Borane-Mediated Silylation of a Metal-Oxo Ligand
David D. Schnaars; Guang Wu; Trevor W. Hayton; Inorganic Chemistry 50 (2011) 4695–4697; doi:10.1021/ic2008649

data_4325357
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W Hayton'
_publ_section_title
;
 Borane-Mediated Silylation of a Metal-Oxo Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4695
_journal_page_last               4697
_journal_paper_doi               10.1021/ic2008649
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C125.5 H115 B F15 N2 O4 Si U'
_chemical_formula_weight         2277.13
_chemical_name_systematic
; 
 U(V)(OSiPh3)(OBCF)(AcNac)2 
;
_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                 98.161(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5521(19)
_cell_length_b                   19.1663(19)
_cell_length_c                   32.687(4)
_cell_measurement_temperature    150(2)
_cell_volume                     10885(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.1726
_diffrn_reflns_av_sigmaI/netI    0.1976
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            82693
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    1.583
_exptl_absorpt_correction_T_max  0.38966
_exptl_absorpt_correction_T_min  0.11509
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            Dark_Red
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4640
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.648
_refine_diff_density_min         -2.511
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1203
_refine_ls_number_reflns         22463
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.2012
_refine_ls_R_factor_gt           0.1051
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1158P)^2^+55.0798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2702
_reflns_number_gt                10838
_reflns_number_total             22463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2008649_si_002_1.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C125.50 H115 B F15 N2 O4 Si U'
_cod_database_code               4325357