Synthesis, Characterization, and Reactivity of a Uranyl β-Diketiminate Complex
Trevor W. Hayton; Guang Wu; Journal of the American Chemical Society 130 (2008) 2005–2014; doi:10.1021/ja077538q

data_4107417
_publ_contact_author             'Trevor W. Hayton'
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of a Uranyl \b-Diketiminate
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2005
_journal_page_last               2014
_journal_paper_doi               10.1021/ja077538q
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C58.5 H71 N2 O4 P2 U'
_chemical_formula_weight         1166.14
_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                109.824(3)
_cell_angle_beta                 106.438(3)
_cell_angle_gamma                90.834(3)
_cell_formula_units_Z            2
_cell_length_a                   20.737(4)
_cell_length_b                   10.882(2)
_cell_length_c                   14.340(3)
_cell_measurement_temperature    150(2)
_cell_volume                     2897.8(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.1477
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23899
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    2.899
_exptl_absorpt_correction_T_max  0.528
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.382
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         11640
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                7438
_reflns_number_total             11640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja077538q-file002_6.cif
_cod_data_source_block           th_2_56
_cod_original_cell_volume        2897.8(9)
_cod_original_formula_sum        'C58.50 H71 N2 O4 P2 U'
_cod_database_code               4107417