TY - JOUR
T1 - Platinum bis(phosphine) complexes of 1,8-naphthosultam
AU - Diamond, Louise M.
AU - Knight, Fergus R.
AU - Randall, Rebecca A. M.
AU - Fuller, Amy L.
AU - Slawin, Alexandra M. Z.
AU - Woollins, J. Derek
N1 - The work in this project was supported by the Engineering and Physical Sciences Research Council (EPSRC).
PY - 2014/11/1
Y1 - 2014/11/1
N2 - A series of bis(phosphine) platinum complexes 1-4 and 6-8 that bear the 1,8-naphthosultam ligand (L) have been synthesised. The nitrogen atom in L was deprotonated with sodium tert-butoxide to form the sodium salt. Metathetical reaction of the sodium salt (1 eq.) with the appropriate cis-dichlorobis(phosphine) platinum (1 eq.) in THF resulted in the formation of platinum complexes [Pt(PR3)2(L)Cl] (R3 = Ph3; 1, Ph2Me; 2, PhMe2; 3, Me3; 4), whilst reaction with [Pt(COD)Cl2] afforded [Pt(COD)(L)Cl] (5). The corresponding reaction employing two equivalents of L, two equivalents of NaOtBu and one equivalent of [Pt(PR3)2Cl2]/[Pt(COD)Cl2] yielded complexes [Pt(PR3)2(L)2] (R3 = Ph2Me; 6, PhMe2; 7, Me3; 8) and [Pt(COD)(L)2] (9). L, 1, 5 and 9 have been fully characterised, principally by multinuclear magnetic resonance and IR spectroscopy and mass spectrometry, the remaining members of the series were analysed by 31P NMR only. Unsymmetrical complexes 1-4 provide examples of AX spin systems, with appropriate satellites attributed to 31P NMR-195Pt coupling. X-ray structures determined for 1,8-naphthosultam L, and complexes 1, 5 and 9 and where appropriate the platinum metal geometry, N-S distance and ligand distortions were compared.
AB - A series of bis(phosphine) platinum complexes 1-4 and 6-8 that bear the 1,8-naphthosultam ligand (L) have been synthesised. The nitrogen atom in L was deprotonated with sodium tert-butoxide to form the sodium salt. Metathetical reaction of the sodium salt (1 eq.) with the appropriate cis-dichlorobis(phosphine) platinum (1 eq.) in THF resulted in the formation of platinum complexes [Pt(PR3)2(L)Cl] (R3 = Ph3; 1, Ph2Me; 2, PhMe2; 3, Me3; 4), whilst reaction with [Pt(COD)Cl2] afforded [Pt(COD)(L)Cl] (5). The corresponding reaction employing two equivalents of L, two equivalents of NaOtBu and one equivalent of [Pt(PR3)2Cl2]/[Pt(COD)Cl2] yielded complexes [Pt(PR3)2(L)2] (R3 = Ph2Me; 6, PhMe2; 7, Me3; 8) and [Pt(COD)(L)2] (9). L, 1, 5 and 9 have been fully characterised, principally by multinuclear magnetic resonance and IR spectroscopy and mass spectrometry, the remaining members of the series were analysed by 31P NMR only. Unsymmetrical complexes 1-4 provide examples of AX spin systems, with appropriate satellites attributed to 31P NMR-195Pt coupling. X-ray structures determined for 1,8-naphthosultam L, and complexes 1, 5 and 9 and where appropriate the platinum metal geometry, N-S distance and ligand distortions were compared.
KW - Platinum
KW - Naphthalene
KW - Sulfam
KW - Complex
KW - X-ray structure
KW - Ray-diffraction data
KW - X-ray
KW - Metal tetrathiolenes
KW - Arenethiolatocopper(I) complexes
KW - Crystal-structures
KW - Ligands
KW - Coordination
KW - Cod
KW - Tetrathionaphthalene
UR - http://www.sciencedirect.com/science/article/pii/S0020169314005489#appd002
U2 - 10.1016/j.ica.2014.08.048
DO - 10.1016/j.ica.2014.08.048
M3 - Article
SN - 0020-1693
VL - 423
SP - 313
EP - 319
JO - Inorganica Chimica Acta
JF - Inorganica Chimica Acta
IS - Part A
ER -