Spin crossover (SCO) materials that switch between two different spin states, that is, the high spin (HS) and the low spin (LS) state, with very different optical, magnetic, and structural properties offer a unique platform to understand the consequences induced by the different electronic configurations of transition metal complexes. Due to the significant changes associated with the spin transition, it can be followed by different techniques such as UV-vis and IR optical spectroscopy, magnetism, crystallography, calorimetric analysis, nuclear magnetic resonance, etc. Hence, a practical experiment for laboratory classes dedicated to the topic of SCO focused on the thermal transition, that is, the transition triggered by temperature, results in a simple yet attractive way to understand not only fundamental concepts of inorganic and physical chemistry but also to get acquainted with the synthesis of nanoparticles and the characterization of inorganic solid samples.