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Synthesis and structure of a manganese(II) coordination polymer assembled with 5-(tert-butyl)isophthalic acid and 1,3-dimethyl-2-imidazolidinone 用 5-(叔丁基)间苯二甲酸和 1,3-二甲基-2-咪唑烷酮组装的锰(II)配位聚合物的合成及其结构
Pub Date : 2024-02-28 DOI: 10.1515/znb-2022-0093
Xin-hong Chang
A manganese(II) coordination polymer [Mn(tbip)(DMI)] n (1), (tbipH2 = 5-(tert-butyl)isophthalic acid, DMI = 1,3-dimethyl-2-imidazolidinone), has been synthesized under “urea-thermal conditions” (i.e. in an excess of urea). Its structure has been determined by single-crystal X-ray diffraction analysis and further characterized by elemental analysis and IR spectra. Complex 1 crystallizes in the monoclinic space group P21/c with Z = 4. In 1, the [tbip]2− ligand bridges the Mn(II) cations to form infinite chains, and the neighbouring chains are connected through [tbip]2− ligands into layers.
一种锰(II)配位聚合物[Mn(tbip)(DMI)] n (1)(tbipH2 = 5-(叔丁基)间苯二甲酸,DMI = 1,3-二甲基-2-咪唑烷酮)是在 "脲热条件"(即过量脲)下合成的。通过单晶 X 射线衍射分析确定了其结构,并通过元素分析和红外光谱进一步确定了其特征。络合物 1 结晶于 Z = 4 的单斜空间群 P21/c。在 1 中,[tbip]2- 配体将 Mn(II) 阳离子桥接成无限链,相邻的链通过 [tbip]2- 配体连接成层。
{"title":"Synthesis and structure of a manganese(II) coordination polymer assembled with 5-(tert-butyl)isophthalic acid and 1,3-dimethyl-2-imidazolidinone","authors":"Xin-hong Chang","doi":"10.1515/znb-2022-0093","DOIUrl":"https://doi.org/10.1515/znb-2022-0093","url":null,"abstract":"A manganese(II) coordination polymer [Mn(tbip)(DMI)]<jats:sub> <jats:italic>n</jats:italic> </jats:sub> (1), (tbipH<jats:sub>2</jats:sub> = 5-(<jats:italic>tert</jats:italic>-butyl)isophthalic acid, DMI = 1,3-dimethyl-2-imidazolidinone), has been synthesized under “urea-thermal conditions” (i.e. in an excess of urea). Its structure has been determined by single-crystal X-ray diffraction analysis and further characterized by elemental analysis and IR spectra. Complex 1 crystallizes in the monoclinic space group <jats:italic>P</jats:italic>2<jats:sub>1</jats:sub>/<jats:italic>c</jats:italic> with <jats:italic>Z</jats:italic> = 4. In 1, the [tbip]<jats:sup>2−</jats:sup> ligand bridges the Mn(II) cations to form infinite chains, and the neighbouring chains are connected through [tbip]<jats:sup>2−</jats:sup> ligands into layers.","PeriodicalId":23831,"journal":{"name":"Zeitschrift für Naturforschung B","volume":"2 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140004312","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
Diguanidinium hexafluoridogermanate(IV) – an organic–inorganic hybrid salt with an antifluorite topology 六氟锗酸二胍(IV)--具有反氟石拓扑结构的有机-无机杂化盐
Pub Date : 2024-02-26 DOI: 10.1515/znb-2024-0007
Jutta Kösters, David Böhnisch, Thomas Jüstel, Rainer Pöttgen
Polycrystalline diguanidinium hexafluoridogermanate (IV) was obtained by co-precipitation from solutions of diguanidinium carbonate and germanium dioxide in 48 % hydrogen fluoride. The [C(NH2)3]2[GeF6] structure was refined from single crystal X-ray diffractometer data: [C(NH2)3]2[TiF6] type, C2/m, a = 1276.67(8), b = 732.70(5), c = 616.37(5) pm, b = 114.497(5)°, wR = 0.0700, 1033 F 2 values, 53 variables. The trigonal planar [C(NH2)3]+ cations and the octahedral [GeF6]2− anions are condensed to double layers through strong H⋯F hydrogen bonds (208–213 pm H⋯F). The centers of gravity of the two building units have an antifluorite-like topology.
通过碳酸二胍和二氧化锗溶液在 48% 氟化氢中的共沉淀,获得了多晶六氟化锗酸二胍 (IV)。[C(NH2)3]2[GeF6]的结构是根据单晶 X 射线衍射仪数据提炼出来的:[C(NH2)3]2[TiF6]型,C2/m,a = 1276.67(8),b = 732.70(5),c = 616.37(5) pm,b = 114.497(5)°,wR = 0.0700,1033 F 2 值,53 个变量。三方平面[C(NH2)3]+阳离子和八面体[GeF6]2-阴离子通过强 H⋯F 氢键(208-213 pm H⋯F)凝聚成双层。两个构建单元的重心具有类似反萤石的拓扑结构。
{"title":"Diguanidinium hexafluoridogermanate(IV) – an organic–inorganic hybrid salt with an antifluorite topology","authors":"Jutta Kösters, David Böhnisch, Thomas Jüstel, Rainer Pöttgen","doi":"10.1515/znb-2024-0007","DOIUrl":"https://doi.org/10.1515/znb-2024-0007","url":null,"abstract":"Polycrystalline diguanidinium hexafluoridogermanate (IV) was obtained by co-precipitation from solutions of diguanidinium carbonate and germanium dioxide in 48 % hydrogen fluoride. The [C(NH<jats:sub>2</jats:sub>)<jats:sub>3</jats:sub>]<jats:sub>2</jats:sub>[GeF<jats:sub>6</jats:sub>] structure was refined from single crystal X-ray diffractometer data: [C(NH<jats:sub>2</jats:sub>)<jats:sub>3</jats:sub>]<jats:sub>2</jats:sub>[TiF<jats:sub>6</jats:sub>] type, <jats:italic>C</jats:italic>2/<jats:italic>m</jats:italic>, <jats:italic>a</jats:italic> = 1276.67(8), <jats:italic>b</jats:italic> = 732.70(5), <jats:italic>c</jats:italic> = 616.37(5) pm, <jats:italic>b</jats:italic> = 114.497(5)°, w<jats:italic>R</jats:italic> = 0.0700, 1033 <jats:italic>F</jats:italic> <jats:sup>2</jats:sup> values, 53 variables. The trigonal planar [C(NH<jats:sub>2</jats:sub>)<jats:sub>3</jats:sub>]<jats:sup>+</jats:sup> cations and the octahedral [GeF<jats:sub>6</jats:sub>]<jats:sup>2−</jats:sup> anions are condensed to double layers through strong H⋯F hydrogen bonds (208–213 pm H⋯F). The centers of gravity of the two building units have an antifluorite-like topology.","PeriodicalId":23831,"journal":{"name":"Zeitschrift für Naturforschung B","volume":"23 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139978738","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
DyIrSn and the Lu3Co2In4-type stannides Sm3Rh2Sn4 and RE 3Ir2Sn4 (RE = Y, Sm, Gd–Tm, Lu) DyIrSn 和 Lu3Co2In4 型锡化物 Sm3Rh2Sn4 和 RE 3Ir2Sn4(RE = Y、Sm、Gd-Tm、Lu)
Pub Date : 2024-02-23 DOI: 10.1515/znb-2024-0004
Lars Schumacher, Aylin Koldemir, Rainer Pöttgen
The Lu3Co2In4-type stannides RE 3Ir2Sn4 (RE = Y, Sm, Gd–Tm, Lu) were synthesized from the elements by arc-melting and subsequent annealing sequences in sealed silica ampoules. For a more comprehensive phase analytical study, the isotypic stannide Sm3Rh2Sn4 and the ZrNiAl-type stannides DyIrSn and LT-YIrSn were also obtained. The polycrystalline samples were characterized through their X-ray powder patterns. The structures of DyIrSn and Gd3Ir2.63(2)Sn3.37(2) (ZrNiAl type, space group P6‾2m), Sm3Ir2.52(2)Sn3.48(1), Gd3Ir2.49(1)Sn3.51(1) and Tm3Ir2.20(3)Sn3.80(3) (Lu3Co2In4 type, space group P6‾) were refined from single-crystal X-ray diffractometer data, revealing residual Ir/Sn disorder in the low-symmetry variants. The RE 3Ir2Sn4 stannides are derived from the equiatomic stannides REIrSn (≍RE 3Rh3Sn3) by partial Ir/Sn substitution. The symmetry reduction from space group P6‾2m to P6‾ is forced by the Ir/Sn ordering within the RE 6 trigonal prisms. The new Sn2 position shows the rare motif of a trigonal planar tin coordination with 289 pm Sn2–Sn1 distances (data for Gd3Ir2.49(1)Sn3.51(1)). 119Sn Mössbauer spectra confirm the two crystallographically independent tin sites in Tm3Ir2Sn4 and the structural disorder in Gd3Ir2Sn4.
在密封的二氧化硅安瓿瓶中,通过电弧熔化和随后的退火顺序,从元素中合成了 Lu3Co2In4 型锡化物 RE 3Ir2Sn4(RE = Y、Sm、Gd-Tm、Lu)。为了进行更全面的相分析研究,还获得了同型锡化物 Sm3Rh2Sn4 和 ZrNiAl 型锡化物 DyIrSn 和 LT-YIrSn。通过 X 射线粉末图谱对多晶样品进行了表征。DyIrSn和Gd3Ir2.63(2)Sn3.37(2)(ZrNiAl型,空间群P6-2m)、Sm3Ir2.52(2)Sn3.48(1)、Gd3Ir2.49(1)Sn3.51(1)和Tm3Ir2.20(3)Sn3.80(3)(Lu3Co2In4 型,空间群 P6-‾)的单晶 X 射线衍射仪数据,揭示了低对称性变体中残余的 Ir/Sn 紊乱。RE 3Ir2Sn4 锡化物是从等原子锡化物 REIrSn (≍RE 3Rh3Sn3)中通过部分 Ir/Sn 置换得到的。空间群 P6‾2m 到 P6‾ 的对称性降低是由于 RE 6 三棱柱内的 Ir/Sn 排序所造成的。新的 Sn2 位置显示出 Sn2-Sn1 间距为 289 pm 的罕见的三叉平面锡配位图案(Gd3Ir2.49(1)Sn3.51(1) 的数据)。119Sn 莫斯鲍尔光谱证实了 Tm3Ir2Sn4 中两个晶体学上独立的锡位点以及 Gd3Ir2Sn4 中的结构紊乱。
{"title":"DyIrSn and the Lu3Co2In4-type stannides Sm3Rh2Sn4 and RE 3Ir2Sn4 (RE = Y, Sm, Gd–Tm, Lu)","authors":"Lars Schumacher, Aylin Koldemir, Rainer Pöttgen","doi":"10.1515/znb-2024-0004","DOIUrl":"https://doi.org/10.1515/znb-2024-0004","url":null,"abstract":"The Lu<jats:sub>3</jats:sub>Co<jats:sub>2</jats:sub>In<jats:sub>4</jats:sub>-type stannides <jats:italic>RE</jats:italic> <jats:sub>3</jats:sub>Ir<jats:sub>2</jats:sub>Sn<jats:sub>4</jats:sub> (<jats:italic>RE</jats:italic> = Y, Sm, Gd–Tm, Lu) were synthesized from the elements by arc-melting and subsequent annealing sequences in sealed silica ampoules. For a more comprehensive phase analytical study, the isotypic stannide Sm<jats:sub>3</jats:sub>Rh<jats:sub>2</jats:sub>Sn<jats:sub>4</jats:sub> and the ZrNiAl-type stannides DyIrSn and LT-YIrSn were also obtained. The polycrystalline samples were characterized through their X-ray powder patterns. The structures of DyIrSn and Gd<jats:sub>3</jats:sub>Ir<jats:sub>2.63(2)</jats:sub>Sn<jats:sub>3.37(2)</jats:sub> (ZrNiAl type, space group <jats:italic>P</jats:italic>6‾2<jats:italic>m</jats:italic>), Sm<jats:sub>3</jats:sub>Ir<jats:sub>2.52(2)</jats:sub>Sn<jats:sub>3.48(1)</jats:sub>, Gd<jats:sub>3</jats:sub>Ir<jats:sub>2.49(1)</jats:sub>Sn<jats:sub>3.51(1)</jats:sub> and Tm<jats:sub>3</jats:sub>Ir<jats:sub>2.20(3)</jats:sub>Sn<jats:sub>3.80(3)</jats:sub> (Lu<jats:sub>3</jats:sub>Co<jats:sub>2</jats:sub>In<jats:sub>4</jats:sub> type, space group <jats:italic>P</jats:italic>6‾) were refined from single-crystal X-ray diffractometer data, revealing residual Ir/Sn disorder in the low-symmetry variants. The <jats:italic>RE</jats:italic> <jats:sub>3</jats:sub>Ir<jats:sub>2</jats:sub>Sn<jats:sub>4</jats:sub> stannides are derived from the equiatomic stannides <jats:italic>RE</jats:italic>IrSn (≍<jats:italic>RE</jats:italic> <jats:sub>3</jats:sub>Rh<jats:sub>3</jats:sub>Sn<jats:sub>3</jats:sub>) by partial Ir/Sn substitution. The symmetry reduction from space group <jats:italic>P</jats:italic>6‾2<jats:italic>m</jats:italic> to <jats:italic>P</jats:italic>6‾ is forced by the Ir/Sn ordering within the <jats:italic>RE</jats:italic> <jats:sub>6</jats:sub> trigonal prisms. The new Sn2 position shows the rare motif of a trigonal planar tin coordination with 289 pm Sn2–Sn1 distances (data for Gd<jats:sub>3</jats:sub>Ir<jats:sub>2.49(1)</jats:sub>Sn<jats:sub>3.51(1)</jats:sub>). <jats:sup>119</jats:sup>Sn Mössbauer spectra confirm the two crystallographically independent tin sites in Tm<jats:sub>3</jats:sub>Ir<jats:sub>2</jats:sub>Sn<jats:sub>4</jats:sub> and the structural disorder in Gd<jats:sub>3</jats:sub>Ir<jats:sub>2</jats:sub>Sn<jats:sub>4</jats:sub>.","PeriodicalId":23831,"journal":{"name":"Zeitschrift für Naturforschung B","volume":"196 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139953195","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
Synthesis and characterization of bis[(dimethylphosphanylethynyl)dimethylsilyl]methane-digold(I) dichloride 双[(二甲基膦酰乙炔基)二甲基硅基]甲烷-二氯化金(I)的合成与表征
Pub Date : 2024-02-22 DOI: 10.1515/znb-2024-0005
Peter Heinrichs, Hans-Georg Stammler, Norbert W. Mitzel
The reaction of chlorodimethylphosphane with dilithiated bis(ethynyldimethylsilyl)methane leads to the corresponding bis[(dimethylphosphanylethynyl)dimethylsilyl]methane (1) which reacts readily with chloroauric acid in the presence of a reductant to form its dinuclear chlorogold(I) complex (2). The terminal chloride units of this compound can be substituted by reaction with nucleophiles. Furthermore, the metallophilic host functionality of the dinuclear complex 2 towards metallophilic atoms such as copper, silver, and thallium was tested. The crystal structure of bis[(dimethylphosphanylethynyl)dimethylsilyl]methane-digold(I) dichloride (2) is presented, which shows chains of the molecules aggregated by intermolecular aurophilic contacts.
氯二甲基膦与二乙炔基二甲基硅基甲烷反应生成相应的双[(二甲基膦乙炔基)二甲基硅基]甲烷 (1),该甲烷在还原剂存在下很容易与氯金酸反应生成其双核氯金(I)络合物 (2)。这种化合物的末端氯单元可以通过与亲核物反应进行取代。此外,还测试了双核络合物 2 对亲金属原子(如铜、银和铊)的亲金属宿主功能。图中展示了双[(二甲基膦酰乙炔基)二甲基硅基]甲烷-二氯化金(I)(2)的晶体结构,其中显示了分子链通过分子间的亲欧接触聚集在一起。
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引用次数: 0
Isopointal intermetallics: the cP24, dca phases as a representative set of examples, along with their vacancy-ordered variants β-Mn and SrSi2 等点状金属间化合物:以 cP24、dca 相为代表的一组实例,以及它们的空位有序变体 β-Mn 和 SrSi2
Pub Date : 2024-02-22 DOI: 10.1515/znb-2024-0002
Oliver Janka, Rainer Pöttgen
The crystal-chemical relationship of the cubic Laves phase MgCu2 (space group F d 3 $dbar{3}$ m, cF24) with the ternary phases Cd2Cu3In, Na2Au3Al, Mg2Rh3P, Li2Pd3B, Ag2Pd3S, Cu3Pt2B, Mo3Al2C, Mo3Ni2N, and V3Ga2N (subgroup P4132, cP24, dca) is discussed based on a group-subgroup scheme. The course of the lattice parameters and the free positional parameters show substantially different distortions and thus clear differences in chemical bonding, classifying these phases as isopointal rather than isotypic (usually they are all assigned to the Mo3Al2C type). The group-subgroup scheme further shows that the β-Mn and SrSi2 structures are vacancy-ordered variants of the cP24, dca phases. The structures of Mn3IrSi and LaIrSi (space group types P213; translationengleiche subgroups) are their ternary ordered versions.
立方拉维斯相 MgCu2(空间群 F d 3 ‾ $dbar{3}$ m,cF24)与三元相 Cd2Cu3In 的晶体化学关系、Na2Au3Al、Mg2Rh3P、Li2Pd3B、Ag2Pd3S、Cu3Pt2B、Mo3Al2C、Mo3Ni2N 和 V3Ga2N(子群 P4132,cP24,dca)的三元相进行了讨论。晶格参数和自由位置参数的变化过程显示出截然不同的畸变,因此化学键也有明显的差异,从而将这些相归类为等点型而非等型相(通常它们都被归类为 Mo3Al2C 型)。基团-亚基方案进一步表明,β-Mn 和 SrSi2 结构是 cP24、dca 相的空位有序变体。Mn3IrSi和LaIrSi(空间群类型P213;平移engleiche亚群)的结构是它们的三元有序版本。
{"title":"Isopointal intermetallics: the cP24, dca phases as a representative set of examples, along with their vacancy-ordered variants β-Mn and SrSi2","authors":"Oliver Janka, Rainer Pöttgen","doi":"10.1515/znb-2024-0002","DOIUrl":"https://doi.org/10.1515/znb-2024-0002","url":null,"abstract":"The crystal-chemical relationship of the cubic Laves phase MgCu<jats:sub>2</jats:sub> (space group <jats:italic>F</jats:italic> <jats:inline-formula> <jats:alternatives> <m:math xmlns:m=\"http://www.w3.org/1998/Math/MathML\" overflow=\"scroll\"> <m:mrow> <m:mi>d</m:mi> <m:mover accent=\"true\"> <m:mn>3</m:mn> <m:mo>‾</m:mo> </m:mover> </m:mrow> </m:math> <jats:tex-math> $dbar{3}$ </jats:tex-math> <jats:inline-graphic xmlns:xlink=\"http://www.w3.org/1999/xlink\" xlink:href=\"graphic/j_znb_2024-0002_ineq_101.png\" /> </jats:alternatives> </jats:inline-formula> <jats:italic>m</jats:italic>, <jats:italic>cF</jats:italic>24) with the ternary phases Cd<jats:sub>2</jats:sub>Cu<jats:sub>3</jats:sub>In, Na<jats:sub>2</jats:sub>Au<jats:sub>3</jats:sub>Al, Mg<jats:sub>2</jats:sub>Rh<jats:sub>3</jats:sub>P, Li<jats:sub>2</jats:sub>Pd<jats:sub>3</jats:sub>B, Ag<jats:sub>2</jats:sub>Pd<jats:sub>3</jats:sub>S, Cu<jats:sub>3</jats:sub>Pt<jats:sub>2</jats:sub>B, Mo<jats:sub>3</jats:sub>Al<jats:sub>2</jats:sub>C, Mo<jats:sub>3</jats:sub>Ni<jats:sub>2</jats:sub>N, and V<jats:sub>3</jats:sub>Ga<jats:sub>2</jats:sub>N (subgroup <jats:italic>P</jats:italic>4<jats:sub>1</jats:sub>32, <jats:italic>cP</jats:italic>24, <jats:italic>dca</jats:italic>) is discussed based on a group-subgroup scheme. The course of the lattice parameters and the free positional parameters show substantially different distortions and thus clear differences in chemical bonding, classifying these phases as isopointal rather than isotypic (usually they are all assigned to the Mo<jats:sub>3</jats:sub>Al<jats:sub>2</jats:sub>C type). The group-subgroup scheme further shows that the <jats:italic>β</jats:italic>-Mn and SrSi<jats:sub>2</jats:sub> structures are vacancy-ordered variants of the <jats:italic>cP</jats:italic>24, <jats:italic>dca</jats:italic> phases. The structures of Mn<jats:sub>3</jats:sub>IrSi and LaIrSi (space group types <jats:italic>P</jats:italic>2<jats:sub>1</jats:sub>3; <jats:italic>translationengleiche</jats:italic> subgroups) are their ternary ordered versions.","PeriodicalId":23831,"journal":{"name":"Zeitschrift für Naturforschung B","volume":"113 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139953160","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
Synthesis, crystal structure, DFT calculations, and Hirshfeld surface analysis of a chlorido-bridged 1D manganese(II) coordination polymer 氯桥 1D 锰(II)配位聚合物的合成、晶体结构、DFT 计算和 Hirshfeld 表面分析
Pub Date : 2024-02-19 DOI: 10.1515/znb-2023-0103
Chao Feng, Linlin Zhu, Jing-Jing Guo
A novel 1D Mn(II) coordination polymer, namely, [Mn3(bpz)2(MeCN)2Cl6] n (1) was synthesized by a solvothermal method based on bpz and MnCl2, where bpz is di(1H-pyrazol-1-yl)methane. The X-ray diffraction data show that the crystal structure of complex 1 is a one-dimensional polymer with two different coordination modes of the Mn(II) ions. The structure was modelled with Density Functional Theory (DFT) calculations and the intermolecular interactions were analyzed using the Hirshfeld surface method.
基于 bpz 和 MnCl2(其中 bpz 为二(1H-吡唑-1-基)甲烷),采用溶热法合成了一种新型一维锰(II)配位聚合物,即 [Mn3(bpz)2(MeCN)2Cl6] n (1)。X 射线衍射数据表明,复合物 1 的晶体结构是一种一维聚合物,其中 Mn(II)离子具有两种不同的配位模式。利用密度泛函理论(DFT)计算对该结构进行了建模,并采用 Hirshfeld 表面法对分子间的相互作用进行了分析。
{"title":"Synthesis, crystal structure, DFT calculations, and Hirshfeld surface analysis of a chlorido-bridged 1D manganese(II) coordination polymer","authors":"Chao Feng, Linlin Zhu, Jing-Jing Guo","doi":"10.1515/znb-2023-0103","DOIUrl":"https://doi.org/10.1515/znb-2023-0103","url":null,"abstract":"A novel 1D Mn(II) coordination polymer, namely, [Mn<jats:sub>3</jats:sub>(bpz)<jats:sub>2</jats:sub>(MeCN)<jats:sub>2</jats:sub>Cl<jats:sub>6</jats:sub>]<jats:sub> <jats:italic>n</jats:italic> </jats:sub> (1) was synthesized by a solvothermal method based on bpz and MnCl<jats:sub>2</jats:sub>, where bpz is di(1<jats:italic>H</jats:italic>-pyrazol-1-yl)methane. The X-ray diffraction data show that the crystal structure of complex 1 is a one-dimensional polymer with two different coordination modes of the Mn(II) ions. The structure was modelled with Density Functional Theory (DFT) calculations and the intermolecular interactions were analyzed using the Hirshfeld surface method.","PeriodicalId":23831,"journal":{"name":"Zeitschrift für Naturforschung B","volume":"36 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139924541","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
A plant cyclic nonapeptide of orbitide type: an electron density study 一种轨道型植物环状非肽:电子密度研究
Pub Date : 2024-02-15 DOI: 10.1515/znb-2023-0105
Peter Luger, Birger Dittrich, Heinz-Jürgen Schmidt
The electron density distribution (EDD) of a plant cyclic nonapeptide of orbitide type was studied. Crystal X-ray diffraction data was obtained from the Cambridge Structural Database (CSD) and refitted using scattering factors of the invariom library, thereby providing aspherical electron density. Bond topological, atomic properties and molecular surfaces (electrostatic potential and Hirshfeld surfaces) were derived. The partial double bond character of the peptide bond was confirmed by the ellipticity ε = 0.25. For eight N–H⋯O hydrogen bonds, atomic charges of contributing atoms differ depending on the type of the accepting oxygen atom. Atomic charge differences between negative main and positive side chains of this nonapeptide result in characteristic features of the electrostatic potential, which shows a positive isosurface around the molecule leading to repulsive interactions in the solid state structure. Weak intermolecular interactions are indicated by insignificant ED concentrations on the Hirshfeld surface except for weak signals at sites of intermolecular N–H⋯O and C–H⋯O hydrogen bonds.
研究了一种植物环状轨道肽的电子密度分布(EDD)。晶体 X 射线衍射数据来自剑桥结构数据库(CSD),并使用 invariom 库的散射因子进行了重新拟合,从而提供了非球面电子密度。得出了键拓扑、原子特性和分子表面(静电位和希尔施菲尔德表面)。椭圆度 ε = 0.25 证实了肽键的部分双键特性。对于 8 个 N-H⋯O 氢键,贡献原子的原子电荷因接受氧原子的类型而异。这种非肽的负主链和正侧链之间的原子电荷差异导致了静电位的特征,在固态结构中,分子周围出现了一个正等值面,导致排斥性相互作用。除了分子间 N-H⋯O 和 C-H⋯O 氢键处的微弱信号外,Hirshfeld 表面上的 ED 浓度并不明显,这表明分子间的相互作用较弱。
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引用次数: 0
The crystal structures and magnetic properties of YbMg0.75In1.25 and Yb6Mg6.41In5.59 YbMg0.75In1.25 和 Yb6Mg6.41In5.59 的晶体结构和磁性能
Pub Date : 2024-02-14 DOI: 10.1515/znb-2023-0106
Maximilian Kai Reimann, Rainer Pöttgen
The quasi-binary system YbMg2-YbIn2 was studied around the equiatomic composition. In contrast to the ordered rare earth (RE) phases REMgIn (ZrNiAl type), ytterbium forms phases with different structures and pronounced Mg/In mixing (M sites). The structures of YbMg0.75In1.25 (CaLiSn type, P3m1, a = 501.95(7), c = 1087.3(2) pm, wR2 = 0.0490, 790 F 2 values, 32 variables) and Yb6Mg6.41In5.59 (Yb6Ir5Ga7 type, P63/mcm, a = 1060.77(14), c = 970.27(16) pm, wR2 = 0.0484, 701 F 2 values, 26 variables) were refined from single-crystal X-ray diffractometer data. YbMg0.75In1.25 is an AlB2 superstructure with a tripling of the subcell. The magnesium and indium atoms form three differently puckered layers of M 6 hexagons. The Yb6Mg6.41In5.59 structure is derived from the hexagonal Laves phase YbMg2 (MgZn2 type, P63/mmc). A klassengleiche symmetry reduction leads to four crystallographically independent M sites for the rows of corner- and face-sharing tetrahedra which allow a composition close to the equiatomic one. The MM distances in both structures cover the broad range from 289 to 331 pm, comparable to the sums of the covalent radii. Temperature dependent magnetic susceptibility studies of the polycrystalline YbMg0.75In1.25 and Yb12Mg13In11 samples indicate Pauli paramagnetism with room temperature values of 2.8(1) × 10−3 emu mol−1 (YbMg0.75In1.25) and 5.2(1) × 10−3 emu mol−1 (Yb12Mg13In11).
围绕等原子成分对准二元体系 YbMg2-YbIn2 进行了研究。与有序稀土(RE)相 REMgIn(ZrNiAl 型)相反,镱形成的相具有不同的结构和明显的镁/铟混合(M 位点)。YbMg0.75In1.25 (CaLiSn 型,P3m1,a = 501.95(7),c = 1087.3(2) pm,wR2 = 0.0490,790 F 2 值,32 个变量)和 Yb6Mg6.41In5.59 (Yb6Ir5.59(Yb6Ir5Ga7 型,P63/mcm,a = 1060.77(14),c = 970.27(16) pm,wR2 = 0.0484,701 F 2 值,26 个变量)是根据单晶 X 射线衍射仪数据精制而成的。YbMg0.75In1.25 是一种 AlB2 超结构,其子单元增加了两倍。镁原子和铟原子形成三个不同的 M 6 六边形皱褶层。Yb6Mg6.41In5.59 结构源自六方拉维斯相 YbMg2(MgZn2 型,P63/mmc)。通过类对称性还原,在角和面共享四面体行中产生了四个晶体学上独立的 M 位点,从而使其成分接近于等原子。这两种结构中的 M-M 间距覆盖了从 289 到 331 pm 的宽广范围,与共价半径之和相当。对多晶 YbMg0.75In1.25 和 Yb12Mg13In11 样品进行的温度相关磁感应强度研究表明,它们具有保利顺磁性,室温值分别为 2.8(1) × 10-3 emu mol-1(YbMg0.75In1.25)和 5.2(1) × 10-3 emu mol-1(Yb12Mg13In11)。
{"title":"The crystal structures and magnetic properties of YbMg0.75In1.25 and Yb6Mg6.41In5.59","authors":"Maximilian Kai Reimann, Rainer Pöttgen","doi":"10.1515/znb-2023-0106","DOIUrl":"https://doi.org/10.1515/znb-2023-0106","url":null,"abstract":"The quasi-binary system YbMg<jats:sub>2</jats:sub>-YbIn<jats:sub>2</jats:sub> was studied around the equiatomic composition. In contrast to the ordered rare earth (<jats:italic>RE</jats:italic>) phases <jats:italic>RE</jats:italic>MgIn (ZrNiAl type), ytterbium forms phases with different structures and pronounced Mg/In mixing (<jats:italic>M</jats:italic> sites). The structures of YbMg<jats:sub>0.75</jats:sub>In<jats:sub>1.25</jats:sub> (CaLiSn type, <jats:italic>P</jats:italic>3<jats:italic>m</jats:italic>1, <jats:italic>a</jats:italic> = 501.95(7), <jats:italic>c</jats:italic> = 1087.3(2) pm, <jats:italic>wR</jats:italic>2 = 0.0490, 790 <jats:italic>F</jats:italic> <jats:sup>2</jats:sup> values, 32 variables) and Yb<jats:sub>6</jats:sub>Mg<jats:sub>6.41</jats:sub>In<jats:sub>5.59</jats:sub> (Yb<jats:sub>6</jats:sub>Ir<jats:sub>5</jats:sub>Ga<jats:sub>7</jats:sub> type, <jats:italic>P</jats:italic>6<jats:sub>3</jats:sub>/<jats:italic>mcm</jats:italic>, <jats:italic>a</jats:italic> = 1060.77(14), <jats:italic>c</jats:italic> = 970.27(16) pm, <jats:italic>wR</jats:italic>2 = 0.0484, 701 <jats:italic>F</jats:italic> <jats:sup>2</jats:sup> values, 26 variables) were refined from single-crystal X-ray diffractometer data. YbMg<jats:sub>0.75</jats:sub>In<jats:sub>1.25</jats:sub> is an AlB<jats:sub>2</jats:sub> superstructure with a tripling of the subcell. The magnesium and indium atoms form three differently puckered layers of <jats:italic>M</jats:italic> <jats:sub>6</jats:sub> hexagons. The Yb<jats:sub>6</jats:sub>Mg<jats:sub>6.41</jats:sub>In<jats:sub>5.59</jats:sub> structure is derived from the hexagonal Laves phase YbMg<jats:sub>2</jats:sub> (MgZn<jats:sub>2</jats:sub> type, <jats:italic>P</jats:italic>6<jats:sub>3</jats:sub>/<jats:italic>mmc</jats:italic>). A <jats:italic>klassengleiche</jats:italic> symmetry reduction leads to four crystallographically independent <jats:italic>M</jats:italic> sites for the rows of corner- and face-sharing tetrahedra which allow a composition close to the equiatomic one. The <jats:italic>M</jats:italic>–<jats:italic>M</jats:italic> distances in both structures cover the broad range from 289 to 331 pm, comparable to the sums of the covalent radii. Temperature dependent magnetic susceptibility studies of the polycrystalline YbMg<jats:sub>0.75</jats:sub>In<jats:sub>1.25</jats:sub> and Yb<jats:sub>12</jats:sub>Mg<jats:sub>13</jats:sub>In<jats:sub>11</jats:sub> samples indicate Pauli paramagnetism with room temperature values of 2.8(1) × 10<jats:sup>−3</jats:sup> emu mol<jats:sup>−1</jats:sup> (YbMg<jats:sub>0.75</jats:sub>In<jats:sub>1.25</jats:sub>) and 5.2(1) × 10<jats:sup>−3</jats:sup> emu mol<jats:sup>−1</jats:sup> (Yb<jats:sub>12</jats:sub>Mg<jats:sub>13</jats:sub>In<jats:sub>11</jats:sub>).","PeriodicalId":23831,"journal":{"name":"Zeitschrift für Naturforschung B","volume":"95 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139770540","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
Synthesis, anti-HIV and cytotoxicity evaluation of chiral 2,5-disubstituted 1,3,4-thiadiazole derivatives bearing the sulfonamide scaffold 带有磺酰胺支架的手性 2,5-二取代 1,3,4-噻二唑衍生物的合成、抗艾滋病毒和细胞毒性评估
Pub Date : 2024-02-13 DOI: 10.1515/znb-2023-0078
Anum Israr, Shahid Hameed, Najim A. Al-Masoudi
In the present study, chiral 2-(4-substiuted phenyl)amino-5-[1-(4-substituted benzenesulphonamido)alkyl]-1,3,4-thiazdiazoles 5a–x were synthesized from enantiopure l-amino acids in a multistep sequence. The starting acids were reacted with arylsulphonyl chlorides to produce N-arylsulfonyl amino acids 1a–h, followed by esterification to obtain the corresponding esters 2a–h. Treatment of esters with hydrazine hydrate afforded the corresponding hydrazides 3a–h. The coupling of hydrazides with aryl isothiocyanates followed by cyclization gave the target thiadiazoles 5a–x in good yields. The new synthesized compounds were assayed against HIV-1 and HIV-2 in MT-4 cells using MTT assay. Compounds 5s, 5v and 5w showed IC50 values of > 1.58, >1.98 and > 2.04 μm with SI > 1, respectively, indicating that these compounds were cytotoxic at concentrations values of 1.58, 1.98 and 2.04 μm, respectively.
在本研究中,手性 2-(4-取代苯基)氨基-5-[1-(4-取代苯磺酰胺基)烷基]-1,3,4-噻二唑 5a-x 以对映体纯 l-氨基酸为原料,通过多步骤合成。起始酸与芳基磺酰氯反应生成 N-芳基磺酰基氨基酸 1a-h,然后进行酯化反应得到相应的酯 2a-h。用肼水合物处理酯类可得到相应的肼 3a-h。酰肼与芳基异硫氰酸酯偶联后环化,得到目标噻二唑 5a-x,收率很高。利用 MTT 法检测了新合成化合物在 MT-4 细胞中对 HIV-1 和 HIV-2 的作用。化合物 5s、5v 和 5w 的 IC50 值分别为 1.58、1.98 和 2.04 μm(SI 值为 1),表明这些化合物在 1.58、1.98 和 2.04 μm 浓度下具有细胞毒性。
{"title":"Synthesis, anti-HIV and cytotoxicity evaluation of chiral 2,5-disubstituted 1,3,4-thiadiazole derivatives bearing the sulfonamide scaffold","authors":"Anum Israr, Shahid Hameed, Najim A. Al-Masoudi","doi":"10.1515/znb-2023-0078","DOIUrl":"https://doi.org/10.1515/znb-2023-0078","url":null,"abstract":"In the present study, chiral 2-(4-substiuted phenyl)amino-5-[1-(4-substituted benzenesulphonamido)alkyl]-1,3,4-thiazdiazoles 5a–x were synthesized from enantiopure <jats:sc>l-</jats:sc>amino acids in a multistep sequence. The starting acids were reacted with arylsulphonyl chlorides to produce <jats:italic>N</jats:italic>-arylsulfonyl amino acids 1a–h, followed by esterification to obtain the corresponding esters 2a–h. Treatment of esters with hydrazine hydrate afforded the corresponding hydrazides 3a–h. The coupling of hydrazides with aryl isothiocyanates followed by cyclization gave the target thiadiazoles 5a–x in good yields. The new synthesized compounds were assayed against HIV-1 and HIV-2 in MT-4 cells using MTT assay. Compounds 5s, 5v and 5w showed IC<jats:sub>50</jats:sub> values of &gt; 1.58, &gt;1.98 and &gt; 2.04 μ<jats:sc>m</jats:sc> with SI &gt; 1, respectively, indicating that these compounds were cytotoxic at concentrations values of 1.58, 1.98 and 2.04 μ<jats:sc>m</jats:sc>, respectively.","PeriodicalId":23831,"journal":{"name":"Zeitschrift für Naturforschung B","volume":"255 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139770503","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
Expansion and adaptation of the M5B12O25(OH) structure type to incorporate di- and trivalent transition metal cations 扩展和调整 M5B12O25(OH) 结构类型,以纳入二价和三价过渡金属阳离子
Pub Date : 2024-01-01 DOI: 10.1515/znb-2023-0082
Leonard C. Pasqualini, Martina Tribus, H. Huppertz
Abstract Five transition metal borates were synthesized in a Walker-type module under high-pressure/high-temperature conditions of 8–9 GPa and 800–1200 °C. They all exhibit the same interpenetrating, anionic borate network B12O2616−, crystallizing in the space group I41/acd, and therefore show high similarities to the borates Ti5B12O26 and Ga5B12O25(OH). Cr5B12O25(OH) and V5B12O25(OH) are isotypic to Ga5B12O25(OH), whereas Mn5Mn0.83B12O26 and Fe5Fe0.14B12O24.3(OH)1.7 feature the partial occupation of an additional, cuboctahedral cavity in the structure. This is due to a partial reduction of the cations to the oxidation state +2, as presented with the novel compound Mn5MnB12O22(OH)4, which only features Mn2+ for charge compensation. These structures feature a twelvefold coordination of manganese and iron.
摘要 在 8-9 GPa 和 800-1200 ℃ 的高压/高温条件下,通过沃克型模块合成了五种过渡金属硼酸盐。它们都表现出相同的互穿阴离子硼酸盐网络 B12O2616-,在空间群 I41/acd 中结晶,因此与硼酸盐 Ti5B12O26 和 Ga5B12O25(OH) 具有高度相似性。Cr5B12O25(OH) 和 V5B12O25(OH) 与 Ga5B12O25(OH) 同型,而 Mn5Mn0.83B12O26 和 Fe5Fe0.14B12O24.3(OH)1.7 的特点是在结构上部分占据了一个额外的立方八面体空腔。这是由于阳离子部分还原为氧化态 +2,如新型化合物 Mn5MnB12O22(OH)4,其电荷补偿特征仅为 Mn2+。这些结构的特点是锰和铁的十二倍配位。
{"title":"Expansion and adaptation of the M5B12O25(OH) structure type to incorporate di- and trivalent transition metal cations","authors":"Leonard C. Pasqualini, Martina Tribus, H. Huppertz","doi":"10.1515/znb-2023-0082","DOIUrl":"https://doi.org/10.1515/znb-2023-0082","url":null,"abstract":"Abstract Five transition metal borates were synthesized in a Walker-type module under high-pressure/high-temperature conditions of 8–9 GPa and 800–1200 °C. They all exhibit the same interpenetrating, anionic borate network B12O2616−, crystallizing in the space group I41/acd, and therefore show high similarities to the borates Ti5B12O26 and Ga5B12O25(OH). Cr5B12O25(OH) and V5B12O25(OH) are isotypic to Ga5B12O25(OH), whereas Mn5Mn0.83B12O26 and Fe5Fe0.14B12O24.3(OH)1.7 feature the partial occupation of an additional, cuboctahedral cavity in the structure. This is due to a partial reduction of the cations to the oxidation state +2, as presented with the novel compound Mn5MnB12O22(OH)4, which only features Mn2+ for charge compensation. These structures feature a twelvefold coordination of manganese and iron.","PeriodicalId":23831,"journal":{"name":"Zeitschrift für Naturforschung B","volume":"122 2","pages":"39 - 49"},"PeriodicalIF":0.0,"publicationDate":"2024-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139453813","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
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