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_7153709
_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         'C18 H26 F3 N3 O5, H2 O'
_chemical_formula_sum            'C18 H28 F3 N3 O6'
_chemical_formula_weight         439.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.020(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5956(13)
_cell_length_b                   7.1768(4)
_cell_length_c                   18.6281(12)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    137.6
_cell_measurement_theta_max      27.088
_cell_measurement_theta_min      2.534
_cell_volume                     2148.7(3)
_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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation (2013)'
_diffrn_ambient_temperature      137.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_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  0.0281
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30981
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         2.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1225 before and 0.0552 after correction.
The Ratio of minimum to maximum transmission is 0.8916.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.158
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 1757 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.25(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4578
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0234P)^2^+1.3913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    0.934
_reflns_Friedel_fraction_max     0.923
_reflns_number_gt                4240
_reflns_number_total             4578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ob00266k2.cif
_cod_data_source_block           mo_moon122_0ma
_cod_original_cell_volume        2148.7(2)
_cod_database_code               7153709
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H15(0.024) H18(0.028) H5(0.028) H28A(0.045) H28B(0.045)
 H28C(0.045) H10(0.037) H9A(0.038) H9B(0.038) H17(0.027) H13A(0.031)
 H13B(0.031) H11(0.039) H14(0.025) H8A(0.036) H8B(0.036) H7(0.025) H4(0.03)
 H12A(0.038) H12B(0.038) H1A(0.074) H1B(0.074) H1C(0.074) H25A(0.051)
 H25B(0.051) H25C(0.051)
 Fixed X: H15(-0.3693) H18(-0.5765) H5(-0.341) H28A(-0.5135) H28B(-0.5877)
 H28C(-0.5023) H10(-0.0995) H9A(-0.1763) H9B(-0.0787) H17(-0.5023) H13A(-
 0.2485) H13B(-0.2232) H11(-0.0964) H14(-0.2512) H8A(-0.1253) H8B(-0.0946) H7(-
 0.262) H4(-0.2614) H12A(-0.0936) H12B(-0.1058) H1A(-0.1676) H1B(-0.259) H1C(-
 0.1886) H25A(-0.4258) H25B(-0.4046) H25C(-0.3903)
 Fixed Y: H15(-0.0019) H18(-0.4207) H5(-0.1406) H28A(-0.3509) H28B(-0.2132)
 H28C(-0.1306) H10(-0.3906) H9A(-0.5047) H9B(-0.5167) H17(-0.0886) H13A(0.0952)
 H13B(0.1306) H11(-0.098) H14(-0.229) H8A(-0.4134) H8B(-0.2248) H7(-0.3452) H4(-
 0.0336) H12A(-0.0035) H12B(0.1385) H1A(0.4984) H1B(0.5626) H1C(0.5299)
 H25A(0.0736) H25B(-0.1066) H25C(0.0973)
 Fixed Z: H15(-0.6921) H18(-0.7868) H5(-0.8149) H28A(-0.639) H28B(-0.6891)
 H28C(-0.6257) H10(-0.4488) H9A(-0.5787) H9B(-0.5549) H17(-0.7506) H13A(-0.567)
 H13B(-0.6392) H11(-0.4299) H14(-0.5895) H8A(-0.6781) H8B(-0.6291) H7(-0.7134)
 H4(-0.9031) H12A(-0.5733) H12B(-0.5127) H1A(-0.8302) H1B(-0.889) H1C(-0.9214)
 H25A(-0.9229) H25B(-0.962) H25C(-0.989)
;