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Horky, Katrin and Schnick, Wolfgang ORCID logoORCID: https://orcid.org/0000-0003-4571-8035 (2017): Ba₃₂[Li₁₅Si₉W₁₆N₆₇O₅]: A Barium-Containing Oxonitridolithotungstosilicate with a Highly Condensed Network Structure. In: European Journal of inorganic Chemistry, No. 7: pp. 1100-1106

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Abstract

The oxonitridolithotungstosilicate Ba-32[Li15Si9W16N67O5] was synthesized by metathesis reaction of the reactive starting compounds Si(NH)(2), LiNH2, LiF, and BaH2 in a radiofrequency furnace at 1000 degrees C by using tungsten crucibles. Single crystals of Ba-32[Li15Si9W16N67O5] were obtained as a byproduct from reaction of the starting materials with the crucible. The crystal structure was solved and refined on the basis of single-crystal X-ray diffraction data [P2(1)/n (no. 14), a = 8.3402(3), b = 8.5465(3), c = 16.6736(6)angstrom, beta = 99.1950(10)degrees, Z = 1, R-1(all) = 0.0302]. Ba-32[Li15Si9W16N67O5] is the first oxonitridolithotungstosilicate containing a three-dimensional network of vertex- (WN4) and edge-sharing (LiN3O, Li/SiN3O, and SiN3O) tetrahedra with Ba2+ ions that fill the voids of the structure. The network is characterized by channels of funfer rings running along [100] as well as channels of sechser and achter rings along [010]. Magnetic measurements verified an oxidation state of +VI for W. X-ray spectroscopy, lattice energy calculations with MAPLE, and X-ray diffraction confirmed the chemical composition and the structural model of Ba-32[Li15Si9W16N67O5]. IR spectra corroborated the absence of N-H bonds. The optical band gap of Ba-32[Li15Si9W16N67O5] has been determined by UV/Vis spectroscopy.

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