Crystal structure of a water oxidation catalyst solvate with composition (NH<sub>4</sub>)<sub>2</sub>[Fe<sup>IV</sup>(<i>L</i>-6H)]·3CH<sub>3</sub>COOH (<i>L</i> = clathrochelate ligand).
Plutenko, Maksym O.; Shylin, Sergii I.; Shova, Sergiu; Blinder, Aleksander V.; Fritsky, Igor O.; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 25–28; doi:10.1107/S2056989023010514

data_2022964
_publ_section_title
;
 Crystal structure of a water oxidation catalyst solvate with composition
 (NH<sub>4</sub>)<sub>2</sub>[Fe<sup>IV</sup>(<i>L</i>-6H)]&#xb7;3CH<sub>3</sub>COOH
 (<i>L</i> = clathrochelate ligand).
;
_journal_coeditor_code           WM5703
_journal_issue                   'Pt 1'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              25
_journal_page_last               28
_journal_paper_doi               10.1107/S2056989023010514
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '(N H4)2 [Fe (C12 H12 N12 O6)], 3C2 H4 O2'
_chemical_formula_moiety
'C12 H12 Fe N12 O6, 2(C H2 O), 2(C2 H4 O2), 2(H4 N)'
_chemical_formula_sum            'C18 H32 Fe N14 O12'
_chemical_formula_weight         692.42
_chemical_name_systematic
'Diammonium {\m-1,3,4,7,8,10,12,13,16,17,19,22-dodecaazatetracyclo[8.8.4.1^3,17^.1^8,12^]tetracosane-5,6,14,15,20,21-hexaonato}ferrate(IV) acetic acid trisolvate'
_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   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 107.616(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5352(2)
_cell_length_b                   11.51780(10)
_cell_length_c                   16.0472(2)
_cell_measurement_reflns_used    18947
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      34.5490
_cell_measurement_theta_min      3.7530
_cell_volume                     2736.70(6)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
CrystaMaker (CrystalMaker, 2017)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Rigaku SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0123
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19869
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         3.146
_diffrn_source                   micro-source
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlisPro (Rigaku OD, 2015) based on
analytical numerical absorption correction using a multifaceted crystal
model (Clark & Reid, 1995)]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.131
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         2431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0287P)^2^+4.4687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0643
_reflns_number_gt                2345
_reflns_number_total             2431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5703sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2022964.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2022964
_cod_database_fobs_code          2022964
_shelx_estimated_absorpt_t_min   0.762
_shelx_estimated_absorpt_t_max   0.921
_shelx_hkl_checksum              43835
_shelx_res_checksum              81827