Abstract
The synthesis of triammonium fulleride (NH4)3C60 by ion exchange of either K3C60 or Rb3C60 with NH4Cl in absolute toluene is reported. According to the Rietveld refinement of a synchrotron radiation-based X-ray diffraction pattern, (NH4)3C60 belongs to the same structure type as both K3C60 and Rb3C60 featuring an fcc lattice with intercalated cations occupying tetrahedral and octahedral cavities of the close-packing formed by fullerene С60 spheres. The ion exchange is incomplete and the final formulation of the product is [(NH4)2.88K0.12]C60. In contrast to earlier suggestions and tabulated ionic radii values, the (NH4)3C60 crystal structure is characterized by a lattice parameter slightly smaller than that of K3C60. A similar reaction between K4C60 and NH4Cl proceeds differently involving the redox step and affords [(NH4)0.48K2.52]C60 again emphasizing the fact that ammonium and potassium in the fulleride phase tend to form substitutional solid solutions. According to low-frequency inductive method, all (NH4)3C60-related phases studied are superconducting with similar temperatures of the superconducting transition around Tc = 16.4 K.
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