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Studies of NO3, Ag(P(CH2CH2CN)3)2>NO3 and NO3 by X-Ray Diffraction and Solid-state Nuclear Magnetic Resonance

DOI: 10.1039/DT9950003691

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 3691 - 3698 (1995)

Update date:2022-09-26

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Authors:

Liu, C. W.Liu, C. W.

Pan, HongjunPan, Hongjun

Fackler, John P.Fackler, John P.

Wu, GangWu, Gang

Wasylishen, Roderick E.Wasylishen, Roderick E.

Shang, MaoyuShang, Maoyu

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Article abstract of DOI:10.1039/DT9950003691

Solid-state magic angle spinning (MAS) 31P NMR spectra of NO3 1, NO3 2 and Ag(P(C6H4Me-m)3)2>NO3 3 have been obtained.In addition, the crystal structures for 2 and 3 have been determined.The results from the high-resolution NMR study are consistent with the known structure of 1 and the structures of 2 and 3.In each case the 31P NMR spectra exhibit resolved splittings arising from 107Ag and 109Ag with 1J(109Ag31P) values of 524, 564 and 517 Hz for 1, 2 and 3, respectively.In 1 the two phosphorous nuclei are crystallogrphically nonequivalent, thus analysis of the 31P NMR spectrum indicates two chemically shifted phosphorous nuclei, δA 9.50 and δB 7.67, with 2J(31PA31PB) = 125 Hz.The two phosphorous nuclei of 2 are crystallographically and magnetically equivalent in the solid state as evident from the cross polarization/MAS 31P NMR spectrum, δ -9.56.Crystals of 2 are trigonal, space group <*> a = 12.204(2), c = 26.418(5) Angstroem, Z = 6.The Ag and P atoms are located on a three-fold rotation axis with Ag at the centre of inversion.The Ag-P bond distance is 2.383(1) Angstroem.The conformation of the cyanoethylphosphine ligands in 2 is analogous to the ribs of an umbrella in which the silver atom is encapsulated by the six cyano groups with an Ag...N separation of 3.439(2) Angstroem.The two phosphorous nuclei in 3 are crystallographically equivalent but magnetically non-equivalent since the molecule sits on a two-fold axis but lacks a centre of inversion.As a consequence of this symmetry the two phosphorous nuclei have identical chemical shifts, δ 11.2; however, 2J(31P31P) can be determined from slow MAS experiments.For 3 the space group is orthorombic Aba2, a = 15.142(1), b = 24.917(2), c = 10.2536(7) Angstrom, Z = 4.The two phosphorous atoms are related by a crystallographically imposed two-fold axis.The nitrate group is chelated symmetrically to the Ag atom.

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