This article describes a program that was developed to introduce senior high school students in Melbourne, Australia to the technique of X-ray crystallography within the context of chemistry research. Students had an opportunity for original experimentation, performing reactions and attempting to grow crystals of reaction products in a school laboratory. The program was remarkably successful, based on student feedback and scientific outcomes. In most cases, the compounds generated by students had not been synthesized before and their structures were previously unknown. X-ray diffraction data were collected on these crystalline products, and the students participated in data analysis and structure determination. New crystal structures were submitted to the international Cambridge Structural Database, with appropriate recognition of the students involved. Two peer-reviewed reports have been accepted for publication in the research literature with the students listed as coauthors. The experiences of the authors in developing this program should be of particular interest to science educators designing outreach activities for high school students.