4,6,7,9,10,12,13,15-Octahydro-2<i>H</i>-1,3-dithiolo[4,5-<i>i</i>][1,4,7,12]dioxadithiacyclotetradecine-2-thione
Hou, Rui-Bin; Li, Bao; Chen, Tie; Yin, Bing-Zhu; Wu, Li-Xin; Acta Crystallographica Section E 65 (2009) o2042–; doi:10.1107/S1600536809029468

data_2222656
_publ_section_title
4,6,7,9,10,12,13,15-Octahydro-2<i>H</i>-1,3-dithiolo[4,5-<i>i</i>][1,4,7,12]dioxadithiacyclotetradecine-2-thione
_journal_coeditor_code           CV2592
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2042
_journal_paper_doi               10.1107/S1600536809029468
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C11 H16 O2 S5'
_chemical_formula_moiety         'C11 H16 O2 S5'
_chemical_formula_sum            'C11 H16 O2 S5'
_chemical_formula_weight         340.54
_chemical_name_systematic
;
4,6,7,9,10,12,13,15-Octahydro-2<i>H</i>-1,3-
dithiolo[4,5-<i>i</i>][1,4,7,12]dioxadithiacyclotetradecine-2-thione
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9201(18)
_cell_length_b                   8.5317(17)
_cell_length_c                   10.128(2)
_cell_measurement_reflns_used    7211
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      3.13
_cell_volume                     765.0(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7527
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  0.9222
_exptl_absorpt_correction_T_min  0.9090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.223
_refine_ls_abs_structure_details 'Flack (1983); 1359 Friedel pairs'
_refine_ls_abs_structure_Flack   0.42(9)
_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     164
_refine_ls_number_reflns         3221
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.1939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                3100
_reflns_number_total             3221
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2592.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2222656
_cod_database_fobs_code          2222656