Biology Reference
In-Depth Information
9.5.3
General Synthetic Procedure for 8-11
°
To the stirred slurry of
1
in acetone at 60
C was added a solution of
the corresponding ligand (L
) in acetone in a 1:1 ratio. Initially,
a clear solution was formed, which upon further stirring overnight
yielded a light yellow precipitate. The solid product was washed
several times with diethylether and dried under vacuum.
4-7
9.5.3.1
Synthesis of the Rectangle 8
¢
Complex
1
(12.1 mg, 0.01 mmol) and 4,4
-bipyridine (
4
; 1.6 mg,
0.01 mmol) were reacted in acetone to obtain
8
in 96% yield. Anal.
calcd. (found) for C
H
N
O
P
Pt
: C, 45.68 (45.47); H, 5.60
104
152
8
12
8
4
3
-
2+
(5.84); N, 4.09 (3.94). ESI-MS (
m
/
z
): 1305.93 [
6
- 2NO
]
, 1187.13
[(
8
- 2NO
3
-
- 2PEt
)]
2+
, 622.07 [8 - 4NO
3
-
]
4+
. IR data (KBr pellet,
3
-1
∫
1
ν
9.29 (s,
2H, anthracene-H), 9.1 (d, 8H, pyridine-H), 8.6 (d, 8H, pyridine-H),
8.4 (s, 2H, anthracene-H), 7.88 (d, 4H, anthracene-H), 7.5 (d, 4H,
anthracene-H), 7.2 (d, 4H, anthracene-H), 1.79 (q, 48H, -CH
/cm
) for 8: 2105 (C
C).
H NMR (CDCl
, 400 MHz):
δ
max
3
), 0.9 (t,
2
72H, -CH
154.0 (16C, 4), 132.2 (8C,
anthracene), 131.5 (4C, anthracene), 127.2 (4C, anthracene), 126.2
(8C, anthracene), 125.6 (4C, anthracene), 122.7 (4C, ethynyl), 122.1
(4C, 4), 87.1 (4C, ethynyl), 14.6 (24C, PEt
).
13
C NMR (CH
NO
+ CD
OD):
δ
3
3
2
3
31
), 7.7 (24C, PEt
).
P NMR
3
3
1
(CDCl
):
δ
14.26 (s,
J
= 2888 Hz).
3
Pt-P
9.5.3.2
Synthesis of the Rectangle 9
Complex
1
(12.1 mg, 0.01 mmol) and
trans
-1,2-bis(4-pyridyl)
ethylene (
5
; 1.8 mg, 0.01 mmol) were reacted in acetone to obtain
9
in 90% yield. Anal. calcd. (found) for C
H
N
O
P
Pt
: C, 46.55
108
156
8
12
8
4
(46.32); H, 5.64 (5.73); N, 4.02 (4.00). ESI-MS (
m
/
z
): 1332.20 [
9
-
3
-
2+
3
-
2+,
3
-
3+
2NO
]
, 1213.53 [
9
- 2NO
- 2PEt
]
867.13 [
9
- 3NO
]
, 634.73
3
[
9
- 4NO
3
-
]
4+
. IR data (KBr pellet,
ν
/cm
-1
) for
9
: 2105 (C
∫
C), 1611
max
1
9.2 (s, 2H, anthracene-H), 8.9 (d,
8H, pyridine-H), 8.39 (s, 2H, anthracene-H), 8.2 (d, 8H, pyridine-H),
7.85 (d, 4H, anthracene-H), 7.5 (d, 4H, anthracene-H), 7.39 (d, 4H,
anthracene-H), 7.18 (s, 4H, C=CH), 1.8 (q, 48H, -CH
(C=C).
H NMR (CDCl
, 400 MHz):
δ
3
), 1.1 (t, 72H,
2
), 133.4
(8C, anthracene), 132.8 (4C, anthracene), 126.9 (8C, anthracene),
123.5 (4C, anthracene), 123.0 (4C, anthracene), 119.1 (4C, ethynyl),
118.2 (4C,
-CH
).
13
C NMR (CH
NO
+ CDCl
):
δ
154.2 (8C,
5
), 150.1 (8C,
5
3
3
2
3
5
), 106.1 (4C,
5
), 87.2 (4C, ethynyl), 15.9 (24C, PEt
), 9.0
3
31
1
(24C, PEt
).
P NMR (CDCl
):
δ
14.5 (s,
J
= 2960 Hz).
3
3
Pt-P
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