Lewis Acid-Mediated β-Hydride Abstraction Reactions of Divalent M(C(SiHMe2)3)2THF2(M = Ca, Yb)
KaKing Yan; Brianna M. Upton; Arkady Ellern; Aaron D. Sadow; Journal of the American Chemical Society 131 (2009) 15110–15111; doi:10.1021/ja9070865

data_4105212
_publ_contact_author_address
;1605 Gilman Hall
Department of Chemistry
Iowa State University
Ames IA 50011
;
_publ_contact_author_email       sadow@iastate.edu
_publ_contact_author_fax         5152940105
_publ_contact_author_name        'Aaron D. Sadow'
_publ_contact_author_phone       5152948069
_publ_section_title
;
 Lewis Acid-Mediated \b-Hydride Abstraction Reactions of Divalent
 M(C(SiHMe2)3)2THF2(M = Ca, Yb)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15110
_journal_page_last               15111
_journal_paper_doi               10.1021/ja9070865
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C40 H40 B2 O Yb, C7 H8'
_chemical_formula_sum            'C47 H48 B2 O Yb'
_chemical_formula_weight         823.51
_chemical_melting_point          438
_chemical_name_common            Yb(HBPh3)2THF
_chemical_name_systematic
'bis(hydridotriphenylborato)tetrahydrofuran ytterbium(II)'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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                   10.2093(8)
_cell_length_b                   15.3491(12)
_cell_length_c                   24.6786(19)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.39
_cell_volume                     3867.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40159
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.56
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.453
_exptl_absorpt_correction_T_max  0.7252
_exptl_absorpt_correction_T_min  0.5168
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_recrystallization_method
'diffusion of pentane into toluene solution'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.042(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         9665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.0341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0559
_reflns_number_gt                9010
_reflns_number_total             9665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9070865_si_006.cif
_cod_data_source_block           YbHBPh3-dication
_cod_database_code               4105212