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_4305841
_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            'C82 H106 Co N2 O5 U'
_chemical_formula_weight         1496.65
_chemical_name_systematic
;
 (bis(diisopropylphenyl)pentane-2,4-di-iminato)dioxouranium(v)dibenzoylmethanate
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 101.739(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.905(3)
_cell_length_b                   18.632(5)
_cell_length_c                   14.527(4)
_cell_measurement_temperature    150(2)
_cell_volume                     3684.9(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.2486
_diffrn_reflns_av_sigmaI/netI    0.3401
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26971
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    2.471
_exptl_absorpt_correction_T_max  0.318
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1542
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.728
_refine_diff_density_min         -2.186
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       0.0120(9)
_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   0.861
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6853
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.2446
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1236P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.2487
_reflns_number_gt                2420
_reflns_number_total             6853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800778j-file001_3.cif
_cod_data_source_block           th_3_01a
_cod_original_cell_volume        3685.0(16)
_cod_database_code               4305841