Electronic Supplementary Information for Dalton Transactions
This journal is © The Royal Society of Chemistry 2007
1
Electronic Supplementary Information for Dalton Transactions
This journal is © The Royal Society of Chemistry 2007
Supporting Informations for:
Silver(I)-organophosphane complexes of electron withdrawing CF
3
- or NO
2
-
substituted scorpionate ligands
Maura Pellei,
a
Simone Alidori,
a
Grazia Papini,
a
Giancarlo Gioia Lobbia,
a
John D. Gorden,
b
H. V. Rasika
Dias,
b
and Carlo Santini
a
a
Dipartimento di Scienze Chimiche, Università di Camerino, via S. Agostino 1, 62032 Camerino (MC), Italy. E-
mail: carlo.santini@unicam.it
b
Department of Chemistry and Biochemistry, Box 19065, The University of Texas at Arlington, Arlington, Texas
76019-0065. E-mail: dias@uta.edu
Material and methods
Elemental analyses (C,H,N,S) were performed in house with a Fisons Instruments 1108 CHNS-O
Elemental Analyser. Melting points were taken on an SMP3 Stuart Scientific Instrument. IR spectra
were recorded from 4000 to 100 cm
-1
with a Perkin-Elmer System 2000 FT-IR instrument. IR
annotations used: m = medium, mbr = medium broad, s = strong, sbr = strong broad, sh = shoulder, w
= weak.
1
H-,
13
C-,
19
F- and
31
P-NMR spectra were recorded on a Oxford-400 Varian spectrometer
(400.4 MHz for
1
H, 100.1 MHz for
13
C, 376.8 MHz for
19
F, and 162.1 MHz for
31
P). Chemical shifts
for
1
H NMR spectra are relative to internal Me
4
Si.
13
C NMR spectra were run with
1
H decoupling, and
the chemical shifts are reported in ppm vs Me
4
Si.
19
F NMR and
31
P NMR chemical shifts were
referenced to an external CFCl
3
and an 85% H
3
PO
4
standard, respectively. The
31
P NMR spectroscopic
data were accumulated with
1
H decoupling. NMR annotations used: d = doublet, dd = double doublet,
dbr = broad doublet, m = multiplet, mbr = broad multiplet, s = singlet, sbr = broad singlet, t = triplet.
Electrospray mass spectra (ESIMS) were obtained in positive- or negative-ion mode on a Series 1100
MSD detector HP spectrometer, using an acetone mobile phase. The compounds were added to the
reagent grade methanol to give solutions of approximate concentration 0.1 mM. These solutions were
injected (1 μl) into the spectrometer via a HPLC HP 1090 Series II fitted with an autosampler. The
pump delivered the solutions to the mass spectrometer source at a flow rate of 300 μl min
-1
, and
nitrogen was employed both as a drying and nebulizing gas. Capillary voltages were typically 4000 V
and 3500 V for the positive- and negative-ion mode, respectively. Confirmation of all major species in