Catalytic C-H Bond Amination from High-Spin Iron Imido Complexes
Evan R. King; Elisabeth T. Hennessy; Theodore A. Betley; Journal of the American Chemical Society 133 (2011) 4917–4923; doi:10.1021/ja110066j

data_4105856
_publ_contact_author_address
;Department of Chemistry and Chemical Biology
Harvard University
Mallinckrodt 306E
12 Oxford Street
Cambridge, MA 02138
;
_publ_contact_author_email       betley@chemistry.harvard.edu
_publ_contact_author_name        'Professor Theodore A. Betley'
_publ_contact_author_phone       617-496-9944
_publ_section_title
;
 Catalytic C-H Bond Amination from High-Spin Iron Imido Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4917
_journal_page_last               4923
_journal_paper_doi               10.1021/ja110066j
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C144 H108 Cl2 Fe2 N6, 4(C6 H6)'
_chemical_formula_sum            'C168 H132 Cl2 Fe2 N6'
_chemical_formula_weight         2417.40
_chemical_name_common            ((ArDpme)FeCl(NC6H5))2
_chemical_name_systematic
;
bis(5-mesityl-1,9-di(2,4,6-triphenylphenyl)dipyrromethenato) diiron(III) 
dichloride mu-(N-imidocyclohexa-2,5-dien-1-yl)anilide
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                94.3420(10)
_cell_angle_beta                 93.7780(10)
_cell_angle_gamma                102.9270(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4691(12)
_cell_length_b                   21.4975(18)
_cell_length_c                   23.560(2)
_cell_measurement_reflns_used    7208
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.776
_cell_measurement_theta_min      2.299
_cell_volume                     7096.2(10)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX II (Bruker AXS, 2009)'
_computing_data_reduction        'SADABS (Bruker AXS, 2009)'
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
A short history of SHELX (Sheldrick, 2007)/Bruker
;
_diffrn_ambient_temperature      273.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_av_sigmaI/netI    0.1122
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            120338
_diffrn_reflns_theta_full        26.79
_diffrn_reflns_theta_max         26.79
_diffrn_reflns_theta_min         1.55
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2008/1 (Bruker,2008) was used for absorption correction.
 R(int) was 0.0701 before and 0.0545 after correction.
 The Ratio of minimum to maximum transmission is 0.85260193133.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            purple
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       prism
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
Disordered hexane molecules with low occupancy were removed because residual 
density was insufficient for modeling
;
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1603
_refine_ls_number_reflns         30299
_refine_ls_number_restraints     1661
_refine_ls_restrained_S_all      0.858
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0708P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1449
_reflns_number_gt                14949
_reflns_number_total             30299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja110066j_si_002_5.cif
_cod_data_source_block           ArDpmeFeClNC6H52
_cod_original_cell_volume        7096.1(10)
_cod_database_code               4105856