Exploring and expanding the Fe-terephthalate metal-organic framework phase space by coordination and oxidation modulation.
Bara, Dominic; Meekel, Emily G.; Pakamorė, Ignas; Wilson, Claire; Ling, Sanliang; Forgan, Ross S.; Materials horizons 8 (2021) 3377–3386; doi:10.1039/d1mh01663f

data_1564910
_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       '\f and \w 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 \l/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/[\s^2^(Fo^2^)+(0.1523P)^2^+53.8512P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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)
;
_shelx_res_checksum              134
_shelx_fab_checksum              23393
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'