Kim Youngsik, Martin Steve W
Department of Materials Science and Engineering, Iowa State University, Ames, Iowa 50011, USA.
Inorg Chem. 2004 May 3;43(9):2773-5. doi: 10.1021/ic035454m.
The thioborate phase Ba7(BS3)4S was synthesized from solid state reaction and its crystal structure determined by single crystal X-ray diffraction analysis. It crystallizes in the monoclinic space group C2/c (No. 15) with a = 10.1750(15) A, b = 23.970(4) A, c = 10.1692(15) A, beta = 90.095(2) degrees, and Z = 4. The structure consists of isolated trigonal planar (BS3)3- anions, and isolated S2- anions and Ba2+ cations. The additional sulfur anions have five-fold barium coordination, while the barium cations are coordinated by eight or nine sulfur atoms. Powder X-ray diffraction patterns from a bulk sample are compared to the calculated diffraction pattern from the single crystal structural analysis, and there is excellent agreement in general. The vibrational modes of the isolated (BS3)3- units were measured from Raman scattering and IR absorption spectra, and the frequencies agree very well with those found for similar orthothioborate phases.
通过固态反应合成了硫代硼酸盐相Ba7(BS3)4S，并通过单晶X射线衍射分析确定了其晶体结构。它结晶于单斜空间群C2/c（编号15），a = 10.1750(15) Å，b = 23.970(4) Å，c = 10.1692(15) Å，β = 90.095(2)°，Z = 4。该结构由孤立的三角平面(BS3)3-阴离子、孤立的S2-阴离子和Ba2+阳离子组成。额外的硫阴离子具有五重钡配位，而钡阳离子由八个或九个硫原子配位。将块状样品的粉末X射线衍射图谱与单晶结构分析计算得到的衍射图谱进行比较，总体上有很好的一致性。从拉曼散射和红外吸收光谱测量了孤立的(BS3)3-单元的振动模式，其频率与类似的正硫代硼酸盐相的频率非常吻合。
