Inorganic Chemistry
Article
remaining solid was redissolved in CH2Cl2 under humid air, and excess
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NEt3 was added. UV−vis spectra indicated the slow formation of 4.
1
Characterization of 4. H NMR: A sample of 1 in CDCl3 was
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treated with excess of NEt3 under air. The formation of 4 was
monitored by UV−vis spectroscopy.30,31 The solution was concen-
trated to give a concentration suitable for 1H NMR spectroscopic
analysis. 1H NMR (400 MHz, T = 298 K): δ = 9.08 (s, 8H, CHpyrrole),
8.28 (br. s, 4 H, CHortho), 8.16 (br. s, 4 H, CHortho), 7.78 (br. s, 12 H,
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by UV−vis spectroscopy prior to recording the IR spectrum of 4 in
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CH2Cl2. IR(CH2Cl2): ν
̃
= 1021 (m, CrO), 998 (s) cm−1.31
ASSOCIATED CONTENT
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■
S
* Supporting Information
Spectral characterization of 1, 4, and 4+; cyclic and square-wave
voltammograms of 1 with/without addition of LiOH; UV−vis
spectrum of the reaction of 1 with excess NH3 in CH2Cl2; UV/
vis spectra of 8 in THF, 8 in THF with exc. NEt3, 8 in CH2Cl2
with exc. NEt3 ; UV−vis spectra of the reaction of 1 with LiCl;
X-band EPR spectrum of 4+; GC of the electrolysis solution of
4 and 100 equiv of norbonene; spectroelectrochemical
oxidation of 4 in the presence of norbonene; Cartesian
coordinates of all optimized structures. This material is available
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AUTHOR INFORMATION
■
Corresponding Author
Author Contributions
The manuscript was written through contributions of all
authors. All authors have given approval to the final version of
the manuscript.
Notes
The authors declare no competing financial interest.
ACKNOWLEDGMENTS
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(30) Liston, D. J.; West, B. O. Inorg. Chem. 1985, 24, 1568−1576.
(31) Groves, J. T.; Kruper, W. J.; Haushalter, R. C.; Butler, W. M.
Inorg. Chem. 1982, 21, 1363−1368.
We thank the Fonds National de la Recherche Luxembourg
(FNR) for financial support through the “SurfAmine” project.
We thank D. Schmitt, M. Mirion, S. Herold, and Prof. S. R.
Waldvogel for assistance with the bulk electrolysis and the GC
measurements.
(32) Budge, J. R.; Gatehouse, B. M. K.; Nesbit, M. C.; West, B. O. J.
Chem. Soc., Chem. Commun. 1981, 370−371.
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