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_1575645
_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            'C35.58 H51 Ag F4.72 N7.79 O11.65 S1.57'
_chemical_formula_weight         1022.30
_chemical_name_systematic
'metal--peptide double helical \b-sheet tape (Val, Val)'
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_Hall           'P 32'
_space_group_name_H-M_alt        'P 32'
_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                120
_cell_formula_units_Z            24
_cell_length_a                   25.794(4)
_cell_length_b                   25.794(4)
_cell_length_c                   50.545(10)
_cell_measurement_reflns_used    205889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.8480
_cell_measurement_theta_min      2.5910
_cell_volume                     29124(9)
_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 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            413996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.222
_diffrn_reflns_theta_min         2.623
_exptl_absorpt_coefficient_mu    4.656
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       needle
_exptl_crystal_F_000             12645
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water, methanol'
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         3.813
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Flack x determined using 35909 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0078(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4807
_refine_ls_number_reflns         80061
_refine_ls_number_restraints     10022
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0736
_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^)+(0.1800P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1946
_refine_ls_wR_factor_ref         0.1992
_reflns_Friedel_coverage         0.984
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                77327
_reflns_number_total             80061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05237h2.cif
_cod_data_source_block           p32_a-coot-82
_cod_depositor_comments
'Adding full bibliography for 1575639--1575646.cif.'
_cod_original_cell_volume        29124(10)
_cod_database_code               1575645
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.167
_shelx_estimated_absorpt_t_max   0.736
_shelx_res_checksum              42806