The synthesis of the metal carboxylates M(II)(1,2-C2B10H11CO2)2, M = Zn, Cu, Ni, and Mo, and M(II){1,2-C2B10H10-(CO2)2}, M = Cu and Ni, are reported. All have been characterized spectroscopically and by elemental analysis. M(II)(1,2-C2B10H11CO2)2, M = Cu and Ni, have been structurally characterized in the solid state by single-crystal X-ray diffraction as Cu2(C2B10H11CO2)4(THF)2 (P2(1)/n, a = 10.327(2) angstrom, b = 13.428(2) angstrom, c = 19.605(6) angstrom, beta = 90.58(2)., V = 2718.5(12) angstrom3, d(calcd) = 1.246 g/cm3, Z = 2) and Ni2(C2B10H11CO2)4(THF)4-EtOH.H2O (Pca2(1), a = 22.403(4) angstrom, b = 13.996(3) angstrom, c = 23.104(5) angstrom, V= 7244(3) angstrom3, d(calcd) = 1.134 g/cm3, Z = 4). The thermolyses of Cu2(C2BoH11CO2)4(THF)2, Cu{1,2-C2B10H10(CO2)2}, Ni2(C2B10H11CO2)4(THF)4.H2O.2THF, and Ni{1,2-C2B10H10(CO2)2} have been investigated by weight loss, infrared spectroscopy, and isolation of the volatile products. The solid-state products have been characterized by elemental analysis, powder X-ray diffraction of crystallized materials, and X-ray photoelectron spectroscopy. This work reveals some further aspects of cluster substituent effects and emphasizes the importance of cluster-central metal link stability relative to cluster stability in making useful solids from linked cluster precursors.