The IR Spectra Analysis and Crystal Structure of V3 (μ3-O) (μ2-O2 CEt)6 (O)2 (THF) 2CHCl3

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The title compound (C24H40Cl6O16V3, Mr = 950.08) was synthesizedfrom the reaction of VCl3 and NaO2CEt in CHCl3 and THF. The crystal structure hasbeen determined by X-ray single-crystal diffraction analysis. It crystallizes in monoclinicspace group C2/c with a = 12.5768(4), b= 16.5601(4), c = 19.3574(7) A, β= 99.879(1)°, V = 3971.3(2) A3, Dc= 1.589g/cm3, μ= 1.157 mm-1, F(000)= 1932, Z=4, R = 0.055, wR = 0. 1539 (I≥2σ(I)). This compound has an un-usual coplanar V3O core with a C2 axis passing through O(1), V(1), O(10): one V-μ3O is short (1. 628 A ), the other two are longer (2. 381 A ). It was characterized byIR, 1 H NMR, and EPR spectra. It was unstable and the decomposition process of thiscompound was studied using IR spectroscopy.
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