F. Ungvary et al., PREPARATION AND X-RAY STRUCTURE OF (1,2-BIS(METHOXYCARBONYL)ETHYL)COBALT TRICARBONYL TRIPHENYLPHOSPHINE AND ITS ACYL PRECURSOR, Organometallics, 12(7), 1993, pp. 2849-2852
The sec-alkylcobalt carbonyl complex MeO2CCH2CH(CO2Me)Co(CO)3PPh3 (3)
and its acyl precursor MeO2CCH2CH(CO2Me)C(=O)Co(CO)3PPh3 (2) were prep
ared in 64 and 60% yields from MeO2CCH2CH(CO2Me)Co(CO)4 (1) and PPh3 a
t room temperature and at 0-degrees, respectively, and were characteri
zed by IR, H-1, C-13-{H-1}, and P-31{H-1} NMR spectroscopy. The solid-
state structure of 3 was determined by a single-crystal X-ray diffract
ion technique. The compound crystallizes in monoclinic space group P2(
1)/n with a = 1522.2(6) pm, b = 1785.8(7) pm, c = 988.0(4) pm, beta =
103.5(2)degrees, Z = 4, and R = R(w) = 0.0995.