A New Route to Neodymium(II) and Dysprosium(II) Iodides

Abstract

Microcrystalline molecular iodides of neodymium(ii) and dysprosium(ii), LnI 2 (THF) 5 and LnI 2 (DME) 3 (Ln Dy, Nd) have been obtained by heating a mixture of the appropriate metal with iodine, subsequently dissolving the products in THF or DME, and crystallization at low temperature. Prolonged drying of DyI 2 (THF) 5 in vacuum yielded a violet powder of composition DyI 2 (THF) 3 . These crystalline complexes are thermally stable, but in the solution their stability is lower. Both NdI 2 and DyI 2 , as well as TmI 2 , dissolve in liquid NH 3 to give unstable blue solutions.

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“…It should be noted that TmX 2 , DyX 2 and NdX 2 (X = Cl, Br, I) had all been identified previously in the solid state and had been shown to contain divalent ions [64,65]. Encouraged by the Tm 2+ result, the synthetic method of Bochkarev and Fagin [56] was used in our lab to obtain crystallographic data on the first molecular complex of Dy 2+ , Eq. (6) [66].…”

“…Although initial attempts to obtain crystallographic data on samples of "TmI 2 were unsuccessful, preparation of a fresh sample made in our lab by the Bochkarev method [56], provided the first example of a molecular divalent thulium complex, TmI 2 (DME) 3 , Eq. (3) [57].…”

“…However, for the next three years neither my lab nor the Bochkarev lab obtained any significant new reductive reactivity from this Tm 2+ complex [56,[58][59][60]61]. The intensely colored green compound reacted quickly with many substrates to give colorless Tm 3+ products, but TmI 3 was the only product readily identified.…”

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“…At a final stage of purification THF and ether were treated with NdI 2 for 10 min before use and collected in a reaction vessel by condensation in vacuum. N-(2,6-Di-isopropylphenyl)-phenanthren-o-iminoquinone [11] and the diiodides LnI 2 (Ln ¼ Nd, Dy) were prepared using procedures described previously [14]. Carbon, hydrogen, and nitrogen analyses were performed by direct combustion with Euro EA 3000 Elemental Analyser.…”

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“…(3) This was a very exciting development since Tm 2+ was more reactive than the Sm 2+ ion that had given a broad range of new chemistry to the lanthanide area. However, for the next three years neither my lab nor the Bochkarev lab obtained any significant new reductive reactivity from this Tm 2+ complex [56,[58][59][60]61]. The intensely colored green compound reacted quickly with many substrates to give colorless Tm 3+ products, but TmI 3 was the only product readily identified.…”