A new tricompartmental acyclic ligand (H(4)L) was prepared and fully characterized. It reacts with zinc, nickel, and copper(II) acetate to yield [Zn(3)L(OAc)(2)].H(2)O (1.H(2)O), [Ni(3)L(OAc)(2)(MeOH)(2)].2MeCN.2MeOH (2.2MeCN.2MeOH), and [Cu(3)L(OAc)(2)].3H(2)O (3.3H(2)O), respectively. 2.2MeCN.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.H(2)O and 2 are unstable in this medium, both suffering partial hydrolysis to produce single crystals of [Zn(3)L(3-Br-5-Cl-Sal)(2)].2MeCN (4.2MeCN; 3-Br-5-Cl-Sal(-) = 3-bromo-5-chlorosalicylaldehydate) and [Ni(3)L(3-Br-5-Cl-Sal)(2)].2MeCN (5.2MeCN) as one of the reaction byproducts, while 3.3H(2)O gives rise to a reaction of ligand displacement, generating crystals of [Cu(3)L(OMe)(2)].MeOH (6.MeOH). Complexes 2.2MeCN.2MeOH, 4.2MeCN, 5.2MeCN, and 6.MeOH were crystallographically characterized, and these studies demonstrate not only the trinucleating ability of the fully deprotonated L(4-) ligand but also its tendency to induce chirality in the isolated compounds. The magnetic characterization of 2, 3.3H(2)O and 6.MeOH shows that the magnetic coupling between adjacent metal ions is weak, with 2 being ferromagnetic and 3.3H(2)O and 6.MeOH antiferromagnetic.