13-[4,5-Bis(methylsulfanyl)-1,3-dithiol-2-ylidene]-6-oxa-3,9,12,14-tetrathiabicyclo[9.3.0]tetradec-1(11)-ene
Hou, Rui-Bin; Li, Bao; Che, Tie; Yin, Bing-Zhu; Wu, Li-Xin; Acta Crystallographica Section E 65 (2009) o2538–; doi:10.1107/S1600536809037301

data_2223499
_publ_section_title
13-[4,5-Bis(methylsulfanyl)-1,3-dithiol-2-ylidene]-6-oxa-3,9,12,14-tetrathiabicyclo[9.3.0]tetradec-1(11)-ene
_journal_coeditor_code           NG2642
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2538
_journal_paper_doi               10.1107/S1600536809037301
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C14 H18 O S8'
_chemical_formula_moiety         'C14 H18 O S8'
_chemical_formula_sum            'C14 H18 O S8'
_chemical_formula_weight         458.76
_chemical_name_common
;
2,3-(5-Oxa-2,8-dithiacycloundecane)-6,7-dimethylthio-1,4,5,8-
tetrathiafulvalene
;
_chemical_name_systematic
;
13-[4,5-bis(methylsulfanyl)-1,3-dithiol-2-ylidene]-6-oxa-3,9,12,14-
tetrathiabicyclo[9.3.0]tetradec-1(11)-ene
;
_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                105.00(3)
_cell_angle_beta                 97.83(3)
_cell_angle_gamma                112.22(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4542(17)
_cell_length_b                   10.158(2)
_cell_length_c                   13.612(3)
_cell_measurement_reflns_used    8201
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.09
_cell_volume                     1008.8(5)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9961
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.9013
_exptl_absorpt_correction_T_min  0.8862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.637
_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     210
_refine_ls_number_reflns         4572
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+0.6622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1702
_reflns_number_gt                3655
_reflns_number_total             4572
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2642.cif
_cod_data_source_block           I
_cod_original_cell_volume        1008.8(3)
_cod_database_code               2223499
_cod_database_fobs_code          2223499