Li Qiang, Xiao Zichen, Chen Liye, Zhang Jin
Acta Crystallogr Sect E Struct Rep Online. 2011 Oct 1;67(Pt 10):m1404-5. doi: 10.1107/S1600536811036063. Epub 2011 Sep 20.
The title complex, (C(4)H(9))(4)N[Mo(6)(C(7)H(6)ClN)O(18)], was prepared by the reaction of (Bu(4)N)(4)[α-Mo(8)O(26)] and 2-methyl-5-chloro-aniline hydro-chloride with N,N'-dicyclo-hexyl-carbodiimide as dehydrating agent in dry acetonitrile solution. The aryl-imido ligand is linked to an Mo atom of the Lindqvist-type hexamolybdate anion by an Mo N triple bond, with a bond length of 1.732 (4) Å and an Mo N-C bond angle of 169.1 (4)°, typical for monodentate imido groups in such hybrid complexes. Due to the inter-action between one H atom in the aryl group and an O atom of a symmetry-related hexa-molybdate cluster, the anions form centrosymmetric dimers in the crystal structure. Weak C-H⋯O contacts are observed between the cations and anions. Unresolved disorder in some of the butyl chains of the ammonium cation is noted.
标题配合物[(C₄H₉)₄N]₂[Mo₆(C₇H₆ClN)O₁₈]是通过在干燥乙腈溶液中,以N,N'-二环己基碳二亚胺作为脱水剂,使(Bu₄N)₄[α-Mo₈O₂₆]与2-甲基-5-氯苯胺盐酸盐反应制备而成。芳基酰亚胺配体通过Mo—N三键与Lindqvist型六钼酸根阴离子的一个Mo原子相连,键长为1.732 (4) Å,Mo—N—C键角为169.1 (4)°,这在这类杂化配合物中是单齿酰亚胺基团的典型特征。由于芳基中的一个H原子与一个对称相关的六钼酸根簇的一个O原子之间存在相互作用,阴离子在晶体结构中形成中心对称的二聚体。在阳离子和阴离子之间观察到弱的C—H⋯O接触。注意到铵阳离子的一些丁基链中存在未解析的无序现象。