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We report on the syntheses and single-crystal structure determinations of the compounds  A   2 SiF 6  ( A  = Tl, Rb, Cs). In comparison to the previous powder-based structure models we achieved more precise atom positions and distances. The compounds crystallize in the K 2 PtCl 6  structure type, space group  Fm3   ‾$&amp;#x203e;{3}$m  (No. 225,  cF 36) with  a  = 8.4749(10) Å,  V  = 608.7(2) Å 3 ,  Z  = 4 at  T  = 100 K for Tl 2 SiF 6 ,  a  = 8.3918(10) Å,  V  = 591.0(2) Å 3 ,  Z  = 4 at  T  = 100 K for Rb 2 SiF 6 , and  a  = 8.8638(11) Å,  V  = 696.4(3) Å 3 ,  Z  = 4 at  T  = 200 K for Cs 2 SiF 6 . For the compound Tl 3 [SiF 6 ]F we present a previously unknown tetragonal modification and correct the crystal structure of its trigonal modification to hexagonal. The tetragonal one crystallizes in the (NH 4 ) 3 [SiF 6 ]F structure type, space group  P 4/ mbm  (No. 127,  tP 22) with  a  = 8.0313(8),  c  = 5.8932(6) Å,  V  = 380.13(7) Å 3 ,  Z  = 2,  T  = 298 K, and the crystal structure of the hexagonal modification is best described in space group  P 6 3   mc  (No. 186,  hP 22) with  a  = 7.8248(4),  c  = 6.8768(4) Å,  V  = 364.64(4) Å 3 ,  Z  = 2,  T  = 100 K.

Single-crystal structures of A 2 SiF 6 ( A = Tl, Rb, Cs), a better structure model for Tl 3 [SiF 6 ]F, and its novel tetragonal polymorph