Tuning the structure, reactivity and magnetic communication of nitride-bridged uranium complexes with the ancillary ligands
Palumbo, Chad T.; Barluzzi, Luciano; Scopelliti, Rosario; Zivkovic, Ivica; Fabrizio, Alberto; Corminboeuf, Clémence; Mazzanti, Marinella; Chemical Science  (2019) –; doi:10.1039/C9SC02149C

data_1552192
_publ_section_title
;
 Tuning the structure, reactivity and magnetic communication of
 nitride-bridged uranium complexes with the ancillary ligands
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02149C
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C72 H162 N O24 Si6 U2, C16 H36 N'
_chemical_formula_sum            'C88 H198 N2 O24 Si6 U2'
_chemical_formula_weight         2313.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 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
;
2019-04-30 deposited with the CCDC.    2019-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.031(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2946(4)
_cell_length_b                   16.3627(3)
_cell_length_c                   25.1526(6)
_cell_measurement_reflns_used    23049
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2050
_cell_measurement_theta_min      2.7480
_cell_volume                     5810.2(2)
_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 4.1.0 (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      100(2)
_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 0.999
_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     34.00  60.00   1.00   35.03    --   19.91-178.00 120.00   26
  2  \w     -8.00  93.00   1.00   35.03    --   19.91  57.00 150.00  101
  3  \w    -13.00  96.00   1.00   35.03    --   19.91  77.00   0.00  109
  4  \w    -51.00  46.00   1.00   35.03    --   19.91 -57.00-120.00   97
  5  \w     35.00  81.00   1.00   35.03    --   19.91 178.00 -90.00   46
  6  \w      5.00  93.00   1.00   35.03    --   19.91  57.00-120.00   88
  7  \w    -20.00  61.00   1.00   35.03    --   19.91 -99.00   0.00   81
  8  \w    -87.00 -60.00   1.00   35.03    --  -20.22 144.00 -14.34   27
  9  \w    -97.00 -53.00   1.00   35.03    --  -20.22 155.00 102.80   44
 10  \w    -45.00  54.00   1.00   35.03    --  -20.22  38.00 120.00   99
;
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            60518
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.489
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.906
_exptl_absorpt_correction_T_max  0.658
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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 dark red'
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       plate
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.199
_refine_diff_density_max         1.659
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.493(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         17734
_refine_ls_number_restraints     696
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+18.5395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                15714
_reflns_number_total             17734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02149c2.cif
_cod_data_source_block           lb690
_cod_original_cell_volume        5810.2(3)
_cod_database_code               1552192
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.441
_shelx_estimated_absorpt_t_max   0.596
_shelx_res_checksum              44313