Homogeneous CO Hydrogenation: Ligand Effects on the Lewis Acid ...

NMR-scale reaction of [1-M 2][B(C 6F 5) 4] with 1 equiv [HPt][PF 6] in the presence of
[hept 4N][BF 4].
A small vial was charged with 29.1 mg (0.0180 mmol) [1-M 2][B(C 6F 5) 4], 17.7 mg (0.0360 mmol,
2 equiv) tetraheptylammonium tetrafluoroborate, and ~0.6 mL C 6D 5Cl. With stirring, 11.6 mg
(0.0180 mmol, 1 equiv) [HPt][PF 6] was added as a solid. The mixture was moved to a J-Young
tube, and allowed to sit for about 3 hours, at which point NMR spectroscopy showed near
complete conversion to the desired boroxycarbene. As in the isolated product, at room
temperature many resonances were quite broad, including the 31 P NMR. Variable temperature
NMR studies were therefore undertaken.
Variable Temperature NMR spectroscopy:
Figure S66. 31 P{ 1 H} NMR from -35 to 95 C.
S58