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_1576463
_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         'C27 H33 Fe, C21 H39 Mg O6'
_chemical_formula_sum            'C48 H72 Fe Mg O6'
_chemical_formula_weight         825.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_formula_units_Z            4
_cell_length_a                   12.38100(10)
_cell_length_b                   15.93360(10)
_cell_length_c                   23.8962(2)
_cell_measurement_reflns_used    25883
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3130
_cell_measurement_theta_min      3.3470
_cell_volume                     4714.10(6)
_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 0.989
_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   -120.00 -32.00   0.50    0.23    --  -48.05 -64.00 171.00  176
  2  \w    -59.00 -33.00   0.50    0.93    --  -86.25  95.00  45.00   52
  3  \w     90.00 137.00   0.50    0.93    --  107.75  67.00 166.00   94
  4  \w     46.00  72.00   0.50    0.93    --  107.75 -64.00 171.00   52
  5  \w    142.00 178.00   0.50    0.93    --  107.75  67.00 166.00   72
  6  \w     47.00  91.00   0.50    0.93    --  107.75 -95.00 -64.00   88
  7  \w     -3.00  22.00   0.50    0.23    --  -48.05  19.00  90.00   50
  8  \w    -62.00  18.00   0.50    0.23    --  -48.05  64.00 -52.00  160
  9  \w     -4.00  24.00   0.50    0.23    --  -48.05  19.00  60.00   56
 10  \w     -4.00  21.00   0.50    0.23    --  -48.05  19.00-120.00   50
 11  \w     -4.00  21.00   0.50    0.23    --  -48.05  19.00 -60.00   50
 12  \w    142.00 168.00   0.50    0.93    --  107.75  15.00  90.00   52
 13  \w     99.00 137.00   0.50    0.93    --  107.75  15.00  90.00   76
 14  \w    100.00 175.00   0.50    0.93    --  107.75  61.00  90.00  150
 15  \w     41.00  67.00   0.50    0.93    --  107.75 -94.00 150.00   52
 16  \w     36.00 109.00   0.50    0.93    --  107.75-125.00 -60.00  146
 17  \w     70.00  96.00   0.50    0.93    --  107.75 -94.00 150.00   52
 18  \w     47.00 130.00   0.50    0.93    --  107.75 -77.00  60.00  166
 19  \w     44.00  78.00   0.50    0.93    --  107.75 -61.00-180.00   68
 20  \w     61.00 107.00   0.50    0.93    --  107.75-125.00  60.00   92
 21  \w    113.00 151.00   0.50    0.93    --  107.75  30.00-120.00   76
 22  \w     41.00  80.00   0.50    0.93    --  107.75 -61.00 -60.00   78
 23  \w     39.00  64.00   0.50    0.93    --  107.75 -61.00  30.00   50
 24  \w    109.00 148.00   0.50    0.93    --  107.75  95.00  45.00   78
 25  \w     39.00  94.00   0.50    0.93    --  107.75 -94.00-180.00  110
 26  \w     38.00  64.00   0.50    0.93    --  107.75-125.00 -90.00   52
 27  \w     38.00  73.00   0.50    0.93    --  107.75 -61.00 -30.00   70
;
_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      -0.0154606000
_diffrn_orient_matrix_UB_12      0.0887993000
_diffrn_orient_matrix_UB_13      -0.0242731000
_diffrn_orient_matrix_UB_21      0.0937601000
_diffrn_orient_matrix_UB_22      -0.0153979000
_diffrn_orient_matrix_UB_23      -0.0411181000
_diffrn_orient_matrix_UB_31      -0.0803829000
_diffrn_orient_matrix_UB_32      -0.0351134000
_diffrn_orient_matrix_UB_33      -0.0432535000
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            38695
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         78.369
_diffrn_reflns_theta_min         3.334
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33973
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 3965 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0090(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         9906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0417P)^2^+1.0618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                9541
_reflns_number_total             9906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08832a2.cif
_cod_data_source_block           neisc83
_cod_depositor_comments
'Adding full bibliography for 1576451--1576463.cif.'
_cod_database_code               1576463
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.410
_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:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), 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)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C21(H21), C23(H23), C30(H30)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              9086
_olex2_submission_original_sample_id neisc83
_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 2.591
_oxdiff_exptl_absorpt_empirical_full_min 0.600