NMR, X-Ray Crystal Structure Studies and Mechanism for Formation of a Novel Di-gallium Complex and 5-Methoxy-4,5,6-triphenyl-4,5-dihydro-1,2,4-triazene-3(2H)-thione

• Published in: Journal of chemical crystallography Vol. 49; no. 3; pp. 131 - 138
• Main Authors: Venkatachalam, T. K., Bernhardt, Paul V., Pierens, G. K., Reutens, D. C.
• Format: Journal Article
• Language: English
• Published: New York Springer US 01-09-2019; Springer Nature B.V
• Subjects: Chemistry; Chemistry and Materials Science; Crystal structure; Crystallography; Crystallography and Scattering Methods; Gallium; Inorganic Chemistry; Lattice parameters; NMR spectroscopy; Organometallic Chemistry; Original Paper; Physical Chemistry; X-ray crystallography; NMR; Synthesis; Triazene; Mechanism
• ISSN: 1074-1542; 1572-8854
• DOI: 10.1007/s10870-018-0745-z

Gallium complexes of bis-thiosemicarbazones were prepared and characterized using NMR and X-ray crystallography. Formation of a gallium nitrate complex was proven by NMR spectroscopy. Surprisingly, this complex was found to convert on standing to a new hydroxido-bridged di-gallium complex. The X-ray crystal structure of the digallium complex is described. Similarly, a triazene compound was formed during the preparation of the gallium complex comprising a tetraphenyl unit in the bis-thiosemicarbazone structure. We propose a mechanism for the formation of both the di-gallium species as well as triazene compound in solution. The lattice parameters for the digallium complex is as follows: a: 17.6854(13) Å, b:16.6492(7) Å, c: 21.4659(14) Å, β = 112.383(8)°.
Graphical Abstract
Gallium complexes of bis-thiosemicarbazones were prepared and were found to convert to a new hydroxido-bridged di-gallium complex