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通过非空缺型 Krebs 型多钨酸盐的重排合成首例 Zn-六方夹心型钨锑酸盐。

Synthesis of the first Zn-hexagon sandwich-tungstoantimonate via rearrangement of a non-lacunary Krebs-type polyoxotungstate.

机构信息

Universität Wien, Fakultät für Chemie, Institut für Biophysikalische Chemie, Althanstraße 14, 1090 Wien, Austria.

出版信息

Dalton Trans. 2018 Nov 13;47(44):15651-15655. doi: 10.1039/c8dt02787k.

DOI:10.1039/c8dt02787k
PMID:30334554
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC6256361/
Abstract

A novel synthetic pathway to obtain the first Zn6 hexagon tungstoantimonate [(Zn(H2O))6(B-α-SbW9O33)2]6- ([Zn6-α-SbW9] (1)) via rearrangement of a non-lacunary Krebs-POM precursor (C12N4H11)4K4[(Mn(H2O)3)2((Mn0.5W0.5)O2)2(B-β-SbW9O33)2] ([Mn-β-SbW9]) has been developed. Addition of ortho-phenylenediamine (opda) in order to optimize the synthesis of [Mn-β-SbW9] led to the crystallization of a novel Krebs-type Zn-POM (C12N4H11)4Na5[((Zn0.8W0.2)(H2O)3)2((Zn0.2W0.8)O2)2(B-β-SbW9O33)2] ([(Zn/W)2-β-SbW9] (2)) comprising four disordered Zn-centers after replacement of MnCl2 with ZnCl2. The compounds were characterized in the solid state by single-crystal and powder X-ray diffraction (XRD), IR spectroscopy, thermogravimetric analysis (TGA) and elemental analysis and in solution by UV-vis spectroscopy and ESI-mass spectrometry. The Krebs-POM archetype and the Zn6 hexagon tungstoantimonate have been investigated towards their interactions with Human Serum Albumin (HSA) as a model protein using SDS-PAGE and trypthophan fluorescence quenching.

摘要

一种通过重排非空缺型 Krebs-POM 前体 (C12N4H11)4K4[(Mn(H2O)3)2((Mn0.5W0.5)O2)2(B-β-SbW9O33)2] ([Mn-β-SbW9]) 获得首例 Zn6 六方钨锑酸盐 [(Zn(H2O))6(B-α-SbW9O33)2]6- ([Zn6-α-SbW9] (1)) 的新型合成途径已被开发出来。为了优化 [Mn-β-SbW9] 的合成,添加邻苯二胺 (opda) 导致了一种新型 Krebs 型 Zn-POM (C12N4H11)4Na5[((Zn0.8W0.2)(H2O)3)2((Zn0.2W0.8)O2)2(B-β-SbW9O33)2] ([(Zn/W)2-β-SbW9] (2)) 的结晶,该化合物在 MnCl2 被 ZnCl2 取代后包含四个无序的 Zn 中心。这些化合物通过单晶和粉末 X 射线衍射 (XRD)、红外光谱、热重分析 (TGA) 和元素分析在固态、紫外可见光谱和电喷雾质谱在溶液中进行了表征。Krebs-POM 原型和 Zn6 六方钨锑酸盐已被研究用于与人血清白蛋白 (HSA) 作为模型蛋白的相互作用,使用 SDS-PAGE 和色氨酸荧光猝灭法。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8e77/6256361/e2ec31c45cbe/c8dt02787k-s1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8e77/6256361/7704d02b1036/c8dt02787k-f1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8e77/6256361/e2ec31c45cbe/c8dt02787k-s1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8e77/6256361/7704d02b1036/c8dt02787k-f1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8e77/6256361/e2ec31c45cbe/c8dt02787k-s1.jpg

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