Iron tris-mesityl: a homoleptic iron(ii) ferrate species for directed C–H activation
Radović, Aleksa; Healy, Maria C.; Datta, Arnadeep; Das, Deborshee; Cai, Likun; Diaz, Steven; Gogoi, Achyut Ranjan; Wolford, Nikki J.; Carpenter, Stephanie H.; Brenessel, William W.; McCamant, David; Gutierrez, Osvaldo; Neidig, Michael L.; Chemical Science  (2026) –; doi:10.1039/D5SC08832A

data_1576458
_publ_section_title
;
 Iron tris-mesityl: a homoleptic iron(ii) ferrate species for directed C-H
 activation.
;
_journal_issue                   14
_journal_name_full               'Chemical science'
_journal_page_first              7002
_journal_page_last               7009
_journal_paper_doi               10.1039/d5sc08832a
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C36 H30 Fe1 N3'
_chemical_formula_sum            'C36 H30 Fe N3'
_chemical_formula_weight         560.48
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-10-24
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-07-30 deposited with the CCDC.	2026-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.0750(4)
_cell_length_b                   15.0750(4)
_cell_length_c                   28.6238(8)
_cell_measurement_reflns_used    8655
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      77.7080
_cell_measurement_theta_min      3.7090
_cell_volume                     5633.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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   -119.00 -55.00   0.50    1.37    --  -47.15-151.00 -27.00  128
  2  \w    -82.00 -22.00   0.50    5.46    --  -91.75 110.00  34.00  120
  3  \w     44.00 108.00   0.50    5.46    --  113.25-110.00 -60.00  128
  4  \w    101.00 178.00   0.50    5.46    --  113.25  36.00  19.00  154
  5  \w     44.00 110.00   0.50    5.46    --  113.25-122.00 133.00  132
  6  \w    -14.00  28.00   0.50    1.37    --  -47.15  19.00 150.00   84
  7  \w    -14.00  28.00   0.50    1.37    --  -47.15  19.00 120.00   84
  8  \w    -14.00  28.00   0.50    1.37    --  -47.15  19.00   0.00   84
  9  \w     42.00  76.00   0.50    5.46    --  113.25 -61.00  30.00   68
 10  \w     42.00  76.00   0.50    5.46    --  113.25 -61.00  90.00   68
 11  \w     42.00 106.00   0.50    5.46    --  113.25 -94.00-150.00  128
 12  \w    101.00 178.00   0.50    5.46    --  113.25  30.00  60.00  154
 13  \w     44.00 111.00   0.50    5.46    --  113.25-125.00-180.00  134
 14  \w     42.00  76.00   0.50    5.46    --  113.25 -61.00-150.00   68
 15  \w     44.00 111.00   0.50    5.46    --  113.25-125.00 150.00  134
 16  \w     42.00  76.00   0.50    5.46    --  113.25 -61.00   0.00   68
 17  \w   -118.00 -32.00   0.50    1.37    --  -47.15 -57.00   0.00  172
 18  \w   -118.00 -32.00   0.50    1.37    --  -47.15 -57.00  90.00  172
 19  \w     25.00 120.00   0.50    1.37    --   47.15  77.00-180.00  190
 20  \w    100.00 163.00   0.50    5.46    --  113.25  15.00 -60.00  126
 21  \w     97.00 178.00   0.50    5.46    --  113.25  61.00 120.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1126238000
_diffrn_orient_matrix_UB_12      -0.0841406000
_diffrn_orient_matrix_UB_13      -0.0068235000
_diffrn_orient_matrix_UB_21      0.0251505000
_diffrn_orient_matrix_UB_22      -0.0192061000
_diffrn_orient_matrix_UB_23      -0.0498392000
_diffrn_orient_matrix_UB_31      0.0252512000
_diffrn_orient_matrix_UB_32      -0.0803621000
_diffrn_orient_matrix_UB_33      0.0190665000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            16014
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         81.301
_diffrn_reflns_theta_min         3.721
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.384
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.991
_exptl_crystal_description       block
_exptl_crystal_F_000             1758
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0651P)^2^+1.5663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2384
_reflns_number_total             2720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08832a2.cif
_cod_data_source_block           neiar15
_cod_depositor_comments
'Adding full bibliography for 1576451--1576463.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1576458
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.614
_shelx_estimated_absorpt_t_min   0.405
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              80300
_shelx_fab_checksum              92890
_olex2_submission_original_sample_id neiar15
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.580
_oxdiff_exptl_absorpt_empirical_full_min 0.665