Self-assembled single-crystalline hydrogen-bonded frameworks: a potential metal-free molecule towards proton conductivity and electrochemical detection of organic and inorganic pollutants
Maheswari, Ganesan; Elancheziyan, Mari; Harathi, Jonnagaddala; Raji, Atchudan; Ashamary, Francis; Mahaan, Ramalingam; Kalambate, Pramod K.; Lee, Hon Man; Rosenkranz, Andreas; Manoj, Devaraj; New Journal of Chemistry 49 (2025) 4205–4217; doi:10.1039/D4NJ05382F

data_7063648
_publ_section_title
;
 Self-assembled single-crystalline hydrogen-bonded frameworks: a potential
 metal-free molecule towards proton conductivity and electrochemical
 detection of organic and inorganic pollutants
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4205
_journal_page_last               4217
_journal_paper_doi               10.1039/D4NJ05382F
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         '2(C10 H4 O8), 2(C11 H11 N5), 3(H2 O)'
_chemical_formula_sum            'C42 H36 N10 O19'
_chemical_formula_weight         984.81
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2025-01-07T10:27:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2025-01-20 deposited with the CCDC.	2025-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.79460(10)
_cell_length_b                   23.1642(4)
_cell_length_c                   22.7365(4)
_cell_measurement_reflns_used    12572
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.871
_cell_measurement_theta_min      1.966
_cell_volume                     1991.73(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0828295
_diffrn_orient_matrix_UB_12      0.0187758
_diffrn_orient_matrix_UB_13      -0.0623906
_diffrn_orient_matrix_UB_21      -0.2153252
_diffrn_orient_matrix_UB_22      0.0556917
_diffrn_orient_matrix_UB_23      0.0063918
_diffrn_orient_matrix_UB_31      0.335821
_diffrn_orient_matrix_UB_32      0.0311036
_diffrn_orient_matrix_UB_33      0.0262458
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22566
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.585
_diffrn_reflns_theta_min         2.728
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.76275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.42.96a (Rigaku Oxford Diffraction, 2023)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       needle
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.26
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         3953
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.8586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0
_reflns_number_gt                3473
_reflns_number_total             3953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj05382f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7063648.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7063648
_shelx_estimated_absorpt_t_min   0.822
_shelx_estimated_absorpt_t_max   0.945
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              81694
_shelx_hkl_checksum              46825