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_4335208
_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            'C42 H30 N4 O4 U'
_chemical_formula_weight         892.73
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.281(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2723(5)
_cell_length_b                   11.8342(3)
_cell_length_c                   18.1568(5)
_cell_measurement_reflns_used    6137
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3489
_cell_measurement_theta_min      3.3657
_cell_volume                     3319.98(17)
_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
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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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    5.00   92.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   57.0000 -180.0000 87

  2 omega  -10.00   89.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   19.0000  120.0000 99

  3 omega   32.00   93.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051 -179.0000   60.0000 61

  4 omega    1.00   76.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051 -115.0000  -83.0000 75

  5 omega  -78.00  -31.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  115.0000    6.0000 47

  6 omega    5.00   94.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   57.0000  -60.0000 89

  7 omega -100.00  -60.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239 -170.0000   30.0000 40

;
_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  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0812
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39686
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    4.941
_exptl_absorpt_correction_T_max  0.8823
_exptl_absorpt_correction_T_min  0.3532
_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 intense pink'
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.340
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         10126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+1.9430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                6032
_reflns_number_total             10126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4006218_si_001_4.cif
_cod_data_source_block           4
_cod_original_cell_volume        3319.99(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4335208