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_1576460
_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 Fe N3, C4 H8 O'
_chemical_formula_sum            'C40 H38 Fe N3 O'
_chemical_formula_weight         632.58
_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             2023-01-04
_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                 91.4460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.08620(10)
_cell_length_b                   9.95440(10)
_cell_length_c                   20.74630(10)
_cell_measurement_reflns_used    29382
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.8210
_cell_measurement_theta_min      3.6620
_cell_volume                     3114.56(4)
_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      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 0.984
_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    -85.00 -11.00   0.50    0.34    --  -47.28 123.00  51.00  148
  2  \w   -103.00 -25.00   0.50    0.34    --  -47.28 149.00-145.00  156
  3  \w   -119.00 -57.00   0.50    0.34    --  -47.28-149.00 167.00  124
  4  \w     33.00  92.00   0.50    0.34    --   47.28-123.00 -29.00  118
  5  \w     47.00 110.00   0.50    0.34    --   47.28-149.00 167.00  126
  6  \w   -103.00 -25.00   0.50    1.35    --  -91.75 149.00-145.00  156
  7  \w   -161.00 -75.00   0.50    1.35    --  -91.75-123.00 -29.00  172
  8  \w     44.00 110.00   0.50    1.35    --  113.25-123.00 -29.00  132
  9  \w     96.00 178.00   0.50    1.35    --  113.25 123.00  51.00  164
 10  \w     79.00 167.00   0.50    1.35    --  113.25 149.00-145.00  176
 11  \w     47.00 129.00   0.50    1.35    --  113.25-149.00 167.00  164
 12  \w    -38.00  26.00   0.50    0.34    --  -47.28  38.00-150.00  128
 13  \w    -14.00  28.00   0.50    0.34    --  -47.28  19.00 150.00   84
 14  \w    -14.00  28.00   0.50    0.34    --  -47.28  19.00-180.00   84
 15  \w    -14.00  28.00   0.50    0.34    --  -47.28  19.00-120.00   84
 16  \w    -27.00  18.00   0.50    0.34    --   47.28 -19.00-150.00   90
 17  \w    -47.00 -20.00   0.50    1.35    --  -91.75  45.00-150.00   54
 18  \w    -47.00 -20.00   0.50    1.35    --  -91.75  45.00-120.00   54
 19  \w     42.00  76.00   0.50    1.35    --  113.25 -61.00  30.00   68
 20  \w    101.00 178.00   0.50    1.35    --  113.25  30.00-150.00  154
 21  \w     42.00  76.00   0.50    1.35    --  113.25 -61.00   0.00   68
 22  \w     91.00 178.00   0.50    1.35    --  113.25  77.00  30.00  174
 23  \w     42.00 106.00   0.50    1.35    --  113.25 -94.00   0.00  128
 24  \w     42.00  76.00   0.50    1.35    --  113.25 -61.00 -60.00   68
 25  \w     44.00 111.00   0.50    1.35    --  113.25-125.00-180.00  134
 26  \w     42.00 106.00   0.50    1.35    --  113.25 -94.00 -30.00  128
 27  \w     42.00 106.00   0.50    1.35    --  113.25 -94.00  30.00  128
 28  \w     44.00 108.00   0.50    1.35    --  113.25-108.00  11.89  128
 29  \w     42.00  76.00   0.50    1.35    --  113.25 -61.00-150.00   68
 30  \w     42.00  76.00   0.50    1.35    --  113.25 -61.00 150.00   68
 31  \w    101.00 178.00   0.50    1.35    --  113.25  45.00 -90.00  154
 32  \w     42.00 106.00   0.50    1.35    --  113.25 -94.00-150.00  128
 33  \w     42.00 106.00   0.50    1.35    --  113.25 -94.00  60.00  128
 34  \w    101.00 178.00   0.50    1.35    --  113.25  30.00-120.00  154
 35  \w   -119.00 -25.00   0.50    0.34    --  -47.28 -77.00 -60.00  188
 36  \w   -120.00 -34.00   0.50    0.34    --  -47.28 -38.00-180.00  172
 37  \w     25.00 120.00   0.50    0.34    --   47.28  77.00 120.00  190
 38  \w     32.00 120.00   0.50    0.34    --   47.28  57.00   0.00  176
 39  \w     25.00 120.00   0.50    0.34    --   47.28  77.00  60.00  190
 40  \w     25.00  89.00   0.50    0.34    --   47.28  77.00-120.00  128
 41  \w     25.00 120.00   0.50    0.34    --   47.28  77.00 150.00  190
;
_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      -0.0102616000
_diffrn_orient_matrix_UB_12      -0.1512938000
_diffrn_orient_matrix_UB_13      -0.0139669000
_diffrn_orient_matrix_UB_21      0.0035036000
_diffrn_orient_matrix_UB_22      -0.0293190000
_diffrn_orient_matrix_UB_23      0.0729348000
_diffrn_orient_matrix_UB_31      -0.1015442000
_diffrn_orient_matrix_UB_32      0.0143305000
_diffrn_orient_matrix_UB_33      0.0021970000
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54363
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.207
_diffrn_reflns_theta_min         3.580
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.167
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72581
_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 violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       plate
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0370P)^2^+2.6568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6236
_reflns_number_total             6710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08832a2.cif
_cod_data_source_block           neiar18
_cod_depositor_comments
'Adding full bibliography for 1576451--1576463.cif.'
_cod_database_code               1576460
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.505
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C28(H28),
  C29(H29), C32(H32), C33(H33), C34(H34), C35(H35)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              63175
_olex2_submission_original_sample_id neiar18
_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 1.354
_oxdiff_exptl_absorpt_empirical_full_min 0.831