@article{ZabelWinterKellingetal.2016, author = {Zabel, Andr{\´e} and Winter, Alette and Kelling, Alexandra and Schilde, Uwe and Strauch, Peter}, title = {Tetrabromidocuprates(II)-Synthesis, Structure and EPR}, series = {International journal of molecular sciences}, volume = {17}, journal = {International journal of molecular sciences}, number = {4}, publisher = {MDPI}, address = {Basel}, doi = {10.3390/ijms17040596}, pages = {14}, year = {2016}, abstract = {Metal-containing ionic liquids (ILs) are of interest for a variety of technical applications, e.g., particle synthesis and materials with magnetic or thermochromic properties. In this paper we report the synthesis of, and two structures for, some new tetrabromidocuprates(II) with several "onium" cations in comparison to the results of electron paramagnetic resonance (EPR) spectroscopic analyses. The sterically demanding cations were used to separate the paramagnetic Cu(II) ions for EPR measurements. The EPR hyperfine structure in the spectra of these new compounds is not resolved, due to the line broadening resulting from magnetic exchange between the still-incomplete separated paramagnetic Cu(II) centres. For the majority of compounds, the principal g values (g|| and gK) of the tensors could be determined and information on the structural changes in the [CuBr4]2- anions can be obtained. The complexes have high potential, e.g., as ionic liquids, as precursors for the synthesis of copper bromide particles, as catalytically active or paramagnetic ionic liquids.}, 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{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{KirsteBrietzkeHoldtetal.2019, author = {Kirste, Matthias and Brietzke, Thomas Martin and Holdt, Hans-J{\"u}rgen and Schilde, Uwe}, title = {The crystal structure of 1,12-diazaperylene, C₁₈H₁₀N₂}, series = {Zeitschrift f{\"u}r Kristallographie - New Crystal Structures}, volume = {234}, journal = {Zeitschrift f{\"u}r Kristallographie - New Crystal Structures}, number = {6}, publisher = {De Gruyter}, address = {Berlin}, issn = {2196-7105}, doi = {10.1515/NCRS-2019-0385}, pages = {1255 -- 1257}, year = {2019}, abstract = {C₁₈H₁₀N₂, monoclinic, P2₁/c (no. 14), a=7.9297(9) {\AA}, b=11.4021(14) {\AA}, c=13.3572(15) {\AA}, β=105.363(8)°, V =1164.5(2) {\AA}³, Z =4, Rgt(F)=0.0325, wRref(F²)=0.0774, T =210(2) K.}, language = {en} } @article{GrunwaldKellingHoldtetal.2017, author = {Grunwald, Nicolas and Kelling, Alexandra and Holdt, Hans-J{\"u}rgen and Schilde, Uwe}, title = {The crystal structure of 1,1′-bisisoquinoline, C18H12N2}, series = {Zeitschrift f{\"u}r Kristallographie : international journal for structural, physical and chemical aspects of crystalline materials. New crystal structures}, volume = {232}, journal = {Zeitschrift f{\"u}r Kristallographie : international journal for structural, physical and chemical aspects of crystalline materials. New crystal structures}, number = {5}, publisher = {de Gruyter}, address = {Berlin}, doi = {10.1515/ncrs-2017-0088}, pages = {839 -- 841}, year = {2017}, abstract = {C18H12N2, tetragonal, I41/a (no. 88), a=13.8885(6) {\AA}, c=13.6718(6) {\AA}, V =2637.2(3) {\AA}3, Z =8, Rgt(F)=0.0295, wRref(F2)=0.0854, T =210 K. CCDC no.: 631823}, 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{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{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{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} } @phdthesis{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}, doi = {10.1186/1752-153X-7-34}, year = {2013}, language = {en} } @article{AdamovichMirskovaMirskovetal.2011, author = {Adamovich, Sergey N. and Mirskova, Anna N. and Mirskov, Rudolf G. and Schilde, Uwe}, title = {Synthesis and crystal structure of 1,4,10,13-tetraoxa-7,16-diazoniumcyclo-octadecane bis(4-chloro-2-methyl-phenoxyacetate)}, series = {Chemistry central journal}, volume = {5}, journal = {Chemistry central journal}, number = {17}, publisher = {BioMed Central}, address = {London}, issn = {1752-153X}, doi = {10.1186/1752-153X-5-23}, pages = {4}, year = {2011}, abstract = {The title compound was prepared by the reaction of 1,4,10,13-tetraoxa-7,16-diazacyclo-octadecane with 4-chloro-2-methyl-phenoxyacetic acid in a ratio of 1:2. The structure has been proved by the data of elemental analysis, IR spectroscopy, NMR ((1)H, (13)C) technique and by X-ray diffraction analysis. Intermolecular hydrogen bonds between the azonium protons and oxygen atoms of the carboxylate groups were found. Immunoactive properties of the title compound have been screened. The compound has the ability to suppress spontaneous and Con A-stimulated cell proliferation in vitro and therefore can be considered as immunodepressant.}, 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{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{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{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{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{AbouserieSchildeTaubert2018, author = {Abouserie, Ahed and Schilde, Uwe and Taubert, Andreas}, title = {The crystal structure of N-butylpyridinium bis(μ2-dichlorido)-tetrachloridodicopper(II), C₁₈H₂₈N₂Cu₂Cl₆}, series = {Zeitschrift f{\"u}r Kristallographie - New Crystal Structures}, volume = {233}, journal = {Zeitschrift f{\"u}r Kristallographie - New Crystal Structures}, number = {4}, publisher = {de Gruyter}, address = {Berlin und M{\"u}nchen}, issn = {2194-4946}, doi = {10.1515/NCRS-2018-0099}, pages = {743 -- 746}, year = {2018}, abstract = {C₉H₁₄Cl₃CuN, monoclinic, P2₁/n (no. 14), a = 9.6625(6) {\AA}, b = 9.3486(3) {\AA}, c = 14.1168(8) {\AA}, β = 102.288(5)°, V = 1245.97(11) {\AA}³, Z = 4, Rgₜ(F) = 0.0182, wRᵣₑf(F²) = 0.0499, T = 210(2) K.}, language = {en} }