Synthesis of Silaoxazolinium Salts Bearing Weakly Coordinating Anions: Structures and Catalytic Activities in the Aldol Reaction
Chandra Sheker Reddy, Anugu; Chen, Zhang; Hatanaka, Tohru; Minami, Tatsuya; Hatanaka, Yasuo; Organometallics 32 (2013) 3575–; doi:10.1021/om400017f

data_4080915
_publ_section_title
;
 Synthesis of Silaoxazolinium Salts Bearing Weakly Coordinating Anions:
 Structures and Catalytic Activities in the Aldol Reaction
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3575
_journal_paper_doi               10.1021/om400017f
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C10 H26 N O Si3, C32 H12 B F24''
_chemical_formula_sum            'C42 H38 B F24 N O Si3'
_chemical_formula_weight         1123.80
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.14(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.957(4)
_cell_length_b                   24.184(5)
_cell_length_c                   10.577(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     2546.9(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223.2
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9989
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.092
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6527
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_standards_decay_%        3.02
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psiscan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.414
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         5992
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.414
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1948
_refine_ls_wR_factor_ref         0.2143
_reflns_number_gt                3902
_reflns_number_total             5992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400017f_si_001.cif
_cod_data_source_block           2c
_cod_original_cell_volume        2547(1)
_cod_original_formula_sum        'C42 H38 B F24 N O Si3 '
_cod_database_code               4080915