CHEMISTRY OF C-TRIMETHYLSILYL-SUBSTITUTED HETEROCARBORANES .13. SYNTHESIS OF A LITHIUM SALT OF 2,3-DICARBA-NIDO-HEXABORATE(1-) - CRYSTAL-STRUCTURE OF THE 1ST DISCRETE C2B4 CARBORANE ANION

被引:12
作者
WANG, Y [1 ]
ZHANG, HM [1 ]
MAGUIRE, JA [1 ]
HOSMANE, NS [1 ]
机构
[1] SO METHODIST UNIV,DEPT CHEM,DALLAS,TX 75275
关键词
D O I
10.1021/om00033a060
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The reaction of nido -2,3- (SiMe3)2-2,3-C2B4H6 with 1 equiv of t-BuLi in TMEDA at 0-degrees-C produces exclusively the solvated monolithium salt [Li(TMEDA)2]+[2,3-(SiMe3)2-2,3-C2B4H5]-(I) as an off-white solid in 84% yield. The H-1, Li-7, B-11 and C-13 NMR spectra and IR spectra of I are all consistent with its crystal structure that is composed of discrete cation and anion units within the unit cell with the closest contact of 5.09 angstrom between them. Compound I crystallizes in the monoclinic space group P2(1/c) with the following unit cell parameters: a = 11.606(5) angstrom, b = 13.459(6) angstrom, c = 20.622-(9) angstrom, beta = 96.94(3)-degrees, V = 3198(2) angstrom3, and Z = 4. Full-matrix least-squares refinements of I converged at R 0.068, and R(w) = 0.078 for 1497 observed reflections.
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页码:3781 / 3784
页数:4
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