Kato Chika Nozaki, Kato Daichi, Kashiwagi Toshifumi, Nagatani Shunpei
Department of Chemistry, Shizuoka University, 836 Ohya, Suruga-ku, Shizuoka 422-8529, Japan.
Research Institute of Green Science and Technology, Shizuoka University, 836 Ohya, Suruga-ku, Shizuoka 422-8529, Japan.
Materials (Basel). 2019 Jul 26;12(15):2383. doi: 10.3390/ma12152383.
The synthesis and molecular structure of a dimeric, mono-aluminum complex composed of two tri-lacunary α-Dawson polyoxometalates, [HAl(B-α-PWO)] (1), is described herein. The tetra--butylammonium salt of 1, [(-CH)N][HAl(B-α-PWO)] (TBA-1) was prepared by passing an aqueous solution of K[B-α-HPWO{Al(OH)}]⋅14HO through an ion-exchange resin column (H-form), followed by addition of tetra--butylammonium bromide. Analytically pure and colorless crystals of TBA-1 were obtained via vapor diffusion from acetonitrile/methanol at ~25 °C. Single-crystal X-ray structure analysis revealed that a six-coordinate aluminum ion was sandwiched between two tri-lacunary α-Dawson-type units, resulting in an overall symmetry. The characterization of TBA-1 was accomplished by elemental analyses, thermogravimetric/differential thermal analyses, Fourier-transform infrared spectroscopy, and solution P nuclear magnetic resonance spectroscopy. The photochromic properties of TBA-1 were also characterized in methanol under light irradiation (λ = 365 nm and ≥400 nm).
本文描述了一种由两个三缺位α-道森多金属氧酸盐组成的二聚单铝配合物[HAl(B-α-PWO)] (1)的合成及其分子结构。1的四丁基铵盐[(-CH)N][HAl(B-α-PWO)] (TBA-1)是通过使K[B-α-HPWO{Al(OH)}]⋅14HO的水溶液通过离子交换树脂柱(H型)，然后加入四丁基溴化铵制备的。通过在约25℃下从乙腈/甲醇中进行气相扩散获得了分析纯的无色TBA-1晶体。单晶X射线结构分析表明，一个六配位铝离子夹在两个三缺位α-道森型单元之间，从而产生了整体对称性。通过元素分析、热重/差热分析、傅里叶变换红外光谱和溶液P核磁共振光谱对TBA-1进行了表征。还在光照(λ = 365 nm和≥400 nm)下于甲醇中对TBA-1的光致变色性质进行了表征。
