Beiträge zur Chemie von Phosphorverbindungen mit Adamantanstruktur. XI. Über Darstellung und Eigenschaften von Phosphoroxidsulfiden der allgemeinen Formel P4O10−nSn (n = 2−9)

Contributions to the Chemistry of Phosphorus Compounds with Adamantane-like Structure. XI. Preparation and Properties of Phosphorus Oxide Sulfides of the General Formula P₄S_10?n S_n (n = 2?9) The reaction of P₄O₁₀ with P₄S₁₀ yields a mixture of phosphorus oxide sulfides of the general formula P₄O_10?nS_n. Depending on the molar ratio P₄O₁₀: P₄S₁₀ in the starting product different amounts of the individual phosphorus oxide sulfides occuring in this reorganization product are formed. Besides the well-known P₄O₆S₄ the compounds P₄O₇S₃, P₄O₅S₅, P₄O₄S₆, P₄O₃S₇, P₄O₂S₈, and P₄OS₉ occuring for the first time were obtained by fractional distillation or crystallization. The compound P₄O₈S₂ was identified by N.M.R. spectroscopy.     

Analysis of post-translational modification and characterization of the domain structure of dynamin A from Dictyostelium discoideum

The post-translational modifications of the 96 kDa protein dynamin A from Dictyostelium discoideum were analyzed using Q-TOF mass spectrometry. The accurate molecular mass of the intact protein revealed a covalent modification causing an additional mass of 42 Da. The modification could be identified as N-terminal acetylation by tandem mass spectrometry. Extracted ion chromatograms for the a(1) and b(1) ion of the tryptic T1 peptide were used to detect the acetylated peptide within 54 nanoelectrospray ionization tandem mass spectra. Owing to the accurate molecular mass of the intact protein, additional covalent modifications could be excluded. In addition to the covalent modification, the domain structure of dynamin A was determined by applying a combination of limited proteolysis, sodium dodecylsulfate polyacrylamide gel electrophoresis, automated tandem mass spectrometry and protein database searching.     

A π-acceptor series for phosphines from51V N.M.R. data on [η5-CpV(CO)3L] complexes

Summary Qualitative molecular orbital considerations of the complexes [⁵-CPV(CO)₃ L] (L = substituted phosphane, SbPh₃, AsPh₃, CN^–) suggest that s' V chemical shift parameters () obtained for these compounds should correlate with the -acceptor abilities of L. Based on observed r-values, the ligands are arranged in sequence of their -acceptor ability, which lies in the order P(OR)₃ > CN^– > PR'₃3 SbPh₃ PPhF₂ > P(i-Bu)₃ P(NR ₂ )₃ > PPh₃ > AsPh₃ Nuclear spin-spin coupling constants J (⁵¹V-³¹ P), line widths H and i.r. data in the (CO) region are also presented.P(OR)₃ = P(OEt)₃, 4-Ethyl-l-phospha-2,6,7-trioxabicyclo[2.2.2]-octane; R = Me, n-Pr; R = Me, Et.     

Synthesen im system {carbonylmetallat/ketenimin/säure}: XXX. Neue ferra- und rhenaazetidine

The metal carbonyl anions [Fe(η-C₅H₅(CO)₂]^? and [Re(CO)₅] undergo regio- and site-specific [2 + 2]-cycloadditions with the ketenimines Ph₂CCNR (R = Me, Ph) to give the (isolable) anionic complexes [L_n$\text{M{C(CPh}{}_2\text{)N(R)C}$(O)}]^? (L_nM = Fe(η-C₅H₅)CO, Re(CO)₄) which have been alkylated and acylated at the exocyclic oxygen atom of the carbonyl function. The result is stable neutral complexes having a metallaazetidine structure which is composed of an α-metallated enamine and an N,O carbene part. IR, ¹H, and ¹³C NMR data are presented.