Helical α/β-depsipeptides with alternating residue types: conformational change from the 11-helix to the 14/15-helix.
Lee, Jaeyeon; Jang, Geunhyeok; Kang, Philjae; Choi, Moon-Gun; Choi, Soo Hyuk; Organic & biomolecular chemistry 14 (2016) 8438–8442; doi:10.1039/c6ob01602b

data_7155250
_publ_section_title
;
 Helical \a/\b-depsipeptides with alternating residue types:
 conformational change from the 11-helix to the 14/15-helix.
;
_journal_issue                   36
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8438
_journal_page_last               8442
_journal_paper_doi               10.1039/c6ob01602b
_journal_volume                  14
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C38 H62 N6 O11'
_chemical_formula_sum            'C38 H62 N6 O11'
_chemical_formula_weight         778.93
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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.
2016-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.429(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7226(16)
_cell_length_b                   10.6558(17)
_cell_length_c                   21.682(3)
_cell_measurement_reflns_used    2787
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      19.69
_cell_measurement_theta_min      2.68
_cell_volume                     2476.6(6)
_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      250.1
_diffrn_measured_fraction_theta_full 0.997
_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  0.1605
_diffrn_reflns_av_unetI/netI     0.1975
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24592
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.047
_diffrn_reflns_theta_min         0.939
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0837 before and 0.0653 after correction.
The Ratio of minimum to maximum transmission is 0.6986.
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    1.045
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
 ?
;
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 1333 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.4(10)
_refine_ls_extinction_coef       0.0027(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         9623
_refine_ls_number_restraints     478
_refine_ls_restrained_S_all      0.791
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.0696
_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^)+(0.0786P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1673
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                3980
_reflns_number_total             9623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ob01602b2.cif
_cod_data_source_block           Aib-ACPC-Lac-ACPC-Ala-ACPC-Aib_moon226
_cod_depositor_comments
'Adding full bibliography for 7155248--7155250.cif.'
_cod_original_cell_volume        2476.6(7)
_cod_database_code               7155250
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Shared sites
{H19A, H19C}
2. Others
 Fixed Uiso: H5(0.05) H12(0.051) H15(0.057) H22(0.049) H32(0.055) H35(0.073)
 H2A(0.198) H2B(0.198) H2C(0.198) H7(0.047) H9A(0.089) H9B(0.089) H10A(0.086)
 H10B(0.086) H11(0.047) H14A(0.077) H14B(0.077) H15A(0.059) H17(0.061)
 H18A(0.096) H18B(0.096) H18C(0.096) H18D(0.096) H19A(0.128) H19B(0.128)
 H20A(0.109) H20B(0.109) H20C(0.109) H20D(0.109) H21(0.06) H24(0.046)
 H27(0.056) H28A(0.089) H28B(0.089) H29A(0.104) H29B(0.104) H30A(0.082)
 H30B(0.082) H31(0.053) H39A(0.215) H39B(0.215) H39C(0.215) H39D(0.2) H39E(0.2)
 H39F(0.2) H40A(0.175) H40B(0.175) H40C(0.175) H40D(0.17) H40E(0.17) H40F(0.17)
 H41A(0.177) H41B(0.177) H41C(0.177) H41D(0.181) H41E(0.181) H41F(0.181)
 H43A(0.092) H43B(0.092) H43C(0.092) H44A(0.101) H44B(0.101) H44C(0.101)
 H47A(0.108) H47B(0.108) H47C(0.108) H50A(0.107) H50B(0.107) H50C(0.107)
 H53A(0.131) H53B(0.131) H53C(0.131) H54A(0.104) H54B(0.104) H54C(0.104)
 H19C(0.086) H19D(0.086)
 Fixed X: H5(0.4122) H12(0.454) H15(0.5827) H22(0.7285) H32(1.0367)
 H35(1.1897) H2A(0.0202) H2B(-0.0783) H2C(0.0414) H7(0.4487) H9A(0.5124)
 H9B(0.4133) H10A(0.2638) H10B(0.3803) H11(0.2275) H14A(0.4597) H14B(0.3161)
 H15A(0.3605) H17(0.64) H18A(0.4414) H18B(0.5835) H18C(0.544) H18D(0.4378)
 H19A(0.5641) H19B(0.4556) H20A(0.6262) H20B(0.7157) H20C(0.586) H20D(0.7203)
 H21(0.5053) H24(0.7165) H27(0.9303) H28A(0.8293) H28B(0.7071) H29A(0.7723)
 H29B(0.8911) H30A(1.0172) H30B(0.918) H31(0.7954) H39A(1.2028) H39B(1.1556)
 H39C(1.0736) H39D(1.063) H39E(1.1205) H39F(1.1743) H40A(1.3831) H40B(1.3775)
 H40C(1.4134) H40D(1.3461) H40E(1.4241) H40F(1.337) H41A(1.0771) H41B(1.1669)
 H41C(1.2107) H41D(1.1676) H41E(1.0835) H41F(1.2189) H43A(0.222) H43B(0.1349)
 H43C(0.1115) H44A(0.4016) H44B(0.3092) H44C(0.4125) H47A(0.5382) H47B(0.4284)
 H47C(0.5371) H50A(0.9065) H50B(0.8147) H50C(0.9067) H53A(1.011) H53B(0.8844)
 H53C(0.9119) H54A(1.102) H54B(0.9877) H54C(1.114) H19C(0.5593) H19D(0.6824)
 Fixed Y: H5(0.1509) H12(0.471) H15(0.5025) H22(0.3041) H32(0.5852)
 H35(0.4414) H2A(0.0077) H2B(-0.0694) H2C(-0.1373) H7(0.346) H9A(0.5513)
 H9B(0.5866) H10A(0.6164) H10B(0.6623) H11(0.4769) H14A(0.3575) H14B(0.3952)
 H15A(0.6099) H17(0.3297) H18A(0.2125) H18B(0.2056) H18C(0.2331) H18D(0.1748)
 H19A(0.0025) H19B(0.034) H20A(0.0049) H20B(0.0811) H20C(0.0038) H20D(0.063)
 H21(0.1853) H24(0.2985) H27(0.5864) H28A(0.7294) H28B(0.7239) H29A(0.8833)
 H29B(0.8929) H30A(0.7857) H30B(0.8355) H31(0.6571) H39A(0.8427) H39B(0.9236)
 H39C(0.8108) H39D(0.7897) H39E(0.7962) H39F(0.8832) H40A(0.6543) H40B(0.7783)
 H40C(0.7858) H40D(0.8032) H40E(0.7592) H40F(0.8789) H41A(0.7234) H41B(0.8322)
 H41C(0.6905) H41D(0.5458) H41E(0.6653) H41F(0.6568) H43A(0.0845) H43B(-0.0239)
 H43C(0.117) H44A(-0.0915) H44B(-0.143) H44C(-0.0431) H47A(0.7304) H47B(0.7836)
 H47C(0.7047) H50A(0.2128) H50B(0.1046) H50C(0.1669) H53A(0.2691) H53B(0.267)
 H53C(0.3779) H54A(0.3462) H54B(0.2568) H54C(0.2426) H19C(0.0064) H19D(0.0876)
 Fixed Z: H5(0.1156) H12(0.1744) H15(0.2781) H22(0.236) H32(0.2544) H35(0.33)
 H2A(-0.0245) H2B(0.0134) H2C(-0.012) H7(0.0966) H9A(0.029) H9B(-0.0242)
 H10A(0.0405) H10B(0.0814) H11(0.1122) H14A(-0.0091) H14B(-0.0179) H15A(0.3033)
 H17(0.3336) H18A(0.3852) H18B(0.4079) H18C(0.4128) H18D(0.3688) H19A(0.3777)
 H19B(0.3284) H20A(0.2672) H20B(0.3141) H20C(0.2776) H20D(0.2907) H21(0.245)
 H24(0.0813) H27(0.1321) H28A(0.0748) H28B(0.1149) H29A(0.1692) H29B(0.127)
 H30A(0.1979) H30B(0.2461) H31(0.2358) H39A(0.3404) H39B(0.3965) H39C(0.3706)
 H39D(0.4444) H39E(0.3779) H39F(0.4315) H40A(0.4392) H40B(0.4793) H40C(0.409)
 H40D(0.3737) H40E(0.4328) H40F(0.4363) H41A(0.479) H41B(0.5025) H41C(0.5074)
 H41D(0.4952) H41E(0.5067) H41F(0.5373) H43A(0.2048) H43B(0.1782) H43C(0.1576)
 H44A(0.0944) H44B(0.1444) H44C(0.1634) H47A(0.2937) H47B(0.2511) H47C(0.2218)
 H50A(0.0738) H50B(0.0939) H50C(0.1433) H53A(0.3908) H53B(0.3515) H53C(0.3986)
 H54A(0.2395) H54B(0.2528) H54C(0.2917) H19C(0.3766) H19D(0.3879)
;