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_7132523
_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
_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                 102.35(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.879(5)
_cell_length_b                   12.595(4)
_cell_length_c                   27.719(12)
_cell_measurement_reflns_used    417
_cell_measurement_temperature    313.11(10)
_cell_measurement_theta_max      55.6260
_cell_measurement_theta_min      3.8620
_cell_volume                     4733(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      air
_diffrn_ambient_temperature      313.11(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 0.999
_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    -53.00  31.00   1.00   25.00    --  -36.03  57.00  60.00   84
  2  \w    -53.00  31.00   1.00   25.00    --  -36.03  57.00 -60.00   84
  3  \w    -53.00  31.00   1.00   25.00    --  -36.03  57.00-180.00   84
  4  \w     20.00 103.00   1.00  100.00    --   85.19 -61.00-120.00   83
  5  \w     21.00 105.00   1.00  100.00    --   85.19-111.00-120.00   84
  6  \w    115.00 150.00   1.00  100.00    --   85.19 111.00 120.00   35
  7  \w     71.00 146.00   1.00  100.00    --   85.19 178.00 120.00   75
  8  \w    103.00 153.00   1.00  100.00    --   85.19  77.00-120.00   50
  9  \w    103.00 149.00   1.00  100.00    --   85.19  77.00  30.00   46
 10  \w    105.00 155.00   1.00  100.00    --   85.19 111.00 -90.00   50
 11  \w    103.00 135.00   1.00  100.00    --   85.19  77.00-150.00   32
 12  \w     69.00 153.00   1.00  100.00    --   85.19  30.00 -30.00   84
 13  \w     17.00 106.00   1.00  100.00    --   85.19 -95.00  90.00   89
 14  \w     68.00 146.00   1.00  100.00    --   85.19  61.00-180.00   78
;
_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      -0.1029896000
_diffrn_orient_matrix_UB_12      -0.0510588000
_diffrn_orient_matrix_UB_13      -0.0139166000
_diffrn_orient_matrix_UB_21      0.0189435000
_diffrn_orient_matrix_UB_22      -0.0569838000
_diffrn_orient_matrix_UB_23      0.0503902000
_diffrn_orient_matrix_UB_31      -0.0440413000
_diffrn_orient_matrix_UB_32      0.0953623000
_diffrn_orient_matrix_UB_33      0.0225969000
_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  0.3680
_diffrn_reflns_av_unetI/netI     0.2645
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7023
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        44.487
_diffrn_reflns_theta_max         44.486
_diffrn_reflns_theta_min         3.871
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00677
_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    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         1867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1789
_refine_ls_R_factor_gt           0.1102
_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^)+(0.1038P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2598
_refine_ls_wR_factor_ref         0.3184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                691
_reflns_number_total             1867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05286a2.cif
_cod_data_source_block           Gamma_1CUB2
_cod_depositor_comments
'Adding full bibliography for 7132521--7132525.cif.'
_cod_database_code               7132523
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H50N50O50
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.845
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C24(H24), C32(H32), C23(H23), C33(H33), C34(H34), C22(H22)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C14(H14), C3(H3), C13(H13), C6(H6), C10(H10), C7(H7), C11(H11)
2.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N1(H1A,H1B), N2(H2A,H2B), N4(H4A,H4B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83539
_shelx_hkl_checksum              63308
_shelx_fab_checksum              99893
_ins_header
;
TITL PMN-C-8-2mM-40C-reprosmart-1 in I2/a 
REM I2/a (#15 in standard setting)
CELL 1.54184  13.878668  12.595229  27.718681  90.0000 102.3506  90.0000
ZERR    2.00   0.005292   0.003543   0.012192   0.0000   0.0433   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=313.1; max=313.1; aver:313.1
TEMP 40
SIZE 0.07 0.13 0.25
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 44.395
_oxdiff_exptl_absorpt_empirical_full_min 0.292