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_4306912
_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         '2(C40 H28 N4 O8 U2), C H2 Cl2'
_chemical_formula_sum            'C40.5 H29 Cl N4 O8 U2'
_chemical_formula_weight         1211.19
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.45(3)
_cell_angle_beta                 77.99(3)
_cell_angle_gamma                81.66(3)
_cell_formula_units_Z            4
_cell_length_a                   15.717(5)
_cell_length_b                   15.993(7)
_cell_length_c                   17.619(5)
_cell_measurement_reflns_used    35412
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3990(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37695
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    8.230
_exptl_absorpt_correction_T_max  0.6380
_exptl_absorpt_correction_T_min  0.3526
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.490
_refine_diff_density_min         -2.984
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         17850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0396P)^2^+60.3343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                12487
_reflns_number_total             17850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0611950si20061026_081030.cif
_cod_data_source_block
'[UO2(salophen)]2-0.5CH2Cl2-Complex_3-0.5CH2Cl2'
_cod_original_cell_volume        3990(2)
_cod_original_formula_sum        'C40.50 H29 Cl N4 O8 U2'
_cod_database_code               4306912