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Crystal‐to‐Crystal Transformations in a Seven‐Coordinated Scandium Complex
Author(s) -
Merkens Carina,
Pecher Oliver,
Steuber Friedrich,
Eisenhut Sascha,
Görne Arno,
Haarmann Frank,
Englert Ulli
Publication year - 2013
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201200386
Subject(s) - scandium , monoclinic crystal system , crystallography , triclinic crystal system , chemistry , phase (matter) , phase transition , crystal (programming language) , crystal structure , materials science , inorganic chemistry , condensed matter physics , organic chemistry , physics , computer science , programming language
Aquatris(3‐cyanopentane‐2, 4‐dionato)scandium(III) undergoes two transformations which can be monitored by X‐ray diffraction as well as solid‐state NMR spectroscopy: At 145 K, the mononuclear complex shows a reversible phase transition; in agreement with the symmetry principle, this transition of the t 2 type proceeds from the monoclinic room temperature phase to triclinic twins at low temperature, the twin law corresponding to a twofold rotation. Under vacuum at room temperature, the aqua ligand of the complex is irreversibly eliminated and the structure rearranges, forming a 1D chain polymer. In both phases of the mononuclear complex as well as in the polymer, the coordination polyhedra around the Sc III atom represent distorted capped trigonal prisms. Solid‐state 45 Sc NMR spectroscopic investigations on powder samples reveal a reversible phase transition of the monoclinic complex at low temperatures. Changes of the NMR signal line shapes for the room and low temperature complex as well as the 1D chain polymer are a fingerprint for different scandium bonding situations.