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_1575642
_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            'C36.35 H53 Ag F4.05 N7.67 O11.7 S1.35'
_chemical_formula_weight         1012.70
_chemical_name_systematic
'metal--peptide double helical \b-sheet tape (Val, Tle)'
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      hexagonal
_space_group_IT_number           178
_space_group_name_Hall           'P 61 2 (0 0 5)'
_space_group_name_H-M_alt        'P 61 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                120
_cell_formula_units_Z            48
_cell_length_a                   32.10(2)
_cell_length_b                   32.10(2)
_cell_length_c                   90.47(7)
_cell_measurement_reflns_used    12386
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.2602
_cell_measurement_theta_min      0.4011
_cell_volume                     80732(9)
_computing_structure_refinement  'SHELXL-2018/3 (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  'EIGER16M (DECTRIS)'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.1116
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            64437
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        16.258
_diffrn_reflns_theta_max         16.258
_diffrn_reflns_theta_min         0.721
_diffrn_source                   'SPring-8 BL41XU'
_exptl_absorpt_coefficient_mu    0.376
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_description       plate
_exptl_crystal_F_000             25124
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform, methanol, methoxycyclopentane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details
;
 Flack x determined using 2040 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.272
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         14431
_refine_ls_number_restraints     985
_refine_ls_restrained_S_all      1.259
_refine_ls_R_factor_all          0.2392
_refine_ls_R_factor_gt           0.1848
_refine_ls_shift/su_max          0.002
_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          0.4253
_refine_ls_wR_factor_ref         0.4788
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7505
_reflns_number_total             14431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05237h2.cif
_cod_data_source_block           p6122_a-coot-18
_cod_depositor_comments
'Adding full bibliography for 1575639--1575646.cif.'
_cod_original_cell_volume        80711(127)
_cod_original_sg_symbol_Hall     'P 61 2 (0 0 -1)'
_cod_original_formula_sum        'C36.35 H53 Ag F4.05 N7.67 O11.70 S1.35'
_cod_database_code               1575642
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              25901