Helical folding of α/β-peptides containing β-amino acids with an eight-membered ring constraint.
Lee, Woohyung; Kwon, Sunmi; Kang, Philjae; Guzei, Ilia A.; Choi, Soo Hyuk; Organic & biomolecular chemistry 12 (2014) 2641–2644; doi:10.1039/c4ob00266k

data_7153711
_publ_section_title
;
 Helical folding of \a/\b-peptides containing \b-amino acids with an
 eight-membered ring constraint.
;
_journal_issue                   17
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2641
_journal_page_last               2644
_journal_paper_doi               10.1039/c4ob00266k
_journal_volume                  12
_journal_year                    2014
_chemical_formula_moiety         'C H Cl3, C21 H37 N3 O6'
_chemical_formula_sum            'C22 H36 Cl3 N3 O6'
_chemical_formula_weight         544.89
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-09-24
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.626(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5371(7)
_cell_length_b                   14.1962(10)
_cell_length_c                   21.2896(15)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    149.9
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.41
_cell_volume                     2856.9(4)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      149.9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0611
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            47046
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         0.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0760 before and 0.0627 after correction.
The Ratio of minimum to maximum transmission is 0.8790.
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    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5661
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+2.5256P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3931
_reflns_number_total             5661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ob00266k2.cif
_cod_data_source_block           mo_moon187_072413_0m
_cod_database_code               7153711
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl34-C31 \\sim Cl35-C31 \\sim Cl32-C31 \\sim Cl33-C31 \\sim Cl36-C31
 with sigma of 0.02
3. Rigid bond restraints
 Cl35, Cl32, Cl33, Cl36, Cl34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl35 \\sim Cl32 \\sim Cl33 \\sim Cl36 \\sim Cl34: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(Cl35) \\sim Ueq, Uanis(Cl32) \\sim Ueq, Uanis(Cl33) \\sim Ueq, Uanis(Cl36) \\sim Ueq, Uanis(Cl34) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Sof(H31a)=Sof(Cl32)=Sof(Cl36)=1-FVAR(1)
 Sof(H31)=Sof(Cl33)=Sof(Cl35)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C31(H31), C31(H31a), C4(H4), C14(H14), C7(H7), C17(H17)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C8(H8a,H8b), C12(H12a,H12b), C9(H9a,H9b), C10(H10a,H10b),
 C11(H11a,H11b)
6.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N15(H15), N18(H18)
6.d Idealised Me refined as rotating group:
 C29(H29a,H29b,H29c), C26(H26a,H26b,H26c), C1(H1a,H1b,H1c), C23(H23a,H23b,
 H23c), C24(H24a,H24b,H24c), C22(H22a,H22b,H22c)
;
_shelxl_version_number           2013-2