TY - JOUR A1 - Kammer, Stefan A1 - Starke, Ines A1 - Pietrucha, Andreas A1 - Kelling, Alexandra A1 - Mickler, Wulfhard A1 - Schilde, Uwe A1 - Dosche, Carsten A1 - Kleinpeter, Erich A1 - Holdt, Hans-Jürgen T1 - 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 JF - Dalton transactions : a journal of inorganic chemistry, including bioinorganic, organometallic, and solid-state chemistry N2 - 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. Y1 - 2012 U6 - https://doi.org/10.1039/c2dt30412k SN - 1477-9226 VL - 41 IS - 34 SP - 10219 EP - 10227 PB - Royal Society of Chemistry CY - Cambridge ER - TY - JOUR A1 - Starke, Ines A1 - Koch, Andreas A1 - Holdt, Hans-Jürgen A1 - Kleinpeter, Erich T1 - 1H, 13C, and 15N NMR study of the solution structure of metabridged bis(benzo-15-crown-5-ether)s Y1 - 1995 ER - TY - JOUR A1 - Leitenberger, Wolfram A1 - Hartmann, Robert A1 - Pietsch, Ullrich A1 - Andritschke, Robert A1 - Starke, Ines A1 - Strüder, Lothar T1 - Application of a pnCCD in X-ray diffraction : a three-dimensional X-ray detector N2 - The first application of a pnCCD detector for X-ray scattering experiments using white synchrotron radiation at BESSY II is presented. A Cd arachidate multilayer was investigated in reflection geometry within the energy range 7 keV < E < 35 keV. At fixed angle of incidence the two-dimensional diffraction pattern containing several multilayer Bragg peaks and respective diffuse-resonant Bragg sheets were observed. Since every pixel of the detector is able to determine the energy of every incoming photon with a resolution Delta E/E similar or equal to 10(-2). a three-dimensional dataset is finally obtained. In order to achieve this energy resolution the detector was operated in the so-called single-photon- counting mode. A full dataset was evaluated taking into account all photons recorded within 10(5) detector frames at a readout rate of 200 Hz. By representing the data in reciprocal-space coordinates, it becomes obvious that this experiment with the pnCCD detector provides the same information as that obtained by combining a large number of monochromatic scattering experiments using conventional area detectors. Y1 - 2008 UR - http://onlinelibrary.wiley.com/iucr/10.1107/S0909049508018931 U6 - https://doi.org/10.1107/S0909049508018931 ER - TY - THES A1 - Starke, Ines T1 - Bestimmung der Konformation, der intramolekularen Beweglichkeit und der Komplexbildungstendenzen von Kronenethern Y1 - 1996 ER - TY - JOUR A1 - Kamm, Birgit A1 - Kamm, Michael A1 - Schmidt, Matthias A1 - Starke, Ines A1 - Kleinpeter, Erich T1 - Chemical and biochemical generation of carbohydrates from lignocellulose-feedstock (Lupinus nootkatensis) : quantification of glucose N2 - Different chemical and enzymatic methods were applied for the hydrolysis of main stems from Lupinus nootkatensis (harvest November 2002). The whole process (all steps) is based on the lignocellulose-feedstock biorefinery regime. The acid hydrolysis of L. was performed with concentrated hydrochloric acid; advantages in this process are exothermic hydrolysis and the possibility of acid recovery. Enzymatic hydrolysis achieved high yields of fermentable carbohydrates (regarding to input cellulose) with high selectivity. However, this way requires the generation of cellulose from L. by chemical pulping. Monosaccharide derivatives thus obtained were identified by their GC retention times and the corresponding MS fragmentation. Hexamethyldisilazane was used as derivatization reagent to prepare the trimethylsilyl derivatives of the carbohydrates and of the degradations products of cellulose from the different fractions. The glucose content was quantified by GC peak integration with respect to an internal standard. Y1 - 2006 UR - http://www.sciencedirect.com/science/journal/00456535 U6 - https://doi.org/10.1016/j.chemosphere.2005.03.073 SN - 0045-6535 ER - TY - JOUR A1 - Starke, Ines A1 - Kammer, Stefan A1 - Grunwald, Nicolas A1 - Schilde, Uwe A1 - Holdt, Hans-Jürgen A1 - Kleinpeter, Erich T1 - Complexation of diazaperylene and bisisoquinoline with transition metal ions in the gas phase studied by electrospray ionization mass spectrometry N2 - The complex formation of the ligands 1,12-diazaperylene (dap), 1,1-bisisoquinoline (bis), 2,2-bipyridine (bpy) and 1,10-phenanthroline (phen) with transition metal ions (M = Fe, Co, Ni, Cu, Zn, Ru, Os, Re, Pd, Pt, Ag and Cd) in the gas phase has been studied by electrospray ionization mass spectrometry. With the exception of Ru, Os, Fe, Ni and Cu, singly charged complexes [MLn]+ (n = 1,2) were observed. The complexes of dap and bis with Ru, Os, Fe and Ni ions, and the mixed ligand complexes with bpy and phen, are preferably of the doubly charged type [ML3]2+. In addition, collision- induced dissociation (CID) measurements were employed to evaluate the relative stabilities of these complexes. The CID experiments of mixed-ligand complexes which contain both dap and phen or dap and bpy exhibit preferential elimination of bpy, indicating that bpy is a weaker ligand than phen and dap. Y1 - 2008 ER - TY - JOUR A1 - Koch, Andreas A1 - Starke, Ines A1 - Kleinpeter, Erich T1 - Conformational study of Dibenzo crown ethers and their complexation with Li+ and Na+ Y1 - 1995 ER - TY - JOUR A1 - Starke, Ines A1 - Fürstenberg, Sylvia A1 - Müller, Holger A1 - Holdt, Hans-Jürgen A1 - Kleinpeter, Erich T1 - Electrospray mass spectrometric studies of the complexational behavior of maleonitrile thiacrown ethers with various metals N2 - Electrospray ionization was employed to study the mass spectrometric behavior of the maleonitrile tetrathiacrown ethers mn12S(4) (1) and mn13S(4) (2) and maleonitrile pentathiacrown ether mn15S(5) (3) and of their complexes with various metal salts (MX2, M=Pd, Pt, Ni, Co, Fe; X=Cl, CrCl3, Ni(BF4)(2), TIPF6 or Cd(NO3)(2)) and Cu(SO3CF3)(2). Both singly charged, [MXL](+) and [MXL2]+, and doubly charged complexes, [MLn](2+) (n = 2-5), were observed. The formation of the different complexes consisting of the transition metal ion, the counterion and the various crown ethers and their subsequent dissociation was also studied by collision-induced dissociation measurements which were also used to evaluate the relative stabilities of the complexes. It was found that the collisional voltages for the dissociation of the complexes were generally greater in the [MXL](+) complexes than in the corresponding [MXL2]+ complexes. Copyright (c) 2006 John Wiley & Sons, Ltd Y1 - 2006 UR - http://onlinelibrary.wiley.com/doi/10.1002/rcm.2384/full U6 - https://doi.org/10.1002/Rcm.2384 ER - TY - JOUR A1 - Starke, Ines A1 - Koch, Andreas A1 - Kammer, Stefan A1 - Holdt, Hans-Jürgen A1 - Möller, Heiko Michael T1 - Electrospray mass spectrometry and molecular modeling study of formation and stability of silver complexes with diazaperylene and bisisoquinoline JF - Journal of mass spectrometry N2 - The complex formation of the following diazaperylene ligands (L) 1,12-diazaperylene 1, 1,1-bisisoquinoline 2, 2,11-disubstituted 1,12-diazaperylenes (alkyl=methyl, ethyl, isopropyl, 3, 5, 7), 3,3-disubstituted 1,1-bisisoquinoline (alkyl=methyl, ethyl, isopropyl, 4, 6, 8 and with R=phenyl, 11 and with pyridine 12), and the 5,8-dimethoxy-substituted diazaperylene 9, 6,6-dimethoxy-substituted bisisoquinoline 10 with AgBF4 was investigated. Collision-induced dissociation measurements were used to evaluate the relative stabilities of the ligands themselves and for the [1:1](+) complexes as well as for the homoleptic and heteroleptic silver [1:2](+) complexes in the gas phase. This method is very useful in rapid screening of the stabilities of new complexes in the gas phase. The influence of the spatial arrangement of the ligands and the type of substituents employed for the complexation were examined. The effect of the preorganization of the diazaperylene on the threshold activation voltages and thus of the relative binding energies of the different complexes are discussed. Density functional theory calculations were used to calculate the optimized structures of the silver complexes and compared with the stabilities of the complexes in the gas phase for the first time. KW - electrospray ionization mass spectrometry and modeling KW - silver(1) complexes KW - stability Y1 - 2018 U6 - https://doi.org/10.1002/jms.4071 SN - 1076-5174 SN - 1096-9888 VL - 53 IS - 5 SP - 408 EP - 418 PB - Wiley CY - Hoboken ER - TY - JOUR A1 - Shainyan, Bagrat A. A1 - Moskalik, Mikail Yu A1 - Starke, Ines A1 - Schilde, Uwe T1 - Formation of unexpected products in the attempted aziridination of styrene with trifluoromethanesulfonyl nitrene N2 - 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. Y1 - 2010 UR - http://www.sciencedirect.com/science/journal/00404020 U6 - https://doi.org/10.1016/j.tet.2010.08.070 SN - 0040-4020 ER -