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A review focusing on the application of NMR spectroscopy to the study of organometallic photochemistry where the photochemical step is performed in situ, i.e. the irradiation of the sample takes place within the probe of the NMR spectrometer. Various experimental designs, taken from all areas of chemical and biological study, that facilitate in situ irradiation are discussed, paying attention to light sources and light delivery methods. The literature covering the application of the in situ method across the field of organometallic chemistry is then reviewed. There is particular emphasis on studies of reactive organometallic compounds with weakly coordinating ligands such as alkane, xenon and other “solvent” species, as complexes with short lifetimes benefit most from application of the in situ illumination method.

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