Karsten Gloe

Technische Universität Dresden, Dresden, Saxony, Germany

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Publications (145)311.95 Total impact

  • [Show abstract] [Hide abstract]
    ABSTRACT: Reaction of equimolar amounts of Cu(OAc)2·H2O and bis[4-(3-ethoxysalicylideneamino)phenyl]methane (H2L1) or bis[4-(3-ethoxysalicylideneamino)phenyl]sulfide (H2L2) in a 1:1 THF/MeOH mixture leads to the formation of structure-analogous CuII helicates of the composition [{Cu2L2}(H2O)2}]·4H2O. The helicates form left- and right-handed hydrogen bonded strands using the bound water molecules as glue. Finally, a compact 3D arrangement of the molecules is achieved by weak π···π and CH···π interactions. The CuII ions possess a strongly distorted tetrahedral arrangement with a N2O2 donor set of the involved diimines. In addition, the molecular structure of the ligand H2L2 was determined and solution studies of the complex formation using UV/Vis and ESI-MS were performed.
    Zeitschrift für anorganische Chemie 09/2015; 641(12). DOI:10.1002/zaac.201500547 · 1.16 Impact Factor
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    ABSTRACT: The interaction of uranyl(VI) nitrate with a series of bis(2-hydroxyaryl)imine (H2L1–H2L5) and bis(2-hydroxyaryl)amine (H2L8, H2L9) derivatives incorporating 1,3-dimethylenebenzene or 1,3-dimethylenecyclohexane bridges between nitrogen sites is reported. Crystalline complexes of type [UO2(H2L)(NO3)2] (where H2L is H2L1–H2L4) were isolated from methanol. X-ray structures of the complexes of H2L1, H2L2 and H2L4 show that each of these neutral ligands bind to their respective centres in a bidentate fashion in which coordination only occurs via each ligand’s hydroxy functions. Two bidentate nitrate anions complete the metal’s coordination sphere in each complex to yield hexagonal bipyramidal coordination geometries. A density functional theory (DFT) investigation of [UO2(H2L1)(NO3)2] in a simulated methanol environment is in accord with this complex maintaining its solid state conformation in solution. Solvent extraction experiments (water/chloroform) employing H2L1–H2L7 in the organic phase and uranyl(VI) nitrate in the aqueous phase showed that both amine derivatives, H2L8 and H2L9, yielded enhanced extraction of over the corresponding imine derivatives, H2L1 and H2L2. These results were further compared with those obtained for the corresponding Schiff bases incorporating 1,2-phenylene and 1,2-cyclohexane bridged ligands, H2L6 and H2L7; these more rigid systems also yielded enhanced extraction of relative to the more flexible Schiff bases H2L1–H2L5. A very significant synergistic enhancement of the extraction of by H2L1–H2L4 and H2L7 was observed in the presence of a 10-fold excess of n-octanoic acid; the influence of pH on extraction efficiency was also investigated. A parallel set of experiments employing H2L1–H2L9 as extractants for europium(III) nitrate indicated a clear uptake preference for over Eu3+ in all cases; separation of the uranyl ion from the rare earths is an important objective in mineral processing.
    Polyhedron 01/2015; DOI:10.1016/j.poly.2015.01.005 · 2.01 Impact Factor
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    ABSTRACT: Two tripodal ligands, each derived from 1,1,1-tris(hydroxymethyl)ethane and terminated respectively by 4-pyridyl (L1) and 2-pyridyl groups (L2), have been synthesised. Competitive seven-metal extraction studies (H2O/CHCl3) incorporating equal concentrations of cobalt(ii), nickel(ii), copper(ii), zinc(ii), silver(i), cadmium(ii), and lead(ii) in the aqueous phase and L1 or L2 in the organic phase showed selective extraction of silver(i) in each case. A parallel solvent extraction experiment involving a related tripodal tris-pyridyl ligand (L3) based on a 1,3,5-substituted aryl ring scaffold and incorporating thioether sulfurs in each tripod arm also showed extraction selectivity for silver(i); extraction efficiencies towards this metal ion fall in the order L3>L1>L2. Physical data are in accord with L1 forming a capsule-like complex of type [Ag3L12]3+ in which silver ions link pairs of pyridyl groups from different ligands. In contrast, L2 yields a complex of type [Ag2L2(NO)3]n whose X-ray structure showed it to be a two-dimensional coordination polymer in which the three pyridyl donors of each L2 coordinate to three silver(i) centres, two of which are crystallographically distinct, with the centres also bonded to bidentate and/or bridging bidentate nitrato groups.
    Australian Journal of Chemistry 01/2015; 68(4):549. DOI:10.1071/CH14540 · 1.56 Impact Factor
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    ABSTRACT: The synthesis, molecular structure as well as in situ spectroelectrochemical and electron spin resonance (ESR) studies of 5,7,8,10,15,17,18,20-octaphenyl-21,23-dithiaporphyrin (S2OPP) are presented. The compound investigated can be reversibly oxidised and reduced to yield the corresponding stable monocation and monoanion species, respectively. The experimental ESR spectrum of S2OPP•+ can be simulated taking into account the splitting constants 2xa N = 2.3 G from two dominating equivalent nitrogen nuclei. The computed spin delocalization at the density functional theory (DFT) for the cation is completely different compared to the spin delocalization of the corresponding monoanion. The largely delocalized unpaired spin density over the heteroatoms of dithiaporphyrin macrocycle was confirmed for the S2OPP•– radical anion. The role of the phenyl substitution in the meso- or β-positions of the parent 21,23-dithiaporphyrin S2P was also investigated theoretically and the results are compared with the normal (N4 core) porphyrin molecule.
    Journal of Solid State Electrochemistry 09/2014; 19(1):123. DOI:10.1007/s10008-014-2626-5 · 2.45 Impact Factor
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    ABSTRACT: A rare, discrete, mixed-valent, heterometallic Fe(III)/Cu(II) cage, [Cu6Fe8L8](ClO4)12·χsolvent (H3L = tris{[2-{(imidazole-4-yl)methylidene}amino]ethyl}amine), was designed and synthesized via metal-ion-directed self-assembly with neutral tripodal metalloligands. The formation of this coordination cage was demonstrated by X-ray crystallography, ESI mass spectrometry, FT-IR, and UV-vis-NIR spectroscopy.
    Inorganic Chemistry 01/2014; 53(2). DOI:10.1021/ic402686s · 4.76 Impact Factor
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    ABSTRACT: The 5,10,15,20-tetraphenyl-21-oxaporphyrin complexes of Mn(II), Co(II), and Zn(II) have been crystallized and studied by X-ray diffraction, NMR and UV/vis spectroscopy, and mass spectrometry as well as cyclic voltammetry. The X-ray structure of the earlier described Cu(II) complex is also reported. All complex structures possess a five-coordinate, approximately square-pyramidal geometry with a slight deviation of the heteroaromatic moieties from planarity. The packing structures are characterized by parallel strands of complex molecules interacting by weak hydrogen bonds. In the case of Zn(II) an octahedral complex has also been isolated using a side-chain hydroxy functionalized oxaporphyrin ligand; the structure was verified by NMR and EXAFS spectroscopy. Cyclic voltammetry studies reveal that the reduction of the complex bound Mn(II), Co(II), and Zn(II) ions is a ligand-centered process whereas the first oxidation step depends on the metal ion present.
    Inorganic Chemistry 01/2013; 52(3). DOI:10.1021/ic302268h · 4.76 Impact Factor
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    ABSTRACT: The structure of glycyl-l-glutamyl-l-phosphoseryl-l-leucine, (C16H29N4O11P)2·3H2O is reported. The dimeric structure is characterized by an unusual absence of head-to-tail chains in connection with an extended intermolecular hydrogen bonding network. Two of the three H2O molecules included in the network are disordered. The protonation constants of the tetrapeptide were determined as log K1 = 1.50, log K2 = 3.63, log K3 = 4.32, log K4 = 6.08 and log K5 = 8.65 by potentiometric pH titration. Graphical Abstract The dimeric structure of glycyl-l-glutamyl-l-phosphoseryl-l-leucine, (C16H29N4O11P)2·3H2O is characterized by the unusual absence of head-to-tail chains in connection with an extended intermolecular hydrogen bonding network.
    Journal of Chemical Crystallography 08/2012; 42(8). DOI:10.1007/s10870-012-0322-9 · 0.50 Impact Factor
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    ABSTRACT: The novel 1,2-bridged calix[6]arene 5 is prepared in a cyclocondensation reaction of 1,3,5,7-tetra-tert-butyl-2,6,9- trioxabicyclo[3.3.1]nona-3,7-diene-4,8-dicarbonylchloride (‘bisdioxine’) 2 with p-tert-butylcalix[6]arene. Elucidation of its structure is based on an X-ray structure determination together with supporting NMR and MS investigations. The new macrocycle 5 offers good complexation properties for Csþ ions.
    Supramolecular Chemistry 04/2012; 2012,24,279-284(4). DOI:10.1080/10610278.2012.658393 · 2.39 Impact Factor
  • Holger Stephan · Manja Kubeil · Kerstin Gloe · Karsten Gloe ·
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    ABSTRACT: This chapter contains sections titled: IntroductionThe Extraction TechniqueThe Technical ProcessThe Extraction EquilibriumPrinciples of Supramolecular ExtractionExamples of Supramolecular ExtractionConclusions and Future PerspectivesAcknowledgmentsReferences
    Analytical Methods in Supramolecular Chemistry, 03/2012: pages 105-127; , ISBN: 9783527329823
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    ABSTRACT: Reaction of equimolar amounts of AgClO4 and bis[4-(2-pyridylmethyleneamino)phenyl] methane (L1) or bis[4-(2-pyridylmethyleneamino)phenyl] ether (L2) in a 1:1 solvent mixture of CH3CN and CH2Cl2 leads to the formation of two infinite coordination polymers of the composition {[Ag(L1)]ClO4·CH3CN}n (1) and {[Ag(L2)]ClO4·CH2Cl2}n (2). Whereas 1 represents a homochiral single-stranded helicate the related complex 2 shows a typical zigzag chain arrangement. Both structures are characterized by a distorted tetrahedral coordination environment of the Ag(I) centres each based on a N4 coordination pattern of two ligand molecules. The resulting strands are connected by a hydrogen bonding network including ClO4− anions and solvent molecules forming 2-D layers. Additional π–π and CH–π interactions between the aromatic parts of the ligand molecules give a 3-D arrangement of the packing. In contrast, a discrete dinuclear metallocycle, [Ag2(L2)2](ClO4)2·CH3OH (3), has been formed by reaction of AgClO4 with L2 when CH2Cl2 in the solvent mixture was replaced by CH3OH. Again each Ag(I) has a distorted tetrahedral geometry and is coordinated to two pyridylimine units of two ligand molecules. Additional weak hydrogen bonds involving perchlorate and solvent molecules as well as edge-to-face and face-to-face π–π interactions allow a 3-D packing arrangement.
    Journal of Inclusion Phenomena 12/2011; 71(3-4). DOI:10.1007/s10847-011-0037-0 · 1.49 Impact Factor
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    ABSTRACT: 4,4′-biphenylene spaced lipophilic bis-β-diketone ligands of the type 4,4′-bis(RC(O)CH2C(O))C12H8 (R = Pr, Ph, hexyl, octyl, nonyl) have been prepared and used for the liquid–liquid extraction of d-block metal ions. These ligands are expected to interact with divalent metal ions to form charge-neutral trinuclear metallocycles of type [M3(L 3 )3(solvent)] as has been demonstrated with the previously reported derivative of H2L 3 (R = t Bu), the X-ray structure of which is reported. Liquid–liquid extraction studies were performed in a two-phase water/chloroform system employing a radiotracer technique for cobalt(II) and zinc(II). These experiments involved the systematic variation of ligand, metal and 4-ethylpyridine concentrations to probe the stoichiometries of the species extracted. Synergistic extraction was observed when 4-ethylpyridine was present with the ligand in the organic phase. Competitive extraction studies demonstrated the ligands are highly selective for copper(II) over cobalt(II), nickel(II), zinc(II) and cadmium(II).
    Journal of Inclusion Phenomena 12/2011; 71(3-4). DOI:10.1007/s10847-011-9954-1 · 1.49 Impact Factor
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    ABSTRACT: The interaction of Cu(II) with three β-diketone ligands of type R1C(O)CH2C(O)R2 (where R1 = 2-, 3-, or 4-pyridyl and R2 = C6H5, respectively), HL1−HL3, along with the X-ray structures and the pKa values of each ligand, are reported. HL1 yields a dimeric complex of type [Cu(L1)2]2. In this structure, two deprotonated HL1 ligands coordinate in a trans planar fashion around each Cu(II) center, one oxygen from each CuL2 unit bridges to an axial site of the second complex unit such that both Cu(II) centers attain equivalent five-coordinate square pyramidal geometries. The two-substituted pyridyl groups in this complex do not coordinate, perhaps reflecting steric factors associated with the closeness of the pyridyl nitrogen to the attached (conjugated) β-diketonato backbone of each ligand. The remaining two Cu(II) species, derived from HL2 and HL3, are both coordination polymers of type [Cu(L)2]n in which the terminal pyridine group of each ligand is intermolecularly linked to an adjacent copper center to generate the respective infinite structures. HL2 was also demonstrated to form a fibrous metallogel when reacted with CuCl2 in an acetonitrile/water mixture under defined conditions.
    Crystal Growth & Design 03/2011; 11(5). DOI:10.1021/cg101629w · 4.89 Impact Factor
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    ABSTRACT: The metal complexation properties of the naturally occurring Maillard reaction product isomaltol HL(2) are investigated by measurement of its stability constants with copper(II), zinc(II), and iron(III) using potentiometric pH titrations in water, by structural and magnetic characterization of its crystalline complex, [Cu(L(2))(2)]·8H(2)O, and by density functional theory calculations. Strong complexation is observed to form the bis(isomaltolato)copper(II) complex incorporating copper in a typical (pseudo-)square-planar geometry. In the solid state, extensive intra- and intermolecular hydrogen bonding involving all three oxygen functions per ligand assembles the complexes into ribbons that interact to form two-dimensional arrays; further hydrogen bonds and π interactions between the furan moiety of the anionic ligands and adjacent copper(II) centers connect the complexes in the third dimension, leading to a compact polymeric three-dimensional (3D) arrangement. The latter interactions involving copper(II), which represent an underappreciated aspect of copper(II) chemistry, are compared to similar interactions present in other copper(II) 3D structures showing interactions with benzene molecules; the results indicate that dispersion forces dominate in the π system to chelated copper(II) ion interactions.
    Inorganic Chemistry 02/2011; 50(4):1498-505. DOI:10.1021/ic102117d · 4.76 Impact Factor
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    ABSTRACT: Keywords: Nickel(II) Zinc(II) Polypyridyl X-ray structure Di(2-picolyl)amine a b s t r a c t The interaction of di(2-picolyl)amine (1) and its secondary N-substituted derivatives, N-(4-pyridylmethyl)-di(2-picolyl)amine (2), N-(4-carboxymethyl-benzyl)-di(2-picolyl)amine (3), N-(4-carboxybenzyl)-di(2-picolyl)amine (4), N-(1-naphthylmethyl)-di(2-picolyl)amine (5), N-(9-anthracenylmethyl)-di(2-picol-yl)amine (6), 1,4-bis[di(2-picolyl)aminomethyl]benzene (7), 1,3-bis[di(2-picolyl)aminomethyl]benzene (8) and 2,4,6-tris[di(2-picolyl)amino]triazine (9) with Ni(II) and/or Zn(II) nitrate has resulted in the isola-tion of [Ni(1)(NO 3) 2 ], [Ni(2)(NO 3) 2 ], [Ni(3)(NO 3) 2 ], [Ni(4)(NO 3) 2 ]ÁCH 3 CN, [Ni(5)(NO 3) 2 ], [Ni(6)(NO 3) 2 ], [Ni 2 (7)(NO 3) 4 ], [Ni 2 (8)(NO 3) 4 ], [Ni 3 (9)(NO 3) 6 ]Á3H 2 O, [Zn(3)(NO 3) 2 ]Á0.5CH 3 OH, [Zn(5)(NO 3) 2 ], [Zn(6) (NO 3) 2 ], [Zn(8)(NO 3) 2 ] and [Zn 2 (9)(NO 3) 4 ]Á0.5H 2 O. X-ray structures of [Ni(4)(NO 3) 2 ]ÁCH 3 CN, [Ni(6)(NO 3) 2 ] and [Zn(5)(NO 3) 2 ] have been obtained. Both nickel complexes exhibit related distorted octahedral coordi-nation geometries in which 4 and 6 are tridentate and bound meridionally via their respective N 3 -donor sets, with the remaining coordination positions in each complex occupied by a monodentate and a bidentate nitrato ligand. For [Ni(4)(NO 3) 2 ]ÁCH 3 CN, intramolecular hydrogen bond interactions are present between the carboxylic OH group on one complex and the oxygen of a monodentate nitrate on an adjacent complex such that the complexes are linked in chains which are in turn crosslinked by intermolecular offset p–p stacking between pyridyl rings in adjacent chains. In the case of [Ni(6)(NO 3) 2 ], two weak CHÁ Á ÁO hydrogen bonds are present between the axial methylene hydrogen atoms on one complex and the oxygen of a mono-dentate nitrate ligand on a second unit such that four hydrogen bonds link pairs of complexes; in addition, an extensive series of p–p stacking interactions link individual complex units throughout the crystal lattice. The X-ray structure of [Zn(5)(NO 3) 2 ] shows that the metal centre once again has a distorted six-coordinated geometry, with the N 3 -donor set of N-(1-naphthylmethyl)-di(2-picolyl)amine (5) coordinating in a merid-ional fashion and the remaining coordination positions occupied by a monodentate and a bidentate nitrato ligand. The crystal lattice is stabilized by weak intermolecular interactions between oxygens on the bound nitrato ligands and aromatic CH hydrogens on adjacent complexes; intermolecular p–p stacking between aromatic rings is also present.
    Polyhedron 01/2011; 30(5). DOI:10.1016/j.poly.2010.12.005 · 2.01 Impact Factor
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    ABSTRACT: ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.
    ChemInform 12/2010; 32(52). DOI:10.1002/chin.200152285
  • [Show abstract] [Hide abstract]
    ABSTRACT: ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.
    ChemInform 12/2010; 30(49). DOI:10.1002/chin.199949240
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    ABSTRACT: The binding and extraction of Ag(I) by tripodal Schiff-base ligands incorporating different aromatic podand arms are reported. These ligands have been synthesized by condensation of tris(2-aminoethyl)amine with benzaldehyde (1), 4-phenylbenzaldehyde (2), 2- (3) and 4-pyridinecarbaldehyde (4). The structures of 1 and of four Ag(I) complexes [Ag(1)]ClO4, [Ag(2)]ClO4, [Ag3(3)2](ClO4)3 and {[Ag3(4)2](ClO4)3}n have been determined by single crystal X-ray diffraction. The structure of 1 shows intramolecular C–Hπ (aromatic) interactions between phenyl rings, while bonding of Ag(I)via Ag–N interactions within the ionophore pocket is confirmed. In [Ag(1)]ClO4, and [Ag(2)]ClO4 additional long-range Ag–H interactions are observed, while π–π stacking occurs in the polynuclear species [Ag3(3)2](ClO4)3 and {[Ag3(4)2](ClO4)3}n. Potentiometric titration, liquid–liquid extraction and 1H NMR spectroscopic studies were performed to probe the nature of the silver complexes in solution. Potentiometric studies confirm increasing complex stability with Ag(I) in the order 2 < 4 < 1 < 3, and enhanced Ag(I)extraction efficiency was observed with both increasing lipophilicity of the ionophore and the presence of additional donor groups. 1H NMR spectroscopic studies were employed to probe the solution complexation behaviour of 1–4 towards Ag(I) and these confirm the formation of primarily 1:1 Ag:L complexes in solution.
    CrystEngComm 12/2010; 12(12). DOI:10.1039/c0ce00255k · 4.03 Impact Factor

  • Zeitschrift fü Chemie 11/2010; 23(11). DOI:10.1002/zfch.19830231115

  • Zeitschrift fü Chemie 11/2010; 19(11). DOI:10.1002/zfch.19790191111

  • Zeitschrift fü Chemie 10/2010; 19(10). DOI:10.1002/zfch.19790191019

Publication Stats

2k Citations
311.95 Total Impact Points


  • 1993-2015
    • Technische Universität Dresden
      • • Food Chemistry
      • • Inorganic Chemistry
      Dresden, Saxony, Germany
  • 2012
    • University of Queensland
      • School of Chemistry and Molecular Biosciences
      Brisbane, Queensland, Australia
  • 2010
    • Deen Dayal Rustagi College
      Khandela, Rajasthan, India
  • 2000
    • University of Bonn
      • Institute for Inorganic Chemistry
      Bonn, North Rhine-Westphalia, Germany
  • 1994-2000
    • Technische Universität Bergakademie Freiberg
      • Institute of Organic Chemistry
      Freiburg, Saxony, Germany
  • 1975-1992
    • Leibniz Institute for Solid State and Materials Research Dresden
      Dresden, Saxony, Germany