Gemstones are pieces of materials that once cut and polished are used as jewels or adornments. Gemstones may be single crystal (such as diamonds), polycrystalline (such as lapis lazuli), or amorphous (such as amber). In any case, gems may have inclusions that may yield a variety of optic effects. It is also important to unravel the crystal structure of the inclusion(s) in order to determine the origin of the gem and to help to understand their formation mechanism. Here, we expand the use of powder diffraction to identify crystalline inclusions in bulk gemstones highlighting Mo Kα radiation to penetrate within compact gems. Initially, rock crystal quartz with rutile needles was investigated and rutile diffraction peaks were more conspicuous in the Mo pattern than in the Cu pattern. Next, rock crystal quartz with beetle legs was characterized and the red iron oxide inclusion was identified as hematite. The study of a fake gem, glass showing aventurine effect, gave the diffraction peaks of metallic copper. Later, polycrystalline gems, moss agate, and aventurine quartz were also studied. The powder patterns of these compact gemstones could be successfully fitted using the Rietveld method. Finally, we discuss opportunities for further improvements in laboratory powder diffraction to characterize inclusions in compact gems.