[AuC
l(SMe
2)] reacts with HC
![](http://pubs.acs.org/images/entities/tbd1.gif)
CR (R = bpy
l = 2,2′-bipyridine-5-y
l (
1), phtpy
l = pheny
l-4-(2,2′:6′,2′′-terpyridine-4-y
l) (
2)) and NEt
3 (1:1:3) to afford the po
lymers [Au(C
![](http://pubs.acs.org/images/entities/tbd1.gif)
CR)]
n (R = bpy
l (
3), phtpy
l (
4)). The new a
lkyne HC
![](http://pubs.acs.org/images/entities/tbd1.gif)
Cphccbpy
l (
5, phccbpy
l = 4-C
6H
4C
![](http://pubs.acs.org/images/entities/tbd1.gif)
Cbpy
l) has been prepared by Sonogashira coup
ling of 4-Me
3SiC
![](http://pubs.acs.org/images/entities/tbd1.gif)
CC
6H
4I and
1 fo
llowed by desi
ly
lation of the resu
lting a
lkyne 4-Me
3SiC
![](http://pubs.acs.org/images/entities/tbd1.gif)
Cphccbpy
l. The a
lkyny
l Au(I) comp
le
xes [Au(C
![](http://pubs.acs.org/images/entities/tbd1.gif)
CR)L] (R = bpy
l, L = PPh
3 (
6), PTo
l3 (
7, To
l = 4-MeC
6H
4), PEt
3 (
8); R = phtpy
l, L = XyNC (
9), PPh
3 (
10); R = phccbpy
l, L = PPh
3 (
11)) have been prepared by reacting: (1)
3 or
4 with L or (2) the corresponding a
lkyne
1,
2, or
5 with [Au(acac)(PPh
3)] (acac = acety
lacetonato). The reaction of
3 or
4 with diphosphines gives [{Au(C
![](http://pubs.acs.org/images/entities/tbd1.gif)
CR)}
2(μ-Ph
2P(CH
2)
xPPh
2)] (R = bpy
l,
x = 1 (
12), 2 (
13), 4 (
14), 10 (
15); R = phtpy
l,
x = 10 (
16)). ESI mass spectrometric studies show that comp
le
xes
12–
14 are in equi
librium with the sa
lts [Au
3(C
![](http://pubs.acs.org/images/entities/tbd1.gif)
Cbpy
l)
2(μ-Ph
2P(CH
2)
xPPh
2)
2][Au(C
![](http://pubs.acs.org/images/entities/tbd1.gif)
Cbpy
l)
2], a
lthough on
ly when
x = 1 (
17) was a significant concentration of the sa
lt detected by NMR spectroscopy and iso
lated. The anionic comp
le
xes PPN[Au(C
![](http://pubs.acs.org/images/entities/tbd1.gif)
CR)
2] (R = bpy
l (
18), phtpy
l (
19), or phccbpy
l (
20)) have been prepared by reaction of the corresponding a
lkynes with PPN[Au(acac)
2]. Comp
le
xes
6,
10,
13,
14,
17, and
18 have been characterized by sing
le-crysta
l X-ray diffraction studies. The a
lkyny
l comp
le
xes are
luminescent at room temperature, disp
laying dua
l emissions.