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Lewis Base Adducts of Group 11 Metal Compounds. Part 24. Co-ordination of Triphenylphosphine with Silver Nitrate. A Solid-state Cross-polarisation Magic Angle Spinning 31P Nuclear Magnetic Resonance, Crystal Structure, and Infrared Spectroscopic Study of Ag(PPh3)nNO3 (n=1-4)

DOI: 10.1039/DT9860001965

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 1965 - 1970 (1986)

Update date:2022-07-30

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Authors:

Barron, Peter F.Barron, Peter F.

Dyason, Jeffery C.Dyason, Jeffery C.

Healy, Peter C.Healy, Peter C.

Engelhardt, Lutz M.Engelhardt, Lutz M.

Skelton, Brian W.Skelton, Brian W.

White, Allan H.White, Allan H.

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Article abstract of DOI:10.1039/DT9860001965

Solid-state cross-polarisation magic angle spinning 31P n.m.r. spectroscopy, single-crystal X-ray stucture determination, and i.r. spectroscopy have been used to investigate the properties of the adducts of triphenylphosphine with silver(I) nitrate: Ag(PPh3)NO3, (1); Ag(PPh3)2NO3, (2); Ag(PPh3)3NO3, (3) and Ag(PPh3)4NO3, (4).The value of 1J(Ag-P) decreases with increasing co-ordination number: (1), 780; (2), 470; (3), 310; and (4), 190 Hz, paralleling solution results.Single-crystal X-ray structure determinations of compounds (2)-(4) have been performed: (2), triclinic, space group P1, a=11.821(3), b=11.990(3), c=13.660(3) Angstroem, α=102.05(2), β=112.80(2), and γ=105.30(2) deg, yielding R=0.036 for 4090 'observed' reflections; Ag-P 2.443(1) and 2.440(1) Angstroem, P-Ag-P 138.21(5) deg; (3), monoclinic, space group P21/n, a=18.984(5), b=13.710(3), c=17.900(4) Angstroem, and β=94.94(2) deg, yielding R=0.053 for 5126 reflections; Ag-P 2.630(2), 2.525(1), and 2.545(2) Angstroem, P-Ag-P 118.37(5), 112.07(4), and 116.44(5) deg; (4), trigonal, space group R3, a=19.07(2) Angstroem, and α=43.77(5) deg, yielding R=0.060 for 1903 observed reflections; Ag-P 2.643(3) and 2.671(4) Angstroem, P-Ag-P 109.49(12) and 109.45(10) deg.Structures (2) and (3) are isomorphous with the analogous triphenylarsine compounds.In all cases the nitrate group is only weakly co-ordinated : Ag-O 2.464(4) and 2.649(4) in (2), 2.684(6) and 2.775(6) Angstroem in (3).These weak interactions are reflected in the small splitting observed for the asymmetric N-O streching vibrational mode compared to the analogous copper(I) compounds.

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