A noncoordinating hydroxyl group was introduced into a metal-organic framework (MOF) by a procedure involving a protection, complexation, and deprotection (PCD) reaction sequence, and the crystal structure of a novel MOF, [Zn(dhybdc)(bpy)]center dot 4DMF (1), was determined. I did not have an interpenetrated structure. The three-dimensional pores had large apertures. Results showed that the PCD method is a novel synthetic method for the introduction of various functional groups into MOFs.