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_7155248
_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         'C H Cl3, C29 H49 N5 O8'
_chemical_formula_sum            'C30 H50 Cl3 N5 O8'
_chemical_formula_weight         715.10
_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             2014-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4773)
;
_audit_update_record
;
2016-01-21 deposited with the CCDC.
2016-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1200(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2919(4)
_cell_length_b                   11.0410(5)
_cell_length_c                   19.2470(10)
_cell_measurement_reflns_used    9536
_cell_measurement_temperature    304
_cell_measurement_theta_max      23.21
_cell_measurement_theta_min      2.64
_cell_volume                     1943.86(16)
_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      304.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44095
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.048
_diffrn_reflns_theta_min         2.135
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0633 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.8822.
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    1.222
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1929 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7676
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0638
_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^)+(0.1095P)^2^+0.4898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1975
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4951
_reflns_number_total             7676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ob01602b2.cif
_cod_data_source_block           mo_moon186_072113_0m_a
_cod_depositor_comments
'Adding full bibliography for 7155248--7155250.cif.'
_cod_original_cell_volume        1943.87(16)
_cod_database_code               7155248
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5(0.072) H12(0.061) H15(0.061) H22(0.069) H25(0.067) H1A(0.166)
 H1B(0.166) H1C(0.166) H7(0.081) H8AA(0.132) H8AB(0.132) H8BC(0.132)
 H8BD(0.132) H9A(0.114) H9B(0.114) H10A(0.093) H10B(0.093) H10C(0.093)
 H10D(0.093) H11(0.063) H14(0.065) H17(0.076) H18A(0.138) H18B(0.138)
 H18C(0.138) H18D(0.138) H19A(0.153) H19B(0.153) H20A(0.118) H20B(0.118)
 H20C(0.118) H20D(0.118) H21(0.074) H29A(0.151) H29B(0.151) H29C(0.151)
 H30A(0.227) H30B(0.227) H30C(0.227) H31A(0.2) H31B(0.2) H31C(0.2) H33A(0.142)
 H33B(0.142) H33C(0.142) H34A(0.12) H34B(0.12) H34C(0.12) H37A(0.137)
 H37B(0.137) H37C(0.137) H40A(0.129) H40B(0.129) H40C(0.129) H41A(0.11)
 H41B(0.11) H41C(0.11) H49A(0.112) H49B(0.112) H50A(0.141) H50B(0.141)
 H51(0.148)
 Fixed X: H5(0.2315) H12(0.244) H15(0.0767) H22(-0.2557) H25(-0.3365)
 H1A(0.3263) H1B(0.2893) H1C(0.4493) H7(0.2413) H8AA(0.4613) H8AB(0.3075)
 H8BC(0.3408) H8BD(0.4972) H9A(0.4334) H9B(0.5703) H10A(0.4816) H10B(0.3182)
 H10C(0.3566) H10D(0.5141) H11(0.5157) H14(0.3188) H17(-0.1264) H18A(-0.0656)
 H18B(-0.2255) H18C(-0.1489) H18D(-0.0756) H19A(-0.2438) H19B(-0.0821) H20A(-
 0.2272) H20B(-0.3193) H20C(-0.3054) H20D(-0.1805) H21(-0.0228) H29A(-0.1758)
 H29B(-0.1542) H29C(-0.0689) H30A(-0.5073) H30B(-0.4414) H30C(-0.4308) H31A(-
 0.1728) H31B(-0.246) H31C(-0.3418) H33A(0.434) H33B(0.4916) H33C(0.5533)
 H34A(0.1337) H34B(0.2289) H34C(0.179) H37A(0.2518) H37B(0.4093) H37C(0.2743)
 H40A(0.0298) H40B(0.0166) H40C(-0.0855) H41A(-0.2894) H41B(-0.1848) H41C(-
 0.3193) H49A(0.3808) H49B(0.2406) H50A(-0.3173) H50B(-0.3372) H51(0.765)
 Fixed Y: H5(0.9814) H12(1.2829) H15(1.3654) H22(1.2937) H25(1.5392)
 H1A(0.5424) H1B(0.6152) H1C(0.615) H7(1.0991) H8AA(1.0293) H8AB(1.083)
 H8BC(1.0332) H8BD(1.0842) H9A(1.2499) H9B(1.2118) H10A(1.3639) H10B(1.3271)
 H10C(1.3681) H10D(1.32) H11(1.1999) H14(1.2953) H17(1.2484) H18A(1.0267)
 H18B(1.0811) H18C(1.0752) H18D(0.9934) H19A(0.9177) H19B(0.9385) H20A(1.0305)
 H20B(1.0947) H20C(1.0877) H20D(0.9906) H21(1.1398) H29A(1.7616) H29B(1.7036)
 H29C(1.6519) H30A(1.6142) H30B(1.6431) H30C(1.739) H31A(1.4414) H31B(1.4898)
 H31C(1.4272) H33A(0.9408) H33B(0.8071) H33C(0.9022) H34A(0.7877) H34B(0.7316)
 H34C(0.8673) H37A(1.4963) H37B(1.4876) H37C(1.5099) H40A(1.5867) H40B(1.5574)
 H40C(1.6551) H41A(1.5318) H41B(1.426) H41C(1.3996) H49A(1.2347) H49B(1.217)
 H50A(0.9762) H50B(1.1183) H51(0.9441)
 Fixed Z: H5(0.2567) H12(0.2749) H15(0.1516) H22(0.2359) H25(0.2346)
 H1A(0.3397) H1B(0.4043) H1C(0.3887) H7(0.351) H8AA(0.459) H8AB(0.4663)
 H8BC(0.4661) H8BD(0.4591) H9A(0.5073) H9B(0.474) H10A(0.4048) H10B(0.4068)
 H10C(0.3933) H10D(0.4262) H11(0.3353) H14(0.1123) H17(0.1211) H18A(0.079)
 H18B(0.0702) H18C(0.053) H18D(0.1172) H19A(0.1519) H19B(0.1922) H20A(0.2597)
 H20B(0.193) H20C(0.2358) H20D(0.2346) H21(0.252) H29A(0.0689) H29B(-0.0029)
 H29C(0.0684) H30A(0.032) H30B(-0.0357) H30C(0.025) H31A(0.0434) H31B(-0.031)
 H31C(0.0181) H33A(0.1555) H33B(0.1617) H33C(0.2198) H34A(0.2048) H34B(0.1533)
 H34C(0.1447) H37A(0.1023) H37B(0.1475) H37C(0.1846) H40A(0.2891) H40B(0.3674)
 H40C(0.325) H41A(0.3632) H41B(0.3941) H41C(0.3345) H49A(0.5057) H49B(0.4471)
 H50A(0.1125) H50B(0.1069) H51(0.388)
;