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首页> 外文期刊>Acta Crystallographica Section E: Crystallographic Communications >Trinuclear nickel coordination complexes of phenanthrene-9,10-dione dioxime
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Trinuclear nickel coordination complexes of phenanthrene-9,10-dione dioxime

机译：菲-9,10-二酮二肟的三核镍配合物

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A trinuclear nickel complex of phenanthrene-9,10-dione dioxime (H2pqd), namely bis-[μ2-9,10-bis-(oxido-imino)-phenanthrene]-bis-[μ2-10-(oxido-imino)phenanthrene-9-one oxime](phenanthrene-9,10-dione dioxime)trinickel(II) toluene disolvate, [Ni3(C14H8N2O2)2(C14H9N2O2)2(C14H10N2O2)]·2C7H8, has been isolated and its crystal structure determined. This complex features three independent NiII atoms that are arranged in a triangular fashion along with five supporting ligands. There are two square-planar NiII atoms and a third pseudo-octa-hedral NiII atom. While the square-planar NiII atoms are stacked, there are no ligand bridges between them. Each square-planar NiII atom, however, bridges with the pseudo-octa--hedral NiII atom through Ni—N—O—Ni and Ni—O—Ni bonds. A fluorido-bor-ation reaction of the proton-bridged species gave the analogous complex bis-(μ2-bis-{[10-(oxido-imino)-9,10-di-hydro-phenanthren-9-yl-idene]amino}di-fluorido-borato)(phenanthrene-9,10-dione dioxime)trinickel(II) dichloromethane trisolvate, [Ni3(C28H16BF2N4O2)4(C14H10N2O2)]·3CH2Cl2, which shows the same binding structure, but features a widened Ni—Ni inter-action between the square-planar NiII atoms. The proton-bridged complex completes the macrocyclic coordination around the square-planar NiII atoms by means of an O—H?O hydrogen bond. Both compounds feature O—H?N hydrogen bonds between the oxime and the N atoms attached to square-planar nickel atom. The nickel units show no direct inter-action with their nearest neighbors in the extended lattice. Two π-stacking inter-actions between adjacent mol-ecules are found: one with a centroid–centroid distance of 3.886?(2)?? and the other with a centroid–centroid distance of 4.256?(3)??. In the latter case, although not aromatic, the distance to the centroid of the central phenanthrene ring is shorter, with a distance of 3.528?(3)??. Toluene mol-ecules occupy the solvent channels that are oriented along the c axis. In the fluorido-boronate structure, the solvent (DCM) was too badly disordered to be modelled, so its contribution was removed using SQUEEZE [Spek (2015). Acta Cryst. C71, 9–18].
机译：菲-9,10-二酮二肟（H2pqd）的三核镍配合物，即双-[μ2-9,10-双-（氧化亚氨基）-菲]-双-[μ2-10-（氧化亚氨基）分离出菲-9-9肟（菲-9,10-二酮二肟）三镍（II）甲苯，[Ni3（C14H8N2O2）2（C14H9N2O2）2（C14H10N2O2）·2C7H8，并确定其晶体结构。该络合物的特征是三个独立的NiII原子与五个支撑配体以三角形方式排列。有两个正方形平面的NiII原子和第三个伪八面体NiII原子。当方形NiII原子堆叠时，它们之间没有配体桥。但是，每个方形NiII原子都通过Ni-N-O-Ni和Ni-O-Ni键与拟八面体NiII原子桥接。质子桥联物种的氟硼酸酯化反应得到类似的复合物双-（μ2-双-{[[10-（氧化亚氨基）-9,10-二氢菲蒽-9-亚基]氨基}-二氟-硼酸酯（菲-9,10-二酮二肟）三镍（II）二氯甲烷三溶剂化物，[Ni3（C28H16BF2N4O2）4（C14H10N2O2）]·3CH2Cl2，具有相同的结合结构，但具有较宽的Ni -Ni平面镍原子之间的相互作用。质子桥联的配合物通过OH H 2 O氢键完成围绕方形NiII原子的大环配位。这两种化合物的特征都是在肟和与方形镍原子相连的N原子之间存在OHHN氢键。镍单元与延伸晶格中的最近邻域没有直接相互作用。发现相邻分子之间有两个π堆积相互作用：一个质心-质心距离为3.886？（2）？另一个质心-质心距离为4.256？（3）??。在后一种情况下，尽管不是芳族的，但到中心菲环的质心的距离更短，为3.528π（3）π。甲苯分子占据沿c轴定向的溶剂通道。在氟硼酸硼酸盐结构中，溶剂（DCM）的杂乱性太强而无法建模，因此使用SQUEEZE删除了其贡献[Spek（2015）。 Acta Cryst。 C71，9-18]。

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