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_4322305
_publ_section_title
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 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)
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_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     'C5 H4 I2 S5'
_chemical_formula_sum            'C5 H4 I2 S5'
_chemical_formula_weight         478.18
_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                 99.30(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.090(6)
_cell_length_b                   6.433(5)
_cell_length_c                   15.731(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      10
_cell_volume                     1207.4(12)
_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           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2728
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         3.35
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    6.023
_exptl_absorpt_correction_T_max  1.291
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   'empirical following North et al.'
_exptl_crystal_colour            blu
_exptl_crystal_density_diffrn    2.631
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.856
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.223
_refine_ls_extinction_coef       0.016(1)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.227
_refine_ls_goodness_of_fit_obs   1.046
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.253
_refine_ls_restrained_S_obs      1.046
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_obs          0.0419
_refine_ls_shift/esd_max         0.079
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0599P)^2^+4.0119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1471
_refine_ls_wR_factor_obs         0.1016
_reflns_number_observed          1828
_reflns_number_total             2640
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9901867_1.cif
_cod_data_source_block           2
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0599P)^2^+4.0119P] 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^)+( 0.0599P)^2^+4.0119P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322305