| Syntheses, properties and structures of copper and nickel complexes of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate |
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| 引用本文： | YAO,Tian-Ming YOU,Xiao-ZengCoordination Chemistry Institute,State Key Laboratory of Coordination Chemistry,Nanjing University,Nanjing 210008,ChinaYANG,Qing-ChuanChemistry Department,Beijing University,Beijing 100871,China. Syntheses, properties and structures of copper and nickel complexes of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate[J]. 中国化学, 1994, 12(3): 248-257. DOI: 10.1002/cjoc.19940120309 |
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| 作者姓名： | YAO Tian-Ming YOU Xiao-ZengCoordination Chemistry Institute State Key Laboratory of Coordination Chemistry Nanjing University Nanjing 210008 ChinaYANG Qing-ChuanChemistry Department Beijing University Beijing 100871 China |
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| 作者单位： | YAO，Tian-Ming YOU，Xiao-ZengCoordination Chemistry Institute，State Key Laboratory of Coordination Chemistry，Nanjing University，Nanjing 210008，ChinaYANG，Qing-ChuanChemistry Department，Beijing University，Beijing 100871，China |
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| 基金项目： | Project supported by grants for key research project in climbing program from the State Science and Technology Commission,and the National Nature Science Foundation of China. |
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| 摘 要： | The reaction of CuCl2-2H2O or NiCl2.6H2O with K2(C5H6S4) [potassium salt of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate] under nitrogen atmosphere resulted in the isolation of [Cu(C5H6S4)2]- or [Ni(C5H6S4)2]- as the tetrabutylammonium salt. Both complexes show characteristic IR and UV-Vis absorptions of transition metal dithiolenes. Cyclic voltammograms contain two waves indicating a two step electrochemical procedure [M(C5H6S4)2]0 = [M(C5H6S4)2]1-= [M(C5H6S4)2]2-. Single crystal structure study has been carried out on the nickel complex. Crystal of [Bu4N][Ni(C5H6S4)2] belongs to monoclinic space group P21/c with a=17.576(5), 6=10.883(2), c=17.773(4) A,B=91.07(2)0, Z=4, and o(calcd.)=1.348 g/cm3. Final result is R=0.059 for 2959 reflections. The NiS4 core exhibits square planar coordination with average Ni-S bond length of 2.134(5) A. There are not anion pairs in crystal. The anions stack along a and c axes while the cations intercalate in them. The nearest S-S contact is 4.429 A. The solid powder ESR s
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Syntheses, properties and structures of copper and nickel complexes of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate |
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| YAO,Tian-Ming YOU,Xiao-ZengCoordination Chemistry Institute,State Key Laboratory of Coordination Chemistry,Nanjing University,Nanjing ,ChinaYANG,Qing-ChuanChemistry Department,Beijing University,Beijing ,China. Syntheses, properties and structures of copper and nickel complexes of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate[J]. Chinese Journal of Chemistry, 1994, 12(3): 248-257. DOI: 10.1002/cjoc.19940120309 |
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| Authors: | YAO Tian-Ming YOU Xiao-ZengCoordination Chemistry Institute State Key Laboratory of Coordination Chemistry Nanjing University Nanjing ChinaYANG Qing-ChuanChemistry Department Beijing University Beijing China |
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| Affiliation: | YAO,Tian-Ming YOU,Xiao-ZengCoordination Chemistry Institute,State Key Laboratory of Coordination Chemistry,Nanjing University,Nanjing 210008,ChinaYANG,Qing-ChuanChemistry Department,Beijing University,Beijing 100871,China |
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| Abstract: | The reaction of CuCl2-2H2O or NiCl2.6H2O with K2(C5H6S4) [potassium salt of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate] under nitrogen atmosphere resulted in the isolation of [Cu(C5H6S4)2]- or [Ni(C5H6S4)2]- as the tetrabutylammonium salt. Both complexes show characteristic IR and UV-Vis absorptions of transition metal dithiolenes. Cyclic voltammograms contain two waves indicating a two step electrochemical procedure [M(C5H6S4)2]0 = [M(C5H6S4)2]1-= [M(C5H6S4)2]2-. Single crystal structure study has been carried out on the nickel complex. Crystal of [Bu4N][Ni(C5H6S4)2] belongs to monoclinic space group P21/c with a=17.576(5), 6=10.883(2), c=17.773(4) A,B=91.07(2)0, Z=4, and o(calcd.)=1.348 g/cm3. Final result is R=0.059 for 2959 reflections. The NiS4 core exhibits square planar coordination with average Ni-S bond length of 2.134(5) A. There are not anion pairs in crystal. The anions stack along a and c axes while the cations intercalate in them. The nearest S-S contact is 4.429 A. The solid powder ESR spectrum of the nickel complex shows three broadening signals at g1=2.097, g2=2.042, g3=2.022. Magnetic susceptibility data for [Bu4N][Ni(CgH6S4)2] reveal enhanced anti-ferromagnetic interaction. |
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| Keywords: | Dithiolene complex copper nickel single crystal. |
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