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Electrospray ionization of THF solutions of preformed [K(18-c-6)][M(COT)2] (M = Dy(III), Y(III); COT = C8H82-,18-c-6 = C12H24O6) yields the isolated species [(M(COT)2)n+1 + nK]- with n = 0-3. High-resolution ion mobility spectrometry combined with density functional theory calculations performed for the n = 0-2 aggregates indicate that anionic multidecker stacks interlinked by potassium cations are formed. The alternating metal ions are aligned linearly COT2--M3+-COT2--K+-COT2--M3+-COT2-. The different M3+ ionic radii lead to slight but
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