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Vanadium hexacarbonyl

Vanadium hexacarbonyl is the inorganic compound with the formula V(CO)<sub>6</sub>. It is a blue-black volatile solid. This highly reactive species is noteworthy from theoretical perspectives as a rare isolable homoleptic metal carbonyl that is paramagnetic. Most species with the formula M<sub>x</sub>(CO)<sub>y</sub> follow the 18-electron rule, whereas V(CO)<sub>6</sub> has 17 valence electrons.

Structure

V(CO)<sub>6</sub> adopts an octahedral coordination geometry and is isostructural with chromium hexacarbonyl, even though they have differing valence electron counts. High resolution X-ray crystallography indicates that the molecule is slightly distorted with two (axial) shorter V–C distances of 1.993(2)&nbsp;Å vs. four (equatorial) 2.005(2)&nbsp;Å. Even though V(−I) is a larger ion than V(0), the V–C distances in are 0.07&nbsp;Å shorter than in the neutral precursor.

Synthesis

According to the original synthesis by Calderazzo, V(CO)<sub>6</sub> is prepared in two-steps via the intermediacy of . In the first step, VCl<sub>3</sub> is reduced with metallic sodium under 200&nbsp;atm CO at 160&nbsp;°C. The solvent for this reduction is typically diglyme, CH<sub>3</sub>OCH<sub>2</sub>CH<sub>2</sub>OCH<sub>2</sub>CH<sub>2</sub>OCH<sub>3</sub>. This triether solubilizes sodium salts, akin to the behavior of a crown ether:

4&nbsp;Na + VCl<sub>3</sub> + 6&nbsp;CO + 2&nbsp;diglyme → [Na(diglyme)<sub>2</sub>][V(CO)<sub>6</sub>] + 3&nbsp;NaCl

The resulting anion is oxidized with acid:

2&nbsp; + 2 H<sub>3</sub>PO<sub>4</sub> → 2&nbsp;V(CO)<sub>6</sub> + H<sub>2</sub> + 2&nbsp;

Reactions

Vanadium hexacarbonyl is thermally unstable. Its primary reaction is reduction to the monoanion , salts of which are well studied. It is also susceptible to substitution by tertiary phosphine ligands, often leading to disproportionation.

V(CO)<sub>6</sub> reacts with sources of the cyclopentadienyl anion to give the orange four-legged piano stool complex (C<sub>5</sub>H<sub>5</sub>)V(CO)<sub>4</sub> (m.p.&nbsp;136&nbsp;°C). Like many charge-neutral organometallic compounds, this half-sandwich species is volatile. In the original preparation of this species, C<sub>5</sub>H<sub>5</sub>HgCl was employed as the source of .

References

Further reading

  • Original synthesis: