Gold(I) thiosulfonate complexes

Article abstract of DOI:10.1016/S0020-1693(02)01445-7

A series of seven gold(I) p-tolylthiosulfonate complexes of the general type (L)A-SS(O)₂C₆H₄-4-Me have been prepared from the reaction of silver p-tolylthiosulfonate with the corresponding precursor complexes (L)AuCl in dichloromethane. Yields in excess of 90% were obtained throughout for tertiary phosphine and isocyanide ligands L=PMe₃, PPh₃, Ph₂(2-Py)P, (4-Me₂NC₆H₄)Ph₂P, ⁱPrNC, and ^tBuNC. The complexes are surprisingly stable and undergo controlled decomposition well above 100°C. The crystal and molecular structures have been determined for three representative examples. The Me₃P and Ph₃P complexes form dimers with short aurophilic bonding [Au-Au 2.9955(3) and 3.0509(2) A?] in a crossed-swords conformation, while for the ^tBuNC complex the monomers with their linear five-atom axes appear as only loosely aggregated dimers with a parallel head-to-tail arrangement [Au-Au 3.5423(3) A?]. In all cases the p-tolylthiosulfonate ligand is S-bonded to the metal center.

Full text of DOI:10.1016/S0020-1693(02)01445-7

Inorganica Chimica Acta 347 (2003) 123ꢂ128
/
www.elsevier.com/locate/ica
Gold(I) thiosulfonate complexes
Patric Rombke, Annette Schier, Frank Wiesbrock, Hubert Schmidbaur *
¨
Anorganisch-Chemisches Institut, Technische Universitat Munchen, Lichtenbergstrasse 4, D-85747 Garching, Germany
¨ ¨
Received 28 April 2002; accepted 18 June 2002
Dedicated to Professor Raphael Uso´n
Abstract
A series of seven gold(I) p-tolylthiosulfonate complexes of the general type (L)AuÃ
/
SS(O)2C6H4Ã
/
4-Me have been prepared from
the reaction of silver p-tolylthiosulfonate with the corresponding precursor complexes (L)AuCl in dichloromethane. Yields in excess
of 90% were obtained throughout for tertiary phosphine and isocyanide ligands LꢀPMe3, PPh3, Ph2(2-Py)P, (4-Me2NC6H4)Ph2P,
/
t
i PrNC, and BuNC. The complexes are surprisingly stable and undergo controlled decomposition well above 100 8C. The crystal
and molecular structures have been determined for three representative examples. The Me3P and Ph3P complexes form dimers with
t
Au 2.9955(3) and 3.0509(2) A] in a crossed-swords conformation, while for the BuNC complex the
˚
short aurophilic bonding [AuÃ
/
monomers with their linear five-atom axes appear as only loosely aggregated dimers with a parallel head-to-tail arrangement [AuÃ
/
˚
Au 3.5423(3) A]. In all cases the p-tolylthiosulfonate ligand is S-bonded to the metal center.
# 2002 Elsevier Science B.V. All rights reserved.
Keywords: Crystal structures; Thiosulfonate complexes; Gold complexes
1. Introduction
Gold(I) complexes of the type LÃ
sotherapy) of common diseases like rheumatoid arthritis
[4], and a (phosphine)gold thioglucose compound [(Et3-
P)AuSR] is presently the most successful oral gold drug
[5]. Gold(I) sulfate (L)AuOS(O)2OAu(L) and sulfonate
complexes (L)AuOS(O)2R have also been described and
have recently gained interest as homogeneous catalysts
for addition reactions of alkynes [6]. This is particularly
true for sulfonates with strongly electronegative sub-
/
AuÃ
/
X with a
neutral and an anionic ligand (L/X) are of current
interest owing to their fascinating structural chemistry
and their potential for applications in a wide variety of
classical and contemporary technologies, and in medi-
cine [1]. Among the ligands L employed for tailoring the
properties of the compounds the large family of tertiary
phosphines and arsines are most prominent [1a,2], but
isocyanides have recently also received considerable
attention [3]. The heavier halides were the most common
counterions X in most fundamental studies, but the
current investigations have focussed almost exclusively
on sulfur-functional components.
stituents RꢀCF3, C2F5 etc. [6g].
/
By contrast, gold(I) thiosulfonate and thiosulfinate
complexes of the types (L)AuSS(O)2R and (L)AuS-
S(O)R, respectively, with L a donor ligand and R an
alkyl or aryl group, have not yet been investigated.
Because compounds with these combinations of ligands
may not only be of interest in pharmacy but also as
precursor complexes for the deposition of gold films on
substrates from solutions or pastes, in the present study
a series of thiosulfonates was synthesized and their
fundamental properties investigated. The compounds
were also expected to have an interesting supramolecu-
lar chemistry based on aurophilic interactions between
the individual molecules [1b].
The thiosulfate complex Na3[Au(S2O3)2] and thiolate
complexes of the type [RSAu]n were among the early
gold(I) complexes employed in chemotherapy (chry-
* Corresponding author. Tel.: ꢁ
3125.
E-mail address: h.schmidbaur@lrz.tum.de (H. Schmidbaur).
/49-89-3209 3130; fax: ꢁ49-89-3209
/
0020-1693/02/$ - see front matter # 2002 Elsevier Science B.V. All rights reserved.
doi:10.1016/S0020-1693(02)01445-7

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P. Rombke et al. / Inorganica Chimica Acta 347 (2003) 123ꢂ
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¨
2. Preparative results
units in the unit cell. The asymmetric unit contains
two independent molecules of very similar geometries.
These two units are aggregated to pairs via a short
A series of six gold(I) p-tolylthiosulfonate compounds
4-Me could readily be prepared by
metathesis from silver p-tolylthiosulfonate (in slight
˚
Au2 contact [2.9955(3) A] (Fig. 1). The
(L)AuÃ
/
SS(O)2C6H4Ã
/
aurophilic Au1Ã
/
thiosulfonate ligands are S-bonded to their gold atoms
with the two molecular axes PÃAuÃS close to 1808 [P1Ã
Au1ÃS11 179.83(5)8, P2ÃAu2ÃS21 176.03(5)8]. The
angles at the bridging sulfur atoms S11 and S21 are
Au1ÃS11ÃS12 99.73(7)8 and Au2ÃS21ÃS22 103.15(6)8,
excess) and the corresponding (L)AuCl complexes in
dichloromethane at ꢃ78 8C with protection against
incandescent light. Yields of the products in excess of
90% were obtained in all cases which include various
tertiary phosphines and alkylisocyanides as ligands L.
Silver chloride is the sole by-product which is easily
separated by filtration.
/
/
/
/
/
/
/
/
/
/
/
respectively. The sulfonate sulfur atoms have a quasi-
tetrahedral environment with two oxygen atoms, the p-
tolyl carbon atom and a sulfur atom bridging to the gold
atoms.
The two molecular axis PÃ
swords conformation with torsional angles P1Ã
Au2ÃP2 102.43(5)8 and S1ÃAu1ÃAu2ÃS2 ꢃ77.50(5)8.
/
AuÃ
/
S have the crossed-
/
Au1Ã
/
/
/
/
/
/
These angles reflect the sterical requirement of the
phosphine and thiosulfonate ligands. Parallel head-to-
tail or head-to-head conformations would lead to
significant sterical conflicts. The mutual approach of
the gold atoms of the components relative to the PÃ
S axes is almost perpendicular as specified by the angles
P1ÃAu1ÃAu2 94.52(4)8 and P2ÃAu2ÃAu1 93.76(3)8, or
S11ÃAu1ÃAu2 85.33(3)8 and S21ÃAu2ÃAu1 85.86(3)8.
These mutual orientations follow the data of a plethora
of model systems reported in the literature on aurophilic
interactions [1b].
/
AuÃ
/
All products were obtained as colorless solids which
are stable at room temperature and soluble in
moderately polar organic solvents, preferably di- and
trichloromethane or tetrahydrofuran, but insoluble in
hydrocarbons such as hexane, benzene or toluene.
The NMR spectra of the solutions in chloroform-d1
or dichloromethane-d2 are in full agreement with the
proposed formulae, and elemental analyses have con-
firmed the composition. The molecular ions are detected
in the mass spectra (FAB), but peaks for dinuclear
cations with higher mass are also observed, which
indicate association in the solid (matrix) state. The two
/
/
/
/
/
/
/
/
Crystals of (Ph3P)AuSS(O)2C6H4Ã
/
4-Me (2), are also
monoclinic, space group C2/c, with Zꢀ
/8 formula units
in the unit cell. The asymmetric unit contains only one
independent molecule, which is part of a centrosymme-
trical dimer associated via aurophilic bonding (Fig. 2).
isocyanide complexes show typical CÅ/N stretching
frequencies in the IR spectra (KBr) with hypsochromic
shifts relative to the free ligands which indicate direct
end-on coordination of the isocyanide function to the
metal atom. There are many reference data in the
literature for this type of gold(I)ꢂ
/
isocyanide coordina-
tion [1a].
It should be noted that most of the analytical and
spectroscopic data would also be in agreement with an
ionic formalism based on homoleptic cations [L2Au]ꢁ
and homoleptic anions [(p-TolSO2S)2Au]ꢃ. Structures
of this kind are common for the corresponding phos-
phonates and other complexes of the seemingly simple
composition ‘LAuX’ [6e,7]. Structural studies for repre-
sentative compounds were therefore indispensable.
Fig. 1. Dimeric units of compound 1 (ORTEP drawing with 50%
probability ellipsoids; H-atoms omitted for clarity). Selected bond
˚
/
lengths (A) and angles (8): Au1Ã
/
P1 2.263(1), Au1Ã
/
S11 2.340(1), Au2Ã
3. Structural studies
P2 2.268(1), Au2Ã
S12ÃO11 1.437(4), S22Ã
1.448(4), S12ÃC101 1.769(6), S22Ã
2.9955(3); P1ÃAu1ÃS11 179.83(5), P2ÃAu2Ã
/
S21 2.332(1), S11Ã
O21 1.442(4), S12Ã
C201 1.764(5), Au1Á Á ÁAu2
S21 176.03(5).
/
S12 2.033(2), S21Ã
/
S22 2.039(2),
/
/
/
O12 1.450(4), S22Ã
/
O22
Crystals of (Me3P)AuSS(O)2C6H4Ã
monoclinic, space group P21/c, with Zꢀ
/
4-Me (1), are
8 formula
/
/
/
/
/
/
/

P. Rombke et al. / Inorganica Chimica Acta 347 (2003) 123ꢂ
/128
125
¨
˚
Fig. 2. Dimeric units of compound 2 (ORTEP drawing with 50% probability ellipsoids; H-atoms omitted for clarity). Selected bond lengths (A) and
angles (8): Au1ÃP1 2.2662(7), Au1ÃS1 2.3286(7), S1ÃS2 2.043(1), S2ÃO1 1.448(2), S2ÃO2 1.441(2), S2ÃC1 1.777(3) Au1Á Á ÁAu1? 3.0509(2); P1ÃAu1Ã
S1 169.94(3).
/
/
/
/
/
/
/
/
The mutual approach of the monomers is similar to the
situation described for the Me3P analogue 1 (above).
Owing to the greater bulk of the phosphine, the Au1Ã
/
˚
Au1? contact is significantly longer [3.0509(2) A] even
though the axis P1ÃAu1ÃS1 is more strongly bent to
facilitate the metalꢂmetal contact [169.94(3)8]. The
angles P1ÃAu1ÃAu1? and S1ÃAu1ÃAu1? [102.63(2),
84.09(2)8] and the dihedral angles P1ÃAu1ÃAu1?ÃP1?
and S1ÃAu1ÃAu1?ÃS1? [ꢃ87.09(2), ꢃ71.90(2)8] also
/
/
/
/
/
/
/
/
/
/
/
/
/
/
/
reflect the bulkiness of the phosphine ligand. The
geometry of the S-bonded thiosulfonate ligand resem-
bles that in 1.
Crystals of (Me3CNC)AuSS(O)2C6H4Ã
/
4-Me (7), are
4 formula
monoclinic, space group P21/c, with Zꢀ
/
units in the unit cell. The asymmetric unit contains
only one molecule. In the crystal lattice, the complex
molecules are apparently only loosely aggregated into
Fig. 3. Dimeric units of compound 7 (ORTEP drawing with 50%
probability ellipsoids; H-atoms omitted for clarity). Selected bond
˚
dimers (Fig. 3). The Au1Ã
/
Au1? distance is as long as
˚
3.5423(3) A and thus at the borderline of the range for
lengths (A) and angles (8): Au1Ã
/
C1 1.972(4), Au1Ã
/
S1 2.288(1), S1Ã
/
S2
N1
N1ÃC1
2.045(1), S2Ã
1.135(6) Au1Á Á ÁAu1? 3.5423(3); C1Ã
178.6(3).
/
O1 1.445(3), S2Ã
/
O2 1.444(3), S2Ã
/
C111 1.771(3), C1Ã
/
which aurophilic bonding should be considered (2.85ꢂ
/
/
Au1ÃP1 176.4(1), Au1Ã
/
/
/
˚
3.50 A). The individual molecule has a quasi-linear axis
comprising no less than five atoms, with the angles at
should be longer and weaker, but also that the
organization should be parallel head-to-tail. This is
confirmed by the packing motif of compound 7 in the
crystal.
In summary therefore the three structures reported for
the new p-tolylthiosulfonates are fully consistent with
the three internal atoms all close to 1808: S1Ã
176.4(1), Au1ÃC1ÃN1 178.6(3), C1ÃN1ÃC11 176.5(4)8.
This axis is bent at the sulfur end with an angle Au1Ã
S1ÃS2 of 102.80(5)8 and tetrahedrally branched at the
carbon end C11. There are no anomalies regarding the
thiosulfonate ligand, which is again S-coordinated to the
gold atom.
/
Au1Ã
/
C1
/
/
/
/
/
/
previous variations in structure of LÃ
/
AuÃ/X molecules.
All sulfonate complexes show remarkable thermal and
chemical stability (to air and moisture) and thus
represent a new class of robust gold(I) complexes. Their
good solubility in common solvents and the broad
choice of ligands L that can be employed suggest a
variety of applications.
The reluctance of compound 7 to undergo intimate
aurophilic interaction is in agreement with structure
reports on other (isocyanate)gold(I) complexes in the
literature [3a,3b] and also with quantum-chemical
calculations [3q]. These calculations not only predicted
that AuÃ
/
Au bonding for complexes with isocyanide

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P. Rombke et al. / Inorganica Chimica Acta 347 (2003) 123ꢂ
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¨
In conclusion it should be noted that gold(I) forms
also a variety of phosphate, phosphonate, and phosphi-
nate, as well as thiophosphate, thiophosphonate and
thiophosphinate complexes with interesting structures
and hitherto unexploited specific properties. The sulfur
and phosphorus compounds show many analogies or
are complementary [7].
for o/p/m/i-Ph; 21.5, s, Me. 31P{1H}: 39.2, s. MS (FAB):
1106 (17) [(Ph3P)2Au2SSO2Tolꢁ
1]ꢁ; 721 (5)
/
[(Ph3P)2Au]ꢁ; 647 (57) [Mꢁ1]ꢁ; 646 (8) [M]ꢁ; 459
/
(100) [(Ph3P)Au]ꢁ. Anal. Calc. for C25H22AuO2S2P
(646.50): C, 46.4; H, 3.4; S, 9.9. Found: C, 46.1; H,
3.4; S, 9.1%.
4.3. [Diphenyl(2-pyridyl)phosphine]gold(I) p-
tolylthiosulfonate (3)
4. Experimental
As described for 1, the compound was prepared with
p-TolSO2SAg (120 mg, 0.41 mmol) and [Ph2(2-
Py)P]AuCl (150 mg, 0.30 mmol); yield 180 mg (93%)
The experiments were carried out in an atmosphere of
dry nitrogen. Solvents were dried and saturated with
nitrogen, and glassware was oven-dried and filled with
nitrogen. Standard equipment was used throughout.
Reaction vessels were protected against incandescent
light when silver salts were involved. The isocyanides
and silver p-tolylthiosulfonate were prepared following
literature methods [8], the phosphines were commer-
cially available.
1
m.p. 133 8C (dec.). NMR (CDCl3, 20 8C), H: 8.78 and
7.83ꢂ
2ꢄ2H, C6H4; 7.68ꢂ
31P{1H}:
38.5,
/
7.72, m, 4H, Py; 7.93 and 7.14, 2ꢄ
7.34, m, 10H, Ph; 2.35, s, 3H, Me.
s. MS (FAB): 1108 (6)
/
d, Jꢀ8.1 Hz,
/
/
/
[L2Au2SSO2Tol]ꢁ; 723 (4) [L2Au]ꢁ; 648 (46) [Mꢁ
/
1]ꢁ; 647 (5) [M]ꢁ; 460 (100) [LAu]ꢁ. Anal. Calc. for
C24H21AuNO2S2P (647.49): C, 44.5; H, 3.2; N, 2.2; S,
9.9. Found: C, 43.8; H, 3.3; N, 2.0; S, 10.5%.
4.1. (Trimethylphosphine)gold(I) p-tolylthiosulfonate
(1)
4.4. [(p-Dimethylaminophenyl)diphenylphosphine]-
gold(I) p-tolylthiosulfonate (4)
Silver p-tolylthiosulfonate (240 mg, 0.82 mmol) was
suspended in CH2Cl2 (10 ml), cooled to ꢃ
/
70 8C and a
As described for 1, the compound was prepared from
p-TolSO2SAg (170 mg, 0.58 mmol) and [(p-
Me2NC6H4)Ph2P]AuCl (300 mg, 0.56 mmol), yield 350
mg (91%), m.p. 127 8C (dec.). NMR (CDCl3, 20 8C), 1H:
solution of (trimethylphosphine)gold(I) chloride (210
mg, 0.68 mmol) in 10 ml of the same solvent slowly
added with stirring. Stirring was continued for 2 h with
exclusion of light. The silver salt slowly converted into
silver chloride. The reaction mixture was filtered, C5H12
was added to the filtrate, and the solution allowed to
7.93 and 7.13, 2ꢄ
and 6.76, 2ꢄd, Jꢀ
10H, Ph; 3.03, s, 6H, NMe2; 2.35, s, 3H, C6H4Me.
31P{1H}:
37.4, s. MS (FAB): 1192 (21)
[L2Au2SSO2Tolꢁ
1]ꢁ; 690 (34) [Mꢁ1]ꢁ; 689 (24)
/
d, Jꢀ
/
7.8 Hz, 2ꢄ
/
2H, C6H4S; 7.77
/
/
6.9 Hz, 2ꢄ/2H, C6H4N; 7.43, m,
warm to ꢃ30 8C and kept at this temperature over
/
night. The colorless precipitate was recrystallized from
CH2Cl2/C5H12, yield 295 mg (94%), m.p. 107 8C (dec.).
/
/
[M]ꢁ; 502 (100) [L2Au]ꢁ. Anal. Calc. for C27H27Au-
NO2PS2 (689.57): C, 47.0; H, 3.9; N, 2.0; S, 9.3. Found:
C, 45.8; H, 3.8; N, 1.9; S, 9.2%.
NMR (CD2Cl2, 20 8C), 1H: 7.91 and 7.23, 2ꢄ
/
d, Jꢀ/8.1
Hz, 2ꢄ
/
2H, o/m-CH; 2.39, s, 3H, MeC; 1.55, d, Jꢀ
/
1.2
Hz, 9H, MeP. 13C{1H}: 148.2, 142.9, 129.3, and 125.7,
all s, i/o/m/p-CH; 21.2, s, MeC; 15.5, d, Jꢀ
MeP. 31P{1H}: ꢃ
5.5, s. MS(FAB) m/z: 733 (64%)
1]ꢁ; 460 (59)
/
56.5 Hz,
4.5. (Isopropylisocyanide)gold(I) p-tolylthiosulfonate
(6)
/
[(Me3P)2AuSSO2Tol]ꢁ; 461 (7.3) [Mꢁ
/
[M]ꢁ; 349 (41) [(Me3P)2Au]ꢁ, 273 (100) [(Me3P)Au]ꢁ.
Anal. Calc. for C10H16AuO2PS2 (460.29): C, 26.1; H,
3.5; S, 13.9. Found: C, 26.6; H, 3.5; S, 13.7%.
As described for 1, from p-TolSO2SAg (150 mg, 0.52
mmol) and (iPrNC)AuCl (150 mg, 0.50 mmol), yield 210
mg (93%), m.p. 132 8C (dec.). NMR (CDCl3, 20 8C), 1H:
7.91 and 7.26, 2ꢄ
/
d, Jꢀ
/
8.1 Hz, 2ꢄ2H, C6H4; 4.09,
/
4.2. (Triphenylphosphine)gold(I) p-tolylthiosulfonate
(2)
sept, Jꢀ6.3 Hz, 1H, CH; 2.41, s, 3H, MeC; 1.53, d, 6H,
/
Me2C. 13C{1H}: 147.6, 142.7, 129.3, and 125.8, all s, i/o/
m/p-CH; 49.5, s, CHMe2; 22.2, s, Me2; 21.5, s, Me; CN
not detected. IR (KBr): 2246 cmꢃ1. Anal. Calc. for
C11H14AuNO2S2 (453.34): C, 29.1; H, 3.1; N, 3.1; S,
14.1. Found: C, 28.9; H, 3.2; N, 3.1; S, 13.8%.
Following the procedure described for 1, the com-
pound was prepared with p-TolSO2SAg (295.1 mg, 0.81
mmol) and (Ph3P)AuCl (400 mg, 0.81 mmol), yield 490
mg (94%), m.p. 154 8C (dec.). NMR (CHCl3, 20 8C), 1H:
7.91 and 7.11, 2ꢄ
/
d, Jꢀ
/
8.0 Hz, 2ꢄ
/
2H, C6H4; 7.60ꢂ
/
4.6. (tButylisocyanide)gold(I) p-tolylthiosulfonate (7)
7.38, m, 15H, Ph; 2.35, s, 3H, Me. 13C{1H}: 148.9, 142.3,
128.5, and 125.8, all s, i/o/m/p-C6H4; 134.2, 132.0, 129.3,
As described for 1, from p-TolSO2SAg (112 mg, 0.38
mmol) and (tBuNC)AuCl (145 mg, 0.34 mmol), yield
and 128.8, d/s/d/d with Jꢀ
/
14.6, ꢂ/, 12.3, and 59.9 Hz,

P. Rombke et al. / Inorganica Chimica Acta 347 (2003) 123ꢂ
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127
¨
Table 1
Crystal data, data collection, and structure refinement for compounds
1, 2 and 7
crystal data, data collection and structure refinement are
summarized in Table 1. Important interatomic distances
and angles are given in the corresponding Figure
Captions.
1
2
7
Empirical formula
C
O2PS2
10H16Au-
C25H22Au-
O2PS2
646.48
C12H16Au-
NO2S2
467.34
5. Supplementary material
M
460.28
148
Temperature (K)
Crystal system
Space group
143
monoclinic
C2/c
143
monoclinic
P21/c
monoclinic
P21/c
Crystallographic data for the structural analyses with
thermal parameters and complete tables of interatomic
distances and angles have been deposited with the
Cambridge Crystallographic Data Centre CCDC Nos.
˚
a (A)
10.9430(2)
14.4000(3)
18.8090(4)
102.748(1)
2890.9(1)
8
28.3641(2)
10.1613(1)
19.5960(2)
124.293(1)
4666.1(1)
8
11.2666(2)
7.9019(1)
16.4825(2)
91.336(1)
1466.9(1)
4
˚
b (A)
˚
c (A)
187777ꢂ
obtained free of charge from The Director, CCDC, 12
Union Road, Cambridge, CB2 1EZ, UK (fax: ꢁ44-
/
18779. Copies of this information may be
b (8)
3
U (A )
˚
Z
/
rcalc (g cmꢃ3
m(Mo Ka) (cmꢃ1
F(000)
)
2.115
105.56
1.841
65.73
2.116
103.06
1223-336-033; e-mail: deposit@ccdc.cam.ac.uk or www:
http://www.ccdc.cam.ac.uk).
)
1744
DELABS
2512
DELABS
888
DELABS
Absorption
correction
Measured reflections 37840
62023
4973
36611
3249
Acknowledgements
Unique reflections
6426
[Rint
0.0767/0.1438 0.360/0.774
ꢀ
/
0.055] [Rint
ꢀ
/
0.039]
[Rint
ꢀ0.058]
/
The work was supported by Fonds der Chemischen
Industrie, Deutsche Forschungsgemeinschaft, Volkswa-
genstiftung, Degussa AG and Heraeus GmbH.
Tmin/max
0.330/0.758
163
Refined parameters
289
280
R1 [I ]
/
2s(I)]
0.0314
0.0808
0.0206
0.0518
0.0260
0.0662
wR2
Weighting scheme a
(Shift/error)max
aꢀ
/
0.0403
5.15
aꢀ
/
0.0000
8.82
aꢀ
/
0.0301
1.15
bꢀ
/
bꢀ
/
bꢀ
/
B/
0.001
B/
0.001
B/0.001
References
sfin(max/min)
ꢃ3
2.015/ꢃ
/
1.142 1.05/ꢃ0.592
/
1.631/ꢃ1.288
/
˚
(e A
)
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a
wR2ꢀ
/
{[a w(Fo2ꢃ
2Fc2)/3.
/
Fc2)2]/a [w(Fo2)2]}1/2
;
wꢀ
/
1/[s2(Fo2)ꢁ
/
(ap)2ꢁ
/
bp]; pꢀ
/
(Fo2ꢁ
/
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150 mg (93%), m.p. 115 8C (dec.). NMR (CDCl3, 20 8C),
1H: 7.76 and 7.36, 2ꢄ
/
d, Jꢀ
/
8.2 Hz, 2ꢄ2H, C6H4; 2.41,
/
s, 3H, Me; 1.57, s, 9H, Me3. 13C{1H}: 141.6, 134.2,
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.
MS (FAB): 748 (43) [L2Au2S2O2Tol]ꢁ; 692 (16)
[L2Au2S2O2TolÃ
C4H8]ꢁ; 468 (81) [Mꢁ1]ꢁ; 467 (9)
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˚
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