(
)
262
F.-W. Lee et al.rJournal of Organometallic Chemistry 552 1998 255–263
Ž
.
Ž
tate a red product. Yield: 0.2 g 33% . Recrystallization
at ambient temperature by diffusion of diethyl ether into
an acetonitrile solution gave red crystals suitable for
reflections minimum and maximum transmission fac-
.
tors 0.340 and 1.000 . Upon averaging the 5095 reflec-
Ž
tions, 4844 of which were uniquely measured, Rint s
X-ray crystallography. nCO Nujol : 1577 cmy1. Calc.
for C34 H57 N6O5Cr2 F18 P3 Mr 1168.78 : C, 34.94; H,
4.92; N, 7.19. Found: C, 35.31; H, 5.06; N, 7.04.
FAB-MS: mrz 358 Me3TACN Cr PhCH2CO2
Ž
.
.
Ž .
0.014 . 4362 reflections with I)3s I were consid-
ered observed and used in the structural analysis. The
structure was solved by heavy-atom Patterson methods,
Ž
.
2q
Ž
w
Ž
.
Ž
.
x
.
.
w
x
expanded using Fourier techniques 38 and refined by
full-matrix least squares using the MSC-Crystal Struc-
w
x
3.6. Structural determination of 1a
ture Package TeXsan 39 on a Silicon Graphics Indy
computer. The 49 non-H atoms were refined anisotropi-
cally and the 46H atoms at calculated positions with
thermal parameters equal to 1.3 times that of the at-
tached C atoms were not refined. Convergence for 442
variable parameters by least squares refinement on F
A pale yellow plate shaped crystal of dimensions
0.15=0.10=0.30 mm was used for data collection at
301 K on a Rigaku AFC7R diffractometer with graphite
˚
Ž
.
monochromatized Mo–K a radiation ls0.71073 A
2
2
with ws4Fo2rs 2 Fo , where s Fo s s I q
2Ž
.
w
2Ž .
Ž
Ž
.
using v–2u scans with v-scan angle 0.68q0.35 tan
y1
2
2
.
Ž
Ž
.
x
Ž .
for 4362 reflections with I)3s I was
u 8 at a scan speed of 16.0 deg min
up to 4 scans for
0.010 Fo
Ž ..
Ž
reflection I-15 s I . Intensity data in the range of
2umax s458; h: 0 to 14; k:y15 to 15; l: y11 to 11 and
3 standard reflections measured after every 300 reflec-
reached at Rs0.031 and wRs0.037 with a goodness-
Ž
.
of-fit of 2.46. Drs max s0.05. The final difference
Fourier map was featureless, with maximum positive
y3
˚
.
tions showed decay of 1.27% , were corrected for decay
and negative peaks of 1.24 and 1.16 e A respectively.
and for Lorentz and polarization effects, and empirical
absorption corrections based on the c-scan of four
Ž
strong reflections minimum and maximum transmis-
4. Supplementary material
.
sion factors 0.945 and 1.000 . Upon averaging the 5132
reflections, 4874 of which were uniquely measured,
Listings of crystal data and refinement, atomic coor-
dinates, calculated coordinates, thermal parameters,
bond lengths and angles and structure factors for 1a, 2
and 3 are available as Supplementary Material from the
authors.
Ž
.
Ž .
Rint s0.048 , 3780 reflections with I)3 s I were
considered observed and used in the structural analysis.
The structure was solved by Patterson methods, ex-
Ž
w x.
panded by Fourier methods PATTY 38 and refined
by full-matrix least squares using the software package
w
x
TeXsan 39 on a Silicon Graphics Indy computer. The
46 H atoms at calculated positions with thermal parame-
ters equal to 1.3 times that of the attached C atoms were
not refined. Convergence for 442 variable parameters
Acknowledgements
We thank The University of Hong Kong and the
Hong Kong Research Grants Council for financial sup-
port.
by least squares refinement on
F
with w s
4Fo2rs 2 Fo , where s Fo s s I q 0.010 Fo
2
2
2 2
Ž
.
2Ž
.
w
2Ž .
Ž .
Ž
. x
for 6327 reflections with I)3 s I was reached at
Rs0.042 and wRs0.051 with a goodness-of-fit of
Ž
.
2.02. Drs max s0.01. The final difference Fourier
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˚
w x
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Ž
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8
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.
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¨
Lee, Fu-Wa
