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_4335205
_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            'C47 H35 Cl2 N5 O2 U'
_chemical_formula_weight         1010.73
_chemical_name_systematic
; 
 ? 
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_cell_angle_beta                 101.394(3)
_cell_angle_gamma                102.627(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0338(4)
_cell_length_b                   12.7361(5)
_cell_length_c                   16.6880(7)
_cell_measurement_reflns_used    12072
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4251
_cell_measurement_theta_min      3.3027
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega    0.00   90.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489    0.0000  -30.0000 90

  2 omega    0.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489 -129.0000   10.0000 85

  3 omega   -5.00   21.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489   77.0000  120.0000 26

  4 omega   24.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489 -128.0000  124.0000 61

  5 omega  -43.00  -17.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489    0.0000  -30.0000 26

  6 omega  -47.00  -18.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489  -37.0000  -30.0000 29

  7 omega    3.00   31.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489  -37.0000  -30.0000 28

  8 omega   -1.00   37.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489   37.0000  120.0000 38

  9 omega   69.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489   77.0000  120.0000 26

 10 omega  -86.00    3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000  -30.0000 89

 11 omega  -57.00   43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000 -120.0000 100

 12 omega  -53.00   45.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   37.0000 -150.0000 98

 13 omega  -95.00    1.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000  120.0000 96

 14 omega  -71.00    3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000 -150.0000 74

;
_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  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41283
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    4.287
_exptl_absorpt_correction_T_max  0.5695
_exptl_absorpt_correction_T_min  0.3767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         5.549
_refine_diff_density_min         -2.664
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         12067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+0.2386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                10446
_reflns_number_total             12067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4006218_si_001_1.cif
_cod_data_source_block           1-Cl
_cod_original_cell_volume        1977.10(13)
_cod_database_code               4335205