Intercepting a Transient Non-Hemic Pyridine N-Oxide Fe(III) Species Involved in Oxygen Atom Transfer Reactions
Vo, Nhat Tam; Herrero, Christian; Guillot, Régis; Inceoglu, Tanya; Leibl, Winfried; Clémancey, Martin; Dubourdeaux, Patrick; Blondin, Geneviève; Aukauloo, Ally; Sircoglou, Marie; Chemical Communications  (2021) –; doi:10.1039/D1CC04521K

data_7129160
_publ_section_title
;
 Intercepting a Transient Non-Hemic Pyridine N-Oxide Fe(III) Species
 Involved in Oxygen Atom Transfer Reactions
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC04521K
_journal_year                    2021
_chemical_formula_moiety         'C25 H12 Cl2 F5 Fe N4 [+ 7/9 (C2 H3 N)]'
_chemical_formula_sum            'C25 H12 Cl2 F5 Fe N4'
_chemical_formula_weight         590.14
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-11-15 deposited with the CCDC.	2021-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   22.4084(16)
_cell_length_b                   22.4084(16)
_cell_length_c                   25.9110(19)
_cell_measurement_reflns_used    8343
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.62
_cell_volume                     11267.7(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker VENTURE PHOTON100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1980
_diffrn_reflns_av_unetI/netI     0.1140
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            100553
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.530
_diffrn_reflns_theta_min         2.623
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.9581
_exptl_absorpt_correction_T_min  0.8971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'apex3 Bruker'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       plate
_exptl_crystal_F_000             5310
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1627
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+72.3132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2070
_reflns_number_total             3835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04521k2.cif
_cod_data_source_block           FeDPPyCl2_ACN_Et2O
_cod_original_cell_volume        11267.7(18)
_cod_database_code               7129160
_shelx_estimated_absorpt_t_min   0.934
_shelx_estimated_absorpt_t_max   0.966
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              38255
_shelx_hkl_checksum              63378
_shelx_fab_checksum              89333