Photolysis and Thermolysis of Bis(imino)pyridine Cobalt Azides: C-H Activation from Putative Cobalt Nitrido Complexes
Crisita Carmen Hojilla Atienza; Amanda C. Bowman; Emil Lobkovsky; Paul J. Chirik; Journal of the American Chemical Society 132 (2010) 16343–16345; doi:10.1021/ja107288x

data_4103548
_publ_section_title
;
 Photolysis and Thermolysis of Bis(imino)pyridine Cobalt Azides: C-H
 Activation from Putative Cobalt Nitrido Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16343
_journal_page_last               16345
_journal_paper_doi               10.1021/ja107288x
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C37 H35 Co N4'
_chemical_formula_sum            'C37 H35 Co N4'
_chemical_formula_weight         594.62
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.844(3)
_cell_angle_beta                 101.392(3)
_cell_angle_gamma                103.947(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8980(6)
_cell_length_b                   13.3037(8)
_cell_length_c                   13.8290(8)
_cell_measurement_reflns_used    8215
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.32
_cell_volume                     1670.19(18)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23051
_diffrn_reflns_theta_full        28.60
_diffrn_reflns_theta_max         28.60
_diffrn_reflns_theta_min         1.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.9230
_exptl_absorpt_correction_T_min  0.8120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details          ' '
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         8338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+0.9292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                6100
_reflns_number_total             8338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107288x_si_001_3.cif
_cod_data_source_block           cca7
_cod_original_cell_volume        1670.19(17)
_cod_database_code               4103548