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

DOI: 10.1039/DT9880002555

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Journal of the Chemical Society, Dalton Transactions p. 2555 - 2564 (1988)

Update date:2022-08-04

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Authors:

Ferguson, George

Kennedy, John D.

Fontaine, Xavier L. R.

Spalding, Faridoon

Spalding, Trevor R.

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Article abstract of DOI:10.1039/DT9880002555

Reaction of (R3 = Et3, Buⁿ3, or Me2Ph) with the <7-TeB10H11>^- anion in refluxing tetrahydrofuran affords the compounds <2,2-(PR3)2-1,2-TePtB10H10> (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 <1H-1H>-COSY experiments, and variable-temperature 1H-<31P> spectroscopy on compound (3) reveals ΔG^*₃₂₈ = 62 kJ mol^-1 for the rotational metal-to-heteroborane bonding fluxionality.

Full text of DOI:10.1039/DT9880002555

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