Reaction of thiones with dihalogens; comparison of the solid state structures of 4,5-bis(methylsulfanyl)-1,3-dithiole-2-thione–diiodine, –dibromine and –iodine monobromide
Bricklebank, Neil; Skabara, Peter J.; Hibbs, David E.; Hursthouse, Michael B.; Abdul Malik, K. M.; Journal of the Chemical Society, Dalton Transactions  (1999) 3007–; doi:10.1039/a903068i

data_7027473
_publ_section_title
;
 Reaction of thiones with dihalogens; comparison of the solid state
 structures of 4,5-bis(methylsulfanyl)-1,3-dithiole-2-thione--diiodine,
 --dibromine and --iodine monobromide
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3007
_journal_paper_doi               10.1039/a903068i
_journal_year                    1999
_chemical_formula_moiety         'C5H6BrS4, Br3, 0.5(Br2)'
_chemical_formula_sum            'C5 H6 Br5 S4'
_chemical_formula_weight         593.89
_chemical_name_systematic
; 
 2-Bromo-4,5-bis(methylthio)-1,3-dithiolium tribromide, Bromine (2:1)
;
_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
_audit_creation_method           SHELXL-93
_cell_angle_alpha                84.060(10)
_cell_angle_beta                 80.958(9)
_cell_angle_gamma                69.198(9)
_cell_formula_units_Z            2
_cell_length_a                   6.4872(6)
_cell_length_b                   7.0403(9)
_cell_length_c                   17.166(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.41
_cell_volume                     722.8(2)
_computing_cell_refinement       'REFINE in MADNES'
_computing_data_collection       MADNES
_computing_data_reduction        'ABSMAD (Karaulov, 1991)'
_computing_molecular_graphics    'SNOOPI (Davies, 1983)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'FAST area detector'
_diffrn_measurement_method       'Darr, Drake, Hursthouse & Malik, 1993'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3011
_diffrn_reflns_theta_max         24.92
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    14.440
_exptl_absorpt_correction_T_max  1.021
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.729
_exptl_crystal_description       prism
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.131
_refine_ls_hydrogen_treatment    'calculated positions (riding model)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_restrained_S_obs      1.131
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_obs          0.0450
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1136
_refine_ls_wR_factor_obs         0.1116
_reflns_number_observed          1577
_reflns_number_total             1973
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903068isup1.cif
_cod_data_source_block           compd2
_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^)+(0.0608P)^2^+0.0000P] 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^)+(0.0608P)^2^+0.0000P] 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 (no. 2)'
_cod_database_code               7027473