基于钼八阴离子构筑的无机有机杂化材料的合成、结构和性质研究
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摘要
多酸簇具有无与伦比的物理和化学性质,可作为构筑新颖多样功能材料的一类基本无机建筑块。本论文的工作主要是设计合成基于八钼酸盐的无机有机杂化化合物。我们分别采用“一锅法”和步控式分步合成方法合成20个化合物,这些化合物可潜在应用于具有半导体性质或者发光性质的材料。另外,我们利用元素分析、红外光谱、热重分析、紫外可见光谱、荧光光谱来表征这些化合物。
1.在水热条件下,我们利用“一锅法”将(NH_4)_6Mo_7O_(24)·6H_2O和有机配体还有过渡金属离子混合合成12个过渡金属化合物修饰的八钼酸盐杂化材料。Cu~II(HL~1)_2(H_2O)_2(Mo_8O_(26)) (1) Cu~II(L~1)_2(Mo_8O_(26))_(0.5) (2) Ni~II(HL~2)_2(H_2O)_2(β-Mo_8O_(26)) (3) [Cu~II(HL~2)_2(Mo_8O_(26))]·2H_2O (4) [Cu_2~II(L~2)_4(Mo_8O_(26))]·3H_2O (5) Cu_3~I(L~2)_2(Mo_8O_(26))_(0.5)Cl (6) Cu_4~I(L~2)_4(Mo_8O_(26)) (7) Cu_2~II(L3)_4(Mo_8O_(26)) (8) [Zn(HL~4)_2(H_2O)(Mo_8O_(26))]-2H_2O (9) Cu_2~II(HL~4)_4(Mo_8O_(26))_2 (10) [Cu~IIL~4(H_2O)(Mo_8O_(26))_(0.5)]·2H_2O (11) [Cu~IIL~4(H_2O)(Mo_8O_(26))_(0.5)]·2H_2O (12)单晶X射线表明除了化合物2和12的多酸阴离子呈θ或γ构型,其他化合物中均呈β构型的过渡金属化合物修饰八钼酸盐形成无机有机杂化化合物。紫外可见漫反射光谱表明含有CuI的化合物含有较低禁带宽度,而且有发光性质。并且,化合物6还具有光导性质。
2.我们合成了三个新颖的共存不同同分异构体或不同构型多钼酸盐的化合物。{[Ni(Mo_8O_(26))(H_2L~5)_2(H_2O)](Mo_8O_(26))(H_2L~5)}·2H_2O (13) {[Co(Mo_8O_(26))(H_2L~5)_2(H_2O)](Mo_8O_(26))[Co(H_2O)_6]}·6H_2O (14) [CuI_6L_(24)(Mo_8O_(26))(Mo_6O_(19))] (15)晶体结构分析表明化合物13是一个共存γ-[Mo_8O_(26)N_2]和γ-[Mo_8O_(28)]的1D+1D超分子结构;化合物14中共存γ-[Mo_8O_(26)]~(4-)和β-[Mo_8O_(26)]~(4-)阴离子;化合物15中既包含β-[Mo_8O_(26)]~(4-)也包含[Mo_6O_(19)]~(2-)。量子化学计算结果表明,在溶液中,从β-[Mo_8O_(26)]~(4-)转化为[Mo_6O_(19)]~(2-)是自发过程。化合物15的禁带宽度为1.69 eV。
3.我们采用“自下而上”策略,步控式合成了5个八钼酸盐均为γ构型的无机有机杂化化合物。[(H_2L~2)_2(Mo_8O_(26))]·4H_2O (16) [Cu_2~I(L~2)_3(Mo_8O_(26))_(0.5)] (17) [(H_2BIMB)(BIMB)_(0.5)(Mo_8O_(26))_(0.5)]·H_2O (18) [Ni(L~2)_2(HBIMB)_2(Mo_8O_(26))]·4H_2O (19) [Zn(BIMB)_2(Mo_8O_(26))_(0.5)] (20)在这五个化合物中,化合物16和18是设计的合成子,作为合成新化合物合成的前驱体,当加入金属离子对前驱体后修饰即得到化合物17、19、20。
Polyoxometalate (POM) clusters have an unparalleled range of physical and chemical properties, acting as a set of versatile inorganic building blocks that can be reliably utilized in the formation of new materials. Our work is focused on the design and preparation of octamolybdate-based inorganic-organic hybrid materials. We have employed“one-pot”synthetic method and step-wise“bottom-up”synthetic strategy to synthesize twenty compounds with potential applications in semiconducting and photoluminescent materials. Furthermore, the compounds were characterized by elemental analysis, FT-IR, TGA, UV-vis spectra, fluorescence spectrometry.
1. Under hydrothermal conditions, we employ the“one-pot”method to synthesize twelve transition-metal complex-modified octamolybdate hybrid materials by mixing (NH_4)_6Mo_7O_(24)·6H_2O, organic ligands (L~1 = 3-((1H-imidazol-1-yl)methyl)pyridine; L~2 = 3-((1H-1,2,4-triazol-1-yl)methyl)pyridine; L3 = 2-(2-Pyridyl)imidazole and L4 = 2-(1-(Pyridine-3-ylmethyl)-1H-imidazol-2-yl)pyridine) and transition metals (Cu, Ni, Zn). Cu~II(HL~1)_2(H_2O)_2(Mo_8O_(26)) (1) Cu~II(L~1)_2(Mo_8O_(26))_(0.5) (2) Ni~II(HL~2)_2(H_2O)_2(β-Mo_8O_(26)) (3) [Cu~II(HL~2)_2(Mo_8O_(26))]·2H_2O (4) [Cu_2~II(L~2)_4(Mo_8O_(26))]·3H_2O (5) Cu_3~I(L~2)_2(Mo_8O_(26))_(0.5)Cl (6) Cu_4~I(L~2)_4(Mo_8O_(26)) (7) Cu_2~II(L3)_4(Mo_8O_(26)) (8) [Zn(HL~4)_2(H_2O)(Mo_8O_(26))]-2H_2O (9) Cu_2~II(HL~4)_4(Mo_8O_(26))_2 (10) [Cu~IIL~4(H_2O)(Mo_8O_(26))_(0.5)]·2H_2O (11) [Cu~IIL~4(H_2O)(Mo_8O_(26))_(0.5)]·2H_2O (12) Single crystal X–ray diffraction results reveal that all the polyanions exhibitβisomer except thatθorγisomers in 2 and 12 respectively. The octamolybdate anions are modified by transition-metal complexes. The UV-vis reflectance spectra reveal that the compounds containing CuI ions not only have lower optical band gaps but also photoluminescent property. More interestingly,compound 6 is photoconductive.
2. Three novel compounds coexisting different isomers or forms of polymolybdate have been successfully synthesized. {[Ni(Mo_8O_(26))(H_2L~1)_2(H_2O)](Mo_8O_(26))(H_2L~1)}·2H_2O (13) {[Co(Mo_8O_(26))(H_2L~1)_2(H_2O)](Mo_8O_(26))[Co(H_2O)_6]}·6H_2O (14) [CuI_6L_(24)(Mo_8O_(26))(Mo_6O_(19))] (15) Crystal structure analysis reveals that 13 is a 1D+1D supramolecular structure coexisting bothγ-[Mo_8O_(26)N_2] andγ-[Mo_8O_(28)] units; 14 hasγ-[Mo_8O_(26)]~(4-) as well asβ-[Mo_8O_(26)]~(4-) anions and 15 is a (3,4,6)-connected 2D network containing bothβ-[Mo_8O_(26)]~(4-) and [Mo_6O_(19)]~(2-) anions. According to quantum chemical calculations,the transformation fromβ-[Mo_8O_(26)]~(4-) to [Mo_6O_(19)]~(2-) is spontaneous in aqueous solution. Compound 15 shows a relatively lower optical band gap 1.69 eV.
3. We have successfully explored the“bottom-up”strategy to step-wisely synthesize five compounds with octamolybdate anion exhibitingγisomer. [(H_2L~1)_2(Mo_8O_(26))]·4H_2O (16) [Cu_2~I(L~1)_3(Mo_8O_(26))_(0.5)] (17) [(H_2BIMB)(BIMB)_(0.5)(Mo_8O_(26))_(0.5)]·H_2O (18) [Ni(BIMB)_2(HBIMB)_2(Mo_8O_(26))]·4H_2O (19) [Zn(BIMB)_2(Mo_8O_(26))_(0.5)] (20) Among them,compounds 16 and 18 are the designed synthons which act as precursors for the formation of compounds 17,19,20 which were obtained by post-modifying the synthons with metal ions. The optical band gap property for the five compounds and the photoluminescence of 20 were also investigeted.
1.在水热条件下,我们利用“一锅法”将(NH_4)_6Mo_7O_(24)·6H_2O和有机配体还有过渡金属离子混合合成12个过渡金属化合物修饰的八钼酸盐杂化材料。Cu~II(HL~1)_2(H_2O)_2(Mo_8O_(26)) (1) Cu~II(L~1)_2(Mo_8O_(26))_(0.5) (2) Ni~II(HL~2)_2(H_2O)_2(β-Mo_8O_(26)) (3) [Cu~II(HL~2)_2(Mo_8O_(26))]·2H_2O (4) [Cu_2~II(L~2)_4(Mo_8O_(26))]·3H_2O (5) Cu_3~I(L~2)_2(Mo_8O_(26))_(0.5)Cl (6) Cu_4~I(L~2)_4(Mo_8O_(26)) (7) Cu_2~II(L3)_4(Mo_8O_(26)) (8) [Zn(HL~4)_2(H_2O)(Mo_8O_(26))]-2H_2O (9) Cu_2~II(HL~4)_4(Mo_8O_(26))_2 (10) [Cu~IIL~4(H_2O)(Mo_8O_(26))_(0.5)]·2H_2O (11) [Cu~IIL~4(H_2O)(Mo_8O_(26))_(0.5)]·2H_2O (12)单晶X射线表明除了化合物2和12的多酸阴离子呈θ或γ构型,其他化合物中均呈β构型的过渡金属化合物修饰八钼酸盐形成无机有机杂化化合物。紫外可见漫反射光谱表明含有CuI的化合物含有较低禁带宽度,而且有发光性质。并且,化合物6还具有光导性质。
2.我们合成了三个新颖的共存不同同分异构体或不同构型多钼酸盐的化合物。{[Ni(Mo_8O_(26))(H_2L~5)_2(H_2O)](Mo_8O_(26))(H_2L~5)}·2H_2O (13) {[Co(Mo_8O_(26))(H_2L~5)_2(H_2O)](Mo_8O_(26))[Co(H_2O)_6]}·6H_2O (14) [CuI_6L_(24)(Mo_8O_(26))(Mo_6O_(19))] (15)晶体结构分析表明化合物13是一个共存γ-[Mo_8O_(26)N_2]和γ-[Mo_8O_(28)]的1D+1D超分子结构;化合物14中共存γ-[Mo_8O_(26)]~(4-)和β-[Mo_8O_(26)]~(4-)阴离子;化合物15中既包含β-[Mo_8O_(26)]~(4-)也包含[Mo_6O_(19)]~(2-)。量子化学计算结果表明,在溶液中,从β-[Mo_8O_(26)]~(4-)转化为[Mo_6O_(19)]~(2-)是自发过程。化合物15的禁带宽度为1.69 eV。
3.我们采用“自下而上”策略,步控式合成了5个八钼酸盐均为γ构型的无机有机杂化化合物。[(H_2L~2)_2(Mo_8O_(26))]·4H_2O (16) [Cu_2~I(L~2)_3(Mo_8O_(26))_(0.5)] (17) [(H_2BIMB)(BIMB)_(0.5)(Mo_8O_(26))_(0.5)]·H_2O (18) [Ni(L~2)_2(HBIMB)_2(Mo_8O_(26))]·4H_2O (19) [Zn(BIMB)_2(Mo_8O_(26))_(0.5)] (20)在这五个化合物中,化合物16和18是设计的合成子,作为合成新化合物合成的前驱体,当加入金属离子对前驱体后修饰即得到化合物17、19、20。
Polyoxometalate (POM) clusters have an unparalleled range of physical and chemical properties, acting as a set of versatile inorganic building blocks that can be reliably utilized in the formation of new materials. Our work is focused on the design and preparation of octamolybdate-based inorganic-organic hybrid materials. We have employed“one-pot”synthetic method and step-wise“bottom-up”synthetic strategy to synthesize twenty compounds with potential applications in semiconducting and photoluminescent materials. Furthermore, the compounds were characterized by elemental analysis, FT-IR, TGA, UV-vis spectra, fluorescence spectrometry.
1. Under hydrothermal conditions, we employ the“one-pot”method to synthesize twelve transition-metal complex-modified octamolybdate hybrid materials by mixing (NH_4)_6Mo_7O_(24)·6H_2O, organic ligands (L~1 = 3-((1H-imidazol-1-yl)methyl)pyridine; L~2 = 3-((1H-1,2,4-triazol-1-yl)methyl)pyridine; L3 = 2-(2-Pyridyl)imidazole and L4 = 2-(1-(Pyridine-3-ylmethyl)-1H-imidazol-2-yl)pyridine) and transition metals (Cu, Ni, Zn). Cu~II(HL~1)_2(H_2O)_2(Mo_8O_(26)) (1) Cu~II(L~1)_2(Mo_8O_(26))_(0.5) (2) Ni~II(HL~2)_2(H_2O)_2(β-Mo_8O_(26)) (3) [Cu~II(HL~2)_2(Mo_8O_(26))]·2H_2O (4) [Cu_2~II(L~2)_4(Mo_8O_(26))]·3H_2O (5) Cu_3~I(L~2)_2(Mo_8O_(26))_(0.5)Cl (6) Cu_4~I(L~2)_4(Mo_8O_(26)) (7) Cu_2~II(L3)_4(Mo_8O_(26)) (8) [Zn(HL~4)_2(H_2O)(Mo_8O_(26))]-2H_2O (9) Cu_2~II(HL~4)_4(Mo_8O_(26))_2 (10) [Cu~IIL~4(H_2O)(Mo_8O_(26))_(0.5)]·2H_2O (11) [Cu~IIL~4(H_2O)(Mo_8O_(26))_(0.5)]·2H_2O (12) Single crystal X–ray diffraction results reveal that all the polyanions exhibitβisomer except thatθorγisomers in 2 and 12 respectively. The octamolybdate anions are modified by transition-metal complexes. The UV-vis reflectance spectra reveal that the compounds containing CuI ions not only have lower optical band gaps but also photoluminescent property. More interestingly,compound 6 is photoconductive.
2. Three novel compounds coexisting different isomers or forms of polymolybdate have been successfully synthesized. {[Ni(Mo_8O_(26))(H_2L~1)_2(H_2O)](Mo_8O_(26))(H_2L~1)}·2H_2O (13) {[Co(Mo_8O_(26))(H_2L~1)_2(H_2O)](Mo_8O_(26))[Co(H_2O)_6]}·6H_2O (14) [CuI_6L_(24)(Mo_8O_(26))(Mo_6O_(19))] (15) Crystal structure analysis reveals that 13 is a 1D+1D supramolecular structure coexisting bothγ-[Mo_8O_(26)N_2] andγ-[Mo_8O_(28)] units; 14 hasγ-[Mo_8O_(26)]~(4-) as well asβ-[Mo_8O_(26)]~(4-) anions and 15 is a (3,4,6)-connected 2D network containing bothβ-[Mo_8O_(26)]~(4-) and [Mo_6O_(19)]~(2-) anions. According to quantum chemical calculations,the transformation fromβ-[Mo_8O_(26)]~(4-) to [Mo_6O_(19)]~(2-) is spontaneous in aqueous solution. Compound 15 shows a relatively lower optical band gap 1.69 eV.
3. We have successfully explored the“bottom-up”strategy to step-wisely synthesize five compounds with octamolybdate anion exhibitingγisomer. [(H_2L~1)_2(Mo_8O_(26))]·4H_2O (16) [Cu_2~I(L~1)_3(Mo_8O_(26))_(0.5)] (17) [(H_2BIMB)(BIMB)_(0.5)(Mo_8O_(26))_(0.5)]·H_2O (18) [Ni(BIMB)_2(HBIMB)_2(Mo_8O_(26))]·4H_2O (19) [Zn(BIMB)_2(Mo_8O_(26))_(0.5)] (20) Among them,compounds 16 and 18 are the designed synthons which act as precursors for the formation of compounds 17,19,20 which were obtained by post-modifying the synthons with metal ions. The optical band gap property for the five compounds and the photoluminescence of 20 were also investigeted.
引文
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