Synthesis and characterization of technetium complexes with phosphoruscontaining ligands. The homoleptic trimethylphosphite, dimethylmethylphosphonite and methyldiethylphosphinite technetium(I) cations

✍ Scribed by Dennis W. Wester; David H. White; Fred W. Miller; Richard T. Dean; John A. Schreifels; Jerry E. Hunt

• Publisher: Elsevier Science
• Year: 1987
• Tongue: English
• Weight: 729 KB
• Volume: 131
• Category: Article
• ISSN: 0020-1693
• DOI: 10.1016/s0020-1693(00)96019-5

✦ Synopsis

Technetium(I)

complexes of trimethylphosphite (tmp), dimethylmethylphosphonite (dmmp) and methyldiethylphosphinite (mdep) have been synthesized through direct interaction of the ligand with sodium pertechnetate.

The homoleptic, hexakis (ligand), cationic complexes can be isolated as tetraphenylborate salts. Characterization using multinuclear NMR of ?c (-422 and -248 ppm versus Tc04-for the tmp and dmmp complexes, respectively) and 31P (158.5 and 248 ppm versus 85% H3PQ4 for the tmp and dmmp complexes, respectively) gives chemical shift values which compare favorably with previous data on Tc-phosphine and transitionmetal-phosphite complexes. Mass spectra (fast atom bombardment and plasma desorption) of the tmp and dmmp complexes exhibit the expected parent peaks and show series of peaks attributed to stepwise loss of ligand molecules or possible decomposition products. X-ray photoelectron spectra of the tmp and dmmp complexes are consistent with formulation as the Tc(1) oxidation state when referenced to wellcharacterized complexes in known oxidation states.