Low-Temperature Syntheses and Characterization of Novel Layered Tellurites, A(2)Mo(3)TeO(12) (A = NH(4), Cs), and "Zero-Dimensional" Tellurites, A(4)Mo(6)Te(2)O(24).6H(2)O (A = Rb, K).
Low-Temperature Syntheses and Characterization of Novel Layered Tellurites, A(2)Mo(3)TeO(12) (A = NH(4), Cs), and "Zero-Dimensional" Tellurites, A(4)Mo(6)Te(2)O(24).6H(2)O (A = Rb, K).
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DOI：
10.1021/ic980102e
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发表时间：
1998-08
影响因子：
4.6
通讯作者：
Vidyavathy Vidyavathy Balraj-Vidyavathy;K. Vidyasagar
中科院分区：
文献类型：
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作者：
Vidyavathy Vidyavathy Balraj-Vidyavathy;K. Vidyasagar
本文报道了新的A（2）Mo（3）TeO（12）（A = NH（4），Cs，Rb，K）化合物的水热合成研究。采用水热法合成了新型非中心对称层状碲酸盐（NH（4））（2）Mo（3）TeO（12）（1）和Cs（2）Mo（3）TeO（12）（2）。它们的结构包含二维六方钨氧化物相关的（Mo（3）TeO（12））（2）（-）阴离子层与NH（4）（+）/Cs（+）离子交错。通过简单的化学计量比反应物在水中的还原反应，合成了新的零维碲酸盐Rb（4）Mo（6）Te（2）O（24）·6 H（2）O（3）和K（4）Mo（6）Te（2）O（24）·6 H（2）O（4），它们含有中心对称的（Mo（6）Te（2）O（24））（4）（-）阴离子聚集体和碱金属离子.在六钼二碲酸盐阴离子中，Mo（6）O（24）平面六角环，由六个MoO（6）八面体的边缘共享形成，两侧被碲覆盖。这两种类型的阴离子具有相同的经验式。Cs（2）Mo（3）TeO（12）（2）也可以通过固相反应制备。所有四个新的碲酸盐已通过单晶X射线衍射研究的结构特征。相关晶体，数据如下：对于1，六方P6（3）空间群，a = 7.332（2）<$，c = 12.028（4）<$，Z = 2：对于2，六方P6（3）空间群，a = 7.3956（10）<$，c = 12.186（2）<$，Z = 2; 3，单斜空间群P2（1）/c，a = 10.0564（14），B = 9.877（8），c = 15.724（3），β = 109.988（11）度，Z = 2;对4，单斜空间群P2（1）/c，a = 9.878（3），B = 9.724（4），c = 15.301（3），β = 108.57（2）度，Z = 2.化合物1-4的低温合成，结构，粉末X-射线衍射，光谱和热研究进行了描述。
Hydrothermal synthetic investigations to prepare new A(2)Mo(3)TeO(12) (A = NH(4), Cs, Rb, K) compounds are described. Novel noncentrosymmetric layered tellurites, (NH(4))(2)Mo(3)TeO(12) (1) and Cs(2)Mo(3)TeO(12) (2), have been synthesized by hydrothermal methods. Their structures contain two-dimensional hexagonal tungsten oxide related (Mo(3)TeO(12))(2)(-) anionic layers interleaved with NH(4)(+)/Cs(+) ions. New "zero-dimensional" tellurites, Rb(4)Mo(6)Te(2)O(24).6H(2)O (3) and K(4)Mo(6)Te(2)O(24).6H(2)O (4), containing discrete centrosymmetric (Mo(6)Te(2)O(24))(4)(-) anionic aggregates and alkali metal ions have been synthesized by simple refluxing of stoichiometric reactants in water. In this hexamolybdoditellurite anion, the Mo(6)O(24) flat hexagonal ring, formed from edge sharing of six MoO(6) octahedra, is capped by tellurium on both sides. The two types of anions have the same empirical formula. Cs(2)Mo(3)TeO(12) (2) could be prepared by a solid state reaction as well. All four new tellurites have been structurally characterized by single-crystal X-ray diffraction studies. Pertinent crystal, data are as follows: for 1, hexagonal space group P6(3), a = 7.332(2) Å, c = 12.028(4) Å, Z = 2; for 2, hexagonal space group P6(3), a = 7.3956(10) Å, c = 12.186(2) Å, Z = 2; for 3, monoclinic space group P2(1)/c, a = 10.0564(14) Å, b = 9.877(8) Å, c = 15.724(3) Å, beta = 109.988(11) degrees, Z = 2; for 4, monoclinic space group P2(1)/c, a = 9.878(3) Å, b = 9.724(4) Å, c = 15.301(3) Å, beta = 108.57(2) degrees, Z = 2. Low-temperature syntheses, structure, and powder X-ray diffraction, spectroscopic, and thermal studies of compounds 1-4 are described.