Preparation, crystal and molecular structure of trans-dioxo(1,4-dithia-8,11-diazacyclotetradecane)technetium(V) hexafluorophosphate

The preparation and X-ray structure of trans- [TcO2(14-ane-N2S2)]PF6 are described. The complex is obtained via a ligand exchange reaction of(n-Bu)4N- [TcOBr4] with 1,4-dithia-8,11-diazacyclotetradecane. The crystals are monoclinic, space group P21/n, with a=9.726(3), b=9.668(2), c=19.262(3) Å, β= 95.84(2)° and Z=4. The structure was solved by the heavy-atom method and refined using the full-matrix least-squares technique up to R=0.036 and Rw= 0.037. The two ions are characterized by the presence of centrosymmetric dimers generated by strong intermolecular hydrogen bonds. © 1989.