Oxo Ligand Silylation in a Uranyl β-Ketoiminate Complex
Jessie L. Brown; Guang Wu; Trevor W. Hayton; Journal of the American Chemical Society 132 (2010) 7248–7249; doi:10.1021/ja1013739

data_4102473
_publ_section_title
;
 Oxo Ligand Silylation in a Uranyl \b-Ketoiminate Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7248
_journal_page_last               7249
_journal_paper_doi               10.1021/ja1013739
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C68 H86 F6 N2 O12 S2 U'
_chemical_formula_weight         1539.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   15.8994(10)
_cell_length_b                   19.2681(13)
_cell_length_c                   22.9828(14)
_cell_measurement_temperature    150(2)
_cell_volume                     7040.8(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_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  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0973
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            60336
_diffrn_reflns_theta_full        27.67
_diffrn_reflns_theta_max         27.67
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    2.439
_exptl_absorpt_correction_T_max  0.279
_exptl_absorpt_correction_T_min  0.213
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.056
_refine_diff_density_min         -1.345
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.036(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         15152
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0951P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                10816
_reflns_number_total             15152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1013739_si_001_2.cif
_cod_data_source_block           complex4
_cod_database_code               4102473