3,9-Dimethyl-2,3-dihydrospiro[carbazole-1,2'-[1,3]dithiolan]-4(9<i>H</i>)-one
Gülle, Sibel; Çaylak Delibaş, Nagihan; Ergün, Yavuz; Hökelek, Tuncer; Acta Crystallographica Section E 69 (2013) o598–o599; doi:10.1107/S1600536813007873

data_2237738
_publ_section_title
;
 3,9-Dimethyl-2,3-dihydrospiro[carbazole-1,2'-[1,3]dithiolan]-4(9<i>H</i>)-one
;
_journal_coeditor_code           XU5690
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o598
_journal_page_last               o599
_journal_paper_doi               10.1107/S1600536813007873
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C16 H17 N O S2'
_chemical_formula_moiety         'C16 H17 N O S2'
_chemical_formula_sum            'C16 H17 N O S2'
_chemical_formula_weight         303.43
_chemical_name_systematic
;
3,9-Dimethyl-2,3-dihydrospiro[carbazole-1,2'-[1,3]dithiolan]-4(9<i>H</i>)-one
;
_space_group_IT_number           61
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.8163(3)
_cell_length_b                   9.8407(2)
_cell_length_c                   17.2913(4)
_cell_measurement_reflns_used    3799
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.67
_cell_volume                     2861.44(10)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material
'WinGX (Farrugia, 2012) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13394
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.9012
_exptl_absorpt_correction_T_min  0.8466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.734
_refine_diff_density_min         -1.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0752
_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^)+(0.0845P)^2^+10.7607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1849
_refine_ls_wR_factor_ref         0.1948
_reflns_number_gt                2912
_reflns_number_total             3540
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu5690.cif
_cod_data_source_block           I
_cod_database_code               2237738
_cod_database_fobs_code          2237738