Synthesis, Structures and Characterization of Two New Pb<sup>II</sup> Polymers Built on a Kinked Flexible Thiodiacetic acid Ligand

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摘要 Two new Pb^II metal-organic coordination polymers, namely, [Pb(tda)]_n (1) and [Pb(tda)(phen)]_n (2) (H₂tda = thiodiglycolic acid, phen = 1,10-phenanthroline), were synthesized under hydrothermal conditions and characterized by elemental analysis, IR, UV spectra, TG technique and X-ray crystallography. Complex 1 crystallizes in the orthorhombic system, space group Iba2 with α = 9.0417(14), b = 19.360(4), c = 7.5741(12) Å, C₄H₄O₄PbS, M_r = 355.32, V = 1325.8(4) Å³, D_c = 3.560 g·cm^-3, F(000) = 1264, μ(MoKa) = 25.711 mm^-1, S = 1.086 and Z = 8. The final refinement gave R = 0.0387 and wR = 0.0986 for 3077 observed reflections with I > 2σ(I). Complex 1 is a 2D infinite grid-like (4,4) topological structure constructed by Pb^II atoms and tda anions, in which tda ligands exhibit bis(syn, syn-bridging bidentate, chelating-bridging tetradentate) mode. Complex 2 crystallizes in the triclinic system, space group Pī with α = 8.3570(17), b = 8.7591(18), c = 10.895(2) Å, α = 76.00(3), β = 80.50(3), γ = 77.61(3)°, C₁₆H₁₂N₂O₄PbS, M_r = 535.53, V = 750.4(3) Å³, D_c = 2.370 g·cm^-3, F(000) = 504, μ(MoKa) = 11.405 mm^-1, S = 1.018 and Z = 2. The final refinement gave R = 0.0332 and wR = 0.0629 for 3360 observed reflections with I > 2σ(I). Complex 2 is a 1D chain structure, in which phen ligands are attached on both sides of the 1D chain and tda ligand exhibits a bis(syn, syn-bridging bidentate, chelating tridentate) mode. Finally, complex 2 is extended into a 2D supramolecular structure by strong π···π stacking interactions.

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	侯向阳
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关键词 ： lead, thiodiacetic acids, crystal structure, characterization

Abstract：Two new Pb^II metal-organic coordination polymers, namely, [Pb(tda)]_n (1) and [Pb(tda)(phen)]_n (2) (H₂tda = thiodiglycolic acid, phen = 1,10-phenanthroline), were synthesized under hydrothermal conditions and characterized by elemental analysis, IR, UV spectra, TG technique and X-ray crystallography. Complex 1 crystallizes in the orthorhombic system, space group Iba2 with α= 9.0417(14), b = 19.360(4), c = 7.5741(12) Å, C₄H₄O₄PbS, M_r = 355.32, V = 1325.8(4) Å³, D_c = 3.560 g·cm^-3, F(000) = 1264, μ(MoKa) = 25.711 mm^-1, S = 1.086 and Z = 8. The final refinement gave R = 0.0387 and wR = 0.0986 for 3077 observed reflections with I > 2σ(I). Complex 1 is a 2D infinite grid-like (4,4) topological structure constructed by Pb^II atoms and tda anions, in which tda ligands exhibit bis(syn, syn-bridging bidentate, chelating-bridging tetradentate) mode. Complex 2 crystallizes in the triclinic system, space group Pī with α = 8.3570(17), b = 8.7591(18), c = 10.895(2) Å, α = 76.00(3), β = 80.50(3), γ = 77.61(3)°, C₁₆H₁₂N₂O₄PbS, M_r = 535.53, V = 750.4(3) Å³, D_c = 2.370 g·cm^-3, F(000) = 504, μ(MoKa) = 11.405 mm^-1, S = 1.018 and Z = 2. The final refinement gave R = 0.0332 and wR = 0.0629 for 3360 observed reflections with I > 2σ(I). Complex 2 is a 1D chain structure, in which phen ligands are attached on both sides of the 1D chain and tda ligand exhibits a bis(syn, syn-bridging bidentate, chelating tridentate) mode. Finally, complex 2 is extended into a 2D supramolecular structure by strong π···π stacking interactions.

Key words： lead thiodiacetic acids crystal structure characterization

收稿日期: 2013-01-22 出版日期: 2013-09-25

基金资助: Supported by Scientific Research Program Funded by Shaanxi Provincial Education Department (No. 11JK0583)

通讯作者: 侯向阳 E-mail: wx2248@126.com

作者简介: 侯向阳: wx2248@126.com

引用本文:

侯向阳;王潇;付峰;王记江. Synthesis, Structures and Characterization of Two New Pb^II Polymers Built on a Kinked Flexible Thiodiacetic acid Ligand[J]. 结构化学, 2013, 32(9): 1339-1347.
HOU Xiang-Yang;WANG Xiao;FU Feng;WANG Ji-Jiang. Synthesis, Structures and Characterization of Two New Pb^II Polymers Built on a Kinked Flexible Thiodiacetic acid Ligand. CHINESE JOURNAL OF STRUCTURAL CHEMISTRY, 2013, 32(9): 1339-1347.

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http://manu30.magtech.com.cn/jghx/CN/ 或 http://manu30.magtech.com.cn/jghx/CN/Y2013/V32/I9/1339

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