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_7151439
_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_compound_source
;
?
;
_chemical_formula_moiety         ' C31 H34 N2 O4 '
_chemical_formula_sum            'C31 H34 N2 O4'
_chemical_formula_weight         498.62
_chemical_melting_point          ?
_chemical_name_systematic
;                                                                               
(1S,3R,6S)-4,7-bis(4-methoxybenzyl)-6-isopropyl-1-phenyl-4,7-diaza-
spiro[2.5]octane-5,8-dione

;
_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             02-27-05
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 96.237(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4793(2)
_cell_length_b                   10.5310(3)
_cell_length_c                   12.0380(4)
_cell_measurement_reflns_used    3043
_cell_measurement_temperature    190
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     1320.62(6)
_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      190
_diffrn_measured_fraction_theta_max 1.000
_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  0.02
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5859
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.34
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.99
_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    1.254
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             532.234
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0366
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         2613
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.000202
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method= Tukey and Prince 
W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 

0.505 0.250 0.185 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0496
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                2613
_reflns_number_total             3196
_reflns_threshold_expression     >1.00\s(I)
_cod_data_source_file            b303348a.txt
_cod_data_source_block           CRYSTALS_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 

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 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        ' C31 H34 N2 O4 '
_cod_database_code               7151439