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_1575782
_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         'C84 H44 Fe3 N9 O13'
_chemical_formula_sum            'C84 H44 Fe3 N9 O13'
_chemical_formula_weight         1554.83
_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                   19.2448(10)
_cell_length_b                   19.2448(10)
_cell_length_c                   11.8172(11)
_cell_measurement_reflns_used    2726
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.3520
_cell_measurement_theta_min      3.7320
_cell_volume                     3790.3(4)
_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    '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 0.989
_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   -157.00 -91.00   0.50   45.05    --  -91.75 -52.00-120.00  132
  2  \w    -80.00 -22.00   0.50   45.05    --  -91.75 105.00-107.00  116
  3  \w    -62.00 -36.00   0.50   45.05    --  -91.75 121.00 151.00   52
  4  \w    -26.00  11.00   0.50   10.51    --  -47.33  19.00 -90.00   74
  5  \w    -12.00  28.00   0.50   10.51    --  -47.33  19.00 -60.00   80
  6  \w    -20.00   7.00   0.50   10.51    --   47.33 -19.00 -90.00   54
  7  \w     63.00 114.00   0.50   10.51    --   47.33 178.00  90.00  102
  8  \w     43.00 109.00   0.50   45.05    --  108.48-125.00  60.00  132
  9  \w     39.00  65.00   0.50   45.05    --  108.48 -57.00 150.00   52
 10  \w     44.00 105.00   0.50   45.05    --  108.48 -99.00  60.00  122
 11  \w     36.00  66.00   0.50   45.05    --  108.48 -57.00 -30.00   60
 12  \w     39.00 104.00   0.50   45.05    --  108.48 -99.00 150.00  130
 13  \w     37.00  62.00   0.50   45.05    --  108.48 -57.00 -90.00   50
 14  \w     43.00 103.00   0.50   45.05    --  108.48 -77.00 150.00  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      -0.0185956000
_diffrn_orient_matrix_UB_12      -0.0282420000
_diffrn_orient_matrix_UB_13      -0.1240191000
_diffrn_orient_matrix_UB_21      -0.0445390000
_diffrn_orient_matrix_UB_22      0.0472111000
_diffrn_orient_matrix_UB_23      -0.0149375000
_diffrn_orient_matrix_UB_31      0.0787934000
_diffrn_orient_matrix_UB_32      0.0742792000
_diffrn_orient_matrix_UB_33      -0.0376392000
_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  0.1007
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16209
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.064
_diffrn_reflns_theta_min         3.740
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.562
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51420
_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    0.681
_exptl_crystal_description       block
_exptl_crystal_F_000             793
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.182(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2899
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0721
_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^)+(0.1316P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2231
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.894
_reflns_number_gt                2208
_reflns_number_total             2899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05093f2.cif
_cod_data_source_block           WYU-107
_cod_depositor_comments
'Adding full bibliography for 1575776--1575784.cif.'
_cod_original_cell_volume        3790.3(5)
_cod_database_code               1575782
_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: 0.818(16)
 0.182(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C0) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00G) \\sim Ueq, Uanis(C00F) \\sim Ueq, Uanis(C00E) \\sim Ueq,
Uanis(C00I) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C00H) \\sim Ueq, Uanis(C00C)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C0(0.5) H0(0.5) C1(0.5) H1(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5)
5.a Ternary CH refined with riding coordinates:
 C005(H005)
5.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00F(H00F), C00G(H00G), C0(H0), C1(H1), C2(H2), C3(H3)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53931
_shelx_fab_checksum              78264
_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 2.084
_oxdiff_exptl_absorpt_empirical_full_min 0.557