Synthesis, Isolation, and Spectroscopic Characterization of Holmium‐Based Mixed‐Metal Nitride Clusterfullerenes: HoxSc3−xN@C80 (x=1, 2)

Abstract The synthesis, isolation and spectroscopic characterization of holmium‐based mixed metal nitride clusterfullerenes Ho x Sc 3− x N@C 80 ( x =1, 2) are reported. Two isomers of Ho x Sc 3− x N@C 80 ( x =1, 2) were synthesized by the reactive gas atmosphere method and isolated by multistep recycling HPLC. The isomeric structures of Ho x Sc 3− x N@C 80 ( x =1, 2) were characterized by laser‐desorption time‐of‐flight (LD‐TOF) mass spectrometry and UV/Vis/NIR, FTIR and Raman spectroscopy. A comparative study of M x Sc 3− x N@C 80 (M=Gd, Dy, Lu, Ho) demonstrates the dependence of their electronic and vibrational properties on the encaged metal. Despite the distinct perturbation induced by 4f 10 electrons, we report the first paramagnetic 13 C NMR study on Ho x Sc 3− x N@C 80 (I; x =1, 2) and confirm I h ‐symmetric cage structure. A 45 Sc NMR study on HoSc 2 N@C 80 (I, II) revealed a temperature‐dependent chemical shift in the temperature range of 268–308 K.