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The crystal structure of Li[N(CH3)4]2[Co(NO2)6] has been determined at 113 and 293 K. The crystals belong to the P3 m 1 space group. They are built up of [Co(NO2)6] 3-octahedra piled along the 3 axes, with the Li ÷ ions sand-1 in an octahedral first coorwiched between them at ~c dination sphere involving six symmetry-related O atoms from the nitro groups. Both [C0(NO2)6] 3-and LiO6 octahedra exhibit D3a symmetry. On cooling, the unit cell contracts: a 3.21% reduction in volume results from a 1.37% contraction of the a edge and a 0.51% contraction of the c edge. Bond distances and angles from the two analyses are not significantly different. The two N--O distances of the nitro group differ significantly [1.2421 (5) and 1.2265 (4)A, at 113 K, 1.242 (2)

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