| Summary: | In the construction of heterobimetallic coordination polymers based on dithiocarbamato–carboxylate (DTCC ligands), platinum as a thiophilic metal center can be replaced by the cheaper nickel or palladium. The compounds Zn[Pd(HL)<sub>2</sub>] and Zn<sub>2</sub>[M(L)<sub>2</sub>] (M = Ni, Pd; L = {SSC-N(CH<sub>2</sub>COO)<sub>2</sub>}<sup>3−</sup>) were prepared in a sequential approach starting from K<sub>3</sub>(L). The products were characterized by IR and NMR spectroscopy, thermal analyses, and single-crystal X-ray diffraction. The products decompose under nitrogen between 300 and 400 °C. Zn[Pd(HL)<sub>2</sub>] · 6H<sub>2</sub>O forms polymeric chains in the solid state, and the Zn<sub>2</sub>[M(L)<sub>2</sub>] · 14H<sub>2</sub>O (M = Ni, Pd) exhibit two-dimensional polymeric structures, each being isotypic with the respective Zn/Pt analogs. While the carboxylate groups in all these products are coordinated to zinc in a κ<i>O</i>-monodentate mode, a structural variant of Zn<sub>2</sub>[Ni(L)<sub>2</sub>] having κ<i>O</i>:κ<i>O</i>′-briding carboxylate groups was also obtained. Exchange of the metal sites in the two Ni/Zn compounds was not observed, and these compounds are therefore diamagnetic.
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