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_4113650
_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            'C62 H102 B2 Co2 N14 Si2'
_chemical_formula_weight         1239.24
_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                88.925(2)
_cell_angle_beta                 79.172(2)
_cell_angle_gamma                79.722(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7096(10)
_cell_length_b                   12.3659(11)
_cell_length_c                   12.3697(10)
_cell_measurement_temperature    173(2)
_cell_volume                     1730.8(3)
_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 0.725
_diffrn_measured_fraction_theta_max 0.725
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8279
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.8961
_exptl_absorpt_correction_T_min  0.8498
_exptl_absorpt_correction_type   'empirical from SADABS'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       Block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0584
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1766
_reflns_number_gt                4187
_reflns_number_total             5478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028267gsi20030109_040711_1.cif
_cod_data_source_block           sun12
_cod_database_code               4113650