Stabilization of 11/9-helical alpha/beta-peptide foldamers in protic solvents
Mihye Lee; Jihyun Shim; Philjae Kang; Moon-Gun Choi; Soo Hyuk Choi; Chem.Commun. 52 (2016) 5950–; doi:

data_7119039
_publ_section_title
;
 Stabilization of 11/9-helical alpha/beta-peptide foldamers in protic
 solvents
;
_journal_name_full               Chem.Commun.
_journal_page_first              5950
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C29 H49 N5 O8'
_chemical_formula_sum            'C29 H49 N5 O8'
_chemical_formula_weight         595.73
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_audit_update_record
;
2016-01-21 deposited with the CCDC.
2016-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7107(7)
_cell_length_b                   17.8054(12)
_cell_length_c                   18.6925(14)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.24
_cell_measurement_theta_min      2.39
_cell_volume                     3232.0(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.840
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 0.840
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            200536
_diffrn_reflns_point_group_measured_fraction_full 0.833
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         24.328
_diffrn_reflns_theta_min         2.179
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.7095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0623 before and 0.0565 after correction.
The Ratio of minimum to maximum transmission is 0.9523.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.028
_refine_ls_abs_structure_details
;
 Flack x determined using 2117 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.06(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0335P)^2^+0.8190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_full    0.825
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5036
_reflns_number_total             5268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc01189f2.cif
_cod_data_source_block           DAla-ACHC_5mer_moon116
_cod_database_code               7119039
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.059) H1B(0.059) H1C(0.059) H4(0.035) H7(0.028) H8A(0.035)
 H8B(0.035) H9A(0.04) H9B(0.04) H10A(0.043) H10B(0.043) H11A(0.035) H11B(0.035)
 H12(0.028) H15(0.026) H18(0.028) H19A(0.036) H19B(0.036) H20A(0.045)
 H20B(0.045) H21A(0.041) H21B(0.041) H22A(0.036) H22B(0.036) H23(0.028)
 H26(0.032) H31A(0.086) H31B(0.086) H31C(0.086) H32A(0.075) H32B(0.075)
 H32C(0.075) H33A(0.066) H33B(0.066) H33C(0.066) H35A(0.065) H35B(0.065)
 H35C(0.065) H38A(0.052) H38B(0.052) H38C(0.052) H41A(0.059) H41B(0.059)
 H41C(0.059) H5(0.034) H13(0.026) H16(0.026) H24(0.028) H27(0.039)
 Fixed X: H1A(1.0383) H1B(1.058) H1C(1.1897) H4(1.0568) H7(0.672) H8A(0.854)
 H8B(0.7027) H9A(0.9096) H9B(0.852) H10A(0.634) H10B(0.75) H11A(0.7512)
 H11B(0.5981) H12(0.5345) H15(0.3757) H18(0.7241) H19A(0.5697) H19B(0.5443)
 H20A(0.6988) H20B(0.7985) H21A(0.8903) H21B(0.7483) H22A(0.9058) H22B(0.927)
 H23(0.7821) H26(0.518) H31A(0.0509) H31B(-0.0503) H31C(-0.0071) H32A(0.2906)
 H32B(0.1424) H32C(0.2379) H33A(0.0672) H33B(0.0365) H33C(0.1871) H35A(0.8761)
 H35B(1.0407) H35C(0.9641) H38A(0.5214) H38B(0.3612) H38C(0.4166) H41A(0.7143)
 H41B(0.744) H41C(0.6359) H5(0.7956) H13(0.6144) H16(0.6561) H24(0.6233)
 H27(0.4694)
 Fixed Y: H1A(0.8705) H1B(0.8536) H1C(0.8672) H4(1.086) H7(1.1423) H8A(1.1867)
 H8B(1.1891) H9A(1.0796) H9B(1.1419) H10A(1.0827) H10B(1.0235) H11A(0.9714)
 H11B(0.968) H12(1.0747) H15(0.9388) H18(0.8128) H19A(0.7275) H19B(0.6883)
 H20A(0.6139) H20B(0.6844) H21A(0.6101) H21B(0.6146) H22A(0.7014) H22B(0.7398)
 H23(0.8169) H26(0.6848) H31A(0.7875) H31B(0.8573) H31C(0.8052) H32A(0.9392)
 H32B(0.9407) H32C(0.8678) H33A(0.9187) H33B(0.9721) H33C(0.9702) H35A(1.0968)
 H35B(1.0952) H35C(1.1657) H38A(1.0345) H38B(1.0414) H38C(0.97) H41A(0.7611)
 H41B(0.6844) H41C(0.6857) H5(1.131) H13(0.9525) H16(0.9209) H24(0.692)
 H27(0.7987)
 Fixed Z: H1A(0.5749) H1B(0.6584) H1C(0.6086) H4(0.6802) H7(0.7773) H8A(0.856)
 H8B(0.8896) H9A(0.9223) H9B(0.9764) H10A(0.9782) H10B(1.0014) H11A(0.8848)
 H11B(0.9166) H12(0.8524) H15(0.6786) H18(0.5934) H19A(0.5427) H19B(0.6186)
 H20A(0.5529) H20B(0.5403) H21A(0.6326) H21B(0.6761) H22A(0.7251) H22B(0.6485)
 H23(0.7132) H26(0.8536) H31A(0.8205) H31B(0.8327) H31C(0.8988) H32A(0.8134)
 H32B(0.776) H32C(0.7693) H33A(0.9622) H33B(0.8952) H33C(0.9299) H35A(0.559)
 H35B(0.5544) H35C(0.5896) H38A(0.5825) H38B(0.6015) H38C(0.5582) H41A(0.9422)
 H41B(0.9003) H41C(0.9649) H5(0.6832) H13(0.7762) H16(0.6654) H24(0.7481)
 H27(0.9486)
;