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_1576784
_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         'C20 H40 Fe N2 O P2, C32 H12 B F24'
_chemical_formula_sum            'C52 H52 B F24 Fe N2 O P2'
_chemical_formula_weight         1305.55
_chemical_name_systematic        C52H53BF24FeN2OP2
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-07-07
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-23 deposited with the CCDC.	2026-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                102.952(4)
_cell_angle_beta                 92.919(4)
_cell_angle_gamma                95.205(4)
_cell_formula_units_Z            2
_cell_length_a                   12.4178(15)
_cell_length_b                   12.6184(15)
_cell_length_c                   18.884(2)
_cell_measurement_reflns_used    9444
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.395
_cell_measurement_theta_min      2.595
_cell_volume                     2864.1(6)
_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  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_detector                 'Bruker Photon II area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            137121
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.423
_diffrn_reflns_theta_min         1.921
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       block
_exptl_crystal_F_000             1326
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.576
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         11723
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0678
_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^)+(0.0629P)^2^+8.5349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11297
_reflns_number_total             11723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc07656k2.cif
_cod_data_source_block           final
_cod_depositor_comments
'Adding full bibliography for 1576777--1576784.cif.'
_cod_original_cell_volume        2864.0(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1576784
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.859
_olex2_refinement_description
;
1. Restrained distances
 H2A-N2
 1 with sigma of 0.02
 H2B-N2
 1 with sigma of 0.02
 C28-F4 \\sim C28-F5 \\sim C28-F6
 with sigma of 0.02
 F21-C51 \\sim F21A-C51
 with sigma of 0.02
 C28-F4A \\sim C28-F5A \\sim C28-F6A
 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
 F19-C51 \\sim F19A-C51
 with sigma of 0.02
 C51-F20 \\sim C51-F20A
 with sigma of 0.02
2. Rigid body (RIGU) restrains
 F5A, F4, F6, F4A, F5, F6A, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(F6A)=Sof(F4A)=Sof(F4)=1-FVAR(1)
 Sof(F6)=Sof(F5)=Sof(F5A)=FVAR(1)
 Sof(F20A)=Sof(F19A)=Sof(F21A)=1-FVAR(2)
 Sof(F21)=Sof(F19)=Sof(F20)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C11(H11A,H11B), C6(H6A,H6B), C19(H19A,H19B), C15(H15A,H15B),
 C17(H17A,H17B), C16(H16A,H16B)
4.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C42(H42), C30(H30), C32(H32), C50(H50), C46(H46), C48(H48),
 C38(H38), C40(H40), C22(H22), C26(H26), C24(H24)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20(H20A,H20B,H20C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              15944
_shelx_hkl_checksum              57451
_olex2_submission_special_instructions 'No special instructions were received'