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_4134065
_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_sum            'C72 H171 N10 O2 Si16 U4'
_chemical_formula_weight         2610.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                92.605(2)
_cell_angle_beta                 92.492(3)
_cell_angle_gamma                109.741(3)
_cell_formula_units_Z            2
_cell_length_a                   12.3775(4)
_cell_length_b                   15.2039(4)
_cell_length_c                   32.5115(10)
_cell_measurement_reflns_used    7282
_cell_measurement_temperature    140.2(6)
_cell_measurement_theta_max      72.4320
_cell_measurement_theta_min      3.0680
_cell_volume                     5741.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.2(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_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   -113.00 -39.00   1.00    7.50    --  -40.91 -38.00-150.00   74
  2  \w    -64.00  29.00   1.00    7.50    --  -40.91  77.00 -60.00   93
  3  \w    -73.00  -6.00   1.00    7.50    --  -40.91 125.00 120.00   67
  4  \w    -48.00  27.00   1.00    7.50    --  -40.91  38.00  30.00   75
  5  \w    -87.00 -49.00   1.00    7.50    --  -40.91 125.00  30.00   38
  6  \w    -19.00  37.00   1.00    7.50    --   40.91 -77.00  90.00   56
  7  \w     53.00  80.00   1.00   30.00    --  105.15-111.00   0.00   27
  8  \w     29.00 131.00   1.00   30.00    --  105.15 -30.00 -30.00  102
  9  \w     76.00 109.00   1.00   30.00    --  105.15-111.00 -60.00   33
 10  \w     76.00 173.00   1.00   30.00    --  105.15  61.00 -30.00   97
 11  \w     48.00  91.00   1.00   30.00    --  105.15 -94.00  60.00   43
 12  \w     29.00 108.00   1.00   30.00    --  105.15-111.00 150.00   79
 13  \w    111.00 140.00   1.00   30.00    --  105.15 111.00 -90.00   29
 14  \w     54.00  79.00   1.00   30.00    --  105.15 -45.00  30.00   25
 15  \w    111.00 139.00   1.00   30.00    --  105.15  77.00 150.00   28
 16  \w     31.00 154.00   1.00   30.00    --  105.15 -15.00 150.00  123
 17  \w     36.00 129.00   1.00   30.00    --  105.15 -61.00-180.00   93
 18  \w     29.00 109.00   1.00   30.00    --  105.15-111.00  30.00   80
 19  \w     27.00 105.00   1.00   30.00    --  105.15 -94.00-180.00   78
;
_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_R_equivalents  0.0861
_diffrn_reflns_av_unetI/netI     0.1268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            43244
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.858
_diffrn_reflns_theta_min         3.094
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.572
_exptl_absorpt_correction_T_max  0.417
_exptl_absorpt_correction_T_min  0.096
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (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 pale orange'
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       plate
_exptl_crystal_F_000             2562
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.109
_refine_diff_density_max         3.235
_refine_diff_density_min         -2.268
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         22238
_refine_ls_number_restraints     1137
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0493P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14040
_reflns_number_total             22238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12804_si_007.cif
_cod_data_source_block           ctp613
_cod_original_cell_volume        5741.5(3)
_cod_database_code               4134065
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.105
_shelx_estimated_absorpt_t_max   0.250
_shelx_res_checksum              1078
_shelx_hkl_checksum              42955
_shelx_fab_checksum              9975