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_4127474
_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         'C75 H163 K2 O31 Si6 U2'
_chemical_formula_sum            'C75 H163 K2 O31 Si6 U2'
_chemical_formula_weight         2283.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-10-23 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5015(3)
_cell_length_b                   18.6524(5)
_cell_length_c                   45.9564(12)
_cell_measurement_reflns_used    11385
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      74.9870
_cell_measurement_theta_min      3.6790
_cell_volume                     11573.4(5)
_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 3.10.3 (CCDC, 2018)'
_computing_publication_material  'CIFTab (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(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 0.992
_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   -112.00 -21.00   1.00   12.50    --  -43.01 -57.00 150.00   91
  2  \w   -124.00 -99.00   1.00   12.50    --  -43.01 -99.00 -30.00   25
  3  \w    -69.00  30.00   1.00   12.50    --  -43.01  57.00  60.00   99
  4  \w    -68.00  30.00   1.00   12.50    --  -43.01  57.00 -60.00   98
  5  \w     36.00  94.00   1.00   12.50    --   43.01-125.00-180.00   58
  6  \w     46.00 108.00   1.00   50.00    --  109.26 -94.00  60.00   62
  7  \w     37.00 136.00   1.00   50.00    --  109.26 -61.00 150.00   99
  8  \w     50.00 135.00   1.00   50.00    --  109.26 -45.00  30.00   85
  9  \w    143.00 168.00   1.00   50.00    --  109.26  30.00 -90.00   25
 10  \w     44.00 138.00   1.00   50.00    --  109.26 -30.00 -60.00   94
 11  \w     91.00 178.00   1.00   50.00    --  109.26  45.00 -30.00   87
 12  \w     82.00 109.00   1.00   50.00    --  109.26 -94.00-180.00   27
 13  \w     34.00  60.00   1.00   50.00    --  109.26-111.00 -30.00   26
 14  \w     88.00 115.00   1.00   50.00    --  109.26-111.00 -30.00   27
 15  \w    106.00 133.00   1.00   50.00    --  109.26 111.00 -90.00   27
 16  \w     64.00 113.00   1.00   50.00    --  109.26-111.00-180.00   49
 17  \w     69.00  96.00   1.00   50.00    --  109.26-111.00 -60.00   27
 18  \w     39.00 122.00   1.00   50.00    --  109.26 -61.00 -90.00   83
 19  \w     61.00 157.00   1.00   50.00    --  109.26 -15.00 120.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, 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  0.1369
_diffrn_reflns_av_unetI/netI     0.1184
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            85892
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.625
_diffrn_reflns_theta_min         3.734
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40112
_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 light colourless'
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       needle
_exptl_crystal_F_000             4668
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.112
_refine_diff_density_max         1.585
_refine_diff_density_min         -2.105
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
;
 Flack x determined using 5922 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.023(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         23679
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                17572
_reflns_number_total             23679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02235_si_006.cif
_cod_data_source_block           ss5
_cod_database_code               4127474
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.197
_shelx_estimated_absorpt_t_max   0.414
_shelx_res_checksum              34258
_shelx_hkl_checksum              98708
_shelx_fab_checksum              4954
_publcif_funding_html
;
;