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_4517404
_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         '0.25(C48 H16 Cl16 O40 U4), 4(H2 O)'
_chemical_formula_sum            'C12 H12 Cl4 O14 U'
_chemical_formula_weight         760.05
_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     dual
_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                 96.415(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8598(7)
_cell_length_b                   11.4960(6)
_cell_length_c                   12.6100(6)
_cell_measurement_reflns_used    3646
_cell_measurement_temperature    285(13)
_cell_measurement_theta_max      29.3660
_cell_measurement_theta_min      3.5550
_cell_volume                     1996.60(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      285(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.850
_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    -19.00  12.00   1.00   45.92    --  -11.73 -99.00-180.00   31
  2  \w    -27.00  49.00   1.00   45.92    --  -11.73  77.00 -90.00   76
  3  \w    -64.00  29.00   1.00   45.92    --  -11.73 -19.00 -60.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0192534000
_diffrn_orient_matrix_UB_12      0.0089164000
_diffrn_orient_matrix_UB_13      -0.0491620000
_diffrn_orient_matrix_UB_21      -0.0369684000
_diffrn_orient_matrix_UB_22      0.0413442000
_diffrn_orient_matrix_UB_23      -0.0151469000
_diffrn_orient_matrix_UB_31      0.0302937000
_diffrn_orient_matrix_UB_32      0.0448580000
_diffrn_orient_matrix_UB_33      0.0236649000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5341
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.733
_diffrn_reflns_theta_min         2.917
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.737
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.528
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+0.2945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2312
_reflns_number_total             2422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03727_si_003.cif
_cod_data_source_block           exp_1123_u
_cod_depositor_comments
'Adding full bibliography for 4517403--4517404.cif.'
_cod_database_code               4517404
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'U Cl2 C6 H6 O2'
_shelx_estimated_absorpt_t_max   0.669
_shelx_estimated_absorpt_t_min   0.335
_reflns_odcompleteness_completeness 99.77
_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              3069
_shelx_hkl_checksum              12558
_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 1.639
_oxdiff_exptl_absorpt_empirical_full_min 0.765