Crystal structure of a new monoclinic polymorph of 2,4-dihydroxybenzaldehyde 4-methylthiosemicarbazone
Salam, M. A.; Hussein, Mouayed A.; Tiekink, Edward R. T.; Acta Crystallographica Section E 71 (2015) 58–61; doi:10.1107/S2056989014026498

data_2240271
_publ_section_title
;
 Crystal structure of a new monoclinic polymorph of
 2,4-dihydroxybenzaldehyde 4-methylthiosemicarbazone
;
_journal_coeditor_code           SU5033
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              58
_journal_page_last               61
_journal_paper_doi               10.1107/S2056989014026498
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C9 H11 N3 O2 S'
_chemical_formula_moiety         'C9 H11 N3 O2 S'
_chemical_formula_sum            'C9 H11 N3 O2 S'
_chemical_formula_weight         225.27
_chemical_name_systematic
;
2,4-Dihydroxybenzaldehyde 4-methylthiosemicarbazone
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.100(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3058(2)
_cell_length_b                   6.05820(10)
_cell_length_c                   22.6041(6)
_cell_measurement_reflns_used    3917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.84
_cell_measurement_theta_min      3.29
_cell_volume                     1000.27(4)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012), <i>QMol</i> (Gans & Shalloway,
2001)
and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2008), PLATON (Spek, 2009 and publCIF
(Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9696
_diffrn_reflns_theta_full        27.495
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         1.802
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  0.9569
_exptl_absorpt_correction_T_min  0.8659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.314
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0336P)^2^+0.7405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                1950
_reflns_number_total             2302
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su5033sup1.cif
_cod_data_source_block           I
_cod_database_code               2240271
_cod_database_fobs_code          2240271
_shelx_estimated_absorpt_t_min   0.867
_shelx_estimated_absorpt_t_max   0.958
_shelx_hkl_checksum              46439
_shelx_res_checksum              75892