Synthesis and characterisation of some azo-containing phosphine complexes of Au(I):: crystal and molecular structure of [Au(C≡CPh){6-P(Ph)2-1-(4-Me2N-C6H4N2)-C10H5-2-OH}]•CHCl3

Reduction of Na[AuCl4] followed by in situ addition of a stoichiometric amount of L{L = 1-(4-R-C6H4)-2-OR ' -6-Ph2P-C10H5; R ' = H, R = Me (I); R = NMe2 (II); R = NO2 (III), R ' = C(O)Me; R = Me (IV); R = NMe2 (V)} affords the Au(I) complexes [LAuCl] 1a-1e (L = I, 1a; II, 1b; III, 1c; IV, 1d; V, 1e) in good yield. Treatment of 1a-1c with two molar equivalents of LiC drop CR " (R " = Ph, " Bu) affords the acetylide containing complexes [Au(C drop CR " )L] 2a-2f {R = Ph, L = I, 2a, L = II, 2b, L = III, 2c; R = " Bu, L = I, 2d, L = II, 2e, L = III, 2f} in good yield. The reaction of Id or le with LiC drop CPh affords 2a and 2b, respectively, in which reaction of the acetylide ion with the complex takes place both at the metal centre and the ester group of the phosphine ligand. All of the compounds have been fully characterised by spectroscopic techniques and 2b(.)CHCl(3) by a single crystal X-ray diffraction study. The solid state structure of 2b(.)CHCl(3) shows a close (Cl3CHC)-C-... dropC pi -interaction and no (AuAu)-Au-... interaction. (C) 2001 Elsevier Science B.V. All rights reserved.