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Structure and Thermal Transformations of Methylammonium Tungstate
Zeitschrift für anorganische und allgemeine Chemie ( IF 1.1 ) Pub Date : 2021-08-10 , DOI: 10.1002/zaac.202100219 Ndaru Candra Sukmana 1 , Sugiarto Sugiarto 1 , Zhenxin Zhang 2 , Masahiro Sadakane 3
Zeitschrift für anorganische und allgemeine Chemie ( IF 1.1 ) Pub Date : 2021-08-10 , DOI: 10.1002/zaac.202100219 Ndaru Candra Sukmana 1 , Sugiarto Sugiarto 1 , Zhenxin Zhang 2 , Masahiro Sadakane 3
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Methylammonium paradodecatungstate, (CH3NH3)10[H2W12O42] ⋅ nH2O, was prepared by the reaction of WO3 or H2WO4 in aqueous methylamine, followed by drying. The [H2W12O42]10− anion consists of two HW3O13 groups containing three edge-sharing WO6 octahedra and two W3O14 groups having two edge-sharing connections. On drying the produced material at 70 °C, some lattice water was released, but this did not affect the [H2W12O42]10− structure, although there was a decrease in the unit cell volume. By adding water, the loss of lattice water and structural changes were reversed. The existence of paradodecatungstate anions was confirmed by single-crystal and powder X-ray diffraction, Fourier transform infrared, Raman, 183W nuclear magnetic resonance, and ultraviolet-visible spectroscopy. When the methylammonium paradodecatungstate was heated to more than 150 °C, CH3NH2 and H2O were released, and amorphous WO3 was observed as an intermediate product and monoclinic WO3 as the final product. These results reveal the structure of methylammonium tungstate, which was first reported in 1909 and now is used as an important negative staining reagent for virus observation, is methylammonium paradodecatungstate.
中文翻译：
钨酸甲基铵的结构和热转化
仲十二钨酸甲基铵，(CH 3 NH 3 ) 10 [H 2 W 12 O 42 ] ⋅ n H 2 O，通过WO 3或H 2 WO 4在甲胺水溶液中的反应制备，然后干燥。[H 2 W 12 O 42 ] 10−阴离子由两个 HW 3 O 13基团组成，其中包含三个共享边缘的 WO 6八面体和两个 W 3 O 14具有两个边共享连接的组。在 70 °C 下干燥生产的材料时，会释放一些晶格水，但这并不影响 [H 2 W 12 O 42 ] 10-结构，尽管晶胞体积有所减少。通过加水，晶格水的损失和结构变化得到逆转。通过单晶和粉末 X 射线衍射、傅里叶变换红外、拉曼、183 W 核磁共振和紫外-可见光谱证实了副十二钨酸盐阴离子的存在。当反十二钨酸甲基铵加热到 150 °C 以上时，CH 3 NH 2和 H 2O被释放，观察到无定形WO 3作为中间产物和单斜晶WO 3作为最终产物。这些结果揭示了1909年首次报道并现在用作病毒观察的重要阴性染色试剂的甲基钨酸铵的结构是甲基钨酸铵。
更新日期：2021-10-01
中文翻译：
钨酸甲基铵的结构和热转化
仲十二钨酸甲基铵，(CH 3 NH 3 ) 10 [H 2 W 12 O 42 ] ⋅ n H 2 O，通过WO 3或H 2 WO 4在甲胺水溶液中的反应制备，然后干燥。[H 2 W 12 O 42 ] 10−阴离子由两个 HW 3 O 13基团组成，其中包含三个共享边缘的 WO 6八面体和两个 W 3 O 14具有两个边共享连接的组。在 70 °C 下干燥生产的材料时，会释放一些晶格水，但这并不影响 [H 2 W 12 O 42 ] 10-结构，尽管晶胞体积有所减少。通过加水，晶格水的损失和结构变化得到逆转。通过单晶和粉末 X 射线衍射、傅里叶变换红外、拉曼、183 W 核磁共振和紫外-可见光谱证实了副十二钨酸盐阴离子的存在。当反十二钨酸甲基铵加热到 150 °C 以上时，CH 3 NH 2和 H 2O被释放，观察到无定形WO 3作为中间产物和单斜晶WO 3作为最终产物。这些结果揭示了1909年首次报道并现在用作病毒观察的重要阴性染色试剂的甲基钨酸铵的结构是甲基钨酸铵。
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