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Synthesis, Isolation, and Spectroscopic Characterization of Holmium‐Based Mixed‐Metal Nitride Clusterfullerenes: Ho x Sc 3− x N@C 80 ( x =1, 2)
Author(s) -
Zhang Yang,
Popov Alexey A.,
Schiemenz Sandra,
Dunsch Lothar
Publication year - 2012
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.201200574
Subject(s) - holmium , characterization (materials science) , nitride , metal , isolation (microbiology) , materials science , crystallography , chemistry , physics , nanotechnology , metallurgy , optics , laser , layer (electronics) , microbiology and biotechnology , biology
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.