#------------------------------------------------------------------------------
#$Date: 2023-01-06 11:34:18 +0200 (Fri, 06 Jan 2023) $
#$Revision: 280164 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/78/1567882.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_1567882
loop_
_publ_author_name
'Hanna, Sylvia L.'
'Debela, Tekalign T.'
'Mroz, Austin M.'
'Syed, Zoha H.'
'Kirlikovali, Kent O.'
'Hendon, Christopher H.'
'Farha, Omar K.'
_publ_section_title
;
 Identification of a metastable uranium metal-organic framework isomer
 through non-equilibrium synthesis.
;
_journal_issue                   44
_journal_name_full               'Chemical science'
_journal_page_first              13032
_journal_page_last               13039
_journal_paper_doi               10.1039/d2sc04783g
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C87 H48 O32 U4'
_chemical_formula_sum            'C87 H48 O32 U4'
_chemical_formula_weight         2557.37
_chemical_name_systematic        NU-1306
_space_group_crystal_system      cubic
_space_group_IT_number           215
_space_group_name_Hall           'P -4 2 3'
_space_group_name_H-M_alt        'P -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-06-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-08-26 deposited with the CCDC.	2022-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   20.90200(10)
_cell_length_b                   20.90200(10)
_cell_length_c                   20.90200(10)
_cell_measurement_reflns_used    3351
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      72
_cell_measurement_theta_min      2.1
_cell_volume                     9131.95(8)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33250
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.004
_diffrn_reflns_theta_min         2.114
_exptl_absorpt_coefficient_mu    5.098
_exptl_absorpt_correction_T_max  0.19
_exptl_absorpt_correction_T_min  0.13
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.465
_exptl_crystal_description       block
_exptl_crystal_F_000             1194
_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.117
_refine_diff_density_max         1.526
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details
;
 Flack x determined using 1325 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.027(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         3351
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1453P)²+0.3780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.1825
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                3137
_reflns_number_total             3351
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc04783g3.cif
_cod_data_source_block           NU-1306
_cod_depositor_comments          'Adding full bibliography for 1567882.cif.'
_cod_original_cell_volume        9131.95(13)
_cod_database_code               1567882
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.235
_shelx_estimated_absorpt_t_min   0.235
_olex2_refinement_description
;
1. Restrained distances
 U1-O2 = U1-O1
 1.8 with sigma of 0.001
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_smtbx_masks_void_probe_radius   5.0
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'-x, z, -y'
'x, -y, -z'
'-x, -z, y'
'-z, -y, x'
'-x, y, -z'
'z, -y, -x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.29977(3) 0.29977(3) 0.29977(3) 0.0953(4) Uani 1 6 d DS T P . .
O1 O 0.34949(5) 0.34949(5) 0.34949(5) 0.107(6) Uani 1 6 d DS T P . .
O2 O 0.25008(5) 0.25008(5) 0.25008(5) 0.127(9) Uani 1 6 d DS T P . .
O3 O 0.2149(4) 0.3800(4) 0.3069(4) 0.111(3) Uani 1 1 d . . . . .
C1 C 0.1917(7) 0.3592(6) 0.3592(6) 0.099(5) Uani 1 2 d S T P . .
C2 C 0.1414(6) 0.3916(6) 0.3916(6) 0.088(4) Uani 1 2 d S T P . .
C3 C 0.1187(5) 0.4506(5) 0.3711(5) 0.094(3) Uani 1 1 d . . . . .
H3 H 0.136464 0.469026 0.334669 0.113 Uiso 1 1 calc R U . . .
C4 C 0.0704(5) 0.4828(5) 0.4031(5) 0.091(3) Uani 1 1 d . . . . .
H4 H 0.053015 0.519671 0.385394 0.109 Uiso 1 1 calc R U . . .
C5 C 0.0480(5) 0.4608(5) 0.4608(5) 0.074(3) Uani 1 2 d S T P . .
C6 C 0.000000 0.500000 0.500000 0.073(5) Uani 1 8 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 '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 180.00(5) . . ?
O1 U1 O3 89.3(3) . 22 ?
O1 U1 O3 89.3(3) . 12 ?
O1 U1 O3 89.3(3) . 24 ?
O1 U1 O3 89.3(3) . 20 ?
O1 U1 O3 89.3(3) . . ?
O1 U1 O3 89.3(3) . 11 ?
O1 U1 C1 87.4(4) . . ?
O1 U1 C1 87.4(4) . 11 ?
O1 U1 C1 87.4(4) . 12 ?
O2 U1 O3 90.7(3) . 11 ?
O2 U1 O3 90.7(3) . 24 ?
O2 U1 O3 90.7(3) . 22 ?
O2 U1 O3 90.7(3) . . ?
O2 U1 O3 90.7(3) . 12 ?
O2 U1 O3 90.7(3) . 20 ?
O2 U1 C1 92.6(4) . . ?
O2 U1 C1 92.6(4) . 11 ?
O2 U1 C1 92.6(4) . 12 ?
O3 U1 O3 172.3(3) 22 12 ?
O3 U1 O3 119.984(11) 24 22 ?
O3 U1 O3 172.3(3) 24 11 ?
O3 U1 O3 172.3(3) . 20 ?
O3 U1 O3 119.983(11) . 11 ?
O3 U1 O3 52.5(3) . 22 ?
O3 U1 O3 119.986(11) . 12 ?
O3 U1 O3 67.5(3) 22 11 ?
O3 U1 O3 52.5(3) 11 20 ?
O3 U1 O3 119.984(11) 24 20 ?
O3 U1 O3 119.984(11) 22 20 ?
O3 U1 O3 52.5(3) 24 12 ?
O3 U1 O3 67.5(3) 12 20 ?
O3 U1 O3 119.984(11) 11 12 ?
O3 U1 O3 67.5(3) . 24 ?
O3 U1 C1 26.29(15) 12 12 ?
O3 U1 C1 146.08(15) 20 . ?
O3 U1 C1 93.73(14) . 12 ?
O3 U1 C1 146.08(16) 24 11 ?
O3 U1 C1 93.73(14) 11 . ?
O3 U1 C1 26.29(15) 11 11 ?
O3 U1 C1 26.29(15) 24 12 ?
O3 U1 C1 146.08(16) 11 12 ?
O3 U1 C1 26.29(15) 22 . ?
O3 U1 C1 93.73(14) 22 11 ?
O3 U1 C1 146.08(15) 12 . ?
O3 U1 C1 93.73(14) 12 11 ?
O3 U1 C1 26.29(15) 20 11 ?
O3 U1 C1 93.73(14) 20 12 ?
O3 U1 C1 146.08(15) . 11 ?
O3 U1 C1 26.29(15) . . ?
O3 U1 C1 146.08(15) 22 12 ?
O3 U1 C1 93.73(14) 24 . ?
C1 U1 C1 119.79(6) 12 11 ?
C1 U1 C1 119.79(6) 11 . ?
C1 U1 C1 119.79(6) 12 . ?
C1 O3 U1 95.4(6) . . ?
O3 C1 U1 58.3(6) . . ?
O3 C1 U1 58.3(6) 22 . ?
O3 C1 O3 116.2(12) . 22 ?
O3 C1 C2 121.9(6) . . ?
O3 C1 C2 121.9(6) 22 . ?
C2 C1 U1 175.6(14) . . ?
C3 C2 C1 121.9(5) 22 . ?
C3 C2 C1 121.9(5) . . ?
C3 C2 C3 115.6(12) . 22 ?
C2 C3 H3 119.0 . . ?
C2 C3 C4 122.0(8) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.7(8) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C4 118.1(11) 22 . ?
C4 C5 C6 120.9(5) 22 . ?
C4 C5 C6 120.9(5) . . ?
C5 C6 C5 115.4(6) 6_566 5_556 ?
C5 C6 C5 98.2(11) 5_556 3_565 ?
C5 C6 C5 115.4(6) 5_556 . ?
C5 C6 C5 115.4(6) 3_565 . ?
C5 C6 C5 98.2(11) 6_566 . ?
C5 C6 C5 115.4(6) 6_566 3_565 ?
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 1.7999(14) . ?
U1 O2 1.7991(14) . ?
U1 O3 2.445(6) 11 ?
U1 O3 2.445(6) 12 ?
U1 O3 2.445(6) 20 ?
U1 O3 2.445(6) . ?
U1 O3 2.445(6) 22 ?
U1 O3 2.445(6) 24 ?
U1 C1 2.861(14) 12 ?
U1 C1 2.861(14) . ?
U1 C1 2.861(14) 11 ?
O3 C1 1.273(10) . ?
C1 C2 1.422(18) . ?
C2 C3 1.389(11) 22 ?
C2 C3 1.389(11) . ?
C3 H3 0.9300 . ?
C3 C4 1.386(11) . ?
C4 H4 0.9300 . ?
C4 C5 1.372(11) . ?
C5 C6 1.533(12) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O3 C1 O3 -7.0(19) . . . 22 ?
U1 O3 C1 C2 174.8(16) . . . . ?
O3 C1 C2 C3 -176.1(16) . . . 22 ?
O3 C1 C2 C3 6(3) 22 . . 22 ?
O3 C1 C2 C3 176.1(16) 22 . . . ?
O3 C1 C2 C3 -6(3) . . . . ?
C1 C2 C3 C4 -178.9(15) . . . . ?
C2 C3 C4 C5 7(2) . . . . ?
C3 C2 C3 C4 -8(2) 22 . . . ?
C3 C4 C5 C4 -6(2) . . . 22 ?
C3 C4 C5 C6 173.2(11) . . . . ?
C4 C5 C6 C5 89.5(12) 22 . . 6_566 ?
C4 C5 C6 C5 -89.5(12) . . . 6_566 ?
C4 C5 C6 C5 -33.7(10) 22 . . 5_556 ?
C4 C5 C6 C5 147.3(14) . . . 5_556 ?
C4 C5 C6 C5 33.7(10) . . . 3_565 ?
C4 C5 C6 C5 -147.3(14) 22 . . 3_565 ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.038 0.280 -0.332 2155.1 241.6 '1 DMF'
