3-(4-Methylphenyl)-4-[(thiosemicarbazono)methyl]-1,2,3-oxadiazol-3-ium-5-olate 1,4-dioxane hemisolvate
Abdul Rahiman, M.; Ravikumar, G. N.; Loh, Wan-Sin; Razak, Ibrahim Abdul; Acta Crystallographica Section E 69 (2013) o727–; doi:10.1107/S1600536813008805

data_2237901
_publ_section_title
;
 3-(4-Methylphenyl)-4-[(thiosemicarbazono)methyl]-1,2,3-oxadiazol-3-ium-5-olate
 1,4-dioxane hemisolvate
;
_journal_coeditor_code           IS5258
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o727
_journal_paper_doi               10.1107/S1600536813008805
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C11 H11 N5 O2 S, 0.5C4 H8 O2'
_chemical_formula_moiety         'C11 H11 N5 O2 S, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C13 H15 N5 O3 S'
_chemical_formula_weight         321.36
_chemical_name_common
;
3-(<i>p</i>-Tolyl)-sydnone-4-thiosemicarbazone 1,4-dioxane hemisolvate
;
_chemical_name_systematic
;
3-(4-Methylphenyl)-4-[(thiosemicarbazono)methyl]-1,2,3-oxadiazol-3-ium-5-olate
1,4-dioxane hemisolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.6890(10)
_cell_angle_beta                 87.1680(10)
_cell_angle_gamma                87.4610(10)
_cell_formula_units_Z            2
_cell_length_a                   7.74630(10)
_cell_length_b                   9.37760(10)
_cell_length_c                   10.4449(2)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      32.66
_cell_measurement_theta_min      2.21
_cell_volume                     745.085(19)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
;
Bruker APEXII CCD area-detector
;
_diffrn_measurement_method       '\f and \w scans'
_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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19865
_diffrn_reflns_theta_full        32.66
_diffrn_reflns_theta_max         32.66
_diffrn_reflns_theta_min         1.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_T_max  0.9444
_exptl_absorpt_correction_T_min  0.9214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         5407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.3100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                4782
_reflns_number_total             5407
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is5258.cif
_cod_data_source_block           I
_cod_database_code               2237901
_cod_database_fobs_code          2237901