Transition of Metastable Cross-α Crystals into Cross-β Fibrils by β-Turn Flipping.
Mondal, Sudipta; Jacoby, Guy; Sawaya, Michael R.; Arnon, Zohar A.; Adler-Abramovich, Lihi; Rehak, Pavel; Vuković, Lela; Shimon, Linda J. W.; Král, Petr; Beck, Roy; Gazit, Ehud; Journal of the American Chemical Society 141 (2019) 363–369; doi:10.1021/jacs.8b10289

data_4133485
_publ_section_title
;
 Transition of Metastable Cross-\a Crystals into Cross-\b Fibrils by
 \b-Turn Flipping.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              363
_journal_page_last               369
_journal_paper_doi               10.1021/jacs.8b10289
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '4(C36 H51 N7 O10), 20(H2 O), 3(O)'
_chemical_formula_sum            'C144 H244 N28 O63'
_chemical_formula_weight         3375.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 109.252(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   8.9084(4)
_cell_length_b                   39.9686(19)
_cell_length_c                   13.1196(6)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      2.42
_cell_volume                     4410.1(4)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Apex2'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker KappaApexII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            72644
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.463
_diffrn_reflns_theta_min         2.038
_diffrn_source                   sealed-tube
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 5876 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         17527
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+1.1817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.933
_reflns_number_gt                14918
_reflns_number_total             17527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10289_si_001.cif
_cod_data_source_block           pep7nh3
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4133485
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.980
_shelx_res_checksum              95509
_shelx_hkl_checksum              71940