6,6-dihydropenicillanate S,S-dioxide 5 was prepared and determined by X-ray crystallography. Single-crystal X-ray diffraction analysis reveals that the molecular structure of compound 5b is enantiomerically pure. The crystal belongs to orthorhombic, space group P2 1 2 1 2 1 , with unit cell parameters a = 6.5366 Å, b = 10.7649(9) Å, c = 15.5879(13) Å, V = 1096.86(16) Å 3 , D x = 1.491 g cm −3 , Z = 4, T = 296(2)K, F(000) = 520, R 1 = 0.0401, and wR 2 = 0.1200. Absolute structure parameter is 0.02(10).
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