Synthesis, Characterization and Crystal Structure of Complex {[Cu(hmtade)][Ni(dmit)2]}2·4DMSO

Chem. J. Chinese Universities ›› 2009, Vol. 30 ›› Issue (12): 2337.

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Synthesis, Characterization and Crystal Structure of Complex {[Cu(hmtade)][Ni(dmit)₂]}₂·4DMSO

XIE Bin^1,2*, ZHANG Xiu-Lan¹, ZOU Li-Ke^1,2, WANG Jun^1,2, LAI Chuan³, WU Yu^1,2, FENG Jian-Shen^1,2

1.College of Chemistry & Pharmaceutical Engineering,
2. University Key Laboratory of Green Catalyst of Sichuan Province,
3. College of Material & Chemical Engineering, Sichuan University of Science & Engineering, Zigong 643000, China)

Received:2009-06-18 Online:2009-12-10 Published:2009-12-10
Contact: XIE Bin. E-mail: xiebinqhg@sina.com.cn
Supported by:
四川省教育厅科研项目(批准号: 2006A110, 07ZA161)、四川省自贡市科技局科研项目(批准号: 08X01)和材料腐蚀与防护四川省高校重点实验室开放基金项目(批准号: 2008CL04)资助.

Abstract

Abstract:

A new complex {[Cu(hmtade)][Ni(dmit)₂]}₂·4DMSO(1)(hmtade=5,7,7,12,14,14-hexamethyl- 1,4,8,11-tetraazacyclotetradeca-4,11-diene, dmit=4,5-dimercapto-1,3-dithiole-2-thione, DMSO=dimethyl sulfoxide) was synthesized and characterized by means of elemental analysis, Infrared, Ultraviolet-visible spectroscopy, and X-ray structure analysis. Complex 1 belongs to monoclinic system, space group P2₁/n with a=1.49952(6) nm, b=1.77229(7) nm, c=3.1275(1) nm, β=102.442(1)°, V=8.1163(5) nm³, D_c=1.558 Mg/m³, Z=8, F(000)=3944, μ(Mo Kα)=1.637 mm^-1, S=1.016, (Δ/σ)_max=0.001, and final R₁=0.0673, wR₂=0.1672[I>2σ(I)]. Two independent structural units of [Cu(hmtade)][Ni(dmit)₂] are found in an asymmetric unit along with four DMSO solvent molecules. Sulfur-bridged heterometal Cu—Ni complex is formed by one dmit ligand of [Cu(hmtade)][Ni(dmit)₂]. The copper(Ⅱ) ion is a five coordinated square pyramidal environment, with Cu—N distances in the region of 0.1949(5)—0.2007(4) nm and Cu—S distances of 0.28913(18)—0.28952(18) nm. The nickel(Ⅱ) ion which is coordinated by four sulfur atoms of two dmit ligands is in the distorted square geometry, and the Ni—S distances fall in the range of 0.21729(16)—0.21905(17) nm. The N—H…O hydrogen bonds are formed between the nitrogen atom of hmtade ligand and DMSO solvent molecule, and the dimmer is formed through intramolecular S…S and S…H short contacts. Finally, one-dimensional zigzag chain, two-dimensional and three-dimensional networks are formed via S…S, S…C or C…H short contacts.

Key words: 4,5-Dimercapto-1,3-dithiole-2-thione; Tetraazamacrocycle; Complex; Crystal structure

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XIE Bin*, ZHANG Xiu-Lan, ZOU Li-Ke, WANG Jun, LAI Chuan, WU Yu, .... Synthesis, Characterization and Crystal Structure of Complex {[Cu(hmtade)][Ni(dmit)₂]}₂·4DMSO[J]. Chem. J. Chinese Universities, 2009, 30(12): 2337.

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Synthesis, Characterization and Crystal Structure of Complex {[Cu(hmtade)][Ni(dmit)₂]}₂·4DMSO

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