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The XRD data for the pair distribution function (PDF) determination were collected independently using a Huber diffractometer in symmetric reflection geometry (up to 2θmax ) 140°) and Ag Kα radiation λ= 0.5609 Å). The PDF was obtained using standard methods. The data were corrected for background, absorption, polarization, Compton and multiple scattering and normalized by the incident flux, the number of scatterers, and the average atomic form factor of the sample to obtain the normalized total scattering function S(Q) (Q ) 4φ sin θ/λ where 2θ is the scattering angle). The reduced radial distribution function, or pair distribution function (PDF) G(r), is obtained from S(Q) through a Fourier transform: G(r)= [4φrF(r)-4φrF0] ) (2/φ)s ∫0Q[S(Q)-1] sin(Qr) dQ. Where F(r) is the atomic pair density function. The function G(r) represents the radial density distribution showing peaks at distances, r, which separate pairs of atoms in the solid. For example, the first strong peak occurs at r 2.2 Å corresponding to the Ge-S nearest neighbor peak in these materials. It is a measure of the short-range atomic order in the solid and does not presume any crystallinity. The procedures used to perform atomic pair distribution function analysis of XRD data have been published elsewhere [Egami, T. Mater. Trans. JIM 1990, 31, 163. Billinge, S. J. L.]
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