Metal–Metal vs Metal–Ligand Cooperation in Iron-Mediated Activation and Catalytic Reduction of Nitrous Oxide and Nitrobenzene
Jori, Nadir; Corona, Helena; Soto, Enrique; Fernandez, Israel; Campos, Jesús; Chemical Science  (2026) –; doi:10.1039/D5SC07656K

data_1576778
_publ_section_title
;
 Metal-metal <i>vs.</i> metal-ligand cooperation in iron-mediated
 activation and catalytic reduction of nitrous oxide and nitrobenzene.
;
_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              9018
_journal_page_last               9026
_journal_paper_doi               10.1039/d5sc07656k
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C26 H44 Fe N O P2, C32 H12 B F24'
_chemical_formula_sum            'C58 H56 B F24 Fe N O P2'
_chemical_formula_weight         1367.63
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-07-22
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7308)
;
_audit_update_record
;
2025-07-23 deposited with the CCDC.	2026-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.049(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1363(7)
_cell_length_b                   18.0228(10)
_cell_length_c                   25.0443(11)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.286
_cell_measurement_theta_min      2.260
_cell_volume                     5896.3(5)
_computing_cell_refinement       'SAINT V8.41 (?, 2016)'
_computing_data_reduction        'SAINT V8.41 (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_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 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            92148
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.381
_diffrn_reflns_theta_min         1.925
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0892 before and 0.0754 after correction.
The Ratio of minimum to maximum transmission is 0.8427.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       rod
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     828
_refine_ls_number_reflns         10810
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0325P)^2^+17.2905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8457
_reflns_number_total             10810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc07656k2.cif
_cod_data_source_block           jcm00625b
_cod_depositor_comments
'Adding full bibliography for 1576777--1576784.cif.'
_cod_database_code               1576778
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.897
_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. Restrained distances
 F5-C34 \\sim F5A-C34
 with sigma of 0.02
 F13-C49 \\sim F13A-C49
 with sigma of 0.02
 F14-C49 \\sim F14A-C49
 with sigma of 0.02
 F6-C34 \\sim F6A-C34
 with sigma of 0.02
 F15-C49 \\sim F15A-C49
 with sigma of 0.02
 C49-F13 \\sim C49-F14 \\sim C49-F15
 with sigma of 0.02
 F4-C34 \\sim F4A-C34
 with sigma of 0.02
 C49-F13A \\sim C49-F14A \\sim C49-F15A
 with sigma of 0.02
 F13-F14 \\sim F14-F15 \\sim F15-F13
 with sigma of 0.02
 F13A-F14A \\sim F14A-F15A \\sim F15A-F13A
 with sigma of 0.02
 C34-F5 \\sim C34-F6 \\sim C34-F4 \\sim C34-F5A \\sim C34-F6A \\sim C34-F4A
 with sigma of 0.02
 F4-F5 \\sim F5-F6 \\sim F6-F4
 with sigma of 0.02
 F4A-F5A \\sim F5A-F6A \\sim F6A-F4A
 with sigma of 0.02
3. Others
 Sof(F5A)=Sof(F6A)=Sof(F4A)=1-FVAR(1)
 Sof(F5)=Sof(F6)=Sof(F4)=FVAR(1)
 Sof(F14A)=Sof(F13A)=Sof(F15A)=1-FVAR(2)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C13(H13A,H13B), C17(H17A,H17B), C19(H19A,H19B), C15(H15A,
 H15B), C11(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 C44(H44), C32(H32), C46(H46), C28(H28), C48(H48), C56(H56), C30(H30),
 C40(H40), C52(H52), C36(H36), C38(H38), C54(H54), C22(H22), C23(H23), C24(H24),
  C26(H26), C25(H25)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C),
 C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C12(H12A,H12B,H12C),
  C14(H14A,H14B,H14C)
;
_shelx_res_checksum              85680
_shelx_hkl_checksum              83377
_olex2_submission_special_instructions 'No special instructions were received'