TY - GEN A1 - Grunwald, Nicolas A1 - Kelling, Alexandra A1 - Holdt, Hans-Jürgen A1 - Schilde, Uwe T1 - The crystal structure of 1,1′-bisisoquinoline, C18H12N2 N2 - C18H12N2, tetragonal, I41/a (no. 88), a=13.8885(6) Å, c=13.6718(6) Å, V =2637.2(3) Å3, Z =8, Rgt(F)=0.0295, wRref(F2)=0.0854, T =210 K. CCDC no.: 631823 T3 - Zweitveröffentlichungen der Universität Potsdam : Mathematisch-Naturwissenschaftliche Reihe - 380 Y1 - 2017 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:517-opus4-401952 ER - TY - JOUR A1 - Grunwald, Nicolas A1 - Kelling, Alexandra A1 - Holdt, Hans-Jürgen A1 - Schilde, Uwe T1 - The crystal structure of 1,1′-bisisoquinoline, C18H12N2 JF - Zeitschrift für Kristallographie : international journal for structural, physical and chemical aspects of crystalline materials. New crystal structures N2 - C18H12N2, tetragonal, I41/a (no. 88), a=13.8885(6) Å, c=13.6718(6) Å, V =2637.2(3) Å3, Z =8, Rgt(F)=0.0295, wRref(F2)=0.0854, T =210 K. CCDC no.: 631823 Y1 - 2017 U6 - https://doi.org/10.1515/ncrs-2017-0088 VL - 232 IS - 5 SP - 839 EP - 841 PB - de Gruyter CY - Berlin ER - TY - JOUR A1 - Grunwald, Nicolas A1 - Kelling, Alexandra A1 - Holdt, Hans-Jürgen A1 - Schilde, Uwe T1 - The crystal structure of 1,1′-bisisoquinoline, C18H12N2 JF - Zeitschrift für Kristallographie : international journal for structural, physical and chemical aspects of crystalline materials ; New crystal structures N2 - C18H12N2, tetragonal, I4(1)/a (no. 88), a = 13.8885(6) angstrom, c = 13.6718(6) angstrom, V = 2637.2(3) angstrom(3), Z = 8, R-gt(F) = 0.0295, wR(ref)(F-2) = 0.0854, T = 210 K. Y1 - 2017 U6 - https://doi.org/10.1515/ncrs-2017-0088 SN - 1433-7266 VL - 232 SP - 839 EP - 841 PB - De Gruyter CY - Berlin ER - TY - JOUR A1 - Brietzke, Thomas Martin A1 - Dietz, Thomas A1 - Kelling, Alexandra A1 - Schilde, Uwe A1 - Bois, Juliana A1 - Kelm, Harald A1 - Reh, Manuel A1 - Schmitz, Markus A1 - Koerzdoerfer, Thomas A1 - Leimkühler, Silke A1 - Wollenberger, Ulla A1 - Krueger, Hans-Joerg A1 - Holdt, Hans-Jürgen T1 - The 1,6,7,12-Tetraazaperylene Bridging Ligand as an Electron Reservoir and Its Disulfonato Derivative as Redox Mediator in an Enzyme-Electrode Process JF - Chemistry - a European journal N2 - The homodinuclear ruthenium(II) complex [{Ru(l-N4Me2)}(2)(-tape)](PF6)(4) {[1](PF6)(4)} (l-N4Me2=N,N-dimethyl-2,11-diaza[3.3](2,6)-pyridinophane, tape=1,6,7,12-tetraazaperylene) can store one or two electrons in the energetically low-lying * orbital of the bridging ligand tape. The corresponding singly and doubly reduced complexes [{Ru(l-N4Me2)}(2)(-tape(.-))](PF6)(3) {[2](PF6)(3)} and [{Ru(l-N4Me2)}(2)(-tape(2-))](PF6)(2) {[3](PF6)(2)}, respectively, were electrochemically generated, successfully isolated and fully characterized by single-crystal X-ray crystallography, spectroscopic methods and magnetic susceptibility measurements. The singly reduced complex [2](PF6)(3) contains the -radical tape(.-) and the doubly reduced [3](PF6)(2) the diamagnetic dianion tape(2-) as bridging ligand, respectively. Nucleophilic aromatic substitution at the bridging tape in [1](4+) by two sulfite units gave the complex [{Ru(l-N4Me2)}(2){-tape-(SO3)(2)}](2+) ([4](2+)). Complex dication [4](2+) was exploited as a redox mediator between an anaerobic homogenous reaction solution of an enzyme system (sulfite/sulfite oxidase) and the electrode via participation of the low-energy *-orbital of the disulfonato-substituted bridging ligand tape-(SO3)(2)(2-) (E-red1=-0.1V versus Ag/AgCl/1m KCl in water). KW - electrochemistry KW - enzyme catalysis KW - N-ligands KW - redox-active ligands KW - ruthenium Y1 - 2017 U6 - https://doi.org/10.1002/chem.201703639 SN - 0947-6539 SN - 1521-3765 VL - 23 SP - 15583 EP - 15587 PB - Wiley-VCH CY - Weinheim ER - TY - JOUR A1 - Mondal, Suvendu Sekhar A1 - Hovestadt, Maximilian A1 - Dey, Subarna A1 - Paula, Carolin A1 - Glomb, Sebastian A1 - Kelling, Alexandra A1 - Schilde, Uwe A1 - Janiak, Christoph A1 - Hartmann, Martin A1 - Holdt, Hans-Jürgen T1 - Synthesis of a partially fluorinated ZIF-8 analog for ethane/ethene separation JF - CrystEngComm N2 - The separation of ethane/ethene mixtures (as well as other paraffin/olefin mixtures) is one of the most important but challenging processes in the petrochemical industry. In this work, we report the synthesis of ZIF-318, isostructural to ZIF-8 but built from the mixed linkers of 2-methylimidazole (L1) and 2-trifluoromethylimidazole (L2) (ZIF-318 = [(Zn(L1)(L2)](n)). The synthesis has been optimized to proceed without ZnO-formation. Using only the L2 linker under solvothermal conditions afforded ZnO-embedded in the H-bonded and non-porous coordination polymer ZnO@[Zn-2(L2)(2)(HCOO)(OH)](n). The slight differences in the size of the substituents (-CH3 vs. -CF3) possibly in combination with different electronic inductive effects led to small but significant changes to the pore size and properties respectively, though the effective pore opening (aperture) size of ZIF-318 remained the same in comparison with ZIF-8. ZIF-318 is chemically (boiling water, methanol, benzene, and wide pH range at room temperature for 1 day), thermally (up to 310 degrees C) stable, and more hydrophobic than ZIF-8 which is proven by contact angle measurement. ZIF-318 can be activated for N-2, CO2, CH4, H-2, ethane, ethane, propane, and propene gases sorptions. Consequently, in breakthrough experiments, the ethane/ethene mixtures can be separated. Y1 - 2017 U6 - https://doi.org/10.1039/c7ce01438d SN - 1466-8033 VL - 19 SP - 5882 EP - 5891 PB - Royal Society of Chemistry CY - Cambridge ER - TY - GEN A1 - Adamovich, Sergey N. A1 - Mirskova, Anna N. A1 - Mirskov, Rudolf G. A1 - Schilde, Uwe T1 - Synthesis and crystal structure of 1,4,10,13-tetraoxa-7,16-diazoniumcyclo-octadecane bis(4-chloro-2-methyl-phenoxyacetate) N2 - The title compound was prepared by the reaction of 1,4,10,13-tetraoxa-7,16-diazacyclo-octadecane with 4-chloro-2-methyl-phenoxyacetic acid in a ratio of 1:2. The structure has been proved by the data of elemental analysis, IR spectroscopy, NMR ( 1 H, 13 C) technique and by X-ray diffraction analysis. Intermolecular hydrogen bonds between the azonium protons and oxygen atoms of the carboxylate groups were found. Immunoactive properties of the title compound have been screened. The compound has the ability to suppress spontaneous and Con A-stimulated cell proliferation in vitro and therefore can be considered as immunodepressant. T3 - Zweitveröffentlichungen der Universität Potsdam : Mathematisch-Naturwissenschaftliche Reihe - 369 KW - salts Y1 - 2017 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:517-opus4-400905 ER - TY - GEN A1 - Mirskova, Anna N. A1 - Adamovich, Sergey N. A1 - Mirskov, Rudolf G. A1 - Schilde, Uwe T1 - Reaction of pharmacological active tris-(2-hydroxyethyl)ammonium 4-chlorophenylsulfanylacetate with ZnCl2 or NiCl2 BT - first conversion of a protic ionic liquid into metallated ionic liquid N2 - The reaction of pharmacological active protic ionic liquid tris-(2-hydroxyethyl)ammonium 4-chlorophenylsulfanylacetate H + N(CH 2 CH 2 OH) 3 ∙ ( - OOCCH 2 SC 6 H 4 Cl-4) (1) with zinc or nickel chloride in a ratio of 2:1 affords stable at room temperature powder-like adducts [H + N(CH 2 CH 2 OH) 3 ] 2 ∙ [M(OOCCH 2 SC 6 H 4 Cl-4) 2 Cl 2 ] 2- , M = Zn (2), Ni (3). By recrystallization from aqueous alcohol compound 2 unexpectedly gives Zn(OOCCH 2 SC 6 H 4 Cl-4) 2 ∙ 2H 2 O (4). Unlike 2, compound 3 gives crystals [N(CH 2 CH 2 OH) 3 ] 2 Ni 2+ · [ - OOCCH 2 SC 6 H 4 Cl-4] 2 (5), which have a structure of metallated ionic liquid. The structure of 5 has been proved by X-ray diffraction analysis. It is the first example of the conversion of a protic ionic liquid into potentially biological active metallated ionic liquid (1 → 3 → 5). T3 - Zweitveröffentlichungen der Universität Potsdam : Mathematisch-Naturwissenschaftliche Reihe - 377 KW - Formate KW - Salts KW - Acids Y1 - 2017 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:517-opus4-401099 ER - TY - GEN A1 - Zehbe, Kerstin A1 - Kollosche, Matthias A1 - Lardong, Sebastian A1 - Kelling, Alexandra A1 - Schilde, Uwe A1 - Taubert, Andreas T1 - Ionogels based on poly(methyl methacrylate) and metal-containing ionic liquids BT - correlation between structure and mechanical and electrical properties N2 - Ionogels (IGs) based on poly(methyl methacrylate) (PMMA) and the metal-containing ionic liquids (ILs) bis-1-butyl-3-methlimidazolium tetrachloridocuprate(II), tetrachloride cobaltate(II), and tetrachlorido manganate(II) have been synthesized and their mechanical and electrical properties have been correlated with their microstructure. Unlike many previous examples, the current IGs show a decreasing stability in stress-strain experiments on increasing IL fractions. The conductivities of the current IGs are lower than those observed in similar examples in the literature. Both effects are caused by a two-phase structure with micrometer-sized IL-rich domains homogeneously dispersed an IL-deficient continuous PMMA phase. This study demonstrates that the IL-polymer miscibility and the morphology of the IGs are key parameters to control the (macroscopic) properties of IGs. T3 - Zweitveröffentlichungen der Universität Potsdam : Mathematisch-Naturwissenschaftliche Reihe - 361 KW - microstructure KW - ionogels KW - ionic liquids KW - phase separation KW - mechanical properties KW - ionic conductivity Y1 - 2017 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:517-opus4-400607 ER - TY - JOUR A1 - Movahedifar, Fahimeh A1 - Modarresi-Alam, Ali Reza A1 - Kleinpeter, Erich A1 - Schilde, Uwe T1 - Dynamic H-1-NMR study of unusually high barrier to rotation about the partial C-N double bond in N,N-dimethyl carbamoyl 5-aryloxytetrazoles JF - Journal of molecular structure N2 - The synthesis of new N,N-dimethyl carbamoyl 5-aryloxytetrazoles have been reported. Their dynamic H-1-NMR via rotation about C-N bonds in moiety of urea group [a; CO-NMe2 and b; (2-tetrazolyl)N-CO rotations] in the solvents CDCl3 (223-333 K) and DMSO (298-363 K) is studied. Accordingly, the free energies of activation, obtained 16.5 and 16.9 kcal mol(-1) respectively, attributed to the conformational isomerization about the Me2N-C=O bond (a rotation). Moreover, a and b barrier to rotations in 5-((4-methylphenoxy)-N,N-dimethyl-2H-tetrazole-2-carboxamide (P) also were computed at level of B3LYP using 6-311++G** basis set. The optimized geometry parameters are in good agreement with X-ray structure data. The computation of energy barrier for a and b was determined 16.9 and 2.5 kcal mol(-1), respectively. The former is completely in agreement with the result obtained via dynamic NMR. X-ray structure analysis data demonstrate that just 2-acylated tetrazole was formed in the case of 5-(p-tolyloxy)-N,N-dimethyl-2H-tetrazole-2-carboxamide. X-ray data also revealed a planar trigonal orientation of the Me2N group which is coplanar to carbonyl group with the partial double-bond C-N character. It also demonstrates the synperiplanar position of C=O group with tetrazolyl ring. On average, in solution the plane containing carbonyl bond is almost perpendicular to the plane of the tetrazolyl ring (because of steric effects as confirmed by B3LY12/6-311++G**) while the plane containing Me2N group is coplanar with carbonyl bond which is in contrast with similar urea derivatives and it demonstrates the unusually high rotational energy barrier of these compounds. (C) 2016 Elsevier B.V. All rights reserved. KW - Dynamic H-1-NMR KW - Carbamoyl tetrazoles KW - Barrier to rotation about C-N bond KW - pi-Stacking KW - B3LYP/6-311++G** Y1 - 2017 U6 - https://doi.org/10.1016/j.molstruc.2016.12.010 SN - 0022-2860 SN - 1872-8014 VL - 1133 SP - 244 EP - 252 PB - Elsevier CY - Amsterdam ER - TY - JOUR A1 - Schilde, Uwe A1 - Paz, Christian A1 - Ortiz, Leandro T1 - Crystal structure of erioflorin isolated from Podanthus mitiqui (L.) JF - Acta Crystallographica Section E : Crystallographic Communications N2 - The title compound, erioflorin, C19H24O6 [systematic name: (1aR,3S,4Z,5aR,8aR,9R,10aR)-1a, 2,3,5a, 7,8,8a, 9,10,10a-decahydro-3-hydroxy-4,10a-dimethyl-8-methylidene-7-oxooxireno[5,6] cyclodeca[1,2-b]furan-9-yl methacrylate], is a tricyclic germacrane sesquiterpene lactone, which was isolated from Podanthus mitiqui (L.). The compound crystallizes in the space group P2(1)2(1)2(1), and its molecular structure consists of a methacrylic ester of a ten-membered ring sesquiterpenoid annelated with an epoxide and a butyrolactone. The structure is stabilized by one intramolecular C-H center dot center dot center dot O hydrogen bond. An O-H center dot center dot center dot O hydrogen bond and further C-H center dot center dot center dot O interactions can be observed in the packing. KW - crystal structure KW - germacrane sesquiterpene lactone KW - Podanthus mitiqui Y1 - 2017 U6 - https://doi.org/10.1107/S2056989017001700 VL - 73 IS - 3 SP - 334 EP - 337 PB - International Union of Crystallography CY - Chester ER -