#------------------------------------------------------------------------------
#$Date: 2026-04-15 03:20:12 +0200 (Wed, 15 Apr 2026) $
#$Revision: 305547 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/7/25/18/7251884.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7251884
loop_
_publ_author_name
'Rabaaoui, Nejmeddine'
'Guesmi, Ahlem'
'Jabeur, Wiem'
'Mhadhbi, Noureddine'
'Ben Hamadi, Naoufel'
'Khezami, Lotfi'
'Cherif, Mourad'
'Naïli, Houcine'
_publ_section_title
;
 High-efficiency electro-Fenton mineralization of triclosan using a novel
 octahedral iron(iii) complex: structure, mechanism, and performance
;
_journal_issue                   22
_journal_name_full               'RSC Advances'
_journal_page_first              19687
_journal_page_last               19701
_journal_paper_doi               10.1039/D6RA01483F
_journal_volume                  16
_journal_year                    2026
_chemical_formula_moiety         'C5 H16 Fe N4 O3, Cl'
_chemical_formula_sum            'C5 H16 Cl Fe N4 O3'
_chemical_formula_weight         271.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-30
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2025-04-25 deposited with the CCDC.	2026-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7188(3)
_cell_length_b                   11.0446(3)
_cell_length_c                   8.5086(3)
_cell_measurement_reflns_used    10232
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.9500
_cell_measurement_theta_min      5.4580
_cell_volume                     1007.29(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.77a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.77a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.77a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00 -40.00   0.50    5.00    --   -7.98 -19.00-149.00   98
  2  ω     -3.00  73.00   0.50    5.00    --   -7.98  19.00  18.00  152
  3  ω      2.00  50.00   0.50    5.00    --    8.29-108.00  91.00   96
  4  ω    -89.00 -40.00   0.50    5.00    --   -7.98 -19.00  90.00   98
  5  ω    -21.00  32.00   0.50    5.00    --    8.29 -77.00  90.00  106
  6  ω     -7.00  39.00   0.50    5.00    --    8.29  57.00  90.00   92
  7  ω     -7.00  39.00   0.50    5.00    --    8.29  57.00-150.00   92
  8  ω    -89.00 -44.00   0.50    5.00    --   -7.98 -19.00 -60.00   90
  9  ω    -21.00  32.00   0.50    5.00    --    8.29 -77.00-120.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0069487000
_diffrn_orient_matrix_UB_12      0.0477583000
_diffrn_orient_matrix_UB_13      0.0550561000
_diffrn_orient_matrix_UB_21      0.0155965000
_diffrn_orient_matrix_UB_22      -0.0401457000
_diffrn_orient_matrix_UB_23      0.0620006000
_diffrn_orient_matrix_UB_31      0.0639382000
_diffrn_orient_matrix_UB_32      0.0150369000
_diffrn_orient_matrix_UB_33      -0.0090871000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12256
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.987
_diffrn_reflns_theta_min         5.478
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.752
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.77a (Rigaku Oxford Diffraction, 2022)
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    1.790
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.21(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2510
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0238
_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/[σ²(Fo²)+(0.0296P)²+0.3075P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0580
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.807
_reflns_number_gt                2444
_reflns_number_total             2510
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d6ra01483f1.cif
_cod_data_source_block           dbufe_autored
_cod_database_code               7251884
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C5 H16 Cl1 Fe1 N4 O3'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.823
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.79(2)
 0.21(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), C2(H2C,H2D), C3(H3C,H3D),
 C4(H4C,H4D), C5(H5A,H5B)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id DBUFe
_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 1.403
_oxdiff_exptl_absorpt_empirical_full_min 0.724
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.56977(2) 0.71121(3) 0.50530(5) 0.00532(10) Uani 1 1 d . . . . .
O1 O 0.64326(16) 0.56956(16) 0.5993(2) 0.0122(4) Uani 1 1 d . . . . .
O2 O 0.73710(17) 0.68837(16) 0.4338(3) 0.0122(4) Uani 1 1 d . . . . .
O3 O 0.84658(16) 0.53452(17) 0.5422(2) 0.0156(4) Uani 1 1 d . . . . .
N1 N 0.4095(2) 0.7084(2) 0.6170(3) 0.0113(5) Uani 1 1 d . . . . .
H1A H 0.356098 0.763460 0.574383 0.014 Uiso 1 1 calc R U . . .
H1B H 0.374159 0.633715 0.610117 0.014 Uiso 1 1 calc R U . . .
N2 N 0.6300(2) 0.8102(2) 0.6796(3) 0.0108(4) Uani 1 1 d . . . . .
H2A H 0.685570 0.767213 0.738053 0.013 Uiso 1 1 calc R U . . .
H2B H 0.669335 0.877126 0.641764 0.013 Uiso 1 1 calc R U . . .
N3 N 0.50253(19) 0.6153(2) 0.3319(3) 0.0111(4) Uani 1 1 d . . . . .
H3A H 0.565870 0.579499 0.277901 0.013 Uiso 1 1 calc R U . . .
H3B H 0.451692 0.556143 0.369934 0.013 Uiso 1 1 calc R U . . .
N4 N 0.5308(2) 0.8535(2) 0.3778(3) 0.0110(4) Uani 1 1 d . . . . .
H4A H 0.463155 0.892435 0.418089 0.013 Uiso 1 1 calc R U . . .
H4B H 0.596472 0.905727 0.378430 0.013 Uiso 1 1 calc R U . . .
C1 C 0.7481(2) 0.5928(2) 0.5253(3) 0.0115(5) Uani 1 1 d . . . . .
C2 C 0.4358(3) 0.7391(3) 0.7837(4) 0.0138(6) Uani 1 1 d . . . . .
H2C H 0.476004 0.670095 0.837864 0.017 Uiso 1 1 calc R U . . .
H2D H 0.357589 0.759635 0.839687 0.017 Uiso 1 1 calc R U . . .
C3 C 0.5224(3) 0.8471(3) 0.7793(3) 0.0137(5) Uani 1 1 d . . . . .
H3C H 0.479578 0.918205 0.733391 0.016 Uiso 1 1 calc R U . . .
H3D H 0.550797 0.868072 0.886612 0.016 Uiso 1 1 calc R U . . .
C4 C 0.4311(2) 0.6967(3) 0.2261(5) 0.0130(7) Uani 1 1 d . . . . .
H4C H 0.347024 0.712460 0.269723 0.016 Uiso 1 1 calc R U . . .
H4D H 0.421687 0.659452 0.120956 0.016 Uiso 1 1 calc R U . . .
C5 C 0.5044(3) 0.8134(3) 0.2145(3) 0.0129(6) Uani 1 1 d . . . . .
H5A H 0.583364 0.799761 0.156692 0.016 Uiso 1 1 calc R U . . .
H5B H 0.455383 0.875642 0.158067 0.016 Uiso 1 1 calc R U . . .
Cl1 Cl 0.26083(5) 0.95782(5) 0.49651(11) 0.01463(13) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
15 4 -1 0.0515
-15 -4 1 0.0515
0 1 12 0.0362
0 -1 -12 0.0662
0 16 -1 0.0291
0 -16 1 0.0291
7 14 -1 0.0365
-7 14 0 0.0380
-5 -15 1 0.0323
7 -14 0 0.0326
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 N1 98.29(9) . . ?
O1 Fe1 N2 90.24(9) . . ?
O1 Fe1 N3 91.38(9) . . ?
O1 Fe1 N4 166.20(9) . . ?
O1 Fe1 C1 34.45(8) . . ?
O2 Fe1 O1 68.97(8) . . ?
O2 Fe1 N1 166.75(9) . . ?
O2 Fe1 N2 90.33(9) . . ?
O2 Fe1 N3 91.96(9) . . ?
O2 Fe1 N4 97.47(9) . . ?
O2 Fe1 C1 34.54(9) . . ?
N1 Fe1 C1 132.54(9) . . ?
N2 Fe1 N1 85.99(10) . . ?
N2 Fe1 N3 177.56(9) . . ?
N2 Fe1 N4 92.39(9) . . ?
N2 Fe1 C1 89.30(9) . . ?
N3 Fe1 N1 91.97(9) . . ?
N3 Fe1 N4 86.46(9) . . ?
N3 Fe1 C1 93.07(9) . . ?
N4 Fe1 N1 95.40(9) . . ?
N4 Fe1 C1 132.00(9) . . ?
C1 O1 Fe1 89.53(14) . . ?
C1 O2 Fe1 90.10(15) . . ?
Fe1 N1 H1A 110.3 . . ?
Fe1 N1 H1B 110.3 . . ?
H1A N1 H1B 108.6 . . ?
C2 N1 Fe1 107.03(17) . . ?
C2 N1 H1A 110.3 . . ?
C2 N1 H1B 110.3 . . ?
Fe1 N2 H2A 109.8 . . ?
Fe1 N2 H2B 109.8 . . ?
H2A N2 H2B 108.3 . . ?
C3 N2 Fe1 109.28(17) . . ?
C3 N2 H2A 109.8 . . ?
C3 N2 H2B 109.8 . . ?
Fe1 N3 H3A 110.0 . . ?
Fe1 N3 H3B 110.0 . . ?
H3A N3 H3B 108.3 . . ?
C4 N3 Fe1 108.62(18) . . ?
C4 N3 H3A 110.0 . . ?
C4 N3 H3B 110.0 . . ?
Fe1 N4 H4A 110.0 . . ?
Fe1 N4 H4B 110.0 . . ?
H4A N4 H4B 108.3 . . ?
C5 N4 Fe1 108.65(16) . . ?
C5 N4 H4A 110.0 . . ?
C5 N4 H4B 110.0 . . ?
O1 C1 Fe1 56.02(11) . . ?
O1 C1 O2 111.3(2) . . ?
O2 C1 Fe1 55.36(12) . . ?
O3 C1 Fe1 176.2(2) . . ?
O3 C1 O1 124.7(2) . . ?
O3 C1 O2 124.0(2) . . ?
N1 C2 H2C 110.6 . . ?
N1 C2 H2D 110.6 . . ?
N1 C2 C3 105.8(3) . . ?
H2C C2 H2D 108.7 . . ?
C3 C2 H2C 110.6 . . ?
C3 C2 H2D 110.6 . . ?
N2 C3 C2 105.9(2) . . ?
N2 C3 H3C 110.6 . . ?
N2 C3 H3D 110.6 . . ?
C2 C3 H3C 110.6 . . ?
C2 C3 H3D 110.6 . . ?
H3C C3 H3D 108.7 . . ?
N3 C4 H4C 110.4 . . ?
N3 C4 H4D 110.4 . . ?
N3 C4 C5 106.7(2) . . ?
H4C C4 H4D 108.6 . . ?
C5 C4 H4C 110.4 . . ?
C5 C4 H4D 110.4 . . ?
N4 C5 C4 107.0(3) . . ?
N4 C5 H5A 110.3 . . ?
N4 C5 H5B 110.3 . . ?
C4 C5 H5A 110.3 . . ?
C4 C5 H5B 110.3 . . ?
H5A C5 H5B 108.6 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.9257(18) . ?
Fe1 O2 1.9107(18) . ?
Fe1 N1 1.963(2) . ?
Fe1 N2 1.953(2) . ?
Fe1 N3 1.954(2) . ?
Fe1 N4 1.955(2) . ?
Fe1 C1 2.322(2) . ?
O1 C1 1.314(3) . ?
O2 C1 1.317(3) . ?
O3 C1 1.245(3) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C2 1.485(4) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 C3 1.488(4) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 C4 1.485(4) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 C5 1.486(4) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C2 C3 1.511(4) . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C4 H4C 0.9900 . ?
C4 H4D 0.9900 . ?
C4 C5 1.512(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 O1 C1 O2 -2.7(2) . . . . ?
Fe1 O1 C1 O3 175.4(3) . . . . ?
Fe1 O2 C1 O1 2.7(2) . . . . ?
Fe1 O2 C1 O3 -175.4(3) . . . . ?
Fe1 N1 C2 C3 45.8(2) . . . . ?
Fe1 N2 C3 C2 37.9(3) . . . . ?
Fe1 N3 C4 C5 39.9(3) . . . . ?
Fe1 N4 C5 C4 39.1(2) . . . . ?
N1 C2 C3 N2 -54.7(3) . . . . ?
N3 C4 C5 N4 -51.7(3) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.79(2)
2 0.21(2)
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
14.6727 3.6297 -0.6075 0.0379 0.0455 0.9982
-14.6727 -3.6297 0.6075 -0.0379 -0.0455 -0.9982
-0.0405 0.5007 11.9820 0.6839 0.7222 -0.1039
0.0405 -0.5007 -11.9820 -0.6839 -0.7222 0.1039
0.0648 15.5555 -0.7040 0.7037 -0.6671 0.2444
-0.0648 -15.5555 0.7040 -0.7037 0.6671 -0.2444
6.5682 13.9471 -1.1647 0.5563 -0.5297 0.6403
-6.9943 13.8180 -0.0475 0.7059 -0.6668 -0.2390
-4.8009 -14.7082 1.0540 -0.6110 0.5809 -0.5377
6.8364 -13.9016 0.0642 -0.7079 0.6687 0.2275
