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The spectrometer followed the pulse shaper–enabled pump-probe 2D IR setup, and a rotational stage was added to control beam incidence angle. In the 2D IR spectrometer, three IR pulses interacted with a sample sequentially to create two vibrational coherences. The first coherence was characterized by scanning t1. The second coherence introduced a macroscopic polarization, which subsequently emitted a third-order IR signal, which was self-heterodyned and detected in frequency domain. Transient pump-probe signal could be obtained by setting t1 = 0 fs. To obtain 2D IR spectra, the free-induction-decay (FID) in t1 was numerically Fourier-transformed.

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