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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Bond distances are not always what they appear to be: discovery and un-discovery of the longest Cr(V) N triple bond
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Bond distances are not always what they appear to be: discovery and un-discovery of the longest Cr(V) N triple bond

机译：键距并不总是看起来像是：最长的Cr（V）N三键的发现和发现

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摘要

The coordination chemistry of CrCl3 with three pentadentate ligands having the [ 1,4,7]-triazacyclononane-1,4-diacetato motif have been investigated. The new resulting six-coordinate Cr(III)-chloro species react cleanly with sodium azide to form the corresponding azido species, which undergo photolysis under irradiation at 419 nm in acetonitrile-water solution to form Cr(V)-nitrido species that are partially hydrolyzed to their corresponding Cr(III)-hydroxo counterparts. Five of these Cr complexes have been characterized by X-ray crystallography. The hydroxo and nitrido species co-crystallize complicating crystal structural refinement. What at first appeared to be the longest Cr N triple bond distance yet observed (1.66 A) was found after re-refinement to be an artifact of positional disorder of the Cr atoms of 73% nitrido and 27% hydroxo species. The re-refined Cr N bond distance is estimated as 1.58 A, which agrees well with the observed Cr N stretching frequency of 971 cm(-1) found by IR spectroscopy. UV-vis data for the "nitrido" complexes suggest that they are all three partially hydrolyzed. These results emphasize the care that must be taken in the characterization of compounds that may co-crystallize with structurally similar analogs.
机译：研究了CrCl3与具有[1,4,7]-三氮杂环壬烷-1,4-二乙酰基的三个五齿配体的配位化学。生成的新六配位Cr（III）-氯物质与叠氮化钠反应干净，形成相应的叠氮基物质，然后在乙腈水溶液中于419 nm的辐射下进行光解，从而部分形成Cr（V）-硝化物质。水解成相应的Cr（III）-羟基对应物这些Cr络合物中的五个已通过X射线晶体学表征。羟基和亚硝基物质共结晶，使晶体结构细化复杂化。重新精制后，最初发现的最长的Cr N三键距离（1.66 A）似乎是73％的亚硝基和27％的羟基物种的Cr原子位置无序的假象。重新精炼的Cr N键距估计为1.58 A，这与通过红外光谱法观察到的971 cm（-1）的Cr N拉伸频率相吻合。 “ nitrido”配合物的紫外可见数据表明它们全部被三个部分水解。这些结果强调在表征可能与结构相似的类似物共结晶的化合物时必须格外小心。

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