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_1575779
_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         'C89 H48 Fe3 N3 O13'
_chemical_formula_sum            'C89 H48 Fe3 N3 O13'
_chemical_formula_weight         1534.85
_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   difmap
_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                   19.7696(7)
_cell_length_b                   19.7696(7)
_cell_length_c                   11.1567(4)
_cell_measurement_reflns_used    6689
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.1490
_cell_measurement_theta_min      3.9630
_cell_volume                     3776.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.132a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.132a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.132a (Rigaku OD, 2024)'
_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      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 0.968
_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  22.00   0.50    6.92    --  -49.06   9.00-168.00   92
  2  \w    -66.00 -30.00   0.50   30.67    --  -90.00 132.00  37.00   72
  3  \w   -160.00 -87.00   0.50   30.67    --  -90.00  -9.00  16.00  146
  4  \w     50.00 110.00   0.50   30.67    --  108.63-127.00-174.00  120
  5  \w    -15.00  12.00   0.50    6.92    --  -49.06  19.00 -90.00   54
  6  \w     94.00 121.00   0.50    6.92    --   49.06-178.00 -90.00   54
  7  \w    -22.00  41.00   0.50    6.92    --   49.06 -38.00   0.00  126
  8  \w   -159.00-110.00   0.50   30.67    --  -90.00 -38.00 120.00   98
  9  \w     39.00  66.00   0.50   30.67    --  108.63 -57.00 -90.00   54
 10  \w     49.00  88.00   0.50   30.67    --  108.63-144.00  16.00   78
 11  \w     39.00  83.00   0.50   30.67    --  108.63 -99.00-120.00   88
 12  \w     94.00 124.00   0.50   30.67    --  108.63-144.00  16.00   60
 13  \w     38.00  66.00   0.50   30.67    --  108.63 -57.00-150.00   56
 14  \w     44.00 104.00   0.50   30.67    --  108.63 -99.00-180.00  120
;
_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      0.0898886000
_diffrn_orient_matrix_UB_12      0.0410432000
_diffrn_orient_matrix_UB_13      0.0040719000
_diffrn_orient_matrix_UB_21      0.0047566000
_diffrn_orient_matrix_UB_22      0.0797435000
_diffrn_orient_matrix_UB_23      -0.0157641000
_diffrn_orient_matrix_UB_31      -0.0021296000
_diffrn_orient_matrix_UB_32      0.0078561000
_diffrn_orient_matrix_UB_33      0.1369413000
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            16520
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.173
_diffrn_reflns_theta_min         3.962
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.556
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.132a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    0.675
_exptl_crystal_description       block
_exptl_crystal_F_000             785
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.304(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2938
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0738
_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^)+(0.1728P)^2^+0.2219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2325
_refine_ls_wR_factor_ref         0.2428
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                2419
_reflns_number_total             2938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05093f2.cif
_cod_data_source_block           WYU-108
_cod_depositor_comments
'Adding full bibliography for 1575776--1575784.cif.'
_cod_original_cell_volume        3776.3(3)
_cod_database_code               1575779
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.784
_shelx_estimated_absorpt_t_min   0.629
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.696(16)
 0.304(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 C6-N006
 1.4 with sigma of 0.02
 C4-C6
 1.4 with sigma of 0.02
 C4-N006
 2.5 with sigma of 0.02
 C5-C4
 1.4 with sigma of 0.02
 C5-C6
 2.5 with sigma of 0.02
 C7-C16
 1.3 with sigma of 0.2
 C7-C32
 1.3 with sigma of 0.2
 C16-C7
 1.4 with sigma of 0.02
 C32_$1-C32
 1.39 with sigma of 0.02
 C32-C32_$2
 1.39 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C6 \\sim N006: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C4 \\sim C6 \\sim N006: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C5 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C5 \\sim C4 \\sim C6: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
C5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C5 \\sim C4 \\sim C6 \\sim N006: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C16: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C32 \\sim C7 \\sim C16 \\sim C5 \\sim C4 \\sim C6: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C32 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C32) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 C32, C32, C32, C32, C32, C32
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.0004
6. Others
 Fixed Sof: H002(0.08333) C0(0.5) H0(0.5) C1(0.5) H1(0.5) C2(0.5) H2(0.5)
 C3(0.5) H3(0.5) C7(0.25) H7(0.25)
7.a Riding coordinates:
 O002(H002), C003(H003), C009(H009), C0(H0), C1(H1), C2(H2), C3(H3), C6(H6),
 C4(H4), C7(H7)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              86150
_shelx_fab_checksum              98215
_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 1.896
_oxdiff_exptl_absorpt_empirical_full_min 0.614