Teaching Crystallography by Determining Small Molecule Structures and 3-D Printing: An Inorganic Chemistry Laboratory Module

Experimental methods for determining 3-D atomic structures, such as crystallography, are rarely taught in the undergraduate curriculum, yet are considered to be the norm for 3-D structure determination in a research setting. Although a fully physical understanding of crystallography takes years of practice, practical applications and basic interpretation of small-molecule crystallography can be readily integrated into undergraduate curricula to give students a research-like laboratory experience. Three 1-h crystallography laboratory modules were developed using the free Olex[superscript 2] software to determine the structure of (dithiolene)[subscript 2]Co(1,3,5-triaza-7-phosphaadamantane)·dichloroethane, while introducing basic crystallography knowledge, crystal evaluation through microscopy, practical structure determination skills, and spatial awareness through 3-D printing. Following implementation in an advanced instrumental analysis class composed of 14 Master's and undergraduate students, the increase of topical knowledge of small molecule crystallography was 18-30% based on tailored assessment surveys, and student feedback was highly positive. This suggests that students without a prior background in crystallography were able to learn and retain information about small molecule crystallography from these laboratory modules.