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The structure, spectroscopic properties and chemical stability of [VS4-(CuPPh3)3 (CuCl)Br2] in CDCl3 solution have been studied by multinuclear NMR tech-nique. Two peaks with relative intensity of 1: 4 are found in the31P-{1H} spectra.Some 13C-{1H} and 1H NMR peaks have the same integral intensity ratio. These com-plemented the results of 31P-{1H} NMR. The experimental results demonstrates that the PPh3 ligand bound to Cu(6) is not equivalent with the four PPh3 ligands bound toCu(2) ~Cu (5 )- It affords an evidence that the title compound in the solution keepssimilar structure to solid state.