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_1572785
_publ_section_title
;
 Intramolecular CH&#x22ef;&#x3c0; attraction mediated conformational
 polymorphism of constrained helical peptides.
;
_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 unk
_chemical_formula_moiety         'C29 H44 N6 O6 S, 4(H2 O)'
_chemical_formula_sum            'C29 H52 N6 O10 S'
_chemical_formula_weight         676.30
_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     dual
_audit_creation_date             2023-02-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_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            4
_cell_length_a                   9.64330(10)
_cell_length_b                   16.0251(2)
_cell_length_c                   22.6439(3)
_cell_measurement_temperature    100(2)
_cell_volume                     3499.27(7)
_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)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    146.00 172.00   0.50    0.57    --  105.63  41.00-107.00   52
  2  \w     44.00  73.00   0.50    0.57    --  105.63 -61.00 -90.00   58
  3  \w     42.00 104.00   0.50    0.57    --  105.63-128.00  43.00  124
  4  \w    -14.00  22.00   0.50    0.14    --   46.55 -19.00 -60.00   72
  5  \w    -25.00  28.00   0.50    0.14    --   46.55 -19.00-180.00  106
  6  \w   -145.00 -92.00   0.50    0.57    -- -104.00 -30.00 -30.00  106
  7  \w   -165.00 -84.00   0.50    0.57    -- -104.00 -80.00 -72.00  162
  8  \w   -106.00 -66.00   0.50    0.14    --  -46.55-141.00-127.00   80
  9  \w   -143.00-117.00   0.50    0.57    -- -104.00-128.00  43.00   52
 10  \w   -145.00-101.00   0.50    0.57    -- -104.00 -61.00 -30.00   88
 11  \w    -67.00 -32.00   0.50    0.57    -- -104.00  61.00  60.00   70
 12  \w    -67.00 -31.00   0.50    0.57    -- -104.00  61.00 120.00   72
 13  \w    -66.00 -35.00   0.50    0.57    -- -104.00  61.00 150.00   62
 14  \w    -88.00 -41.00   0.50    0.57    -- -104.00  77.00 120.00   94
 15  \w    -64.00 -31.00   0.50    0.57    -- -104.00  61.00 -30.00   66
 16  \w   -101.00 -31.00   0.50    0.57    -- -104.00  77.00-150.00  140
 17  \w    -59.00 -31.00   0.50    0.57    -- -104.00  61.00-120.00   56
 18  \w    -42.00  26.00   0.50    0.14    --  -46.55  41.00-107.00  136
 19  \w    -20.00   7.00   0.50    0.14    --  -46.55  19.00-150.00   54
 20  \w    -22.00  12.00   0.50    0.14    --  -46.55  19.00 -30.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0828391000
_diffrn_orient_matrix_UB_12      -0.0808963000
_diffrn_orient_matrix_UB_13      0.0106484000
_diffrn_orient_matrix_UB_21      0.0062263000
_diffrn_orient_matrix_UB_22      0.0152878000
_diffrn_orient_matrix_UB_23      0.0670998000
_diffrn_orient_matrix_UB_31      -0.1364324000
_diffrn_orient_matrix_UB_32      0.0496876000
_diffrn_orient_matrix_UB_33      -0.0034088000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20927
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.532
_diffrn_reflns_theta_min         3.379
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.335
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 2761 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7023
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0576P)^2^+1.1071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                6717
_reflns_number_total             7023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02545h2.cif
_cod_data_source_block           aav-r-0416-cube_auto
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_absolute_configuration' value 'unK' was changed
to 'unk' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               1572785
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N S'
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.690
_olex2_refinement_description
;
1. Restrained distances
 O43-H43A = O43-H43B
 0.87 with sigma of 0.02
 O44-H44A = O44-H44B
 0.87 with sigma of 0.02
 O45-H45A = O45-H45B
 0.87 with sigma of 0.02
 H44A-H44B
 1.38 with sigma of 0.04
 H43A-H43B
 1.38 with sigma of 0.04
 H45A-H45B
 1.38 with sigma of 0.04
2.a Free rotating group:
 O46(H46A,H46B)
2.b Ternary CH refined with riding coordinates:
 C15(H15), C3(H3), C6(H6), C12(H12), C9(H9), C38(H38), C1(H1)
2.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C19(H19A,H19B), C2(H2A,H2B), C18(H18A,H18B), C20(H20A,H20B)
2.d Aromatic/amide H refined with riding coordinates:
 N4(H4), N7(H7), N13(H13), N10(H10), N27(H27), C26(H26), C22(H22), C25(H25),
 C23(H23), C24(H24)
2.e X=CH2 refined with riding coordinates:
 N32(H32A,H32B)
2.f Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C30(H30A,H30B,
 H30C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              2738
_shelx_hkl_checksum              84855
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.440
_oxdiff_exptl_absorpt_empirical_full_min 0.749