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首页> 外文期刊>Chemistry: A European journal >Metal-and Ligand-Directed One-Pot Syntheses, Crystal Structures, and Properties of Novel Oxo-Centered Tetra-and Hexametallic Clusters
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Metal-and Ligand-Directed One-Pot Syntheses, Crystal Structures, and Properties of Novel Oxo-Centered Tetra-and Hexametallic Clusters

机译：金属和配体定向的一锅合成，晶体结构和新型以氧为中心的四元和六金属簇的性质

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Starting from closely related metal-ligand combinations, completely differenic oligomeric metal clusters are synthesized. Whereas, picoline-tetrazolylamide HL~1 (1) and zinc or nickel acetate afforded [2 X 2] grids [M_4(L~1)_8] (2), slightly different N-(2-methylthiazole-5-yl)-thiazole-2-carboxamide HL~2 (5a) and nickel acetate yielded the monometallic complex [Ni(L~2)_2(OH_2)_2] (6). In contrast, reaction of 5a with zinc acetate produced the tetrametallic zinc cluster [Zn_4O(L~2)_4(OAc))2] (7). Even more surprising, when 3-methyl-substituted HL~3 (5b) instead of 2-methyl-substituted HL~2 (5a) was allowed to react under identical conditions with zinc acetate, the cluster [Zn_4O(L~3)_4Cl_2] (8) crystallized from dichloromethane. Clusters 7 and 8 areisostructural. As for 7, in 8 two of the edges of the tetrahedron of zinc ions are doubly bridged, two are singly bridged, and the other two are nonbridged. On the otherhand, when iron(II) acetate under aerobic conditions was allowed to react with 5a, the unprecedented complex [{Fe_3O(L~2)_2(OAc)_4}_2O] (9) was isolated. Cluster 9 is composed of two trimetallic, triangular mu_3-O~(2-)-centered [Fe_3O(L~2)_2(OAc)_4]~+ modules, linked by an almost linear mu_2-O~(2-) bridge. The Mossbauer spectrum together with cyclic voltammetric and square wave voltammetric measurements of 9 are reported, and 6-9 were characterized unequivocally by single-crystal X-ray structure analyses.
机译：从紧密相关的金属-配体组合开始，可以合成完全不同的低聚金属簇。而甲基吡啶-四唑基甲酰胺HL〜1（1）和醋酸锌或镍镍提供[2 X 2]网格[M_4（L〜1）_8]（2），略有不同的N-（2-甲基噻唑-5-基）-噻唑-2-羧酰胺HL〜2（5a）和乙酸镍生成单金属络合物[Ni（L〜2）_2（OH_2）_2]（6）。相反，5a与乙酸锌反应生成四金属锌簇[Zn_4O（L〜2）_4（OAc））2]（7）。更令人惊讶的是，当3-甲基取代的HL〜3（5b）代替2-甲基取代的HL〜2（5a）在相同条件下与乙酸锌反应时，簇[Zn_4O（L〜3）_4Cl_2 〔8〕从二氯甲烷中结晶。聚类7和8是同构的。至于7，在8个锌离子四面体的边缘中有两个是双桥的，两个是单桥的，另外两个是非桥的。另一方面，当使好氧条件下的乙酸铁（II）与5a反应时，分离出前所未有的络合物[{Fe_3O（L〜2）_2（OAc）_4} _2O]（9）。团簇9由两个以三金属，以mu_3-O〜（2-）为中心的三角形[Fe_3O（L〜2）_2（OAc）_4]〜+模块组成，通过几乎线性的mu_2-O〜（2-）桥连接。报告了Mossbauer光谱以及9次的循环伏安法和方波伏安法测量，并且通过单晶X射线结构分析明确地表征了6-9个。

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