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_1576454
_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, C18 H36 K N2 O6'
_chemical_formula_sum            'C57 H60 Fe K N5 O6'
_chemical_formula_weight         1006.05
_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             2021-03-19
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2024-07-30 deposited with the CCDC.	2026-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6152(2)
_cell_length_b                   13.0318(2)
_cell_length_c                   31.1990(4)
_cell_measurement_reflns_used    27632
_cell_measurement_temperature    232.99(10)
_cell_measurement_theta_max      77.1470
_cell_measurement_theta_min      2.8850
_cell_volume                     5061.33(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      232.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_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  22.00   0.50    3.46    --  -49.75  39.00  82.00  106
  2  \w     42.00 121.00   0.50    3.46    --   49.75  39.00  82.00  158
  3  \w    -21.00  43.00   0.50    3.46    --   49.75 -39.00 -72.00  128
  4  \w   -155.00 -76.00   0.50   13.86    --  -84.25 -39.00 -72.00  158
  5  \w     98.00 177.00   0.50   13.86    --  105.75  39.00  82.00  158
  6  \w   -121.00 -70.00   0.50    3.46    --  -49.75-125.00  90.00  102
  7  \w   -121.00 -42.00   0.50    3.46    --  -49.75 -39.00 -72.00  158
  8  \w   -121.00 -70.00   0.50    3.46    --  -49.75-125.00-120.00  102
  9  \w    -23.00   5.00   0.50    3.46    --   49.75 -19.00-180.00   56
 10  \w    -23.00   5.00   0.50    3.46    --   49.75 -19.00 150.00   56
 11  \w    -42.00 -12.00   0.50   13.86    --  -84.25  45.00-120.00   60
 12  \w    -42.00 -12.00   0.50   13.86    --  -84.25  45.00 -90.00   60
 13  \w     98.00 164.00   0.50   13.86    --  105.75  15.00  60.00  132
 14  \w     34.00 109.00   0.50   13.86    --  105.75 -94.00  30.00  150
 15  \w     34.00  87.00   0.50   13.86    --  105.75 -61.00  90.00  106
 16  \w     34.00  87.00   0.50   13.86    --  105.75 -61.00 120.00  106
 17  \w     34.00 109.00   0.50   13.86    --  105.75 -94.00 -30.00  150
 18  \w     34.00 109.00   0.50   13.86    --  105.75 -94.00  60.00  150
 19  \w     34.00  87.00   0.50   13.86    --  105.75 -61.00  60.00  106
 20  \w     97.00 178.00   0.50   13.86    --  105.75  45.00-120.00  162
 21  \w     34.00  87.00   0.50   13.86    --  105.75 -61.00 150.00  106
 22  \w     34.00  87.00   0.50   13.86    --  105.75 -61.00-180.00  106
 23  \w     34.00  87.00   0.50   13.86    --  105.75 -61.00 -30.00  106
 24  \w     34.00 116.00   0.50   13.86    --  105.75-125.00   0.00  164
 25  \w     34.00  87.00   0.50   13.86    --  105.75 -61.00   0.00  106
 26  \w     34.00  87.00   0.50   13.86    --  105.75 -61.00-120.00  106
 27  \w     47.00 122.00   0.50   13.86    --  105.75 -77.00-150.00  150
 28  \w     37.00  87.00   0.50   13.86    --  105.75 -61.00-150.00  100
 29  \w    128.00 164.00   0.50   13.86    --  105.75  15.00 120.00   72
 30  \w     47.00  73.00   0.50   13.86    --  105.75 -94.00-180.00   52
 31  \w    100.00 128.00   0.50   13.86    --  105.75  30.00   0.00   56
;
_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      0.1067031000
_diffrn_orient_matrix_UB_12      0.0584957000
_diffrn_orient_matrix_UB_13      0.0018730000
_diffrn_orient_matrix_UB_21      0.0114604000
_diffrn_orient_matrix_UB_22      0.0054642000
_diffrn_orient_matrix_UB_23      0.0498845000
_diffrn_orient_matrix_UB_31      0.0615769000
_diffrn_orient_matrix_UB_32      -0.1025514000
_diffrn_orient_matrix_UB_33      0.0037220000
_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  0.0675
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            66201
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.879
_diffrn_reflns_theta_min         2.871
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.576
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green-black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       needle
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         10634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0844P)^2^+0.7555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9158
_reflns_number_total             10634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08832a2.cif
_cod_data_source_block           neinw64
_cod_depositor_comments
'Adding full bibliography for 1576451--1576463.cif.'
_cod_database_code               1576454
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.473
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
  C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C28(H28),
  C29(H29), C30(H30), C32(H32), C33(H33), C35(H35), C36(H36), C37(H37)
;
_shelx_res_checksum              10769
_olex2_submission_original_sample_id neinw64
_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 1.914
_oxdiff_exptl_absorpt_empirical_full_min 0.568