Bioadhesive supramolecular hydrogel from unprotected, short d,l-peptides with Phe-Phe and Leu-Asp-Val motifs.
Cringoli, Maria Cristina; Romano, Chiara; Parisi, Evelina; Waddington, Lynne J.; Melchionna, Michele; Semeraro, Sabrina; De Zorzi, Rita; Grönholm, Mikaela; Marchesan, Silvia; Chemical communications (Cambridge, England) 56 (2020) 3015–3018; doi:10.1039/c9cc09947f

data_7125884
_publ_section_title
;
 Bioadhesive supramolecular hydrogel from unprotected, short d,l-peptides
 with Phe-Phe and Leu-Asp-Val motifs.
;
_journal_issue                   20
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3015
_journal_page_last               3018
_journal_paper_doi               10.1039/c9cc09947f
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_compound_source        Synthesis
_chemical_formula_moiety
'2(C32 H45 N5 O8), C2 H F3 O2, 4(C H4 O), 2 (H2 O)'
_chemical_formula_sum            'C70 H111 F3 N10 O24'
_chemical_formula_weight         1533.68
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2019-05-17T19:45:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-05-17 deposited with the CCDC.	2020-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.35(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5290(19)
_cell_length_b                   23.743(5)
_cell_length_c                   18.276(4)
_cell_measurement_reflns_used    20107
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.253
_cell_measurement_theta_min      1.104
_cell_measurement_wavelength     0.7
_cell_volume                     4109.5(15)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Pilatus 2M detector'
_diffrn_detector_type            'Pilatus 2M detector'
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device       'Single axis'
_diffrn_measurement_device_type  'Huber 4-circles Kappa Goniometer'
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20107
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         28.253
_diffrn_reflns_theta_min         1.104
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_source_type              Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1640
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 5705 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.5(4)
_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   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         20107
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0939
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1694P)^2^+3.0821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.256
_refine_ls_wR_factor_ref         0.2819
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    0.96
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                15159
_reflns_number_total             20107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09947f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7125884.cif.'
_cod_original_cell_volume        4109.5(14)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C70  H111  N10  O24  F3'
_cod_database_code               7125884
_shelx_res_checksum              93206