Twisted Structure of a Cyclic Hexapeptide Containing a Combination of Alternating l-Leu-d-Leu-Aib Segments
Yosuke Demizu; Saori Nagoya; Mitsunobu Doi; Yukiko Sato; Masakazu Tanaka; Masaaki Kurihara; Journal of Organic Chemistry 77 (2012) 9361–9365; doi:10.1021/jo301509c

data_4027591
_publ_section_title
;
 Twisted Structure of a Cyclic Hexapeptide Containing a Combination of
 Alternating l-Leu-d-Leu-Aib Segments
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9361
_journal_page_last               9365
_journal_paper_doi               10.1021/jo301509c
_journal_volume                  77
_journal_year                    2012
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C32 H58 N6 O6, C H4 O'
_chemical_formula_sum            'C33 H62 N6 O7'
_chemical_formula_weight         654.89
_chemical_name_common            cyclo(Leu-D-Leu-Aib)2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.33(3)
_cell_angle_beta                 67.47(3)
_cell_angle_gamma                83.35(3)
_cell_formula_units_Z            2
_cell_length_a                   11.759(2)
_cell_length_b                   13.661(3)
_cell_length_c                   13.815(3)
_cell_measurement_reflns_used    4960
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      22.1
_cell_measurement_theta_min      2.3
_cell_volume                     1963.7(9)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      240(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16743
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 16743
_diffrn_standards_interval_time  480
_diffrn_standards_number         138
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.7773
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.2(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         7947
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1606P)^2^+0.1566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2134
_refine_ls_wR_factor_ref         0.2288
_reflns_number_gt                6209
_reflns_number_total             7947
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo301509c_si_002.cif
_cod_data_source_block           cll
_cod_original_cell_volume        1963.7(7)
_cod_original_sg_symbol_H-M      'P 1 '
_cod_database_code               4027591