TY - JOUR A1 - Kozlevcar, Bojan A1 - Gamez, Patrick A1 - de Gelder, Rene A1 - Jaglicic, Zvonko A1 - Strauch, Peter A1 - Kitanovski, Nives A1 - Reedijk, Jan T1 - Counterion and solvent effects on the primary coordination sphere of copper(II) Bis(3,5-dimethylpyrazol-1-yl)acetic acid coordination compounds JF - European journal of inorganic chemistry : a journal of ChemPubSoc Europe N2 - Four copper(II) coordination compounds with the neutral ligand bis(3,5-dimethylpyrazol-1-yl)acetic acid (Hbdmpza, C(12)H(16)N(4)O(2)) and its anionic form (bdmpza(-)), namely [Cu(Hbdmpza)(2)](HSO(4))(2) (1), [Cu(Hbdmpza)(2)]Cl(2) (2), [Cu(bdmpza)(2)](CH(3)COOH)(H(2)O) (3), and [Cu(bdmpza)(2)][Cu(2)(O(2)CCH(3))(4)] (4) have been synthesized starting from different metal salts. All the compounds have been fully characterized by physical and analytical methods. In addition, a single-crystal XRD analysis revealed the 3D structure of 1, which exhibits tridentate, vicinal N,N,O-coordination of two symmetry-related Hbdmpza ligands in an elongated octahedral arrangement with four equatorial nitrogen atoms and two axial oxygen atoms. The neutral carboxylic moiety acts as a hydrogen-bond donor to a HSO(4)(-) counterion. The two hydrogensulfates form a unique hydrogen-bonded pair (HSO(4)(-))(2) with very short O center dot center dot center dot O distances (2.59 angstrom) bridged between adjacent [Cu(HL)(2)](2+) coordination units. Also a short O center dot center dot center dot O contact (2.54 angstrom) is present between the C-OH and an 0 of a hydrogensulfate. A characteristic IR C=O vibration is observed at 1700 cm(-1) for 1 and 2, whereas the v(as)(O(2)C) vibration is present at 1650 cm(-1) for 3 and 4. These IR data strongly suggest the presence of Hbdmpza ligands in 1 and 2 and the deprotonated form bdmpza- in 3 and 4. A mononuclear coordination unit [CuL(2)], as proven for 1 by X-ray diffraction, is also proposed for the other compounds 2-4. In compound 4, an additional dinuclear [Cu(2)(O(2)CCH(3))(4)] neutral coordination unit is present, as deduced from the vibration bands v(as)(O(2)C) at 1600 cm(-1) and v(s)(O(2)C) at 1420 cm(-1), which are typical of a carboxylate function, and from the two-species analysis of the chi(M)T(T) curve of the magnetic susceptibility data (2J = -322 cm(-1)). Also, the EPR spectra recorded at different temperatures agree with this structure. KW - Copper KW - Coordination modes KW - Hydrogen bonds KW - Counterions KW - Solvent effects Y1 - 2011 U6 - https://doi.org/10.1002/ejic.201100410 SN - 1434-1948 IS - 24 SP - 3650 EP - 3655 PB - Wiley-Blackwell CY - Malden ER - TY - JOUR A1 - Neumann, Mike A1 - Noeske, Robert A1 - Bach, Grete A1 - Glaubauf, Thomas A1 - Bartoszek, Michael A1 - Strauch, Peter T1 - A procedure for rapid determination of the silicon content in plant materials JF - Zeitschrift für Naturforschung : B, Chemical sciences N2 - An efficient, reliable and low-cost procedure to determine the silicon content in plant material is presented which allows to monitor the agricultural aspects like growth and yield. The presented procedure consists of a hydrochloric acid pre-treatment and a subsequent thermal oxidation. The method is compared to other processes like dissolution in hydrofluoric acid combined with ICP OES, energy-dispersive X-ray fluorescence spectroscopy (EDXRF) or aqua regia treatment. KW - Silica Determination KW - Silicon Content KW - Plant Material Y1 - 2011 SN - 0932-0776 VL - 66 IS - 3 SP - 289 EP - 294 PB - De Gruyter CY - Tübingen ER - TY - JOUR A1 - Awad, Duha Jawad A1 - Schilde, Uwe A1 - Strauch, Peter T1 - 4,4 '-Bis(tert-butyl)-2,2 '-bipyridinedichlorometal(II) - Synthesis, structure and EPR spectroscopy JF - Inorganica chimica acta : the international inorganic chemistry journal N2 - 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. KW - 4,4 '-Bis(tert-butyl)-2,2 '-bipyridine KW - X-ray structure KW - EPR KW - Copper(II) KW - Transition metals Y1 - 2011 U6 - https://doi.org/10.1016/j.ica.2010.08.035 SN - 0020-1693 VL - 365 IS - 1 SP - 127 EP - 132 PB - Elsevier CY - Lausanne ER - TY - JOUR A1 - Farra, Ramzi A1 - Thiel, Kerstin A1 - Winter, Alette A1 - Klamroth, Tillmann A1 - Poeppl, Andreas A1 - Kelling, Alexandra A1 - Schilde, Uwe A1 - Taubert, Andreas A1 - Strauch, Peter T1 - Tetrahalidocuprates(II)-structure and EPR spectroscopy Part 1: Tetrabromidocuprates(II) JF - New journal of chemistry N2 - Tetrahalidocuprates(II) show a high degree of structural flexibility. We present the results of crystallographic and electron paramagnetic resonance (EPR) spectroscopic analyses of four new tetrabromidocuprate(II) compounds and compare the results with previously reported data. The cations in the new compounds are the sterically demanding benzyltriphenylphosphonium, methyltriphenylphosphonium, tetraphenylphosphonium, and hexadecyltrimethylammonium ions; they were used to achieve a reasonable separation of the paramagnetic Cu(II) ions for EPR spectroscopy. X-Ray crystallography shows that in all four complexes the [CuBr4](2-) units have a distorted tetrahedral coordination geometry which is in agreement with DFT calculations. The EPR hyperfine structure was not resolved. This is due to the exchange broadening resulting from still incomplete separation of the paramagnetic Cu(II) centres. Nevertheless, the principal values of the electron Zeemann tensor (g(parallel to) and g(perpendicular to)) of the complexes could be determined. A correlation of structural (X-ray) parameters with the spin density at the copper centres (DFT) is well reflected in the EPR spectra of the bromidocuprates. This enables the correlation of X-ray and EPR parameters to predict the structure of tetrabromidocuprates in physical states other than the crystalline state. As a result, we provide a method to structurally characterize [CuBr4](2-) in, for example, ionic liquids or in solution, which has important implications for e.g. catalysis or materials science. Y1 - 2011 U6 - https://doi.org/10.1039/c1nj20271e SN - 1144-0546 VL - 35 IS - 12 SP - 2793 EP - 2803 PB - Royal Society of Chemistry CY - Cambridge ER - TY - JOUR A1 - Thiel, Kerstin A1 - Klamroth, Tillmann A1 - Strauch, Peter A1 - Taubert, Andreas T1 - On the interaction of ascorbic acid and the tetrachlorocuprate ion [CuCl4](2-) in CuCl nanoplatelet formation from an ionic liquid precursor (ILP) JF - Physical chemistry, chemical physics : a journal of European Chemical Societies N2 - The formation of CuCl nanoplatelets from the ionic liquid precursor (ILP) butylpyridinium tetrachlorocuprate [C4Py](2)[CuCl4] using ascorbic acid as a reducing agent was investigated. In particular, electron paramagnetic resonance (EPR) spectroscopy was used to evaluate the interaction between ascorbic acid and the Cu(II) ion before reduction to Cu(I). EPR spectroscopy suggests that the [CuCl4](2-) ion in the neat IL is a distorted tetrahedron, consistent with DFT calculations. Addition of ascorbic acid leads to the removal of one chloride from the [CuCl4](2-) anion, as shown by DFT and the loss of symmetry by EPR. DFT furthermore suggests that the most stable adduct is formed when only one hydroxyl group of the ascorbic acid coordinates to the Cu(II) ion. Y1 - 2011 U6 - https://doi.org/10.1039/c1cp20648f SN - 1463-9076 VL - 13 IS - 30 SP - 13537 EP - 13543 PB - Royal Society of Chemistry CY - Cambridge ER -