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_7153710
_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, C35 H53 N5 O8'
_chemical_formula_sum            'C36 H54 Cl3 N5 O8'
_chemical_formula_weight         791.19
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-01-07
_audit_creation_method
;
  Olex2 1.2-dev
  (compiled Jan  7 2013 12:20:32, GUI svn.r4391)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.635(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.660(2)
_cell_length_b                   10.3977(11)
_cell_length_c                   31.516(2)
_cell_measurement_reflns_used    9234
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.608
_cell_measurement_theta_min      2.837
_cell_volume                     8171.8(13)
_computing_cell_refinement       'SAINT+ Ver. 7.68A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2012.14-3 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT+ Ver. 7.68A'
_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  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2012)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            163431
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         73.277
_diffrn_reflns_theta_min         1.771
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.476
_exptl_absorpt_correction_T_max  0.4654
_exptl_absorpt_correction_T_min  0.3213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0924 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.6904.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.556
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.166
_refine_diff_density_max         1.453
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         16214
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0660P)^2^+13.1250P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14121
_reflns_number_total             16214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ob00266k2.cif
_cod_data_source_block           choi02
_cod_original_cell_volume        8171.6(13)
_cod_database_code               7153710
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H29C,H29D} of C29, H26 of C26, H24 of C24, H31 of C31, H32 of C32, H33 of
  C33, H34 of C34, H35 of C35, H1A of N1A, H2A of N2A, H3A of N3A, H4A of N4A,
  H5A of N5A, H6A of C6A, H9A of C9A, {H10A,H10B} of C10A, H5 of N5, H4 of N4,
  H3 of N3, H2 of N2, H1 of N1, H2SA of C2SA, H2S of C2S, H1S of C1S, {H11A,
  H11B} of C11A, {H12A,H12B} of C12A, {H13A,H13B} of C13A, H14A of C14A, H16A
  of C16A, H19A of C19A, {H20A,H20B} of C20A, {H21A,H21B} of C21A, {H22A,H22B}
  of C22A, {H23A,H23B} of C23A, H24A of C24A, H26A of C26A, {H29A,H29B} of C29A,
   H31A of C31A, H32A of C32A, H33A of C33A, H34A of C34A, H6 of C6, H9 of C9,
  {H10C,H10D} of C10, {H11C,H11D} of C11, {H12C,H12D} of C12, {H13C,H13D} of
  C13, H14 of C14, H16 of C16, H19 of C19, {H20C,H20D} of C20, {H21C,H21D} of
  C21, {H22C,H22D} of C22, {H23C,H23D} of C23, H35A of C35A
 At 1.5 times of:
  {H27D,H27E,H27F} of C27, {H1AA,H1AB,H1AC} of C1A, {H2AA,H2AB,H2AC} of C2A,
  {H3AA,H3AB,H3AC} of C3A, {H7AA,H7AB,H7AC} of C7A, {H2B,H2C,H2D} of C2, {H1B,
  H1C,H1D} of C1, {H17A,H17B,H17C} of C17A, {H27A,H27B,H27C} of C27A, {H3B,H3C,
  H3D} of C3, {H7A,H7B,H7C} of C7, {H17D,H17E,H17F} of C17
2. Restrained distances
 N1-H1 ~ N2-H2 ~ N3-H3 ~ N4-H4 ~ N5-H5 ~ N1A-H1A ~ N2A-H2A ~ N3A-H3A ~ N4A-H4A
 ~ N5A-H5A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2SA) = Uanis(Cl4A) = Uanis(Cl5A) = Uanis(Cl6A)
4. Others
 Sof(Cl4)=Sof(Cl5)=Sof(Cl6)=Sof(C2S)=Sof(H2S)=1-Sof(Cl5)=1-Sof(Cl5)=1-Sof(Cl5)=
 1-Sof(Cl5)=1-Sof(Cl5)
5.a Free rotating group:
 Cl4A(Cl5A,Cl6A,C2SA,H2SA)
5.b Ternary CH refined with riding coordinates:
 C1S(H1S), C2S(H2S), C6(H6), C9(H9), C14(H14), C16(H16), C19(H19), C24(H24),
 C26(H26), C6A(H6A), C9A(H9A), C14A(H14A), C16A(H16A), C19A(H19A), C24A(H24A),
 C26A(H26A)
5.c Secondary CH2 refined with riding coordinates:
 C10(H10C,H10D), C11(H11C,H11D), C12(H12C,H12D), C13(H13C,H13D), C20(H20C,
 H20D), C21(H21C,H21D), C22(H22C,H22D), C23(H23C,H23D), C29(H29C,H29D),
 C10A(H10A,H10B), C11A(H11A,H11B), C12A(H12A,H12B), C13A(H13A,H13B), C20A(H20A,
 H20B), C21A(H21A,H21B), C22A(H22A,H22B), C23A(H23A,H23B), C29A(H29A,H29B)
5.d Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C31A(H31A), C32A(H32A),
 C33A(H33A), C34A(H34A), C35A(H35A)
5.e Idealised Me refined as rotating group:
 C1(H1B,H1C,H1D), C2(H2B,H2C,H2D), C3(H3B,H3C,H3D), C7(H7A,H7B,H7C), C17(H17D,
 H17E,H17F), C27(H27D,H27E,H27F), C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC),
 C3A(H3AA,H3AB,H3AC), C7A(H7AA,H7AB,H7AC), C17A(H17A,H17B,H17C), C27A(H27A,H27B,
 H27C)
;
_shelx_estimated_absorpt_t_max   0.684
_shelx_estimated_absorpt_t_min   0.340
_shelx_res_checksum              87517
_shelxl_version_number           2012-9