29890-05-9Relevant articles and documents
Preparation of solid-state samples of a transition metal coordination compound for synchrotron radiation photoemission studies
Crotti, Corrado,Farnetti, Erica,Celestino, Teresa,Fontana, Stefano
, p. 141 - 157 (2003)
The aim of this research was to identify a sample preparation method suitable for the study of transition metal complexes by photoemission spectroscopy with synchrotron radiation as the X-ray source, even in the case where the compound is not evaporable. Solid-phase samples of W(CO)4(dppe) [dppe=1,2-bis(diphenylphosphino)ethane] were prepared according to different methods and their synchrotron radiation XPS spectra measured. The spectra acquired from samples prepared by spin coating show core level peaks only slightly broader than the spectrum recorded from UHV evaporated samples. Moreover, for these samples the reproducibility of the binding energy values is excellent. The dependence of the spin coating technique on parameters such as solvent and solution concentration, spinning speed and support material was studied. The same preparation method also allowed the acquisition of valence band spectra, the main peaks of which were clearly resolved. The results suggest that use of the spin coating technique may allow us to reveal small differences in core level binding energies due to ligand substitution.
Synthesis, spectroscopy and electronic structure of the vinylidene and alkynyl complexes [W(CCHR)(dppe)(η-C7H7)]+ and [W(CCR)(dppe)(η-C7H7)]n+ (n = 0 or 1)
Lancashire, Hannah N.,Brown, Neil J.,Carthy, Laura,Collison, David,Fitzgerald, Emma C.,Edge, Ruth,Helliwell, Madeleine,Holden, Mark,Low, Paul J.,McDouall, Joseph J. W.,Whiteley, Mark W.
, p. 1267 - 1278 (2011)
The first examples of vinylidene complexes of the cycloheptatrienyl tungsten system [W(CCHR)(dppe)(η-C7H7)]+ (dppe = Ph2PCH2CH2PPh2; R = H, 3; Ph, 4; C6H4-4
Rapid synthesis of Group VI carbonyl complexes by coupling borohydride catalysis and microwave heating
Birdwhistell, Kurt R.,Schulz, Brian E.,Dizon, Paula M.
, p. 69 - 71 (2013/01/15)
Several Group VI tetracarbonyl phosphine and tertiary amine complexes [M(CO)4 L2, M = Cr, Mo, W, L2 = 2PPh 3, dppm, dppe, dppp, dppb, bpy, phen, dppf] were synthesized in minutes in the microwave at moderate temperature, atmospheric pressure, and utilizing NaBH4 as a catalyst. The reactions were optimized by careful solvent selection. The octahedral complexes were isolated in percent yields ranging from 17 to 95. The lower temperatures, shorter reaction times, benign solvents, and lower pressures as compared to the traditional thermal syntheses provide a rapid, eco-friendly synthetic route to these common Group VI complexes.