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A 35‐year‐old mystery solved: a facile synthetic route and structural confirmation of tetrachlorobis(diethyl ether)tungsten(IV)
Acta Crystallographica Section C ( IF 0.8 ) Pub Date : 2021-03-12 , DOI: 10.1107/s2053229621002412
Thomas E. Shaw , Alfred P. Sattelberger , Titel Jurca

The true identity of the diethyl ether adduct of tungsten(IV) chloride, WCl4(Et2O)x, has been in doubt since 1985. Initially postulated as the bis‐adduct, WCl4(Et2O)2, questions arose when elemental analyses were more in line with a mono‐ether adduct, viz. WCl4(Et2O). It was proposed that this was due to the thermal instability of the bis‐adduct. Here, we report the room‐temperature X‐ray crystal structure and Hirshfeld surface characteristics of trans‐tetrachloridobis(diethyl ether)tungsten(IV), trans‐WCl4(Et2O)2 or trans‐[WCl4(C4H10O)2]. The compound crystallizes, with half of the molecule in the asymmetric unit, in the centrosymmetric space group P21/n. The W—O distance is 2.070 (2) Å, while the W—Cl distances are 2.3586 (10) and 2.3554 (10) Å.

中文翻译:

一个35岁的谜团得以解决:简便的合成路线和四氯二(二乙醚)钨(IV)的结构确认

自1985年以来,人们就一直怀疑氯化钨(IV)的二乙醚加合物WCl 4(Et 2 O)x的真实身份。最初假定为双加合物WCl 4(Et 2 O)2,这引起了疑问。当元素分析更符合单醚加合物时,即。WCl 4(Et 2 O)。有人提出,这是由于双加合物的热不稳定性所致。在这里,我们报告了室温X射线晶体结构和反式四氯双(二乙基)钨(IV),反式WCl 4(Et 2O)2反式[WCl 4(C 4 H 10 O)2 ]。该化合物在中心对称的空间基团P 2 1 / n中具有一半的分子在不对称单元中结晶。W-O距离为2.070(2)Å,而W-C1距离为2.3586(10)和2.3554(10)Å。
更新日期:2021-04-05
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