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The title compounds, C 9 H 12 O 6 and C 10 H 14 O 6 , were formed by careful hydrolysis of the corresponding diethyl esters. Their single crystals were grown from an ethyl acetate/hexane mixture. Crystals of both compounds have monoclinic ( P 2 1 ) symmetry with a single mol-ecule in the asymmetric unit. Both crystal structures are very similar and display four -CO-OH⋯O=C(OH)- hydrogen bonds, forming a two-dimensional double-layered framework.

(2R,3R)-1,4-Dioxaspiro[4.4]nonane-2,3-dicarboxylic and (2R,3R)-1,4-dioxaspiro[4.5]decane-2,3-dicarboxylic acids