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_7119038
_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         'C20 H35 N3 O6'
_chemical_formula_sum            'C20 H35 N3 O6'
_chemical_formula_weight         413.51
_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                   9.1953(5)
_cell_length_b                   15.9688(8)
_cell_length_c                   16.3770(9)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.64
_cell_measurement_theta_min      2.49
_cell_volume                     2404.8(2)
_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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42177
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.984
_diffrn_reflns_theta_min         2.487
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0727 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.7417.
The \l/2 correction factor is 0.0015.
;
_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    1.142
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.097
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 1525 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4720
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0326P)^2^+0.4296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3935
_reflns_number_total             4720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc01189f2.cif
_cod_data_source_block           DAla-mACHC-DAla_moon200
_cod_database_code               7119038
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5(0.025) H13(0.024) H16(0.026) H1A(0.071) H1B(0.071) H1C(0.071)
 H4(0.028) H7(0.027) H8A(0.036) H8B(0.036) H9A(0.038) H9B(0.038) H10(0.036)
 H11A(0.028) H11B(0.028) H12(0.026) H15(0.024) H20A(0.05) H20B(0.05) H20C(0.05)
 H21A(0.049) H21B(0.049) H21C(0.049) H22A(0.05) H22B(0.05) H22C(0.05)
 H24A(0.042) H24B(0.042) H24C(0.042) H26A(0.065) H26B(0.065) H26C(0.065)
 H28A(0.04) H28B(0.04) H28C(0.04)
 Fixed X: H5(0.6699) H13(0.5941) H16(0.3121) H1A(0.3471) H1B(0.311)
 H1C(0.4551) H4(0.6542) H7(0.854) H8A(1.0782) H8B(1.0818) H9A(1.0609)
 H9B(1.1935) H10(1.05) H11A(0.814) H11B(0.8058) H12(0.8443) H15(0.3907)
 H20A(0.2827) H20B(0.415) H20C(0.4209) H21A(0.6574) H21B(0.6532) H21C(0.6708)
 H22A(0.4494) H22B(0.4221) H22C(0.2971) H24A(0.4174) H24B(0.4253) H24C(0.5335)
 H26A(1.0315) H26B(1.0155) H26C(1.1678) H28A(0.3719) H28B(0.3518) H28C(0.2323)
 Fixed Y: H5(0.3934) H13(0.2) H16(0.3004) H1A(0.3063) H1B(0.2629) H1C(0.2374)
 H4(0.4318) H7(0.3245) H8A(0.3325) H8B(0.2683) H9A(0.2246) H9B(0.2028)
 H10(0.1076) H11A(0.151) H11B(0.0798) H12(0.1812) H15(0.2541) H20A(0.548)
 H20B(0.6118) H20C(0.5204) H21A(0.4902) H21B(0.5832) H21C(0.5048) H22A(0.5392)
 H22B(0.6225) H22C(0.5531) H24A(0.4408) H24B(0.4897) H24C(0.5143) H26A(0.0725)
 H26B(0.0036) H26C(0.0501) H28A(0.1418) H28B(0.1159) H28C(0.1731)
 Fixed Z: H5(0.2845) H13(0.2749) H16(0.4777) H1A(-0.0367) H1B(0.0491)
 H1C(0.0002) H4(0.1256) H7(0.3406) H8A(0.2632) H8B(0.338) H9A(0.169)
 H9B(0.2286) H10(0.3014) H11A(0.1945) H11B(0.2633) H12(0.3659) H15(0.3298)
 H20A(0.5718) H20B(0.5847) H20C(0.6247) H21A(0.5546) H21B(0.5182) H21C(0.4582)
 H22A(0.3765) H22B(0.4286) H22C(0.4217) H24A(0.2392) H24B(0.154) H24C(0.2266)
 H26A(0.1304) H26B(0.2008) H26C(0.1871) H28A(0.4665) H28B(0.3727) H28C(0.4167)
;