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_1575784
_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 H41 B3 Fe3 N3 O16'
_chemical_formula_sum            'C71 H41 B3 Fe3 N3 O16'
_chemical_formula_weight         1392.05
_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   mixed
_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                   19.3746(5)
_cell_length_b                   19.3746(5)
_cell_length_c                   11.6627(3)
_cell_measurement_reflns_used    6544
_cell_measurement_temperature    293(3)
_cell_measurement_theta_max      76.4160
_cell_measurement_theta_min      3.7810
_cell_volume                     3791.36(17)
_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(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.941
_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   -109.00 -55.00   0.50    1.91    --  -50.55-152.00 121.00  108
  2  \w    -79.00 -18.00   0.50    7.64    --  -90.00  89.00 -71.00  122
  3  \w    112.00 138.00   0.50    7.64    --  108.07  57.00-178.00   52
  4  \w    145.00 172.00   0.50    7.64    --  108.07  57.00-178.00   54
  5  \w   -106.00 -73.00   0.50    1.91    --  -50.55-125.00 -60.00   66
  6  \w    -26.00  20.00   0.50    1.91    --  -50.55  19.00 150.00   92
  7  \w    -18.00  15.00   0.50    1.91    --   50.55 -19.00-150.00   66
  8  \w    -85.00 -21.00   0.50    7.64    --  -90.00 125.00 -90.00  128
  9  \w    -61.00 -18.00   0.50    7.64    --  -90.00  57.00  90.00   86
 10  \w     40.00  66.00   0.50    7.64    --  108.07 -57.00-180.00   52
 11  \w    107.00 171.00   0.50    7.64    --  108.07  38.00-120.00  128
 12  \w     47.00 109.00   0.50    7.64    --  108.07-125.00 150.00  124
 13  \w     36.00  65.00   0.50    7.64    --  108.07 -57.00 150.00   58
 14  \w     41.00  66.00   0.50    7.64    --  108.07 -57.00-120.00   50
 15  \w     98.00 123.00   0.50    7.64    --  108.07 122.00   4.00   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      -0.0494262000
_diffrn_orient_matrix_UB_12      0.0241779000
_diffrn_orient_matrix_UB_13      0.0762410000
_diffrn_orient_matrix_UB_21      -0.0049721000
_diffrn_orient_matrix_UB_22      -0.0587600000
_diffrn_orient_matrix_UB_23      0.0930624000
_diffrn_orient_matrix_UB_31      0.0771446000
_diffrn_orient_matrix_UB_32      0.0662474000
_diffrn_orient_matrix_UB_33      0.0547470000
_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  0.0601
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12115
_diffrn_reflns_point_group_measured_fraction_full 0.887
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.439
_diffrn_reflns_theta_min         3.790
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.530
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83857
_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    0.610
_exptl_crystal_description       block
_exptl_crystal_F_000             709
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.274(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2591
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0835
_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^)+(0.1818P)^2^+1.2253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2474
_refine_ls_wR_factor_ref         0.2654
_reflns_Friedel_coverage         0.679
_reflns_Friedel_fraction_full    0.769
_reflns_Friedel_fraction_max     0.707
_reflns_number_gt                2216
_reflns_number_total             2591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05093f2.cif
_cod_data_source_block           WYU-102
_cod_depositor_comments
'Adding full bibliography for 1575776--1575784.cif.'
_cod_original_cell_volume        3791.4(2)
_cod_database_code               1575784
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.632
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.726(19)
 0.274(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 C4-N007
 1.4 with sigma of 0.02
 B8-C3
 1.4 with sigma of 0.02
 N007-C4
 1.4 with sigma of 0.02
 C3-C4
 2.5 with sigma of 0.02
 C2-C3
 1.4 with sigma of 0.02
 C2-C4
 1.4 with sigma of 0.02
 C2-N007
 2.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.001 and sigma
for terminal atoms of 3.8 within 2A
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C1(0.5) H1(0.5) C0(0.5) H0(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5)
 C4(0.25) H4(0.25) C2(0.25) H2(0.25) O3(0.25) H3(0.25)
6.a Riding coordinates:
 O3(H3)
6.b Ternary CH refined with riding coordinates:
 C003(H003)
6.c Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C1(H1), C0(H0), C5(H5), C6(H6), C4(H4), C2(H2)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90483
_shelx_fab_checksum              80823
_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 1.959
_oxdiff_exptl_absorpt_empirical_full_min 0.719