Recrystallization of (02N)&H from dioxane yields the triple aggregate (02N)3CH...0(CH2CH2)*0...HC(N02)3 with the shortest C(H)-.O distances reported so far of 293.7(1) pm.Studies aimed at isolation and structure determination of aci-nitromethane tautomers [R2C=N(O)OHlnl have included trinitromethane, cube-shaped crystals of which, (cubic space group Pa-3/205) with melting point 298.5 K, can be grown by 10 mbar sublimation at 281 K.273 Attempts to crystallize from dioxane solution, however, yielded white needles, which after 10-2 mbar sublimation melted at 316.5 K and also can be obtained from HCC13 on n-pentane infusion.2.4 Their structure analysis (Fig. 1) took us by surprise: instead of an expected polymorphic modification of (02N)&H, the CH...O bridged double adduct to dioxane was detected.t

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