A detailed study of barium aluminate glycolate, Ba[Al-2(C2H4O2)(4)], a compound in which aluminum is in 5-coordination with respect to oxygen has been carried out using XRD, FTIR, solid-state NMR, and ESCA. There is a unique set of ESCA core-level binding energies for this material, between those for compounds containing 6- and 4-coordinate A1. NMR detects the presence of a 6-coordinate Al impurity in the "distillation" Ba-AP compound, but the Al(2p) peaks for compounds containing 5- and 6-coordinate Al are too close to be resolved by ESCA.