A new tricompartmental acyclic ligand (H4L) was prepared and fully characterized. It reacts with zinc, nickel, and copper(II) acetate to yield [Zn3L(OAc)(2)]center dot H2O (1 center dot H2O), [Ni3L(OAc)(2)(MeOH)(2)]center dot 2MeCN center dot 2MeOH (2 center dot 2MeCN center dot 2 MeOH), and [Cu3L(OAc)(2)]center dot 3H(2)O (3 center dot 3H(2)O), respectively. 2 center dot 2MeCN center dot 2MeOH precipitates as single crystals, which lose the solvates upon drying to give 2. The reactivity of the acetate complexes in a methanol/acetonitrile basic medium in air was investigated. Thus, 1 center dot H2O and 2 are unstable in this medium, both suffering partial hydrolysis to produce single crystals of [Zn3L(3-Br-5-Cl-Sal)(2)]center dot 2MeCN (4 center dot 2MeCN; 3-Br-5-Cl-Sal(-) = 3-bromo-5-chlorosalicylaldehydate) and [Ni3L(3-Br-5-Cl-Sal)(2)]center dot 2MeCN (5 center dot 2MeCN) as one of the reaction byproducts, while 3 center dot 3H(2)O gives rise to a reaction of ligand displacement, generating crystals of [Cu3L(OMe)(2)]center dot MeOH (6 center dot MeOH). Complexes 2 center dot 2MeCN center dot 2MeOH, 4 center dot 2MeCN, 5 center dot 2MeCN, and 6 center dot MeOH were crystallographically characterized, and these studies demonstrate not only the trinucleating ability of the fully deprotonated L4- ligand but also its tendency to induce chirality in the isolated compounds. The magnetic characterization of 2,3 center dot 3H(2)O and 6 center dot MeOH shows that the magnetic coupling between adjacent metal ions is weak, with 2 being ferromagnetic and 3 center dot 3H(2)O and 6 center dot MeOH antiferromagnetic.