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_1576459
_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         'C33 H18 F6 Fe N3'
_chemical_formula_sum            'C33 H18 F6 Fe N3'
_chemical_formula_weight         626.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-03-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2024-07-30 deposited with the CCDC.	2026-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.10500(10)
_cell_length_b                   23.3523(2)
_cell_length_c                   12.21890(10)
_cell_measurement_reflns_used    18880
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      78.9570
_cell_measurement_theta_min      3.7860
_cell_volume                     2573.17(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_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      99.99(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 0.987
_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   -120.00 -35.00   0.50    4.28    --  -47.28 -37.00 134.00  170
  2  \w    -37.00  26.00   0.50    4.28    --  -47.28  37.00 -69.00  126
  3  \w     35.00 121.00   0.50    4.28    --   47.28  37.00 -69.00  172
  4  \w    -26.00  41.00   0.50    4.28    --   47.28 -37.00 134.00  134
  5  \w   -165.00 -79.00   0.50   17.13    --  -91.75 -37.00 134.00  172
  6  \w    101.00 178.00   0.50   17.13    --  113.25  37.00 -69.00  154
  7  \w    -86.00 -13.00   0.50    4.28    --  -47.28 125.00  30.00  146
  8  \w    -14.00  28.00   0.50    4.28    --  -47.28  19.00  60.00   84
  9  \w    -14.00  28.00   0.50    4.28    --  -47.28  19.00  90.00   84
 10  \w    -47.00 -20.00   0.50   17.13    --  -91.75  45.00 150.00   54
 11  \w    -47.00 -20.00   0.50   17.13    --  -91.75  45.00  90.00   54
 12  \w     42.00  76.00   0.50   17.13    --  113.25 -61.00  30.00   68
 13  \w     44.00 111.00   0.50   17.13    --  113.25-125.00  90.00  134
 14  \w    101.00 178.00   0.50   17.13    --  113.25  30.00-150.00  154
 15  \w    101.00 178.00   0.50   17.13    --  113.25  30.00-120.00  154
 16  \w     42.00 136.00   0.50   17.13    --  113.25 -77.00 -90.00  188
 17  \w     42.00  76.00   0.50   17.13    --  113.25 -61.00  90.00   68
 18  \w     42.00  76.00   0.50   17.13    --  113.25 -61.00 -90.00   68
 19  \w    101.00 178.00   0.50   17.13    --  113.25  30.00 120.00  154
 20  \w     42.00  76.00   0.50   17.13    --  113.25 -61.00 120.00   68
 21  \w     44.00 111.00   0.50   17.13    --  113.25-125.00 -60.00  134
 22  \w     42.00 136.00   0.50   17.13    --  113.25 -77.00  90.00  188
 23  \w     42.00  76.00   0.50   17.13    --  113.25 -61.00 -30.00   68
 24  \w     42.00  76.00   0.50   17.13    --  113.25 -61.00-180.00   68
 25  \w     44.00 111.00   0.50   17.13    --  113.25-125.00-150.00  134
 26  \w     42.00 106.00   0.50   17.13    --  113.25 -94.00-180.00  128
 27  \w     42.00  76.00   0.50   17.13    --  113.25 -61.00   0.00   68
 28  \w     42.00 106.00   0.50   17.13    --  113.25 -94.00 150.00  128
 29  \w     42.00 106.00   0.50   17.13    --  113.25 -94.00  90.00  128
 30  \w     32.00 120.00   0.50    4.28    --   47.28  57.00 -30.00  176
 31  \w     25.00 120.00   0.50    4.28    --   47.28  77.00  90.00  190
 32  \w     35.00 120.00   0.50    4.28    --   47.28  38.00  60.00  170
 33  \w     34.00  93.00   0.50    4.28    --   47.28-125.00 -30.00  118
 34  \w     25.00 120.00   0.50    4.28    --   47.28  77.00   0.00  190
 35  \w     25.00 120.00   0.50    4.28    --   47.28  77.00-120.00  190
 36  \w     25.00 120.00   0.50    4.28    --   47.28  77.00-180.00  190
 37  \w    101.00 150.00   0.50   17.13    --  113.25  45.00 -30.00   98
 38  \w    101.00 178.00   0.50   17.13    --  113.25  30.00  30.00  154
;
_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      -0.0256698000
_diffrn_orient_matrix_UB_12      0.0261931000
_diffrn_orient_matrix_UB_13      0.1114860000
_diffrn_orient_matrix_UB_21      0.1649285000
_diffrn_orient_matrix_UB_22      0.0169745000
_diffrn_orient_matrix_UB_23      0.0229376000
_diffrn_orient_matrix_UB_31      -0.0364799000
_diffrn_orient_matrix_UB_32      0.0581232000
_diffrn_orient_matrix_UB_33      -0.0569517000
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41066
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.348
_diffrn_reflns_theta_min         3.786
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.361
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.80a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       needle
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0600P)^2^+1.6186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4954
_reflns_number_total             5567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08832a2.cif
_cod_data_source_block           neiar22
_cod_depositor_comments
'Adding full bibliography for 1576451--1576463.cif.'
_cod_database_code               1576459
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.536
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C15(H15),
 C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C26(H26), C30(H30), C31(H31),
  C32(H32), C33(H33)
;
_shelx_res_checksum              96283
_olex2_submission_original_sample_id neiar22
_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 1.324
_oxdiff_exptl_absorpt_empirical_full_min 0.783