Facile Access to the Hydrazone Functionalized PdGeS Cluster [{R<sup>N</sup>Ge(μ-S)<sub>3</sub>}<sub>4</sub>Pd<sub>6</sub>] from the Thiogermanate Anion [{R<sup>N</sup>Ge}<sub>2</sub>(μ-S)<sub>2</sub>S<sub>2</sub>]<sup>2−</sup>
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The decanuclear ternary PdGeS cluster [{RNGe(μ-S)3}4Pd6]·MeOH (2·MeOH) has been obtained in high yield by a two-step reaction, involving the derivatization of the carbonyl functionalized adamantane-like [(R1Ge)4(μ-S)6] (R1 = CMe2CH2COMe) with N2H4·H2O, and a subsequent reaction of the resulting hydrazone functionalized thiogermanate (NH3NH2)2[(RNGe)2(μ-S)2S2] (RN = CMe2CH2CMeNNH2, 1) with an acidic solution of (N,N′-tmeda)Pd(NO3)2. Cluster 2 has an elegant molecular structure which can be viewed as an RN ligated ensemble of four edge-sharing [Pd3GeS3] defect hetercubanes that meet at an unoccupied center. Thus, the cluster consists of six square-planar coordinated PdII ions at the vertices of a regular octahedron with four faces capped by four [RNGeS3]3− units. The title compounds were structurally characterized by means of single-crystal X-ray diffraction as well as physical property measurements. Moreover, density functional theory calculations were performed to gain insight into the unique coordination situation of the hydrazone substituent.
