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Radical cations of chalcogenanthrenes with halogenido metalate anions. Part I: tetramethoxythianthrene 具有卤代金属酸阴离子的查尔根蒽的辐射阳离子。第一部分:四甲氧基噻蒽
Pub Date : 2024-07-05 DOI: 10.1515/znb-2024-0016
Karen-Christina Schipmann, Jörg Daniels, Johannes Beck
The electron-rich molecule tetramethoxythianthrene TMO-TA can readily be oxidized to the radical cation using various transition metal halides in acetonitrile as solvent. Reactions with CuBr2, FeCl3, AuCl3, NbCl5, and CuCl2 yield dark blue or black crystals of [TMO-TA]2[CuBr4] (2), [TMO-TA][FeCl4] · CH3CN (3), [TMO-TA][AuCl4] (4), [TMO-TA][NbCl6] · CH3CN (6), and [TMO-TA]5[Cu2Cl6]2 · 2 CH3CN (7). [TMO-TA]2[Ta2OF10] (5) was obtained by anodic oxidation of TMO-TA in the presence of (Nbu4)2[Ta2OF10] as electrolyte. Using mercury(II) bromide, no redox reaction occurs. Instead, the colorless complex [HgBr2(TMO-TA)] (1) is formed. In the crystal structures of the compounds 2–7, the almost planar radical cations show different types of arrangements. Pair formation of the [TMO-TA]•+ radicals to [TMO-TA]2 2+ dimers with the typical intra-pair S⋯S bonds of 3.1–3.2 Å lengths is predominant. Compounds 6 and 7 contain stacks of planar TMO-TA molecules in equidistant arrangement without pair formation and the unique feature of rotation of each adjacent cation by about 30°. Compounds 2, 5, and 7 are electrical semiconductors with band gaps between 0.62 and 1.4 eV, reflecting the arrangement of the radical cations. While 5 is diamagnetic, the magnetic momenta of 2 and 7 correspond only to the expected paramagnetic momenta of magnetically dilute Cu2+ ions. Electrons on the organic radicals are strongly paired in all compounds.
以乙腈为溶剂,使用各种过渡金属卤化物,富电子分子四甲氧基噻蒽 TMO-TA 很容易被氧化成自由基阳离子。与 CuBr2、FeCl3、AuCl3、NbCl5 和 CuCl2 反应生成深蓝色或黑色晶体 [TMO-TA]2[CuBr4] (2)、[CH3CN (3)、[TMO-TA][AuCl4] (4)、[TMO-TA][NbCl6] - CH3CN (6) 和 [TMO-TA]5[Cu2Cl6]2 - 2 CH3CN (7)。[TMO-TA]2[Ta2OF10](5)是以 (Nbu4)2[Ta2OF10] 为电解质,通过阳极氧化 TMO-TA 而得到的。使用溴化汞(II)时,不会发生氧化还原反应。相反,形成了无色的复合物 [HgBr2(TMO-TA)] (1)。在化合物 2-7 的晶体结构中,几乎是平面的自由基阳离子呈现出不同的排列方式。[TMO-TA]-+自由基成对形成的[TMO-TA]2 2+ 二聚体具有典型的对内 S⋯S 键(长度为 3.1-3.2 Å),这种情况占主导地位。化合物 6 和 7 包含等距排列的平面 TMO-TA 分子堆栈,没有形成配对,而且每个相邻阳离子都旋转了约 30°。化合物 2、5 和 7 是带隙介于 0.62 和 1.4 eV 之间的电半导体,反映了自由基阳离子的排列。5 是二磁性的,而 2 和 7 的磁矩仅与预期的磁性稀释 Cu2+ 离子的顺磁矩一致。在所有化合物中,有机自由基上的电子都是强配对的。
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引用次数: 0
Magnetic properties of the solid solutions CePt1−x Au x Al (x = 0.1–0.9) 固溶体 CePt1-x Au x Al(x = 0.1-0.9 )的磁性能
Pub Date : 2024-07-02 DOI: 10.1515/znb-2024-0040
Konstantin Renner, Fabian Eustermann, Oliver Niehaus, Oliver Janka
Members of the solid solutions CePt1–x Au x Al have been synthesized from the elements and pure samples could be obtained for the whole range of x from 0.1–0.9. Powder X-ray diffraction patterns indicated the TiNiSi-type structure (orthorhombic, space group Pnma) for the whole series, consistent with the end members CePtAl and CeAuAl. The lattice parameters and therefore also the unit cell volumes evolve in a linear fashion when going from CePtAl to CeAuAl. Magnetic susceptibility and magnetization investigations were performed for the compounds with x = 0.1, 0.2, 0.3, 0.5, 0.7 and 0.9. The results show that the ferromagnetic ground state of CePtAl gets destabilized for small degrees of substitution (x = 0.1) resulting in a lower Curie temperature. For larger values of x, changes towards an antiferromagnetic ground state are observed, in line with pure CeAuAl.
从这些元素中合成了固溶体 CePt1-x Au x Al,并在 0.1-0.9 的整个 x 范围内获得了纯样品。粉末 X 射线衍射图样显示整个系列具有 TiNiSi- 型结构(正交,空间群 Pnma),与最终成员 CePtAl 和 CeAuAl 一致。从 CePtAl 到 CeAuAl,晶格参数以及单胞体积呈线性发展。对 x = 0.1、0.2、0.3、0.5、0.7 和 0.9 的化合物进行了磁感应强度和磁化研究。结果表明,当取代度较小(x = 0.1)时,CePtAl 的铁磁基态会变得不稳定,从而导致居里温度降低。当 x 值越大时,观察到向反铁磁基态的变化,这与纯 CeAuAl 的情况一致。
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引用次数: 0
Gadolinium spin dilution in the ferromagnetic solid solutions Gd2–x Y x Cu2Mg 铁磁固溶体 Gd2-x Y x Cu2Mg 中的钆自旋稀释
Pub Date : 2024-07-02 DOI: 10.1515/znb-2024-0029
Maximilian Kai Reimann, Wilma Pröbsting, Theresa Block, Rainer Pöttgen
Samples of the solid solution Gd2–x Y x Cu2Mg (in steps of x = 0.2) were synthesized from the elements in sealed tantalum ampoules in a high-frequency furnace. The polycrystalline samples were characterized by X-ray powder diffraction. The structure of Gd0.988(6)Y1.012(6)Cu2Mg was refined from single-crystal X-ray diffractometer data: Mo2B2Fe type, P4/mbm, a = 762.83(4), c = 375.48(2) pm, wR2 = 0.0277, 285 F 2 values and 13 variables. Single-crystal data gave no hint for Gd/Y ordering. All samples behave like Curie-Weiss paramagnets with stable trivalent gadolinium and ferromagnetic ordering at low temperature. Within the solid solution the Curie temperature drops almost linearly from T C = 113.5(1) K for Gd2Cu2Mg to 9.3(1) K for Gd0.2Y1.8Cu2Mg, allowing a precise adjustment of the magnetic ordering temperature through gadolinium spin dilution.
固溶体 Gd2-x Y x Cu2Mg 样品(以 x = 0.2 为步长)是在高频炉中从密封的钽安瓿瓶中的元素合成的。通过 X 射线粉末衍射对多晶样品进行了表征。Gd0.988(6)Y1.012(6)Cu2Mg 的结构是从单晶 X 射线衍射仪数据中提炼出来的:Mo2B2Fe 型,P4/mbm,a = 762.83(4),c = 375.48(2) pm,wR2 = 0.0277,285 F 2 值和 13 个变量。单晶数据没有提示 Gd/Y 排序。所有样品在低温下都表现为具有稳定三价钆和铁磁有序性的居里-魏斯顺磁体。在固溶体中,居里温度从 Gd2Cu2Mg 的 T C = 113.5(1) K 几乎线性下降到 Gd0.2Y1.8Cu2Mg 的 9.3(1) K,从而可以通过钆自旋稀释精确调节磁有序温度。
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引用次数: 0
On the interaction of Lewis acids on pyrroles and indoles 路易斯酸与吡咯和吲哚的相互作用
Pub Date : 2024-06-29 DOI: 10.1515/znb-2024-0003
Horst Hartmann, Jens Schönewerk
Although the ability of Lewis acids to initiate oligomerisation or polymerisation of pyrroles and indoles is known, no reliable information was available on the structures of the complexes formed therewith. Using 1H NMR spectroscopy, an attempt has now been made to elucidate the structures of the complexes formed by the treatment of pyrroles and indoles with AlCl3.
虽然路易斯酸引发吡咯和吲哚低聚或聚合的能力已经为人所知,但关于与之形成的复合物的结构却没有可靠的信息。现在,我们尝试使用 1H NMR 光谱来阐明用 AlCl3 处理吡咯和吲哚所形成的络合物的结构。
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引用次数: 0
The isotypic series of tetragonal lanthanoid(III) fluoride oxoarsenates(III) Ln 5F3[AsO3]4 (Ln = Eu–Lu) 氟化镧系元素(III)氧化砷酸盐(III)Ln 5F3[AsO3]4(Ln = Eu-Lu)的同种型系列
Pub Date : 2024-06-27 DOI: 10.1515/znb-2024-0030
Ralf J. C. Locke, Florian Ledderboge, Felix C. Goerigk, Frank C. Zimmer, Thomas Schleid
The new fluoride-containing lanthanoid(III) oxoarsenates(III) with the composition Ln 5F3[AsO3]4 (Ln = Eu–Lu) could be obtained through partial metallothermic reduction from mixtures of the corresponding trifluorides (LnF3) and the metals (Ln) with As2O3 upon heating in fused silica ampoules. They all crystallize tetragonally in the space group P4/ncc with lattice parameters ranging from a = 1164.71(8) pm and c = 1097.95(7) pm for Eu5F3[AsO4]4 down to a = 1125.72(8) pm and c = 1061.16(7) pm for Lu5F3[AsO3]4 for Z = 4 as consequence of the lanthanoid contraction. The crystal structure exhibits three positions for the trications occupied by one As3+ and two Ln 3+ species. The lanthanoids occur with two different coordination polyhedra consisting of a fluoride-capped oxygen cube [(Ln1)O8F]14− and a bicapped trigonal prism [(Ln2)O6F2]11− of F and O2− anions. A surprisingly diverse Ln 3+ cation coordination for the F anions is noteworthy, as (F1) has contact to five, but (F2) to only two of them. The crystallographically unique As3+ cation is coordinated in a discrete ψ 1-tetrahedron [AsO3]3− by three oxygen atoms. The lone-pairs of electrons at the As3+ centers point into empty channels along [001], flanked by four columns of condensed [(Ln1)O8F]14− polyhedra. As rather short oxygen-fluorine distances are present within this structural feature, the absence of (OH) units apt to replace F needed to be verified by single-crystal Raman spectroscopy. The composition Ln 5F3[AsO3] was also confirmed by electron-beam microprobe (EDXS) measurements and the phase purity of selected samples could be proven by powder X-ray diffractometry (PXRD).
在熔融石英安瓿瓶中加热相应的三氟化物(LnF3)和金属(Ln)与 As2O3 的混合物,通过部分金属热还原法可获得成分为 Ln 5F3[AsO3]4(Ln = Eu-Lu)的新型含氟镧系(III)氧胂酸盐(III)。它们都在空间群 P4/ncc 中呈四边形结晶,晶格参数从 Eu5F3[AsO4]4 的 a = 1164.71(8) pm 和 c = 1097.95(7) pm 到 Z = 4 的 Lu5F3[AsO3]4 的 a = 1125.72(8) pm 和 c = 1061.16(7) pm 不等,这是镧系收缩的结果。晶体结构显示了由一个 As3+ 和两个 Ln 3+ 物种占据的三个位置。镧系元素具有两种不同的配位多面体,包括一个氟化物封顶的氧立方体[(Ln1)O8F]14-和一个由 F- 和 O2- 阴离子组成的双封顶三棱柱[(Ln2)O6F2]11-。值得注意的是,F- 阴离子的 Ln 3+ 阳离子配位具有惊人的多样性,(F1)- 与五个阳离子接触,但 (F2)- 仅与其中两个阳离子接触。晶体学上独特的 As3+ 阳离子在离散的 ψ 1 四面体 [AsO3]3- 中与三个氧原子配位。As3+ 中心的孤电子对沿着 [001] 指向空通道,两侧是四列缩合的 [(Ln1)O8F]14-多面体。由于这一结构特征中的氧氟距离很短,因此需要通过单晶拉曼光谱来验证是否存在可替代 F- 的 (OH)- 单元。电子束微探针(EDXS)测量也证实了 Ln 5F3[AsO3] 的组成,粉末 X 射线衍射仪(PXRD)也证明了所选样品的相纯度。
{"title":"The isotypic series of tetragonal lanthanoid(III) fluoride oxoarsenates(III) Ln 5F3[AsO3]4 (Ln = Eu–Lu)","authors":"Ralf J. C. Locke, Florian Ledderboge, Felix C. Goerigk, Frank C. Zimmer, Thomas Schleid","doi":"10.1515/znb-2024-0030","DOIUrl":"https://doi.org/10.1515/znb-2024-0030","url":null,"abstract":"The new fluoride-containing lanthanoid(III) oxoarsenates(III) with the composition <jats:italic>Ln</jats:italic> <jats:sub>5</jats:sub>F<jats:sub>3</jats:sub>[AsO<jats:sub>3</jats:sub>]<jats:sub>4</jats:sub> (<jats:italic>Ln</jats:italic> = Eu–Lu) could be obtained through partial metallothermic reduction from mixtures of the corresponding trifluorides (<jats:italic>Ln</jats:italic>F<jats:sub>3</jats:sub>) and the metals (<jats:italic>Ln</jats:italic>) with As<jats:sub>2</jats:sub>O<jats:sub>3</jats:sub> upon heating in fused silica ampoules. They all crystallize tetragonally in the space group <jats:italic>P</jats:italic>4/<jats:italic>ncc</jats:italic> with lattice parameters ranging from <jats:italic>a</jats:italic> = 1164.71(8) pm and <jats:italic>c</jats:italic> = 1097.95(7) pm for Eu<jats:sub>5</jats:sub>F<jats:sub>3</jats:sub>[AsO<jats:sub>4</jats:sub>]<jats:sub>4</jats:sub> down to <jats:italic>a</jats:italic> = 1125.72(8) pm and <jats:italic>c</jats:italic> = 1061.16(7) pm for Lu<jats:sub>5</jats:sub>F<jats:sub>3</jats:sub>[AsO<jats:sub>3</jats:sub>]<jats:sub>4</jats:sub> for <jats:italic>Z</jats:italic> = 4 as consequence of the lanthanoid contraction. The crystal structure exhibits three positions for the trications occupied by one As<jats:sup>3+</jats:sup> and two <jats:italic>Ln</jats:italic> <jats:sup>3+</jats:sup> species. The lanthanoids occur with two different coordination polyhedra consisting of a fluoride-capped oxygen cube [(<jats:italic>Ln</jats:italic>1)O<jats:sub>8</jats:sub>F]<jats:sup>14−</jats:sup> and a bicapped trigonal prism [(<jats:italic>Ln</jats:italic>2)O<jats:sub>6</jats:sub>F<jats:sub>2</jats:sub>]<jats:sup>11−</jats:sup> of F<jats:sup>−</jats:sup> and O<jats:sup>2−</jats:sup> anions. A surprisingly diverse <jats:italic>Ln</jats:italic> <jats:sup>3+</jats:sup> cation coordination for the F<jats:sup>−</jats:sup> anions is noteworthy, as (F1)<jats:sup>−</jats:sup> has contact to five, but (F2)<jats:sup>−</jats:sup> to only two of them. The crystallographically unique As<jats:sup>3+</jats:sup> cation is coordinated in a discrete <jats:italic>ψ</jats:italic> <jats:sup>1</jats:sup>-tetrahedron [AsO<jats:sub>3</jats:sub>]<jats:sup>3−</jats:sup> by three oxygen atoms. The lone-pairs of electrons at the As<jats:sup>3+</jats:sup> centers point into empty channels along [001], flanked by four columns of condensed [(<jats:italic>Ln</jats:italic>1)O<jats:sub>8</jats:sub>F]<jats:sup>14−</jats:sup> polyhedra. As rather short oxygen-fluorine distances are present within this structural feature, the absence of (OH)<jats:sup>−</jats:sup> units apt to replace F<jats:sup>−</jats:sup> needed to be verified by single-crystal Raman spectroscopy. The composition <jats:italic>Ln</jats:italic> <jats:sub>5</jats:sub>F<jats:sub>3</jats:sub>[AsO<jats:sub>3</jats:sub>] was also confirmed by electron-beam microprobe (EDXS) measurements and the phase purity of selected samples could be proven by powder X-ray diffractometry (PXRD).","PeriodicalId":23831,"journal":{"name":"Zeitschrift für Naturforschung B","volume":"26 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-06-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141505316","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
The crystal structures of the ternary intermetallics RE 2Pd2Cd (RE = Nd, Sm, Gd, Dy) and RE 2Ga2Mg (RE = Tb, Er, Tm, Lu) at 90 K 三元金属间化合物 RE 2Pd2Cd(RE = Nd、Sm、Gd、Dy)和 RE 2Ga2Mg(RE = Tb、Er、Tm、Lu)在 90 K 时的晶体结构
Pub Date : 2024-06-25 DOI: 10.1515/znb-2024-0014
Maximilian Kai Reimann, Jutta Kösters, Tautvydas Bieliauskas, Rainer Pöttgen
The crystal structures of the U3Si2-related intermetallic compounds RE 2Pd2Cd (RE = Nd, Sm, Gd, Dy) and RE 2Ga2Mg (RE = Tb, Er, Tm, Lu) were studied from single crystal X-ray diffraction data at T = 90 K in order to understand the slightly enhanced U 33 displacements of the 2a positions in their room temperature structures. The compounds Sm2Pd2Cd, Gd2Pd2Cd and Dy2Pd2Cd show a decrease of the ratio of U 33 to U 11 for the cadmium atoms, leading to a more isotropic behavior at low temperature, keeping the P4/mbm space group symmetry. Nd2Pd2Cd shows a translationengleiche symmetry reduction to space group P4bm along with a weak puckering effect with shorter (342.7 pm) and longer (345.7 pm) Cd–Nd distances within the Cd@Nd8 square prisms. This new, non-centrosymmetric superstructure variant was also observed for the magnesium compounds Tb2Ga2.069Mg0.931, Er2Ga2.104Mg0.896, Tm2Ga2.097Mg0.903 and Lu2Ga2.173Mg0.827, which show small degrees of Mg/Ga mixing.
根据单晶 X 射线衍射数据,研究了 U3Si2 相关金属间化合物 RE 2Pd2Cd(RE = Nd、Sm、Gd、Dy)和 RE 2Ga2Mg(RE = Tb、Er、Tm、Lu)在 T = 90 K 时的晶体结构,以了解其室温结构中 2a 位置的 U 33 位移略微增强的情况。Sm2Pd2Cd、Gd2Pd2Cd 和 Dy2Pd2Cd 化合物显示出镉原子的 U 33 与 U 11 之比减小,从而在低温下表现出更大的各向同性,保持了 P4/mbm 空间群对称性。Nd2Pd2Cd 在 Cd@Nd8 方棱柱内的 Cd-Nd 间距较短(342.7 pm)和较长(345.7 pm)时,显示出平移棱对称性降低到 P4bm 空间群,同时出现微弱的起皱效应。在镁化合物 Tb2Ga2.069Mg0.931、Er2Ga2.104Mg0.896、Tm2Ga2.097Mg0.903 和 Lu2Ga2.173Mg0.827 中也观察到了这种新的、非中心对称的超结构变体,它们显示出较小程度的镁/镓混合。
{"title":"The crystal structures of the ternary intermetallics RE 2Pd2Cd (RE = Nd, Sm, Gd, Dy) and RE 2Ga2Mg (RE = Tb, Er, Tm, Lu) at 90 K","authors":"Maximilian Kai Reimann, Jutta Kösters, Tautvydas Bieliauskas, Rainer Pöttgen","doi":"10.1515/znb-2024-0014","DOIUrl":"https://doi.org/10.1515/znb-2024-0014","url":null,"abstract":"The crystal structures of the U<jats:sub>3</jats:sub>Si<jats:sub>2</jats:sub>-related intermetallic compounds <jats:italic>RE</jats:italic> <jats:sub>2</jats:sub>Pd<jats:sub>2</jats:sub>Cd (<jats:italic>RE</jats:italic> = Nd, Sm, Gd, Dy) and <jats:italic>RE</jats:italic> <jats:sub>2</jats:sub>Ga<jats:sub>2</jats:sub>Mg (<jats:italic>RE</jats:italic> = Tb, Er, Tm, Lu) were studied from single crystal X-ray diffraction data at <jats:italic>T</jats:italic> = 90 K in order to understand the slightly enhanced <jats:italic>U</jats:italic> <jats:sub>33</jats:sub> displacements of the 2<jats:italic>a</jats:italic> positions in their room temperature structures. The compounds Sm<jats:sub>2</jats:sub>Pd<jats:sub>2</jats:sub>Cd, Gd<jats:sub>2</jats:sub>Pd<jats:sub>2</jats:sub>Cd and Dy<jats:sub>2</jats:sub>Pd<jats:sub>2</jats:sub>Cd show a decrease of the ratio of <jats:italic>U</jats:italic> <jats:sub>33</jats:sub> to <jats:italic>U</jats:italic> <jats:sub>11</jats:sub> for the cadmium atoms, leading to a more isotropic behavior at low temperature, keeping the <jats:italic>P</jats:italic>4/<jats:italic>mbm</jats:italic> space group symmetry. Nd<jats:sub>2</jats:sub>Pd<jats:sub>2</jats:sub>Cd shows a <jats:italic>translationengleiche</jats:italic> symmetry reduction to space group <jats:italic>P</jats:italic>4<jats:italic>bm</jats:italic> along with a weak puckering effect with shorter (342.7 pm) and longer (345.7 pm) Cd–Nd distances within the Cd@Nd<jats:sub>8</jats:sub> square prisms. This new, non-centrosymmetric superstructure variant was also observed for the magnesium compounds Tb<jats:sub>2</jats:sub>Ga<jats:sub>2.069</jats:sub>Mg<jats:sub>0.931</jats:sub>, Er<jats:sub>2</jats:sub>Ga<jats:sub>2.104</jats:sub>Mg<jats:sub>0.896</jats:sub>, Tm<jats:sub>2</jats:sub>Ga<jats:sub>2.097</jats:sub>Mg<jats:sub>0.903</jats:sub> and Lu<jats:sub>2</jats:sub>Ga<jats:sub>2.173</jats:sub>Mg<jats:sub>0.827</jats:sub>, which show small degrees of Mg/Ga mixing.","PeriodicalId":23831,"journal":{"name":"Zeitschrift für Naturforschung B","volume":"104 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-06-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141514691","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Hydrothermal syntheses, structures and properties of two zinc complexes based on an azobenzene carboxylate ligand 基于偶氮苯羧酸配体的两种锌配合物的水热合成、结构和性质
Pub Date : 2024-06-25 DOI: 10.1515/znb-2023-0114
Mou-Yi Zhang, Lei Guan
Two zinc complexes [Zn(LH)2(phen)] (1) and [Zn(L)(H2O)] n (2) (LH = 2-hydroxy-5-((3-nitrophenyl)azo)-benzoate, phen = 1,10-phenanthroline) were synthesized by hydrothermal methods and characterized by elemental analysis and IR spectroscopy. Complexes 1 and 2 crystallize in mononuclear and polymeric structures, respectively, where ligands L 2− are coordinated to the zinc ions via their carboxylate and phenolate groups in η 2,μ 2,κ 2 and η 2,μ 2,κ 1 mode, respectively. Introduction of the auxiliary chelating phen ligand results in the chelation of the zinc ions in 1 through both the phen ligand and the carboxylate group of the first LH anion assisted further by the monodentate carboxylate group of the second LH anion. In complex 2 the L 2− anions act as tridentate ligands utilizing their carboxylate and phenolate groups to coordinate to three zinc ions. The phenolate oxygen atom bridges two zinc ions resulting in the generation of a layer structure. Fluorescence measurements have indicated that complexes 1 and 2 exhibit similar luminescence emissions around 393 and 387 nm, respectively, which originate from intra-ligand π-π* transitions. The emission intensities were strengthened relative to the sodium complex NaLH owing to the enhancement of the rigidity of the aromatic system through the coordination interactions of the ligands with the more tightly bound zinc ions. Furthermore, the suspension of complex 2 can be used to selectively detect Fe3+ cations via the luminescence quenching process.
通过水热法合成了两种锌配合物 [Zn(LH)2(phen)] (1) 和 [Zn(L)(H2O)] n (2)(LH- = 2-羟基-5-((3-硝基苯基)偶氮)-苯甲酸酯,phen = 1,10-菲罗啉),并通过元素分析和红外光谱对其进行了表征。配合物 1 和 2 分别以单核和聚合物结构结晶,其中配体 L 2- 通过其羧基和苯酚基分别以 η 2,μ 2,κ 2 和 η 2,μ 2,κ 1 模式与锌离子配位。辅助螯合剂 phen 配体的引入导致 1 中的锌离子通过 phen 配体和第一个 LH- 阴离子的羧酸基团螯合,并进一步得到第二个 LH- 阴离子的单齿羧酸基团的帮助。在复合物 2 中,L 2-阴离子作为三叉配体,利用其羧基和苯酚基与三个锌离子配位。苯酚氧原子将两个锌离子连接起来,形成了层状结构。荧光测量结果表明,复合物 1 和 2 分别在 393 纳米和 387 纳米附近发出类似的荧光,这些荧光来自配体内部的 π-π* 转变。与钠络合物 NaLH 相比,发射强度有所增强,这是因为配体与结合更紧密的锌离子之间的配位相互作用增强了芳香系统的刚性。此外,络合物 2 的悬浮液可用于通过发光淬灭过程选择性地检测 Fe3+ 阳离子。
{"title":"Hydrothermal syntheses, structures and properties of two zinc complexes based on an azobenzene carboxylate ligand","authors":"Mou-Yi Zhang, Lei Guan","doi":"10.1515/znb-2023-0114","DOIUrl":"https://doi.org/10.1515/znb-2023-0114","url":null,"abstract":"Two zinc complexes [Zn(<jats:italic>L</jats:italic>H)<jats:sub>2</jats:sub>(phen)] (1) and [Zn(<jats:italic>L</jats:italic>)(H<jats:sub>2</jats:sub>O)]<jats:sub> <jats:italic>n</jats:italic> </jats:sub> (2) (<jats:italic>L</jats:italic>H<jats:sup>−</jats:sup> = 2-hydroxy-5-((3-nitrophenyl)azo)-benzoate, phen = 1,10-phenanthroline) were synthesized by hydrothermal methods and characterized by elemental analysis and IR spectroscopy. Complexes 1 and 2 crystallize in mononuclear and polymeric structures, respectively, where ligands <jats:italic>L</jats:italic> <jats:sup>2−</jats:sup> are coordinated to the zinc ions via their carboxylate and phenolate groups in <jats:italic>η</jats:italic> <jats:sup>2</jats:sup>,<jats:italic>μ</jats:italic> <jats:sub>2</jats:sub>,<jats:italic>κ</jats:italic> <jats:sup>2</jats:sup> and <jats:italic>η</jats:italic> <jats:sup>2</jats:sup>,<jats:italic>μ</jats:italic> <jats:sub>2</jats:sub>,<jats:italic>κ</jats:italic> <jats:sup>1</jats:sup> mode, respectively. Introduction of the auxiliary chelating phen ligand results in the chelation of the zinc ions in 1 through both the phen ligand and the carboxylate group of the first <jats:italic>L</jats:italic>H<jats:sup>−</jats:sup> anion assisted further by the monodentate carboxylate group of the second <jats:italic>L</jats:italic>H<jats:sup>−</jats:sup> anion. In complex 2 the <jats:italic>L</jats:italic> <jats:sup>2−</jats:sup> anions act as tridentate ligands utilizing their carboxylate and phenolate groups to coordinate to three zinc ions. The phenolate oxygen atom bridges two zinc ions resulting in the generation of a layer structure. Fluorescence measurements have indicated that complexes 1 and 2 exhibit similar luminescence emissions around 393 and 387 nm, respectively, which originate from intra-ligand π-π<jats:sup>*</jats:sup> transitions. The emission intensities were strengthened relative to the sodium complex Na<jats:italic>L</jats:italic>H owing to the enhancement of the rigidity of the aromatic system through the coordination interactions of the ligands with the more tightly bound zinc ions. Furthermore, the suspension of complex 2 can be used to selectively detect Fe<jats:sup>3+</jats:sup> cations via the luminescence quenching process.","PeriodicalId":23831,"journal":{"name":"Zeitschrift für Naturforschung B","volume":"40 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-06-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141505317","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Bi- and tridentate phosphanegold(I) chloride units linked by organosilane backbones 由有机硅烷骨架连接的双叉和三叉磷金(I)氯化物单元
Pub Date : 2024-06-24 DOI: 10.1515/znb-2024-0026
Peter Heinrichs, Beate Neumann, Hans-Georg Stammler, Norbert W. Mitzel
The tridentate ligand tris(dimethylphosphanyl-methyl)phenylsilane was prepared by the reaction of phenyltrichlorosilane with three equivalents of dimethylphosphanylmethyl lithium. This ligand and the bifunctional bis(dimethylphosphanylmethyl)dimethylsilane were converted into their corresponding gold(I) chloride complexes with three and two AuCl functions, respectively. The complexes were investigated for their ability to form intra- or intermolecular aurophilic interactions.
三叉配体三(二甲基膦酰甲基)苯基硅烷是通过苯基三氯硅烷与三当量的二甲基膦酰甲基锂反应制备的。这种配体和双官能双(二甲基膦酰甲基)二甲基硅烷分别被转化成相应的具有三个和两个 AuCl 官能的氯化金(I)络合物。研究人员对这些配合物形成分子内或分子间亲欧相互作用的能力进行了研究。
{"title":"Bi- and tridentate phosphanegold(I) chloride units linked by organosilane backbones","authors":"Peter Heinrichs, Beate Neumann, Hans-Georg Stammler, Norbert W. Mitzel","doi":"10.1515/znb-2024-0026","DOIUrl":"https://doi.org/10.1515/znb-2024-0026","url":null,"abstract":"The tridentate ligand tris(dimethylphosphanyl-methyl)phenylsilane was prepared by the reaction of phenyltrichlorosilane with three equivalents of dimethylphosphanylmethyl lithium. This ligand and the bifunctional bis(dimethylphosphanylmethyl)dimethylsilane were converted into their corresponding gold(I) chloride complexes with three and two AuCl functions, respectively. The complexes were investigated for their ability to form intra- or intermolecular aurophilic interactions.","PeriodicalId":23831,"journal":{"name":"Zeitschrift für Naturforschung B","volume":"166 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-06-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141505318","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Mechanochemical synthesis and structural characterization of the I2-II-IV-VI4 quaternary chalcogenide Ag2CdGeSe4 I2-II-IV-VI4四元砷化镓 Ag2CdGeSe4 的机械化学合成与结构表征
Pub Date : 2024-04-29 DOI: 10.1515/znb-2023-0113
Kevin D. Profita, Thomas Bredow, Eva M. Heppke
Ag2CdGeSe4 – a I2-II-IV-VI4 quaternary chalcogenide – was synthesized by a mechanochemical synthesis route with a subsequent annealing step inside of a glass ampoule. Detailed analysis and structural investigation using X-ray powder diffraction (PXRD) indicate that Ag2CdGeSe4 crystallizes in the wurtzstannite-type structure with space group Pmn21. For Rietveld refinements, all cubic diamond/sphalerite- and hexagonal diamond/wurtzite-related structure types including all subgroups of the wurtzstannite-type structure were considered. Quantum-chemical calculations were carried out at density-functional theory (DFT) level. The results do not allow an unambiguous verification of the experimentally observed Ag2CdGeSe4 type, due to the small energy differences between the structures. Comparison of calculated and measured UV/Vis data, however, support the results of the Rietveld refinement.
Ag2CdGeSe4是一种I2-II-IV-VI4四元瑀,是通过机械化学合成路线合成的,随后在玻璃安瓿瓶中进行了退火处理。利用 X 射线粉末衍射(PXRD)进行的详细分析和结构研究表明,Ag2CdGeSe4 结晶为空间群 Pmn21 的钨锡矿型结构。在进行里特维尔德细化时,考虑了所有立方体金刚石/闪长岩和六方体金刚石/钨锰铁矿相关的结构类型,包括钨锰铁矿型结构的所有亚群。量子化学计算是在密度泛函理论(DFT)水平上进行的。由于结构间的能量差异较小,计算结果无法明确验证实验观察到的 Ag2CdGeSe4 类型。然而,计算和测量的紫外/可见光数据的比较支持了里特维尔德细化的结果。
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引用次数: 0
High-pressure/high-temperature synthesis, single-crystal structure analysis, and spectroscopic data of γ-Eu(BO2)3 and γ-Gd(BO2)3 γ-Eu(BO2)3和γ-Gd(BO2)3的高压/高温合成、单晶结构分析和光谱数据
Pub Date : 2024-04-20 DOI: 10.1515/znb-2024-0013
Tobias A. Teichtmeister, Alexander Hugo Bernhart, Hubert Huppertz
Orthorhombic crystals of the compounds γ-Eu(BO2)3 and γ-Gd(BO2)3 were obtained by high-pressure/high-temperature syntheses at 10.5 GPa and 1100 and 900 °C, respectively. The structures were solved by single-crystal X-ray diffraction methods. The two compounds crystallize with four formula units per cell in the space group Pca21 (no. 29) with the unit cell parameters a = 18.2729(7), b = 4.4076(2), c = 4.2505(1) Å (Ln = Eu), and a = 18.2591(6), b = 4.4055(1), c = 4.2477(1) Å (Ln = Gd). Their infrared spectra and the luminescence spectrum of γ-Eu(BO2)3 are discussed.
分别在 10.5 GPa、1100 和 900 °C条件下通过高压/高温合成获得了γ-Eu(BO2)3 和 γ-Gd(BO2)3化合物的正方晶。通过单晶 X 射线衍射方法解决了其结构问题。这两种化合物在空间群 Pca21(编号 29)中每个晶胞有四个公式单元,晶胞参数为 a = 18.2729(7),b = 4.4076(2),c = 4.2505(1)埃(Ln = Eu),以及 a = 18.2591(6),b = 4.4055(1),c = 4.2477(1)埃(Ln = Gd)。讨论了它们的红外光谱和 γ-Eu(BO2)3 的发光光谱。
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引用次数: 0
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Zeitschrift für Naturforschung B
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