Synthesis and structural characterization of highly chlorinated, brominated, iodinated, and methylated carborane anions, 1-H-CB9X9-, 1-NH2-CB9X9- (X = Cl, Br, I), and 1-H-CB9(CH3)9-

被引：53

作者：

Tsang, CW ^{[1
]}

Yang, QC ^{[1
]}

Sze, ETP ^{[1
]}

Mak, TCW ^{[1
]}

Chan, DTW ^{[1
]}

Xie, ZW ^{[1
]}

机构：

[1] Chinese Univ Hong Kong, Dept Chem, Shatin, Hong Kong, Peoples R China

来源：

INORGANIC CHEMISTRY | 2000年 / 39卷 / 16期

关键词：

D O I：

10.1021/ic000137q

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

The highly chlorinated, brominated, and iodinated carborane anions 1-R-CB9X9- (R = H, NH2; X = Cl, Br, I) were prepared in high yields by treatment of [Me3NH][1-R-CB9H9] with excess ICI, Br-2/triflic acid, and I-2/triflicacid, respectively, in sealed tubes at 180-240 degrees C. With the aid of a Pd catalyst, B-I bonds could be converted into the B-Me bonds by treatment with excess MeMgBr, which led to the preparation of the permethylated species 1-H-CB9Me9- in good yield. These new anions were fully characterized by H-1, C-13, and B-11 NMR, IR, and negative-ion MALDI MS spectroscopy. Some were further characterized by single-crystal X-ray analyses. The weakly coordinating nature of these new anions was probed by Si-29 chemical shifts.

引用

页码：3582 / 3589

页数：8

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