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_4130969
_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_formula_moiety         'C41 H67 N5 O8'
_chemical_formula_sum            'C41 H67 N5 O8'
_chemical_formula_weight         757.99
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-15
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2014.11.26 svn.r3098 for OlexSys, GUI svn.r4953)
;
_cell_angle_alpha                89.214(12)
_cell_angle_beta                 89.300(15)
_cell_angle_gamma                89.609(13)
_cell_formula_units_Z            4
_cell_length_a                   12.826(4)
_cell_length_b                   16.245(5)
_cell_length_c                   21.953(6)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.324
_cell_measurement_theta_min      2.233
_cell_volume                     4573(2)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX2 Ver. 2014.7-1 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008-2014)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008-2014)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008-2014)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2014)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            99732
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         1.254
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1444 before and 0.0419 after correction.
The Ratio of minimum to maximum transmission is 0.9286.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         18605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+1.7243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15884
_reflns_number_total             18605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b08235_si_001.cif
_cod_data_source_block           choi04_sq
_cod_database_code               4130969
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.972
_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(H6), C11(H11), C13(H13), C18(H18), C20(H20), C25(H25), C27(H27), C32(H32),
 C34(H34), C39(H39), C6A(H6A), C11A(H11A), C13A(H13A), C18A(H18A), C20A(H20A),
 C25A(H25A), C27A(H27A), C32A(H32A), C34A(H34A), C39A(H39A)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C21(H21A,H21B), C22(H22A,H22B),
  C23(H23A,H23B), C24(H24A,H24B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,
 H30B), C31(H31A,H31B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C38(H38A,H38B), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10A(H10C,
 H10D), C14A(H14C,H14D), C15A(H15C,H15D), C16A(H16C,H16D), C17A(H17C,H17D),
 C21A(H21C,H21D), C22A(H22C,H22D), C23A(H23C,H23D), C24A(H24C,H24D), C28A(H28C,
 H28D), C29A(H29C,H29D), C30A(H30C,H30D), C31A(H31C,H31D), C35A(H35C,H35D),
 C36A(H36C,H36D), C37A(H37C,H37D), C38A(H38C,H38D)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C41(H41A,H41B,H41C),
 C1A(H1AB,H1AC,H1AD), C2A(H2AB,H2AC,H2AD), C3A(H3AB,H3AC,H3AD), C41A(H41D,H41E,
 H41F)
;
_shelx_res_checksum              77283
_shelx_hkl_checksum              41185
_shelx_fab_checksum              16342
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'