Air oxidation-induced single-crystal-to-single-crystal transformation of a mixed-valence tetranuclear Fe(II)-Fe(III) complex
Shin, Jong Won; Ullah , Ihsan; Tokunaga, Ryuya; Hayami, Shinya; Min, Kil Sik; Dalton Transactions  (2022) –; doi:10.1039/D2DT02551E

data_7711241
_publ_section_title
;
 Air oxidation-induced single-crystal-to-single-crystal transformation of
 a mixed-valence tetranuclear Fe(II)-Fe(III) complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02551E
_journal_year                    2022
_chemical_formula_moiety         'C44 H58 Fe4 N12 O8 Se4, 5(C H4 O)'
_chemical_formula_sum            'C49 H78 Fe4 N12 O13 Se4'
_chemical_formula_weight         1582.46
_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
;
2022-09-06 deposited with the CCDC.	2022-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.52(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.912(4)
_cell_length_b                   17.656(4)
_cell_length_c                   20.462(4)
_cell_measurement_reflns_used    138195
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.50
_cell_measurement_theta_min      0.37
_cell_volume                     6399(3)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL BL2D-SMDC Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    ORTEP
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.65000
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41155
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        22.955
_diffrn_reflns_theta_max         29.620
_diffrn_reflns_theta_min         1.489
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    2.523
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.098
_refine_diff_density_min         -1.723
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.00272(14)
_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   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         11675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0746P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9130
_reflns_number_total             11675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02551e2.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7711241
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.632
_shelx_estimated_absorpt_t_max   0.928
_shelx_res_checksum              68810
_shelx_hkl_checksum              74835