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Treatment of the 1‐ferrocenylethanone thiosemicarbazone ligands (η5‐C5H5)Fe(η5‐C5H4)C(Me)=NN(H)C(=S)NHR [R = H (a), Me (b)] with K2[PdCl4] gave the novel heterometallic octanuclear palladium(II) compounds [Pd{(η5‐C5H5)Fe(η5‐C5H3)C(Me)=NN=C(S)NHR}]4 [R = H (1a), Me (1b)] as tetramers, after deprotonation of the NH group, with the ligands acting as terdentate donors through the [C,N,S] atoms. Treatment with nucleophiles cleaves the tetrameric clusters giving compounds in which splitting only of the Pd−Sbridging bonds has occurred. The strength of the Pd−Schelating bond hinders its cleavage. Thus, treatment of 1a or 1b with Ph2P(CH2)nPPh2 [n = 2 (dppe), 3 (dppp), 4 (dppb)] in a 1:2 molar ratio gave the tetranuclear species 2a−4a and 2b−4b, respectively, and treatment with PPh2R gave the dinuclear compounds 5a−7a and 5b−6b [R = Ph (5a, 5b), Et (6a, 6b), Me (7a)]. The complexes described are the first fully characterized cyclometallated palladium(II) complexes with 1‐ferrocenylethanone thiosemicarbazone ligands. The crystal and molecular structure of compound 5b have been determined by X‐ray crystallography. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004)

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