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_4107412
_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 H82 Cl2 N4 O4 U2'
_chemical_formula_weight         1446.24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.570(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.803(3)
_cell_length_b                   14.124(2)
_cell_length_c                   24.465(4)
_cell_measurement_temperature    150(1)
_cell_volume                     5953.9(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.1191
_diffrn_reflns_av_sigmaI/netI    0.1733
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            40348
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    5.568
_exptl_absorpt_correction_T_max  0.394
_exptl_absorpt_correction_T_min  0.243
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       plate
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.671
_refine_diff_density_min         -1.942
_refine_diff_density_rms         0.464
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         11818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                6128
_reflns_number_total             11818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja077538q-file002_1.cif
_cod_data_source_block           th191
_cod_original_cell_volume        5954.0(16)
_cod_database_code               4107412