A polycrystalline sample of YbCoO3 was prepared using a water-soluble complex method at relatively low temperatures. Common chelating ligands such as citric acid were employed for the synthesis of complex-based precursors, followed by thermal decomposition of the precursors at high temperatures. X-ray diffraction data were collected and the crystal structure was refined by the Rietveld method. The structure of YbCoO3 can be described as a sesquioxide C-M2O3-like structure with space group Ia-3 and unit-cell parameter a=10.4470 (2). The Yb3+ and the Co3+ cations are found to preferentially occupy the two nonequivalent 8d and 24d sites, respectively. The two independent atoms Yb/Co have octahedral coordination; however, the degrees of distortion of their coordination polyhedron are different. The relationship between the title compound and the orthorhombic Perovskite structure of YbCoO3 reported in the literature is established.
