| Summary: | The reaction of diazotetracyanocyclopentadiene with copper powder in the presence of NEt<sub>4</sub>Cl yields, unexpectedly, besides the known NEt<sub>4</sub>[C<sub>5</sub>H(CN)<sub>4</sub>] (3), the NEt<sub>4</sub> salt of octacyanofulvalenediide (NEt<sub>4</sub>)<sub>2</sub>[C<sub>10</sub>(CN)<sub>8</sub>] (<b>5</b>), which can be transformed via reaction with AgNO<sub>3</sub> to the corresponding Ag<sup>+</sup> salt (<b>4</b>), which in turn can be reacted with KCl to yield the corresponding K<sup>+</sup> salt <b>6</b>. The molecular and crystal structures of <b>4</b>–<b>6</b> could be determined, and show a significantly twisted aromatic dianion which uses all its nitrile groups for coordination to the metals; <b>4</b> and <b>6</b> form three-dimensional coordination polymers with fourfold coordinated Ag<sup>+</sup> and eightfold coordinated K<sup>+</sup> cations.
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