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Crystal structure and optical properties of a two-sited EuIII compound: an EuIII ion coordinated by two [EuIII(DOTA)]− complexes (DOTA is 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetate)
Acta Crystallographica Section C ( IF 0.8 ) Pub Date : 2021-06-10 , DOI: 10.1107/s2053229621005647 Maria Storm Thomsen 1 , Anders Ø Madsen 2 , Thomas Just Sørensen 1
Acta Crystallographica Section C ( IF 0.8 ) Pub Date : 2021-06-10 , DOI: 10.1107/s2053229621005647 Maria Storm Thomsen 1 , Anders Ø Madsen 2 , Thomas Just Sørensen 1
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The structure and solid-state luminescence properties of an EuIII compound with two different lanthanide sites, [Eu(μ-O)5(OH)(H2O)2][Eu(DOTA)(H2O)]2 (DOTA is 1,4,7,10-tetrazacyclododecane-1,4,7,10-tetraacetate, C16H24N4O8), were determined. The compound crystallizes in a laminar structure in the triclinic space group P
, where the two sites are a free europium(III) ion and an [Eu(DOTA)(H2O)]− complex. The crystal structure was determined using complex data treatment due to nonmerohedral twinning. Experimental data sets were recorded with large redundancy and separated according to scattering domains in order to obtain a reliable structure. In the first site, the [Eu(DOTA)(H2O)]− complex was found to adopt a capped twisted square-antiprismatic (cTSAP) conformation, where a capping water molecule increased the coordination number of the europium(III) site to nine (CN = 9). In the second site, the europium(III) ion was found to be coordinated by two water molecules, one hydroxide group and five oxide groups from neighbouring [Eu(DOTA)(H2O)]− complexes. The coordination geometry of this site was found to be a compressed square antiprism (SAP) and the coordination number of the europium(III) ion was found to be eight (CN = 8). A large increase in the rate constant of luminescence was observed for EuIII in [Eu(DOTA)(H2O)]− in solid-state luminescence spectroscopy measurements compared to in solution, which led to investigations of single crystals in deuterated media to exclude additional effects of quenching. We conclude that the most probable cause of the decrease in the observed luminescence lifetimes is the high asymmetry of the coordination environment of [Eu(DOTA)(D2O)]− in the [Eu(μ-O)5(OD)(D2O)2][Eu(DOTA)(D2O)]2 crystals.
中文翻译：
双位 EuIII 化合物的晶体结构和光学性质：由两个 [EuIII(DOTA)]- 配合物配位的 EuIII 离子（DOTA 是 1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸酯）
的Eu的结构和固态发光性能III与两个不同的镧系元素位点的化合物，[欧盟（μ-O）5（OH）（H 2 O）2 ] [铕（DOTA）（H 2 O）] 2（ DOTA 是 1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸酯，C 16 H 24 N 4 O 8 )，被测定。该化合物在三斜空间群P中以层状结构结晶，其中两个位点是一个游离的铕 (III) 离子和一个 [Eu(DOTA)(H 2 O)] -复杂的。由于非多面体孪晶，晶体结构是使用复杂的数据处理确定的。实验数据集以大冗余记录并根据散射域进行分离以获得可靠的结构。在第一个位点，发现 [Eu(DOTA)(H 2 O)] -复合物采用加帽扭曲方形反棱柱 (cTSAP) 构象，其中加帽水分子增加了铕 (III) 位点的配位数到九（CN = 9）。在第二个位置，发现铕（III）离子由来自相邻 [Eu(DOTA)(H 2 O)]的两个水分子、一个氢氧化物基团和五个氧化物基团配位-复合体。发现该站点的配位几何是压缩的方形反棱镜 (SAP)，发现铕 (III) 离子的配位数为 8 (CN = 8)。在固态发光光谱测量中观察到[Eu(DOTA)(H 2 O)] -中Eu III的发光速率常数比在溶液中显着增加，这导致了对氘化介质中单晶的研究排除淬火的额外影响。我们得出结论，观察到的发光寿命减少的最可能原因是 [Eu(DOTA)(D 2 O)] -在 [Eu(μ-O) 5 (OD)( d 2O) 2 ][Eu(DOTA)(D 2 O)] 2晶体。
更新日期：2021-07-04
, where the two sites are a free europium(III) ion and an [Eu(DOTA)(H2O)]− complex. The crystal structure was determined using complex data treatment due to nonmerohedral twinning. Experimental data sets were recorded with large redundancy and separated according to scattering domains in order to obtain a reliable structure. In the first site, the [Eu(DOTA)(H2O)]− complex was found to adopt a capped twisted square-antiprismatic (cTSAP) conformation, where a capping water molecule increased the coordination number of the europium(III) site to nine (CN = 9). In the second site, the europium(III) ion was found to be coordinated by two water molecules, one hydroxide group and five oxide groups from neighbouring [Eu(DOTA)(H2O)]− complexes. The coordination geometry of this site was found to be a compressed square antiprism (SAP) and the coordination number of the europium(III) ion was found to be eight (CN = 8). A large increase in the rate constant of luminescence was observed for EuIII in [Eu(DOTA)(H2O)]− in solid-state luminescence spectroscopy measurements compared to in solution, which led to investigations of single crystals in deuterated media to exclude additional effects of quenching. We conclude that the most probable cause of the decrease in the observed luminescence lifetimes is the high asymmetry of the coordination environment of [Eu(DOTA)(D2O)]− in the [Eu(μ-O)5(OD)(D2O)2][Eu(DOTA)(D2O)]2 crystals.
中文翻译：
双位 EuIII 化合物的晶体结构和光学性质：由两个 [EuIII(DOTA)]- 配合物配位的 EuIII 离子（DOTA 是 1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸酯）
的Eu的结构和固态发光性能III与两个不同的镧系元素位点的化合物，[欧盟（μ-O）5（OH）（H 2 O）2 ] [铕（DOTA）（H 2 O）] 2（ DOTA 是 1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸酯，C 16 H 24 N 4 O 8 )，被测定。该化合物在三斜空间群P中以层状结构结晶
，其中两个位点是一个游离的铕 (III) 离子和一个 [Eu(DOTA)(H 2 O)] -复杂的。由于非多面体孪晶，晶体结构是使用复杂的数据处理确定的。实验数据集以大冗余记录并根据散射域进行分离以获得可靠的结构。在第一个位点，发现 [Eu(DOTA)(H 2 O)] -复合物采用加帽扭曲方形反棱柱 (cTSAP) 构象，其中加帽水分子增加了铕 (III) 位点的配位数到九（CN = 9）。在第二个位置，发现铕（III）离子由来自相邻 [Eu(DOTA)(H 2 O)]的两个水分子、一个氢氧化物基团和五个氧化物基团配位-复合体。发现该站点的配位几何是压缩的方形反棱镜 (SAP)，发现铕 (III) 离子的配位数为 8 (CN = 8)。在固态发光光谱测量中观察到[Eu(DOTA)(H 2 O)] -中Eu III的发光速率常数比在溶液中显着增加，这导致了对氘化介质中单晶的研究排除淬火的额外影响。我们得出结论，观察到的发光寿命减少的最可能原因是 [Eu(DOTA)(D 2 O)] -在 [Eu(μ-O) 5 (OD)( d 2O) 2 ][Eu(DOTA)(D 2 O)] 2晶体。
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