Side chain-specific 11/9-helix propensity of α/β-peptides with alternating residue types.
Lee, Jaeyeon; Shim, Jihyun; Kang, Philjae; Choi, Moon-Gun; Choi, Soo Hyuk; Organic & biomolecular chemistry 16 (2018) 433–438; doi:10.1039/c7ob02816d

data_7156022
_publ_section_title
;
 Side chain-specific 11/9-helix propensity of \a/\b-peptides with
 alternating residue types.
;
_journal_issue                   3
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              433
_journal_page_last               438
_journal_paper_doi               10.1039/c7ob02816d
_journal_volume                  16
_journal_year                    2018
_chemical_absolute_configuration rm
_chemical_formula_moiety         '2(C H Cl3), C31 H53 N5 O8'
_chemical_formula_sum            'C33 H55 Cl6 N5 O8'
_chemical_formula_weight         862.52
_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             2014-03-13
_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.
2017-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1637(4)
_cell_length_b                   17.2472(5)
_cell_length_c                   25.5023(9)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    219.9
_cell_measurement_theta_max      23.380
_cell_measurement_theta_min      2.33
_cell_volume                     4470.4(3)
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      219.9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.995
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39981
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.971
_diffrn_reflns_theta_min         2.326
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0422 before and 0.0387 after correction.
The Ratio of minimum to maximum transmission is 0.9352.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 2437 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.003(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0772
_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^)+(0.1449P)^2^+2.2869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2108
_refine_ls_wR_factor_ref         0.2342
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                6492
_reflns_number_total             8711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ob02816d2.cif
_cod_data_source_block           A-ACHC-V-ACHC-A_moon223
_cod_depositor_comments          'Adding full bibliography for 7156022.cif.'
_cod_database_code               7156022
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5(0.055) H13(0.058) H16(0.047) H24(0.039) H27(0.042) H1A(0.187)
 H1B(0.187) H1C(0.187) H4(0.063) H7(0.056) H8A(0.079) H8B(0.079) H9A(0.091)
 H9B(0.091) H10A(0.105) H10B(0.105) H11A(0.085) H11B(0.085) H12(0.063)
 H15(0.055) H18(0.048) H19A(0.071) H19B(0.071) H20A(0.078) H20B(0.078)
 H21A(0.067) H21B(0.067) H22A(0.057) H22B(0.057) H23(0.043) H26(0.041)
 H31A(0.163) H31B(0.163) H31C(0.163) H32A(0.256) H32B(0.256) H32C(0.256)
 H33A(0.24) H33B(0.24) H33C(0.24) H35A(0.128) H35B(0.128) H35C(0.128)
 H38(0.079) H39A(0.153) H39B(0.153) H39C(0.153) H40A(0.179) H40B(0.179)
 H40C(0.179) H43A(0.077) H43B(0.077) H43C(0.077) H60A(0.135) H60(0.135)
 H50(0.126)
 Fixed X: H5(-0.0958) H13(0.1992) H16(0.184) H24(0.1682) H27(0.5144)
 H1A(0.0744) H1B(0.0421) H1C(-0.0405) H4(-0.2086) H7(-0.0113) H8A(0.0285) H8B(-
 0.0901) H9A(0.0723) H9B(0.0477) H10A(0.2749) H10B(0.2624) H11A(0.3413)
 H11B(0.2153) H12(0.2116) H15(0.1499) H18(0.0103) H19A(-0.2087) H19B(-0.2054)
 H20A(-0.361) H20B(-0.2576) H21A(-0.2823) H21B(-0.248) H22A(-0.0655) H22B(-
 0.0622) H23(-0.0269) H26(0.3779) H31A(0.3691) H31B(0.3985) H31C(0.3024)
 H32A(0.5668) H32B(0.4996) H32C(0.4115) H33A(0.6103) H33B(0.6771) H33C(0.6809)
 H35A(-0.2819) H35B(-0.2688) H35C(-0.159) H38(0.333) H39A(0.4165) H39B(0.5207)
 H39C(0.4709) H40A(0.4048) H40B(0.4482) H40C(0.3006) H43A(0.5063) H43B(0.3618)
 H43C(0.4067) H60A(0.2376) H60(0.2563) H50(-0.0555)
 Fixed Y: H5(1.1387) H13(1.1724) H16(0.9133) H24(0.9463) H27(0.7893)
 H1A(1.2592) H1B(1.1732) H1C(1.2433) H4(1.2279) H7(1.1848) H8A(1.2818)
 H8B(1.3127) H9A(1.4109) H9B(1.3973) H10A(1.4008) H10B(1.3347) H11A(1.2813)
 H11B(1.3122) H12(1.2) H15(1.0521) H18(0.8431) H19A(0.8251) H19B(0.888)
 H20A(0.9196) H20B(0.9869) H21A(0.9675) H21B(0.8784) H22A(1.0009) H22B(0.9463)
 H23(0.8379) H26(0.9168) H31A(0.6429) H31B(0.6179) H31C(0.6882) H32A(0.8157)
 H32B(0.7575) H32C(0.8083) H33A(0.6178) H33B(0.6872) H33C(0.6853) H35A(1.0998)
 H35B(1.1151) H35C(1.0672) H38(0.9642) H39A(0.9627) H39B(0.9768) H39C(1.0473)
 H40A(1.1234) H40B(1.0619) H40C(1.0913) H43A(0.8755) H43B(0.8937) H43C(0.8067)
 H60A(1.144) H60(1.1278) H50(0.889)
 Fixed Z: H5(0.1124) H13(0.1365) H16(0.1243) H24(0.0049) H27(0.0202)
 H1A(0.3023) H1B(0.3199) H1C(0.3429) H4(0.1861) H7(0.0398) H8A(-0.019)
 H8B(0.0153) H9A(0) H9B(0.0608) H10A(0.0455) H10B(0.0027) H11A(0.0818)
 H11B(0.112) H12(0.0311) H15(0.1656) H18(0.0928) H19A(0.0768) H19B(0.122)
 H20A(0.0544) H20B(0.0638) H21A(-0.0251) H21B(-0.0189) H22A(0) H22B(-0.0501)
 H23(0.0037) H26(0.0158) H31A(0.1945) H31B(0.1359) H31C(0.1475) H32A(0.1921)
 H32B(0.232) H32C(0.194) H33A(0.1598) H33B(0.1905) H33C(0.1284) H35A(0.1659)
 H35B(0.227) H35C(0.1971) H38(0.1848) H39A(0.1006) H39B(0.1457) H39C(0.1112)
 H40A(0.1817) H40B(0.2244) H40C(0.2225) H43A(-0.0559) H43B(-0.0757) H43C(-
 0.067) H60A(-0.1516) H60(-0.1441) H50(0.3236)
;