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N,N-Dialkylamino(thiocarbonyl)-N′-picolylbenzamidines react with (NEt4)2[M(CO)3X3] (M = Re, X = Br; M = Tc, X = Cl) under formation of neutral [M(CO)3L] complexes in high yields. The monoanionic NNS ligands bind in a facial coordination mode and can readily be modified at the (CS)NR1R2 moiety. The complexes [99Tc(CO)3(LPyMor)] and [Re(CO)3(L)] (L = LPyMor, LPyEt) were characterized by X-ray diffraction. Reactions of [99mTc(CO)3(H2O)3]+ with the N′-thiocarbamoylpicolylbenzamidines give the corresponding 99mTc complexes. The ester group in HLPyCOOEt allows linkage between biomolecules and the metal core.
Tricarbonylrhenium(I) and -technetium(I) halide (halide = Cl and Br) complexes of ligands derived from 4,5-diazafluoren-9-one (df) and 1,10-phenanthroline-5,6-dione (phen) derivatives of benzoic and 2-hydroxybenzoic acid hydrazides have been prepared. The complexes have been characterized by elemental analysis, MS, IR, 1H NMR and absorption and emission UV/Vis spectroscopic methods. The metal centres (ReI and TcI) are coordinated through the nitrogen imine atoms and establish five-membered chelate rings, whereas the hydrazone groups stand uncoordinated. The 1H NMR spectra suggest the same behaviour in solution on the basis of only marginal variations in the chemical shifts of the hydrazine protons.
Air- and water-stable phenyl complexes with nitridotechnetium(V) cores can be prepared by straightforward procedures. [TcNPh2(PPh3)2] is formed by the reaction of [TcNCl2(PPh3)2] with PhLi. The analogous N-heterocyclic carbene (NHC) compound [TcNPh2(HLPh)2], where HLPh is 1,3,4-triphenyl-1,2,4-triazol-5-ylidene, is available from (NBu4)[TcNCl4] and HLPh or its methoxo-protected form. The latter compound allows the comparison of different Tc–C bonds within one compound. Surprisingly, the Tc chemistry with such NHCs does not resemble that of corresponding Re complexes, where CH activation and orthometalation dominate.
AgTcO4 reacts with R3ECl compounds (E = C, Si, Ge, Sn, Pb; R = Me, iPr, tBu, Ph), tBu2SnCl2, or PhMgCl under formation of novel trioxotechnetium(VII) derivatives. The carbon and silicon derivatives readily undergo decomposition, which was proven by 99Tc NMR spectroscopy and the isolation of decomposition products such as [TcOCl3(THF)(OH2)]. Compounds [Ph3GeOTcO3], [(THF)Ph3SnOTcO3], [(O3TcO)SntBu2(OH)]2, and [(THF)4Mg(OTcO3)2] are more stable and were isolated in crystalline form and characterized by X-ray diffraction.
[{ReN(PMe2Ph)3}{ReO3N}]2 – Structural Evidence for the Nitridotrioxorhenate(VII) Anion, [ReO3N]2−
(2005)
Oxorhenium(V) complexes [ReOX3(PPh3)2] (X = Cl, Br) react with phenylacetylene under formation of complexes with ylide-type ligands. Compounds of the compositions [ReOCl3(PPh3){C(Ph)C(H)(PPh3)}] (1), [ReOBr3(OPPh3){C(Ph)C(H)(PPh3)}] (2), and [ReOBr3(OPPh3){C(H)C(Ph)(PPh3)}] (3) were isolated and characterized by X-ray diffraction. They contain a ligand, which was formed by a nucleophilic attack of released PPh3 at coordinated phenylacetylene. The structures of the products show that there is no preferable position for this attack. Cleavage of the Re–C bond in 3 and dimerization of the organic ligand resulted in the formation of the [{(PPh3)(H)CC(Ph)}2]2+ cation, which crystallized as its [(ReOBr4)(OReO3)]2– salt.
An amperometric bi-enzyme biosensor based on substrate recycling principle for the amplification of the sensor signal has been developed for the detection of adrenaline in blood. Adrenaline can be used as biomarker verifying successful adrenal venous sampling procedure. The adrenaline biosensor has been realized via modification of a galvanic oxygen sensor with a bi-enzyme membrane combining a genetically modified laccase and a pyrroloquinoline quinone-dependent glucose dehydrogenase. The measurement conditions such as pH value and temperature were optimized to enhance the sensor performance. A high sensitivity and a low detection limit of about 0.5–1 nM adrenaline have been achieved in phosphate buffer at pH 7.4, relevant for measurements in blood samples. The sensitivity of the biosensor to other catecholamines such as noradrenaline, dopamine and dobutamine has been studied. Finally, the sensor has been successfully applied for the detection of adrenaline in human blood plasma.
Using the OpenSim software and verified anatomical data, a computer model for the calculation of biomechanical parameters is developed and used to determine the effect of a reattachment of the Supraspinatus muscle with a medial displacement of the muscle attachment point, which may be necessary for a rupture of the supraspinatus tendon. The results include the influence of the operation on basic biomechanical parameters such as the lever arm, as well as the calculated the muscle activations for the supraspinatus and deltoid. In addition, the influence on joint stability is examined by an analysis of the joint reaction force. The study provides a detailed description of the used model, as well as medical findings to a reattachment of the supraspinatus.
Mit der Software OpenSim und überprüften anatomischen Daten wird ein Computermodell zur Berechnung von biomechanischen Parametern entwickelt und genutzt, um den Effekt einer Refixierung des Supraspinatusmuskels mit einer medialen Verschiebung des Muskelansatzpunktes zu ermitteln, wie sie unter anderem nach einem Riss der Supraspinatussehne notwendig sein kann. Die Ergebnisse umfassen hierbei den Einfluss der Operation auf grundlegende biomechanische Parameter wie den Hebelarm sowie die berechneten Muskelaktivierungen für den Supraspinatus und Deltoideus. Zusätzlich wird der Einfluss auf die Gelenkstabilität betrachtet und durch eine Analyse der Gelenkreaktionskraft untersucht. Die Studie bietet eine detaillierte Beschreibung des genutzten Modells, sowie medizinische Erkenntnisse zu einer Refixierung des Supraspinatus.
Particularly multiparous elderly women may suffer from vaginal vault prolapse after hysterectomy due to weak support from lax apical ligaments. A decreased amount of estrogen and progesterone in older age is assumed to remodel the collagen thereby reducing tissue stiffness. Sacrocolpopexy is either performed as open or laparoscopic surgery using prosthetic mesh implants to substitute lax ligaments. Y-shaped mesh models (DynaMesh, Gynemesh, and Ultrapro) are implanted in a 3D female pelvic floor finite element model in the extraperitoneal space from the vaginal cuff to the first sacral (S1) bone below promontory. Numerical simulations are conducted during Valsalva maneuver with weakened tissues modeled by reduced tissue stiffness. Tissues are modeled as incompressible, isotropic hyperelastic materials whereas the meshes are modeled either as orthotropic linear elastic or as isotropic hyperlastic materials. The positions of the vaginal cuff and the bladder base are calculated from the pubococcygeal line for female pelvic floor at rest, for prolapse and after repair using the three meshes. Due to mesh mechanics and mesh pore deformation along the loaded direction, the DynaMesh with regular rectangular mesh pores is found to provide better mechanical support to the organs than the Gynemesh and the Ultrapro with irregular hexagonal mesh pores.
Insbesondere ältere, mehrgebährende Frauen leiden häufiger an einem Scheidenvorfall nach einer Hysterektomie aufgrund der schwachen Unterstützung durch laxe apikale Bänder. Es wird angenommen, dass eine verringerte Menge an Östrogen und Progesteron im höheren Alter das Kollagen umformt, wodurch die Gewebesteifigkeit reduziert wird. Die Sakrokolpopexie ist eine offene oder laparoskopische Operation, die mit prothetischen Netzimplantaten durchgeführt wird, um laxe Bänder zu ersetzen. Y-förmige Netzmodelle (DynaMesh, Gynemesh und Ultrapro) werden in einem 3D-Modell des weiblichen Beckenbodens im extraperitonealen Raum vom Vaginalstumpf bis zum Promontorium implantiert. Numerische Simulationen werden während des Valsalva-Manövers mit geschwächtem Gewebe durchgeführt, das durch eine reduzierte Gewebesteifigkeit modelliert wird. Die Gewebe werden als inkompressible, isotrop hyperelastische Materialien modelliert, während die Netze entweder als orthotrope linear elastische oder als isotrope hyperlastische Materialien modelliert werden. Die Positionen des Vaginalstumpfs, der Blase und der Harnröhrenachse werden anhand der Pubococcygeallinie aus der Ruhelage, für den Prolaps und nach der Reparatur unter Verwendung der drei Netze berechnet. Aufgrund der Netzmechanik und der Netzporenverformung bietet das DynaMesh mit regelmäßigen rechteckigen Netzporen eine bessere mechanische Unterstützung und eine Neupositionierung des Scheidengewölbes, der Blase und der Urethraachse als Gynemesh und Ultrapro mit unregelmäßigen hexagonalen Netzporen.
The methodological discourse of mixed-methods research offers general procedures to combine quantitative and qualitative methods for investigating complex fields of research such as higher education. However, integrating different methods still poses considerable challenges. To move beyond general recommendations for mixed-methods research, this chapter proposes to discuss methodological issues with respect to a particular research domain. Taking current studies on the transition to higher education as an example, the authors first provide an overview of the potentials and limitations of quantitative and qualitative methods in the research domain. Second, they show the need for a conceptual framework grounded in the theory of the research object to guide the integration of different methods and findings. Finally, an example study that investigates transition with regard to the interplay of the individual student and the institutional context serves to illustrate the guiding role of theory. The framework integrates different theoretical perspectives on transition, informs the selection of the research methods, and defines the nexus of the two strands that constitute the mixed-methods design. As the interplay of individual and context is of concern for teaching and learning in general, the example presented may be fruitful for the wider field of higher education research.