. Can. J. Chem. 69, 2122 (1991).The reaction of tin(I1) fluoride with fluorosulfuric acid has been shown to produce tin(I1) bisfluorosulfate. Crystals of S~( O S O Z F )~ are monoclinic, space group P21/c with a = 5.195(1), b = 9.709(1), c = 13.861(1) A, P = 110.12(1)", Z = 4, R = 0.029, and R, = 0.030 for 1461 unique reflections. The structure consists of a three-dimensional framework of fluorosulfate groups linked by 0-Sn-0 bridges with the two crystallographically independent fluorosulfates acting as tridentate bridging ligands between tin atoms. There are four short bonds (Sn-0 = 2.338(3), 2.350(3), 2.398(4), and 2.427(3) A) and two longer ones (Sn-0 = 2.695(3) and 2.702(3) A) around tin. The four short bonds have a disphenoidal, A L E , primary geometry with the lone pair occupying an equatorial site. If the two longer interactions are also considered the geometry is distorted octahedral, AX4Y2E. Two more non-bonding contacts of 3.420 (4)