#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:23:26 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179628 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/92/4509283.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4509283
loop_
_publ_author_name
'Thuéry, Pierre'
_publ_section_title
;
 Uranyl Ion Complexes with Cucurbit[5]uril: from Molecular Capsules to
 Uranyl-Organic Frameworks
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1208
_journal_page_last               1215
_journal_paper_doi               10.1021/cg8011603
_journal_volume                  9
_journal_year                    2009
_chemical_formula_sum            'C32 H54 K2 N20 O37 U4'
_chemical_formula_weight         2341.27
_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                 97.141(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2911(5)
_cell_length_b                   14.2734(10)
_cell_length_c                   17.7435(12)
_cell_measurement_reflns_used    82565
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.27
_cell_volume                     2837.4(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and four ω scans with 2° steps (395 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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            82565
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.651
_exptl_absorpt_correction_T_max  0.497
_exptl_absorpt_correction_T_min  0.393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.141
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5598
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0285
_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)+(0.0333P)²+0.2529P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                3870
_reflns_number_total             5598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg8011603sup1.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4509283
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
U1 U 0.982322(16) 0.112716(18) 1.057537(12) 0.01554(8) Uani 1 1 d .
U2 U 0.007300(16) 0.113699(18) 0.442208(12) 0.01546(8) Uani 1 1 d .
K1 K 0.70628(16) 0.2500 0.93784(12) 0.0270(5) Uani 1 2 d S
K2 K 0.29571(17) 0.2500 0.55824(13) 0.0354(6) Uani 1 2 d S
O1 O 0.8238(3) 0.1020(3) 1.0438(3) 0.0206(10) Uani 1 1 d .
O2 O 1.1421(4) 0.1242(3) 1.0743(3) 0.0238(10) Uani 1 1 d .
O3 O 0.1664(4) 0.0995(3) 0.4417(3) 0.0268(11) Uani 1 1 d .
O4 O -0.1518(3) 0.1287(3) 0.4413(2) 0.0202(10) Uani 1 1 d .
O5 O 0.9633(4) 0.0600(3) 1.1861(3) 0.0261(11) Uani 1 1 d .
O6 O 0.9636(4) 0.0653(3) 1.3108(2) 0.0285(11) Uani 1 1 d .
O7 O 0.9700(5) 0.2500 0.9805(3) 0.0204(14) Uani 1 2 d S
H7 H 0.9904 0.2500 0.9368 0.024 Uiso 1 2 d SR
O8 O 0.9845(4) 0.0519(3) 0.9361(2) 0.0210(10) Uani 1 1 d .
H8 H 0.9203 0.0593 0.8979 0.025 Uiso 1 1 d R
O9 O 0.9638(5) 0.2500 1.1278(3) 0.0206(14) Uani 1 2 d S
H9 H 0.8906 0.2500 1.1462 0.025 Uiso 1 2 d SR
O10 O 0.0447(5) 0.2500 0.5202(3) 0.0171(14) Uani 1 2 d S
H10 H 0.0036 0.2500 0.5598 0.020 Uiso 1 2 d SR
O11 O -0.0170(4) -0.0515(3) 0.4366(2) 0.0182(10) Uani 1 1 d .
H11 H -0.0818 -0.0636 0.3950 0.022 Uiso 1 1 d R
O12 O 0.0192(5) 0.2500 0.3707(3) 0.0200(14) Uani 1 2 d S
H12 H 0.0804 0.2500 0.3475 0.024 Uiso 1 2 d SR
O13A O 0.5319(12) 0.2500 0.7895(9) 0.072(5) Uani 0.704(18) 2 d SPU
O13B O 0.458(6) 0.2500 0.716(4) 0.072(5) Uani 0.296(9) 2 d SPU
O14 O 0.5157(4) 0.1452(4) 0.9701(3) 0.0355(12) Uani 1 1 d .
O15 O 0.1896(5) 0.1413(5) 0.6676(3) 0.0639(19) Uani 1 1 d .
O16 O 0.7379(5) 0.0804(4) 0.8699(3) 0.0455(14) Uani 1 1 d .
O17 O 0.3966(5) 0.0737(4) 0.5810(3) 0.0473(15) Uani 1 1 d .
O18 O 0.8561(5) 0.2500 0.8165(4) 0.046(2) Uani 1 2 d S
O19 O 0.5206(5) 0.2500 0.5251(4) 0.0259(16) Uani 1 2 d S
O20 O 1.2993(5) 0.2500 1.1557(4) 0.0355(18) Uani 1 2 d S
O21 O -0.3027(6) 0.2500 0.3510(4) 0.0385(19) Uani 1 2 d S
O22 O 0.7623(6) 0.2500 1.2005(4) 0.050(2) Uani 1 2 d S
O23 O 0.2280(5) 0.2500 0.3031(4) 0.0346(18) Uani 1 2 d S
O24 O 0.4583(7) 0.2500 0.3728(5) 0.067(3) Uani 1 2 d SU
O25 O 0.5370(6) 0.2500 1.1228(4) 0.040(2) Uani 1 2 d S
N1 N 0.3187(5) 0.1664(6) 0.9183(4) 0.053(2) Uani 1 1 d .
N2 N 0.4200(6) 0.0470(5) 0.8779(4) 0.0460(19) Uani 1 1 d .
N3 N 0.2866(6) 0.0421(6) 0.7577(4) 0.056(2) Uani 1 1 d .
N4 N 0.1896(6) 0.1654(6) 0.7962(4) 0.056(2) Uani 1 1 d .
N5 N 0.5800(7) -0.0041(5) 0.8085(4) 0.0472(19) Uani 1 1 d .
N6 N 0.7314(6) 0.0318(5) 0.7443(4) 0.049(2) Uani 1 1 d .
N7 N 0.5909(6) 0.0359(5) 0.6281(3) 0.0419(17) Uani 1 1 d .
N8 N 0.4433(7) -0.0159(5) 0.6891(4) 0.0487(19) Uani 1 1 d .
N9 N 0.8201(5) 0.1736(5) 0.7012(3) 0.0396(17) Uani 1 1 d .
N10 N 0.6869(4) 0.1727(5) 0.5823(3) 0.0313(15) Uani 1 1 d .
C1 C 0.9813(5) 0.0993(5) 1.2487(4) 0.0257(14) Uani 1 1 d .
H1 H 1.0109 0.1602 1.2494 0.031 Uiso 1 1 calc R
C2 C 0.4271(7) 0.1205(6) 0.9264(4) 0.045(2) Uani 1 1 d .
C3 C 0.2292(7) 0.1179(7) 0.8680(5) 0.054(2) Uani 1 1 d .
H3 H 0.1620 0.0976 0.8940 0.065 Uiso 1 1 calc R
C4 C 0.3014(8) 0.0319(7) 0.8401(5) 0.058(3) Uani 1 1 d .
H4 H 0.2687 -0.0279 0.8553 0.070 Uiso 1 1 calc R
C5 C 0.2185(8) 0.1185(7) 0.7354(5) 0.055(2) Uani 1 1 d .
C6 C 0.5185(8) -0.0157(7) 0.8742(5) 0.055(2) Uani 1 1 d .
H6A H 0.4892 -0.0795 0.8748 0.066 Uiso 1 1 calc R
H6B H 0.5753 -0.0070 0.9193 0.066 Uiso 1 1 calc R
C7 C 0.3246(8) -0.0257(7) 0.7071(5) 0.061(3) Uani 1 1 d .
H7A H 0.3170 -0.0873 0.7291 0.073 Uiso 1 1 calc R
H7B H 0.2706 -0.0235 0.6601 0.073 Uiso 1 1 calc R
C8 C 0.6874(8) 0.0401(6) 0.8126(4) 0.045(2) Uani 1 1 d .
C9 C 0.5482(9) -0.0496(7) 0.7352(5) 0.058(2) Uani 1 1 d .
H9A H 0.5457 -0.1179 0.7408 0.070 Uiso 1 1 calc R
C10 C 0.6519(8) -0.0194(6) 0.6896(5) 0.053(2) Uani 1 1 d .
H10A H 0.6916 -0.0740 0.6703 0.063 Uiso 1 1 calc R
C11 C 0.4693(8) 0.0351(6) 0.6289(5) 0.047(2) Uani 1 1 d .
C12 C 0.8394(7) 0.0815(7) 0.7299(5) 0.055(2) Uani 1 1 d .
H12A H 0.8931 0.0846 0.7769 0.067 Uiso 1 1 calc R
H12B H 0.8788 0.0454 0.6939 0.067 Uiso 1 1 calc R
C13 C 0.6446(7) 0.0779(6) 0.5668(4) 0.044(2) Uani 1 1 d .
H13A H 0.5865 0.0784 0.5217 0.052 Uiso 1 1 calc R
H13B H 0.7112 0.0393 0.5561 0.052 Uiso 1 1 calc R
C14 C 0.8337(8) 0.2500 0.7460(7) 0.049(4) Uani 1 2 d S
C15 C 0.8025(5) 0.1950(6) 0.6218(4) 0.041(2) Uani 1 1 d .
H15 H 0.8669 0.1697 0.5956 0.049 Uiso 1 1 calc R
C16 C 0.6204(8) 0.2500 0.5598(5) 0.030(2) Uani 1 2 d S
C17 C 0.2941(9) 0.2500 0.9595(7) 0.046(3) Uani 1 2 d S
H17A H 0.3426 0.2500 1.0086 0.055 Uiso 1 2 calc SR
H17B H 0.2109 0.2500 0.9681 0.055 Uiso 1 2 calc SR
C18 C 0.1249(10) 0.2500 0.7901(7) 0.059(4) Uani 1 2 d S
H18A H 0.0719 0.2500 0.8292 0.071 Uiso 1 2 calc SR
H18B H 0.0751 0.2500 0.7415 0.071 Uiso 1 2 calc SR
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'
K K 0.2009 0.2494 '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
O1 U1 O2 178.31(18) . .
O1 U1 O8 88.15(17) . .
O2 U1 O8 93.51(17) . .
O1 U1 O9 89.4(2) . .
O2 U1 O9 89.4(2) . .
O8 U1 O9 144.69(16) . .
O1 U1 O8 94.10(17) . 3_757
O2 U1 O8 86.17(17) . 3_757
O8 U1 O8 69.87(17) . 3_757
O9 U1 O8 145.42(16) . 3_757
O1 U1 O7 90.36(19) . .
O2 U1 O7 90.3(2) . .
O8 U1 O7 77.41(16) . .
O9 U1 O7 67.39(17) . .
O8 U1 O7 146.78(15) 3_757 .
O1 U1 O5 84.12(17) . .
O2 U1 O5 94.39(18) . .
O8 U1 O5 139.86(16) . .
O9 U1 O5 74.69(16) . .
O8 U1 O5 71.49(14) 3_757 .
O7 U1 O5 141.72(16) . .
O4 U2 O3 179.15(19) . .
O4 U2 O11 89.20(17) . 3_556
O3 U2 O11 91.66(17) . 3_556
O4 U2 O12 91.20(19) . .
O3 U2 O12 88.09(19) . .
O11 U2 O12 145.52(16) 3_556 .
O4 U2 O11 90.42(17) . .
O3 U2 O11 89.89(17) . .
O11 U2 O11 69.53(17) 3_556 .
O12 U2 O11 144.93(15) . .
O4 U2 O10 90.73(18) . .
O3 U2 O10 89.44(19) . .
O11 U2 O10 77.89(15) 3_556 .
O12 U2 O10 67.62(17) . .
O11 U2 O10 147.38(15) . .
O4 U2 O6 86.64(17) . 1_454
O3 U2 O6 92.71(18) . 1_454
O11 U2 O6 139.87(15) 3_556 1_454
O12 U2 O6 74.52(17) . 1_454
O11 U2 O6 70.62(15) . 1_454
O10 U2 O6 141.99(16) . 1_454
O14 K1 O14 66.2(2) 4_565 .
O14 K1 O16 136.14(17) 4_565 .
O14 K1 O16 76.04(15) . .
O14 K1 O16 76.04(15) 4_565 4_565
O14 K1 O16 136.14(17) . 4_565
O16 K1 O16 123.5(2) . 4_565
O14 K1 O18 134.52(14) 4_565 .
O14 K1 O18 134.52(14) . .
O16 K1 O18 63.53(12) . .
O16 K1 O18 63.53(12) 4_565 .
O14 K1 O7 137.16(14) 4_565 .
O14 K1 O7 137.16(14) . .
O16 K1 O7 86.07(13) . .
O16 K1 O7 86.07(13) 4_565 .
O18 K1 O7 62.09(18) . .
O14 K1 O1 123.18(15) 4_565 .
O14 K1 O1 77.53(13) . .
O16 K1 O1 65.58(14) . .
O16 K1 O1 144.87(15) 4_565 .
O18 K1 O1 102.16(13) . .
O7 K1 O1 59.64(11) . .
O14 K1 O1 77.53(13) 4_565 4_565
O14 K1 O1 123.18(15) . 4_565
O16 K1 O1 144.87(15) . 4_565
O16 K1 O1 65.58(14) 4_565 4_565
O18 K1 O1 102.16(13) . 4_565
O7 K1 O1 59.64(11) . 4_565
O1 K1 O1 88.65(18) . 4_565
O14 K1 O13A 75.1(2) 4_565 .
O14 K1 O13A 75.1(2) . .
O16 K1 O13A 74.30(15) . .
O16 K1 O13A 74.30(15) 4_565 .
O18 K1 O13A 74.7(3) . .
O7 K1 O13A 136.8(3) . .
O1 K1 O13A 135.65(9) . .
O1 K1 O13A 135.65(9) 4_565 .
O19 K2 O17 69.38(11) . .
O19 K2 O17 69.38(11) . 4_565
O17 K2 O17 130.5(2) . 4_565
O19 K2 O10 153.7(2) . .
O17 K2 O10 114.59(11) . .
O17 K2 O10 114.59(11) 4_565 .
O19 K2 O15 129.60(18) . .
O17 K2 O15 66.92(18) . .
O17 K2 O15 126.36(18) 4_565 .
O10 K2 O15 70.76(17) . .
O19 K2 O15 129.60(18) . 4_565
O17 K2 O15 126.36(18) . 4_565
O17 K2 O15 66.92(18) 4_565 4_565
O10 K2 O15 70.76(16) . 4_565
O15 K2 O15 65.7(3) . 4_565
O19 K2 O13B 74.4(11) . .
O17 K2 O13B 71.8(3) . .
O17 K2 O13B 71.8(3) 4_565 .
O10 K2 O13B 131.8(11) . .
O15 K2 O13B 69.1(9) . .
O15 K2 O13B 69.1(9) 4_565 .
O19 K2 O3 103.13(13) . .
O17 K2 O3 68.37(14) . .
O17 K2 O3 148.09(16) 4_565 .
O10 K2 O3 58.92(11) . .
O15 K2 O3 83.01(14) . .
O15 K2 O3 127.26(17) 4_565 .
O13B K2 O3 137.85(10) . .
O19 K2 O3 103.12(13) . 4_565
O17 K2 O3 148.09(16) . 4_565
O17 K2 O3 68.37(14) 4_565 4_565
O10 K2 O3 58.92(11) . 4_565
O15 K2 O3 127.26(17) . 4_565
O15 K2 O3 83.01(14) 4_565 4_565
O13B K2 O3 137.85(10) . 4_565
O3 K2 O3 84.19(17) . 4_565
U1 O1 K1 112.37(18) . .
U1 O2 O20 134.6(2) . .
U2 O3 K2 107.15(19) . .
U2 O4 O21 127.9(2) . .
C1 O5 U1 132.6(4) . .
C1 O6 U2 134.9(4) . 1_656
U1 O7 U1 110.6(2) . 4_565
U1 O7 K1 97.52(15) . .
U1 O7 K1 97.52(15) 4_565 .
U1 O7 H7 121.9 . .
U1 O7 H7 121.9 4_565 .
K1 O7 H7 98.4 . .
U1 O8 U1 110.12(17) . 3_757
U1 O8 H8 122.2 . .
U1 O8 H8 104.4 3_757 .
U1 O9 U1 113.3(2) . 4_565
U1 O9 H9 109.3 . .
U1 O9 H9 109.3 4_565 .
U2 O10 U2 108.7(2) . 4_565
U2 O10 K2 103.71(14) . .
U2 O10 K2 103.71(14) 4_565 .
U2 O10 H10 112.7 . .
U2 O10 H10 112.7 4_565 .
K2 O10 H10 114.6 . .
U2 O11 U2 110.47(17) 3_556 .
U2 O11 H11 124.9 3_556 .
U2 O11 H11 106.0 . .
U2 O12 U2 112.8(2) 4_565 .
U2 O12 H12 111.7 4_565 .
U2 O12 H12 111.7 . .
C2 O14 K1 128.3(5) . .
C5 O15 K2 135.4(5) . .
C8 O16 K1 134.1(5) . .
C11 O17 K2 137.0(5) . .
C14 O18 K1 133.0(6) . .
C16 O19 K2 137.3(6) . .
C2 N1 C3 112.4(7) . .
C2 N1 C17 124.4(7) . .
C3 N1 C17 123.1(8) . .
C2 N2 C6 121.9(7) . .
C2 N2 C4 113.0(8) . .
C6 N2 C4 124.5(8) . .
C5 N3 C7 124.4(8) . .
C5 N3 C4 111.1(8) . .
C7 N3 C4 124.0(9) . .
C5 N4 C18 122.8(9) . .
C5 N4 C3 112.9(9) . .
C18 N4 C3 124.3(9) . .
C8 N5 C6 121.8(7) . .
C8 N5 C9 112.0(7) . .
C6 N5 C9 125.5(8) . .
C8 N6 C10 112.1(8) . .
C8 N6 C12 121.0(8) . .
C10 N6 C12 126.4(7) . .
C11 N7 C13 121.7(7) . .
C11 N7 C10 111.7(7) . .
C13 N7 C10 126.1(7) . .
C11 N8 C7 122.2(8) . .
C11 N8 C9 112.6(8) . .
C7 N8 C9 124.9(7) . .
C14 N9 C12 122.6(7) . .
C14 N9 C15 113.6(8) . .
C12 N9 C15 123.2(7) . .
C16 N10 C15 113.3(7) . .
C16 N10 C13 122.9(6) . .
C15 N10 C13 123.8(6) . .
O5 C1 O6 126.3(6) . .
O5 C1 H1 116.8 . .
O6 C1 H1 116.8 . .
O14 C2 N2 126.8(8) . .
O14 C2 N1 124.5(8) . .
N2 C2 N1 108.7(7) . .
N1 C3 N4 115.6(7) . .
N1 C3 C4 102.6(7) . .
N4 C3 C4 101.6(7) . .
N1 C3 H3 112.1 . .
N4 C3 H3 112.1 . .
C4 C3 H3 112.1 . .
N2 C4 N3 115.9(6) . .
N2 C4 C3 102.9(7) . .
N3 C4 C3 103.7(8) . .
N2 C4 H4 111.3 . .
N3 C4 H4 111.3 . .
C3 C4 H4 111.3 . .
O15 C5 N4 125.6(11) . .
O15 C5 N3 123.8(9) . .
N4 C5 N3 110.6(8) . .
N2 C6 N5 114.9(7) . .
N2 C6 H6A 108.5 . .
N5 C6 H6A 108.5 . .
N2 C6 H6B 108.5 . .
N5 C6 H6B 108.5 . .
H6A C6 H6B 107.5 . .
N8 C7 N3 116.1(7) . .
N8 C7 H7A 108.3 . .
N3 C7 H7A 108.3 . .
N8 C7 H7B 108.3 . .
N3 C7 H7B 108.3 . .
H7A C7 H7B 107.4 . .
O16 C8 N5 125.0(7) . .
O16 C8 N6 125.7(9) . .
N5 C8 N6 109.3(8) . .
N8 C9 N5 116.9(7) . .
N8 C9 C10 103.3(7) . .
N5 C9 C10 102.8(7) . .
N8 C9 H9A 111.1 . .
N5 C9 H9A 111.1 . .
C10 C9 H9A 111.1 . .
N6 C10 N7 115.4(7) . .
N6 C10 C9 103.6(7) . .
N7 C10 C9 102.9(7) . .
N6 C10 H10A 111.4 . .
N7 C10 H10A 111.4 . .
C9 C10 H10A 111.4 . .
O17 C11 N8 126.3(9) . .
O17 C11 N7 124.6(8) . .
N8 C11 N7 109.1(8) . .
N9 C12 N6 114.8(6) . .
N9 C12 H12A 108.6 . .
N6 C12 H12A 108.6 . .
N9 C12 H12B 108.6 . .
N6 C12 H12B 108.6 . .
H12A C12 H12B 107.6 . .
N7 C13 N10 113.9(6) . .
N7 C13 H13A 108.8 . .
N10 C13 H13A 108.8 . .
N7 C13 H13B 108.8 . .
N10 C13 H13B 108.8 . .
H13A C13 H13B 107.7 . .
O18 C14 N9 125.9(5) . .
O18 C14 N9 125.9(5) . 4_565
N9 C14 N9 108.1(10) . 4_565
N9 C15 N10 116.1(6) . .
N9 C15 C15 102.3(5) . 4_565
N10 C15 C15 102.8(4) . 4_565
N9 C15 H15 111.6 . .
N10 C15 H15 111.6 . .
C15 C15 H15 111.6 4_565 .
O19 C16 N10 126.1(4) . 4_565
O19 C16 N10 126.1(4) . .
N10 C16 N10 107.8(8) 4_565 .
N1 C17 N1 111.4(10) . 4_565
N1 C17 H17A 109.3 . .
N1 C17 H17A 109.3 4_565 .
N1 C17 H17B 109.3 . .
N1 C17 H17B 109.3 4_565 .
H17A C17 H17B 108.0 . .
N4 C18 N4 118.0(10) . 4_565
N4 C18 H18A 107.8 . .
N4 C18 H18A 107.8 4_565 .
N4 C18 H18B 107.8 . .
N4 C18 H18B 107.8 4_565 .
H18A C18 H18B 107.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.783(4) .
U1 O2 1.799(4) .
U1 O8 2.326(4) .
U1 O9 2.346(3) .
U1 O8 2.380(4) 3_757
U1 O7 2.383(3) .
U1 O5 2.436(4) .
U1 U1 3.8580(5) 3_757
U1 U1 3.9191(6) 4_565
U1 K1 4.0520(18) .
U2 O4 1.807(4) .
U2 O3 1.809(4) .
U2 O11 2.316(4) 3_556
U2 O12 2.336(3) .
U2 O11 2.375(4) .
U2 O10 2.394(3) .
U2 O6 2.422(4) 1_454
U2 U2 3.8539(5) 3_556
U2 U2 3.8910(6) 4_565
U2 K2 4.1184(18) .
K1 O14 2.739(4) 4_565
K1 O14 2.739(5) .
K1 O16 2.747(6) .
K1 O16 2.747(6) 4_565
K1 O18 2.899(6) .
K1 O7 2.980(6) .
K1 O1 3.023(5) .
K1 O1 3.023(5) 4_565
K1 O13A 3.085(17) .
K1 U1 4.0521(18) 4_565
K2 O19 2.677(6) .
K2 O17 2.771(6) .
K2 O17 2.771(6) 4_565
K2 O10 2.831(6) .
K2 O15 2.862(5) .
K2 O15 2.862(5) 4_565
K2 O13B 3.15(8) .
K2 O3 3.205(5) .
K2 O3 3.205(5) 4_565
O2 O20 2.797(7) .
O4 O21 2.791(7) .
O5 C1 1.239(7) .
O6 C1 1.243(7) .
O6 U2 2.422(4) 1_656
O7 U1 2.383(3) 4_565
O7 H7 0.8367 .
O8 U1 2.380(4) 3_757
O8 H8 0.9341 .
O9 U1 2.346(3) 4_565
O9 H9 0.9255 .
O10 U2 2.394(3) 4_565
O10 H10 0.8896 .
O11 U2 2.316(4) 3_556
O11 H11 0.9880 .
O12 U2 2.336(3) 4_565
O12 H12 0.8470 .
O14 C2 1.238(8) .
O15 C5 1.250(10) .
O16 C8 1.242(10) .
O17 C11 1.236(10) .
O18 C14 1.244(13) .
O19 C16 1.215(11) .
N1 C2 1.380(10) .
N1 C3 1.440(10) .
N1 C17 1.444(9) .
N2 C2 1.353(10) .
N2 C6 1.435(10) .
N2 C4 1.438(10) .
N3 C5 1.364(12) .
N3 C7 1.422(11) .
N3 C4 1.459(10) .
N4 C5 1.343(11) .
N4 C18 1.408(9) .
N4 C3 1.464(11) .
N5 C8 1.361(11) .
N5 C6 1.439(10) .
N5 C9 1.458(10) .
N6 C8 1.372(9) .
N6 C10 1.438(11) .
N6 C12 1.460(11) .
N7 C11 1.374(10) .
N7 C13 1.440(9) .
N7 C10 1.449(9) .
N8 C11 1.355(10) .
N8 C7 1.423(10) .
N8 C9 1.436(11) .
N9 C14 1.347(9) .
N9 C12 1.416(11) .
N9 C15 1.431(8) .
N10 C16 1.366(8) .
N10 C15 1.438(8) .
N10 C13 1.450(10) .
C1 H1 0.9300 .
C3 C4 1.587(13) .
C3 H3 0.9800 .
C4 H4 0.9800 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C9 C10 1.565(12) .
C9 H9A 0.9800 .
C10 H10A 0.9800 .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 N9 1.347(9) 4_565
C15 C15 1.571(17) 4_565
C15 H15 0.9800 .
C16 N10 1.366(8) 4_565
C17 N1 1.444(9) 4_565
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C18 N4 1.408(9) 4_565
C18 H18A 0.9700 .
C18 H18B 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
O8 H8 O16 0.93 2.08 2.913(7) 147.8 .
O9 H9 O22 0.93 1.84 2.752(8) 169.1 .
O11 H11 O15 0.99 1.90 2.822(7) 154.2 3_556
O12 H12 O23 0.85 1.93 2.775(8) 175.1 .
