Copper-Catalyzed Regiodivergent Silacarboxylation of Allenes with Carbon Dioxide and a Silylborane.
Tani, Yosuke; Fujihara, Tetsuaki; Terao, Jun; Tsuji, Yasushi; Journal of the American Chemical Society  (2014) 141212124847001–; doi:10.1021/ja512040c

data_4123090
_publ_section_title
;
 Copper-Catalyzed Regiodivergent Silacarboxylation of Allenes with Carbon
 Dioxide and a Silylborane.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141212124847001
_journal_paper_doi               10.1021/ja512040c
_journal_year                    2014
_chemical_formula_moiety         'C10 H10 O2 Si'
_chemical_formula_sum            'C10 H10 O2 Si'
_chemical_formula_weight         190.27
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                68.123(11)
_cell_angle_beta                 83.058(14)
_cell_angle_gamma                77.859(14)
_cell_formula_units_Z            4
_cell_length_a                   6.799(2)
_cell_length_b                   17.085(5)
_cell_length_c                   17.516(5)
_cell_measurement_reflns_used    3032
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.07
_cell_volume                     1843.9(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15128
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             400.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.480
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     397
_refine_ls_number_reflns         8093
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0990P)^2^+0.5433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2242
_reflns_number_gt                5467
_reflns_number_total             8093
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja512040c_si_002.cif
_cod_data_source_block           tani130204b
_cod_original_cell_volume        1843.9(10)
_cod_database_code               4123090