Probing assembly/disassembly of ordered molecular hydrogels.
Ramalhete, Susana M.; Nartowski, Karol P.; Green, Hayley; Angulo, Jesús; Iuga, Dinu; Fábián, László; Lloyd, Gareth O.; Khimyak, Yaroslav Z.; Faraday discussions 255 (2025) 495–519; doi:10.1039/d4fd00081a

data_1571705
_publ_section_title
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 Probing assembly/disassembly of ordered molecular hydrogels.
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_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              495
_journal_page_last               519
_journal_paper_doi               10.1039/d4fd00081a
_journal_volume                  255
_journal_year                    2025
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C9 H12 N2 O2, 1.5(H2 O)'
_chemical_formula_sum            'C9 H15 N2 O3.5'
_chemical_formula_weight         207.23
_chemical_name_systematic        4-aminophenylalanine
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2024-04-22 deposited with the CCDC.	2024-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.681(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9813(9)
_cell_length_b                   11.3702(15)
_cell_length_c                   14.985(2)
_cell_measurement_reflns_used    2454
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      3.26
_cell_volume                     1017.0(2)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2591
_diffrn_reflns_point_group_measured_fraction_full 0.507
_diffrn_reflns_point_group_measured_fraction_max 0.520
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.776
_diffrn_reflns_theta_min         1.362
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0849 before and 0.0664 after correction.
 The Ratio of minimum to maximum transmission is 0.78.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 17879 reflections, Rint = 0.1228
 (3378 with I > 3sig(I), Rint = 0.0726)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       needle
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   -1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         2591
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0573
_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^)+(0.1105P)^2^+0.2343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1654
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                2295
_reflns_number_total             2591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4fd00081a2.cif
_cod_data_source_block           5529
_cod_depositor_comments
;
         Adding full bibliography for 1571705.cif.

2025-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C18 H30 N4 O7'
_cod_original_formula_weight         414.46
_cod_original_formula_moiety         '2(C9 H12 N2 O2), 3(H2 O)'
_cod_original_formula_units_Z            2
_cod_database_code               1571705
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.470(9) 0.461(5) 0.069(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O1-Hb
 1.9 with sigma of 0.02
 O002-Ha
 1.9 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C00R) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.2
Uanis(C00E) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2
5.a Free rotating group:
 O005(H00y,H), O006(H00z,Ha), O009(H00,Hb)
5.b Rotating group:
 N007(H00a,H00b), N00D(H00n,H00o)
5.c Ternary CH refined with riding coordinates:
 C00I(H00r), C00P(H00P)
5.d Secondary CH2 refined with riding coordinates:
 C00N(H00f,H00h), C00Q(H00v,H00w)
5.e Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00H(H00q), C00K(H00K), C00L(H00L), C00M(H00s), C00O(H00u),
 C00S(H00x), C00T(H00T)
5.f Idealised Me refined as rotating group:
 N008(H00i,H00j,H00m), N00B(H00c,H00d,H00e)
;
_olex2_submission_special_instructions 'No special instructions were received'