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_7132525
_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         '4(C5 H3 O2), 8(H2 O), C29 H32 N8'
_chemical_formula_sum            'C49 H60 N8 O16'
_chemical_formula_weight         1017.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_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                62.706(2)
_cell_angle_beta                 89.940(2)
_cell_angle_gamma                63.745(2)
_cell_formula_units_Z            2
_cell_length_a                   13.6429(3)
_cell_length_b                   15.3717(3)
_cell_length_c                   16.0809(3)
_cell_measurement_reflns_used    30035
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.6930
_cell_measurement_theta_min      4.2360
_cell_volume                     2600.16(13)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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     17.00  49.00   1.00    4.56    --   36.95  67.00 111.68   32
  2  \w     20.00  59.00   1.00    4.56    --   36.95  57.00  90.00   39
  3  \w      4.00  29.00   1.00    4.56    --   36.95  89.00 -83.48   25
  4  \w     63.00  92.00   1.00    4.56    --   36.95  67.00 111.68   29
  5  \w     77.00 103.00   1.00    4.56    --   36.95  57.00-150.00   26
  6  \w     78.00 104.00   1.00    4.56    --   36.95  38.00   0.00   26
  7  \w     23.00  49.00   1.00    4.56    --   36.95  38.00-150.00   26
  8  \w      8.00  73.00   1.00    4.56    --   36.95 -99.00   0.00   65
  9  \w     51.00  98.00   1.00    4.56    --   36.95  68.00-121.92   47
 10  \w     73.00 100.00   1.00    4.56    --   36.95  32.00 -12.00   27
 11  \w     64.00 103.00   1.00    4.56    --   36.95  71.00   7.90   39
 12  \w     59.00  86.00   1.00    4.56    --   36.95  19.00 -60.00   27
 13  \w      7.00  32.00   1.00    4.56    --   36.95  83.00  53.11   25
 14  \w    -34.00  59.00   1.00    4.56    --   36.95 -19.00  60.00   93
 15  \w      5.00  30.00   1.00    4.56    --   36.95  87.00  -6.75   25
 16  \w     65.00 102.00   1.00    4.56    --   36.95  38.00-150.00   37
 17  \w    -27.00  56.00   1.00    4.56    --   36.95 -38.00 150.00   83
 18  \w     19.00  61.00   1.00    4.56    --   36.95  38.00   0.00   42
 19  \w     11.00  64.00   1.00    4.56    --   36.95 -77.00-120.00   53
 20  \w     76.00 102.00   1.00    4.56    --   36.95  57.00  90.00   26
 21  \w     22.00  63.00   1.00    4.56    --   36.95  57.00-150.00   41
 22  \w     22.00  49.00   1.00    4.56    --   36.95  57.00 -30.00   27
 23  \w      4.00  29.00   1.00    4.56    --   36.95  89.00-131.39   25
 24  \w    -26.00  50.00   1.00    4.56    --   36.95 -57.00  30.00   76
 25  \w     70.00 102.00   1.00    4.56    --   36.95  38.00-180.00   32
 26  \w     16.00  62.00   1.00    4.56    --   36.95  71.00   7.90   46
 27  \w     16.00  42.00   1.00    4.56    --   36.95  68.00-121.92   26
 28  \w    -31.00  -6.00   1.00    4.56    --   36.95   0.00-150.00   25
 29  \w     37.00  88.00   1.00    4.56    --   36.95-125.00-180.00   51
 30  \w      4.00  29.00   1.00    4.56    --   36.95  89.00 140.72   25
 31  \w      4.00  30.00   1.00    4.56    --   36.95  89.00-164.73   26
 32  \w     30.00  56.00   1.00    4.56    --   36.95  38.00-180.00   26
 33  \w     16.00  43.00   1.00    4.56    --   36.95  32.00 -12.00   27
 34  \w     15.00  42.00   1.00    4.56    --   36.95  19.00 -60.00   27
 35  \w     -3.00 104.00   1.00    4.56    --   36.95   0.00-150.00  107
 36  \w     40.00  95.00   1.00    4.56    --   36.95  38.00  90.00   55
 37  \w     91.00 117.00   1.00   18.25    --  111.00  64.00 -60.00   26
 38  \w     94.00 120.00   1.00   18.25    --  111.00  50.00  60.00   26
 39  \w     94.00 130.00   1.00   18.25    --  111.00  50.00 150.00   36
 40  \w    153.00 178.00   1.00   18.25    --  111.00  64.00 120.00   25
 41  \w     91.00 118.00   1.00   18.25    --  111.00  64.00 120.00   27
 42  \w     43.00 106.00   1.00   18.25    --  111.00 -92.00  30.00   63
 43  \w     41.00  81.00   1.00   18.25    --  111.00 -20.00 148.65   40
 44  \w     94.00 120.00   1.00   18.25    --  111.00  50.00   0.00   26
 45  \w    143.00 169.00   1.00   18.25    --  111.00  64.00-180.00   26
 46  \w     87.00 152.00   1.00   18.25    --  111.00  25.00 120.00   65
 47  \w     57.00 109.00   1.00   18.25    --  111.00-111.00-150.00   52
 48  \w    123.00 177.00   1.00   18.25    --  111.00  64.00   0.00   54
 49  \w     91.00 117.00   1.00   18.25    --  111.00  64.00-180.00   26
 50  \w     91.00 117.00   1.00   18.25    --  111.00  64.00   0.00   26
 51  \w     91.00 117.00   1.00   18.25    --  111.00  64.00  60.00   26
 52  \w    132.00 178.00   1.00   18.25    --  111.00  64.00  60.00   46
 53  \w     91.00 117.00   1.00   18.25    --  111.00  64.00-120.00   26
 54  \w    132.00 171.00   1.00   18.25    --  111.00  64.00-120.00   39
 55  \w     93.00 134.00   1.00   18.25    --  111.00  38.00   0.00   41
 56  \w     94.00 120.00   1.00   18.25    --  111.00  50.00 120.00   26
 57  \w    131.00 176.00   1.00   18.25    --  111.00  50.00 120.00   45
 58  \w     94.00 125.00   1.00   18.25    --  111.00  50.00-150.00   31
 59  \w     94.00 120.00   1.00   18.25    --  111.00  50.00 -60.00   26
 60  \w    130.00 156.00   1.00   18.25    --  111.00  50.00 -60.00   26
 61  \w    122.00 148.00   1.00   18.25    --  111.00  25.00 -60.00   26
 62  \w     95.00 122.00   1.00   18.25    --  111.00  50.00-180.00   27
 63  \w    133.00 169.00   1.00   18.25    --  111.00  64.00  30.00   36
 64  \w     88.00 131.00   1.00   18.25    --  111.00 -64.00-150.00   43
 65  \w     41.00 127.00   1.00   18.25    --  111.00 -15.00  59.01   86
 66  \w     91.00 117.00   1.00   18.25    --  111.00  64.00  30.00   26
 67  \w     77.00 108.00   1.00   18.25    --  111.00-111.00-120.00   31
 68  \w     94.00 120.00   1.00   18.25    --  111.00  50.00-120.00   26
 69  \w     91.00 139.00   1.00   18.25    --  111.00  64.00 150.00   48
 70  \w    143.00 169.00   1.00   18.25    --  111.00  38.00-120.00   26
 71  \w    125.00 178.00   1.00   18.25    --  111.00  64.00  90.00   53
 72  \w     49.00  75.00   1.00   18.25    --  111.00 -64.00-150.00   26
 73  \w     91.00 117.00   1.00   18.25    --  111.00  64.00  90.00   26
 74  \w     86.00 156.00   1.00   18.25    --  111.00  25.00 -30.00   70
 75  \w    133.00 174.00   1.00   18.25    --  111.00  64.00 -90.00   41
 76  \w     91.00 117.00   1.00   18.25    --  111.00  64.00 -90.00   26
 77  \w     93.00 118.00   1.00   18.25    --  111.00  38.00 120.00   25
 78  \w     67.00 109.00   1.00   18.25    --  111.00-111.00 -30.00   42
 79  \w     46.00  71.00   1.00   18.25    --  111.00 -92.00-150.00   25
 80  \w    102.00 137.00   1.00   18.25    --  111.00 178.00  90.00   35
 81  \w     94.00 120.00   1.00   18.25    --  111.00  50.00  30.00   26
 82  \w     92.00 135.00   1.00   18.25    --  111.00  38.00-150.00   43
 83  \w    144.00 169.00   1.00   18.25    --  111.00  50.00 -30.00   25
 84  \w     94.00 121.00   1.00   18.25    --  111.00  50.00 -30.00   27
 85  \w     68.00 129.00   1.00   18.25    --  111.00 -38.00  60.00   61
 86  \w     92.00 126.00   1.00   18.25    --  111.00  38.00-120.00   34
 87  \w    131.00 157.00   1.00   18.25    --  111.00  38.00  60.00   26
 88  \w     92.00 121.00   1.00   18.25    --  111.00  38.00  60.00   29
 89  \w    126.00 152.00   1.00   18.25    --  111.00  64.00 -30.00   26
 90  \w     43.00  73.00   1.00   18.25    --  111.00-111.00-120.00   30
 91  \w     50.00  95.00   1.00   18.25    --  111.00 -50.00-150.00   45
 92  \w     87.00 120.00   1.00   18.25    --  111.00  25.00 -90.00   33
 93  \w    143.00 176.00   1.00   18.25    --  111.00  38.00 150.00   33
 94  \w     93.00 118.00   1.00   18.25    --  111.00  38.00-180.00   25
 95  \w     94.00 131.00   1.00   18.25    --  111.00  38.00 150.00   37
 96  \w    140.00 176.00   1.00   18.25    --  111.00  64.00-150.00   36
 97  \w     86.00 112.00   1.00   18.25    --  111.00  25.00 150.00   26
 98  \w    131.00 157.00   1.00   18.25    --  111.00  25.00 150.00   26
 99  \w     41.00  90.00   1.00   18.25    --  111.00 -25.00 -30.00   49
100  \w    104.00 134.00   1.00   18.25    --  111.00 -25.00 -30.00   30
101  \w     92.00 130.00   1.00   18.25    --  111.00  38.00 -90.00   38
102  \w     92.00 117.00   1.00   18.25    --  111.00  64.00 -30.00   25
103  \w     66.00  96.00   1.00   18.25    --  111.00 178.00  90.00   30
104  \w     89.00 124.00   1.00   18.25    --  111.00  25.00  90.00   35
105  \w     86.00 115.00   1.00   18.25    --  111.00  25.00  30.00   29
106  \w     75.00 105.00   1.00   18.25    --  111.00 -92.00-120.00   30
107  \w     93.00 118.00   1.00   18.25    --  111.00  38.00  30.00   25
108  \w     91.00 117.00   1.00   18.25    --  111.00  64.00-150.00   26
109  \w     94.00 140.00   1.00   18.25    --  111.00  50.00  90.00   46
110  \w     81.00 109.00   1.00   18.25    --  111.00-111.00 150.00   28
111  \w     86.00 121.00   1.00   18.25    --  111.00  25.00  60.00   35
112  \w     60.00 109.00   1.00   18.25    --  111.00-111.00 120.00   49
113  \w     45.00  79.00   1.00   18.25    --  111.00 -38.00 -30.00   34
114  \w     89.00 125.00   1.00   18.25    --  111.00 -38.00 -30.00   36
115  \w     74.00 118.00   1.00   18.25    --  111.00 -64.00 -30.00   44
116  \w     43.00  78.00   1.00   18.25    --  111.00-111.00 150.00   35
117  \w     94.00 145.00   1.00   18.25    --  111.00  50.00 -90.00   51
118  \w     86.00 164.00   1.00   18.25    --  111.00  25.00   0.00   78
119  \w     82.00 109.00   1.00   18.25    --  111.00-111.00  30.00   27
120  \w     88.00 113.00   1.00   18.25    --  111.00  25.00-150.00   25
121  \w    126.00 166.00   1.00   18.25    --  111.00  25.00-150.00   40
122  \w     88.00 118.00   1.00   18.25    --  111.00  25.00 -60.00   30
123  \w    123.00 149.00   1.00   18.25    --  111.00  50.00-180.00   26
124  \w     61.00  97.00   1.00   18.25    --  111.00 -77.00 120.00   36
125  \w    111.00 138.00   1.00   18.25    --  111.00 -77.00 120.00   27
126  \w     43.00  94.00   1.00   18.25    --  111.00 -50.00 -60.00   51
127  \w    143.00 169.00   1.00   18.25    --  111.00  64.00 -60.00   26
128  \w    146.00 172.00   1.00   18.25    --  111.00  50.00 150.00   26
129  \w    100.00 131.00   1.00   18.25    --  111.00 -20.00 148.65   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0927888000
_diffrn_orient_matrix_UB_12      -0.1030494000
_diffrn_orient_matrix_UB_13      -0.0015069000
_diffrn_orient_matrix_UB_21      -0.0912090000
_diffrn_orient_matrix_UB_22      -0.0097964000
_diffrn_orient_matrix_UB_23      -0.0454278000
_diffrn_orient_matrix_UB_31      0.0032546000
_diffrn_orient_matrix_UB_32      0.0786212000
_diffrn_orient_matrix_UB_33      -0.1017442000
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59597
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.895
_diffrn_reflns_theta_min         3.730
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89009
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       prism
_exptl_crystal_F_000             1076
_exptl_crystal_recrystallization_method
'Crystallised using tetra-amidinium.4Cl with TBA2.cubanedicarboxylate in 50%EtOH in water. Final concentration of tetra-amidinium = 2 mM'
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         10469
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0602P)^2^+2.3789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9656
_reflns_number_total             10469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05286a2.cif
_cod_data_source_block           Beta_1CUB2
_cod_depositor_comments
'Adding full bibliography for 7132521--7132525.cif.'
_cod_original_cell_volume        2600.17(11)
_cod_database_code               7132525
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C39H54N8O12
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.807
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H17B-H16B
 2.38 with sigma of 0.02
 H17A-H17B
 1.4 with sigma of 0.01
 H10A-H10B
 1.4 with sigma of 0.01
 H10A-O10_$1
 2.12 with sigma of 0.02
 O140-H14B
 0.88 with sigma of 0.01
3.a Free rotating group:
 O130(H13A,H13B), O120(H12A,H12B), O160(H16A,H16B), O100(H10A,H10B), O150(H15A,
 H15B), O110(H11A,H11B), O140(H14A), O170(H17A,H17B)
3.b Ternary CH refined with riding coordinates:
 C64(H64), C62(H62), C54(H54), C52(H52), C53(H53), C11(H11), C43(H43),
 C42(H42), C44(H44), C47(H47), C45(H45), C46(H46)
3.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C27(H27), C23(H23), C3(H3), C31(H31), C22(H22), C12(H12), C7(H7),
 C15(H15), C28(H28), C9(H9), C30(H30), C4(H4), C20(H20), C14(H14), C6(H6)
3.d X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N5(H5A,H5B), N6(H6A,H6B), N8(H8A,H8B), N3(H3A,H3B), N4(H4A,H4B),
 N7(H7A,H7B), N2(H2A,H2B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97901
_shelx_hkl_checksum              26345
_shelx_fab_checksum              49831
_ins_header
;
TITL PMN-C-8-2mM_repro_1 in P1 
REM P1 (#1 in standard setting)
CELL 1.54184  13.642899  15.371658  16.080858  62.7056  89.9400  63.7451
ZERR    5.00   0.000272   0.000291   0.000277   0.0018   0.0015   0.0019
LATT -1
SFAC C H N O
UNIT 195.00 270.00 40.00 60.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.09 0.16 0.27
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 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.793