The crystal structure of ReB 2 has been determined from powder data. The unit cell is hexagonal; a=2.900 and c=7.478 A; there are two ReB 2 units per unit cell. The structure may be described in terms of alternating layers of rhenium and boron atoms; the former are planar, the latter are puckered. The two boron atoms show up clearly in difference maps (@z, 2x, Zobs. --@z, 2x, ZRe)" B-B bond lengths are 1.82 ~; shortest Re-B distance are 2.23 and 2.26 A.
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Placa et al. (1962) studied this question.