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_7132524
_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      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_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                 96.002(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6434(3)
_cell_length_b                   16.4405(5)
_cell_length_c                   26.1717(8)
_cell_measurement_reflns_used    7889
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      74.6510
_cell_measurement_theta_min      3.1850
_cell_volume                     4982.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_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 0.979
_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    -83.00 -11.00   0.50   20.00    --  -46.45 115.00-160.00  144
  2  \w    -80.00 -45.00   0.50   20.00    --  -46.45-171.00 -32.00   70
  3  \w     30.00  77.00   0.50   20.00    --   46.45-115.00 109.00   94
  4  \w     70.00 108.00   0.50   80.00    --  107.75 171.00 -18.00   76
  5  \w     69.00 103.00   0.50   80.00    --  107.75-115.00 109.00   68
  6  \w    115.00 151.00   0.50   80.00    --  107.75 115.00-160.00   72
  7  \w     98.00 123.00   0.50   80.00    --  107.75-171.00 -32.00   50
  8  \w      0.00  29.00   0.50   20.00    --  -46.45  19.00  90.00   58
  9  \w    -19.00  26.00   0.50   20.00    --  -46.45  38.00 -30.00   90
 10  \w     -7.00  27.00   0.50   20.00    --  -46.45  19.00-150.00   68
 11  \w     -8.00  30.00   0.50   20.00    --  -46.45  19.00 120.00   76
 12  \w     -2.00  24.00   0.50   20.00    --  -46.45  19.00-180.00   52
 13  \w     96.00 174.00   0.50   80.00    --  107.75  30.00  30.00  156
 14  \w     32.00  58.00   0.50   80.00    --  107.75 -30.00  60.00   52
 15  \w     37.00  66.00   0.50   80.00    --  107.75 -45.00 -90.00   58
 16  \w     32.00  58.00   0.50   80.00    --  107.75 -30.00-150.00   52
 17  \w     63.00  94.00   0.50   80.00    --  107.75 -95.00 -60.00   62
 18  \w     45.00 103.00   0.50   80.00    --  107.75 -95.00 120.00  116
 19  \w     33.00  59.00   0.50   80.00    --  107.75 -30.00  30.00   52
 20  \w     86.00 112.00   0.50   80.00    --  107.75 -77.00 -30.00   52
 21  \w     41.00  68.00   0.50   80.00    --  107.75 -45.00 120.00   54
 22  \w     38.00  63.00   0.50   80.00    --  107.75 -77.00  90.00   50
 23  \w     33.00  58.00   0.50   80.00    --  107.75 -30.00   0.00   50
 24  \w     33.00  59.00   0.50   80.00    --  107.75 -30.00 -90.00   52
 25  \w     84.00 121.00   0.50   80.00    --  107.75 -77.00  90.00   74
 26  \w     38.00  64.00   0.50   80.00    --  107.75 -45.00-120.00   52
 27  \w     44.00  90.00   0.50   80.00    --  107.75 -95.00 -90.00   92
 28  \w     34.00  64.00   0.50   80.00    --  107.75 -95.00 150.00   60
 29  \w     81.00 106.00   0.50   80.00    --  107.75 -95.00 150.00   50
 30  \w     34.00  59.00   0.50   80.00    --  107.75 -30.00  90.00   50
 31  \w     45.00 112.00   0.50   80.00    --  107.75-125.00-120.00  134
 32  \w     34.00  59.00   0.50   80.00    --  107.75 -30.00 -30.00   50
 33  \w     42.00  73.00   0.50   80.00    --  107.75 -77.00 -30.00   62
 34  \w     37.00  64.00   0.50   80.00    --  107.75 -45.00 -60.00   54
 35  \w     33.00  59.00   0.50   80.00    --  107.75 -30.00-120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0204001000
_diffrn_orient_matrix_UB_12      -0.0831898000
_diffrn_orient_matrix_UB_13      0.0264944000
_diffrn_orient_matrix_UB_21      -0.0096390000
_diffrn_orient_matrix_UB_22      0.0401523000
_diffrn_orient_matrix_UB_23      0.0525645000
_diffrn_orient_matrix_UB_31      -0.1311066000
_diffrn_orient_matrix_UB_32      -0.0159302000
_diffrn_orient_matrix_UB_33      -0.0059813000
_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  0.0378
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20473
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.253
_diffrn_reflns_theta_min         3.179
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_recrystallization_method
'Crystallized using tetra-amidinium.4Cl with TBA2.cubanedicarboxylate in 90% EtOH in water. Final concentration of tetra-amidinium = 1 mM'
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5243
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0856
_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^)+(0.1529P)^2^+6.4509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2519
_refine_ls_wR_factor_ref         0.2652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4180
_reflns_number_total             5243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05286a2.cif
_cod_data_source_block           Delta_1CUB2
_cod_depositor_comments
'Adding full bibliography for 7132521--7132525.cif.'
_cod_database_code               7132524
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H50N50O50
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.872
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 C10-C11A
 1.4 with sigma of 0.01
 C5-C4
 1.4 with sigma of 0.005
 C3-C8
 1.4 with sigma of 0.005
 C11A-C12A
 1.4 with sigma of 0.01
 C14A-C15A
 1.4 with sigma of 0.01
 C12A-C13
 1.4 with sigma of 0.01
 C7-C6
 1.4 with sigma of 0.005
 C13-C14
 1.4 with sigma of 0.01
 C13-C14A
 1.4 with sigma of 0.01
 C14-C15
 1.4 with sigma of 0.01
 C15A-C10
 1.4 with sigma of 0.01
 C15-C10
 1.4 with sigma of 0.01
 C8-C7
 1.4 with sigma of 0.005
 C10-C11
 1.4 with sigma of 0.01
 C6-C5
 1.4 with sigma of 0.005
 C11-C12
 1.4 with sigma of 0.01
 C4-C3
 1.4 with sigma of 0.005
 C12-C13
 1.4 with sigma of 0.01
3. Others
 Fixed Sof: C12A(0.5) H12A(0.5) C11A(0.5) H11A(0.5) C15(0.5) H15(0.5) C14(0.5)
 H14(0.5) C14A(0.5) H14A(0.5) C15A(0.5) H15A(0.5) C11(0.5) H11(0.5) C12(0.5)
 H12(0.5)
4.a Ternary CH refined with riding coordinates:
 C32(H32), C34(H34), C33(H33), C24(H24), C22(H22), C23(H23)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C5(H5), C4(H4), C12A(H12A), C11A(H11A), C15(H15), C14(H14),
 C14A(H14A), C15A(H15A), C11(H11), C12(H12)
4.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), N4(H4A,H4B), N3(H3A,H3B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36879
_shelx_hkl_checksum              5712
_shelx_fab_checksum              22661
_ins_header
;
TITL PMN-C-1-CUB-Block-90EtOH_auto_repro in I2/a 
REM I2/a (#15 in standard setting)
CELL 1.54184  11.643430  16.440511  26.171720  90.0000  96.0022  90.0000
ZERR    2.00   0.000253   0.000460   0.000809   0.0000   0.0023   0.0000
LATT  2
SYMM -x+1/2, y,-z 
SFAC C H N O
UNIT 100.00 100.00 100.00 100.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.09 0.11 0.21
TREF
HKLF 4
END
;
_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 1.489
_oxdiff_exptl_absorpt_empirical_full_min 0.633