Diastereoselective synthesis of quaternary alpha-amino acids from diketopiperazine templates.
Davies, Stephen G.; Garner, A. Christopher; Ouzman, Jaqueline V. A.; Roberts, Paul M.; Smith, Andrew D.; Snow, Emma J.; Thomson, James E.; Tamayo, Juan A.; Vickers, Richard J.; Organic & biomolecular chemistry 5 (2007) 2138–2147; doi:10.1039/b704475e

data_7151123
_publ_section_title
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 Diastereoselective synthesis of quaternary alpha-amino acids from
 diketopiperazine templates.
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_journal_issue                   13
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2138
_journal_page_last               2147
_journal_paper_doi               10.1039/b704475e
_journal_volume                  5
_journal_year                    2007
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C31 H43 N3 O7'
_chemical_formula_sum            'C31 H43 N3 O7'
_chemical_formula_weight         569.70
_chemical_melting_point          ?
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4150(1)
_cell_length_b                   33.8450(4)
_cell_length_c                   9.5680(2)
_cell_measurement_reflns_used    5411
_cell_measurement_temperature    190
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3048.85(8)
_computing_cell_refinement
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
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_computing_data_collection
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COLLECT (Nonius BV, 1997)
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_computing_data_reduction
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
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_computing_molecular_graphics
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CAMERON (Watkin et al 1996)
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_computing_publication_material
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CRYSTALS (Watkin et al 2001)
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_computing_structure_refinement
;
CRYSTALS (Watkin et al 2001)
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_computing_structure_solution
;
USER DEFINED STRUCTURE SOLUTION
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_diffrn_ambient_temperature      190
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type
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Enraf Nonius Kappa CCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10838
_diffrn_reflns_theta_full        22.939
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         5.110
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1224.000
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.33
_refine_ls_extinction_coef       1073.3(2290)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   0.9600
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         3329
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.000159
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994)
W = [weight] * [1-(deltaF/6*sigmaF)^2]^2

1.87 0.953 1.33
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0845
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0722
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              43
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                3329
_reflns_number_total             3860
_reflns_threshold_expression     I>1.00u(I)
_cod_data_source_file            b704475e.txt
_cod_data_source_block           2
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               7151123