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In this study, we report on the X-ray diffraction analysis of the pentapeptide, Boc-Tyr-d-Ala-Gly-(NMe-Phe)-(Met-O-Me), C35H49N5O9S .1.125H(2)O. This is a protected intermediate in the solution phase synthesis of metkephamid (LY127,623), Tyr-D-Ala-Gly-NMe-Phe-Met-NH2. The peptide crystallizes in the monoclinic space group C2 with two peptide molecules and three solvent (water) molecules in the asymmetric unit. The peptide has an extended conformation similar to other Met-enkephalins