Casellas Hélène, Roubeau Olivier, Teat Simon J, Masciocchi Norberto, Galli Simona, Sironi Angelo, Gamez Patrick, Reedijk Jan
Leiden Institute of Chemistry, PO Box 9502, 2300 RA Leiden, The Netherlands.
Inorg Chem. 2007 May 28;46(11):4583-91. doi: 10.1021/ic0702015. Epub 2007 Apr 18.
Reaction of nickel(II) nitrate with the dpyatriz ligand, namely 2,4,6-tris(bis(pyridin-2-yl)amino)-1,3,5-triazine, in acetonitrile produces a tetranuclear NiII coordination compound, [Ni4(dpyatriz)2(NO3)8(CH3CN)2(H2O)2].2CH3CN (1), the crystal structure of which has been determined by X-ray diffraction using a synchrotron source. 1 has been characterized by IR and UV-vis spectroscopy, elemental and thermogravimetric analyses, and magnetic susceptibility measurements. Its solid-state structure exhibits remarkable anion...pi interactions between coordinated nitrate ions and the triazine rings. In addition, a thorough X-ray powder diffraction study has revealed a number of pseudopolymorphic phases (2-5), resulting from various degrees of hydration/solvation of the [Ni4(dpyatriz)2] core. The interconversion scheme among the different phases has been determined using controlled heating, and the basic structural features of the different pseudopolymorphs have been assessed through ab initio powder diffraction methods.
硝酸镍（II）与dpyatriz配体（即2,4,6-三（双（吡啶-2-基）氨基）-1,3,5-三嗪）在乙腈中反应生成四核NiII配位化合物[Ni4(dpyatriz)2(NO3)8(CH3CN)2(H2O)2].2CH3CN (1)，其晶体结构已通过使用同步辐射源的X射线衍射确定。1已通过红外光谱和紫外可见光谱、元素分析和热重分析以及磁化率测量进行了表征。其固态结构在配位硝酸根离子和三嗪环之间表现出显著的阴离子……π相互作用。此外，一项全面的X射线粉末衍射研究揭示了一些假多晶型相（2 - 5），这些相是由[Ni4(dpyatriz)2]核的不同程度的水合/溶剂化产生的。已使用控制加热确定了不同相之间的相互转化方案，并通过从头算粉末衍射方法评估了不同假多晶型物的基本结构特征。
