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The 17 O NMR of bromoperoxidase in Tris buffer at pH 8 treated with 17 O-enriched H 2 O 2 reveals direct binding of peroxide to active site vanadium both in the symmetric and asymmetric modes, the latter possibly due to hydroperoxide. In addition, non-active site HVO 2 (O 2 ) 22- is detected. The results are counter-checked with NMR data on peroxovanadium model compounds.