@article{AwadConradKochetal.2010, author = {Awad, Duha Jawad and Conrad, Franziska and Koch, Andreas and Schilde, Uwe and Poeppl, Andreas and Strauch, Peter}, title = {1,10-phenanthroline-dithiolate mixed ligand transition metal complexes : synthesis, characterization and EPR spectroscopy}, issn = {0020-1693}, doi = {10.1016/j.ica.2010.01.021}, year = {2010}, abstract = {A series of new N2S2 mixed ligand transition metal complexes, where N-2 is phenanthroline and S-2 is 1,2- dithiooxalate (dto) or 1,2-dithiosquarate (dtsq), has been synthesized and characterized. IR spectra reveal that the 1,2- dithiolate ligands are coordinated via the sulfur atoms forming a N2S2 coordination sphere. The copper(II) complex [Cu(phen)(dto)] was studied by EPR spectroscopy as a diamagnetically diluted powder. The diamagnetic dilution resulted from doping of the copper complex into the isostructural host lattice of the nickel complex [Ni(phen)(dto)]. The electronic situation in the frontier orbitals of the copper complex calculated from the experimental data is compared to the results of EHT and DFT calculations. Furthermore, one side product, chlorobis(1,10-phenanthroline)copper(I) ethanol solvate hydrate [(phen)(2)CuCl]center dot C2H5OH center dot H2O, was formed by a reduction process and characterized by X-ray diffraction. In the crystal packing one-dimensional columns of dimers are formed, stabilized by significant pi-pi interactions.}, language = {en} } @article{KammerStarkePietruchaetal.2012, author = {Kammer, Stefan and Starke, Ines and Pietrucha, Andreas and Kelling, Alexandra and Mickler, Wulfhard and Schilde, Uwe and Dosche, Carsten and Kleinpeter, Erich and Holdt, Hans-J{\"u}rgen}, title = {1,12-Diazaperylene and 2,11-dialkylated-1,12-diazaperylene iridium(III) complexes [Ir((CN)-N-boolean AND)(2)((NN)-N-boolean AND)]PF6: new supramolecular assemblies}, series = {Dalton transactions : a journal of inorganic chemistry, including bioinorganic, organometallic, and solid-state chemistry}, volume = {41}, journal = {Dalton transactions : a journal of inorganic chemistry, including bioinorganic, organometallic, and solid-state chemistry}, number = {34}, publisher = {Royal Society of Chemistry}, address = {Cambridge}, issn = {1477-9226}, doi = {10.1039/c2dt30412k}, pages = {10219 -- 10227}, year = {2012}, abstract = {A series of new monocationic iridium(III) complexes [Ir((CN)-N-boolean AND)(2)((NN)-N-boolean AND)]PF6 with "large-surface" alpha,alpha'-diimin ligands (NN)-N-boolean AND (dap = 1,12-diazaperylene, dmedap = 2,11-dimethyl-1,12-diazaperylene, dipdap = 2,11-diisopropyl-1,12-diazaperylene) and different cyclometalating ligands (CN)-N-boolean AND (piq = 1-phenylisoquinoline, bzq = benzo[h]quinoline, ppz = 1-phenylpyrazole, thpy = 2-(2-thienyl)pyridine, ppy = 2-phenylpyridine, meppy = 2-(4-methylphenyl)pyridine, dfppy = 2-(2,4-difluorophenyl)pyridine) were synthesized. The solid structures of the complexes [Ir(piq)(2)(dap)]PF6, [Ir(bzq)(2)(dap)]PF6, [Ir(ppy)(2)(dipdap)]PF6, [Ir(piq)(2)(dmedap)]PF6, [Ir(ppy)(2)(dap)]PF6 and [Ir(ppz)(2)(dap)]PF6 are reported. In [Ir(piq)(2)(dap)]PF6, the dap ligand and one of the piq ligands of each cationic complex are involved in pi-pi stacking interactions forming supramolecular channels running along the crystallographic c axis. In the crystalline [Ir(bzq)(2)(dap)]PF6 pi-pi stacking interactions between the metal complexes lead to the formation of a 2D layer structure. In addition, CH-pi interactions were found in all compounds, which are what stabilizes the solid structure. In particular, a significant number of them were found in [Ir(piq)(2)(dap)]PF6 and [Ir(bzq)(2)(dap)]PF6. The crystal structures of [Ir(ppy)(2)(dipdap)]PF6 and [Ir(ppy)(2)(dmedap)]PF6 are also presented, being the first examples of bis-cyclometalated iridium(III) complexes with phenanthroline-type alpha,alpha'-diimin ligands bearing bulky alkyl groups in the neighbourhood of the N-donor atoms. These ligands implicate a distorted octahedral coordination geometry that in turn destabilized the Ir-N-N boolean AND N bonds. The new iridium (III) complexes are not luminescent. All compounds show an electrochemically irreversible anodic peak between 1.15 and 1.58 V, which is influenced by the different cyclometalated ligands. All of the new complexes show two reversible successive one-electron "large-surface" ligand-centred reductions around -0.70 V and -1.30 V. Electrospray ionisation mass spectrometry (ESI-MS) and collision induced decomposition (CID) measurements were used to investigate the stability of the new complexes. Thereby, the stability agreed well with the order of the Ir-N-N boolean AND N bond lengths.}, language = {en} } @article{WenzelWehseSchildeetal.2004, author = {Wenzel, Barbara and Wehse, Burkhard and Schilde, Uwe and Strauch, Peter}, title = {1,2-Dithioquadratato- und 1,2-Dithiooxalatoindate(III) = 1,2-dithiosquarato- and 1,2-dithiooxalatoindates(III)}, year = {2004}, abstract = {Indium(III) chloride forms in water with potassium 1,2-dithiooxalate (dto) and potassium 1,2-dithiosquarate (dtsq) stable coordination compounds. Due to the higher bridging ability of the 1,2-dithiooxalate ligand in all cases only thiooxalate bridged binuclear complexes were found. From 1,2-dithioquadratate with an identical donor atom set mononuclear trischelates could be isolated. Five crystalline complexes, (BzlMe(3)N)(4)[(dto)(2)In(dto)In(dto)(2)] (1), (BzlPh(3)P)(4)[(dto)(2)In(dto)In(dto)(2)] (2), (BzlMe(3)N)(3)[In(dtsq)(3)] (3), (Bu4N)(3)[In(dtsq)(3)] (4) and (Ph4P)[In(dtsq)(2)(DMF)(2)] (5), have been isolated and characterized by X-ray analyses. Due to the type of the complex and the cations involved these compounds crystallize in different space groups with the following parameters: 1, monoclinic in P2(1)/c with a = 14.4035(5) Angstrom, b = 10.8141(5) Angstrom, c = 23.3698(9) Angstrom, beta = 124.664(2)degrees, and Z = 2; 2, triclinic in P (1) over bar with a = 11.3872(7) Angstrom, b = 13.6669(9) Angstrom, c = 17.4296(10) Angstrom, alpha = 88.883(5)degrees, beta = 96.763(1)degrees, gamma = 74.587(5)degrees, and Z = 1; 3, hexagonal in R3 with a = 20.6501(16) Angstrom, b = 20.6501(16) Angstrom, c = 19.0706(13) Angstrom and Z = 6; 4, monoclinic in P21/c with a = 22.7650(15) Angstrom, b = 20.4656(10) Angstrom, c = 14.4770(9) Angstrom, P}, language = {de} } @article{PoleschnerHeydenreichSchilde2000, author = {Poleschner, Helmut and Heydenreich, Matthias and Schilde, Uwe}, title = {13C, 19F and 77Se NMR study of vicinal (E)-fluoro(organylseleno)olefins and [(E)- fluoroalkenyl]diorganylselenonium salts}, year = {2000}, abstract = {Selenides of the type R1Se-EMe3 (E = Si, Ge, Sn, Pb) react with xenon difluoride by cleavage of the Se-E bond to yield the R1Se-F intermediate and the fluorides Me3E-F, whereas the Se-C bond in PhSe-tBu (E = C) is stable against XeF2. The presence of R1Se-F intermediates is confirmed by addition to acetylenes (4-octyne, 3-hexyne). Thus, the fluoroselenenylation of acetylenes gives fluoro(organylseleno)olefins in preparative yields. In the cases of E = Si, Ge, Sn, and Pb, aryl and n-alkyl groups are suitable as the substituent R1. The X-ray crystal structural analysis of (E)-3- (p-carboxyphenylseleno)-4-fluorohex-3-ene - the first example of an uncharged fluoroselenoolefin synthesized from p- EtO2C-C6H4-Se-SnMe3, XeF2, and 3-hexyne followed by an ester hydrolysis - shows that the addition of the selenenylfluoride intermediate to the acetylene proceeds via a trans-addition, as is known for the R2Se2-XeF2 reagents.}, language = {en} } @article{AwadSchildeStrauch2011, author = {Awad, Duha Jawad and Schilde, Uwe and Strauch, Peter}, title = {4,4 '-Bis(tert-butyl)-2,2 '-bipyridinedichlorometal(II) - Synthesis, structure and EPR spectroscopy}, series = {Inorganica chimica acta : the international inorganic chemistry journal}, volume = {365}, journal = {Inorganica chimica acta : the international inorganic chemistry journal}, number = {1}, publisher = {Elsevier}, address = {Lausanne}, issn = {0020-1693}, doi = {10.1016/j.ica.2010.08.035}, pages = {127 -- 132}, year = {2011}, abstract = {Due to the better solubility of the 4,4'-substituted bipyridine ligand a series of 4,4'0-bis(tert-butyl)-2,2'-bipyridinedichlorometal(II) complexes, [M(tbbpy)Cl(2)], with M = Cu, Ni, Zn, Pd, Pt was synthesised and characterised. The blue copper complex 4,4'-bis(tert-butyl)-2,2'-bipyridinedichlorocopper(II) was isolated in two different polymorphic forms, as prisms 1 with a solvent inclusion and solvent-free as needles 2. Both structures were determined by X-ray structure analysis. They crystallise in the monoclinic space group P2(1)/c with four molecules in the unit cell, but with different unit cells and packing motifs. Whereas in the prisms 1, with the unit cell parameters a = 12.1613(12), b = 10.6363(7), c = 16.3074(15) angstrom, eta = 94.446(8)degrees, the packing is dominated by intra-and intermolecular hydrogen bonds, in the needles 2, with a = 7.738(1), b = 18. 333(2), c = 13.291(3) angstrom, beta = 97.512(15)degrees, only intramolecular hydrogen bonds appear and the complex molecules are arranged in columns which are stabilised by p-p-stacking interactions. In both complexes the copper has a tetrahedrally distorted coordination sphere. These copper complexes were also studied by EPR spectroscopy in solution, as frozen glass and diamagnetically diluted powder with the analogue [Pd(tbbpy)Cl(2)] as host lattice.}, language = {en} } @article{ZehmFudickarHansetal.2008, author = {Zehm, Daniel and Fudickar, Werner and Hans, Melanie and Schilde, Uwe and Kelling, Alexandra and Linker, Torsten}, title = {9,10-Diarylanthracenes as molecular switches : syntheses, properties, isomerisations and their reactions with singlet oxygen}, issn = {0947-6539}, year = {2008}, abstract = {A series of 9,10-diarylanthracenes with various substituents at the ortho positions have been synthesised by palladium-catalysed cross-coupling reactions. Such compounds exhibit interesting physical properties and can be applied as molecular switches. Despite the high steric demand of the substituents, products were formed in moderate-to-good yields. In some cases, microwave conditions further improved yields. Bis-coupling afforded two isomers (syn and anti) that do not interconvert at room temperature. These products were easily separated and their relative stereochemistries were unequivocally assigned by NMR spectroscopy and X-ray analysis. The syn and anti isomers exhibit different physical properties (e.g., melting points and solubilities) and interconversion by rotation around the aryl-aryl axis commences at <100 °C for fluoro-substituted diarylanthracenes and at >300 °C for alkyl- or alkoxy-substituted diarylanthracenes. The reactions with singlet oxygen were studied separately and revealed different reactivities and reaction pathways. The yields and reactivities depend on the size and electronic nature of the substituents. The anti isomers form the same 9,10-endoperoxides as the syn species, occasionally accompanied by unexpected 1,4-endoperoxides as byproducts. Thermolysis of the endoperoxides exclusively yielded the syn isomers. The interesting rotation around the aryl-aryl axis allows the application of 9,10-diarylanthracenes as molecular switches, which are triggered by light and air under mild conditions. Finally, the oxygenation and thermolysis sequence provides a simple, synthetic access to a single stereoisomer (syn) from an unselective coupling step.}, language = {en} } @article{SchmidtStaudeKellingetal.2011, author = {Schmidt, Bernd and Staude, Lucia and Kelling, Alexandra and Schilde, Uwe}, title = {A Cross-Metathesis-Conjugate addition route to enantiopure gamma-Butyrolactams and gamma-Lactones from a C-2-Symmetric Precursor}, series = {European journal of organic chemistry}, journal = {European journal of organic chemistry}, number = {9}, publisher = {Wiley-Blackwell}, address = {Malden}, issn = {1434-193X}, doi = {10.1002/ejoc.201001528}, pages = {1721 -- 1727}, year = {2011}, abstract = {A protected derivative of (3R, 4R)-hexa-1,5-diene-3,4-diol, a conveniently accessible C-2-symmetric building block, undergoes single or double cross metathesis with methyl acryl-ate. The cross metathesis products are amenable to stereoselective conjugate addition reactions and can be converted into either gamma-butyrolactones or gamma-lactams.}, language = {en} } @article{WessigWawrzinekMoellnitzetal.2011, author = {Wessig, Pablo and Wawrzinek, Robert and Moellnitz, Kristian and Feldbusch, Elvira and Schilde, Uwe}, title = {A new class of fluorescent dyes based on 1,3-benzodioxole and [1,3]-dioxolo[4.5-f]benzodioxole}, series = {Tetrahedron letters}, volume = {52}, journal = {Tetrahedron letters}, number = {46}, publisher = {Elsevier}, address = {Oxford}, issn = {0040-4039}, doi = {10.1016/j.tetlet.2011.09.058}, pages = {6192 -- 6195}, year = {2011}, abstract = {We report on synthesis and photophysical properties of a new class of fluorescent dyes. They are characterized by large Stokes-shifts, long fluorescence lifetimes in organic solvents and a pronounced dependency of the fluorescence lifetime on the solvent polarity. Also worthy of note is the high bleaching stability. To provide access to biochemical and medical applications a series of derivatives were prepared, which exhibit specific reactivity towards different biologically relevant functional groups (carboxylic acids, amines, maleimides, N-hydroxysuccinimide esters). Furthermore, two alkynes were prepared, which could be used in 'Click' chemistry.}, language = {en} } @article{MondalBhuniaKellingetal.2014, author = {Mondal, Suvendu Sekhar and Bhunia, Asamanjoy and Kelling, Alexandra and Schilde, Uwe and Janiak, Christoph and Holdt, Hans-J{\"u}rgen}, title = {A supramolecular Co(II)(14)- metal-organic cube in a hydrogen-bonded network and a Co(II)-organic framework with a flexible methoxy substituent}, series = {Chemical communications}, volume = {50}, journal = {Chemical communications}, number = {41}, publisher = {Royal Society of Chemistry}, address = {Cambridge}, issn = {1359-7345}, doi = {10.1039/c3cc49698h}, pages = {5441 -- 5443}, year = {2014}, abstract = {The reaction of 4,5-dicyano-2-methoxyimidazole (L1) with Co(NO3)(2.) 6H(2)O under solvothermal conditions in DMF, a MOF, IFP-8 and a hydrogen-bonded network consisting of tetradecanuclear Co(II)(14)-metal organic cube (1) are achieved. 1 shows the bcu net with 14 cobalt atoms.}, language = {en} } @article{MondalBhuniaKellingetal.2014, author = {Mondal, Suvendu Sekhar and Bhunia, Asamanjoy and Kelling, Alexandra and Schilde, Uwe and Janiak, Christoph and Holdt, Hans-J{\"u}rgen}, title = {A supramolecular Co(II)₁₄-metal-organic cube in a hydrogen-bonded network and a Co(II)-organic framework with a flexible methoxy substituent}, series = {Chemical communications : ChemComm}, volume = {2014}, journal = {Chemical communications : ChemComm}, number = {41}, publisher = {Royal Society of Chemistry}, issn = {2046-2069}, doi = {10.1039/c3cc49698h}, pages = {5441 -- 5443}, year = {2014}, abstract = {The reaction of 4,5-dicyano-2-methoxyimidazole (L1) with Co(NO3)2·6H2O under solvothermal conditions in DMF, a MOF, IFP-8 and a hydrogen-bonded network consisting of tetradecanuclear Co(II)14-metal organic cube (1) are achieved. 1 shows the bcu net with 14 cobalt atoms.}, language = {en} } @article{GroboschSchildeTiersch2006, author = {Grobosch, Thomas and Schilde, Uwe and Tiersch, Brigitte}, title = {Abtrennung von Arsen und anderer Schwermetalle mit impr{\"a}gnierten Adsorberpolymeren - teil 2: Abtrennung von Blei, Kupfer, Nickel und Zink}, issn = {0009-286X}, doi = {10.1002/cite.200500171}, year = {2006}, language = {de} } @article{UhlemannGroboschSchildeetal.1996, author = {Uhlemann, Erhard and Grobosch, Thomas and Schilde, Uwe and Feistel, Lothar}, title = {Abtrennung von Arsen(V) aus Grundwasser mittels Ionenaustauscher}, year = {1996}, language = {de} } @article{MuellerKellingSchildeetal.2009, author = {M{\"u}ller, Holger and Kelling, Alexandra and Schilde, Uwe and Holdt, Hans-J{\"u}rgen}, title = {Ag(I)-, Hg(II)- und Pt(II)-Komplexe von Maleonitril-thiakronenethern}, issn = {0932-0776}, year = {2009}, abstract = {The synthesis and single crystal X-ray structures of eight AgI, HgII, and PtII complexes with the thiacrown ethers maleonitrile-tetrathia-12-crown-4 (mn12S4), maleonitrile-tetrathia-13-crown-4 (mn13S4), and maleonitrile- pentathia-15-crown-5 (mn15S5) (1) are reported. The ligand mn15S5 was synthesized for the first time and characterized by X-ray diffraction. With silver(I) perchlorate and silver(I) tetrafluoroborate it forms the chiral complexes [Ag(mn15S5)]ClO4·CH3NO2 (2) and [Ag(mn15S5)]BF4·CH3NO2·0.25H2O (3) with half-sandwich moieties. AgI is located in a distorted tetrahedral coordination environment, involving three sulfur atoms of the crown cycle and a fourth one of the adjacent half-sandwich moiety, forming a helical structure. The reaction of Hg(ClO4)2 with mn13S4 yielded the dinuclear complex [Hg2(mn13S4)3](ClO4)4 (4) containing two half-sandwich moieties with a third ligand molecule as a bridging unit. Mercury(II) chloride and mercury(II) iodide react with mn12S4 and mn13S4 to form complexes of the general composition [HgX2(L)] (X = Cl, I; L = mn12S4, mn13S4): [HgCl2(mn12S4)] (5), [HgI2(mn12S4)] (6), [HgCl2(mn13S4)] (7) or [HgX2(L)2] (X = I; L = mn13S4): [HgI2(mn13S4)2] (8). Only one or two sulfur atoms of the ligand are involved in the complexation, and chain or ribbon structures are formed. In these compounds the HgX2 units (X = Cl, I) are preserved, coordinated by sulfur atoms of bridging mn12S4 or mn13S4 ligands. In all complexes of this type, the metal atoms are not coordinated inside the cavity, but in an exocyclic mode, because the diameter of the macrocycle is too small. Additionally, the PtCl2 complex of mn12S4 was investigated, where PtII is coordinated in an exocyclic mode forming the complex [PtCl2(mn12S4)] (9). Two of the four sulfur atoms of the macrocycle are bonded to the metal giving together with both chlorine atoms a square-planar coordination geometry. Together with a long-range interaction with a further sulfur atom of the macrocycle a square-pyramidal coordination environment is formed.}, language = {de} } @article{AbouserieZehbeMetzneretal.2017, author = {Abouserie, Ahed and Zehbe, Kerstin and Metzner, Philipp and Kelling, Alexandra and G{\"u}nter, Christina and Schilde, Uwe and Strauch, Peter and K{\"o}rzd{\"o}rfer, Thomas and Taubert, Andreas}, title = {Alkylpyridinium Tetrahalidometallate Ionic Liquids and Ionic Liquid Crystals: Insights into the Origin of Their Phase Behavior}, series = {European journal of inorganic chemistry : a journal of ChemPubSoc Europe}, journal = {European journal of inorganic chemistry : a journal of ChemPubSoc Europe}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {1434-1948}, doi = {10.1002/ejic.201700826}, pages = {5640 -- 5649}, year = {2017}, abstract = {Six N-alkylpyridinium salts [CnPy](2)[MCl4] (n = 4 or 12 and M = Co, Cu, Zn) were synthesized, and their structure and thermal properties were studied. The [C4Py](2)[MCl4] compounds are monoclinic and crystallize in the space group P2(1)/n. The crystals of the longer chain analogues [C12Py](2)[MCl4] are triclinic and crystallize in the space group P (1) over bar. Above the melting temperature, all compounds are ionic liquids (ILs). The derivatives with the longer C12 chain exhibit liquid crystallinity and the shorter chain compounds only show a melting transition. Consistent with single-crystal analysis, electron paramagnetic resonance spectroscopy suggests that the [CuCl4](2-) ions in the Cu-based ILs have a distorted tetrahedral geometry.}, language = {en} } @article{AbouserieZehbeMetzneretal.2017, author = {Abouserie, Ahed and Zehbe, Kerstin and Metzner, Philipp and Kelling, Alexandra and G{\"u}nter, Christina and Schilde, Uwe and Strauch, Peter and K{\"o}rzd{\"o}rfer, Thomas and Taubert, Andreas}, title = {Alkylpyridinium Tetrahalidometallate Ionic Liquids and Ionic Liquid Crystals: Insights into the Origin of Their Phase Behavior}, series = {European journal of inorganic chemistry : a journal of ChemPubSoc Europe}, journal = {European journal of inorganic chemistry : a journal of ChemPubSoc Europe}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {1434-1948}, doi = {10.1002/ejic.201700826}, pages = {5640 -- 5649}, year = {2017}, abstract = {Six N-alkylpyridinium salts [CnPy](2)[MCl4] (n = 4 or 12 and M = Co, Cu, Zn) were synthesized, and their structure and thermal properties were studied. The [C4Py](2)[MCl4] compounds are monoclinic and crystallize in the space group P2(1)/n. The crystals of the longer chain analogues [C12Py](2)[MCl4] are triclinic and crystallize in the space group P (1) over bar. Above the melting temperature, all compounds are ionic liquids (ILs). The derivatives with the longer C12 chain exhibit liquid crystallinity and the shorter chain compounds only show a melting transition. Consistent with single-crystal analysis, electron paramagnetic resonance spectroscopy suggests that the [CuCl4](2-) ions in the Cu-based ILs have a distorted tetrahedral geometry.}, language = {en} } @article{SteeplesKellingSchildeetal.2016, author = {Steeples, Elliot and Kelling, Alexandra and Schilde, Uwe and Esposito, Davide}, title = {Amino acid-derived N-heterocyclic carbene palladium complexes for aqueous phase Suzuki-Miyaura couplings}, series = {New journal of chemistry}, volume = {40}, journal = {New journal of chemistry}, publisher = {Royal Society of Chemistry}, address = {Cambridge}, issn = {1144-0546}, doi = {10.1039/c5nj03337c}, pages = {4922 -- 4930}, year = {2016}, abstract = {In this work, three ligands produced from amino acids were synthesized and used to produce five bis- and PEPPSI-type palladium-NHC complexes using a novel synthesis route from sustainable starting materials. Three of these complexes were used as precatalysts in the aqueous-phase Suzuki-Miyaura coupling of various substrates displaying high activity. TEM and mercury poisoning experiments provide evidence for Pd-nanoparticle formation stabilized in water.}, language = {en} } @article{DebatinBehrensWeberetal.2012, author = {Debatin, Franziska and Behrens, Karsten and Weber, Jens and Baburin, Igor A. and Thomas, Arne and Schmidt, Johannes and Senkovska, Irena and Kaskel, Stefan and Kelling, Alexandra and Hedin, Niklas and Bacsik, Zoltan and Leoni, Stefano and Seifert, Gotthard and J{\"a}ger, Christian and G{\"u}nter, Christina and Schilde, Uwe and Friedrich, Alwin and Holdt, Hans-J{\"u}rgen}, title = {An isoreticular family of microporous metal-organic frameworks based on zinc and 2-substituted imidazolate-4-amide-5-imidate Syntheses, structures and properties}, series = {Chemistry - a European journal}, volume = {18}, journal = {Chemistry - a European journal}, number = {37}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {0947-6539}, doi = {10.1002/chem.201200889}, pages = {11630 -- 11640}, year = {2012}, abstract = {We report on a new series of isoreticular frameworks based on zinc and 2-substituted imidazolate-4-amide-5-imidate (IFP-14, IFP=imidazolate framework Potsdam) that form one-dimensional, microporous hexagonal channels. Varying R in the 2-substitued linker (R=Me (IFP-1), Cl (IFP-2), Br (IFP-3), Et (IFP-4)) allowed the channel diameter (4.01.7 angstrom), the polarisability and functionality of the channel walls to be tuned. Frameworks IFP-2, IFP-3 and IFP-4 are isostructural to previously reported IFP-1. The structures of IFP-2 and IFP-3 were solved by X-ray crystallographic analyses. The structure of IFP-4 was determined by a combination of PXRD and structure modelling and was confirmed by IR spectroscopy and 1H MAS and 13C CP-MAS NMR spectroscopy. All IFPs showed high thermal stability (345400?degrees C); IFP-1 and IFP-4 were stable in boiling water for 7 d. A detailed porosity analysis was performed on the basis of adsorption measurements by using various gases. The potential of the materials to undergo specific interactions with CO2 was investigated by measuring the isosteric heats of adsorption. The capacity to adsorb CH4 (at 298 K), CO2 (at 298 K) and H2 (at 77 K) at high pressure were also investigated. In situ IR spectroscopy showed that CO2 is physisorbed on IFP-14 under dry conditions and that both CO2 and H2O are physisorbed on IFP-1 under moist conditions.}, language = {en} } @article{MoskalikAstakhovaSchildeetal.2014, author = {Moskalik, Mikhail Yu. and Astakhova, Vera V. and Schilde, Uwe and Sterkhova, Irina V. and Shainyan, Bagrat A.}, title = {Assembling of 3,6-diazabicyclo[3.1.0]hexane framework in oxidative triflamidation of substituted buta-1,3-dienes}, series = {Tetrahedron}, volume = {70}, journal = {Tetrahedron}, number = {45}, publisher = {Elsevier}, address = {Oxford}, issn = {0040-4020}, doi = {10.1016/j.tet.2014.09.050}, pages = {8636 -- 8641}, year = {2014}, language = {en} } @article{WessigMatthesSchildeetal.2013, author = {Wessig, Pablo and Matthes, Annika and Schilde, Uwe and Kelling, Alexandra}, title = {Asymmetric synthesis of (1,5)Naphthalenophanes by Dehydro-Diels-Alder reaction}, series = {European journal of organic chemistry}, journal = {European journal of organic chemistry}, number = {11}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {1434-193X}, doi = {10.1002/ejoc.201201594}, pages = {2123 -- 2129}, year = {2013}, abstract = {An asymmetric variant of the dehydro-Diels-Alder (DDA) reaction has been developed and applied in the atropselective synthesis of various (1,5)naphthalenophanes. Whereas the suitability of the photochemically induced DDA (PDDA) was limited, the thermally induced DDA provided the desired product, depending on the chiral auxiliary used and the length of the linker, with nearly perfect stereoselectivity. Furthermore, the mechanism of the DDA was investigated by means of DFT calculations, and a stepwise mechanism involving 1,4-biradicals was suggested.}, language = {en} } @article{StrauchNeumannKellingetal.2015, author = {Strauch, Peter and Neumann, Mike and Kelling, Alexandra and Schilde, Uwe}, title = {Bis(1,2-dithiosquarato)nickelates(II): Synthesis, Structure, EPR and Thermal Behavior}, series = {Acta chimica Slovenica}, volume = {62}, journal = {Acta chimica Slovenica}, number = {2}, publisher = {Drustvo}, address = {Ljubljana}, issn = {1318-0207}, pages = {288 -- 296}, year = {2015}, abstract = {1,2-Dithiosquaratonickelates are available by direct synthesis from metal salts with dipotassium-1,2-dithiosquarate and the appropriate counter cations. The synthesis and characterization, including mass spectrometry, of a series 1,2-dithiosquaratonickelates(II), [Ni(dtsq)(2)](2-), with several "onium" cations is reported and the X-ray structures of two diamagnetic complexes, (HexPh(3)P)(2)[Ni(dtsq)(2)] and (BuPh3P)(2)[Ni(dtsq)(2)] with sterically demanding counter ions are presented. The diamagnetic nickel complexes have been doped as host lattices with traces of Cu(II) to measure EPR for additional structural information. The thermal behavior of this series is studied by thermogravimetry and differential thermal analysis (TG/DTA). The thermolysis in air as well as under nitrogen atmosphere of these complexes results in nickel oxide nano-particles in all cases, which are characterized by X-ray powder diffraction.}, language = {en} } @article{UhlemannSchildeWeller1995, author = {Uhlemann, Erhard and Schilde, Uwe and Weller, Frank}, title = {Calcium- und Bariumkomplexe mit 1-Phenyl-3-methyl-4-benzoyl-pyrazol-5-on}, year = {1995}, language = {de} } @article{SchmidtRiemerSchilde2014, author = {Schmidt, Bernd and Riemer, Martin and Schilde, Uwe}, title = {Chroman-4-ones via microwave-promoted domino claisen rearrangement-oxa-michael addition: Synthesis of tabchromones A and B}, series = {Synlett : accounts and rapid communications in synthetic organic chemistry}, volume = {25}, journal = {Synlett : accounts and rapid communications in synthetic organic chemistry}, number = {20}, publisher = {Thieme}, address = {Stuttgart}, issn = {0936-5214}, doi = {10.1055/s-0034-1379364}, pages = {2943 -- 2946}, year = {2014}, abstract = {Allyl phenyl ethers with a pendant enone substituent undergo, upon microwave irradiation, a domino sequence of Claisen rearrangement and 6-endo-trig-cyclization to furnish functionalized chroman-4-ones. The natural products tabchromones A and B were synthesized via this method.}, language = {en} } @article{CoyBarreraCucaSuarezSefkowetal.2012, author = {Coy-Barrera, Ericsson D. and Cuca-Suarez, Luis E. and Sefkow, Michael and Schilde, Uwe}, title = {Cinerin C: a macrophyllin-type bicyclo[3.2.1]octane neolignan from Pleurothyrium cinereum (Lauraceae)}, series = {Acta crystallographica : Section C, Crystal structure communications}, volume = {68}, journal = {Acta crystallographica : Section C, Crystal structure communications}, number = {2}, publisher = {Wiley-Blackwell}, address = {Hoboken}, issn = {0108-2701}, doi = {10.1107/S0108270112030946}, pages = {O320 -- +}, year = {2012}, abstract = {The structure of naturally-occurring cinerin C [systematic name: (7S,8R,3'R,4'S,5'R)-Delta(8')-4'-hydroxy-5,5',3'-trimethoxy-3,4-methylenedioxy-2',3',4',5'-tetrahydro-2'-oxo-7.3',8.5'-neolignan], isolated from the ethanol extract of leaves of Pleurothyrium cinereum (Lauraceae), has previously been established by NMR and HRMS spectroscopy, and its absolute configuration established by circular dichroism measurements. For the first time, its crystal strucure has now been established by single-crystal X-ray analysis, as the monohydrate, C22H26O7 center dot H2O. The bicyclooctane moiety comprises fused cyclopentane and cyclohexenone rings which are almost coplanar. An intermolecular O-H center dot center dot center dot O hydrogen bond links the 4'-OH and 5'-OCH3 groups along the c axis.}, language = {en} } @article{StarkeKammerGrunwaldetal.2008, author = {Starke, Ines and Kammer, Stefan and Grunwald, Nicolas and Schilde, Uwe and Holdt, Hans-J{\"u}rgen and Kleinpeter, Erich}, title = {Complexation of diazaperylene and bisisoquinoline with transition metal ions in the gas phase studied by electrospray ionization mass spectrometry}, year = {2008}, abstract = {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.}, language = {en} } @article{RathAnandSankaretal.2003, author = {Rath, Harapriya and Anand, V. G. and Sankar, J. and Venkatraman, S. and Chandrashekar, T. K. and Joshi, Bhawani S. and Khetrapal, C. L. and Schilde, Uwe and Senge, Mathias O.}, title = {Core-Modified Hexaphyrins; Characterization of Two- and Four-Ring Inverted 26 {\^o} Aromatic Macrocycles}, year = {2003}, language = {en} } @article{UhlemannSchildeHefeleetal.1994, author = {Uhlemann, Erhard and Schilde, Uwe and Hefele, Heike and Ludwig, Eberhard}, title = {Crystal and molecular structure of 2,2'-dihydroxyazobenzene}, issn = {0023-4753}, year = {1994}, language = {en} } @article{PeikowMaternPeteretal.2005, author = {Peikow, Dirk and Matern, Christa-Maria and Peter, Martin G. and Schilde, Uwe}, title = {Crystal structure of (1,4,7,10,13-pentaoxacyclopentadecane-O,O ',O '',O ''')(trifluoromethanesulfonato-O,O ')sodium, Na(C10H20O5)(CF3SO3)}, year = {2005}, abstract = {C11H20F3NaO8S, monoclinic, P121/nil (no. 11), a = 7.947(1) angstrom, b = 12.056(1) angstrom, c = 9.083(1) angstrom, P = 106.01 (1)degrees, V = 836.4 angstrom(3), Z = 2, R-gt(F) = 0.043, wR(ref)(F-2) = 0.120, T = 210 K.}, language = {en} } @article{WessigMoellnitzKellingetal.2011, author = {Wessig, Pablo and M{\"o}llnitz, Kristian and Kelling, Alexandra and Schilde, Uwe}, title = {Crystal structure of 1r,2c,3c,4t,5t,6t-1,2,3,4,5,6-hexakis-trimethylsilanyloxy-cyclohexane, C24H60O6Si6}, series = {Zeitschrift f{\"u}r Kristallographie : international journal for structural, physical and chemical aspects of crystalline materials ; New crystal structures}, volume = {226}, journal = {Zeitschrift f{\"u}r Kristallographie : international journal for structural, physical and chemical aspects of crystalline materials ; New crystal structures}, number = {2}, publisher = {De Gruyter Oldenbourg}, address = {M{\"u}nchen}, issn = {1433-7266}, doi = {10.1524/ncrs.2011.0105}, pages = {228 -- 230}, year = {2011}, abstract = {C24H60O6Si6, triclinic, P (1) over bar (no. 2), a = 11.307(2) angstrom, b = 12.159(2) angstrom, = 16.576(2) angstrom, alpha = 109.47(1)degrees, beta = 94.64(1)degrees, gamma = 111.65(1)degrees, V = 1942.3 angstrom(3), Z = 2, R-gt(F) = 0.043, wR(ref)(F-2) = 0.118, T = 210 K.}, language = {en} } @article{WessigMatthesSchilde2010, author = {Wessig, Pablo and Matthes, Annika and Schilde, Uwe}, title = {Crystal structure of 3,4-diacetyl-15,21-dioxatetracyclo- [23.4.0.02,7.06,11]nonacosa-1(29),2,4,6,8,10,25,27- octaene- 14,22-dione{\`u}water (1:2), C31H32O6 · 2H2O}, issn = {1433-7266}, year = {2010}, language = {en} } @article{UhlemannSchildeBansseetal.1995, author = {Uhlemann, Erhard and Schilde, Uwe and Banße, Wolfgang and Ludwig, Eberhard}, title = {Crystal structure of bis(1,3-diphenyl-1,3-dionato)oxo-vanadium(IV), C30H2205V}, issn = {0044-2968}, year = {1995}, language = {en} } @article{SchildeMicklerUhlemann1997, author = {Schilde, Uwe and Mickler, Wulfhard and Uhlemann, Erhard}, title = {Crystal structure of bis(1-phenyl-5-cyclohexyl-pentane-1,3-dionato-copper(II)}, issn = {0044-2968}, year = {1997}, language = {en} } @article{UhlemannSchildeMickler1996, author = {Uhlemann, Erhard and Schilde, Uwe and Mickler, Wulfhard}, title = {Crystal structure of bis(1-phenyldecane-1,3-dionato)-copper(II), Cu(C16H21O2)2}, issn = {0044-2968}, year = {1996}, language = {en} } @article{HahnKellingSchildeetal.2008, author = {Hahn, Simone and Kelling, Alexandra and Schilde, Uwe and Holdt, Hans-J{\"u}rgen}, title = {Crystal structure of bis(2-ethylthiomethylpyridine)platinum(II) hexachloroplatinate, [Pt(C8H11NS)2][PtCl6]}, issn = {1433-7266}, doi = {10.1524/ncrs.2008.0216}, year = {2008}, abstract = {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.}, language = {en} } @article{LinkerFudickarKellingetal.2013, author = {Linker, Torsten and Fudickar, Werner and Kelling, Alexandra and Schilde, Uwe}, title = {Crystal structure of dimethyl 1,4-dioxaspiro[4,5]dec-6-ene-(8R)-[(3,5-dinitrobenzoyl)oxa]-(2R,3R)-dica rboxylate, C19H18N2O12}, series = {Zeitschrift f{\"u}r Kristallographie : international journal for structural, physical and chemical aspects of crystalline materials ; New crystal structures}, volume = {228}, journal = {Zeitschrift f{\"u}r Kristallographie : international journal for structural, physical and chemical aspects of crystalline materials ; New crystal structures}, number = {2}, publisher = {De Gruyter Oldenbourg}, address = {M{\"u}nchen}, issn = {1433-7266}, doi = {10.1524/ncrs.2013.0123}, pages = {241 -- 242}, year = {2013}, abstract = {C19H18N2O12, orthorhombic, P2(1)2(1)2(1) (no. 19), a = 6.2472(6) angstrom, b = 17.576(2) angstrom, c = 18.848(3) angstrom, V = 2069.6 angstrom(3), Z = 4, R-gt(F) = 0.0393, wR(ref)(F-2) = 0.0694, T = 210 K.}, language = {en} } @article{SchildePazOrtiz2017, author = {Schilde, Uwe and Paz, Christian and Ortiz, Leandro}, title = {Crystal structure of erioflorin isolated from Podanthus mitiqui (L.)}, series = {Acta Crystallographica Section E : Crystallographic Communications}, volume = {73}, journal = {Acta Crystallographica Section E : Crystallographic Communications}, number = {3}, publisher = {International Union of Crystallography}, address = {Chester}, doi = {10.1107/S2056989017001700}, pages = {334 -- 337}, year = {2017}, abstract = {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.}, language = {en} } @article{UhlemannHefeleLudwigetal.1996, author = {Uhlemann, Erhard and Hefele, Heike and Ludwig, Eberhard and Schilde, Uwe}, title = {Crystal structure of methoxo-oxo[benzoylaceton-salicyl hydrazonato(2-)]vanadium(V), C18H17N2O5V}, issn = {0044-2968}, year = {1996}, language = {en} } @article{ElamparuthiLinkerKellingetal.2009, author = {Elamparuthi, Elangovan and Linker, Torsten and Kelling, Alexandra and Schilde, Uwe}, title = {Crystal structure of methyl 3,4-di-O-benzyl-2-deoxy-2-C-nitromethyl-alpha-D-arabinopyranoside, C21H25NO6}, issn = {1433-7266}, doi = {10.1524/ncrs.2009.0027}, year = {2009}, language = {en} } @article{KovacsTothKleinpeteretal.2003, author = {Kovacs, J. and Toth, G. and Kleinpeter, Erich and Schilde, Uwe}, title = {Crystal structure of trans, cis-({\~n})-3{\"i}-4-fluorophenyl)-2-phenylspiro[2H-1-benzothiopyran-34H,2{\"i}-oxiran]-4-one 1- oxide, C22H15FO3S}, issn = {1433-7266}, year = {2003}, language = {en} } @article{LinkerBramborgKellingetal.2013, author = {Linker, Torsten and Bramborg, Andrea and Kelling, Alexandra and Schilde, Uwe}, title = {Crystal structure of trans-1,4-di-(2-(allyloxyethyl)-cyclohexa-2,5-diene-1,4-dicarboxylic acid, C18H24O6}, series = {Zeitschrift f{\"u}r Kristallographie : international journal for structural, physical and chemical aspects of crystalline materials ; New crystal structures}, volume = {228}, journal = {Zeitschrift f{\"u}r Kristallographie : international journal for structural, physical and chemical aspects of crystalline materials ; New crystal structures}, number = {2}, publisher = {De Gruyter Oldenbourg}, address = {M{\"u}nchen}, issn = {1433-7266}, doi = {10.1524/ncrs.2013.0124}, pages = {243 -- 244}, year = {2013}, abstract = {C18H24O6, triclinic, P (1) over bar (no. 2), a = 5.726(1) angstrom, b = 8.845(2) angstrom, c = 9.557(2) angstrom, alpha = 105.27(1)degrees, beta = 102.76(1)degrees, gamma = 103.49(1)degrees, V = 433.0 angstrom(3), Z = 1, R-gt(F) = 0.0412, wR(ref)(F-2) = 0.1075, T = 210 K.}, language = {en} } @article{ShainyanSuslovaSchilde2008, author = {Shainyan, Bagrat A. and Suslova, Elena N. and Schilde, Uwe}, title = {Crystal structures and theoretical calculations of trans -2,4,4-trimethyl-4-silathiane 1-oxide and 4,4-dimethyl- 4-silathiane 1,1-dioxide}, issn = {1040-0400}, year = {2008}, abstract = {The crystal and molecular structures of trans-2,4,4-trimethyl-4-silathiane 1-oxide 1 and 4,4-dimethyl-4- silathiane 1,1-dioxide 2 were determined by single crystal X-ray diffraction. Both compounds have the chair conformation with the 2-Me and the S=O group in compound 1 occupying the equatorial positions. The DFT (B3LYP/6-311G(d,p)) and MP2 (MP2/6-311G(d,p)) theoretical calculations nicely reproduce the X-ray experimental geometry. The obtained results are discussed in connection with the electronic and structural properties of the compounds.}, language = {en} } @article{SchildeKellingUmbreenetal.2016, author = {Schilde, Uwe and Kelling, Alexandra and Umbreen, Sumaira and Linker, Torsten}, title = {Crystal structures of three bicyclic carbohydrate derivatives}, series = {Acta crystallographica Section E ; Crystallographic communications}, volume = {72}, journal = {Acta crystallographica Section E ; Crystallographic communications}, number = {12}, publisher = {IUCR}, address = {Chester}, issn = {2056-9890}, doi = {10.1107/S2056989016018727}, pages = {1839 -- 1844}, year = {2016}, abstract = {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.}, language = {en} } @article{SchildeKellingUmbreenetal.2016, author = {Schilde, Uwe and Kelling, Alexandra and Umbreen, Sumaira and Linker, Torsten}, title = {Crystal structures of three bicyclic carbohydrate derivatives}, series = {Acta crystallographica, Section E, Crystallographic communications}, volume = {72}, journal = {Acta crystallographica, Section E, Crystallographic communications}, publisher = {International Union of Crystallography}, address = {Chester}, issn = {2056-9890}, doi = {10.1107/S2056989016018727}, pages = {1839 -- +}, year = {2016}, abstract = {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.}, language = {en} } @article{KruegerKellingLinkeretal.2019, author = {Krueger, Tobias and Kelling, Alexandra and Linker, Torsten and Schilde, Uwe}, title = {Crystal structures of three cyclohexane‑based γ‑spirolactams}, series = {BMC Chemistry}, volume = {13}, journal = {BMC Chemistry}, number = {69}, publisher = {Springer International Publishing}, address = {Basel}, issn = {2661-801X}, doi = {10.1186/s13065-019-0586-7}, pages = {9}, year = {2019}, abstract = {The title compounds, 2-azaspiro[4.5]deca-1-one, C₉H₁₅NO, (1a), cis-8-methyl-2-azaspiro[4.5]deca-1-one, C₁₀H₁₇NO, (1b), and trans-8-methyl-2-azaspiro[4.5]deca-1-one, C₁₀H₁₇NO, (1c), were synthesized from benzoic acids 2 in only 3 steps in high yields. Crystallization from n-hexane afforded single crystals, suitable for X-ray diffraction. Thus, the configurations, conformations, and interesting crystal packing effects have been determined unequivocally. The bicyclic skeleton consists of a lactam ring, attached by a spiro junction to a cyclohexane ring. The lactam ring adopts an envelope conformation and the cyclohexane ring has a chair conformation. The main difference between compound 1b and compound 1c is the position of the carbonyl group on the 2-pyrrolidine ring with respect to the methyl group on the 8-position of the cyclohexane ring, which is cis (1b) or trans (1c). A remarkable feature of all three compounds is the existence of a mirror plane within the molecule. Given that all compounds crystallize in centrosymmetric space groups, the packing always contains interesting enantiomer-like pairs. Finally, the structures are stabilized by intermolecular N-H···O hydrogen bonds.}, language = {en} } @article{SchmidtElizarovSchildeetal.2015, author = {Schmidt, Bernd and Elizarov, Nelli and Schilde, Uwe and Kelling, Alexandra}, title = {Dual Role of Acetanilides: Traceless Removal of a Directing Group through Deacetylation/Diazotation and Palladium-Catalyzed C-C-Coupling Reactions}, series = {The journal of organic chemistry}, volume = {80}, journal = {The journal of organic chemistry}, number = {9}, publisher = {American Chemical Society}, address = {Washington}, issn = {0022-3263}, doi = {10.1021/acs.joc.5b00272}, pages = {4223 -- 4234}, year = {2015}, abstract = {The acetamide group enables regioselective oxidative ortho-C-H activation reactions, such as Pd-catalyzed acylation. The synthetic utility of these transformations can be significantly enhanced by using the acetamide as a quasi-leaving group in a subsequent conventional Pd-catalyzed coupling or cross-coupling reaction. The concept is illustrated herein for the synthesis of o-alkenyl- and o-arylphenones, which have potential for the synthesis of arylated aromatic heterocycles.}, language = {en} } @article{MovahedifarModarresiAlamKleinpeteretal.2017, author = {Movahedifar, Fahimeh and Modarresi-Alam, Ali Reza and Kleinpeter, Erich and Schilde, Uwe}, title = {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}, series = {Journal of molecular structure}, volume = {1133}, journal = {Journal of molecular structure}, publisher = {Elsevier}, address = {Amsterdam}, issn = {0022-2860}, doi = {10.1016/j.molstruc.2016.12.010}, pages = {244 -- 252}, year = {2017}, abstract = {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.}, language = {en} } @article{StrauchKossmannKellingetal.2016, author = {Strauch, Peter and Kossmann, Alexander and Kelling, Alexandra and Schilde, Uwe}, title = {EPR on bis(1,2-dithiosquarato)cuprate(II) in the bis(1,2-dithiosquarato)nickelate(II) host lattice - structure and spectroscopy}, series = {Chemical papers}, volume = {70}, journal = {Chemical papers}, publisher = {De Gruyter}, address = {Berlin}, issn = {0366-6352}, doi = {10.1515/chempap-2015-0154}, pages = {61 -- 68}, year = {2016}, abstract = {EPR spectroscopy is a well suited analytical tool to monitor the electronic situation around paramagnetic metal centres as copper(II) and therefore the structural influences on the paramagnetic ion. 1,2-Dithiosquaratometalates are available by direct synthesis from metal salts with dipotassium-1,2-dithiosquarate and the appropriate counter cations. Synthesis and characterisation of bis(benzyltributylammonium)1,2-dithiosquaratonickelate(II), (BzlBu(3)N)(2)[Ni(dtsq)(2)], and bis(benzyltributylammonium)1,2-dithiosquaratocuprate(II), (BzlBu(3)N)(2)[Cu(dtsq)(2)], with benzyltributylammonium as the counter ion is reported and the X-ray structures of two complexes, (BzlBu(3)N)(2)[Ni(dtsq)(2)] and (BzlBu(3)N)(2)[Cu(dtsq)(2)], are presented. Both complexes, crystallising in the monoclinic space group P2(1)/c, are isostructural with only small differences in the coordination sphere due to the different metal ions. The diamagnetic nickel complex is therefore well suited as a host lattice for the paramagnetic Cu(II) complex to measure EPR for additional structural information. (c) 2015 Institute of Chemistry, Slovak Academy of Sciences}, language = {en} } @article{AwadKochMickleretal.2012, author = {Awad, Duha Jawad and Koch, Andreas and Mickler, Wulfhard and Schilde, Uwe and Strauch, Peter}, title = {EPR spectroscopy of 4, 4 '-Bis(tert-butyl)-2, 2 '-bipyridine-1, 2-dithiolatocuprates(II) in host lattices with different coordination geometries}, series = {Zeitschrift f{\"u}r anorganische und allgemeine Chemie}, volume = {638}, journal = {Zeitschrift f{\"u}r anorganische und allgemeine Chemie}, number = {6}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {0044-2313}, doi = {10.1002/zaac.201100517}, pages = {965 -- 975}, year = {2012}, abstract = {A series of new heteroleptic MN2S2 transition metal complexes with M = Cu2+ for EPR measurements and as diamagnetic hosts Ni2+, Zn2+, and Pd2+ were synthesized and characterized. The ligands are N2 = 4, 4'-bis(tert-butyl)-2, 2'-bipyridine (tBu2bpy) and S2 =1, 2-dithiooxalate, (dto), 1, 2-dithiosquarate, (dtsq), maleonitrile-1, 2-dithiolate, or 1, 2-dicyanoethene-1, 2-dithiolate, (mnt). The CuII complexes were studied by EPR in solution and as powders, diamagnetically diluted in the isostructural planar [NiII(tBu2bpy)(S2)] or[PdII(tBu2bpy)(S2)] as well as in tetrahedrally coordinated[ZnII(tBu2bpy)(S2)] host structures to put steric stress on the coordination geometry of the central CuN2S2 unit. The spin density contributions for different geometries calculated from experimental parameters are compared with the electronic situation in the frontier orbital, namely in the semi-occupied molecular orbital (SOMO) of the copper complex, derived from quantum chemical calculations on different levels (EHT and DFT). One of the hosts, [NiII(tBu2bpy)(mnt)], is characterized by X-ray structure analysis to prove the coordination geometry. The complex crystallizes in a square-planar coordination mode in the monoclinic space group P21/a with Z = 4 and the unit cell parameters a = 10.4508(10) angstrom, b = 18.266(2) angstrom, c = 12.6566(12) angstrom, beta = 112.095(7)degrees. Oxidation and reductions potentials of one of the host complexes, [Ni(tBu2bpy)(mnt)], were obtained by cyclovoltammetric measurements.}, language = {en} } @article{WessigPickSchilde2011, author = {Wessig, Pablo and Pick, Charlotte and Schilde, Uwe}, title = {First example of an atropselective dehydro-Diels-Alder (ADDA) reaction}, series = {Tetrahedron letters}, volume = {52}, journal = {Tetrahedron letters}, number = {32}, publisher = {Elsevier}, address = {Oxford}, issn = {0040-4039}, doi = {10.1016/j.tetlet.2011.06.024}, pages = {4221 -- 4223}, year = {2011}, abstract = {A new concept of a stereoselective synthesis of axially chiral biaryls, formed in the course of the dehydro-Diels-Alder (DDA) reaction, has been disclosed. It is based on asymmetric induction of the newly formed chirality axis by a chirality center, which is present in the two synthesized DDA reactants. Depending on the different length of the linkers joining the alkyne moieties the DDA reaction may be triggered photochemically or thermally, where only the thermal variant was stereoselective.}, language = {en} } @article{HeydenreichPoleschnerSchilde1996, author = {Heydenreich, Matthias and Poleschner, Helmut and Schilde, Uwe}, title = {Fluoroselenenylation of Acetylenes with Xenon Difluoride-Diorganyl Diselenides : synthesis and structure elucidation of functionalized Vicinal (E)-Fluoro(organylseleno)olefins}, year = {1996}, language = {en} } @article{ShainyanMoskalikStarkeetal.2010, author = {Shainyan, Bagrat A. and Moskalik, Mikail Yu and Starke, Ines and Schilde, Uwe}, title = {Formation of unexpected products in the attempted aziridination of styrene with trifluoromethanesulfonyl nitrene}, issn = {0040-4020}, doi = {10.1016/j.tet.2010.08.070}, year = {2010}, abstract = {The reaction of styrene with trifluoromethanesulfonyl nitrene generated from trifluoromethanesulfonamide in the system (t-BuOCl+NaI) results in the formation of trifluoro-N-[2-phenyl-2-(trifluoromethylsulfonyl) aminoethyl]methanesulfonamide, 1-pheny1-2-iodo-ethanol, and 2,5-diphenyl-1,4-bis(trifluoromethyl sulfonyl)piperazine rather than the expected product of aziridination, 2-phenyl-1-(trifluoromethylsulfonyl) aziridine. The mechanism of the reaction is discussed.}, language = {en} } @article{MondalBhuniaBaburinetal.2013, author = {Mondal, Suvendu Sekhar and Bhunia, Asamanjoy and Baburin, Igor A. and J{\"a}ger, Christian and Kelling, Alexandra and Schilde, Uwe and Seifert, Gotthard and Janiak, Christoph and Holdt, Hans-J{\"u}rgen}, title = {Gate effects in a hexagonal zinc-imidazolate-4-amide-5-imidate framework with flexible methoxy substituents and CO2 selectivity}, series = {Chemical communications}, volume = {49}, journal = {Chemical communications}, number = {69}, publisher = {Royal Society of Chemistry}, address = {Cambridge}, issn = {1359-7345}, doi = {10.1039/c3cc42156b}, pages = {7599 -- 7601}, year = {2013}, abstract = {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 N-2 and CH4 gases.}, language = {en} } @article{MondalBhuniaBaburinetal.2008, author = {Mondal, Suvendu Sekhar and Bhunia, Asamanjoy and Baburin, Igor A. and J{\"a}ger, Christian and Kelling, Alexandra and Schilde, Uwe and Seiert, Gotthard and Janiak, Christoph and Holdt, Hans-J{\"u}rgen}, title = {Gate effects in a hexagonal zinc-imidazolate-4-amide-5-imidate framework with flexible methoxy substituents and CO2 selectivity}, doi = {10.1039/C3CC42156B}, year = {2008}, abstract = {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.}, language = {en} } @article{MondalBhuniaKellingetal.2014, author = {Mondal, Suvendu Sekhar and Bhunia, Asamanjoy and Kelling, Alexandra and Schilde, Uwe and Janiak, Christoph and Holdt, Hans-J{\"u}rgen}, title = {Giant Zn-14 molecular building block in hydrogen-bonded network with permanent porosity for gas uptake}, series = {Journal of the American Chemical Society}, volume = {136}, journal = {Journal of the American Chemical Society}, number = {1}, publisher = {American Chemical Society}, address = {Washington}, issn = {0002-7863}, doi = {10.1021/ja410595q}, pages = {44 -- 47}, year = {2014}, abstract = {In situ imidazolate-4,5-diamide-2-olate linker generation leads to the formation of a [Zn-14(L2)(12)(O)-(OH)(2)(H2O)(4)] molecular building block (MBB) with a Zn-6 octahedron inscribed in a Zn-8 cube. The MBBs connect by amide-amide hydrogen bonds to a 3D robust supramolecular network which can be activated for N-2, CO2, CH4, and H-2 gas sorption.}, language = {en} } @article{SieboldKellingSchildeetal.2005, author = {Siebold, M. and Kelling, Alexandra and Schilde, Uwe and Strauch, Peter}, title = {Heterobimetallic 3d-4-complexes with bis(1;2-dithiooxalato)nickelate(II) as planar bridging block}, issn = {0932-0776}, year = {2005}, abstract = {Planar bis(1,2-dithiooxalato)nickelates(II) react in aqueous solutions of lanthanide ions to form pentanuclear, heterobimetallic complexes of the general composition [{Ln(H2O)(n)}(2)- {Ni(dto)(2)}(3)] (.) xH(2)O (Ln = Y3+, La3+, Ce3+, Pr3+, Nd3+, Sm3+, Eu3+, Gd3+, Tb3+, Dy3+, Ho3+, Er3+, Tm3+, Yb3+, Lu3+; n = 4 or 5; x = 9-12). With [{Nd(H2O)(5)}(2){Ni(S2C2O2)(2)}(3)] (.) xH(2)O (x = 10-12) (1) and [{Er(H2O)(4)}(2){Ni(S2C2O2)(2)}(3)] (.) xH(2)O (x = 9- 10) (2) we were able to isolate two complexes of this series as single crystals, which were characterized by X-ray structure analysis. Depending on the individual ionic radii of the lanthanide ions, the compounds crystallize in two different crystal systems with the following unit cell parameters: 1, monoclinic in P2(1)/c with a = 11.3987(13), b = 11.4878(8), c = 20.823(2)angstrom , beta = 98.907(9)degrees and Z = 2; 2, triclinic in P (1) over bar with a = 10.5091(6), b = 11.0604(6), c = 11.2823(6) angstrom, alpha = 107.899(4)degrees, beta = 91.436(4)degrees, gamma = 112.918(4)degrees and Z = 1. The channels and cavities appearing in the packing of the molecules are occupied by uncoordinated water molecules. High magnetic moments up to 14.65 BM./f.u. have been observed at room temperature due to the combined moments of the individual lanthanide ions}, language = {en} } @article{BrietzkeKellingSchildeetal.2016, author = {Brietzke, Thomas Martin and Kelling, Alexandra and Schilde, Uwe and Mickler, Wulfhard and Holdt, Hans-J{\"u}rgen}, title = {Heterodinuclear Ruthenium(II) Complexes of the Bridging Ligand 1,6,7,12-Tetraazaperylene with Iron(II), Cobalt(II), Nickel(II), as well as Palladium(II) and Platinum(II)}, series = {Zeitschrift f{\~A}¼r anorganische und allgemeine Chemie}, volume = {642}, journal = {Zeitschrift f{\~A}¼r anorganische und allgemeine Chemie}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {0044-2313}, doi = {10.1002/zaac.201500645}, pages = {8 -- 13}, year = {2016}, abstract = {The first heterodinuclear ruthenium(II) complexes of the 1,6,7,12-tetraazaperylene (tape) bridging ligand with iron(II), cobalt(II), and nickel(II) were synthesized and characterized. The metal coordination sphere in this complexes is filled by the tetradentate N,N-dimethyl-2,11-diaza[3.3](2,6)-pyridinophane (L-N4Me2) ligand, yielding complexes of the general formula [(L-N4Me2)Ru(mu-tape)M(L-N4Me2)](ClO4)(2)(PF6)(2) with M = Fe {[2](ClO4)(2)(PF6)(2)}, Co {[3](ClO4)(2)(PF6)(2)}, and Ni {[4](ClO4)(2)(PF6)(2)}. Furthermore, the heterodinuclear tape ruthenium(II) complexes with palladium(II)- and platinum(II)-dichloride [(bpy)(2)Ru(-tape)PdCl2](PF6)(2) {[5](PF6)(2)} and [(dmbpy)(2)Ru(-tape)PtCl2](PF6)(2) {[6](PF6)(2)}, respectively were also prepared. The molecular structures of the complex cations [2](4+) and [4](4+) were discussed on the basis of the X-ray structures of [2](ClO4)(4)MeCN and [4](ClO4)(4)MeCN. The electrochemical behavior and the UV/Vis absorption spectra of the heterodinuclear tape ruthenium(II) complexes were explored and compared with the data of the analogous mono- and homodinuclear ruthenium(II) complexes of the tape bridging ligand.}, language = {en} } @article{AlrefaiMondalWrucketal.2019, author = {Alrefai, Anas and Mondal, Suvendu Sekhar and Wruck, Alexander and Kelling, Alexandra and Schilde, Uwe and Brandt, Philipp and Janiak, Christoph and Schoenfeld, Sophie and Weber, Birgit and Rybakowski, Lawrence and Herrman, Carmen and Brennenstuhl, Katlen and Eidner, Sascha and Kumke, Michael Uwe and Behrens, Karsten and G{\"u}nter, Christina and M{\"u}ller, Holger and Holdt, Hans-J{\"u}rgen}, title = {Hydrogen-bonded supramolecular metal-imidazolate frameworks: gas sorption, magnetic and UV/Vis spectroscopic properties}, series = {Journal of Inclusion Phenomena and Macrocyclic Chemistry}, volume = {94}, journal = {Journal of Inclusion Phenomena and Macrocyclic Chemistry}, number = {3-4}, publisher = {Springer}, address = {Dordrecht}, issn = {1388-3127}, doi = {10.1007/s10847-019-00926-6}, pages = {155 -- 165}, year = {2019}, abstract = {By varying reaction parameters for the syntheses of the hydrogen-bonded metal-imidazolate frameworks (HIF) HIF-1 and HIF-2 (featuring 14 Zn and 14 Co atoms, respectively) to increase their yields and crystallinity, we found that HIF-1 is generated in two different frameworks, named as HIF-1a and HIF-1b. HIF-1b is isostructural to HIF-2. We determined the gas sorption and magnetic properties of HIF-2. In comparison to HIF-1a (Brunauer-Emmett-Teller (BET) surface area of 471m(2) g(-1)), HIF-2 possesses overall very low gas sorption uptake capacities [BET(CO2) surface area=85m(2) g(-1)]. Variable temperature magnetic susceptibility measurement of HIF-2 showed antiferromagnetic exchange interactions between the cobalt(II) high-spin centres at lower temperature. Theoretical analysis by density functional theory confirmed this finding. The UV/Vis-reflection spectra of HIF-1 (mixture of HIF-1a and b), HIF-2 and HIF-3 (with 14 Cd atoms) were measured and showed a characteristic absorption band centered at 340nm, which was indicative for differences in the imidazolate framework.}, language = {en} } @article{UhlemannProchaskaLudwigetal.1996, author = {Uhlemann, Erhard and Prochaska, Krystyna and Ludwig, Eberhard and Schilde, Uwe}, title = {Hydrolyse von Trifluoracetylaceton-Salicylhydrazon : Struktur von Acetonsalicylhydrazon}, year = {1996}, language = {de} } @article{MondalMuellerJungingeretal.2014, author = {Mondal, Suvendu Sekhar and Mueller, Holger and Junginger, Matthias and Kelling, Alexandra and Schilde, Uwe and Strehmel, Veronika and Holdt, Hans-J{\"u}rgen}, title = {Imidazolium 2-substituted 4,5-dicyanoimidazolate ionic liquids: synthesis, crystal structures and structure-thermal property relationships}, series = {Chemistry - a European journal}, volume = {20}, journal = {Chemistry - a European journal}, number = {26}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {0947-6539}, doi = {10.1002/chem.201304934}, pages = {8170 -- 8181}, year = {2014}, abstract = {Thirty six novel ionic liquids (ILs) with 1-butyl-3-methylimidazolium and 3-methyl-1-octylimidazolium cations paired with 2-substitited 4,5-dicyanoimidazolate anions (substituent at C2=chloro, bromo, methoxy, vinyl, amino, methyl, ethyl, propyl, isopropyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl, undecyl and phenyl) have been synthesized and characterized by using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and single-crystal X-ray crystallography. The effects of cation and anion type and structure on the thermal properties of the resulting ionic liquids, including several room temperature ionic liquids (RTILs) are examined and discussed. ILs exhibited large liquid and crystallization ranges and formed glasses on cooling with glass transition temperatures in the range of -22 to -68 degrees C. The effects of alkyl substituents of the imidazolate anion reflected the crystallization, melting points and thermal decomposition of the ILs. The Coulombic packing force, van der Waals forces and size of the anions can be considered for altering the thermal transitions. Three crystal structures of the ILs were determined and the effects of changes to the cations and anions on the packing of the structure were investigated.}, language = {en} } @article{MirskovaAdamovichMirskovetal.2015, author = {Mirskova, Anna N. and Adamovich, Sergey N. and Mirskov, Rudolf G. and Kolesnikova, Olga P. and Schilde, Uwe}, title = {Immunoactive ionic liquids based on 2-hydroxyethylamines and 1-R-indol-3-ylsulfanylacetic acids. Crystal and molecular structure of immunodepressant tris-(2-hydroxyethyl)ammonium indol-3-ylsulfanylacetate}, series = {Open chemistry : formerly Central European journal of chemistry}, volume = {13}, journal = {Open chemistry : formerly Central European journal of chemistry}, number = {1}, publisher = {De Gruyter Open}, address = {Warsaw}, issn = {2391-5420}, doi = {10.1515/chem-2015-0018}, pages = {149 -- 155}, year = {2015}, abstract = {Immunoactive ionic liquids (2-hydroxyethyl) ammonium 1-R-indol-3-ylsulfanyl-acetates HN+R1R2(CH2CH2OH)center dot O-(O)CCH2S-Ind-R-3-1(1-5), were synthesized by the reaction of (2-hydroxyethyl)amines with indol-3-ylsulfanylacetic- or 1-benzylindol-3-ylsulfanylacetic acid. 1: R-1 = R-2 = CH2CH2OH, R-3 = H; 2: R-1 =CH3, R-2=CH2CH2OH, R3 = H; 3: R-1 = R-2 = CH3, R-3 = H; 4: R-1 = R-2 = CH2CH2OH, R-3 = CH2C6H5; 5: R-1 = CH3; R-2 = CH2CH2OH; R-3 = CH2C6H5. The structure of each compound was elucidated by IR, NMR H-1, C-13, and N-15 techniques and their composition was confirmed by elemental analysis. The crystal structure of tris-(2-hydroxyethyl) ammonium indol-3-ylsulfanylacetate was investigated by X-ray diffraction analysis. Immunoactive properties of the title compounds were screened.}, language = {en} } @article{DebatinThomasKellingetal.2010, author = {Debatin, Franziska and Thomas, Arne and Kelling, Alexandra and Hedin, Niklas and Bacsik, Zoltan and Senkovska, Irena and Kaskel, Stefan and Junginger, Matthias and M{\"u}ller, Holger and Schilde, Uwe and J{\"a}ger, Christian and Friedrich, Alwin and Holdt, Hans-J{\"u}rgen}, title = {In situ synthesis of an imidazolate-4-amide-5-imidate ligand and formation of a microporous zinc-organic framework with H2-and CO2-storage ability}, issn = {1433-7851}, doi = {10.1002/anie.200906188}, year = {2010}, abstract = {Narrow channels with polar walls are the structural and functional features responsible for the high capacity of a zinc-organic framework based on an imidazolate-amide-imidate ligand for the uptake of H2 and CO2 (see structure: orange Zn, blue N, red O, dark gray C, light gray H). The rigid and stable chelating ligand was synthesized in situ by partial hydrolysis of a dicyanoimidazole compound.}, language = {en} } @article{KukeMarmodeeEidneretal.2010, author = {Kuke, S. and Marmodee, Bettina and Eidner, Sascha and Schilde, Uwe and Kumke, Michael Uwe}, title = {Intramolecular deactivation processes in complexes of salicylic acid or glycolic acid with Eu(III)}, issn = {0584-8539}, year = {2010}, abstract = {The complexation of Eu(III) by 2-hydroxy benzoic acid (2HB) or glycolic acid (GL) was investigated using steady- state and time-resolved laser spectroscopy. Experiments were carried out in H2O as well as in D2O in the temperature range of View the MathML source. The Eu(III) luminescence spectra and luminescence decay times were evaluated with respect to the temperature dependence of (i) the luminescence decay time ;, (ii) the energy of the View the MathML source transition, (iii) the width of the View the MathML source transition, and (iv) the asymmetry ratio calculated from the luminescence intensities of the View the MathML source and View the MathML source transition, respectively. The differences in ligand-related luminescence quenching are discussed. Based on the temperature dependence of the luminescence decay times an activation energy for the ligand-specific non-radiative deactivation in Eu(III)-2HB or Eu(III)-GL complexes was determined. It is stressed that ligand-specific quenching processes (other than OH quenching induced by water molecules) need to be determined and considered in detail, in order to extract speciation- relevant information from luminescence data (e.g., estimation of the number of water molecules nH2O in the first coordination sphere of Eu(III)). In case of 2HB, conclusions drawn from the evaluation of the Eu(III) luminescence are compared with results of a X-ray structure analysis.}, language = {en} } @article{BaierKellingSchildeetal.2016, author = {Baier, Heiko and Kelling, Alexandra and Schilde, Uwe and Holdt, Hans-J{\"u}rgen}, title = {Investigation of the Catalytic Activity of a 2-Phenylidenepyridine Palladium(II) Complex Bearing 4,5-Dicyano-1,3-bis(mesityl)imidazol-2-ylidene in the Mizoroki-Heck Reaction}, series = {Zeitschrift f{\~A}¼r anorganische und allgemeine Chemie}, volume = {642}, journal = {Zeitschrift f{\~A}¼r anorganische und allgemeine Chemie}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {0044-2313}, doi = {10.1002/zaac.201500625}, pages = {140 -- 147}, year = {2016}, abstract = {The phenylidenepyridine (ppy) palladacycles [PdCl(ppy)(IMes)] (4) [IMes = 1,3-bis(mesityl) imidazol-2-ylidene] and [PdCl(ppy){(CN)(2)IMes}] (6) [(CN)(2)IMes = 4,5-dicyano-1,3-bis(mesityl) imidazol-2-ylidene] were prepared by facile two step syntheses, starting with the reaction of palladium(II) chloride with 2-phenylpyridine followed by subsequent addition of the NHC ligand to the precatalyst precursor [PdCl(ppy)](2). Suitable crystals for the X-ray analysis of the complexes 4 and 6 were obtained. It was shown that 6 has a shorter NHC-palladium bond than the IMes complex 4. The difference of the palladium carbene bond lengths based on the higher pi-acceptor strength of (CN)(2)IMes in comparison to IMes. Thus, (CN)(2)IMes should stabilize the catalytically active central palladium atom better than IMes. As a measure for the pi-acceptor strength of (CN)(2)IMes compared to IMes, the selone (CN)(2)IMes center dot Se (7) was prepared and characterized by Se-77-NMR spectroscopy. The pi-acceptor strength of 7 was illuminated by the shift of its Se-77-NMR signal. The Se-77-NMR signal of 7 was shifted to much higher frequencies than the Se-77-NMR signal of IMes center dot Se. Catalytic experiments using the Mizoroki-Heck reaction of aryl chlorides with n-butyl acrylate showed that 6 is the superior performer in comparison to 4. Using complex 6, an extensive substrate screening of 26 different aryl bromides with n-butyl acrylate was performed. Complex 6 is a suitable precatalyst for para-substituted aryl bromides. The catalytically active species was identified by mercury poisoning experiments to be palladium nanoparticles.}, language = {en} } @article{ZehbeKolloscheLardongetal.2016, author = {Zehbe, Kerstin and Kollosche, Matthias and Lardong, Sebastian and Kelling, Alexandra and Schilde, Uwe and Taubert, Andreas}, title = {Ionogels Based on Poly(methyl methacrylate) and Metal-Containing Ionic Liquids: Correlation between Structure and Mechanical and Electrical Properties}, series = {International journal of molecular sciences}, volume = {17}, journal = {International journal of molecular sciences}, publisher = {MDPI}, address = {Basel}, issn = {1422-0067}, doi = {10.3390/ijms17030391}, pages = {16}, year = {2016}, abstract = {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.}, language = {en} } @article{UhlemannFriedrichHinscheetal.1995, author = {Uhlemann, Erhard and Friedrich, Alwin and Hinsche, Gerald and Mickler, Wulfhard and Schilde, Uwe}, title = {Komplexbildung und Metallextraktion mit heterocyclischen ß-Dicarbonylverbindungen im Vergleich : Struktur von 3-Phenyl-4-benzoyl-isoxazol-5-on}, year = {1995}, language = {de} } @article{UhlemannLudwigHefeleetal.1994, author = {Uhlemann, Erhard and Ludwig, Eberhard and Hefele, Heike and Schilde, Uwe}, title = {Komplexe von Vanadium und Titan mit 2,2'-Dihydroxy-azobenzen : Kristallstrukturen von 2,2'- Dihydroxy-azobenzenato(2-)oxo-methoxo-methanol-vanadium(V) und {\ae}-Oxo-bis[2,2'-dihy droxy-azobenzenato(2-)]-oxo- vanadium(V)]}, year = {1994}, language = {de} } @article{UhlemannDuvinageSchilde2008, author = {Uhlemann, Jacqueline and Duvinage, Brigitte and Schilde, Uwe}, title = {Kontexte und Kompetenzen : Komplexverbindungen experimentell erkunden}, issn = {1617-5638}, year = {2008}, language = {de} } @article{UhlemannBansseLudwigetal.1995, author = {Uhlemann, Erhard and Banße, Wolfgang and Ludwig, Eberhard and Schilde, Uwe and Weller, Frank}, title = {Ligand Exchange Reactions of Bis(acetyl-acetonato)dioxomolybdenum(VI) and Molybdenum Hexacarbonyl}, year = {1995}, language = {en} } @article{UhlemannBansseLudwigetal.1995, author = {Uhlemann, Erhard and Banße, Wolfgang and Ludwig, Eberhard and Schilde, Uwe and Weller, Frank and Lehmann, Andreas}, title = {Ligandenaustauschreaktionen von Bis(acetylacetonato)dioxo-molybd{\"a}n(VI). Kristallstrukturen von Salicyl- aldehyd-benzoylhydrazonato(2-)]dioxom ethanol-molybd{\"a}n(VI) und [Benzoylacetonbenzoylhydrazonato(2)]dioxo- triphenylphosphan-oxidmolybd{\"a}n(VI)}, year = {1995}, language = {de} } @article{SchwarzeTraegerKellingetal.2013, author = {Schwarze, Thomas and Traeger, Juliane and Kelling, Alexandra and Schilde, Uwe and Holdt, Hans-J{\"u}rgen}, title = {Macrocyclic dithiomaleonitriles for an efficient PdCl2 coordination}, series = {Inorganica chimica acta : the international inorganic chemistry journal}, volume = {408}, journal = {Inorganica chimica acta : the international inorganic chemistry journal}, number = {2}, publisher = {Elsevier}, address = {Lausanne}, issn = {0020-1693}, doi = {10.1016/j.ica.2013.08.020}, pages = {53 -- 58}, year = {2013}, abstract = {We have synthesized a set of new unsaturated macrocyclic dithioethers with an increasing number of flexible methylene units 1-7 (Scheme 2) to investigate the correlation between the ring size of these ligands, the chelation effect and the consequences for an efficient PdCl2 coordination. The dithioethers 1-7 and the complex [PdCl2(4)]center dot CHCl3 were characterized by X-ray diffraction analysis. The crystal structures of 1-7 show that 2-7 are better preorganized chelating ligands for an exocyclic PdCl2 coordination than 1. The chelation effect of 1-7, the orientation of the sulfur atoms and the S center dot center dot center dot S donor distances, are influenced by the flexibility of the methylene units. In this series the unsaturated macrocyclic ligands 5 and 6 are the best chelating ligands for an efficient PdCl2 coordination. Comparative solvent extraction experiments with mn-12S(2)O(2) (mn = maleonitrile) reveal that the low interface activity of the new ligands reduces the extraction rate. However, a comparison with open-chain dithiomaleonitriles shows the impact of the macrocyclic effect of 4 and 5 on the extraction yield.}, language = {en} } @article{GonzalezChavarriaDupratRoaetal.2020, author = {Gonzalez-Chavarria, Ivan and Duprat, Felix and Roa, Francisco J. and Jara, Nery and Toledo, Jorge R. and Miranda, Felipe and Becerra, Jose and Inostroza, Alejandro and Kelling, Alexandra and Schilde, Uwe and Heydenreich, Matthias and Paz, Cristian}, title = {Maytenus disticha extract and an isolated β-Dihydroagarofuran induce mitochondrial depolarization and apoptosis in human cancer cells by increasing mitochondrial reactive oxygen species}, series = {Biomolecules}, volume = {10}, journal = {Biomolecules}, number = {3}, publisher = {MDPI}, address = {Basel}, issn = {2218-273X}, doi = {10.3390/biom10030377}, pages = {15}, year = {2020}, abstract = {Maytenus disticha (Hook F.), belonging to the Celastraceae family, is an evergreen shrub, native of the central southern mountains of Chile. Previous studies demonstrated that the total extract of M. disticha (MD) has an acetylcholinesterase inhibitory activity along with growth regulatory and insecticidal activities. beta-Dihydroagarofurans sesquiterpenes are the most active components in the plant. However, its activity in cancer has not been analyzed yet. Here, we demonstrate that MD has a cytotoxic activity on breast (MCF-7), lung (PC9), and prostate (C4-2B) human cancer cells with an IC50 (mu g/mL) of 40, 4.7, and 5 mu g/mL, respectively, an increasing Bax/Bcl2 ratio, and inducing a mitochondrial membrane depolarization. The beta-dihydroagarofuran-type sesquiterpene (MD-6), dihydromyricetin (MD-9), and dihydromyricetin-3-O-beta-glucoside (MD-10) were isolated as the major compounds from MD extracts. From these compounds, only MD-6 showed cytotoxic activity on MCF-7, PC9, and C4-2B with an IC50 of 31.02, 17.58, and 42.19 mu M, respectively. Furthermore, the MD-6 increases cell ROS generation, and MD and MD-6 induce a mitochondrial superoxide generation and apoptosis on MCF-7, PC9, and C4-2B, which suggests that the cytotoxic effect of MD is mediated in part by the beta-dihydroagarofuran-type that induces apoptosis by a mitochondrial dysfunction.}, language = {en} } @article{HoldtMuellerKellingetal.2006, author = {Holdt, Hans-J{\"u}rgen and M{\"u}ller, Holger and Kelling, Alexandra and Drexler, Hans-Joachim and M{\"u}ller, Thomas and Schwarze, Thomas and Schilde, Uwe and Starke, Ines}, title = {Mercury(II) chloride and iodide complexes of dithia- and tetrathiacrown ethers}, issn = {0044-2313}, doi = {10.1002/zaac.200500281}, year = {2006}, abstract = {The complexes [(HgCl2)(2)((ch)(2)30S(4)O(6))] (1), [HgCl,(mn21S(2)O(5))] (2), [HgCl2(ch18S(2)O(4))] (3) and [HgI(meb12S(2)O(2))](2)[Hg2I6] (4) have been synthesized, characterized and their crystal structures were determined. In [(HgCl2)(2)((ch)(2)3OS(4)O(6))] two HgCl2 units are discretely bonded within the ligand cavity of the 30-membered dichinoxaline-tetrathia-30-crown-10 ((ch)(2)30S(4)O(6)) forming a binuclear complex. HgCl2 forms I : I "in-cavity" complexes with the 21-membered maleonitrile-dithia-21-crown-7(mn21S(2)O(5)) ligand and the 18-membered chinoxaline- dithia-18-crown-6 (ch18S(2)O(4)) ligand, respectively. The 12-membered 4-methyl-benzo-dithia-12-crown-4 (meb12S(2)O(2)) ligand gave with two equivalents HgI2 the compound [HgI(meb12S(2)O(2))](2)[Hg2I6]. In the cation [HgI(meb12S(2)O(2))](+) meb12S(2)O(2) forms with the cation HgI+ a half-sandwich complex}, language = {en} } @article{SardarianInalooModarresiAlametal.2019, author = {Sardarian, Ali Reza and Inaloo, Iman Dindarloo and Modarresi-Alam, Ali Reza and Kleinpeter, Erich and Schilde, Uwe}, title = {Metal-Free Regioselective Monocyanation of Hydroxy-, Alkoxy-, and Benzyloxyarenes by Potassium Thiocyanate and Silica Sulfuric Acid as a Cyanating Agent}, series = {The journal of organic chemistry}, volume = {84}, journal = {The journal of organic chemistry}, number = {4}, publisher = {American Chemical Society}, address = {Washington}, issn = {0022-3263}, doi = {10.1021/acs.joc.8b02191}, pages = {1748 -- 1756}, year = {2019}, abstract = {A novel and efficient metal- and solvent-free regioselective para-C-H cyanation of hydroxy-, alkoxy-, and benzyloxyarene derivatives has been introduced, using nontoxic potassium thiocyanate as a cyanating reagent in the presence of silica sulfuric acid (SSA). The desired products are obtained in good to high yields without any toxic byproducts.}, language = {en} } @article{WessigGerngrossFreyseetal.2016, author = {Wessig, Pablo and Gerngross, Maik and Freyse, Daniel and Bruhn, P. and Przezdziak, Marc and Schilde, Uwe and Kelling, Alexandra}, title = {Molecular Rods Based on Oligo-spiro-thioketals}, series = {The journal of organic chemistry}, volume = {81}, journal = {The journal of organic chemistry}, publisher = {American Chemical Society}, address = {Washington}, issn = {0022-3263}, doi = {10.1021/acs.joc.5b02670}, pages = {1125 -- 1136}, year = {2016}, abstract = {We report on an extension of the previously established concept of oligospiroketal (OSK) rods by replacing a part or all ketal moieties by thioketals leading to oligospirothioketal (OSTK) rods. In this way, some crucial problems arising from the reversible formation of ketals are circumvented. Furthermore, the stability of the rods toward hydrolysis is considerably improved. To successfully implement this concept, we first developed a number of new oligothiol building blocks and improved the synthetic accessibility of known oligothiols, respectively. Another advantage of thioacetals is that terephthalaldehyde (TAA) sleeves, which are too flexible in the case of acetals can be used in OSTK rods. The viability of the OSTK approach was demonstrated by the successful preparation of some OSTK rods with a length of some nanometers.}, language = {en} } @article{UhlemannKraudeltLudwigetal.1996, author = {Uhlemann, Erhard and Kraudelt, Heide and Ludwig, Eberhard and Schilde, Uwe}, title = {Molek{\"u}lstrukturen von Tautomeren des Benzoylaceton-benzoylhydrazons}, year = {1996}, language = {de} } @article{BrietzkeMicklerKellingetal.2012, author = {Brietzke, Thomas Martin and Mickler, Wulfhard and Kelling, Alexandra and Schilde, Uwe and Kr{\"u}ger, Hans-Joerg and Holdt, Hans-J{\"u}rgen}, title = {Mono- and dinuclear Ruthenium(II)-1,6,7,12-Tetraazaperylene complexes of N,N '-Dimethyl-2,11-diaza[3.3](2,6)-pyridinophane}, series = {European journal of inorganic chemistry : a journal of ChemPubSoc Europe}, journal = {European journal of inorganic chemistry : a journal of ChemPubSoc Europe}, number = {29}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {1434-1948}, doi = {10.1002/ejic.201200667}, pages = {4632 -- 4643}, year = {2012}, abstract = {Ruthenium(II) complexes [Ru(L-N4Me2)(dape)](PF6)2 {[1](PF6)2}, [Ru(L-N4Me2)(tape)](PF6)2 {[2](PF6)2}, and [{Ru(L-N4Me2)}2(mu-tape)](PF6)4 {[3](PF6)4} were synthesized in two reaction steps by first reacting [Ru(DMSO)4Cl2] with tetraazamacrocyclic ligand N,N'-dimethyl-2,11-diaza[3.3](2,6)-pyridinophane (L-N4Me2) in ethanol under microwave irradiation to the intermediate [Ru(L-N4Me2)Cl2], which was subsequently, without further isolation, reacted with 1,12-diazaperylene (dape) or 1,6,7,12-tetraazaperylene (tape). X-ray structures of [Ru(L-N4Me2)(dape)](PF6)2, [Ru(L-N4Me2)(tape)](PF6)2.acetone, and [{Ru(L-N4Me2)}2(mu-tape)](ClO4)4.MeCN were determined. The UV/Vis absorption spectra of [1](PF6)2, [2](PF6)2, and [3](PF6)4 in acetonitrile display intense low-energy dp(Ru)?p* (dape or tape) MLCT absorption bands centered at 579, 637, and 794 nm, respectively. Reversible metal oxidations for the bimetallic complex [{Ru(L-N4Me2)}2(mu-tape)]4+ ([3]4+) are detected at 1.69 and 1.28 V vs. SCE. The potential difference ?E = 410 mV and the intervalence-charge-transfer (IVCT) transition at 2472 nm indicate a high degree of electronic interaction between the two ruthenium ions mediated through the tape bridging ligand. All three complexes, [1]2+, [2]2+, and [3]4+, were characterized by UV/Vis spectroelectrochemistry. The monooxidized and monoreduced states, [1]3+, [2]3+, [3]5+, and [1]+, [2]+, [3]3+, are accessible by reversible one-electron oxidation and one-electron reduction processes, respectively, as documented by the observation of several stable isosbestic points in the spectral progressions. The second reduction in each complex and the second oxidation in [3]4+ prove to be irreversible in these spectroelectrochemical experiments. Monoreduced species [1]+, [2]+, and [3]3+ yield EPR signals indicating that the unpaired electron is mainly centered on the large surface ligands dape or tape.}, language = {en} } @article{KimSchildeLinker2005, author = {Kim, Boo Geun and Schilde, Uwe and Linker, Torsten}, title = {New radical approaches to 3-deoxy-D-oct-2-ulosonic acids (KDO)}, issn = {0039-7881}, year = {2005}, abstract = {Two different approaches. with an unsaturated carbohydrate as a radical acceptor and a carbohydrate derived aldehyde as a radical precursor, led to key intermediates in the synthesis of 3-deoxy-D-oct-2-ulosonic acids (KDO). Manganese(III) acetate and cerium(IV) ammonium nitrate were the reagents of choice for the oxidative generation of radicals, whereas samarium(II) iodide was employed for reductive couplings. Both strategies were realized by using easily available starting materials, with acetic acid as C-2 and ethyl acrylate as C-3 building blocks, respectively}, language = {en} } @article{BenassiBregullaFriedrichetal.1998, author = {Benassi, Rois and Bregulla, Antje and Friedrich, Alwin and Henning, Dietrich and Heydenreich, Matthias and Mickler, Wulfhard and Kleinpeter, Erich and Kempter, Gerhard and Schilde, Uwe and Taddei, F.}, title = {NMR spectroscopic and theoretical structural study of 5-exo-methylene-substituted hydantoins}, year = {1998}, language = {en} } @article{ShainyanMoskalikAstakhovaetal.2014, author = {Shainyan, Bagrat A. and Moskalik, Mikhail Yu and Astakhova, Vera V. and Schilde, Uwe}, title = {Novel design of 3,8-diazabicyclo[3.2.1]octane framework in oxidative sulfonamidation of 1,5-hexadiene}, series = {Tetrahedron}, volume = {70}, journal = {Tetrahedron}, number = {30}, publisher = {Elsevier}, address = {Oxford}, issn = {0040-4020}, doi = {10.1016/j.tet.2014.04.095}, pages = {4547 -- 4551}, year = {2014}, abstract = {1,5-Hexadiene reacts with trifluoromethanesulfonamide in the oxidative system (t-BuOCl+Nal) to give trans-2,5-bis(iodomethyl)-1-(trifluoromethylsulfonyl)pyrrolidine 5 and 3,8-bis(trifluoromethylsulfonyl)-3,8-diazabicyclo[3.2.1]octane 6. With arenesulfonamides ArSO2NH2 (Ar=Ph, Tol), the reaction stops at the formation of the trans and cis isomers of 2,5-bis(iodomethyl)-1-(arenesulfonyl)pyrrolidine 7 and 8 (1:1). The cis isomers of 7 and 8 do not undergo cyclization to the corresponding 3,8-disubstituted 3,8-diazabicyclo[3.2.1]octanes. The reaction with triflamide represents the first example of one-pot two-step route to 3,8-diazabicyclo[3.2.1]octane system. (C) 2014 Elsevier Ltd. All rights reserved.}, language = {en} } @article{MoskalikShainyanAstakhovaetal.2013, author = {Moskalik, Mikhail Yu and Shainyan, Bagrat A. and Astakhova, Vera V. and Schilde, Uwe}, title = {Oxidative addition of trifluoromethanesulfonamide to cycloalkadienes}, series = {Tetrahedron}, volume = {69}, journal = {Tetrahedron}, number = {2}, publisher = {Elsevier}, address = {Oxford}, issn = {0040-4020}, doi = {10.1016/j.tet.2012.10.099}, pages = {705 -- 711}, year = {2013}, abstract = {In the oxidative system (t-BuOCl+NaI) trifluoromethanesulfonamide is regio- and stereoselectively added to only one double bond of cyclopentadiene and 1,3-cyclohexadiene giving rise to 1,1,1-trifluoro-N-(5-iodocyclopent-2-en-1-yl)methanesulfonamide 7 and trans-N,N'-cyclohex-3-en-1,2-diylbis(1,1,1-trifluoromethanesulfonamide) 8. The structure of 7 and 8 was determined by X-ray, NMR, and MS. With 1,4-cyclohexadiene, addition to both double bonds occurs with the formation of N,N'-(4-chloro-5-iodocyclohexan-1,2-diyl)bis(1,1,1-trifluoromethanesulfonamide) 9. Under the action of sodium iodide in acetone, the latter product undergoes halogenophilic attack with the reduction of the CHI group and elimination of HCl to give trans-N,N'-cyclohex-4-en-1,2-diylbis(1,1,1-trifluoromethanesulfonamide) 10, whose structure was also determined by X-ray analysis. 1,3,5-Cycloheptatriene under these conditions is oxidized to benzaldehyde and does not react with trifluoromethanesulfonamide.}, language = {en} } @article{MeshcheryakovMoskalikKellingetal.2008, author = {Meshcheryakov, Vladimir I. and Moskalik, Mikail Yu. and Kelling, Alexandra and Schilde, Uwe and Ushakov, Igor A. and Shainyan, Bagrat A.}, title = {Oxymethylation of trifluoromethanesulfonamide with paraformaldehyde in ethyl acetate}, issn = {1070-4280}, doi = {10.1134/S1070428008020206}, year = {2008}, abstract = {Acid-catalyzed reaction of trifluoromethanesulfonamide with paraformaldehyde in ethyl acetate led to the formation of oxymethylated products that did not form in the reaction carried out in sulfuric acid. Following products were obtained: 5-trifluoromethylsulfonyl-1,3-dioxazinane, 3,7-bis-(trifluoromethylsulfonyl)-1,5,3,7-dioxadiazocane, and a complex of trifluoromethanesulfonamide with 2,4,8,10-tetraoxospiro[5,5]undecene, 1:1. The spiroring resulted from the cyclization of pentaerythritol under the action of formaldehyde. The pentaerythritol formed in its turn by oxymethylation of the methyl group of ethyl acetate with paraformaldehyde followed by the reduction of the COOEt group into CH2 OH by the formaldehyde.}, language = {en} } @article{SchmidtBergerKellingetal.2011, author = {Schmidt, Bernd and Berger, Ren{\´e} and Kelling, Alexandra and Schilde, Uwe}, title = {Pd-Catalyzed [2+2+1] coupling of alkynes and arenes phenol diazonium salts as mechanistic trapdoors}, series = {Chemistry - a European journal}, volume = {17}, journal = {Chemistry - a European journal}, number = {25}, publisher = {Wiley-Blackwell}, address = {Malden}, issn = {0947-6539}, doi = {10.1002/chem.201100609}, pages = {7032 -- 7040}, year = {2011}, abstract = {Alkynes and phenol diazonium salts undergo a Pd-catalyzed [2+2+1] cyclization reaction to spiro[4,5]decatetraene-7-ones. This structure was confirmed for one example by X-ray single-crystal structure analysis. The reaction is believed to proceed through oxidative addition of the phenol diazonium cation to Pd(0), subsequent insertion of two alkynes, followed by irreversible spirocyclization.}, language = {en} } @article{SchmidtHoelterKellingetal.2011, author = {Schmidt, Bernd and H{\"o}lter, Frank and Kelling, Alexandra and Schilde, Uwe}, title = {Pd-Catalyzed arylation reactions with phenol diazonium salts application in the synthesis of diarylheptanoids}, series = {The journal of organic chemistry}, volume = {76}, journal = {The journal of organic chemistry}, number = {9}, publisher = {American Chemical Society}, address = {Washington}, issn = {0022-3263}, doi = {10.1021/jo2002787}, pages = {3357 -- 3365}, year = {2011}, abstract = {The first total synthesis of the natural product (3S,7R)-5,6-dehydro-de-O-methyl centrolobine and various analogues is reported, using a highly regio- and diastereoselective Mizoroki-Heck reaction of phenol diazonium salts and enantiopure dihydropyrans. The assigned relative configuration was confirmed by single-crystal X-ray structure analysis, but a revision of the absolute configuration is proposed based on polarimetric measurement.}, language = {en} } @article{SieboldKorabikSchildeetal.2008, author = {Siebold, Matthias and Korabik, Maria and Schilde, Uwe and Mrozinski, Jerzy and Strauch, Peter}, title = {Pentanuclear heterobimetallic 3d-4f complexes of Ln2M3-type - structure and magnetism}, issn = {0366-6352}, year = {2008}, abstract = {From a series of pentanuclear, heterobimetallic complexes of the general composition [{Ln(H2O)n}2{Ni(dto)2}3] · xH2O, four complexes (Ln = Gd(III) with n = 4; Ln = Dy(III), Ho(III), or Er(III), with n = 5; x = 9-12; dto = 1,2- dithiooxalate) were studied due to their large magnetic moments (up to 14.65 B.M.). The magnetic properties of these complete series were measured at room temperature and the temperature dependent magnetic properties of the complexes Gd2Ni3, Dy2Ni3, Ho2Ni3, and Er2Ni3 were studied at room temperature down to 1.8 K. Whereas the intramolecular metal- metal distances were rather long (Ni1-Ni2: 11.0-11.5 {\AA}; Ln-Ni: 6.0-6.3 {\AA}), relatively short intermolecular metal-metal distances (Ni1-Ni2;: 3.5 {\AA}; Er-Er;: 6.0 {\AA}) were found in the crystal lattice, giving rise to weak intermolecular metal-metal interactions. These weak spin interactions were also supported by the EPR spectrum of a powdered sample of the diamagnetically undiluted Gd2Ni3 complex.}, language = {en} } @article{TraegerKellingSchildeetal.2012, author = {Tr{\"a}ger, J. and Kelling, A. and Schilde, Uwe and Holdt, H. -J.}, title = {rac-1-[(2-Methoxyethyl)sulfanyl]-2-[(2-methoxyethyl)sulfinyl]benzene and its PdCl2 complex}, series = {Acta crystallographica : Section C, Crystal structure communications}, volume = {68}, journal = {Acta crystallographica : Section C, Crystal structure communications}, number = {9}, publisher = {Wiley-Blackwell}, address = {Hoboken}, issn = {0108-2701}, doi = {10.1107/S0108270112032192}, pages = {M238 -- +}, year = {2012}, abstract = {As an extension of recent findings on the recovery of palladium with dithioether extractants, single crystals of the chelating vicinal thioether sulfoxide ligand rac-1-[(2-methoxyethyl)sulfanyl]-2-[(2-methoxyethyl)sulfinyl]benzene, C12H18O3S2, (I), and its square-planar dichloridopalladium complex, rac-dichlorido{1-[(2-methoxyethyl)sulfanyl]-2-[(2-methoxyethyl)sulfinyl]benzene-?2S,S'}palladium(II), [PdCl2(C12H18O3S2)], (II), have been synthesized and their structures analysed. The molecular structure of (II) is the first ever characterized involving a dihalogenidePdII complex in which the palladium is bonded to both a thioether and a sulfoxide functional group. The structural and stereochemical characteristics of the ligand are compared with those of the analogous dithioether compound [Traeger et al. (2012). Eur. J. Inorg. Chem. pp. 23412352]. The sulfinyl O atom suppresses the electron-pushing and mesomeric effect of the SC...;CS unit in ligand (I), resulting in bond lengths significantly different than in the dithioether reference compound. In contrast, in complex (II), those bond lengths are nearly the same as in the analogous dithioether complex. As observed previously, there is an interaction between the central PdII atom and the O atom that is situated above the plane.}, language = {en} } @article{MirskovaAdamovichMirskovetal.2013, author = {Mirskova, Anna N. and Adamovich, Sergey N. and Mirskov, Rudolf G. and Schilde, Uwe}, title = {Reaction of pharmacological active tris-(2-hydroxyethyl)ammonium 4-chlorophenylsulfanylacetate with ZnCl2 or NiCl2: first conversion of a protic ionic liquid into metallated ionic liquid}, series = {CHEMISTRY CENTRAL JOURNAL}, volume = {7}, journal = {CHEMISTRY CENTRAL JOURNAL}, publisher = {BIOMED CENTRAL LTD}, address = {LONDON}, issn = {1752-153X}, doi = {10.1186/1752-153X-7-34}, pages = {5}, year = {2013}, abstract = {The reaction of pharmacological active protic ionic liquid tris-(2-hydroxyethyl)ammonium 4-chlorophenylsulfanylacetate H+N(CH2CH2OH)(3) center dot (-OOCCH2SC6H4Cl-4) (1) with zinc or nickel chloride in a ratio of 2:1 affords stable at room temperature powder-like adducts [H+N(CH2CH2OH)(3)](2) center dot [M(OOCCH2SC6H4Cl-4)(2)Cl-2](2-), M = Zn (2), Ni (3). By recrystallization from aqueous alcohol compound 2 unexpectedly gives Zn(OOCCH2SC6H4Cl-4)(2) center dot 2H(2)O (4). Unlike 2, compound 3 gives crystals [N(CH2CH2OH)(3)](2)Ni2+ center dot [-OOCCH2SC6H4Cl-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).}, language = {en} } @article{MoskalikShainyanSchilde2011, author = {Moskalik, Mikail Yu. and Shainyan, Bagrat A. and Schilde, Uwe}, title = {Reaction of trifluoromethanesulfonamide with alkenes and cycloocta-1,5-diene under oxidative conditions direct assembly of 9-heterobicyclo[4.2.1]nonanes}, series = {Russian journal of organic chemistry}, volume = {47}, journal = {Russian journal of organic chemistry}, number = {9}, publisher = {Pleiades Publ.}, address = {New York}, issn = {1070-4280}, doi = {10.1134/S1070428011090016}, pages = {1271 -- 1277}, year = {2011}, abstract = {Reactions of trifluoromethanesulfonamide with alpha-methylstyrene, 2-methylpent-1-ene, and cycloocta-1,5-diene in the system t-BuOCl-NaI were studied. In the reaction with alpha-methylstyrene 1-iodo-2-phenylpropan-2-ol was the only isolated product. The reaction with 2-methylpent-1-ene gave a mixture of N,N'-(2-methylpentane-1,2-diyl)bis(trifluoromethanesulfonamide), trifluoro-N-(2-hydroxy-2-methylpentyl)-methanesulfonamide, and N,N'-[oxybis(2-methylpentan-2,1-diyl)]bis(trifluoromethanesulfonamide). Trifluoromethanesulfonamide reacted with cycloocta-1,5-diene to produce a mixture of 2,5-diiodo-9-(trifluoromethylsulfonyl)-9-azabicyclo[4.2.1]nonane and 2,5-diiodo-9-oxabicyclo[4.2.1]nonane; this reaction may be regarded as the first example of direct assembly of bicyclononane skeleton.}, language = {en} } @article{UhlemannLudwigHefeleetal.1995, author = {Uhlemann, Erhard and Ludwig, Eberhard and Hefele, Heike and Friedrich, Alwin and Kallies, Bernd and Schilde, Uwe and Hahn, Ekkehardt}, title = {Reaktionen und thermisches Verhalten oxofreier Vanadium(IV)-Komplexe. Kristallstrukturen von Methoxo- oxo[thenoyltrifluoraceton-salicylhydrazo-nato(2-)]vanadium(V) und Methoxo-oxo[benzoylaceton-salicylhydra-zonato(2- )]vanadium(V)}, year = {1995}, language = {de} } @article{UhlemannSchildeKraudeltetal.1995, author = {Uhlemann, Erhard and Schilde, Uwe and Kraudelt, Heide and Gohlke, Ulrich}, title = {Selectivity of amidoxime polymers for the sorption of gallate}, year = {1995}, language = {en} } @article{GroboschMicklerFeisteletal.2006, author = {Grobosch, Thomas and Mickler, Wulfhard and Feistel, Lothar and Schilde, Uwe}, title = {Separation of arsenic and other heavy metals with impregnated adsorber polymers : chapter 1: synthesis of the impregnation medium and separation of arsenic}, issn = {0009-286X}, doi = {10.1002/cite.200500170}, year = {2006}, language = {en} } @article{UhlemannSchildeKraudelt1994, author = {Uhlemann, Erhard and Schilde, Uwe and Kraudelt, Heide}, title = {Separation of the oxoanions of germanium, tin, arsenic, antimony, tellurium, molybdenum and tungsten with a special chelating resin containing methylaminoglucitol groups}, year = {1994}, language = {en} } @article{ShainyanTolstikovaSchilde2012, author = {Shainyan, Bagrat A. and Tolstikova, Ljudmila L. and Schilde, Uwe}, title = {Simple methods for the preparation of N-triflyl guanidines and the structure of compounds with the CF3SO2N=C-N fragment}, series = {Journal of fluorine chemistry}, volume = {135}, journal = {Journal of fluorine chemistry}, number = {1}, publisher = {Elsevier}, address = {Lausanne}, issn = {0022-1139}, doi = {10.1016/j.fluchem.2011.12.004}, pages = {261 -- 264}, year = {2012}, abstract = {Two novel and simple approaches to N-triflyl guanidines are elaborated. Owing to very strong conjugation the formally double C=N bond of TIN=C(NHR)(2) is longer than the formally single N-C bonds. Energetic effect of the triflylgroup on the conjugation in the N-C=N moiety is estimated to be >= 150 kcal/mol.}, language = {en} } @article{KruegerKellingSchildeetal.2016, author = {Kr{\"u}ger, Tobias and Kelling, Alexandra and Schilde, Uwe and Linker, Torsten}, title = {Simple Synthesis of gamma-Spirolactams by Birch Reduction of Benzoic Acids}, series = {European journal of organic chemistry}, journal = {European journal of organic chemistry}, number = {6}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {1434-193X}, doi = {10.1002/ejoc.201601650}, pages = {1074 -- 1077}, year = {2016}, abstract = {A convenient synthesis of gamma-spirolactams in only two steps was developed. Birch reduction of benzoic acids and immediate alkylation with chloroacetonitrile afforded cyclohexadienes in high yields. The products could be isolated by crystallization on a large scale in analytically pure form. Subsequent hydrogenation with platinum(IV) oxide as the catalyst reduced the nitrile functionality and the double bonds in the same step with excellent stereoselectivity. The relative configurations were determined unequivocally by X-ray analyses. Direct cyclization of the intermediary formed amino acids afforded the desired gamma-spirolactams in excellent overall yields. The procedure is characterized by few steps, cheap reagents, and can be performed on a large scale, interesting for industrial processes.}, language = {en} } @article{UhlemannSchildeKraudelt1994, author = {Uhlemann, Erhard and Schilde, Uwe and Kraudelt, Heide}, title = {Sorption of coinage metal cyano complexes by a chelating resin containing amino-glucitol groups}, year = {1994}, language = {en} } @article{KlinkaBalentovaBernatetal.2006, author = {Klinka, Karel D. and Balentova, Eva and Bern{\´a}t, Juraj and Imrich, J{\´a}n and Vavrusov{\´a}, Martina and Pihlaja, Kalevi and Koch, Andreas and Kleinpeter, Erich and Kelling, Alexandra and Schilde, Uwe}, title = {Structural revision of products resulting from the reaction of methylhydrazine with acridin-9-yl isothiocyanate due to unexpected acridinyl migration And further reactions}, issn = {1551-7004}, year = {2006}, abstract = {The reaction of methyl acridin-9-ylthiosemicarbazide under basic conditions with methyl bromoacetate resulted in a 1,3-thiazolin-4-one structure as provided by X-ray crystallography. The structure forced a re-evaluation of the reactant methyl acridin-9-ylthiosemicarbazide, originally thought to be 2-methyl 4-acridin-9-ylthiosemicarbazide based on synthetic expectations, but which when examined by X-ray crystallography was found to be in fact the isomeric 2- methyl 1-acridin-9-ylthiosemicarbazide resulting from rearrangement via a spiro form which it is in equilibrium with in solution. The product resulting from reaction with methyl iodide was also studied and the previously reported semicarbazide produced by reaction with MNO was re-examined. In both cases, the 1,2 isomer rather than the 2,4 isomer was found to be present based on the sign of the 3JCH3,N11 coupling. Full characterization of the compounds was rendered by 1H, 13C, and 15N solution-state NMR, and in the solid state, by both 13C and 15N NMR.}, language = {en} } @article{ShainyanMeshcheryakovSterkhovaetal.2008, author = {Shainyan, Bagrat A. and Meshcheryakov, Vladimir I. and Sterkhova, I. V. and Kelling, Alexandra and Schilde, Uwe}, title = {Structure of the molecule of 1,2-bis(1-ethyl-1 H -1,2,3-triazol-4-yl)diazene 1-oxide in the crystal and in solutions}, issn = {1070-4280}, year = {2008}, abstract = {Reduction of 4-nitro-1-ethyl-1H-1,2,3-triazole with aluminum in alkaline medium resulted in a syn-isomer of 1,2- bis(1-ethyl-1H-1,2,3-triazol-4-yl)diazene 1-oxide. The latter according to the data of X-ray diffraction analysis existed in the crystal as the most stable s-cis,s-trans-conformer, and in solution, as showed NMR data, as a mixture of s-cis,s-trans- and s-trans,s-trans-conformers. The data of quantum-chemical calculations are in agreement with the results of the structural studies.}, language = {en} } @article{SetoMaDavisetal.2012, author = {Seto, Jong and Ma, Yurong and Davis, Sean A. and Meldrum, Fiona and Gourrier, Aurelien and Kim, Yi-Yeoun and Schilde, Uwe and Sztucki, Michael and Burghammer, Manfred and Maltsev, Sergey and J{\"a}ger, Christian and C{\"o}lfen, Helmut}, title = {Structure-property relationships of a biological mesocrystal in the adult sea urchin spine}, series = {Proceedings of the National Academy of Sciences of the United States of America}, volume = {109}, journal = {Proceedings of the National Academy of Sciences of the United States of America}, number = {10}, publisher = {National Acad. of Sciences}, address = {Washington}, issn = {0027-8424}, doi = {10.1073/pnas.1109243109}, pages = {3699 -- 3704}, year = {2012}, abstract = {Structuring overmany length scales is a design strategy widely used in Nature to create materials with unique functional properties. We here present a comprehensive analysis of an adult sea urchin spine, and in revealing a complex, hierarchical structure, showhow Nature fabricates a material which diffracts as a single crystal of calcite and yet fractures as a glassy material. Each spine comprises a highly oriented array of Mg-calcite nanocrystals in which amorphous regions and macromolecules are embedded. It is postulated that this mesocrystalline structure forms via the crystallization of a dense array of amorphous calcium carbonate (ACC) precursor particles. A residual surface layer of ACC and/or macromolecules remains around the nanoparticle units which creates the mesocrystal structure and contributes to the conchoidal fracture behavior. Nature's demonstration of howcrystallization of an amorphous precursor phase can create a crystalline material with remarkable properties therefore provides inspiration for a novel approach to the design and synthesis of synthetic composite materials.}, language = {en} } @article{UhlemannKraudeltSchilde1995, author = {Uhlemann, Erhard and Kraudelt, Heide and Schilde, Uwe}, title = {Struktur und ausgew{\"a}hlte Reaktionen von ReCl4(PPh3)2}, year = {1995}, language = {de} } @article{UhlemannKraudeltHinscheetal.1995, author = {Uhlemann, Erhard and Kraudelt, Heide and Hinsche, Gerald and Schilde, Uwe}, title = {Struktur von Bis(3-phenyl-4-benzoyl-isoxazol-5-onato)kupfer(II)}, year = {1995}, language = {de} } @article{MondalBhuniaAttallahetal.2016, author = {Mondal, Suvendu Sekhar and Bhunia, Asamanjoy and Attallah, Ahmed G. and Matthes, Philipp R. and Kelling, Alexandra and Schilde, Uwe and M{\"u}ller-Buschbaum, Klaus and Krause-Rehberg, Reinhard and Janiak, Christoph and Holdt, Hans-J{\"u}rgen}, title = {Study of the Discrepancies between Crystallographic Porosity and Guest Access into Cadmium-Imidazolate Frameworks and Tunable Luminescence Properties by Incorporation of Lanthanides}, series = {Chemistry - a European journal}, volume = {22}, journal = {Chemistry - a European journal}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {0947-6539}, doi = {10.1002/chem.201504757}, pages = {6905 -- 6913}, year = {2016}, abstract = {An extended member of the isoreticular family of metal-imidazolate framework structures, IFP-6 (IFP=imidazolate framework Potsdam), based on cadmium metal and an in situ functionalized 2-methylimidazolate-4-amide-5-imidate linker is reported. A porous 3D framework with 1D hexagonal channels with accessible pore windows of 0.52nm has been synthesized by using an ionic liquid (IL) linker precursor. IFP-6 shows significant gas uptake capacity only for CO2 and CH4 at elevated pressure, whereas it does not adsorb N-2, H-2, and CH4 under atmospheric conditions. IFP-6 is assumed to deteriorate at the outside of the material during the activation process. This closing of the metal-organic framework (MOF) pores is proven by positron annihilation lifetime spectroscopy (PALS), which revealed inherent crystal defects. PALS results support the conservation of the inner pores of IFP-6. IFP-6 has also been successfully loaded with luminescent trivalent lanthanide ions (Ln(III)=Tb, Eu, and Sm) in a bottom-up one-pot reaction through the in situ generation of the linker ligand and in situ incorporation of photoluminescent Ln ions into the constituting network. The results of photoluminescence investigations and powder XRD provide evidence that the Ln ions are not doped as connectivity centers into the frameworks, but are instead located within the pores of the MOFs. Under UV light irradiation, Tb@IFP-6 and Eu@IFP-6 ((exc)=365nm) exhibit observable emission changes to a greenish and reddish color, respectively, as a result of strong Ln 4f emissions.}, language = {en} } @article{KammerMuellerGrunwaldetal.2006, author = {Kammer, Stefan and M{\"u}ller, Holger and Grunwald, Nicolas and Bellin, Anja and Kelling, Alexandra and Schilde, Uwe and Mickler, Wulfhard and Dosche, Carsten and Holdt, Hans-J{\"u}rgen}, title = {Supramolecular assemblies with honeycomb structures by pi-pi stacking of octahedral metal complexes of 1,12- diazaperylene}, issn = {1343-1948}, doi = {10.1002/ejic.200600092}, year = {2006}, abstract = {Homoleptic Ni-II and Fe-II complexes of the "large-surface" phenanthroline-type ligand 1,12-diazaperylene (dap), [Ni(dap)(3)](BF4)(2) (1) and [Fe(dap)(3)](PF6)(2) (2), respectively, were synthesized. In the crystal structure the complex cation [M(dap)(3)](2+) (M = Ni, Fe) exhibits C-3 symmetry and interacts with three other cations by pi-pi stacking. It forms a new metalla-supramolecular assembly with a honeycomb structure containing nanochannels running parallel to the crystallographic c axis. Aggregation by pi-pi stacking between metal complexes of "large-surface" ligands should give new perspectives for inorganic supramolecular chemistry.}, language = {en} }