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_7027470
_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         C5H6S5.Br2
_chemical_formula_sum            'C5 H6 Br2 S5'
_chemical_formula_weight         386.22
_chemical_name_systematic
; 
4,5-Bis(methylthio)-1,3-dithiole-2-thione dibromine
;
_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                69.042(13)
_cell_angle_beta                 87.146(11)
_cell_angle_gamma                87.880(8)
_cell_formula_units_Z            2
_cell_length_a                   6.9403(9)
_cell_length_b                   8.3128(14)
_cell_length_c                   10.554(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.87
_cell_measurement_theta_min      2.62
_cell_volume                     567.8(3)
_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 diffractometer'
_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  0.0778
_diffrn_reflns_av_sigmaI/netI    0.1124
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1581
_diffrn_reflns_theta_max         24.87
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    8.003
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    2.259
_exptl_crystal_description       prism
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.975
_refine_ls_goodness_of_fit_obs   1.125
_refine_ls_hydrogen_treatment    'Calculated positions (riding model)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1181
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.965
_refine_ls_restrained_S_obs      1.108
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_obs          0.0492
_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^)+(0.0607P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1346
_refine_ls_wR_factor_obs         0.1325
_reflns_number_observed          882
_reflns_number_total             1181
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903068isup1.cif
_cod_data_source_block           1BR2
_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^)+(0.0607P)^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^)+(0.0607P)^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_cell_volume        567.8(2)
_cod_original_sg_symbol_H-M      'P-1 (no. 2)'
_cod_database_code               7027470