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_1576457
_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_absolute_configuration ad
_chemical_formula_moiety         'C33 H18 F6 Fe N3, C18 H36 K N2 O6'
_chemical_formula_sum            'C51 H54 F6 Fe K N5 O6'
_chemical_formula_weight         1041.94
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-06-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-10-25 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            12
_cell_length_a                   14.66160(10)
_cell_length_b                   14.66160(10)
_cell_length_c                   75.2940(6)
_cell_measurement_reflns_used    96666
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.4840
_cell_measurement_theta_min      3.6490
_cell_volume                     14016.96(18)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (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      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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -31.00  26.00   0.38    0.25    --  -47.28  38.00 -44.00  150
  2  \w   -118.00 -72.78   0.38    0.25    --  -47.28-128.00 106.00  119
  3  \w     35.00 119.36   0.38    0.25    --   47.28  38.00 -44.00  222
  4  \w   -162.00 -72.70   0.38    1.00    --  -91.75-128.00 106.00  235
  5  \w    -79.00 -19.72   0.38    1.00    --  -91.75  92.00  75.00  156
  6  \w   -160.00 -81.72   0.38    1.00    --  -91.75-111.00  78.00  206
  7  \w   -163.00 -79.78   0.38    1.00    --  -91.75 -87.00  26.00  219
  8  \w    101.00 177.00   0.38    1.00    --  113.25  38.00 -44.00  200
  9  \w    103.00 176.72   0.38    1.00    --  113.25 111.00 173.00  194
 10  \w     42.00 103.94   0.38    1.00    --  113.25 -92.00 -37.00  163
 11  \w    101.00 177.00   0.38    1.00    --  113.25  87.00 144.00  200
 12  \w     -9.00  26.72   0.38    0.25    --  -47.28  19.00-180.00   94
 13  \w     -9.00  26.72   0.38    0.25    --  -47.28  19.00  90.00   94
 14  \w     -9.00  26.72   0.38    0.25    --  -47.28  19.00 120.00   94
 15  \w     35.00 119.36   0.38    0.25    --   47.28  38.00  60.00  222
 16  \w     32.00 119.02   0.38    0.25    --   47.28  57.00  90.00  229
 17  \w   -163.00 -70.28   0.38    1.00    --  -91.75 -77.00  90.00  244
 18  \w   -163.00 -70.28   0.38    1.00    --  -91.75 -77.00  60.00  244
 19  \w   -163.00 -70.66   0.38    1.00    --  -91.75 -75.00  34.42  243
 20  \w   -163.00 -72.94   0.38    1.00    --  -91.75 -69.00  93.35  237
 21  \w   -163.00 -75.98   0.38    1.00    --  -91.75 -61.00  60.00  229
 22  \w   -163.00 -74.84   0.38    1.00    --  -91.75 -64.00  57.55  232
 23  \w     97.00 177.18   0.38    1.00    --  113.25  61.00  90.00  211
 24  \w     91.00 176.88   0.38    1.00    --  113.25  77.00  30.00  226
 25  \w     97.00 177.18   0.38    1.00    --  113.25  61.00  30.00  211
 26  \w     42.00 105.08   0.38    1.00    --  113.25 -94.00 -90.00  166
 27  \w     44.00 109.74   0.38    1.00    --  113.25-125.00-120.00  173
 28  \w     42.00 105.08   0.38    1.00    --  113.25 -94.00  30.00  166
 29  \w    101.00 177.00   0.38    1.00    --  113.25  30.00  30.00  200
 30  \w     95.00 176.70   0.38    1.00    --  113.25 125.00 -30.00  215
 31  \w     42.00  82.28   0.38    1.00    --  113.25 -61.00 -60.00  106
 32  \w     97.00 177.18   0.38    1.00    --  113.25  61.00  60.00  211
 33  \w     91.00 176.88   0.38    1.00    --  113.25  77.00  60.00  226
 34  \w     42.00  82.28   0.38    1.00    --  113.25 -61.00   0.00  106
 35  \w    101.00 177.00   0.38    1.00    --  113.25  30.00  60.00  200
 36  \w     84.00 170.64   0.38    1.00    --  113.25 142.00  -8.00  228
 37  \w    102.00 178.00   0.38    1.00    --  113.25  92.00  75.00  200
 38  \w     35.00 119.36   0.38    0.25    --   47.28  38.00-180.00  222
 39  \w     25.00 120.00   0.38    0.25    --   47.28  77.00 -60.00  250
 40  \w     25.00 120.00   0.38    0.25    --   47.28  77.00-120.00  250
 41  \w     25.00 120.00   0.38    0.25    --   47.28  77.00   0.00  250
 42  \w     25.00 120.00   0.38    0.25    --   47.28  77.00-180.00  250
;
_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      0.0087893000
_diffrn_orient_matrix_UB_12      -0.0969007000
_diffrn_orient_matrix_UB_13      0.0052605000
_diffrn_orient_matrix_UB_21      0.1083197000
_diffrn_orient_matrix_UB_22      0.0727961000
_diffrn_orient_matrix_UB_23      0.0084448000
_diffrn_orient_matrix_UB_31      -0.0537690000
_diffrn_orient_matrix_UB_32      -0.0058858000
_diffrn_orient_matrix_UB_33      0.0178851000
_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  0.0438
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       95
_diffrn_reflns_limit_l_min       -91
_diffrn_reflns_number            99250
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.403
_diffrn_reflns_theta_min         3.674
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.083
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             6504
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 3107 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(3)
_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     421
_refine_ls_number_reflns         6745
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0603P)^2^+17.4680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.977
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                6574
_reflns_number_total             6745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08832a2.cif
_cod_data_source_block           neiar25
_cod_depositor_comments
'Adding full bibliography for 1576451--1576463.cif.'
_cod_original_cell_volume        14017.0(2)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               1576457
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.705
_shelx_estimated_absorpt_t_min   0.514
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
2.b 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)
;
_shelx_res_checksum              64693
_olex2_submission_original_sample_id neiar25
_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 1.173
_oxdiff_exptl_absorpt_empirical_full_min 0.839