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_4122753
_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
;
 0.938(C46 H57 Co N6 O), 0.062(C46 H56 Co N6 O), Cl, C4 H8 O, 0.157(H2 O)
;
_chemical_formula_sum            'C50 H65.25 Cl Co N5.94 O2.16'
_chemical_formula_weight         878.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   19.0807(18)
_cell_length_b                   42.120(5)
_cell_length_c                   22.668(2)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.79
_cell_volume                     18218(3)
_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      120(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            73344
_diffrn_reflns_theta_full        27.16
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             7489
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.639
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         10051
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.671
_refine_ls_R_factor_all          0.0948
_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^)+(0.0260P)^2^+3.0278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                6982
_reflns_number_total             10051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja508144j_si_002.cif
_cod_data_source_block           mk1209b
_cod_depositor_comments
'Adding full bibliography for 4122752--4122753.cif.'
_cod_original_cell_volume        18217(3)
_cod_original_sg_symbol_Hall     -C2b2bc
_cod_original_sg_symbol_H-M      Ccca
_cod_database_code               4122753