reactions and sample manipulations were carried out using standard
Schlenk techniques under nitrogen and in dried solvents. All of the
reagents were commercial products (Aldrich) of the highest purity
available and were used as received, except [NR4]2[Pt3n(CO)6n] (n = 2–4)1 (link) and
[NR4]2[Ni6CO)12] (R =
Et, Bu),44 (link) which have been prepared according
to the literature. Analyses of C, H, and N were obtained with a Thermo
Quest Flash EA 1112NC instrument. Analysis of Ni and Pt were performed
by microwave plasma-atomic emission spectrometry on a Agilent 4210
MP-AES instrument. IR spectra were recorded on a PerkinElmer Spectrum
One interferometer in CaF2 cells. ESI mass spectra were
recorded on a Waters Micromass ZQ4000 instrument using CH3CN as the solvent (source temperature 150 °C; capillary voltage
2.54 kV; infusion flow 20 μL/min; cone voltage 10 V). 195Pt and 13C{1H} NMR measurements were performed
on Varian Mercury Plus 400 MHz and Varian Inova 300 MHz spectrometers.
The carbon chemical shifts were referenced to a nondeuterated aliquot
of the solvent. The platinum chemical shifts were referenced to external
Na2PtCl6 (1.2 M in D2O). Structure
drawings have been created with SCHAKAL99.45 Caution! CO and Ni(CO)4 may be
generated during manipulation of these compounds. All of the operations
must be carried out under a well-ventilated fume hood.