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Combining insights from diffuse reflection infrared Fourier transform spectroscopy and X-ray pair distribution function (PDF) analysis has the potential to deepen our understanding of complex materials systems including heterogeneous catalysts and host-guest systems. This article describes the development of instrumentation and non-ambient reaction cells that enable combined PDF-IR studies without compromise to either measurement. Through careful selection of the IR spectrometer and optics, the IR instrument and reaction cell were adapted to allow angular dispersive X-ray measurements without change to the active IR components. The PDF and diffraction data obtained with this experimental configuration are shown to be of similar quality and resolution to standard capillary-based measurements. Simultaneous combined measurements are demonstrated for desorption of guests from within a Prussian blue analog.
