... SOC. A 1970, 2087. 0020-1669/84/1323-0373$01.50/0 0 1984 American Chemical Society Page 2. 374 Inorganic Chemistry, Vol. 23, No. ... At this point, the mixture was doubled in volume with cold oxygen-free H 2 0 and allowed to cool sealed under N, in a freezer overnight. ...