Comparative study on proton conductivity of a polypyridinyl multicarboxylate-based hydrogen-bonded organic framework and related chitosan composite membrane
Kang, Lu-Lu; Zuo, Shuai-Wu; Han, Bing-Xue; Li, Gang; New Journal of Chemistry 47 (2023) 1299–1307; doi:10.1039/D2NJ04779A

data_7062119
_publ_section_title
;
 Comparative study on proton conductivity of a polypyridinyl
 multicarboxylate-based hydrogen-bonded organic framework and related
 chitosan composite membrane
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1299
_journal_page_last               1307
_journal_paper_doi               10.1039/D2NJ04779A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C24 H15 N3 O6, 4(H2 O)'
_chemical_formula_sum            'C24 H23 N3 O10'
_chemical_formula_weight         513.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-14 deposited with the CCDC.	2022-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.417(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9842(3)
_cell_length_b                   18.7164(7)
_cell_length_c                   15.8121(5)
_cell_measurement_reflns_used    2252
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.8960
_cell_measurement_theta_min      4.7000
_cell_volume                     2360.79(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   -104.00 -11.00   1.00    6.00    --  -33.50 -37.00 -30.00   93
  2  \w   -105.00 -79.00   1.00    6.00    --  -33.50 178.00  30.00   26
  3  \w     26.00  73.00   1.00    6.00    --   36.47 -99.00  90.00   47
  4  \w     16.00 106.00   1.00    6.00    --   36.47  77.00 -90.00   90
  5  \w     -2.00  33.00   1.00    6.00    --   36.47 -99.00 -30.00   35
  6  \w     57.00  83.00   1.00    6.00    --   36.47 178.00 120.00   26
  7  \w     12.00  86.00   1.00    6.00    --   36.47  77.00-150.00   74
  8  \w     93.00 125.00   1.00   12.00    --  108.00  61.00  30.00   32
  9  \w    110.00 157.00   1.00   12.00    --  108.00 111.00  60.00   47
 10  \w     39.00 112.00   1.00   12.00    --  108.00-111.00-120.00   73
 11  \w     60.00 122.00   1.00   12.00    --  108.00 -61.00 -90.00   62
 12  \w     49.00  98.00   1.00   12.00    --  108.00 -94.00  60.00   49
 13  \w    138.00 176.00   1.00   12.00    --  108.00  61.00  30.00   38
 14  \w    100.00 138.00   1.00   12.00    --  108.00 111.00   0.00   38
 15  \w     41.00 104.00   1.00   12.00    --  108.00 -94.00 -90.00   63
 16  \w     72.00 150.00   1.00   12.00    --  108.00  15.00 120.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0172683000
_diffrn_orient_matrix_UB_12      -0.0438163000
_diffrn_orient_matrix_UB_13      -0.0816612000
_diffrn_orient_matrix_UB_21      0.0359096000
_diffrn_orient_matrix_UB_22      0.0691774000
_diffrn_orient_matrix_UB_23      -0.0489432000
_diffrn_orient_matrix_UB_31      0.1889852000
_diffrn_orient_matrix_UB_32      -0.0091014000
_diffrn_orient_matrix_UB_33      0.0209911000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8515
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.056
_diffrn_reflns_theta_max         67.056
_diffrn_reflns_theta_min         3.661
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4219
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1036P)^2^+1.0507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.2002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3050
_reflns_number_total             4219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04779a2.cif
_cod_data_source_block           lg202007hbx7
_cod_depositor_comments          'Adding full bibliography for 7062119.cif.'
_cod_original_cell_volume        2360.78(16)
_cod_database_code               7062119
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C14H15N2O4Ce1
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.892
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O9-H9A
 0.9 with sigma of 0.02
 O9-H9B
 0.9 with sigma of 0.02
3.a Riding coordinates:
 O7(H7A,H7B), O10(H10A,H10B)
3.b Free rotating group:
 O8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24)
3.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              7201
_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 3.421
_oxdiff_exptl_absorpt_empirical_full_min 0.719