117931-60-9Relevant articles and documents
Metallaheteroborane Chemistry. Part 3. Synthesis of (R3 = Et3, Bun3, or Me2Ph), their Characterisation by Nuclear Magnetic Resonance Spectroscopy, and the Crystal and Molecular Structure of
Ferguson, George,Kennedy, John D.,Fontaine, Xavier L. R.,Spalding, Faridoon,Spalding, Trevor R.
, p. 2555 - 2564 (1988)
Reaction of (R3 = Et3, Bun3, or Me2Ph) with the - anion in refluxing tetrahydrofuran affords the compounds (R3 = Et3 (1), Bun3 (2) or Me2Ph (3)> as the major products.An X-ray diffraction study of (1) (recystallised from CH2Cl2) shows the crystals to be monoclinic, space group Cc with four molecules in a unit cell of dimensions a = 10.387(2), b = 17.227(4), c = 14.447(3) Angstroem, and β = 106.83(2) degree.The final R factor was 0.020 for 2 601 observed reflections.Principal interatomic distances are Pt-Te 2.704(1), Pt-P 2.320(2) and 2.341(2), Pt-B 2.248(7) - 2.295(9), Te-B 2.291(8) - 2.404(8) Angstroem.The compounds, together with the - precursor, have been examined by n. m. r. spectroscopy, and several interesting features are noted.Relative sign information for the various nJ(195Pt -1H) couplings to the heteroborane cluster protons is apparent from two-dimensional -COSY experiments, and variable-temperature 1H- spectroscopy on compound (3) reveals ΔG*328 = 62 kJ mol-1 for the rotational metal-to-heteroborane bonding fluxionality.
