P-31 CP-MAS NMR, VIBRATIONAL, AND X-RAY CHARACTERIZATION OF THE ADDUCTS OF TRIPHENYLPHOSPHINE SULFIDE WITH ICL AND IBR

The reactions between triphenylphosphine sulfide (Ph3PS) and ICl in CC l4 and IBr in CH2Cl2 in 1:1 molar ratio give the solid adducts Ph3PS . ICl (I) and Ph3PS . IBr (II) whose structures have been solved by X-r ay diffraction. Compounds I and II consist of discrete molecule units and feature the S-I-Cl or S-I-Br linear group. The S-I bond distances in I, II (2.641(1), 2.665(1) Angstrom respectively) and in compound 2P h(3)PS . 3I(2) (III) (2.729(2) Angstrom) are correlable to the net inc rease in the I-X (X = Cl, Br, I) bond distance. The structural feature s of I, II and III are in accordance with P-31 CP-MAS NMR, FT-Raman an d FT-IR spectral data, and elucidate the nature of the donor (Ph3PS)-a cceptor (ICl, IBr, I-2) interaction.