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Reduction of C 60  with the alkali metals A = K, Rb and Cs in tetrahydrofuran as a solvent and addition of [2.2.2]crypt [1], dimethylformamide and cyclohexane lead to the formation of crystalline samples of [A([2.2.2]crypt)] 2 [C 60 ](C 6 H 12 ) 2 (C 3 H 7 NO) 2 (C 4 H 8 O) 2  (A = K, Rb, Cs) 1a, 1b and 1c as major fractions. As a by-product of compound 1a, a second minor fraction containing [K([2.2.2]crypt)] 2 [C 60 ](C 3 H 7 NO) 4  2 was obtained. The structures of the four compounds have been determined by single-crystal X-ray analyses. The [C 60 ] 2−  dianions are predominantly ordered. As the main structural motif the structures of compounds 1a, 1b and 1c contain pseudo-hexagonal layers of [C 60 ] 2−  dianions. Compound 1c contains a rare example of a Cs +  sequestering [2.2.2]crypt molecule. The packing of the ionic units in compound 2 also shows layers of distorted hexagons formed by [C 60 ] 2−  dianions which arranged in pairs with short contacts of 10.3 Å between their centers of gravity.

Synthesis and Crystal Structure Analysis of C 60 Fulleride Dianions in Solvates of [A([2.2.2]crypt)] 2 [C 60 ] (A = K, Rb, Cs)