Helix-forming aliphatic homo-δ-peptide foldamers based on the conformational restriction effects of cyclopropane.
Nagata, Makoto; Watanabe, Mizuki; Doi, Ryohei; Uemura, Mai; Ochiai, Nanase; Ichinose, Wataru; Fujiwara, Koichi; Sato, Yoshihiro; Kameda, Tomoshi; Takeuchi, Koh; Shuto, Satoshi; Organic & biomolecular chemistry 21 (2023) 970–980; doi:10.1039/d2ob01715f

data_7159012
_publ_section_title
;
 Helix-forming aliphatic homo-&#x3b4;-peptide foldamers based on the
 conformational restriction effects of cyclopropane.
;
_journal_issue                   5
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              970
_journal_page_last               980
_journal_paper_doi               10.1039/d2ob01715f
_journal_volume                  21
_journal_year                    2023
_chemical_formula_moiety         'C H Cl3, C54 H90 N6 O9'
_chemical_formula_sum            'C55 H91 Cl3 N6 O9'
_chemical_formula_weight         1086.68
_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   geom
_audit_creation_date             2020-12-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2020-12-10 deposited with the CCDC.	2022-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.487(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.84115(18)
_cell_length_b                   34.7841(6)
_cell_length_c                   10.17820(18)
_cell_measurement_reflns_used    24800
_cell_measurement_temperature    133
_cell_measurement_theta_max      68.23
_cell_measurement_theta_min      4.90
_cell_volume                     3090.8(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      133.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            35992
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         4.898
_exptl_absorpt_coefficient_mu    1.779
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 2759 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.075(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         11242
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.4409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1437
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                8495
_reflns_number_total             11242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob01715f2.cif
_cod_data_source_block           nachexamer
_cod_depositor_comments
'Adding full bibliography for 7159010--7159012.cif.'
_cod_database_code               7159012
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.784
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C9(H9), C11(H11), C13(H13), C16(H16), C18(H18),
 C20(H20), C21(H21), C24(H24), C26(H26), C28(H28), C29(H29), C32(H32), C34(H34),
  C36(H36), C37(H37), C40(H40), C42(H42), C44(H44), C47(H47), C49(H49),
 C51(H51), C55(H55)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C19(H19A,H19B), C27(H27A,H27B), C35(H35A,H35B), C43(H43A,
 H43B), C50(H50A,H50B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C25(H25A,H25B,
 H25C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C38(H38A,H38B,H38C), C41(H41A,
 H41B,H41C), C45(H45A,H45B,H45C), C48(H48A,H48B,H48C), C52(H52A,H52B,H52C),
 C54(H54A,H54B,H54C)
;
_shelx_res_checksum              84377
_olex2_submission_special_instructions 'No special instructions were received'