The reactions of L-ascorbic acid in aqueous Cd-II and Gd-III 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 CoC2O4 . 2H(2)O and those of Gd-III 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(C2O4)(3) . 6H(2)O is reported for the first time. (C) 1997 Elsevier Science Ltd.