The synthesis of 1,1'-bis(N-ter-butyl-N-hydroxyamino)ferrocene 1, is described, and the X-ray analysis showed eclipsed positions of the two ter-butylhydroxyamino groups; this structure can be explained by the interactions of the hydroxyl hydrogens with the nitrogen atoms of the other ter-butylhydroxyamino group. This interaction is maintained in solution and may explain that the oxidation of 1 using Ag2O gave a decomposition reaction instead of the expected 1,1'-bis(N-ter-butylaminoxy)ferrocene. (C) 2002 Published by Elsevier Science B.V.