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_4127473
_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_formula_moiety         'C73 H162 K2 O26 Si6 U2'
_chemical_formula_sum            'C73 H162 K2 O26 Si6 U2'
_chemical_formula_weight         2178.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 91.5652(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.26268(13)
_cell_length_b                   17.70163(18)
_cell_length_c                   21.97679(18)
_cell_measurement_reflns_used    29871
_cell_measurement_temperature    140.01(10)
_cell_measurement_theta_max      76.4990
_cell_measurement_theta_min      4.3900
_cell_volume                     5546.47(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      140.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -67.00  30.00   1.00    1.00    --  -43.01  57.00  30.00   97
  2  \w    -59.00 -11.00   1.00    1.00    --  -43.01  37.00-180.00   48
  3  \w   -109.00 -17.00   1.00    1.00    --  -43.01 -57.00-120.00   92
  4  \w     13.00  81.00   1.00    1.00    --   43.01 -99.00-150.00   68
  5  \w     52.00  78.00   1.00    4.00    --  112.00 -77.00-180.00   26
  6  \w     83.00 108.00   1.00    4.00    --  112.00 -77.00-180.00   25
  7  \w     70.00 116.00   1.00    4.00    --  112.00-111.00-150.00   46
  8  \w     50.00 114.00   1.00    4.00    --  112.00-111.00 -60.00   64
  9  \w     70.00 113.00   1.00    4.00    --  112.00-111.00  30.00   43
 10  \w     68.00  94.00   1.00    4.00    --  112.00-111.00  60.00   26
 11  \w     56.00  89.00   1.00    4.00    --  112.00 -94.00 -30.00   33
 12  \w     40.00 115.00   1.00    4.00    --  112.00-111.00-120.00   75
 13  \w     39.00 112.00   1.00    4.00    --  112.00 -45.00 -60.00   73
 14  \w     94.00 178.00   1.00    4.00    --  112.00  30.00  30.00   84
 15  \w    134.00 173.00   1.00    4.00    --  112.00  61.00 -60.00   39
 16  \w    136.00 173.00   1.00    4.00    --  112.00  61.00-120.00   37
 17  \w    152.00 177.00   1.00    4.00    --  112.00  61.00-180.00   25
 18  \w    102.00 129.00   1.00    4.00    --  112.00  61.00-120.00   27
 19  \w     95.00 167.00   1.00    4.00    --  112.00  45.00 -30.00   72
 20  \w    118.00 146.00   1.00    4.00    --  112.00 111.00  90.00   28
 21  \w    113.00 178.00   1.00    4.00    --  112.00 111.00   0.00   65
 22  \w    101.00 157.00   1.00    4.00    --  112.00 111.00-150.00   56
 23  \w     84.00 169.00   1.00    4.00    --  112.00  61.00 -90.00   85
 24  \w     84.00 112.00   1.00    4.00    --  112.00  61.00 -60.00   28
 25  \w     85.00 140.00   1.00    4.00    --  112.00  61.00-180.00   55
 26  \w     29.00  55.00   1.00    4.00    --  112.00 -94.00-120.00   26
 27  \w     38.00  92.00   1.00    4.00    --  112.00-111.00-180.00   54
 28  \w     39.00 116.00   1.00    4.00    --  112.00-111.00 -30.00   77
 29  \w     36.00 115.00   1.00    4.00    --  112.00-111.00  90.00   79
 30  \w     43.00 116.00   1.00    4.00    --  112.00-111.00 150.00   73
 31  \w     30.00  89.00   1.00    4.00    --  112.00 -94.00  90.00   59
 32  \w    -86.00  -7.00   1.00    1.00    --  -43.01 125.00  60.00   79
 33  \w   -123.00 -87.00   1.00    1.00    --  -43.01 -99.00  30.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_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_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62550
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.768
_diffrn_reflns_theta_min         3.649
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.923
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.156
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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 pale yellow'
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       prism
_exptl_crystal_F_000             2228
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.171
_refine_diff_density_max         2.621
_refine_diff_density_min         -2.834
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.000066(17)
_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   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         11623
_refine_ls_number_restraints     960
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0801P)^2^+20.7608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10895
_reflns_number_total             11623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02235_si_002.cif
_cod_data_source_block           mf457
_cod_database_code               4127473
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.176
_shelx_estimated_absorpt_t_max   0.282
_shelx_res_checksum              25224
_shelx_hkl_checksum              12623
_shelx_fab_checksum              4389