Molybdenum(III) chloride explained

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

Notes and References

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

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