Abstract

One-pot reactions of [MCl 2(cod)] (cod= cyclo-octa-1,5-diene; M=Pt, Pd) with two equiv of PPh 3 or AsPh 3, one equiv of thiosalicylic acid, and an excess of triethylamine base, followed by the addition of excess Na[BPh 4] to the hot reaction mixture gives complexes [(Ph 3E) 2M(SC 6H 4CO 2)⋯HNEt 3] +[BPh 4] − (E=P, As). Analogous pyridinium and platinum–thioglycolate [(Ph 3P) 2Pt(SCH 2CO 2)] derivatives were also prepared. An X-ray crystal structure determination on [(Ph 3P) 2Pt(SC 6H 4CO 2)⋯HNEt 3] +[BPh 4] − reveals hydrogen-bonding between the NH proton and the carbonyl group of the thiosalicylate ligand, the major effect of which is to flatten the platinum–thiosalicylate moiety. NMR spectroscopic data indicate that the hydrogen-bonding interaction persists in solution.

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