Reaction of the Uranyl(VI) Ion (UO22+) with a Triamidoamine Ligand: Preparation and Structural Characterization of a Mixed-Valent Uranium(V/VI) Oxo-Imido Dimer
Paul B. Duval; Carol J. Burns; Wayne E. Buschmann; David L. Clark; David E. Morris; Brian L. Scott; Inorganic Chemistry 40 (2001) 5491–5496; doi:10.1021/ic010155n

data_4320373
_publ_section_title
;
 Reaction of the Uranyl(VI) Ion (UO22+) with a Triamidoamine Ligand:
 Preparation and Structural Characterization of a Mixed-Valent
 Uranium(V/VI) Oxo-Imido Dimer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5491
_journal_page_last               5496
_journal_paper_doi               10.1021/ic010155n
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C52 H118 Cl0 K N8 O9 Si4 U2'
_chemical_formula_weight         1627.06
_chemical_name_systematic
;
?
;
_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                101.374(1)
_cell_angle_beta                 103.757(1)
_cell_angle_gamma                109.340(1)
_cell_formula_units_Z            1
_cell_length_a                   12.1144(6)
_cell_length_b                   12.6084(6)
_cell_length_c                   14.5072(7)
_cell_measurement_temperature    203(2)
_cell_volume                     1936.60(16)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker P4/CCD'
_diffrn_measurement_method       '\f and \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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7257
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    4.338
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             817
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.972
_refine_diff_density_min         -2.390
_refine_diff_density_rms         0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.303
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         7257
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.304
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                6521
_reflns_number_total             7257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010155n.cif
_cod_data_source_block           ccd124
_cod_database_code               4320373