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Niobium(V) chloride

Niobium(V) chloride, also known as niobium pentachloride, is a yellow crystalline solid. It hydrolyzes in air, and samples are often contaminated with small amounts of NbOCl<sub>3</sub>. It is often used as a precursor to other compounds of niobium. NbCl<sub>5</sub> may be purified by sublimation.

Structure and properties

Niobium(V) chloride forms chloro-bridged dimers in the solid state (see figure). Each niobium centre is six-coordinate, but the octahedral coordination is significantly distorted. The equatorial niobium–chlorine bond lengths are 225&nbsp;pm (terminal) and 256&nbsp;pm (bridging), whilst the axial niobium-chlorine bonds are 229.2 pm and are deflected inwards to form an angle of 83.7° with the equatorial plane of the molecule. The Nb–Cl–Nb angle at the bridge is 101.3°. The Nb–Nb distance is 398.8&nbsp;pm, too long for any metal-metal interaction. NbBr<sub>5</sub>, NbI<sub>5</sub>, TaCl<sub>5</sub> TaBr<sub>5</sub> and TaI<sub>5</sub> are isostructural with NbCl<sub>5</sub>.

Preparation

Industrially, niobium pentachloride is obtained by direct chlorination of niobium metal at 300 to 350&nbsp;°C:

2Nb + 5Cl<sub>2</sub> → 2NbCl<sub>5</sub>

In the laboratory, niobium pentachloride is often prepared from Nb<sub>2</sub>O<sub>5</sub>, the main challenge being incomplete reaction to give NbOCl<sub>3</sub>. The conversion can be effected with thionyl chloride: It also can be prepared by chlorination of niobium pentoxide in the presence of carbon at 300&nbsp;°C.

Uses

Niobium(V) chloride is the main precursor to the alkoxides of niobium, which find uses in sol-gel processing. It is also the precursor to many other Nb-containing reagents, including most organoniobium compounds.

In organic synthesis, NbCl<sub>5</sub> is a very specialized Lewis acid in activating alkenes for the carbonyl-ene reaction and the Diels-Alder reaction. Niobium chloride can also generate N-acyliminium compounds from certain pyrrolidines which are substrates for nucleophiles such as allyltrimethylsilane, indole, or the silyl enol ether of benzophenone.

References

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