晶体培养描述文献案例2

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晶体培养描述文献案例2

最近，B站有小伙伴留言如图1所示问题。

▲图1 问题描述

该论文为“Eur. J.Inorg. Chem. 2003, 2406–2412.DOI [1]: 10.1002/ejic.200200677.”，其反应示意图如图2所示（由ChemBioDraw[2]绘制），反应和结晶描述如下：

实验描述

大意

A mixture of [N(C4H9)4]4[α-Mo8O26]  (8.00 g, 3.7 mmol), Mn(CH3COO)3·2H2O (1.49  g, 5.6 mmol) and (HOCH2)3CNH2 (1.56 g, 12.8  mmol) in 150 mL of acetonitrile was refluxed for 16 h. The orange solution was  cooled to room temperature and filtered to remove a very fine black solid.  The filtrate was exposed to ether vapor. After 2 h, a white precipitate was  filtered off. The orange filtrate was again exposed to ether vapor for  several days. Large orange crystals were obtained. They were isolated by  filtration, washed with a small amount of acetonitrile and ether, and dried  under vacuum. The crystal for X-ray analysis contained 2 H2O.

将[N(C4H9)4]4[α-Mo8O26]（8.00 g, 3.7 mmol）、Mn(CH3COO)3·2H2O（1.49 g, 5.6 mmol）和(HOCH2)3CNH2（1.56 g, 12.8 mmol）混于150毫升乙腈回流反应16小时。将所得橙色溶液冷却至室温，滤除非常细的黑色固体。将滤液暴露在乙醚蒸气中。2小时后，滤出白色沉淀。过滤后的橙色滤液再次暴露于乙醚蒸气中数日。获得大颗橙色晶体。过滤分离，用少量乙腈和乙醚洗涤，并在真空下干燥。用于X射线分析的晶体含有2分子结晶水。

▲图2 反应式

[N(C4H9)4]3[MnMo6O18{(OCH2)3CNH2}2]·2H2O（CCDC [3]: 189392）结构如图3所示（由Olex2[4]呈现），该结构未添加氢原子，其中一个四丁基铵阳离子的碳原子以及游离水分子未作各向异性精修。

▲图3 CCDC 189392结构

论文可从期刊主页下载，晶体数据可从CCDC晶体数据库下载，也可以从以下链接下载：

链接:https://pan.baidu.com/s/1z-sdqqnGUNXqzyuUWvo8Fg?pwd=k65q

提取码: k65q

参考文献

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[3]   (a)Allen, F. H. The Cambridge Structural Database: A Quarter of a Million CrystalStructures and Rising. Acta Cryst. 2002, B58, 380–388. DOI:10.1107/S0108768102003890. (b) Groom, C. R.; Bruno, I. J.; Lightfoot, M.P.; Ward, S. C. The Cambridge Structural Database. Acta Cryst. 2016, B72, 171–179. DOI:10.1107/S2052520616003954. (c) Mitchell, J.; Robertson, J. H.; Raithby,P. R. Cambridge Crystallographic Data Centre (CCDC). Comprehensive Coordination Chemistry III 2021, 413–437. DOI:10.1016/B978-0-12-409547-2.14829-2.

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