Supramolecular hydrogels from unprotected dipeptides: a comparative study on stereoisomers and structural isomers.
Bellotto, Ottavia; Kralj, Slavko; De Zorzi, Rita; Geremia, Silvano; Marchesan, Silvia; Soft matter 16 (2020) 10151–10157; doi:10.1039/d0sm01191f

data_1558981
_publ_section_title
;
 Supramolecular hydrogels from unprotected dipeptides: a comparative study
 on stereoisomers and structural isomers.
;
_journal_issue                   44
_journal_name_full               'Soft matter'
_journal_page_first              10151
_journal_page_last               10157
_journal_paper_doi               10.1039/d0sm01191f
_journal_volume                  16
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_compound_source        Synthesis
_chemical_formula_moiety         'C15  H22  N2  O3, 4.5 (H2 O1)'
_chemical_formula_sum            'C15 H31 N2 O7.5'
_chemical_formula_weight         359.42
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_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      2.4.5
_audit_creation_date             2020-06-26T19:29:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-06-29 deposited with the CCDC.	2020-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.900(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.870(4)
_cell_length_b                   5.7700(10)
_cell_length_c                   19.890(3)
_cell_measurement_reflns_used    2679
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.521
_cell_measurement_theta_min      1.048
_cell_measurement_wavelength     0.7
_cell_volume                     1862.0(6)
_computing_cell_refinement       'Mosflm (Battye, 2011)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'Mosflm (Battye, 2011)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Pilatus 2M detector'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Huber 4-circles kappa goniometer'
_diffrn_measurement_device_type  'Single axis'
_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  0.090
_diffrn_reflns_av_unetI/netI     0.078
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2679
_diffrn_reflns_point_group_measured_fraction_full 0.545
_diffrn_reflns_point_group_measured_fraction_max 0.542
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         28.521
_diffrn_reflns_theta_min         1.048
_diffrn_source                   'Elettra BL XRD1'
_diffrn_source_type              Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             780
_exptl_crystal_recrystallization_method
'Spontaneous crystallization from hydrogel of the compound'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   2.0(19)
_refine_ls_extinction_coef       0.072(8)
_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   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     258
_refine_ls_number_reflns         2679
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0772
_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^)+(0.1168P)^2^+5.5207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2235
_refine_ls_wR_factor_ref         0.2284
_reflns_Friedel_coverage         0
_reflns_Friedel_fraction_full    0
_reflns_Friedel_fraction_max     0
_reflns_number_gt                2583
_reflns_number_total             2679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sm01191f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 1558981.cif.'
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C15  H31  N2  O7.50'
_cod_database_code               1558981
_shelx_estimated_absorpt_t_min   0.987
_shelx_estimated_absorpt_t_max   1
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              32683
_shelx_hkl_checksum              14051