1,4-Benzenedisulfonic acid (H2BDS) as terephthalic acid analogue for the preparation of coordination polymers: the examples of M(BDS)(NMP)3 (M = Mn, Fe, Co; NMP = N-methylpyrrolidone)

1,4-Benzenedisulfonic acid (H2BDS) as terephthalic acid analogue for the preparation of coordination polymers: the examples of M(BDS)(NMP)3 (M = Mn, Fe, Co; NMP = N-methylpyrrolidone)
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1,4-苯二磺酸 (H2BDS) 作为对苯二甲酸类似物,用于制备配位聚合物:M(BDS)(NMP)3 的示例(M = Mn、Fe、Co;NMP = N-甲基吡咯烷酮)

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发表时间:
2015
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通讯作者:
M. Wickleder
M. Wickleder
中科院分区:
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文献类型:
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作者:
Christina Zitzer;Thomas W. T. Muesmann;J. Christoffers;M. Wickleder

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以N-甲基吡咯烷酮(NMP)为溶剂,1,4-苯二磺酸(H2 BDS)分别与锰、铁、钴的盐进行溶剂热反应,合成了新的二磺酸盐M(BDS)(NMP)3(M = Mn,Fe,Co)。同型化合物结晶具有三斜对称性(P,Z = 2; M = Mn:a = 916.84(3)pm,B = 965.57(3)pm,c = 1437.87(5)pm,α = 95.297(2)°,β = 97.834(2)°,γ = 92.576(2)°,R1/wR2(I0 > 2σ(I0))= 0.0300/0.0701; M = Fe:a = 911.98(5)pm,B = 960.75(5)pm,c = 1432.41(8)pm,α = 94.951(2)°,β = 98.050(3)°,γ = 92.029(2)°,R1/wR2(I0 > 2σ(I0))= 0.0238/0.0689; M = Co:a = 911.3(1)pm,B = 959.5(1)pm,c = 1428.6(2)pm,α = 94.791(5)°,β = 98.229(5)°,γ = 91.873(6)°,R1/wR2(I0 > 2σ(I0))= 0.0264/0.0684)。在晶体结构中,Mn ~(2+)、Fe ~(2+)和Co ~(2+)以八面体氧配位的方式与三个单齿二磺酸基和三个NMP分子配位。二磺酸基团将金属离子连接成无限层。热分析研究表明,化合物的去溶剂化发生在50 °C和330 °C之间的温度范围内。无溶剂的磺酸盐显示出高达近500 °C的显著高稳定性。通过DSC/TG测量和X射线粉末衍射研究了其热行为。
The solvothermal reactions of 1,4-benzenedisulfonic acid, H2BDS, with suitable salts of manganese, iron, and cobalt led to the new disulfonates M(BDS)(NMP)3 (M = Mn, Fe, Co), when N-methylpyrrolidone (NMP) was used as the solvent. The isotypic compounds crystallize with triclinic symmetry (P, Z = 2; M = Mn: a = 916.84(3) pm, b = 965.57(3) pm, c = 1437.87(5) pm, α = 95.297(2)°, β = 97.834(2)°, γ = 92.576(2)°, R1/wR2(I0 > 2σ(I0)) = 0.0300/0.0701; M = Fe: a = 911.98(5) pm, b = 960.75(5) pm, c = 1432.41(8) pm, α = 94.951(2)°, β = 98.050(3)°, γ = 92.029(2)°, R1/wR2(I0 > 2σ(I0)) = 0.0238/0.0689; M = Co: a = 911.3(1) pm, b = 959.5(1) pm, c = 1428.6(2) pm, α = 94.791(5)°, β = 98.229(5)°, γ = 91.873(6)°, R1/wR2(I0 > 2σ(I0)) = 0.0264/0.0684). In the crystal structure, the M2+ ions (Mn2+, Fe2+ and Co2+) are in octahedral oxygen coordination of three monodentate disulfonate groups and three NMP molecules. The disulfonate groups link the metal ions into infinite layers. Thermoanalytical investigations showed that the desolvation of the compounds occurred in a temperature range between 50 °C and 330 °C. The solvent free sulfonates showed remarkable high stabilities up to nearly 500 °C. The thermal behaviour was investigated by DSC/TG measurements and X-ray powder diffraction.