To reproducibly obtain phase-pure ZnSe(L) powders of sufficient crystallinity, we employed a ligand-exchange approach. Powder samples of ZnSe(ba) were incubated at temperatures of 100 (for eea and bza ligands; vide infra) or 140 °C (for all other ligands) in neat ligand for 5 days under autogenous pressure. All samples synthesized by ligand exchange show powder patterns with sharp reflections and distinct from that of the parent ZnSe(ba) (Figure ). The three lowest angle reflections of each powder pattern, which are assigned to the (00n) family of planes, serve to indicate the interlayer spacing between the ZnSe basal planes enforced by the capping ligands in the ligand-exchanged LHs. The interlayer spacing, calculated with Bragg's Law, decreases or increases with respect to that found in ZnSe(ba) in accordance with the length of the exchanged ligand. The ZnSe basal planes remain unchanged after ligand exchange.