Some mixed 1,3-dithia-2-arsacyclopentane derivatives with phosphorous based 1,1-dithiolato ligands of the types SCH2CH2SAsS(S)POGO {where G = -CH(Me)-CH(Me)- and -C(Me)(2)-C(Me)(2)-} and SCH2CH2SAsS(S)PX2 {where X = OPrn, OPri, OPh and Ph} have been synthesized by the reaction of 2-chloro-1,3-dithia-2-arsacyclopentane and ammonium/sodium salt of corresponding ligands in equimolar ratio in refluxing anhydrous benzene solution. These yellow crystalline solid/semi-solid derivatives have been characterized by elemental analysis (C, H, S and As), molecular weights, melting points as well as spectral [UV, IR and NMR (H-1, C-13 and P-31)] studies. Antibacterial and antifungal activities of free ligands and their arsenic(III) complexes have also been screened.
1,3-dithia-2-stannacyclopentane derivatives of diorganodithiophosphates of the, types SCH2CH2SSn[S2P(OR)(2)]Cl (I) and SCH2CH2SSn[S2P(OR)(2)](2) (II) [where R = Et, n-Pr, i-Pr, n-Bu, i-Bu and Ph] have been synthesized (in 78-95% yields) by the reaction of 2,2-dichloro-1,3-dithia-2-stannacyclopentane and sodium/ammonium salts of diorganodithiophosphates in 1:1 and 1:2 molar ratios respectively, in anhydrous benzene. All these newly synthesized complexes are insoluble in common organic solvents and are difficult to be analysed by conventional techniques. We have applied elemental analyses, IR and solid-state NMR (H-1, C-13 and P-31) techniques to obtain structural information of these complexes.
A brief account of the synthesis, spectroscopic characterization and the antimicrobial (bacterial and fungal) behaviour of bis (diorganodithiocarbamato)organodithiocarbonatobismuth(III) complexes is presented. The reaction of bis (diorganodithiocarbamato)bismuth(III) chloride with potassium organodithiocarbonate in equimolar ratio yielded the corresponding mixed derivatives of the type [R′ 2 NCS 2 ] 2 BiS 2 COR [where, R′ = CH 3 and C 2 H 5 ; R = Et, Pr n , Pr i , Bu n and Bu i ]. These have been characterized by molecular weight determinations, melting points (only solid complexes) and elemental (C, H, N, S and Bi) analysis as well as spectral IR and NMR [ 1 H and 13 C] studies. The antibacterial and antifungal activities of the free ligands and their bismuth complexes were found in vitro by the disc diffusion method. The complexes showed good antibacterial and antifungal effect on some selected bacterial and fungal strains. The antimicrobial activities of two standard antibiotics (Chloroamphenicol and Terbinafin) were also measured and compared with these complexes. Copyright © 2005 John Wiley & Sons, Ltd.
Mixed bis(N,N'-dialkyldithiocarbamato)arsenic(III) alkylenedithiophosphate complexes of the type (R2NCS2)(2)AsS(2)POGO [where R = Me and Et; G = -CH2C(CH3)(2)CH2-, -CH2C(C2HS5)(2)CH2-, -CH(CH3)CH(CH3)- and -C(CH3)(2)C(CH3)(2)-] have been synthesized and characterized by elemental (C, H, N, S and As) analysis, molecular weights, melting points as well as spectral [UV, IR and NMR (H-1, C-13 and P-31)] studies. The antibacterial and antifungal activities of the free ligands and their arsenic(III) complexes were found in vitro by the disc diffusion method. The complexes showed good antibacterial and antifungal effect to some selected bacterial and fungal strain. Two standard antibiotics (chloroamphenicol and terbinafin) were used for comparison with these complexes.
Some mixed 1,3-dithia-2-stibacyclopentane derivatives with phosphorus based dithiolato ligands of the types SCH2CH2SS¯bS(S)POGO¯ {where G = CH(Me)CH(Me) and C(Me)2C(Me)2} and SCH2CH2SS¯bS(S)P(OR)2 {where R = Prn, Bun and Ph} have been synthesized by the reaction of 2-chloro-1,3-dithia-2-stibacyclopentane and the ammonium/sodium salt of the corresponding phosphorus based ligands in an equimolar ratio in anhydrous benzene solution. These yellow crystalline solid/semi-solid derivatives have been characterized by elemental analysis (C, H, S and Sb), molecular weights, melting point as well as spectral [UV, IR and NMR (1H, 13C and 31P)] studies. Single crystal X-ray diffraction analyses of 1,3-dithia-2-stibacyclopentane 2,3-butylenedithiophosphate revealed a monodentate mode of bonding of the dithiophosphate ligand in the complex. The free ligands and their antimony(III) complexes have also been screened for their antibacterial and antifungal activities.
We report here on dialkyldithiocarbamates complexes of the type [C6H3(CH3)S2MS2CNR2] (M = As and Bi; R = CH3, C2H5 and CH2–CH2), prepared by the reaction of toluene-3,4-dithiolatoarsenic(III) and -bismuth(III) chlorides [C6H3(CH3)S2MCl] (M = As and Bi) with sodium/ammonium salts of dialkyldithiocarbamates [XS2CNR2] (X = Na and NH4; R = CH3, C2H5 and CH2–CH2). The new derivatives were characterized by melting point, elemental analysis (C, H, N, S and As/Bi) and spectroscopic studies (IR, 1H and 13C NMR). Single crystal X-ray diffraction analyses of toluene-3,4-dithiolatoarsenic(III) dimethyldithiocarbamate and toluene-3,4-dithiolatoarsenic(III) pyrrolidine-dithiocarbamate revealed a monodentate chelating mode of the dimethyl as well as the pyrrolidine-dithiocarbamate moieties in these complexes.
1,3-dithia-2-stannacyclopentane derivatives with dialkyldithiocarbamates of the types SCH(2)CH(2)SSn[S(2)CNR(2)]Cl (I) and SCH(2)CH(2)SSn[S(2)CNR(2)](2) (II) (where R = CH(3), C(2)H(5) and -CH(2)-CH(2)-) have been synthesized by the reaction of 2,2-dichloro-1,3-dithia-2-stannacyclopentane and sodium/ammonium salts of dialkyldithiocarbamates in 1:1 and 1:2 molar ratios, respectively, in anhydrous benzene. These newly synthesized derivatives have been characterized by elemental analyses (C, H, N, S and Sn), thermal [thermogravimetry (TG) and differential thermal analyses (DTA)] as well as spectral [UV, IR and multinuclear NMR ((1)H, (13)C and (119)Sn)] studies. The monodentate behaviour of the dialkyldithiocarbamate ligands was confirmed by IR and (119)Sn NMR spectral data and distorted tetrahedral structures have been suggested for both type (I) and (II) compounds. The free ligands and their tin complexes have also been screened for their antibacterial and antifungal activities. These results made it desirable to delineate a comparison between free ligands and their tin complexes. These exhibit higher antibacterial effect than some of the previously investigated antibiotics.
Some mixed sulfur ligand complexes of bismuth(III) have been synthesized by the reactions of bis(dialkyldithiocarbamato)bismuth(III) chloride with sodium/ammonium diorganodithiophosphates in equimolar ratio in anhydrous benzene there will be a yield of: bis(dialkyldithiocarbamato)diorganodithiophosphatobismuth(III) of the type [(R'2NCS2)(2)BiS2- P(OR)(2)], where R' = Me and Et and R = Et, n-Pr, i-Pr, n-Bu, i-Bu and Ph. These newly synthesized complexes have been characterized by elemental (C, H, N, S and Bi) analysis, molecular weight determination and spectral [UV, IR and NMR (H-1, C-13 and (31)p)] studies. The free ligand and its mixed metal complexes were tested in vitro against a number of microorganisms to assess their antimicrobial properties. The results are indeed positive. In addition to these studies, the complexes also show good antibacterial effect over some of the previously investigated antibiotics. Copyright (c) 2005 John Wiley & Sons, Ltd.
The reactions of bis(dialkyldithiocarbamato)arsenic(III)chloride with sodium salts of dialkyldithiophosphates in 1:1 molar ratio give the corresponding mixed derivatives of the type[R2NCS2](2)AsS2P(OR')(2) [where, R = CH3 and C2H5; R' = Et, Pr-n, Pr-i, Bu-n and Bu-i]. These derivatives are yellow crystalline solids or yellow viscous liquids. All these newly synthesized derivatives are soluble in common organic solvents such as benzene, chloroform, carbondisulphide, acetone, and dichloromethane. These derivatives have been characterized by melting points (only solid derivatives). elemental analysis (C, H, N, S, and As) as well as spectral IR, NMR [H-1, C-13, and P-31] studies. Based on. these studies tentative structures for thew derivatives have been proposed.
The reactions of [R2NCS2](2)AsCl with KS2COR' in 1:1 molar ratio at room temperature readily gave mixed derivatives of the type [R2NCS2](2)AsS2COR' [where, R = CH3 and C2H5; R' = Et, Pr-n, Pr-i, Bu-n and Bu-i]. These derivatives are yellow crystalline solids. All these newly synthesized derivatives are soluble in common organic solvents like benzene, chloroform, carbondisulphide, acetone and dichloromethane etc. These derivatives have been characterized by melting points, elemental analysis (C, H, N, S and As) as well as spectral IR, NMR [H-1 and C-13] studies. On the basis of these studies tentative structures for these derivatives have been proposed.
Some mixed toluene-3,4-dithiolatobismuth(III) alkyl dithiocarbonate derivatives of the type SC6II3(CH3)SBiS2COR (where R = Me, Et. n-Pr, i-Pr n-Bu, and i-Bu) have been synthesized by the reaction of the potassium salts of alkyl dithiocarbonates and toluene-3,4-dithiolatobismuth(ill) chloride in equimolar ratio in an anhydrous carbon disulfide/acetone mixture. These newly synthesized derivatives have been characterized by elemental analyses, melting point determinations, as well as IR and NMR spectral studies. On the basis of these studies, tentative structures for these derivatives have been proposed.
Some toluene-3,4-dithiolatobismuth(III) dialkyldithiophosphate derivatives of the type SC6H3(CH3)SBiS2P(OR)(2) [where R = Et, n-Pr, i-Pr, n-Bu and i-Bu] have been synthesised by the reactions of toluene-3,4-dithiolatobismuth(III) chloride with sodium salts of dialkyldithiophosphates in equimolar ratios in refluxing anhydrous acetone. These newly synthesised dark gray derivatives are soluble in common organic solvents like acetone, benzene, chloroform and dichloromethane. All these derivatives have been characterized by elemental analysis (C, H, S and Bi) melting points as well as IR and NMR (H-1, C-13 and P-31) spectral Studies. On the basis of above spectral data, the tentative structures for these compounds have been proposed.
Some toluene-3,4-dithiolatoarsenic(III) alkyldithiocarbonate derivatives of the type SC6H3(CH3)SAsS2COR [where, R = Et, n-Pr, i-Pr, n-Bu and i-Bu] have been synthesised by the reactions of toluene-3,4-dithiolatoarsenic(III) chloride with potassium salts of alkyldithiocarbonates in equimolar ratios in anhydrous benzene and carbondisulphide (1:1) mixture at room temperature. All these derivatives are soluble in common organic solvents like benzene, carbon disulfide, chloroform, acetone and DMSO. These newly synthesised derivatives have been characterized by elemental analysis (C,H, S and As) melting points as well as IR and NMR (H-1 and C-13) spectral studies. The structures of these compounds have been confirmed by their analytical and spectral data.