Dinitrogen cleavage by a dinuclear uranium(iii) complex.
Jori, Nadir; Keener, Megan; Rajeshkumar, Thayalan; Scopelliti, Rosario; Maron, Laurent; Mazzanti, Marinella; Chemical science 14 (2023) 13485–13494; doi:10.1039/d3sc05253b

data_1570263
_publ_section_title
;
 Dinitrogen cleavage by a dinuclear uranium(iii) complex.
;
_journal_issue                   46
_journal_name_full               'Chemical science'
_journal_page_first              13485
_journal_page_last               13494
_journal_paper_doi               10.1039/d3sc05253b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C72 H162 K O25 Si6 U2, C18 H36 K N2 O6'
_chemical_formula_sum            'C90 H198 K2 N2 O31 Si6 U2'
_chemical_formula_weight         2527.29
_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
_audit_update_record
;
2023-06-27 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.007(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1169(7)
_cell_length_b                   42.662(4)
_cell_length_c                   21.4737(17)
_cell_measurement_reflns_used    4411
_cell_measurement_temperature    140.01(10)
_cell_measurement_theta_max      72.6290
_cell_measurement_theta_min      3.7370
_cell_volume                     12600.8(17)
_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      140.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.921
_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    -67.00  27.00   1.00   10.00    --  -42.88  57.00-180.00   94
  2  \w    -87.00 -42.00   1.00   10.00    --  -42.88 125.00-120.00   45
  3  \w   -115.00 -18.00   1.00   10.00    --  -42.88 -57.00  30.00   97
  4  \w   -124.00 -87.00   1.00   10.00    --  -42.88 -99.00-180.00   37
  5  \w    -37.00  27.00   1.00   10.00    --  -42.88  37.00 -60.00   64
  6  \w     33.00  98.00   1.00   40.00    --  105.68 -94.00  90.00   65
  7  \w     47.00 103.00   1.00   40.00    --  105.68 -94.00 150.00   56
  8  \w     52.00 103.00   1.00   40.00    --  105.68 -30.00  30.00   51
  9  \w     32.00 115.00   1.00   40.00    --  105.68-125.00  30.00   83
 10  \w     92.00 119.00   1.00   40.00    --  105.68 -45.00 -60.00   27
 11  \w     36.00  96.00   1.00   40.00    --  105.68 -30.00-180.00   60
 12  \w     76.00 107.00   1.00   40.00    --  105.68 -94.00   0.00   31
 13  \w     78.00 178.00   1.00   40.00    --  105.68  30.00  90.00  100
;
_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  0.1780
_diffrn_reflns_av_unetI/netI     0.2262
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61653
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.876
_diffrn_reflns_theta_min         3.376
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.844
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense red'
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             5224
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.042
_refine_diff_density_max         3.277
_refine_diff_density_min         -3.585
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1252
_refine_ls_number_reflns         23873
_refine_ls_number_restraints     1262
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.2142
_refine_ls_R_factor_gt           0.1184
_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^)+(0.1205P)^2^+27.0916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2749
_refine_ls_wR_factor_ref         0.3568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9876
_reflns_number_total             23873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05253b2.cif
_cod_data_source_block           nj177
_cod_depositor_comments
'Adding full bibliography for 1570263--1570267.cif.'
_cod_original_cell_volume        12600.8(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1570263
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.419
_shelx_estimated_absorpt_t_max   0.708
_shelx_res_checksum              56117