Niobium(V) chloride explained

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 NbOCl3. It is often used as a precursor to other compounds of niobium. NbCl5 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 pm (terminal) and 256 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 pm, too long for any metal-metal interaction.[1] NbBr5, NbI5, TaCl5 TaBr5 and TaI5 are isostructural with NbCl5.

Preparation

Industrially, niobium pentachloride is obtained by direct chlorination of niobium metal at 300 to 350 °C:[2]

2Nb + 5Cl2 → 2NbCl5

In the laboratory, niobium pentachloride is often prepared from Nb2O5, the main challenge being incomplete reaction to give NbOCl3. The conversion can be effected with thionyl chloride:[3] It also can be prepared by chlorination of niobium pentoxide in the presence of carbon at 300 °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, NbCl5 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.[4]

References

  1. Cotton, F.A., P. A. Kibala, M. Matusz and R. B. W. Sandor . 1991 . Structure of the Second Polymorph of Niobium Pentachloride . . 47 . 2435–2437 . 10.1107/S0108270191000239 . 11.
  2. Encyclopedia: Joachim Eckert . Hermann C. Starck . Niobium and Niobium Compounds. Ullmann's Encyclopedia of Industrial Chemistry. 2005. Wiley-VCH. Weinheim. 10.1002/14356007.a17_251. 3-527-30673-0.
  3. Book: 10.1002/9780470132401.ch24. 9. Niobium(V) Chloride and Hexachloroniobates(V). 1957. Brown. D.. Inorganic Syntheses. 88–92. 978-0-470-13240-1.
  4. Andrade, C. K. Z. . Rocha, R. O. . Russowsky, D. . Godoy, M. N. . amp . 2005 . Studies on the Niobium Pentachloride-Mediated Nucleophilic Additions to an Enantiopure Cyclic N-acyliminium Ion Derived from (S)-malic acid . J. Braz. Chem. Soc. . 16 . 535–539 . 10.1590/S0103-50532005000400007 . 3b . free . 10183/24558 . free .

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