Synthesis 2005(19): 3373-3379  
DOI: 10.1055/s-2005-918438
PAPER
© Georg Thieme Verlag Stuttgart · New York

Synthesis of 2,2′,3,3′-Tetramethyl- and 2,2′,3,3′-Tetra-tert-butylfulvalene: Attractive­ Platforms for Dinuclear Transition Metal Fragments, as Exemplified by (η 5:η 5-2,2′,3,3′-t-Bu4C10H4)M2(CO) n (M = Fe, Ru, Os, Mo) and First X-ray Crystal Structures of Fulvalene Diiron and Diosmium Complexes

Bolin Zhua,b, Ognjen Š. Miljanića,b, K. Peter C. Vollhardt*a,b, Michael J. Westa,b
a Center for New Directions in Organic Synthesis, Department of Chemistry, University of California at Berkeley, Berkeley, CA 94720, USA
b Chemical Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA 94720-1460, USA
Fax: +1(510)6435208; e-Mail: kpcv@berkeley.edu;
Further Information

Publication History

Received 1 August 2005
Publication Date:
25 October 2005 (online)

Abstract

2,2′,3,3′-Tetramethylfulvalene (4) and 2,2′,3,3′-tetra-tert-butylfulvalene (7) were synthesized by two different routes. The potential of these systems to function as ligands to transition metals was explored with the more readily made 7, resulting in the preparation of the dinuclear complexes (η 5:η 5-t-Bu4C10H4)M2(CO)4 (M = Fe, Ru, Os, 8-10) and (η 5:η 5-t-Bu4C10H4)Mo2(CO)6 (11). The molecular structures of complexes 8 and 10 were determined by X-ray diffraction. Complexes 9 and 10 rearranged on irradiation to their (µ 2-η 1:η 5-cyclopentadienyl)2M2(CO)4 isomers 12 and 13, respectively, thermally reversible for 12, while 8 was photoinert.

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Zhu, B.; Miljanić, O. Š.; Vollhardt, K. P. C.; West, M. J., to be published.

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CCDC-278400 and CCDC-278401 contain the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/conts/retrieving.html (or from the Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(1223)336033; or deposit@ccdc.cam.ac.uk).