Center for Materials Crystallography, Department of Chemistry and iNANO, Aarhus University, Aarhus C, Denmark.
Dalton Trans. 2012 Sep 14;41(34):10347-53. doi: 10.1039/c2dt30278k. Epub 2012 Jul 18.
High resolution single crystal synchrotron X-ray diffraction data measured at 15(2) K were used to solve the structure of the complex intermetallic Zintl phase, Yb(11)AlSb(9) (space group Iba2), made up of Yb cations and polyanions along with isolated Sb anions. The 15(2) K cell parameters are a = 11.7383(4) Å, b = 12.3600(4) Å, c = 16.6796(6) Å. The temperature dependence of the structure was investigated through high resolution synchrotron powder X-ray diffraction (PXRD) data measured from 90 K to 1000 K. Rietveld refinements of the crystal structure revealed near linear thermal expansion of Yb(11)AlSb(9) with expansion coefficients of 1.49(2) × 10(-5) K(-1), 1.71(3) × 10(-5) K(-1), 1.13(1) × 10(-5) K(-1) for a, b and c, respectively. The chemical bonding in Yb(11)AlSb(9) was analyzed using atomic Hirshfeld surfaces, and the analysis supports the presence of the structural elements of Yb cations, AlSb(4) tetrahedra, Sb(2) dimers and isolated Sb(3-) anions. However, indications of interatomic interactions between the Zintl anions and the Yb cations were also observed.
在 15(2) K 下测量的高分辨率单晶同步加速器 X 射线衍射数据用于解决复杂的 Zintl 相 Yb(11)AlSb(9)（空间群 Iba2）的结构，该结构由 Yb 阳离子和多阴离子以及孤立的 Sb 阴离子组成。15(2) K 的晶胞参数为 a = 11.7383(4) Å, b = 12.3600(4) Å, c = 16.6796(6) Å。通过从 90 K 到 1000 K 测量的高分辨率同步加速器粉末 X 射线衍射 (PXRD) 数据研究了结构的温度依赖性。晶体结构的 Rietveld 精修表明 Yb(11)AlSb(9)的热膨胀近乎线性，膨胀系数分别为 1.49(2) × 10(-5) K(-1)、1.71(3) × 10(-5) K(-1)、1.13(1) × 10(-5) K(-1)。使用原子 Hirshfeld 表面分析了 Yb(11)AlSb(9)中的化学键，分析结果支持 Yb 阳离子、AlSb(4)四面体、Sb(2)二聚体和孤立 Sb(3-)阴离子的结构元素的存在。然而，也观察到 Zintl 阴离子和 Yb 阳离子之间的原子间相互作用的迹象。
