New mechanistic insight into intramolecular aromatic ligand hydroxylation and benzyl alcohol oxidation initiated by well-defined (μ-peroxo)diiron(III) complex
Sekino, Mio; Furutachi, Hideki; Tojo, Rina; Hishi, Ayumi; Kajikawa, Hanako; Suzuki, Takatoshi; Suzuki, Kaito; Fujinami, Shuhei; Akine, Shigehisa; Sakata, Yoko; Ohta, Takehiro; Hayami, Shinya; Suzuki, Masatatsu; Chem. Commun.  (2017) –; doi:10.1039/C7CC04382A

data_7120439
_publ_section_title
;
 New mechanistic insight into intramolecular aromatic ligand hydroxylation
 and benzyl alcohol oxidation initiated by well-defined
 (\m-peroxo)diiron(III) complex
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04382A
_journal_year                    2017
_chemical_formula_moiety         C135.60H150.40B2Cl19Fe2N13.40O9.30
_chemical_formula_sum            'C135.6 H150.4 B2 Cl19 Fe2 N13.4 O9.3'
_chemical_formula_weight         2923.55
_chemical_name_common
;
[LFe2(O2)(MeOH)(Ph3CCO2)](Ph4B)2(CH2Cl2)9.5(MeOH)3.3(MeCN)3.4
;
_chemical_name_systematic        1-O2-MeOH
_chemical_properties_physical    ', Heat-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-06 deposited with the CCDC.
2017-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.4186(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.972(3)
_cell_length_b                   35.165(4)
_cell_length_c                   21.803(3)
_cell_measurement_reflns_used    110030
_cell_measurement_temperature    123
_cell_measurement_theta_max      23.049
_cell_measurement_theta_min      2.828
_cell_volume                     14895(3)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 14.4613
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Rigaku Mercury (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1313
_diffrn_reflns_av_unetI/netI     0.0816
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            110030
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        23.049
_diffrn_reflns_theta_max         23.049
_diffrn_reflns_theta_min         2.828
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.5469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC Inc., 2006)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             6069
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/acetonitrile/methanol'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.307
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2003
_refine_ls_number_reflns         20745
_refine_ls_number_restraints     584
_refine_ls_restrained_S_all      1.294
_refine_ls_R_factor_all          0.1890
_refine_ls_R_factor_gt           0.1780
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1592P)^2^+92.4610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4028
_refine_ls_wR_factor_ref         0.4096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19050
_reflns_number_total             20745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04382a3.cif
_cod_data_source_block           ymst21
_cod_original_formula_sum        'C135.60 H150.40 B2 Cl19 Fe2 N13.40 O9.30'
_cod_database_code               7120439
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.819
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              80243