Identification and Reactivity of Cyclometalated Iron(II) Intermediates in Triazole-Directed Iron-Catalyzed C-H Activation.
Boddie, Theresa E.; Carpenter, Stephanie H.; Baker, Tessa M.; DeMuth, Joshua C.; Cera, Gianpiero; Brennessel, William W.; Ackermann, Lutz; Neidig, Michael L.; Journal of the American Chemical Society 141 (2019) 12338–12345; doi:10.1021/jacs.9b05269

data_4128618
_publ_section_title
;
 Identification and Reactivity of Cyclometalated Iron(II) Intermediates in
 Triazole-Directed Iron-Catalyzed C-H Activation.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12338
_journal_page_last               12345
_journal_paper_doi               10.1021/jacs.9b05269
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C108 H104 Br0.55 Cl1.45 Fe2 Mg N8 O4 P4'
_chemical_formula_sum            'C108 H104 Br0.55 Cl1.45 Fe2 Mg N8 O4 P4'
_chemical_formula_weight         1933.17
_chemical_name_common            neiti17
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.2467(4)
_cell_length_b                   30.2467(4)
_cell_length_c                   40.3458(9)
_cell_measurement_reflns_used    26399
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.13
_cell_measurement_theta_min      2.36
_cell_volume                     36910.9(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -51.00 -13.00   0.50  219.58    --  -84.25  30.00   0.00   76
  2  \w   -109.00 -83.00   0.50   54.90    --  -49.62 162.00 -74.00   52
  3  \w   -140.00-115.00   0.50  219.58    --  -84.25-117.00  47.00   50
  4  \w   -119.00 -47.00   0.50   54.90    --  -49.62-162.00-102.00  144
  5  \w     61.00  86.00   0.50   54.90    --   49.62-162.00-102.00   50
  6  \w     54.00  81.00   0.50  219.58    --  105.75-117.00  47.00   54
  7  \w     34.00  72.00   0.50  219.58    --  105.75 -30.00 -90.00   76
  8  \w     33.00  82.00   0.50  219.58    --  105.75 -15.00 -30.00   98
  9  \w     37.00  72.00   0.50  219.58    --  105.75 -30.00-150.00   70
 10  \w     34.00  69.00   0.50  219.58    --  105.75 -30.00-180.00   70
 11  \w     68.00 158.00   0.50  219.58    --  105.75 162.00 -74.00  180
 12  \w    113.00 138.00   0.50  219.58    --  105.75 117.00 135.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0324898000
_diffrn_orient_matrix_UB_12      -0.0391814000
_diffrn_orient_matrix_UB_13      -0.0010881000
_diffrn_orient_matrix_UB_21      -0.0049689000
_diffrn_orient_matrix_UB_22      -0.0058685000
_diffrn_orient_matrix_UB_23      0.0377181000
_diffrn_orient_matrix_UB_31      -0.0389387000
_diffrn_orient_matrix_UB_32      -0.0320229000
_diffrn_orient_matrix_UB_33      -0.0056248000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0936
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            137719
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.150
_diffrn_reflns_theta_min         2.338
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.696
_exptl_crystal_description       needle
_exptl_crystal_F_000             8063
_exptl_crystal_size_max          0.471
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.039(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         37460
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0978P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1745
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.924
_reflns_number_gt                25726
_reflns_number_total             37460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05269_si_002.cif
_cod_data_source_block           neiti17
_cod_original_cell_volume        36910.9(13)
_cod_database_code               4128618
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.425
_shelx_estimated_absorpt_t_max   0.953
_shelx_res_checksum              27726
_shelx_hkl_checksum              5721
_shelx_fab_checksum              31196