| Summary: | The thermal decomposition of (XMebpyH)<sub>3</sub>(H<sub>3</sub>O)[W(CN)<sub>8</sub>]·3H<sub>2</sub>O (where XMebpy denotes 4Mebpy 4,4′-dimethyl-2,2′-bipyridine or 5Mebpy 5,5′-dimethyl-2,2′-bipyridine) in glycerol results in the coordination of XMebpy. Salts of the anion formula [W(CN)<sub>6</sub>(XMebpy)]<sup>2−</sup> were isolated for PPh<sub>4</sub><sup>+</sup> and/or AsPh<sub>4</sub><sup>+</sup> cations as well as for K<sup>+</sup>, Rb<sup>+</sup>, and Cs<sup>+</sup> ones. X-ray single-crystal analyses for tetraphenyl-phosphonium and tetraphenyl-arsonium cations are described. IR, UV-Vis, and cyclic voltammetry data are presented. The results were compared with those for [W(CN)<sub>6</sub>(bpy)]<sup>2−</sup> (bpy = 2,2′-bipyridine) ion salts.
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