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Single-crystals of Ca 14 Al 10 Zn 6 O 35  suitable for structural investigations were grown from slow cooling of a melt with the same chemical composition in the range between 1300 and 1000 °C. Diffraction experiments performed at ambient temperature yielded the following crystallographic data: space group  F 23,  a  = 14.8468 (6) Å,  V  = 3272.6 (2) Å 3 ,  Z  = 4. Structure determination and subsequent least‐squares refinements resulted in a residual of  R (| F |) = 1.49% for 753 independent observed reflections and 55 parameters. The chiral structure is based on a tetrahedral framework of corner sharing (Zn,Al)O 4 -tetrahedra. Zn–Al-distributions among the four crystallographically independent T-sites have been studied. A detailed topological analysis based on natural tiles is presented. Actually, the net can be constructed from a total of four different cages (tiles). The largest cavities (face symbol: [3 16 . 6 16 ]) have volumes of about 680 Å 3  and host [AlO 6 ][Ca 14 O 36 ] heteropolyhedral clusters consisting of a central [AlO 6 ] – octahedron surrounded by [CaO 6 ]- and [CaO 7 ]-groups. The calcium cations provide linkage to the tetrahedral framework, in other words, the [AlO 6 ]-unit in the barycenter of the cluster is not directly connected to the framework. Furthermore, thermal expansion has been studied in the interval between 25 and 790 °C using  in-situ  high‐temperature single‐crystal diffraction. No indications for a structural phase transition were observed. From the evolution of the lattice parameters the thermal expansion tensor has been obtained. The response of the structure to variable temperature has been discussed.

High-temperature behavior and structural studies on Ca 14 Al 10 Zn 6 O 35