Structural Characterization and Reactivity of UO2(salophen)L and [UO2(salophen)]2: Dimerization of UO2(salophen) Fragments in Noncoordinating Solvents (salophen =N,N'-Disalicylidene-o-phenylenediaminate, L =N,N-Dimethylformamide, Dimethyl Sulfoxide)
Koichiro Takao; Yasuhisa Ikeda; Inorganic Chemistry 46 (2007) 1550–1562; doi:10.1021/ic0611950

data_4306910
_publ_section_title
;
Structural Characterization and Reactivity of UO2(salophen)L and
[UO2(salophen)]2: Dimerization of UO2(salophen) Fragments in
Noncoordinating Solvents (salophen
=N,N'-Disalicylidene-o-phenylenediaminate, L =N,N-Dimethylformamide,
Dimethyl Sulfoxide)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1550
_journal_page_last               1562
_journal_paper_doi               10.1021/ic0611950
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C23 H21 N3 O5 U, C H2 Cl2'
_chemical_formula_sum            'C24 H23 Cl2 N3 O5 U'
_chemical_formula_weight         742.38
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.65(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.667(4)
_cell_length_b                   9.608(3)
_cell_length_c                   24.859(10)
_cell_measurement_reflns_used    26142
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_volume                     2503.9(16)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23518
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    6.736
_exptl_absorpt_correction_T_max  0.2371
_exptl_absorpt_correction_T_min  0.2371
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.00272(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0262P)^2^+5.3741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                5274
_reflns_number_total             5734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0611950si20061026_080954.cif
_cod_data_source_block           UO2(salophen)DMFCH2Cl2-Complex_1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4306910