C-H Bond Activation by an Isolated Dinuclear U(III)/U(IV) Nitride.
Palumbo, Chad T.; Scopelliti, Rosario; Zivkovic, Ivica; Mazzanti, Marinella; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b12804

data_4134066
_publ_section_title
;
 C-H Bond Activation by an Isolated Dinuclear U(III)/U(IV) Nitride.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12804
_journal_year                    2020
_chemical_formula_moiety         'C46 H78 N4 O Si6 U2'
_chemical_formula_sum            'C46 H78 N4 O Si6 U2'
_chemical_formula_weight         1347.72
_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'
_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                 103.954(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1022(5)
_cell_length_b                   13.8129(5)
_cell_length_c                   26.1373(7)
_cell_measurement_reflns_used    14000
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      31.7240
_cell_measurement_theta_min      3.4650
_cell_volume                     6342.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Mercury 4.2.0 (CCDC, 2019)'
_computing_publication_material  'CIFtab (Sheldrick, 2016)'
_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 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.923
_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   -105.00 -77.00   1.00   85.00    --  -17.94 178.00-180.00   28
  2  \w    -14.00  42.00   1.00   85.00    --   18.87  77.00-180.00   56
  3  \w    -13.00  55.00   1.00   85.00    --   18.87  77.00   0.00   68
  4  \w     39.00 102.00   1.00   85.00    --   18.87-178.00 150.00   63
  5  \w    -56.00  34.00   1.00   85.00    --   18.87 -37.00-180.00   90
  6  \w    -13.00  96.00   1.00   85.00    --   18.87  19.00   0.00  109
;
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.2036
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            36216
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.812
_diffrn_reflns_theta_min         3.212
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.244
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.476
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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 dark brown'
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       plate
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.169
_refine_diff_density_max         2.395
_refine_diff_density_min         -1.978
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         36216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.820
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0292P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17107
_reflns_number_total             36216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12804_si_006.cif
_cod_data_source_block           ctp602_sq
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4134066
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.442
_shelx_estimated_absorpt_t_max   0.471
_shelx_res_checksum              30815
_shelx_hkl_checksum              24288
_shelx_fab_checksum              82865