CO<sub>2</sub> and CO/H<sub>2</sub> Conversion to Methoxide by a Uranium(IV) Hydride.
Falcone, Marta; Scopelliti, Rosario; Mazzanti, Marinella; Journal of the American Chemical Society 141 (2019) 9570–9577; doi:10.1021/jacs.9b02235

data_4127477
_publ_section_title
;
 CO<sub>2</sub> and CO/H<sub>2</sub> Conversion to Methoxide by a
 Uranium(IV) Hydride.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9570
_journal_page_last               9577
_journal_paper_doi               10.1021/jacs.9b02235
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C73 H166 K2 O26 Si6 U2'
_chemical_formula_sum            'C73 H166 K2 O26 Si6 U2'
_chemical_formula_weight         2182.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 93.337(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9751(2)
_cell_length_b                   18.1064(3)
_cell_length_c                   22.0854(5)
_cell_measurement_reflns_used    24191
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.4260
_cell_measurement_theta_min      4.3760
_cell_volume                     5578.99(18)
_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    'Mercury 4.0.0 (CCDC, 2018)'
_computing_publication_material  'CIFTab (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_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   -115.00 -20.00   1.00    5.00    --  -40.91 -38.00  30.00   95
  2  \w    -62.00 -14.00   1.00    5.00    --  -40.91  57.00-180.00   48
  3  \w   -113.00 -17.00   1.00    5.00    --  -40.91 -38.00 -60.00   96
  4  \w      1.00  69.00   1.00    5.00    --   40.91 -99.00 -90.00   68
  5  \w     50.00  97.00   1.00    5.00    --   40.91-125.00  30.00   47
  6  \w     20.00  47.00   1.00    5.00    --   40.91 -99.00-120.00   27
  7  \w     18.00  87.00   1.00    5.00    --   40.91  38.00-150.00   69
  8  \w     87.00 175.00   1.00   20.00    --  107.03  45.00 -30.00   88
  9  \w     34.00 128.00   1.00   20.00    --  107.03 -45.00 -30.00   94
 10  \w     31.00 127.00   1.00   20.00    --  107.03 -77.00 150.00   96
 11  \w     79.00 118.00   1.00   20.00    --  107.03-125.00-180.00   39
 12  \w     35.00  66.00   1.00   20.00    --  107.03-125.00-180.00   31
 13  \w     42.00 128.00   1.00   20.00    --  107.03 -45.00 150.00   86
 14  \w    106.00 133.00   1.00   20.00    --  107.03 -61.00   0.00   27
 15  \w    145.00 176.00   1.00   20.00    --  107.03 125.00-150.00   31
 16  \w    113.00 173.00   1.00   20.00    --  107.03 125.00  60.00   60
 17  \w     91.00 118.00   1.00   20.00    --  107.03-125.00 -30.00   27
 18  \w     25.00 109.00   1.00   20.00    --  107.03 -94.00   0.00   84
 19  \w     24.00 175.00   1.00   20.00    --  107.03   0.00 -60.00  151
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23280
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.030
_diffrn_reflns_theta_min         3.158
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.865
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.077
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       needle
_exptl_crystal_F_000             2236
_exptl_crystal_size_max          0.696
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.493
_refine_diff_density_min         -2.289
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Flack x determined using 8657 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(6)
_refine_ls_extinction_coef       0.00038(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         23280
_refine_ls_number_restraints     1680
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0888P)^2^+6.5728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.840
_reflns_Friedel_fraction_full    0.923
_reflns_Friedel_fraction_max     0.876
_reflns_number_gt                22110
_reflns_number_total             23280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02235_si_005.cif
_cod_data_source_block           mf589_sq
_cod_database_code               4127477
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.055
_shelx_estimated_absorpt_t_max   0.638
_shelx_res_checksum              86699
_shelx_hkl_checksum              22408
_shelx_fab_checksum              44951