Identification of a metastable uranium metal-organic framework isomer through non-equilibrium synthesis.
Hanna, Sylvia L.; Debela, Tekalign T.; Mroz, Austin M.; Syed, Zoha H.; Kirlikovali, Kent O.; Hendon, Christopher H.; Farha, Omar K.; Chemical science 13 (2022) 13032–13039; doi:10.1039/d2sc04783g

data_1567882
_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/[\s^2^(Fo^2^)+(0.1453P)^2^+0.3780P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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
_shelx_res_checksum              29486
_shelx_hkl_checksum              47611
_shelx_fab_checksum              96657
_olex2_submission_special_instructions 'No special instructions were received'