Nguyen Hung Huy, N. Huy, T. T. Nguyet, Pham Chien Thang
{"title":"Picolinoyl(4-乙基硫代氨基脲)及其新型杂电性Cu(II)配合物的合成与结构表征","authors":"Nguyen Hung Huy, N. Huy, T. T. Nguyet, Pham Chien Thang","doi":"10.25073/2588-1140/vnunst.5342","DOIUrl":null,"url":null,"abstract":"The ligand picolinoyl(4-ethylthiosemicarbazide) HL was synthesized by the reaction of picolinohydrazide and ethyl isothiocyanate in absolute ethanol. The structure of HL was characterized by spectroscopic methods such as IR, 1H, and 13C NMR spectroscopy. One-pot reaction of CuCl2 and equimolar amounts of HL and o-phenanthroline in CH2Cl2/MeOH mixture with the presence of a supporting base like pyridine gave rise to a new heteroleptic cationic Cu(II) complex with the composition of [Cu(L)(o-phen)]+. Crystalline PF6– salt was obtained after workup with (n-Bu4N)(PF6) and single-crystal structure of the complex was determined. The spectroscopic data and X-ray crystallography demonstrated that the Cu(II) ion is five-coordinate with the coordination sphere consisted of (S, N1, Npyridine) and (N, N) donor sets belonging to the singly deprotonated ligand {L–} and o-phenanthroline, respectively.","PeriodicalId":23524,"journal":{"name":"VNU Journal of Science: Natural Sciences and Technology","volume":"50 1","pages":""},"PeriodicalIF":0.0000,"publicationDate":"2022-11-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Synthesis and Structural Characterization of Picolinoyl (4-ethylthiosemicarbazide) and its New Heteroleptic Cu(II) Complex\",\"authors\":\"Nguyen Hung Huy, N. Huy, T. T. Nguyet, Pham Chien Thang\",\"doi\":\"10.25073/2588-1140/vnunst.5342\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"The ligand picolinoyl(4-ethylthiosemicarbazide) HL was synthesized by the reaction of picolinohydrazide and ethyl isothiocyanate in absolute ethanol. The structure of HL was characterized by spectroscopic methods such as IR, 1H, and 13C NMR spectroscopy. One-pot reaction of CuCl2 and equimolar amounts of HL and o-phenanthroline in CH2Cl2/MeOH mixture with the presence of a supporting base like pyridine gave rise to a new heteroleptic cationic Cu(II) complex with the composition of [Cu(L)(o-phen)]+. Crystalline PF6– salt was obtained after workup with (n-Bu4N)(PF6) and single-crystal structure of the complex was determined. The spectroscopic data and X-ray crystallography demonstrated that the Cu(II) ion is five-coordinate with the coordination sphere consisted of (S, N1, Npyridine) and (N, N) donor sets belonging to the singly deprotonated ligand {L–} and o-phenanthroline, respectively.\",\"PeriodicalId\":23524,\"journal\":{\"name\":\"VNU Journal of Science: Natural Sciences and Technology\",\"volume\":\"50 1\",\"pages\":\"\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2022-11-24\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"VNU Journal of Science: Natural Sciences and Technology\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.25073/2588-1140/vnunst.5342\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"VNU Journal of Science: Natural Sciences and Technology","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.25073/2588-1140/vnunst.5342","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
Synthesis and Structural Characterization of Picolinoyl (4-ethylthiosemicarbazide) and its New Heteroleptic Cu(II) Complex
The ligand picolinoyl(4-ethylthiosemicarbazide) HL was synthesized by the reaction of picolinohydrazide and ethyl isothiocyanate in absolute ethanol. The structure of HL was characterized by spectroscopic methods such as IR, 1H, and 13C NMR spectroscopy. One-pot reaction of CuCl2 and equimolar amounts of HL and o-phenanthroline in CH2Cl2/MeOH mixture with the presence of a supporting base like pyridine gave rise to a new heteroleptic cationic Cu(II) complex with the composition of [Cu(L)(o-phen)]+. Crystalline PF6– salt was obtained after workup with (n-Bu4N)(PF6) and single-crystal structure of the complex was determined. The spectroscopic data and X-ray crystallography demonstrated that the Cu(II) ion is five-coordinate with the coordination sphere consisted of (S, N1, Npyridine) and (N, N) donor sets belonging to the singly deprotonated ligand {L–} and o-phenanthroline, respectively.