The structure of nitrosonium octafluoroxenate(VI), 2NOF \cdot XeF6, has been determined by means of single-crystal x-ray counter methods (R-index = 0.046, weighted R-index = 0.042). The space group is Pnma, with a = 8.914(10) angstroms, b = 5.945(10) angstroms, and c = 12.83(2) angstroms (the numbers in parentheses are the standard deviations to the least significant digit or digits); the calculated density (ρ ) is 3.354 grams per cubic centimeter, and there are four formula units per unit cell. The material consists of well-separated NO+ and (XeF8)2- ions; the structural formula is thus (NO)2 (XeF8). The anion configuration is that of a slightly distorted Archimedean antiprism. The observed distortion appears incompatible with a lone-pair repulsion model. Xenon-fluorine bond lengths of 1.971(7), 1.946(5), 1.958(7), 2.052(5), and 2.099(5) angstroms were found.