Crystal structure of 3-methylpyridine-2-carbaldehyde 4-methylthiosemicarbazone monohydrate
Mokhtaruddin, Nur Shuhada Mohd; Ravoof, Thahira Begum S. A.; Tahir, Mohamed Ibrahim Mohamed; Tiekink, Edward R. T.; Acta Crystallographica Section E 71 (2015) o253–o254; doi:10.1107/S2056989015005034

data_2240523
_publ_section_title
;
 Crystal structure of 3-methylpyridine-2-carbaldehyde
 4-methylthiosemicarbazone monohydrate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o253
_journal_page_last               o254
_journal_paper_doi               10.1107/S2056989015005034
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C9 H12 N4 S, H2 O'
_chemical_formula_moiety         'C9 H12 N4 S, H2 O'
_chemical_formula_sum            'C9 H14 N4 O S'
_chemical_formula_weight         226.30
_chemical_name_systematic
;
3-Methyl-1-{(<i>E</i>)-[(3-methylpyridin-2-yl)methylidene]amino}thiourea
monohydrate
;
_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                 102.816(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4493(3)
_cell_length_b                   13.6989(3)
_cell_length_c                   8.0235(3)
_cell_measurement_reflns_used    7855
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.2334
_cell_measurement_theta_min      3.2234
_cell_volume                     1119.90(6)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2011)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg,
2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2015)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1952
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Xcaliber Eos Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14591
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         71.374
_diffrn_reflns_theta_min         4.339
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2011)
;
_exptl_crystal_colour            pale-brown
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       prism
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.254
_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     150
_refine_ls_number_reflns         2160
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0657P)^2^+0.3425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                2044
_reflns_number_total             2160
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7381sup1.cif
_cod_data_source_block           I
_cod_database_code               2240523
_cod_database_fobs_code          2240523
_shelx_estimated_absorpt_t_min   0.530
_shelx_estimated_absorpt_t_max   0.794
_shelx_hkl_checksum              93942
_shelx_res_checksum              62032