The existence of cation-vacancy sites in fullerides might lead to long-range ordering and generate a new vacancy-ordered superstructure. The purpose of this work is to search whether or not long-range ordering of vacant tetrahedral sites, namely superstructure emerges in nonstoichiometric fulleride. Therefore, with cation-vacancy sites is synthesized using a precursor method to avoid inadequate stoichiometry control and formation of impurity phases within the target composition. For this purpose, first, phase-pure K6 C60, Ba6 C60 and Cs6 C60 precursors are synthesized. Stoichiometric quantities of these precursors are used for further reaction with C60 to afford . | Turkish Journal of Chemistry Turk J Chem 2020 44 1463-1470 http chem TÜBİTAK Research Article doi kim-2005-78 Synthesis and structural analysis of nonstoichiometric ternary fulleride Havva Esma OKUR KUTAY Department of Chemistry Faculty of Engineering and Natural Sciences Bursa Technical University Bursa Turkey Received Accepted Published Online Final Version Abstract The existence of cation-vacancy sites in fullerides might lead to long-range ordering and generate a new vacancy-ordered superstructure. The purpose of this work is to search whether or not long-range ordering of vacant tetrahedral sites namely superstructure emerges in nonstoichiometric fulleride. Therefore with cation-vacancy sites is synthesized using a precursor method to avoid inadequate stoichiometry control and formation of impurity phases within the target composition. For this purpose first phase-pure K6C60 Ba6C60 and Cs6C60 precursors are synthesized. Stoichiometric quantities of these precursors are used for further reaction with C60 to afford . Rietveld analysis of the high-resolution synchrotron X-ray powder diffraction data of the precursors and confirms that K6C60 Ba6C60 and Cs6C60 are single-phase and they crystallize in a body-centered- cubic structure Im3 as reported in the literature. The analysis also shows that phase can be perfectly modeled using a face-centered cubic structure. No new peaks appear which could have implied the appearance of a superstructure. This suggests that there is no long-range ordered arrangement of vacant tetrahedral sites in . Key words Cation-vacancy solid-state synthesis A6C60 nonstoichiometric fullerides 1. Introduction The intercalated products of fullerides display unique structural magnetic and electronic properties which depend on the amount size and nature of the .