Keggin型磷钼、砷钼杂多阴离子无机—有机混配超分子化合物的晶体结构及性质的研究
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摘要
采用中温水热法合成六个Keggin型磷钼、砷钼杂多阴离子无机-有机混配超分子化合物，通过X-单晶衍射得到他们的单晶结构；并利用红外，差热-热重分析等对它们进行表征。
利用Keggin型磷钼杂多阴离子为主体，4-氨基吡啶和3-氨基吡啶为配体合成两个新型无机-有机混配超分子化合物1和化合物2，磷钼杂多阴离子与4-氨基吡啶的配合物(4-C_5H_7N_2)_3(PMo_(12)O_(40))·(4-C_5H_6N_2)·H_2O(1)，属于单斜晶系，C2/c空间群，晶胞参数为：a=11.7094(4)(A|°)，α=90°，b=25.7946(9)(A|°),β=97.2050°，c=16.6748(6)(A|°)，γ=90°，V= 4996.7(3)(A|°)~3，Z=4，R_(gt)(F)= 0.0456，ωR_(ref)(F~2)=0.1419；磷钼杂多阴离子与3-氨基配合物(3-C_5H_7N_2)_3(PMo_(12)O_(40))·2(3-C_5H_6N_2)2·6(H_2O) (2)，属于四方晶系，P42/n空间群，晶胞参数为：a=14.2864(2)(A|°)，α=90°，b=14.2864(2)(A|°),β=90°，c=29.0414(8)(A|°)，γ=90°，V=5927.4(2)(A|°)~3，Z=4，R_(gt)(F)= 0.0575，ωR_(ref)(F~2)=0.1633；配合物1和配合物2通过大量的氢键作用形成三维空间网状超分子结构。
利用Keggin型磷钼杂多阴离子为主体，4-甲基吡啶和3-甲基吡啶为配体合成两个新型无机-有机混配超分子化合物3和化合物4，磷钼杂多阴离子与4-甲基吡啶的配合物(4-C_6H_8N)_3(PMo_(12)O_(40)) (3)，属于单斜晶系，P2(1)/c空间群，晶胞参数为：a = 19.7004(3)(A|°)，α= 90°，b = 14.0785(2)(A|°),β= 91.3590(10)°，c = 33.0209(5)(A|°)，γ= 90°，V= 9155.8(2)(A|°)~3，Z=8，R_(gt)(F)=0.0350，ωR_(ref)(F~2)= 0.0730；磷钼杂多阴离子与3-甲基吡啶的配合物(3-C_6H_8N)_4(PMo_(12)O_(40))·H_2O(4)，属于单斜晶系，C2/c空间群，晶胞参数为：a = 19.4997(4)(A|°)，α= 90°，b = 12.5836(3)(A|°),β= 109.5730(10)°，c =22.5405(5)(A|°)，γ= 90°，V= 5211.3(2)(A|°)~3，Z=4，R_(gt)(F)= 0.0698，ωR_(ref)(F~2)=0.1849；配合物3和配合物4通过大量的氢键作用形成一维无限链状超分子结构。
利用Keggin型磷钼、砷钼杂多阴离子为主体，苯并咪唑为配体合成两个新型无机-有机混配超分子化合物5和化合物6，磷钼杂多阴离子与苯并咪唑的配合物(C_7H_7N_2)_4(PMo_(12)O_(40))·2(H_2O) (5)，属于三斜晶系，P-1空间群，晶胞参数为：a=9.8405(7)(A|°)，α=70.494(5)°，b=11.3588(7)(A|°),β=82.285(5)°，c=13.8561(10)(A|°)，γ=71.161(6)°，V=1381.08(16)(A|°)~3，Z=1，R_(gt)(F)=0.0631，ωR_(ref)(F~2)=0.1392；砷钼杂多阴离子与苯并咪唑超分子配合物(C_7H_7N_2)_3(AsMo_(12)O_(40))·2C_7H_6N_2·3(H_2O) (6)，属于三斜晶系，P-1空间群，晶胞参数为：a = 12.3353(4)(A|°)，α= 95.6630(10)°，b = 13.2649(4)(A|°),β= 100.1720(10)°，c = 20.2878(6)(A|°)，γ= 99.3940(10)°，V= 3195.72(17)(A|°)~3，Z=2，R_(gt)(F)= 0.0329，ωR_(ref)(F~2)= 0.1080。配合物5和配合物6通过大量的氢键作用和弱π-π堆积作用形成一维无限链状超分子结构。
实验结果表明它们都含有Keggin结构杂多酸阴离子，部分有机分子配体以质子化的形式作为抗衡阳离子存在于配合物当中，部分配合物还含有以分子形式存在的有机分子和结晶水。本论文还以催化降减丙酮为探针，对它们的催化性能进行探索研究，阶段性的研究结果表明，配合物3和配合物5具有一定的催化活性，更多更深入的研究还在进行中。
Six Keggin-type phosphormolybdate, arsenicmolybdate polyoxometalatesanion organic-inorganic hybrid supramolecular compounds weresynthsised by hydrothermal methods at moderate temperature and all thecrystal structures were abtained by X-crystal diffraction. They werecharacterized by IR and TG-DTA.
Two new inorganic-organic hybrid supramolecular compound 1 andcompound 2 were synthesised with Keggin-type phosphomolybdate anion asthe main body and 4-aminopyridine or 3-aminopyridine as a ligand. Thecompound (4-C_5H_7N_2)_3(PMo_(12)O_(40))·(4-C_5H_6N_2)·H_2O (1) was consisted ofphosphormolybdate anion and 4-aminopyridine was crystallized in themonoclinic, space group: C2/c, a=11.7094(4)(A|°),α=90°, b=25.7946(9)(A|°),β=97.2050°, c=16.6748(6)(A|°),γ=90°, V= 4996.7(3)(A|°)~3, Z=4, R_(gt)(F)=0.0456,ωR_(ref)(F~2)=0.142.The compound (3-C_5H_7N_2)_3(PMo_(12)O_(40))·4(3-C5H6N2)·6H_2O(2) consisted of phosphormolybdate and 3-aminopyridine was crystallizedin the tetragonal, space group: P42/n, a=14.2864(2)(A|°),α=90°, b=14.2864(A|°),β=90°, c=29.0414(8)(A|°),γ=90°, V=5927.4(2)(A|°)~3, Z=4, R_(gt)(F)=0.0575,ωR_(ref)(F~2)=0.1633. Both of compound 1 and compound 2 were formedinfinite three-dimensional framework via lots of hydrogen-bonds.
Two new inorganic-organic hybrid supramolecular compound 3 andcompound 4 were synthesised with Keggin-type phosphomolybdate anion asthe main body and 4-picoline or 3-picoline as a ligand. The compound(4-C_6H_8N)_3(PMo_(12)O_(40)) (3) was consisted of phosphormolybdate and4-picoline was crystallized in the monoclinic, space group: P2(1)/c, a =19.7004(3)(A|°),α= 90°, b = 14.0785(2)(A|°),β= 91.3590(10)°, c = 33.0209(5)(A|°),γ= 90°, V= 9155.8(2)(A|°)~3, Z=8, R_(gt)(F)= 0.0350,ωR_(ref)(F~2)= 0.0730. Thecompound (3-C_6H_8N)_4(PMo_(12)O_(40))·H_2O(4) consisted of phosphormolybdateand 3-picoline was crystallized in the monoclinic, space group: C2/c, a =19.4997(4)(A|°),α= 90°, b = 12.5836(3)(A|°),β= 109.5730(10)°, c = 22.5405(5)(A|°),γ= 90°, V= 5211.3(2)(A|°)~3, Z=4, R_(gt)(F)= 0.0698,ωR_(ref)(F~2)= 0.1849. Bothof compound 3 and compound 4 were formed infinite one-dimensional chainvia lots of hydrogen-bonds.
Two new inorganic-organic hybrid supramolecular compound 5 andcompound 6 were synthesised with Keggin-type phosphomolybdate anion or arsenicmolybdate anion as the main body and benzimidazole as a ligand.The compound (C_7H_7N_2)_4(PMo_(12)O_(40))·2H_2O (5) consisted of phosphormolybdateand benzimidazole was crystallized in the triclinic, space group:P-1, a=9.8405(7)(A|°),α=70.494(5)°, b=11.3588(7)(A|°),β=82.285(5)°,c=13.8561(10)(A|°),γ=71.161(6)°, V=1381.08(16)(A|°)~3, Z=1, R_(gt)(F)=0.0631,ωR_(ref)(F~2)=0.1392. The compound (C_7H_7N_2)_3(AsMo_(12)O_(40))·2C_7H_6N_2·3H_2O (6)consisted of arsenicmolybdate and benzimidazole was crystallized in thetriclinic, space group: P-1, a = 12.3353(4)(A|°),α= 95.6630(10)°, b =13.2649(4)(A|°),β= 100.1720(10)°, c = 20.2878(6)(A|°),γ= 99.3940(10)°, V=3195.72(17)(A|°)~3, Z=2, R_(gt)(F)= 0.0329,ωR_(ref)(F~2)= 0.1080. Both of compound5 and compound 6 were formed infinite one-dimensional chain via lots ofhydrogen-bonds and weakπ-πstacking action.
The results indicate that they all contain Keggin structure heteropolyacid anion, some of the organic ligand protonated as the counter cation werepresent in these compounds, some organic molecules and water moleculesnot protonated were also contained in some of these compounds. In thispaper, catalytic reduction of acetone as a probe was researched to exploratethe catalytic properties of these compounds, the stage results showed thatcomplound 3 and compound 5 have some catalytic activity, further researchis still in progress.
利用Keggin型磷钼杂多阴离子为主体，4-氨基吡啶和3-氨基吡啶为配体合成两个新型无机-有机混配超分子化合物1和化合物2，磷钼杂多阴离子与4-氨基吡啶的配合物(4-C_5H_7N_2)_3(PMo_(12)O_(40))·(4-C_5H_6N_2)·H_2O(1)，属于单斜晶系，C2/c空间群，晶胞参数为：a=11.7094(4)(A|°)，α=90°，b=25.7946(9)(A|°),β=97.2050°，c=16.6748(6)(A|°)，γ=90°，V= 4996.7(3)(A|°)~3，Z=4，R_(gt)(F)= 0.0456，ωR_(ref)(F~2)=0.1419；磷钼杂多阴离子与3-氨基配合物(3-C_5H_7N_2)_3(PMo_(12)O_(40))·2(3-C_5H_6N_2)2·6(H_2O) (2)，属于四方晶系，P42/n空间群，晶胞参数为：a=14.2864(2)(A|°)，α=90°，b=14.2864(2)(A|°),β=90°，c=29.0414(8)(A|°)，γ=90°，V=5927.4(2)(A|°)~3，Z=4，R_(gt)(F)= 0.0575，ωR_(ref)(F~2)=0.1633；配合物1和配合物2通过大量的氢键作用形成三维空间网状超分子结构。
利用Keggin型磷钼杂多阴离子为主体，4-甲基吡啶和3-甲基吡啶为配体合成两个新型无机-有机混配超分子化合物3和化合物4，磷钼杂多阴离子与4-甲基吡啶的配合物(4-C_6H_8N)_3(PMo_(12)O_(40)) (3)，属于单斜晶系，P2(1)/c空间群，晶胞参数为：a = 19.7004(3)(A|°)，α= 90°，b = 14.0785(2)(A|°),β= 91.3590(10)°，c = 33.0209(5)(A|°)，γ= 90°，V= 9155.8(2)(A|°)~3，Z=8，R_(gt)(F)=0.0350，ωR_(ref)(F~2)= 0.0730；磷钼杂多阴离子与3-甲基吡啶的配合物(3-C_6H_8N)_4(PMo_(12)O_(40))·H_2O(4)，属于单斜晶系，C2/c空间群，晶胞参数为：a = 19.4997(4)(A|°)，α= 90°，b = 12.5836(3)(A|°),β= 109.5730(10)°，c =22.5405(5)(A|°)，γ= 90°，V= 5211.3(2)(A|°)~3，Z=4，R_(gt)(F)= 0.0698，ωR_(ref)(F~2)=0.1849；配合物3和配合物4通过大量的氢键作用形成一维无限链状超分子结构。
利用Keggin型磷钼、砷钼杂多阴离子为主体，苯并咪唑为配体合成两个新型无机-有机混配超分子化合物5和化合物6，磷钼杂多阴离子与苯并咪唑的配合物(C_7H_7N_2)_4(PMo_(12)O_(40))·2(H_2O) (5)，属于三斜晶系，P-1空间群，晶胞参数为：a=9.8405(7)(A|°)，α=70.494(5)°，b=11.3588(7)(A|°),β=82.285(5)°，c=13.8561(10)(A|°)，γ=71.161(6)°，V=1381.08(16)(A|°)~3，Z=1，R_(gt)(F)=0.0631，ωR_(ref)(F~2)=0.1392；砷钼杂多阴离子与苯并咪唑超分子配合物(C_7H_7N_2)_3(AsMo_(12)O_(40))·2C_7H_6N_2·3(H_2O) (6)，属于三斜晶系，P-1空间群，晶胞参数为：a = 12.3353(4)(A|°)，α= 95.6630(10)°，b = 13.2649(4)(A|°),β= 100.1720(10)°，c = 20.2878(6)(A|°)，γ= 99.3940(10)°，V= 3195.72(17)(A|°)~3，Z=2，R_(gt)(F)= 0.0329，ωR_(ref)(F~2)= 0.1080。配合物5和配合物6通过大量的氢键作用和弱π-π堆积作用形成一维无限链状超分子结构。
实验结果表明它们都含有Keggin结构杂多酸阴离子，部分有机分子配体以质子化的形式作为抗衡阳离子存在于配合物当中，部分配合物还含有以分子形式存在的有机分子和结晶水。本论文还以催化降减丙酮为探针，对它们的催化性能进行探索研究，阶段性的研究结果表明，配合物3和配合物5具有一定的催化活性，更多更深入的研究还在进行中。
Six Keggin-type phosphormolybdate, arsenicmolybdate polyoxometalatesanion organic-inorganic hybrid supramolecular compounds weresynthsised by hydrothermal methods at moderate temperature and all thecrystal structures were abtained by X-crystal diffraction. They werecharacterized by IR and TG-DTA.
Two new inorganic-organic hybrid supramolecular compound 1 andcompound 2 were synthesised with Keggin-type phosphomolybdate anion asthe main body and 4-aminopyridine or 3-aminopyridine as a ligand. Thecompound (4-C_5H_7N_2)_3(PMo_(12)O_(40))·(4-C_5H_6N_2)·H_2O (1) was consisted ofphosphormolybdate anion and 4-aminopyridine was crystallized in themonoclinic, space group: C2/c, a=11.7094(4)(A|°),α=90°, b=25.7946(9)(A|°),β=97.2050°, c=16.6748(6)(A|°),γ=90°, V= 4996.7(3)(A|°)~3, Z=4, R_(gt)(F)=0.0456,ωR_(ref)(F~2)=0.142.The compound (3-C_5H_7N_2)_3(PMo_(12)O_(40))·4(3-C5H6N2)·6H_2O(2) consisted of phosphormolybdate and 3-aminopyridine was crystallizedin the tetragonal, space group: P42/n, a=14.2864(2)(A|°),α=90°, b=14.2864(A|°),β=90°, c=29.0414(8)(A|°),γ=90°, V=5927.4(2)(A|°)~3, Z=4, R_(gt)(F)=0.0575,ωR_(ref)(F~2)=0.1633. Both of compound 1 and compound 2 were formedinfinite three-dimensional framework via lots of hydrogen-bonds.
Two new inorganic-organic hybrid supramolecular compound 3 andcompound 4 were synthesised with Keggin-type phosphomolybdate anion asthe main body and 4-picoline or 3-picoline as a ligand. The compound(4-C_6H_8N)_3(PMo_(12)O_(40)) (3) was consisted of phosphormolybdate and4-picoline was crystallized in the monoclinic, space group: P2(1)/c, a =19.7004(3)(A|°),α= 90°, b = 14.0785(2)(A|°),β= 91.3590(10)°, c = 33.0209(5)(A|°),γ= 90°, V= 9155.8(2)(A|°)~3, Z=8, R_(gt)(F)= 0.0350,ωR_(ref)(F~2)= 0.0730. Thecompound (3-C_6H_8N)_4(PMo_(12)O_(40))·H_2O(4) consisted of phosphormolybdateand 3-picoline was crystallized in the monoclinic, space group: C2/c, a =19.4997(4)(A|°),α= 90°, b = 12.5836(3)(A|°),β= 109.5730(10)°, c = 22.5405(5)(A|°),γ= 90°, V= 5211.3(2)(A|°)~3, Z=4, R_(gt)(F)= 0.0698,ωR_(ref)(F~2)= 0.1849. Bothof compound 3 and compound 4 were formed infinite one-dimensional chainvia lots of hydrogen-bonds.
Two new inorganic-organic hybrid supramolecular compound 5 andcompound 6 were synthesised with Keggin-type phosphomolybdate anion or arsenicmolybdate anion as the main body and benzimidazole as a ligand.The compound (C_7H_7N_2)_4(PMo_(12)O_(40))·2H_2O (5) consisted of phosphormolybdateand benzimidazole was crystallized in the triclinic, space group:P-1, a=9.8405(7)(A|°),α=70.494(5)°, b=11.3588(7)(A|°),β=82.285(5)°,c=13.8561(10)(A|°),γ=71.161(6)°, V=1381.08(16)(A|°)~3, Z=1, R_(gt)(F)=0.0631,ωR_(ref)(F~2)=0.1392. The compound (C_7H_7N_2)_3(AsMo_(12)O_(40))·2C_7H_6N_2·3H_2O (6)consisted of arsenicmolybdate and benzimidazole was crystallized in thetriclinic, space group: P-1, a = 12.3353(4)(A|°),α= 95.6630(10)°, b =13.2649(4)(A|°),β= 100.1720(10)°, c = 20.2878(6)(A|°),γ= 99.3940(10)°, V=3195.72(17)(A|°)~3, Z=2, R_(gt)(F)= 0.0329,ωR_(ref)(F~2)= 0.1080. Both of compound5 and compound 6 were formed infinite one-dimensional chain via lots ofhydrogen-bonds and weakπ-πstacking action.
The results indicate that they all contain Keggin structure heteropolyacid anion, some of the organic ligand protonated as the counter cation werepresent in these compounds, some organic molecules and water moleculesnot protonated were also contained in some of these compounds. In thispaper, catalytic reduction of acetone as a probe was researched to exploratethe catalytic properties of these compounds, the stage results showed thatcomplound 3 and compound 5 have some catalytic activity, further researchis still in progress.
引文
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