A novel organotin complex [(n-Bu)3Sn(OCOC5H4NO)]n has been synthesized and characterized by elemental analysis, IR and ^1H NMR. The crystal structure has been determined by X-ray single-crystal diffraction. The cr...A novel organotin complex [(n-Bu)3Sn(OCOC5H4NO)]n has been synthesized and characterized by elemental analysis, IR and ^1H NMR. The crystal structure has been determined by X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P2 1/c with a = 8.982(2), b = 17.908(4), c = 13.219(3) A, β= 96.981(4)°, Z = 4, V= 2110.6(8) A^3, Dc = 1.347 g/cm^3, μ(MoKa) = 12.23 cm^-1, F(000) = 880, R = 0.0497 and wR = 0.1263. In the molecular structure of the title complex, the tin atoms are five-coordinated in a distorted trigonal bipyramidal geometry. A one-dimensional linear polymer is formed through an interaction between the O atoms of pyridine-3-carboxylic acid N-oxide and tin atoms of an adjacent molecule.展开更多
Three cyclohexyltin complexes of N-(3,5-dibromosalicylidene)valine(H_2L), Cy_3Sn(HL)(1), Cy_2SnL(2), and Cy2 SnL ·Cy_3Sn Cl(3)(Cy = cyclohexyl), have been synthesized and characterized by elemental ...Three cyclohexyltin complexes of N-(3,5-dibromosalicylidene)valine(H_2L), Cy_3Sn(HL)(1), Cy_2SnL(2), and Cy2 SnL ·Cy_3Sn Cl(3)(Cy = cyclohexyl), have been synthesized and characterized by elemental analysis, IR, and ~1H and ^(13) C NMR spectra. The crystal structures of 2 and 3 have been determined. Complex 2 belongs to the monoclinic system, space group P21/n with a = 21.250(8), b = 10.837(4), c = 23.050(8) ?, b = 93.193(9)°, V = 5300(3) ?~3, Z = 8, D_c = 1.659 g/cm^3, m = 4.004 mm^(-1), F(000) = 2624, R = 0.0471 and wR = 0.1015. Complex 3 belongs to the monoclinic system, space group P21 with a = 10.3452(10), b = 18.7665(18), c = 12.1483(12) ?, b = 103.374(2)°, V = 2294.5(4) ?3, Z = 2, D_c = 1.542 g/cm^3, m = 2.923 mm^(-1), F(000) = 1072, R = 0.0428 and wR = 0.0936. Complex 2 has a distorted trigonal bipyramidal geometry with the axial locations occupied by one carboxylate oxygen and a phenolic oxygen of the ligand, and 3 reveals that the two tin atoms are joined via the carbonyl atom of the ligand to form a mixed organotin binuclear complex. Bioassay results show that 1 and 2 have good in vitro antibacterial activity against Escherichia coli.展开更多
A novel anionic organotin(Ⅳ) complex {[(pClCHCH)Sn(HO)(Cl)OCOCH(O)CH(O)COSn(HO)(Cl)(p-ClCHCH)]·2(HNEt)}(1) was synthesized by the reaction of di(p-chlorobenzy)tin dichloride with the D-tartaric acid in 2:1 molar...A novel anionic organotin(Ⅳ) complex {[(pClCHCH)Sn(HO)(Cl)OCOCH(O)CH(O)COSn(HO)(Cl)(p-ClCHCH)]·2(HNEt)}(1) was synthesized by the reaction of di(p-chlorobenzy)tin dichloride with the D-tartaric acid in 2:1 molar in the presence of an organic base triethylamine. The structure was characterized by elemental analysis, IR, TG, XRD and single-crystal X-ray diffraction. It crystallizes in triclinic, P1 space group, with a = 0.7067(1), b = 1.9762(3), c = 2.2383(3) nm, α = 91.544(2)°, β = 90.075(2)°, γ = 90.110(2)°, V = 3.1247(7) nm~3, Z = 3, Dc = 1.621 g/cm~3, m(Mo Kα) = 16.29 cm–1, F(000) = 1530, R = 0.0394, wR = 0.1092,(Δρ)max = 1224 and(Δρ)min = –840 e/nm~3. The stabilities, orbital energies and composition characteristics of some frontier molecular orbitals of 1 have been carefully investigated with quantum chemistry calculation. In addition, the in vitro antitumor activity suggested that 1 had stronger inhibitory activity on H460, MCF7 than on A549.展开更多
The title compound,{[n-Bu_(2)Sn(O_(2)CCH_(2)CS_(2)NC_(4)H_(8))]_(2)O}_(2),has been synthesized by the reaction of(tetrahydro-pyrrodithiolocarbamoylthio)acetic acid with the di-n-bubyltin oxide in1∶1molar ratio.The co...The title compound,{[n-Bu_(2)Sn(O_(2)CCH_(2)CS_(2)NC_(4)H_(8))]_(2)O}_(2),has been synthesized by the reaction of(tetrahydro-pyrrodithiolocarbamoylthio)acetic acid with the di-n-bubyltin oxide in1∶1molar ratio.The complex has been characterized by elemental analysis,IR and NMR.The crystal structure of it has been determined by X-ray single crystal diffraction.And the results showed that the crystal belongs to triclinic system with space group P1and some crystal parameters:a=1.2202(9)nm,b=1.3158(10)nm,c=1.3804(10)nm,α=111.215(9)°,β=99.357(9)°,γ=96.075(10)°,V=2.006(2)nm 3,Z=1,F(000)=908,μ=1.489mm^(-1),D c=1.474g·cm^(-3),R_(1)=0.0375,wR_(2)=0.0839.The complex has a centrosymmetric dimer structure mode with a four-membered central endo-cyclic Sn_(2)O_(2)unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom which has a distorted octahedron.Each of the endo-cyclic tin atoms exhibits a distorted trigonal bipyramid coordination geometry with an additional weak coordination carboxylate oxygen.Four carboxylate ligands are divided into two types.And two of them are bidentate and connecting to each of exo-cyclic tin atoms by using both oxygen atoms,whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom only.CCDC:220513.展开更多
Two novel diethyltin(IV) complexes of N-salicylidenevaline (H2L1) and N-Sali- cylidenetryptophan (H2L^2), Et2SrtL^1 1 and Et2SnL^2 2, were synthesized and characterized by elemental analysis, IR, ^1H NMR and X-r...Two novel diethyltin(IV) complexes of N-salicylidenevaline (H2L1) and N-Sali- cylidenetryptophan (H2L^2), Et2SrtL^1 1 and Et2SnL^2 2, were synthesized and characterized by elemental analysis, IR, ^1H NMR and X-ray single-crystal diffraction analysis. Complex 1 belongs to the trigonal system, space group R-3 with a = b = 19.2730(5), c = 23.6890(13)A^°, V= 7620.4(5) A^°^3, Z = 6, Dc= 1.553 g/cm^3,μ= 1.518 mm^-1, F(000) = 3600, R = 0.0238 and wR = 0.0636. Complex 2 is of monoelinie system, space group P21/c with a = 13.7550(8), b = 11.5425(7), c = 12.7876(7)A^°, β= 93.585(1)°, V = 2026.3(2) A^°^3, Z = 4, Dc= 1.548 g/cm^3,μ = 1.286 mm^-1, F(000) = 976, R = 0.0298 and wR = 0.0722. Complex 1 is a cyclic trimer with a macrocyclic 12-membered ring structure formed by the bidentate bridging coordination of carboxylate group to tin atoms. The tin atom is six-coordinated in a distorted octahedral geometry. In complex 2, the distorted trigonal bipyramidal Et2SnL2 units are linked into polymeric chains by the weak Sn…O interaction involving Sn and the earbonyl O of an adjacent ligand, and the chains are further connected by intermolecular N-H…O hydrogen bonds to form a two-dimensional supramolecular structure.展开更多
A novel heterocyclic hexacoordinate organotin(Ⅳ) complex, bis(O-vanillin)-semi ethylenediamino dibenzyltin (VEDBT) was synthesized by the reaction of dibenzyltin dichloride with bis(O-vanillin)-semiethyenediamine, it...A novel heterocyclic hexacoordinate organotin(Ⅳ) complex, bis(O-vanillin)-semi ethylenediamino dibenzyltin (VEDBT) was synthesized by the reaction of dibenzyltin dichloride with bis(O-vanillin)-semiethyenediamine, its structure has been characterized by spectral methods. The electrodes using VEDBT as a neutral carrier show high selectivity for salicylate anions.展开更多
A novel ionic organotin complex{[Ph_(2)Sn]_(2)[2,6-(O_(2)C)_(2)]C_(5)H_(3)N}_(3)H_(2)O}^(2-)[HNEt_(3)]^(2+)has been unexpectedly obtained by the reaction of Ph_(3)SnCl and 2,6-pyridine dicarboxylic acid in 1:1 molar r...A novel ionic organotin complex{[Ph_(2)Sn]_(2)[2,6-(O_(2)C)_(2)]C_(5)H_(3)N}_(3)H_(2)O}^(2-)[HNEt_(3)]^(2+)has been unexpectedly obtained by the reaction of Ph_(3)SnCl and 2,6-pyridine dicarboxylic acid in 1:1 molar ratio in the presence of organic base Et_(3)N.Possible dephenylation mechanism was illustrated.The X-ray diffraction study has shown that the title complex consists of cation moiety[HNEt_(3)]^(+)and anion moiety{[Ph_(2)Sn]_(2)[2,6-(O_(2)C_(2))C_(5)H_(3)N]_(3)H_(2)O}^(2-)with tin(IV)in a pengonal bipyramidal coordination geometry.展开更多
The diorganotin(Ⅳ) complexes of N-(3,5-dibromosalicylidene)-α-amino acid, R2Sn(2-O-3,5-Br2C6H2CH= NCHRCOO)(where R=H, Me, i-Pr, Bz; R'=n-Bu, Cy), were synthesized by the reactions of diorganotin dichlorides...The diorganotin(Ⅳ) complexes of N-(3,5-dibromosalicylidene)-α-amino acid, R2Sn(2-O-3,5-Br2C6H2CH= NCHRCOO)(where R=H, Me, i-Pr, Bz; R'=n-Bu, Cy), were synthesized by the reactions of diorganotin dichlorides with in situ formed potassium salt of N-(3,5-dibromosalicylidene)-α-amino acid and characterized by elemental analysis, IR and NMR (^1H, ^13C and ^119Sn) spectra. The crystal structures of n-Bu2Sn(2-O-3,5-Br2C6H2CH= NCHRCOO)(R=i-Pr, Bz) and Cy2Sn(2-O-3,5-Br2C6H2CH=NCHRCOO)(R=Me, Bz) were determined by X-ray single crystal diffraction and showed that the tin atoms are in a distorted trigonal bipyramidal geometry to form five- and six-membered chelate rings with the tridentate ligand. Bioassay results indicated that the compounds possess better in vitro antitumour activity against three human tumour cell lines, HeLa, CoLo205 and MCF-7, than cis-platin and moderate anti-bacterial activity against two bacteria, E. coli and S. aureus.展开更多
Three new dimethyltin complexes of N-(3-methoxysalicylidene)-α-amino acid,(CH3)2Sn(3-CH3O-2-OC6H3CH=NCHRCOO)(R = H,1;CH3,2;(CH3)2CH,3),have been synthe-sized by treating dimethyltin dichloride with the pota...Three new dimethyltin complexes of N-(3-methoxysalicylidene)-α-amino acid,(CH3)2Sn(3-CH3O-2-OC6H3CH=NCHRCOO)(R = H,1;CH3,2;(CH3)2CH,3),have been synthe-sized by treating dimethyltin dichloride with the potassium salt of the ligand and characterized by elemental analysis,IR and 1H NMR spectra.The crystal structure of [(CH3)2Sn(3-CH3O-2-OC6H3CH=NCH2COO)(CH3OH)]2 H2O(1a),formed from methanol solution of 1,has been deter-mined.The crystal belongs to the monoclinic system,space group C/2c with a = 20.636(3),b = 7.8854(9),c = 20.668(2) ,β= 113.265(2)°,V = 3089.7(6) 3,Z = 4,Dc = 1.707 g/cm3,= 1.675 mm-1,F(000) = 1592,R = 0.0301 and wR = 0.0841.In complex 1a,the tin atom is six-coordinate and possesses a distorted [SnC2NO3] octahedral geometry with the two methyl groups occupying the trans positions.The weak Sn O interactions and intermolecular hydrogen bonds connected the molecules into an infinite chain.展开更多
The Schiff base organotin(IV) complex {[4-Et2NC6H3(O)C=NC6H3(O)-5-NO2](n- Bu2Sn)}2 has been synthesized via the reaction between 4-(diethylamino) salicylaldehyde-2-arnino- 4-nitrophenol Schiff base (H2L) a...The Schiff base organotin(IV) complex {[4-Et2NC6H3(O)C=NC6H3(O)-5-NO2](n- Bu2Sn)}2 has been synthesized via the reaction between 4-(diethylamino) salicylaldehyde-2-arnino- 4-nitrophenol Schiff base (H2L) and dibutyltin oxide. Complex C1 has been characterized by IR, 1H NMR, 13C NMR spectra, and elemental analysis, and its crystal structure was determined by X-ray diffraction, It crystallizes in the monoclinic system, space group P21/n with a = 15.6559(8), b = 9.1657(5), c = 18.8351(10) ]A, β = 107.3440(10)°, Z = 4, V = 2579.9(2) A3, Dc = 1.442 Mg.m-3, μ(MoKa) = 1.025 mm-1, F(000) = 1152, R = 0.0250 and wR = 0.0633. The central Sn atom is coordinated in a hexadentate manner to assume a distorted octahedral configuration. Complex C1 was studied by TGA analysis in air atmosphere. The interaction between complex C1 and the herring sperm DNA was realized through the intercalation of the complex based on the studies by EB fluorescent probe.展开更多
A novel seven-coordinated organotin complex [ nBu 2Sn-(OOCC 5H 4N-2) 2(H 2O)] was unexpectedly synthesized by reaction of nBu 3SnCl with 2-pyridinecarboxylic acid in 1∶1 molar ratio in the presence of ...A novel seven-coordinated organotin complex [ nBu 2Sn-(OOCC 5H 4N-2) 2(H 2O)] was unexpectedly synthesized by reaction of nBu 3SnCl with 2-pyridinecarboxylic acid in 1∶1 molar ratio in the presence of organic base Et 3N. The crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to rhombohedral with space group R-3c, a=1.5807(3) nm, b=1.5807(3) nm, c=1.5807(3) nm, α=105.717(2)°, β=105.717(2)°, γ=105.717(2)°, Z=6, V=3.397(8) nm 3, D c=1.452 g/cm 3, μ=1.158 mm -1, F(000)=1512, R 1=0.0447, wR 2=0.1038. In crystal, the tin atoms rendered seven-coordinate in a distorted pentagonal bipyramidal geometry. The two-dimensional network structure was formed by H-bonding interaction between the free oxygen atoms of carboxyl groups and the coordinated water molecules.展开更多
Two dibenzyltin compounds,{[C6H5O(O)C=N-N=C(Ph)COO](m-Cl-C6H4CH2)2-Sn(CH3OH)}2(1)and{[p-Me-C6H4O(O)C=N-N=C(Ph)COO](m-Cl-C6H4CH2)2Sn(CH3OH)}2(2),have been synthesized by microwave“one pot”reaction with benzoylhydrazi...Two dibenzyltin compounds,{[C6H5O(O)C=N-N=C(Ph)COO](m-Cl-C6H4CH2)2-Sn(CH3OH)}2(1)and{[p-Me-C6H4O(O)C=N-N=C(Ph)COO](m-Cl-C6H4CH2)2Sn(CH3OH)}2(2),have been synthesized by microwave“one pot”reaction with benzoylhydrazine(or p-methyl benzhydrazine),phenylglyoxylic acid and di-m-chlorobenzyltin dichloride.Compound 2 contains two crystals 2a and 2b.The compounds have been characterized with IR,elemental analysis,1H,13C and 119Sn NMR spectra,H RMS.Three crystals are all binuclear molecules with a Sn2O2 four-membered ring plane,and each Sn atom center is seven-coordinated with[SnO4C2N]to form a distorted pentagonal bipyramidal configuration.In vitro antitumor activities of all compounds and carboplatin were evaluated by MTT against three human cancer cells such as NCI-H460(lung cancer cells),HepG2(liver cancer cells)and MCF7(breast cancer cells),and compound 2 exhibited better antitumor activity.展开更多
A novel seven coordinate dimer bis[(2,6 pyridinedicarboxylato)(methanol)dibenzyltin(IV)] was synthesized by the reaction of (PhCH 2) 3SnCl with 2,6 pyridine dicarboxylic acid in 1∶1 molar ratio in methan...A novel seven coordinate dimer bis[(2,6 pyridinedicarboxylato)(methanol)dibenzyltin(IV)] was synthesized by the reaction of (PhCH 2) 3SnCl with 2,6 pyridine dicarboxylic acid in 1∶1 molar ratio in methanol solution. The structure was characterized by elemental analysis, IR and 1H NMR spectra, and the crystal structure was determined by X ray single crystal diffraction analysis. The crystal belongs to monoclinic space group P 2 1/ n, a =0 96250(19) nm, b =1 0947(2) nm, c =1 9965(4) nm, β =92 31(3)°, Z =2, V =2 1019(7) nm 3, D c=1 574 g/cm 3, μ =1 248 mm -1 , F (000)=1000, R 1=0 0675, wR 2=0 0836. In the crystals of the complex, each tin atom is seven coordinated in a distorted bipyramidal structure.展开更多
基金The project was supported by the National Natural Science Foundation of China (No. 20271025), the Natural Science Foundation of Shandong Province (No. Z2001B02) and the State Key Laboratory of Crystal Material
文摘A novel organotin complex [(n-Bu)3Sn(OCOC5H4NO)]n has been synthesized and characterized by elemental analysis, IR and ^1H NMR. The crystal structure has been determined by X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P2 1/c with a = 8.982(2), b = 17.908(4), c = 13.219(3) A, β= 96.981(4)°, Z = 4, V= 2110.6(8) A^3, Dc = 1.347 g/cm^3, μ(MoKa) = 12.23 cm^-1, F(000) = 880, R = 0.0497 and wR = 0.1263. In the molecular structure of the title complex, the tin atoms are five-coordinated in a distorted trigonal bipyramidal geometry. A one-dimensional linear polymer is formed through an interaction between the O atoms of pyridine-3-carboxylic acid N-oxide and tin atoms of an adjacent molecule.
基金Financially supported by Shandong Provincial Natural Science Foundation(ZR2013BM007)the Research Award Fund for Outstanding Young Scientists in Shandong Province(BS2014CL015)the National Natural Science Foundation of China(21302110)
文摘Three cyclohexyltin complexes of N-(3,5-dibromosalicylidene)valine(H_2L), Cy_3Sn(HL)(1), Cy_2SnL(2), and Cy2 SnL ·Cy_3Sn Cl(3)(Cy = cyclohexyl), have been synthesized and characterized by elemental analysis, IR, and ~1H and ^(13) C NMR spectra. The crystal structures of 2 and 3 have been determined. Complex 2 belongs to the monoclinic system, space group P21/n with a = 21.250(8), b = 10.837(4), c = 23.050(8) ?, b = 93.193(9)°, V = 5300(3) ?~3, Z = 8, D_c = 1.659 g/cm^3, m = 4.004 mm^(-1), F(000) = 2624, R = 0.0471 and wR = 0.1015. Complex 3 belongs to the monoclinic system, space group P21 with a = 10.3452(10), b = 18.7665(18), c = 12.1483(12) ?, b = 103.374(2)°, V = 2294.5(4) ?3, Z = 2, D_c = 1.542 g/cm^3, m = 2.923 mm^(-1), F(000) = 1072, R = 0.0428 and wR = 0.0936. Complex 2 has a distorted trigonal bipyramidal geometry with the axial locations occupied by one carboxylate oxygen and a phenolic oxygen of the ligand, and 3 reveals that the two tin atoms are joined via the carbonyl atom of the ligand to form a mixed organotin binuclear complex. Bioassay results show that 1 and 2 have good in vitro antibacterial activity against Escherichia coli.
基金Supported by the Open Fund Project innovation platform of Key Laboratory of Higher Educational Institutions of Hunan Province(GN16K01)Scientific&Technological Projects of Hengyang(2016KL03)+1 种基金Aid programs for Science and Technology Innovative Research Team in Higher Educational Institutions of Hunan Provincethe Key Discipline of Hunan Province,Project funding for research and innovation experiment of university students in Hunan Province
文摘A novel anionic organotin(Ⅳ) complex {[(pClCHCH)Sn(HO)(Cl)OCOCH(O)CH(O)COSn(HO)(Cl)(p-ClCHCH)]·2(HNEt)}(1) was synthesized by the reaction of di(p-chlorobenzy)tin dichloride with the D-tartaric acid in 2:1 molar in the presence of an organic base triethylamine. The structure was characterized by elemental analysis, IR, TG, XRD and single-crystal X-ray diffraction. It crystallizes in triclinic, P1 space group, with a = 0.7067(1), b = 1.9762(3), c = 2.2383(3) nm, α = 91.544(2)°, β = 90.075(2)°, γ = 90.110(2)°, V = 3.1247(7) nm~3, Z = 3, Dc = 1.621 g/cm~3, m(Mo Kα) = 16.29 cm–1, F(000) = 1530, R = 0.0394, wR = 0.1092,(Δρ)max = 1224 and(Δρ)min = –840 e/nm~3. The stabilities, orbital energies and composition characteristics of some frontier molecular orbitals of 1 have been carefully investigated with quantum chemistry calculation. In addition, the in vitro antitumor activity suggested that 1 had stronger inhibitory activity on H460, MCF7 than on A549.
文摘The title compound,{[n-Bu_(2)Sn(O_(2)CCH_(2)CS_(2)NC_(4)H_(8))]_(2)O}_(2),has been synthesized by the reaction of(tetrahydro-pyrrodithiolocarbamoylthio)acetic acid with the di-n-bubyltin oxide in1∶1molar ratio.The complex has been characterized by elemental analysis,IR and NMR.The crystal structure of it has been determined by X-ray single crystal diffraction.And the results showed that the crystal belongs to triclinic system with space group P1and some crystal parameters:a=1.2202(9)nm,b=1.3158(10)nm,c=1.3804(10)nm,α=111.215(9)°,β=99.357(9)°,γ=96.075(10)°,V=2.006(2)nm 3,Z=1,F(000)=908,μ=1.489mm^(-1),D c=1.474g·cm^(-3),R_(1)=0.0375,wR_(2)=0.0839.The complex has a centrosymmetric dimer structure mode with a four-membered central endo-cyclic Sn_(2)O_(2)unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom which has a distorted octahedron.Each of the endo-cyclic tin atoms exhibits a distorted trigonal bipyramid coordination geometry with an additional weak coordination carboxylate oxygen.Four carboxylate ligands are divided into two types.And two of them are bidentate and connecting to each of exo-cyclic tin atoms by using both oxygen atoms,whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom only.CCDC:220513.
基金supported by the NNSFC (20701027)the Post-Doctor Innovation Project of Shandong Province (200702021) the Key Laboratory of Colloid Interface Chemistry of Ministry of Education (200707)
文摘Two novel diethyltin(IV) complexes of N-salicylidenevaline (H2L1) and N-Sali- cylidenetryptophan (H2L^2), Et2SrtL^1 1 and Et2SnL^2 2, were synthesized and characterized by elemental analysis, IR, ^1H NMR and X-ray single-crystal diffraction analysis. Complex 1 belongs to the trigonal system, space group R-3 with a = b = 19.2730(5), c = 23.6890(13)A^°, V= 7620.4(5) A^°^3, Z = 6, Dc= 1.553 g/cm^3,μ= 1.518 mm^-1, F(000) = 3600, R = 0.0238 and wR = 0.0636. Complex 2 is of monoelinie system, space group P21/c with a = 13.7550(8), b = 11.5425(7), c = 12.7876(7)A^°, β= 93.585(1)°, V = 2026.3(2) A^°^3, Z = 4, Dc= 1.548 g/cm^3,μ = 1.286 mm^-1, F(000) = 976, R = 0.0298 and wR = 0.0722. Complex 1 is a cyclic trimer with a macrocyclic 12-membered ring structure formed by the bidentate bridging coordination of carboxylate group to tin atoms. The tin atom is six-coordinated in a distorted octahedral geometry. In complex 2, the distorted trigonal bipyramidal Et2SnL2 units are linked into polymeric chains by the weak Sn…O interaction involving Sn and the earbonyl O of an adjacent ligand, and the chains are further connected by intermolecular N-H…O hydrogen bonds to form a two-dimensional supramolecular structure.
文摘A novel heterocyclic hexacoordinate organotin(Ⅳ) complex, bis(O-vanillin)-semi ethylenediamino dibenzyltin (VEDBT) was synthesized by the reaction of dibenzyltin dichloride with bis(O-vanillin)-semiethyenediamine, its structure has been characterized by spectral methods. The electrodes using VEDBT as a neutral carrier show high selectivity for salicylate anions.
文摘A novel ionic organotin complex{[Ph_(2)Sn]_(2)[2,6-(O_(2)C)_(2)]C_(5)H_(3)N}_(3)H_(2)O}^(2-)[HNEt_(3)]^(2+)has been unexpectedly obtained by the reaction of Ph_(3)SnCl and 2,6-pyridine dicarboxylic acid in 1:1 molar ratio in the presence of organic base Et_(3)N.Possible dephenylation mechanism was illustrated.The X-ray diffraction study has shown that the title complex consists of cation moiety[HNEt_(3)]^(+)and anion moiety{[Ph_(2)Sn]_(2)[2,6-(O_(2)C_(2))C_(5)H_(3)N]_(3)H_(2)O}^(2-)with tin(IV)in a pengonal bipyramidal coordination geometry.
基金Project supported by the Natural Science Foundation of Shandong Province (No. Z2002F01), the State Key Laboratory of Crystal Materials (No. 2005B 103) and the Scientific Research Foundation of Qufu Normal University.
文摘The diorganotin(Ⅳ) complexes of N-(3,5-dibromosalicylidene)-α-amino acid, R2Sn(2-O-3,5-Br2C6H2CH= NCHRCOO)(where R=H, Me, i-Pr, Bz; R'=n-Bu, Cy), were synthesized by the reactions of diorganotin dichlorides with in situ formed potassium salt of N-(3,5-dibromosalicylidene)-α-amino acid and characterized by elemental analysis, IR and NMR (^1H, ^13C and ^119Sn) spectra. The crystal structures of n-Bu2Sn(2-O-3,5-Br2C6H2CH= NCHRCOO)(R=i-Pr, Bz) and Cy2Sn(2-O-3,5-Br2C6H2CH=NCHRCOO)(R=Me, Bz) were determined by X-ray single crystal diffraction and showed that the tin atoms are in a distorted trigonal bipyramidal geometry to form five- and six-membered chelate rings with the tridentate ligand. Bioassay results indicated that the compounds possess better in vitro antitumour activity against three human tumour cell lines, HeLa, CoLo205 and MCF-7, than cis-platin and moderate anti-bacterial activity against two bacteria, E. coli and S. aureus.
基金supported by the Natural Science Foundation of Shandong Province (ZR2010BL012)thescientific research projects of Binzhou University (BZXYG0901,BZXYQNLG200912,BZXYFB20100403)
文摘Three new dimethyltin complexes of N-(3-methoxysalicylidene)-α-amino acid,(CH3)2Sn(3-CH3O-2-OC6H3CH=NCHRCOO)(R = H,1;CH3,2;(CH3)2CH,3),have been synthe-sized by treating dimethyltin dichloride with the potassium salt of the ligand and characterized by elemental analysis,IR and 1H NMR spectra.The crystal structure of [(CH3)2Sn(3-CH3O-2-OC6H3CH=NCH2COO)(CH3OH)]2 H2O(1a),formed from methanol solution of 1,has been deter-mined.The crystal belongs to the monoclinic system,space group C/2c with a = 20.636(3),b = 7.8854(9),c = 20.668(2) ,β= 113.265(2)°,V = 3089.7(6) 3,Z = 4,Dc = 1.707 g/cm3,= 1.675 mm-1,F(000) = 1592,R = 0.0301 and wR = 0.0841.In complex 1a,the tin atom is six-coordinate and possesses a distorted [SnC2NO3] octahedral geometry with the two methyl groups occupying the trans positions.The weak Sn O interactions and intermolecular hydrogen bonds connected the molecules into an infinite chain.
基金supported by the Natural Science Foundation of Hunan Province (No. 13JJ3112)Scientific & Technological Projects of Hunan Province (No. 2013TZ2025, 2014FJ3060)+2 种基金Scientific Research Fund of Hunan Provincial Education Department of China (14C0171)the Foundation of Key Laboratory of Functional Organometallic Materials,University of Hunan Province(No. 13K03, 13K04, 13K05)the Science Foundation of Hengyang Normal University (No. 12C45, 13A21)
文摘The Schiff base organotin(IV) complex {[4-Et2NC6H3(O)C=NC6H3(O)-5-NO2](n- Bu2Sn)}2 has been synthesized via the reaction between 4-(diethylamino) salicylaldehyde-2-arnino- 4-nitrophenol Schiff base (H2L) and dibutyltin oxide. Complex C1 has been characterized by IR, 1H NMR, 13C NMR spectra, and elemental analysis, and its crystal structure was determined by X-ray diffraction, It crystallizes in the monoclinic system, space group P21/n with a = 15.6559(8), b = 9.1657(5), c = 18.8351(10) ]A, β = 107.3440(10)°, Z = 4, V = 2579.9(2) A3, Dc = 1.442 Mg.m-3, μ(MoKa) = 1.025 mm-1, F(000) = 1152, R = 0.0250 and wR = 0.0633. The central Sn atom is coordinated in a hexadentate manner to assume a distorted octahedral configuration. Complex C1 was studied by TGA analysis in air atmosphere. The interaction between complex C1 and the herring sperm DNA was realized through the intercalation of the complex based on the studies by EB fluorescent probe.
文摘A novel seven-coordinated organotin complex [ nBu 2Sn-(OOCC 5H 4N-2) 2(H 2O)] was unexpectedly synthesized by reaction of nBu 3SnCl with 2-pyridinecarboxylic acid in 1∶1 molar ratio in the presence of organic base Et 3N. The crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to rhombohedral with space group R-3c, a=1.5807(3) nm, b=1.5807(3) nm, c=1.5807(3) nm, α=105.717(2)°, β=105.717(2)°, γ=105.717(2)°, Z=6, V=3.397(8) nm 3, D c=1.452 g/cm 3, μ=1.158 mm -1, F(000)=1512, R 1=0.0447, wR 2=0.1038. In crystal, the tin atoms rendered seven-coordinate in a distorted pentagonal bipyramidal geometry. The two-dimensional network structure was formed by H-bonding interaction between the free oxygen atoms of carboxyl groups and the coordinated water molecules.
基金supported by the Hengyang Normal University College Students Innovation and Entrepreneurship Training Program(No.cxcy1944)Scientific Research Fund of Hunan Provincial Education Department of China(No.19C0279)+1 种基金Hengyang Normal University Industrial Supported Project(Nos.HXKJ201907,HXKJ201908,HXKJ201911,HXKJ201946,HXKJ201947)Foundation of Key Laboratory of Functional Organometallic Materials,University of Hunan Province(No.GN19K07)。
文摘Two dibenzyltin compounds,{[C6H5O(O)C=N-N=C(Ph)COO](m-Cl-C6H4CH2)2-Sn(CH3OH)}2(1)and{[p-Me-C6H4O(O)C=N-N=C(Ph)COO](m-Cl-C6H4CH2)2Sn(CH3OH)}2(2),have been synthesized by microwave“one pot”reaction with benzoylhydrazine(or p-methyl benzhydrazine),phenylglyoxylic acid and di-m-chlorobenzyltin dichloride.Compound 2 contains two crystals 2a and 2b.The compounds have been characterized with IR,elemental analysis,1H,13C and 119Sn NMR spectra,H RMS.Three crystals are all binuclear molecules with a Sn2O2 four-membered ring plane,and each Sn atom center is seven-coordinated with[SnO4C2N]to form a distorted pentagonal bipyramidal configuration.In vitro antitumor activities of all compounds and carboplatin were evaluated by MTT against three human cancer cells such as NCI-H460(lung cancer cells),HepG2(liver cancer cells)and MCF7(breast cancer cells),and compound 2 exhibited better antitumor activity.
文摘A novel seven coordinate dimer bis[(2,6 pyridinedicarboxylato)(methanol)dibenzyltin(IV)] was synthesized by the reaction of (PhCH 2) 3SnCl with 2,6 pyridine dicarboxylic acid in 1∶1 molar ratio in methanol solution. The structure was characterized by elemental analysis, IR and 1H NMR spectra, and the crystal structure was determined by X ray single crystal diffraction analysis. The crystal belongs to monoclinic space group P 2 1/ n, a =0 96250(19) nm, b =1 0947(2) nm, c =1 9965(4) nm, β =92 31(3)°, Z =2, V =2 1019(7) nm 3, D c=1 574 g/cm 3, μ =1 248 mm -1 , F (000)=1000, R 1=0 0675, wR 2=0 0836. In the crystals of the complex, each tin atom is seven coordinated in a distorted bipyramidal structure.