The determination of the molecular structure in solution is an important target of the modern chemistry. In many fields, the knowledge of the structural and the dynamics information in solution are a fundamental tool for a complete understanding of chemical processes, from catalytic mechanisms to biological activities of proteins. However there is not a general strategy to approach the problem of solution structural study for any type of molecule. This book proposes a methodology to investigate the structure and the dynamics in solution of chiral ytterbium(III) complexes, based on a combined use of spectroscopic techniques such as Nuclear Magnetic Resonance and Circular Dichroism. This method has been applied here to the study of several ytterbium(III) complexes, recently proposed in scientific literature as catalysts for stereoselective organic reactions. The results evidenced that the structure in solution is sometime different from that one obtained in the solid state from X-ray crystallographic diffraction, furnishing a more suitable basis for the investigation of the catalytic mechanism in solution phase. Furthermore, one chapter has been dedicated to the use of Yb(III) ions as probe for the determination of the absolute configuration of an important class of molecules such as chiral 1,2-diols. This is also an example to how this methodology can be extended to other fields of chemistry.