Efficient capture of trace benzene vapor by metal-organic frameworks modified with macrocyclic pyridyl ligands.
Liang, Gang; Chen, De-Jian; Long, Zhu-Jun; Zhuo, Hao; Zhong, Xiao-Feng; Chen, Xiong-Hai; Shao, Huai-Yu; Mo, Zong-Wen; Chen, Xiao-Ming; Chemical science 16 (2025) 19867–19875; doi:10.1039/d5sc05093f

data_1575781
_publ_section_title
;
 Efficient capture of trace benzene vapor by metal-organic frameworks
 modified with macrocyclic pyridyl ligands.
;
_journal_issue                   42
_journal_name_full               'Chemical science'
_journal_page_first              19867
_journal_page_last               19875
_journal_paper_doi               10.1039/d5sc05093f
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C84 H45 Fe3 N9 O13, 6(C4.5 H4.5), [+ solvents]'
_chemical_formula_sum            'C99 H60 Fe3 N9 O13'
_chemical_formula_weight         1751.11
_space_group_crystal_system      hexagonal
_space_group_IT_number           187
_space_group_name_Hall           'P -6 2'
_space_group_name_H-M_alt        'P -6 m 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-03-14 deposited with the CCDC.	2025-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   19.1879(7)
_cell_length_b                   19.1879(7)
_cell_length_c                   11.9176(5)
_cell_measurement_reflns_used    3441
_cell_measurement_temperature    150.00(13)
_cell_measurement_theta_max      72.9000
_cell_measurement_theta_min      4.5420
_cell_volume                     3799.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.00(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -24.00  24.00   0.50   13.07    --   48.37 -12.00-120.00   96
  2  \w    -84.00 -24.00   0.50   52.29    --  -91.75 119.00 153.00  120
  3  \w   -137.00 -78.00   0.50   52.29    --  -91.75-121.00 148.00  118
  4  \w    103.00 170.00   0.50   52.29    --  109.07 124.00 128.00  134
  5  \w     40.00 109.00   0.50   52.29    --  109.07-121.00 148.00  138
  6  \w     42.00  96.00   0.50   52.29    --  109.07 -99.00 -90.00  108
  7  \w     37.00  63.00   0.50   52.29    --  109.07 -57.00 -90.00   52
  8  \w     84.00 110.00   0.50   52.29    --  109.07-125.00 120.00   52
  9  \w     44.00  70.00   0.50   52.29    --  109.07-125.00 120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0584658000
_diffrn_orient_matrix_UB_12      0.0322031000
_diffrn_orient_matrix_UB_13      0.0169173000
_diffrn_orient_matrix_UB_21      0.0707301000
_diffrn_orient_matrix_UB_22      0.0868275000
_diffrn_orient_matrix_UB_23      -0.0111029000
_diffrn_orient_matrix_UB_31      -0.0139412000
_diffrn_orient_matrix_UB_32      -0.0034875000
_diffrn_orient_matrix_UB_33      -0.1276364000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1109
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11221
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.574
_diffrn_reflns_theta_min         4.566
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.591
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    0.765
_exptl_crystal_description       block
_exptl_crystal_F_000             899
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.365
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.36(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.263
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2755
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.295
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.1041
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2887
_refine_ls_wR_factor_ref         0.3106
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_full    0.850
_reflns_Friedel_fraction_max     0.807
_reflns_number_gt                2174
_reflns_number_total             2755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05093f2.cif
_cod_data_source_block           C6H6@WYU-107
_cod_depositor_comments
'Adding full bibliography for 1575776--1575784.cif.'
_cod_database_code               1575781
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.782
_shelx_estimated_absorpt_t_min   0.625
_reflns_odcompleteness_completeness 97.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.63626
 0.36374
2. Restrained distances
 C7-C8_$1
 1.39 with sigma of 0.02
 C35B-C31B
 1.39 with sigma of 0.02
 C7-C8
 2.8 with sigma of 0.02
 C31B-C35B_$3
 2.8 with sigma of 0.02
 C6-C5
 1.4 with sigma of 0.002
 C7-C7_$2
 2.3 with sigma of 0.01
 C8_$1-C7
 1.39 with sigma of 0.002
 C31B-C35B
 1.39 with sigma of 0.02
 C35B_$3-C35B_$4
 2.3 with sigma of 0.02
 C35B_$3-C31B
 2.8 with sigma of 0.02
3. Restrained planarity
 C31B, C31B_$4, C35B_$4, C35B, C31B_$3, C35B_$3
 with sigma of 0.1
4. Rigid bond restraints
 C31B, C35B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C31B \\sim C35B: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
C31B \\sim C31B \\sim C31B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C35B \\sim C31B: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
C5 \\sim C6: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
C7 \\sim C8: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
Uanis(C35B) \\sim Ueq, Uanis(C31B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C31B) \\sim Ueq, Uanis(C35B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(N003) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C00G) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(C9) \\sim Ueq, Uanis(C00G) \\sim Ueq, Uanis(N003) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Fixed Sof: H002(0.083333) C0(0.5) H0(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5)
 C4(0.5) H4(0.5) C7(0.125) H7(0.125) C8(0.125) H8(0.125) C31B(0.125)
 H31B(0.125) C35B(0.125) H35B(0.125)
7.a Riding coordinates:
 C0(H0), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C31B(H31B),
 C35B(H35B)
7.b Ternary CH refined with riding coordinates:
 O002(H002), C00B(H00B)
7.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C00F(H00F), C00G(H00G)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7080
_shelx_fab_checksum              33947
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 6.493
_oxdiff_exptl_absorpt_empirical_full_min 0.243