Location of Ge and extra-framework species in the zeolite ITQ-24

The germanosilicate ITQ-24 (IWR framework type) was synthesized in fluoride medium using 1,3,5-tris(1,2-dimethylimidazolium) benzene as the structure directing agent (SDA). A structure analysis of the as-synthesized ITQ-24 material using synchrotron powder diffraction data and difference electron density calculations have allowed the fluoride ions and the germanium atoms to be located and the conformation of the SDA to be determined. The benzyl ring is perpendicular to the b axis with the three imidazolium moieties forming a “T-shaped” arrangement. Ge atoms replace some of the Si in the double-4-ring (d4r) and in one of the single-4-rings (s4r). The other s4r contains only Si. Fluoride ions are in the d4r units. Initially, the space group Cmmm (highest possible symmetry) was assumed, but the framework geometry was strained. An independent evaluation of the symmetry using the powder charge flipping algorithm in Superflip led to a successful refinement with reasonable geometry and a refined composition of |[(C_6H_3)(C_7H_(10)N_2)_3]_2F_2|[Si_(40.2)Ge_(15.8)O_(112)] in the space group Pban.