Synthesis and Characterization of Oxidized W6S8L6 Clusters

Inorg. Chem., 40 (12), 2660 -2665, 2001. 10.1021/ic001099d S0020-1669(00)01099-5
Web Release Date: May 4, 2001

Synthesis and Characterization of Oxidized W₆S₈L₆ Clusters

Laurie I. Hill, Song Jin, Ran Zhou, D. Venkataraman, and Francis J. DiSalvo*

Baker Laboratories, Department of Chemistry and Chemical Biology, Cornell University, Ithaca, New York 14853

Received October 3, 2000

Abstract:

Cationic [W₆S₈L₆]PF₆ (L = PEt₃ (3), 4-tert-butylpyridine (4)) clusters were successfully synthesized and isolated for the first time by reacting the corresponding neutral W₆S₈L₆ (L = PEt₃ (1), 4-tert-butylpyridine (2)) clusters with [Cp₂Fe]PF₆ as the oxidant. The products 3 and 4 were characterized by NMR spectroscopy, mass spectroscopy, and X-ray crystallography (only for 3) and shown to be the desired oxidized W₆S₈ clusters with a metal electron count of 19. Magnetic property studies showed that they are paramagnetic compounds with S = ¹/₂. Their chemical properties and stability are also reported. Crystal data for 3·2THF: space group, R (No. 148); a = 13.91170(10) Å; c = 32.4106(2) Å; Z = 3.

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