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_4024528
_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         'C38 H50 Br2 N4 O9, 2(C H4 O)'
_chemical_formula_sum            'C40 H58 Br2 N4 O11'
_chemical_formula_weight         930.70
_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             'Jan 28 10:59:55 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                   10.14170(10)
_cell_length_b                   16.2309(2)
_cell_length_c                   27.0320(4)
_cell_measurement_reflns_used    9625
_cell_measurement_temperature    123
_cell_measurement_theta_max      62.0428
_cell_measurement_theta_min      3.1688
_cell_volume                     4449.71(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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega   24.00   75.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        2.5071   45.0000  330.0000    0.0000    0.0000 51

  2 omega   -8.00   42.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        2.5071  -95.0000  137.0000    0.0000    0.0000 50

  3 omega   24.00   73.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        2.5071   45.0000  300.0000    0.0000    0.0000 49

  4 omega  -55.00    6.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433    0.0000   60.0000    0.0000    0.0000 61

  5 omega -115.00  -51.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433    0.0000    0.0000    0.0000    0.0000 64

  6 omega  -61.00   -9.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   45.0000   30.0000    0.0000    0.0000 52

  7 omega -162.00 -103.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -77.0000  330.0000    0.0000    0.0000 59

  8 omega -109.00  -56.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -45.0000  270.0000    0.0000    0.0000 53

  9 omega   61.00  118.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933  -77.0000  270.0000    0.0000    0.0000 57

 10 omega   61.00  117.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933  -77.0000    0.0000    0.0000    0.0000 56

 11 omega   15.00   41.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933  -95.0000  292.0000    0.0000    0.0000 26

 12 omega   71.00  107.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933  -77.0000   90.0000    0.0000    0.0000 36

;
_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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            15559
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        62.13
_diffrn_reflns_theta_max         62.13
_diffrn_reflns_theta_min         3.18
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.811
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66536
_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    1.389
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         6662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+1.0079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                6171
_reflns_number_total             6662
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo900222g_si_003.cif
_cod_data_source_block           h007
_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 
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_cod_database_code               4024528