@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{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{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{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{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{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{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{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{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} }