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The new supertetrahedral compounds  M SiAs 2 ,  M GaSiAs 3  and  mC / tI - M  4 Ga 5 SiAs 9  ( M  = Sr, Eu) have been synthesized by solid-state reactions at high temperatures. The structures were determined by single crystal or powder X-ray diffraction.  M SiAs 2  and  M GaSiAs 3  crystallize in the monoclinic TlGaSe 2 - and RbCuSnS 3 -type structures, respectively (space group  C 2/ c ). These are topologically hierarchical variants of the tetragonal HgI 2 -type structure with stacked layers of T2 or T3 supertetrahedra. The T4 compounds  M  4 Ga 5 SiAs 9  are dimorphic and form new structure types in the space groups  C 2/ c  and  I 4 1 / amd , respectively. The latter exhibits coinciding layer stacking as known from tetragonal HgI 2 . The T4 compounds close the gap between the longer known T2 types and the recently reported compounds with T5 and T6 supertetrahedra. Measurements of the optical band gap, electrical resistivity and Hall Effect support the semiconducting nature of  M  4 Ga 5 SiAs 9 . Magnetization measurements confirm Eu 2+  in Eu 4 Ga 5 SiAs 9  and indicate ferromagnetism below  T  = 2 K.

New layered supertetrahedral compounds T2- M SiAs 2 , T3- M GaSiAs 3 and polytypic T4- M 4 Ga 5 SiAs 9 ( M = Sr, Eu)