Hydrogen-bonded frameworks containing aliphatic 3D linkers show high-capacity water vapour sorption.
Muang-Non, Phonlakrit; Zhou, Carmen; Macreadie, Lauren K.; White, Nicholas G.; Chemical communications (Cambridge, England) 60 (2024) 746–749; doi:10.1039/d3cc05286a

data_7132522
_publ_section_title
;
 Hydrogen-bonded frameworks containing aliphatic 3D linkers show
 high-capacity water vapour sorption.
;
_journal_issue                   6
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              746
_journal_page_last               749
_journal_paper_doi               10.1039/d3cc05286a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C29 H32 N8, 2(C10 H6 O4)'
_chemical_formula_sum            'C49 H44 N8 O8'
_chemical_formula_weight         872.92
_space_group_crystal_system      tetragonal
_space_group_IT_number           118
_space_group_name_Hall           'P -4 -2n'
_space_group_name_H-M_alt        'P -4 n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     other
_audit_creation_date             2023-07-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-12-06 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.5856(15)
_cell_length_b                   23.5856(15)
_cell_length_c                   7.5250(4)
_cell_measurement_reflns_used    870
_cell_measurement_temperature    150
_cell_measurement_theta_max      56.9230
_cell_measurement_theta_min      5.3060
_cell_volume                     4186.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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   -103.00 -20.00   1.00   40.00    --  -36.03 -57.00  30.00   83
  2  \w     78.00 134.00   1.00  155.00    --   85.03 178.00 150.00   56
  3  \w    115.00 148.00   1.00  155.00    --   85.03 111.00 150.00   33
  4  \w     54.00 149.00   1.00  155.00    --   85.03  15.00   0.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            5646
_diffrn_reflns_point_group_measured_fraction_full 0.820
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        60.805
_diffrn_reflns_theta_max         60.805
_diffrn_reflns_theta_min         4.191
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.693
_exptl_crystal_description       needle
_exptl_crystal_F_000             916
_exptl_crystal_recrystallization_method
'Crystallized using tetra-amidinium.4Cl with TBA2.cubanedicarboxylate in 80% EtOH in water. Final concentration of tetra-amidinium = 0.50 mM.'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 498 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.5(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2614
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0770
_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^)+(0.1513P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2132
_refine_ls_wR_factor_ref         0.2342
_reflns_Friedel_coverage         0.478
_reflns_Friedel_fraction_full    0.607
_reflns_Friedel_fraction_max     0.607
_reflns_number_gt                1888
_reflns_number_total             2614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05286a2.cif
_cod_data_source_block           1CUB2
_cod_depositor_comments
'Adding full bibliography for 7132521--7132525.cif.'
_cod_original_cell_volume        4186.0(6)
_cod_database_code               7132522
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.874
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 C2-N1
 1.31 with sigma of 0.005
 C2-N2
 1.31 with sigma of 0.005
 C14_$1-C14
 1.55 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C13, C12, C14, C11, C10, O2, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C12(H12), C13(H13), C14(H14)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C7(H7), C8(H8)
4.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              65455
_shelx_hkl_checksum              15056
_shelx_fab_checksum              98330
_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
;