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_4105854
_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         'C66 H50 N2, 3(C6 H6)'
_chemical_formula_sum            'C84 H68 N2'
_chemical_formula_weight         1105.40
_chemical_name_common            (ArDpme)H
_chemical_name_systematic
;
5-mesityl-1,9-di(2,4,6-triphenylphenyl)dipyrromethene
;
_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                75.509(2)
_cell_angle_beta                 85.664(2)
_cell_angle_gamma                65.022(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5350(5)
_cell_length_b                   13.6512(6)
_cell_length_c                   20.4250(8)
_cell_measurement_reflns_used    16710
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.187
_cell_volume                     3065.6(2)
_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      99.84
_diffrn_detector_area_resol_mean 8.0
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41971
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.76
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2008/1 (Bruker,2008) was used for absorption correction.
 R(int) was 0.0834 before and 0.0489 after correction.
 The Ratio of minimum to maximum transmission is 0.828326180258.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         12519
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0476P)^2^+0.9970P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                9929
_reflns_number_total             12519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja110066j_si_002_3.cif
_cod_data_source_block           ArDpmeH
_cod_database_code               4105854