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_4127475
_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         'C76 H170 K2 N2 O25 Si6 U2'
_chemical_formula_sum            'C76 H170 K2 N2 O25 Si6 U2'
_chemical_formula_weight         2234.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.406(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8521(7)
_cell_length_b                   13.9941(4)
_cell_length_c                   33.3790(8)
_cell_measurement_reflns_used    16609
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      73.5060
_cell_measurement_theta_min      3.3440
_cell_volume                     11108.6(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      139.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_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  0.1174
_diffrn_reflns_av_unetI/netI     0.1082
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            67482
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         2.655
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.921
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.252
_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            yellow
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       prism
_exptl_crystal_F_000             4584
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.076
_refine_diff_density_max         7.762
_refine_diff_density_min         -2.150
_refine_diff_density_rms         0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1102
_refine_ls_number_reflns         19457
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0976
_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^)+(0.1320P)^2^+118.9176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2384
_refine_ls_wR_factor_ref         0.2647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14088
_reflns_number_total             19457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02235_si_004.cif
_cod_data_source_block           mf566
_cod_database_code               4127475
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.200
_shelx_estimated_absorpt_t_max   0.519
_shelx_res_checksum              57623
_shelx_hkl_checksum              1984
_shelx_fab_checksum              43531