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_4024532
_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         '2(C38 H50 Br2 N4 O9), C2 H5 O'
_chemical_formula_sum            'C39 H52.5 Br2 N4 O9.5'
_chemical_formula_weight         1778.30
_chemical_name_systematic        ?
_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             'Jul 14 12:21:01 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                   10.19490(10)
_cell_length_b                   16.36340(10)
_cell_length_c                   50.9856(4)
_cell_measurement_reflns_used    38028
_cell_measurement_temperature    123
_cell_measurement_theta_max      66.5051
_cell_measurement_theta_min      2.5952
_cell_volume                     8505.58(12)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -22.00   36.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137   77.0000   90.0000    0.0000    0.0000 58

  2 omega  -33.00   16.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137  -45.0000   90.0000    0.0000    0.0000 49

  3 omega    9.00   67.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137   77.0000  240.0000    0.0000    0.0000 58

  4 omega  -16.00   29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137   45.0000   60.0000    0.0000    0.0000 45

  5 omega   17.00   56.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137   45.0000  300.0000    0.0000    0.0000 39

  6 omega   17.00   59.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137   45.0000  210.0000    0.0000    0.0000 42

  7 omega -115.00  -62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -45.0000  240.0000    0.0000    0.0000 53

  8 omega  -69.00  -11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   77.0000   60.0000    0.0000    0.0000 58

  9 omega -118.00  -64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   45.0000   60.0000    0.0000    0.0000 54

 10 omega -116.00  -62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  113.0000   97.0000    0.0000    0.0000 54

 11 omega   69.00  127.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000  210.0000    0.0000    0.0000 58

 12 omega   60.00  118.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   77.0000    0.0000    0.0000    0.0000 58

 13 omega  118.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000    0.0000  270.0000    0.0000    0.0000 60

 14 omega   15.00  127.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000  120.0000    0.0000    0.0000 112

 15 omega   68.00  119.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000    0.0000    0.0000    0.0000 51

 16 omega   76.00  114.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000   60.0000    0.0000    0.0000 38

 17 omega  115.00  168.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000  300.0000    0.0000    0.0000 53

 18 omega   82.00  110.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000    0.0000    0.0000    0.0000 28

 19 omega   69.00  106.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000  300.0000    0.0000    0.0000 37

 20 omega   66.00  118.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000  210.0000    0.0000    0.0000 52

 21 omega   66.00  159.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000  270.0000    0.0000    0.0000 93

 22 omega  107.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000    0.0000   30.0000    0.0000    0.0000 71

;
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            58646
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.63
_diffrn_reflns_theta_max         66.63
_diffrn_reflns_theta_min         2.84
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.889
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79549
_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    1.389
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3684
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.424
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         14747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0390P)^2^+8.2879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                14212
_reflns_number_total             14747
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo900222g_si_007.cif
_cod_data_source_block           h132
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C39 H52.5 B N4 O9.5 R2' to 'C39 H52.5 Br2 N4 O9.5'.

 Antanas Vaitkus,
 2017-01-10

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_original_formula_sum        'C39 H52.50 BR2 N4 O9.50'
_cod_database_code               4024532