Synthesis and characterization of a new cyclic phosph(V)azane ligand [(C6H5N)P(O)H]2 and its zinc(II) complex

Abstract

The new cyclic phosph(V)azane ligand [(C6H5N)P(O)H]2 (2) is obtained from the reaction between PCl3 and PhNH2 in toluene followed by controlled hydrolysis of the product in an H2O–CHCl3 solution. Compound 2 is the first example of P(V) dimer [(µ-NC6H5)P(H)=O]2, a P2N2 ring with two P(O)H moieties. The reaction of 2 with ZnCl2 in a molar ratio of 1 : 1 in tetrahydrofuran yields the cyclophosph(V)azane complex Cl2Zn[(C6H5N)P(O)H]2 (3) in which Zn–O bonds form directly between a cyclic phosph(V)azane ligand and Zn(II). The products have been characterized by infrared, multinuclear (1H, 31P, 13C) NMR, mass spectrometry, and elemental analysis.