 d . . . H3C H 0.5272 0.5618 0.2895 0.077 Uiso 1 1 calc R . . H3D H 0.4481 0.5373 0.2757 0.077 Uiso 1 1 calc R . . C4 C 0.5388(8) 0.4939(4) 0.2838(4) 0.085(4) Uani 1 1 d . . . H4A H 0.5132 0.4704 0.2666 0.128 Uiso 1 1 calc R . . H4C H 0.5349 0.4877 0.3119 0.128 Uiso 1 1 calc R . . H4D H 0.5922 0.4950 0.2809 0.128 Uiso 1 1 calc R . . C5 C 0.5818(5) 0.5687(4) 0.2203(4) 0.057(3) Uani 1 1 d . . . H5C H 0.6170 0.5432 0.2216 0.069 Uiso 1 1 calc R . . H5D H 0.6024 0.5899 0.2417 0.069 Uiso 1 1 calc R . . C6 C 0.5755(6) 0.5916(4) 0.1787(4) 0.070(4) Uani 1 1 d . . . H6A H 0.5730 0.5690 0.1576 0.105 Uiso 1 1 calc R . . H6B H 0.6199 0.6105 0.1783 0.105 Uiso 1 1 calc R . . H6C H 0.5297 0.6099 0.1738 0.105 Uiso 1 1 calc R . . C7 C -0.0476(6) 0.8678(4) 0.0223(3) 0.051(3) Uani 1 1 d . . . H7A H -0.1016 0.8764 0.0186 0.062 Uiso 1 1 calc R . . H7B H -0.0233 0.8782 0.0492 0.062 Uiso 1 1 calc R . . C8 C -0.0108(7) 0.8912(4) -0.0095(4) 0.068(4) Uani 1 1 d . . . H8A H -0.0134 0.9233 -0.0058 0.102 Uiso 1 1 calc R . . H8B H -0.0376 0.8832 -0.0363 0.102 Uiso 1 1 calc R . . H8C H 0.0422 0.8820 -0.0069 0.102 Uiso 1 1 calc R . . C9 C 0.0401(5) 0.8024(3) 0.0357(3) 0.040(3) Uani 1 1 d . . . H9A H 0.0599 0.8180 0.0611 0.048 Uiso 1 1 calc R . . H9B H 0.0716 0.8108 0.0155 0.048 Uiso 1 1 calc R . . C10 C 0.0453(5) 0.7518(4) 0.0428(4) 0.060(3) Uani 1 1 d . . . H10G H 0.0982 0.7434 0.0517 0.090 Uiso 1 1 calc R . . H10H H 0.0257 0.7363 0.0177 0.090 Uiso 1 1 calc R . . H10I H 0.0153 0.7435 0.0634 0.090 Uiso 1 1 calc R . . C11 C -0.0745(6) 0.7962(4) -0.0186(3) 0.055(3) Uani 1 1 d . . . H11E H -0.0748 0.7635 -0.0157 0.066 Uiso 1 1 calc R . . H11F H -0.0419 0.8036 -0.0387 0.066 Uiso 1 1 calc R . . C12 C -0.1567(5) 0.8127(4) -0.0342(3) 0.057(3) Uani 1 1 d . . . H12A H -0.1788 0.7954 -0.0579 0.085 Uiso 1 1 calc R . . H12B H -0.1555 0.8441 -0.0415 0.085 Uiso 1 1 calc R . . H12C H -0.1875 0.8090 -0.0130 0.085 Uiso 1 1 calc R . . C13 C 0.0937(6) 0.6851(5) 0.2571(3) 0.076(5) Uani 1 1 d . . . H13A H 0.0946 0.6558 0.2705 0.092 Uiso 1 1 calc R . . H13B H 0.0430 0.6983 0.2566 0.092 Uiso 1 1 calc R . . C14 C 0.1582(7) 0.7174(4) 0.2823(4) 0.068(4) Uani 1 1 d . . . H14A H 0.1557 0.7153 0.3111 0.102 Uiso 1 1 calc R . . H14B H 0.1491 0.7481 0.2733 0.102 Uiso 1 1 calc R . . H14C H 0.2084 0.7080 0.2777 0.102 Uiso 1 1 calc R . . C15 C 0.1112(6) 0.7223(4) 0.1927(4) 0.062(4) Uani 1 1 d . . . H15C H 0.1493 0.7419 0.2086 0.074 Uiso 1 1 calc R . . H15D H 0.0615 0.7373 0.1905 0.074 Uiso 1 1 calc R . . C16 C 0.1309(5) 0.7176(3) 0.1502(3) 0.040(3) Uani 1 1 d . . . H16A H 0.1381 0.7471 0.1392 0.060 Uiso 1 1 calc R . . H16B H 0.0896 0.7023 0.1328 0.060 Uiso 1 1 calc R . . H16C H 0.1776 0.7004 0.1515 0.060 Uiso 1 1 calc R . . C17 C 0.0442(6) 0.6498(4) 0.1914(4) 0.065(4) Uani 1 1 d . . . H17C H 0.0588 0.6417 0.1653 0.078 Uiso 1 1 calc R . . H17D H -0.0033 0.6671 0.1858 0.078 Uiso 1 1 calc R . . C18 C 0.0300(5) 0.6063(4) 0.2146(3) 0.056(3) Uani 1 1 d . . . H18A H 0.0783 0.5915 0.2240 0.085 Uiso 1 1 calc R . . H18B H -0.0032 0.5865 0.1966 0.085 Uiso 1 1 calc R . . H18C H 0.0059 0.6139 0.2378 0.085 Uiso 1 1 calc R . . C19I C 0.6011(8) 0.7677(6) 0.1562(5) 0.042(4) Uiso 0.647(15) 1 d P . . C19J C 0.5599(14) 0.7554(10) 0.1252(8) 0.044(8) Uiso 0.353(15) 1 d P . . C20 C 0.6258(5) 0.7220(3) 0.1483(3) 0.040(2) Uani 1 1 d . . . C21I C 0.5666(8) 0.8464(5) 0.1303(5) 0.039(4) Uiso 0.647(15) 1 d P . . C21J C 0.6012(13) 0.8265(9) 0.1617(8) 0.035(7) Uiso 0.353(15) 1 d P . . C22 C 0.6339(6) 0.8703(4) 0.1600(3) 0.054(3) Uani 1 1 d . . . C23I C 0.5222(7) 0.7781(5) 0.0872(5) 0.036(4) Uiso 0.647(15) 1 d P . . C23J C 0.5218(14) 0.8292(9) 0.0908(8) 0.042(8) Uiso 0.353(15) 1 d P . . C24 C 0.4984(5) 0.8085(3) 0.0493(3) 0.043(3) Uani 1 1 d . . . C25 C 1.0789(9) 0.7677(6) -0.0825(6) 0.102(5) Uani 1 1 d U . . C26 C 1.0306(7) 0.7647(4) -0.1203(4) 0.069(4) Uani 1 1 d . . . H26A H 0.9882 0.7853 -0.1209 0.104 Uiso 1 1 calc R . . H26B H 1.0113 0.7343 -0.1243 0.104 Uiso 1 1 calc R . . H26C H 1.0591 0.7723 -0.1418 0.104 Uiso 1 1 calc R . . C27 C 0.8268(6) 0.9263(4) 0.2572(4) 0.048(3) Uani 1 1 d . . . C28 C 0.8392(6) 0.8896(4) 0.2292(3) 0.060(3) Uani 1 1 d . . . H28A H 0.7917 0.8832 0.2111 0.090 Uiso 1 1 calc R . . H28B H 0.8562 0.8630 0.2448 0.090 Uiso 1 1 calc R . . H28C H 0.8777 0.8985 0.2133 0.090 Uiso 1 1 calc R . . C29 C 0.6395(11) 0.6054(6) 0.0419(6) 0.111(6) Uani 1 1 d U . . C30 C 0.7179(8) 0.5969(5) 0.0493(5) 0.101(5) Uani 1 1 d U . . H30A H 0.7273 0.5666 0.0408 0.152 Uiso 1 1 calc R . . H30B H 0.7372 0.6001 0.0781 0.152 Uiso 1 1 calc R . . H30C H 0.7438 0.6180 0.0341 0.152 Uiso 1 1 calc R . . C31 C 1.3414(8) 0.7546(5) 0.3344(5) 0.073(4) Uani 1 1 d . . . C32 C 1.3725(7) 0.7816(4) 0.3045(4) 0.071(4) Uani 1 1 d . . . H32G H 1.3407 0.7781 0.2781 0.107 Uiso 1 1 calc R . . H32H H 1.4241 0.7717 0.3031 0.107 Uiso 1 1 calc R . . H32I H 1.3735 0.8129 0.3125 0.107 Uiso 1 1 calc R . . C33 C 0.2986(17) 0.5546(10) -0.1033(9) 0.176(10) Uani 1 1 d U . . C34 C 0.3641(15) 0.5262(10) -0.1128(8) 0.229(12) Uani 1 1 d U . . H34E H 0.4121 0.5389 -0.0995 0.343 Uiso 1 1 calc R . . H34F H 0.3632 0.5257 -0.1419 0.343 Uiso 1 1 calc R . . H34G H 0.3591 0.4959 -0.1030 0.343 Uiso 1 1 calc R . . C35 C 0.1413(6) 0.6322(4) 0.0228(4) 0.062(4) Uani 1 1 d . . . C36 C 0.2150(6) 0.6383(4) 0.0099(4) 0.068(4) Uani 1 1 d . . . H36A H 0.2552 0.6272 0.0308 0.102 Uiso 1 1 calc R . . H36B H 0.2232 0.6699 0.0054 0.102 Uiso 1 1 calc R . . H36C H 0.2157 0.6219 -0.0152 0.102 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.02623(17) 0.02106(19) 0.0275(2) 0.00108(16) 0.00436(13) 0.00037(14) O1A 0.038(3) 0.023(4) 0.023(3) -0.002(3) 0.001(2) 0.001(3) O2A 0.032(3) 0.018(3) 0.034(4) -0.001(3) 0.005(3) 0.001(2) O3A 0.044(4) 0.025(4) 0.032(4) 0.003(3) -0.002(3) 0.004(3) O4A 0.037(3) 0.034(4) 0.034(4) 0.006(3) 0.014(3) 0.002(3) O5A 0.037(3) 0.028(4) 0.025(4) -0.003(3) 0.011(3) 0.001(3) O6A 0.034(3) 0.020(4) 0.031(4) -0.005(3) 0.010(3) 0.004(3) O7A 0.024(3) 0.023(4) 0.034(4) 0.005(3) 0.003(2) -0.001(2) O8A 0.017(3) 0.035(4) 0.043(4) -0.008(3) 0.003(2) -0.002(3) O9A 0.030(3) 0.022(4) 0.036(4) 0.000(3) 0.004(3) -0.001(2) O10A 0.031(3) 0.032(4) 0.027(4) -0.003(3) 0.005(3) -0.004(3) C8A 0.037(6) 0.094(11) 0.063(8) 0.047(7) -0.002(5) 0.001(6) C9A 0.060(6) 0.077(7) 0.085(8) 0.031(6) -0.016(5) -0.013(6) C10A 0.065(8) 0.095(12) 0.087(11) 0.043(9) 0.006(7) 0.030(7) C11A 0.031(5) 0.030(6) 0.038(6) -0.009(4) 0.005(4) -0.001(4) C19A 0.109(10) 0.061(9) 0.040(8) -0.023(6) -0.011(7) -0.028(7) C20A 0.068(7) 0.035(7) 0.059(8) -0.002(6) -0.014(6) -0.006(5) C21A 0.046(7) 0.056(9) 0.118(12) -0.005(8) -0.007(7) -0.007(6) C22A 0.032(5) 0.032(6) 0.032(6) 0.001(4) 0.004(4) -0.006(4) C23A 0.057(6) 0.027(6) 0.024(6) 0.004(4) 0.006(4) 0.010(4) C31A 0.069(7) 0.032(7) 0.047(7) 0.009(5) 0.017(5) 0.007(5) C32A 0.042(5) 0.038(7) 0.055(7) 0.000(5) 0.003(5) -0.006(5) C33A 0.048(6) 0.063(8) 0.037(7) 0.004(6) 0.007(5) -0.024(5) C34A 0.027(5) 0.040(6) 0.032(6) 0.013(5) 0.002(4) -0.003(4) C45A 0.027(4) 0.029(6) 0.036(6) -0.007(4) 0.007(4) -0.004(4) C56A 0.027(4) 0.026(6) 0.035(6) 0.003(4) -0.004(4) -0.004(4) C64A 0.070(7) 0.020(6) 0.034(6) -0.002(4) 0.010(5) -0.011(5) C65A 0.050(6) 0.033(6) 0.048(7) 0.002(5) 0.010(5) -0.015(5) C66A 0.047(6) 0.029(6) 0.050(7) -0.004(5) 0.019(5) -0.004(4) C67A 0.027(4) 0.025(5) 0.032(6) 0.013(4) 0.015(4) 0.009(4) C68A 0.033(5) 0.042(6) 0.018(5) -0.001(4) 0.006(4) -0.010(4) U2 0.02445(17) 0.0237(2) 0.0273(2) -0.00116(16) 0.00433(12) 0.00051(14) O1B 0.025(3) 0.028(4) 0.030(4) 0.003(3) 0.007(2) 0.007(3) O2B 0.028(3) 0.023(4) 0.025(4) 0.004(3) 0.007(2) 0.002(2) O3B 0.041(3) 0.032(4) 0.031(4) 0.007(3) 0.003(3) -0.014(3) O4B 0.034(3) 0.032(4) 0.037(4) 0.002(3) 0.007(3) 0.002(3) O5B 0.039(3) 0.019(4) 0.037(4) 0.004(3) 0.006(3) 0.011(3) O6B 0.031(3) 0.023(4) 0.023(3) -0.001(3) 0.005(2) 0.005(2) O7B 0.027(3) 0.027(4) 0.028(4) 0.001(3) 0.003(2) 0.002(2) O8B 0.025(3) 0.028(4) 0.043(4) -0.006(3) 0.002(3) 0.002(3) O9B 0.037(3) 0.020(4) 0.033(4) -0.002(3) 0.011(3) 0.001(3) O10B 0.037(3) 0.025(4) 0.027(4) -0.001(3) 0.008(3) 0.001(3) C8B 0.045(6) 0.038(7) 0.074(9) 0.004(6) 0.016(5) 0.002(5) C9B 0.063(7) 0.053(8) 0.054(8) -0.003(6) -0.006(6) -0.027(6) C10B 0.047(6) 0.030(7) 0.099(10) 0.027(6) 0.016(6) -0.004(5) C11B 0.033(5) 0.028(6) 0.037(6) 0.016(5) 0.008(4) 0.003(4) C19B 0.059(6) 0.043(7) 0.034(6) 0.003(5) -0.006(5) -0.006(5) C20B 0.086(8) 0.037(7) 0.027(6) 0.000(5) -0.006(5) -0.035(6) C21B 0.074(7) 0.047(8) 0.043(7) -0.016(6) -0.002(6) -0.004(6) C22B 0.029(5) 0.031(6) 0.027(6) 0.003(4) 0.000(4) -0.001(4) C23B 0.048(6) 0.029(6) 0.041(6) 0.000(5) 0.017(4) -0.007(5) C31B 0.058(7) 0.045(8) 0.072(9) -0.009(6) -0.003(6) 0.007(6) C32B 0.075(7) 0.033(7) 0.059(8) 0.017(6) 0.001(6) 0.012(5) C33B 0.063(7) 0.057(8) 0.050(8) 0.017(6) 0.000(6) 0.003(6) C34B 0.039(5) 0.037(6) 0.023(5) 0.005(4) -0.002(4) -0.003(4) C42B 0.103(7) 0.072(8) 0.080(8) -0.039(6) -0.005(6) 0.017(6) C43B 0.077(8) 0.050(9) 0.115(12) -0.024(8) 0.036(8) 0.012(7) C44B 0.174(14) 0.037(8) 0.077(10) 0.023(7) 0.067(10) 0.047(9) C45B 0.034(5) 0.021(5) 0.026(5) 0.005(4) 0.001(4) 0.009(4) C53B 0.056(6) 0.051(8) 0.038(7) -0.014(5) 0.006(5) 0.011(5) C54B 0.096(9) 0.036(7) 0.050(8) -0.009(6) 0.002(6) 0.030(6) C55B 0.047(6) 0.071(8) 0.030(6) 0.008(6) 0.015(5) -0.001(5) C56B 0.030(5) 0.031(6) 0.019(5) -0.004(4) -0.005(4) -0.004(4) C64B 0.086(8) 0.056(9) 0.044(8) 0.002(6) 0.000(6) 0.019(6) C65B 0.059(7) 0.081(10) 0.048(8) 0.030(7) 0.007(6) -0.007(6) C66B 0.055(6) 0.066(9) 0.041(7) 0.003(6) -0.010(5) 0.015(6) C67B 0.032(5) 0.024(6) 0.039(6) 0.002(4) 0.002(4) 0.002(4) C68B 0.035(5) 0.013(5) 0.044(6) 0.002(4) 0.006(4) -0.004(4) N1 0.046(5) 0.028(5) 0.047(6) -0.004(4) 0.002(4) 0.003(4) N2 0.029(4) 0.028(5) 0.048(5) -0.003(4) 0.008(3) 0.008(3) N3 0.030(4) 0.054(6) 0.045(6) 0.018(5) 0.010(4) 0.011(4) N4 0.027(4) 0.037(5) 0.032(5) 0.008(4) 0.003(3) -0.002(3) N5 0.125(9) 0.209(11) 0.132(9) -0.024(8) 0.024(7) -0.001(8) N6 0.088(8) 0.063(8) 0.085(9) -0.010(7) 0.023(6) 0.000(6) N7 0.155(15) 0.102(14) 0.31(3) -0.062(15) 0.094(16) 0.000(11) N8 0.136(10) 0.061(9) 0.078(10) -0.016(7) 0.043(8) -0.016(7) N9 0.38(4) 0.73(8) 0.26(4) 0.07(4) 0.10(3) 0.27(5) N10 0.073(8) 0.086(10) 0.167(14) 0.044(9) 0.046(8) 0.030(7) C1 0.048(6) 0.043(7) 0.058(8) -0.003(6) 0.011(5) -0.004(5) C2 0.042(6) 0.030(7) 0.120(12) -0.005(7) 0.004(6) 0.002(5) C3 0.074(8) 0.041(8) 0.073(10) -0.009(7) 0.000(6) 0.027(6) C4 0.108(10) 0.067(10) 0.079(11) -0.006(8) 0.011(8) 0.035(8) C5 0.029(5) 0.050(8) 0.094(10) -0.017(7) 0.014(5) -0.005(5) C6 0.060(7) 0.065(9) 0.096(11) -0.026(8) 0.044(7) -0.014(6) C7 0.061(7) 0.036(7) 0.055(8) -0.011(6) 0.001(5) 0.002(5) C8 0.093(9) 0.029(7) 0.075(10) 0.009(6) -0.005(7) -0.010(6) C9 0.037(5) 0.038(7) 0.048(7) 0.008(5) 0.013(4) 0.001(4) C10 0.042(6) 0.059(9) 0.075(9) 0.032(7) 0.000(5) 0.003(5) C11 0.055(7) 0.052(8) 0.059(8) -0.008(6) 0.011(5) -0.001(6) C12 0.044(6) 0.081(10) 0.046(7) -0.007(6) 0.011(5) 0.012(6) C13 0.051(7) 0.138(14) 0.042(8) 0.007(8) 0.011(5) 0.054(8) C14 0.081(8) 0.063(9) 0.065(9) -0.019(7) 0.027(7) 0.008(7) C15 0.047(6) 0.069(9) 0.074(9) 0.030(7) 0.024(6) 0.028(6) C16 0.030(5) 0.041(7) 0.046(7) 0.011(5) -0.001(4) 0.002(4) C17 0.055(7) 0.073(10) 0.060(9) 0.010(7) -0.014(6) -0.001(6) C18 0.025(5) 0.069(9) 0.073(9) 0.043(7) 0.001(5) -0.006(5) C20 0.042(5) 0.034(6) 0.044(7) 0.008(5) 0.009(4) -0.006(4) C22 0.051(6) 0.057(8) 0.049(7) -0.013(6) -0.005(5) 0.011(5) C24 0.045(6) 0.034(6) 0.049(7) 0.002(5) 0.006(5) 0.002(4) C25 0.083(8) 0.136(10) 0.091(9) -0.003(8) 0.022(7) 0.010(7) C26 0.080(8) 0.071(10) 0.051(8) 0.003(7) -0.004(6) 0.017(7) C27 0.049(6) 0.053(8) 0.046(8) -0.007(6) 0.016(5) -0.001(5) C28 0.047(6) 0.083(10) 0.049(8) -0.013(7) 0.007(5) 0.012(6) C29 0.105(8) 0.099(9) 0.136(10) -0.018(8) 0.042(8) -0.013(8) C30 0.094(7) 0.095(7) 0.101(7) 0.009(6) -0.024(5) -0.018(6) C31 0.096(10) 0.045(9) 0.077(11) -0.019(8) 0.014(8) -0.003(7) C32 0.106(10) 0.054(9) 0.059(9) -0.005(7) 0.026(7) -0.009(7) C33 0.174(12) 0.169(13) 0.178(13) -0.011(9) 0.014(9) -0.003(9) C34 0.223(14) 0.240(15) 0.226(15) -0.005(10) 0.049(10) -0.001(10) C35 0.042(7) 0.074(10) 0.077(10) 0.000(7) 0.025(6) 0.007(6) C36 0.045(6) 0.085(10) 0.072(9) -0.022(8) 0.006(6) -0.017(6) _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 U1 O9A 1.786(5) . ? U1 O10A 1.815(6) . ? U1 O1A 2.203(5) . ? U1 O2A 2.244(5) . ? U1 O7A 2.285(5) . ? U1 O6A 2.301(6) . ? O1A C1A 1.329(10) . ? O2A C13A 1.356(10) . ? O3A C22A 1.446(10) . ? O3A C23A 1.451(10) . ? O4A C25A 1.372(10) . ? O5A C36A 1.371(10) . ? O6A C47A 1.364(10) . ? O7A C58A 1.362(10) . ? O8A C67A 1.422(9) . ? O8A C68A 1.442(10) . ? C1A C6A 1.383(12) . ? C1A C2A 1.435(11) . ? C2A C3A 1.382(11) . ? C2A C11A 1.516(12) . ? C3A C4A 1.393(12) . ? C4A C5A 1.376(11) . ? C4A C7A 1.548(12) . ? C5A C6A 1.405(12) . ? C6A C68A 1.512(11) . ? C7A C8A 1.518(13) . ? C7A C10A 1.532(15) . ? C7A C9A 1.545(14) . ? C11A C12A 1.515(11) . ? C12A C17A 1.376(11) . ? C12A C13A 1.411(11) . ? C13A C14A 1.405(12) . ? C14A C15A 1.412(11) . ? C14A C22A 1.518(11) . ? C15A C16A 1.394(11) . ? C16A C17A 1.390(12) . ? C16A C18A 1.535(13) . ? C18A C20A 1.521(14) . ? C18A C19A 1.525(14) . ? C18A C21A 1.542(13) . ? C23A C24A 1.506(12) . ? C24A C29A 1.385(11) . ? C24A C25A 1.406(11) . ? C25A C26A 1.401(11) . ? C26A C27A 1.385(11) . ? C26A C34A 1.518(11) . ? C27A C28A 1.409(11) . ? C28A C29A 1.402(11) . ? C28A C30A 1.515(12) . ? C30A C33A 1.528(12) . ? C30A C31A 1.541(12) . ? C30A C32A 1.554(11) . ? C34A C35A 1.522(12) . ? C35A C40A 1.379(12) . ? C35A C36A 1.395(11) . ? C36A C37A 1.428(11) . ? C37A C38A 1.371(12) . ? C37A C45A 1.492(12) . ? C38A C39A 1.378(12) . ? C39A C40A 1.409(12) . ? C39A C41A 1.550(13) . ? C41A C43I 1.53(4) . ? C41A C44A 1.541(17) . ? C41A C42A 1.592(19) . ? C41A C44I 1.61(4) . ? C41A C43A 1.60(2) . ? C41A C42I 1.69(5) . ? C45A C46A 1.511(11) . ? C46A C51A 1.383(12) . ? C46A C47A 1.400(11) . ? C47A C48A 1.402(12) . ? C48A C49A 1.390(12) . ? C48A C56A 1.530(11) . ? C49A C50A 1.383(12) . ? C50A C51A 1.399(12) . ? C50A C52A 1.547(14) . ? C52A C53I 1.50(4) . ? C52A C53A 1.52(2) . ? C52A C55I 1.53(3) . ? C52A C54A 1.58(2) . ? C52A C55A 1.60(2) . ? C52A C54I 1.75(4) . ? C56A C57A 1.494(11) . ? C57A C62A 1.393(12) . ? C57A C58A 1.407(11) . ? C58A C59A 1.394(11) . ? C59A C60A 1.390(11) . ? C59A C67A 1.494(11) . ? C60A C61A 1.398(11) . ? C61A C62A 1.405(12) . ? C61A C63A 1.543(12) . ? C63A C64A 1.526(12) . ? C63A C66A 1.533(12) . ? C63A C65A 1.546(11) . ? U2 O9B 1.780(5) . ? U2 O10B 1.811(5) . ? U2 O1B 2.213(6) . ? U2 O2B 2.246(5) . ? U2 O7B 2.288(5) . ? U2 O6B 2.301(6) . ? O1B C1B 1.371(10) . ? O2B C13B 1.364(9) . ? O3B C22B 1.440(10) . ? O3B C23B 1.453(10) . ? O4B C25B 1.380(10) . ? O5B C36B 1.377(10) . ? O6B C47B 1.358(10) . ? O7B C58B 1.350(9) . ? O8B C67B 1.423(9) . ? O8B C68B 1.432(10) . ? C1B C6B 1.368(12) . ? C1B C2B 1.420(11) . ? C2B C3B 1.382(11) . ? C2B C11B 1.522(11) . ? C3B C4B 1.405(12) . ? C4B C5B 1.409(11) . ? C4B C7B 1.516(12) . ? C5B C6B 1.414(11) . ? C6B C68B 1.492(11) . ? C7B C10B 1.526(13) . ? C7B C9B 1.538(12) . ? C7B C8B 1.547(13) . ? C11B C12B 1.499(11) . ? C12B C17B 1.398(11) . ? C12B C13B 1.409(11) . ? C13B C14B 1.404(11) . ? C14B C15B 1.377(11) . ? C14B C22B 1.518(11) . ? C15B C16B 1.406(12) . ? C16B C17B 1.378(12) . ? C16B C18B 1.536(12) . ? C18B C21B 1.523(13) . ? C18B C19B 1.524(12) . ? C18B C20B 1.543(12) . ? C23B C24B 1.509(12) . ? C24B C29B 1.397(12) . ? C24B C25B 1.424(12) . ? C25B C26B 1.385(12) . ? C26B C27B 1.406(12) . ? C26B C34B 1.497(12) . ? C27B C28B 1.390(12) . ? C28B C29B 1.390(12) . ? C28B C30B 1.561(13) . ? C30B C32B 1.518(13) . ? C30B C33B 1.531(14) . ? C30B C31B 1.532(13) . ? C34B C35B 1.522(12) . ? C35B C36B 1.378(12) . ? C35B C40B 1.413(12) . ? C36B C37B 1.397(11) . ? C37B C38B 1.408(12) . ? C37B C45B 1.497(12) . ? C38B C39B 1.388(12) . ? C39B C40B 1.392(12) . ? C39B C41B 1.499(13) . ? C41B C44B 1.504(14) . ? C41B C42B 1.529(14) . ? C41B C43B 1.543(13) . ? C45B C46B 1.512(11) . ? C46B C51B 1.380(11) . ? C46B C47B 1.426(11) . ? C47B C48B 1.404(11) . ? C48B C49B 1.393(11) . ? C48B C56B 1.502(11) . ? C49B C50B 1.397(11) . ? C50B C51B 1.391(11) . ? C50B C52B 1.509(12) . ? C52B C55B 1.530(12) . ? C52B C53B 1.538(12) . ? C52B C54B 1.547(13) . ? C56B C57B 1.513(12) . ? C57B C62B 1.388(11) . ? C57B C58B 1.395(11) . ? C58B C59B 1.412(11) . ? C59B C60B 1.379(11) . ? C59B C67B 1.494(11) . ? C60B C61B 1.407(12) . ? C61B C62B 1.374(12) . ? C61B C63B 1.516(12) . ? C63B C65B 1.516(13) . ? C63B C64B 1.539(14) . ? C63B C66B 1.547(13) . ? N1 C1 1.499(12) . ? N1 C5 1.518(11) . ? N1 C3 1.526(13) . ? N2 C11 1.469(12) . ? N2 C7 1.509(12) . ? N2 C9 1.507(11) . ? N3 C13 1.439(12) . ? N3 C15 1.488(12) . ? N3 C17 1.533(13) . ? N4 C19J 1.43(3) . ? N4 C21I 1.459(16) . ? N4 C23I 1.542(15) . ? N4 C19I 1.548(17) . ? N4 C23J 1.58(3) . ? N4 C21J 1.59(3) . ? N5 C25 1.183(19) . ? N6 C27 1.133(13) . ? N7 C29 1.28(2) . ? N8 C31 1.151(16) . ? N9 C33 1.28(3) . ? N10 C35 1.122(13) . ? C1 C2 1.508(13) . ? C3 C4 1.496(15) . ? C5 C6 1.520(15) . ? C7 C8 1.491(14) . ? C9 C10 1.514(13) . ? C11 C12 1.531(13) . ? C13 C14 1.605(16) . ? C15 C16 1.508(14) . ? C17 C18 1.536(14) . ? C19I C20 1.454(18) . ? C19J C20 1.61(3) . ? C21I C22 1.573(17) . ? C21J C22 1.42(3) . ? C23I C24 1.541(17) . ? C23J C24 1.49(3) . ? C25 C26 1.391(19) . ? C27 C28 1.463(15) . ? C29 C30 1.38(2) . ? C31 C32 1.445(18) . ? C33 C34 1.50(3) . ? C35 C36 1.440(14) . ? 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 O9A U1 O10A 176.8(2) . . ? O9A U1 O1A 93.8(2) . . ? O10A U1 O1A 86.9(2) . . ? O9A U1 O2A 87.9(2) . . ? O10A U1 O2A 95.3(2) . . ? O1A U1 O2A 83.5(2) . . ? O9A U1 O7A 84.8(2) . . ? O10A U1 O7A 91.9(2) . . ? O1A U1 O7A 101.2(2) . . ? O2A U1 O7A 171.56(19) . . ? O9A U1 O6A 94.0(2) . . ? O10A U1 O6A 85.7(2) . . ? O1A U1 O6A 169.88(19) . . ? O2A U1 O6A 90.4(2) . . ? O7A U1 O6A 85.96(19) . . ? C1A O1A U1 138.6(5) . . ? C13A O2A U1 128.8(5) . . ? C22A O3A C23A 113.8(6) . . ? C47A O6A U1 123.1(5) . . ? C58A O7A U1 130.8(5) . . ? C67A O8A C68A 112.4(6) . . ? O1A C1A C6A 121.5(7) . . ? O1A C1A C2A 120.5(8) . . ? C6A C1A C2A 118.0(8) . . ? C3A C2A C1A 119.0(8) . . ? C3A C2A C11A 121.7(7) . . ? C1A C2A C11A 119.3(7) . . ? C2A C3A C4A 123.1(8) . . ? C5A C4A C3A 117.2(8) . . ? C5A C4A C7A 123.8(9) . . ? C3A C4A C7A 118.9(7) . . ? C4A C5A C6A 121.8(9) . . ? C1A C6A C5A 120.8(8) . . ? C1A C6A C68A 117.4(8) . . ? C5A C6A C68A 121.7(8) . . ? C8A C7A C10A 108.4(10) . . ? C8A C7A C9A 107.8(9) . . ? C10A C7A C9A 108.7(9) . . ? C8A C7A C4A 112.0(8) . . ? C10A C7A C4A 109.0(8) . . ? C9A C7A C4A 110.8(9) . . ? C2A C11A C12A 114.5(7) . . ? C17A C12A C13A 119.6(8) . . ? C17A C12A C11A 122.0(8) . . ? C13A C12A C11A 118.4(8) . . ? O2A C13A C14A 120.8(7) . . ? O2A C13A C12A 120.8(8) . . ? C14A C13A C12A 118.3(8) . . ? C13A C14A C15A 120.0(8) . . ? C13A C14A C22A 118.5(7) . . ? C15A C14A C22A 121.4(8) . . ? C16A C15A C14A 121.7(9) . . ? C17A C16A C15A 116.5(8) . . ? C17A C16A C18A 121.4(8) . . ? C15A C16A C18A 122.1(9) . . ? C12A C17A C16A 123.9(8) . . ? C20A C18A C19A 109.6(9) . . ? C20A C18A C16A 112.5(8) . . ? C19A C18A C16A 108.7(8) . . ? C20A C18A C21A 107.4(9) . . ? C19A C18A C21A 108.5(9) . . ? C16A C18A C21A 110.1(9) . . ? O3A C22A C14A 108.8(7) . . ? O3A C23A C24A 112.8(7) . . ? C29A C24A C25A 119.0(8) . . ? C29A C24A C23A 120.9(8) . . ? C25A C24A C23A 120.1(8) . . ? O4A C25A C26A 121.8(8) . . ? O4A C25A C24A 118.5(8) . . ? C26A C25A C24A 119.7(8) . . ? C27A C26A C25A 118.9(8) . . ? C27A C26A C34A 120.0(8) . . ? C25A C26A C34A 121.1(8) . . ? C26A C27A C28A 123.6(8) . . ? C29A C28A C27A 115.1(8) . . ? C29A C28A C30A 120.0(8) . . ? C27A C28A C30A 125.0(8) . . ? C24A C29A C28A 123.6(8) . . ? C28A C30A C33A 111.6(7) . . ? C28A C30A C31A 109.9(7) . . ? C33A C30A C31A 108.6(8) . . ? C28A C30A C32A 110.5(7) . . ? C33A C30A C32A 107.7(7) . . ? C31A C30A C32A 108.6(8) . . ? C26A C34A C35A 112.7(6) . . ? C40A C35A C36A 120.1(8) . . ? C40A C35A C34A 120.1(8) . . ? C36A C35A C34A 119.8(8) . . ? O5A C36A C35A 119.1(7) . . ? O5A C36A C37A 121.0(7) . . ? C35A C36A C37A 119.8(8) . . ? C38A C37A C36A 117.4(8) . . ? C38A C37A C45A 120.8(8) . . ? C36A C37A C45A 121.7(8) . . ? C37A C38A C39A 124.1(9) . . ? C38A C39A C40A 117.4(9) . . ? C38A C39A C41A 121.5(8) . . ? C40A C39A C41A 121.1(8) . . ? C35A C40A C39A 121.0(9) . . ? C43I C41A C44A 139.6(19) . . ? C43I C41A C39A 109.9(18) . . ? C44A C41A C39A 109.7(9) . . ? C43I C41A C42A 58.7(19) . . ? C44A C41A C42A 110.6(11) . . ? C39A C41A C42A 113.6(9) . . ? C43I C41A C44I 120(2) . . ? C44A C41A C44I 34.7(16) . . ? C39A C41A C44I 110.9(17) . . ? C42A C41A C44I 131.9(18) . . ? C43I C41A C43A 50.3(18) . . ? C44A C41A C43A 108.9(11) . . ? C39A C41A C43A 108.1(10) . . ? C42A C41A C43A 105.7(11) . . ? C44I C41A C43A 76.0(18) . . ? C43I C41A C42I 104(2) . . ? C44A C41A C42I 73.4(17) . . ? C39A C41A C42I 104.6(18) . . ? C42A C41A C42I 45.3(16) . . ? C44I C41A C42I 106(2) . . ? C43A C41A C42I 143.8(19) . . ? C42I C42A C43I 129(3) . . ? C37A C45A C46A 111.7(7) . . ? C51A C46A C47A 120.4(8) . . ? C51A C46A C45A 119.1(8) . . ? C47A C46A C45A 120.1(8) . . ? O6A C47A C48A 120.6(8) . . ? O6A C47A C46A 120.7(8) . . ? C48A C47A C46A 118.7(8) . . ? C49A C48A C47A 118.8(8) . . ? C49A C48A C56A 119.4(8) . . ? C47A C48A C56A 121.8(8) . . ? C50A C49A C48A 123.6(9) . . ? C49A C50A C51A 116.3(9) . . ? C49A C50A C52A 123.9(9) . . ? C51A C50A C52A 119.7(8) . . ? C46A C51A C50A 122.0(8) . . ? C53I C52A C53A 47.7(15) . . ? C53I C52A C55I 116(2) . . ? C53A C52A C55I 133.6(17) . . ? C53I C52A C50A 118.4(17) . . ? C53A C52A C50A 111.3(11) . . ? C55I C52A C50A 113.1(15) . . ? C53I C52A C54A 128.2(19) . . ? C53A C52A C54A 110.5(12) . . ? C55I C52A C54A 37.7(12) . . ? C50A C52A C54A 113.3(11) . . ? C53I C52A C55A 59.2(16) . . ? C53A C52A C55A 106.4(11) . . ? C55I C52A C55A 71.5(14) . . ? C50A C52A C55A 108.1(10) . . ? C54A C52A C55A 106.9(12) . . ? C53I C52A C54I 106(2) . . ? C53A C52A C54I 60.9(15) . . ? C55I C52A C54I 96.5(19) . . ? C50A C52A C54I 102.7(15) . . ? C54A C52A C54I 59.3(15) . . ? C55A C52A C54I 149.1(17) . . ? C57A C56A C48A 116.0(7) . . ? C62A C57A C58A 118.7(8) . . ? C62A C57A C56A 120.5(8) . . ? C58A C57A C56A 120.8(8) . . ? O7A C58A C59A 118.0(7) . . ? O7A C58A C57A 121.4(7) . . ? C59A C58A C57A 120.4(8) . . ? C60A C59A C58A 119.0(8) . . ? C60A C59A C67A 120.1(7) . . ? C58A C59A C67A 120.9(7) . . ? C59A C60A C61A 122.6(8) . . ? C60A C61A C62A 116.8(8) . . ? C60A C61A C63A 121.8(8) . . ? C62A C61A C63A 121.3(8) . . ? C57A C62A C61A 122.3(8) . . ? C64A C63A C66A 109.1(8) . . ? C64A C63A C61A 112.0(7) . . ? C66A C63A C61A 108.6(7) . . ? C64A C63A C65A 108.8(7) . . ? C66A C63A C65A 109.5(7) . . ? C61A C63A C65A 108.9(7) . . ? O8A C67A C59A 108.0(6) . . ? O8A C68A C6A 106.3(7) . . ? O9B U2 O10B 177.9(3) . . ? O9B U2 O1B 91.6(2) . . ? O10B U2 O1B 88.5(2) . . ? O9B U2 O2B 87.1(2) . . ? O10B U2 O2B 95.1(2) . . ? O1B U2 O2B 85.9(2) . . ? O9B U2 O7B 84.6(2) . . ? O10B U2 O7B 93.2(2) . . ? O1B U2 O7B 101.18(19) . . ? O2B U2 O7B 169.25(19) . . ? O9B U2 O6B 95.6(2) . . ? O10B U2 O6B 84.6(2) . . ? O1B U2 O6B 170.78(18) . . ? O2B U2 O6B 88.70(19) . . ? O7B U2 O6B 85.27(19) . . ? C1B O1B U2 135.5(5) . . ? C13B O2B U2 122.1(5) . . ? C22B O3B C23B 114.9(6) . . ? C47B O6B U2 123.6(5) . . ? C58B O7B U2 133.9(4) . . ? C67B O8B C68B 113.3(6) . . ? C6B C1B O1B 119.4(7) . . ? C6B C1B C2B 121.8(8) . . ? O1B C1B C2B 118.7(8) . . ? C3B C2B C1B 116.7(8) . . ? C3B C2B C11B 120.1(7) . . ? C1B C2B C11B 122.7(7) . . ? C2B C3B C4B 124.2(7) . . ? C3B C4B C5B 116.6(8) . . ? C3B C4B C7B 120.6(7) . . ? C5B C4B C7B 122.7(8) . . ? C4B C5B C6B 120.8(8) . . ? C1B C6B C5B 119.7(7) . . ? C1B C6B C68B 120.4(8) . . ? C5B C6B C68B 119.8(8) . . ? C4B C7B C10B 113.3(7) . . ? C4B C7B C9B 109.8(8) . . ? C10B C7B C9B 108.7(9) . . ? C4B C7B C8B 110.0(8) . . ? C10B C7B C8B 106.7(8) . . ? C9B C7B C8B 108.2(8) . . ? C12B C11B C2B 117.7(7) . . ? C17B C12B C13B 118.4(8) . . ? C17B C12B C11B 121.0(8) . . ? C13B C12B C11B 120.3(8) . . ? O2B C13B C14B 121.4(7) . . ? O2B C13B C12B 119.3(7) . . ? C14B C13B C12B 119.2(8) . . ? C15B C14B C13B 120.0(8) . . ? C15B C14B C22B 120.5(8) . . ? C13B C14B C22B 119.5(7) . . ? C14B C15B C16B 122.3(8) . . ? C17B C16B C15B 116.5(8) . . ? C17B C16B C18B 125.3(8) . . ? C15B C16B C18B 118.2(8) . . ? C16B C17B C12B 123.5(8) . . ? C21B C18B C19B 110.6(8) . . ? C21B C18B C16B 110.1(7) . . ? C19B C18B C16B 110.9(8) . . ? C21B C18B C20B 107.4(8) . . ? C19B C18B C20B 106.6(7) . . ? C16B C18B C20B 111.2(7) . . ? O3B C22B C14B 107.3(6) . . ? O3B C23B C24B 112.7(7) . . ? C29B C24B C25B 117.1(8) . . ? C29B C24B C23B 122.2(8) . . ? C25B C24B C23B 120.7(8) . . ? O4B C25B C26B 122.3(8) . . ? O4B C25B C24B 116.6(8) . . ? C26B C25B C24B 121.1(8) . . ? C25B C26B C27B 118.4(8) . . ? C25B C26B C34B 122.9(8) . . ? C27B C26B C34B 118.7(8) . . ? C28B C27B C26B 123.0(9) . . ? C27B C28B C29B 116.4(9) . . ? C27B C28B C30B 122.1(9) . . ? C29B C28B C30B 121.3(8) . . ? C28B C29B C24B 123.9(9) . . ? C32B C30B C33B 110.3(9) . . ? C32B C30B C31B 108.4(8) . . ? C33B C30B C31B 110.2(9) . . ? C32B C30B C28B 110.9(8) . . ? C33B C30B C28B 107.9(8) . . ? C31B C30B C28B 109.1(8) . . ? C26B C34B C35B 112.8(7) . . ? C36B C35B C40B 118.5(8) . . ? C36B C35B C34B 121.1(8) . . ? C40B C35B C34B 120.4(8) . . ? O5B C36B C35B 118.4(7) . . ? O5B C36B C37B 119.7(8) . . ? C35B C36B C37B 121.9(8) . . ? C36B C37B C38B 116.8(8) . . ? C36B C37B C45B 122.6(8) . . ? C38B C37B C45B 120.2(8) . . ? C39B C38B C37B 123.9(8) . . ? C38B C39B C40B 116.3(9) . . ? C38B C39B C41B 120.9(8) . . ? C40B C39B C41B 122.6(9) . . ? C39B C40B C35B 122.4(9) . . ? C39B C41B C44B 113.9(9) . . ? C39B C41B C42B 108.4(8) . . ? C44B C41B C42B 108.1(10) . . ? C39B C41B C43B 112.5(8) . . ? C44B C41B C43B 107.5(9) . . ? C42B C41B C43B 106.0(10) . . ? C37B C45B C46B 111.4(7) . . ? C51B C46B C47B 119.9(8) . . ? C51B C46B C45B 119.6(7) . . ? C47B C46B C45B 120.1(8) . . ? O6B C47B C48B 122.5(7) . . ? O6B C47B C46B 119.6(7) . . ? C48B C47B C46B 117.9(8) . . ? C49B C48B C47B 119.5(7) . . ? C49B C48B C56B 119.7(7) . . ? C47B C48B C56B 120.8(7) . . ? C48B C49B C50B 123.6(8) . . ? C49B C50B C51B 115.6(8) . . ? C49B C50B C52B 124.1(7) . . ? C51B C50B C52B 120.1(7) . . ? C46B C51B C50B 123.4(8) . . ? C50B C52B C55B 110.6(7) . . ? C50B C52B C53B 112.8(7) . . ? C55B C52B C53B 108.3(8) . . ? C50B C52B C54B 110.3(8) . . ? C55B C52B C54B 107.1(8) . . ? C53B C52B C54B 107.6(8) . . ? C48B C56B C57B 114.5(7) . . ? C62B C57B C58B 118.6(8) . . ? C62B C57B C56B 120.0(8) . . ? C58B C57B C56B 121.4(8) . . ? O7B C58B C57B 121.0(8) . . ? O7B C58B C59B 119.9(7) . . ? C57B C58B C59B 118.9(8) . . ? C60B C59B C58B 119.6(8) . . ? C60B C59B C67B 121.3(8) . . ? C58B C59B C67B 119.1(8) . . ? C59B C60B C61B 122.9(9) . . ? C62B C61B C60B 115.3(8) . . ? C62B C61B C63B 124.8(8) . . ? C60B C61B C63B 119.9(8) . . ? C61B C62B C57B 124.7(9) . . ? C65B C63B C61B 110.9(8) . . ? C65B C63B C64B 109.1(9) . . ? C61B C63B C64B 112.0(8) . . ? C65B C63B C66B 109.4(9) . . ? C61B C63B C66B 109.0(8) . . ? C64B C63B C66B 106.4(8) . . ? O8B C67B C59B 109.5(7) . . ? O8B C68B C6B 107.8(7) . . ? C1 N1 C5 111.8(8) . . ? C1 N1 C3 115.0(8) . . ? C5 N1 C3 113.0(8) . . ? C11 N2 C7 114.9(8) . . ? C11 N2 C9 112.2(7) . . ? C7 N2 C9 109.5(7) . . ? C13 N3 C15 114.2(10) . . ? C13 N3 C17 109.9(9) . . ? C15 N3 C17 107.8(8) . . ? C21I N4 C23I 113.9(9) . . ? C21I N4 C19I 113.5(10) . . ? C23I N4 C19I 106.7(9) . . ? C19J N4 C23J 112.3(15) . . ? C19J N4 C21J 109.8(15) . . ? C23J N4 C21J 105.4(14) . . ? N1 C1 C2 113.0(9) . . ? C4 C3 N1 114.7(9) . . ? N1 C5 C6 110.3(8) . . ? C8 C7 N2 113.9(9) . . ? N2 C9 C10 111.0(7) . . ? N2 C11 C12 111.7(9) . . ? N3 C13 C14 110.3(10) . . ? N3 C15 C16 115.5(9) . . ? N3 C17 C18 112.1(9) . . ? C20 C19I N4 117.2(12) . . ? N4 C19J C20 114.8(17) . . ? N4 C21I C22 113.4(10) . . ? C22 C21J N4 114.9(17) . . ? N4 C23I C24 111.8(10) . . ? C24 C23J N4 112.5(18) . . ? N5 C25 C26 170(2) . . ? N6 C27 C28 178.4(13) . . ? N7 C29 C30 162(2) . . ? N8 C31 C32 176.7(15) . . ? N9 C33 C34 162(3) . . ? N10 C35 C36 177.7(15) . . ? #==END data_6 _database_code_CSD 153525 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53.50 H57.50 N3.50 O14 U2' _chemical_formula_weight 1449.59 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' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2810(4) _cell_length_b 25.6482(16) _cell_length_c 17.9607(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.454(3) _cell_angle_gamma 90.00 _cell_volume 5140.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 33418 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent orange' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_method ? _exptl_crystal_F_000 2796 _exptl_absorpt_coefficient_mu 6.364 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.180 _exptl_absorpt_correction_T_max 0.225 _exptl_absorpt_process_details 'program MULABS from PLATON (Spek, 1997)' _exptl_special_details '\f scans with 2\% steps' _diffrn_ambient_temperature 100(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 33418 _diffrn_reflns_av_R_equivalents 0.1033 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8887 _reflns_number_gt 5945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and expanded by subsequent Fourier-difference synthesis. One pyridine molecule is disordered around a symmetry centre and the nitrogen atom has not been differentiated from the carbon ones. All non-hydrogen atoms have been refined anisotropically. The hydrogen atoms have been introduced at calculated positions (except those of the ions or molecules O13 and O14 and the one bound to the nitrogen atom in the pyridinium ion, which have not been found on the difference-Fourier map, nor introduced) as riding atoms and constrained to ride on their parent atom with a displacement factor equal to 1.2 (CH, CH2) or 1.5 (CH3) times that of this atom. The four highest residual density peaks are located near the uranium atoms as a result of imperfect absorption correction. All other peaks are lower than 0.9 eA-3. 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^)+(0.0611P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8887 _refine_ls_number_parameters 662 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1265 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 1.708 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.177 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 U1 U 1.26225(3) 0.214503(16) 0.890422(18) 0.02410(11) Uani 1 1 d . . . U2 U 1.54839(3) 0.214783(16) 0.788707(18) 0.02355(11) Uani 1 1 d . . . O1 O 1.2094(6) 0.2950(3) 0.9222(4) 0.0318(17) Uani 1 1 d . . . O2 O 1.0249(5) 0.2191(3) 0.8808(4) 0.0295(15) Uani 1 1 d . . . O3 O 1.1866(5) 0.1333(3) 0.8945(4) 0.0307(16) Uani 1 1 d . . . O4 O 1.3012(5) 0.0777(3) 0.7443(4) 0.0323(16) Uani 1 1 d . . . O5 O 1.5821(5) 0.1347(3) 0.7438(3) 0.0271(15) Uani 1 1 d . . . O6 O 1.6463(6) 0.2237(3) 0.6618(4) 0.0296(16) Uani 1 1 d . . . O7 O 1.6312(5) 0.2931(3) 0.7849(4) 0.0292(15) Uani 1 1 d . . . O8 O 1.3698(5) 0.3706(3) 0.7931(3) 0.0296(16) Uani 1 1 d . . . O9 O 1.3209(5) 0.2056(3) 0.9880(4) 0.0325(17) Uani 1 1 d . . . O10 O 1.2118(5) 0.2231(2) 0.7929(3) 0.0226(14) Uani 1 1 d . . . O11 O 1.6666(5) 0.1998(3) 0.8645(3) 0.0305(16) Uani 1 1 d . . . O12 O 1.4261(5) 0.2278(3) 0.7158(3) 0.0277(15) Uani 1 1 d . . . O13 O 1.4387(5) 0.2569(3) 0.8719(4) 0.0386(18) Uani 1 1 d . . . O14 O 1.4100(5) 0.1548(3) 0.8443(4) 0.0397(18) Uani 1 1 d . . . C1 C 1.1336(8) 0.3255(4) 0.8741(5) 0.031(2) Uani 1 1 d . . . C2 C 1.1788(8) 0.3693(4) 0.8395(5) 0.030(2) Uani 1 1 d . . . C3 C 1.1010(8) 0.3987(4) 0.7899(6) 0.035(2) Uani 1 1 d . . . H3 H 1.1303 0.4276 0.7672 0.042 Uiso 1 1 calc R . . C4 C 0.9777(9) 0.3862(4) 0.7726(5) 0.033(2) Uani 1 1 d . . . C5 C 0.9378(8) 0.3434(4) 0.8086(6) 0.029(2) Uani 1 1 d . . . H5 H 0.8568 0.3351 0.7987 0.034 Uiso 1 1 calc R . . C6 C 1.0129(7) 0.3118(4) 0.8593(5) 0.025(2) Uani 1 1 d . . . C7 C 0.8958(9) 0.4182(4) 0.7171(7) 0.044(3) Uani 1 1 d . . . H7A H 0.8967 0.4048 0.6673 0.066 Uiso 1 1 calc R . . H7B H 0.9224 0.4537 0.7194 0.066 Uiso 1 1 calc R . . H7C H 0.8158 0.4164 0.7292 0.066 Uiso 1 1 calc R . . C8 C 0.9690(9) 0.2672(4) 0.8996(6) 0.038(3) Uani 1 1 d . . . H8A H 0.9866 0.2731 0.9534 0.046 Uiso 1 1 calc R . . H8B H 0.8828 0.2643 0.8862 0.046 Uiso 1 1 calc R . . C9 C 0.9591(8) 0.1727(4) 0.8979(5) 0.027(2) Uani 1 1 d . . . H9A H 0.8742 0.1806 0.8927 0.032 Uiso 1 1 calc R . . H9B H 0.9855 0.1621 0.9495 0.032 Uiso 1 1 calc R . . C10 C 0.9793(8) 0.1295(4) 0.8463(5) 0.028(2) Uani 1 1 d . . . C11 C 1.0982(8) 0.1097(4) 0.8469(5) 0.030(2) Uani 1 1 d . . . C12 C 1.1175(7) 0.0691(4) 0.7987(5) 0.024(2) Uani 1 1 d . . . C13 C 1.0215(8) 0.0474(4) 0.7533(5) 0.029(2) Uani 1 1 d . . . H13 H 1.0354 0.0205 0.7210 0.035 Uiso 1 1 calc R . . C14 C 0.9041(8) 0.0641(4) 0.7538(6) 0.033(2) Uani 1 1 d . . . C15 C 0.8866(8) 0.1059(4) 0.7995(6) 0.030(2) Uani 1 1 d . . . H15 H 0.8092 0.1186 0.7986 0.036 Uiso 1 1 calc R . . C16 C 0.8003(9) 0.0367(4) 0.7061(7) 0.044(3) Uani 1 1 d . . . H16A H 0.8200 0.0007 0.7005 0.066 Uiso 1 1 calc R . . H16B H 0.7853 0.0529 0.6574 0.066 Uiso 1 1 calc R . . H16C H 0.7300 0.0393 0.7301 0.066 Uiso 1 1 calc R . . C17 C 1.2423(8) 0.0488(4) 0.7990(5) 0.027(2) Uani 1 1 d . . . H17A H 1.2879 0.0527 0.8489 0.033 Uiso 1 1 calc R . . H17B H 1.2393 0.0121 0.7862 0.033 Uiso 1 1 calc R . . C18 C 1.4084(9) 0.0520(4) 0.7282(6) 0.035(2) Uani 1 1 d . . . H18A H 1.3910 0.0155 0.7170 0.042 Uiso 1 1 calc R . . H18B H 1.4695 0.0536 0.7722 0.042 Uiso 1 1 calc R . . C19 C 1.4546(8) 0.0765(4) 0.6635(6) 0.031(2) Uani 1 1 d . . . C20 C 1.5404(8) 0.1170(4) 0.6760(5) 0.026(2) Uani 1 1 d . . . C21 C 1.5864(8) 0.1374(4) 0.6132(5) 0.027(2) Uani 1 1 d . . . C22 C 1.5470(8) 0.1184(4) 0.5417(5) 0.025(2) Uani 1 1 d . . . H22 H 1.5792 0.1322 0.5011 0.030 Uiso 1 1 calc R . . C23 C 1.4598(9) 0.0789(4) 0.5285(6) 0.034(2) Uani 1 1 d . . . C24 C 1.4190(9) 0.0591(4) 0.5915(5) 0.031(2) Uani 1 1 d . . . H24 H 1.3636 0.0320 0.5847 0.038 Uiso 1 1 calc R . . C25 C 1.4143(10) 0.0599(5) 0.4514(6) 0.046(3) Uani 1 1 d . . . H25A H 1.3414 0.0778 0.4324 0.068 Uiso 1 1 calc R . . H25B H 1.3990 0.0231 0.4530 0.068 Uiso 1 1 calc R . . H25C H 1.4731 0.0664 0.4189 0.068 Uiso 1 1 calc R . . C26 C 1.6863(9) 0.1771(4) 0.6254(5) 0.033(2) Uani 1 1 d . . . H26A H 1.7553 0.1622 0.6568 0.040 Uiso 1 1 calc R . . H26B H 1.7100 0.1866 0.5774 0.040 Uiso 1 1 calc R . . C27 C 1.7252(9) 0.2687(4) 0.6551(6) 0.032(2) Uani 1 1 d . . . H27A H 1.7543 0.2677 0.6069 0.038 Uiso 1 1 calc R . . H27B H 1.7938 0.2674 0.6946 0.038 Uiso 1 1 calc R . . C28 C 1.6573(7) 0.3172(4) 0.6616(5) 0.026(2) Uani 1 1 d . . . C29 C 1.6118(8) 0.3282(4) 0.7296(5) 0.027(2) Uani 1 1 d . . . C30 C 1.5476(7) 0.3757(4) 0.7344(5) 0.024(2) Uani 1 1 d . . . C31 C 1.5330(7) 0.4087(4) 0.6753(5) 0.027(2) Uani 1 1 d . . . H31 H 1.4917 0.4396 0.6796 0.032 Uiso 1 1 calc R . . C32 C 1.5768(8) 0.3988(4) 0.6081(6) 0.030(2) Uani 1 1 d . . . C33 C 1.6382(8) 0.3527(4) 0.6021(5) 0.030(2) Uani 1 1 d . . . H33 H 1.6674 0.3452 0.5576 0.036 Uiso 1 1 calc R . . C34 C 1.5606(10) 0.4390(4) 0.5435(6) 0.039(3) Uani 1 1 d . . . H34A H 1.6315 0.4399 0.5198 0.059 Uiso 1 1 calc R . . H34B H 1.5469 0.4729 0.5633 0.059 Uiso 1 1 calc R . . H34C H 1.4932 0.4293 0.5071 0.059 Uiso 1 1 calc R . . C35 C 1.4957(7) 0.3866(4) 0.8048(6) 0.031(2) Uani 1 1 d . . . H35A H 1.5395 0.3675 0.8466 0.038 Uiso 1 1 calc R . . H35B H 1.5018 0.4236 0.8165 0.038 Uiso 1 1 calc R . . C36 C 1.3103(8) 0.3846(4) 0.8563(5) 0.032(2) Uani 1 1 d . . . H36A H 1.3171 0.4219 0.8651 0.038 Uiso 1 1 calc R . . H36B H 1.3480 0.3668 0.9012 0.038 Uiso 1 1 calc R . . N1 N 1.2504(7) 0.3115(4) 0.6738(5) 0.043(2) Uani 1 1 d . . . C37 C 1.3029(8) 0.3158(4) 0.6134(5) 0.029(2) Uani 1 1 d . . . H37 H 1.3854 0.3208 0.6187 0.035 Uiso 1 1 calc R . . C38 C 1.2390(8) 0.3132(4) 0.5441(6) 0.037(3) Uani 1 1 d . . . H38 H 1.2755 0.3167 0.5012 0.044 Uiso 1 1 calc R . . C39 C 1.1173(10) 0.3050(5) 0.5390(6) 0.045(3) Uani 1 1 d . . . H39 H 1.0710 0.3020 0.4919 0.054 Uiso 1 1 calc R . . C40 C 1.0633(9) 0.3014(4) 0.6029(6) 0.036(3) Uani 1 1 d . . . H40 H 0.9808 0.2970 0.5993 0.043 Uiso 1 1 calc R . . C41 C 1.1320(8) 0.3044(4) 0.6704(6) 0.034(2) Uani 1 1 d . . . H41 H 1.0978 0.3016 0.7143 0.041 Uiso 1 1 calc R . . N2 N 1.5523(7) 0.3135(4) 0.9884(5) 0.041(2) Uani 1 1 d . . . C42 C 1.6699(8) 0.3156(5) 0.9969(6) 0.037(3) Uani 1 1 d . . . H42 H 1.7090 0.3100 0.9555 0.044 Uiso 1 1 calc R . . C43 C 1.7373(10) 0.3261(4) 1.0669(6) 0.040(3) Uani 1 1 d . . . H43 H 1.8204 0.3279 1.0717 0.048 Uiso 1 1 calc R . . C44 C 1.6801(9) 0.3337(4) 1.1294(6) 0.039(3) Uani 1 1 d . . . H44 H 1.7236 0.3398 1.1767 0.047 Uiso 1 1 calc R . . C45 C 1.5573(10) 0.3320(5) 1.1190(7) 0.043(3) Uani 1 1 d . . . H45 H 1.5162 0.3373 1.1596 0.052 Uiso 1 1 calc R . . C46 C 1.4933(9) 0.3222(4) 1.0473(6) 0.036(3) Uani 1 1 d . . . H46 H 1.4100 0.3217 1.0404 0.043 Uiso 1 1 calc R . . N3 N 1.5317(8) 0.0888(4) 0.9386(5) 0.042(2) Uani 1 1 d . . . C47 C 1.6333(9) 0.0759(5) 0.9163(6) 0.042(3) Uani 1 1 d . . . H47 H 1.6449 0.0846 0.8676 0.051 Uiso 1 1 calc R . . C48 C 1.7243(11) 0.0498(5) 0.9617(8) 0.060(4) Uani 1 1 d . . . H48 H 1.7946 0.0409 0.9436 0.072 Uiso 1 1 calc R . . C49 C 1.7089(11) 0.0375(6) 1.0339(8) 0.069(4) Uani 1 1 d . . . H49 H 1.7695 0.0210 1.0661 0.082 Uiso 1 1 calc R . . C50 C 1.6003(11) 0.0503(6) 1.0581(7) 0.063(4) Uani 1 1 d . . . H50 H 1.5874 0.0425 1.1068 0.076 Uiso 1 1 calc R . . C51 C 1.5126(10) 0.0747(5) 1.0085(6) 0.049(3) Uani 1 1 d . . . H51 H 1.4387 0.0817 1.0235 0.059 Uiso 1 1 calc R . . C52 C 1.3830(13) 0.4944(7) 1.0036(10) 0.079(5) Uani 1 1 d . . . H52 H 1.3014 0.4898 1.0045 0.095 Uiso 1 1 calc R . . C53 C 1.4612(13) 0.4609(5) 1.0397(8) 0.061(4) Uani 1 1 d . . . H53 H 1.4342 0.4346 1.0686 0.073 Uiso 1 1 calc R . . C54 C 1.5776(14) 0.4644(7) 1.0351(10) 0.082(5) Uani 1 1 d . . . H54 H 1.6312 0.4395 1.0577 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.02330(19) 0.0301(2) 0.01898(19) 0.00132(16) 0.00342(12) 0.00087(14) U2 0.02420(19) 0.0253(2) 0.0215(2) 0.00257(15) 0.00473(12) 0.00147(14) O1 0.037(4) 0.036(5) 0.024(4) -0.010(3) 0.006(3) 0.006(3) O2 0.023(3) 0.028(4) 0.039(4) 0.002(3) 0.012(3) 0.001(3) O3 0.034(4) 0.032(5) 0.028(4) 0.006(3) 0.009(3) 0.002(3) O4 0.032(4) 0.025(4) 0.042(4) 0.013(3) 0.012(3) 0.010(3) O5 0.035(4) 0.022(4) 0.026(4) 0.006(3) 0.010(3) 0.002(3) O6 0.035(4) 0.024(4) 0.033(4) 0.001(3) 0.016(3) -0.002(3) O7 0.031(3) 0.033(5) 0.025(4) 0.001(3) 0.005(3) -0.001(3) O8 0.020(3) 0.040(5) 0.030(4) -0.014(3) 0.009(3) -0.010(3) O9 0.026(4) 0.045(5) 0.028(4) 0.004(3) 0.009(3) -0.004(3) O10 0.023(3) 0.012(4) 0.032(4) 0.002(3) 0.004(2) 0.001(2) O11 0.029(4) 0.041(5) 0.023(4) 0.002(3) 0.006(3) 0.002(3) O12 0.029(3) 0.034(5) 0.020(4) -0.001(3) 0.002(2) 0.003(3) O13 0.019(3) 0.068(6) 0.029(4) -0.006(4) 0.003(3) 0.003(3) O14 0.025(4) 0.055(5) 0.041(4) 0.020(4) 0.009(3) 0.014(3) C1 0.029(5) 0.042(7) 0.021(5) -0.008(4) 0.003(4) 0.008(4) C2 0.034(5) 0.037(7) 0.019(5) -0.011(4) 0.003(4) 0.002(4) C3 0.036(6) 0.027(6) 0.044(7) -0.006(5) 0.012(4) -0.008(4) C4 0.039(6) 0.033(7) 0.024(5) 0.000(4) 0.001(4) 0.006(4) C5 0.028(5) 0.016(6) 0.044(6) -0.004(4) 0.011(4) 0.004(4) C6 0.022(5) 0.025(6) 0.030(5) -0.008(4) 0.008(4) 0.000(4) C7 0.035(6) 0.026(7) 0.068(8) 0.002(6) 0.001(5) 0.004(4) C8 0.033(6) 0.044(8) 0.040(7) 0.001(5) 0.018(4) -0.002(5) C9 0.022(5) 0.029(6) 0.029(5) 0.008(4) 0.004(4) 0.003(4) C10 0.035(5) 0.024(6) 0.027(5) 0.003(4) 0.011(4) 0.001(4) C11 0.024(5) 0.038(7) 0.031(6) 0.018(5) 0.008(4) 0.000(4) C12 0.028(5) 0.021(6) 0.026(5) 0.009(4) 0.014(4) -0.001(4) C13 0.037(6) 0.021(6) 0.030(6) 0.005(4) 0.005(4) -0.001(4) C14 0.036(6) 0.024(6) 0.040(6) 0.006(5) 0.011(4) -0.007(4) C15 0.023(5) 0.024(6) 0.044(6) 0.011(5) 0.009(4) 0.002(4) C16 0.033(6) 0.024(7) 0.074(9) -0.003(6) 0.002(5) -0.002(4) C17 0.043(6) 0.020(6) 0.021(5) -0.001(4) 0.008(4) 0.010(4) C18 0.040(6) 0.028(6) 0.039(6) 0.005(5) 0.013(4) 0.005(4) C19 0.029(5) 0.026(6) 0.039(6) 0.012(5) 0.010(4) 0.010(4) C20 0.027(5) 0.021(6) 0.033(6) 0.006(4) 0.012(4) 0.012(4) C21 0.037(5) 0.022(6) 0.022(5) 0.011(4) 0.010(4) 0.011(4) C22 0.046(5) 0.016(5) 0.014(5) 0.011(4) 0.011(4) 0.013(4) C23 0.051(6) 0.020(6) 0.031(6) -0.008(4) 0.010(4) 0.006(5) C24 0.046(6) 0.020(6) 0.029(6) 0.007(4) 0.009(4) 0.005(4) C25 0.066(8) 0.036(8) 0.037(7) -0.008(5) 0.017(5) -0.001(6) C26 0.055(6) 0.029(7) 0.020(5) 0.001(4) 0.020(4) 0.004(5) C27 0.041(6) 0.023(6) 0.036(6) 0.003(4) 0.017(4) 0.000(4) C28 0.022(5) 0.028(6) 0.029(5) -0.002(4) 0.008(3) -0.006(4) C29 0.028(5) 0.031(6) 0.023(5) 0.004(4) 0.001(4) -0.006(4) C30 0.025(5) 0.013(5) 0.032(5) -0.006(4) -0.002(4) -0.002(4) C31 0.021(5) 0.036(6) 0.023(5) 0.002(4) 0.000(3) -0.008(4) C32 0.035(5) 0.010(5) 0.044(6) 0.000(4) 0.004(4) 0.004(4) C33 0.030(5) 0.033(6) 0.027(5) -0.008(4) 0.008(4) -0.016(4) C34 0.063(7) 0.014(6) 0.043(7) 0.001(5) 0.013(5) 0.006(5) C35 0.020(5) 0.029(6) 0.045(6) -0.008(5) 0.005(4) -0.005(4) C36 0.027(5) 0.038(7) 0.031(6) -0.017(5) 0.005(4) -0.009(4) N1 0.037(5) 0.066(8) 0.025(5) 0.007(5) 0.004(4) 0.005(4) C37 0.029(5) 0.025(6) 0.032(6) 0.005(4) 0.004(4) -0.001(4) C38 0.032(6) 0.035(7) 0.045(7) 0.012(5) 0.011(4) 0.003(5) C39 0.051(7) 0.053(8) 0.028(6) 0.004(5) -0.004(5) -0.015(5) C40 0.030(6) 0.033(7) 0.045(7) 0.000(5) 0.011(4) 0.003(4) C41 0.027(6) 0.041(7) 0.033(6) 0.005(5) 0.000(4) 0.013(4) N2 0.031(5) 0.066(7) 0.024(5) -0.016(4) -0.001(3) 0.001(4) C42 0.033(6) 0.044(8) 0.035(6) -0.007(5) 0.012(4) 0.001(5) C43 0.047(6) 0.016(6) 0.053(7) -0.006(5) -0.001(5) 0.001(5) C44 0.052(7) 0.035(7) 0.029(6) 0.005(5) 0.001(5) -0.005(5) C45 0.059(7) 0.030(7) 0.047(7) -0.003(5) 0.024(5) 0.006(5) C46 0.032(5) 0.043(8) 0.036(6) -0.004(5) 0.015(4) -0.005(5) N3 0.041(5) 0.038(6) 0.045(6) 0.007(4) 0.007(4) 0.007(4) C47 0.041(6) 0.051(8) 0.037(6) 0.017(5) 0.010(5) 0.009(5) C48 0.049(7) 0.060(10) 0.077(10) 0.037(8) 0.026(6) 0.021(6) C49 0.051(8) 0.081(12) 0.073(10) 0.046(8) 0.003(6) 0.020(7) C50 0.065(9) 0.079(11) 0.045(8) 0.034(7) 0.007(6) 0.005(7) C51 0.046(7) 0.063(9) 0.038(7) 0.025(6) 0.005(5) 0.009(6) C52 0.056(9) 0.060(12) 0.116(14) 0.008(10) -0.005(8) 0.023(8) C53 0.080(10) 0.044(9) 0.062(9) 0.003(7) 0.019(7) 0.013(7) C54 0.080(11) 0.065(12) 0.102(13) 0.007(10) 0.013(9) 0.043(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O10 1.774(6) . ? U1 O9 1.795(6) . ? U1 O1 2.245(7) . ? U1 O3 2.256(7) . ? U1 O13 2.334(7) . ? U1 O14 2.492(7) . ? U1 O2 2.661(6) . ? U1 U2 3.9359(4) . ? U2 O12 1.789(6) . ? U2 O11 1.801(6) . ? U2 O7 2.221(7) . ? U2 O5 2.260(7) . ? U2 O13 2.340(7) . ? U2 O14 2.502(7) . ? U2 O6 2.685(6) . ? O1 C1 1.368(11) . ? O2 C8 1.447(12) . ? O2 C9 1.459(11) . ? O3 C11 1.356(12) . ? O4 C18 1.444(11) . ? O4 C17 1.466(11) . ? O5 C20 1.319(11) . ? O6 C26 1.464(11) . ? O6 C27 1.474(11) . ? O7 C29 1.334(11) . ? O8 C36 1.446(11) . ? O8 C35 1.464(10) . ? O8 N1 2.802(11) . ? O10 N1 3.191(11) . ? O12 N1 2.944(11) . ? O13 N2 2.709(11) . ? O14 N3 2.635(11) . ? C1 C6 1.393(13) . ? C1 C2 1.415(15) . ? C2 C3 1.379(14) . ? C2 C36 1.522(13) . ? C3 C4 1.416(13) . ? C4 C5 1.382(14) . ? C4 C7 1.499(13) . ? C5 C6 1.406(13) . ? C6 C8 1.478(14) . ? C9 C10 1.483(13) . ? C10 C15 1.382(13) . ? C10 C11 1.432(13) . ? C11 C12 1.391(14) . ? C12 C13 1.375(13) . ? C12 C17 1.500(12) . ? C13 C14 1.392(13) . ? C14 C15 1.381(15) . ? C14 C16 1.518(13) . ? C18 C19 1.480(13) . ? C19 C24 1.371(14) . ? C19 C20 1.416(14) . ? C20 C21 1.410(12) . ? C21 C22 1.383(13) . ? C21 C26 1.512(14) . ? C22 C23 1.408(14) . ? C23 C24 1.381(13) . ? C23 C25 1.487(13) . ? C27 C28 1.474(13) . ? C28 C33 1.396(13) . ? C28 C29 1.421(13) . ? C29 C30 1.426(13) . ? C30 C31 1.348(13) . ? C30 C35 1.497(13) . ? C31 C32 1.393(13) . ? C32 C33 1.381(14) . ? C32 C34 1.544(14) . ? N1 C37 1.315(12) . ? N1 C41 1.340(13) . ? C37 C38 1.346(13) . ? C38 C39 1.379(14) . ? C39 C40 1.380(15) . ? C40 C41 1.341(14) . ? N2 C42 1.314(12) . ? N2 C46 1.348(12) . ? C42 C43 1.397(14) . ? C43 C44 1.388(15) . ? C44 C45 1.372(15) . ? C45 C46 1.403(15) . ? N3 C47 1.312(13) . ? N3 C51 1.353(13) . ? C47 C48 1.385(15) . ? C48 C49 1.369(16) . ? C49 C50 1.398(17) . ? C50 C51 1.380(15) . ? C52 C53 1.329(18) . ? C52 C54 1.38(2) 3_867 ? C53 C54 1.33(2) . ? C54 C52 1.38(2) 3_867 ? 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 O10 U1 O9 177.1(3) . . ? O10 U1 O1 94.5(3) . . ? O9 U1 O1 86.7(3) . . ? O10 U1 O3 94.5(2) . . ? O9 U1 O3 86.4(3) . . ? O1 U1 O3 136.4(2) . . ? O10 U1 O13 87.6(2) . . ? O9 U1 O13 89.9(3) . . ? O1 U1 O13 82.6(3) . . ? O3 U1 O13 140.3(3) . . ? O10 U1 O14 83.2(2) . . ? O9 U1 O14 94.5(3) . . ? O1 U1 O14 149.8(2) . . ? O3 U1 O14 73.6(2) . . ? O13 U1 O14 67.2(3) . . ? O10 U1 O2 75.9(2) . . ? O9 U1 O2 107.0(2) . . ? O1 U1 O2 70.9(2) . . ? O3 U1 O2 70.2(2) . . ? O13 U1 O2 147.3(2) . . ? O14 U1 O2 136.2(2) . . ? O10 U1 U2 72.99(18) . . ? O9 U1 U2 104.13(19) . . ? O1 U1 U2 112.50(17) . . ? O3 U1 U2 110.90(16) . . ? O13 U1 U2 32.70(18) . . ? O14 U1 U2 38.07(17) . . ? O2 U1 U2 148.87(14) . . ? O12 U2 O11 177.2(3) . . ? O12 U2 O7 95.2(3) . . ? O11 U2 O7 87.0(3) . . ? O12 U2 O5 93.5(3) . . ? O11 U2 O5 86.1(3) . . ? O7 U2 O5 135.9(2) . . ? O12 U2 O13 87.6(3) . . ? O11 U2 O13 91.0(3) . . ? O7 U2 O13 82.3(3) . . ? O5 U2 O13 141.3(3) . . ? O12 U2 O14 87.0(3) . . ? O11 U2 O14 90.2(3) . . ? O7 U2 O14 149.1(2) . . ? O5 U2 O14 74.4(2) . . ? O13 U2 O14 67.0(3) . . ? O12 U2 O6 74.5(2) . . ? O11 U2 O6 108.0(2) . . ? O7 U2 O6 70.7(2) . . ? O5 U2 O6 70.3(2) . . ? O13 U2 O6 145.6(2) . . ? O14 U2 O6 138.6(2) . . ? O12 U2 U1 75.1(2) . . ? O11 U2 U1 102.4(2) . . ? O7 U2 U1 113.15(17) . . ? O5 U2 U1 110.89(15) . . ? O13 U2 U1 32.60(18) . . ? O14 U2 U1 37.91(16) . . ? O6 U2 U1 149.56(14) . . ? C1 O1 U1 122.0(6) . . ? C8 O2 C9 113.2(7) . . ? C8 O2 U1 119.4(6) . . ? C9 O2 U1 119.2(5) . . ? C11 O3 U1 129.6(6) . . ? C18 O4 C17 112.2(7) . . ? C20 O5 U2 125.9(6) . . ? C26 O6 C27 112.0(7) . . ? C26 O6 U2 120.1(5) . . ? C27 O6 U2 117.7(5) . . ? C29 O7 U2 127.6(6) . . ? C36 O8 C35 111.7(7) . . ? C36 O8 N1 120.5(5) . . ? C35 O8 N1 127.5(5) . . ? U1 O10 N1 134.0(3) . . ? U2 O12 N1 137.9(4) . . ? U1 O13 U2 114.7(3) . . ? U1 O13 N2 117.2(3) . . ? U2 O13 N2 120.4(3) . . ? U1 O14 U2 104.0(3) . . ? U1 O14 N3 119.5(3) . . ? U2 O14 N3 110.8(3) . . ? O1 C1 C6 118.6(9) . . ? O1 C1 C2 119.9(8) . . ? C6 C1 C2 121.4(9) . . ? C3 C2 C1 118.8(9) . . ? C3 C2 C36 119.7(10) . . ? C1 C2 C36 121.5(9) . . ? C2 C3 C4 121.9(10) . . ? C5 C4 C3 117.0(9) . . ? C5 C4 C7 122.3(9) . . ? C3 C4 C7 120.8(10) . . ? C4 C5 C6 123.7(9) . . ? C1 C6 C5 117.2(9) . . ? C1 C6 C8 119.4(9) . . ? C5 C6 C8 123.4(9) . . ? O2 C8 C6 110.9(8) . . ? O2 C9 C10 110.4(7) . . ? C15 C10 C11 118.3(9) . . ? C15 C10 C9 122.4(8) . . ? C11 C10 C9 119.3(9) . . ? O3 C11 C12 123.9(8) . . ? O3 C11 C10 116.6(9) . . ? C12 C11 C10 119.5(9) . . ? C13 C12 C11 119.4(8) . . ? C13 C12 C17 121.2(9) . . ? C11 C12 C17 119.4(8) . . ? C12 C13 C14 122.6(10) . . ? C15 C14 C13 117.5(9) . . ? C15 C14 C16 121.8(9) . . ? C13 C14 C16 120.6(10) . . ? C14 C15 C10 122.6(9) . . ? O4 C17 C12 109.9(7) . . ? O4 C18 C19 111.3(8) . . ? C24 C19 C20 119.1(9) . . ? C24 C19 C18 120.9(10) . . ? C20 C19 C18 119.9(9) . . ? O5 C20 C21 119.2(9) . . ? O5 C20 C19 122.7(8) . . ? C21 C20 C19 117.9(9) . . ? C22 C21 C20 120.5(9) . . ? C22 C21 C26 120.2(8) . . ? C20 C21 C26 119.1(9) . . ? C21 C22 C23 122.0(8) . . ? C24 C23 C22 115.9(9) . . ? C24 C23 C25 122.1(10) . . ? C22 C23 C25 122.0(9) . . ? C19 C24 C23 124.5(10) . . ? O6 C26 C21 110.1(7) . . ? O6 C27 C28 109.1(7) . . ? C33 C28 C29 119.6(9) . . ? C33 C28 C27 120.9(8) . . ? C29 C28 C27 119.5(9) . . ? O7 C29 C28 117.8(9) . . ? O7 C29 C30 124.1(8) . . ? C28 C29 C30 118.1(9) . . ? C31 C30 C29 119.6(9) . . ? C31 C30 C35 122.0(9) . . ? C29 C30 C35 118.4(9) . . ? C30 C31 C32 123.3(10) . . ? C33 C32 C31 117.9(9) . . ? C33 C32 C34 121.3(9) . . ? C31 C32 C34 120.7(9) . . ? C32 C33 C28 121.5(9) . . ? O8 C35 C30 108.6(7) . . ? O8 C36 C2 109.3(7) . . ? C37 N1 C41 122.7(9) . . ? C37 N1 O8 111.2(7) . . ? C41 N1 O8 118.2(7) . . ? C37 N1 O12 84.5(6) . . ? C41 N1 O12 122.8(8) . . ? O8 N1 O12 88.2(3) . . ? C37 N1 O10 137.3(8) . . ? C41 N1 O10 72.6(6) . . ? O8 N1 O10 88.3(3) . . ? O12 N1 O10 57.5(2) . . ? N1 C37 C38 120.9(9) . . ? C37 C38 C39 117.5(10) . . ? C38 C39 C40 120.8(10) . . ? C41 C40 C39 118.7(10) . . ? N1 C41 C40 119.3(10) . . ? C42 N2 C46 120.6(9) . . ? C42 N2 O13 117.8(7) . . ? C46 N2 O13 117.6(7) . . ? N2 C42 C43 121.2(10) . . ? C44 C43 C42 120.0(10) . . ? C45 C44 C43 117.7(10) . . ? C44 C45 C46 120.2(10) . . ? N2 C46 C45 120.2(10) . . ? C47 N3 C51 118.8(9) . . ? C47 N3 O14 111.2(7) . . ? C51 N3 O14 128.9(7) . . ? N3 C47 C48 123.1(10) . . ? C49 C48 C47 118.9(11) . . ? C48 C49 C50 118.7(11) . . ? C51 C50 C49 118.9(11) . . ? N3 C51 C50 121.5(11) . . ? C53 C52 C54 120.1(15) . 3_867 ? C52 C53 C54 121.2(15) . . ? C53 C54 C52 118.5(14) . 3_867 ? #==END data_7 _database_code_CSD 153526 # LOW QUALITY STRUCTURE DUE TO POOR SINGLE-CRYSTALS. # MUST BE CONSIDERED AS A RELIABLE MODEL # AND NOT AS A HIGH PRECISION STRUCTURE. _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C114 H185.50 N3.50 O29.50 U4' _chemical_formula_weight 3029.28 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' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 42.749(9) _cell_length_b 17.169(5) _cell_length_c 43.577(10) _cell_angle_alpha 90.00 _cell_angle_beta 117.829(12) _cell_angle_gamma 90.00 _cell_volume 28285(5) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 81335 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.0 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method ? _exptl_crystal_F_000 11984 _exptl_absorpt_coefficient_mu 4.629 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.352 _exptl_absorpt_correction_T_max 0.429 _exptl_absorpt_process_details 'program MULABS from PLATON (Spek, 1997)' _exptl_special_details '\f scans with 2\% steps' _diffrn_ambient_temperature 110(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 81335 _diffrn_reflns_av_R_equivalents 0.084 _diffrn_reflns_av_sigmaI/netI 0.103 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 20.82 _reflns_number_total 23002 _reflns_number_gt 3777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and expanded by subsequent Fourier-difference synthesis. The aromatic rings have been refined as idealized hexagons. One triethylammonium molecule (corresponding to N1) has been found, then, being unstable on refinement, was fixed in the following refinement cycles. Uranium, oxygen and nitrogen atoms (unless atom N1) only have been refined anisotropically in order to keep the number of parameters within the limits of the program. Hydrogen atoms were not introduced. 1.2 (CH, CH2) or 1.5 (CH3) times that of the parent atom. 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^)+(0.0223P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23002 _refine_ls_number_parameters 1328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2728 _refine_ls_R_factor_gt 0.1156 _refine_ls_wR_factor_ref 0.2136 _refine_ls_wR_factor_gt 0.1494 _refine_ls_goodness_of_fit_ref 0.860 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 1.359 _refine_ls_shift/su_mean 0.025 _diffrn_measured_fraction_theta_max 0.777 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.777 _refine_diff_density_max 1.119 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.126 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 U1A U 0.56856(10) -0.2043(3) 0.84951(10) 0.0827(14) Uani 1 1 d . . . U2A U 0.53967(10) -0.2153(3) 0.72791(10) 0.0850(14) Uani 1 1 d . . . U3A U 0.43495(11) -0.2045(3) 0.69742(11) 0.0979(16) Uani 1 1 d . . . U4A U 0.46285(9) -0.1997(3) 0.82336(9) 0.0750(14) Uani 1 1 d . . . O1A O 0.6020(12) -0.209(3) 0.9100(3) 0.063(19) Uani 1 1 d . . . O2A O 0.6263(13) -0.208(3) 0.8584(12) 0.052(17) Uani 1 1 d . . . O3A O 0.6582(11) -0.1346(13) 0.8130(3) 0.037(16) Uani 1 1 d . . . O4A O 0.6014(9) -0.2417(18) 0.7542(9) 0.06(2) Uani 1 1 d . . . O5A O 0.5342(14) -0.227(2) 0.6762(7) 0.10(2) Uani 1 1 d . . . O6A O 0.4611(11) -0.238(3) 0.6063(11) 0.033(15) Uani 1 1 d . . . O7A O 0.4091(12) -0.220(3) 0.6408(12) 0.047(17) Uani 1 1 d . . . O8A O 0.3767(4) -0.2184(19) 0.6867(8) 0.054(17) Uani 1 1 d . . . O9A O 0.3437(14) -0.121(3) 0.7296(13) 0.064(19) Uani 1 1 d . . . O10A O 0.4012(11) -0.218(3) 0.7935(11) 0.037(15) Uani 1 1 d . . . O11A O 0.4577(12) -0.207(3) 0.8724(11) 0.041(15) Uani 1 1 d . . . O12A O 0.5387(10) -0.227(2) 0.9443(10) 0.061(14) Uani 1 1 d . . . O13A O 0.5649(10) -0.309(3) 0.8488(10) 0.059(15) Uani 1 1 d . . . O14A O 0.5735 -0.1069 0.8506 0.077 Uani 1 1 d . . . O15A O 0.5312(13) -0.313(3) 0.7307(12) 0.097(18) Uani 1 1 d . . . O16A O 0.5469(13) -0.1094(9) 0.7254(13) 0.095 Uiso 1 1 d . . . O17A O 0.4468(11) -0.3012(10) 0.7103(10) 0.082(17) Uani 1 1 d . . . O18A O 0.4290(11) -0.1047(9) 0.6878(10) 0.056(15) Uani 1 1 d . . . O19A O 0.4639(9) -0.304(2) 0.8219(9) 0.037(12) Uani 1 1 d . . . O20A O 0.4623(12) -0.102(3) 0.8261(11) 0.071(16) Uani 1 1 d . . . O21A O 0.5622(16) -0.205(4) 0.7896(14) 0.14(2) Uani 1 1 d . . . O22A O 0.4444(13) -0.183(4) 0.7582(15) 0.16(3) Uani 1 1 d . . . O23A O 0.5239(4) -0.198(3) 0.8661(8) 0.065(15) Uani 1 1 d . . . O24A O 0.5069(3) -0.177(3) 0.8002(5) 0.080(18) Uani 1 1 d . . . O25A O 0.4938(6) -0.171(3) 0.7434(9) 0.10(2) Uani 1 1 d . . . O26A O 0.4807(12) -0.200(3) 0.6866(12) 0.093(18) Uani 1 1 d . . . C1A C 0.6178(14) -0.244(2) 0.9412(10) 0.068(14) Uiso 1 1 d G . . C2A C 0.6033(10) -0.246(2) 0.9638(14) 0.070(14) Uiso 1 1 d G . . C3A C 0.6169(12) -0.296(3) 0.9922(11) 0.069(14) Uiso 1 1 d G . . C4A C 0.6452(12) -0.345(2) 0.9978(10) 0.065(14) Uiso 1 1 d G . . C5A C 0.6597(10) -0.343(3) 0.9752(14) 0.063(14) Uiso 1 1 d G . . C6A C 0.6460(14) -0.293(3) 0.9469(12) 0.063(13) Uiso 1 1 d G . . C7A C 0.6624(11) -0.405(2) 1.0299(10) 0.11(4) Uiso 1 1 d . . . C8A C 0.7024(10) -0.397(3) 1.0473(13) 0.07(3) Uiso 1 1 d . . . C9A C 0.648(2) -0.387(5) 1.0553(15) 0.11(7) Uiso 1 1 d . . . C10A C 0.6517(15) -0.488(2) 1.0156(16) 0.09(3) Uiso 1 1 d . . . C11A C 0.6633(17) -0.292(4) 0.9256(17) 0.05(2) Uiso 1 1 d . . . C12A C 0.6745(11) -0.213(2) 0.9137(12) 0.039(12) Uiso 1 1 d G . . C13A C 0.6566(9) -0.179(3) 0.8811(10) 0.046(12) Uiso 1 1 d G . . C14A C 0.6695(12) -0.111(3) 0.8738(9) 0.051(13) Uiso 1 1 d G . . C15A C 0.7004(12) -0.078(2) 0.8990(13) 0.049(13) Uiso 1 1 d G . . C16A C 0.7183(9) -0.112(2) 0.9316(11) 0.047(12) Uiso 1 1 d G . . C17A C 0.7054(11) -0.180(3) 0.9390(9) 0.044(12) Uiso 1 1 d G . . C18A C 0.7548(10) -0.062(3) 0.9587(11) 0.09(3) Uiso 1 1 d . . . C19A C 0.7702(19) -0.107(5) 0.9927(12) 0.333 Uiso 1 1 d . . . C20A C 0.7416(19) 0.019(3) 0.9614(19) 0.14(4) Uiso 1 1 d . . . C21A C 0.7785(13) -0.062(4) 0.941(2) 0.134 Uiso 1 1 d . . . C22A C 0.658(3) -0.081(4) 0.8371(12) 0.11(5) Uiso 1 1 d . . . C23A C 0.640(3) -0.101(4) 0.7799(13) 0.14(4) Uiso 1 1 d . . . C24A C 0.6435(11) -0.161(2) 0.7556(11) 0.096(11) Uiso 1 1 d G . . C25A C 0.6211(10) -0.223(2) 0.7393(11) 0.096(11) Uiso 1 1 d G . . C26A C 0.6255(11) -0.267(2) 0.7149(10) 0.096(11) Uiso 1 1 d G . . C27A C 0.6524(13) -0.249(3) 0.7067(11) 0.096(11) Uiso 1 1 d G . . C28A C 0.6749(11) -0.187(3) 0.7229(12) 0.096(11) Uiso 1 1 d G . . C29A C 0.6704(10) -0.143(3) 0.7474(12) 0.096(11) Uiso 1 1 d G . . C30A C 0.7025(9) -0.188(2) 0.7089(10) 0.05(2) Uiso 1 1 d . . . C31A C 0.7392(9) -0.178(4) 0.7395(13) 0.11(3) Uiso 1 1 d . . . C32A C 0.6940(15) -0.121(3) 0.6832(14) 0.11(3) Uiso 1 1 d . . . C33A C 0.6998(16) -0.266(3) 0.6911(16) 0.134 Uiso 1 1 d . . . C34A C 0.604(2) -0.348(5) 0.704(2) 0.10(3) Uiso 1 1 d . . . C35A C 0.5689(18) -0.341(5) 0.6647(12) 0.12(2) Uiso 1 1 d G . . C36A C 0.543(2) -0.283(4) 0.6553(19) 0.12(2) Uiso 1 1 d G . . C37A C 0.5183(17) -0.275(3) 0.621(2) 0.12(2) Uiso 1 1 d G . . C38A C 0.5186(16) -0.324(4) 0.5956(13) 0.12(2) Uiso 1 1 d G . . C39A C 0.544(2) -0.382(4) 0.6051(17) 0.12(2) Uiso 1 1 d G . . C40A C 0.5692(18) -0.391(4) 0.640(2) 0.12(2) Uiso 1 1 d G . . C41A C 0.5497(14) -0.440(3) 0.5785(13) 0.11(3) Uiso 1 1 d . . . C42A C 0.5161(17) -0.440(4) 0.5440(14) 0.12(4) Uiso 1 1 d . . . C43A C 0.5808(19) -0.410(5) 0.574(2) 0.10(6) Uiso 1 1 d . . . C44A C 0.557(2) -0.522(3) 0.5940(18) 0.147 Uiso 1 1 d . . . C45A C 0.495(2) -0.195(5) 0.614(2) 0.09(3) Uiso 1 1 d . . . C46A C 0.435(2) -0.172(4) 0.5983(19) 0.07(3) Uiso 1 1 d . . . C47A C 0.3965(10) -0.206(3) 0.5816(16) 0.083(15) Uiso 1 1 d G . . C48A C 0.3879(14) -0.235(3) 0.6064(9) 0.087(15) Uiso 1 1 d G . . C49A C 0.3564(16) -0.276(3) 0.5961(12) 0.084(15) Uiso 1 1 d G . . C50A C 0.3336(11) -0.287(3) 0.5610(15) 0.080(14) Uiso 1 1 d G . . C51A C 0.3422(12) -0.258(3) 0.5362(8) 0.082(14) Uiso 1 1 d G . . C52A C 0.3737(14) -0.217(3) 0.5465(13) 0.079(14) Uiso 1 1 d G . . C53A C 0.3160(11) -0.266(3) 0.4945(10) 0.13(4) Uiso 1 1 d . . . C54A C 0.2812(12) -0.300(4) 0.4897(16) 0.16(4) Uiso 1 1 d . . . C55A C 0.3337(17) -0.319(4) 0.4796(13) 0.10(3) Uiso 1 1 d . . . C56A C 0.311(2) -0.185(3) 0.4786(14) 0.14(5) Uiso 1 1 d . . . C57A C 0.343(2) -0.301(5) 0.620(2) 0.09(3) Uiso 1 1 d . . . C58A C 0.3227(10) -0.251(2) 0.6353(10) 0.075(15) Uiso 1 1 d G . . C59A C 0.3426(9) -0.210(3) 0.6659(10) 0.075(16) Uiso 1 1 d G . . C60A C 0.3286(10) -0.144(2) 0.6735(10) 0.075(15) Uiso 1 1 d G . . C61A C 0.2948(10) -0.119(2) 0.6504(12) 0.068(14) Uiso 1 1 d G . . C62A C 0.2750(8) -0.160(3) 0.6197(10) 0.067(14) Uiso 1 1 d G . . C63A C 0.2889(9) -0.226(3) 0.6122(9) 0.071(14) Uiso 1 1 d G . . C64A C 0.2308(9) -0.150(2) 0.5930(9) 0.12(4) Uiso 1 1 d . . . C65A C 0.2151(13) -0.228(3) 0.5950(18) 0.14(4) Uiso 1 1 d . . . C66A C 0.2280(15) -0.132(4) 0.5577(9) 0.08(4) Uiso 1 1 d . . . C67A C 0.2196(12) -0.083(3) 0.6085(15) 0.08(3) Uiso 1 1 d . . . C68A C 0.3484(15) -0.089(3) 0.7034(16) 0.024(18) Uiso 1 1 d . . . C69A C 0.3631(19) -0.074(4) 0.7586(19) 0.06(2) Uiso 1 1 d . . . C70A C 0.3598(14) -0.106(3) 0.7931(11) 0.082(15) Uiso 1 1 d G . . C71A C 0.3773(12) -0.176(4) 0.8067(14) 0.079(15) Uiso 1 1 d G . . C72A C 0.3733(12) -0.213(2) 0.8330(14) 0.078(14) Uiso 1 1 d G . . C73A C 0.3519(13) -0.181(3) 0.8457(11) 0.077(15) Uiso 1 1 d G . . C74A C 0.3344(11) -0.111(3) 0.8321(14) 0.082(15) Uiso 1 1 d G . . C75A C 0.3383(13) -0.074(2) 0.8058(14) 0.082(15) Uiso 1 1 d G . . C76A C 0.3060(11) -0.072(2) 0.8426(11) 0.10(3) Uiso 1 1 d . . . C77A C 0.2691(10) -0.084(4) 0.8127(15) 0.10(3) Uiso 1 1 d . . . C78A C 0.3098(17) -0.111(4) 0.8754(13) 0.13(4) Uiso 1 1 d . . . C79A C 0.3143(18) 0.014(2) 0.8489(19) 0.165 Uiso 1 1 d . . . C80A C 0.3921(18) -0.287(3) 0.8519(11) 0.07(5) Uiso 1 1 d . . . C81A C 0.4201(11) -0.276(3) 0.8892(8) 0.074(14) Uiso 1 1 d G . . C82A C 0.4508(13) -0.235(3) 0.8956(11) 0.069(14) Uiso 1 1 d G . . C83A C 0.4757(10) -0.218(3) 0.9295(14) 0.078(14) Uiso 1 1 d G . . C84A C 0.4700(11) -0.242(3) 0.9570(9) 0.082(14) Uiso 1 1 d G . . C85A C 0.4394(13) -0.282(3) 0.9506(10) 0.081(14) Uiso 1 1 d G . . C86A C 0.4144(10) -0.299(3) 0.9167(12) 0.077(14) Uiso 1 1 d G . . C87A C 0.4351(11) -0.316(2) 0.9835(10) 0.08(3) Uiso 1 1 d . . . C88A C 0.4316(18) -0.246(3) 1.0034(13) 0.13(4) Uiso 1 1 d . . . C89A C 0.4678(13) -0.363(3) 1.0061(12) 0.08(3) Uiso 1 1 d . . . C90A C 0.4022(13) -0.366(4) 0.9695(16) 0.113 Uiso 1 1 d . . . C91A C 0.5116(17) -0.177(4) 0.9390(16) 0.04(2) Uiso 1 1 d . . . C92A C 0.5709(19) -0.193(4) 0.9565(17) 0.05(2) Uiso 1 1 d . . . U1B U 1.01784(9) -0.2789(2) 0.80321(8) 0.0576(12) Uani 1 1 d . . . U2B U 0.99055(9) -0.2941(2) 0.67756(8) 0.0580(12) Uani 1 1 d . . . U3B U 0.88510(8) -0.2886(2) 0.64930(8) 0.0564(11) Uani 1 1 d . . . U4B U 0.91117(9) -0.2678(2) 0.77099(8) 0.0570(12) Uani 1 1 d . . . O1B O 1.0499(9) -0.290(2) 0.8603(9) 0.040(12) Uani 1 1 d . . . O2B O 1.0725(11) -0.292(3) 0.8097(10) 0.065(15) Uani 1 1 d . . . O3B O 1.1092(11) -0.407(2) 0.7727(11) 0.057(15) Uani 1 1 d . . . O4B O 1.0491(11) -0.297(3) 0.7055(10) 0.062(15) Uani 1 1 d . . . O5B O 0.9998(11) -0.329(2) 0.6348(10) 0.055(15) Uani 1 1 d . . . O6B O 0.9154(9) -0.284(2) 0.5591(8) 0.027(11) Uani 1 1 d . . . O7B O 0.8527(9) -0.300(2) 0.5921(9) 0.041(13) Uani 1 1 d . . . O8B O 0.8286(10) -0.287(2) 0.6418(9) 0.051(13) Uani 1 1 d . . . O9B O 0.8045(12) -0.380(3) 0.6875(11) 0.074(17) Uani 1 1 d . . . O10B O 0.8506(11) -0.266(2) 0.7464(10) 0.065(15) Uani 1 1 d . . . O11B O 0.9064(11) -0.266(2) 0.8171(10) 0.069(15) Uani 1 1 d . . . O12B O 0.9895(8) -0.2505(18) 0.8913(8) 0.015(10) Uani 1 1 d . . . O13B O 1.0229(12) -0.174(2) 0.8062(11) 0.069(17) Uani 1 1 d . . . O14B O 1.0101(10) -0.378(2) 0.8003(10) 0.043(13) Uani 1 1 d . . . O15B O 0.9922(9) -0.191(2) 0.6744(9) 0.029(12) Uani 1 1 d . . . O16B O 0.9915(10) -0.392(2) 0.6853(9) 0.039(13) Uani 1 1 d . . . O17B O 0.8827(11) -0.184(2) 0.6459(10) 0.052(15) Uani 1 1 d . . . O18B O 0.8885(10) -0.395(2) 0.6538(9) 0.040(13) Uani 1 1 d . . . O19B O 0.9095(9) -0.1641(19) 0.7685(9) 0.016(11) Uani 1 1 d . . . O20B O 0.9126(9) -0.3652(5) 0.7733(8) 0.023(11) Uani 1 1 d . . . O21B O 1.0083(11) -0.271(3) 0.7376(11) 0.072(16) Uani 1 1 d . . . O22B O 0.8920(10) -0.286(2) 0.7096(9) 0.045(13) Uani 1 1 d . . . O23B O 0.9712(5) -0.254(2) 0.8179(7) 0.058(15) Uani 1 1 d . . . O24B O 0.9575(10) -0.259(2) 0.7525(10) 0.056(15) Uani 1 1 d . . . O25B O 0.9470(9) -0.266(2) 0.6987(9) 0.036(12) Uani 1 1 d . . . O26B O 0.9297(9) -0.292(2) 0.6321(9) 0.044(13) Uani 1 1 d . . . C1B C 1.0630(11) -0.246(2) 0.8908(9) 0.045(12) Uiso 1 1 d G . . C2B C 1.0511(9) -0.251(2) 0.9155(12) 0.044(12) Uiso 1 1 d G . . C3B C 1.0702(12) -0.215(3) 0.9476(10) 0.038(11) Uiso 1 1 d G . . C4B C 1.1012(11) -0.175(2) 0.9551(9) 0.037(11) Uiso 1 1 d G . . C5B C 1.1131(9) -0.170(2) 0.9305(12) 0.037(11) Uiso 1 1 d G . . C6B C 1.0940(12) -0.206(3) 0.8983(10) 0.045(12) Uiso 1 1 d G . . C7B C 1.1200(18) -0.133(4) 0.9901(18) 0.05(2) Uiso 1 1 d . . . C8B C 1.1619(17) -0.157(4) 1.0094(16) 0.05(2) Uiso 1 1 d . . . C9B C 1.115(2) -0.147(5) 1.018(2) 0.11(3) Uiso 1 1 d . . . C10B C 1.1215(18) -0.044(4) 0.9856(18) 0.06(2) Uiso 1 1 d . . . C11B C 1.1120(14) -0.196(3) 0.8720(13) 0.016(17) Uiso 1 1 d . . . C12B C 1.1238(13) -0.283(2) 0.8668(14) 0.049(13) Uiso 1 1 d G . . C13B C 1.1049(10) -0.325(3) 0.8365(11) 0.054(13) Uiso 1 1 d G . . C14B C 1.1167(12) -0.399(3) 0.8331(10) 0.052(13) Uiso 1 1 d G . . C15B C 1.1474(13) -0.429(2) 0.8600(14) 0.049(13) Uiso 1 1 d G . . C16B C 1.1662(10) -0.387(3) 0.8903(11) 0.047(13) Uiso 1 1 d G . . C17B C 1.1544(12) -0.313(3) 0.8936(10) 0.051(13) Uiso 1 1 d G . . C18B C 1.1979(15) -0.426(4) 0.9195(15) 0.09(3) Uiso 1 1 d . . . C19B C 1.197(2) -0.514(4) 0.922(2) 0.11(3) Uiso 1 1 d . . . C20B C 1.224(3) -0.402(6) 0.906(3) 0.08(6) Uiso 1 1 d . . . C21B C 1.208(3) -0.387(5) 0.954(2) 0.12(4) Uiso 1 1 d . . . C22B C 1.096(2) -0.436(5) 0.796(2) 0.09(3) Uiso 1 1 d . . . C23B C 1.086(2) -0.446(5) 0.737(2) 0.08(3) Uiso 1 1 d . . . C24B C 1.0964(12) -0.390(3) 0.7151(9) 0.045(8) Uiso 1 1 d G . . C25B C 1.0752(10) -0.328(3) 0.6960(12) 0.045(8) Uiso 1 1 d G . . C26B C 1.0794(10) -0.297(2) 0.6688(11) 0.045(8) Uiso 1 1 d G . . C27B C 1.1048(11) -0.327(2) 0.6606(9) 0.045(8) Uiso 1 1 d G . . C28B C 1.1260(9) -0.388(2) 0.6798(11) 0.045(8) Uiso 1 1 d G . . C29B C 1.1218(10) -0.420(2) 0.7070(10) 0.045(8) Uiso 1 1 d G . . C30B C 1.1532(11) -0.422(3) 0.6664(12) 0.08(6) Uiso 1 1 d . . . C31B C 1.1731(18) -0.354(4) 0.662(2) 0.09(5) Uiso 1 1 d . . . C32B C 1.1317(17) -0.464(4) 0.6322(13) 0.13(4) Uiso 1 1 d . . . C33B C 1.1786(15) -0.478(4) 0.6937(16) 0.14(4) Uiso 1 1 d . . . C34B C 1.0594(13) -0.221(3) 0.6500(13) 0.017(16) Uiso 1 1 d . . . C45B C 0.944(2) -0.330(5) 0.555(2) 0.09(3) Uiso 1 1 d . . . C35B C 1.0288(13) -0.238(3) 0.6129(9) 0.072(14) Uiso 1 1 d G . . C36B C 0.9978(15) -0.281(3) 0.6024(13) 0.073(14) Uiso 1 1 d G . . C37B C 0.9736(11) -0.286(3) 0.5674(15) 0.077(14) Uiso 1 1 d G . . C38B C 0.9805(12) -0.248(3) 0.5429(9) 0.073(14) Uiso 1 1 d G . . C39B C 1.0114(14) -0.206(3) 0.5534(11) 0.075(14) Uiso 1 1 d G . . C40B C 1.0356(10) -0.201(3) 0.5885(13) 0.069(14) Uiso 1 1 d G . . C41B C 1.0188(12) -0.193(3) 0.5204(11) 0.09(4) Uiso 1 1 d . . . C42B C 1.0142(18) -0.271(4) 0.5021(14) 0.11(3) Uiso 1 1 d . . . C43B C 1.0563(14) -0.163(4) 0.5335(17) 0.11(3) Uiso 1 1 d . . . C44B C 0.9921(18) -0.134(4) 0.4963(15) 0.20(6) Uiso 1 1 d . . . C46B C 0.8836(19) -0.331(4) 0.5453(17) 0.05(2) Uiso 1 1 d . . . C47B C 0.8510(9) -0.281(2) 0.5372(13) 0.045(8) Uiso 1 1 d G . . C48B C 0.8385(11) -0.269(2) 0.5611(9) 0.045(8) Uiso 1 1 d G . . C49B C 0.8101(12) -0.219(3) 0.5532(11) 0.045(8) Uiso 1 1 d G . . C50B C 0.7943(9) -0.181(2) 0.5214(13) 0.045(8) Uiso 1 1 d G . . C51B C 0.8068(11) -0.193(2) 0.4975(9) 0.045(8) Uiso 1 1 d G . . C52B C 0.8352(12) -0.243(3) 0.5054(11) 0.045(8) Uiso 1 1 d G . . C53B C 0.791(2) -0.150(5) 0.459(2) 0.09(3) Uiso 1 1 d . . . C54B C 0.777(2) -0.217(5) 0.430(2) 0.09(3) Uiso 1 1 d . . . C55B C 0.756(2) -0.104(5) 0.455(2) 0.08(3) Uiso 1 1 d . . . C56B C 0.8251(18) -0.091(4) 0.4687(17) 0.06(2) Uiso 1 1 d . . . C57B C 0.7943(15) -0.215(4) 0.5817(14) 0.036(19) Uiso 1 1 d . . . C58B C 0.7818(15) -0.287(3) 0.5876(16) 0.067(14) Uiso 1 1 d G . . C59B C 0.7975(11) -0.321(3) 0.6204(13) 0.073(14) Uiso 1 1 d G . . C60B C 0.7806(16) -0.382(3) 0.6278(11) 0.078(15) Uiso 1 1 d G . . C61B C 0.7481(16) -0.409(3) 0.6024(17) 0.074(14) Uiso 1 1 d G . . C62B C 0.7325(11) -0.375(3) 0.5697(14) 0.069(14) Uiso 1 1 d G . . C63B C 0.7493(15) -0.314(3) 0.5623(11) 0.066(14) Uiso 1 1 d G . . C64B C 0.699(2) -0.403(5) 0.545(2) 0.09(3) Uiso 1 1 d . . . C65B C 0.6810(16) -0.361(3) 0.5077(16) 0.033(19) Uiso 1 1 d . . . C66B C 0.666(3) -0.377(6) 0.556(3) 0.16(4) Uiso 1 1 d . . . C67B C 0.702(2) -0.510(5) 0.539(2) 0.10(3) Uiso 1 1 d . . . C68B C 0.805(2) -0.422(4) 0.656(2) 0.07(3) Uiso 1 1 d . . . C69B C 0.8239(19) -0.423(4) 0.7196(19) 0.06(2) Uiso 1 1 d . . . C70B C 0.8141(12) -0.388(3) 0.7476(10) 0.062(13) Uiso 1 1 d G . . C71B C 0.8298(11) -0.316(3) 0.7595(12) 0.063(13) Uiso 1 1 d G . . C72B C 0.8244(11) -0.276(2) 0.7846(12) 0.054(13) Uiso 1 1 d G . . C73B C 0.8035(12) -0.309(3) 0.7977(10) 0.062(13) Uiso 1 1 d G . . C74B C 0.7878(10) -0.381(3) 0.7859(12) 0.063(13) Uiso 1 1 d G . . C75B C 0.7932(11) -0.421(2) 0.7608(12) 0.060(13) Uiso 1 1 d G . . C76B C 0.7640(11) -0.424(2) 0.8015(10) 0.11(4) Uiso 1 1 d . . . C77B C 0.7756(17) -0.392(4) 0.8377(11) 0.14(4) Uiso 1 1 d . . . C78B C 0.7254(9) -0.405(3) 0.7777(15) 0.08(3) Uiso 1 1 d . . . C79B C 0.7706(16) -0.511(2) 0.8024(17) 0.107 Uiso 1 1 d . . . C80B C 0.8342(17) -0.204(5) 0.7992(17) 0.06(2) Uiso 1 1 d . . . C81B C 0.8700(9) -0.207(2) 0.8404(7) 0.037(11) Uiso 1 1 d G . . C82B C 0.9015(11) -0.244(2) 0.8473(9) 0.028(11) Uiso 1 1 d G . . C83B C 0.9280(8) -0.252(2) 0.8813(11) 0.031(11) Uiso 1 1 d G . . C84B C 0.9231(9) -0.222(2) 0.9085(7) 0.027(11) Uiso 1 1 d G . . C85B C 0.8916(10) -0.185(2) 0.9015(8) 0.031(11) Uiso 1 1 d G . . C86B C 0.8651(8) -0.177(2) 0.8675(10) 0.037(11) Uiso 1 1 d G . . C87B C 0.8880(11) -0.159(2) 0.9361(10) 0.17(5) Uiso 1 1 d . . . C88B C 0.9193(17) -0.107(4) 0.9580(13) 0.17(5) Uiso 1 1 d . . . C89B C 0.8534(16) -0.116(4) 0.9240(16) 0.14(4) Uiso 1 1 d . . . C90B C 0.8884(15) -0.233(3) 0.9554(11) 0.06(2) Uiso 1 1 d . . . C91B C 0.954(3) -0.302(6) 0.883(2) 0.13(4) Uiso 1 1 d . . . C92B C 1.023(2) -0.305(5) 0.909(2) 0.10(3) Uiso 1 1 d . . . N1 N 0.5697 0.0232 0.8878 0.120 Uiso 1 1 d . . . C1 C 0.5462 0.0891 0.8626 0.120 Uiso 1 1 d . . . C2 C 0.5018 0.0837 0.8452 0.150 Uiso 1 1 d . . . C3 C 0.5654 0.0280 0.9201 0.120 Uiso 1 1 d . . . C4 C 0.5647 0.1018 0.9394 0.150 Uiso 1 1 d . . . C5 C 0.6028 -0.0200 0.9074 0.120 Uiso 1 1 d . . . C6 C 0.6413 -0.0043 0.9287 0.150 Uiso 1 1 d . . . N2 N 0.4744(15) -0.445(5) 0.7535(17) 0.06(5) Uani 1 1 d . . . C7 C 0.5004(18) -0.402(6) 0.7841(18) 0.15(5) Uiso 1 1 d . . . C8 C 0.511(3) -0.459(6) 0.814(3) 0.13(4) Uiso 1 1 d . . . C9 C 0.4870(19) -0.487(4) 0.7318(18) 0.08(3) Uiso 1 1 d . . . C10 C 0.472(2) -0.484(5) 0.6923(18) 0.121 Uiso 1 1 d . . . C11 C 0.4357(15) -0.439(6) 0.7406(16) 0.14(4) Uiso 1 1 d . . . C12 C 0.415(2) -0.446(7) 0.761(3) 0.201 Uiso 1 1 d . . . N3 N 0.9954(14) -0.491(3) 0.6239(14) 0.050(17) Uani 1 1 d . . . C13 C 0.9750(17) -0.565(4) 0.6357(16) 0.04(2) Uiso 1 1 d . . . C14 C 0.9336(16) -0.506(3) 0.6177(15) 0.029(19) Uiso 1 1 d . . . C15 C 1.041(2) -0.498(5) 0.654(2) 0.08(3) Uiso 1 1 d . . . C16 C 1.053(2) -0.591(6) 0.658(2) 0.11(3) Uiso 1 1 d . . . C17 C 0.9943(17) -0.518(4) 0.5869(16) 0.04(2) Uiso 1 1 d . . . C18 C 1.0109(17) -0.483(4) 0.5776(16) 0.036(19) Uiso 1 1 d . . . N4 N 0.9645(17) -0.506(4) 0.7622(16) 0.08(2) Uani 1 1 d . . . C19 C 0.9404(18) -0.554(4) 0.7750(18) 0.05(2) Uiso 1 1 d . . . C20 C 0.9542(16) -0.512(4) 0.8134(16) 0.04(2) Uiso 1 1 d . . . C21 C 0.9356(19) -0.491(4) 0.7187(19) 0.058 Uiso 1 1 d . . . C22 C 0.903(2) -0.553(5) 0.694(2) 0.09(3) Uiso 1 1 d . . . C23 C 0.9828(16) -0.572(4) 0.7620(16) 0.04(2) Uiso 1 1 d . . . C24 C 1.0057(18) -0.527(4) 0.7396(18) 0.06(2) Uiso 1 1 d . . . N5 N 1.062(3) -0.547(5) 0.930(3) 0.08(3) Uani 1 1 d . . . C25 C 1.086(2) -0.583(11) 0.922(5) 0.11(7) Uiso 1 1 d . . . C26 C 1.121(4) -0.589(8) 0.927(4) 0.13(5) Uiso 1 1 d . . . C27 C 1.023(2) -0.581(5) 0.912(2) 0.09(3) Uiso 1 1 d . . . C28 C 1.0031(19) -0.508(4) 0.9129(18) 0.06(2) Uiso 1 1 d . . . C29 C 1.077(3) -0.551(8) 0.969(4) 0.12(5) Uiso 1 1 d . . . C30 C 1.088(3) -0.602(7) 0.984(3) 0.07(4) Uiso 1 1 d . . . N6 N 1.1614(16) -0.231(5) 0.7837(17) 0.09(2) Uani 1 1 d . . . C31 C 1.162(3) -0.233(5) 0.7506(19) 0.06(4) Uiso 1 1 d . . . C32 C 1.1418(17) -0.169(4) 0.7247(17) 0.05(2) Uiso 1 1 d . . . C33 C 1.178(3) -0.305(5) 0.798(3) 0.19(5) Uiso 1 1 d . . . C34 C 1.214(3) -0.323(6) 0.802(3) 0.17(5) Uiso 1 1 d . . . C35 C 1.172(3) -0.161(6) 0.805(3) 0.14(5) Uiso 1 1 d . . . C36 C 1.169(3) -0.164(6) 0.838(3) 0.154 Uiso 1 1 d . . . N7 N 0.3006(19) -0.320(5) 0.7177(19) 0.11(3) Uani 1 1 d . . . C37 C 0.306(3) -0.380(6) 0.743(3) 0.11(4) Uiso 1 1 d . . . C38 C 0.328(4) -0.386(8) 0.782(3) 0.06(5) Uiso 1 1 d . . . C39 C 0.293(3) -0.253(6) 0.734(3) 0.15(5) Uiso 1 1 d . . . C40 C 0.256(3) -0.264(6) 0.729(2) 0.12(4) Uiso 1 1 d . . . C41 C 0.282(2) -0.330(5) 0.680(2) 0.07(3) Uiso 1 1 d . . . C42 C 0.2978(18) -0.396(4) 0.6686(17) 0.06(2) Uiso 1 1 d . . . O1 O 1.061(2) -0.440(5) 0.872(2) 0.05(3) Uani 1 1 d . . . O2 O 1.0879(12) -0.224(3) 0.7622(12) 0.076(17) Uani 1 1 d . . . O3 O 0.3741(12) -0.293(3) 0.7426(12) 0.073(17) Uani 1 1 d . . . O4 O 0.8312(18) -0.477(4) 0.5816(16) 0.10(3) Uani 1 1 d . . . O5 O 1.0645(13) -0.568(3) 0.8400(13) 0.087(18) Uani 1 1 d . . . O6 O 0.6331(19) -0.321(4) 0.8122(19) 0.10(3) Uani 1 1 d . . . O7 O 0.8178(13) -0.197(3) 0.6888(14) 0.11(2) Uani 1 1 d . . . C43 C 0.6157(16) -0.400(4) 0.8136(15) 0.04(2) Uiso 1 1 d . . . C44 C 0.7756(13) -0.192(4) 0.6704(16) 0.06(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1A 0.076(3) 0.081(4) 0.099(4) 0.001(3) 0.047(3) -0.004(3) U2A 0.069(3) 0.111(4) 0.084(3) -0.004(3) 0.044(3) -0.002(3) U3A 0.078(3) 0.121(4) 0.090(4) -0.001(3) 0.035(3) -0.004(3) U4A 0.055(3) 0.104(4) 0.065(3) -0.006(3) 0.027(2) -0.002(3) O1A 0.06(2) 0.06(2) 0.06(2) -0.002(12) 0.032(14) 0.001(12) O2A 0.06(2) 0.05(2) 0.05(2) -0.002(12) 0.025(13) -0.001(12) O3A 0.032(18) 0.044(19) 0.035(19) 0.002(12) 0.017(13) -0.006(12) O4A 0.06(2) 0.06(2) 0.05(2) -0.005(12) 0.028(14) 0.002(12) O5A 0.10(3) 0.09(3) 0.09(3) 0.006(12) 0.033(15) 0.000(12) O6A 0.037(18) 0.033(19) 0.032(18) 0.005(11) 0.020(13) -0.003(11) O7A 0.039(19) 0.05(2) 0.05(2) 0.010(12) 0.017(13) -0.001(12) O8A 0.06(2) 0.05(2) 0.05(2) -0.007(12) 0.022(13) 0.000(12) O9A 0.06(2) 0.06(2) 0.07(2) -0.002(12) 0.029(14) 0.006(12) O10A 0.040(18) 0.037(19) 0.036(18) 0.002(12) 0.019(12) -0.002(12) O11A 0.046(19) 0.040(19) 0.035(18) -0.004(12) 0.017(13) 0.005(12) O12A 0.063(17) 0.055(18) 0.058(17) -0.007(11) 0.023(12) -0.003(12) O13A 0.061(18) 0.057(19) 0.063(18) 0.006(11) 0.033(12) -0.008(11) O14A 0.077 0.077 0.074 0.005 0.033 0.009 O15A 0.10(2) 0.10(2) 0.10(2) 0.004(12) 0.047(13) -0.006(12) O17A 0.09(2) 0.08(2) 0.082(19) 0.005(12) 0.041(13) -0.002(12) O18A 0.056(18) 0.051(18) 0.054(18) 0.005(11) 0.020(12) 0.004(11) O19A 0.040(16) 0.035(17) 0.037(16) 0.014(11) 0.019(11) -0.008(11) O20A 0.072(19) 0.07(2) 0.070(19) 0.006(12) 0.033(13) -0.003(12) O21A 0.15(3) 0.15(3) 0.14(3) 0.004(12) 0.068(15) -0.004(12) O22A 0.17(3) 0.16(3) 0.16(3) 0.005(12) 0.070(17) -0.003(12) O23A 0.063(18) 0.067(19) 0.060(18) -0.003(12) 0.023(12) -0.005(12) O24A 0.08(2) 0.08(2) 0.08(2) -0.002(12) 0.039(13) 0.006(12) O25A 0.10(2) 0.10(2) 0.10(2) 0.000(12) 0.043(14) -0.003(12) O26A 0.10(2) 0.09(2) 0.09(2) 0.006(12) 0.041(13) -0.004(12) U1B 0.050(2) 0.071(4) 0.051(3) -0.008(2) 0.022(2) -0.004(2) U2B 0.057(3) 0.068(3) 0.052(3) -0.006(2) 0.028(2) -0.008(2) U3B 0.052(2) 0.068(3) 0.050(2) -0.001(2) 0.024(2) -0.004(2) U4B 0.054(3) 0.066(3) 0.050(3) -0.001(2) 0.024(2) -0.001(2) O1B 0.037(16) 0.037(16) 0.040(16) 0.000(11) 0.013(11) -0.002(11) O2B 0.070(18) 0.062(19) 0.066(18) 0.008(12) 0.035(12) -0.002(12) O3B 0.058(18) 0.053(18) 0.056(18) -0.002(11) 0.024(12) 0.002(11) O4B 0.065(18) 0.066(19) 0.063(18) -0.005(12) 0.035(12) -0.005(12) O5B 0.056(18) 0.045(18) 0.053(18) 0.006(11) 0.016(12) 0.000(11) O6B 0.035(15) 0.024(16) 0.021(15) -0.005(11) 0.014(11) -0.001(11) O7B 0.041(16) 0.036(17) 0.045(16) 0.002(11) 0.020(11) -0.005(11) O8B 0.048(17) 0.050(17) 0.049(17) 0.003(12) 0.018(12) 0.004(12) O9B 0.07(2) 0.08(2) 0.07(2) -0.002(12) 0.034(13) -0.006(12) O10B 0.065(18) 0.070(19) 0.062(18) -0.002(12) 0.031(12) -0.001(12) O11B 0.067(18) 0.062(19) 0.068(18) 0.005(12) 0.024(12) -0.001(12) O12B 0.019(13) 0.011(13) 0.010(13) 0.005(8) 0.004(9) 0.002(8) O13B 0.07(2) 0.08(2) 0.066(19) -0.001(12) 0.037(13) 0.005(12) O14B 0.039(16) 0.045(17) 0.046(16) -0.003(11) 0.020(12) 0.014(11) O15B 0.038(16) 0.025(16) 0.025(16) 0.002(11) 0.015(11) 0.005(11) O16B 0.043(17) 0.035(17) 0.030(16) -0.009(11) 0.009(12) 0.001(11) O17B 0.051(18) 0.053(19) 0.048(18) 0.002(11) 0.021(12) -0.006(11) O18B 0.040(16) 0.041(17) 0.035(16) -0.007(11) 0.015(12) 0.005(11) O19B 0.017(12) 0.018(12) 0.014(12) 0.000(5) 0.008(7) -0.003(5) O20B 0.016(14) 0.030(15) 0.019(15) -0.004(11) 0.004(11) 0.005(11) O21B 0.072(19) 0.07(2) 0.070(19) 0.001(12) 0.033(13) 0.002(12) O22B 0.053(16) 0.052(17) 0.033(16) 0.000(11) 0.024(12) 0.002(11) O23B 0.060(18) 0.057(19) 0.054(18) 0.008(11) 0.023(12) -0.002(11) O24B 0.056(18) 0.060(19) 0.052(18) 0.000(11) 0.027(12) 0.001(11) O25B 0.035(16) 0.036(17) 0.038(16) 0.002(11) 0.017(12) -0.003(11) O26B 0.047(16) 0.052(17) 0.035(16) -0.002(11) 0.021(12) 0.002(11) N2 0.06(5) 0.06(5) 0.07(5) 0.002(13) 0.03(3) 0.002(13) N3 0.06(2) 0.05(2) 0.05(2) -0.007(12) 0.027(13) 0.001(12) N4 0.08(2) 0.08(2) 0.07(2) 0.005(12) 0.037(15) 0.002(12) N5 0.08(3) 0.08(3) 0.08(3) 0.004(12) 0.035(19) -0.004(12) N6 0.09(3) 0.09(3) 0.09(3) 0.003(12) 0.043(15) -0.002(12) N7 0.12(3) 0.12(3) 0.11(3) 0.001(12) 0.057(17) -0.003(12) O1 0.05(3) 0.05(3) 0.05(3) -0.002(12) 0.023(17) -0.001(12) O2 0.08(2) 0.08(2) 0.07(2) 0.000(12) 0.034(13) 0.002(12) O3 0.07(2) 0.08(2) 0.07(2) 0.006(12) 0.036(13) 0.001(12) O4 0.10(3) 0.10(3) 0.10(3) 0.000(12) 0.047(16) 0.003(12) O5 0.09(2) 0.09(2) 0.09(2) 0.011(12) 0.041(13) -0.010(12) O6 0.10(3) 0.10(3) 0.10(3) 0.000(12) 0.048(18) -0.009(12) O7 0.11(2) 0.11(2) 0.10(2) -0.001(12) 0.050(14) 0.001(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1A O14A 1.68(1) . ? U1A O13A 1.81(5) . ? U1A O23A 2.34(5) . ? U1A O2A 2.31(5) . ? U1A O1A 2.34(2) . ? U1A O21A 2.49(6) . ? U1A O24A 2.55(2) . ? U1A U4A 4.113(6) . ? U1A U2A 4.850(6) . ? U2A O15A 1.72(6) . ? U2A O16A 1.857(13) . ? U2A O5A 2.16(2) . ? U2A O21A 2.40(6) . ? U2A O26A 2.33(5) . ? U2A O4A 2.38(5) . ? U2A O25A 2.47(5) . ? U2A U3A 4.036(6) . ? U3A O17A 1.750(12) . ? U3A O18A 1.753(12) . ? U3A O26A 2.22(5) . ? U3A O7A 2.20(5) . ? U3A O25A 2.44(2) . ? U3A O8A 2.32(4) . ? U3A O22A 2.51(6) . ? U3A U4A 5.044(6) . ? U4A O20A 1.68(5) . ? U4A O19A 1.79(5) . ? U4A O11A 2.25(5) . ? U4A O10A 2.35(5) . ? U4A O23A 2.40(2) . ? U4A O22A 2.58(6) . ? U4A O24A 2.55(2) . ? O1A C1A 1.35(6) . ? O2A C13A 1.30(5) . ? O2A O6 2.92(10) . ? O3A C22A 1.398(13) . ? O3A C23A 1.402(13) . ? O4A C25A 1.316(9) . ? O4A O6 2.62(9) . ? O5A C36A 1.505(13) . ? O6A C45A 1.52(8) . ? O6A C46A 1.52(8) . ? O7A C48A 1.37(5) . ? O8A C59A 1.315(9) . ? O8A O3 2.80(7) . ? O9A C68A 1.36(7) . ? O9A C69A 1.40(8) . ? O10A C71A 1.56(6) . ? O10A O3 2.35(7) . ? O11A C82A 1.27(5) . ? O12A C91A 1.38(6) . ? O12A C92A 1.36(7) . ? O14A N1 2.81(3) . ? O17A N2 3.00(2) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C2A C92A 1.56(7) . ? C3A C4A 1.3900 . ? C4A C5A 1.3900 . ? C4A C7A 1.62(3) . ? C5A C6A 1.3900 . ? C6A C11A 1.43(7) . ? C7A C8A 1.518(12) . ? C7A C9A 1.521(13) . ? C7A C10A 1.525(13) . ? C11A C12A 1.59(8) . ? C12A C13A 1.3900 . ? C12A C17A 1.3900 . ? C13A C14A 1.3900 . ? C14A C15A 1.3900 . ? C14A C22A 1.525(13) . ? C15A C16A 1.3900 . ? C16A C17A 1.3900 . ? C16A C18A 1.685(19) . ? C18A C21A 1.522(6) . ? C18A C20A 1.522(6) . ? C18A C19A 1.523(6) . ? C23A C24A 1.523(13) . ? C24A C25A 1.3900 . ? C24A C29A 1.3900 . ? C25A C26A 1.3900 . ? C26A C27A 1.3900 . ? C26A C34A 1.62(9) . ? C27A C28A 1.3900 . ? C28A C29A 1.3900 . ? C28A C30A 1.56(2) . ? C30A C33A 1.519(9) . ? C30A C31A 1.521(9) . ? C30A C32A 1.522(9) . ? C34A C35A 1.67(9) . ? C35A C36A 1.3900 . ? C35A C40A 1.3900 . ? C36A C37A 1.3900 . ? C37A C38A 1.3900 . ? C37A C45A 1.64(9) . ? C38A C39A 1.3900 . ? C39A C40A 1.3900 . ? C39A C41A 1.63(3) . ? C41A C44A 1.517(13) . ? C41A C43A 1.521(13) . ? C41A C42A 1.521(13) . ? C46A C47A 1.55(8) . ? C47A C48A 1.3900 . ? C47A C52A 1.3900 . ? C48A C49A 1.3900 . ? C49A C50A 1.3900 . ? C49A C57A 1.48(8) . ? C50A C51A 1.3900 . ? C51A C52A 1.3900 . ? C51A C53A 1.64(2) . ? C53A C54A 1.516(12) . ? C53A C55A 1.517(13) . ? C53A C56A 1.520(9) . ? C57A C58A 1.56(9) . ? C58A C59A 1.3900 . ? C58A C63A 1.3900 . ? C59A C60A 1.3900 . ? C60A C61A 1.3900 . ? C60A C68A 1.52(6) . ? C61A C62A 1.3900 . ? C62A C63A 1.3900 . ? C62A C64A 1.70(2) . ? C64A C67A 1.520(6) . ? C64A C65A 1.520(6) . ? C64A C66A 1.521(6) . ? C69A C70A 1.67(8) . ? C70A C71A 1.3900 . ? C70A C75A 1.3900 . ? C71A C72A 1.3900 . ? C72A C73A 1.3900 . ? C72A C80A 1.522(13) . ? C73A C74A 1.3900 . ? C74A C75A 1.3900 . ? C74A C76A 1.63(3) . ? C76A C78A 1.520(13) . ? C76A C77A 1.519(13) . ? C76A C79A 1.522(13) . ? C80A C81A 1.517(13) . ? C81A C82A 1.3900 . ? C81A C86A 1.3900 . ? C82A C83A 1.3900 . ? C83A C84A 1.3900 . ? C83A C91A 1.56(7) . ? C84A C85A 1.3900 . ? C85A C86A 1.3900 . ? C85A C87A 1.63(3) . ? C87A C90A 1.517(13) . ? C87A C89A 1.519(13) . ? C87A C88A 1.519(13) . ? U1B O14B 1.72(5) . ? U1B O13B 1.81(5) . ? U1B O1B 2.22(4) . ? U1B O2B 2.23(5) . ? U1B O23B 2.40(4) . ? U1B O24B 2.52(4) . ? U1B O21B 2.70(5) . ? U1B U4B 4.102(5) . ? U1B U2B 5.044(5) . ? U2B O16B 1.70(5) . ? U2B O15B 1.78(4) . ? U2B O5B 2.16(5) . ? U2B O4B 2.21(4) . ? U2B O21B 2.39(5) . ? U2B O26B 2.43(4) . ? U2B O25B 2.48(4) . ? U2B U3B 4.082(5) . ? U3B O17B 1.79(5) . ? U3B O18B 1.84(4) . ? U3B O7B 2.23(4) . ? U3B O8B 2.28(4) . ? U3B O26B 2.35(4) . ? U3B O22B 2.50(4) . ? U3B O25B 2.54(4) . ? U3B U4B 4.896(5) . ? U4B O20B 1.68(1) . ? U4B O19B 1.78(4) . ? U4B O11B 2.11(5) . ? U4B O10B 2.29(4) . ? U4B O22B 2.43(4) . ? U4B O24B 2.47(4) . ? U4B O23B 2.43(2) . ? O1B C1B 1.40(5) . ? O1B O1 2.62(4) . ? O2B C13B 1.45(5) . ? O2B O2 2.71(6) . ? O3B C22B 1.48(9) . ? O3B C23B 1.54(8) . ? O4B C25B 1.46(5) . ? O4B O2 2.57(4) . ? O5B C36B 1.61(5) . ? O5B N3 2.80(4) . ? O6B C46B 1.44(7) . ? O6B C45B 1.55(8) . ? O7B C48B 1.31(4) . ? O7B O4 3.13(4) . ? O8B C59B 1.35(5) . ? O8B O7 2.77(7) . ? O9B C69B 1.45(7) . ? O9B C68B 1.54(8) . ? O10B C71B 1.52(5) . ? O10B O7 2.53(7) . ? O11B C82B 1.48(5) . ? O12B C92B 1.57(9) . ? O12B C91B 1.65(10) . ? O14B N4 2.89(4) . ? C1B C6B 1.3900 . ? C1B C2B 1.3900 . ? C2B C3B 1.3900 . ? C2B C92B 1.44(9) . ? C3B C4B 1.3900 . ? C4B C5B 1.3900 . ? C4B C7B 1.53(7) . ? C5B C6B 1.3900 . ? C6B C11B 1.66(6) . ? C7B C9B 1.35(9) . ? C7B C10B 1.55(8) . ? C7B C8B 1.64(8) . ? C11B C12B 1.62(6) . ? C12B C13B 1.3900 . ? C12B C17B 1.3900 . ? C13B C14B 1.3900 . ? C14B C15B 1.3900 . ? C14B C22B 1.56(9) . ? C15B C16B 1.3900 . ? C16B C17B 1.3900 . ? C16B C18B 1.51(6) . ? C18B C21B 1.518(13) . ? C18B C19B 1.520(13) . ? C18B C20B 1.520(13) . ? C23B C24B 1.56(8) . ? C24B C25B 1.3900 . ? C24B C29B 1.3900 . ? C25B C26B 1.3900 . ? C26B C27B 1.3900 . ? C26B C34B 1.56(6) . ? C27B C28B 1.3900 . ? C28B C29B 1.3900 . ? C28B C30B 1.63(3) . ? C30B C31B 1.518(13) . ? C30B C33B 1.521(13) . ? C30B C32B 1.521(13) . ? C34B C35B 1.56(6) . ? C45B C37B 1.35(8) . ? C35B C36B 1.3900 . ? C35B C40B 1.3900 . ? C36B C37B 1.3900 . ? C37B C38B 1.3900 . ? C38B C39B 1.3900 . ? C39B C40B 1.3900 . ? C39B C41B 1.63(3) . ? C41B C43B 1.517(13) . ? C41B C44B 1.522(13) . ? C41B C42B 1.523(13) . ? C46B C47B 1.53(7) . ? C47B C48B 1.3900 . ? C47B C52B 1.3900 . ? C48B C49B 1.3900 . ? C49B C50B 1.3900 . ? C49B C57B 1.67(6) . ? C50B C51B 1.3900 . ? C51B C52B 1.3900 . ? C51B C53B 1.67(8) . ? C53B C54B 1.58(10) . ? C53B C55B 1.62(10) . ? C53B C56B 1.68(10) . ? C57B C58B 1.42(7) . ? C58B C59B 1.3900 . ? C58B C63B 1.3900 . ? C59B C60B 1.3900 . ? C60B C68B 1.37(8) . ? C60B C61B 1.3900 . ? C61B C62B 1.3900 . ? C62B C63B 1.3900 . ? C62B C64B 1.42(9) . ? C64B C65B 1.62(9) . ? C64B C66B 1.73(12) . ? C64B C67B 1.86(11) . ? C69B C70B 1.58(7) . ? C70B C71B 1.3900 . ? C70B C75B 1.3900 . ? C71B C72B 1.3900 . ? C72B C80B 1.37(8) . ? C72B C73B 1.3900 . ? C73B C74B 1.3900 . ? C74B C75B 1.3900 . ? C74B C76B 1.64(3) . ? C76B C77B 1.515(13) . ? C76B C78B 1.519(13) . ? C76B C79B 1.521(12) . ? C80B C81B 1.73(7) . ? C81B C82B 1.3900 . ? C81B C86B 1.3900 . ? C82B C83B 1.3900 . ? C83B C91B 1.37(10) . ? C83B C84B 1.3900 . ? C84B C85B 1.3900 . ? C85B C86B 1.3900 . ? C85B C87B 1.64(3) . ? C87B C88B 1.515(13) . ? C87B C89B 1.516(13) . ? C87B C90B 1.516(13) . ? N1 C5 1.4703 . ? N1 C3 1.5016 . ? N1 C1 1.5689 . ? C1 C2 1.6848 . ? C3 C4 1.5305 . ? C5 C6 1.4880 . ? N2 C7 1.476(19) . ? N2 C11 1.482(14) . ? N2 C9 1.483(12) . ? C7 C8 1.524(13) . ? C9 C10 1.529(14) . ? C11 C12 1.528(13) . ? N3 C17 1.66(7) . ? N3 C13 1.75(8) . ? N3 C15 1.76(8) . ? C13 C14 1.86(8) . ? C15 C16 1.67(10) . ? C17 C18 1.14(7) . ? N4 C23 1.39(7) . ? N4 C19 1.61(8) . ? N4 C21 1.73(8) . ? C19 C20 1.66(8) . ? C21 C22 1.69(9) . ? C23 C24 1.84(9) . ? N5 C25 1.35(14) . ? N5 C29 1.48(13) . ? N5 C27 1.59(10) . ? N5 O1 3.12(13) . ? C25 C26 1.42(16) . ? C27 C28 1.52(9) . ? C29 C30 1.07(13) . ? N6 C35 1.451(7) . ? N6 C31 1.451(6) . ? N6 C33 1.451(6) . ? N6 O2 2.83(8) . ? C31 C32 1.523(13) . ? C33 C34 1.523(13) . ? C35 C36 1.521(13) . ? N7 C37 1.450(6) . ? N7 C41 1.450(6) . ? N7 C39 1.451(6) . ? N7 O3 2.84(8) . ? C37 C38 1.518(13) . ? C39 C40 1.519(13) . ? C41 C42 1.521(13) . ? O1 O5 2.65(10) . ? O6 C43 1.555(13) . ? O7 C44 1.597(13) . ? 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 O14A U1A O13A 177.9(13) . . ? O14A U1A O23A 93.3(11) . . ? O13A U1A O23A 88.4(18) . . ? O14A U1A O2A 84.8(14) . . ? O13A U1A O2A 93.1(19) . . ? O23A U1A O2A 155.6(13) . . ? O14A U1A O1A 90.1(14) . . ? O13A U1A O1A 89.2(19) . . ? O23A U1A O1A 79.1(14) . . ? O2A U1A O1A 76.5(17) . . ? O14A U1A O21A 89.1(15) . . ? O13A U1A O21A 91(2) . . ? O23A U1A O21A 128.1(15) . . ? O2A U1A O21A 76.3(19) . . ? O1A U1A O21A 152.7(19) . . ? O14A U1A O24A 84.8(10) . . ? O13A U1A O24A 96.9(17) . . ? O23A U1A O24A 65.2(7) . . ? O2A U1A O24A 138.5(12) . . ? O1A U1A O24A 143.5(14) . . ? O21A U1A O24A 63.5(14) . . ? O14A U1A U4A 95.48(17) . . ? O13A U1A U4A 86.6(13) . . ? O23A U1A U4A 30.1(6) . . ? O2A U1A U4A 174.4(11) . . ? O1A U1A U4A 109.1(13) . . ? O21A U1A U4A 98.1(14) . . ? O24A U1A U4A 36.2(3) . . ? O14A U1A U2A 92.00(15) . . ? O13A U1A U2A 88.1(13) . . ? O23A U1A U2A 120.7(6) . . ? O2A U1A U2A 83.7(11) . . ? O1A U1A U2A 159.8(13) . . ? O21A U1A U2A 7.7(14) . . ? O24A U1A U2A 56.6(5) . . ? U4A U1A U2A 90.67(10) . . ? O15A U2A O16A 177(2) . . ? O15A U2A O5A 93(2) . . ? O16A U2A O5A 88(2) . . ? O15A U2A O26A 89(2) . . ? O16A U2A O26A 90(2) . . ? O5A U2A O26A 69.6(18) . . ? O15A U2A O4A 90.2(17) . . ? O16A U2A O4A 92.2(17) . . ? O5A U2A O4A 92.3(15) . . ? O26A U2A O4A 161.8(13) . . ? O15A U2A O21A 89(2) . . ? O16A U2A O21A 90(2) . . ? O5A U2A O21A 164.8(19) . . ? O26A U2A O21A 125.5(19) . . ? O4A U2A O21A 72.7(15) . . ? O15A U2A O25A 94(2) . . ? O16A U2A O25A 83.5(19) . . ? O5A U2A O25A 126.7(14) . . ? O26A U2A O25A 57.8(13) . . ? O4A U2A O25A 140.4(7) . . ? O21A U2A O25A 68.0(16) . . ? O15A U2A U3A 80.3(16) . . ? O16A U2A U3A 97.1(15) . . ? O5A U2A U3A 95.5(14) . . ? O26A U2A U3A 26.7(12) . . ? O4A U2A U3A 168.0(7) . . ? O21A U2A U3A 99.7(14) . . ? O25A U2A U3A 34.6(5) . . ? O15A U2A U1A 85.2(15) . . ? O16A U2A U1A 93.5(15) . . ? O5A U2A U1A 171.9(12) . . ? O26A U2A U1A 118.2(12) . . ? O4A U2A U1A 79.8(5) . . ? O21A U2A U1A 8.0(15) . . ? O25A U2A U1A 61.3(7) . . ? U3A U2A U1A 92.03(11) . . ? O17A U3A O18A 172(2) . . ? O17A U3A O7A 99.3(19) . . ? O18A U3A O7A 85.0(19) . . ? O17A U3A O26A 87(2) . . ? O18A U3A O26A 88(2) . . ? O7A U3A O26A 78.2(17) . . ? O17A U3A O8A 95.1(17) . . ? O18A U3A O8A 91.7(17) . . ? O7A U3A O8A 80.3(15) . . ? O26A U3A O8A 158.5(15) . . ? O17A U3A O25A 86.0(19) . . ? O18A U3A O25A 86.7(18) . . ? O7A U3A O25A 137.3(16) . . ? O26A U3A O25A 59.6(15) . . ? O8A U3A O25A 141.8(13) . . ? O17A U3A O22A 86(2) . . ? O18A U3A O22A 92(2) . . ? O7A U3A O22A 161.7(16) . . ? O26A U3A O22A 119.8(16) . . ? O8A U3A O22A 81.7(13) . . ? O25A U3A O22A 60.3(9) . . ? O17A U3A U2A 75.0(14) . . ? O18A U3A U2A 98.0(14) . . ? O7A U3A U2A 105.2(12) . . ? O26A U3A U2A 28.2(11) . . ? O8A U3A U2A 169.2(11) . . ? O25A U3A U2A 35.1(11) . . ? O22A U3A U2A 93.0(11) . . ? O17A U3A U4A 77.3(14) . . ? O18A U3A U4A 100.2(14) . . ? O7A U3A U4A 164.3(12) . . ? O26A U3A U4A 116.6(11) . . ? O8A U3A U4A 84.7(8) . . ? O25A U3A U4A 58.3(11) . . ? O22A U3A U4A 8.5(14) . . ? U2A U3A U4A 88.85(11) . . ? O20A U4A O19A 178.1(17) . . ? O20A U4A O11A 89(2) . . ? O19A U4A O11A 89.7(18) . . ? O20A U4A O10A 97(2) . . ? O19A U4A O10A 83.6(17) . . ? O11A U4A O10A 86.3(16) . . ? O20A U4A O23A 88.9(19) . . ? O19A U4A O23A 90.0(16) . . ? O11A U4A O23A 79.5(16) . . ? O10A U4A O23A 164.4(15) . . ? O20A U4A O22A 88(2) . . ? O19A U4A O22A 94.2(19) . . ? O11A U4A O22A 159.0(15) . . ? O10A U4A O22A 73.7(15) . . ? O23A U4A O22A 121.1(14) . . ? O20A U4A O24A 85.1(19) . . ? O19A U4A O24A 95.8(16) . . ? O11A U4A O24A 143.4(13) . . ? O10A U4A O24A 130.2(11) . . ? O23A U4A O24A 64.5(11) . . ? O22A U4A O24A 56.7(11) . . ? O20A U4A U1A 92.8(16) . . ? O19A U4A U1A 87.0(12) . . ? O11A U4A U1A 108.6(11) . . ? O10A U4A U1A 162.4(11) . . ? O23A U4A U1A 29.3(10) . . ? O22A U4A U1A 92.3(10) . . ? O24A U4A U1A 36.2(3) . . ? O20A U4A U3A 95.1(15) . . ? O19A U4A U3A 86.7(11) . . ? O11A U4A U3A 162.4(12) . . ? O10A U4A U3A 76.2(10) . . ? O23A U4A U3A 117.7(10) . . ? O22A U4A U3A 8.2(14) . . ? O24A U4A U3A 54.1(5) . . ? U1A U4A U3A 88.41(11) . . ? C1A O1A U1A 155(4) . . ? C13A O2A U1A 136(3) . . ? C13A O2A O6 113(3) . . ? U1A O2A O6 110.1(18) . . ? C22A O3A C23A 108.2(10) . . ? C25A O4A U2A 122(3) . . ? C25A O4A O6 116(3) . . ? U2A O4A O6 121.3(4) . . ? C36A O5A U2A 140(2) . . ? C45A O6A C46A 103(3) . . ? C48A O7A U3A 169(3) . . ? C59A O8A U3A 150(3) . . ? C59A O8A O3 100(2) . . ? U3A O8A O3 110.2(9) . . ? C68A O9A C69A 106(4) . . ? C71A O10A U4A 119(2) . . ? C71A O10A O3 119(2) . . ? U4A O10A O3 121.7(19) . . ? C82A O11A U4A 159(3) . . ? C92A O12A C91A 114(3) . . ? U1A O14A N1 140.03(13) . . ? U3A O17A N2 163(2) . . ? U2A O21A U1A 164(3) . . ? U4A O22A U3A 163(3) . . ? U1A O23A U4A 120.6(16) . . ? U4A O24A U1A 107.6(5) . . ? U3A O25A U2A 110.3(15) . . ? U3A O26A U2A 125(2) . . ? O1A C1A C2A 123(2) . . ? O1A C1A C6A 116(2) . . ? C2A C1A C6A 120.0 . . ? C1A C2A C3A 120.0 . . ? C1A C2A C92A 119(5) . . ? C3A C2A C92A 121(5) . . ? C2A C3A C4A 120.0 . . ? C5A C4A C3A 120.0 . . ? C5A C4A C7A 117(4) . . ? C3A C4A C7A 123(4) . . ? C6A C5A C4A 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A C11A 117(5) . . ? C1A C6A C11A 123(5) . . ? C8A C7A C9A 110.8(13) . . ? C8A C7A C10A 110.3(12) . . ? C9A C7A C10A 110.2(13) . . ? C8A C7A C4A 108.7(12) . . ? C9A C7A C4A 108.5(12) . . ? C10A C7A C4A 108.3(12) . . ? C6A C11A C12A 123(6) . . ? C13A C12A C17A 120.00(6) . . ? C13A C12A C11A 126(4) . . ? C17A C12A C11A 114(4) . . ? O2A C13A C14A 120(5) . . ? O2A C13A C12A 120(5) . . ? C14A C13A C12A 120.0 . . ? C13A C14A C15A 120.0 . . ? C13A C14A C22A 123(6) . . ? C15A C14A C22A 115(6) . . ? C16A C15A C14A 120.00(6) . . ? C17A C16A C15A 120.0 . . ? C17A C16A C18A 127(3) . . ? C15A C16A C18A 113(3) . . ? C16A C17A C12A 120.0 . . ? C21A C18A C20A 113.5(10) . . ? C21A C18A C19A 113.5(10) . . ? C20A C18A C19A 113.5(10) . . ? C21A C18A C16A 105.1(9) . . ? C20A C18A C16A 105.1(9) . . ? C19A C18A C16A 105.1(9) . . ? O3A C22A C14A 117(5) . . ? O3A C23A C24A 105(4) . . ? C25A C24A C29A 120.0 . . ? C25A C24A C23A 128(5) . . ? C29A C24A C23A 112(5) . . ? O4A C25A C24A 112.7(8) . . ? O4A C25A C26A 126.2(9) . . ? C24A C25A C26A 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A C34A 124(4) . . ? C25A C26A C34A 115(4) . . ? C26A C27A C28A 120.0 . . ? C29A C28A C27A 120.0 . . ? C29A C28A C30A 135(3) . . ? C27A C28A C30A 105(3) . . ? C28A C29A C24A 120.00(6) . . ? C33A C30A C31A 110.3(11) . . ? C33A C30A C32A 110.4(11) . . ? C31A C30A C32A 110.8(11) . . ? C33A C30A C28A 108.8(11) . . ? C31A C30A C28A 108.3(11) . . ? C32A C30A C28A 108.2(11) . . ? C26A C34A C35A 111(6) . . ? C36A C35A C40A 120.0 . . ? C36A C35A C34A 123(7) . . ? C40A C35A C34A 116(7) . . ? C35A C36A C37A 120.0 . . ? C35A C36A O5A 123(7) . . ? C37A C36A O5A 116(7) . . ? C38A C37A C36A 120.0 . . ? C38A C37A C45A 126(7) . . ? C36A C37A C45A 113(7) . . ? C39A C38A C37A 120.0 . . ? C38A C39A C40A 120.0 . . ? C38A C39A C41A 126(5) . . ? C40A C39A C41A 114(5) . . ? C39A C40A C35A 120.0 . . ? C44A C41A C43A 110.7(13) . . ? C44A C41A C42A 110.6(13) . . ? C43A C41A C42A 110.6(13) . . ? C44A C41A C39A 108.5(13) . . ? C43A C41A C39A 108.1(13) . . ? C42A C41A C39A 108.2(13) . . ? O6A C45A C37A 93(6) . . ? O6A C46A C47A 110(5) . . ? C48A C47A C52A 120.0 . . ? C48A C47A C46A 112(5) . . ? C52A C47A C46A 128(5) . . ? O7A C48A C49A 120(6) . . ? O7A C48A C47A 120(6) . . ? C49A C48A C47A 120.0 . . ? C48A C49A C50A 120.0 . . ? C48A C49A C57A 124(6) . . ? C50A C49A C57A 115(5) . . ? C51A C50A C49A 120.0 . . ? C50A C51A C52A 120.0 . . ? C50A C51A C53A 122(4) . . ? C52A C51A C53A 117(4) . . ? C51A C52A C47A 120.0 . . ? C54A C53A C55A 111.3(13) . . ? C54A C53A C56A 110.9(12) . . ? C55A C53A C56A 110.9(12) . . ? C54A C53A C51A 107.9(12) . . ? C55A C53A C51A 108.0(12) . . ? C56A C53A C51A 107.7(13) . . ? C49A C57A C58A 128(7) . . ? C59A C58A C63A 120.0 . . ? C59A C58A C57A 119(4) . . ? C63A C58A C57A 117(4) . . ? O8A C59A C60A 112.5(9) . . ? O8A C59A C58A 126.3(10) . . ? C60A C59A C58A 120.0 . . ? C59A C60A C61A 120.0 . . ? C59A C60A C68A 126(3) . . ? C61A C60A C68A 114(3) . . ? C62A C61A C60A 120.0 . . ? C63A C62A C61A 120.0 . . ? C63A C62A C64A 112(2) . . ? C61A C62A C64A 126(2) . . ? C62A C63A C58A 120.0 . . ? C67A C64A C65A 113.9(10) . . ? C67A C64A C66A 114.0(10) . . ? C65A C64A C66A 113.9(10) . . ? C67A C64A C62A 104.6(9) . . ? C65A C64A C62A 104.5(9) . . ? C66A C64A C62A 104.5(9) . . ? O9A C68A C60A 103(5) . . ? O9A C69A C70A 111(6) . . ? C71A C70A C75A 120.0 . . ? C71A C70A C69A 115(5) . . ? C75A C70A C69A 125(5) . . ? C70A C71A C72A 120.0 . . ? C70A C71A O10A 124(5) . . ? C72A C71A O10A 116(5) . . ? C73A C72A C71A 120.0 . . ? C73A C72A C80A 113(6) . . ? C71A C72A C80A 126(6) . . ? C72A C73A C74A 120.0 . . ? C75A C74A C73A 120.0 . . ? C75A C74A C76A 116(4) . . ? C73A C74A C76A 124(4) . . ? C74A C75A C70A 120.0 . . ? C78A C76A C77A 110.9(13) . . ? C78A C76A C79A 110.5(13) . . ? C77A C76A C79A 110.6(13) . . ? C78A C76A C74A 108.4(13) . . ? C77A C76A C74A 108.4(13) . . ? C79A C76A C74A 108.1(12) . . ? C81A C80A C72A 115(4) . . ? C82A C81A C86A 120.0 . . ? C82A C81A C80A 118.6(13) . . ? C86A C81A C80A 121.3(14) . . ? O11A C82A C83A 114(5) . . ? O11A C82A C81A 125(5) . . ? C83A C82A C81A 120.0 . . ? C84A C83A C82A 120.00(7) . . ? C84A C83A C91A 117(4) . . ? C82A C83A C91A 123(4) . . ? C85A C84A C83A 120.0 . . ? C84A C85A C86A 120.0 . . ? C84A C85A C87A 119(3) . . ? C86A C85A C87A 121(3) . . ? C85A C86A C81A 120.00(6) . . ? C90A C87A C89A 110.8(13) . . ? C90A C87A C88A 111.1(13) . . ? C89A C87A C88A 110.9(13) . . ? C90A C87A C85A 108.1(13) . . ? C89A C87A C85A 108.0(13) . . ? C88A C87A C85A 107.8(13) . . ? O12A C91A C83A 114(5) . . ? O12A C92A C2A 118(6) . . ? O14B U1B O13B 175.8(19) . . ? O14B U1B O1B 89.5(16) . . ? O13B U1B O1B 91.0(18) . . ? O14B U1B O2B 93.7(17) . . ? O13B U1B O2B 90.4(19) . . ? O1B U1B O2B 77.8(14) . . ? O14B U1B O23B 92.4(16) . . ? O13B U1B O23B 83.6(17) . . ? O1B U1B O23B 82.6(11) . . ? O2B U1B O23B 159.4(12) . . ? O14B U1B O24B 89.4(16) . . ? O13B U1B O24B 88.0(16) . . ? O1B U1B O24B 147.1(13) . . ? O2B U1B O24B 135.1(14) . . ? O23B U1B O24B 64.5(11) . . ? O14B U1B O21B 92.6(16) . . ? O13B U1B O21B 88.7(17) . . ? O1B U1B O21B 154.4(13) . . ? O2B U1B O21B 76.7(14) . . ? O23B U1B O21B 122.7(11) . . ? O24B U1B O21B 58.5(13) . . ? O14B U1B U4B 82.8(12) . . ? O13B U1B U4B 93.2(14) . . ? O1B U1B U4B 113.2(10) . . ? O2B U1B U4B 168.4(10) . . ? O23B U1B U4B 32.2(5) . . ? O24B U1B U4B 34.2(9) . . ? O21B U1B U4B 92.4(9) . . ? O14B U1B U2B 86.0(13) . . ? O13B U1B U2B 95.1(14) . . ? O1B U1B U2B 157.1(10) . . ? O2B U1B U2B 80.2(10) . . ? O23B U1B U2B 119.9(5) . . ? O24B U1B U2B 55.4(9) . . ? O21B U1B U2B 7.3(10) . . ? U4B U1B U2B 88.51(9) . . ? O16B U2B O15B 173.9(16) . . ? O16B U2B O5B 84.2(16) . . ? O15B U2B O5B 100.4(15) . . ? O16B U2B O4B 87.4(18) . . ? O15B U2B O4B 89.3(17) . . ? O5B U2B O4B 81.6(15) . . ? O16B U2B O21B 89.1(17) . . ? O15B U2B O21B 85.0(16) . . ? O5B U2B O21B 153.6(15) . . ? O4B U2B O21B 72.6(14) . . ? O16B U2B O26B 95.3(16) . . ? O15B U2B O26B 89.4(15) . . ? O5B U2B O26B 81.8(14) . . ? O4B U2B O26B 162.8(13) . . ? O21B U2B O26B 124.3(13) . . ? O16B U2B O25B 94.0(16) . . ? O15B U2B O25B 84.3(14) . . ? O5B U2B O25B 147.7(13) . . ? O4B U2B O25B 130.6(14) . . ? O21B U2B O25B 58.1(13) . . ? O26B U2B O25B 66.2(12) . . ? O16B U2B U3B 90.2(13) . . ? O15B U2B U3B 91.8(12) . . ? O5B U2B U3B 111.5(10) . . ? O4B U2B U3B 166.4(10) . . ? O21B U2B U3B 93.9(10) . . ? O26B U2B U3B 30.8(9) . . ? O25B U2B U3B 36.2(8) . . ? O16B U2B U1B 82.2(12) . . ? O15B U2B U1B 92.1(11) . . ? O5B U2B U1B 155.0(10) . . ? O4B U2B U1B 77.0(10) . . ? O21B U2B U1B 8.3(11) . . ? O26B U2B U1B 120.2(9) . . ? O25B U2B U1B 54.5(8) . . ? U3B U2B U1B 89.40(9) . . ? O17B U3B O18B 178.7(18) . . ? O17B U3B O7B 91.0(17) . . ? O18B U3B O7B 90.3(15) . . ? O17B U3B O8B 87.8(17) . . ? O18B U3B O8B 93.0(16) . . ? O7B U3B O8B 77.1(13) . . ? O17B U3B O26B 91.3(17) . . ? O18B U3B O26B 88.4(16) . . ? O7B U3B O26B 79.3(13) . . ? O8B U3B O26B 156.3(13) . . ? O17B U3B O22B 92.7(16) . . ? O18B U3B O22B 86.5(16) . . ? O7B U3B O22B 152.1(13) . . ? O8B U3B O22B 75.4(13) . . ? O26B U3B O22B 128.2(12) . . ? O17B U3B O25B 85.1(15) . . ? O18B U3B O25B 93.5(15) . . ? O7B U3B O25B 145.1(13) . . ? O8B U3B O25B 137.1(12) . . ? O26B U3B O25B 66.2(12) . . ? O22B U3B O25B 62.7(12) . . ? O17B U3B U2B 93.5(13) . . ? O18B U3B U2B 85.6(12) . . ? O7B U3B U2B 111.0(9) . . ? O8B U3B U2B 171.7(9) . . ? O26B U3B U2B 31.9(8) . . ? O22B U3B U2B 96.3(8) . . ? O25B U3B U2B 35.1(8) . . ? O17B U3B U4B 89.6(13) . . ? O18B U3B U4B 89.5(12) . . ? O7B U3B U4B 158.1(9) . . ? O8B U3B U4B 81.0(9) . . ? O26B U3B U4B 122.6(8) . . ? O22B U3B U4B 6.5(9) . . ? O25B U3B U4B 56.7(8) . . ? U2B U3B U4B 90.80(9) . . ? O20B U4B O19B 179.9(16) . . ? O20B U4B O11B 88.5(16) . . ? O19B U4B O11B 91.5(16) . . ? O20B U4B O10B 92.3(16) . . ? O19B U4B O10B 87.6(15) . . ? O11B U4B O10B 81.7(15) . . ? O20B U4B O22B 85.3(15) . . ? O19B U4B O22B 94.7(15) . . ? O11B U4B O22B 156.6(14) . . ? O10B U4B O22B 76.1(13) . . ? O20B U4B O24B 94.0(15) . . ? O19B U4B O24B 86.1(15) . . ? O11B U4B O24B 139.3(14) . . ? O10B U4B O24B 138.6(14) . . ? O22B U4B O24B 63.7(13) . . ? O20B U4B O23B 93.1(15) . . ? O19B U4B O23B 87.0(15) . . ? O11B U4B O23B 74.5(15) . . ? O10B U4B O23B 155.4(14) . . ? O22B U4B O23B 128.3(13) . . ? O24B U4B O23B 64.9(13) . . ? O20B U4B U1B 85.9(12) . . ? O19B U4B U1B 94.2(11) . . ? O11B U4B U1B 105.1(11) . . ? O10B U4B U1B 172.9(10) . . ? O22B U4B U1B 96.9(9) . . ? O24B U4B U1B 35.0(9) . . ? O23B U4B U1B 31.7(10) . . ? O20B U4B U3B 88.5(11) . . ? O19B U4B U3B 91.4(11) . . ? O11B U4B U3B 163.1(11) . . ? O10B U4B U3B 81.8(10) . . ? O22B U4B U3B 6.7(9) . . ? O24B U4B U3B 57.5(9) . . ? O23B U4B U3B 122.3(10) . . ? U1B U4B U3B 91.25(10) . . ? C1B O1B U1B 141(2) . . ? C1B O1B O1 113.1(19) . . ? U1B O1B O1 105.6(14) . . ? C13B O2B U1B 134(3) . . ? C13B O2B O2 108(2) . . ? U1B O2B O2 118.3(17) . . ? C22B O3B C23B 107(3) . . ? C25B O4B U2B 132(2) . . ? C25B O4B O2 102(2) . . ? U2B O4B O2 125.1(18) . . ? C36B O5B U2B 131(2) . . ? C36B O5B N3 113.1(19) . . ? U2B O5B N3 113.4(16) . . ? C46B O6B C45B 108(2) . . ? C48B O7B U3B 150(3) . . ? C48B O7B O4 106.4(19) . . ? U3B O7B O4 103.8(13) . . ? C59B O8B U3B 137(3) . . ? C59B O8B O7 108(2) . . ? U3B O8B O7 115.4(14) . . ? C69B O9B C68B 112(3) . . ? C71B O10B U4B 123(2) . . ? C71B O10B O7 119(2) . . ? U4B O10B O7 116.7(17) . . ? C82B O11B U4B 166(3) . . ? C92B O12B C91B 108.9(18) . . ? U1B O14B N4 147.8(19) . . ? U3B O17B O5 47.6(11) . . ? U2B O21B U1B 164(2) . . ? U4B O22B U3B 166.7(18) . . ? U1B O23B U4B 116.1(14) . . ? U4B O24B U1B 110.8(15) . . ? U2B O25B U3B 108.7(13) . . ? U3B O26B U2B 117.3(15) . . ? C6B C1B C2B 120.0 . . ? C6B C1B O1B 114.1(15) . . ? C2B C1B O1B 124.9(16) . . ? C3B C2B C1B 120.0 . . ? C3B C2B C92B 122(5) . . ? C1B C2B C92B 117(5) . . ? C4B C3B C2B 120.0 . . ? C3B C4B C5B 120.0 . . ? C3B C4B C7B 118(4) . . ? C5B C4B C7B 122(4) . . ? C6B C5B C4B 120.00(6) . . ? C5B C6B C1B 120.0 . . ? C5B C6B C11B 114(4) . . ? C1B C6B C11B 126(4) . . ? C9B C7B C10B 109(7) . . ? C9B C7B C4B 125(7) . . ? C10B C7B C4B 112(5) . . ? C9B C7B C8B 96(6) . . ? C10B C7B C8B 102(5) . . ? C4B C7B C8B 110(5) . . ? C12B C11B C6B 106(4) . . ? C13B C12B C17B 120.0 . . ? C13B C12B C11B 122(4) . . ? C17B C12B C11B 118(4) . . ? C14B C13B C12B 120.0 . . ? C14B C13B O2B 122(4) . . ? C12B C13B O2B 118(4) . . ? C13B C14B C15B 120.00(6) . . ? C13B C14B C22B 115(5) . . ? C15B C14B C22B 125(5) . . ? C16B C15B C14B 120.0 . . ? C17B C16B C15B 120.0 . . ? C17B C16B C18B 122(5) . . ? C15B C16B C18B 117(5) . . ? C16B C17B C12B 120.00(6) . . ? C21B C18B C19B 110.8(13) . . ? C21B C18B C20B 110.7(13) . . ? C19B C18B C20B 110.7(13) . . ? C21B C18B C16B 112(6) . . ? C19B C18B C16B 117(5) . . ? C20B C18B C16B 95(6) . . ? O3B C22B C14B 110(6) . . ? C24B C23B O3B 97(5) . . ? C25B C24B C29B 120.0 . . ? C25B C24B C23B 123(4) . . ? C29B C24B C23B 114(4) . . ? C26B C25B C24B 120.0 . . ? C26B C25B O4B 122(4) . . ? C24B C25B O4B 118(4) . . ? C25B C26B C27B 120.0 . . ? C25B C26B C34B 121(4) . . ? C27B C26B C34B 119(4) . . ? C28B C27B C26B 120.0 . . ? C29B C28B C27B 120.0 . . ? C29B C28B C30B 124(3) . . ? C27B C28B C30B 115(3) . . ? C28B C29B C24B 120.0 . . ? C31B C30B C33B 110.7(13) . . ? C31B C30B C32B 110.7(13) . . ? C33B C30B C32B 110.5(13) . . ? C31B C30B C28B 108.2(13) . . ? C33B C30B C28B 108.2(13) . . ? C32B C30B C28B 108.3(13) . . ? C35B C34B C26B 112(4) . . ? C37B C45B O6B 108(6) . . ? C36B C35B C40B 120.0 . . ? C36B C35B C34B 131(4) . . ? C40B C35B C34B 109(4) . . ? C35B C36B C37B 120.0 . . ? C35B C36B O5B 109(4) . . ? C37B C36B O5B 130(4) . . ? C45B C37B C36B 124(6) . . ? C45B C37B C38B 116(6) . . ? C36B C37B C38B 120.0 . . ? C39B C38B C37B 120.0 . . ? C40B C39B C38B 120.0 . . ? C40B C39B C41B 128(3) . . ? C38B C39B C41B 109(3) . . ? C39B C40B C35B 120.0 . . ? C43B C41B C44B 110.7(13) . . ? C43B C41B C42B 110.5(13) . . ? C44B C41B C42B 110.8(13) . . ? C43B C41B C39B 108.6(13) . . ? C44B C41B C39B 108.0(13) . . ? C42B C41B C39B 108.1(13) . . ? O6B C46B C47B 111(5) . . ? C48B C47B C52B 120.0 . . ? C48B C47B C46B 122(4) . . ? C52B C47B C46B 118(4) . . ? O7B C48B C49B 116(4) . . ? O7B C48B C47B 124(4) . . ? C49B C48B C47B 120.0 . . ? C48B C49B C50B 120.0 . . ? C48B C49B C57B 117(4) . . ? C50B C49B C57B 123(4) . . ? C49B C50B C51B 120.0 . . ? C50B C51B C52B 120.0 . . ? C50B C51B C53B 125(4) . . ? C52B C51B C53B 115(4) . . ? C51B C52B C47B 120.0 . . ? C54B C53B C55B 107(7) . . ? C54B C53B C56B 127(7) . . ? C55B C53B C56B 112(7) . . ? C54B C53B C51B 108(6) . . ? C55B C53B C51B 104(6) . . ? C56B C53B C51B 96(5) . . ? C58B C57B C49B 114(5) . . ? C59B C58B C63B 120.0 . . ? C59B C58B C57B 121(5) . . ? C63B C58B C57B 118(5) . . ? O8B C59B C60B 128(5) . . ? O8B C59B C58B 112(5) . . ? C60B C59B C58B 120.0 . . ? C68B C60B C59B 110(6) . . ? C68B C60B C61B 127(6) . . ? C59B C60B C61B 120.0 . . ? C62B C61B C60B 120.0 . . ? C63B C62B C61B 120.0 . . ? C63B C62B C64B 123(6) . . ? C61B C62B C64B 117(6) . . ? C62B C63B C58B 120.0 . . ? C62B C64B C65B 116(7) . . ? C62B C64B C66B 112(7) . . ? C65B C64B C66B 96(6) . . ? C62B C64B C67B 109(6) . . ? C65B C64B C67B 109(6) . . ? C66B C64B C67B 115(7) . . ? C60B C68B O9B 105(6) . . ? O9B C69B C70B 108(5) . . ? C71B C70B C75B 120.0 . . ? C71B C70B C69B 112(5) . . ? C75B C70B C69B 128(5) . . ? C70B C71B C72B 120.0 . . ? C70B C71B O10B 128(4) . . ? C72B C71B O10B 111(4) . . ? C80B C72B C73B 107(5) . . ? C80B C72B C71B 133(5) . . ? C73B C72B C71B 120.00(6) . . ? C72B C73B C74B 120.0 . . ? C73B C74B C75B 120.0 . . ? C73B C74B C76B 122(3) . . ? C75B C74B C76B 118(3) . . ? C74B C75B C70B 120.0 . . ? C77B C76B C78B 110.9(13) . . ? C77B C76B C79B 111.0(13) . . ? C78B C76B C79B 110.7(13) . . ? C77B C76B C74B 108.1(13) . . ? C78B C76B C74B 108.2(13) . . ? C79B C76B C74B 107.8(13) . . ? C72B C80B C81B 113(5) . . ? C82B C81B C86B 120.0 . . ? C82B C81B C80B 122(3) . . ? C86B C81B C80B 117(3) . . ? C83B C82B C81B 120.0 . . ? C83B C82B O11B 122(3) . . ? C81B C82B O11B 118(3) . . ? C91B C83B C84B 128(5) . . ? C91B C83B C82B 111(5) . . ? C84B C83B C82B 120.0 . . ? C85B C84B C83B 120.0 . . ? C84B C85B C86B 120.0 . . ? C84B C85B C87B 115(3) . . ? C86B C85B C87B 125(3) . . ? C85B C86B C81B 120.0 . . ? C88B C87B C89B 111.1(13) . . ? C88B C87B C90B 111.4(13) . . ? C89B C87B C90B 111.2(13) . . ? C88B C87B C85B 107.5(13) . . ? C89B C87B C85B 107.8(13) . . ? C90B C87B C85B 107.7(13) . . ? C83B C91B O12B 108(7) . . ? C2B C92B O12B 102(6) . . ? C5 N1 C3 89.3 . . ? C5 N1 C1 154.0 . . ? C3 N1 C1 107.4 . . ? C5 N1 O14A 68.5 . . ? C3 N1 O14A 130.4 . . ? C1 N1 O14A 111.1 . . ? N1 C1 C2 119.6 . . ? N1 C3 C4 127.1 . . ? N1 C5 C6 139.1 . . ? C7 N2 C11 123.1(14) . . ? C7 N2 C9 118.6(13) . . ? C11 N2 C9 117.7(11) . . ? C7 N2 O17A 93.5(8) . . ? C11 N2 O17A 70.3(8) . . ? C9 N2 O17A 99.0(8) . . ? N2 C7 C8 104(8) . . ? N2 C9 C10 128.0(17) . . ? N2 C11 C12 128.6(19) . . ? C17 N3 C13 107(4) . . ? C17 N3 C15 103(4) . . ? C13 N3 C15 105(4) . . ? C17 N3 O5B 114.5(8) . . ? C13 N3 O5B 132.4(9) . . ? C15 N3 O5B 88.9(8) . . ? N3 C13 C14 89(4) . . ? C16 C15 N3 109(6) . . ? C18 C17 N3 117(6) . . ? C23 N4 C19 92(5) . . ? C23 N4 C21 103(5) . . ? C19 N4 C21 102(5) . . ? C23 N4 O14B 113.6(7) . . ? C19 N4 O14B 124.3(8) . . ? C21 N4 O14B 117.6(8) . . ? N4 C19 C20 98(5) . . ? C22 C21 N4 124(6) . . ? N4 C23 C24 96(5) . . ? C25 N5 C29 107(10) . . ? C25 N5 C27 116(10) . . ? C29 N5 C27 110(9) . . ? C25 N5 O1 78(10) . . ? C29 N5 O1 141(8) . . ? C27 N5 O1 101(6) . . ? N5 C25 C26 149(10) . . ? C28 C27 N5 99(7) . . ? C30 C29 N5 125(10) . . ? C35 N6 C31 121(8) . . ? C35 N6 C33 120(9) . . ? C31 N6 C33 100(7) . . ? C35 N6 O2 99(6) . . ? C31 N6 O2 102(5) . . ? C33 N6 O2 114(6) . . ? N6 C31 C32 117(7) . . ? N6 C33 C34 119(9) . . ? N6 C35 C36 116(9) . . ? C37 N7 C41 125(9) . . ? C37 N7 C39 101(8) . . ? C41 N7 C39 121(8) . . ? C37 N7 O3 94(6) . . ? C41 N7 O3 112(5) . . ? C39 N7 O3 98(5) . . ? N7 C37 C38 134(10) . . ? N7 C39 C40 107(8) . . ? N7 C41 C42 112(7) . . ? O1B O1 O5 139.4(8) . . ? O1B O1 N5 132.3(8) . . ? O5 O1 N5 87(3) . . ? O4B O2 O2B 104.3(13) . . ? O4B O2 N6 114.6(9) . . ? O2B O2 N6 110.9(9) . . ? O10A O3 O8A 111.8(12) . . ? O10A O3 N7 114.8(11) . . ? O8A O3 N7 103.2(3) . . ? O1 O5 O17B 72.9(2) . . ? C43 O6 O4A 116.5(3) . . ? C43 O6 O2A 110.3(10) . . ? O4A O6 O2A 98.3(11) . . ? C44 O7 O10B 119.6(9) . . ? C44 O7 O8B 101.3(8) . . ? O10B O7 O8B 105.2(12) . . ? #===END