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The bis(-butylimido)-molybdenum(VI) framework has been used successfully in the design of vapor-phase precursors for molybdenum-containing thin films, so understanding its thermal behavior is important for such applications. Here, we report the thermal decomposition mechanism for a series of volatile bis(alkylimido)-dichloromolybdenum(VI) adducts with neutral ,'-chelating ligands, to probe the stability and decomposition pathways for these molecules. The alkyl groups explored were -butyl, -pentyl, 1-adamantyl, and a cyclic imido (from 2,5-dimethylhexane-2,5-diamine). We also report the synthesis of the new -octyl imido adducts, (OctN)MoCl·L (L = ,,','-tetramethylethylenediamine or 2,2'-bipyridine), which have been fully characterized by spectroscopic techniques as well as single-crystal X-ray diffraction and thermal analysis. We found that the decomposition of all compounds follows the same general pathway, proceeding first by the dissociation of the chelating ligand to give the coordinatively unsaturated species (RN)MoCl. Subsequent dimerization results in either an imido bridged adduct, [(RN)Mo(μ-NR)Cl], or a chloride bridged adduct, [(RN)Mo(μ-Cl)Cl], depending on the size of the R group. The dimeric species then likely undergoes an intramolecular γ-hydrogen transfer to yield a nitrido-amido adduct, (RHN)MoNCl, and an alkene. Ultimately, the resulting molybdenum species appears to decompose into free alkylamine and MoN or MoC. The thermolysis reactions have been monitored using H NMR spectroscopy, and the volatile decomposition products were analyzed using gas chromatography-mass spectrometry. A key intermediate has also been detected using electron ionization high-resolution mass spectrometry. Finally, a detailed computational investigation supports the mechanism outlined above and helps explain the relative stabilities of different ,'-chelated bis(alkylimido)-dichloromolybdenum(VI) adducts.
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Anal Biochem
December 2024
Dept. of Gerontology (AgeTech-Service Convergence Major), Graduate School of East-West Medical Science, Kyung Hee University, Yongin, Republic of Korea. Electronic address:
Triazolium α-cyclodextrin click cluster-magnetic agarose bead conjugate (CCC-MAB) was used to enrich phosphatidylinositol bisphosphates in brain tissue. The enriched sample was phosphate-methylated and analyzed by MALDI-TOF-MS/MS in positive ion mode. CCC-MAB effectively removed weak-binding interferences from the phosphoinositide extract and improved the signal-to-noise ratio.
View Article and Find Full Text PDFChem Res Toxicol
December 2024
University of Missouri, Department of Chemistry, 125 Chemistry Building, Columbia, Missouri 65211, United States.
Apurinic/apyrimidinic endonuclease 1 (APE1) is a central enzyme in the base excision repair (BER) pathway. APE1 catalyzes incision of the phosphodiester linkage on the 5'-side of apurinic/apyrimidinic (AP) sites during the repair of damaged nucleobases in cellular DNA. Inhibition of this enzyme can potentiate the action of DNA-damaging chemotherapeutic agents.
View Article and Find Full Text PDFPhys Chem Chem Phys
December 2024
School of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou, Jiangsu 225002, China.
Carboncones and fullerenes are exemplary π-conjugated carbon nanomaterials with unsaturated, positively curved surfaces, enabling the attachment of atoms or functional groups to enhance their physicochemical properties. However, predicting and understanding the addition patterns in functionalized carboncones and fullerenes are extremely challenging due to the formidable complexity of the regioselectivity exhibited in the adducts. Existing predictive models fall short in systems where the carbon molecular framework undergoes severe distortion upon high degrees of addition.
View Article and Find Full Text PDFFront Bioeng Biotechnol
December 2024
Orthopedics Department, The Second Affiliated Hospital of Guangzhou University of Chinese Medicine (Guangdong Provincial Hospital of Chinese Medicine), Guangzhou, China.
Background: Anterior tibial laxity is considered to be a risk factor for knee injuries, including anterior cruciate ligament ruptures. The anterior cruciate ligament reconstruction also aims to restore anterior tibial laxity. While anterior tibial laxity is considered to be linked to dynamic knee stability, the mechanisms connecting anterior tibial laxity to these stability issues are not fully understood.
View Article and Find Full Text PDFAm J Physiol Lung Cell Mol Physiol
December 2024
Center for Environmental Medicine, Asthma, and Lung Biology, University of North Carolina at Chapel Hill, Chapel Hill, North Carolina.
Acute exposure to ozone (O) causes upper and lower airway inflammation. We and others have previously demonstrated that O oxidizes lipids, particularly cholesterol, into electrophilic oxysterols, such as secosterol B (SecoB), which can adduct proteins, thus altering cellular signaling pathways. To investigate how O-derived oxysterols influence cytokine and chemokine release, nasal epithelial cells (HNECs) from healthy donors (N = 18 donors) were exposed to 0.
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