The synthesis of the first phosphorylated derivatives of p-tert-butylthioca
lix[4]arene was achieved by reaction with phosphorus trichloride. The produ
ct containing two cyclic P(III) atoms is not hydrolytically stable. The fla
ttened 1,2-alternate conformation of a P(IV) derivative was established by
H-1, C-13, P-31 NMR experiments and X-ray analysis. (C) 1999 Elsevier Scien
ce Ltd. All rights reserved.