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1.
Three novel phosphoramidate ligands with formula , R = Nicotinamide(nia), R′ = NHC(CH3)3(L1), NH(C6H11) (L2); R = isonicotinamide(iso), NH(C6H11) (L3) and their new organotin(IV) complexes with formula SnCl2(CH3)2(X)2, X = L1 (C1), L2 (C2), L3 (C3) plus SnCl2(CH3)2(L4)2(C4), L4 = isoP(O)[NHC(CH3)3]2, were synthesized and characterized by 1H, 13C, 31P,119Sn NMR, IR, UV-Vis spectroscopy and elemental analysis. Two novel complexes of nia and iso with formula SnCl2(CH3)2(X)2, X = nia (C5), iso (C6) were also prepared and all the complexes were spectroscopically studied in comparison to their related ligands and to each other. The crystal structure of complexes C1, C3, C4, and C5 were determined by X-ray crystallography. -Sn-Cl···H-N- major hydrogen bonds beside other electrostatic interactions produced a three dimensional polymeric cluster in the crystalline lattice of C1, C3, C5 and a two dimensional polymeric chain in C4. Results showed that coordination of the phosphoramidate ligand (L4) to Sn in C4 has been occurred from the nitrogen site of the pyridine ring similar to C5,C6 in which there is no PO donor site; however, in C1 and C3 the active donor site of corresponding ligands is PO. It seems that in these complexes there is a competition between PO and Npyridine donor sites and the influential factor which determines the winner site is the type of substituents on phosphorus atom.  相似文献   

2.
A series of organotin (IV) complexes with 6-amino-1,3,5-triazine-2,4-dithiol of the type [(RnSnCl4−n)2 (C3H2N4S2)] (n = 3: R = Me 1, n-Bu 2, PhCH23, Ph 4; n = 2: R = Me 5, n-Bu 6, PhCH27, Ph 8) have been synthesized. All the complexes 1-8 have been characterized by elemental analysis, IR, 1H and 13C NMR spectra. Among them complexes 1, 4, 5 and 8 have also been characterized by X-ray crystallography diffraction analyses, which revealed that the tin atoms of complexes 1, 4, 5 and 8 are all five-coordinated with distorted trigonal bipyramid geometries.  相似文献   

3.
Four triorganotin(IV) complexes constructed from tetrafluorophthalic acid (H2tfp) with a 1?:?1?:?1 molar ratio of H2tfp: Et3N: R3SnCl gave two of type {[R3Sn (tfp)].Et3NH}4 (R?=?Me 1, R?=?n-Bu 2), and two of type [R3Sn (tfp).Et3NH] n (R?=?PhCH2 3, Ph 4). All the complexes are characterized by elemental, IR, 1H, 13C and 119Sn NMR analyses. Complexes 1 and 4 were also confirmed by X-ray crystallography. Complex 1 is tetranuclear with a 28-membered C16O8Sn4 macrocyclic ring system with a cavity. The supramolecular structure of 1 has been found to consist of a three-dimensional network built up by intermolecular N–H?···?O, C–H?···?O hydrogen bonds and C–F?···?F weak interactions. Complex 4 is an infinite polymeric structure. The salient feature of the supramolecular structure of 4 is that of a two-dimensional plane, in which intermolecular N–H?···?O and C–H?···?π hydrogen bonds are important.  相似文献   

4.
A series of diorganotin(IV) and triorganotin(IV) compounds of the type [R2Sn(pca)2ClSnR3]2 (RPhCH21, 2-ClC6H4CH22, 2-FC6H4CH23, 4-FC6H4CH24, 4-CNC6H4CH25, 4-ClC6H4CH26, 2,4-Cl2C6H3CH27; Hpca2-methylpyrazine-5-acid), [(nBu)3Sn(pca)]8, [(CH3)2Cl2Sn(pca)Sn(CH3)2(pca)]9, {[(nBu)2Sn(pca)]2O}210 and {[Ph2Sn(pca)]3O2[Ph2Sn(OCH3)]} 11 have been obtained by reactions of 2-methylpyrazine-5-acid with triorganotin(IV) chloride, diorganotin(IV) dichloride, and diorganotin(IV) oxide. All compounds were characterized by elemental, IR, and NMR spectra analyses. The crystal structure of compounds 1, 8-11 were determined by X-ray single crystal diffraction, which revealed that compound 1 was tetranuclear macrocyclic structures with seven-coordinate and five-coordinate tin atoms, compounds 8 and 9 were polymeric chain structures with five-coordinate and seven-coordinate tin atoms, compounds 10 and 11 were monomeric structures with six-coordinate and five-coordinate tin atoms.  相似文献   

5.
Four new complexes have been synthesized based on the 2,4,5-trifluoro-3-methoxybenzoic acid and 4,4′-bipy of the type [R3Sn(OOCC6HF3OCH3)]2·(4,4′-bpy). All complexes were characterized by elemental, IR, 1H, 13C and 119Sn NMR spectra analyses. Complexes 1 and 4 were also characterized by X-ray crystallography. Crystal structures of 1 and 4 show that the coordination number of tin atom is five and the 2D network is connected by intermolecular C–H···O interactions.  相似文献   

6.
A series of organotin(IV) complexes, [Bu2Sn(C6H5O2S)2] (1), [Bu3Sn(C6H5O2S)] (2), [Oct2Sn(C6H5O2S)2] (3) of 2-thiopheneacetic acid (HL) have been prepared and characterized through FT-IR and NMR spectroscopy. The crystal structure of 2 has been confirmed by X-ray single crystal analysis, in which tin adopts a trigonal bipyramidal geometry. The synthesized complexes have been screened for antibacterial, DNA protection, and enzyme inhibition activities against acetylcholinesterase as well as butylcholenesterase.  相似文献   

7.
A series of new triorganotin(IV) pyridinecarboxylates with 6-hydroxynicotinic acid (6-OH-3-nicH), 5-hydroxynicotinic acid (5-OH-3-nicH) and 2-hydroxyisonicotinic acid (2-OH-4-isonicH) of the types: [R3Sn (6-OH-3-nic)·L]n (I) (R = Ph, L = Ph·EtOH, 1; R = Bn, L = H2O·EtOH, 2; R = Me, L = 0, 3; R = n-Bu, L = 0, 4), [R3Sn (5-OH-3-nic)]n (II) (R = Ph, 5; R = Bn, 6; R = Me, 7; R = n-Bu, 8), [R3Sn (2-OH-4-isonic·L)]n (III) (R = Bn, 9, L = MeOH; R = Me, L = 0, 10; R = Ph, 11, L = 0.5EtOH) have been synthesized. All the complexes were characterized by elemental analysis, TGA, IR and NMR (1H, 13C, 119Sn) spectroscopy analyses. Among them, except for complexes 5 and 6, all complexes were also characterized by X-ray crystallography diffraction analysis. Crystal structures show that complexes 1-10 adopt 1D infinite chain structures which are generated by the bidentate O, O or N, O and the five-coordinated tin centers. Significant O-H?O, and N-H?O intermolecular hydrogen bonds stabilize these structures. Complex 11 is a 42-membered macrocycle containing six tin atoms, and forms a 2D network by intermolecular N-H?O hydrogen.  相似文献   

8.
Five new organotin(IV) complexes, [(R3Sn)(O2C15H13)] n (R?=?Me: 1; nBu: 2), [RSn(O)(O2C15H13)]6 (R?=?Ph: 3), [(R2Sn)2(O2C15H13)2(μ 3-O)]2 (R?=?Me: 4), and [(R2Sn)(O2C15H13)2] (R?=?nBu: 5), have been prepared by the reaction of 2,3-diphenylpropionic acid and the corresponding organotin chloride with sodium ethoxide in methanol. All the complexes were characterized by elemental analysis, FT-IR, NMR (1H, 13C, 119Sn) spectroscopy, TGA, and X-ray crystallography. The structural analyses reveal that 1 and 2 are 1-D infinite polymeric chains with Sn in syn–anti conformation. Complex 3 has a drum structure with six Sn centers. Complex 4 has a supramolecular chain-like ladder through weak intermolecular Sn?···?O interactions. Complex 5 is a monomer, connected into a 1-D polymer through intermolecular C–H?···?O interactions. Complexes 1 and 5 crystallize in the orthorhombic space groups P212121 and P21212, which are chiral space groups.  相似文献   

9.
A series of new triorganotin(IV) pyridinedicarboxylates [(C2H5)3NH][(Me3Sn)3(2,6-pdc)2(H2O)2] (1), [(C2H5)3NH][(Ph3Sn)3(2,6-pdc)2(H2O)2] (2), [(C2H5)3NH]{[(PhCH2)3Sn]3(2,6-pdc)2(H2O)2} (3), [Me3Sn(3,5-pdc)]n (4), [Ph3Sn(3,5-pdc)]n (5), [(PhCH2)3Sn(3,5-pdc)]n (6), [(Me3Sn)2(2,5-pdc)]n (7), [(Ph3Sn)2(2,5-pdc)]n (8) and {[(PhCH2)3Sn]2(2,5-pdc)}n (9) were synthesized by the reaction of trimethyltin(IV), triphenyltin(IV) or tribenzyltin(IV) chloride with 2,6(3,5 or 2,5)-H2pdc (pdc = pyridinedicarboxylate) when triethylamine was added. Complexes 1-9 have been characterized by elemental, IR, 1H, 13C and 119Sn NMR analyses. Among them complexes 1, 5 and 7 have also been characterized by X-ray crystallographic diffraction analyses. Complex 1 has a trinuclear structure and forms a 2D supramolecular structure due to the coordinated water molecules via hydrogen bonds to the pendant O atoms of the carboxyl groups and the N atoms derived of the pyridine ring. Complex 5 forms a 1D polymeric chain by the intermolecular Sn?N (N atom derived of pyridine ring) interactions. Complex 7 has a network structure where 2,5-pyridinedicarboxylate acts as a tetradentate ligand coordinated to trimethyltin(IV) ions.  相似文献   

10.
Several novel organotin(IV) complexes with formula SnCl2(CH3)2(X)2, X = C6H5C(O)NHP(O)(NC4H8)2 (1), C6H5C(O)NHP(O)(NC5H10)2 (2), C6H5C(O)NHP(O)[N(CH3)(C6H11)]2 (3), C6H5C(O)NHP(O)[NH-C(CH3)3]2 (4) were synthesized and characterized by 1H, 13C, 31P NMR, IR spectroscopy and elemental analysis. The structures have been determined for each of the four compounds. Compound 1 exists in the form of two symmetrically independent molecules in the crystalline state due to differences in their similar torsion angles. In all of the four structures there are intramolecular -Sn-Cl?H-N- hydrogen bonds, in addition to weak C-H?O and C-H?Cl hydrogen bonds. Both 1H and 13C NMR spectra show the coupling of 119/117Sn nuclei with methyl proton and carbon atoms. The δ(31P) of these complexes are in upfields with respect to their corresponding reported ligands. The spectroscopic and structural properties of these complexes were compared with those corresponding ligands.  相似文献   

11.
A series of new organotin (IV) complexes with 3-hydroxy-2-pyridinecarboxylic acid (3-OH-2-picH) of two types: R2SnCl(3-OH-2-pic) (I) (R = Me 1, n-Bu 2, Ph 3, PhCH24) and R2 Sn(3-OH-2-pic)2 (II) (R = Me 5, n-Bu 6, Ph 7, PhCH28)have been synthesized by reactions of diorganotin (IV) dichloride with 3-hydroxy-2-pyridinecarboxylic acid in the presence of sodium ethoxide. All complexes are characterized by elemental analyses, IR spectra and NMR spectra analyses. Among them, complexes 1, 5, 6 and 7 are also characterized by X-ray crystallography diffraction analyses. Complex 1 is a 1D polymeric chain with six-coordinate tin atoms and the packing of complex 1 is stabilized by the C-H?Cl intermolecular weak interactions, thus a 2D network of 1 is formed. Complex 5 is also a 1D polymeric chain with seven-coordinate tin atoms. Complex 6 is a zigzag polymeric chain linked by Sn?O intermolecular weak interactions. Complex 7 is a monomeric complex with distorted octahedral geometry.  相似文献   

12.
The di- and trialkyltin(IV) complexes of composition R2SnCl2−x (OAr), and n-Bu3Sn(OAr) (R = n-Bu and Me; x = 1 and 2; OAr = OC6H3Bu t -2-Me-4) have been synthesized by the reactions of di-n-butyl and dimethyltin dichlorides and tri-n-butyltin(IV) chloride with 2-tert-butyl-4-methylphenol and triethylamine in tetrahydrofuran. The reaction of triphenyltin chloride with trimethylsilyl-2-t-butyl-4-methylphenoxide in the same solvent however, gives a complex of composition Ph3Sn(OAr). The complexes have been characterized by microanalyses, molar conductance measurements, molecular weight determinations and IR and 1H, 13C and 119Sn NMR and mass spectral studies. Thermal behaviour of the complexes has been studied by TGA and DTA techniques. From the non-isothermal TG data, the kinetic and thermodynamic parameters have been calculated employing Coats-Redfern equation and the mechanism of decomposition has been computed using non-isothermal kinetic method. Thermal investigations on the blends of poly(methylmethacrylate). PMMA, with organotin(IV)-2-tert-butyl-4-methylphenoxides have shown increased thermal stability compared to pure PMMA suggesting thereby their potential as additives towards PMMA.  相似文献   

13.
Tri- and diorganotin(IV) dicarboxylates derived from trans-glutaconic acid and acetone 1,3-dicarboxylic acid were prepared. Their structure was studied using NMR, IR, and MS data. All of these compounds (except for compound 2a) are polymeric in the solid state and depolymerise upon dissolving in deuteriochloroform to give monomeric particles with four-coordinated central tin atoms. X-ray crystallography was used to characterize (E)-bis(tributylstannyl) pent-2-enedioate (1a). This compound crystallizes in a monoclinic space group system. The supramolecular organization of 1a can be described as layered polymeric sheets constructed of forty-membered rings that are interconnected on four different sites to the third dimension. Each layer assembled of the forty-membered rings, is made up of six triorganotin fragments and six trans-glutaconic acids, where four of them are incorporated in the core of the ring and other two are bidentate bridging and participating in the ring system by three atoms of CO2 group only.  相似文献   

14.
Some new tri- and diorganotin(IV) complexes of the general formula, R3Sn(H2L) and R′2Sn(HL) [where R = Me, n-Pr, n-Bu and Ph; R′ = Me, n-Bu, Ph and n-Oct; H3L = Schiff base (abbreviated as tren(4-Me-5-ImH)3) derived from condensation of tris(2-aminoethyl)amine (tren) and 4-methyl-5-imidazolecarboxaldehyde (4-Me-5-ImH)] have been synthesized. The coordination behaviour of Schiff base towards organotin(IV) moieties is discussed on the basis of infrared and far-infrared, 119Sn Mössbauer and multinuclear (1H, 13C and 119Sn) magnetic resonance (NMR) spectroscopic studies. Thermal studies of all of the synthesized organotin(IV) complexes have been carried out using TG, DTG and DTA techniques. The residues thus obtained from pyrolysis of the studied complexes have been characterized by X-ray powder diffraction analysis and IR. The newly synthesized complexes have been tested for their anti-inflammatory activity and toxicity (LD50).  相似文献   

15.
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   

16.
The di- and triorganotin(IV) derivatives of anthracenecarboxylic acid, Ph2MeSnOC(O)C14H9 (2), Me3SnOC(O)C14H9 (3), Me2Sn[OC(O)C14H9]2 · CH3OH (4) Ph3SnOC(O)C14H9 · CH3OH (5), Ph2EtSnOC(O)C14H9 (6), Ph2Sn[OC(O)(C14H9)]2 (7) and PhMe2SnOC(O)C14H9 (8) were synthesized by the reaction of Ph2MeSnI, Me3SnCl, Me2SnCl2, Ph3SnCl, Ph2EtSnI, Ph2SnCl2, and PhMe2SnI with 9-anthracenecarboxylic acid, respectively, with the aid of potassium iso-propoxide. All complexes were characterized by elemental analysis, mass spectrometry, IR, 1H, 13C and 119Sn NMR spectroscopes. The molecular structures of complexes 2, 3 and 4 were determined by single crystal X-ray analysis. The X-ray structures reveal that complex 2 and 3 adopt a polymeric trans-C3SnO2 trigonal bipyamidal configuration with the oxygen atoms occupying axial positions. Complex 4 adopts a monomeric structure with two carboxylates coordinated to tin in a monodentate form from axial and equatorial positions, and with the coordination number raised to five as the methanol occupies the apical position of the trigonal bipyramid.  相似文献   

17.
The novel macrocyclic complex (n-Bu2SnL)4·2C6H61 (LH2 = naphthalene-1,4-dicarboxylic acid, C6H6 = benzene) has been synthesized by the reaction of di-n-butyltin oxide and rigid naphthalene-1,4-dicarboxylic acid. Single crystal X-ray diffraction analyse shows that complex 1 has a centrosymmetric tetranuclear diorganotin dicarboxylate with 36-membered macrocycle, which is formed by n-Bu2Sn and ligand alternately linking. All four Sn atoms are hexacoordinated, and the coordination environment can be considered as a skew-trapezoidal bipyramidal with an anisobidentate coordination mode of the carboxylate groups. Luminescent property study of complex 1 has shown that the fluorescent peak was blue-shifted and the fluorescent intensity strengthened markedly compared with ligand. Pilot studies indicated that complex 1 has shown good antitumor activities. This complex 1 is likely to serve as a new model for further investigation on the structure-antitumor activity relationship.  相似文献   

18.
Four new diorganotin(IV) complexes, R2SnL (L?=?La: R?=?Me 1, Ph 2; L?=?Lb: R?=?Me 3, and Ph 4), have been synthesized by reaction of hydrazone ONO donors, 5-bromo-2-hydroxybenzaldehyde furan-2-carbohydrazone (H2La) and 2-hydroxynaphthaldehyde furan-2-carbohydrazone (H2Lb) with diorganotin(IV) dichloride in the presence of a base. The compounds have been investigated by elemental analysis and IR, 1H NMR, and 119Sn NMR spectroscopies. Spectroscopic studies show that the hydrazone is a tridentate dianionic ligand, coordinating via the imine nitrogen and phenolic and enolic oxygens. The structures of H2Lb and 3 have also been confirmed by X-ray crystallography. The results show that the structure of 3 is a distorted square pyramid with imine nitrogen in apical position. The in vitro antibacterial activities of ligands and complexes have been evaluated against gram-positive (Bacillus cereus and Staphylococcus aureus) and gram-negative (Escherichia coli and Pseudomonas aeruginosa) bacteria. H2La and H2Lb show no activity but the diphenyltin(IV) complexes exhibit good activities towards two bacterial strains in comparison with standard bacterial drugs.  相似文献   

19.
Four organotin(IV) compounds, [Bu6Sn6O6(L1)6] (1), [Bu6Sn6O6(L2)4(L3)2] (2), [Bu8Sn4O2(L2)4] (3) and [Ph3Sn(L2)] (4), were obtained by reactions of BuSnOH, Bu2SnO and Ph3SnOH with 4-((6-chloropyridin-3-yl)methylamino)benzonic acid (HL1), 4-((pyridin-2-yl)methylamino)benzonic acid (HL2) and p-aminobenzoic acid (HL3). 1 is a hexameric cluster, existing in a drum-like structure with prismatic Sn6O6 core. Compound 2 is a mixed drum, containing two kinds of carboxylic acid anions. Compound 3 possesses a Sn4O4 ladder structure. In 2 and 3, two-dimensional supramolecular structures are formed by the intermolecular hydrogen-bonding interactions. Compound 4 is a monomer with a dimer formed through π–π stacking between adjacent L2 anions. Compounds 14 were characterized by elemental analyses and IR spectra.  相似文献   

20.
The new sodium bis(1-methyl-1H-imidazol-2-ylthio)acetate, Na[(S-tim)2CHCO2], has been prepared in ethanol solution using 2-mercapto-1-methylimidazole, dibromoacetic acid and NaOH. New di- and tri-organotin(IV) derivatives have been synthesized from reaction between SnRnCl4−n (R = Ph, Cy and nBu, n = 2-3) acceptors and Na[(S-tim)2CHCO2]. Complexes of the type {[κ1O-(S-tim)2CHCO2]SnR3} and related decarboxylated species {[κ2N,N-(S-tim)2CH2]SnR2Cl2} have been obtained and characterized by elemental analyses, FT-IR, ESIMS and multinuclear (1H, 13C and 119Sn) NMR spectral data. The adduct {κ1O-[(S-tim)2CHCO2]Sn(H2O)(C4H9)3} was characterized by single crystal X-ray studies. The dichloromethane reaction solution of {κ1O-[(S-tim)2CHCO2]Sn(C6H5)3} was re-crystallized and the decarboxylated species {[(S-tim)2CH2]SnCl(H2O)(C6H5)3} was obtained as a crystalline solid and characterized by X-ray crystallography.  相似文献   

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