Biometals
the literature procedure. Solid PdCl2(NCMe)2 (0.06 g,
0.25 mmol) was added to a dichloromethane solution
of 2-(2-(diphenylphosphino)ethyl)pyridine (L1)
(0.15 g, 0.50 mmol) and stirred at room temperature
overnight. The solvent was removed in vacuo and a
yellow powder was obtained, which was recrystallized
from a mixture of dichloromethane and hexane to give
3. Yield = 0.16 g, 80 % (0.16 g). 1H NMR (CDCl3):
9.49 (d, 1H, J = 5.6 Hz), 7.84 (q, 4H, J = 7.6 Hz),
7.79 (t, 1H), 7.46 (m, 6H), 7.33 (d, 1H, J = 7.6 Hz),
7.25 (t, 1H), 3.46 (dt, 2H, J = 17.2 & 26.8 Hz), 2.20
(t, 2H). 31P{1H} (CDCl3): 25.34 (s, 1P). 13C{1H}
NMR (CDCl3): 23.1, 23.3, 30.9; 35.8; 123.4; 125.2;
128,7, 128.8, 128.9; 129.3; 131.8; 133.3, 133.4; 139.9;
155.8; 158.6, 158.7. Anal. Calcd. for C38H36N2P2-
PdCl2ÁCH2Cl2: C, 48.53; H, 4.17; N, 2.76 %. Found:
C, 48.66; H, 3.77; N, 2.98 %.
some crystalized with solvents, as such the structures
are reported as supplementary materials.
A crystal of 1 (as a representative procedure) of
dimensions 0.18 9 0.17 9 0.06 mm-3 was selected
and glued on to the tip of a glass fibre. The crystal was
then mounted in a stream of cold nitrogen at 100(1) K
and centred in the X-ray beam by using a video
camera. The crystal evaluation and data collection
was performed on a Bruker APEXII diffractometer
˚
with Mo Ka (k = 0.71073 A) radiation and diffrac-
tometer to crystal distance of 4.00 cm. The initial cell
matrix was obtained from three series of scans at
different starting angles. Each series consisted of 12
frames collected at intervals of 0.5° in a 6° range with
the exposure time of 10 s per frame. The reflections
were successfully indexed by an automated indexing
routine built in the APEXII program suite (Bruker-
AXS 2009). The final cell constants were calculated
from a set of strong reflections from the actual data
collection.
{Bis-(2-(2-(diphenylphosphino)
ethyl)pyridyl}platinum(II) chloride (4)
The data was collected by using the full sphere data
collection routine to survey the reciprocal space to the
A
dichloromethane solution (20 ml) of 2-(2-
˚
extent of a full sphere to a resolution of 0.75 A. A total
diphenylphosphino)ethylpyridine (0.15 g, 0.50 mmol)
was stirred at room temperature to which [PtCl2(-
SMe2)2] (0.20 g, 0.50 mmol) was added. The solution
was stirred overnight; and after removal of solvent the
crude product purified by recrystallizing from dichlor-
omethane and hexane. Yield = 0.17 g, 75 %. 1H NMR
(CDCl3): 9.58 (d, 1H, J = 6.0 Hz), 7.82 (m, 5H), 7.45
(m, 6H), 7.30 (d, 1H, J = 7.6 Hz), 7.20 (t, 1H), 3.45 (dt,
2H, J = 14.8 & 26.8 Hz), 2.21 (t, 2H). 31P{1H}
(CDCl3): 2.06 (s, 1P, JPt-P = 4668 & 4676 Hz).
13C{1H} NMR (d6-DMSO): 20.5; 21.0; 35.8; 124.0;
125.9; 128.5, 128.6; 129.3; 131.4, 131.5; 133.0, 133.2;
140.2; 154.6; 159.2, 159.3. Anal. Calcd. for C19H18-
NPPtCl2: C, 39.34; H, 3.20; N, 2.35 %. Found, C,
39.84; H, 2.89; N, 2.25 %.
of 4286 data points were harvested by collecting 1991
frames at intervals of 0.5° scans in x and u with
exposure times of 10 s per frame. These highly
redundant data sets were corrected for Lorentz and
polarization effects. The absorption correction was
based on fitting a function to the empirical transmis-
sion surface as sampled by multiple equivalent
measurements (Bruker-AXS 2009).
The systematic absences in the diffraction data
were uniquely consistent for the space group P1 that
yielded chemically reasonable and computationally
stable results of refinement. A successful solution by
the direct methods of SIR92 provided all non-hydro-
gen atoms from the E-map (Altomore et al. 1993). All
non-hydrogen atoms were refined with anisotropic
displacement coefficients. All hydrogen atoms except
those on the solvent water molecules were included in
the structure factor calculation at idealized positions
and were allowed to ride on the neighbouring atoms
with relative isotropic displacement coefficients. The
final least-squares refinement of 205 parameters
against 4286 data points resulted in residuals R (based
on F2 for I C 2r) and wR (based on F2 for all data) of
0.0198 and 0.0515, respectively. The final difference
Fourier map was featureless. The molecular diagrams
X-ray data collection, structure solution
and refinement
Single crystals of complexes 1–4 suitable for X-ray
diffraction were obtained by slow diffusion of hexane
into dichloromethane solution of the respective com-
pound. The structures were determined in order to
confirm the identity of all four complexes proposed
from their NMR data. Some of these structures have
been reported in the literature, although in our hands
123
Gama, Ntombenhle H.
