93
Beekman et al.
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(1991).
7. A.W. Cordes, R.C. Haddon, R.T. Oakley, L.F. Schneemeyer, J.V.
Waszczak, K.M. Young, and N.M. Zimmerman. J. Am. Chem.
Soc. 113, 582 (1991).
8. C.D. Bryan, A.W. Cordes, J.D. Goddard, R.C Haddon, R.G.
Hicks, C.D. MacKinnon, R.C. Mawhinney, R.T. Oakley, T.T.M.
Palstra, and A.S. Perel. J. Am. Chem. Soc. 118, 330 (1996).
9. A.W. Cordes, R.C. Haddon, R.G. Hicks, D.K. Kennepohl, R.T.
Oakley, T.T.M. Palstra, L.F. Schneemeyer, S.R. Scott, and J.V.
Waszczak. Chem. Mater. 5, 820 (1993).
Fig. 3 (7) and Fig. 4 (6). Crystal structure reports, and addi-
tional tables of final positional parameters, bond lengths and
angles, hydrogen atom coordinates, and anisotropic displace-
ment parameters for both 6 and 7 have been deposited as sup-
plementary material.6
Electrochemistry
For the voltammetric experiments the vacuum-tight all-glass
cell with Pt electrodes that has been described previously (18)
was employed. The cell was charged with electrolyte
(NnBu4PF6) and the solvent, dry degassed CH3CN or CH2Cl2,
was transferred on a vacuum line. Samples and ferrocene as an
internal reference were added to the cell using break-seal tech-
niques. The ferricenium/ferrocene couple is observed in this
system at +0.38 V (CH3CN) and +0.48 V (CH2Cl2) vs. SCE at
25°C. Cyclic voltammetric (scan rates ν = 20–500 mV s–1) and
phase-sensitive alternating current experiments (ω = 610 Hz,
ν = 10 mV s–1) were carried out with a PAR 170 electrochemi-
cal system.
10. W.M. Davis, R.G. Hicks, R.T. Oakley, B. Zhao, and N.J. Taylor.
Can. J. Chem. 71, 180 (1993).
11. A.W. Cordes, R.C. Haddon, R.G. Hicks, R.T. Oakley, and T.T.M.
Palstra. Inorg. Chem. 31, 1802 (1992).
12. A.W. Cordes, R.C. Haddon, R.G. Hicks, D.K. Kennepohl, R.T.
Oakley, L.F. Schneemeyer, and J.V. Waszczak. Inorg. Chem. 32,
1554 (1993).
13. A.J. Banister, N. Bricklebank, W. Clegg, M.R.J. Elsegood, C.I.
Gregory, I. Lavender, J.M. Rawson, and B.K. Tanner. J. Chem.
Soc. Chem. Commun. 679 (1995).
14. A.J. Banister, N. Bricklebank, I. Lavender, J.M. Rawson, C.I.
Gregory, B.K. Tanner, W. Clegg, M.R.J. Elsegood, and F.
Palacio. Angew. Chem. Int. Ed. Engl. 35, 2533 (1996).
15. R.T. Boeré and K.H. Moock. J. Am. Chem. Soc. 117, 4775
(1995).
16. M.A. McCall, J.R. Caldwell, H.G. Moore, and H.M. Beard. J.
Macromol. Sci. Chem. A3, 911 (1969).
17. R.T. Boeré, R.G. Hicks, and R.T. Oakley. Inorg. Synth. 21, 94
(1997).
18. K.H. Moock and M.H. Rock. J. Chem. Soc. Dalton Trans. 2459
(1993).
Acknowledgments
We thank Prof. Robert Thompson, University of British Co-
lumbia, for a preliminary magnetic susceptibility measurement
at room temperature, and Dr. Robert Haddon, Bell Labs, for
the VT measurements. Dr. Ralph Weber of Bruker, U.S.A.,
provided time on the EMX spectrometer, and we thank the
staff at Bruker for their assistance. The Natural Sciences and
Engineering Research Council of Canada and the University
of Lethbridge Research Fund provided financial support.
19. R.T. Boeré, K.H. Moock, and M.Z. Parvez. Z. Anorg. Allg.
Chem. 520, 1589 (1994).
20. C.M. Aherne, A.J. Banister, I.B. Gorrell, M.I. Hansford, Z.V.
Hauptman, A.W. Luke, and J.M. Rawson. J. Chem. Soc. Dalton
Trans. 967 (1993).
21. P. Del Bel Belluz, A.W. Cordes, E.M. Kristof, P.V. Kristof, S.W.
Liblong, and R.T. Oakley. J. Am. Chem. Soc. 111, 9276 (1989).
22. J.B. Flanagan, S. Margel, A.J. Bard, and F.C. Anson. J. Am.
Chem. Soc. 100, 4248 (1978).
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6
This material may be purchased from: The Depository of
Unpublished Data, Document Delivery, CISTI, National
Research Council Canada, Ottawa, Canada K1A 0S2. The crystal
structure reports, including tables of bond lengths, bond angles,
and atomic coordinates, have also been deposited with the
Cambridge Crystallographic Data Centre, and can be obtained on
request from The Director, Cambridge Crystallographic Data
Centre, University Chemical Laboratory, 12 Union Road,
Cambridge, CB2 1EZ, U.K.
© 1998 NRC Canada