Intramolecular C-H Activation by Inferred Terminal Cobalt Imido Intermediates
Sunita Thyagarajan; Daniel T. Shay; Christopher D. Incarvito; Arnold L. Rheingold; Klaus H. Theopold; Journal of the American Chemical Society 125 (2003) 4440–4441; doi:10.1021/ja028267g

data_4113651
_publ_section_title
;
 Intramolecular C-H Activation by Inferred Terminal Cobalt Imido
 Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4440
_journal_page_last               4441
_journal_paper_doi               10.1021/ja028267g
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C32 H61 B Co N7 Si'
_chemical_formula_weight         641.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 97.321(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4593(13)
_cell_length_b                   10.4460(11)
_cell_length_c                   29.652(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3827.7(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            15998
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  0.9509
_exptl_absorpt_correction_T_min  0.8623
_exptl_absorpt_correction_type   'empirical from SADABS'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.334
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         7137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.334
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.088
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.2026
_reflns_number_gt                5064
_reflns_number_total             7137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028267gsi20030109_040711_2.cif
_cod_data_source_block           sun10
_cod_original_cell_volume        3827.8(7)
_cod_database_code               4113651