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_4107415
_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            'C75 H93 F3 N2 O7 P2 S U'
_chemical_formula_weight         1523.54
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.114(5)
_cell_length_b                   20.457(3)
_cell_length_c                   20.698(3)
_cell_measurement_temperature    150(2)
_cell_volume                     14021(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1706
_diffrn_reflns_av_sigmaI/netI    0.1964
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            111954
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    2.453
_exptl_absorpt_correction_T_max  0.272
_exptl_absorpt_correction_T_min  0.223
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       rod
_exptl_crystal_F_000             6224
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.107
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         14303
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.1521
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0583P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                5823
_reflns_number_total             14303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja077538q-file002_4.cif
_cod_data_source_block           th195squeeze
_cod_original_cell_volume        14020(3)
_cod_database_code               4107415