Cobalt-catalyzed trimethylsilylmethylmagnesium-promoted radical alkenylation of alkyl halides: a complement to the Heck reaction.
Affo, Walter; Ohmiya, Hirohisa; Fujioka, Takuma; Ikeda, Yousuke; Nakamura, Tomoaki; Yorimitsu, Hideki; Oshima, Koichiro; Imamura, Yuki; Mizuta, Tsutomu; Miyoshi, Katsuhiko; Journal of the American Chemical Society 128 (2006) 8068–8077; doi:10.1021/ja061417t

data_4101285
_publ_section_title
;
 Cobalt-catalyzed trimethylsilylmethylmagnesium-promoted radical
 alkenylation of alkyl halides: a complement to the Heck reaction.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8068
_journal_page_last               8077
_journal_paper_doi               10.1021/ja061417t
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C69 H82 Cl4 Co2 O3 P4'
_chemical_formula_weight         1343.0
_chemical_name_systematic
; 
 dichlorobis(1,6-bisdiphenylphosphinohexane)cobalt 
;
_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                75.2910(10)
_cell_angle_beta                 66.2910(10)
_cell_angle_gamma                65.1760(10)
_cell_formula_units_Z            2
_cell_length_a                   15.3800(2)
_cell_length_b                   15.4040(2)
_cell_length_c                   18.3530(4)
_cell_measurement_temperature    200(2)
_cell_volume                     3594.25(10)
_computing_cell_refinement       HKL
_computing_data_collection       HKL
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Mac Science DIP2030 Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15654
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  0.8970
_exptl_absorpt_correction_T_min  0.7660
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' blue'
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ' cubic'
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0056(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         15654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          2.059
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+5.1013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1617
_reflns_number_gt                11530
_reflns_number_total             15654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja061417tsi20060301_012931.cif
_cod_data_source_block           CoCl2dpph
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4101285