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_4036318
_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_formula_moiety         'C70 H128 N12 O15, C3 H7 N O'
_chemical_formula_sum            'C73 H135 N13 O16'
_chemical_formula_weight         1450.94
_chemical_name_systematic
; 
 Boc-(L-Leu-L-Leu-Aib-D-Leu-D-Leu-Aib)2-OMe 
;
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 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            4
_cell_length_a                   10.7793(10)
_cell_length_b                   21.212(2)
_cell_length_c                   38.195(4)
_cell_measurement_reflns_used    9485
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.34
_cell_volume                     8733.3(15)
_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      90
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0808
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            58240
_diffrn_reflns_theta_full        23.82
_diffrn_reflns_theta_max         23.82
_diffrn_reflns_theta_min         1.10
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_count 58240
_diffrn_standards_interval_time  540
_diffrn_standards_number         560
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.5669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colour
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel pairs'
_refine_ls_abs_structure_Flack   -2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.681
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         7414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.681
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0983
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0028P)^2^+2.1320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.1636
_reflns_number_gt                7307
_reflns_number_total             7414
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo5b01541_si_001.cif
_cod_data_source_block           leua6
_cod_original_cell_volume        8733.4(14)
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4036318