حتضري وتشخيص عدد من معقدات ايونات

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1 حتضري وتشخيص عدد من معقدات ايونات Mn (II), Co (II), Ni (II), Cu (II), Hg (II) مع مزيج من ليكاندات السكارين و حامض الباربيتيوريك و الثايوباربيتيوريك Mn (II), Co (II), Ni (II), Cu (II), Hg (II) :: C.H.N.S H.NMR M(BA) (sac)(h 2 O) 4 M(TBA) (sac)(h 2 O) 4 Cl Cl Mn (II), Co (II), Ni (II), Cu (II) M= BA = Barbituric acid. TBA = Thiobarbituric acid

2 sac= Saccharine. Hg (II) Hg(BA)(sac) Cl Hg(TBA)(sac) Cl Fahlberg, Saccharin 0 0 (Hsac;,-dioxo-,2-benzothiazole--one;O-benzoicSulfimide) C 7 H 5 NSO O-toluenesulfonamide Fahlberg, Remsen

3 PKa= US National Toxicology Program

4 7 C=O S=O N-H 8 Barbituric acide (9) (BA) 2 0 C 4 H 4 N 2 O 864 Barbitursaure 859 kakulus diimide

5 Thio barbituric acide (TBA) 0 TBA C TBA TBA HCV C, malondi aldehyde BA 2 SDI Aldrich Fluka BDH Melting point Elemental Analyzer Apparatus model

6 Molar 7 SHIMADZO JENWEAY DMSO Conductivity meter PCM 5 Spectrophoto meter KBR Cintra 5 V. V Visible Souble Deam speatro meter Brucker BM Bruker 7 MHZ avance instrument M(BA)(sac) (H 2 O) 4 M = Mn, Co, Ni, Cu, Hg BA = Barbituric acid Cl 0 2 Mn(BA)(sac) (H 2 O) 4 Cl MnCl 2. 4H 2 O Co(BA)(sac) (H 2 O) 4 Cl

7 HgCl CoCl 2. 6H 2 O 7677 Ni(BA)(sac) (H 2 O) 4 Cl NiCl 2. 6H 2 O 7677 Cu(BA)(sac) (H 2 O) 4 Cl CuCl 2. 2H 2 O 7677 Hg(BA)(sac) Cl M(TBA)(sac) (H 2 O) 4 M = Mn, Co, Ni, Cu, Hg TBA = Thio Barbituric acid Cl 2 2 Mn(TBA)(sac) (H 2 O) 4 Cl MnCl 2. 4H 2 O Co(TBA)(sac) (H 2 O) 4 Cl 8 CoCl 2. 6H 2 O

8 Ni(TBA)(sac) (H 2 O) 4 8 NiCl 2. 6H 2 O Cu(TBA)(sac) (H 2 O) 4 8 CuCl 2. 2H 2 O Hg(TBA)(sac) Cl HgCl 2 Cl Cl Micro Elemental analysis CHNS 0 M.P No. Molecular formula Color Yield% Or Decompo sition [ ]Cl Element & Metal analyses found. / (calc.)% C H N S (28.0).4 (.4) 8.89 (8.6) 6.78 (6.85) 2 [ ]Cl [ ]Cl (27.62).8 (.) 8.82 (8.8) 6.7 (6.80) 4 [ ]Cl [ ]Cl (24.2).48 (.5) 7.69 (7.67) 5.87 (5.87) 6 [ ] Cl [ ] Cl (26.62) (.2) (8.59) (.0 ) 8 [ ] Cl (26.8).27 (.2) 8.5 (8.60) 9 [ ] Cl [ ] Cl (25.0) (.50) (7.99) Molar Conductivity Measurement.02 (.0 ) 6.05 (5.98) 2 25) (0 - M)

9 [Hg(BA)(sac)] Cl,[M(TBA)(sac)(H 2 O) 4 ] Cl NO. : 2 5 Complex No. ( (0 - M) [M(BA)(sac)(H 2 O) 4 ] Cl [Hg(TBA)(sac)] Cl ) DMSO (0 - M) DMSO [Mn(BA)(sac)(H 2 O) 4 ] Cl 40 2 [Co(BA)(sac)(H 2 O) 4 ] Cl 5 [Ni(BA)(sac)(H 2 O) 4 ] Cl 68 4 [Cu(BA)(sac)(H 2 O) 4 ] Cl 50 5 [Hg(BA)(sac)] Cl 66 6 [Mn(TBA)(sac)(H 2 O) 4 ] Cl 4 7 [Co(TBA)(sac)(H 2 O) 4 ] Cl 55 8 [Ni(TBA)(sac)(H 2 O) 4 ] Cl 4 9 [Cu(TBA)(sac)(H 2 O) 4 ] Cl 69 0 [Hg(TBA)(sac)] Cl 54 Magnetic Measurements 5.69,6.0 B.M 7 (2), (4,) (.97,.9 B.M) (II) (.0,2.89 B.M) (II) (II) (II) (II) (.69,2.06 B.M

10 No. ( eff ) ( A ) Complex (Gram Susceptibility) χ g 0-6 c. g. s. u χ M 0-6 c. g. s. u Diamagne. correction 0-6 c. g. s. u χ A 0-6 c. g. s. u (D) ( g ) μ eff B.M. [Mn(BA)(sac)(H2O)4] Cl Configuration 2 [Co(BA)(ac)(H2O)4] Cl [Ni(BA)(sac)(H2O)4] Cl Octahedral 4 [Cu(BA)(sac)(H2O)4] Cl [Hg(BA)(Sac)] Cl Diamag. Linear 6 [Mn(TBA)(sac)(H2O)4] Cl [Co(TBA)(sac)(H2O)4] Cl [Ni(TBA)(sac)(H2O)4] Cl Octahedral 9 [Cu(TBA)(sac)(H2O)4] Cl [Hg(TBA)(sac)] Cl Diamag. Linear 7 DMSO Electronic Spectra 7 4 M 0 6 S 6 A g 5 (II) (6) t 2 g 5 eg T g (F) 4 T g (F) 4 T g (F) 4 T 2 g (F) ( ) cm - 4 A 2 g (F) ( 2 ) cm - 4 T g (P) ( ) cm

11 (t 2 g 6 eg ) (II) 2 Eg (7,2) (II) (26067, (7600,7627cm - ),( 674, 5708 cm - ) 4 T g (F) 4 T 2 g (F), ( 4 T g(f) 4 T g(p) ( 4 T g(f) 4 (7) (II) 2 T 2 g cm - ) 4 A 2 g(f) NO. Complex Bands v cm - Assignment Suggested Geometry [Mn(BA)(sac)(H 2 O) 4 ] Cl Octahedral [Co(BA)(sac)(H 2 O) 4 ] Cl [Ni(BA)(sac)(H 2 O) 4 ] Cl [Cu(BA)(sac)(H 2 O) 4 ] Cl T g (F) 4 T 2 g (F) 4 T g (F) 4 A 2 g (F) 4 T g (F) 4 T g (P) A 2 g (F) T g (F) A 2 g (F) T g (P) C.T 2 Eg 2 T 2 g C.T Octahedral Octahedral Octahedral 5 [Hg(BA)(sac)] Cl Linear 6 [Mn(TBA)(sac)(H 2 O) 4 ] Cl Octahedral 7 [Co(TBA)(sac)(H 2 O) 4 ] Cl Octahedral 8 [Ni(TBA)(sac)(H 2 O) 4 ] Cl T g (F) 4 T 2 g (F) 4 T g (F) 4 A 2 g (F) 4 T g (F) 4 T g (P) A 2 g (F) T g (F) A 2 g (F) T g (P) C.T Octahedral Eg 2 T 9 [Cu(TBA)(sac)(H 2 O) 4 ] Cl 2 g Octahedral 2894 C.T 0 [Hg(TBA)(sac)] Cl Linear

12 [M(BA) (sac) (H 2 O)] Cl M= Mn (II), Co (II), Ni (II), Cu (II) BA= Barbituric acid. M-O M-N BA C=O 727 [Hg(BA) (sac)] Cl BA= Barbituric acid Hg-N C=O [ M (TBA) (sac) (H 2 O) 4 ] Cl M= Mn (II), Co (II), Ni(II), Cu(II) TBA= Thio barbituric acid M-S C=S 7 TBA

13 N-H TBA [ Hg (TBA) (sac) ] Cl TBA= Thiobarbituric acid 775 C=S 45 M-S 7 TBA 449 N-H 7 الجدول )5( يوضح جرددات حزم االشعة جحث الحمراء لليكاندات والمعقدات المحضرة ) - Cm ( No. of ligand and complexes (C-H) Saccharine (S02) (C=S) (M- (M- S) N) (M O (NH/NH2 Ar Alph V(C0) V(CNS) Sym Asym ) ) Nasac 099w 072w s S(6)s As(966)s 45 s 259 s BA TBA [ ] Cl 08 w 2924 s 672 s 9 s 76 m 26 w m 2 [ ] Cl 0 w 2960 w 65 s 4 m 20 m 256 w m 488 s 45 m [ ] Cl 27 w 29 w 68 m 52 s 66 m 2 7 w w 462 m 60 s 4 [ ] Cl 2998 m 295 m 67 s 7 m 59 w 259 m w 49 m 8 s 5 [ ] Cl 200 m 2978 w 7 s 54 s 80 m 270 m s - 60 m 6 [ ] Cl 02 w 2977 w 655 m 40 s 56 m 268 s 00 m 40 w 540 s - 42 s 7 [ ] Cl 000 w 2995 m 645 s 49 s 67 m 284 s 987 m 4 s 557 s - 44 s 8 [ ] Cl 004 w 2990 w 647 s 64 m 5 m 276 m 997 m 424 w 542 w m 9 [ ] Cl 47 w 2968 m 649 m 6 s 72 m 22 m 982 s Very Weak 582 s m 0 [ ] Cl 02 w 297 m 657 s 6 s 6 m 266 s 005 s 45 m 50 w s S = Strong, m = medium, W = Weak, Ar = Aromatic, Alph = Aliphatic (- ppm.4.2 ppm [Hg(TBA)(sac)] Cl (NH) 7-8 ppm 6 0 CH 2 -)

14 [Hg(TBA)(sac)] Cl 4 [Hg(BA)(sac)] Cl ppm.6 (- (NH).6 ppm 7-8 ppm 2 CH 2 -)

15 [Hg(BA)(sac)] Cl 5 [M (BA)(sac)(H 2 O) 4 ]Cl [M (BA)(sac)(H 2 O) 4 ]Cl, M= Mn +2, Co +2, Ni +2, Cu +2. [Complex -4] [Hg(BA)(sac)]Cl

16 [Hg(BA)(sac)] Cl Complex 5 [M(TBA)(sac)(H 2 O) 4 ]Cl [M(TBA)(sac)(H 2 O) 4 ]Cl, M= Mn +2, Co +2, Ni +2, Cu +2. [Complex 6-9] [Hg(TBA)(sac)]Cl

17 [Hg(TBA)(sac)]Cl Complex 0. I. Remsen, C, Fahlberg, Ber. Dtsch. Chem. Ges., 2, 469(879). 2. I. Remsen, C, Fahlberg, J. Am. Chem. Soc.,, 426( ).. E. J Baran and V.T. Yilmaz, Coord. Chem. Rev., 250,980(2006). 4. E. J. Baran. Quim. Nova., 28, 26(2005). 5. M. J. Price, G. C. Biava, L. B. Oser, E. E. Vogin, J. Steinfeld, L. H. Lwy, Science, 67, (970). 6. K. M. A. Malik, S. Z. Haider, M. A. Hossain, M. B. Hursthouse, Acta. Cryst., 40, 696(984). 7. C. A. McAuliffe and W. Leavason, " Phosphine Arsine and Stibine Complexes of Transition Elements" Elesevier Scientific Publishing Company, Nether Lands (979). 8. P. M. Bhatt, N. V. Ravindra, B. Banerjee, G. R. Desiraiu, Chem. Commun., 07 (2005). 9. A. A. Mustafa, M. Sc. thesis, Tikrit University, (205). 0. F. A. Cotton, G. Wilkinson,"Advanced Inorganic Chemistry",6 th ed,. John Wily and Sons, New York,76,(999).. R.K. Lonibala, T. R. Rao, R. K. Dvi, J. Chem, Sci.,8,27, (2006). 2. D. G. Holah and C. N. Murphy, Inorg. Nucl. Chem. Letters, 8, (972").. M. Nohoyama, K.Nonoyma, J Inorg. Nucl Chem.,4,2567(98). 4. R.K. Verma, B.K.Mishar, K.C.Satplathy,Asian.J Chem,. 2,65 (997). 5. N. G. Alobaidy, A. M. idtiawe, National journal of Chemistry, Volume, 2, - 2 (2006). 6. B. N. Figis "introduction to Ligand Field", Interscience, New York, 48-49, 258, 9 (967)

18 7. D. Nicholls. "the Chemistry of Iron, Coblt and Nickel" Pergamon press Oxford, 087, 088, , 09, 5 (975). 8. O. V. Quinzani, S.Tarulli, O. E.Piro, E. J. Baran, E. E.Castellano, Z. Naturforsh., B : Sci., 52, 8 (997) 9. N. A. Dayaaf, M. Sc. thesis, Tikrit university (202) R. M. Ramadan, S.M. EI- Medani, O.A. M. Ali and H. A. Mohmad. J.Coord. Chem.,57,pp.7 (2004). 22. G.L. Hiessler and D. A. Tarr," Inorganic Chemistry" rd ed,. Person Prentce, Hall, International edition, (2004). Abstract This thesis includes, preparation and diagnosis of new twenty-one complex Of ions Mn (II), Co (II), Ni (II), Cu (II), Hg (II) With a mixture of saccharin legends and Barbituric / Thiobarbituric acid. The work included interaction of elements ions above With a mixture of saccharin legends and Barbituric / Thiobarbituric acid with Mole fraction (: : ) (Metal : saccharin : Barbituric or Thiobarbituric acid ) complexes were Diagnosed that have been prepared by fusion degrees, the magnetic sensitivity, careful analysis of the elements (CHNS), molar Electrical conductivity techniques and and infrared spectrum, electronic spectrum and Nuclear Magnetic Resonance spectrum of the proton (H.NMR) techniques. and Through the results that were obtained chemical formulas were suggested for the first part complexes were as follows: - M(BA) (sac)(h 2 O) 4 Cl M(TBA) (sac)(h 2 O) 4 Cl Whereas Mn (II), Co (II), Ni (II), Cu (II) M= BA = Barbituric acid. TBA = Thiobarbituric acid. sac= Saccharine. And it had a octahedral geometric shape Where Saccharine was linked to the central metal by nitrogen atom And Barbituric acid was linked to the central metal by oxygen atom. And Thiobarbituric acid was linked to the central metal by sulfur atom. And complexes Hg (II) have chemical formulas Cl Hg(BA)(sac) Cl Hg(TBA)(sac) With linear geometric structure. Where Saccharine was linked to the central metal by nitrogen atom And Barbituric acid was linked to the central metal by oxygen atom. And Thiobarbituric acid was linked to the central metal by sulfur atom

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