The radical ions of acenaphtho[1,2-b][1,4]dithiine derivatives and acenaphtho[1,2-b][1,4]oxathiine: Solution EPR and ENDOR studies. The X-ray crystal structures of 8,9-bis(methylsulfanyl)acenaphtho[1,2-b][1,4]dithiine and its complexes with 7,7,8,8-tetracyano-p-quinodimethane (TCNQ), 2,5-dibromo-TCNQ and iodine
Bryce, Martin R.; Lay, Alexander K.; Chesney, Antony; Batsanov, Andrei S.; Howard, Judith A. K.; Buser, Urs; Gerson, Fabian; Merstetter, Pascal; Journal of the Chemical Society, Perkin Transactions 2  (1999) 755–; doi:10.1039/a809872g

data_7213002
_publ_section_title
;
 The radical ions of acenaphtho[1,2-b][1,4]dithiine derivatives and
 acenaphtho[1,2-b][1,4]oxathiine: Solution EPR and ENDOR studies. The
 X-ray crystal structures of
 8,9-bis(methylsulfanyl)acenaphtho[1,2-b][1,4]dithiine and its complexes
 with 7,7,8,8-tetracyano-p-quinodimethane (TCNQ), 2,5-dibromo-TCNQ and
 iodine
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              755
_journal_paper_doi               10.1039/a809872g
_journal_year                    1999
_chemical_formula_moiety         'C16 H12 S4 1+, I3 1-, 2(I2)'
_chemical_formula_sum            'C16 H12 I7 S4'
_chemical_formula_weight         1220.80
_chemical_name_systematic
; 
 8,9-di(methylsulfanyl)acenaphthyleno[1,2-b][1,4]dithiine bis(diiodine)
 triiodide
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                64.76(1)
_cell_angle_beta                 78.80(1)
_cell_angle_gamma                79.74(1)
_cell_formula_units_Z            2
_cell_length_a                   10.420(1)
_cell_length_b                   11.263(1)
_cell_length_c                   13.087(1)
_cell_measurement_reflns_used    512
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      12
_cell_volume                     1354.9(2)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Siemens CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17175
_diffrn_reflns_theta_max         30.25
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  '16 h'
_diffrn_standards_number         212
_exptl_absorpt_coefficient_mu    8.330
_exptl_absorpt_correction_T_max  0.4191
_exptl_absorpt_correction_T_min  0.2586
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.992
_exptl_crystal_description       rhombohedron
_exptl_crystal_F_000             1086
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.152
_refine_diff_density_min         -1.886
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.104
_refine_ls_goodness_of_fit_obs   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         7262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_restrained_S_obs      1.109
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_obs          0.0395
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+3.6829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0992
_refine_ls_wR_factor_obs         0.0881
_reflns_number_observed          5770
_reflns_number_total             7267
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809872gsup1.cif
_cod_data_source_block           5(I7)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+3.6829P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+3.6829P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7213002