# 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 # 1. SUBMISSION DETAILS _publ_contact_author 'P. Thuery' _publ_contact_address ; Dr Pierre Thuery CEA/Sacley SCM (CNRS URA 331) Bat. 125 91191 Gif-sur-Yvette FRANCE ; _publ_contact_author_phone '16(1)69 08 63 29' _publ_contact_author_fax '16(1)69 08 66 40' _publ_contact_author_email thuery@drecam.cea.fr _publ_requested_journal 'New J. Chem.' loop_ _publ_author_name 'B. Masci' 'M. Nierlich' 'P. Thuery' _publ_section_title ; Trigonal versus tetragonal or pentagonal coordination of uranyl ion by p-R-tert-butylhexahomotrioxacalix[3]arene: solid state and solution investigations. ; data_3 _database_code_CSD 172883 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H43 N O8 U' _chemical_formula_weight 819.71 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.3031(6) _cell_length_b 19.6564(8) _cell_length_c 19.6680(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6302.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 41417 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepipedic _exptl_crystal_colour 'translucent intense orange' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method ? _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 5.202 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.446 _exptl_absorpt_correction_T_max 0.594 _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 41417 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5961 _reflns_number_gt 4467 _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 atom bound to N has been found on the Fourier-difference map and introduced as a riding atom 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 (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^)+(0.0059P)^2^+10.8520P] 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 5961 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.550 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.097 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 U U 0.284079(9) -0.305462(8) 0.544024(8) 0.02330(5) Uani 1 1 d . . . O1 O 0.27679(17) -0.25560(15) 0.44251(14) 0.0265(7) Uani 1 1 d . . . O2 O 0.1441(2) -0.34366(15) 0.47659(14) 0.0294(7) Uani 1 1 d . . . O3 O 0.23754(17) -0.40386(15) 0.58349(16) 0.0275(7) Uani 1 1 d . . . O4 O 0.23573(18) -0.32866(15) 0.71471(16) 0.0294(7) Uani 1 1 d . . . O5 O 0.36970(17) -0.26676(15) 0.62229(15) 0.0262(7) Uani 1 1 d . . . O6 O 0.30964(18) -0.15144(16) 0.54161(16) 0.0322(7) Uani 1 1 d . . . O7 O 0.36645(18) -0.35320(16) 0.50751(15) 0.0300(7) Uani 1 1 d . . . O8 O 0.20114(17) -0.25762(14) 0.57967(14) 0.0219(6) Uani 1 1 d . . . C1 C 0.2251(3) -0.1430(2) 0.4448(2) 0.0261(10) Uani 1 1 d . . . C2 C 0.2141(3) -0.2127(2) 0.4324(2) 0.0246(9) Uani 1 1 d . . . C3 C 0.1371(3) -0.2382(2) 0.4145(2) 0.0269(10) Uani 1 1 d . . . C4 C 0.0725(3) -0.1927(3) 0.4042(2) 0.0340(11) Uani 1 1 d . . . H4 H 0.0213 -0.2096 0.3920 0.041 Uiso 1 1 calc R . . C5 C 0.0826(3) -0.1231(3) 0.4118(2) 0.0364(12) Uani 1 1 d . . . C6 C 0.1591(3) -0.0986(3) 0.4336(2) 0.0340(12) Uani 1 1 d . . . H6 H 0.1662 -0.0522 0.4407 0.041 Uiso 1 1 calc R . . C7 C 0.0124(3) -0.0743(3) 0.3998(3) 0.0509(16) Uani 1 1 d . . . H7A H -0.0286 -0.0960 0.3723 0.076 Uiso 1 1 calc R . . H7B H 0.0324 -0.0345 0.3769 0.076 Uiso 1 1 calc R . . H7C H -0.0111 -0.0614 0.4427 0.076 Uiso 1 1 calc R . . C8 C 0.1262(3) -0.3140(3) 0.4104(2) 0.0338(12) Uani 1 1 d . . . H8A H 0.0703 -0.3246 0.3973 0.041 Uiso 1 1 calc R . . H8B H 0.1628 -0.3327 0.3764 0.041 Uiso 1 1 calc R . . C9 C 0.1162(3) -0.4131(2) 0.4842(2) 0.0293(10) Uani 1 1 d . . . H9A H 0.1582 -0.4444 0.4688 0.035 Uiso 1 1 calc R . . H9B H 0.0671 -0.4204 0.4573 0.035 Uiso 1 1 calc R . . C10 C 0.0981(3) -0.4248(2) 0.5586(2) 0.0247(10) Uani 1 1 d . . . C11 C 0.1611(3) -0.4145(2) 0.6061(2) 0.0247(10) Uani 1 1 d . . . C12 C 0.1441(3) -0.4146(2) 0.6755(2) 0.0276(10) Uani 1 1 d . . . C13 C 0.0645(3) -0.4302(2) 0.6968(2) 0.0286(10) Uani 1 1 d . . . H13 H 0.0528 -0.4304 0.7431 0.034 Uiso 1 1 calc R . . C14 C 0.0020(3) -0.4456(2) 0.6508(2) 0.0273(10) Uani 1 1 d . . . C15 C 0.0196(3) -0.4411(2) 0.5815(2) 0.0283(11) Uani 1 1 d . . . H15 H -0.0218 -0.4492 0.5500 0.034 Uiso 1 1 calc R . . C16 C -0.0825(3) -0.4670(2) 0.6758(3) 0.0354(12) Uani 1 1 d . . . H16A H -0.0915 -0.5140 0.6650 0.053 Uiso 1 1 calc R . . H16B H -0.1236 -0.4397 0.6540 0.053 Uiso 1 1 calc R . . H16C H -0.0856 -0.4607 0.7241 0.053 Uiso 1 1 calc R . . C17 C 0.2114(3) -0.3981(2) 0.7251(2) 0.0300(10) Uani 1 1 d . . . H17A H 0.1920 -0.4043 0.7713 0.036 Uiso 1 1 calc R . . H17B H 0.2577 -0.4282 0.7178 0.036 Uiso 1 1 calc R . . C18 C 0.3105(3) -0.3121(2) 0.7497(2) 0.0271(10) Uani 1 1 d . . . H18A H 0.3549 -0.3406 0.7335 0.033 Uiso 1 1 calc R . . H18B H 0.3041 -0.3194 0.7982 0.033 Uiso 1 1 calc R . . C19 C 0.3290(3) -0.2384(2) 0.7356(2) 0.0255(10) Uani 1 1 d . . . C20 C 0.3543(3) -0.2196(2) 0.6696(2) 0.0236(10) Uani 1 1 d . . . C21 C 0.3627(3) -0.1505(2) 0.6541(2) 0.0258(10) Uani 1 1 d . . . C22 C 0.3500(3) -0.1024(2) 0.7042(2) 0.0307(11) Uani 1 1 d . . . H22 H 0.3559 -0.0566 0.6933 0.037 Uiso 1 1 calc R . . C23 C 0.3285(3) -0.1200(2) 0.7707(2) 0.0263(10) Uani 1 1 d . . . C24 C 0.3177(2) -0.1888(2) 0.7847(2) 0.0259(10) Uani 1 1 d . . . H24 H 0.3024 -0.2018 0.8283 0.031 Uiso 1 1 calc R . . C25 C 0.3159(3) -0.0664(2) 0.8250(3) 0.0374(12) Uani 1 1 d . . . H25A H 0.2622 -0.0469 0.8203 0.056 Uiso 1 1 calc R . . H25B H 0.3565 -0.0314 0.8201 0.056 Uiso 1 1 calc R . . H25C H 0.3210 -0.0869 0.8691 0.056 Uiso 1 1 calc R . . C26 C 0.3795(3) -0.1302(2) 0.5809(2) 0.0319(11) Uani 1 1 d . . . H26A H 0.3868 -0.0813 0.5775 0.038 Uiso 1 1 calc R . . H26B H 0.4289 -0.1523 0.5645 0.038 Uiso 1 1 calc R . . C27 C 0.3049(3) -0.1204(2) 0.4756(2) 0.0306(11) Uani 1 1 d . . . H27A H 0.3506 -0.1348 0.4475 0.037 Uiso 1 1 calc R . . H27B H 0.3063 -0.0712 0.4796 0.037 Uiso 1 1 calc R . . N N 0.0860(2) -0.16289(19) 0.6209(2) 0.0305(9) Uani 1 1 d . . . H1 H 0.1212 -0.1871 0.5915 0.037 Uiso 1 1 d R . . C28 C 0.1088(3) -0.1876(4) 0.6887(3) 0.0540(16) Uani 1 1 d . . . H28A H 0.1629 -0.1706 0.7000 0.065 Uiso 1 1 calc R . . H28B H 0.1117 -0.2369 0.6877 0.065 Uiso 1 1 calc R . . C29 C 0.0491(4) -0.1662(5) 0.7441(3) 0.092(3) Uani 1 1 d . . . H29A H 0.0473 -0.1175 0.7466 0.138 Uiso 1 1 calc R . . H29B H 0.0670 -0.1843 0.7870 0.138 Uiso 1 1 calc R . . H29C H -0.0046 -0.1834 0.7337 0.138 Uiso 1 1 calc R . . C30 C 0.0054(3) -0.1882(3) 0.5958(3) 0.0396(12) Uani 1 1 d . . . H30A H -0.0376 -0.1682 0.6234 0.048 Uiso 1 1 calc R . . H30B H -0.0023 -0.1722 0.5496 0.048 Uiso 1 1 calc R . . C31 C -0.0044(4) -0.2628(3) 0.5965(4) 0.080(3) Uani 1 1 d . . . H31A H 0.0401 -0.2835 0.5722 0.121 Uiso 1 1 calc R . . H31B H -0.0554 -0.2748 0.5752 0.121 Uiso 1 1 calc R . . H31C H -0.0044 -0.2787 0.6427 0.121 Uiso 1 1 calc R . . C32 C 0.0862(4) -0.0871(3) 0.6111(4) 0.0586(17) Uani 1 1 d . . . H32A H 0.0702 -0.0775 0.5645 0.070 Uiso 1 1 calc R . . H32B H 0.0447 -0.0676 0.6405 0.070 Uiso 1 1 calc R . . C33 C 0.1641(4) -0.0526(3) 0.6245(4) 0.075(2) Uani 1 1 d . . . H33A H 0.1760 -0.0545 0.6723 0.112 Uiso 1 1 calc R . . H33B H 0.1602 -0.0060 0.6104 0.112 Uiso 1 1 calc R . . H33C H 0.2072 -0.0747 0.5996 0.112 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 U 0.02118(8) 0.02421(8) 0.02451(8) -0.00023(8) 0.00131(8) 0.00178(8) O1 0.0230(15) 0.0300(16) 0.0265(17) 0.0018(13) 0.0031(14) 0.0000(14) O2 0.0373(18) 0.0283(17) 0.0225(16) 0.0029(13) -0.0014(14) -0.0078(15) O3 0.0238(17) 0.0246(17) 0.0342(18) 0.0019(14) 0.0037(13) -0.0012(13) O4 0.0326(19) 0.0193(16) 0.0362(18) 0.0069(14) -0.0064(15) -0.0032(13) O5 0.0211(15) 0.0299(18) 0.0277(17) -0.0032(14) 0.0018(14) 0.0010(13) O6 0.0361(17) 0.0362(18) 0.0243(16) 0.0060(15) -0.0072(15) -0.0138(14) O7 0.0271(17) 0.0337(18) 0.0293(17) 0.0028(14) 0.0078(14) 0.0062(15) O8 0.0242(16) 0.0175(15) 0.0241(15) -0.0002(12) -0.0017(13) 0.0015(12) C1 0.028(2) 0.030(2) 0.021(2) 0.0042(18) 0.000(2) -0.002(2) C2 0.023(2) 0.033(3) 0.0175(19) 0.0059(17) 0.0019(19) 0.001(2) C3 0.023(2) 0.038(3) 0.020(2) 0.006(2) 0.0012(19) -0.005(2) C4 0.024(2) 0.051(3) 0.027(2) 0.017(3) -0.001(2) -0.006(3) C5 0.030(3) 0.046(3) 0.033(3) 0.018(2) 0.004(2) 0.003(2) C6 0.035(3) 0.034(3) 0.033(3) 0.018(2) 0.005(2) 0.000(2) C7 0.034(3) 0.052(4) 0.067(4) 0.035(3) 0.004(3) 0.008(3) C8 0.029(2) 0.050(3) 0.022(2) 0.002(2) -0.0023(19) -0.012(2) C9 0.031(2) 0.027(3) 0.029(2) -0.007(2) 0.003(2) -0.001(2) C10 0.028(2) 0.012(2) 0.034(3) -0.0016(19) 0.004(2) 0.0025(18) C11 0.021(2) 0.018(2) 0.035(3) 0.002(2) 0.003(2) 0.0003(19) C12 0.033(2) 0.016(2) 0.034(3) 0.003(2) 0.002(2) 0.001(2) C13 0.034(3) 0.018(2) 0.034(3) 0.000(2) 0.004(2) 0.000(2) C14 0.029(2) 0.014(2) 0.040(3) 0.000(2) 0.007(2) 0.0010(19) C15 0.033(3) 0.018(2) 0.034(3) -0.003(2) 0.003(2) 0.000(2) C16 0.029(3) 0.031(3) 0.046(3) 0.003(2) 0.007(2) -0.001(2) C17 0.039(3) 0.018(2) 0.033(2) 0.0069(19) 0.002(2) 0.000(2) C18 0.032(2) 0.021(2) 0.029(2) 0.002(2) -0.0025(19) 0.000(2) C19 0.023(2) 0.027(3) 0.026(2) 0.006(2) -0.0056(19) -0.0017(19) C20 0.020(2) 0.027(2) 0.025(2) -0.0001(19) -0.001(2) 0.0011(19) C21 0.031(3) 0.025(2) 0.021(2) 0.0039(19) -0.005(2) -0.006(2) C22 0.035(3) 0.020(2) 0.037(3) 0.006(2) -0.004(2) -0.007(2) C23 0.027(2) 0.021(2) 0.032(3) -0.001(2) -0.005(2) 0.0014(19) C24 0.022(2) 0.028(2) 0.028(2) 0.002(2) -0.0025(18) 0.001(2) C25 0.047(3) 0.028(3) 0.037(3) -0.005(2) -0.006(2) -0.004(2) C26 0.033(3) 0.032(3) 0.032(3) 0.005(2) -0.004(2) -0.013(2) C27 0.037(3) 0.029(3) 0.026(2) 0.0054(19) 0.000(2) -0.005(2) N 0.032(2) 0.025(2) 0.035(2) -0.0026(18) 0.0056(19) 0.0040(17) C28 0.030(3) 0.097(5) 0.036(3) 0.000(3) -0.010(2) 0.015(3) C29 0.049(4) 0.198(9) 0.029(3) -0.014(4) -0.004(3) 0.020(5) C30 0.037(3) 0.043(3) 0.039(3) -0.007(3) -0.007(2) 0.013(3) C31 0.033(3) 0.049(4) 0.159(8) -0.049(5) -0.007(4) 0.004(3) C32 0.051(3) 0.033(3) 0.092(5) 0.001(3) 0.020(3) 0.004(3) C33 0.054(4) 0.043(4) 0.128(7) -0.022(4) 0.036(4) -0.008(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 U O7 1.789(3) . ? U O8 1.790(3) . ? U O5 2.213(3) . ? U O3 2.218(3) . ? U O1 2.227(3) . ? U O2 2.744(3) . ? U O6 3.056(3) . ? U O4 3.478(3) . ? O1 C2 1.340(5) . ? O1 O2 2.850(4) . ? O1 O6 2.877(4) . ? O1 O5 3.853(4) . ? O1 O3 4.073(4) . ? O2 C9 1.446(5) . ? O2 C8 1.456(5) . ? O2 O3 2.853(4) . ? O3 C11 1.339(5) . ? O3 O4 2.974(4) . ? O3 O5 3.534(4) . ? O4 C17 1.436(5) . ? O4 C18 1.437(5) . ? O4 O5 3.091(4) . ? O5 C20 1.337(5) . ? O5 O6 2.935(4) . ? O6 C26 1.439(5) . ? O6 C27 1.437(5) . ? C1 C6 1.403(6) . ? C1 C2 1.403(6) . ? C1 C27 1.503(6) . ? C2 C3 1.395(6) . ? C3 C4 1.397(6) . ? C3 C8 1.502(7) . ? C4 C5 1.386(7) . ? C5 C6 1.404(7) . ? C5 C7 1.512(7) . ? C9 C10 1.510(6) . ? C10 C15 1.394(6) . ? C10 C11 1.405(6) . ? C11 C12 1.394(6) . ? C12 C13 1.398(6) . ? C12 C17 1.503(6) . ? C13 C14 1.396(6) . ? C14 C15 1.395(6) . ? C14 C16 1.521(6) . ? C18 C19 1.505(6) . ? C19 C24 1.386(6) . ? C19 C20 1.411(6) . ? C20 C21 1.400(6) . ? C21 C22 1.381(6) . ? C21 C26 1.518(6) . ? C22 C23 1.396(6) . ? C23 C24 1.390(6) . ? C23 C25 1.516(6) . ? N C28 1.468(6) . ? N C30 1.489(6) . ? N C32 1.502(6) . ? C28 C29 1.519(7) . ? C30 C31 1.476(8) . ? C32 C33 1.464(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 O7 U O8 179.38(13) . . ? O7 U O5 89.20(12) . . ? O8 U O5 91.34(12) . . ? O7 U O3 86.55(12) . . ? O8 U O3 93.59(11) . . ? O5 U O3 105.79(11) . . ? O7 U O1 84.90(12) . . ? O8 U O1 94.56(11) . . ? O5 U O1 120.39(11) . . ? O3 U O1 132.78(11) . . ? O7 U O2 106.66(12) . . ? O8 U O2 72.84(11) . . ? O5 U O2 162.72(10) . . ? O3 U O2 69.27(10) . . ? O1 U O2 69.07(10) . . ? O7 U O6 114.27(12) . . ? O8 U O6 65.71(11) . . ? O5 U O6 65.43(10) . . ? O3 U O6 156.33(10) . . ? O1 U O6 63.73(10) . . ? O2 U O6 112.15(8) . . ? O7 U O4 119.26(11) . . ? O8 U O4 61.29(10) . . ? O5 U O4 61.09(9) . . ? O3 U O4 58.02(9) . . ? O1 U O4 155.60(9) . . ? O2 U O4 104.02(8) . . ? O6 U O4 100.12(8) . . ? C9 O2 C8 114.0(3) . . ? C17 O4 C18 112.5(3) . . ? C26 O6 C27 113.9(3) . . ? C6 C1 C2 118.8(4) . . ? C6 C1 C27 122.9(4) . . ? C2 C1 C27 118.1(4) . . ? O1 C2 C3 119.8(4) . . ? O1 C2 C1 119.4(4) . . ? C3 C2 C1 120.6(4) . . ? C2 C3 C4 119.0(4) . . ? C2 C3 C8 118.4(4) . . ? C4 C3 C8 122.5(4) . . ? C5 C4 C3 121.8(4) . . ? C4 C5 C6 118.4(5) . . ? C4 C5 C7 121.3(5) . . ? C6 C5 C7 120.2(5) . . ? C1 C6 C5 121.1(5) . . ? O2 C8 C3 109.0(4) . . ? O2 C9 C10 107.8(3) . . ? C15 C10 C11 119.3(4) . . ? C15 C10 C9 121.9(4) . . ? C11 C10 C9 118.6(4) . . ? O3 C11 C12 120.8(4) . . ? O3 C11 C10 118.8(4) . . ? C12 C11 C10 120.4(4) . . ? C11 C12 C13 118.6(4) . . ? C11 C12 C17 119.3(4) . . ? C13 C12 C17 122.1(4) . . ? C14 C13 C12 122.1(4) . . ? C15 C14 C13 118.0(4) . . ? C15 C14 C16 121.3(4) . . ? C13 C14 C16 120.7(4) . . ? C10 C15 C14 121.3(4) . . ? O4 C17 C12 108.4(3) . . ? O4 C18 C19 107.5(3) . . ? C24 C19 C20 119.7(4) . . ? C24 C19 C18 121.5(4) . . ? C20 C19 C18 118.7(4) . . ? O5 C20 C21 120.2(4) . . ? O5 C20 C19 120.9(4) . . ? C21 C20 C19 118.9(4) . . ? C22 C21 C20 119.6(4) . . ? C22 C21 C26 121.6(4) . . ? C20 C21 C26 118.6(4) . . ? C21 C22 C23 122.4(4) . . ? C24 C23 C22 117.3(4) . . ? C24 C23 C25 121.2(4) . . ? C22 C23 C25 121.5(4) . . ? C19 C24 C23 122.0(4) . . ? O6 C26 C21 106.9(3) . . ? O6 C27 C1 106.5(3) . . ? C28 N C30 114.5(4) . . ? C28 N C32 116.4(5) . . ? C30 N C32 106.9(4) . . ? N C28 C29 113.4(5) . . ? C31 C30 N 115.1(4) . . ? C33 C32 N 116.0(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 N H1 O8 0.94 1.92 2.766(5) 148.5 . #===END data_4 _database_code_CSD 172884 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H71 N O9 U' _chemical_formula_weight 1020.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2~1~/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 14.0317(7) _cell_length_b 21.9727(14) _cell_length_c 16.3246(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.837(3) _cell_angle_gamma 90.00 _cell_volume 4817.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16508 _cell_measurement_theta_min 2.77 _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 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method ? _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 3.420 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.355 _exptl_absorpt_correction_T_max 0.710 _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 16508 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8591 _reflns_number_gt 5895 _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 from Patterson map interpretation and subsequent Fourier-difference synthesis. One tert-butyl group in each half-molecule is disordered over six (molecule A) or four (molecule B) positions related by the symmetry plane, which have been refined with some restraints. The methanol molecule is also disordered over two positions, which have been fixed in the last refinement cycles. All non-hydrogen atoms were refined with anisotropic displacement parameters, except some of the disordered ones. Some bond lengths in the propylammonium ions depart from usual values, probably due to some unresolved disorder. 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. Some short contacts exist between hydrogen atoms of symmetry- related arms of the ammonium cations, which is seemingly to be ascribed to the disorder affecting these ions, maybe not perfectly modelled. Solvent accessible voids of 92 A^3^ may indicate the presence of unresolved solvent molecules. 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^)+(0.0697P)^2^+13.5004P] 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 8591 _refine_ls_number_parameters 555 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1541 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 1.232 _refine_diff_density_min -1.703 _refine_diff_density_rms 0.128 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 -0.17329(3) 0.2500 0.74291(3) 0.03928(15) Uani 1 2 d S . . O1A O -0.0126(5) 0.2500 0.7417(4) 0.0326(16) Uani 1 2 d S . . O2A O -0.0304(4) 0.3636(2) 0.8417(4) 0.0427(13) Uani 1 1 d . . . O3A O -0.2365(4) 0.3440(3) 0.7300(4) 0.0526(15) Uani 1 1 d . . . O4A O -0.3455(5) 0.2500 0.7831(5) 0.046(2) Uani 1 2 d S . . O5A O -0.2048(7) 0.2500 0.6287(6) 0.066(3) Uani 1 2 d S . . O6A O -0.1368(5) 0.2500 0.8564(5) 0.0347(16) Uani 1 2 d S . . C1A C 0.0704(8) 0.2500 0.8093(6) 0.032(2) Uani 1 2 d S . . C2A C 0.1134(5) 0.3063(3) 0.8440(5) 0.0329(16) Uani 1 1 d . . . C3A C 0.2043(5) 0.3037(4) 0.9068(5) 0.0370(18) Uani 1 1 d . . . H3E H 0.2347 0.3402 0.9287 0.044 Uiso 1 1 calc R . . C4A C 0.2525(6) 0.2500 0.9391(6) 0.034(2) Uani 1 2 d SD . . C5A C 0.3564(8) 0.2500 1.0034(7) 0.045(3) Uani 1 2 d SD . . C6A C 0.4252(10) 0.2914(8) 0.9682(12) 0.147(7) Uiso 1 1 d D . . C7A C 0.3985(13) 0.3104(6) 1.0331(14) 0.163(8) Uiso 1 1 d D . . C8A C 0.3540(13) 0.2881(8) 1.0824(8) 0.141(7) Uiso 1 1 d D . . C9A C 0.0589(5) 0.3638(4) 0.8158(5) 0.0393(18) Uani 1 1 d . . . H9E H 0.1002 0.3982 0.8412 0.047 Uiso 1 1 calc R . . H9F H 0.0423 0.3674 0.7540 0.047 Uiso 1 1 calc R . . C10A C -0.0846(6) 0.4205(4) 0.8260(6) 0.047(2) Uani 1 1 d . . . H10E H -0.0989 0.4319 0.7663 0.057 Uiso 1 1 calc R . . H10F H -0.0458 0.4526 0.8610 0.057 Uiso 1 1 calc R . . C11A C -0.1799(6) 0.4104(4) 0.8489(7) 0.051(2) Uani 1 1 d . . . C12A C -0.2505(6) 0.3705(4) 0.7993(6) 0.043(2) Uani 1 1 d . . . C13A C -0.3352(6) 0.3551(4) 0.8252(6) 0.044(2) Uani 1 1 d . . . C14A C -0.3497(6) 0.3826(4) 0.8961(6) 0.045(2) Uani 1 1 d . . . H14A H -0.4065 0.3727 0.9118 0.053 Uiso 1 1 calc R . . C15A C -0.2833(6) 0.4247(4) 0.9456(6) 0.045(2) Uani 1 1 d . . . C16A C -0.1972(6) 0.4371(4) 0.9210(6) 0.050(2) Uani 1 1 d . . . H16A H -0.1502 0.4640 0.9538 0.061 Uiso 1 1 calc R . . C17A C -0.3015(6) 0.4572(4) 1.0224(7) 0.054(2) Uani 1 1 d . . . C18A C -0.2122(9) 0.4485(6) 1.1017(8) 0.087(4) Uani 1 1 d . . . H18A H -0.2243 0.4691 1.1495 0.131 Uiso 1 1 calc R . . H18C H -0.1536 0.4650 1.0909 0.131 Uiso 1 1 calc R . . H18D H -0.2026 0.4058 1.1143 0.131 Uiso 1 1 calc R . . C19A C -0.3197(9) 0.5252(4) 1.0030(8) 0.071(3) Uani 1 1 d . . . H19A H -0.3665 0.5301 0.9474 0.107 Uiso 1 1 calc R . . H19C H -0.2581 0.5446 1.0041 0.107 Uiso 1 1 calc R . . H19G H -0.3460 0.5434 1.0454 0.107 Uiso 1 1 calc R . . C20A C -0.3910(8) 0.4322(5) 1.0452(7) 0.066(3) Uani 1 1 d . . . H20A H -0.4499 0.4390 0.9985 0.099 Uiso 1 1 calc R . . H20C H -0.3975 0.4525 1.0954 0.099 Uiso 1 1 calc R . . H20G H -0.3824 0.3894 1.0562 0.099 Uiso 1 1 calc R . . C21A C -0.4032(6) 0.3052(4) 0.7751(6) 0.048(2) Uani 1 1 d . . . H21A H -0.4592 0.2991 0.7978 0.057 Uiso 1 1 calc R . . H21C H -0.4287 0.3167 0.7153 0.057 Uiso 1 1 calc R . . U2 U 0.18191(3) 0.2500 0.32978(3) 0.05091(17) Uani 1 2 d S . . O1B O 0.0207(6) 0.2500 0.2508(4) 0.0403(18) Uani 1 2 d S . . O2B O 0.0372(5) 0.3646(3) 0.3620(4) 0.0553(16) Uani 1 1 d . . . O3B O 0.2399(5) 0.3444(4) 0.3464(4) 0.072(2) Uani 1 1 d . . . O4B O 0.3535(7) 0.2500 0.4509(6) 0.064(3) Uani 1 2 d S . . O5B O 0.2112(7) 0.2500 0.2313(6) 0.082(4) Uani 1 2 d S . . O6B O 0.1465(5) 0.2500 0.4249(5) 0.0377(17) Uani 1 2 d S . . C1B C -0.0609(9) 0.2500 0.2783(7) 0.040(3) Uani 1 2 d S . . C2B C -0.1055(6) 0.3045(4) 0.2920(5) 0.0409(19) Uani 1 1 d . . . C3B C -0.1945(6) 0.3037(4) 0.3102(5) 0.047(2) Uani 1 1 d . . . H3F H -0.2230 0.3406 0.3184 0.056 Uiso 1 1 calc R . . C4B C -0.2445(8) 0.2500 0.3168(7) 0.048(3) Uani 1 2 d SD . . C5B C -0.3496(12) 0.2500 0.3329(8) 0.089(6) Uani 1 2 d SD . . C6B C -0.4103(11) 0.3037(8) 0.2852(14) 0.156(7) Uani 1 1 d DU . . C7B C -0.3413(19) 0.2880(14) 0.4140(15) 0.120(11) Uani 0.50 1 d PDU . . C9B C -0.0511(7) 0.3642(4) 0.2903(6) 0.051(2) Uani 1 1 d . . . H9G H -0.0336 0.3677 0.2373 0.062 Uiso 1 1 calc R . . H9H H -0.0936 0.3982 0.2942 0.062 Uiso 1 1 calc R . . C10B C 0.0911(8) 0.4204(4) 0.3725(7) 0.076(4) Uani 1 1 d . . . H10C H 0.0528 0.4526 0.3885 0.091 Uiso 1 1 calc R . . H10D H 0.1041 0.4318 0.3193 0.091 Uiso 1 1 calc R . . C11B C 0.1886(9) 0.4112(5) 0.4423(7) 0.070(3) Uani 1 1 d . . . C12B C 0.2570(8) 0.3712(5) 0.4266(6) 0.062(3) Uani 1 1 d . . . C13B C 0.3427(7) 0.3548(5) 0.4890(6) 0.058(3) Uani 1 1 d . . . C14B C 0.3628(7) 0.3836(5) 0.5686(7) 0.065(3) Uani 1 1 d . . . H14B H 0.4212 0.3742 0.6110 0.078 Uiso 1 1 calc R . . C15B C 0.2975(8) 0.4258(4) 0.5859(7) 0.066(3) Uani 1 1 d . . . C16B C 0.2122(9) 0.4380(5) 0.5207(8) 0.077(4) Uani 1 1 d . . . H16B H 0.1679 0.4664 0.5309 0.093 Uiso 1 1 calc R . . C17B C 0.3190(9) 0.4585(5) 0.6743(8) 0.083(4) Uani 1 1 d . . . C18B C 0.2281(14) 0.4396(9) 0.7162(12) 0.143(7) Uani 1 1 d . . . H18B H 0.2186 0.4718 0.7529 0.215 Uiso 1 1 calc R . . H18E H 0.2456 0.4028 0.7488 0.215 Uiso 1 1 calc R . . H18F H 0.1675 0.4334 0.6710 0.215 Uiso 1 1 calc R . . C19B C 0.3060(12) 0.5230(7) 0.6681(10) 0.118(5) Uani 1 1 d U . . H19D H 0.3120 0.5395 0.7238 0.177 Uiso 1 1 calc R . . H19E H 0.2413 0.5322 0.6304 0.177 Uiso 1 1 calc R . . H19F H 0.3561 0.5405 0.6458 0.177 Uiso 1 1 calc R . . C20B C 0.4074(11) 0.4328(7) 0.7391(9) 0.106(5) Uani 1 1 d U . . H20D H 0.4656 0.4386 0.7202 0.158 Uiso 1 1 calc R . . H20E H 0.3974 0.3901 0.7460 0.158 Uiso 1 1 calc R . . H20F H 0.4163 0.4532 0.7928 0.158 Uiso 1 1 calc R . . C21B C 0.4114(8) 0.3060(6) 0.4724(7) 0.076(3) Uani 1 1 d . . . H21B H 0.4368 0.3180 0.4255 0.091 Uiso 1 1 calc R . . H21E H 0.4674 0.2999 0.5230 0.091 Uiso 1 1 calc R . . N1 N 0.0358(6) 0.2500 0.5881(6) 0.036(2) Uani 1 2 d S . . H1 H 0.0164 0.2500 0.6499 0.043 Uiso 1 2 d SR . . C1 C -0.0069(13) 0.3024(7) 0.5388(8) 0.113(5) Uani 1 1 d U . . H1A H 0.0467 0.3189 0.5192 0.136 Uiso 1 1 calc R . . H1B H -0.0546 0.2858 0.4883 0.136 Uiso 1 1 calc R . . C2 C -0.0507(10) 0.3495(5) 0.5579(8) 0.075(3) Uani 1 1 d U . . H2A H -0.0019 0.3647 0.6088 0.090 Uiso 1 1 calc R . . H2B H -0.1026 0.3315 0.5786 0.090 Uiso 1 1 calc R . . C3 C -0.0952(13) 0.4022(7) 0.5190(9) 0.112(5) Uani 1 1 d U . . H3A H -0.0591 0.4368 0.5482 0.168 Uiso 1 1 calc R . . H3B H -0.1627 0.4039 0.5213 0.168 Uiso 1 1 calc R . . H3C H -0.0945 0.4026 0.4603 0.168 Uiso 1 1 calc R . . C4 C 0.1426(12) 0.2722(7) 0.6141(10) 0.040(4) Uani 0.50 1 d P . . C5 C 0.2217(13) 0.2744(8) 0.6608(14) 0.055(5) Uani 0.50 1 d P . . C6 C 0.3186(10) 0.2500 0.7030(11) 0.065(4) Uani 1 2 d S . . N2 N -0.0279(6) 0.2500 0.0716(5) 0.0319(19) Uani 1 2 d S . . H2 H -0.0058 0.2500 0.1234 0.038 Uiso 1 2 d SR . . C7 C 0.0149(12) 0.3029(7) 0.0447(9) 0.109(5) Uani 1 1 d U . . H7C H 0.0565 0.2863 0.0120 0.131 Uiso 1 1 calc R . . H7D H -0.0409 0.3217 0.0029 0.131 Uiso 1 1 calc R . . C8 C 0.0659(10) 0.3488(5) 0.0848(7) 0.084(4) Uani 1 1 d U . . H8A H 0.1247 0.3292 0.1217 0.100 Uiso 1 1 calc R . . H8B H 0.0276 0.3612 0.1229 0.100 Uiso 1 1 calc R . . C9 C 0.1018(10) 0.4015(6) 0.0666(8) 0.088(4) Uani 1 1 d U . . H9A H 0.0762 0.4095 0.0064 0.132 Uiso 1 1 calc R . . H9B H 0.1732 0.3995 0.0823 0.132 Uiso 1 1 calc R . . H9C H 0.0820 0.4336 0.0981 0.132 Uiso 1 1 calc R . . C10 C -0.1348(11) 0.2719(7) 0.0464(10) 0.037(4) Uani 0.50 1 d P . . C11 C -0.2058(13) 0.2751(7) 0.0594(10) 0.041(4) Uani 0.50 1 d P . . C12 C -0.3066(10) 0.2500 0.0552(9) 0.060(4) Uani 1 2 d S . . O1 O -0.3834 0.3793 0.5784 0.100 Uiso 0.50 1 d P . . O2 O -0.2781 0.4374 0.6057 0.100 Uiso 0.50 1 d P . . C13 C -0.3788 0.4424 0.5697 0.100 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0299(2) 0.0576(3) 0.0284(2) 0.000 0.00534(18) 0.000 O1A 0.033(4) 0.039(4) 0.026(4) 0.000 0.010(3) 0.000 O2A 0.042(3) 0.031(3) 0.064(4) 0.008(3) 0.030(3) 0.006(2) O3A 0.045(3) 0.066(4) 0.044(3) 0.018(3) 0.009(3) 0.006(3) O4A 0.025(4) 0.050(5) 0.057(5) 0.000 0.005(4) 0.000 O5A 0.047(5) 0.104(8) 0.043(5) 0.000 0.005(4) 0.000 O6A 0.037(4) 0.031(4) 0.040(4) 0.000 0.017(3) 0.000 C1A 0.032(5) 0.038(6) 0.028(5) 0.000 0.011(5) 0.000 C2A 0.032(4) 0.038(4) 0.033(4) 0.002(3) 0.018(3) -0.001(3) C3A 0.024(3) 0.046(5) 0.042(4) -0.004(4) 0.011(3) -0.004(3) C4A 0.026(5) 0.038(6) 0.039(6) 0.000 0.011(5) 0.000 C5A 0.025(5) 0.067(9) 0.042(7) 0.000 0.009(5) 0.000 C9A 0.034(4) 0.035(5) 0.050(5) 0.005(4) 0.013(4) -0.003(3) C10A 0.044(5) 0.030(5) 0.074(6) 0.014(4) 0.027(4) 0.009(4) C11A 0.041(4) 0.036(5) 0.080(7) 0.017(4) 0.026(5) 0.004(4) C12A 0.033(4) 0.042(5) 0.052(5) 0.014(4) 0.009(4) 0.008(4) C13A 0.032(4) 0.041(5) 0.053(5) 0.015(4) 0.006(4) 0.010(3) C14A 0.031(4) 0.041(5) 0.066(6) 0.010(4) 0.021(4) 0.007(3) C15A 0.031(4) 0.036(5) 0.069(6) 0.006(4) 0.016(4) 0.011(3) C16A 0.041(4) 0.032(5) 0.082(7) 0.003(4) 0.023(5) 0.006(4) C17A 0.041(5) 0.037(5) 0.086(7) -0.002(5) 0.021(5) 0.004(4) C18A 0.069(7) 0.105(10) 0.085(8) -0.021(7) 0.019(7) 0.029(7) C19A 0.085(8) 0.037(5) 0.106(9) -0.009(5) 0.048(7) -0.001(5) C20A 0.072(7) 0.050(6) 0.091(8) -0.008(5) 0.047(6) -0.005(5) C21A 0.030(4) 0.049(5) 0.058(6) 0.009(4) 0.003(4) 0.007(4) U2 0.0406(3) 0.0807(4) 0.0372(3) 0.000 0.0205(2) 0.000 O1B 0.040(4) 0.057(5) 0.030(4) 0.000 0.020(3) 0.000 O2B 0.058(4) 0.041(4) 0.056(4) 0.004(3) -0.001(3) -0.007(3) O3B 0.075(5) 0.097(6) 0.049(4) 0.018(4) 0.024(4) -0.028(4) O4B 0.043(5) 0.100(8) 0.055(6) 0.000 0.025(5) 0.000 O5B 0.050(6) 0.155(12) 0.047(6) 0.000 0.024(5) 0.000 O6B 0.041(4) 0.035(4) 0.042(4) 0.000 0.019(4) 0.000 C1B 0.052(7) 0.040(7) 0.031(6) 0.000 0.015(5) 0.000 C2B 0.050(5) 0.044(5) 0.029(4) -0.002(3) 0.011(4) 0.001(4) C3B 0.041(4) 0.064(6) 0.033(4) -0.002(4) 0.006(4) 0.008(4) C4B 0.050(7) 0.069(9) 0.025(6) 0.000 0.011(5) 0.000 C5B 0.060(9) 0.18(2) 0.034(8) 0.000 0.015(8) 0.000 C6B 0.125(10) 0.156(11) 0.188(11) 0.013(9) 0.048(8) 0.019(8) C7B 0.114(13) 0.139(14) 0.116(13) -0.015(9) 0.047(10) 0.005(9) C9B 0.056(5) 0.043(5) 0.045(5) 0.001(4) -0.003(4) 0.007(4) C10B 0.082(7) 0.039(6) 0.076(7) 0.019(5) -0.023(6) -0.018(5) C11B 0.079(7) 0.040(6) 0.076(7) 0.015(5) -0.003(6) -0.014(5) C12B 0.060(6) 0.071(7) 0.049(5) 0.011(5) 0.009(5) -0.033(6) C13B 0.041(5) 0.076(7) 0.061(6) 0.013(5) 0.023(5) -0.010(5) C14B 0.051(5) 0.060(7) 0.074(7) 0.017(5) 0.004(5) -0.022(5) C15B 0.062(6) 0.041(6) 0.077(7) 0.004(5) -0.008(6) -0.005(5) C16B 0.073(7) 0.037(6) 0.097(9) 0.001(5) -0.016(7) -0.003(5) C17B 0.091(8) 0.042(6) 0.081(8) -0.014(5) -0.029(7) 0.008(5) C18B 0.133(14) 0.147(17) 0.148(16) -0.070(13) 0.038(13) -0.028(13) C19B 0.134(9) 0.085(8) 0.114(9) -0.001(7) 0.001(7) 0.009(7) C20B 0.117(8) 0.093(8) 0.092(7) 0.000(6) 0.007(7) 0.030(7) C21B 0.056(6) 0.116(10) 0.058(6) -0.004(6) 0.022(5) -0.032(6) N1 0.033(5) 0.039(5) 0.038(5) 0.000 0.015(4) 0.000 C1 0.153(9) 0.121(9) 0.077(7) 0.039(6) 0.052(7) 0.058(7) C2 0.092(7) 0.068(6) 0.080(6) 0.014(5) 0.046(5) 0.019(5) C3 0.149(9) 0.102(8) 0.091(7) 0.009(6) 0.045(7) 0.046(7) C4 0.042(9) 0.049(11) 0.028(8) -0.005(6) 0.007(8) -0.016(6) C5 0.033(9) 0.057(12) 0.080(14) 0.009(9) 0.023(10) 0.007(7) C6 0.041(7) 0.066(10) 0.083(11) 0.000 0.012(7) 0.000 N2 0.040(5) 0.028(5) 0.027(4) 0.000 0.009(4) 0.000 C7 0.125(6) 0.104(6) 0.096(6) 0.004(4) 0.030(5) -0.029(5) C8 0.110(7) 0.068(6) 0.063(6) -0.003(5) 0.010(6) -0.036(6) C9 0.113(8) 0.081(7) 0.076(6) -0.004(5) 0.036(6) -0.038(6) C10 0.028(7) 0.046(11) 0.044(9) 0.009(6) 0.018(7) 0.013(6) C11 0.043(9) 0.038(9) 0.033(9) 0.001(6) -0.004(8) -0.008(7) C12 0.041(7) 0.083(11) 0.062(9) 0.000 0.024(7) 0.000 _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 O6A 1.773(7) . ? U1 O5A 1.788(9) . ? U1 O3A 2.233(6) 4_565 ? U1 O3A 2.233(6) . ? U1 O1A 2.261(7) . ? U1 O4A 2.681(8) . ? U1 O2A 3.313(6) . ? U1 O2B 8.024(7) . ? O1A C1A 1.353(12) . ? O2A C9A 1.435(9) . ? O2A C10A 1.447(9) . ? O3A C12A 1.337(10) . ? O3A O2 2.826(6) . ? O3A O1 2.832(5) . ? O4A C21A 1.443(9) 4_565 ? O4A C21A 1.443(9) . ? C1A C2A 1.421(9) . ? C1A C2A 1.421(9) 4_565 ? C2A C3A 1.386(10) . ? C2A C9A 1.479(11) . ? C3A C4A 1.386(9) . ? C4A C3A 1.386(9) 4_565 ? C4A C5A 1.529(12) . ? C5A C7A 1.477(9) . ? C5A C7A 1.477(9) 4_565 ? C5A C8A 1.547(9) 4_565 ? C5A C8A 1.547(9) . ? C5A C6A 1.553(19) 4_565 ? C5A C6A 1.553(19) . ? C6A C7A 1.29(3) . ? C7A C8A 1.25(3) . ? C8A C8A 1.68(4) 4_565 ? C10A C11A 1.505(11) . ? C11A C12A 1.394(12) . ? C11A C16A 1.398(13) . ? C12A C13A 1.413(11) . ? C13A C14A 1.373(12) . ? C13A C21A 1.525(12) . ? C14A C15A 1.393(12) . ? C15A C16A 1.406(12) . ? C15A C17A 1.527(13) . ? C17A C20A 1.512(13) . ? C17A C18A 1.531(15) . ? C17A C19A 1.533(13) . ? U2 O6B 1.763(7) . ? U2 O5B 1.770(9) . ? U2 O3B 2.216(8) . ? U2 O3B 2.216(8) 4_565 ? U2 O1B 2.256(7) . ? U2 O4B 2.636(9) . ? O1B C1B 1.347(13) . ? O2B C10B 1.425(11) . ? O2B C9B 1.437(10) . ? O3B C12B 1.392(12) . ? O4B C21B 1.460(12) . ? O4B C21B 1.460(12) 4_565 ? C1B C2B 1.399(10) 4_565 ? C1B C2B 1.399(10) . ? C2B C3B 1.365(12) . ? C2B C9B 1.521(12) . ? C3B C4B 1.394(11) . ? C4B C3B 1.394(11) 4_565 ? C4B C5B 1.570(18) . ? C5B C6B 1.53(2) . ? C5B C6B 1.53(2) 4_565 ? C5B C7B 1.541(10) 4_565 ? C5B C7B 1.541(10) . ? C7B C7B 1.67(6) 4_565 ? C10B C11B 1.519(14) . ? C11B C16B 1.358(16) . ? C11B C12B 1.380(16) . ? C12B C13B 1.380(14) . ? C13B C14B 1.397(15) . ? C13B C21B 1.519(16) . ? C14B C15B 1.390(15) . ? C15B C16B 1.379(14) . ? C15B C17B 1.560(15) . ? C17B C19B 1.429(18) . ? C17B C20B 1.488(15) . ? C17B C18B 1.67(2) . ? N1 C1 1.432(14) . ? N1 C1 1.432(14) 4_565 ? N1 C4 1.514(17) . ? N1 C4 1.514(17) 4_565 ? C1 C2 1.287(16) . ? C2 C3 1.381(16) . ? C4 C4 0.97(3) 4_565 ? C4 C5 1.15(2) . ? C4 C5 1.54(2) 4_565 ? C5 C5 1.07(4) 4_565 ? C5 C6 1.44(2) . ? C5 C4 1.54(2) 4_565 ? C6 C5 1.44(2) 4_565 ? N2 C7 1.434(15) . ? N2 C7 1.434(15) 4_565 ? N2 C10 1.514(16) 4_565 ? N2 C10 1.514(16) . ? C7 C8 1.299(16) . ? C8 C9 1.331(15) . ? C10 C10 0.96(3) 4_565 ? C10 C11 1.08(2) . ? C10 C11 1.49(2) 4_565 ? C11 C11 1.10(3) 4_565 ? C11 C10 1.49(2) 4_565 ? C11 C12 1.50(2) . ? C12 C11 1.50(2) 4_565 ? O1 C13 1.3964 . ? O2 C13 1.3685 . ? 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 O6A U1 O5A 177.6(4) . . ? O6A U1 O3A 94.91(18) . 4_565 ? O5A U1 O3A 85.97(19) . 4_565 ? O6A U1 O3A 94.91(18) . . ? O5A U1 O3A 85.97(19) . . ? O3A U1 O3A 135.3(3) 4_565 . ? O6A U1 O1A 91.3(3) . . ? O5A U1 O1A 86.4(3) . . ? O3A U1 O1A 111.64(16) 4_565 . ? O3A U1 O1A 111.64(16) . . ? O6A U1 O4A 75.7(3) . . ? O5A U1 O4A 106.7(3) . . ? O3A U1 O4A 70.25(16) 4_565 . ? O3A U1 O4A 70.25(16) . . ? O1A U1 O4A 166.9(2) . . ? O6A U1 O2A 62.62(15) . . ? O5A U1 O2A 116.11(19) . . ? O3A U1 O2A 155.54(18) 4_565 . ? O3A U1 O2A 61.12(18) . . ? O1A U1 O2A 62.61(13) . . ? O4A U1 O2A 109.99(14) . . ? O6A U1 O2B 138.6(2) . . ? O5A U1 O2B 39.4(3) . . ? O3A U1 O2B 116.23(16) 4_565 . ? O3A U1 O2B 82.04(16) . . ? O1A U1 O2B 53.22(16) . . ? O4A U1 O2B 138.58(16) . . ? O2A U1 O2B 80.48(10) . . ? C9A O2A C10A 113.8(6) . . ? C21A O4A C21A 114.4(8) 4_565 . ? O1A C1A C2A 119.4(5) . . ? O1A C1A C2A 119.4(5) . 4_565 ? C2A C1A C2A 121.1(10) . 4_565 ? C3A C2A C1A 116.9(7) . . ? C3A C2A C9A 123.2(7) . . ? C1A C2A C9A 119.8(7) . . ? C2A C3A C4A 124.0(7) . . ? C3A C4A C3A 116.7(9) 4_565 . ? C3A C4A C5A 121.6(4) 4_565 . ? C3A C4A C5A 121.6(4) . . ? C7A C5A C7A 128.0(17) . 4_565 ? C7A C5A C4A 115.9(8) . . ? C7A C5A C4A 115.9(8) 4_565 . ? C7A C5A C8A 108.4(15) . 4_565 ? C4A C5A C8A 109.0(8) . 4_565 ? C7A C5A C8A 108.4(15) 4_565 . ? C4A C5A C8A 109.0(8) . . ? C7A C5A C6A 114.5(14) . 4_565 ? C4A C5A C6A 108.5(8) . 4_565 ? C8A C5A C6A 142.3(12) . 4_565 ? C7A C5A C6A 114.5(14) 4_565 . ? C4A C5A C6A 108.5(8) . . ? C8A C5A C6A 142.3(12) 4_565 . ? C7A C6A C6A 108.9(11) . 4_565 ? C8A C7A C6A 135.9(12) . . ? C7A C8A C8A 113.0(11) . 4_565 ? O2A C9A C2A 108.8(6) . . ? O2A C10A C11A 106.7(6) . . ? C12A C11A C16A 119.1(8) . . ? C12A C11A C10A 118.7(9) . . ? C16A C11A C10A 122.1(9) . . ? O3A C12A C11A 120.8(8) . . ? O3A C12A C13A 119.5(8) . . ? C11A C12A C13A 119.6(8) . . ? C14A C13A C12A 119.3(8) . . ? C14A C13A C21A 123.1(8) . . ? C12A C13A C21A 117.4(8) . . ? C13A C14A C15A 122.9(8) . . ? C14A C15A C16A 116.7(8) . . ? C14A C15A C17A 122.9(8) . . ? C16A C15A C17A 120.4(8) . . ? C11A C16A C15A 122.1(9) . . ? C20A C17A C15A 112.4(8) . . ? C20A C17A C18A 106.4(9) . . ? C15A C17A C18A 110.2(7) . . ? C20A C17A C19A 107.7(8) . . ? C15A C17A C19A 110.0(9) . . ? C18A C17A C19A 110.1(9) . . ? O4A C21A C13A 107.9(6) . . ? O6B U2 O5B 177.2(4) . . ? O6B U2 O3B 94.57(19) . . ? O5B U2 O3B 86.4(2) . . ? O6B U2 O3B 94.57(19) . 4_565 ? O5B U2 O3B 86.4(2) . 4_565 ? O3B U2 O3B 138.8(4) . 4_565 ? O6B U2 O1B 90.7(3) . . ? O5B U2 O1B 86.5(4) . . ? O3B U2 O1B 110.0(2) . . ? O3B U2 O1B 110.0(2) 4_565 . ? O6B U2 O4B 76.6(3) . . ? O5B U2 O4B 106.2(4) . . ? O3B U2 O4B 71.64(19) . . ? O3B U2 O4B 71.64(19) 4_565 . ? O1B U2 O4B 167.3(3) . . ? C10B O2B C9B 114.0(7) . . ? C21B O4B C21B 114.8(12) . 4_565 ? O1B C1B C2B 121.1(5) . 4_565 ? O1B C1B C2B 121.1(5) . . ? C2B C1B C2B 117.8(11) 4_565 . ? C3B C2B C1B 120.2(9) . . ? C3B C2B C9B 120.7(8) . . ? C1B C2B C9B 119.1(8) . . ? C2B C3B C4B 122.8(9) . . ? C3B C4B C3B 115.8(10) . 4_565 ? C3B C4B C5B 122.1(5) . . ? C3B C4B C5B 122.1(5) 4_565 . ? C6B C5B C6B 100.9(19) . 4_565 ? C6B C5B C7B 138.4(18) . 4_565 ? C6B C5B C7B 85.0(16) 4_565 4_565 ? C6B C5B C7B 85.0(16) . . ? C6B C5B C7B 138.4(18) 4_565 . ? C7B C5B C7B 66(3) 4_565 . ? C6B C5B C4B 109.0(9) . . ? C6B C5B C4B 109.0(9) 4_565 . ? C7B C5B C4B 107.6(11) 4_565 . ? C7B C5B C4B 107.6(11) . . ? C5B C7B C7B 57.2(13) . 4_565 ? O2B C9B C2B 108.1(7) . . ? O2B C10B C11B 107.9(7) . . ? C16B C11B C12B 117.3(10) . . ? C16B C11B C10B 124.7(12) . . ? C12B C11B C10B 117.9(11) . . ? C11B C12B C13B 122.2(10) . . ? C11B C12B O3B 120.4(9) . . ? C13B C12B O3B 117.4(11) . . ? C12B C13B C14B 117.8(10) . . ? C12B C13B C21B 121.0(10) . . ? C14B C13B C21B 121.2(9) . . ? C15B C14B C13B 121.6(9) . . ? C16B C15B C14B 116.6(11) . . ? C16B C15B C17B 121.2(11) . . ? C14B C15B C17B 122.2(9) . . ? C11B C16B C15B 124.3(12) . . ? C19B C17B C20B 119.3(11) . . ? C19B C17B C15B 113.8(11) . . ? C20B C17B C15B 112.4(10) . . ? C19B C17B C18B 100.3(13) . . ? C20B C17B C18B 101.2(12) . . ? C15B C17B C18B 107.4(9) . . ? O4B C21B C13B 107.5(8) . . ? C1 N1 C1 106.9(16) . 4_565 ? C1 N1 C4 96.8(10) . . ? C1 N1 C4 129.4(11) 4_565 . ? C1 N1 C4 129.5(11) . 4_565 ? C1 N1 C4 96.8(10) 4_565 4_565 ? C2 C1 N1 131.4(11) . . ? C1 C2 C3 138.3(12) . . ? C4 C4 C5 92.4(12) 4_565 . ? C4 C4 N1 71.2(6) 4_565 . ? C5 C4 N1 152.3(16) . . ? N1 C4 C5 116.0(11) . 4_565 ? C6 C5 C4 115.8(13) . 4_565 ? C7 N2 C7 108.2(15) . 4_565 ? C7 N2 C10 130.1(10) . 4_565 ? C7 N2 C10 97.4(9) 4_565 4_565 ? C7 N2 C10 97.4(9) . . ? C7 N2 C10 130.1(10) 4_565 . ? C8 C7 N2 133.9(13) . . ? C7 C8 C9 138.8(13) . . ? C10 C10 C11 93.8(12) 4_565 . ? C11 C10 N2 113.0(11) 4_565 . ? C10 C11 C11 86.2(12) . 4_565 ? C10 C11 C12 113.5(11) 4_565 . ? C13 O1 O3A 108.51(14) . . ? C13 O2 O3A 109.84(12) . . ? 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 O1A 1.12 1.66 2.782(11) 179.9 . N2 H2 O1B 0.81 2.00 2.804(11) 168.8 . #===END data_5 _database_code_CSD 172885 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H57 N O8 U' _chemical_formula_weight 917.92 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 orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.8676(4) _cell_length_b 17.6548(11) _cell_length_c 26.4488(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4140.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 26957 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent intense orange' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method ? _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 3.968 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.199 _exptl_absorpt_correction_T_max 0.551 _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 26957 _diffrn_reflns_av_R_equivalents 0.1166 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4042 _reflns_number_gt 3181 _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. One tert-butyl group and one C atom of the n-butylammonium ion were found disordered over two positions. The n-butylammonium ion is further disordered over two positions related by the symmetry plane. All non-hydrogen atoms were refined with anisotropic displacement parameters. Two of the hydrogen atoms bound to N 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. The highest residual electron density peak is located near U as a result of an imperfect absorption correction. A solvent accessible void of 33 A^3^ may indicate the presence of an unresolved solvent molecule. 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^)+(0.1092P)^2^+8.2068P] 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 4042 _refine_ls_number_parameters 286 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1494 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.216 _refine_diff_density_min -1.449 _refine_diff_density_rms 0.187 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 U U 0.67664(4) 0.2500 0.381026(14) 0.03573(19) Uani 1 2 d S . . O1 O 0.7641(8) 0.2500 0.4583(3) 0.0406(17) Uani 1 2 d S . . O2 O 0.5924(9) 0.1111(3) 0.4415(3) 0.069(2) Uani 1 1 d . . . O3 O 0.6478(6) 0.1493(3) 0.3327(2) 0.0362(11) Uani 1 1 d . . . O4 O 0.3974(8) 0.2500 0.2857(3) 0.0353(15) Uani 1 2 d S . . O5 O 0.8716(10) 0.2500 0.3621(3) 0.062(3) Uani 1 2 d S . . O6 O 0.4822(8) 0.2500 0.3994(3) 0.0311(14) Uani 1 2 d S . . C1 C 0.6704(10) 0.2500 0.4977(4) 0.032(2) Uani 1 2 d S . . C2 C 0.6173(8) 0.1810(4) 0.5184(3) 0.0343(15) Uani 1 1 d . . . C3 C 0.5250(8) 0.1826(4) 0.5599(3) 0.0333(15) Uani 1 1 d . . . H3 H 0.4913 0.1369 0.5733 0.040 Uiso 1 1 calc R . . C4 C 0.4793(12) 0.2500 0.5829(4) 0.036(2) Uani 1 2 d S . . C5 C 0.3845(15) 0.2500 0.6319(4) 0.045(3) Uani 1 2 d S . . C6 C 0.234(2) 0.2094(10) 0.6277(8) 0.058(5) Uani 0.50 1 d P . . C7 C 0.336(2) 0.1624(9) 0.6466(6) 0.047(4) Uani 0.50 1 d P . . C8 C 0.483(2) 0.2266(9) 0.6755(6) 0.059(5) Uani 0.50 1 d P . . C9 C 0.6614(8) 0.1097(4) 0.4910(3) 0.0392(17) Uani 1 1 d . . . H9A H 0.7702 0.1069 0.4878 0.047 Uiso 1 1 calc R . . H9B H 0.6271 0.0657 0.5097 0.047 Uiso 1 1 calc R . . C10 C 0.6097(9) 0.0434(4) 0.4118(3) 0.0341(15) Uani 1 1 d . . . H10A H 0.5869 -0.0009 0.4321 0.041 Uiso 1 1 calc R . . H10B H 0.7126 0.0392 0.3997 0.041 Uiso 1 1 calc R . . C11 C 0.5029(8) 0.0487(4) 0.3682(3) 0.0313(15) Uani 1 1 d . . . C12 C 0.5248(8) 0.1048(4) 0.3316(3) 0.0335(15) Uani 1 1 d . . . C13 C 0.4153(9) 0.1159(4) 0.2932(3) 0.0347(16) Uani 1 1 d . . . C14 C 0.2921(8) 0.0672(4) 0.2912(3) 0.0362(16) Uani 1 1 d . . . H14 H 0.2221 0.0735 0.2653 0.043 Uiso 1 1 calc R . . C15 C 0.2687(9) 0.0090(4) 0.3264(3) 0.0369(16) Uani 1 1 d . . . C16 C 0.3757(9) 0.0018(4) 0.3647(3) 0.0351(15) Uani 1 1 d . . . H16 H 0.3621 -0.0357 0.3890 0.042 Uiso 1 1 calc R . . C17 C 0.1289(9) -0.0421(5) 0.3227(3) 0.0423(18) Uani 1 1 d . . . C18 C 0.1357(11) -0.1064(5) 0.3609(4) 0.059(2) Uani 1 1 d . . . H18A H 0.2273 -0.1345 0.3562 0.089 Uiso 1 1 calc R . . H18B H 0.0508 -0.1393 0.3562 0.089 Uiso 1 1 calc R . . H18C H 0.1333 -0.0859 0.3946 0.089 Uiso 1 1 calc R . . C19 C -0.0139(10) 0.0041(5) 0.3322(3) 0.053(2) Uani 1 1 d . . . H19A H -0.1004 -0.0285 0.3302 0.079 Uiso 1 1 calc R . . H19B H -0.0221 0.0432 0.3072 0.079 Uiso 1 1 calc R . . H19C H -0.0091 0.0266 0.3652 0.079 Uiso 1 1 calc R . . C20 C 0.1193(12) -0.0747(7) 0.2684(4) 0.067(3) Uani 1 1 d . . . H20A H 0.2072 -0.1047 0.2616 0.100 Uiso 1 1 calc R . . H20B H 0.1138 -0.0338 0.2445 0.100 Uiso 1 1 calc R . . H20C H 0.0308 -0.1057 0.2654 0.100 Uiso 1 1 calc R . . C21 C 0.4315(8) 0.1820(4) 0.2575(3) 0.0359(16) Uani 1 1 d . . . H21A H 0.5337 0.1844 0.2445 0.043 Uiso 1 1 d . . . H21B H 0.3627 0.1767 0.2293 0.043 Uiso 1 1 d . . . N N 0.1854(11) 0.2500 0.3696(4) 0.043(2) Uani 1 2 d SD . . H1 H 0.2503 0.2500 0.3441 0.052 Uiso 1 2 d SR . . H2 H 0.0974 0.2500 0.3533 0.052 Uiso 1 2 d SR . . C22 C 0.1862(18) 0.1772(6) 0.3936(4) 0.044(4) Uani 0.50 1 d PD . . C23A C 0.2579(12) 0.1415(7) 0.4430(4) 0.042(3) Uani 0.302(15) 1 d PDU . . C23B C 0.1396(19) 0.1789(7) 0.4481(5) 0.027(3) Uani 0.198(15) 1 d PDU . . C24 C 0.1361(17) 0.0988(7) 0.4696(5) 0.044(3) Uani 0.50 1 d PDU . . C25 C 0.098(2) 0.0992(10) 0.5247(5) 0.054(4) Uani 0.50 1 d PDU . . H25A H 0.1841 0.1147 0.5439 0.081 Uiso 0.50 1 calc PR . . H25B H 0.0675 0.0493 0.5349 0.081 Uiso 0.50 1 calc PR . . H25C H 0.0162 0.1340 0.5306 0.081 Uiso 0.50 1 calc PR . . 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 U 0.0308(3) 0.0451(3) 0.0312(3) 0.000 0.00017(16) 0.000 O1 0.041(4) 0.043(4) 0.038(4) 0.000 -0.002(4) 0.000 O2 0.101(5) 0.035(3) 0.071(4) -0.028(3) -0.049(4) 0.037(3) O3 0.044(3) 0.027(2) 0.037(3) 0.003(2) 0.009(2) 0.002(2) O4 0.048(4) 0.021(3) 0.037(4) 0.000 0.003(3) 0.000 O5 0.035(4) 0.115(9) 0.037(4) 0.000 0.005(4) 0.000 O6 0.035(4) 0.020(3) 0.037(3) 0.000 0.003(3) 0.000 C1 0.035(5) 0.029(5) 0.033(5) 0.000 0.003(4) 0.000 C2 0.039(4) 0.025(4) 0.038(4) -0.002(3) -0.010(3) 0.006(3) C3 0.041(4) 0.023(3) 0.036(4) 0.006(3) -0.005(3) 0.001(3) C4 0.046(6) 0.026(5) 0.036(5) 0.000 0.004(5) 0.000 C5 0.046(7) 0.051(7) 0.036(6) 0.000 0.015(5) 0.000 C6 0.061(11) 0.028(10) 0.085(14) -0.022(9) 0.006(10) -0.021(8) C7 0.076(12) 0.031(8) 0.034(8) 0.002(7) 0.014(8) -0.002(8) C8 0.094(13) 0.043(11) 0.039(8) 0.017(6) 0.005(9) 0.017(8) C9 0.045(4) 0.027(4) 0.046(4) -0.005(3) -0.011(3) 0.007(3) C10 0.047(4) 0.020(3) 0.035(4) -0.003(3) 0.002(3) 0.005(3) C11 0.041(4) 0.017(3) 0.036(3) 0.001(2) 0.002(3) 0.004(3) C12 0.036(3) 0.027(3) 0.038(4) -0.005(3) 0.009(3) 0.004(3) C13 0.049(4) 0.021(3) 0.033(4) 0.001(3) 0.005(3) 0.008(3) C14 0.040(4) 0.033(4) 0.036(4) -0.001(3) -0.005(3) 0.013(3) C15 0.047(4) 0.024(3) 0.040(4) -0.003(3) 0.001(4) 0.006(3) C16 0.044(4) 0.023(3) 0.039(4) 0.002(3) 0.007(3) 0.004(3) C17 0.048(4) 0.036(4) 0.043(4) -0.002(3) -0.001(4) 0.001(3) C18 0.057(5) 0.038(5) 0.083(7) 0.011(5) -0.001(5) -0.010(4) C19 0.052(5) 0.054(5) 0.052(5) 0.011(4) 0.004(4) 0.008(4) C20 0.057(5) 0.074(7) 0.069(6) -0.028(5) 0.009(5) -0.022(5) C21 0.051(4) 0.023(4) 0.033(4) -0.002(3) 0.001(3) 0.007(3) N 0.042(6) 0.046(6) 0.042(5) 0.000 0.003(4) 0.000 C22 0.063(11) 0.031(8) 0.037(8) 0.006(6) 0.011(7) -0.004(7) C23A 0.040(5) 0.043(6) 0.042(5) 0.015(5) 0.005(5) 0.011(5) C23B 0.034(7) 0.022(7) 0.024(7) 0.009(6) 0.015(6) 0.001(6) C24 0.058(6) 0.029(5) 0.044(5) 0.020(5) 0.020(5) 0.004(5) C25 0.070(8) 0.042(7) 0.049(7) 0.011(6) 0.006(7) 0.000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O6 1.791(7) . ? U O5 1.799(9) . ? U O1 2.186(7) . ? U O3 2.205(5) . ? U O3 2.205(5) 7_565 ? U O2 3.022(8) . ? U O4 3.534(7) . ? O1 C1 1.333(12) . ? O1 O2 2.921(8) . ? O1 O3 3.907(8) . ? O2 C10 1.438(8) . ? O2 C9 1.446(10) . ? O2 O3 2.998(9) . ? O3 C12 1.345(9) . ? O3 O4 3.104(8) . ? O3 O3 3.555(10) 7_565 ? O4 C21 1.445(8) . ? O4 C21 1.445(8) 7_565 ? C1 C2 1.416(9) 7_565 ? C1 C2 1.416(9) . ? C2 C3 1.369(10) . ? C2 C9 1.504(10) . ? C3 C4 1.397(9) . ? C4 C3 1.397(9) 7_565 ? C4 C5 1.544(15) . ? C5 C8 1.51(2) . ? C5 C8 1.51(2) 7_565 ? C5 C6 1.51(2) . ? C5 C6 1.52(2) 7_565 ? C5 C7 1.652(17) . ? C5 C7 1.652(17) 7_565 ? C6 C7 1.32(3) . ? C6 C6 1.43(4) 7_565 ? C10 C11 1.496(10) . ? C11 C12 1.399(10) . ? C11 C16 1.403(10) . ? C12 C13 1.419(11) . ? C13 C14 1.392(11) . ? C13 C21 1.507(10) . ? C14 C15 1.401(11) . ? C15 C16 1.395(12) . ? C15 C17 1.536(12) . ? C17 C18 1.520(12) . ? C17 C19 1.527(11) . ? C17 C20 1.551(12) . ? N C22 1.434(9) . ? N C22 1.434(9) 7_565 ? C22 C23B 1.501(9) . ? C22 C23A 1.584(9) . ? C23A C23B 1.247(19) . ? C23A C24 1.493(9) . ? C23B C24 1.525(9) . ? C24 C25 1.496(9) . ? 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 O6 U O5 179.6(3) . . ? O6 U O1 95.1(3) . . ? O5 U O1 85.4(4) . . ? O6 U O3 92.61(19) . . ? O5 U O3 87.1(2) . . ? O1 U O3 125.70(14) . . ? O6 U O3 92.61(19) . 7_565 ? O5 U O3 87.1(2) . 7_565 ? O1 U O3 125.70(14) . 7_565 ? O3 U O3 107.5(3) . 7_565 ? O6 U O2 67.58(17) . . ? O5 U O2 112.63(19) . . ? O1 U O2 65.97(14) . . ? O3 U O2 67.93(17) . . ? O3 U O2 158.87(19) 7_565 . ? O6 U O4 61.2(3) . . ? O5 U O4 118.3(3) . . ? O1 U O4 156.3(2) . . ? O3 U O4 60.32(14) . . ? O3 U O4 60.32(14) 7_565 . ? O2 U O4 101.80(14) . . ? C10 O2 C9 115.8(6) . . ? C21 O4 C21 112.4(7) . 7_565 ? O1 C1 C2 120.6(5) . 7_565 ? O1 C1 C2 120.6(5) . . ? C2 C1 C2 118.7(9) 7_565 . ? C3 C2 C1 119.4(7) . . ? C3 C2 C9 123.9(7) . . ? C1 C2 C9 116.6(7) . . ? C2 C3 C4 122.7(7) . . ? C3 C4 C3 116.9(9) . 7_565 ? C3 C4 C5 121.6(5) . . ? C3 C4 C5 121.6(5) 7_565 . ? C8 C5 C6 115.9(12) . . ? C8 C5 C6 134.1(13) 7_565 . ? C8 C5 C6 134.1(13) . 7_565 ? C8 C5 C6 115.9(12) 7_565 7_565 ? C8 C5 C4 109.1(12) . . ? C8 C5 C4 109.1(12) 7_565 . ? C6 C5 C4 114.6(11) . . ? C6 C5 C4 114.6(11) 7_565 . ? C8 C5 C7 103.2(11) 7_565 . ? C6 C5 C7 103.3(13) 7_565 . ? C4 C5 C7 109.9(7) . . ? C8 C5 C7 103.2(11) . 7_565 ? C6 C5 C7 103.3(13) . 7_565 ? C4 C5 C7 109.9(7) . 7_565 ? C7 C5 C7 138.8(14) . 7_565 ? C7 C6 C6 128.9(10) . 7_565 ? C6 C7 C8 104.3(13) . . ? O2 C9 C2 108.2(6) . . ? O2 C10 C11 107.6(6) . . ? C12 C11 C16 119.0(7) . . ? C12 C11 C10 119.4(6) . . ? C16 C11 C10 121.5(6) . . ? O3 C12 C11 120.7(7) . . ? O3 C12 C13 119.4(6) . . ? C11 C12 C13 119.9(7) . . ? C14 C13 C12 118.6(6) . . ? C14 C13 C21 122.0(7) . . ? C12 C13 C21 119.3(7) . . ? C13 C14 C15 123.0(7) . . ? C16 C15 C14 116.7(7) . . ? C16 C15 C17 122.7(7) . . ? C14 C15 C17 120.6(7) . . ? C15 C16 C11 122.7(7) . . ? C18 C17 C19 108.8(7) . . ? C18 C17 C15 111.4(7) . . ? C19 C17 C15 110.2(7) . . ? C18 C17 C20 110.0(8) . . ? C19 C17 C20 107.7(7) . . ? C15 C17 C20 108.6(7) . . ? O4 C21 C13 107.5(5) . . ? C22 N C22 127.5(13) . 7_565 ? N C22 C23B 113.9(11) . . ? N C22 C23A 136.4(12) . . ? C24 C23A C22 107.5(9) . . ? C22 C23B C24 110.2(9) . . ? C23A C24 C25 128.5(14) . . ? C25 C24 C23B 111.3(12) . . ? 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 N H1 O4 0.89 2.02 2.908(12) 179.6 . N H2 O5 0.89 2.02 2.790(13) 144.5 1_455 #===END data_6 _database_code_CSD 172886 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H69 N O9 U' _chemical_formula_weight 1006.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.2169(6) _cell_length_b 16.5010(5) _cell_length_c 24.4065(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.739(2) _cell_angle_gamma 90.00 _cell_volume 9366.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 63517 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent intense orange' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method ? _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 3.517 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.580 _exptl_absorpt_correction_T_max 0.839 _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 63517 _diffrn_reflns_av_R_equivalents 0.0822 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.68 _reflns_number_total 17694 _reflns_number_gt 12894 _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. Solvent accessible voids of 84 A^3^ may indicate the presence of unresolved solvent molecules. The hydrogen atoms bound to O and 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 (three N-H bond lengths are shorter than usual, but have been kept as experimentally found). 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. The highest residual electron density peak may correspond to an unresolved solvent molecule. 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^)+(0.0253P)^2^+8.1354P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00022(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 17694 _refine_ls_number_parameters 1034 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.817 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.113 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 0.096920(9) 0.695763(13) 0.284035(11) 0.03110(7) Uani 1 1 d . . . O1A O 0.01007(16) 0.7558(2) 0.25820(19) 0.0345(10) Uani 1 1 d . . . O2A O 0.01506(16) 0.6556(2) 0.16307(18) 0.0341(9) Uani 1 1 d . . . O3A O 0.13955(17) 0.6774(2) 0.22129(18) 0.0343(9) Uani 1 1 d . . . O4A O 0.19801(17) 0.5571(3) 0.31682(19) 0.0403(11) Uani 1 1 d . . . O5A O 0.15603(17) 0.6871(2) 0.37883(19) 0.0387(10) Uani 1 1 d . . . O6A O 0.03682(18) 0.6651(3) 0.36759(19) 0.0436(11) Uani 1 1 d . . . O7A O 0.12006(17) 0.7980(2) 0.28733(19) 0.0376(10) Uani 1 1 d . . . O8A O 0.07362(16) 0.5929(2) 0.28027(17) 0.0300(9) Uani 1 1 d . . . C1A C -0.0550(2) 0.6878(4) 0.2920(3) 0.0330(13) Uani 1 1 d . . . C2A C -0.0373(2) 0.7086(3) 0.2457(3) 0.0314(13) Uani 1 1 d . . . C3A C -0.0666(2) 0.6800(3) 0.1886(3) 0.0329(14) Uani 1 1 d . . . C4A C -0.1181(3) 0.6390(4) 0.1757(3) 0.0375(15) Uani 1 1 d . . . H4A H -0.1381 0.6202 0.1373 0.045 Uiso 1 1 calc R . . C5A C -0.1406(3) 0.6253(4) 0.2183(3) 0.0350(14) Uani 1 1 d . . . C6A C -0.1069(3) 0.6468(4) 0.2770(3) 0.0375(14) Uani 1 1 d . . . H6A H -0.1196 0.6332 0.3068 0.045 Uiso 1 1 calc R . . C7A C -0.1997(3) 0.5865(4) 0.2044(3) 0.0413(15) Uani 1 1 d . . . C8A C -0.2369(3) 0.6447(4) 0.2243(3) 0.0442(16) Uani 1 1 d . . . H8A1 H -0.2200 0.6508 0.2667 0.066 Uiso 1 1 calc R . . H8A2 H -0.2750 0.6229 0.2127 0.066 Uiso 1 1 calc R . . H8A3 H -0.2387 0.6966 0.2059 0.066 Uiso 1 1 calc R . . C9A C -0.2322(3) 0.5709(5) 0.1388(4) 0.061(2) Uani 1 1 d . . . H9A1 H -0.2364 0.6208 0.1173 0.092 Uiso 1 1 calc R . . H9A2 H -0.2695 0.5494 0.1323 0.092 Uiso 1 1 calc R . . H9A3 H -0.2113 0.5326 0.1252 0.092 Uiso 1 1 calc R . . C10A C -0.1932(3) 0.5050(4) 0.2384(4) 0.058(2) Uani 1 1 d . . . H10A H -0.1716 0.4676 0.2250 0.087 Uiso 1 1 calc R . . H10B H -0.2305 0.4828 0.2308 0.087 Uiso 1 1 calc R . . H10C H -0.1733 0.5143 0.2802 0.087 Uiso 1 1 calc R . . C11A C -0.0405(2) 0.6936(4) 0.1428(3) 0.0335(13) Uani 1 1 d . . . H11A H -0.0652 0.6706 0.1049 0.040 Uiso 1 1 calc R . . H11B H -0.0366 0.7512 0.1373 0.040 Uiso 1 1 calc R . . C12A C 0.0400(3) 0.6529(4) 0.1191(3) 0.0368(14) Uani 1 1 d . . . H12A H 0.0538 0.7063 0.1145 0.044 Uiso 1 1 calc R . . H12B H 0.0112 0.6363 0.0812 0.044 Uiso 1 1 calc R . . C13A C 0.0892(3) 0.5933(4) 0.1388(3) 0.0343(14) Uani 1 1 d . . . C14A C 0.1363(2) 0.6083(3) 0.1915(3) 0.0309(13) Uani 1 1 d . . . C15A C 0.1799(3) 0.5491(4) 0.2137(3) 0.0365(14) Uani 1 1 d . . . C16A C 0.1767(2) 0.4808(4) 0.1815(3) 0.0337(14) Uani 1 1 d . . . H16A H 0.2061 0.4429 0.1962 0.040 Uiso 1 1 calc R . . C17A C 0.1314(3) 0.4646(4) 0.1272(3) 0.0355(14) Uani 1 1 d . . . C18A C 0.0878(3) 0.5221(4) 0.1081(3) 0.0352(14) Uani 1 1 d . . . H18A H 0.0561 0.5123 0.0732 0.042 Uiso 1 1 calc R . . C19A C 0.1310(3) 0.3860(4) 0.0939(3) 0.0389(15) Uani 1 1 d . . . C20A C 0.0737(3) 0.3723(4) 0.0418(3) 0.0532(19) Uani 1 1 d . . . H20A H 0.0660 0.4171 0.0148 0.080 Uiso 1 1 calc R . . H20B H 0.0435 0.3679 0.0564 0.080 Uiso 1 1 calc R . . H20C H 0.0757 0.3232 0.0215 0.080 Uiso 1 1 calc R . . C21A C 0.1774(4) 0.3904(4) 0.0678(4) 0.058(2) Uani 1 1 d . . . H21A H 0.1776 0.3408 0.0473 0.087 Uiso 1 1 calc R . . H21B H 0.2144 0.3983 0.0992 0.087 Uiso 1 1 calc R . . H21C H 0.1693 0.4349 0.0404 0.087 Uiso 1 1 calc R . . C22A C 0.1422(3) 0.3128(4) 0.1360(3) 0.0433(16) Uani 1 1 d . . . H22A H 0.1388 0.2637 0.1139 0.065 Uiso 1 1 calc R . . H22B H 0.1145 0.3126 0.1542 0.065 Uiso 1 1 calc R . . H22C H 0.1802 0.3167 0.1663 0.065 Uiso 1 1 calc R . . C23A C 0.2256(3) 0.5622(4) 0.2749(3) 0.0389(15) Uani 1 1 d . . . H23A H 0.2552 0.5210 0.2836 0.047 Uiso 1 1 calc R . . H23B H 0.2433 0.6149 0.2773 0.047 Uiso 1 1 calc R . . C24A C 0.2367(3) 0.5694(4) 0.3782(3) 0.0392(15) Uani 1 1 d . . . H24A H 0.2534 0.6232 0.3834 0.047 Uiso 1 1 calc R . . H24B H 0.2675 0.5298 0.3897 0.047 Uiso 1 1 calc R . . C25A C 0.2018(3) 0.5597(4) 0.4151(3) 0.0365(14) Uani 1 1 d . . . C26A C 0.1603(3) 0.6194(4) 0.4116(3) 0.0358(14) Uani 1 1 d . . . C27A C 0.1224(3) 0.6072(4) 0.4397(3) 0.0356(14) Uani 1 1 d . . . C28A C 0.1286(3) 0.5375(4) 0.4742(3) 0.0407(15) Uani 1 1 d . . . H28A H 0.1038 0.5300 0.4937 0.049 Uiso 1 1 calc R . . C29A C 0.1701(3) 0.4787(4) 0.4806(3) 0.0375(15) Uani 1 1 d . . . C30A C 0.2056(3) 0.4918(4) 0.4491(3) 0.0379(15) Uani 1 1 d . . . H30A H 0.2330 0.4528 0.4513 0.046 Uiso 1 1 calc R . . C31A C 0.1735(3) 0.4029(4) 0.5185(3) 0.0454(17) Uani 1 1 d . . . C32A C 0.2267(3) 0.3507(4) 0.5255(3) 0.0514(18) Uani 1 1 d . . . H32A H 0.2611 0.3817 0.5453 0.077 Uiso 1 1 calc R . . H32B H 0.2248 0.3345 0.4870 0.077 Uiso 1 1 calc R . . H32C H 0.2273 0.3034 0.5486 0.077 Uiso 1 1 calc R . . C33A C 0.1197(3) 0.3510(5) 0.4879(4) 0.070(2) Uani 1 1 d . . . H33A H 0.1197 0.3067 0.5133 0.105 Uiso 1 1 calc R . . H33B H 0.1199 0.3303 0.4511 0.105 Uiso 1 1 calc R . . H33C H 0.0860 0.3836 0.4799 0.105 Uiso 1 1 calc R . . C34A C 0.1782(3) 0.4272(5) 0.5804(3) 0.058(2) Uani 1 1 d . . . H34A H 0.1461 0.4609 0.5773 0.087 Uiso 1 1 calc R . . H34B H 0.2133 0.4567 0.6001 0.087 Uiso 1 1 calc R . . H34C H 0.1782 0.3795 0.6029 0.087 Uiso 1 1 calc R . . C35A C 0.0740(3) 0.6675(4) 0.4295(3) 0.0437(16) Uani 1 1 d . . . H35A H 0.0526 0.6534 0.4537 0.052 Uiso 1 1 calc R . . H35B H 0.0895 0.7216 0.4404 0.052 Uiso 1 1 calc R . . C36A C -0.0169(2) 0.7069(4) 0.3548(3) 0.0385(15) Uani 1 1 d . . . H36A H -0.0105 0.7649 0.3598 0.046 Uiso 1 1 calc R . . H36B H -0.0346 0.6889 0.3816 0.046 Uiso 1 1 calc R . . U2 U 0.449332(10) 0.419860(13) 0.659062(10) 0.03067(7) Uani 1 1 d . . . O1B O 0.48902(17) 0.3570(2) 0.74818(18) 0.0349(9) Uani 1 1 d . . . O2B O 0.57452(17) 0.4349(3) 0.71566(19) 0.0390(10) Uani 1 1 d . . . O3B O 0.49090(16) 0.4259(2) 0.59417(18) 0.0324(9) Uani 1 1 d . . . O4B O 0.40420(16) 0.5567(3) 0.55887(19) 0.0394(11) Uani 1 1 d . . . O5B O 0.35623(17) 0.4420(2) 0.6222(2) 0.0391(10) Uani 1 1 d . . . O6B O 0.40063(18) 0.4692(3) 0.7503(2) 0.0426(11) Uani 1 1 d . . . O7B O 0.43102(18) 0.3181(2) 0.63406(18) 0.0356(10) Uani 1 1 d . . . O8B O 0.46761(16) 0.5211(2) 0.68457(18) 0.0315(9) Uani 1 1 d . . . C1B C 0.4879(3) 0.4321(4) 0.8308(3) 0.0404(15) Uani 1 1 d . . . C2B C 0.5177(3) 0.4011(4) 0.7972(3) 0.0377(15) Uani 1 1 d . . . C3B C 0.5760(3) 0.4171(3) 0.8130(3) 0.0350(14) Uani 1 1 d . . . C4B C 0.6057(3) 0.4560(4) 0.8670(3) 0.0415(16) Uani 1 1 d . . . H4B H 0.6446 0.4669 0.8779 0.050 Uiso 1 1 calc R . . C5B C 0.5797(3) 0.4789(4) 0.9047(3) 0.0429(16) Uani 1 1 d . . . C6B C 0.5206(3) 0.4705(4) 0.8843(3) 0.0436(16) Uani 1 1 d . . . H6B H 0.5017 0.4913 0.9072 0.052 Uiso 1 1 calc R . . C7B C 0.6169(4) 0.5137(4) 0.9660(3) 0.058(2) Uani 1 1 d . . . C8B C 0.6476(4) 0.5896(4) 0.9602(4) 0.071(3) Uani 1 1 d . . . H8B1 H 0.6199 0.6311 0.9411 0.107 Uiso 1 1 calc R . . H8B2 H 0.6698 0.5783 0.9368 0.107 Uiso 1 1 calc R . . H8B3 H 0.6727 0.6078 0.9990 0.107 Uiso 1 1 calc R . . C9B C 0.5809(4) 0.5332(5) 1.0025(4) 0.080(3) Uani 1 1 d . . . H9B1 H 0.6057 0.5518 1.0412 0.121 Uiso 1 1 calc R . . H9B2 H 0.5610 0.4853 1.0063 0.121 Uiso 1 1 calc R . . H9B3 H 0.5535 0.5747 0.9828 0.121 Uiso 1 1 calc R . . C10B C 0.6612(4) 0.4478(5) 1.0007(3) 0.070(2) Uani 1 1 d . . . H10D H 0.6827 0.4664 1.0404 0.105 Uiso 1 1 calc R . . H10E H 0.6869 0.4375 0.9811 0.105 Uiso 1 1 calc R . . H10F H 0.6412 0.3987 1.0021 0.105 Uiso 1 1 calc R . . C11B C 0.6038(3) 0.3942(4) 0.7708(3) 0.0389(15) Uani 1 1 d . . . H11C H 0.6440 0.4098 0.7872 0.047 Uiso 1 1 calc R . . H11D H 0.6015 0.3361 0.7646 0.047 Uiso 1 1 calc R . . C12B C 0.6047(3) 0.4305(4) 0.6759(3) 0.0373(14) Uani 1 1 d . . . H12C H 0.5996 0.3774 0.6575 0.045 Uiso 1 1 calc R . . H12D H 0.6455 0.4395 0.6977 0.045 Uiso 1 1 calc R . . C13B C 0.5803(2) 0.4943(3) 0.6297(3) 0.0321(13) Uani 1 1 d . . . C14B C 0.5216(2) 0.4911(3) 0.5915(3) 0.0307(13) Uani 1 1 d . . . C15B C 0.4963(2) 0.5548(3) 0.5529(3) 0.0303(13) Uani 1 1 d . . . C16B C 0.5301(2) 0.6179(4) 0.5491(3) 0.0339(14) Uani 1 1 d . . . H16B H 0.5130 0.6598 0.5226 0.041 Uiso 1 1 calc R . . C17B C 0.5897(3) 0.6221(3) 0.5834(3) 0.0348(14) Uani 1 1 d . . . C18B C 0.6129(2) 0.5604(3) 0.6239(3) 0.0318(13) Uani 1 1 d . . . H18B H 0.6518 0.5626 0.6483 0.038 Uiso 1 1 calc R . . C19B C 0.6261(3) 0.6925(4) 0.5758(3) 0.0396(15) Uani 1 1 d . . . C20B C 0.6902(3) 0.6789(4) 0.6109(4) 0.054(2) Uani 1 1 d . . . H20D H 0.7117 0.7208 0.6014 0.082 Uiso 1 1 calc R . . H20E H 0.7011 0.6271 0.6007 0.082 Uiso 1 1 calc R . . H20F H 0.6981 0.6803 0.6527 0.082 Uiso 1 1 calc R . . C21B C 0.6098(3) 0.7704(4) 0.5991(4) 0.058(2) Uani 1 1 d . . . H21D H 0.6123 0.7620 0.6390 0.086 Uiso 1 1 calc R . . H21E H 0.5711 0.7853 0.5742 0.086 Uiso 1 1 calc R . . H21F H 0.6356 0.8130 0.5988 0.086 Uiso 1 1 calc R . . C22B C 0.6174(3) 0.7008(5) 0.5100(3) 0.058(2) Uani 1 1 d . . . H22D H 0.6422 0.7425 0.5060 0.086 Uiso 1 1 calc R . . H22E H 0.5781 0.7146 0.4868 0.086 Uiso 1 1 calc R . . H22F H 0.6266 0.6503 0.4962 0.086 Uiso 1 1 calc R . . C23B C 0.4326(2) 0.5514(4) 0.5175(3) 0.0366(15) Uani 1 1 d . . . H23C H 0.4208 0.5960 0.4895 0.044 Uiso 1 1 calc R . . H23D H 0.4225 0.5010 0.4954 0.044 Uiso 1 1 calc R . . C24B C 0.3425(2) 0.5532(4) 0.5308(3) 0.0374(15) Uani 1 1 d . . . H24C H 0.3302 0.5001 0.5135 0.045 Uiso 1 1 calc R . . H24D H 0.3284 0.5934 0.4995 0.045 Uiso 1 1 calc R . . C25B C 0.3194(2) 0.5700(4) 0.5783(3) 0.0345(14) Uani 1 1 d . . . C26B C 0.3324(2) 0.5139(4) 0.6245(3) 0.0363(14) Uani 1 1 d . . . C27B C 0.3208(2) 0.5328(4) 0.6752(3) 0.0365(14) Uani 1 1 d . . . C28B C 0.2922(3) 0.6067(4) 0.6751(3) 0.0398(15) Uani 1 1 d . . . H28B H 0.2839 0.6195 0.7081 0.048 Uiso 1 1 calc R . . C29B C 0.2758(3) 0.6610(4) 0.6277(3) 0.0417(16) Uani 1 1 d . . . C30B C 0.2911(2) 0.6411(4) 0.5801(3) 0.0401(15) Uani 1 1 d . . . H30B H 0.2818 0.6770 0.5484 0.048 Uiso 1 1 calc R . . C31B C 0.2435(3) 0.7388(5) 0.6277(3) 0.0487(18) Uani 1 1 d . . . C32B C 0.2549(3) 0.7684(5) 0.6894(4) 0.059(2) Uani 1 1 d . . . H32D H 0.2381 0.8211 0.6873 0.089 Uiso 1 1 calc R . . H32E H 0.2956 0.7716 0.7117 0.089 Uiso 1 1 calc R . . H32F H 0.2382 0.7314 0.7086 0.089 Uiso 1 1 calc R . . C33B C 0.1814(4) 0.7264(6) 0.5953(5) 0.091(3) Uani 1 1 d U . . H33D H 0.1739 0.7112 0.5550 0.137 Uiso 1 1 calc R . . H33E H 0.1613 0.7758 0.5956 0.137 Uiso 1 1 calc R . . H33F H 0.1684 0.6842 0.6142 0.137 Uiso 1 1 calc R . . C34B C 0.2641(4) 0.8088(5) 0.5985(4) 0.083(3) Uani 1 1 d . . . H34D H 0.2498 0.8005 0.5563 0.125 Uiso 1 1 calc R . . H34E H 0.3054 0.8100 0.6144 0.125 Uiso 1 1 calc R . . H34F H 0.2498 0.8594 0.6068 0.125 Uiso 1 1 calc R . . C35B C 0.3394(3) 0.4764(4) 0.7264(3) 0.0440(16) Uani 1 1 d . . . H35C H 0.3268 0.4966 0.7567 0.053 Uiso 1 1 calc R . . H35D H 0.3221 0.4236 0.7137 0.053 Uiso 1 1 calc R . . C36B C 0.4241(3) 0.4254(4) 0.8061(3) 0.0411(15) Uani 1 1 d . . . H36C H 0.4128 0.3689 0.7996 0.049 Uiso 1 1 calc R . . H36D H 0.4091 0.4479 0.8340 0.049 Uiso 1 1 calc R . . N1A N 0.0055(2) 0.4239(3) 0.2422(2) 0.0350(12) Uani 1 1 d . . . H1A H 0.0328 0.4294 0.2701 0.042 Uiso 1 1 d R . . H2A H -0.0008 0.3805 0.2462 0.042 Uiso 1 1 d R . . C37A C -0.0104(3) 0.4512(4) 0.1799(3) 0.0396(15) Uani 1 1 d . . . H37A H 0.0166 0.4286 0.1645 0.048 Uiso 1 1 calc R . . H37B H -0.0074 0.5098 0.1792 0.048 Uiso 1 1 calc R . . C38A C -0.0704(3) 0.4264(4) 0.1402(3) 0.0442(16) Uani 1 1 d . . . H38A H -0.0977 0.4543 0.1526 0.053 Uiso 1 1 calc R . . H38B H -0.0749 0.3686 0.1444 0.053 Uiso 1 1 calc R . . C39A C -0.0834(3) 0.4460(4) 0.0752(3) 0.057(2) Uani 1 1 d . . . H39A H -0.0805 0.5040 0.0707 0.068 Uiso 1 1 calc R . . H39B H -0.0551 0.4198 0.0632 0.068 Uiso 1 1 calc R . . C40A C -0.1434(4) 0.4177(5) 0.0347(4) 0.072(2) Uani 1 1 d . . . H40A H -0.1468 0.3605 0.0396 0.107 Uiso 1 1 calc R . . H40B H -0.1495 0.4290 -0.0059 0.107 Uiso 1 1 calc R . . H40C H -0.1716 0.4459 0.0448 0.107 Uiso 1 1 calc R . . C41A C -0.0259(3) 0.4638(4) 0.2762(3) 0.0386(15) Uani 1 1 d . . . H41A H -0.0647 0.4426 0.2627 0.046 Uiso 1 1 calc R . . H41B H -0.0282 0.5217 0.2687 0.046 Uiso 1 1 calc R . . C42A C 0.0046(4) 0.4486(5) 0.3417(3) 0.063(2) Uani 1 1 d . . . H42A H 0.0403 0.4789 0.3563 0.075 Uiso 1 1 calc R . . H42B H 0.0141 0.3915 0.3480 0.075 Uiso 1 1 calc R . . C43A C -0.0311(4) 0.4723(5) 0.3773(4) 0.064(2) Uani 1 1 d . . . H43A H -0.0056 0.4925 0.4158 0.076 Uiso 1 1 calc R . . H43B H -0.0570 0.5159 0.3569 0.076 Uiso 1 1 calc R . . C44A C -0.0629(5) 0.4078(7) 0.3853(6) 0.110(4) Uani 1 1 d U . . H44A H -0.0764 0.3748 0.3502 0.165 Uiso 1 1 calc R . . H44B H -0.0952 0.4283 0.3926 0.165 Uiso 1 1 calc R . . H44C H -0.0391 0.3758 0.4185 0.165 Uiso 1 1 calc R . . N1B N 0.4922(2) 0.6880(3) 0.7512(2) 0.0363(12) Uani 1 1 d . . . H1B H 0.4815 0.6873 0.7173 0.044 Uiso 1 1 d R . . H2B H 0.4977 0.7446 0.7583 0.044 Uiso 1 1 d R . . C37B C 0.4467(3) 0.6629(4) 0.7727(3) 0.0416(16) Uani 1 1 d . . . H37C H 0.4434 0.6043 0.7710 0.050 Uiso 1 1 calc R . . H37D H 0.4101 0.6852 0.7465 0.050 Uiso 1 1 calc R . . C38B C 0.4594(3) 0.6909(4) 0.8359(3) 0.0491(17) Uani 1 1 d . . . H38C H 0.4673 0.7487 0.8389 0.059 Uiso 1 1 calc R . . H38D H 0.4934 0.6633 0.8629 0.059 Uiso 1 1 calc R . . C39B C 0.4089(3) 0.6736(5) 0.8542(4) 0.060(2) Uani 1 1 d . . . H39C H 0.4014 0.6158 0.8521 0.072 Uiso 1 1 calc R . . H39D H 0.3746 0.7005 0.8269 0.072 Uiso 1 1 calc R . . C40B C 0.4222(4) 0.7036(5) 0.9175(4) 0.079(3) Uani 1 1 d . . . H40D H 0.4535 0.6729 0.9450 0.119 Uiso 1 1 calc R . . H40E H 0.3888 0.6969 0.9270 0.119 Uiso 1 1 calc R . . H40F H 0.4325 0.7599 0.9204 0.119 Uiso 1 1 calc R . . C41B C 0.5496(3) 0.6493(4) 0.7816(3) 0.0409(15) Uani 1 1 d . . . H41C H 0.5449 0.5915 0.7851 0.049 Uiso 1 1 calc R . . H41D H 0.5682 0.6716 0.8213 0.049 Uiso 1 1 calc R . . C42B C 0.5866(3) 0.6647(4) 0.7463(3) 0.0524(18) Uani 1 1 d . . . H42C H 0.5734 0.6299 0.7116 0.063 Uiso 1 1 calc R . . H42D H 0.5811 0.7204 0.7325 0.063 Uiso 1 1 calc R . . C43B C 0.6499(3) 0.6502(5) 0.7804(4) 0.059(2) Uani 1 1 d . . . H43C H 0.6685 0.6434 0.7526 0.070 Uiso 1 1 calc R . . H43D H 0.6550 0.6003 0.8030 0.070 Uiso 1 1 calc R . . C44B C 0.6784(3) 0.7189(5) 0.8224(4) 0.079(3) Uani 1 1 d . . . H44D H 0.6709 0.7690 0.8008 0.118 Uiso 1 1 calc R . . H44E H 0.7191 0.7097 0.8402 0.118 Uiso 1 1 calc R . . H44F H 0.6632 0.7217 0.8529 0.118 Uiso 1 1 calc R . . O9A O 0.12200(18) 0.4262(3) 0.2948(2) 0.0492(12) Uani 1 1 d . . . H9A H 0.1415 0.4722 0.2982 0.059 Uiso 1 1 d R . . C45A C 0.1614(3) 0.3605(4) 0.3097(3) 0.0493(18) Uani 1 1 d . . . H45A H 0.1888 0.3685 0.2916 0.074 Uiso 1 1 calc R . . H45B H 0.1409 0.3108 0.2955 0.074 Uiso 1 1 calc R . . H45C H 0.1813 0.3579 0.3520 0.074 Uiso 1 1 calc R . . O9B O 0.4424(2) 0.6914(3) 0.6299(2) 0.0515(12) Uani 1 1 d . . . H9B H 0.4341 0.6453 0.6070 0.062 Uiso 1 1 d R . . C45B C 0.4253(3) 0.7505(4) 0.5842(3) 0.057(2) Uani 1 1 d . . . H45D H 0.4318 0.8037 0.6016 0.086 Uiso 1 1 calc R . . H45E H 0.3852 0.7440 0.5601 0.086 Uiso 1 1 calc R . . H45F H 0.4473 0.7440 0.5601 0.086 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 0.03034(12) 0.02789(11) 0.03376(14) 0.00006(10) 0.01096(10) -0.00071(10) O1A 0.030(2) 0.028(2) 0.040(3) -0.0042(19) 0.0087(19) 0.0032(17) O2A 0.032(2) 0.039(2) 0.031(2) 0.0063(19) 0.0118(19) 0.0083(19) O3A 0.037(2) 0.033(2) 0.034(2) -0.0024(18) 0.0144(19) -0.0066(18) O4A 0.032(2) 0.057(3) 0.029(2) 0.000(2) 0.0075(19) -0.009(2) O5A 0.041(2) 0.033(2) 0.036(3) 0.004(2) 0.009(2) -0.0012(19) O6A 0.040(2) 0.056(3) 0.029(2) -0.003(2) 0.006(2) 0.016(2) O7A 0.037(2) 0.030(2) 0.045(3) -0.004(2) 0.014(2) -0.0037(18) O8A 0.027(2) 0.031(2) 0.028(2) -0.0014(17) 0.0072(17) 0.0004(17) C1A 0.031(3) 0.034(3) 0.034(4) 0.000(3) 0.012(3) 0.003(3) C2A 0.031(3) 0.026(3) 0.037(4) 0.000(3) 0.013(3) 0.004(2) C3A 0.033(3) 0.026(3) 0.039(4) 0.004(3) 0.012(3) 0.002(3) C4A 0.034(3) 0.031(3) 0.045(4) -0.001(3) 0.012(3) 0.007(3) C5A 0.036(3) 0.034(3) 0.037(4) 0.000(3) 0.016(3) 0.003(3) C6A 0.034(3) 0.038(3) 0.042(4) 0.000(3) 0.016(3) 0.002(3) C7A 0.031(3) 0.043(4) 0.049(4) -0.005(3) 0.015(3) -0.003(3) C8A 0.034(3) 0.040(4) 0.059(5) 0.005(3) 0.019(3) 0.000(3) C9A 0.041(4) 0.079(6) 0.063(5) -0.023(4) 0.020(4) -0.017(4) C10A 0.045(4) 0.043(4) 0.086(6) 0.003(4) 0.026(4) -0.003(3) C11A 0.032(3) 0.032(3) 0.032(3) 0.005(3) 0.008(3) 0.001(3) C12A 0.041(3) 0.038(3) 0.033(4) 0.005(3) 0.016(3) 0.001(3) C13A 0.036(3) 0.035(3) 0.034(4) 0.008(3) 0.016(3) 0.002(3) C14A 0.033(3) 0.032(3) 0.031(3) 0.000(3) 0.016(3) -0.001(3) C15A 0.031(3) 0.044(4) 0.036(4) 0.000(3) 0.015(3) -0.005(3) C16A 0.032(3) 0.038(3) 0.033(4) 0.008(3) 0.015(3) 0.007(3) C17A 0.036(3) 0.041(3) 0.032(4) 0.004(3) 0.015(3) 0.001(3) C18A 0.036(3) 0.039(3) 0.028(3) 0.007(3) 0.010(3) -0.005(3) C19A 0.044(4) 0.042(4) 0.035(4) 0.000(3) 0.020(3) 0.006(3) C20A 0.060(5) 0.050(4) 0.042(4) -0.012(3) 0.012(4) 0.011(4) C21A 0.085(6) 0.047(4) 0.061(5) 0.003(4) 0.049(5) 0.016(4) C22A 0.049(4) 0.043(4) 0.040(4) -0.002(3) 0.019(3) -0.002(3) C23A 0.030(3) 0.044(4) 0.044(4) -0.001(3) 0.016(3) -0.006(3) C24A 0.031(3) 0.044(4) 0.034(4) 0.000(3) 0.003(3) -0.004(3) C25A 0.034(3) 0.038(3) 0.031(4) -0.006(3) 0.004(3) -0.008(3) C26A 0.038(3) 0.034(3) 0.032(4) -0.003(3) 0.009(3) -0.001(3) C27A 0.035(3) 0.034(3) 0.034(4) -0.001(3) 0.010(3) 0.002(3) C28A 0.034(3) 0.052(4) 0.031(4) -0.001(3) 0.007(3) -0.008(3) C29A 0.031(3) 0.040(3) 0.030(4) 0.001(3) -0.001(3) -0.004(3) C30A 0.037(3) 0.036(3) 0.033(4) 0.000(3) 0.005(3) -0.002(3) C31A 0.042(4) 0.046(4) 0.040(4) 0.008(3) 0.007(3) -0.009(3) C32A 0.055(4) 0.042(4) 0.045(5) 0.011(3) 0.006(4) -0.003(3) C33A 0.065(5) 0.061(5) 0.059(5) 0.019(4) -0.003(4) -0.026(4) C34A 0.055(4) 0.068(5) 0.045(5) 0.019(4) 0.013(4) -0.005(4) C35A 0.045(4) 0.051(4) 0.030(4) -0.008(3) 0.009(3) 0.004(3) C36A 0.031(3) 0.042(4) 0.042(4) -0.001(3) 0.014(3) 0.007(3) U2 0.03495(12) 0.02852(12) 0.02989(13) -0.00125(10) 0.01403(10) -0.00237(10) O1B 0.045(2) 0.028(2) 0.029(2) -0.0032(18) 0.011(2) -0.0025(19) O2B 0.035(2) 0.046(3) 0.035(3) 0.011(2) 0.013(2) 0.009(2) O3B 0.035(2) 0.032(2) 0.034(2) -0.0043(18) 0.0169(19) -0.0033(18) O4B 0.026(2) 0.060(3) 0.032(2) -0.008(2) 0.0110(19) -0.001(2) O5B 0.035(2) 0.034(2) 0.051(3) -0.010(2) 0.020(2) -0.0062(19) O6B 0.040(2) 0.042(2) 0.050(3) 0.013(2) 0.022(2) 0.001(2) O7B 0.045(2) 0.028(2) 0.034(2) -0.0020(18) 0.017(2) -0.0013(19) O8B 0.033(2) 0.032(2) 0.031(2) -0.0005(18) 0.0132(18) 0.0013(18) C1B 0.058(4) 0.031(3) 0.035(4) 0.001(3) 0.021(3) 0.000(3) C2B 0.051(4) 0.030(3) 0.029(4) 0.001(3) 0.012(3) 0.000(3) C3B 0.046(4) 0.027(3) 0.027(3) 0.006(3) 0.007(3) 0.004(3) C4B 0.050(4) 0.028(3) 0.037(4) 0.006(3) 0.007(3) 0.001(3) C5B 0.059(4) 0.035(3) 0.023(3) -0.001(3) 0.003(3) -0.001(3) C6B 0.067(5) 0.034(3) 0.030(4) -0.001(3) 0.018(3) 0.005(3) C7B 0.080(6) 0.047(4) 0.034(4) -0.004(3) 0.009(4) -0.001(4) C8B 0.094(6) 0.049(5) 0.047(5) -0.009(4) 0.001(5) -0.014(4) C9B 0.116(8) 0.075(6) 0.039(5) -0.022(4) 0.019(5) 0.007(6) C10B 0.100(7) 0.055(5) 0.035(5) -0.002(4) 0.004(4) 0.007(5) C11B 0.038(3) 0.038(3) 0.033(4) 0.007(3) 0.004(3) 0.006(3) C12B 0.039(3) 0.041(3) 0.035(4) 0.006(3) 0.017(3) 0.004(3) C13B 0.033(3) 0.030(3) 0.037(4) -0.002(3) 0.018(3) 0.002(3) C14B 0.035(3) 0.030(3) 0.031(3) -0.006(3) 0.016(3) -0.002(3) C15B 0.032(3) 0.035(3) 0.026(3) -0.004(2) 0.013(3) 0.001(3) C16B 0.034(3) 0.034(3) 0.038(4) 0.002(3) 0.019(3) 0.003(3) C17B 0.045(4) 0.031(3) 0.036(4) -0.011(3) 0.023(3) -0.008(3) C18B 0.026(3) 0.038(3) 0.030(3) 0.000(3) 0.010(3) 0.002(3) C19B 0.042(3) 0.037(3) 0.042(4) -0.004(3) 0.019(3) -0.006(3) C20B 0.043(4) 0.045(4) 0.073(6) -0.004(4) 0.021(4) -0.010(3) C21B 0.062(5) 0.043(4) 0.077(6) -0.006(4) 0.036(5) -0.003(4) C22B 0.071(5) 0.061(5) 0.043(5) -0.001(4) 0.026(4) -0.016(4) C23B 0.037(3) 0.046(4) 0.032(4) -0.004(3) 0.019(3) 0.001(3) C24B 0.030(3) 0.047(4) 0.033(4) -0.006(3) 0.011(3) 0.002(3) C25B 0.021(3) 0.039(3) 0.042(4) -0.010(3) 0.011(3) 0.000(3) C26B 0.029(3) 0.035(3) 0.045(4) -0.009(3) 0.016(3) -0.004(3) C27B 0.030(3) 0.045(4) 0.036(4) -0.003(3) 0.014(3) -0.009(3) C28B 0.032(3) 0.047(4) 0.042(4) -0.012(3) 0.017(3) -0.007(3) C29B 0.037(3) 0.048(4) 0.042(4) -0.006(3) 0.018(3) -0.001(3) C30B 0.029(3) 0.052(4) 0.037(4) -0.002(3) 0.009(3) 0.000(3) C31B 0.041(4) 0.060(4) 0.043(4) -0.006(4) 0.013(3) 0.014(3) C32B 0.050(4) 0.055(5) 0.071(6) -0.015(4) 0.021(4) 0.011(4) C33B 0.066(5) 0.089(6) 0.098(7) -0.044(5) 0.009(5) 0.025(4) C34B 0.103(7) 0.059(5) 0.089(7) -0.001(5) 0.038(6) 0.030(5) C35B 0.044(4) 0.043(4) 0.053(5) -0.001(3) 0.027(4) -0.004(3) C36B 0.054(4) 0.036(3) 0.037(4) -0.001(3) 0.023(3) -0.001(3) N1A 0.033(3) 0.028(3) 0.036(3) -0.004(2) 0.005(2) -0.003(2) C37A 0.042(4) 0.037(3) 0.043(4) 0.005(3) 0.020(3) 0.000(3) C38A 0.044(4) 0.038(4) 0.047(4) -0.001(3) 0.013(3) -0.003(3) C39A 0.068(5) 0.045(4) 0.050(5) 0.007(3) 0.015(4) 0.001(4) C40A 0.080(6) 0.059(5) 0.051(5) 0.003(4) -0.003(4) -0.005(4) C41A 0.041(3) 0.033(3) 0.042(4) -0.002(3) 0.017(3) -0.001(3) C42A 0.084(6) 0.059(5) 0.046(5) 0.010(4) 0.026(4) 0.032(4) C43A 0.098(6) 0.048(4) 0.059(5) 0.005(4) 0.046(5) 0.013(5) C44A 0.120(7) 0.105(7) 0.137(8) 0.002(6) 0.084(6) 0.002(6) N1B 0.045(3) 0.031(3) 0.032(3) 0.000(2) 0.013(2) -0.002(2) C37B 0.042(4) 0.037(3) 0.048(4) -0.002(3) 0.019(3) -0.002(3) C38B 0.058(4) 0.041(4) 0.054(5) 0.004(3) 0.027(4) -0.001(3) C39B 0.069(5) 0.057(5) 0.061(5) 0.003(4) 0.034(5) -0.005(4) C40B 0.110(8) 0.080(6) 0.071(6) 0.011(5) 0.061(6) 0.009(6) C41B 0.041(4) 0.035(3) 0.043(4) 0.001(3) 0.012(3) 0.002(3) C42B 0.051(4) 0.052(4) 0.055(5) -0.002(4) 0.022(4) 0.007(4) C43B 0.052(4) 0.056(5) 0.066(6) -0.005(4) 0.020(4) 0.011(4) C44B 0.048(5) 0.066(6) 0.104(8) -0.007(5) 0.009(5) 0.004(4) O9A 0.034(2) 0.036(2) 0.071(4) 0.006(2) 0.014(2) -0.003(2) C45A 0.044(4) 0.044(4) 0.057(5) 0.008(3) 0.016(4) -0.002(3) O9B 0.068(3) 0.042(3) 0.035(3) -0.003(2) 0.011(2) -0.002(2) C45B 0.071(5) 0.052(4) 0.048(5) -0.003(4) 0.021(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O7A 1.776(4) . ? U1 O8A 1.788(4) . ? U1 O3A 2.206(4) . ? U1 O5A 2.220(4) . ? U1 O1A 2.260(4) . ? U1 O2A 2.950(4) . ? O1A C2A 1.358(7) . ? O1A O2A 2.893(6) . ? O1A O6A 2.904(6) . ? O1A O5A 3.889(6) . ? O1A O3A 3.927(5) . ? O2A C11A 1.436(6) . ? O2A C12A 1.437(7) . ? O2A O3A 2.925(6) . ? O3A C14A 1.338(7) . ? O3A O4A 2.983(6) . ? O3A O5A 3.708(6) . ? O4A C23A 1.445(7) . ? O4A C24A 1.452(7) . ? O4A O5A 3.042(6) . ? O5A C26A 1.353(7) . ? O5A O6A 2.934(6) . ? O6A C35A 1.439(7) . ? O6A C36A 1.443(7) . ? C1A C6A 1.389(8) . ? C1A C2A 1.408(8) . ? C1A C36A 1.495(8) . ? C2A C3A 1.385(8) . ? C3A C4A 1.388(8) . ? C3A C11A 1.519(8) . ? C4A C5A 1.380(8) . ? C5A C6A 1.400(9) . ? C5A C7A 1.536(8) . ? C7A C9A 1.512(10) . ? C7A C8A 1.545(9) . ? C7A C10A 1.554(9) . ? C12A C13A 1.511(8) . ? C13A C18A 1.386(8) . ? C13A C14A 1.394(8) . ? C14A C15A 1.412(8) . ? C15A C16A 1.358(8) . ? C15A C23A 1.508(9) . ? C16A C17A 1.401(8) . ? C17A C18A 1.389(8) . ? C17A C19A 1.530(8) . ? C19A C20A 1.527(9) . ? C19A C21A 1.536(9) . ? C19A C22A 1.539(9) . ? C24A C25A 1.492(9) . ? C25A C30A 1.374(8) . ? C25A C26A 1.416(8) . ? C26A C27A 1.390(8) . ? C27A C28A 1.398(9) . ? C27A C35A 1.519(8) . ? C28A C29A 1.391(9) . ? C29A C30A 1.404(9) . ? C29A C31A 1.538(9) . ? C31A C34A 1.523(10) . ? C31A C33A 1.532(9) . ? C31A C32A 1.548(9) . ? U2 O8B 1.780(4) . ? U2 O7B 1.785(4) . ? U2 O5B 2.196(4) . ? U2 O3B 2.214(4) . ? U2 O1B 2.264(4) . ? U2 O2B 2.927(4) . ? O1B C2B 1.348(7) . ? O1B O2B 2.873(6) . ? O1B O6B 2.913(6) . ? O1B O5B 3.830(6) . ? O1B O3B 3.945(6) . ? O2B C11B 1.428(7) . ? O2B C12B 1.448(7) . ? O2B O3B 2.903(6) . ? O3B C14B 1.342(7) . ? O3B O4B 2.954(6) . ? O3B O5B 3.724(5) . ? O4B C24B 1.439(7) . ? O4B C23B 1.450(6) . ? O4B O5B 2.980(6) . ? O5B C26B 1.341(7) . ? O5B O6B 2.919(6) . ? O6B C35B 1.429(7) . ? O6B C36B 1.451(7) . ? C1B C6B 1.398(9) . ? C1B C2B 1.404(9) . ? C1B C36B 1.489(9) . ? C2B C3B 1.394(9) . ? C3B C4B 1.396(9) . ? C3B C11B 1.500(9) . ? C4B C5B 1.372(9) . ? C5B C6B 1.383(9) . ? C5B C7B 1.536(9) . ? C7B C8B 1.509(10) . ? C7B C9B 1.530(11) . ? C7B C10B 1.555(10) . ? C12B C13B 1.491(8) . ? C13B C18B 1.405(8) . ? C13B C14B 1.413(8) . ? C14B C15B 1.391(8) . ? C15B C16B 1.372(8) . ? C15B C23B 1.503(8) . ? C16B C17B 1.411(8) . ? C17B C18B 1.381(8) . ? C17B C19B 1.536(8) . ? C19B C21B 1.524(9) . ? C19B C20B 1.525(9) . ? C19B C22B 1.542(9) . ? C24B C25B 1.510(8) . ? C25B C30B 1.383(8) . ? C25B C26B 1.397(9) . ? C26B C27B 1.411(8) . ? C27B C28B 1.417(9) . ? C27B C35B 1.482(9) . ? C28B C29B 1.394(9) . ? C29B C30B 1.398(9) . ? C29B C31B 1.521(9) . ? C31B C33B 1.472(10) . ? C31B C32B 1.502(10) . ? C31B C34B 1.548(11) . ? N1A C37A 1.486(8) . ? N1A C41A 1.502(7) . ? C37A C38A 1.504(9) . ? C38A C39A 1.526(10) . ? C39A C40A 1.525(10) . ? C41A C42A 1.503(9) . ? C42A C43A 1.522(10) . ? C43A C44A 1.392(12) . ? N1B C41B 1.491(7) . ? N1B C37B 1.494(7) . ? C37B C38B 1.522(9) . ? C38B C39B 1.531(9) . ? C39B C40B 1.532(11) . ? C41B C42B 1.515(9) . ? C42B C43B 1.508(10) . ? C43B C44B 1.511(11) . ? O9A C45A 1.420(7) . ? O9B C45B 1.417(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 O7A U1 O8A 179.65(19) . . ? O7A U1 O3A 85.52(17) . . ? O8A U1 O3A 94.17(16) . . ? O7A U1 O5A 86.40(17) . . ? O8A U1 O5A 93.88(16) . . ? O3A U1 O5A 113.81(15) . . ? O7A U1 O1A 82.07(16) . . ? O8A U1 O1A 97.96(15) . . ? O3A U1 O1A 123.10(15) . . ? O5A U1 O1A 120.44(15) . . ? O7A U1 O2A 110.44(16) . . ? O8A U1 O2A 69.28(15) . . ? O3A U1 O2A 67.33(13) . . ? O5A U1 O2A 163.06(13) . . ? O1A U1 O2A 65.91(13) . . ? C11A O2A C12A 113.9(4) . . ? C23A O4A C24A 114.0(4) . . ? C35A O6A C36A 112.9(5) . . ? C6A C1A C2A 117.7(6) . . ? C6A C1A C36A 122.7(6) . . ? C2A C1A C36A 119.6(5) . . ? O1A C2A C3A 120.1(5) . . ? O1A C2A C1A 119.0(5) . . ? C3A C2A C1A 120.8(5) . . ? C2A C3A C4A 118.8(6) . . ? C2A C3A C11A 118.5(5) . . ? C4A C3A C11A 122.7(6) . . ? C5A C4A C3A 122.0(6) . . ? C4A C5A C6A 117.7(6) . . ? C4A C5A C7A 123.3(6) . . ? C6A C5A C7A 119.0(5) . . ? C1A C6A C5A 122.1(6) . . ? C9A C7A C5A 112.7(6) . . ? C9A C7A C8A 107.0(6) . . ? C5A C7A C8A 109.1(5) . . ? C9A C7A C10A 108.7(6) . . ? C5A C7A C10A 110.4(5) . . ? C8A C7A C10A 108.8(6) . . ? O2A C11A C3A 108.9(5) . . ? O2A C12A C13A 109.0(5) . . ? C18A C13A C14A 119.0(5) . . ? C18A C13A C12A 122.2(6) . . ? C14A C13A C12A 118.7(5) . . ? O3A C14A C13A 120.3(5) . . ? O3A C14A C15A 120.4(5) . . ? C13A C14A C15A 119.3(5) . . ? C16A C15A C14A 119.3(6) . . ? C16A C15A C23A 122.9(6) . . ? C14A C15A C23A 117.7(5) . . ? C15A C16A C17A 123.3(6) . . ? C18A C17A C16A 116.0(6) . . ? C18A C17A C19A 124.0(6) . . ? C16A C17A C19A 120.0(5) . . ? C13A C18A C17A 123.0(6) . . ? C20A C19A C17A 112.1(5) . . ? C20A C19A C21A 106.8(6) . . ? C17A C19A C21A 109.4(5) . . ? C20A C19A C22A 108.1(6) . . ? C17A C19A C22A 110.3(5) . . ? C21A C19A C22A 110.0(5) . . ? O4A C23A C15A 107.5(5) . . ? O4A C24A C25A 106.8(5) . . ? C30A C25A C26A 118.8(6) . . ? C30A C25A C24A 122.1(6) . . ? C26A C25A C24A 118.9(6) . . ? O5A C26A C27A 119.9(5) . . ? O5A C26A C25A 119.9(6) . . ? C27A C26A C25A 120.1(6) . . ? C26A C27A C28A 118.6(6) . . ? C26A C27A C35A 119.1(6) . . ? C28A C27A C35A 122.2(6) . . ? C29A C28A C27A 123.0(6) . . ? C28A C29A C30A 116.3(6) . . ? C28A C29A C31A 119.9(6) . . ? C30A C29A C31A 123.7(6) . . ? C25A C30A C29A 123.0(6) . . ? C34A C31A C33A 110.3(6) . . ? C34A C31A C29A 110.4(6) . . ? C33A C31A C29A 109.1(5) . . ? C34A C31A C32A 107.8(6) . . ? C33A C31A C32A 108.0(6) . . ? C29A C31A C32A 111.4(5) . . ? O6A C35A C27A 108.0(5) . . ? O6A C36A C1A 107.3(5) . . ? O8B U2 O7B 179.54(18) . . ? O8B U2 O5B 94.51(16) . . ? O7B U2 O5B 85.51(17) . . ? O8B U2 O3B 94.46(16) . . ? O7B U2 O3B 85.94(16) . . ? O5B U2 O3B 115.25(16) . . ? O8B U2 O1B 97.78(16) . . ? O7B U2 O1B 81.80(16) . . ? O5B U2 O1B 118.37(15) . . ? O3B U2 O1B 123.52(15) . . ? O8B U2 O2B 70.67(15) . . ? O7B U2 O2B 109.31(16) . . ? O5B U2 O2B 165.18(13) . . ? O3B U2 O2B 67.12(13) . . ? O1B U2 O2B 65.78(13) . . ? C11B O2B C12B 113.2(4) . . ? C24B O4B C23B 113.6(4) . . ? C35B O6B C36B 114.1(5) . . ? C6B C1B C2B 117.0(6) . . ? C6B C1B C36B 124.6(6) . . ? C2B C1B C36B 118.4(6) . . ? O1B C2B C3B 119.6(6) . . ? O1B C2B C1B 119.3(6) . . ? C3B C2B C1B 121.0(6) . . ? C2B C3B C4B 118.1(6) . . ? C2B C3B C11B 119.0(6) . . ? C4B C3B C11B 122.9(6) . . ? C5B C4B C3B 122.7(6) . . ? C4B C5B C6B 117.2(6) . . ? C4B C5B C7B 119.0(7) . . ? C6B C5B C7B 123.8(7) . . ? C5B C6B C1B 123.2(6) . . ? C8B C7B C9B 108.7(7) . . ? C8B C7B C5B 111.2(6) . . ? C9B C7B C5B 111.7(7) . . ? C8B C7B C10B 110.2(7) . . ? C9B C7B C10B 107.0(7) . . ? C5B C7B C10B 108.0(6) . . ? O2B C11B C3B 108.8(5) . . ? O2B C12B C13B 107.5(5) . . ? C18B C13B C14B 117.9(5) . . ? C18B C13B C12B 122.5(5) . . ? C14B C13B C12B 119.6(5) . . ? O3B C14B C15B 121.1(5) . . ? O3B C14B C13B 118.4(5) . . ? C15B C14B C13B 120.5(5) . . ? C16B C15B C14B 119.0(5) . . ? C16B C15B C23B 122.9(6) . . ? C14B C15B C23B 118.0(5) . . ? C15B C16B C17B 122.9(6) . . ? C18B C17B C16B 116.7(5) . . ? C18B C17B C19B 122.4(6) . . ? C16B C17B C19B 120.8(6) . . ? C17B C18B C13B 122.7(6) . . ? C21B C19B C20B 107.1(6) . . ? C21B C19B C17B 109.5(5) . . ? C20B C19B C17B 111.9(6) . . ? C21B C19B C22B 111.4(6) . . ? C20B C19B C22B 106.8(6) . . ? C17B C19B C22B 110.0(5) . . ? O4B C23B C15B 107.6(5) . . ? O4B C24B C25B 107.1(5) . . ? C30B C25B C26B 120.0(6) . . ? C30B C25B C24B 122.5(6) . . ? C26B C25B C24B 117.3(5) . . ? O5B C26B C25B 121.5(6) . . ? O5B C26B C27B 118.7(6) . . ? C25B C26B C27B 119.8(6) . . ? C26B C27B C28B 117.9(6) . . ? C26B C27B C35B 119.7(6) . . ? C28B C27B C35B 122.4(6) . . ? C29B C28B C27B 122.7(6) . . ? C28B C29B C30B 116.9(6) . . ? C28B C29B C31B 122.0(6) . . ? C30B C29B C31B 121.1(6) . . ? C25B C30B C29B 122.4(6) . . ? C33B C31B C32B 109.5(6) . . ? C33B C31B C29B 110.0(6) . . ? C32B C31B C29B 112.3(6) . . ? C33B C31B C34B 109.5(7) . . ? C32B C31B C34B 104.5(7) . . ? C29B C31B C34B 110.9(6) . . ? O6B C35B C27B 109.6(5) . . ? O6B C36B C1B 109.1(5) . . ? C37A N1A C41A 116.2(5) . . ? N1A C37A C38A 112.5(5) . . ? C37A C38A C39A 111.8(6) . . ? C40A C39A C38A 111.8(6) . . ? N1A C41A C42A 110.6(5) . . ? C41A C42A C43A 113.1(6) . . ? C44A C43A C42A 112.5(8) . . ? C41B N1B C37B 115.8(5) . . ? N1B C37B C38B 112.6(5) . . ? C37B C38B C39B 111.5(6) . . ? C38B C39B C40B 110.6(7) . . ? N1B C41B C42B 109.6(5) . . ? C43B C42B C41B 114.3(7) . . ? C42B C43B C44B 112.3(6) . . ? 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 H2A O1A 0.75 2.07 2.801(6) 166.1 2_545 N1A H1A O9A 0.76 2.09 2.713(6) 138.7 . N1B H2B O1B 0.95 1.90 2.827(6) 163.8 2_656 N1B H1B O9B 0.76 1.98 2.732(7) 171.2 . O9A H9A O4A 0.89 1.92 2.799(6) 167.1 . O9B H9B O4B 0.92 1.84 2.754(6) 170.0 . #===END data_7 _database_code_CSD 172887 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H69 N O11 U' _chemical_formula_weight 1026.03 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 orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 19.3226(7) _cell_length_b 16.4355(7) _cell_length_c 14.1831(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4504.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 29971 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent intense orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method ? _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 3.661 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.476 _exptl_absorpt_correction_T_max 0.746 _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 29971 _diffrn_reflns_av_R_equivalents 0.0975 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4428 _reflns_number_gt 3042 _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. One tert-butyl group was found disordered over two positions, which were refined with occupancies constrained to sum to unity. The water molecule (O8) was affected with a 0.5 occupancy factor so as to keep a physically meaningful displacement parameter and to take into account the impossibility of the simultaneous occupation of its symmetry-related position located at a distance of 1.10 A. All non-hydrogen atoms were refined with anisotropic displacement parameters. Some constraints have been applied to the badly resolved ammonium ion. The hydrogen atoms bound to O and N atoms have not been found on the Fourier-difference map, nor introduced. All other hydrogen atoms (except those in the disordered parts) were introduced 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^)+(0.0523P)^2^+18.6722P] 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 4428 _refine_ls_number_parameters 310 _refine_ls_number_restraints 82 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1292 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.247 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.138 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 U U 0.700778(18) 0.2500 0.24600(3) 0.02732(14) Uani 1 2 d S . . O1 O 0.6378(4) 0.2500 0.1134(5) 0.043(2) Uani 1 2 d S . . O2 O 0.7184(3) 0.1077(3) 0.1379(3) 0.0431(15) Uani 1 1 d . . . O3 O 0.7264(3) 0.1439(3) 0.3383(3) 0.0327(12) Uani 1 1 d . . . O4 O 0.8542(4) 0.2500 0.4040(5) 0.0338(17) Uani 1 2 d S . . O5 O 0.6178(4) 0.2500 0.2998(5) 0.0365(18) Uani 1 2 d S . . O6 O 0.7867(3) 0.2500 0.1987(5) 0.0277(16) Uani 1 2 d S . . C1 C 0.6748(5) 0.2500 0.0335(7) 0.034(3) Uani 1 2 d S . . C2 C 0.6961(4) 0.1761(5) -0.0071(5) 0.0311(16) Uani 1 1 d . . . C3 C 0.7327(4) 0.1775(4) -0.0904(5) 0.0300(16) Uani 1 1 d . . . H3A H 0.7461 0.1284 -0.1175 0.036 Uiso 1 1 calc R . . C4 C 0.7504(5) 0.2500 -0.1357(6) 0.024(2) Uani 1 2 d S . . C5 C 0.7869(5) 0.2500 -0.2334(7) 0.032(2) Uani 1 2 d S . . C6 C 0.8309(7) 0.1758(7) -0.2469(8) 0.082(3) Uani 1 1 d U . . H6A H 0.8524 0.1778 -0.3078 0.123 Uiso 1 1 calc R . . H6B H 0.8026 0.1280 -0.2424 0.123 Uiso 1 1 calc R . . H6C H 0.8660 0.1742 -0.1990 0.123 Uiso 1 1 calc R . . C7 C 0.7310(9) 0.2500 -0.3076(11) 0.080(5) Uani 1 2 d SU . . H7A H 0.7501 0.2500 -0.3703 0.120 Uiso 1 2 d S . . H7B H 0.7014 0.2023 -0.3012 0.120 Uiso 0.50 1 d P . . C9 C 0.6827(5) 0.1001(5) 0.0481(5) 0.045(2) Uani 1 1 d . . . H9A H 0.6334 0.0933 0.0584 0.054 Uiso 1 1 calc R . . H9B H 0.6997 0.0531 0.0139 0.054 Uiso 1 1 calc R . . C10 C 0.7253(4) 0.0319(5) 0.1880(5) 0.0354(18) Uani 1 1 d . . . H10A H 0.7334 -0.0122 0.1438 0.042 Uiso 1 1 calc R . . H10B H 0.6830 0.0202 0.2223 0.042 Uiso 1 1 calc R . . C11 C 0.7855(4) 0.0386(5) 0.2559(5) 0.0330(16) Uani 1 1 d . . . C12 C 0.7830(4) 0.0966(5) 0.3276(5) 0.0319(17) Uani 1 1 d . . . C13 C 0.8400(4) 0.1071(5) 0.3862(5) 0.0311(17) Uani 1 1 d . . . C14 C 0.8968(4) 0.0561(5) 0.3761(5) 0.0319(16) Uani 1 1 d . . . H14A H 0.9340 0.0625 0.4171 0.038 Uiso 1 1 calc R . . C15 C 0.9006(4) -0.0049(5) 0.3067(5) 0.0374(18) Uani 1 1 d . . . C16 C 0.8438(4) -0.0103(5) 0.2462(5) 0.0360(16) Uani 1 1 d . . . H16A H 0.8449 -0.0482 0.1976 0.043 Uiso 1 1 calc R . . C17 C 0.9650(4) -0.0593(6) 0.2954(7) 0.044(2) Uani 1 1 d . . . C18A C 0.9702(11) -0.1145(15) 0.3928(15) 0.063(6) Uani 0.490(16) 1 d PU . . C18B C 1.0210(13) -0.0496(17) 0.3806(18) 0.085(8) Uani 0.510(16) 1 d PU . . C19A C 1.0289(10) -0.0070(13) 0.2941(19) 0.062(6) Uani 0.490(16) 1 d PU . . C19B C 1.0056(11) -0.0318(14) 0.2073(16) 0.069(7) Uani 0.510(16) 1 d PU . . C20A C 0.9598(12) -0.1152(17) 0.2087(18) 0.070(7) Uani 0.490(16) 1 d PU . . C20B C 0.9445(11) -0.1457(14) 0.2831(19) 0.070(7) Uani 0.510(16) 1 d PU . . C21 C 0.8402(4) 0.1765(5) 0.4564(5) 0.0353(18) Uani 1 1 d . . . H21A H 0.7957 0.1803 0.4877 0.042 Uiso 1 1 calc R . . H21B H 0.8756 0.1679 0.5038 0.042 Uiso 1 1 calc R . . N N 0.9309(6) 0.2500 0.2051(9) 0.090(6) Uani 1 2 d S . . C22 C 0.9425(7) 0.1733(10) 0.1431(11) 0.108(4) Uani 1 1 d DU . . H22A H 0.9920 0.1637 0.1400 0.129 Uiso 1 1 calc R . . H22B H 0.9223 0.1273 0.1761 0.129 Uiso 1 1 calc R . . C23 C 0.916(3) 0.172(2) 0.0450(17) 0.108(4) Uani 1 1 d DU . . H23A H 0.8654 0.1742 0.0431 0.129 Uiso 1 1 calc R . . H23B H 0.9319 0.1255 0.0097 0.129 Uiso 1 1 calc R . . C24 C 0.9475(18) 0.2500 0.011(3) 0.108(4) Uani 1 2 d SDU . . H24A H 0.9298 0.2500 -0.0533 0.129 Uiso 1 2 calc SR . . C25 C 1.0244(18) 0.2500 -0.010(3) 0.102(12) Uani 1 2 d SDU . . H25A H 1.0417 0.2977 -0.0467 0.153 Uiso 1 1 d . . . H25B H 1.0519 0.2500 0.0480 0.153 Uiso 1 2 d S . . O7 O 0.6742(5) 0.0846(6) 0.5096(5) 0.094(3) Uani 1 1 d . . . C26 C 0.6403(8) 0.0135(9) 0.4769(9) 0.109(5) Uani 1 1 d . . . H26A H 0.6537 0.0030 0.4129 0.164 Uiso 1 1 calc R . . H26B H 0.5911 0.0213 0.4800 0.164 Uiso 1 1 calc R . . H26C H 0.6532 -0.0319 0.5157 0.164 Uiso 1 1 calc R . . O8 O 0.5047(6) 0.2166(8) 0.1257(9) 0.060(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.0256(2) 0.0319(2) 0.0245(2) 0.000 0.00242(19) 0.000 O1 0.030(4) 0.072(6) 0.027(4) 0.000 0.004(3) 0.000 O2 0.065(4) 0.035(3) 0.030(3) 0.009(2) -0.015(3) -0.023(3) O3 0.029(3) 0.037(3) 0.033(3) 0.011(2) 0.004(2) 0.001(2) O4 0.045(4) 0.030(4) 0.027(3) 0.000 0.004(3) 0.000 O5 0.033(4) 0.051(5) 0.025(4) 0.000 -0.003(3) 0.000 O6 0.031(4) 0.025(4) 0.026(3) 0.000 0.002(3) 0.000 C1 0.025(5) 0.050(7) 0.027(5) 0.000 -0.002(4) 0.000 C2 0.035(4) 0.030(4) 0.028(3) 0.003(3) -0.003(3) -0.006(4) C3 0.039(4) 0.023(4) 0.029(4) -0.004(3) -0.003(3) -0.002(3) C4 0.024(5) 0.024(5) 0.025(5) 0.000 -0.003(4) 0.000 C5 0.034(5) 0.025(5) 0.036(6) 0.000 0.010(5) 0.000 C6 0.100(7) 0.064(6) 0.083(6) 0.012(5) 0.051(6) 0.029(5) C7 0.071(8) 0.117(10) 0.052(7) 0.000 0.004(6) 0.000 C9 0.062(6) 0.043(5) 0.030(4) 0.012(4) -0.011(4) -0.025(5) C10 0.044(4) 0.030(4) 0.032(4) 0.008(3) -0.004(3) -0.011(4) C11 0.037(4) 0.035(4) 0.028(3) 0.004(4) 0.004(3) -0.008(3) C12 0.036(4) 0.030(4) 0.030(4) 0.005(3) 0.010(3) 0.001(3) C13 0.034(4) 0.031(4) 0.028(3) 0.004(3) 0.005(3) -0.005(3) C14 0.032(4) 0.034(4) 0.030(4) -0.001(3) -0.002(3) -0.001(4) C15 0.039(4) 0.039(5) 0.034(4) -0.003(3) 0.008(4) -0.001(4) C16 0.045(4) 0.035(4) 0.029(3) -0.004(4) 0.006(4) -0.008(3) C17 0.040(5) 0.036(5) 0.056(5) -0.014(4) 0.005(4) 0.004(4) C18A 0.057(9) 0.065(10) 0.067(9) 0.003(8) 0.008(7) 0.027(8) C18B 0.080(11) 0.094(11) 0.082(10) -0.020(8) -0.017(8) 0.020(9) C19A 0.038(8) 0.049(9) 0.099(11) -0.009(8) 0.015(8) 0.001(7) C19B 0.064(9) 0.070(10) 0.072(9) 0.016(8) 0.022(8) 0.016(8) C20A 0.068(10) 0.075(11) 0.067(10) -0.024(8) -0.002(8) 0.014(8) C20B 0.063(9) 0.053(9) 0.093(11) -0.006(8) 0.007(8) 0.012(7) C21 0.049(5) 0.035(4) 0.021(3) 0.004(3) 0.001(3) 0.008(4) N 0.031(6) 0.195(19) 0.044(7) 0.000 0.005(5) 0.000 C22 0.102(6) 0.102(6) 0.119(6) 0.0014(15) 0.014(4) 0.0000(14) C23 0.102(6) 0.102(6) 0.118(6) 0.0006(10) 0.013(4) 0.0000(10) C24 0.102(6) 0.103(6) 0.118(6) 0.000 0.013(4) 0.000 C25 0.105(15) 0.114(15) 0.087(14) 0.000 -0.018(10) 0.000 O7 0.119(7) 0.096(7) 0.066(5) 0.004(5) 0.014(5) -0.028(6) C26 0.144(14) 0.094(11) 0.089(9) 0.005(8) -0.001(9) -0.044(11) O8 0.041(7) 0.075(11) 0.065(7) -0.005(6) -0.001(6) -0.006(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 U O5 1.776(7) . ? U O6 1.790(7) . ? U O3 2.236(5) 7_565 ? U O3 2.236(5) . ? U O1 2.240(7) . ? U O2 2.818(6) . ? U O2 2.818(6) 7_565 ? U C1 3.056(10) . ? U O4 3.716(7) . ? O1 C1 1.340(12) . ? O1 O8 2.637(13) . ? O1 O2 2.832(8) . ? O1 O3 4.019(8) . ? O2 C10 1.440(9) . ? O2 C9 1.453(9) . ? O2 O3 2.909(7) . ? O3 C12 1.350(9) . ? O3 O7 2.806(9) . ? O3 O4 3.162(8) . ? O3 O3 3.486(11) 7_565 ? O4 C21 1.443(8) . ? O4 C21 1.443(8) 7_565 ? O6 N 2.788(13) . ? C1 C2 1.404(9) . ? C1 C2 1.404(9) 7_565 ? C2 C3 1.378(10) . ? C2 C9 1.497(10) . ? C3 C4 1.396(9) . ? C4 C3 1.396(8) 7_565 ? C4 C5 1.554(13) . ? C5 C6 1.499(12) . ? C5 C6 1.499(12) 7_565 ? C5 C7 1.508(19) . ? C10 C11 1.514(10) . ? C11 C16 1.391(11) . ? C11 C12 1.396(10) . ? C12 C13 1.389(10) . ? C13 C14 1.388(10) . ? C13 C21 1.515(10) . ? C14 C15 1.408(10) . ? C15 C16 1.396(11) . ? C15 C17 1.541(11) . ? C17 C20B 1.49(2) . ? C17 C19A 1.50(2) . ? C17 C20A 1.54(2) . ? C17 C19B 1.54(2) . ? C17 C18B 1.63(2) . ? C17 C18A 1.66(2) . ? C18A C18B 1.46(3) . ? C18A C20B 1.71(3) . ? C18B C19A 1.42(3) . ? C19A C19B 1.37(3) . ? C19B C20A 1.63(3) . ? C20A C20B 1.21(3) . ? N C22 1.554(16) . ? N C22 1.554(16) 7_565 ? N O8 2.845(17) 4 ? N O8 2.845(17) 6_656 ? C22 C23 1.48(3) . ? C23 C24 1.50(4) . ? C24 C23 1.50(4) 7_565 ? C24 C25 1.52(5) . ? O7 C26 1.417(15) . ? O8 O8 1.10(3) 7_565 ? O8 O4 2.989(13) 6_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 U O6 176.6(3) . . ? O5 U O3 87.04(18) . 7_565 ? O6 U O3 90.81(18) . 7_565 ? O5 U O3 87.04(18) . . ? O6 U O3 90.81(18) . . ? O3 U O3 102.4(3) 7_565 . ? O5 U O1 82.6(3) . . ? O6 U O1 100.9(3) . . ? O3 U O1 127.76(14) 7_565 . ? O3 U O1 127.76(14) . . ? O5 U O2 110.08(16) . . ? O6 U O2 71.55(16) . . ? O3 U O2 159.90(18) 7_565 . ? O3 U O2 69.19(18) . . ? O1 U O2 66.97(13) . . ? O5 U O2 110.08(16) . 7_565 ? O6 U O2 71.55(16) . 7_565 ? O3 U O2 69.19(18) 7_565 7_565 ? O3 U O2 159.90(18) . 7_565 ? O1 U O2 66.97(13) . 7_565 ? O2 U O2 112.2(2) . 7_565 ? O5 U C1 106.0(3) . . ? O6 U C1 77.4(3) . . ? O3 U C1 127.89(14) 7_565 . ? O3 U C1 127.89(14) . . ? O1 U C1 23.5(3) . . ? O2 U C1 58.87(11) . . ? O2 U C1 58.87(11) 7_565 . ? O5 U O4 117.4(2) . . ? O6 U O4 59.1(2) . . ? O3 U O4 57.98(14) 7_565 . ? O3 U O4 57.98(14) . . ? O1 U O4 160.0(2) . . ? O2 U O4 103.40(13) . . ? O2 U O4 103.40(13) 7_565 . ? C1 U O4 136.5(2) . . ? C10 O2 C9 113.7(6) . . ? C21 O4 C21 113.6(7) . 7_565 ? O1 C1 C2 120.1(5) . . ? O1 C1 C2 120.1(5) . 7_565 ? C2 C1 C2 119.7(9) . 7_565 ? O1 C1 U 41.7(5) . . ? C2 C1 U 110.8(5) . . ? C2 C1 U 110.8(5) 7_565 . ? C3 C2 C1 119.1(7) . . ? C3 C2 C9 123.4(7) . . ? C1 C2 C9 117.2(7) . . ? C2 C3 C4 122.3(7) . . ? C3 C4 C3 117.2(9) 7_565 . ? C3 C4 C5 121.4(4) 7_565 . ? C3 C4 C5 121.4(4) . . ? C6 C5 C6 108.9(12) . 7_565 ? C6 C5 C7 108.5(8) . . ? C6 C5 C7 108.5(8) 7_565 . ? C6 C5 C4 111.8(6) . . ? C6 C5 C4 111.8(6) 7_565 . ? C7 C5 C4 107.4(9) . . ? O2 C9 C2 107.7(6) . . ? O2 C10 C11 108.7(6) . . ? C16 C11 C12 119.7(7) . . ? C16 C11 C10 121.1(7) . . ? C12 C11 C10 119.2(7) . . ? O3 C12 C13 120.2(7) . . ? O3 C12 C11 120.2(7) . . ? C13 C12 C11 119.5(7) . . ? C12 C13 C14 119.4(7) . . ? C12 C13 C21 119.2(7) . . ? C14 C13 C21 121.4(7) . . ? C13 C14 C15 122.9(7) . . ? C16 C15 C14 115.7(7) . . ? C16 C15 C17 122.4(7) . . ? C14 C15 C17 121.9(7) . . ? C11 C16 C15 122.7(7) . . ? C19A C17 C20A 112.7(14) . . ? C20B C17 C15 110.5(10) . . ? C19A C17 C15 109.4(10) . . ? C20A C17 C15 112.1(10) . . ? C20B C17 C19B 108.7(15) . . ? C15 C17 C19B 109.0(10) . . ? C20B C17 C18B 111.0(15) . . ? C15 C17 C18B 113.7(11) . . ? C19B C17 C18B 103.6(14) . . ? C19A C17 C18A 105.9(14) . . ? C20A C17 C18A 110.2(15) . . ? C15 C17 C18A 106.2(9) . . ? O4 C21 C13 107.0(5) . . ? C22 N C22 108.5(14) . 7_565 ? C22 N O6 97.3(7) . . ? C22 N O6 97.3(7) 7_565 . ? C22 N O8 124.1(8) . 4 ? C22 N O8 104.4(8) 7_565 4 ? O6 N O8 121.9(5) . 4 ? C22 N O8 104.4(8) . 6_656 ? C22 N O8 124.1(8) 7_565 6_656 ? O6 N O8 121.9(5) . 6_656 ? C23 C22 N 119(2) . . ? C22 C23 C24 98(2) . . ? C23 C24 C23 117(5) . 7_565 ? C23 C24 C25 118(3) . . ? C23 C24 C25 118(3) 7_565 . ? C26 O7 O3 99.7(7) . . ? O8 O8 O1 78.0(3) 7_565 . ? O8 O8 O4 79.4(2) 7_565 6_556 ? O1 O8 O4 154.4(5) . 6_556 ?