Hydrothermal synthesis and crystal structure of an inorganic-organic hybrid heteropolymolybdate (C 4 H 16 N 3 ) 2 [NiMo
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TRUCTURE OF ORGANIC COMPOUNDS
Hydrothermal Synthesis and Crystal Structure of an Inorganic–Organic Hybrid Heteropolymolybdate (C4H16N3)2[NiMo12O40]Cl2 ⋅ 9H2O1 M. M. Ftini and A. Haddad Laboratoire de Matériaux et Cristallochimie (LMC), Département de Chimie, Faculté des Sciences Monastir, Tunisie email: [email protected] Received June 12, 2013
Abstract—A novel inorganic–organic hybrid polyoxomolybdate (C4H16N3)2[NiMo12O40]Cl2 ⋅ 9H2O has been synthesized under hydrothermal conditions and structurally caracterised by elemental analysis, TG, IR and single crystal Xray diffraction. The crystals are orthorhombic, a = 10.138(3) Å, b = 19.508(2) Å, c = 26.790(4) Å, Z = 4, sp. gr. Pcnb. Keggin polyoxomolybdate anion [NiMo12O40]4–, protonated diethylen etriamine molecules, chloride anions and water molecules are linked via a large number of hydrogen bonds. DOI: 10.1134/S1063774514060091 1
INTRODUCTION The chemistry of polyoxometalates (POMs) is rap idly growing field because of their applications in diverse areas, such as biomedical chemistry, optical material, eletrochromism, catalysis, magnetism, sorp tion properties, etc., as well as the diversity of their structures [1–8]. One of the recent advance is the exploration of combining POMs and organic mole cules via selfassembly through intermolecular weak interactions that could lead to a variety of interesting properties [9, 10]. The first polyanion [PMo12O40]3– was reported by Berzelius and then structurally determined by Keggin [11–13]. The general formula of such anions can be expressed as [XM12O40]n– (M = W, Mo; X = P, Si, B, Ge, etc). Crystal structures of many Keggin anions have been reported, such as [PMo12O40]3– [14] and [SiMo12O40]4– [15]. Interestingly, [SiM12O40]4– (M = Mo, W) is usually present in combination with organic ammonium cations [15–27]. [GeMo12O40]4– repre sents an example of 1D organic–inorganic hybrid based on a Keggintype structure and an isopolyanion [Mo6O22]8– [28]. Another compound containing poly anion [GeMo12O40]4– represents a structure in which POMs form inorganic layer [29]. Limited examples of Keggin polyoxometalates [ZnM12O40]6–, only [NiMo12O40]6– and [CoMo12O40]6– have been repre sented [30, 31]. Our aim was to synthesize new organic–inorganic hybrid materials containing the Keggintype POMs [NiMo12O40]4– and the organic polyamine molecule as 1 The article is published in the original.
a counterion by hydrothermal reactions. In this paper, we report the hydrothermal synthesis of dode camolybdonickelate (C4H16N3)2[NiMo12O40]Cl2 ⋅ 9H2O. The structure of the compound was characterized by single crystal Xray diffraction, infrared spectroscopy, elemental analysis and thermogravimetric analysis. EXPERIMENTAL Hydrothermal syntheses. A mixture of ammonium molybdate tetrahydrate (NH4)6[Mo7O24] ⋅ 4H2O (1.23 g, 1 mmol) and nickel chloride hexahydrate NiCl2 ⋅ 6H2O (0.138 g, 0.5 mmol) were dissolved in 50 mL of water. Diehylenetriamine (H2N–C2H4– NH–C2H4–NH2) (1 mL, 1mmol) was added slowly to the mixture under stirring and the p
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