CRYSTAL-STRUCTURE, AND VARIABLE-TEMPERATURE PROTON AND C-13 NMR-SPECTRA OF THE 9-MEMBERED RING COMPLEX (E,Z-PPH(2)CH(2)C((T)BU)=N-N=C((T)BU)CH(2)PPH(2))]
Sd. Perera et al., CRYSTAL-STRUCTURE, AND VARIABLE-TEMPERATURE PROTON AND C-13 NMR-SPECTRA OF THE 9-MEMBERED RING COMPLEX (E,Z-PPH(2)CH(2)C((T)BU)=N-N=C((T)BU)CH(2)PPH(2))], Journal of organometallic chemistry, 462(1-2), 1993, pp. 221-224
Treatment of [Cr(CO)(4)(nbd)] (nbd = norbornadiene) with Z,Z-PPh(2)CH(
2)C((t)Bu)=N-N=C((t)Bu)CH(2)PPh(2) gave the title compound 2b, the str
ucture of which was determined by a single crystal X-ray diffraction s
tudy. The proton NMR spectrum of 26 at 308 K and 400 MHz showed that f
or each of the methylene groups the protons are equivalent, but the sp
ectrum is temperature dependent and at 188 K the slow exchange limitin
g spectrum is obtained, with all methylene hydrogens chemically non-eq
uivalent; corresponding changes were observed in the C-13-(H-1) NMR sp
ectrum. The behaviour is due to the fluxionality of the 9-membered rin
g.