Crystallographic characterization of the 9/11-helix: a left-handed helix for 1 : 1 α/β-peptides containing L-α-amino acid residues.
Seo, Nuri; Kim, Yujin; Lee, Jieun; Kim, Jieun; Kang, Philjae; Guzei, Ilia A.; Lee, Ha-Jin; Choi, Soo Hyuk; Organic & biomolecular chemistry 23 (2025) 6133–6137; doi:10.1039/d5ob00621j

data_7160571
_publ_section_title
;
 Crystallographic characterization of the 9/11-helix: a left-handed helix
 for 1&#x2009;:&#x2009;1 &#x3b1;/&#x3b2;-peptides containing
 L-&#x3b1;-amino acid residues.
;
_journal_issue                   25
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6133
_journal_page_last               6137
_journal_paper_doi               10.1039/d5ob00621j
_journal_volume                  23
_journal_year                    2025
_chemical_formula_moiety         'C47 H79 N7 O10'
_chemical_formula_sum            'C47 H79 N7 O10'
_chemical_formula_weight         902.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1py5ph
_audit_creation_date             2016-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-09-29 deposited with the CCDC.	2025-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                99.67(3)
_cell_angle_beta                 93.03(3)
_cell_angle_gamma                106.32(3)
_cell_formula_units_Z            6
_cell_length_a                   18.468(4)
_cell_length_b                   19.384(4)
_cell_length_c                   23.636(5)
_cell_measurement_reflns_used    116481
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.915
_cell_measurement_theta_min      2.268
_cell_volume                     7960(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.63000
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.1145
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            92826
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        20.499
_diffrn_reflns_theta_max         20.499
_diffrn_reflns_theta_min         1.351
_diffrn_source                   'Fixed gap multiple wiggler beamline'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dull light colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2940
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.0038(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.817
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1763
_refine_ls_number_reflns         21364
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.817
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0989P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6329
_reflns_number_total             21364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ob00621j2.cif
_cod_data_source_block           nr_b21_yjc39
_cod_depositor_comments
'Adding full bibliography for 7160569--7160571.cif.'
_cod_database_code               7160571
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C138) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
3.a Ternary CH refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C15(H15), C20(H20), C21(H21), C23(H23), C30(H30),
 C35(H35), C38(H38), C40(H40), C45(H45), C50(H50), C53(H53), C55(H55),
 C133(H133), C136(H136), C138(H138), C143(H143), C148(H148), C151(H151),
 C153(H153), C158(H158), C163(H163), C166(H166), C168(H168), C173(H173),
 C178(H178), C181(H181), C183(H183), C69(H69), C72(H72), C74(H74), C79(H79),
 C84(H84), C87(H87), C89(H89), C94(H94), C99(H99), C102(H102), C104(H104),
 C109(H109), C114(H114), C117(H117), C119(H119)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C22(H22A,H22B), C25(H25A,H25B),
 C26(H26A,H26B), C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B), C51(H51A,H51B),
  C52(H52A,H52B), C54(H54A,H54B), C134(H13A,H13B), C135(H13C,H13D), C137(H13E,
 H13F), C149(H14D,H14E), C150(H15A,H15B), C152(H15C,H15D), C164(H16D,H16E),
 C165(H16F,H16G), C167(H16H,H16I), C179(H17D,H17E), C180(H18A,H18B), C182(H18C,
 H18D), C70(H70A,H70B), C71(H71A,H71B), C73(H73A,H73B), C85(H85A,H85B),
 C86(H86A,H86B), C88(H88A,H88B), C100(H10A,H10B), C101(H10C,H10D), C103(H10E,
 H10F), C115(H11G,H11H), C116(H11I,H11J), C118(H11K,H11L)
3.c Aromatic/amide H refined with riding coordinates:
 N12(H12), N17(H17), N27(H27), N32(H32), N42(H42), N47(H47), N57(H57),
 N140(H140), N145(H145), N155(H155), N160(H160), N170(H170), N175(H175),
 N185(H185), N76(H76), N81(H81), N91(H91), N96(H96), N106(H106), N111(H111),
 N121(H121)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C31(H31A,H31B,H31C), C41(H41A,H41B,H41C), C46(H46A,H46B,H46C), C56(H56A,
 H56B,H56C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C),
 C129(H12A,H12B,H12C), C139(H13G,H13H,H13I), C144(H14A,H14B,H14C), C154(H15E,
 H15F,H15G), C159(H15H,H15I,H15J), C169(H16J,H16K,H16L), C174(H17A,H17B,H17C),
 C184(H18E,H18F,H18G), C190(H19A,H19B,H19C), C191(H19D,H19E,H19F), C192(H19G,
 H19H,H19I), C65(H65A,H65B,H65C), C75(H75A,H75B,H75C), C80(H80A,H80B,H80C),
 C90(H90A,H90B,H90C), C95(H95A,H95B,H95C), C105(H10G,H10H,H10I), C110(H11D,H11E,
 H11F), C120(H12D,H12E,H12F), C126(H12G,H12H,H12I), C127(H12J,H12K,H12L),
 C128(H12M,H12N,H12O)
;
_shelx_res_checksum              15338
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'