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_7713226
_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 H29 F3 Fe N5 O3 S, C F3 O3 S'
_chemical_formula_sum            'C19 H29 F6 Fe N5 O6 S2'
_chemical_formula_weight         657.44
_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                 99.9130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6666(4)
_cell_length_b                   14.8989(6)
_cell_length_c                   18.1683(8)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      66.64
_cell_measurement_theta_min      3.86
_cell_volume                     2577.56(19)
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36732
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.663
_diffrn_reflns_theta_max         66.663
_diffrn_reflns_theta_min         3.860
_exptl_absorpt_coefficient_mu    7.037
_exptl_absorpt_correction_T_max  0.6294
_exptl_absorpt_correction_T_min  0.2598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'apex3 bruker'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.00098(7)
_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   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0216P)^2^+2.9748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4421
_reflns_number_total             4561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00393k2.cif
_cod_data_source_block           '[((cyclenCB-CH2py)FeIIOTf)OTf]'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7713226
_shelx_estimated_absorpt_t_min   0.288
_shelx_estimated_absorpt_t_max   0.644
_shelx_res_checksum              3959