TY - JOUR A1 - Holdt, Hans-Jürgen A1 - Müller, Holger A1 - Potter, Matthias A1 - Kelling, Alexandra A1 - Schilde, Uwe A1 - Starke, Ines A1 - Heydenreich, Matthias A1 - Kleinpeter, Erich T1 - The first sandwich complex with an octa(thioether) coordination sphere : Bis(maleonitrile-tetrathia-12-crown- 4)silver(I) N2 - The new tetrathiacrown ethers maleonitrile-tetrathia-12-crown-4 (mn12S(4)) and maleonitrile-tetrathia-13-crown- 4 (mn13S(4)) have been prepared and characterised by X-ray crystallographic analysis. These crown ethers form 2:1, 3:2 and 1: 1 complexes with AgY (Y = BF4, PF6). The crystal structures of [Ag(mn12S(4))(2)]BF4 (3a), [Ag(mn13S(4))(2)]BF4 (4a) and [Ag-2(mn13S(4))(3)](PF6)(2) (6b) have been determined. Compound 3a contains the centrosymmetric sandwich complex cation [Ag(mn12S(4))(2)](+) where each mn12S(4) ligand is coordinated to the Ag centre in an endo manner through all four S atoms. The 2:1 complex [Ag(mn12S(4))(2)](+) is the first sandwich complex with a tetrathiacrown ether and the first complex with an octa(thioether) coordination sphere. The crystal structure of compound 4a also reveals a 2:1 complex. This complex, [Ag(mnl3S(4))(2)](+), exhibits a half-sandwich structure. One mn13S(4) ligand coordinates to Ag+ by all four S donor atoms and the other 13S(4) crown by only one S atom. Compound 6b contains a dinuclear Ag complex. The Ag complexes 3a,b-8a,b were also studied by electrospray ionisation mass spectrometry. Collision-induced dissociation (CID) was used to compare the relative stability of 2:1 complexes [AgL2]+ and 1:1 complexes [AgL](+) (L = mn12S(4), mn13S(4)). The C-13 NMR chemical shifts of 2:1 and 1:1 Ag complexes and their corresponding free ligands were also estimated and compared. The free energy of the barrier of ring inversion (Delta G(double dagger)) for [Ag(mn12S(4))(2)](+) was determined to be 64 kJmol(-1). Y1 - 2006 UR - http://www3.interscience.wiley.com/cgi-bin/jhome/27721/ U6 - https://doi.org/10.1002/ejic.200501109 SN - 1434-1948 ER - TY - JOUR A1 - Hahn, Simone A1 - Kelling, Alexandra A1 - Schilde, Uwe A1 - Holdt, Hans-Jürgen T1 - Crystal structure of bis(2-ethylthiomethylpyridine)platinum(II) hexachloroplatinate, [Pt(C8H11NS)2][PtCl6] N2 - C16H22Cl6N2Pt2S2, orthorhombic, Pbca (no. 61), a = 15.5660(8) angstrom, b = 17.4892(9) angstrom, c = 18.161 (1) angstrom, V = 4944. 1 angstrom(3), Z = 8, R-gt(F) = 0.030, wR(ref)(F-2) = 0.055, T = 210 K. Y1 - 2008 UR - http://zkrist_ncs.cpfs.mpg.de/pdf223-4/216_1267-2377.pdf U6 - https://doi.org/10.1524/ncrs.2008.0216 SN - 1433-7266 ER - TY - JOUR A1 - Schilde, Uwe A1 - Erk, Çakil A1 - Kleinpeter, Erich T1 - The crystal and molecular structures of sodium and barium complexes of dibenzo-24-crown-8 ether N2 - The sodium and barium isothiocyanate complexes of 6,7,9,10,12,13,20,21,23,24,26,27-dodecahydrodibenzo[b,n]- 1,4,7,10,13,16,19,22-octaoxacyclotetracosin (dibenzo-24-crown-8 ether = DB24C8) were synthesized and analyzed by X-ray diffraction. The sodium complex, [Na(DB24C8)(NCS)(H2O)] 1, crystallizes in the orthorhombic space group Fdd2 with 16 molecules in the unit cell. The coordination number of Na is 6 and the central ion is located in a distorted octahedric environment. Only four of the crown ether oxygen atoms are involved. The coordination polyhedron is completed by the isothiocanate anion and by a water molecule, which is stabilized by hydrogen bonds. The barium complex, [Ba(DB24C8)(NCS)(2)] 2, crystallizes in the trigonale space group P3(1)21 with 3 molecules in the unit cell. Crystallographic C-2 symmetry is observed for the complex. The coordination number of Ba is 10. Barium is coordinated with the eight oxygen atoms of the macrocyclic ligand and with two isothiocyanate anions. The absolute structure was estimated using the FLACK parameter Y1 - 2006 U6 - https://doi.org/10.1524/zkri.2006.221.3.231 ER - TY - JOUR A1 - Starke, Ines A1 - Kammer, Stefan A1 - Grunwald, Nicolas A1 - Schilde, Uwe A1 - Holdt, Hans-Jürgen A1 - Kleinpeter, Erich T1 - Complexation of diazaperylene and bisisoquinoline with transition metal ions in the gas phase studied by electrospray ionization mass spectrometry N2 - The complex formation of the ligands 1,12-diazaperylene (dap), 1,1-bisisoquinoline (bis), 2,2-bipyridine (bpy) and 1,10-phenanthroline (phen) with transition metal ions (M = Fe, Co, Ni, Cu, Zn, Ru, Os, Re, Pd, Pt, Ag and Cd) in the gas phase has been studied by electrospray ionization mass spectrometry. With the exception of Ru, Os, Fe, Ni and Cu, singly charged complexes [MLn]+ (n = 1,2) were observed. The complexes of dap and bis with Ru, Os, Fe and Ni ions, and the mixed ligand complexes with bpy and phen, are preferably of the doubly charged type [ML3]2+. In addition, collision- induced dissociation (CID) measurements were employed to evaluate the relative stabilities of these complexes. The CID experiments of mixed-ligand complexes which contain both dap and phen or dap and bpy exhibit preferential elimination of bpy, indicating that bpy is a weaker ligand than phen and dap. Y1 - 2008 ER - TY - JOUR A1 - Schilde, Uwe A1 - Kelling, Alexandra A1 - Umbreen, Sumaira A1 - Linker, Torsten T1 - Crystal structures of three bicyclic carbohydrate derivatives JF - Acta crystallographica Section E ; Crystallographic communications N2 - The title compounds, [(1R,3R,4R,5R,6S)-4,5-bis(acetyloxy)-7-oxo-2-oxabicyclo- [4.2.0]octan-3-yl]methyl acetate, C14H18O8, (I), [(1S,4R,5S,6R)-5-acetyloxy-7- hydroxyimino-2-oxobicyclo[4.2.0]octan-4-yl acetate, C11H15NO6, (II), and [(3aR,5R,6R,7R,7aS)-6,7-bis(acetyloxy)-2-oxooctahydropyrano[3,2-b]pyrrol-5- yl]methyl acetate, C14H19NO8, (III), are stable bicyclic carbohydrate derivatives. They can easily be synthesized in a few steps from commercially available glycals. As a result of the ring strain from the four-membered rings in (I) and (II), the conformations of the carbohydrates deviate strongly from the ideal chair form. Compound (II) occurs in the boat form. In the five-membered lactam (III), on the other hand, the carbohydrate adopts an almost ideal chair conformation. As a result of the distortion of the sugar rings, the configurations of the three bicyclic carbohydrate derivatives could not be determined from their NMR coupling constants. From our three crystal structure determinations, we were able to establish for the first time the absolute configurations of all new stereocenters of the carbohydrate rings. KW - crystal structure KW - carbohydrate deriv­atives KW - conformation KW - configuration Y1 - 2016 U6 - https://doi.org/10.1107/S2056989016018727 SN - 2056-9890 VL - 72 IS - 12 SP - 1839 EP - 1844 PB - IUCR CY - Chester ER - TY - GEN A1 - Schilde, Uwe A1 - Kelling, Alexandra A1 - Umbreen, Sumaira A1 - Linker, Torsten T1 - Crystal structures of three bicyclic carbohydrate derivatives N2 - The title compounds, [(1R,3R,4R,5R,6S)-4,5-bis­(acet­yloxy)-7-oxo-2-oxabi­cyclo[4.2.0]octan-3-yl]methyl acetate, C14H18O8, (I), [(1S,4R,5S,6R)-5-acet­yloxy-7-hy­droxy­imino-2-oxobi­cyclo­[4.2.0]octan-4-yl acetate, C11H15NO6, (II), and [(3aR,5R,6R,7R,7aS)-6,7-bis­(acet­yloxy)-2-oxo­octa­hydro­pyrano[3,2-b]pyrrol-5-yl]methyl acetate, C14H19NO8, (III), are stable bicyclic carbohydrate derivatives. They can easily be synthesized in a few steps from commercially available glycals. As a result of the ring strain from the four-membered rings in (I) and (II), the conformations of the carbohydrates deviate strongly from the ideal chair form. Compound (II) occurs in the boat form. In the five-membered lactam (III), on the other hand, the carbohydrate adopts an almost ideal chair conformation. As a result of the distortion of the sugar rings, the configurations of the three bicyclic carbohydrate derivatives could not be determined from their NMR coupling constants. From our three crystal structure determinations, we were able to establish for the first time the absolute configurations of all new stereocenters of the carbohydrate rings. T3 - Zweitveröffentlichungen der Universität Potsdam : Mathematisch-Naturwissenschaftliche Reihe - 296 KW - crystal structure KW - carbohydrate deriv­atives KW - conformation KW - configuration Y1 - 2016 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:517-opus4-100833 ER - TY - GEN A1 - Winter, Alette A1 - Thiel, Kerstin A1 - Zabel, André A1 - Klamroth, Tillmann A1 - Pöppl, Andreas A1 - Kelling, Alexandra A1 - Schilde, Uwe A1 - Taubert, Andreas A1 - Strauch, Peter T1 - Tetrahalidocuprates(II) – structure and EPR spectroscopy BT - Part 2: tetrachloridocuprates(II) N2 - We present and discuss the results of crystallographic and electron paramagnetic resonance (EPR) spectroscopic analyses of five tetrachloridocuprate(II) complexes to supply a useful tool for the structural characterisation of the [CuCl4]2− moiety in the liquid state, for example in ionic liquids, or in solution. Bis(benzyltriethylammonium)-, bis(trimethylphenylammonium)-, bis(ethyltriphenylphosphonium)-, bis(benzyltriphenylphosphonium)-, and bis(tetraphenylarsonium)tetrachloridocuprate(II) were synthesised and characterised by elemental, IR, EPR and X-ray analyses. The results of the crystallographic analyses show distorted tetrahedral coordination geometry of all [CuCl4]2− anions in the five complexes and prove that all investigated complexes are stabilised by hydrogen bonds of different intensities. Despite the use of sterically demanding ammonium, phosphonium and arsonium cations to obtain the separation of the paramagnetic Cu(II) centres for EPR spectroscopy no hyperfine structure was observed in the EPR spectra but the principal values of the electron Zeeman tensor, g∥ and g⊥, could be determined. With these EPR data and the crystallographic parameters we were able to carry out a correlation study to anticipate the structural situation of tetrachloridocuprates in different physical states. This correlation is in good agreement with DFT calculations. T3 - Zweitveröffentlichungen der Universität Potsdam : Mathematisch-Naturwissenschaftliche Reihe - 240 KW - electron-spin resonance KW - liquid-crystal precursors KW - copper(II) halide salts KW - ionic liquid KW - square planar KW - tetrachlorocuprate(II) salts KW - molecular-structure KW - magnetic-properties KW - paramagnetic-resonance KW - temperature phase Y1 - 2013 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:517-opus4-95012 SP - 1019 EP - 1030 ER - TY - GEN A1 - Mondal, Suvendu Sekhar A1 - Bhunia, Asamanjoy A1 - Demeshko, Serhiy A1 - Kelling, Alexandra A1 - Schilde, Uwe A1 - Janiak, Christoph A1 - Holdt, Hans-Jürgen T1 - Synthesis of a Co(II)–imidazolate framework from an anionic linker precursor BT - gas-sorption and magnetic properties N2 - A Co(II)–imidazolate-4-amide-5-imidate based MOF, IFP-5, is synthesized by using an imidazolate anion-based novel ionic liquid as a linker precursor under solvothermal conditions. IFP-5 shows significant amounts of gas (N2, CO2, CH4 and H2) uptake capacities. IFP-5 exhibits an independent high spin Co(II) centre and antiferromagnetic coupling. T3 - Zweitveröffentlichungen der Universität Potsdam : Mathematisch-Naturwissenschaftliche Reihe - 235 KW - building-blocks KW - carbon-dioxide capture KW - exchange KW - ionic liquids KW - ionothermal synthesis KW - ligand KW - metal-organic frameworks KW - solvent KW - surface KW - zeolitic imidazolate frameworks Y1 - 2013 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:517-opus4-94424 SP - 39 EP - 42 ER - TY - GEN A1 - Mondal, Suvendu Sekhar A1 - Dey, Subarna A1 - Baburin, Igor A. A1 - Kelling, Alexandra A1 - Schilde, Uwe A1 - Seifert, Gotthard A1 - Janiak, Christoph A1 - Holdt, Hans-Jürgen T1 - Syntheses of two imidazolate-4-amide-5-imidate linker-based hexagonal metal–organic frameworks with flexible ethoxy substituent N2 - A rare example of in situ linker generation with the formation of soft porous Zn- and Co-MOFs (IFP-9 and -10, respectively) is reported. The flexible ethoxy groups of IFP-9 and -10 protrude into the 1D hexagonal channels. The gas-sorption behavior of both materials for H2, CO2 and CH4 showed wide hysteretic isotherms, typical for MOFs having a flexible substituent which can give rise to a gate effect. T3 - Zweitveröffentlichungen der Universität Potsdam : Mathematisch-Naturwissenschaftliche Reihe - 234 KW - adsorption KW - behavior KW - carbon-dioxide KW - crystals KW - gases KW - ligand KW - pressure KW - selectivity KW - temperature KW - zinc Y1 - 2013 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:517-opus4-94360 SP - 9394 EP - 9399 ER - TY - GEN A1 - Mondal, Suvendu Sekhar A1 - Bhunia, Asamanjoy A1 - Baburin, Igor A. A1 - Jäger, Christian A1 - Kelling, Alexandra A1 - Schilde, Uwe A1 - Seifert, Gotthard A1 - Janiak, Christoph A1 - Holdt, Hans-Jürgen T1 - Gate effects in a hexagonal zinc-imidazolate-4-amide-5-imidate framework with flexible methoxy substituents and CO2 selectivity N2 - A new imidazolate-4-amide-5-imidate based MOF, IFP-7, is generated, having flexible methoxy groups, which act as molecular gates for guest molecules. This allows highly selective CO2 sorption over N2 and CH4 gases. T3 - Zweitveröffentlichungen der Universität Potsdam : Mathematisch-Naturwissenschaftliche Reihe - 233 KW - adsorption KW - capacity KW - carbon-dioxide capture KW - coordination polymer KW - flexibility KW - hydrogen storage KW - ligand KW - metal-organic frameworks KW - mixed-matrix membranes KW - separation Y1 - 2013 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:517-opus4-94341 SP - 7599 EP - 7601 ER -