Ferrocene-containing Schiff bases and their Sn(iv) complexes with two non-conjugated redox-active fragments: dependence of spectroscopic and redox properties on complexation and solvent
Proshutinskaya, Varvara Yu.; Krylova, Irina V.; Shangin, Pavel G.; Vilman, Victoriya A.; Minyaev, Mikhail E.; Gorbunov, Dmitry E.; Gritsan, Nina P.; Nikolaevskaya, Elena N.; Egorov, Mikhail P.; Tretyakov, Evgeny V.; Syroeshkin, Mikhail A.; New Journal of Chemistry 50 (2026) 3906–3925; doi:10.1039/D5NJ04462F

data_7064255
_publ_section_title
;
 Ferrocene-containing Schiff bases and their Sn(iv) complexes with two
 non-conjugated redox-active fragments: dependence of spectroscopic and
 redox properties on complexation and solvent
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3906
_journal_page_last               3925
_journal_paper_doi               10.1039/D5NJ04462F
_journal_volume                  50
_journal_year                    2026
_chemical_formula_moiety         'C24 H22 Fe N4 O2'
_chemical_formula_sum            'C24 H22 Fe N4 O2'
_chemical_formula_weight         454.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-05-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-24 deposited with the CCDC.	2026-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.88798(12)
_cell_length_b                   11.87134(7)
_cell_length_c                   20.52860(14)
_cell_measurement_reflns_used    26454
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.8790
_cell_measurement_theta_min      4.3110
_cell_volume                     4115.63(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.117a 64-bit (release 26-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015)'
_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 0.994
_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   -122.00  -8.00   0.50    3.50    --  -42.78 -17.00-123.00  228
  2  \w   -115.00 -69.00   0.50    3.50    --  -42.78-132.00-168.00   92
  3  \w     42.00 104.00   0.50    3.50    --   42.78-138.00  15.00  124
  4  \w     21.00  85.00   0.50    3.50    --   42.78-108.00  87.00  128
  5  \w    -91.00 -24.00   0.50   14.00    --  -96.00 132.00 -99.00  134
  6  \w    -95.00 -22.00   0.50   14.00    --  -96.00 138.00  76.00  146
  7  \w   -177.00-109.00   0.50   14.00    --  -96.00 -17.00-123.00  136
  8  \w    -52.00 -27.00   0.50   14.00    --  -96.00 108.00-176.00   50
  9  \w     76.00 101.00   0.50   14.00    --  117.50-108.00  87.00   50
 10  \w    125.00 150.00   0.50   14.00    --  117.50 108.00-176.00   50
 11  \w     89.00 132.00   0.50   14.00    --  117.50 138.00  76.00   86
 12  \w     81.00 117.00   0.50   14.00    --  117.50-132.00-168.00   72
 13  \w     81.00 178.00   0.50   14.00    --  117.50  17.00  45.00  194
 14  \w    -25.00  36.00   0.50    3.50    --  -42.78  19.00-180.00  122
 15  \w     13.00  41.00   0.50    3.50    --   42.78  91.00  84.64   56
 16  \w     44.00  90.00   0.50   14.00    --  117.50 -95.00  30.00   92
 17  \w     47.00  73.00   0.50   14.00    --  117.50 -77.00  90.00   52
 18  \w     65.00  90.00   0.50   14.00    --  117.50-125.00  30.00   50
 19  \w     46.00  71.00   0.50   14.00    --  117.50 -61.00  30.00   50
 20  \w     61.00 104.00   0.50   14.00    --  117.50 -95.00  90.00   86
 21  \w    115.00 151.00   0.50   14.00    --  117.50 -86.00  42.22   72
 22  \w     49.00  87.00   0.50   14.00    --  117.50-125.00-150.00   76
 23  \w     44.00  69.00   0.50   14.00    --  117.50 -61.00-180.00   50
 24  \w     97.00 129.00   0.50   14.00    --  117.50  30.00  60.00   64
 25  \w    146.00 172.00   0.50   14.00    --  117.50  30.00  60.00   52
 26  \w     47.00  72.00   0.50   14.00    --  117.50-125.00  90.00   50
 27  \w     97.00 172.00   0.50   14.00    --  117.50  61.00  90.00  150
 28  \w     75.00 100.00   0.50   14.00    --  117.50 -95.00-150.00   50
 29  \w     45.00  71.00   0.50   14.00    --  117.50 -86.00  42.22   52
 30  \w     92.00 144.00   0.50   14.00    --  117.50  77.00 150.00  104
 31  \w    150.00 178.00   0.50   14.00    --  117.50  77.00 150.00   56
 32  \w     78.00 104.00   0.50   14.00    --  117.50   0.00 -30.00   52
 33  \w    136.00 178.00   0.50   14.00    --  117.50   0.00 -30.00   84
 34  \w     96.00 121.00   0.50   14.00    --  117.50 125.00  90.00   50
 35  \w     44.00  69.00   0.50   14.00    --  117.50 -77.00   0.00   50
 36  \w     73.00  99.00   0.50   14.00    --  117.50 -77.00   0.00   52
 37  \w    107.00 149.00   0.50   14.00    --  117.50 -82.00 102.99   84
 38  \w     44.00  77.00   0.50   14.00    --  117.50 -95.00 -90.00   66
 39  \w     59.00  92.00   0.50   14.00    --  117.50 -77.00  30.00   66
 40  \w     44.00 105.00   0.50   14.00    --  117.50 -77.00 -90.00  122
 41  \w    123.00 174.00   0.50   14.00    --  117.50 125.00 -90.00  102
 42  \w     89.00 121.00   0.50   14.00    --  117.50  77.00  30.00   64
 43  \w    126.00 152.00   0.50   14.00    --  117.50  77.00  30.00   52
 44  \w     44.00  71.00   0.50   14.00    --  117.50 -61.00 -90.00   54
 45  \w     45.00  88.00   0.50   14.00    --  117.50 -95.00 120.00   86
 46  \w     59.00  85.00   0.50   14.00    --  117.50-125.00-180.00   52
 47  \w     64.00  90.00   0.50   14.00    --  117.50 -88.00  96.46   52
 48  \w     98.00 129.00   0.50   14.00    --  117.50 -88.00  96.46   62
 49  \w     73.00  98.00   0.50   14.00    --  117.50 -77.00-150.00   50
 50  \w     72.00 104.00   0.50   14.00    --  117.50 -77.00 -60.00   64
 51  \w     44.00  81.00   0.50   14.00    --  117.50 -95.00-180.00   74
 52  \w     52.00  78.00   0.50   14.00    --  117.50 -95.00 -60.00   52
 53  \w     57.00  83.00   0.50   14.00    --  117.50-125.00 -30.00   52
 54  \w     58.00 111.00   0.50   14.00    --  117.50   7.00  52.95  106
 55  \w    131.00 165.00   0.50   14.00    --  117.50 125.00-120.00   68
 56  \w     44.00  69.00   0.50   14.00    --  117.50 -61.00   0.00   50
 57  \w    114.00 140.00   0.50   14.00    --  117.50 125.00 150.00   52
 58  \w     95.00 120.00   0.50   14.00    --  117.50  61.00-150.00   50
 59  \w    101.00 127.00   0.50   14.00    --  117.50  61.00 -60.00   52
 60  \w     44.00  83.00   0.50   14.00    --  117.50 -86.00  11.73   78
 61  \w    126.00 151.00   0.50   14.00    --  117.50 -86.00  11.73   50
 62  \w     53.00  79.00   0.50   14.00    --  117.50  11.00  30.36   52
 63  \w     44.00  69.00   0.50   14.00    --  117.50 -61.00-120.00   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      -0.0636093000
_diffrn_orient_matrix_UB_12      -0.0231178000
_diffrn_orient_matrix_UB_13      0.0520611000
_diffrn_orient_matrix_UB_21      0.0619445000
_diffrn_orient_matrix_UB_22      0.0189717000
_diffrn_orient_matrix_UB_23      0.0540488000
_diffrn_orient_matrix_UB_31      -0.0209748000
_diffrn_orient_matrix_UB_32      0.1262402000
_diffrn_orient_matrix_UB_33      0.0015028000
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53108
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.015
_diffrn_reflns_theta_min         4.307
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.118
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.117a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+1.5433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4141
_reflns_number_total             4470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj04462f2.cif
_cod_data_source_block           853005
_cod_depositor_comments
'Adding full bibliography for 7064255--7064256.cif.'
_cod_database_code               7064255
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H22FeN4O2
_chemical_oxdiff_usercomment     853005
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.360
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
 C23(H23), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              68367
_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 1.435
_oxdiff_exptl_absorpt_empirical_full_min 0.858