K. Mashima et al. / Journal of Organometallic Chemistry 607 (2000) 51–56
55
Table 3
reflections. An empirical absorption correction was ap-
plied on the basis of azimuthal scans. The data was
corrected for Lorentz and polarization effects.
Crystal and refinement data for 8a
Formula
C65H62NCl7P4Ru2
The structure of complex 8a was solved by a direct
method (SHELXS-86) [33] and refined by the full-matrix
least-squares method. Measured non-equivalent reflec-
tions were used for the structure determination. In the
subsequent refinement, the function Sꢀ(ꢀFoꢀ−ꢀFcꢀ)2 was
minimized, where ꢀFoꢀ and ꢀFcꢀ are the observed and
calculated structure factor amplitudes, respectively. The
agreement indices are defined as R1=S(ꢀꢀFoꢀ−ꢀFcꢀꢀ)/
SꢀFoꢀ and wR2=[Sꢀ(F2o−Fc2)2/S(ꢀF4o)]1/2. The posi-
tions of all non-hydrogen atoms for all complexes were
found from a difference Fourier electron density map
and refined anisotropically. All hydrogen atoms were
Formula weight
Crystal system
Space group
1431.618
Triclinic
(
P1 (c2)
,
a (A)
15.700(4)
33.96(1)
13.137(4)
98.48(3)
104.04(2)
87.74(2)
4
,
b (A)
,
c (A)
h (°)
i (°)
k (°)
Z
3
,
V (A )
6720(3)
1.415
Mo–Ka
+h, +k, 9l
0.27×0.20×0.17
8.61
Dcalc (g cm−3
)
Radiation
Reflections measured
Crystal size (mm)
Absorption coefficient (cm−1
Scan mode
Temperature (°C)
2q max (°)
,
placed in calculated positions (CꢀH=0.95 A) and kept
)
fixed. All calculations were performed using the
ꢀ
TEXSAN crystallographic software package.
23
55.1
Data collected
31 990
Unique data
30 851 (Rint=0.072)
30 837
1423
Acknowledgements
No. of observations
No. of variables
R [I\3|(I)]
We thank Dr N. Sayo (Takasago International
Corp., Japan) for his helpful discussions. This work
was financially supported by a Grant-in-Aid for Scien-
tific Research on Priority Area (no. 283, ‘Innovative
Synthetic Reactions’) from the Ministry of Education,
Science and Culture, Japan. Y.M. is a research fellow
of the Japan Society for the Promotion of Science,
1998–2000.
0.064
Rw [I\3|(I)]
R1 (all data)
0.064
0.189
0.190
1.38
wR2 (all data)
Goodness-of-fit on F2
−3
,
Largest difference peak and hole (e A
)
2.28 and −1.91
crystallized from a mixture of dichloromethane (15 ml)
and hexane (15 ml). Orange–yellow crystals of 8a (87.4
mg, 47% yield) were obtained; m.p. 284–286 (dec.).
References
2
1H-NMR (270 MHz, CDCl3, 30°C): l 1.09 (t, JHH
=
7.3 Hz, 6H, ꢀCH2CH3), 2.92 (m, 4H, ꢀCH2CH3), 6.8–
7.7 (m, 48H, aromatic protons), 8.16 (broad s, 2H,
H2N). 31P{1H}-NMR (109 MHz, CDCl3, 30°C): l 79.7
(s). Elemental analyses showed that 8a crystallized with
free diethylammonium chloride, and thus did not give a
satisfactory result.
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Single crystals suitable for X-ray measurements were
obtained by recrystallization of 8a from a mixture of
dichloromethane and hexane. A crystal of 8a was sealed
in a glass capillary under an argon atmosphere, and
then was mounted on a Rigaku AFC-7R four-circle
diffractometer for data collection using Mo–Ka
(graphite monochromated, u=0.71069) radiation. Rel-
evant crystal and data statistics are summarized in
Table 3. The unit cell parameters and the orientation
matrix at 23°C were determined by a least-squares fit to
2q values of 25 strong higher reflections. Three stan-
dard reflections were chosen and monitored every 150
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Asymm. 2 (1991) 47.
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