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Synthesis And Structural Characterization Of Schiff Base Complexes

Posted on:2010-06-22Degree:MasterType:Thesis
Country:ChinaCandidate:L ChangFull Text:PDF
GTID:2121360275456263Subject:Inorganic Chemistry
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Schiff bases and their metallic complexes have been widely investigated for more than a century. These complexes have been known for their biological activity and catalytic activity. The preface of this thesis introduces the recent advances in the synthesis and applications of Schiff base and their complexes. They have potential applications as antibacterial reagents, antiviral reagents, anticancer reagents and enzyme inhibitors, etc. Schiff base complexes have been extensively investigated at home and abroad, but the research on 2-nitroaniline Schiff bases is rare, so we synthesized and studied the 2-nitroaniline Schiff bases and their complexes. Moreover, we have also investigated the salen Schiff base complexes.In this paper, we designed and synthesized 2-nitroaniline Schiff base complexes and salen Schiff base complexes. These compounds were characterized by single-crystal X-ray analysis, 1H NMR, IR, UV-vis, TG, etc. The main contents are described as follows:(1) Schiff base complex [Co2(CHNA)2], where H2CHNA is N-(3-carboxylsalicy-lidene)-2-nitroaniline, was synthesized and characterized by IR spectrum, fluorescence spectrum and single-crystal analysis. The crystal belongs to monoclinic system, space group P21/c, crystal parameter: a = 0.83398(6) nm, b = 1.10454(8) nm,c= 1.33681(9) nm,α=90.00°,β=99.6040(10)°,γ=90.00°,Z=2,R1=0.0449,wR2=0.1113. In the molecular unit, the Co(Ⅱ) ions are bridged by two phenolate oxygen atoms of the ligands. Each metal centre has a distorted octahedral geometry.(2) Schiff base complex Cu(SANA)2, where H2SANA is N-salicylidene-2-nitroaniline, was synthesized and characterized by IR spectrum, fluorescence spectrum and single-crystal analysis. The crystal belongs to triclinic system, space group P-1, crystal parameter: a=0.73179(14)nm,b=1.0928(2)nm,c=1.5505(3)nm,α=81.616(4)°,β=81.966(4)°,γ=74.171(4)°,Z=2,R1=0.0683,wR2=0.1628. The copper(Ⅱ) ion is tetracoordinated in a parallelogram geometry, with the ligands acting as bidentate NO-chelators.(3) Schiff base ligand H2OS, N,N'-bis(salicylidene)-o-phenylenediamine, was synthesized and characterized by IR spectrum, 1H NMR and single-crystal analysis. The crystal belongs to monoclinic system, space group P21c, crystal parameter: a=0.59808(5)nm,b=1.65765(14)nm,c=1.63651(15)nm,α=90°,β=91.487°,γ=90°,Z=4,R1=0.0415,wR2=0.1140.(4) Schiff base complex Sn(OS)·Cl2, where H2OS is N,N'-bis(salicylidene)-o-phenylenediamine, was synthesized and characterized by IR spectrum, fluorescence spectrum and single-crystal analysis. The crystal belongs to triclinic system, space group P-1, crystal parameter: a=0.75333(4)nm,b=0.98398(5)nm,c=1.26177(7)nm,α=96.4060(10)°,β=94.6070(10)°,γ=102.8400(10)°,Z=2,R1=0.0270,wR2=0.0669. The tin(Ⅳ) ion is hexacoordinated in a octahedral geometry.(5) Schiff base complex Ni(OS), where H2OS is N,N'-bis(salicylidene)-o-phenylenediamine, was synthesized and characterized by IR spectrum, fluorescence spectrum and single-crystal analysis. The crystal belongs to rhombic system, space group P 2121 21, crystal parameter: a=0.54649(8)nm,b=1.6588r2)nm,c=1.7281(2)nm,α=90°,β=90°,γ=90°,Z=4,R1=0.0246,wR2=0.0551.The nickel atom is in a planar coordination site of [N2O2], and it deviates from the mean plane by only 0.71 pm.(6) The complex [Cu(phen)2Cl]·ClO4·H2O, where phen is 1,10-phenanthroline, was synthesized. Its crystal structure has been determined by X-ray analysis. The crystal belongs to monoclinic system, space group P21/n, a=1.18086(8)nm,b=1.52855(10)nm,c=1.29572(9)nm,α=90°,β=93.1770(10)°,γ=90°,V=2.3352(3)nm3,Z=4,R1=0.0481,wR2=0.1424. The copper atom is in a triangular bipyramid geometry.(7) The ternary complex [Cu(C8H4O4,)(C12H8N2)(H2O)]·(CH3)2NCHO, where C8H4O42- is 3-carboxylsalicylaldehyde dianion and C12H8N2 is o-phenanthroline, was synthesized. The crystal belongs to triclinic crystal system, P-1 space group, with a=0.96936(6)nm,b=1.09020(12)nm,c=1.12800(7)nm,α=103.8340(10)°,β=109.7640(10)°,γ=98.6040(10)°,Z=2,R1=0.0360,wR2=0.1108. The Cu(Ⅱ) ion is pentacoordinated in a tetragonal pyramidal geometry, with two O atoms of 3-carboxylsalicylaldehyde dianion and two N atoms of o-phenanthroline occupying the square plane, and the water's O atom locating at the axial site.
Keywords/Search Tags:Characterization
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