The 2-hydroxybenzaldehyde [(1E)-1-pyridin-2-ylethylidene]hydrazone (HL 2 ) ligand was prepared and its rhenium(I) complexes [ReX(CO) 3 (HL 2 )] were obtained by reaction with fac-[ReX(CO) 3 (CH 3 CN) 2 ] (X = Cl, Br) in chloroform. The compounds were characterized by elemental analysis, mass spectrometry, and IR, UV/Vis, and 1 H NMR spectroscopy. Furthermore, the structures were also established by X-ray diffraction. The aromatic rings are almost coplanar in the ligand structure, and the configuration around the hydrazone group is strongly dominated by the presence of an intramo-

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The reaction of [ReX(CO)5] with thiosemicarbazones H2L(R) derived from beta-keto esters (X = Cl, Br; R = Me, Ph) allowed the isolation of cyclic trimeric complexes [Re3(pyz(R))3(CO)9], where pyz(R) is the pyrazolonate corresponding to the thiosemicarbazone. Electron spray ionization Fourier transform ion cyclotron resonance mass spectrometry (ESI-FTICR-MS) monitoring of the reactions of H2L(Ph) in toluene confirmed that the trimer was formed in the reaction mixture and no higher oligomer was detected. These studies, together with the X-ray structures of the trimeric complexes, afford new insight into the factors influencing the self-assembly of pyrazolonaterhenium(I) complexes.

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