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_4134064
_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         'C32 H90 N5 O2 Si8 U2'
_chemical_formula_sum            'C32 H90 N5 O2 Si8 U2'
_chemical_formula_weight         1277.86
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                84.395(13)
_cell_angle_beta                 76.525(13)
_cell_angle_gamma                77.750(13)
_cell_formula_units_Z            2
_cell_length_a                   10.4218(16)
_cell_length_b                   12.6637(19)
_cell_length_c                   21.703(3)
_cell_measurement_reflns_used    1097
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      62.0660
_cell_measurement_theta_min      3.9920
_cell_volume                     2718.6(7)
_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 4.1.3 (CCDC, 2019)'
_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      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -110.00 -20.00   1.00   10.00    --  -42.76 -57.00  60.00   90
  2  \w    -69.00  30.00   1.00   10.00    --  -42.76  57.00-150.00   99
  3  \w    -90.00  -7.00   1.00   10.00    --  -42.76 125.00 -90.00   83
  4  \w   -123.00 -87.00   1.00   10.00    --  -42.76 -99.00-150.00   36
  5  \w   -115.00 -87.00   1.00   10.00    --  -42.76 -99.00 120.00   28
  6  \w     75.00 117.00   1.00   40.00    --  105.68-125.00-150.00   42
  7  \w     87.00 134.00   1.00   40.00    --  105.68 -61.00  30.00   47
  8  \w     40.00 116.00   1.00   40.00    --  105.68 -77.00-180.00   76
  9  \w     39.00 125.00   1.00   40.00    --  105.68 -45.00 -90.00   86
 10  \w     57.00  84.00   1.00   40.00    --  105.68 -94.00 120.00   27
 11  \w     41.00 123.00   1.00   40.00    --  105.68 -45.00-180.00   82
 12  \w     40.00  66.00   1.00   40.00    --  105.68-125.00-150.00   26
 13  \w     36.00 124.00   1.00   40.00    --  105.68 -45.00   0.00   88
 14  \w     68.00 118.00   1.00   40.00    --  105.68-125.00   0.00   50
 15  \w    106.00 174.00   1.00   40.00    --  105.68  77.00 -30.00   68
 16  \w     53.00 108.00   1.00   40.00    --  105.68 -94.00  30.00   55
 17  \w     18.00 169.00   1.00   40.00    --  105.68   0.00 150.00  151
;
_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_unetI/netI     0.2637
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9935
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         3.576
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.552
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_correction_T_min  0.325
_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            'metallic dark black'
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       plate
_exptl_crystal_F_000             1258
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.056
_refine_diff_density_max         4.264
_refine_diff_density_min         -2.371
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.804
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         9935
_refine_ls_number_restraints     481
_refine_ls_restrained_S_all      0.787
_refine_ls_R_factor_all          0.1816
_refine_ls_R_factor_gt           0.0824
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0884P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1817
_refine_ls_wR_factor_ref         0.2128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3820
_reflns_number_total             9935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12804_si_009.cif
_cod_data_source_block           ctp419
_cod_database_code               4134064
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.228
_shelx_estimated_absorpt_t_max   0.423
_shelx_res_checksum              20879
_shelx_hkl_checksum              6264