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Molybdenum(III) chloride is the inorganic compound with the formula MoCl3. It forms purple crystals.[1]

Synthesis and structure

Molybdenum(III) chloride is synthesized by the reduction of molybdenum(V) chloride with hydrogen.[2] A higher yield is produced by the reduction of pure molybdenum(V) chloride with anhydrous tin(II) chloride as the reducing agent.[3]

Molybdenum trichloride exists as two polymorphs: alpha (α) and beta (β). The alpha structure is similar to that of aluminum chloride (AlCl3). In this structure, molybdenum has octahedral coordination geometry and exhibits cubic close-packing in its crystalline structure. The beta structure, however, exhibits hexagonal close packing.[4]

Ether complexes

Molybdenum trichloride gives a ether complexes MoCl3(thf)3 and MoCl3(Et2O)3. They are beige, paramagnetic solids. Both feature octahedral Mo centers. The diethyl ether complex is synthesized by reducing a Et2O solution of MoCl5 with tin powder.[5] Older procedures involve stepwise reduction involving isolation of the Mo(IV)-thf complex.[6]

Hexa(tert-butoxy)dimolybdenum(III) is prepared by the salt metathesis reaction from MoCl3(thf)3:[7]

2 MoCl3(thf)3 + 6 LiOBu-t → Mo2(OBu-t)6 + 6 LiCl + 6 thf

References

  1. ^ Perry DL (2011). Handbook of Inorganic Compounds (2nd ed.). Boca Raton: Taylor & Francis. p. 279. ISBN 978-1-4398-1461-1.
  2. ^ Couch DE, Brenner A (1959). "Preparation of Trichloride and Tetrachloride of Molybdenum". Journal of Research of the National Bureau of Standards Section A. 63A (2): 185–188. doi:10.6028/jres.063A.013. PMC 5287202. PMID 31216151.
  3. ^ Larson ML (1970). "Preparation of Some Metal Halides- Anhydrous Molybdenum Halides and Oxide Halides - A Summary". Inorganic Syntheses. Vol. 12. pp. 178–181.
  4. ^ Hillebrecht H, Schmidt PJ, Rotter HW, Thiele G, Zönnchen P, Bengel H, Cantow HJ, Magonov SN, Whangbo MH (1997). "Structural and scanning microscopy studies of layered compounds MCl3 (M= Mo, Ru, Cr) and MOCl2 (M= V, Nb, Mo, Ru, Os)". Journal of Alloys and Compounds. 246 (1–2): 70–79. doi:10.1016/S0925-8388(96)02465-6.
  5. ^ Maria, Sébastien; Poli, Rinaldo (2014). "Ether Complexes of Molybdenum(III) and Molybdenum(IV) chlorides". Inorganic Syntheses: Volume 36 (PDF). Inorganic Syntheses. Vol. 36. pp. 15–18. doi:10.1002/9781118744994.ch03. ISBN 9781118744994.
  6. ^ Dilworth, Jonathan R.; Richards, Raymond L. (1990). "The Synthesis of Molybdenum and Tungsten Dinitrogen Complexes". Inorganic Syntheses. Inorganic Syntheses. Vol. 28. pp. 33–43. doi:10.1002/9780470132593.ch7. ISBN 9780470132593.
  7. ^ Broderick, Erin M.; Browne, Samuel C.; Johnson, Marc J. A. (2014). "Dimolybdenum and Ditungsten Hexa(Alkoxides)". Inorganic Syntheses: Volume 36. Inorganic Syntheses. Vol. 36. pp. 95–102. doi:10.1002/9781118744994.ch18. ISBN 9781118744994.


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