Mixed-Ligand Uranyl(V) β-Diketiminate/β-Diketonate Complexes: Synthesis and Characterization
Trevor W. Hayton; Guang Wu; Inorganic Chemistry 47 (2008) 7415–7423; doi:10.1021/ic800778j

data_4305840
_publ_contact_author             'Trevor W. Hayton'
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_section_title
;
Mixed-Ligand Uranyl(V) \b-Diketiminate/\b-Diketonate Complexes: Synthesis
and Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7415
_journal_page_last               7423
_journal_paper_doi               10.1021/ic800778j
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C50 H66 N2 O4 U'
_chemical_formula_weight         997.08
_chemical_name_systematic
;
(bis(diisopropylphenyl)pentane-2,4-di-iminato)dioxo uranium(dibenzoylmethanate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.090(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8812(10)
_cell_length_b                   22.638(2)
_cell_length_c                   18.8387(17)
_cell_measurement_temperature    150(2)
_cell_volume                     4639.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0718
_diffrn_reflns_av_sigmaI/netI    0.1397
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25197
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    3.542
_exptl_absorpt_correction_T_max  0.331
_exptl_absorpt_correction_T_min  0.151
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.882
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.824
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9259
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                4892
_reflns_number_total             9259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800778j-file001_2.cif
_cod_data_source_block           th209
_cod_original_cell_volume        4639.6(7)
_cod_database_code               4305840