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首页> 外文期刊>Zeitschrift fur Naturforschung, B. A Journal of Chemical Sciences >Synthesis and crystal structures of ATi[Nb6Cl18] compounds (A = K, Rb, Cs, In, Tl)
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Synthesis and crystal structures of ATi[Nb6Cl18] compounds (A = K, Rb, Cs, In, Tl)

机译：ATi [Nb6Cl18]化合物（A = K，Rb，Cs，In，Tl）的合成和晶体结构

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摘要

New quaternary niobium cluster chlorides corresponding to the general formula ATi[Nb6Cl18] (A = K, Rb, Cs, In, Tl) have been synthesized in sealed quartz tubes at 720 degrees C, starting from stoichiometric amounts of NbCl5, niobium metal, TiCl3, and ACI (A = K, Rb, Cs), or In or Tl metals. The structures of RbTi[Nb6Cl18] and CsTi[Nb6Cl18] were determined using single crystal X-ray diffraction. RbTi[Nb6Cl18] crystallizes in the rhombohedral crystal system, space group R (3) over bar (no. 148), Z = 3, with lattice parameters: a = 9.163(4), c = 25.014(14) Angstrom (hexagonal setting). The structure refinement converged to R-1 = 0.044 and wR(2) = 0.058 for all data. In this structure, discrete [Nb6Cl18](4-) cluster units are linked by Rb+ and Ti3+ cations, located in a 12-coordinated anticubeoctahedral and octahedral chloride coordination environment, respectively. In contrast, CsTi[Nb6Cl18] crystallizes in the trigonal crystal system, space group P (3) over bar 1c (no. 163), Z = 2. The lattice parameters were determined to be a = 9.1075(6), c = 17.0017(8) Angstrom. The structure refinement gives the reliability factors R-1 = 0.029 and wR(2) = 0.063 for all data. The structure is built up of discrete octahedral [Nb6Cl18](4-) cluster units, linked by Cs+ and Ti3+ cations which are located in a distorted hexagonal antiprismatic and octahedral chloride coordination environment, respectively The structures of the compounds ATi[Nb6Cl18] (A = K, In, Tl) were found to be isotypic with RbTi[NbsCl(18)], and their unit cell parameters were refined using X-ray powder diffraction analysis. [References: 19]
机译：从化学计量的NbCl5，铌金属，TiCl3开始，在720摄氏度的密封石英管中合成了对应于通式ATi [Nb6Cl18]（A = K，Rb，Cs，In，Tl）的新的季铵簇氯化物，以及ACI（A = K，Rb，Cs）或In或Tl金属。使用单晶X射线衍射确定RbTi [Nb6Cl18]和CsTi [Nb6Cl18]的结构。 RbTi [Nb6Cl18]在菱面体晶体系统中结晶，在棒（编号148）上方的空间群R（3），Z = 3，晶格参数：a = 9.163（4），c = 25.014（14）埃（六边形） ）。对于所有数据，结构优化收敛到R-1 = 0.044和wR（2）= 0.058。在这种结构中，离散的[Nb6Cl18]（4-）簇单元通过Rb +和Ti3 +阳离子相连，分别位于12配位的八面体和八面体氯化物配位环境中。相反，CsTi [Nb6Cl18]在三角晶系中结晶，在棒1c（编号163）上方的空间群P（3），Z =2。晶格参数确定为a = 9.1075（6），c = 17.0017 （8）埃。结构细化给出了所有数据的可靠性因子R-1 = 0.029和wR（2）= 0.063。该结构由离散的八面体[Nb6Cl18]（4-）簇单元组成，这些簇单元分别由Cs +和Ti3 +阳离子连接，分别位于扭曲的六方反棱柱和八面体氯化物配位环境中。化合物ATi [Nb6Cl18]（A ＝ K，In，T1）与RbTi [NbsCl（18）]是同型的，并使用X射线粉末衍射分析对它们的晶胞参数进行精制。 [参考：19]

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