Cation assisted binding and cleavage of dinitrogen by uranium complexes
Jori, Nadir; Rajeshkumar, Thayalan; Scopelliti, Rosario; Z̆ivković, Ivica; Sienkiewicz, Andrzej; Maron, Laurent; Mazzanti, Marinella; Chemical Science 13 (2022) 9232–9242; doi:10.1039/D2SC02530B

data_1567299
_publ_section_title
;
 Cation assisted binding and cleavage of dinitrogen by uranium complexes
;
_journal_issue                   32
_journal_name_full               'Chemical Science'
_journal_page_first              9232
_journal_page_last               9242
_journal_paper_doi               10.1039/D2SC02530B
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C72 H162 O25 Rb Si6 U2'
_chemical_formula_sum            'C72 H162 O25 Rb Si6 U2'
_chemical_formula_weight         2158.08
_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
_audit_update_record
;
2022-02-24 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                71.888(6)
_cell_angle_beta                 81.133(6)
_cell_angle_gamma                71.005(6)
_cell_formula_units_Z            2
_cell_length_a                   13.7997(11)
_cell_length_b                   16.5080(11)
_cell_length_c                   25.0252(18)
_cell_measurement_reflns_used    2529
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      71.1280
_cell_measurement_theta_min      5.0890
_cell_volume                     5114.5(7)
_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 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 0.997
_diffrn_measured_fraction_theta_max 0.957
_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    -46.00 -11.00   1.00   10.00    --  -43.13 125.00 120.00   35
  2  \w    -71.00  30.00   1.00   10.00    --  -43.13  57.00  30.00  101
  3  \w   -107.00 -22.00   1.00   10.00    --  -43.13 -57.00-120.00   85
  4  \w   -107.00 -80.00   1.00   10.00    --  -43.13 -99.00   0.00   27
  5  \w   -123.00 -84.00   1.00   10.00    --  -43.13 -99.00 -60.00   39
  6  \w     27.00  91.00   1.00   10.00    --   43.13-125.00-180.00   64
  7  \w     40.00 116.00   1.00   40.00    --  105.68-125.00  30.00   76
  8  \w     34.00  65.00   1.00   40.00    --  105.68 -61.00-150.00   31
  9  \w     38.00 112.00   1.00   40.00    --  105.68 -77.00   0.00   74
 10  \w     60.00 131.00   1.00   40.00    --  105.68 -45.00  90.00   71
 11  \w     44.00 129.00   1.00   40.00    --  105.68 -45.00   0.00   85
 12  \w     55.00  82.00   1.00   40.00    --  105.68 -94.00 -60.00   27
 13  \w     42.00 118.00   1.00   40.00    --  105.68-125.00-180.00   76
 14  \w    110.00 178.00   1.00   40.00    --  105.68  77.00 150.00   68
 15  \w     48.00 109.00   1.00   40.00    --  105.68 -94.00-150.00   61
 16  \w     48.00 117.00   1.00   40.00    --  105.68 -45.00-150.00   69
 17  \w     18.00 174.00   1.00   40.00    --  105.68   0.00 -30.00  156
;
_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     0.3321
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22172
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.332
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.590
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_correction_T_min  0.480
_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            'clear dark orange'
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2198
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.057
_refine_diff_density_max         5.654
_refine_diff_density_min         -4.529
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         22172
_refine_ls_number_restraints     1619
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.2321
_refine_ls_R_factor_gt           0.0858
_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^)+(0.0692P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.2326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7384
_reflns_number_total             22172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02530b2.cif
_cod_data_source_block           nj68
_cod_depositor_comments
'Adding full bibliography for 1567298--1567305.cif.'
_cod_database_code               1567299
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.349
_shelx_estimated_absorpt_t_max   0.584
_shelx_res_checksum              80059
_shelx_hkl_checksum              65554