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_1575780
_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         'C77 H41 Fe3 N3 O16'
_chemical_formula_sum            'C77 H41 Fe3 N3 O16'
_chemical_formula_weight         1431.68
_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   geom
_atom_sites_solution_primary     dual
_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                   19.4911(12)
_cell_length_b                   19.4911(12)
_cell_length_c                   11.4691(11)
_cell_measurement_reflns_used    2674
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      64.9600
_cell_measurement_theta_min      3.8300
_cell_volume                     3773.4(5)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(2)
_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 0.987
_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    -26.00  18.00   0.50   16.15    --  -56.42  42.00-116.00   88
  2  \w   -146.00 -81.00   0.50   16.15    --  -56.42 -79.00 -71.00  130
  3  \w   -105.00 -33.00   0.50   20.15    -- -106.00 160.00 -79.00  144
  4  \w     73.00 114.00   0.50   20.15    --  112.84  42.00-116.00   82
  5  \w    -63.00 -37.00   0.50    4.04    --    0.00 118.00 128.00   52
  6  \w      4.00  56.00   0.50    4.04    --    0.00 -99.00 150.00  104
  7  \w   -145.00 -96.00   0.50   16.15    --  -56.42 -99.00   0.00   98
  8  \w     -8.00  20.00   0.50   16.15    --  -56.42  19.00-180.00   56
  9  \w    -15.00  10.00   0.50   16.15    --  -56.42  19.00 -90.00   50
 10  \w    -52.00 -23.00   0.50   20.15    -- -106.00  50.00 -30.00   58
 11  \w   -164.00 -67.00   0.50   20.15    -- -106.00 -64.00  60.00  194
 12  \w    -96.00 -54.00   0.50   20.15    -- -106.00 178.00 -60.00   84
 13  \w     31.00  56.00   0.50   20.15    --  112.84 -50.00 150.00   50
 14  \w     32.00  57.00   0.50   20.15    --  112.84 -50.00  30.00   50
 15  \w     79.00 128.00   0.50   20.15    --  112.84 178.00 120.00   98
 16  \w    107.00 156.00   0.50   20.15    --  112.84 111.00   0.00   98
 17  \w     29.00  56.00   0.50   20.15    --  112.84 -50.00  90.00   54
 18  \w     30.00  56.00   0.50   20.15    --  112.84 -50.00 120.00   52
 19  \w    121.00 175.00   0.50   20.15    --  112.84  42.00-116.00  108
;
_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      0.0097694000
_diffrn_orient_matrix_UB_12      -0.0373099000
_diffrn_orient_matrix_UB_13      0.1127123000
_diffrn_orient_matrix_UB_21      -0.0828805000
_diffrn_orient_matrix_UB_22      -0.0726953000
_diffrn_orient_matrix_UB_23      -0.0182405000
_diffrn_orient_matrix_UB_31      0.0367703000
_diffrn_orient_matrix_UB_32      -0.0407232000
_diffrn_orient_matrix_UB_33      -0.0708708000
_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  0.0681
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11616
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.994
_diffrn_reflns_theta_min         3.854
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19990
_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    0.630
_exptl_crystal_description       block
_exptl_crystal_F_000             730
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.125(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2668
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0779
_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^)+(0.1599P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2085
_refine_ls_wR_factor_ref         0.2179
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.909
_reflns_Friedel_fraction_max     0.882
_reflns_number_gt                2140
_reflns_number_total             2668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05093f2.cif
_cod_data_source_block           WYU-101
_cod_depositor_comments
'Adding full bibliography for 1575776--1575784.cif.'
_cod_original_cell_volume        3773.4(6)
_cod_database_code               1575780
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.951
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.875(17)
 0.125(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C5-N003
 1.4 with sigma of 0.02
 C6-C5
 1.4 with sigma of 0.02
 C6-N003
 2.5 with sigma of 0.02
 C12-C5
 2.5 with sigma of 0.02
 C12-C6
 1.4 with sigma of 0.02
 C27-C12
 1.4 with sigma of 0.02
 O30-C27
 1.4 with sigma of 0.02
 C27-O30
 1.4 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N003: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
C6 \\sim C5 \\sim N003: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C12 \\sim C6 \\sim C5: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C27 \\sim C12: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O30 \\sim C27: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C5) \\sim Ueq, Uanis(N003) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N003) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N003
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C1(0.5) H1(0.5) C0(0.5) H0(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5)
 C5(0.25) H5(0.25) O30(0.25)
7.a Ternary CH refined with riding coordinates:
 C004(H004)
7.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C1(H1), C0(H0), C2(H2), C3(H3), C5(H5), C6(H6)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16354
_shelx_fab_checksum              95763
_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 3.788
_oxdiff_exptl_absorpt_empirical_full_min 0.487