L.-C. Song et al. / Journal of Organometallic Chemistry 626 (2001) 192–198
197
2. Solid state reaction method. A 50-ml Schlenk flask
was charged with 0.155 g (0.3 mmol) of [(h5-
MeCOC5H4)2Mo2(CO)4] and 0.123 g (0.3 mmol) of
Ph2Te2. The finely powdered and uniformly mixed
reaction mixture was heated at 60°C for 3 h. After
TLC separation using CH2Cl2 as eluent, 0.245 g
(88%) of 3 was obtained.
2CH3), 4.22 (q, J=7.2 Hz, 4H, 2CH2), 5.40–5.70
(m, 4H, 2H3, 2H4), 5.74–5.94 (m, 4H, 2H2, 2H5),
7.08–7.62 (m, 10H, 2C6H5).
2. Solid state reaction method. A 50-ml Schlenk flask
was charged with 0.226 g (0.3 mmol) of [(h5-
EtO2CC5H4)2W2(CO)4] and 0.123 g (0.3 mmol) of
Ph2Te2. The finely powdered and uniformly mixed
reaction mixture was heated at 60°C for 3 h. After
TLC separation using CH2Cl2 as eluent, 0.282 g
(81%) of 6 was obtained.
3.4. Preparation of 4
The same procedure as that for 1 was followed, but
0.694 g (1.0 mmol) of [(h5-MeCOC5H4)2W2(CO)4] was
used instead of [(h5-C5H5)2Mo2(CO)4]. Using CH2Cl2 as
eluent, the main band afforded 0.870 g (79%) of 4 as a
brown solid. m.p. 147–148°C. Anal. Found: C, 32.14;
H 2.12. Calc. for C30H24O6Te2W2: C, 32.66; H, 2.19%.
IR (KBr disk, cm−1): acetyl carbonyl CꢂO 1682s;
3.7. Preparation of 7 and 8
The same procedure as that for 1 was followed, but
0.462 g (1.0 mmol) of [(h5-MeC5H4)2Mo2(CO)4] was
used instead of [(C5H5)2Mo2(CO)4]. Using acetone–
petroleum ether (v/v=1:5) as eluent, from the first
main band 0.276 g (34%) of 7 was obtained as a brown
solid. m.p. 135–137°C. Anal. Found: C, 38.54; H, 2.72.
Calc. for C28H24Mo2O4Te2: C, 38.29; H, 2.97%. IR
(KBr disk, cm−1): terminal CꢀO 1943s, 1916vs, 1846vs,
1829s. 1H-NMR (CHCl3-d): l=1.96 (s, 6H, 2CH3),
5.02–5.32 (m, 8H, 2C5H4), 7.12–7.50 (m, 10H, 2C6H5).
The second main band afforded 0.196 g (24%) of 8 as a
green solid. m.p. 178–180°C. Anal. Found: C, 33.76;
H, 2.03. Calc. for C31H28Mo2O5Te3: C, 33.72; H,
2.22%. IR (KBr disk, cm−1): terminal CꢀO 1981vs,
1955vs, 1920s, 1861s. 1H-NMR (CHCl3-d): l=2.29,
2.38 (s,s, 3H, CH3), 5.34–5.68 (m, 4H, C5H4), 6.96–
7.42 (m, 15H, 3C6H5). Crystal growing of 8 in acetone–
hexane (v/v=1:3) gave 8 with one molecule of acetone,
as a green crystal. Anal. Found: C, 35.01; H, 2.91. Calc.
for C31H28Mo2O5Te3·C2H6O: C, 35.28; H, 2.67%.
1
terminal CꢀO 1927vs, 1859vs, 1835s. H-NMR (CHCl3-
d): l=2.12 (s, 6H, 2CH3), 5.44–5.90 (m, 8H, 2C5H4),
7.04–7.60 (m, 10H, 2C6H5).
3.5. Preparation of 5
1. Solution reaction method. The same procedure as
that for 1 was followed, but 0.725 g (1.0 mmol) of
[(h5-MeO2CC5H4)2W2(CO)4] was used instead of
[(h5-C5H5)2Mo2(CO)4]. Using CH2Cl2 as eluent, the
main band gave 0.929 g (82%) of 5 as a brown solid.
m.p. 139–141°C. Anal. Found: C, 31.89; H, 2.12.
Calc. for C30H24O8Te2W2: C, 31.74; H, 2.13%. IR
(KBr disk, cm−1): ester carbonyl CꢂO 1720s; termi-
1
nal CꢀO 1956vs, 1919vs, 1894vs, 1865s, 1824s. H-
NMR (CHCl3-d): l=3.73 (s, 6H, 2CH3), 5.36–5.70
(m, 4H, 2H3, 2H4), 5.74–5.96 (m, 4H, 2H2, 2H5),
7.00–7.64 (m, 10H, 2C6H5).
3.8. X-ray structure determination of 6
2. Solid state reaction method. A 50-ml Schlenk flask
was charged with 0.218 g (0.3 mmol) of [(h5-
MeO2CC5H4)2W2(CO)4] and 0.123 g (0.3 mmol) of
Ph2Te2. The finely powdered and uniformly mixed
reaction mixture was heated at 60°C for 3 h. After
TLC separation using CH2Cl2 as eluent, 0.285 g
(84%) of 5 was obtained.
Single crystals of 6 suitable for X-ray diffraction
analysis were grown by slow evaporation of its
CH2Cl2–hexane (v/v=1:2) solution at about 5°C. The
single crystal of 6 (0.2×0.2×0.3 mm3) was glued to a
glass fiber and mounted on a Rigaku ACF 7R diffrac-
tometer. Data were collected at room temperature,
using graphite-monochromated Mo–Ka radiation (u=
,
0.71069 A). A total of 4397 independent reflections
3.6. Preparation of 6
were collected at 20°C by the ꢀ–2q scan mode, of
which 3923 independent reflections with I]3|(I) were
considered to be observed and used in subsequent
refinement. The data were corrected for Lorentz polar-
ization factors and empirical absorption. Crystallo-
graphic data are listed in Table 3.
1. Solution reaction method. The same procedure as
that for 1 was followed, but 0.754 g (1.0 mmol) of
[(h5-EtO2CC5H4)2W2(CO)4] was used instead of
[(h5-C5H5)2Mo2(CO)4]. Using CH2Cl2 as eluent, the
main band afforded 0.898 g (77%) of 6 as a brown
solid. m.p. 154–156°C. Anal. Found: C, 32.96; H,
2.50. Calc. for C32H28O8Te2W2: C, 33.04; H, 2.43%.
IR (KBr disk, cm−1): ester carbonyl CꢂO 1713vs;
terminal CꢀO 1948vs, 1919vs, 1890vs, 1871s, 1828vs.
1H-NMR (CHCl3-d): l=1.26 (t, J=7.2 Hz, 6H,
3.9. X-ray structure determination of 8
Single crystals of 8 suitable for X-ray diffraction
analysis were grown by slow evaporation of its ace-
tone–hexane (v/v=1:3) solution at about 5°C. The
Song, Li-Cheng
