Synthesis, Structure of Borylmagnesium, and Its Reaction with Benzaldehyde to Form Benzoylborane
Makoto Yamashita; Yuta Suzuki; Yasutomo Segawa; Kyoko Nozaki; Journal of the American Chemical Society 129 (2007) 9570–9571; doi:10.1021/ja073037t

data_4109748
_publ_section_title
;
 Synthesis, Structure of Borylmagnesium, and Its Reaction with
 Benzaldehyde to Form Benzoylborane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9570
_journal_page_last               9571
_journal_paper_doi               10.1021/ja073037t
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C34 H52 B Br Mg N2 O2'
_chemical_formula_weight         635.81
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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                   13.305(6)
_cell_length_b                   13.785(6)
_cell_length_c                   19.459(8)
_cell_measurement_reflns_used    8824
_cell_measurement_temperature    103.1500
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0631
_cell_volume                     3569(3)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'RIGAKU/MSC Meacury CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23442
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_T_max  0.8406
_exptl_absorpt_correction_T_min  0.6144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       Block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack (1983), 2762 Friedel pairs'
_refine_ls_abs_structure_Flack   0.008(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         6279
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0741
_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^)+(0.0292P)^2^+5.7238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                5393
_reflns_number_total             6279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073037tsi20070705_014209.cif
_cod_data_source_block           3
_cod_database_code               4109748