Crystal structure of a 1,1,2,2-tetrachloroethane-solvated hydrazinecarbothioamide compound
Riyadh, Sayed; Hughes, David L.; Said, Musa A.; Acta Crystallographica Section E Crystallographic Communications 73 (2017) 1271–; doi:10.1107/S2056989017010830

data_2020839
_publ_section_title
;
 Crystal structure of a 1,1,2,2-tetrachloroethane-solvated
 hydrazinecarbothioamide compound
;
_journal_coeditor_code           HB7686
_journal_issue                   9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1271
_journal_paper_doi               10.1107/S2056989017010830
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C15 H15 N5 O2 S, C2 H2 Cl4'
_chemical_formula_moiety         'C15 H15 N5 O2 S, C2 H2 Cl4'
_chemical_formula_structural
'2-O,4-OH-C6H3-N=NH-C6H4c(Me)=NNHC(=O)NH2, C2H2Cl4'
_chemical_formula_sum            'C17 H17 Cl4 N5 O2 S'
_chemical_formula_weight         497.21
_chemical_name_systematic
;
[(1-{4-[2-(2,4-Dihydroxyphenyl)diazen-1-yl]phenyl}ethylidene)amino]thiourea
1,1,2,2-tetrachloroethane monosolvate
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.563(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9124(2)
_cell_length_b                   17.6155(5)
_cell_length_c                   20.3351(6)
_cell_measurement_reflns_used    5694
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.73
_cell_measurement_theta_min      3.54
_cell_volume                     2104.02(11)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
ORTEP (Johnson, 1976; Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      295.0(10)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/Sapphire3 CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28750
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.613
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.786
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         3675
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0938P)^2^+8.2654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2035
_reflns_number_gt                3213
_reflns_number_total             3675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7686sup1.cif
_cod_data_source_block           I
_cod_database_code               2020839
_cod_database_fobs_code          2020839
_shelx_hkl_checksum              89003
_shelx_res_checksum              40730