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Synthesis and Characterization of New 19-Vertex Macropolyhedral Boron Hydrides

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https://figshare.com/articles/dataset/Synthesis_and_Characterization_of_New_19-Vertex_Macropolyhedral_Boron_Hydrides/3626190
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The new boron hydride anions 10-R-B19H19- (R = H, Thx) were synthesized by the reaction of M2[B18H20] (M = Na, K) with HBRCl·SMe2 (R = H, Thx) or HBCl2·SMe2 in diethyl ether. The anions are comprised of edge-sharing, nido 10- and 11-vertex cluster fragments, and are characterized by their 11B, 11B{1H}, and 11B−11B COSY NMR spectra. The salt [(Ph3P)2N][B19H20]·0.5THF crystallized in the triclinic space group P1̄ (a = 12.6344(2) Å, b = 13.5978(2) Å, c = 14.1401(2) Å; α = 77.402(2)°, β = 81.351(2)°, γ = 73.253(2)°). Possible synthetic pathways are discussed. The dianion B19H192- is formed by deprotonation of B19H20- with Proton Sponge (1,8-bis(dimethylamino)naphthalene) in THF, and is identified on the basis of its 11B, 11B{1H}, and 11B−11B COSY NMR spectra.
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2016-08-18
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