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_1576451
_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         'C39 H24 Fe N3'
_chemical_formula_sum            'C39 H24 Fe N3'
_chemical_formula_weight         590.46
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-07-30
_audit_creation_method
;
Olex2 1.5-ac6-015
(compiled 2023.12.04 svn.r209d9fb2 for Rigaku Oxford Diffraction, GUI svn.r6873)
;
_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            4
_cell_length_a                   15.0670(6)
_cell_length_b                   15.0670(6)
_cell_length_c                   15.2096(6)
_cell_measurement_reflns_used    4731
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.7490
_cell_measurement_theta_min      3.3830
_cell_volume                     2990.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (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 0.983
_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 -93.00   0.50    1.19    --  -48.05-127.00 175.00   52
  2  \w     95.00 125.00   0.50    4.74    --  107.75  55.00 139.00   60
  3  \w    150.00 175.00   0.50    4.74    --  107.75  55.00 139.00   50
  4  \w     36.00  68.00   0.50    4.74    --  107.75 -55.00  -2.00   64
  5  \w   -120.00 -93.00   0.50    1.19    --  -48.05-125.00  60.00   54
  6  \w     -4.00  21.00   0.50    1.19    --  -48.05  19.00  90.00   50
  7  \w   -111.00 -68.00   0.50    1.19    --  -48.05-143.00   5.00   86
  8  \w    -44.00 -18.00   0.50    4.74    --  -86.25  45.00  90.00   52
  9  \w    108.00 159.00   0.50    4.74    --  107.75  30.00-180.00  102
 10  \w     36.00  62.00   0.50    4.74    --  107.75 -94.00 120.00   52
 11  \w     41.00  87.00   0.50    4.74    --  107.75 -94.00  60.00   92
 12  \w     79.00 104.00   0.50    4.74    --  107.75 -94.00 120.00   50
 13  \w     37.00 106.00   0.50    4.74    --  107.75-107.00  -7.00  138
;
_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      -0.0286820000
_diffrn_orient_matrix_UB_12      -0.0987224000
_diffrn_orient_matrix_UB_13      0.0514238000
_diffrn_orient_matrix_UB_21      -0.0731083000
_diffrn_orient_matrix_UB_22      -0.0639658000
_diffrn_orient_matrix_UB_23      -0.0746577000
_diffrn_orient_matrix_UB_31      0.0883982000
_diffrn_orient_matrix_UB_32      -0.0064164000
_diffrn_orient_matrix_UB_33      -0.0450662000
_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  0.0365
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9024
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.925
_diffrn_reflns_theta_min         3.387
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.286
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple-black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       needle
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+1.0079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1860
_reflns_number_total             2104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08832a2.cif
_cod_data_source_block           neisc85
_cod_depositor_comments
'Adding full bibliography for 1576451--1576463.cif.'
_cod_original_cell_volume        2990.2(3)
_cod_database_code               1576451
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.413
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10)
;
_shelx_res_checksum              1418
_shelx_fab_checksum              13490
_olex2_submission_original_sample_id neisc85
_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 1.697
_oxdiff_exptl_absorpt_empirical_full_min 0.648