The reaction of 1,3,5-benzenetricarboxylic acid (H(3)BTC) with ZnSO(4).6H(2)O in a DMF-water solution afforded two new metal-organic frameworks [Zn(6)(mu(3)-OH)(2)(BTC)(4)(DMF)(2.5)(H(2)O)(2)].[Zn(H(2)O)(3)(DMF)(3)].3.1H(2)O (1) and Zn(2)(HBTC)(BTC)(H(2)O)(3)].DMA.3H(2)O (2). Both compounds are thermally stable and can be prepared reproducibly. Rehydration experiments on compound 2 demonstrate reversible dehydration and rehydration while 1 rehydrates to a different crystalline material. Network analysis revealed a binodal (3,6)-net for 1 and a (3,5)-net for 2, both rare topologies.