Synthesis and Characterization of the First Tetracyanamidogallate

• Published in: European journal of inorganic chemistry Vol. 2013; no. 36; pp. 6091 - 6096
• Main Authors: Kalmutzki, Markus, Ströbele, Markus, Kroeker, Scott, Wren, John E. C., Meyer, H. Jürgen
• Format: Journal Article
• Language: English
• Published: Weinheim WILEY-VCH Verlag 09.12.2013; WILEY‐VCH Verlag; Wiley Subscription Services, Inc
• Subjects: Crystal structure; Cyanamidogallates; Decomposition reactions; Diffraction; Diffraction patterns; Disorders; Metathesis; NMR spectroscopy; Solid-state reactions; Spinning; Tubes; X ray diffraction
• ISSN: 1434-1948; 1099-0682
• DOI: 10.1002/ejic.201301090

A tetracyanamidogallate with the formula LiSr2[Ga(CN2)4] was prepared from stoichiometric mixtures of SrF2, GaF3, and Li2(CN2) in a fused silica tube. The formation of LiSr2[Ga(CN2)4] by solid‐state metathesis was studied by differential scanning calorimetry. A crystalline powder of LiSr2[Ga(CN2)4] was studied by X‐ray powder diffraction, and powder patterns were indexed isotypically to LiSr2[Al(CN2)4]. The crystal structure of LiSr2[Ga(CN2)4] was refined by single‐crystal X‐ray diffraction, thus indicating a disorder of Li+ and Ga3+ ions that was investigated by the means of 71Ga solid‐state magic‐angle spinning (MAS) NMR spectroscopic measurements and DFT calculations. The employment of the solid‐state metathesis reaction has been used for the development of the tetracyanamidogallate compound LiSr2[Ga(CN2)4], the structure of which contains infinite chains of corner‐sharing [LiGa(CN2)4]4– tetrahedra.