#------------------------------------------------------------------------------
#$Date: 2021-12-07 06:03:46 +0200 (Tue, 07 Dec 2021) $
#$Revision: 271237 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/49/1564910.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_1564910
loop_
_publ_author_name
'Bara, Dominic'
'Meekel, Emily G.'
'Pakamorė, Ignas'
'Wilson, Claire'
'Ling, Sanliang'
'Forgan, Ross S.'
_publ_section_title
;
 Exploring and expanding the Fe-terephthalate metal-organic framework
 phase space by coordination and oxidation modulation.
;
_journal_issue                   12
_journal_name_full               'Materials horizons'
_journal_page_first              3377
_journal_page_last               3386
_journal_paper_doi               10.1039/d1mh01663f
_journal_volume                  8
_journal_year                    2021
_chemical_formula_moiety         Fe(III)2Fe(II)3(O)(C8H3O4Br)3(H2O)3
_chemical_formula_sum            'C24 H15 Br3 Fe3 O16'
_chemical_formula_weight         966.64
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d :2'
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc28395w
_audit_creation_date             2020-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-07 deposited with the CCDC.	2021-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3069(11)
_cell_length_b                   16.3069(11)
_cell_length_c                   52.852(4)
_cell_measurement_reflns_used    8291
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.30
_cell_volume                     14054.1(17)
_computing_cell_refinement       'SAINT V8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            35038
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.409
_diffrn_reflns_theta_min         2.296
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.350
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
 wR2(int) was 0.1261 before and 0.0811 after correction. The Ratio 
 of minimum to maximum transmission is 0.6536. The λ/2 correction 
 factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.914
_exptl_crystal_description       tablet
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         4705
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0843
_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/[σ²(Fo²)+(0.1523P)²+53.8512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2480
_refine_ls_wR_factor_ref         0.2759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3171
_reflns_number_total             4705
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1mh01663f2.cif
_cod_data_source_block           Fe_BDC_Br
_cod_depositor_comments
'Adding full bibliography for 1564910--1564914.cif.'
_cod_original_cell_volume        14054(2)
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               1564910
_shelx_shelxl_version_number     2018/3
_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_max   0.872
_shelx_estimated_absorpt_t_min   0.511
_olex2_refinement_description
;
1. Restrained distances
 C4-C2 = C4-C3_$1 = C3_$1-C2_$1 = C6_$1-C2_$1 = C6_$1-C5 = C5-C2
 1.39 with sigma of 0.02
 Br2-C5 = Br2A-C5 = Br1A-C4 = Br1-C4 = Br3-C9 = Br3A-C9
 1.899 with sigma of 0.02
 C9A-C9_$2 = C9-C8 = C9A-C8
 1.39 with sigma of 0.02
2. Restrained planarity
 C2, C2_$1, C3_$1, C4, C5, C6_$1
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Br1 \\sim Br1A \\sim Br2 \\sim Br2A \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim
C6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Br3 \\sim Br3A \\sim C9 \\sim C9A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: Br1(0.125) Br1A(0.125) Br2(0.125) Br2A(0.125) Br3(0.125)
 Br3A(0.125) C3(0.5) C4(0.5) C5(0.5) C6(0.5) C9(0.5) C9A(0.5)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'
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
Br1 Br 0.6630(8) -0.0242(6) 0.4295(2) 0.137(4) Uani 0.125 1 d D U . A 2
Br1A Br 0.7193(8) 0.0094(7) 0.43733(15) 0.134(4) Uani 0.125 1 d D U . A 1
Br2 Br 0.6978(6) 0.1393(6) 0.32791(14) 0.111(3) Uani 0.125 1 d D U . B 1
Br2A Br 0.7342(6) 0.1742(5) 0.33617(17) 0.092(3) Uani 0.125 1 d D U . B 2
Br3 Br 0.6890(5) 0.0438(6) 0.4762(2) 0.107(3) Uani 0.125 1 d D U . . .
Br3A Br 0.6722(6) 0.0066(6) 0.46428(19) 0.109(3) Uani 0.125 1 d D U . . .
Fe1 Fe 0.500000 0.250000 0.37814(2) 0.0309(3) Uani 1 4 d S T P . .
Fe2 Fe 0.59983(5) 0.250000 0.43280(2) 0.0327(3) Uani 1 2 d S T P . .
O1 O 0.500000 0.250000 0.41599(10) 0.0291(11) Uani 1 4 d S T P . .
O2 O 0.5918(2) 0.1575(2) 0.37600(7) 0.0511(8) Uani 1 1 d . . . . .
O3 O 0.6557(2) 0.1628(2) 0.41285(7) 0.0623(11) Uani 1 1 d . . . . .
O4 O 0.5678(2) 0.1622(3) 0.45810(8) 0.0682(12) Uani 1 1 d . . . . .
O5 O 0.500000 0.250000 0.33858(14) 0.065(2) Uani 1 4 d S T P . .
O6 O 0.7112(3) 0.250000 0.45375(11) 0.0656(15) Uani 1 2 d S T P . .
C1 C 0.6451(3) 0.1368(3) 0.39075(10) 0.0459(11) Uani 1 1 d . . . . .
C2 C 0.7059(3) 0.0712(3) 0.38265(11) 0.0561(12) Uani 1 1 d D U . . .
C3 C 0.7045(7) 0.0392(6) 0.3588(2) 0.060(2) Uiso 0.5 1 d D U . . .
C4 C 0.7309(7) 0.0106(7) 0.40026(19) 0.067(3) Uiso 0.5 1 d D U . . .
C5 C 0.7351(8) 0.0745(7) 0.3574(2) 0.077(3) Uiso 0.5 1 d D U . . .
C6 C 0.7637(7) 0.0427(7) 0.4001(2) 0.063(3) Uiso 0.5 1 d D U . . .
C7 C 0.500000 0.1362(4) 0.46488(13) 0.0494(16) Uani 1 2 d S T P . .
C8 C 0.500000 0.0654(5) 0.48299(14) 0.061(2) Uani 1 2 d DS T P . .
C9 C 0.5750(7) 0.0163(9) 0.4859(3) 0.082(3) Uiso 0.5 1 d D U . . .
C9A C 0.5704(7) 0.0471(8) 0.4961(3) 0.068(3) Uiso 0.5 1 d D U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
O O 0.0106 0.0060 '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'
loop_
_citation_id
_citation_doi
_citation_year
1 10.33774/chemrxiv-2021-lkt60 2021
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
C5 Br2A Br2A 145.5(5) . 29 ?
Br3A Br3 C9 75.4(9) . . ?
Br3 Br3A C9 77.6(9) . . ?
O1 Fe1 O2 93.03(10) . 22_655 ?
O1 Fe1 O2 93.03(10) . . ?
O1 Fe1 O2 93.03(10) . 10_554 ?
O1 Fe1 O2 93.03(10) . 29 ?
O1 Fe1 O5 180.0 . . ?
O2 Fe1 O2 89.4(2) 22_655 . ?
O2 Fe1 O2 173.9(2) 22_655 29 ?
O2 Fe1 O2 173.9(2) 10_554 . ?
O2 Fe1 O2 90.3(2) 22_655 10_554 ?
O2 Fe1 O2 89.4(2) 29 10_554 ?
O2 Fe1 O2 90.3(2) 29 . ?
O5 Fe1 O2 86.97(10) . 29 ?
O5 Fe1 O2 86.97(10) . . ?
O5 Fe1 O2 86.97(10) . 22_655 ?
O5 Fe1 O2 86.97(10) . 10_554 ?
O1 Fe2 O3 98.50(15) . . ?
O1 Fe2 O3 98.50(15) . 29 ?
O1 Fe2 O4 95.16(15) . 29 ?
O1 Fe2 O4 95.16(15) . . ?
O1 Fe2 O6 177.3(2) . . ?
O3 Fe2 O3 91.2(3) . 29 ?
O3 Fe2 O4 166.30(16) 29 . ?
O3 Fe2 O4 166.30(16) . 29 ?
O3 Fe2 O4 87.84(19) 29 29 ?
O3 Fe2 O4 87.84(19) . . ?
O3 Fe2 O6 83.41(16) 29 . ?
O3 Fe2 O6 83.41(16) . . ?
O4 Fe2 O4 89.9(3) 29 . ?
O4 Fe2 O6 82.91(16) . . ?
O4 Fe2 O6 82.91(16) 29 . ?
Fe2 O1 Fe1 118.62(15) . . ?
Fe2 O1 Fe1 118.63(15) 10_554 . ?
Fe2 O1 Fe2 122.8(3) . 10_554 ?
C1 O2 Fe1 131.8(3) . . ?
C1 O3 Fe2 132.2(3) . . ?
C7 O4 Fe2 131.5(4) . . ?
O2 C1 O3 126.9(4) . . ?
O2 C1 C2 118.8(4) . . ?
O3 C1 C2 114.3(4) . . ?
C3 C2 C1 121.3(6) . . ?
C3 C2 C4 110.1(7) . . ?
C3 C2 C5 31.8(6) . . ?
C3 C2 C6 119.5(8) . . ?
C4 C2 C1 119.6(6) . . ?
C4 C2 C5 123.2(7) . . ?
C5 C2 C1 117.2(6) . . ?
C6 C2 C1 119.3(6) . . ?
C6 C2 C4 30.8(6) . . ?
C6 C2 C5 113.9(7) . . ?
C2 C3 C4 124.3(9) . 15_535 ?
C2 C3 C6 111.3(9) . 15_535 ?
C4 C3 C6 28.4(6) 15_535 15_535 ?
C2 C4 Br1 123.3(8) . . ?
C2 C4 Br1A 129.2(8) . . ?
C3 C4 Br1 117.2(8) 15_535 . ?
C3 C4 Br1A 113.5(8) 15_535 . ?
C3 C4 C2 115.2(8) 15_535 . ?
C2 C5 Br2 131.1(8) . . ?
C2 C5 Br2A 124.2(8) . . ?
C2 C5 C4 106.5(8) . 15_535 ?
C2 C5 C6 117.1(9) . 15_535 ?
C4 C5 Br2 112.6(8) 15_535 . ?
C4 C5 Br2A 129.2(8) 15_535 . ?
C6 C5 Br2 111.0(8) 15_535 . ?
C6 C5 Br2A 115.0(8) 15_535 . ?
C6 C5 C4 27.2(6) 15_535 15_535 ?
C2 C6 C5 120.6(9) . 15_535 ?
O4 C7 O4 126.7(7) . 22_655 ?
O4 C7 C8 116.6(3) . . ?
O4 C7 C8 116.6(3) 22_655 . ?
C9 C8 C7 119.1(6) . . ?
C9 C8 C7 119.1(6) 22_655 . ?
C9 C8 C9 112.7(12) 22_655 . ?
C9A C8 C7 119.2(6) 22_655 . ?
C9A C8 C7 119.2(6) . . ?
C9A C8 C9 29.8(7) . . ?
C9A C8 C9 29.8(7) 22_655 22_655 ?
C9A C8 C9 121.7(7) . 22_655 ?
C9A C8 C9 121.7(7) 22_655 . ?
C9A C8 C9A 113.6(12) 22_655 . ?
Br3A C9 Br3 26.9(4) . . ?
C8 C9 Br3 129.2(9) . . ?
C8 C9 Br3A 130.9(9) . . ?
C9A C9 Br3 113.0(9) 6_556 . ?
C9A C9 Br3A 112.2(9) 6_556 . ?
C9A C9 C8 115.2(10) 6_556 . ?
C8 C9A C9 123.0(11) . 6_556 ?
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
Br1 C4 1.982(12) . ?
Br1A C4 1.969(12) . ?
Br2 C5 1.978(12) . ?
Br2A Br2A 2.471(15) 29 ?
Br2A C5 1.975(12) . ?
Br3 Br3A 0.917(13) . ?
Br3 C9 1.979(13) . ?
Br3A C9 1.961(13) . ?
Fe1 O1 2.000(6) . ?
Fe1 O2 2.128(3) 22_655 ?
Fe1 O2 2.128(3) . ?
Fe1 O2 2.128(3) 10_554 ?
Fe1 O2 2.128(3) 29 ?
Fe1 O5 2.090(7) . ?
Fe2 O1 1.855(3) . ?
Fe2 O3 1.991(3) 29 ?
Fe2 O3 1.991(3) . ?
Fe2 O4 2.028(3) 29 ?
Fe2 O4 2.028(3) . ?
Fe2 O6 2.128(5) . ?
O2 C1 1.216(6) . ?
O3 C1 1.254(6) . ?
O4 C7 1.237(5) . ?
C1 C2 1.519(6) . ?
C2 C3 1.364(11) . ?
C2 C4 1.418(11) . ?
C2 C5 1.420(11) . ?
C2 C6 1.397(11) . ?
C3 C4 1.404(13) 15_535 ?
C3 C6 1.569(16) 15_535 ?
C5 C6 1.421(13) 15_535 ?
C7 C8 1.501(9) . ?
C8 C9 1.470(12) . ?
C8 C9 1.470(12) 22_655 ?
C8 C9A 1.373(11) . ?
C8 C9A 1.373(11) 22_655 ?
C9 C9A 1.408(12) 6_556 ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.176 0.657 0.052 7120 623 ' '
