For a typical metalation, 50 mg PyrBpyCMP were dispersed in 4 ml acetonitrile, then 0.32 ml of a 0.015 M suspension of [Cp*RhCl2]2 in acetonitrile were added and the suspension was stirred for 24 h at room temperature. The supernatant was removed by centrifugation and the solid washed with MeOH until the supernatant after centrifugation remains colourless. The solid was dried under reduced pressure first at room temperature, then at 80°C.