Gas-phase IR photoacoustic (PA) spectra have been obtained for the volatile, solid pentacarbonyl(methyl)metal(I) complexes, CH<sub>3</sub>Mn(CO)<sub>5</sub> and CH<sub>3</sub>Re(CO)<sub>5</sub>. The gaseous samples were apparently produced directly in the PA sample cup as the result of local surface heating effects. Vibrational assignments are given for the gas-phase spectra, especially for the binary <i>v</i>(CO) overtone and combinations which absorb in the near-IR region at ~4000 cm<sup>−1</sup>. The data provide further support for near-IR/PA spectroscopy being a useful technique for the rapid, non-destructive identification of small amounts of organometallic carbonyl complexes.

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