Benzaldehyde 1-(2,3,4-tri-<i>O</i>-acetyl-β-<small>D</small>-xylopyranosyl)thiosemicarbazone
Bo Yang; Shu-Sheng Zhang; Yan-Fang Wang; Xue-Mei Li; Kui Jiao; M. Kassim; Yamin, Bohari M.; Acta Crystallographica Section E 60 (2004) o1902–o1904; doi:10.1107/S1600536804023542

data_2204316
_publ_section_title
;Benzaldehyde
 1-(2,3,4-tri-<i>O</i>-acetyl-\b-<small>D</small>-xylopyranosyl)thiosemicarbazone
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1902
_journal_page_last               o1904
_journal_paper_doi               10.1107/S1600536804023542
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C19 H23 N3 O7 S'
_chemical_formula_moiety         'C19 H23 N3 O7 S'
_chemical_formula_sum            'C19 H23 N3 O7 S'
_chemical_formula_weight         437.46
_chemical_name_systematic
;
Benzaldehyde 1-(2,3,4-tri-O-acetyl-\b-D-xylopyranosyl)thiosemicarbazone
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8789(9)
_cell_length_b                   12.6890(13)
_cell_length_c                   19.506(2)
_cell_measurement_reflns_used    3603
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.5
_cell_volume                     2197.6(4)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990)
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Simens SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8924
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.9573
_exptl_absorpt_correction_T_min  0.9138
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.179
_refine_ls_abs_structure_details 'Flack (1983), 1652 Friedel pairs [CHECK?]'
_refine_ls_abs_structure_Flack   0.05(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0459P)^2^+0.3313P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                3603
_reflns_number_total             3873
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv6371.cif
_cod_data_source_block           I
_cod_database_code               2204316
_cod_database_fobs_code          2204316