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_1575776
_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         'C71 H44 Fe3 N6 O13'
_chemical_formula_sum            'C71 H44 Fe3 N6 O13'
_chemical_formula_weight         1356.67
_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                   19.4243(8)
_cell_length_b                   19.4243(8)
_cell_length_c                   11.5952(6)
_cell_measurement_reflns_used    1854
_cell_measurement_temperature    293.1(2)
_cell_measurement_theta_max      54.2730
_cell_measurement_theta_min      4.5570
_cell_volume                     3788.8(3)
_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      293.1(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 0.973
_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   -140.00 -76.00   0.50   29.11    --  -56.42-123.00 -96.00  128
  2  \w     77.00 128.00   0.50   29.11    --   56.42 154.00-125.00  102
  3  \w   -106.00 -38.00   0.50   29.11    -- -106.00 154.00-125.00  136
  4  \w    -75.00 -44.00   0.50   29.11    -- -106.00 121.00  75.00   62
  5  \w    -78.00 -40.00   0.50   29.11    -- -106.00 123.00 -15.00   76
  6  \w     35.00  62.00   0.50   29.11    --  112.84 -57.00 -30.00   54
  7  \w     21.00  56.00   0.50    7.28    --    0.00 -99.00  60.00   70
  8  \w    -56.00 -27.00   0.50    7.28    --    0.00 123.00 -15.00   58
  9  \w    -25.00  21.00   0.50   29.11    --  -56.42  19.00-150.00   92
 10  \w    -25.00   2.00   0.50   29.11    --  -56.42  19.00 -60.00   54
 11  \w    -24.00   5.00   0.50   29.11    --  -56.42  19.00-180.00   58
 12  \w     -1.00  24.00   0.50   29.11    --  -56.42  19.00 -90.00   50
 13  \w    -63.00 -26.00   0.50   29.11    -- -106.00  64.00  90.00   74
 14  \w   -104.00 -24.00   0.50   29.11    -- -106.00  77.00 -90.00  160
 15  \w    -65.00 -39.00   0.50   29.11    -- -106.00 178.00-150.00   52
 16  \w    -76.00 -30.00   0.50   29.11    -- -106.00  64.00 -90.00   92
 17  \w    -49.00 -23.00   0.50   29.11    -- -106.00  50.00-150.00   52
 18  \w     22.00 104.00   0.50   29.11    --  112.84 -92.00 150.00  164
 19  \w     29.00  54.00   0.50   29.11    --  112.84 -50.00  30.00   50
 20  \w     42.00  67.00   0.50   29.11    --  112.84 -64.00 120.00   50
;
_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      0.0750878000
_diffrn_orient_matrix_UB_12      0.0481725000
_diffrn_orient_matrix_UB_13      -0.0740070000
_diffrn_orient_matrix_UB_21      0.0483067000
_diffrn_orient_matrix_UB_22      0.0402168000
_diffrn_orient_matrix_UB_23      0.1095515000
_diffrn_orient_matrix_UB_31      0.0204271000
_diffrn_orient_matrix_UB_32      -0.0667471000
_diffrn_orient_matrix_UB_33      0.0126153000
_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  0.1238
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10626
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.195
_diffrn_reflns_theta_min         4.553
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25032
_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    0.595
_exptl_crystal_description       block
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2589
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1554
_refine_ls_R_factor_gt           0.0946
_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^)+(0.1992P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2693
_refine_ls_wR_factor_ref         0.3330
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_full    0.871
_reflns_Friedel_fraction_max     0.824
_reflns_number_gt                1278
_reflns_number_total             2589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05093f2.cif
_cod_data_source_block           WYU-100
_cod_depositor_comments
'Adding full bibliography for 1575776--1575784.cif.'
_cod_original_cell_volume        3788.8(4)
_cod_database_code               1575776
_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: 0.77(3)
 0.23(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
3. Restrained distances
 C00A-C007
 1.4 with sigma of 0.02
 C004-C00A
 1.4 with sigma of 0.02
 C1-N003
 1.4 with sigma of 0.02
 C3-N003
 2.5 with sigma of 0.02
 C3-C1
 1.4 with sigma of 0.02
 C2-C3
 1.4 with sigma of 0.02
 C2-C1
 2.5 with sigma of 0.02
 O005-C00B
 1.4 with sigma of 0.02
 C4B-H4B
 0.9 with sigma of 0.02
4. Rigid bond restraints
 N15, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C3 \\sim N003: within 2A with sigma of 0.01 and sigma for terminal atoms of 3.8
within 2A
C2 \\sim C1 \\sim C3: within 2A with sigma of 0.01 and sigma for terminal atoms
of 3.8 within 2A
C2: within 2A with sigma of 0.01 and sigma for terminal atoms of 3.8 within 2A
N15 \\sim C2: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C006) \\sim Ueq, Uanis(C004) \\sim Ueq, Uanis(C007) \\sim Ueq,
Uanis(C00A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
6. Others
 Fixed Sof: C1(0.25) H1(0.25) C3(0.25) H3(0.25) H15a(0.25) H15b(0.25) C4B(0.5)
 H4B(0.5) C8B(0.5) H8B(0.5) C8A(0.5) H8A(0.5) C4A(0.5) H4A(0.5)
7.a Ternary CH refined with riding coordinates:
 C006(H006), C4B(H4B), C8B(H8B)
7.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C1(H1), C3(H3), C8A(H8A), C4A(H4A)
7.c X=CH2 refined with riding coordinates:
 N15(H15a,H15b)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              43773
_shelx_fab_checksum              18158
_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 2.870
_oxdiff_exptl_absorpt_empirical_full_min 0.516