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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Syntheses, solid state and solution structures of the palladium(ii) complexes of malonamide-derived open-chain and macrocyclic ligands
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Syntheses, solid state and solution structures of the palladium(ii) complexes of malonamide-derived open-chain and macrocyclic ligands

机译：丙二酰胺衍生的开链和大环配体的钯（ii）配合物的合成，固态和溶液结构

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摘要

The crystal structures of the palladium(ii) complexes of the open-chain and macrocyclic ligands PdL~1·3H_2O, PdL ~2·6H_2O and PdL~3·5H_2O have been determined (H_2L~1 = 1,4,8,11-tetraazaundecane-5, 7-dione, H_2L~2 = 1,4,8,11-tetraazacyclotetradecane-5,7- dione, H_2L~3 = 1,4,8,11-tetraazacyclotridecane-5,7-dione). The coordination polyhedra of the palladium(ii) ions in all complexes are formed by two deprotonated amide and two amine donors with Pd-N distances being similar in PdL~1 and PdL~2 and substantially shorter in PdL~3. A detailed analysis of the ~1H NMR spectra of the macrocyclic complexes supports the formation in aqueous solution of only N-meso isomers of both compounds in agreement with the X-ray data. The spectra of the palladium(ii) macrocyclic complexes are shifted downfield as a whole as compared to those of the nickel(ii) analogues with the shifts being essentially non-uniform. The latter feature can be related to the differences in magnetic anisotropy of the M-N bonds. The maxima of d-d absorption bands of the palladium(ii) complexes demonstrate weaker dependence on the macrocycle size as compared to those of the nickel(ii) analogues. Both macrocyclic compounds PdL~2·6H_2O and PdL~3·5H _2O are characterized by lamellar crystal structures consisting of interleaved layers formed by macrocyclic units and by water molecules with similar metal complex layers and different 2D water sheets. A columnar crystal structure is inherent for PdL~1·3H_2O with the water molecules present as discrete (H_2O)_3 clusters.
机译：确定了开链和大环配体PdL〜1·3H_2O，PdL〜2·6H_2O和PdL〜3·5H_2O的钯（ii）配合物的晶体结构（H_2L〜1 = 1,4,8,11 -四氮杂十二烷-5，7-二酮，H_2L〜2 = 1,4,8,11-四氮杂环十四烷-5,7-二酮，H_2L〜3 = 1,4,8,11-四氮杂环十三烷-5,7-二酮）。所有配合物中钯（ii）离子的配位多面体由两个去质子化的酰胺和两个胺供体形成，Pd-N距离在PdL-1和PdL-2中相似，而在PdL-3中则短得多。大环配合物的〜1H NMR光谱的详细分析支持两种化合物仅在水溶液中形成X射线数据，这是两种化合物的N-间位异构体。与镍（ii）类似物的光谱相比，钯（ii）大环络合物的光谱总体上向低场偏移，其偏移基本上是不均匀的。后一个特征可以与M-N键的磁各向异性的差异有关。与镍（ii）类似物相比，钯（ii）配合物的d-d吸收带最大值显示出对大环尺寸的依赖性更弱。大环化合物PdL〜2·6H_2O和PdL〜3·5H_2O均具有层状晶体结构，该层状晶体结构由大环单元和具有相似金属络合物层和不同二维水位的水分子形成的交错层组成。 PdL〜1·3H_2O具有固有的柱状晶体结构，水分子以离散的（H_2O）_3簇存在。

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