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Synthesis, Crystal Structure and Vibrational Spectrum of 2,3,5‐Triphenyltetrazolium Hexachloridoniobate(V) and Oxidotetrachloridoniobate(V) Acetonitrile, [TPT][NbCl 6 ] and [TPT][NbOCl 4 (CH 3 CN)]
Author(s) -
Gjikaj Mimoza,
Xie Tao,
Brockner Wolfgang
Publication year - 2009
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.200900174
Subject(s) - acetonitrile , chemistry , crystallography , raman spectroscopy , octahedron , crystal structure , ion , molecule , ionic bonding , hydrate , infrared spectroscopy , hydrogen bond , organic chemistry , physics , optics
Single crystals of 2,3,5‐triphenyltetrazolium hexachloridoniobate(V) [TPT][NbCl 6 ] ( 1 ) and of 2,3,5‐triphenyltetrazolium oxidotetrachloridoniobate(V) [TPT][NbOCl 4 (CH 3 CN)] ( 2 ) could be obtained and their crystal structures were determined. The structure of 1 is isotypic to that of the recently characterized [TPT][SbCl 6 ] and built up by [TPT] + and octahedral [NbCl 6 ] – ions. The ionic compound 2 contains [TPT] + and [NbOCl 4 (CH 3 CN)] – ions. The nitrogen atom of the acetonitrile solvate molecule is coordinated to the niobium ion in the trans ‐position to the oxido ligand. The Nb–O bond length of 169.6 pm corresponds to a double bond. The [TPT][NbOCl 4 (CH 3 CN)] formation obviously proceeds via NbOCl 3 with the hydrate [TPT]Cl · H 2 O. The FT‐Raman and FT‐IR/FIR spectra of both compounds were recorded and interpreted, especially with respect to the inorganic structure parts. The melting temperatures of 1 and 2 are given.