Extent of Helical Induction Caused by Introducing α-Aminoisobutyric Acid into an Oligovaline Sequence.
Tsuji, Genichiro; Misawa, Takashi; Doi, Mitsunobu; Demizu, Yosuke; ACS omega 3 (2018) 6395–6399; doi:10.1021/acsomega.8b01030

data_4516059
_publ_section_title
;
 Extent of Helical Induction Caused by Introducing \a-Aminoisobutyric Acid
 into an Oligovaline Sequence.
;
_journal_issue                   6
_journal_name_full               'ACS omega'
_journal_page_first              6395
_journal_page_last               6399
_journal_paper_doi               10.1021/acsomega.8b01030
_journal_volume                  3
_journal_year                    2018
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C62 H112 N12 O15, 1.5(C H4 O)'
_chemical_formula_sum            'C63.5 H118 N12 O16.5'
_chemical_formula_weight         1313.70
_chemical_name_systematic
; 
 Boc-(Val-Val-Aib)4-OMe.3MeOH 
;
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_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                88.192(7)
_cell_angle_beta                 87.296(7)
_cell_angle_gamma                79.182(7)
_cell_formula_units_Z            2
_cell_length_a                   10.612(5)
_cell_length_b                   17.232(8)
_cell_length_c                   21.162(10)
_cell_measurement_reflns_used    5291
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.25
_cell_measurement_theta_min      2.14
_cell_volume                     3796(3)
_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 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0824
_diffrn_reflns_av_sigmaI/netI    0.1456
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27123
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        3.20
_diffrn_standards_interval_count 27123
_diffrn_standards_interval_time  360
_diffrn_standards_number         152
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.556402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            0.30
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1430
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.6(16)
_refine_ls_extinction_coef       'Flack (1983), 0 Friedel pairs'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1660
_refine_ls_number_reflns         14000
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_gt           0.0922
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1422P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2264
_refine_ls_wR_factor_ref         0.2515
_reflns_number_gt                7867
_reflns_number_total             14000
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ao8b01030_si_002.cif
_cod_data_source_block           vva1
_cod_depositor_comments
;

2020-08-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      P1
_cod_original_formula_moiety     '2(C62 H112 N12 O15), 3(C H4 O)'
_cod_original_formula_sum        'C127 H236 N24 O33'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     2627.41
_cod_database_code               4516059