4,6,7,9,10,12-Hexahydro-1,3-dithiolo[4,5-<i>f</i>][1,4,9]oxadithiacycloundecine-2-thione
Hou, Rui-Bin; Li, Bao; Yin, Bing-Zhu; Wu, Li-Xin; Acta Crystallographica Section E 65 (2009) o1710–; doi:10.1107/S1600536809024003

data_2222287
_publ_section_title
4,6,7,9,10,12-Hexahydro-1,3-dithiolo[4,5-<i>f</i>][1,4,9]oxadithiacycloundecine-2-thione
_journal_coeditor_code           CV2573
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1710
_journal_paper_doi               10.1107/S1600536809024003
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C9 H12 O S5'
_chemical_formula_moiety         'C9 H12 O S5'
_chemical_formula_sum            'C9 H12 O S5'
_chemical_formula_weight         296.49
_chemical_name_systematic
;
4,6,7,9,10,12-Hexahydro-1,3-
dithiolo[4,5-<i>f</i>][1,4,9]oxadithiacycloundecine-2-thione
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.10(3)
_cell_angle_beta                 106.58(3)
_cell_angle_gamma                112.74(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3425(17)
_cell_length_b                   8.9611(18)
_cell_length_c                   9.820(2)
_cell_measurement_reflns_used    5678
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.02
_cell_measurement_theta_min      3.43
_cell_volume                     622.2(3)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_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  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6141
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  0.8996
_exptl_absorpt_correction_T_min  0.8767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+0.2783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                2560
_reflns_number_total             2813
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2573.cif
_cod_data_source_block           I
_cod_original_cell_volume        622.2(2)
_cod_database_code               2222287
_cod_database_fobs_code          2222287