5-磺酸基间苯二甲酸与稀土金属配位聚合物的晶体结构与表征
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摘要
本论文主要研究了不同结构的配合物的合成方法。我们共合成了5个稀土配合物并对其进行了单晶X-射线衍射、X-射线粉末衍射、红外光谱、热重分析等一系列的表征,考察了不同反应条件对配合物的影响。
用水和乙醇(C2H5OH)的混合溶剂,在水热条件、常温条件以及简单加热的条件下我们制备了SIP与稀土金属Ce和La的配合物[La(SIP)?(H2O)4]n【1】、[Ce(SIP)(H2O)4]n【2】、{[Ce(SIP)(H2O)3]?(H2O)}n【3】、{[La(SIP)(H2O)3]?H2O}n【4】、[Ce(SIP)?5H2O]?3H2O【5】和[Cu(C5H3O4N)?2H2O]【6】。
配合物【1】是水热条件下,NaH2SIP与La(NO3)3·6H2O的摩尔比为1:1的条件下反应得到的3-D结构配位聚合物。在此配合物中,SIP上的两个羧基和磺酸基均参与了配位;两个羧基均以螯合的形式与金属连接,而磺酸基中只有一个氧原子与金属配位,构成了一个具有孔洞的2-D层;氢键和π-π作用力的存在使配合物进一步构筑成3-D结构。而配合物【2】是常温条件下,NaH2SIP与Ce(NO3)3·6H2O摩尔比为3:1的条件下反应得到的与配合物【1】结构相同的配合物。
配合物【3】是在NaH2SIP与Ce(NO3)3·6H2O的配比为1:1,以水和乙醇作为混合溶剂,采用溶剂热的方式反应得到。该配合物中五个SIP与Ce配位,每个SIP的两个羧基均参与了配位,其中一个羧基以螯合的形式连接一个金属,另一个羟基上的两个氧原子均以桥联的方式连接两个Ce离子,而磺酸基中有两个氧原子分别连接两个金属离子;磺酸基在此配合物中起了一定的联接作用,使配位聚合物构成了一个三维的结构。配合物【4】是在80℃的反应条件下得到的与配合物【3】结构相同的配合物。
配合物【5】是在常温下,NaH2SIP与Ce(NO3)3·6H2O以1:1摩尔比的反应合成得到的配位化合物。该配合物结构是由一维长链与水分子构成的3-D构架。在此配合物中,与金属离子Ce配位的两个SIP离子均是羧酸基团以螯合的形式参与配位,形成Zigzag形的一维长链。
配合物【6】是用H2PDA与CuCl2?2H2O在蒸馏水和乙醇的混合溶剂在简单加热条件下反应制得的。虽然反应体系中还加入了NaVO3?2H2O,但是V没有参与配位,只得到了2?6-吡啶二羧酸参与配位的简单配合物。
In coordination chemistry,the coordination ability of sulfonic groups is relatively weak compared with carboxyl groups in organic ligands. Sulfonic group have three oxygen atoms, so it made these ligands have so much more varities of coordination style. If other proper groups are introduced into these ligands, more coordination compounds with novel structure can be obtained. And the coordination ability of carboxyl groups is very strong, when they are combined in ligands with sulfonic groups, the ability of them would be improved greatly. So we studied the reaction of 5-sulfoisophthalic acid monosodium salt and Rare Earth Metal in this paper, mainly studying synthesis method of coordination which have different structures.We had synthexized six compounds and made some characterizations through crystal X-ray diffraction, X-ray powder diffraction, IR and thermogravimetric analysis,and investigate that coordination compounds were influenced by different reaction conditions
[La(SIP)?(H2O)4]n [1] and [Ce(SIP)(H2O)4]n [2] were obtained respectively by mixing the 5-sulfoisophthalic acid monosodium salt with La(NO3)?6H2O hydrothermal condition and with Ce(NO3)3?6H2O at normal temperature, respectively. In structure of compound [1] , center metal ions La (Ⅲ) show nine-coordination feature; Every La (Ⅲ) was surrounded by three SIP, including two oxygens of two carboxyl groups which coordinate with metal ion by chelating and one sulfonic oxygen atom by bridging in these structures. Meanwhile, the La (Ⅲ) atoms coordinate with four oxygens atoms which offer by four water molecules. And every SIP coordinated with three La (Ⅲ) ions through its two carboxylic groups and the sulfo group. Compound [2] is a reported compound.
{[Ce(SIP)(H2O)3]?(H2O)}n [3] and {[La(SIP)(H2O)3]?H2O}n [4] were obtained by mixing the 5-sulfoisophthalic acid monosodium salt with La(NO3)?6H2O in hydro-thermal condition and with Ce(NO3)3?6H2O at normal temperature, respectively. The structure of compound [3] is a asymmetric unit which contains one Ce (Ⅲ) ion, five SIP, three coordinating water molecules and one free water molecules. Center ions Ce (Ⅲ) coordinated with nine oxygen, including four carboxylic oxygen atoms (O1,O2, O6, O7) of three SIPs, two sulfo oxygen atoms (O4,O3A) of other two SIP molecules and another three oxygen atoms of three coordinated water molecules. Compound [4] was a reported complex.
[Ce(SIP)?5H2O]n?3H2O [5] was obtained by mixing the 5-sulfoisophthalic acid monosodium salt with Ce(NO3)3? 6H2O directly. This compound is a asymmetric structure, which contains a Ce (Ⅲ), eight water molecules and one SIP. The Ce (Ⅲ) atoms show the property of nine-coordination, in which including four carboxylic oxygen atoms of two SIP connecting with metal atom by chelating and five oxygen atoms of five water molecules. Meanwhile there are another three free water molecules in the compound, and two carboxylic groups of one SIP connected the two Ce (Ⅲ). Metal ions Ce (Ⅲ) and SIP form an infinite long Zigzag chain, and a stable 2-D construction is formed due to the superimposition of benzene and strong effects ofπ-πstacking. In this complex, the sulfo group don't participate in coordination.
[Cu(C5H3O4N)?2H2O] [6] was obtained by mixing the 2,6-Dipicolinic acid with CuCl2?2H2O and NaVO3?2H2O directly, but no vanadium compound was gained. In compound [6], Cu (Ⅱ) ions coordinate with other five atoms. This compound looks like a butterfly, in which two carboxylic oxygen atoms and one N atom of one 2,6-Dipicolinic acid coordinate with metal atom, and other two oxygen atoms of two water molecules also participate coordinating.
Three compounds are new polymer and the three others are existing compounds among the six synthesized compounds.
用水和乙醇(C2H5OH)的混合溶剂,在水热条件、常温条件以及简单加热的条件下我们制备了SIP与稀土金属Ce和La的配合物[La(SIP)?(H2O)4]n【1】、[Ce(SIP)(H2O)4]n【2】、{[Ce(SIP)(H2O)3]?(H2O)}n【3】、{[La(SIP)(H2O)3]?H2O}n【4】、[Ce(SIP)?5H2O]?3H2O【5】和[Cu(C5H3O4N)?2H2O]【6】。
配合物【1】是水热条件下,NaH2SIP与La(NO3)3·6H2O的摩尔比为1:1的条件下反应得到的3-D结构配位聚合物。在此配合物中,SIP上的两个羧基和磺酸基均参与了配位;两个羧基均以螯合的形式与金属连接,而磺酸基中只有一个氧原子与金属配位,构成了一个具有孔洞的2-D层;氢键和π-π作用力的存在使配合物进一步构筑成3-D结构。而配合物【2】是常温条件下,NaH2SIP与Ce(NO3)3·6H2O摩尔比为3:1的条件下反应得到的与配合物【1】结构相同的配合物。
配合物【3】是在NaH2SIP与Ce(NO3)3·6H2O的配比为1:1,以水和乙醇作为混合溶剂,采用溶剂热的方式反应得到。该配合物中五个SIP与Ce配位,每个SIP的两个羧基均参与了配位,其中一个羧基以螯合的形式连接一个金属,另一个羟基上的两个氧原子均以桥联的方式连接两个Ce离子,而磺酸基中有两个氧原子分别连接两个金属离子;磺酸基在此配合物中起了一定的联接作用,使配位聚合物构成了一个三维的结构。配合物【4】是在80℃的反应条件下得到的与配合物【3】结构相同的配合物。
配合物【5】是在常温下,NaH2SIP与Ce(NO3)3·6H2O以1:1摩尔比的反应合成得到的配位化合物。该配合物结构是由一维长链与水分子构成的3-D构架。在此配合物中,与金属离子Ce配位的两个SIP离子均是羧酸基团以螯合的形式参与配位,形成Zigzag形的一维长链。
配合物【6】是用H2PDA与CuCl2?2H2O在蒸馏水和乙醇的混合溶剂在简单加热条件下反应制得的。虽然反应体系中还加入了NaVO3?2H2O,但是V没有参与配位,只得到了2?6-吡啶二羧酸参与配位的简单配合物。
In coordination chemistry,the coordination ability of sulfonic groups is relatively weak compared with carboxyl groups in organic ligands. Sulfonic group have three oxygen atoms, so it made these ligands have so much more varities of coordination style. If other proper groups are introduced into these ligands, more coordination compounds with novel structure can be obtained. And the coordination ability of carboxyl groups is very strong, when they are combined in ligands with sulfonic groups, the ability of them would be improved greatly. So we studied the reaction of 5-sulfoisophthalic acid monosodium salt and Rare Earth Metal in this paper, mainly studying synthesis method of coordination which have different structures.We had synthexized six compounds and made some characterizations through crystal X-ray diffraction, X-ray powder diffraction, IR and thermogravimetric analysis,and investigate that coordination compounds were influenced by different reaction conditions
[La(SIP)?(H2O)4]n [1] and [Ce(SIP)(H2O)4]n [2] were obtained respectively by mixing the 5-sulfoisophthalic acid monosodium salt with La(NO3)?6H2O hydrothermal condition and with Ce(NO3)3?6H2O at normal temperature, respectively. In structure of compound [1] , center metal ions La (Ⅲ) show nine-coordination feature; Every La (Ⅲ) was surrounded by three SIP, including two oxygens of two carboxyl groups which coordinate with metal ion by chelating and one sulfonic oxygen atom by bridging in these structures. Meanwhile, the La (Ⅲ) atoms coordinate with four oxygens atoms which offer by four water molecules. And every SIP coordinated with three La (Ⅲ) ions through its two carboxylic groups and the sulfo group. Compound [2] is a reported compound.
{[Ce(SIP)(H2O)3]?(H2O)}n [3] and {[La(SIP)(H2O)3]?H2O}n [4] were obtained by mixing the 5-sulfoisophthalic acid monosodium salt with La(NO3)?6H2O in hydro-thermal condition and with Ce(NO3)3?6H2O at normal temperature, respectively. The structure of compound [3] is a asymmetric unit which contains one Ce (Ⅲ) ion, five SIP, three coordinating water molecules and one free water molecules. Center ions Ce (Ⅲ) coordinated with nine oxygen, including four carboxylic oxygen atoms (O1,O2, O6, O7) of three SIPs, two sulfo oxygen atoms (O4,O3A) of other two SIP molecules and another three oxygen atoms of three coordinated water molecules. Compound [4] was a reported complex.
[Ce(SIP)?5H2O]n?3H2O [5] was obtained by mixing the 5-sulfoisophthalic acid monosodium salt with Ce(NO3)3? 6H2O directly. This compound is a asymmetric structure, which contains a Ce (Ⅲ), eight water molecules and one SIP. The Ce (Ⅲ) atoms show the property of nine-coordination, in which including four carboxylic oxygen atoms of two SIP connecting with metal atom by chelating and five oxygen atoms of five water molecules. Meanwhile there are another three free water molecules in the compound, and two carboxylic groups of one SIP connected the two Ce (Ⅲ). Metal ions Ce (Ⅲ) and SIP form an infinite long Zigzag chain, and a stable 2-D construction is formed due to the superimposition of benzene and strong effects ofπ-πstacking. In this complex, the sulfo group don't participate in coordination.
[Cu(C5H3O4N)?2H2O] [6] was obtained by mixing the 2,6-Dipicolinic acid with CuCl2?2H2O and NaVO3?2H2O directly, but no vanadium compound was gained. In compound [6], Cu (Ⅱ) ions coordinate with other five atoms. This compound looks like a butterfly, in which two carboxylic oxygen atoms and one N atom of one 2,6-Dipicolinic acid coordinate with metal atom, and other two oxygen atoms of two water molecules also participate coordinating.
Three compounds are new polymer and the three others are existing compounds among the six synthesized compounds.
引文
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