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_1575640
_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            'C35 H50 Ag F3 N7.5 O11.5 S'
_chemical_formula_weight         956.75
_chemical_name_systematic
'metal--peptide helical \b-sheet tape (Thr, Tle)'
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      tetragonal
_space_group_IT_number           95
_space_group_name_Hall           'P 4cw 2c'
_space_group_name_H-M_alt        'P 43 2 2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   22.89(3)
_cell_length_b                   22.89(3)
_cell_length_c                   51.99(5)
_cell_measurement_reflns_used    1032
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.6199
_cell_measurement_theta_min      0.5730
_cell_volume                     27240(6)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.2810
_diffrn_reflns_av_unetI/netI     0.1445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            44622
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        22.604
_diffrn_reflns_theta_max         22.604
_diffrn_reflns_theta_min         1.368
_diffrn_source                   'SPring-8 BL26B1'
_exptl_absorpt_coefficient_mu    0.948
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.933
_exptl_crystal_description       needle
_exptl_crystal_F_000             7912
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform, methanol, isobutyl acetate'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.200
_refine_ls_abs_structure_details
;
 Flack x determined using 643 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.298
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         6493
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.3066
_refine_ls_R_factor_gt           0.1939
_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^)+(0.2600P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4502
_refine_ls_wR_factor_ref         0.5295
_reflns_Friedel_coverage         0.726
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2605
_reflns_number_total             6493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05237h2.cif
_cod_data_source_block           p4322_s_a1-coot-17
_cod_depositor_comments
'Adding full bibliography for 1575639--1575646.cif.'
_cod_original_cell_volume        27240(76)
_cod_original_formula_sum        'C35 H50 Ag F3 N7.50 O11.50 S'
_cod_database_code               1575640
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              57065