Crystal structure of (2<i>E</i>)-<i>N</i>-methyl-2-(2-oxo-1,2-dihydroacenaphthylen-1-ylidene)hydrazinecarbothioamide
Vimala, G.; Govindaraj, J.; Haribabu, J.; Karvembu, R.; SubbiahPandi, A.; Acta Crystallographica Section E 70 (2014) 415–417; doi:10.1107/S1600536814023216

data_2240121
_publ_section_title
;
 Crystal structure of
 (2<i>E</i>)-<i>N</i>-methyl-2-(2-oxo-1,2-dihydroacenaphthylen-1-ylidene)hydrazinecarbothioamide
;
_journal_coeditor_code           SU2796
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              415
_journal_page_last               417
_journal_paper_doi               10.1107/S1600536814023216
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C14 H11 N3 O S'
_chemical_formula_moiety         'C14 H11 N3 O S'
_chemical_formula_sum            'C14 H11 N3 O S'
_chemical_formula_weight         269.33
_chemical_name_systematic
(2<i>E</i>)-<i>N</i>-Methyl-2-(2-oxo-1,2-dihydroacenaphthylen-1-ylidene)hydrazinecarbothioamide
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1110(6)
_cell_length_b                   10.0547(11)
_cell_length_c                   21.497(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1320.9(2)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2008)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2008)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2008)
;
_computing_molecular_graphics
;
<i>ORTEP-3 for Windows</i> (Farrugia, 2012) and PLATON (Spek,
2009)
;
_computing_publication_material
;
<i>SHELXL97</i> (Sheldrick, 2008) and <i>PLATON</i> (Spek,
2009)
;
_computing_structure_refinement
;
<i>SHELXL97</i> (Sheldrick, 2008)
;
_computing_structure_solution
;
<i>SHELXS97</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker SMART 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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23135
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.23
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.213
_refine_ls_abs_structure_details
;
Flack (1983); Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.02(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.2048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                2929
_reflns_number_total             3941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            su2796sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1320.8(2)
_cod_database_code               2240121
_cod_database_fobs_code          2240121