By reacting the dialkynes HCequivalent toC(Ar)Cequivalent toCH [Ar = 1,3-C6H4 (mphen). 1,3-(C6HMe3-2,4,6) (mes), 1,4-(C6Me4-2,3,5,6) (dur)] with [AuC1L] [L = dimethylsulfide (dms), tetrahydrothiophene (tht)] in the presence of an excess of Et3N the polymeric complexes [AuCequivalent toC(Ar)Cequivalent toCAu](n) [Ar = mphen (1), mes (2) dur (3)] were prepared. Upon reaction of these complexes with two equivalents of phosphine or isocyanide ligands (L), complexes [LAuCequivalent toC(Ar)Cequivalent toCAuL] [Ar = mes, L = (BuNC)-Bu-1 (4), XyNC (5); Ar = dur, L = PPh3 (6), (BuNC)-Bu-1 (7)] were prepared in good yields. The complex [(1)BuNCAuCequivalent toC(mphen)Cequivalent toCAuCN(t)Bu] (8) was prepared by reaction of the corresponding diethynylarene with 2 equiv. of [AuCl((CNBu)-Bu-t)] in the presence of NEt3. By reacting the appropriate diethynylarene with 2 equiv. of [Au(acac)PPh3], complexes [Ph(3)PAuCequivalent toC(Ar)Cequivalent toCAuPPh(3)] [Ar = mphen (9), mes (10)] were prepared. The carbene complex [((BuNH)-Bu-t)(Et2N)CAuCequivalent toC(mes)Cequivalent toCAuC((NHBu)-Bu-t)(NEt2)] (11) was obtained by reacting the corresponding isocyanide complex 4 with diethylamine. The crystal structures of complexes 9 and 10 have been determined by X-ray diffraction studies. In both cases one of the gold atoms is in an essentially linear environment [CAuP: 176.95(14) (9) 177.19(8)degrees (10)] while the other CAuP bond angle is appreciably bent [170.07(11) (9), 171.22(8)degrees (10)]. (C) 2002 Elsevier Science B.V. All rights reserved.