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#$Date: 2025-10-06 11:24:31 +0300 (Mon, 06 Oct 2025) $
#$Revision: 302567 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/06/7250673.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7250673
loop_
_publ_author_name
'Schumann, Erik'
'Störr, Bianca'
'Böhme, Uwe'
'Walter, Dominic'
'Mertens, Florian'
_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, ω 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/[σ²(Fo²)+(0.1185P)²+12.5038P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.796
_shelx_estimated_absorpt_t_max   0.854
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.76473(8) 0.27223(8) 0.250000 0.0174(3) Uani 1 2 d S T P . .
O1 O 0.666667 0.333333 0.250000 0.0183(15) Uani 1 6 d S T P . .
O2 O 0.8697(3) 0.3747(3) 0.3614(3) 0.0245(7) Uani 1 1 d . . . . .
O3 O 0.8433(3) 0.5251(3) 0.3619(3) 0.0274(8) Uani 1 1 d . . . . .
C1 C 0.8884(4) 0.4695(4) 0.3961(4) 0.0216(9) Uani 1 1 d . . . . .
C2 C 0.9690(4) 0.5219(4) 0.4815(4) 0.0224(9) Uani 1 1 d D . . . .
H2 H 0.950(6) 0.581(4) 0.519(5) 0.034 Uiso 1 1 d D U . . .
O4 O 0.8724(5) 0.2052(5) 0.250000 0.0291(11) Uani 1 2 d DS T P . .
H4A H 0.952(2) 0.231(9) 0.250000 0.044 Uiso 1 2 d DS U P . .
H4B H 0.877(9) 0.138(5) 0.250000 0.044 Uiso 1 2 d DS U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
20 30 23 0.0748
30 3 29 0.0786
15 -13 0 0.0742
6 5 -6 0.0971
-17 30 16 0.0785
-30 8 -1 0.0824
-15 -3 -13 0.0580
-30 15 -11 0.0862
-30 19 15 0.0981
-9 -23 30 0.1174
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O3 95.75(11) . 12_666 ?
O1 Fe1 O3 95.75(11) . 3_665 ?
O3 Fe1 O3 90.9(2) 12_666 3_665 ?
O1 Fe1 O2 96.20(10) . . ?
O3 Fe1 O2 168.04(15) 12_666 . ?
O3 Fe1 O2 88.07(16) 3_665 . ?
O1 Fe1 O2 96.20(10) . 10_556 ?
O3 Fe1 O2 88.07(16) 12_666 10_556 ?
O3 Fe1 O2 168.04(15) 3_665 10_556 ?
O2 Fe1 O2 90.4(2) . 10_556 ?
O1 Fe1 O4 180.00(16) . . ?
O3 Fe1 O4 84.25(15) 12_666 . ?
O3 Fe1 O4 84.25(15) 3_665 . ?
O2 Fe1 O4 83.79(15) . . ?
O2 Fe1 O4 83.80(15) 10_556 . ?
Fe1 O1 Fe1 120.0 3_665 . ?
Fe1 O1 Fe1 120.0 3_665 2_655 ?
Fe1 O1 Fe1 120.0 . 2_655 ?
C1 O2 Fe1 132.0(3) . . ?
C1 O3 Fe1 132.4(3) . 2_655 ?
O2 C1 O3 125.4(4) . . ?
O2 C1 C2 118.7(4) . . ?
O3 C1 C2 115.9(4) . . ?
C2 C2 C1 122.3(6) 7_766 . ?
C2 C2 H2 128(4) 7_766 . ?
C1 C2 H2 107(4) . . ?
Fe1 O4 H4A 139(7) . . ?
Fe1 O4 H4B 146(7) . . ?
H4A O4 H4B 75(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.8925(9) . ?
Fe1 O3 2.003(4) 12_666 ?
Fe1 O3 2.003(4) 3_665 ?
Fe1 O2 2.004(3) . ?
Fe1 O2 2.004(3) 10_556 ?
Fe1 O4 2.077(5) . ?
O2 C1 1.263(6) . ?
O3 C1 1.266(6) . ?
C1 C2 1.456(7) . ?
C2 C2 1.339(10) 7_766 ?
C2 H2 1.071(10) . ?
O4 H4A 0.954(10) . ?
O4 H4B 0.951(10) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Fe1 O1 Fe1 45.77(12) 12_666 . . 3_665 ?
O3 Fe1 O1 Fe1 -45.77(12) 3_665 . . 3_665 ?
O2 Fe1 O1 Fe1 -134.45(11) . . . 3_665 ?
O2 Fe1 O1 Fe1 134.44(11) 10_556 . . 3_665 ?
O3 Fe1 O1 Fe1 -134.23(12) 12_666 . . 2_655 ?
O3 Fe1 O1 Fe1 134.23(12) 3_665 . . 2_655 ?
O2 Fe1 O1 Fe1 45.55(11) . . . 2_655 ?
O2 Fe1 O1 Fe1 -45.56(11) 10_556 . . 2_655 ?
Fe1 O2 C1 O3 -2.6(8) . . . . ?
Fe1 O2 C1 C2 178.1(3) . . . . ?
Fe1 O3 C1 O2 1.9(8) 2_655 . . . ?
Fe1 O3 C1 C2 -178.8(3) 2_655 . . . ?
O2 C1 C2 C2 5.8(9) . . . 7_766 ?
O3 C1 C2 C2 -173.5(6) . . . 7_766 ?
