Department of Chemistry, University of Ottawa, 10 Marie-Curie, Ottawa, ON K1N6N5, Canada.
Dalton Trans. 2010 Feb 14;39(6):1504-10. doi: 10.1039/b918082f. Epub 2009 Dec 4.
The synthesis and structure of a novel complex with the formula NaCo(III)(2)(dmo)(2)(mu-N(3))(3)(N(3))(2), , are reported. Complex was synthesized from the reaction of 1-(dimethylamino)propan-2-one oxime (Hdmo), CoCl(2).6H(2)O, and NaN(3) in MeOH. It crystallizes in the monoclinic space group C2/c. The molecular structure consists of one Na(I) and two Co(III) ions bridged by two oxime ligands, two end-to-end azide and three end-on azide anions. The units are linked, forming a 1-D chain. This complex was characterized by UV-Vis spectroscopy where the data confirm the presence of low-spin Co(III) ions. Solid-state (23)Na NMR experiments indicate the presence of one magnetically unique site in the repeating unit, that sample purity in the bulk powdered form is high, and that it possesses microcrystalline order. Solid-state (59)Co NMR experiments at ultra-high field (B(0) = 21.1 T) are in agreement with the structure obtained through X-ray crystallography where the Co(III) ions are coordinated to five nitrogen atoms as well as an oxygen atom.
报道了一种新型配合物NaCo(III)(2)(dmo)(2)(mu-N(3))(3)(N(3))(2)的合成与结构, 。配合物由 1-(二甲氨基)丙-2-酮肟(Hdmo)、CoCl(2).6H(2)O 和 NaN(3)在 MeOH 中反应合成。它在单斜空间群 C2/c 中结晶。分子结构由两个肟配体、两个首尾相连的叠氮化物阴离子和三个端接端接的叠氮化物阴离子桥接的一个 Na(I)和两个 Co(III)离子组成。这些单元通过一维链连接在一起。该配合物通过紫外可见光谱进行了表征,数据证实存在低自旋 Co(III)离子。固态 (23)Na NMR 实验表明,在重复单元中存在一个独特的磁性位点,表明样品在块状粉末形式下的纯度很高,并且具有微晶有序性。在超高磁场 (B(0) = 21.1 T)下进行的固态 (59)Co NMR 实验与通过 X 射线晶体学获得的结构一致,其中 Co(III)离子与五个氮原子以及一个氧原子配位。