Synthesis of Monohalogeno Derivatives of <i>closo</i>-[B<sub>9</sub>H<sub>9</sub>]<sup>2-</sup>. Crystal Structures of (Ph<sub>4</sub>P)<sub>2</sub>[1-XB<sub>9</sub>H<sub>8</sub>]·CH<sub>3</sub>CN (X = Cl, Br, I)
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By reaction of Na2[B9H9] with the appropriate N-halogenosuccinimide, the monohalogenated anion [1-XB9H8]2- (X = Cl, Br, or I) is formed. The X-ray diffraction analyses performed on single crystals of (Ph4P)2[1-XB9H8]· CH3CN (X = Cl, Br, I) reveal that the tricapped trigonal prismatic geometry of the cluster is retained after substitution in the 1-position. Crystallographic data are as follows for (Ph4P)2[1-XB9H8]·CH3CN. X = Cl, Br: monoclinic, space group P21, a = 10.7 Å, b = 32.9 Å, c = 13.8 Å, β = 96°, Z = 4, R1 = 0.038 and R1 = 0.036, respectively. X = I: monoclinic, space group P21/n, a = 10.5 Å, b = 13.6 Å, c = 33.4 Å, β = 94°, Z = 4, R1 = 0.094. The compounds have been characterized by vibrational and 11B NMR spectroscopy as well.
创建时间：
2016-08-18
