KZrF5 is triclinic (P (1) over bar) with a = 7.370(1) Angstrom, b = 8.
461(1) Angstrom, c = 10.711(1) Angstrom, alpha = 75.04(1)degrees, beta
= 71.57(1)degrees, gamma = 66.13(2)degrees and Z = 6. The crystal str
ucture was refined from 5056 reflections to a conventional R = 0.031 (
R-w = 0.033). The structure is built of layers of corners and edges-sh
aring (ZrF8)-F-IV polyhedra stacking parallel to the (111) plane. Thes
e (ZrF5)(-) layers are held together by potassium ions. Homologous com
pounds have been evidenced for RbZrF5 and MTbF5 (M = K, Rb). Structure
of layered (MMF5)-M-I-F-IV compounds are discussed in term of plane n
ets.