“…52,77,78,102 Several reports among these document the preparation of homopolymers with alkyne-functional backbones through condensation or ring-opening polymerization and their subsequent reaction with cobalt 89,103,104 or platinum. 105 To enable the incorporation of multiple types of metallic nanoparticles within the same copolymeric matrix, we are ultimately interested in the preparation of ABC triblock copolymers such as poly(vinylpyridine)-block-polystyreneblock-poly(alkyne-functional monomer) (PVP-PS-PAFm). 91,106 To set the stage for these studies, we began with investigations into the preparation of diblock copolymers of styrene and a range of alkyne-functional monomers, including 4-phenylethynylstyrene, 4-hexynylstyrene, 4-(trimethylsilylethynyl)styrene, 4-[(3-hexynyloxy)-methyl]styrene, and 4-[(3-decynyloxy)methyl]-styrene (Fig.…”