A. T. Numan, I. O. Issa, Leqaa Khalid
2008
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journal of kerbala university
Abstract
The [2-hydroxy -1,2-diphynel-ethanone oxime] was reacted with 1,2dichloroethan to give the new ligand [H2L].this ligand was reacted with some metal ions (Co(II),Ni(II),Cu(II),Zn(II) and Cd(II) in methanol as a solvent to give a series of new (1:1)complexes of the general formula [ M(HL)]Cl ,( where : M= Co(II),Ni(II),Cu(II),Zn(II) and Cd(II)) are isolated All compounds have been characterized by spectroscopic methods [ I.R , U.V -Vis ] atomic absorption . Chloride content along with conductivity measurements. From the above data the proposed molecular structure for (Co, Cu, Ni, Zn and Cd) complexes adopting a tetrahedral structure. :ةصلاخلا ذممم ذ ثحبذممم دينجثحبشنمممضتتبرمممت ثحبلامممضت ب [2-[2-(2-Hydroxyimino-1,2-diphenyl-ethoxy)-ethoxy]-1,2diphenyl-ethanone] oxime [H2L] ب ب. ب دمممم ثحب ممممج د ابلممممابمممممثرو ب ب دمممم ة حب مممم ببوممممابذمممم دينجثحب ممممج د ابثمممموبعب دممممك حبوسةممممجكب ،دممممنوبوممممابثنممممسكدحوزنب شمصدن ثح (Co(II),Ni(II),Cu(II),Zn(II) and Cd(II) ب ب ممسنبوببمم د لجثبدلمماوبوة دممكناثح (1:1) ب ب مم ةيتبرممنح بب اد ثحب غنصثحب حرب حذق اثحبلابةذ ذجب جسجا [M(HL)]Cl ب برنح (Co(II),Ni(II),Cu(II),Zn(II) and Cd(II) =M) . ب ب ب ن نلثحبقشلثدبب د كشاثحبوناجب صخش ب ن مس ن ثحبقةملب مششحوبلأحشماتثحب متتب مششحب بب منثدلثح – ب ،شاثح ب من ب مم ستةاثحب نجنممصةلثحب دممنوبوممابعببوبسد ممص تحب دممجسدوبسةممجيثحبدةمملتاوبشممصدن جثباسزممثحبذدممصلاتحب ممنلدنلاو بحةلمسثحب دمبسببيمشبةم وببمنثدتلثحبلمابد نج بدنجصحب لثحب دنل اثحبىج بًحلأدنبب غحش ثحببيشثحبححشلوحبثتب.ب ن،دبش يثح . حذق اثحبونا ث Introduction: Oxim compounds and their complexes play a great importance in medicine, industry, and biochemistry [1]. This in turn has stimulated research into the coordination chemistry of ligands having other functions in addition to the oxime function [2]. One of the analytical application of oxime compounds their use as an were precipitants for some transition metals [3]. Oxime amine compounds play an important role in radiopharmaceuticals and related nuclear medicine [4,6]. Angle off and Co-workers [7] reported the synthesis of 1,10 – phenanthroline – 2.9 –dicarbaldehyeioxime by reacting 1,10phenanthroline-2,9dicarbaldehyde with hydroxylamine, this ligand and its complexes with (Co(II),Ni(II),Cu(II),Zn(II) and Cd(II) were designed as potential agents for nucleis hydrolysis. In this paper the synthesis and characterization new [2-[2-(2-hydroxyimino-1,2diphenyl-ethoxy)-ethoxy]-1,2-diphenyl-ethanone oxime [H2L] which derived from the reaction of [2-hydroxy -1,2-diphynel-ethanone oxime] and [1,2 dichloroethane] were reported and were also studied their metal complexes with cobalt, nickel, copper, zinc and cadmium ions. Experimental: Reagents were purchased form Fluka and Redial – Dehenge chemical Co. I.R spectra were record as ( KBr ) discs using a shimadzu 8300 FTIR spectrophotometer. Electronic spectra of the compounds were measured in the region (200–1100) nm for 10-3 M solution in (DMF) at 25 c using a shimadzu, 160 spectrophotometer 1cm matched quartz cell. While metal Scientific. 2008 4 Journal of Kerbala University , Vol. 6 No. 279 contents of the complexes were determined by atomic absorption (A.A) technique a shimadzu AA 680 G atomic absorption spectrophotometer. The HPLC complexes were determined by using a Shimadzu in this technique 2020.injected into a column of the type (ODS – C18) using (70:30) methanol – water, isocratic system with flow rate (1ml / min) at 25 0C and wave length ( nm). Electrical conductivity measurements of the complexes were recorded of 25c for 10-3 M solutions of the sample in (DMF) using a pw 9526 digital conductivity meter. Synthesis of ligand (H2L): A solution of [1,2dichloroethan] 0.25 g, (2.5 mmol) was added slowly to a mixture of [2hydroxy -1,2-diphynel-ethanone oxime 1.14g, (5.0 mmol) dissolved in methanol 5mL with KOH. The mixture was refluxed for 4hrs, and then stirred at room temperature for 1hrs. Solid was collected by filtration , and dried under vacuum for 24hr , to give [H2L] as Yellow solid , yield 1.5g , 62% m.p ( 131 – 133c ) . Synthesis of complexes: CoCl2 .6H2O (0.074gm, 0.31 mmol) was suspended in 5mL methanol. To this suspension a mixture of 0.15g, (0.31 mmol) of [H2L] in 5mL methanol was added and allowed to reflux for 2hrs. A green precipitate formed, recrystalization washed with 1mL Benzene to give 0.1157g, (65%) m.p (148 – 150 0C) .Synthesis of [Ni (HL)]Cl (2), [Cu(HL)]Cl (3), [Zn (HL)]Cl (4) and [Cd (HL)]Cl Complexes:The method used to prepare these complexes was similar to that mentioned in preparation of [Co (HL)]Cl complex. Table (1) stated weight of starting materials, % yield and some physical properties of the prepared complexes. table (1) some physical properties of the complexes and their reactants quantities. Compound ب ْ ب m.p 0C dec. Color Weight of metal Weight of product (g) Yield % Metal content (calc.) % Chloride content g mmole [Co(HL)]Cl 250 bluegreen 0.074 0.31 0.1157 60 9.66 (9.67) Nil [Ni(HL)]Cl 235 green 0.064 0.31 0.115 60 9.54 (9.64) Nil [Cu(HL)]Cl 242 green 0.053 0.31 0.137 72 12.4 (10.35) Nil