Oligopeptides with Equal Amounts of l- and d-Amino Acids May Prefer a Helix Screw Sense
Yosuke Demizu; Hiroko Yamashita; Norikazu Yamazaki; Yukiko Sato; Mitsunobu Doi; Masakazu Tanaka; Masaaki Kurihara; Journal of Organic Chemistry 78 (2013) 12106–12113; doi:10.1021/jo402133e

data_4028830
_publ_contact_author_email       demizu@nihs.go.jp
_publ_contact_author_fax         +81-3-3707-6950
_publ_contact_author_name        'Yosuke Demizu Ph.D'
_publ_contact_author_phone       +81-3-3700-1141
_publ_section_title
;
 Oligopeptides with Equal Amounts of l- and d-Amino Acids May Prefer a
 Helix Screw Sense
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              12106
_journal_page_last               12113
_journal_paper_doi               10.1021/jo402133e
_journal_volume                  78
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_sum            'C54 H101 N9 O13'
_chemical_formula_weight         1084.44
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.154(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.493(2)
_cell_length_b                   20.119(4)
_cell_length_c                   14.627(3)
_cell_measurement_reflns_used    7065
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.72
_cell_measurement_theta_min      2.25
_cell_volume                     3382.2(11)
_computing_cell_refinement       'SAINTPLUS (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINTPLUS (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Seldrick & Gould, 1996)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker AXS SMART APEX (CCD area detector)'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator
'Bruker AXS Montel (conforcal multilayer optics)'
_diffrn_radiation_source         'MacScience M18XCE (rotating anode)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0914
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15754
_diffrn_reflns_theta_full        22.21
_diffrn_reflns_theta_max         22.21
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 15754
_diffrn_standards_interval_time  780
_diffrn_standards_number         228
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel pairs'
_refine_ls_abs_structure_Flack   4(5)
_refine_ls_extinction_coef       0.024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   2.182
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         4309
_refine_ls_number_restraints     259
_refine_ls_restrained_S_all      2.417
_refine_ls_R_factor_all          0.1210
_refine_ls_R_factor_gt           0.1138
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2691
_refine_ls_wR_factor_ref         0.2709
_reflns_number_gt                3615
_reflns_number_total             4309
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo402133e_si_002.cif
_cod_data_source_block           nine2
_cod_original_cell_volume        3382.1(12)
_cod_database_code               4028830