Organometallics
ARTICLE
X-ray Crystallography. Crystal data for compounds 1ꢀ12 are
given in Tables 3ꢀ5, and further details of the structure determinations
are in the Supporting Information. Bond lengths and angles are listed in
Table 1. Crystals were examined variously on a Bruker APEX CCD area
detector diffractometer using graphite-monochromated Mo Kα radia-
tion (λ = 0.71073 Å), or on an Oxford Diffraction SuperNova Atlas
CCD diffractometer using mirror-monochromated Cu Kα radiation
(λ = 1.5418 Å). Intensities were integrated from data recorded on 0.3
(APEX) or 1° (SuperNova) frames by ω rotation. Cell parameters were
refined from the observed positions of all strong reflections in each data
set. Semiempirical absorption correction based on symmetry-equivalent
and repeat reflections (APEX) or Gaussian grid face-indexed absorption
correction with a beam profile correction (Supernova) were applied.
The structures were solved variously by direct and heavy atom methods
and were refined by full-matrix least-squares on all unique F2 values, with
anisotropic displacement parameters for all non-hydrogen atoms, and
with constrained riding hydrogen geometries; Uiso(H) was set at 1.2
(1.5 for methyl groups) times Ueq of the parent atom. The methanide
hydrogens were initially located in the Fourier difference map to confirm
the methanide geometries and were subsequently idealized and refined
using a riding model. The largest features in final difference syntheses
were close to heavy atoms and were of no chemical significance. Highly
disordered solvent molecules of crystallization in 3, 4, and 10 could
not be modeled and were treated with the Platon SQUEEZE
procedure.31 Programs were Bruker AXS SMART32 and CrysAlisPro33
(control), Bruker AXS SAINT32 and CrysAlisPro33 (integration), and
SHELXTL34 and OLEX235 were employed for structure solution and
refinement and for molecular graphics.
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’ ASSOCIATED CONTENT
(27) Van Vleck, J. H. Theory of Electric and Magnetic Susceptibilities;
Oxford University Press: Oxford, U.K., 1932.
(28) Cotton, S. Lanthanide and Actinide Chemistry; Wiley: Chichester,
U.K., 2006.
S
Supporting Information. CIF files giving crystallographic
b
data for 1ꢀ12. This material is available free of charge via the
(29) Evans, W. J.; Hozbor, M. J. Organomet. Chem. 1987, 326, 299
and references therein.
’ AUTHOR INFORMATION
(30) Wooles, A. J.; Mills, D. P.; Lewis, W.; Blake, A. J.; Liddle, S. T.
Dalton Trans. 2010, 39, 500.
(31) Spek, A. L. Platon; University of Utrecht: Utrecht, The
Netherlands, 2000.
Corresponding Author
*E-mail: stephen.liddle@nottingham.ac.uk.
(32) SMART and SAINT; Bruker AXS Inc.: Madison, WI, 2001.
(33) CrysAlis PRO; Agilent Technologies: Yarnton, England, 2010.
(34) Sheldrick, G. M. Acta Crystallogr., Sect. A 2008, 64, 112.
(35) Dolomanov, O.V.; Bourhis, L. J.; Gildea, R. J.; Howard, J. A. K.;
Puschmann, H. J. Appl. Crystallogr. 2009, 42, 339.
’ ACKNOWLEDGMENT
We thank the Royal Society for a University Research Fellowship
(S.T.L.), and the EPSRC, European Research Council, and
the University of Nottingham for generously supporting
this work.
’ REFERENCES
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dx.doi.org/10.1021/om200729x |Organometallics 2011, 30, 5326–5337