A monoclinic polymorph of (1<i>E</i>,5<i>E</i>)-1,5-bis(2-hydroxybenzylidene)thiocarbonohydrazide
Schmitt, Bonell; Gerber, Thomas; Hosten, Eric; Betz, Richard; Acta Crystallographica Section E 67 (2011) o2206–o2207; doi:10.1107/S1600536811030340

data_2231186
_publ_section_title
;
 A monoclinic polymorph of
 (1<i>E</i>,5<i>E</i>)-1,5-bis(2-hydroxybenzylidene)thiocarbonohydrazide
;
_journal_coeditor_code           KJ2182
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2206
_journal_page_last               o2207
_journal_paper_doi               10.1107/S1600536811030340
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C15 H14 N4 O2 S'
_chemical_formula_moiety         'C15 H14 N4 O2 S'
_chemical_formula_sum            'C15 H14 N4 O2 S'
_chemical_formula_weight         314.36
_chemical_name_systematic
;
(1<i>E</i>,5<i>E</i>)-1,5-bis(2-hydroxybenzylidene)thiocarbonohydrazide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 91.2250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.60200(10)
_cell_length_b                   7.4260(2)
_cell_length_c                   34.5220(8)
_cell_measurement_reflns_used    3781
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      3.27
_cell_volume                     1435.80(6)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            13304
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0484
_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^+0.6828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                2830
_reflns_number_total             3578
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kj2182.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2231186
_cod_database_fobs_code          2231186