Structure-Property Relationship Study of <i>N</i>-(Hydroxy)Peptides for the Design of Self-Assembled Parallel β-Sheets.
Richaud, Alexis D.; Roche, Stéphane P; The Journal of organic chemistry 85 (2020) 12329–12342; doi:10.1021/acs.joc.0c01441

data_4038773
_publ_section_title
;
 Structure-Property Relationship Study of <i>N</i>-(Hydroxy)Peptides for
 the Design of Self-Assembled Parallel \b-Sheets.
;
_journal_issue                   19
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12329
_journal_page_last               12342
_journal_paper_doi               10.1021/acs.joc.0c01441
_journal_volume                  85
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C14 H25 N3 O7'
_chemical_formula_sum            'C14 H25 N3 O7'
_chemical_formula_weight         347.37
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90.242(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5051(18)
_cell_length_b                   8.8409(18)
_cell_length_c                   20.790(4)
_cell_measurement_reflns_used    2811
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      11.82
_cell_measurement_theta_min      2.17
_cell_volume                     1747.0(6)
_computing_cell_refinement       'APEX II v2014.11-0 (Bruker, 2014)'
_computing_data_collection       '15IDD, ChemMatCARS, 2019'
_computing_data_reduction        'APEX II v2014.11-0 (Bruker, 2014)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2016)'
_computing_publication_material  'SHELXTL (Bruker, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2016)'
_computing_structure_solution    'SHELX (Bruker, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Pilatus1M pixel array detector'
_diffrn_detector_area_resol_mean 5.8
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details      '0.5 degree frames measured for 1 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'huber three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'silicon  1 1 1 and 3 1 1'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1178
_diffrn_reflns_av_unetI/netI     0.1065
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39900
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         14.614
_diffrn_reflns_theta_min         1.139
_exptl_absorpt_coefficient_mu    0.041
_exptl_absorpt_correction_T_max  0.7438
_exptl_absorpt_correction_T_min  0.6130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick; 2018'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.004
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 1650 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -4.0(10)
_refine_ls_extinction_coef       0.23(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6458
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0986P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1873
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                4346
_reflns_number_total             6458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01441_si_002.cif
_cod_data_source_block           s19031
_cod_depositor_comments          'Adding full bibliography for 4038773.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4038773
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.999
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              44948
_shelx_hkl_checksum              71106