Topological Study of the Structures of Heterochiral Peptides Containing Equal Amounts of l-Leu and d-Leu.
Demizu, Yosuke; Yamashita, Hiroko; Doi, Mitsunobu; Misawa, Takashi; Oba, Makoto; Tanaka, Masakazu; Kurihara, Masaaki; The Journal of organic chemistry 80 (2015) 8597–8603; doi:10.1021/acs.joc.5b01541

data_4036319
_publ_section_title
;
 Topological Study of the Structures of Heterochiral Peptides Containing
 Equal Amounts of l-Leu and d-Leu.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8597
_journal_page_last               8603
_journal_paper_doi               10.1021/acs.joc.5b01541
_journal_volume                  80
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C70 H128 N12 O15, C4 H8 O '
_chemical_formula_sum            'C74 H136 N12 O16'
_chemical_formula_weight         1449.95
_chemical_name_systematic
; 
 Boc-Leu-Leu-Aib-(DLeu-Leu-Aib)2-OMe.butanone 
;
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclininc
_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                90.109(2)
_cell_angle_beta                 90.496(2)
_cell_angle_gamma                101.438(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7549(13)
_cell_length_b                   14.0615(17)
_cell_length_c                   14.0682(17)
_cell_measurement_reflns_used    8910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.19
_cell_volume                     2085.2(4)
_computing_cell_refinement       'SAINT-PLUS (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT-PLUS (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD (Bruker APEX)'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'conforcal (Bruker Montel)'
_diffrn_radiation_source         'rotating anode (M18XCE)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18249
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        2.84
_diffrn_standards_interval_count 18249
_diffrn_standards_interval_time  360
_diffrn_standards_number         245
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.7878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel pairs'
_refine_ls_abs_structure_Flack   0.1(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         9006
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.3708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                8447
_reflns_number_total             9006
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo5b01541_si_002.cif
_cod_data_source_block           dda
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4036319