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Study On Synthesis, Characterization And Crystal Structure Of Single-oxime Ligands And Its Copper(Ⅱ) And Nickel(Ⅱ)Complexes

Posted on:2015-01-16Degree:MasterType:Thesis
Country:ChinaCandidate:Q ChengFull Text:PDF
GTID:2181330434461046Subject:Inorganic Chemistry
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The carbonyl compounds including ketones or aldehydes reaction withhydroxylamines are kind of very important ligands containing O and N atoms,generates avery important ligands—oxime ligands.It is easy to form metal organiccomplexes,therefore,as a kind of potential chelating agent widely attention.It is easy to formmetal organic complexes.The main reason is the oxygen atoms of oxime compounds havegreat electronegativing and have good coordination with metal atoms.On the base of a large of scientific research,scientists first found that transition metaland their derivatives of complexes exhibit special performance in a few fields,s-uch asfunctional materials,oxidation-reduction,catalysis,etc. Even some oxime com-plexes arehaving relatively excellentanti-cancer,tuberculosis,anti-bacterial pharmaco-logical effectsetc.Therefore,preparing new oxime ligands and their complexes,studyi-ng theirproperties,structures and the relationships between oxime ligands and the me-tal ions, willpiay very important role at research their mechanism of reantion.In this paper,4-aminoacetophenone oxime was synthetized by4-aminoacetoph-enoneand hydroxylamine sulfate. Then, three ligands were synthetized by synthsis by4-aminoacetophenone oxime with3,5-dibromosalicylaldehyde,3-hydroxysalicylaldehyde and4-methoxysalicylaldehyde, respectively. The three ligandsare:HL1(1-(4-{[(E)-3,5-dibromo-2-hydroxybenzylidene]-amino}phenyl)ethanone oxime),H2L2(1-(4-{[(E)-3-hydroxy-2-hydroxybenzylidene]amino}phenyl)ethanone oxime andHL3(1-(4-{[(E)-4-Methoxy-2-hydroxybenzylidene]amino}phenyl)ethanone oxime),respectively.We use4-methoxy with hydroxylamine hydrochloride and salicylaldehydedirectly synthesis of schiff base reaction ligand4, HL4, HL4{[(E)-4-methoxyl-2-hydroxybenzylidene]oxime}.Then, use the synthetic monoxime ligandswith transition metal acetic salt,preaparing their complexes. These ligands and theircomplexes have been characterized by elementary analysis, Infrared spectra analysis,Ultraviolet spectra analysis and X-ray single crystal diffraction et. al. The single crystalsstructures of the ligands and their complexes have been determined by X-ray single crystaldiffraction, and the crystallography date has been shown as below.Try all kinds of training methods of single crystal,and under different solvent systems andcultivate ligands and compounds of single crystal.Eventually developing four single crystalsof the ligands and their complexes, which are HL1, H2L2, two different metalcomplexes,one is Cu(II) complexe with HL3, the other is Ni(II) complexe with HL4.The allhave been obtained by nature evaporation or gaseous diffusion method. Their structures were determined by X-ray single crystal diffraction and the structure parameters are list asfollowing:Crystal data of HL1, empirical formula:C15H12Br2N2O2,Mr:411.90,monoclinic, spacegroup: P2(1)/c, cell parameters: a=12.2181(11),b=15.0209(14),c=8.6640(7),α=90°,β=108.232(1)°,γ=90°,Z=4,V=1510.3(2)3,R1=0.0514,wR2=0.1149;Crystal data of H2L2, empirical formula: C15H13N2O3,Mr:269.08,monoclinic, space group:C2(1)/c, cell parameters:a=17.0284(16),b=15.2097(15),c=14.5756(12),α=90°,β=118.545(2)°,γ=90°,Z=8,V=3316.2(5)3,R1=0.0531,wR2=0.1162;Crystal data of Cu(II) complex with HL3Cu(L3)2, empirical formula:C32H30CuN4O6,Mr:629.76,monoclinic, space group: P2(1)/c, cell parameters:a=10.3561(9),b=17.3002(16),c=8.3000(6),α=90°,β=101.399(2)°,γ=90°,Z=2,V=1457.7(2)3,R1=0.0454,wR2=0.0930;Crystal data of Ni(II) complex with HL4Ni(L4)2, empirical formula:C16H16NiN2O6,Mr:368.91,monoclinic, space group: P2(1)/c, cell parameters:a=6.4406(8),b=18.356(2),c=8.2859(11),α=90°,β=124.633(2)°,γ=90°,Z=2,V=806.02(17)3,R1=0.0600,wR2=0.1476;...
Keywords/Search Tags:Single oxime, Cu(II) Complex, Synthesis, Characterization, Crystalstructure
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