Enantioselective Preparation of a Stable Boronate Complex Stereogenic Only at Boron
Peter F. Kaiser; Jonathan M. White; Craig A. Hutton; Journal of the American Chemical Society 130 (2008) 16450–16451; doi:10.1021/ja8044629

data_4108786
_publ_section_title
;
 Enantioselective Preparation of a Stable Boronate Complex Stereogenic
 Only at Boron
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16450
_journal_page_last               16451
_journal_paper_doi               10.1021/ja8044629
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C25 H18 B N O3'
_chemical_formula_weight         391.21
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.372(10)
_cell_angle_beta                 95.847(9)
_cell_angle_gamma                98.583(12)
_cell_formula_units_Z            2
_cell_length_a                   5.936(3)
_cell_length_b                   10.222(5)
_cell_length_c                   16.668(9)
_cell_measurement_reflns_used    720
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.96
_cell_measurement_theta_min      2.50
_cell_volume                     978.4(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0777
_diffrn_reflns_av_sigmaI/netI    0.1297
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4521
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       rod
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.845
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.845
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1370
_reflns_number_gt                1781
_reflns_number_total             3333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8044629_si_002.cif
_cod_data_source_block           jmwpk2
_cod_original_cell_volume        978.3(8)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4108786