A family of group 13 organometallic macrocyclic phthalates [(MMe2)2(mu-O2C)(2)-1,2-C6H4](2) (where M = Al (1), Ga (2), In (3)) is prepared, and the reactivity of these homologous carboxylates toward various monodentate Lewis bases is investigated. The studies provide the first structurally characterized methylinditun [{(Me2In)(mu-O2C)(2)-1,2-C6H4}{Me2In(THF)}](n), (4) and methylaluminum [{(Me2Al)(mu-O2C)(2)-1,2-C6H4}{Me2Al(py-Me)}](n) (5) ID coordination polymers stabilized by dicarbwrylate ligands as a result of disruption of the parent tetranuclear macrocyclic structural motifs in 3 and 1 by the incoming donor ligands. The molecular and crystal structures of the reported compounds are examined by spectroscopic studies and single-crystal X-ray diffraction.