Dipeptide self-assembly into water-channels and gel biomaterial
Bellotto, Ottavia; Pierri, Giovanni; Rozhin, Petr; Polentarutti, Maurizio; Kralj, Slavko; D'Andrea, Paola; Tedesco, Consiglia; Marchesan, Silvia; Organic & Biomolecular Chemistry  (2022) –; doi:10.1039/D2OB00622G

data_7158676
_publ_section_title
;
 Dipeptide self-assembly into water-channels and gel biomaterial
;
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_paper_doi               10.1039/D2OB00622G
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety         '4(C14 H20 N2 O3), 4(H2O)'
_chemical_formula_sum            'C56 H88 N8 O16'
_chemical_formula_weight         1129.34
_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_space_group_name_H-M_alt        'I 4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-25 deposited with the CCDC.	2022-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.947(3)
_cell_length_b                   22.947(3)
_cell_length_c                   5.6120(11)
_cell_measurement_reflns_used    13478
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.743
_cell_measurement_theta_min      1.236
_cell_volume                     2955.1(8)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_type            'Pilatus 2M detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Huber 4-circles kappa geometry'
_diffrn_measurement_device_type  'single axis'
_diffrn_measurement_method       'rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            13478
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         29.743
_diffrn_reflns_theta_min         1.236
_diffrn_source_type              Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       needle
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 974 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.9(10)
_refine_ls_extinction_coef       0.013(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   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         4314
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0899P)^2^+2.4128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1921
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                2954
_reflns_number_total             4314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob00622g2.cif
_cod_data_source_block           x4esxt-03aug213322_a
_cod_original_cell_volume        2955.1(10)
_cod_database_code               7158676
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O3W(0.25) O2W(0.25) O1W(0.25) O4W(0.25)
 Fixed Uiso: O1W(0.10247)
3.a Free rotating group:
 O1(O3,O2,N2,N1,C2,C4,C6,C3,C11,C1,C5,C10,C12,C7,C9,C8,C13,C14)
3.b Ternary CH refined with riding coordinates:
 C3(H3), C1(H1), C12(H12)
3.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
3.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C11(H11), C10(H10), C7(H7), C9(H9), C8(H8)
3.e Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              41963
_olex2_submission_special_instructions 'No special instructions were received'