Precipitation reactions using ammonia yield a novel cobalt hydroxide phase that is structurally and compositionally similar to ␣-nickel hydroxide. The use of other synthetic methods yields the well-known -Co(OH) 2 . The slab composition, mode of anion inclusion, and thermal behavior of the hydroxides obtained by ammonia precipitation are similar to those of ␣-nickel hydroxide; however, the materials are poorly ordered. A DIFFaX simulation of the powder X-ray diffraction patterns offers the best visual match with the observed patterns for a 50% stacking disorder and a disc radius between 100 and 1000 Å.