Photochemically Promoted Transition Metal-Free Cross-Coupling of Acylsilanes with Organoboronic Esters
Kazuta Ito; Hiroto Tamashima; Nobuharu Iwasawa; Hiroyuki Kusama; Journal of the American Chemical Society 133 (2011) 3716–3719; doi:10.1021/ja1102597

data_4105774
_publ_section_title
;
 Photochemically Promoted Transition Metal-Free Cross-Coupling of
 Acylsilanes with Organoboronic Esters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3716
_journal_page_last               3719
_journal_paper_doi               10.1021/ja1102597
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C22 H29 B Br2 O3 Si'
_chemical_formula_weight         540.17
_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                98.365(2)
_cell_angle_beta                 111.260(4)
_cell_angle_gamma                105.751(5)
_cell_formula_units_Z            2
_cell_length_a                   11.106(5)
_cell_length_b                   11.266(5)
_cell_length_c                   11.436(5)
_cell_measurement_reflns_used    2894
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.3367
_cell_measurement_theta_min      2.3115
_cell_volume                     1235.1(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi 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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9728
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    3.350
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6173
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       prism
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.1900
_exptl_crystal_size_mid          0.1600
_exptl_crystal_size_min          0.1400
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0577P)^2^+0.5626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                4062
_reflns_number_total             5457
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1102597_si_001.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        1235.1(9)
_cod_database_code               4105774