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_1575646
_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            'C46.63 H71.33 Ag0.92 F4.9 N7.82 O11.43 S1.63'
_chemical_formula_weight         1168.76
_chemical_name_systematic
'metal--peptide helical \b-sheet tape (Val, Val) with C12'
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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            48
_cell_length_a                   24.635(7)
_cell_length_b                   44.065(12)
_cell_length_c                   103.30(2)
_cell_measurement_reflns_used    6289
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.6199
_cell_measurement_theta_min      0.5730
_cell_volume                     112136(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.4047
_diffrn_reflns_av_unetI/netI     0.2159
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       79
_diffrn_reflns_limit_l_min       -79
_diffrn_reflns_number            368763
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        22.559
_diffrn_reflns_theta_max         22.559
_diffrn_reflns_theta_min         0.855
_diffrn_source                   'SPring-8 BL26B1'
_exptl_absorpt_coefficient_mu    0.714
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.831
_exptl_crystal_description       rod
_exptl_crystal_F_000             29310
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform, methanol, ethyl acetate'
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details
;
 Flack x determined using 4791 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.089(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3588
_refine_ls_number_reflns         52904
_refine_ls_number_restraints     3246
_refine_ls_restrained_S_all      1.279
_refine_ls_R_factor_all          0.3468
_refine_ls_R_factor_gt           0.1885
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2100P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4201
_refine_ls_wR_factor_ref         0.5110
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                17982
_reflns_number_total             52904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05237h2.cif
_cod_data_source_block           p212121_m2-coot-35
_cod_depositor_comments
'Adding full bibliography for 1575639--1575646.cif.'
_cod_original_cell_volume        112134(50)
_cod_original_formula_sum        'C46.63 H71.33 Ag0.92 F4.90 N7.82 O11.43 S1.63'
_cod_database_code               1575646
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              38628