@article{StrauchKossmannKellingetal.2016, author = {Strauch, Peter and Kossmann, Alexander and Kelling, Alexandra and Schilde, Uwe}, title = {EPR on bis(1,2-dithiosquarato)cuprate(II) in the bis(1,2-dithiosquarato)nickelate(II) host lattice - structure and spectroscopy}, series = {Chemical papers}, volume = {70}, journal = {Chemical papers}, publisher = {De Gruyter}, address = {Berlin}, issn = {0366-6352}, doi = {10.1515/chempap-2015-0154}, pages = {61 -- 68}, year = {2016}, abstract = {EPR spectroscopy is a well suited analytical tool to monitor the electronic situation around paramagnetic metal centres as copper(II) and therefore the structural influences on the paramagnetic ion. 1,2-Dithiosquaratometalates are available by direct synthesis from metal salts with dipotassium-1,2-dithiosquarate and the appropriate counter cations. Synthesis and characterisation of bis(benzyltributylammonium)1,2-dithiosquaratonickelate(II), (BzlBu(3)N)(2)[Ni(dtsq)(2)], and bis(benzyltributylammonium)1,2-dithiosquaratocuprate(II), (BzlBu(3)N)(2)[Cu(dtsq)(2)], with benzyltributylammonium as the counter ion is reported and the X-ray structures of two complexes, (BzlBu(3)N)(2)[Ni(dtsq)(2)] and (BzlBu(3)N)(2)[Cu(dtsq)(2)], are presented. Both complexes, crystallising in the monoclinic space group P2(1)/c, are isostructural with only small differences in the coordination sphere due to the different metal ions. The diamagnetic nickel complex is therefore well suited as a host lattice for the paramagnetic Cu(II) complex to measure EPR for additional structural information. (c) 2015 Institute of Chemistry, Slovak Academy of Sciences}, language = {en} } @article{ZabelWinterKellingetal.2016, author = {Zabel, Andre 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}, publisher = {MDPI}, address = {Basel}, issn = {1422-0067}, 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 g(perpendicular to)) 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{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{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{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} } @misc{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}, url = {http://nbn-resolving.de/urn:nbn:de:kobv:517-opus4-91470}, 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{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} }