Tin(IV)and organotin(IV) derivatives of bis(pyrazolyl)acetate: synthesis, spectroscopic characterization and behaviour in solution. X-ray single crystal study of bis(pyrazol-1-yl)acetatotri-iodotin(IV) [SnI3(bdmpza)]

Synthesis and characterization of the first diorganotin(IV) complexes containing mixed arylazobenzoic acids and having skew trapezoidal bypiramidal geometry

Synthesis and characterization of diorganotin(IV) complexes ofN-(2-pyridylmethylene)arylamines and mutagenicity testingin vivo of Et2SnCl2�[L4=N-(2-pyridylmethylene)-4-toluidine]

Diorganotin(IV) dichloride complexes of the type R 2 SnCl 2 .L (R = methyl, ethyl, vinyl, t-butyl, n-butyl or phenyl; L=N-(2-pyridylmethylene)arylamine) have been synthesized and characterized on the basis of IR, NMR and 119 Sn Mossbauer studies. Investigation of the complexes indicated that N-(2-pyridylmethylene)arylamines form distorted trans-octahedral complexes with R 2 SnCl 2 similar to the well-known R 2 SnCl 2 .L. Cytogenetic toxicology testing has been performed for Et 2 SnCl 2 .L 4 [L 4 = N-(2-pyridylmethylene)-4-toluidine] in mouse bone-marrow cells in vivo since such testing is a regulatory requirement before new drugs are released. This tin compound induced delay in cell-cycle k…

Synthesis and spectroscopic studies (Mo¨ssbauer, IR and NMR) of [R2SnCl2bipym] (R = butyl or phenyl) and the crystal and molecular structure of [Ph2SnCl2bipym]

Abstract The complexes [R 2 SnCl 2 bipym] (R = phenyl or butyl, bipym = 2,2′,6,6′-bipyrimidine) were synthesized and studied in solution by 1 H- and 13 C-NMR spectroscopy and in the solid state by IR and Mo¨ssbauer spectroscopy. The latter was also performed in frozen ethanolic solution. The structure of the phenyl complex was determined by single crystal diffraction methods. The value obtained for the angle C-SN-C in the phenyl compound is 169.3(2)° (X-ray) and 151° (Mo¨ssbauer), but the assignment of an octahedral configuration by Mo¨ssbauer spectroscopy is consistent with the structure determined by diffraction. The butyl complex is also octahedral and the two techniques show better agre…

Spectroscopic and X-ray structural characterization of complexes of lead(II)

Synthesis and characterization of bis[dicarboxylatotetraorganodistannoxane] units involving 5-[(E)-2-(aryl)-1-diazenyl]-2-hydroxybenzoic acids: an investigation of structures by X-ray diffraction, NMR, electrospray ionisation MS and assessment of in vitro cytotoxicity.

Abstract Reactions of 5-[(E)-2-(aryl)-1-diazenyl]-2-hydroxybenzoic acids (LHH′, where the aryl group is an R-substituted phenyl ring such that for L1HH′: R = H; L2HH′: R = 2′-CH3; L3HH′: R = 3′-CH3; L4HH′: R = 4′-CH3; L5HH′: R = 4′-Cl; L6HH′: R = 4′-Br) with nBu2SnO in a 1:1 molar ratio yielded complexes of composition {[nBu2Sn(LH)]2O}2. The complexes have been characterized by 1H, 13C, 119Sn NMR, ESI-MS, IR and 119mSn Mossbauer spectroscopic techniques in combination with elemental analyses. The crystal structures of {[nBu2Sn(L1H)]2O}2 (1), {[nBu2Sn(L4H)]2O}2 (4), {[nBu2Sn(L5H)]2O}2 (5) and {[nBu2Sn(L6H)]2O}2 (6) were determined. The compounds are centrosymmetric tetranuclear bis(dicarboxy…

Investigations on organoantimony compounds XI. Triorganoantimony(V) compounds containing potentially tridentate ligands

Triorganoantimony(V) compounds of the types RSbVL, in which R = Me or Ph, and L represents a potentially tridentate dianionic Schiff base ligand of the ONO or SNO type, have been synthesized and investigated by spectroscopic (UV, IR, PMR) methods. Molecular weight determinations in benzene reveal the monomeric nature of these compounds. The free ligands, HL, used in this study are:,′-(methylidynenitrilo)diphenol (HSab), -(o-hydroxyphenyl)benzothiazoline (H-Sat), -(o_hydroxyanilino)crotonophenone (HBah), 4-(o-hydroxyphenylimino)--pentanone (HAah) and -acetonyl--methylbenzothiazoline (HAat). Both the UV and the IR data suggest hexacoordinate molecular structures for the complexes RSbL in whic…

Synthesis and characterization of triorganotin(IV) complexes of 5-[(E)-2-(aryl)-1-diazenyl]-2-hydroxybenzoic acids.

Abstract The triphenyltin and tri-n-butyltin complexes of some 5-[(E)-2-(aryl)-1-diazenyl]-2-hydroxybenzoic acids have been synthesized and characterized by 1H-, 13C-, 119Sn-NMR, IR and 119mSn Mossbauer spectroscopic techniques in combination with elemental analysis. The crystal structures of triphenyltin 5-[(E)-2-(aryl)-1-diazenyl]-2-hydroxybenzoates (aryl=phenyl, 2-methylphenyl, 3-methylphenyl and 4-methoxyphenyl) are reported. Both X-ray and 119Sn Mossbauer data indicate that the triphenyltin complexes adopt a monomeric distorted tetrahedral configuration with the carboxylate ligand coordinating in a monodentate mode. By contrast, 119Sn Mossbauer spectroscopy shows that each tributyltin …

Diphenyltin(IV) complexes of the 5-[(E)-2-(aryl)-1-diazenyl]quinolin-8-olates: Synthesis and multinuclear NMR, 119Sn Mössbauer, electrospray ionization MS, X-ray characterization and assessment of in vitro cytotoxicity

Abstract A series of cis-bis{5-[(E)-2-(aryl)-1-diazenyl]quinolinolato}diphenyltin(IV) complexes have been synthesized and characterized by 1H, 13C, 119Sn NMR, ESI-MS, IR and 119mSn Mossbauer spectroscopic techniques in combination with elemental analysis. The structures of a ligand L6H (i.e., 5-[(E)-2-(4-ethoxyphenyl)-1-diazenyl]quinolin-8-ol) and three diphenyltin(IV) complexes, viz., Ph2Sn(L1)2 · (CH3)2CO (1), Ph2Sn(L4)2 (4) and Ph2Sn(L5)2 (5) (L = 5-[(E)-2-(aryl)-1-diazenyl]quinolin-8-ol: aryl = phenyl – (L1H); 4′-methylphenyl – (L4H) and 4′-bromophenyl – (L5H)) were determined by single crystal X-ray diffraction. In general, the complexes were found to adopt a distorted cis-octahedral a…

Synthesis and characterization of the first diorganotin(IV) complexes containing mixed arylazobenzoic acids and having skew trapezoidal bipyramidal geometry

Abstract Three diorganotin(IV) complexes of the type, [R 2 Sn(L a H)(L b H)] (R =  n Bu or Me and, L a H and L b H are two different 5-[( E )-2-(aryl)-1-diazenyl]-2-hydroxybenzoate residues; a: aryl = 4′-Cl-(held constant) and b: aryl = 4′-Me or 4′-Br) have been prepared either by reacting n Bu 2 SnO, L a HH′ and L b HH′ (1:1:1) in anhydrous toluene or by reacting Me 2 SnCl 2 , L a HNa and L b HNa (1:1:1) in anhydrous methanol. The products were characterized by microanalysis, IR, NMR ( 1 H, 13 C, 119 Sn) and 119m Sn Mossbauer spectroscopy. A full characterization of the structures of the complexes [ n Bu 2 Sn(L a H)(L b H)] ( 1 and 2 ) and [Me 2 Sn(L a H)(L b H)] ( 3 ) in the solid state w…

Synthesis, characterization of diorganotin(IV) complexes of N-(2-hydroxyarylidene)aminoacetic acid and antitumour screening in vivo in ehrlich ascites carcinoma cells

Some new diorganotin(IV) complexes have been prepared by reacting potassium N-(2-hydroxyarylidene)aminoacetate with R2SnCl2(R = Me,nBu,Ph). The complexes have been characterized by 1H,13C,119Sn NMR, IR and 119mSn Mössbauer spectroscopic techniques in combination with elemental analysis. In the solid state, the complexes possess penta- and hexa-coordinated tin centres. The hexa-coordinated tin complexes were found to dissociate in solution, giving rise to penta-coordinated species as revealed by 119Sn NMR spectroscopy. Antitumour screening in vivo of the complexes L4snPh2,L4SnPh2· Ph3SnCl and L4SntBU2·t Bu2SnCl2 (L4 = N-(2-hydroxyacetophenone)aminoacetate) is also reported. Copyright © 2001 …

Synthesis, spectroscopic studies (Mössbauer and infrared), and the crystal and molecular structure of the organotin(IV)-pyrazine adducts [Sn(CH3)2Cl2]2pyz and [Sn(CH3)2Br2pyz]

Two adducts [Sn(CH 3 ) 2 Cl 2 ] 2 pyz ( Ia ) and Sn- (CH 3 ) 2 Br 2 pyz] ( Ib ) (pyz = pyrazine) have been synthesized and characterized in the solid state. Infrared and Mossbauer spectroscopies suggest a five- coordinated species for the Ia complex with an angular CSnC bond and a six-coordinated compound with a linear CSnC bond for the Ib complex. X-ray diffraction studies confirm a distorted trigonal bipyramidal geometry with N, Cl axial atoms and Cl and methyls in the equatorial plane for Ia where the Cl ax SnN bond angle is the lowest one reported to date and the Cl eq Sn bond distance the longest one with regard to similar complexes. This molecule has a short contact of 3.47 A b…

Complexes of organometallic compounds

Abstract The novel organobismuth(V) derivatives Ph 3 BiCl(Ox) and Ph 3 BiBr(Ox) (Ox − = 8-quinolinate) have been synthesized, and their configuration investigated in the solid state and in solution. The complexes are assumed to be octahedral in the solid, with Ox − acting as a chelating base and the halide atoms coordinating to bismuth. Tentative assignments of infrared bands in the 300–80 cm −1 region to BiHal and other skeletal modes are proposed. The main effect of solvents appears to be the weakening and breaking of BiN-bonds.

The synthesis and structural characterization of some triorganotin(IV) complexes of 2-{[(E)-1-(2-hydroxyaryl)alkylidene]amino}acetic acid. Crystal and molecular structures of Ph3Sn(2-OHC6H4C(H)NCH2COO) and Me3Sn(2-OHC6H4C(CH3)NCH2COO)

Abstract Triorganotin(IV) derivatives of 2-{[(E)-1-(2-hydroxyaryl)alkylidene]amino}acetic acid have been synthesized and characterized by 1H, 13C, 119Sn-NMR, 119Sn Mossbauer and IR spectroscopic techniques in combination with elemental analyses. The crystal structures of triphenyltin 2-{[(E)-1-(2-hydroxyphenyl)methylidene]amino}acetate and trimethyltin 2-{[(E)-1-(2-hydroxyphenyl)ethylidene]amino}acetate are reported. The X-ray structures reveal that the complexes adopt a polymeric trans-O2SnC3 trigonal bipyramidal configuration with the R groups in the equatorial positions and the axial locations occupied by a carboxylate oxygen from the ligand and the phenolic oxygen of the ligand on an ad…

Synthesis and characterization of trbenzyltin(IV) and dibenzyltin(IV) complexes of 2-((2Z)-3-hydroxy-1-methyl-2-butenylidene)amino)acetic acid: Crystal structure of tribenzyl(2-(2Z)-3-hydroxy-1-methyl-2-butenylidene)amino)acetato)tin(IV).

Reactions of equimolar quantities of potassium 2-{[(2Z)-3-hydroxy-1-methyl-2-butenylidene]amino}acetate, with R n SnX4−n (R: benzyl– and n=2 or 3) in methanol yielded products of compositions LHSn(PhCH2)3 and LSn(PhCH2)2, respectively. The complexes were characterized by microanalysis, IR, NMR (1H, 13C, 119Sn) and 119mSn Mossbauer spectroscopy. A full characterization of the structure of the complex, tribenzyl{2-{[(2Z)-3-hydroxy-1-methyl-2-butenylidene]amino}acetato}tin(IV), was carried out by single crystal X-ray crystallography. The compound exists as centrosymmetric dimers in which two ligand molecules bridge the two tin centres. Each of the tin atoms in the dimeric unit is five coordina…

Complexes of organometallic compounds. XLVI. Synthesis of adducts formed by organotin(IV) trichlorides with 1,2-bis(diphenylphosphino)ethane, and their characterization by mössbauer and infrared spectroscopy

Abstract Adducts between RSnCl 3 (R = Me, Bu n , Oct n , Ph) and 1,2-bisz(diphenylphosphino)ethane, DPE, have 1:1 composition. In Mossbauer spectroscopic experiences at variable absorber temperature the area under the resonant peaks, A, has been measured for RSnCl 3 ·DPE, R = Me, Ph; slopes plots of in A vs. T suggest strong coupling between Mossbauer atoms, which has been interpreted in terms of solid state polymeric structures, due to DPE acting as a bridging bis-monodentate ligand. Infrared data indicate the covalency of SnCl bonds. Three possible structural isomers of octahedral type are then proposed, one having trans -P 2 and two cis -P 2 atoms. A choice between these structures has …

The first authenticated example of triorganotin(IV) perchlorate complexes of some heterocyclic bases

Abstract A convenient method is reported for the synthesis of some novel complexes of composition (R 3 SnL 2 ) ClO 4 where L represents pyridine, γ-picoline, 2,2′-bipyridine and 1,10-phenanthroline; and R  n Bu or Ph. All of the new ionic complexes have been characterized by elemental analysis, molar conductance, infrared, multinuclear nuclear magnetic resonance ( 1 H, 13 C and 119 Sn) and 119 Sn Mossbauer spectroscopies. The complexes of composition (R 3 SnL 2 )ClO 4 exist both in solution and in the solid state with trans -trigonal bipyramidal structure where the R-groups occupy the equatorial positions while the ligands are in the axial position.

Di-n-octyltin(IV) complexes with 5-[(E)-2-(aryl)-1-diazenyl]-2-hydroxybenzoic acid: Syntheses and assessment of solid state structures by 119Sn Mössbauer and X-ray diffraction and further insight into the solution structures using electrospray ionization MS, 119Sn NMR and variable temperature NMR spectroscopy

Abstract Reactions of 5-[( E )-2-(aryl)-1-diazenyl]-2-hydroxybenzoic acids (LHH′, where the aryl group is an R-substituted phenyl ring such that for L 1 HH′: X = H; L 2 HH′: X=2′-OCH 3 ; L 3 HH′: X = 3′-CH 3 ; L 4 HH′: X = 4′-CH 3 ; L 5 HH′:X = 4′-Cl) with n Oct 2 SnO in 2:1 and 1:1 molar ratios have been investigated. Two types of complexes, n Oct 2 Sn(LH) 2 and {[ n Oct 2 Sn(LH)] 2 O} 2 , were isolated and they have been characterized by 1 H, 13 C, 119 Sn NMR, ESI-MS, IR and 119m Sn Mossbauer spectroscopic techniques in combination with elemental analyses. The crystal structures of n Oct 2 Sn(L 1 H) 2 ( 1 ), {[ n Oct 2 Sn(L 2 H)] 2 O} 2 ( 3 ) and {[ n Oct 2 Sn(L 3 H)] 2 O} 2 ( 4 ) were de…

119Sn Mössbauer spectroscopic studies of the products of the reaction of triorganotin(IV) derivatives with 6-thiopurine

Abstract A structural study of the products of the reaction of R 3 Sn IV derivatives (R = Me, Bu n , Ph) with 6-thiopurine, 6-TPH 2 , and its sodium salt, 6-TPHNa, has been undertaken using Mossbauer spectroscopy and the point-charge model rationalization of the Mossbauer parameter nuclear quadrupole splitting. The synthetic reactions have been carried out at ca . 0 °C, 20 °C and 50 °C. The Mossbauer spectra of the complexes AlK 3 Sn(6-TPH) are consistent with the occurrence of two distinct tin(IV) sites in samples prepared at the lower temperature, while one only site appears by increasing the temperature of the reaction. Two tin sites constantly occur in the products of the reactions invo…

Synthesis and characterization of triphenyltin(IV) 5-[(E)-2-(aryl)-1-diazenyl]-2-hydroxybenzoates. Crystal and molecular structures of Ph3Sn{O2CC6H3-p-OH[NN(C6H4-4-CH3)]} and the 2,2′-bipyridine adduct Ph3Sn{O2CC6H3-p-OH[NN(C6H4-2-CH3)]}OH2·C10H8N2

Abstract Triphenyltin 5-[(E)-2-(4-methylphenyl)-1-diazenyl]-2-hydroxybenzoate, Ph3SnL2H, has been prepared and characterized, its structure determined by X-ray crystallography, and the structure compared with those of its homologues. Two polymorphs were isolated from the same crystallization attempt. The reactivity of tetrahedral Ph3SnL1H (L1H = 5-[(E)-2-(2-methylphenyl)-1-diazenyl]-2-hydroxybenzoate) towards 2,2′-bipyridine (bipy) has been investigated to ascertain the ability of bipy to coordinate to the Sn-complex and the resultant changes in the molecular architecture. The crystal structure of the product revealed that the bipy moiety does not coordinate to the Sn atom, but forms a cycl…

Diphenyltiv(VI) complexes with substituted 5-azoxines: synthesis, structural characterization and assessment of in vitro cytotoxicity.

DIPHENYLTIN(IV)COMPLEXES OF THE 5-[(E)-2-(ARYL)-1-DIAZENYL]QUINOLIN-8-OLATES: SYNTHESIS AND MULTINUCLEAR NMR, 119SN MOSSBAUER, ELECTROSPRAY IONIZATION MS, X-RAY CHARACTERIZATION AND ASSESSMENT OF IN VITRO CYTOTOXICITY

Synthesis, spectroscopic (Mössbauer, IR and NMR) and X-ray structural studies of diorganotin complexes of 2,2′-bipyrimidine and further NMR studies of diorganotin-pyrazine and — 2,2′-azopyridine complexes

Abstract The ligand 2,2′-bipyrimidine (bipym) was reacted with diorganotins R 2 SnCl 2 (R = methyl, ethyl) and complexes of the types R 2 SnCl 2 bipym, R 2 SnCl 2 bipym · bipym and (R 2 SnCl 2 ) 2 bipym were synthesized and studied by 1 H and 13 C NMR spectroscopy in solution, and by IR and Mossbauer spectroscopy in the solid state and frozen solutions. The complexes Et 2 SnCl 2 bipym · bipym and (Et 2 SnCl 2 ) 2 bipym were characterized by X-ray diffraction methods. In both complexes the tin environment is octahedral with chloro atoms in a cis disposition, the ethyl groups in a trans disposition and two N atoms from the ligand bipym. the second complex is a centrosymmetric binuclear specie…

Itinerari archeologici della Sicilia nord-occidentale:Himera.Caratterizzazione di reperti ceramici provenienti dalla necropoli di Pestavecchia

Relationship between XPS core binding energies and atomic charge in adducts of SnIV derivatives with pyrazine, and comparison with mössbauer isomer shift data

Abstract Adducts Snhal·pyz (hal = Cl, Br, I; pyz = pyrazine), RnSnCl 4−n ·pyz (n = 1, R = Me, Bu n , Oct n , Ph; n = 2, R = Ph) and SnCl 4 ·(pyz) 2 have been investigated by X-ray photoelectron spectroscopy. Binding energy (b.e.) values are discussed in the light of structural characteristics of the adducts as well as of valence state electronegativities of atoms and groups bound to tin. Sn 3d 5 2 b.e.s, corrected for the Madelung potential at the metal atom, linearly correlate with both partial atomic charges on tin, accounting for relaxation upon ionization, and 119 Sn Mossbauer isomer shifts. The results are interpreted in terms of six-coordinated, octahedral type, configurations of the …

Itinerari archeologici della Sicilia occidentale: Himera. Studio di reperti ceramici

Arcaeological routes of northern Sicily: Himera characterization of ceramic findings from Pestavecchia necropolis

Synthesis, characterization and crystal structures of polymeric and dimeric triphenyltin(IV) complexes of 4-[((E)-1-{2-hydroxy-5-[(E)-2-(2-carboxyphenyl)-1-diazenyl]phenyl}methylidene)amino]aryls

Abstract The triphenyltin(IV) complexes of 4-[((E)-1-{2-hydroxy-5-[(E)-2-(2-carboxyphenyl)-1-diazenyl]phenyl}methylidene)amino]aryls (aryls = 4-CH3, 4-Br, 4-Cl, 4-OCH3) have been synthesized and characterized by 1H-, 13C-, 119Sn-NMR, ESI mass spectrometry, IR and 119mSn Mossbauer spectroscopic techniques in combination with elemental analysis. The crystal structures of a representative carboxylate ligand (aryl = 4-CH3) and three Sn complexes, viz., polymeric (Ph3Sn[O2CC6H4{N N(C6H3-4-OH(C(H) NC6H4X-4))}-o])n (X = Me (1) and Br (2)) and dimeric (Ph3Sn[O2CC6H4{N N(C6H3-4-OH(C(H) NC6H4X-4))}-o])2 (X = OMe (4)) complexes are reported. The coordination environment in each complex is trigonal bip…

Synthesis and chemico-physical characterization of tin(IV) complexes with some crown ethers

Abstract Some neutral adducts of diorganotin(IV) perchlorates and thiocyanates with three crown-ethers have been synthesised; they are of the type Me 2 SnX 2 L m · n H 2 O where m = 1 or 2, n = 2 or 4, X = ClO 4 or NCS, and L = 18-crown-6, 15-crown-5, and 12-crown-4. The values for m and n have been correlated with the coordinating ability of the two anions and with the steric hindrance by the crown ether molecules. From infrared and Mossbauer data, an octahedral coordination geometry is proposed for all the complexes. The Mossbauer parameters are discussed in terms of the electronegativity of the ligands on the tin(IV) center and of the distortions produced in the coordination polyhedra by…

Tin(IV) and organotin(IV) derivatives of bis(pyrazolyl)acetate: Synthesis, spectroscopic characterization and behaviour in solution.

Abstract Novel heteroscorpionate-containing tin and organotin(IV) complexes, [SnRnX3 − n(L)], R = Me, Bun, Ph, or cy; X = Cl, Br or I, n = 0, 1, 2 or 3; L = bis(pyrazol-1-yl)acetate (bpza) or bis(3,5-dimethylpyrazol-1-yl)acetate (bdmpza), have been synthesized and characterized by spectral (IR, 1H, 13C and 119Sn NMR, 119mSn Mossbauer) and analytical data. In [SnI3(bdmpza)], the ligand is fac-N,N′,O-tridentate, the three iodine atoms thus also fac about the six-coordinate tin(IV) atom. Neutral bpzaH reacts with BunSnCl3, PhSnCl3 and SnCl4 in Et2O in the absence of base, yielding 1:1 adducts [XSnCl3(bpzaH)] (X = R or Cl).

Precursors of aza-macrocycles: Characterization of substituted phenanthrolines and related bases. Crystal and molecular structure of dichloro-d i-n-butyl(2,2',6,6'-bipyrimidine)tin(IV)

The synthesis, characterization and 1~ NMR spectra of some substituted 1,lO-phenantrolines are described. These are precursors of azacyclophanes which are, along with their metal complexes, insoluble in polar solvents. It is suggested that the use of substituted 2,2’, 6,6’ -bipyrimidines as precursors would lead to soluble macrocycles. The crystal and molecular structure of dichloro-di-n-butyl(2,2’,6,6’-bipyr

Organotin(IV) Complexes of Aromatic Acid Hydrazides: Preparation and Spectroscopic Studies

Abstract The ability of aromatic acid hydrazides, RCONHNH, to act as bidentate chelating agents towards diorganotin(IV) dichlorides has been investigated. The structure of the complexes were deduced from IR, NMR and Mossbauer spectroscopic techniques in combination with analytical data. The R2SnCI2.L complexes have octahedral geometry where the tin atom is chelated with one ligand (via carbonyl oxygen and hydrazinic nitrogen atoms), two chlorine atoms are in equatorial positions while the R groups are in the axial positions.

Synthesis and characterization of some diorganotin(IV) complexes of Schiff bases derived from a non-protein amino acid. Crystal structures of {HO2CC6H4[NC(H)}{C(CH3)CH(CH3)-3-OH]-p} and its di-n-butyltin(IV) complex (nBu2Sn{O2CC6H4[NC(H)}{C(CH3)CH(CH3)-3-OH]-p}2)

Diorganotin(IV) complexes R2Sn(LH)2 (R = Me, nBu) and {[nBu2Sn(LH)]2O}2 (LH = 4-[(2Z)-(3-hydroxy-1-methyl-2-butenylidene)amino]benzoate and 4-[{(E)-1-(2-hydroxyphenyl)methylidene}mino]benzoate) have been reported. The complexes were characterized by elemental analysis, IR, NMR (1H, 13C, 119Sn) and 119mSn Mossbauer spectroscopy. Crystal structures of a ligand {HO2CC6H4[NC(H)}{C(CH3)CH(CH3)-3-OH]-p} and one of its di-n-butyltin(IV) complexes (nBu2Sn{O2CC6H4[NC(H)}{C(CH3)CH(CH3)-3-OH]-p}2) were determined. The spectroscopic data suggest that R2Sn(LH)2 complexes have skew-trapezoidal bipyramidal structure while {[nBu2Sn(LH)]2O}2 complexes adopt a dimeric tetraorganodistannoxane structure in the…

Complexes of Organometallic Compounds. XXVII. Studies on Diorganolead (IV) Moieties Six-coordinated by ONNO Tetradentate Ligands

New complexes R2PbL, where L2− are the dianions in the “planar” SCHIFF base form, of the tetradentate ONNO ligands α, α′ (ethylenedinitrilo)dicresol and 2,2′ bis-benzoxazoline, were synthesized. Their configuration was investigated at the solid state by infrared spectroscopy, and in solution phase mainly by electronic and PMR spectroscopy. An octahedral type structure with linear CPbC moieties, and the ONNO ligand atoms chelating PbIV in a square plane, was advanced. Darstellung neuer Komplexverbindungen: R2PbL (R = CH3, C2H5, C6H5; L−2 sind zweiwertige Anionen, in der „planaren” SCHIFFSCHEN Basen-Konfiguration, der vierzahnigen ONNO-Liganden Disalicylal-athylendiamin und Glyoxal-bis-[2-hyd…

XPS structural data and correlation with Mossbauer spectra for Tin-organic compounds: adducts of RnSnCl4-n with 1,2-bis(diphenylphosphino)ethane

Abstract Core level X-ray photoelectron spectra of 1:1 adducts of SnCl4 and RSnCl3 with DPE {[RnSnCl4−n} · DPE (n = 1, R = Me, Bun, Octn, Phn; n = 2, R = Ph; DPE = 1,2-bis(diphenylphosphino)ethane], have been measured in solid phase. The Sn3d 5 2 binding energies, corrected for the Madelung potential at the metal atom, are well correlated with both partial atomic charge on tin, accounting for relaxation upon ionization, and 119Sn Mossbauer isomer shifts. The results are discussed in terms of these molecular parameters.

Complexes of organometallic compounds. XLVIII. Mössbauer and other studies on pyrazine derivatives of tin(IV) compounds. A relationship between isomer shift and charge on tin

Abstract Adducts RSnCl 3 ·pyz (R = Me, Bu n , Oct n , Ph; pyz = pyrazine) have been synthesized and characterized in the solid state. It has been determined that RSnCl 3 ·pyz are polymeric compounds, where the ligand acts as bridging bis-monodentate and the tin atoms attain the coordination number six. This has been duduced from: i) temperature dependent Mossbauer spectroscopy; ii) the correlation between Mossbauer isomer shift, δ, and electrical charge on tin, Q Sn , concerning pyrazine adducts of RSnCl 3 and others; iii) an infrared study of the coordinated ligand in RSnCl 3 ·pyz. Other implications of the Mossbauer T dependent study ( e.g. , the decrease of the Debye temperature in RSnCl…

Synthesis, characterization, cytotoxic activity and crystal structures of tri- and di-organotin(IV) complexes constructed from the β-{[(E)-1-(2-hydroxyaryl)alkylidene]amino}propionate and β-{[(2Z)-(3-hydroxy-1-methyl-2-butenylidene)]amino}propionate skeletons

Abstract Reactions of potassium β-{[(E)-1-(2-hydroxyaryl)alkylidene]amino}propionates (L1HK-L3HK) and potassium β-{[(2Z)-(3-hydroxy-1-methyl-2- butenylidene)]amino}propionate (L4HK) with R3SnCl (R = Ph and nBu) and nBu2SnCl2 yielded complexes of composition Ph3SnL1H (1), Ph3SnL2H (2), Ph3SnL4H (3), nBu3SnL1H (4), and {[nBu2Sn(L2H)]2O}2 (5) and {[nBu2Sn(L3H)]2O}2 (6), respectively. These complexes have been characterized by 1H, 13C, 119Sn NMR, ESI-MS, IR and 119mSn Mossbauer spectroscopic techniques in combination with elemental analyses. The crystal structures of 1, 4, 5 and 6 were determined. In the solid state, compound 1 is a one-dimensional polymer built from SnPh3 moieties bridged by s…

Organotin(IV) complexes ofN-[(2Z)-3-hydroxy-1-methyl-2-butenylidene]glycine

Organotin(IV) derivatives of N-[(2Z)-3-hydroxy-1-methyl-2-butenylidene]glycine have been synthesized and characterized by 1H, 13C, 119Sn NMR, 119Sn Mossbauer, and IR spectroscopy along with elemental analyses. The di- and triorganotin(IV) complexes were readily obtained from the reactions of organotin halides and sodium/potassium N-[(2Z)-3-hydroxy-1-methyl-2-butenylidene]glycinate. The diorganotin compound reacted with Ph3SnCl in refluxing benzene to give the mixed organotin dinuclear complex of composition Ph2Sn(2-OC(CH3)-C(H)C(CH3)NCH2COO)·Ph3SnCl, which was characterized by single crystal X-ray structure determination. © 2003 Wiley Periodicals, Inc. Heteroatom Chem 14:149–154, 2003; Publ…

Complexes of Tin(II) with 4-acyl-5-pyrazolonates: synthesis, spectroscopic and X-ray structural characterization

Adducts of tin(IV) and organotin(IV) derivatives with 2,2′-azopyridine II. Crystal and molecular structure of SnMe2Br2AZP and further mössbauer and photoelectronic spectroscopic studies

Abstract A series of adducts of tin(IV) derivatives with 2,2′-azopyridine, AZP, has been studied by Mossbauer and X-ray photoelectronic spectroscopies and the crystal and molecular structure of SnMe2Br2- AZP has been determined. The linear correlation of the Mossbauer parameter isomer shift with partial atomic charge on tin suggests the occurrence of a single homologous series of isostructural adducts. The correlation of the Mossbauer parameter quadrupole splitting and C-Sn-C bond angle permits their calculation in SnMe2X2AZP adducts (X = Cl, Br). The N1s binding energies, obtained by XPS data, pointed out two slightly different values for both pyridinic and azo-group nitrogens. The crystal…

Characterization of some triphenyltin(IV) complexes of 5-(arylazo)salicylaldehyde ligands using IR, 1H, 13C, 119Sn NMR and 119Sn Mössbauer spectroscopy

Abstract Coordination complexes of 5-(arylazo)salicylaldehyde with triphenyltin chloride have been prepared and subjected to IR, multinuclear NMR (1H, 13C, 119Sn) and 119Sn Mossbauer spectroscopy. 5-(Arylazo)salicylaldehyde forms two types of complexes viz. triorganotin adducts and phenoxides. In the adducts, the protonated ligand coordinates through the aldehydic oxygen atom while in phenoxides, the coordination occurs via the phenolic oxygen atom and the oxygen atom of the aldehydic group. The spectroscopic data suggest that both types of complexes adopt a cis-trigonal bipyramidal geometry around tin.

Synthesis and characterization of thiphenyltin(IV) 5[(E)-2-(aryl)-1-diazenyl]-2-hydroxybenzoates. Crystal and molecular structures of Ph3Sn[O2CC6H3-p-OH(C6H4-4-CH3]and the 2,2'-bipyridine adduct Ph3Sn[O2CC6H3-p-OH(N=N(C6H4-2-CH3)]OH2.C10H8N2

Tin(IV) and organotin(IV) complexes containing mono or bidentate N-donor ligands

Abstract A series of adducts of the type [(L # ) y R n SnX 4− n ]· z H 2 O (L # =1-methylimidazole, y =1 or 2, R=Me, Et, Bu n or Ph, n =1, 2 or 3, X=Cl, Br or I, z =0, 1/2 or 1) has been characterized in the solid state and in solution by analyses, spectral (IR, 119 Sn Mossbauer, and 1 H, 13 C and 119 Sn NMR) data and conductivity measurements. The molecular weight determinations and the NMR data indicate that these organotin(IV) complexes partly dissociate in chloroform and acetone solution. The donor L # interacts with [(CH 3 ) 3 SnNO 3 ], yielding the 2:1 ionic complex [(L # ) 2 (CH 3 ) 3 Sn]NO 3 . The derivative [(L # ) 2 (CH 3 ) 2 SnCl 2 ] reacts with NaClO 4 , AgNO 3 , NaBPh 4 and KSC…

Syinthesis and spectroscopic and X-ray structural Characterization of R2Sn(IV)-Oxydiacetate and -Iminoacetate complexes

Investigations on organoantimony compounds

Abstract Diorganoantimony(V) complexes of the type R 2 SbClTrid (R = Me, Ph) containing dianionic, potentially tridentate Schiff-base ligands with ONO donor atoms (Trid 2− ) have been prepared and characterized. IR and NMR data suggest an octahedral coordination environment for the antimony atom with meridional arrangement of the ONO ligand atoms and a linear CSbC skeleton.

Tin( II ) and Lead( II ) 4‐Acyl‐5‐pyrazolonates: Synthesis, Spectroscopic and X‐ray Structural Characterization

Novel tin(II) β-diketonate Sn(Q)2 complexes [HQ = 1-R1-3-R3-4-R4(C=O)-pyrazol-5-one; HQC: R1 = Ph, R3 = Me, R4 = Cy; HQS: R1 = Ph, R3 = Me, R4 = CHPh2; HQL: R1 = Ph, R3 = Me, R4 = CH2Ph; HQT: R1 = Ph, R3 = Me, R4 = CH2tBu; HQE: R1 = Ph, R3 = Me, R4 = Et; HQB: R1 = Ph, R3 = Me, R4 = tBu; HQW: R1 = Ph, R3 = Me, R4 = p-(tBu)Ph; HQR: R1 = Ph, R3 = Me, R4 = p-[(CH2)5CH3]Ph; HQN: R1 = p-NO2Ph, R3 = Me, R4 = Ph; HQM: R1 = Me, R3 = Me, R4 = Ph; HQD: R1 = Me, R3 = Me, R4 = Me; HQP: R1 = Ph, R3 = Ph, R4 = Ph; HQG: R1 = Ph, R3 = Ph, R4 = Me; HQF: R1 = p-CF3Ph, R3 = Me, R4 = Ph; HQH: R1 = p-CF3Ph, R3 = Me, R4 = Me] have been isolated and characterized by single-crystal X-ray diffraction analyses, IR, 1…

Synthesis and characterization of some dibutylbis{5-[(E)-2-(aryl)-1-diazenyl]-2-hydroxybenzoato}tin(IV) compounds. Toxicity studies of di- and tri-organotin complexes on the second instar ofAedes aegypti mosquito larvae

The preparation and spectroscopic characterization of some complexes of the type Bu2Sn(LH)2 (LH = 5-[(E)-2-(aryl)-1-diazenyl]-2-hydroxybenzoate) are reported. On the basis of spectroscopic evidence (1H, 13C, 119Sn NMR, IR and 119mSn Mossbauer) the compounds were judged to adopt the usual dicarboxylato structural type with a skew trapezoidal arrangement. This was further confirmed by X-ray crystallography in the case of Bu2Sn(L5H)2 (L5H = 5-[(E)-2-(4-chlorophenyl)-1-diazenyl]-2-hydroxybenzoate). Toxicity studies of the di- and tri-organotin compounds on the second larval instar of Aedes aegypti mosquito larvae are reported. Copyright © 2003 John Wiley & Sons, Ltd.

6-Thiopurine complexes of organotin(IV) moieties. Synthesis and structural characterization by infrared and Mössbauer spectroscopy

Abstract The novel complexes Me3Sn(6-TP−1) and Bun2Sn(6-TP−1)2, where 6-TP−1 is the mono-anion of 6-thiopurine, have been synthesized. The sites of stannylation of 6-TP have been inferred from the known directions of electrophilic substitution reactions of 6-TP itself. The compounds have been characterized by infrared and Mossbauer spectroscopy. A solid state polymeric structure has been proposed for Me3Sn(6-TP−1), where planar SnC3 skeletons are bridged by 6-TP−1 (thione tautomer) axially bound to Sn through N(3) and N(1) atoms. For Bun2Sn(6-TP−1)2, a molecular structure has been advanced, with the ‘aromatic’ ligand anions chelating Sn by S-N(7) atoms.

Synthesis and characterization of triphenyltin(IV) complexes of azocarboxylates. Crystal structures of a ligand, HO2CC6H4{N=N(C6H3-4-OH(C(H)=NC6H4CH3-4))}-o hemihydrate, and triphenyltin complexes Ph3Sn[O2CC6H4{N=N(C6H3-4-OH(C(H)=NC6H4X-4))}-o] (X = Br, Me (polymeric) and OMe (dimeric))

Synthesis and structural studies by infrared and Mössbauer spectroscopy of adducts of tin(IV) and organotin(IV) derivatives with 2,2′-azopyridine

Abstract A number of complexes have been prepared by the reaction between 2,2′-azopyridine(AZP) and tin(IV) halides and organotin(IV) halides, and characterized by elemental analysis and infrared and variable temperature 119Sn Mossbauer spectroscopies. All of the new compounds have 1:1 stoichiometry, with the AZP ligand occupying two coordination sites by bonding through one of the ring and one of the azo group nitrogen atoms, to give rise to distorted octahedral structures. In the diorganotin complexes the two organic groups occupy trans positions. The infrared and Mossbauer spectroscopic data suggest that these compounds are monomeric in the solid state.

Re-visiting of 5-[(E)-2-(aryl)-1-diazenyl]-quinolin-8-ol with tweaking of Sn–Ph groups: Synthesis, spectroscopic characterization and X-ray crystallography

Abstract Reactions of sodium 5-[(E)-2-(aryl)-1-diazenyl]quinolin-8-olates (LH, where the aryl group is an R-substituted phenyl ring such that for L1H: R = H; L2H: R = 2′-CH3; L3H: R = 3′-CH3; L4H: R = 4′-CH3; L5H: R = 4′-OCH3 and L6H: R = 4′-OC2H5) with Ph3SnCl in a 1:1 molar ratio yielded complexes of composition Ph3SnL. The complexes have been characterized by 1H, 13C, 119Sn NMR, IR and 119mSn Mossbauer spectroscopic techniques in combination with elemental analyses. The crystal structures of Ph3SnL1 · 0.5C6H6 (1), Ph3SnL2 (2), Ph3SnL5 · C6H6 (5) and Ph3SnL6 · 0.5C6H6 (6) were determined. The results of the X-ray studies indicated that the benzene solvated compounds 1, 5 and 6 are distort…