4-Methoxybenzaldehyde 4-(2,3,4,6-tetra-<i>O</i>-acetyl-β-<small>D</small>-glucopyranosyl)thiosemicarbazone
Shu-Sheng Zhang; Bo Yang; Ji-Zhi Li; Qing Liu; Xue-Mei Li; Kui Jiao; M. Kassim; Yamin, Bohari. M.; Acta Crystallographica Section E 60 (2004) o2050–o2052; doi:10.1107/S1600536804025589

data_2204568
_publ_section_title
;4-Methoxybenzaldehyde
 4-(2,3,4,6-tetra-<i>O</i>-acetyl-\b-<small>D</small>-glucopyranosyl)thiosemicarbazone
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2050
_journal_page_last               o2052
_journal_paper_doi               10.1107/S1600536804025589
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C23 H29 N3 O10 S'
_chemical_formula_moiety         'C23 H29 N3 O10 S'
_chemical_formula_sum            'C23 H29 N3 O10 S'
_chemical_formula_weight         539.55
_chemical_name_systematic
;
4-Methoxybenzaldehyde
4-(2,3,4,6-tetra-O-acetyl-\b-D-glucopyranosyl)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                   8.7678(5)
_cell_length_b                   17.6042(9)
_cell_length_c                   17.9730(9)
_cell_measurement_reflns_used    6318
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      1.5
_cell_volume                     2774.1(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Siemens 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  0.0777
_diffrn_reflns_av_sigmaI/netI    0.0734
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35973
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         1.62
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.9779
_exptl_absorpt_correction_T_min  0.9597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.195
_refine_ls_abs_structure_details 'Flack (1983), 2757 Friedel pairs'
_refine_ls_abs_structure_Flack   0.14(15)
_refine_ls_extinction_coef       0.0038(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1674
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1011P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1755
_refine_ls_wR_factor_ref         0.2164
_reflns_number_gt                2708
_reflns_number_total             6318
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj6012.cif
_cod_data_source_block           I
_cod_database_code               2204568
_cod_database_fobs_code          2204568