806
TORUBAEV et al.
C(5)
C(6)
C(4)
C(7)
C(14)
C(13)
C(3)
C(2)
C(9)
C(8)
C(1)
I(1)
C(12)
C(10)
C(11)
Te(1)
I(2)
I(3)
Fig. 1. Molecule IA in crystal structure I.
formed consisted of thick needles of complex II and
prisms of the known complex III [6].
Fe(CO)5
20°C, THF
Ph
I
Ph
Te I
Ph
Ph
Te
Fe
Below are the IR spectra and elemental analysis data
for complexes II and III.
OC
OC
I
I
IR (KBr, cm–1): 2125 s, 2085 s, 2070 s. IR (heptane,
CO
cm–1): 2125 m, 2075 s, 2060 m.
For C17H11TeI3O2Te(II) (M = 827.43)
EXPERIMENTAL
anal. calcd. (%):
C, 24.68;
H 1.34.
H 0.87.
All manipulations dealing with the synthesis and Found (%):
C, 20.88;
For C4FeI2O4(III) (M = 421.70)
anal. calcd. (%):
isolation of the complexes were carried out under pure
argon in dehydrated solvents. IR spectra were recorded
on a Specord 75IR spectrophotometer for pellets with
KBr and solutions in heptane.
C, 11.39.
The complexes are unstable under the conditions of
column chromatography. The crystals of complexes II
and III for X-ray diffraction analysis were selected by
mechanical separation.
Synthesis of PhTeI2HC=CPhI (I). Triiodo(phe-
nyl)tellurium (1.15 g, 2 mmol) (prepared from PhTe2
(0.4 g) and I2 (0.75 g)) and phenylacetylene (0.22 ml,
2 mmol) were refluxed in THF (30 ml) for 12 h. The
solvent was removed in a water aspirator vacuum. The
orange red residue was washed with light petroleum.
The product was extracted with CH2Cl2 and precipi-
tated by concentrating the extract with heptane in a
water aspirator vacuum. Crystals suitable for X-ray dif-
fraction analysis were grown from a concentrated solu-
tion of complex I in CH2Cl2–heptane (1 : 1).
X-ray diffraction analysis. Selected crystallo-
graphic parameters and a summary of data collection
and refinement for structures I–III are given in Table 1.
All structures were solved by the direct method and
refined by the least-squares method on F2 in the aniso-
tropic (for H atoms, isotropic) approximation with the
SHELXTL program package [7]. The hydrogen atoms
were located geometrically. Selected bond lengths and
angles in structures I–III are given in Tables 2 and 3.
Atomic coordinates and other structural parameters of
complexes I–III have been deposited with the Cam-
bridge Crystallographic Data Center (CCDC
nos. 688683 (I), 690063 (II), and 688684 (III); see
http://www.ccdc.cam.ac.uk/data_request/cif).
For C14H11I3Te (M = 687.55) anal. calcd. (%):
C, 24.46; H, 1.61.
Found (%): C, 24.70; H, 1.85.
IR (KBr, cm–1): 720 s, 680 s, 650 s.
Synthesis of (CO)3FeI2(PhTe–CH=CPhI) (II) and
Fe(CO)4I2 (III). Iron pentacarbonyl (0.04 ml,
0.28 mmol) was added in one portion at room tempera-
ture to a magnetically stirred orange red solution of
complex I (0.16 g, 0.23 mmol) in diethyl ether (30 ml).
RESULTS AND DISCUSSION
We carried out a reaction of PhTeI3 with phenylacet-
Stirring was continued for an additional 30 min. The ylene in boiling THF. More prolonged reflux was
reaction mixture turned deep red and homogeneous and required, in contrast to analogous reactions with
no longer contained the starting complex I (TLC data). (aryl)dibromotellurium(IV) and (aryl)dichlorotellu-
The solution was concentrated with heptane (5 ml) rium(IV) usually completed in 3–10 h. The resulting
in vacuo to slight turbidity. The concentrate was kept at dark orange crystals of the adduct were stable in air and
–10°ë for 12 h. The dark red crystalline precipitate that soluble in polar organic solvents. According to X-ray
RUSSIAN JOURNAL OF COORDINATION CHEMISTRY Vol. 34 No. 11 2008
Torubaev
