Technische Universität Chemnitz, Strasse der Nationen 62, 09111 Chemnitz, Germany.
Chemistry. 2011 Dec 23;17(52):14805-10. doi: 10.1002/chem.201102437. Epub 2011 Nov 25.
The reaction of [Bi(22)O(26)(OSiMe(2)tBu)(14)] (1) in THF with salicylic acid gave [Bi(22)O(24)(HSal)(14)] (2) first, which was converted into [Bi(38)O(45)(HSal)(22)(OH)(2)(DMSO)(16.5)]·DMSO·H(2)O (3·DMSO·H(2)O) after dissolution and crystallization from DMSO. Single-crystal X-ray diffraction analysis and ESI mass spectrometry associated with infrared multi-photon dissociation (IRMPD) tandem MS experiments confirm the formation of the large and quite stable bismuth oxido cluster 3. The reaction of compound 2 with the butoxycarbonyl(BOC)-protected amino acids phenylalanine and valine (BOC-PheOH and BOC-ValOH), respectively, resulted in the formation of chiral [Bi(38)O(45)(BOC-AA)(22)(OH)(2)] (AA=deprotonated amino acid), as shown by a combination of different analytical techniques such as elemental analysis, dynamic light scattering, circular dichroism spectroscopy, and ESI mass spectrometry.
[Bi(22)O(26)(OSiMe(2)tBu)(14)]（1）在四氢呋喃中与水杨酸反应首先得到[Bi(22)O(24)(HSal)(14)]（2），然后将其溶解并从 DMSO 中结晶得到[Bi(38)O(45)(HSal)(22)(OH)(2)(DMSO)(16.5)]·DMSO·H(2)O（3·DMSO·H(2)O）。通过单晶 X 射线衍射分析和 ESI 质谱与红外多光子解离（IRMPD）串联 MS 实验相结合，证实了大而稳定的氧化铋氧簇 3 的形成。化合物 2 与 Boc-保护的氨基酸苯丙氨酸和缬氨酸（BOC-PheOH 和 BOC-ValOH）的反应分别导致手性[Bi(38)O(45)(BOC-AA)(22)(OH)(2)]（AA=脱质子氨基酸）的形成，这通过元素分析、动态光散射、圆二色光谱和 ESI 质谱等多种分析技术的组合得到证实。
