Synthesis and spectroscopic characterization of methylnitro-closo-hexaborates and crystal structures of cis-(Ph4As)2 [B6H4(CH3)(NO2)], fac-(Ph4As)2[B6H3(CH3)(NO2)2]•CH3CN and mer-(Ph4P)2[B6H3(CH3)(NO2)c2]

被引:0
|
作者
Drewes, C [1 ]
Preetz, W [1 ]
机构
[1] Univ Kiel, Inst Anorgan Chem, D-24098 Kiel, Germany
来源
ZEITSCHRIFT FUR NATURFORSCHUNG SECTION B-A JOURNAL OF CHEMICAL SCIENCES | 1999年 / 54卷 / 03期
关键词
methylnitrotetrahydro-closo-hexaborate(2-); methyldinitrotryhydro-closo-hexaborate(2-); crystal structure; B-11 NMR spectra; vibrational spectra;
D O I
暂无
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
By electrochemical oxidation of (n-Bu4N)[B6H6(CH3)] in the presence of nitrite ions and of the base DBU in dichloromethane solution cis- and trans-[B6H4(CH3)(No-2)](2-), fac- [B6H3(CH3)(NO2)(2)](2-) and mer-[B6H3(CH3)(NO2)(c)(2)](2-) are formed. X-ray diffraction analyses have been performed on single crystals of Cis-(Ph4As)(2)[B6H4(CH3)(NO2)] (1) (monoclinic, space group P2(1)/a, a = 20.063(2), b = 10.858(1), c = 21.384(2) A, beta = 105.818(9)degrees, Z = 4), fac-(Ph4As)(2)[B6H3 (CH3)(NO2)(2)] CH3CN (2) (triclinic, space group <P(1)over bar>, a = 10.333(3), b = 10.695(3), c = 22.833(6) Angstrom, alpha = 93.91(3), beta = 96.79(3), gamma = 101-.56(2)degrees, Z = 2), and mer-(Ph4P)(2) [B6H3(CH3)(NO2)(C)(2)] (3) (triclinic, space group PT, a = 10.100(1), b, = 10.402(3, c = 22.923(3) Angstrom, alpha = 96.328(18), beta = 89.928(12), gamma = 107.963(16)degrees, Z = 2). The B-11 NMR spectra and the vibrational spectra of the methylnitro compounds are discussed and compared with those of the monomethyl- and mononitro-closo-hexaborates.
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页码:349 / 356
页数:8
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