Reduction of Pentavalent Uranyl to U(IV) Facilitated by Oxo Functionalization
David D. Schnaars; Guang Wu; Trevor W. Hayton; Journal of the American Chemical Society 131 (2009) 17532–17533; doi:10.1021/ja906880d

data_4105428
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W Hayton'
_publ_section_title
;
 Reduction of Pentavalent Uranyl to U(IV) Facilitated by Oxo
 Functionalization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17532
_journal_page_last               17533
_journal_paper_doi               10.1021/ja906880d
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C94 H85 B2 Cl2 Co F30 N O4 U'
_chemical_formula_weight         2252.11
_chemical_name_systematic
; 
 ? 
;
_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                100.010(2)
_cell_angle_beta                 97.933(2)
_cell_angle_gamma                91.626(2)
_cell_formula_units_Z            2
_cell_length_a                   13.443(2)
_cell_length_b                   16.074(2)
_cell_length_c                   21.500(3)
_cell_measurement_temperature    150(2)
_cell_volume                     4524.7(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_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  0.0809
_diffrn_reflns_av_sigmaI/netI    0.2035
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37164
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    2.144
_exptl_absorpt_correction_T_max  0.32753
_exptl_absorpt_correction_T_min  0.25815
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       Block
_exptl_crystal_F_000             2242
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.160
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         18084
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1868
_reflns_number_gt                8421
_reflns_number_total             18084
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906880d_si_002_1.cif
_cod_data_source_block           5
_cod_original_cell_volume        4524.7(12)
_cod_database_code               4105428