Synthesis, single crystal X-ray structure and W-band (95 GHz) EPR spectroscopy of a new anionic isoindoline aminoxyl: synthesis and characterisation of some derivatives
Homoleptic eight-fold coordinated methylisocyanide complexes of W(IV) and
W(V) have been prepared for the first time. The reaction of [NBu4]4[W(CN)8] with methyl triflate
MeOTf gives [W(CNMe)8][OTf]4. The even stronger methylating mixture of methyl fluoride MeF
and arsenic pentafluoride AsF5 in liquid sulfur dioxide SO2 is able to fully alkylate both
[NBu4]4[W(CN)8] and [NBu4]3[W(CN)8]. The paramagnetic octakis(methylisocyanide)-
tungsten(V) [W(CNMe)8][AsF6]5 is thermally highly unstable above −30 °C. All compounds have been characterized via single-crystal X-ray diffraction, IR and Raman, as well as NMR or EPR
spectroscopy<br>
Homoleptic eight-fold coordinated methylisocyanide complexes of W(IV) and
W(V) have been prepared for the first time. The reaction of [NBu4]4[W(CN)8] with methyl triflate
MeOTf gives [W(CNMe)8][OTf]4. The even stronger methylating mixture of methyl fluoride MeF
and arsenic pentafluoride AsF5 in liquid sulfur dioxide SO2 is able to fully alkylate both
[NBu4]4[W(CN)8] and [NBu4]3[W(CN)8]. The paramagnetic octakis(methylisocyanide)-
tungsten(V) [W(CNMe)8][AsF6]5 is thermally highly unstable above −30 °C. All compounds have been characterized via single-crystal X-ray diffraction, IR and Raman, as well as NMR or EPR
spectroscopy<br>
The use of a sodium in sodium chloride dispersion is systematically evaluated for the synthesis of nickel(0) and nickel(I) complexes from readily-prepared nickel(II) precursors. A variety of complexes with phosphine and bipyridine-type ligands were accessed, although some reactions were found to produce mixtures of nickel(0) and nickel(I), and yields were highly variable. Several new nickel(I) complexes were obtained, and these were characterised using techniques including NMR spectroscopy, EPR spectroscopy, and single crystal X-ray diffraction analysis.
The binding of O2 at a four-coordinate cobaltous porphyrin site within a metal–organic framework is examined through single-crystal X-ray diffraction, EPR spectroscopy, and O2 adsorption measurements.
Uniaxial compression tests and hydrostatic tests at pressures up to 27 kbars have been performed to determine operating slip systems in single crystal and polycrystal1ine beryllium. A recent study has been made of wave propagation in single crystal beryllium by shock loading to selectively activate various slip systems, and this has been followed by a study of wave propagation and spallation in textured, polycrystal1ine beryllium. An alteration in the X-ray diffraction pattern has been noted after shock loading, but this alteration has not yet been correlated with any structural change occurring during shock loading of polycrystal1ine beryllium.This study is being conducted in an effort to characterize the effects of shock loading on textured, polycrystal1ine beryllium. Samples were fabricated from a billet of Kawecki-Berylco hot pressed HP-10 beryllium.
AbstractA new type of inclusion complex, S(–)-1 phenyl ethyl ammonium percholorate complex of R-(–)-2-ethyl - N - benzyl - 4, 7, 10, 13 - tetraoxa -1- azacyclopentadecane, has been prepared and studied by NMR, IR and single crystal X-ray diffraction techniques. The compound crystallizes in space group
Eightfold Electrophilic Methylation of Octacyanotungstate [W(CN)8]4−/3−: Preparation of Homoleptic, Eight-coordinate Methylisocyanide Complexes [W(CNMe)8]4+/5+