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Addition of an excess of solid NH4PF6 was added until the
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solution became opaque. The resulting white solid was fil-
tered and discarded. The remaining solvent of a purple solu-
tion was then removed under through rotary evaporation.
The resulting solid was then sonicated in EtOH to remove
excess NH4PF6 and the remaining solid was filtered and
dried under reduced pressure to yield a gray-green solid.
Crystallographic data are provided in the SI. Yield = 194 mg
(0.26 mmol, 96%). Anal. Calcd for NiC24H22N6P2F12: C,
38.79; H, 2.98; N, 11.31. Found: C, 39.06; H, 2.72; N, 11.36.
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General procedure for photo-assisted reductive coupling re-
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Solution preparations were performed inside a N2-filled
glove box to confirm inert atmosphere. Vials were sealed in
the glovebox, then removed from the glovebox and per-
formed on the benchtop in closed vials. For a typical exper-
iment, 3.0 mg (3.2 × 10-6 mols) of PS, 2.4 mg (3.2 × 10-6
mols) of Cat, and 106 µl (0.8 × 10-3 mols) of TEOA were
mixed with 0.32 × 10-3 mols of substrate (100 times that of
the catalyst or the photosensitizer) in 4 ml of anhydrous ac-
etonitrile in a 12 ml glass vial with TFE/SIL O/T cap. The
catalytic solution was stirred under a white light source
passed through a longpass 400 nm cut-off filter for a period
of 12 – 18 hours. During the irradiation, a fan was used to
prevent heating of the vials on the stir plate. Monitoring the
temperature during the reaction showed the reactions were
o
o
performed at a temperature range of 23 C to 28 C. The
products were purified by column chromotography using ei-
ther diethylether or pentane or pentane/diethylether or hex-
ane or hexane/ethyl acetate mixture as eluent.
Spectroscopic characterization of all products can be found
in the supporting information. Data match previously re-
ported data for all previously reported compounds.
ASSOCIATED CONTENT
Supporting Information.
1H,13C NMR product spectra, crystal structures, cyclic volt-
ammorgram of Cat, UV-Vis of Cat. References to previ-
ously reported compounds. This material is available free of
AUTHOR INFORMATION
Corresponding Author
*vannucci@mailbox.sc.edu
ACKNOWLEDGMENT
The authors gratefully acknowledge support for this work by
the University of South Carolina.
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