We report the synthesis of a single-phase sample of the superconducting crystalline approximant Au64.0Ge22.0Yb14.0 and present a structure model refined by Rietveld analysis for X-ray diffraction data.Quasicrystals (QCs) are metallic alloys that possess long-range, quasi-periodic structures with diffraction symmetries forbidden to conventional crystals, while approximant crystals (ACs) are alloys whose composition is close to that of QCs and whose unit cell has atomic decorations similar to those of the QCs. In this Short Note, we report a detailed structure analysis of the AGY(I) AC. For AGY(II), we are unable to provide a structure model owing to the lack of a single-phase sample.Polycrystalline samples of the optimally compositioncontrolled compound Au 64.0 Ge 22.0 Yb 14.0 were synthesized, and their structures were characterized by powder X-ray diffraction using Cu Kα-radiation. Details of the sample preparation and X-ray diffraction analysis experiments were described in Refs. 3 and 1, respectively. Figure 1 shows a powder X-ray diffraction pattern of AGY(I), indicating the body-centered cubic structure (space group Im3) with a lattice parameter a = 1.4724(2) nm. The Rietveld analysis successfully converged with R-factors, R wp = 5.41%, R I = 0.95%, and R F = 0.59% (for the structure parameters, see Table I), assuming that the cluster center is occupied by an orientationally disordered tetrahedron. 4 This suggests that the alloy has a similar structure to the Tsaitype 1/1 AAY AC. This structure model contains 9 crystallographic sites and includes 174.1 atoms in total in a unit cell, which corresponds to the chemical * E-mail: deguchi@edu3.phys.nagoya-u.ac.jp Figure 2 shows the structure model for the AGY(I) AC. As shown in Fig. 2(a), the cluster center (M7 site) is occupied by Au atoms with an occupancy of 26.9%. The complicated shape of the cluster center, in which 4 atoms in total are ideally included, indicates an average of variously oriented tetrahedrons. The second shell [ Fig. 2(b)] is a dodecahedron, in which there are Au/Ge mixed sites named M2 and M4 sites. The third shell [ Fig. 2(c)] is an icosahedron, in which Yb ions exclusively occupy the Yb1 site. The icosahedron is surrounded by an icosidodecahedron [ Fig. 2(d)] in which the M1 and M6 sites are almost occupied by Au atoms and the M8 site is occupied by Ge with an occupancy of 95%. These shells, i.e., the dodecahedron, icosahedron, and icosidodecahedron compose the so-called Tsai-type cluster. Finally, Tsaitype clusters are embedded in the cage composed of M3 and M5 [ Fig. 2(e)]. The periodic arrangement of this cage 1