Hi Alejandro, A couple of things jump out at me: First, you say the data goes out to 10Ang^-1. That seems short for Cr in a Cr-Fe alloy, and implies either non-ideal data collection (as Sven alluded to: pinholes in a transmission sample, data collected in fluorescence, or a surface-contaminated e-yield measurement), or a highly disordered Cr environment.
4) About the nature of the alloy, from our experience we know that Cr is behaving in a very similar way to Fe here, so we should have a random substitutional alloy. From high resolution x-ray diffraction data we know that part of the Fe has not been alloyed, so there remain some 'clusters' of Fe.
To paraphrase, the sample is not a random mixture of Cr and Fe in a bcc lattice, which seems a little strange to me, as bcc Cr and Fe have very similar lattice constants -- I don't know whether they form a uniform solid solution, but you are studying this sample, so it might not be as simple as a random substitution, right??? Do you know the fraction of Fe atoms that has been alloyed? Do you know how much of the sample is crystalline, and what the defect density is? These all might be important: You're assuming that all Cr is surrounded by Cr, in a single bcc environment. Suppose there were two or more Cr environments, with slightly different Cr-metal distances. By assuming 1 environment, you'd end up with a sigma2 that included the static disorder of having multiple environments. .. which could all be related to having such a short data range. By the way, any such issue would completely negate the assertion that there is a simple relation between the diffraction and XAFS sigma^2. The assertion that sigma^2 <= 2 definitely assumes that all atoms are on a single set of lattice points. For example, it is not a very useful guideline for amorphous systems. Hope that helps, --Matt