Crystal structures of two hydrazinecarbothioamide derivatives: (<i>E</i>)-<i>N</i>-ethyl-2-[(4-oxo-4<i>H</i>-chromen-3-yl)methylidene]hydrazinecarbothioamide hemihydrate and (<i>E</i>)-2-[(4-chloro-2<i>H</i>-chromen-3-yl)methylidene]-<i>N</i>-phenylhydrazinecarbothioamide
Gangadharan, Rajeswari; Haribabu, Jebiti; Karvembu, Ramasamy; Sethusankar, K.; Acta Crystallographica Section E 71 (2015) 305–308; doi:10.1107/S2056989015003369

data_2240442
_publ_section_title
;
 Crystal structures of two hydrazinecarbothioamide derivatives:
 (<i>E</i>)-<i>N</i>-ethyl-2-[(4-oxo-4<i>H</i>-chromen-3-yl)methylidene]hydrazinecarbothioamide
 hemihydrate and
 (<i>E</i>)-2-[(4-chloro-2<i>H</i>-chromen-3-yl)methylidene]-<i>N</i>-phenylhydrazinecarbothioamide
;
_journal_coeditor_code           SU5078
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              305
_journal_page_last               308
_journal_paper_doi               10.1107/S2056989015003369
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C13 H13 N3 O2 S, 0.5H2 O'
_chemical_formula_moiety         'C13 H13 N3 O2 S, 0.5(H2 O)'
_chemical_formula_sum            'C13 H14 N3 O2.5 S'
_chemical_formula_weight         284.33
_chemical_name_systematic
'(<i>E</i>)-<i>N</i>-Ethyl-2-[(4-oxo-4<i>H</i>-chromen-3-yl)methylidene]hydrazinecarbothioamide hemihydrate'
_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                114.379(2)
_cell_angle_beta                 95.751(3)
_cell_angle_gamma                94.200(2)
_cell_formula_units_Z            4
_cell_length_a                   8.2858(2)
_cell_length_b                   12.5422(4)
_cell_length_c                   14.3520(5)
_cell_measurement_reflns_used    5579
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.63
_cell_measurement_theta_min      1.57
_cell_volume                     1340.81(8)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) 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
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f 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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19142
_diffrn_reflns_theta_full        26.63
_diffrn_reflns_theta_max         26.63
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5579
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0658P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                2764
_reflns_number_total             5579
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su5078sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1340.81(7)
_cod_database_code               2240442
_cod_database_fobs_code          2240442