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Synthesis And Characterization Of Schiff Base Complexes Of Amino-acids And O-Aminol-phenols

Posted on:2008-03-24Degree:MasterType:Thesis
Country:ChinaCandidate:Y L HaoFull Text:PDF
GTID:2121360215972243Subject:Inorganic Chemistry
Abstract/Summary:PDF Full Text Request
Schiff-base and its transition metal complexes have significant biologic activity in antiviral and antibacterial aspect, and their biologic activity has connection with metal complex, so they are noticeable research objects all the while. Amino acids constitute a essential structural cell because they are the basal building module from which proteins and enzymes are constructed. Meanwhile, amino acids are of difunctional groups, which can coordinate via the carboxylate and/or amino groups. Metal complexes are active centres of biomolecules, such as proteins and enzymes. So it is very impontant to study on amino acids complexes. The researches of heteropolymetallic complexes are intersection which locates in life science and material science, especially the research of heteropolymetallic coupling complexes is the basic of the design in molecule material. The Schiff-base complexes containing phenolic oxygens have become the hotplot, which has been studied extensively by lots of chemists.In view of reasons above, we designed and synthesized 3-carboxyl-salicylaldehyde and its Schiff-base ligands of amino acids and amino-phenol. Meanwhile, we obtained corresponding metal complexes. These complexes MM' L are of strong coupling effect between metal ions. These compounds were characterized by single-crystal X-ray analysis, HNMR, IR, UV-vis, TG, etc. The main contents are described as follow:(1)Schiff-base complex [Cu(HALS)·2H2O]·2H2O, where H3ALS is the 3-carboxyl-salicylidene alanine, was synthesized and characterized by elemental analysis, IR spectra and single-crystal analysis. The crystal belongs to triclinic system, space group P-1, crystal parameter: a=0.7248(5)nm, b=0.8784(6)nm, c=1.820(8)nm,α=81.155(8)°,β=87.591(8)°,γ=87.094(8)°, Z=2, R1=0.0885, wR2=0.2262; The copper atom is in a square-pyramidal field with the base formed by the nitrogen, the phenolic oxygen, carboxyl oxygen of the alanine and a water molecule. Schiff-base complexes Na2Cu2(ALS)2·H2O, Cu3(ALS)2·3H2O, Mn3(ALS)2·H2O, Ni2Cu(ALS)2·6H2O, Cu2Zn(ALS)2·3H2O, Mn2Cu(ALS)2·5H2O and Co3(ALS)2·3H2O were synthesized and characterized with elemental analysis, IR spectroscopy and TG analysis.(2)Schiff-base complex [Cu(HSES)·2H2O]·H2O, where H3SES is the 3-carboxyl-salicylidene serine, was synthesized and characterized by elemental analysis, IR spectra and single-crystal analysis. The crystal belongs to monoclinic system, space group C2/c, a=1.6666(6)nm, b=0.7744(3)nm, c=2.1991(9)nm,α=90°,β=90°,γ=90°, Z=8, R1=0.0510, wR2=0.1211. The copper atom is in the square-pyramidal. Schiff-base complexes Cu3(SES)2·6H2O, Mn(CuSES)2·3H2O, Ni(CuSES)2·5H2O, Zn(CuSES)2·4H2O were synthesized and characterized with elemental analysis, IR spectroscopy and TG analysis.(3) Schiff-base complex [Cu(HVAS)·2H2O]·2H2O·H2O, where H3VAS is the 3-carboxyl-salicylidene valine, was synthesized and characterized by elemental analysis, IR spectra and single-crystal analysis. The crystal belongs to triclinic system, a=0.7679(5)nm, b=0.8528(6)nm, c=1.3794(9)nm,α=96.461(8)°,β=100.605(8)°,γ=108.059(7)°, Z=2, R1=0.0885, wR2=0.2262, Schiff-base complexes Cu3(VAS)2·6H2O, Mn(CuVAS)2·4H2O, Ni(CuVAS)2·4H2O and Zn(CuVAS)2·4H2O were synthesized and characterized with elemental analysis, IR spectroscopy and TG analysis.(4) 3-Carboxylsalicylidene-o-aminophenlol (H3AS) and its complexes Fe3(AS)2·H2O, Mn3(AS)·4H2O, Co3(AS)·2H2O, Ni3(AS)·6H2O and Cu3(AS)·3H2O; 3-Carboxylsalicylidene-2-amino-4-methyphenol (H3AMS) and its complexes Fe3(AMS)2·2H2O, Ni3(AMS)2·6H2O, Co3(AMS)·3H2O, Mn3(AMS)·3H2O and Cu3(AMS)·3H2O were synthesized and characterized with mass spectrum analysis, 1HNMR analysis, IR spectroscopy. Magnetic measurement shows that strong antiferromagetic spin exchange interaction exists in Cu3(AS)·3H2O and Ni3(AS)·6H2O.(5)The complex [Cu(sal)·(C12H8N2)]·4H2O, where sal is the 3-carboxyl-salicylidene, C12H8N2 is 1, 10-phenanthroline, were obtained through selfassembly. Its crystal structure has been determined by X-ray analysis. The crystal belongs to triclinic system, space group P-1. a=0.67302(10)nm, b=1.10211(19)nm, c=1.4883(2)nm,α=109.275(2)°,β=91.991(2)°,γ=103.514(2)°, Z=2, R1=0.0479, wR2=0.1136, The copper atom is in a planar coordination site of N2O2.
Keywords/Search Tags:Characterization
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