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_4024531
_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_absolute_configuration ad
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C22 H31 Br N2 O6'
_chemical_formula_sum            'C22 H31 Br N2 O6'
_chemical_formula_weight         499.39
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_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_date             'Oct 27 11:58:53 2008'
_audit_creation_method           'PLATON <TABLE ACC> option'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.18536(6)
_cell_length_b                   17.91432(12)
_cell_length_c                   21.08060(15)
_cell_measurement_reflns_used    13297
_cell_measurement_temperature    123
_cell_measurement_theta_max      66.4911
_cell_measurement_theta_min      2.4638
_cell_volume                     2335.87(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -35.00   -4.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  107.0000  340.0000    0.0000    0.0000 31

  2 omega   55.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  153.0000   40.0000    0.0000    0.0000 33

  3 omega   -6.00   32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137 -121.0000  119.0000    0.0000    0.0000 38

  4 omega  -90.00  -32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137  -77.0000   30.0000    0.0000    0.0000 58

  5 omega -115.00  -62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -45.0000  240.0000    0.0000    0.0000 53

  6 omega -171.00 -107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -20.0000   10.0000    0.0000    0.0000 64

  7 omega -169.00 -101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000 -107.0000   61.0000    0.0000    0.0000 68

  8 omega -120.00  -65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  121.0000   21.0000    0.0000    0.0000 55

  9 omega  118.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000    0.0000  120.0000    0.0000    0.0000 60

 10 omega   66.00  119.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000  180.0000    0.0000    0.0000 53

 11 omega   69.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000    0.0000    0.0000    0.0000 58

 12 omega   51.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   20.0000  349.0000    0.0000    0.0000 64

 13 omega   66.00  119.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000   60.0000    0.0000    0.0000 53

 14 omega   69.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000  180.0000    0.0000    0.0000 58

 15 omega -178.00   -1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000   30.0000    0.0000    0.0000 177

 16 omega -178.00   -1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000   60.0000    0.0000    0.0000 177

 17 omega -178.00   -1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000  210.0000    0.0000    0.0000 177

 18 omega -178.00 -134.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000  240.0000    0.0000    0.0000 44

;
_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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19627
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.69
_diffrn_reflns_theta_max         66.69
_diffrn_reflns_theta_min         3.24
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.734
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.041(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.6014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                3777
_reflns_number_total             4015
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo900222g_si_006.cif
_cod_data_source_block           h220
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_database_code               4024531