#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/07/7050759.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7050759
loop_
_publ_author_name
'Masci, Bernardo'
'Nierlich, Martine'
'Thuéry, Pierre'
_publ_section_title
;
 Trigonal versus tetragonal or pentagonal coordination of the uranyl
 ion by hexahomotrioxacalix[3]arenes: solid state and solution
 investigations
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              120
_journal_paper_doi               10.1039/b108947c
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C45 H69 N O9 U'
_chemical_formula_weight         1006.04
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.739(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.2169(6)
_cell_length_b                   16.5010(5)
_cell_length_c                   24.4065(7)
_cell_measurement_reflns_used    63517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.62
_cell_volume                     9366.3(5)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            63517
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.517
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent intense orange'
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.817
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.00022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1034
_refine_ls_number_reflns         17694
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0253P)²+8.1354P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                12894
_reflns_number_total             17694
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108947c.txt
_cod_data_source_block           6
_cod_original_cell_volume        9366.3(4)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7050759
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'
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_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'
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_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_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 .
