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_1576461
_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 H15 F9 Fe N3'
_chemical_formula_sum            'C33 H15 F9 Fe N3'
_chemical_formula_weight         680.33
_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
_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                 98.1220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.46120(10)
_cell_length_b                   23.5947(2)
_cell_length_c                   12.11550(10)
_cell_measurement_reflns_used    15525
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.0960
_cell_measurement_theta_min      5.0650
_cell_volume                     2677.47(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, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_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    -82.00  -2.00   0.50    1.25    --  -47.03 111.00-131.00  160
  2  \w     24.00  84.00   0.50    1.25    --   47.03-111.00 134.00  120
  3  \w   -160.00 -81.00   0.50    5.00    --  -91.75-111.00 134.00  158
  4  \w    -82.00 -23.00   0.50    5.00    --  -91.75 111.00-131.00  118
  5  \w     45.00 108.00   0.50    5.00    --  113.25-111.00 134.00  126
  6  \w    103.00 178.00   0.50    5.00    --  113.25 111.00-131.00  150
  7  \w    -14.00  28.00   0.50    1.25    --  -47.03  19.00 120.00   84
  8  \w    -14.00  28.00   0.50    1.25    --  -47.03  19.00 -30.00   84
  9  \w    -14.00  28.00   0.50    1.25    --  -47.03  19.00   0.00   84
 10  \w   -119.00 -32.00   0.50    1.25    --  -47.03 -57.00  30.00  174
 11  \w    -14.00  28.00   0.50    1.25    --  -47.03  19.00-150.00   84
 12  \w    -47.00 -20.00   0.50    5.00    --  -91.75  45.00-180.00   54
 13  \w    -47.00 -20.00   0.50    5.00    --  -91.75  45.00  90.00   54
 14  \w    100.00 178.00   0.50    5.00    --  113.25  15.00 -30.00  156
 15  \w     42.00  76.00   0.50    5.00    --  113.25 -61.00-150.00   68
 16  \w     42.00  76.00   0.50    5.00    --  113.25 -61.00 -30.00   68
 17  \w     42.00 106.00   0.50    5.00    --  113.25 -94.00  60.00  128
 18  \w     42.00 136.00   0.50    5.00    --  113.25 -77.00-180.00  188
 19  \w     42.00  76.00   0.50    5.00    --  113.25 -61.00-180.00   68
 20  \w     42.00  76.00   0.50    5.00    --  113.25 -61.00 120.00   68
 21  \w     42.00  76.00   0.50    5.00    --  113.25 -61.00  30.00   68
 22  \w     97.00 178.00   0.50    5.00    --  113.25  61.00 -90.00  162
 23  \w     42.00 106.00   0.50    5.00    --  113.25 -94.00 150.00  128
 24  \w    100.00 178.00   0.50    5.00    --  113.25  15.00   0.00  156
 25  \w     42.00 106.00   0.50    5.00    --  113.25 -94.00-180.00  128
 26  \w     42.00 106.00   0.50    5.00    --  113.25 -94.00  30.00  128
 27  \w     44.00 111.00   0.50    5.00    --  113.25-125.00 -90.00  134
 28  \w     42.00  76.00   0.50    5.00    --  113.25 -61.00 -60.00   68
 29  \w     42.00 106.00   0.50    5.00    --  113.25 -94.00  90.00  128
 30  \w     42.00  76.00   0.50    5.00    --  113.25 -61.00 -90.00   68
 31  \w   -120.00 -24.00   0.50    1.25    --  -47.03 -77.00 -60.00  192
 32  \w   -119.00 -32.00   0.50    1.25    --  -47.03 -57.00 120.00  174
 33  \w   -119.00 -64.00   0.50    1.25    --  -47.03 -57.00 -30.00  110
 34  \w   -120.00 -34.00   0.50    1.25    --  -47.03 -38.00-180.00  172
;
_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      0.0154082000
_diffrn_orient_matrix_UB_12      0.0639224000
_diffrn_orient_matrix_UB_13      0.0247691000
_diffrn_orient_matrix_UB_21      0.1364373000
_diffrn_orient_matrix_UB_22      0.0015438000
_diffrn_orient_matrix_UB_23      -0.0558690000
_diffrn_orient_matrix_UB_31      -0.0903633000
_diffrn_orient_matrix_UB_32      0.0132713000
_diffrn_orient_matrix_UB_33      -0.1130349000
_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  0.0352
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33566
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.187
_diffrn_reflns_theta_min         3.747
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81725
_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    1.688
_exptl_crystal_description       plate
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+2.5292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5139
_reflns_number_total             5726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08832a2.cif
_cod_data_source_block           neiar21
_cod_depositor_comments
'Adding full bibliography for 1576451--1576463.cif.'
_cod_database_code               1576461
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         FeN3F9C33H21
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.567
_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), C11(H11), C13(H13), C15(H15), C19(H19),
 C20(H20), C22(H22), C24(H24), C26(H26), C30(H30), C31(H31), C33(H33)
;
_shelx_res_checksum              15990
_olex2_submission_original_sample_id neiar21
_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 1.211
_oxdiff_exptl_absorpt_empirical_full_min 0.848