Asymmetric synthesis of substituted 1-aminocyclopropane-1-carboxylic acids via diketopiperazine methodology
Elena Buñuel; Steven D. Bull; Stephen G. Davies; A. Christopher Garner; Edward D. Savory; Andrew D. Smith; Richard J. Vickers; David J. Watkin; Org. Biomol. Chem. 1 (2003) 2531–2542; doi:10.1039/b303348a

data_7151438
_publ_section_title
;
 Asymmetric synthesis of substituted 1-aminocyclopropane-1-carboxylic
 acids via diketopiperazine methodology
;
_journal_issue                   14
_journal_name_full               'Org. Biomol. Chem.'
_journal_page_first              2531
_journal_page_last               2542
_journal_paper_doi               10.1039/b303348a
_journal_volume                  1
_journal_year                    2003
_chemical_absolute_configuration unk
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C27 H20 N2 O4 '
_chemical_formula_sum            'C27 H20 N2 O4'
_chemical_formula_weight         436.47
_chemical_name_systematic
;                                                                               
?                                                                               
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             02-18-11
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 99.9280(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2515(1)
_cell_length_b                   28.6084(4)
_cell_length_c                   9.4481(1)
_cell_measurement_reflns_used    5605
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2463.19(5)
_computing_cell_refinement
; 
Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_molecular_graphics
; 
CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
CRYSTALS (Watkin et al 2001) 
;
_computing_structure_refinement
; 
CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution
; 
SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
; 
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  0.01
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10759
_diffrn_reflns_theta_full        27.331
_diffrn_reflns_theta_max         27.468
_diffrn_reflns_theta_min         5.138
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             912.000
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.23
_refine_ls_extinction_coef       369.459
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   0.9234
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         5686
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.014797
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method = SHELXL 97 (Sheldrick, 1997) 
W = q / [Sigma^2(F*)+(P(1)p)^2+P(2)p+P(4)+P(5)Sin(theta) ] 

0.844E-01 0.663 0.00 0.00 0.00 0.333 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1407
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1407
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                5686
_reflns_number_total             5686
_reflns_threshold_expression     I>-3.00u(I)
_cod_data_source_file            b303348a.txt
_cod_data_source_block           es59d_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/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 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        ' C27 H20 N2 O4 '
_cod_database_code               7151438