High-energy X-ray diffraction measurements were carried out at 26 A degrees C for aqueous 1.0, 2.0 and 2.05 mol% disodium adenosine 5'-triphosphate (ATP) and 2.0 and 2.05 mol% disodium adenosine 5'-diphosphate (ADP) solutions in order to obtain direct experimental information on the intramolecular conformations of ATP and ADP molecules in aqueous solutions. Observed interference terms were analyzed in terms of the intramolecular geometry of the ATP and ADP molecules. Dihedral angles between adenine and the ribose group (t (1)), ribose-ring and methylene group of ribose (t (2)), and the methylene group of ribose and triphosphate (or diphosphate) group (t (3)), were determined through the least-squares fitting procedure of the observed interference term.