Structure and Bonding of Diiodine Adducts of the Sulfur-Rich Donors 1,3-Dithiacyclohexane-2-thione (ptc) and 4,5-Ethylenedithio-1,3-dithiole-2-thione (ttb)
Francesco Bigoli; Paola Deplano; Andrea Ienco; Carlo Mealli; Maria Laura Mercuri; Maria Angela Pellinghelli; Gloria Pintus; Giuseppe Saba; Emanuele F. Trogu; Inorganic Chemistry 38 (1999) 4626–4636; doi:10.1021/ic9901867

data_4322306
_publ_section_title
;
 Structure and Bonding of Diiodine Adducts of the Sulfur-Rich Donors
 1,3-Dithiacyclohexane-2-thione (ptc) and
 4,5-Ethylenedithio-1,3-dithiole-2-thione (ttb)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4626
_journal_page_last               4636
_journal_paper_doi               10.1021/ic9901867
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        'chemical synthesis'
_chemical_formula_analytical     'C4 H6 I2 S3'
_chemical_formula_sum            'C4 H6 I2 S3'
_chemical_formula_weight         404.07
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.43(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.691(6)
_cell_length_b                   9.010(6)
_cell_length_c                   13.237(5)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      10
_cell_volume                     1008.2(10)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Philips PW 1100 local upgrade'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Philips PW 1100 diffractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKar
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2279
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    6.787
_exptl_absorpt_correction_T_max  1.4051
_exptl_absorpt_correction_T_min  0.7081
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blu
_exptl_crystal_density_diffrn    2.662
_exptl_crystal_description       prism
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.775
_refine_ls_goodness_of_fit_obs   0.900
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         2192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.775
_refine_ls_restrained_S_obs      0.900
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_obs          0.0305
_refine_ls_shift/esd_max         0.163
_refine_ls_shift/esd_mean        0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0262P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0661
_refine_ls_wR_factor_obs         0.0611
_reflns_number_observed          1420
_reflns_number_total             2192
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9901867_2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0262P)^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^)+( 0.0262P)^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_database_code               4322306