Stable Right- and Left-Handed Peptide Helices containing Cα-Tetrasubstituted α-Amino Acids
Andreas A. Grauer; Chiara Cabrele; Manfred Zabel; Burkhard König; Journal of Organic Chemistry 74 (2009) 3718–3726; doi:10.1021/jo900222g

data_4024529
_publ_section_title
;
Stable Right- and Left-Handed Peptide Helices containing
C\a-Tetrasubstituted \a-Amino Acids
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3718
_journal_page_last               3726
_journal_paper_doi               10.1021/jo900222g
_journal_volume                  74
_journal_year                    2009
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C54 H69 Br3 N6 O12'
_chemical_formula_sum            'C108 H138 Br6 N12 O24'
_chemical_formula_weight         1233.86
_chemical_name_systematic        ?
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_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_date             'Sep 30 09:36:52 2008'
_audit_creation_method           'PLATON <TABLE ACC> option'
_cell_angle_alpha                90
_cell_angle_beta                 104.3050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.51660(10)
_cell_length_b                   28.6529(2)
_cell_length_c                   15.38410(10)
_cell_measurement_reflns_used    32078
_cell_measurement_temperature    123
_cell_measurement_theta_max      66.4963
_cell_measurement_theta_min      2.9557
_cell_volume                     6200.50(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
;
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega  -63.00  -12.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  -45.0000   30.0000    0.0000    0.0000 51

  2 omega  -13.00   39.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  -45.0000  180.0000    0.0000    0.0000 52

  3 omega  -14.00   39.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  -45.0000  270.0000    0.0000    0.0000 53

  4 omega  -16.00   35.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137   45.0000  300.0000    0.0000    0.0000 51

  5 omega   28.00   64.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137 -117.0000   72.0000    0.0000    0.0000 36

  6 omega   20.00   58.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137 -161.0000  228.0000    0.0000    0.0000 38

  7 omega  -41.00  -15.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  117.0000  107.0000    0.0000    0.0000 26

  8 omega  -61.00  -11.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  -45.0000  330.0000    0.0000    0.0000 50

  9 omega -115.00  -62.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -45.0000   30.0000    0.0000    0.0000 53

 10 omega  -62.00   -1.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000  180.0000    0.0000    0.0000 61

 11 omega -163.00 -114.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000 -161.0000  228.0000    0.0000    0.0000 49

 12 omega -115.00  -62.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -45.0000  210.0000    0.0000    0.0000 53

 13 omega -141.00  -89.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  161.0000   78.0000    0.0000    0.0000 52

 14 omega -160.00  -70.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000 -161.0000  101.0000    0.0000    0.0000 90

 15 omega -141.00  -89.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  161.0000  311.0000    0.0000    0.0000 52

 16 omega   60.00  118.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   77.0000   60.0000    0.0000    0.0000 58

 17 omega    5.00   64.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000    0.0000   30.0000    0.0000    0.0000 59

 18 omega   19.00  120.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000  330.0000    0.0000    0.0000 101

 19 omega   94.00  127.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000    0.0000    0.0000    0.0000 33

 20 omega   20.00   70.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000 -161.0000   48.0000    0.0000    0.0000 50

 21 omega   60.00  109.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   77.0000   30.0000    0.0000    0.0000 49

 22 omega   15.00   72.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000  180.0000    0.0000    0.0000 57

 23 omega  115.00  168.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000    0.0000    0.0000    0.0000 53

 24 omega   68.00  116.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000  210.0000    0.0000    0.0000 48

 25 omega   96.00  125.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  161.0000  258.0000    0.0000    0.0000 29

 26 omega  115.00  154.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000   60.0000    0.0000    0.0000 39

 27 omega  125.00  166.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000  180.0000    0.0000    0.0000 41

 28 omega   68.00  117.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000   30.0000    0.0000    0.0000 49

 29 omega   60.00   86.00   1.0000    7.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000 -117.0000   20.0000    0.0000    0.0000 26

;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            52330
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.69
_diffrn_reflns_theta_max         66.69
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.902
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent, colourless'
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_refine_diff_density_max         2.494
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.058(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1352
_refine_ls_number_reflns         21037
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+7.0558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1488
_reflns_number_gt                19220
_reflns_number_total             21037
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo900222g_si_004.cif
_cod_data_source_block           h184w
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C108 H138 B N12 O24 R6' to 'C108 H138 Br6 N12 O24'.

 Antanas Vaitkus,
 2017-01-10

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C108 H138 BR6 N12 O24'
_cod_database_code               4024529