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_7129159
_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 '
_chemical_formula_sum            'C25 H12 Cl2 F5 Fe N4'
_chemical_formula_weight         590.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                 104.497(8)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   19.907(3)
_cell_length_b                   13.511(2)
_cell_length_c                   26.718(5)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      66.62
_cell_measurement_theta_min      3.42
_cell_volume                     6957(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker VENTURE PHOTON100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            52122
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.749
_diffrn_reflns_theta_max         66.749
_diffrn_reflns_theta_min         3.417
_exptl_absorpt_coefficient_mu    7.755
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX3'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       plate
_exptl_crystal_F_000             3540
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.407
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.000081(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         6155
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          1.693
_refine_ls_shift/su_mean         0.047
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+22.4063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5818
_reflns_number_total             6155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04521k2.cif
_cod_data_source_block           FeDPPyCl2_Acetone
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7129159
_shelx_estimated_absorpt_t_min   0.238
_shelx_estimated_absorpt_t_max   0.698
_shelx_res_checksum              10570
_shelx_hkl_checksum              74