Die Reaktion von C7H8W(CO)3 mit HBF4 in Propionsaureanhydrid fuhrt unter Protonierung des olefinischen Ringliganden zu [C7H9W(CO)3]+, das in Losung stark solvatisiert vorliegt. Es reagiert mit einer Reihe von Lewis-Basen L sehr bereitwillig zu den Komplexkationen [C7H9W(CO)3L]+ (L = PPh3, AsPh3, SbPh3, P(OMe)3, P(OPh)3), die als Tetrafluoroborate isoliert werden konnen. Mit 1,2-Bis(diphenylphosphino)-athan (PP) im Molverhaltnis 1:1 entsteht ausschlieslich der Zweikernkomplex [{C7H9W(CO)3}2(PP)]2+. Die Umsetzung von C7H8W(CO)3 mit HCl ergibt den Neutralkomplex C7H9W(CO)3Cl. Die NMR-Spektren der Kationen [C7H9W(CO)3L]+ und [{C7H9W(CO)3}2(PP)]2+, die zugleich die ersten Vertreter von π-Cycloheptadienyl-Wolframverbindungen darstellen, werden diskutiert.
Studies on the Reactivity of Metal π-Complexes. XIX. Synthesis and Properties of π-Cycloheptadienyl Tungsten Complexes
The reaction of C7H8W(CO)3 with HBF4 in propionic anhydride leads by protonation of the olefinic ring ligand to give the cation [C7H9W(CO)3]+ which is highly solvated in solution. It reacts smoothly with a number of Lewis bases L to give the corresponding complexes [C7H9W(CO)3L]+ which are isolated as the BF4 salts. With a 1:1 ratio of 1,2-bis(diphenylphosphino)-ethane (PP) the only observed product is [{C7H9W(CO)3}2(PP)]2+. The reaction of C7H8W(CO)3 with HCl yields the uncharged compound C7H9W(CO)3Cl. The n.m.r. spectra of the cation [C7H9W(CO)3L]+ and [{C7H9W(CO)3}2(PP)]2+ which are the first representatives of π-Cycloheptadienyl tungsten complexes are discussed.
[1]
H. Werner,et al.
Studies on the reactivity of metal π-complexes
,
1974
.
[2]
H. Werner,et al.
Untersuchungen zur reaktivität von metall-π-komplexen
,
1973
.
[3]
G. Natile,et al.
Use of the mass spectrometer in the elucidation of organometallic complex structures: study of two new carbonyl clusters of cobalt, SCo4(CO)9[P(CH3)2]2 and S2Co3(CO)7P(CH3)2
,
1972
.
[4]
P. Petrovskii,et al.
Protonation of metal carbonyl complexes: II. A PMR spectroscopic study of protonation in arenechromium tricarbonyls and arenechromium dicarbonyl triphenylphosphines
,
1972
.
[5]
C. P. Lillya,et al.
Tricarbonyl(arene)chromium hydride cations. Structure
,
1972
.
[6]
M. I. Foreman,et al.
A proton magnetic resonance study of π-cycloheptadienyl complexes of manganese tricarbonyl
,
1971
.
[7]
R. Shubkin,et al.
Chemistry of the cyclopentadienylmetal Carbonyls V. (A) reactions of cyclopentadienylmolybdenum and-tungsten tricarbonyl halides with group va donor ligands
,
1967
.
[8]
J. H. Richards,et al.
PROTONATION OF METALLOCENES BY STRONG ACIDS. STRUCTURE OF THE CATION
,
1960
.
[9]
H. Dauben,et al.
π-TROPENIUM-MOLYBDENUM-TRICARBONYL FLUOROBORATE
,
1958
.