Crystal structure of triphenylphosphine sulfide diiodine; the first crystallographically characterised 1∶1 molecular charge-transfer complex of a tertiary phosphine sulfide with diiodine
Apperley, David C.; Bricklebank, Neil; Burns, Sally L.; Hibbs, David E.; Hursthouse, Michael B.; Abdul Malik, K. M.; Journal of the Chemical Society, Dalton Transactions  (1998) 1289–; doi:10.1039/a709121d

data_7027987
_publ_section_title
;
 Crystal structure of triphenylphosphine sulfide diiodine; the first
 crystallographically characterised 1&#x2236;1 molecular charge-transfer
 complex of a tertiary phosphine sulfide with diiodine
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1289
_journal_paper_doi               10.1039/a709121d
_journal_year                    1998
_chemical_formula_moiety         C18H15I2PS
_chemical_formula_sum            'C18 H15 I2 P S'
_chemical_formula_weight         548.13
_chemical_name_systematic        Triphenylphosphinesulfide-diiodide
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-93
_cell_angle_alpha                90.00
_cell_angle_beta                 97.400(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.618(2)
_cell_length_b                   9.454(3)
_cell_length_c                   15.930(6)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      1.94
_cell_volume                     1884.5(10)
_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      293(2)
_diffrn_measurement_device       'FAST area detector diffractomer'
_diffrn_measurement_method       'Darr, Drake, Hursthose & Malik, 1993)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode generator, Mo anode)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7642
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    3.527
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   'DIFABS (Walker & Stuart, 1983)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.799
_refine_ls_goodness_of_fit_obs   0.956
_refine_ls_hydrogen_treatment    'calculated positions, riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.799
_refine_ls_restrained_S_obs      0.956
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_obs          0.0270
_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^)+(0.0185P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0572
_refine_ls_wR_factor_obs         0.0543
_reflns_number_observed          1878
_reflns_number_total             2875
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            d709121sup1.cif
_cod_data_source_block           C18H15I2PS
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0185P)^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^)+(0.0185P)^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      'P2(1)/n  (No. 14)'
_cod_database_code               7027987