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_4325358
_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            'C116 H117 B Co F15 N2 O4 Si U'
_chemical_formula_weight         2223.98
_chemical_name_systematic
; 
 ?
;
_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                 90.449(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.581(2)
_cell_length_b                   30.018(4)
_cell_length_c                   20.994(3)
_cell_measurement_temperature    150(2)
_cell_volume                     10449(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 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.1304
_diffrn_reflns_av_sigmaI/netI    0.1645
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55887
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.798
_exptl_absorpt_correction_T_max  0.29886
_exptl_absorpt_correction_T_min  0.21541
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            Dark_Orange
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       Block
_exptl_crystal_F_000             4528
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.735
_refine_diff_density_min         -4.519
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.293
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1150
_refine_ls_number_reflns         20098
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.291
_refine_ls_R_factor_all          0.1895
_refine_ls_R_factor_gt           0.1336
_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^)+(0.0798P)^2^+63.2176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2331
_refine_ls_wR_factor_ref         0.2542
_reflns_number_gt                13327
_reflns_number_total             20098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2008649_si_002_2.cif
_cod_data_source_block           2
_cod_database_code               4325358