Microsoft Word - 209-225 209 | Chemistry 2016) عام 1العدد ( 29مجلة إبن الهيثم للعلوم الصرفة و التطبيقية المجلد Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 Synthesis and Characterization of [Benzyl (2-hydroxy-1- naphthylidene) hydrazine carbodithioate] and Its Metal Complexes With [Co(II), Ni(II), Cu(II), Zn(II), and Cd(II)] Ions Basim I. Al-Abdaly Noor K. Ahmed Dept. of Chemistry/ Collage of Science/ University Baghdad Received in:17/September/2015,Accepted in:12/October/2015 Abstract The formation of Co(II), Ni(II), Cu(II), Zn(II), and Cd(II)-complexes (C1-C5) respectively was studied with new Schiff base ligand [benzyl(2-hydroxy-1-naphthalidene) hydrazine carbodithioate derived from reaction of 2-hydroxy-1-naphthaldehyde and benzyl hydrazine carbodithioate. The suggested structures of the ligand and its complexes have been determined by using C.H.N.S analyzer, thermal analysis, FT-IR, U.V-Visible, 1HNMR, 13CNMR , conductivity measurement , magnetic susceptibility and atomic absorption. According to these studies, the ligand coordinates as a tridentate with metal ions through nitrogen atom of azomethane , oxygen atom of hydroxyl, and sulfur atom of thione and the ratio of ligand to metal (M:L) as (1:2) all the complexes were octahedral except copper-complex was distorted octahedral. Key words: Schiff base ligand. 210 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 Introduction Schiff bases are typically formed by the condensation of a primary amine and an aldehyde or ketone. Schiff bases are generally bidentate, tridentate, tetradentate or polydentat ligands [1]. The type of aliphatic Schiff's bases are relatively unstable in aqueous acid or base solution where hydrolyzed back to their aldehydes or ketones and amines, while aromatic counterparts are stable due to the resonance [2,3] . Schiff bases are the significant compounds owing to their wide range of biological activities and industrial applications [4]. Benzyl hydrazinecarbodithioate (SBDTC) is interesting due to the fact that its derivatives have the potential to be modified in various ways by introducing several different substituents [5]. 2-Hydroxy Schiff base ligands are very important due to the existence of (O–H···N and N–H···O) type hydrogen bonds tautomer’s between of enol- imine and keto-enamine forms [6]. The spectra of different Schiff -bases have been studied in polar and nonpolar solvents and mixed solvents, it was established that the tautomeric equilibrium in 2-hydroxy-1-naphthylidene aniline Schiff bases depend on the polarity of the solvent, the acidity of the medium, the temperature and the strength of the hydrogen bond[7]. Schiff bases are used in drug. It is well known that the shape of a certain molecule is the most important factor that affects drug activity. The four major factors that affect the properties of a drug are: its ability to chelate with metal ions, its lipophilicity, steric effects and electronic effects [8]. This paper reports the synthesis and characterization of new Schiff base ligand derived from reaction 2-hydroxy-1- naphthaldehyde and benzyl hydrazine carbodithioate and its complexes with Co(II), Ni(II), Cu(II), Zn(II) and Cd(II). Experimental Materials and instruments All reagents and solvents are of highest purity and used as obtained from the manufacture. Melting points were determined by using (Gallenkamp melting point apparatus) at Baghdad University. U.V-Vis. Spectra were performed in a mixture of ethanol and acetone (2:1) on a (Shimadzu UV-1800) in the range (200-1100) nm at Baghdad University. IR-Spectra were recorded on a (Shimadzu FTIR- 8400s) in the range (400-4000)cm-1 using KBr disk, and ( 250- 4000) cm-1 using CsI disk at Baghdad University . The 1HNMR spectra were gained on the (Advance III 400 Bruker 400 MHZ) using DMSO as solvent at Iran / Isfahan University. The element analysis (C.H.N.S) was gained on a (Euro EA 3000) at Ibn Al- Haitham, Baghdad University. Thermal analyses (TG-DTG) were gained on a (Shimadzu 60-H Thermo Gravimetric Analyzer) at college of Education for Pure Science Ibn Al- Haitham, Baghdad University. Atomic absorption spectroscopy was gained on a(GBC 933 plus Absorption Spectrophotometer) at Bagdad University. Molar conductivity measurements (at conc. 10-3M) in DMSO were carried out by using Hunts capacitors Trade Mark British at Bagdad University. Magnetic susceptibility were gained on the Auto Magnetic Susceptibility Balance Model Sherwood Scientific) at Al-Mustansiriyah University . 211 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 Synthesis of Schiff base ligand [benzyl(2-hydroxy-1-naphthyldiene) hydrazine carbodithioate] A solution of (0.99gm, 0.005 mole from benzyl hydrazine carbodithioate (SBDTC) in (35ml) of hot ethanol (99.9%) was added to solution of 2-hydroxy-1-naphthaldehyde (0.86gm ,0.005 mole) in (35ml) of hot ethanol (99.9 %).The mixture was heated with stirring (reflux 6h), then the mixture was cooled in IC-bath to complete the recrystallization. The yellow product was washed in cold ethanol and recrystallized and dried overnight in vacuum desiccator that contains silica gel (yield 70%, m.p. 204-206°C) as shown in Scheme(1)[9]. Scheme(1) Synthesis of complexes The mole ratio of synthesis complexes was (1:2)(M:L). Schiff base L (0.176 gm ,0.0005 mole) was dissolved in mixture of acetone and absolute ethanol (20 ml of ethanol + 10 ml of acetone) and heated at 70 0C with stirring until became clear solution. A half mole of metal salts [as acetate in cobalt(II)( 0.0622gm),zinc(II)(0.0548gm), and cadmium(II)(0.0665gm), as chloride in nickel (II)(0.059gm) and copper(II)(0.0606gm)] was dissolved in absolute ethanol (10ml) and heated. Both solutions were mixed together and heated with stirring (reflux 10 h). Then the mixture is allowed to cool and the precipitate formed filtered off. Results and discussion The Schiff base ligand was prepared by the condensation reaction. The element microanalysis data of the prepared (L) and its complexes with [Co(II), Ni(II), Cu(II), Zn(II), and Cd(II) ] ions are in good convention with the calculated results from expected formula of each synthesized compounds as listed in table(1). Thermal analysis of L and its metal complexes The first stage of mass-lose is resulted in the temperature ranges (140-430),(180- 455),(160-290), (165-315),(80-210), and (180-310) oC were defined for the ligand (L) and its complexes (C1,C2,C3,C4, and C5) respectively. As evidenced from calculated and observed mass-loss, where, the first stage of mass-loss to confirm the existing of water hydration and solvent molecules. The final stage of mass-loss in the thermal decomposition of some complexes gave oxides or sulfide as final residue depending on the altimetry between the metal and binding atom of the ligand. This refers to the stability of these oxides or sulfides within the decimate temperatures range. The ligand and its complexes are stable at room temperature. The thermal analyses data of ligand and its complexes were listed in the table (2). The Thermograph of the ligand(L) and its Co-complex(C1) are shown in the figures(1 and 2). 212 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 Spectroscopic Characterization FT-IR Spectra The FT-IR spectra of synthesized ligand and its synthesized complexes were recorded in (KBr) and (CsI) disk . The IR spectrum of ligand (L) was showed a sharp absorption band at (1622.02 cm-1) which attributed to stretching vibration of υ(C=N) which was shifted to (1616.24, , 1616.24, 1616.24, 1620.21.and 1618.17cm-1) in the (C1-C5) respectively[10,11]. The weak band appeared at (1083.92cm-1) is assigned to vibration of υ (C=S)[12,13]. IR spectra of complexes show no more v(N-H) peak but do no exhibit a v(C=S) band since the thiones groups was relatively unstable in the monomeric forms and have a tendency to change into more stable thiol form by enethiolization process[14] .However they show v(C-S) band at around (975.91-1000.00)cm-1. These indicate that the complexation occurred between Schiff base and metal ion in the solid state, the ligand remains in the thione form. The sharp and strong band appeared at (1319.22cm-1) which is attributed to vibration of υ (C-N) of the ligand which was shifted to (1336.58 cm-1with shoulder in C1, 1338.51 cm-1 and became weak in C2, 1336.56 cm-1 in C3, 1330.88 cm-1in C4, and 1325.01 cm-1 in C5) [15]. The weak band appeared at (3028.03cm-1) was attributed to vibration of υ (NH) in the ligand [16], while absorption bands appeared at (528.46-553.51cm-1) were attributed to υ (M-N) for C1-C5 respectively[6,17].The absorption bands appeared at (374-383cm-1) were attributed to stretching vibrations of υ (M-S) for C1-C5 respectively[18,19]. The absorption bands appeared at (450- 478cm-1) were attributed to stretching vibrations of υ (M-O) for C1-C5 respectively [1]. While the weak absorption bands appeared at (3409.91-3446.56 cm-1) were assigned to υ(H2O) , υ (OH) [5,20]. The IR spectra of ligand and its Co-complex (C1) are shown in the figures(3and 4) and the data listed in the table(3). Molar Conductance The molar conductance of all synthesized complexes were measured in DMSO at room temperature. The values obtained lie in the range (3.3-24.0 S.cm2.mol-1), these indicate that all the synthesized complexes are non-electrolyte. The data of molar conductance were listed in the table(4). Magnetic Susceptibility According to the magnetic moment values, all synthesized complexes are paramagnetic except complexes (C4 and C5) are diamagnetic because the Zinc and Cadmium ions have filled d-orbital. The data of magnetic susceptibilities were listed in the table(4). Electronic Spectra The UV-Vis. Spectra of the ligand and its metal complexes were established in mixed of ethanol and acetone (2:1) at (10-4M) at room temperature in the region (200-1100)nm. The ligand showed bands at (265,335) nm assign to ( π→ π* and n→π*) transitions , which are shifted to [(263,311), (291, 326), (273, 327), (266, 334), and (320)] nm in C1-C5 respectively[16,22]. In addition the ligand spectrum showed three high intensity bands appeared in the near Visible region at (381,400,and 475) nm were assigned to intra-ligand charge transfer (ILCT), which are shifted to [(411,434,464), (406,430), (418), (415), (410)] nm in the(C1-C5) respectively [21,23]. While C1 appeared bands at (709, 787, 806) nm, C2 appeared three bands at (544, 592,and 649) nm, and C3 appeared band at(680)nm and these bands were attributed to d-d transitions[17,18,22]. There is no d-d transition in C4, and C5 213 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 because of fill d-orbital in the Zn and Cd ions. The electronic spectra of the ligand and its Co- complex (C1) were shown in the figures (5 and 6) and their data were listed in table(4). The NMR Spectra 1HNMR Spectra The 1HNMR Spectra for ligand and its (Zn(II)-L) (C4) complex were registered in DMSO as solvent. The free ligand showed multiple peaks from δ(7.22- 8.07ppm) refer to aromatic ring which are shifted to δ (6.96-8.07ppm) in the C4 [17,24,25]. The peak appeared at δ(9.2ppm) referred to the proton of azomethine group (CH=N) in the ligand that was shifted to δ( 9.50 ppm) in the C4 complex[21,25]. The peak appeared at δ (4.60ppm) was attributed to chemical shift of S-CH2 proton for ligand and shifted to δ(4.41 ppm) in the C4 complex [4,16].The peak appearance of a signal at δ (11.08 ppm) attributed to OH- aromatic for ligand that sifted to δ (10.00 ppm) in the C4complex[14, 25]. The peak appeared at δ (13.50 ppm) was attributed to NH group for ligand [4,26,27]. The 1HNMR of complexes show no more v(N-H) peak but do no exhibit a δ (C=S) band since the thiones groups was relatively unstable in the monomeric forms and have a tendency to change into more stable thiol form by enethiolization process[14]. The weak peak appeared at δ (2.09 ppm) and sharp peak appeared at δ (1.91ppm ) refer to CH3 of ethanol in ligand and its Zn-complex, and the peak appeared at δ(3.42-3.6) ppm refer to protons of H2O of moisture for DMSO in the ligand and refer to water molecule in the Zn- complex, the peak appeared at δ(2.51-2.68)ppm referred to the solvent [28,29] . The 1HNMR spectrum of (L) and its Zn-complex (C4) are shown in the Figures (7 and 8) and listed in the table (5). 13CNMR Spectra In the free ligand, the aromatic carbons appeared in the range δ(109.13- 136.90 ppm) which were shifted to δ(106.96-138.65ppm) in the C4 [30,31]. The peak appeared at δ (158.27ppm) referred to the C-OH for naphthalene ring for ligand which was shifted to δ (162.50ppm) in the C4, the azomethine group appeared a peak at δ(146.09 ppm) in the ligand which was shifted to δ(154.30ppm) in the C4 [4,16]. The peak appeared at δ(194.42ppm) in the ligand which referred to δ(C=S). The peak appeared at δ(172.15ppm)which was assigned to δ(C-S) in the C4 [4,30].The methyl carbons of the ligand appeared at δ(37.45ppm), which was shifted to δ (34.18 ppm) in the C4 [4].The peak appeared at (39.23-40.08 ppm ) was corresponded to the solvent peak (DMSO). The 13CNMR spectra for (L) and its Zn-complex (C4) were shown in the Figures (9 and 10) and listed in the table (6). According to the spectral data and measurements mentioned above of the synthesized complexes, the suggested structures of these complexes (C1,C2,C4 and C5) were concluded as octahedral geometry except copper-complex(C3) was appeared as a distorted octahedral as shown in figures(11-15). Conclusion The Schiff base (L) was found to be linked with [Co(II), Ni(II), Cu(II), Zn(II), and Cd(II)] ions through nitrogen atom of azomethane group , sulfur atom of thiocarbonyl, and oxygen atom of hydroxyl group. The chemical structure for the ligand and its complexes have been studied by different physiochemical techniques FTIR, NMR, UV-Vis spectroscopies, thermal analysis ,atomic absorption, conductivity measurements, magnetic Susceptibilities and element analysis were gave a results corresponding to mole ratio of (2:1) and the structures of the 214 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. 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(2010) “Solution-Phase Synthesis of a Combinatorial N,N′-Disubstituted Thiourea Library: Complexation, Characterization and Biological Studies”, Thesis, 231. 216 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 27. Fikriye, T. E.; Ulvi, A. and Nebahat, D. (2011) ”Synthesis and characterization of new thiourea derivatives substituted 1,10phenanthroline and crown ether”,Main Group Chemistry, (10), 17-23. 28. Surya, G. K. P.;Tisa, E. T.; Inessa, B. and Arjun, P. (2008) “Efficient green synthesis of α- aminonitriles, precursors of α-amino acids”, Royal Society of Chemistry, (10), 1105-1110. 29. Reda, A.A. A. and Abdel-Nasser, M. A. A. (2013) “Synthesis, Spectroscopic Characterization and Potentiometric Studies of a Tetradentate [N2O2] Schiff Base, N,N'-bis(2- hydroxybenzylidene)-1,1-diaminoethane and Its Co(II),Ni(II),Cu(II) and Zn(II) Complexes”, Int. J. Electrochem. Sci., (8) , 8686 – 8699. 30. Tarjeet ,S.; Ram, L. and Girija, .S. S. (2013), “Chemoselective N-benzoylation of aminophenols employing benzoylisothiocyanates” , Arabian Journal of Chemistry, 1-4. 31. Jaigeeth, D. and Prashant, S. P. (2010) “Biodegradation of phenanthrene by Alcaligenes sp. Strain PPH: partial puri¢cationand characterization of1-hydroxy-2-naphthoic acid hydroxylase”, Fems Microbiol Lett , (311), 93–101. Table (1): Physical properties and analytical data of ligand and its metal complexes. Sym. Color Decom. Temp. (m.p.)oC %Yield % Element Analysis Found (Cal.) % Metal Found (Cal.) %C %H %N %S L yellow 204-206 70 63.98 (63.33) 4.79 (5.52) 7.76 7.03 16.80 16.08 - C1 brown 186 68 59.43 (59.02) 4.41 (4.28) 6.88 (7.06) 13.29 (16.14) 7.15 (7.42) C2 brown >260 66 59.48 (58.84) 4.03 (4.53) 6.76 (6.86) 13.93 (15.69) 7.31 (7.19) C3 green 172 70 57.77 (57.71) 3.96 (4.80) 5.64 (6.56) 14.34 (15.01) 7.44 (7.45) C4 golden yellow 230 64 57.48 (57.74) 4.81 (4.57) 5.75 (6.73) 14.89 (15.37) 7.35 (7.86) C5 yellow 240 68 52.74 (53.19) 3.58 (4.43) 5.81 (6.20) 11.93 (14.18) 12.00 (12.45) 217 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 Table (2):The thermal analysis data (TG and DTG) of ligand and its metals complexes. Comp. Step Temp.range of decom- position at TG oC Peak temp. at DTG oC Suggested formula of loss % Mass loss Found Cal. L 1 140-430 240 EtOH, C6H6CH2 C10H6(OH)CH 73.70 73.62 2 430-595 540 CNHN 9.38 10.30 3 > 595 - S2 16.91 16.08 C1 1 180-455 234.8 0.5 EtOH, 0.5H2O, C10H6, C6H5CH2, C6H5 41.67 41.11 2 455-592 499.7 C10H6CHNNCSS,H HCNN 35.69 36.07 3 >592 OH, CH2SCS, CoO 22.63 22.94 C2 1 160-290 220 EtOH, 0.5H2O, C10H6OH 24.55 24.15 2 290- 322 312 C10H5CH2S 14.31 15.07 3 322-455 372 C6H5CH2 11.53 11.15 4 455-595 518 C6H5CH(OH)CHN, NCS 28.23 27.83 5 >595 - CHNNCS, NiS 21.42 21.53 C3 1 165-315 240 1.5EtOH,H2O 2C10H6CH 42.18 42.82 2 315- 395 355 C6H5CH2 10.11 10.67 3 395-595 495 C6H5CH2SCSNN, S, C,H 28.54 28.15 4 >595 NNS, OH ,CuO 19.19 18.36 C4 1 80-210 108 EtOH , H2O C3H3 11.63 12.39 2 210-405 323 C3H2 CH2 , 2C10H6 36.37 36.56 3 405-590 273 C10H7SCNNCH, SCNNCH 31.38 31.39 4 >592 183.3 OH,S2 ,ZnO 20.62 19.64 C5 1 180-310 273.4 EtOH, 2H2O, C6H5CH2 C10H6CH, 34.53 34.79 2 310-595 531.3 C6H5CH2, HCN,NHN 24.52 24.04 3 >595 CHNNCSS,NNCSS, OH,H, CdO 40.97 41.37 218 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 Table(3): Infrared spectral data of ligand and its complexes. Comp. υ C=N cm-1 υ C=S cm-1 υ C-N cm-1 υ C-S cm-1 υ H2O cm-1 υ M-N cm-1 υ M-S cm-1 υ M-O cm-1 L 1622.02 1083.92 1319.22 - 3420 _ _ - C1 1616.24 - 1336.56 987.49 3421.48 550.00 379.95 450.00 C2 1616.24 - 1338.51 1000.00 3446.56 553.53 383.81 470.60 C3 1616.02 - 1336.58 985.56 3421.48 540.03 379.95 478.31 C4 1620.21 - 1330.88 983.70 3433.29 536.17 374.16 464.81 C5 1618.17 - 1325.01 975.91 3409.91 528.46 360.60 462.88   Table (4): The electronic data and conductivity measurement of ligand and its complexes. Comp Wave length λ(nm) Wave no. ῡ (cm -1 ) Assignment Molar. cond. (S. cm 2 mol-1) μeff (B.M) Suggested Geometry L 265 335 381 400 475 37736 29851 21186 25000 26247 π→ π* n→π* IC.T IC.T IC.T - - - C1 263 311 411 434 464 709 787 806 38023 32154 24331 23041 21552 14104 12706 12406 π→ π* n→π* C.T. L→M C.T. L→M C.T. L→M 4T1g(F)→ 4T1g(P) 4T1g(F)→4A2g(F) 4T1g(F)→4T2g(F) 13.0 4.5 Octahedral C2 291 326 406 430 544 592 649 24691 23256 24691 23256 18382 16891 15408 π→ π* n→ π* C.T. L→M C.T. L→M 3A2g(F)→3T1g(P) 3A2g(F)→3T1g (F) 3A2g(F)→3T2g (F) 9.5 2.5 Octahedral C3 234 249 273 327 418 680 42735 40161 36630 30581 23923 14706 π→ π* π→ π* π→ π* n→ π* C.T. L→M 2Eg→2T2g 24.0 1 distorted octahedral C4 266 334 415 37594 29940 24096 π→ π* n → π* C.T. L→M 5.0 Diamagnetic octahedral C5 320 410 31250 24390 n → π* C.T. L→M 3.3 Diamagnetic octahedral 219 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 Table (5): The 1HNMR spectral data of ligand and its complexes. Assignment L Zn(L)2 Ar-H δ(7.22- 8.07ppm) δ (6.96-8.07 ppm) CH=N δ(9.20 ppm) δ(9.50ppm) S-CH2 δ(4.60ppm) δ(4.41ppm) Ar-OH δ(11.08ppm) δ(10.00ppm) CS NH δ(13.50ppm) - CH3 δ(2.03ppm) δ(1.89ppm) Table (6): The 13CNMR spectral data of ligand and its complexes. Assignments L Zn(L)2 Ar-C δ(109.13- 136.90 ppm) δ (106.96-138.65 ppm) CH=N δ(146.09 ppm) δ(154.3ppm) S-CH2 δ(37.45ppm) δ(34.18ppm) C-OH δ(158.27ppm) δ(162.50ppm) CS δ(194.42ppm) δ(172.15ppm) CH3 δ (37.45 ppm) δ (34.18 ppm) Figure (1): Thermograph of L. 220 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 Figure (2): Thermograph of C1. Figure (3): The FTIR spectrum of L. 221 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 Figure (4): The FTIR spectrum of C1. Figure (5): The electronic spectrum for L. 222 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 Figure (6): The electronic spectrum for C1. Figure (7): The 1HNMR spectrum of L. 223 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 Figure (8): The 1HNMR spectrum of C4. Figure (9): The 13 CNMR spectrum of L. Figure (10): The 13 CNMR spectrum of C4. 224 | Chemistry 2016) عام 1العدد ( 29لمجلد ا مجلة إبن الهيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 Figure(11): The structure of [Co(L1)2](0.5H2O) Figure(12): The structure of [Ni(L1)2] (0.5H2O ) (0.5 EtOH). (EtOH). Figure (13): The structure of [Cu(L1)2](H2O) Figure(14): The structure of [Zn(L1)2] (H2O) (1.5EtOH). (EtOH). Figure (15): The structure of [Cd(L1)2](2H2O) (EtOH). 225 | Chemistry 2016) عام 1العدد ( 29مجلة إبن الهيثم للعلوم الصرفة و التطبيقية المجلد Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 29 (1) 2016 كاربوداي نفثاليدين ) هيدرازين -1-هيدروكسي -2بنزايل (تحضير وتشخيص مع األيونات الفلزية هثايوات ومعقدات [Co(II), Ni(II), Cu(II), Zn(II), and Cd(II)] باسم أبراهيم العبدلي نور كاظم احمد بغداد قسم الكيمياء / كلية العلوم/ جامعة 2015تشرين األول//12،قبل في: 2015أيلول//17استلم في: الخالصة قاعدة شف مع ليكاند Co(II), Ni(II), Cu(II), Zn(II), and Cd(II)] [أليونات الفلزية تحضير معقدات لتم نفثالديهايد -1- هيدروكسي-2والمشتق من تفاعل ثايوات ]نفثاليدين) هيدرازين كاربوداي -1- هيدروكسي-2بنزايل ([جديدة بية للمعقدات المحضرة وفقا للتحليل الدقيق للعناصر , التحليل شخصت الصيغة التركيبنزايل هيدرازين كاربوداي ثايوات. و , قياسات التوصيلية, الحساسية CNMR13 ,HNMR1المرئية ,-الحراري , االشعة تحت الحمراء, االشعة فوق البنفسجية السطوح بأستثناء ثماني أذ أظهرت هذه القياسات بأن المعقدات المحضرة ذات شكل ,المغناطيسية و االمتصاص الذري الليكاند ) ويتناسق 1:2هي ( (M:L) أن النسبة بين الليكاند وااليون الفلزي.و معقد النحاس ذي شكل ثماني السطوح المشوه ذرة النتروجين لاليزوميثين وذرة الكبريت للثايوكاربون وذرة االوكسجين السن مع االيون الفلزي من خالل ثالثيبشكل لمجموعة الهيدروكسيل. .: ليكند قاعدة شفالكلمات المفتاحية