SYNTHESIS AND CRYSTAL STRUCTURE OF M[NB6CL15] (M=IN, TL) - NEW TERNARY NIOBIUM HALIDES WITH BRIDGED [NB6CL18](4-) CLUSTERS

Womelsdorf H.; Lachgar A.; Meyer HJ.

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SYNTHESIS AND CRYSTAL STRUCTURE OF M[NB6CL15] (M=IN, TL) - NEW TERNARY NIOBIUM HALIDES WITH BRIDGED [NB6CL18](4-) CLUSTERS

机译：M [NB6CL15]（M = IN，TL）-桥接[NB6CL18]（4-）簇的新型三元铌的合成及晶体结构

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New ternary niobium chlorides corresponding to the formula M[Nb6Cl15] (M = In, Tl) were synthesized from solid state reactions of NbCl5, niobium metal, and MCl3 at 720 degrees C. The crystal structure of In[Nb6Cl15] was determined from single crystal X-ray diffraction studies. The structure was refined in the orthorhombic symmetry (space group Pmma, Z=4) with a=1786.6(1)pm, b=1345.52(8)pm, c = 929.34(8) pm, R-F = 0.028 and R-W = 0.037, GooF = 1.06 for ail 1552 unique reflections. The lattice parameters of the isotypic Tl[Nb6Cl15] compound were refined from X-ray powder diffraction data: a = 1785.9(2)pm, b = 1347.2(2) pm, c = 930.2(1) pm. The structure of In[Nb6Cl15] is made up of [Nb6Cl18](4-) clusters linked to each other through terminal chloride ligands to form two sets of chains perpendicular to each other. The chains are linked through other terminal ligands to yield a three-dimensional network. The In+ or Tl+ ions are located in a ten coordination site (distorted bicapped cubic geometry) made up of eight inner and two outer chloride ligands. [References: 28]

机译：由NbCl5，铌金属和MCl3在720摄氏度的固相反应合成了新的与式M [Nb6Cl15]（M = In，Tl）对应的三元氯化铌。In[Nb6Cl15]的晶体结构由单晶确定晶体X射线衍射研究。该结构以正交对称（空间组Pmma，Z = 4）进行了精炼，a = 1786.6（1）pm，b = 1345.52（8）pm，c = 929.34（8）pm，RF = 0.028和RW = 0.037，对于所有1552个唯一反射，GooF = 1.06。从X射线粉末衍射数据中细化了同型Tl [Nb6Cl15]化合物的晶格参数：a = 1785.9（2）pm，b = 1347.2（2）pm，c = 930.2（1）pm。 In [Nb6Cl15]的结构由[Nb6Cl18]（4-）簇组成，这些簇通过末端氯化物配体相互连接，形成两组互相垂直的链。链通过其他末端配体连接以产生三维网络。 In +或Tl +离子位于由八个内部和两个外部氯化物配体组成的十个配位位置（扭曲的二阶立方几何形状）中。 [参考：28]

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《Zeitschrift fur Anorganische und Allgemeine Chemie》 |1997年第6期|共5页
作者
Womelsdorf H.; Lachgar A.; Meyer HJ.;
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正文语种 eng
中图分类化学;
关键词
Innb6cl15; Tlnb6cl15; Preparation; Crystal structure; Chemistry; Chlorides; Tantalum; Units;

机译：In [nb6cl15];Tl [nb6cl15];制备;晶体结构;化学性质;氯化物;钽;单位;

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SYNTHESIS AND CRYSTAL STRUCTURE OF M[NB6CL15] (M=IN, TL) - NEW TERNARY NIOBIUM HALIDES WITH BRIDGED [NB6CL18](4-) CLUSTERS

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