terpretation of the 21 K phase transition; methyl hydrogen ordering is a possibility, if the acetate ions lie on twofold axes. On the other hand, the reported variability in the magnitude of the 21 K Cp-curve peak may well be related to the variability in diffraction pattern and domain size, found by us.We thank Professor E. F. Westrum for suggesting this problem and Dr Magda E1-Fass for performing the high-temperature crystallizations.References FRANZOSINI,P., PLAUTZ, W. A. & WESTRUM, E. F. (1983 The molecule is situated on a mirror plane giving a cubane structure of Na and H atoms. The structure thus consists of two interpenetrating tetrahedra of Na and hydridic H atoms at alternate corners of the very distorted cube. One of the Na atoms which lies on the mirror plane is coordinated to an ether molecule. Each hydridic H is bonded to the B of one trimethylboron group, thus forming a larger tetrahedron of B atoms. The tetrameric units are stacked along the b direction via interactions between the two Na atoms on the mirror plane and methyl H atoms of trimethylboron units in neighbouring tetramers. These chains are loosely held together in a two-dimensional network.Introduction. Hydrides of the type MBR 3 H (M = alkali metal, R = alkyl) are readily prepared from MH and R3B (e.g. Brown & Krishnamurthy, 1978;Brown,