Palladium(II) and Platinum(II) Saccharinate Complexes
line product, whereas pale yellow crystals of 3 appeared after two vs, 1108 s, 1046 m, 948 s, 772 m, 747 m, 698 w, 674 s, 600 s, 539
–1
weeks.
m, 519 m cm .
[
Pt(aepy) ](sac)
2
O
2
·2H
2
O
(4): Yield 60.6 %. M.p. 142–147 °C.
Complexes 2 and 4 were prepared as follows: A solution of ampy or
C
28
H
32
N
6
8
S
2
Pt (839.81): calcd. C 40.0, H 3.5, N 10.0; found C 40.2,
H 3.7, N 10.1 %. IR (KBr): ν˜ = 3551 sb, 3444 sb, 3184 sb, 3101 sb,
958 vw, 1623 vs, 1581 vs, 1486 m, 1458 m, 1343 m, 1326 m, 1255
vs, 1151 vs, 1119 vs, 1051 m, 1011 w, 950 vs, 779 m, 751 m, 706 w,
aepy (0.8 mmol) in MeOH (15 mL) was mixed with a solution of
K
2
[PtCl
for 48 hours at room temperature. The yellow solid was separated and
dissolved in 200 mL water. The solid AgNO (0.14 g, 0.8 mmol) was
4
] (0.17 g, 0.4 mmol), dissolved in water (5 mL), and stirred
2
3
–1
6
75 m, 636 w, 605 s, 543 m, 468 w cm .
added to this solution and heated under reflux for six hours. The pre-
cipitate of AgCl was removed by filtering through Celite paste to ob-
tain a clear solution. Afterwards, the filtrate was concentrated to 10 mL X-ray Crystallography
followed by the addition of Na(sac)·2H O (0.8 mmol, 0.20 g) and was
2
The data collection was performed with a Stoe-IPDS-2 diffractometer
equipped with a graphite monochromated Mo-K radiation (α =
.71073 Å). The structure was solved by direct methods using
SHELXS-97 [11] and refined by a full-matrix least-squares procedure
using the program SHELXL-97 [11]. All non-hydrogen atoms were
easily found from the difference Fourier map and refined anisotropi-
cally. All carbon and amine hydrogen atoms were included using a
riding model, whereas the water hydrogen atoms were refined freely.
Details of crystal data, data collection, structure solution and refine-
ment are given in Table 1.
heated under reflux for 4 hours. The clear solution was kept at room
temperature and prismatic crystals of 2 and 4 were obtained after two
weeks.
α
0
[
Pd(ampy)
2
](sac)
Pd (687.08): calcd. C 45.5, H 3.5, N 12.2; found C 45.6,
H 3.9, N 12.2 %. IR (KBr): ν˜ = 3105 sb, 3048 s, 1638 vs, 1569 vs,
495 m, 1434 m, 1332 m, 1262 vs, 1197 m, 1140 vs, 1115 vs, 1050
2
(1): Yield 82.0 %. M.p. 248–255 °C.
26 24 6 6 2
C H N O S
1
–1
m, 944 vs, 886 m, 756 s, 678 m, 608 s, 539 m, 433 w cm .
[
Pt(ampy)
2
](sac)
Pt (775.72): calcd. C 40.2, H 3.1, N 10.8; found C 40.0,
H 2.9, N 10.6 %. IR (KBr): ν˜ = 3138 sb, 3018 sb, 2921 w, 1636 vs,
573 s, 1496 m, 1453 m, 1384 m, 1328 m, 1264 vs, 1207 w, 1144 vs,
114 vs, 1050 w, 1017 w, 948 vs, 883 m, 757 vs, 679 s, 630 w, 603
2
(2): Yield 60.4 %. M.p. 291–299 °C.
CCDC-737649 (2), CCDC-737650 (3), and CCDC-737651(4) contain
the supplementary crystallographic data for this paper. These data can
be obtained free of charge from The Cambridge Crystallographic Data
Centre via www.ccdc.cam.ac.uk/data_request/cif.
26 24 6 6 2
C H N O S
1
1
–
1
s, 542 m, 528 m, 440 m cm .
Results and Discussion
Syntheses and Spectral Properties
[
Pd(aepy)
comp.). C28
found C 44.5, H 4.2, N 10.9 %. IR (KBr): ν˜ = 3461 sb, 3281 sb, 3036
2
](sac)
2
·2H
2
O (3): Yield 48.4 %. M.p. 230–235 °C (de-
H N O S Pd (751.14): calcd. C 44.8, H 4.3, N 11.28;
32 6 8 2
Complexes 2–4 were synthesized in moderate yields,
w, 2921 w, 1629 vs, 1582 s, 1487 w, 1450 m, 1328 m, 1254 vs, 1144 whereas complex 1 was obtained in a high yield (over 80 %).
Table 1. Details of crystal data collection and refinement for 2–4.
Compound
2
3
4
Empirical formula
C
26
H
24
N
6
O
6
S
2
Pt
C
28
H
32
N
6
O
8
S
2
Pd
C
28 32 6 8 2
H N O S Pt
–
1
FW /g·mol
T /K
775.72
150
751.14
150
839.81
296
Radiation, λ /Å
Crystal system
Space group
a /Å
0.71073
0.71073
triclinic
P1
0.71073
triclinic
monoclinic
¯
¯
P1
P2
1
/c
7.2267(4)
24.0712(9)
8.5557(5)
7.9287(4)
8.0454(4)
12.5150(7)
737.19(7)
1
7.6861(10)
8.9917(12)
b /Å
c /Å
11.5101(14)
765.87(17)
1
3
V /Å
1302.61(12)
2
Z
–
3
D
c
/g·cm
1.978
5.603
760
1.692
1.821
–
1
μ /mm
0.833
4.777
F(000)
384
416
Crystal size /mm
θ range /°
Index range
0.50 × 0.41 × 0.20
1.69/26.50
0.48 × 0.30 × 0.05
1.70/28.08
–9 ≤ h ≤ 9,
–10 ≤ k ≤ 10,
–15 ≤ l ≤ 15
7884
0.54 × 0.40 × 0.27
2.35/26.49
–8 ≤ h ≤ 9,
–11 ≤ k ≤ 11,
–14 ≤ l ≤ 14
11124
–8 ≤ h ≤ 9,
–
30 ≤ k ≤ 30,
10 ≤ l ≤ 10
–
Reflections collected
9842
Independent reflections (Rint
)
2692 (0.0527)
Numerical
2692/0/187
1.047
3044 (0.0235)
Numerical
3044/3/211
1.083
3181 (0.0225)
Numerical
3181/3/211
1.114
Absorption correction
Data / restraints/ parameters
2
S on F
Final R indices [I > 2σ(I)]
wR indices (all data)
0.0252
0.0306
0.0124
0.0581
0.0779
0.0317
–
3
Largest diff. peak and hole /e·Å
1.387 and –1.657
0.553 and –0.737
0.472 and –0.701
Z. Anorg. Allg. Chem. 2010, 610–615
© 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
www.zaac.wiley-vch.de
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