Designing anti-bacterial supramolecular gels from primary ammonium dicarboxylate (PAD) salts for self-delivery applications.
Roy, Nabanita; Ghosh, Subhajit; Dutta, Abhishek; Dastidar, Parthasarathi; Faraday discussions 260 (2025) 283–309; doi:10.1039/d4fd00154k

data_1573601
_publ_section_title
;
 Designing anti-bacterial supramolecular gels from primary ammonium
 dicarboxylate (PAD) salts for self-delivery applications.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              283
_journal_page_last               309
_journal_paper_doi               10.1039/d4fd00154k
_journal_volume                  260
_journal_year                    2025
_chemical_formula_moiety         '1.5(C6 H8 O4), 3(C8 H12 N O)'
_chemical_formula_sum            'C33 H48 N3 O9'
_chemical_formula_weight         630.74
_chemical_name_systematic        ADIPIC-2TYRAMINE
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-07-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-09-23 deposited with the CCDC.	2025-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                88.897(2)
_cell_angle_beta                 70.005(2)
_cell_angle_gamma                65.733(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4038(8)
_cell_length_b                   12.7819(7)
_cell_length_c                   13.6007(8)
_cell_measurement_reflns_used    4565
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.29
_cell_volume                     1681.25(18)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      145.01
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_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  0.0501
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16204
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.469
_diffrn_reflns_theta_min         2.294
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1156 before and 0.0573 after correction.
The Ratio of minimum to maximum transmission is 0.8162.
The \l/2 correction factor is Not present.
;
_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    1.246
_exptl_crystal_description       needle
_exptl_crystal_F_000             678
_exptl_crystal_preparation       'Methanol- diethylether mixture'
_exptl_crystal_recrystallization_method 'slow evaporation'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         6172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0332P)^2^+0.5083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4327
_reflns_number_total             6172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4fd00154k2.cif
_cod_data_source_block           mo_pd050722_0m_a
_cod_depositor_comments
'Adding full bibliography for 1573600--1573608.cif.'
_cod_database_code               1573601
_shelx_shelxl_version_number     2018/3
_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) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C14(H14A,H14B), C33(H33A,H33B), C32(H32A,H32B), C16(H16A,
 H16B), C13(H13A,H13B), C10(H10A,H10B), C11(H11A,H11B), C2(H2A,H2B), C1(H1D,
 H1E), C25(H25A,H25B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C31(H31), C27(H27), C30(H30), C5(H5), C4(H4), C7(H7), C8(H8),
 C22(H22), C23(H23), C19(H19), C20(H20)
2.c Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N1(H1A,H1B,H1C), N2(H2C,H2D,H2E)
2.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O1(H1), O4(H4A)
;
_shelx_res_checksum              45604
_shelx_hkl_checksum              58499
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_original_sample_id ADP-2TYRAMINE
_olex2_submission_special_instructions 'No special instructions were received'