金属有机膦酸配位聚合物的合成、表征及晶体结构研究
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摘要
金属有机膦酸配位聚合物因其结构上的多样性以及在离子交换、嵌入材料、吸附材料、质子导电材料和催化材料等领域具有潜在的应用前景，已引起人们的广泛关注。
本文利用低温水热合成技术，以具有手性结构特征的功能性有机膦酸RPO_3H_2为构筑单元(R为手性或非手性功能性有机基团，结构中含有-OH，-NH_2或-COOH等功能性基团中的一种或几种)，通过直接反应法或引入模板剂法成功地合成了8种未见文献报道的新型金属有机膦酸配位聚合物的晶体材料，并利用X-射线单晶衍射、IR光谱和TG-DTA分析对所合成材料的晶体结构及骨架热稳定性进行了研究。
在所合成的8种金属有机膦酸配位聚合物中，有机配体包括三种：α-氨基乙膦酸，L-脯氨酸-N-甲基-瞵酸和2-羟基膦酰基乙酸，配位金属离子共8种，化合物中有机膦酸作为桥连配体通过功能性基团中的氧原子连接MO_n多面体(M代表金属，n代表氧原子个数)形成二维层状或三维空旷骨架结构。化合物的化学式如下：Zn[O_3PCH(NH_2)CH_3]·2H_2O(1)，Pb_4O[O_3PCH_2-NC_4H_7-CO_2]_2(2)，Mg_(0.5)Cd[O_3PCH(OH)CO_2](3)，Na_2[Cd_2(H_2O)_3(O_3PCH(OH)CO_2)_2]·2H_2O(4)，NaCo[O_3PCH(OH)CO_2](5)，NaMn[O_3PCH(OH)CO_2](6)，[NH_3CH_2CH_2NH_3][Fe_2(O_3PCH(OH)CO_2)_2(H_2O)_2]·2H_2O(7)和[NH_2CH_2CH_2NH_2][Sb_2{O_3PCH(OH)CO_2}_2](8)。其中前6种化合物通过直接反应法获得，X-射线单晶衍射实验表明化合物(5)和(6)具有三维骨架结构，其余为二维层状结构：化合物(7)和(8)通过引入模板剂乙二胺获得，具有二维层状结构，乙二胺分子位于孔道中。TG-DTA分析表明，该类化合物均具有较稳定的骨架结构。
Metal phosphonate coordination polymers have attracted a great deal of research interest due to their structural diversities and many potential and practical applications in catalysis, ion exchange, intercalation chemistry, absorption, proton conduction, and so on.
In this work, we have devoted effort toward hydrothermal synthesis of the metal-organic coordination polymers by using organophosphonic acid ligands RPO_3H_2 (R = chiral or achiral organic groups with functional groups such as -OH, -NH_2 and -COOH ) with chiral groups as chiral building units to obtain possible new types of materials with potential applications. Eight novel metal phosphonate coordination polymers were hydrothermally synthesized by using direct reaction or organic-amine as template agent, and characterized by using X-ray single-crystal diffraction, IR spectroscopy and thermogravimetric analysis.
Three kinds of organophosphonic acid ligands, such as a-aminoethylphosphonic acid, (S)-proline-N-methyl- phosphonic acid and 2-hydroxyphosphonoacetic acid were used in the synthesis of metal phosphonate coordination polymers. In the structure of these compounds, the MO_n (M = metal, n = the number of oxygen atoms) polyhedral are bridged by the oxygen atoms from the functional groups of the organophosphonic acid ligands, resulting in the formation of two-dimensional layer or three-dimensional open framework. The chemical constitution formulas are listed as follow: Zn[O_3PCH(NH_2)CH_3]·2H_2O (1) Pb_4O[O_3PCH_2-NC_4H_7-CO_2]_2 (2), Mg_(0.5)Cd[O_3PCH(OH)CO_2] (3), Na_2[Cd_2(H_2O)_3(O_3PCH-(OH)CO_2)_2]-2H_2O (4) , NaCo[O_3PCH(OH)CO_2] (5) , NaMn[O_3PCH(OH)CO_2] (6) , [NH_3CH_2CH_2NH_3][Fe_2(O_3PCH(OH)CO_2)_2(H_2O)_2]-2H_2O (7) and [NH_2CH_2CH2NH_2][Sb_2-{O_3PCH(OH)CO_2}_2] (8) . Compounds (1) ~ (6) are obtained by the direct reaction, and the single-crystal X-ray diffraction analysis shows that the compounds (5) and (6) feature three-dimensional open framework structure, and the other four compounds form two-dimensional layer structure. Compounds (7) and (8) are synthesized by using organic-amine as template agent, X-ray diffraction analysis shows that the two compounds feature two-dimensional layer structure, and the ethylenediamine cations are located in the
本文利用低温水热合成技术，以具有手性结构特征的功能性有机膦酸RPO_3H_2为构筑单元(R为手性或非手性功能性有机基团，结构中含有-OH，-NH_2或-COOH等功能性基团中的一种或几种)，通过直接反应法或引入模板剂法成功地合成了8种未见文献报道的新型金属有机膦酸配位聚合物的晶体材料，并利用X-射线单晶衍射、IR光谱和TG-DTA分析对所合成材料的晶体结构及骨架热稳定性进行了研究。
在所合成的8种金属有机膦酸配位聚合物中，有机配体包括三种：α-氨基乙膦酸，L-脯氨酸-N-甲基-瞵酸和2-羟基膦酰基乙酸，配位金属离子共8种，化合物中有机膦酸作为桥连配体通过功能性基团中的氧原子连接MO_n多面体(M代表金属，n代表氧原子个数)形成二维层状或三维空旷骨架结构。化合物的化学式如下：Zn[O_3PCH(NH_2)CH_3]·2H_2O(1)，Pb_4O[O_3PCH_2-NC_4H_7-CO_2]_2(2)，Mg_(0.5)Cd[O_3PCH(OH)CO_2](3)，Na_2[Cd_2(H_2O)_3(O_3PCH(OH)CO_2)_2]·2H_2O(4)，NaCo[O_3PCH(OH)CO_2](5)，NaMn[O_3PCH(OH)CO_2](6)，[NH_3CH_2CH_2NH_3][Fe_2(O_3PCH(OH)CO_2)_2(H_2O)_2]·2H_2O(7)和[NH_2CH_2CH_2NH_2][Sb_2{O_3PCH(OH)CO_2}_2](8)。其中前6种化合物通过直接反应法获得，X-射线单晶衍射实验表明化合物(5)和(6)具有三维骨架结构，其余为二维层状结构：化合物(7)和(8)通过引入模板剂乙二胺获得，具有二维层状结构，乙二胺分子位于孔道中。TG-DTA分析表明，该类化合物均具有较稳定的骨架结构。
Metal phosphonate coordination polymers have attracted a great deal of research interest due to their structural diversities and many potential and practical applications in catalysis, ion exchange, intercalation chemistry, absorption, proton conduction, and so on.
In this work, we have devoted effort toward hydrothermal synthesis of the metal-organic coordination polymers by using organophosphonic acid ligands RPO_3H_2 (R = chiral or achiral organic groups with functional groups such as -OH, -NH_2 and -COOH ) with chiral groups as chiral building units to obtain possible new types of materials with potential applications. Eight novel metal phosphonate coordination polymers were hydrothermally synthesized by using direct reaction or organic-amine as template agent, and characterized by using X-ray single-crystal diffraction, IR spectroscopy and thermogravimetric analysis.
Three kinds of organophosphonic acid ligands, such as a-aminoethylphosphonic acid, (S)-proline-N-methyl- phosphonic acid and 2-hydroxyphosphonoacetic acid were used in the synthesis of metal phosphonate coordination polymers. In the structure of these compounds, the MO_n (M = metal, n = the number of oxygen atoms) polyhedral are bridged by the oxygen atoms from the functional groups of the organophosphonic acid ligands, resulting in the formation of two-dimensional layer or three-dimensional open framework. The chemical constitution formulas are listed as follow: Zn[O_3PCH(NH_2)CH_3]·2H_2O (1) Pb_4O[O_3PCH_2-NC_4H_7-CO_2]_2 (2), Mg_(0.5)Cd[O_3PCH(OH)CO_2] (3), Na_2[Cd_2(H_2O)_3(O_3PCH-(OH)CO_2)_2]-2H_2O (4) , NaCo[O_3PCH(OH)CO_2] (5) , NaMn[O_3PCH(OH)CO_2] (6) , [NH_3CH_2CH_2NH_3][Fe_2(O_3PCH(OH)CO_2)_2(H_2O)_2]-2H_2O (7) and [NH_2CH_2CH2NH_2][Sb_2-{O_3PCH(OH)CO_2}_2] (8) . Compounds (1) ~ (6) are obtained by the direct reaction, and the single-crystal X-ray diffraction analysis shows that the compounds (5) and (6) feature three-dimensional open framework structure, and the other four compounds form two-dimensional layer structure. Compounds (7) and (8) are synthesized by using organic-amine as template agent, X-ray diffraction analysis shows that the two compounds feature two-dimensional layer structure, and the ethylenediamine cations are located in the
引文
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