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Syntheses, Crystal Structue Rs And Spectroscopic Prope Rties Of Single-Oxime Ligands And Its Co(Ⅱ) And Ni(Ⅱ) Complexes

Posted on:2016-08-15Degree:MasterType:Thesis
Country:ChinaCandidate:H X GuoFull Text:PDF
GTID:2271330464974204Subject:Inorganic Chemistry
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Oxime compounds are a kind of special important ligand s, because those ligands contain nitrogen and oxygen atom. This kind of compounds are obtained by the reaction of the aldehydes or ketones with hydroxylamine. As this kind of compounds contain(-C=N-OR) groups, So they can be widely used in analytical chemistry, coordination chemistry and metal metallurgy. O xime compounds contain oxygen atoms which have large electronegativity and better coordination effect with metal atoms,so it is easy to form a metal-organic complexe.People pay more attentions to chemical properties of oxime compounds, because they are widely used in the sterilization, insecticidal, anti-cancer and anti- viral and other fields, especially in analytical chemistry, medicine, metal corrosion and functional materials. So preparation of new oxime type ligand s and their metal complexes and studying of their properties, structures and interactions between metal ions and ligands play important role in development of coordination chemistry.In this thesis, two kinds of intermediate are obtained by the reaction of the 4-amino acetophenone with methoxyammonium hydrochloride and ethoxyamine hydrochloride, respectively. Then HL1: 1-(4-{[(E)-5-bromine-2- hydroxy benzene methylene] amino} aceto phenone)methoxy oxime, HL2:1-(4-{[(E)-3,5-dibromo-2- hydroxy benzene methylene] amino} acetophenone) methoxy oxime, HL3:1-(4-{[(E)-4-methoxy-2-hydroxy benzene methylene] amino} acetophenone) methoxy oxime, HL4:1-(4-{[(E)-3,5-dichloro-2- hydroxy benzene methylene chloride] amino} acetophenone) ethoxy oxime, HL5:1-(4-{[(E)-3,5-dibromo-2-hydroxy benzene methylene] amino} acetophenone)ethoxy oxime, HL6:1-(4- {[(E)-3 ethoxy methylene]-2-hydroxy benzene amino} acetophenone)methoxy oxime and HL7:1-(4- {[(E)-5 nitro-2- hydroxy benzene methylene] amino} acetophenone) methoxy oxime are obtained by the reaction of the two kinds of intermediate with Salicylaldehyde derivatives. Those compounds were characterizated by melting point, solubility analysis, elemental analysis, IR, UV absorption spectroscopy and analytical testing methods conventionally.Five single crystals of ligands and metal complexes(HL1, HL2-Co(II) complex, HL2-Ni(II) complex, HL4, HL5) are obtained by method of natural volatilization in the different solvent system,respectively. By using of X-ray single crystal diffraction analysis to determine these complexes composition and spatial configuration. Crystallography data are as follows:HL1: Empirical formula, C16H14 Br N2O2, Formula weight, 346.20, Crystal system, Monoclinic, Space gyoup, P2(1)/c, Unit call dimensions: a = 33.758(5) ?, b = 7.1117(16) ?, c = 6.2194(9) ?, α = 90°, β = 92.133(13)°, γ = 90°, Z =4, V = 1492.1(5) ?3, R1 = 0.0718, w R2= 0.2267;HL2-Co(Ⅱ): Empirical formula, C32H26Br4 Co N4O4, Formula weight, 909.10, Crystal system, Monoclinic, Space gyoup, Cc, Unit call dimensions: a = 17.4281(16) ?, b = 16.5658(15) ?, c = 23.3340(19) ?, α = 90°, β = 101.226(2)°, γ = 90°, Z =8, V = 6607.9(10) ?3, R1 = 0.0557, w R2 = 0.1158;HL3-Ni(Ⅱ): Empirical formula, C34H34N4 Ni O6, Formula weight, 653.36, Crystal system, Monoclinic, Space gyoup, P2(1)/c, Unit call dimensions: a = 10.5538(5) ?, b = 6.1691(2) ?, c = 24.2831(9) ?, α = 90°, β = 100.519(4)°, γ = 90°, Z =2, V = 1554.44(11) ?3, R1 = 0.0402, w R2 =0.0973;HL4: Empirical formula, C17H16Cl2N2O2, Formula weight, 351.22, Crystal system, Monoclinic, Space gyoup, P2(1)/c, Unit call dimensions: a = 9.1238(4) ?, b = 13.0575(4) ?, c = 14.3740(5) ?, α = 90°, β = 104.616(4)°, γ = 90°, Z =4, V = 1657.02(11) ?3, R1 = 0.0460, w R2 =0.1120;HL5: Empirical formula, C17H17Br2N2O2, Formula weight, 441.14, Crystal system, Monoclinic, Space gyoup, P2(1)/c, Unit call dimensions: a = 9.2648(14) ?, b = 13.3034(16) ?, c = 14.510(2) ?, α = 90°, β =105.261(15)°, γ = 90°, Z = 4, V = 1725.3(4)?3, R1 = 0.0708, w R2 = 0.2141;...
Keywords/Search Tags:Single Oxime, Co(Ⅱ) Complex, Ni(Ⅱ) Complex, Synthesis, Crystal Structure, Characterization
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