#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/07/7050757.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_7050757
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            'C46 H71 N O9 U'
_chemical_formula_weight         1020.07
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 106.837(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0317(7)
_cell_length_b                   21.9727(14)
_cell_length_c                   16.3246(7)
_cell_measurement_reflns_used    16508
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.77
_cell_volume                     4817.4(4)
_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 0.913
_diffrn_measured_fraction_theta_max 0.913
_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  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16508
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.420
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_correction_T_min  0.355
_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    1.406
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.232
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         8591
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0566
_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)+(0.0697P)²+13.5004P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1541
_reflns_number_gt                5895
_reflns_number_total             8591
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108947c.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      P2~1~/m
_cod_database_code               7050757
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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_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
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_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_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 .
