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48. Hydrocarbon Conversion

Author

Cassar, L., Coulson, D. R., Calcagno, B., Casey, C. P., Cenini, S., Clerici, M., Conti, F., Deganello, G., Fahey, D. R., Masters, C., Osborn, J., Schrock, R. R., Yamamoto, A., Tsutsui, Minoru, editor, and Ugo, Renato, editor

Published
1977
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49. CYCLOHEPTATRIENYL BRIDGED HETEROBIMETALLIC COMPLEXES - SYNTHESIS, FLUXIONAL BEHAVIOR AND X-RAY CRYSTAL-STRUCTURE OF SYN-[(MU-ETA(3)ETA(2)-C7H7)FE(CO)(3)PT(ETA(2),SIGMA(1)-C8H12-C5H5)]

Author

Airoldi, M, Beringhelli, T, Deganello, G, Gennaro, G, Moret, M, Saiano, F, Sironi, A, AIROLDI, M, BERINGHELLI, T, DEGANELLO, G, GENNARO, G, SAIANO, F, SIRONI, A., MORET, MASSIMO, Airoldi, M, Beringhelli, T, Deganello, G, Gennaro, G, Moret, M, Saiano, F, Sironi, A, AIROLDI, M, BERINGHELLI, T, DEGANELLO, G, GENNARO, G, SAIANO, F, SIRONI, A., and MORET, MASSIMO

Abstract

The reaction of [(eta(5)-C7H7)Fe(CO)(3)](-) with [(eta(4)-C8H12)(eta(5)-C5H5)Pt](+) leads to the formation of syn-[(mu-eta(3);eta(2)-C7H7)Fe(CO)(3)Pt(eta(2),sigma(1)-C8H12-H-12-C5H5)] (1), a bridged cycloheptatrienyl complex with an Fe-Pt bond. In solution two structural isomers of 1 are present in roughly the same concentration, whereas in the solid only one isomer is detected. Both isomers are fluxional and undergo ring whizzing of the C7H7 ring. The slow-exchange limiting NMR spectrum of the cycloheptatrienyl unit cannot be reached even at low temperature (similar to 173 K). The C7H7 ring has an uncoordinated double bond and the cyclopentadienyl unit is linked to the C8H12 ring through an sp2 carbon; the resulting cyclooctenyl unit is coordinated eta(2),sigma(1) to platinum. The C5H5 transfer, mediated by platinum, can be of interest in the synthesis of the skeleton of natural occurring products. Crystal data for syn-[(mu-eta(3);eta(2)-C7H7)Fe(CO)(3)Pt(eta(2),sigma(1)-C8H12-C5H5)]: monoclinic, space group C2/c (No.15), a=45.197(6),b=13.306(1), c=7.509(1) Angstrom, beta=92.95(1)degrees, V=4509.8(9) Angstrom(3), Z=8 R=0.033, R(w)=0.080.

Published
1995

50. Citrate-nitrate auto-combustion synthesis of perovskite-type nanopowders: a systematic approach

Author

Deganello F., Marcì G., and Deganello G.

Abstract

Citrate-nitrate auto-combustion synthesis is used to prepare an iron, a cobalt and a cerium-perovskite. The influence of different synthesis conditions on the combustion process, phase composition, textural and morphological properties is studied in detail by X-ray diffraction, nitrogen adsorption and scanning electron microscopy. Results show that the combustion intensity increases from iron, to cerium, to cobalt-perovskite. Conversely, the combustion intensity decreases and thus the safety and the gain of the combustion process increase by using high fuel/oxidant ratios, low pH values or combustion reactors with high heat dispersion capacity. High fuel/oxidant ratios increase particle size and may enhance dopant segregation. Low citric acid/metal nitrates ratios may cause precipitation of the most insoluble compounds or segregation of the dopant. High citric acid/metal nitrates ratios increase the formation temperature of the perovskite-type structure. Low pH values are deleterious for the phase composition and/or for the morphology of the final product, although at high pH values dopant segregation may occur.

Published
2009

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