A Simple Synthesis of Alliin and allo-Alliin: X-ray Diffraction Analysis and Determination of Their Absolute Configurations.
Hakamata, Wataru; Koyama, Ryosuke; Tanida, Mizuki; Haga, Tomomi; Hirano, Takako; Akao, Makoto; Kumagai, Hitomi; Nishio, Toshiyuki; Journal of agricultural and food chemistry 63 (2015) 10778–10784; doi:10.1021/acs.jafc.5b05501

data_1540696
_publ_section_title
;
 A Simple Synthesis of Alliin and allo-Alliin: X-ray Diffraction Analysis
 and Determination of Their Absolute Configurations.
;
_journal_issue                   50
_journal_name_full               'Journal of agricultural and food chemistry'
_journal_page_first              10778
_journal_page_last               10784
_journal_paper_doi               10.1021/acs.jafc.5b05501
_journal_volume                  63
_journal_year                    2015
_chemical_formula_sum            'C12 H21 N O5 S'
_chemical_formula_weight         291.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0359(3)
_cell_length_b                   10.9281(4)
_cell_length_c                   15.2645(5)
_cell_measurement_temperature    93.00(10)
_cell_volume                     1507.30(9)
_computing_data_collection
'Bruker Instrument Service V4.2.0 (Bruker AXS Inc., 2014)'
_computing_molecular_graphics    'XSHELL V6.3.1 (Bruker AXS Inc., 2004)'
_computing_publication_material
'Generate Report V2014.1 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 1997)'
_diffrn_ambient_temperature      93.00(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19055
_diffrn_reflns_theta_full        74.59
_diffrn_reflns_theta_max         74.59
_diffrn_reflns_theta_min         4.98
_diffrn_source                   'micro focus sealed tube'
_diffrn_source_type              'INCOATEC I\mS'
_exptl_absorpt_coefficient_mu    2.058
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.256
_refine_ls_abs_structure_details
;
Flack x determined using 1211 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(6)
_refine_ls_extinction_coef       0.0018(4)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3065
_refine_ls_number_restraints     172
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.3306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                2938
_reflns_number_total             3065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jf5b05501_si_001.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 1540696.cif.'
_cod_database_code               1540696