Preparation and X-ray analysis of potassium (2,3-dichlorophenyl)glucosinolate
Vo, Quan V.; Trenerry, Craige; Rochfort, Simone; White, Jonathan; Hughes, Andrew B.; Acta Crystallographica Section C 70 (2014) 588–594; doi:10.1107/S2053229614009115

data_2019550
_publ_section_title
;
 Preparation and X-ray analysis of potassium
 (2,3-dichlorophenyl)glucosinolate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              588
_journal_page_last               594
_journal_paper_doi               10.1107/S2053229614009115
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C21 H23 Cl2 N O10 S'
_chemical_formula_moiety         'C21 H23 Cl2 N O10 S'
_chemical_formula_sum            'C21 H23 Cl2 N O10 S'
_chemical_formula_weight         552.36
_chemical_name_systematic
;
<i>S</i>-(2,3,4,6-Tetra-<i>O</i>-acetyl-\a-<i>D</i>-glucopyranosyl)-2,3-\
dichlorophenylacetothiohydroxymate
;
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.786(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.1967(2)
_cell_length_b                   15.1383(4)
_cell_length_c                   11.9441(3)
_cell_measurement_reflns_used    3604
_cell_measurement_temperature    130.0
_cell_measurement_theta_max      29.2036
_cell_measurement_theta_min      2.8966
_cell_volume                     1268.99(6)
_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova (Dual, Cu at zero, Atlas)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6348
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.3706
_exptl_crystal_size_mid          0.3152
_exptl_crystal_size_min          0.1400
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.187
_refine_ls_abs_structure_details 'Flack (1983), <b>???? Friedel pairs</b>'
_refine_ls_abs_structure_Flack   -0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         3790
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+0.0094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0692
_reflns_number_gt                3535
_reflns_number_total             3790
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            sf3222sup1.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 2019550--2019551.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2019550
_cod_database_fobs_code          2019550