Four new five-coordinated anionic tin(Ⅳ) complexes with a form of [R_ n NH_ 4- n ][PhSn( μ 2-SCH_2COO)_2] were synthesized via the reaction of mercaptoacetic acid with phenyltin trichloride in the presence of dif...Four new five-coordinated anionic tin(Ⅳ) complexes with a form of [R_ n NH_ 4- n ][PhSn( μ 2-SCH_2COO)_2] were synthesized via the reaction of mercaptoacetic acid with phenyltin trichloride in the presence of different organic bases and characterized by means of IR, 1H NMR and MS spectroscopies. The crystal structure of [( i -Pr)_2NH_2] [PhSn( μ 2-SCH_2COO)_2] was determined by X-ray diffraction. In the crystal structure,the tin atom is five-coordinated and exists in trigonal bipyramid geometry with cell parameters a =1.1766(11) nm, b =1.3144(14) nm, c =1.3336(15) nm,β =90° and Z =4.展开更多
Chelate tetra(acetylacetonato) tin(Ⅳ) was prepared and used as catalyst for polytrimethylene terephthalate synthesis.It exhibited higher catalytic activity than tetrabutyl titanate,butyltinhydroxide oxide and dibutyl...Chelate tetra(acetylacetonato) tin(Ⅳ) was prepared and used as catalyst for polytrimethylene terephthalate synthesis.It exhibited higher catalytic activity than tetrabutyl titanate,butyltinhydroxide oxide and dibutyltin oxide.Decrease in reaction time, content of terminal carboxyl group,color intensity and increase in intrinsic viscosity were observed.The unique molecular structure can be considered as factor remarkably improving the catalytic activity of tetra(acetylacetonato) tin(Ⅳ).展开更多
Axially substituted tin phthalocyanines, namely dichloride-tetra-（α-pentyloxy） tin （Ⅳ） phthalocyanine 2, dihydroxy-tetra-（α-pentyloxy） tin （Ⅳ） phthalocyanine 3 and its dimmer di-μ-oxo-tetra-（α-pentyloxy...Axially substituted tin phthalocyanines, namely dichloride-tetra-（α-pentyloxy） tin （Ⅳ） phthalocyanine 2, dihydroxy-tetra-（α-pentyloxy） tin （Ⅳ） phthalocyanine 3 and its dimmer di-μ-oxo-tetra-（α-pentyloxy） tin（Ⅳ） phthalocyanine 4 were synthesized. The catalytic effect of H2O-free CaCl2 in quinoline was used for condensation of dihydroxy tin phthalocyanine 3 to the cofacially array dimmer 4. Their structures were characterized by UV-vis, IR, elemental analysis, MS, as well as ^1HNMR spectroscopy.展开更多
Three tin ? complexes with N,N- dialkyl dithiocarbamates Ph3SnS2CN(CH3)C6 H5 (1),Ph3SnS2CN(C4H8NH) (2) and Sn(Cl)2(S2CNEt2)2 (3) have been synthesized. Th e crystal structures have been determined by X- ray sin- <I...Three tin ? complexes with N,N- dialkyl dithiocarbamates Ph3SnS2CN(CH3)C6 H5 (1),Ph3SnS2CN(C4H8NH) (2) and Sn(Cl)2(S2CNEt2)2 (3) have been synthesized. Th e crystal structures have been determined by X- ray sin- <IMG SRC="IMAGE/0915 0031.JPG" HEIGHT=11 WIDTH=12>gle crystal diffraction. A crystal of the complex 1 is triclinic with space group , a=0.9485(3)nm, b=1.0491(3)nm, c=1.3631(4)nm, α =70.996(4)° , β =72.294(4)° , γ =79.609(4)° , Z=2, V=1.2168(6)nm3, <IMG SR C="IMAGE/09150032.JPG" HEIGHT=11 WIDTH=12>Dc=1.453g· cm- 3, μ =1.234mm- 1, R =0.0442, wR=0.0858. A crystal of the complex 2 is monoclinic with space group P2 (1)/c, a=1.2214(2)nm, b=1.1651(2)nm, c=1.5769(3)nm,β =99.039(2)° , Z=2, V=2.21 62(7)nm3, Dc=1.532g· cm- 3, μ =1.352mm- 1, R=0.0267, wR=0.0591. A crystal of the complex 3 is triclinic with space group , a=0.7179(2)nm, b=0.9256(3)nm, c=1 .5327(5)nm,α =93.857(4)° ,β =98.992(4)° , γ =109.481(4)° , Z=2, V=0.9405(5 )nm3, Dc=1.717g· cm- 3, μ =2.076mm- 1, R=0.0263, wR=0.0662. In the complexes 1 and 2 the tin atoms rendered five- coordination in a distorted tigonal bipyr amidal structure and in the complex 3 the tin atom rendered six- coordination i n a distorted octahedron structure. CCDC: 1, 179918; 2, 180024; 3, 180004.展开更多
Five-coordinated anionic tin(Ⅳ) complexes with the form [Ph 2Sn(μ 2-SCH 2COO)Cl]·[R nNH 4-n] were synthesized by the reaction of mercaptoacetic acid with diphenyltin dichloride in the presence of organic amines...Five-coordinated anionic tin(Ⅳ) complexes with the form [Ph 2Sn(μ 2-SCH 2COO)Cl]·[R nNH 4-n] were synthesized by the reaction of mercaptoacetic acid with diphenyltin dichloride in the presence of organic amines. All of the compounds synthesized were characterized by elemental analysis, IR, 1H NMR. The crystal structures of [C 5H 5NH][Ph 2Sn(μ 2-SCH 2COO)Cl](6) and [PhMeNH 2]· [Ph 2Sn(μ 2-SCH 2COO)Cl](8) were determined by X-ray diffraction. In the crystal structure, there were trigonal bipyramid geometries with five-coordinated tin atom and hydrogen-bonding interaction between anionic and cationic ions. Crystals of compound 6 were monoclinic, space group P2 1/n, a= 1.034 7(4) nm, b=1.396 8(5) nm, c=1.405 6(5) nm, β=95.366(6)°, Z=4; Crystals of compound 8 were monoclinic, space group P2 1/c, a=0.922 9(3) nm, b=1.334 5(5) nm, c= 1.838 5(7) nm, β=93.673(7)°, Z=4.展开更多
文摘Four new five-coordinated anionic tin(Ⅳ) complexes with a form of [R_ n NH_ 4- n ][PhSn( μ 2-SCH_2COO)_2] were synthesized via the reaction of mercaptoacetic acid with phenyltin trichloride in the presence of different organic bases and characterized by means of IR, 1H NMR and MS spectroscopies. The crystal structure of [( i -Pr)_2NH_2] [PhSn( μ 2-SCH_2COO)_2] was determined by X-ray diffraction. In the crystal structure,the tin atom is five-coordinated and exists in trigonal bipyramid geometry with cell parameters a =1.1766(11) nm, b =1.3144(14) nm, c =1.3336(15) nm,β =90° and Z =4.
基金the National High Technology Research and Development Program of China(No. 2003AA321010)the Innovation Research Fund of Graduate University,Chinese Academy of Sciences(2006)
文摘Chelate tetra(acetylacetonato) tin(Ⅳ) was prepared and used as catalyst for polytrimethylene terephthalate synthesis.It exhibited higher catalytic activity than tetrabutyl titanate,butyltinhydroxide oxide and dibutyltin oxide.Decrease in reaction time, content of terminal carboxyl group,color intensity and increase in intrinsic viscosity were observed.The unique molecular structure can be considered as factor remarkably improving the catalytic activity of tetra(acetylacetonato) tin(Ⅳ).
文摘Axially substituted tin phthalocyanines, namely dichloride-tetra-（α-pentyloxy） tin （Ⅳ） phthalocyanine 2, dihydroxy-tetra-（α-pentyloxy） tin （Ⅳ） phthalocyanine 3 and its dimmer di-μ-oxo-tetra-（α-pentyloxy） tin（Ⅳ） phthalocyanine 4 were synthesized. The catalytic effect of H2O-free CaCl2 in quinoline was used for condensation of dihydroxy tin phthalocyanine 3 to the cofacially array dimmer 4. Their structures were characterized by UV-vis, IR, elemental analysis, MS, as well as ^1HNMR spectroscopy.
文摘Three tin ? complexes with N,N- dialkyl dithiocarbamates Ph3SnS2CN(CH3)C6 H5 (1),Ph3SnS2CN(C4H8NH) (2) and Sn(Cl)2(S2CNEt2)2 (3) have been synthesized. Th e crystal structures have been determined by X- ray sin- <IMG SRC="IMAGE/0915 0031.JPG" HEIGHT=11 WIDTH=12>gle crystal diffraction. A crystal of the complex 1 is triclinic with space group , a=0.9485(3)nm, b=1.0491(3)nm, c=1.3631(4)nm, α =70.996(4)° , β =72.294(4)° , γ =79.609(4)° , Z=2, V=1.2168(6)nm3, <IMG SR C="IMAGE/09150032.JPG" HEIGHT=11 WIDTH=12>Dc=1.453g· cm- 3, μ =1.234mm- 1, R =0.0442, wR=0.0858. A crystal of the complex 2 is monoclinic with space group P2 (1)/c, a=1.2214(2)nm, b=1.1651(2)nm, c=1.5769(3)nm,β =99.039(2)° , Z=2, V=2.21 62(7)nm3, Dc=1.532g· cm- 3, μ =1.352mm- 1, R=0.0267, wR=0.0591. A crystal of the complex 3 is triclinic with space group , a=0.7179(2)nm, b=0.9256(3)nm, c=1 .5327(5)nm,α =93.857(4)° ,β =98.992(4)° , γ =109.481(4)° , Z=2, V=0.9405(5 )nm3, Dc=1.717g· cm- 3, μ =2.076mm- 1, R=0.0263, wR=0.0662. In the complexes 1 and 2 the tin atoms rendered five- coordination in a distorted tigonal bipyr amidal structure and in the complex 3 the tin atom rendered six- coordination i n a distorted octahedron structure. CCDC: 1, 179918; 2, 180024; 3, 180004.
文摘Five-coordinated anionic tin(Ⅳ) complexes with the form [Ph 2Sn(μ 2-SCH 2COO)Cl]·[R nNH 4-n] were synthesized by the reaction of mercaptoacetic acid with diphenyltin dichloride in the presence of organic amines. All of the compounds synthesized were characterized by elemental analysis, IR, 1H NMR. The crystal structures of [C 5H 5NH][Ph 2Sn(μ 2-SCH 2COO)Cl](6) and [PhMeNH 2]· [Ph 2Sn(μ 2-SCH 2COO)Cl](8) were determined by X-ray diffraction. In the crystal structure, there were trigonal bipyramid geometries with five-coordinated tin atom and hydrogen-bonding interaction between anionic and cationic ions. Crystals of compound 6 were monoclinic, space group P2 1/n, a= 1.034 7(4) nm, b=1.396 8(5) nm, c=1.405 6(5) nm, β=95.366(6)°, Z=4; Crystals of compound 8 were monoclinic, space group P2 1/c, a=0.922 9(3) nm, b=1.334 5(5) nm, c= 1.838 5(7) nm, β=93.673(7)°, Z=4.
