3aH,4H,5H,8H,9H,9aH-Cycloocta[d][1,3]dioxole-2-thione
Schollmeyer, Dieter; Kammler, Claudia; Detert, Heiner; IUCrData 9 (2024) x241019–; doi:10.1107/S2414314624010198

data_1573077
_publ_section_title
;
 3aH,4H,5H,8H,9H,9aH-Cycloocta[d][1,3]dioxole-2-thione
;
_journal_coeditor_code           BT4155
_journal_issue                   11
_journal_name_full               IUCrData
_journal_page_first              x241019
_journal_paper_doi               10.1107/S2414314624010198
_journal_volume                  9
_journal_year                    2024
_chemical_formula_iupac          'C9 H12 O2 S'
_chemical_formula_moiety         'C9 H12 O2 S'
_chemical_formula_sum            'C9 H12 O2 S'
_chemical_formula_weight         184.25
_chemical_name_systematic
3a<i>H</i>,4<i>H</i>,5<i>H</i>,8<i>H</i>,9<i>H</i>,9a<i>H</i>-Cycloocta[<i>d</i>][1,3]dioxole-2-thione
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5555(9)
_cell_length_b                   15.7119(17)
_cell_length_c                   7.4892(8)
_cell_measurement_reflns_used    3621
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.99
_cell_volume                     889.05(17)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (Stoe & Cie, 2020)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (Stoe & Cie, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (Stoe & Cie, 2020)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3713
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.959
_diffrn_reflns_theta_min         2.992
_diffrn_source                   'sealed X-ray tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_T_max  0.9885
_exptl_absorpt_correction_T_min  0.8984
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       needle
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.290
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1963
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+2.2293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                1439
_reflns_number_total             1963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bt4155.cif
_cod_data_source_block           I
_cod_database_code               1573077
_shelx_estimated_absorpt_t_min   0.839
_shelx_estimated_absorpt_t_max   0.991
_shelx_hkl_checksum              3424
_shelx_res_checksum              95640