Synthesis, spectroscopic investigations and crystal structures of organotin(IV) derivatives of 2-amino-1-cyclopentene-1-carbodithioic acid

The organotin(IV) chlorides RnSnCl4-n, (n = 2, R = Bu-n or Ph; and n = 3, R = Ph) react with 2-amino-1-cyclopentene-1-carbodithioic acid (ACDA) to giv e [Ph2SnCl(ACDA)] (1), [Ph2Sn(ACDA)(2)] (2), [Ph3Sn(ACDA)] (3) and [Bu2Sn(A CDA)(2)] (4). The new complexes have been characterized by elemental analys is, UV-Vis, IR, H-1 NMR,Sn-119 NMR spectroscopy and mass spectrometry. On t he basis of Sn-119 NMR data the effective coordination number in solution i s five. The structures of 1, 3 and 4 have been confirmed by X-ray crystallo graphy. Crystals of 1 are monoclinic with space group P2(1)/n. The tin envi ronment is distorted trigonal bipyramid with Cl and sulfur atoms in epical positions. Crystals of 3 are orthorombic, P2(1)2(1)2(1), and the structure is distorted trigonal bipyramid with one sulfur and phenyl in the axial pos ition. Complex 4 crystallizes in the triclinic space group, P (1) over bar, and the Sn atom shows extremely irregular octahedral coordination with fou r S atoms laying in the equatorial plane. In all complexes ACDA coordinates as an anisobidentate ligand and its orientation lends to form a NHS intram olecular hydrogen bond. The packing is also stabilized by intermolecular hy drogen bonding. (C) 2001 Elsevier Science B.V. All rights reserved.