Full-range mid-infrared spectra were measured during the reaction of CpCo(CO)<sub>2</sub> with nitrosyl chloride by interfacing a rapid-mixing stopped-flow device with an ultra-rapid-scanning Fourier transform infrared (FT-IR) spectrometer having a temporal resolution of 5 ms. Changes to the data acquisition hardware of this spectrometer now allow a sequence of well over 2000 spectra to be collected without interruption. Two transient species were observed spectroscopically during the first 500 ms of the reaction of CpCo(CO)<sub>2</sub> with nitrosyl chloride. The shortest-lived species that was observed, [CpCo(CO)<sub>2</sub>(NO)]<sup>+</sup>, had a half-life of ∼20 ms at 25 °C and ∼70 ms at 10 °C. This intermediate transformed into a longer-lived (∼0.5 s) intermediate, CpCo(NO)Cl. Potential intermediate species with one CO and one NO ligand, such as [CpCo(CO)(NO)]<sup>+</sup> and CpCo(CO)(NO)Cl, were not observed, although the possibility that they exist cannot be ruled out.

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