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_4335206
_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            'C98 H76 N8 O4 U2'
_chemical_formula_weight         1905.73
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_symmetry_space_group_name_Hall  '-P 1'
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
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;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9653
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;
  1 omega   35.00   92.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   37.0000  -30.0000 57

  2 omega   32.00   57.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051 -179.0000 -180.0000 25

  3 omega  -42.00   46.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  -57.0000 -120.0000 88

  4 omega  -42.00    3.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000 -180.0000 45

  5 omega  -88.00   -1.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000   30.0000 87

  6 omega  -57.00   43.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000  150.0000 100

  7 omega  -33.00   -5.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000  -60.0000 28

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
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_diffrn_reflns_av_sigmaI/netI    0.2388
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_diffrn_reflns_limit_h_min       -13
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_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
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_exptl_absorpt_coefficient_mu    4.324
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.3218
_exptl_crystal_size_mid          0.1904
_exptl_crystal_size_min          0.0207
_refine_diff_density_max         2.983
_refine_diff_density_min         -1.895
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7739
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1516
_reflns_number_gt                4456
_reflns_number_total             7739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4006218_si_001_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        1897.75(15)
_cod_database_code               4335206