C-H Bond Oxidation Catalyzed by an Imine-Based Iron Complex: A Mechanistic Insight.
Olivo, Giorgio; Nardi, Martina; Vìdal, Diego; Barbieri, Alessia; Lapi, Andrea; Gómez, Laura; Lanzalunga, Osvaldo; Costas, Miquel; Di Stefano, Stefano; Inorganic chemistry 54 (2015) 10141–10152; doi:10.1021/acs.inorgchem.5b01500

data_4346432
_publ_section_title
;
 C-H Bond Oxidation Catalyzed by an Imine-Based Iron Complex: A
 Mechanistic Insight.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10141
_journal_page_last               10152
_journal_paper_doi               10.1021/acs.inorgchem.5b01500
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C24 H22 Fe N6, C F3 O3 S, Cl O4'
_chemical_formula_sum            'C25 H22 Cl F3 Fe N6 O7 S'
_chemical_formula_weight         698.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.8510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9977(10)
_cell_length_b                   13.7820(10)
_cell_length_c                   16.4446(12)
_cell_measurement_reflns_used    7999
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.19
_cell_volume                     2847.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21207
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.193
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.592536
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v2.10 BRUKER 2001'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6362
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0685
_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^)+(0.1393P)^2^+1.6341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1761
_refine_ls_wR_factor_ref         0.1814
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                5978
_reflns_number_total             6362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01500_si_003.cif
_cod_data_source_block           x3
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4346432
_shelxl_version_number           2013-3
_shelx_res_checksum              98796
_shelx_hkl_checksum              73931