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_1564912
_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         '[Fe3O(C8H4O4)3(C3H7NO3)BF4]'
_chemical_formula_sum            'C33 H33 B F4 Fe3 N3 O16'
_chemical_formula_weight         981.98
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc28392s
_audit_creation_date             2020-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-08 deposited with the CCDC.	2021-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   12.6391(8)
_cell_length_b                   12.6391(8)
_cell_length_c                   18.3551(14)
_cell_measurement_reflns_used    8599
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.90
_cell_volume                     2539.3(3)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16518
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.292
_diffrn_reflns_theta_min         2.896
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0760 before and 0.0537 after correction. The Ratio of minimum to maximum transmission is 0.8788. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2161
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0428P)^2^+8.1639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1390
_reflns_Friedel_coverage         0.760
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                2120
_reflns_number_total             2161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1mh01663f2.cif
_cod_data_source_block           Fe3ODMF3BDC3BF4
_cod_depositor_comments
'Adding full bibliography for 1564910--1564914.cif.'
_cod_original_cell_volume        2539.3(4)
_cod_database_code               1564912
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.898
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.89(6)
 0.11(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 F2-B1 = F1-B1
 1.365 with sigma of 0.02
 F1_$2-F2_$2
 2.22 with sigma of 0.02
 F1-F2
 2.22 with sigma of 0.02
 O1S-C2S_$1
 1.236 with sigma of 0.02
 N3S_$1-C4S_$1 = N3S-C4T
 1.454 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C4S \\sim C4T \\sim N3S \\sim C2S \\sim O1S: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
F2 \\sim B1 \\sim F1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
5. Others
 Fixed Sof: C2S(0.5) H2S(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5) C4T(0.5)
 F1(0.33333) F2(0.33333) B1(0.16667)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C2S(H2S)
6.b Idealised Me refined as rotating group:
 C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              2378
_shelx_fab_checksum              46730
_olex2_submission_special_instructions 'No special instructions were received'