Hi, Jim-
The anatomical ROI and the diffusion data probably came through different routes (they certainly started from different datasets). Have you mapped the FreeSurfer output into the diffusion space? At that point, the ROIs should definitely be in the diffusion space. What is the processing each have undergone? It would be better to explore this first before applying 3dresample, because just resampling grids might not actually be appropriate (even if it doesn't result in an error, the ROI might not really be where it "should" be in the diffusion space).
For example, merging these sources of data is accomplished in the FATCAT_DEMO2, described here:
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afni.nimh.nih.gov]
--pt