Synthesis of Electron-Rich Uranium(IV) Complexes Supported by Tridentate Schiff Base Ligands and Their Multi-Electron Redox Chemistry
Clément Camp; Julie Andrez; Jacques Pécaut; Marinella Mazzanti; Inorganic Chemistry 52 (2013) 7078–7086; doi:10.1021/ic4006218

data_4335207
_publ_section_title
;
 Synthesis of Electron-Rich Uranium(IV) Complexes Supported by Tridentate
 Schiff Base Ligands and Their Multi-Electron Redox Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7078
_journal_page_last               7086
_journal_paper_doi               10.1021/ic4006218
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C78.5 H60.5 N8.5 O4 U'
_chemical_formula_weight         1424.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.506(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   45.625(2)
_cell_length_b                   15.8387(9)
_cell_length_c                   18.5959(13)
_cell_measurement_reflns_used    3653
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4118
_cell_measurement_theta_min      3.3590
_cell_volume                     12586.7(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -92.00  -43.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  137.0000 -139.0000 49

  2 omega  -55.00   37.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000  150.0000 92

  3 omega  -98.00   15.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -19.0000 -150.0000 113

  4 omega  -97.00    1.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000   30.0000 98

  5 omega  -53.00  -28.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   37.0000  -60.0000 25

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1193
_diffrn_reflns_av_sigmaI/netI    0.1343
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31319
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    2.640
_exptl_absorpt_correction_T_max  0.9466
_exptl_absorpt_correction_T_min  0.5536
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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)
;
_exptl_crystal_colour            'translucent dark red'
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       plate
_exptl_crystal_F_000             5720
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.465
_refine_diff_density_min         -1.712
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         9013
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+79.6526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                5650
_reflns_number_total             9013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4006218_si_001_3.cif
_cod_data_source_block           3
_cod_original_cell_volume        12586.6(13)
_cod_original_formula_sum        'C78.50 H60.50 N8.50 O4 U'
_cod_database_code               4335207