Mixed valence tungsten(IV,V) compounds with layered structures (Part II1)): Synthesis and crystal structures of Cu1-xW2O2Cl6 and Cu1-xW4O4Cl10

Beck  J; Kusterer  C

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Mixed valence tungsten(IV,V) compounds with layered structures (Part II1)): Synthesis and crystal structures of Cu1-xW2O2Cl6 and Cu1-xW4O4Cl10

机译：具有层状结构的混合价钨（IV，V）化合物（第II1部分）：Cu1-xW2O2Cl6和Cu1-xW4O4Cl10的合成和晶体结构

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The reaction of CuCl with WOCl3 at 400 degrees C leads to a Mixture of Cu1-xW2O2Cl6 (1) and Cu1-xW4O4Cl10 (2) in form of black lustrous needles. Both compounds crystallize in space group C2/m with a = 12.7832(5) angstrom, b = 3.7656(2) angstrom, c = 10.7362(3) angstrom, beta = 119.169(2)degrees for 1 and a = 12.8367(19) angstrom, b = 3.7715(7) angstrom, c = 15.955(3) angstrom, beta = 102.736(5)degrees for 2. The structures are made up of WO2Cl4 octahedra. In the case of 1 two octahedra are edge-sharing via chlorine atoms to form pairs which are linked via the trans-positioned oxygen atoms to form infinite double strands (infinity)(1)W2O4/2Cl2/2Cl4. In the structure of 2 two of these double strands are condensed via terminal chlorine atoms to form quadruple strands (infinity)(1)W4O8/2Cl6/2Cl4. Like for all members of the M-xW2O2X6 structure family (X = Cl, Br) nonstochiometry with respect to the cations M was observed. The copper content of 1 and 2 was derived from the site occupation factors of the respective structure refinements. For several crystals examined the copper content varied between x = 0.27 and 0.17 for 1 and x = 0.04 for 2. In both structures the oxochlorotungstate strands are negatively charged and connected to layers by the monovalent copper ions, which are tetrahedrally coordinated by the non-bridging chlorine atoms of the strands. The structure models imply disorder of the Cu+ ions over closely neighboured sites.

机译：CuCl 与 WOCl3 在 400 °C 下的反应导致 Cu1-x[W2O2Cl6] （1）和 Cu1-x[W4O4Cl10] （2）的混合物，呈黑色有光泽的针状。两种化合物都在空间群 C2/m 中结晶，a = 12.7832（5）埃，b = 3.7656（2）埃，c = 10.7362（3）埃，β = 119.169（2）度 1 和 a = 12.8367（19）埃，b = 3.7715（7）埃，c = 15.955（3）埃，β = 102.736（5）度 2。结构由 WO2Cl4 八面体组成。在 1 的情况下，两个八面体通过氯原子边缘共享以形成对，这些对通过反式定位的氧原子连接以形成无限双链（无穷大）（1）[W2O4/2Cl2/2Cl4]。在结构中 2 其中两条双链通过末端氯原子缩合形成四链（无穷大）（1）[W4O8/2Cl6/2Cl4]。与 M-x[W2O2X6] 结构家族（X = Cl， Br）的所有成员一样，观察到关于阳离子 M 的非化学计量。1 和 2 的铜含量来自各自结构细化的场地占用因素。对于检查的几个晶体，铜含量在 x = 0.27 和 0.17 之间变化，对于 1，x = 0.04 对于 2。在这两种结构中，氧代氯钨酸链都带负电并通过一价铜离子连接到层上，一价铜离子由链的非桥接氯原子四面体配位。结构模型表明Cu+离子在紧密相邻的位点上是无序的。

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《Zeitschrift fur Anorganische und Allgemeine Chemie》 |2008年第3期|587-592|共6页
作者
Beck J; Kusterer C;
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作者单位

Inst Anorgan Chem Univ, D-53121 Bonn, Germany;

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正文语种英语
中图分类化学;
关键词
tungsten; copper; halgenooxotungstates; mixed valence compounds; MICROSCOPY;

机译：钨;铜;卤氧钨酸盐;混合价化合物;显微术;

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Mixed valence tungsten(IV,V) compounds with layered structures (Part II1)): Synthesis and crystal structures of Cu1-xW2O2Cl6 and Cu1-xW4O4Cl10

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