In an attempt to both prepare nanocrystalline bismuth and understand the fundamental chemistry behind the formation of this potentially interesting material, we have examined the reduction of BiCl3 in the presence of strongly coordinating solvents and ligands. These studies have resulted in the formation of bismuth powders with approximate average particle sizes of between 20 and 40 nm which exhibit large size distributions. The simultaneous reduction of both gold and bismuth precursors, done in an attempt to better control the final particle size, instead produces Au2Bi of comparable dimensions. There is no evidence that the ligands utilized in either of these systems remain bound to the final product. These nanocrystalline powders have been characterized through XRD and TEM, and full details of the synthesis are presented.