Self-Templated, Enantioselective Assembly of an Amyloid-like Dipeptide into Multifunctional Hierarchical Helical Arrays
Wang, Yuefei; Li, Qing; Zhang, Jiaxing; Qi, Wei; You, Shengping; Su, Rongxin; He, Zhimin; ACS Nano  (2021) –; doi:10.1021/acsnano.1c00746

data_4518755
_publ_section_title
;
 Self-Templated, Enantioselective Assembly of an Amyloid-like Dipeptide
 into Multifunctional Hierarchical Helical Arrays
;
_journal_name_full               'ACS Nano'
_journal_paper_doi               10.1021/acsnano.1c00746
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety
'2(C29 H27 Fe N2 O4), 3(C3 H2 F6 O), 2(H2 O), C5 H14 N2'
_chemical_formula_sum            'C72 H78 F18 Fe2 N6 O13'
_chemical_formula_weight         1689.10
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
????
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.318(4)
_cell_length_b                   17.786(4)
_cell_length_c                   24.349(5)
_cell_measurement_reflns_used    18592
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9103
_cell_measurement_theta_min      1.4178
_cell_volume                     7500(3)
_computing_cell_refinement       crystalclear
_computing_data_collection       crystalclear
_computing_data_reduction        crystalclear
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'rigaku saturn70 ccd'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            76095
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.890
_diffrn_reflns_theta_min         1.443
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             3480
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 4640 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(7)
_refine_ls_extinction_coef       0.0029(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1011
_refine_ls_number_reflns         17898
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0902P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1707
_reflns_Friedel_coverage         0.841
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                14591
_reflns_number_total             17898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nn1c00746_si_003.cif
_cod_data_source_block           shelxl
_cod_database_code               4518755
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.925
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Free rotating group:
 O12(H12A,H12B), O13(H13C,H13D)
3.b Ternary CH refined with riding coordinates:
 C12(H12), C21(H21), C41(H41), C50(H50), C65(H65), C68(H68), C71(H71), C60(H60)
3.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C23(H23A,H23B), C42(H42A,H42B), C52(H52A,H52B), N5(H5A,H5B),
 N6(H6A,H6B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B)
3.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C1(H1A), C2(H2A), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7),
 C8(H8), C9(H9), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C25(H25),
 C26(H26), C27(H27), C28(H28), C29(H29), N3(H3A), N4(H4A), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C44(H44),
  C45(H45), C46(H46), C47(H47), C48(H48), C54(H54), C55(H55), C56(H56),
 C57(H57), C58(H58)
3.e Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C)
3.f Idealised tetrahedral OH refined as rotating group:
 O9(H9A), O10(H10), O11(H11)
;
_shelx_res_checksum              28234
_shelx_hkl_checksum              27591
_olex2_submission_special_instructions 'No special instructions were received'