Catalytic oxidation properties of an acid-resistant cross-bridged cyclen Fe(II) complex. Influence of the rigid donor backbone and protonation on the reactivity.
Rebilly, Jean-Noël; Herrero, Christian; Sénéchal-David, Katell; Guillot, Régis; Banse, Frédéric; Dalton Transactions  (2023) –; doi:10.1039/D3DT00393K

data_7713227
_publ_section_title
;
 Catalytic oxidation properties of an acid-resistant cross-bridged cyclen
 Fe(II) complex. Influence of the rigid donor backbone and protonation on
 the reactivity.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00393K
_journal_year                    2023
_chemical_formula_moiety         'C18 H32 Fe N5 O, 2(C F3 O3 S)'
_chemical_formula_sum            'C20 H32 F6 Fe N5 O7 S2'
_chemical_formula_weight         688.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-08 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.596(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0222(9)
_cell_length_b                   12.1505(6)
_cell_length_c                   12.1044(5)
_cell_measurement_reflns_used    8407
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      2.18
_cell_volume                     2750.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            62137
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.535
_diffrn_reflns_theta_min         1.999
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  0.9461
_exptl_absorpt_correction_T_min  0.8791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX2'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       plate
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.753
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         8322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.0743
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1161P)^2^+2.6530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4707
_reflns_number_total             8322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00393k2.cif
_cod_data_source_block           '[((cyclenCB-CH2py)FeIII(OMe))OTf2]'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7713227
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              82369