#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:39:03 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179540 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/09/4500937.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_4500937
loop_
_publ_author_name
'Thuéry, Pierre'
_publ_section_title
;
 Uranyl--Alkali Metal Ion Heterometallic Complexes with Cucurbit[6]uril
 and a Sulfonated Catechol
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3282
_journal_paper_doi               10.1021/cg2005375
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C48 H66 N24 Na2 O44 S4 U2'
_chemical_formula_weight         2333.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 113.284(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.4467(5)
_cell_length_b                   15.8288(3)
_cell_length_c                   16.1585(5)
_cell_measurement_reflns_used    126112
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      2.35
_cell_volume                     3629.03(18)
_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, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and six ω scans with 2° steps (453 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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            126112
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.709
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_density_diffrn    2.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.528
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0262
_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)+(0.0328P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                7769
_reflns_number_total             9363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2005375_si_002.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4500937
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
U U 0.917173(7) 0.565535(6) 0.786370(7) 0.01612(4) Uani 1 1 d .
Na Na 0.25409(9) 0.88786(8) 0.48466(9) 0.0281(3) Uani 1 1 d .
S1 S 0.70949(5) 0.54394(5) 0.57914(5) 0.01864(15) Uani 1 1 d .
S2 S 0.44991(5) 0.79033(5) 0.46550(5) 0.01906(15) Uani 1 1 d .
O1 O 0.96185(14) 0.61979(13) 0.71593(14) 0.0220(5) Uani 1 1 d .
O2 O 0.88010(14) 0.50734(13) 0.85986(14) 0.0225(5) Uani 1 1 d .
O3 O 0.79767(13) 0.66024(12) 0.75083(13) 0.0189(4) Uani 1 1 d .
O4 O 0.72437(14) 0.81084(13) 0.77195(13) 0.0215(4) Uani 1 1 d .
H4 H 0.7754 0.7786 0.8130 0.026 Uiso 1 1 d R
O5 O 0.78174(14) 0.51057(13) 0.66346(13) 0.0204(4) Uani 1 1 d .
O6 O 0.63085(15) 0.48686(14) 0.54197(15) 0.0276(5) Uani 1 1 d .
O7 O 0.75145(17) 0.56950(14) 0.51649(16) 0.0292(5) Uani 1 1 d .
O8 O 0.48514(14) 0.82777(13) 0.40034(14) 0.0231(5) Uani 1 1 d .
O9 O 0.41052(14) 0.85364(14) 0.50528(14) 0.0246(5) Uani 1 1 d .
O10 O 0.38833(14) 0.71913(13) 0.42411(14) 0.0242(5) Uani 1 1 d .
O11 O 0.95342(15) 0.43379(12) 0.72649(15) 0.0243(5) Uani 1 1 d .
H11A H 0.9048 0.4082 0.6753 0.029 Uiso 1 1 d R
H11B H 0.9976 0.4374 0.6995 0.029 Uiso 1 1 d R
O12 O 1.07851(14) 0.52205(14) 0.87451(14) 0.0252(5) Uani 1 1 d .
H12A H 1.1046 0.5167 0.9293 0.030 Uiso 1 1 d R
H12B H 1.1368 0.5345 0.8642 0.030 Uiso 1 1 d R
O13 O 0.13850(14) 0.86306(13) 0.34312(14) 0.0242(5) Uani 1 1 d .
O14 O -0.22046(15) 1.05182(13) 0.20988(15) 0.0227(5) Uani 1 1 d .
O15 O 0.26034(14) 1.03709(14) 0.46409(14) 0.0232(5) Uani 1 1 d .
O16 O -0.11129(14) 1.22403(13) 0.33155(14) 0.0233(5) Uani 1 1 d .
O17 O 0.29041(15) 1.07842(13) 0.68040(15) 0.0240(5) Uani 1 1 d .
O18 O -0.06797(14) 1.29683(15) 0.57158(15) 0.0271(5) Uani 1 1 d .
O19 O 0.25482(16) 0.73877(16) 0.50564(16) 0.0347(6) Uani 1 1 d .
H19A H 0.2848 0.7115 0.4801 0.042 Uiso 1 1 d R
H19B H 0.1915 0.7149 0.4760 0.042 Uiso 1 1 d R
O20 O 0.2053(2) 0.90520(19) 0.60139(19) 0.0507(7) Uani 1 1 d .
H20A H 0.2101 0.9392 0.6387 0.061 Uiso 1 1 d R
H20B H 0.1839 0.8690 0.6248 0.061 Uiso 1 1 d R
O21 O 0.89476(16) 0.46832(15) 0.49349(15) 0.0305(5) Uani 1 1 d .
H21A H 0.8497 0.4945 0.4959 0.037 Uiso 1 1 d R
H21B H 0.8960 0.4168 0.5141 0.037 Uiso 1 1 d R
O22 O 1.08086(16) 0.45407(15) 0.65753(16) 0.0303(5) Uani 1 1 d .
H22A H 1.1411 0.4758 0.6815 0.036 Uiso 1 1 d R
H22B H 1.0613 0.4745 0.6120 0.036 Uiso 1 1 d R
N1 N -0.01138(17) 0.85181(16) 0.23231(16) 0.0198(5) Uani 1 1 d .
N2 N 0.06710(16) 0.97187(16) 0.24450(16) 0.0191(5) Uani 1 1 d .
N3 N -0.08102(17) 1.04946(15) 0.19036(17) 0.0188(5) Uani 1 1 d .
N4 N -0.16052(17) 0.92992(14) 0.17475(17) 0.0180(5) Uani 1 1 d .
N5 N 0.14537(17) 1.09314(16) 0.33448(16) 0.0193(5) Uani 1 1 d .
N6 N 0.20345(16) 1.17407(15) 0.45619(16) 0.0180(5) Uani 1 1 d .
N7 N 0.04987(16) 1.24167(15) 0.40900(16) 0.0173(5) Uani 1 1 d .
N8 N -0.00265(16) 1.17171(15) 0.27978(16) 0.0187(5) Uani 1 1 d .
N9 N 0.22829(16) 1.20527(15) 0.61140(16) 0.0186(5) Uani 1 1 d .
N10 N 0.20489(16) 1.16630(15) 0.73243(16) 0.0179(5) Uani 1 1 d .
N11 N 0.06595(17) 1.25641(16) 0.69308(17) 0.0204(5) Uani 1 1 d .
N12 N 0.07496(16) 1.27757(16) 0.56103(16) 0.0191(5) Uani 1 1 d .
C1 C 0.71734(19) 0.68446(18) 0.68604(18) 0.0159(6) Uani 1 1 d .
C2 C 0.67960(19) 0.76416(18) 0.69558(18) 0.0172(6) Uani 1 1 d .
C3 C 0.60003(19) 0.79695(18) 0.62894(19) 0.0180(6) Uani 1 1 d .
H3 H 0.5793 0.8510 0.6345 0.022 Uiso 1 1 calc R
C4 C 0.55081(19) 0.74802(18) 0.55268(18) 0.0174(6) Uani 1 1 d .
C5 C 0.5816(2) 0.66830(18) 0.54316(18) 0.0178(6) Uani 1 1 d .
H5 H 0.5462 0.6350 0.4940 0.021 Uiso 1 1 calc R
C6 C 0.6667(2) 0.63763(18) 0.60790(19) 0.0176(6) Uani 1 1 d .
C7 C 0.0716(2) 0.89302(19) 0.28043(19) 0.0190(6) Uani 1 1 d .
C8 C -0.0769(2) 0.90373(18) 0.16091(19) 0.0179(6) Uani 1 1 d .
H8 H -0.0932 0.8778 0.1016 0.022 Uiso 1 1 calc R
C9 C -0.0217(2) 0.98837(18) 0.16980(19) 0.0180(6) Uani 1 1 d .
H9 H -0.0133 1.0026 0.1144 0.022 Uiso 1 1 calc R
C10 C -0.1597(2) 1.01404(19) 0.19380(18) 0.0192(6) Uani 1 1 d .
C11 C 0.14668(19) 1.02797(19) 0.27214(19) 0.0188(6) Uani 1 1 d .
H11C H 0.1490 1.0547 0.2190 0.023 Uiso 1 1 calc R
H11D H 0.2038 0.9949 0.3001 0.023 Uiso 1 1 calc R
C12 C -0.0681(2) 1.13992(18) 0.1941(2) 0.0206(6) Uani 1 1 d .
H12C H -0.1288 1.1667 0.1800 0.025 Uiso 1 1 calc R
H12D H -0.0462 1.1564 0.1479 0.025 Uiso 1 1 calc R
C13 C 0.2081(2) 1.09546(19) 0.4230(2) 0.0190(6) Uani 1 1 d .
C14 C 0.09861(19) 1.17353(18) 0.30509(19) 0.0179(6) Uani 1 1 d .
H14 H 0.1149 1.1990 0.2579 0.021 Uiso 1 1 calc R
C15 C 0.13398(19) 1.22785(18) 0.39169(18) 0.0165(6) Uani 1 1 d .
H15 H 0.1616 1.2812 0.3832 0.020 Uiso 1 1 calc R
C16 C -0.0302(2) 1.21301(18) 0.33909(19) 0.0189(6) Uani 1 1 d .
C17 C 0.26717(19) 1.20441(19) 0.54333(18) 0.0188(6) Uani 1 1 d .
H17A H 0.2866 1.2613 0.5364 0.023 Uiso 1 1 calc R
H17B H 0.3231 1.1691 0.5643 0.023 Uiso 1 1 calc R
C18 C 0.0457(2) 1.30772(19) 0.46948(18) 0.0195(6) Uani 1 1 d .
H18A H 0.0861 1.3541 0.4681 0.023 Uiso 1 1 calc R
H18B H -0.0183 1.3290 0.4489 0.023 Uiso 1 1 calc R
C19 C 0.2455(2) 1.14374(18) 0.67505(19) 0.0187(6) Uani 1 1 d .
C20 C 0.17381(19) 1.27438(18) 0.62418(19) 0.0179(6) Uani 1 1 d .
H20 H 0.2054 1.3288 0.6279 0.022 Uiso 1 1 calc R
C21 C 0.1661(2) 1.25143(18) 0.71450(19) 0.0190(6) Uani 1 1 d .
H21 H 0.2020 1.2907 0.7628 0.023 Uiso 1 1 calc R
C22 C 0.0163(2) 1.27769(18) 0.6051(2) 0.0206(6) Uani 1 1 d .
C23 C 0.23128(19) 1.12703(19) 0.82056(19) 0.0190(6) Uani 1 1 d .
H23A H 0.2897 1.0961 0.8350 0.023 Uiso 1 1 calc R
H23B H 0.2426 1.1709 0.8655 0.023 Uiso 1 1 calc R
C24 C 0.0234(2) 1.23708(19) 0.7556(2) 0.0221(6) Uani 1 1 d .
H24A H -0.0378 1.2642 0.7349 0.027 Uiso 1 1 calc R
H24B H 0.0621 1.2613 0.8137 0.027 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'
Na Na 0.0362 0.0249 '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'
S S 0.1246 0.1234 '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
O2 U O1 175.96(9) . .
O2 U O3 93.85(9) . .
O1 U O3 90.10(9) . .
O2 U O5 87.67(8) . .
O1 U O5 94.44(8) . .
O3 U O5 71.04(7) . .
O2 U O8 90.62(8) . 4_676
O1 U O8 89.35(9) . 4_676
O3 U O8 78.21(7) . 4_676
O5 U O8 149.00(7) . 4_676
O2 U O12 89.32(9) . .
O1 U O12 86.80(9) . .
O3 U O12 151.50(7) . .
O5 U O12 137.44(7) . .
O8 U O12 73.43(7) 4_676 .
O2 U O11 90.40(9) . .
O1 U O11 87.20(9) . .
O3 U O11 138.68(7) . .
O5 U O11 68.10(7) . .
O8 U O11 142.89(7) 4_676 .
O12 U O11 69.49(7) . .
O20 Na O13 117.04(11) . .
O20 Na O9 123.87(11) . .
O13 Na O9 116.51(10) . .
O20 Na O19 89.21(11) . .
O13 Na O19 86.04(9) . .
O9 Na O19 78.83(9) . .
O20 Na O15 92.31(10) . .
O13 Na O15 95.05(8) . .
O9 Na O15 98.65(9) . .
O19 Na O15 177.48(10) . .
O6 S1 O7 114.67(14) . .
O6 S1 O5 111.45(13) . .
O7 S1 O5 111.01(13) . .
O6 S1 C6 107.19(14) . .
O7 S1 C6 105.44(13) . .
O5 S1 C6 106.49(13) . .
O9 S2 O10 115.27(13) . .
O9 S2 O8 111.98(13) . .
O10 S2 O8 109.81(13) . .
O9 S2 C4 107.53(13) . .
O10 S2 C4 106.43(13) . .
O8 S2 C4 105.14(13) . .
C1 O3 U 143.64(18) . .
C2 O4 H4 108.9 . .
S1 O5 U 136.53(12) . .
S2 O8 U 130.49(12) . 4_575
S2 O9 Na 132.87(13) . .
U O11 H11A 118.4 . .
U O11 H11B 116.7 . .
H11A O11 H11B 95.1 . .
U O12 H12A 128.0 . .
U O12 H12B 129.0 . .
H12A O12 H12B 96.3 . .
C7 O13 Na 145.5(2) . .
C13 O15 Na 139.5(2) . .
Na O19 H19A 114.0 . .
Na O19 H19B 111.4 . .
H19A O19 H19B 101.4 . .
Na O20 H20A 137.9 . .
Na O20 H20B 127.7 . .
H20A O20 H20B 93.3 . .
H21A O21 H21B 109.9 . .
H22A O22 H22B 101.4 . .
C7 N1 C24 121.9(2) . 3_576
C7 N1 C8 112.5(2) . .
C24 N1 C8 125.0(2) 3_576 .
C7 N2 C11 122.6(2) . .
C7 N2 C9 113.0(2) . .
C11 N2 C9 124.0(2) . .
C10 N3 C12 121.2(3) . .
C10 N3 C9 112.8(2) . .
C12 N3 C9 125.4(3) . .
C10 N4 C23 122.5(3) . 3_576
C10 N4 C8 112.5(2) . .
C23 N4 C8 124.6(2) 3_576 .
C13 N5 C14 111.9(2) . .
C13 N5 C11 123.0(2) . .
C14 N5 C11 122.7(2) . .
C13 N6 C15 113.1(2) . .
C13 N6 C17 124.3(2) . .
C15 N6 C17 122.3(2) . .
C16 N7 C15 112.0(2) . .
C16 N7 C18 121.6(2) . .
C15 N7 C18 121.4(2) . .
C16 N8 C12 123.2(2) . .
C16 N8 C14 113.2(2) . .
C12 N8 C14 123.0(2) . .
C19 N9 C20 112.6(2) . .
C19 N9 C17 123.4(2) . .
C20 N9 C17 123.8(2) . .
C19 N10 C21 111.9(2) . .
C19 N10 C23 122.0(2) . .
C21 N10 C23 121.6(2) . .
C22 N11 C24 124.0(2) . .
C22 N11 C21 111.7(2) . .
C24 N11 C21 124.2(2) . .
C22 N12 C18 122.2(2) . .
C22 N12 C20 111.3(2) . .
C18 N12 C20 122.9(2) . .
O3 C1 C6 124.9(3) . .
O3 C1 C2 117.8(2) . .
C6 C1 C2 117.3(2) . .
O4 C2 C3 118.6(3) . .
O4 C2 C1 119.6(2) . .
C3 C2 C1 121.8(3) . .
C2 C3 C4 119.1(3) . .
C2 C3 H3 120.4 . .
C4 C3 H3 120.4 . .
C5 C4 C3 120.9(3) . .
C5 C4 S2 119.5(2) . .
C3 C4 S2 119.6(2) . .
C4 C5 C6 119.7(3) . .
C4 C5 H5 120.1 . .
C6 C5 H5 120.1 . .
C5 C6 C1 120.8(3) . .
C5 C6 S1 115.7(2) . .
C1 C6 S1 123.2(2) . .
O13 C7 N2 126.3(3) . .
O13 C7 N1 125.4(3) . .
N2 C7 N1 108.3(2) . .
N1 C8 N4 114.9(2) . .
N1 C8 C9 103.2(2) . .
N4 C8 C9 103.1(2) . .
N1 C8 H8 111.7 . .
N4 C8 H8 111.7 . .
C9 C8 H8 111.7 . .
N2 C9 N3 113.8(2) . .
N2 C9 C8 103.0(2) . .
N3 C9 C8 102.8(2) . .
N2 C9 H9 112.2 . .
N3 C9 H9 112.2 . .
C8 C9 H9 112.2 . .
O14 C10 N3 125.4(3) . .
O14 C10 N4 125.8(3) . .
N3 C10 N4 108.7(3) . .
N2 C11 N5 114.3(2) . .
N2 C11 H11C 108.7 . .
N5 C11 H11C 108.7 . .
N2 C11 H11D 108.7 . .
N5 C11 H11D 108.7 . .
H11C C11 H11D 107.6 . .
N3 C12 N8 114.7(2) . .
N3 C12 H12C 108.6 . .
N8 C12 H12C 108.6 . .
N3 C12 H12D 108.6 . .
N8 C12 H12D 108.6 . .
H12C C12 H12D 107.6 . .
O15 C13 N6 126.5(3) . .
O15 C13 N5 125.6(3) . .
N6 C13 N5 107.9(2) . .
N5 C14 N8 114.7(2) . .
N5 C14 C15 103.9(2) . .
N8 C14 C15 102.8(2) . .
N5 C14 H14 111.6 . .
N8 C14 H14 111.6 . .
C15 C14 H14 111.6 . .
N6 C15 N7 114.7(2) . .
N6 C15 C14 102.8(2) . .
N7 C15 C14 103.6(2) . .
N6 C15 H15 111.7 . .
N7 C15 H15 111.7 . .
C14 C15 H15 111.7 . .
O16 C16 N8 126.3(3) . .
O16 C16 N7 125.9(3) . .
N8 C16 N7 107.8(2) . .
N6 C17 N9 114.6(2) . .
N6 C17 H17A 108.6 . .
N9 C17 H17A 108.6 . .
N6 C17 H17B 108.6 . .
N9 C17 H17B 108.6 . .
H17A C17 H17B 107.6 . .
N12 C18 N7 111.9(2) . .
N12 C18 H18A 109.2 . .
N7 C18 H18A 109.2 . .
N12 C18 H18B 109.2 . .
N7 C18 H18B 109.2 . .
H18A C18 H18B 107.9 . .
O17 C19 N10 125.0(3) . .
O17 C19 N9 126.2(3) . .
N10 C19 N9 108.8(2) . .
N9 C20 N12 115.6(2) . .
N9 C20 C21 102.9(2) . .
N12 C20 C21 102.5(2) . .
N9 C20 H20 111.7 . .
N12 C20 H20 111.7 . .
C21 C20 H20 111.7 . .
N11 C21 N10 114.5(2) . .
N11 C21 C20 103.5(2) . .
N10 C21 C20 103.0(2) . .
N11 C21 H21 111.7 . .
N10 C21 H21 111.7 . .
C20 C21 H21 111.7 . .
O18 C22 N12 125.3(3) . .
O18 C22 N11 125.4(3) . .
N12 C22 N11 109.3(2) . .
N4 C23 N10 113.2(2) 3_576 .
N4 C23 H23A 108.9 3_576 .
N10 C23 H23A 108.9 . .
N4 C23 H23B 108.9 3_576 .
N10 C23 H23B 108.9 . .
H23A C23 H23B 107.8 . .
N11 C24 N1 114.9(3) . 3_576
N11 C24 H24A 108.5 . .
N1 C24 H24A 108.5 3_576 .
N11 C24 H24B 108.5 . .
N1 C24 H24B 108.5 3_576 .
H24A C24 H24B 107.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U O2 1.768(2) .
U O1 1.769(2) .
U O3 2.2686(19) .
U O5 2.4068(19) .
U O8 2.412(2) 4_676
U O12 2.430(2) .
U O11 2.455(2) .
Na O20 2.308(3) .
Na O13 2.312(2) .
Na O9 2.368(2) .
Na O19 2.384(3) .
Na O15 2.393(2) .
S1 O6 1.441(2) .
S1 O7 1.458(2) .
S1 O5 1.476(2) .
S1 C6 1.759(3) .
S2 O9 1.448(2) .
S2 O10 1.456(2) .
S2 O8 1.486(2) .
S2 C4 1.768(3) .
O3 C1 1.325(3) .
O4 C2 1.368(3) .
O4 H4 0.9527 .
O8 U 2.412(2) 4_575
O11 H11A 0.9598 .
O11 H11B 0.9463 .
O12 H12A 0.8197 .
O12 H12B 0.9980 .
O13 C7 1.221(3) .
O14 C10 1.224(4) .
O15 C13 1.234(4) .
O16 C16 1.222(4) .
O17 C19 1.229(3) .
O18 C22 1.234(3) .
O19 H19A 0.8499 .
O19 H19B 0.9790 .
O20 H20A 0.7893 .
O20 H20B 0.8234 .
O21 H21A 0.8247 .
O21 H21B 0.8785 .
O22 H22A 0.9218 .
O22 H22B 0.7501 .
N1 C7 1.374(4) .
N1 C24 1.443(4) 3_576
N1 C8 1.452(4) .
N2 C7 1.367(4) .
N2 C11 1.437(4) .
N2 C9 1.449(3) .
N3 C10 1.360(4) .
N3 C12 1.444(4) .
N3 C9 1.458(4) .
N4 C10 1.366(4) .
N4 C23 1.442(4) 3_576
N4 C8 1.456(4) .
N5 C13 1.375(4) .
N5 C14 1.448(4) .
N5 C11 1.448(4) .
N6 C13 1.368(4) .
N6 C15 1.442(3) .
N6 C17 1.444(3) .
N7 C16 1.381(4) .
N7 C15 1.450(4) .
N7 C18 1.450(4) .
N8 C16 1.360(4) .
N8 C12 1.444(4) .
N8 C14 1.452(4) .
N9 C19 1.364(4) .
N9 C20 1.444(4) .
N9 C17 1.447(4) .
N10 C19 1.357(4) .
N10 C21 1.456(4) .
N10 C23 1.457(4) .
N11 C22 1.364(4) .
N11 C24 1.439(4) .
N11 C21 1.448(4) .
N12 C22 1.356(4) .
N12 C18 1.446(4) .
N12 C20 1.464(3) .
C1 C6 1.405(4) .
C1 C2 1.423(4) .
C2 C3 1.376(4) .
C3 C4 1.398(4) .
C3 H3 0.9300 .
C4 C5 1.379(4) .
C5 C6 1.403(4) .
C5 H5 0.9300 .
C8 C9 1.563(4) .
C8 H8 0.9800 .
C9 H9 0.9800 .
C11 H11C 0.9700 .
C11 H11D 0.9700 .
C12 H12C 0.9700 .
C12 H12D 0.9700 .
C14 C15 1.546(4) .
C14 H14 0.9800 .
C15 H15 0.9800 .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C20 C21 1.554(4) .
C20 H20 0.9800 .
C21 H21 0.9800 .
C23 N4 1.442(4) 3_576
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C24 N1 1.443(4) 3_576
C24 H24A 0.9700 .
C24 H24B 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
O4 H4 O10 0.95 1.95 2.786(3) 145.6 4_676
O11 H11A O18 0.96 2.58 3.228(3) 125.1 1_645
O11 H11B O22 0.95 1.69 2.637(3) 173.6 .
O12 H12A O15 0.82 2.14 2.815(3) 139.5 2_646
O12 H12B O17 1.00 1.70 2.665(3) 160.2 2_646
O19 H19A O10 0.85 2.13 2.869(3) 145.3 .
O19 H19B O18 0.98 1.76 2.712(3) 162.6 3_576
O20 H20A O14 0.79 2.39 3.042(3) 140.3 3_576
O20 H20B O16 0.82 2.13 2.951(4) 171.9 3_576
O21 H21A O7 0.82 2.05 2.873(3) 171.8 .
O21 H21B O18 0.88 2.09 2.953(3) 166.9 1_645
O22 H22A O14 0.92 2.05 2.844(3) 143.6 4_776
O22 H22B O21 0.75 2.26 2.887(3) 142.1 3_766
