Probing the Role of the C-H...O Hydrogen Bond Stabilized Polypeptide Chain Reversal at the C-terminus of Designed Peptide Helices. Structural Characterization of Three Decapeptides
Subrayashastry Aravinda; Narayanaswamy Shamala; Abhishek Bandyopadhyay; Padmanabhan Balaram; Journal of the American Chemical Society 125 (2003) 15065–15075; doi:10.1021/ja0372762

data_4114462
_publ_section_title
;
 Probing the Role of the C-H...O Hydrogen Bond Stabilized Polypeptide
 Chain Reversal at the C-terminus of Designed Peptide Helices. Structural
 Characterization of Three Decapeptides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15065
_journal_page_last               15075
_journal_paper_doi               10.1021/ja0372762
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C53 H96 N10 O13 * H2O'
_chemical_formula_sum            'C53 H98 N10 O14'
_chemical_formula_weight         1099.40
_chemical_name_common
;
Boc-Leu-Aib-Val-Aib-Leu-Aib-Val-D-Ala-D-Leu-Aib-OMe
;
_chemical_name_systematic
; 
 t-Butyloxycarbonyl-leucyl-(alpha-aminoisobutyryl)-valyl-(alpha-aminoisobutyryl)
 -leucyl-(alpha-aminoisobutyryl)-valyl-D-alanyl-D-leucyl-(alpha-aminoisobutyryl)
 methyl ester monohydrate
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.185(6)
_cell_length_b                   30.163(8)
_cell_length_c                   25.969(10)
_cell_measurement_temperature    293(2)
_cell_volume                     15811(9)
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXD (Sheldrick and Schneider, 2001)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean NA
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER AXS SMART APEX CCD with Mo source'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1194
_diffrn_reflns_av_sigmaI/netI    0.1759
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            48890
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.067
_exptl_crystal_colour            'colour less'
_exptl_crystal_density_diffrn    0.922
_exptl_crystal_description       'thin plates'
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    'riding on C or N to which bonded'
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     684
_refine_ls_number_reflns         11301
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.513
_refine_ls_R_factor_all          0.2156
_refine_ls_R_factor_gt           0.1064
_refine_ls_shift/su_max          5.555
_refine_ls_shift/su_mean         0.530
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1854
_refine_ls_wR_factor_ref         0.2346
_reflns_number_gt                4967
_reflns_number_total             11301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0372762si20030715_034742_3.cif
_cod_data_source_block           lud-10
_cod_database_code               4114462