This two-part laboratory experiment is concerned with investigating key aspects of the Suzuki-- Miyaura cross-coupling reaction. The first part of this experiment utilizes high-throughput experimentation techniques to reinforce, explore, and extend fundamental concepts that are presented in the classroom. In contrast, the second part employs guided-inquiry learning strategies to challenge students to design, set up, and perform a preparative-scale Suzuki-Miyaura reaction and suggest workup and isolation protocols. By design, this experiment, which represents one of the final experiments performed in the third-year undergraduate chemistry laboratory program, serves as a capstone learning experience for students.