# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Thuery, Pierre' 'Masci, B.' 'Nierlich, M.' _publ_contact_author 'Dr Pierre Thuery' _publ_contact_address ; SCM CEA / Saclay Batiment 125 Gif-sur-Yvette 91191 FRANCE ; _publ_contact_author_phone '33 01 69 08 63 29' _publ_contact_author_fax '33 1 69 08 66 40' _publ_contact_author_email thuery@drecam.cea.fr _publ_requested_journal 'New J. Chem.' _publ_section_title ; Supramolecular assemblies from uranyl ion complexes of hexahomotrioxacalix[3]arenes and protonated [2.2.2]cryptand ; data_3 _database_code_CSD 181042 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H82 N2 O14 U' _chemical_formula_weight 1221.25 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3837(6) _cell_length_b 20.2772(6) _cell_length_c 21.5187(6) _cell_angle_alpha 66.410(2) _cell_angle_beta 79.842(2) _cell_angle_gamma 79.466(2) _cell_volume 5617.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 39075 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent intense orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method ? _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 2.953 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.466 _exptl_absorpt_correction_T_max 0.478 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _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 39075 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.68 _reflns_number_total 19770 _reflns_number_gt 14480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _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 subsequent Fourier-difference synthesis. Two tert-butyl groups (one in each of the two independent molecules A and B) were found disordered and were modelled with two positions affected with occupancies constrained to sum to unity and restraints on displacement parameters. The presence of a void of 81 A^3^ may indicate the presence of disordered, unresolved solvent molecule. All non-hydrogen atoms were refined with anisotropic displacement parameters, except the disordered ones. The hydrogen atoms bound to N atoms have been found on the Fourier-difference map and introduced as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. All other hydrogen atoms (except those in the disordered parts) were introduced at calculated positions as riding atoms with an isotropic displacement parameter 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^)+(0.0230P)^2^+4.4785P] 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 19770 _refine_ls_number_parameters 1289 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.947 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.109 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 -0.005979(14) 0.794424(11) 0.800614(10) 0.02093(6) Uani 1 1 d . . . O1A O 0.0262(3) 0.67881(19) 0.81289(19) 0.0265(9) Uani 1 1 d . . . O2A O 0.1816(3) 0.76226(18) 0.74189(18) 0.0271(9) Uani 1 1 d . . . O3A O 0.0494(3) 0.88911(19) 0.71680(18) 0.0267(9) Uani 1 1 d . . . O4A O 0.0013(3) 0.9459(2) 0.8343(2) 0.0489(13) Uani 1 1 d . . . O5A O -0.1239(3) 0.8240(2) 0.87130(18) 0.0314(9) Uani 1 1 d . . . O6A O -0.0278(3) 0.6741(2) 0.9533(2) 0.0459(12) Uani 1 1 d . . . O7A O -0.0925(3) 0.8013(2) 0.74699(18) 0.0278(9) Uani 1 1 d . . . O8A O 0.0770(2) 0.78783(18) 0.85530(16) 0.0209(8) Uani 1 1 d . . . C1A C 0.0825(4) 0.5935(3) 0.9168(3) 0.0231(12) Uani 1 1 d . . . C2A C 0.0994(4) 0.6364(3) 0.8471(3) 0.0241(12) Uani 1 1 d . . . C3A C 0.1914(4) 0.6367(3) 0.8134(2) 0.0193(11) Uani 1 1 d . . . C4A C 0.2647(4) 0.5900(3) 0.8495(3) 0.0229(12) Uani 1 1 d . . . H4A H 0.3260 0.5896 0.8267 0.027 Uiso 1 1 calc R . . C5A C 0.2511(4) 0.5443(3) 0.9176(3) 0.0240(12) Uani 1 1 d . . . C6A C 0.1589(4) 0.5485(3) 0.9505(3) 0.0247(12) Uani 1 1 d . . . H6A H 0.1478 0.5202 0.9968 0.030 Uiso 1 1 calc R . . C7A C 0.3319(4) 0.4921(3) 0.9558(3) 0.0313(14) Uani 1 1 d . . . C8A C 0.3042(4) 0.4143(3) 0.9861(3) 0.0416(16) Uani 1 1 d . . . H8A1 H 0.2465 0.4125 1.0166 0.062 Uiso 1 1 calc R . . H8A2 H 0.3543 0.3812 1.0106 0.062 Uiso 1 1 calc R . . H8A3 H 0.2946 0.4010 0.9498 0.062 Uiso 1 1 calc R . . C9A C 0.4259(4) 0.4924(3) 0.9109(3) 0.0428(17) Uani 1 1 d . . . H9A1 H 0.4177 0.4813 0.8730 0.064 Uiso 1 1 calc R . . H9A2 H 0.4726 0.4566 0.9369 0.064 Uiso 1 1 calc R . . H9A3 H 0.4467 0.5394 0.8943 0.064 Uiso 1 1 calc R . . C10A C 0.3449(5) 0.5112(4) 1.0162(3) 0.0491(19) Uani 1 1 d . . . H10A H 0.3656 0.5583 0.9990 0.074 Uiso 1 1 calc R . . H10B H 0.3918 0.4758 1.0425 0.074 Uiso 1 1 calc R . . H10C H 0.2855 0.5112 1.0446 0.074 Uiso 1 1 calc R . . C11A C 0.2101(4) 0.6895(3) 0.7408(3) 0.0248(12) Uani 1 1 d . . . H11A H 0.2770 0.6835 0.7242 0.030 Uiso 1 1 calc R . . H11B H 0.1732 0.6816 0.7113 0.030 Uiso 1 1 calc R . . C12A C 0.2274(4) 0.8181(3) 0.6852(2) 0.0243(12) Uani 1 1 d . . . H12A H 0.1979 0.8295 0.6443 0.029 Uiso 1 1 calc R . . H12B H 0.2941 0.8009 0.6771 0.029 Uiso 1 1 calc R . . C13A C 0.2180(4) 0.8849(3) 0.7014(3) 0.0237(12) Uani 1 1 d . . . C14A C 0.1276(4) 0.9161(3) 0.7180(3) 0.0234(12) Uani 1 1 d . . . C15A C 0.1188(4) 0.9743(3) 0.7394(3) 0.0248(12) Uani 1 1 d . . . C16A C 0.2001(4) 1.0035(3) 0.7376(2) 0.0244(12) Uani 1 1 d . . . H16A H 0.1935 1.0428 0.7507 0.029 Uiso 1 1 calc R . . C17A C 0.2912(4) 0.9760(3) 0.7170(2) 0.0221(12) Uani 1 1 d . . . C18A C 0.2979(4) 0.9150(3) 0.7004(2) 0.0225(12) Uani 1 1 d . . . H18A H 0.3577 0.8940 0.6882 0.027 Uiso 1 1 calc R . . C19A C 0.3815(4) 1.0084(3) 0.7139(3) 0.0240(12) Uani 1 1 d . . . C20A C 0.4481(4) 0.9513(3) 0.7640(3) 0.0357(15) Uani 1 1 d . . . H20A H 0.4625 0.9086 0.7534 0.054 Uiso 1 1 calc R . . H20B H 0.4173 0.9392 0.8098 0.054 Uiso 1 1 calc R . . H20C H 0.5060 0.9708 0.7598 0.054 Uiso 1 1 calc R . . C21A C 0.3582(4) 1.0761(3) 0.7322(3) 0.0357(15) Uani 1 1 d . . . H21A H 0.4160 1.0956 0.7283 0.054 Uiso 1 1 calc R . . H21B H 0.3277 1.0631 0.7782 0.054 Uiso 1 1 calc R . . H21C H 0.3164 1.1120 0.7015 0.054 Uiso 1 1 calc R . . C22A C 0.4332(4) 1.0306(3) 0.6416(3) 0.0287(13) Uani 1 1 d . . . H22A H 0.4454 0.9898 0.6281 0.043 Uiso 1 1 calc R . . H22B H 0.4925 1.0467 0.6405 0.043 Uiso 1 1 calc R . . H22C H 0.3944 1.0692 0.6108 0.043 Uiso 1 1 calc R . . C23A C 0.0213(4) 0.9995(3) 0.7666(3) 0.0294(13) Uani 1 1 d . . . H23A H 0.0202 1.0467 0.7684 0.035 Uiso 1 1 calc R . . H23B H -0.0256 1.0032 0.7377 0.035 Uiso 1 1 calc R . . C24A C -0.0919(4) 0.9582(3) 0.8679(3) 0.0340(14) Uani 1 1 d . . . H24A H -0.1405 0.9630 0.8398 0.041 Uiso 1 1 calc R . . H24B H -0.0986 1.0021 0.8770 0.041 Uiso 1 1 calc R . . C25A C -0.1005(4) 0.8933(3) 0.9332(3) 0.0260(13) Uani 1 1 d . . . C26A C -0.1135(4) 0.8280(3) 0.9302(3) 0.0252(12) Uani 1 1 d . . . C27A C -0.1128(4) 0.7647(3) 0.9911(3) 0.0238(12) Uani 1 1 d . . . C28A C -0.0993(4) 0.7686(3) 1.0511(3) 0.0253(12) Uani 1 1 d . . . H28A H -0.0974 0.7263 1.0902 0.030 Uiso 1 1 calc R . . C29A C -0.0882(4) 0.8339(3) 1.0562(3) 0.0275(13) Uani 1 1 d . . . C30A C -0.0894(4) 0.8950(3) 0.9951(3) 0.0288(13) Uani 1 1 d . . . H30A H -0.0824 0.9392 0.9962 0.035 Uiso 1 1 calc R . . C31A C -0.0725(4) 0.8357(3) 1.1239(3) 0.0337(14) Uani 1 1 d . . . C32A C 0.0249(9) 0.7933(7) 1.1451(6) 0.037(3) Uiso 0.507(9) 1 d PU . . C32C C 0.0105(10) 0.8889(7) 1.1078(7) 0.046(4) Uiso 0.493(9) 1 d PU . . C33A C -0.0862(11) 0.9081(8) 1.1247(7) 0.053(3) Uiso 0.507(9) 1 d PU . . C33C C -0.1625(10) 0.8722(7) 1.1524(7) 0.043(3) Uiso 0.493(9) 1 d PU . . C34A C -0.1518(10) 0.7903(7) 1.1844(7) 0.044(4) Uiso 0.507(9) 1 d P . . C34C C -0.0335(10) 0.7647(8) 1.1750(7) 0.047(4) Uiso 0.493(9) 1 d PU . . C35A C -0.1179(4) 0.6937(3) 0.9866(3) 0.0302(13) Uani 1 1 d . . . H35A H -0.1298 0.6569 1.0318 0.036 Uiso 1 1 calc R . . H35B H -0.1689 0.6983 0.9604 0.036 Uiso 1 1 calc R . . C36A C -0.0146(4) 0.6031(3) 0.9522(3) 0.0275(13) Uani 1 1 d . . . H36A H -0.0621 0.5984 0.9279 0.033 Uiso 1 1 calc R . . H36B H -0.0200 0.5669 0.9984 0.033 Uiso 1 1 calc R . . N1A N 0.2286(3) 0.7823(2) 0.9415(2) 0.0215(10) Uani 1 1 d . . . H1A H 0.2701 0.7819 0.9622 0.026 Uiso 1 1 d R . . N2A N 0.5450(4) 0.8342(3) 1.1122(2) 0.0398(13) Uani 1 1 d . . . O9A O 0.2388(3) 0.8780(2) 1.00416(19) 0.0286(9) Uani 1 1 d . . . O10A O 0.3774(3) 0.9592(2) 1.0703(2) 0.0438(11) Uani 1 1 d . . . O11A O 0.3007(3) 0.6876(2) 1.05763(18) 0.0289(9) Uani 1 1 d . . . O12A O 0.4236(3) 0.7089(2) 1.17880(19) 0.0413(11) Uani 1 1 d . . . O13A O 0.4219(3) 0.7917(2) 0.90732(18) 0.0271(9) Uani 1 1 d . . . O14A O 0.5650(3) 0.8020(2) 0.98930(19) 0.0379(10) Uani 1 1 d . . . C37A C 0.1480(4) 0.8394(3) 0.9474(3) 0.0268(13) Uani 1 1 d . . . H37A H 0.1109 0.8549 0.9093 0.032 Uiso 1 1 calc R . . H37B H 0.1065 0.8191 0.9892 0.032 Uiso 1 1 calc R . . C38A C 0.1857(4) 0.9034(3) 0.9475(3) 0.0335(14) Uani 1 1 d . . . H38A H 0.2261 0.9249 0.9054 0.040 Uiso 1 1 calc R . . H38B H 0.1336 0.9398 0.9517 0.040 Uiso 1 1 calc R . . C39A C 0.2875(5) 0.9325(3) 1.0050(3) 0.0368(15) Uani 1 1 d . . . H39A H 0.2428 0.9746 1.0050 0.044 Uiso 1 1 calc R . . H39B H 0.3338 0.9474 0.9650 0.044 Uiso 1 1 calc R . . C40A C 0.3364(5) 0.9012(3) 1.0684(3) 0.0442(17) Uani 1 1 d . . . H40A H 0.2911 0.8827 1.1084 0.053 Uiso 1 1 calc R . . H40B H 0.3854 0.8619 1.0668 0.053 Uiso 1 1 calc R . . C41A C 0.4324(5) 0.9374(4) 1.1267(3) 0.0510(19) Uani 1 1 d . . . H41A H 0.4023 0.9008 1.1661 0.061 Uiso 1 1 calc R . . H41B H 0.4325 0.9789 1.1384 0.061 Uiso 1 1 calc R . . C42A C 0.5331(5) 0.9077(4) 1.1113(3) 0.0485(18) Uani 1 1 d . . . H42A H 0.5583 0.9397 1.0666 0.058 Uiso 1 1 calc R . . H42B H 0.5708 0.9081 1.1443 0.058 Uiso 1 1 calc R . . C43A C 0.2000(4) 0.7066(3) 0.9753(3) 0.0251(12) Uani 1 1 d . . . H43A H 0.2418 0.6743 0.9564 0.030 Uiso 1 1 calc R . . H43B H 0.1352 0.7071 0.9680 0.030 Uiso 1 1 calc R . . C44A C 0.2075(4) 0.6813(3) 1.0510(3) 0.0331(14) Uani 1 1 d . . . H44A H 0.1617 0.7110 1.0708 0.040 Uiso 1 1 calc R . . H44B H 0.1949 0.6312 1.0743 0.040 Uiso 1 1 calc R . . C45A C 0.3094(4) 0.6971(3) 1.1188(3) 0.0289(13) Uani 1 1 d . . . H45A H 0.2864 0.6573 1.1586 0.035 Uiso 1 1 calc R . . H45B H 0.2727 0.7421 1.1192 0.035 Uiso 1 1 calc R . . C46A C 0.4147(4) 0.6988(3) 1.1188(3) 0.0302(14) Uani 1 1 d . . . H46A H 0.4513 0.6537 1.1187 0.036 Uiso 1 1 calc R . . H46B H 0.4378 0.7383 1.0786 0.036 Uiso 1 1 calc R . . C47A C 0.5210(4) 0.7068(4) 1.1887(3) 0.0414(16) Uani 1 1 d . . . H47A H 0.5635 0.6918 1.1551 0.050 Uiso 1 1 calc R . . H47B H 0.5332 0.6712 1.2336 0.050 Uiso 1 1 calc R . . C48A C 0.5415(5) 0.7792(4) 1.1823(3) 0.0403(16) Uani 1 1 d . . . H48A H 0.4929 0.7971 1.2112 0.048 Uiso 1 1 calc R . . H48B H 0.6021 0.7730 1.1991 0.048 Uiso 1 1 calc R . . C49A C 0.2746(4) 0.7992(3) 0.8695(2) 0.0253(12) Uani 1 1 d . . . H49A H 0.2406 0.7807 0.8460 0.030 Uiso 1 1 calc R . . H49B H 0.2721 0.8513 0.8452 0.030 Uiso 1 1 calc R . . C50A C 0.3761(4) 0.7649(3) 0.8702(3) 0.0280(13) Uani 1 1 d . . . H50A H 0.3790 0.7125 0.8919 0.034 Uiso 1 1 calc R . . H50B H 0.4074 0.7772 0.8239 0.034 Uiso 1 1 calc R . . C51A C 0.5148(4) 0.7532(3) 0.9183(3) 0.0333(14) Uani 1 1 d . . . H51A H 0.5400 0.7376 0.8809 0.040 Uiso 1 1 calc R . . H51B H 0.5109 0.7103 0.9601 0.040 Uiso 1 1 calc R . . C52A C 0.5810(4) 0.7998(4) 0.9235(3) 0.0371(15) Uani 1 1 d . . . H52A H 0.6465 0.7801 0.9149 0.045 Uiso 1 1 calc R . . H52B H 0.5703 0.8485 0.8895 0.045 Uiso 1 1 calc R . . C53A C 0.6251(5) 0.8465(4) 0.9964(3) 0.0471(18) Uani 1 1 d . . . H53A H 0.5975 0.8969 0.9788 0.057 Uiso 1 1 calc R . . H53B H 0.6871 0.8420 0.9709 0.057 Uiso 1 1 calc R . . C54A C 0.6349(4) 0.8217(4) 1.0712(3) 0.0473(19) Uani 1 1 d . . . H54A H 0.6579 0.7703 1.0886 0.057 Uiso 1 1 calc R . . H54B H 0.6821 0.8471 1.0764 0.057 Uiso 1 1 calc R . . U2 U 0.540793(14) 0.691102(10) 0.713147(9) 0.01992(6) Uani 1 1 d . . . O1B O 0.6004(3) 0.60719(19) 0.80608(18) 0.0272(9) Uani 1 1 d . . . O2B O 0.6002(3) 0.5521(2) 0.70327(19) 0.0334(10) Uani 1 1 d . . . O3B O 0.4606(2) 0.67690(19) 0.63992(18) 0.0243(8) Uani 1 1 d . . . O4B O 0.5441(3) 0.81880(19) 0.53311(19) 0.0281(9) Uani 1 1 d . . . O5B O 0.5234(2) 0.81053(18) 0.68514(17) 0.0215(8) Uani 1 1 d . . . O6B O 0.6867(3) 0.73387(19) 0.75950(18) 0.0265(9) Uani 1 1 d . . . O7B O 0.4311(3) 0.68869(19) 0.76730(18) 0.0261(9) Uani 1 1 d . . . O8B O 0.6464(2) 0.69544(18) 0.65544(17) 0.0211(8) Uani 1 1 d . . . C1B C 0.7639(4) 0.6128(3) 0.8068(2) 0.0237(12) Uani 1 1 d . . . C2B C 0.6920(4) 0.5791(3) 0.7989(3) 0.0237(12) Uani 1 1 d . . . C3B C 0.7153(4) 0.5202(3) 0.7799(2) 0.0218(12) Uani 1 1 d . . . C4B C 0.8115(4) 0.4924(3) 0.7723(3) 0.0257(13) Uani 1 1 d . . . H4B H 0.8270 0.4524 0.7598 0.031 Uiso 1 1 calc R . . C5B C 0.8845(4) 0.5220(3) 0.7825(2) 0.0230(12) Uani 1 1 d . . . C6B C 0.8586(4) 0.5832(3) 0.7990(2) 0.0217(11) Uani 1 1 d . . . H6B H 0.9060 0.6051 0.8049 0.026 Uiso 1 1 calc R . . C7B C 0.9903(4) 0.4901(3) 0.7762(3) 0.0258(12) Uani 1 1 d . . . C8B C 1.0522(4) 0.5506(3) 0.7298(3) 0.0298(13) Uani 1 1 d . . . H8B1 H 1.1181 0.5307 0.7291 0.045 Uiso 1 1 calc R . . H8B2 H 1.0425 0.5884 0.7473 0.045 Uiso 1 1 calc R . . H8B3 H 1.0345 0.5702 0.6843 0.045 Uiso 1 1 calc R . . C9B C 1.0065(4) 0.4319(3) 0.7466(3) 0.0379(15) Uani 1 1 d . . . H9B1 H 0.9837 0.4517 0.7026 0.057 Uiso 1 1 calc R . . H9B2 H 0.9727 0.3921 0.7765 0.057 Uiso 1 1 calc R . . H9B3 H 1.0732 0.4153 0.7420 0.057 Uiso 1 1 calc R . . C10B C 1.0235(4) 0.4575(3) 0.8483(3) 0.0352(15) Uani 1 1 d . . . H10D H 0.9851 0.4204 0.8781 0.053 Uiso 1 1 calc R . . H10E H 1.0170 0.4950 0.8659 0.053 Uiso 1 1 calc R . . H10F H 1.0889 0.4368 0.8457 0.053 Uiso 1 1 calc R . . C11B C 0.6360(4) 0.4943(3) 0.7627(3) 0.0265(13) Uani 1 1 d . . . H11C H 0.6592 0.4510 0.7531 0.032 Uiso 1 1 calc R . . H11D H 0.5859 0.4830 0.8006 0.032 Uiso 1 1 calc R . . C12B C 0.5411(4) 0.5330(3) 0.6674(3) 0.0289(13) Uani 1 1 d . . . H12C H 0.4762 0.5326 0.6895 0.035 Uiso 1 1 calc R . . H12D H 0.5644 0.4852 0.6669 0.035 Uiso 1 1 calc R . . C13B C 0.5447(4) 0.5890(3) 0.5958(3) 0.0250(12) Uani 1 1 d . . . C14B C 0.5036(4) 0.6608(3) 0.5861(3) 0.0251(12) Uani 1 1 d . . . C15B C 0.5127(4) 0.7152(3) 0.5203(3) 0.0242(12) Uani 1 1 d . . . C16B C 0.5598(4) 0.6973(3) 0.4658(3) 0.0275(13) Uani 1 1 d . . . H16B H 0.5650 0.7338 0.4226 0.033 Uiso 1 1 calc R . . C17B C 0.5994(4) 0.6268(3) 0.4736(3) 0.0297(13) Uani 1 1 d . . . C18B C 0.5912(4) 0.5737(3) 0.5398(3) 0.0291(13) Uani 1 1 d . . . H18B H 0.6179 0.5263 0.5465 0.035 Uiso 1 1 calc R . . C19B C 0.6510(5) 0.6061(4) 0.4138(3) 0.0389(15) Uani 1 1 d . . . C20B C 0.7535(6) 0.5679(5) 0.4277(4) 0.045(2) Uiso 0.862(9) 1 d PU . . C20C C 0.766(4) 0.602(3) 0.413(3) 0.047(8) Uiso 0.138(9) 1 d PU . . C21B C 0.5939(6) 0.5547(5) 0.4038(4) 0.055(2) Uiso 0.862(9) 1 d PU . . C21C C 0.684(4) 0.508(3) 0.443(3) 0.055(16) Uiso 0.138(9) 1 d P . . C22B C 0.6584(6) 0.6753(4) 0.3449(4) 0.048(2) Uiso 0.862(9) 1 d P . . C22C C 0.572(4) 0.611(3) 0.369(3) 0.051(9) Uiso 0.138(9) 1 d PU . . C23B C 0.4751(4) 0.7917(3) 0.5122(3) 0.0272(13) Uani 1 1 d . . . H23C H 0.4654 0.8209 0.4650 0.033 Uiso 1 1 calc R . . H23D H 0.4147 0.7931 0.5404 0.033 Uiso 1 1 calc R . . C24B C 0.5113(4) 0.8850(3) 0.5438(3) 0.0232(12) Uani 1 1 d . . . H24C H 0.4505 0.8816 0.5722 0.028 Uiso 1 1 calc R . . H24D H 0.5036 0.9254 0.5006 0.028 Uiso 1 1 calc R . . C25B C 0.5852(4) 0.8956(3) 0.5785(3) 0.0210(11) Uani 1 1 d . . . C26B C 0.5912(4) 0.8532(3) 0.6490(3) 0.0190(11) Uani 1 1 d . . . C27B C 0.6669(4) 0.8563(3) 0.6789(3) 0.0221(12) Uani 1 1 d . . . C28B C 0.7356(4) 0.9022(3) 0.6413(3) 0.0245(12) Uani 1 1 d . . . H28B H 0.7858 0.9034 0.6626 0.029 Uiso 1 1 calc R . . C29B C 0.7307(4) 0.9461(3) 0.5727(3) 0.0231(12) Uani 1 1 d . . . C30B C 0.6547(4) 0.9412(3) 0.5427(3) 0.0213(11) Uani 1 1 d . . . H30B H 0.6504 0.9697 0.4968 0.026 Uiso 1 1 calc R . . C31B C 0.8035(4) 0.9993(3) 0.5303(3) 0.0275(13) Uani 1 1 d . . . C32B C 0.7501(4) 1.0771(3) 0.5079(3) 0.0421(17) Uani 1 1 d . . . H32A H 0.7238 1.0877 0.5475 0.063 Uiso 1 1 calc R . . H32B H 0.6998 1.0807 0.4823 0.063 Uiso 1 1 calc R . . H32C H 0.7937 1.1110 0.4799 0.063 Uiso 1 1 calc R . . C33B C 0.8825(4) 0.9943(3) 0.5720(3) 0.0373(16) Uani 1 1 d . . . H33A H 0.8551 1.0077 0.6100 0.056 Uiso 1 1 calc R . . H33B H 0.9277 1.0267 0.5437 0.056 Uiso 1 1 calc R . . H33C H 0.9139 0.9456 0.5885 0.056 Uiso 1 1 calc R . . C34B C 0.8487(4) 0.9838(3) 0.4670(3) 0.0394(16) Uani 1 1 d . . . H34A H 0.8912 1.0189 0.4400 0.059 Uiso 1 1 calc R . . H34B H 0.7997 0.9868 0.4406 0.059 Uiso 1 1 calc R . . H34C H 0.8835 0.9361 0.4807 0.059 Uiso 1 1 calc R . . C35B C 0.6748(4) 0.8088(3) 0.7530(3) 0.0209(11) Uani 1 1 d . . . H35C H 0.7290 0.8184 0.7679 0.025 Uiso 1 1 calc R . . H35D H 0.6178 0.8187 0.7812 0.025 Uiso 1 1 calc R . . C36B C 0.7347(4) 0.6832(3) 0.8170(3) 0.0255(12) Uani 1 1 d . . . H36C H 0.6924 0.6757 0.8590 0.031 Uiso 1 1 calc R . . H36D H 0.7903 0.7022 0.8200 0.031 Uiso 1 1 calc R . . N1B N 0.8334(3) 0.7092(2) 0.5626(2) 0.0214(10) Uani 1 1 d . . . H1B H 0.8974 0.7119 0.5344 0.026 Uiso 1 1 d R . . N2B N 1.2503(3) 0.7194(2) 0.3492(2) 0.0290(11) Uani 1 1 d . . . O9B O 1.0140(3) 0.72280(19) 0.58438(18) 0.0239(8) Uani 1 1 d . . . O10B O 1.1952(3) 0.7384(2) 0.48308(19) 0.0319(9) Uani 1 1 d . . . O11B O 0.9415(3) 0.6186(2) 0.50229(18) 0.0298(9) Uani 1 1 d . . . O12B O 1.1702(3) 0.57599(19) 0.4212(2) 0.0308(9) Uani 1 1 d . . . O13B O 0.8916(3) 0.8053(2) 0.43666(18) 0.0290(9) Uani 1 1 d . . . O14B O 1.0721(3) 0.8196(2) 0.2956(2) 0.0387(11) Uani 1 1 d . . . C37B C 0.8541(4) 0.7067(3) 0.6299(3) 0.0273(13) Uani 1 1 d . . . H37C H 0.7973 0.7255 0.6524 0.033 Uiso 1 1 calc R . . H37D H 0.8728 0.6570 0.6594 0.033 Uiso 1 1 calc R . . C38B C 0.9325(4) 0.7513(3) 0.6180(3) 0.0314(14) Uani 1 1 d . . . H38C H 0.9133 0.8015 0.5900 0.038 Uiso 1 1 calc R . . H38D H 0.9468 0.7492 0.6611 0.038 Uiso 1 1 calc R . . C39B C 1.0908(4) 0.7632(3) 0.5720(3) 0.0313(14) Uani 1 1 d . . . H39C H 1.0946 0.7721 0.6125 0.038 Uiso 1 1 calc R . . H39D H 1.0791 0.8097 0.5350 0.038 Uiso 1 1 calc R . . C40B C 1.1833(4) 0.7239(3) 0.5539(3) 0.0328(14) Uani 1 1 d . . . H40C H 1.2353 0.7397 0.5654 0.039 Uiso 1 1 calc R . . H40D H 1.1839 0.6722 0.5797 0.039 Uiso 1 1 calc R . . C41B C 1.2876(4) 0.7101(4) 0.4610(3) 0.0416(16) Uani 1 1 d . . . H41C H 1.2915 0.6579 0.4753 0.050 Uiso 1 1 calc R . . H41D H 1.3355 0.7203 0.4815 0.050 Uiso 1 1 calc R . . C42B C 1.3059(4) 0.7449(3) 0.3838(3) 0.0395(16) Uani 1 1 d . . . H42C H 1.2906 0.7971 0.3697 0.047 Uiso 1 1 calc R . . H42D H 1.3730 0.7347 0.3698 0.047 Uiso 1 1 calc R . . C43B C 0.8003(4) 0.6408(3) 0.5696(3) 0.0266(12) Uani 1 1 d . . . H43C H 0.7622 0.6503 0.5332 0.032 Uiso 1 1 calc R . . H43D H 0.7612 0.6215 0.6129 0.032 Uiso 1 1 calc R . . C44B C 0.8865(4) 0.5863(3) 0.5660(3) 0.0286(13) Uani 1 1 d . . . H44C H 0.9235 0.5751 0.6033 0.034 Uiso 1 1 calc R . . H44D H 0.8667 0.5418 0.5690 0.034 Uiso 1 1 calc R . . C45B C 1.0381(4) 0.5869(3) 0.5001(3) 0.0293(13) Uani 1 1 d . . . H45C H 1.0421 0.5345 0.5179 0.035 Uiso 1 1 calc R . . H45D H 1.0727 0.6006 0.5270 0.035 Uiso 1 1 calc R . . C46B C 1.0785(4) 0.6155(3) 0.4261(3) 0.0362(15) Uani 1 1 d . . . H46C H 1.0377 0.6087 0.3983 0.043 Uiso 1 1 calc R . . H46D H 1.0835 0.6669 0.4103 0.043 Uiso 1 1 calc R . . C47B C 1.2210(4) 0.6006(3) 0.3543(3) 0.0362(15) Uani 1 1 d . . . H47C H 1.1764 0.6277 0.3211 0.043 Uiso 1 1 calc R . . H47D H 1.2528 0.5592 0.3438 0.043 Uiso 1 1 calc R . . C48B C 1.2935(4) 0.6481(3) 0.3492(3) 0.0323(14) Uani 1 1 d . . . H48C H 1.3308 0.6238 0.3874 0.039 Uiso 1 1 calc R . . H48D H 1.3364 0.6546 0.3076 0.039 Uiso 1 1 calc R . . C49B C 0.7688(4) 0.7762(3) 0.5273(3) 0.0292(13) Uani 1 1 d . . . H49C H 0.7776 0.8155 0.5398 0.035 Uiso 1 1 calc R . . H49D H 0.7029 0.7672 0.5408 0.035 Uiso 1 1 calc R . . C50B C 0.7933(4) 0.7965(3) 0.4510(3) 0.0362(15) Uani 1 1 d . . . H50C H 0.7814 0.7585 0.4379 0.043 Uiso 1 1 calc R . . H50D H 0.7553 0.8413 0.4262 0.043 Uiso 1 1 calc R . . C51B C 0.9315(4) 0.8066(3) 0.3711(3) 0.0332(14) Uani 1 1 d . . . H51C H 0.8953 0.8436 0.3363 0.040 Uiso 1 1 calc R . . H51D H 0.9303 0.7601 0.3686 0.040 Uiso 1 1 calc R . . C52B C 1.0322(4) 0.8227(3) 0.3601(3) 0.0339(15) Uani 1 1 d . . . H52C H 1.0335 0.8705 0.3598 0.041 Uiso 1 1 calc R . . H52D H 1.0678 0.7871 0.3961 0.041 Uiso 1 1 calc R . . C53B C 1.1669(5) 0.8372(3) 0.2752(3) 0.0465(18) Uani 1 1 d . . . H53C H 1.1821 0.8592 0.3041 0.056 Uiso 1 1 calc R . . H53D H 1.1716 0.8724 0.2286 0.056 Uiso 1 1 calc R . . C54B C 1.2382(4) 0.7710(3) 0.2798(3) 0.0350(15) Uani 1 1 d . . . H54C H 1.2182 0.7462 0.2550 0.042 Uiso 1 1 calc R . . H54D H 1.2994 0.7868 0.2573 0.042 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 0.02075(12) 0.02339(11) 0.01918(11) -0.00776(9) -0.00431(8) -0.00284(8) O1A 0.023(2) 0.0232(19) 0.030(2) -0.0064(18) -0.0057(17) -0.0020(16) O2A 0.037(2) 0.0170(18) 0.021(2) -0.0015(17) 0.0009(16) -0.0066(16) O3A 0.021(2) 0.0249(19) 0.030(2) -0.0029(18) -0.0112(16) -0.0026(16) O4A 0.031(3) 0.045(3) 0.032(2) 0.010(2) 0.0131(19) 0.014(2) O5A 0.022(2) 0.050(3) 0.0199(19) -0.0127(19) -0.0057(16) 0.0009(18) O6A 0.035(3) 0.037(2) 0.078(3) -0.043(2) 0.028(2) -0.021(2) O7A 0.025(2) 0.032(2) 0.027(2) -0.0106(18) -0.0054(16) -0.0008(17) O8A 0.026(2) 0.0210(18) 0.0175(18) -0.0084(16) -0.0042(15) -0.0032(15) C1A 0.028(3) 0.021(3) 0.022(3) -0.008(2) -0.004(2) -0.008(2) C2A 0.026(3) 0.020(3) 0.028(3) -0.010(3) -0.004(2) -0.005(2) C3A 0.024(3) 0.018(3) 0.017(3) -0.008(2) -0.001(2) -0.002(2) C4A 0.021(3) 0.021(3) 0.026(3) -0.011(2) 0.001(2) -0.002(2) C5A 0.028(3) 0.020(3) 0.022(3) -0.003(2) -0.005(2) -0.007(2) C6A 0.032(3) 0.021(3) 0.019(3) -0.002(2) -0.004(2) -0.011(2) C7A 0.030(3) 0.027(3) 0.029(3) 0.001(3) -0.009(3) -0.005(2) C8A 0.034(4) 0.027(3) 0.051(4) -0.002(3) -0.008(3) -0.001(3) C9A 0.031(4) 0.040(4) 0.046(4) -0.001(3) -0.013(3) -0.004(3) C10A 0.047(4) 0.055(4) 0.044(4) -0.009(4) -0.025(3) -0.008(3) C11A 0.028(3) 0.020(3) 0.025(3) -0.007(2) 0.001(2) -0.004(2) C12A 0.026(3) 0.030(3) 0.017(3) -0.008(2) -0.001(2) -0.007(2) C13A 0.033(3) 0.018(3) 0.018(3) -0.002(2) -0.004(2) -0.009(2) C14A 0.029(3) 0.022(3) 0.016(3) 0.002(2) -0.007(2) -0.010(2) C15A 0.031(3) 0.019(3) 0.015(3) 0.001(2) -0.001(2) 0.000(2) C16A 0.040(3) 0.016(3) 0.015(3) -0.005(2) 0.001(2) -0.003(2) C17A 0.028(3) 0.021(3) 0.012(2) -0.001(2) 0.000(2) -0.004(2) C18A 0.028(3) 0.022(3) 0.013(2) -0.004(2) -0.001(2) -0.001(2) C19A 0.028(3) 0.024(3) 0.021(3) -0.008(2) -0.006(2) -0.004(2) C20A 0.036(4) 0.038(3) 0.032(3) -0.006(3) -0.010(3) -0.013(3) C21A 0.040(4) 0.035(3) 0.043(4) -0.022(3) -0.004(3) -0.013(3) C22A 0.027(3) 0.030(3) 0.029(3) -0.010(3) -0.001(2) -0.007(2) C23A 0.035(3) 0.019(3) 0.025(3) -0.002(3) -0.005(2) 0.004(2) C24A 0.030(3) 0.033(3) 0.028(3) -0.009(3) 0.005(3) 0.006(3) C25A 0.021(3) 0.030(3) 0.018(3) -0.003(3) 0.001(2) 0.001(2) C26A 0.016(3) 0.034(3) 0.025(3) -0.013(3) -0.002(2) 0.002(2) C27A 0.021(3) 0.028(3) 0.024(3) -0.014(3) 0.001(2) 0.001(2) C28A 0.024(3) 0.020(3) 0.026(3) -0.007(3) 0.001(2) 0.001(2) C29A 0.028(3) 0.028(3) 0.026(3) -0.012(3) -0.005(2) 0.003(2) C30A 0.031(3) 0.018(3) 0.033(3) -0.009(3) 0.001(3) -0.001(2) C31A 0.043(4) 0.030(3) 0.029(3) -0.014(3) -0.006(3) 0.002(3) C35A 0.025(3) 0.039(3) 0.025(3) -0.009(3) -0.002(2) -0.008(3) C36A 0.033(3) 0.022(3) 0.029(3) -0.011(3) 0.000(3) -0.009(2) N1A 0.024(2) 0.021(2) 0.021(2) -0.006(2) -0.0039(19) -0.0068(18) N2A 0.038(3) 0.061(4) 0.024(3) -0.018(3) -0.003(2) -0.012(3) O9A 0.028(2) 0.030(2) 0.032(2) -0.0151(19) -0.0075(17) -0.0031(17) O10A 0.054(3) 0.041(3) 0.050(3) -0.024(2) -0.019(2) -0.011(2) O11A 0.031(2) 0.031(2) 0.025(2) -0.0088(18) -0.0105(17) -0.0044(17) O12A 0.034(3) 0.071(3) 0.026(2) -0.024(2) -0.0068(19) -0.009(2) O13A 0.025(2) 0.029(2) 0.026(2) -0.0085(18) -0.0062(16) -0.0007(17) O14A 0.034(2) 0.057(3) 0.026(2) -0.017(2) 0.0008(18) -0.017(2) C37A 0.025(3) 0.029(3) 0.029(3) -0.015(3) -0.006(2) 0.001(2) C38A 0.036(4) 0.027(3) 0.037(3) -0.010(3) -0.014(3) 0.001(3) C39A 0.044(4) 0.029(3) 0.042(4) -0.013(3) -0.015(3) -0.007(3) C40A 0.060(5) 0.039(4) 0.045(4) -0.016(3) -0.025(3) -0.015(3) C41A 0.062(5) 0.059(5) 0.041(4) -0.020(4) -0.011(4) -0.020(4) C42A 0.054(5) 0.069(5) 0.035(4) -0.023(4) -0.009(3) -0.025(4) C43A 0.024(3) 0.025(3) 0.026(3) -0.008(3) -0.005(2) -0.006(2) C44A 0.036(4) 0.035(3) 0.024(3) -0.003(3) -0.008(3) -0.007(3) C45A 0.038(4) 0.028(3) 0.014(3) 0.001(3) -0.004(2) -0.006(3) C46A 0.034(3) 0.032(3) 0.020(3) -0.003(3) -0.007(2) -0.001(3) C47A 0.032(4) 0.060(4) 0.034(3) -0.019(3) -0.008(3) -0.002(3) C48A 0.037(4) 0.063(4) 0.025(3) -0.014(3) -0.011(3) -0.015(3) C49A 0.028(3) 0.033(3) 0.015(3) -0.008(3) -0.001(2) -0.009(2) C50A 0.023(3) 0.036(3) 0.027(3) -0.015(3) -0.001(2) -0.006(2) C51A 0.029(3) 0.044(4) 0.027(3) -0.017(3) 0.004(3) -0.003(3) C52A 0.028(3) 0.052(4) 0.025(3) -0.011(3) 0.006(3) -0.007(3) C53A 0.034(4) 0.072(5) 0.036(4) -0.018(4) -0.002(3) -0.020(3) C54A 0.025(4) 0.079(5) 0.034(3) -0.012(4) -0.007(3) -0.016(3) U2 0.01893(12) 0.02116(11) 0.01883(11) -0.00707(9) 0.00038(8) -0.00418(8) O1B 0.029(2) 0.027(2) 0.0206(19) -0.0045(17) -0.0001(16) -0.0049(17) O2B 0.043(3) 0.026(2) 0.029(2) 0.0013(19) -0.0164(19) -0.0167(18) O3B 0.019(2) 0.029(2) 0.028(2) -0.0138(18) -0.0018(16) -0.0045(16) O4B 0.026(2) 0.026(2) 0.036(2) -0.0158(18) -0.0093(17) 0.0019(16) O5B 0.021(2) 0.0188(18) 0.0221(19) -0.0066(16) -0.0003(15) -0.0016(15) O6B 0.039(2) 0.0189(19) 0.0210(19) -0.0055(17) -0.0071(17) -0.0022(16) O7B 0.024(2) 0.028(2) 0.024(2) -0.0088(17) 0.0016(16) -0.0065(16) O8B 0.0190(19) 0.0210(18) 0.0197(18) -0.0049(16) -0.0003(15) -0.0024(15) C1B 0.033(3) 0.023(3) 0.010(2) -0.001(2) 0.000(2) -0.006(2) C2B 0.023(3) 0.026(3) 0.014(3) -0.001(2) -0.001(2) -0.002(2) C3B 0.033(3) 0.016(3) 0.015(3) 0.000(2) -0.007(2) -0.007(2) C4B 0.034(3) 0.016(3) 0.021(3) 0.002(2) -0.009(2) -0.003(2) C5B 0.029(3) 0.022(3) 0.014(3) -0.002(2) -0.006(2) -0.003(2) C6B 0.026(3) 0.024(3) 0.014(3) -0.006(2) -0.004(2) -0.003(2) C7B 0.026(3) 0.027(3) 0.023(3) -0.008(3) -0.003(2) -0.002(2) C8B 0.021(3) 0.031(3) 0.033(3) -0.010(3) -0.001(2) -0.001(2) C9B 0.040(4) 0.030(3) 0.045(4) -0.019(3) -0.001(3) 0.001(3) C10B 0.031(3) 0.038(3) 0.030(3) -0.007(3) -0.009(3) 0.002(3) C11B 0.025(3) 0.026(3) 0.024(3) -0.004(3) -0.005(2) -0.003(2) C12B 0.030(3) 0.030(3) 0.031(3) -0.011(3) -0.010(3) -0.010(3) C13B 0.025(3) 0.027(3) 0.027(3) -0.010(3) -0.009(2) -0.008(2) C14B 0.022(3) 0.030(3) 0.027(3) -0.011(3) -0.008(2) -0.005(2) C15B 0.026(3) 0.022(3) 0.027(3) -0.010(3) -0.010(2) -0.003(2) C16B 0.028(3) 0.032(3) 0.024(3) -0.011(3) -0.007(2) -0.002(2) C17B 0.030(3) 0.038(3) 0.027(3) -0.015(3) -0.009(3) -0.005(3) C18B 0.025(3) 0.031(3) 0.039(3) -0.021(3) -0.006(3) -0.002(2) C19B 0.041(4) 0.050(4) 0.032(3) -0.022(3) -0.007(3) -0.006(3) C23B 0.029(3) 0.027(3) 0.025(3) -0.007(3) -0.009(2) -0.002(2) C24B 0.018(3) 0.026(3) 0.024(3) -0.010(2) 0.002(2) -0.001(2) C25B 0.015(3) 0.017(3) 0.028(3) -0.007(2) -0.002(2) 0.003(2) C26B 0.017(3) 0.016(3) 0.020(3) -0.005(2) 0.001(2) 0.000(2) C27B 0.025(3) 0.015(3) 0.026(3) -0.009(2) -0.003(2) 0.000(2) C28B 0.019(3) 0.024(3) 0.028(3) -0.007(3) -0.005(2) 0.000(2) C29B 0.023(3) 0.018(3) 0.025(3) -0.006(2) -0.004(2) 0.001(2) C30B 0.020(3) 0.024(3) 0.016(3) -0.002(2) -0.004(2) -0.003(2) C31B 0.024(3) 0.023(3) 0.029(3) -0.002(3) -0.006(2) -0.005(2) C32B 0.036(4) 0.024(3) 0.052(4) 0.004(3) -0.011(3) -0.005(3) C33B 0.025(3) 0.034(3) 0.041(4) 0.001(3) -0.003(3) -0.012(3) C34B 0.034(4) 0.041(4) 0.033(3) -0.002(3) 0.003(3) -0.015(3) C35B 0.019(3) 0.020(3) 0.022(3) -0.006(2) 0.000(2) -0.007(2) C36B 0.031(3) 0.026(3) 0.018(3) -0.007(2) -0.007(2) 0.001(2) N1B 0.023(2) 0.020(2) 0.021(2) -0.006(2) -0.0039(18) -0.0032(18) N2B 0.026(3) 0.030(3) 0.028(3) -0.010(2) 0.003(2) -0.003(2) O9B 0.021(2) 0.029(2) 0.028(2) -0.0172(18) 0.0015(16) -0.0071(16) O10B 0.022(2) 0.044(2) 0.031(2) -0.015(2) -0.0031(17) -0.0031(18) O11B 0.030(2) 0.031(2) 0.026(2) -0.0120(18) 0.0032(17) -0.0026(17) O12B 0.027(2) 0.025(2) 0.038(2) -0.0154(19) 0.0085(18) 0.0000(17) O13B 0.023(2) 0.036(2) 0.0200(19) -0.0060(18) 0.0050(16) -0.0035(17) O14B 0.037(3) 0.041(2) 0.029(2) -0.009(2) 0.0034(19) 0.003(2) C37B 0.024(3) 0.034(3) 0.024(3) -0.012(3) -0.002(2) -0.002(2) C38B 0.027(3) 0.046(4) 0.035(3) -0.028(3) -0.004(3) -0.007(3) C39B 0.029(3) 0.037(3) 0.033(3) -0.016(3) -0.004(3) -0.009(3) C40B 0.028(3) 0.040(4) 0.032(3) -0.014(3) -0.004(3) -0.010(3) C41B 0.021(3) 0.066(5) 0.046(4) -0.031(4) -0.002(3) -0.003(3) C42B 0.026(3) 0.044(4) 0.051(4) -0.023(3) 0.012(3) -0.015(3) C43B 0.027(3) 0.028(3) 0.031(3) -0.017(3) 0.001(2) -0.010(2) C44B 0.031(3) 0.027(3) 0.030(3) -0.016(3) 0.005(2) -0.004(2) C45B 0.021(3) 0.030(3) 0.039(3) -0.019(3) 0.000(2) 0.000(2) C46B 0.030(4) 0.032(3) 0.043(4) -0.014(3) 0.004(3) -0.005(3) C47B 0.039(4) 0.036(3) 0.034(3) -0.018(3) 0.001(3) 0.002(3) C48B 0.026(3) 0.035(3) 0.032(3) -0.014(3) -0.001(2) 0.005(3) C49B 0.019(3) 0.030(3) 0.028(3) -0.005(3) 0.001(2) 0.004(2) C50B 0.030(3) 0.043(4) 0.023(3) -0.003(3) -0.001(3) 0.000(3) C51B 0.031(3) 0.035(3) 0.020(3) -0.001(3) 0.001(2) 0.002(3) C52B 0.037(4) 0.026(3) 0.027(3) -0.001(3) 0.005(3) -0.004(3) C53B 0.048(4) 0.031(3) 0.038(4) 0.001(3) 0.017(3) -0.004(3) C54B 0.028(3) 0.034(3) 0.030(3) -0.006(3) 0.012(3) -0.002(3) _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 O8A 1.772(3) . ? U1 O7A 1.793(4) . ? U1 O3A 2.204(3) . ? U1 O1A 2.220(4) . ? U1 O5A 2.236(4) . ? U1 O2A 2.848(4) . ? O1A C2A 1.352(6) . ? O2A C12A 1.444(6) . ? O2A C11A 1.467(6) . ? O3A C14A 1.346(6) . ? O4A C24A 1.437(7) . ? O4A C23A 1.445(6) . ? O5A C26A 1.337(6) . ? O6A C36A 1.427(6) . ? O6A C35A 1.435(7) . ? O9A C39A 1.419(7) . ? O9A C38A 1.420(6) . ? O10A C40A 1.426(7) . ? O10A C41A 1.440(7) . ? O11A C44A 1.406(7) . ? O11A C45A 1.433(6) . ? O12A C46A 1.417(7) . ? O12A C47A 1.444(7) . ? O13A C50A 1.426(6) . ? O13A C51A 1.426(7) . ? O14A C52A 1.410(7) . ? O14A C53A 1.424(7) . ? C1A C6A 1.397(7) . ? C1A C2A 1.404(7) . ? C1A C36A 1.488(8) . ? C2A C3A 1.392(7) . ? C3A C4A 1.395(7) . ? C3A C11A 1.509(7) . ? C4A C5A 1.386(7) . ? C5A C6A 1.395(8) . ? C5A C7A 1.529(7) . ? C7A C9A 1.516(8) . ? C7A C8A 1.545(8) . ? C7A C10A 1.545(9) . ? C12A C13A 1.507(7) . ? C13A C18A 1.389(7) . ? C13A C14A 1.392(8) . ? C14A C15A 1.405(8) . ? C15A C16A 1.393(8) . ? C15A C23A 1.503(7) . ? C16A C17A 1.396(7) . ? C17A C18A 1.402(7) . ? C17A C19A 1.540(7) . ? C19A C22A 1.527(7) . ? C19A C20A 1.542(7) . ? C19A C21A 1.541(8) . ? C24A C25A 1.498(7) . ? C25A C30A 1.383(8) . ? C25A C26A 1.399(8) . ? C26A C27A 1.420(7) . ? C27A C28A 1.375(8) . ? C27A C35A 1.499(8) . ? C28A C29A 1.410(8) . ? C29A C30A 1.400(8) . ? C29A C31A 1.528(8) . ? C31A C33A 1.452(15) . ? C31A C34C 1.501(15) . ? C31A C33C 1.527(15) . ? C31A C32A 1.543(13) . ? C31A C34A 1.657(14) . ? C32C C33A 1.398(19) . ? C33A C33C 1.342(19) . ? C33C C34A 1.511(18) . ? C34A C34C 1.688(19) . ? N1A C49A 1.501(6) . ? N1A C37A 1.509(7) . ? N1A C43A 1.512(6) . ? N2A C42A 1.460(9) . ? N2A C48A 1.472(7) . ? N2A C54A 1.474(8) . ? C37A C38A 1.495(8) . ? C39A C40A 1.496(8) . ? C41A C42A 1.498(10) . ? C43A C44A 1.516(7) . ? C45A C46A 1.521(8) . ? C47A C48A 1.498(9) . ? C49A C50A 1.498(7) . ? C51A C52A 1.504(8) . ? C53A C54A 1.507(8) . ? U2 O8B 1.776(3) . ? U2 O7B 1.784(4) . ? U2 O5B 2.226(3) . ? U2 O1B 2.231(3) . ? U2 O3B 2.241(4) . ? U2 O6B 2.871(4) . ? U2 O2B 2.873(4) . ? O1B C2B 1.344(6) . ? O2B C12B 1.436(6) . ? O2B C11B 1.444(6) . ? O3B C14B 1.344(6) . ? O4B C23B 1.430(6) . ? O4B C24B 1.434(6) . ? O5B C26B 1.344(6) . ? O6B C36B 1.445(6) . ? O6B C35B 1.450(6) . ? O9B C38B 1.421(6) . ? O9B C39B 1.419(6) . ? O10B C40B 1.416(7) . ? O10B C41B 1.427(7) . ? O11B C45B 1.421(6) . ? O11B C44B 1.422(6) . ? O12B C46B 1.423(7) . ? O12B C47B 1.429(7) . ? O13B C51B 1.417(6) . ? O13B C50B 1.422(7) . ? O14B C52B 1.426(7) . ? O14B C53B 1.421(7) . ? C1B C6B 1.394(7) . ? C1B C2B 1.407(7) . ? C1B C36B 1.506(7) . ? C2B C3B 1.378(7) . ? C3B C4B 1.403(8) . ? C3B C11B 1.494(7) . ? C4B C5B 1.391(7) . ? C5B C6B 1.393(7) . ? C5B C7B 1.545(7) . ? C7B C9B 1.517(8) . ? C7B C8B 1.549(7) . ? C7B C10B 1.549(7) . ? C12B C13B 1.503(7) . ? C13B C18B 1.391(8) . ? C13B C14B 1.414(8) . ? C14B C15B 1.406(7) . ? C15B C16B 1.391(8) . ? C15B C23B 1.496(7) . ? C16B C17B 1.393(8) . ? C17B C18B 1.401(8) . ? C17B C19B 1.538(8) . ? C19B C20C 1.64(5) . ? C19B C21B 1.536(11) . ? C19B C22C 1.58(5) . ? C19B C20B 1.555(10) . ? C19B C22B 1.585(10) . ? C24B C25B 1.492(7) . ? C25B C30B 1.394(7) . ? C25B C26B 1.422(7) . ? C26B C27B 1.382(7) . ? C27B C28B 1.395(7) . ? C27B C35B 1.509(7) . ? C28B C29B 1.392(7) . ? C29B C30B 1.401(7) . ? C29B C31B 1.543(7) . ? C31B C34B 1.525(8) . ? C31B C33B 1.534(8) . ? C31B C32B 1.545(8) . ? N1B C43B 1.491(6) . ? N1B C49B 1.499(6) . ? N1B C37B 1.510(7) . ? N2B C54B 1.459(7) . ? N2B C42B 1.460(8) . ? N2B C48B 1.467(7) . ? C37B C38B 1.495(7) . ? C39B C40B 1.495(8) . ? C41B C42B 1.518(8) . ? C43B C44B 1.515(7) . ? C45B C46B 1.505(8) . ? C47B C48B 1.506(8) . ? C49B C50B 1.516(7) . ? C51B C52B 1.499(8) . ? C53B C54B 1.513(8) . ? 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 O8A U1 O7A 178.48(16) . . ? O8A U1 O3A 93.55(14) . . ? O7A U1 O3A 87.27(15) . . ? O8A U1 O1A 94.56(14) . . ? O7A U1 O1A 85.93(15) . . ? O3A U1 O1A 127.86(14) . . ? O8A U1 O5A 89.64(14) . . ? O7A U1 O5A 88.86(15) . . ? O3A U1 O5A 113.50(14) . . ? O1A U1 O5A 117.96(14) . . ? O8A U1 O2A 70.71(14) . . ? O7A U1 O2A 110.80(14) . . ? O3A U1 O2A 66.60(12) . . ? O1A U1 O2A 67.99(12) . . ? O5A U1 O2A 160.16(12) . . ? C12A O2A C11A 113.5(4) . . ? C24A O4A C23A 114.8(4) . . ? C36A O6A C35A 115.0(4) . . ? C39A O9A C38A 112.4(4) . . ? C40A O10A C41A 113.4(5) . . ? C44A O11A C45A 114.1(4) . . ? C46A O12A C47A 113.5(4) . . ? C50A O13A C51A 110.2(4) . . ? C52A O14A C53A 111.9(4) . . ? C6A C1A C2A 118.6(5) . . ? C6A C1A C36A 123.3(5) . . ? C2A C1A C36A 117.9(5) . . ? O1A C2A C3A 119.8(5) . . ? O1A C2A C1A 119.8(5) . . ? C3A C2A C1A 120.4(5) . . ? C2A C3A C4A 118.3(5) . . ? C2A C3A C11A 119.7(5) . . ? C4A C3A C11A 121.9(5) . . ? C5A C4A C3A 123.5(5) . . ? C4A C5A C6A 116.4(5) . . ? C4A C5A C7A 122.7(5) . . ? C6A C5A C7A 120.9(5) . . ? C1A C6A C5A 122.6(5) . . ? C9A C7A C5A 113.4(5) . . ? C9A C7A C8A 108.2(5) . . ? C5A C7A C8A 108.9(5) . . ? C9A C7A C10A 109.3(5) . . ? C5A C7A C10A 109.6(5) . . ? C8A C7A C10A 107.3(5) . . ? O2A C11A C3A 106.5(4) . . ? O2A C12A C13A 109.4(4) . . ? C18A C13A C14A 120.1(5) . . ? C18A C13A C12A 121.0(5) . . ? C14A C13A C12A 118.9(5) . . ? O3A C14A C13A 120.7(5) . . ? O3A C14A C15A 120.1(5) . . ? C13A C14A C15A 119.1(5) . . ? C16A C15A C14A 119.3(5) . . ? C16A C15A C23A 123.0(5) . . ? C14A C15A C23A 117.6(5) . . ? C17A C16A C15A 122.5(5) . . ? C16A C17A C18A 116.7(5) . . ? C16A C17A C19A 123.0(5) . . ? C18A C17A C19A 120.3(5) . . ? C13A C18A C17A 122.0(5) . . ? C22A C19A C17A 109.3(4) . . ? C22A C19A C20A 109.1(5) . . ? C17A C19A C20A 109.8(4) . . ? C22A C19A C21A 107.9(4) . . ? C17A C19A C21A 112.0(5) . . ? C20A C19A C21A 108.7(5) . . ? O4A C23A C15A 106.2(4) . . ? O4A C24A C25A 105.7(4) . . ? C30A C25A C26A 119.6(5) . . ? C30A C25A C24A 122.0(5) . . ? C26A C25A C24A 118.3(5) . . ? O5A C26A C25A 121.4(5) . . ? O5A C26A C27A 120.1(5) . . ? C25A C26A C27A 118.5(5) . . ? C28A C27A C26A 120.0(5) . . ? C28A C27A C35A 121.4(5) . . ? C26A C27A C35A 118.4(5) . . ? C27A C28A C29A 122.9(5) . . ? C30A C29A C28A 115.3(5) . . ? C30A C29A C31A 123.4(5) . . ? C28A C29A C31A 121.2(5) . . ? C25A C30A C29A 123.7(5) . . ? C33A C31A C34C 130.0(9) . . ? C33A C31A C29A 114.0(7) . . ? C34C C31A C29A 115.5(7) . . ? C34C C31A C33C 113.6(8) . . ? C29A C31A C33C 109.6(7) . . ? C33A C31A C32A 112.9(9) . . ? C29A C31A C32A 110.0(6) . . ? C33C C31A C32A 140.0(8) . . ? C34C C31A C32C 103.9(8) . . ? C29A C31A C32C 107.8(6) . . ? C33C C31A C32C 105.6(8) . . ? C33A C31A C34A 106.0(8) . . ? C29A C31A C34A 108.5(6) . . ? C32A C31A C34A 104.9(7) . . ? C32C C31A C34A 143.3(8) . . ? C34C C32A C32C 120.6(14) . . ? C33A C32C C32A 103.7(11) . . ? C33C C33A C32C 135.4(14) . . ? C33A C33C C34A 121.2(13) . . ? C33C C34A C34C 104.6(10) . . ? C32A C34C C34A 132.6(14) . . ? O6A C35A C27A 106.9(4) . . ? O6A C36A C1A 106.4(4) . . ? C49A N1A C37A 112.6(4) . . ? C49A N1A C43A 113.0(4) . . ? C37A N1A C43A 112.3(4) . . ? C42A N2A C48A 111.9(5) . . ? C42A N2A C54A 109.6(5) . . ? C48A N2A C54A 111.1(5) . . ? C38A C37A N1A 110.6(5) . . ? O9A C38A C37A 107.3(4) . . ? O9A C39A C40A 107.8(5) . . ? O10A C40A C39A 106.0(5) . . ? O10A C41A C42A 112.8(6) . . ? N2A C42A C41A 114.7(6) . . ? N1A C43A C44A 107.4(4) . . ? O11A C44A C43A 107.2(4) . . ? O11A C45A C46A 106.5(4) . . ? O12A C46A C45A 106.8(5) . . ? O12A C47A C48A 111.7(5) . . ? N2A C48A C47A 114.3(5) . . ? C50A C49A N1A 109.4(4) . . ? O13A C50A C49A 107.5(5) . . ? O13A C51A C52A 111.3(5) . . ? O14A C52A C51A 109.8(5) . . ? O14A C53A C54A 107.8(5) . . ? N2A C54A C53A 113.3(5) . . ? O8B U2 O7B 176.94(16) . . ? O8B U2 O5B 91.17(14) . . ? O7B U2 O5B 88.05(15) . . ? O8B U2 O1B 97.61(14) . . ? O7B U2 O1B 85.23(15) . . ? O5B U2 O1B 125.93(13) . . ? O8B U2 O3B 90.01(14) . . ? O7B U2 O3B 87.31(15) . . ? O5B U2 O3B 104.18(13) . . ? O1B U2 O3B 128.90(13) . . ? O8B U2 O6B 70.39(14) . . ? O7B U2 O6B 112.01(14) . . ? O5B U2 O6B 68.39(11) . . ? O1B U2 O6B 65.00(12) . . ? O3B U2 O6B 158.39(12) . . ? O8B U2 O2B 70.60(14) . . ? O7B U2 O2B 109.71(14) . . ? O5B U2 O2B 160.07(12) . . ? O1B U2 O2B 66.51(12) . . ? O3B U2 O2B 68.90(12) . . ? O6B U2 O2B 110.84(10) . . ? C12B O2B C11B 116.5(4) . . ? C23B O4B C24B 114.9(4) . . ? C26B O5B U2 124.2(3) . . ? C36B O6B C35B 114.6(4) . . ? C38B O9B C39B 110.4(4) . . ? C40B O10B C41B 112.0(4) . . ? C45B O11B C44B 113.8(4) . . ? C46B O12B C47B 113.8(4) . . ? C51B O13B C50B 113.1(4) . . ? C52B O14B C53B 114.1(5) . . ? C6B C1B C2B 119.0(5) . . ? C6B C1B C36B 123.2(5) . . ? C2B C1B C36B 117.6(5) . . ? O1B C2B C3B 120.0(5) . . ? O1B C2B C1B 119.6(5) . . ? C3B C2B C1B 120.3(5) . . ? C2B C3B C4B 118.8(5) . . ? C2B C3B C11B 117.0(5) . . ? C4B C3B C11B 124.0(5) . . ? C5B C4B C3B 122.8(5) . . ? C4B C5B C6B 116.8(5) . . ? C4B C5B C7B 122.9(5) . . ? C6B C5B C7B 120.2(5) . . ? C5B C6B C1B 122.2(5) . . ? C9B C7B C5B 112.6(5) . . ? C9B C7B C8B 108.0(5) . . ? C5B C7B C8B 110.5(4) . . ? C9B C7B C10B 109.4(5) . . ? C5B C7B C10B 108.1(4) . . ? C8B C7B C10B 108.2(5) . . ? O2B C11B C3B 107.2(4) . . ? O2B C12B C13B 107.2(4) . . ? C18B C13B C14B 119.2(5) . . ? C18B C13B C12B 122.6(5) . . ? C14B C13B C12B 118.1(5) . . ? O3B C14B C15B 120.9(5) . . ? O3B C14B C13B 120.0(5) . . ? C15B C14B C13B 119.0(5) . . ? C16B C15B C14B 119.7(5) . . ? C16B C15B C23B 122.2(5) . . ? C14B C15B C23B 118.1(5) . . ? C15B C16B C17B 122.5(5) . . ? C16B C17B C18B 116.9(5) . . ? C16B C17B C19B 123.1(5) . . ? C18B C17B C19B 119.9(5) . . ? C13B C18B C17B 122.6(5) . . ? C20C C19B C21B 130(2) . . ? C20C C19B C22C 143(3) . . ? C20C C19B C17B 109(2) . . ? C21B C19B C17B 108.8(6) . . ? C22C C19B C17B 106(2) . . ? C21B C19B C20B 109.3(6) . . ? C22C C19B C20B 139(2) . . ? C17B C19B C20B 111.3(5) . . ? C21B C19B C22B 108.0(6) . . ? C17B C19B C22B 111.4(6) . . ? C20B C19B C22B 108.0(6) . . ? C17B C19B C21C 110.2(18) . . ? C22B C19B C21C 138.4(18) . . ? C20B C20C C22B 110(6) . . ? C22C C21B C21C 139(3) . . ? C21B C21C C20B 104(3) . . ? C21B C22C C22B 116(4) . . ? O4B C23B C15B 107.2(4) . . ? O4B C24B C25B 106.3(4) . . ? C30B C25B C26B 118.2(5) . . ? C30B C25B C24B 122.0(5) . . ? C26B C25B C24B 119.5(4) . . ? O5B C26B C27B 121.2(4) . . ? O5B C26B C25B 119.4(5) . . ? C27B C26B C25B 119.3(5) . . ? C26B C27B C28B 120.8(5) . . ? C26B C27B C35B 119.0(5) . . ? C28B C27B C35B 120.2(5) . . ? C29B C28B C27B 121.6(5) . . ? C28B C29B C30B 116.9(5) . . ? C28B C29B C31B 123.0(5) . . ? C30B C29B C31B 120.0(4) . . ? C25B C30B C29B 123.1(5) . . ? C34B C31B C33B 108.9(5) . . ? C34B C31B C32B 109.2(5) . . ? C33B C31B C32B 108.5(5) . . ? C34B C31B C29B 110.5(5) . . ? C33B C31B C29B 111.6(4) . . ? C32B C31B C29B 108.0(4) . . ? O6B C35B C27B 107.8(4) . . ? O6B C36B C1B 108.0(4) . . ? C43B N1B C49B 113.7(4) . . ? C43B N1B C37B 112.1(4) . . ? C49B N1B C37B 111.7(4) . . ? C54B N2B C42B 112.2(5) . . ? C54B N2B C48B 110.7(5) . . ? C42B N2B C48B 110.6(5) . . ? C38B C37B N1B 109.7(4) . . ? O9B C38B C37B 108.2(5) . . ? O9B C39B C40B 111.5(5) . . ? O10B C40B C39B 109.5(5) . . ? O10B C41B C42B 109.2(5) . . ? N2B C42B C41B 113.1(5) . . ? N1B C43B C44B 108.8(4) . . ? O11B C44B C43B 106.9(4) . . ? O11B C45B C46B 106.1(4) . . ? O12B C46B C45B 107.1(5) . . ? O12B C47B C48B 110.9(5) . . ? N2B C48B C47B 112.9(5) . . ? N1B C49B C50B 107.9(4) . . ? O13B C50B C49B 106.1(5) . . ? O13B C51B C52B 107.7(5) . . ? O14B C52B C51B 106.5(5) . . ? O14B C53B C54B 111.9(5) . . ? N2B C54B C53B 114.6(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1A O9A 0.80 2.40 2.806(6) 112.3 . N1A H1A O11A 0.80 2.22 2.712(5) 119.9 . N1A H1A O13A 0.80 2.29 2.768(6) 118.6 . N1B H1B O9B 1.01 2.23 2.801(5) 114.3 . N1B H1B O11B 1.01 2.22 2.762(6) 112.4 . N1B H1B O13B 1.01 2.20 2.722(5) 110.6 . #===END data_4 _database_code_CSD 181043 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C91 H134 N2 O24 U2' _chemical_formula_weight 2116.06 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 Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 13.4667(7) _cell_length_b 39.338(2) _cell_length_c 18.4026(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.062(4) _cell_angle_gamma 90.00 _cell_volume 9734.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 54920 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepipedic _exptl_crystal_colour 'translucent intense orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method ? _exptl_crystal_F_000 4280 _exptl_absorpt_coefficient_mu 3.392 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.351 _exptl_absorpt_correction_T_max 0.507 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _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 54920 _diffrn_reflns_av_R_equivalents 0.0880 _diffrn_reflns_av_sigmaI/netI 0.0995 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.68 _reflns_number_total 30945 _reflns_number_gt 15198 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _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 subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. Some restraints have been applied to the displacement parameters of some atoms which behave badly when treated anisotropically, possibly due to unresolved disorder (particularly in the tert-butyl groups and the chains of the cryptands) and also to some C-C and C-O distances in the cryptands. The hydrogen atoms bound to N atoms and to the O atoms of the solvent molecules have not been found on the Fourier-difference map, nor introduced. All other hydrogen atoms were introduced at calculated positions as riding atoms with an isotropic displacement parameter 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0684P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(8) _refine_ls_number_reflns 30945 _refine_ls_number_parameters 2181 _refine_ls_number_restraints 614 _refine_ls_R_factor_all 0.1815 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.2117 _refine_ls_wR_factor_gt 0.1667 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.909 _refine_diff_density_min -1.306 _refine_diff_density_rms 0.143 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 0.77457(7) 0.03274(2) 0.43353(5) 0.0422(2) Uani 1 1 d . . . O1A O 0.6310(8) 0.0603(3) 0.4372(7) 0.041(3) Uani 1 1 d . . . O2A O 0.7971(9) 0.1036(3) 0.4204(8) 0.050(4) Uani 1 1 d . . . O3A O 0.9147(10) 0.0437(4) 0.3798(6) 0.047(4) Uani 1 1 d . . . O4A O 1.0175(9) 0.0050(4) 0.5120(8) 0.053(4) Uani 1 1 d . . . O5A O 0.7831(9) -0.0191(3) 0.4817(7) 0.044(3) Uani 1 1 d . . . O6A O 0.6460(9) 0.0213(3) 0.5716(9) 0.058(4) Uani 1 1 d . . . O7A O 0.7289(10) 0.0136(3) 0.3505(7) 0.048(4) Uani 1 1 d . . . O8A O 0.8271(8) 0.0499(3) 0.5195(8) 0.046(4) Uani 1 1 d . . . C1A C 0.5674(13) 0.0752(4) 0.5519(11) 0.045(5) Uani 1 1 d D . . C2A C 0.6122(12) 0.0829(5) 0.4892(11) 0.040(5) Uani 1 1 d . . . C3A C 0.6462(13) 0.1183(5) 0.4772(11) 0.038(5) Uani 1 1 d . . . C4A C 0.6265(13) 0.1414(5) 0.5283(11) 0.043(5) Uani 1 1 d . . . H4A H 0.6474 0.1637 0.5219 0.052 Uiso 1 1 calc R . . C5A C 0.5758(13) 0.1335(5) 0.5910(11) 0.041(5) Uani 1 1 d . . . C6A C 0.5512(13) 0.1007(5) 0.6024(11) 0.039(5) Uani 1 1 d U . . H6A H 0.5224 0.0950 0.6456 0.047 Uiso 1 1 calc R . . C7A C 0.5540(16) 0.1615(6) 0.6461(14) 0.061(7) Uani 1 1 d . . . C8A C 0.5011(18) 0.1502(6) 0.7088(14) 0.081(9) Uani 1 1 d . . . H8A1 H 0.4857 0.1695 0.7381 0.121 Uiso 1 1 calc R . . H8A2 H 0.5422 0.1346 0.7372 0.121 Uiso 1 1 calc R . . H8A3 H 0.4407 0.1390 0.6924 0.121 Uiso 1 1 calc R . . C9A C 0.4871(14) 0.1895(5) 0.6080(13) 0.057(7) Uani 1 1 d . . . H9A1 H 0.4282 0.1791 0.5861 0.085 Uiso 1 1 calc R . . H9A2 H 0.5232 0.2005 0.5712 0.085 Uiso 1 1 calc R . . H9A3 H 0.4686 0.2059 0.6435 0.085 Uiso 1 1 calc R . . C10A C 0.6502(16) 0.1795(7) 0.6760(13) 0.074(8) Uani 1 1 d . . . H10A H 0.6329 0.1984 0.7059 0.112 Uiso 1 1 calc R . . H10B H 0.6868 0.1876 0.6361 0.112 Uiso 1 1 calc R . . H10C H 0.6905 0.1637 0.7045 0.112 Uiso 1 1 calc R . . C11A C 0.7084(14) 0.1239(6) 0.4121(11) 0.050(6) Uani 1 1 d . . . H11A H 0.6707 0.1175 0.3679 0.060 Uiso 1 1 calc R . . H11B H 0.7259 0.1477 0.4086 0.060 Uiso 1 1 calc R . . C12A C 0.8783(16) 0.1123(6) 0.3754(13) 0.063(7) Uani 1 1 d . . . H12A H 0.8820 0.1368 0.3712 0.075 Uiso 1 1 calc R . . H12B H 0.8644 0.1031 0.3270 0.075 Uiso 1 1 calc R . . C13A C 0.9743(12) 0.0996(5) 0.4036(9) 0.029(4) Uani 1 1 d U . . C14A C 0.9874(18) 0.0633(5) 0.4085(12) 0.052(6) Uani 1 1 d . . . C15A C 1.0762(14) 0.0510(5) 0.4456(11) 0.041(5) Uani 1 1 d . . . C16A C 1.1450(14) 0.0733(5) 0.4668(11) 0.046(5) Uani 1 1 d U . . H16A H 1.2047 0.0649 0.4871 0.056 Uiso 1 1 calc R . . C17A C 1.1358(13) 0.1077(5) 0.4614(10) 0.039(5) Uani 1 1 d . . . C18A C 1.0502(16) 0.1217(5) 0.4328(11) 0.050(6) Uani 1 1 d U . . H18A H 1.0412 0.1452 0.4322 0.060 Uiso 1 1 calc R . . C19A C 1.2180(14) 0.1328(5) 0.4899(12) 0.053(6) Uani 1 1 d DU . . C20A C 1.183(2) 0.1578(6) 0.5449(13) 0.093(9) Uani 1 1 d DU . . H20A H 1.2182 0.1541 0.5909 0.139 Uiso 1 1 calc R . . H20B H 1.1129 0.1548 0.5503 0.139 Uiso 1 1 calc R . . H20C H 1.1949 0.1806 0.5286 0.139 Uiso 1 1 calc R . . C21A C 1.3035(19) 0.1121(7) 0.5212(17) 0.113(11) Uani 1 1 d DU . . H21A H 1.3556 0.1270 0.5393 0.169 Uiso 1 1 calc R . . H21B H 1.2815 0.0983 0.5603 0.169 Uiso 1 1 calc R . . H21C H 1.3281 0.0977 0.4840 0.169 Uiso 1 1 calc R . . C22A C 1.246(2) 0.1534(8) 0.4248(18) 0.122(12) Uani 1 1 d U . . H22A H 1.3166 0.1560 0.4256 0.184 Uiso 1 1 calc R . . H22B H 1.2150 0.1754 0.4265 0.184 Uiso 1 1 calc R . . H22C H 1.2231 0.1420 0.3810 0.184 Uiso 1 1 calc R . . C23A C 1.0830(16) 0.0135(6) 0.4543(11) 0.056(6) Uani 1 1 d . . . H23A H 1.0616 0.0021 0.4093 0.067 Uiso 1 1 calc R . . H23B H 1.1509 0.0067 0.4676 0.067 Uiso 1 1 calc R . . C24A C 0.9930(15) -0.0303(5) 0.5162(13) 0.057(6) Uani 1 1 d . . . H24A H 1.0515 -0.0435 0.5312 0.069 Uiso 1 1 calc R . . H24B H 0.9676 -0.0386 0.4691 0.069 Uiso 1 1 calc R . . C25A C 0.9128(14) -0.0339(5) 0.5730(10) 0.042(5) Uani 1 1 d . . . C26A C 0.8127(15) -0.0269(5) 0.5543(11) 0.043(5) Uani 1 1 d U . . C27A C 0.7420(12) -0.0262(4) 0.6056(11) 0.034(5) Uani 1 1 d . . . C28A C 0.7717(14) -0.0329(5) 0.6774(12) 0.048(6) Uani 1 1 d . . . H28A H 0.7252 -0.0315 0.7128 0.058 Uiso 1 1 calc R . . C29A C 0.8753(15) -0.0421(5) 0.6989(11) 0.046(5) Uani 1 1 d . . . C30A C 0.9402(15) -0.0409(6) 0.6438(13) 0.056(6) Uani 1 1 d U . . H30A H 1.0071 -0.0450 0.6556 0.067 Uiso 1 1 calc R . . C31A C 0.9102(14) -0.0495(5) 0.7766(10) 0.039(5) Uani 1 1 d U . . C32A C 0.9745(15) -0.0818(5) 0.7828(11) 0.053(6) Uani 1 1 d . . . H32A H 0.9472 -0.0988 0.7500 0.080 Uiso 1 1 calc R . . H32B H 0.9754 -0.0903 0.8317 0.080 Uiso 1 1 calc R . . H32C H 1.0411 -0.0765 0.7704 0.080 Uiso 1 1 calc R . . C33A C 0.8253(16) -0.0535(6) 0.8289(13) 0.066(7) Uani 1 1 d . . . H33A H 0.7826 -0.0340 0.8250 0.100 Uiso 1 1 calc R . . H33B H 0.8528 -0.0554 0.8780 0.100 Uiso 1 1 calc R . . H33C H 0.7877 -0.0736 0.8164 0.100 Uiso 1 1 calc R . . C34A C 0.9739(14) -0.0200(5) 0.8034(10) 0.048(6) Uani 1 1 d . . . H34A H 1.0278 -0.0170 0.7720 0.072 Uiso 1 1 calc R . . H34B H 0.9999 -0.0246 0.8520 0.072 Uiso 1 1 calc R . . H34C H 0.9343 0.0003 0.8033 0.072 Uiso 1 1 calc R . . C35A C 0.6412(14) -0.0146(5) 0.5883(12) 0.047(6) Uani 1 1 d . . . H35A H 0.6124 -0.0270 0.5468 0.057 Uiso 1 1 calc R . . H35B H 0.6002 -0.0183 0.6293 0.057 Uiso 1 1 calc R . . C36A C 0.5509(13) 0.0390(4) 0.5670(13) 0.048(6) Uani 1 1 d D . . H36A H 0.5080 0.0292 0.5286 0.058 Uiso 1 1 calc R . . H36B H 0.5185 0.0366 0.6126 0.058 Uiso 1 1 calc R . . U2 U 1.05316(9) 0.20547(2) 1.18369(6) 0.0663(3) Uani 1 1 d . . . O1B O 1.2141(13) 0.2113(4) 1.1738(10) 0.091(6) Uani 1 1 d . . . O2B O 1.1476(10) 0.1423(4) 1.1913(8) 0.059(4) Uani 1 1 d . . . O3B O 0.9657(10) 0.1690(3) 1.2434(7) 0.047(4) Uani 1 1 d . . . O4B O 0.8069(12) 0.1855(4) 1.1231(9) 0.072(5) Uani 1 1 d U . . O5B O 0.9554(14) 0.2468(5) 1.1399(11) 0.093(6) Uani 1 1 d U . . O6B O 1.1182(19) 0.2413(5) 1.0365(13) 0.129(8) Uani 1 1 d . . . O7B O 1.0700(14) 0.2288(4) 1.2647(9) 0.089(6) Uani 1 1 d . . . O8B O 1.0317(12) 0.1817(4) 1.1006(8) 0.066(5) Uani 1 1 d . . . C1B C 1.273(2) 0.2092(6) 1.0549(17) 0.079(8) Uani 1 1 d . . . C2B C 1.260(2) 0.1923(8) 1.1218(17) 0.080(8) Uani 1 1 d U . . C3B C 1.2880(17) 0.1605(7) 1.1274(16) 0.071(8) Uani 1 1 d . . . C4B C 1.3354(17) 0.1438(6) 1.0750(17) 0.081(9) Uani 1 1 d . . . H4B H 1.3507 0.1208 1.0797 0.098 Uiso 1 1 calc R . . C5B C 1.360(2) 0.1617(6) 1.0152(15) 0.103(11) Uani 1 1 d D . . C6B C 1.323(2) 0.1939(8) 0.9984(18) 0.099(10) Uani 1 1 d U . . H6B H 1.3309 0.2044 0.9537 0.119 Uiso 1 1 calc R . . C7B C 1.4441(16) 0.1428(5) 0.9721(11) 0.122(12) Uani 1 1 d DU . . C8B C 1.396(2) 0.1128(5) 0.9324(16) 0.131(13) Uani 1 1 d DU . . H8B1 H 1.3359 0.1068 0.9551 0.196 Uiso 1 1 calc R . . H8B2 H 1.4409 0.0939 0.9345 0.196 Uiso 1 1 calc R . . H8B3 H 1.3806 0.1189 0.8826 0.196 Uiso 1 1 calc R . . C9B C 1.4869(17) 0.1685(6) 0.9206(13) 0.097(10) Uani 1 1 d DU . . H9B1 H 1.5378 0.1578 0.8939 0.145 Uiso 1 1 calc R . . H9B2 H 1.4351 0.1767 0.8873 0.145 Uiso 1 1 calc R . . H9B3 H 1.5151 0.1872 0.9481 0.145 Uiso 1 1 calc R . . C10B C 1.524(2) 0.1309(10) 1.0290(18) 0.08(8) Uani 1 1 d DU . . H10D H 1.5760 0.1194 1.0051 0.114 Uiso 1 1 calc R . . H10E H 1.5512 0.1502 1.0550 0.114 Uiso 1 1 calc R . . H10F H 1.4948 0.1156 1.0625 0.114 Uiso 1 1 calc R . . C11B C 1.2570(13) 0.1396(5) 1.1924(11) 0.046(5) Uani 1 1 d U . . H11C H 1.2774 0.1161 1.1877 0.055 Uiso 1 1 calc R . . H11D H 1.2869 0.1487 1.2374 0.055 Uiso 1 1 calc R . . C12B C 1.1064(15) 0.1159(7) 1.2385(12) 0.070(8) Uani 1 1 d . . . H12C H 1.1137 0.1226 1.2892 0.084 Uiso 1 1 calc R . . H12D H 1.1408 0.0944 1.2327 0.084 Uiso 1 1 calc R . . C13B C 0.9963(17) 0.1124(5) 1.2143(12) 0.050(6) Uani 1 1 d . . . C14B C 0.9361(19) 0.1396(5) 1.2166(12) 0.057(7) Uani 1 1 d . . . C15B C 0.8311(18) 0.1346(7) 1.1860(12) 0.060(7) Uani 1 1 d . . . C16B C 0.8008(15) 0.1031(6) 1.1642(12) 0.056(6) Uani 1 1 d U . . H16B H 0.7350 0.1010 1.1466 0.067 Uiso 1 1 calc R . . C17B C 0.8621(15) 0.0720(7) 1.1657(12) 0.060(7) Uani 1 1 d . . . C18B C 0.9622(13) 0.0808(6) 1.1902(13) 0.058(7) Uani 1 1 d . . . H18B H 1.0090 0.0634 1.1898 0.070 Uiso 1 1 calc R . . C19B C 0.8292(15) 0.0371(6) 1.1494(16) 0.067(8) Uani 1 1 d . . . C20B C 0.8537(16) 0.0301(6) 1.0717(17) 0.089(10) Uani 1 1 d . . . H20D H 0.8146 0.0447 1.0396 0.133 Uiso 1 1 calc R . . H20E H 0.8390 0.0068 1.0601 0.133 Uiso 1 1 calc R . . H20F H 0.9231 0.0344 1.0661 0.133 Uiso 1 1 calc R . . C21B C 0.7184(16) 0.0352(6) 1.1573(14) 0.074(7) Uani 1 1 d U . . H21D H 0.6850 0.0493 1.1210 0.111 Uiso 1 1 calc R . . H21E H 0.7030 0.0431 1.2048 0.111 Uiso 1 1 calc R . . H21F H 0.6966 0.0121 1.1510 0.111 Uiso 1 1 calc R . . C22B C 0.8832(19) 0.0112(6) 1.1995(14) 0.076(8) Uani 1 1 d . . . H22D H 0.8590 -0.0112 1.1881 0.114 Uiso 1 1 calc R . . H22E H 0.8713 0.0165 1.2493 0.114 Uiso 1 1 calc R . . H22F H 0.9533 0.0122 1.1927 0.114 Uiso 1 1 calc R . . C23B C 0.7657(16) 0.1660(6) 1.1786(13) 0.063(7) Uani 1 1 d . . . H23C H 0.6975 0.1598 1.1651 0.075 Uiso 1 1 calc R . . H23D H 0.7671 0.1786 1.2239 0.075 Uiso 1 1 calc R . . C24B C 0.757(2) 0.2178(8) 1.1140(17) 0.104(10) Uani 1 1 d U . . H24C H 0.7605 0.2301 1.1598 0.125 Uiso 1 1 calc R . . H24D H 0.6881 0.2143 1.0989 0.125 Uiso 1 1 calc R . . C25B C 0.807(2) 0.2377(7) 1.0582(17) 0.082(8) Uani 1 1 d U . . C26B C 0.903(2) 0.2474(6) 1.0749(15) 0.071(7) Uani 1 1 d U . . C27B C 0.9477(19) 0.2637(8) 1.0119(18) 0.104(10) Uani 1 1 d DU . . C28B C 0.8983(17) 0.2687(6) 0.9440(13) 0.057(6) Uani 1 1 d U . . H28B H 0.9320 0.2791 0.9071 0.069 Uiso 1 1 calc R . . C29B C 0.8048(19) 0.2590(6) 0.9305(14) 0.065(7) Uani 1 1 d U . . C30B C 0.760(2) 0.2398(8) 0.9917(19) 0.111(11) Uani 1 1 d U . . H30B H 0.6991 0.2291 0.9834 0.134 Uiso 1 1 calc R . . C31B C 0.7485(19) 0.2653(6) 0.8623(14) 0.065(7) Uani 1 1 d U . . C32B C 0.641(2) 0.2534(8) 0.8565(19) 0.128(12) Uani 1 1 d U . . H32D H 0.6386 0.2302 0.8406 0.192 Uiso 1 1 calc R . . H32E H 0.6039 0.2674 0.8221 0.192 Uiso 1 1 calc R . . H32F H 0.6131 0.2552 0.9032 0.192 Uiso 1 1 calc R . . C33B C 0.800(2) 0.2452(7) 0.7988(15) 0.094(9) Uani 1 1 d U . . H33D H 0.8677 0.2397 0.8144 0.140 Uiso 1 1 calc R . . H33E H 0.8004 0.2592 0.7561 0.140 Uiso 1 1 calc R . . H33F H 0.7643 0.2247 0.7878 0.140 Uiso 1 1 calc R . . C34B C 0.745(3) 0.3034(9) 0.843(2) 0.150(15) Uani 1 1 d U . . H34D H 0.6822 0.3127 0.8564 0.224 Uiso 1 1 calc R . . H34E H 0.7520 0.3063 0.7922 0.224 Uiso 1 1 calc R . . H34F H 0.7979 0.3150 0.8701 0.224 Uiso 1 1 calc R . . C35B C 1.0560(19) 0.2714(7) 1.0285(16) 0.091(9) Uani 1 1 d DU . . H35C H 1.0626 0.2846 1.0730 0.110 Uiso 1 1 calc R . . H35D H 1.0801 0.2853 0.9896 0.110 Uiso 1 1 calc R . . C36B C 1.226(3) 0.2460(10) 1.048(2) 0.142(14) Uani 1 1 d U . . H36C H 1.2417 0.2590 1.0920 0.171 Uiso 1 1 calc R . . H36D H 1.2527 0.2580 1.0072 0.171 Uiso 1 1 calc R . . N1 N 0.9066(10) 0.0854(4) 0.6638(9) 0.043(4) Uani 1 1 d . . . N2 N 0.9928(13) 0.1459(5) 0.9503(10) 0.055(5) Uani 1 1 d . . . O1 O 1.0778(13) 0.0697(5) 0.7434(11) 0.091(6) Uani 1 1 d U . . O2 O 1.1222(10) 0.0956(4) 0.8869(7) 0.052(4) Uani 1 1 d . . . O3 O 0.9557(13) 0.1529(4) 0.6732(9) 0.078(5) Uani 1 1 d D . . O4 O 1.0003(10) 0.1845(3) 0.8074(8) 0.048(4) Uani 1 1 d . . . O5 O 0.7790(17) 0.0757(5) 0.7820(13) 0.142(9) Uani 1 1 d DU . . O6 O 0.8081(16) 0.1021(6) 0.9184(13) 0.126(8) Uani 1 1 d U . . C1 C 0.9967(17) 0.0776(7) 0.6257(12) 0.084(9) Uani 1 1 d D . . H1A H 1.0276 0.0988 0.6123 0.101 Uiso 1 1 calc R . . H1B H 0.9777 0.0656 0.5811 0.101 Uiso 1 1 calc R . . C2 C 1.0737(16) 0.0563(6) 0.6695(11) 0.060(6) Uani 1 1 d DU . . H2A H 1.0540 0.0326 0.6692 0.072 Uiso 1 1 calc R . . H2B H 1.1382 0.0581 0.6488 0.072 Uiso 1 1 calc R . . C3 C 1.1643(16) 0.0601(5) 0.7876(11) 0.051(6) Uani 1 1 d U . . H3A H 1.2192 0.0749 0.7768 0.062 Uiso 1 1 calc R . . H3B H 1.1827 0.0370 0.7760 0.062 Uiso 1 1 calc R . . C4 C 1.146(2) 0.0624(6) 0.8656(12) 0.079(9) Uani 1 1 d . . . H4C H 1.0919 0.0473 0.8764 0.094 Uiso 1 1 calc R . . H4D H 1.2050 0.0549 0.8937 0.094 Uiso 1 1 calc R . . C5 C 1.1068(15) 0.0964(5) 0.9632(10) 0.042(5) Uani 1 1 d U . . H5A H 1.1651 0.0881 0.9910 0.051 Uiso 1 1 calc R . . H5B H 1.0500 0.0826 0.9745 0.051 Uiso 1 1 calc R . . C6 C 1.0882(14) 0.1334(4) 0.9801(10) 0.036(5) Uani 1 1 d . . . H6C H 1.0912 0.1364 1.0325 0.044 Uiso 1 1 calc R . . H6D H 1.1408 0.1469 0.9608 0.044 Uiso 1 1 calc R . . C7 C 0.840(2) 0.1102(6) 0.6239(18) 0.107(10) Uani 1 1 d DU . . H7A H 0.7834 0.1151 0.6525 0.128 Uiso 1 1 calc R . . H7B H 0.8156 0.1003 0.5781 0.128 Uiso 1 1 calc R . . C8 C 0.8955(18) 0.1431(5) 0.6093(11) 0.080(8) Uani 1 1 d D . . H8A H 0.9377 0.1398 0.5687 0.097 Uiso 1 1 calc R . . H8B H 0.8482 0.1609 0.5965 0.097 Uiso 1 1 calc R . . C9 C 0.9757(14) 0.1879(5) 0.6783(12) 0.049(6) Uani 1 1 d . . . H9A H 0.9142 0.2004 0.6832 0.059 Uiso 1 1 calc R . . H9B H 1.0057 0.1957 0.6345 0.059 Uiso 1 1 calc R . . C10 C 1.0430(17) 0.1943(6) 0.7413(12) 0.059(6) Uani 1 1 d . . . H10G H 1.1042 0.1817 0.7360 0.071 Uiso 1 1 calc R . . H10H H 1.0594 0.2183 0.7434 0.071 Uiso 1 1 calc R . . C11 C 1.048(2) 0.1930(5) 0.8727(12) 0.069(8) Uani 1 1 d . . . H11E H 1.0582 0.2174 0.8746 0.083 Uiso 1 1 calc R . . H11F H 1.1134 0.1823 0.8759 0.083 Uiso 1 1 calc R . . C12 C 0.9928(17) 0.1824(6) 0.9353(11) 0.061(7) Uani 1 1 d . . . H12E H 0.9244 0.1898 0.9272 0.073 Uiso 1 1 calc R . . H12F H 1.0203 0.1941 0.9782 0.073 Uiso 1 1 calc R . . C13 C 0.873(2) 0.0526(9) 0.679(2) 0.135(13) Uani 1 1 d DU . . H13A H 0.9213 0.0411 0.7119 0.162 Uiso 1 1 calc R . . H13B H 0.8645 0.0394 0.6351 0.162 Uiso 1 1 calc R . . C14 C 0.774(2) 0.0558(7) 0.7156(13) 0.108(10) Uani 1 1 d DU . . H14A H 0.7257 0.0661 0.6814 0.130 Uiso 1 1 calc R . . H14B H 0.7500 0.0332 0.7266 0.130 Uiso 1 1 calc R . . C15 C 0.733(4) 0.0597(10) 0.8442(16) 0.10(2) Uani 1 1 d DU . . H15A H 0.7767 0.0437 0.8698 0.118 Uiso 1 1 calc R . . H15B H 0.6702 0.0486 0.8299 0.118 Uiso 1 1 calc R . . C16 C 0.717(4) 0.0917(11) 0.888(3) 0.095(18) Uani 1 1 d DU . . H16C H 0.6887 0.1094 0.8566 0.114 Uiso 1 1 calc R . . H16D H 0.6718 0.0872 0.9259 0.114 Uiso 1 1 calc R . . C17 C 0.816(3) 0.1346(10) 0.959(2) 0.135(14) Uani 1 1 d U . . H17A H 0.7621 0.1362 0.9919 0.162 Uiso 1 1 calc R . . H17B H 0.8099 0.1535 0.9252 0.162 Uiso 1 1 calc R . . C18 C 0.9153(17) 0.1362(7) 1.0018(13) 0.069(8) Uani 1 1 d . . . H18C H 0.9128 0.1530 1.0403 0.083 Uiso 1 1 calc R . . H18D H 0.9310 0.1143 1.0238 0.083 Uiso 1 1 calc R . . U3 U 0.62205(9) 0.48043(2) 0.84129(6) 0.0686(3) Uani 1 1 d . . . O1C O 0.4876(13) 0.4498(5) 0.8386(9) 0.078(5) Uani 1 1 d . . . O2C O 0.6610(14) 0.4116(4) 0.8190(8) 0.080(5) Uani 1 1 d . . . O3C O 0.7709(13) 0.4744(3) 0.7901(8) 0.067(5) Uani 1 1 d . . . O4C O 0.8310(11) 0.5149(4) 0.9254(8) 0.062(4) Uani 1 1 d U . . O5C O 0.6035(10) 0.5304(4) 0.8972(9) 0.058(4) Uani 1 1 d . . . O6C O 0.4738(10) 0.4801(4) 0.9822(8) 0.057(4) Uani 1 1 d U . . O7C O 0.5749(13) 0.4989(4) 0.7586(10) 0.087(6) Uani 1 1 d U . . O8C O 0.6737(10) 0.4628(3) 0.9253(7) 0.048(4) Uani 1 1 d . . . C1C C 0.4205(14) 0.4261(6) 0.9445(14) 0.054(6) Uani 1 1 d . . . C2C C 0.4737(18) 0.4213(6) 0.8809(14) 0.066(7) Uani 1 1 d . . . C3C C 0.515(2) 0.3907(6) 0.8651(16) 0.070(8) Uani 1 1 d . . . C4C C 0.5023(19) 0.3637(7) 0.9109(15) 0.072(8) Uani 1 1 d . . . H4C1 H 0.5312 0.3429 0.9003 0.086 Uiso 1 1 calc R . . C5C C 0.4452(17) 0.3665(7) 0.9753(15) 0.069(7) Uani 1 1 d . . . C6C C 0.4055(16) 0.3987(7) 0.9922(15) 0.065(7) Uani 1 1 d . . . H6C1 H 0.3703 0.4017 1.0338 0.078 Uiso 1 1 calc R . . C7C C 0.4267(16) 0.3381(6) 1.0259(15) 0.082(8) Uani 1 1 d DU . . C8C C 0.3214(18) 0.3323(9) 1.0462(17) 0.126(14) Uani 1 1 d D . . H8C1 H 0.2809 0.3265 1.0035 0.189 Uiso 1 1 calc R . . H8C2 H 0.3198 0.3140 1.0807 0.189 Uiso 1 1 calc R . . H8C3 H 0.2961 0.3526 1.0675 0.189 Uiso 1 1 calc R . . C9C C 0.478(2) 0.3054(6) 1.0083(17) 0.112(11) Uani 1 1 d DU . . H9C1 H 0.4737 0.2898 1.0481 0.168 Uiso 1 1 calc R . . H9C2 H 0.5470 0.3099 1.0006 0.168 Uiso 1 1 calc R . . H9C3 H 0.4471 0.2957 0.9650 0.168 Uiso 1 1 calc R . . C10C C 0.464(3) 0.3462(10) 1.1046(16) 0.157(15) Uani 1 1 d DU . . H10I H 0.4347 0.3669 1.1202 0.235 Uiso 1 1 calc R . . H10J H 0.4466 0.3280 1.1361 0.235 Uiso 1 1 calc R . . H10K H 0.5354 0.3487 1.1065 0.235 Uiso 1 1 calc R . . C11C C 0.576(2) 0.3878(6) 0.8021(13) 0.064(6) Uani 1 1 d . . . H11G H 0.5392 0.3946 0.7579 0.077 Uiso 1 1 calc R . . H11H H 0.6000 0.3647 0.7965 0.077 Uiso 1 1 calc R . . C12C C 0.750(2) 0.4033(6) 0.7795(13) 0.079(9) Uani 1 1 d . . . H12G H 0.7445 0.4124 0.7304 0.095 Uiso 1 1 calc R . . H12H H 0.7593 0.3789 0.7770 0.095 Uiso 1 1 calc R . . C13C C 0.8348(19) 0.4199(6) 0.8235(13) 0.060(7) Uani 1 1 d . . . C14C C 0.8438(19) 0.4565(6) 0.8295(14) 0.057(6) Uani 1 1 d . . . C15C C 0.9160(18) 0.4713(6) 0.8686(16) 0.065(8) Uani 1 1 d . . . C16C C 0.9870(19) 0.4539(7) 0.9075(17) 0.083(9) Uani 1 1 d . . . H16E H 1.0337 0.4651 0.9379 0.100 Uiso 1 1 calc R . . C17C C 0.988(2) 0.4170(7) 0.9001(15) 0.079(8) Uani 1 1 d U . . C18C C 0.9102(17) 0.4016(6) 0.8568(13) 0.063(6) Uani 1 1 d U . . H18E H 0.9107 0.3781 0.8508 0.076 Uiso 1 1 calc R . . C19C C 1.0686(2) 0.3971(4) 0.9424(8) 0.072(7) Uani 1 1 d U . . C20C C 1.1317(19) 0.3813(7) 0.8847(12) 0.138(13) Uani 1 1 d U . . H20G H 1.1823 0.3672 0.9079 0.208 Uiso 1 1 calc R . . H20H H 1.0901 0.3677 0.8522 0.208 Uiso 1 1 calc R . . H20I H 1.1623 0.3989 0.8577 0.208 Uiso 1 1 calc R . . C21C C 1.1346(17) 0.4186(6) 0.9951(12) 0.118(12) Uani 1 1 d U . . H21G H 1.1836 0.4043 1.0195 0.177 Uiso 1 1 calc R . . H21H H 1.0943 0.4290 1.0304 0.177 Uiso 1 1 calc R . . H21I H 1.1672 0.4359 0.9684 0.177 Uiso 1 1 calc R . . C22C C 1.0193(17) 0.3688(5) 0.9848(12) 0.094(10) Uani 1 1 d . . . H22G H 0.9635 0.3600 0.9562 0.140 Uiso 1 1 calc R . . H22H H 0.9970 0.3778 1.0296 0.140 Uiso 1 1 calc R . . H22I H 1.0665 0.3510 0.9952 0.140 Uiso 1 1 calc R . . C23C C 0.9113(15) 0.5103(5) 0.8787(12) 0.056(6) Uani 1 1 d U . . H23E H 0.9731 0.5189 0.9011 0.067 Uiso 1 1 calc R . . H23F H 0.8980 0.5216 0.8324 0.067 Uiso 1 1 calc R . . C24C C 0.7990(17) 0.5486(6) 0.9337(14) 0.073(8) Uani 1 1 d . . . H24E H 0.7693 0.5572 0.8882 0.087 Uiso 1 1 calc R . . H24F H 0.8546 0.5631 0.9489 0.087 Uiso 1 1 calc R . . C25C C 0.7235(16) 0.5479(7) 0.9912(13) 0.067(8) Uani 1 1 d . . . C26C C 0.6269(18) 0.5370(6) 0.9679(14) 0.061(7) Uani 1 1 d . . . C27C C 0.5563(13) 0.5307(4) 1.0211(11) 0.036(4) Uani 1 1 d U . . C28C C 0.5866(15) 0.5350(6) 1.0959(13) 0.052(6) Uani 1 1 d . . . H28C H 0.5428 0.5291 1.1312 0.063 Uiso 1 1 calc R . . C29C C 0.6828(15) 0.5480(5) 1.1181(11) 0.044(5) Uani 1 1 d . . . C30C C 0.7507(18) 0.5530(5) 1.0629(12) 0.052(6) Uani 1 1 d . . . H30C H 0.8153 0.5599 1.0757 0.062 Uiso 1 1 calc R . . C31C C 0.7123(19) 0.5526(6) 1.1992(14) 0.065(7) Uani 1 1 d . . . C32C C 0.8015(17) 0.5268(6) 1.2191(14) 0.070(7) Uani 1 1 d . . . H32G H 0.8195 0.5283 1.2702 0.105 Uiso 1 1 calc R . . H32H H 0.8578 0.5326 1.1917 0.105 Uiso 1 1 calc R . . H32I H 0.7806 0.5041 1.2073 0.105 Uiso 1 1 calc R . . C33C C 0.6364(17) 0.5465(6) 1.2505(13) 0.063(7) Uani 1 1 d . . . H33G H 0.5814 0.5615 1.2403 0.095 Uiso 1 1 calc R . . H33H H 0.6141 0.5233 1.2462 0.095 Uiso 1 1 calc R . . H33I H 0.6636 0.5504 1.2991 0.095 Uiso 1 1 calc R . . C34C C 0.7559(19) 0.5884(6) 1.2121(16) 0.084(9) Uani 1 1 d . . . H34G H 0.7030 0.6042 1.2190 0.127 Uiso 1 1 calc R . . H34H H 0.7917 0.5952 1.1707 0.127 Uiso 1 1 calc R . . H34I H 0.8004 0.5882 1.2547 0.127 Uiso 1 1 calc R . . C35C C 0.4580(15) 0.5144(5) 0.9991(13) 0.058(7) Uani 1 1 d . . . H35E H 0.4133 0.5162 1.0385 0.070 Uiso 1 1 calc R . . H35F H 0.4278 0.5261 0.9570 0.070 Uiso 1 1 calc R . . C36C C 0.3876(17) 0.4608(6) 0.9644(15) 0.073(8) Uani 1 1 d . . . H36E H 0.3498 0.4711 0.9238 0.088 Uiso 1 1 calc R . . H36F H 0.3458 0.4597 1.0056 0.088 Uiso 1 1 calc R . . U4 U 0.90238(7) 0.28672(2) 1.59222(6) 0.0539(3) Uani 1 1 d . . . O1D O 0.8394(14) 0.3272(4) 1.6582(10) 0.080(6) Uani 1 1 d . . . O2D O 0.9927(11) 0.3564(4) 1.5717(8) 0.060(4) Uani 1 1 d . . . O3D O 1.0629(11) 0.2870(4) 1.5626(8) 0.062(4) Uani 1 1 d . . . O4D O 0.9447(11) 0.2472(4) 1.4494(9) 0.059(4) Uani 1 1 d . . . O5D O 0.8125(13) 0.2407(4) 1.5690(8) 0.072(5) Uani 1 1 d . . . O6D O 0.6540(13) 0.3010(5) 1.5750(10) 0.091(6) Uani 1 1 d U . . O7D O 0.9511(11) 0.2667(4) 1.6747(8) 0.064(4) Uani 1 1 d . . . O8D O 0.8510(9) 0.3078(3) 1.5114(7) 0.046(4) Uani 1 1 d . . . C1D C 0.6893(19) 0.3546(5) 1.6220(13) 0.055(6) Uani 1 1 d . . . C2D C 0.792(2) 0.3541(6) 1.6345(12) 0.055(6) Uani 1 1 d . . . C3D C 0.8530(16) 0.3833(5) 1.6128(11) 0.044(6) Uani 1 1 d . . . C4D C 0.8048(19) 0.4122(6) 1.5834(13) 0.068(8) Uani 1 1 d . . . H4D1 H 0.8426 0.4304 1.5679 0.081 Uiso 1 1 calc R . . C5D C 0.7019(18) 0.4143(6) 1.5770(13) 0.065(7) Uani 1 1 d . . . C6D C 0.6430(17) 0.3838(6) 1.5918(12) 0.055(6) Uani 1 1 d . . . H6D1 H 0.5747 0.3838 1.5811 0.066 Uiso 1 1 calc R . . C7D C 0.6480(16) 0.4463(6) 1.5471(16) 0.072(9) Uani 1 1 d . . . C8D C 0.677(2) 0.4525(8) 1.4700(15) 0.100(10) Uani 1 1 d . . . H8D1 H 0.7476 0.4558 1.4696 0.150 Uiso 1 1 calc R . . H8D2 H 0.6436 0.4725 1.4510 0.150 Uiso 1 1 calc R . . H8D3 H 0.6581 0.4333 1.4403 0.150 Uiso 1 1 calc R . . C9D C 0.5366(18) 0.4472(9) 1.556(2) 0.139(16) Uani 1 1 d . . . H9D1 H 0.5088 0.4252 1.5452 0.209 Uiso 1 1 calc R . . H9D2 H 0.5067 0.4636 1.5227 0.209 Uiso 1 1 calc R . . H9D3 H 0.5237 0.4535 1.6048 0.209 Uiso 1 1 calc R . . C10D C 0.693(2) 0.4767(7) 1.5991(17) 0.100(10) Uani 1 1 d U . . H10L H 0.7620 0.4721 1.6119 0.150 Uiso 1 1 calc R . . H10M H 0.6568 0.4779 1.6425 0.150 Uiso 1 1 calc R . . H10N H 0.6875 0.4979 1.5735 0.150 Uiso 1 1 calc R . . C11D C 0.9645(16) 0.3804(6) 1.6225(13) 0.060(6) Uani 1 1 d . . . H11I H 0.9957 0.4021 1.6139 0.072 Uiso 1 1 calc R . . H11J H 0.9839 0.3729 1.6715 0.072 Uiso 1 1 calc R . . C12D C 1.098(2) 0.3554(7) 1.5593(14) 0.085(9) Uani 1 1 d . . . H12I H 1.1340 0.3461 1.6018 0.102 Uiso 1 1 calc R . . H12J H 1.1220 0.3783 1.5516 0.102 Uiso 1 1 calc R . . C13D C 1.1168(14) 0.3338(5) 1.4937(10) 0.038(5) Uani 1 1 d . . . C14D C 1.0918(14) 0.3001(5) 1.5014(13) 0.051(6) Uani 1 1 d . . . C15D C 1.0881(16) 0.2791(5) 1.4380(11) 0.046(5) Uani 1 1 d U . . C16D C 1.1315(14) 0.2912(5) 1.3734(10) 0.046(5) Uani 1 1 d . . . H16F H 1.1364 0.2774 1.3327 0.055 Uiso 1 1 calc R . . C17D C 1.1676(16) 0.3262(5) 1.3744(11) 0.051(6) Uani 1 1 d . . . C18D C 1.1536(16) 0.3475(6) 1.4356(13) 0.059(7) Uani 1 1 d . . . H18F H 1.1700 0.3704 1.4346 0.071 Uiso 1 1 calc R . . C19D C 1.2116(17) 0.3383(7) 1.3005(15) 0.073(7) Uani 1 1 d DU . . C20D C 1.217(3) 0.3785(10) 1.298(2) 0.175(17) Uani 1 1 d U . . H20J H 1.1503 0.3875 1.2930 0.263 Uiso 1 1 calc R . . H20K H 1.2530 0.3854 1.2569 0.263 Uiso 1 1 calc R . . H20L H 1.2492 0.3868 1.3419 0.263 Uiso 1 1 calc R . . C21D C 1.141(3) 0.3286(9) 1.236(2) 0.146(15) Uani 1 1 d U . . H21J H 1.0958 0.3471 1.2247 0.219 Uiso 1 1 calc R . . H21K H 1.1039 0.3087 1.2473 0.219 Uiso 1 1 calc R . . H21L H 1.1788 0.3241 1.1939 0.219 Uiso 1 1 calc R . . C22D C 1.308(2) 0.3201(10) 1.282(2) 0.164(16) Uani 1 1 d DU . . H22J H 1.3357 0.3307 1.2410 0.246 Uiso 1 1 calc R . . H22K H 1.2943 0.2967 1.2715 0.246 Uiso 1 1 calc R . . H22L H 1.3553 0.3215 1.3234 0.246 Uiso 1 1 calc R . . C23D C 1.0482(14) 0.2449(5) 1.4428(11) 0.042(5) Uani 1 1 d . . . H23G H 1.0623 0.2321 1.3996 0.050 Uiso 1 1 calc R . . H23H H 1.0788 0.2333 1.4848 0.050 Uiso 1 1 calc R . . C24D C 0.8832(19) 0.2162(6) 1.4402(14) 0.076(7) Uani 1 1 d U . . H24G H 0.8944 0.2059 1.3934 0.091 Uiso 1 1 calc R . . H24H H 0.9028 0.1999 1.4779 0.091 Uiso 1 1 calc R . . C25D C 0.7788(17) 0.2241(5) 1.4443(16) 0.059(7) Uani 1 1 d . . . C26D C 0.7477(15) 0.2386(6) 1.5092(13) 0.049(6) Uani 1 1 d . . . C27D C 0.652(2) 0.2480(6) 1.5136(13) 0.062(7) Uani 1 1 d . . . C28D C 0.5827(15) 0.2434(5) 1.4527(13) 0.053(6) Uani 1 1 d . . . H28D H 0.5166 0.2499 1.4554 0.063 Uiso 1 1 calc R . . C29D C 0.6151(14) 0.2296(6) 1.3916(13) 0.052(6) Uani 1 1 d . . . C30D C 0.7127(18) 0.2192(5) 1.3857(14) 0.058(7) Uani 1 1 d . . . H30D H 0.7330 0.2092 1.3431 0.069 Uiso 1 1 calc R . . C31D C 0.5414(15) 0.2220(6) 1.3217(15) 0.063(7) Uani 1 1 d . . . C32D C 0.5715(18) 0.2451(7) 1.2581(13) 0.074(8) Uani 1 1 d U . . H32J H 0.6385 0.2399 1.2465 0.111 Uiso 1 1 calc R . . H32K H 0.5672 0.2685 1.2723 0.111 Uiso 1 1 calc R . . H32L H 0.5275 0.2410 1.2163 0.111 Uiso 1 1 calc R . . C33D C 0.5424(18) 0.1851(5) 1.2985(13) 0.068(7) Uani 1 1 d . . . H33J H 0.4991 0.1821 1.2558 0.101 Uiso 1 1 calc R . . H33K H 0.5198 0.1711 1.3370 0.101 Uiso 1 1 calc R . . H33L H 0.6088 0.1786 1.2879 0.101 Uiso 1 1 calc R . . C34D C 0.4303(17) 0.2321(7) 1.3361(15) 0.080(8) Uani 1 1 d . . . H34J H 0.3945 0.2365 1.2906 0.120 Uiso 1 1 calc R . . H34K H 0.4300 0.2521 1.3659 0.120 Uiso 1 1 calc R . . H34L H 0.3990 0.2137 1.3606 0.120 Uiso 1 1 calc R . . C35D C 0.6199(17) 0.2664(6) 1.5841(13) 0.065(7) Uani 1 1 d U . . H35G H 0.5483 0.2657 1.5875 0.078 Uiso 1 1 calc R . . H35H H 0.6513 0.2562 1.6274 0.078 Uiso 1 1 calc R . . C36D C 0.638(2) 0.3225(6) 1.6344(13) 0.070(7) Uani 1 1 d . . . H36G H 0.6633 0.3121 1.6794 0.083 Uiso 1 1 calc R . . H36H H 0.5670 0.3265 1.6380 0.083 Uiso 1 1 calc R . . N3 N 0.7290(10) 0.4251(4) 1.0696(9) 0.040(4) Uani 1 1 d DU . . N4 N 0.7988(11) 0.3446(5) 1.3634(10) 0.048(5) Uani 1 1 d . . . O7 O 0.618(2) 0.4209(7) 1.1976(15) 0.149(9) Uani 1 1 d U . . O8 O 0.6356(14) 0.3853(5) 1.3307(11) 0.098(6) Uani 1 1 d U . . O9 O 0.8824(18) 0.4377(7) 1.1698(15) 0.141(9) Uani 1 1 d U . . O10 O 0.9166(14) 0.3975(5) 1.3044(11) 0.093(6) Uani 1 1 d U . . O11 O 0.7736(17) 0.3605(6) 1.0913(13) 0.125(8) Uani 1 1 d U . . O12 O 0.8224(17) 0.3206(6) 1.2258(13) 0.121(7) Uani 1 1 d U . . C19 C 0.640(2) 0.4506(7) 1.0794(14) 0.170(16) Uani 1 1 d DU . . H19A H 0.6654 0.4736 1.0817 0.205 Uiso 1 1 calc R . . H19B H 0.5938 0.4490 1.0370 0.205 Uiso 1 1 calc R . . C20 C 0.5849(19) 0.4440(7) 1.1448(12) 0.074(8) Uani 1 1 d D . . H20M H 0.5780 0.4657 1.1690 0.089 Uiso 1 1 calc R . . H20N H 0.5184 0.4370 1.1282 0.089 Uiso 1 1 calc R . . C21 C 0.566(2) 0.4239(8) 1.2652(19) 0.118(12) Uani 1 1 d DU . . H21M H 0.6072 0.4364 1.3006 0.142 Uiso 1 1 calc R . . H21N H 0.5052 0.4370 1.2556 0.142 Uiso 1 1 calc R . . C22 C 0.539(3) 0.3905(9) 1.297(2) 0.150(15) Uani 1 1 d DU . . H22M H 0.5207 0.3735 1.2606 0.180 Uiso 1 1 calc R . . H22N H 0.4874 0.3923 1.3320 0.180 Uiso 1 1 calc R . . C23 C 0.6198(18) 0.3563(7) 1.3768(14) 0.083(8) Uani 1 1 d DU . . H23I H 0.6084 0.3357 1.3487 0.099 Uiso 1 1 calc R . . H23J H 0.5650 0.3599 1.4081 0.099 Uiso 1 1 calc R . . C24 C 0.7201(18) 0.3556(9) 1.4200(16) 0.112(11) Uani 1 1 d DU . . H24I H 0.7190 0.3394 1.4596 0.134 Uiso 1 1 calc R . . H24J H 0.7362 0.3779 1.4398 0.134 Uiso 1 1 calc R . . C25 C 0.8185(17) 0.4466(9) 1.0498(17) 0.186(19) Uani 1 1 d DU . . H25A H 0.8470 0.4362 1.0079 0.223 Uiso 1 1 calc R . . H25B H 0.7940 0.4688 1.0347 0.223 Uiso 1 1 calc R . . C26 C 0.8991(15) 0.4517(6) 1.1056(12) 0.057(6) Uani 1 1 d DU . . H26A H 0.9599 0.4423 1.0881 0.069 Uiso 1 1 calc R . . H26B H 0.9094 0.4759 1.1125 0.069 Uiso 1 1 calc R . . C27 C 0.9718(19) 0.4304(7) 1.2078(15) 0.075(8) Uani 1 1 d U . . H27A H 1.0224 0.4472 1.1983 0.090 Uiso 1 1 calc R . . H27B H 0.9960 0.4080 1.1961 0.090 Uiso 1 1 calc R . . C28 C 0.942(2) 0.4322(7) 1.2826(16) 0.089(10) Uani 1 1 d . . . H28E H 0.8852 0.4472 1.2859 0.106 Uiso 1 1 calc R . . H28F H 0.9963 0.4410 1.3141 0.106 Uiso 1 1 calc R . . C29 C 0.9125(19) 0.3943(5) 1.3817(12) 0.063(7) Uani 1 1 d . . . H29A H 0.8583 0.4075 1.3999 0.076 Uiso 1 1 calc R . . H29B H 0.9745 0.4013 1.4066 0.076 Uiso 1 1 calc R . . C30 C 0.895(2) 0.3573(8) 1.3894(18) 0.100(10) Uani 1 1 d U . . H30E H 0.9456 0.3453 1.3636 0.120 Uiso 1 1 calc R . . H30F H 0.9048 0.3514 1.4405 0.120 Uiso 1 1 calc R . . C31 C 0.701(3) 0.4008(5) 1.0136(17) 0.083(18) Uani 1 1 d DU . . H31A H 0.7192 0.4100 0.9673 0.099 Uiso 1 1 calc R . . H31B H 0.6295 0.3983 1.0117 0.099 Uiso 1 1 calc R . . C32 C 0.7450(19) 0.3677(6) 1.0221(12) 0.068(7) Uani 1 1 d D . . H32M H 0.8022 0.3663 0.9924 0.082 Uiso 1 1 calc R . . H32N H 0.6971 0.3508 1.0044 0.082 Uiso 1 1 calc R . . C33 C 0.796(2) 0.3232(8) 1.1005(17) 0.101(10) Uani 1 1 d U . . H33M H 0.8199 0.3132 1.0565 0.121 Uiso 1 1 calc R . . H33N H 0.7391 0.3105 1.1158 0.121 Uiso 1 1 calc R . . C34 C 0.881(2) 0.3255(8) 1.163(2) 0.115(13) Uani 1 1 d . . . H34M H 0.9306 0.3077 1.1589 0.137 Uiso 1 1 calc R . . H34N H 0.9138 0.3475 1.1639 0.137 Uiso 1 1 calc R . . C35 C 0.863(2) 0.3000(7) 1.2813(15) 0.088(9) Uani 1 1 d U . . H35I H 0.9347 0.3034 1.2865 0.105 Uiso 1 1 calc R . . H35J H 0.8510 0.2762 1.2696 0.105 Uiso 1 1 calc R . . C36 C 0.816(2) 0.3090(9) 1.3506(19) 0.115(12) Uani 1 1 d U . . H36I H 0.7533 0.2971 1.3515 0.138 Uiso 1 1 calc R . . H36J H 0.8586 0.3003 1.3908 0.138 Uiso 1 1 calc R . . O13 O 0.8647(15) 0.5188(5) 0.6917(11) 0.103(7) Uani 1 1 d U . . C37 C 0.801(2) 0.5489(8) 0.6877(18) 0.115(11) Uani 1 1 d U . . H37A H 0.8051 0.5604 0.7338 0.173 Uiso 1 1 calc R . . H37B H 0.7337 0.5422 0.6760 0.173 Uiso 1 1 calc R . . H37C H 0.8232 0.5639 0.6507 0.173 Uiso 1 1 calc R . . O14 O 1.199(3) 0.2667(11) 1.671(2) 0.107(13) Uani 1 1 d DU . . C38 C 1.265(3) 0.2549(13) 1.617(2) 0.092(18) Uani 1 1 d DU . . H38A H 1.2311 0.2553 1.5703 0.137 Uiso 1 1 calc R . . H38B H 1.2861 0.2321 1.6289 0.137 Uiso 1 1 calc R . . H38C H 1.3223 0.2695 1.6172 0.137 Uiso 1 1 calc R . . O15 O 0.9384(15) 0.1180(6) 0.8037(12) 0.113(7) Uani 1 1 d U . . O16 O 0.986(3) 0.3231(12) 1.800(3) 0.139(17) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0376(4) 0.0479(5) 0.0406(5) 0.0025(4) -0.0021(3) -0.0025(4) O1A 0.017(7) 0.065(9) 0.040(9) 0.002(7) -0.007(6) 0.004(6) O2A 0.028(8) 0.062(9) 0.059(10) 0.028(8) -0.001(7) -0.008(6) O3A 0.060(9) 0.070(10) 0.011(7) 0.008(6) 0.009(7) -0.001(8) O4A 0.040(8) 0.072(11) 0.048(10) 0.008(8) 0.014(7) -0.003(7) O5A 0.033(8) 0.049(8) 0.050(10) -0.004(7) 0.005(7) -0.012(6) O6A 0.034(8) 0.038(8) 0.104(14) 0.001(8) 0.013(8) -0.009(6) O7A 0.059(9) 0.056(9) 0.028(8) -0.012(7) -0.012(7) -0.008(7) O8A 0.023(7) 0.049(9) 0.063(10) -0.009(7) -0.011(7) -0.013(6) C1A 0.017(10) 0.068(15) 0.050(15) -0.011(11) 0.005(10) -0.001(9) C2A 0.019(10) 0.051(13) 0.050(14) -0.023(10) 0.007(10) 0.001(9) C3A 0.026(11) 0.048(13) 0.039(13) 0.014(10) 0.001(9) 0.002(9) C4A 0.027(11) 0.056(13) 0.045(14) 0.013(11) -0.007(10) -0.016(10) C5A 0.025(11) 0.049(13) 0.049(14) -0.003(10) 0.005(10) -0.002(9) C6A 0.025(8) 0.045(8) 0.047(9) -0.007(7) -0.009(7) 0.000(7) C7A 0.050(14) 0.060(15) 0.078(19) 0.010(13) 0.031(13) -0.004(12) C8A 0.090(19) 0.048(15) 0.11(2) -0.013(14) 0.054(17) -0.013(13) C9A 0.031(12) 0.037(12) 0.10(2) 0.001(12) -0.003(13) 0.014(10) C10A 0.065(17) 0.09(2) 0.063(19) -0.011(15) -0.017(14) -0.023(15) C11A 0.038(13) 0.069(15) 0.041(14) 0.017(11) -0.008(11) 0.009(11) C12A 0.066(17) 0.058(15) 0.066(18) -0.013(12) 0.032(14) -0.021(12) C13A 0.023(7) 0.043(8) 0.020(7) -0.005(6) -0.003(6) -0.008(6) C14A 0.076(17) 0.043(13) 0.041(14) -0.004(10) 0.028(13) -0.018(12) C15A 0.023(11) 0.051(13) 0.050(14) -0.020(10) 0.005(10) -0.001(9) C16A 0.032(8) 0.056(9) 0.053(9) -0.001(7) 0.017(7) 0.005(7) C17A 0.019(10) 0.070(14) 0.027(12) -0.008(10) 0.013(9) -0.002(9) C18A 0.055(9) 0.051(9) 0.047(9) 0.013(7) 0.020(8) -0.005(8) C19A 0.042(8) 0.057(9) 0.061(10) -0.005(8) 0.015(8) 0.009(7) C20A 0.091(12) 0.101(12) 0.087(12) -0.012(9) 0.001(9) 0.002(9) C21A 0.110(14) 0.110(14) 0.116(14) -0.008(9) -0.011(9) 0.004(9) C22A 0.125(15) 0.120(15) 0.121(15) 0.001(10) -0.002(10) -0.007(9) C23A 0.065(16) 0.080(17) 0.025(13) 0.004(11) 0.021(11) 0.008(13) C24A 0.049(13) 0.030(11) 0.092(19) 0.025(12) -0.008(13) 0.009(10) C25A 0.040(12) 0.053(12) 0.033(13) 0.013(9) 0.009(10) 0.013(10) C26A 0.046(9) 0.039(8) 0.044(9) 0.025(7) 0.002(7) -0.009(7) C27A 0.019(10) 0.039(11) 0.045(13) 0.014(9) 0.002(9) 0.007(8) C28A 0.036(12) 0.065(14) 0.046(14) 0.011(11) 0.011(11) -0.001(11) C29A 0.041(12) 0.056(14) 0.039(14) 0.004(10) -0.003(11) -0.001(10) C30A 0.036(8) 0.064(10) 0.069(10) 0.001(8) 0.002(8) 0.009(7) C31A 0.036(8) 0.044(8) 0.036(8) 0.015(7) -0.008(7) 0.001(7) C32A 0.055(14) 0.058(14) 0.045(14) 0.017(11) -0.013(12) -0.001(11) C33A 0.057(15) 0.077(17) 0.065(18) 0.014(14) -0.002(13) -0.014(13) C34A 0.042(12) 0.081(16) 0.020(12) -0.002(10) -0.006(10) -0.020(11) C35A 0.036(12) 0.058(14) 0.048(14) 0.017(11) 0.006(10) -0.017(10) C36A 0.019(10) 0.044(13) 0.081(18) 0.003(11) -0.004(11) 0.007(9) U2 0.1014(8) 0.0431(5) 0.0568(7) -0.0057(5) 0.0265(6) -0.0062(5) O1B 0.107(14) 0.065(12) 0.104(16) -0.038(11) 0.033(12) -0.025(10) O2B 0.041(9) 0.060(10) 0.076(12) 0.025(8) 0.005(8) -0.019(7) O3B 0.056(9) 0.057(9) 0.027(8) 0.004(7) -0.009(7) 0.002(7) O4B 0.079(8) 0.074(8) 0.065(8) 0.013(7) 0.019(7) 0.036(7) O5B 0.111(9) 0.073(9) 0.097(10) -0.004(8) 0.011(8) 0.019(7) O6B 0.18(2) 0.049(12) 0.16(2) 0.003(13) 0.032(18) 0.004(14) O7B 0.143(16) 0.052(10) 0.073(13) -0.032(9) 0.029(12) -0.031(11) O8B 0.099(12) 0.048(9) 0.052(11) -0.016(8) 0.021(9) 0.030(9) C1B 0.11(2) 0.022(12) 0.10(2) -0.011(13) 0.016(19) -0.005(13) C2B 0.073(11) 0.080(11) 0.088(12) 0.003(9) 0.006(9) -0.025(9) C3B 0.047(15) 0.061(17) 0.10(2) -0.003(15) -0.020(15) -0.013(13) C4B 0.058(17) 0.052(16) 0.14(3) 0.005(17) 0.045(18) -0.012(13) C5B 0.10(2) 0.068(19) 0.15(3) 0.012(19) 0.06(2) 0.013(18) C6B 0.103(12) 0.094(12) 0.101(13) 0.002(9) 0.017(9) -0.014(9) C7B 0.125(14) 0.125(14) 0.117(14) 0.002(10) 0.020(10) -0.001(10) C8B 0.130(15) 0.139(16) 0.125(15) -0.008(10) 0.021(10) -0.003(10) C9B 0.096(12) 0.096(12) 0.098(13) -0.002(9) 0.012(9) -0.002(9) C10B 0.08(8) 0.08(8) 0.08(8) 0.001(10) 0.003(11) 0.000(10) C11B 0.037(8) 0.054(9) 0.047(9) 0.004(7) -0.008(7) -0.013(7) C12B 0.033(13) 0.12(2) 0.052(17) 0.034(15) 0.002(12) -0.024(13) C13B 0.066(16) 0.030(11) 0.053(15) 0.002(10) -0.006(12) 0.009(11) C14B 0.082(18) 0.043(13) 0.048(15) -0.013(11) 0.029(13) 0.015(12) C15B 0.054(16) 0.093(19) 0.037(15) -0.009(13) 0.026(12) 0.017(14) C16B 0.033(8) 0.070(10) 0.065(10) -0.005(8) 0.013(8) 0.002(8) C17B 0.032(13) 0.09(2) 0.056(16) -0.006(13) 0.006(12) -0.022(12) C18B 0.017(11) 0.055(14) 0.10(2) 0.014(13) 0.015(12) 0.000(10) C19B 0.040(13) 0.042(14) 0.12(2) -0.043(15) 0.027(15) -0.019(11) C20B 0.036(13) 0.072(19) 0.16(3) -0.010(19) 0.011(17) -0.018(13) C21B 0.054(10) 0.079(11) 0.091(11) -0.008(9) 0.017(8) 0.000(8) C22B 0.079(19) 0.068(17) 0.08(2) -0.017(15) 0.024(16) -0.001(15) C23B 0.059(15) 0.069(16) 0.062(17) 0.012(13) 0.019(13) 0.000(12) C24B 0.109(13) 0.103(13) 0.102(13) 0.006(9) 0.018(9) 0.020(9) C25B 0.086(11) 0.077(11) 0.084(12) -0.008(9) 0.008(9) 0.016(9) C26B 0.085(11) 0.058(10) 0.072(11) -0.005(8) 0.007(9) 0.015(8) C27B 0.115(13) 0.097(13) 0.099(13) -0.006(9) 0.000(9) 0.006(9) C28B 0.068(10) 0.050(9) 0.054(10) -0.002(8) 0.005(8) 0.022(8) C29B 0.081(11) 0.053(9) 0.064(10) -0.008(8) 0.018(9) 0.016(8) C30B 0.115(13) 0.110(14) 0.111(14) 0.006(9) 0.015(9) 0.003(9) C31B 0.073(10) 0.055(10) 0.067(10) -0.009(8) 0.008(8) 0.017(8) C32B 0.129(14) 0.128(15) 0.128(15) 0.006(10) 0.006(10) 0.012(10) C33B 0.093(12) 0.095(12) 0.094(12) 0.000(9) 0.017(9) 0.002(9) C34B 0.153(17) 0.147(17) 0.148(17) 0.001(10) 0.006(10) -0.001(10) C35B 0.102(12) 0.076(11) 0.096(12) 0.002(9) 0.006(9) 0.000(9) C36B 0.144(16) 0.136(17) 0.148(17) 0.007(10) 0.009(10) -0.008(10) N1 0.016(8) 0.050(11) 0.063(12) 0.005(9) 0.015(8) -0.001(7) N2 0.059(12) 0.063(13) 0.042(12) 0.015(9) 0.014(10) 0.015(10) O1 0.087(9) 0.099(9) 0.087(9) -0.027(8) -0.013(8) 0.020(8) O2 0.061(10) 0.058(10) 0.037(9) -0.009(7) 0.007(8) 0.003(7) O3 0.128(15) 0.033(9) 0.069(12) -0.017(8) -0.038(11) 0.021(9) O4 0.055(9) 0.038(8) 0.052(10) 0.001(7) 0.026(8) -0.011(7) O5 0.139(11) 0.153(12) 0.134(12) -0.008(9) 0.019(9) -0.003(9) O6 0.118(11) 0.140(11) 0.119(11) -0.026(9) 0.005(9) -0.001(9) C1 0.083(19) 0.12(2) 0.055(18) -0.016(15) 0.005(15) 0.040(17) C2 0.057(10) 0.073(10) 0.050(10) -0.018(8) 0.000(8) 0.013(8) C3 0.053(9) 0.047(9) 0.053(9) 0.008(7) -0.014(8) 0.016(7) C4 0.13(2) 0.068(17) 0.044(16) -0.015(12) 0.034(16) 0.019(16) C5 0.049(9) 0.049(9) 0.029(8) -0.001(7) 0.004(7) -0.011(7) C6 0.044(12) 0.034(11) 0.031(12) -0.009(8) 0.007(10) -0.008(9) C7 0.106(13) 0.111(13) 0.103(13) -0.002(9) 0.004(9) 0.008(9) C8 0.12(2) 0.044(15) 0.08(2) 0.018(14) 0.007(18) -0.006(16) C9 0.039(12) 0.058(14) 0.052(15) -0.017(11) 0.018(11) 0.001(10) C10 0.057(15) 0.074(17) 0.045(16) 0.008(12) -0.013(13) -0.017(12) C11 0.14(2) 0.030(12) 0.041(15) 0.005(10) 0.021(16) 0.022(14) C12 0.085(17) 0.076(17) 0.023(13) 0.011(11) 0.019(12) 0.035(14) C13 0.139(16) 0.135(16) 0.131(16) -0.001(10) 0.003(10) -0.001(10) C14 0.105(13) 0.105(13) 0.115(13) -0.012(9) 0.003(9) -0.006(9) C15 0.10(2) 0.10(2) 0.10(2) 0.004(10) 0.008(10) -0.007(10) C16 0.09(2) 0.10(2) 0.10(2) -0.001(10) 0.014(10) -0.005(10) C17 0.132(16) 0.138(16) 0.134(16) 0.000(10) 0.001(10) 0.005(10) C18 0.063(17) 0.083(19) 0.060(19) -0.033(14) 0.007(15) -0.030(14) U3 0.0977(8) 0.0559(6) 0.0543(6) 0.0059(5) 0.0231(6) 0.0294(6) O1C 0.103(14) 0.085(13) 0.045(11) -0.015(9) -0.005(10) 0.019(11) O2C 0.133(16) 0.073(12) 0.035(10) -0.015(8) 0.023(10) 0.014(11) O3C 0.118(14) 0.036(9) 0.047(10) 0.008(7) 0.005(10) 0.012(9) O4C 0.065(7) 0.054(7) 0.072(8) -0.005(6) 0.039(7) 0.012(6) O5C 0.059(10) 0.049(9) 0.067(12) -0.006(8) 0.012(9) 0.015(7) O6C 0.052(7) 0.053(7) 0.064(8) 0.000(6) 0.004(6) -0.004(6) O7C 0.108(9) 0.073(8) 0.080(9) 0.011(7) 0.003(8) 0.029(7) O8C 0.070(10) 0.045(8) 0.030(8) 0.000(6) 0.004(7) 0.023(7) C1C 0.025(12) 0.064(16) 0.072(18) 0.000(13) -0.004(12) -0.003(10) C2C 0.075(18) 0.053(16) 0.068(19) 0.008(13) -0.003(15) -0.020(13) C3C 0.09(2) 0.050(16) 0.07(2) -0.019(14) -0.016(16) -0.002(14) C4C 0.076(19) 0.069(19) 0.07(2) -0.016(15) -0.028(16) -0.022(14) C5C 0.045(15) 0.08(2) 0.07(2) 0.012(15) -0.021(14) -0.016(14) C6C 0.041(14) 0.076(19) 0.08(2) 0.002(15) -0.023(13) 0.008(13) C7C 0.075(11) 0.080(11) 0.091(11) 0.001(9) 0.008(9) 0.002(9) C8C 0.13(3) 0.16(3) 0.09(3) 0.06(2) 0.05(2) 0.01(2) C9C 0.120(13) 0.111(13) 0.107(13) -0.002(9) 0.012(9) 0.006(9) C10C 0.163(17) 0.151(18) 0.156(18) 0.011(10) 0.009(10) -0.002(10) C11C 0.079(10) 0.056(9) 0.056(10) 0.002(8) -0.014(8) -0.006(8) C12C 0.15(3) 0.059(16) 0.034(15) -0.002(12) 0.025(17) 0.015(17) C13C 0.089(19) 0.047(14) 0.045(16) 0.010(11) 0.012(14) 0.026(13) C14C 0.066(16) 0.041(13) 0.066(18) 0.010(12) 0.019(14) -0.005(12) C15C 0.038(14) 0.063(17) 0.10(2) -0.001(15) 0.036(15) 0.006(13) C16C 0.051(16) 0.072(19) 0.13(3) 0.015(17) 0.046(18) -0.002(14) C17C 0.080(11) 0.081(11) 0.078(11) 0.005(9) 0.016(9) 0.006(9) C18C 0.070(10) 0.054(9) 0.067(10) -0.002(8) 0.023(8) 0.017(8) C19C 0.064(10) 0.074(10) 0.080(11) 0.000(8) 0.018(8) 0.023(8) C20C 0.137(16) 0.142(16) 0.138(16) 0.008(10) 0.016(10) 0.005(10) C21C 0.116(14) 0.116(14) 0.122(14) 0.012(9) 0.006(10) -0.003(9) C22C 0.12(2) 0.09(2) 0.08(2) 0.011(17) 0.066(19) -0.006(18) C23C 0.043(8) 0.063(9) 0.063(10) 0.006(8) 0.024(8) 0.008(7) C24C 0.059(17) 0.09(2) 0.064(18) 0.026(15) -0.005(14) 0.029(14) C25C 0.033(13) 0.12(2) 0.045(16) -0.007(15) 0.005(12) -0.021(13) C26C 0.074(17) 0.049(14) 0.061(18) -0.025(12) 0.010(14) 0.011(12) C27C 0.031(8) 0.030(7) 0.045(9) 0.003(7) -0.012(7) 0.009(6) C28C 0.038(12) 0.061(15) 0.056(16) -0.005(12) -0.013(11) -0.007(11) C29C 0.042(13) 0.049(13) 0.043(14) -0.007(10) 0.008(11) 0.025(10) C30C 0.056(9) 0.048(9) 0.051(9) -0.019(7) -0.005(8) 0.007(7) C31C 0.074(18) 0.058(16) 0.064(19) -0.017(13) 0.024(15) -0.004(13) C32C 0.061(16) 0.068(17) 0.08(2) 0.000(13) -0.021(14) 0.031(13) C33C 0.075(18) 0.062(16) 0.052(17) -0.002(12) -0.014(14) 0.016(13) C34C 0.078(19) 0.062(18) 0.11(3) 0.000(16) 0.005(17) -0.026(14) C35C 0.054(15) 0.044(13) 0.079(18) -0.015(12) 0.023(13) -0.001(11) C36C 0.061(16) 0.057(16) 0.10(2) -0.008(15) 0.014(15) -0.021(13) U4 0.0623(6) 0.0499(5) 0.0496(6) 0.0069(4) 0.0041(4) -0.0071(5) O1D 0.108(15) 0.059(11) 0.077(13) -0.003(10) 0.043(11) -0.017(11) O2D 0.044(9) 0.072(11) 0.064(12) -0.025(9) 0.003(8) -0.002(8) O3D 0.084(11) 0.064(10) 0.040(10) 0.005(8) 0.024(9) 0.002(9) O4D 0.048(9) 0.041(9) 0.089(13) -0.002(8) 0.008(9) -0.011(7) O5D 0.108(14) 0.070(11) 0.039(10) 0.014(8) 0.019(10) -0.034(10) O6D 0.103(9) 0.086(9) 0.086(9) -0.010(7) 0.034(8) -0.018(8) O7D 0.073(11) 0.054(10) 0.066(11) 0.003(8) -0.002(9) -0.028(8) O8D 0.043(8) 0.066(10) 0.028(8) 0.007(7) -0.009(7) 0.009(7) C1D 0.068(17) 0.041(13) 0.057(17) -0.023(11) 0.015(13) -0.018(12) C2D 0.083(19) 0.051(15) 0.032(14) -0.010(11) 0.003(13) -0.016(13) C3D 0.070(16) 0.023(10) 0.041(13) -0.004(9) 0.032(12) -0.004(10) C4D 0.083(19) 0.056(16) 0.067(18) -0.015(13) 0.037(15) -0.039(14) C5D 0.068(17) 0.060(16) 0.072(19) -0.004(13) 0.041(14) -0.003(13) C6D 0.060(15) 0.060(15) 0.047(15) 0.012(11) 0.026(12) -0.006(12) C7D 0.041(14) 0.061(16) 0.12(3) 0.015(16) 0.045(16) 0.006(12) C8D 0.10(2) 0.13(3) 0.08(2) 0.03(2) 0.014(18) 0.039(19) C9D 0.041(17) 0.19(4) 0.18(4) 0.09(3) 0.01(2) 0.01(2) C10D 0.103(12) 0.096(13) 0.103(13) -0.005(9) 0.021(9) 0.003(9) C11D 0.058(16) 0.066(16) 0.054(17) -0.010(12) -0.028(13) 0.003(12) C12D 0.14(3) 0.071(19) 0.044(18) 0.003(14) -0.026(18) -0.030(18) C13D 0.041(12) 0.047(12) 0.028(12) -0.009(9) 0.008(10) -0.025(9) C14D 0.037(12) 0.044(13) 0.072(18) -0.005(11) 0.011(12) 0.015(10) C15D 0.059(9) 0.050(9) 0.031(8) 0.010(7) 0.010(7) -0.010(7) C16D 0.052(13) 0.056(13) 0.032(12) -0.014(10) 0.020(10) -0.014(11) C17D 0.061(14) 0.048(13) 0.047(14) 0.006(10) 0.035(12) -0.019(11) C18D 0.063(15) 0.047(14) 0.070(18) 0.015(12) 0.018(14) -0.004(11) C19D 0.060(10) 0.077(11) 0.084(11) 0.010(9) 0.009(9) 0.005(8) C20D 0.184(19) 0.172(19) 0.169(19) 0.006(10) 0.012(10) 0.000(10) C21D 0.153(17) 0.147(17) 0.139(17) 0.003(10) 0.006(10) -0.012(10) C22D 0.163(18) 0.166(18) 0.164(18) 0.004(10) 0.026(10) 0.009(10) C23D 0.045(13) 0.052(13) 0.028(12) 0.007(9) -0.005(10) -0.016(10) C24D 0.092(11) 0.060(10) 0.076(11) 0.008(8) 0.002(9) -0.012(8) C25D 0.037(13) 0.047(13) 0.10(2) 0.010(13) 0.033(15) 0.003(11) C26D 0.030(13) 0.063(15) 0.054(17) 0.017(12) 0.008(12) -0.009(11) C27D 0.072(18) 0.073(17) 0.041(16) 0.005(12) -0.005(14) -0.028(14) C28D 0.038(13) 0.051(13) 0.072(18) 0.001(12) 0.033(13) -0.003(10) C29D 0.025(12) 0.061(15) 0.071(18) 0.004(13) 0.004(12) -0.008(10) C30D 0.074(18) 0.033(12) 0.068(18) -0.016(11) 0.022(14) -0.011(11) C31D 0.033(13) 0.056(15) 0.10(2) -0.014(14) -0.003(14) 0.010(11) C32D 0.073(11) 0.088(11) 0.062(11) 0.000(8) 0.009(8) -0.005(8) C33D 0.090(19) 0.056(15) 0.059(17) -0.020(12) 0.023(14) -0.003(13) C34D 0.060(17) 0.08(2) 0.09(2) -0.005(16) -0.038(16) -0.007(14) C35D 0.068(10) 0.053(9) 0.073(10) -0.002(8) 0.010(8) -0.019(8) C36D 0.085(11) 0.065(10) 0.060(10) -0.012(8) 0.013(8) -0.015(8) N3 0.021(6) 0.047(7) 0.052(8) 0.001(7) -0.004(6) 0.003(6) N4 0.024(9) 0.057(12) 0.060(13) -0.014(9) -0.005(9) 0.008(8) O7 0.161(12) 0.154(12) 0.135(12) 0.012(9) 0.027(9) 0.033(9) O8 0.081(9) 0.113(10) 0.103(10) 0.013(8) 0.013(8) 0.019(8) O9 0.135(11) 0.149(11) 0.139(11) 0.011(7) 0.004(7) -0.014(7) O10 0.105(9) 0.094(9) 0.079(9) 0.013(8) -0.014(8) -0.011(8) O11 0.155(11) 0.104(10) 0.112(11) 0.008(8) -0.014(9) 0.026(9) O12 0.131(11) 0.120(11) 0.112(11) -0.002(9) 0.009(9) 0.031(9) C19 0.171(17) 0.173(17) 0.168(17) 0.008(7) 0.017(7) 0.008(7) C20 0.091(19) 0.092(19) 0.042(15) 0.034(13) 0.034(14) 0.032(15) C21 0.110(14) 0.127(14) 0.121(14) -0.004(10) 0.021(10) 0.015(9) C22 0.143(17) 0.159(17) 0.148(17) 0.012(10) 0.007(10) 0.005(10) C23 0.078(11) 0.084(11) 0.086(12) 0.011(9) 0.005(9) 0.000(9) C24 0.112(13) 0.117(14) 0.107(14) 0.010(9) 0.010(9) 0.007(9) C25 0.19(2) 0.19(2) 0.18(2) 0.012(10) 0.005(10) -0.007(10) C26 0.038(8) 0.069(10) 0.064(10) 0.002(8) -0.009(8) -0.007(8) C27 0.064(11) 0.075(11) 0.086(12) 0.005(9) -0.003(9) 0.012(8) C28 0.08(2) 0.08(2) 0.09(2) 0.026(17) -0.034(18) -0.057(16) C29 0.091(18) 0.050(14) 0.052(16) -0.015(11) 0.036(14) -0.018(13) C30 0.099(13) 0.099(13) 0.103(13) 0.004(9) 0.003(9) -0.006(9) C31 0.09(2) 0.075(19) 0.08(2) -0.003(10) -0.009(10) 0.003(10) C32 0.086(19) 0.075(17) 0.042(16) -0.020(12) -0.005(14) 0.029(14) C33 0.111(13) 0.087(12) 0.103(13) -0.003(9) -0.010(9) 0.019(9) C34 0.08(2) 0.08(2) 0.20(4) -0.01(2) 0.05(3) 0.007(16) C35 0.099(12) 0.082(12) 0.082(12) 0.000(9) 0.005(9) 0.017(9) C36 0.121(14) 0.110(14) 0.114(14) -0.004(9) 0.001(10) 0.009(9) O13 0.105(10) 0.105(10) 0.102(10) 0.004(8) 0.012(8) 0.004(8) C37 0.118(14) 0.111(14) 0.117(14) 0.001(9) 0.013(9) 0.000(9) O14 0.105(15) 0.109(16) 0.107(16) 0.004(10) 0.003(10) 0.002(10) C38 0.09(2) 0.09(2) 0.09(2) 0.000(10) -0.001(10) 0.004(10) O15 0.121(10) 0.111(10) 0.107(10) 0.002(8) 0.003(8) 0.004(8) O16 0.143(19) 0.138(19) 0.135(19) -0.004(10) 0.000(10) 0.004(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O7A 1.782(13) . ? U1 O8A 1.827(13) . ? U1 O3A 2.219(13) . ? U1 O1A 2.222(12) . ? U1 O5A 2.225(14) . ? U1 O2A 2.817(14) . ? U1 O6A 3.182(15) . ? U1 O4A 3.671(14) . ? O1A C2A 1.34(2) . ? O2A C11A 1.44(2) . ? O2A C12A 1.45(2) . ? O3A C14A 1.33(3) . ? O4A C24A 1.43(2) . ? O4A C23A 1.46(2) . ? O5A C26A 1.41(2) . ? O6A C35A 1.45(2) . ? O6A C36A 1.46(2) . ? C1A C2A 1.36(3) . ? C1A C6A 1.39(3) . ? C1A C36A 1.47(3) . ? C2A C3A 1.49(3) . ? C3A C4A 1.34(3) . ? C3A C11A 1.51(3) . ? C4A C5A 1.41(3) . ? C5A C6A 1.35(3) . ? C5A C7A 1.54(3) . ? C7A C8A 1.46(3) . ? C7A C10A 1.55(3) . ? C7A C9A 1.57(3) . ? C12A C13A 1.46(3) . ? C13A C18A 1.43(3) . ? C13A C14A 1.44(3) . ? C14A C15A 1.43(3) . ? C15A C16A 1.32(3) . ? C15A C23A 1.49(3) . ? C16A C17A 1.36(3) . ? C17A C18A 1.36(3) . ? C17A C19A 1.55(3) . ? C19A C21A 1.50(3) . ? C19A C20A 1.51(3) . ? C19A C22A 1.51(4) . ? C24A C25A 1.55(3) . ? C25A C30A 1.36(3) . ? C25A C26A 1.40(3) . ? C26A C27A 1.38(3) . ? C27A C28A 1.38(3) . ? C27A C35A 1.45(2) . ? C28A C29A 1.48(3) . ? C29A C30A 1.37(3) . ? C29A C31A 1.51(3) . ? C31A C34A 1.51(3) . ? C31A C32A 1.54(3) . ? C31A C33A 1.54(3) . ? U2 O7B 1.756(15) . ? U2 O8B 1.803(15) . ? U2 O3B 2.190(14) . ? U2 O1B 2.197(18) . ? U2 O5B 2.217(19) . ? U2 O2B 2.792(15) . ? U2 O6B 3.22(2) . ? U2 O4B 3.530(18) . ? O1B C2B 1.39(3) . ? O2B C11B 1.48(2) . ? O2B C12B 1.48(2) . ? O3B C14B 1.31(2) . ? O4B C23B 1.41(2) . ? O4B C24B 1.44(3) . ? O5B C26B 1.35(3) . ? O6B C35B 1.45(3) . ? O6B C36B 1.47(4) . ? C1B C6B 1.41(4) . ? C1B C2B 1.42(4) . ? C1B C36B 1.58(4) . ? C2B C3B 1.31(4) . ? C3B C4B 1.35(3) . ? C3B C11B 1.53(3) . ? C4B C5B 1.36(4) . ? C5B C6B 1.39(4) . ? C5B C7B 1.60(2) . ? C7B C8B 1.51(3) . ? C7B C9B 1.52(3) . ? C7B C10B 1.54(3) . ? C12B C13B 1.53(3) . ? C13B C14B 1.34(3) . ? C13B C18B 1.39(3) . ? C14B C15B 1.51(3) . ? C15B C16B 1.36(3) . ? C15B C23B 1.52(3) . ? C16B C17B 1.48(3) . ? C17B C18B 1.44(3) . ? C17B C19B 1.47(3) . ? C19B C20B 1.51(4) . ? C19B C21B 1.51(3) . ? C19B C22B 1.53(4) . ? C24B C25B 1.48(4) . ? C25B C26B 1.37(4) . ? C25B C30B 1.35(4) . ? C26B C27B 1.48(4) . ? C27B C35B 1.51(4) . ? C27B C28B 1.40(4) . ? C28B C29B 1.33(3) . ? C29B C31B 1.45(3) . ? C29B C30B 1.51(4) . ? C31B C32B 1.52(4) . ? C31B C34B 1.54(4) . ? C31B C33B 1.60(3) . ? N1 C13 1.40(4) . ? N1 C1 1.47(3) . ? N1 C7 1.49(3) . ? N2 C6 1.46(3) . ? N2 C12 1.46(3) . ? N2 C18 1.50(3) . ? O1 C3 1.44(3) . ? O1 C2 1.46(3) . ? O2 C4 1.40(3) . ? O2 C5 1.43(2) . ? O3 C9 1.41(3) . ? O3 C8 1.44(3) . ? O4 C11 1.38(3) . ? O4 C10 1.43(2) . ? O5 C14 1.45(3) . ? O5 C15 1.47(3) . ? O6 C16 1.38(5) . ? O6 C17 1.48(4) . ? C1 C2 1.53(3) . ? C3 C4 1.47(3) . ? C5 C6 1.51(3) . ? C7 C8 1.53(3) . ? C9 C10 1.45(3) . ? C11 C12 1.47(3) . ? C13 C14 1.53(4) . ? C15 C16 1.51(3) . ? C17 C18 1.52(4) . ? U3 O7C 1.773(17) . ? U3 O8C 1.800(13) . ? U3 O1C 2.173(19) . ? U3 O5C 2.240(14) . ? U3 O3C 2.272(17) . ? U3 O2C 2.793(16) . ? U3 O6C 3.357(15) . ? U3 O4C 3.419(19) . ? O1C C2C 1.38(3) . ? O2C C12C 1.47(3) . ? O2C C11C 1.49(3) . ? O3C C14C 1.38(3) . ? O4C C24C 1.40(3) . ? O4C C23C 1.43(2) . ? O5C C26C 1.35(3) . ? O6C C35C 1.41(2) . ? O6C C36C 1.41(2) . ? C1C C6C 1.41(3) . ? C1C C2C 1.42(3) . ? C1C C36C 1.49(3) . ? C2C C3C 1.37(3) . ? C3C C4C 1.37(4) . ? C3C C11C 1.46(3) . ? C4C C5C 1.45(3) . ? C5C C6C 1.41(3) . ? C5C C7C 1.48(3) . ? C7C C8C 1.50(3) . ? C7C C9C 1.51(3) . ? C7C C10C 1.54(3) . ? C12C C13C 1.51(4) . ? C13C C18C 1.36(3) . ? C13C C14C 1.45(3) . ? C14C C15C 1.31(3) . ? C15C C16C 1.35(4) . ? C15C C23C 1.55(3) . ? C16C C17C 1.46(4) . ? C17C C18C 1.42(4) . ? C17C C19C 1.52(4) . ? C19C C20C 1.53(5) . ? C19C C22C 1.53(5) . ? C19C C21C 1.53(5) . ? C24C C25C 1.51(3) . ? C25C C30C 1.37(3) . ? C25C C26C 1.41(3) . ? C26C C27C 1.42(3) . ? C27C C28C 1.43(3) . ? C27C C35C 1.51(3) . ? C28C C29C 1.43(3) . ? C29C C30C 1.42(3) . ? C29C C31C 1.53(3) . ? C31C C33C 1.45(3) . ? C31C C34C 1.54(3) . ? C31C C32C 1.60(3) . ? U4 O7D 1.804(16) . ? U4 O8D 1.809(13) . ? U4 O1D 2.199(17) . ? U4 O5D 2.207(16) . ? U4 O3D 2.257(15) . ? U4 O2D 3.031(16) . ? U4 O4D 3.132(16) . ? U4 O6D 3.390(19) . ? O1D C2D 1.30(3) . ? O2D C11D 1.40(2) . ? O2D C12D 1.45(3) . ? O3D C14D 1.32(2) . ? O4D C23D 1.41(2) . ? O4D C24D 1.48(3) . ? O5D C26D 1.37(3) . ? O6D C36D 1.41(3) . ? O6D C35D 1.45(3) . ? C1D C2D 1.39(3) . ? C1D C6D 1.41(3) . ? C1D C36D 1.47(3) . ? C2D C3D 1.48(3) . ? C3D C4D 1.40(3) . ? C3D C11D 1.51(3) . ? C4D C5D 1.39(3) . ? C5D C6D 1.47(3) . ? C5D C7D 1.54(3) . ? C7D C9D 1.52(3) . ? C7D C8D 1.51(3) . ? C7D C10D 1.63(4) . ? C12D C13D 1.51(3) . ? C13D C18D 1.32(3) . ? C13D C14D 1.38(3) . ? C14D C15D 1.43(3) . ? C15D C16D 1.43(2) . ? C15D C23D 1.45(3) . ? C16D C17D 1.46(3) . ? C17D C18D 1.42(3) . ? C17D C19D 1.59(3) . ? C19D C21D 1.54(4) . ? C19D C20D 1.58(4) . ? C19D C22D 1.54(3) . ? C24D C25D 1.45(3) . ? C25D C30D 1.37(3) . ? C25D C26D 1.41(3) . ? C26D C27D 1.35(3) . ? C27D C28D 1.43(3) . ? C27D C35D 1.57(3) . ? C28D C29D 1.34(3) . ? C29D C30D 1.39(3) . ? C29D C31D 1.61(3) . ? C31D C33D 1.51(3) . ? C31D C32D 1.55(3) . ? C31D C34D 1.58(3) . ? N3 C31 1.44(3) . ? N3 C25 1.53(3) . ? N3 C19 1.58(3) . ? N4 C30 1.45(3) . ? N4 C36 1.44(4) . ? N4 C24 1.58(3) . ? O7 C20 1.39(3) . ? O7 C21 1.47(4) . ? O8 C23 1.44(3) . ? O8 C22 1.43(4) . ? O9 C26 1.33(3) . ? O9 C27 1.39(3) . ? O10 C29 1.43(3) . ? O10 C28 1.47(3) . ? O11 C32 1.34(3) . ? O11 C33 1.51(3) . ? O12 C35 1.39(3) . ? O12 C34 1.45(3) . ? C19 C20 1.47(4) . ? C21 C22 1.49(3) . ? C23 C24 1.53(4) . ? C25 C26 1.47(3) . ? C27 C28 1.46(4) . ? C29 C30 1.48(4) . ? C31 C32 1.44(3) . ? C33 C34 1.58(4) . ? C35 C36 1.50(4) . ? O13 C37 1.46(3) . ? O14 C38 1.44(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7A U1 O8A 176.1(7) . . ? O7A U1 O3A 87.9(6) . . ? O8A U1 O3A 90.9(5) . . ? O7A U1 O1A 88.3(6) . . ? O8A U1 O1A 95.2(5) . . ? O3A U1 O1A 132.9(5) . . ? O7A U1 O5A 87.9(6) . . ? O8A U1 O5A 89.0(6) . . ? O3A U1 O5A 109.2(5) . . ? O1A U1 O5A 117.5(5) . . ? O7A U1 O2A 112.2(6) . . ? O8A U1 O2A 70.8(5) . . ? O3A U1 O2A 70.8(5) . . ? O1A U1 O2A 67.5(4) . . ? O5A U1 O2A 159.8(5) . . ? O7A U1 O6A 116.5(5) . . ? O8A U1 O6A 64.1(5) . . ? O3A U1 O6A 153.5(5) . . ? O1A U1 O6A 62.2(4) . . ? O5A U1 O6A 64.6(4) . . ? O2A U1 O6A 105.9(4) . . ? O7A U1 O4A 118.1(5) . . ? O8A U1 O4A 58.2(5) . . ? O3A U1 O4A 58.1(4) . . ? O1A U1 O4A 153.1(4) . . ? O5A U1 O4A 62.9(4) . . ? O2A U1 O4A 103.3(4) . . ? O6A U1 O4A 98.9(3) . . ? C11A O2A C12A 117.2(16) . . ? C24A O4A C23A 114.4(17) . . ? C35A O6A C36A 115.5(13) . . ? C2A C1A C6A 119.7(17) . . ? C2A C1A C36A 117.0(18) . . ? C6A C1A C36A 122.8(19) . . ? O1A C2A C1A 124.5(18) . . ? O1A C2A C3A 116.3(17) . . ? C1A C2A C3A 119.2(17) . . ? C4A C3A C2A 117.1(17) . . ? C4A C3A C11A 126.4(19) . . ? C2A C3A C11A 116.2(18) . . ? C3A C4A C5A 123.1(19) . . ? C6A C5A C4A 118.3(19) . . ? C6A C5A C7A 121.5(19) . . ? C4A C5A C7A 120.1(19) . . ? C5A C6A C1A 122(2) . . ? C8A C7A C5A 115.1(19) . . ? C8A C7A C10A 107(2) . . ? C5A C7A C10A 112.1(17) . . ? C8A C7A C9A 105.9(19) . . ? C5A C7A C9A 109(2) . . ? C10A C7A C9A 106.6(19) . . ? O2A C11A C3A 109.1(16) . . ? O2A C12A C13A 113.5(19) . . ? C18A C13A C14A 120(2) . . ? C18A C13A C12A 122(2) . . ? C14A C13A C12A 117.9(18) . . ? O3A C14A C15A 125.0(19) . . ? O3A C14A C13A 117(2) . . ? C15A C14A C13A 117(2) . . ? C16A C15A C14A 118(2) . . ? C16A C15A C23A 126(2) . . ? C14A C15A C23A 115.6(18) . . ? C15A C16A C17A 125(2) . . ? C16A C17A C18A 120(2) . . ? C16A C17A C19A 123.1(19) . . ? C18A C17A C19A 116.5(19) . . ? C17A C18A C13A 118(2) . . ? C21A C19A C20A 111(2) . . ? C21A C19A C22A 112(2) . . ? C20A C19A C22A 106(2) . . ? C21A C19A C17A 108(2) . . ? C20A C19A C17A 113.5(17) . . ? C22A C19A C17A 106(2) . . ? O4A C23A C15A 105.6(16) . . ? O4A C24A C25A 107.2(17) . . ? C30A C25A C26A 118.8(18) . . ? C30A C25A C24A 120.0(19) . . ? C26A C25A C24A 120.9(18) . . ? C27A C26A C25A 121.8(19) . . ? C27A C26A O5A 118.5(18) . . ? C25A C26A O5A 119.7(17) . . ? C26A C27A C28A 118.4(18) . . ? C26A C27A C35A 121.9(19) . . ? C28A C27A C35A 119.3(17) . . ? C27A C28A C29A 121.6(17) . . ? C30A C29A C28A 115(2) . . ? C30A C29A C31A 121.9(19) . . ? C28A C29A C31A 123.0(18) . . ? C25A C30A C29A 124.2(19) . . ? C34A C31A C29A 107.7(16) . . ? C34A C31A C32A 107.7(17) . . ? C29A C31A C32A 112.0(18) . . ? C34A C31A C33A 107.5(18) . . ? C29A C31A C33A 114.1(17) . . ? C32A C31A C33A 107.7(17) . . ? O6A C35A C27A 107.5(15) . . ? C1A C36A O6A 109.5(15) . . ? O7B U2 O8B 178.2(8) . . ? O7B U2 O3B 88.0(6) . . ? O8B U2 O3B 91.1(6) . . ? O7B U2 O1B 86.1(8) . . ? O8B U2 O1B 95.6(7) . . ? O3B U2 O1B 132.1(7) . . ? O7B U2 O5B 88.4(8) . . ? O8B U2 O5B 90.4(7) . . ? O3B U2 O5B 109.8(6) . . ? O1B U2 O5B 117.5(7) . . ? O7B U2 O2B 112.7(7) . . ? O8B U2 O2B 68.5(6) . . ? O3B U2 O2B 69.3(4) . . ? O1B U2 O2B 69.5(5) . . ? O5B U2 O2B 158.7(6) . . ? O7B U2 O6B 117.2(7) . . ? O8B U2 O6B 63.4(7) . . ? O3B U2 O6B 152.6(6) . . ? O1B U2 O6B 64.5(7) . . ? O5B U2 O6B 63.6(6) . . ? O2B U2 O6B 106.8(5) . . ? O7B U2 O4B 117.5(7) . . ? O8B U2 O4B 60.7(6) . . ? O3B U2 O4B 59.4(4) . . ? O1B U2 O4B 155.7(5) . . ? O5B U2 O4B 61.3(6) . . ? O2B U2 O4B 103.6(4) . . ? O6B U2 O4B 97.2(6) . . ? C11B O2B C12B 110.3(15) . . ? C23B O4B C24B 111.4(18) . . ? C35B O6B C36B 118(2) . . ? C6B C1B C2B 122(3) . . ? C6B C1B C36B 123(3) . . ? C2B C1B C36B 116(3) . . ? C3B C2B O1B 127(3) . . ? C3B C2B C1B 118(3) . . ? O1B C2B C1B 115(3) . . ? C2B C3B C4B 123(3) . . ? C2B C3B C11B 119(3) . . ? C4B C3B C11B 117(2) . . ? C3B C4B C5B 118(3) . . ? C4B C5B C6B 123(2) . . ? C4B C5B C7B 112(2) . . ? C6B C5B C7B 125(2) . . ? C5B C6B C1B 114(3) . . ? C8B C7B C9B 112.6(10) . . ? C8B C7B C10B 110.9(10) . . ? C9B C7B C10B 110.6(10) . . ? C8B C7B C5B 107.7(10) . . ? C9B C7B C5B 107.6(10) . . ? C10B C7B C5B 107.0(10) . . ? O2B C11B C3B 105.4(17) . . ? O2B C12B C13B 106.2(17) . . ? C14B C13B C18B 122(2) . . ? C14B C13B C12B 120(2) . . ? C18B C13B C12B 118(2) . . ? O3B C14B C13B 123(2) . . ? O3B C14B C15B 121(2) . . ? C13B C14B C15B 116(2) . . ? C16B C15B C14B 119(2) . . ? C16B C15B C23B 123(2) . . ? C14B C15B C23B 117(2) . . ? C15B C16B C17B 126(2) . . ? C18B C17B C19B 124(2) . . ? C18B C17B C16B 109(2) . . ? C19B C17B C16B 128(2) . . ? C13B C18B C17B 127(2) . . ? C17B C19B C20B 107(2) . . ? C17B C19B C21B 108.4(19) . . ? C20B C19B C21B 110(2) . . ? C17B C19B C22B 112(2) . . ? C20B C19B C22B 109(2) . . ? C21B C19B C22B 111(2) . . ? O4B C23B C15B 104.9(17) . . ? O4B C24B C25B 109(2) . . ? C26B C25B C30B 125(3) . . ? C26B C25B C24B 117(3) . . ? C30B C25B C24B 117(3) . . ? C25B C26B O5B 129(3) . . ? C25B C26B C27B 111(3) . . ? O5B C26B C27B 119(3) . . ? C35B C27B C28B 124(3) . . ? C35B C27B C26B 111(3) . . ? C28B C27B C26B 125(3) . . ? C29B C28B C27B 122(3) . . ? C28B C29B C31B 124(2) . . ? C28B C29B C30B 115(3) . . ? C31B C29B C30B 121(3) . . ? C25B C30B C29B 121(3) . . ? C29B C31B C32B 117(2) . . ? C29B C31B C34B 112(3) . . ? C32B C31B C34B 105(2) . . ? C29B C31B C33B 109(2) . . ? C32B C31B C33B 104(2) . . ? C34B C31B C33B 109(2) . . ? C27B C35B O6B 114(3) . . ? O6B C36B C1B 107(3) . . ? C13 N1 C1 101(2) . . ? C13 N1 C7 121(2) . . ? C1 N1 C7 113.1(19) . . ? C6 N2 C12 113.2(19) . . ? C6 N2 C18 107.9(18) . . ? C12 N2 C18 112.0(18) . . ? C3 O1 C2 115.0(18) . . ? C4 O2 C5 110.0(17) . . ? C9 O3 C8 114.4(18) . . ? C11 O4 C10 119.1(18) . . ? C14 O5 C15 114.9(11) . . ? C16 O6 C17 120(3) . . ? N1 C1 C2 115(2) . . ? O1 C2 C1 106.5(19) . . ? O1 C3 C4 111(2) . . ? O2 C4 C3 113(2) . . ? O2 C5 C6 104.9(16) . . ? N2 C6 C5 113.6(18) . . ? N1 C7 C8 111(2) . . ? O3 C8 C7 110(2) . . ? O3 C9 C10 109(2) . . ? O4 C10 C9 111.7(19) . . ? O4 C11 C12 112(2) . . ? C11 C12 N2 115.6(18) . . ? N1 C13 C14 108(3) . . ? O5 C14 C13 114(3) . . ? O5 C15 C16 98(3) . . ? O6 C16 C15 109(4) . . ? O6 C17 C18 110(3) . . ? N2 C18 C17 108(3) . . ? O7C U3 O8C 177.9(8) . . ? O7C U3 O1C 87.1(8) . . ? O8C U3 O1C 95.1(7) . . ? O7C U3 O5C 89.5(7) . . ? O8C U3 O5C 89.5(6) . . ? O1C U3 O5C 112.6(6) . . ? O7C U3 O3C 88.3(7) . . ? O8C U3 O3C 90.4(6) . . ? O1C U3 O3C 133.3(6) . . ? O5C U3 O3C 113.8(5) . . ? O7C U3 O2C 109.4(7) . . ? O8C U3 O2C 71.7(5) . . ? O1C U3 O2C 67.8(6) . . ? O5C U3 O2C 161.0(5) . . ? O3C U3 O2C 70.2(5) . . ? O7C U3 O6C 117.7(6) . . ? O8C U3 O6C 63.5(5) . . ? O1C U3 O6C 59.0(5) . . ? O5C U3 O6C 64.1(5) . . ? O3C U3 O6C 153.4(5) . . ? O2C U3 O6C 103.5(4) . . ? O7C U3 O4C 118.3(7) . . ? O8C U3 O4C 59.6(5) . . ? O1C U3 O4C 153.5(5) . . ? O5C U3 O4C 63.4(4) . . ? O3C U3 O4C 60.4(5) . . ? O2C U3 O4C 107.1(5) . . ? O6C U3 O4C 99.3(3) . . ? C12C O2C C11C 113.0(19) . . ? C24C O4C C23C 115.7(17) . . ? C35C O6C C36C 115.8(17) . . ? C6C C1C C2C 120(2) . . ? C6C C1C C36C 120(2) . . ? C2C C1C C36C 120(2) . . ? C3C C2C O1C 122(2) . . ? C3C C2C C1C 122(2) . . ? O1C C2C C1C 116(2) . . ? C2C C3C C4C 119(3) . . ? C2C C3C C11C 119(3) . . ? C4C C3C C11C 122(3) . . ? C3C C4C C5C 122(3) . . ? C6C C5C C4C 118(3) . . ? C6C C5C C7C 117(3) . . ? C4C C5C C7C 125(3) . . ? C5C C6C C1C 119(3) . . ? C8C C7C C9C 112(3) . . ? C8C C7C C5C 118(2) . . ? C9C C7C C5C 114(2) . . ? C8C C7C C10C 94(2) . . ? C9C C7C C10C 104(2) . . ? C5C C7C C10C 112(2) . . ? C3C C11C O2C 104.1(19) . . ? O2C C12C C13C 104.6(19) . . ? C18C C13C C14C 116(3) . . ? C18C C13C C12C 122(2) . . ? C14C C13C C12C 122(2) . . ? C15C C14C O3C 123(2) . . ? C15C C14C C13C 123(3) . . ? O3C C14C C13C 114(2) . . ? C14C C15C C16C 123(3) . . ? C14C C15C C23C 118(2) . . ? C16C C15C C23C 118(3) . . ? C15C C16C C17C 118(3) . . ? C16C C17C C18C 118(3) . . ? C16C C17C C19C 118(2) . . ? C18C C17C C19C 124(3) . . ? C13C C18C C17C 122(2) . . ? C20C C19C C22C 109(3) . . ? C20C C19C C21C 110(2) . . ? C22C C19C C21C 109(3) . . ? C20C C19C C17C 105(3) . . ? C22C C19C C17C 109(2) . . ? C21C C19C C17C 114(2) . . ? O4C C23C C15C 103.6(17) . . ? O4C C24C C25C 106(2) . . ? C30C C25C C26C 122(2) . . ? C30C C25C C24C 121(2) . . ? C26C C25C C24C 116(2) . . ? O5C C26C C27C 120(2) . . ? O5C C26C C25C 121(2) . . ? C27C C26C C25C 119(2) . . ? C26C C27C C28C 118.4(19) . . ? C26C C27C C35C 120(2) . . ? C28C C27C C35C 121(2) . . ? C29C C28C C27C 122(2) . . ? C30C C29C C28C 117(2) . . ? C30C C29C C31C 123(2) . . ? C28C C29C C31C 120.2(19) . . ? C25C C30C C29C 122(2) . . ? C33C C31C C29C 117(2) . . ? C33C C31C C34C 109(2) . . ? C29C C31C C34C 110(2) . . ? C33C C31C C32C 107(2) . . ? C29C C31C C32C 107.4(18) . . ? C34C C31C C32C 106(2) . . ? O6C C35C C27C 109.0(17) . . ? O6C C36C C1C 107.4(19) . . ? O7D U4 O8D 178.0(7) . . ? O7D U4 O1D 89.2(7) . . ? O8D U4 O1D 88.8(7) . . ? O7D U4 O5D 88.6(6) . . ? O8D U4 O5D 92.0(6) . . ? O1D U4 O5D 118.5(6) . . ? O7D U4 O3D 84.0(6) . . ? O8D U4 O3D 97.3(6) . . ? O1D U4 O3D 122.1(6) . . ? O5D U4 O3D 118.7(6) . . ? O7D U4 O2D 111.7(5) . . ? O8D U4 O2D 67.7(5) . . ? O1D U4 O2D 65.4(5) . . ? O5D U4 O2D 159.6(5) . . ? O3D U4 O2D 64.5(5) . . ? O7D U4 O4D 114.5(6) . . ? O8D U4 O4D 67.5(5) . . ? O1D U4 O4D 156.2(6) . . ? O5D U4 O4D 63.4(5) . . ? O3D U4 O4D 65.2(5) . . ? O2D U4 O4D 104.6(4) . . ? O7D U4 O6D 117.7(6) . . ? O8D U4 O6D 61.0(5) . . ? O1D U4 O6D 61.6(6) . . ? O5D U4 O6D 65.7(6) . . ? O3D U4 O6D 158.3(5) . . ? O2D U4 O6D 103.8(4) . . ? O4D U4 O6D 103.1(4) . . ? C11D O2D C12D 115.3(17) . . ? C23D O4D C24D 119.2(18) . . ? C36D O6D C35D 114.2(18) . . ? C2D C1D C6D 120(2) . . ? C2D C1D C36D 116(2) . . ? C6D C1D C36D 124(2) . . ? O1D C2D C1D 122(2) . . ? O1D C2D C3D 117(2) . . ? C1D C2D C3D 120(2) . . ? C4D C3D C2D 119(2) . . ? C4D C3D C11D 123.1(19) . . ? C2D C3D C11D 118(2) . . ? C3D C4D C5D 121(2) . . ? C4D C5D C6D 119(2) . . ? C4D C5D C7D 122(2) . . ? C6D C5D C7D 119(2) . . ? C1D C6D C5D 120(2) . . ? C9D C7D C8D 114(3) . . ? C9D C7D C5D 116(2) . . ? C8D C7D C5D 109(2) . . ? C9D C7D C10D 105(2) . . ? C8D C7D C10D 109(2) . . ? C5D C7D C10D 104(2) . . ? O2D C11D C3D 106.1(17) . . ? O2D C12D C13D 110.4(19) . . ? C18D C13D C14D 125(2) . . ? C18D C13D C12D 120(2) . . ? C14D C13D C12D 114.1(19) . . ? O3D C14D C13D 123(2) . . ? O3D C14D C15D 118.2(19) . . ? C13D C14D C15D 118(2) . . ? C16D C15D C14D 119.1(19) . . ? C16D C15D C23D 121.8(19) . . ? C14D C15D C23D 118.9(17) . . ? C15D C16D C17D 116.9(17) . . ? C18D C17D C16D 120.4(17) . . ? C18D C17D C19D 125.0(19) . . ? C16D C17D C19D 114.3(19) . . ? C13D C18D C17D 118(2) . . ? C21D C19D C20D 104(3) . . ? C21D C19D C17D 110(2) . . ? C20D C19D C17D 110(2) . . ? C21D C19D C22D 102(3) . . ? C20D C19D C22D 115(3) . . ? C17D C19D C22D 114(2) . . ? O4D C23D C15D 108.5(18) . . ? C25D C24D O4D 111(2) . . ? C30D C25D C26D 121(2) . . ? C30D C25D C24D 121(3) . . ? C26D C25D C24D 118(3) . . ? C27D C26D O5D 121(2) . . ? C27D C26D C25D 119(2) . . ? O5D C26D C25D 120(2) . . ? C26D C27D C28D 120(2) . . ? C26D C27D C35D 119(2) . . ? C28D C27D C35D 121(2) . . ? C29D C28D C27D 119(2) . . ? C28D C29D C30D 123(2) . . ? C28D C29D C31D 122(2) . . ? C30D C29D C31D 115(2) . . ? C25D C30D C29D 118(2) . . ? C33D C31D C32D 110(2) . . ? C33D C31D C34D 108.0(19) . . ? C32D C31D C34D 106(2) . . ? C33D C31D C29D 113(2) . . ? C32D C31D C29D 108.7(19) . . ? C34D C31D C29D 112(2) . . ? O6D C35D C27D 103.6(18) . . ? O6D C36D C1D 107.5(18) . . ? C31 N3 C25 111.9(18) . . ? C31 N3 C19 109.4(16) . . ? C25 N3 C19 106.9(16) . . ? C30 N4 C36 104(2) . . ? C30 N4 C24 108(2) . . ? C36 N4 C24 120(2) . . ? C20 O7 C21 113(3) . . ? C23 O8 C22 102(2) . . ? C26 O9 C27 110(2) . . ? C29 O10 C28 112(2) . . ? C32 O11 C33 111(2) . . ? C35 O12 C34 117(3) . . ? C20 C19 N3 114(3) . . ? O7 C20 C19 122(3) . . ? C22 C21 O7 114(3) . . ? C21 C22 O8 94(3) . . ? O8 C23 C24 99(2) . . ? C23 C24 N4 105(2) . . ? C26 C25 N3 118(3) . . ? O9 C26 C25 114(3) . . ? O9 C27 C28 101(2) . . ? C27 C28 O10 107(3) . . ? O10 C29 C30 101(2) . . ? N4 C30 C29 117(3) . . ? N3 C31 C32 116(3) . . ? C31 C32 O11 113(2) . . ? O11 C33 C34 99(3) . . ? O12 C34 C33 100(2) . . ? O12 C35 C36 109(3) . . ? N4 C36 C35 117(3) . . ? #===END data_5 _database_code_CSD 181044 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H104 N2 O22 U2' _chemical_formula_weight 2185.93 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 P21/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 25.3546(11) _cell_length_b 13.8369(9) _cell_length_c 28.0625(14) _cell_angle_alpha 90.00 _cell_angle_beta 112.456(4) _cell_angle_gamma 90.00 _cell_volume 9098.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 54783 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent intense orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method ? _exptl_crystal_F_000 4360 _exptl_absorpt_coefficient_mu 3.631 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.390 _exptl_absorpt_correction_T_max 0.748 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _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 54783 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.68 _reflns_number_total 16835 _reflns_number_gt 8352 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _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 subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms bound to N atoms have been found on the Fourier-difference map and introduced as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. All other hydrogen atoms were introduced at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 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^)+(0.0469P)^2^+10.5772P] 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 16835 _refine_ls_number_parameters 1153 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1737 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.1583 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.028 _refine_diff_density_min -1.240 _refine_diff_density_rms 0.148 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 0.59654(2) 0.22995(3) 0.426925(17) 0.04396(15) Uani 1 1 d . . . O1A O 0.6763(3) 0.2116(6) 0.4122(3) 0.045(2) Uani 1 1 d . . . O2A O 0.6594(3) 0.3842(6) 0.4585(3) 0.049(2) Uani 1 1 d . . . O3A O 0.5633(3) 0.3200(6) 0.4739(3) 0.045(2) Uani 1 1 d . . . O4A O 0.4537(4) 0.2962(6) 0.3855(3) 0.058(2) Uani 1 1 d . . . O5A O 0.5339(4) 0.1195(6) 0.3808(3) 0.052(2) Uani 1 1 d . . . O6A O 0.5924(3) 0.1676(5) 0.2976(3) 0.049(2) Uani 1 1 d . . . O7A O 0.6255(4) 0.1486(6) 0.4794(3) 0.057(2) Uani 1 1 d . . . O8A O 0.5692(3) 0.3072(5) 0.3728(3) 0.046(2) Uani 1 1 d . . . C1A C 0.6789(5) 0.2505(8) 0.3296(4) 0.035(3) Uani 1 1 d . . . C2A C 0.6878(4) 0.2753(9) 0.3811(4) 0.040(3) Uani 1 1 d . . . C3A C 0.7070(5) 0.3677(8) 0.4002(4) 0.045(3) Uani 1 1 d . . . C4A C 0.7171(4) 0.4343(8) 0.3674(4) 0.035(3) Uani 1 1 d . . . H4A H 0.7302 0.4956 0.3800 0.042 Uiso 1 1 calc R . . C5A C 0.7083(4) 0.4124(8) 0.3153(4) 0.033(3) Uani 1 1 d . . . C6A C 0.6882(5) 0.3184(8) 0.2991(4) 0.039(3) Uani 1 1 d . . . H6A H 0.6807 0.3020 0.2650 0.047 Uiso 1 1 calc R . . C7A C 0.7149(5) 0.4890(9) 0.2807(5) 0.045(3) Uani 1 1 d . . . C8A C 0.7111(5) 0.5852(9) 0.2912(5) 0.047(3) Uani 1 1 d . . . H8A H 0.7091 0.6025 0.3224 0.057 Uiso 1 1 calc R . . C9A C 0.7103(5) 0.6578(10) 0.2562(6) 0.059(4) Uani 1 1 d . . . H9A H 0.7060 0.7222 0.2635 0.071 Uiso 1 1 calc R . . C10A C 0.7160(5) 0.6327(11) 0.2105(5) 0.053(4) Uani 1 1 d . . . H10A H 0.7154 0.6808 0.1871 0.064 Uiso 1 1 calc R . . C11A C 0.7225(5) 0.5375(10) 0.1993(5) 0.054(4) Uani 1 1 d . . . H11A H 0.7282 0.5207 0.1695 0.065 Uiso 1 1 calc R . . C12A C 0.7201(5) 0.4665(10) 0.2343(5) 0.048(3) Uani 1 1 d . . . H12A H 0.7222 0.4018 0.2262 0.057 Uiso 1 1 calc R . . C13A C 0.7144(5) 0.3931(9) 0.4538(4) 0.047(3) Uani 1 1 d . . . H13A H 0.7419 0.3500 0.4779 0.056 Uiso 1 1 calc R . . H13B H 0.7285 0.4588 0.4615 0.056 Uiso 1 1 calc R . . C14A C 0.6483(5) 0.4579(9) 0.4911(4) 0.047(3) Uani 1 1 d . . . H14A H 0.6714 0.5147 0.4929 0.056 Uiso 1 1 calc R . . H14B H 0.6584 0.4331 0.5258 0.056 Uiso 1 1 calc R . . C15A C 0.5861(5) 0.4850(9) 0.4689(4) 0.044(3) Uani 1 1 d . . . C16A C 0.5459(5) 0.4088(10) 0.4611(4) 0.043(3) Uani 1 1 d . . . C17A C 0.4882(5) 0.4337(10) 0.4395(5) 0.046(3) Uani 1 1 d . . . C18A C 0.4714(5) 0.5277(10) 0.4257(4) 0.050(3) Uani 1 1 d . . . H18A H 0.4326 0.5412 0.4099 0.060 Uiso 1 1 calc R . . C19A C 0.5102(5) 0.6035(10) 0.4343(5) 0.049(3) Uani 1 1 d . . . C20A C 0.5682(5) 0.5791(9) 0.4565(4) 0.046(3) Uani 1 1 d . . . H20A H 0.5954 0.6277 0.4630 0.056 Uiso 1 1 calc R . . C21A C 0.4929(6) 0.7082(12) 0.4183(5) 0.062(4) Uani 1 1 d . . . C22A C 0.5243(6) 0.7658(11) 0.4009(5) 0.065(4) Uani 1 1 d . . . H22A H 0.5567 0.7413 0.3972 0.078 Uiso 1 1 calc R . . C23A C 0.5086(8) 0.8633(13) 0.3883(7) 0.093(6) Uani 1 1 d . . . H23A H 0.5320 0.9047 0.3790 0.111 Uiso 1 1 calc R . . C24A C 0.4582(9) 0.8956(14) 0.3899(7) 0.103(6) Uani 1 1 d U . . H24A H 0.4472 0.9595 0.3816 0.123 Uiso 1 1 calc R . . C25A C 0.4229(9) 0.8324(15) 0.4039(7) 0.110(6) Uani 1 1 d U . . H25A H 0.3876 0.8533 0.4029 0.132 Uiso 1 1 calc R . . C26A C 0.4415(7) 0.7377(11) 0.4193(5) 0.074(4) Uani 1 1 d U . . H26A H 0.4196 0.6957 0.4300 0.089 Uiso 1 1 calc R . . C27A C 0.4454(5) 0.3478(10) 0.4269(4) 0.054(4) Uani 1 1 d . . . H27A H 0.4535 0.3065 0.4568 0.065 Uiso 1 1 calc R . . H27B H 0.4065 0.3712 0.4161 0.065 Uiso 1 1 calc R . . C28A C 0.4277(5) 0.2034(9) 0.3743(4) 0.049(3) Uani 1 1 d . . . H28A H 0.3870 0.2086 0.3664 0.058 Uiso 1 1 calc R . . H28B H 0.4443 0.1607 0.4036 0.058 Uiso 1 1 calc R . . C29A C 0.4380(5) 0.1646(8) 0.3285(5) 0.047(3) Uani 1 1 d . . . C30A C 0.4918(5) 0.1307(8) 0.3338(4) 0.042(3) Uani 1 1 d . . . C31A C 0.5007(5) 0.1064(8) 0.2885(4) 0.042(3) Uani 1 1 d . . . C32A C 0.4583(5) 0.1177(8) 0.2404(5) 0.044(3) Uani 1 1 d . . . H32A H 0.4658 0.1038 0.2112 0.052 Uiso 1 1 calc R . . C33A C 0.4039(5) 0.1499(9) 0.2349(5) 0.045(3) Uani 1 1 d . . . C34A C 0.3953(5) 0.1747(8) 0.2790(4) 0.045(3) Uani 1 1 d . . . H34A H 0.3599 0.1989 0.2758 0.054 Uiso 1 1 calc R . . C35A C 0.3598(6) 0.1714(9) 0.1825(5) 0.050(3) Uani 1 1 d . . . C36A C 0.3716(6) 0.2000(9) 0.1401(5) 0.056(4) Uani 1 1 d . . . H36A H 0.4095 0.2058 0.1437 0.067 Uiso 1 1 calc R . . C37A C 0.3292(5) 0.2200(9) 0.0928(4) 0.050(3) Uani 1 1 d . . . H37A H 0.3387 0.2365 0.0649 0.060 Uiso 1 1 calc R . . C38A C 0.2720(6) 0.2154(9) 0.0868(5) 0.056(4) Uani 1 1 d . . . H38A H 0.2429 0.2326 0.0558 0.068 Uiso 1 1 calc R . . C39A C 0.2603(6) 0.1849(9) 0.1279(5) 0.059(4) Uani 1 1 d . . . H39A H 0.2223 0.1790 0.1238 0.070 Uiso 1 1 calc R . . C40A C 0.3011(6) 0.1626(9) 0.1744(5) 0.060(4) Uani 1 1 d . . . H40A H 0.2907 0.1416 0.2011 0.072 Uiso 1 1 calc R . . C41A C 0.5591(5) 0.0777(9) 0.2921(5) 0.048(3) Uani 1 1 d . . . H41A H 0.5771 0.0360 0.3216 0.058 Uiso 1 1 calc R . . H41B H 0.5567 0.0432 0.2612 0.058 Uiso 1 1 calc R . . C42A C 0.6521(5) 0.1547(8) 0.3092(4) 0.044(3) Uani 1 1 d . . . H42A H 0.6586 0.1373 0.2784 0.052 Uiso 1 1 calc R . . H42B H 0.6677 0.1044 0.3348 0.052 Uiso 1 1 calc R . . U2 U 0.243706(19) 0.78759(3) -0.032828(17) 0.04175(15) Uani 1 1 d . . . O1B O 0.2492(3) 0.6993(5) -0.0969(3) 0.047(2) Uani 1 1 d . . . O2B O 0.1979(4) 0.6164(6) -0.0289(4) 0.055(2) Uani 1 1 d . . . O3B O 0.1860(3) 0.7941(5) 0.0106(3) 0.047(2) Uani 1 1 d . . . O4B O 0.2906(3) 0.8827(6) 0.0768(3) 0.047(2) Uani 1 1 d . . . O5B O 0.3018(3) 0.9121(5) -0.0239(3) 0.040(2) Uani 1 1 d . . . O6B O 0.3772(3) 0.7553(5) -0.0477(3) 0.042(2) Uani 1 1 d . . . O7B O 0.1894(3) 0.8551(5) -0.0806(3) 0.045(2) Uani 1 1 d . . . O8B O 0.2988(3) 0.7212(5) 0.0140(3) 0.0390(19) Uani 1 1 d . . . C1B C 0.3332(5) 0.6071(8) -0.0828(4) 0.039(3) Uani 1 1 d . . . C2B C 0.2785(5) 0.6144(8) -0.0855(4) 0.039(3) Uani 1 1 d . . . C3B C 0.2514(5) 0.5346(9) -0.0728(4) 0.039(3) Uani 1 1 d . . . C4B C 0.2813(5) 0.4478(8) -0.0583(4) 0.037(3) Uani 1 1 d . . . H4B H 0.2637 0.3944 -0.0505 0.044 Uiso 1 1 calc R . . C5B C 0.3375(5) 0.4408(8) -0.0554(4) 0.035(3) Uani 1 1 d . . . C6B C 0.3631(5) 0.5207(8) -0.0671(4) 0.039(3) Uani 1 1 d . . . H6B H 0.4007 0.5166 -0.0645 0.047 Uiso 1 1 calc R . . C7B C 0.3692(5) 0.3491(8) -0.0347(4) 0.039(3) Uani 1 1 d . . . C8B C 0.4260(5) 0.3502(9) 0.0016(4) 0.045(3) Uani 1 1 d . . . H8B H 0.4456 0.4083 0.0113 0.055 Uiso 1 1 calc R . . C9B C 0.4522(5) 0.2634(9) 0.0225(4) 0.048(3) Uani 1 1 d . . . H9B H 0.4893 0.2637 0.0469 0.057 Uiso 1 1 calc R . . C10B C 0.4237(6) 0.1771(11) 0.0076(5) 0.061(4) Uani 1 1 d . . . H10B H 0.4421 0.1201 0.0224 0.074 Uiso 1 1 calc R . . C11B C 0.3699(6) 0.1727(9) -0.0282(5) 0.051(3) Uani 1 1 d . . . H11B H 0.3512 0.1138 -0.0380 0.061 Uiso 1 1 calc R . . C12B C 0.3432(5) 0.2588(9) -0.0498(4) 0.048(3) Uani 1 1 d . . . H12B H 0.3067 0.2563 -0.0753 0.057 Uiso 1 1 calc R . . C13B C 0.1932(5) 0.5468(9) -0.0700(5) 0.052(4) Uani 1 1 d . . . H13C H 0.1660 0.5702 -0.1028 0.063 Uiso 1 1 calc R . . H13D H 0.1797 0.4851 -0.0627 0.063 Uiso 1 1 calc R . . C14B C 0.1590(6) 0.6013(10) -0.0030(6) 0.065(4) Uani 1 1 d . . . H14C H 0.1523 0.5327 -0.0009 0.078 Uiso 1 1 calc R . . H14D H 0.1228 0.6323 -0.0222 0.078 Uiso 1 1 calc R . . C15B C 0.1846(5) 0.6431(9) 0.0500(6) 0.048(3) Uani 1 1 d . . . C16B C 0.1985(5) 0.7423(9) 0.0547(5) 0.043(3) Uani 1 1 d . . . C17B C 0.2284(5) 0.7849(8) 0.1011(4) 0.038(3) Uani 1 1 d . . . C18B C 0.2388(5) 0.7316(9) 0.1461(5) 0.048(3) Uani 1 1 d . . . H18B H 0.2570 0.7609 0.1781 0.058 Uiso 1 1 calc R . . C19B C 0.2226(6) 0.6378(11) 0.1437(6) 0.055(4) Uani 1 1 d . . . C20B C 0.1958(6) 0.5935(10) 0.0962(7) 0.063(4) Uani 1 1 d . . . H20B H 0.1851 0.5290 0.0951 0.076 Uiso 1 1 calc R . . C21B C 0.2378(7) 0.5786(11) 0.1940(7) 0.074(5) Uani 1 1 d . . . C22B C 0.2849(8) 0.6066(13) 0.2368(6) 0.082(5) Uani 1 1 d . . . H22B H 0.3064 0.6602 0.2354 0.099 Uiso 1 1 calc R . . C23B C 0.2999(9) 0.5504(15) 0.2836(7) 0.109(7) Uani 1 1 d . . . H23B H 0.3298 0.5696 0.3136 0.131 Uiso 1 1 calc R . . C24B C 0.2698(9) 0.4703(15) 0.2832(8) 0.103(6) Uani 1 1 d U . . H24B H 0.2838 0.4286 0.3113 0.123 Uiso 1 1 calc R . . C25B C 0.2206(9) 0.4472(13) 0.2443(7) 0.103(6) Uani 1 1 d U . . H25B H 0.1972 0.3983 0.2478 0.123 Uiso 1 1 calc R . . C26B C 0.2051(9) 0.5025(14) 0.1958(8) 0.101(6) Uani 1 1 d U . . H26B H 0.1733 0.4852 0.1669 0.122 Uiso 1 1 calc R . . C27B C 0.2511(5) 0.8851(8) 0.1020(4) 0.041(3) Uani 1 1 d . . . H27C H 0.2201 0.9293 0.0842 0.049 Uiso 1 1 calc R . . H27D H 0.2700 0.9070 0.1373 0.049 Uiso 1 1 calc R . . C28B C 0.3141(5) 0.9752(8) 0.0752(4) 0.042(3) Uani 1 1 d . . . H28C H 0.3263 1.0060 0.1088 0.051 Uiso 1 1 calc R . . H28D H 0.2859 1.0163 0.0503 0.051 Uiso 1 1 calc R . . C29B C 0.3651(5) 0.9592(8) 0.0596(5) 0.038(3) Uani 1 1 d . . . C30B C 0.3555(5) 0.9244(8) 0.0100(4) 0.041(3) Uani 1 1 d . . . C31B C 0.4017(5) 0.9014(8) -0.0034(4) 0.037(3) Uani 1 1 d . . . C32B C 0.4567(5) 0.9198(8) 0.0319(5) 0.044(3) Uani 1 1 d . . . H32B H 0.4874 0.9041 0.0230 0.053 Uiso 1 1 calc R . . C33B C 0.4675(5) 0.9606(8) 0.0797(5) 0.043(3) Uani 1 1 d . . . C34B C 0.4211(5) 0.9766(8) 0.0940(4) 0.040(3) Uani 1 1 d . . . H34B H 0.4276 0.9992 0.1270 0.049 Uiso 1 1 calc R . . C35B C 0.5259(5) 0.9890(8) 0.1160(4) 0.039(3) Uani 1 1 d . . . C36B C 0.5738(5) 0.9316(9) 0.1225(4) 0.047(3) Uani 1 1 d . . . H36B H 0.5687 0.8734 0.1047 0.057 Uiso 1 1 calc R . . C37B C 0.6281(5) 0.9588(10) 0.1543(5) 0.057(4) Uani 1 1 d . . . H37B H 0.6592 0.9195 0.1580 0.068 Uiso 1 1 calc R . . C38B C 0.6357(6) 1.0454(10) 0.1807(5) 0.055(4) Uani 1 1 d . . . H38B H 0.6722 1.0644 0.2023 0.066 Uiso 1 1 calc R . . C39B C 0.5893(5) 1.1040(9) 0.1752(5) 0.048(3) Uani 1 1 d . . . H39B H 0.5942 1.1622 0.1930 0.058 Uiso 1 1 calc R . . C40B C 0.5366(5) 1.0745(9) 0.1432(4) 0.045(3) Uani 1 1 d . . . H40B H 0.5058 1.1145 0.1393 0.054 Uiso 1 1 calc R . . C41B C 0.3912(5) 0.8539(7) -0.0547(4) 0.036(3) Uani 1 1 d . . . H41C H 0.3598 0.8849 -0.0821 0.043 Uiso 1 1 calc R . . H41D H 0.4250 0.8569 -0.0629 0.043 Uiso 1 1 calc R . . C42B C 0.3605(5) 0.6966(8) -0.0924(4) 0.044(3) Uani 1 1 d . . . H42C H 0.3935 0.6799 -0.1001 0.053 Uiso 1 1 calc R . . H42D H 0.3337 0.7314 -0.1216 0.053 Uiso 1 1 calc R . . N1 N 0.5200(5) 0.4727(9) 0.2870(4) 0.068(4) Uani 1 1 d . . . H1 H 0.4877 0.5291 0.2612 0.081 Uiso 1 1 d R . . N2 N 0.4093(4) 0.6268(6) 0.1049(3) 0.035(2) Uani 1 1 d . . . H2 H 0.4474 0.5966 0.1314 0.042 Uiso 1 1 d R . . O1 O 0.3955(4) 0.4934(6) 0.2369(3) 0.057(2) Uani 1 1 d . . . O2 O 0.3662(3) 0.4556(5) 0.1311(3) 0.043(2) Uani 1 1 d . . . O3 O 0.5309(4) 0.6686(8) 0.2894(3) 0.068(3) Uani 1 1 d . . . O4 O 0.4551(3) 0.7296(6) 0.1960(3) 0.058(2) Uani 1 1 d . . . O5 O 0.5141(3) 0.4980(6) 0.1809(3) 0.048(2) Uani 1 1 d . . . O6 O 0.5078(3) 0.5752(6) 0.0878(3) 0.045(2) Uani 1 1 d . . . C1 C 0.4738(6) 0.4163(11) 0.2995(5) 0.066(4) Uani 1 1 d . . . H1A H 0.4628 0.3589 0.2781 0.079 Uiso 1 1 calc R . . H1B H 0.4894 0.3961 0.3353 0.079 Uiso 1 1 calc R . . C2 C 0.4233(6) 0.4771(12) 0.2901(5) 0.074(5) Uani 1 1 d . . . H2A H 0.3975 0.4452 0.3032 0.088 Uiso 1 1 calc R . . H2B H 0.4347 0.5383 0.3080 0.088 Uiso 1 1 calc R . . C3 C 0.3617(6) 0.4109(9) 0.2118(5) 0.057(4) Uani 1 1 d . . . H3A H 0.3362 0.3933 0.2287 0.068 Uiso 1 1 calc R . . H3B H 0.3863 0.3562 0.2135 0.068 Uiso 1 1 calc R . . C4 C 0.3276(5) 0.4375(9) 0.1559(5) 0.048(3) Uani 1 1 d . . . H4C H 0.3020 0.3851 0.1387 0.057 Uiso 1 1 calc R . . H4D H 0.3048 0.4947 0.1543 0.057 Uiso 1 1 calc R . . C5 C 0.3368(5) 0.4931(8) 0.0806(4) 0.043(3) Uani 1 1 d . . . H5A H 0.3054 0.5339 0.0799 0.051 Uiso 1 1 calc R . . H5B H 0.3216 0.4407 0.0562 0.051 Uiso 1 1 calc R . . C6 C 0.3788(5) 0.5505(8) 0.0669(4) 0.038(3) Uani 1 1 d . . . H6C H 0.4069 0.5066 0.0633 0.045 Uiso 1 1 calc R . . H6D H 0.3590 0.5808 0.0336 0.045 Uiso 1 1 calc R . . C7 C 0.5587(6) 0.5228(12) 0.3317(5) 0.071(5) Uani 1 1 d . . . H7A H 0.5905 0.4809 0.3505 0.086 Uiso 1 1 calc R . . H7B H 0.5392 0.5392 0.3544 0.086 Uiso 1 1 calc R . . C8 C 0.5803(5) 0.6121(12) 0.3163(6) 0.077(5) Uani 1 1 d . . . H8C H 0.6059 0.6465 0.3464 0.092 Uiso 1 1 calc R . . H8D H 0.6006 0.5970 0.2941 0.092 Uiso 1 1 calc R . . C9 C 0.5419(6) 0.7561(11) 0.2670(6) 0.079(5) Uani 1 1 d . . . H9C H 0.5632 0.7418 0.2456 0.095 Uiso 1 1 calc R . . H9D H 0.5640 0.8007 0.2939 0.095 Uiso 1 1 calc R . . C10 C 0.4845(6) 0.7997(11) 0.2348(5) 0.084(5) Uani 1 1 d . . . H10C H 0.4629 0.8133 0.2562 0.101 Uiso 1 1 calc R . . H10D H 0.4894 0.8595 0.2190 0.101 Uiso 1 1 calc R . . C11 C 0.4008(5) 0.7595(8) 0.1639(4) 0.049(3) Uani 1 1 d . . . H11C H 0.4034 0.8146 0.1434 0.059 Uiso 1 1 calc R . . H11D H 0.3790 0.7784 0.1842 0.059 Uiso 1 1 calc R . . C12 C 0.3720(5) 0.6753(8) 0.1289(4) 0.044(3) Uani 1 1 d . . . H12C H 0.3609 0.6278 0.1487 0.052 Uiso 1 1 calc R . . H12D H 0.3375 0.6984 0.1016 0.052 Uiso 1 1 calc R . . C13 C 0.5496(6) 0.4081(10) 0.2613(5) 0.054(4) Uani 1 1 d . . . H13E H 0.5879 0.4318 0.2685 0.065 Uiso 1 1 calc R . . H13F H 0.5524 0.3429 0.2747 0.065 Uiso 1 1 calc R . . C14 C 0.5163(5) 0.4081(10) 0.2053(5) 0.056(4) Uani 1 1 d . . . H14E H 0.5327 0.3608 0.1894 0.067 Uiso 1 1 calc R . . H14F H 0.4777 0.3878 0.1991 0.067 Uiso 1 1 calc R . . C15 C 0.5645(5) 0.5176(10) 0.1705(5) 0.055(4) Uani 1 1 d . . . H15A H 0.5742 0.4619 0.1544 0.066 Uiso 1 1 calc R . . H15B H 0.5965 0.5317 0.2023 0.066 Uiso 1 1 calc R . . C16 C 0.5514(5) 0.6033(9) 0.1348(5) 0.051(3) Uani 1 1 d . . . H16A H 0.5388 0.6574 0.1498 0.061 Uiso 1 1 calc R . . H16B H 0.5853 0.6228 0.1290 0.061 Uiso 1 1 calc R . . C17 C 0.4743(5) 0.6526(8) 0.0570(5) 0.044(3) Uani 1 1 d . . . H17A H 0.4508 0.6280 0.0232 0.052 Uiso 1 1 calc R . . H17B H 0.4996 0.7013 0.0526 0.052 Uiso 1 1 calc R . . C18 C 0.4367(5) 0.6984(9) 0.0811(5) 0.051(3) Uani 1 1 d . . . H18C H 0.4593 0.7434 0.1075 0.061 Uiso 1 1 calc R . . H18D H 0.4070 0.7350 0.0550 0.061 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 0.0510(3) 0.0432(3) 0.0394(3) 0.0005(2) 0.0192(2) -0.0049(2) O1A 0.043(5) 0.050(5) 0.041(5) 0.001(4) 0.013(4) 0.001(4) O2A 0.050(5) 0.053(6) 0.049(5) -0.012(4) 0.026(4) -0.013(4) O3A 0.049(5) 0.047(5) 0.043(5) 0.001(4) 0.022(4) -0.005(4) O4A 0.073(6) 0.066(6) 0.054(5) -0.022(5) 0.045(5) -0.031(5) O5A 0.068(6) 0.053(6) 0.040(5) 0.001(4) 0.026(5) -0.016(4) O6A 0.046(5) 0.031(5) 0.071(6) -0.001(4) 0.024(5) -0.003(4) O7A 0.067(6) 0.053(6) 0.051(5) 0.021(4) 0.023(5) 0.003(4) O8A 0.045(5) 0.051(5) 0.040(5) -0.011(4) 0.014(4) 0.001(4) C1A 0.035(6) 0.033(7) 0.036(6) -0.003(5) 0.013(5) 0.000(5) C2A 0.026(6) 0.053(8) 0.035(6) 0.001(6) 0.004(5) 0.010(6) C3A 0.051(8) 0.042(8) 0.028(6) 0.000(5) -0.001(6) -0.001(6) C4A 0.035(7) 0.029(6) 0.038(7) 0.003(5) 0.011(6) 0.001(5) C5A 0.023(6) 0.046(7) 0.031(6) 0.003(5) 0.013(5) -0.007(5) C6A 0.049(8) 0.038(7) 0.027(6) -0.008(5) 0.012(6) -0.001(5) C7A 0.030(7) 0.049(8) 0.059(9) -0.005(6) 0.019(6) 0.006(6) C8A 0.038(7) 0.059(9) 0.044(8) 0.015(6) 0.015(6) -0.001(6) C9A 0.046(8) 0.044(9) 0.078(11) 0.002(7) 0.013(8) 0.002(6) C10A 0.040(8) 0.072(11) 0.038(8) 0.016(7) 0.004(6) 0.003(7) C11A 0.040(8) 0.073(10) 0.037(7) 0.008(7) 0.001(6) -0.009(7) C12A 0.035(7) 0.065(9) 0.043(8) 0.000(7) 0.015(6) -0.004(6) C13A 0.046(8) 0.048(8) 0.045(8) -0.007(6) 0.016(6) 0.001(6) C14A 0.041(8) 0.069(9) 0.035(7) -0.019(6) 0.021(6) -0.002(6) C15A 0.055(9) 0.047(8) 0.031(7) -0.017(6) 0.018(6) -0.012(6) C16A 0.042(8) 0.062(9) 0.028(7) 0.007(6) 0.020(6) 0.002(7) C17A 0.045(8) 0.060(9) 0.042(7) -0.002(6) 0.028(6) -0.003(7) C18A 0.042(8) 0.087(11) 0.024(6) -0.007(6) 0.018(6) 0.004(7) C19A 0.043(8) 0.063(9) 0.044(8) -0.005(6) 0.018(7) -0.012(7) C20A 0.055(9) 0.040(8) 0.046(8) -0.013(6) 0.023(7) -0.003(6) C21A 0.052(9) 0.095(12) 0.051(8) 0.021(8) 0.033(7) 0.020(8) C22A 0.070(10) 0.064(11) 0.076(10) 0.005(8) 0.046(8) -0.004(8) C23A 0.085(13) 0.075(13) 0.116(15) 0.007(11) 0.035(12) -0.006(10) C24A 0.109(10) 0.090(9) 0.113(10) 0.020(8) 0.046(8) 0.002(8) C25A 0.112(10) 0.115(10) 0.111(10) 0.022(8) 0.051(8) 0.011(8) C26A 0.083(8) 0.075(8) 0.074(8) 0.028(6) 0.041(6) 0.000(7) C27A 0.055(9) 0.093(11) 0.033(7) -0.004(7) 0.038(6) 0.004(7) C28A 0.046(7) 0.062(9) 0.045(7) -0.005(6) 0.025(6) -0.013(6) C29A 0.047(8) 0.036(7) 0.062(9) -0.013(6) 0.026(7) -0.008(6) C30A 0.052(8) 0.043(8) 0.032(7) 0.000(5) 0.018(6) -0.013(6) C31A 0.057(8) 0.039(7) 0.038(7) -0.007(5) 0.027(7) -0.017(6) C32A 0.059(9) 0.034(7) 0.043(7) -0.007(5) 0.025(7) -0.019(6) C33A 0.048(8) 0.046(8) 0.040(7) -0.011(6) 0.017(7) -0.002(6) C34A 0.042(7) 0.049(8) 0.042(7) -0.017(6) 0.014(6) -0.020(6) C35A 0.057(9) 0.045(8) 0.066(9) -0.022(7) 0.042(8) -0.011(6) C36A 0.060(9) 0.052(9) 0.071(10) -0.026(7) 0.044(8) -0.009(7) C37A 0.058(9) 0.057(9) 0.026(6) -0.007(6) 0.004(6) -0.011(7) C38A 0.056(9) 0.061(9) 0.045(8) -0.023(7) 0.011(7) -0.003(7) C39A 0.056(9) 0.064(10) 0.059(9) -0.015(7) 0.026(8) -0.008(7) C40A 0.071(10) 0.055(9) 0.053(9) -0.007(7) 0.024(8) -0.008(7) C41A 0.042(8) 0.053(8) 0.051(8) -0.002(6) 0.019(7) 0.000(6) C42A 0.045(8) 0.048(8) 0.040(7) -0.004(6) 0.018(6) 0.002(6) U2 0.0371(3) 0.0376(3) 0.0437(3) 0.0015(2) 0.0078(2) 0.0032(2) O1B 0.043(5) 0.043(5) 0.045(5) 0.004(4) 0.006(4) 0.008(4) O2B 0.055(6) 0.043(5) 0.077(7) -0.012(5) 0.036(5) 0.005(4) O3B 0.038(5) 0.041(5) 0.057(5) -0.005(4) 0.012(4) 0.002(4) O4B 0.041(5) 0.049(5) 0.057(6) -0.010(4) 0.026(4) -0.004(4) O5B 0.033(5) 0.042(5) 0.037(4) -0.006(4) 0.007(4) 0.000(4) O6B 0.062(5) 0.039(5) 0.032(4) -0.002(3) 0.024(4) 0.002(4) O7B 0.042(5) 0.040(5) 0.046(5) -0.001(4) 0.008(4) 0.007(4) O8B 0.028(4) 0.045(5) 0.039(4) 0.000(4) 0.007(3) 0.004(4) C1B 0.047(8) 0.041(7) 0.029(6) -0.009(5) 0.014(6) 0.001(6) C2B 0.041(8) 0.037(7) 0.031(7) 0.001(5) 0.004(6) -0.004(6) C3B 0.024(6) 0.052(8) 0.042(7) -0.013(6) 0.014(6) -0.004(5) C4B 0.045(8) 0.032(7) 0.024(6) -0.005(5) 0.002(6) -0.006(5) C5B 0.040(7) 0.036(7) 0.027(6) -0.005(5) 0.010(6) -0.003(5) C6B 0.041(7) 0.053(8) 0.027(6) -0.006(5) 0.015(6) 0.005(6) C7B 0.055(8) 0.034(7) 0.035(7) 0.000(5) 0.026(6) 0.002(6) C8B 0.049(8) 0.052(9) 0.035(7) 0.001(6) 0.017(6) -0.006(6) C9B 0.035(7) 0.056(9) 0.043(7) 0.006(6) 0.006(6) 0.023(6) C10B 0.075(11) 0.066(11) 0.059(9) 0.007(8) 0.043(9) 0.026(8) C11B 0.061(9) 0.047(8) 0.050(8) 0.009(6) 0.028(7) 0.005(7) C12B 0.044(7) 0.059(9) 0.044(7) 0.003(6) 0.022(6) 0.009(6) C13B 0.035(7) 0.051(9) 0.072(10) -0.011(7) 0.021(7) -0.006(6) C14B 0.052(9) 0.046(9) 0.103(13) -0.007(8) 0.035(9) -0.004(7) C15B 0.027(7) 0.048(9) 0.073(10) -0.012(7) 0.023(7) 0.002(6) C16B 0.033(7) 0.057(9) 0.047(7) 0.008(6) 0.024(6) 0.015(6) C17B 0.043(7) 0.030(7) 0.041(7) 0.011(6) 0.018(6) 0.006(6) C18B 0.052(8) 0.056(9) 0.046(7) 0.001(6) 0.030(6) 0.009(7) C19B 0.054(9) 0.066(10) 0.070(10) 0.007(8) 0.051(8) 0.007(7) C20B 0.057(9) 0.044(9) 0.108(13) -0.008(9) 0.052(9) -0.006(7) C21B 0.089(12) 0.054(10) 0.112(15) 0.003(10) 0.076(12) 0.020(9) C22B 0.110(15) 0.095(14) 0.050(10) -0.002(9) 0.039(10) 0.012(11) C23B 0.141(19) 0.114(17) 0.075(14) -0.021(12) 0.044(13) 0.005(14) C24B 0.111(10) 0.102(10) 0.107(10) 0.005(8) 0.055(8) -0.006(8) C25B 0.113(10) 0.099(9) 0.093(9) 0.018(8) 0.035(8) 0.005(8) C26B 0.116(10) 0.102(10) 0.106(10) -0.006(8) 0.064(8) 0.006(8) C27B 0.042(7) 0.052(8) 0.033(7) -0.013(6) 0.019(6) -0.004(6) C28B 0.059(8) 0.036(7) 0.040(7) -0.010(5) 0.028(6) -0.025(6) C29B 0.030(7) 0.033(7) 0.049(8) -0.002(5) 0.013(6) 0.002(5) C30B 0.049(8) 0.033(7) 0.040(7) 0.006(5) 0.015(6) -0.003(6) C31B 0.035(7) 0.043(7) 0.038(7) 0.001(5) 0.021(6) 0.000(5) C32B 0.033(7) 0.039(7) 0.057(8) 0.002(6) 0.015(6) 0.001(5) C33B 0.052(8) 0.035(7) 0.041(7) 0.000(5) 0.017(6) -0.013(6) C34B 0.039(7) 0.051(8) 0.040(7) -0.019(6) 0.025(6) -0.014(6) C35B 0.037(7) 0.042(7) 0.040(7) -0.001(6) 0.017(6) 0.001(6) C36B 0.058(9) 0.051(8) 0.043(8) -0.002(6) 0.030(7) 0.011(7) C37B 0.024(7) 0.078(11) 0.057(9) -0.002(8) 0.002(7) -0.005(6) C38B 0.057(9) 0.075(10) 0.030(7) -0.003(7) 0.013(7) -0.013(8) C39B 0.028(7) 0.060(9) 0.046(8) -0.008(6) 0.002(6) -0.008(6) C40B 0.044(8) 0.062(9) 0.028(6) -0.002(6) 0.011(6) 0.002(6) C41B 0.039(7) 0.028(7) 0.042(7) 0.004(5) 0.018(6) 0.000(5) C42B 0.053(8) 0.042(8) 0.046(7) -0.004(6) 0.030(6) 0.009(6) N1 0.069(9) 0.095(10) 0.043(7) 0.017(6) 0.024(6) 0.022(7) N2 0.038(6) 0.031(5) 0.038(6) -0.004(4) 0.016(5) 0.000(4) O1 0.070(6) 0.062(6) 0.035(5) -0.004(4) 0.017(5) -0.014(5) O2 0.048(5) 0.045(5) 0.032(4) 0.007(4) 0.012(4) 0.003(4) O3 0.061(7) 0.081(7) 0.052(6) -0.006(5) 0.012(5) 0.001(6) O4 0.039(5) 0.068(6) 0.044(5) -0.005(4) -0.009(4) 0.007(4) O5 0.045(5) 0.067(6) 0.036(5) 0.008(4) 0.021(4) 0.009(4) O6 0.039(5) 0.059(6) 0.034(5) 0.007(4) 0.011(4) 0.010(4) C1 0.070(11) 0.094(12) 0.052(9) 0.019(8) 0.043(8) 0.013(9) C2 0.068(11) 0.119(14) 0.038(8) -0.008(8) 0.025(8) -0.011(10) C3 0.077(10) 0.042(8) 0.050(8) -0.015(6) 0.024(8) -0.023(7) C4 0.043(8) 0.051(8) 0.056(8) -0.003(6) 0.027(7) -0.007(6) C5 0.048(8) 0.040(7) 0.041(7) -0.010(6) 0.018(6) -0.001(6) C6 0.045(7) 0.040(7) 0.028(6) -0.002(5) 0.015(6) 0.009(5) C7 0.050(10) 0.115(14) 0.049(9) -0.012(9) 0.019(8) 0.010(9) C8 0.021(7) 0.106(13) 0.075(11) -0.037(10) -0.011(8) 0.013(8) C9 0.055(10) 0.088(12) 0.074(10) -0.033(9) 0.000(8) -0.022(9) C10 0.077(11) 0.084(12) 0.060(9) -0.029(8) -0.010(9) -0.002(9) C11 0.057(8) 0.050(8) 0.043(7) 0.000(6) 0.021(6) 0.002(6) C12 0.047(8) 0.043(7) 0.045(7) -0.004(6) 0.023(6) 0.007(6) C13 0.057(9) 0.074(10) 0.049(8) 0.029(7) 0.039(7) 0.023(7) C14 0.049(8) 0.073(10) 0.052(8) 0.000(7) 0.027(7) 0.015(7) C15 0.042(8) 0.086(11) 0.043(8) 0.020(7) 0.023(7) 0.018(7) C16 0.040(8) 0.058(9) 0.054(8) 0.006(7) 0.017(7) -0.001(6) C17 0.045(8) 0.026(7) 0.055(8) -0.002(6) 0.015(6) 0.002(5) C18 0.050(8) 0.052(9) 0.044(7) 0.012(6) 0.010(6) -0.004(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 O8A 1.768(8) . ? U1 O7A 1.775(7) . ? U1 O3A 2.203(8) . ? U1 O5A 2.228(8) . ? U1 O1A 2.227(8) . ? U1 O2A 2.609(8) . ? U1 O4A 3.478(9) . ? U1 O6A 3.692(9) . ? O1A C2A 1.348(13) . ? O2A C13A 1.456(14) . ? O2A C14A 1.467(13) . ? O3A C16A 1.308(13) . ? O4A C28A 1.423(13) . ? O4A C27A 1.447(13) . ? O5A C30A 1.352(12) . ? O6A C42A 1.433(13) . ? O6A C41A 1.477(13) . ? C1A C6A 1.351(15) . ? C1A C2A 1.417(15) . ? C1A C42A 1.500(14) . ? C2A C3A 1.401(15) . ? C3A C4A 1.396(15) . ? C3A C13A 1.483(16) . ? C4A C5A 1.422(14) . ? C5A C6A 1.409(14) . ? C5A C7A 1.490(16) . ? C7A C8A 1.375(16) . ? C7A C12A 1.393(17) . ? C8A C9A 1.399(17) . ? C9A C10A 1.390(18) . ? C10A C11A 1.379(17) . ? C11A C12A 1.408(16) . ? C14A C15A 1.503(16) . ? C15A C20A 1.379(16) . ? C15A C16A 1.425(16) . ? C16A C17A 1.397(16) . ? C17A C18A 1.378(16) . ? C17A C27A 1.555(17) . ? C18A C19A 1.395(17) . ? C19A C20A 1.401(16) . ? C19A C21A 1.530(18) . ? C21A C22A 1.343(18) . ? C21A C26A 1.376(19) . ? C22A C23A 1.412(19) . ? C23A C24A 1.37(2) . ? C24A C25A 1.41(2) . ? C25A C26A 1.41(2) . ? C28A C29A 1.505(16) . ? C29A C34A 1.404(16) . ? C29A C30A 1.396(16) . ? C30A C31A 1.415(16) . ? C31A C32A 1.375(15) . ? C31A C41A 1.499(16) . ? C32A C33A 1.399(16) . ? C33A C34A 1.380(16) . ? C33A C35A 1.498(17) . ? C35A C36A 1.392(17) . ? C35A C40A 1.421(17) . ? C36A C37A 1.380(16) . ? C37A C38A 1.397(17) . ? C38A C39A 1.364(18) . ? C39A C40A 1.356(17) . ? U2 O8B 1.766(6) . ? U2 O7B 1.776(7) . ? U2 O5B 2.217(7) . ? U2 O1B 2.222(8) . ? U2 O3B 2.234(9) . ? U2 O2B 2.658(9) . ? U2 O4B 3.132(8) . ? U2 O6B 3.594(8) . ? O1B C2B 1.362(13) . ? O2B C14B 1.447(16) . ? O2B C13B 1.473(14) . ? O3B C16B 1.360(13) . ? O4B C28B 1.419(12) . ? O4B C27B 1.432(13) . ? O5B C30B 1.342(12) . ? O6B C42B 1.416(12) . ? O6B C41B 1.442(12) . ? C1B C2B 1.363(16) . ? C1B C6B 1.395(15) . ? C1B C42B 1.491(16) . ? C2B C3B 1.416(16) . ? C3B C4B 1.395(15) . ? C3B C13B 1.518(16) . ? C4B C5B 1.399(16) . ? C5B C6B 1.385(15) . ? C5B C7B 1.495(15) . ? C7B C12B 1.400(15) . ? C7B C8B 1.410(15) . ? C8B C9B 1.390(15) . ? C9B C10B 1.375(17) . ? C10B C11B 1.352(17) . ? C11B C12B 1.389(15) . ? C14B C15B 1.492(18) . ? C15B C16B 1.410(16) . ? C15B C20B 1.397(18) . ? C16B C17B 1.364(15) . ? C17B C18B 1.399(15) . ? C17B C27B 1.497(15) . ? C18B C19B 1.356(17) . ? C19B C20B 1.387(18) . ? C19B C21B 1.55(2) . ? C21B C26B 1.35(2) . ? C21B C22B 1.39(2) . ? C22B C23B 1.45(2) . ? C23B C24B 1.34(2) . ? C24B C25B 1.35(2) . ? C25B C26B 1.48(2) . ? C28B C29B 1.532(16) . ? C29B C34B 1.400(14) . ? C29B C30B 1.405(16) . ? C30B C31B 1.397(16) . ? C31B C32B 1.390(14) . ? C31B C41B 1.511(15) . ? C32B C33B 1.385(16) . ? C33B C34B 1.397(16) . ? C33B C35B 1.494(15) . ? C35B C40B 1.377(15) . ? C35B C36B 1.403(15) . ? C36B C37B 1.378(15) . ? C37B C38B 1.382(17) . ? C38B C39B 1.388(17) . ? C39B C40B 1.359(14) . ? N1 C7 1.441(16) . ? N1 C13 1.515(16) . ? N1 C1 1.555(17) . ? N2 C6 1.490(12) . ? N2 C18 1.504(14) . ? N2 C12 1.511(14) . ? O1 C2 1.405(14) . ? O1 C3 1.440(13) . ? O2 C5 1.424(12) . ? O2 C4 1.422(14) . ? O3 C9 1.439(17) . ? O3 C8 1.424(14) . ? O4 C11 1.389(13) . ? O4 C10 1.436(14) . ? O5 C14 1.409(14) . ? O5 C15 1.441(14) . ? O6 C16 1.414(13) . ? O6 C17 1.434(12) . ? C1 C2 1.468(18) . ? C3 C4 1.518(16) . ? C5 C6 1.493(16) . ? C7 C8 1.48(2) . ? C9 C10 1.516(18) . ? C11 C12 1.519(15) . ? C13 C14 1.474(16) . ? C15 C16 1.506(16) . ? C17 C18 1.504(16) . ? 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 O8A U1 O7A 177.0(4) . . ? O8A U1 O3A 93.4(3) . . ? O7A U1 O3A 89.6(4) . . ? O8A U1 O5A 87.6(3) . . ? O7A U1 O5A 91.4(3) . . ? O3A U1 O5A 112.6(3) . . ? O8A U1 O1A 89.7(3) . . ? O7A U1 O1A 87.9(4) . . ? O3A U1 O1A 139.3(3) . . ? O5A U1 O1A 108.1(3) . . ? O8A U1 O2A 77.6(3) . . ? O7A U1 O2A 103.4(3) . . ? O3A U1 O2A 70.0(3) . . ? O5A U1 O2A 165.1(3) . . ? O1A U1 O2A 71.1(3) . . ? O8A U1 O4A 62.4(3) . . ? O7A U1 O4A 119.5(3) . . ? O3A U1 O4A 57.5(2) . . ? O5A U1 O4A 64.3(3) . . ? O1A U1 O4A 150.6(2) . . ? O2A U1 O4A 108.7(2) . . ? O8A U1 O6A 56.1(3) . . ? O7A U1 O6A 121.0(3) . . ? O3A U1 O6A 147.9(2) . . ? O5A U1 O6A 61.5(2) . . ? O1A U1 O6A 58.6(2) . . ? O2A U1 O6A 108.1(2) . . ? O4A U1 O6A 95.61(18) . . ? C13A O2A C14A 114.7(8) . . ? C28A O4A C27A 115.2(9) . . ? C42A O6A C41A 115.5(8) . . ? C6A C1A C2A 118.7(10) . . ? C6A C1A C42A 122.4(10) . . ? C2A C1A C42A 118.4(11) . . ? O1A C2A C3A 118.6(10) . . ? O1A C2A C1A 120.9(11) . . ? C3A C2A C1A 120.5(11) . . ? C4A C3A C2A 118.4(11) . . ? C4A C3A C13A 122.0(11) . . ? C2A C3A C13A 119.7(11) . . ? C3A C4A C5A 122.8(10) . . ? C6A C5A C4A 115.1(10) . . ? C6A C5A C7A 124.2(10) . . ? C4A C5A C7A 120.4(10) . . ? C1A C6A C5A 124.5(10) . . ? C8A C7A C12A 117.1(13) . . ? C8A C7A C5A 120.9(12) . . ? C12A C7A C5A 121.7(11) . . ? C7A C8A C9A 121.9(13) . . ? C8A C9A C10A 119.3(13) . . ? C11A C10A C9A 120.8(13) . . ? C10A C11A C12A 117.9(13) . . ? C7A C12A C11A 122.7(13) . . ? O2A C13A C3A 108.6(10) . . ? O2A C14A C15A 109.6(9) . . ? C20A C15A C16A 120.8(12) . . ? C20A C15A C14A 122.1(11) . . ? C16A C15A C14A 117.1(11) . . ? O3A C16A C17A 122.5(12) . . ? O3A C16A C15A 120.4(11) . . ? C17A C16A C15A 117.0(12) . . ? C18A C17A C16A 121.0(12) . . ? C18A C17A C27A 122.9(12) . . ? C16A C17A C27A 115.8(12) . . ? C17A C18A C19A 122.7(12) . . ? C18A C19A C20A 116.5(12) . . ? C18A C19A C21A 123.8(12) . . ? C20A C19A C21A 119.6(11) . . ? C15A C20A C19A 121.9(12) . . ? C22A C21A C26A 122.0(15) . . ? C22A C21A C19A 121.6(13) . . ? C26A C21A C19A 116.3(13) . . ? C21A C22A C23A 120.6(16) . . ? C24A C23A C22A 118.6(17) . . ? C23A C24A C25A 120.4(19) . . ? C26A C25A C24A 119.3(19) . . ? C21A C26A C25A 118.6(16) . . ? O4A C27A C17A 104.9(9) . . ? O4A C28A C29A 107.0(10) . . ? C34A C29A C30A 119.5(12) . . ? C34A C29A C28A 119.3(12) . . ? C30A C29A C28A 120.7(11) . . ? O5A C30A C29A 121.2(11) . . ? O5A C30A C31A 120.9(12) . . ? C29A C30A C31A 117.9(11) . . ? C32A C31A C30A 121.4(12) . . ? C32A C31A C41A 118.6(11) . . ? C30A C31A C41A 119.6(11) . . ? C31A C32A C33A 120.9(12) . . ? C34A C33A C32A 117.8(11) . . ? C34A C33A C35A 121.0(12) . . ? C32A C33A C35A 120.5(12) . . ? C33A C34A C29A 122.4(12) . . ? C36A C35A C40A 116.2(13) . . ? C36A C35A C33A 124.8(12) . . ? C40A C35A C33A 118.9(12) . . ? C35A C36A C37A 122.4(13) . . ? C36A C37A C38A 119.9(13) . . ? C39A C38A C37A 117.6(12) . . ? C40A C39A C38A 123.5(14) . . ? C39A C40A C35A 120.1(14) . . ? O6A C41A C31A 107.1(9) . . ? O6A C42A C1A 105.3(9) . . ? O8B U2 O7B 178.7(4) . . ? O8B U2 O5B 91.0(3) . . ? O7B U2 O5B 88.1(3) . . ? O8B U2 O1B 92.3(3) . . ? O7B U2 O1B 87.0(3) . . ? O5B U2 O1B 105.9(3) . . ? O8B U2 O3B 96.4(3) . . ? O7B U2 O3B 84.8(3) . . ? O5B U2 O3B 116.9(3) . . ? O1B U2 O3B 136.0(3) . . ? O8B U2 O2B 74.9(3) . . ? O7B U2 O2B 106.0(3) . . ? O5B U2 O2B 165.7(3) . . ? O1B U2 O2B 73.0(3) . . ? O3B U2 O2B 68.0(3) . . ? O8B U2 O4B 66.0(3) . . ? O7B U2 O4B 114.5(3) . . ? O5B U2 O4B 64.9(2) . . ? O1B U2 O4B 155.2(2) . . ? O3B U2 O4B 62.0(2) . . ? O2B U2 O4B 110.0(2) . . ? O8B U2 O6B 60.6(3) . . ? O7B U2 O6B 118.1(3) . . ? O5B U2 O6B 59.7(2) . . ? O1B U2 O6B 59.0(2) . . ? O3B U2 O6B 155.5(2) . . ? O2B U2 O6B 109.9(2) . . ? O4B U2 O6B 98.33(18) . . ? C14B O2B C13B 115.6(9) . . ? C28B O4B C27B 112.0(9) . . ? C42B O6B C41B 115.4(8) . . ? C2B C1B C6B 120.0(12) . . ? C2B C1B C42B 117.4(11) . . ? C6B C1B C42B 122.4(11) . . ? O1B C2B C1B 122.0(11) . . ? O1B C2B C3B 117.2(11) . . ? C1B C2B C3B 120.7(11) . . ? C4B C3B C2B 118.9(11) . . ? C4B C3B C13B 120.7(11) . . ? C2B C3B C13B 120.2(11) . . ? C3B C4B C5B 120.3(11) . . ? C6B C5B C4B 119.4(10) . . ? C6B C5B C7B 122.5(11) . . ? C4B C5B C7B 117.8(10) . . ? C1B C6B C5B 120.8(12) . . ? C12B C7B C8B 117.4(11) . . ? C12B C7B C5B 121.3(10) . . ? C8B C7B C5B 121.3(10) . . ? C9B C8B C7B 119.1(11) . . ? C10B C9B C8B 120.7(11) . . ? C11B C10B C9B 122.0(13) . . ? C10B C11B C12B 118.0(13) . . ? C11B C12B C7B 122.7(11) . . ? O2B C13B C3B 108.8(9) . . ? O2B C14B C15B 108.9(11) . . ? C16B C15B C20B 115.8(12) . . ? C16B C15B C14B 118.0(13) . . ? C20B C15B C14B 126.2(13) . . ? O3B C16B C17B 119.4(11) . . ? O3B C16B C15B 117.7(11) . . ? C17B C16B C15B 122.6(11) . . ? C16B C17B C18B 118.5(11) . . ? C16B C17B C27B 119.1(10) . . ? C18B C17B C27B 122.3(11) . . ? C19B C18B C17B 120.7(12) . . ? C18B C19B C20B 119.9(13) . . ? C18B C19B C21B 119.8(14) . . ? C20B C19B C21B 120.2(14) . . ? C19B C20B C15B 121.8(13) . . ? C26B C21B C22B 121.5(18) . . ? C26B C21B C19B 120.2(17) . . ? C22B C21B C19B 118.3(15) . . ? C21B C22B C23B 118.5(18) . . ? C24B C23B C22B 119.0(19) . . ? C23B C24B C25B 123(2) . . ? C24B C25B C26B 118(2) . . ? C21B C26B C25B 119.1(19) . . ? O4B C27B C17B 107.9(9) . . ? O4B C28B C29B 106.7(9) . . ? C34B C29B C30B 119.2(11) . . ? C34B C29B C28B 121.6(11) . . ? C30B C29B C28B 119.2(10) . . ? O5B C30B C31B 120.7(11) . . ? O5B C30B C29B 119.4(11) . . ? C31B C30B C29B 119.9(11) . . ? C32B C31B C30B 118.9(11) . . ? C32B C31B C41B 121.5(11) . . ? C30B C31B C41B 119.6(10) . . ? C33B C32B C31B 122.6(12) . . ? C32B C33B C34B 117.8(11) . . ? C32B C33B C35B 123.0(12) . . ? C34B C33B C35B 119.1(11) . . ? C33B C34B C29B 121.2(11) . . ? C40B C35B C36B 115.9(11) . . ? C40B C35B C33B 122.5(11) . . ? C36B C35B C33B 121.5(11) . . ? C37B C36B C35B 122.0(12) . . ? C36B C37B C38B 119.0(13) . . ? C39B C38B C37B 120.5(12) . . ? C40B C39B C38B 118.4(12) . . ? C39B C40B C35B 124.1(12) . . ? O6B C41B C31B 104.1(9) . . ? O6B C42B C1B 108.7(9) . . ? C7 N1 C13 113.7(11) . . ? C7 N1 C1 111.5(11) . . ? C13 N1 C1 111.4(11) . . ? C6 N2 C18 110.5(9) . . ? C6 N2 C12 113.1(9) . . ? C18 N2 C12 112.3(9) . . ? C2 O1 C3 110.8(10) . . ? C5 O2 C4 110.8(9) . . ? C9 O3 C8 114.5(12) . . ? C11 O4 C10 112.9(10) . . ? C14 O5 C15 113.0(9) . . ? C16 O6 C17 115.4(9) . . ? C2 C1 N1 110.6(12) . . ? O1 C2 C1 109.3(12) . . ? O1 C3 C4 108.1(10) . . ? O2 C4 C3 108.7(10) . . ? O2 C5 C6 107.3(9) . . ? N2 C6 C5 114.7(9) . . ? N1 C7 C8 110.6(12) . . ? O3 C8 C7 105.3(12) . . ? O3 C9 C10 107.0(12) . . ? O4 C10 C9 106.6(11) . . ? O4 C11 C12 107.7(9) . . ? N2 C12 C11 113.6(10) . . ? C14 C13 N1 108.8(10) . . ? O5 C14 C13 114.7(11) . . ? O5 C15 C16 107.2(10) . . ? O6 C16 C15 107.3(10) . . ? O6 C17 C18 112.0(10) . . ? N2 C18 C17 113.7(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O1 1.16 2.22 2.937(15) 116.7 . N1 H1 O3 1.16 2.21 2.724(16) 103.2 . N1 H1 O5 1.16 2.62 2.944(14) 94.3 . N2 H2 O4 1.05 2.54 2.764(11) 90.9 . N2 H2 O6 1.05 2.32 2.811(12) 107.0 .