The structures of [(2,5-norbornadiene)Rh{C(Ph)CPh2}(PPh3)] (1) and its reaction product
with
CH3CO2H were elucidated by 1H, 13C, and 31P NMR spectroscopy, mass spectrometry,
and single-crystal X-ray analysis. The presence of two conformational
isomers of 1 was verified by NMR spectroscopy, which
was well-supported by DFT calculations. Phenylacetylene was polymerized
using 1 as a catalyst with [M]0/[Rh] = 10
and quenched with CH3CO2H and CH3CO2D. The incorporation of H and D at the polymer ends
was confirmed by MALDI-TOF mass spectrometry and 1H and 1H–13C HSQC NMR spectroscopy. The polymerization
degree was calculated to be 11 by 1H NMR spectroscopy,
which agreed well with the theoretical value.