A method for controlled growth of large MIL-88A crystals
Schumann, Erik; Störr, Bianca; Böhme, Uwe; Walter, Dominic; Mertens, Florian; CrystEngComm 27 (2025) 5404–5412; doi:10.1039/D5CE00498E

data_7250673
_publ_section_title
;
 A method for controlled growth of large MIL-88A crystals
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              5404
_journal_page_last               5412
_journal_paper_doi               10.1039/D5CE00498E
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C12 H12 Fe3 O16'
_chemical_formula_sum            'C12 H12 Fe3 O16'
_chemical_formula_weight         579.77
_chemical_name_common            'Eisen-MOF mit Fumarsaeure'
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-02-26 deposited with the CCDC.	2025-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.6085(4)
_cell_length_b                   13.6085(4)
_cell_length_c                   12.7623(5)
_cell_measurement_reflns_used    20888
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.98
_cell_volume                     2046.82(12)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      153
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      ' 316 frames, detector distance = 114 mm'
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29813
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.092
_diffrn_reflns_theta_min         2.352
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.088
_exptl_absorpt_correction_T_max  0.9005
_exptl_absorpt_correction_T_min  0.7945
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    0.941
_exptl_crystal_description       Prism
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1736
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0683
_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^)+(0.1185P)^2^+12.5038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1584
_reflns_number_total             1736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00498e2.cif
_cod_data_source_block           femofc3d_sq
_cod_depositor_comments          'Adding full bibliography for 7250673.cif.'
_cod_original_cell_volume        2046.82(14)
_cod_database_code               7250673
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.796
_shelx_estimated_absorpt_t_max   0.854
_shelx_res_checksum              35907
_shelx_fab_checksum              76466