Engineering β-sheet morphologies <i>via</i> metal cross-linking and side chain modifications.
Tsunekawa, Eisuke; Nakama, Takahiro; Fujita, Makoto; Sawada, Tomohisa; Chemical science 16 (2025) 18832–18837; doi:10.1039/d5sc05237h

data_1575641
_publ_section_title
;
 Engineering &#x3b2;-sheet morphologies <i>via</i> metal cross-linking and
 side chain modifications.
;
_journal_issue                   40
_journal_name_full               'Chemical science'
_journal_page_first              18832
_journal_page_last               18837
_journal_paper_doi               10.1039/d5sc05237h
_journal_volume                  16
_journal_year                    2025
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C34.75 H52.25 N7.25 O9'
_chemical_formula_weight         715.58
_chemical_name_systematic        'pentapeptide ligand (Val, Val)'
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-01-29 deposited with the CCDC.	2025-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                83.96(3)
_cell_angle_beta                 73.23(3)
_cell_angle_gamma                83.06(3)
_cell_formula_units_Z            4
_cell_length_a                   14.238(3)
_cell_length_b                   16.076(3)
_cell_length_c                   18.830(4)
_cell_measurement_reflns_used    6864
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.3347
_cell_measurement_theta_min      0.5730
_cell_volume                     4085.2(16)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'EIGER4M (DECTRIS)'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.000
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.887
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27974
_diffrn_reflns_point_group_measured_fraction_full 0.837
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        30.533
_diffrn_reflns_theta_max         30.533
_diffrn_reflns_theta_min         1.594
_diffrn_source                   'SPring-8 BL26B1'
_exptl_absorpt_coefficient_mu    0.216
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       plate
_exptl_crystal_F_000             1534
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMF, methanol'
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Flack x determined using 5946 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.09(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.337
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1797
_refine_ls_number_reflns         15039
_refine_ls_number_restraints     3524
_refine_ls_restrained_S_all      1.254
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.1307
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3378
_refine_ls_wR_factor_ref         0.3514
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.786
_reflns_Friedel_fraction_max     0.786
_reflns_number_gt                13793
_reflns_number_total             15039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05237h2.cif
_cod_data_source_block           p1_3-coot-12
_cod_depositor_comments
'Adding full bibliography for 1575639--1575646.cif.'
_cod_database_code               1575641
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.994
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              13401