Experimental and Theoretical Approaches to Redox Innocence of Ligands in Uranyl Complexes: What Is Formal Oxidation State of Uranium in Reductant of Uranyl(VI)?
Takao, Koichiro; Tsushima, Satoru; Ogura, Toshinari; Tsubomura, Taro; Ikeda, Yasuhisa; Inorganic chemistry 53 (2014) 5772–5780; doi:10.1021/ic5006314

data_4338476
_publ_section_title
;
 Experimental and Theoretical Approaches to Redox Innocence of Ligands in
 Uranyl Complexes: What Is Formal Oxidation State of Uranium in Reductant
 of Uranyl(VI)?
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5772
_journal_page_last               5780
_journal_paper_doi               10.1021/ic5006314
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C28 H20 N4 O8 U2'
_chemical_formula_sum            'C28 H20 N4 O8 U2'
_chemical_formula_weight         1016.55
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.4373(5)
_cell_length_b                   12.5919(4)
_cell_length_c                   14.7778(5)
_cell_measurement_reflns_used    14954
_cell_measurement_temperature    213
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.10
_cell_volume                     2686.50(16)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      213
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24726
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.105
_exptl_absorpt_correction_T_max  0.008
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856.00
_exptl_crystal_size_max          0.456
_exptl_crystal_size_mid          0.432
_exptl_crystal_size_min          0.400
_refine_diff_density_max         1.530
_refine_diff_density_min         -1.630
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3070
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0000P)^2^+15.6642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                2396
_reflns_number_total             3070
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic5006314_si_002.cif
_cod_data_source_block           130912_UO2ghaDMSO_a_
_cod_depositor_comments          'Adding full bibliography for 4338476.cif.'
_cod_database_code               4338476