4-Phenyl-1,2,4-tri-aza-spiro-[4.5]dec-1-ene-3-thione.
Akkurt, Mehmet; Mague, Joel T.; Mohamed, Shaaban K.; Hassan, Alaa A.; Albayati, Mustafa R.; Acta crystallographica. Section E, Structure reports online 69 (2013) o1259–; doi:10.1107/S1600536813019120

data_2311170
_publ_section_title
;
 4-Phenyl-1,2,4-tri-aza-spiro-[4.5]dec-1-ene-3-thione.
;
_journal_coeditor_code           TK5237
_journal_issue                   'Pt 8'
_journal_name_full
'Acta crystallographica. Section E, Structure reports online'
_journal_page_first              o1259
_journal_paper_doi               10.1107/S1600536813019120
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C13 H15 N3 S'
_chemical_formula_moiety         'C13 H15 N3 S'
_chemical_formula_sum            'C13 H15 N3 S'
_chemical_formula_weight         245.34
_chemical_name_systematic
;
4-Phenyl-1,2,4-triazaspiro[4.5]dec-1-ene-3-thione
;
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.4952(9)
_cell_length_b                   7.4845(7)
_cell_length_c                   34.692(3)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.61
_cell_measurement_theta_min      2.45
_cell_volume                     2465.5(4)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3660
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            41202
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        28.67
_diffrn_reflns_theta_max         28.67
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2013)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
' W=1/[\S^2^(FO^2^)+(0.0483P)^2^+1.0447P]  where P=(FO^2^+2FC^2^)/3 '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1044
_reflns_number_gt                2899
_reflns_number_total             3168
_reflns_threshold_expression     I>2\s(I)
_publcif_datablock.id            {cc36d388-8c62-4938-bf6f-2547d5f8b28f}
_cod_data_source_file            tk5237sup1.cif
_cod_data_source_block           I
_cod_database_code               2311170