Fluorido-bridged robust metal-organic frameworks for efficient C<sub>2</sub>H<sub>2</sub>/CO<sub>2</sub> separation under moist conditions.
Gu, Yi-Ming; Yuan, You-You; Chen, Cai-Lin; Zhao, Sheng-Sheng; Sun, Tian-Jun; Han, Yu; Liu, Xiao-Wei; Lai, Zhiping; Wang, Shu-Dong; Chemical science 14 (2023) 1472–1478; doi:10.1039/d2sc06699h

data_1568298
_publ_section_title
;
 Fluorido-bridged robust metal-organic frameworks for efficient
 C<sub>2</sub>H<sub>2</sub>/CO<sub>2</sub> separation under moist
 conditions.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              1472
_journal_page_last               1478
_journal_paper_doi               10.1039/d2sc06699h
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C24 H8 F14 Fe6 O20, 6(C2 H7 N)'
_chemical_formula_sum            'C36 H50 F14 Fe6 N6 O20'
_chemical_formula_weight         1487.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2020-12-15 deposited with the CCDC.	2023-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8365(11)
_cell_length_b                   18.0784(13)
_cell_length_c                   20.7460(12)
_cell_measurement_reflns_used    7155
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      26.53
_cell_measurement_theta_min      2.56
_cell_volume                     6314.6(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_unetI/netI     0.1094
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43177
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         2.306
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.449
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1268 before and 0.0620 after correction.
The Ratio of minimum to maximum transmission is 0.8667.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       plate
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         14488
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0642P)^2^+16.6884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1689
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                9812
_reflns_number_total             14488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06699h2.cif
_cod_data_source_block           1_pl
_cod_depositor_comments          'Adding full bibliography for 1568298.cif.'
_cod_database_code               1568298
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.531
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(3)
 0.48(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N02W-H02W
 0.91 with sigma of 0.02
 H02W-C03W
 2 with sigma of 0.02
 H02W-C03W = C03W-C044
 2 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N1 \\sim C26: within 2A with sigma of 0.0001 and sigma for terminal atoms of
0.0002 within 2A
F00S \\sim O6 \\sim O5 \\sim F3 \\sim O4 \\sim O1 \\sim O2 \\sim O3: within 2A
with sigma of 0.0001 and sigma for terminal atoms of 0.0002 within 2A
O16 \\sim F9 \\sim F10 \\sim O14 \\sim F12 \\sim F13 \\sim O19 \\sim O18:
within 2A with sigma of 0.0001 and sigma for terminal atoms of 0.0002 within 2A
F5 \\sim F6 \\sim O7 \\sim O8: within 2A with sigma of 0.0001 and sigma for
terminal atoms of 0.0002 within 2A
C5 \\sim O \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.00001 and
sigma for terminal atoms of 0.00002 within 2A
C04K \\sim C048: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
C04J \\sim C04D \\sim C03Z \\sim C03O \\sim C046 \\sim C04E \\sim C03W \\sim
C044 \\sim C04K \\sim C048: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Uanis(C04K) = Uanis(C048)
5.a Riding coordinates:
 N02J(H02J), N02K(H02K)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C12(H12), C21(H21), C4(H4), C3(H3), C22(H22), C11(H11),
 N02H(H02H)
5.c Idealised Me refined as rotating group:
 C04D(H04A,H04B,H04C), C04J(H04D,H04E,H04F), C048(H04G,H04H,H04I), C04K(H04J,
 H04K,H04L), C046(H04M,H04N,H04O), C04E(H04P,H04Q,H04R), C03O(H03A,H03B,H03C),
 C03Z(H03D,H03E,H03F), C03W(H03G,H03H,H03I), C044(H04S,H04T,H04U), C26(H26A,
 H26B,H26C), C25(H25A,H25B,H25C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              11970
_shelx_fab_checksum              10226
_olex2_submission_special_instructions 'No special instructions were received'