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_1575783
_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         'C81.998 H38 Fe3 N6 O19'
_chemical_formula_sum            'C82 H38 Fe3 N6 O19'
_chemical_formula_weight         1578.73
_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     iterative
_audit_creation_date             2025-01-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-02-15 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                   19.7386(16)
_cell_length_b                   19.7386(16)
_cell_length_c                   11.0140(12)
_cell_measurement_reflns_used    3576
_cell_measurement_temperature    150(10)
_cell_measurement_theta_max      64.5430
_cell_measurement_theta_min      3.9930
_cell_volume                     3716.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.962
_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    -79.00 -18.00   0.50   45.44    --  -90.00  92.00-164.00  122
  2  \w   -109.00 -83.00   0.50   45.44    --  -90.00  85.00  95.00   52
  3  \w    122.00 178.00   0.50   45.44    --  108.07  58.00  92.00  112
  4  \w    -19.00  13.00   0.50   15.61    --  -50.36  19.00-150.00   64
  5  \w    -23.00  23.00   0.50   15.61    --  -50.36  19.00 150.00   92
  6  \w   -119.00 -94.00   0.50   15.61    --  -50.36-125.00-150.00   50
  7  \w   -107.00 -73.00   0.50   15.61    --  -50.36-125.00 -90.00   68
  8  \w   -113.00 -78.00   0.50   15.61    --  -50.36-125.00   0.00   70
  9  \w    -85.00 -22.00   0.50   45.44    --  -90.00 125.00-180.00  126
 10  \w    -50.00 -19.00   0.50   45.44    --  -90.00  85.00  95.00   62
 11  \w   -132.00 -92.00   0.50   45.44    --  -90.00 -19.00 150.00   80
 12  \w    101.00 173.00   0.50   45.44    --  108.07  38.00 120.00  144
 13  \w     36.00  61.00   0.50   45.44    --  108.07 -57.00-120.00   50
 14  \w     39.00  65.00   0.50   45.44    --  108.07 -57.00 150.00   52
 15  \w     36.00  65.00   0.50   45.44    --  108.07 -57.00  60.00   58
 16  \w     36.00  61.00   0.50   45.44    --  108.07 -57.00-150.00   50
 17  \w     36.00  65.00   0.50   45.44    --  108.07 -57.00   0.00   58
;
_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      0.0446295000
_diffrn_orient_matrix_UB_12      0.0626541000
_diffrn_orient_matrix_UB_13      0.0976739000
_diffrn_orient_matrix_UB_21      0.0001914000
_diffrn_orient_matrix_UB_22      0.0627851000
_diffrn_orient_matrix_UB_23      -0.0833251000
_diffrn_orient_matrix_UB_31      -0.0783116000
_diffrn_orient_matrix_UB_32      -0.0160392000
_diffrn_orient_matrix_UB_33      0.0553691000
_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  0.0820
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17225
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         81.383
_diffrn_reflns_theta_min         4.014
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    0.705
_exptl_crystal_description       block
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2874
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.0926
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2589
_refine_ls_wR_factor_ref         0.2943
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     0.867
_reflns_number_gt                1695
_reflns_number_total             2874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05093f2.cif
_cod_data_source_block           WYU-106
_cod_depositor_comments
'Adding full bibliography for 1575776--1575784.cif.'
_cod_original_cell_volume        3716.3(7)
_cod_database_code               1575783
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.83(2)
 0.17(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 N005-C8
 1.4 with sigma of 0.02
 C5-N7
 1.4 with sigma of 0.02
 C8-C6
 1.4 with sigma of 0.02
 C5-C6
 1.4 with sigma of 0.02
 O24-C33
 1.2 with sigma of 0.02
 C004-C006
 1.4 with sigma of 0.02
 C12-C10
 1.39 with sigma of 0.02
 C33-C12
 1.5 with sigma of 0.02
 C10_$4-C10_$2
 2.3 with sigma of 0.02
 C12-C10_$2
 2.8 with sigma of 0.02
 C12_$4-C12
 2.3 with sigma of 0.02
 C10_$4-C12_$5
 2.8 with sigma of 0.02
4. Restrained planarity
 C10_$4, C12_$4, C10_$2, C12_$5, C10, C12
 with sigma of 0.1
5. Rigid bond restraints
 O24, C33, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C008, C006, C00B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
C33 \\sim C12 \\sim C6 \\sim C5 \\sim C8 \\sim N005: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 2 within 3.8A
C33 \\sim C12: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 2
within 3.8A
C33 \\sim O24 \\sim C12: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 2 within 3.8A
O24 \\sim C33 \\sim C12: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 2 within 3.8A
C10 \\sim C12 \\sim C33 \\sim O24 \\sim N7: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
Uanis(N7) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C008) \\sim Ueq, Uanis(C00B) \\sim Ueq, Uanis(C006) \\sim Ueq,
Uanis(C004) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
7. Rigid body (RIGU) restrains
 C5, N7, C6, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C008, C00B, C006
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
8. Others
 Fixed Sof: C0(0.5) H0(0.5) C4B(0.5) H4B(0.5) C1(0.5) H1(0.5) C4A(0.5)
 H4A(0.5) C5(0.1665) C6(0.25) H6(0.25) C8(0.25) H8(0.25) O24(0.5)
9.a Riding coordinates:
 C0(H0), C4B(H4B), C1(H1), C4A(H4A)
9.b Ternary CH refined with riding coordinates:
 C004(H004)
9.c Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C6(H6), C8(H8)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44013
_shelx_fab_checksum              38362
_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 1.456
_oxdiff_exptl_absorpt_empirical_full_min 0.691