Intramolecular CH⋯π attraction mediated conformational polymorphism of constrained helical peptides.
Sun, Jinming; Tian, Zi-You; Liu, Jianbo; Wan, Chuan; Dai, Chuan; Liu, Zhihong; Xing, Yun; Wu, Yujie; Hou, Zhanfeng; Han, Wei; Yin, Feng; Ye, Yuxin; Li, Zigang; Chemical science 15 (2024) 14264–14272; doi:10.1039/d4sc02545h

data_1572786
_publ_section_title
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 Intramolecular CH&#x22ef;&#x3c0; attraction mediated conformational
 polymorphism of constrained helical peptides.
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_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              14264
_journal_page_last               14272
_journal_paper_doi               10.1039/d4sc02545h
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration Unknow
_chemical_formula_moiety         'C30 H46 N6 O6 S'
_chemical_formula_sum            'C30 H46 N6 O6 S'
_chemical_formula_weight         618.79
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-11-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
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_audit_update_record
;
2023-09-01 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.47390(10)
_cell_length_b                   10.47390(10)
_cell_length_c                   61.7275(8)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      68.41
_cell_measurement_theta_min      2.62
_cell_volume                     6771.67(13)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       77
_diffrn_reflns_limit_l_min       -78
_diffrn_reflns_number            40369
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.077
_diffrn_reflns_theta_min         2.863
_exptl_absorpt_coefficient_mu    1.247
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 2264 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7029
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      4.144
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0494P)^2^+2.7186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.657
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                6302
_reflns_number_total             7029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02545h2.cif
_cod_data_source_block           aal-r-0425_auto_sx
_cod_original_cell_volume        6771.67(16)
_cod_database_code               1572786
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.855
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H18 of N18, H27 of N27, H15 of N15, H9 of N9, {H40A,H40B,
  H40C} of C40, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  {H30A,H30B,H30C} of C30, {H42A,H42B,H42C} of C42, H32A of N32, {H41A,H41B,
  H41C} of C41, {H43A,H43B,H43C} of C43, {H43D,H43E,H43F} of C43A
2. Restrained distances
 H10-H40C
 2.2 with sigma of 0.02
 N12-C13 \\sim N12-C13A
 with sigma of 0.02
 C14-C13 \\sim C14-C13A
 with sigma of 0.02
 N12-C43 \\sim N12-C43A
 with sigma of 0.04
 C13-C43 \\sim C13A-C43A
 with sigma of 0.02
 C14-C43 \\sim C14-C43A
 with sigma of 0.04
 N32-H32A \\sim N32-H32B
 with sigma of 0.02
3. Others
 Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(1)
 Sof(H12)=Sof(C13)=Sof(H13)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C19(H19), C7(H7), C16(H16), C10(H10), C39(H39), C13(H13), C13A(H13A)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C20(H20A,H20B), C3(H3A,H3B), C6(H6A,H6B), C4(H4A,H4B), C38(H38A,
 H38B)
4.c Me refined with riding coordinates:
 C40(H40A,H40B,H40C)
4.d Aromatic/amide H refined with riding coordinates:
 N15(H15), N18(H18), N27(H27), N9(H9), N12(H12), N12(H12A), C26(H26), C22(H22),
  C25(H25), C24(H24), C23(H23)
4.e Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C30(H30A,H30B,H30C), C41(H41A,H41B,H41C), C43(H43A,H43B,
 H43C), C43A(H43D,H43E,H43F)
4.f Idealised tetrahedral OH refined as rotating group:
 N32(H32A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30781
_shelx_hkl_checksum              6250
_shelx_fab_checksum              2084
_olex2_submission_special_instructions 'No special instructions were received'