The reaction of trialkylaluminum compounds with diphenic acid in a 2:1 molar ratio results in the formation of novel dialkylaluminum dicarboxylates [Et4Al2(OOCC12H8COO)](3) (1) and [Bu4Al2(OCCC12H8CCO)](2) (2). Molecular structures of the compounds have been determined by X-ray crystallography. Compound 1 is a hexamer with a skeleton framework consisting of four fused heterocyclic rings, one 27-membered and three Al2O4C2 8-membered. Compound 2 is a centrosymmetric tetramer with a skeleton framework consisting of three fused heterocyclic findings, one 18-membered and two Al2O4C2 8-membered. The structures of the compounds reveal R4Al2O4C2 subunits, each linked through diphenyl C12H8 bridges. Each of the aluminum atoms is bonded to two alkyl groups and two oxygen atoms originating from two different dicarboxylate moieties.