[NBu4][BPh4] to the reaction mixture to inhibit ion pairing as was done in other Sm II reactions. It is important to note that while the CfI3•nH2O (n ≤ 6) is obviously hydrated that this material has been dried in vacuo, and this process is known to convert hexahydrates to monohydrates. CfI3•nH2O (n ≤ 6) rapidly decomposes in the presence of O2 or even excess water (as does Cf(18crown-6)I2), thus these reactions are conducted in a glovebox under an argon atmosphere. No further removal of coordinated or lattice water is necessary because the Al/Hg amalgam also removes the water from the reaction mixture via its reduction and subsequent precipitation of few minutes to a peach-brown color as shown in Figure . We have evidence that [Cf III (18crown-6)(H2O)(CH3CN)I]I2 is first reduced to [Cf II (18-crown-6)(H2O)2(CH3CN)]I2, and that the water is lost to the amalgam to yield the desired Cf(18-crown-6)I2 complex. It should be noted that if the mother liquor is removed from the amalgam at this stage its color will revert back to the original yellow-green color of the starting solution. While crystals can be isolated from this solution, they contain a mixture of Cf II and Cf III in the form of [Cf(18-crown-