Elsevier

Ultrasonics Sonochemistry

Volume 41, March 2018, Pages 590-599
Ultrasonics Sonochemistry

Sonochemical synthesis and characterization of new seven coordinated zinc, cadmium and mercury nitrate complexes: New precursors for nanostructure metal oxides

https://doi.org/10.1016/j.ultsonch.2017.10.025Get rights and content

Highlights

  • The nitrate complexes of group 12 elements with a tridentate ligand were synthesized.

  • X-ray diffraction analysis shows that the central metal is seven-coordinated.

  • The geometry around metal center is a distorted pentagonal bipyramid.

  • Hirshfeld surfaces (HS) analysis was used for further investigation of the structure.

  • The direct thermolysis of zinc and cadmium nitrate complexes led to metal oxide nanoparticles.

Abstract

The nitrate complexes of group 12 elements with a tridentate Schiff base ligand (L = (E)-N1-((E)-3- phenylallylidene)-N2-(2-((E)-((E)-3-phenylallylidene) amino)ethyl) ethane-1,2-diamine) were synthesized via sonochemical process and characterized by various physical and chemical methods. The structural analysis of the zinc nitrate complex by single crystal X-ray diffraction analysis shows that the central atom is seven-coordinated by three nitrogen atoms from the Schiff base ligand as well as four oxygen atoms from two different nitrate anions. The geometry around the metal center can be described as a distorted pentagonal bipyramid. The crystal packing analysis of zinc nitrate complex indicates that the intermolecular interactions related to nitrate groups plays the essential role in the orientation of supramolecular structure. Hirshfeld surfaces (HS) and their corresponding fingerprint plots (FP) have been also used for further investigation of crystal structure of zinc nitrate complex. Furthermore thermal analyses (TG/DTG) of three nanostructure complexes were carried out and discussed. Finally, direct thermolysis of zinc and cadmium nitrate complexes in air atmosphere led to the production of zinc and cadmium oxide nanoparticles.

Introduction

There is a demonstrated interest in the synthesis and structural characterization of metal complexes particularly in areas including catalysis, medicine, agriculture, polymer industries, bioinorganic chemistry, microbiology and optical industries [1], [2], [3], [4], [5], [6]. By the combination of different types of ligands and metal ions in varied ratios the synthesis of a range of metal coordination compounds can be achieved providing the opportunity to design various compounds for different scientific purposes [7]. Among the various metal compounds, those with Schiff base ligands are significant [8]. These ligands are readily prepared and coordinate with a broad spectrum of metal ions. Under favourable conditions some Schiff base complexes can form extended supramolecular structures stabilized by non-covalent intermolecular interaction such as hydrogen bonding [9] that extend their applications to include solar cells [10], biological systems [11], magnetic and conducting materials [12], gas storage [13], nano-materials [14], catalytic and pharmaceutical industry [15], [16]. The broad scope of structural properties demonstrated by Schiff base complexes underlies their important role in many scientific applications. Synthesis of coordination compounds in nano-meter size is a new trend in inorganic chemistry and has attracted much attention due to their unique properties which arise due to the large number of surface molecules in comparison to the bulk [17], [18]. Among the different methods that have been used for the synthesis of nano structures, the sonochemical procedure has become popular due to the rapid synthesis, product quality, environmentally friendly and low cast [19], [20]. A literature survey indicates that synthesis of different inorganic Zn, Cd and Hg compounds have been reported [21], [22], [23], [24] but the reports for nano structure coordination compound with tridentate Schiff base ligands and their use as precursors for the preparation of nanostructure metal oxide are rarely found. Metal oxides play a key role in many areas of science [25]. In technological applications, oxides are used in the fabrication of microelectronic devises, sensors, catalysts, ceramics, optoelectronic devices, anticorrosion coatings and fuel cells [26], [27]. Herein, we extend our previous work [28], [29], [30], [31], [32], [33], and report the synthesis and characterization of some new Zn, Cd and Hg complexes of a tridentate Schiff base ligand entitled as (E)-N1-((E)-3-phenylallylidene)-N2-(2-((E)-((E)-3-phenylallylidene) amino) ethyl) ethane-1, 2-diamine. The nano-structure and metal oxide of the complexes were also prepared under ultrasonic irradiation and calcination method respectively.

Section snippets

Materials and methods

All materials used in the synthetic and analytical procedures were purchased from Merck, Aldrich and/or BDH chemical companies in high purity and were used as received.

For recording of UV–Visible spectra of the compounds in the range of 200–800 nm, a JASCO-V570 spectrophotometer instrument was applied. The FT/IR spectrum of all compounds were carried out on a JASCO-FT/IR680 instrument in the range of 4000–400 cm−1 as KBr discs. 1H and 13C NMR spectra of the ligand and its zinc, cadmium and

Physical and analytical data

Based on physical and analytical data collected in Table 1, the general formula; ML(NO3)2 (M = Zn, Cd and Hg) is proposed for the complexes that has been presented in Scheme 1. The X-ray crystallography of ZnL(NO3)2 proved the suggested structure for the complexes as exhibited in Scheme 1. All compounds are stable at room temperature. Chloroform, dichloromethane, dimethylformamide and dimethylsulfoxide are suitable solvents for the synthesized compounds as the solubility test indicated. Melting

Conclusion

Three new metal nitrate complex with general formula of ML(NO3)2 (M = Zn, Cd and Hg and L = (L = (E)-N1-((E)-3- phenylallylidene)-N2-(2-((E)-((E)-3-phenylallylidene) amino)ethyl) ethane-1,2-diamine) prepared via ultrasonic method and characterized by various physical and chemical techniques. The crystal structure of ZnL(NO3)2 was determined by single crystal X-ray diffraction analysis. On the basis of structural data, the zinc atom is coordinated to three nitrogen atoms from schiff base ligand

Acknowledgement

Partial support of this work by Yasouj University is acknowledged.

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