Silylation of the Uranyl Ion Using B(C6F5)3-Activated Et3SiH
David D. Schnaars; Guang Wu; Trevor W. Hayton; Inorganic Chemistry 50 (2011) 9642–9649; doi:10.1021/ic201385h

data_4326400
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W Hayton'
_publ_section_title
;
 Silylation of the Uranyl Ion Using B(C6F5)3-Activated Et3SiH
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9642
_journal_page_last               9649
_journal_paper_doi               10.1021/ic201385h
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C70 H94 N2 O4 Si2 U'
_chemical_formula_weight         1321.68
_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                 97.991(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6522(8)
_cell_length_b                   17.5193(10)
_cell_length_c                   15.3466(9)
_cell_measurement_temperature    150(2)
_cell_volume                     3368.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26773
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    2.491
_exptl_absorpt_correction_T_max  0.29406
_exptl_absorpt_correction_T_min  0.24118
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            Dark-Red
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0703
_reflns_number_gt                4503
_reflns_number_total             6764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201385h_si_001_3.cif
_cod_data_source_block           3
_cod_database_code               4326400