Crystallization of [Sb(S2CNEt2)2l] from chloroform gives an adduct [Sb(S2CNEt2)2l]·CHCl3. Single-crystal X-ray structure determination shows the complex to be comprised of a polymeric chain of the form -Sb(S2CNEt2)2-I-Sb(S2CNEt 2)2- with bridging iodine atoms linking Sb(S2CNEt2)2 units; the chloroform molecule is strongly hydrogen bonded to the polymer via the iodine atoms. Crystals are orthorhombic, space group Pcab, with a = 19.237(8), b = 12.534(5), c = 19.535(7) Å, and Z = 8, with the polymer chain parallel to b. Crystallization from methylene chloride instead with excess of iodine yields an adduct [Sb(S2CNEt2)2l]·(0.5l2) x, x ≤ 1. The unit-cell dimensions are a ca. 22.5, b ca. 10.0, c ca. 19.2 Å, Z = 8, and the space group Pbcn. Again the structure is a polymeric unit (similar to the above) running parallel to b with adjacent strands linked by l2 molecules charge-transfer bonded at the iodide units. As the molecular iodine content of the complex rises, its sites become increasingly populated, bonding the polymer strands more compactly and decreasing the cell volume.
|Number of pages||6|
|Journal||Journal of the Chemical Society, Dalton Transactions|
|Publication status||Published - 1981|