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吡罗昔康及其金属配合物的结构研究、光谱、热、X射线和质谱表征

Structure investigation, spectral, thermal, X-ray and mass characterization of piroxicam and its metal complexes.

作者信息

Zayed M A, Nour El-Dien F A, Mohamed Gehad G, El-Gamel Nadia E A

机构信息

Chemistry Department, Faculty of Science, Cairo University, Giza, Egypt.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2004 Oct;60(12):2843-52. doi: 10.1016/j.saa.2003.12.051.

Abstract

M(H2L)22.yH2O (where H2L: neutral piroxicam (Pir), A: Cl- in case of Ni(II) or acetate anion in case of Cu(II) and Zn(II) ions and y=0-2.5) and M(H2L)3z.yH2O (A: SO4(2-) in case of Fe(II) ion (z=1) or Cl(-) in case of Fe(III) (z=3) and Co(II) ions (z=2) and y=1-4) chelates are prepared and characterized using elemental analyses, IR, magnetic and electronic reflectance measurements, mass spectra and thermal analyses. IR spectra reveal that Pir behaves a neutral bidentate ligand coordinated to the metal ions through the pyridyl-N and carbonyl-O of the amide moiety. The reflectance and magnetic moment measurements reveal that these chelates have tetrahedral, square planar and octahedral geometrical structures. Mass spectra and thermal analyses are also used to confirm the proposed formulae and the possible fragments resulted from fragmentation of Pir and its chelates. The thermal behaviour of the chelates (TGA and DTA) are discussed in detail and the thermal stability of the anhydrous chelates follow the order Ni(II) congruent with Cu(II) Fe(II)<Zn(II)<Fe(III)<Co(II) chelates. The water molecules are removed in the first step while the Pir molecule is removed in the second and subsequent steps. X-ray powder diffraction was also used as a confirmatory tool to elucidate the crystallinity of the chelates.

摘要

制备了M(H₂L)₂₂·yH₂O(其中H₂L:中性吡罗昔康(Pir),A:Ni(II)时为Cl⁻,Cu(II)和Zn(II)离子时为醋酸根阴离子,y = 0 - 2.5)和M(H₂L)₃ₓ·yH₂O(A:Fe(II)离子时为SO₄²⁻(x = 1),Fe(III)时为Cl⁻(x = 3),Co(II)离子时为Cl⁻(x = 2),y = 1 - 4)螯合物,并通过元素分析、红外光谱、磁性和电子反射测量、质谱和热分析对其进行了表征。红外光谱表明,Pir表现为中性双齿配体,通过酰胺部分的吡啶基-N和羰基-O与金属离子配位。反射率和磁矩测量表明,这些螯合物具有四面体、平面正方形和八面体几何结构。质谱和热分析也用于确认所提出的化学式以及Pir及其螯合物碎片化产生的可能碎片。详细讨论了螯合物的热行为(热重分析和差示热分析),无水螯合物的热稳定性顺序为Ni(II)≅Cu(II)<Fe(II)<Zn(II)<Fe(III)<Co(II)螯合物。第一步去除水分子,第二步及后续步骤去除Pir分子。还使用X射线粉末衍射作为确认工具来阐明螯合物的结晶度。

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