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1.
Some organotin(IV) triazolates of general formula RnSn(L)4 − n (where R = Me, n-Bu and Ph for n = 2; R = Me, n-Pr and n-Bu for n = 3 and HL = 3-amino-5-mercapto-1,2,4-triazole) have been synthesized by the reaction of R2SnCl2/R3SnCl with NaL in 1:2/1:1 molar ratio. Whereas, Oct2SnL2 has been synthesized azeotropically by the reaction of Oct2SnO and HL in 1:2 molar ratio. As good single crystals were not obtained, a large number of experimental techniques, viz. UV/Vis, IR, far-IR, multinuclear (1H, 13C and 119Sn) NMR and 119Sn Mössbauer spectroscopic studies, were used to accomplish a definitive characterization and determination of their most probable structures. In these compounds triazole acts as a monoanionic bidentate ligand, coordinating through Sexo and N(4). The IR and 119Sn Mössbauer spectroscopic studies allow us to deduce a highly distorted cis-trigonal-bipyramidal structure for R3SnL and a distorted skew trapezoidal-bipyramidal structure for R2SnL2, in the solid state. However, 1H, 13C and 119Sn NMR spectral studies revealed that weak bonding between tin and N(4) is further weakened in the solution leading to pseudo-tetrahedral/tetrahedral structure. 相似文献
2.
Mala Nath Pramendra K. Saini Xueqing Song 《Journal of organometallic chemistry》2008,693(13):2271-2278
The tetradendate macrocyclic ligands, [H2L-1 = 5,12-dioxa-7,14-dimethyl-1,4,8,11-tetraazacyclotetradeca-1,8-diene] and [H2L-2 = 6,14-dioxa-8,16-dimethyl-1,5,9,13-tetraazacyclohexadeca-1,9-diene] have been prepared by the condensation reaction of 1,2-diaminoethane and 1,3-diaminopropane, respectively, with ethyl acetoacetate in methanol at room temperature. The diorganotin(IV) complexes of general formula [R2Sn(L-1)/R2Sn(L-2)] (R = Me, n-Bu and Ph) have been synthesized by template condensation reaction of 1,2-diaminoethane or 1,3-diaminopropane and ethyl acetoacetate with R2SnCl2 (R = Me or Ph) or n-Bu2SnO in 2:2:1 molar ratio at ambient temperature (35 ± 2 °C) in methanol. The solid-state characterization of resulting complexes have been carried out by elemental analysis, IR, recently developed DART-mass, solid-state 13C NMR, 119mSn Mössbauer spectroscopic studies. These studies suggest that in all of the studied complexes, the macrocyclic ligands act as tetradentate coordinating through four nitrogen atoms giving a skew-trapezoidal bipyramidal environment around tin center. Since, the studied diorganotin(IV) macrocyclic complexes are insoluble in common organic solvents, hence good crystals could not be grown for single crystal X-ray crystallographic studies. Thermal studies of all of the studied complexes have also been carried out in the temperature range 0-1000 °C using TG, DTG and DTA techniques. The end product of pyrolysis is SnO2 confirmed by XRD analysis. 相似文献
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4.
Fabio Marchetti Claudio Pettinari Riccardo Pettinari Carlo Santini Allan H. White 《Journal of organometallic chemistry》2005,690(8):1878-1888
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 Mössbauer) 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). 相似文献
5.
《Journal of Coordination Chemistry》2012,65(23):3837-3844
The Schiff bases H2L1 and H2L2 have been prepared by the reaction of 2-amino-4-chlorophenol with pyrrole-2-carbaldehyde and 2-hydroxy-1-naphtaldehyde, respectively, and HL3 from reaction of 2-(aminomethyl)pyridine with 2-hydroxy-1-naphtaldehyde. Organotin complexes [SnPh2(L1)] (1), [SnPh2(L2)] (2), [SnMe2(L2)] (3) and [SnPhCl2(L3)] (4) were synthesized from reaction of SnPh2Cl2 and SnMe2Cl2 with these Schiff bases. The synthesized complexes have been investigated by elemental analysis and FT-IR, 1H NMR and 119Sn NMR spectroscopy. In complexes the Schiff bases are completely deprotonated and coordinated to tin as tridentate ligands via phenolic oxygen, pyrrolic, and imine nitrogens in 1, two phenolic oxygens and imine nitrogen in 2 and 3, and phenolic oxygen, imine and pyridine nitrogens in 4. The coordination number of tin in 1, 2, and 3 is five and in 4 is six. 相似文献
6.
Nath M Jairath R Eng G Song X Kumar A 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2005,61(13-14):3155-3161
New diorganotin(IV) derivatives of the general formula R2Sn(Umb)2 (where R = n-Bu, n-Oct and Ph; Umb = umbelliferone anion) have been synthesized either by the reaction of R2SnO with umbelliferone under azeotropic removal of water or by the reaction of R2SnCl2 with sodium salt of umbelliferone. Further, the adducts of the general formula R2Sn(Umb)2.phen (where R = n-Bu and n-Oct; phen = 1,10-phenanthroline) have also been synthesized by the interaction of R2Sn(Umb)2 with 1,10-phenanthroline. The bonding and coordination behavior in these derivatives are discussed on the basis of IR and 119Sn M?ssbauer spectroscopic studies in solid state. Their coordination behavior in solution is discussed by the multinuclear (1H, 13C and 119Sn) NMR spectral studies. The M?ssbauer and IR studies indicate that umbelliferone acts as a monoanionic bidentate ligand in R2Sn(Umb)2 coordinating through O(7) and O(1). A distorted octahedral geometry around tin has been proposed for R2Sn(Umb)2 as well as for R2Sn(Umb)2.phen in solid state. The newly synthesized derivatives have been tested for their anti-inflammatory and cardiovascular activities. The average LD50 value >1000 mg kg(-1) of these compounds indicates their safety margin. 相似文献
7.
Rati Agrawal Varsha Goyal Raakhi Gupta Pradeep Bhatnagar G. Bhargavi 《Phosphorus, sulfur, and silicon and the related elements》2016,191(7):1030-1035
A three-component reaction of dimethyltin dibromide with imidazo[1,2-a]pyridine, pyridine derivatives, or isoquinoline and allyl bromide in refluxing ethanol affords the ionic complex, bis(1-allylcycloiminium) dimethyltetrabromostannate (II). The reaction involves N-allylation of cycloimine accompanied by the coordination of two bromide ions with the tin atom of dimethyltin dibromide. The complexes have been characterized by infrared and 1H NMR, 13C NMR, and 119Sn NMR studies. The X-ray crystal structure analysis of a complex reveals the tin atom to be hexacoordinated and the dimethyltetrabromostannate (II) anion having octahedral geometry. Some of the complexes tested for their insecticidal activity are found to exhibit strong activity against Tribolium castaneum insect with LC50 ranging from 0.4 to 0.8 ppm. 相似文献
8.
Zafar A. Siddiqi M. Shahid Sarvendra Kumar Mohd Khalid Shabana Noor 《Journal of organometallic chemistry》2009,694(23):3768-301
Two novel dinuclear organotin(IV) complexes [n-Bu2Sn(imda)(H2O)]2·Bipy (1) and [n-Bu2Sn(imda)(H2O)]2·Phen (2) [H2imda = iminodiacetic acid, Bipy = 2,2′-bipyridine and Phen = 1,10-phenanthroline] were synthesised and characterized employing IR, 1H, 13C, 119Sn NMR, and 119Sn Mössbauer spectroscopic and elemental analyses. Single crystal X-ray crystallography of 1 has confirmed that it is a binuclear Sn(IV) species formed via carboxylate bridges where each metal adopted a seven coordinate distorted pentagonal bipyramidal geometry. The iminodiacetate dianion (imda2−) acts as a potential tridentate [N,O,O] carboxylate bridging ligand. The packing revealed that the additional α-diimine (Bipy or Phen) does not coordinate to metal ion. However, its presence in the crystal lattice as spacer helps for the formation of a supramolecular framework by bringing the two binuclear species close enough through extensive H-bonding. The in vitro cytotoxicity of compounds 1 and 2 indicate better results than cisplatin against three tumor cell lines investigated. 相似文献
9.
New triorganotin(IV) derivatives of the general formula R3Sn(Umb) (where, R = Me, n-Bu and Ph; Umb = umbelliferone anion) have been synthesized using sodium salt method. Further, the adducts of the general formula R3Sn(Umb) · phen (where R = Me and Ph; phen = 1,10-phenanthroline) have also been synthesized by the interaction of the triorganotin(IV) derivatives of umbelliferone with 1,10-phenanthroline. The bonding and coordination behavior of these derivatives are discussed on the basis of IR, NMR (1H, 13C and 119Sn), and 119Sn Mössbauer spectroscopic studies. These investigations indicate that umbelliferone acts as a monoanionic bidentate ligand in R3Sn(Umb) coordinating through O(7) and O(1) in the solid-state. These polymeric R3Sn(Umb) derivatives (where R = Me and n-Bu) have been proposed to have a trans-trigonal bipyramidal geometry with the three R groups in equatorial positions, while the axial positions are occupied by a phenolic oxygen and the O(1) atom from the adjacent molecule. A pseudotetrahedral geometry has been suggested for Ph3Sn(Umb). A distorted octahedral geometry around tin has been proposed for R3Sn(Umb) · phen, in which umbelliferone anion acts as a monodentate ligand coordinating through phenolic oxygen O(7). The newly synthesized derivatives have been assayed for their anti-inflammatory, cardiovascular and anti-microbial activities. The average LD50 values >1000 mg kg−1 of these derivatives indicate their safety margin. Among all the compounds tested, Ph3Sn(Umb) · phen has been found to show potent anti-inflammatory activity with low mammalian toxicity and mild hypotensive activity. 相似文献
10.
Rajkumar Joshi Guruaribam Shashikumar Sharma Vikrant Kumar Athar Adil Hashmi Satyendra Kumar R. Achila M. Ejaz Hussain 《应用有机金属化学》2006,20(11):740-746
A heteroscorpionate ligand, potassium hydrobis(benzoato)(salicylaldehyde)borate (KL), has been synthesized. This was converted into organotin complexes R2SnL2 and R3SnL complexes by mixing and stirring with a methanolic solution/suspension of organotin chloride. The ligand and its complexes were characterized by elemental analyses and spectral studies (IR, 1H NMR, 13C NMR, ESI mass spectra and Thermo gravimetric analysis (TGA)). Antibacterial and antifungal studies of these compounds were evaluated by the disc diffusion method at variable concentration against three species of bacteria (Staphylococcus aureus, Klebsiella pneumonia and Bacillius subtillis) and two species of fungi (Asperjillius fiavus and Candida albicans). It was found that triorganotin derivatives (R3SnL) of the ligand were more effective as compared with diorganotin derivatives (R2SnL2). The organotin complexes of borates were tested for their algicidal activity on the cyanobacterial strains Aulosira fertilissma, Anabaena species, Anabaena variabilis and Nostoc muscorum and showed high to moderate toxicity towards the above species. The ligand and its complexes were also tested for its pH effect on soil in vitro for a duration of more than one month and it was found that they are able to kill pests without damaging the soil quality. Copyright © 2006 John Wiley & Sons, Ltd. 相似文献
11.
Maura Pellei Giancarlo Gioia Lobbia Riccardo Spagna 《Journal of organometallic chemistry》2006,691(8):1615-1621
New mono-, di- and tri-organotin(IV) derivatives containing the neutral bis(2-pyridylthio)methane ligand, [(pyS)2CH2] and tris(2-pyridylthio)methane ligand, [(pyS)3CH] have been synthesized from reaction with SnRnCl4−n (R = Me, nBu, Ph and Cy, n = 1-3) acceptors. Mono-nuclear adducts of the type {[(pyS)2CH2]RnSnCl4−n} and {[(pyS)3CH]RnSnCl4−n} have been obtained and characterized by elemental analyses, FT-IR, ESI-MS, multinuclear (1H and 119Sn) NMR spectral data. The 1H and 119Sn NMR and ESI-MS data suggest for the triorganotin(IV) derivatives a complete dissociation of the compounds in solution. The mono- and di-organotin(IV) derivatives show a greater stability in solution, and their spectroscopic data are in accordance with the existence of six-coordinated RSnCl3N2 or R2SnCl2N2 species. 相似文献
12.
《Journal of Coordination Chemistry》2012,65(19):3395-3402
The reaction of 2-thiazoline-2-thione (TZDSH) with SnR2Cl2 (R=Ph 1, Me 2, Bu 3) in dry ethanol in the presence of sodium ethoxide leads to [SnR2(C3H4NS2)2] (1, 2, and 3), respectively. Reaction between TZDSH and SnPh2Cl2 in dichloromethane and dry ethanol in an inert atmosphere produces [SnPh2Cl2(C3H5NS2)2] (4). The yields of the products were over 80%. These new complexes have been characterized by IR, UV-Vis, multinuclear (1H, 13C, and 119Sn) NMR spectroscopy, and mass spectrometry, as well as elemental analysis. 相似文献
13.
《Journal of Coordination Chemistry》2012,65(7):1142-1152
The Schiff base has been synthesized by reacting tranexamic acid with indol-3-carboxyaldehyde in the first step and then with carbon disulfide at room temperature in the second step. The homobimetallic complexes have been synthesized by reaction of Schiff base with R2SnCl2 and R3SnCl in 1?:?2?M ratio under stirring, where R?=?methyl, n-butyl and phenyl. The ligand and complexes have been characterized by elemental analysis, FT-IR, multinuclear NMR (1H, 13C and 119Sn) and semi-empirical study. IR data reveal the bidentate nature of the ligand. Five- or six-coordinate geometry was confirmed in solution by NMR spectroscopy. The homobimetallic complexes and ligand were tested in vitro against some pathogenic bacteria and fungi to assess their antimicrobial properties. The complexes show biological activities with few exceptions. 相似文献
14.
Attila Szorcsik Michelangelo Scopelliti Lorenzo Pellerito 《Journal of organometallic chemistry》2005,690(9):2243-2253
Twenty-two n-butyltin(IV) and t-butyltin(IV) complexes of ligands containing an -OH (-CO) group or -OH and -COOH groups and an aromatic {N} donor atom were prepared by metathetical reactions. On the basis of the FT-IR and Mössbauer spectroscopic data, molecular structures were assigned to these compounds. The binding sites of the ligands were identified by means of FT-IR spectroscopic measurements, and it was found that in most cases the organotin(IV) moiety reacts with the phenolic form of these ligands. In the complexes with -OH and -COOH functions, the -COOH group is coordinated to the organotin(IV) centres in a monodentate manner. The 119Sn Mössbauer and the FT-IR studies support the formation of trigonal bipyramidal (TBP) and octahedral (Oh) molecular structures. Furthermore, X-ray diffraction analysis has been performed on the n-butyltin(IV)- and t-butyltin(IV)-8-quinol 8-olato-O,N single crystals. The hexacoordinated tin centres exhibit cis-octahedral geometry in both complexes. 相似文献
15.
《Journal of Coordination Chemistry》2012,65(5):409-420
New organotin(IV) derivatives containing the anionic ligand bis(3,5-dimethylpyrazolyl)dithioacetate [L2CS2]? have been synthesized by reaction of SnR n X4? n (R?=?Me, Ph, n Bu or Cy; n?=?1–3) acceptors and Li[L2CS2]. Mononuclear complexes of the type [L2CS2]R n SnCl4? n ?1} have been obtained and fully characterized by elemental analyses and FT-IR in the solid state, and by NMR (1H and 119Sn) spectroscopy, conductivity measurements and electrospray ionization mass spectrometry (ESI-MS) in solution. ESI-MS spectra of methanol solutions of diorganotin derivatives, recorded with fragmentor potentials of 0, 50, 100 and 150?V, show the occurrence at 150?V of peaks attributable to the loss of the CS2 group from the ligands and the formation of stable tetraorganodistannoxane species. 相似文献
16.
Attila Szorcsik István Kökény Michelangelo Scopelliti Lorenzo Pellerito 《Journal of organometallic chemistry》2007,692(16):3409-3414
Diorganotin(IV)-complexes of the N-nitroso-N-phenylhydroxylaminates (hereinafter cupf), Et2Sn(cupf)2 (1), Bu2Sn(cupf)2 (2), {[Bu2Sn(cupf)]2O}2 (3), t-Bu2Sn(cupf)2 (4) and Oc2Sn(cupf)2 (5, 6) were prepared and characterised by FT-IR and Mössbauer spectroscopic measurements. The binding modes of the ligand were identified by FT-IR spectroscopy, and it was found that the ligand is coordinated in chelating or bridging mode to the organotin(IV) center. The 119Sn Mössbauer and FT-IR studies support the formation of trans-Oh (1-6) structures. The X-ray diffraction analysis of 4 revealed that the tin centre is in a skew-trapezoidal geometry defined by four donors derived from the cupferronato ligands and two carbon atoms from the tin-bound tbutyl substituents. The 119Sn NMR investigations indicate that in solution 4 retains its hexacoordinated nature. 相似文献
17.
o-Cyclohexadiamine (the base component of tetraplatin) adducts of Ph2Sn(OCOCH3)2, nBu2Sn(OCOH3)2, (PhCH2)2Sn(OCOCH3)2, PhSn(OCOCF3)3, BuSn(OCOCH3)3 and Sn(OCOCH3)4 have been synthesized and characterized by elemental analysis and spectroscopy. The compounds appear to be the first such adducts in their class. 相似文献
18.
《Journal of Coordination Chemistry》2012,65(20):3741-3758
The synthesis of trinuclear Sn(IV) complexes 5a–h – prepared in a one-pot reaction of 2-amino-4-R-phenol (R=H, Me, Cl, NO2), 2-pyridine-carboxaldehyde, 1,3,5-benzenetricarboxylic acid (trimesic acid, H3BTC), and dibutyl and dioctyltin oxides – is described. These compounds were characterized by elemental analysis, mass spectrometry, IR, and multinuclear NMR spectroscopy. The structures of 5a and 5b were also determined by single-crystal X-ray analysis. The trinuclear tin system is formed by bridges through the carboxylate moieties. The metal centers are seven-coordinate and the coordination polyhedron of tin can be depicted as distorted pentagonal-bipyramidal (PBP), where the equatorial plane consists of three oxygens and two nitrogens and the organic groups occupy the axial positions. The work presented here combines the useful properties of Schiff bases and H3BTC ligands in the formation of organotin(IV) complexes, and investigates the likely antioxidant (DPPH and TBARS) and anti-inflammatory activity (TPA) of the new substances. 相似文献
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20.
Bhattacharya S 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2005,61(13-14):3145-3149
Five new monorganotin(IV) compounds with thiobenzoate ligand, [BuSn(SOCPh)2]2O (1), [BuSn(O)(SOCPh)]2 (2), BuSn(Cl)(SOCPh)2 (3), BuSn(Cl)2(SOCPh) (4) and [BuSn(OH)(Cl)(SOCPh)]2 (5) were synthesized and characterized by elemental analyses, IR, 1H and 13C NMR spectroscopy. 119Sn NMR spectroscopy was used to determine the coordination geometry around Sn(IV) in the cases of 2 and 4. 1, 2 and 5 are dimeric while 3 and 4 are monomeric. In all these molecules the thiobenzoate ion is coordinated only through its sulfur atom. Molecular structures of the compounds have been optimized by MM2 calculations. Semi-empirical quantum mechanical calculations (PM3 method) were performed to explain the monodentate-bonding pattern of thiobenzoate ligand. 相似文献