1
Modular self-assembled multiporphyrin cages with tunable shape
Enzo Alessio,
a
Massimo Casanova,
a
Ennio Zangrando
a
and Elisabetta Iengo*
a
a
Department of Chemical and Pharmaceutical Sciences, University of Trieste, Italy. Fax:
+390405583903; Tel: +390405583955; E-mail: eiengo@units.it
Electronic Supplementary Information
1D and 2D NMR experiments were recorded at 500 MHz on a Varian 500 spectrometer. Proton
peak positions were referenced to the peak of residual non deuterated solvent (set at δ 7.26 for
CDCl
3
).
Solvents for spectroscopic measurements were of spectroscopic grade, all the other solvents were of
reagent grade quality, and used as received. CDCl
3
, used in NMR experiments, was treated with
basic alumina prior to use.
Abbreviations: 4'-cisDPyP = 5,10-bis(4'-pyridyl)-15,20-diphenylporphyrin, 4'-transDPyP = 5,15-
bis(4'-pyridyl)-10,20-diphenylporphyrin, 4'-transPyPDI = N,N'-di(4-pyridyl)-perylene-3,4:9,10-
tetracarboxylic acid bisimide, tpt = 2,4,6-tris(4-pyridyl)triazine, 4'-TPyP = 5,15,10,20-(4'-pyridyl)-
porphyrin, 4'-TPhPyP = 5,15,10,20-(4'-pyridylphenyl)-porphyrin.
4-(4-formylphenyl)pyridine and pyrrole were purchased from Aldrich. Metallacycle 1 was
synthesized as previously reported.
9
tpt was synthesized as reported in the literature.
1S
4'-TPhPyP
was synthesized according to literature procedures, via condensation of 4-(4-formylphenyl)pyridine
and pyrrole.
2S
Synthesis of 2 - 4: metallacycle 1 (20 mg, 1.1 × 10
-2
mmol) and tpt (5 mg, 1.65 × 10
-2
mmol) were
dissolved in CHCl
3
(20 mL) and the solution was stirred at room temperature for 15 min.
Concentration in vacuo to ca. 5 mL followed by addition of n-hexane induced the precipitation of 2
as a violet solid, that was isolated by filtration, washed with n-hexane and vacuum dried (21 mg,
95%). A similar procedure was followed for 3 and 4: equimolar amounts of 1 (20 mg, 1.1 × 10
-2
mmol) and 4'-TPyP (3 mg, 5.49 × 10
-3
mmol) or 4'-TPyP (5 mg, 5.49 × 10
-3
mmol) yielded 3 (22
mg, 95%) or 4 (24 mg, 95%), respectively, as a dark-violet solids.
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This journal is © The Royal Society of Chemistry 2012