Abstract A precise structural determination of KPbCr 2F 9 was carried out. The symmetry is orthorhombic with a = 9.81(5), b = 5.412(3), c = 13.93(1) Å, and Pnma. The structure was refined from 1285 X-ray reflections by full-matrix least squares to an R = 0.041. The lattice is made up of double chains (Cr 2F 9) 3 n− n running along the b axis with Pb and K atoms ensuring its cohesion. The results of the magnetic studies are reported and discussed.