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_4024527
_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           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             'Dec 04 13:50:20 2007'
_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                   6.1755(3)
_cell_length_b                   12.6779(6)
_cell_length_c                   30.4159(11)
_cell_measurement_reflns_used    3011
_cell_measurement_temperature    123
_cell_measurement_theta_max      62.0573
_cell_measurement_theta_min      3.4859
_cell_volume                     2381.33(18)
_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 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
  1 omega  -25.00   32.00   1.0000    2.6000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       -1.2571  -75.0000    0.0000    0.0000    0.0000 57

  2 omega  -41.00    1.00   1.0000    2.6000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        2.5071  102.0000 -122.0000    0.0000    0.0000 42

  3 omega  -72.00  -19.00   1.0000    2.6000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        2.5071  -45.0000  120.0000    0.0000    0.0000 53

  4 omega -115.00  -58.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   75.0000    0.0000    0.0000    0.0000 57

  5 omega -107.00  -54.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -54.0000   49.0000    0.0000    0.0000 53

  6 omega  -61.00   -8.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   45.0000  240.0000    0.0000    0.0000 53

  7 omega -107.00  -53.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -61.0000  355.0000    0.0000    0.0000 54

  8 omega -112.00  -59.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   57.0000  146.0000    0.0000    0.0000 53

  9 omega    3.00   47.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933 -102.0000  133.0000    0.0000    0.0000 44

 10 omega  107.00  142.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   45.0000  240.0000    0.0000    0.0000 35

 11 omega  106.00  159.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   45.0000  120.0000    0.0000    0.0000 53

 12 omega  105.00  162.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   75.0000    0.0000    0.0000    0.0000 57

;
_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  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            7259
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        62.35
_diffrn_reflns_theta_max         62.35
_diffrn_reflns_theta_min         3.78
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.682
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50429
_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    1.393
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.556
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0708
_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^)+(0.1202P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.1928
_reflns_number_gt                2402
_reflns_number_total             3553
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo900222g_si_002.cif
_cod_data_source_block           g250
_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               4024527