Journal
CHEMICAL SCIENCE
Volume 3, Issue 5, Pages 1656-1661Publisher
ROYAL SOC CHEMISTRY
DOI: 10.1039/c2sc01050j
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Funding
- Royal Society
- EPSRC
- Diamond Light Source Ltd
- Advanced Light Source
- Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy [DE-AC02-05CH11231]
- Biotechnology and Biological Sciences Research Council [BB/C507088/1] Funding Source: researchfish
- Engineering and Physical Sciences Research Council [EP/D072859/1, EP/I01974X/1] Funding Source: researchfish
- EPSRC [EP/D072859/1, EP/I01974X/1] Funding Source: UKRI
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Pd-3(OAc)(5)NO2, an impurity in Pd(OAc)(2) {formally Pd-3(OAc)(6)}, emerges as a serious issue in the synthesis of pure Pd-II complexes derived from Pd(OAc)(2), for example in our C-H activation precatalyst, Pd(OAc)(2)(pip)(2) (pip piperidine). A previous proposal that nitrite anion can be formed by oxidation of CH3CN by metallic Pd and air, leading to cyclo(ortho)palladated complexes containing nitrite anion, e.g. Pd(NO2)(C boolean AND N) L (C boolean AND N = papaverine; L = CH3CN or DMSO) can be explained by Pd-3(OAc)(5)NO2 acting as the nitrite source. Finally, photocrystallographic metastable linkage isomerisation and complete conversion to an oxygen-bound nitrito complex Pd(eta(1)-ONO)(C boolean AND N)PPh3 has been observed.
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