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_7158675
_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         '2(C14 H20 N2 O3), 5(H2 O)'
_chemical_formula_sum            'C28 H50 N4 O11'
_chemical_formula_weight         618.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-23
_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                 114.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.615(4)
_cell_length_b                   6.7520(14)
_cell_length_c                   13.402(3)
_cell_measurement_reflns_used    13945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.750
_cell_measurement_theta_min      2.162
_cell_volume                     1610.5(7)
_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 0.985
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device       'Huber 4-circles kappa geometry'
_diffrn_measurement_device_type  'single axis'
_diffrn_measurement_method       'rotating crystal'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0107
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13945
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         29.750
_diffrn_reflns_theta_min         2.162
_diffrn_source                   'Elettra XRD1 BL'
_diffrn_source_type              Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       needle
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 1896 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_coef       0.023(3)
_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   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         4372
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0489P)^2^+0.3528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0714
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    0.925
_reflns_Friedel_fraction_max     0.858
_reflns_number_gt                4354
_reflns_number_total             4372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob00622g2.cif
_cod_data_source_block           x4esxt-04aug043254_a
_cod_database_code               7158675
_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.a Ternary CH refined with riding coordinates:
 C3(H3), C1(H1), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C14(H14), C13(H13), C11(H11), C10(H10), C12(H12)
2.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              65011
_olex2_submission_special_instructions 'No special instructions were received'