I've made these kinds of matrix measurements several times since I got my
hands on a VNA. It's not too hard and actually a lot of fun. I've found
that if I've been careful, the reciprocal measurements are usually within 1%
or better. This holds true even when the values themselves are really
strange, as they can be when there's a parasitic radiator coupling into the
array.
Usually I do the measurements using only impedance measurements which is
very straight forward but occasionally I'll use the transmission mode and a
current transformer to do a direct measurement of coupling. Both ways seem
to work fine as long as I pay attention to the details.
73, Rudy
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