The reactions of l-ascorbic acid in aqueous Co I I and Gd I I I solutions were investigated at pH values of 2, 6 and 12. IR spectral studies revealed that the initially formed metal-ascorbates slowly decompose to the solid oxalate complexes in a pH-independent manner. The compositions of the cobalt oxalates were defined as CoC 2 O 4 2H 2 O and those of Gd I I I showed variations due to the stereochemical changes in the precursor ascorbate complexes related to pH. X-ray crystal analyses were performed and the structure of Gd 2 (C 2 O 4 ) 3 6H 2 O is reported for the first time.