Mixed halocarborane anions, 1-H-CB11Y5X6- (X, Y = Cl, Br, I), have been prepared by treatment of [Me3NH]-[1-H-CB11H5X6] (X = Cl, Br, I) with proper halogenating reagents at 180-220 degreesC in a sealed tube in high yield. These new anions are fully characterized by H-1, C-13, and B-11 NMR, IR, and negative-ion MALDI MS spectroscopy. Some are further confirmed by single-crystal X-ray analyses. The weakly coordinating nature of these anions is probed by Si-29 chemical shifts of the resulting Pr3Si(1-H-CB11Y5X6) compounds. The results suggest that the coordinating ability of these anions is mainly dependent on the substituents at 7-12 positions (namely, X atoms), and the contribution from the upper belt substituents Y is relatively small. These suggestions are consistent with the results obtained from the structural study of silver salts of mixed halo- and perhalocarborane anions.
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