An intermediate in a new synthesis approach to β-substituted β-hydroxyaspartame
Johny Wehbe; Valérie Rolland; Jean Martinez; Marc Rolland; Acta Crystallographica Section C 59 (2003) o473–o475; doi:10.1107/S0108270103014057

data_2013416
_publ_section_title
;
 An intermediate in a new synthesis approach to \b-substituted
 \b-hydroxyaspartame
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o473
_journal_page_last               o475
_journal_paper_doi               10.1107/S0108270103014057
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C21 H34 Br N O6'
_chemical_formula_moiety         'C21 H34 Br N O6'
_chemical_formula_sum            'C21 H34 Br N O6'
_chemical_formula_weight         476.39
_chemical_name_systematic
;
(2'R,3'R,5'R,2S,3S)-3-bromomethyl-3-hydroxy-2-[(2'-hydroxy-2',6',6'-
trimethylbicyclo[3.1.1]hept-3'-ylidene)amino]succinic acid
;
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 118.031(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.546(2)
_cell_length_b                   10.321(3)
_cell_length_c                   11.594(4)
_cell_measurement_reflns_used    24309
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.58
_cell_measurement_theta_min      3.52
_cell_volume                     1219.5(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Software (Nonius, 1997)'
_computing_data_reduction
'Denzo (Otwinowski & Minor, 1997) and Scalepack'
_computing_molecular_graphics    'OrtepII (Johnson, 1976), Platon (Spek, 2001)'
_computing_publication_material  'MaXus (Mackay et al., 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Nonius KappaCCD area-detector'
_diffrn_measurement_method       \f-scan
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24309
_diffrn_reflns_theta_full        28.58
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         3.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.718
_exptl_absorpt_correction_T_max  0.709
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.574
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2981
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0432P)^2^+0.5864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                2981
_reflns_number_total             3231
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn1023.cif
_cod_data_source_block           IIb
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1219.6(6)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2013416
_cod_database_fobs_code          2013416