A supramolecular hydrogel derived from a simple organic salt capable of proton conduction.
Chakraborty, Poulami; Das, Bikash; Pal, Pulak; Datta, Subhadeep; Bera, Sourabh; Dastidar, Parthasarathi; Chemical communications (Cambridge, England) 56 (2020) 5251–5254; doi:10.1039/d0cc01467b

data_7126287
_publ_section_title
;
 A supramolecular hydrogel derived from a simple organic salt capable of
 proton conduction.
;
_journal_issue                   39
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5251
_journal_page_last               5254
_journal_paper_doi               10.1039/d0cc01467b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C6 H5 O3 S, C7 H10 N, 0.5(H2 O)'
_chemical_formula_sum            'C13 H16 N O3.5 S'
_chemical_formula_weight         274.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-10-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-10-09 deposited with the CCDC.	2020-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.619(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.768(8)
_cell_length_b                   5.5762(12)
_cell_length_c                   15.750(3)
_cell_measurement_reflns_used    3604
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.29
_cell_measurement_theta_min      2.63
_cell_volume                     2644.0(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33600
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.485
_diffrn_reflns_theta_min         1.353
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1010 before and 0.0643 after correction. The Ratio of minimum to maximum transmission is 0.9211. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         2713
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0889P)^2^+1.1837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1532
_reflns_number_total             2713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01467b3.cif
_cod_data_source_block           BSBA
_cod_depositor_comments
'Adding full bibliography for 7126286--7126291.cif.'
_cod_original_formula_sum        'C13 H16 N O3.50 S'
_cod_database_code               7126287
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.916
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C8-C13A
 1.3 with sigma of 0.02
3. Others
 Fixed Sof: O1B(0.48215) O3A(0.51785) O2B(0.48215) C13A(0.48215) H13A(0.48215)
 C12A(0.48215) H12A(0.48215) C11A(0.48215) H11A(0.48215) C10A(0.48215)
 H10A(0.48215) C9A(0.48215) H9A(0.48215) C4B(0.48215) H4B(0.48215) C6B(0.48215)
 H6B(0.48215) C5B(0.48215) H5B(0.48215) C2B(0.48215) H2B(0.48215) C3B(0.48215)
 H3B(0.48215) C6A(0.51785) H6A(0.51785) C5A(0.51785) H5A(0.51785) C4A(0.51785)
 H4A(0.51785) C3A(0.51785) H3A(0.51785) C2A(0.51785) H2A(0.51785) H4C(0.5)
 H4D(0.5) C13B(0.51785) H13B(0.51785) C9B(0.51785) H9B(0.51785) C12B(0.51785)
 H12B(0.51785) C11B(0.51785) H11B(0.51785) C10B(0.51785) H10B(0.51785)
 O2A(0.51785) O1A(0.51785) O3B(0.48215)
4.a Free rotating group:
 O4(H4C,H4D)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
4.c Aromatic/amide H refined with riding coordinates:
 C13A(H13A), C12A(H12A), C11A(H11A), C10A(H10A), C9A(H9A), C4B(H4B), C6B(H6B),
 C5B(H5B), C2B(H2B), C3B(H3B), C6A(H6A), C5A(H5A), C4A(H4A), C3A(H3A), C2A(H2A),
  C13B(H13B), C9B(H9B), C12B(H12B), C11B(H11B), C10B(H10B)
4.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              52859
_olex2_submission_special_instructions 'No special instructions were received'