5,8-Diethyl-6,9-dithioxo-2,3,5,6,8,9-hexahydro-1<i>H</i>-3a,5,8,9a-tetraazaphenalene-4,7-dione
Yadava, Umesh; Goel, Atul; Ram, Vishnu Ji; Maulik, Prakas R.; Acta Crystallographica Section E 62 (2006) o4991–o4993; doi:10.1107/S1600536806041286

data_2210986
_publ_section_title
5,8-Diethyl-6,9-dithioxo-2,3,5,6,8,9-hexahydro-1<i>H</i>-3a,5,8,9a-tetraazaphenalene-4,7-dione
_journal_coeditor_code           FB2024
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4991
_journal_page_last               o4993
_journal_paper_doi               10.1107/S1600536806041286
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C13 H16 N4 O2 S2'
_chemical_formula_moiety         'C13 H16 N4 O2 S2'
_chemical_formula_sum            'C13 H16 N4 O2 S2'
_chemical_formula_weight         324.42
_chemical_melting_point          468
_chemical_name_common            Tetraazaphenalene
_chemical_name_systematic
;
5,8-Diethyl-6,9-dithioxo-2,3,5,6,8,9-hexahydro-(1H)-3a,5,8,9a-
tetraazaphenalene-4,7-dione
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.33(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.155(2)
_cell_length_b                   10.261(2)
_cell_length_c                   14.382(3)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      12.502
_cell_measurement_theta_min      5.194
_cell_volume                     1464.0(5)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL-NT
_computing_publication_material  SHELXTL-NT
_computing_structure_refinement  SHELXTL-NT
_computing_structure_solution    'SHELXTL-NT (Bruker, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       \q/2\q
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3740
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.375
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.704
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    64
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0680
_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^)+(0.1273P)^2^+1.5323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1936
_refine_ls_wR_factor_ref         0.2188
_reflns_number_gt                2180
_reflns_number_total             2863
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fb2024.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2210986
_cod_database_fobs_code          2210986