Four compounds consisting of molecular loops formed from two quadruply bonded Mo-2(DAniF)(2) (DAniF = N,N'-di-p-anisylformamidinate) units Linked by two dicarboxylate anions have been prepared in high purity and essentially quantitative yields. These compounds have been characterized by crystallography and NMR spectroscopy and display electrochemical behavior dependent on the nature of the dicarboxylate anion. However, the electronic communication between the two Mo-2(4+) units is not strong. As denoted by the dicarboxylate linkers, the compounds are malonate, 1, 1,4-phenylendiacetate, 2, homophthalate, 3, and trans-cyclopentane-1,2-dicarboxylate, 4.