Some new complexes of rhenium containing monocoordinating acetylacetone viz. [Re(NO)(acac)2(Cl)H2O], Re(NO)(acac)3(acacH)(H2O)2 have been synthesized by reacting acetylacetone with either Re(NO)Cl3 · H2O or Re(NO)(OH)3 · H2O. The preparation of [Re(NO)(py)(acac)2(Cl) · H2O], [Re(NO)(acac)(OH)(Cl) · H2O], [Re2(NO)2(acacH)3(acac)2 · Cl4], [Re(NO)(acac)2(OH) · H2O] · 2 H2O have also been described. These complexes were characterized through their elemental analyses, u.v., vis, i.r., 1Hn.m.r., magnetic, and conductance data. Copyright © 1987 Verlag GmbH & Co. KGaA, Weinheim