12/10-Helical β-Peptide with Dynamic Folding Propensity: Coexistence of Right- and Left-Handed Helices in an Enantiomeric Foldamer.
Shin, Seonho; Lee, Mihye; Guzei, Ilia A.; Kang, Young Kee; Choi, Soo Hyuk; Journal of the American Chemical Society 138 (2016) 13390–13395; doi:10.1021/jacs.6b08235

data_4130971
_publ_section_title
;
 12/10-Helical \b-Peptide with Dynamic Folding Propensity: Coexistence of
 Right- and Left-Handed Helices in an Enantiomeric Foldamer.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13390
_journal_page_last               13395
_journal_paper_doi               10.1021/jacs.6b08235
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H74 N6 O7'
_chemical_formula_sum            'C44 H74 N6 O7'
_chemical_formula_weight         799.09
_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   mixed
_audit_creation_date             2015-04-01
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.03.31 svn.r3164 for OlexSys, GUI svn.r5023)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.663(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5874(16)
_cell_length_b                   23.587(3)
_cell_length_c                   16.789(3)
_cell_measurement_reflns_used    9510
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.62
_cell_measurement_theta_min      3.24
_cell_volume                     4579.3(12)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX2 Ver. 2015.1-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '0.8\% \w and 0.8\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            179483
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         74.760
_diffrn_reflns_theta_min         2.637
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.7062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 8556 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1089
_refine_ls_number_reflns         18654
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0444P)^2^+1.1587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                18215
_reflns_number_total             18654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b08235_si_001.cif
_cod_data_source_block           choi17
_cod_original_cell_volume        4579.1(11)
_cod_database_code               4130971
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6A), C8(H8), C12(H12), C14(H14), C19(H19), C21(H21), C23(H23), C27(H27),
 C29(H29), C34(H34), C36(H36), C38(H38), C42(H42), C6A(H6AB), C8A(H8A),
 C12A(H12A), C14A(H14A), C19A(H19A), C21A(H21A), C23A(H23A), C27A(H27A),
 C29A(H29A), C34A(H34A), C36A(H36A), C38A(H38A), C42A(H42A)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C11(H11A,H11B), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B), C18(H18A,H18B), C22(H22A,H22B), C25(H25A,H25B), C26(H26A,H26B),
  C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C37(H37A,
 H37B), C40(H40A,H40B), C41(H41A,H41B), C7A(H7AA,H7AB), C10A(H10C,H10D),
 C11A(H11C,H11D), C15A(H15C,H15D), C16A(H16C,H16D), C17A(H17C,H17D), C18A(H18C,
 H18D), C22A(H22C,H22D), C25A(H25C,H25D), C26A(H26C,H26D), C30A(H30C,H30D),
 C31A(H31C,H31D), C32A(H32C,H32D), C33A(H33C,H33D), C37A(H37C,H37D), C40A(H40C,
 H40D), C41A(H41C,H41D)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C9(H9A,H9B,H9C), C24(H24A,
 H24B,H24C), C39(H39A,H39B,H39C), C44(H44A,H44B,H44C), C1A(H1AB,H1AC,H1AD),
 C2A(H2AB,H2AC,H2AD), C3A(H3AB,H3AC,H3AD), C9A(H9AA,H9AB,H9AC), C24A(H24D,H24E,
 H24F), C39A(H39D,H39E,H39F), C44A(H44D,H44E,H44F)
;
_shelx_res_checksum              97871
_shelx_hkl_checksum              18087
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'