A Redox-Innocent Uranium(IV)-Quinoid Metal-Organic Framework.
Refn, Vanja E.; Kubus, Mariusz; Mossin, Susanne; Larsen, René Wugt; Pedersen, Kasper S.; ACS omega 5 (2020) 3462–3466; doi:10.1021/acsomega.9b03727

data_4517403
_publ_section_title
;
 A Redox-Innocent Uranium(IV)-Quinoid Metal-Organic Framework.
;
_journal_issue                   7
_journal_name_full               'ACS omega'
_journal_page_first              3462
_journal_page_last               3466
_journal_paper_doi               10.1021/acsomega.9b03727
_journal_volume                  5
_journal_year                    2020
_chemical_formula_moiety         'C6 H2 Cl2 O5 U0.5, 2(H2 O)'
_chemical_formula_sum            'C6 H6 Cl2 O7 U0.5'
_chemical_formula_weight         380.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-02-21
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.847(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7293(4)
_cell_length_b                   11.3630(4)
_cell_length_c                   12.5175(4)
_cell_measurement_reflns_used    6974
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      29.4390
_cell_measurement_theta_min      3.8710
_cell_volume                     1942.65(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -17.00  87.00   1.00   34.16    --   10.79  77.00 120.00  104
  2  \w    -28.00  61.00   1.00   34.16    --  -11.73  57.00   0.00   89
  3  \w    -20.00   5.00   1.00   34.16    --  -11.73 -99.00-180.00   25
  4  \w    -32.00  -5.00   1.00   34.16    --  -11.73 -19.00 -30.00   27
  5  \w    -87.00  21.00   1.00   34.16    --  -11.73 -77.00-120.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0323828000
_diffrn_orient_matrix_UB_12      0.0103201000
_diffrn_orient_matrix_UB_13      -0.0396945000
_diffrn_orient_matrix_UB_21      -0.0252290000
_diffrn_orient_matrix_UB_22      -0.0426532000
_diffrn_orient_matrix_UB_23      -0.0336536000
_diffrn_orient_matrix_UB_31      -0.0318411000
_diffrn_orient_matrix_UB_32      0.0443521000
_diffrn_orient_matrix_UB_33      -0.0231732000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9176
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.494
_diffrn_reflns_theta_min         2.760
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear blackish black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.599
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.528
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0183
_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^)+(0.0226P)^2^+4.4107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2323
_reflns_number_total             2437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03727_si_002.cif
_cod_data_source_block           exp_1124_u120k
_cod_depositor_comments
'Adding full bibliography for 4517403--4517404.cif.'
_cod_original_cell_volume        1942.64(11)
_cod_original_formula_sum        'C6 H6 Cl2 O7 U0.50'
_cod_database_code               4517403
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'U Cl2 C4 H4 O2'
_shelx_estimated_absorpt_t_max   0.467
_shelx_estimated_absorpt_t_min   0.267
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O6(H6A,H6B), O7(H7A,H7B)
2.b Rotating group:
 O5(H5A,H5B)
;
_shelx_res_checksum              36081
_shelx_hkl_checksum              8659
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.551
_oxdiff_exptl_absorpt_empirical_full_min 0.751