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

Table 1 (cont.)
Structure solution and Refinement
Structure solution program SHELXS-97 (Sheldrick, 2008)
Primary solution method Direct methods
Secondary solution method Difference Fourier map
Hydrogen placement Geometric positions
Structure refinement program SHELXL-97 (Sheldrick, 2008)
Refinement method Full matrix least-squares on F 2
Data / restraints / parameters 29574 / 117 / 983
Treatment of hydrogen atoms Riding
Goodness-of-fit on F 2 2.971
Final R indices [I>2σ(I), 24164 reflections] R1 = 0.0371, wR2 = 0.0708
R indices (all data) R1 = 0.0515, wR2 = 0.0713
Type of weighting scheme used Sigma
Weighting scheme used w=1/σ 2 (Fo 2 )
Max shift/error 0.005
Average shift/error 0.000
Largest diff. peak and hole 4.938 and -2.452 e.Å -3
Special Refinement Details
Crystals were mounted on a glass fiber using Paratone oil then placed on the diffractometer under a
nitrogen stream at 100K.
One of the borabicylcononane ligands is disordered by a rotation around the B-C bond. Both the minor
(34%) and major (66%) components were restrained to the same geometry as the ordered ligand. The minor
component was refined as isotropic and the major component was refined as anisotropic but was restrained to
simulate isotropic behavior. The dichloroethane solvent of crystallization was also disordered with both orientations
apparently sharing one common Cl site and the ethyl portion flipped about the approximated Cl-Cl vector. The
minor component (34%) was refined isotropically and the major component (66%) anisotropically; no geometry
restraints were imposed.
S184