Mc. Suen et al., SYNTHESES, STRUCTURES AND SPECTROSCOPIC STUDIES OF QUADRUPLY BONDED COMPLEXES CONTAINING BRIDGING ACETATE AND ETA(3)-ETP LIGANDS (ETP = PH2PCH2CH2P(PH)CH2CH2PPH2), Journal of the Chinese Chemical Society, 45(2), 1998, pp. 263-268
The quadruply bonded complexes containing bridging acetate and polyden
tate phosphine ligands of die type Mo-2(O2CCR3)X-3(eta(3)-etp) (R = H,
X = Br, 1; R = F, X = Cl, 2; R = F, X = Br, 3; etp = Ph2PCH2CH2P(Ph)C
H2CH2PPh2) were prepared by reactions of MO2(O2CCR3)X-2(PPh3)(2) with
etp in CH2X2. Their UV-vis and P-31{H-1}-NMR spectra have been recorde
d, and the structure of 1 has been determined by X-ray crystallography
. Crystal data for 1.2CH(2)Br(2): space group P2(1)/c, a = 13.924(7) A
ngstrom, b = 21.157(4) Angstrom, c = 14.427(5) Angstrom, beta = 101.82
(3)degrees, V = 4159(2) Angstrom(3), Z = 4, with final residuals R = 0
.0797 and Rw = 0.0793. The absorption wavelengths of the delta --> del
ta transitions and the chemical shifts and the coupling constants of
the P-31 {H-1}-NMR spectra of these complexes are dependent on the nat
ures of the halogen atoms and the acetate ligands.