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9.5.3.12 Synthesis of the Prism 23
A solution of the ligand
(5.4 mg, 0.01 mmol) in acetone was added
to a suspension of clip type of metal acceptor
22
(18.1 mg, 0.015
mmol) in acetone. After heating for 5 min at 50 ºC a fluorescent
yellow solution formed, which after stirring for more than 12 h gave
a yellow precipitate. The precipitate after washing with acetone
gave
1
23
(23 mg) in 93% yield. Anal. calcd. for C
H
N
O
P
Pt
:
204
252
14
18
12
6
1
C, 51.80; H, 5.37; N, 4.15. Found: C, 51.42; H, 5.51; N, 4.33.
H NMR
(CDCl
), 8.4 (s,
3H, anthra-H), 7.8 (m, 18H, Ph-H and anthra-H), 7.5 (m, 18H, Py-H
, 400 MHz):
δ
9.2 (s, 3H, anthra-H), 9.2 (d, 12H, Py-H
3
α
β
and anthra-H), 7.3 (m, 6H, anthra-H), 7.1 (d, 12H, Ph-H), 1.9 (q, 72H,
PEt
31
1
), 1.2 (t, 108H, PEt
).
P{
H} NMR (CDCl
, 120 MHz):
δ
14.34
3
3
3
1
3
-
3+
(s,
J
= 2880 Hz). MS (ESI)
m
/
z
: 1396.27 [M - 3PEt
- 3NO
]
,
P-Pt
3
1122.27 [M - 4NO
3
-
]
4+
, 1003.33 [M - 4PEt
- 4NO
3
-
]
4+
. Melting
3
point: (>180
°
C, dec.).
Acknowledgments
Authors sincerely acknowledge Dr. Sushobhan Ghosh and Mr. Arun
K. Bar for their contributions to this work. Authors also thank the
Department of Science and Technology, India, for the financial
support.
References
1
.
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, pp. 3727-3729.
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Kinetically
stabilized
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,
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