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_1576462
_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         'C33 H24 Fe1 N3'
_chemical_formula_sum            'C33 H24 Fe N3'
_chemical_formula_weight         518.40
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-11-01
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_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            6
_cell_length_a                   16.5115(2)
_cell_length_b                   16.5115(2)
_cell_length_c                   15.46360(10)
_cell_measurement_reflns_used    14776
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      78.5220
_cell_measurement_theta_min      3.0950
_cell_volume                     3651.02(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (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      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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    -84.00 -11.00   0.50    2.49    --  -47.02 123.00-144.00  146
  2  \w   -163.00 -72.00   0.50    9.97    --  -91.75-127.00  58.00  182
  3  \w     94.00 178.00   0.50    9.97    --  113.25 127.00 134.00  168
  4  \w     -3.00  28.00   0.50    2.49    --  -47.02  19.00 -60.00   62
  5  \w   -120.00 -73.00   0.50    2.49    --  -47.02-125.00 -90.00   94
  6  \w    -24.00  62.00   0.50    2.49    --   47.02 -57.00-180.00  172
  7  \w     42.00  80.00   0.50    9.97    --  113.25 -61.00-120.00   76
  8  \w     42.00 111.00   0.50    9.97    --  113.25-125.00 -90.00  138
  9  \w    101.00 178.00   0.50    9.97    --  113.25  30.00 120.00  154
 10  \w    100.00 172.00   0.50    9.97    --  113.25  15.00  60.00  144
 11  \w     42.00 111.00   0.50    9.97    --  113.25-125.00-150.00  138
 12  \w    100.00 172.00   0.50    9.97    --  113.25  15.00 -30.00  144
 13  \w     42.00 108.00   0.50    9.97    --  113.25-106.00  86.04  132
 14  \w     42.00  80.00   0.50    9.97    --  113.25 -61.00  60.00   76
 15  \w     24.00 120.00   0.50    2.49    --   47.02  77.00 -90.00  192
 16  \w     24.00 120.00   0.50    2.49    --   47.02  77.00  30.00  192
 17  \w     24.00 120.00   0.50    2.49    --   47.02  77.00 150.00  192
 18  \w   -163.00-138.00   0.50    9.97    --  -91.75 -63.00 -93.70   50
;
_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      0.0456936000
_diffrn_orient_matrix_UB_12      -0.0612455000
_diffrn_orient_matrix_UB_13      0.0087047000
_diffrn_orient_matrix_UB_21      -0.0971877000
_diffrn_orient_matrix_UB_22      -0.0885702000
_diffrn_orient_matrix_UB_23      -0.0046085000
_diffrn_orient_matrix_UB_31      0.0084780000
_diffrn_orient_matrix_UB_32      -0.0013460000
_diffrn_orient_matrix_UB_33      -0.0991708000
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29954
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.186
_diffrn_reflns_theta_min         3.090
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red-violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       needle
_exptl_crystal_F_000             1614
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.035
_refine_diff_density_max         2.123
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0837P)^2^+0.7963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2494
_reflns_number_total             2644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08832a2.cif
_cod_data_source_block           neiar04
_cod_depositor_comments
'Adding full bibliography for 1576451--1576463.cif.'
_cod_original_cell_volume        3651.02(9)
_cod_database_code               1576462
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.298
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.511(2)
 0.489(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Shared sites
{N1, C1'}
{C1, N1'}
{N2, C17'}
4. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C1')
Uanis(C1) = Uanis(N1')
Uanis(N2) = Uanis(C17')
5. Others
 Sof(C1')=Sof(N1')=1-FVAR(1)
 Sof(N1)=Sof(C1)=FVAR(1)
 Fixed Sof: N2(0.5) C17'(0.5)
6.a Riding coordinates:
 C2(H2), C11(H11), C12(H12)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15)
;
_shelx_res_checksum              38886
_olex2_submission_original_sample_id neiar04
_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 1.583
_oxdiff_exptl_absorpt_empirical_full_min 0.649