3,9-Bis(dicyanomethylene)-2,4,8,10-tetrathiaspiro[5.5]undecane
Zhou, Zheng-Rong; Xu, Wei; Xia, Yi; Wang, Quan-Rui; Ding, Zong-Biao; Chen, Min-Qin; Hua, Zhong-Yi; Tao, Feng-Gang; Acta Crystallographica Section C 57 (2001) 471–472; doi:10.1107/S0108270101000543

data_2011843
_publ_section_title
;
 3,9-Bis(dicyanomethylene)-2,4,8,10-tetrathiaspiro[5.5]undecane
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              471
_journal_page_last               472
_journal_paper_doi               10.1107/S0108270101000543
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C13 H8 N4 S4'
_chemical_formula_sum            'C13 H8 N4 S4'
_chemical_formula_weight         348.47
_chemical_name_systematic
2,2'-(2,4,8,10-tetrathiaspiro[5.5]undecane-3,9-diylidene)bis(propanedinitrile)
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 95.53(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.596(8)
_cell_length_b                   7.157(2)
_cell_length_c                   16.498(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.25
_cell_measurement_theta_min      6.90
_cell_volume                     1480.4(11)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1992)
;
_computing_data_reduction
'TEXSAN ((Molecular Structure Corporation, 1985)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .461
_diffrn_measured_fraction_theta_max .461
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .039
_diffrn_reflns_av_sigmaI/netI    .066
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            1370
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        -1.18
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .638
_exptl_absorpt_correction_T_max  .883
_exptl_absorpt_correction_T_min  .832
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         .674
_refine_diff_density_min         -.346
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          .103
_refine_ls_R_factor_gt           .057
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0659P)^2^+6.8039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .177
_reflns_number_gt                872
_reflns_number_total             1307
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bj1015.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2011843
_cod_database_fobs_code          2011843