Sub calibration often ends up being a little bit science, a little bit art, and a little bit guesswork. An SPL meter will be a
big help for calibration, although the sub's still a bit tricky because of the typical SPL meter's difficulty measuring such low frequencies. In addition to the test tones, you might want to try some bass-heavy source material that you're familiar with and adjust a bit to produce the sound that you like (which may be a few dB "hotter" or "cooler" than a truly flat response). You might also play around with my
Devious Tiny Disc (there's a CD version if you don't have access to a DVD burner) or other sweep test tones to hear a frequency sweep from 20Hz up (the DTD goes up to about 6000Hz). The "pink noise" test tones will be better for dialing the sub in, but the sweep may be helpful for getting a feel for volume levels and sub/speaker integration.