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_4024526
_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         'C22 H31 Br N2 O6'
_chemical_formula_sum            'C22 H31 Br N2 O6'
_chemical_formula_weight         499.39
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Dec 04 13:26:39 2007'
_audit_creation_method           'PLATON <TABLE ACC> option'
_cell_angle_alpha                90
_cell_angle_beta                 106.897(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0217(5)
_cell_length_b                   6.13650(10)
_cell_length_c                   20.6038(5)
_cell_measurement_reflns_used    5801
_cell_measurement_temperature    123
_cell_measurement_theta_max      62.0552
_cell_measurement_theta_min      2.2426
_cell_volume                     2301.19(10)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -35.00   23.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       -1.2571   75.0000    0.0000    0.0000    0.0000 58

  2 omega   21.00   74.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       -1.2571   45.0000    0.0000    0.0000    0.0000 53

  3 omega  -25.00   28.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        2.5071   45.0000  120.0000    0.0000    0.0000 53

  4 omega  -72.00  -19.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        2.5071  -45.0000  240.0000    0.0000    0.0000 53

  5 omega    6.00   51.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        2.5071 -110.0000  335.0000    0.0000    0.0000 45

  6 omega -115.00  -59.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   75.0000  120.0000    0.0000    0.0000 56

  7 omega  -61.00   -6.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   75.0000    0.0000    0.0000    0.0000 55

  8 omega  -60.00   -9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   45.0000    0.0000    0.0000    0.0000 51

  9 omega  -60.00   -9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   45.0000  240.0000    0.0000    0.0000 51

 10 omega -106.00  -51.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -75.0000  120.0000    0.0000    0.0000 55

 11 omega -114.00  -56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  106.0000   78.0000    0.0000    0.0000 58

 12 omega -110.00  -58.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   45.0000    0.0000    0.0000    0.0000 52

 13 omega -115.00  -59.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   75.0000    0.0000    0.0000    0.0000 56

 14 omega -119.00  -64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  119.0000   83.0000    0.0000    0.0000 55

 15 omega -158.00 -106.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -40.0000   34.0000    0.0000    0.0000 52

 16 omega -107.00  -53.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -59.0000  141.0000    0.0000    0.0000 54

 17 omega -112.00  -57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  105.0000  220.0000    0.0000    0.0000 55

 18 omega -108.00  -57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -40.0000   34.0000    0.0000    0.0000 51

 19 phi     -2.00   62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   84.3933    0.0000     -        0.0000    0.0000 64

 20 omega  126.00  157.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   45.0000  120.0000    0.0000    0.0000 31

 21 omega   30.00   60.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933  -45.0000    0.0000    0.0000    0.0000 30

 22 omega   81.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   45.0000  240.0000    0.0000    0.0000 28

 23 omega  107.00  160.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   38.0000  -17.0000    0.0000    0.0000 53

 24 omega  110.00  138.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   43.0000  230.0000    0.0000    0.0000 28

;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7262
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        62.28
_diffrn_reflns_theta_max         62.28
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3078
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0972P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                2855
_reflns_number_total             3078
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo900222g_si_001.cif
_cod_data_source_block           g255
_cod_depositor_comments
;
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      'C 2'
_cod_database_code               4024526