A Zwitterionic Carbanion Frustrated by Boranes - Dihydrogen Cleavage with Weak Lewis Acids via an "Inverse" Frustrated Lewis Pair Approach
Hui Li; Adelia J. A. Aquino; David B. Cordes; Fernando Hung-Low; William L. Hase; Clemens Krempner; Journal of the American Chemical Society 135 (2013) 16066–16069; doi:10.1021/ja409330h

data_4121076
_publ_contact_author_address
;Department of Chemistry and Biochemistry
Texas Tech University
Lubbock, TX 79409
USA
;
_publ_contact_author_email       Clemens.Krempner@ttu.edu
_publ_contact_author_name        'Clemens Krempner'
_publ_section_title
;
 A Zwitterionic Carbanion Frustrated by Boranes - Dihydrogen Cleavage with
 Weak Lewis Acids via an "Inverse" Frustrated Lewis Pair Approach
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16066
_journal_page_last               16069
_journal_paper_doi               10.1021/ja409330h
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C16 H40 Na O6 Si3, C18 H16 B, C4 H8 O'
_chemical_formula_sum            'C38 H64 B Na O7 Si3'
_chemical_formula_weight         750.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   12.568(3)
_cell_length_b                   12.568(3)
_cell_length_c                   15.851(3)
_cell_measurement_reflns_used    4921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.94
_cell_measurement_theta_min      2.27
_cell_volume                     2168.3(8)
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26750
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.9919
_exptl_absorpt_correction_T_min  0.9350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       platelet
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The SQUEEZED electron density of 82 e^-^/cell was accounted for as two
 molecules of THF solvent, at 40 e^-^ each.  This allows for one molecule of
 THF per complex.  This solvent has been included in the final formula, formula
 weight, calculated density, \m and F(000).
;
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         3475
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1344P)^2^+0.5920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2262
_refine_ls_wR_factor_ref         0.2442
_reflns_number_gt                2433
_reflns_number_total             3475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409330h_si_003_3.cif
_cod_data_source_block           4
_cod_original_cell_volume        2168.2(7)
_cod_database_code               4121076