An Intermediate Cobalt(IV) Nitrido Complex and its N-Migratory Insertion Product.
Zolnhofer, Eva M.; Käß, Martina; Khusniyarov, Marat M.; Heinemann, Frank W.; Maron, Laurent; van Gastel, Maurice; Bill, Eckhard; Meyer, Karsten; Journal of the American Chemical Society 136 (2014) 15072–15078; doi:10.1021/ja508144j

data_4122752
_publ_section_title
;
 An Intermediate Cobalt(IV) Nitrido Complex and its N-Migratory Insertion
 Product.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15072
_journal_page_last               15078
_journal_paper_doi               10.1021/ja508144j
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C46 H57 Co N6 O, C24 H20 B'
_chemical_formula_sum            'C70 H77 B Co N6 O'
_chemical_formula_weight         1088.12
_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                 114.012(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8314(7)
_cell_length_b                   17.0079(7)
_cell_length_c                   20.8227(8)
_cell_measurement_reflns_used    7180
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.70
_cell_measurement_theta_min      4.33
_cell_volume                     5768.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37354
_diffrn_reflns_theta_full        67.70
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.76
_exptl_absorpt_coefficient_mu    2.713
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.381
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         10342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0600P)^2^+3.8942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                8177
_reflns_number_total             10342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja508144j_si_002.cif
_cod_data_source_block           ez1301_cu
_cod_depositor_comments
'Adding full bibliography for 4122752--4122753.cif.'
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4122752