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revealed the
formation of a planar triplatinum structure with a central nitrogen
atom. From the molecular structure it was found out that the Pt-N-
Pt angles are in the expected range 117-121
The crystal structure of the iodide analogue of
14
. The geometry around
the Pt metal was found to be distorted square planar with the I-Pt-P
angle calculated to be in the range 89.3-92.1
°
°
, and the C-Pt-P angles
between 85.7 and 91.1
°
.
9.3.2.2
Syntheses and Characterization of the
Supramolecular Prisms 17 and 18
The cationic prisms
17
and
18
were prepared by 2:3 self-assembly
of the tridentate acceptor
14
and the ditopic donors
15
and
16
. On
treating
4,4
¢
,4
¢¢
-tris[ethynyl-
trans
-Pt(PEt
)
(NO
)]triphenylamine
3
2
3
acceptor with 1.5 equivalents of the donor
in a mixture of
methanol and dichloromethane for 30 min, the self-assembly of
the prism
15
as a single product resulted. There was an immediate
change in the color of the reaction mixture from light yellow to
intense yellow. This reaction may either result in the formation of
a discrete nanoscopic prism
17
17
or in the formation of a polymeric
31
P NMR spectrum of the reaction mixture
confirmed the formation of a highly symmetric species
product. However, the
17
by the
195
appearance of a sharp singlet with concomitant
Pt satellites,
shifted 5 ppm upfield (-Δ
. The upfield shift of the
phosphorus signal is indicative of the ligand-to-metal coordination.
The
δ
) relative to
14
1
H NMR spectrum is also indicative of the formation of a discrete
self-assembled prism
17
(Fig. 9.10). Similarly, the prism
18
was
prepared by the reaction of the acceptor
14
with the 1.5 equivalents
of the donor
C. The product
formed as the yellow precipitate was washed with acetone several
times.
16
in acetone medium for 12 h at 50
°
31
P NMR of the product in CDCl
showed a sharp singlet at
3
15.6 ppm.
An upfield shift of 4.5 ppm of the
31
1
P{
H} NMR signal of
14
upon
reaction with
and the complete disappearance of the peak due
to the starting acceptor clearly indicated the formation of a single
product (Fig. 9.11).
16
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