Catalytic ammonia oxidation mediated by high-spin Fe(iii) complex: combined experimental and DFT study
Usman, Mohammad; Hussein, Mohamed A.T.; Kandiel, Tarek A.; Yamani, Zain H.; Shaikh, M. Nasiruzzaman; Catalysis Science & Technology 16 (2026) 124–136; doi:10.1039/D5CY01107H

data_1576219
_publ_section_title
;
 Catalytic ammonia oxidation mediated by high-spin Fe(iii) complex:
 combined experimental and DFT study
;
_journal_issue                   1
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              124
_journal_page_last               136
_journal_paper_doi               10.1039/D5CY01107H
_journal_volume                  16
_journal_year                    2026
_chemical_formula_moiety         'C22 H24 Cl Fe N2 O4, H2 O'
_chemical_formula_sum            'C22 H26 Cl Fe N2 O5'
_chemical_formula_weight         489.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-09-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-09-15 deposited with the CCDC.	2025-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                87.8740(10)
_cell_angle_beta                 82.5000(10)
_cell_angle_gamma                68.3490(10)
_cell_formula_units_Z            4
_cell_length_a                   10.3050(3)
_cell_length_b                   11.2133(3)
_cell_length_c                   20.3260(6)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.19
_cell_volume                     2164.19(11)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36985
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.375
_diffrn_reflns_theta_min         1.954
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0840 before and 0.0491 after correction.
The Ratio of minimum to maximum transmission is 0.8904.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.531
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         10797
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0254P)^2^+5.9244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1267
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9403
_reflns_number_total             10797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cy01107h2.cif
_cod_data_source_block           mnsu_19_0m_a
_cod_depositor_comments          'Adding full bibliography for 1576219.cif.'
_cod_database_code               1576219
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.814
_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, All O(H,H) groups
2. Rigid body (RIGU) restrains
 C22, O3, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Free rotating group:
 O10(H10E,H10F), O9(H9C,H9D)
3.b Ternary CH refined with riding coordinates:
 C13(H13), C13A(H13A), C8A(H8A), C8(H8)
3.c Secondary CH2 refined with riding coordinates:
 C12A(H12A,H12B), C9A(H9AA,H9AB), C12(H12C,H12D), C11A(H11A,H11B), C9(H9A,H9B),
  C10A(H10A,H10B), C11(H11C,H11D), C10(H10C,H10D)
3.d Aromatic/amide H refined with riding coordinates:
 C14A(H14A), C3A(H3A), C18A(H18A), C5A(H5A), C3(H3), C4(H4), C5(H5), C4A(H4A),
 C7A(H7A), C14(H14), C16A(H16A), C7(H7), C17A(H17A), C16(H16), C17(H17),
 C18(H18)
3.e Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6)
3.f Idealised Me refined as rotating group:
 C22A(H22A,H22B,H22C), C21A(H21A,H21B,H21C), C22(H22D,H22E,H22F), C21(H21D,
 H21E,H21F)
;
_shelx_res_checksum              98456
_olex2_submission_special_instructions 'No special instructions were received'