TY - JOUR A1 - Tisato, F. A1 - Refosco, F. A1 - Porchia, M. A1 - Bolzati, C. A1 - Bandoli, G. A1 - Dolmella, A. A1 - Duatti, A. A1 - Boschi, A. A1 - Jung, C. M. A1 - Pietzsch, H.-J. A1 - Kraus, Werner T1 - The Crucial Role of the Diphosphine Heteroatom X in the Stereochemistry and Stabilization of the Substitution-Inert [M(N)(PXP)]2+ Metal Fragments (M = Tc, Re; PXP = Diphosphine Ligand) N2 - The nature of the heteroatom X incorporated in the five-membered PXP-diphosphine bridging chain was found to play a primary unit role both in the overall stability and in the stereochemical arrangement of nitrido-containing [M(N)(PXP)]2+ metal fragments (M = Tc, Re). Thus, by mixing PXP ligands with labile [Re(N)Cl4]- and Tc(N)Cl2(PPh3)2 nitrido precursors in CH2Cl2/MeOH mixtures, a series of neutral M(N)Cl2(PXP) complexes (M = Tc, 1-5; M = Re, 8, 9) was collected. In the resulting distorted octahedrons, PXP adopted facial or meridional coordination, and combination with halide co-ligands produced three different stereochemical arrangements, that is, fac,cis, mer,cis, and mer,trans, depending primarily on the nature of the diphosphine heteroatom X. When X = NH, mer,cis-Tc(N)Cl2(PNP1), 1, was the only isomer formed. Alternatively, when a tertiary amine nitrogen (X = NR; R = CH3, CH2CH2OCH3) was introduced in the bridging chain, fac,cis-M(N)Cl2(PN(R)P) complexes (M = Tc, 2, 3; M = Re, 8f) were obtained. Isomerization into the mer,cis-Re(N)Cl2(PN(R)P), 8m, species was observed only in the case of rhenium when the tertiary amine group carried the less encumbering methyl substituent. fac,cis-Tc(N)Cl2(PSP), 4f, was isolated in the solid state when X = S, but a mixture of fac,cis-Tc(N)Cl2(PSP) and mer,trans-Tc(N)Cl2(PSP), 4m, isomers was found in equilibrium in the solution state. A similar equilibrium between fac,cis-M(N)Cl2(POP) (M = Tc, 5f; M = Re, 9f) and mer,trans-M(N)Cl2(POP) (M = Tc, 5m; M = Re, 9m) species was detected in POP-containing complexes. The molecular structure of all of these complexes was assessed by means of conventional physicochemical techniques including multinuclear NMR spectroscopy and X-ray diffraction analysis of representative mer,cis-Tc(N)Cl2(PN(H)P), 1, fac,cis-Tc(N)Cl2(PSP), 4f, and mer,cis-Re(N)Cl2(PN(Me)P), 8m, compounds. PY - 2004 DO - https://doi.org/10.1021/ic049139r SN - 0020-1669 SN - 1520-510X VL - 43 IS - 26 SP - 8617 EP - 8625 PB - American Chemical Society CY - Washington, DC AN - OPUS4-5546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hiebl, B. A1 - Ascher, Lena A1 - Luetzow, K. A1 - Kratz, K. A1 - Gruber, C. A1 - Mrowietz, C. A1 - Nehring, M. E. A1 - Lendlein, A. A1 - Franke, R.- P. A1 - Jung, F. T1 - Albumin solder covalently bound to a polymer membrane: New approach to improve binding strength in laser tissue soldering in-vitro N2 - Laser tissue soldering (LTS) based on indocyanine green (ICG)-mediated heat- denaturation of proteins might be a promising alternative technique for micro-suturing, but up to now the Problem of too weak shear strength of the solder welds in comparison to sutures is not solved. Earlier reports gave promising results showing that solder supported by carrier materials can enhance the cohesive strength of the liquid solder. In these studies, the solder was applied to the carriers by dip coating. Higher reliability of the connection between the solder and the carrier material is expected when the solder is bound covalently to the carrier material. In the present study a poly(ether imide) (PEI) membrane served as carrier material and ICG- supplemented albumin as solder substrate. The latter was covalently coupled to the carrier membrane under physiological conditions to prevent structural protein changes. As laser source a diode continuous-wave laser emitting at 808 nm with intensities between 250mW and 1500mW was utilized. The Albumin functionalized carrier membrane was placed onto the tunica media of explanted pig thoracic aortae forming an overlapping area of approximately 0.5×0.5 cm2. All tests were performed in a dry state to prevent laser light absorption by water. Infrared spectroscopy, spectro-photometrical determination of the secondary and Primary amine groups after acid orange II staining, contact angle measurements, and atomic force microscopy proved the successful functionalization of the PEI membrane with albumin. A laser power of 450mW LTS could generate a membrane-blood vessel connection which was characterized by a shear strength of 0.08±0.002MPa, corresponding to 15% of the tensile strength of the native blood vessel. Theoretically, an overlapping zone of 4.1mmaround the entire circumference of the blood vessel could have provided shear strength of the PEI membrane-blood vessel compound identical to the tensile strength of the native blood vessel. These in-vitro results confirmed the beneficial effects of solder reinforcement by carrier membranes, and suggest LTS with covalently bound solders on PEI substrates for further studies in animal models. KW - Tissue soldering KW - Albumin KW - Polymer membrane KW - Laser PY - 2018 DO - https://doi.org/10.3233/CH-189108 SN - 1386-0291 SN - 1875-8622 VL - 69 IS - 1-2 SP - 317 EP - 326 PB - IOS Press AN - OPUS4-45149 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kraus, Werner A1 - Walther, M. A1 - Jung, C. M. A1 - Emmerling, Franziska A1 - Pietzsch, H.-J. T1 - Bromotricarbonyl{15-[2-(methylsulfanyl)ethylsulfanyl]pentadecanoic acid-kappa2S,S'}rhenium(I) N2 - The title compound, [ReBr(C18H36O2S2)(CO)3], was synthesized and characterized as a non-radioactive surrogate of a novel Tc-containing fatty acid derivative prepared according to the tricarbonyl/dithioether design with the objective of developing new Tc-based radiopharmaceuticals for the non-invasive diagnosis of myocardial metabolism. The Re chelate contains the metal in the oxidation state +1 and is attached to the terminal position of a fatty acid. The complex formation was accomplished by a ligand exchange reaction using [NBu4]2[Re(CO)3Br3] as starting material. KW - Fatty acid KW - Tc-compound KW - Radio-pharmaceutical PY - 2006 DO - https://doi.org/10.1107/S1600536806024081 SN - 1600-5368 VL - 62 IS - 7 SP - m1660 EP - m1662 PB - Munksgaard CY - Copenhagen AN - OPUS4-12529 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Walther, M. A1 - Jung, C. M. A1 - Bergmann, R. A1 - Pietzsch, J. A1 - Rode, K. A1 - Fahmy, K. A1 - Mirtschink, P. A1 - Stehr, S. A1 - Heintz, A. A1 - Wunderlich, G. A1 - Kraus, Werner A1 - Pietzsch, H.-J. A1 - Kropp, J. A1 - Deussen, A. A1 - Spies, H. T1 - Synthesis and Biological Evaluation of a New Type of 99mTechnetium-Labeled Fatty Acid for Myocardial Metabolism Imaging PY - 2007 SN - 1043-1802 SN - 1520-4812 VL - 18 SP - 216 EP - 230 CY - Washington, DC AN - OPUS4-14514 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zeleny, R. A1 - Voorspoels, S. A1 - Ricci, M. A1 - Becker, Roland A1 - Jung, Christian A1 - Bremser, Wolfram A1 - Sittidech, M. A1 - Panyawathanakit, N. A1 - Wong, W. F. A1 - Choi, S.M. A1 - Lo, K.C. A1 - Yeung, W. Y. A1 - Kim, D.H. A1 - Han, J. A1 - Ryu, J. A1 - Mingwu, S. A1 - Chao, W. A1 - Schantz, M.M. A1 - Lippa, K.A. A1 - Matsuyama, S. T1 - Evaluation of the state-of-the-art measurement capabilities for selected PBDEs and decaBB in plastic by the international intercomparison CCQM-P114 N2 - An international intercomparison involving eight national metrology institutes (NMIs) was conducted to establish their current measurement capabilities for determining five selected congeners from the brominated flame retardant classes polybrominated diphenyl ethers and polybrominated biphenyls. A candidate reference material consisting of polypropylene fortified with technical mixtures of penta-, octa- and decabromo diphenyl ether and decabromo biphenyl, which was thoroughly assessed for material homogeneity and stability, was used as study material. The analytical procedures applied by the participants differed with regard to sample pre-treatment, extraction, clean-up, employed calibrants and type of calibration procedure as well as regarding analytical methods used for separation, identification and quantification of the flame retardant congeners (gas chromatography coupled to an electron capture detector (GC-ECD), gas chromatography-mass spectrometry in the electron ionisation mode (GC-EI-MS), gas chromatography-mass spectrometry in the electron capture negative ionisation mode (GC-ECNI-MS), and liquid chromatography-inductive coupled plasma-mass spectrometry (LC-ICP-MS)). The laboratory means agreed well with relative standard deviations of the mean of means of 1.9%, 4.8%, 5.5% and 5.4% for brominated diphenyl ether (BDE) 47, 183 and 209 and for the brominated biphenyl (BB) congener 209, respectively. For BDE 206, a relative standard deviation of 28.5% was obtained. For all five congeners, within-laboratory relative standard deviations of six measurements obtained under intermediate precision conditions were between 1% and 10%, and reported expanded measurements uncertainties typically ranged from 4% to 10% (8% to 14% for BDE 206). Furthermore, the results are in good agreement with those obtained in the characterization exercise for determining certified values for the flame retardant congeners in the same material. The results demonstrate the state-of-the-art measurement capabilities of NMIs for quantifying representative BDE congeners and BB 209 in a polymer. The outcome of this intercomparison (pilot study) in conjunction with possible improvements for employing exclusively calibrants with thoroughly assessed purity suggests that a key comparison aiming at underpinning calibration and measurement capability (CMC) claims of NMIs can be conducted. KW - Flame retardants KW - Polymer KW - Polybrominated diphenyl ethers (PBDEs) KW - Polybrominated biphenyls (PBBs) KW - International intercomparison PY - 2010 DO - https://doi.org/10.1007/s00216-009-3314-7 SN - 1618-2642 SN - 1618-2650 VL - 396 IS - 4 SP - 1501 EP - 1511 PB - Springer CY - Berlin AN - OPUS4-22905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jung, C. M. A1 - Heintz, A. A1 - Kraus, Werner A1 - Wunderlich, G. A1 - Leibnitz, Peter A1 - Pietzsch, H.-J. A1 - Kropp, J. A1 - Deussen, A. A1 - Spies, H. ED - Marino, N. T1 - Technetium- and Rhenium-Labelled Fatty Acids as Model Compounds for Myocardial Metabolism Imaging N2 - In an attempt to develop new technetium-based radiopharmaceuticals for the non-invasive diagnosis of oxidative myocardial metabolism, rhenium model compounds according to the ‚3+1' mixed ligand approach as well as the organometallic tricarbonyl-design were synthesized. The geometrical impact of different chelates on the integrity of the fatty acid head structure was determined by single crystal X-ray analyses. To evaluate the diagnostic potential of the analogous Technetium-99m compounds, fatty acid complexes of the ‚3+1' mixed ligand type were prepared on n.c.a.-level and studied in the isolated constant-flow-perfused guinea pig heart model; compared to established [123I]Iodine-labelled fatty acid radiotracers, the tested Technetium-99m derivatives showed a specific, however significantly lower myocardial extraction rate. T2 - 6th International Symposium on Technetium in Chemistry and Nuclear Medicine CY - Bressanone, Italy DA - 2002-09-04 KW - Fatty acids KW - Metabolism KW - Myocardial Imaging KW - Rhenium KW - Technetium-99m PY - 2002 UR - http://www.fzd.de/db/!Publications?pSelYear=2002&pLang=en&pNid=0&pSelWithSubmitted=0&pSelSort=TITEL&pSelPublForm=4&pSelPage=2 SN - 88-86281-73-0 N1 - Serientitel: Technetium, rhenium and other metals in chemistry and nuclear medicine – Series title: Technetium, rhenium and other metals in chemistry and nuclear medicine VL - 6 IS - 6 SP - 443 EP - 445 PB - SGEditoriali CY - Padova AN - OPUS4-1999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jung, C. M. A1 - Kraus, Werner A1 - Leibnitz, Peter A1 - Pietzsch, H.-J. A1 - Kropp, J. A1 - Spies, H. T1 - Synthesis and First Crystal Structure of Rhenium Complexes derived from omega-Functionalized Fatty Acids as Model Compounds of Technetium Tracers for Myocardial Metabolism Imaging N2 - In an attempt to develop new technetium-based radiopharmaceuticals for the noninvasive diagnosis of myocardial metabolism, we have synthesized three examples of novel metal-containing fatty acid derivatives according to the 3+1 mixed-ligand and the Schiff base/tricarbonyl design. The chelates contain the metal core in the oxidation states +5 and +1, respectively, and are attached to the end-position of a fatty acid chain. The complex formation was accomplished by ligand-exchange reactions with three different rhenium precursors, whereas the inactive rhenium metal was utilized as a surrogate of the technetium radionuclide. The molecular structures of the fatty acid complexes 7, 10 and 14 were determined by single-crystal X-ray diffraction analyses and impressively show a general problem in technetium tracer research, namely the significant structural alterations of bioactive molecules by coordination even to small metal chelates. KW - Rhenium KW - Technetium KW - Fatty acids KW - Drug research KW - Radiopharmaceuticals PY - 2002 DO - https://doi.org/10.1002/1099-0682(200205)2002:5<1219::AID-EJIC1219>3.0.CO;2-N SN - 1434-1948 SN - 1099-0682 VL - 2002 IS - 5 SP - 1219 EP - 1225 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-1552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Renz, F. A1 - Zaba, C. A1 - Roßberg, L. A1 - Jung, S. A1 - Klein, M. A1 - Klingelhöfer, G. A1 - Wünsche, A. A1 - Reinhardt, S. A1 - Menzel, Michael T1 - Spin transition in heptanuclear star-shaped iron(III)-antimony(V) NCS- and CN-bridged compounds N2 - The precursor [FeIII(L)Cl] (LH2 = N,N'-bis(2'-hydroxy-benzyliden)-1,6-diamino-3-azahexane) has been prepared and Mössbauer spectroscopy assigned a high-spin (S = 5/2) state at room temperature. The precursor is combined with the bridging units [SbV(X)6]- (X = CN-, NCS-) to yield star-shaped heptanuclear clusters [(LFeIII-X)6SbV]Cl5. The star-shaped compounds are in general high-spin systems at room temperature. On cooling to 20 K some of the iron(III) centers switch to the low-spin state as indicated by Mössbauer spectroscopy, i.e. multiple electronic transitions. While the cyano-bridged complex performs a multiple spin transition the thiocyanate-compound shows no significant population at both temperatures. KW - Heptanuclear KW - High-spin molecule KW - SbV KW - Multistability KW - Multiple spin transition PY - 2009 DO - https://doi.org/10.1016/j.poly.2008.12.027 SN - 0277-5387 VL - 28 IS - 9-10 SP - 2036 EP - 2038 PB - Elsevier CY - Amsterdam [u.a.] ; Jena AN - OPUS4-19659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -