W. Kaim et al. / Journal of Organometallic Chemistry 637–639 (2001) 167–171
171
(342 mg, 73%). Anal. Found: C, 41.68; H, 5.40. Calc.
for C32H50ClF6FeOsP3 (923.16 g mol−1): C, 41.63; H,
5.46%. 1H-NMR (acetone-d6): l 1.13–1.28 (m, 12H,
CH(CH3)2), 1.38 (d, 6H, CH(CH3)2, 3J=6.9 Hz), 1.40–
1.57 (m, 12H, CH(CH3)2), 2.56 (sept, 4H,
CH(CH3)2,3J=7.0 Hz), 2.64 (s, 3H, CH3), 4.27 (s, br,
FcꢀH), 4.48 (s, br, FcꢀH), 4.54 (s, br, FcꢀH), 4.89 (s,
Cl(dppf)](PF6)·CH3CN. Copies of this information may
be obtained free of charge from The Director, CCDC,
12 Union Road, Cambridge CB2 1EZ, UK (Fax: +44-
1223-336033; e-mail: deposit@ccdc.cam.ac.uk or www:
http://www.ccdc.cam.ac.uk).
3
br, FcꢀH), 6.10 (d, 2H, Cym, J=6.1 Hz), 7.11 (d, 2H,
Acknowledgements
3
Cym, J=5.8 Hz) 7.47–7.76 (m, Ph). 31P-NMR (ace-
tone-d6): l −5.15 (Fc(PR2)2), −143.54 (PF6).
This work has been supported within the Landes-
forschungsschwerpunktprogramm Baden-Wu¨rttemberg,
by the Volkswagenstiftung and the Fonds der Chemis-
chen Industrie. We also thank the German–Czech sci-
entific exchange program for support.
4.2. Instrumentation
EPR spectra were recorded in the X band on a
Bruker System ESP 300 equipped with a Bruker
ER035M gaussmeter and a HP 5350B microwave coun-
1
ter. H- and 31P-NMR spectra were taken on Bruker
References
AC 250 and AC 400 spectrometers. UV–vis absorption
spectra were recorded on a Bruins Instruments Omega
10 spectrophotometer. Cyclic voltammetry was carried
out in 0.1 M Bu4NPF6 solutions using a three-electrode
configuration (glassy carbon electrode, Pt counter elec-
trode, Ag ꢁ AgCl reference) and a PAR 273 potentiostat
and function generator. The ferrocene/ferrocenium cou-
ple served as an internal reference. Spectroelectrochem-
ical measurements were performed using an OTTLE
cell [15] for UV–vis spectra and a two-electrode capil-
lary for EPR studies [20].
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4.3. Crystallography
Yellow single crystals of [(Cym)OsCl(dppf)]-
(PF6)·CH3CN were obtained from a saturated solution
of the compound in MeCN, cooled to 5 °C. The struc-
ture of [(Cym)OsCl(dppf)](PF6)·CH3CN was solved by
direct methods. The refinement was carried out employ-
ing full-matrix least-squares procedures [21]. All non-
hydrogen atoms were refined anisotropically. The
hydrogen atoms were introduced at proper geometric
positions and treated according to the riding model
with isotropic thermal parameters fixed at 20% greater
than that of the bonded atom. Anisotropic thermal
parameters were refined for all non-hydrogen atoms.
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5. Supplementary material
Crystallographic data for the structural analysis have
been deposited with the Cambridge Crystallographic
Data Centre, CCDC no. 151761 for [(Cym)Os-
[21] SHELXTLN, Version 5.1, Bruker AXS, 1998.