#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:26:43 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180339 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/08/7200845.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_7200845
loop_
_publ_author_name
'Thuéry, Pierre'
_publ_section_title
;
 Uranyl ion complexes of cucurbit[7]uril with zero-, one- and
 two-dimensionality
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1150
_journal_paper_doi               10.1039/b822872h
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C42 H80 N32 O55 U4'
_chemical_formula_weight         2865.50
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 127.974(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.9954(8)
_cell_length_b                   17.6794(7)
_cell_length_c                   20.5253(6)
_cell_measurement_reflns_used    121095
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.05
_cell_volume                     8580.2(5)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and four ω scans with 2° steps (400 frames)'
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            121095
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.652
_exptl_absorpt_correction_T_max  0.465
_exptl_absorpt_correction_T_min  0.339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5456
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.042
_refine_diff_density_min         -2.469
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         8106
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0522P)²+68.8977P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                6653
_reflns_number_total             8106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b822872h.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7200845
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.336568(10) 0.438880(14) 0.793810(15) 0.02500(9) Uani 1 1 d . . .
U2 U 0.222102(10) 0.445509(14) 0.824652(15) 0.02575(9) Uani 1 1 d . . .
O1 O 0.3877(2) 0.4328(3) 0.9008(3) 0.0453(14) Uani 1 1 d . . .
O2 O 0.2859(2) 0.4449(4) 0.6848(3) 0.0469(16) Uani 1 1 d . . .
O3 O 0.2743(2) 0.4513(3) 0.9337(3) 0.0330(11) Uani 1 1 d . . .
O4 O 0.1676(2) 0.4434(3) 0.7165(3) 0.0373(13) Uani 1 1 d . . .
O5 O 0.27782(17) 0.5145(3) 0.8030(3) 0.0249(10) Uani 1 1 d . . .
H5 H 0.2553 0.5536 0.7678 0.030 Uiso 1 1 d R . .
O6 O 0.2768(2) 0.3677(3) 0.8067(3) 0.0409(13) Uani 1 1 d . . .
H6 H 0.2805 0.3131 0.8136 0.049 Uiso 1 1 d R . .
O7 O 0.3480(3) 0.3128(3) 0.7589(5) 0.075(2) Uani 1 1 d . . .
H7A H 0.3813 0.2894 0.7869 0.090 Uiso 1 1 d R . .
H7B H 0.3202 0.2806 0.7128 0.090 Uiso 1 1 d R . .
O8 O 0.3612(2) 0.5712(3) 0.7942(4) 0.0454(14) Uani 1 1 d . . .
H8A H 0.3871 0.5904 0.8024 0.055 Uiso 1 1 d R . .
H8B H 0.3336 0.5844 0.7413 0.055 Uiso 1 1 d R . .
O9 O 0.1995(2) 0.3175(3) 0.8401(4) 0.0438(13) Uani 1 1 d . . .
H9A H 0.2316 0.3066 0.8947 0.053 Uiso 1 1 d R . .
H9B H 0.2030 0.2849 0.8126 0.053 Uiso 1 1 d R . .
O10 O 0.20088(19) 0.5778(3) 0.8278(3) 0.0294(10) Uani 1 1 d . . .
H10A H 0.1596 0.5899 0.7797 0.035 Uiso 1 1 d R . .
H10B H 0.2085 0.5877 0.8774 0.035 Uiso 1 1 d R . .
O11 O 0.1469(3) 0.2058(5) 0.9587(4) 0.072(2) Uani 1 1 d . . .
O12 O 0.1642(3) 0.1647(4) 0.8759(5) 0.0703(19) Uani 1 1 d . . .
O13 O 0.0773(3) 0.1841(3) 0.8280(4) 0.0595(17) Uani 1 1 d . . .
O14 O 0.1889(2) 0.2790(3) 1.1186(4) 0.0566(17) Uani 1 1 d . . .
O15 O 0.2758(2) 0.3125(3) 1.2134(3) 0.0474(14) Uani 1 1 d . . .
O16 O 0.2072(2) 0.3925(3) 1.1667(3) 0.0397(12) Uani 1 1 d . . .
O17 O 0.41262(19) 0.4369(3) 0.7832(3) 0.0283(10) Uani 1 1 d . . .
O18 O 0.67276(19) 0.3267(3) 0.9017(3) 0.0314(10) Uani 1 1 d . . .
O19 O 0.51207(18) 0.3454(3) 0.9819(3) 0.0293(10) Uani 1 1 d . . .
O20 O 0.70834(19) 0.1296(3) 0.9598(3) 0.0303(11) Uani 1 1 d . . .
O21 O 0.52891(19) 0.1376(3) 1.0111(3) 0.0344(11) Uani 1 1 d . . .
O22 O 0.64694(18) -0.0491(3) 0.8357(3) 0.0267(10) Uani 1 1 d . . .
O23 O 0.46308(18) -0.0247(3) 0.8674(3) 0.0290(10) Uani 1 1 d . . .
O24 O 0.4454(5) 0.2405(8) 0.8552(7) 0.061(4) Uani 0.50 1 d P . .
H24A H 0.4362 0.2001 0.8269 0.073 Uiso 0.50 1 d PR . .
H24B H 0.4625 0.2762 0.8454 0.073 Uiso 0.50 1 d PR . .
O25 O 0.4491(2) 0.6318(3) 0.8188(4) 0.0562(16) Uani 1 1 d . . .
O26 O 0.0940(3) 0.6062(4) 0.7066(5) 0.091(3) Uani 1 1 d U . .
H26A H 0.0758 0.5515 0.6887 0.110 Uiso 1 1 d R . .
H26B H 0.1006 0.6086 0.6692 0.110 Uiso 1 1 d R . .
O27 O 0.2197(2) 0.3253(3) 0.9866(4) 0.0557(16) Uani 1 1 d . . .
H27A H 0.2071 0.2890 0.9962 0.067 Uiso 1 1 d R . .
H27B H 0.2491 0.3500 1.0388 0.067 Uiso 1 1 d R . .
O28 O 0.5438(4) 0.7009(6) 0.9498(6) 0.041(3) Uani 0.50 1 d PU . .
H28A H 0.5144 0.6772 0.9133 0.049 Uiso 0.50 1 d PR . .
H28B H 0.5754 0.6653 0.9713 0.049 Uiso 0.50 1 d PR . .
O29 O 0.0567(6) 0.5976(10) 0.8183(10) 0.088(5) Uani 0.50 1 d PU . .
H29A H 0.0502 0.5654 0.7785 0.105 Uiso 0.50 1 d PR . .
H29B H 0.0754 0.5608 0.8688 0.105 Uiso 0.50 1 d PR . .
N1 N 0.1294(3) 0.1868(4) 0.8879(5) 0.0532(19) Uani 1 1 d . . .
N2 N 0.2232(2) 0.3275(3) 1.1662(4) 0.0352(14) Uani 1 1 d . . .
N3 N 0.5004(2) 0.4778(3) 0.8301(3) 0.0230(11) Uani 1 1 d . . .
N4 N 0.5698(2) 0.4846(3) 0.8037(3) 0.0254(12) Uani 1 1 d . . .
N5 N 0.5663(2) 0.4226(3) 0.9658(3) 0.0258(12) Uani 1 1 d . . .
N6 N 0.6054(2) 0.3196(3) 1.0427(3) 0.0233(11) Uani 1 1 d . . .
N7 N 0.6734(2) 0.3157(3) 1.0141(3) 0.0236(11) Uani 1 1 d . . .
N8 N 0.6320(2) 0.4156(3) 0.9332(3) 0.0241(11) Uani 1 1 d . . .
N9 N 0.6181(2) 0.1845(3) 1.0660(3) 0.0257(12) Uani 1 1 d . . .
N10 N 0.5995(2) 0.0626(3) 1.0306(3) 0.0249(12) Uani 1 1 d . . .
N11 N 0.6723(2) 0.0582(3) 1.0127(3) 0.0216(11) Uani 1 1 d . . .
N12 N 0.6889(2) 0.1810(3) 1.0432(3) 0.0242(11) Uani 1 1 d . . .
N13 N 0.5586(2) -0.0522(3) 0.9493(3) 0.0244(12) Uani 1 1 d . . .
N14 N 0.5009(2) -0.1094(3) 0.8274(3) 0.0245(12) Uani 1 1 d . . .
N15 N 0.5780(2) -0.1236(3) 0.8188(3) 0.0252(12) Uani 1 1 d . . .
N16 N 0.6320(2) -0.0558(3) 0.9326(3) 0.0237(12) Uani 1 1 d . . .
C1 C 0.4448(3) 0.4637(4) 0.7707(4) 0.0228(14) Uani 1 1 d . . .
C2 C 0.5243(2) 0.5212(4) 0.7977(4) 0.0237(13) Uani 1 1 d . . .
H2 H 0.5345 0.5726 0.8202 0.028 Uiso 1 1 calc R . .
C3 C 0.5252(3) 0.4805(4) 0.9179(4) 0.0247(14) Uani 1 1 d . . .
H3A H 0.5430 0.5295 0.9402 0.030 Uiso 1 1 calc R . .
H3B H 0.4953 0.4756 0.9230 0.030 Uiso 1 1 calc R . .
C4 C 0.6269(2) 0.4762(4) 0.8811(4) 0.0259(14) Uani 1 1 d . . .
H4A H 0.6528 0.4665 0.8687 0.031 Uiso 1 1 calc R . .
H4B H 0.6382 0.5234 0.9116 0.031 Uiso 1 1 calc R . .
C5 C 0.5566(3) 0.3602(4) 0.9955(4) 0.0241(13) Uani 1 1 d . . .
C6 C 0.6247(3) 0.4274(4) 0.9960(4) 0.0240(13) Uani 1 1 d . . .
H6A H 0.6431 0.4740 1.0273 0.029 Uiso 1 1 calc R . .
C7 C 0.6525(2) 0.3560(4) 1.0513(4) 0.0239(13) Uani 1 1 d . . .
H7 H 0.6830 0.3694 1.1089 0.029 Uiso 1 1 calc R . .
C8 C 0.6605(3) 0.3493(4) 0.9447(4) 0.0269(14) Uani 1 1 d . . .
C9 C 0.6123(3) 0.2565(4) 1.0933(4) 0.0296(15) Uani 1 1 d . . .
H9C H 0.6456 0.2652 1.1499 0.036 Uiso 1 1 calc R . .
H9D H 0.5799 0.2544 1.0930 0.036 Uiso 1 1 calc R . .
C10 C 0.7144(2) 0.2543(4) 1.0562(4) 0.0267(14) Uani 1 1 d . . .
H10C H 0.7369 0.2528 1.0369 0.032 Uiso 1 1 calc R . .
H10D H 0.7397 0.2648 1.1150 0.032 Uiso 1 1 calc R . .
C11 C 0.5765(3) 0.1296(4) 1.0327(4) 0.0274(14) Uani 1 1 d . . .
C12 C 0.6720(3) 0.1544(4) 1.0922(4) 0.0219(13) Uani 1 1 d . . .
H12 H 0.7020 0.1616 1.1515 0.026 Uiso 1 1 calc R . .
C13 C 0.6591(3) 0.0697(3) 1.0690(4) 0.0219(13) Uani 1 1 d . . .
H13 H 0.6823 0.0373 1.1179 0.026 Uiso 1 1 calc R . .
C14 C 0.6918(3) 0.1240(4) 1.0010(4) 0.0230(13) Uani 1 1 d . . .
C15 C 0.5753(3) -0.0103(4) 1.0229(4) 0.0279(14) Uani 1 1 d . . .
H15A H 0.5423 -0.0034 1.0207 0.033 Uiso 1 1 calc R . .
H15B H 0.6025 -0.0401 1.0716 0.033 Uiso 1 1 calc R . .
C16 C 0.6835(2) -0.0156(4) 0.9975(4) 0.0246(14) Uani 1 1 d . . .
H16A H 0.7035 -0.0449 1.0482 0.029 Uiso 1 1 calc R . .
H16B H 0.7080 -0.0111 0.9817 0.029 Uiso 1 1 calc R . .
C17 C 0.5038(3) -0.0584(4) 0.8813(4) 0.0255(14) Uani 1 1 d . . .
C18 C 0.5968(2) -0.0987(4) 0.9461(4) 0.0225(13) Uani 1 1 d . . .
H18 H 0.6190 -0.1330 0.9936 0.027 Uiso 1 1 calc R . .
C19 C 0.5557(2) -0.1422(4) 0.8627(4) 0.0242(14) Uani 1 1 d . . .
H19 H 0.5562 -0.1968 0.8714 0.029 Uiso 1 1 calc R . .
C20 C 0.6208(3) -0.0738(3) 0.8594(4) 0.0216(13) Uani 1 1 d . . .
C21 C 0.4483(2) -0.1475(4) 0.7656(4) 0.0266(14) Uani 1 1 d . . .
H21A H 0.4220 -0.1386 0.7773 0.032 Uiso 1 1 calc R . .
H21B H 0.4553 -0.2015 0.7698 0.032 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
O1 U1 O2 178.6(2) . . ?
O1 U1 O5 93.2(2) . . ?
O2 U1 O5 87.9(2) . . ?
O1 U1 O6 88.0(2) . . ?
O2 U1 O6 93.1(2) . . ?
O5 U1 O6 67.97(17) . . ?
O1 U1 O17 88.0(2) . . ?
O2 U1 O17 90.6(2) . . ?
O5 U1 O17 145.45(16) . . ?
O6 U1 O17 146.54(16) . . ?
O1 U1 O7 98.1(3) . . ?
O2 U1 O7 81.4(3) . . ?
O5 U1 O7 143.95(18) . . ?
O6 U1 O7 78.30(19) . . ?
O17 U1 O7 69.40(18) . . ?
O1 U1 O8 91.4(3) . . ?
O2 U1 O8 88.2(2) . . ?
O5 U1 O8 72.01(17) . . ?
O6 U1 O8 139.87(18) . . ?
O17 U1 O8 73.44(17) . . ?
O7 U1 O8 141.2(2) . . ?
O4 U2 O3 176.6(2) . . ?
O4 U2 O5 89.38(19) . . ?
O3 U2 O5 91.76(19) . . ?
O4 U2 O6 89.2(2) . . ?
O3 U2 O6 94.2(2) . . ?
O5 U2 O6 67.73(17) . . ?
O4 U2 O22 85.58(19) . 3_455 ?
O3 U2 O22 91.70(19) . 3_455 ?
O5 U2 O22 145.57(15) . 3_455 ?
O6 U2 O22 145.98(16) . 3_455 ?
O4 U2 O10 89.9(2) . . ?
O3 U2 O10 87.3(2) . . ?
O5 U2 O10 74.45(15) . . ?
O6 U2 O10 142.17(17) . . ?
O22 U2 O10 71.52(15) 3_455 . ?
O4 U2 O9 91.6(2) . . ?
O3 U2 O9 89.4(2) . . ?
O5 U2 O9 143.38(16) . . ?
O6 U2 O9 75.68(17) . . ?
O22 U2 O9 70.89(16) 3_455 . ?
O10 U2 O9 142.15(17) . . ?
U1 O5 U2 112.76(19) . . ?
U1 O5 H5 126.5 . . ?
U2 O5 H5 106.1 . . ?
U1 O6 U2 111.3(2) . . ?
U1 O6 H6 121.5 . . ?
U2 O6 H6 126.3 . . ?
U1 O7 H7A 122.9 . . ?
U1 O7 H7B 129.1 . . ?
H7A O7 H7B 107.9 . . ?
U1 O8 H8A 133.5 . . ?
U1 O8 H8B 101.0 . . ?
H8A O8 H8B 101.8 . . ?
U2 O9 H9A 100.4 . . ?
U2 O9 H9B 112.5 . . ?
H9A O9 H9B 101.3 . . ?
U2 O10 H10A 110.8 . . ?
U2 O10 H10B 108.9 . . ?
H10A O10 H10B 111.1 . . ?
C1 O17 U1 155.9(4) . . ?
C20 O22 U2 152.5(4) . 3_545 ?
H24A O24 H24B 114.8 . . ?
H26A O26 H26B 94.8 . . ?
H27A O27 H27B 108.9 . . ?
H28A O28 H28B 105.9 . . ?
H29A O29 H29B 100.8 . . ?
O11 N1 O13 121.6(8) . . ?
O11 N1 O12 120.0(8) . . ?
O13 N1 O12 118.2(8) . . ?
O14 N2 O16 120.8(6) . . ?
O14 N2 O15 119.9(6) . . ?
O16 N2 O15 119.2(6) . . ?
C1 N3 C2 111.3(5) . . ?
C1 N3 C3 121.8(5) . . ?
C2 N3 C3 121.5(5) . . ?
C1 N4 C2 113.0(5) 2_656 . ?
C1 N4 C4 123.2(5) 2_656 . ?
C2 N4 C4 123.6(5) . . ?
C5 N5 C3 123.6(5) . . ?
C5 N5 C6 112.6(5) . . ?
C3 N5 C6 123.5(5) . . ?
C5 N6 C9 122.2(5) . . ?
C5 N6 C7 113.0(5) . . ?
C9 N6 C7 123.4(5) . . ?
C8 N7 C7 113.7(5) . . ?
C8 N7 C10 122.5(5) . . ?
C7 N7 C10 122.5(5) . . ?
C8 N8 C6 112.7(5) . . ?
C8 N8 C4 121.6(5) . . ?
C6 N8 C4 122.9(5) . . ?
C11 N9 C9 121.6(5) . . ?
C11 N9 C12 112.6(5) . . ?
C9 N9 C12 123.4(5) . . ?
C11 N10 C15 122.8(5) . . ?
C11 N10 C13 112.4(5) . . ?
C15 N10 C13 120.5(5) . . ?
C14 N11 C16 123.1(5) . . ?
C14 N11 C13 111.8(5) . . ?
C16 N11 C13 121.3(5) . . ?
C14 N12 C10 123.1(5) . . ?
C14 N12 C12 112.6(5) . . ?
C10 N12 C12 122.2(5) . . ?
C17 N13 C18 113.5(5) . . ?
C17 N13 C15 122.0(5) . . ?
C18 N13 C15 123.9(5) . . ?
C17 N14 C21 120.2(5) . . ?
C17 N14 C19 111.4(5) . . ?
C21 N14 C19 122.9(5) . . ?
C20 N15 C19 113.1(5) . . ?
C20 N15 C21 122.7(6) . 2_656 ?
C19 N15 C21 123.6(5) . 2_656 ?
C20 N16 C18 112.0(5) . . ?
C20 N16 C16 121.6(5) . . ?
C18 N16 C16 124.2(5) . . ?
O17 C1 N3 124.8(6) . . ?
O17 C1 N4 125.8(6) . 2_656 ?
N3 C1 N4 109.3(5) . 2_656 ?
N4 C2 N3 115.4(5) . . ?
N4 C2 C2 102.3(6) . 2_656 ?
N3 C2 C2 103.2(5) . 2_656 ?
N4 C2 H2 111.7 . . ?
N3 C2 H2 111.7 . . ?
C2 C2 H2 111.7 2_656 . ?
N5 C3 N3 113.1(5) . . ?
N5 C3 H3A 109.0 . . ?
N3 C3 H3A 109.0 . . ?
N5 C3 H3B 109.0 . . ?
N3 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
N8 C4 N4 113.3(5) . . ?
N8 C4 H4A 108.9 . . ?
N4 C4 H4A 108.9 . . ?
N8 C4 H4B 108.9 . . ?
N4 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
O19 C5 N6 126.9(6) . . ?
O19 C5 N5 124.9(6) . . ?
N6 C5 N5 108.2(5) . . ?
N8 C6 N5 114.4(5) . . ?
N8 C6 C7 103.2(5) . . ?
N5 C6 C7 103.1(5) . . ?
N8 C6 H6A 111.8 . . ?
N5 C6 H6A 111.8 . . ?
C7 C6 H6A 111.8 . . ?
N7 C7 N6 114.9(5) . . ?
N7 C7 C6 103.1(5) . . ?
N6 C7 C6 103.1(5) . . ?
N7 C7 H7 111.7 . . ?
N6 C7 H7 111.7 . . ?
C6 C7 H7 111.7 . . ?
O18 C8 N7 126.8(6) . . ?
O18 C8 N8 125.9(6) . . ?
N7 C8 N8 107.3(6) . . ?
N9 C9 N6 113.4(5) . . ?
N9 C9 H9C 108.9 . . ?
N6 C9 H9C 108.9 . . ?
N9 C9 H9D 108.9 . . ?
N6 C9 H9D 108.9 . . ?
H9C C9 H9D 107.7 . . ?
N12 C10 N7 113.7(5) . . ?
N12 C10 H10C 108.8 . . ?
N7 C10 H10C 108.8 . . ?
N12 C10 H10D 108.8 . . ?
N7 C10 H10D 108.8 . . ?
H10C C10 H10D 107.7 . . ?
O21 C11 N10 125.8(6) . . ?
O21 C11 N9 126.7(6) . . ?
N10 C11 N9 107.5(5) . . ?
N9 C12 N12 114.0(5) . . ?
N9 C12 C13 103.3(5) . . ?
N12 C12 C13 103.1(5) . . ?
N9 C12 H12 111.9 . . ?
N12 C12 H12 111.9 . . ?
C13 C12 H12 111.9 . . ?
N11 C13 N10 113.9(5) . . ?
N11 C13 C12 104.1(5) . . ?
N10 C13 C12 104.0(5) . . ?
N11 C13 H13 111.4 . . ?
N10 C13 H13 111.4 . . ?
C12 C13 H13 111.4 . . ?
O20 C14 N12 126.2(6) . . ?
O20 C14 N11 125.7(6) . . ?
N12 C14 N11 108.1(5) . . ?
N10 C15 N13 113.3(5) . . ?
N10 C15 H15A 108.9 . . ?
N13 C15 H15A 108.9 . . ?
N10 C15 H15B 108.9 . . ?
N13 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
N11 C16 N16 112.5(5) . . ?
N11 C16 H16A 109.1 . . ?
N16 C16 H16A 109.1 . . ?
N11 C16 H16B 109.1 . . ?
N16 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
O23 C17 N13 127.1(6) . . ?
O23 C17 N14 124.4(6) . . ?
N13 C17 N14 108.4(6) . . ?
N13 C18 N16 113.5(5) . . ?
N13 C18 C19 102.5(5) . . ?
N16 C18 C19 102.8(5) . . ?
N13 C18 H18 112.4 . . ?
N16 C18 H18 112.4 . . ?
C19 C18 H18 112.4 . . ?
N14 C19 N15 114.3(5) . . ?
N14 C19 C18 103.8(5) . . ?
N15 C19 C18 102.4(5) . . ?
N14 C19 H19 111.9 . . ?
N15 C19 H19 111.9 . . ?
C18 C19 H19 111.9 . . ?
O22 C20 N15 125.9(6) . . ?
O22 C20 N16 124.8(6) . . ?
N15 C20 N16 109.3(5) . . ?
N14 C21 N15 114.1(5) . 2_656 ?
N14 C21 H21A 108.7 . . ?
N15 C21 H21A 108.7 2_656 . ?
N14 C21 H21B 108.7 . . ?
N15 C21 H21B 108.7 2_656 . ?
H21A C21 H21B 107.6 . . ?
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 O1 1.743(5) . ?
U1 O2 1.772(5) . ?
U1 O5 2.309(4) . ?
U1 O6 2.335(5) . ?
U1 O17 2.422(4) . ?
U1 O7 2.430(6) . ?
U1 O8 2.451(5) . ?
U1 U2 3.8572(3) . ?
U2 O4 1.771(5) . ?
U2 O3 1.777(5) . ?
U2 O5 2.322(4) . ?
U2 O6 2.337(5) . ?
U2 O22 2.403(4) 3_455 ?
U2 O10 2.436(5) . ?
U2 O9 2.439(5) . ?
O5 H5 0.9251 . ?
O6 H6 0.9728 . ?
O7 H7A 0.8886 . ?
O7 H7B 0.9714 . ?
O8 H8A 0.7663 . ?
O8 H8B 0.9022 . ?
O9 H9A 0.9451 . ?
O9 H9B 0.8564 . ?
O10 H10A 1.0245 . ?
O10 H10B 0.9113 . ?
O11 N1 1.250(10) . ?
O12 N1 1.272(10) . ?
O13 N1 1.262(9) . ?
O14 N2 1.230(8) . ?
O15 N2 1.273(8) . ?
O16 N2 1.247(8) . ?
O17 C1 1.235(8) . ?
O18 C8 1.215(8) . ?
O19 C5 1.214(8) . ?
O20 C14 1.218(8) . ?
O21 C11 1.216(8) . ?
O22 C20 1.229(8) . ?
O22 U2 2.403(4) 3_545 ?
O23 C17 1.225(8) . ?
O24 H24A 0.8525 . ?
O24 H24B 0.9096 . ?
O26 H26A 1.0593 . ?
O26 H26B 0.9009 . ?
O27 H27A 0.8259 . ?
O27 H27B 0.9767 . ?
O28 H28A 0.8387 . ?
O28 H28B 0.9863 . ?
O29 H29A 0.9132 . ?
O29 H29B 1.0479 . ?
N3 C1 1.351(8) . ?
N3 C2 1.462(8) . ?
N3 C3 1.467(8) . ?
N4 C1 1.356(8) 2_656 ?
N4 C2 1.444(8) . ?
N4 C4 1.460(8) . ?
N5 C5 1.374(8) . ?
N5 C3 1.429(8) . ?
N5 C6 1.458(8) . ?
N6 C5 1.360(8) . ?
N6 C9 1.450(8) . ?
N6 C7 1.459(8) . ?
N7 C8 1.363(8) . ?
N7 C7 1.440(8) . ?
N7 C10 1.460(8) . ?
N8 C8 1.382(8) . ?
N8 C6 1.449(8) . ?
N8 C4 1.454(8) . ?
N9 C11 1.385(9) . ?
N9 C9 1.444(8) . ?
N9 C12 1.454(8) . ?
N10 C11 1.383(9) . ?
N10 C15 1.440(8) . ?
N10 C13 1.449(8) . ?
N11 C14 1.388(8) . ?
N11 C16 1.428(8) . ?
N11 C13 1.448(8) . ?
N12 C14 1.367(8) . ?
N12 C10 1.442(8) . ?
N12 C12 1.456(8) . ?
N13 C17 1.356(8) . ?
N13 C18 1.443(8) . ?
N13 C15 1.466(9) . ?
N14 C17 1.387(8) . ?
N14 C21 1.445(8) . ?
N14 C19 1.448(8) . ?
N15 C20 1.343(8) . ?
N15 C19 1.454(8) . ?
N15 C21 1.455(8) 2_656 ?
N16 C20 1.359(8) . ?
N16 C18 1.460(8) . ?
N16 C16 1.462(8) . ?
C1 N4 1.356(8) 2_656 ?
C2 C2 1.563(12) 2_656 ?
C2 H2 0.9800 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C7 1.552(9) . ?
C6 H6A 0.9800 . ?
C7 H7 0.9800 . ?
C9 H9C 0.9700 . ?
C9 H9D 0.9700 . ?
C10 H10C 0.9700 . ?
C10 H10D 0.9700 . ?
C12 C13 1.547(9) . ?
C12 H12 0.9800 . ?
C13 H13 0.9800 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C18 C19 1.563(9) . ?
C18 H18 0.9800 . ?
C19 H19 0.9800 . ?
C21 N15 1.455(8) 2_656 ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
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
O5 H5 O16 0.93 1.90 2.778(7) 157.9 6_565
O6 H6 O14 0.97 1.96 2.863(8) 152.6 7_557
O7 H7A O24 0.89 1.76 2.640(14) 170.2 .
O8 H8A O25 0.77 1.83 2.591(8) 176.7 .
O9 H9A O27 0.95 2.15 2.682(9) 114.3 .
O9 H9B O14 0.86 2.86 3.369(8) 120.2 7_557
O10 H10A O26 1.02 1.60 2.627(8) 177.2 .
O10 H10B O20 0.91 1.85 2.736(6) 163.1 3_455
O24 H24A O26 0.85 1.81 2.606(15) 154.4 4_546
O26 H26A O23 1.06 1.69 2.720(8) 163.4 4_556
O27 H27A O11 0.83 2.08 2.832(10) 151.9 .
O28 H28A O25 0.84 1.89 2.720(12) 170.6 .
