1,3,5,7-Tetrakis(4-iodophenyl) adamantane was reacted with 2-methyl-3-butyn-2-ol and phenylacetylene under Pd-catalyzed Hecb coupling conditions to give the two corresponding tetraacetylene derivatives. Deprotection of the first gave the derivative with free terminal acetylenes. Thermal cure of both acetylene-containing monomers was monitored by FTIR. The cure products were then characterized by solid-state C-13 cross-polarization magic-angle spinning (CP/MAS) nuclear magnetic resonance (NMR) spectroscopy. This technique was combined with dipolar dephasing, in which resonances that are protonated are differentiated from those which are nonprotonated, to help clarify product Composition. Both NMR and FTIR confirmed the presence of adamantane in the otherwise all-aromatic structures. TGA analysis indicated that these highly cross-linked materials began to degrade at ca. 450 and 490 degrees C, respectively, in air, confirming their excellent thermooxidative properties.