Synthesis of new Calpha-tetrasubstituted alpha-amino acids.
Grauer, Andreas A.; König, Burkhard; Beilstein journal of organic chemistry 5 (2009) 5–; doi:10.3762/bjoc.5.5

data_4029747
_publ_section_title
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 Synthesis of new Calpha-tetrasubstituted alpha-amino acids.
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_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              5
_journal_paper_doi               10.3762/bjoc.5.5
_journal_volume                  5
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C15 H27 N O5'
_chemical_formula_sum            'C15 H27 N O5'
_chemical_formula_weight         301.38
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1882(3)
_cell_length_b                   10.6160(4)
_cell_length_c                   16.3593(5)
_cell_measurement_reflns_used    2710
_cell_measurement_temperature    123
_cell_measurement_theta_max      66.6099
_cell_measurement_theta_min      2.6982
_cell_volume                     1769.39(10)
_computing_cell_refinement
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
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_computing_data_reduction
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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 0.967
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
  1 omega  -49.00  -23.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  130.0000   14.0000    0.0000    0.0000 26

  2 omega  -24.00   17.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137 -100.0000   58.0000    0.0000    0.0000 41

  3 omega  -31.00    1.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  100.0000  343.0000    0.0000    0.0000 32

  4 omega  -39.00   14.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137   45.0000   30.0000    0.0000    0.0000 53

  5 omega  -68.00  -15.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   45.0000  150.0000    0.0000    0.0000 53

  6 omega -172.00 -134.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000 -100.0000   58.0000    0.0000    0.0000 38

  7 omega -165.00 -119.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -45.0000   90.0000    0.0000    0.0000 46

  8 omega  115.00  168.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000    0.0000    0.0000    0.0000 53

  9 omega   47.00   83.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000 -100.0000  238.0000    0.0000    0.0000 36

 10 omega   69.00  125.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000    0.0000    0.0000    0.0000 56

 11 omega   60.00  113.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   77.0000  330.0000    0.0000    0.0000 53

 12 omega   15.00   66.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000  120.0000    0.0000    0.0000 51

;
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4695
_diffrn_reflns_reduction_process
;
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_diffrn_reflns_theta_full        66.69
_diffrn_reflns_theta_max         66.69
_diffrn_reflns_theta_min         4.97
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61542
_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            'translucent colourless'
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.0(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2087
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0623
_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^)+(0.1221P)^2^+0.5004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.1896
_reflns_number_gt                1759
_reflns_number_total             2087
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            1860-5397-5-5-S2.cif
_cod_data_source_block           h210
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/Beilstein/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
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_cod_database_code               4029747