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_1575777
_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         'C71.359 H36.026 Fe3 N3.998 O15'
_chemical_formula_sum            'C71.36 H36.03 Fe3 N4 O15'
_chemical_formula_weight         1356.94
_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     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                   19.5213(6)
_cell_length_b                   19.5213(6)
_cell_length_c                   11.4015(6)
_cell_measurement_reflns_used    4872
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.5380
_cell_measurement_theta_min      3.8280
_cell_volume                     3762.8(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    '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 0.981
_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    -45.00  23.00   0.50   10.22    --  -48.55  43.00  -3.00  136
  2  \w   -106.00 -80.00   0.50   45.87    --  -91.75 -51.00 133.00   52
  3  \w    -48.00 -23.00   0.50   45.87    --  -91.75  43.00  -3.00   50
  4  \w   -157.00-124.00   0.50   45.87    --  -91.75 -51.00 133.00   66
  5  \w   -118.00 -80.00   0.50   10.22    --  -48.55-125.00  60.00   76
  6  \w   -116.00 -78.00   0.50   10.22    --  -48.55-125.00  90.00   76
  7  \w    -66.00 -19.00   0.50   45.87    --  -91.75  57.00  60.00   94
  8  \w    -66.00 -26.00   0.50   45.87    --  -91.75  57.00 150.00   80
  9  \w    -48.00 -22.00   0.50   45.87    --  -91.75  57.00-120.00   52
 10  \w     56.00 110.00   0.50   45.87    --  108.82-125.00-120.00  108
 11  \w    106.00 171.00   0.50   45.87    --  108.82 125.00-120.00  130
 12  \w     39.00  65.00   0.50   45.87    --  108.82 -57.00 -60.00   52
 13  \w     37.00  65.00   0.50   45.87    --  108.82 -57.00-180.00   56
 14  \w     40.00  66.00   0.50   45.87    --  108.82 -57.00-120.00   52
 15  \w     39.00  66.00   0.50   45.87    --  108.82 -57.00-150.00   54
 16  \w    103.00 173.00   0.50   45.87    --  108.82 127.00-158.00  140
;
_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      0.0508455000
_diffrn_orient_matrix_UB_12      -0.0365440000
_diffrn_orient_matrix_UB_13      -0.0365748000
_diffrn_orient_matrix_UB_21      0.0246560000
_diffrn_orient_matrix_UB_22      0.0500930000
_diffrn_orient_matrix_UB_23      -0.1128308000
_diffrn_orient_matrix_UB_31      0.0715100000
_diffrn_orient_matrix_UB_32      0.0666921000
_diffrn_orient_matrix_UB_33      0.0647772000
_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  0.0618
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16498
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.404
_diffrn_reflns_theta_min         3.877
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.543
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46657
_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    0.599
_exptl_crystal_description       block
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.104(15)
_refine_ls_extinction_coef       0.0014(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2889
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0734
_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^)+(0.1695P)^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         0.2275
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                2053
_reflns_number_total             2889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05093f2.cif
_cod_data_source_block           WYU-103
_cod_depositor_comments
'Adding full bibliography for 1575776--1575784.cif.'
_cod_database_code               1575777
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.630
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.896(16)
 0.104(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Shared sites
{N1, C4}
4. Restrained distances
 C10-C12
 1.4 with sigma of 0.02
 N005-C16
 1.4 with sigma of 0.02
 C16-C10
 1.4 with sigma of 0.02
 C4-C27
 1.4 with sigma of 0.02
 C5-C4
 2.8 with sigma of 0.02
 C6-C27
 1.4 with sigma of 0.02
 C5-C6
 1.4 with sigma of 0.02
 C6-C5
 1.4 with sigma of 0.02
 C5-C27
 2.5 with sigma of 0.02
 O11-C27
 1.2 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C16) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C27) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N005) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) = Uanis(C4)
6. 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
 C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
7. Others
 Fixed Sof: N005(0.16668) C0(0.5) H0(0.5) C1(0.5) H1(0.5) C10(0.16775)
 H10(0.16775) C12(0.08333) C16(0.16775) H16(0.16775) C2(0.5) H2(0.5) C3(0.5)
 H3(0.5) N1(0.1665) C4(0.08333) C5(0.02778) C6(0.08333) C27(0.16667)
 O11(0.16667)
8.a Ternary CH refined with riding coordinates:
 C004(H004)
8.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C0(H0), C1(H1), C10(H10), C16(H16), C2(H2), C3(H3)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30772
_shelx_fab_checksum              94713
_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 1.771
_oxdiff_exptl_absorpt_empirical_full_min 0.391