#------------------------------------------------------------------------------
#$Date: 2018-10-05 14:19:55 +0200 (vie 05 de oct de 2018) $
#$Revision: 211332 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/28/7012880.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_7012880
loop_
_publ_author_name
'Pierre Thuéry'
'Bernardo Masci'
_publ_section_title
;
 Synthesis and crystal structure of 1:2 mixed uranyl/alkali metal ions
 (Li+, Na+, K+, Cs+) complexes of
 p-tert-butyltetrahomodioxacalix[4]arene
;
_journal_issue                   12
_journal_name_full               'Dalton Trans.'
_journal_page_first              2411
_journal_page_last               2417
_journal_paper_doi               10.1039/b302233a
_journal_year                    2003
_chemical_formula_sum            'C54 H90 Na2 O17 U'
_chemical_formula_weight         1295.27
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.961(6)
_cell_angle_beta                 106.010(6)
_cell_angle_gamma                93.142(4)
_cell_formula_units_Z            2
_cell_length_a                   12.5111(12)
_cell_length_b                   15.2227(15)
_cell_length_c                   16.7853(11)
_cell_measurement_reflns_used    19838
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.94
_cell_volume                     3028.6(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, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_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  0.0830
_diffrn_reflns_av_sigmaI/netI    0.1136
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19838
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    2.758
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.430
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.242
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         10421
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0705
_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)+(0.1251P)²+0.9778P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1755
_refine_ls_wR_factor_ref         0.1917
_reflns_number_gt                8180
_reflns_number_total             10421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302233a.txt
_cod_data_source_block           2
_cod_database_code               7012880
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
U U 0.72544(3) 0.68655(2) 0.69226(2) 0.03126(14) Uani 1 1 d . . .
Na1 Na 0.5997(4) 0.5425(3) 0.4556(3) 0.0504(10) Uani 1 1 d . . .
Na2 Na 0.9130(5) 0.8953(4) 0.8247(3) 0.0744(15) Uani 1 1 d . . .
O1 O 0.5490(5) 0.7278(4) 0.6407(4) 0.0398(15) Uani 1 1 d . . .
O2 O 0.7683(5) 0.7718(4) 0.6016(4) 0.0339(13) Uani 1 1 d . . .
O3 O 1.0025(5) 0.8220(4) 0.7237(4) 0.0373(14) Uani 1 1 d . . .
O4 O 0.8985(5) 0.6382(5) 0.7343(4) 0.0387(15) Uani 1 1 d . . .
O5 O 0.6756(5) 0.5940(4) 0.7740(4) 0.0340(14) Uani 1 1 d . . .
O6 O 0.5145(5) 0.7246(4) 0.8146(4) 0.0365(14) Uani 1 1 d . . .
O7 O 0.6892(5) 0.5939(4) 0.6062(4) 0.0378(14) Uani 1 1 d . . .
O8 O 0.7636(5) 0.7791(4) 0.7775(4) 0.0359(14) Uani 1 1 d . . .
C1 C 0.4379(7) 0.8149(6) 0.7109(6) 0.035(2) Uani 1 1 d . . .
C2 C 0.5056(7) 0.8058(6) 0.6577(6) 0.037(2) Uani 1 1 d . . .
C3 C 0.5196(7) 0.8770(6) 0.6126(6) 0.036(2) Uani 1 1 d . . .
C4 C 0.4775(8) 0.9578(6) 0.6357(6) 0.037(2) Uani 1 1 d . . .
H4 H 0.4901 1.0059 0.6096 0.044 Uiso 1 1 calc R . .
C5 C 0.4193(8) 0.9703(6) 0.6941(6) 0.037(2) Uani 1 1 d . . .
C6 C 0.3971(8) 0.8950(7) 0.7292(6) 0.041(2) Uani 1 1 d . . .
H6 H 0.3534 0.8996 0.7660 0.049 Uiso 1 1 calc R . .
C7 C 0.3769(8) 1.0602(7) 0.7192(7) 0.042(2) Uani 1 1 d . . .
C8 C 0.4059(11) 1.0810(8) 0.8158(7) 0.060(3) Uani 1 1 d . . .
H8A H 0.3973 1.1425 0.8325 0.089 Uiso 1 1 calc R . .
H8B H 0.4818 1.0696 0.8401 0.089 Uiso 1 1 calc R . .
H8C H 0.3567 1.0439 0.8349 0.089 Uiso 1 1 calc R . .
C9 C 0.4319(11) 1.1374(8) 0.6909(8) 0.060(3) Uani 1 1 d . . .
H9A H 0.4083 1.1306 0.6307 0.089 Uiso 1 1 calc R . .
H9B H 0.5117 1.1376 0.7101 0.089 Uiso 1 1 calc R . .
H9C H 0.4105 1.1927 0.7139 0.089 Uiso 1 1 calc R . .
C10 C 0.2517(10) 1.0549(8) 0.6786(8) 0.056(3) Uani 1 1 d . . .
H10A H 0.2230 1.1074 0.7003 0.083 Uiso 1 1 calc R . .
H10B H 0.2160 1.0031 0.6910 0.083 Uiso 1 1 calc R . .
H10C H 0.2370 1.0508 0.6189 0.083 Uiso 1 1 calc R . .
C11 C 0.5773(7) 0.8688(6) 0.5454(6) 0.035(2) Uani 1 1 d . . .
H11A H 0.5345 0.8956 0.4990 0.042 Uiso 1 1 calc R . .
H11B H 0.5770 0.8060 0.5248 0.042 Uiso 1 1 calc R . .
C12 C 0.6954(7) 0.9106(6) 0.5713(5) 0.0338(19) Uani 1 1 d . . .
C13 C 0.7854(8) 0.8585(6) 0.5999(5) 0.034(2) Uani 1 1 d . . .
C14 C 0.8961(8) 0.9008(7) 0.6200(6) 0.039(2) Uani 1 1 d . . .
C15 C 0.9140(9) 0.9916(7) 0.6166(7) 0.044(2) Uani 1 1 d . . .
H15 H 0.9869 1.0179 0.6302 0.053 Uiso 1 1 calc R . .
C16 C 0.8270(8) 1.0430(6) 0.5937(6) 0.040(2) Uani 1 1 d . . .
C17 C 0.7180(8) 1.0008(6) 0.5694(6) 0.037(2) Uani 1 1 d . . .
H17 H 0.6586 1.0343 0.5515 0.045 Uiso 1 1 calc R . .
C18 C 0.8491(8) 1.1451(6) 0.5945(6) 0.048(3) Uani 1 1 d D . .
C19A C 0.7984(15) 1.1981(12) 0.6552(11) 0.059(5) Uiso 0.67(2) 1 d PD . .
C20A C 0.8014(14) 1.1631(11) 0.5044(8) 0.050(4) Uiso 0.67(2) 1 d PD . .
C21A C 0.9738(10) 1.1765(12) 0.6159(11) 0.057(5) Uiso 0.67(2) 1 d PD . .
C19B C 0.742(3) 1.190(3) 0.589(4) 0.092(16) Uiso 0.33(2) 1 d PD . .
C20B C 0.900(4) 1.158(4) 0.524(2) 0.087(15) Uiso 0.33(2) 1 d PD . .
C21B C 0.912(3) 1.189(3) 0.6833(13) 0.071(12) Uiso 0.33(2) 1 d PD . .
C22 C 0.9910(7) 0.8457(7) 0.6422(6) 0.037(2) Uani 1 1 d . . .
H22A H 0.9781 0.7921 0.6008 0.045 Uiso 1 1 calc R . .
H22B H 1.0594 0.8789 0.6420 0.045 Uiso 1 1 calc R . .
C23 C 1.0825(8) 0.7576(7) 0.7395(6) 0.040(2) Uani 1 1 d . . .
H23A H 1.1575 0.7859 0.7502 0.048 Uiso 1 1 calc R . .
H23B H 1.0678 0.7110 0.6911 0.048 Uiso 1 1 calc R . .
C24 C 1.0717(8) 0.7187(7) 0.8148(6) 0.042(2) Uani 1 1 d . . .
C25 C 0.9824(7) 0.6585(6) 0.8080(6) 0.0343(19) Uani 1 1 d . . .
C26 C 0.9798(7) 0.6163(7) 0.8764(6) 0.037(2) Uani 1 1 d . . .
C27 C 1.0636(9) 0.6402(7) 0.9505(6) 0.044(2) Uani 1 1 d . . .
H27 H 1.0606 0.6119 0.9956 0.053 Uiso 1 1 calc R . .
C28 C 1.1506(9) 0.7029(7) 0.9619(7) 0.047(2) Uani 1 1 d . . .
C29 C 1.1563(8) 0.7411(7) 0.8914(7) 0.046(2) Uani 1 1 d . . .
H29 H 1.2166 0.7818 0.8956 0.055 Uiso 1 1 calc R . .
C30 C 1.2429(10) 0.7328(8) 1.0468(7) 0.056(3) Uani 1 1 d . . .
C31 C 1.2512(14) 0.8352(11) 1.0721(10) 0.086(4) Uani 1 1 d U . .
H31A H 1.3121 0.8536 1.1221 0.129 Uiso 1 1 calc R . .
H31B H 1.1828 0.8519 1.0825 0.129 Uiso 1 1 calc R . .
H31C H 1.2639 0.8636 1.0275 0.129 Uiso 1 1 calc R . .
C32 C 1.3530(13) 0.7007(12) 1.0408(10) 0.083(4) Uani 1 1 d U . .
H32A H 1.4115 0.7272 1.0899 0.124 Uiso 1 1 calc R . .
H32B H 1.3689 0.7173 0.9918 0.124 Uiso 1 1 calc R . .
H32C H 1.3487 0.6370 1.0368 0.124 Uiso 1 1 calc R . .
C33 C 1.2133(13) 0.6992(11) 1.1181(9) 0.077(4) Uani 1 1 d U . .
H33A H 1.1827 0.6381 1.1010 0.116 Uiso 1 1 calc R . .
H33B H 1.1590 0.7343 1.1343 0.116 Uiso 1 1 calc R . .
H33C H 1.2791 0.7036 1.1649 0.116 Uiso 1 1 calc R . .
C34 C 0.8868(8) 0.5421(7) 0.8696(6) 0.039(2) Uani 1 1 d . . .
H34A H 0.8531 0.5178 0.8108 0.047 Uiso 1 1 calc R . .
H34B H 0.9203 0.4945 0.8975 0.047 Uiso 1 1 calc R . .
C35 C 0.7960(8) 0.5734(7) 0.9074(6) 0.039(2) Uani 1 1 d . . .
C36 C 0.6952(8) 0.5978(6) 0.8589(6) 0.036(2) Uani 1 1 d . . .
C37 C 0.6137(8) 0.6213(6) 0.8980(7) 0.040(2) Uani 1 1 d . . .
C38 C 0.6345(9) 0.6239(7) 0.9824(7) 0.047(2) Uani 1 1 d . . .
H38 H 0.5786 0.6411 1.0063 0.056 Uiso 1 1 calc R . .
C39 C 0.7322(9) 0.6028(7) 1.0349(5) 0.053(3) Uani 1 1 d D . .
C40 C 0.8135(9) 0.5763(7) 0.9943(6) 0.046(2) Uani 1 1 d . . .
H40 H 0.8807 0.5602 1.0262 0.055 Uiso 1 1 calc R . .
C41 C 0.7531(8) 0.6068(6) 1.1299(6) 0.058(3) Uani 1 1 d DU . .
C42A C 0.7782(18) 0.5137(9) 1.1516(10) 0.068(6) Uiso 0.532(17) 1 d PDU . .
C43A C 0.6432(13) 0.6261(15) 1.1512(11) 0.085(7) Uiso 0.532(17) 1 d PDU . .
C44A C 0.8451(14) 0.6755(12) 1.1793(9) 0.076(7) Uiso 0.532(17) 1 d PDU . .
C42B C 0.698(2) 0.5265(12) 1.1492(12) 0.084(8) Uiso 0.468(17) 1 d PDU . .
C43B C 0.711(2) 0.6926(11) 1.1642(11) 0.077(7) Uiso 0.468(17) 1 d PDU . .
C44B C 0.8807(10) 0.6134(17) 1.1704(11) 0.082(7) Uiso 0.468(17) 1 d PDU . .
C45 C 0.5016(8) 0.6411(6) 0.8437(6) 0.037(2) Uani 1 1 d . . .
H45A H 0.4736 0.5937 0.7961 0.045 Uiso 1 1 calc R . .
H45B H 0.4482 0.6442 0.8761 0.045 Uiso 1 1 calc R . .
C46 C 0.4167(8) 0.7350(7) 0.7510(7) 0.044(2) Uani 1 1 d . . .
H46A H 0.3552 0.7436 0.7750 0.052 Uiso 1 1 calc R . .
H46B H 0.3966 0.6818 0.7088 0.052 Uiso 1 1 calc R . .
O9 O 0.4511(7) 0.5992(5) 0.5063(5) 0.0535(19) Uani 1 1 d . . .
O10 O 0.4923(7) 0.5321(6) 0.3181(5) 0.060(2) Uani 1 1 d . . .
O11 O 0.7670(10) 0.4767(8) 0.4626(7) 0.105(4) Uani 1 1 d D . .
O12 O 0.6922(7) 0.6796(5) 0.4436(5) 0.0558(19) Uani 1 1 d . . .
O13 O 0.8667(7) 0.8954(6) 0.9574(6) 0.068(2) Uani 1 1 d . . .
O14 O 1.0720(9) 0.9792(7) 0.8997(6) 0.082(3) Uani 1 1 d U . .
O15 O 0.7510(10) 0.9861(7) 0.7868(6) 0.088(3) Uani 1 1 d U . .
O16 O 0.6473(8) 0.8776(7) 0.8966(6) 0.078(3) Uani 1 1 d DU . .
O17 O 0.9312(8) 0.5224(6) 0.6075(6) 0.071(3) Uani 1 1 d D . .
C47 C 0.3664(18) 0.6304(15) 0.4472(13) 0.116(7) Uani 1 1 d U . .
H47A H 0.3114 0.6519 0.4732 0.173 Uiso 1 1 calc R . .
H47B H 0.3321 0.5828 0.4019 0.173 Uiso 1 1 calc R . .
H47C H 0.3974 0.6780 0.4259 0.173 Uiso 1 1 calc R . .
C48 C 0.4632(17) 0.6062(13) 0.2804(12) 0.102(5) Uani 1 1 d U . .
H48A H 0.4189 0.5873 0.2233 0.153 Uiso 1 1 calc R . .
H48B H 0.5296 0.6415 0.2814 0.153 Uiso 1 1 calc R . .
H48C H 0.4208 0.6410 0.3105 0.153 Uiso 1 1 calc R . .
C49A C 0.8117(15) 0.4213(12) 0.4075(10) 0.072(5) Uani 0.79(3) 1 d PDU . .
C49B C 0.8795(18) 0.513(3) 0.484(3) 0.045(14) Uani 0.21(3) 1 d PDU . .
C50 C 0.7849(12) 0.6841(10) 0.4126(9) 0.071(4) Uani 1 1 d U . .
H50A H 0.8089 0.7453 0.4136 0.106 Uiso 1 1 calc R . .
H50B H 0.7649 0.6530 0.3560 0.106 Uiso 1 1 calc R . .
H50C H 0.8445 0.6570 0.4470 0.106 Uiso 1 1 calc R . .
C51 C 0.8942(12) 0.8134(9) 0.9839(9) 0.069(3) Uani 1 1 d U . .
H51A H 0.8768 0.8105 1.0358 0.104 Uiso 1 1 calc R . .
H51B H 0.9726 0.8087 0.9920 0.104 Uiso 1 1 calc R . .
H51C H 0.8519 0.7653 0.9419 0.104 Uiso 1 1 calc R . .
C52 C 1.1587(16) 0.9970(14) 0.8658(12) 0.099(5) Uani 1 1 d U . .
H52A H 1.2187 1.0333 0.9079 0.149 Uiso 1 1 calc R . .
H52B H 1.1325 1.0280 0.8192 0.149 Uiso 1 1 calc R . .
H52C H 1.1849 0.9420 0.8471 0.149 Uiso 1 1 calc R . .
C53 C 0.5833(11) 0.9079(11) 0.9516(9) 0.078(4) Uani 1 1 d D . .
H53A H 0.5670 0.8601 0.9794 0.117 Uiso 1 1 calc R . .
H53B H 0.5148 0.9265 0.9193 0.117 Uiso 1 1 calc R . .
H53C H 0.6252 0.9569 0.9922 0.117 Uiso 1 1 calc R . .
C54 C 0.9611(14) 0.4469(9) 0.6477(10) 0.084(4) Uani 1 1 d DU . .
H54A H 0.9307 0.4479 0.6939 0.126 Uiso 1 1 calc R . .
H54B H 1.0410 0.4489 0.6668 0.126 Uiso 1 1 calc R . .
H54C H 0.9318 0.3936 0.6077 0.126 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'
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'
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
O8 U O7 179.0(3) . . ?
O8 U O5 92.3(3) . . ?
O7 U O5 88.4(3) . . ?
O8 U O2 91.9(3) . . ?
O7 U O2 87.4(3) . . ?
O5 U O2 175.7(2) . . ?
O8 U O4 91.1(3) . . ?
O7 U O4 88.2(3) . . ?
O5 U O4 85.9(2) . . ?
O2 U O4 95.2(2) . . ?
O8 U O1 93.1(3) . . ?
O7 U O1 87.5(3) . . ?
O5 U O1 94.9(2) . . ?
O2 U O1 83.7(2) . . ?
O4 U O1 175.7(2) . . ?
O10 Na1 O11 110.7(4) . . ?
O10 Na1 O12 89.3(3) . . ?
O11 Na1 O12 88.5(4) . . ?
O10 Na1 O9 91.4(3) . . ?
O11 Na1 O9 156.6(4) . . ?
O12 Na1 O9 99.6(3) . . ?
O10 Na1 O9 103.2(3) . 2_666 ?
O11 Na1 O9 81.0(4) . 2_666 ?
O12 Na1 O9 165.8(3) . 2_666 ?
O9 Na1 O9 86.7(3) . 2_666 ?
O10 Na1 O7 163.5(3) . . ?
O11 Na1 O7 83.3(3) . . ?
O12 Na1 O7 82.3(3) . . ?
O9 Na1 O7 76.2(3) . . ?
O9 Na1 O7 87.0(3) 2_666 . ?
O14 Na2 O8 162.6(5) . . ?
O14 Na2 O13 87.1(4) . . ?
O8 Na2 O13 81.9(3) . . ?
O14 Na2 O3 92.6(3) . . ?
O8 Na2 O3 89.5(3) . . ?
O13 Na2 O3 147.5(4) . . ?
O14 Na2 O15 112.5(5) . . ?
O8 Na2 O15 80.2(3) . . ?
O13 Na2 O15 85.1(4) . . ?
O3 Na2 O15 124.3(4) . . ?
C23 O3 C22 109.8(7) . . ?
C23 O3 Na2 126.1(6) . . ?
C22 O3 Na2 123.7(5) . . ?
C46 O6 C45 109.8(7) . . ?
U O7 Na1 147.1(4) . . ?
U O8 Na2 133.9(3) . . ?
C6 C1 C2 120.7(9) . . ?
C6 C1 C46 122.0(8) . . ?
C2 C1 C46 117.3(9) . . ?
O1 C2 C1 121.5(8) . . ?
O1 C2 C3 119.2(9) . . ?
C1 C2 C3 119.0(9) . . ?
C4 C3 C2 116.7(9) . . ?
C4 C3 C11 120.4(8) . . ?
C2 C3 C11 122.9(9) . . ?
C5 C4 C3 124.4(9) . . ?
C4 C5 C6 116.2(9) . . ?
C4 C5 C7 122.9(9) . . ?
C6 C5 C7 120.9(9) . . ?
C1 C6 C5 122.3(9) . . ?
C10 C7 C9 108.0(10) . . ?
C10 C7 C5 109.1(9) . . ?
C9 C7 C5 112.4(8) . . ?
C10 C7 C8 111.4(9) . . ?
C9 C7 C8 107.0(9) . . ?
C5 C7 C8 109.0(9) . . ?
C3 C11 C12 115.5(8) . . ?
C17 C12 C13 119.5(8) . . ?
C17 C12 C11 120.4(8) . . ?
C13 C12 C11 120.0(8) . . ?
O2 C13 C12 121.9(8) . . ?
O2 C13 C14 120.4(9) . . ?
C12 C13 C14 117.5(8) . . ?
C15 C14 C13 120.5(9) . . ?
C15 C14 C22 121.2(8) . . ?
C13 C14 C22 118.4(9) . . ?
C16 C15 C14 122.0(9) . . ?
C15 C16 C17 117.9(9) . . ?
C15 C16 C18 121.0(9) . . ?
C17 C16 C18 121.1(8) . . ?
C12 C17 C16 122.5(9) . . ?
C20B C18 C21B 118(3) . . ?
C20B C18 C19B 113(3) . . ?
C21B C18 C19B 97(3) . . ?
C19A C18 C21A 109.6(12) . . ?
C19A C18 C20A 112.2(12) . . ?
C21A C18 C20A 103.6(11) . . ?
C19A C18 C16 110.8(10) . . ?
C20B C18 C16 109(2) . . ?
C21B C18 C16 108.7(18) . . ?
C19B C18 C16 110(2) . . ?
C21A C18 C16 112.8(10) . . ?
C20A C18 C16 107.7(10) . . ?
O3 C22 C14 110.0(7) . . ?
O3 C23 C24 107.8(8) . . ?
C25 C24 C29 120.1(10) . . ?
C25 C24 C23 120.3(8) . . ?
C29 C24 C23 119.6(9) . . ?
O4 C25 C24 120.3(8) . . ?
O4 C25 C26 120.3(8) . . ?
C24 C25 C26 119.3(9) . . ?
C27 C26 C25 118.9(9) . . ?
C27 C26 C34 119.7(9) . . ?
C25 C26 C34 121.4(8) . . ?
C28 C27 C26 124.0(10) . . ?
C27 C28 C29 116.7(10) . . ?
C27 C28 C30 124.1(10) . . ?
C29 C28 C30 119.2(10) . . ?
C28 C29 C24 120.8(10) . . ?
C33 C30 C32 109.3(11) . . ?
C33 C30 C31 102.8(12) . . ?
C32 C30 C31 112.3(12) . . ?
C33 C30 C28 112.1(11) . . ?
C32 C30 C28 110.2(11) . . ?
C31 C30 C28 110.0(10) . . ?
C35 C34 C26 113.8(8) . . ?
C40 C35 C36 119.3(9) . . ?
C40 C35 C34 118.4(8) . . ?
C36 C35 C34 122.3(9) . . ?
O5 C36 C37 121.0(9) . . ?
O5 C36 C35 120.3(8) . . ?
C37 C36 C35 118.7(9) . . ?
C38 C37 C36 120.1(9) . . ?
C38 C37 C45 121.7(9) . . ?
C36 C37 C45 118.2(9) . . ?
C37 C38 C39 124.9(10) . . ?
C38 C39 C40 114.7(8) . . ?
C38 C39 C41 123.5(8) . . ?
C40 C39 C41 121.8(8) . . ?
C35 C40 C39 122.3(9) . . ?
C42B C41 C43B 111.4(8) . . ?
C44A C41 C42A 111.2(8) . . ?
C44A C41 C39 112.2(7) . . ?
C42B C41 C39 111.3(8) . . ?
C43B C41 C39 108.3(7) . . ?
C42A C41 C39 108.3(7) . . ?
C42B C41 C44B 110.5(8) . . ?
C43B C41 C44B 107.5(8) . . ?
C39 C41 C44B 107.7(7) . . ?
C44A C41 C43A 110.4(8) . . ?
C42A C41 C43A 106.3(7) . . ?
C39 C41 C43A 108.2(7) . . ?
O6 C45 C37 109.5(7) . . ?
O6 C46 C1 109.4(8) . . ?
C47 O9 Na1 115.4(10) . . ?
C47 O9 Na1 114.8(11) . 2_666 ?
Na1 O9 Na1 93.3(3) . 2_666 ?
C48 O10 Na1 122.7(10) . . ?
C49B O11 Na1 132(2) . . ?
C49A O11 Na1 137.1(11) . . ?
C50 O12 Na1 123.3(8) . . ?
C51 O13 Na2 106.7(8) . . ?
C52 O14 Na2 122.4(10) . . ?
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
U O8 1.803(6) . ?
U O7 1.813(6) . ?
U O5 2.273(6) . ?
U O2 2.282(6) . ?
U O4 2.281(6) . ?
U O1 2.294(6) . ?
U Na2 3.859(5) . ?
U Na1 4.102(4) . ?
U U 8.4845(10) 2_666 ?
Na1 O10 2.307(9) . ?
Na1 O11 2.351(11) . ?
Na1 O12 2.390(9) . ?
Na1 O9 2.403(9) . ?
Na1 O9 2.433(9) 2_666 ?
Na1 O7 2.460(8) . ?
Na1 Na1 3.516(9) 2_666 ?
Na2 O14 2.251(11) . ?
Na2 O8 2.383(8) . ?
Na2 O13 2.451(11) . ?
Na2 O3 2.456(8) . ?
Na2 O15 2.503(13) . ?
O1 C2 1.360(12) . ?
O1 O9 2.723(10) . ?
O2 C13 1.332(11) . ?
O2 O12 2.708(10) . ?
O3 C23 1.437(11) . ?
O3 C22 1.434(11) . ?
O4 C25 1.367(11) . ?
O4 O17 2.707(11) . ?
O5 C36 1.371(11) . ?
O6 C46 1.418(11) . ?
O6 C45 1.441(11) . ?
O6 O16 2.740(11) . ?
O7 O9 3.000(10) . ?
C1 C6 1.376(14) . ?
C1 C2 1.389(14) . ?
C1 C46 1.513(13) . ?
C2 C3 1.435(13) . ?
C3 C4 1.411(14) . ?
C3 C11 1.494(13) . ?
C4 C5 1.373(13) . ?
C5 C6 1.406(14) . ?
C5 C7 1.542(14) . ?
C7 C10 1.518(15) . ?
C7 C9 1.526(15) . ?
C7 C8 1.543(15) . ?
C11 C12 1.498(12) . ?
C12 C17 1.393(14) . ?
C12 C13 1.426(13) . ?
C13 C14 1.424(13) . ?
C14 C15 1.398(15) . ?
C14 C22 1.485(13) . ?
C15 C16 1.375(15) . ?
C16 C17 1.401(14) . ?
C16 C18 1.562(13) . ?
C18 C19A 1.509(9) . ?
C18 C20B 1.521(10) . ?
C18 C21B 1.519(10) . ?
C18 C19B 1.522(10) . ?
C18 C21A 1.534(9) . ?
C18 C20A 1.534(9) . ?
C23 C24 1.502(14) . ?
C24 C25 1.375(14) . ?
C24 C29 1.407(13) . ?
C25 C26 1.398(13) . ?
C26 C27 1.377(14) . ?
C26 C34 1.545(14) . ?
C27 C28 1.361(15) . ?
C28 C29 1.406(16) . ?
C28 C30 1.558(15) . ?
C30 C33 1.491(19) . ?
C30 C32 1.512(19) . ?
C30 C31 1.55(2) . ?
C34 C35 1.516(14) . ?
C35 C40 1.407(14) . ?
C35 C36 1.399(13) . ?
C36 C37 1.394(13) . ?
C37 C38 1.363(15) . ?
C37 C45 1.518(13) . ?
C38 C39 1.379(14) . ?
C39 C40 1.419(15) . ?
C39 C41 1.535(11) . ?
C41 C44A 1.485(8) . ?
C41 C42B 1.491(9) . ?
C41 C43B 1.531(9) . ?
C41 C42A 1.539(8) . ?
C41 C44B 1.544(9) . ?
C41 C43A 1.546(8) . ?
O9 C47 1.39(2) . ?
O9 Na1 2.433(9) 2_666 ?
O9 O11 3.108(16) 2_666 ?
O10 C48 1.385(19) . ?
O10 O5 2.726(10) 2_666 ?
O11 C49B 1.413(10) . ?
O11 C49A 1.413(9) . ?
O11 O17 2.690(15) . ?
O12 C50 1.399(15) . ?
O13 C51 1.411(16) . ?
O13 O16 2.636(13) . ?
O13 O14 2.746(14) 2_777 ?
O14 C52 1.39(2) . ?
O16 C53 1.427(9) . ?
O17 C54 1.428(9) . ?
