Acquiring preferred mode of aggregation through positional antagonism for saponification triggered gelation
Chand, Prem; Kumar, Ashish; New Journal of Chemistry 47 (2023) 6135–6143; doi:10.1039/D2NJ04858B

data_7062305
_publ_section_title
;
 Acquiring preferred mode of aggregation through positional antagonism for
 saponification triggered gelation
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6135
_journal_page_last               6143
_journal_paper_doi               10.1039/D2NJ04858B
_journal_volume                  47
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_compound_source        '5-aminoisophthalic acid and o-vanillin'
_chemical_formula_moiety         '2(C26 H25 N3 O6)'
_chemical_formula_sum            'C52 H50 N6 O12'
_chemical_formula_weight         951.010
_chemical_melting_point          351
_chemical_name_common            HLB
_chemical_name_systematic
diethyl-5-(2-hydroxy-3-methoxy-5-phenyldiazenyl)benzylidene-aminoisophthalate
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2023-02-17
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.02.15 svn.rb8c1d4dc for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2023-02-20 deposited with the CCDC.	2023-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                62.200(2)
_cell_angle_beta                 80.9796(15)
_cell_angle_gamma                87.5397(16)
_cell_formula_units_Z            2
_cell_length_a                   7.52118(14)
_cell_length_b                   19.1168(4)
_cell_length_c                   19.7439(4)
_cell_measurement_reflns_used    70435
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5700
_cell_measurement_theta_min      2.1630
_cell_volume                     2478.61(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9997
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.9997
_diffrn_reflns_Laue_measured_fraction_max 0.9997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            71966
_diffrn_reflns_point_group_measured_fraction_full 0.9997
_diffrn_reflns_point_group_measured_fraction_max 0.9997
_diffrn_reflns_theta_full        24.9999
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.88643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)'
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_meas      1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1000.714
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol, Dichloromethane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.7678
_refine_diff_density_min         -0.2667
_refine_diff_density_rms         0.0563
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             9.9726
_refine_ls_extinction_coef       0.0019
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0566
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    107
_refine_ls_number_parameters     796
_refine_ls_number_reflns         8723
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.0336
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1180P)^2^+0.4443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.2175
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              22
_reflns_limit_k_min              -20
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                5568
_reflns_number_total             8723
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj04858b2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7062305--7062306.cif.'
_cod_original_cell_volume        2478.6(1)
_cod_database_code               7062305
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5A-C16A \\sim O5B-C16B
 with sigma of 0.02
 O6A-C15A \\sim O6B-C15B
 with sigma of 0.02
 C13A-C14A \\sim C13A-C14B
 with sigma of 0.02
 C14A-C15A \\sim C14B-C15B
 with sigma of 0.02
 C14A-C19A \\sim C14B-C19B
 with sigma of 0.02
 C15A-C16A \\sim C15B-C16B
 with sigma of 0.02
 C16A-C17A \\sim C16B-C17B
 with sigma of 0.02
 C21A-C22A \\sim C21B-C22B
 with sigma of 0.02
 C22A-C23A \\sim C22B-C23B
 with sigma of 0.02
 C23A-C24A \\sim C23B-C24B
 with sigma of 0.02
 C24A-C25A \\sim C24B-C25B
 with sigma of 0.02
 O5A-C15A \\sim O5B-C15B
 with sigma of 0.04
 O5A-C17A \\sim O5B-C17B
 with sigma of 0.04
 O5A-C26A \\sim O5B-C26B
 with sigma of 0.04
 O6A-C14A \\sim O6B-C14B
 with sigma of 0.04
 O6A-C16A \\sim O6B-C16B
 with sigma of 0.04
 C13A-C15A \\sim C13A-C15B
 with sigma of 0.04
 C13A-C19A \\sim C13A-C19B
 with sigma of 0.04
 C14A-C16A \\sim C14B-C16B
 with sigma of 0.04
 C15A-C17A \\sim C15B-C17B
 with sigma of 0.04
 C15A-C19A \\sim C15B-C19B
 with sigma of 0.04
 C16A-C26A \\sim C16B-C26B
 with sigma of 0.04
 C17A-C19A \\sim C17B-C19B
 with sigma of 0.04
 C21A-C23A \\sim C21B-C23B
 with sigma of 0.04
 C21A-C25A \\sim C21B-C25B
 with sigma of 0.04
 C22A-C24A \\sim C22B-C24B
 with sigma of 0.04
 C23A-C25A \\sim C23B-C25B
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 O5A, C26A, C22A, O6A, C20A, N2A, C24A, N3A, C19A, C14A, C21A, C15A, C23A,
 C16A, C25A, C17A, C18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6B, N2B, N3B, C14B, C25B, C15B, C26B, C16B, C22B, C17B, C23B, C24B, C18B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O6B, C26B, C23B, N2B, C21B, N3B, C25B, C14B, C20B, C15B, C22B, C16B, C24B,
 C17B, O5B, C18B, C19B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H13b)=Sof(O6B)=Sof(H6B)=Sof(C14B)=Sof(C15B)=Sof(C16B)=Sof(C17B)=Sof(H17B)=
 Sof(C19B)=Sof(H19B)=Sof(C21B)=Sof(H21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=
 Sof(H23B)=Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(H25B)=Sof(O5B)=Sof(C26B)=Sof(H26d)=
 Sof(H26e)=Sof(H26f)=Sof(N2B)=Sof(N3B)=Sof(C18B)=Sof(C20B)=1-FVAR(1)
 Sof(O5A)=Sof(O6A)=Sof(H6A)=Sof(N2A)=Sof(N3A)=Sof(H13A)=Sof(C14A)=Sof(C15A)=
 Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=
 Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=
 Sof(H24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26a)=Sof(H26b)=Sof(H26c)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C11(H11c,H11d), C8A(H8Aa,H8Ab), C11A(H11a,H11b)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C13(H13), C17(H17), C19(H19), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C1A(H1A), C3A(H3A), C5A(H5A), C13A(H13A),
 C13A(H13b), C17A(H17A), C19A(H19A), C21A(H21A), C22A(H22A), C23A(H23A),
 C24A(H24A), C25A(H25A), C17B(H17B), C19B(H19B), C21B(H21B), C22B(H22B),
 C23B(H23B), C24B(H24B), C25B(H25B)
5.c Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C12(H12d,H12e,H12f), C20(H20a,H20b,H20c), C9A(H9Aa,H9Ab,
 H9Ac), C12A(H12a,H12b,H12c), C26A(H26a,H26b,H26c), C26B(H26d,H26e,H26f)
5.d Idealised tetrahedral OH refined as rotating group:
 O6(H6), O6A(H6A), O6B(H6B)
;
_olex2_submission_special_instructions 'No special instructions were received'