Heteroleptic gold complexes with 4,5-diselenolate-1,3-dithiole-2-thione (C3S2Se22-, dsit)

Article abstract of DOI:10.1139/v98-101

The reaction of (NBu₄)₂[Zn(dsit)₂] (dsit = 4,5-diselenolate-1,3- dithiole-2-thione) with AuClL in a 1:4 ratio leads to [Au₂(dsit)L₂] (L = PPh₃ (1), PPh₂Me (2)), transferring the diselenolate group. Complex 2 reacts further with equimolar amounts of [Au(OClO₃)L], affording the trinuclear complex [Au₃(dsit)(PPh₂Me)₃]ClO₄ (3). When the reaction of (NBu₄)₂[Zn(dsit)₂] with [Au₂Cl₂(P-P)] was carried out in a 1:2 ratio, complexes [Au₂(dsit)(P-P)](n) (P-P = dppe (1,2- bis(diphenylphosphine)ethane), n = 1 (4); P-P = dppm (bis(diphenylphosphine)methane), n = 2 (5)) are obtained. Anionic derivatives such as (NBu₄)[Au(dsit)₂] (6) could be obtained by reaction of the zinc complex with (NBu₄)[AuBr₄] in a 1:1 ratio while other gold complexes require a tin complex as ligand transfer so [Sn(dsit)Me₂] (7), obtained from the zinc complex and [SnCl₂Me₂], reacts with PPN[Au(C₆F₅)Cl] (PPN = bis(triphenylphosphine)iminium) or [AuBr₂(S₂CNR₂)] affording [AU(dsit)(S₂CNR₂)] (R = Me (8); R: Bz (9)) or (PPN)₂[Au₂(dsit)(C₆F₅)₂] (10), respectively. Electrochemical oxidation of 6 gives (NBu₄)_0.4[Au(dsit)₂] (11) and the reaction with (TTF)₃(BF₄)₂ (TTF = tetrathiafulvalene) affords (TTF)[Au(dsit)₂] (12). Electrical conductivities of these complexes at room temperature in compacted pellets are 3 x 10^-8 (11) and 5 x 10^-3 (12) S cm^-1.

Full text of DOI:10.1139/v98-101

1033
Heteroleptic gold complexes with 4,5-
diselenolate-1,3-dithiole-2-thione (C3S3Se2 , dsit)
2–
Elena Cerrada and Mariano Laguna
Abstract: The reaction of (NBu4)2[Zn(dsit)2] (dsit = 4,5-diselenolate-1,3-dithiole-2-thione) with AuClL in a 1:4 ratio
leads to [Au2(dsit)L2] (L = PPh3 (1), PPh2Me (2)), transferring the diselenolate group. Complex 2 reacts further with
equimolar amounts of [Au(OClO3)L], affording the trinuclear complex [Au3(dsit)(PPh2Me)3]ClO4 (3). When the
reaction of (NBu4)2[Zn(dsit)2] with [Au2Cl2(P-P)] was carried out in a 1:2 ratio, complexes [Au2(dsit)(P-P)]n (P-P =
dppe (1,2-bis(diphenylphosphine)ethane), n = 1 (4); P-P = dppm (bis(diphenylphosphine)methane), n = 2 (5)) are
obtained. Anionic derivatives such as (NBu4)[Au(dsit)2] (6) could be obtained by reaction of the zinc complex with
(NBu4)[AuBr4] in a 1:1 ratio while other gold complexes require a tin complex as ligand transfer. So [Sn(dsit)Me2] (7),
obtained from the zinc complex and [SnCl2Me2], reacts with PPN[Au(C6F5)Cl] (PPN =
bis(triphenylphosphine)iminium) or [AuBr2(S2CNR2)] affording [Au(dsit)(S2CNR2)] (R = Me (8); R = Bz (9)) or
(PPN)2[Au2(dsit)(C6F5)2] (10), respectively. Electrochemical oxidation of 6 gives (NBu4)0.4[Au(dsit)2] (11) and the
reaction with (TTF)3(BF4)2 (TTF = tetrathiafulvalene) affords (TTF)[Au(dsit)2] (12). Electrical conductivities of these
complexes at room temperature in compacted pellets are 3 × 10–8 (11) and 5 × 10–3 (12) S cm–1.
Key words: diselenolate, dsit, gold complexes, tin complexes.
Résumé : La réaction du (NBu4)2[Zn(dsit)2] (dsit = 4,5-disélénaloate-1,3-dithiole-2-thione) avec le AuClL dans un
rapport de 1 : 4 conduit au [Au2(dsit)L2] (L = PPh3 (1), PPh2Me (2)) avec transfert du groupe disélénolate. Le
complexe 2 réagit ultérieurement avec des quantités équimolaires de [Au(OClO3)L] pour conduire au complexe
trinucléaire [Au3(dsit)(PPh2Me)3]ClO4 (3). Lorsqu’on fait réagir le (NBu4)2[Zn(dsit)2] avec du [Au2Cl2(P-P)] dans un
rapport de 1 : 2, on obtient des complexes [Au2(dsit)(P-P)]n (P-P = dppe [1,2-bis(diphénylphosphine)éthane], n = 1 (4);
P-P = dppm [bis(diphénylphosphine)méthane], n = 2 (5)). On peut obtenir des dérivés anioniques, tel que le
(NBu4)[Au(dsit)2] (6), en faisant réagir le complexe de zinc avec du (NBu4)[AuBr4] dans un rapport de 1 : 1; pour la
préparation d’autres complexes de l’or, il est nécessaire d’utiliser un complexe d’étain comme ligand de transfert.
Ainsi, le complexe [Sn(dsit)Me2] (7), obtenu à partir du complexe de zinc et du [SnCl2Me2], réagit avec le
PPN[Au(C6F5)Cl] (PPN = bis(triphénylphosphine)iminium) ou le [AuBr2(S2CNR2)] pour conduire respectivement au
[Au(dsit)(S2CNR2)] (R = Me (8); R = Bz (9)) et au (PPN)2[Au2(dsit)(C6F5)2] (10). L’oxydation électrochimique du
composé 6 conduit au (NBu4)0,4[Au(dsit)2] (11) alors que sa réaction avec le (TTF)3(BF4)2 (TTF = tétrathiafulvalène)
mène au (TTF)[Au(dsit)2] (12). Les conductivités électriques de ces complexes, à la température ambiante, sous la
forme de pastilles, sont 3 × 10–8 (11) et 5 × 10–3 (12) S cm–1.
Mots clés : disélénolate, dsit, complexes d’or, complexes d’étain.
[Traduit par la Rédaction] Cerrada and Laguna 1037
EDT-TTF[Ni(dmit)2], which is superconducting at ambient
pressure (4). The dmit ligand acts in all these complexes as a
Metal complexes containing 4,5-dithiolate-1,3-dithiole-2-
bidentate chelate but the coordination chemistry of this
thione (C3S52–, dmit) have been investigated because of the
ligand is very rich, at least in gold chemistry, where coordi-
high conductivity reported in certain of them (1, 2). Since
nation as µ2 (11–13) and µ3 (12) bridging modes in di-, tri-,
the discovery in 1986 of the first formally inorganic molecu-
and tetra-nuclear complexes have been described.
lar superconductor (3) (TTF)[Ni(dmit)2]2 (TTF = tetra-
Substituting selenium atoms for sulphur atoms in dmit has
led to a number of new ligands such as dsit (C3S3Se2), dsise
(C3S4Se), dmise (C3S2Se3), and dsis (C3Se5) (14–17)
(Fig. 1). They have been investigated because they are ex-
thiafulvalene), a great number of (cation)x[M(dmit)2] (M =
Ni, Pd, and Pt; cation = TTF or NMe4 and 0 ˜ x ˜ 2) have
been synthesized (4–10), including the recently reported α-
pected to enable more effective molecular interaction
through the selenium–selenium contacts due to the more dif-
fuse and spatially extended p and d orbitals of the selenium
atom as compared with sulphur. However, to date only a few
Received October 10, 1997.
E. Cerrada and M. Laguna.1 Departamento de Química
Inorgánica, Instituto de Ciencia de Materiales de Aragón,
Universidad de Zaragoza-C.S.I.C., 50009 Zaragoza, Spain.
complexes of these ligands have been reported and those
1
with
metallic
behaviour
are
scarce,
namely,
Author to whom correspondence may be addressed.
Telephone: 34-976-761181. Fax: 34-976-761187. E-mail:
mlaguna@posta.unizar.es
[NHMe3][Ni(dmise)2]2 (18), [NMe4][Ni(dmise)2]2 (19), and
[NMe4][Pd(dsise)2]2 (20).
Can. J. Chem. 76: 1033–1037 (1998)
© 1998 NRC Canada

1034
Can. J. Chem. Vol. 76, 1998
Fig. 1.
[Au2(dsit)L2] (L = PPh3 (1), PPh2Me (2)), [Au2(dsit)(P-
P)]n (P-P = dppe, n = 1 (4); P-P = dppm, n = 2 (5)),
(NBu4)[Au(dsit)2] (6), [Sn(C3S3Se2)Me2] (7)
To an acetone (20 mL) solution of (NBu4)2[Zn(dsit)2]
(56 mg, 0.05 mmol) under a dinitrogen atmosphere was
added [AuCl(PPh3)] (98 mg, 0.2 mmol), [AuCl(Ph2Me)]
(86 mg, 0.2 mmol), [Au2(µ-dppe)Cl2] (86 mg, 0.1 mmol), or
[Au2(µ-dppm)Cl2] (85 mg, 0.1 mmol). Orange solids precip-
itated immediately in the case of 4 and 5; these were filtered
off, washed with acetone, and dried under vacuum. In the
other cases orange solutions were obtained. After stirring for
1 h, the solutions were concentrated to 1 mL. Addition of di-
ethyl ether (15 mL) gave a pale solid, which was filtered off.
The resulting solution was concentrated to 5 mL. Addition
of n-hexane (10 mL) led to precipitation of 1 and 2 as yel-
low solids The solids were filtered off, washed with water,
and recrystallized with diethyl ether – hexane. Formation of
This paper reports a systematic study of the coordination
7
was accomplished similarly, but starting from
properties of dsit as a ligand in gold(I) and gold(III) chemistry,
giving rise to novel bridging coordination modes, through
the useful transfer of dsit from zinc and tin complexes, such
as [NBu4]2[Zn(dsit)2] and [Sn(dsit)Me2]. Gold complexes
with the dsit acting as µ2 (e.g., [Au2(dsit)(PPh2Me)2]) or µ3
(e.g., [Au3(dsit)(PPh2Me)3]ClO4) bridging ligand are re-
ported among others, with the dsit acting in a chelate form
(e.g., [Au(dsit)(S2CNMe2)]). Complex [Bu4N][Au(dsit)2] un-
dergoes oxidation to give fractional oxidation state com-
plexes [NBu4]0.4[Au(dsit)2] or reacts with (TTF)3(BF4)2
affording [TTF][Au(dsit)2] (TTF = tetrathiafulvalene). Both
gold complexes show low electrical conductivity in com-
pacted pellets, 3 × 10–8 and 5 × 10–3 S cm–1,, respectively.
(NEt4)2[Zn(dsit)2] (45 mg, 0.05 mmol) and SnCl2Me2
(22 mg, 0.1 mmol).
Complex 6 was formed similarly but starting from
NBu4[AuBr4] (38 mg, 0.05 mmol) and (NBu4)2[Zn(dsit)2]
(56 mg, 0.05 mmol) and using diethyl ether to precipitate a
garnet solid, which was filtered off, washed with water, and
recrystallized from dichloromethane – diethyl ether.
[Au3(dsit)(PPh2Me)3]ClO4 (3)
To
a
dichloromethane (20 mL) solution of
[AuCl(PPh2Me)] (43 mg, 0.1 mmol) was added AgClO4
(21 mg, 0.1 mmol). After 1 h of stirring the suspension was
filtered through a 1 cm layer of Celite. [Au2(dsit)(PPh2Me)2]
(110 mg, 0.1 mmol) was added to the resulting solution. Af-
ter being stirred for 2 h, the solution was concentrated to
2 mL. Addition of n-hexane led to precipitation of an orange
solid. ΛM in acetone (5 × 10–4 M) 107 Ω–1 cm2 mol–1.
Q2[Zn(dsit)2] (Q = NBu4, NEt4) (21), [AuCl(PPh3)] (22),
[AuCl(PPh2Me)] (22), [Au2(µ-dppe)Cl2] (dppe = 1,2-bis(di-
phenylphosphine)ethane) (23), [Au2(µ-dppm)Cl2] (dppm =
bis(diphenylphosphine)methane) (23), PPN[Au(C6F5)Cl]
[Au(dsit)(S2CNR2)] (R = Me (8), CH2Ph (Bz) (9)),
(PPN)2[Au2(dsit)(C6F5)2] (10)
To an acetone (20 mL) solution of [Sn(dsit)Me2] (39 mg,
0.1 mmol) under a dinitrogen atmosphere was added
[AuBr2(S2CNMe2)] (47 mg, 0.1 mmol), [AuBr2(S2CNBz2)]
(63 mg, 0.1 mmol), or PPN[Au(C6F5)Cl] (180 mg,
0.2 mmol). Dark brown (8) and green (9) solids inmediately
appeared and were filtered off and dried under vacuum. In
the other case, the solution was concentrated to 1 mL. Addi-
tion of n-hexane (15 mL) gave a brown solid (10), which
was filtered off.
(PPN
= bis(triphenylphosphine)iminium) (24), [AuBr2-
(S2CNR2)] (25), and (TTF)3(BF4)2 (26) were prepared by lit-
erature procedures. [Au(OClO3)(PPh2Me)] was synthesized
from [AuCl(PPh2Me)] with AgClO4 in dichloromethane. All
other reagents were commercially available.
IR spectra were recorded on a Perkin–Elmer 559 or 883
spectrophotometer, over the range 4000–250 cm–1, using
Nujol mulls between polyethylene sheets, and Raman spec-
tra were recorded using a Dilor XY spectrometer with a
multichannel diode array detector and λ (Ar+) = 514.5 nm.
NMR spectra were recorded on a Varian Unity 300 spec-
trometer in CDCl3 solutions (1H (300 MHz), 31P{1H}
(121.4 MHz), and 19F (282.2 MHz)) using tetramethylsilane,
H3PO4 (85%, external), and CFCl3 as references. Mass spec-
tra were recorded with the VG Autospec LSIMS technique
using 3-nitrobenzylalcohol as matrix and a cesium gun. The
C, H, N, and S analyses were performed with a Perkin–
Elmer 2400 microanalyser; Au was determined by ashing
the samples with an aqueous solution of hydrazine. Conduc-
tivities were measured in acetone with a Philips PW 9509
apparatus. Electrical conductivities were measured in com-
pacted pressed pellets at room temperature.
(NBu4)0.4[Au(dsit)2] (11)
An
acetonitrile
solution
(10
mL)
containing
(NBu4)[Au(dsit)2] (24 mg, 24 mmol) and NBu4ClO4 (27 mg,
80 mmol) was subjected to controlled-current (1.2 µA) elec-
trolysis for 15 days in an H-type glass cell consisting of
platinum wires (27). Black microcrystals (7 mg) of complex
11 produced on the anode were collected and washed with
acetonitrile.
(TTF)[Au(dsit)2] (12)
To an acetonitrile (20 mL) solution of NBu4[Au(dsit)2]
(101 mg, 0.1 mmol) was added (TTF)3(BF4)2 (102 mg,
© 1998 NRC Canada

Cerrada and Laguna
1035
Scheme 1.
0.13 mmol). A dark garnet solid precipitated immediately
and was filtered off and dried under vacuum.
m/z (%): 1669 (9), 1, and 1483 (8), 2. The trinuclear gold(I)
complex [Au3(dsit)(PPh2Me)3](ClO4) (3) can be obtained by
reaction of complex 2 with a fresh solution of [Au-
(OClO3)(PPh2Me)]. The corresponding PPh3 derivative is
not obtained in a pure form. Complex 3 shows conductivity
in acetone solution (5 × 10–4 M) corresponding to a 1:1 elec-
trolyte, in agreement with its formulation (32). The mass
spectrum shows the parent ion peak with the lack of the
ClO4 anion at m/z 1483 (17%). The 1H NMR spectrum
shows a CH3 doublet at 2.4 ppm (2JP–H = 7.8 Hz) and the
31P{1H} NMR spectrum consists of a broad singlet at room
temperature, which is resolved into two singlets with a 2:1
intensity ratio at –80°C, as did the dmit complex
[Au3(dmit)(PPh2Me)3](ClO4) (31). In accordance with all
these data we believe that complexes 1–3 have similar struc-
tures as those reported for the dmit derivatives with the dsit
acting as µ2 and µ3 bridging ligands as represented in
Scheme 1.
The syntheses of dmit and dsit complexes reported to date
have been carried out mainly from the COPh protected de-
rivatives, C3S5(COPh)2 and C3S3Se2(COPh)2, respectively.
The reaction of these stable derivatives with ethanol solu-
tions of EtONa yields fresh solutions of C3S5Na2 or
C3S3Se2Na2, which further react with the corresponding
halo–metal complexes (17, 28, 29). This method does not
yield good results with the dsit and gold(I) complexes
[AuClL] (L
= PPh3, PPh2Me). The preparation of
[Au2(dsit)L2] (L = PPh3, 1; PPh2Me, 2) can be achieved
through the use of the zinc derivative (NBu4)2[Zn(dsit)2]
with the corresponding [AuClL] complexes in a 1:4 ratio in
acetone solutions (reaction (i), Scheme 1) in a similar way to
those reported for dmit derivatives (30). The reaction works
in very mild conditions such as 1 h reaction time at room
temperature. The lack of solubility of the by-product
(NBu4)2[ZnCl4] in diethyl ether permits the separation of
complexes 1 and 2 in good yields (Table 1).
The spectroscopic properties of these complexes are in
agreement with their formulation, showing one singlet in the
31P{1H} NMR spectrum, displaced slightly low field with
respect to the [Au2(dmit)L2] derivatives (31). The mass
spectra (LSIMS +) are very informative, showing the parent
peak M+ at m/z (%) 1210 (15), 1, and 1086 (12), 2, with the
expected isotopic distributions, which in this case are illus-
trative because of the presence of six isotopes of selenium. It
is noteworthy that, as happened in the dithiolate mass spec-
tra (30, 31), there are signals assignable to [M + Au L]+ at
The zinc derivative (NBu4)2[Zn(dsit)2] reacts with
[Au2Cl2(P-P)2] (P-P = dppm, dppe) in a 1:2 ratio with the
transfer of a diselenolate group. New complexes [Au2
(dsit)(P-P)]n (P-P = dppe, n = 1, 4 ; P-P = dppm, n = 2, 5)
appear as insoluble yellow solids in the reaction solvent, ac-
etone. The 31P{1H} NMR spectra show a single resonance at
δ 33.7 ppm for 4 and an AA′XX′ system for 5: δA
36.7 ppm, δX = 27.1 ppm, JAA = 112 Hz, JAX = JA′X
=
=
2
2
2
46 Hz. All these values are very close to those reported for
the dmit derivatives (12, 13) and are displaced slightly low
field with respect to them with the exception of δA. It is
noteworthy that although the differences are small (one CH2
group) between the diphosphines used, dppm and dppe, the
spectroscopic properties of complexes 4 and 5 are very dif-
ferent. Similar 31P{1H} NMR spectral patterns have been
© 1998 NRC Canada

1036
Can. J. Chem. Vol. 76, 1998
Table 1. Analytical and spectroscopic data for complexes 1–12.
Anal. found (calcd.)(%)
Complex
Yield (%)
70
C
H
S
N
31P {1H}
37.1(s)
1H NMR CH3 or CH2
—
1[Au2(dsit)(PPh3)2]
39.5
(38.8)
33.3
(33.1)
31.5
(31.9)
32.2
(32.4)
32.0
(31.5)
15.5
(15.0)
12.3
(11.9)
28.5
(28.1)
50.5
(49.9)
17.2
(17.0)
13.9
(14.7)
2.6
(2.5)
2.3
(2.3)
2.1
(2.5)
2.0
(2.2)
2.1
(2.1)
1.3
(1.5)
0.9
(1.0)
1.6
(1.7)
3.4
(2.9)
1.8
(1.7)
0.3
(0.4)
8.15
(8.0)
8.8
(8.9)
6.6
(6.1)
8.4
(8.9)
8.7
(9.0)
24.3
(24.1)
26.5
(26.4)
20.6
(21.1)
4.8
(4.6)
21.4
(22.0)
33.2
(32.7)
—
2[Au2(dsit)(PPh2Me)2]
3[Au3(dsit)(PPh2Me)3]ClO4
4[Au2(dsit)(dppe)]
68
65
75
85
90
90
72
50
—
65
—
—
—
—
20.9(s)
1.92(2J(PH) 4 Hz)
2.46(2J(PH) 7.8 Hz)
2.62(s)
20.2(s,br)a
33.7(s)
5 [Au4(dsit)2(dppm)2]
7 [Sn(dsit)Me2]
36.7(m)
27.1(m)
—
4.45(m), 4.25(m)
1.27(2J(SnH) 60 Hz)
b
8 [Au(dsit)(S2CNMe2)]
9 [Au(dsit)(S2CNBz2)]
10 (PPN)2[Au2(dsit)(C6F5)2]
11 (NBu4)0.4[Au(dsit)2]c
12 (TTF)[Au(dsit)2]d
a
2.6
(2.3)
1.8
(1.9)
1.5
(1.3)
0.6
—
—
—
—
—
b
—
—
—
(0.7)
—
In (CD3)2CO at room temp. At –80°C: 20.7(s) and 18.5(s).
Insoluble.
Au: Anal. found 23.1, calcd. 22.5.
Au: Anal. found 20.6, calcd. 20.1.
b
c
d
observed in the dmit derivatives and in fact their structures
[Au2(dmit)(dppe)] (13) and [Au2(dmit)(dppm)]2 (12) are
very different. The spectroscopic properties indicate a simi-
lar structure for the dmit and dsit derivatives, dinuclear for 4
and tetranuclear for 5, although other polynuclear structures
are not ruled out (Scheme 1). The mass spectra of these
complexes are not helpful because only Au(dsit) and Au(P-
P) fragments appear.
The use of the zinc derivative as the diselenolate transfer-
ring group can be extended to the preparation of gold(III)
complexes, but in this case only the reaction with
(NBu4)[AuBr4] works in a clean way to give the previously
described (NBu4)[Au(dsit)2] (6) (33) in a very good yield.
Because of the square planar coordination of gold(III), the
dsit ligand acts as a bidentate chelate ligand in this complex.
The preparation of anionic gold(I) complexes or gold(III)
derivatives requires other transferring metal complexes. For
this reason we tested the preparation of the dsit–tin deriva-
tive, which can be obtained from the reaction of
(NBu4)2[Zn(dsit)2] with [SnCl2Me2] (reaction (vi)). The re-
or to the anionic gold(I) derivative (PPN)[Au(C6F5)Cl] (PPN
= Ph3PϭNϭPPh3), affording the mononuclear [Au(dsit)-
(S2CNR2)] (R = Me, 8; CH2Ph (Bz), 9) or the dinuclear
gold(I) complex (PPN)2[Au2(dsit)(C6F5)2] (10). In both
cases the reaction by-product [SnCl2Me2] can be separated
from the reaction mixture because of its solubility in acetone
or hexane, respectively. Due to the insolubility of complexes
8 and 9, data from measurements in solution were not avail-
able. Complex 10 shows three signals in the 19F NMR spec-
trum: –115.4 (m, Fo), –163.3 (t, Fp), –164.6 (m, Fm) in
accordance with two equivalent C6F5 groups. Complex 10
shows in the mass spectrum (LSIMS–) a signal correspond-
ing to the anion at m/z 821 (3%). The coordination of dsit
ligand in compounds 6, 8, and 9 should be as bidentate che-
late because of the preferred square planar arrangement of
the gold(III) center, whereas the prefered linear array at
gold(I) centers induces a coordination of dsit as µ2- or µ3-
bridge as proposed for compounds 1–5 and 10.Unfortu-
nately, all attempts to obtain crystals of good quality for X-
ray studies of the new complexes were unsuccessful and do
not permit us to confirm the proposed coordination proper-
ties of the dsit ligand in gold chemistry.
sulting tin [Sn(dsit)Me2]
7 and the zinc by-product
(NBu4)2[ZnCl4] complexes can be easily separated because
1
of their different solubilities in diethyl ether. The H NMR
The preparation of fractional charge complexes has usu-
ally been achieved by starting from anionic complexes. In
our case neither gold(I) anionic 10, nor neutral derivatives, 1
and 2, give non-integral derivatives. On the contrary, the
electrochemical oxidation of an acetonitrile solution of
(NBu4)[Au(dsit)2] 6 in the presence of NBu4ClO4 affords
black microcrystals of complex: (NBu4)0.4[Au(dsit)2] 11,
spectrum of 7 shows a singlet for methyl groups bonded to
tin flanked by a broad pair of satellite peaks (2JSn–H = 60.0 Hz).
Although there are two active tin isotopes, 117Sn and 119Sn,
the different coupling constants are not resolved in this case.
Complex 7 is a suitable reagent for transferring the dsit to
different dithiocarbamate gold(III) complexes [AuBr2(S2CNR2)]
© 1998 NRC Canada

Cerrada and Laguna
1037
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1050 and 1025 cm–1 corresponding to the ν(CϭS) band and
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CϭC of the TTF molecule in accordance with a formulation
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