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X-ray crystallography To obtain crystal structures of covalent adducts, compounds 5e and 6a were incubated overnight at 37 C with PDE at a 10:1 molar ratio (2 mM compound: 200 M protein) in HEPES buffer (20 mM HEPES, 150 mM NaCl, pH = 7.5) containing 1% DMSO