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首页> 外文期刊>Zeitschrift fur Naturforschung, B. A Journal of Chemical Sciences >Synthesis and crystal structures of ATiNb6Cl18 compounds (A = K, Rb, Cs, In, Tl)
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Synthesis and crystal structures of ATiNb6Cl18 compounds (A = K, Rb, Cs, In, Tl)

机译：ATiNb6Cl18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 ATiNb6Cl18 (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 RbTiNb6Cl18 and CsTiNb6Cl18 were determined using single crystal X-ray diffraction. RbTiNb6Cl18 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, CsTiNb6Cl18 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 ATiNb6Cl18 (A = K, In, Tl) were found to be isotypic with RbTiNbsCl(18), and their unit cell parameters were refined using X-ray powder diffraction analysis. References: 19
机译：在720°C的密封石英管中，从NbCl5、金属铌、TiCl3和ACI（A = K、Rb、Cs）或In或Tl金属的化学计量量量开始，合成了与通式ATi[Nb6Cl18]（A = K，Rb，Cs，In，Tl）相对应的新型季铌簇氯化物。采用单晶X射线衍射法测定了RbTi[Nb6Cl18]和CsTi[Nb6Cl18]的结构。RbTi[Nb6Cl18]在菱面体晶体体系中结晶，空间群R（3）超过bar（编号148），Z = 3，晶格参数：a = 9.163（4），c = 25.014（14）埃（六边形设置）。对于所有数据，结构细化收敛为 R-1 = 0.044 和 wR（2） = 0.058。在这种结构中，离散的 [Nb6Cl18]（4-） 团簇单元通过 Rb+ 和 Ti3+ 阳离子连接，分别位于 12 配位的反立方八面体和八面体氯化物配位环境中。相反，CsTi[Nb6Cl18]在三角晶体系统中结晶，空间群P（3）在1c（编号163）上，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-）团簇单元组成，由Cs+和Ti3+阳离子连接，分别位于扭曲的六边形反棱柱形和八面体氯化物配位环境中，发现化合物ATi[Nb6Cl18]（A = K，In，Tl）的结构与RbTi[NbsCl（18）]同型，并利用X射线粉末衍射分析细化了其晶胞参数。[参考文献： 19]

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