Abstract
X-ray structural analyses have been carried out on the 5-nitro-1,1,3,3-tetramethylisoindolin-2-yloxyl free radical (NTMIO) and its precursor 5-nitro-1,1,3,3-tetramethylisoindoline (NTMI). A mixed single crystal of about 2% NTMIO in NTMI has been prepared and subjected to a detailed ESR examination. The X-ray analyses of NTMIO and NTMI showed that the two have different crystal habits but the dimensions of the two molecules are almost identical hence a small amount of NTMIO in NTMI would not be expected to perturb the lattice of the latter. The unit cell of NTMIO shows that the packing of the structure is normal and that there are no intermolecular distances below 3.41 A showing that hydrogen bonding is not present. The bond distances and angles of the heterocyclic ring of NTMIO are generally more closely related to saturated rather than to unsaturated five-membered ring nitroxyl radicals. ESR parameters are compared for TMIO in solution, in frozen solution and in a single crystal of NTMI.
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